Reactions of Titanium Hydrazinediido Complexes with Unsaturated Organic Substrates
Weitershaus, Katharina; Lloret Fillol, Julio; Wadepohl, Hubert; Gade, Lutz H.; Organometallics 28 (2009) 4747–; doi:10.1021/om900428d

data_4069824
_publ_section_title
;
 Reactions of Titanium Hydrazinediido Complexes with Unsaturated Organic
 Substrates
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4747
_journal_paper_doi               10.1021/om900428d
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C41 H45 N5 S Ti'
_chemical_formula_weight         687.78
_chemical_properties_physical    air-sensitive
_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     heavy
_atom_sites_solution_secondary   direct
_audit_block_code                ga_kw22
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.934(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5567(11)
_cell_length_b                   18.8324(17)
_cell_length_c                   15.3320(14)
_cell_measurement_reflns_used    7987
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.94
_cell_measurement_theta_min      2.27
_cell_volume                     3606.2(6)
_computing_cell_refinement
;
SAINT (Bruker AXS, 1997-2008)
;
_computing_data_collection       'SMART (Bruker AXS, 1997-2003)'
_computing_data_reduction        'SAINT (Bruker AXS, 1997-2008)'
_computing_molecular_graphics    'PLATON (Spek, 1980-2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (Beurskens et al., 1999-2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997801
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'CCD area detector (Bruker AXS Smart 1000)'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            87398
_diffrn_reflns_theta_full        30.5084
_diffrn_reflns_theta_max         32.27
_diffrn_reflns_theta_min         2.00
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.7031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (Sheldrick & Bruker AXS, 2004-2008)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         12171
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0468P)^2^+3.0534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1262
_reflns_number_gt                9722
_reflns_number_total             12171
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900428d_si_002.cif
_cod_data_source_block           ga_kw22
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4069824
_audit_block_refno               799