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_1571995
_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
'C106 H162 Ag36 Ni5 O80 Si2 W20, 20[CH3CN], 88[H2O]'
_chemical_formula_sum            'C146 H398 Ag36 N20 Ni5 O168 Si2 W20'
_chemical_formula_weight         13032.87
_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                91.397(4)
_cell_angle_beta                 95.125(4)
_cell_angle_gamma                110.459(4)
_cell_formula_units_Z            2
_cell_length_a                   20.495(3)
_cell_length_b                   23.774(3)
_cell_length_c                   31.972(4)
_cell_measurement_reflns_used    9598
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.956
_cell_measurement_theta_min      2.326
_cell_volume                     14511(3)
_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 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker duo apex2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            471758
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.083
_diffrn_reflns_theta_max         25.083
_diffrn_reflns_theta_min         1.970
_exptl_absorpt_coefficient_mu    10.675
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.2865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.983
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             12196
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         4.402
_refine_diff_density_min         -5.533
_refine_diff_density_rms         0.411
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2295
_refine_ls_number_reflns         49547
_refine_ls_number_restraints     5540
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0984
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1377P)^2^+951.1781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2608
_refine_ls_wR_factor_ref         0.2765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                40259
_reflns_number_total             49547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01502a2.cif
_cod_data_source_block           ag36-ni_sq_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1571992--1571998.cif.
;
_cod_original_cell_volume        14512(3)
_cod_database_code               1571995
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C31-C32
 1.3 with sigma of 0.01
 C33-C32
 1.54 with sigma of 0.01
 C35-C33
 1.54 with sigma of 0.01
 C43-C44
 1.3 with sigma of 0.01
 C45-C44
 1.54 with sigma of 0.01
 C45-C48
 1.54 with sigma of 0.01
 C45-C47
 1.54 with sigma of 0.01
 C45-C46
 1.54 with sigma of 0.01
 C46-C47
 2.53 with sigma of 0.01
 C46-C48
 2.53 with sigma of 0.01
 C47-C48
 2.53 with sigma of 0.01
 C44-C48
 2.7 with sigma of 0.01
 C81-C84
 1.54 with sigma of 0.01
 C81-C82
 1.54 with sigma of 0.01
 C81-C83
 1.54 with sigma of 0.01
 C8-C7
 1.3 with sigma of 0.01
 C8-C9
 1.54 with sigma of 0.01
 C9-C12
 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
 C12-C11
 2.53 with sigma of 0.01
 C12-C10
 2.53 with sigma of 0.01
 C11-C10
 2.53 with sigma of 0.01
 C93-C96
 1.54 with sigma of 0.01
 C93-C95
 1.54 with sigma of 0.01
 C93-C94
 1.54 with sigma of 0.01
 C96-C95
 2.53 with sigma of 0.01
 C96-C94
 2.53 with sigma of 0.01
 C95-C94
 2.53 with sigma of 0.01
 C2-C3
 1.54 with sigma of 0.01
 C57-C58
 1.54 with sigma of 0.01
 C57-C59
 1.54 with sigma of 0.01
 C57-C60
 1.54 with sigma of 0.01
 C58-C59
 2.53 with sigma of 0.01
 C58-C60
 2.53 with sigma of 0.01
 C59-C60
 2.53 with sigma of 0.01
 C33-C34
 1.54 with sigma of 0.01
 C33-C35
 1.54 with sigma of 0.01
 C33-C36
 1.54 with sigma of 0.01
 C34-C35
 2.53 with sigma of 0.01
 C34-C36
 2.53 with sigma of 0.01
 C35-C36
 2.53 with sigma of 0.01
 C50-C51
 1.54 with sigma of 0.01
 C51-C54
 1.54 with sigma of 0.01
 C51-C52
 1.54 with sigma of 0.01
 C51-C53
 1.54 with sigma of 0.01
 C54-C52
 2.53 with sigma of 0.01
 C54-C53
 2.53 with sigma of 0.01
 C52-C53
 2.53 with sigma of 0.01
 C52-C50
 2.7 with sigma of 0.01
 C39-C41
 1.54 with sigma of 0.01
 C39-C40
 1.54 with sigma of 0.01
 C39-C42
 1.54 with sigma of 0.01
 C41-C40
 2.53 with sigma of 0.01
 C40-C42
 2.53 with sigma of 0.01
 C41-C42
 2.53 with sigma of 0.01
 C37-C38
 1.3 with sigma of 0.01
 C38-C39
 1.54 with sigma of 0.01
 C3-C6
 1.54 with sigma of 0.01
 C3-C4
 1.54 with sigma of 0.01
 C3-C5
 1.54 with sigma of 0.01
 C6-C4
 2.53 with sigma of 0.01
 C6-C5
 2.53 with sigma of 0.01
 C4-C5
 2.53 with sigma of 0.01
 C27-C26
 1.54 with sigma of 0.01
 C27-C30
 1.54 with sigma of 0.01
 C27-C28
 1.54 with sigma of 0.01
 C27-C29
 1.54 with sigma of 0.01
 C25-C26
 1.3 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
 C19-C20
 1.3 with sigma of 0.01
 C20-C21
 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
 C21-C24
 1.54 with sigma of 0.01
 C24-C23
 2.53 with sigma of 0.01
 C24-C22
 2.53 with sigma of 0.01
 C22-C23
 2.53 with sigma of 0.01
 C63-C62
 1.54 with sigma of 0.01
 C61-C62
 1.3 with sigma of 0.01
 C63-C65
 1.54 with sigma of 0.01
 C63-C64
 1.54 with sigma of 0.01
 C63-C66
 1.54 with sigma of 0.01
 C65-C64
 2.53 with sigma of 0.01
 C65-C66
 2.53 with sigma of 0.01
 C64-C66
 2.53 with sigma of 0.01
 C67-C68
 1.3 with sigma of 0.01
 C68-C69
 1.54 with sigma of 0.01
 C69-C70
 1.54 with sigma of 0.01
 C69-C71
 1.54 with sigma of 0.01
 C69-C72
 1.54 with sigma of 0.01
 C70-C71
 2.53 with sigma of 0.01
 C71-C72
 2.53 with sigma of 0.01
 C70-C72
 2.53 with sigma of 0.01
 C85-C86
 1.3 with sigma of 0.01
 C86-C87
 1.54 with sigma of 0.01
 C87-C88
 1.54 with sigma of 0.01
 C87-C89
 1.54 with sigma of 0.01
 C87-C90
 1.54 with sigma of 0.01
 C88-C89
 2.53 with sigma of 0.01
 C88-C90
 2.53 with sigma of 0.01
 C89-C90
 2.53 with sigma of 0.01
 C13-C14
 1.3 with sigma of 0.01
 C14-C15
 1.54 with sigma of 0.01
 C15-C16
 1.54 with sigma of 0.01
 C16-C15
 1.54 with sigma of 0.01
 C17-C15
 1.54 with sigma of 0.01
 C18-C15
 1.54 with sigma of 0.01
 C16-C17
 2.53 with sigma of 0.01
 C17-C18
 2.53 with sigma of 0.01
 C16-C18
 2.53 with sigma of 0.01
 C79-C80
 1.3 with sigma of 0.01
 C1-C2
 1.3 with sigma of 0.01
3. Rigid bond restraints
 Ag1, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Ag8A, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Ag15, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Ag16, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Ag6A, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C8 \\sim C7 \\sim C56 \\sim C43 \\sim C80 \\sim C55 \\sim C60 \\sim C31 \\sim
C44 \\sim C35 \\sim C12 \\sim C9 \\sim C81 \\sim C45 \\sim C82 \\sim C79 \\sim
C58 \\sim C57 \\sim C34 \\sim C10 \\sim C59 \\sim C83 \\sim C98 \\sim C1 \\sim
C49 \\sim C13 \\sim C92 \\sim C97 \\sim C86 \\sim C74 \\sim C85 \\sim C101
\\sim C73 \\sim C62 \\sim C37 \\sim C102 \\sim C2 \\sim C75 \\sim C93 \\sim C76
\\sim C15 \\sim C99 \\sim C94 \\sim C87 \\sim C91 \\sim C38 \\sim C18 \\sim C50
\\sim C6 \\sim C61 \\sim C88 \\sim C16 \\sim C14 \\sim C90 \\sim C39 \\sim C89
\\sim C5 \\sim C77 \\sim C54 \\sim C4 \\sim C63 \\sim C3 \\sim C66 \\sim C78
\\sim C100 \\sim C36 \\sim C32 \\sim C33 \\sim C67 \\sim C71 \\sim C72 \\sim
C69 \\sim C68 \\sim C52 \\sim C46 \\sim C47 \\sim C48 \\sim C17 \\sim C53 \\sim
C103 \\sim C84 \\sim C64 \\sim C105 \\sim C104 \\sim C106 \\sim C11 \\sim C70
\\sim C40 \\sim C96 \\sim C95 \\sim C51 \\sim C41 \\sim C42 \\sim C25 \\sim C26
\\sim C30 \\sim C27 \\sim C29 \\sim C28 \\sim C19 \\sim C21 \\sim C20 \\sim C23
\\sim C22 \\sim C24 \\sim C65: within 4A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 4A
Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C64) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C51) \\sim Ueq,
Uanis(C58) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Ag14) = Uanis(C1)
Uanis(C1) = Uanis(C6) = Uanis(C5) = Uanis(C4) = Uanis(C3)
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. Others
 Sof(Ag1A)=1-FVAR(1)
 Sof(Ag21)=FVAR(1)
 Sof(Ag2A)=1-FVAR(2)
 Sof(Ag26)=FVAR(2)
 Sof(Ag3A)=1-FVAR(3)
 Sof(Ag23)=FVAR(3)
 Sof(Ag4A)=1-FVAR(4)
 Sof(Ag29)=FVAR(4)
 Sof(Ag5A)=1-FVAR(5)
 Sof(Ag1)=FVAR(5)
 Sof(Ag6A)=1-FVAR(6)
 Sof(Ag4)=FVAR(6)
 Sof(Ag7A)=1-FVAR(7)
 Sof(Ag34)=FVAR(7)
 Sof(Ag8A)=1-FVAR(8)
 Sof(Ag5)=FVAR(8)
7.a Ternary CH refined with riding coordinates:
 O6(H6), O66(H66), O65(H65)
7.b Me refined with riding coordinates:
 C60(H60A,H60B,H60C), C35(H35A,H35B,H35C), C12(H12A,H12B,H12C), C58(H58A,H58B,
 H58C), C34(H34A,H34B,H34C), C10(H10A,H10B,H10C), C59(H59A,H59B,H59C), C83(H83A,
 H83B,H83C), C101(H10D,H10E,H10F), C102(H10G,H10H,H10I), C76(H76A,H76B,H76C),
 C94(H94A,H94B,H94C), C18(H18A,H18B,H18C), C88(H88A,H88B,H88C), C16(H16A,H16B,
 H16C), C90(H90A,H90B,H90C), C89(H89A,H89B,H89C), C77(H77A,H77B,H77C), C4(H4A,
 H4B,H4C), C66(H66A,H66B,H66C), C78(H78A,H78B,H78C), C100(H10J,H10K,H10L),
 C36(H36A,H36B,H36C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C52(H52A,H52B,
 H52C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C17(H17A,
 H17B,H17C), C53(H53A,H53B,H53C), C84(H84A,H84B,H84C), C64(H64A,H64B,H64C),
 C104(H10M,H10N,H10O), C106(H10P,H10Q,H10R), C11(H11A,H11B,H11C), C70(H70A,H70B,
 H70C), C40(H40A,H40B,H40C), C96(H96A,H96B,H96C), C95(H95A,H95B,H95C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C),
 C28(H28A,H28B,H28C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C65(H65A,H65B,H65C)
7.c Idealised Me refined as rotating group:
 C82(H82A,H82B,H82C), C6(H6A,H6B,H6C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              50500
_shelx_hkl_checksum              56420
_shelx_fab_checksum              56849
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'