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_1515434
_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         'C38 H27 N5 O14 Ti, 2 (C H Cl3)'
_chemical_formula_sum            'C40 H29 Cl6 N5 O14 Ti'
_chemical_formula_weight         1064.28
_chemical_name_common            '(Hob)Ti(O2C12H4[NO2]4) . 2 CHCl3'
_chemical_name_systematic
;
(2'-(4-p-tolyl-2,4-butanedionato)-biphenyl-2-N-methylacetohydroxamato)-
(3,3',5,5'-tetranitrobiphenyl-2,2'-diolato)titanium(IV)
dichloroform 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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.792(2)
_cell_angle_beta                 102.423(2)
_cell_angle_gamma                93.434(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2931(4)
_cell_length_b                   13.3440(5)
_cell_length_c                   15.1141(6)
_cell_measurement_reflns_used    5632
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.94
_cell_measurement_theta_min      2.51
_cell_volume                     2200.11(15)
_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      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33459
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  0.9571
_exptl_absorpt_correction_T_min  0.9139
_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            yellow
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1080
_exptl_crystal_recrystallization_method
;
Crystals were grown by layering a concentrated solution of the complex
in CHCl3 with hexane.
;
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         9014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0514P)^2^+1.6477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1150
_reflns_number_gt                6501
_reflns_number_total             9014
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0sc00468e.txt
_cod_data_source_block           tetranitro
_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_cell_volume        2200.11(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1515434