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_4320254
_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            'C15 H19 B Mn N9 O3 S3'
_chemical_formula_weight         535.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 105.730(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.560(8)
_cell_length_b                   14.499(5)
_cell_length_c                   15.183(6)
_cell_measurement_reflns_used    2089
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      1.7
_cell_volume                     4568(3)
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP3 for Windows (L. J. Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS Smart'
_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  0.1211
_diffrn_reflns_av_sigmaI/netI    0.1507
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10833
_diffrn_reflns_theta_full        23.99
_diffrn_reflns_theta_max         23.99
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.794
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.794
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                1450
_reflns_number_total             3578
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010398f_5.cif
_cod_data_source_block           5
_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_database_code               4320254