Trapping reactions with highly unstable hydrides of antimony and bismuth
Schneider, Selina; von Hänisch, Carsten; Chemical Communications  (2022) –; doi:10.1039/D1CC06741A

data_7129457
_publ_section_title
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 Trapping reactions with highly unstable hydrides of antimony and bismuth
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06741A
_journal_year                    2022
_chemical_formula_moiety         'C59 H85 Bi Cl2 Ga2 N4'
_chemical_formula_sum            'C59 H85 Bi Cl2 Ga2 N4'
_chemical_formula_weight         1269.62
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Light-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     dual
_audit_creation_date             2021-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-29 deposited with the CCDC.	2021-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                97.837(2)
_cell_angle_beta                 93.446(2)
_cell_angle_gamma                96.306(2)
_cell_formula_units_Z            4
_cell_length_a                   11.9815(6)
_cell_length_b                   19.7185(8)
_cell_length_c                   25.2053(12)
_cell_measurement_reflns_used    9152
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.37
_cell_volume                     5846.5(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker D8 Quest'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            226883
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.473
_diffrn_reflns_theta_min         1.901
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.048
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1117 before and 0.0652 after correction. The Ratio of minimum to maximum transmission is 0.8477. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       block
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.111
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1314
_refine_ls_number_reflns         29466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0218P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22472
_reflns_number_total             29466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06741a2.cif
_cod_data_source_block           compound-3
_cod_database_code               7129457
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.662
_shelx_estimated_absorpt_t_min   0.464
_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. Others
 Fixed Sof: Bi2(0.95) Bi1(0.95) C15(0.65) H15(0.65) C16(0.65) H16A(0.65)
 H16B(0.65) H16C(0.65) C17(0.65) H17A(0.65) H17B(0.65) H17C(0.65) C15'(0.35)
 H15'(0.35) C17'(0.35) H17D(0.35) H17E(0.35) H17F(0.35) C16'(0.35) H16D(0.35)
 H16E(0.35) H16F(0.35) Bi2'(0.05) Bi1'(0.05)
3.a Ternary CH refined with riding coordinates:
 C56(H56), C74(H74), C24(H24), C112(H112), C44(H44), C27(H27), C100(H100),
 C83(H83), C71(H71), C53(H53), C41(H41), C115(H115), C12(H12), C86(H86),
 C103(H103), C15(H15), C15'(H15')
3.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C61(H61), C39(H39), C38(H38), C79(H79), C90(H90), C69(H69),
 C108(H108), C49(H49), C50(H50), C20(H20), C37(H37), C98(H98), C51(H51),
 C109(H109), C67(H67), C2(H2), C96(H96), C110(H110), C68(H68), C97(H97),
 C22(H22), C9(H9), C21(H21), C81(H81), C10(H10), C8(H8), C80(H80)
3.c Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C93(H93A,H93B,H93C), C34(H34A,H34B,H34C), C33(H33A,H33B,
 H33C), C59(H59A,H59B,H59C), C64(H64A,H64B,H64C), C117(H11A,H11B,H11C),
 C45(H45A,H45B,H45C), C118(H11D,H11E,H11F), C92(H92A,H92B,H92C), C84(H84A,H84B,
 H84C), C116(H11G,H11H,H11I), C58(H58A,H58B,H58C), C5(H5A,H5B,H5C), C75(H75A,
 H75B,H75C), C25(H25A,H25B,H25C), C46(H46A,H46B,H46C), C57(H57A,H57B,H57C),
 C26(H26A,H26B,H26C), C113(H11J,H11K,H11L), C29(H29A,H29B,H29C), C114(H11M,H11N,
 H11O), C101(H10A,H10B,H10C), C43(H43A,H43B,H43C), C76(H76A,H76B,H76C), C4(H4A,
 H4B,H4C), C28(H28A,H28B,H28C), C85(H85A,H85B,H85C), C72(H72A,H72B,H72C),
 C54(H54A,H54B,H54C), C102(H10D,H10E,H10F), C42(H42A,H42B,H42C), C55(H55A,H55B,
 H55C), C13(H13A,H13B,H13C), C105(H10G,H10H,H10I), C104(H10J,H10K,H10L),
 C14(H14A,H14B,H14C), C73(H73A,H73B,H73C), C87(H87A,H87B,H87C), C88(H88A,H88B,
 H88C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C17'(H17D,H17E,H17F),
 C16'(H16D,H16E,H16F)
;
_shelx_res_checksum              56107
_olex2_submission_special_instructions 'No special instructions were received'