Preparation of New Monoanionic "Scorpionate" Ligands: Synthesis and Structural Characterization of Titanium(IV) Complexes Bearing This Class of Ligand
A. Otero; J. Fernández-Baeza; A. Antiñolo; F. Carrillo-Hermosilla; J. Tejeda; A. Lara-Sánchez; L. Sánchez-Barba; M. Fernández-López; A. M. Rodríguez; I. López-Solera; Inorganic Chemistry 41 (2002) 5193–5202; doi:10.1021/ic020319f

data_4318583
_publ_section_title
;
 Preparation of New Monoanionic "Scorpionate" Ligands: Synthesis and
 Structural Characterization of Titanium(IV) Complexes Bearing This Class
 of Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5193
_journal_page_last               5202
_journal_paper_doi               10.1021/ic020319f
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C36 H44 Cl14 N8 S6 Ti'
_chemical_formula_weight         1257.3
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.000(0)
_cell_angle_beta                 91.670(3)
_cell_angle_gamma                90.000(0)
_cell_formula_units_Z            4
_cell_length_a                   22.380(4)
_cell_length_b                   13.837(9)
_cell_length_c                   18.574(4)
_cell_measurement_temperature    210(2)
_cell_volume                     5749(4)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XCAD4 (Harms, Wocadlo, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       '\w/2\q 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  0.0879
_diffrn_reflns_av_sigmaI/netI    0.1818
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5206
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.03
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.049
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.0000(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   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5037
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.2470
_refine_ls_R_factor_gt           0.0843
_refine_ls_shift/su_max          0.920
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2043
_refine_ls_wR_factor_ref         0.2794
_reflns_number_gt                2042
_reflns_number_total             5037
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020319f_3.cif
_cod_data_source_block           7
_cod_original_cell_volume        5749(3)
_cod_original_formula_sum        'C36 H44 Cl14 N8 S6 Ti1'
_cod_database_code               4318583