#------------------------------------------------------------------------------ #$Date: 2025-08-19 11:43:10 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301803 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/67/2206719.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_2206719 loop_ _publ_author_name 'Fu, Yun-Long' 'Xu, Zhi-Wei' 'Ren, Jia-Lin' 'Ng, Seik Weng' _publ_section_title ; Bis[N-methylpiperidinium(2+)] di-\m-chloro-bis[tetrachlorobismuthate(III)] dihydrate ; _journal_coeditor_code HK6031 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m1719 _journal_page_last m1720 _journal_paper_doi 10.1107/S1600536805024451 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '(C5 H14 N2)2 [Bi2 Cl10], 2H2 O' _chemical_formula_moiety '2C5 H14 N2 2+, Bi2 Cl10, 2H2 O' _chemical_formula_sum 'C10 H32 Bi2 Cl10 N4 O2' _chemical_formula_weight 1012.86 _chemical_name_systematic ; Bis[N-methylpiperidinium(2+)] di-\m-chloro-bis[tetrachlorobismuthate(III)] dihydrate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _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 92.9250(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 7.7443(6) _cell_length_b 18.550(2) _cell_length_c 9.9726(8) _cell_measurement_reflns_used 3612 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 28.2 _cell_measurement_theta_min 2.2 _cell_volume 1430.8(2) _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 0.98 _diffrn_measured_fraction_theta_max 0.98 _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 0.030 _diffrn_reflns_av_sigmaI/netI 0.035 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 9046 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 2.2 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 13.232 _exptl_absorpt_correction_T_max 0.504 _exptl_absorpt_correction_T_min 0.183 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 2.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 944 _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.78 _refine_diff_density_min -0.93 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.01 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 128 _refine_ls_number_reflns 3219 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.01 _refine_ls_R_factor_all 0.034 _refine_ls_R_factor_gt 0.027 _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^)+(0.0326P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.061 _refine_ls_wR_factor_ref 0.064 _reflns_number_gt 2724 _reflns_number_total 3219 _reflns_threshold_expression I>2\s(I) _cod_data_source_file hk6031.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2206719 _cod_database_fobs_code 2206719 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 Bi1 0.52096(2) 0.408310(10) 0.62536(2) 0.03328(7) Uani d . 1 Bi Cl1 0.2510(2) 0.49955(7) 0.51750(10) 0.0427(3) Uani d . 1 Cl Cl2 0.7876(2) 0.32776(7) 0.68320(10) 0.0511(3) Uani d . 1 Cl Cl3 0.3186(2) 0.33389(7) 0.77410(10) 0.0490(3) Uani d . 1 Cl Cl4 0.5779(2) 0.49496(8) 0.82970(10) 0.0573(4) Uani d . 1 Cl Cl5 0.4211(2) 0.31313(7) 0.42400(10) 0.0435(3) Uani d . 1 Cl O1w 0.0223(5) 0.4698(2) 0.7953(4) 0.0610(10) Uani d . 1 O N1 -0.1117(6) 0.6074(2) 0.7515(4) 0.0430(10) Uani d . 1 N N2 0.1893(5) 0.6761(2) 0.8749(4) 0.0370(10) Uani d . 1 N C1 0.1881(7) 0.6476(3) 0.7356(5) 0.0420(10) Uani d . 1 C C2 0.0099(7) 0.6477(3) 0.6702(5) 0.0440(10) Uani d . 1 C C3 -0.1149(7) 0.6366(3) 0.8901(5) 0.0460(10) Uani d . 1 C C4 0.0664(7) 0.6358(3) 0.9562(5) 0.0430(10) Uani d . 1 C C5 0.3669(7) 0.6762(3) 0.9409(6) 0.059(2) Uani d . 1 C H1w1 0.1206 0.4674 0.8375 0.073 Uiso d . 1 H H1w2 -0.0493 0.4367 0.8208 0.073 Uiso d . 1 H H1n1 -0.0803 0.5607 0.7551 0.052 Uiso calc R 1 H H1n2 -0.2186 0.6099 0.7119 0.052 Uiso calc R 1 H H2n 0.1529 0.7222 0.8701 0.045 Uiso calc R 1 H H1a 0.2328 0.5987 0.7374 0.050 Uiso calc R 1 H H1b 0.2635 0.6768 0.6831 0.050 Uiso calc R 1 H H2a -0.0299 0.6971 0.6591 0.053 Uiso calc R 1 H H2b 0.0127 0.6260 0.5818 0.053 Uiso calc R 1 H H3a -0.1913 0.6076 0.9422 0.056 Uiso calc R 1 H H3b -0.1588 0.6856 0.8872 0.056 Uiso calc R 1 H H4a 0.0642 0.6572 1.0448 0.051 Uiso calc R 1 H H4b 0.1054 0.5863 0.9667 0.051 Uiso calc R 1 H H5a 0.3619 0.6934 1.0314 0.088 Uiso calc R 1 H H5b 0.4404 0.7073 0.8919 0.088 Uiso calc R 1 H H5c 0.4127 0.6281 0.9417 0.088 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 0.03710(10) 0.02650(10) 0.03630(10) -0.00090(10) 0.00270(10) 0.00030(10) Cl1 0.0396(6) 0.0416(6) 0.0472(7) 0.0032(5) 0.0060(5) 0.0009(5) Cl2 0.0499(8) 0.0421(7) 0.0603(8) 0.0113(6) -0.0078(6) 0.0005(6) Cl3 0.0564(8) 0.0386(6) 0.0533(7) -0.0054(5) 0.0164(6) 0.0013(5) Cl4 0.0765(10) 0.0484(7) 0.0483(7) -0.0170(7) 0.0150(7) -0.0151(6) Cl5 0.0455(7) 0.0406(6) 0.0442(6) -0.0034(5) 0.0002(6) -0.0073(5) O1w 0.063(3) 0.042(2) 0.078(3) -0.002(2) 0.015(2) 0.000(2) N1 0.040(2) 0.042(2) 0.047(2) -0.008(2) -0.005(2) -0.002(2) N2 0.040(2) 0.027(2) 0.044(2) 0.002(2) 0.001(2) -0.004(2) C1 0.042(3) 0.041(3) 0.043(3) 0.001(2) 0.011(2) -0.001(2) C2 0.054(3) 0.043(3) 0.036(3) -0.006(2) 0.001(2) 0.002(2) C3 0.049(3) 0.043(3) 0.048(3) -0.004(2) 0.012(3) -0.004(2) C4 0.055(3) 0.034(3) 0.040(3) -0.004(2) 0.003(2) -0.001(2) C5 0.041(3) 0.056(3) 0.077(4) 0.004(3) -0.014(3) -0.009(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' O O 0.0106 0.0060 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 Bi1 Cl1 . 3_666 85.28(4) yes Cl1 Bi1 Cl2 . . 170.19(4) yes Cl1 Bi1 Cl3 . . 94.49(4) yes Cl1 Bi1 Cl4 . . 91.17(5) yes Cl1 Bi1 Cl5 . . 86.12(4) yes Cl1 Bi1 Cl2 3_666 . 87.17(4) yes Cl1 Bi1 Cl3 3_666 . 174.37(4) yes Cl1 Bi1 Cl4 3_666 . 86.42(4) yes Cl1 Bi1 Cl5 3_666 . 100.13(4) yes Cl2 Bi1 Cl3 . . 93.64(5) yes Cl2 Bi1 Cl4 . . 94.60(5) yes Cl2 Bi1 Cl5 . . 89.05(4) yes Cl3 Bi1 Cl4 . . 87.97(4) yes Cl3 Bi1 Cl5 . . 85.46(4) yes Cl4 Bi1 Cl5 . . 172.67(4) yes Bi1 Cl1 Bi1 . 3_666 94.72(4) no C2 N1 C3 . . 111.6(4) no C4 N2 C1 . . 110.9(4) no C4 N2 C5 . . 111.2(4) no C1 N2 C5 . . 111.9(4) no N2 C1 C2 . . 111.6(4) no N1 C2 C1 . . 111.1(4) no N1 C3 C4 . . 109.9(4) no N2 C4 C3 . . 111.2(4) no H1w1 O1w H1w2 . . 112.6 no C2 N1 H1n1 . . 109.3 no C3 N1 H1n1 . . 109.3 no C2 N1 H1n2 . . 109.3 no C3 N1 H1n2 . . 109.3 no H1n1 N1 H1n2 . . 108.0 no C4 N2 H2n . . 107.5 no C1 N2 H2n . . 107.5 no C5 N2 H2n . . 107.5 no N2 C1 H1a . . 109.3 no C2 C1 H1a . . 109.3 no N2 C1 H1b . . 109.3 no C2 C1 H1b . . 109.3 no H1a C1 H1b . . 108.0 no N1 C2 H2a . . 109.4 no C1 C2 H2a . . 109.4 no N1 C2 H2b . . 109.4 no C1 C2 H2b . . 109.4 no H2a C2 H2b . . 108.0 no N1 C3 H3a . . 109.7 no C4 C3 H3a . . 109.7 no N1 C3 H3b . . 109.7 no C4 C3 H3b . . 109.7 no H3a C3 H3b . . 108.2 no N2 C4 H4a . . 109.4 no C3 C4 H4a . . 109.4 no N2 C4 H4b . . 109.4 no C3 C4 H4b . . 109.4 no H4a C4 H4b . . 108.0 no N2 C5 H5a . . 109.5 no N2 C5 H5b . . 109.5 no H5a C5 H5b . . 109.5 no N2 C5 H5c . . 109.5 no H5a C5 H5c . . 109.5 no H5b C5 H5c . . 109.5 no 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 Bi1 Cl1 . 2.8570(10) yes Bi1 Cl1 3_666 2.8850(10) yes Bi1 Cl2 . 2.5900(10) yes Bi1 Cl3 . 2.6080(10) yes Bi1 Cl4 . 2.6150(10) yes Bi1 Cl5 . 2.7550(10) yes N1 C2 . 1.477(6) no N1 C3 . 1.486(6) no N2 C4 . 1.484(6) no N2 C1 . 1.486(6) no N2 C5 . 1.494(6) no C1 C2 . 1.496(7) no C3 C4 . 1.521(7) no O1w H1w1 . 0.85 no O1w H1w2 . 0.87 no N1 H1n1 . 0.90 no N1 H1n2 . 0.90 no N2 H2n . 0.900 no C1 H1a . 0.97 no C1 H1b . 0.97 no C2 H2a . 0.97 no C2 H2b . 0.97 no C3 H3a . 0.97 no C3 H3b . 0.97 no C4 H4a . 0.97 no C4 H4b . 0.97 no C5 H5a . 0.96 no C5 H5b . 0.96 no C5 H5c . 0.96 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 O1w H1w2 Cl2 1_455 0.87 2.72 3.360(4) 131 yes O1w H1w1 Cl3 . 0.85 3.00 3.423(4) 113 no N1 H1n1 O1w . 0.90 1.90 2.781(6) 167 yes N1 H1n2 Cl5 3_566 0.90 2.47 3.248(5) 145 yes N2 H2n Cl3 2_556 0.90 2.54 3.281(4) 140 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 _geom_torsion_publ_flag Cl3 Bi1 Cl1 Bi1 . 3_666 174.36(4) no Cl4 Bi1 Cl1 Bi1 . 3_666 86.31(4) no Cl5 Bi1 Cl1 Bi1 . 3_666 -100.51(4) no Cl1 Bi1 Cl1 Bi1 3_666 3_666 0.0 no C4 N2 C1 C2 . . 55.2(5) no C5 N2 C1 C2 . . -179.9(4) no C3 N1 C2 C1 . . 56.6(5) no N2 C1 C2 N1 . . -55.5(5) no C2 N1 C3 C4 . . -56.5(5) no C1 N2 C4 C3 . . -55.6(5) no C5 N2 C4 C3 . . 179.2(4) no N1 C3 C4 N2 . . 56.1(5) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139068288