Porphyrins Fused with Strongly Electron-Donating 1,3-Dithiol-2-ylidene Moieties: Redox Control by Metal Cation Complexation and Anion Binding
Nathan L. Bill; Masatoshi Ishida; Steffen Bähring; Jong Min Lim; Sangsu Lee; Christina M. Davis; Vincent M. Lynch; Kent A. Nielsen; Jan O. Jeppesen; Kei Ohkubo; Shunichi Fukuzumi; Dongho Kim; Jonathan L. Sessler; Journal of the American Chemical Society 135 (2013) 10852–10862; doi:10.1021/ja404830y

data_4120152
_publ_section_title
;
 Porphyrins Fused with Strongly Electron-Donating 1,3-Dithiol-2-ylidene
 Moieties: Redox Control by Metal Cation Complexation and Anion Binding
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10852
_journal_page_last               10862
_journal_paper_doi               10.1021/ja404830y
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C42 H32 N4 S8, C2 H3 N'
_chemical_formula_sum            'C43 H35 N4 S8'
_chemical_formula_weight         864.23
_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                112.244(2)
_cell_angle_beta                 93.709(3)
_cell_angle_gamma                90.497(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7903(9)
_cell_length_b                   12.3315(10)
_cell_length_c                   15.2801(12)
_cell_measurement_reflns_used    31774
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2050.6(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0909
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9340
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       prisms
_exptl_crystal_F_000             898
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;

;
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         9340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0632
_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^)+(0.0870P)^2^+0.1090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1628
_refine_ls_wR_factor_ref         0.1701
_reflns_number_gt                7535
_reflns_number_total             9340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja404830y_si_003.cif
_cod_data_source_block           shelxl
_cod_database_code               4120152