Lewis Acid promoted titanium alkylidene formation: off-cycle intermediates relevant to olefin trimerization catalysis.
Sattler, Aaron; VanderVelde, David G.; Labinger, Jay A.; Bercaw, John E.; Journal of the American Chemical Society 136 (2014) 10790–10800; doi:10.1021/ja5055687

data_4122280
_publ_section_title
;
 Lewis Acid promoted titanium alkylidene formation: off-cycle
 intermediates relevant to olefin trimerization catalysis.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10790
_journal_page_last               10800
_journal_paper_doi               10.1021/ja5055687
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C45 H69 N O2 Si2 Ti'
_chemical_formula_weight         760.09
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                97.266(3)
_cell_angle_beta                 97.906(3)
_cell_angle_gamma                100.804(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6385(5)
_cell_length_b                   11.1526(6)
_cell_length_c                   20.9436(12)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.15
_cell_measurement_theta_min      2.51
_cell_volume                     2163.4(2)
_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-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            97117
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.142
_diffrn_reflns_theta_min         1.882
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.6937
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       plate
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.172
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         16165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+0.7918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1280
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11982
_reflns_number_total             16165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5055687_si_004.cif
_cod_data_source_block           SIMES10
_cod_depositor_comments
'Adding full bibliography for 4122278--4122281.cif.'
_cod_database_code               4122280
_shelx_estimated_absorpt_t_min   0.846
_shelx_estimated_absorpt_t_max   0.972
_shelxl_version_number           2014-2
_shelx_res_checksum              19935
_shelx_hkl_checksum              37442