Vanadium(V) Complexes of a Chelating Dianionic [ONNO]-Type Amine Bis(Phenolate) Ligand: Synthesis and Solid State and Solution Structures
Fabien Wolff; Christian Lorber; Robert Choukroun; Bruno Donnadieu; Inorganic Chemistry 42 (2003) 7839–7845; doi:10.1021/ic034742f

data_4312616
_publ_contact_author             'Dr. Robert Choukroun, Dr. Christian Lorber'
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
UPR-CNRS 8241
205, route de Narbonne
31077 Toulouse cedex, France   
;
_publ_contact_author_email
'choukrou@lcc-toulouse.fr or lorber@lcc-toulouse.fr'
_publ_contact_author_fax         ' 33 (0) 5 61 55 30 03 '
_publ_section_title
;
 Vanadium(V) Complexes of a Chelating Dianionic [ONNO]-Type Amine
 Bis(Phenolate) Ligand: Synthesis and Solid State and Solution Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7839
_journal_page_last               7845
_journal_paper_doi               10.1021/ic034742f
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C25 H37 N2 O4 V'
_chemical_formula_weight         480.51
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.
_cell_angle_beta                 103.462(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.008(2)
_cell_length_b                   13.075(1)
_cell_length_c                   13.863(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.15
_cell_volume                     2469.3(5)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       \f
_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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18908
_diffrn_reflns_theta_full        26.10
_diffrn_reflns_theta_max         26.10
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  5
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+0.4841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                3898
_reflns_number_total             4820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034742fsi20030630_051806_2.cif
_cod_data_source_block           1a
_cod_original_cell_volume        2469.2(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4312616