Hydridotris(thioxotriazolyl)borate (Tt), an Ambidentate (N3/S3) Tripodal Ligand. X-ray Crystal Structures of Sodium, Bismuth(III), Tin(IV), and Manganese(I) Complexes
Philip J. Bailey; Maurizio Lanfranchi; Luciano Marchiò; Simon Parsons; Inorganic Chemistry 40 (2001) 5030–5035; doi:10.1021/ic010398f

data_4320253
_publ_contact_author             '     Dr. Philip J. Bailey'
_publ_section_title
;
 Hydridotris(thioxotriazolyl)borate (Tt), an Ambidentate (N3/S3) Tripodal
 Ligand. X-ray Crystal Structures of Sodium, Bismuth(III), Tin(IV), and
 Manganese(I) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5030
_journal_page_last               5035
_journal_paper_doi               10.1021/ic010398f
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C12 H19 B Cl3 N9 S3 Sn'
_chemical_formula_weight         621.39
_chemical_name_systematic
;
 ?
;
_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                 105.936(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.397(2)
_cell_length_b                   11.1712(19)
_cell_length_c                   12.9856(15)
_cell_measurement_reflns_used    10193
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5
_cell_measurement_theta_min      2
_cell_volume                     2287.2(5)
_computing_molecular_graphics    'ORTEP3 for Windows (L. J. Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker AXS Smart Apex'
_diffrn_measurement_method       omega-scan
_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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12650
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    1.762
_exptl_absorpt_correction_T_max  0.862019
_exptl_absorpt_correction_T_min  0.715489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+0.0502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0554
_reflns_number_gt                4212
_reflns_number_total             4648
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010398f_4.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2287.3(6)
_cod_database_code               4320253