Dimeric polybismuth heteroanion of [Rh@Bi10(RhCO)5]2- built of Bi10-bowl and Rh@(Rh-CO)5 square pyramidal
Zang, Yipeng; Wang, Yuyue; Sang, Rui-Li; Xu, Li; Dalton Transactions  (2023) –; doi:10.1039/D3DT02402D

data_7714109
_publ_section_title
;
 Dimeric polybismuth heteroanion of [Rh@Bi10(RhCO)5]2- built of Bi10-bowl
 and Rh@(Rh-CO)5 square pyramidal
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02402D
_journal_year                    2023
_chemical_formula_moiety
'C67 H105 Bi20 K3 N8 O28 Rh12, C18 H35 K N2 O6, 3(C), 4(N), [+ solvents]'
_chemical_formula_sum            'C88 H140 Bi20 K4 N14 O34 Rh12'
_chemical_formula_weight         7509.05
_chemical_name_systematic        'C88 H140 Bi20 K4 N14 O34  Rh12'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Efflorescent,Deliquescent,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-09-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-09-09 deposited with the CCDC.	2023-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                97.547(3)
_cell_angle_beta                 101.929(3)
_cell_angle_gamma                100.646(3)
_cell_formula_units_Z            2
_cell_length_a                   16.6076(15)
_cell_length_b                   17.1151(16)
_cell_length_c                   29.840(3)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.19
_cell_volume                     8028.0(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      160.02
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0986
_diffrn_reflns_av_unetI/netI     0.0783
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            98743
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        23.929
_diffrn_reflns_theta_max         23.929
_diffrn_reflns_theta_min         2.257
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.183
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.2295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1644 before and 0.0733 after correction.
The Ratio of minimum to maximum transmission is 0.3081.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.106
_exptl_crystal_description       block
_exptl_crystal_F_000             6628
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.024
_refine_diff_density_min         -1.563
_refine_diff_density_rms         0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1549
_refine_ls_number_reflns         24727
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+130.3474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1132
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18025
_reflns_number_total             24727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02402d2.cif
_cod_data_source_block           mo_m-75_0m
_cod_database_code               7714109
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.205
_shelx_estimated_absorpt_t_min   0.090
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N6-N75
 3 with sigma of 0.02
3. Rigid bond restraints
 C030, C67
 with sigma for 1-2 distances of 0.1 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C56) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(C60) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C42) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C51) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C42) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C02J) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C60) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C74) \\sim Ueq, Uanis(C49) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C47(H47A,H47B), C52(H52A,H52B), C60(H60A,H60B), C65(H65A,
 H65B), C66(H66A,H66B), C69(H69A,H69B), C70(H70A,H70B), C72(H72A,H72B),
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C22(H22A,H22B), C20(H20A,
 H20B), C23(H23A,H23B), C24(H24A,H24B), C76(H76A,H76B), C02U(H02O,H02P),
 C02R(H02A,H02B), C02W(H02Q,H02R), C02X(H02K,H02L), C02F(H02C,H02D), C02J(H02E,
 H02F), C02K(H02G,H02H), C02P(H02M,H02N), C02N(H02I,H02J), C21(H21A,H21B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C030(H03A,
 H03B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C77(H77A,H77B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C59(H59A,H59B), C67(H67A,H67B),
  C64(H64A,H64B), C63(H63A,H63B), C68(H68A,H68B), C73(H73A,H73B), C79(H79A,
 H79B), C62(H62A,H62B), C58(H58A,H58B), C57(H57A,H57B), C56(H56A,H56B),
 C54(H54A,H54B), C78(H78A,H78B), C48(H48A,H48B), C45(H45A,H45B), C44(H44A,H44B),
  C43(H43A,H43B), C25(H25A,H25B), C41(H41A,H41B), C40(H40A,H40B), C39(H39A,
 H39B), C38(H38A,H38B), C55(H55A,H55B), C42(H42A,H42B)
5.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C61(H61), C53(H53), C50(H50)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              21560
_shelx_fab_checksum              60157
_olex2_submission_special_instructions 'No special instructions were received'