#------------------------------------------------------------------------------ #$Date: 2016-02-18 15:37:37 +0000 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100977.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_1100977 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 'C8 H10 Br2 Cd N4 O0' _chemical_formula_weight 434.42 _chemical_name_common '[CdBr2(N,N'-dimethylbiimidazole)]n' _space_group_IT_number 43 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'F 2 -2d' _symmetry_space_group_name_H-M 'F d d 2' _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 8 _cell_length_a 30.503(5) _cell_length_b 4.8598(9) _cell_length_c 16.322(3) _cell_measurement_reflns_used 1807 _cell_measurement_temperature 273(2) _cell_volume 2419.5(7) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 273(2) _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.980 _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 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 2879 _diffrn_reflns_theta_full 25.03 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_min 2.67 _exptl_absorpt_coefficient_mu 8.384 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.3983 _exptl_absorpt_correction_type SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1632 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _refine_diff_density_max 2.614 _refine_diff_density_min -1.329 _refine_diff_density_rms 0.271 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.07(4) _refine_ls_extinction_coef 0.0010(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.512 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 70 _refine_ls_number_reflns 962 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.511 _refine_ls_R_factor_all 0.0978 _refine_ls_R_factor_gt 0.0861 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1527P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2436 _refine_ls_wR_factor_ref 0.2717 _reflns_number_gt 788 _reflns_number_total 962 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic048280xsi20041208_095610_4.cif _cod_data_source_block '[CdBr2(N,N'-dimethylbiimidazole)]n' _cod_original_cell_volume 2419.6(7) _cod_database_code 1100977 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' 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 Cd Cd 0.5000 0.0000 0.12845(14) 0.0594(8) Uani 1 2 d S . . Br Br 0.44072(8) 0.2702(3) 0.05554(9) 0.0698(9) Uani 1 1 d . . . N1 N 0.4633(6) -0.252(3) 0.2211(11) 0.054(4) Uani 1 1 d . . . N2 N 0.4439(6) -0.554(3) 0.3193(12) 0.055(3) Uani 1 1 d . . . C1 C 0.4782(6) -0.460(3) 0.2711(14) 0.057(5) Uani 1 1 d . . . C2 C 0.4031(8) -0.427(5) 0.2960(16) 0.077(6) Uani 1 1 d . . . H2A H 0.3750 -0.4645 0.3151 0.092 Uiso 1 1 calc R . . C3 C 0.4159(5) -0.239(4) 0.2390(13) 0.073(7) Uani 1 1 d . . . H3A H 0.3968 -0.1149 0.2141 0.088 Uiso 1 1 calc R . . C4 C 0.4487(11) -0.768(5) 0.385(3) 0.107(13) Uani 1 1 d . . . H4A H 0.4789 -0.8207 0.3890 0.161 Uiso 1 1 calc R . . H4B H 0.4314 -0.9264 0.3705 0.161 Uiso 1 1 calc R . . H4C H 0.4388 -0.6948 0.4359 0.161 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 Cd 0.0533(12) 0.0730(14) 0.0520(12) 0.000 0.000 0.0054(7) Br 0.0631(15) 0.0722(14) 0.0740(17) 0.0066(11) -0.0152(10) 0.0021(6) N1 0.062(10) 0.060(8) 0.039(9) 0.003(5) 0.022(7) 0.004(6) N2 0.056(8) 0.052(6) 0.058(9) 0.009(6) -0.007(7) 0.016(6) C1 0.039(10) 0.058(9) 0.075(13) 0.022(8) -0.015(9) -0.002(7) C2 0.063(13) 0.105(13) 0.063(13) -0.007(12) 0.030(11) -0.009(11) C3 0.019(7) 0.15(2) 0.051(11) -0.023(9) 0.031(8) 0.008(8) C4 0.087(17) 0.094(18) 0.14(3) -0.003(13) 0.09(2) -0.001(10) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 Cd N1 95.3(10) 2_655 . ? N1 Cd Br 104.1(5) 2_655 2_655 ? N1 Cd Br 112.9(4) . 2_655 ? N1 Cd Br 112.9(4) 2_655 . ? N1 Cd Br 104.1(5) . . ? Br Cd Br 123.92(13) 2_655 . ? C1 N1 C3 103.8(15) . . ? C1 N1 Cd 129.5(15) . . ? C3 N1 Cd 126.7(13) . . ? C1 N2 C2 111.2(15) . . ? C1 N2 C4 124.0(16) . . ? C2 N2 C4 125(2) . . ? N1 C1 C1 121.4(17) . 2_645 ? N1 C1 N2 109.2(16) . . ? C1 C1 N2 129.3(14) 2_645 . ? C3 C2 N2 102.8(17) . . ? C2 C3 N1 112.7(18) . . ? 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 Cd N1 2.244(15) 2_655 ? Cd N1 2.244(15) . ? Cd Br 2.532(2) 2_655 ? Cd Br 2.532(2) . ? N1 C1 1.38(2) . ? N1 C3 1.48(2) . ? N2 C1 1.39(3) . ? N2 C2 1.44(3) . ? N2 C4 1.50(4) . ? C1 C1 1.38(4) 2_645 ? C2 C3 1.36(3) . ?