Charge-Transfer Salts of Octamethylferrocenyl Thioethers and [M(mnt)2]- Complexes (M = Ni, Co, Pt). Synthesis, Structure, and Physical Properties
Stefan Zürcher; Volker Gramlich; Dieter von Arx; Antonio Togni; Inorganic Chemistry 37 (1998) 4015–4021; doi:10.1021/ic9802045

data_4322932
_publ_section_title
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 Charge-Transfer Salts of Octamethylferrocenyl Thioethers and [M(mnt)2]-
 Complexes (M = Ni, Co, Pt). Synthesis, Structure, and Physical Properties
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4015
_journal_page_last               4021
_journal_paper_doi               10.1021/ic9802045
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C28 H30 Fe N4 Ni S6'
_chemical_formula_weight         729.48
_chemical_name_common            '[Fe(C5Me4SMe)2][Ni(mnt)2]'
_chemical_name_systematic
;
 ?
;
_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                65.27(2)
_cell_angle_beta                 77.77(2)
_cell_angle_gamma                80.78(2)
_cell_formula_units_Z            2
_cell_length_a                   8.649(3)
_cell_length_b                   14.080(4)
_cell_length_c                   15.358(4)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      20
_cell_volume                     1654.8(9)
_computing_cell_refinement       'STOE DIF4'
_computing_data_collection       'PICKER STOE DIF4'
_computing_data_reduction        'STOE REDU4'
_computing_molecular_graphics    SHELXLTL-Plus
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'PICKER 4-circle Stoe upgrade'
_diffrn_measurement_method       ' \w scans'
_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  0.0133
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3362
_diffrn_reflns_theta_max         20.04
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 120
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.411
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       needle
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0000(26)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.051
_refine_ls_goodness_of_fit_obs   1.121
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         3091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.121
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_obs          0.0467
_refine_ls_shift/esd_max         -1.160
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1050P)^2^+0.1664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1323
_refine_ls_wR_factor_obs         0.1293
_reflns_number_observed          2651
_reflns_number_total             3091
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9802045_1.cif
_cod_data_source_block           '[Fe(C5Me4SMe)2][Ni(mnt)2]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1050P)^2^+0.1664P] 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^)+(0.1050P)^2^+0.1664P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322932