Stibine as a reagent in molecular chemistry - targeted synthesis of primary and secondary stibanyl-gallanes and their lighter homologues.
Schneider, Selina; Ivlev, Sergei; von Hänisch, Carsten; Chemical communications (Cambridge, England) 57 (2021) 3781–3784; doi:10.1039/d0cc08419k

data_7128022
_publ_section_title
;
 Stibine as a reagent in molecular chemistry - targeted synthesis of
 primary and secondary stibanyl-gallanes and their lighter homologues.
;
_journal_issue                   31
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3781
_journal_page_last               3784
_journal_paper_doi               10.1039/d0cc08419k
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C58 H85 Ga2 N4 Sb'
_chemical_formula_sum            'C58 H85 Ga2 N4 Sb'
_chemical_formula_weight         1099.48
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Heat-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-12-30 deposited with the CCDC.	2021-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                85.495(2)
_cell_angle_beta                 85.477(2)
_cell_angle_gamma                64.209(2)
_cell_formula_units_Z            2
_cell_length_a                   14.3990(7)
_cell_length_b                   14.4137(7)
_cell_length_c                   14.9394(7)
_cell_measurement_reflns_used    9004
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.4043
_cell_measurement_theta_min      2.7387
_cell_volume                     2779.6(2)
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_collection       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker AXS Inc., 2019)'
_computing_molecular_graphics    'Diamond v4.6.4 (Brandenburg, 2020)'
_computing_publication_material  'APEX3 v2019.1-0 (Bruker AXS)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'PHOTON 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    '0.8 mm diameter'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            96707
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.591
_diffrn_reflns_theta_min         2.261
_diffrn_source                   'microfocus X-ray tube'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.484
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.7074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1278
_refine_ls_number_reflns         35068
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0273P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0588
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                31955
_reflns_number_total             35068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc08419k2.cif
_cod_data_source_block           SSP239
_cod_depositor_comments
'Adding full bibliography for 7128021--7128025.cif.'
_cod_database_code               7128022
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.741
_shelx_estimated_absorpt_t_max   0.824
_exptl_absorpt_special_details
;Several point groups were tested due to pseudo-merohedral twinning. The best
result in terms of R1 and wR2 was achieved in point group -1.
;
_shelx_res_checksum              22356
_shelx_hkl_checksum              23780