A classical [V10O28]6− anion templated high-nuclearity silver thiolate cluster
Li, Li; Zhu, Yanjie; Han, Baoliang; Wang, Qiongyi; Zheng, Luming; Feng, Lei; Sun, Di; Wang, Zhi; Chemical Communications  (2022) –; doi:10.1039/D2CC03003A

data_7130430
_publ_section_title
;
 A classical [V10O28]6&#x2212; anion templated high-nuclearity silver
 thiolate cluster
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03003A
_journal_year                    2022
_chemical_formula_moiety
'C354H458Ag50F24N6O54S32V10, 2(C3 H7 N O), 4[CF3COO], 10[C3H7NO]'
_chemical_formula_sum            'C398 H542 Ag50 F36 N18 O74 S32 V10'
_chemical_formula_weight         14375.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-07-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-07-18 deposited with the CCDC.	2022-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.7718(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.6844(3)
_cell_length_b                   27.1429(2)
_cell_length_c                   36.5460(4)
_cell_measurement_reflns_used    42361
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      75.3920
_cell_measurement_theta_min      2.6700
_cell_volume                     25465.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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     47.00 109.00   1.00    1.20    --   48.32  14.00 110.00   62
  2  \w    -24.00   3.00   1.00    1.20    --   48.32 -14.00 -60.00   27
  3  \w    -21.00  26.00   1.00    1.20    --  -48.32  14.00 110.00   47
  4  \w   -122.00 -57.00   1.00    1.20    --  -48.32 -14.00 -60.00   65
  5  \w    -42.00  24.00   1.00    1.20    --  -48.32  38.00-120.00   66
  6  \w    -42.00 -13.00   1.00    7.50    --  -86.25  38.00  90.00   29
  7  \w    -85.00 -13.00   1.00    7.50    --  -86.25 125.00 150.00   72
  8  \w   -120.00 -94.00   1.00    7.50    --  -86.25 -14.00 -60.00   26
  9  \w     92.00 178.00   1.00    7.50    --  106.49  14.00 110.00   86
 10  \w     99.00 177.00   1.00    7.50    --  106.49  19.00   0.00   78
 11  \w     40.00  66.00   1.00    7.50    --  106.49 -57.00  90.00   26
 12  \w     35.00  66.00   1.00    7.50    --  106.49 -57.00  30.00   31
 13  \w     34.00 106.00   1.00    7.50    --  106.49 -99.00  60.00   72
 14  \w     34.00 104.00   1.00    7.50    --  106.49 -99.00 -90.00   70
 15  \w     37.00 111.00   1.00    7.50    --  106.49-125.00-150.00   74
 16  \w     39.00  65.00   1.00    7.50    --  106.49 -57.00-120.00   26
 17  \w     34.00  66.00   1.00    7.50    --  106.49 -57.00 120.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0591231000
_diffrn_orient_matrix_UB_12      -0.0092378000
_diffrn_orient_matrix_UB_13      0.0033786000
_diffrn_orient_matrix_UB_21      0.0023446000
_diffrn_orient_matrix_UB_22      -0.0041185000
_diffrn_orient_matrix_UB_23      -0.0419701000
_diffrn_orient_matrix_UB_31      0.0100374000
_diffrn_orient_matrix_UB_32      0.0558342000
_diffrn_orient_matrix_UB_33      -0.0025027000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            145654
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         2.684
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.328
_exptl_absorpt_correction_T_max  0.175
_exptl_absorpt_correction_T_min  0.038
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_description       block
_exptl_crystal_F_000             14128
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.129
_refine_diff_density_max         3.775
_refine_diff_density_min         -3.430
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2756
_refine_ls_number_reflns         44825
_refine_ls_number_restraints     1760
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1575
_refine_ls_R_factor_gt           0.1448
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1304P)^2^+1135.0790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3506
_refine_ls_wR_factor_ref         0.3593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                37311
_reflns_number_total             44825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03003a2.cif
_cod_data_source_block           Ag50
_cod_original_cell_volume        25465.9(5)
_cod_database_code               7130430
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Ag50C380H500N12F36O68S32V10
_reflns_odcompleteness_completeness 98.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C4-C8
 1.54 with sigma of 0.01
 O1W-Ag2A
 2.6 with sigma of 0.01
 C142-C147
 2.35 with sigma of 0.01
 C179-C147
 2.35 with sigma of 0.01
 N1-C142 = N1-C147 = N1-C179
 1.45 with sigma of 0.01
 C157-C14 = C157-C155 = C157-C16 = C157-C14A = C157-C16A = C157-C15 = C157-C15A
 1.54 with sigma of 0.01
 C54-C49 = C54-C22A = C54-C20A = C54-C21A = C54-C21 = C54-C20 = C54-C22
 1.54 with sigma of 0.01
 C22A-C20A
 2.51 with sigma of 0.01
 C155-C14
 2.51 with sigma of 0.01
 C21A-C22A
 2.51 with sigma of 0.01
 N2-C146 = N2-C149 = N2-C180
 1.45 with sigma of 0.01
 C14-C15
 2.51 with sigma of 0.01
 C14-C16
 2.51 with sigma of 0.01
 C149-C180
 2.35 with sigma of 0.01
 C162-C13A = C162-C11A = C162-C13 = C162-C11 = C162-C12 = C162-C12A = C162-C129
 1.54 with sigma of 0.01
 C146-C180
 2.35 with sigma of 0.01
 C8-C4 = C8-C7 = C8-C10 = C8-C9
 1.54 with sigma of 0.01
 C12-C11
 2.51 with sigma of 0.01
 C13-C12
 2.51 with sigma of 0.01
 C12-C129
 2.51 with sigma of 0.01
 C149-C146
 2.35 with sigma of 0.01
 C10-C7
 2.51 with sigma of 0.01
 C11-C13
 2.51 with sigma of 0.01
 C7-C4
 2.51 with sigma of 0.01
 C9-C7
 2.51 with sigma of 0.01
 N4-C172 = N4-C173 = N4-C174
 1.45 with sigma of 0.01
 C13-C129
 2.51 with sigma of 0.01
 C173-C174
 2.35 with sigma of 0.01
 C174-C172
 2.35 with sigma of 0.01
 C9A-C7A
 2.51 with sigma of 0.01
 C11-C129
 2.51 with sigma of 0.01
 C10-C4
 2.51 with sigma of 0.01
 F1A-F3A
 2.35 with sigma of 0.01
 C9A-C8A
 1.54 with sigma of 0.01
 C10-C9
 2.51 with sigma of 0.01
 C9A-C10A
 2.51 with sigma of 0.01
 F2A-F1A
 2.35 with sigma of 0.01
 C4A-C9A
 2.51 with sigma of 0.01
 F3-F2
 2.35 with sigma of 0.01
 F3-C140 = F2A-C140 = F2-C140 = F1A-C140 = F1-C140 = F3A-C140
 1.45 with sigma of 0.01
 F2-F1
 2.35 with sigma of 0.01
 F1-F3
 2.35 with sigma of 0.01
 F3A-F2A
 2.35 with sigma of 0.01
 C9-C4
 2.51 with sigma of 0.01
 S1-C1
 1.85 with sigma of 0.01
 C173-C172
 2.35 with sigma of 0.01
 O18-C172
 1.25 with sigma of 0.01
 N4-O18
 2.35 with sigma of 0.01
 C175-F10
 1.45 with sigma of 0.01
 F11-C175
 1.45 with sigma of 0.01
 F12-F11
 2.35 with sigma of 0.01
 F12-F10
 2.35 with sigma of 0.01
 F10-F11
 2.35 with sigma of 0.01
 F12-C175
 1.45 with sigma of 0.01
 C16-C155
 2.51 with sigma of 0.01
 C155-C16A
 2.51 with sigma of 0.01
 C155-C14A
 2.51 with sigma of 0.01
 C16A-C155
 2.51 with sigma of 0.01
 C155-C15
 2.51 with sigma of 0.01
 C15A-C155
 2.51 with sigma of 0.01
 C15A-C14A
 2.51 with sigma of 0.01
 C16A-C15A
 2.51 with sigma of 0.01
 C16-C15
 2.51 with sigma of 0.01
 C16A-C14A
 2.51 with sigma of 0.01
 C178-F8
 1.45 with sigma of 0.01
 C34-O22
 1.25 with sigma of 0.01
 C178-C34
 1.55 with sigma of 0.01
 C178-F9
 1.45 with sigma of 0.01
 O21-O22
 2.15 with sigma of 0.01
 C178-F7
 1.45 with sigma of 0.01
 C34-O21
 1.25 with sigma of 0.01
 C140-C121
 1.55 with sigma of 0.01
 C160-C105
 2.51 with sigma of 0.01
 C158-C160
 2.51 with sigma of 0.01
 C159-C105
 2.51 with sigma of 0.01
 C159-C160
 2.51 with sigma of 0.01
 C158-C159
 2.51 with sigma of 0.01
 C138-C105 = C138-C158 = C138-C159 = C138-C160
 1.54 with sigma of 0.01
 C158-C105
 2.51 with sigma of 0.01
 C166-C143 = C166-C167 = C166-C168 = C166-C87
 1.54 with sigma of 0.01
 C11A-C12A
 2.51 with sigma of 0.01
 C13A-C12A
 2.51 with sigma of 0.01
 C13A-C11A
 2.51 with sigma of 0.01
 C13A-C129
 2.51 with sigma of 0.01
 C11A-C129
 2.51 with sigma of 0.01
 C12A-C129
 2.51 with sigma of 0.01
 C142-C179
 2.35 with sigma of 0.01
 C142-O17
 1.25 with sigma of 0.01
 O17-N1
 2.35 with sigma of 0.01
 F7-F9
 2.35 with sigma of 0.01
 F9-F8
 2.35 with sigma of 0.01
 F7-F8
 2.35 with sigma of 0.01
 S1A-C2A
 2.75 with sigma of 0.01
 C1A-S1A
 1.85 with sigma of 0.01
 S1A-C6A
 2.75 with sigma of 0.01
 C7A-C8A = C10A-C8A = C4A-C8A
 1.54 with sigma of 0.01
 C10A-C7A
 2.51 with sigma of 0.01
 C5A-C8A
 2.51 with sigma of 0.01
 C7A-C4A
 2.51 with sigma of 0.01
 C4A-C7A
 2.51 with sigma of 0.01
 C4A-C10A
 2.51 with sigma of 0.01
 C21A-C20A
 2.51 with sigma of 0.01
 C21-C20
 2.51 with sigma of 0.01
 C22-C21
 2.51 with sigma of 0.01
 C22-C20
 2.51 with sigma of 0.01
 C165-C18A = C165-C17 = C165-C19 = C165-C19A = C165-C83
 1.54 with sigma of 0.01
 C165-C17A
 1.54 with sigma of 0.01
 C165-C18
 1.54 with sigma of 0.01
 C19A-C18A
 2.51 with sigma of 0.01
 C19-C18
 2.51 with sigma of 0.01
 C17-C19
 2.51 with sigma of 0.01
 C18A-C17A
 2.51 with sigma of 0.01
 C17A-C19A
 2.51 with sigma of 0.01
 C18-C17
 2.51 with sigma of 0.01
 C83-C18A
 2.51 with sigma of 0.01
 C83-C19
 2.51 with sigma of 0.01
 C17-C83
 2.51 with sigma of 0.01
 C18-C83
 2.51 with sigma of 0.01
 C17A-C83
 2.51 with sigma of 0.01
 C83-C19A
 2.51 with sigma of 0.01
 F4-C123 = F5A-C123 = F4A-C123 = F6-C123 = F6A-C123 = F5-C123
 1.45 with sigma of 0.01
 F5-F6
 2.35 with sigma of 0.01
 F4-F5
 2.35 with sigma of 0.01
 F5A-F6A
 2.35 with sigma of 0.01
 F6-F4
 2.35 with sigma of 0.01
 F4A-F5A
 2.35 with sigma of 0.01
 F6A-F4A
 2.35 with sigma of 0.01
 O25-C146
 1.25 with sigma of 0.01
 N2-O25
 2.35 with sigma of 0.01
 C90-C120 = C90-C126 = C90-C127 = C90-C163
 1.54 with sigma of 0.01
3. Restrained planarity
 C142, C147, C179, N1, O17
 with sigma of 0.01
 C146, C149, C180, N2, O25
 with sigma of 0.01
 C172, C173, C174, N4, O18
 with sigma of 0.01
 C104, C105, C106, C138
 with sigma of 0.01
 C129, C130, C134, C162
 with sigma of 0.01
 C3A, C4A, C5A, C8A
 with sigma of 0.01
 C1A, C2A, C6A, S1A
 with sigma of 0.01
 C4, C8, C3, C5
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Ag4 \\sim Ag4A \\sim Ag5B: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008 within 1.7A
O1W \\sim O1WA: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 1.7A
C39 \\sim C56 \\sim C69 \\sim C73 \\sim C75 \\sim C81 \\sim C111 \\sim C125
\\sim C128 \\sim C35: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008 within 1.7A
C142 \\sim C147 \\sim C179 \\sim N1 \\sim O17: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008 within 1.7A
C20 \\sim C20A \\sim C21 \\sim C21A \\sim C22 \\sim C22A \\sim C23 \\sim C32
\\sim C37 \\sim C44 \\sim C49 \\sim C51 \\sim C54: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008 within 1.7A
C146 \\sim C149 \\sim C180 \\sim N2 \\sim O25: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008 within 1.7A
C14 \\sim C14A \\sim C15 \\sim C15A \\sim C16 \\sim C16A \\sim C150 \\sim C151
\\sim C152 \\sim C153 \\sim C154 \\sim C155 \\sim C157: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008 within 1.7A
C11 \\sim C11A \\sim C12 \\sim C12A \\sim C13 \\sim C13A \\sim C129 \\sim C130
\\sim C131 \\sim C132 \\sim C133 \\sim C134 \\sim C162: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008 within 1.7A
C1 \\sim C1A \\sim C2 \\sim C2A \\sim C3 \\sim C3A \\sim C4 \\sim C4A \\sim C5
\\sim C5A \\sim C6 \\sim C6A \\sim C7 \\sim C7A \\sim C8 \\sim C8A \\sim C9
\\sim C9A \\sim C10 \\sim C10A: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008 within 1.7A
C172 \\sim C173 \\sim C174 \\sim N4 \\sim O18: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008 within 1.7A
Ag2 \\sim Ag2A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 1.7A
Ag9 \\sim Ag9A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 1.7A
C121 \\sim C140 \\sim F1 \\sim F1A \\sim F2 \\sim F2A \\sim F3 \\sim F3A \\sim
O19 \\sim O20: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 1.7A
Ag8 \\sim Ag8A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 1.7A
Ag7 \\sim Ag7A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 1.7A
S1 \\sim S1A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 1.7A
Ag1 \\sim Ag1A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 1.7A
Ag3 \\sim Ag3A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 1.7A
Ag5 \\sim Ag5A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 1.7A
Ag4B \\sim Ag13: within 1.7A with sigma of 0.004 and sigma for terminal atoms
of 0.008 within 1.7A
Ag2B \\sim Ag11: within 1.7A with sigma of 0.004 and sigma for terminal atoms
of 0.008 within 1.7A
Ag3B \\sim Ag12: within 1.7A with sigma of 0.004 and sigma for terminal atoms
of 0.008 within 1.7A
Ag1B \\sim Ag10: within 1.7A with sigma of 0.004 and sigma for terminal atoms
of 0.008 within 1.7A
C47 \\sim C175 \\sim F10 \\sim F11 \\sim F12 \\sim O15 \\sim O16: within 1.7A
with sigma of 0.004 and sigma for terminal atoms of 0.008 within 1.7A
C92 \\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C110
\\sim C137 \\sim C161: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008 within 1.7A
C34 \\sim C178 \\sim F7 \\sim F8 \\sim F9 \\sim O21 \\sim O22: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008 within 1.7A
C43 \\sim C50 \\sim C74 \\sim C93 \\sim C122 \\sim C136 \\sim C139 \\sim C145
\\sim C176 \\sim C177: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008 within 1.7A
C104 \\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C138 \\sim
C158 \\sim C159 \\sim C160: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008 within 1.7A
C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C143 \\sim C166
\\sim C167 \\sim C168: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008 within 1.7A
C17 \\sim C17A \\sim C18 \\sim C18A \\sim C19 \\sim C19A \\sim C24 \\sim C41
\\sim C52 \\sim C68 \\sim C83 \\sim C96 \\sim C165: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008 within 1.7A
C114 \\sim C123 \\sim F4 \\sim F4A \\sim F5 \\sim F5A \\sim F6 \\sim F6A \\sim
O23 \\sim O24: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 1.7A
O2W \\sim O2WA: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 1.7A
C42 \\sim C59 \\sim C72 \\sim C82 \\sim C90 \\sim C94 \\sim C120 \\sim C126
\\sim C127 \\sim C163: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008 within 1.7A
C64 \\sim C65 \\sim C76 \\sim C79 \\sim C113 \\sim C118 \\sim C60 \\sim C36
\\sim C28 \\sim C57: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008 within 1.7A
C26 \\sim C27 \\sim C33 \\sim C48 \\sim C62 \\sim C71 \\sim C77 \\sim C91 \\sim
C119 \\sim C156: within 1.7A with sigma of 0.004 and sigma for terminal atoms
of 0.008 within 1.7A
C164 \\sim C66 \\sim C117 \\sim C135 \\sim C58 \\sim C80 \\sim C63 \\sim C53
\\sim C95 \\sim C97: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008 within 1.7A
C148 \\sim C141 \\sim C124 \\sim C144 \\sim C116 \\sim C115 \\sim C112 \\sim
C78 \\sim C38 \\sim C55: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008 within 1.7A
C70 \\sim C46 \\sim C45 \\sim C67: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008 within 1.7A
O26 \\sim C170 \\sim N3 \\sim C171 \\sim C169: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008 within 1.7A
Uanis(O1WA) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02
Uanis(O1W) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02
5. Others
 1*[Sof(Ag4)]+1*[Sof(Ag4A)]+1*[Sof(Ag5B)]=1 with esd of 0.0001
 Sof(Ag8A)=1-FVAR(1)
 Sof(Ag8)=FVAR(1)
 Sof(Ag7A)=1-FVAR(2)
 Sof(Ag7)=FVAR(2)
 Sof(Ag5A)=1-FVAR(3)
 Sof(Ag5)=FVAR(3)
 Sof(Ag3A)=1-FVAR(4)
 Sof(Ag3)=FVAR(4)
 Sof(S1A)=1-FVAR(5)
 Sof(S1)=FVAR(5)
 Sof(Ag6)=1-FVAR(6)
 Sof(Ag6A)=FVAR(6)
 Sof(Ag1A)=1-FVAR(7)
 Sof(Ag1)=FVAR(7)
 Sof(Ag2)=1-FVAR(8)
 Sof(Ag2A)=FVAR(8)
 Sof(Ag13)=1-FVAR(9)
 Sof(Ag4B)=FVAR(9)
 Sof(Ag2B)=1-FVAR(10)
 Sof(Ag11)=FVAR(10)
 Sof(Ag3B)=1-FVAR(11)
 Sof(Ag12)=FVAR(11)
 Sof(Ag1B)=1-FVAR(12)
 Sof(Ag10)=FVAR(12)
 Sof(Ag9A)=1-FVAR(13)
 Sof(Ag9)=FVAR(13)
 Fixed Sof: C1A(0.5) C2A(0.5) H2A(0.5) C3A(0.5) H3A(0.5) C4A(0.5) C5A(0.5)
 H5A(0.5) C6A(0.5) H6A(0.5) C4(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) C1(0.5)
 C2(0.5) H2(0.5) C3(0.5) H3(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) C7A(0.5)
 H7AA(0.5) H7AB(0.5) H7AC(0.5) C8(0.5) C8A(0.5) C9(0.5) H9A(0.5) H9B(0.5)
 H9C(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) H9AC(0.5) C10(0.5) H10A(0.5) H10B(0.5)
 H10C(0.5) C10A(0.5) H10D(0.5) H10E(0.5) H10F(0.5) C11(0.5) H11A(0.5) H11B(0.5)
 H11C(0.5) C11A(0.5) H11D(0.5) H11E(0.5) H11F(0.5) C12(0.5) H12A(0.5) H12B(0.5)
 H12C(0.5) C12A(0.5) H12D(0.5) H12E(0.5) H12F(0.5) C13(0.5) H13A(0.5) H13B(0.5)
 H13C(0.5) C13A(0.5) H13D(0.5) H13E(0.5) H13F(0.5) C14(0.5) H14A(0.5) H14B(0.5)
 H14C(0.5) C14A(0.5) H14D(0.5) H14E(0.5) H14F(0.5) C15(0.5) H15A(0.5) H15B(0.5)
 H15C(0.5) C15A(0.5) H15D(0.5) H15E(0.5) H15F(0.5) C16(0.5) H16A(0.5) H16B(0.5)
 H16C(0.5) C16A(0.5) H16D(0.5) H16E(0.5) H16F(0.5) C17(0.5) H17A(0.5) H17B(0.5)
 H17C(0.5) C17A(0.5) H17D(0.5) H17E(0.5) H17F(0.5) C18(0.5) H18A(0.5) H18B(0.5)
 H18C(0.5) C18A(0.5) H18D(0.5) H18E(0.5) H18F(0.5) C19(0.5) H19A(0.5) H19B(0.5)
 H19C(0.5) C19A(0.5) H19D(0.5) H19E(0.5) H19F(0.5) C20(0.5) H20A(0.5) H20B(0.5)
 H20C(0.5) C20A(0.5) H20D(0.5) H20E(0.5) H20F(0.5) C21(0.5) H21A(0.5) H21B(0.5)
 H21C(0.5) C21A(0.5) H21D(0.5) H21E(0.5) H21F(0.5) C22(0.5) H22A(0.5) H22B(0.5)
 H22C(0.5) C22A(0.5) H22D(0.5) H22E(0.5) H22F(0.5) F1(0.5) F1A(0.5) F2(0.5)
 F2A(0.5) F3(0.5) F3A(0.5) F4(0.5) F4A(0.5) F5(0.5) F5A(0.5) F6(0.5) F6A(0.5)
 O1W(0.5) O1WA(0.5) O2W(0.5) O2WA(0.5)
6.a Riding coordinates:
 C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC), C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC),
 C10(H10A,H10B,H10C), C10A(H10D,H10E,H10F), C11(H11A,H11B,H11C), C11A(H11D,H11E,
 H11F), C12(H12A,H12B,H12C), C12A(H12D,H12E,H12F), C13(H13A,H13B,H13C),
 C13A(H13D,H13E,H13F), C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C15(H15A,H15B,
 H15C), C15A(H15D,H15E,H15F), C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F),
 C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F), C18(H18A,H18B,H18C), C18A(H18D,H18E,
 H18F), C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F), C20(H20A,H20B,H20C),
 C20A(H20D,H20E,H20F), C21(H21A,H21B,H21C), C21A(H21D,H21E,H21F), C22(H22A,H22B,
 H22C), C22A(H22D,H22E,H22F), C46(H46A,H46B,H46C), C64(H64A,H64B,H64C),
 C67(H67A,H67B,H67C), C70(H70A,H70B,H70C), C91(H91A,H91B,H91C), C92(H92A,H92B,
 H92C), C111(H11G,H11H,H11I), C113(H11J,H11K,H11L), C117(H11M,H11N,H11O),
 C118(H11P,H11Q,H11R), C119(H11S,H11T,H11U), C122(H12G,H12H,H12I), C124(H12J,
 H12K,H12L), C126(H12M,H12N,H12O), C127(H12P,H12Q,H12R), C128(H12S,H12T,H12U),
 C135(H13G,H13H,H13I), C136(H13J,H13K,H13L), C137(H13M,H13N,H13O), C139(H13P,
 H13Q,H13R), C143(H14G,H14H,H14I), C144(H14J,H14K,H14L), C147(H14M,H14N,H14O),
 C148(H14P,H14Q,H14R), C149(H14S,H14T,H14U), C156(H15G,H15H,H15I), C158(H15J,
 H15K,H15L), C159(H15M,H15N,H15O), C160(H16G,H16H,H16I), C161(H16J,H16K,H16L),
 C163(H16M,H16N,H16O), C164(H16P,H16Q,H16R), C167(H16S,H16T,H16U), C168(H16V,
 H16W,H16X), C179(H17G,H17H,H17I), C180(H18G,H18H,H18I), C169(H16Y,H,HA),
 C171(H17P,H17Q,H17R), C173(H17J,H17K,H17L), C174(H17M,H17N,H17O)
6.b Me refined with riding coordinates:
 C75(H75A,H75B,H75C)
6.c Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C5(H5), C6(H6), C2(H2), C3(H3),
 C30(H30), C31(H31), C32(H32), C33(H33), C36(H36), C37(H37), C40(H40), C41(H41),
  C42(H42), C44(H44), C48(H48), C51(H51), C52(H52), C55(H55), C56(H56),
 C57(H57), C60(H60), C61(H61), C63(H63), C68(H68), C71(H71), C72(H72), C73(H73),
  C76(H76), C77(H77), C78(H78), C80(H80), C81(H81), C82(H82), C85(H85),
 C86(H86), C88(H88), C89(H89), C94(H94), C95(H95), C96(H96), C97(H97), C98(H98),
  C99(H99), C101(H101), C102(H102), C104(H104), C106(H106), C107(H107),
 C109(H109), C112(H112), C116(H116), C125(H125), C130(H130), C131(H131),
 C133(H133), C134(H134), C142(H142), C146(H146), C150(H150), C151(H151),
 C153(H153), C154(H154), C176(H176), C145(H145), C93(H93), C177(H177),
 C170(H170), C172(H172)
6.d Fitted hexagon refined as free rotating group:
 C1A(C2A,C3A,C4A,C5A,C6A), C4(C5,C6,C1,C2,C3), C84(C85,C86,C87,C88,C89),
 C98(C99,C100,C101,C102,C103), C104(C105,C106,C107,C108,C109), C129(C130,C131,
 C132,C133,C134), C150(C151,C152,C153,C154,C155), C176(C50,C145,C93,C43,C177)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1320 electrons were 
found in a volume of 5246\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
2[CF3COO], 5[C3H7NO] per Asymmetric Unit 
which account for 1240 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              25460
_shelx_hkl_checksum              41753
_shelx_fab_checksum              67789
_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 1.491
_oxdiff_exptl_absorpt_empirical_full_min 0.680