Low-Valent Gallium, Indium, and Tin Compounds That Contain a Highly Fluorinated Tris(pyrazolyl)borate Ligand: Syntheses and Characterization of [HB(3,5-(CF3)2Pz)3]Ga, [HB(3,5-(CF3)2Pz)3]In, and [HB(3,5-(CF3)2Pz)3]Sn(CF3SO3)
H. V. Rasika Dias; Wiechang Jin; Inorganic Chemistry 39 (2000) 815–819; doi:10.1021/ic9912171

data_4300221
_publ_section_title
;
Low-Valent Gallium, Indium, and Tin Compounds That Contain a Highly
Fluorinated Tris(pyrazolyl)borate Ligand: Syntheses and Characterization
of [HB(3,5-(CF3)2Pz)3]Ga, [HB(3,5-(CF3)2Pz)3]In, and
[HB(3,5-(CF3)2Pz)3]Sn(CF3SO3)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              815
_journal_page_last               819
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C29 H20 B F18 Ga2 I3 N6'
_chemical_formula_weight         1325.46
_chemical_name_common            '[(CF3)2Tp]Ga-GaI3.2(toluene)'
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   19.159(3)
_cell_length_b                   19.159(3)
_cell_length_c                   20.717(4)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      12.54
_cell_measurement_theta_min      2.33
_cell_volume                     6585.7(19)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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      183(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            7035
_diffrn_reflns_theta_full        22.51
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        6.24
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.443
_exptl_absorpt_correction_T_max  0.9706
_exptl_absorpt_correction_T_min  0.7940
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.52
_refine_diff_density_max         1.194
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       0.00001(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         5559
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0874P)^2^+14.9771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1628
_reflns_number_gt                4385
_reflns_number_total             5559
_reflns_threshold_expression     >2sigma(I)
_cod_original_cell_volume        6585.6(18)
_cod_database_code               4300221
_journal_paper_doi 10.1021/ic9912171