#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/67/2206718.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_2206718 loop_ _publ_author_name 'Fu, Yun-Long' 'Xu, Zhi-Wei' 'Ren, Jia-Lin' 'Ng, Seik Weng' _publ_section_title ; Diethylenetriaminium(3+) hexachlorobismuthate(III) ; _journal_coeditor_code HK6030 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m1717 _journal_page_last m1718 _journal_paper_doi 10.1107/S1600536805024438 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '(C4 H16 N3) [Bi Cl6]' _chemical_formula_moiety 'C4 H16 N3 3+, Bi Cl6 3-' _chemical_formula_sum 'C4 H16 Bi Cl6 N3' _chemical_formula_weight 527.88 _chemical_name_systematic ; Diethylenetriaminium(3+) hexachlorobismuthate(III) ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 6.8466(3) _cell_length_b 15.6680(8) _cell_length_c 13.6328(7) _cell_measurement_reflns_used 6004 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 28.7 _cell_measurement_theta_min 3.0 _cell_volume 1462.42(12) _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_collection 'SMART (Bruker, 2002)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measurement_device_type 'Bruker APEX area-detector' _diffrn_measurement_method '\f and \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 0.049 _diffrn_reflns_av_sigmaI/netI 0.045 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 12004 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 2.0 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 13.124 _exptl_absorpt_correction_T_max 0.420 _exptl_absorpt_correction_T_min 0.138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 2.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 984 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.35 _refine_diff_density_min -0.89 _refine_ls_abs_structure_details 'Flack (1983), 1379 Friedel pairs' _refine_ls_abs_structure_Flack -0.034(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 129 _refine_ls_number_reflns 3302 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.02 _refine_ls_R_factor_all 0.033 _refine_ls_R_factor_gt 0.031 _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^)+(0.048P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.080 _refine_ls_wR_factor_ref 0.081 _reflns_number_gt 3119 _reflns_number_total 3302 _reflns_threshold_expression I>2\s(I) _cod_data_source_file hk6030.cif _cod_data_source_block I _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. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 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. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 1462.40(10) _cod_database_code 2206718 _cod_database_fobs_code 2206718 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, 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 Bi1 -0.04626(3) 0.872500(10) 0.74634(2) 0.03150(10) Uani d . 1 Bi Cl1 -0.1992(3) 0.98590(10) 0.61800(10) 0.0404(4) Uani d . 1 Cl Cl2 -0.2096(3) 0.74400(10) 0.65230(10) 0.0416(4) Uani d . 1 Cl Cl3 0.0879(3) 0.76090(10) 0.88450(10) 0.0512(4) Uani d . 1 Cl Cl4 0.1199(3) 1.00780(9) 0.85510(10) 0.0409(4) Uani d . 1 Cl Cl5 0.2507(3) 0.85190(10) 0.61050(10) 0.0486(4) Uani d . 1 Cl Cl6 -0.3744(3) 0.89000(10) 0.8439(2) 0.0649(5) Uani d . 1 Cl N1 0.1724(9) 1.1126(4) 0.5229(4) 0.0490(10) Uani d . 1 N N2 0.4934(8) 1.0950(3) 0.7459(4) 0.0360(10) Uani d . 1 N N3 0.8330(9) 1.1544(3) 0.9500(4) 0.0400(10) Uani d . 1 N C1 0.2676(14) 1.0775(5) 0.6100(6) 0.058(2) Uani d . 1 C C2 0.4315(10) 1.1324(4) 0.6501(4) 0.0370(10) Uani d . 1 C C3 0.6488(9) 1.1453(4) 0.7960(5) 0.0360(10) Uani d . 1 C C4 0.6585(9) 1.1156(4) 0.9023(5) 0.0390(10) Uani d . 1 C H1a 0.1197 1.1637 0.5376 0.058 Uiso calc R 1 H H1b 0.0777 1.0768 0.5029 0.058 Uiso calc R 1 H H1c 0.2611 1.1190 0.4748 0.058 Uiso calc R 1 H H2a 0.3888 1.0916 0.7857 0.043 Uiso calc R 1 H H2b 0.5374 1.0416 0.7357 0.043 Uiso calc R 1 H H3a 0.9416 1.1377 0.9181 0.048 Uiso calc R 1 H H3b 0.8395 1.1372 1.0129 0.048 Uiso calc R 1 H H3c 0.8234 1.2117 0.9478 0.048 Uiso calc R 1 H H1d 0.3197 1.0217 0.5940 0.070 Uiso calc R 1 H H1e 0.1702 1.0699 0.6609 0.070 Uiso calc R 1 H H2c 0.5405 1.1331 0.6046 0.044 Uiso calc R 1 H H2d 0.3866 1.1905 0.6594 0.044 Uiso calc R 1 H H3d 0.6182 1.2057 0.7932 0.043 Uiso calc R 1 H H3e 0.7735 1.1362 0.7639 0.043 Uiso calc R 1 H H4a 0.5410 1.1328 0.9368 0.046 Uiso calc R 1 H H4b 0.6676 1.0539 0.9047 0.046 Uiso calc R 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 Bi1 0.03530(10) 0.02880(10) 0.03040(10) -0.00170(10) 0.00340(10) -0.00270(10) Cl1 0.0447(9) 0.0374(8) 0.0390(8) 0.0057(7) -0.0011(7) -0.0013(6) Cl2 0.0419(8) 0.0373(7) 0.0455(9) -0.0061(7) 0.0021(7) -0.0061(7) Cl3 0.0690(10) 0.0414(8) 0.0430(9) -0.0017(9) -0.0048(9) 0.0066(7) Cl4 0.0449(9) 0.0354(7) 0.0425(9) -0.0008(7) -0.0006(7) -0.0032(6) Cl5 0.0474(9) 0.0357(8) 0.0630(10) -0.0007(7) 0.0154(8) 0.0007(7) Cl6 0.0620(10) 0.0650(10) 0.0680(10) -0.0100(10) 0.0320(10) -0.0150(10) N1 0.042(3) 0.065(4) 0.039(3) -0.001(3) -0.005(2) -0.008(3) N2 0.038(2) 0.035(2) 0.034(3) -0.001(2) -0.003(2) 0.002(2) N3 0.045(3) 0.037(3) 0.037(3) 0.001(3) -0.005(2) -0.001(2) C1 0.066(5) 0.049(4) 0.059(5) -0.011(4) -0.018(4) 0.006(3) C2 0.041(3) 0.035(3) 0.034(3) 0.000(3) -0.002(3) 0.001(2) C3 0.033(3) 0.038(3) 0.036(3) -0.004(3) 0.004(3) -0.002(3) C4 0.038(3) 0.044(3) 0.034(3) -0.004(3) -0.001(2) 0.001(3) 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' Bi Bi -4.1077 10.2566 '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_publ_flag Cl1 Bi1 Cl2 91.33(5) yes Cl1 Bi1 Cl3 176.08(6) yes Cl1 Bi1 Cl4 90.12(5) yes Cl1 Bi1 Cl5 85.87(5) yes Cl1 Bi1 Cl6 85.85(6) yes Cl2 Bi1 Cl3 89.36(5) yes Cl2 Bi1 Cl4 177.37(5) yes Cl2 Bi1 Cl5 84.10(5) yes Cl2 Bi1 Cl6 87.90(6) yes Cl3 Bi1 Cl4 89.04(5) yes Cl3 Bi1 Cl5 98.05(6) yes Cl3 Bi1 Cl6 90.32(7) yes Cl4 Bi1 Cl6 90.03(6) yes Cl4 Bi1 Cl5 98.19(5) yes Cl5 Bi1 Cl6 168.33(7) yes C3 N2 C2 113.3(5) no N1 C1 C2 114.2(6) no N2 C2 C1 107.6(5) no N2 C3 C4 107.8(5) no N3 C4 C3 109.0(5) no C1 N1 H1a 109.5 no C1 N1 H1b 109.5 no H1a N1 H1b 109.5 no C1 N1 H1c 109.5 no H1a N1 H1c 109.5 no H1b N1 H1c 109.5 no C3 N2 H2a 108.9 no C2 N2 H2a 108.9 no C3 N2 H2b 108.9 no C2 N2 H2b 108.9 no H2a N2 H2b 107.7 no C4 N3 H3a 109.5 no C4 N3 H3b 109.5 no H3a N3 H3b 109.5 no C4 N3 H3c 109.5 no H3a N3 H3c 109.5 no H3b N3 H3c 109.5 no N1 C1 H1d 108.7 no C2 C1 H1d 108.7 no N1 C1 H1e 108.7 no C2 C1 H1e 108.7 no H1d C1 H1e 107.6 no N2 C2 H2c 110.2 no C1 C2 H2c 110.2 no N2 C2 H2d 110.2 no C1 C2 H2d 110.2 no H2c C2 H2d 108.5 no N2 C3 H3d 110.2 no C4 C3 H3d 110.2 no N2 C3 H3e 110.2 no C4 C3 H3e 110.2 no H3d C3 H3e 108.5 no N3 C4 H4a 109.9 no C3 C4 H4a 109.9 no N3 C4 H4b 109.9 no C3 C4 H4b 109.9 no H4a C4 H4b 108.3 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Bi1 Cl1 2.705(2) yes Bi1 Cl2 2.636(2) yes Bi1 Cl3 2.729(2) yes Bi1 Cl4 2.826(2) yes Bi1 Cl5 2.769(2) yes Bi1 Cl6 2.625(2) yes N1 C1 1.462(9) no N2 C3 1.490(8) no N2 C2 1.493(8) no N3 C4 1.490(8) no C1 C2 1.520(10) no C3 C4 1.524(8) no N1 H1a 0.90 no N1 H1b 0.90 no N1 H1c 0.90 no N2 H2a 0.90 no N2 H2b 0.90 no N3 H3a 0.90 no N3 H3b 0.90 no N3 H3c 0.90 no C1 H1d 0.97 no C1 H1e 0.97 no C2 H2c 0.97 no C2 H2d 0.97 no C3 H3d 0.97 no C3 H3e 0.97 no C4 H4a 0.97 no C4 H4b 0.97 no 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 N1 H1a Cl3 4_556 0.90 2.34 3.188(6) 157 yes N1 H1b Cl6 2_474 0.90 2.63 3.182(6) 121 yes N1 H1c Cl3 2_574 0.90 2.48 3.191(6) 137 yes N2 H2a Cl4 . 0.90 2.45 3.259(6) 150 yes N2 H2b Cl1 1_655 0.90 2.57 3.224(6) 130 yes N3 H3a Cl4 1_655 0.90 2.52 3.288(6) 143 yes N3 H3a Cl2 4_656 0.90 2.66 3.250(6) 124 yes N3 H3b Cl1 2_575 0.90 2.59 3.305(6) 137 yes N3 H3c Cl5 4_656 0.90 2.39 3.254(5) 161 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 _geom_torsion_publ_flag C3 N2 C2 C1 -177.4(6) no N1 C1 C2 N2 171.9(6) no C2 N2 C3 C4 164.7(5) no N2 C3 C4 N3 170.9(5) no