#------------------------------------------------------------------------------ #$Date: 2012-02-24 19:13:23 +0200 (Fri, 24 Feb 2012) $ #$Revision: 34330 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/31/68/4316829.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_4316829 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_volume 49 _journal_year 2010 _chemical_formula_moiety 'C9 H16 Au2 Br4 N8 Ni1 O1.00' _chemical_formula_sum 'C9 H16 Au2 Br4 N8 Ni O' _chemical_formula_weight 1024.54 _chemical_name_systematic ' ' _space_group_IT_number 11 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _cell_angle_alpha 90 _cell_angle_beta 106.587(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.4178(3) _cell_length_b 14.1538(6) _cell_length_c 10.3633(4) _cell_measurement_reflns_used 9928 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 32.62 _cell_measurement_theta_min 2.51 _cell_volume 1183.34(8) _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 0.997 _diffrn_measured_fraction_theta_max 0.979 _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 0.044 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 21355 _diffrn_reflns_theta_full 28.378 _diffrn_reflns_theta_max 32.618 _diffrn_reflns_theta_min 2.050 _exptl_absorpt_coefficient_mu 19.922 _exptl_absorpt_correction_T_max 0.7464 _exptl_absorpt_correction_T_min 0.3096 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour amber _exptl_crystal_density_diffrn 2.875 _exptl_crystal_description plate _exptl_crystal_F_000 920 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _refine_diff_density_max 4.11 _refine_diff_density_min -1.45 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.1586 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 129 _refine_ls_number_reflns 2826 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0465 _refine_ls_shift/su_max 0.0098427 _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 0.1230 _refine_ls_wR_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.0660 _reflns_limit_h_max 12 _reflns_limit_h_min -12 _reflns_limit_k_max 21 _reflns_limit_k_min 0 _reflns_limit_l_max 15 _reflns_limit_l_min 0 _reflns_number_gt 2986 _reflns_number_total 4381 _reflns_threshold_expression I>2.0\s(I) _oxford_diffrn_Wilson_B_factor 2.60 _oxford_diffrn_Wilson_scale 532.66 _oxford_refine_ls_r_factor_ref 0.0451 _oxford_refine_ls_scale 0.04942(13) _oxford_reflns_number_all 4369 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _[local]_cod_data_source_file ic101357y_si_001_1.cif _[local]_cod_data_source_block NiPolymer _[local]_cod_chemical_formula_sum_orig 'C9 H16 Au2 Br4 N8 Ni1 O1.00' _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_database_code 4316829 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z x,-y+1/2,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 0.5000 0.0000 0.0301 1.0000 Uani S . . . . . . Au2 Au 0.71336(6) 0.7500 -0.09732(5) 0.0423 1.0000 Uani S T . . . . . Br1 Br 0.70118(13) 0.49916(7) -0.04420(11) 0.0512 1.0000 Uani . . . . . . . Br2 Br 1.0067(2) 0.7500 -0.0829(2) 0.0694 1.0000 Uani S T . . . . . Br3 Br 0.4198(2) 0.7500 -0.1142(2) 0.0729 1.0000 Uani S T . . . . . Ni1 Ni 1.0000 0.5000 0.5000 0.0341 1.0000 Uani S . . . . . . O1 O 0.177(3) 0.7500 0.359(3) 0.071(4) 0.512(19) Uiso DS . P . 1 . . O2 O 0.282(3) 0.7500 0.274(3) 0.071(4) 0.488(19) Uiso DS . P . 2 . . N1 N 1.0350(12) 0.5074(6) 0.3074(8) 0.0481 1.0000 Uani . . . . . . . N2 N 0.632(3) 0.7500 -0.4114(18) 0.0933 1.0000 Uani S T . . . . . N3 N 0.809(2) 0.7500 0.2155(15) 0.0793 1.0000 Uani S T . . . . . N11 N 0.8082(11) 0.4040(7) 0.4259(9) 0.0569 1.0000 Uani . . . . . . . N12 N 0.8101(11) 0.5993(7) 0.4364(8) 0.0558 1.0000 Uani . . . . . . . C1 C 1.0261(12) 0.5042(6) 0.1969(9) 0.0369 1.0000 Uani . . . . . . . C2 C 0.6636(18) 0.7500 -0.2974(15) 0.0502 1.0000 Uani S T . . . . . C3 C 0.775(2) 0.7500 0.1049(18) 0.0661 1.0000 Uani S T . . . . . C4 C 0.299(3) 0.7500 0.373(3) 0.23(2) 1.0000 Uiso DS . . . . . . C11 C 0.6510(15) 0.4559(13) 0.4025(19) 0.0996 1.0000 Uani . . . . . . . C12 C 0.6562(17) 0.5487(12) 0.3519(16) 0.0885 1.0000 Uani . . . . . . . H111 H 0.5602 0.4215 0.3415 0.35(11) 1.0000 Uiso R . . . . . . H112 H 0.6304 0.4625 0.4897 0.35(11) 1.0000 Uiso R . . . . . . H113 H 0.8152 0.3542 0.4886 0.11(3) 1.0000 Uiso R . . . . . . H114 H 0.8136 0.3787 0.3424 0.11(3) 1.0000 Uiso R . . . . . . H121 H 0.6656 0.5426 0.2613 0.34(11) 1.0000 Uiso R . . . . . . H122 H 0.5569 0.5841 0.3509 0.34(11) 1.0000 Uiso R . . . . . . H123 H 0.8424 0.6471 0.3846 0.11(3) 1.0000 Uiso R . . . . . . H124 H 0.7866 0.6271 0.5123 0.11(3) 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 0.0405(2) 0.0358(2) 0.01535(18) 0.00060(14) 0.01024(15) 0.00116(17) Au2 0.0507(3) 0.0391(3) 0.0367(3) 0.0000 0.0118(2) 0.0000 Br1 0.0414(5) 0.0671(7) 0.0452(5) -0.0007(4) 0.0124(4) 0.0005(4) Br2 0.0463(8) 0.0573(9) 0.0994(14) 0.0000 0.0124(8) 0.0000 Br3 0.0622(10) 0.0877(12) 0.0774(12) 0.0000 0.0339(9) 0.0000 Ni1 0.0440(8) 0.0424(8) 0.0169(6) -0.0008(5) 0.0103(6) -0.0008(6) N1 0.064(6) 0.058(5) 0.026(4) 0.001(3) 0.018(4) -0.005(4) N2 0.121(15) 0.089(12) 0.062(10) 0.0000 0.013(10) 0.0000 N3 0.124(15) 0.070(10) 0.043(8) 0.0000 0.023(8) 0.0000 N11 0.070(6) 0.059(5) 0.039(4) -0.008(4) 0.011(4) -0.018(5) N12 0.066(6) 0.064(5) 0.040(4) 0.007(4) 0.019(4) 0.019(4) C1 0.044(5) 0.044(5) 0.026(4) 0.002(3) 0.015(3) 0.001(4) C2 0.043(7) 0.058(9) 0.047(8) 0.0000 0.009(6) 0.0000 C3 0.092(14) 0.043(8) 0.060(11) 0.0000 0.015(9) 0.0000 C11 0.028(6) 0.110(13) 0.140(15) 0.018(11) -0.009(7) -0.015(7) C12 0.067(9) 0.102(12) 0.084(10) 0.017(9) 0.002(7) 0.016(8) 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' Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421 1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' 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 2_765 Au1 . C1 2_765 89.9(3) yes Br1 2_765 Au1 . Br1 . 179.995 yes C1 2_765 Au1 . Br1 . 90.1(3) yes Br1 2_765 Au1 . C1 . 90.1(3) yes C1 2_765 Au1 . C1 . 179.994 yes Br1 . Au1 . C1 . 89.9(3) yes Br2 . Au2 . Br3 . 179.42(6) yes Br2 . Au2 . C2 . 88.4(4) yes Br3 . Au2 . C2 . 91.0(4) yes Br2 . Au2 . C3 . 88.9(5) yes Br3 . Au2 . C3 . 91.6(5) yes C2 . Au2 . C3 . 177.3(6) yes Au1 . Br1 . Br1 2_665 156.03(6) yes Au2 . Br2 . Br3 1_655 171.65(10) yes Au2 . Br3 . Br2 1_455 171.07(9) yes N1 2_766 Ni1 . N12 2_766 88.2(3) yes N1 2_766 Ni1 . N11 2_766 89.2(3) yes N12 2_766 Ni1 . N11 2_766 83.1(4) yes N1 2_766 Ni1 . N1 . 179.995 yes N12 2_766 Ni1 . N1 . 91.8(3) yes N11 2_766 Ni1 . N1 . 90.8(3) yes N1 2_766 Ni1 . N11 . 90.8(3) yes N12 2_766 Ni1 . N11 . 96.9(4) yes N11 2_766 Ni1 . N11 . 179.994 yes N1 . Ni1 . N11 . 89.2(3) yes N1 2_766 Ni1 . N12 . 91.8(3) yes N12 2_766 Ni1 . N12 . 179.995 yes N11 2_766 Ni1 . N12 . 96.9(4) yes N1 . Ni1 . N12 . 88.2(3) yes N11 . Ni1 . N12 . 83.1(4) yes Ni1 . N1 . C1 . 167.6(9) yes Ni1 . N11 . C11 . 107.6(8) yes Ni1 . N11 . H113 . 110.0 no C11 . N11 . H113 . 111.1 no Ni1 . N11 . H114 . 110.4 no C11 . N11 . H114 . 108.2 no H113 . N11 . H114 . 109.5 no Ni1 . N12 . C12 . 108.3(8) yes Ni1 . N12 . H123 . 109.9 no C12 . N12 . H123 . 110.2 no Ni1 . N12 . H124 . 109.8 no C12 . N12 . H124 . 109.1 no H123 . N12 . H124 . 109.5 no Au1 . C1 . N1 . 177.5(9) yes Au2 . C2 . N2 . 178.6(16) yes Au2 . C3 . N3 . 179.8(19) yes N11 . C11 . C12 . 113.7(11) yes N11 . C11 . H111 . 111.2 no C12 . C11 . H111 . 108.9 no N11 . C11 . H112 . 106.5 no C12 . C11 . H112 . 106.7 no H111 . C11 . H112 . 109.6 no N12 . C12 . C11 . 109.6(11) yes N12 . C12 . H121 . 107.9 no C11 . C12 . H121 . 107.2 no N12 . C12 . H122 . 110.6 no C11 . C12 . H122 . 111.4 no H121 . C12 . H122 . 110.1 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_765 2.4247(10) yes Au1 . C1 2_765 1.990(9) yes Au1 . Br1 . 2.4247(10) yes Au1 . C1 . 1.990(9) yes Au2 . Br2 . 2.4313(16) yes Au2 . Br3 . 2.4270(18) yes Au2 . C2 . 1.995(15) yes Au2 . C3 . 2.010(17) yes Br1 . Br1 2_665 3.753(2) yes Br2 . Br3 1_655 3.583(3) yes Ni1 . N1 2_766 2.101(8) yes Ni1 . N12 2_766 2.089(8) yes Ni1 . N11 2_766 2.082(8) yes Ni1 . N1 . 2.101(8) yes Ni1 . N11 . 2.082(8) yes Ni1 . N12 . 2.089(8) yes O1 . C4 . 0.993(10) yes O2 . C4 . 0.995(10) yes N1 . C1 . 1.128(12) yes N2 . C2 . 1.13(2) yes N3 . C3 . 1.10(2) yes N11 . C11 . 1.472(17) yes N11 . H113 . 0.950 no N11 . H114 . 0.950 no N12 . C12 . 1.520(18) yes N12 . H123 . 0.950 no N12 . H124 . 0.950 no C11 . C12 . 1.42(2) yes C11 . H111 . 0.972 no C11 . H112 . 0.973 no C12 . H121 . 0.968 no C12 . H122 . 0.972 no