Novel aspects of the transamination reaction between Ti(NMe2)4 and primary amines.
Lorber, Christian; Vendier, Laure; Dalton transactions (Cambridge, England : 2003) 42 (2013) 12203–12219; doi:10.1039/c3dt50840d

data_7021667
_publ_section_title
;
 Novel aspects of the transamination reaction between Ti(NMe2)4 and
 primary amines.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12203
_journal_page_last               12219
_journal_paper_doi               10.1039/c3dt50840d
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C14 H12 Cl4 N3 V1'
_chemical_formula_sum            'C14 H14 Cl4 N3 V'
_chemical_formula_weight         417.02
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   23.961(5)
_cell_length_b                   32.093(6)
_cell_length_c                   8.9451(18)
_cell_measurement_reflns_used    4788
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.0956
_cell_measurement_theta_min      2.5446
_cell_measurement_wavelength     0.71073
_cell_volume                     6879(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    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      -0.0600051941
_diffrn_orient_matrix_UB_12      0.0183516362
_diffrn_orient_matrix_UB_13      -0.0045592516
_diffrn_orient_matrix_UB_21      0.0517871912
_diffrn_orient_matrix_UB_22      0.0215761865
_diffrn_orient_matrix_UB_23      -0.0045264792
_diffrn_orient_matrix_UB_31      0.0018702122
_diffrn_orient_matrix_UB_32      -0.0085871932
_diffrn_orient_matrix_UB_33      -0.0211137574
_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  0.0404
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17470
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         32.17
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  0.8912
_exptl_absorpt_correction_T_min  0.7926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       losange
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.099
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         5691
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                3938
_reflns_number_total             5691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50840d.txt
_cod_data_source_block           '[V(N-2,6-Cl2-C6H3)(NMe2)(NH-2,6-Cl2-C6H3)]2'
_cod_database_code               7021667