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_2020622
_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 (C21 H34 B N6 S3) Cl2 (C5 H5)], 0.5C6 H6'
_chemical_formula_moiety         'C26 H39 B Cl2 N6 S3 Zr, 0.5C6 H6'
_chemical_formula_sum            'C29 H42 B Cl2 N6 S3 Zr'
_chemical_formula_weight         743.79
_chemical_name_systematic
'Dichlorido(\h^5^-cyclopentadienyl)[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>H</i>]zirconium(IV) benzene hemisolvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.130(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.761(3)
_cell_length_b                   11.358(2)
_cell_length_c                   20.730(4)
_cell_measurement_reflns_used    6566
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.28
_cell_volume                     3397.9(11)
_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 0.997
_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  0.1709
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            53472
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.505
_diffrn_reflns_theta_min         1.551
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6575
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.583
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         10340
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0225P)^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         0.1062
_reflns_number_gt                5386
_reflns_number_total             10340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yp3125sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 2020622--2020626.cif.'
_cod_original_cell_volume        3397.8(12)
_cod_database_code               2020622
_shelx_estimated_absorpt_t_min   0.927
_shelx_estimated_absorpt_t_max   0.973
_shelx_hkl_checksum              10642
_shelx_res_checksum              54529