data_General _audit_creation_date '2010-03-14' _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Tamotsu Inabe' _publ_contact_author_email 'inabe@sci.hokudai.ac.jp' _publ_contact_author_fax '81-11-706-3511' _publ_contact_author_phone '81-11-706-3511' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'Crystals' #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Metallic one-dimensional conductors composed of axially ligated (phthalocyanato)CoIII with supramolecular cations of A(EtOH)4 (A = Na and K) ; #============================================================================== data__K-salt_________________ #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C76 H56 Co2 K N20 O4' _chemical_formula_moiety 'C76 H56 Co2 K N20 O4' _chemical_formula_weight 1470.37 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n' _symmetry_space_group_name_Hall '-P 4bc' _symmetry_Int_Tables_number 86 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 '+X,+Y,+Z' 2 '-Y,1/2+X,1/2+Z' 3 '1/2-X,1/2-Y,+Z' 4 '1/2+Y,-X,1/2+Z' 5 '-X,-Y,-Z' 6 '+Y,1/2-X,1/2-Z' 7 '1/2+X,1/2+Y,-Z' 8 '1/2-Y,+X,1/2-Z' #------------------------------------------------------------------------------ _cell_length_a 21.370(2) _cell_length_b 21.370(2) _cell_length_c 7.4607(8) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 3407.2(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 28207 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 298 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1514.00 _exptl_absorpt_coefficient_mu 0.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.597 _exptl_absorpt_correction_T_max 0.940 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 298 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 29709 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3898 _reflns_number_gt 2190 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1232 _refine_ls_number_restraints ? _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 3898 _refine_ls_number_parameters 248 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0009Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 1.130 _refine_diff_density_min -0.905 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'K' 'K' 0.2009 0.2494 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.0033 0.0016 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Co' 'Co' 0.3494 0.9721 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Co(1) Co 0.0000 1.0000 1.0000 0.02704(14) Uani 1.0 4 d . . . K(1) K -0.2500 0.7500 0.7500 0.0945(7) Uani 1.0 2 d . . . O(1) O -0.1567(2) 0.8027(3) 0.9243(8) 0.167(2) Uani 1.0 8 d . . . N(1) N -0.00911(10) 1.06968(10) 0.8374(3) 0.0292(7) Uani 1.0 8 d . . . N(2) N 0.05864(11) 1.03627(10) 0.5953(4) 0.0330(7) Uani 1.0 8 d . . . N(3) N 0.05198(10) 0.95734(10) 0.8274(3) 0.0287(6) Uani 1.0 8 d . . . N(4) N 0.07328(11) 0.86082(10) 0.9848(4) 0.0335(7) Uani 1.0 8 d . . . N(5) N -0.11623(13) 0.92876(13) 0.8702(4) 0.0506(9) Uani 1.0 8 d . . . C(1) C 0.02112(12) 1.07647(13) 0.6767(4) 0.0305(8) Uani 1.0 8 d . . . C(2) C 0.07156(13) 0.98122(13) 0.6662(4) 0.0303(8) Uani 1.0 8 d . . . C(3) C 0.11313(12) 0.93696(13) 0.5780(4) 0.0309(8) Uani 1.0 8 d . . . C(4) C 0.14438(13) 0.93868(14) 0.4160(4) 0.0361(9) Uani 1.0 8 d . . . C(5) C 0.17946(15) 0.88683(15) 0.3698(5) 0.0459(10) Uani 1.0 8 d . . . C(6) C 0.18437(15) 0.83565(15) 0.4844(5) 0.0467(10) Uani 1.0 8 d . . . C(7) C 0.15391(14) 0.83404(14) 0.6466(5) 0.0392(9) Uani 1.0 8 d . . . C(8) C 0.11746(13) 0.88539(12) 0.6917(4) 0.0309(8) Uani 1.0 8 d . . . C(9) C 0.07913(12) 0.89986(12) 0.8482(4) 0.0303(8) Uani 1.0 8 d . . . C(10) C 0.03969(13) 0.87527(12) 1.1275(4) 0.0313(8) Uani 1.0 8 d . . . C(11) C 0.02798(13) 0.83082(13) 1.2722(4) 0.0330(8) Uani 1.0 8 d . . . C(12) C 0.04539(15) 0.76886(13) 1.2951(5) 0.0413(9) Uani 1.0 8 d . . . C(13) C 0.02270(17) 0.73844(14) 1.4459(5) 0.0501(10) Uani 1.0 8 d . . . C(14) C -0.01470(16) 0.76857(15) 1.5698(5) 0.0501(10) Uani 1.0 8 d . . . C(15) C -0.03217(15) 0.83148(14) 1.5484(5) 0.0426(9) Uani 1.0 8 d . . . C(16) C -0.01020(13) 0.86099(13) 1.3955(4) 0.0330(8) Uani 1.0 8 d . . . C(17) C -0.07312(14) 0.95701(13) 0.9104(4) 0.0334(8) Uani 1.0 8 d . . . C(18) C -0.1155(6) 0.7708(4) 1.0643(12) 0.211(5) Uani 1.0 8 d . . . C(19) C -0.1189(3) 0.7091(5) 1.036(3) 0.293(7) Uani 1.0 8 d . . . H(1) H 0.1413 0.9741 0.3394 0.0431(13) Uiso 1.0 8 calc R . . H(2) H 0.2014 0.8866 0.2591 0.0551(14) Uiso 1.0 8 calc R . . H(3) H 0.2087 0.8007 0.4483 0.0561(14) Uiso 1.0 8 calc R . . H(4) H 0.1577 0.7994 0.7258 0.0472(14) Uiso 1.0 8 calc R . . H(5) H 0.0720 0.7484 1.2115 0.0495(14) Uiso 1.0 8 calc R . . H(6) H 0.0332 0.6957 1.4644 0.0601(15) Uiso 1.0 8 calc R . . H(7) H -0.0288 0.7462 1.6722 0.0601(15) Uiso 1.0 8 calc R . . H(8) H -0.0580 0.8527 1.6325 0.0510(14) Uiso 1.0 8 calc R . . H(9) H -0.1244 0.7862 1.1810 0.2528 Uiso 1.0 8 calc R . . H(10) H -0.0737 0.7811 1.0329 0.2527 Uiso 1.0 8 calc R . . H(11) H -0.1609 0.6994 1.0049 0.351(10) Uiso 1.0 8 calc R . . H(12) H -0.1097 0.6924 1.1508 0.351(10) Uiso 1.0 8 calc R . . H(13) H -0.0914 0.6914 0.9496 0.351(10) Uiso 1.0 8 calc R . . H(14) H -0.1573 0.8488 0.9011 0.2003 Uiso 1.0 8 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co(1) 0.0292(3) 0.0256(3) 0.0263(3) 0.0027(3) 0.0039(3) 0.0039(3) K(1) 0.0811(9) 0.0811(9) 0.121(2) 0.0000 0.0000 0.0000 O(1) 0.183(3) 0.103(5) 0.215(5) -0.053(4) -0.041(4) 0.011(5) N(1) 0.0316(13) 0.0273(12) 0.0287(13) 0.0042(10) 0.0021(11) 0.0043(11) N(2) 0.0361(14) 0.0319(13) 0.0309(13) 0.0038(10) 0.0054(11) 0.0061(11) N(3) 0.0317(13) 0.0259(12) 0.0285(12) 0.0034(10) 0.0044(11) 0.0043(11) N(4) 0.0396(13) 0.0277(12) 0.0333(14) 0.0032(10) 0.0085(12) 0.0046(12) N(5) 0.0454(17) 0.0509(18) 0.056(2) -0.0061(14) -0.0001(15) -0.0032(15) C(1) 0.0301(15) 0.0302(15) 0.0312(15) -0.0006(12) 0.0014(13) 0.0049(13) C(2) 0.0283(15) 0.0328(16) 0.0300(15) -0.0003(12) 0.0037(13) 0.0010(13) C(3) 0.0283(15) 0.0326(15) 0.0319(15) 0.0032(12) -0.0007(13) 0.0022(13) C(4) 0.0353(16) 0.0386(17) 0.0345(17) 0.0054(13) 0.0074(14) 0.0058(15) C(5) 0.0449(19) 0.055(2) 0.0379(19) 0.0085(16) 0.0127(16) 0.0005(16) C(6) 0.0480(19) 0.0399(17) 0.052(2) 0.0138(14) 0.0169(17) -0.0004(17) C(7) 0.0427(18) 0.0315(16) 0.0434(19) 0.0049(14) 0.0088(15) 0.0034(15) C(8) 0.0301(15) 0.0290(15) 0.0336(16) -0.0001(12) 0.0025(13) 0.0013(13) C(9) 0.0324(15) 0.0262(14) 0.0322(16) 0.0025(12) 0.0049(13) 0.0019(13) C(10) 0.0351(16) 0.0272(15) 0.0316(16) 0.0018(12) 0.0014(13) 0.0062(13) C(11) 0.0360(16) 0.0311(15) 0.0320(16) 0.0025(12) 0.0012(14) 0.0057(13) C(12) 0.0536(19) 0.0295(16) 0.0410(18) 0.0082(14) 0.0097(16) 0.0053(14) C(13) 0.072(3) 0.0284(17) 0.050(2) 0.0088(16) 0.0098(18) 0.0129(16) C(14) 0.066(3) 0.0411(19) 0.0430(19) 0.0027(16) 0.0132(18) 0.0170(16) C(15) 0.0485(19) 0.0392(18) 0.0401(18) 0.0033(14) 0.0099(15) 0.0083(15) C(16) 0.0346(16) 0.0292(15) 0.0352(17) 0.0017(12) 0.0034(14) 0.0053(13) C(17) 0.0388(17) 0.0332(16) 0.0282(16) 0.0059(13) 0.0076(14) 0.0028(14) C(18) 0.173(12) 0.303(8) 0.156(8) 0.063(9) -0.116(8) -0.060(7) C(19) 0.201(5) 0.064(9) 0.61(3) 0.033(6) 0.095(9) 0.038(13) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _computing_structure_refinement 'CRYSTALS (Carruthers, et al., 1999)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Co(1) N(1) 1.931(3) yes . . Co(1) N(1) 1.931(3) yes . 5_577 Co(1) N(3) 1.929(3) yes . . Co(1) N(3) 1.929(3) yes . 5_577 Co(1) C(17) 1.932(3) yes . . Co(1) C(17) 1.932(3) yes . 5_577 K(1) O(1) 2.633(5) yes . . K(1) O(1) 2.633(5) yes . 3_465 K(1) O(1) 2.633(5) yes . 6_456 K(1) O(1) 2.633(5) yes . 8_566 O(1) C(18) 1.527(11) yes . . N(1) C(1) 1.369(4) yes . . N(1) C(10) 1.371(4) yes . 5_577 N(2) C(1) 1.323(4) yes . . N(2) C(2) 1.319(4) yes . . N(3) C(2) 1.372(4) yes . . N(3) C(9) 1.367(4) yes . . N(4) C(9) 1.323(4) yes . . N(4) C(10) 1.321(4) yes . . N(5) C(17) 1.142(4) yes . . C(1) C(16) 1.460(4) yes . 5_577 C(2) C(3) 1.455(4) yes . . C(3) C(4) 1.382(5) yes . . C(3) C(8) 1.394(4) yes . . C(4) C(5) 1.381(5) yes . . C(5) C(6) 1.392(5) yes . . C(6) C(7) 1.375(5) yes . . C(7) C(8) 1.387(4) yes . . C(8) C(9) 1.459(4) yes . . C(10) C(11) 1.459(4) yes . . C(11) C(12) 1.386(4) yes . . C(11) C(16) 1.389(4) yes . . C(12) C(13) 1.387(5) yes . . C(13) C(14) 1.381(5) yes . . C(14) C(15) 1.404(5) yes . . C(15) C(16) 1.385(5) yes . . C(18) C(19) 1.338(13) yes . . O(1) H(14) 1.000 no . . C(4) H(1) 0.950 no . . C(5) H(2) 0.950 no . . C(6) H(3) 0.950 no . . C(7) H(4) 0.950 no . . C(12) H(5) 0.950 no . . C(13) H(6) 0.950 no . . C(14) H(7) 0.950 no . . C(15) H(8) 0.950 no . . C(18) H(9) 0.950 no . . C(18) H(10) 0.950 no . . C(19) H(11) 0.950 no . . C(19) H(12) 0.950 no . . C(19) H(13) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(1) Co(1) N(1) 180.00(13) yes . . 5_577 N(1) Co(1) N(3) 90.18(10) yes . . . N(1) Co(1) N(3) 89.82(10) yes . . 5_577 N(1) Co(1) C(17) 93.89(11) yes . . . N(1) Co(1) C(17) 86.11(11) yes . . 5_577 N(1) Co(1) N(3) 89.82(10) yes 5_577 . . N(1) Co(1) N(3) 90.18(10) yes 5_577 . 5_577 N(1) Co(1) C(17) 86.11(11) yes 5_577 . . N(1) Co(1) C(17) 93.89(11) yes 5_577 . 5_577 N(3) Co(1) N(3) 180.00(13) yes . . 5_577 N(3) Co(1) C(17) 90.59(11) yes . . . N(3) Co(1) C(17) 89.41(11) yes . . 5_577 N(3) Co(1) C(17) 89.41(11) yes 5_577 . . N(3) Co(1) C(17) 90.59(11) yes 5_577 . 5_577 C(17) Co(1) C(17) 180.00(17) yes . . 5_577 O(1) K(1) O(1) 120.82(17) yes . . 3_465 O(1) K(1) O(1) 104.11(15) yes . . 6_456 O(1) K(1) O(1) 104.11(15) yes . . 8_566 O(1) K(1) O(1) 104.11(15) yes 3_465 . 6_456 O(1) K(1) O(1) 104.11(15) yes 3_465 . 8_566 O(1) K(1) O(1) 120.82(17) yes 6_456 . 8_566 K(1) O(1) C(18) 125.7(5) yes . . . Co(1) N(1) C(1) 125.75(18) yes . . . Co(1) N(1) C(10) 126.13(19) yes . . 5_577 C(1) N(1) C(10) 107.5(3) yes . . 5_577 C(1) N(2) C(2) 121.5(3) yes . . . Co(1) N(3) C(2) 125.80(18) yes . . . Co(1) N(3) C(9) 126.40(19) yes . . . C(2) N(3) C(9) 107.7(3) yes . . . C(9) N(4) C(10) 121.7(3) yes . . . N(1) C(1) N(2) 128.3(3) yes . . . N(1) C(1) C(16) 110.2(3) yes . . 5_577 N(2) C(1) C(16) 121.5(3) yes . . 5_577 N(2) C(2) N(3) 128.3(3) yes . . . N(2) C(2) C(3) 121.8(3) yes . . . N(3) C(2) C(3) 109.9(3) yes . . . C(2) C(3) C(4) 132.3(3) yes . . . C(2) C(3) C(8) 106.2(3) yes . . . C(4) C(3) C(8) 121.4(3) yes . . . C(3) C(4) C(5) 117.3(3) yes . . . C(4) C(5) C(6) 121.2(3) yes . . . C(5) C(6) C(7) 121.6(3) yes . . . C(6) C(7) C(8) 117.3(3) yes . . . C(3) C(8) C(7) 121.0(3) yes . . . C(3) C(8) C(9) 106.4(3) yes . . . C(7) C(8) C(9) 132.6(3) yes . . . N(3) C(9) N(4) 127.8(3) yes . . . N(3) C(9) C(8) 109.8(3) yes . . . N(4) C(9) C(8) 122.4(3) yes . . . N(1) C(10) N(4) 127.9(3) yes 5_577 . . N(1) C(10) C(11) 109.6(3) yes 5_577 . . N(4) C(10) C(11) 122.5(3) yes . . . C(10) C(11) C(12) 131.8(3) yes . . . C(10) C(11) C(16) 106.8(3) yes . . . C(12) C(11) C(16) 121.3(3) yes . . . C(11) C(12) C(13) 117.0(3) yes . . . C(12) C(13) C(14) 121.8(3) yes . . . C(13) C(14) C(15) 121.6(3) yes . . . C(14) C(15) C(16) 116.1(3) yes . . . C(1) C(16) C(11) 105.9(3) yes 5_577 . . C(1) C(16) C(15) 131.8(3) yes 5_577 . . C(11) C(16) C(15) 122.2(3) yes . . . Co(1) C(17) N(5) 174.3(3) yes . . . O(1) C(18) C(19) 107.5(9) yes . . . K(1) O(1) H(14) 109.113 no . . . C(18) O(1) H(14) 124.398 no . . . C(3) C(4) H(1) 120.945 no . . . C(5) C(4) H(1) 121.729 no . . . C(4) C(5) H(2) 119.206 no . . . C(6) C(5) H(2) 119.571 no . . . C(5) C(6) H(3) 119.027 no . . . C(7) C(6) H(3) 119.320 no . . . C(6) C(7) H(4) 121.772 no . . . C(8) C(7) H(4) 120.878 no . . . C(11) C(12) H(5) 121.254 no . . . C(13) C(12) H(5) 121.742 no . . . C(12) C(13) H(6) 119.040 no . . . C(14) C(13) H(6) 119.178 no . . . C(13) C(14) H(7) 119.134 no . . . C(15) C(14) H(7) 119.267 no . . . C(14) C(15) H(8) 122.401 no . . . C(16) C(15) H(8) 121.532 no . . . O(1) C(18) H(9) 110.905 no . . . O(1) C(18) H(10) 105.703 no . . . C(19) C(18) H(9) 118.507 no . . . C(19) C(18) H(10) 103.826 no . . . H(9) C(18) H(10) 109.465 no . . . C(18) C(19) H(11) 107.743 no . . . C(18) C(19) H(12) 102.476 no . . . C(18) C(19) H(13) 117.838 no . . . H(11) C(19) H(12) 109.480 no . . . H(11) C(19) H(13) 109.466 no . . . H(12) C(19) H(13) 109.472 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 N(1) Co(1) N(3) C(2) 4.20(17) no . . . . N(1) Co(1) N(3) C(9) 179.74(18) no . . . . N(3) Co(1) N(1) C(1) -5.76(18) no . . . . N(3) Co(1) N(1) C(10) -175.94(17) no . . . 5_577 N(1) Co(1) N(3) C(2) 175.80(17) no . . 5_577 5_577 N(1) Co(1) N(3) C(9) 0.26(18) no . . 5_577 5_577 N(3) Co(1) N(1) C(1) 174.24(18) no 5_577 . . . N(3) Co(1) N(1) C(10) 4.06(17) no 5_577 . . 5_577 C(17) Co(1) N(1) C(1) -96.36(18) no . . . . C(17) Co(1) N(1) C(10) 93.46(18) no . . . 5_577 C(17) Co(1) N(1) C(1) 83.64(18) no 5_577 . . . C(17) Co(1) N(1) C(10) -86.54(18) no 5_577 . . 5_577 N(1) Co(1) N(3) C(2) -175.80(17) no 5_577 . . . N(1) Co(1) N(3) C(9) -0.26(18) no 5_577 . . . N(3) Co(1) N(1) C(1) -174.24(18) no . . 5_577 5_577 N(3) Co(1) N(1) C(10) -4.06(17) no . . 5_577 . N(1) Co(1) N(3) C(2) -4.20(17) no 5_577 . 5_577 5_577 N(1) Co(1) N(3) C(9) -179.74(18) no 5_577 . 5_577 5_577 N(3) Co(1) N(1) C(1) 5.76(18) no 5_577 . 5_577 5_577 N(3) Co(1) N(1) C(10) 175.94(17) no 5_577 . 5_577 . C(17) Co(1) N(1) C(1) -83.64(18) no . . 5_577 5_577 C(17) Co(1) N(1) C(10) 86.54(18) no . . 5_577 . C(17) Co(1) N(1) C(1) 96.36(18) no 5_577 . 5_577 5_577 C(17) Co(1) N(1) C(10) -93.46(18) no 5_577 . 5_577 . C(17) Co(1) N(3) C(2) 98.10(18) no . . . . C(17) Co(1) N(3) C(9) -86.37(18) no . . . . C(17) Co(1) N(3) C(2) -81.90(18) no 5_577 . . . C(17) Co(1) N(3) C(9) 93.63(18) no 5_577 . . . C(17) Co(1) N(3) C(2) 81.90(18) no . . 5_577 5_577 C(17) Co(1) N(3) C(9) -93.63(18) no . . 5_577 5_577 C(17) Co(1) N(3) C(2) -98.10(18) no 5_577 . 5_577 5_577 C(17) Co(1) N(3) C(9) 86.37(18) no 5_577 . 5_577 5_577 O(1) K(1) O(1) C(18) 55.9(4) no . . 3_465 3_465 O(1) K(1) O(1) C(18) 55.9(4) no 3_465 . . . O(1) K(1) O(1) C(18) -172.2(3) no . . 6_456 6_456 O(1) K(1) O(1) C(18) -60.4(4) no 6_456 . . . O(1) K(1) O(1) C(18) 60.4(4) no . . 8_566 8_566 O(1) K(1) O(1) C(18) 172.2(3) no 8_566 . . . O(1) K(1) O(1) C(18) 60.4(4) no 3_465 . 6_456 6_456 O(1) K(1) O(1) C(18) 172.2(3) no 6_456 . 3_465 3_465 O(1) K(1) O(1) C(18) -172.2(3) no 3_465 . 8_566 8_566 O(1) K(1) O(1) C(18) -60.4(4) no 8_566 . 3_465 3_465 O(1) K(1) O(1) C(18) -55.9(4) no 6_456 . 8_566 8_566 O(1) K(1) O(1) C(18) -55.9(4) no 8_566 . 6_456 6_456 K(1) O(1) C(18) C(19) 22.4(9) no . . . . Co(1) N(1) C(1) N(2) 4.8(4) no . . . . Co(1) N(1) C(1) C(16) -171.18(14) no . . . 5_577 Co(1) N(1) C(10) N(4) -6.5(4) no . . 5_577 5_577 Co(1) N(1) C(10) C(11) 171.13(14) no . . 5_577 5_577 C(1) N(1) C(10) N(4) -178.2(3) no . . 5_577 5_577 C(1) N(1) C(10) C(11) -0.5(3) no . . 5_577 5_577 C(10) N(1) C(1) N(2) 176.5(3) no 5_577 . . . C(10) N(1) C(1) C(16) 0.5(3) no 5_577 . . 5_577 C(1) N(2) C(2) N(3) -2.1(5) no . . . . C(1) N(2) C(2) C(3) -179.5(3) no . . . . C(2) N(2) C(1) N(1) 0.2(5) no . . . . C(2) N(2) C(1) C(16) 175.7(3) no . . . 5_577 Co(1) N(3) C(2) N(2) -1.2(4) no . . . . Co(1) N(3) C(2) C(3) 176.49(14) no . . . . Co(1) N(3) C(9) N(4) 3.4(4) no . . . . Co(1) N(3) C(9) C(8) -177.03(14) no . . . . C(2) N(3) C(9) N(4) 179.6(3) no . . . . C(2) N(3) C(9) C(8) -0.8(3) no . . . . C(9) N(3) C(2) N(2) -177.4(3) no . . . . C(9) N(3) C(2) C(3) 0.3(3) no . . . . C(9) N(4) C(10) N(1) -3.0(5) no . . . 5_577 C(9) N(4) C(10) C(11) 174.3(3) no . . . . C(10) N(4) C(9) N(3) -2.2(5) no . . . . C(10) N(4) C(9) C(8) 178.3(3) no . . . . N(1) C(1) C(16) C(11) -0.3(3) no . . 5_577 5_577 N(1) C(1) C(16) C(15) 177.4(3) no . . 5_577 5_577 N(2) C(1) C(16) C(11) -176.6(3) no . . 5_577 5_577 N(2) C(1) C(16) C(15) 1.1(5) no . . 5_577 5_577 N(2) C(2) C(3) C(4) -2.5(5) no . . . . N(2) C(2) C(3) C(8) 178.3(3) no . . . . N(3) C(2) C(3) C(4) 179.6(3) no . . . . N(3) C(2) C(3) C(8) 0.4(3) no . . . . C(2) C(3) C(4) C(5) -178.2(3) no . . . . C(2) C(3) C(8) C(7) 179.9(3) no . . . . C(2) C(3) C(8) C(9) -0.9(3) no . . . . C(4) C(3) C(8) C(7) 0.6(4) no . . . . C(4) C(3) C(8) C(9) 179.8(3) no . . . . C(8) C(3) C(4) C(5) 0.9(4) no . . . . C(3) C(4) C(5) C(6) -1.7(5) no . . . . C(4) C(5) C(6) C(7) 1.0(5) no . . . . C(5) C(6) C(7) C(8) 0.5(5) no . . . . C(6) C(7) C(8) C(3) -1.3(5) no . . . . C(6) C(7) C(8) C(9) 179.7(3) no . . . . C(3) C(8) C(9) N(3) 1.1(3) no . . . . C(3) C(8) C(9) N(4) -179.3(3) no . . . . C(7) C(8) C(9) N(3) -179.8(3) no . . . . C(7) C(8) C(9) N(4) -0.2(5) no . . . . N(1) C(10) C(11) C(12) 176.3(3) no 5_577 . . . N(1) C(10) C(11) C(16) -0.3(3) no 5_577 . . . N(4) C(10) C(11) C(12) -1.5(5) no . . . . N(4) C(10) C(11) C(16) -178.1(3) no . . . . C(10) C(11) C(12) C(13) -175.9(3) no . . . . C(10) C(11) C(16) C(1) 0.0(3) no . . . 5_577 C(10) C(11) C(16) C(15) 178.0(3) no . . . . C(12) C(11) C(16) C(1) -177.1(3) no . . . 5_577 C(12) C(11) C(16) C(15) 0.9(5) no . . . . C(16) C(11) C(12) C(13) 0.3(5) no . . . . C(11) C(12) C(13) C(14) -1.1(5) no . . . . C(12) C(13) C(14) C(15) 0.6(5) no . . . . C(13) C(14) C(15) C(16) 0.6(5) no . . . . C(14) C(15) C(16) C(1) 176.0(3) no . . . 5_577 C(14) C(15) C(16) C(11) -1.4(5) no . . . . #============================================================================== data__Na-salt_______________ #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C76 H56 Co2 N20 Na O4 ' _chemical_formula_moiety 'C76 H56 Co2 N20 Na O4 ' _chemical_formula_weight 1454.27 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n' _symmetry_space_group_name_Hall '-P 4bc' _symmetry_Int_Tables_number 86 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 '+X,+Y,+Z' 2 '-Y,1/2+X,1/2+Z' 3 '1/2-X,1/2-Y,+Z' 4 '1/2+Y,-X,1/2+Z' 5 '-X,-Y,-Z' 6 '+Y,1/2-X,1/2-Z' 7 '1/2+X,1/2+Y,-Z' 8 '1/2-Y,+X,1/2-Z' #------------------------------------------------------------------------------ _cell_length_a 21.163(4) _cell_length_b 21.163(4) _cell_length_c 7.4140(13) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 3320.7(11) _cell_formula_units_Z 2 _cell_measurement_reflns_used 22734 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 273.1 #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1498.00 _exptl_absorpt_coefficient_mu 0.576 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.440 _exptl_absorpt_correction_T_max 0.891 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 273.1 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 28214 _diffrn_reflns_av_R_equivalents 0.140 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3815 _reflns_number_gt 1688 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.0939 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 1702 _refine_ls_number_parameters 248 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 1794.1400 2496.9800 892.1740 ; _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.44 _refine_diff_density_min -0.74 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Co' 'Co' 0.349 0.972 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Na' 'Na' 0.036 0.025 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Co(1) Co 0.5000 0.0000 0.5000 0.0186(2) Uani 1.00 2 d S . . Na(1) Na 0.2500 0.2500 0.2500 0.0629(13) Uani 1.00 4 d S . . O(1) O 0.3319(2) 0.2003(2) 0.4008(7) 0.0710(16) Uani 1.00 1 d . . . N(1) N 0.44105(17) 0.03725(17) 0.9093(5) 0.0219(10) Uani 1.00 1 d . . . N(2) N 0.50935(17) 0.07092(16) 0.6631(5) 0.0199(9) Uani 1.00 1 d . . . N(3) N 0.57325(17) 0.14123(16) 0.4823(6) 0.0229(9) Uani 1.00 1 d . . . N(4) N 0.55231(17) 0.04273(16) 0.3255(5) 0.0181(9) Uani 1.00 1 d . . . N(5) N 0.3834(2) 0.0743(2) 0.3725(5) 0.0295(12) Uani 1.00 1 d . . . C(1) C 0.3825(2) -0.1161(2) 0.8147(6) 0.0211(12) Uani 1.00 1 d . . . C(2) C 0.3462(2) -0.1679(2) 0.8602(6) 0.0257(12) Uani 1.00 1 d . . . C(3) C 0.3158(2) -0.1659(2) 1.0272(7) 0.0286(13) Uani 1.00 1 d . . . C(4) C 0.3207(2) -0.1141(2) 1.1421(6) 0.0270(13) Uani 1.00 1 d . . . C(5) C 0.3557(2) -0.0611(2) 1.0939(6) 0.0240(12) Uani 1.00 1 d . . . C(6) C 0.3869(2) -0.0642(2) 0.9283(6) 0.0224(11) Uani 1.00 1 d . . . C(7) C 0.4282(2) -0.0185(2) 0.8392(6) 0.0189(11) Uani 1.00 1 d . . . C(8) C 0.4783(2) 0.0782(2) 0.8256(7) 0.0209(12) Uani 1.00 1 d . . . C(9) C 0.4894(2) 0.1411(2) 0.8969(6) 0.0233(12) Uani 1.00 1 d . . . C(10) C 0.4669(2) 0.1713(2) 1.0504(6) 0.0281(13) Uani 1.00 1 d . . . C(11) C 0.4837(2) 0.2345(2) 1.0729(7) 0.0308(13) Uani 1.00 1 d . . . C(12) C 0.5219(2) 0.2653(2) 0.9436(7) 0.0328(14) Uani 1.00 1 d . . . C(13) C 0.5446(2) 0.2345(2) 0.7919(6) 0.0265(12) Uani 1.00 1 d . . . C(14) C 0.5273(2) 0.1722(2) 0.7704(6) 0.0222(11) Uani 1.00 1 d . . . C(15) C 0.5391(2) 0.1265(2) 0.6263(6) 0.0209(11) Uani 1.00 1 d . . . C(16) C 0.5790(2) 0.1015(2) 0.3439(6) 0.0219(12) Uani 1.00 1 d . . . C(17) C 0.4267(2) 0.0438(2) 0.4110(6) 0.0229(12) Uani 1.00 1 d . . . C(18) C 0.3707(5) 0.2899(4) 0.5667(18) 0.138(5) Uani 1.00 1 d . . . C(19) C 0.3784(3) 0.2222(3) 0.5304(12) 0.077(2) Uani 1.00 1 d . . . H(1) H 0.3420 -0.2030 0.7812 0.031 Uiso 1.00 1 c R . . H(2) H 0.2912 -0.2011 1.0642 0.034 Uiso 1.00 1 c R . . H(3) H 0.2996 -0.1149 1.2552 0.032 Uiso 1.00 1 c R . . H(4) H 0.3584 -0.0249 1.1692 0.029 Uiso 1.00 1 c R . . H(5) H 0.4414 0.1495 1.1354 0.034 Uiso 1.00 1 c R . . H(6) H 0.4696 0.2568 1.1765 0.037 Uiso 1.00 1 c R . . H(7) H 0.5320 0.3087 0.9608 0.039 Uiso 1.00 1 c R . . H(8) H 0.5709 0.2553 0.7067 0.032 Uiso 1.00 1 c R . . H(9) H 0.3275 0.3011 0.5518 0.166 Uiso 1.00 1 c R . . H(10) H 0.3956 0.3125 0.4818 0.166 Uiso 1.00 1 c R . . H(11) H 0.3839 0.3004 0.6854 0.166 Uiso 1.00 1 c R . . H(12) H 0.3733 0.2005 0.6417 0.092 Uiso 1.00 1 c R . . H(13) H 0.4194 0.2140 0.4837 0.092 Uiso 1.00 1 c R . . H(14) H 0.3370 0.1461 0.3779 0.085 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co(1) 0.0194(5) 0.0160(4) 0.0204(3) -0.0013(3) 0.0019(4) -0.0014(4) Na(1) 0.0530(19) 0.0530(19) 0.083(4) 0.0000 0.0000 0.0000 O(1) 0.066(3) 0.054(2) 0.094(3) 0.007(2) -0.015(3) -0.006(2) N(1) 0.0195(19) 0.0214(19) 0.025(2) -0.0040(15) 0.0010(17) -0.0030(17) N(2) 0.0191(19) 0.0167(18) 0.024(2) -0.0021(14) 0.0037(17) 0.0011(16) N(3) 0.0220(18) 0.0202(17) 0.026(2) -0.0006(13) -0.0021(19) -0.001(2) N(4) 0.0196(18) 0.0155(18) 0.019(2) -0.0010(14) 0.0039(16) -0.0043(16) N(5) 0.027(2) 0.033(2) 0.029(2) -0.0003(18) 0.001(2) 0.003(2) C(1) 0.019(2) 0.023(2) 0.022(2) 0.0006(17) -0.0012(19) 0.004(2) C(2) 0.024(2) 0.022(2) 0.031(2) -0.0003(19) 0.006(2) -0.002(2) C(3) 0.025(2) 0.023(2) 0.038(3) -0.0060(18) 0.008(2) 0.004(2) C(4) 0.027(2) 0.032(2) 0.023(2) -0.003(2) 0.007(2) 0.001(2) C(5) 0.024(2) 0.024(2) 0.024(2) -0.0017(19) -0.000(2) -0.002(2) C(6) 0.023(2) 0.023(2) 0.021(2) 0.0009(19) 0.002(2) 0.001(2) C(7) 0.015(2) 0.021(2) 0.021(2) 0.0024(17) 0.001(2) -0.001(2) C(8) 0.017(2) 0.020(2) 0.026(2) 0.0004(18) -0.002(2) -0.001(2) C(9) 0.026(2) 0.021(2) 0.023(2) 0.0012(18) -0.002(2) -0.001(2) C(10) 0.030(2) 0.027(2) 0.027(2) -0.004(2) 0.006(2) -0.006(2) C(11) 0.038(2) 0.026(2) 0.028(2) -0.002(2) 0.004(2) -0.010(2) C(12) 0.041(2) 0.023(2) 0.034(3) -0.005(2) 0.002(2) -0.007(2) C(13) 0.031(2) 0.021(2) 0.028(2) -0.004(2) 0.005(2) -0.004(2) C(14) 0.023(2) 0.021(2) 0.022(2) 0.0015(18) -0.001(2) 0.001(2) C(15) 0.016(2) 0.027(2) 0.020(2) -0.0003(18) 0.0012(19) 0.000(2) C(16) 0.021(2) 0.022(2) 0.022(2) 0.0025(18) 0.002(2) -0.004(2) C(17) 0.026(2) 0.018(2) 0.025(2) -0.0059(19) 0.003(2) -0.001(2) C(18) 0.145(10) 0.072(6) 0.199(14) 0.005(6) -0.053(9) -0.045(7) C(19) 0.077(5) 0.068(4) 0.085(6) -0.012(4) -0.012(5) 0.005(4) #============================================================================== _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SIR92' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Co(1) N(2) 1.937(3) yes . . Co(1) N(2) 1.937(3) yes . 5_656 Co(1) N(4) 1.928(3) yes . . Co(1) N(4) 1.928(3) yes . 5_656 Co(1) C(17) 1.924(4) yes . . Co(1) C(17) 1.924(4) yes . 5_656 Na(1) O(1) 2.315(5) yes . . Na(1) O(1) 2.315(5) yes . 3_555 Na(1) O(1) 2.315(4) yes . 6_555 Na(1) O(1) 2.315(4) yes . 8_555 O(1) C(19) 1.451(10) yes . . N(1) C(7) 1.317(5) yes . . N(1) C(8) 1.325(5) yes . . N(2) C(8) 1.381(6) yes . . N(2) C(15) 1.362(5) yes . . N(3) C(15) 1.326(6) yes . . N(3) C(16) 1.333(6) yes . . N(4) C(7) 1.388(6) yes . 5_656 N(4) C(16) 1.373(5) yes . . N(5) C(17) 1.157(6) yes . . C(1) C(2) 1.381(6) yes . . C(1) C(6) 1.386(6) yes . . C(1) C(16) 1.462(6) yes . 5_656 C(2) C(3) 1.396(7) yes . . C(3) C(4) 1.393(7) yes . . C(4) C(5) 1.389(6) yes . . C(5) C(6) 1.395(6) yes . . C(6) C(7) 1.462(6) yes . . C(8) C(9) 1.451(6) yes . . C(9) C(10) 1.389(6) yes . . C(9) C(14) 1.399(6) yes . . C(10) C(11) 1.394(6) yes . . C(11) C(12) 1.414(7) yes . . C(12) C(13) 1.386(7) yes . . C(13) C(14) 1.379(6) yes . . C(14) C(15) 1.463(6) yes . . C(18) C(19) 1.468(12) yes . . O(1) H(14) 1.165 no . . C(2) H(1) 0.950 no . . C(3) H(2) 0.950 no . . C(4) H(3) 0.950 no . . C(5) H(4) 0.950 no . . C(10) H(5) 0.950 no . . C(11) H(6) 0.950 no . . C(12) H(7) 0.950 no . . C(13) H(8) 0.950 no . . C(18) H(9) 0.950 no . . C(18) H(10) 0.950 no . . C(18) H(11) 0.950 no . . C(19) H(12) 0.950 no . . C(19) H(13) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(2) Co(1) N(2) 180.0(2) yes . . 5_656 N(2) Co(1) N(4) 89.81(15) yes . . . N(2) Co(1) N(4) 90.19(15) yes . . 5_656 N(2) Co(1) C(17) 85.58(17) yes . . . N(2) Co(1) C(17) 94.42(17) yes . . 5_656 N(2) Co(1) N(4) 90.19(15) yes 5_656 . . N(2) Co(1) N(4) 89.81(15) yes 5_656 . 5_656 N(2) Co(1) C(17) 94.42(17) yes 5_656 . . N(2) Co(1) C(17) 85.58(17) yes 5_656 . 5_656 N(4) Co(1) N(4) 180.0(2) yes . . 5_656 N(4) Co(1) C(17) 90.38(17) yes . . . N(4) Co(1) C(17) 89.62(17) yes . . 5_656 N(4) Co(1) C(17) 89.62(17) yes 5_656 . . N(4) Co(1) C(17) 90.38(17) yes 5_656 . 5_656 C(17) Co(1) C(17) 180.0(2) yes . . 5_656 O(1) Na(1) O(1) 122.24(19) yes . . 3_555 O(1) Na(1) O(1) 103.49(17) yes . . 6_555 O(1) Na(1) O(1) 103.49(17) yes . . 8_555 O(1) Na(1) O(1) 103.49(17) yes 3_555 . 6_555 O(1) Na(1) O(1) 103.49(17) yes 3_555 . 8_555 O(1) Na(1) O(1) 122.24(19) yes 6_555 . 8_555 Na(1) O(1) C(19) 133.1(4) yes . . . C(7) N(1) C(8) 121.5(4) yes . . . Co(1) N(2) C(8) 125.6(2) yes . . . Co(1) N(2) C(15) 126.2(3) yes . . . C(8) N(2) C(15) 107.4(3) yes . . . C(15) N(3) C(16) 121.4(3) yes . . . Co(1) N(4) C(7) 126.0(2) yes . . 5_656 Co(1) N(4) C(16) 126.5(3) yes . . . C(7) N(4) C(16) 107.5(3) yes 5_656 . . C(2) C(1) C(6) 121.1(4) yes . . . C(2) C(1) C(16) 132.3(4) yes . . 5_656 C(6) C(1) C(16) 106.5(3) yes . . 5_656 C(1) C(2) C(3) 116.7(4) yes . . . C(2) C(3) C(4) 122.1(4) yes . . . C(3) C(4) C(5) 121.1(4) yes . . . C(4) C(5) C(6) 116.2(4) yes . . . C(1) C(6) C(5) 122.7(4) yes . . . C(1) C(6) C(7) 106.8(4) yes . . . C(5) C(6) C(7) 130.5(4) yes . . . N(1) C(7) N(4) 128.1(4) yes . . 5_656 N(1) C(7) C(6) 122.5(4) yes . . . N(4) C(7) C(6) 109.3(3) yes 5_656 . . N(1) C(8) N(2) 128.2(4) yes . . . N(1) C(8) C(9) 121.6(4) yes . . . N(2) C(8) C(9) 110.1(3) yes . . . C(8) C(9) C(10) 131.7(4) yes . . . C(8) C(9) C(14) 106.2(4) yes . . . C(10) C(9) C(14) 121.9(4) yes . . . C(9) C(10) C(11) 116.9(4) yes . . . C(10) C(11) C(12) 120.5(4) yes . . . C(11) C(12) C(13) 122.1(4) yes . . . C(12) C(13) C(14) 116.9(4) yes . . . C(9) C(14) C(13) 121.7(4) yes . . . C(9) C(14) C(15) 106.1(3) yes . . . C(13) C(14) C(15) 132.2(4) yes . . . N(2) C(15) N(3) 128.1(4) yes . . . N(2) C(15) C(14) 110.2(3) yes . . . N(3) C(15) C(14) 121.7(3) yes . . . N(3) C(16) N(4) 127.6(4) yes . . . N(3) C(16) C(1) 122.5(4) yes . . 5_656 N(4) C(16) C(1) 109.9(4) yes . . 5_656 Co(1) C(17) N(5) 172.9(4) yes . . . O(1) C(19) C(18) 110.9(7) yes . . . Na(1) O(1) H(14) 116.5 no . . . C(19) O(1) H(14) 110.3 no . . . C(1) C(2) H(1) 121.5 no . . . C(3) C(2) H(1) 121.8 no . . . C(2) C(3) H(2) 119.0 no . . . C(4) C(3) H(2) 118.9 no . . . C(3) C(4) H(3) 119.3 no . . . C(5) C(4) H(3) 119.5 no . . . C(4) C(5) H(4) 122.1 no . . . C(6) C(5) H(4) 121.7 no . . . C(9) C(10) H(5) 121.0 no . . . C(11) C(10) H(5) 122.1 no . . . C(10) C(11) H(6) 119.7 no . . . C(12) C(11) H(6) 119.8 no . . . C(11) C(12) H(7) 118.9 no . . . C(13) C(12) H(7) 119.0 no . . . C(12) C(13) H(8) 121.6 no . . . C(14) C(13) H(8) 121.5 no . . . C(19) C(18) H(9) 109.1 no . . . C(19) C(18) H(10) 107.9 no . . . C(19) C(18) H(11) 111.4 no . . . H(9) C(18) H(10) 109.5 no . . . H(9) C(18) H(11) 109.5 no . . . H(10) C(18) H(11) 109.5 no . . . O(1) C(19) H(12) 110.2 no . . . O(1) C(19) H(13) 108.6 no . . . C(18) C(19) H(12) 107.4 no . . . C(18) C(19) H(13) 110.2 no . . . H(12) C(19) H(13) 109.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 N(2) Co(1) N(4) C(16) -0.9(3) ? . . . . N(2) Co(1) N(4) C(7) 176.4(3) ? . . . 5_656 N(4) Co(1) N(2) C(8) 173.8(3) ? . . . . N(4) Co(1) N(2) C(15) 5.1(3) ? . . . . N(2) Co(1) N(4) C(16) -179.1(3) ? . . 5_656 5_656 N(2) Co(1) N(4) C(7) 3.6(3) ? . . 5_656 . N(4) Co(1) N(2) C(8) -6.2(3) ? 5_656 . . . N(4) Co(1) N(2) C(15) -174.9(3) ? 5_656 . . . N(2) Co(1) C(17) N(5) -10(3) ? . . . . C(17) Co(1) N(2) C(8) 83.4(3) ? . . . . C(17) Co(1) N(2) C(15) -85.3(3) ? . . . . N(2) Co(1) C(17) N(5) -170(3) ? . . 5_656 5_656 C(17) Co(1) N(2) C(8) -96.6(3) ? 5_656 . . . C(17) Co(1) N(2) C(15) 94.7(3) ? 5_656 . . . N(2) Co(1) N(4) C(16) 179.1(3) ? 5_656 . . . N(2) Co(1) N(4) C(7) -3.6(3) ? 5_656 . . 5_656 N(4) Co(1) N(2) C(8) 6.2(3) ? . . 5_656 5_656 N(4) Co(1) N(2) C(15) 174.9(3) ? . . 5_656 5_656 N(2) Co(1) N(4) C(16) 0.9(3) ? 5_656 . 5_656 5_656 N(2) Co(1) N(4) C(7) -176.4(3) ? 5_656 . 5_656 . N(4) Co(1) N(2) C(8) -173.8(3) ? 5_656 . 5_656 5_656 N(4) Co(1) N(2) C(15) -5.1(3) ? 5_656 . 5_656 5_656 N(2) Co(1) C(17) N(5) 170(3) ? 5_656 . . . C(17) Co(1) N(2) C(8) 96.6(3) ? . . 5_656 5_656 C(17) Co(1) N(2) C(15) -94.7(3) ? . . 5_656 5_656 N(2) Co(1) C(17) N(5) 10(3) ? 5_656 . 5_656 5_656 C(17) Co(1) N(2) C(8) -83.4(3) ? 5_656 . 5_656 5_656 C(17) Co(1) N(2) C(15) 85.3(3) ? 5_656 . 5_656 5_656 N(4) Co(1) C(17) N(5) -100(3) ? . . . . C(17) Co(1) N(4) C(16) 84.7(3) ? . . . . C(17) Co(1) N(4) C(7) -98.0(3) ? . . . 5_656 N(4) Co(1) C(17) N(5) -80(3) ? . . 5_656 5_656 C(17) Co(1) N(4) C(16) -95.3(3) ? 5_656 . . . C(17) Co(1) N(4) C(7) 82.0(3) ? 5_656 . . 5_656 N(4) Co(1) C(17) N(5) 80(3) ? 5_656 . . . C(17) Co(1) N(4) C(16) 95.3(3) ? . . 5_656 5_656 C(17) Co(1) N(4) C(7) -82.0(3) ? . . 5_656 . N(4) Co(1) C(17) N(5) 100(3) ? 5_656 . 5_656 5_656 C(17) Co(1) N(4) C(16) -84.7(3) ? 5_656 . 5_656 5_656 C(17) Co(1) N(4) C(7) 98.0(3) ? 5_656 . 5_656 . O(1) Na(1) O(1) C(19) -58.7(6) ? . . 3_555 3_555 O(1) Na(1) O(1) C(19) -58.7(6) ? 3_555 . . . O(1) Na(1) O(1) C(19) -57.1(6) ? . . 6_555 6_555 O(1) Na(1) O(1) C(19) -174.4(6) ? 6_555 . . . O(1) Na(1) O(1) C(19) 174.4(6) ? . . 8_555 8_555 O(1) Na(1) O(1) C(19) 57.1(6) ? 8_555 . . . O(1) Na(1) O(1) C(19) 174.4(6) ? 3_555 . 6_555 6_555 O(1) Na(1) O(1) C(19) 57.1(6) ? 6_555 . 3_555 3_555 O(1) Na(1) O(1) C(19) -57.1(6) ? 3_555 . 8_555 8_555 O(1) Na(1) O(1) C(19) -174.4(6) ? 8_555 . 3_555 3_555 O(1) Na(1) O(1) C(19) 58.7(6) ? 6_555 . 8_555 8_555 O(1) Na(1) O(1) C(19) 58.7(6) ? 8_555 . 6_555 6_555 Na(1) O(1) C(19) C(18) -1.2(10) ? . . . . C(7) N(1) C(8) N(2) -1.1(7) ? . . . . C(7) N(1) C(8) C(9) 176.1(4) ? . . . . C(8) N(1) C(7) C(6) -179.5(4) ? . . . . C(8) N(1) C(7) N(4) -2.1(7) ? . . . 5_656 Co(1) N(2) C(8) N(1) 6.3(6) ? . . . . Co(1) N(2) C(8) C(9) -171.1(3) ? . . . . Co(1) N(2) C(15) N(3) -7.9(6) ? . . . . Co(1) N(2) C(15) C(14) 170.4(2) ? . . . . C(8) N(2) C(15) N(3) -178.3(4) ? . . . . C(8) N(2) C(15) C(14) 0.1(3) ? . . . . C(15) N(2) C(8) N(1) 176.7(4) ? . . . . C(15) N(2) C(8) C(9) -0.7(5) ? . . . . C(15) N(3) C(16) N(4) 0.7(7) ? . . . . C(15) N(3) C(16) C(1) -178.7(4) ? . . . 5_656 C(16) N(3) C(15) N(2) 4.4(7) ? . . . . C(16) N(3) C(15) C(14) -173.7(4) ? . . . . Co(1) N(4) C(7) N(1) 0.2(6) ? . . 5_656 5_656 Co(1) N(4) C(7) C(6) -177.5(2) ? . . 5_656 5_656 Co(1) N(4) C(16) N(3) -1.7(6) ? . . . . Co(1) N(4) C(16) C(1) 177.7(2) ? . . . 5_656 C(7) N(4) C(16) N(3) -179.4(4) ? 5_656 . . . C(7) N(4) C(16) C(1) -0.0(4) ? 5_656 . . 5_656 C(16) N(4) C(7) N(1) 177.9(4) ? . . 5_656 5_656 C(16) N(4) C(7) C(6) 0.3(4) ? . . 5_656 5_656 C(2) C(1) C(6) C(5) 0.5(7) ? . . . . C(2) C(1) C(6) C(7) -179.6(4) ? . . . . C(6) C(1) C(2) C(3) -1.7(6) ? . . . . C(2) C(1) C(16) N(3) -0.2(6) ? . . 5_656 5_656 C(2) C(1) C(16) N(4) 179.3(4) ? . . 5_656 5_656 C(16) C(1) C(2) C(3) 179.4(4) ? 5_656 . . . C(6) C(1) C(16) N(3) -179.2(4) ? . . 5_656 5_656 C(6) C(1) C(16) N(4) 0.2(5) ? . . 5_656 5_656 C(16) C(1) C(6) C(5) 179.7(4) ? 5_656 . . . C(16) C(1) C(6) C(7) -0.4(5) ? 5_656 . . . C(1) C(2) C(3) C(4) 1.0(6) ? . . . . C(2) C(3) C(4) C(5) 0.9(7) ? . . . . C(3) C(4) C(5) C(6) -2.1(6) ? . . . . C(4) C(5) C(6) C(1) 1.4(6) ? . . . . C(4) C(5) C(6) C(7) -178.5(4) ? . . . . C(1) C(6) C(7) N(1) 178.2(4) ? . . . . C(1) C(6) C(7) N(4) 0.4(5) ? . . . 5_656 C(5) C(6) C(7) N(1) -1.8(7) ? . . . . C(5) C(6) C(7) N(4) -179.6(4) ? . . . 5_656 N(1) C(8) C(9) C(10) -0.2(6) ? . . . . N(1) C(8) C(9) C(14) -176.6(4) ? . . . . N(2) C(8) C(9) C(10) 177.4(4) ? . . . . N(2) C(8) C(9) C(14) 1.1(5) ? . . . . C(8) C(9) C(10) C(11) -175.5(4) ? . . . . C(8) C(9) C(14) C(13) 177.0(4) ? . . . . C(8) C(9) C(14) C(15) -1.0(4) ? . . . . C(10) C(9) C(14) C(13) 0.2(6) ? . . . . C(10) C(9) C(14) C(15) -177.7(4) ? . . . . C(14) C(9) C(10) C(11) 0.3(6) ? . . . . C(9) C(10) C(11) C(12) -0.1(6) ? . . . . C(10) C(11) C(12) C(13) -0.7(8) ? . . . . C(11) C(12) C(13) C(14) 1.2(7) ? . . . . C(12) C(13) C(14) C(9) -0.9(7) ? . . . . C(12) C(13) C(14) C(15) 176.4(4) ? . . . . C(9) C(14) C(15) N(2) 0.6(5) ? . . . . C(9) C(14) C(15) N(3) 179.1(4) ? . . . . C(13) C(14) C(15) N(2) -177.0(4) ? . . . . C(13) C(14) C(15) N(3) 1.4(7) ? . . . . #============================================================================== # End of CIF #==============================================================================