Crystal structure of bis(octahydrocyclopenta[c]pyrrolium)pentachlorobismuthate(III), (C7NH14)2BiCl5
Ma, Yuxin; Hao, Munan; Zhong, Xin; Zhou, Junyan; Zhang, Zeyu; Jin, Shifeng; Zhao, Changchun; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1461–1462; doi:10.1515/ncrs-2020-0358

data_8105494
_publ_section_title
;
 Crystal structure of
 bis(octahydrocyclopenta[c]pyrrolium)pentachlorobismuthate(III),
 (C7NH14)2BiCl5
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1461
_journal_page_last               1462
_journal_paper_doi               10.1515/ncrs-2020-0358
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'Bi Cl5, 2(C7 H14 N)'
_chemical_formula_sum            'C14 H28 Bi Cl5 N2'
_chemical_formula_weight         610.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 104.3220(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6087(3)
_cell_length_b                   7.4645(2)
_cell_length_c                   21.7967(6)
_cell_measurement_reflns_used    5327
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.419
_cell_measurement_theta_min      2.894
_cell_volume                     2145.34(10)
_computing_cell_refinement       'Bruker Smart [1]'
_computing_data_collection       'Bruker Smart [1]'
_computing_data_reduction        'Bruker Smart [1]'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            35963
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.419
_diffrn_reflns_theta_min         2.894
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    8.839
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_density_meas      1.890
_exptl_crystal_density_method    'theoretical calculation'
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             1176.0
_exptl_crystal_size_max          0.980
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.240
_exptl_transmission_factor_max   0.120
_exptl_transmission_factor_min   0.034
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         5327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+0.8204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0528
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4813
_reflns_number_total             5374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0358_suppl.cif
_cod_data_source_block           (c7nh14)2bicl5
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               8105494
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C13(H13), C2(H2), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C12(H12A,H12B), C10(H10A,H10B), C14(H14A,H14B), N1(H1A,H1B),
 C7(H7A,H7B), C1(H1C,H1D), C5(H5A,H5B), C3(H3A,H3B), C4(H4A,H4B), N2(H2A,H2B),
 C11(H11A,H11B)
;