Controlled Synthesis of a Structurally Characterized Family of Sterically Constrained Heterocyclic Alkoxy-Modified Titanium Alkoxides
Timothy J. Boyle; Robin M. Sewell; Leigh Anna M. Ottley; Harry D. Pratt; Christopher J. Quintana; Scott D. Bunge; Inorganic Chemistry 46 (2007) 1825–1835; doi:10.1021/ic0618798

data_4307363
_publ_contact_author_address     '1001 University Blvd, Albuquerque, NM 87106'
_publ_contact_author_email       tjboyle@sandia.gov
_publ_contact_author_fax         '(505) 272-7336'
_publ_contact_author_name        'Timothy J. Boyle et.al.'
_publ_section_title
;
Controlled Synthesis of a Structurally Characterized Family of Sterically
Constrained Heterocyclic Alkoxy-Modified Titanium Alkoxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1825
_journal_page_last               1835
_journal_paper_doi               10.1021/ic0618798
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C36 H66 N2 O10 Si2 Ti'
_chemical_formula_sum            'C36 H66 N2 O10 Si2 Ti'
_chemical_formula_weight         790.96
_chemical_name_common            '(24) Ti(OPy)2(TOBS)2'
_space_group_IT_number           2
_symmetry_cell_setting           monoclinic
_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                108.046(9)
_cell_angle_beta                 97.543(9)
_cell_angle_gamma                103.088(10)
_cell_formula_units_Z            2
_cell_length_a                   9.198(6)
_cell_length_b                   14.460(9)
_cell_length_c                   18.529(12)
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      1.54
_cell_volume                     2228(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      203(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15477
_diffrn_reflns_theta_full        25.29
_diffrn_reflns_theta_max         25.29
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       irregular
_exptl_crystal_F_000             852.0
_exptl_crystal_size_max          0.445
_exptl_crystal_size_mid          0.338
_exptl_crystal_size_min          0.099
_refine_diff_density_max         1.216
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0965
_refine_ls_shift/su_max          0.353
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+26.0146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2633
_refine_ls_wR_factor_ref         0.2655
_reflns_number_gt                7035
_reflns_number_total             7886
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0618798si20061106_104430_19.cif
_cod_data_source_block           c:\frames\6ma281\worko\6ma281s
_cod_database_code               4307363