# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Geisheimer, Andrew' 'Wen Huang.' 'Pacradouni, Vighen' 'Sabok-Sayr, Seyed' 'Sonier, Jeff' 'Leznoff, Daniel' _publ_contact_author_name 'Leznoff, Daniel' _publ_contact_author_email dleznoff@sfu.ca _publ_section_title ; Magnetic properties of isostructural M(H2O)4[Au(CN)4]2-based coordination polymers (M = Mn, Co, Ni, Cu, Zn) by SQUID and mSR studies ; # Attachment '- DLeznoff MAuCN4.cif' #============================================================================= data_{[Mn(H2O)4][Au(CN)4]2(H2O)4} _database_code_depnum_ccdc_archive 'CCDC 800212' #TrackingRef '- DLeznoff MAuCN4.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C8 H16 Au2 Mn1 N8 O8' _chemical_formula_moiety 'C8 H16 Au2 Mn1 N8 O8' _chemical_formula_weight 801.13 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------ _cell_length_a 6.6823(2) _cell_length_b 8.5837(3) _cell_length_c 10.1917(3) _cell_angle_alpha 93.0570(10) _cell_angle_beta 104.628(2) _cell_angle_gamma 99.897(2) _cell_volume 554.34(3) _cell_formula_units_Z 1 _cell_measurement_reflns_used 28266 _cell_measurement_theta_min 2.076 _cell_measurement_theta_max 40.598 _cell_measurement_temperature 293 _exptl_crystal_description chunk _exptl_crystal_colour colourless _exptl_crystal_size_min 0.11 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.53 _exptl_crystal_density_diffrn 2.400 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 367 _exptl_absorpt_coefficient_mu 13.807 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4448 _exptl_absorpt_correction_T_max 0.7457 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area Detector' _diffrn_radiation_monochromator graphite _diffrn_measurement_method \w\f _diffrn_ambient_temperature 293 _diffrn_reflns_number 28266 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_theta_min 2.076 _diffrn_reflns_theta_max 40.598 _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 29.637 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number ? _diffrn_standards_decay_% ? #========================================================================== # 8. REFINEMENT DATA # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_number_total 6922 _reflns_number_gt 4219 _reflns_threshold_expression I>2.5\s(I _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0328 _refine_ls_number_reflns 4023 _refine_ls_number_restraints 0 _refine_ls_number_parameters 129 _refine_ls_goodness_of_fit_ref 0.9637 _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_ls_shift/su_max 0.000170 _refine_diff_density_max 1.18 _refine_diff_density_min -1.35 _reflns_limit_h_min -12 _reflns_limit_h_max 11 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 18 #_refine_ls_R_factor_ref 0.294 #_reflns_number_all 6922 _refine_ls_R_factor_all 0.0677 _refine_ls_wR_factor_all 0.0502 # Number of reflections with Friedels Law is 6922 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7101 #--------------------------------------------------------- _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_coef 17.1(11) _refine_ls_extinction_method 'Larson (1970), Equation 22' # _refine_ls_scale 0.1881(3) _exptl_absorpt_process_details . _refine_ls_abs_structure_Flack . _refine_ls_abs_structure_details . # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . #========================================================== # 9. General computing _computing_data_collection ; Bruker SMART ; _computing_cell_refinement ; Bruker SMART ; _computing_data_reduction ; Bruker SAINT ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _computing_structure_refinement ; Crystals ; #=================================================================== # 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 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' 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' 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' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' #============================================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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 _atom_site_attached_hydrogens Au1 Au 0.5000 0.0000 0.5000 0.0268 1.0000 Uani S . . . . . Au2 Au 1.0000 0.5000 0.5000 0.0318 1.0000 Uani S . . . . . Mn1 Mn 1.0000 0.0000 1.0000 0.0261 1.0000 Uani S . . . . . O1 O 1.0195(5) 0.2571(3) 1.0313(3) 0.0357 1.0000 Uani . . . . . . O2 O 0.7440(5) -0.0361(4) 1.0954(3) 0.0459 1.0000 Uani . . . . . . O3 O 0.6009(6) 0.5535(4) 0.8280(4) 0.0618 1.0000 Uani . . . . . . O4 O 0.5834(5) 0.2946(4) 0.9971(4) 0.0548 1.0000 Uani . . . . . . N11 N 0.7744(6) -0.0073(4) 0.7970(3) 0.0402 1.0000 Uani . . . . . . N12 N 0.4200(7) 0.3380(5) 0.5775(5) 0.0599 1.0000 Uani . . . . . . N21 N 0.8294(7) 0.1565(5) 0.3518(5) 0.0605 1.0000 Uani . . . . . . N22 N 1.0097(8) 0.3847(6) 0.7871(4) 0.0622 1.0000 Uani . . . . . . C11 C 0.6756(6) -0.0038(5) 0.6889(3) 0.0329 1.0000 Uani . . . . . . C12 C 0.4469(6) 0.2146(5) 0.5494(4) 0.0384 1.0000 Uani . . . . . . C21 C 0.8913(7) 0.2800(5) 0.4075(4) 0.0425 1.0000 Uani . . . . . . C22 C 1.0040(7) 0.4243(5) 0.6808(4) 0.0415 1.0000 Uani . . . . . . H11 H 1.1467 0.3006 1.0947 0.100(10) 1.0000 Uiso R . . . . . H12 H 1.0102 0.3016 0.9496 0.100(10) 1.0000 Uiso R . . . . . H21 H 0.7925 -0.0059 1.1888 0.107(10) 1.0000 Uiso R . . . . . H22 H 0.6790 -0.1405 1.0804 0.107(10) 1.0000 Uiso R . . . . . H31 H 0.5152 0.5894 0.8749 0.126(10) 1.0000 Uiso R . . . . . H32 H 0.5189 0.4858 0.7524 0.126(10) 1.0000 Uiso R . . . . . H41 H 0.7162 0.2703 1.0144 0.120(10) 1.0000 Uiso R . . . . . H42 H 0.5749 0.3780 0.9440 0.120(10) 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 0.02705(9) 0.03341(11) 0.01507(7) 0.00141(6) -0.00314(6) 0.00624(7) Au2 0.03513(10) 0.03413(11) 0.02332(9) 0.00030(7) 0.00706(7) 0.00119(8) Mn1 0.0292(3) 0.0298(4) 0.0151(3) 0.0015(2) -0.0022(2) 0.0068(3) O1 0.0443(15) 0.0309(14) 0.0299(12) 0.0032(10) 0.0067(11) 0.0063(12) O2 0.0423(15) 0.0553(19) 0.0357(14) -0.0072(13) 0.0137(12) -0.0038(13) O3 0.0520(19) 0.061(2) 0.063(2) -0.0216(19) 0.0040(17) 0.0088(17) O4 0.0392(16) 0.049(2) 0.074(2) -0.0021(18) 0.0109(16) 0.0122(15) N11 0.0464(18) 0.047(2) 0.0204(12) 0.0058(13) -0.0055(12) 0.0100(15) N12 0.065(3) 0.047(3) 0.061(3) -0.007(2) 0.004(2) 0.016(2) N21 0.067(3) 0.051(3) 0.059(3) -0.012(2) 0.027(2) -0.010(2) N22 0.086(3) 0.064(3) 0.038(2) 0.015(2) 0.020(2) 0.010(2) C11 0.0356(16) 0.040(2) 0.0185(13) 0.0032(13) -0.0009(12) 0.0070(14) C12 0.0369(18) 0.044(2) 0.0302(17) -0.0010(16) 0.0004(14) 0.0104(16) C21 0.050(2) 0.043(2) 0.0313(18) -0.0043(16) 0.0142(17) -0.0032(18) C22 0.053(2) 0.041(2) 0.0306(18) 0.0037(16) 0.0134(17) 0.0046(18) 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 . C12 2_656 1.997(4) yes Au1 . C11 2_656 1.991(3) yes Au1 . C11 . 1.991(3) yes Au1 . C12 . 1.997(4) yes Au1 . N21 . 3.132(4) yes Au1 . N21 2_656 3.132(4) yes Au2 . C21 2_766 1.994(4) yes Au2 . C22 2_766 1.982(4) yes Au2 . C21 . 1.994(4) yes Au2 . C22 . 1.982(4) yes Au2 . N12 1_655 3.282(5) yes Au2 . N12 2_666 3.282(5) yes Mn1 . N11 2_757 2.221(3) yes Mn1 . O1 2_757 2.190(3) yes Mn1 . O2 2_757 2.158(3) yes Mn1 . O1 . 2.190(3) yes Mn1 . O2 . 2.158(3) yes Mn1 . N11 . 2.221(3) yes O1 . H11 . 0.931 no O1 . H12 . 0.927 no O2 . H21 . 0.931 no O2 . H22 . 0.913 no O3 . H31 . 0.914 no O3 . H32 . 0.927 no O4 . H41 . 0.923 no O4 . H42 . 0.921 no N11 . C11 . 1.138(4) yes N12 . C12 . 1.138(6) yes N21 . C21 . 1.133(6) yes N22 . C22 . 1.146(6) yes 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 C12 2_656 Au1 . C11 2_656 90.66(16) yes C12 2_656 Au1 . C11 . 89.34(16) yes C11 2_656 Au1 . C11 . 179.994 yes C12 2_656 Au1 . C12 . 179.994 yes C11 2_656 Au1 . C12 . 89.34(16) yes C11 . Au1 . C12 . 90.66(16) yes C12 2_656 Au1 . N21 . 90.13(15) yes C11 2_656 Au1 . N21 . 77.13(14) yes C11 . Au1 . N21 . 102.87(14) yes C12 . Au1 . N21 . 89.87(15) yes C12 2_656 Au1 . N21 2_656 89.87(15) yes C11 2_656 Au1 . N21 2_656 102.87(14) yes C11 . Au1 . N21 2_656 77.13(14) yes C12 . Au1 . N21 2_656 90.13(15) yes N21 . Au1 . N21 2_656 179.996 yes C21 2_766 Au2 . C22 2_766 91.51(18) yes C21 2_766 Au2 . C21 . 179.994 yes C22 2_766 Au2 . C21 . 88.49(18) yes C21 2_766 Au2 . C22 . 88.49(18) yes C22 2_766 Au2 . C22 . 179.994 yes C21 . Au2 . C22 . 91.51(18) yes C21 2_766 Au2 . N12 1_655 102.39(17) yes C22 2_766 Au2 . N12 1_655 104.31(16) yes C21 . Au2 . N12 1_655 77.61(17) yes C22 . Au2 . N12 1_655 75.69(16) yes C21 2_766 Au2 . N12 2_666 77.61(17) yes C22 2_766 Au2 . N12 2_666 75.69(16) yes C21 . Au2 . N12 2_666 102.39(17) yes C22 . Au2 . N12 2_666 104.31(16) yes N12 1_655 Au2 . N12 2_666 179.996 yes N11 2_757 Mn1 . O1 2_757 89.85(12) yes N11 2_757 Mn1 . O2 2_757 90.78(13) yes O1 2_757 Mn1 . O2 2_757 89.31(12) yes N11 2_757 Mn1 . O1 . 90.15(12) yes O1 2_757 Mn1 . O1 . 179.995 yes O2 2_757 Mn1 . O1 . 90.69(12) yes N11 2_757 Mn1 . O2 . 89.22(13) yes O1 2_757 Mn1 . O2 . 90.69(12) yes O2 2_757 Mn1 . O2 . 179.995 yes O1 . Mn1 . O2 . 89.31(12) yes N11 2_757 Mn1 . N11 . 179.995 yes O1 2_757 Mn1 . N11 . 90.15(12) yes O2 2_757 Mn1 . N11 . 89.22(13) yes O1 . Mn1 . N11 . 89.85(12) yes O2 . Mn1 . N11 . 90.78(13) yes Mn1 . O1 . H11 . 108.2 no Mn1 . O1 . H12 . 110.4 no H11 . O1 . H12 . 110.9 no Mn1 . O2 . H21 . 111.0 no Mn1 . O2 . H22 . 109.9 no H21 . O2 . H22 . 109.5 no H31 . O3 . H32 . 109.3 no H41 . O4 . H42 . 110.3 no Mn1 . N11 . C11 . 173.1(4) yes C12 . N12 . Au2 1_455 131.9(4) yes C21 . N21 . Au1 . 104.2(3) yes Au1 . C11 . N11 . 179.2(4) yes Au1 . C12 . N12 . 178.8(4) yes Au2 . C21 . N21 . 178.2(4) yes Au2 . C22 . N22 . 178.0(4) yes 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 O1 . H11 . O3 2_767 157 0.93 1.88 2.762(6) yes O1 . H12 . N22 . 176 0.93 1.84 2.763(6) yes O2 . H21 . N21 1_556 150 0.93 2.05 2.890(6) yes O2 . H22 . O4 2_657 147 0.91 1.96 2.769(6) yes O3 . H31 . O4 2_667 162 0.91 1.91 2.793(6) yes O3 . H32 . N12 . 164 0.93 2.03 2.927(6) yes O4 . H41 . O1 . 168 0.92 2.01 2.922(6) yes O4 . H42 . O3 . 171 0.92 1.97 2.888(6) yes #===END #=============================================================================== data_{[Co(H2O)4][Au(CN)4]2(H2O)4} _database_code_depnum_ccdc_archive 'CCDC 800213' #TrackingRef '- DLeznoff MAuCN4.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C8 H16 Au2 Co1 N8 O8' _chemical_formula_moiety 'C8 H16 Au2 Co1 N8 O8' _chemical_formula_weight 805.14 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------ _cell_length_a 6.6483(10) _cell_length_b 8.5123(15) _cell_length_c 10.0840(18) _cell_angle_alpha 92.779(15) _cell_angle_beta 105.677(14) _cell_angle_gamma 99.743(14) _cell_volume 538.85(17) _cell_formula_units_Z 1 _cell_measurement_reflns_used 6294 _cell_measurement_theta_min 2.104 _cell_measurement_theta_max 38.997 _cell_measurement_temperature 293 _exptl_crystal_description chunk _exptl_crystal_colour orange _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.28 _exptl_crystal_density_diffrn 2.481 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 369 _exptl_absorpt_coefficient_mu 14.388 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.137 _exptl_absorpt_correction_T_max 0.237 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area Detector' _diffrn_radiation_monochromator graphite _diffrn_measurement_method \w\f _diffrn_ambient_temperature 293 _diffrn_reflns_number 6294 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min 2.104 _diffrn_reflns_theta_max 38.997 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 38.997 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number ? _diffrn_standards_decay_% ? #========================================================================== # 8. REFINEMENT DATA # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_number_total 6292 _reflns_number_gt 3754 _reflns_threshold_expression I>2.5\s(I _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0381 _refine_ls_number_reflns 3651 _refine_ls_number_restraints 0 _refine_ls_number_parameters 129 _refine_ls_goodness_of_fit_ref 1.2849 _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_ls_shift/su_max 0.000079 _refine_diff_density_max 2.63 _refine_diff_density_min -2.16 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 17 #_refine_ls_R_factor_ref 0.329 #_reflns_number_all 6292 _refine_ls_R_factor_all 0.838 _refine_ls_wR_factor_all 0.0439 # Number of reflections with Friedels Law is 6292 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6286 #--------------------------------------------------------- _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_coef 62(2) _refine_ls_extinction_method 'Larson (1970), Equation 22' # _refine_ls_scale 1.996(4) _exptl_absorpt_process_details . _refine_ls_abs_structure_Flack . _refine_ls_abs_structure_details . # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . #========================================================== # 9. General computing _computing_data_collection ; Bruker SMART ; _computing_cell_refinement ; Bruker SMART ; _computing_data_reduction ; Bruker SAINT ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _computing_structure_refinement ; Crystals ; #=================================================================== # 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' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 '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 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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 _atom_site_attached_hydrogens Au1 Au 0.5000 0.0000 0.5000 0.0241 1.0000 Uani S . . . . . Au2 Au 1.0000 0.5000 0.5000 0.0291 1.0000 Uani S . . . . . Co1 Co 1.0000 0.0000 1.0000 0.0224 1.0000 Uani S . . . . . O1 O 1.0190(6) 0.2465(4) 1.0322(4) 0.0312 1.0000 Uani . . . . . . O2 O 0.7532(6) -0.0339(4) 1.0902(4) 0.0376 1.0000 Uani . . . . . . O3 O 0.6017(7) 0.5559(5) 0.8292(5) 0.0565 1.0000 Uani . . . . . . O4 O 0.5807(7) 0.2907(5) 0.9966(5) 0.0515 1.0000 Uani . . . . . . N11 N 0.7826(6) -0.0081(5) 0.8027(4) 0.0317 1.0000 Uani . . . . . . N12 N 0.4197(9) 0.3390(6) 0.5779(6) 0.0534 1.0000 Uani . . . . . . N21 N 0.8349(9) 0.1526(6) 0.3517(6) 0.0546 1.0000 Uani . . . . . . N22 N 1.0072(9) 0.3839(7) 0.7892(5) 0.0556 1.0000 Uani . . . . . . C11 C 0.6798(7) -0.0048(5) 0.6927(4) 0.0278 1.0000 Uani . . . . . . C12 C 0.4477(8) 0.2163(6) 0.5493(5) 0.0330 1.0000 Uani . . . . . . C21 C 0.8932(9) 0.2773(7) 0.4074(6) 0.0396 1.0000 Uani . . . . . . C22 C 1.0048(9) 0.4246(7) 0.6840(5) 0.0399 1.0000 Uani . . . . . . H11 H 1.1462 0.2910 1.0937 0.069(10) 1.0000 Uiso R . . . . . H12 H 1.0080 0.2899 0.9505 0.069(10) 1.0000 Uiso R . . . . . H21 H 0.8040 -0.0053 1.1830 0.077(10) 1.0000 Uiso R . . . . . H22 H 0.6866 -0.1384 1.0745 0.077(10) 1.0000 Uiso R . . . . . H31 H 0.5165 0.5949 0.8744 0.098(10) 1.0000 Uiso R . . . . . H32 H 0.5198 0.4903 0.7530 0.098(10) 1.0000 Uiso R . . . . . H41 H 0.7138 0.2682 1.0133 0.094(10) 1.0000 Uiso R . . . . . H42 H 0.5699 0.3738 0.9433 0.094(10) 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 0.02441(12) 0.02873(13) 0.01352(10) -0.00005(8) -0.00272(7) 0.00351(9) Au2 0.03192(13) 0.03071(14) 0.02150(12) 0.00023(10) 0.00664(9) -0.00027(10) Co1 0.0244(4) 0.0253(4) 0.0137(3) 0.0001(3) -0.0004(3) 0.0043(3) O1 0.0389(19) 0.0274(16) 0.0244(15) 0.0020(13) 0.0064(14) 0.0026(14) O2 0.0356(18) 0.043(2) 0.0304(18) -0.0048(15) 0.0115(15) -0.0048(15) O3 0.043(2) 0.057(3) 0.060(3) -0.022(2) 0.005(2) 0.006(2) O4 0.034(2) 0.045(2) 0.073(3) -0.001(2) 0.013(2) 0.0082(19) N11 0.034(2) 0.035(2) 0.0185(15) 0.0004(14) -0.0028(14) 0.0042(16) N12 0.057(3) 0.043(3) 0.054(3) -0.005(2) 0.006(3) 0.012(3) N21 0.064(3) 0.048(3) 0.049(3) -0.012(2) 0.026(3) -0.008(3) N22 0.077(4) 0.054(3) 0.035(3) 0.013(2) 0.017(3) 0.006(3) C11 0.030(2) 0.029(2) 0.0177(16) 0.0016(15) -0.0023(15) 0.0027(17) C12 0.027(2) 0.036(3) 0.029(2) -0.0014(19) -0.0009(17) 0.0038(19) C21 0.044(3) 0.040(3) 0.035(3) 0.000(2) 0.015(2) 0.002(2) C22 0.044(3) 0.043(3) 0.029(2) 0.005(2) 0.009(2) 0.001(2) 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 . C12 2_656 1.995(5) yes Au1 . C11 2_656 1.993(4) yes Au1 . C11 . 1.993(4) yes Au1 . C12 . 1.995(5) yes Au1 . N21 . 3.145(5) yes Au1 . N21 2_656 3.145(5) yes Au2 . C21 2_766 1.996(6) yes Au2 . C22 2_766 1.987(5) yes Au2 . C21 . 1.996(6) yes Au2 . C22 . 1.987(5) yes Au2 . N12 1_655 3.240(5) yes Au2 . N12 2_666 3.240(5) yes Co1 . N11 2_757 2.110(4) yes Co1 . O1 2_757 2.085(3) yes Co1 . O2 2_757 2.068(3) yes Co1 . O1 . 2.085(3) yes Co1 . O2 . 2.068(3) yes Co1 . N11 . 2.110(4) yes O1 . H11 . 0.910 no O1 . H12 . 0.910 no O2 . H21 . 0.910 no O2 . H22 . 0.910 no O3 . H31 . 0.910 no O3 . H32 . 0.910 no O4 . H41 . 0.910 no O4 . H42 . 0.910 no N11 . C11 . 1.139(5) yes N12 . C12 . 1.129(6) yes N21 . C21 . 1.130(7) yes N22 . C22 . 1.128(7) yes 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 C12 2_656 Au1 . C11 2_656 90.71(19) yes C12 2_656 Au1 . C11 . 89.29(19) yes C11 2_656 Au1 . C11 . 179.994 yes C12 2_656 Au1 . C12 . 179.994 yes C11 2_656 Au1 . C12 . 89.29(19) yes C11 . Au1 . C12 . 90.71(19) yes C12 2_656 Au1 . N21 . 89.26(19) yes C11 2_656 Au1 . N21 . 77.52(17) yes C11 . Au1 . N21 . 102.48(17) yes C12 . Au1 . N21 . 90.74(19) yes C12 2_656 Au1 . N21 2_656 90.74(19) yes C11 2_656 Au1 . N21 2_656 102.48(17) yes C11 . Au1 . N21 2_656 77.52(17) yes C12 . Au1 . N21 2_656 89.26(19) yes N21 . Au1 . N21 2_656 179.996 yes C21 2_766 Au2 . C22 2_766 91.4(2) yes C21 2_766 Au2 . C21 . 179.994 yes C22 2_766 Au2 . C21 . 88.6(2) yes C21 2_766 Au2 . C22 . 88.6(2) yes C22 2_766 Au2 . C22 . 179.994 yes C21 . Au2 . C22 . 91.4(2) yes C21 2_766 Au2 . N12 1_655 103.2(2) yes C22 2_766 Au2 . N12 1_655 103.29(19) yes C21 . Au2 . N12 1_655 76.8(2) yes C22 . Au2 . N12 1_655 76.71(19) yes C21 2_766 Au2 . N12 2_666 76.8(2) yes C22 2_766 Au2 . N12 2_666 76.71(19) yes C21 . Au2 . N12 2_666 103.2(2) yes C22 . Au2 . N12 2_666 103.29(19) yes N12 1_655 Au2 . N12 2_666 179.996 yes N11 2_757 Co1 . O1 2_757 90.79(15) yes N11 2_757 Co1 . O2 2_757 90.80(15) yes O1 2_757 Co1 . O2 2_757 88.70(14) yes N11 2_757 Co1 . O1 . 89.21(15) yes O1 2_757 Co1 . O1 . 179.994 yes O2 2_757 Co1 . O1 . 91.30(14) yes N11 2_757 Co1 . O2 . 89.20(15) yes O1 2_757 Co1 . O2 . 91.30(14) yes O2 2_757 Co1 . O2 . 179.994 yes O1 . Co1 . O2 . 88.70(14) yes N11 2_757 Co1 . N11 . 179.995 yes O1 2_757 Co1 . N11 . 89.21(15) yes O2 2_757 Co1 . N11 . 89.20(15) yes O1 . Co1 . N11 . 90.79(15) yes O2 . Co1 . N11 . 90.80(15) yes Co1 . O1 . H11 . 109.4 no Co1 . O1 . H12 . 109.3 no H11 . O1 . H12 . 109.5 no Co1 . O2 . H21 . 110.1 no Co1 . O2 . H22 . 110.1 no H21 . O2 . H22 . 109.5 no H31 . O3 . H32 . 109.5 no H41 . O4 . H42 . 109.5 no Co1 . N11 . C11 . 173.9(4) yes C12 . N12 . Au2 1_455 132.3(4) yes C21 . N21 . Au1 . 102.6(4) yes Au1 . C11 . N11 . 179.7(4) yes Au1 . C12 . N12 . 179.5(5) yes Au2 . C21 . N21 . 177.9(5) yes Au2 . C22 . N22 . 179.0(5) yes 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 O1 . H11 . O3 2_767 157 0.91 1.89 2.752(8) yes O1 . H12 . N22 . 176 0.91 1.85 2.754(8) yes O2 . H21 . N21 1_556 149 0.91 2.06 2.880(8) yes O2 . H22 . O4 2_657 147 0.91 1.95 2.756(8) yes O3 . H31 . O4 2_667 163 0.91 1.90 2.779(8) yes O3 . H32 . N12 . 164 0.91 2.02 2.903(8) yes O4 . H41 . O1 . 171 0.91 2.03 2.929(8) yes O4 . H42 . O3 . 170 0.91 1.99 2.891(8) yes #===END #=============================================================================== data_{[Ni(H2O)4][Au(CN)4]2(H2O)4} _database_code_depnum_ccdc_archive 'CCDC 800214' #TrackingRef '- DLeznoff MAuCN4.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C8 H16 Au2 Ni1 N8 O8' _chemical_formula_moiety 'C8 H16 Au2 Ni1 N8 O8' _chemical_formula_weight 804.90 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------ _cell_length_a 6.6216(9) _cell_length_b 8.5492(9) _cell_length_c 10.0117(12) _cell_angle_alpha 92.749(10) _cell_angle_beta 105.997(10) _cell_angle_gamma 99.633(10) _cell_volume 534.47(12) _cell_formula_units_Z 1 _cell_measurement_reflns_used 4491 _cell_measurement_theta_min 2.122 _cell_measurement_theta_max 34.483 _cell_measurement_temperature 293 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_min 0.09 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_max 0.48 _exptl_crystal_density_diffrn 2.501 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 370 _exptl_absorpt_coefficient_mu 14.610 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.012 _exptl_absorpt_correction_T_max 0.269 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area Detector' _diffrn_radiation_monochromator graphite _diffrn_measurement_method \w\f _diffrn_ambient_temperature 293 _diffrn_reflns_number 4491 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min 2.122 _diffrn_reflns_theta_max 34.483 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 31.380 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number ? _diffrn_standards_decay_% ? #========================================================================== # 8. REFINEMENT DATA # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_number_total 4489 _reflns_number_gt 2968 _reflns_threshold_expression I>2.5\s(I _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_gt 0.0720 _refine_ls_wR_factor_ref 0.0699 _refine_ls_number_reflns 2878 _refine_ls_number_restraints 0 _refine_ls_number_parameters 129 _refine_ls_goodness_of_fit_ref 1.1962 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 0.00P] ,where P=p(6)*max(Fo^2^,0) + (1-p(6))Fc^2^ ; _refine_ls_shift/su_max 0.000056 _refine_diff_density_max 7.18 _refine_diff_density_min -3.68 _reflns_limit_h_min -10 _reflns_limit_h_max 9 _reflns_limit_k_min -13 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 15 #_refine_ls_R_factor_ref 0.0555 #_reflns_number_all 4489 _refine_ls_R_factor_all 0.0912 _refine_ls_wR_factor_all 0.0801 # Number of reflections with Friedels Law is 4489 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4553 #--------------------------------------------------------- _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_coef 37(4) _refine_ls_extinction_method 'Larson (1970), Equation 22' # _refine_ls_scale 3.400(13) _exptl_absorpt_process_details . _refine_ls_abs_structure_Flack . _refine_ls_abs_structure_details . # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . #========================================================== # 9. General computing _computing_data_collection ; Bruker SMART ; _computing_cell_refinement ; Bruker SMART ; _computing_data_reduction ; Bruker SAINT ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _computing_structure_refinement ; Crystals ; #=================================================================== # 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' Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421 1.0341 '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 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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 _atom_site_attached_hydrogens Au1 Au 0.5000 0.0000 0.5000 0.0253 1.0000 Uani S . . . . . Au2 Au 1.0000 0.5000 0.5000 0.0309 1.0000 Uani S . . . . . Ni1 Ni 1.0000 0.0000 1.0000 0.0241 1.0000 Uani S . . . . . O1 O 1.0192(12) 0.2426(8) 1.0342(7) 0.0334 1.0000 Uani . . . . . . O2 O 0.7499(11) -0.0338(8) 1.0862(7) 0.0403 1.0000 Uani . . . . . . O3 O 0.6024(13) 0.5613(9) 0.8266(8) 0.0582 1.0000 Uani . . . . . . O4 O 0.5806(13) 0.2944(10) 0.9954(9) 0.0509 1.0000 Uani . . . . . . N11 N 0.7868(12) -0.0049(8) 0.8046(7) 0.0338 1.0000 Uani . . . . . . N12 N 0.4206(18) 0.3399(10) 0.5750(10) 0.0546 1.0000 Uani . . . . . . N21 N 0.8298(18) 0.1560(11) 0.3500(10) 0.0577 1.0000 Uani . . . . . . N22 N 1.014(2) 0.3831(12) 0.7923(11) 0.0623 1.0000 Uani . . . . . . C11 C 0.6842(14) -0.0019(10) 0.6952(9) 0.0308 1.0000 Uani . . . . . . C12 C 0.4457(16) 0.2155(11) 0.5473(9) 0.0354 1.0000 Uani . . . . . . C21 C 0.8921(17) 0.2792(11) 0.4065(11) 0.0389 1.0000 Uani . . . . . . C22 C 1.0067(16) 0.4243(11) 0.6858(10) 0.0374 1.0000 Uani . . . . . . H11 H 1.1464 0.2860 1.0975 0.17(4) 1.0000 Uiso R . . . . . H12 H 1.0099 0.2870 0.9524 0.17(4) 1.0000 Uiso R . . . . . H21 H 0.7983 -0.0037 1.1797 0.17(4) 1.0000 Uiso R . . . . . H22 H 0.6849 -0.1383 1.0712 0.17(4) 1.0000 Uiso R . . . . . H31 H 0.5167 0.5972 0.8735 0.19(4) 1.0000 Uiso R . . . . . H32 H 0.5204 0.4936 0.7510 0.19(4) 1.0000 Uiso R . . . . . H41 H 0.7135 0.2701 1.0127 0.19(4) 1.0000 Uiso R . . . . . H42 H 0.5722 0.3778 0.9423 0.19(4) 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 0.0234(2) 0.0294(2) 0.01769(19) 0.00212(14) -0.00247(14) 0.00434(15) Au2 0.0326(3) 0.0315(2) 0.0261(2) 0.00253(17) 0.00752(18) 0.00059(18) Ni1 0.0245(7) 0.0266(7) 0.0181(6) 0.0049(5) 0.0004(5) 0.0047(6) O1 0.040(4) 0.032(3) 0.028(3) 0.002(2) 0.010(3) 0.005(3) O2 0.034(3) 0.049(4) 0.034(3) -0.001(3) 0.010(3) -0.002(3) O3 0.043(4) 0.065(5) 0.056(5) -0.016(4) 0.003(4) 0.006(4) O4 0.037(4) 0.049(4) 0.064(5) -0.001(4) 0.009(4) 0.011(4) N11 0.036(4) 0.034(4) 0.023(3) 0.004(3) -0.003(3) 0.002(3) N12 0.065(6) 0.039(4) 0.053(6) -0.005(4) 0.007(5) 0.010(4) N21 0.066(7) 0.044(5) 0.054(6) -0.017(4) 0.015(5) -0.005(5) N22 0.078(8) 0.060(6) 0.048(6) 0.016(5) 0.018(5) 0.008(6) C11 0.027(4) 0.033(4) 0.027(4) 0.002(3) 0.003(3) -0.001(3) C12 0.035(5) 0.037(4) 0.029(4) 0.001(3) 0.000(3) 0.010(4) C21 0.036(5) 0.034(4) 0.044(5) 0.001(4) 0.016(4) -0.006(4) C22 0.039(5) 0.034(4) 0.036(5) 0.003(3) 0.011(4) -0.003(4) 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 . C11 2_656 2.001(9) yes Au1 . C12 2_656 1.995(9) yes Au1 . C11 . 2.001(9) yes Au1 . C12 . 1.995(9) yes Au1 . N21 . 3.135(10) yes Au1 . N21 2_656 3.135(10) yes Au2 . C22 2_766 1.990(9) yes Au2 . C21 2_766 1.990(9) yes Au2 . C21 . 1.990(9) yes Au2 . C22 . 1.990(9) yes Au2 . N12 1_655 3.228(10) yes Au2 . N12 2_666 3.228(10) yes Ni1 . N11 2_757 2.067(7) yes Ni1 . O1 2_757 2.062(6) yes Ni1 . O2 2_757 2.055(6) yes Ni1 . O1 . 2.062(6) yes Ni1 . O2 . 2.055(6) yes Ni1 . N11 . 2.067(7) yes O1 . H11 . 0.910 no O1 . H12 . 0.910 no O2 . H21 . 0.910 no O2 . H22 . 0.910 no O3 . H31 . 0.910 no O3 . H32 . 0.910 no O4 . H41 . 0.910 no O4 . H42 . 0.910 no N11 . C11 . 1.122(10) yes N12 . C12 . 1.136(12) yes N21 . C21 . 1.127(12) yes N22 . C22 . 1.129(12) yes 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 C11 2_656 Au1 . C12 2_656 90.8(3) yes C11 2_656 Au1 . C11 . 179.994 yes C12 2_656 Au1 . C11 . 89.2(3) yes C11 2_656 Au1 . C12 . 89.2(3) yes C12 2_656 Au1 . C12 . 179.994 yes C11 . Au1 . C12 . 90.8(3) yes C11 2_656 Au1 . N21 . 77.5(3) yes C12 2_656 Au1 . N21 . 90.3(3) yes C11 . Au1 . N21 . 102.5(3) yes C12 . Au1 . N21 . 89.7(3) yes C11 2_656 Au1 . N21 2_656 102.5(3) yes C12 2_656 Au1 . N21 2_656 89.7(3) yes C11 . Au1 . N21 2_656 77.5(3) yes C12 . Au1 . N21 2_656 90.3(3) yes N21 . Au1 . N21 2_656 179.996 yes C22 2_766 Au2 . C21 2_766 91.4(4) yes C22 2_766 Au2 . C21 . 88.6(4) yes C21 2_766 Au2 . C21 . 179.994 yes C22 2_766 Au2 . C22 . 179.994 yes C21 2_766 Au2 . C22 . 88.6(4) yes C21 . Au2 . C22 . 91.4(4) yes C22 2_766 Au2 . N12 1_655 102.8(3) yes C21 2_766 Au2 . N12 1_655 103.3(4) yes C21 . Au2 . N12 1_655 76.7(4) yes C22 . Au2 . N12 1_655 77.2(3) yes C22 2_766 Au2 . N12 2_666 77.2(3) yes C21 2_766 Au2 . N12 2_666 76.7(4) yes C21 . Au2 . N12 2_666 103.3(4) yes C22 . Au2 . N12 2_666 102.8(3) yes N12 1_655 Au2 . N12 2_666 179.996 yes N11 2_757 Ni1 . O1 2_757 90.6(3) yes N11 2_757 Ni1 . O2 2_757 90.0(3) yes O1 2_757 Ni1 . O2 2_757 88.5(3) yes N11 2_757 Ni1 . O1 . 89.4(3) yes O1 2_757 Ni1 . O1 . 179.994 yes O2 2_757 Ni1 . O1 . 91.5(3) yes N11 2_757 Ni1 . O2 . 90.0(3) yes O1 2_757 Ni1 . O2 . 91.5(3) yes O2 2_757 Ni1 . O2 . 179.994 yes O1 . Ni1 . O2 . 88.5(3) yes N11 2_757 Ni1 . N11 . 179.994 yes O1 2_757 Ni1 . N11 . 89.4(3) yes O2 2_757 Ni1 . N11 . 90.0(3) yes O1 . Ni1 . N11 . 90.6(3) yes O2 . Ni1 . N11 . 90.0(3) yes Ni1 . O1 . H11 . 109.4 no Ni1 . O1 . H12 . 109.4 no H11 . O1 . H12 . 109.5 no Ni1 . O2 . H21 . 110.1 no Ni1 . O2 . H22 . 110.1 no H21 . O2 . H22 . 109.5 no H31 . O3 . H32 . 109.5 no H41 . O4 . H42 . 109.5 no Ni1 . N11 . C11 . 174.6(8) yes C12 . N12 . Au2 1_455 131.7(9) yes C21 . N21 . Au1 . 103.9(7) yes Au1 . C11 . N11 . 179.2(8) yes Au1 . C12 . N12 . 178.1(10) yes Au2 . C21 . N21 . 178.0(10) yes Au2 . C22 . N22 . 178.7(10) yes 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 O1 . H11 . O3 2_767 156 0.91 1.88 2.735(14) yes O1 . H12 . N22 . 175 0.91 1.84 2.749(14) yes O2 . H21 . N21 1_556 151 0.91 2.07 2.901(14) yes O2 . H22 . O4 2_657 148 0.91 1.95 2.762(14) yes O3 . H31 . O4 2_667 163 0.91 1.88 2.765(14) yes O3 . H32 . N12 . 164 0.91 2.03 2.913(14) yes O4 . H41 . O1 . 172 0.91 2.03 2.933(14) yes O4 . H42 . O3 . 171 0.91 2.01 2.911(14) yes #===END #=============================================================================== data_{[Cu(H2O)4][Au(CN)4]2(H2O)4} _database_code_depnum_ccdc_archive 'CCDC 800215' #TrackingRef '- DLeznoff MAuCN4.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C8 H16 Au2 Cu1 N8 O8' _chemical_formula_moiety 'C8 H16 Au2 Cu1 N8 O8' _chemical_formula_weight 809.74 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------ _cell_length_a 6.4798(2) _cell_length_b 12.4272(3) _cell_length_c 13.6182(3) _cell_angle_alpha 98.2940(10) _cell_angle_beta 94.5860(10) _cell_angle_gamma 101.1370(10) _cell_volume 1058.13(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 48507 _cell_measurement_theta_min 2.083 _cell_measurement_theta_max 45.281 _cell_measurement_temperature 100 _exptl_crystal_description chunk _exptl_crystal_colour green _exptl_crystal_size_min 0.27 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_max 0.55 _exptl_crystal_density_diffrn 2.541 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 742 _exptl_absorpt_coefficient_mu 14.875 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3885 _exptl_absorpt_correction_T_max 0.7489 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area Detector' _diffrn_radiation_monochromator graphite _diffrn_measurement_method \w\f _diffrn_ambient_temperature 100 _diffrn_reflns_number 48507 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_theta_min 2.083 _diffrn_reflns_theta_max 45.281 _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 27.168 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number ? _diffrn_standards_decay_% ? #========================================================================== # 8. REFINEMENT DATA # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_number_total 15657 _reflns_number_gt 12155 _reflns_threshold_expression I>2.5\s(I _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.0429 _refine_ls_number_reflns 11745 _refine_ls_number_restraints 0 _refine_ls_number_parameters 1251 _refine_ls_goodness_of_fit_ref 0.9517 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.00P)^2^ + 0.00P] ,where P=p(6)*max(Fo^2^,0) + (1-p(6))Fc^2^ ; _refine_ls_shift/su_max 0.000851 _refine_diff_density_max 4.85 _refine_diff_density_min -4.63 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -23 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 27 #_refine_ls_R_factor_ref 0.0327 #_reflns_number_all 15657 _refine_ls_R_factor_all 0.0466 _refine_ls_wR_factor_all 0.0492 # Number of reflections with Friedels Law is 15657 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 17716 #--------------------------------------------------------- _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_coef none _refine_ls_extinction_method . _exptl_absorpt_process_details . _refine_ls_abs_structure_Flack . _refine_ls_abs_structure_details . # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . #========================================================== # 9. General computing _computing_data_collection ; Bruker SMART ; _computing_cell_refinement ; Bruker SMART ; _computing_data_reduction ; Bruker SAINT ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _computing_structure_refinement ; Crystals ; #=================================================================== # 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 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' 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' 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' Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' #============================================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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 _atom_site_attached_hydrogens Au1 Au -0.256161(17) 0.760084(9) 0.246177(8) 0.0106 1.0000 Uani . . . . . . Au2 Au -0.5000 1.0000 0.5000 0.0135 1.0000 Uani S . . . . . Au3 Au 0.0000 0.5000 0.0000 0.0118 1.0000 Uani S . . . . . Cu1 Cu 0.0000 0.5000 0.5000 0.0109 1.0000 Uani S . . . . . Cu2 Cu -0.5000 1.0000 0.0000 0.0108 1.0000 Uani S . . . . . O1 O -0.0951(4) 0.7978(2) 0.6399(2) 0.0239 1.0000 Uani . . . . . . O2 O -0.4402(4) 0.6331(2) 0.6477(2) 0.0246 1.0000 Uani . . . . . . O3 O -0.0721(4) 0.8501(2) 0.8515(2) 0.0237 1.0000 Uani . . . . . . O4 O -0.4142(4) 0.6813(2) 0.8577(2) 0.0265 1.0000 Uani . . . . . . O11 O 0.1121(4) 0.62974(18) 0.60787(17) 0.0160 1.0000 Uani . . . . . . O12 O -0.2737(4) 0.46608(18) 0.55667(18) 0.0179 1.0000 Uani . . . . . . O21 O -0.3583(4) 1.15365(19) 0.11584(18) 0.0191 1.0000 Uani . . . . . . O22 O -0.7741(4) 0.97763(19) 0.05758(18) 0.0203 1.0000 Uani . . . . . . N11 N -0.1325(5) 0.6145(2) 0.4030(2) 0.0201 1.0000 Uani . . . . . . N12 N -0.5396(5) 0.5470(3) 0.1135(2) 0.0257 1.0000 Uani . . . . . . N13 N -0.3930(4) 0.9047(2) 0.0915(2) 0.0168 1.0000 Uani . . . . . . N14 N 0.0283(5) 0.9708(3) 0.3801(2) 0.0264 1.0000 Uani . . . . . . N21 N -0.6093(6) 0.7515(3) 0.3936(3) 0.0293 1.0000 Uani . . . . . . N22 N -0.5599(6) 0.9090(3) 0.7005(3) 0.0324 1.0000 Uani . . . . . . N31 N 0.0783(6) 0.7537(3) 0.0901(3) 0.0273 1.0000 Uani . . . . . . N32 N -0.0610(6) 0.4275(3) 0.2084(2) 0.0280 1.0000 Uani . . . . . . C11 C -0.1765(5) 0.6676(2) 0.3457(2) 0.0157 1.0000 Uani . . . . . . C12 C -0.4365(5) 0.6246(3) 0.1617(2) 0.0179 1.0000 Uani . . . . . . C13 C -0.3410(5) 0.8522(2) 0.1477(2) 0.0152 1.0000 Uani . . . . . . C14 C -0.0745(5) 0.8939(2) 0.3309(2) 0.0173 1.0000 Uani . . . . . . C21 C -0.5688(6) 0.8426(3) 0.4309(3) 0.0206 1.0000 Uani . . . . . . C22 C -0.5385(6) 0.9442(3) 0.6284(3) 0.0214 1.0000 Uani . . . . . . C31 C 0.0470(5) 0.6608(3) 0.0579(2) 0.0185 1.0000 Uani . . . . . . C32 C -0.0404(6) 0.4557(3) 0.1328(3) 0.0193 1.0000 Uani . . . . . . H11 H -0.0907 0.8029 0.7074 0.097(7) 1.0000 Uiso R . . . . . H12 H -0.0753 0.8672 0.6233 0.097(7) 1.0000 Uiso R . . . . . H21 H -0.5729 0.6447 0.6330 0.097(7) 1.0000 Uiso R . . . . . H22 H -0.3433 0.6949 0.6420 0.097(7) 1.0000 Uiso R . . . . . H31 H 0.0605 0.8374 0.8636 0.095(7) 1.0000 Uiso R . . . . . H32 H -0.1693 0.7878 0.8557 0.095(7) 1.0000 Uiso R . . . . . H41 H -0.4277 0.6125 0.8751 0.101(7) 1.0000 Uiso R . . . . . H42 H -0.4210 0.6753 0.7900 0.101(7) 1.0000 Uiso R . . . . . H111 H 0.0373 0.6837 0.6013 0.087(7) 1.0000 Uiso R . . . . . H112 H 0.0977 0.6079 0.6683 0.087(7) 1.0000 Uiso R . . . . . H121 H -0.2966 0.5249 0.5995 0.090(7) 1.0000 Uiso R . . . . . H122 H -0.2859 0.4054 0.5877 0.090(7) 1.0000 Uiso R . . . . . H211 H -0.4302 1.2080 0.1061 0.092(7) 1.0000 Uiso R . . . . . H212 H -0.3740 1.1359 0.1777 0.092(7) 1.0000 Uiso R . . . . . H221 H -0.7876 1.0376 0.1016 0.093(7) 1.0000 Uiso R . . . . . H222 H -0.7984 0.9158 0.0870 0.093(7) 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 0.01124(4) 0.00938(4) 0.01167(4) 0.00442(3) -0.00075(3) 0.00240(3) Au2 0.01476(7) 0.01099(6) 0.01610(7) 0.00470(5) 0.00422(5) 0.00310(5) Au3 0.01352(6) 0.01016(5) 0.01194(6) 0.00304(4) 0.00227(5) 0.00192(5) Cu1 0.0114(2) 0.00962(18) 0.0110(2) 0.00252(15) -0.00030(15) 0.00082(15) Cu2 0.0118(2) 0.00961(18) 0.0117(2) 0.00467(15) -0.00094(15) 0.00237(15) O1 0.0224(12) 0.0158(10) 0.0330(14) 0.0047(9) 0.0010(10) 0.0032(9) O2 0.0147(11) 0.0213(11) 0.0348(15) -0.0017(10) -0.0028(10) 0.0031(9) O3 0.0169(11) 0.0185(11) 0.0328(14) -0.0017(10) -0.0021(10) 0.0025(9) O4 0.0226(13) 0.0203(11) 0.0374(15) 0.0068(10) 0.0013(11) 0.0054(10) O11 0.0184(11) 0.0147(9) 0.0142(9) 0.0022(7) -0.0002(8) 0.0024(8) O12 0.0181(10) 0.0147(9) 0.0224(11) 0.0061(8) 0.0061(8) 0.0030(8) O21 0.0233(12) 0.0181(10) 0.0174(10) 0.0046(8) 0.0025(8) 0.0064(9) O22 0.0224(12) 0.0148(9) 0.0252(12) 0.0062(8) 0.0063(9) 0.0041(8) N11 0.0245(14) 0.0187(11) 0.0185(12) 0.0091(10) -0.0014(10) 0.0053(10) N12 0.0247(15) 0.0180(12) 0.0298(16) -0.0010(11) -0.0051(12) -0.0001(11) N13 0.0204(12) 0.0143(10) 0.0162(11) 0.0053(8) -0.0013(9) 0.0044(9) N14 0.0277(16) 0.0171(12) 0.0308(16) 0.0021(11) -0.0043(12) 0.0003(11) N21 0.0297(17) 0.0164(12) 0.041(2) 0.0023(12) 0.0112(15) 0.0026(12) N22 0.043(2) 0.0317(17) 0.0247(16) 0.0121(13) 0.0073(15) 0.0066(15) N31 0.0315(18) 0.0159(12) 0.0332(17) 0.0014(11) 0.0096(14) 0.0010(11) N32 0.039(2) 0.0282(15) 0.0184(14) 0.0096(12) 0.0055(13) 0.0050(14) C11 0.0172(13) 0.0130(10) 0.0167(12) 0.0038(9) -0.0009(10) 0.0025(9) C12 0.0162(13) 0.0170(12) 0.0214(14) 0.0047(10) -0.0006(10) 0.0057(10) C13 0.0170(12) 0.0133(10) 0.0156(12) 0.0056(9) -0.0019(9) 0.0032(9) C14 0.0190(14) 0.0138(11) 0.0196(13) 0.0039(10) -0.0003(10) 0.0048(10) C21 0.0197(15) 0.0186(13) 0.0242(16) 0.0057(11) 0.0078(12) 0.0020(11) C22 0.0252(16) 0.0173(13) 0.0226(15) 0.0044(11) 0.0036(12) 0.0051(11) C31 0.0194(14) 0.0162(12) 0.0199(14) 0.0036(10) 0.0057(11) 0.0016(10) C32 0.0227(15) 0.0157(12) 0.0197(14) 0.0034(10) 0.0025(11) 0.0044(11) 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 . C11 . 1.997(3) yes Au1 . C12 . 1.998(3) yes Au1 . C13 . 1.994(3) yes Au1 . C14 . 1.989(3) yes Au1 . N21 . 3.159(3) yes Au1 . N31 . 3.158(3) yes Au2 . C21 2_476 1.994(4) yes Au2 . C22 2_476 1.988(3) yes Au2 . C21 . 1.994(4) yes Au2 . C22 . 1.988(3) yes Au2 . N14 1_455 3.278(3) yes Au2 . N14 2_576 3.278(3) yes Au3 . C31 2_565 1.995(3) yes Au3 . C32 2_565 1.987(3) yes Au3 . C31 . 1.995(3) yes Au3 . C32 . 1.987(3) yes Au3 . N12 1_655 3.156(3) yes Au3 . N12 2_465 3.156(3) yes Cu1 . N11 2_566 2.312(2) yes Cu1 . O11 2_566 1.995(2) yes Cu1 . O12 2_566 1.986(2) yes Cu1 . O11 . 1.995(2) yes Cu1 . O12 . 1.986(2) yes Cu1 . N11 . 2.312(2) yes Cu2 . O21 2_475 2.280(2) yes Cu2 . N13 2_475 2.010(2) yes Cu2 . O22 2_475 1.985(2) yes Cu2 . O21 . 2.280(2) yes Cu2 . O22 . 1.985(2) yes Cu2 . N13 . 2.010(2) yes O1 . H11 . 0.910 no O1 . H12 . 0.910 no O2 . H21 . 0.910 no O2 . H22 . 0.910 no O3 . H31 . 0.910 no O3 . H32 . 0.910 no O4 . H41 . 0.910 no O4 . H42 . 0.910 no O11 . H111 . 0.910 no O11 . H112 . 0.910 no O12 . H121 . 0.910 no O12 . H122 . 0.910 no O21 . H211 . 0.910 no O21 . H212 . 0.910 no O22 . H221 . 0.910 no O22 . H222 . 0.910 no N11 . C11 . 1.145(3) yes N12 . C12 . 1.142(4) yes N13 . C13 . 1.146(3) yes N14 . C14 . 1.142(4) yes N21 . C21 . 1.143(5) yes N22 . C22 . 1.139(4) yes N31 . C31 . 1.148(4) yes N32 . C32 . 1.144(4) yes 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 C11 . Au1 . C12 . 90.10(12) yes C11 . Au1 . C13 . 178.93(12) yes C12 . Au1 . C13 . 89.63(12) yes C11 . Au1 . C14 . 89.34(12) yes C12 . Au1 . C14 . 179.35(11) yes C13 . Au1 . C14 . 90.94(12) yes C11 . Au1 . N21 . 74.51(11) yes C12 . Au1 . N21 . 87.98(11) yes C13 . Au1 . N21 . 104.44(11) yes C14 . Au1 . N21 . 92.17(11) yes C11 . Au1 . N31 . 105.32(11) yes C12 . Au1 . N31 . 88.14(11) yes C13 . Au1 . N31 . 75.71(11) yes C14 . Au1 . N31 . 91.70(11) yes N21 . Au1 . N31 . 176.12(8) yes C21 2_476 Au2 . C22 2_476 88.38(14) yes C21 2_476 Au2 . C21 . 179.994 yes C22 2_476 Au2 . C21 . 91.62(14) yes C21 2_476 Au2 . C22 . 91.62(14) yes C22 2_476 Au2 . C22 . 179.994 yes C21 . Au2 . C22 . 88.38(14) yes C21 2_476 Au2 . N14 1_455 104.39(12) yes C22 2_476 Au2 . N14 1_455 72.62(12) yes C21 . Au2 . N14 1_455 75.61(12) yes C22 . Au2 . N14 1_455 107.38(12) yes C21 2_476 Au2 . N14 2_576 75.61(12) yes C22 2_476 Au2 . N14 2_576 107.38(12) yes C21 . Au2 . N14 2_576 104.39(12) yes C22 . Au2 . N14 2_576 72.62(12) yes N14 1_455 Au2 . N14 2_576 179.996 yes C31 2_565 Au3 . C32 2_565 91.54(13) yes C31 2_565 Au3 . C31 . 179.994 yes C32 2_565 Au3 . C31 . 88.46(13) yes C31 2_565 Au3 . C32 . 88.46(13) yes C32 2_565 Au3 . C32 . 179.994 yes C31 . Au3 . C32 . 91.54(13) yes C31 2_565 Au3 . N12 1_655 102.60(12) yes C32 2_565 Au3 . N12 1_655 104.89(12) yes C31 . Au3 . N12 1_655 77.40(12) yes C32 . Au3 . N12 1_655 75.11(12) yes C31 2_565 Au3 . N12 2_465 77.40(12) yes C32 2_565 Au3 . N12 2_465 75.11(12) yes C31 . Au3 . N12 2_465 102.60(12) yes C32 . Au3 . N12 2_465 104.89(12) yes N12 1_655 Au3 . N12 2_465 179.996 yes N11 2_566 Cu1 . O11 2_566 90.23(10) yes N11 2_566 Cu1 . O12 2_566 90.66(10) yes O11 2_566 Cu1 . O12 2_566 92.16(10) yes N11 2_566 Cu1 . O11 . 89.77(10) yes O11 2_566 Cu1 . O11 . 179.994 yes O12 2_566 Cu1 . O11 . 87.84(10) yes N11 2_566 Cu1 . O12 . 89.34(10) yes O11 2_566 Cu1 . O12 . 87.84(10) yes O12 2_566 Cu1 . O12 . 179.994 yes O11 . Cu1 . O12 . 92.16(10) yes N11 2_566 Cu1 . N11 . 179.995 yes O11 2_566 Cu1 . N11 . 89.77(10) yes O12 2_566 Cu1 . N11 . 89.34(10) yes O11 . Cu1 . N11 . 90.23(10) yes O12 . Cu1 . N11 . 90.66(10) yes O21 2_475 Cu2 . N13 2_475 89.48(10) yes O21 2_475 Cu2 . O22 2_475 92.61(10) yes N13 2_475 Cu2 . O22 2_475 89.67(10) yes O21 2_475 Cu2 . O21 . 179.995 yes N13 2_475 Cu2 . O21 . 90.52(10) yes O22 2_475 Cu2 . O21 . 87.39(10) yes O21 2_475 Cu2 . O22 . 87.39(10) yes N13 2_475 Cu2 . O22 . 90.33(10) yes O22 2_475 Cu2 . O22 . 179.994 yes O21 . Cu2 . O22 . 92.61(10) yes O21 2_475 Cu2 . N13 . 90.52(10) yes N13 2_475 Cu2 . N13 . 179.994 yes O22 2_475 Cu2 . N13 . 90.33(10) yes O21 . Cu2 . N13 . 89.48(10) yes O22 . Cu2 . N13 . 89.67(10) yes H11 . O1 . H12 . 109.5 no H21 . O2 . H22 . 109.5 no H31 . O3 . H32 . 109.5 no H41 . O4 . H42 . 109.5 no Cu1 . O11 . H111 . 109.2 no Cu1 . O11 . H112 . 109.3 no H111 . O11 . H112 . 109.5 no Cu1 . O12 . H121 . 112.4 no Cu1 . O12 . H122 . 112.6 no H121 . O12 . H122 . 109.5 no Cu2 . O21 . H211 . 108.4 no Cu2 . O21 . H212 . 108.6 no H211 . O21 . H212 . 109.5 no Cu2 . O22 . H221 . 112.8 no Cu2 . O22 . H222 . 112.9 no H221 . O22 . H222 . 109.5 no Cu1 . N11 . C11 . 169.9(3) yes C12 . N12 . Au3 1_455 132.4(3) yes Cu2 . N13 . C13 . 175.6(3) yes C14 . N14 . Au2 1_655 129.0(3) yes C21 . N21 . Au1 . 98.5(2) yes C31 . N31 . Au1 . 101.9(2) yes Au1 . C11 . N11 . 179.4(3) yes Au1 . C12 . N12 . 179.9(3) yes Au1 . C13 . N13 . 178.9(3) yes Au1 . C14 . N14 . 179.3(3) yes Au2 . C21 . N21 . 178.2(3) yes Au2 . C22 . N22 . 177.9(3) yes Au3 . C31 . N31 . 178.4(3) yes Au3 . C32 . N32 . 178.0(3) yes 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 O1 . H11 . O3 . 167 0.91 1.95 2.848(5) yes O1 . H12 . N14 2_576 167 0.91 1.98 2.879(5) yes O2 . H21 . O11 1_455 165 0.91 2.01 2.899(5) yes O2 . H22 . O1 . 165 0.91 1.86 2.745(5) yes O3 . H31 . O21 2_576 166 0.91 1.91 2.800(5) yes O3 . H32 . O4 . 166 0.91 1.86 2.757(5) yes O4 . H41 . N12 2_466 169 0.91 1.98 2.882(5) yes O4 . H42 . O2 . 169 0.91 1.92 2.820(5) yes O11 . H111 . O1 . 158 0.91 1.83 2.696(5) yes O11 . H112 . N32 2_566 176 0.91 1.82 2.726(5) yes O12 . H121 . O2 . 156 0.91 1.85 2.711(5) yes O12 . H122 . N21 2_466 157 0.91 2.00 2.857(5) yes O21 . H211 . O4 2_476 156 0.91 1.89 2.748(5) yes O21 . H212 . N22 2_476 173 0.91 1.88 2.785(5) yes O22 . H221 . O3 2_476 153 0.91 1.87 2.714(5) yes O22 . H222 . N31 1_455 154 0.91 2.03 2.872(5) yes #===END #=============================================================================== data_{[Zn(H2O)4][Au(CN)4]2(H2O)4} _database_code_depnum_ccdc_archive 'CCDC 800216' #TrackingRef '- DLeznoff MAuCN4.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C8 H16 Au2 N8 O8 Zn1' _chemical_formula_moiety 'C8 H16 Au2 N8 O8 Zn1' _chemical_formula_weight 811.58 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------ _cell_length_a 6.6384(4) _cell_length_b 8.5458(5) _cell_length_c 10.0854(6) _cell_angle_alpha 92.839(3) _cell_angle_beta 105.320(3) _cell_angle_gamma 99.872(4) _cell_volume 540.93(6) _cell_formula_units_Z 1 _cell_measurement_reflns_used 27963 _cell_measurement_theta_min 2.104 _cell_measurement_theta_max 44.942 _cell_measurement_temperature 293 _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_min 0.43 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_max 0.70 _exptl_crystal_density_diffrn 2.491 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 372 _exptl_absorpt_coefficient_mu 14.674 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4025 _exptl_absorpt_correction_T_max 0.7489 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area Detector' _diffrn_radiation_monochromator graphite _diffrn_measurement_method \w\f _diffrn_ambient_temperature 293 _diffrn_reflns_number 27963 _diffrn_reflns_av_R_equivalents 0.076 _diffrn_reflns_theta_min 2.104 _diffrn_reflns_theta_max 44.942 _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.617 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number ? _diffrn_standards_decay_% ? #========================================================================== # 8. REFINEMENT DATA # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_number_total 8339 _reflns_number_gt 4160 _reflns_threshold_expression I>2.5\s(I _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.0555 _refine_ls_number_reflns 3866 _refine_ls_number_restraints 0 _refine_ls_number_parameters 129 _refine_ls_goodness_of_fit_ref 0.9132 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 0.00P] ,where P=p(6)*max(Fo^2^,0) + (1-p(6))Fc^2^ ; _refine_ls_shift/su_max 0.000062 _refine_diff_density_max 3.64 _refine_diff_density_min -3.16 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 20 #_refine_ls_R_factor_ref 0.0424 #_reflns_number_all 8339 _refine_ls_R_factor_all 0.1122 _refine_ls_wR_factor_all 0.0963 # Number of reflections with Friedels Law is 8339 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 8881 #--------------------------------------------------------- _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_coef 13.5(18) _refine_ls_extinction_method 'Larson (1970), Equation 22' # _refine_ls_scale 0.5616(13) _exptl_absorpt_process_details . _refine_ls_abs_structure_Flack . _refine_ls_abs_structure_details . # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . #========================================================== # 9. General computing _computing_data_collection ; Bruker SMART ; _computing_cell_refinement ; Bruker SMART ; _computing_data_reduction ; Bruker SAINT ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _computing_structure_refinement ; Crystals ; #=================================================================== # 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 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' 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' 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' 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' 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' #============================================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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 _atom_site_attached_hydrogens Au1 Au 0.5000 0.0000 0.5000 0.0222 1.0000 Uani S . . . . . Au2 Au 1.0000 0.5000 0.5000 0.0272 1.0000 Uani S . . . . . Zn1 Zn 1.0000 0.0000 1.0000 0.0235 1.0000 Uani S . . . . . O1 O 1.0169(8) 0.2474(5) 1.0323(5) 0.0311 1.0000 Uani . . . . . . O2 O 0.7493(8) -0.0333(6) 1.0905(5) 0.0406 1.0000 Uani . . . . . . O3 O 0.6029(9) 0.5579(7) 0.8283(7) 0.0588 1.0000 Uani . . . . . . O4 O 0.5814(9) 0.2937(7) 0.9958(7) 0.0514 1.0000 Uani . . . . . . N11 N 0.7805(9) -0.0067(7) 0.8007(5) 0.0340 1.0000 Uani . . . . . . N12 N 0.4215(11) 0.3403(8) 0.5753(7) 0.0524 1.0000 Uani . . . . . . N21 N 0.8324(12) 0.1546(8) 0.3510(8) 0.0570 1.0000 Uani . . . . . . N22 N 1.0130(13) 0.3837(9) 0.7890(7) 0.0577 1.0000 Uani . . . . . . C11 C 0.6799(10) -0.0036(7) 0.6913(5) 0.0275 1.0000 Uani . . . . . . C12 C 0.4476(11) 0.2161(8) 0.5476(7) 0.0348 1.0000 Uani . . . . . . C21 C 0.8917(12) 0.2787(9) 0.4065(7) 0.0387 1.0000 Uani . . . . . . C22 C 1.0072(12) 0.4236(8) 0.6826(7) 0.0367 1.0000 Uani . . . . . . H11 H 1.1438 0.2912 1.0939 0.108(15) 1.0000 Uiso R . . . . . H12 H 1.0082 0.2902 0.9506 0.108(15) 1.0000 Uiso R . . . . . H21 H 0.7914 -0.0020 1.1828 0.068(15) 1.0000 Uiso R . . . . . H22 H 0.6753 -0.1356 1.0752 0.068(15) 1.0000 Uiso R . . . . . H31 H 0.5171 0.5953 0.8742 0.136(15) 1.0000 Uiso R . . . . . H32 H 0.5217 0.4921 0.7524 0.136(15) 1.0000 Uiso R . . . . . H41 H 0.7142 0.2709 1.0123 0.132(15) 1.0000 Uiso R . . . . . H42 H 0.5719 0.3766 0.9426 0.132(15) 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 0.02439(14) 0.02920(16) 0.00822(11) 0.00158(10) -0.00307(9) 0.00431(11) Au2 0.03232(17) 0.03052(17) 0.01643(14) 0.00172(12) 0.00686(12) -0.00026(13) Zn1 0.0284(4) 0.0284(4) 0.0102(3) 0.0014(3) -0.0006(3) 0.0056(4) O1 0.041(3) 0.029(2) 0.023(2) 0.0048(17) 0.0067(18) 0.0085(19) O2 0.040(3) 0.049(3) 0.029(2) -0.006(2) 0.013(2) -0.005(2) O3 0.046(3) 0.057(4) 0.062(4) -0.022(3) 0.004(3) 0.003(3) O4 0.038(3) 0.047(3) 0.068(4) 0.001(3) 0.013(3) 0.008(3) N11 0.039(3) 0.041(3) 0.0150(19) 0.0026(19) -0.0025(18) 0.007(2) N12 0.057(4) 0.049(4) 0.047(4) -0.005(3) 0.005(3) 0.016(3) N21 0.066(5) 0.047(4) 0.051(4) -0.020(3) 0.024(4) -0.014(3) N22 0.082(5) 0.057(4) 0.033(3) 0.014(3) 0.017(4) 0.005(4) C11 0.032(3) 0.033(3) 0.014(2) 0.0027(19) -0.0002(19) 0.006(2) C12 0.036(3) 0.034(3) 0.029(3) -0.001(2) 0.002(2) 0.005(3) C21 0.045(4) 0.043(4) 0.027(3) 0.000(3) 0.016(3) -0.004(3) C22 0.051(4) 0.037(3) 0.020(3) 0.006(2) 0.010(3) 0.002(3) 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 . C12 2_656 1.996(7) yes Au1 . C11 2_656 1.987(5) yes Au1 . C11 . 1.987(5) yes Au1 . C12 . 1.996(7) yes Au1 . N21 . 3.134(7) yes Au1 . N21 2_656 3.134(7) yes Au2 . C21 2_766 1.996(7) yes Au2 . C22 2_766 1.976(6) yes Au2 . C21 . 1.996(7) yes Au2 . C22 . 1.976(6) yes Au2 . N12 1_655 3.249(7) yes Au2 . N12 2_666 3.249(7) yes Zn1 . N11 2_757 2.140(5) yes Zn1 . O1 2_757 2.102(4) yes Zn1 . O2 2_757 2.086(5) yes Zn1 . O1 . 2.102(4) yes Zn1 . O2 . 2.086(5) yes Zn1 . N11 . 2.140(5) yes O1 . H11 . 0.910 no O1 . H12 . 0.910 no O2 . H21 . 0.910 no O2 . H22 . 0.910 no O3 . H31 . 0.910 no O3 . H32 . 0.910 no O4 . H41 . 0.910 no O4 . H42 . 0.910 no N11 . C11 . 1.134(6) yes N12 . C12 . 1.137(9) yes N21 . C21 . 1.129(9) yes N22 . C22 . 1.135(8) yes 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 C12 2_656 Au1 . C11 2_656 91.1(3) yes C12 2_656 Au1 . C11 . 88.9(3) yes C11 2_656 Au1 . C11 . 179.994 yes C12 2_656 Au1 . C12 . 179.994 yes C11 2_656 Au1 . C12 . 88.9(3) yes C11 . Au1 . C12 . 91.1(3) yes C12 2_656 Au1 . N21 . 90.2(3) yes C11 2_656 Au1 . N21 . 77.6(2) yes C11 . Au1 . N21 . 102.4(2) yes C12 . Au1 . N21 . 89.8(3) yes C12 2_656 Au1 . N21 2_656 89.8(3) yes C11 2_656 Au1 . N21 2_656 102.4(2) yes C11 . Au1 . N21 2_656 77.6(2) yes C12 . Au1 . N21 2_656 90.2(3) yes N21 . Au1 . N21 2_656 179.996 yes C21 2_766 Au2 . C22 2_766 91.4(3) yes C21 2_766 Au2 . C21 . 179.994 yes C22 2_766 Au2 . C21 . 88.6(3) yes C21 2_766 Au2 . C22 . 88.6(3) yes C22 2_766 Au2 . C22 . 179.994 yes C21 . Au2 . C22 . 91.4(3) yes C21 2_766 Au2 . N12 1_655 102.9(3) yes C22 2_766 Au2 . N12 1_655 103.7(3) yes C21 . Au2 . N12 1_655 77.1(3) yes C22 . Au2 . N12 1_655 76.3(3) yes C21 2_766 Au2 . N12 2_666 77.1(3) yes C22 2_766 Au2 . N12 2_666 76.3(3) yes C21 . Au2 . N12 2_666 102.9(3) yes C22 . Au2 . N12 2_666 103.7(3) yes N12 1_655 Au2 . N12 2_666 179.996 yes N11 2_757 Zn1 . O1 2_757 90.18(19) yes N11 2_757 Zn1 . O2 2_757 90.5(2) yes O1 2_757 Zn1 . O2 2_757 88.1(2) yes N11 2_757 Zn1 . O1 . 89.82(19) yes O1 2_757 Zn1 . O1 . 179.995 yes O2 2_757 Zn1 . O1 . 91.9(2) yes N11 2_757 Zn1 . O2 . 89.5(2) yes O1 2_757 Zn1 . O2 . 91.9(2) yes O2 2_757 Zn1 . O2 . 179.994 yes O1 . Zn1 . O2 . 88.1(2) yes N11 2_757 Zn1 . N11 . 179.995 yes O1 2_757 Zn1 . N11 . 89.82(19) yes O2 2_757 Zn1 . N11 . 89.5(2) yes O1 . Zn1 . N11 . 90.18(19) yes O2 . Zn1 . N11 . 90.5(2) yes Zn1 . O1 . H11 . 108.7 no Zn1 . O1 . H12 . 109.0 no H11 . O1 . H12 . 109.5 no Zn1 . O2 . H21 . 113.0 no Zn1 . O2 . H22 . 113.0 no H21 . O2 . H22 . 109.5 no H31 . O3 . H32 . 109.5 no H41 . O4 . H42 . 109.5 no Zn1 . N11 . C11 . 173.6(6) yes C12 . N12 . Au2 1_455 131.8(6) yes C21 . N21 . Au1 . 103.3(6) yes Au1 . C11 . N11 . 179.2(6) yes Au1 . C12 . N12 . 178.8(7) yes Au2 . C21 . N21 . 178.3(7) yes Au2 . C22 . N22 . 178.3(7) yes 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 O1 . H11 . O3 2_767 158 0.91 1.89 2.751(10) yes O1 . H12 . N22 . 176 0.91 1.86 2.764(10) yes O2 . H21 . N21 1_556 154 0.91 2.04 2.881(10) yes O2 . H22 . O4 2_657 153 0.91 1.93 2.767(10) yes O3 . H31 . O4 2_667 163 0.91 1.89 2.777(10) yes O3 . H32 . N12 . 164 0.91 2.04 2.925(10) yes O4 . H41 . O1 . 171 0.91 2.01 2.915(10) yes O4 . H42 . O3 . 170 0.91 1.99 2.892(10) yes #===END