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_4115586
_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            'C25 H40 Fe N3 O6'
_chemical_formula_weight         534.45
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                79.81(2)
_cell_angle_beta                 79.28(2)
_cell_angle_gamma                89.99(2)
_cell_formula_units_Z            8
_cell_length_a                   12.468(2)
_cell_length_b                   17.667(3)
_cell_length_c                   25.111(4)
_cell_measurement_reflns_used    24747
_cell_measurement_temperature    100(2)
_cell_volume                     5345.9(16)
_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       ' 852 images a 0.5 deg(\w)/63 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_sigmaI/netI    0.1151
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -32
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_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.9171
_exptl_absorpt_correction_T_min  0.7787
_exptl_absorpt_correction_type   'MulScanAbs, Platon99 program suite'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       'transparent plate'
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.238
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1285
_refine_ls_number_reflns         13738
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.062
_refine_ls_restrained_S_obs      1.237
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_obs          0.0646
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_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+1.7424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1800
_refine_ls_wR_factor_obs         0.1576
_reflns_number_observed          8280
_reflns_number_total             13821
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja004305p_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+1.7424P] 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^)+(0.0860P)^2^+1.7424P] 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        5345.9(15)
_cod_database_code               4115586