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

data_7129455
_publ_section_title
;
 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         'C76 H104 Bi2 Cl2 Ga2 N4, 2(C7 H8)'
_chemical_formula_sum            'C90 H120 Bi2 Cl2 Ga2 N4'
_chemical_formula_weight         1886.19
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-08
_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                 90.248(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.3919(16)
_cell_length_b                   18.5682(13)
_cell_length_c                   13.8017(11)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.20
_cell_measurement_theta_min      1.65
_cell_volume                     4200.8(6)
_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
_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 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'IPDS 2'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm, multiple pinhole'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            51477
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.209
_diffrn_reflns_theta_min         1.657
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           0.000
_diffrn_source_power             0.000
_diffrn_source_voltage           0
_exptl_absorpt_coefficient_mu    4.920
_exptl_absorpt_correction_T_max  0.2894
_exptl_absorpt_correction_T_min  0.1395
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   'STOE X-AREA, LANA 1.83.8'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       block
_exptl_crystal_F_000             1900
_exptl_crystal_size_rad          0.092
_refine_diff_density_max         1.980
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         11288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8486
_reflns_number_total             11288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06741a2.cif
_cod_data_source_block           compound-5
_cod_database_code               7129455
_shelx_shelxl_version_number     2016/6
_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.a Ternary CH refined with riding coordinates:
 C15(H15), C12(H12), C24(H24), C27(H27)
2.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C10(H10), C2(H2), C20(H20), C32(H32), C8(H8), C22(H22), C21(H21),
 C9(H9), C44(H44), C43(H43), C40(H40), C42(H42), C41(H41)
2.c Idealised Me refined as rotating group:
 C36(H36a,H36b,H36c), C17(H17a,H17b,H17c), C4(H4a,H4b,H4c), C25(H25a,H25b,
 H25c), C38(H38a,H38b,H38c), C29(H29a,H29b,H29c), C37(H37a,H37b,H37c), C5(H5a,
 H5b,H5c), C16(H16a,H16b,H16c), C14(H14a,H14b,H14c), C26(H26a,H26b,H26c),
 C28(H28a,H28b,H28c), C13(H13a,H13b,H13c), C45(H45a,H45b,H45c)
;
_shelx_res_checksum              71897
_olex2_submission_special_instructions 'No special instructions were received'