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_4120156
_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+, Cl 1-, C16 H36 N 1+, C H2 Cl2'
_chemical_formula_sum            'C59 H68 Cl3 N5 S8 Zn'
_chemical_formula_weight         1275.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.706(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5587(13)
_cell_length_b                   17.4010(15)
_cell_length_c                   24.074(2)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.8
_cell_measurement_theta_min      2.7
_cell_volume                     6358.1(9)
_computing_cell_refinement       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_collection       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_reduction        'Apex II release 2010, Bruker AXS, Inc.'
_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      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius Kappa CCD with Bruker Apex II detector'
_diffrn_measurement_method       '\w and \f-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  0.0990
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            140754
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS.  Apex II release 2010, Bruker AXS, Inc.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       laths
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.763
_refine_diff_density_min         -1.651
_refine_diff_density_rms         0.321
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.249
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         11203
_refine_ls_number_restraints     456
_refine_ls_restrained_S_all      1.232
_refine_ls_R_factor_all          0.2200
_refine_ls_R_factor_gt           0.2099
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1496P)^2^+487.1732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5358
_refine_ls_wR_factor_ref         0.5424
_reflns_number_gt                9835
_reflns_number_total             11203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja404830y_si_007.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        6358.2(9)
_cod_database_code               4120156