#------------------------------------------------------------------------------ #$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $ #$Revision: 176467 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/31/68/4316837.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_4316837 loop_ _publ_author_name 'Jeffrey S. Ovens' 'Andrew R. Geisheimer' 'Alexei A. Bokov' 'Zuo-Guang Ye' '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_email dleznoff@sfu.ca _publ_contact_author_fax +1-778-782-3765 _publ_contact_author_name 'Daniel B. Leznoff' _publ_contact_author_phone +1-778-782-4887 _publ_section_title ; The Use of Polarizable [AuX2(CN)2]- (X = Br, I) Building Blocks Toward the Formation of Birefringent Coordination Polymers ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 9609 _journal_page_last 9616 _journal_paper_doi 10.1021/ic101357y _journal_volume 49 _journal_year 2010 _chemical_formula_moiety 'C19 H11 Au2 Br4 Cu1 N7' _chemical_formula_sum 'C19 H11 Au2 Br4 Cu N7' _chemical_formula_weight 1114.44 _chemical_name_systematic ? _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _cell_angle_alpha 90 _cell_angle_beta 94.091(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.6901(3) _cell_length_b 16.0919(6) _cell_length_c 20.6901(7) _cell_measurement_reflns_used 9892 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 32.48 _cell_measurement_theta_min 2.53 _cell_volume 2553.84(16) _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 293 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.913 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.062 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 32955 _diffrn_reflns_theta_full 30.568 _diffrn_reflns_theta_max 35.962 _diffrn_reflns_theta_min 1.605 _exptl_absorpt_coefficient_mu 18.567 _exptl_absorpt_correction_T_max 0.7471 _exptl_absorpt_correction_T_min 0.3858 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour green _exptl_crystal_density_diffrn 2.898 _exptl_crystal_description plate _exptl_crystal_F_000 2004 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _refine_diff_density_max 2.50 _refine_diff_density_min -2.68 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.0402 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 299 _refine_ls_number_reflns 4456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1522 _refine_ls_R_factor_gt 0.0527 _refine_ls_shift/su_max 0.0009422 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F) + ( 0.02P)^2^ + 0.10P] ,where P=(max(Fo,0) + 2Fc)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1044 _refine_ls_wR_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.0528 _reflns_limit_h_max 12 _reflns_limit_h_min -12 _reflns_limit_k_max 25 _reflns_limit_k_min 0 _reflns_limit_l_max 33 _reflns_limit_l_min 0 _reflns_number_gt 4872 _reflns_number_total 11019 _reflns_threshold_expression I>2.0\s(I) _oxford_diffrn_Wilson_B_factor 2.36 _oxford_diffrn_Wilson_scale 667.87 _oxford_refine_ls_r_factor_ref 0.0459 _oxford_refine_ls_scale 0.04852(8) _oxford_reflns_number_all 11019 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _cod_data_source_file ic101357y_si_001_9.cif _cod_data_source_block CuTerpy _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to the built-in table from CIF Core 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 the built-in table from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_original_formula_sum 'C19 H11 Au2 Br4 Cu1 N7' _cod_database_code 4316837 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 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 -0.17364(5) 0.81818(3) 0.312648(18) 0.0370 1.0000 Uani . . . . . . . Au2 Au 0.14625(5) 0.54048(3) 0.261285(18) 0.0399 1.0000 Uani . . . . . . . Br1 Br 0.10453(18) 0.74768(10) 0.32027(7) 0.0689 1.0000 Uani . . . . . . . Br2 Br -0.46109(16) 0.87964(9) 0.30448(6) 0.0604 1.0000 Uani . . . . . . . Br3 Br 0.41604(16) 0.61373(9) 0.24548(6) 0.0586 1.0000 Uani . . . . . . . Br4 Br -0.1255(2) 0.47078(10) 0.27696(8) 0.0736 1.0000 Uani . . . . . . . Cu1 Cu -0.14277(16) 0.70232(8) 0.07916(6) 0.0375 1.0000 Uani . . . . . . . N1 N -0.2330(13) 0.7573(7) 0.1690(5) 0.0571 1.0000 Uani . . . . . . . N2 N -0.0936(13) 0.8902(7) 0.4516(5) 0.0558 1.0000 Uani . . . . . . . N3 N -0.0236(12) 0.6134(6) 0.1326(5) 0.0467 1.0000 Uani . . . . . . . N4 N 0.2882(17) 0.4816(8) 0.3986(5) 0.0790 1.0000 Uani . . . . . . . N10 N 0.0646(11) 0.7800(5) 0.0759(4) 0.0375 1.0000 Uani . . . . . . . N20 N -0.2275(11) 0.7744(5) 0.0090(4) 0.0352 1.0000 Uani . . . . . . . N30 N -0.3723(11) 0.6460(6) 0.0553(4) 0.0364 1.0000 Uani . . . . . . . C1 C -0.2173(15) 0.7773(8) 0.2226(5) 0.0457 1.0000 Uani . . . . . . . C2 C -0.1221(14) 0.8636(7) 0.4013(5) 0.0386 1.0000 Uani . . . . . . . C3 C 0.0444(14) 0.5833(7) 0.1768(5) 0.0425 1.0000 Uani . . . . . . . C4 C 0.2411(16) 0.5010(8) 0.3483(6) 0.0555 1.0000 Uani . . . . . . . C11 C 0.2107(16) 0.7817(8) 0.1150(6) 0.0521 1.0000 Uani . . . . . . . C12 C 0.3436(16) 0.8353(8) 0.1083(7) 0.0572 1.0000 Uani . . . . . . . C13 C 0.3259(17) 0.8927(9) 0.0600(6) 0.0605 1.0000 Uani . . . . . . . C14 C 0.1732(16) 0.8947(8) 0.0193(6) 0.0529 1.0000 Uani . . . . . . . C15 C 0.0458(14) 0.8387(7) 0.0293(5) 0.0390 1.0000 Uani . . . . . . . C21 C -0.1231(14) 0.8340(6) -0.0109(5) 0.0366 1.0000 Uani . . . . . . . C22 C -0.1770(16) 0.8841(7) -0.0630(5) 0.0481 1.0000 Uani . . . . . . . C23 C -0.3380(18) 0.8688(8) -0.0927(5) 0.0549 1.0000 Uani . . . . . . . C24 C -0.4424(16) 0.8058(8) -0.0733(5) 0.0507 1.0000 Uani . . . . . . . C25 C -0.3841(14) 0.7576(6) -0.0209(4) 0.0363 1.0000 Uani . . . . . . . C31 C -0.4712(14) 0.6852(7) 0.0063(5) 0.0408 1.0000 Uani . . . . . . . C32 C -0.6325(14) 0.6562(7) -0.0151(5) 0.0454 1.0000 Uani . . . . . . . C33 C -0.6979(16) 0.5857(8) 0.0144(6) 0.0555 1.0000 Uani . . . . . . . C34 C -0.5982(16) 0.5479(8) 0.0656(6) 0.0543 1.0000 Uani . . . . . . . C35 C -0.4383(15) 0.5810(8) 0.0838(5) 0.0467 1.0000 Uani . . . . . . . H111 H 0.2216 0.7430 0.1484 0.053(11) 1.0000 Uiso R . . . . . . H121 H 0.4427 0.8341 0.1367 0.060(11) 1.0000 Uiso R . . . . . . H131 H 0.4161 0.9296 0.0534 0.066(11) 1.0000 Uiso R . . . . . . H141 H 0.1586 0.9334 -0.0141 0.054(11) 1.0000 Uiso R . . . . . . H221 H -0.1061 0.9264 -0.0769 0.052(11) 1.0000 Uiso R . . . . . . H231 H -0.3794 0.9020 -0.1271 0.053(11) 1.0000 Uiso R . . . . . . H241 H -0.5500 0.7955 -0.0951 0.050(11) 1.0000 Uiso R . . . . . . H321 H -0.6983 0.6830 -0.0485 0.049(11) 1.0000 Uiso R . . . . . . H331 H -0.8048 0.5632 -0.0001 0.059(11) 1.0000 Uiso R . . . . . . H341 H -0.6418 0.5031 0.0876 0.058(11) 1.0000 Uiso R . . . . . . H351 H -0.3699 0.5549 0.1170 0.049(11) 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 0.0354(2) 0.0433(3) 0.03182(19) -0.00326(18) -0.00060(15) 0.00011(19) Au2 0.0393(2) 0.0456(3) 0.0335(2) 0.00079(19) -0.00647(16) 0.00992(19) Br1 0.0479(8) 0.0878(11) 0.0690(8) -0.0223(8) -0.0095(6) 0.0217(7) Br2 0.0447(7) 0.0789(9) 0.0561(7) -0.0101(7) -0.0054(6) 0.0162(6) Br3 0.0386(7) 0.0850(10) 0.0511(7) -0.0036(7) -0.0047(5) -0.0006(6) Br4 0.0626(9) 0.0784(10) 0.0796(10) 0.0121(8) 0.0035(7) -0.0156(8) Cu1 0.0320(7) 0.0496(8) 0.0294(6) 0.0055(6) -0.0079(5) -0.0020(6) N1 0.048(6) 0.083(8) 0.041(5) -0.013(5) 0.001(4) 0.004(5) N2 0.045(6) 0.074(8) 0.048(6) -0.009(5) -0.001(5) -0.005(5) N3 0.038(5) 0.050(6) 0.051(6) 0.003(5) -0.004(4) -0.003(5) N4 0.096(10) 0.103(10) 0.037(6) 0.005(6) -0.004(6) 0.026(8) N10 0.036(5) 0.038(5) 0.037(5) -0.001(4) -0.007(4) 0.003(4) N20 0.039(5) 0.042(5) 0.024(4) -0.003(4) -0.005(3) 0.007(4) N30 0.032(5) 0.051(6) 0.024(4) 0.004(4) -0.008(3) -0.001(4) C1 0.043(7) 0.058(8) 0.037(6) -0.004(6) 0.005(5) 0.005(6) C2 0.034(6) 0.045(7) 0.037(6) -0.005(5) 0.002(4) 0.001(5) C3 0.039(6) 0.046(7) 0.041(6) 0.011(5) -0.005(5) 0.007(5) C4 0.053(8) 0.061(8) 0.051(7) 0.005(7) -0.004(6) 0.018(6) C11 0.046(7) 0.056(8) 0.053(7) 0.005(6) -0.010(6) 0.001(6) C12 0.035(7) 0.068(9) 0.067(8) -0.009(7) -0.008(6) -0.003(6) C13 0.046(8) 0.070(9) 0.066(8) -0.009(7) 0.006(6) -0.016(7) C14 0.048(7) 0.059(8) 0.052(7) -0.006(6) 0.010(6) -0.009(6) C15 0.042(6) 0.038(6) 0.036(5) -0.004(5) -0.001(4) -0.003(5) C21 0.045(6) 0.032(6) 0.033(5) -0.002(4) 0.000(4) 0.000(5) C22 0.060(8) 0.046(7) 0.037(6) 0.004(5) -0.002(5) 0.000(6) C23 0.072(9) 0.053(8) 0.037(6) 0.013(6) -0.015(6) 0.001(7) C24 0.048(7) 0.065(9) 0.036(6) 0.001(6) -0.016(5) 0.010(6) C25 0.038(6) 0.040(6) 0.029(5) -0.005(4) -0.010(4) 0.006(5) C31 0.034(6) 0.052(7) 0.036(5) -0.004(5) -0.003(4) 0.004(5) C32 0.035(6) 0.053(7) 0.047(6) 0.001(6) -0.008(5) 0.003(5) C33 0.040(7) 0.068(9) 0.057(7) -0.014(7) -0.008(6) -0.007(6) C34 0.052(8) 0.054(8) 0.056(7) 0.007(6) -0.002(6) -0.020(6) C35 0.040(7) 0.062(8) 0.037(6) 0.008(6) 0.003(5) -0.010(6) 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' 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' 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 Br1 . Au1 . Br2 . 176.15(5) yes Br1 . Au1 . C1 . 89.7(3) yes Br2 . Au1 . C1 . 88.7(3) yes Br1 . Au1 . C2 . 89.7(3) yes Br2 . Au1 . C2 . 92.0(3) yes C1 . Au1 . C2 . 177.1(5) yes Br3 . Au2 . Br4 . 178.64(5) yes Br3 . Au2 . C3 . 90.0(3) yes Br4 . Au2 . C3 . 89.4(3) yes Br3 . Au2 . C4 . 90.9(4) yes Br4 . Au2 . C4 . 89.7(4) yes C3 . Au2 . C4 . 177.3(5) yes Au1 . Br1 . Br3 . 148.73(5) yes Au2 . Br3 . Br1 . 68.68(4) yes N1 . Cu1 . N3 . 88.9(4) yes N1 . Cu1 . N10 . 94.4(4) yes N3 . Cu1 . N10 . 97.4(4) yes N1 . Cu1 . N20 . 106.3(4) yes N3 . Cu1 . N20 . 164.7(4) yes N10 . Cu1 . N20 . 80.2(3) yes N1 . Cu1 . N30 . 93.7(4) yes N3 . Cu1 . N30 . 100.0(4) yes N10 . Cu1 . N30 . 160.9(3) yes N20 . Cu1 . N30 . 81.0(4) yes Cu1 . N1 . C1 . 154.3(9) yes Cu1 . N3 . C3 . 157.7(10) yes Cu1 . N10 . C11 . 128.3(8) yes Cu1 . N10 . C15 . 114.2(7) yes C11 . N10 . C15 . 117.5(10) yes Cu1 . N20 . C21 . 119.0(7) yes Cu1 . N20 . C25 . 117.9(7) yes C21 . N20 . C25 . 122.9(9) yes Cu1 . N30 . C31 . 113.8(7) yes Cu1 . N30 . C35 . 127.2(7) yes C31 . N30 . C35 . 118.9(9) yes Au1 . C1 . N1 . 175.0(11) yes Au1 . C2 . N2 . 179.3(10) yes Au2 . C3 . N3 . 172.6(10) yes Au2 . C4 . N4 . 176.3(12) yes N10 . C11 . C12 . 124.0(12) yes N10 . C11 . H111 . 117.7 no C12 . C11 . H111 . 118.3 no C11 . C12 . C13 . 118.2(12) yes C11 . C12 . H121 . 121.0 no C13 . C12 . H121 . 120.8 no C12 . C13 . C14 . 119.6(12) yes C12 . C13 . H131 . 120.4 no C14 . C13 . H131 . 120.0 no C13 . C14 . C15 . 118.5(12) yes C13 . C14 . H141 . 121.0 no C15 . C14 . H141 . 120.4 no C14 . C15 . N10 . 122.1(10) yes C14 . C15 . C21 . 123.8(10) yes N10 . C15 . C21 . 114.1(9) yes C15 . C21 . N20 . 112.5(9) yes C15 . C21 . C22 . 127.2(10) yes N20 . C21 . C22 . 120.3(10) yes C21 . C22 . C23 . 117.2(11) yes C21 . C22 . H221 . 121.2 no C23 . C22 . H221 . 121.6 no C22 . C23 . C24 . 122.1(11) yes C22 . C23 . H231 . 119.6 no C24 . C23 . H231 . 118.3 no C23 . C24 . C25 . 118.8(11) yes C23 . C24 . H241 . 120.6 no C25 . C24 . H241 . 120.6 no C24 . C25 . N20 . 118.6(10) yes C24 . C25 . C31 . 127.7(10) yes N20 . C25 . C31 . 113.6(8) yes C25 . C31 . N30 . 113.6(9) yes C25 . C31 . C32 . 124.8(10) yes N30 . C31 . C32 . 121.5(10) yes C31 . C32 . C33 . 118.7(10) yes C31 . C32 . H321 . 120.9 no C33 . C32 . H321 . 120.4 no C32 . C33 . C34 . 119.2(11) yes C32 . C33 . H331 . 120.8 no C34 . C33 . H331 . 120.0 no C33 . C34 . C35 . 118.1(11) yes C33 . C34 . H341 . 120.8 no C35 . C34 . H341 . 121.0 no C34 . C35 . N30 . 123.5(11) yes C34 . C35 . H351 . 118.4 no N30 . C35 . H351 . 118.1 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 . Br1 . 2.4166(13) yes Au1 . Br2 . 2.4166(12) yes Au1 . C1 . 1.982(11) yes Au1 . C2 . 1.989(10) yes Au2 . Br3 . 2.4284(14) yes Au2 . Br4 . 2.4142(15) yes Au2 . C3 . 1.987(10) yes Au2 . C4 . 1.998(12) yes Br1 . Br3 . 3.6481(19) yes Cu1 . N1 . 2.214(10) yes Cu1 . N3 . 1.991(10) yes Cu1 . N10 . 2.032(9) yes Cu1 . N20 . 1.934(8) yes Cu1 . N30 . 2.014(8) yes N1 . C1 . 1.153(13) yes N2 . C2 . 1.132(13) yes N3 . C3 . 1.130(12) yes N4 . C4 . 1.121(14) yes N10 . C11 . 1.337(13) yes N10 . C15 . 1.349(13) yes N20 . C21 . 1.335(13) yes N20 . C25 . 1.342(12) yes N30 . C31 . 1.376(12) yes N30 . C35 . 1.320(13) yes C11 . C12 . 1.352(17) yes C11 . H111 . 0.929 no C12 . C13 . 1.360(18) yes C12 . H121 . 0.929 no C13 . C14 . 1.396(17) yes C13 . H131 . 0.931 no C14 . C15 . 1.359(16) yes C14 . H141 . 0.932 no C15 . C21 . 1.493(14) yes C21 . C22 . 1.385(14) yes C22 . C23 . 1.366(16) yes C22 . H221 . 0.931 no C23 . C24 . 1.372(17) yes C23 . H231 . 0.927 no C24 . C25 . 1.381(14) yes C24 . H241 . 0.929 no C25 . C31 . 1.475(15) yes C31 . C32 . 1.369(15) yes C32 . C33 . 1.399(16) yes C32 . H321 . 0.933 no C33 . C34 . 1.400(16) yes C33 . H331 . 0.929 no C34 . C35 . 1.368(15) yes C34 . H341 . 0.929 no C35 . H351 . 0.934 no