Tetradentate Bis(hydroxamate) and Hydroxamate-Diketonate Ligands and Their Titanium(IV) Complexes
Natcharee Kongprakaiwoot; Bruce C. Noll; Seth N. Brown; Inorganic Chemistry 47 (2008) 11902–11909; doi:10.1021/ic8016479

data_4306788
_publ_section_title
;
Tetradentate Bis(hydroxamate) and Hydroxamate-Diketonate Ligands and Their
Titanium(IV) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11902
_journal_page_last               11909
_journal_paper_doi               10.1021/ic8016479
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C32 H37 N O6 Ti'
_chemical_formula_sum            'C32 H37 N O6 Ti'
_chemical_formula_weight         579.53
_chemical_name_common            (Hob)Ti(OiPr)2
_chemical_name_systematic
;
 (Biphenyl-2'-(4''-p-tolyl-2'',4''-butanedionato)-2-(N-methylacetohydroxamato))-
diisopropoxytitanium(IV)
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.389(13)
_cell_angle_beta                 67.345(8)
_cell_angle_gamma                80.338(15)
_cell_formula_units_Z            2
_cell_length_a                   11.0070(12)
_cell_length_b                   11.816(3)
_cell_length_c                   12.4624(12)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.17
_cell_volume                     1436.8(4)
_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 .998
_diffrn_measured_fraction_theta_max .998
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            53248
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_T_max  0.9665
_exptl_absorpt_correction_T_min  0.8981
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             612
_exptl_crystal_recrystallization_method
;
 Crystals were grown by slow diffusion of hexanes into benzene.
;
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         .347
_refine_diff_density_min         -.385
_refine_diff_density_rms         .051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         7216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0467P)^2^+0.7036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                5911
_reflns_number_total             7216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8016479_si_001_2.cif
_cod_data_source_block           mixtioipr2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'difmap and geom' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4306788