Vanadium Diaminebis(phenolate) Complexes: Syntheses, Structures, and Reactivity in Sulfoxidation Catalysis
Sónia Barroso; Pedro Adão; Filipe Madeira; M. Teresa Duarte; João Costa Pessoa; Ana M. Martins; Inorganic Chemistry 49 (2010) 7452–7463; doi:10.1021/ic1007704

data_4316267
_publ_contact_author_address
;
 Centro de Qu\'imica Estrutural, Instituto Superior T\'ecnico, 
 Av. Rovisco Pais, 1049-001 Lisboa, Portugal. 
;
_publ_contact_author_email       ana.martins@ist.utl.pt
_publ_contact_author_name        'Ana M. Martins'
_publ_section_title
;
 Vanadium Diaminebis(phenolate) Complexes: Syntheses, Structures, and
 Reactivity in Sulfoxidation Catalysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7452
_journal_page_last               7463
_journal_paper_doi               10.1021/ic1007704
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C68 H108 N4 O7 V2, C4 H10 O'
_chemical_formula_sum            'C72 H118 N4 O8 V2'
_chemical_formula_weight         1269.58
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.332(8)
_cell_angle_beta                 89.037(8)
_cell_angle_gamma                89.870(8)
_cell_formula_units_Z            2
_cell_length_a                   11.5810(18)
_cell_length_b                   16.401(3)
_cell_length_c                   20.171(3)
_cell_measurement_reflns_used    1626
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.17
_cell_measurement_theta_min      1.85
_cell_volume                     3705.9(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'BRUKER SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick,1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1491
_diffrn_reflns_av_sigmaI/netI    0.2304
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38464
_diffrn_reflns_theta_full        25.17
_diffrn_reflns_theta_max         25.17
_diffrn_reflns_theta_min         1.85
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.9702
_exptl_absorpt_correction_T_min  0.9558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.719
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     778
_refine_ls_number_reflns         12987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.2226
_refine_ls_R_factor_gt           0.0867
_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^)+(0.1268P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2092
_refine_ls_wR_factor_ref         0.2563
_reflns_number_gt                5306
_reflns_number_total             12987
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic1007704_si_003_5.cif
_cod_data_source_block           5
_cod_original_cell_volume        3705.9(10)
_cod_database_code               4316267