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_2020624
_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 (C14 H24 B N4 S2) Cl2 (C5 H5)]'
_chemical_formula_moiety         'C19 H29 B Cl2 N4 S2 Zr'
_chemical_formula_sum            'C19 H29 B Cl2 N4 S2 Zr'
_chemical_formula_weight         550.51
_chemical_name_systematic
'[Bis(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>]dichlorido(\h^5^-cyclopentadienyl)zirconium(IV)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.814(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.202(3)
_cell_length_b                   18.210(6)
_cell_length_c                   13.356(4)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      2.24
_cell_volume                     2481.0(13)
_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 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  0.0718
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40175
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.548
_diffrn_reflns_theta_min         1.525
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6500
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.418
_refine_diff_density_min         -0.566
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   -0.06(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         15132
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0535P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1291
_reflns_number_gt                10542
_reflns_number_total             15132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yp3125sup1.cif
_cod_data_source_block           III
_cod_depositor_comments
'Adding full bibliography for 2020622--2020626.cif.'
_cod_original_cell_volume        2481.1(14)
_cod_database_code               2020624
_shelx_estimated_absorpt_t_min   0.870
_shelx_estimated_absorpt_t_max   0.951
_shelx_hkl_checksum              10967
_shelx_res_checksum              97607