Synthesis, Characterization, and Application of Vanadium-Salan Complexes in Oxygen Transfer Reactions
Pedro Adão; João Costa Pessoa; Rui T. Henriques; Maxim L. Kuznetsov; Fernando Avecilla; Mannar R. Maurya; Umesh Kumar; Isabel Correia; Inorganic Chemistry 48 (2009) 3542–3561; doi:10.1021/ic8017985

data_4301928
_publ_contact_author_address
;
Centro Quimica Estrutural
Instituto Superior Tecnico, TU Lisbon
Av. Rovisco Pais, 1049-001
LISBOA, Portugal
;
_publ_contact_author_email       joao.pessoa@mail.ist.utl.pt
_publ_contact_author_name        'Costa--Pessoa, Jo\~ao'
_publ_section_title
;
Synthesis, Characterization, and Application of Vanadium-Salan Complexes
in Oxygen Transfer Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3542
_journal_page_last               3561
_journal_paper_doi               10.1021/ic8017985
_journal_volume                  48
_journal_year                    2009
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C20 H28 N2 O2, C3 H8 O, H2 O, 2(Cl)'
_chemical_formula_sum            'C23 H38 Cl2 N2 O4'
_chemical_formula_weight         477.45
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 117.3800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.0813(4)
_cell_length_b                   16.0307(7)
_cell_length_c                   9.8496(4)
_cell_measurement_temperature    100(2)
_cell_volume                     1273.27(10)
_computing_cell_refinement       'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0149
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9352
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  0.9258
_exptl_absorpt_correction_T_min  0.8878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'North et al., 1968'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.277
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         4337
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0551P)^2^+0.7346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                4232
_reflns_number_total             4337
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8017985_si_002_2.cif
_cod_data_source_block           1c
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1273.27(9)
_cod_original_sg_symbol_Hall     P2yb
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4301928