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_4327196
_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_moiety         'C56 H40 N8 P4 Ti, 3(C4 H8 O)'
_chemical_formula_sum            'C68 H64 N8 O3 P4 Ti'
_chemical_formula_weight         1213.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                100.778(3)
_cell_angle_beta                 108.108(3)
_cell_angle_gamma                106.802(3)
_cell_formula_units_Z            2
_cell_length_a                   13.188(3)
_cell_length_b                   14.913(3)
_cell_length_c                   18.002(3)
_cell_measurement_reflns_used    8301
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.0
_cell_volume                     3068.8(11)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0959
_diffrn_reflns_av_sigmaI/netI    0.1279
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30460
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         11155
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.1658
_refine_ls_R_factor_gt           0.1015
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1123P)^2^+1.8595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2324
_refine_ls_wR_factor_ref         0.2751
_reflns_number_gt                6731
_reflns_number_total             11155
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2021066_si_001_1.cif
_cod_data_source_block           w061130a
_cod_original_cell_volume        3068.9(10)
_cod_database_code               4327196