Vanadium(V) Complexes of 2,2'-Thiobis(4-methyl-6-tert-butylphenol) (H2mbp2S) and 2,2'-Sulfinylbis(4-methyl-6-tert-butylphenol) (H2mbp2SO)
Charles R. Cornman; Katherine M. Geiser-Bush; Jeff W. Kampf; Inorganic Chemistry 38 (1999) 4303–4308; doi:10.1021/ic9900253

data_4322445
_publ_section_title
;
 Vanadium(V) Complexes of 2,2'-Thiobis(4-methyl-6-tert-butylphenol)
 (H2mbp2S) and 2,2'-Sulfinylbis(4-methyl-6-tert-butylphenol) (H2mbp2SO)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4303
_journal_page_last               4308
_journal_paper_doi               10.1021/ic9900253
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C55 H74 O8 S2 V2'
_chemical_formula_weight         1029.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   35.6184(2)
_cell_length_b                   35.6184(2)
_cell_length_c                   13.52170(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.29
_cell_volume                     14856.30(16)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      158(2)
_diffrn_measurement_device       'Siemens SMART-CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1513
_diffrn_reflns_av_sigmaI/netI    0.0914
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31551
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.388
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.035
_exptl_crystal_description       needle
_exptl_crystal_F_000             4914
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.150
_refine_ls_goodness_of_fit_obs   1.244
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         4315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_restrained_S_obs      1.244
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_obs          0.0996
_refine_ls_shift/esd_max         -0.113
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1273P)^2^+211.1177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2638
_refine_ls_wR_factor_obs         0.2359
_reflns_number_observed          3092
_reflns_number_total             4322
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9900253_1.cif
_cod_data_source_block           Complex1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1273P)^2^+211.1177P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1273P)^2^+211.1177P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        14856.3(2)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4322445