# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef 'DLeznoff_AuBr2CN2_reduction.cif' #============================================================================= # 1. SUBMISSION DETAILS _publ_contact_author_name 'Daniel B. Leznoff' _publ_contact_author_address ; Leznoff, Daniel B. Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; _publ_contact_author_phone +1-778-782-4887 _publ_contact_author_fax +1-778-782-3765 _publ_contact_author_email dleznoff@sfu.ca #============================================================================= # 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_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 ; ; # 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 J.S.Ovens ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; D.B.Leznoff ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; ## -------------------REFERENCES ----------------------## _publ_section_references ; 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 #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 ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; #=============================================================================== # 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_ZnPyzAu3 _database_code_depnum_ccdc_archive 'CCDC 811552' #TrackingRef 'DLeznoff_AuBr2CN2_reduction.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C12 H10 Au2 Br4 N8 Zn1' _chemical_formula_moiety 'C12 H10 Au2 Br4 N8 Zn1' _chemical_formula_weight 1045.20 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z x,-y,z -x,y,-z x+1/2,-y+1/2,z -x+1/2,y+1/2,-z #------------------------------------------------ _cell_length_a 16.6452(7) _cell_length_b 7.1043(3) _cell_length_c 11.6029(5) _cell_angle_alpha 90 _cell_angle_beta 121.110(2) _cell_angle_gamma 90 _cell_volume 1174.74(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7680 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 36.33 _cell_measurement_temperature 150(2) _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 2.955 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 20.287 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4048 _exptl_absorpt_correction_T_max 0.7476 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _diffrn_reflns_number 3033 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min 2.050 _diffrn_reflns_theta_max 36.400 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 31.026 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 2527 _refine_ls_number_restraints 2 _refine_ls_number_parameters 87 _oxford_refine_ls_R_factor_ref 0.0538 _refine_ls_wR_factor_ref 0.0987 _refine_ls_goodness_of_fit_ref 0.9727 # The values computed from all data _oxford_reflns_number_all 3033 _refine_ls_R_factor_all 0.0691 _refine_ls_wR_factor_all 0.1458 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2594 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_gt 0.1003 _reflns_number_total 3033 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F) + ( 0.02P)^2^ + 0.75P] ,where P=(max(Fo,0) + 2Fc)/3 ; _refine_ls_shift/su_max 0.0008837 _refine_diff_density_min -4.55 _refine_diff_density_max 8.23 _reflns_limit_h_min -27 _reflns_limit_h_max 23 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_refine_ls_scale 0.0673(3) _oxford_diffrn_Wilson_B_factor 1.21 _oxford_diffrn_Wilson_scale 294.66 # Number of reflections with Friedels Law is 3033 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2864 #--------------------------------------------------------- _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 none # none if no extinction, _refine_ls_extinction_method None #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) CRYSTALS (Watkin, 1988) ; #=================================================================== # 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' 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' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 '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 # TODO check _oxford_atom_site_special_shape 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 0.37419(3) 0.0000 0.48466(5) 0.0157 1.0000 Uani S T . . . . . Br1 Br 0.45707(15) 0.2869(3) 0.5100(2) 0.0254 0.5000 Uani . . . . 1 . . Br2 Br 0.28913(16) -0.2938(3) 0.4634(3) 0.0283 0.5000 Uani . . . . 2 . . Zn1 Zn 0.5000 0.0000 1.0000 0.0265 1.0000 Uani S T . . . . . N1 N 0.2766(11) 0.0000 0.1672(13) 0.0392 1.0000 Uani S T . . . . . N2 N 0.4677(13) 0.0000 0.7956(14) 0.0440 1.0000 Uani S T . . . . . N11 N 0.5000 -0.308(2) 1.0000 0.0248 1.0000 Uani S T . . . . . N21 N 0.6505(9) 0.0000 1.0763(14) 0.0285 1.0000 Uani S T . . . . . C1 C 0.3129(13) 0.0000 0.2832(14) 0.0303 1.0000 Uani S T . . . . . C2 C 0.4329(11) 0.0000 0.6815(14) 0.0261 1.0000 Uani S T . . . . . C12 C 0.4389(9) -0.406(2) 0.8929(11) 0.0304 1.0000 Uani . . . . . . . C22 C 0.7248(9) 0.0000 1.106(2) 0.0344 1.0000 Uani S T . . . . . C23 C 0.8260(12) 0.000000(7) 1.1534(17) 0.0364 1.0000 Uani S T . . . . . H121 H 0.3961 -0.3405 0.8159 0.15(10) 1.0000 Uiso R . . . . . . H231 H 0.8368 0.0000 1.0806 0.15(10) 1.0000 Uiso RS . . . . . . H232 H 0.8534 0.1233 1.2069 0.15(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 0.0150(2) 0.0192(2) 0.0129(2) 0.0000 0.00712(15) 0.0000 Br1 0.0249(9) 0.0188(8) 0.0310(10) 0.0036(7) 0.0133(8) -0.0025(7) Br2 0.0273(9) 0.0252(10) 0.0341(11) -0.0045(8) 0.0170(9) -0.0094(8) Zn1 0.0199(10) 0.0426(15) 0.0132(9) 0.0000 0.0058(8) 0.0000 N1 0.026(6) 0.084(14) 0.008(5) 0.0000 0.009(4) 0.0000 N2 0.042(9) 0.078(14) 0.008(5) 0.0000 0.010(5) 0.0000 N11 0.027(6) 0.031(6) 0.020(5) 0.0000 0.015(5) 0.0000 N21 0.019(5) 0.044(8) 0.024(6) 0.0000 0.012(5) 0.0000 C1 0.033(7) 0.047(10) 0.008(5) 0.0000 0.008(5) 0.0000 C2 0.019(5) 0.048(9) 0.009(5) 0.0000 0.006(4) 0.0000 C12 0.030(5) 0.042(7) 0.016(4) 0.000(4) 0.010(4) -0.005(5) C22 0.006(5) 0.026(7) 0.046(10) 0.0000 -0.005(5) 0.0000 C23 0.024(7) 0.067(13) 0.016(6) 0.0000 0.009(5) 0.0000 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 . Br1 5_555 2.392(2) yes Au1 . Br1 . 2.392(2) yes Au1 . Br2 . 2.460(2) yes Au1 . C1 . 2.011(14) yes Au1 . C2 . 1.966(14) yes Br1 . Br1 2_666 3.407(4) yes Zn1 . N11 5_555 2.185(15) yes Zn1 . N21 2_657 2.183(13) yes Zn1 . N2 2_657 2.143(14) yes Zn1 . N2 . 2.143(14) yes Zn1 . N11 . 2.185(15) yes Zn1 . N21 . 2.183(13) yes N1 . C1 . 1.156(18) yes N2 . C2 . 1.138(19) yes N11 . C12 6_657 1.326(14) yes N11 . C12 . 1.326(14) yes N21 . C22 . 1.100(19) yes C12 . C12 5_545 1.34(3) yes C12 . H121 . 0.929 no C22 . C23 . 1.48(2) yes C23 . H232 5_555 1.033 no C23 . H231 . 0.950 no C23 . H232 . 1.033 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 Br1 5_555 Au1 . Br1 . 116.82(11) yes Br1 5_555 Au1 . C1 . 93.2(3) yes Br1 . Au1 . C1 . 93.2(3) yes Br1 5_555 Au1 . C2 . 87.0(2) yes Br1 . Au1 . C2 . 87.0(2) yes C1 . Au1 . C2 . 179.4(7) yes Br1 2_666 Br1 . Au1 . 169.81(13) yes N11 5_555 Zn1 . N21 2_657 90.000(4) yes N11 5_555 Zn1 . N2 2_657 90.000(4) yes N21 2_657 Zn1 . N2 2_657 91.6(6) yes N11 5_555 Zn1 . N2 . 90.000(4) yes N21 2_657 Zn1 . N2 . 88.4(6) yes N2 2_657 Zn1 . N2 . 179.995 yes N11 5_555 Zn1 . N11 . 179.995 yes N21 2_657 Zn1 . N11 . 90.000(4) yes N2 2_657 Zn1 . N11 . 90.000(4) yes N2 . Zn1 . N11 . 90.000(4) yes N11 5_555 Zn1 . N21 . 90.000(4) yes N21 2_657 Zn1 . N21 . 179.995 yes N2 2_657 Zn1 . N21 . 88.4(6) yes N2 . Zn1 . N21 . 91.6(6) yes N11 . Zn1 . N21 . 90.000(4) yes Zn1 . N2 . C2 . 166.5(17) yes Zn1 . N11 . C12 6_657 121.7(8) yes Zn1 . N11 . C12 . 121.7(8) yes C12 6_657 N11 . C12 . 116.5(16) yes Zn1 . N21 . C22 . 175.1(16) yes Au1 . C1 . N1 . 179.1(17) yes Au1 . C2 . N2 . 179.3(16) yes C12 5_545 C12 . N11 . 121.7(8) yes C12 5_545 C12 . H121 . 120.0 no N11 . C12 . H121 . 118.3 no N21 . C22 . C23 . 177(2) yes H232 5_555 C23 . C22 . 106.8 no H232 5_555 C23 . H231 . 107.9 no C22 . C23 . H231 . 111.7 no H232 5_555 C23 . H232 . 115.9 no C22 . C23 . H232 . 106.8 no H231 . C23 . H232 . 107.9 no data_ZnPyzAu1 _database_code_depnum_ccdc_archive 'CCDC 811553' #TrackingRef 'DLeznoff_AuBr2CN2_reduction.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C8 H4 Au2 N6 Zn1' _chemical_formula_moiety 'C8 H4 Au2 N6 Zn1' _chemical_formula_weight 643.47 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'F m m m' 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 x+1/2,y,z+1/2 -x+1/2,-y,-z+1/2 x+1/2,y+1/2,z -x+1/2,-y+1/2,-z x,y,-z -x,-y,z x,y+1/2,-z+1/2 -x,-y+1/2,z+1/2 x+1/2,y,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y+1/2,-z -x+1/2,-y+1/2,z -x,y,z x,-y,-z -x,y+1/2,z+1/2 x,-y+1/2,-z+1/2 -x+1/2,y,z+1/2 x+1/2,-y,-z+1/2 -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y,z -x,y,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 x+1/2,-y,z+1/2 -x+1/2,y,-z+1/2 x+1/2,-y+1/2,z -x+1/2,y+1/2,-z #------------------------------------------------ _cell_length_a 11.4055(4) _cell_length_b 17.3296(6) _cell_length_c 7.0938(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1402.11(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4193 _cell_measurement_theta_min 3.57 _cell_measurement_theta_max 44.17 _cell_measurement_temperature 296(2) _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 3.048 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 22.558 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2804 _exptl_absorpt_correction_T_max 0.7488 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 296(2) _diffrn_reflns_number 9919 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_theta_min 2.351 _diffrn_reflns_theta_max 44.500 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 31.026 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 1059 _refine_ls_number_restraints 4 _refine_ls_number_parameters 41 _oxford_refine_ls_R_factor_ref 0.0317 _refine_ls_wR_factor_ref 0.0386 _refine_ls_goodness_of_fit_ref 0.9680 # The values computed from all data _oxford_reflns_number_all 1547 _refine_ls_R_factor_all 0.0469 _refine_ls_wR_factor_all 0.0514 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1094 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_gt 0.0389 _reflns_number_total 2809 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F) + ( 0.03P)^2^ + 0.00P] ,where P=(max(Fo,0) + 2Fc)/3 ; _refine_ls_shift/su_max 0.0000650 _refine_diff_density_min -2.41 _refine_diff_density_max 1.79 _reflns_limit_h_min 0 _reflns_limit_h_max 22 _reflns_limit_k_min 0 _reflns_limit_k_max 34 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_refine_ls_scale 0.0653(2) _oxford_diffrn_Wilson_B_factor 2.10 _oxford_diffrn_Wilson_scale 1352.50 # Number of reflections with Friedels Law is 1547 # Number of reflections without Friedels Law is 2809 # Theoretical number of reflections is about 1408 #--------------------------------------------------------- _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 none # none if no extinction, _refine_ls_extinction_method 'Larson (1970), Equation 22' _refine_ls_extinction_coef 75(4) #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) CRYSTALS (Watkin, 1988) ; #=================================================================== # 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' 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' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 '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' 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' #============================================================================== # 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 # TODO check _oxford_atom_site_special_shape 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 0.2500 0.2500 0.0000 0.0446 1.0000 Uani S T . . . . . Zn1 Zn 0.5000 0.5000 0.0000 0.0210 1.0000 Uani S T . . . . . N1 N 0.3696(3) 0.41148(18) 0.0000 0.0392 1.0000 Uani S T . . . . . N2 N 0.5000 0.5000 0.3064(5) 0.0273 1.0000 Uani S T . . . . . C1 C 0.3238(4) 0.3530(2) 0.0000 0.0414 1.0000 Uani S T . . . . . C2 C 0.500000(7) 0.5658(3) 0.4023(9) 0.0454 0.644(9) Uani S T P . 1 . . C3 C 0.4022(6) 0.500000(7) 0.4035(9) 0.0281 0.356(9) Uani S T P . 2 . . H2 H 0.5000 0.6158 0.3339 0.06(3) 0.644(9) Uiso RS . P . 1 . . H3 H 0.3294 0.5000 0.3386 0.06(3) 0.356(9) Uiso RS . P . 2 . . 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 0.04826(15) 0.02791(11) 0.05773(18) 0.0000 0.0000 -0.01946(7) Zn1 0.0274(3) 0.01360(19) 0.0219(2) 0.0000 0.0000 0.0000 N1 0.0464(16) 0.0273(11) 0.0440(14) 0.0000 0.0000 -0.0163(11) N2 0.0366(17) 0.0256(13) 0.0197(12) 0.0000 0.0000 0.0000 C1 0.0466(19) 0.0303(15) 0.0472(17) 0.0000 0.0000 -0.0190(14) C2 0.072(5) 0.026(2) 0.038(3) 0.0024(17) 0.0000 0.0000 C3 0.017(3) 0.054(5) 0.014(2) 0.0000 0.0005(17) 0.0000 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 . C1 16_555 1.974(3) yes Au1 . Au1 21_555 3.54690(15) yes Au1 . Au1 21_554 3.54690(15) yes Au1 . C1 . 1.974(3) yes Zn1 . N2 2_665 2.174(3) yes Zn1 . N1 25_565 2.137(3) yes Zn1 . N1 17_655 2.137(3) yes Zn1 . N1 10_665 2.137(3) yes Zn1 . N1 . 2.137(3) yes Zn1 . N2 . 2.174(3) yes N1 . C1 . 1.140(4) yes N2 . C2 10_665 1.328(6) yes N2 . C2 . 1.328(6) yes C2 . C2 9_556 1.387(12) yes C2 . H2 . 0.993 no C3 . C3 9_556 1.369(12) yes C3 . H3 . 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 C1 16_555 Au1 . Au1 21_555 90.000(3) yes C1 16_555 Au1 . Au1 21_554 90.000(3) yes Au1 21_555 Au1 . Au1 21_554 179.997 yes C1 16_555 Au1 . C1 . 179.994 yes Au1 21_555 Au1 . C1 . 90.000(3) yes Au1 21_554 Au1 . C1 . 90.000(3) yes N2 2_665 Zn1 . N1 25_565 90.000 yes N2 2_665 Zn1 . N1 17_655 90.000 yes N1 25_565 Zn1 . N1 17_655 179.995 yes N2 2_665 Zn1 . N1 10_665 90.000 yes N1 25_565 Zn1 . N1 10_665 88.2(2) yes N1 17_655 Zn1 . N1 10_665 91.8(2) yes N2 2_665 Zn1 . N1 . 90.000 yes N1 25_565 Zn1 . N1 . 91.8(2) yes N1 17_655 Zn1 . N1 . 88.2(2) yes N1 10_665 Zn1 . N1 . 179.995 yes N2 2_665 Zn1 . N2 . 179.995 yes N1 25_565 Zn1 . N2 . 90.000 yes N1 17_655 Zn1 . N2 . 90.000 yes N1 10_665 Zn1 . N2 . 90.000 yes N1 . Zn1 . N2 . 90.000 yes Zn1 . N1 . C1 . 163.2(4) yes Zn1 . N2 . C2 10_665 120.8(3) yes Zn1 . N2 . C2 . 120.8(3) yes C2 10_665 N2 . C2 . 118.4(6) yes Au1 . C1 . N1 . 177.9(4) yes C2 9_556 C2 . N2 . 120.8(3) yes C2 9_556 C2 . H2 . 119.2 no N2 . C2 . H2 . 120.0 no C3 9_556 C3 . N2 . 121.7(3) yes C3 9_556 C3 . H3 . 119.0 no N2 . C3 . H3 . 119.3 no data_CoBipyAu3 _database_code_depnum_ccdc_archive 'CCDC 811554' #TrackingRef 'DLeznoff_AuBr2CN2_reduction.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C42 H52 Au3 Br6 Co1 N11' _chemical_formula_moiety 'C42 H52 Au3 Br6 Co1 N11' _chemical_formula_weight 1840.20 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c c m' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y,z+1/2 x,-y,-z+1/2 x,-y,z+1/2 -x,y,-z+1/2 -x,-y,z x,y,-z #------------------------------------------------ _cell_length_a 11.450(3) _cell_length_b 11.467(3) _cell_length_c 20.944(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2750.0(12) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1464 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 22.20 _cell_measurement_temperature 296(2) _exptl_crystal_description block _exptl_crystal_colour amber _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 2.222 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1710 _exptl_absorpt_coefficient_mu 12.672 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4475 _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 APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 296(2) _diffrn_reflns_number 3392 _diffrn_reflns_av_R_equivalents 0.100 _diffrn_reflns_theta_min 1.776 _diffrn_reflns_theta_max 28.506 _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 31.026 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 1875 _refine_ls_number_restraints 0 _refine_ls_number_parameters 158 _oxford_refine_ls_R_factor_ref 0.0358 _refine_ls_wR_factor_ref 0.0369 _refine_ls_goodness_of_fit_ref 1.0261 # The values computed from all data _oxford_reflns_number_all 3392 _refine_ls_R_factor_all 0.0838 _refine_ls_wR_factor_all 0.0611 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1986 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_gt 0.0378 _reflns_number_total 3392 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F) + ( 0.02P)^2^ + 0.00P] ,where P=(max(Fo,0) + 2Fc)/3 ; _refine_ls_shift/su_max 0.0004279 _refine_diff_density_min -0.94 _refine_diff_density_max 0.94 _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _oxford_refine_ls_scale 0.03929(7) _oxford_diffrn_Wilson_B_factor 3.10 _oxford_diffrn_Wilson_scale 972.38 # Number of reflections with Friedels Law is 3392 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3488 #--------------------------------------------------------- _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 none # none if no extinction, _refine_ls_extinction_method None #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) CRYSTALS (Watkin, 1988) ; #=================================================================== # 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' 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' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 '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 # TODO check _oxford_atom_site_special_shape 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 1.0000 1.0000 0.5000 0.0280 1.0000 Uani S T . . . . . Au2 Au 0.76250(6) 0.68991(6) 0.5000 0.0684 1.0000 Uani S T . . . . . Br11 Br 1.06060(13) 0.79633(12) 0.5000 0.0525 1.0000 Uani S T . . 1 . . Br21 Br 0.70489(17) 0.89443(17) 0.5000 0.0946 1.0000 Uani S T . . . . . Br22 Br 0.8194(3) 0.4872(2) 0.5000 0.1348 1.0000 Uani S T . . . . . Co1 Co 1.0000 1.0000 0.7500 0.0223 1.0000 Uani S T . . . . . N1 N 1.0000 1.0000 0.6493(4) 0.0315 1.0000 Uani S T . . . . . N2 N 0.7555(12) 0.6835(11) 0.6479(7) 0.1078 1.0000 Uani . . . . . . . N11 N 1.0000 0.8114(8) 0.7500 0.0301 1.0000 Uani S T . . . . . N21 N 0.8101(8) 1.0000 0.7500 0.0314 1.0000 Uani S T . . . . . N31 N 0.5000 0.5000 0.2500 0.1431 1.0000 Uani S T . . . . . C1 C 1.0000 1.0000 0.5945(5) 0.0290 1.0000 Uani S T . . . . . C2 C 0.7599(11) 0.6893(12) 0.5946(8) 0.0832 1.0000 Uani . . . . . . . C12 C 1.0393(8) 0.7474(7) 0.7001(4) 0.0375 1.0000 Uani . . . . . . . C13 C 1.0383(8) 0.6275(7) 0.6972(4) 0.0429 1.0000 Uani . . . . . . . C14 C 1.0000 0.5645(10) 0.7500 0.0343 1.0000 Uani S T . . . . . C22 C 0.7485(8) 0.9549(9) 0.7027(4) 0.0489 1.0000 Uani . . . . . . . C23 C 0.6283(8) 0.9555(9) 0.7005(4) 0.0518 1.0000 Uani . . . . . . . C24 C 0.5644(10) 1.0000 0.7500 0.0441 1.0000 Uani S T . . . . . C32 C 0.600(2) 0.432(2) 0.2925(15) 0.2191 1.0000 Uani . . . . . . . C33 C 0.551(3) 0.359(2) 0.3289(15) 0.2199 1.0000 Uani . . . . . . . C34 C 0.6623(19) 0.283(2) 0.3631(14) 0.1757 1.0000 Uani . . . . . . . C35 C 0.611(2) 0.226(2) 0.4117(12) 0.2122 1.0000 Uani . . . . . . . H121 H 1.0688 0.7881 0.6655 0.056(14) 1.0000 Uiso R . . . . . . H131 H 1.0642 0.5893 0.6603 0.056(14) 1.0000 Uiso R . . . . . . H221 H 0.7900 0.9192 0.6690 0.056(14) 1.0000 Uiso R . . . . . . H231 H 0.5903 0.9228 0.6653 0.056(14) 1.0000 Uiso R . . . . . . H321 H 0.6401 0.4858 0.3193 0.32(5) 1.0000 Uiso R . . . . . . H322 H 0.6545 0.3947 0.2651 0.32(5) 1.0000 Uiso R . . . . . . H331 H 0.5002 0.3958 0.3585 0.32(5) 1.0000 Uiso R . . . . . . H332 H 0.5078 0.3070 0.3028 0.32(5) 1.0000 Uiso R . . . . . . H341 H 0.7186 0.3360 0.3791 0.32(5) 1.0000 Uiso R . . . . . . H342 H 0.6994 0.2283 0.3355 0.32(5) 1.0000 Uiso R . . . . . . H351 H 0.6666 0.1838 0.4359 0.32(5) 1.0000 Uiso R . . . . . . H352 H 0.5734 0.2819 0.4385 0.32(5) 1.0000 Uiso R . . . . . . H353 H 0.5543 0.1742 0.3948 0.32(5) 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 0.0353(4) 0.0294(4) 0.0192(3) 0.0000 0.0000 0.0013(3) Au2 0.0580(4) 0.0529(4) 0.0944(5) 0.0000 0.0000 -0.0074(3) Br11 0.0725(11) 0.0346(8) 0.0506(8) 0.0000 0.0000 0.0126(7) Br21 0.0784(13) 0.0612(13) 0.1441(18) 0.0000 0.0000 0.0085(10) Br22 0.185(3) 0.0591(15) 0.161(2) 0.0000 0.0000 0.0225(14) Co1 0.0260(11) 0.0210(11) 0.0199(8) 0.0000 0.0000 0.0000 N1 0.037(6) 0.036(6) 0.021(4) 0.0000 0.0000 0.002(5) N2 0.125(12) 0.090(10) 0.109(9) -0.001(9) -0.012(9) -0.029(8) N11 0.030(5) 0.029(5) 0.032(5) 0.0000 -0.002(5) 0.0000 N21 0.027(5) 0.036(6) 0.031(5) -0.005(6) 0.0000 0.0000 N31 0.17(4) 0.06(2) 0.20(3) 0.0000 0.0000 0.0000 C1 0.035(7) 0.018(6) 0.034(6) 0.0000 0.0000 -0.007(5) C2 0.069(9) 0.081(10) 0.100(10) -0.009(9) 0.002(9) -0.016(7) C12 0.059(6) 0.023(5) 0.031(4) 0.005(4) 0.014(4) -0.004(4) C13 0.068(7) 0.027(5) 0.034(5) 0.003(4) 0.007(4) 0.002(5) C14 0.042(7) 0.020(6) 0.040(6) 0.0000 0.000(7) 0.0000 C22 0.028(5) 0.075(7) 0.044(5) -0.016(5) 0.010(4) -0.012(5) C23 0.029(6) 0.083(8) 0.044(6) -0.024(5) -0.007(4) -0.010(5) C24 0.030(7) 0.054(9) 0.049(7) -0.005(8) 0.0000 0.0000 C32 0.17(3) 0.16(3) 0.32(4) -0.07(3) 0.09(2) -0.008(19) C33 0.15(3) 0.22(3) 0.29(4) 0.04(3) 0.06(2) -0.04(2) C34 0.099(17) 0.19(2) 0.23(3) -0.02(2) 0.030(18) -0.010(15) C35 0.14(2) 0.32(4) 0.17(2) -0.01(2) -0.052(18) -0.05(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 . Br11 2_776 2.4364(15) yes Au1 . C1 2_776 1.979(10) yes Au1 . Br11 . 2.4364(15) yes Au1 . C1 . 1.979(10) yes Au2 . C2 8_556 1.981(16) yes Au2 . Br21 . 2.436(2) yes Au2 . Br22 . 2.414(3) yes Au2 . C2 . 1.981(16) yes Br11 . Br22 2_766 3.530(3) yes Co1 . N21 6_756 2.175(9) yes Co1 . N11 7_775 2.163(9) yes Co1 . N1 4_576 2.109(8) yes Co1 . N1 . 2.109(8) yes Co1 . N11 . 2.163(9) yes Co1 . N21 . 2.175(9) yes N1 . C1 . 1.148(11) yes N2 . C2 . 1.121(15) yes N11 . C12 6_756 1.353(9) yes N11 . C12 . 1.353(9) yes N21 . C22 4_576 1.321(10) yes N21 . C22 . 1.321(10) yes N31 . C32 4_565 1.65(3) yes N31 . C32 6_655 1.65(3) yes N31 . C32 7_665 1.65(3) yes N31 . C32 . 1.65(3) yes C12 . C13 . 1.377(11) yes C12 . H121 . 0.926 no C13 . C14 . 1.392(10) yes C13 . H131 . 0.936 no C14 . C14 7_765 1.48(2) yes C22 . C23 . 1.377(12) yes C22 . H221 . 0.945 no C23 . C24 . 1.367(11) yes C23 . H231 . 0.936 no C24 . C24 7_675 1.47(2) yes C32 . C33 . 1.26(3) yes C32 . H321 . 0.950 no C32 . H322 . 0.950 no C33 . C34 . 1.70(4) yes C33 . H331 . 0.950 no C33 . H332 . 0.950 no C34 . C35 . 1.34(3) yes C34 . H341 . 0.950 no C34 . H342 . 0.950 no C35 . H351 . 0.950 no C35 . H352 . 0.950 no C35 . H353 . 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 Br11 2_776 Au1 . C1 2_776 90.00(2) yes Br11 2_776 Au1 . Br11 . 179.995 yes C1 2_776 Au1 . Br11 . 90.00(2) yes Br11 2_776 Au1 . C1 . 90.00(2) yes C1 2_776 Au1 . C1 . 179.994 yes Br11 . Au1 . C1 . 90.00(2) yes C2 8_556 Au2 . Br21 . 90.0(4) yes C2 8_556 Au2 . Br22 . 90.0(4) yes Br21 . Au2 . Br22 . 179.94(9) yes C2 8_556 Au2 . C2 . 178.2(7) yes Br21 . Au2 . C2 . 90.0(4) yes Br22 . Au2 . C2 . 90.0(4) yes Au1 . Br11 . Br22 2_766 173.63(8) yes Au2 . Br22 . Br11 2_766 172.74(13) yes N21 6_756 Co1 . N11 7_775 90.00(2) yes N21 6_756 Co1 . N1 4_576 90.00(2) yes N11 7_775 Co1 . N1 4_576 90.00(2) yes N21 6_756 Co1 . N1 . 90.00(2) yes N11 7_775 Co1 . N1 . 90.00(2) yes N1 4_576 Co1 . N1 . 179.995 yes N21 6_756 Co1 . N11 . 90.00(2) yes N11 7_775 Co1 . N11 . 179.995 yes N1 4_576 Co1 . N11 . 90.00(2) yes N1 . Co1 . N11 . 90.00(2) yes N21 6_756 Co1 . N21 . 179.995 yes N11 7_775 Co1 . N21 . 90.00(2) yes N1 4_576 Co1 . N21 . 90.00(2) yes N1 . Co1 . N21 . 90.00(2) yes N11 . Co1 . N21 . 90.00(2) yes Co1 . N1 . C1 . 179.990 yes Co1 . N11 . C12 6_756 122.8(5) yes Co1 . N11 . C12 . 122.8(5) yes C12 6_756 N11 . C12 . 114.3(9) yes Co1 . N21 . C22 4_576 122.3(5) yes Co1 . N21 . C22 . 122.3(5) yes C22 4_576 N21 . C22 . 115.5(10) yes C32 4_565 N31 . C32 6_655 114.5(19) yes C32 4_565 N31 . C32 7_665 123.7(19) yes C32 6_655 N31 . C32 7_665 91.8(20) yes C32 4_565 N31 . C32 . 91.8(20) yes C32 6_655 N31 . C32 . 123.7(19) yes C32 7_665 N31 . C32 . 114.5(19) yes Au1 . C1 . N1 . 179.990 yes Au2 . C2 . N2 . 176.4(14) yes N11 . C12 . C13 . 125.0(8) yes N11 . C12 . H121 . 116.9 no C13 . C12 . H121 . 118.1 no C12 . C13 . C14 . 119.0(8) yes C12 . C13 . H131 . 120.1 no C14 . C13 . H131 . 120.9 no C14 7_765 C14 . C13 6_756 121.2(5) yes C14 7_765 C14 . C13 . 121.2(5) yes C13 6_756 C14 . C13 . 117.5(11) yes N21 . C22 . C23 . 123.8(9) yes N21 . C22 . H221 . 117.5 no C23 . C22 . H221 . 118.6 no C22 . C23 . C24 . 120.8(9) yes C22 . C23 . H231 . 119.2 no C24 . C23 . H231 . 120.0 no C24 7_675 C24 . C23 4_576 122.4(6) yes C24 7_675 C24 . C23 . 122.4(6) yes C23 4_576 C24 . C23 . 115.3(11) yes N31 . C32 . C33 . 109(3) yes N31 . C32 . H321 . 110.5 no C33 . C32 . H321 . 106.7 no N31 . C32 . H322 . 110.1 no C33 . C32 . H322 . 110.7 no H321 . C32 . H322 . 109.5 no C32 . C33 . C34 . 105(3) yes C32 . C33 . H331 . 111.8 no C34 . C33 . H331 . 114.3 no C32 . C33 . H332 . 107.6 no C34 . C33 . H332 . 108.0 no H331 . C33 . H332 . 109.5 no C33 . C34 . C35 . 104(2) yes C33 . C34 . H341 . 108.7 no C35 . C34 . H341 . 109.9 no C33 . C34 . H342 . 114.5 no C35 . C34 . H342 . 110.2 no H341 . C34 . H342 . 109.5 no C34 . C35 . H351 . 110.9 no C34 . C35 . H352 . 108.9 no H351 . C35 . H352 . 109.5 no C34 . C35 . H353 . 108.6 no H351 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no data_ZnBipyAu3 _database_code_depnum_ccdc_archive 'CCDC 811555' #TrackingRef 'DLeznoff_AuBr2CN2_reduction.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C42 H52 Au3 Br6 N11 Zn1' _chemical_formula_moiety 'C42 H52 Au3 Br6 N11 Zn1' _chemical_formula_weight 1846.65 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c c m' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y,z+1/2 x,-y,-z+1/2 x,-y,z+1/2 -x,y,-z+1/2 -x,-y,z x,y,-z #------------------------------------------------ _cell_length_a 11.4507(19) _cell_length_b 11.4635(19) _cell_length_c 21.121(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2772.4(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2722 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 19.78 _cell_measurement_temperature 296(2) _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 2.212 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 12.703 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5041 _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 APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 296(2) _diffrn_reflns_number 31324 _diffrn_reflns_av_R_equivalents 0.104 _diffrn_reflns_theta_min 1.776 _diffrn_reflns_theta_max 28.601 _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.456 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 2019 _refine_ls_number_restraints 0 _refine_ls_number_parameters 158 _oxford_refine_ls_R_factor_ref 0.0343 _refine_ls_wR_factor_ref 0.0349 _refine_ls_goodness_of_fit_ref 1.0176 # The values computed from all data _oxford_reflns_number_all 3523 _refine_ls_R_factor_all 0.0822 _refine_ls_wR_factor_all 0.0582 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2126 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_gt 0.0364 _reflns_number_total 3523 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F) + ( 0.02P)^2^ + 0.00P] ,where P=(max(Fo,0) + 2Fc)/3 ; _refine_ls_shift/su_max 0.0002782 _refine_diff_density_min -0.97 _refine_diff_density_max 1.12 _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _oxford_refine_ls_scale 0.03838(6) _oxford_diffrn_Wilson_B_factor 2.94 _oxford_diffrn_Wilson_scale 1099.63 # Number of reflections with Friedels Law is 3523 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3454 #--------------------------------------------------------- _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 none # none if no extinction, _refine_ls_extinction_method None #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) CRYSTALS (Watkin, 1988) ; #=================================================================== # 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' 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' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 '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 # TODO check _oxford_atom_site_special_shape 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 1.0000 1.0000 0.5000 0.0289 1.0000 Uani S T . . . . . Au2 Au 0.31063(6) 0.76274(6) 0.5000 0.0688 1.0000 Uani S T . . . . . Br11 Br 0.79699(12) 0.93891(13) 0.5000 0.0540 1.0000 Uani S T . . . . . Br21 Br 0.10622(17) 0.70567(17) 0.5000 0.0995 1.0000 Uani S T . . . . . Br22 Br 0.5138(2) 0.8185(3) 0.5000 0.1409 1.0000 Uani S T . . . . . Zn1 Zn 1.0000 1.0000 0.7500 0.0256 1.0000 Uani S T . . . . . N1 N 1.0000 1.0000 0.6479(4) 0.0351 1.0000 Uani S T . . . . . N2 N 0.3165(12) 0.7563(12) 0.6458(7) 0.1122 1.0000 Uani . . . . . . . N11 N 1.0000 0.8100(8) 0.7500 0.0344 1.0000 Uani S T . . . . . N21 N 0.8091(8) 1.0000 0.7500 0.0306 1.0000 Uani S T . . . . . N31 N 0.5000 0.5000 0.2500 0.1393 1.0000 Uani S T . . . . . C1 C 1.0000 1.0000 0.5943(5) 0.0333 1.0000 Uani S T . . . . . C2 C 0.3140(12) 0.7597(12) 0.5944(7) 0.0807 1.0000 Uani . . . . . . . C12 C 1.0469(9) 0.7475(8) 0.7031(4) 0.0487 1.0000 Uani . . . . . . . C13 C 1.0452(10) 0.6284(8) 0.7008(5) 0.0599 1.0000 Uani . . . . . . . C14 C 1.0000 0.5645(10) 0.7500 0.0413 1.0000 Uani S T . . . . . C22 C 0.7470(8) 0.9628(9) 0.7002(4) 0.0436 1.0000 Uani . . . . . . . C23 C 0.6275(7) 0.9615(8) 0.6984(4) 0.0472 1.0000 Uani . . . . . . . C24 C 0.5643(9) 1.0000 0.7500 0.0376 1.0000 Uani S T . . . . . C32 C 0.571(2) 0.409(3) 0.2115(13) 0.2139 1.0000 Uani . . . . . . . C33 C 0.640(3) 0.444(3) 0.1672(14) 0.2371 1.0000 Uani . . . . . . . C34 C 0.719(2) 0.3391(19) 0.1383(15) 0.1819 1.0000 Uani . . . . . . . C35 C 0.775(2) 0.392(2) 0.0880(12) 0.2011 1.0000 Uani . . . . . . . H121 H 1.0832 0.7884 0.6698 0.044(12) 1.0000 Uiso R . . . . . . H131 H 1.0785 0.5900 0.6660 0.058(12) 1.0000 Uiso R . . . . . . H221 H 0.7889 0.9367 0.6652 0.038(12) 1.0000 Uiso R . . . . . . H231 H 0.5885 0.9349 0.6622 0.042(12) 1.0000 Uiso R . . . . . . H321 H 0.6166 0.3648 0.2408 0.38(6) 1.0000 Uiso R . . . . . . H322 H 0.5180 0.3583 0.1906 0.38(6) 1.0000 Uiso R . . . . . . H331 H 0.6923 0.4975 0.1870 0.38(6) 1.0000 Uiso R . . . . . . H332 H 0.5962 0.4840 0.1358 0.38(6) 1.0000 Uiso R . . . . . . H341 H 0.7755 0.3080 0.1669 0.34(6) 1.0000 Uiso R . . . . . . H342 H 0.6695 0.2783 0.1241 0.34(6) 1.0000 Uiso R . . . . . . H351 H 0.8214 0.3370 0.0653 0.35(6) 1.0000 Uiso R . . . . . . H352 H 0.8233 0.4527 0.1034 0.35(6) 1.0000 Uiso R . . . . . . H353 H 0.7172 0.4231 0.0606 0.35(6) 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 0.0290(4) 0.0362(4) 0.0214(2) 0.0000 0.0000 -0.0016(3) Au2 0.0521(4) 0.0562(4) 0.0981(5) 0.0000 0.0000 0.0078(3) Br11 0.0353(8) 0.0726(10) 0.0541(8) 0.0000 0.0000 -0.0127(7) Br21 0.0607(12) 0.0805(13) 0.157(2) 0.0000 0.0000 -0.0087(10) Br22 0.0588(14) 0.195(3) 0.169(2) 0.0000 0.0000 -0.0222(14) Zn1 0.0249(9) 0.0272(10) 0.0247(7) 0.0000 0.0000 0.0000 N1 0.027(5) 0.052(7) 0.026(4) 0.0000 0.0000 -0.002(5) N2 0.110(11) 0.088(9) 0.139(11) -0.006(9) 0.014(10) 0.005(8) N11 0.033(5) 0.028(5) 0.043(5) 0.0000 0.002(6) 0.0000 N21 0.025(5) 0.036(6) 0.031(5) -0.002(5) 0.0000 0.0000 N31 0.08(2) 0.20(4) 0.14(2) 0.0000 0.0000 0.0000 C1 0.023(6) 0.035(7) 0.042(6) 0.0000 0.0000 -0.009(5) C2 0.066(8) 0.072(9) 0.103(10) 0.009(9) 0.015(9) 0.013(7) C12 0.068(6) 0.030(5) 0.048(6) 0.005(5) 0.025(5) 0.001(5) C13 0.091(8) 0.035(6) 0.054(6) 0.000(5) 0.022(6) 0.004(6) C14 0.034(7) 0.031(7) 0.058(8) 0.0000 -0.002(7) 0.0000 C22 0.032(5) 0.061(6) 0.038(5) -0.011(4) 0.000(4) 0.003(4) C23 0.024(5) 0.077(7) 0.041(5) -0.014(5) -0.002(4) -0.008(5) C24 0.019(6) 0.062(9) 0.032(6) -0.007(7) 0.0000 0.0000 C32 0.17(3) 0.25(4) 0.23(3) -0.01(2) -0.06(2) 0.06(2) C33 0.23(3) 0.25(3) 0.23(3) 0.10(3) 0.10(2) 0.03(3) C34 0.19(3) 0.102(16) 0.25(3) 0.017(19) -0.04(2) 0.012(15) C35 0.29(4) 0.16(2) 0.15(2) -0.054(17) -0.01(2) -0.06(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 . Br11 2_776 2.4278(14) yes Au1 . C1 2_776 1.991(10) yes Au1 . Br11 . 2.4278(14) yes Au1 . C1 . 1.991(10) yes Au2 . C2 8_556 1.995(16) yes Au2 . Br21 . 2.430(2) yes Au2 . Br22 . 2.412(3) yes Au2 . C2 . 1.995(16) yes Br11 . Br22 . 3.525(3) yes Zn1 . N21 6_756 2.186(9) yes Zn1 . N11 7_775 2.178(9) yes Zn1 . N1 4_576 2.156(8) yes Zn1 . N1 . 2.156(8) yes Zn1 . N11 . 2.178(9) yes Zn1 . N21 . 2.186(9) yes N1 . C1 . 1.133(12) yes N2 . C2 . 1.086(16) yes N11 . C12 6_756 1.336(10) yes N11 . C12 . 1.336(10) yes N21 . C22 4_576 1.340(10) yes N21 . C22 . 1.340(10) yes N31 . C32 4_565 1.56(3) yes N31 . C32 6_655 1.56(3) yes N31 . C32 7_665 1.56(3) yes N31 . C32 . 1.56(3) yes C12 . C13 . 1.367(12) yes C12 . H121 . 0.941 no C13 . C14 . 1.373(12) yes C13 . H131 . 0.936 no C14 . C14 7_765 1.48(2) yes C22 . C23 . 1.369(11) yes C22 . H221 . 0.931 no C23 . C24 . 1.381(10) yes C23 . H231 . 0.935 no C24 . C24 7_675 1.47(2) yes C32 . C33 . 1.29(3) yes C32 . H321 . 0.950 no C32 . H322 . 0.950 no C33 . C34 . 1.63(3) yes C33 . H331 . 0.950 no C33 . H332 . 0.950 no C34 . C35 . 1.38(3) yes C34 . H341 . 0.950 no C34 . H342 . 0.950 no C35 . H351 . 0.950 no C35 . H352 . 0.950 no C35 . H353 . 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 Br11 2_776 Au1 . C1 2_776 90.000(13) yes Br11 2_776 Au1 . Br11 . 179.995 yes C1 2_776 Au1 . Br11 . 90.000(13) yes Br11 2_776 Au1 . C1 . 90.000(13) yes C1 2_776 Au1 . C1 . 179.994 yes Br11 . Au1 . C1 . 90.000(13) yes C2 8_556 Au2 . Br21 . 90.8(4) yes C2 8_556 Au2 . Br22 . 89.2(4) yes Br21 . Au2 . Br22 . 179.76(9) yes C2 8_556 Au2 . C2 . 177.0(8) yes Br21 . Au2 . C2 . 90.8(4) yes Br22 . Au2 . C2 . 89.2(4) yes Au1 . Br11 . Br22 . 173.72(8) yes Au2 . Br22 . Br11 . 172.33(13) yes N21 6_756 Zn1 . N11 7_775 90.000(13) yes N21 6_756 Zn1 . N1 4_576 90.000(13) yes N11 7_775 Zn1 . N1 4_576 90.000(13) yes N21 6_756 Zn1 . N1 . 90.000(13) yes N11 7_775 Zn1 . N1 . 90.000(13) yes N1 4_576 Zn1 . N1 . 179.995 yes N21 6_756 Zn1 . N11 . 90.000(13) yes N11 7_775 Zn1 . N11 . 179.995 yes N1 4_576 Zn1 . N11 . 90.000(13) yes N1 . Zn1 . N11 . 90.000(13) yes N21 6_756 Zn1 . N21 . 179.995 yes N11 7_775 Zn1 . N21 . 90.000(13) yes N1 4_576 Zn1 . N21 . 90.000(13) yes N1 . Zn1 . N21 . 90.000(13) yes N11 . Zn1 . N21 . 90.000(13) yes Zn1 . N1 . C1 . 179.990 yes Zn1 . N11 . C12 6_756 122.5(5) yes Zn1 . N11 . C12 . 122.5(5) yes C12 6_756 N11 . C12 . 115.1(10) yes Zn1 . N21 . C22 4_576 122.0(5) yes Zn1 . N21 . C22 . 122.0(5) yes C22 4_576 N21 . C22 . 115.9(10) yes C32 4_565 N31 . C32 6_655 117.1(20) yes C32 4_565 N31 . C32 7_665 95(3) yes C32 6_655 N31 . C32 7_665 117(2) yes C32 4_565 N31 . C32 . 117(2) yes C32 6_655 N31 . C32 . 95(3) yes C32 7_665 N31 . C32 . 117.1(20) yes Au1 . C1 . N1 . 179.990 yes Au2 . C2 . N2 . 178.9(15) yes N11 . C12 . C13 . 123.8(9) yes N11 . C12 . H121 . 117.6 no C13 . C12 . H121 . 118.5 no C12 . C13 . C14 . 120.7(9) yes C12 . C13 . H131 . 119.4 no C14 . C13 . H131 . 119.8 no C14 7_765 C14 . C13 . 122.2(6) yes C14 7_765 C14 . C13 6_756 122.2(6) yes C13 . C14 . C13 6_756 115.6(12) yes N21 . C22 . C23 . 123.7(8) yes N21 . C22 . H221 . 116.9 no C23 . C22 . H221 . 119.4 no C22 . C23 . C24 . 119.9(9) yes C22 . C23 . H231 . 120.2 no C24 . C23 . H231 . 120.0 no C24 7_675 C24 . C23 4_576 121.6(5) yes C24 7_675 C24 . C23 . 121.6(5) yes C23 4_576 C24 . C23 . 116.9(10) yes N31 . C32 . C33 . 119(3) yes N31 . C32 . H321 . 107.6 no C33 . C32 . H321 . 107.9 no N31 . C32 . H322 . 108.3 no C33 . C32 . H322 . 104.3 no H321 . C32 . H322 . 109.5 no C32 . C33 . C34 . 112(3) yes C32 . C33 . H331 . 105.5 no C34 . C33 . H331 . 107.0 no C32 . C33 . H332 . 109.4 no C34 . C33 . H332 . 113.0 no H331 . C33 . H332 . 109.5 no C33 . C34 . C35 . 103(2) yes C33 . C34 . H341 . 114.6 no C35 . C34 . H341 . 110.0 no C33 . C34 . H342 . 109.0 no C35 . C34 . H342 . 110.7 no H341 . C34 . H342 . 109.5 no C34 . C35 . H351 . 111.0 no C34 . C35 . H352 . 109.0 no H351 . C35 . H352 . 109.5 no C34 . C35 . H353 . 108.3 no H351 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no data_ZnBipyAu1 _database_code_depnum_ccdc_archive 'CCDC 811556' #TrackingRef 'DLeznoff_AuBr2CN2_reduction.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C13.32 H8 Au2 Br0.68 N5.32 Zn1' _chemical_formula_moiety 'C13.32 H8 Au2 Br0.68 N5.32 Zn1' _chemical_formula_weight 756.21 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y,-z+1/2 -x+1/2,-y,z+1/2 x,-y+1/2,z -x,y+1/2,-z -x+1/2,y+1/2,z+1/2 x+1/2,-y+1/2,-z+1/2 #------------------------------------------------ _cell_length_a 11.59130(10) _cell_length_b 9.90550(10) _cell_length_c 14.6572(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1682.90(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3767 _cell_measurement_theta_min 3.54 _cell_measurement_theta_max 34.27 _cell_measurement_temperature 296(2) _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 2.983 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1347.189 _exptl_absorpt_coefficient_mu 20.405 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4176 _exptl_absorpt_correction_T_max 0.7468 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 296(2) _diffrn_reflns_number 26830 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min 2.240 _diffrn_reflns_theta_max 34.830 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 34.133 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 2304 _refine_ls_number_restraints 28 _refine_ls_number_parameters 129 _oxford_refine_ls_R_factor_ref 0.0287 _refine_ls_wR_factor_ref 0.0354 _refine_ls_goodness_of_fit_ref 1.0723 # The values computed from all data _oxford_reflns_number_all 3816 _refine_ls_R_factor_all 0.0605 _refine_ls_wR_factor_all 0.0505 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2386 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_gt 0.0362 _reflns_number_total 3816 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F) + ( 0.00P)^2^ + 0.05P] ,where P=(max(Fo,0) + 2Fc)/3 ; _refine_ls_shift/su_max 0.0073518 _refine_diff_density_min -1.60 _refine_diff_density_max 1.68 _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_refine_ls_scale 0.05704(8) _oxford_diffrn_Wilson_B_factor 2.91 _oxford_diffrn_Wilson_scale 358.50 # Number of reflections with Friedels Law is 3816 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3652 #--------------------------------------------------------- _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 none # none if no extinction, _refine_ls_extinction_method None #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) CRYSTALS (Watkin, 1988) ; #=================================================================== # 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' 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' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 '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 # TODO check _oxford_atom_site_special_shape 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 0.41389(2) 0.2500 0.27301(2) 0.0409 1.0000 Uani DS TU . . . . . Au2 Au 0.32470(2) 0.7500 0.67470(3) 0.0419 1.0000 Uani S T . . . . . Br1 Br 0.49608(15) 0.2500 0.12300(11) 0.0573 0.673(5) Uani DS T P . 1 . . Zn1 Zn 0.31705(7) 0.2500 0.60848(7) 0.0349 1.0000 Uani S T . . . . . N1 N 0.5149(6) 0.2500 0.0794(6) 0.0831 0.327(5) Uani DS TU P . 2 . . N2 N 0.3278(4) 0.2500 0.4725(4) 0.0515 1.0000 Uani DS TU . . . . . N3 N 0.3226(4) 0.4371(5) 0.6597(4) 0.0497 1.0000 Uani . . . . . . . N11 N 0.5146(5) 0.2500 0.6142(5) 0.0450 1.0000 Uani S T . . . . . N18 N 1.1288(5) 0.2500 0.6148(5) 0.0343 1.0000 Uani S T . . . . . C1 C 0.4801(5) 0.2500 0.1533(6) 0.0665 0.327(5) Uani DS TU P . 2 . . C2 C 0.3569(3) 0.2500 0.3966(4) 0.0441 1.0000 Uani DS TU . . . . . C3 C 0.3234(4) 0.5498(6) 0.6677(5) 0.0448 1.0000 Uani . . . . . . . C12 C 0.5764(5) 0.3601(7) 0.6133(8) 0.0864 1.0000 Uani . . . . . . . C13 C 0.6950(5) 0.3665(7) 0.6123(7) 0.0847 1.0000 Uani . . . . . . . C14 C 0.7580(6) 0.2500 0.6121(6) 0.0374 1.0000 Uani S T . . . . . C15 C 0.8861(6) 0.2500 0.6129(5) 0.0347 1.0000 Uani S T . . . . . C16 C 0.9495(4) 0.3689(6) 0.6135(5) 0.0446 1.0000 Uani . . . . . . . C17 C 1.0690(4) 0.3637(6) 0.6155(5) 0.0479 1.0000 Uani . . . . . . . H121 H 0.5354 0.4402 0.6114 0.085(13) 1.0000 Uiso R . . . . . . H131 H 0.7328 0.4505 0.6114 0.085(13) 1.0000 Uiso R . . . . . . H161 H 0.9115 0.4517 0.6135 0.085(13) 1.0000 Uiso R . . . . . . H171 H 1.1106 0.4442 0.6166 0.085(13) 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 0.03035(14) 0.04934(17) 0.04297(19) 0.0000 -0.00196(12) 0.0000 Au2 0.02906(13) 0.03016(13) 0.0664(2) 0.0000 0.00093(13) 0.0000 Br1 0.0688(11) 0.0626(10) 0.0406(11) 0.0000 0.0072(8) 0.0000 Zn1 0.0282(4) 0.0280(4) 0.0486(6) 0.0000 0.0017(4) 0.0000 N1 0.081(17) 0.12(2) 0.050(13) 0.0000 0.001(13) 0.0000 N2 0.036(4) 0.073(5) 0.046(4) 0.0000 -0.001(3) 0.0000 N3 0.028(2) 0.038(2) 0.083(4) -0.012(3) -0.002(2) -0.0029(18) N11 0.024(3) 0.049(4) 0.062(5) 0.0000 -0.002(3) 0.0000 N18 0.020(2) 0.035(3) 0.047(4) 0.0000 -0.001(2) 0.0000 C1 0.057(13) 0.088(16) 0.055(11) 0.0000 0.011(11) 0.0000 C2 0.027(3) 0.061(5) 0.044(4) 0.0000 -0.001(3) 0.0000 C3 0.025(2) 0.037(3) 0.072(4) -0.009(3) 0.000(2) -0.0002(19) C12 0.025(3) 0.045(3) 0.190(11) 0.017(5) 0.002(4) 0.008(2) C13 0.026(3) 0.038(3) 0.189(10) 0.014(5) 0.003(4) -0.001(2) C14 0.020(3) 0.042(4) 0.050(5) 0.0000 0.000(3) 0.0000 C15 0.026(3) 0.048(4) 0.031(4) 0.0000 -0.002(3) 0.0000 C16 0.026(2) 0.038(3) 0.070(4) -0.006(3) -0.001(2) 0.0011(19) C17 0.026(2) 0.042(3) 0.076(5) -0.003(3) -0.004(3) -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 . Au2 7_544 3.1184(4) yes Au1 . Au2 6_646 3.1256(4) yes Au1 . Br1 . 2.3961(16) yes Au1 . C2 . 1.928(7) yes Au2 . C3 5_565 1.985(6) yes Au2 . C3 . 1.985(6) yes Zn1 . N18 1_455 2.184(6) yes Zn1 . N3 5_555 2.000(5) yes Zn1 . N2 . 1.998(6) yes Zn1 . N3 . 2.000(5) yes Zn1 . N11 . 2.291(6) yes N1 . C1 . 1.156(14) yes N2 . C2 . 1.162(9) yes N3 . C3 . 1.123(7) yes N11 . C12 5_555 1.305(7) yes N11 . C12 . 1.305(7) yes N18 . C17 5_555 1.323(6) yes N18 . C17 . 1.323(6) yes C12 . C13 . 1.377(8) yes C12 . H121 . 0.925 no C13 . C14 . 1.366(7) yes C13 . H131 . 0.940 no C14 . C15 . 1.484(10) yes C15 . C16 5_555 1.388(6) yes C15 . C16 . 1.388(6) yes C16 . C17 . 1.386(7) yes C16 . H161 . 0.930 no C17 . H171 . 0.932 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 7_544 Au1 . Au2 6_646 166.675(13) yes Au2 7_544 Au1 . Br1 . 85.91(4) yes Au2 6_646 Au1 . Br1 . 80.77(4) yes Au2 7_544 Au1 . C2 . 97.47(8) yes Au2 6_646 Au1 . C2 . 95.85(8) yes Br1 . Au1 . C2 . 176.62(8) yes C3 5_565 Au2 . Au1 7_555 90.99(15) yes C3 5_565 Au2 . Au1 6_656 91.15(14) yes Au1 7_555 Au2 . Au1 6_656 138.283(13) yes C3 5_565 Au2 . C3 . 174.0(4) yes Au1 7_555 Au2 . C3 . 90.99(15) yes Au1 6_656 Au2 . C3 . 91.15(14) yes N18 1_455 Zn1 . N3 5_555 90.91(14) yes N18 1_455 Zn1 . N2 . 96.0(2) yes N3 5_555 Zn1 . N2 . 111.86(18) yes N18 1_455 Zn1 . N3 . 90.91(14) yes N3 5_555 Zn1 . N3 . 135.8(4) yes N2 . Zn1 . N3 . 111.86(18) yes N18 1_455 Zn1 . N11 . 175.5(3) yes N3 5_555 Zn1 . N11 . 87.39(14) yes N2 . Zn1 . N11 . 88.5(2) yes N3 . Zn1 . N11 . 87.39(14) yes Zn1 . N2 . C2 . 166.8(2) yes Zn1 . N3 . C3 . 163.9(7) yes Zn1 . N11 . C12 5_555 123.2(3) yes Zn1 . N11 . C12 . 123.2(3) yes C12 5_555 N11 . C12 . 113.4(7) yes Zn1 1_655 N18 . C17 5_555 121.6(3) yes Zn1 1_655 N18 . C17 . 121.6(3) yes C17 5_555 N18 . C17 . 116.7(6) yes N1 . C1 . Au1 . 176.82(10) yes N2 . C2 . Au1 . 176.77(10) yes Au2 . C3 . N3 . 177.0(7) yes N11 . C12 . C13 . 125.9(6) yes N11 . C12 . H121 . 115.8 no C13 . C12 . H121 . 118.2 no C12 . C13 . C14 . 119.7(6) yes C12 . C13 . H131 . 120.4 no C14 . C13 . H131 . 119.9 no C13 . C14 . C13 5_555 115.4(7) yes C13 . C14 . C15 . 122.3(3) yes C13 5_555 C14 . C15 . 122.3(3) yes C14 . C15 . C16 5_555 122.0(3) yes C14 . C15 . C16 . 122.0(3) yes C16 5_555 C15 . C16 . 116.1(6) yes C15 . C16 . C17 . 119.8(5) yes C15 . C16 . H161 . 119.8 no C17 . C16 . H161 . 120.3 no C16 . C17 . N18 . 123.7(5) yes C16 . C17 . H171 . 119.1 no N18 . C17 . H171 . 117.2 no