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_1552760
_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         'C148 H194 Ag44 O84 S38 V10'
_chemical_formula_sum            'C148 H194 Ag44 O84 S38 V10'
_chemical_formula_weight         9790.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-10-18
_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                60.809(7)
_cell_angle_beta                 70.785(4)
_cell_angle_gamma                78.996(4)
_cell_formula_units_Z            1
_cell_length_a                   19.9658(6)
_cell_length_b                   20.2722(14)
_cell_length_c                   20.4027(12)
_cell_measurement_reflns_used    11909
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      26.9170
_cell_measurement_theta_min      3.4550
_cell_volume                     6803.0(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -26.00  29.00   1.00  120.00    --   -4.32 -99.00 -30.00   55
  2  \w    -15.00  69.00   1.00  120.00    --   -4.32  29.00  53.00   84
  3  \w    -78.00   4.00   1.00  120.00    --   -4.32 -29.00-107.00   82
  4  \w     -5.00  78.00   1.00  120.00    --    5.49  37.00-180.00   83
  5  \w    -67.00  19.00   1.00  120.00    --    5.49 -57.00-150.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0126980000
_diffrn_orient_matrix_UB_12      -0.0191645000
_diffrn_orient_matrix_UB_13      0.0413340000
_diffrn_orient_matrix_UB_21      0.0066347000
_diffrn_orient_matrix_UB_22      -0.0352139000
_diffrn_orient_matrix_UB_23      -0.0009461000
_diffrn_orient_matrix_UB_31      0.0348132000
_diffrn_orient_matrix_UB_32      -0.0018240000
_diffrn_orient_matrix_UB_33      0.0028949000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1071
_diffrn_reflns_av_unetI/netI     0.1061
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            76924
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.370
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.766
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.390
_exptl_crystal_description       block
_exptl_crystal_F_000             4660
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.277
_refine_diff_density_min         -1.816
_refine_diff_density_rms         0.303
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1457
_refine_ls_number_reflns         24752
_refine_ls_number_restraints     359
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0858
_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^)+(0.1282P)^2^+52.3725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2125
_refine_ls_wR_factor_ref         0.2387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16252
_reflns_number_total             24752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nr04045e2.cif
_cod_data_source_block           SD_Ag44a
_cod_database_code               1552760
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         CHSAg
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.753
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C4-C3
 1.55 with sigma of 0.01
 C32-C31
 1.55 with sigma of 0.01
 C6-C5A
 1.55 with sigma of 0.01
 C6-C5
 1.55 with sigma of 0.01
 C4-C3A
 1.55 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim O21 \\sim O22 \\sim
O23 \\sim S12: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C7 \\sim C8 \\sim S4: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
C25 \\sim C26 \\sim S8: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
O15 \\sim O16 \\sim O17 \\sim S17: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008
C5 \\sim C5A \\sim C6 \\sim S3: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C3 \\sim C3A \\sim C4: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
Uanis(C6) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.01
Uanis(O4) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.01
Uanis(O3) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.01
4. Others
 Sof(Ag1A)=1-FVAR(1)
 Sof(Ag1)=FVAR(1)
 Fixed Sof: C3(0.7) H3A(0.7) H3B(0.7) H3C(0.7) C3A(0.3) H3AA(0.3) H3AB(0.3)
 H3AC(0.3) H4BC(0.4) H4BD(0.4) H4AA(0.6) H4AB(0.6) C5(0.4) H5A(0.4) H5B(0.4)
 H5C(0.4) C5A(0.6) H5AA(0.6) H5AB(0.6) H5AC(0.6) H6BC(0.6) H6BD(0.6) H6AA(0.4)
 H6AB(0.4)
5.a Rotating group:
 O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4BC,H4BD), C4(H4AA,H4AB), C6(H6BC,H6BD), C6(H6AA,H6AB),
 C7(H7A,H7B), C9(H9A,H9B), C11(H11A,H11B), C26(H26A,H26B), C28(H28A,H28B),
 C29(H29A,H29B), C32(H32A,H32B)
5.c Me refined with riding coordinates:
 C3A(H3AA,H3AB,H3AC)
5.d Aromatic/amide H refined with riding coordinates:
 C14(H14), C18(H18), C17(H17), C16(H16), C15(H15), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47),
 C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
  C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C64(H64), C65(H65),
 C66(H66), C67(H67), C68(H68), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74)
5.e Fitted hexagon refined as free rotating group:
 C14(C13,C18,C17,C16,C15)
5.f Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC),
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C25(H25A,H25B,H25C),
  C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              98368
_shelx_fab_checksum              29260
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.160
_oxdiff_exptl_absorpt_empirical_full_min 0.833