data_global
_audit_update_record
;
2010-09-14 # Formatted by publCIF
;
#===========================================================================
# 1. SUBMISSION DETAILS
#===========================================================================
# Name and address of author for correspondence
_publ_contact_author_name 'Sylvain Bernes'
_publ_contact_author_address
;
Universidad Aut\'onoma de Nuevo Le\'on
Facultad de Ciencias Qu\'imicas
Av. Universidad S/N
Ciudad Universitaria
San Nicol\'as de los Garza
Nuevo Le\'on 66451
Mexico
;
_publ_contact_author_phone ?
_publ_contact_author_fax ?
_publ_contact_author_email sylvain_bernes@hotmail.com
_publ_contact_author_id_iucr 9661
_publ_requested_journal Crystals
_publ_requested_category ?
_publ_requested_coeditor_name ?
_publ_contact_letter ?
#============================================================================
# 2. PROCESSING SUMMARY (IUCr Office Use Only)
#===========================================================================
_journal_date_recd_electronic 2008-05-14
_journal_date_to_coeditor ?
_journal_date_from_coeditor ?
_journal_date_accepted ?
_journal_date_printers_first ?
_journal_date_printers_final ?
_journal_date_proofs_out ?
_journal_date_proofs_in ?
_journal_coeditor_name ?
_journal_coeditor_code ?
_journal_paper_category ?
_journal_coeditor_notes ?
_journal_techeditor_code ?
_iucr_compatibility_tag ACTA95
_journal_techeditor_notes ?
_journal_coden_ASTM ?
_journal_name_full ?
_journal_year ?
_journal_volume ?
_journal_issue ?
_journal_page_first ?
_journal_page_last ?
_journal_suppl_publ_number ?
_journal_suppl_publ_pages ?
#============================================================================
# 3. TITLE AND AUTHOR LIST
#===========================================================================
_publ_section_title ?
_publ_section_title_footnote .
loop_
_publ_author_name
_publ_author_footnote
_publ_author_email
_publ_author_address
"Olgu\'in, Juan" . juan.olguintalavera@ucd.ie
;
University College Dublin
School of Chemistry and Chemical Biology
Belfield
Dublin, 4
Ireland
;
"Bern\`es, Sylvain" . sylvain_bernes@Hotmail.com
;
Universidad Aut\'onoma de Nuevo Le\'on, UANL
Facultad de Ciencias Qu\'imicas
Av. Universidad S/N
Ciudad Universitaria
San Nicol\'as de los Garza
Nuevo Le\'on CP 66451
Mexico
;
"Gasque, Laura" . gasquel@unam.mx
;
Universidad Nacional Aut\'onoma de M\'exico, UNAM
Facultad de Qu\'imica
Ciudad Universitaria
M\'exico D.F., CP 04510
Mexico
;
#============================================================================
# 4. TEXT
#===========================================================================
_publ_section_synopsis .
_publ_section_abstract .
_publ_section_related_literature .
_publ_section_comment .
_publ_section_exptl_prep .
_exptl_special_details ?
_publ_section_exptl_refinement .
_publ_section_references
;
Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P.,
Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst.
39, 453--457.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
Siemens (1996). XSCANS (Version 2.21). Siemens Analytical X-ray
Instruments Inc., Madison, Wisconsin, USA.
;
_publ_section_figure_captions ?
_publ_section_table_legends ?
_publ_section_acknowledgements ?
#===========================================================================
# 5. STRUCTURE [Cu2(H2O)4(dimeim)].(BF4)4 (1)
#===========================================================================
data_1
# clave original: CuDBO (ICUAP, 2003)
# clave original:
# clave Tesis:
_database_code_CAS ?
_database_code_CSD ?
_audit_creation_method SHELXL97
_audit_creation_date 2011-08-26
loop_
_audit_contact_author_name
_audit_contact_author_address
_audit_contact_author_email
_audit_contact_author_fax
_audit_contact_author_phone
'Bern\`es, Sylvain'
;
Universidad Aut\'onoma de Nuevo Le\'on, UANL
Facultad de Ciencias Qu\'imicas
Av. Universidad S/N
Ciudad Universitaria
San Nicol\'as de los Garza
Nuevo Le\'on CP 66451
Mexico
;
sylvain_bernes@Hotmail.com . .
_chemical_name_systematic
;
[\m-2,2'-(2,8-Dimethyl-4,7,10,12-tetrahydrodi-imidazo[4,5-c:4',5'-
h][1,6]diazecine-5,11(1H,6H)-diyl)bis(N,N-
dimethylethanamine)]-tetra-aqua-di-copper(ii) tetrakis(tetrafluoridoborate)
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C20 H44 Cu2 N8 O4, 4(B F4)'
_chemical_formula_sum 'C20 H44 B4 Cu2 F16 N8 O4'
_chemical_formula_weight 934.95
_chemical_compound_source methanol
_chemical_absolute_configuration .
_chemical_optical_rotation ?
_chemical_properties_physical ?
_chemical_properties_biological ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'B' 'B' 0.0013 0.0007
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'F' 'F' 0.0171 0.0103
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cu' 'Cu' 0.3201 1.2651
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.455(2)
_cell_length_b 12.0445(17)
_cell_length_c 16.493(2)
_cell_angle_alpha 87.469(10)
_cell_angle_beta 83.061(14)
_cell_angle_gamma 75.465(14)
_cell_volume 1804.7(5)
_cell_formula_units_Z 2
_cell_measurement_temperature 296(2)
_cell_measurement_reflns_used 75
_cell_measurement_theta_min 4.59
_cell_measurement_theta_max 12.54
_exptl_crystal_description prism
_exptl_crystal_colour blue
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.721
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 948
_exptl_absorpt_coefficient_mu 1.303
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_correction_T_min 0.31049
_exptl_absorpt_correction_T_max 0.35601
_exptl_absorpt_process_details 'XSCANS (Siemens, 1996)'
_exptl_special_details ?
_diffrn_ambient_temperature 296(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Siemens P4'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 3
_diffrn_standards_interval_count 97
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
1 1 -3
1 2 3
1 -2 -2
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% 2
_diffrn_reflns_number 14469
_diffrn_reflns_av_R_equivalents 0.0306
_diffrn_reflns_av_sigmaI/netI 0.0389
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_theta_min 1.75
_diffrn_reflns_theta_max 26.25
_reflns_number_total 7246
_reflns_number_gt 6004
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'XSCANS (Siemens, 1996)'
_computing_cell_refinement XSCANS
_computing_data_reduction XSCANS
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'MERCURY CSD 2.0 (Macrae et al., 2006)'
_computing_publication_material SHELXL97
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+6.9514P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7246
_refine_ls_number_parameters 517
_refine_ls_number_restraints 12
_refine_ls_number_constraints 0
_refine_ls_R_factor_all 0.0753
_refine_ls_R_factor_gt 0.0631
_refine_ls_wR_factor_ref 0.1812
_refine_ls_wR_factor_gt 0.1730
_refine_ls_goodness_of_fit_ref 1.119
_refine_ls_restrained_S_all 1.118
_refine_ls_shift/su_max 0.010
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.43130(7) 0.27126(5) 0.37936(4) 0.03086(17) Uani 1 1 d . . .
O1 O 0.5093(5) 0.3586(4) 0.4789(3) 0.0510(10) Uani 1 1 d D . .
H1B H 0.454(6) 0.401(6) 0.516(3) 0.076 Uiso 1 1 d D . .
H1C H 0.590(4) 0.335(6) 0.499(4) 0.076 Uiso 1 1 d D . .
O2 O 0.5255(5) 0.3656(3) 0.2984(3) 0.0478(10) Uani 1 1 d D . .
H2B H 0.591(5) 0.312(4) 0.275(4) 0.072 Uiso 1 1 d D . .
H2C H 0.570(6) 0.408(5) 0.319(4) 0.072 Uiso 1 1 d D . .
N1 N 0.7870(4) -0.0049(4) 0.4021(2) 0.0330(9) Uani 1 1 d . . .
H1A H 0.8765 -0.0408 0.4071 0.040 Uiso 1 1 calc R . .
C2 C 0.7438(5) 0.1028(4) 0.3733(3) 0.0339(10) Uani 1 1 d . . .
N3 N 0.5984(4) 0.1307(3) 0.3733(2) 0.0301(8) Uani 1 1 d . . .
C4 C 0.5511(5) 0.0357(4) 0.4022(3) 0.0266(9) Uani 1 1 d . . .
C5 C 0.6657(5) -0.0492(4) 0.4226(3) 0.0282(9) Uani 1 1 d . . .
C6 C 0.3886(5) 0.0485(4) 0.4071(3) 0.0290(9) Uani 1 1 d . . .
H6A H 0.3591 0.0464 0.3529 0.035 Uiso 1 1 calc R . .
H6B H 0.3605 -0.0128 0.4401 0.035 Uiso 1 1 calc R . .
N7 N 0.3182(4) 0.1619(3) 0.4453(2) 0.0281(8) Uani 1 1 d . . .
C8 C 0.1612(5) 0.2024(4) 0.4294(3) 0.0341(11) Uani 1 1 d . . .
H8A H 0.0983 0.1748 0.4722 0.041 Uiso 1 1 calc R . .
H8B H 0.1478 0.1734 0.3776 0.041 Uiso 1 1 calc R . .
C9 C 0.1212(6) 0.3332(5) 0.4273(3) 0.0396(12) Uani 1 1 d . . .
H9A H 0.0233 0.3618 0.4109 0.047 Uiso 1 1 calc R . .
H9B H 0.1215 0.3619 0.4813 0.047 Uiso 1 1 calc R . .
N10 N 0.2287(5) 0.3742(4) 0.3688(3) 0.0365(9) Uani 1 1 d . . .
C11 C 0.1993(8) 0.3620(6) 0.2835(4) 0.0575(16) Uani 1 1 d . . .
H11A H 0.1015 0.4054 0.2763 0.086 Uiso 1 1 calc R . .
H11B H 0.2086 0.2826 0.2730 0.086 Uiso 1 1 calc R . .
H11C H 0.2689 0.3902 0.2463 0.086 Uiso 1 1 calc R . .
C12 C 0.2144(8) 0.4987(5) 0.3845(5) 0.0598(17) Uani 1 1 d . . .
H12A H 0.1198 0.5430 0.3721 0.090 Uiso 1 1 calc R . .
H12B H 0.2901 0.5245 0.3504 0.090 Uiso 1 1 calc R . .
H12C H 0.2244 0.5082 0.4408 0.090 Uiso 1 1 calc R . .
C13 C 0.8449(6) 0.1772(5) 0.3460(4) 0.0479(14) Uani 1 1 d . . .
H13A H 0.7905 0.2476 0.3234 0.072 Uiso 1 1 calc R . .
H13B H 0.9199 0.1384 0.3052 0.072 Uiso 1 1 calc R . .
H13C H 0.8896 0.1937 0.3918 0.072 Uiso 1 1 calc R . .
C14 C 0.6647(6) -0.1609(4) 0.4652(3) 0.0318(10) Uani 1 1 d . . .
H14A H 0.7438 -0.2202 0.4387 0.038 Uiso 1 1 calc R . .
H14B H 0.5728 -0.1799 0.4590 0.038 Uiso 1 1 calc R . .
Cu2 Cu 0.87001(7) 0.75648(5) 0.13216(4) 0.03362(18) Uani 1 1 d . . .
O21 O 0.9887(6) 0.8571(4) 0.0388(3) 0.0590(11) Uani 1 1 d D . .
H21B H 0.937(7) 0.899(6) 0.005(3) 0.088 Uiso 1 1 d D . .
H21C H 1.068(5) 0.825(7) 0.010(4) 0.088 Uiso 1 1 d D . .
O22 O 0.9225(5) 0.8388(4) 0.2225(3) 0.0500(10) Uani 1 1 d D . .
H22B H 0.958(7) 0.797(5) 0.262(3) 0.075 Uiso 1 1 d D . .
H22C H 0.984(6) 0.879(5) 0.210(4) 0.075 Uiso 1 1 d D . .
N21 N 1.2450(5) 0.4892(4) 0.0971(2) 0.0333(9) Uani 1 1 d . . .
H21A H 1.3372 0.4554 0.0901 0.040 Uiso 1 1 calc R . .
C22 C 1.1879(5) 0.5935(4) 0.1299(3) 0.0315(10) Uani 1 1 d . . .
N23 N 1.0418(4) 0.6192(3) 0.1316(2) 0.0305(8) Uani 1 1 d . . .
C24 C 1.0086(5) 0.5259(4) 0.0999(3) 0.0275(9) Uani 1 1 d . . .
C25 C 1.1335(5) 0.4448(4) 0.0762(3) 0.0291(9) Uani 1 1 d . . .
C26 C 0.8494(5) 0.5366(4) 0.0940(3) 0.0286(9) Uani 1 1 d . . .
H26A H 0.7976 0.5281 0.1475 0.034 Uiso 1 1 calc R . .
H26B H 0.8371 0.4784 0.0584 0.034 Uiso 1 1 calc R . .
N27 N 0.7923(4) 0.6544(3) 0.0592(2) 0.0282(8) Uani 1 1 d . . .
C28 C 0.6289(5) 0.6934(5) 0.0747(3) 0.0379(11) Uani 1 1 d . . .
H28A H 0.5945 0.6635 0.1270 0.045 Uiso 1 1 calc R . .
H28B H 0.5840 0.6660 0.0323 0.045 Uiso 1 1 calc R . .
C29 C 0.5881(6) 0.8233(5) 0.0751(3) 0.0426(13) Uani 1 1 d . . .
H29A H 0.6161 0.8529 0.0215 0.051 Uiso 1 1 calc R . .
H29B H 0.4826 0.8516 0.0881 0.051 Uiso 1 1 calc R . .
N30 N 0.6659(5) 0.8629(4) 0.1373(3) 0.0408(10) Uani 1 1 d . . .
C31 C 0.5836(8) 0.8551(6) 0.2202(4) 0.0604(18) Uani 1 1 d . . .
H31A H 0.4835 0.8985 0.2201 0.091 Uiso 1 1 calc R . .
H31B H 0.6290 0.8855 0.2602 0.091 Uiso 1 1 calc R . .
H31C H 0.5857 0.7763 0.2334 0.091 Uiso 1 1 calc R . .
C32 C 0.6637(9) 0.9853(5) 0.1217(5) 0.0659(19) Uani 1 1 d . . .
H32A H 0.5637 1.0299 0.1238 0.099 Uiso 1 1 calc R . .
H32B H 0.7145 0.9939 0.0687 0.099 Uiso 1 1 calc R . .
H32C H 0.7116 1.0116 0.1625 0.099 Uiso 1 1 calc R . .
C33 C 1.2767(7) 0.6647(5) 0.1615(4) 0.0469(13) Uani 1 1 d . . .
H33A H 1.2125 0.7268 0.1926 0.070 Uiso 1 1 calc R . .
H33B H 1.3304 0.6951 0.1164 0.070 Uiso 1 1 calc R . .
H33C H 1.3443 0.6183 0.1958 0.070 Uiso 1 1 calc R . .
C34 C 1.1526(6) 0.3372(4) 0.0299(3) 0.0320(10) Uani 1 1 d . . .
H34A H 1.0589 0.3170 0.0342 0.038 Uiso 1 1 calc R . .
H34B H 1.2212 0.2757 0.0551 0.038 Uiso 1 1 calc R . .
B1 B 1.1459(11) 1.0576(8) 0.1633(5) 0.066(2) Uani 1 1 d . . .
F1 F 1.2130(10) 1.0987(7) 0.2161(5) 0.150(3) Uani 1 1 d . . .
F2 F 1.2243(10) 1.0403(8) 0.0903(4) 0.173(4) Uani 1 1 d . . .
F3 F 1.1113(13) 0.9670(8) 0.1983(7) 0.213(5) Uani 1 1 d . . .
F4 F 1.0222(10) 1.1336(10) 0.1488(5) 0.196(5) Uani 1 1 d . . .
B2 B 0.2488(8) 0.4447(6) 0.6669(4) 0.0474(15) Uani 1 1 d . . .
F5 F 0.3942(6) 0.4263(5) 0.6758(5) 0.135(3) Uani 1 1 d . . .
F6 F 0.2322(9) 0.4494(6) 0.5876(3) 0.129(2) Uani 1 1 d . . .
F7 F 0.1785(6) 0.5462(4) 0.7023(3) 0.0905(15) Uani 1 1 d . . .
F8 F 0.1959(6) 0.3579(4) 0.7059(4) 0.0972(17) Uani 1 1 d . . .
B3 B 0.6241(7) 0.3026(6) 0.0944(4) 0.0457(15) Uani 1 1 d . . .
F9 F 0.7140(8) 0.2568(6) 0.0284(3) 0.139(3) Uani 1 1 d . . .
F10 F 0.6941(5) 0.2809(5) 0.1646(3) 0.0910(16) Uani 1 1 d . . .
F11 F 0.4970(6) 0.2627(4) 0.1051(4) 0.0962(16) Uani 1 1 d . . .
F12 F 0.5696(5) 0.4195(4) 0.0803(4) 0.0845(15) Uani 1 1 d . . .
B4 B 0.8321(7) 0.1881(6) 0.5998(4) 0.0434(14) Uani 1 1 d . . .
F13 F 0.7157(6) 0.1888(5) 0.6546(4) 0.113(2) Uani 1 1 d . . .
F14 F 0.7909(6) 0.2591(4) 0.5339(3) 0.0910(16) Uani 1 1 d . . .
F15 F 0.9372(6) 0.2275(4) 0.6327(3) 0.0802(13) Uani 1 1 d . . .
F16 F 0.8991(4) 0.0780(3) 0.5719(3) 0.0715(12) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0326(3) 0.0287(3) 0.0306(3) 0.0023(2) -0.0028(2) -0.0071(2)
O1 0.054(3) 0.055(3) 0.044(2) -0.0109(19) -0.0074(19) -0.013(2)
O2 0.055(2) 0.042(2) 0.047(2) 0.0064(17) 0.0041(19) -0.0190(19)
N1 0.0242(19) 0.039(2) 0.032(2) 0.0021(17) -0.0022(16) -0.0027(17)
C2 0.032(2) 0.039(3) 0.030(2) 0.000(2) -0.0013(19) -0.008(2)
N3 0.027(2) 0.029(2) 0.033(2) 0.0005(16) -0.0026(16) -0.0054(16)
C4 0.028(2) 0.028(2) 0.023(2) -0.0056(17) -0.0012(17) -0.0061(18)
C5 0.030(2) 0.031(2) 0.022(2) -0.0048(17) 0.0012(17) -0.0067(19)
C6 0.029(2) 0.031(2) 0.028(2) -0.0019(18) -0.0064(18) -0.0066(19)
N7 0.0263(19) 0.0280(19) 0.030(2) 0.0027(15) -0.0062(15) -0.0053(15)
C8 0.023(2) 0.039(3) 0.037(3) 0.007(2) -0.0031(19) -0.005(2)
C9 0.032(3) 0.041(3) 0.041(3) 0.002(2) -0.004(2) 0.001(2)
N10 0.039(2) 0.031(2) 0.038(2) 0.0053(17) -0.0054(18) -0.0062(18)
C11 0.061(4) 0.073(4) 0.038(3) 0.009(3) -0.018(3) -0.012(3)
C12 0.062(4) 0.029(3) 0.081(5) 0.004(3) -0.001(3) -0.003(3)
C13 0.033(3) 0.063(4) 0.054(3) 0.018(3) -0.010(2) -0.024(3)
C14 0.037(3) 0.029(2) 0.027(2) -0.0041(18) -0.0026(19) -0.0039(19)
Cu2 0.0377(3) 0.0315(3) 0.0314(3) -0.0069(2) -0.0044(2) -0.0068(3)
O21 0.065(3) 0.056(3) 0.055(3) 0.008(2) 0.000(2) -0.018(2)
O22 0.065(3) 0.044(2) 0.044(2) -0.0086(17) -0.019(2) -0.014(2)
N21 0.030(2) 0.041(2) 0.027(2) -0.0009(17) -0.0064(16) -0.0037(17)
C22 0.035(3) 0.040(3) 0.022(2) 0.0009(18) -0.0032(18) -0.013(2)
N23 0.035(2) 0.034(2) 0.0230(19) -0.0038(15) -0.0019(16) -0.0091(17)
C24 0.033(2) 0.032(2) 0.018(2) 0.0008(17) 0.0002(17) -0.0106(19)
C25 0.033(2) 0.033(2) 0.021(2) -0.0009(17) -0.0031(18) -0.0073(19)
C26 0.031(2) 0.030(2) 0.026(2) -0.0011(17) -0.0016(18) -0.0095(19)
N27 0.028(2) 0.031(2) 0.0257(19) -0.0049(15) -0.0027(15) -0.0057(16)
C28 0.029(3) 0.048(3) 0.036(3) -0.012(2) -0.002(2) -0.007(2)
C29 0.038(3) 0.045(3) 0.038(3) -0.008(2) -0.006(2) 0.007(2)
N30 0.045(3) 0.037(2) 0.038(2) -0.0061(18) -0.005(2) -0.0023(19)
C31 0.061(4) 0.076(4) 0.034(3) -0.018(3) 0.006(3) 0.001(3)
C32 0.075(5) 0.038(3) 0.083(5) -0.006(3) -0.022(4) -0.004(3)
C33 0.047(3) 0.060(4) 0.040(3) -0.007(3) -0.004(2) -0.025(3)
C34 0.039(3) 0.029(2) 0.026(2) 0.0004(18) -0.0039(19) -0.007(2)
B1 0.085(6) 0.070(5) 0.047(4) 0.004(4) -0.009(4) -0.029(5)
F1 0.189(8) 0.153(6) 0.144(6) -0.040(5) -0.047(6) -0.089(6)
F2 0.194(8) 0.201(8) 0.078(4) -0.019(5) 0.035(5) 0.017(7)
F3 0.324(14) 0.172(8) 0.229(10) 0.090(7) -0.140(10) -0.188(9)
F4 0.143(7) 0.254(11) 0.130(6) 0.065(7) 0.003(5) 0.046(7)
B2 0.051(4) 0.046(4) 0.044(4) -0.001(3) -0.001(3) -0.011(3)
F5 0.064(3) 0.095(4) 0.245(9) 0.043(5) -0.031(4) -0.021(3)
F6 0.205(7) 0.131(5) 0.047(3) -0.012(3) -0.016(4) -0.028(5)
F7 0.117(4) 0.058(3) 0.089(3) -0.020(2) -0.006(3) -0.007(3)
F8 0.100(4) 0.073(3) 0.120(4) 0.014(3) 0.015(3) -0.041(3)
B3 0.042(3) 0.053(4) 0.040(3) 0.002(3) -0.007(3) -0.007(3)
F9 0.138(5) 0.173(6) 0.044(3) -0.004(3) 0.010(3) 0.068(5)
F10 0.072(3) 0.128(4) 0.059(3) -0.013(3) -0.022(2) 0.010(3)
F11 0.090(4) 0.082(3) 0.131(5) 0.023(3) -0.041(3) -0.039(3)
F12 0.061(3) 0.057(2) 0.134(4) 0.024(3) -0.024(3) -0.011(2)
B4 0.036(3) 0.047(3) 0.046(3) -0.006(3) -0.011(3) -0.003(3)
F13 0.087(4) 0.129(5) 0.111(4) -0.026(4) 0.050(3) -0.027(3)
F14 0.103(4) 0.093(3) 0.067(3) 0.008(2) -0.040(3) 0.006(3)
F15 0.094(3) 0.063(3) 0.095(3) 0.004(2) -0.049(3) -0.024(2)
F16 0.055(2) 0.053(2) 0.102(3) -0.025(2) -0.011(2) -0.0005(18)
_geom_special_details ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.988(4) . ?
Cu1 N3 2.002(4) . ?
Cu1 N10 2.026(4) . ?
Cu1 N7 2.088(4) . ?
Cu1 O1 2.276(4) . ?
O1 H1B 0.848(10) . ?
O1 H1C 0.848(10) . ?
O2 H2B 0.846(10) . ?
O2 H2C 0.845(10) . ?
N1 C2 1.343(6) . ?
N1 C5 1.383(6) . ?
N1 H1A 0.8600 . ?
C2 N3 1.330(6) . ?
C2 C13 1.487(7) . ?
N3 C4 1.376(6) . ?
C4 C5 1.355(7) . ?
C4 C6 1.498(6) . ?
C5 C14 1.492(7) . ?
C6 N7 1.491(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
N7 C8 1.493(6) . ?
N7 C14 1.504(6) 2_656 ?
C8 C9 1.525(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N10 1.476(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N10 C11 1.486(7) . ?
N10 C12 1.503(7) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 N7 1.504(6) 2_656 ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
Cu2 O22 2.001(4) . ?
Cu2 N23 2.006(4) . ?
Cu2 N30 2.026(5) . ?
Cu2 N27 2.073(4) . ?
Cu2 O21 2.280(5) . ?
O21 H21B 0.847(10) . ?
O21 H21C 0.848(10) . ?
O22 H22B 0.848(10) . ?
O22 H22C 0.849(10) . ?
N21 C22 1.346(6) . ?
N21 C25 1.380(6) . ?
N21 H21A 0.8600 . ?
C22 N23 1.335(6) . ?
C22 C33 1.490(7) . ?
N23 C24 1.379(6) . ?
C24 C25 1.358(7) . ?
C24 C26 1.494(7) . ?
C25 C34 1.495(6) . ?
C26 N27 1.501(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
N27 C28 1.491(6) . ?
N27 C34 1.505(6) 2_765 ?
C28 C29 1.515(8) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 N30 1.492(7) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
N30 C32 1.481(8) . ?
N30 C31 1.500(8) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 N27 1.505(6) 2_765 ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
B1 F3 1.308(11) . ?
B1 F1 1.317(11) . ?
B1 F2 1.331(11) . ?
B1 F4 1.332(12) . ?
B2 F6 1.332(9) . ?
B2 F7 1.356(8) . ?
B2 F5 1.362(9) . ?
B2 F8 1.373(8) . ?
B3 F9 1.344(8) . ?
B3 F10 1.386(8) . ?
B3 F12 1.392(8) . ?
B3 F11 1.392(9) . ?
B4 F13 1.335(8) . ?
B4 F15 1.378(8) . ?
B4 F14 1.384(8) . ?
B4 F16 1.390(7) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 N3 96.96(17) . . ?
O2 Cu1 N10 91.79(17) . . ?
N3 Cu1 N10 159.74(18) . . ?
O2 Cu1 N7 169.21(17) . . ?
N3 Cu1 N7 83.01(15) . . ?
N10 Cu1 N7 85.02(16) . . ?
O2 Cu1 O1 87.65(18) . . ?
N3 Cu1 O1 96.27(17) . . ?
N10 Cu1 O1 102.33(17) . . ?
N7 Cu1 O1 103.09(16) . . ?
Cu1 O1 H1B 125(5) . . ?
Cu1 O1 H1C 126(5) . . ?
H1B O1 H1C 104(2) . . ?
Cu1 O2 H2B 99(5) . . ?
Cu1 O2 H2C 115(5) . . ?
H2B O2 H2C 106(3) . . ?
C2 N1 C5 109.6(4) . . ?
C2 N1 H1A 125.2 . . ?
C5 N1 H1A 125.2 . . ?
N3 C2 N1 109.2(4) . . ?
N3 C2 C13 126.4(5) . . ?
N1 C2 C13 124.4(5) . . ?
C2 N3 C4 106.4(4) . . ?
C2 N3 Cu1 139.0(4) . . ?
C4 N3 Cu1 110.9(3) . . ?
C5 C4 N3 110.5(4) . . ?
C5 C4 C6 134.2(4) . . ?
N3 C4 C6 115.2(4) . . ?
C4 C5 N1 104.2(4) . . ?
C4 C5 C14 129.2(4) . . ?
N1 C5 C14 126.3(4) . . ?
N7 C6 C4 106.1(4) . . ?
N7 C6 H6A 110.5 . . ?
C4 C6 H6A 110.5 . . ?
N7 C6 H6B 110.5 . . ?
C4 C6 H6B 110.5 . . ?
H6A C6 H6B 108.7 . . ?
C6 N7 C8 111.2(4) . . ?
C6 N7 C14 112.2(3) . 2_656 ?
C8 N7 C14 112.1(4) . 2_656 ?
C6 N7 Cu1 102.8(3) . . ?
C8 N7 Cu1 106.7(3) . . ?
C14 N7 Cu1 111.3(3) 2_656 . ?
N7 C8 C9 108.0(4) . . ?
N7 C8 H8A 110.1 . . ?
C9 C8 H8A 110.1 . . ?
N7 C8 H8B 110.1 . . ?
C9 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
N10 C9 C8 109.6(4) . . ?
N10 C9 H9A 109.8 . . ?
C8 C9 H9A 109.8 . . ?
N10 C9 H9B 109.8 . . ?
C8 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
C9 N10 C11 110.4(5) . . ?
C9 N10 C12 108.6(4) . . ?
C11 N10 C12 109.0(5) . . ?
C9 N10 Cu1 108.4(3) . . ?
C11 N10 Cu1 106.1(4) . . ?
C12 N10 Cu1 114.3(4) . . ?
N10 C11 H11A 109.5 . . ?
N10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N10 C12 H12A 109.5 . . ?
N10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C2 C13 H13A 109.5 . . ?
C2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C5 C14 N7 114.2(4) . 2_656 ?
C5 C14 H14A 108.7 . . ?
N7 C14 H14A 108.7 2_656 . ?
C5 C14 H14B 108.7 . . ?
N7 C14 H14B 108.7 2_656 . ?
H14A C14 H14B 107.6 . . ?
O22 Cu2 N23 96.65(17) . . ?
O22 Cu2 N30 91.92(18) . . ?
N23 Cu2 N30 164.77(18) . . ?
O22 Cu2 N27 167.50(18) . . ?
N23 Cu2 N27 82.99(16) . . ?
N30 Cu2 N27 85.92(17) . . ?
O22 Cu2 O21 89.82(19) . . ?
N23 Cu2 O21 94.13(17) . . ?
N30 Cu2 O21 98.47(19) . . ?
N27 Cu2 O21 102.67(17) . . ?
Cu2 O21 H21B 116(6) . . ?
Cu2 O21 H21C 122(6) . . ?
H21B O21 H21C 105(3) . . ?
Cu2 O22 H22B 116(5) . . ?
Cu2 O22 H22C 117(5) . . ?
H22B O22 H22C 103(2) . . ?
C22 N21 C25 109.7(4) . . ?
C22 N21 H21A 125.1 . . ?
C25 N21 H21A 125.1 . . ?
N23 C22 N21 109.2(4) . . ?
N23 C22 C33 126.7(5) . . ?
N21 C22 C33 124.1(5) . . ?
C22 N23 C24 106.2(4) . . ?
C22 N23 Cu2 140.0(3) . . ?
C24 N23 Cu2 110.3(3) . . ?
C25 C24 N23 110.5(4) . . ?
C25 C24 C26 133.6(4) . . ?
N23 C24 C26 115.7(4) . . ?
C24 C25 N21 104.3(4) . . ?
C24 C25 C34 129.4(4) . . ?
N21 C25 C34 126.0(4) . . ?
C24 C26 N27 105.5(4) . . ?
C24 C26 H26A 110.6 . . ?
N27 C26 H26A 110.6 . . ?
C24 C26 H26B 110.6 . . ?
N27 C26 H26B 110.6 . . ?
H26A C26 H26B 108.8 . . ?
C28 N27 C26 111.9(4) . . ?
C28 N27 C34 112.3(4) . 2_765 ?
C26 N27 C34 111.9(3) . 2_765 ?
C28 N27 Cu2 105.0(3) . . ?
C26 N27 Cu2 102.4(3) . . ?
C34 N27 Cu2 112.8(3) 2_765 . ?
N27 C28 C29 107.7(4) . . ?
N27 C28 H28A 110.2 . . ?
C29 C28 H28A 110.2 . . ?
N27 C28 H28B 110.2 . . ?
C29 C28 H28B 110.2 . . ?
H28A C28 H28B 108.5 . . ?
N30 C29 C28 109.0(4) . . ?
N30 C29 H29A 109.9 . . ?
C28 C29 H29A 109.9 . . ?
N30 C29 H29B 109.9 . . ?
C28 C29 H29B 109.9 . . ?
H29A C29 H29B 108.3 . . ?
C32 N30 C29 109.3(5) . . ?
C32 N30 C31 107.0(5) . . ?
C29 N30 C31 108.9(5) . . ?
C32 N30 Cu2 114.4(4) . . ?
C29 N30 Cu2 107.1(3) . . ?
C31 N30 Cu2 110.1(4) . . ?
N30 C31 H31A 109.5 . . ?
N30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N30 C32 H32A 109.5 . . ?
N30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C22 C33 H33A 109.5 . . ?
C22 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C22 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C25 C34 N27 114.2(4) . 2_765 ?
C25 C34 H34A 108.7 . . ?
N27 C34 H34A 108.7 2_765 . ?
C25 C34 H34B 108.7 . . ?
N27 C34 H34B 108.7 2_765 . ?
H34A C34 H34B 107.6 . . ?
F3 B1 F1 106.2(8) . . ?
F3 B1 F2 115.3(10) . . ?
F1 B1 F2 112.5(10) . . ?
F3 B1 F4 108.2(10) . . ?
F1 B1 F4 110.3(10) . . ?
F2 B1 F4 104.3(8) . . ?
F6 B2 F7 110.2(6) . . ?
F6 B2 F5 109.3(7) . . ?
F7 B2 F5 107.5(7) . . ?
F6 B2 F8 111.1(7) . . ?
F7 B2 F8 109.7(6) . . ?
F5 B2 F8 109.0(6) . . ?
F9 B3 F10 111.5(6) . . ?
F9 B3 F12 109.0(6) . . ?
F10 B3 F12 112.2(6) . . ?
F9 B3 F11 111.6(7) . . ?
F10 B3 F11 109.6(6) . . ?
F12 B3 F11 102.6(5) . . ?
F13 B4 F15 111.4(6) . . ?
F13 B4 F14 110.5(6) . . ?
F15 B4 F14 107.1(6) . . ?
F13 B4 F16 111.5(6) . . ?
F15 B4 F16 107.0(5) . . ?
F14 B4 F16 109.1(5) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C2 N3 -0.5(6) . . . . ?
C5 N1 C2 C13 179.4(5) . . . . ?
N1 C2 N3 C4 -0.9(5) . . . . ?
C13 C2 N3 C4 179.1(5) . . . . ?
N1 C2 N3 Cu1 153.9(4) . . . . ?
C13 C2 N3 Cu1 -26.1(9) . . . . ?
O2 Cu1 N3 C2 45.8(5) . . . . ?
N10 Cu1 N3 C2 160.8(5) . . . . ?
N7 Cu1 N3 C2 -145.0(5) . . . . ?
O1 Cu1 N3 C2 -42.6(5) . . . . ?
O2 Cu1 N3 C4 -160.1(3) . . . . ?
N10 Cu1 N3 C4 -45.2(6) . . . . ?
N7 Cu1 N3 C4 9.0(3) . . . . ?
O1 Cu1 N3 C4 111.5(3) . . . . ?
C2 N3 C4 C5 2.1(5) . . . . ?
Cu1 N3 C4 C5 -160.5(3) . . . . ?
C2 N3 C4 C6 -179.7(4) . . . . ?
Cu1 N3 C4 C6 17.7(5) . . . . ?
N3 C4 C5 N1 -2.3(5) . . . . ?
C6 C4 C5 N1 180.0(5) . . . . ?
N3 C4 C5 C14 171.9(4) . . . . ?
C6 C4 C5 C14 -5.8(9) . . . . ?
C2 N1 C5 C4 1.7(5) . . . . ?
C2 N1 C5 C14 -172.7(4) . . . . ?
C5 C4 C6 N7 131.8(5) . . . . ?
N3 C4 C6 N7 -45.8(5) . . . . ?
C4 C6 N7 C8 161.5(4) . . . . ?
C4 C6 N7 C14 -72.0(5) . . . 2_656 ?
C4 C6 N7 Cu1 47.7(4) . . . . ?
O2 Cu1 N7 C6 58.3(9) . . . . ?
N3 Cu1 N7 C6 -32.1(3) . . . . ?
N10 Cu1 N7 C6 131.5(3) . . . . ?
O1 Cu1 N7 C6 -127.0(3) . . . . ?
O2 Cu1 N7 C8 -58.8(10) . . . . ?
N3 Cu1 N7 C8 -149.2(3) . . . . ?
N10 Cu1 N7 C8 14.4(3) . . . . ?
O1 Cu1 N7 C8 115.9(3) . . . . ?
O2 Cu1 N7 C14 178.6(8) . . . 2_656 ?
N3 Cu1 N7 C14 88.1(3) . . . 2_656 ?
N10 Cu1 N7 C14 -108.3(3) . . . 2_656 ?
O1 Cu1 N7 C14 -6.7(3) . . . 2_656 ?
C6 N7 C8 C9 -150.2(4) . . . . ?
C14 N7 C8 C9 83.3(5) 2_656 . . . ?
Cu1 N7 C8 C9 -38.8(4) . . . . ?
N7 C8 C9 N10 53.0(5) . . . . ?
C8 C9 N10 C11 76.4(5) . . . . ?
C8 C9 N10 C12 -164.1(5) . . . . ?
C8 C9 N10 Cu1 -39.4(5) . . . . ?
O2 Cu1 N10 C9 -176.6(3) . . . . ?
N3 Cu1 N10 C9 67.6(6) . . . . ?
N7 Cu1 N10 C9 13.7(3) . . . . ?
O1 Cu1 N10 C9 -88.6(3) . . . . ?
O2 Cu1 N10 C11 64.8(4) . . . . ?
N3 Cu1 N10 C11 -51.0(7) . . . . ?
N7 Cu1 N10 C11 -104.9(4) . . . . ?
O1 Cu1 N10 C11 152.8(4) . . . . ?
O2 Cu1 N10 C12 -55.3(4) . . . . ?
N3 Cu1 N10 C12 -171.1(5) . . . . ?
N7 Cu1 N10 C12 135.0(4) . . . . ?
O1 Cu1 N10 C12 32.7(4) . . . . ?
C4 C5 C14 N7 -99.7(6) . . . 2_656 ?
N1 C5 C14 N7 73.4(6) . . . 2_656 ?
C25 N21 C22 N23 0.1(5) . . . . ?
C25 N21 C22 C33 178.2(5) . . . . ?
N21 C22 N23 C24 1.2(5) . . . . ?
C33 C22 N23 C24 -176.8(5) . . . . ?
N21 C22 N23 Cu2 -154.4(4) . . . . ?
C33 C22 N23 Cu2 27.6(8) . . . . ?
O22 Cu2 N23 C22 -49.5(5) . . . . ?
N30 Cu2 N23 C22 -173.4(6) . . . . ?
N27 Cu2 N23 C22 143.0(5) . . . . ?
O21 Cu2 N23 C22 40.8(5) . . . . ?
O22 Cu2 N23 C24 155.5(3) . . . . ?
N30 Cu2 N23 C24 31.6(8) . . . . ?
N27 Cu2 N23 C24 -11.9(3) . . . . ?
O21 Cu2 N23 C24 -114.2(3) . . . . ?
C22 N23 C24 C25 -2.1(5) . . . . ?
Cu2 N23 C24 C25 161.4(3) . . . . ?
C22 N23 C24 C26 -178.7(4) . . . . ?
Cu2 N23 C24 C26 -15.1(5) . . . . ?
N23 C24 C25 N21 2.1(5) . . . . ?
C26 C24 C25 N21 177.8(5) . . . . ?
N23 C24 C25 C34 -171.7(4) . . . . ?
C26 C24 C25 C34 4.0(9) . . . . ?
C22 N21 C25 C24 -1.4(5) . . . . ?
C22 N21 C25 C34 172.7(4) . . . . ?
C25 C24 C26 N27 -130.6(5) . . . . ?
N23 C24 C26 N27 44.9(5) . . . . ?
C24 C26 N27 C28 -161.0(4) . . . . ?
C24 C26 N27 C34 72.0(4) . . . 2_765 ?
C24 C26 N27 Cu2 -49.0(4) . . . . ?
O22 Cu2 N27 C28 62.3(9) . . . . ?
N23 Cu2 N27 C28 151.4(3) . . . . ?
N30 Cu2 N27 C28 -18.1(3) . . . . ?
O21 Cu2 N27 C28 -115.9(3) . . . . ?
O22 Cu2 N27 C26 -54.7(9) . . . . ?
N23 Cu2 N27 C26 34.4(3) . . . . ?
N30 Cu2 N27 C26 -135.1(3) . . . . ?
O21 Cu2 N27 C26 127.1(3) . . . . ?
O22 Cu2 N27 C34 -175.1(7) . . . 2_765 ?
N23 Cu2 N27 C34 -86.0(3) . . . 2_765 ?
N30 Cu2 N27 C34 104.5(3) . . . 2_765 ?
O21 Cu2 N27 C34 6.7(3) . . . 2_765 ?
C26 N27 C28 C29 153.9(4) . . . . ?
C34 N27 C28 C29 -79.3(5) 2_765 . . . ?
Cu2 N27 C28 C29 43.6(4) . . . . ?
N27 C28 C29 N30 -56.4(5) . . . . ?
C28 C29 N30 C32 163.1(5) . . . . ?
C28 C29 N30 C31 -80.3(5) . . . . ?
C28 C29 N30 Cu2 38.7(5) . . . . ?
O22 Cu2 N30 C32 59.9(4) . . . . ?
N23 Cu2 N30 C32 -175.8(6) . . . . ?
N27 Cu2 N30 C32 -132.5(4) . . . . ?
O21 Cu2 N30 C32 -30.2(5) . . . . ?
O22 Cu2 N30 C29 -178.8(4) . . . . ?
N23 Cu2 N30 C29 -54.5(8) . . . . ?
N27 Cu2 N30 C29 -11.2(4) . . . . ?
O21 Cu2 N30 C29 91.1(4) . . . . ?
O22 Cu2 N30 C31 -60.6(4) . . . . ?
N23 Cu2 N30 C31 63.7(8) . . . . ?
N27 Cu2 N30 C31 107.0(4) . . . . ?
O21 Cu2 N30 C31 -150.7(4) . . . . ?
C24 C25 C34 N27 101.6(6) . . . 2_765 ?
N21 C25 C34 N27 -71.0(6) . . . 2_765 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A F16 0.86 2.12 2.955(6) 162.3 2_756 .
N21 H21A F12 0.86 2.12 2.954(6) 163.6 1_655 .
N1 H1A F15 0.86 2.54 3.253(6) 140.9 2_756 .
N21 H21A F11 0.86 2.45 3.149(7) 138.7 1_655 .
O1 H1B F6 0.848(10) 2.23(4) 2.979(9) 147(7) . .
O1 H1C F14 0.848(10) 2.030(15) 2.870(7) 171(6) . .
O2 H2B F10 0.846(10) 1.96(5) 2.643(6) 137(7) . .
O2 H2C F5 0.845(10) 2.11(4) 2.858(8) 148(7) 2_666 .
O2 H2C F7 0.845(10) 2.55(4) 3.232(7) 139(5) 2_666 .
O21 H21B F2 0.847(10) 2.29(3) 3.109(10) 162(8) 2_775 .
O21 H21B F4 0.847(10) 2.55(6) 3.104(10) 124(6) 2_775 .
O21 H21C F9 0.848(10) 2.08(2) 2.908(8) 164(7) 2_765 .
O22 H22B F15 0.848(10) 2.08(4) 2.857(6) 152(7) 2_766 .
O22 H22C F3 0.849(10) 1.782(18) 2.624(9) 172(7) . .
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 26.25
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 0.865
_refine_diff_density_min -0.519
_refine_diff_density_rms 0.102
#===========================================================================
# 6. SHELX CODE
#===========================================================================
_iucr_refine_instructions_details
;
TITL cudbo in P-1 LAST...
CELL 0.71073 9.4555 12.0445 16.4925 87.469 83.061 75.465
ZERR 2.00 0.0020 0.0017 0.0024 0.010 0.014 0.014
LATT 1
SFAC C H B N O F CU
UNIT 40 88 8 16 8 32 4
TEMP 23
L.S. 24
ACTA
OMIT 2 1 0
OMIT 7 3 1
OMIT 2 3 8
OMIT 3 -6 4
OMIT 3 -4 7
OMIT -2 -2 7
OMIT 2 4 2
OMIT 5 0 7
OMIT 3 -5 10
OMIT 2 5 3
OMIT -2 0 6
OMIT -2 -4 7
OMIT 7 1 9
BOND $H
CONF
WPDB -2
FMAP 2
PLAN 10
EQIV $1 -x+1, -y+1, -z+1
EQIV $2 -x+2, -y, -z+1
EQIV $3 -x+2, -y+2, -z
EQIV $4 -x+2, -y+1, -z
EQIV $5 -x+2, -y+1, -z+1
EQIV $6 x+1, y, z
HTAB O1 F6
HTAB O1 F14
HTAB O2 F10
HTAB O2 F5_$1
HTAB O2 F7_$1
HTAB N1 F16_$2
HTAB N1 F15_$2
HTAB O21 F2_$3
HTAB O21 F4_$3
HTAB O21 F9_$4
HTAB O22 F15_$5
HTAB O22 F3
HTAB N21 F12_$6
HTAB N21 F11_$6
DFIX 0.85 0.01 O1 H1B
DFIX 0.85 0.01 O1 H1C
DFIX 1.34 0.02 H1B H1C
DFIX 0.85 0.01 O2 H2B
DFIX 0.85 0.01 O2 H2C
DFIX 1.34 0.02 H2B H2C
DFIX 0.85 0.01 O21 H21B
DFIX 0.85 0.01 O21 H21C
DFIX 1.34 0.02 H21B H21C
DFIX 0.85 0.01 O22 H22B
DFIX 0.85 0.01 O22 H22C
DFIX 1.34 0.02 H22B H22C
WGHT 0.067300 6.951400
FVAR 0.38290
CU1 7 0.431296 0.271256 0.379361 11.00000 0.03262 0.02869 =
0.03056 0.00232 -0.00283 -0.00707
O1 5 0.509273 0.358597 0.478911 11.00000 0.05449 0.05506 =
0.04446 -0.01091 -0.00743 -0.01300
H1B 2 0.453596 0.400772 0.515709 11.00000 -1.50000
H1C 2 0.589959 0.335280 0.499273 11.00000 -1.50000
O2 5 0.525519 0.365614 0.298445 11.00000 0.05481 0.04242 =
0.04678 0.00636 0.00412 -0.01899
H2B 2 0.591040 0.312093 0.274788 11.00000 -1.50000
H2C 2 0.570466 0.408368 0.318542 11.00000 -1.50000
N1 4 0.787039 -0.004901 0.402100 11.00000 0.02419 0.03943 =
0.03195 0.00215 -0.00219 -0.00272
AFIX 43
H1A 2 0.876510 -0.040825 0.407082 11.00000 -1.20000
AFIX 0
C2 1 0.743760 0.102798 0.373252 11.00000 0.03158 0.03914 =
0.03021 -0.00018 -0.00132 -0.00834
N3 4 0.598430 0.130695 0.373344 11.00000 0.02720 0.02944 =
0.03254 0.00049 -0.00258 -0.00545
C4 1 0.551080 0.035710 0.402245 11.00000 0.02849 0.02754 =
0.02345 -0.00557 -0.00119 -0.00614
C5 1 0.665736 -0.049233 0.422581 11.00000 0.03036 0.03139 =
0.02161 -0.00479 0.00120 -0.00673
C6 1 0.388613 0.048538 0.407059 11.00000 0.02884 0.03062 =
0.02815 -0.00194 -0.00642 -0.00659
AFIX 23
H6A 2 0.359135 0.046412 0.352934 11.00000 -1.20000
H6B 2 0.360506 -0.012762 0.440114 11.00000 -1.20000
AFIX 0
N7 4 0.318182 0.161890 0.445264 11.00000 0.02629 0.02796 =
0.02964 0.00273 -0.00621 -0.00528
C8 1 0.161181 0.202418 0.429398 11.00000 0.02345 0.03941 =
0.03678 0.00708 -0.00309 -0.00457
AFIX 23
H8A 2 0.098296 0.174779 0.472250 11.00000 -1.20000
H8B 2 0.147843 0.173449 0.377634 11.00000 -1.20000
AFIX 0
C9 1 0.121217 0.333228 0.427268 11.00000 0.03155 0.04097 =
0.04081 0.00207 -0.00413 0.00053
AFIX 23
H9A 2 0.023266 0.361822 0.410939 11.00000 -1.20000
H9B 2 0.121545 0.361858 0.481284 11.00000 -1.20000
AFIX 0
N10 4 0.228708 0.374170 0.368774 11.00000 0.03870 0.03133 =
0.03776 0.00535 -0.00535 -0.00621
C11 1 0.199323 0.362025 0.283546 11.00000 0.06104 0.07270 =
0.03823 0.00903 -0.01767 -0.01174
AFIX 137
H11A 2 0.101478 0.405387 0.276310 11.00000 -1.50000
H11B 2 0.208623 0.282622 0.272974 11.00000 -1.50000
H11C 2 0.268882 0.390219 0.246283 11.00000 -1.50000
AFIX 0
C12 1 0.214438 0.498728 0.384454 11.00000 0.06233 0.02936 =
0.08096 0.00404 -0.00073 -0.00337
AFIX 137
H12A 2 0.119787 0.543001 0.372115 11.00000 -1.50000
H12B 2 0.290063 0.524518 0.350445 11.00000 -1.50000
H12C 2 0.224351 0.508206 0.440813 11.00000 -1.50000
AFIX 0
C13 1 0.844909 0.177184 0.346011 11.00000 0.03349 0.06286 =
0.05353 0.01756 -0.01032 -0.02385
AFIX 137
H13A 2 0.790476 0.247578 0.323449 11.00000 -1.50000
H13B 2 0.919941 0.138355 0.305168 11.00000 -1.50000
H13C 2 0.889630 0.193655 0.391824 11.00000 -1.50000
AFIX 0
C14 1 0.664684 -0.160930 0.465175 11.00000 0.03651 0.02924 =
0.02738 -0.00414 -0.00256 -0.00395
AFIX 23
H14A 2 0.743806 -0.220239 0.438708 11.00000 -1.20000
H14B 2 0.572807 -0.179931 0.458971 11.00000 -1.20000
AFIX 0
CU2 7 0.870008 0.756485 0.132156 11.00000 0.03768 0.03151 =
0.03142 -0.00687 -0.00437 -0.00683
O21 5 0.988668 0.857067 0.038756 11.00000 0.06466 0.05621 =
0.05503 0.00763 -0.00002 -0.01762
H21B 2 0.936964 0.898885 0.005125 11.00000 -1.50000
H21C 2 1.068210 0.825220 0.010221 11.00000 -1.50000
O22 5 0.922521 0.838763 0.222515 11.00000 0.06536 0.04435 =
0.04439 -0.00860 -0.01889 -0.01364
H22B 2 0.957873 0.797071 0.261655 11.00000 -1.50000
H22C 2 0.983599 0.879326 0.209586 11.00000 -1.50000
N21 4 1.245038 0.489232 0.097063 11.00000 0.02953 0.04123 =
0.02727 -0.00087 -0.00637 -0.00367
AFIX 43
H21A 2 1.337151 0.455415 0.090087 11.00000 -1.20000
AFIX 0
C22 1 1.187907 0.593456 0.129936 11.00000 0.03489 0.03986 =
0.02184 0.00088 -0.00319 -0.01323
N23 4 1.041828 0.619181 0.131599 11.00000 0.03450 0.03431 =
0.02298 -0.00378 -0.00193 -0.00906
C24 1 1.008631 0.525888 0.099936 11.00000 0.03321 0.03155 =
0.01828 0.00077 0.00017 -0.01065
C25 1 1.133485 0.444828 0.076242 11.00000 0.03289 0.03257 =
0.02139 -0.00092 -0.00306 -0.00734
C26 1 0.849363 0.536557 0.093991 11.00000 0.03058 0.02958 =
0.02625 -0.00105 -0.00159 -0.00947
AFIX 23
H26A 2 0.797611 0.528094 0.147481 11.00000 -1.20000
H26B 2 0.837098 0.478437 0.058430 11.00000 -1.20000
AFIX 0
N27 4 0.792293 0.654384 0.059174 11.00000 0.02753 0.03095 =
0.02569 -0.00494 -0.00273 -0.00566
C28 1 0.628950 0.693361 0.074735 11.00000 0.02936 0.04780 =
0.03558 -0.01188 -0.00242 -0.00667
AFIX 23
H28A 2 0.594543 0.663464 0.126952 11.00000 -1.20000
H28B 2 0.584023 0.665973 0.032329 11.00000 -1.20000
AFIX 0
C29 1 0.588055 0.823285 0.075075 11.00000 0.03754 0.04471 =
0.03756 -0.00794 -0.00587 0.00651
AFIX 23
H29A 2 0.616087 0.852855 0.021498 11.00000 -1.20000
H29B 2 0.482585 0.851596 0.088078 11.00000 -1.20000
AFIX 0
N30 4 0.665890 0.862935 0.137292 11.00000 0.04453 0.03662 =
0.03774 -0.00606 -0.00533 -0.00231
C31 1 0.583601 0.855130 0.220182 11.00000 0.06068 0.07615 =
0.03353 -0.01840 0.00574 0.00088
AFIX 137
H31A 2 0.483478 0.898542 0.220051 11.00000 -1.50000
H31B 2 0.628969 0.885520 0.260177 11.00000 -1.50000
H31C 2 0.585708 0.776336 0.233352 11.00000 -1.50000
AFIX 0
C32 1 0.663721 0.985350 0.121699 11.00000 0.07459 0.03800 =
0.08336 -0.00571 -0.02153 -0.00383
AFIX 137
H32A 2 0.563746 1.029869 0.123823 11.00000 -1.50000
H32B 2 0.714451 0.993946 0.068657 11.00000 -1.50000
H32C 2 0.711561 1.011590 0.162508 11.00000 -1.50000
AFIX 0
C33 1 1.276697 0.664738 0.161496 11.00000 0.04742 0.06029 =
0.03996 -0.00716 -0.00415 -0.02535
AFIX 137
H33A 2 1.212508 0.726816 0.192611 11.00000 -1.50000
H33B 2 1.330444 0.695058 0.116447 11.00000 -1.50000
H33C 2 1.344350 0.618271 0.195766 11.00000 -1.50000
AFIX 0
C34 1 1.152575 0.337226 0.029853 11.00000 0.03937 0.02927 =
0.02632 0.00045 -0.00392 -0.00660
AFIX 23
H34A 2 1.058852 0.317037 0.034204 11.00000 -1.20000
H34B 2 1.221156 0.275653 0.055130 11.00000 -1.20000
AFIX 0
B1 3 1.145942 1.057629 0.163281 11.00000 0.08526 0.07001 =
0.04661 0.00422 -0.00932 -0.02918
F1 6 1.213039 1.098688 0.216090 11.00000 0.18931 0.15331 =
0.14368 -0.04022 -0.04716 -0.08856
F2 6 1.224281 1.040287 0.090287 11.00000 0.19402 0.20127 =
0.07773 -0.01896 0.03463 0.01705
F3 6 1.111296 0.966982 0.198273 11.00000 0.32438 0.17236 =
0.22889 0.08978 -0.13960 -0.18751
F4 6 1.022203 1.133623 0.148845 11.00000 0.14320 0.25408 =
0.12989 0.06454 0.00250 0.04578
B2 3 0.248821 0.444711 0.666880 11.00000 0.05083 0.04620 =
0.04368 -0.00093 -0.00130 -0.01120
F5 6 0.394231 0.426269 0.675767 11.00000 0.06441 0.09503 =
0.24474 0.04254 -0.03118 -0.02059
F6 6 0.232229 0.449353 0.587636 11.00000 0.20458 0.13053 =
0.04666 -0.01183 -0.01643 -0.02756
F7 6 0.178474 0.546225 0.702254 11.00000 0.11673 0.05796 =
0.08897 -0.02004 -0.00552 -0.00692
F8 6 0.195874 0.357893 0.705929 11.00000 0.09994 0.07315 =
0.12047 0.01380 0.01528 -0.04091
B3 3 0.624053 0.302625 0.094387 11.00000 0.04165 0.05346 =
0.04002 0.00231 -0.00711 -0.00732
F9 6 0.714039 0.256808 0.028437 11.00000 0.13764 0.17260 =
0.04362 -0.00371 0.01031 0.06830
F10 6 0.694078 0.280865 0.164631 11.00000 0.07195 0.12789 =
0.05940 -0.01345 -0.02249 0.00963
F11 6 0.496954 0.262685 0.105056 11.00000 0.09038 0.08239 =
0.13056 0.02269 -0.04078 -0.03950
F12 6 0.569644 0.419514 0.080264 11.00000 0.06079 0.05724 =
0.13426 0.02363 -0.02374 -0.01093
B4 3 0.832091 0.188065 0.599763 11.00000 0.03610 0.04670 =
0.04554 -0.00590 -0.01125 -0.00294
F13 6 0.715739 0.188843 0.654595 11.00000 0.08677 0.12948 =
0.11070 -0.02601 0.04979 -0.02675
F14 6 0.790933 0.259072 0.533946 11.00000 0.10344 0.09328 =
0.06685 0.00778 -0.04006 0.00563
F15 6 0.937178 0.227541 0.632709 11.00000 0.09392 0.06307 =
0.09547 0.00377 -0.04896 -0.02407
F16 6 0.899050 0.078050 0.571852 11.00000 0.05520 0.05259 =
0.10238 -0.02492 -0.01101 -0.00050
HKLF 4
REM cudbo in P-1 LAST...
REM R1 = 0.0631 for 6004 Fo > 4sig(Fo) and 0.0753 for all 7246 data
REM 517 parameters refined using 12 restraints
END
WGHT 0.0679 6.7312
REM Highest difference peak 0.865, deepest hole -0.519, 1-sigma level 0.102
Q1 1 1.2849 0.7982 0.1250 11.00000 0.05 0.86
Q2 1 0.4637 0.7210 0.1248 11.00000 0.05 0.86
Q3 1 1.0020 1.0385 0.1795 11.00000 0.05 0.85
Q4 1 0.6359 0.2795 0.3662 11.00000 0.05 0.68
Q5 1 0.2249 0.2568 0.3617 11.00000 0.05 0.65
Q6 1 0.1426 0.4341 0.6174 11.00000 0.05 0.65
Q7 1 1.2300 0.9514 0.1241 11.00000 0.05 0.62
Q8 1 0.0362 0.3219 0.3693 11.00000 0.05 0.62
Q9 1 0.3891 0.3563 0.6417 11.00000 0.05 0.62
Q10 1 0.7808 0.3023 0.0554 11.00000 0.05 0.59
;
#===========================================================================
# 7. Structure factors for 1
#===========================================================================
#
# h,k,l, Fc-squared, Fo-squared, sigma(Fo-squared) and status flag
#
#data_cudbo
_shelx_title ' cudbo in P-1 LAST...'
_shelx_refln_list_code 4
_shelx_F_calc_maximum 246.92
#_exptl_crystal_F_000 948.00
_reflns_d_resolution_high 0.8035
#loop_
# _symmetry_equiv_pos_as_xyz
# 'x, y, z'
# '-x, -y, -z'
#_cell_length_a 9.4555
#_cell_length_b 12.0445
#_cell_length_c 16.4925
#_cell_angle_alpha 87.469
#_cell_angle_beta 83.061
#_cell_angle_gamma 75.465
#
_shelx_F_squared_multiplier 1.000
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_calc
_refln_F_squared_meas
_refln_F_squared_sigma
_refln_observed_status
1 0 0 47.66 49.26 3.48 o
2 0 0 4875.57 5398.61 98.56 o
3 0 0 8671.37 8641.44 108.62 o
4 0 0 923.36 812.97 23.12 o
5 0 0 1020.32 1158.38 30.03 o
6 0 0 97.70 69.32 5.97 o
7 0 0 1517.62 1651.46 43.68 o
8 0 0 0.64 6.24 5.66 o
9 0 0 342.91 317.36 10.27 o
10 0 0 47.16 69.62 18.38 o
11 0 0 199.52 178.75 34.48 o
-11 1 0 46.92 36.64 11.42 o
-10 1 0 954.60 1044.14 42.05 o
-9 1 0 27.61 48.59 6.26 o
-8 1 0 10.07 8.01 14.08 o
-7 1 0 215.58 206.66 21.83 o
-6 1 0 374.44 342.74 25.00 o
-5 1 0 2441.73 2953.96 152.51 o
-4 1 0 8823.41 8295.82 254.78 o
-3 1 0 24078.02 24167.80 187.23 o
-2 1 0 2060.61 2018.72 46.34 o
-1 1 0 9351.63 8741.91 72.72 o
0 1 0 135.38 34.82 1.47 o
1 1 0 6395.25 5589.98 118.10 o
3 1 0 349.13 277.44 8.93 o
4 1 0 991.87 724.80 21.90 o
5 1 0 6.01 58.47 7.59 o
6 1 0 538.63 433.95 23.05 o
7 1 0 86.86 77.00 8.22 o
8 1 0 52.55 50.52 6.54 o
9 1 0 4.84 3.94 6.21 o
10 1 0 910.89 825.97 23.97 o
11 1 0 70.09 85.01 13.62 o
-10 2 0 15.06 24.70 12.15 o
-9 2 0 23.54 15.26 10.37 o
-8 2 0 33.84 35.25 9.31 o
-7 2 0 187.33 224.08 17.02 o
-6 2 0 52.11 53.50 5.95 o
-5 2 0 660.98 653.41 63.16 o
-4 2 0 5795.49 6074.24 105.27 o
-3 2 0 1553.45 1673.85 68.75 o
-2 2 0 10573.09 11041.68 117.48 o
-1 2 0 287.08 255.40 6.67 o
0 2 0 8062.28 7137.30 69.20 o
1 2 0 2570.70 3093.85 77.79 o
2 2 0 17.62 41.53 7.03 o
3 2 0 8.03 16.20 3.01 o
4 2 0 46.59 44.71 7.40 o
5 2 0 1224.85 1154.01 30.58 o
6 2 0 21.51 27.55 7.23 o
7 2 0 4897.42 5079.60 110.15 o
8 2 0 112.75 155.35 9.00 o
9 2 0 23.43 22.36 7.20 o
10 2 0 37.93 26.49 26.57 o
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-3 -5 18 250.00 215.57 15.44 o
-2 -5 18 0.49 16.88 9.94 o
-1 -5 18 38.63 68.91 12.48 o
0 -5 18 114.53 89.64 14.15 o
1 -5 18 0.46 6.06 10.41 o
2 -5 18 96.71 117.41 13.54 o
3 -5 18 11.65 42.21 21.18 o
-3 -4 18 64.56 32.04 11.83 o
-2 -4 18 0.43 13.14 9.53 o
-1 -4 18 418.08 451.26 18.52 o
0 -4 18 25.76 26.37 9.52 o
1 -4 18 4.71 1.52 11.05 o
2 -4 18 30.64 22.80 10.22 o
3 -4 18 355.03 376.27 17.24 o
4 -4 18 79.79 100.03 12.33 o
-4 -3 18 36.99 37.15 11.48 o
-3 -3 18 135.20 156.84 13.09 o
-2 -3 18 14.85 -5.72 9.42 o
-1 -3 18 119.90 116.59 26.91 o
0 -3 18 382.11 408.61 17.14 o
1 -3 18 6.03 3.56 8.16 o
2 -3 18 281.98 319.08 16.25 o
3 -3 18 29.03 31.57 10.95 o
4 -3 18 308.41 294.48 32.81 o
5 -3 18 0.60 22.20 12.50 o
-4 -2 18 178.04 211.36 47.30 o
-3 -2 18 189.50 178.77 13.45 o
-2 -2 18 0.43 14.46 8.98 o
-1 -2 18 411.44 423.00 20.94 o
0 -2 18 29.04 39.73 8.29 o
1 -2 18 0.42 15.29 8.55 o
2 -2 18 10.99 16.26 9.09 o
3 -2 18 607.53 556.70 49.59 o
4 -2 18 67.00 62.92 10.72 o
5 -2 18 6.92 88.44 12.32 o
-4 -1 18 211.92 216.23 20.05 o
-3 -1 18 1.40 -10.12 11.83 o
-2 -1 18 15.85 10.25 9.74 o
-1 -1 18 151.98 154.54 12.63 o
0 -1 18 697.12 755.82 20.50 o
1 -1 18 31.47 18.51 11.32 o
2 -1 18 11.74 18.62 12.92 o
3 -1 18 42.66 55.59 14.15 o
4 -1 18 3.81 2.19 10.71 o
5 -1 18 18.23 39.06 12.31 o
6 -1 18 163.43 129.30 16.68 o
-4 0 18 455.44 466.10 22.59 o
-3 0 18 36.69 35.80 10.44 o
-2 0 18 4.19 7.95 9.03 o
-1 0 18 517.05 512.51 17.74 o
0 0 18 159.11 132.81 11.38 o
1 0 18 16.14 48.66 10.40 o
2 0 18 23.86 11.53 9.99 o
3 0 18 355.78 336.06 15.91 o
4 0 18 0.49 34.49 21.89 o
5 0 18 131.72 130.19 12.75 o
6 0 18 455.67 425.67 19.49 o
-4 1 18 175.05 190.58 22.13 o
-3 1 18 269.02 241.95 14.91 o
-2 1 18 173.91 141.23 13.43 o
-1 1 18 23.72 20.35 8.06 o
0 1 18 994.40 944.89 27.59 o
1 1 18 0.31 8.58 7.93 o
2 1 18 470.83 426.89 16.57 o
3 1 18 211.54 181.20 13.75 o
4 1 18 78.72 54.21 13.33 o
5 1 18 365.57 380.25 17.55 o
6 1 18 237.48 266.55 18.03 o
-3 2 18 180.47 166.72 19.10 o
-2 2 18 5.16 11.13 8.67 o
-1 2 18 405.96 356.68 16.47 o
0 2 18 5.29 1.58 11.46 o
1 2 18 10.27 24.46 8.93 o
2 2 18 125.88 174.90 21.76 o
3 2 18 690.06 557.70 35.50 o
4 2 18 15.11 23.59 10.77 o
5 2 18 1.06 28.98 12.15 o
6 2 18 518.64 483.63 21.11 o
-3 3 18 26.24 13.51 10.54 o
-2 3 18 6.42 3.46 9.86 o
-1 3 18 5.78 7.33 8.34 o
0 3 18 450.57 469.16 31.72 o
1 3 18 7.24 19.77 8.03 o
2 3 18 849.29 723.62 19.93 o
3 3 18 95.35 154.30 14.80 o
4 3 18 30.84 52.86 13.47 o
5 3 18 181.06 224.01 19.78 o
6 3 18 0.74 7.24 11.90 o
-2 4 18 116.83 129.79 12.93 o
-1 4 18 442.23 466.89 25.17 o
0 4 18 0.01 -3.04 12.14 o
1 4 18 3.16 -6.78 6.78 o
2 4 18 120.49 224.67 30.28 o
3 4 18 274.98 286.29 15.11 o
4 4 18 54.50 58.21 11.86 o
5 4 18 194.88 234.95 16.10 o
6 4 18 43.90 63.01 13.85 o
-2 5 18 176.39 153.07 12.41 o
-1 5 18 16.42 23.28 20.05 o
0 5 18 8.64 13.83 9.11 o
1 5 18 53.97 44.43 9.38 o
2 5 18 124.79 155.60 13.13 o
3 5 18 18.88 7.51 18.79 o
4 5 18 1.74 45.90 16.44 o
5 5 18 269.58 308.08 16.82 o
6 5 18 48.53 26.96 13.21 o
-1 6 18 516.33 491.16 19.97 o
0 6 18 31.36 34.44 12.65 o
1 6 18 959.86 881.41 22.93 o
2 6 18 261.98 268.75 16.32 o
3 6 18 366.73 361.88 17.12 o
4 6 18 14.43 9.70 11.15 o
5 6 18 25.65 25.19 13.06 o
1 7 18 41.47 63.89 15.18 o
2 7 18 321.20 312.92 15.59 o
3 7 18 90.73 107.83 11.96 o
4 7 18 12.60 44.75 17.49 o
0 -5 19 16.39 -10.54 10.54 o
-2 -4 19 32.65 88.74 22.92 o
-1 -4 19 7.12 25.16 10.18 o
0 -4 19 31.84 15.75 14.77 o
1 -4 19 108.20 120.33 27.32 o
2 -4 19 73.82 72.35 11.61 o
-2 -3 19 516.12 467.74 18.33 o
-1 -3 19 5.47 8.74 9.44 o
0 -3 19 81.34 99.56 14.87 o
1 -3 19 186.96 198.65 14.12 o
2 -3 19 25.13 51.52 10.25 o
3 -3 19 3.40 5.05 12.12 o
-2 -2 19 2.79 62.21 26.36 o
-1 -2 19 78.73 83.80 11.05 o
0 -2 19 61.14 68.83 27.38 o
1 -2 19 129.54 135.28 11.47 o
2 -2 19 335.92 340.72 17.42 o
3 -2 19 108.73 109.96 13.87 o
4 -2 19 132.83 134.85 13.64 o
-3 -1 19 6.18 3.90 9.89 o
-2 -1 19 127.97 151.98 13.72 o
-1 -1 19 0.70 13.09 12.82 o
0 -1 19 151.23 201.64 16.03 o
1 -1 19 91.97 113.76 22.30 o
2 -1 19 18.73 15.14 13.81 o
3 -1 19 16.40 -1.24 9.62 o
4 -1 19 146.23 186.82 15.37 o
5 -1 19 107.72 128.08 16.04 o
-3 0 19 331.98 362.79 18.59 o
-2 0 19 0.45 5.15 12.62 o
-1 0 19 18.19 27.33 10.35 o
0 0 19 81.32 84.54 11.07 o
1 0 19 281.79 302.13 15.94 o
2 0 19 21.21 15.59 10.23 o
3 0 19 0.18 -2.80 10.16 o
4 0 19 710.06 669.61 22.30 o
5 0 19 12.36 13.71 10.53 o
-2 1 19 111.72 120.02 13.95 o
-1 1 19 0.58 13.00 8.15 o
0 1 19 133.39 148.11 12.03 o
1 1 19 342.63 320.27 15.07 o
2 1 19 8.24 0.13 9.89 o
3 1 19 176.30 184.94 14.67 o
4 1 19 11.28 21.98 10.19 o
5 1 19 247.31 316.55 18.22 o
-2 2 19 145.47 144.45 14.22 o
-1 2 19 1.49 1.94 18.35 o
0 2 19 122.38 89.08 10.01 o
1 2 19 203.11 220.18 13.85 o
2 2 19 86.13 82.36 17.46 o
3 2 19 9.04 29.23 10.34 o
4 2 19 284.09 325.03 17.23 o
5 2 19 29.72 23.07 12.30 o
-2 3 19 78.05 124.36 15.00 o
-1 3 19 13.08 11.66 10.32 o
0 3 19 139.63 144.71 14.07 o
1 3 19 475.74 408.28 26.91 o
2 3 19 55.90 45.83 9.16 o
3 3 19 274.02 279.72 16.04 o
4 3 19 0.02 -10.03 10.03 o
5 3 19 33.42 23.72 13.36 o
-1 4 19 9.04 7.43 14.97 o
0 4 19 29.04 49.70 9.15 o
1 4 19 27.54 27.11 8.99 o
2 4 19 19.61 33.35 8.72 o
3 4 19 8.81 17.67 16.54 o
4 4 19 323.32 316.25 17.19 o
5 4 19 0.36 4.69 10.03 o
0 5 19 366.00 344.73 16.78 o
1 5 19 4.46 8.68 9.79 o
2 5 19 127.39 95.55 19.44 o
3 5 19 554.83 511.07 21.76 o
4 5 19 3.34 15.02 10.40 o
2 6 19 31.59 39.35 9.98 o
3 6 19 2.66 7.35 9.57 o
0 -2 20 533.23 524.00 29.67 o
1 -2 20 0.85 -0.28 9.18 o
2 -2 20 151.38 170.72 26.84 o
-1 -1 20 406.93 390.30 19.44 o
0 -1 20 1.03 7.05 11.56 o
1 -1 20 3.93 5.74 8.44 o
2 -1 20 20.80 29.09 11.68 o
3 -1 20 553.01 558.51 46.35 o
-1 0 20 4.54 16.07 9.81 o
0 0 20 431.28 447.85 17.92 o
1 0 20 17.86 28.49 16.30 o
2 0 20 158.84 145.37 25.54 o
3 0 20 30.30 6.55 15.69 o
-1 1 20 367.56 349.51 24.96 o
0 1 20 6.77 6.04 8.76 o
1 1 20 7.29 28.03 9.31 o
2 1 20 0.35 9.98 9.74 o
3 1 20 126.65 120.53 18.07 o
0 2 20 287.06 318.51 18.75 o
1 2 20 2.72 16.29 9.34 o
2 2 20 457.63 449.44 18.58 o
3 2 20 34.64 20.92 13.57 o
1 3 20 3.79 12.46 8.98 o
2 3 20 0.49 72.13 11.93 o
3 3 20 205.81 190.36 16.27 o
2 4 20 515.19 500.20 29.50 o
#===========================================================================
# 8. STRUCTURE [Cu2(H2O)2(F)2(dimeim)].(BF4)2.2H2O (2)
#===========================================================================
data_2
# clave original: CuDBC (ICUAP, 2003)
# clave original:
# clave Tesis:
_database_code_CAS ?
_database_code_CSD ?
_audit_creation_method SHELXL97
_audit_creation_date 2011-08-26
loop_
_audit_contact_author_name
_audit_contact_author_address
_audit_contact_author_email
_audit_contact_author_fax
_audit_contact_author_phone
'Bern\`es, Sylvain'
;
Universidad Aut\'onoma de Nuevo Le\'on, UANL
Facultad de Ciencias Qu\'imicas
Av. Universidad S/N
Ciudad Universitaria
San Nicol\'as de los Garza
Nuevo Le\'on CP 66451
Mexico
;
sylvain_bernes@Hotmail.com . .
_chemical_name_systematic
;
[\m-2,2'-(2,8-Dimethyl-4,7,10,12-tetrahydrodi-imidazo[4,5-c:4',5'-
h][1,6]diazecine-5,11(1H,6H)-diyl) bis(N,N-
dimethylethanamine)]-di-aqua-difluorido-di-copper(ii) bis(tetrafluoridoborate)
dihydrate
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C20 H40 Cu2 F2 N8 O2, 2(B F4), 2(H2 O)'
_chemical_formula_sum 'C20 H44 B2 Cu2 F10 N8 O4'
_chemical_formula_weight 799.33
_chemical_compound_source methanol
_chemical_absolute_configuration .
_chemical_optical_rotation ?
_chemical_properties_physical ?
_chemical_properties_biological ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'B' 'B' 0.0013 0.0007
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'F' 'F' 0.0171 0.0103
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cu' 'Cu' 0.3201 1.2651
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_Int_Tables_number 14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 10.4816(9)
_cell_length_b 7.0223(7)
_cell_length_c 22.732(3)
_cell_angle_alpha 90.00
_cell_angle_beta 95.913(8)
_cell_angle_gamma 90.00
_cell_volume 1664.3(3)
_cell_formula_units_Z 2
_cell_measurement_temperature 296(2)
_cell_measurement_reflns_used 64
_cell_measurement_theta_min 4.87
_cell_measurement_theta_max 12.49
_exptl_crystal_description prism
_exptl_crystal_colour blue
_exptl_crystal_size_max 0.68
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.12
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.595
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 820
_exptl_absorpt_coefficient_mu 1.374
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_correction_T_min 0.24433
_exptl_absorpt_correction_T_max 0.29630
_exptl_absorpt_process_details 'XSCANS (Siemens, 1996)'
_exptl_special_details ?
_diffrn_ambient_temperature 296(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker P4'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 2
_diffrn_standards_interval_count 98
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-1 -1 4
1 -1 -4
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% 0.5
_diffrn_reflns_number 5831
_diffrn_reflns_av_R_equivalents 0.0278
_diffrn_reflns_av_sigmaI/netI 0.0354
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_theta_min 1.95
_diffrn_reflns_theta_max 25.00
_reflns_number_total 2924
_reflns_number_gt 2161
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'XSCANS (Siemens, 1996)'
_computing_cell_refinement XSCANS
_computing_data_reduction XSCANS
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'MERCURY CSD 2.0 (Macrae et al., 2006)'
_computing_publication_material SHELXL-97
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+2.1934P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method SHELXL97
_refine_ls_extinction_coef 0.0047(9)
_refine_ls_extinction_expression
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns 2924
_refine_ls_number_parameters 224
_refine_ls_number_restraints 6
_refine_ls_number_constraints 0
_refine_ls_R_factor_all 0.0583
_refine_ls_R_factor_gt 0.0417
_refine_ls_wR_factor_ref 0.1278
_refine_ls_wR_factor_gt 0.1129
_refine_ls_goodness_of_fit_ref 1.055
_refine_ls_restrained_S_all 1.054
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.06756(4) 0.24937(6) 0.144422(16) 0.02909(19) Uani 1 1 d . . .
O1 O 0.0452(3) -0.0199(4) 0.19138(12) 0.0514(8) Uani 1 1 d D . .
H11 H 0.028(4) -0.030(7) 0.2269(7) 0.077 Uiso 1 1 d D . .
H12 H -0.002(4) -0.102(6) 0.1723(17) 0.077 Uiso 1 1 d D . .
F2 F -0.0143(2) 0.4102(3) 0.19710(9) 0.0463(6) Uani 1 1 d . . .
N1 N -0.2552(3) 0.1377(5) 0.02864(13) 0.0357(7) Uani 1 1 d . . .
H1A H -0.3331 0.1048 0.0177 0.043 Uiso 1 1 calc R . .
C2 C -0.2104(3) 0.1934(6) 0.08313(16) 0.0349(8) Uani 1 1 d . . .
N3 N -0.0859(3) 0.2316(4) 0.08490(13) 0.0301(7) Uani 1 1 d . . .
C4 C -0.0518(3) 0.2022(5) 0.02837(15) 0.0295(8) Uani 1 1 d . . .
C5 C -0.1557(3) 0.1415(5) -0.00760(15) 0.0309(8) Uani 1 1 d . . .
C6 C 0.0853(3) 0.2396(5) 0.02066(15) 0.0288(7) Uani 1 1 d . . .
H6A H 0.1014 0.3755 0.0193 0.035 Uiso 1 1 calc R . .
H6B H 0.1076 0.1829 -0.0158 0.035 Uiso 1 1 calc R . .
N7 N 0.1624(3) 0.1519(4) 0.07258(12) 0.0296(7) Uani 1 1 d . . .
C8 C 0.2950(4) 0.2307(6) 0.08214(17) 0.0382(9) Uani 1 1 d . . .
H8A H 0.2956 0.3616 0.0685 0.046 Uiso 1 1 calc R . .
H8B H 0.3521 0.1570 0.0600 0.046 Uiso 1 1 calc R . .
C9 C 0.3395(4) 0.2214(6) 0.14785(18) 0.0435(10) Uani 1 1 d . . .
H9A H 0.3485 0.0895 0.1602 0.052 Uiso 1 1 calc R . .
H9B H 0.4226 0.2825 0.1555 0.052 Uiso 1 1 calc R . .
N10 N 0.2447(3) 0.3190(5) 0.18224(14) 0.0395(8) Uani 1 1 d . . .
C11 C 0.2590(5) 0.5285(7) 0.1791(2) 0.0665(14) Uani 1 1 d . . .
H11B H 0.3459 0.5631 0.1922 0.100 Uiso 1 1 calc R . .
H11C H 0.2021 0.5882 0.2040 0.100 Uiso 1 1 calc R . .
H11D H 0.2382 0.5700 0.1390 0.100 Uiso 1 1 calc R . .
C12 C 0.2675(5) 0.2562(8) 0.24504(19) 0.0631(15) Uani 1 1 d . . .
H12B H 0.3526 0.2918 0.2609 0.095 Uiso 1 1 calc R . .
H12C H 0.2584 0.1204 0.2471 0.095 Uiso 1 1 calc R . .
H12D H 0.2061 0.3160 0.2676 0.095 Uiso 1 1 calc R . .
C13 C -0.2884(4) 0.2093(7) 0.1346(2) 0.0523(12) Uani 1 1 d . . .
H13A H -0.2321 0.2218 0.1705 0.078 Uiso 1 1 calc R . .
H13B H -0.3401 0.0972 0.1367 0.078 Uiso 1 1 calc R . .
H13C H -0.3429 0.3192 0.1296 0.078 Uiso 1 1 calc R . .
C14 C 0.1615(3) -0.0638(5) 0.06897(14) 0.0322(8) Uani 1 1 d . . .
H14A H 0.2382 -0.1120 0.0916 0.039 Uiso 1 1 calc R . .
H14B H 0.0882 -0.1111 0.0874 0.039 Uiso 1 1 calc R . .
O3 O -0.0898(3) 0.7030(5) 0.12912(15) 0.0567(8) Uani 1 1 d D . .
H31 H -0.1703(13) 0.704(8) 0.121(3) 0.085 Uiso 1 1 d D . .
H32 H -0.073(4) 0.603(5) 0.149(2) 0.085 Uiso 1 1 d D . .
B1 B 0.5359(6) 0.7327(9) 0.0843(3) 0.0608(15) Uani 1 1 d . . .
F11 F 0.5071(4) 0.8784(7) 0.0446(2) 0.1190(15) Uani 1 1 d . . .
F12 F 0.4597(5) 0.5886(7) 0.0690(2) 0.157(2) Uani 1 1 d . . .
F13 F 0.5112(7) 0.8022(10) 0.1374(2) 0.176(3) Uani 1 1 d . . .
F14 F 0.6592(4) 0.7030(9) 0.0821(4) 0.189(3) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0303(3) 0.0348(3) 0.0223(3) -0.00379(17) 0.00353(17) -0.00217(18)
O1 0.077(2) 0.0490(18) 0.0300(14) 0.0034(13) 0.0126(14) -0.0183(16)
F2 0.0526(13) 0.0550(14) 0.0315(11) -0.0118(10) 0.0056(10) 0.0090(12)
N1 0.0249(15) 0.0454(19) 0.0367(16) -0.0053(14) 0.0028(12) -0.0010(14)
C2 0.0287(18) 0.042(2) 0.0338(19) -0.0091(17) 0.0032(15) 0.0018(16)
N3 0.0317(16) 0.0351(16) 0.0245(14) -0.0034(12) 0.0075(12) -0.0004(13)
C4 0.0304(18) 0.0319(18) 0.0269(17) -0.0002(14) 0.0056(14) 0.0025(15)
C5 0.0311(18) 0.0340(19) 0.0276(17) -0.0009(15) 0.0031(14) 0.0034(15)
C6 0.0315(18) 0.0314(18) 0.0237(16) -0.0005(14) 0.0048(13) -0.0038(15)
N7 0.0270(15) 0.0353(16) 0.0265(14) -0.0020(13) 0.0036(12) -0.0049(13)
C8 0.0279(18) 0.053(2) 0.0344(19) -0.0070(17) 0.0063(15) -0.0064(17)
C9 0.0283(19) 0.060(3) 0.041(2) -0.0123(19) -0.0008(16) -0.0066(18)
N10 0.0378(17) 0.0475(19) 0.0328(16) -0.0069(15) 0.0017(13) -0.0060(16)
C11 0.065(3) 0.051(3) 0.085(4) -0.023(3) 0.017(3) -0.018(2)
C12 0.051(3) 0.106(4) 0.030(2) -0.004(2) -0.0061(19) -0.005(3)
C13 0.041(2) 0.076(3) 0.043(2) -0.014(2) 0.0185(19) -0.005(2)
C14 0.0336(19) 0.036(2) 0.0261(17) -0.0017(15) 0.0009(14) 0.0012(16)
O3 0.062(2) 0.0554(19) 0.0519(19) 0.0069(15) 0.0014(16) -0.0135(16)
B1 0.050(3) 0.065(4) 0.064(4) 0.016(3) -0.008(3) -0.019(3)
F11 0.089(3) 0.124(3) 0.137(3) 0.045(3) -0.022(2) -0.003(2)
F12 0.169(4) 0.145(4) 0.162(4) -0.028(3) 0.043(4) -0.107(4)
F13 0.216(6) 0.217(6) 0.096(4) -0.007(4) 0.010(4) -0.100(5)
F14 0.057(2) 0.177(5) 0.325(9) 0.068(5) -0.014(4) 0.020(3)
_geom_special_details ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 F2 1.912(2) . ?
Cu1 N3 1.997(3) . ?
Cu1 N10 2.024(3) . ?
Cu1 N7 2.111(3) . ?
Cu1 O1 2.196(3) . ?
O1 H11 0.848(10) . ?
O1 H12 0.846(10) . ?
N1 C2 1.337(5) . ?
N1 C5 1.394(4) . ?
N1 H1A 0.8600 . ?
C2 N3 1.329(5) . ?
C2 C13 1.499(5) . ?
N3 C4 1.384(4) . ?
C4 C5 1.361(5) . ?
C4 C6 1.490(5) . ?
C5 C14 1.493(5) 3 ?
C6 N7 1.492(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
N7 C8 1.491(4) . ?
N7 C14 1.517(5) . ?
C8 C9 1.520(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N10 1.493(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N10 C11 1.481(6) . ?
N10 C12 1.490(5) . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C11 H11D 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C12 H12D 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C5 1.493(5) 3 ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
O3 H31 0.845(10) . ?
O3 H32 0.847(10) . ?
B1 F12 1.314(7) . ?
B1 F14 1.315(8) . ?
B1 F13 1.352(9) . ?
B1 F11 1.377(7) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F2 Cu1 N3 94.53(10) . . ?
F2 Cu1 N10 92.45(11) . . ?
N3 Cu1 N10 160.54(13) . . ?
F2 Cu1 N7 162.38(11) . . ?
N3 Cu1 N7 82.31(11) . . ?
N10 Cu1 N7 85.56(12) . . ?
F2 Cu1 O1 97.29(11) . . ?
N3 Cu1 O1 99.01(12) . . ?
N10 Cu1 O1 98.10(13) . . ?
N7 Cu1 O1 100.32(12) . . ?
Cu1 O1 H11 126(3) . . ?
Cu1 O1 H12 115(3) . . ?
H11 O1 H12 105(2) . . ?
C2 N1 C5 109.2(3) . . ?
C2 N1 H1A 125.4 . . ?
C5 N1 H1A 125.4 . . ?
N3 C2 N1 109.7(3) . . ?
N3 C2 C13 125.0(3) . . ?
N1 C2 C13 125.3(3) . . ?
C2 N3 C4 106.8(3) . . ?
C2 N3 Cu1 138.9(3) . . ?
C4 N3 Cu1 111.8(2) . . ?
C5 C4 N3 109.7(3) . . ?
C5 C4 C6 134.9(3) . . ?
N3 C4 C6 115.3(3) . . ?
C4 C5 N1 104.6(3) . . ?
C4 C5 C14 129.0(3) . 3 ?
N1 C5 C14 125.7(3) . 3 ?
C4 C6 N7 106.5(3) . . ?
C4 C6 H6A 110.4 . . ?
N7 C6 H6A 110.4 . . ?
C4 C6 H6B 110.4 . . ?
N7 C6 H6B 110.4 . . ?
H6A C6 H6B 108.6 . . ?
C8 N7 C6 112.5(3) . . ?
C8 N7 C14 112.3(3) . . ?
C6 N7 C14 111.7(3) . . ?
C8 N7 Cu1 105.8(2) . . ?
C6 N7 Cu1 102.6(2) . . ?
C14 N7 Cu1 111.4(2) . . ?
N7 C8 C9 108.3(3) . . ?
N7 C8 H8A 110.0 . . ?
C9 C8 H8A 110.0 . . ?
N7 C8 H8B 110.0 . . ?
C9 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
N10 C9 C8 109.9(3) . . ?
N10 C9 H9A 109.7 . . ?
C8 C9 H9A 109.7 . . ?
N10 C9 H9B 109.7 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
C11 N10 C12 109.5(4) . . ?
C11 N10 C9 110.8(3) . . ?
C12 N10 C9 108.4(3) . . ?
C11 N10 Cu1 108.2(3) . . ?
C12 N10 Cu1 112.6(3) . . ?
C9 N10 Cu1 107.3(2) . . ?
N10 C11 H11B 109.5 . . ?
N10 C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N10 C11 H11D 109.5 . . ?
H11B C11 H11D 109.5 . . ?
H11C C11 H11D 109.5 . . ?
N10 C12 H12B 109.5 . . ?
N10 C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N10 C12 H12D 109.5 . . ?
H12B C12 H12D 109.5 . . ?
H12C C12 H12D 109.5 . . ?
C2 C13 H13A 109.5 . . ?
C2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C5 C14 N7 114.5(3) 3 . ?
C5 C14 H14A 108.6 3 . ?
N7 C14 H14A 108.6 . . ?
C5 C14 H14B 108.6 3 . ?
N7 C14 H14B 108.6 . . ?
H14A C14 H14B 107.6 . . ?
H31 O3 H32 106(2) . . ?
F12 B1 F14 116.1(7) . . ?
F12 B1 F13 110.4(5) . . ?
F14 B1 F13 111.8(6) . . ?
F12 B1 F11 108.2(5) . . ?
F14 B1 F11 104.1(5) . . ?
F13 B1 F11 105.5(6) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C2 N3 -0.8(4) . . . . ?
C5 N1 C2 C13 179.6(4) . . . . ?
N1 C2 N3 C4 1.4(4) . . . . ?
C13 C2 N3 C4 -179.0(4) . . . . ?
N1 C2 N3 Cu1 -157.9(3) . . . . ?
C13 C2 N3 Cu1 21.7(7) . . . . ?
F2 Cu1 N3 C2 -49.7(4) . . . . ?
N10 Cu1 N3 C2 -160.3(4) . . . . ?
N7 Cu1 N3 C2 147.8(4) . . . . ?
O1 Cu1 N3 C2 48.5(4) . . . . ?
F2 Cu1 N3 C4 151.7(2) . . . . ?
N10 Cu1 N3 C4 41.1(5) . . . . ?
N7 Cu1 N3 C4 -10.8(2) . . . . ?
O1 Cu1 N3 C4 -110.1(2) . . . . ?
C2 N3 C4 C5 -1.5(4) . . . . ?
Cu1 N3 C4 C5 164.0(2) . . . . ?
C2 N3 C4 C6 179.4(3) . . . . ?
Cu1 N3 C4 C6 -15.1(4) . . . . ?
N3 C4 C5 N1 1.0(4) . . . . ?
C6 C4 C5 N1 179.9(4) . . . . ?
N3 C4 C5 C14 -169.6(3) . . . 3 ?
C6 C4 C5 C14 9.3(7) . . . 3 ?
C2 N1 C5 C4 -0.2(4) . . . . ?
C2 N1 C5 C14 170.8(4) . . . 3 ?
C5 C4 C6 N7 -134.9(4) . . . . ?
N3 C4 C6 N7 43.9(4) . . . . ?
C4 C6 N7 C8 -160.7(3) . . . . ?
C4 C6 N7 C14 72.0(3) . . . . ?
C4 C6 N7 Cu1 -47.4(3) . . . . ?
F2 Cu1 N7 C8 70.2(4) . . . . ?
N3 Cu1 N7 C8 150.8(2) . . . . ?
N10 Cu1 N7 C8 -13.9(2) . . . . ?
O1 Cu1 N7 C8 -111.3(2) . . . . ?
F2 Cu1 N7 C6 -47.9(4) . . . . ?
N3 Cu1 N7 C6 32.7(2) . . . . ?
N10 Cu1 N7 C6 -132.0(2) . . . . ?
O1 Cu1 N7 C6 130.6(2) . . . . ?
F2 Cu1 N7 C14 -167.5(3) . . . . ?
N3 Cu1 N7 C14 -86.9(2) . . . . ?
N10 Cu1 N7 C14 108.4(2) . . . . ?
O1 Cu1 N7 C14 10.9(2) . . . . ?
C6 N7 C8 C9 150.2(3) . . . . ?
C14 N7 C8 C9 -82.8(4) . . . . ?
Cu1 N7 C8 C9 38.9(3) . . . . ?
N7 C8 C9 N10 -54.2(4) . . . . ?
C8 C9 N10 C11 -77.6(4) . . . . ?
C8 C9 N10 C12 162.3(3) . . . . ?
C8 C9 N10 Cu1 40.3(4) . . . . ?
F2 Cu1 N10 C11 -57.1(3) . . . . ?
N3 Cu1 N10 C11 53.9(5) . . . . ?
N7 Cu1 N10 C11 105.4(3) . . . . ?
O1 Cu1 N10 C11 -154.8(3) . . . . ?
F2 Cu1 N10 C12 64.0(3) . . . . ?
N3 Cu1 N10 C12 175.0(4) . . . . ?
N7 Cu1 N10 C12 -133.5(3) . . . . ?
O1 Cu1 N10 C12 -33.7(3) . . . . ?
F2 Cu1 N10 C9 -176.7(3) . . . . ?
N3 Cu1 N10 C9 -65.7(5) . . . . ?
N7 Cu1 N10 C9 -14.2(3) . . . . ?
O1 Cu1 N10 C9 85.6(3) . . . . ?
C8 N7 C14 C5 -94.2(4) . . . 3 ?
C6 N7 C14 C5 33.2(4) . . . 3 ?
Cu1 N7 C14 C5 147.3(2) . . . 3 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H11 F2 0.848(10) 1.798(15) 2.635(3) 169(5) 2_545 .
O1 H12 O3 0.846(10) 1.873(12) 2.716(4) 174(5) 1_545 .
N1 H1A F11 0.86 2.19 2.974(5) 150.9 3_565 .
N1 H1A F11 0.86 2.43 3.137(5) 139.5 1_445 .
O3 H31 F14 0.845(10) 1.911(19) 2.736(6) 165(6) 1_455 .
O3 H32 F2 0.847(10) 1.804(13) 2.644(4) 171(5) . .
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.749
_refine_diff_density_min -0.784
_refine_diff_density_rms 0.080
#===========================================================================
# 9. SHELX CODE
#===========================================================================
_iucr_refine_instructions_details
;
TITL cudbc in P2(1)/c
CELL 0.71073 10.4816 7.0223 22.7318 90.000 95.913 90.000
ZERR 2.00 0.0009 0.0007 0.0030 0.000 0.008 0.000
LATT 1
SYMM -X, 0.5+Y, 0.5-Z
SFAC C H B N O F CU
UNIT 40 88 4 16 8 20 4
TEMP 23
OMIT -1 0 2
OMIT 0 0 2
L.S. 12
ACTA
CONF
BOND $H
WPDB -2
FMAP 2
HTAB
PLAN 10
EQIV $1 -x, y-1/2, -z+1/2
EQIV $2 x, y-1, z
EQIV $3 -x, -y+1, -z
EQIV $4 x-1, y-1, z
EQIV $5 x-1, y, z
HTAB O1 F2_$1
HTAB O1 O3_$2
HTAB N1 F11_$3
HTAB N1 F11_$4
HTAB O3 F14_$5
HTAB O3 F2
DFIX 0.85 0.01 O1 H11
DFIX 0.85 0.01 O1 H12
DFIX 1.34 0.02 H11 H12
DFIX 0.85 0.01 O3 H31
DFIX 0.85 0.01 O3 H32
DFIX 1.34 0.02 H31 H32
WGHT 0.064500 2.193400
EXTI 0.004659
FVAR 0.32254
CU1 7 0.067565 0.249365 0.144422 11.00000 0.03032 0.03480 =
0.02231 -0.00379 0.00353 -0.00217
O1 5 0.045210 -0.019950 0.191379 11.00000 0.07672 0.04905 =
0.02999 0.00340 0.01264 -0.01835
H11 2 0.027796 -0.030424 0.226869 11.00000 -1.50000
H12 2 -0.001744 -0.101774 0.172301 11.00000 -1.50000
F2 6 -0.014331 0.410165 0.197098 11.00000 0.05262 0.05503 =
0.03146 -0.01180 0.00563 0.00897
N1 4 -0.255208 0.137720 0.028641 11.00000 0.02489 0.04539 =
0.03671 -0.00534 0.00276 -0.00099
AFIX 43
H1A 2 -0.333065 0.104794 0.017681 11.00000 -1.20000
AFIX 0
C2 1 -0.210418 0.193425 0.083133 11.00000 0.02870 0.04224 =
0.03375 -0.00913 0.00322 0.00175
N3 4 -0.085932 0.231556 0.084904 11.00000 0.03173 0.03510 =
0.02450 -0.00336 0.00752 -0.00039
C4 1 -0.051849 0.202228 0.028374 11.00000 0.03037 0.03188 =
0.02688 -0.00016 0.00559 0.00249
C5 1 -0.155700 0.141467 -0.007597 11.00000 0.03113 0.03401 =
0.02762 -0.00091 0.00306 0.00340
C6 1 0.085349 0.239570 0.020655 11.00000 0.03149 0.03145 =
0.02372 -0.00048 0.00479 -0.00377
AFIX 23
H6A 2 0.101359 0.375475 0.019340 11.00000 -1.20000
H6B 2 0.107633 0.182930 -0.015840 11.00000 -1.20000
AFIX 0
N7 4 0.162368 0.151917 0.072576 11.00000 0.02698 0.03533 =
0.02653 -0.00201 0.00358 -0.00490
C8 1 0.294980 0.230738 0.082136 11.00000 0.02792 0.05296 =
0.03436 -0.00699 0.00634 -0.00637
AFIX 23
H8A 2 0.295643 0.361628 0.068536 11.00000 -1.20000
H8B 2 0.352116 0.157043 0.060034 11.00000 -1.20000
AFIX 0
C9 1 0.339544 0.221418 0.147855 11.00000 0.02834 0.06031 =
0.04086 -0.01234 -0.00080 -0.00659
AFIX 23
H9A 2 0.348512 0.089473 0.160219 11.00000 -1.20000
H9B 2 0.422601 0.282490 0.155518 11.00000 -1.20000
AFIX 0
N10 4 0.244704 0.319017 0.182237 11.00000 0.03777 0.04748 =
0.03280 -0.00688 0.00169 -0.00597
C11 1 0.258951 0.528505 0.179089 11.00000 0.06456 0.05147 =
0.08546 -0.02296 0.01718 -0.01752
AFIX 137
H11B 2 0.345855 0.563077 0.192204 11.00000 -1.50000
H11C 2 0.202078 0.588195 0.204011 11.00000 -1.50000
H11D 2 0.238153 0.570023 0.139011 11.00000 -1.50000
AFIX 0
C12 1 0.267469 0.256228 0.245037 11.00000 0.05110 0.10612 =
0.02980 -0.00416 -0.00613 -0.00534
AFIX 137
H12B 2 0.352570 0.291812 0.260878 11.00000 -1.50000
H12C 2 0.258395 0.120421 0.247072 11.00000 -1.50000
H12D 2 0.206110 0.315989 0.267632 11.00000 -1.50000
AFIX 0
C13 1 -0.288418 0.209330 0.134630 11.00000 0.04141 0.07562 =
0.04285 -0.01399 0.01849 -0.00506
AFIX 137
H13A 2 -0.232144 0.221766 0.170509 11.00000 -1.50000
H13B 2 -0.340123 0.097167 0.136711 11.00000 -1.50000
H13C 2 -0.342924 0.319238 0.129640 11.00000 -1.50000
AFIX 0
C14 1 0.161485 -0.063795 0.068973 11.00000 0.03363 0.03632 =
0.02610 -0.00168 0.00090 0.00125
AFIX 23
H14A 2 0.238232 -0.111980 0.091599 11.00000 -1.20000
H14B 2 0.088223 -0.111125 0.087357 11.00000 -1.20000
AFIX 0
O3 5 -0.089755 0.703008 0.129123 11.00000 0.06204 0.05541 =
0.05187 0.00691 0.00143 -0.01355
H31 2 -0.170306 0.704123 0.121100 11.00000 -1.50000
H32 2 -0.073241 0.603107 0.149397 11.00000 -1.50000
B1 3 0.535927 0.732723 0.084303 11.00000 0.05018 0.06527 =
0.06397 0.01567 -0.00849 -0.01902
F11 6 0.507054 0.878444 0.044595 11.00000 0.08860 0.12426 =
0.13718 0.04481 -0.02178 -0.00329
F12 6 0.459748 0.588629 0.068967 11.00000 0.16937 0.14471 =
0.16207 -0.02848 0.04295 -0.10682
F13 6 0.511209 0.802185 0.137441 11.00000 0.21563 0.21679 =
0.09575 -0.00728 0.00970 -0.09986
F14 6 0.659224 0.703029 0.082065 11.00000 0.05659 0.17732 =
0.32535 0.06807 -0.01409 0.01983
HKLF 4
REM cudbc in P2(1)/c
REM R1 = 0.0417 for 2161 Fo > 4sig(Fo) and 0.0583 for all 2924 data
REM 224 parameters refined using 6 restraints
END
WGHT 0.0643 2.1367
REM Highest difference peak 0.749, deepest hole -0.784, 1-sigma level 0.080
Q1 1 0.5668 0.5821 0.1295 11.00000 0.05 0.75
Q2 1 0.4997 0.8428 0.1430 11.00000 0.05 0.57
Q3 1 0.6646 0.6763 0.0618 11.00000 0.05 0.45
Q4 1 0.4283 0.7873 0.1100 11.00000 0.05 0.42
Q5 1 0.6145 0.7793 0.0476 11.00000 0.05 0.39
Q6 1 0.4793 0.8867 0.0983 11.00000 0.05 0.37
Q7 1 0.4495 0.7404 0.0560 11.00000 0.05 0.36
Q8 1 0.4491 0.8485 0.0946 11.00000 0.05 0.34
Q9 1 0.1446 0.1956 0.0985 11.00000 0.05 0.30
Q10 1 0.4259 0.6268 0.0705 11.00000 0.05 0.30
;
#===========================================================================
# 10. Structure factors for 2
#===========================================================================
#
# h,k,l, Fc-squared, Fo-squared, sigma(Fo-squared) and status flag
#
#data_cudbc
_shelx_title ' cudbc in P2(1)/c'
_shelx_refln_list_code 4
_shelx_F_calc_maximum 246.13
#_exptl_crystal_F_000 820.00
_reflns_d_resolution_high 0.8410
#loop_
# _symmetry_equiv_pos_as_xyz
# 'x, y, z'
# '-x, y+1/2, -z+1/2'
# '-x, -y, -z'
# 'x, -y-1/2, z-1/2'
#_cell_length_a 10.4816
#_cell_length_b 7.0223
#_cell_length_c 22.7318
#_cell_angle_alpha 90.000
#_cell_angle_beta 95.913
#_cell_angle_gamma 90.000
_shelx_F_squared_multiplier 1.000
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_calc
_refln_F_squared_meas
_refln_F_squared_sigma
_refln_observed_status
1 0 0 20486.01 21930.82 124.46 o
2 0 0 4513.81 4870.18 109.27 o
3 0 0 730.17 726.63 24.44 o
4 0 0 4274.56 3923.50 98.92 o
5 0 0 11145.99 10269.78 160.13 o
6 0 0 2025.22 2033.09 69.93 o
7 0 0 5235.87 4995.12 134.09 o
8 0 0 1948.12 1962.68 76.75 o
9 0 0 1777.07 1916.87 66.21 o
10 0 0 873.52 913.26 29.06 o
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-5 1 19 256.89 251.71 9.33 o
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-3 1 19 31.39 23.56 6.72 o
-2 1 19 26.08 13.46 5.10 o
-1 1 19 2.55 -3.32 5.73 o
0 1 19 44.57 57.19 7.23 o
1 1 19 139.83 164.84 13.53 o
2 1 19 36.36 17.12 6.36 o
3 1 19 5.76 0.81 5.99 o
4 1 19 91.71 80.96 12.13 o
5 1 19 64.57 57.00 8.95 o
6 1 19 14.28 5.02 6.32 o
7 1 19 3.04 9.22 8.45 o
-9 2 19 1.63 -0.87 12.30 o
-8 2 19 58.04 37.88 15.67 o
-7 2 19 51.46 59.41 14.71 o
-6 2 19 3.21 0.41 5.81 o
-5 2 19 165.73 199.17 12.02 o
-4 2 19 7.98 3.04 7.30 o
-3 2 19 80.01 73.58 8.63 o
-2 2 19 230.11 241.67 12.30 o
-1 2 19 78.47 80.21 23.70 o
0 2 19 2.94 18.13 9.85 o
1 2 19 179.49 146.03 10.40 o
2 2 19 219.15 220.85 29.47 o
3 2 19 6.36 9.33 6.58 o
4 2 19 211.87 216.73 25.82 o
5 2 19 280.91 253.84 18.49 o
6 2 19 48.43 30.38 13.37 o
7 2 19 21.40 25.28 16.63 o
-8 3 19 27.50 -10.38 13.84 o
-7 3 19 0.02 6.06 13.17 o
-6 3 19 1.72 -1.69 6.37 o
-5 3 19 5.03 3.02 8.03 o
-4 3 19 29.84 27.93 8.62 o
-3 3 19 18.66 3.12 8.70 o
-2 3 19 271.60 273.81 12.58 o
-1 3 19 84.10 92.16 9.03 o
0 3 19 17.11 15.82 7.86 o
1 3 19 29.37 32.41 7.58 o
2 3 19 18.11 2.56 6.71 o
3 3 19 2.23 5.14 6.77 o
4 3 19 11.99 7.46 7.44 o
5 3 19 4.04 9.70 8.94 o
6 3 19 3.38 -0.59 8.03 o
-7 4 19 34.56 0.19 11.92 o
-6 4 19 3.68 4.70 8.12 o
-5 4 19 189.70 202.49 17.00 o
-4 4 19 219.63 193.67 19.28 o
-3 4 19 89.66 86.78 14.05 o
-2 4 19 19.12 10.71 8.68 o
-1 4 19 190.64 190.72 18.52 o
0 4 19 76.28 57.56 12.49 o
1 4 19 31.09 -0.12 8.13 o
2 4 19 0.03 -5.10 10.96 o
3 4 19 106.29 86.44 13.30 o
4 4 19 0.46 -5.70 5.70 o
5 4 19 146.38 127.68 17.15 o
-5 5 19 9.69 3.60 16.82 o
-4 5 19 0.05 -2.85 5.84 o
-3 5 19 0.55 -2.74 5.70 o
-2 5 19 0.17 -4.76 8.41 o
-1 5 19 11.02 4.82 7.34 o
0 5 19 3.36 -0.07 8.40 o
1 5 19 2.77 -1.93 7.13 o
2 5 19 29.62 26.02 11.64 o
3 5 19 5.25 1.23 12.45 o
-9 0 20 3.54 -1.83 9.90 o
-8 0 20 177.14 102.49 23.27 o
-7 0 20 402.94 414.40 32.51 o
-6 0 20 508.62 488.51 27.46 o
-5 0 20 846.41 846.92 19.29 o
-4 0 20 1071.74 1281.59 35.80 o
-3 0 20 170.25 176.23 11.85 o
-2 0 20 975.67 988.94 24.08 o
-1 0 20 528.24 519.51 34.15 o
0 0 20 209.09 205.11 12.31 o
1 0 20 555.20 512.70 35.11 o
2 0 20 1393.29 1592.21 40.95 o
3 0 20 1083.67 910.47 23.55 o
4 0 20 863.60 1005.34 54.47 o
5 0 20 249.90 198.37 17.13 o
6 0 20 38.68 19.98 14.85 o
7 0 20 257.36 179.61 32.11 o
-9 1 20 601.69 578.11 33.18 o
-8 1 20 636.57 688.02 30.06 o
-7 1 20 124.99 151.27 15.27 o
-6 1 20 11.28 6.30 4.89 o
-5 1 20 218.42 235.32 8.64 o
-4 1 20 1398.04 1339.01 25.77 o
-3 1 20 1317.62 1363.62 25.27 o
-2 1 20 161.78 116.35 7.39 o
-1 1 20 2388.21 2500.54 37.89 o
0 1 20 2097.26 2100.18 34.81 o
1 1 20 322.72 360.04 13.19 o
2 1 20 178.34 175.00 7.94 o
3 1 20 37.89 35.29 5.92 o
4 1 20 688.29 790.86 19.10 o
5 1 20 1174.00 1180.61 24.15 o
6 1 20 1167.67 1166.92 24.54 o
7 1 20 216.50 208.66 18.80 o
-8 2 20 226.46 181.91 25.38 o
-7 2 20 394.68 374.77 30.00 o
-6 2 20 396.07 383.85 62.08 o
-5 2 20 354.77 348.68 20.28 o
-4 2 20 516.26 611.10 18.76 o
-3 2 20 7.69 4.92 8.27 o
-2 2 20 4.68 0.53 6.25 o
-1 2 20 34.48 51.70 10.14 o
0 2 20 184.94 196.72 14.04 o
1 2 20 338.57 342.06 15.06 o
2 2 20 273.89 261.33 38.66 o
3 2 20 168.48 140.94 14.52 o
4 2 20 99.32 89.67 11.94 o
5 2 20 0.83 -4.30 8.22 o
6 2 20 8.98 -0.89 7.32 o
-8 3 20 406.51 383.51 31.83 o
-7 3 20 94.49 99.02 19.61 o
-6 3 20 6.29 1.22 6.68 o
-5 3 20 12.00 1.45 7.19 o
-4 3 20 762.75 802.50 46.76 o
-3 3 20 1647.33 1589.39 37.26 o
-2 3 20 737.56 742.54 57.49 o
-1 3 20 1134.84 1129.95 74.89 o
0 3 20 706.29 746.13 27.18 o
1 3 20 81.83 28.73 13.04 o
2 3 20 92.90 72.70 14.33 o
3 3 20 79.78 103.04 14.18 o
4 3 20 587.17 555.68 46.27 o
5 3 20 930.64 1007.13 32.28 o
6 3 20 1088.55 1109.82 36.10 o
-6 4 20 563.22 504.51 26.27 o
-5 4 20 370.17 398.00 21.99 o
-4 4 20 353.52 315.52 29.57 o
-3 4 20 34.95 34.73 10.93 o
-2 4 20 25.47 13.31 9.02 o
-1 4 20 6.42 0.38 7.55 o
0 4 20 363.35 371.66 21.83 o
1 4 20 760.01 757.39 28.57 o
2 4 20 309.43 262.77 21.40 o
3 4 20 199.19 218.50 26.49 o
4 4 20 171.27 188.52 38.41 o
-4 5 20 75.77 57.93 16.64 o
-3 5 20 561.49 440.61 24.24 o
-2 5 20 830.76 937.59 31.53 o
-1 5 20 852.96 884.09 60.23 o
0 5 20 288.65 322.24 21.57 o
1 5 20 0.69 -2.14 6.19 o
2 5 20 53.16 27.74 12.65 o
-8 1 21 0.01 -3.48 7.16 o
-7 1 21 27.61 19.81 12.11 o
-6 1 21 1.09 1.68 5.01 o
-5 1 21 1.24 0.01 4.75 o
-4 1 21 0.67 5.41 5.05 o
-3 1 21 0.17 3.76 4.83 o
-2 1 21 131.19 119.65 9.39 o
-1 1 21 39.85 41.41 8.89 o
0 1 21 16.75 24.63 6.55 o
1 1 21 193.66 212.41 8.83 o
2 1 21 3.56 1.20 5.21 o
3 1 21 28.28 9.15 6.07 o
4 1 21 0.43 -4.61 4.61 o
5 1 21 60.88 48.40 9.18 o
6 1 21 28.41 9.12 6.43 o
-8 2 21 3.07 32.39 14.23 o
-7 2 21 23.91 4.33 11.25 o
-6 2 21 39.12 14.95 17.21 o
-5 2 21 56.17 24.73 16.11 o
-4 2 21 50.98 30.97 13.82 o
-3 2 21 0.11 2.47 5.98 o
-2 2 21 11.96 11.28 7.14 o
-1 2 21 82.45 80.59 25.24 o
0 2 21 201.31 144.99 11.27 o
1 2 21 155.96 145.74 10.38 o
2 2 21 6.54 -5.86 5.86 o
3 2 21 1.30 -2.61 6.22 o
4 2 21 8.22 8.81 9.19 o
5 2 21 2.28 -1.84 7.50 o
6 2 21 0.89 7.87 7.61 o
-7 3 21 3.62 14.32 8.94 o
-6 3 21 70.92 78.42 14.04 o
-5 3 21 1.09 1.81 7.29 o
-4 3 21 15.25 7.44 12.02 o
-3 3 21 29.24 22.47 11.47 o
-2 3 21 9.15 1.46 6.80 o
-1 3 21 2.08 4.58 8.12 o
0 3 21 49.41 25.11 10.19 o
1 3 21 291.13 319.69 19.17 o
2 3 21 21.90 -0.88 7.48 o
3 3 21 0.73 -4.28 5.71 o
4 3 21 22.73 8.14 8.93 o
5 3 21 36.89 19.13 20.67 o
-6 4 21 3.36 -1.04 6.76 o
-5 4 21 9.77 1.79 7.51 o
-4 4 21 15.40 4.55 8.88 o
-3 4 21 0.27 -3.89 9.18 o
-2 4 21 39.92 22.78 11.07 o
-1 4 21 9.53 -1.64 8.51 o
0 4 21 5.82 -5.67 6.69 o
1 4 21 37.17 22.83 11.36 o
2 4 21 7.90 9.31 8.22 o
3 4 21 27.98 14.34 11.48 o
4 4 21 71.79 80.66 21.58 o
-3 5 21 9.03 5.79 8.22 o
-2 5 21 21.06 7.24 8.77 o
-1 5 21 48.21 52.28 14.77 o
0 5 21 6.33 -6.70 6.70 o
1 5 21 15.00 17.32 9.08 o
-8 0 22 556.67 571.71 37.61 o
-7 0 22 179.01 171.81 23.65 o
-6 0 22 12.12 -7.11 8.75 o
-5 0 22 421.25 400.20 20.89 o
-4 0 22 1943.73 1935.14 62.39 o
-3 0 22 2075.02 1939.74 41.29 o
-2 0 22 1840.82 1912.61 41.00 o
-1 0 22 1201.02 1138.86 37.98 o
0 0 22 241.80 217.06 15.72 o
1 0 22 566.44 557.69 17.02 o
2 0 22 569.56 520.90 43.09 o
3 0 22 1004.19 1124.75 32.51 o
4 0 22 942.18 888.34 30.82 o
5 0 22 1561.17 1555.18 40.51 o
6 0 22 797.58 839.85 52.48 o
-8 1 22 203.98 222.39 37.88 o
-7 1 22 838.77 776.25 39.83 o
-6 1 22 1041.27 1050.03 23.17 o
-5 1 22 1079.75 1153.85 23.42 o
-4 1 22 275.80 254.55 17.97 o
-3 1 22 15.17 7.82 6.00 o
-2 1 22 552.90 652.88 11.98 o
-1 1 22 549.86 650.85 32.48 o
0 1 22 715.22 703.86 12.82 o
1 1 22 674.95 748.13 18.23 o
2 1 22 1070.61 1076.81 28.51 o
3 1 22 648.29 678.82 18.69 o
4 1 22 68.05 32.68 8.16 o
5 1 22 2.66 6.74 5.89 o
6 1 22 60.75 58.06 9.29 o
-7 2 22 59.95 41.91 24.90 o
-6 2 22 72.82 22.68 14.18 o
-5 2 22 300.25 296.74 18.93 o
-4 2 22 866.64 862.08 53.84 o
-3 2 22 1087.25 1081.35 41.68 o
-2 2 22 1196.26 1205.61 33.69 o
-1 2 22 1057.47 1027.49 61.07 o
0 2 22 386.89 371.22 20.02 o
1 2 22 124.39 103.64 14.90 o
2 2 22 344.24 347.44 29.09 o
3 2 22 867.90 886.66 31.02 o
4 2 22 802.11 885.92 36.95 o
5 2 22 747.48 607.59 28.67 o
-6 3 22 785.78 850.36 31.29 o
-5 3 22 589.46 573.95 25.14 o
-4 3 22 329.24 362.25 22.37 o
-3 3 22 86.07 82.32 14.61 o
-2 3 22 80.32 43.20 16.05 o
-1 3 22 372.13 430.17 21.73 o
0 3 22 659.09 655.91 26.93 o
1 3 22 371.40 417.41 21.79 o
2 3 22 330.44 332.28 20.24 o
3 3 22 169.32 184.50 16.06 o
4 3 22 3.94 -6.05 6.05 o
-5 4 22 306.14 313.88 39.81 o
-4 4 22 909.01 911.79 33.81 o
-3 4 22 1339.27 1423.19 40.70 o
-2 4 22 911.25 901.98 31.94 o
-1 4 22 614.77 632.55 42.61 o
0 4 22 286.13 261.29 20.19 o
1 4 22 2.13 -3.78 5.81 o
2 4 22 185.37 185.15 18.92 o
3 4 22 486.30 472.84 67.56 o
-7 1 23 10.28 6.78 8.19 o
-6 1 23 44.10 35.02 11.84 o
-5 1 23 43.88 29.20 10.60 o
-4 1 23 54.90 39.60 9.87 o
-3 1 23 34.19 13.40 9.54 o
-2 1 23 16.60 7.71 5.75 o
-1 1 23 15.91 12.75 6.81 o
0 1 23 17.29 17.97 6.66 o
1 1 23 1.33 1.26 5.59 o
2 1 23 11.83 12.51 7.33 o
3 1 23 0.94 -3.11 5.11 o
4 1 23 0.91 0.41 5.53 o
5 1 23 0.96 -0.17 5.19 o
-6 2 23 15.61 -3.79 8.84 o
-5 2 23 0.71 3.01 7.10 o
-4 2 23 1.07 -6.40 6.40 o
-3 2 23 122.78 108.52 15.86 o
-2 2 23 88.72 91.95 16.19 o
-1 2 23 0.06 4.95 7.63 o
0 2 23 178.23 162.06 16.58 o
1 2 23 72.61 65.09 14.08 o
2 2 23 0.28 -0.56 7.72 o
3 2 23 5.30 -6.27 6.27 o
4 2 23 5.20 -6.24 6.24 o
-5 3 23 0.87 -3.20 7.45 o
-4 3 23 3.58 2.29 6.40 o
-3 3 23 1.20 0.20 6.88 o
-2 3 23 0.57 -1.74 6.60 o
-1 3 23 0.40 1.37 7.38 o
0 3 23 1.27 7.03 7.78 o
1 3 23 0.02 7.47 6.87 o
2 3 23 1.26 -1.41 6.05 o
3 3 23 1.83 2.33 7.85 o
-3 4 23 74.76 66.98 14.83 o
-2 4 23 127.12 107.01 17.33 o
-1 4 23 25.82 -2.75 8.75 o
0 4 23 102.56 87.32 15.77 o
1 4 23 210.91 217.74 19.31 o
-6 0 24 944.99 1050.33 115.81 o
-5 0 24 598.42 612.74 27.22 o
-4 0 24 109.55 97.50 15.36 o
-3 0 24 128.34 99.25 19.40 o
-2 0 24 486.63 500.57 23.59 o
-1 0 24 1187.49 1264.73 34.66 o
0 0 24 1064.57 1161.59 73.34 o
1 0 24 996.51 981.55 36.04 o
2 0 24 761.86 789.84 91.69 o
3 0 24 273.87 250.75 32.64 o
4 0 24 3.47 5.39 7.73 o
-6 1 24 113.70 96.36 11.93 o
-5 1 24 237.07 207.14 13.27 o
-4 1 24 745.10 703.26 19.81 o
-3 1 24 1361.03 1336.32 34.51 o
-2 1 24 966.69 926.49 22.17 o
-1 1 24 266.84 256.71 13.51 o
0 1 24 47.26 31.09 10.35 o
1 1 24 283.28 299.25 29.88 o
2 1 24 670.44 705.86 20.25 o
3 1 24 746.52 826.25 35.41 o
4 1 24 700.90 658.41 26.74 o
-6 2 24 883.65 848.20 44.55 o
-5 2 24 315.74 323.34 63.95 o
-4 2 24 134.26 102.14 26.97 o
-3 2 24 0.78 5.05 7.51 o
-2 2 24 109.28 149.10 16.58 o
-1 2 24 481.62 423.40 22.34 o
0 2 24 343.40 344.58 21.36 o
1 2 24 472.11 407.37 24.14 o
2 2 24 700.10 763.89 29.71 o
3 2 24 279.22 268.04 20.26 o
-4 3 24 1016.93 975.50 34.09 o
-3 3 24 1333.84 1396.40 40.77 o
-2 3 24 955.02 949.05 88.77 o
-1 3 24 509.38 541.23 28.66 o
0 3 24 56.72 26.94 11.70 o
1 3 24 55.76 43.81 12.81 o
2 3 24 388.42 326.65 22.71 o
-5 1 25 0.01 0.81 4.83 o
-4 1 25 6.99 3.60 5.92 o
-3 1 25 79.97 94.15 13.89 o
-2 1 25 109.02 108.98 11.77 o
-1 1 25 16.15 11.42 7.34 o
0 1 25 0.14 -0.21 5.04 o
1 1 25 1.06 4.02 5.40 o
2 1 25 0.34 7.32 5.84 o
3 1 25 0.01 -1.84 5.75 o
-4 2 25 0.97 -6.23 6.23 o
-3 2 25 31.00 23.12 10.98 o
-2 2 25 7.49 3.08 7.88 o
-1 2 25 7.40 23.06 10.67 o
0 2 25 13.07 9.41 9.10 o
1 2 25 8.16 4.78 8.36 o
2 2 25 2.26 9.17 8.26 o
-2 3 25 3.01 -6.48 16.39 o
-1 3 25 9.41 -0.22 7.98 o
0 3 25 7.51 19.12 12.45 o
-4 0 26 517.05 471.42 34.48 o
-3 0 26 980.08 1012.45 46.72 o
-2 0 26 565.23 596.84 26.37 o
-1 0 26 110.96 149.90 20.18 o
0 0 26 52.19 53.80 16.10 o
1 0 26 493.08 528.85 26.96 o
2 0 26 833.64 880.50 31.83 o
-4 1 26 31.08 24.23 8.53 o
-3 1 26 0.91 -5.10 5.31 o
-2 1 26 100.13 75.52 10.95 o
-1 1 26 633.90 701.04 20.73 o
0 1 26 967.75 974.65 24.41 o
1 1 26 600.26 604.00 25.00 o
-2 2 26 703.96 737.37 34.34 o
-1 2 26 339.51 338.11 21.36 o
0 2 26 42.24 16.45 11.96 o
#===========================================================================
# 11. C'est fini
#===========================================================================
#EOF