Imido−Titanium/Molybdenum Heterobimetallic Systems. Switching from η6-Arene to Fischer-Type Aminocarbene Complexes by Tuning Reactivity Conditions
Lorber, Christian; Vendier, Laure; Organometallics 29 (2010) 1127–; doi:10.1021/om900825a

data_4067304
_publ_section_title
;
 Imido&#x2212;Titanium/Molybdenum Heterobimetallic Systems. Switching from
 \h6-Arene to Fischer-Type Aminocarbene Complexes by Tuning Reactivity
 Conditions
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1127
_journal_paper_doi               10.1021/om900825a
_journal_volume                  29
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C26 H43 Mo1 N5 O6 Ti1'
_chemical_formula_sum            'C26 H43 Mo N5 O6 Ti'
_chemical_formula_weight         665.49
_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                 113.001(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6408(5)
_cell_length_b                   25.6907(10)
_cell_length_c                   13.1933(7)
_cell_measurement_reflns_used    11522
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.1106
_cell_measurement_theta_min      2.6156
_cell_measurement_wavelength     0.71073
_cell_volume                     3319.9(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      -0.0102372196
_diffrn_orient_matrix_UB_12      -0.024503346
_diffrn_orient_matrix_UB_13      0.0202972122
_diffrn_orient_matrix_UB_21      -0.0649425816
_diffrn_orient_matrix_UB_22      0.0082998249
_diffrn_orient_matrix_UB_23      -0.0031579451
_diffrn_orient_matrix_UB_31      -0.0302747931
_diffrn_orient_matrix_UB_32      -0.009566345
_diffrn_orient_matrix_UB_33      -0.0547640115
_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  0.0352
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25658
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.66
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.85648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.27 (release 29-05-2008 CrysAlis171 .NET)
        (compiled May 29 2008,13:12:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.5
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         6789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0362P)^2^+0.0221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                5133
_reflns_number_total             6789
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om900825a_si_001.cif
_cod_data_source_block           6
_cod_database_code               4067304