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_4120155
_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 H30 N4 S8 2-, Zn 2+, 2 C3 H6 O, H2 O, C4 H8 O'
_chemical_formula_sum            'C52 H52 N4 O5 S8 Zn'
_chemical_formula_weight         1134.83
_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                113.127(3)
_cell_angle_beta                 96.240(4)
_cell_angle_gamma                93.010(3)
_cell_formula_units_Z            2
_cell_length_a                   12.755(2)
_cell_length_b                   13.918(2)
_cell_length_c                   16.006(3)
_cell_measurement_reflns_used    32130
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     2583.5(7)
_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 0.966
_diffrn_measured_fraction_theta_max 0.966
_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     0.71075
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1156
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8784
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.639
_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    1.459
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         1.149
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         8784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0747
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1280P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1954
_refine_ls_wR_factor_ref         0.2182
_reflns_number_gt                5811
_reflns_number_total             8784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja404830y_si_006.cif
_cod_data_source_block           shelxl
_cod_database_code               4120155