Two structurally new Lindqvist hexaniobate-templated silver thiolate clusters.
Zhao, Zichen; Zhao, Mengyun; Deng, Lan; Li, Qing; Zhang, Jing; Su, Haifeng; Lv, Hongjin; Yang, Guo-Yu; Chemical communications (Cambridge, England) 60 (2024) 5415–5418; doi:10.1039/d4cc00681j

data_7132979
_publ_section_title
;
 Two structurally new Lindqvist hexaniobate-templated silver thiolate
 clusters.
;
_journal_issue                   41
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5415
_journal_page_last               5418
_journal_paper_doi               10.1039/d4cc00681j
_journal_volume                  60
_journal_year                    2024
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'C82 H183 Ag41 K Nb6 O31 S26.5, 2[H3O], 2[H9O4], 1.5[H2O]'
_chemical_formula_sum            'C82 H210 Ag41 K Nb6 O42.5 S26.5'
_chemical_formula_weight         7745.31
_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_Hall           'P 4n 2n'
_space_group_name_H-M_alt        'P 42 21 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-04-17 deposited with the CCDC.	2024-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.1512(5)
_cell_length_b                   32.1512(5)
_cell_length_c                   17.6732(3)
_cell_measurement_reflns_used    22600
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      23.7790
_cell_measurement_theta_min      2.3650
_cell_volume                     18268.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -45.00  30.00   0.50   10.00    --   11.28 -27.00  34.00  150
  2  \w     64.00  90.00   0.50   10.00    --   11.28 178.00  30.00   52
  3  \w    -74.00 -30.00   0.50   10.00    --   11.28 -19.00 120.00   88
  4  \w      5.00  30.00   0.50   10.00    --  -14.56 -99.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0124823000
_diffrn_orient_matrix_UB_12      0.0178648000
_diffrn_orient_matrix_UB_13      0.0062399000
_diffrn_orient_matrix_UB_21      -0.0164247000
_diffrn_orient_matrix_UB_22      0.0128692000
_diffrn_orient_matrix_UB_23      -0.0130424000
_diffrn_orient_matrix_UB_31      -0.0077949000
_diffrn_orient_matrix_UB_32      0.0014957000
_diffrn_orient_matrix_UB_33      0.0374429000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0920
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            77451
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.141
_diffrn_reflns_theta_min         2.003
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.017
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.816
_exptl_crystal_description       plate
_exptl_crystal_F_000             14632
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.542
_refine_diff_density_min         -2.224
_refine_diff_density_rms         0.228
_refine_ls_abs_structure_details
;
 Flack x determined using 4233 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         22246
_refine_ls_number_restraints     314
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1399
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1310P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2074
_refine_ls_wR_factor_ref         0.2356
_reflns_Friedel_coverage         0.769
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.783
_reflns_number_gt                12930
_reflns_number_total             22246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00681j2.cif
_cod_data_source_block           2_auto
_cod_depositor_comments
'Adding full bibliography for 7132978--7132979.cif.'
_cod_original_cell_volume        18268.8(6)
_cod_original_formula_sum        'C82 H210 Ag41 K Nb6 O42.50 S26.50'
_cod_database_code               7132979
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.434
_shelx_estimated_absorpt_t_min   0.314
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Shared sites
{Ag29, K1}
2. Restrained distances
 C34-C36
 2.5 with sigma of 0.02
 C36-C35
 1.5 with sigma of 0.02
 C34-C35
 1.5 with sigma of 0.02
 C9-C7
 2.5 with sigma of 0.02
 O14-O13
 2.5 with sigma of 0.02
 C1-C3
 2.5 with sigma of 0.02
 S1-C2
 1.9 with sigma of 0.02
 C3-C2
 1.6 with sigma of 0.02
 C2-C1
 1.6 with sigma of 0.02
 C31-C33
 2.5 with sigma of 0.02
 C32-C33
 1.5 with sigma of 0.02
 C31-C32
 1.5 with sigma of 0.02
 S11-C32
 1.9 with sigma of 0.02
 C20-C19
 1.5 with sigma of 0.02
 C21-C20
 1.5 with sigma of 0.02
 C21-C19
 2.7 with sigma of 0.02
 C12-C10
 2.5 with sigma of 0.02
 C12-C11
 1.5 with sigma of 0.02
 C11-C10
 1.5 with sigma of 0.02
 C30-C29
 1.5 with sigma of 0.02
 C30-C28
 2.5 with sigma of 0.02
 C28-C29
 1.5 with sigma of 0.02
 C13-C15
 2.5 with sigma of 0.02
 C14-C15
 1.5 with sigma of 0.02
 C14-C13
 1.5 with sigma of 0.02
 C41-O16
 1.4 with sigma of 0.02
 C41-C42
 1.6 with sigma of 0.02
 C23-C22
 1.5 with sigma of 0.02
 C24-C23
 1.5 with sigma of 0.02
 C24-C22
 2.5 with sigma of 0.02
 S8-C23
 1.9 with sigma of 0.02
 O15-C41
 1.4 with sigma of 0.02
 O15-O16
 2 with sigma of 0.02
 C37-C38
 1.6 with sigma of 0.02
 C18-C17
 1.5 with sigma of 0.02
 C18-C16
 2.5 with sigma of 0.02
 S6-C17
 1.9 with sigma of 0.02
 C17-C16
 1.5 with sigma of 0.02
 O12-C37
 1.1 with sigma of 0.02
 O19-Ag12
 2.6 with sigma of 0.02
 Ag12-O19
 2.55 with sigma of 0.02
 O16-O15
 2.01 with sigma of 0.02
 Ag27-O16
 2.2 with sigma of 0.02
 Ag7-O15
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O16: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
1.7A
C38: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
1.7A
O19: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of
0.0025 and sigma for terminal atoms of 0.005
Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.0025 and sigma for
terminal atoms of 0.005
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of
0.025 and sigma for terminal atoms of 0.01
Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(O14) \\sim Ueq: with sigma of 0.0025 and sigma for terminal atoms of 0.005
Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.0025 and sigma for
terminal atoms of 0.001
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of
0.0025 and sigma for terminal atoms of 0.005
Uanis(C21) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of
0.0025 and sigma for terminal atoms of 0.005
Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of
0.0025 and sigma for terminal atoms of 0.005
Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of
0.0025 and sigma for terminal atoms of 0.005
Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.0025 and sigma for
terminal atoms of 0.005
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of
0.0025 and sigma for terminal atoms of 0.005
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O16) \\sim Ueq: with sigma of 0.00025 and sigma for terminal atoms of
0.0005
Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of
0.0025 and sigma for terminal atoms of 0.005
Uanis(O15) \\sim Ueq: with sigma of 0.00025 and sigma for terminal atoms of
0.0005
Uanis(O12) \\sim Ueq: with sigma of 0.0025 and sigma for terminal atoms of 0.005
Uanis(C38) \\sim Ueq: with sigma of 0.0025 and sigma for terminal atoms of 0.001
Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of
0.0025 and sigma for terminal atoms of 0.005
Uanis(O19) \\sim Ueq: with sigma of 0.0025 and sigma for terminal atoms of 0.005
Uanis(Ag29) = Uanis(K1)
Uanis(C34) = Uanis(C35) = Uanis(C36)
Uanis(C3) = Uanis(C2)
Uanis(C40) = Uanis(C39)
Uanis(C3) = Uanis(C2) = Uanis(C1)
Uanis(C31) = Uanis(C32) = Uanis(C33)
Uanis(C20) = Uanis(C21) = Uanis(C19)
Uanis(C12) = Uanis(C11) = Uanis(C10)
Uanis(C28) = Uanis(C29) = Uanis(C30)
Uanis(C13) = Uanis(C14) = Uanis(C15)
Uanis(C41) = Uanis(C42)
Uanis(C24) = Uanis(C23) = Uanis(C22)
Uanis(O15) = Uanis(O16)
Uanis(C38) = Uanis(C37)
Uanis(C18) = Uanis(C17) = Uanis(C16)
4. Others
 Sof(Ag20)=1-FVAR(1)
 Sof(Ag19)=FVAR(1)
 Sof(Ag26)=1-FVAR(2)
 Sof(Ag25)=FVAR(2)
 Sof(Ag28)=1-FVAR(3)
 Sof(Ag27)=FVAR(3)
 Sof(Ag21)=1-FVAR(4)
 Sof(Ag22)=FVAR(4)
 Sof(Ag16)=1-FVAR(5)
 Sof(Ag15)=FVAR(5)
 Sof(Ag14)=1-FVAR(6)
 Sof(Ag13)=FVAR(6)
 Sof(Ag23)=1-FVAR(7)
 Sof(Ag24)=FVAR(7)
 Sof(Ag18)=1-FVAR(8)
 Sof(Ag17)=FVAR(8)
 Sof(Ag30)=1-FVAR(9)
 Sof(Ag12)=FVAR(9)
 Fixed Sof: Ag29(0.5) K1(0.5) H38A(0.5) H38B(0.5) H38C(0.5)
 Fixed X: C39(0.374439) C40(0.36727) C41(0.50762) C42(0.55612) C37(0.126141)
 C38(0.0909)
 Fixed Y: C39(0.02603) C40(-0.01712) C41(0.11905) C42(0.10557) C37(0.126141)
 C38(0.0909)
 Fixed Z: C39(0.456509) C40(0.448) C41(0.56079) C42(0.563351) C37(0.5) C38(0.5)
5.a Riding coordinates:
 C17(H17), C26(H26), C27(H27A,H27B,H27C), C25(H25A,H25B,H25C), C35(H35),
 C36(H36A,H36B,H36C), C34(H34A,H34B,H34C), C8(H8), C9(H9A,H9B,H9C), C7(H7A,H7B,
 H7C), C5(H5), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C2(H2), C3(H3A,H3B,H3C),
 C40(H40A,H40B,H40C), C1(H1A,H1B,H1C), C32(H32), C31(H31A,H31B,H31C), C33(H33A,
 H33B,H33C), C20(H20), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C12(H12A,H12B,
 H12C), C11(H11), C10(H10A,H10B,H10C), C30(H30A,H30B,H30C), C29(H29), C28(H28A,
 H28B,H28C), C14(H14), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C42(H42A,H42B,
 H42C), C24(H24A,H24B,H24C), C23(H23), C22(H22A,H22B,H22C), C38(H38A,H38B,H38C),
  C16(H16A,H16B,H16C), C18(H18A,H18B,H18C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              27675
_shelx_hkl_checksum              95616
_shelx_fab_checksum              65428
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.572
_oxdiff_exptl_absorpt_empirical_full_min 0.451