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_4300220
_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_paper_doi               10.1021/ic9912171
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C21 H6 B F27 N8 O3 S Sn'
_chemical_formula_weight         1092.90
_chemical_name_common            '[(CF3)2Tp]Sn(CF3SO3).(CF3)2PzH'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 98.299(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2039(11)
_cell_length_b                   15.1935(15)
_cell_length_c                   22.096(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      4.75
_cell_volume                     3389.7(6)
_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      193(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5772
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        12.89
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.686
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         4407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+3.6753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0783
_reflns_number_gt                3910
_reflns_number_total             4407
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               4300220