#------------------------------------------------------------------------------
#$Date: 2023-02-24 08:35:21 +0100 (Fri 24 de Feb de 2023) $
#$Revision: 281114 $
#$URL: svn://www.crystallography.net/cod/cif/7/13/13/7131324.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7131324
loop_
_publ_author_name
'Yang, Weiwei'
'Wang, Haiying'
'Chang, Rong'
'Feng, Zhitao'
'Zhu, Yumei'
'Sue, Andrew C.-H.'
_publ_section_title
;
 Handcuff-like metallo-pseudorotaxanes consisting of tiara[5]arene wheels
 and dimeric silver trifluoroacetate axles.
;
_journal_issue                   17
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2457
_journal_page_last               2460
_journal_paper_doi               10.1039/d2cc06951b
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'Ag2 C4 F6 O4, C H Cl3, C45 H50 O10'
_chemical_formula_sum            'C50 H51 Ag2 Cl3 F6 O14'
_chemical_formula_weight         1311.99
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-10-15 deposited with the CCDC.	2023-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.10780(10)
_cell_length_b                   20.0062(2)
_cell_length_c                   21.6776(2)
_cell_measurement_reflns_used    19450
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      73.3070
_cell_measurement_theta_min      3.0160
_cell_volume                     5250.99(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     25.00  84.00   0.50    0.05    --   35.61-102.00  80.00  118
  2  ω   -105.00 -40.00   0.50    0.15    -- -100.00 113.00 -88.00  130
  3  ω   -177.00-132.00   0.50    0.15    -- -100.00 -26.00 -95.00   90
  4  ω    -93.00 -54.00   0.50    0.15    -- -100.00 -26.00 -95.00   78
  5  ω     27.00 110.00   0.50    0.15    --  109.32-102.00  80.00  166
  6  ω    100.00 127.00   0.50    0.15    --  109.32 102.00-176.00   54
  7  ω    -37.00  82.00   0.50    0.05    --   35.61 -26.00 -95.00  238
  8  ω      7.00 112.00   0.50    0.05    --   35.61  77.00-180.00  210
  9  ω    -69.00 -19.00   0.50    0.15    -- -100.00 111.00  30.00  100
 10  ω   -137.00 -89.00   0.50    0.15    -- -100.00 179.00  60.00   96
 11  ω    -70.00 -45.00   0.50    0.15    -- -100.00 179.00  60.00   50
 12  ω     88.00 178.00   0.50    0.15    --  109.32 111.00 120.00  180
 13  ω     49.00  75.00   0.50    0.15    --  109.32 -94.00 120.00   52
 14  ω     36.00  73.00   0.50    0.15    --  109.32 -94.00 -30.00   74
 15  ω     29.00 112.00   0.50    0.15    --  109.32-111.00 -90.00  166
 16  ω     78.00 106.00   0.50    0.15    --  109.32 -94.00 -30.00   56
 17  ω     71.00 172.00   0.50    0.15    --  109.32  77.00-120.00  202
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0813975000
_diffrn_orient_matrix_UB_12      -0.0532441000
_diffrn_orient_matrix_UB_13      -0.0239077000
_diffrn_orient_matrix_UB_21      0.0904305000
_diffrn_orient_matrix_UB_22      -0.0538106000
_diffrn_orient_matrix_UB_23      0.0060775000
_diffrn_orient_matrix_UB_31      -0.0375286000
_diffrn_orient_matrix_UB_32      -0.0140871000
_diffrn_orient_matrix_UB_33      0.0666024000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26674
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.742
_diffrn_reflns_theta_min         3.006
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.143
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.003
_refine_diff_density_min         -1.481
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Flack x determined using 3911 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         10225
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1033P)²+9.4501P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1713
_reflns_Friedel_coverage         0.787
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.948
_reflns_number_gt                9688
_reflns_number_total             10225
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc06951b2.cif
_cod_data_source_block           20210907-yww-dmp5-ag-2
_cod_database_code               7131324
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Rigid bond restraints
 O13, Ag3
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 Ag2, O13
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
O13: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O13) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4. Others
 Sof(Ag3)=1-FVAR(1)
 Sof(Ag2)=FVAR(1)
 Sof(Ag4)=1-FVAR(2)
 Sof(Ag1)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C50(H50)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C13(H13A,H13B), C31(H31A,H31B), C39(H39A,H39B), C40(H40A,H40B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C15(H15), C16(H16), C17(H17), C19(H19), C21(H21), C23(H23), C25(H25),
 C32(H32), C35(H35)
5.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C)
;
_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 3.339
_oxdiff_exptl_absorpt_empirical_full_min 0.436
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.56682(6) 0.44522(4) 0.65057(3) 0.0455(3) Uani 0.892(3) 1 d . . P A 1
Ag2 Ag 0.50728(7) 0.56368(5) 0.58043(5) 0.0473(4) Uani 0.684(3) 1 d . U P A 1
Cl1 Cl 0.9462(3) 0.21819(19) 0.82767(13) 0.0759(8) Uani 1 1 d . . . . .
Cl2 Cl 1.0583(3) 0.32713(15) 0.76507(16) 0.0770(8) Uani 1 1 d . . . . .
Cl3 Cl 1.0361(3) 0.19802(14) 0.7070(2) 0.0924(13) Uani 1 1 d . . . . .
O1 O 0.8063(4) 0.3182(3) 0.6631(2) 0.0338(11) Uani 1 1 d . . . . .
O2 O 0.4693(5) 0.3792(3) 0.8138(3) 0.0425(14) Uani 1 1 d . . . . .
O3 O 0.6508(5) 0.7320(3) 0.5993(3) 0.0372(12) Uani 1 1 d . . . . .
O4 O 0.2401(5) 0.4412(3) 0.4370(3) 0.0468(14) Uani 1 1 d . . . . .
O5 O 0.3785(6) 0.6147(3) 0.7722(3) 0.0564(19) Uani 1 1 d . . . . .
O6 O 0.2285(5) 0.6681(3) 0.5444(3) 0.0412(12) Uani 1 1 d . . . . .
O7 O 0.8001(5) 0.5573(3) 0.7532(3) 0.0474(14) Uani 1 1 d . . . . .
F1 F 0.1878(6) 0.4607(4) 0.7192(3) 0.079(2) Uani 1 1 d . . . . .
O8 O 0.5934(5) 0.5982(3) 0.4052(3) 0.0439(13) Uani 1 1 d . . . . .
F2 F 0.1459(6) 0.5342(3) 0.6522(4) 0.078(2) Uani 1 1 d . . . . .
O9 O 0.3676(5) 0.2760(4) 0.6051(3) 0.0539(16) Uani 1 1 d . . . . .
C1 C 0.6977(6) 0.3070(3) 0.6474(3) 0.0251(12) Uani 1 1 d . . . . .
O10 O 0.6701(6) 0.3507(4) 0.4514(4) 0.0598(18) Uani 1 1 d . . . . .
O11 O 0.7275(6) 0.4675(4) 0.6069(4) 0.0611(19) Uani 1 1 d . . . . .
F3 F 0.1528(6) 0.4311(4) 0.6258(4) 0.079(2) Uani 1 1 d . . . . .
C2 C 0.6455(6) 0.3999(3) 0.7735(3) 0.0233(12) Uani 1 1 d . . . . .
C3 C 0.4170(6) 0.6819(3) 0.5214(3) 0.0270(13) Uani 1 1 d . . . . .
C4 C 0.6219(6) 0.3089(3) 0.6959(3) 0.0270(13) Uani 1 1 d . . . . .
C5 C 0.6564(6) 0.3253(3) 0.7611(3) 0.0255(13) Uani 1 1 d . . . . .
H5A H 0.732450 0.311659 0.767379 0.031 Uiso 1 1 calc R . . . .
H5B H 0.610528 0.300707 0.789889 0.031 Uiso 1 1 calc R . . . .
C6 C 0.4027(6) 0.6722(3) 0.6740(4) 0.0314(15) Uani 1 1 d . . . . .
H6 H 0.327065 0.671692 0.666742 0.038 Uiso 1 1 calc R . . . .
C7 C 0.5570(7) 0.6433(3) 0.7391(3) 0.0313(14) Uani 1 1 d . . . . .
C8 C 0.4827(8) 0.3367(4) 0.4754(4) 0.0390(18) Uani 1 1 d . . . . .
C9 C 0.4068(6) 0.5804(3) 0.4318(3) 0.0296(14) Uani 1 1 d . . . . .
C10 C 0.7174(7) 0.5124(4) 0.7672(3) 0.0316(15) Uani 1 1 d . . . . .
C11 C 0.4294(6) 0.4568(3) 0.4164(3) 0.0316(14) Uani 1 1 d . . . . .
O12 O 0.3895(6) 0.4501(4) 0.6711(4) 0.063(2) Uani 1 1 d . . . . .
C12 C 0.5641(8) 0.3744(4) 0.4484(4) 0.0396(17) Uani 1 1 d . . . . .
C13 C 0.6040(8) 0.6129(3) 0.7970(4) 0.0368(17) Uani 1 1 d . . . . .
H13A H 0.554565 0.621962 0.831150 0.044 Uiso 1 1 calc R . . . .
H13B H 0.674457 0.633814 0.806073 0.044 Uiso 1 1 calc R . . . .
F4 F 0.9106(7) 0.5761(4) 0.5876(6) 0.112(4) Uani 1 1 d . . . . .
C14 C 0.4721(6) 0.7015(3) 0.6315(3) 0.0288(14) Uani 1 1 d . . . . .
C15 C 0.6626(7) 0.2931(4) 0.5872(3) 0.0328(15) Uani 1 1 d . . . . .
H15 H 0.714160 0.290246 0.555538 0.039 Uiso 1 1 calc R . . . .
C16 C 0.7298(6) 0.4432(4) 0.7584(3) 0.0276(13) Uani 1 1 d . . . . .
H16 H 0.795435 0.426457 0.742353 0.033 Uiso 1 1 calc R . . . .
C17 C 0.5106(6) 0.6661(3) 0.4862(3) 0.0301(14) Uani 1 1 d . . . . .
H17 H 0.576353 0.689103 0.492689 0.036 Uiso 1 1 calc R . . . .
C18 C 0.4439(7) 0.6436(3) 0.7277(4) 0.0352(16) Uani 1 1 d . . . . .
C19 C 0.5358(6) 0.4940(3) 0.8073(3) 0.0302(15) Uani 1 1 d . . . . .
H19 H 0.470906 0.510642 0.824271 0.036 Uiso 1 1 calc R . . . .
C20 C 0.3460(7) 0.4174(4) 0.4426(4) 0.0388(17) Uani 1 1 d . . . . .
C21 C 0.3143(6) 0.5973(3) 0.4662(3) 0.0287(14) Uani 1 1 d . . . . .
H21 H 0.248669 0.574192 0.459908 0.034 Uiso 1 1 calc R . . . .
F5 F 0.9299(6) 0.4771(5) 0.5650(5) 0.099(3) Uani 1 1 d . . . . .
C22 C 0.5517(7) 0.2836(3) 0.5745(3) 0.0339(15) Uani 1 1 d . . . . .
C23 C 0.6275(7) 0.6715(3) 0.6962(3) 0.0310(14) Uani 1 1 d . . . . .
H23 H 0.703220 0.671072 0.703267 0.037 Uiso 1 1 calc R . . . .
C24 C 0.3179(6) 0.6485(3) 0.5104(3) 0.0274(13) Uani 1 1 d . . . . .
C25 C 0.3748(8) 0.3577(4) 0.4718(4) 0.0418(18) Uani 1 1 d . . . . .
H25 H 0.319596 0.331456 0.489233 0.050 Uiso 1 1 calc R . . . .
C26 C 0.4754(6) 0.2861(4) 0.6215(4) 0.0357(16) Uani 1 1 d . . . . .
C27 C 0.6205(7) 0.5374(3) 0.7912(3) 0.0302(14) Uani 1 1 d . . . . .
C28 C 0.5482(6) 0.4251(3) 0.7980(3) 0.0272(13) Uani 1 1 d . . . . .
C29 C 0.5052(6) 0.6156(4) 0.4413(3) 0.0307(14) Uani 1 1 d . . . . .
F6 F 0.8769(7) 0.5438(8) 0.4973(4) 0.140(6) Uani 1 1 d . . . . .
C30 C 0.5855(6) 0.7008(3) 0.6419(3) 0.0302(14) Uani 1 1 d . . . . .
O13 O 0.6833(7) 0.5605(6) 0.5586(5) 0.084(2) Uani 1 1 d . U . . .
C31 C 0.4256(6) 0.7331(3) 0.5729(3) 0.0312(14) Uani 1 1 d . . . . .
H31A H 0.353049 0.751518 0.581379 0.037 Uiso 1 1 calc R . . . .
H31B H 0.473263 0.769472 0.559876 0.037 Uiso 1 1 calc R . . . .
C32 C 0.5383(7) 0.4353(4) 0.4195(3) 0.0372(16) Uani 1 1 d . . . . .
H32 H 0.594275 0.461197 0.402394 0.045 Uiso 1 1 calc R . . . .
C33 C 0.8845(8) 0.3219(5) 0.6144(4) 0.047(2) Uani 1 1 d . . . . .
H33A H 0.856232 0.350080 0.582186 0.070 Uiso 1 1 calc GR . . . .
H33B H 0.897782 0.277944 0.598284 0.070 Uiso 1 1 calc GR . . . .
H33C H 0.952447 0.340274 0.629725 0.070 Uiso 1 1 calc GR . . . .
C34 C 0.3235(7) 0.4847(3) 0.6417(4) 0.0356(16) Uani 1 1 d . . . . .
C35 C 0.5098(6) 0.2986(3) 0.6826(3) 0.0287(13) Uani 1 1 d . . . . .
H35 H 0.457897 0.300028 0.714150 0.034 Uiso 1 1 calc R . . . .
O14 O 0.3415(7) 0.5259(5) 0.6015(5) 0.088(3) Uani 1 1 d . . . . .
C36 C 0.7436(7) 0.5155(4) 0.5731(4) 0.0431(19) Uani 1 1 d . . . . .
C37 C 0.2860(7) 0.2830(5) 0.6521(6) 0.055(2) Uani 1 1 d . . . . .
H37A H 0.214154 0.275050 0.634850 0.082 Uiso 1 1 calc GR . . . .
H37B H 0.288964 0.327451 0.668692 0.082 Uiso 1 1 calc GR . . . .
H37C H 0.299954 0.251240 0.684352 0.082 Uiso 1 1 calc GR . . . .
C38 C 0.3669(8) 0.4035(5) 0.8353(5) 0.058(3) Uani 1 1 d . . . . .
H38A H 0.333105 0.430441 0.803921 0.087 Uiso 1 1 calc GR . . . .
H38B H 0.378552 0.430054 0.871637 0.087 Uiso 1 1 calc GR . . . .
H38C H 0.319478 0.366540 0.845079 0.087 Uiso 1 1 calc GR . . . .
C39 C 0.4016(7) 0.5234(4) 0.3858(3) 0.0354(16) Uani 1 1 d . . . . .
H39A H 0.453357 0.531759 0.352552 0.042 Uiso 1 1 calc R . . . .
H39B H 0.328040 0.521084 0.368240 0.042 Uiso 1 1 calc R . . . .
C40 C 0.5130(9) 0.2716(4) 0.5080(4) 0.046(2) Uani 1 1 d . . . . .
H40A H 0.571238 0.249329 0.485206 0.056 Uiso 1 1 calc R . . . .
H40B H 0.449125 0.242287 0.508477 0.056 Uiso 1 1 calc R . . . .
C41 C 0.2674(8) 0.6327(4) 0.7752(5) 0.049(2) Uani 1 1 d . . . . .
H41A H 0.229143 0.615324 0.739865 0.073 Uiso 1 1 calc GR . . . .
H41B H 0.261218 0.680556 0.775706 0.073 Uiso 1 1 calc GR . . . .
H41C H 0.235202 0.614699 0.812102 0.073 Uiso 1 1 calc GR . . . .
C42 C 0.7677(7) 0.7290(5) 0.6077(5) 0.054(2) Uani 1 1 d . . . . .
H42A H 0.803677 0.752114 0.574548 0.080 Uiso 1 1 calc GR . . . .
H42B H 0.791056 0.683113 0.608088 0.080 Uiso 1 1 calc GR . . . .
H42C H 0.786884 0.749646 0.646219 0.080 Uiso 1 1 calc GR . . . .
C43 C 0.2018(8) 0.4784(5) 0.6601(5) 0.048(2) Uani 1 1 d . . . . .
C44 C 0.1263(7) 0.6393(5) 0.5288(4) 0.046(2) Uani 1 1 d . . . . .
H44A H 0.114827 0.642995 0.485145 0.070 Uiso 1 1 calc GR . . . .
H44B H 0.068197 0.662295 0.550216 0.070 Uiso 1 1 calc GR . . . .
H44C H 0.126217 0.593040 0.540497 0.070 Uiso 1 1 calc GR . . . .
C45 C 0.6940(7) 0.6340(6) 0.4147(4) 0.051(2) Uani 1 1 d . . . . .
H45A H 0.750497 0.615698 0.388578 0.077 Uiso 1 1 calc GR . . . .
H45B H 0.716053 0.629982 0.457032 0.077 Uiso 1 1 calc GR . . . .
H45C H 0.683004 0.680243 0.404711 0.077 Uiso 1 1 calc GR . . . .
C46 C 0.8643(9) 0.5283(6) 0.5542(6) 0.060(3) Uani 1 1 d . . . . .
C47 C 0.9045(8) 0.5305(5) 0.7345(6) 0.057(3) Uani 1 1 d . . . . .
H47A H 0.895413 0.505448 0.697063 0.085 Uiso 1 1 calc GR . . . .
H47B H 0.932492 0.501714 0.766266 0.085 Uiso 1 1 calc GR . . . .
H47C H 0.955577 0.566439 0.727596 0.085 Uiso 1 1 calc GR . . . .
C48 C 0.1513(9) 0.4000(6) 0.4586(7) 0.067(3) Uani 1 1 d . . . . .
H48A H 0.158688 0.355891 0.441627 0.101 Uiso 1 1 calc GR . . . .
H48B H 0.082168 0.418936 0.445851 0.101 Uiso 1 1 calc GR . . . .
H48C H 0.153677 0.397547 0.502815 0.101 Uiso 1 1 calc GR . . . .
C49 C 0.7567(10) 0.3929(8) 0.4363(7) 0.085(4) Uani 1 1 d . . . . .
H49A H 0.745503 0.410522 0.395608 0.127 Uiso 1 1 calc GR . . . .
H49B H 0.824858 0.368470 0.437550 0.127 Uiso 1 1 calc GR . . . .
H49C H 0.759712 0.429083 0.465418 0.127 Uiso 1 1 calc GR . . . .
C50 C 0.9756(7) 0.2558(5) 0.7568(4) 0.0449(19) Uani 1 1 d . . . . .
H50 H 0.905416 0.269815 0.738442 0.054 Uiso 1 1 calc R . . . .
Ag3 Ag 0.4947(2) 0.5148(2) 0.54253(13) 0.0743(13) Uani 0.316(3) 1 d . U P A 2
Ag4 Ag 0.5563(7) 0.5170(7) 0.6668(3) 0.082(4) Uani 0.108(3) 1 d . . P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Ag1 Ag2 80.23(18) . . ?
O12 Ag1 Ag2 80.03(19) . . ?
O12 Ag1 O11 160.0(3) . . ?
O13 Ag2 Ag1 81.2(3) . . ?
O13 Ag2 O14 158.2(4) . . ?
O14 Ag2 Ag1 80.6(2) . . ?
C1 O1 C33 117.5(6) . . ?
C28 O2 C38 117.7(6) . . ?
C30 O3 C42 117.9(6) . . ?
C20 O4 C48 118.2(7) . . ?
C18 O5 C41 118.7(7) . . ?
C24 O6 C44 116.7(6) . . ?
C10 O7 C47 117.4(6) . . ?
C29 O8 C45 117.2(7) . . ?
C26 O9 C37 117.4(7) . . ?
O1 C1 C4 116.0(6) . . ?
O1 C1 C15 123.5(6) . . ?
C4 C1 C15 120.5(7) . . ?
C12 O10 C49 119.2(8) . . ?
C36 O11 Ag1 123.7(6) . . ?
C16 C2 C5 120.6(6) . . ?
C16 C2 C28 119.5(6) . . ?
C28 C2 C5 119.9(6) . . ?
C17 C3 C31 119.7(6) . . ?
C24 C3 C17 119.7(6) . . ?
C24 C3 C31 120.5(6) . . ?
C1 C4 C5 121.9(6) . . ?
C1 C4 C35 118.4(7) . . ?
C35 C4 C5 119.6(6) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
C4 C5 C2 110.8(5) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
C14 C6 H6 119.4 . . ?
C14 C6 C18 121.2(7) . . ?
C18 C6 H6 119.4 . . ?
C18 C7 C13 121.4(7) . . ?
C23 C7 C13 119.4(8) . . ?
C23 C7 C18 119.2(7) . . ?
C12 C8 C25 119.4(8) . . ?
C12 C8 C40 119.6(8) . . ?
C25 C8 C40 120.9(9) . . ?
C21 C9 C29 119.1(6) . . ?
C21 C9 C39 120.2(7) . . ?
C29 C9 C39 120.6(7) . . ?
O7 C10 C16 122.3(7) . . ?
C27 C10 O7 117.7(7) . . ?
C27 C10 C16 120.0(7) . . ?
C20 C11 C39 120.6(7) . . ?
C32 C11 C20 119.3(7) . . ?
C32 C11 C39 120.1(7) . . ?
C34 O12 Ag1 123.7(6) . . ?
C34 O12 Ag4 102.2(6) . . ?
O10 C12 C8 117.6(7) . . ?
O10 C12 C32 122.0(8) . . ?
C8 C12 C32 120.4(8) . . ?
C7 C13 H13A 109.1 . . ?
C7 C13 H13B 109.1 . . ?
C7 C13 C27 112.3(6) . . ?
H13A C13 H13B 107.9 . . ?
C27 C13 H13A 109.1 . . ?
C27 C13 H13B 109.1 . . ?
C6 C14 C30 119.2(7) . . ?
C6 C14 C31 120.6(7) . . ?
C30 C14 C31 120.2(7) . . ?
C1 C15 H15 119.8 . . ?
C22 C15 C1 120.5(7) . . ?
C22 C15 H15 119.8 . . ?
C2 C16 C10 120.5(6) . . ?
C2 C16 H16 119.8 . . ?
C10 C16 H16 119.8 . . ?
C3 C17 H17 120.0 . . ?
C3 C17 C29 120.1(7) . . ?
C29 C17 H17 120.0 . . ?
O5 C18 C6 123.6(8) . . ?
O5 C18 C7 116.3(7) . . ?
C6 C18 C7 120.2(7) . . ?
C27 C19 H19 120.0 . . ?
C27 C19 C28 120.0(7) . . ?
C28 C19 H19 120.0 . . ?
O4 C20 C11 116.2(7) . . ?
O4 C20 C25 124.8(9) . . ?
C25 C20 C11 119.0(8) . . ?
C9 C21 H21 119.3 . . ?
C9 C21 C24 121.4(7) . . ?
C24 C21 H21 119.3 . . ?
C15 C22 C40 120.3(8) . . ?
C26 C22 C15 120.0(7) . . ?
C26 C22 C40 119.7(8) . . ?
C7 C23 H23 119.7 . . ?
C7 C23 C30 120.6(7) . . ?
C30 C23 H23 119.7 . . ?
O6 C24 C3 116.9(6) . . ?
O6 C24 C21 123.6(7) . . ?
C3 C24 C21 119.5(6) . . ?
C8 C25 C20 121.6(9) . . ?
C8 C25 H25 119.2 . . ?
C20 C25 H25 119.2 . . ?
O9 C26 C22 116.2(7) . . ?
O9 C26 C35 123.6(8) . . ?
C22 C26 C35 120.2(7) . . ?
C10 C27 C13 120.1(7) . . ?
C10 C27 C19 119.8(6) . . ?
C19 C27 C13 120.0(7) . . ?
O2 C28 C2 116.4(6) . . ?
O2 C28 C19 123.3(6) . . ?
C2 C28 C19 120.2(7) . . ?
O8 C29 C9 117.0(6) . . ?
O8 C29 C17 122.8(7) . . ?
C9 C29 C17 120.2(7) . . ?
O3 C30 C14 117.2(6) . . ?
O3 C30 C23 123.1(7) . . ?
C14 C30 C23 119.7(7) . . ?
C36 O13 Ag2 123.9(8) . . ?
C36 O13 Ag3 108.6(8) . . ?
C3 C31 C14 110.9(5) . . ?
C3 C31 H31A 109.5 . . ?
C3 C31 H31B 109.5 . . ?
C14 C31 H31A 109.5 . . ?
C14 C31 H31B 109.5 . . ?
H31A C31 H31B 108.0 . . ?
C11 C32 C12 120.1(8) . . ?
C11 C32 H32 120.0 . . ?
C12 C32 H32 120.0 . . ?
O1 C33 H33A 109.5 . . ?
O1 C33 H33B 109.5 . . ?
O1 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O12 C34 C43 116.3(7) . . ?
O14 C34 O12 129.1(9) . . ?
O14 C34 C43 114.5(8) . . ?
C4 C35 C26 120.4(7) . . ?
C4 C35 H35 119.8 . . ?
C26 C35 H35 119.8 . . ?
C34 O14 Ag2 123.1(7) . . ?
C34 O14 Ag3 119.0(7) . . ?
O11 C36 C46 116.1(8) . . ?
O13 C36 O11 130.5(9) . . ?
O13 C36 C46 112.5(9) . . ?
O9 C37 H37A 109.5 . . ?
O9 C37 H37B 109.5 . . ?
O9 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O2 C38 H38A 109.5 . . ?
O2 C38 H38B 109.5 . . ?
O2 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C9 C39 C11 111.2(6) . . ?
C9 C39 H39A 109.4 . . ?
C9 C39 H39B 109.4 . . ?
C11 C39 H39A 109.4 . . ?
C11 C39 H39B 109.4 . . ?
H39A C39 H39B 108.0 . . ?
C8 C40 C22 112.0(6) . . ?
C8 C40 H40A 109.2 . . ?
C8 C40 H40B 109.2 . . ?
C22 C40 H40A 109.2 . . ?
C22 C40 H40B 109.2 . . ?
H40A C40 H40B 107.9 . . ?
O5 C41 H41A 109.5 . . ?
O5 C41 H41B 109.5 . . ?
O5 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O3 C42 H42A 109.5 . . ?
O3 C42 H42B 109.5 . . ?
O3 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
F1 C43 F3 106.8(8) . . ?
F1 C43 C34 113.1(8) . . ?
F2 C43 F1 106.5(9) . . ?
F2 C43 F3 107.3(8) . . ?
F2 C43 C34 113.0(7) . . ?
F3 C43 C34 109.8(8) . . ?
O6 C44 H44A 109.5 . . ?
O6 C44 H44B 109.5 . . ?
O6 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O8 C45 H45A 109.5 . . ?
O8 C45 H45B 109.5 . . ?
O8 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
F4 C46 C36 112.1(10) . . ?
F5 C46 F4 102.1(10) . . ?
F5 C46 C36 113.3(9) . . ?
F6 C46 F4 107.5(12) . . ?
F6 C46 F5 106.7(12) . . ?
F6 C46 C36 114.2(9) . . ?
O7 C47 H47A 109.5 . . ?
O7 C47 H47B 109.5 . . ?
O7 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O4 C48 H48A 109.5 . . ?
O4 C48 H48B 109.5 . . ?
O4 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O10 C49 H49A 109.5 . . ?
O10 C49 H49B 109.5 . . ?
O10 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
Cl1 C50 Cl2 112.2(5) . . ?
Cl1 C50 H50 107.7 . . ?
Cl2 C50 H50 107.7 . . ?
Cl3 C50 Cl1 110.2(5) . . ?
Cl3 C50 Cl2 111.3(5) . . ?
Cl3 C50 H50 107.7 . . ?
O13 Ag3 Ag4 67.3(3) . . ?
O14 Ag3 O13 129.6(4) . . ?
O14 Ag3 Ag4 70.9(3) . . ?
O12 Ag4 Ag3 78.8(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 Ag2 2.9064(10) . ?
Ag1 O11 2.209(7) . ?
Ag1 O12 2.194(7) . ?
Ag2 O13 2.184(9) . ?
Ag2 O14 2.192(8) . ?
Cl1 C50 1.747(9) . ?
Cl2 C50 1.752(10) . ?
Cl3 C50 1.742(10) . ?
O1 C1 1.377(9) . ?
O1 C33 1.420(10) . ?
O2 C28 1.369(9) . ?
O2 C38 1.411(10) . ?
O3 C30 1.366(9) . ?
O3 C42 1.429(11) . ?
O4 C20 1.372(10) . ?
O4 C48 1.433(13) . ?
O5 C18 1.374(10) . ?
O5 C41 1.395(12) . ?
O6 C24 1.367(9) . ?
O6 C44 1.405(10) . ?
O7 C10 1.378(9) . ?
O7 C47 1.431(12) . ?
F1 C43 1.339(12) . ?
O8 C29 1.368(9) . ?
O8 C45 1.427(11) . ?
F2 C43 1.316(11) . ?
O9 C26 1.368(10) . ?
O9 C37 1.426(13) . ?
C1 C4 1.397(10) . ?
C1 C15 1.400(10) . ?
O10 C12 1.370(11) . ?
O10 C49 1.385(16) . ?
O11 C36 1.225(11) . ?
F3 C43 1.342(13) . ?
C2 C5 1.523(8) . ?
C2 C16 1.378(10) . ?
C2 C28 1.386(9) . ?
C3 C17 1.402(10) . ?
C3 C24 1.394(10) . ?
C3 C31 1.519(9) . ?
C4 C5 1.509(10) . ?
C4 C35 1.403(10) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6 0.9300 . ?
C6 C14 1.378(11) . ?
C6 C18 1.390(11) . ?
C7 C13 1.506(10) . ?
C7 C18 1.391(12) . ?
C7 C23 1.381(11) . ?
C8 C12 1.371(13) . ?
C8 C25 1.375(13) . ?
C8 C40 1.528(11) . ?
C9 C21 1.387(10) . ?
C9 C29 1.398(11) . ?
C9 C39 1.517(10) . ?
C10 C16 1.406(10) . ?
C10 C27 1.377(11) . ?
C11 C20 1.402(12) . ?
C11 C32 1.390(11) . ?
C11 C39 1.525(10) . ?
O12 C34 1.234(10) . ?
O12 Ag4 2.425(13) . ?
C12 C32 1.404(11) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C27 1.530(9) . ?
F4 C46 1.322(15) . ?
C14 C30 1.391(11) . ?
C14 C31 1.526(10) . ?
C15 H15 0.9300 . ?
C15 C22 1.384(12) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C17 C29 1.407(10) . ?
C19 H19 0.9300 . ?
C19 C27 1.388(11) . ?
C19 C28 1.400(9) . ?
C20 C25 1.396(11) . ?
C21 H21 0.9300 . ?
C21 C24 1.402(10) . ?
F5 C46 1.318(13) . ?
C22 C26 1.376(12) . ?
C22 C40 1.535(10) . ?
C23 H23 0.9300 . ?
C23 C30 1.411(10) . ?
C25 H25 0.9300 . ?
C26 C35 1.409(11) . ?
F6 C46 1.280(14) . ?
O13 C36 1.201(13) . ?
O13 Ag3 2.484(10) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32 0.9300 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 O14 1.220(11) . ?
C34 C43 1.531(13) . ?
C35 H35 0.9300 . ?
O14 Ag3 2.263(10) . ?
C36 C46 1.540(13) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50 0.9800 . ?
Ag3 Ag4 2.795(8) . ?
