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_7113308
_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         'C30 H38 Fe2, 3(C12 H2.70 F1.30 N4)'
_chemical_formula_sum            'C66 H46.1 F3.9 Fe2 N12'
_chemical_formula_weight         1193.05
_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                109.672(2)
_cell_angle_beta                 104.195(3)
_cell_angle_gamma                98.167(3)
_cell_formula_units_Z            1
_cell_length_a                   8.7096(17)
_cell_length_b                   12.026(2)
_cell_length_c                   14.473(3)
_cell_measurement_reflns_used    3650
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.49
_cell_volume                     1341.3(4)
_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 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0629
_diffrn_reflns_av_sigmaI/netI    0.1274
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5945
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.9677
_exptl_absorpt_correction_T_min  0.8484
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             613
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.121
_refine_diff_density_min         -1.819
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         4568
_refine_ls_number_restraints     306
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_gt           0.1107
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2783
_refine_ls_wR_factor_ref         0.2914
_reflns_number_gt                3787
_reflns_number_total             4568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc01296h1.cif
_cod_data_source_block           npF2(30)
_cod_original_formula_sum        'C66 H46.10 F3.90 Fe2 N12'
_cod_database_code               7113308