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_4115720
_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 H44 N2 Pd S2], [Et3NH]+, (OCOCH3)- '
_chemical_formula_sum            'C36 H63 N3 O2 Pd S2'
_chemical_formula_weight         740.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 105.90(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.301(2)
_cell_length_b                   14.9776(12)
_cell_length_c                   17.4278(12)
_cell_measurement_reflns_used    8017
_cell_measurement_temperature    100(2)
_cell_volume                     8108.8(13)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SAINT'
_computing_data_reduction        'Siemens SAINT'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Siemens SMART CCD-Detector'
_diffrn_measurement_method       '\w, 0.3 deg/frame'
_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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44295
_diffrn_reflns_theta_max         33.88
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_type   'gaussian, face indexed'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.110
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         14813
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_refine_ls_R_factor_obs          0.0347
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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^)+(0.0432P)^2^+5.0691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0901
_refine_ls_wR_factor_obs         0.0844
_reflns_number_observed          11560
_reflns_number_total             14824
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja011155p_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+5.0691P] 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^)+(0.0432P)^2^+5.0691P] 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        8108.8(10)
_cod_database_code               4115720