Supramolecular multi-electron redox photosensitisers comprising a ring-shaped Re(i) tetranuclear complex and a polyoxometalate.
Takahashi, Maria; Asatani, Tsuyoshi; Morimoto, Tatsuki; Kamakura, Yoshinobu; Fujii, Kotaro; Yashima, Masatomo; Hosokawa, Naoki; Tamaki, Yusuke; Ishitani, Osamu; Chemical science 14 (2023) 691–704; doi:10.1039/d2sc04252e

data_1568032
_publ_section_title
;
 Supramolecular multi-electron redox photosensitisers comprising a
 ring-shaped Re(i) tetranuclear complex and a polyoxometalate.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              691
_journal_page_last               704
_journal_paper_doi               10.1039/d2sc04252e
_journal_volume                  14
_journal_year                    2023
_chemical_formula_sum            'C84 H80 F6 N4 O4 P5 Re2'
_chemical_formula_weight         1850.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-02-22 deposited with the CCDC.	2022-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.942(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.0838(11)
_cell_length_b                   16.4902(8)
_cell_length_c                   38.9836(11)
_cell_measurement_reflns_used    15658
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.1570
_cell_measurement_theta_min      2.4020
_cell_volume                     18626.9(13)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0834
_diffrn_reflns_av_unetI/netI     0.0845
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            75368
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.422
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.739
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.29528
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             7384
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         3.212
_refine_diff_density_min         -1.698
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         16375
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.0894
_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^)+(0.1529P)^2^+26.6479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2470
_refine_ls_wR_factor_ref         0.2719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9155
_reflns_number_total             16375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04252e2.cif
_cod_data_source_block           Ring(PF6)4
_cod_depositor_comments
'Adding full bibliography for 1568032--1568033.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1568032
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.922
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              4841
_shelx_hkl_checksum              27433
_platon_squeeze_void_probe_radius 1.20