Molecular structures of tris(1-<i>tert</i>-butyl-2-mercaptoimidazolyl)hydroborate complexes of titanium, zirconium and hafnium
Rong, Yi; Sambade, David; Parkin, Gerard; Acta Crystallographica Section C 72 (2016) 806–812; doi:10.1107/S2053229616008925

data_2020626
_publ_section_title
;
 Molecular structures of
 tris(1-<i>tert</i>-butyl-2-mercaptoimidazolyl)hydroborate complexes of
 titanium, zirconium and hafnium
;
_journal_coeditor_code           YP3125
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              806
_journal_page_last               812
_journal_paper_doi               10.1107/S2053229616008925
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Hf (C7 H7)3 (C21 H34 B N6 S3)], 4C6 H6'
_chemical_formula_moiety         'C42 H55 B Hf N6 S3, 4(C6 H6)'
_chemical_formula_sum            'C66 H79 B Hf N6 S3'
_chemical_formula_weight         1241.83
_chemical_name_systematic
;Tribenzyl[tris(1-<i>tert</i>-butyl-2-sulfanylidene-2,3-dihydro-1<i>H</i>-imidazol-3-yl)borato-\k^3^<i>S</i>,<i>S</i>',<i>S</i>'']hafnium(IV) benzene
tetrasolvate
;
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.1441(13)
_cell_length_b                   23.1441(13)
_cell_length_c                   23.1441(13)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.13
_cell_measurement_theta_min      2.16
_cell_volume                     12397.1(12)
_computing_cell_refinement
;
SAINT (Bruker, 2011)
;
_computing_data_collection
;
APEX2 (Bruker, 2011)
;
_computing_data_reduction
;
SAINT (Bruker, 2011)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2399
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            128334
_diffrn_reflns_theta_full        24.990
_diffrn_reflns_theta_max         24.990
_diffrn_reflns_theta_min         1.524
_exptl_absorpt_coefficient_mu    1.828
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6570
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       block
_exptl_crystal_F_000             5136
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.314
_refine_diff_density_min         -0.903
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3649
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+97.7410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.1979
_reflns_number_gt                2164
_reflns_number_total             3649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yp3125sup1.cif
_cod_data_source_block           V
_cod_depositor_comments
'Adding full bibliography for 2020622--2020626.cif.'
_cod_original_cell_volume        12397(2)
_cod_database_code               2020626
_shelx_estimated_absorpt_t_min   0.838
_shelx_estimated_absorpt_t_max   0.914
_shelx_hkl_checksum              17229
_shelx_res_checksum              9803