Synthesis, molecular structure (X-ray and DFT), and solution behavior of titanium 4-Acyl-5-pyrazolonates. Correlations with related antitumor beta-diketonato derivatives.
Caruso, Francesco; Pettinari, Claudio; Marchetti, Fabio; Natanti, Paolo; Phillips, Christine; Tanski, Joseph; Rossi, Miriam; Inorganic chemistry 46 (2007) 7553–7560; doi:10.1021/ic700935x

data_4333401
_publ_section_title
;
 Synthesis, molecular structure (X-ray and DFT), and solution behavior of
 titanium 4-Acyl-5-pyrazolonates. Correlations with related antitumor
 beta-diketonato derivatives.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7553
_journal_page_last               7560
_journal_paper_doi               10.1021/ic700935x
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C36 H48 N4 O6 Ti'
_chemical_formula_sum            'C36 H48 N4 O6 Ti'
_chemical_formula_weight         680.68
_chemical_name_systematic
;
bis(4-(3,3-dimethylbutanoyl-3-methyl-1-phenyl)pyrazolon-
5-ato-O,O')-diethoxy-titanium(iv)
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2007-03-11
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.047(4)
_cell_length_b                   11.296(2)
_cell_length_c                   16.169(3)
_cell_measurement_temperature    243(2)
_cell_volume                     3661.5(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0672
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24986
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.282
_exptl_absorpt_correction_T_max  0.9820
_exptl_absorpt_correction_T_min  0.9512
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6139
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                4290
_reflns_number_total             6139
_reflns_threshold_expression     >1.5sigma(I)
_cod_data_source_file            ic700935xsup1.cif
_cod_data_source_block           Ti-mononuclear
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

 Adding full bibliography for 4333401--4333402.cif.
;
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               4333401