Covalently Attached Porphycene-Ferrocene Dyads: Synthesis, Redox-Switched Emission, and Observation of the Charge-Separated State.
Abe, Masaaki; Yamada, Hiroaki; Okawara, Toru; Fujitsuka, Mamoru; Majima, Tetsuro; Hisaeda, Yoshio; Inorganic chemistry 55 (2016) 7–9; doi:10.1021/acs.inorgchem.5b02078

data_4346757
_publ_section_title
;
 Covalently Attached Porphycene-Ferrocene Dyads: Synthesis, Redox-Switched
 Emission, and Observation of the Charge-Separated State.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7
_journal_page_last               9
_journal_paper_doi               10.1021/acs.inorgchem.5b02078
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C45 H50 Cl2 Fe N4 O2'
_chemical_formula_weight         805.64
_chemical_name_common            FcCH2COOPc
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                85.9253(17)
_cell_angle_beta                 85.6604(17)
_cell_angle_gamma                70.0440(17)
_cell_formula_units_Z            1
_cell_length_a                   7.5292(9)
_cell_length_b                   7.5813(9)
_cell_length_c                   18.337(2)
_cell_measurement_reflns_used    9538
_cell_measurement_temperature    296.(2)
_cell_measurement_theta_max      30.7466
_cell_measurement_theta_min      2.8618
_cell_volume                     979.9(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13992
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         1.12
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.990
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.485
_refine_ls_abs_structure_details
;
Flack x determined using 4721 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.679(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         10381
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+1.1366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                9947
_reflns_number_total             10381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02078_si_002.cif
_cod_data_source_block           I
_cod_database_code               4346757