Dihydrogen and Silane Addition to Base-Free, Monomeric Bis(cyclopentadienyl)titanium Oxides
Tamara E. Hanna; Emil Lobkovsky; Paul J. Chirik; Inorganic Chemistry 46 (2007) 2359–2361; doi:10.1021/ic070205+

data_4327254
_publ_contact_author_address
;Department of Chemistry
Northwestern University
Evanston, IL 60208-3113
;
_publ_contact_author_email       krp@northwestern.edu
_publ_contact_author_name        'Kenneth R. Poeppelmeier'
_publ_section_title
;
 Dihydrogen and Silane Addition to Base-Free, Monomeric
 Bis(cyclopentadienyl)titanium Oxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2359
_journal_page_last               2361
_journal_paper_doi               10.1021/ic070205+
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C34 H46 O Si2 Ti'
_chemical_formula_weight         574.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 104.178(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1305(13)
_cell_length_b                   8.6746(9)
_cell_length_c                   21.761(2)
_cell_measurement_reflns_used    4065
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      2.54
_cell_volume                     3135.2(5)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_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  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27277
_diffrn_reflns_theta_full        24.76
_diffrn_reflns_theta_max         24.76
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  0.9815
_exptl_absorpt_correction_T_min  0.8648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         5308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.107
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+0.9595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                3697
_reflns_number_total             5308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0702052Bsi20070204_032138.cif
_cod_data_source_block           th27
_cod_database_code               4327254