#------------------------------------------------------------------------------ #$Date: 2011-03-31 14:48:06 +0300 (Thu, 31 Mar 2011) $ #$Revision: 17004 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4316830.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_4316830 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 'C18 H36 Au1 Br2 N3' _chemical_formula_sum 'C18 H36 Au Br2 N3' _chemical_formula_weight 651.28 _chemical_name_systematic ' ' _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _cell_angle_alpha 90 _cell_angle_beta 103.000(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.7350(4) _cell_length_b 12.8898(6) _cell_length_c 20.3423(10) _cell_measurement_reflns_used 4933 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.73 _cell_measurement_theta_min 2.67 _cell_volume 2487.2(2) _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 0.998 _diffrn_measured_fraction_theta_max 0.994 _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 0.029 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 13433 _diffrn_reflns_theta_full 31.026 _diffrn_reflns_theta_max 31.659 _diffrn_reflns_theta_min 2.055 _exptl_absorpt_coefficient_mu 9.133 _exptl_absorpt_correction_T_max 0.7463 _exptl_absorpt_correction_T_min 0.5016 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.738 _exptl_crystal_description block _exptl_crystal_F_000 1256 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.88 _refine_diff_density_min -0.65 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.0647 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 112 _refine_ls_number_reflns 2352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0332 _refine_ls_shift/su_max 0.0003852 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F) + ( 0.00P)^2^ + 0.03P] ,where P=(max(Fo,0) + 2Fc)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0407 _refine_ls_wR_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0285 _reflns_limit_h_max 14 _reflns_limit_h_min -14 _reflns_limit_k_max 18 _reflns_limit_k_min 0 _reflns_limit_l_max 29 _reflns_limit_l_min 0 _reflns_number_gt 2474 _reflns_number_total 4167 _reflns_threshold_expression I>2.0\s(I) _oxford_diffrn_Wilson_B_factor 3.55 _oxford_diffrn_Wilson_scale 341.03 _oxford_refine_ls_r_factor_ref 0.0301 _oxford_refine_ls_scale 0.06289(7) _oxford_reflns_number_all 4167 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _[local]_cod_data_source_file ic101357y_si_001_2.cif _[local]_cod_data_source_block diBromo _[local]_cod_chemical_formula_sum_orig 'C18 H36 Au1 Br2 N3' _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 4316830 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+1/2 x,-y,z+1/2 -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 0.7500 0.7500 0.5000 0.0507 1.0000 Uani S . . . . . . Br1 Br 0.56040(6) 0.62674(4) 0.49153(3) 0.0779 1.0000 Uani . . . . . . . N1 N 0.7758(6) 0.6937(4) 0.3543(3) 0.1018 1.0000 Uani . . . . . . . N2 N 0.5000 0.4408(3) 0.2500 0.0415 1.0000 Uani S T . . . . . C1 C 0.7670(6) 0.7131(4) 0.4065(3) 0.0680 1.0000 Uani . . . . . . . C2 C 0.4182(4) 0.3694(3) 0.1957(2) 0.0480 1.0000 Uani . . . . . . . C3 C 0.3260(5) 0.4227(3) 0.1355(2) 0.0540 1.0000 Uani . . . . . . . C4 C 0.2397(5) 0.3436(4) 0.0884(2) 0.0654 1.0000 Uani . . . . . . . C5 C 0.1551(5) 0.3922(4) 0.0240(2) 0.0793 1.0000 Uani . . . . . . . C6 C 0.5974(4) 0.5122(3) 0.2224(2) 0.0481 1.0000 Uani . . . . . . . C7 C 0.7118(4) 0.4605(4) 0.1946(2) 0.0604 1.0000 Uani . . . . . . . C8 C 0.8042(5) 0.5415(5) 0.1726(3) 0.0794 1.0000 Uani . . . . . . . C9 C 0.9238(5) 0.4948(6) 0.1473(3) 0.1025 1.0000 Uani . . . . . . . H21 H 0.4842 0.3279 0.1794 0.052(3) 1.0000 Uiso R . . . . . . H22 H 0.3597 0.3260 0.2155 0.052(3) 1.0000 Uiso R . . . . . . H31 H 0.3832 0.4605 0.1118 0.062(3) 1.0000 Uiso R . . . . . . H32 H 0.2640 0.4690 0.1509 0.062(3) 1.0000 Uiso R . . . . . . H41 H 0.3020 0.2937 0.0767 0.073(3) 1.0000 Uiso R . . . . . . H42 H 0.1767 0.3103 0.1111 0.073(3) 1.0000 Uiso R . . . . . . H51 H 0.1024 0.3410 -0.0045 0.083(3) 1.0000 Uiso R . . . . . . H52 H 0.2179 0.4255 0.0012 0.083(3) 1.0000 Uiso R . . . . . . H53 H 0.0926 0.4421 0.0356 0.083(3) 1.0000 Uiso R . . . . . . H61 H 0.6423 0.5569 0.2580 0.057(3) 1.0000 Uiso R . . . . . . H62 H 0.5414 0.5523 0.1872 0.057(3) 1.0000 Uiso R . . . . . . H71 H 0.7680 0.4182 0.2285 0.072(3) 1.0000 Uiso R . . . . . . H72 H 0.6699 0.4188 0.1569 0.072(3) 1.0000 Uiso R . . . . . . H81 H 0.8420 0.5848 0.2101 0.097(3) 1.0000 Uiso R . . . . . . H82 H 0.7479 0.5819 0.1377 0.097(3) 1.0000 Uiso R . . . . . . H91 H 0.9800 0.5476 0.1340 0.119(3) 1.0000 Uiso R . . . . . . H92 H 0.9802 0.4544 0.1823 0.119(3) 1.0000 Uiso R . . . . . . H93 H 0.8861 0.4515 0.1098 0.119(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 0.05435(13) 0.03656(12) 0.06332(16) -0.00325(13) 0.01789(10) -0.00607(11) Br1 0.0745(3) 0.0635(3) 0.1031(4) -0.0171(3) 0.0353(3) -0.0276(3) N1 0.159(5) 0.071(4) 0.085(4) -0.013(3) 0.047(4) -0.030(3) N2 0.050(2) 0.032(2) 0.044(3) 0.0000 0.013(2) 0.0000 C1 0.095(4) 0.043(3) 0.070(4) -0.006(3) 0.028(3) -0.014(3) C2 0.055(2) 0.040(2) 0.049(2) -0.007(2) 0.0131(19) -0.0038(18) C3 0.063(3) 0.051(3) 0.047(3) -0.002(2) 0.012(2) -0.002(2) C4 0.067(3) 0.062(3) 0.065(3) -0.006(3) 0.009(2) -0.005(2) C5 0.077(3) 0.095(4) 0.059(3) -0.009(3) -0.001(3) -0.006(3) C6 0.058(2) 0.042(2) 0.046(2) 0.0054(19) 0.0138(19) -0.0065(19) C7 0.056(2) 0.069(3) 0.060(3) 0.002(3) 0.022(2) -0.006(2) C8 0.068(3) 0.097(4) 0.080(4) 0.021(3) 0.030(3) -0.007(3) C9 0.070(3) 0.163(7) 0.083(4) 0.020(4) 0.035(3) -0.007(4) 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' 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 4_666 Au1 . C1 4_666 90.07(15) yes Br1 4_666 Au1 . Br1 . 179.995 yes C1 4_666 Au1 . Br1 . 89.93(15) yes Br1 4_666 Au1 . C1 . 89.93(15) yes C1 4_666 Au1 . C1 . 179.994 yes Br1 . Au1 . C1 . 90.07(15) yes Au1 . Br1 . Br1 2_666 150.77(3) yes C2 5_655 N2 . C6 5_655 111.6(2) yes C2 5_655 N2 . C2 . 105.3(4) yes C6 5_655 N2 . C2 . 111.6(2) yes C2 5_655 N2 . C6 . 111.6(2) yes C6 5_655 N2 . C6 . 105.3(4) yes C2 . N2 . C6 . 111.6(2) yes Au1 . C1 . N1 . 179.2(6) yes N2 . C2 . C3 . 115.6(3) yes N2 . C2 . H21 . 108.0 no C3 . C2 . H21 . 107.5 no N2 . C2 . H22 . 108.3 no C3 . C2 . H22 . 107.9 no H21 . C2 . H22 . 109.5 no C2 . C3 . C4 . 110.5(4) yes C2 . C3 . H31 . 109.6 no C4 . C3 . H31 . 109.2 no C2 . C3 . H32 . 108.9 no C4 . C3 . H32 . 109.1 no H31 . C3 . H32 . 109.5 no C3 . C4 . C5 . 112.6(4) yes C3 . C4 . H41 . 108.6 no C5 . C4 . H41 . 108.5 no C3 . C4 . H42 . 108.8 no C5 . C4 . H42 . 108.8 no H41 . C4 . H42 . 109.5 no C4 . C5 . H51 . 110.7 no C4 . C5 . H52 . 109.0 no H51 . C5 . H52 . 109.5 no C4 . C5 . H53 . 108.7 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no N2 . C6 . C7 . 116.4(3) yes N2 . C6 . H61 . 107.8 no C7 . C6 . H61 . 107.5 no N2 . C6 . H62 . 108.0 no C7 . C6 . H62 . 107.6 no H61 . C6 . H62 . 109.5 no C6 . C7 . C8 . 110.1(4) yes C6 . C7 . H71 . 109.5 no C8 . C7 . H71 . 109.1 no C6 . C7 . H72 . 109.5 no C8 . C7 . H72 . 109.2 no H71 . C7 . H72 . 109.5 no C7 . C8 . C9 . 112.6(5) yes C7 . C8 . H81 . 108.5 no C9 . C8 . H81 . 108.8 no C7 . C8 . H82 . 108.5 no C9 . C8 . H82 . 109.0 no H81 . C8 . H82 . 109.5 no C8 . C9 . H91 . 110.6 no C8 . C9 . H92 . 109.0 no H91 . C9 . H92 . 109.5 no C8 . C9 . H93 . 108.8 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 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 . Br1 4_666 2.4120(5) yes Au1 . C1 4_666 2.003(6) yes Au1 . Br1 . 2.4120(5) yes Au1 . C1 . 2.003(6) yes Br1 . Br1 2_666 3.5156(11) yes N1 . C1 . 1.113(6) yes N2 . C2 5_655 1.519(5) yes N2 . C6 5_655 1.516(5) yes N2 . C2 . 1.519(5) yes N2 . C6 . 1.516(5) yes C2 . C3 . 1.511(5) yes C2 . H21 . 0.950 no C2 . H22 . 0.950 no C3 . C4 . 1.517(6) yes C3 . H31 . 0.950 no C3 . H32 . 0.950 no C4 . C5 . 1.516(6) yes C4 . H41 . 0.950 no C4 . H42 . 0.950 no C5 . H51 . 0.950 no C5 . H52 . 0.950 no C5 . H53 . 0.950 no C6 . C7 . 1.513(6) yes C6 . H61 . 0.950 no C6 . H62 . 0.950 no C7 . C8 . 1.510(6) yes C7 . H71 . 0.950 no C7 . H72 . 0.950 no C8 . C9 . 1.500(7) yes C8 . H81 . 0.950 no C8 . H82 . 0.950 no C9 . H91 . 0.950 no C9 . H92 . 0.950 no C9 . H93 . 0.950 no