Inorganic–organic hybrid supramolecular architectures based on Keggin polyoxometalates and crown ether: synthesis, crystal structure and electrochemical properties
Shi, Jianhang; Zhang, Hongxu; Wang, Peisen; Wang, Pai; Zha, Junjie; Liu, Yi; Gautam, Jagadis; Zhang, Lu-Nan; Wang, Yue; Xie, Ju; Ni, Lubin; Diao, Guowang; Wei, Yongge; CrystEngComm 23 (2021) 8482–8489; doi:10.1039/D1CE01203G

data_7243820
_publ_section_title
;
 Inorganic--organic hybrid supramolecular architectures based on Keggin
 polyoxometalates and crown ether: synthesis, crystal structure and
 electrochemical properties
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              8482
_journal_page_last               8489
_journal_paper_doi               10.1039/D1CE01203G
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C52 H102 K4 N2 O64 Si W12'
_chemical_formula_sum            'C52 H102 K4 N2 O64 Si W12'
_chemical_formula_weight         4170.04
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-05-28 deposited with the CCDC.	2021-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.730(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9948(7)
_cell_length_b                   25.5334(13)
_cell_length_c                   14.1995(7)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.20
_cell_volume                     4859.2(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0587
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49529
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.567
_diffrn_reflns_theta_min         1.969
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.426
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1380 before and 0.0662 after correction.
The Ratio of minimum to maximum transmission is 0.5656.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.850
_exptl_crystal_description       block
_exptl_crystal_F_000             3836
_exptl_crystal_size_max          0.292
_exptl_crystal_size_mid          0.266
_exptl_crystal_size_min          0.263
_refine_diff_density_max         1.617
_refine_diff_density_min         -1.505
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         11169
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0134P)^2^+44.2829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8168
_reflns_number_total             11169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01203g2.cif
_cod_data_source_block           2CH3CN-4Crown@SiW12
_cod_depositor_comments
'Adding full bibliography for 7243819--7243820.cif.'
_cod_database_code               7243820
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C25
 1.15 with sigma of 0.01
 C25-C26
 1.5 with sigma of 0.01
3. Others
 Fixed Sof: W6(0.33333) W6'(0.33333) W6''(0.33333) O19(0.5) O19'(0.5) O20(0.5)
 O20'(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,
 H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C1(H1A,H1B), C2(H2A,H2B),
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
4.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C)
;
_shelx_res_checksum              11026
_shelx_hkl_checksum              24756
_olex2_submission_special_instructions 'No special instructions were received'