Titanium(IV)-Mediated Conversion of Carboxamides to Amidines and Implications for Catalytic Transamidation
Kissounko, Denis A.; Guzei, Ilia A.; Gellman, Samuel H.; Stahl, Shannon S.; Organometallics 24 (2005) 5208–; doi:10.1021/om050768y

data_4076195
_publ_section_title
;
 Titanium(IV)-Mediated Conversion of Carboxamides to Amidines and
 Implications for Catalytic Transamidation
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5208
_journal_paper_doi               10.1021/om050768y
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C37 H53 Cl3 O3 Ti3'
_chemical_formula_weight         795.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.116(2)
_cell_angle_beta                 86.828(3)
_cell_angle_gamma                89.553(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9874(9)
_cell_length_b                   11.7443(9)
_cell_length_c                   19.1979(14)
_cell_measurement_temperature    100(2)
_cell_volume                     1914.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13315
_diffrn_reflns_theta_full        26.67
_diffrn_reflns_theta_max         26.67
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_T_max  0.8214
_exptl_absorpt_correction_T_min  0.7210
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         13318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0657P)^2^+0.3664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1150
_reflns_number_gt                10827
_reflns_number_total             13318
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050768ysi20050905_041217.cif
_cod_data_source_block           stahl39
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4076195