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_7132978
_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_formula_moiety         'C97 H203 Ag45 Nb6 O47 S23'
_chemical_formula_sum            'C97 H203 Ag45 Nb6 O47 S23'
_chemical_formula_weight         8270.57
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-03-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-03-25 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            8
_cell_length_a                   28.7435(6)
_cell_length_b                   28.3372(6)
_cell_length_c                   48.7703(15)
_cell_measurement_reflns_used    22671
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      27.8830
_cell_measurement_theta_min      2.1920
_cell_volume                     39723.9(17)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -24.00  79.74   0.38   52.78    --   14.05  38.00 140.00  273
  2  \w   -107.00 -47.72   0.38   52.78    --  -17.33-178.00-150.00  156
  3  \w     -5.00  26.16   0.38   52.78    --  -17.33 -99.00 -30.00   82
;
_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      -0.0053928000
_diffrn_orient_matrix_UB_12      -0.0204870000
_diffrn_orient_matrix_UB_13      0.0077555000
_diffrn_orient_matrix_UB_21      -0.0105613000
_diffrn_orient_matrix_UB_22      -0.0102487000
_diffrn_orient_matrix_UB_23      -0.0117083000
_diffrn_orient_matrix_UB_31      0.0216304000
_diffrn_orient_matrix_UB_32      -0.0100826000
_diffrn_orient_matrix_UB_33      -0.0037948000
_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  0.1186
_diffrn_reflns_av_unetI/netI     0.1232
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            139769
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.951
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.946
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01145
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.766
_exptl_crystal_description       block
_exptl_crystal_F_000             31120
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         4.178
_refine_diff_density_min         -2.067
_refine_diff_density_rms         0.292
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2098
_refine_ls_number_reflns         34941
_refine_ls_number_restraints     1895
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.0761
_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^)+(0.0974P)^2^+339.3565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1835
_refine_ls_wR_factor_ref         0.2071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21899
_reflns_number_total             34941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00681j2.cif
_cod_data_source_block           nb-4_auto
_cod_depositor_comments
'Adding full bibliography for 7132978--7132979.cif.'
_cod_database_code               7132978
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Nb O Ag S'
_shelx_estimated_absorpt_t_max   0.453
_shelx_estimated_absorpt_t_min   0.423
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O19-C95 = O5-C95
 1.24 with sigma of 0.02
 C22-C75 = C22-C45 = C96-C55 = C63-C55 = C47-C41 = C47-C40 = C51-C49 = C17-C49
 = C37-C38 = C59-C35 = C35-C58 = C31-C16 = C53-C16 = O21-C3 = C72-C56 = C92-C56
 = C43-C9 = C8-C43 = C61-C12 = C61-C86 = C88-C73 = C42-C88 = C10-C80 = C10-C27 =
  C36-C93 = C36-C66 = C52-C85 = C2-C85 = C74-C83 = C44-C83 = C19-C79 = C28-C79 =
  C24-C90 = C18-C90 = C78-C4 = C4-C89 = C67-C77 = C67-C62 = C34-C26 = C34-C71 =
 C46-C25 = C46-C69 = C82-C70 = C21-C70 = C65-C91 = C65-C14
 1.49 with sigma of 0.01
 C29-C64 = C76-C54 = C1-C60 = C13-C39 = C30-C15 = C57-C3 = C32-C6 = C37-C38 =
 C48-C95 = C11-C81 = C23-C20 = C50-C98 = C68-C33 = C94-C87
 1.49 with sigma of 0.01
 C32-C6
 1.49 with sigma of 0.01
 C5-C84 = C97-C84
 1.49 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O41 \\sim O16 \\sim O8 \\sim O4 \\sim O39 \\sim O23 \\sim O13 \\sim O28 \\sim
O35 \\sim O42 \\sim O36 \\sim O38 \\sim O25 \\sim O26 \\sim O27 \\sim O30 \\sim
O33 \\sim O34 \\sim O47 \\sim O48 \\sim O24 \\sim O37 \\sim O12 \\sim O22 \\sim
O31 \\sim O2 \\sim O15 \\sim O29 \\sim O11 \\sim O40 \\sim O17 \\sim O43 \\sim
O6 \\sim O44 \\sim O18 \\sim O45 \\sim O21 \\sim O46 \\sim O1 \\sim O32 \\sim
O10 \\sim O3 \\sim O19 \\sim O5 \\sim O14 \\sim O7 \\sim O20: within 4A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 4A
C98 \\sim C12 \\sim C86 \\sim C50 \\sim C61 \\sim C85 \\sim C36 \\sim C56 \\sim
C70 \\sim C73 \\sim C88 \\sim C90 \\sim C16 \\sim C47 \\sim C53 \\sim C33 \\sim
C54 \\sim C76 \\sim C69 \\sim C79 \\sim C81 \\sim C91 \\sim C14 \\sim C38 \\sim
C58 \\sim C35 \\sim C40 \\sim C49 \\sim C51 \\sim C55 \\sim C37 \\sim C63 \\sim
C65 \\sim C68 \\sim C75 \\sim C71 \\sim C80 \\sim C74 \\sim C77 \\sim C82 \\sim
C87 \\sim C83 \\sim C84 \\sim C92 \\sim C93 \\sim C94 \\sim C62 \\sim C97 \\sim
C52 \\sim C21 \\sim C28 \\sim C26 \\sim C18 \\sim C27 \\sim C2 \\sim C24 \\sim
C66 \\sim C34 \\sim C9 \\sim C43 \\sim C8 \\sim C44 \\sim C3 \\sim C57 \\sim
C31 \\sim C59 \\sim C5 \\sim C67 \\sim C10 \\sim C72 \\sim C19 \\sim C78 \\sim
C89 \\sim C32 \\sim C4 \\sim C41 \\sim C17 \\sim C96 \\sim C6 \\sim C30 \\sim
C39 \\sim C60 \\sim C15 \\sim C42 \\sim C1 \\sim C11 \\sim C13 \\sim C48 \\sim
C95 \\sim C23 \\sim C25 \\sim C46 \\sim C20 \\sim C45 \\sim C22 \\sim C29 \\sim
C64: within 4.5A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
4.5A
Uanis(C22) = Uanis(C45) = Uanis(C75)
4. Others
 Sof(Ag8A)=1-FVAR(1)
 Sof(Ag8B)=FVAR(1)
 Sof(Ag4B)=1-FVAR(2)
 Sof(Ag4A)=FVAR(2)
 Sof(Ag3B)=1-FVAR(3)
 Sof(Ag3A)=FVAR(3)
 Sof(Ag5B)=1-FVAR(4)
 Sof(Ag5A)=FVAR(4)
 Sof(Ag1B)=1-FVAR(5)
 Sof(Ag1A)=FVAR(5)
 Sof(Ag2B)=1-FVAR(6)
 Sof(Ag2A)=FVAR(6)
 Sof(Ag7B)=1-FVAR(7)
 Sof(Ag7A)=FVAR(7)
 Sof(Ag9A)=1-FVAR(8)
 Sof(Ag9B)=FVAR(8)
 Sof(Ag6B)=1-FVAR(9)
 Sof(Ag6A)=FVAR(9)
 Fixed X: C22(0.75102)
 Fixed Y: C22(0.181381)
 Fixed Z: C22(0.183841)
5.a Ternary CH refined with riding coordinates:
 C61(H61), C85(H85), C36(H36), C56(H56), C70(H70), C88(H88), C90(H90),
 C16(H16), C47(H47), C79(H79), C35(H35), C49(H49), C55(H55), C65(H65), C83(H83),
  C84(H84), C34(H34), C43(H43), C67(H67), C10(H10), C4(H4), C46(H46), C22(H22)
5.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C86(H86A,H86B,H86C), C50(H50A,H50B,H50C), C73(H73A,H73B,
 H73C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C69(H69A,H69B,H69C), C91(H91A,
 H91B,H91C), C14(H14A,H14B,H14C), C38(H38A,H38B,H38C), C58(H58A,H58B,H58C),
 C40(H40A,H40B,H40C), C51(H51A,H51B,H51C), C63(H63A,H63B,H63C), C68(H68A,H68B,
 H68C), C75(H75A,H75B,H75C), C71(H71A,H71B,H71C), C80(H80A,H80B,H80C), C74(H74A,
 H74B,H74C), C77(H77A,H77B,H77C), C82(H82A,H82B,H82C), C92(H92A,H92B,H92C),
 C93(H93A,H93B,H93C), C94(H94A,H94B,H94C), C62(H62A,H62B,H62C), C97(H97A,H97B,
 H97C), C52(H52A,H52B,H52C), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C26(H26A,
 H26B,H26C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C2(H2A,H2B,H2C),
 C24(H24A,H24B,H24C), C66(H66A,H66B,H66C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C),
 C44(H44A,H44B,H44C), C57(H57A,H57B,H57C), C31(H31A,H31B,H31C), C59(H59A,H59B,
 H59C), C5(H5A,H5B,H5C), C72(H72A,H72B,H72C), C19(H19A,H19B,H19C), C78(H78A,
 H78B,H78C), C89(H89A,H89B,H89C), C32(H32A,H32B,H32C), C41(H41A,H41B,H41C),
 C17(H17A,H17B,H17C), C96(H96A,H96B,H96C), C30(H30A,H30B,H30C), C39(H39A,H39B,
 H39C), C60(H60A,H60B,H60C), C42(H42A,H42B,H42C), C11(H11A,H11B,H11C), C48(H48A,
 H48B,H48C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C45(H45A,H45B,H45C),
 C29(H29A,H29B,H29C)
;
_shelx_res_checksum              91884
_shelx_hkl_checksum              43917
_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 37.625
_oxdiff_exptl_absorpt_empirical_full_min 0.230