Synthesis and structural characterization of the first completely alkyl-substituted Ga‒Sb Lewis acid‒base adducts †
Schulz, Stephan; Nieger, Martin; Journal of the Chemical Society, Dalton Transactions  (2000) 639–; doi:10.1039/a908969a

data_7009154
_publ_section_title
;
 Synthesis and structural characterization of the first completely
 alkyl-substituted Ga--Sb Lewis acid--base adducts&#x200A;&#x2020;
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              639
_journal_paper_doi               10.1039/a908969a
_journal_year                    2000
_chemical_formula_sum            'C18 H42 Ga Sb'
_chemical_formula_weight         449.99
_chemical_name_systematic
; 
 Tri(tert.butyl)gallium-triethylantimon-adduct 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.905(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1615(3)
_cell_length_b                   9.5735(2)
_cell_length_c                   16.0291(4)
_cell_measurement_reflns_used    41202
_cell_measurement_temperature    123(2)
_cell_volume                     2172.88(8)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       Collect
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 2 deg.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40096
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    2.477
_exptl_absorpt_correction_T_max  '0.6789 (0.6372; theor.)'
_exptl_absorpt_correction_T_min  '0.4766 (0.4777; theor.)'
_exptl_absorpt_correction_type   'empirical from multiple refl.'
_exptl_absorpt_process_details   'MULABS (Platon98; cf Blessing, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         '1.601 (near Sb)'
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         5368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+10.0050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1140
_reflns_number_gt                5048
_reflns_number_total             5368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a908969a.txt
_cod_data_source_block           s36_mul_compound_5
_cod_original_sg_symbol_H-M      'P2(1)/c (No.14)'
_cod_database_code               7009154