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_1571994
_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 H203 Ag38 Co4 N5 O55 Si W9, C2 H3 N, 20[CH3CN], 80[H2O], 0.5[], 0.5[]'
_chemical_formula_sum            'C176 H426 Ag38 Co4 N26 O135 Si W9'
_chemical_formula_weight         11084.92
_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                105.088(14)
_cell_angle_beta                 94.144(13)
_cell_angle_gamma                92.363(14)
_cell_formula_units_Z            2
_cell_length_a                   21.95(2)
_cell_length_b                   23.43(2)
_cell_length_c                   30.98(3)
_cell_measurement_reflns_used    8800
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.172
_cell_measurement_theta_min      2.167
_cell_volume                     15313(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 0.950
_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  0.0923
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            318704
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.330
_diffrn_reflns_theta_min         1.929
_exptl_absorpt_coefficient_mu    6.029
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.403
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             10636
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         3.494
_refine_diff_density_min         -3.192
_refine_diff_density_rms         0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2245
_refine_ls_number_reflns         53219
_refine_ls_number_restraints     3886
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1316
_refine_ls_R_factor_gt           0.0997
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+862.0457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2225
_refine_ls_wR_factor_ref         0.2444
_reflns_Friedel_coverage         0.000
_reflns_number_gt                38646
_reflns_number_total             53219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01502a2.cif
_cod_data_source_block           ag38-co_sq_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

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        15319(24)
_cod_database_code               1571994
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.394
_shelx_estimated_absorpt_t_min   0.351
_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
 C50-C51
 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
 C51-C54
 1.54 with sigma of 0.01
 C52-C53
 2.53 with sigma of 0.01
 C52-C54
 2.53 with sigma of 0.01
 C53-C54
 2.53 with sigma of 0.01
 C99-C100
 1.54 with sigma of 0.01
 C99-C101
 1.54 with sigma of 0.01
 C99-C102
 1.54 with sigma of 0.01
 C100-C101
 2.53 with sigma of 0.01
 C100-C102
 2.53 with sigma of 0.01
 C101-C102
 2.53 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
 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
 C70-C72
 2.53 with sigma of 0.01
 C71-C72
 2.53 with sigma of 0.01
 C122-C123
 1.54 with sigma of 0.01
 C123-C124
 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
 C124-C125
 2.53 with sigma of 0.01
 C124-C126
 2.53 with sigma of 0.01
 C125-C126
 2.53 with sigma of 0.01
 C75-C76
 1.54 with sigma of 0.01
 C87-C88
 1.54 with sigma of 0.01
 C13-C14
 1.3 with sigma of 0.01
 C25-C26
 1.3 with sigma of 0.01
 C37-C38
 1.3 with sigma of 0.01
 C49-C50
 1.3 with sigma of 0.01
 C67-C68
 1.3 with sigma of 0.01
 C79-C80
 1.3 with sigma of 0.01
 C109-C110
 1.3 with sigma of 0.01
 C115-C116
 1.3 with sigma of 0.01
 C85-C86
 1.3 with sigma of 0.01
 C121-C122
 1.3 with sigma of 0.01
 C103-C104
 1.3 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C7 \\sim C19 \\sim C25 \\sim C74 \\sim C62 \\sim C61 \\sim C37 \\sim C16 \\sim
C43 \\sim C13 \\sim C73 \\sim C1 \\sim C8 \\sim C109 \\sim C133 \\sim C17 \\sim
C20 \\sim C103 \\sim C15 \\sim C14 \\sim C45 \\sim C10 \\sim C26 \\sim C2 \\sim
C63 \\sim C21 \\sim C24 \\sim C44 \\sim C27 \\sim C134 \\sim C3 \\sim C105
\\sim C91 \\sim C67 \\sim C108 \\sim C79 \\sim C64 \\sim C18 \\sim C5 \\sim C93
\\sim C128 \\sim C75 \\sim C110 \\sim C4 \\sim C104 \\sim C68 \\sim C66 \\sim
C29 \\sim C92 \\sim C69 \\sim C9 \\sim C127 \\sim C30 \\sim C38 \\sim C6 \\sim
C80 \\sim C48 \\sim C107 \\sim C81 \\sim C131 \\sim C106 \\sim C23 \\sim C47
\\sim C95 \\sim C116 \\sim C31 \\sim C111 \\sim C132 \\sim C114 \\sim C113
\\sim C115 \\sim C41 \\sim C40 \\sim C39 \\sim C32 \\sim C120 \\sim C112 \\sim
C12 \\sim C28 \\sim C94 \\sim C78 \\sim C22 \\sim C118 \\sim C46 \\sim C36
\\sim C65 \\sim C11 \\sim C35 \\sim C130 \\sim C84 \\sim C83 \\sim C82 \\sim
C129 \\sim C96 \\sim C77 \\sim C57 \\sim C55 \\sim C76 \\sim C70 \\sim C71
\\sim C58 \\sim C59 \\sim C56 \\sim C85 \\sim C86 \\sim C90 \\sim C34 \\sim C42
\\sim C119 \\sim C89 \\sim C87 \\sim C72 \\sim C117 \\sim C49 \\sim C50 \\sim
C98 \\sim C97 \\sim C52 \\sim C54 \\sim C51 \\sim C102 \\sim C100 \\sim C99
\\sim C33 \\sim C101 \\sim C60 \\sim C53 \\sim C88 \\sim C121 \\sim C122 \\sim
C123 \\sim C124 \\sim C125 \\sim C126 \\sim C136 \\sim C135: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C54) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C125) \\sim Ueq, Uanis(C134)
\\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C97) \\sim Ueq,
Uanis(C99) \\sim Ueq, Uanis(C123) \\sim Ueq, Uanis(C122) \\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.a Ternary CH refined with riding coordinates:
 O9(H9), O8(H8)
5.b Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C10(H10A,H10B,H10C), C24(H24A,H24B,
 H24C), C134(H13A,H13B,H13C), C108(H10D,H10E,H10F), C64(H64A,H64B,H64C),
 C18(H18A,H18B,H18C), C5(H5A,H5B,H5C), C128(H12A,H12B,H12C), C4(H4A,H4B,H4C),
 C66(H66A,H66B,H66C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C6(H6A,H6B,H6C),
  C48(H48A,H48B,H48C), C107(H10G,H10H,H10I), C106(H10J,H10K,H10L), C23(H23A,
 H23B,H23C), C47(H47A,H47B,H47C), C95(H95A,H95B,H95C), C132(H13D,H13E,H13F),
 C114(H11A,H11B,H11C), C113(H11D,H11E,H11F), C41(H41A,H41B,H41C), C40(H40A,H40B,
 H40C), C120(H12D,H12E,H12F), C112(H11G,H11H,H11I), C12(H12G,H12H,H12I),
 C28(H28A,H28B,H28C), C94(H94A,H94B,H94C), C78(H78A,H78B,H78C), C22(H22A,H22B,
 H22C), C118(H11J,H11K,H11L), C46(H46A,H46B,H46C), C36(H36A,H36B,H36C),
 C65(H65A,H65B,H65C), C11(H11M,H11N,H11O), C35(H35A,H35B,H35C), C130(H13G,H13H,
 H13I), C84(H84A,H84B,H84C), C83(H83A,H83B,H83C), C82(H82A,H82B,H82C), C96(H96A,
 H96B,H96C), C77(H77A,H77B,H77C), C76(H76A,H76B,H76C), C71(H71A,H71B,H71C),
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C90(H90A,H90B,H90C), C34(H34A,H34B,
 H34C), C42(H42A,H42B,H42C), C119(H11P,H11Q,H11R), C89(H89A,H89B,H89C),
 C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C102(H10M,H10N,H10O), C100(H10P,H10Q,
 H10R), C101(H10S,H10T,H10U), C60(H60A,H60B,H60C), C53(H53A,H53B,H53C),
 C88(H88A,H88B,H88C), C124(H12J,H12K,H12L), C125(H12M,H12N,H12O), C126(H12P,
 H12Q,H12R)
5.c Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C136(H13J,H13K,H13L)
;
_shelx_res_checksum              20290
_shelx_hkl_checksum              46551
_shelx_fab_checksum              10309
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'