Structure, Stability, and Catalytic Activity of Fluorine-Bridged Complexes IPr·GaCl2(μ-F)EFn‒1(EFn‒= SbF6‒, PF6‒, or BF4‒)
Bour, Christophe; Monot, Julien; Tang, Shun; Guillot, Régis; Farjon, Jonathan; Gandon, Vincent; Organometallics 33 (2014) 594–; doi:10.1021/om4012054

data_4082330
_publ_section_title
;
 Structure, Stability, and Catalytic Activity of Fluorine-Bridged
 Complexes IPr&#x00B7;GaCl2(\m-F)EFn--1(EFn--= SbF6--, PF6--, or BF4--)
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              594
_journal_paper_doi               10.1021/om4012054
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H36 Cl2 F6 Ga N2 Sb, C6 H14'
_chemical_formula_sum            'C33 H50 Cl2 F6 Ga N2 Sb'
_chemical_formula_weight         851.13
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7680(5)
_cell_length_b                   16.7346(10)
_cell_length_c                   21.5019(13)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.36
_cell_measurement_theta_min      2.25
_cell_volume                     3514.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            36716
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         1.89
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'kappa X8 APEX II Bruker ICMMO'
_exptl_absorpt_coefficient_mu    1.745
_exptl_absorpt_correction_T_max  0.9368
_exptl_absorpt_correction_T_min  0.6034
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.674
_refine_diff_density_min         -2.435
_refine_diff_density_rms         0.214
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         10672
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1180P)^2^+10.1002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.1825
_reflns_number_gt                9652
_reflns_number_total             10672
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4012054_si_001.cif
_cod_data_source_block           1a
_cod_original_formula_sum        'C33 H50 Cl2 F6 Ga N2 Sb '
_cod_database_code               4082330