Ligand-interchange reactions between M(iv) (M = Ti, V) oxide bis-acetylacetonates and halides of high-valent group 4 and 5 metals. A synthetic and electrochemical study.
Funaioli, Tiziana; Marchetti, Fabio; Pampaloni, Guido; Zacchini, Stefano; Dalton transactions (Cambridge, England : 2003) 42 (2013) 14168–14177; doi:10.1039/c3dt51378e

data_7021896
_publ_section_title
;
 Ligand-interchange reactions between M(iv) (M = Ti, V) oxide
 bis-acetylacetonates and halides of high-valent group 4 and 5 metals. A
 synthetic and electrochemical study.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14168
_journal_page_last               14177
_journal_paper_doi               10.1039/c3dt51378e
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C11 H16 Cl F2 O4 Ti'
_chemical_formula_weight         333.59
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.637(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.348(2)
_cell_length_b                   15.929(5)
_cell_length_c                   12.843(4)
_cell_measurement_reflns_used    5327
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.179
_cell_measurement_theta_min      2.5575
_cell_volume                     1502.6(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7195
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  0.8927
_exptl_absorpt_correction_T_min  0.8421
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.432
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2926
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.1051
_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^)+(0.0417P)^2^+18.8955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2541
_refine_ls_wR_factor_ref         0.2550
_reflns_number_gt                2802
_reflns_number_total             2926
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51378e.txt
_cod_data_source_block           p21n
_cod_original_cell_volume        1502.6(9)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7021896