Phenylthiyl Radical Complexes of Gallium(III), Iron(III), and Cobalt(III) and Comparison with Their Phenoxyl Analogues
Shuji Kimura; Eckhard Bill; Eberhard Bothe; Thomas Weyhermüller; Karl Wieghardt; Journal of the American Chemical Society 123 (2001) 6025–6039; doi:10.1021/ja004305p

data_4115589
_publ_section_title
;
 Phenylthiyl Radical Complexes of Gallium(III), Iron(III), and Cobalt(III)
 and Comparison with Their Phenoxyl Analogues
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6025
_journal_page_last               6039
_journal_paper_doi               10.1021/ja004305p
_journal_volume                  123
_journal_year                    2001
_chemical_formula_structural     '[C25 H38 Co N3 O4 S], 1 1/6 H2O'
_chemical_formula_sum            'C25 H40.33 Co N3 O5.17 S'
_chemical_formula_weight         556.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_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            12
_cell_length_a                   27.694(5)
_cell_length_b                   27.694(5)
_cell_length_c                   13.188(3)
_cell_measurement_reflns_used    10697
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      1.00
_cell_volume                     8760(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\w, 526 images a 1 deg./120 sec.'
_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  0.3472
_diffrn_reflns_av_sigmaI/netI    0.1497
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13187
_diffrn_reflns_theta_max         17.50
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_type   'Not measured'
_exptl_crystal_colour            'red orange'
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       'very thin needle'
_exptl_crystal_F_000             3548
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.991
_refine_ls_goodness_of_fit_obs   1.200
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         1850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_restrained_S_obs      1.200
_refine_ls_R_factor_all          0.1601
_refine_ls_R_factor_obs          0.0726
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0904P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2404
_refine_ls_wR_factor_obs         0.1652
_reflns_number_observed          924
_reflns_number_total             1857
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja004305p_4.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0904P)^2^+0.0000P] 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^)+(0.0904P)^2^+0.0000P] 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        8759.5(30)
_cod_database_code               4115589