Oxidative Transformation of a Tetrathia S-Confused Isophlorin into Porphyrin Cation.
Panchal, Santosh P.; Anand, Venkataramanarao G.; Organic letters 19 (2017) 4854–4857; doi:10.1021/acs.orglett.7b02317

data_1547565
_publ_section_title
;
 Oxidative Transformation of a Tetrathia S-Confused Isophlorin into
 Porphyrin Cation.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              4854
_journal_page_last               4857
_journal_paper_doi               10.1021/acs.orglett.7b02317
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         "'C44 H7 Cl F20 S4, 2(C H2 C12)'"
_chemical_formula_sum            'C46 H11 Cl5 F20 S4'
_chemical_formula_weight         1249.04
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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                101.832(7)
_cell_angle_beta                 96.687(9)
_cell_angle_gamma                104.041(8)
_cell_formula_units_Z            1
_cell_length_a                   8.198(3)
_cell_length_b                   10.441(4)
_cell_length_c                   13.934(5)
_cell_measurement_reflns_used    4278
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.25
_cell_volume                     1115.0(7)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.972
_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  0.0703
_diffrn_reflns_av_unetI/netI     0.0839
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18286
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.572
_diffrn_reflns_theta_min         1.516
_exptl_absorpt_coefficient_mu    0.635
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             616.0
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.357
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.30(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.342
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         8227
_refine_ls_number_restraints     691
_refine_ls_restrained_S_all      1.316
_refine_ls_R_factor_all          0.1227
_refine_ls_R_factor_gt           0.0843
_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^)+(0.1000P)^2^+0.4895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2099
_refine_ls_wR_factor_ref         0.2298
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                5829
_reflns_number_total             11348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b02317_si_002.cif
_cod_data_source_block           7a
_cod_database_code               1547565
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              89690
_shelx_hkl_checksum              20138