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_4332513
_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            'C25.66667 H51.33333 B10 N2 Si Ti'
_chemical_formula_weight         572.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.254(2)
_cell_angle_beta                 108.672(2)
_cell_angle_gamma                98.419(2)
_cell_formula_units_Z            6
_cell_length_a                   15.4358(11)
_cell_length_b                   16.3485(12)
_cell_length_c                   21.8045(16)
_cell_measurement_temperature    293(2)
_cell_volume                     5134.8(7)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0673
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27758
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8880
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         18006
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1115P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1942
_reflns_number_gt                10964
_reflns_number_total             18006
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0604664sup1.cif
_cod_data_source_block           10(2/3toluene)
_cod_original_cell_volume        5134.8(6)
_cod_original_sg_symbol_H-M      P(-1)
_cod_database_code               4332513