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_7128024
_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         'C29 H44 Ga N2 P'
_chemical_formula_sum            'C29 H44 Ga N2 P'
_chemical_formula_weight         521.35
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Heat-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     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                90
_cell_angle_beta                 90.8880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.1045(11)
_cell_length_b                   9.6018(6)
_cell_length_c                   33.3947(19)
_cell_measurement_reflns_used    9089
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.6340
_cell_measurement_theta_min      2.2070
_cell_volume                     5804.5(6)
_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  0.0386
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            140725
_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         29.664
_diffrn_reflns_theta_min         2.207
_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    1.021
_exptl_absorpt_correction_T_max  0.8597
_exptl_absorpt_correction_T_min  0.7102
_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    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.204
_refine_diff_density_max         1.432
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.00097(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         16395
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+5.8150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13464
_reflns_number_total             16395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc08419k2.cif
_cod_data_source_block           SSP242
_cod_depositor_comments
'Adding full bibliography for 7128021--7128025.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7128024
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.635
_shelx_estimated_absorpt_t_max   0.819
_shelx_res_checksum              54319
_shelx_hkl_checksum              72105