#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/49/2204952.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2204952 loop_ _publ_author_name 'Zhang, Hui' 'Fang, Liang' _publ_section_title ; Bis(pyridinium) tetrabromocadmate(II) monohydrate ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m101 _journal_page_last m102 _journal_paper_doi 10.1107/S1600536804029897 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '(C5 H6 N)2 [Cd Br4], H2 O' _chemical_formula_moiety '2C5 H6 N +, Br4 Cd 2-, H2 O' _chemical_formula_sum 'C10 H14 Br4 Cd N2 O' _chemical_formula_weight 610.27 _chemical_name_systematic ; Bis(pyridinium) tetrabromocadmate(II) monohydrate ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _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 14.951(2) _cell_length_b 9.1564(15) _cell_length_c 12.815(2) _cell_measurement_reflns_used 2299 _cell_measurement_temperature 223(2) _cell_measurement_theta_max 28.32 _cell_measurement_theta_min 2.09 _cell_volume 1754.3(5) _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_collection 'SMART (Bruker, 1998)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _diffrn_ambient_temperature 223(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker AXS APEX CCD' _diffrn_measurement_method \w _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 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 22963 _diffrn_reflns_theta_full 28.32 _diffrn_reflns_theta_max 28.32 _diffrn_reflns_theta_min 2.09 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 10.346 _exptl_absorpt_correction_T_max 0.355 _exptl_absorpt_correction_T_min 0.234 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 1136 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.657 _refine_diff_density_min -0.662 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 2299 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.102 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0296 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0272P)^2^+2.3887P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.0767 _reflns_number_gt 1776 _reflns_number_total 2299 _reflns_threshold_expression I>2\s(I) _cod_data_source_file rz6012.cif _cod_data_source_block I _cod_database_code 2204952 _cod_database_fobs_code 2204952 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Cd1 0.37721(3) 0.2500 0.75084(4) 0.03605(13) Uani d S 1 Cd Br1 0.34626(3) 0.02430(6) 0.86495(4) 0.04565(14) Uani d . 1 Br Br2 0.54582(4) 0.2500 0.70170(5) 0.04547(18) Uani d S 1 Br Br3 0.29500(5) 0.2500 0.57349(6) 0.0527(2) Uani d S 1 Br O1 0.5712(4) 0.2500 0.9546(4) 0.0560(14) Uani d S 1 O N1 0.3121(4) 0.7500 0.5065(5) 0.0622(18) Uani d S 1 N H1 0.2629 0.7500 0.4704 0.075 Uiso calc SR 1 H N2 0.4451(4) 0.2500 0.1020(4) 0.0407(13) Uani d S 1 N H2 0.4880 0.2500 0.0562 0.049 Uiso calc SR 1 H C3 0.3471(4) 0.8746(6) 0.5322(4) 0.0545(14) Uani d . 1 C H3 0.3176 0.9615 0.5136 0.065 Uiso calc R 1 H C4 0.4229(4) 0.8813(7) 0.5837(4) 0.0702(18) Uani d . 1 C H4 0.4479 0.9718 0.6025 0.084 Uiso calc R 1 H C5 0.4655(6) 0.7500 0.6099(7) 0.090(4) Uani d S 1 C H5 0.5211 0.7500 0.6442 0.108 Uiso calc SR 1 H C6 0.4133(3) 0.1227(5) 0.1360(4) 0.0439(11) Uani d . 1 C H6 0.4379 0.0348 0.1112 0.053 Uiso calc R 1 H C7 0.3455(3) 0.1200(5) 0.2061(4) 0.0439(11) Uani d . 1 C H7 0.3225 0.0305 0.2300 0.053 Uiso calc R 1 H C8 0.3109(4) 0.2500 0.2419(5) 0.0422(15) Uani d S 1 C H8 0.2639 0.2500 0.2905 0.051 Uiso calc SR 1 H H9 0.629(5) 0.2500 0.952(6) 0.05(2) Uiso d S 1 H H10 0.569(6) 0.2500 0.884(7) 0.08(3) Uiso d S 1 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cd1 0.0342(2) 0.0373(2) 0.0366(2) 0.000 -0.0030(2) 0.000 Br1 0.0463(3) 0.0434(3) 0.0472(3) -0.0070(2) -0.0024(2) 0.0083(2) Br2 0.0356(3) 0.0657(5) 0.0351(4) 0.000 0.0053(3) 0.000 Br3 0.0520(4) 0.0547(4) 0.0514(4) 0.000 -0.0226(3) 0.000 O1 0.038(3) 0.094(4) 0.036(3) 0.000 0.006(2) 0.000 N1 0.044(4) 0.092(6) 0.051(4) 0.000 0.007(3) 0.000 N2 0.041(3) 0.051(3) 0.030(3) 0.000 0.006(2) 0.000 C3 0.058(3) 0.047(3) 0.058(3) 0.013(3) 0.011(3) 0.001(3) C4 0.079(5) 0.075(4) 0.056(4) -0.024(4) 0.012(3) -0.033(3) C5 0.048(5) 0.170(12) 0.053(5) 0.000 -0.024(4) 0.000 C6 0.043(3) 0.038(3) 0.051(3) 0.005(2) 0.006(2) -0.004(2) C7 0.042(3) 0.040(3) 0.050(3) -0.004(2) 0.006(2) 0.007(2) C8 0.028(3) 0.055(4) 0.043(4) 0.000 0.010(3) 0.000 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' 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' O O 0.0106 0.0060 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Br1 Cd1 Br1 7_565 . 106.84(3) yes Br1 Cd1 Br3 7_565 . 114.474(19) ? Br1 Cd1 Br3 . . 114.474(19) yes Br1 Cd1 Br2 7_565 . 108.188(18) ? Br1 Cd1 Br2 . . 108.188(18) yes Br3 Cd1 Br2 . . 104.38(3) yes H9 O1 H10 . . 90(7) ? C3 N1 C3 7_575 . 123.2(7) ? C3 N1 H1 7_575 . 118.4 ? C3 N1 H1 . . 118.4 ? C6 N2 C6 . 7_565 122.2(6) ? C6 N2 H2 . . 118.9 ? C6 N2 H2 7_565 . 118.9 ? N1 C3 C4 . . 121.1(6) ? N1 C3 H3 . . 119.5 ? C4 C3 H3 . . 119.5 ? C3 C4 C5 . . 118.2(6) ? C3 C4 H4 . . 120.9 ? C5 C4 H4 . . 120.9 ? C4 C5 C4 7_575 . 118.2(8) ? C4 C5 H5 7_575 . 120.9 ? C4 C5 H5 . . 120.9 ? N2 C6 C7 . . 120.0(5) ? N2 C6 H6 . . 120.0 ? C7 C6 H6 . . 120.0 ? C6 C7 C8 . . 119.1(5) ? C6 C7 H7 . . 120.5 ? C8 C7 H7 . . 120.5 ? C7 C8 C7 . 7_565 119.7(6) ? C7 C8 H8 . . 120.1 ? C7 C8 H8 7_565 . 120.1 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cd1 Br1 7_565 2.5736(6) ? Cd1 Br1 . 2.5736(6) yes Cd1 Br3 . 2.5838(9) yes Cd1 Br2 . 2.5983(9) yes O1 H9 . 0.86(8) ? O1 H10 . 0.90(9) ? N1 C3 . 1.297(6) ? N1 H1 . 0.8700 ? N2 C6 . 1.331(5) ? N2 H2 . 0.8700 ? C3 C4 . 1.314(8) ? C3 H3 . 0.9400 ? C4 C5 . 1.402(8) ? C4 H4 . 0.9400 ? C5 H5 . 0.9400 ? C6 C7 . 1.355(6) ? C6 H6 . 0.9400 ? C7 C8 . 1.377(6) ? C7 H7 . 0.9400 ? C8 H8 . 0.9400 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N2 H2 O1 1_554 0.87 1.80 2.669(7) 176 yes O1 H9 Br3 6_657 0.86(8) 2.50(8) 3.365(6) 175(7) yes O1 H10 Br2 . 0.90(9) 2.36(9) 3.263(6) 174(8) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion C3 N1 C3 C4 7_575 . 2.3(12) N1 C3 C4 C5 . . 0.3(10) C3 C4 C5 C4 . 7_575 -2.7(13) C6 N2 C6 C7 7_565 . 1.0(10) N2 C6 C7 C8 . . -0.5(8) C6 C7 C8 C7 . 7_565 0.0(10)