Capture of [Bi4]6− and [Bi3]5− anions by [Rh(L)]+ (L = COD) cations in the closo heteroatomic clusters {Bi4[Rh(L)]4}2− and {Bi3[Rh(L)]3}2−
Liang, Zhibing; Lin, Lifang; Liang, Yuanwei; Wang, Yi; New Journal of Chemistry 47 (2023) 3993–3998; doi:10.1039/D2NJ05883A

data_7062234
_publ_section_title
;
 Capture of [Bi4]6&#x2212; and [Bi3]5&#x2212; anions by [Rh(L)]+ (L = COD)
 cations in the closo heteroatomic clusters {Bi4[Rh(L)]4}2&#x2212; and
 {Bi3[Rh(L)]3}2&#x2212;
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3993
_journal_page_last               3998
_journal_paper_doi               10.1039/D2NJ05883A
_journal_volume                  47
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H64 K2 N4 O12, C32 H48 Bi4 Rh4, 2(C7 H8)'
_chemical_formula_sum            'C37 H64 Bi2 K N2 O6 Rh2'
_chemical_formula_weight         1295.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2015 & ZCIF'
_audit_update_record
;
2022-11-20 deposited with the CCDC.	2023-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.0637(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6378(7)
_cell_length_b                   17.7192(9)
_cell_length_c                   17.8331(9)
_cell_measurement_reflns_used    9721
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.2
_cell_volume                     4306.6(4)
_computing_cell_refinement       'Apex2, Saint'
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        'Apex2, Saint'
_computing_molecular_graphics    'Olex2 (Dolomanov, 2009)'
_computing_publication_material  'Apex2, SHELXL-2015, Platon (Spek, 2015)'
_computing_structure_refinement  'ShelXL-2015 (Sheldrick, 2015c)'
_computing_structure_solution    'ShelXT-2014 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0339273
_diffrn_orient_matrix_UB_12      -0.0381894
_diffrn_orient_matrix_UB_13      -0.0330913
_diffrn_orient_matrix_UB_21      -0.0541758
_diffrn_orient_matrix_UB_22      -0.0036399
_diffrn_orient_matrix_UB_23      0.0361529
_diffrn_orient_matrix_UB_31      -0.0360239
_diffrn_orient_matrix_UB_32      0.0413922
_diffrn_orient_matrix_UB_33      -0.0273209
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43747
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         1.848
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    9.040
_exptl_absorpt_correction_T_max  0.196
_exptl_absorpt_correction_T_min  0.108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Krause et al, 2015)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.999
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.132
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details
;
Flack x (Flack, 1983) determined using 8011 quotients 
[(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1110
_refine_ls_number_reflns         24120
_refine_ls_number_restraints     1130
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0140P)^2^+3.8820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0682
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.925
_reflns_number_gt                19963
_reflns_number_total             24120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj05883a2.cif
_cod_data_source_block           GDOU01
_cod_depositor_comments
'Adding full bibliography for 7062234--7062235.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7062234
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.126
_shelx_estimated_absorpt_t_max   0.293
_shelx_res_checksum              98748