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_1571998
_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 Ni4 O55 Si W9, C2 H3 N, 60[CH3CN], 10[H2O]'
_chemical_formula_sum            'C256 H407 Ag38 N66 Ni4 O65 Si W9'
_chemical_formula_weight         11466.09
_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                105.433(4)
_cell_angle_beta                 94.447(4)
_cell_angle_gamma                91.978(4)
_cell_formula_units_Z            2
_cell_length_a                   21.941(3)
_cell_length_b                   23.391(4)
_cell_length_c                   30.897(5)
_cell_measurement_reflns_used    9788
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.103
_cell_measurement_theta_min      2.275
_cell_volume                     15214(4)
_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 0.956
_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  0.1106
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.956
_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            522184
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.278
_diffrn_reflns_theta_min         1.865
_exptl_absorpt_coefficient_mu    6.093
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.503
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             11006
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         5.694
_refine_diff_density_min         -2.699
_refine_diff_density_rms         0.313
_refine_ls_extinction_coef       0.000473(19)
_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   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2270
_refine_ls_number_reflns         52814
_refine_ls_number_restraints     4933
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0936
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1113P)^2^+547.9963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2318
_refine_ls_wR_factor_ref         0.2526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                37465
_reflns_number_total             52814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01502a2.cif
_cod_data_source_block           ag38-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_database_code               1571998
_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
 C33-C34
 1.54 with sigma of 0.01
 C51-C52
 1.54 with sigma of 0.01
 C75-C78
 1.54 with sigma of 0.01
 C15-C17
 1.54 with sigma of 0.01
 C75-C76
 1.54 with sigma of 0.01
 C57-C60
 1.54 with sigma of 0.01
 C75-C77
 1.54 with sigma of 0.01
 C93-C94
 1.54 with sigma of 0.01
 C15-C14
 1.54 with sigma of 0.01
 C51-C53
 1.54 with sigma of 0.01
 C1-C2
 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
 C56-C57
 1.3 with sigma of 0.01
 C37-C38
 1.3 with sigma of 0.01
 C61-C62
 1.3 with sigma of 0.01
 C124-C126
 1.3 with sigma of 0.01
 C19-C20
 1.3 with sigma of 0.01
 C79-C80
 1.3 with sigma of 0.01
 C115-C116
 1.3 with sigma of 0.01
 C128-C129
 1.54 with sigma of 0.01
 C129-C130
 1.54 with sigma of 0.01
 C129-C132
 1.54 with sigma of 0.01
 C129-C131
 1.54 with sigma of 0.01
 C130-C131
 2.53 with sigma of 0.01
 C131-C132
 2.53 with sigma of 0.01
 C130-C132
 2.53 with sigma of 0.01
 C128-C132
 2.6 with sigma of 0.01
 C35-C34
 2.53 with sigma of 0.01
 C35-C36
 2.53 with sigma of 0.01
 C34-C36
 2.53 with sigma of 0.01
 N1-O55
 1.2 with sigma of 0.01
 N1-O56
 1.2 with sigma of 0.01
 N1-O57
 1.2 with sigma of 0.01
 C97-Ag29
 2.22 with sigma of 0.01
 C97-Ag11
 1.996 with sigma of 0.01
 C97-C98
 1.3 with sigma of 0.01
 C98-C99
 1.54 with sigma of 0.01
 C99-C100
 1.54 with sigma of 0.01
 C119-C120
 2.53 with sigma of 0.01
 C118-C120
 2.53 with sigma of 0.01
 C119-C118
 2.53 with sigma of 0.01
 C117-C119
 1.54 with sigma of 0.01
 C117-C118
 1.54 with sigma of 0.01
 C117-C120
 1.54 with sigma of 0.01
 H11E-H11L
 2.6 with sigma of 0.01
3. Rigid bond restraints
 Si1, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Si1, O8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Ag9, O56
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
O1 \\sim O4 \\sim O6 \\sim O8 \\sim O10 \\sim O12 \\sim O14 \\sim O16 \\sim O18
\\sim O20 \\sim O22 \\sim O24 \\sim O26 \\sim O28 \\sim O30 \\sim O32 \\sim O34
\\sim O36 \\sim O38 \\sim O40 \\sim O41 \\sim O21 \\sim O11 \\sim O23 \\sim O3
\\sim O25 \\sim O13 \\sim O27 \\sim O7 \\sim O29 \\sim O15 \\sim O31 \\sim O2
\\sim O33 \\sim O17 \\sim O35 \\sim O9 \\sim O37 \\sim O19 \\sim O39 \\sim O5
\\sim O45 \\sim O42 \\sim O44 \\sim O43 \\sim O47 \\sim O46 \\sim O49 \\sim O48
\\sim O53 \\sim O50 \\sim O51 \\sim O56 \\sim O57 \\sim O55 \\sim O37A \\sim
O21A: within 4A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
4A
C33 \\sim C34 \\sim C35 \\sim C36: within 2A with sigma of 0.007 and sigma for
terminal atoms of 0.001 within 2A
Uanis(C132) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C126)
\\sim Ueq, Uanis(C129) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C124) \\sim Ueq,
Uanis(C131) \\sim Ueq, Uanis(C128) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C112)
\\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C119) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O37A) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O37) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(Ag14) = Uanis(Ag1A) = Uanis(Ag3A) = Uanis(Ag2A)
Uanis(Si1) = Uanis(O8)
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(Ag14)=FVAR(1)
 Sof(Ag2A)=1-FVAR(2)
 Sof(Ag25)=FVAR(2)
 Sof(Ag3A)=1-FVAR(3)
 Sof(Ag34)=FVAR(3)
 Sof(O37A)=1-FVAR(4)
 Sof(O37)=FVAR(4)
 Sof(O21A)=1-FVAR(5)
 Sof(O21)=FVAR(5)
7.a Riding coordinates:
 C123(H12M,H12N,H12O), C124(H12G,H12H,H12I)
7.b Ternary CH refined with riding coordinates:
 O28(H28), O30(H30), O9(H9)
7.c Me refined with riding coordinates:
 C90(H90A,H90B,H90C), C89(H89A,H89B,H89C), C47(H47A,H47B,H47C), C11(H11A,H11B,
 H11C), C88(H88A,H88B,H88C), C122(H12A,H12B,H12C), C60(H60A,H60B,H60C),
 C136(H13A,H13B,H13C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C10(H10A,H10B,
 H10C), C133(H13D,H13E,H13F), C84(H84A,H84B,H84C), C4(H4A,H4B,H4C), C5(H5A,H5B,
 H5C), C30(H30A,H30B,H30C), C24(H24A,H24B,H24C), C12(H12D,H12E,H12F), C72(H72A,
 H72B,H72C), C29(H29A,H29B,H29C), C48(H48A,H48B,H48C), C106(H10D,H10E,H10F),
 C107(H10G,H10H,H10I), C41(H41A,H41B,H41C), C83(H83A,H83B,H83C), C108(H10J,H10K,
 H10L), C22(H22A,H22B,H22C), C82(H82A,H82B,H82C), C113(H11D,H11E,H11F),
 C28(H28A,H28B,H28C), C58(H58A,H58B,H58C), C23(H23A,H23B,H23C), C46(H46A,H46B,
 H46C), C59(H59A,H59B,H59C), C6(H6A,H6B,H6C), C76(H76A,H76B,H76C), C77(H77A,
 H77B,H77C), C18(H18A,H18B,H18C), C64(H64A,H64B,H64C), C42(H42A,H42B,H42C),
 C78(H78A,H78B,H78C), C96(H96A,H96B,H96C), C16(H16A,H16B,H16C), C95(H95A,H95B,
 H95C), C52(H52A,H52B,H52C), C34(H34A,H34B,H34C), C40(H40A,H40B,H40C), C35(H35A,
 H35B,H35C), C94(H94A,H94B,H94C), C114(H11G,H11H,H11I), C112(H11J,H11K,H11L),
 C54(H54A,H54B,H54C), C102(H10M,H10N,H10O), C36(H36A,H36B,H36C), C53(H53A,H53B,
 H53C), C17(H17A,H17B,H17C), C100(H10P,H10Q,H10R), C66(H66A,H66B,H66C),
 C101(H10S,H10T,H10U), C65(H65A,H65B,H65C), C131(H13G,H13H,H13I), C132(H13J,
 H13K,H13L), C130(H13M,H13N,H13O), C120(H12J,H12K,H12L), C119(H11P,H11Q,H11R)
7.d Idealised Me refined as rotating group:
 C118(H11M,H11N,H11O)
;
_shelx_res_checksum              52200
_shelx_hkl_checksum              585
_shelx_fab_checksum              76809
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'