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_1515433
_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         'C42 H39 N O6 Ti, C D Cl3'
_chemical_formula_sum            'C43 H39 Cl3 D N O6 Ti'
_chemical_formula_weight         822.01
_chemical_name_common            '(Hob)Ti(O2C12H4Me4) . CDCl3'
_chemical_name_systematic
;
(2'-(4-p-tolyl-2,4-butanedionato)-biphenyl-2-N-methylacetohydroxamato)-
(3,3',5,5'-tetramethylbiphenyl-2,2'-diolato)titanium(IV)
deuteriochloroform 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                109.3684(14)
_cell_angle_beta                 96.4954(15)
_cell_angle_gamma                106.9980(17)
_cell_formula_units_Z            2
_cell_length_a                   12.0648(5)
_cell_length_b                   12.6467(5)
_cell_length_c                   14.4497(14)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    99(2)
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.78
_cell_volume                     1934.4(2)
_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      99(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28893
_diffrn_reflns_theta_full        26.67
_diffrn_reflns_theta_max         26.67
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.9265
_exptl_absorpt_correction_T_min  0.8845
_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            colorless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_recrystallization_method
;
Crystals were deposited from a concentrated solution of the complex
in CDCl3.
;
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         7854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+1.2134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                6583
_reflns_number_total             7854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0sc00468e.txt
_cod_data_source_block           hobbiph
_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_original_formula_sum        'C43 H39 D Cl3 N O6 Ti'
_cod_database_code               1515433