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_1571996
_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
'C140 H213 Ag37 N3 O83 Si2 W20 Zn5, 2(C2 H3 N), 30[CH3CN]'
_chemical_formula_sum            'C204 H309 Ag37 N35 O83 Si2 W20 Zn5'
_chemical_formula_weight         12631.06
_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                76.713(3)
_cell_angle_beta                 81.315(2)
_cell_angle_gamma                83.548(3)
_cell_formula_units_Z            2
_cell_length_a                   21.433(2)
_cell_length_b                   25.176(2)
_cell_length_c                   27.986(2)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.256
_cell_measurement_theta_min      2.287
_cell_volume                     14481(2)
_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 0.931
_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  0.0722
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            522688
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.604
_diffrn_reflns_theta_min         1.929
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    10.828
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.3748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.897
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             11678
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         4.080
_refine_diff_density_min         -4.958
_refine_diff_density_rms         0.334
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2691
_refine_ls_number_reflns         50744
_refine_ls_number_restraints     6163
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0862
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+1153.0521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1773
_refine_ls_wR_factor_ref         0.1937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                39300
_reflns_number_total             50744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01502a2.cif
_cod_data_source_block           ag37-zn_sq_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_database_code               1571996
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.233
_shelx_estimated_absorpt_t_min   0.173
_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
 C75-C77
 1.54 with sigma of 0.01
 C75-C76
 1.54 with sigma of 0.01
 C93-C95
 1.54 with sigma of 0.01
 C69-C71
 1.54 with sigma of 0.01
 C107-C108
 2.53 with sigma of 0.01
 C123-C125
 1.54 with sigma of 0.01
 C123-C124
 1.54 with sigma of 0.01
 C123-C126
 1.54 with sigma of 0.01
 C99-C101
 1.54 with sigma of 0.01
 C125-C124
 2.53 with sigma of 0.01
 C125-C126
 2.53 with sigma of 0.01
 C124-C126
 2.53 with sigma of 0.01
 C117-C119
 1.54 with sigma of 0.01
 C89-C88
 2.53 with sigma of 0.01
 C89-C90
 2.53 with sigma of 0.01
 C88-C90
 2.53 with sigma of 0.01
 C9-C12
 1.54 with sigma of 0.01
 C9-C10
 1.54 with sigma of 0.01
 C9-C11
 1.54 with sigma of 0.01
 C12-C10
 2.53 with sigma of 0.01
 C12-C11
 2.53 with sigma of 0.01
 C10-C11
 2.53 with sigma of 0.01
 C27-C30
 1.54 with sigma of 0.01
 C27-C29
 1.54 with sigma of 0.01
 C104-C105
 1.54 with sigma of 0.01
 C100-C102
 2.53 with sigma of 0.01
 C100-C101
 2.53 with sigma of 0.01
 C102-C101
 2.53 with sigma of 0.01
 C52-C51
 1.54 with sigma of 0.01
 C51-C54
 1.54 with sigma of 0.01
 C51-C53
 1.54 with sigma of 0.01
 C27-C28
 1.54 with sigma of 0.01
 C57-C58
 1.54 with sigma of 0.01
 C26-C27
 1.54 with sigma of 0.01
 C2-C1
 1.2 with sigma of 0.01
 C2-C3
 1.54 with sigma of 0.01
 C20-C21
 1.54 with sigma of 0.01
 C22-C21
 1.54 with sigma of 0.01
 C23-C21
 1.54 with sigma of 0.01
 C24-C21
 1.54 with sigma of 0.01
 C45-C47
 1.54 with sigma of 0.01
 C55-C56
 1.3 with sigma of 0.01
 C68-C67
 1.3 with sigma of 0.01
 C98-C97
 1.3 with sigma of 0.01
 C62-C61
 1.3 with sigma of 0.01
 C79-C80
 1.3 with sigma of 0.01
 C37-C38
 1.3 with sigma of 0.01
 C103-C104
 1.3 with sigma of 0.01
 C1-Ag3A
 2.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C93 \\sim C64 \\sim C8 \\sim C71 \\sim C34 \\sim C36 \\sim C17 \\sim C55 \\sim
C11 \\sim C108 \\sim C3 \\sim C6 \\sim C98 \\sim C95 \\sim C4 \\sim C5 \\sim
C124 \\sim C56 \\sim C57 \\sim C27 \\sim C30 \\sim C51 \\sim C54 \\sim C28
\\sim C143 \\sim C144 \\sim C53 \\sim C7 \\sim C85 \\sim C129 \\sim C128 \\sim
C31 \\sim C73 \\sim C77 \\sim C25 \\sim C97 \\sim C79 \\sim C67 \\sim C127
\\sim C91 \\sim C116 \\sim C131 \\sim C32 \\sim C92 \\sim C115 \\sim C74 \\sim
C76 \\sim C33 \\sim C109 \\sim C15 \\sim C80 \\sim C75 \\sim C37 \\sim C18
\\sim C130 \\sim C38 \\sim C39 \\sim C13 \\sim C29 \\sim C9 \\sim C135 \\sim
C70 \\sim C43 \\sim C65 \\sim C90 \\sim C45 \\sim C19 \\sim C107 \\sim C14
\\sim C62 \\sim C133 \\sim C78 \\sim C81 \\sim C94 \\sim C44 \\sim C132 \\sim
C136 \\sim C16 \\sim C49 \\sim C134 \\sim C59 \\sim C122 \\sim C61 \\sim C86
\\sim C26 \\sim C111 \\sim C117 \\sim C125 \\sim C40 \\sim C20 \\sim C96 \\sim
C69 \\sim C121 \\sim C35 \\sim C66 \\sim C60 \\sim C88 \\sim C110 \\sim C50
\\sim C83 \\sim C63 \\sim C52 \\sim C119 \\sim C84 \\sim C87 \\sim C114 \\sim
C10 \\sim C42 \\sim C113 \\sim C72 \\sim C126 \\sim C82 \\sim C112 \\sim C101
\\sim C47 \\sim C12 \\sim C123 \\sim C41 \\sim C120 \\sim C100 \\sim C46 \\sim
C89 \\sim C48 \\sim C58 \\sim C118 \\sim C102 \\sim C99 \\sim C68 \\sim C1
\\sim C22 \\sim C105 \\sim C106 \\sim C104 \\sim C141 \\sim C142 \\sim C24
\\sim C23 \\sim C21 \\sim C2 \\sim C103 \\sim C137 \\sim C138 \\sim C139 \\sim
C140: within 4A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
4A
Uanis(C1) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(N2) \\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(Ag32)=FVAR(1)
 Sof(Ag2A)=1-FVAR(2)
 Sof(Ag31)=FVAR(2)
 Sof(Ag3A)=1-FVAR(3)
 Sof(Ag1)=FVAR(3)
 Sof(Ag4A)=1-FVAR(4)
 Sof(Ag9)=FVAR(4)
 Sof(Ag5A)=1-FVAR(5)
 Sof(Ag7)=FVAR(5)
6.a Riding coordinates:
 C144(H14D,H14E,H14F), C140(H14A,H14B,H14C)
6.b Ternary CH refined with riding coordinates:
 O6(H6), O7(H7), O5(H5)
6.c Me refined with riding coordinates:
 C64(H64A,H64B,H64C), C71(H71A,H71B,H71C), C34(H34A,H34B,H34C), C36(H36A,H36B,
 H36C), C17(H17A,H17B,H17C), C11(H11A,H11B,H11C), C108(H10A,H10B,H10C), C6(H6A,
 H6B,H6C), C95(H95A,H95B,H95C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C124(H12A,
 H12B,H12C), C30(H30A,H30B,H30C), C54(H54A,H54B,H54C), C28(H28A,H28B,H28C),
 C53(H53A,H53B,H53C), C77(H77A,H77B,H77C), C131(H13A,H13B,H13C), C76(H76A,H76B,
 H76C), C18(H18A,H18B,H18C), C130(H13D,H13E,H13F), C70(H70A,H70B,H70C),
 C65(H65A,H65B,H65C), C90(H90A,H90B,H90C), C107(H10D,H10E,H10F), C78(H78A,H78B,
 H78C), C94(H94A,H94B,H94C), C132(H13G,H13H,H13I), C136(H13J,H13K,H13L),
 C16(H16A,H16B,H16C), C134(H13M,H13N,H13O), C59(H59A,H59B,H59C), C125(H12D,H12E,
 H12F), C40(H40A,H40B,H40C), C96(H96A,H96B,H96C), C35(H35A,H35B,H35C), C66(H66A,
 H66B,H66C), C60(H60A,H60B,H60C), C88(H88A,H88B,H88C), C83(H83A,H83B,H83C),
 C52(H52A,H52B,H52C), C119(H11D,H11E,H11F), C84(H84A,H84B,H84C), C114(H11G,H11H,
 H11I), C10(H10G,H10H,H10I), C42(H42A,H42B,H42C), C113(H11J,H11K,H11L),
 C72(H72A,H72B,H72C), C126(H12G,H12H,H12I), C82(H82A,H82B,H82C), C112(H11M,H11N,
 H11O), C101(H10J,H10K,H10L), C47(H47A,H47B,H47C), C12(H12J,H12K,H12L),
 C41(H41A,H41B,H41C), C120(H12M,H12N,H12O), C100(H10M,H10N,H10O), C46(H46A,H46B,
 H46C), C89(H89A,H89B,H89C), C48(H48A,H48B,H48C), C58(H58A,H58B,H58C),
 C118(H11P,H11Q,H11R), C102(H10P,H10Q,H10R), C22(H22A,H22B,H22C), C106(H10S,
 H10T,H10U), C142(H14G,H14H,H14I), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C),
 C138(H13P,H13Q,H13R)
6.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C)
;
_shelx_res_checksum              16551
_shelx_hkl_checksum              67784
_shelx_fab_checksum              76522
_platon_squeeze_special_details
;
A solvent mask was calculated and 1327 electrons were 
found in a volume of 3712\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
30[CH3CN] per Asymmetric Unit 
which account for 1320 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'