Trichloro[tris(3-mesitylpyrazol-1-yl)borohydrido]titanium dichloromethane disolvate
Michiue, Kenji; Steele, Ian; Casagrande, Osvaldo L.; Jordan, Richard F.; Acta Crystallographica Section E 62 (2006) m2297–m2298; doi:10.1107/S1600536806032788

data_2210039
_publ_section_title
;
 Trichloro[tris(3-mesitylpyrazol-1-yl)borohydrido]titanium
 dichloromethane disolvate
;
_journal_coeditor_code           AC2031
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2297
_journal_page_last               m2298
_journal_paper_doi               10.1107/S1600536806032788
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Ti (C36 H40 B N6) Cl3], 2C H2 Cl2'
_chemical_formula_moiety         'C36 H40 B Cl3 N6 Ti, 2C H2 Cl2'
_chemical_formula_sum            'C38 H44 B Cl7 N6 Ti'
_chemical_formula_weight         891.65
_chemical_name_systematic
;
Trichloro[tris(3-mesitylpyrazol-1-yl)borohydrido]titanium dichloromethane
disolvate
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.484(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.964(3)
_cell_length_b                   22.940(7)
_cell_length_c                   11.844(4)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.48
_cell_volume                     2150.0(13)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SADABS (Bruker, 2002)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2002)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16493
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.641
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3894
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+0.8057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                3026
_reflns_number_total             3894
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ac2031.cif
_cod_data_source_block           I
_cod_original_cell_volume        2149.9(12)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2210039
_cod_database_fobs_code          2210039