Azadistibiridines and stabilised-iminobismuthane: reactivity of small inorganic rings in heavy main group chemistry.
Palui, Prasenjit; Bollenbeck, Matthias; Meleschko, Daniel; Brehm, Philipp; Gomila, Rosa M.; Schnakenburg, Gregor; Frontera, Antonio; Bismuto, Alessandro; Chemical science 16 (2025) 16894–16903; doi:10.1039/d5sc03416g

data_1575509
_publ_section_title
;
 Azadistibiridines and stabilised-iminobismuthane: reactivity of small
 inorganic rings in heavy main group chemistry.
;
_journal_issue                   36
_journal_name_full               'Chemical science'
_journal_page_first              16894
_journal_page_last               16903
_journal_paper_doi               10.1039/d5sc03416g
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C55 H105 N O2 S Sb2 Si8'
_chemical_formula_sum            'C55 H105 N O2 S Sb2 Si8'
_chemical_formula_weight         1312.67
_chemical_name_systematic        MB043
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-25
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-01 deposited with the CCDC.	2025-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.608(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.2212(7)
_cell_length_b                   13.1556(4)
_cell_length_c                   24.2421(8)
_cell_measurement_reflns_used    21160
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.55
_cell_measurement_theta_min      1.99
_cell_volume                     7023.0(4)
_computing_cell_refinement
;
X-Area Recipe 2.0.1 (STOE, 2023)
;
_computing_data_collection
;
X-Area WinXpose 2.0.29.0 (STOE, 2023)
;
_computing_data_reduction
;
X-Area Integrate 2.5.15.0 (STOE, 2023)
X-Area LANA 2.7.12 (STOE, 2023)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.3, Darmstadt 2023
;
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      '73 frames, detector distance = 70 mm'
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37454
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.997
_diffrn_source                   'Anton Paar Primux50'
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  0.9161
_exptl_absorpt_correction_T_min  0.2937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            'clear greenish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plank
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_crystal_size_rad          0.060
_refine_diff_density_max         1.185
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         16697
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0543P)^2^+18.0200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11588
_reflns_number_total             16697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03416g3.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 1575509--1575515.cif.'
_cod_database_code               1575509
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.728
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C39 \\sim C38 \\sim C41 \\sim C40: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
3.a Ternary CH refined with riding coordinates:
 C7(H7), C18(H18), C31(H31), C42(H42)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C27(H27), C29(H29), C50(H50), C51(H51), C53(H53), C54(H54)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              37036
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '70.0 mm'
_stoe_evaluation_lana_completeness 95.9
_stoe_evaluation_lana_max_2theta_available 66.9
_stoe_evaluation_lana_max_2theta_desired 66.9
_stoe_evaluation_lana_mean_redundancy 2.1
_stoe_evaluation_lana_number_refls_after_or 54177
_stoe_evaluation_lana_number_refls_outliers 7051
_stoe_evaluation_lana_number_refls_total 61228
_stoe_evaluation_lana_number_refls_unique 26314
_stoe_evaluation_lana_number_refls_written 54177
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_table
;
2Theta           6.6   13.8   21.0   28.2   35.4   42.6   49.8   57.0   64.2
<Resolution>    4.90   2.82   1.91   1.44   1.16   0.97   0.84   0.74   0.67
N(total)         220   1163   2630   4563   6854   8689  10783  13276  13050
<Redundancy>     1.9    2.2    2.1    2.2    2.2    2.1    2.0    2.0    2.1
Complet. [%%]    88.9   93.6   95.4   96.5   97.7   97.2   98.1   97.1   91.8
<I/sigma>      120.4   73.2   43.1   27.6   15.7    8.9    5.2    2.3    0.8
R(int)         0.038  0.033  0.032  0.033  0.046  0.070  0.104  0.208  0.419
;
_stoe_measurement_identifier     8332
_stoe_measurement_max_exposure_per_frame '120.0 s'
_stoe_measurement_mean_exposure_per_frame '120.0 s'
_stoe_measurement_min_exposure_per_frame '120.0 s'
_stoe_measurement_total_exposure_time '2.4 h'
_stoe_measurement_total_frame_number 73
_stoe_measurement_total_run_number 1