Routes to New N-Heterocyclic Carbene Titanium(IV) Imido Complexes
Lorber, Christian; Vendier, Laure; Organometallics 27 (2008) 2774–; doi:10.1021/om800121g

data_4071348
_publ_section_title
;
 Routes to New N-Heterocyclic Carbene Titanium(IV) Imido Complexes
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2774
_journal_paper_doi               10.1021/om800121g
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C44 H54 Cl2 N5 Ti'
_chemical_formula_sum            'C44 H54 Cl2 N5 Ti'
_chemical_formula_weight         771.69
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 93.401(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1103(5)
_cell_length_b                   11.5282(4)
_cell_length_c                   24.8172(9)
_cell_measurement_reflns_used    8707
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.0666
_cell_measurement_theta_min      2.6987
_cell_measurement_wavelength     0.71073
_cell_volume                     4315.4(3)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      -0.0292904387
_diffrn_orient_matrix_UB_12      -0.0471108491
_diffrn_orient_matrix_UB_13      0.003636075
_diffrn_orient_matrix_UB_21      -0.0036493316
_diffrn_orient_matrix_UB_22      -0.0092126521
_diffrn_orient_matrix_UB_23      -0.0283114298
_diffrn_orient_matrix_UB_31      0.0366829037
_diffrn_orient_matrix_UB_32      -0.0385860056
_diffrn_orient_matrix_UB_33      0.0022949172
_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  0.0646
_diffrn_reflns_av_unetI/netI     0.0949
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            33133
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.7
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.357
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         8827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1544
_reflns_number_gt                4634
_reflns_number_total             8827
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om800121g-file001.cif
_cod_data_source_block           (2)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4071348