Titanium Hydrazido and Imido Complexes: Synthesis, Structure, Reactivity, and Relevance to Alkyne Hydroamination
Yahong Li; Yanhui Shi; Aaron L. Odom; Journal of the American Chemical Society 126 (2004) 1794–1803; doi:10.1021/ja038320g

data_4112203
_publ_section_title
;
 Titanium Hydrazido and Imido Complexes: Synthesis, Structure, Reactivity,
 and Relevance to Alkyne Hydroamination
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1794
_journal_page_last               1803
_journal_paper_doi               10.1021/ja038320g
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C34 H50 Cl4 I N7 Ti'
_chemical_formula_weight         873.41
_chemical_name_common            '[Ti(NNMe3)(But-bpy)(dpma)]I'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.375(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.154(3)
_cell_length_b                   15.074(4)
_cell_length_c                   19.552(5)
_cell_measurement_temperature    293(2)
_cell_volume                     4137.1(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18390
_diffrn_reflns_theta_full        23.30
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    1.244
_exptl_absorpt_correction_T_max  0.8181
_exptl_absorpt_correction_T_min  0.6985
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.52
_refine_diff_density_max         2.694
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       0.0007(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         5940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0863
_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^)+(0.1335P)^2^+47.7586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2504
_refine_ls_wR_factor_ref         0.2671
_reflns_number_gt                4147
_reflns_number_total             5940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja038320gsi20030908_023011_7.cif
_cod_data_source_block           yahong1t
_cod_original_cell_volume        4137.1(17)
_cod_database_code               4112203