Influence of the Ti−O−C Angle on the Oxygen-to-Titanium π-Donation in [Cp2*Ti(III)OR] Complexes∥
Gyepes, Róbert; Varga, Vojtech; Horáček, Michal; Kubišta, Jiří; Pinkas, Jiří; Mach, Karel; Organometallics 29 (2010) 3780–; doi:10.1021/om1003495

data_4066204
_publ_section_title
;
 Influence of the Ti&#x2212;O&#x2212;C Angle on the Oxygen-to-Titanium
 \p-Donation in [Cp2*Ti(III)OR] Complexes&#x2225;
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3780
_journal_paper_doi               10.1021/om1003495
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C30 H45 O Ti'
_chemical_formula_sum            'C30 H45 O Ti'
_chemical_formula_weight         469.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.2571(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0960(3)
_cell_length_b                   14.5667(3)
_cell_length_c                   19.8181(6)
_cell_measurement_reflns_used    6055
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2566.02(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\w and \p scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42807
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  0.9599
_exptl_absorpt_correction_T_min  0.7235
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale grey'
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+1.5418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1201
_reflns_number_gt                4285
_reflns_number_total             5873
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1003495_si_001.cif
_cod_data_source_block           compound_3
_cod_original_cell_volume        2566.01(13)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4066204