#------------------------------------------------------------------------------ #$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $ #$Revision: 176453 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/01/56/7015615.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7015615 loop_ _publ_author_name 'Ovens, Jeffrey S.' 'Leznoff, Daniel B.' _publ_section_title ; Thermally triggered reductive elimination of bromine from Au(III) as a path to Au(I)-based coordination polymers. ; _journal_issue 16 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 4140 _journal_page_last 4146 _journal_paper_doi 10.1039/c0dt01772h _journal_volume 40 _journal_year 2011 _chemical_formula_moiety 'C13.32 H8 Au2 Br0.68 N5.32 Zn1' _chemical_formula_sum 'C13.32 H8 Au2 Br0.68 N5.32 Zn' _chemical_formula_weight 756.21 _chemical_name_systematic ? _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.59130(10) _cell_length_b 9.90550(10) _cell_length_c 14.6572(2) _cell_measurement_reflns_used 3767 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 34.27 _cell_measurement_theta_min 3.54 _cell_volume 1682.90(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) CRYSTALS (Watkin, 1988) ; _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 26830 _diffrn_reflns_theta_full 34.133 _diffrn_reflns_theta_max 34.830 _diffrn_reflns_theta_min 2.240 _exptl_absorpt_coefficient_mu 20.405 _exptl_absorpt_correction_T_max 0.7468 _exptl_absorpt_correction_T_min 0.4176 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.983 _exptl_crystal_description plate _exptl_crystal_F_000 1347.189 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.68 _refine_diff_density_min -1.60 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.0723 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 129 _refine_ls_number_reflns 2304 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0301 _refine_ls_shift/su_max 0.0073518 _refine_ls_structure_factor_coef F _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_weighting_scheme calc _refine_ls_wR_factor_all 0.0505 _refine_ls_wR_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0354 _reflns_limit_h_max 18 _reflns_limit_h_min 0 _reflns_limit_k_max 15 _reflns_limit_k_min 0 _reflns_limit_l_max 23 _reflns_limit_l_min 0 _reflns_number_gt 2386 _reflns_number_total 3816 _reflns_threshold_expression I>2.0\s(I) _oxford_diffrn_Wilson_B_factor 2.91 _oxford_diffrn_Wilson_scale 358.50 _oxford_refine_ls_r_factor_ref 0.0287 _oxford_refine_ls_scale 0.05704(8) _oxford_reflns_number_all 3816 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _cod_data_source_file c0dt01772h.txt _cod_data_source_block ZnBipyAu1 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius ; _cod_original_formula_sum 'C13.32 H8 Au2 Br0.68 N5.32 Zn1' _cod_database_code 7015615 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 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_ _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' 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 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