Enclosing classical polyoxometallates in silver nanoclusters.
Wang, Zhi; Sun, Yi-Ming; Qu, Qing-Ping; Liang, Yu-Xin; Wang, Xing-Po; Liu, Qing-Yun; Kurmoo, Mohamedally; Su, Hai-Feng; Tung, Chen-Ho; Sun, Di; Nanoscale 11 (2019) 10927–10931; doi:10.1039/c9nr04045e

data_1552762
_publ_section_title
;
 Enclosing classical polyoxometallates in silver nanoclusters.
;
_journal_issue                   22
_journal_name_full               Nanoscale
_journal_page_first              10927
_journal_page_last               10931
_journal_paper_doi               10.1039/c9nr04045e
_journal_volume                  11
_journal_year                    2019
_chemical_formula_moiety
'0.5(C262 H370 Ag92 O146 S74 V20), C6 H5 O3 S'
_chemical_formula_sum            'C137 H190 Ag46 O76 S38 V10'
_chemical_formula_weight         9742.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-03-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-03-04 deposited with the CCDC.	2019-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.5766(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.7510(15)
_cell_length_b                   30.6808(17)
_cell_length_c                   19.5302(11)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.050
_cell_measurement_theta_min      2.222
_cell_volume                     12391.3(12)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37341
_diffrn_reflns_point_group_measured_fraction_full 0.783
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.857
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.283
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0628 before and 0.0388 after correction.
The Ratio of minimum to maximum transmission is 0.8535.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.611
_exptl_crystal_description       block
_exptl_crystal_F_000             9240
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         4.890
_refine_diff_density_min         -1.408
_refine_diff_density_rms         0.221
_refine_ls_abs_structure_details
;
 Flack x determined using 5563 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.378(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1182
_refine_ls_number_reflns         17925
_refine_ls_number_restraints     375
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.080
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1034P)^2^+209.6466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1593
_refine_ls_wR_factor_ref         0.1672
_reflns_Friedel_coverage         0.609
_reflns_Friedel_fraction_full    0.594
_reflns_Friedel_fraction_max     0.610
_reflns_number_gt                16009
_reflns_number_total             17925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nr04045e2.cif
_cod_data_source_block           SD_Ag46
_cod_database_code               1552762
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O21-S20
 1.45 with sigma of 0.05
 O29-O28
 2.35 with sigma of 0.01
 C13-O36
 1.25 with sigma of 0.01
 C13-O35
 1.25 with sigma of 0.01
 C12-C11
 1.55 with sigma of 0.01
 C9-C10
 1.55 with sigma of 0.01
 S17-C39
 1.75 with sigma of 0.01
 C53-O21
 2.5 with sigma of 0.01
 C58-S20
 2.5 with sigma of 0.01
 C8-C7
 1.55 with sigma of 0.01
 C26-C27
 1.55 with sigma of 0.01
 C26-S11
 2.75 with sigma of 0.01
 C46-C45
 1.55 with sigma of 0.01
 C31-C32
 1.39 with sigma of 0.01
 C29-C30
 1.39 with sigma of 0.01
 C30-C31
 1.39 with sigma of 0.01
 C29-C34
 1.39 with sigma of 0.01
 C66-C65
 1.55 with sigma of 0.01
 O40A-S1A
 1.45 with sigma of 0.01
 S1A-O41A
 1.45 with sigma of 0.01
 O40A-O41A
 2.35 with sigma of 0.01
 O40A-O42A
 2.35 with sigma of 0.01
 O42A-O41A
 2.35 with sigma of 0.01
 O40A-C77
 2.75 with sigma of 0.01
3. Restrained planarity
 C40, C39, C44, C43, C42, C41, S17
 with sigma of 0.01
 C29, C30, C31, C32, C34, C33
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O19 \\sim O20 \\sim O21 \\sim S20: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008
C52 \\sim C51 \\sim C50 \\sim C49 \\sim C48 \\sim C47 \\sim O27 \\sim O28 \\sim
O29 \\sim S21: within 1.7A with sigma of 0.002 and sigma for terminal atoms of
0.004
C13 \\sim O35 \\sim O36: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
C11 \\sim C12 \\sim S2: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
C22 \\sim C23: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C16 \\sim O33 \\sim O34 \\sim
S15: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.08
C40 \\sim C39 \\sim C44 \\sim C43 \\sim C42 \\sim C41 \\sim O37 \\sim O38 \\sim
O39 \\sim S17: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.08
C37 \\sim C38: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C53 \\sim C58 \\sim C57 \\sim C56 \\sim C55 \\sim C54 \\sim O19 \\sim O20 \\sim
O21 \\sim S20: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.08
C1 \\sim C6 \\sim C5 \\sim C4 \\sim C3 \\sim C2: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.08
C26 \\sim C27 \\sim S11: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
O40A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.08
O40A \\sim O41A \\sim O42A \\sim S1A: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.08
O40A \\sim O41A \\sim O42A \\sim S1A \\sim C79 \\sim C78 \\sim C77 \\sim C81
\\sim C80 \\sim C82: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.08
C67 \\sim C68: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.08
C62 \\sim C63 \\sim C64 \\sim C59 \\sim C60 \\sim C61: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C29 \\sim C30 \\sim C31 \\sim C32 \\sim C34 \\sim C33 \\sim O30 \\sim O31 \\sim
O32 \\sim S16: within 1.7A with sigma of 0.002 and sigma for terminal atoms of
0.008
C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim O24 \\sim O25 \\sim
O26 \\sim S19: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.08
C14 \\sim C15 \\sim S14: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
Uanis(O14) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.02
Uanis(C67) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.2
5. Others
 Fixed Sof: Ag1(0.75) Ag1A(0.25) C6(0.5) H6(0.5) C5(0.5) C4(0.5) H4(0.5)
 C3(0.5) H3(0.5) C2(0.5) H2(0.5) H7A(0.5) H7B(0.5) C8(0.5) H8A(0.5) H8B(0.5)
 H8C(0.5) C17(0.5) H17(0.5) C18(0.5) H18(0.5) C19(0.5) H19(0.5) C20(0.5)
 H20(0.5) C21(0.5) H21(0.5) C16(0.5) H22A(0.5) H22B(0.5) C23(0.5) H23A(0.5)
 H23B(0.5) H23C(0.5) H68A(0.5) H68B(0.5) H68C(0.5) C62(0.5) H62(0.5) C63(0.5)
 H63(0.5) C64(0.5) H64(0.5) C59(0.5) C60(0.5) H60(0.5) C61(0.5) H61(0.5)
6.a Riding coordinates:
 C6(H6), C5(H5), C4(H4), C2(H2), C7(H7A,H7B), C9(H9A,H9B,H9C), C15(H15A,H15B,
 H15C), C22(H22A,H22B), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C37(H37A,H37B,
 H37C), C67(H67)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B), C24(H24A,H24B), C27(H27A,
 H27B), C36(H36A,H36B), C38(H38A,H38B), C45(H45A,H45B), C66(H66A,H66B),
 C69(H69A,H69B)
6.c Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C46(H46A,H46B,H46C), C68(H68A,H68B,H68C)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C40(H40), C44(H44), C43(H43), C42(H42), C41(H41),
  C51(H51), C50(H50), C49(H49), C48(H48), C47(H47), C58(H58), C57(H57),
 C56(H56), C55(H55), C54(H54), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76),
  C62(H62), C63(H63), C64(H64), C60(H60), C61(H61), C79(H79), C78(H78),
 C81(H81), C80(H80), C82(H82)
6.e Fitted hexagon refined as free rotating group:
 C1(C6,C5,C4,C3,C2), C17(C18,C19,C20,C21,C16), C40(C39,C44,C43,C42,C41),
 C52(C51,C50,C49,C48,C47), C53(C58,C57,C56,C55,C54), C71(C72,C73,C74,C75,C76),
 C62(C63,C64,C59,C60,C61), C79(C78,C77,C81,C80,C82)
6.f Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C23(H23A,H23B,H23C), C35(H35A,H35B,H35C), C70(H70A,H70B,
 H70C), C65(H65A,H65B,H65C)
;
_shelx_res_checksum              75712
_shelx_fab_checksum              38335
_olex2_submission_special_instructions 'No special instructions were received'