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_4112202
_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            'C38 H51 N7 Ti'
_chemical_formula_weight         653.76
_chemical_name_common            Ti(NNMe2)(But-bpy)(dpma)
_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                 102.151(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.997(11)
_cell_length_b                   20.424(17)
_cell_length_c                   14.061(12)
_cell_measurement_temperature    293(2)
_cell_volume                     3649(5)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0719
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30270
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.270
_exptl_absorpt_correction_T_max  0.8103
_exptl_absorpt_correction_T_min  0.7105
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            dark_blue
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       plate
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0018(3)
_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   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0504P)^2^+2.5710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1225
_reflns_number_gt                3471
_reflns_number_total             5254
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja038320gsi20030908_023011_6.cif
_cod_data_source_block           alo8t
_cod_database_code               4112202