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_7128021
_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 Sb'
_chemical_formula_sum            'C29 H44 Ga N2 Sb'
_chemical_formula_weight         612.13
_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     dual
_audit_creation_date             2020-12-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-30 deposited with the CCDC.	2021-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.326(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1395(9)
_cell_length_b                   10.0131(5)
_cell_length_c                   18.1242(9)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.68
_cell_measurement_theta_min      2.38
_cell_volume                     2999.9(3)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker D8 Quest'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            96904
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.731
_diffrn_reflns_theta_min         2.330
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.816
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0668 before and 0.0480 after correction. The Ratio of minimum to maximum transmission is 0.8890. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.426
_exptl_crystal_size_mid          0.407
_exptl_crystal_size_min          0.346
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         8511
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0229
_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^)+(0.0223P)^2^+1.9871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7494
_reflns_number_total             8511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc08419k2.cif
_cod_data_source_block           ssp234_0m
_cod_depositor_comments
'Adding full bibliography for 7128021--7128025.cif.'
_cod_database_code               7128021
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.572
_shelx_estimated_absorpt_t_min   0.512
_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
 1.55 with sigma of 0.02
 Sb1'-H1A = Sb1'-H1B
 1.7 with sigma of 0.02
 Sb1'-H1B
 1.75 with sigma of 0.02
 Sb1-H1A = Sb1-H1B
 1.7 with sigma of 0.02
 Sb1-H1B
 1.6 with sigma of 0.02
 Sb1-H1A
 1.8 with sigma of 0.02
3. Others
 Fixed Sof: Sb1(0.5) Sb1'(0.5)
4.a Ternary CH refined with riding coordinates:
 C27(H27), C12(H12), C24(H24), C15(H15)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C20(H20), C22(H22), C21(H21), C8(H8), C10(H10), C9(H9)
4.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C29(H29A,H29B,H29C), C4(H4A,H4B,H4C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C26(H26A,H26B,
 H26C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              39009
_shelx_hkl_checksum              16307
_olex2_submission_special_instructions 'No special instructions were received'