#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100975.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_1100975 loop_ _publ_author_name 'Ruili Sang' 'Li Xu' _publ_section_title ; A Series of Single, Double, and Triple Me2biim-Bridged Dinuclear, Trinuclear, and Polymeric Complexes: Syntheses, Crystal Structures, and Luminescent Properties ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3731 _journal_page_last 3737 _journal_paper_doi 10.1021/ic048280x _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C16 H20 Cl4 N8 Zn2' _chemical_formula_weight 596.94 _chemical_name_common '[Zn2Cl4(Me2biim)2]' _space_group_IT_number 60 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_space_group_name_H-M 'P b c n' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 11.747(3) _cell_length_b 13.566(4) _cell_length_c 14.367(4) _cell_measurement_reflns_used 4804 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.4835 _cell_measurement_theta_min 3.0043 _cell_volume 2289.5(11) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 16589 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 3.00 _exptl_absorpt_coefficient_mu 2.583 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7696 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1200 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.899 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 136 _refine_ls_number_reflns 2628 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.137 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0414 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1409 _refine_ls_wR_factor_ref 0.1452 _reflns_number_gt 2479 _reflns_number_total 2628 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic048280xsi20041208_095610_2.cif _cod_data_source_block '[Zn2Cl4(Me2biim)2](2)' _cod_database_code 1100975 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.70612(3) 0.14367(3) 0.26112(3) 0.01592(17) Uani 1 1 d . . . Cl1 Cl 0.81157(7) 0.22266(6) 0.15533(6) 0.0291(2) Uani 1 1 d . . . Cl2 Cl 0.79637(6) 0.06033(6) 0.37429(6) 0.0263(2) Uani 1 1 d . . . N1 N 0.6069(2) 0.24222(19) 0.32896(17) 0.0167(5) Uani 1 1 d . . . N2 N 0.4852(2) 0.35913(19) 0.3655(2) 0.0194(6) Uani 1 1 d . . . N3 N 0.61317(19) 0.04948(18) 0.18255(18) 0.0165(5) Uani 1 1 d . . . N4 N 0.5085(2) -0.07612(19) 0.13540(17) 0.0170(5) Uani 1 1 d . . . C1 C 0.5232(2) 0.2996(2) 0.29783(19) 0.0156(6) Uani 1 1 d . . . C2 C 0.6225(2) 0.2674(2) 0.4209(2) 0.0180(6) Uani 1 1 d . . . H2A H 0.6759 0.2393 0.4607 0.022 Uiso 1 1 calc R . . C3 C 0.5476(3) 0.3396(2) 0.4444(2) 0.0197(6) Uani 1 1 d . . . H3A H 0.5400 0.3698 0.5021 0.024 Uiso 1 1 calc R . . C4 C 0.3974(3) 0.4348(3) 0.3571(3) 0.0317(8) Uani 1 1 d . . . H4A H 0.3669 0.4343 0.2951 0.047 Uiso 1 1 calc R . . H4B H 0.4300 0.4983 0.3699 0.047 Uiso 1 1 calc R . . H4C H 0.3375 0.4217 0.4009 0.047 Uiso 1 1 calc R . . C5 C 0.5302(2) -0.0129(2) 0.20517(19) 0.0162(6) Uani 1 1 d . . . C6 C 0.5819(3) -0.0537(2) 0.0642(2) 0.0202(6) Uani 1 1 d . . . H6A H 0.5873 -0.0856 0.0070 0.024 Uiso 1 1 calc R . . C7 C 0.6453(2) 0.0244(2) 0.09347(19) 0.0178(6) Uani 1 1 d . . . H7A H 0.7014 0.0559 0.0588 0.021 Uiso 1 1 calc R . . C8 C 0.4213(3) -0.1534(2) 0.1342(2) 0.0259(7) Uani 1 1 d . . . H8A H 0.3817 -0.1539 0.1926 0.039 Uiso 1 1 calc R . . H8B H 0.4569 -0.2162 0.1243 0.039 Uiso 1 1 calc R . . H8C H 0.3683 -0.1406 0.0848 0.039 Uiso 1 1 calc 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 Zn 0.0158(2) 0.0184(3) 0.0136(3) 0.00036(13) 0.00134(11) 0.00019(12) Cl1 0.0359(5) 0.0317(5) 0.0198(4) -0.0006(3) 0.0093(3) -0.0133(3) Cl2 0.0273(4) 0.0312(5) 0.0204(4) 0.0038(3) -0.0023(3) 0.0093(3) N1 0.0196(11) 0.0176(12) 0.0130(11) 0.0000(9) -0.0004(9) 0.0004(10) N2 0.0198(12) 0.0223(14) 0.0161(13) -0.0032(9) -0.0018(10) 0.0034(10) N3 0.0148(11) 0.0191(12) 0.0155(12) -0.0004(9) 0.0007(9) 0.0024(9) N4 0.0157(12) 0.0182(13) 0.0170(12) -0.0004(10) -0.0026(9) 0.0020(9) C1 0.0163(12) 0.0166(14) 0.0139(14) 0.0009(11) 0.0013(11) -0.0028(11) C2 0.0227(14) 0.0182(14) 0.0132(13) 0.0010(11) -0.0036(11) -0.0027(11) C3 0.0236(15) 0.0222(15) 0.0133(14) -0.0030(11) -0.0027(11) -0.0006(12) C4 0.0345(19) 0.0348(19) 0.0257(17) -0.0089(14) -0.0053(14) 0.0157(15) C5 0.0147(12) 0.0181(14) 0.0158(14) -0.0006(11) -0.0006(11) 0.0030(11) C6 0.0221(14) 0.0237(16) 0.0149(14) -0.0037(12) -0.0015(12) 0.0064(12) C7 0.0152(12) 0.0219(15) 0.0164(14) 0.0007(11) 0.0020(10) 0.0044(11) C8 0.0296(17) 0.0251(16) 0.0231(17) -0.0049(13) -0.0005(14) -0.0071(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn N3 112.02(10) . . ? N1 Zn Cl1 109.27(8) . . ? N3 Zn Cl1 102.85(8) . . ? N1 Zn Cl2 104.81(7) . . ? N3 Zn Cl2 109.90(8) . . ? Cl1 Zn Cl2 118.17(4) . . ? C1 N1 C2 106.0(2) . . ? C1 N1 Zn 130.5(2) . . ? C2 N1 Zn 123.32(19) . . ? C1 N2 C3 107.7(3) . . ? C1 N2 C4 126.8(3) . . ? C3 N2 C4 125.4(3) . . ? C5 N3 C7 105.7(2) . . ? C5 N3 Zn 131.3(2) . . ? C7 N3 Zn 121.77(19) . . ? C5 N4 C6 107.2(2) . . ? C5 N4 C8 126.7(2) . . ? C6 N4 C8 126.1(3) . . ? N1 C1 N2 110.8(2) . . ? N1 C1 C1 125.7(3) . 3_655 ? N2 C1 C1 123.5(3) . 3_655 ? C3 C2 N1 109.3(3) . . ? C2 C3 N2 106.2(3) . . ? N3 C5 N4 111.3(2) . . ? N3 C5 C5 124.6(2) . 3_655 ? N4 C5 C5 124.2(2) . 3_655 ? C7 C6 N4 106.6(3) . . ? C6 C7 N3 109.3(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn N1 2.024(2) . ? Zn N3 2.025(3) . ? Zn Cl1 2.2344(9) . ? Zn Cl2 2.2463(9) . ? N1 C1 1.332(4) . ? N1 C2 1.376(4) . ? N2 C1 1.340(4) . ? N2 C3 1.375(4) . ? N2 C4 1.460(4) . ? N3 C5 1.330(4) . ? N3 C7 1.377(4) . ? N4 C5 1.344(4) . ? N4 C6 1.373(4) . ? N4 C8 1.465(4) . ? C1 C1 1.478(5) 3_655 ? C2 C3 1.360(4) . ? C5 C5 1.471(5) 3_655 ? C6 C7 1.361(4) . ?