Diferrocenylbispyrylium Salts and Electron-Rich Diferrocenylbispyran from Oxidative Coupling of Ferrocenylpyran. Induced Electron Transfer C−C Bond Making/Breaking Involving a Metallocenyl Radical Intermediate
Ba, Fatou; Cabon, Nolwenn; Robin-Le Guen, Françoise; Le Poul, Pascal; Le Poul, Nicolas; Le Mest, Yves; Golhen, Stéphane; Caro, Bertrand; Organometallics 27 (2008) 6396–; doi:10.1021/om800638q

data_4072178
_publ_section_title
;
 Diferrocenylbispyrylium Salts and Electron-Rich Diferrocenylbispyran from
 Oxidative Coupling of Ferrocenylpyran. Induced Electron Transfer
 C&#x2212;C Bond Making/Breaking Involving a Metallocenyl Radical
 Intermediate
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6396
_journal_paper_doi               10.1021/om800638q
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C56 H42 Fe2 O2'
_chemical_formula_weight         858.60
_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                109.8370(10)
_cell_angle_beta                 99.3270(10)
_cell_angle_gamma                90.9180(10)
_cell_formula_units_Z            4
_cell_length_a                   12.9686(3)
_cell_length_b                   16.0334(3)
_cell_length_c                   21.8690(5)
_cell_measurement_reflns_used    17332
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.733
_cell_measurement_theta_min      0.998
_cell_volume                     4208.49(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_sigmaI/netI    0.1056
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31133
_diffrn_reflns_theta_full        26.71
_diffrn_reflns_theta_max         26.71
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1784
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1081
_refine_ls_number_reflns         17721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1654
_refine_ls_R_factor_gt           0.0711
_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^)+(0.1019P)^2^+0.5081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1709
_refine_ls_wR_factor_ref         0.2271
_reflns_number_gt                8149
_reflns_number_total             17721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800638q_si_001.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4072178