Biferrocenium salts with magnetite-like mixed-valence iron: coexistence of Fe3+ and Fe2.5+ in the crystal
Tomoyuki Mochida; Eri Nagabuchi; Masashi Takahashi; Hatsumi Mori; Chem.Commun. 50 (2014) 2481–; doi:10.1039/c3cc49568j

data_7112039
_publ_section_title
;
 Biferrocenium salts with magnetite-like mixed-valence iron: coexistence
 of Fe3+ and Fe2.5+ in the crystal
;
_journal_name_full               Chem.Commun.
_journal_page_first              2481
_journal_paper_doi               10.1039/c3cc49568j
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         '2(C26 H30 Fe2 S2), 3(C8 N4 Ni S4)'
_chemical_formula_sum            'C76 H60 Fe4 N12 Ni3 S16'
_chemical_formula_weight         2053.85
_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-97
_cell_angle_alpha                95.436(3)
_cell_angle_beta                 92.971(3)
_cell_angle_gamma                103.641(3)
_cell_formula_units_Z            1
_cell_length_a                   10.4988(14)
_cell_length_b                   12.0318(16)
_cell_length_c                   17.227(2)
_cell_measurement_temperature    173
_cell_volume                     2099.0(5)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13596
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    1.778
_exptl_absorpt_correction_T_max  0.9323
_exptl_absorpt_correction_T_min  0.6175
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.049
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8525
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0796P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1454
_reflns_number_gt                5921
_reflns_number_total             8525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc49568j.txt
_cod_data_source_block           1
_cod_database_code               7112039