Synthesis, Structural Characterization, Reactivity, and Thermal Stability of [η5:σ-Me2C(C5H4)(C2B10H10)]Ti(R)(NMe2)
Wang, Hong; Wang, Yaorong; Chan, Hoi-Shan; Xie, Zuowei; Inorganic Chemistry 45 (2006) 5675–5683; doi:10.1021/ic0604664

data_4332509
_publ_section_title
;
 Synthesis, Structural Characterization, Reactivity, and Thermal Stability
 of [\h5:\s-Me2C(C5H4)(C2B10H10)]Ti(R)(NMe2)
;
_journal_issue                   14
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5675
_journal_page_last               5683
_journal_paper_doi               10.1021/ic0604664
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C37 H64 B20 N2 Ti2'
_chemical_formula_weight         848.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.138(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.823(3)
_cell_length_b                   11.9792(16)
_cell_length_c                   21.382(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4658.6(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1845
_diffrn_reflns_av_sigmaI/netI    0.2798
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24922
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7510
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         8225
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.2304
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.096
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.2030
_reflns_number_gt                2500
_reflns_number_total             8225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0604664sup1.cif
_cod_data_source_block           3(2toluene)
_cod_original_cell_volume        4658.6(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4332509