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

data_7129458
_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         'C64 H87 Bi Cl2 Ga2 N4'
_chemical_formula_sum            'C64 H87 Bi Cl2 Ga2 N4'
_chemical_formula_weight         1331.76
_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'
_symmetry_Int_Tables_number      2
_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                105.047(6)
_cell_angle_beta                 100.889(6)
_cell_angle_gamma                98.819(7)
_cell_formula_units_Z            2
_cell_length_a                   14.3525(11)
_cell_length_b                   15.4208(13)
_cell_length_c                   17.6984(14)
_cell_measurement_reflns_used    19058
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.46
_cell_measurement_theta_min      1.35
_cell_volume                     3629.2(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 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 0.9914
_diffrn_measured_fraction_theta_max 0.9914
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            58852
_diffrn_reflns_theta_full        29.1808
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         1.56
_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    3.264
_exptl_absorpt_correction_T_max  0.3891
_exptl_absorpt_correction_T_min  0.2559
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   'STOE X-AREA, LANA, 1.83.8'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.2186
_exptl_crystal_description       block
_exptl_crystal_F_000             1350.1042
_exptl_crystal_size_rad          0.104
_refine_diff_density_max         1.4567
_refine_diff_density_min         -0.6094
_refine_diff_density_rms         0.1398
_refine_ls_d_res_high            0.7289
_refine_ls_d_res_low             13.0272
_refine_ls_goodness_of_fit_ref   0.9302
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    134
_refine_ls_number_parameters     678
_refine_ls_number_reflns         19467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9302
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              20
_reflns_limit_k_min              -21
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                16269
_reflns_number_total             19467
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1cc06741a2.cif
_cod_data_source_block           compound-4
_cod_database_code               7129458
_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:
 C41(H41), C24(H24), C15(H15), C44(H44), C27(H27), C56(H56), C12(H12), C53(H53)
2.b Aromatic/amide H refined with riding coordinates:
 C60(H60), C64(H64), C31(H31), C21(H21), C63(H63), C20(H20), C22(H22),
 C10(H10), C8(H8), C9(H9), C37(H37), C39(H39), C51(H51), C49(H49), C38(H38),
 C61(H61), C62(H62), C2(H2), C50(H50)
2.c Idealised Me refined as rotating group:
 C33(H33a,H33b,H33c), C42(H42a,H42b,H42c), C28(H28a,H28b,H28c), C46(H46a,H46b,
 H46c), C34(H34a,H34b,H34c), C25(H25a,H25b,H25c), C17(H17a,H17b,H17c), C43(H43a,
 H43b,H43c), C4(H4a,H4b,H4c), C16(H16a,H16b,H16c), C5(H5a,H5b,H5c), C26(H26a,
 H26b,H26c), C45(H45a,H45b,H45c), C55(H55a,H55b,H55c), C14(H14a,H14b,H14c),
 C29(H29a,H29b,H29c), C13(H13a,H13b,H13c), C54(H54a,H54b,H54c), C57(H57a,H57b,
 H57c), C58(H58a,H58b,H58c)
;
_olex2_submission_special_instructions 'No special instructions were received'