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_1575512
_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         '2(C51 H107 Br2 Ge N Sb2 Si9), C4 H10 O'
_chemical_formula_sum            'C106 H224 Br4 Ge2 N2 O Sb4 Si18'
_chemical_formula_weight         3000.37
_chemical_name_systematic        DM-PP-20
_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
_audit_creation_date             2024-02-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-04-01 deposited with the CCDC.	2025-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.868(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.7931(4)
_cell_length_b                   13.6137(2)
_cell_length_c                   27.7062(4)
_cell_measurement_reflns_used    82998
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.78
_cell_measurement_theta_min      1.55
_cell_volume                     7421.4(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            66932
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.563
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    2.38
_exptl_absorpt_correction_T_max  0.8097
_exptl_absorpt_correction_T_min  0.0984
_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 yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             3084
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.570
_refine_diff_density_min         -2.468
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         17895
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+33.9016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1474
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14766
_reflns_number_total             17895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03416g3.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 1575509--1575515.cif.'
_cod_database_code               1575512
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.648
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C55-C54 = C53-C52
 1.5 with sigma of 0.01
 O-C54 = O-C53
 1.39 with sigma of 0.01
 O-C53 = O-C54
 1.4 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C14 \\sim C15 \\sim C15S \\sim C16 \\sim C16S \\sim C17 \\sim C17S: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002
O \\sim C52 \\sim C53 \\sim C54 \\sim C55: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002
4. Others
 Sof(C15S)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16S)=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=Sof(C17S)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
 Fixed Sof: O(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C53(0.5) H53A(0.5)
 H53B(0.5) C54(0.5) H54A(0.5) H54B(0.5) C55(0.5) H55A(0.5) H55B(0.5) H55C(0.5)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C18(H18), C31(H31), C42(H42)
5.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C54(H54A,H54B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C27(H27), C29(H29)
5.d 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), C15S(H15D,H15E,
 H15F), C16(H16A,H16B,H16C), C16S(H16D,H16E,H16F), C17(H17A,H17B,H17C),
 C17S(H17D,H17E,H17F), 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),
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              33632
_olex2_submission_special_instructions 'No special instructions were received'