Proton-Coupled Redox Switching in an Annulated π-Extended Core-Modified Octaphyrin.
Sarma, Tridib; Kim, Gakhyun; Sen, Sajal; Cha, Won-Young; Duan, Zhiming; Moore, Matthew D.; Lynch, Vincent M.; Zhang, Zhan; Kim, Dongho; Sessler, Jonathan L.; Journal of the American Chemical Society 140 (2018) 12111–12119; doi:10.1021/jacs.8b06938

data_4132847
_publ_section_title
;
 Proton-Coupled Redox Switching in an Annulated \p-Extended Core-Modified
 Octaphyrin.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12111
_journal_page_last               12119
_journal_paper_doi               10.1021/jacs.8b06938
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety
'C84 H64 N4 S6 2+, 2 Cl 1-, H2 O, 5 C H Cl3, C5 H12'
_chemical_formula_sum            'C94 H83 Cl17 N4 O S6'
_chemical_formula_weight         2079.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5497(17)
_cell_length_b                   16.7205(17)
_cell_length_c                   49.892(7)
_cell_measurement_reflns_used    1911
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.1
_cell_measurement_theta_min      3.20
_cell_volume                     10469(2)
_computing_cell_refinement
'CrysAlisPro V 1.171.38.43f, Agilent Technologies'
_computing_data_collection
'CrysAlisPro V 1.171.38.43f, Agilent Technologies'
_computing_data_reduction
'CrysAlisPro V 1.171.38.43f, Agilent Technologies'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'Shelxl-2016/6, Sheldrick, G. M.'
_computing_structure_refinement  'Shelxl-2016/6, Sheldrick, G. M.'
_computing_structure_solution
;

Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8. SHELXT.  An Integrated Space Group 
and Crystal Structure Determination Program.  

;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Agilent SuperNova with Atlas S2 CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1513
_diffrn_reflns_av_unetI/netI     0.2592
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            35080
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.385
_diffrn_reflns_theta_min         2.787
_diffrn_source                   'sealed microfocus tube'
_exptl_absorpt_coefficient_mu    5.555
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       plate
_exptl_crystal_F_000             4272
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Flack x determined using 1074 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1145
_refine_ls_number_reflns         20049
_refine_ls_number_restraints     781
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.2229
_refine_ls_R_factor_gt           0.1417
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0819P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2946
_refine_ls_wR_factor_ref         0.3695
_reflns_Friedel_coverage         0.792
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.914
_reflns_number_gt                8032
_reflns_number_total             20049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b06938_si_002.cif
_cod_data_source_block           shelx
_cod_database_code               4132847
_shelx_shelxl_version_number     2016/6
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              2603
_shelx_hkl_checksum              74555
_shelx_fab_checksum              27244