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_4115588
_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_sum            'C17 H22 Fe N3 O4 S'
_chemical_formula_weight         420.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.293(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3937(6)
_cell_length_b                   13.8182(12)
_cell_length_c                   17.329(2)
_cell_measurement_reflns_used    7106
_cell_measurement_temperature    100(2)
_cell_volume                     1770.0(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-scan, 674 frames a 1 deg., 150 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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30347
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    0.999
_exptl_absorpt_correction_type   'Not measured'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       'opaque block'
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.051
_refine_ls_goodness_of_fit_obs   1.090
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         5161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.090
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_obs          0.0250
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+0.6881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0687
_refine_ls_wR_factor_obs         0.0671
_reflns_number_observed          4600
_reflns_number_total             5163
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja004305p_3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+0.6881P] 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^)+(0.0326P)^2^+0.6881P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4115588