Development of non-closed silver clusters by transition-metal-coordination-cluster substituted polyoxometalate templates.
Ge, Rui; Cai, Ping-Wei; Sun, Cai; Sun, Yan-Qiong; Li, Xin-Xiong; Zheng, Shou-Tian; Chemical science 15 (2024) 12543–12549; doi:10.1039/d4sc01502a

data_1571993
_publ_section_title
;
 Development of non-closed silver clusters by
 transition-metal-coordination-cluster substituted polyoxometalate
 templates.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              12543
_journal_page_last               12549
_journal_paper_doi               10.1039/d4sc01502a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety
'C112 H169 Ag35.166 Co5 O80 Si2 W20, 0.834(Ag), 6[CH3CN], 1[H2O], 1[1]'
_chemical_formula_sum            'C124 H189 Ag36 Co5 N6 O81 Si2 W20'
_chemical_formula_weight         10970.95
_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   geom
_audit_creation_date             2024-06-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-06-19 deposited with the CCDC.	2024-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                96.159(2)
_cell_angle_beta                 92.500(2)
_cell_angle_gamma                105.258(2)
_cell_formula_units_Z            2
_cell_length_a                   20.3864(15)
_cell_length_b                   21.2135(17)
_cell_length_c                   31.864(2)
_cell_measurement_reflns_used    9550
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.368
_cell_volume                     13180.5(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'sealed tube'
_diffrn_measurement_method       'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            406681
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.164
_diffrn_reflns_theta_max         25.164
_diffrn_reflns_theta_min         1.994
_exptl_absorpt_coefficient_mu    11.659
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.764
_exptl_crystal_description       plate
_exptl_crystal_F_000             9916
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         5.328
_refine_diff_density_min         -3.505
_refine_diff_density_rms         0.289
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2327
_refine_ls_number_reflns         45516
_refine_ls_number_restraints     4212
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0916P)^2^+258.1277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1692
_refine_ls_wR_factor_ref         0.1809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                35237
_reflns_number_total             45516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01502a2.cif
_cod_data_source_block           ag36-co_sq
_cod_depositor_comments
'Adding full bibliography for 1571992--1571998.cif.'
_cod_original_cell_volume        13180.3(17)
_cod_database_code               1571993
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.274
_shelx_estimated_absorpt_t_min   0.228
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C73-C76
 1.54 with sigma of 0.01
 C73-C75
 1.54 with sigma of 0.01
 C73-C74
 1.54 with sigma of 0.01
 C79-C81
 1.54 with sigma of 0.01
 C79-C82
 1.54 with sigma of 0.01
 C79-C80
 1.54 with sigma of 0.01
 C91-C93
 1.54 with sigma of 0.01
 C91-C94
 1.54 with sigma of 0.01
 C91-C92
 1.54 with sigma of 0.01
 C55-C57
 1.54 with sigma of 0.01
 C55-C58
 1.54 with sigma of 0.01
 C7-C10
 1.54 with sigma of 0.01
 C7-C8
 1.54 with sigma of 0.01
 C103-C104
 1.54 with sigma of 0.01
 C103-C106
 1.54 with sigma of 0.01
 C103-C105
 1.54 with sigma of 0.01
 C19-C22
 1.54 with sigma of 0.01
 C19-C21
 1.54 with sigma of 0.01
 C19-C20
 1.54 with sigma of 0.01
 C13-C14
 1.54 with sigma of 0.01
 C13-C16
 1.54 with sigma of 0.01
 C13-C15
 1.54 with sigma of 0.01
 C109-C111
 1.54 with sigma of 0.01
 C109-C112
 1.54 with sigma of 0.01
 C109-C110
 1.54 with sigma of 0.01
 C43-C44
 1.54 with sigma of 0.01
 C43-C45
 1.54 with sigma of 0.01
 C43-C46
 1.54 with sigma of 0.01
 C49-C50
 1.54 with sigma of 0.01
 C49-C52
 1.54 with sigma of 0.01
 C49-C51
 1.54 with sigma of 0.01
 C67-C70
 1.54 with sigma of 0.01
 C67-C68
 1.54 with sigma of 0.01
 C31-C33
 1.54 with sigma of 0.01
 C31-C34
 1.54 with sigma of 0.01
 C31-C32
 1.54 with sigma of 0.01
 C25-C28
 1.54 with sigma of 0.01
 C25-C27
 1.54 with sigma of 0.01
 C25-C26
 1.54 with sigma of 0.01
 C97-C98
 1.54 with sigma of 0.01
 C97-C100
 1.54 with sigma of 0.01
 C97-C99
 1.54 with sigma of 0.01
 C61-C62
 1.54 with sigma of 0.01
 C61-C63
 1.54 with sigma of 0.01
 C61-C64
 1.54 with sigma of 0.01
 C59-C60
 1.2 with sigma of 0.01
 C76-C75
 2.53 with sigma of 0.01
 C76-C74
 2.53 with sigma of 0.01
 C75-C74
 2.53 with sigma of 0.01
 C82-C81
 2.53 with sigma of 0.01
 C81-C80
 2.53 with sigma of 0.01
 C82-C80
 2.53 with sigma of 0.01
 C93-C94
 2.53 with sigma of 0.01
 C93-C92
 2.53 with sigma of 0.01
 C94-C92
 2.53 with sigma of 0.01
 C57-C58
 2.53 with sigma of 0.01
 C10-C8
 2.53 with sigma of 0.01
 C104-C106
 2.53 with sigma of 0.01
 C104-C105
 2.53 with sigma of 0.01
 C105-C106
 2.53 with sigma of 0.01
 C22-C21
 2.53 with sigma of 0.01
 C22-C20
 2.53 with sigma of 0.01
 C21-C20
 2.53 with sigma of 0.01
 C14-C16
 2.53 with sigma of 0.01
 C14-C15
 2.53 with sigma of 0.01
 C16-C15
 2.53 with sigma of 0.01
 C111-C112
 2.53 with sigma of 0.01
 C111-C110
 2.53 with sigma of 0.01
 C112-C110
 2.53 with sigma of 0.01
 C44-C45
 2.53 with sigma of 0.01
 C44-C46
 2.53 with sigma of 0.01
 C46-C45
 2.53 with sigma of 0.01
 C50-C52
 2.53 with sigma of 0.01
 C50-C51
 2.53 with sigma of 0.01
 C52-C51
 2.53 with sigma of 0.01
 C70-C68
 2.53 with sigma of 0.01
 C98-C100
 2.53 with sigma of 0.01
 C100-C99
 2.53 with sigma of 0.01
 C98-C99
 2.53 with sigma of 0.01
 C28-C27
 2.53 with sigma of 0.01
 C26-C27
 2.53 with sigma of 0.01
 C28-C26
 2.53 with sigma of 0.01
 C33-C34
 2.53 with sigma of 0.01
 C33-C32
 2.53 with sigma of 0.01
 C34-C32
 2.53 with sigma of 0.01
 C62-C63
 2.53 with sigma of 0.01
 C87-C86
 2.53 with sigma of 0.01
 C87-C88
 2.53 with sigma of 0.01
 C86-C88
 2.53 with sigma of 0.01
 H63C-H64B
 2.1 with sigma of 0.01
 C11-C12
 1.3 with sigma of 0.01
 C29-C30
 1.3 with sigma of 0.01
 C47-C48
 1.3 with sigma of 0.01
 C89-C90
 1.3 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C71 \\sim C72 \\sim C73 \\sim C76 \\sim C75 \\sim C74 \\sim C77 \\sim C78 \\sim
C79 \\sim C81 \\sim C82 \\sim C80 \\sim C89 \\sim C90 \\sim C91 \\sim C93 \\sim
C94 \\sim C92 \\sim C53 \\sim C54 \\sim C55 \\sim C57 \\sim C58 \\sim C5 \\sim
C6 \\sim C7 \\sim C10 \\sim C8 \\sim C101 \\sim C102 \\sim C103 \\sim C104
\\sim C106 \\sim C105 \\sim C83 \\sim C84 \\sim C85 \\sim C17 \\sim C18 \\sim
C19 \\sim C22 \\sim C21 \\sim C20 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim
C16 \\sim C15 \\sim C107 \\sim C108 \\sim C109 \\sim C111 \\sim C112 \\sim C110
\\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C35 \\sim C36
\\sim C37 \\sim C38 \\sim C40 \\sim C39 \\sim C47 \\sim C48 \\sim C49 \\sim C50
\\sim C52 \\sim C51 \\sim C65 \\sim C66 \\sim C67 \\sim C70 \\sim C68 \\sim C30
\\sim C31 \\sim C33 \\sim C34 \\sim C32 \\sim C23 \\sim C24 \\sim C25 \\sim C28
\\sim C27 \\sim C26 \\sim C95 \\sim C96 \\sim C97 \\sim C98 \\sim C100 \\sim
C99 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C2 \\sim C1 \\sim
C3 \\sim C4 \\sim C29 \\sim C87 \\sim C86 \\sim C88 \\sim C69 \\sim C64 \\sim
C56 \\sim C9: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(C29) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C109)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Ag1A)=1-FVAR(1)
 Sof(Ag14)=FVAR(1)
 Sof(Ag2A)=1-FVAR(2)
 Sof(Ag13)=FVAR(2)
 Fixed Sof: W1(0.9) W4(0.9) W4A(0.1) W1A(0.1)
6.a Ternary CH refined with riding coordinates:
 O16(H16)
6.b Me refined with riding coordinates:
 C76(H76A,H76B,H76C), C75(H75A,H75B,H75C), C74(H74A,H74B,H74C), C81(H81A,H81B,
 H81C), C82(H82A,H82B,H82C), C80(H80A,H80B,H80C), C93(H93A,H93B,H93C), C94(H94A,
 H94B,H94C), C92(H92A,H92B,H92C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C),
 C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C104(H10D,H10E,H10F), C106(H10G,H10H,
 H10I), C105(H10J,H10K,H10L), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C),
 C20(H20A,H20B,H20C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C15(H15A,H15B,
 H15C), C111(H11A,H11B,H11C), C112(H11D,H11E,H11F), C110(H11G,H11H,H11I),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C38(H38A,H38B,
 H38C), C40(H40A,H40B,H40C), C39(H39A,H39B,H39C), C50(H50A,H50B,H50C), C52(H52A,
 H52B,H52C), C51(H51A,H51B,H51C), C70(H70A,H70B,H70C), C68(H68A,H68B,H68C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C32(H32A,H32B,H32C), C28(H28A,H28B,
 H28C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C98(H98A,H98B,H98C),
 C100(H10M,H10N,H10O), C99(H99A,H99B,H99C), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C87(H87A,H87B,H87C), C86(H86A,H86B,
 H86C), C88(H88A,H88B,H88C), C64(H64A,H64B,H64C)
6.c Idealised Me refined as rotating group:
 C69(H69A,H69B,H69C), C56(H56A,H56B,H56C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              18308
_shelx_hkl_checksum              62449
_shelx_fab_checksum              25412
_platon_squeeze_special_details
;
A solvent mask was calculated and 274 electrons were 
found in a volume of 4110\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
6[CH3CN], 1[H2O], 1[1] per Asymmetric Unit 
which account for 284 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'