Synthesis and Structural Characterization of 1,2,4-Diazaphospholide Complexes of Titanium(IV) and Titanium(III)
Wenjun Zheng; Ibon Alkorta; Dongming Yang; Li Wan; Mingang Zhao; José Elguero; Inorganic Chemistry 50 (2011) 12408–12410; doi:10.1021/ic2021066

data_4327197
_publ_section_title
;
 Synthesis and Structural Characterization of 1,2,4-Diazaphospholide
 Complexes of Titanium(IV) and Titanium(III)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12408
_journal_page_last               12410
_journal_paper_doi               10.1021/ic2021066
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C30 H54 N6 P3 Ti'
_chemical_formula_weight         639.60
_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                77.521(7)
_cell_angle_beta                 76.365(8)
_cell_angle_gamma                70.433(7)
_cell_formula_units_Z            2
_cell_length_a                   10.321(5)
_cell_length_b                   12.592(6)
_cell_length_c                   16.792(8)
_cell_measurement_reflns_used    1899
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.616
_cell_measurement_theta_min      2.273
_cell_volume                     1975.8(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0950
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10391
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.9277
_exptl_absorpt_correction_T_min  0.8714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_description       block
_exptl_crystal_F_000             686
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         7210
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1511
_refine_ls_R_factor_gt           0.0992
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1076P)^2^+0.1943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2110
_refine_ls_wR_factor_ref         0.2402
_reflns_number_gt                4509
_reflns_number_total             7210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2021066_si_001_2.cif
_cod_data_source_block           110410fm
_cod_original_cell_volume        1975.9(17)
_cod_database_code               4327197