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_1571992
_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         'C134 H204 Ag38 N5 O55 Si W9 Zn4, C2 H3 N'
_chemical_formula_sum            'C216 H367 Ag38 N46 O75 Si W9 Zn4'
_chemical_formula_weight         10851.81
_chemical_name_systematic        Ag38-Zn
_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             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                104.882(4)
_cell_angle_beta                 94.518(4)
_cell_angle_gamma                92.303(4)
_cell_formula_units_Z            2
_cell_length_a                   21.911(3)
_cell_length_b                   23.503(3)
_cell_length_c                   30.979(4)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.110
_cell_measurement_theta_min      2.329
_cell_volume                     15340(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            599652
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.820
_exptl_absorpt_coefficient_mu    6.103
_exptl_absorpt_correction_T_max  0.2586
_exptl_absorpt_correction_T_min  0.1704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.349
_exptl_crystal_description       block
_exptl_crystal_F_000             10342
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         5.426
_refine_diff_density_min         -1.925
_refine_diff_density_rms         0.251
_refine_ls_extinction_coef       0.000093(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2238
_refine_ls_number_reflns         52059
_refine_ls_number_restraints     6486
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0797
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1087P)^2^+367.6919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2019
_refine_ls_wR_factor_ref         0.2262
_reflns_Friedel_coverage         0.000
_reflns_number_gt                38709
_reflns_number_total             52059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01502a2.cif
_cod_data_source_block           ag38-zn_sq
_cod_depositor_comments
'Adding full bibliography for 1571992--1571998.cif.'
_cod_database_code               1571992
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.361
_shelx_estimated_absorpt_t_min   0.311
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, H44 of O44
 At 1.2 times of:
  H45 of O45, H43 of O43
2. Restrained distances
 C27-C28
 1.54 with sigma of 0.01
 C27-C29
 1.54 with sigma of 0.01
 C27-C30
 1.54 with sigma of 0.01
 C9-C11
 1.54 with sigma of 0.01
 C9-C10
 1.54 with sigma of 0.01
 C9-C12
 1.54 with sigma of 0.01
 C123-C125
 1.54 with sigma of 0.01
 C123-C126
 1.54 with sigma of 0.01
 C123-C124
 1.54 with sigma of 0.01
 C21-C20
 1.54 with sigma of 0.01
 C21-C24
 1.54 with sigma of 0.01
 C21-C22
 1.54 with sigma of 0.01
 C21-C23
 1.54 with sigma of 0.01
 C117-C118
 1.54 with sigma of 0.01
 C117-C119
 1.54 with sigma of 0.01
 C28-C29
 2.53 with sigma of 0.01
 C28-C30
 2.53 with sigma of 0.01
 C29-C30
 2.53 with sigma of 0.01
 C11-C10
 2.53 with sigma of 0.01
 C11-C12
 2.53 with sigma of 0.01
 C12-C10
 2.53 with sigma of 0.01
 C136-C135
 1.54 with sigma of 0.01
 C49-C50
 1.54 with sigma of 0.01
 C7-C8
 1.3 with sigma of 0.01
 C69-C72
 1.54 with sigma of 0.01
 C19-C20
 1.3 with sigma of 0.01
 C25-C26
 1.3 with sigma of 0.01
 C85-C86
 1.3 with sigma of 0.01
 C103-C104
 1.3 with sigma of 0.01
 C121-C122
 1.3 with sigma of 0.01
 H13F-H84B
 2.45 with sigma of 0.01
 C81-C84
 1.54 with sigma of 0.01
3. Rigid bond restraints
 Ag28, C79
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 All non-hydrogen atoms
 with sigma for 1-2 distances of 1.5 and sigma for 1-3 distances of 1.5
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97
\\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104
\\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim C111
\\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim C117 \\sim C118
\\sim C119 \\sim C120 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125
\\sim C126 \\sim C127 \\sim C128 \\sim C129 \\sim C130 \\sim C131 \\sim C132
\\sim C133 \\sim C134 \\sim C135 \\sim C136: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3.8A
Ag38 \\sim N5: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C27) \\sim
Ueq, Uanis(C33) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C69) \\sim Ueq,
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C85) \\sim Ueq,
Uanis(C86) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C121) \\sim Ueq,
Uanis(C122) \\sim Ueq, Uanis(C127) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N5) \\sim Ueq, Uanis(Ag6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Ag6) = Uanis(C7)
5. 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
6.a Riding coordinates:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C70(H70A,
 H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C76(H76A,H76B,H76C),
 C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C82(H82A,H82B,H82C), C83(H83A,H83B,
 H83C), C84(H84A,H84B,H84C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C90(H90A,
 H90B,H90C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C100(H10D,H10E,H10F),
 C101(H10G,H10H,H10I), C102(H10J,H10K,H10L), C106(H10M,H10N,H10O), C107(H10P,
 H10Q,H10R), C108(H10S,H10T,H10U), C112(H11D,H11E,H11F), C113(H11G,H11H,H11I),
 C114(H11J,H11K,H11L), C118(H11M,H11N,H11O), C119(H11P,H11Q,H11R), C120(H12D,
 H12E,H12F), C124(H12G,H12H,H12I), C125(H12J,H12K,H12L), C126(H12M,H12N,H12O),
 C128(H12P,H12Q,H12R), C130(H13A,H13B,H13C), C132(H13D,H13E,H13F), C134(H13G,
 H13H,H13I), O44(H44)
6.b Ternary CH refined with riding coordinates:
 O43(H43), O45(H45)
6.c Me refined with riding coordinates:
 C94(H94A,H94B,H94C)
6.d Idealised Me refined as rotating group:
 C135(H13J,H13K,H13L)
;
_shelx_res_checksum              15010
_shelx_hkl_checksum              48993
_shelx_fab_checksum              38310
_platon_squeeze_special_details
;
A solvent mask was calculated and 2183 electrons were 
found in a volume of 5987\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
40[CH3CN], 20[H2O], 1[1] per Asymmetric Unit 
which account for 2160 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'