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

data_7129454
_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         'C33 H52 Ga N2 Sb'
_chemical_formula_sum            'C33 H52 Ga N2 Sb'
_chemical_formula_weight         668.28
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Light-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-25
_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                 100.403(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4394(4)
_cell_length_b                   21.1659(7)
_cell_length_c                   15.5452(5)
_cell_measurement_reflns_used    9548
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.31
_cell_measurement_theta_min      2.18
_cell_volume                     3378.4(2)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker D8 Quest'
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9994
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            98202
_diffrn_reflns_theta_full        25.9983
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.92
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.619
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.7019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0786 before and 0.0477 after correction. The Ratio of minimum to maximum transmission is 0.9459. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.3138
_exptl_crystal_description       plate
_exptl_crystal_F_000             1382.8953
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.171
_refine_diff_density_max         0.6372
_refine_diff_density_min         -0.4380
_refine_diff_density_rms         0.1329
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             10.5829
_refine_ls_goodness_of_fit_ref   1.0707
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    74
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6629
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.0705
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+1.1825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0629
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -12
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              -9
_reflns_number_gt                6056
_reflns_number_total             6629
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1cc06741a2.cif
_cod_data_source_block           compound-1
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7129454
_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
 Sb1-H1
 1.71 with sigma of 0.02
3. Others
 Fixed Sof: Sb1'(0.25) Sb1(0.75)
4.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C27(H27), C24(H24)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C2(H2)
4.c Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C5(H5a,H5b,H5c),
 C29(H29a,H29b,H29c), C26(H26a,H26b,H26c), C17(H17a,H17b,H17c), C33(H33a,H33b,
 H33c), C16(H16a,H16b,H16c), C32(H32a,H32b,H32c), C25(H25a,H25b,H25c), C31(H31a,
 H31b,H31c), C28(H28a,H28b,H28c)
;
_olex2_submission_special_instructions 'No special instructions were received'