Hydrogallation of Trimethylsilylethynylbenzenes: Generation of Potential Di- and Tripodal Chelating Lewis Acids
Uhl, Werner; Bock, Henrik R.; Breher, Frank; Claesener, Michael; Haddadpour, Sima; Jasper, Beate; Hepp, Alexander; Organometallics 26 (2007) 2363–; doi:10.1021/om061118c

data_4072890
_publ_section_title
;
 Hydrogallation of Trimethylsilylethynylbenzenes:&#x00A0; Generation of
 Potential Di- and Tripodal Chelating Lewis Acids
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2363
_journal_paper_doi               10.1021/om061118c
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C39 H75 Ga3 Si3'
_chemical_formula_weight         837.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.265(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8729(4)
_cell_length_b                   22.0394(7)
_cell_length_c                   15.4207(4)
_cell_measurement_temperature    153(2)
_cell_volume                     4639.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0941
_diffrn_reflns_av_sigmaI/netI    0.1073
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26180
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    1.830
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         8669
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.080
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0752P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1640
_reflns_number_gt                5253
_reflns_number_total             8669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om061118csi20061213_043016.cif
_cod_data_source_block           C39_H75_Ga3_Si3_(7b)
_cod_database_code               4072890