#------------------------------------------------------------------------------ #$Date: 2011-06-21 23:26:54 +0300 (Tue, 21 Jun 2011) $ #$Revision: 21204 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/7015613.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_7015613 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_volume 40 _journal_year 2011 _chemical_formula_moiety 'C42 H52 Au3 Br6 Co1 N11' _chemical_formula_sum 'C42 H52 Au3 Br6 Co N11' _chemical_formula_weight 1840.20 _chemical_name_systematic ; ; _space_group_IT_number 49 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2 2c' _symmetry_space_group_name_H-M 'P c c m' _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 2 _cell_length_a 11.450(3) _cell_length_b 11.467(3) _cell_length_c 20.944(5) _cell_measurement_reflns_used 1464 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 22.20 _cell_measurement_theta_min 2.51 _cell_volume 2749.9(12) _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 0.996 _diffrn_measured_fraction_theta_max 0.942 _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 0.100 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3392 _diffrn_reflns_theta_full 31.026 _diffrn_reflns_theta_max 28.506 _diffrn_reflns_theta_min 1.776 _exptl_absorpt_coefficient_mu 12.672 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.4475 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour amber _exptl_crystal_density_diffrn 2.222 _exptl_crystal_description block _exptl_crystal_F_000 1710 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.94 _refine_diff_density_min -0.94 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.0261 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 158 _refine_ls_number_reflns 1875 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0386 _refine_ls_shift/su_max 0.0004279 _refine_ls_structure_factor_coef F _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_weighting_scheme calc _refine_ls_wR_factor_all 0.0611 _refine_ls_wR_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0369 _reflns_limit_h_max 14 _reflns_limit_h_min 0 _reflns_limit_k_max 14 _reflns_limit_k_min 0 _reflns_limit_l_max 28 _reflns_limit_l_min 0 _reflns_number_gt 1986 _reflns_number_total 3392 _reflns_threshold_expression I>2.0\s(I) _oxford_diffrn_Wilson_B_factor 3.10 _oxford_diffrn_Wilson_scale 972.38 _oxford_refine_ls_r_factor_ref 0.0358 _oxford_refine_ls_scale 0.03929(7) _oxford_reflns_number_all 3392 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _[local]_cod_data_source_file c0dt01772h.txt _[local]_cod_data_source_block CoBipyAu3 _[local]_cod_chemical_formula_sum_orig 'C42 H52 Au3 Br6 Co1 N11' _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_cell_volume 2750.0(12) _cod_database_code 7015613 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 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_ _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' 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 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