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_4306789
_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         'C31 H31 N O7 Ti'
_chemical_formula_sum            'C31 H31 N O7 Ti'
_chemical_formula_weight         577.47
_chemical_name_common            (Hob)Ti(OCH2CMe2CO2)
_chemical_name_systematic
;
 (Biphenyl-2'-(4''-p-tolyl-2'',4''-butanedionato)-2-(N-methylacetohydroxamato))
(2,2-dimethyl-3-oxypropionato)titanium(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   none
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.254(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5051(6)
_cell_length_b                   11.2042(4)
_cell_length_c                   16.9288(6)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      2.54
_cell_volume                     2739.68(18)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            88006
_diffrn_reflns_theta_full        31.58
_diffrn_reflns_theta_max         31.58
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.9337
_exptl_absorpt_correction_T_min  0.8724
_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            yellow
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             1208
_exptl_crystal_recrystallization_method
;
 Crystals were grown by allowing a solution of the compound in 1:2
CH2Cl2:hexanes to stand at 10 deg C overnight.
;
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         9179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0632P)^2^+1.2739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                8043
_reflns_number_total             9179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8016479_si_001_3.cif
_cod_data_source_block           mixpiv
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_database_code               4306789