Keggin-type polyoxometalate-containing metal‒organic hybrids as friction materials for triboelectric nanogenerators
Zhang, Ying-Ying; Hu, Mingjun; Shao, Zhichao; Huang, Chao; Qin, Qi; Mi, Liwei; CrystEngComm 23 (2021) 5184–5189; doi:10.1039/D1CE00332A

data_7242570
_publ_section_title
;
 Keggin-type polyoxometalate-containing metal--organic hybrids as friction
 materials for triboelectric nanogenerators
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              5184
_journal_page_last               5189
_journal_paper_doi               10.1039/D1CE00332A
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C36 H32 Cu N12 O42 W12 Zn'
_chemical_formula_sum            'C36 H25 Cu N12 O42 W12 Zn'
_chemical_formula_weight         3632.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-12-04
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-12-08 deposited with the CCDC.	2021-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.738(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.296(6)
_cell_length_b                   15.241(6)
_cell_length_c                   16.158(7)
_cell_measurement_reflns_used    8678
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.48
_cell_volume                     3470(3)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0532
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            54164
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.477
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.534
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.7961
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.477
_exptl_crystal_description       block
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.391
_refine_diff_density_min         -2.860
_refine_diff_density_rms         0.233
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         12199
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0366
_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^)+79.7720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.990
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                11379
_reflns_number_total             12199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00332a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7242569--7242570.cif.'
_cod_original_cell_volume        3470(2)
_cod_database_code               7242570
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53(2)
 0.47(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 Cu0E-H33A \\sim Cu0E-H33B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C10 \\sim C8 \\sim C31 \\sim C19 \\sim N12 \\sim C29: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C11 \\sim N7 \\sim C24 \\sim C22 \\sim C2 \\sim C9: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C35 \\sim C5 \\sim C12 \\sim C33 \\sim C7: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
N10 \\sim C25 \\sim C13 \\sim C23 \\sim C27 \\sim C28: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C4 \\sim N3 \\sim C16 \\sim N4 \\sim N9 \\sim C3: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
O8 \\sim W4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O27 \\sim W8: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C1 \\sim C32 \\sim C36 \\sim N11 \\sim C15 \\sim C34: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
5.a Free rotating group:
 O33(H33A,H33B)
5.b Rotating group:
 O31(H31A,H31B)
5.c Aromatic/amide H refined with riding coordinates:
 N8(H8), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13), N10(H10A),
 C15(H15), C17(H17), N11(H11A), C19(H19), N12(H12), C21(H21), C22(H22),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
5.d Fitted hexagon refined as free rotating group:
 N2(C14,N1,C6,N6,C20), C16(N4,C3,N9,C4,N3)
;
_shelx_res_checksum              75557
_shelx_fab_checksum              97342
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'