Chemical control of the monovalent-divalent electron-transfer phase transition in biferrocenium-TCNQ salts
Tomoyuki Mochida; Yusuke Funasako; Kousuke Takazawa; Masashi Takahashi; Michio M. Matsushita; Tadashi Sugawara; Chem.Commun. 50 (2014) 5473–; doi:10.1039/C4CC01296H

data_7113309
_publ_section_title
;
 Chemical control of the monovalent-divalent electron-transfer phase
 transition in biferrocenium-TCNQ salts
;
_journal_name_full               Chem.Commun.
_journal_page_first              5473
_journal_paper_doi               10.1039/C4CC01296H
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C29 H35 Fe2, 3(C12 H3 F N4)'
_chemical_formula_sum            'C65 H44 F3 Fe2 N12'
_chemical_formula_weight         1161.82
_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                109.208(2)
_cell_angle_beta                 105.134(2)
_cell_angle_gamma                97.578(2)
_cell_formula_units_Z            1
_cell_length_a                   8.6943(11)
_cell_length_b                   12.0631(16)
_cell_length_c                   14.3534(18)
_cell_measurement_reflns_used    5995
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.49
_cell_volume                     1332.5(3)
_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      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6379
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.9209
_exptl_absorpt_correction_T_min  0.9091
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             597
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         4620
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+1.2167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1072
_reflns_number_gt                4444
_reflns_number_total             4620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc01296h1.cif
_cod_data_source_block           iBunPeF1
_cod_database_code               7113309