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

data_7129456
_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         'C60 H90 Bi2 Ga2 N4'
_chemical_formula_sum            'C60 H90 Bi2 Ga2 N4'
_chemical_formula_weight         1424.75
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive,Light-sensitive
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-06
_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                90
_cell_angle_beta                 99.647(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2670(5)
_cell_length_b                   14.2718(6)
_cell_length_c                   19.6277(9)
_cell_measurement_reflns_used    9820
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.32
_cell_volume                     3387.7(3)
_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  0.0674
_diffrn_reflns_av_unetI/netI     0.0348
_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       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            130245
_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         28.891
_diffrn_reflns_theta_min         2.105
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.000
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0924 before and 0.0652 after correction. The Ratio of minimum to maximum transmission is 0.8140. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.086
_refine_diff_density_max         7.311
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         8895
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0784P)^2^+30.1890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6857
_reflns_number_total             8895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06741a2.cif
_cod_data_source_block           compound-2
_cod_database_code               7129456
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.626
_shelx_estimated_absorpt_t_min   0.418
_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. Restrained distances
 Ga1-H
 1.52 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C28(H28), C16(H16), C25(H25), C13(H13)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C21(H21), C11(H11), C22(H22), C23(H23), C9(H9), C10(H10)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C1(H1A,H1B,H1C), C30(H30A,H30B,H30C), C15(H15A,H15B,H15C), C27(H27A,H27B,H27C),
  C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              66424
_shelx_fab_checksum              14077
_olex2_submission_special_instructions 'No special instructions were received'