Protonation Dependent Topological Dichotomy of Core Modified Hexaphyrins: Synthesis, Characterization, and Excited State Dynamics.
Mallick, Abhijit; Oh, Juwon; Majewski, Marcin A.; Stępień, Marcin; Kim, Dongho; Rath, Harapriya; The Journal of organic chemistry 82 (2017) 556–566; doi:10.1021/acs.joc.6b02576

data_4032233
_publ_section_title
;
 Protonation Dependent Topological Dichotomy of Core Modified Hexaphyrins:
 Synthesis, Characterization, and Excited State Dynamics.
;
_journal_issue                   1
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              556
_journal_page_last               566
_journal_paper_doi               10.1021/acs.joc.6b02576
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C74 H42 F10 N4 S4, 2(C7 H8), 3O'
_chemical_formula_sum            'C88 H58 F10 N4 O3 S4'
_chemical_formula_weight         1537.62
_chemical_melting_point          230
_chemical_name_common            'Expanded phorphyrin'
_chemical_name_systematic        'Fused Heterocyclic macrocycle'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                113.593(5)
_cell_angle_beta                 100.841(6)
_cell_angle_gamma                90.554(6)
_cell_formula_units_Z            2
_cell_length_a                   12.123(6)
_cell_length_b                   18.835(10)
_cell_length_c                   19.026(10)
_cell_measurement_reflns_used    5092
_cell_measurement_temperature    100
_cell_measurement_theta_max      20.31
_cell_measurement_theta_min      2.26
_cell_volume                     3893(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16224
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        20.401
_diffrn_reflns_theta_max         20.401
_diffrn_reflns_theta_min         1.185
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'bluish green'
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.518
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     985
_refine_ls_number_reflns         7442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0677
_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^)+(0.1282P)^2^+8.4530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1828
_refine_ls_wR_factor_ref         0.2107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5497
_reflns_number_total             7442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b02576_si_004.cif
_cod_data_source_block           shelx
_cod_database_code               4032233
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.980
_shelx_res_checksum              54376
_shelx_hkl_checksum              37660