#============================================================================= data_global #============================================================================= # 1. SUBMISSION DETAILS _publ_contact_author_name 'Daniel B. Leznoff' _publ_contact_author_address ; Department of Chemistry Simon Fraser University 8888 University Drive Burnaby BC Canada V5A 1S6 ; _publ_contact_author_phone '+1-778-782-4887' _publ_contact_author_fax '+1-778-782-3768' _publ_contact_author_email 'dleznoff@sfu.ca' _publ_requested_journal 'Dalton' #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _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_coeditor_notes ; ? ; _journal_techeditor_code ? _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 ; Vapochromic behaviour of M[Au(CN)2]2-based coordination polymers (M = Co, Ni) ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Lefebvre, Julie' ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; 'Korcok, Jasmine L.' ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; 'Katz, Michael J.' ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; 'Leznoff, Daniel B.' ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; #============================================================================== # 4. TEXT _publ_section_abstract ; ? #Insert appropriate text here if wanted. ; _publ_section_comment ; ? #Insert appropriate text here if wanted. ; _publ_section_experimental ; ? #Insert appropriate text here if wanted. ; ## -------------------REFERENCES ----------------------## _publ_section_references ; Gabe, E.J.; White, P.S.; Enright, G.D. DIFRAC A Fortran 77 Control Routine for 4-Circle Diffractometers, N.R.C., Ottawa, 1995. Gabe, E.J., Le Page, Y., Charland,.J.-P., Lee, F.L. and White, P.S. (1989) J. Appl. Cryst., 22, 384-387. International Tables for X-ray Crystallography, Vol. IV, (1974) Kynoch Press, Birmingham, England. Johnson, C.K., (1976) ORTEP - A Fortran Thermal Ellipsoid Plot Program, Technical Report ORNL-5138, Oak Ridge National Lab., U.S.A. Le Page, Y., (1988) J. Appl. Cryst., 21, 983-984. Le Page, Y. and Gabe, E.J., (1979) J. Appl. Cryst., 12, 464-466. # CRYSTALS # Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. # Extinction correction # Larson, A.C. (1970), Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294 #CAMERON # Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. #ORTEP-3 version 1.073 # Farrugia, L.J., (1997) J. Appl. Cryst. 30, 565. # SIR92 # Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 # SHELXS 86 # Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. ? #Insert any other references here ; _publ_section_figure_captions ; ? #Insert figure captions here if wanted ; _publ_section_acknowledgements ; ? #Insert any acknowledgements here. ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_Zn[Au(CN)2]2(DMSO)2 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C8 H12 Au2 N4 O2 S2 Zn1' _chemical_formula_moiety 'C8 H12 Au2 N4 O2 S2 Zn1' _chemical_formula_weight 719.66 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' #------------------------------------------------ _cell_length_a 7.8403(11) _cell_length_b 12.8395(12) _cell_length_c 16.4572(17) _cell_angle_alpha 90 _cell_angle_beta 98.891(10) _cell_angle_gamma 90 _cell_volume 1636.8(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 43 _cell_measurement_theta_min 23.5 _cell_measurement_theta_max 25.5 _cell_measurement_temperature 293 _exptl_crystal_description 'chunk' _exptl_crystal_colour 'colourless' _exptl_crystal_size_min 0.14 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_max 0.42 _exptl_crystal_density_diffrn 2.920 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 19.592 _exptl_absorpt_correction_type 'Psi-scan' _exptl_absorpt_correction_T_min 0.073 _exptl_absorpt_correction_T_max 0.262 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Enraf-Nonius CAD4F Diffractometer' _diffrn_radiation_monochromator grphite _diffrn_measurement_method \w/2\q _diffrn_ambient_temperature 293 _diffrn_reflns_number 5010 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min 2.021 _diffrn_reflns_theta_max 30.064 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.064 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_standards_interval_time 100 _diffrn_standards_interval_count 60 _diffrn_standards_number 2 _diffrn_standards_decay_% 2.381 #========================================================================== # 8. REFINEMENT DATA # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_number_total 4801 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 2953 _refine_ls_number_restraints 0 _refine_ls_number_parameters 177 _oxford_refine_ls_R_factor_ref 0.0342 _refine_ls_wR_factor_ref 0.0396 _refine_ls_goodness_of_fit_ref 1.5426 _refine_ls_shift/su_max 0.001292 # The values computed from all data _oxford_reflns_number_all 4801 _refine_ls_R_factor_all 0.0849 _refine_ls_wR_factor_all 0.0430 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3040 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_gt 0.0401 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 0.00P] ,where P=p(6)*max(Fo^2^,0) + (1-p(6))Fc^2^ ; _refine_diff_density_max 2.09 _refine_diff_density_min -1.52 _reflns_limit_h_min -11 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_refine_ls_scale 0.9367(17) _oxford_diffrn_Wilson_B_factor 2.89 _oxford_diffrn_Wilson_scale 1.32 # Number of reflections with Friedels Law is 4801 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4802 #--------------------------------------------------------- _chemical_name_systematic ; ; # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment constr # none if no extinction, _refine_ls_extinction_method 'Larson (1970), Equation 22' # Extinction coefficient _refine_ls_extinction_coef 16.0(15) #========================================================== # 9. General computing _computing_data_collection 'NRC DIFRAC' _computing_data_reduction 'NRC DIFRAC' _computing_cell_refinement 'NRC DIFRAC' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'Ortep/CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Au -2.0133 8.8022 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956 12.0658 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' #============================================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Au1 Au 2.10662(5) 0.78728(3) 0.66625(2) 0.0408 1.0000 Uani . . . . . . . Au2 Au 1.97927(5) 0.98541(3) 0.23055(2) 0.0447 1.0000 Uani . . . . . . . Zn1 Zn 1.63548(13) 0.74399(8) 0.40261(5) 0.0272 1.0000 Uani . . . . . . . S1 S 1.3400(3) 0.92498(19) 0.38442(14) 0.0387 1.0000 Uani . . . . . . . S2 S 1.4014(3) 0.66469(19) 0.53399(14) 0.0381 1.0000 Uani . . . . . . . O1 O 1.4898(9) 0.8707(5) 0.4379(4) 0.0384 1.0000 Uani . . . . . . . O2 O 1.5259(9) 0.6386(5) 0.4749(4) 0.0423 1.0000 Uani . . . . . . . N1 N 1.8198(10) 0.7738(6) 0.5121(4) 0.0385 1.0000 Uani . . . . . . . N2 N 2.4263(11) 0.7892(7) 0.8038(4) 0.0411 1.0000 Uani . . . . . . . N3 N 1.7592(12) 0.8519(7) 0.3316(5) 0.0481 1.0000 Uani . . . . . . . N4 N 2.2114(10) 1.1262(6) 0.1380(5) 0.0398 1.0000 Uani . . . . . . . C1 C 1.9215(12) 0.7785(7) 0.5701(5) 0.0385 1.0000 Uani . . . . . . . C2 C 2.3078(13) 0.7924(7) 0.7558(5) 0.0379 1.0000 Uani . . . . . . . C3 C 1.8354(13) 0.9002(9) 0.2939(6) 0.0468 1.0000 Uani . . . . . . . C4 C 2.1244(12) 1.0752(8) 0.1712(5) 0.0398 1.0000 Uani . . . . . . . C5 C 1.1952(14) 0.9591(9) 0.4544(7) 0.0578 1.0000 Uani . . . . . . 3 C6 C 1.4160(15) 1.0522(8) 0.3670(6) 0.0504 1.0000 Uani . . . . . . 3 C7 C 1.2193(14) 0.5868(10) 0.5007(7) 0.0590 1.0000 Uani . . . . . . 3 C8 C 1.4841(16) 0.5978(9) 0.6254(6) 0.0548 1.0000 Uani . . . . . . 3 H51 H 1.1416 0.8978 0.4705 0.07(2) 1.0000 Uiso R . . . . . . H52 H 1.2576 0.9919 0.5015 0.07(2) 1.0000 Uiso R . . . . . . H53 H 1.1094 1.0054 0.4281 0.07(2) 1.0000 Uiso R . . . . . . H61 H 1.4973 1.0484 0.3299 0.06(2) 1.0000 Uiso R . . . . . . H62 H 1.4698 1.0814 0.4176 0.06(2) 1.0000 Uiso R . . . . . . H63 H 1.3216 1.0948 0.3441 0.06(2) 1.0000 Uiso R . . . . . . H71 H 1.1597 0.6139 0.4504 0.10(3) 1.0000 Uiso R . . . . . . H72 H 1.1448 0.5874 0.5411 0.10(3) 1.0000 Uiso R . . . . . . H73 H 1.2548 0.5174 0.4924 0.10(3) 1.0000 Uiso R . . . . . . H81 H 1.5859 0.6318 0.6511 0.09(2) 1.0000 Uiso R . . . . . . H82 H 1.4006 0.5979 0.6616 0.09(2) 1.0000 Uiso R . . . . . . H83 H 1.5106 0.5279 0.6129 0.09(2) 1.0000 Uiso 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0309(2) 0.0524(3) 0.03498(18) -0.00166(17) -0.00746(14) 0.00710(19) Au2 0.0325(2) 0.0605(3) 0.0411(2) 0.01385(18) 0.00597(15) -0.01314(19) Zn1 0.0219(5) 0.0322(5) 0.0270(4) 0.0008(4) 0.0020(4) 0.0001(4) S1 0.0348(13) 0.0358(13) 0.0418(12) -0.0034(10) -0.0060(10) 0.0065(11) S2 0.0407(14) 0.0359(13) 0.0401(12) 0.0027(10) 0.0140(10) 0.0057(11) O1 0.037(4) 0.033(4) 0.043(3) 0.001(3) 0.001(3) 0.008(3) O2 0.045(4) 0.042(4) 0.045(4) 0.004(3) 0.023(3) 0.001(3) N1 0.031(4) 0.043(5) 0.039(4) 0.001(3) -0.003(3) 0.003(4) N2 0.034(4) 0.052(5) 0.036(4) 0.006(4) -0.001(3) 0.000(4) N3 0.051(6) 0.052(5) 0.042(4) 0.008(4) 0.009(4) -0.012(5) N4 0.036(5) 0.045(5) 0.040(4) 0.009(4) 0.010(4) -0.003(4) C1 0.029(5) 0.042(6) 0.040(5) 0.000(4) -0.009(4) 0.006(4) C2 0.040(6) 0.036(5) 0.035(4) 0.002(4) -0.006(4) 0.007(5) C3 0.031(5) 0.069(7) 0.040(5) 0.013(5) 0.004(4) -0.014(5) C4 0.030(5) 0.050(6) 0.037(5) 0.003(4) -0.001(4) -0.008(5) C5 0.040(6) 0.062(8) 0.075(8) 0.005(6) 0.019(6) 0.004(6) C6 0.056(7) 0.046(6) 0.047(6) 0.012(5) 0.003(5) 0.001(6) C7 0.040(6) 0.077(9) 0.058(6) 0.004(6) -0.001(5) -0.003(6) C8 0.065(8) 0.059(7) 0.040(5) -0.004(5) 0.007(5) 0.000(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Au1 . Au2 2_976 3.4942(6) yes Au1 . C1 . 1.978(8) yes Au1 . C2 . 1.986(9) yes Au2 . C3 . 1.980(10) yes Au2 . C4 . 1.980(10) yes Zn1 . N2 4_464 2.166(8) yes Zn1 . N4 3_945 2.104(8) yes Zn1 . O1 . 2.120(6) yes Zn1 . O2 . 2.074(6) yes Zn1 . N1 . 2.163(7) yes Zn1 . N3 . 2.139(8) yes S1 . O1 . 1.523(6) yes S1 . C5 . 1.792(10) yes S1 . C6 . 1.777(10) yes S2 . O2 . 1.518(6) yes S2 . C7 . 1.760(11) yes S2 . C8 . 1.767(10) yes N1 . C1 . 1.147(11) yes N2 . C2 . 1.123(11) yes N3 . C3 . 1.114(11) yes N4 . C4 . 1.143(11) yes C5 . H51 . 0.950 no C5 . H52 . 0.950 no C5 . H53 . 0.950 no C6 . H61 . 0.950 no C6 . H62 . 0.950 no C6 . H63 . 0.950 no C7 . H71 . 0.950 no C7 . H72 . 0.950 no C7 . H73 . 0.950 no C8 . H81 . 0.950 no C8 . H82 . 0.950 no C8 . H83 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Au2 2_976 Au1 . C1 . 105.3(3) yes Au2 2_976 Au1 . C2 . 78.6(3) yes C1 . Au1 . C2 . 174.7(4) yes Au1 2_976 Au2 . C3 . 92.2(3) yes Au1 2_976 Au2 . C4 . 85.5(3) yes C3 . Au2 . C4 . 177.5(4) yes N2 4_464 Zn1 . N4 3_945 91.3(3) yes N2 4_464 Zn1 . O1 . 88.8(3) yes N4 3_945 Zn1 . O1 . 175.7(3) yes N2 4_464 Zn1 . O2 . 88.3(3) yes N4 3_945 Zn1 . O2 . 91.2(3) yes O1 . Zn1 . O2 . 93.2(3) yes N2 4_464 Zn1 . N1 . 172.5(3) yes N4 3_945 Zn1 . N1 . 92.9(3) yes O1 . Zn1 . N1 . 87.4(3) yes O2 . Zn1 . N1 . 85.4(3) yes N2 4_464 Zn1 . N3 . 94.1(3) yes N4 3_945 Zn1 . N3 . 87.9(3) yes O1 . Zn1 . N3 . 87.8(3) yes O2 . Zn1 . N3 . 177.4(3) yes N1 . Zn1 . N3 . 92.3(3) yes O1 . S1 . C5 . 104.4(5) yes O1 . S1 . C6 . 105.4(4) yes C5 . S1 . C6 . 98.1(5) yes O2 . S2 . C7 . 104.3(5) yes O2 . S2 . C8 . 104.5(5) yes C7 . S2 . C8 . 99.3(5) yes Zn1 . O1 . S1 . 126.3(4) yes Zn1 . O2 . S2 . 126.0(4) yes Zn1 . N1 . C1 . 172.7(8) yes Zn1 4_665 N2 . C2 . 169.5(8) yes Zn1 . N3 . C3 . 172.9(10) yes Zn1 3_955 N4 . C4 . 167.3(8) yes Au1 . C1 . N1 . 176.9(9) yes Au1 . C2 . N2 . 174.9(9) yes Au2 . C3 . N3 . 177.5(9) yes Au2 . C4 . N4 . 178.4(9) yes S1 . C5 . H51 . 109.2 no S1 . C5 . H52 . 109.6 no H51 . C5 . H52 . 109.5 no S1 . C5 . H53 . 109.5 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no S1 . C6 . H61 . 109.3 no S1 . C6 . H62 . 109.6 no H61 . C6 . H62 . 109.5 no S1 . C6 . H63 . 109.5 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no S2 . C7 . H71 . 109.3 no S2 . C7 . H72 . 109.5 no H71 . C7 . H72 . 109.5 no S2 . C7 . H73 . 109.6 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.5 no S2 . C8 . H81 . 109.1 no S2 . C8 . H82 . 109.6 no H81 . C8 . H82 . 109.5 no S2 . C8 . H83 . 109.7 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C6 . H62 . O1 2_876 159 0.95 2.43 3.332(15) yes C8 . H83 . O2 2_866 154 0.95 2.57 3.450(15) yes