Redox-Active Tripodal Aminetris(aryloxide) Complexes of Titanium(IV)
Davide Lionetti; Andrew J. Medvecz; Vesela Ugrinova; Mauricio Quiroz-Guzman; Bruce C. Noll; Seth N. Brown; Inorganic Chemistry 49 (2010) 4687–4697; doi:10.1021/ic100347h

data_4315523
_publ_section_title
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 Redox-Active Tripodal Aminetris(aryloxide) Complexes of Titanium(IV)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4687
_journal_page_last               4697
_journal_paper_doi               10.1021/ic100347h
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C36 H48 Cl N O6 Ti, C6 H6'
_chemical_formula_sum            'C42 H54 Cl N O6 Ti'
_chemical_formula_weight         752.21
_chemical_name_common            '[N(CH2C6H2-3-tBu-5-OMe-2-O)3]TiCl . C6H6'
_chemical_name_systematic
;
 [Nitrilotris(4-methoxy-6-tert-butyl-o-cresolato)] 
chlorotitanium(IV) benzene solvate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9631(4)
_cell_length_b                   16.7443(6)
_cell_length_c                   26.4720(10)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.40
_cell_volume                     3972.9(3)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2008)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  'XCIF (Sheldrick, 2008)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            47204
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.329
_exptl_absorpt_correction_T_max  0.8963
_exptl_absorpt_correction_T_min  0.8245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Blessing, R. H. (1995) Acta Cryst. A51, 33-38.

 Sheldrick, G. M. (2004) SADABS, University of G\"ottingen, Germany.
;
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1600
_exptl_crystal_recrystallization_method
;
 Crystals were grown by slow evaporation from benzene.
;
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         9703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0445P)^2^+0.1774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                9091
_reflns_number_total             9703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100347h_si_002_3.cif
_cod_data_source_block           omecl
_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 
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_cod_database_code               4315523