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_2020625
_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
'[Zr (C7 H11 N2 S) Cl2 (C7 H12 N2 S) (C5 H5)], C6 H6'
_chemical_formula_moiety         'C19 H28 Cl2 N4 S2 Zr, C6 H6'
_chemical_formula_sum            'C25 H34 Cl2 N4 S2 Zr'
_chemical_formula_weight         616.80
_chemical_name_systematic
;(1-<i>tert</i>-butyl-2,3-dihydro-1<i>H</i>-imidazole-2-thione-\k<i>S</i>)(1-<i>tert</i>-butyl-2-sulfanylidene-1<i>H</i>-imidazol-3-ido-\k^2^<i>N</i>^3^,<i>S</i>)dichlorido(\h^5^-cyclopentadienyl)zirconium(IV)
benzene monosolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                93.930(3)
_cell_angle_beta                 92.094(3)
_cell_angle_gamma                118.274(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5741(17)
_cell_length_b                   10.7222(17)
_cell_length_c                   14.246(4)
_cell_measurement_reflns_used    6838
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.17
_cell_volume                     1414.7(5)
_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      125(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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  0.0707
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22462
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.534
_diffrn_reflns_theta_min         1.437
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6564
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.167
_refine_diff_density_min         -0.709
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         8562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                5590
_reflns_number_total             8562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yp3125sup1.cif
_cod_data_source_block           IV
_cod_depositor_comments
'Adding full bibliography for 2020622--2020626.cif.'
_cod_database_code               2020625
_shelx_estimated_absorpt_t_min   0.922
_shelx_estimated_absorpt_t_max   0.978
_shelx_hkl_checksum              46273
_shelx_res_checksum              19451