Anion-templated silver thiolated clusters effected by carboxylate ligands
Xia, Yuhan; Xia, Xin-Yan; Fang, Jun-Jie; Liu, Zheng; Xie, Yun-Peng; Lu, Xing; Dalton Transactions  (2022) –; doi:10.1039/D2DT02194C

data_7711080
_publ_section_title
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 Anion-templated silver thiolated clusters effected by carboxylate ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02194C
_journal_year                    2022
_chemical_formula_moiety         'C35 H46 Ag10 O12 S5.5'
_chemical_formula_sum            'C35 H46 Ag10 O12 S5.5'
_chemical_formula_weight         1913.75
_chemical_name_systematic        xyh03
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-06-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-21 deposited with the CCDC.	2022-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.531(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.032(2)
_cell_length_b                   26.7363(18)
_cell_length_c                   15.9173(12)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    296.3
_cell_measurement_theta_max      24.20
_cell_measurement_theta_min      2.67
_cell_volume                     12670.5(15)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36753
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.443
_diffrn_reflns_theta_min         2.323
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.242
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0981 before and 0.0615 after correction.
The Ratio of minimum to maximum transmission is 0.6118.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.006
_exptl_crystal_description       block
_exptl_crystal_F_000             7280
_exptl_crystal_preparation
;
stir for 2h
solvothermal
;
_exptl_crystal_recrystallization_method 'at room temperature'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.519
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         11636
_refine_ls_number_restraints     269
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1454
_refine_ls_R_factor_gt           0.0799
_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^)+(0.0855P)^2^+452.5862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1953
_refine_ls_wR_factor_ref         0.2505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6159
_reflns_number_total             11636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02194c2.cif
_cod_data_source_block           xyh20211229_158_1_3_0m_a
_cod_original_cell_volume        12670.4(16)
_cod_original_formula_sum        'C35 H46 Ag10 O12 S5.50'
_cod_database_code               7711080
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.738
_shelx_estimated_absorpt_t_min   0.660
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C35-C34 = C41-C34 = C33-C34 = C36-C34 = C8-C9 = C01T-C9 = C10-C9 = C40-C9 =
 C39-C2 = C3-C2 = C38-C2 = C1-C2 = C01Q-C31 = C14A-C31 = C32-C31 = C30-C31 =
 C21-C20 = C01N-C20 = C19-C20 = C37-C20
 1.54 with sigma of 0.01
 O6A-C7 = C7-O5A
 1.2 with sigma of 0.02
 O6A-O5A
 2.078 with sigma of 0.04
 S3-C01T \\sim S3-C8 \\sim S3-C10 \\sim S3-C40
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S1 \\sim O2 \\sim O1 \\sim O4 \\sim O3 \\sim C34 \\sim C33 \\sim C35 \\sim C36
\\sim C41 \\sim C9 \\sim C10 \\sim C8 \\sim C40 \\sim C01T \\sim C2 \\sim C1
\\sim C3 \\sim C38 \\sim C39 \\sim C20 \\sim C19 \\sim C21 \\sim C37 \\sim C01N
\\sim C01Q \\sim C14A \\sim C32 \\sim C31 \\sim C30: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
O5 \\sim O6 \\sim C7 \\sim O6A \\sim O5A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(H31A)=Sof(C14A)=Sof(H14B)=Sof(H14C)=Sof(H14D)=Sof(C01Q)=Sof(H01A)=
 Sof(H01B)=Sof(H01C)=1-FVAR(1)
 Sof(H31)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C30)=Sof(H30A)=Sof(H30B)=
 Sof(H30C)=FVAR(1)
 Sof(H9B)=Sof(C01T)=Sof(H01D)=Sof(H01E)=Sof(H01F)=Sof(C40)=Sof(H40A)=Sof(H40B)=
 Sof(H40C)=1-FVAR(2)
 Sof(H9A)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C8)=Sof(H8A)=Sof(H8B)=
 Sof(H8C)=FVAR(2)
 Sof(H34A)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C41)=Sof(H41A)=Sof(H41B)=
 Sof(H41C)=1-FVAR(3)
 Sof(H34)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C35)=Sof(H35A)=Sof(H35B)=
 Sof(H35C)=FVAR(3)
 Sof(H20A)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C01N)=Sof(H01G)=
 Sof(H01H)=Sof(H01I)=1-FVAR(4)
 Sof(H20)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C21)=Sof(H21A)=Sof(H21B)=
 Sof(H21C)=FVAR(4)
 Sof(H2B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=1-FVAR(5)
 Sof(H2A)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(H3C)=FVAR(5)
 Sof(Ag0B)=1-FVAR(6)
 Sof(Ag7)=FVAR(6)
 Sof(Ag)=1-FVAR(7)
 Sof(Ag5)=FVAR(7)
 Sof(O6A)=Sof(O5A)=1-FVAR(8)
 Sof(O5)=Sof(O6)=FVAR(8)
 Fixed Sof: O2(0.5) O1(0.5) O4(0.5) O3(0.5)
5.a Riding coordinates:
 C33(H33A,H33B,H33C), C30(H30A,H30B,H30C), C40(H40A,H40B,H40C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C)
5.b Ternary CH refined with riding coordinates:
 C34(H34), C34(H34A), C20(H20), C20(H20A), C2(H2A), C2(H2B), C9(H9A), C9(H9B),
 C31(H31), C31(H31A)
5.c Aromatic/amide H refined with riding coordinates:
 C14(H14A), C13(H13), C17(H17), C16(H16), C24(H24), C25(H25), C27(H27),
 C28(H28), C6(H6), C4(H4)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C10(H10A,H10B,H10C), C19(H19A,H19B,H19C),
 C21(H21A,H21B,H21C), C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C8(H8A,H8B,H8C),
  C14A(H14B,H14C,H14D), C01Q(H01A,H01B,H01C), C01T(H01D,H01E,H01F), C36(H36A,
 H36B,H36C), C41(H41A,H41B,H41C), C37(H37A,H37B,H37C), C01N(H01G,H01H,H01I)
5.e Idealised tetrahedral OH refined as rotating group:
 O14(H14)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              6781
_shelx_hkl_checksum              7386
_shelx_fab_checksum              59044
_olex2_exptl_crystal_mounting_method nothing
_olex2_submission_original_sample_id xyh03
_olex2_submission_special_instructions 'No special instructions were received'