Engineering cofacial porphyrin dimers using lacunary polyoxotungstates
Yamaguchi, Masahiro; Yonesato, Kentaro; Shioya, Kaito; Li, Chifeng; Murata, Kei; Ishii, Kazuyuki; Yamaguchi, Kazuya; Suzuki, Kosuke; Chemical Science 16 (2025) 9178–9185; doi:10.1039/D5SC00814J

data_1574476
_publ_section_title
;
 Engineering cofacial porphyrin dimers using lacunary polyoxotungstates
;
_journal_issue                   21
_journal_name_full               'Chemical Science'
_journal_page_first              9178
_journal_page_last               9185
_journal_paper_doi               10.1039/D5SC00814J
_journal_volume                  16
_journal_year                    2025
_chemical_formula_sum            'C100 H68 N20 O124 Si4 W36'
_chemical_formula_weight         10264.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-01-17 deposited with the CCDC.	2025-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                66.2043(6)
_cell_angle_beta                 85.0443(4)
_cell_angle_gamma                69.9358(5)
_cell_formula_units_Z            2
_cell_length_a                   28.75606(13)
_cell_length_b                   31.5544(2)
_cell_length_c                   34.30222(19)
_cell_measurement_reflns_used    213999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      15.1630
_cell_measurement_theta_min      0.5750
_cell_volume                     26701.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       'Rigaku RAPID AUTO'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector
'DECTRIS PILATUS3 X CdTe 1M; Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'SPring-8 BL02B1 Four-circle diffractometer'
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Si(311) double-crystal monochrometer'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4132
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            735910
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        14.354
_diffrn_reflns_theta_max         14.966
_diffrn_reflns_theta_min         0.503
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.888
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             9040
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.020
_refine_diff_density_min         -1.999
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2557
_refine_ls_number_reflns         109209
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+61.7468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                92084
_reflns_number_total             109209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00814j2.cif
_cod_data_source_block           Hybrid-III
_cod_depositor_comments
'Adding full bibliography for 1574475--1574476.cif.'
_cod_database_code               1574476
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.834
_shelx_estimated_absorpt_t_max   0.834
_shelx_res_checksum              26174
_shelx_fab_checksum              57867