5,20-Diheterohexaphyrins: metal-template-free synthesis and aromaticity switching
Umetani, Masataka; Kim, Jinseok; Tanaka, Takayuki; Kim, Dongho; Osuka, Atsuhiro; Chemical Communications  (2019) –; doi:10.1039/C9CC05580K

data_7123966
_publ_section_title
;
 5,20-Diheterohexaphyrins: metal-template-free synthesis and aromaticity
 switching
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05580K
_journal_year                    2019
_chemical_formula_moiety         'C32 H29 N3 S1, C H Cl3'
_chemical_formula_sum            'C33 H30 Cl3 N3 S'
_chemical_formula_weight         607.05
_chemical_name_systematic        5,20-dithiahexaphyrin
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-06-15 deposited with the CCDC.    2019-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.395(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8418(3)
_cell_length_b                   16.1286(2)
_cell_length_c                   14.8743(3)
_cell_measurement_reflns_used    22673
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      73.3220
_cell_measurement_theta_min      3.6420
_cell_volume                     2999.80(11)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41279
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.821
_diffrn_reflns_theta_min         3.653
_exptl_absorpt_coefficient_mu    3.626
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1264
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.236
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0912P)^2^+2.2185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5088
_reflns_number_total             5980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05580k2.cif
_cod_data_source_block           171204umetani
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_formula_sum        'C33 H30 Cl3 N3 S1'
_cod_database_code               7123966
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              97807