Synthesis of heteroleptic gallium-substituted antimony hydrides by stepwise β-H elimination.
Helling, Christoph; Wölper, Christoph; Schulz, Stephan; Dalton transactions (Cambridge, England : 2003) 49 (2020) 11835–11842; doi:10.1039/d0dt01937b

data_7705353
_publ_section_title
;
 Synthesis of heteroleptic gallium-substituted antimony hydrides by
 stepwise \b-H elimination.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11835
_journal_page_last               11842
_journal_paper_doi               10.1039/d0dt01937b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C41 H59 Cl Ga N2 Sb'
_chemical_formula_weight         806.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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-2017/1
_audit_update_record
;
2020-05-27 deposited with the CCDC.	2020-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                105.056(3)
_cell_angle_beta                 90.827(4)
_cell_angle_gamma                97.901(4)
_cell_formula_units_Z            4
_cell_length_a                   12.5644(10)
_cell_length_b                   16.2940(13)
_cell_length_c                   20.5464(14)
_cell_measurement_reflns_used    9320
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.31
_cell_measurement_theta_min      2.24
_cell_volume                     4017.9(5)
_computing_cell_refinement       'BRUKER APEX2(v2009.5-1)'
_computing_data_collection       'BRUKER APEX2(v2009.5-1)'
_computing_data_reduction        'BRUKER APEX2(v2009.5-1)'
_computing_molecular_graphics    'ORTEP/PLATON (Spek)'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'BRUKER APEX2(v2009.5-1)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_device_type  'Bruker D8 KAPPA II (APEX II detector)'
_diffrn_measurement_method       'Data collection strategy APEX 2/COSMO'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            143731
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.348
_diffrn_reflns_theta_min         1.434
_exptl_absorpt_coefficient_mu    1.438
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.128
_refine_diff_density_max         2.201
_refine_diff_density_min         -3.789
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         27366
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+5.4857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22087
_reflns_number_total             27366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01937b2.cif
_cod_data_source_block           ch_309m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7705353
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.778
_shelx_estimated_absorpt_t_max   0.837
_shelx_res_checksum              63446