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_4301931
_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         '4(C56 H52 N4 O7 V2), 6(C3 H8 O), O4, C3 O'
_chemical_formula_sum            'C245 H264 N16 O39 V8'
_chemical_formula_weight         4464.24
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 98.3800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   24.8548(19)
_cell_length_b                   13.8673(11)
_cell_length_c                   33.590(3)
_cell_measurement_temperature    100(2)
_cell_volume                     11453.8(16)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0651
_diffrn_reflns_av_sigmaI/netI    0.1049
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            64390
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         0.61
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  0.9442
_exptl_absorpt_correction_T_min  0.8618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'North et al., 1968'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4684
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.243
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.031(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1395
_refine_ls_number_reflns         28112
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0670
_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^)+(0.0949P)^2^+6.0705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1852
_reflns_number_gt                19287
_reflns_number_total             28112
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8017985_si_002_5.cif
_cod_data_source_block           19c
_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        11453.9(15)
_cod_original_sg_symbol_Hall     C2y
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               4301931