A redox-active inorganic crown ether based on a polyoxometalate capsule.
Tamai, Nanako; Ogiwara, Naoki; Hayashi, Eri; Kamata, Keigo; Misawa, Toshiyuki; Ito, Takeru; Kojima, Tatsuhiro; Segado, Mireia; Petrus, Enric; Bo, Carles; Uchida, Sayaka; Chemical science 14 (2023) 5453–5459; doi:10.1039/d3sc01077e

data_1568966
_publ_section_title
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 A redox-active inorganic crown ether based on a polyoxometalate capsule.
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_journal_issue                   20
_journal_name_full               'Chemical science'
_journal_page_first              5453
_journal_page_last               5459
_journal_paper_doi               10.1039/d3sc01077e
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'Cs10 Fe30 Mo72 O382, 12(Mo), P'
_chemical_formula_sum            'Cs10 Fe30 Mo84 O382 P'
_chemical_formula_weight         17206.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2ac'
_space_group_name_H-M_alt        'C c m e'
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
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2023-02-19 deposited with the CCDC.	2023-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.0800(7)
_cell_length_b                   36.9265(7)
_cell_length_c                   34.8114(6)
_cell_measurement_reflns_used    26243
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.21
_cell_measurement_theta_min      1.15
_cell_volume                     45094.0(15)
_computing_cell_refinement       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_reduction        'RAPID-AUTO (Rigaku Corporation)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'RIGAKU 1/4chi goniometer with PILATUS3 X CdTe 1M'
_diffrn_measurement_method       'w scan'
_diffrn_radiation_monochromator  Si(311)
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4132
_diffrn_reflns_av_R_equivalents  0.1201
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            357699
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        14.354
_diffrn_reflns_theta_max         15.563
_diffrn_reflns_theta_min         0.576
_diffrn_source                   'SPring-8 BL02B1 bending magnet'
_exptl_absorpt_coefficient_mu    3.621
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.534
_exptl_crystal_description       prism
_exptl_crystal_F_000             31716
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.726
_refine_diff_density_min         -4.117
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1375
_refine_ls_number_reflns         26198
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0701
_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^)+(0.0958P)^2^+2011.8396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1797
_refine_ls_wR_factor_ref         0.1939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20166
_reflns_number_total             26198
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01077e2.cif
_cod_data_source_block           shelx_sq
_cod_depositor_comments          'Adding full bibliography for 1568966.cif.'
_cod_original_sg_symbol_Hall     '-C 2bc 2bc'
_cod_original_sg_symbol_H-M      'C c m b'
_cod_database_code               1568966
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(Mo30) = Uanis(Mo18)
Uanis(Mo34) = Uanis(Mo16)
Uanis(Mo31) = Uanis(Mo8)
Uanis(Mo5A) = Uanis(Mo5)
Uanis(Mo3A) = Uanis(Mo3)
2. Others
 Sof(Mo)=1-FVAR(1)
 Sof(Mo12)=FVAR(1)
 Sof(Mo20)=1-FVAR(2)
 Sof(Mo19)=FVAR(2)
 Sof(Mo6A)=1-FVAR(3)
 Sof(Mo6)=FVAR(3)
 Sof(Mo8B)=1-FVAR(4)
 Sof(Mo8A)=FVAR(4)
 Sof(Mo11)=1-FVAR(5)
 Sof(Mo28)=FVAR(5)
 Sof(Mo29)=1-FVAR(6)
 Sof(Mo17)=FVAR(6)
 Sof(Mo1A)=1-FVAR(7)
 Sof(Mo1)=FVAR(7)
 Sof(Mo31)=0.5*(1-FVAR(9))
 Sof(Mo8)=0.5*FVAR(9)
 Sof(Mo32)=1-FVAR(9)
 Sof(Mo14)=FVAR(9)
 Sof(Mo2A)=Sof(Mo33)=1-FVAR(10)
 Sof(Mo2)=Sof(Mo15)=FVAR(10)
 Sof(Mo4A)=1-FVAR(11)
 Sof(Mo4)=FVAR(11)
 Sof(Mo34)=0.5*(1-FVAR(13))
 Sof(Mo16)=0.5*FVAR(13)
 Sof(Mo30)=0.5*(1-FVAR(14))
 Sof(Mo18)=0.5*FVAR(14)
 Sof(Mo7A)=1-FVAR(14)
 Sof(Mo7)=FVAR(14)
 Sof(Mo35)=0.5*(1-FVAR(16))
 Sof(Mo13)=0.5*FVAR(16)
 Sof(Mo3A)=1-FVAR(16)
 Sof(Mo3)=FVAR(16)
 Sof(Mo5A)=1-FVAR(17)
 Sof(Mo5)=FVAR(17)
 Sof(Mo10)=1-FVAR(18)
 Sof(Mo36)=FVAR(18)
 Sof(Mo9A)=1-FVAR(19)
 Sof(Mo9)=FVAR(19)
 Fixed Sof: Cs4(0.5) Mo21(0.5) Mo22(0.5) Mo23(0.5) Mo24(0.5) Mo25(0.25)
 Mo26(0.25) Mo27(0.5)
;
_shelx_res_checksum              15574
_shelx_hkl_checksum              3617
_shelx_fab_checksum              34536
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'