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_4312617
_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            'C22 H30 Cl N2 O3 V'
_chemical_formula_weight         456.87
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I -2ya'
_symmetry_space_group_name_H-M   'I 1 a 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                 105.296(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.035(2)
_cell_length_b                   11.1489(6)
_cell_length_c                   27.935(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.15
_cell_volume                     4516.7(7)
_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      180(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0817
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            17555
_diffrn_reflns_theta_full        26.11
_diffrn_reflns_theta_max         26.11
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  6
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         8710
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.446
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1186
_reflns_number_gt                6599
_reflns_number_total             8710
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034742fsi20030630_051806_3.cif
_cod_data_source_block           2
_cod_original_cell_volume        4516.6(7)
_cod_original_sg_symbol_H-M      'I a'
_cod_database_code               4312617