Gauging electronic dissymmetry in bis-chelates of titanium(iv) using sterically and electronically variable 2,2′-biphenoxides
Kongprakaiwoot, Natcharee; Quiroz-Guzman, Mauricio; Oliver, Allen G.; Brown, Seth N.; Chemical Science 2 (2011) 331–; doi:10.1039/c0sc00468e

data_1515432
_publ_section_title
;
 Gauging electronic dissymmetry in bis-chelates of titanium(iv) using
 sterically and electronically variable 2,2&#x2032;-biphenoxides
;
_journal_issue                   2
_journal_name_full               'Chemical Science'
_journal_page_first              331
_journal_paper_doi               10.1039/c0sc00468e
_journal_volume                  2
_journal_year                    2011
_chemical_formula_moiety         'C50 H44 O6 Ti, 0.5 (C6 H14)'
_chemical_formula_sum            'C53 H51 O6 Ti'
_chemical_formula_weight         831.84
_chemical_name_common            '(Bob)Ti(O2C12H4Me4) . 0.5 C6H14'
_chemical_name_systematic
;
(2,2'-Biphenylbis(4-p-tolyl-2,4-butanedionato))-
(3,3',5,5'-tetramethylbiphenyl-2,2'-diolato)titanium(IV)
hemihexane solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                87.903(2)
_cell_angle_beta                 87.712(3)
_cell_angle_gamma                88.606(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5360(15)
_cell_length_b                   10.7745(17)
_cell_length_c                   21.214(3)
_cell_measurement_reflns_used    1462
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.88
_cell_measurement_theta_min      4.22
_cell_volume                     2175.9(6)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'XL (Sheldrick, 2001)'
_computing_structure_solution    'XS (Sheldrick, 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11691
_diffrn_reflns_theta_full        20.99
_diffrn_reflns_theta_max         20.99
_diffrn_reflns_theta_min         3.99
_exptl_absorpt_coefficient_mu    0.274
_exptl_absorpt_correction_T_max  0.9973
_exptl_absorpt_correction_T_min  0.9891
_exptl_absorpt_correction_type   numerical
_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
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             878
_exptl_crystal_recrystallization_method
;
Crystals were deposited from a saturated solution of the complex
in hexane at room temperature.
;
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         3568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0575P)^2^+0.4964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                2563
_reflns_number_total             3568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0sc00468e.txt
_cod_data_source_block           bobme4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1515432