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_4322936
_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            'C34 H42 Co Fe N4 S6'
_chemical_formula_weight         813.86
_chemical_name_common            '[Fe(C5Me4StBu)2][Co(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                104.79(2)
_cell_angle_beta                 97.21(2)
_cell_angle_gamma                107.47(2)
_cell_formula_units_Z            2
_cell_length_a                   10.007(5)
_cell_length_b                   14.481(7)
_cell_length_c                   15.024(7)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      20
_cell_volume                     1959.1(17)
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4013
_diffrn_reflns_theta_max         50.00
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 120
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    9.494
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       prism
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0012(2)
_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   1.070
_refine_ls_goodness_of_fit_obs   1.113
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         4013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_restrained_S_obs      1.113
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_obs          0.0505
_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^)+(0.0984P)^2^+0.4746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1364
_refine_ls_wR_factor_obs         0.1240
_reflns_number_observed          3150
_reflns_number_total             4013
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9802045_5.cif
_cod_data_source_block           '[Fe(C5Me4StBu)2][Co(mnt)2]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0984P)^2^+0.4746P] 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^)+(0.0984P)^2^+0.4746P] 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_original_cell_volume        1959.1(16)
_cod_database_code               4322936