Half-Sandwich Titanium(IV) Complexes with Kläui's Tripod Ligand
Tony C. H. Lam; Eddie Y. Y. Chan; Wing-Leung Mak; Samuel M. F. Lo; Ian D. Williams; Wing-Tak Wong; Wa-Hung Leung; Inorganic Chemistry 42 (2003) 1842–1847; doi:10.1021/ic020287w

data_4313331
_publ_section_title
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 Half-Sandwich Titanium(IV) Complexes with Kl\"aui's Tripod Ligand
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1842
_journal_page_last               1847
_journal_paper_doi               10.1021/ic020287w
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C23 H35 Cl5 Co O11 P3 Ti'
_chemical_formula_weight         864.50
_chemical_name_common            '[LOEtTi(Cl4cat)Cl]'
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.298(8)
_cell_length_b                   14.489(7)
_cell_length_c                   14.396(7)
_cell_measurement_temperature    293(2)
_cell_volume                     3608(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0545
_diffrn_reflns_av_sigmaI/netI    0.1119
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1921
_diffrn_reflns_theta_max         19.99
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            Brown?
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       Bar
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.082
_refine_ls_goodness_of_fit_obs   1.282
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         1765
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.115
_refine_ls_restrained_S_obs      1.274
_refine_ls_R_factor_all          0.1634
_refine_ls_R_factor_obs          0.0734
_refine_ls_shift/esd_max         -0.097
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+8.7000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1791
_refine_ls_wR_factor_obs         0.1372
_reflns_number_observed          887
_reflns_number_total             1772
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020287w_4.cif
_cod_data_source_block           LOEtTi(Cl4cat)Cl
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+8.7000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+8.7000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3608.1(30)
_cod_database_code               4313331