Experimental Evidence for the Noninnocence of o-Aminothiophenolates: Coordination Chemistry of o-Iminothionebenzosemiquinonate(1-) π-Radicals with Ni(II), Pd(II), Pt(II)
Diran Herebian; Eberhard Bothe; Eckhard Bill; Thomas Weyhermüller; Karl Wieghardt; Journal of the American Chemical Society 123 (2001) 10012–10023; doi:10.1021/ja011155p

data_4115721
_publ_section_title
;
 Experimental Evidence for the Noninnocence of o-Aminothiophenolates:
 Coordination Chemistry of o-Iminothionebenzosemiquinonate(1-) \p-Radicals
 with Ni(II), Pd(II), Pt(II)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10012
_journal_page_last               10023
_journal_paper_doi               10.1021/ja011155p
_journal_volume                  123
_journal_year                    2001
_chemical_formula_structural     '[C28 H42 N2 Pt S2], CH2Cl2'
_chemical_formula_sum            'C29 H44 Cl2 N2 Pt S2'
_chemical_formula_weight         750.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.793(2)
_cell_length_b                   9.8009(8)
_cell_length_c                   28.039(3)
_cell_measurement_reflns_used    13638
_cell_measurement_temperature    100(2)
_cell_volume                     6538.5(10)
_computing_cell_refinement       'Nonius Collect'
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'Nonius Collect'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius Kappa-CCD'
_diffrn_measurement_method       '208 images a 1 deg. in \w and 300 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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15778
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    4.603
_exptl_absorpt_correction_T_max  0.7953
_exptl_absorpt_correction_T_min  0.5463
_exptl_absorpt_correction_type   'gaussian, face indexed'
_exptl_crystal_colour            turquoise
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       'transparent needle'
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.155
_refine_ls_goodness_of_fit_obs   1.266
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6142
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.177
_refine_ls_restrained_S_obs      1.265
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_obs          0.0422
_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^)+(0.0000P)^2^+9.0587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0942
_refine_ls_wR_factor_obs         0.0819
_reflns_number_observed          4177
_reflns_number_total             6214
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja011155p_3.cif
_cod_data_source_block           3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+9.0587P] 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^)+(0.0000P)^2^+9.0587P] 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               4115721