#------------------------------------------------------------------------------ #$Date: 2012-02-26 23:34:47 +0200 (Sun, 26 Feb 2012) $ #$Revision: 35909 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/01/56/7015612.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_7015612 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 'C8 H4 Au2 N6 Zn1' _chemical_formula_sum 'C8 H4 Au2 N6 Zn' _chemical_formula_weight 643.47 _chemical_name_systematic ; ; _space_group_IT_number 69 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-F 2 2' _symmetry_space_group_name_H-M 'F m m 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 4 _cell_length_a 11.4055(4) _cell_length_b 17.3296(6) _cell_length_c 7.0938(3) _cell_measurement_reflns_used 4193 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 44.17 _cell_measurement_theta_min 3.57 _cell_volume 1402.11(9) _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 0.997 _diffrn_measured_fraction_theta_max 0.985 _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 0.057 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 9919 _diffrn_reflns_theta_full 31.026 _diffrn_reflns_theta_max 44.500 _diffrn_reflns_theta_min 2.351 _exptl_absorpt_coefficient_mu 22.558 _exptl_absorpt_correction_T_max 0.7488 _exptl_absorpt_correction_T_min 0.2804 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 3.048 _exptl_crystal_description plate _exptl_crystal_F_000 1128 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.79 _refine_diff_density_min -2.41 _refine_ls_extinction_coef 75(4) _refine_ls_extinction_method 'Larson (1970), Equation 22' _refine_ls_goodness_of_fit_ref 0.9680 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 41 _refine_ls_number_reflns 1059 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0322 _refine_ls_shift/su_max 0.0000650 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F) + ( 0.03P)^2^ + 0.00P] ,where P=(max(Fo,0) + 2Fc)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0514 _refine_ls_wR_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0386 _reflns_limit_h_max 22 _reflns_limit_h_min 0 _reflns_limit_k_max 34 _reflns_limit_k_min 0 _reflns_limit_l_max 13 _reflns_limit_l_min 0 _reflns_number_gt 1094 _reflns_number_total 2809 _reflns_threshold_expression I>2.0\s(I) _oxford_diffrn_Wilson_B_factor 2.10 _oxford_diffrn_Wilson_scale 1352.50 _oxford_refine_ls_r_factor_ref 0.0317 _oxford_refine_ls_scale 0.0653(2) _oxford_reflns_number_all 1547 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _[local]_cod_data_source_file c0dt01772h.txt _[local]_cod_data_source_block ZnPyzAu1 _[local]_cod_chemical_formula_sum_orig 'C8 H4 Au2 N6 Zn1' _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_database_code 7015612 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 x+1/2,y,z+1/2 -x+1/2,-y,-z+1/2 x+1/2,y+1/2,z -x+1/2,-y+1/2,-z x,y,-z -x,-y,z x,y+1/2,-z+1/2 -x,-y+1/2,z+1/2 x+1/2,y,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y+1/2,-z -x+1/2,-y+1/2,z -x,y,z x,-y,-z -x,y+1/2,z+1/2 x,-y+1/2,-z+1/2 -x+1/2,y,z+1/2 x+1/2,-y,-z+1/2 -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y,z -x,y,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 x+1/2,-y,z+1/2 -x+1/2,y,-z+1/2 x+1/2,-y+1/2,z -x+1/2,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 0.2500 0.2500 0.0000 0.0446 1.0000 Uani S T . . . . . Zn1 Zn 0.5000 0.5000 0.0000 0.0210 1.0000 Uani S T . . . . . N1 N 0.3696(3) 0.41148(18) 0.0000 0.0392 1.0000 Uani S T . . . . . N2 N 0.5000 0.5000 0.3064(5) 0.0273 1.0000 Uani S T . . . . . C1 C 0.3238(4) 0.3530(2) 0.0000 0.0414 1.0000 Uani S T . . . . . C2 C 0.500000(7) 0.5658(3) 0.4023(9) 0.0454 0.644(9) Uani S T P . 1 . . C3 C 0.4022(6) 0.500000(7) 0.4035(9) 0.0281 0.356(9) Uani S T P . 2 . . H2 H 0.5000 0.6158 0.3339 0.06(3) 0.644(9) Uiso RS . P . 1 . . H3 H 0.3294 0.5000 0.3386 0.06(3) 0.356(9) Uiso RS . P . 2 . . 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 0.04826(15) 0.02791(11) 0.05773(18) 0.0000 0.0000 -0.01946(7) Zn1 0.0274(3) 0.01360(19) 0.0219(2) 0.0000 0.0000 0.0000 N1 0.0464(16) 0.0273(11) 0.0440(14) 0.0000 0.0000 -0.0163(11) N2 0.0366(17) 0.0256(13) 0.0197(12) 0.0000 0.0000 0.0000 C1 0.0466(19) 0.0303(15) 0.0472(17) 0.0000 0.0000 -0.0190(14) C2 0.072(5) 0.026(2) 0.038(3) 0.0024(17) 0.0000 0.0000 C3 0.017(3) 0.054(5) 0.014(2) 0.0000 0.0005(17) 0.0000 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' 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 C1 16_555 Au1 . Au1 21_555 90.000(3) yes C1 16_555 Au1 . Au1 21_554 90.000(3) yes Au1 21_555 Au1 . Au1 21_554 179.997 yes C1 16_555 Au1 . C1 . 179.994 yes Au1 21_555 Au1 . C1 . 90.000(3) yes Au1 21_554 Au1 . C1 . 90.000(3) yes N2 2_665 Zn1 . N1 25_565 90.000 yes N2 2_665 Zn1 . N1 17_655 90.000 yes N1 25_565 Zn1 . N1 17_655 179.995 yes N2 2_665 Zn1 . N1 10_665 90.000 yes N1 25_565 Zn1 . N1 10_665 88.2(2) yes N1 17_655 Zn1 . N1 10_665 91.8(2) yes N2 2_665 Zn1 . N1 . 90.000 yes N1 25_565 Zn1 . N1 . 91.8(2) yes N1 17_655 Zn1 . N1 . 88.2(2) yes N1 10_665 Zn1 . N1 . 179.995 yes N2 2_665 Zn1 . N2 . 179.995 yes N1 25_565 Zn1 . N2 . 90.000 yes N1 17_655 Zn1 . N2 . 90.000 yes N1 10_665 Zn1 . N2 . 90.000 yes N1 . Zn1 . N2 . 90.000 yes Zn1 . N1 . C1 . 163.2(4) yes Zn1 . N2 . C2 10_665 120.8(3) yes Zn1 . N2 . C2 . 120.8(3) yes C2 10_665 N2 . C2 . 118.4(6) yes Au1 . C1 . N1 . 177.9(4) yes C2 9_556 C2 . N2 . 120.8(3) yes C2 9_556 C2 . H2 . 119.2 no N2 . C2 . H2 . 120.0 no C3 9_556 C3 . N2 . 121.7(3) yes C3 9_556 C3 . H3 . 119.0 no N2 . C3 . H3 . 119.3 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 . C1 16_555 1.974(3) yes Au1 . Au1 21_555 3.54690(15) yes Au1 . Au1 21_554 3.54690(15) yes Au1 . C1 . 1.974(3) yes Zn1 . N2 2_665 2.174(3) yes Zn1 . N1 25_565 2.137(3) yes Zn1 . N1 17_655 2.137(3) yes Zn1 . N1 10_665 2.137(3) yes Zn1 . N1 . 2.137(3) yes Zn1 . N2 . 2.174(3) yes N1 . C1 . 1.140(4) yes N2 . C2 10_665 1.328(6) yes N2 . C2 . 1.328(6) yes C2 . C2 9_556 1.387(12) yes C2 . H2 . 0.993 no C3 . C3 9_556 1.369(12) yes C3 . H3 . 0.950 no