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_4318584
_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            'C16 H23 Cl3 N4 O3 Ti'
_chemical_formula_weight         473.63
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                90.00
_cell_angle_beta                 100.470(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9870(10)
_cell_length_b                   16.2090(10)
_cell_length_c                   16.9960(10)
_cell_measurement_temperature    293(2)
_cell_volume                     2163.7(3)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1131
_diffrn_reflns_av_sigmaI/netI    0.2881
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5376
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.789
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         5208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.2943
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.184
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.2225
_reflns_number_gt                1761
_reflns_number_total             5208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020319f_4.cif
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318584