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

data_4071353
_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_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C35 H38 Cl5 N5 Ti'
_chemical_formula_sum            'C35 H38 Cl5 N5 Ti'
_chemical_formula_weight         753.85
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 111.287(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1170(8)
_cell_length_b                   10.8360(7)
_cell_length_c                   14.5802(9)
_cell_measurement_reflns_used    5485
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.0901
_cell_measurement_theta_min      2.5993
_cell_measurement_wavelength     0.71073
_cell_volume                     1783.8(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      -0.0117636258
_diffrn_orient_matrix_UB_12      -0.0363939685
_diffrn_orient_matrix_UB_13      -0.0429487386
_diffrn_orient_matrix_UB_21      -0.0038786451
_diffrn_orient_matrix_UB_22      0.0542437828
_diffrn_orient_matrix_UB_23      -0.028260067
_diffrn_orient_matrix_UB_31      0.0616110511
_diffrn_orient_matrix_UB_32      -0.0034840688
_diffrn_orient_matrix_UB_33      0.009431882
_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  0.0553
_diffrn_reflns_av_unetI/netI     0.1006
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12910
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.84818
_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            yellow
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.125
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         6510
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1355P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1895
_refine_ls_wR_factor_ref         0.2093
_reflns_number_gt                4506
_reflns_number_total             6510
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om800121g-file001.cif
_cod_data_source_block           (5)
_cod_database_code               4071353