# Electronic Supplementary Material (ESI) for Polymer Chemistry.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_b19183_a_sq
_database_code_depnum_ccdc_archive 'CCDC 2266289'
loop_
_audit_author_name
_audit_author_address
'Jeffery A. Bertke'
;Georgetown University
United States of America
;
_audit_update_record             
;
2023-05-29 deposited with the CCDC.	2023-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            'Diadamantanocyclophane dialdehyde (DADA)'
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H50 O2 S4'
_chemical_formula_sum            'C44 H50 O2 S4'
_chemical_formula_weight         739.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6958(3)
_cell_length_b                   17.1453(5)
_cell_length_c                   18.5627(6)
_cell_angle_alpha                85.106(2)
_cell_angle_beta                 77.072(2)
_cell_angle_gamma                78.794(2)
_cell_volume                     2947.43(16)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9955
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      25.28
_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_F_000             1182
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.019
_exptl_absorpt_coefficient_mu    0.278
_shelx_estimated_absorpt_T_min   0.916
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94680
_exptl_absorpt_correction_T_max  0.99415
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_measurement_device       'Bruker D8 Quest/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            89166
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_av_R_equivalents  0.1494
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.191
_diffrn_reflns_theta_max         25.464
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10864
_reflns_number_gt                6870
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_reduction        
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2016) 
;
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELX-2018-1 (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXLE v932 (Hubschle, 2011)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
Structure was phased by intrinsic methods (Sheldrick, 2015).  Systematic 
conditions suggested the ambiguous space group.  The space group choice 
was confirmed by successful convergence of the full-matrix least-squares 
refinement on F².  The final map had no significant features.  A final 
analysis of variance between observed and calculated structure factors 
showed little dependence on amplitude and resolution. 

For the data crystal, mean I was less than 1 for reflections beyond 
1Å resolution.  Reflections between 1 and 0.83Å resolution were used 
for least-squares refinement to improve the data-to-variable ratio at the 
expense of agreement factors.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0560P)²+2.5754P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10864
_refine_ls_number_parameters     676
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0559
_refine_ls_wR_factor_ref         0.1388
_refine_ls_wR_factor_gt          0.1169
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
S1 S 0.48930(9) 0.12822(5) 0.72002(5) 0.0279(2) Uani 1 1 d . . . . .
S2 S 0.96589(9) 0.32429(5) 0.75988(5) 0.0297(2) Uani 1 1 d . . . . .
S3 S 1.01950(9) 0.78199(5) 0.61266(5) 0.0279(2) Uani 1 1 d . . . . .
S4 S 0.53351(9) 0.61138(5) 0.53217(5) 0.0310(2) Uani 1 1 d . . . . .
S5 S 1.00770(10) 0.45909(5) 0.16831(5) 0.0359(2) Uani 1 1 d . . . . .
S6 S 0.52079(11) 0.29653(6) 0.08702(6) 0.0440(3) Uani 1 1 d . . . . .
O1 O 0.3148(3) 0.19544(15) 0.87663(15) 0.0460(7) Uani 1 1 d . . . . .
O2 O 1.2195(2) 0.70719(13) 0.46109(13) 0.0318(6) Uani 1 1 d . . . . .
C1 C 0.4736(3) 0.28569(17) 0.75019(18) 0.0220(7) Uani 1 1 d . . . . .
C2 C 0.4880(3) 0.27819(18) 0.82436(18) 0.0234(7) Uani 1 1 d . . . . .
C3 C 0.5879(4) 0.31493(18) 0.84540(18) 0.0242(8) Uani 1 1 d . . . . .
H3 H 0.599480 0.308061 0.895160 0.029 Uiso 1 1 calc R U . . .
C4 C 0.6710(4) 0.36125(18) 0.79577(18) 0.0240(8) Uani 1 1 d . . . . .
C5 C 0.6375(3) 0.37993(17) 0.72558(18) 0.0221(7) Uani 1 1 d . . . . .
C6 C 0.5420(3) 0.34020(17) 0.70330(18) 0.0214(7) Uani 1 1 d . . . . .
H6 H 0.523696 0.350877 0.654915 0.026 Uiso 1 1 calc R U . . .
C7 C 0.4080(4) 0.2303(2) 0.8827(2) 0.0325(9) Uani 1 1 d . . . . .
H7 H 0.432152 0.226591 0.929867 0.039 Uiso 1 1 calc R U . . .
C8 C 0.3983(3) 0.23195(18) 0.71898(19) 0.0252(8) Uani 1 1 d . . . . .
H8A H 0.393218 0.250243 0.667436 0.030 Uiso 1 1 calc R U . . .
H8B H 0.298534 0.235726 0.748190 0.030 Uiso 1 1 calc R U . . .
C9 C 0.6597(3) 0.12770(19) 0.65259(18) 0.0245(7) Uani 1 1 d . . . . .
H9A H 0.666323 0.088838 0.614909 0.029 Uiso 1 1 calc R U . . .
H9B H 0.656860 0.180897 0.627025 0.029 Uiso 1 1 calc R U . . .
C10 C 0.7973(3) 0.10741(18) 0.68369(18) 0.0208(7) Uani 1 1 d . . . . .
C11 C 0.8014(4) 0.03123(19) 0.7337(2) 0.0297(8) Uani 1 1 d . . . . .
H11A H 0.718254 0.038077 0.776209 0.036 Uiso 1 1 calc R U . . .
H11B H 0.794902 -0.013967 0.705597 0.036 Uiso 1 1 calc R U . . .
C12 C 0.9420(4) 0.0135(2) 0.7619(2) 0.0316(8) Uani 1 1 d . . . . .
H12 H 0.943579 -0.035984 0.794687 0.038 Uiso 1 1 calc R U . . .
C13 C 1.0701(4) 0.0008(2) 0.6962(2) 0.0352(9) Uani 1 1 d . . . . .
H13A H 1.064269 -0.044365 0.667893 0.042 Uiso 1 1 calc R U . . .
H13B H 1.161024 -0.011822 0.714167 0.042 Uiso 1 1 calc R U . . .
C14 C 1.0680(4) 0.07713(19) 0.64606(19) 0.0274(8) Uani 1 1 d . . . . .
H14 H 1.151556 0.069353 0.602954 0.033 Uiso 1 1 calc R U . . .
C15 C 0.9269(3) 0.09484(19) 0.61827(18) 0.0250(8) Uani 1 1 d . . . . .
H15A H 0.925231 0.143199 0.585049 0.030 Uiso 1 1 calc R U . . .
H15B H 0.921039 0.049876 0.589658 0.030 Uiso 1 1 calc R U . . .
C16 C 0.8107(3) 0.17597(17) 0.72797(17) 0.0188(7) Uani 1 1 d . . . . .
H16A H 0.727893 0.184417 0.770545 0.023 Uiso 1 1 calc R U . . .
H16B H 0.807611 0.225428 0.696215 0.023 Uiso 1 1 calc R U . . .
C17 C 0.9515(3) 0.15897(19) 0.75643(18) 0.0231(7) Uani 1 1 d . . . . .
C18 C 1.0782(3) 0.14591(19) 0.69045(18) 0.0260(8) Uani 1 1 d . . . . .
H18A H 1.169366 0.134026 0.708161 0.031 Uiso 1 1 calc R U . . .
H18B H 1.078457 0.195041 0.658305 0.031 Uiso 1 1 calc R U . . .
C19 C 0.9529(4) 0.08226(19) 0.80561(19) 0.0296(8) Uani 1 1 d . . . . .
H19A H 1.043058 0.069817 0.824306 0.036 Uiso 1 1 calc R U . . .
H19B H 0.871060 0.089929 0.848688 0.036 Uiso 1 1 calc R U . . .
C20 C 0.9610(4) 0.22554(19) 0.80458(19) 0.0285(8) Uani 1 1 d . . . . .
H20A H 1.048521 0.208946 0.825142 0.034 Uiso 1 1 calc R U . . .
H20B H 0.877278 0.230002 0.846813 0.034 Uiso 1 1 calc R U . . .
C21 C 0.8017(4) 0.3841(2) 0.8127(2) 0.0308(8) Uani 1 1 d . . . . .
H21A H 0.799635 0.375313 0.866299 0.037 Uiso 1 1 calc R U . . .
H21B H 0.801741 0.441298 0.799628 0.037 Uiso 1 1 calc R U . . .
C22 C 0.7062(3) 0.43779(18) 0.67662(18) 0.0228(7) Uani 1 1 d . . . . .
C23 C 0.7630(3) 0.48798(18) 0.64034(18) 0.0226(7) Uani 1 1 d . . . . .
C24 C 0.8425(3) 0.54306(17) 0.59461(17) 0.0189(7) Uani 1 1 d . . . . .
C25 C 0.9384(3) 0.57705(17) 0.62315(17) 0.0175(7) Uani 1 1 d . . . . .
H25 H 0.945684 0.565102 0.673235 0.021 Uiso 1 1 calc R U . . .
C26 C 1.0226(3) 0.62747(17) 0.58034(17) 0.0196(7) Uani 1 1 d . . . . .
C27 C 1.0224(3) 0.63708(17) 0.50424(17) 0.0189(7) Uani 1 1 d . . . . .
C28 C 0.9226(3) 0.60586(17) 0.47712(17) 0.0207(7) Uani 1 1 d . . . . .
H28 H 0.920638 0.614524 0.426094 0.025 Uiso 1 1 calc R U . . .
C29 C 0.8259(3) 0.56264(17) 0.52145(17) 0.0200(7) Uani 1 1 d . . . . .
C30 C 1.1190(3) 0.68154(18) 0.44971(19) 0.0244(8) Uani 1 1 d . . . . .
H30 H 1.100028 0.690707 0.401353 0.029 Uiso 1 1 calc R U . . .
C31 C 1.0972(3) 0.67653(18) 0.61706(19) 0.0244(8) Uani 1 1 d . . . . .
H31A H 1.200391 0.668904 0.592636 0.029 Uiso 1 1 calc R U . . .
H31B H 1.090221 0.657909 0.669503 0.029 Uiso 1 1 calc R U . . .
C32 C 0.8408(4) 0.78657(19) 0.67039(18) 0.0264(8) Uani 1 1 d . . . . .
H32A H 0.834342 0.733316 0.694670 0.032 Uiso 1 1 calc R U . . .
H32B H 0.829893 0.823990 0.709910 0.032 Uiso 1 1 calc R U . . .
C33 C 0.7125(3) 0.81226(18) 0.63181(17) 0.0223(7) Uani 1 1 d . . . . .
C34 C 0.5740(4) 0.8253(2) 0.69235(18) 0.0312(8) Uani 1 1 d . . . . .
H34A H 0.578145 0.867210 0.724948 0.037 Uiso 1 1 calc R U . . .
H34B H 0.566001 0.775534 0.722950 0.037 Uiso 1 1 calc R U . . .
C35 C 0.4415(4) 0.8502(2) 0.65739(19) 0.0315(9) Uani 1 1 d . . . . .
H35 H 0.352523 0.858513 0.697408 0.038 Uiso 1 1 calc R U . . .
C36 C 0.4540(4) 0.92802(19) 0.61157(19) 0.0314(8) Uani 1 1 d . . . . .
H36A H 0.457944 0.970307 0.643791 0.038 Uiso 1 1 calc R U . . .
H36B H 0.368729 0.945096 0.589182 0.038 Uiso 1 1 calc R U . . .
C37 C 0.5914(3) 0.91495(18) 0.55036(18) 0.0244(8) Uani 1 1 d . . . . .
H37 H 0.599542 0.965615 0.520089 0.029 Uiso 1 1 calc R U . . .
C38 C 0.7234(4) 0.89001(18) 0.58544(18) 0.0254(8) Uani 1 1 d . . . . .
H38A H 0.812054 0.882514 0.546135 0.030 Uiso 1 1 calc R U . . .
H38B H 0.728778 0.932354 0.617247 0.030 Uiso 1 1 calc R U . . .
C39 C 0.7005(3) 0.74842(17) 0.58222(17) 0.0179(7) Uani 1 1 d . . . . .
H39A H 0.693343 0.698104 0.612034 0.021 Uiso 1 1 calc R U . . .
H39B H 0.789118 0.738882 0.543009 0.021 Uiso 1 1 calc R U . . .
C40 C 0.5700(3) 0.77147(18) 0.54607(17) 0.0207(7) Uani 1 1 d . . . . .
C41 C 0.5830(3) 0.85033(18) 0.50088(18) 0.0242(8) Uani 1 1 d . . . . .
H41A H 0.670343 0.842397 0.460813 0.029 Uiso 1 1 calc R U . . .
H41B H 0.498492 0.867212 0.477874 0.029 Uiso 1 1 calc R U . . .
C42 C 0.4333(3) 0.7854(2) 0.60770(19) 0.0279(8) Uani 1 1 d . . . . .
H42A H 0.347756 0.801605 0.585468 0.034 Uiso 1 1 calc R U . . .
H42B H 0.423440 0.735355 0.637589 0.034 Uiso 1 1 calc R U . . .
C43 C 0.5640(4) 0.70894(19) 0.49276(19) 0.0270(8) Uani 1 1 d . . . . .
H43A H 0.655880 0.701468 0.455701 0.032 Uiso 1 1 calc R U . . .
H43B H 0.486668 0.731128 0.465865 0.032 Uiso 1 1 calc R U . . .
C44 C 0.7016(3) 0.54408(19) 0.49497(19) 0.0255(8) Uani 1 1 d . . . . .
H44A H 0.690585 0.488504 0.510301 0.031 Uiso 1 1 calc R U . . .
H44B H 0.721389 0.548748 0.440243 0.031 Uiso 1 1 calc R U . . .
C45 C 0.7253(4) 0.51782(19) 0.16805(18) 0.0255(8) Uani 1 1 d . . . . .
C46 C 0.6533(4) 0.47812(19) 0.23009(18) 0.0282(8) Uani 1 1 d . . . . .
C47 C 0.5481(4) 0.4366(2) 0.22307(19) 0.0321(9) Uani 1 1 d . . . . .
H47 H 0.502923 0.408326 0.265225 0.038 Uiso 1 1 calc R U . . .
C48 C 0.5064(3) 0.43490(19) 0.15616(19) 0.0265(8) Uani 1 1 d . . . . .
C49 C 0.5626(4) 0.48481(19) 0.09815(18) 0.0266(8) Uani 1 1 d . . . . .
C50 C 0.6717(4) 0.52432(19) 0.10442(18) 0.0249(8) Uani 1 1 d . . . . .
H50 H 0.710488 0.556686 0.063721 0.030 Uiso 1 1 calc R U . . .
O3 O 0.7727(4) 0.51122(18) 0.31985(16) 0.0601(9) Uani 1 1 d . . . . .
C51 C 0.6854(5) 0.4780(2) 0.3039(2) 0.0431(10) Uani 1 1 d . . . . .
H51 H 0.632393 0.449048 0.342743 0.052 Uiso 1 1 calc R U . . .
C52 C 0.8640(4) 0.5442(2) 0.1654(2) 0.0375(9) Uani 1 1 d . . . . .
H52A H 0.853576 0.577521 0.207957 0.045 Uiso 1 1 calc R U . . .
H52B H 0.888783 0.576878 0.119430 0.045 Uiso 1 1 calc R U . . .
C53 C 1.0326(4) 0.4146(2) 0.07991(19) 0.0346(9) Uani 1 1 d . . . . .
H53A H 0.969700 0.449349 0.050391 0.042 Uiso 1 1 calc R U . . .
H53B H 1.133297 0.413898 0.053178 0.042 Uiso 1 1 calc R U . . .
C54 C 1.0012(4) 0.3294(2) 0.08287(18) 0.0262(8) Uani 1 1 d . . . . .
C55 C 1.0851(4) 0.27363(19) 0.13360(19) 0.0277(8) Uani 1 1 d . . . . .
H55A H 1.189423 0.272794 0.115494 0.033 Uiso 1 1 calc R U . . .
H55B H 1.057138 0.293557 0.184283 0.033 Uiso 1 1 calc R U . . .
C56 C 1.0542(4) 0.1901(2) 0.13527(19) 0.0301(8) Uani 1 1 d . . . . .
H56 H 1.109003 0.154707 0.168951 0.036 Uiso 1 1 calc R U . . .
C57 C 0.8928(4) 0.1906(2) 0.16343(18) 0.0270(8) Uani 1 1 d . . . . .
H57A H 0.861915 0.210387 0.214169 0.032 Uiso 1 1 calc R U . . .
H57B H 0.873488 0.135828 0.165136 0.032 Uiso 1 1 calc R U . . .
C58 C 0.8071(3) 0.24486(19) 0.11153(18) 0.0250(8) Uani 1 1 d . . . . .
C59 C 0.8401(3) 0.32832(18) 0.11037(17) 0.0212(7) Uani 1 1 d . . . . .
H59A H 0.808160 0.348639 0.160880 0.025 Uiso 1 1 calc R U . . .
H59B H 0.785400 0.364155 0.077687 0.025 Uiso 1 1 calc R U . . .
C60 C 1.0466(4) 0.2973(2) 0.00486(18) 0.0342(9) Uani 1 1 d . . . . .
H60A H 0.992497 0.332313 -0.028571 0.041 Uiso 1 1 calc R U . . .
H60B H 1.150415 0.297312 -0.014396 0.041 Uiso 1 1 calc R U . . .
C61 C 1.0172(4) 0.2128(2) 0.0063(2) 0.0367(9) Uani 1 1 d . . . . .
H61 H 1.048103 0.192733 -0.044946 0.044 Uiso 1 1 calc R U . . .
C62 C 1.1016(4) 0.1584(2) 0.0569(2) 0.0366(9) Uani 1 1 d . . . . .
H62A H 1.205986 0.157310 0.038438 0.044 Uiso 1 1 calc R U . . .
H62B H 1.083118 0.103547 0.057660 0.044 Uiso 1 1 calc R U . . .
C63 C 0.8568(4) 0.2136(2) 0.03351(19) 0.0332(9) Uani 1 1 d . . . . .
H63A H 0.836890 0.159093 0.033848 0.040 Uiso 1 1 calc R U . . .
H63B H 0.802947 0.248063 -0.000363 0.040 Uiso 1 1 calc R U . . .
C64 C 0.6464(4) 0.2439(2) 0.1431(2) 0.0350(9) Uani 1 1 d . . . . .
H64A H 0.619782 0.267372 0.192273 0.042 Uiso 1 1 calc R U . . .
H64B H 0.633231 0.187715 0.150658 0.042 Uiso 1 1 calc R U . . .
C65 C 0.4157(4) 0.3780(2) 0.1451(2) 0.0425(10) Uani 1 1 d . . . . .
H65A H 0.337248 0.406809 0.121474 0.051 Uiso 1 1 calc R U . . .
H65B H 0.371330 0.355658 0.193759 0.051 Uiso 1 1 calc R U . . .
C66 C 0.5167(4) 0.4937(2) 0.0293(2) 0.0335(9) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

_exptl_special_details           
; 
One distinct cell was identified using APEX3 (Bruker, 2016).  Seven 
frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2016) then corrected for absorption by integration 
using SAINT/SADABS v2014/2 (Bruker, 2016) to sort, merge, and scale 
the combined data.  No decay correction was applied.    
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 0.00 0.1440
1.00 0.00 0.00 0.0670
0.00 0.00 1.00 0.0220
0.00 0.00 -1.00 0.0360
0.00 -1.00 0.00 0.0070
0.00 1.00 0.00 0.0090

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
S1 C8 1.826(3) . ?
S1 C9 1.835(3) . ?
S2 C20 1.825(3) . ?
S2 C21 1.840(4) . ?
S3 C32 1.813(4) . ?
S3 C31 1.821(3) . ?
S4 C43 1.818(3) . ?
S4 C44 1.835(3) . ?
S5 C53 1.816(4) . ?
S5 C52 1.817(4) . ?
S6 C64 1.833(4) . ?
S6 C65 1.834(4) . ?
O1 C7 1.205(4) . ?
O2 C30 1.210(4) . ?
C1 C6 1.383(4) . ?
C1 C2 1.407(5) . ?
C1 C8 1.504(4) . ?
C2 C3 1.392(5) . ?
C2 C7 1.472(5) . ?
C3 C4 1.386(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.408(4) . ?
C4 C21 1.501(4) . ?
C5 C6 1.399(4) . ?
C5 C22 1.444(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.537(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C16 1.532(4) . ?
C10 C15 1.535(4) . ?
C10 C11 1.536(4) . ?
C11 C12 1.535(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C19 1.520(5) . ?
C12 C13 1.529(5) . ?
C12 H12 1.0000 . ?
C13 C14 1.539(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C18 1.525(5) . ?
C14 C15 1.535(4) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.539(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.525(5) . ?
C17 C19 1.535(4) . ?
C17 C20 1.537(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.190(4) . ?
C23 C24 1.435(4) . ?
C24 C25 1.403(4) . ?
C24 C29 1.408(4) . ?
C25 C26 1.383(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.409(4) . ?
C26 C31 1.500(4) . ?
C27 C28 1.393(4) . ?
C27 C30 1.485(4) . ?
C28 C29 1.388(4) . ?
C28 H28 0.9500 . ?
C29 C44 1.495(4) . ?
C30 H30 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.545(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C39 1.526(4) . ?
C33 C38 1.532(4) . ?
C33 C34 1.538(5) . ?
C34 C35 1.539(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C42 1.528(5) . ?
C35 C36 1.530(5) . ?
C35 H35 1.0000 . ?
C36 C37 1.539(5) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C41 1.524(4) . ?
C37 C38 1.535(4) . ?
C37 H37 1.0000 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.533(4) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C43 1.537(4) . ?
C40 C42 1.538(4) . ?
C40 C41 1.540(4) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C50 1.381(4) . ?
C45 C46 1.403(5) . ?
C45 C52 1.489(5) . ?
C46 C47 1.387(5) . ?
C46 C51 1.472(5) . ?
C47 C48 1.393(5) . ?
C47 H47 0.9500 . ?
C48 C49 1.396(5) . ?
C48 C65 1.489(5) . ?
C49 C50 1.393(5) . ?
C49 C66 1.431(4) . ?
C50 H50 0.9500 . ?
O3 C51 1.207(5) . ?
C51 H51 0.9500 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.542(5) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.533(4) . ?
C54 C60 1.533(5) . ?
C54 C59 1.534(4) . ?
C55 C56 1.515(5) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C57 1.534(5) . ?
C56 C62 1.537(5) . ?
C56 H56 1.0000 . ?
C57 C58 1.546(4) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 C59 1.523(4) . ?
C58 C63 1.529(5) . ?
C58 C64 1.539(5) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 C61 1.528(5) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 C63 1.521(5) . ?
C61 C62 1.523(5) . ?
C61 H61 1.0000 . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 C66 1.195(7) 2_665 ?

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
C8 S1 C9 104.29(15) . . ?
C20 S2 C21 102.16(16) . . ?
C32 S3 C31 103.22(16) . . ?
C43 S4 C44 104.21(16) . . ?
C53 S5 C52 103.64(17) . . ?
C64 S6 C65 103.33(18) . . ?
C6 C1 C2 118.2(3) . . ?
C6 C1 C8 119.2(3) . . ?
C2 C1 C8 122.3(3) . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 C7 116.0(3) . . ?
C1 C2 C7 124.5(3) . . ?
C4 C3 C2 121.8(3) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 117.9(3) . . ?
C3 C4 C21 121.5(3) . . ?
C5 C4 C21 120.4(3) . . ?
C6 C5 C4 119.5(3) . . ?
C6 C5 C22 120.9(3) . . ?
C4 C5 C22 119.5(3) . . ?
C1 C6 C5 121.5(3) . . ?
C1 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
O1 C7 C2 126.6(4) . . ?
O1 C7 H7 116.7 . . ?
C2 C7 H7 116.7 . . ?
C1 C8 S1 112.4(2) . . ?
C1 C8 H8A 109.1 . . ?
S1 C8 H8A 109.1 . . ?
C1 C8 H8B 109.1 . . ?
S1 C8 H8B 109.1 . . ?
H8A C8 H8B 107.9 . . ?
C10 C9 S1 116.2(2) . . ?
C10 C9 H9A 108.2 . . ?
S1 C9 H9A 108.2 . . ?
C10 C9 H9B 108.2 . . ?
S1 C9 H9B 108.2 . . ?
H9A C9 H9B 107.4 . . ?
C16 C10 C15 108.5(2) . . ?
C16 C10 C11 108.7(3) . . ?
C15 C10 C11 108.5(3) . . ?
C16 C10 C9 110.6(2) . . ?
C15 C10 C9 108.1(3) . . ?
C11 C10 C9 112.2(3) . . ?
C12 C11 C10 109.7(3) . . ?
C12 C11 H11A 109.7 . . ?
C10 C11 H11A 109.7 . . ?
C12 C11 H11B 109.7 . . ?
C10 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
C19 C12 C13 109.5(3) . . ?
C19 C12 C11 110.2(3) . . ?
C13 C12 C11 109.5(3) . . ?
C19 C12 H12 109.2 . . ?
C13 C12 H12 109.2 . . ?
C11 C12 H12 109.2 . . ?
C12 C13 C14 109.1(3) . . ?
C12 C13 H13A 109.9 . . ?
C14 C13 H13A 109.9 . . ?
C12 C13 H13B 109.9 . . ?
C14 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
C18 C14 C15 110.1(3) . . ?
C18 C14 C13 109.1(3) . . ?
C15 C14 C13 108.8(3) . . ?
C18 C14 H14 109.6 . . ?
C15 C14 H14 109.6 . . ?
C13 C14 H14 109.6 . . ?
C10 C15 C14 110.4(3) . . ?
C10 C15 H15A 109.6 . . ?
C14 C15 H15A 109.6 . . ?
C10 C15 H15B 109.6 . . ?
C14 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
C10 C16 C17 111.7(2) . . ?
C10 C16 H16A 109.3 . . ?
C17 C16 H16A 109.3 . . ?
C10 C16 H16B 109.3 . . ?
C17 C16 H16B 109.3 . . ?
H16A C16 H16B 107.9 . . ?
C18 C17 C19 108.8(3) . . ?
C18 C17 C20 112.2(3) . . ?
C19 C17 C20 107.1(3) . . ?
C18 C17 C16 108.8(3) . . ?
C19 C17 C16 108.1(3) . . ?
C20 C17 C16 111.7(3) . . ?
C17 C18 C14 110.5(3) . . ?
C17 C18 H18A 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C12 C19 C17 110.3(3) . . ?
C12 C19 H19A 109.6 . . ?
C17 C19 H19A 109.6 . . ?
C12 C19 H19B 109.6 . . ?
C17 C19 H19B 109.6 . . ?
H19A C19 H19B 108.1 . . ?
C17 C20 S2 117.1(2) . . ?
C17 C20 H20A 108.0 . . ?
S2 C20 H20A 108.0 . . ?
C17 C20 H20B 108.0 . . ?
S2 C20 H20B 108.0 . . ?
H20A C20 H20B 107.3 . . ?
C4 C21 S2 110.1(2) . . ?
C4 C21 H21A 109.6 . . ?
S2 C21 H21A 109.6 . . ?
C4 C21 H21B 109.6 . . ?
S2 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
C23 C22 C5 175.7(3) . . ?
C22 C23 C24 174.9(3) . . ?
C25 C24 C29 119.9(3) . . ?
C25 C24 C23 119.5(3) . . ?
C29 C24 C23 120.6(3) . . ?
C26 C25 C24 121.8(3) . . ?
C26 C25 H25 119.1 . . ?
C24 C25 H25 119.1 . . ?
C25 C26 C27 118.0(3) . . ?
C25 C26 C31 119.5(3) . . ?
C27 C26 C31 122.1(3) . . ?
C28 C27 C26 119.2(3) . . ?
C28 C27 C30 116.4(3) . . ?
C26 C27 C30 124.4(3) . . ?
C29 C28 C27 122.8(3) . . ?
C29 C28 H28 118.6 . . ?
C27 C28 H28 118.6 . . ?
C28 C29 C24 117.0(3) . . ?
C28 C29 C44 121.5(3) . . ?
C24 C29 C44 121.3(3) . . ?
O2 C30 C27 126.1(3) . . ?
O2 C30 H30 117.0 . . ?
C27 C30 H30 117.0 . . ?
C26 C31 S3 112.0(2) . . ?
C26 C31 H31A 109.2 . . ?
S3 C31 H31A 109.2 . . ?
C26 C31 H31B 109.2 . . ?
S3 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
C33 C32 S3 117.0(2) . . ?
C33 C32 H32A 108.1 . . ?
S3 C32 H32A 108.1 . . ?
C33 C32 H32B 108.1 . . ?
S3 C32 H32B 108.1 . . ?
H32A C32 H32B 107.3 . . ?
C39 C33 C38 108.8(3) . . ?
C39 C33 C34 107.8(3) . . ?
C38 C33 C34 108.8(3) . . ?
C39 C33 C32 112.0(2) . . ?
C38 C33 C32 111.5(3) . . ?
C34 C33 C32 107.8(3) . . ?
C33 C34 C35 110.4(3) . . ?
C33 C34 H34A 109.6 . . ?
C35 C34 H34A 109.6 . . ?
C33 C34 H34B 109.6 . . ?
C35 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
C42 C35 C36 109.7(3) . . ?
C42 C35 C34 109.9(3) . . ?
C36 C35 C34 109.0(3) . . ?
C42 C35 H35 109.4 . . ?
C36 C35 H35 109.4 . . ?
C34 C35 H35 109.4 . . ?
C35 C36 C37 109.1(3) . . ?
C35 C36 H36A 109.9 . . ?
C37 C36 H36A 109.9 . . ?
C35 C36 H36B 109.9 . . ?
C37 C36 H36B 109.9 . . ?
H36A C36 H36B 108.3 . . ?
C41 C37 C38 110.0(3) . . ?
C41 C37 C36 109.2(3) . . ?
C38 C37 C36 109.6(3) . . ?
C41 C37 H37 109.3 . . ?
C38 C37 H37 109.3 . . ?
C36 C37 H37 109.3 . . ?
C33 C38 C37 109.8(3) . . ?
C33 C38 H38A 109.7 . . ?
C37 C38 H38A 109.7 . . ?
C33 C38 H38B 109.7 . . ?
C37 C38 H38B 109.7 . . ?
H38A C38 H38B 108.2 . . ?
C33 C39 C40 112.7(2) . . ?
C33 C39 H39A 109.1 . . ?
C40 C39 H39A 109.1 . . ?
C33 C39 H39B 109.1 . . ?
C40 C39 H39B 109.1 . . ?
H39A C39 H39B 107.8 . . ?
C39 C40 C43 112.2(2) . . ?
C39 C40 C42 108.4(3) . . ?
C43 C40 C42 112.0(3) . . ?
C39 C40 C41 108.0(2) . . ?
C43 C40 C41 107.8(3) . . ?
C42 C40 C41 108.5(2) . . ?
C37 C41 C40 110.6(3) . . ?
C37 C41 H41A 109.5 . . ?
C40 C41 H41A 109.5 . . ?
C37 C41 H41B 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 108.1 . . ?
C35 C42 C40 110.1(3) . . ?
C35 C42 H42A 109.6 . . ?
C40 C42 H42A 109.6 . . ?
C35 C42 H42B 109.6 . . ?
C40 C42 H42B 109.6 . . ?
H42A C42 H42B 108.2 . . ?
C40 C43 S4 117.6(2) . . ?
C40 C43 H43A 107.9 . . ?
S4 C43 H43A 107.9 . . ?
C40 C43 H43B 107.9 . . ?
S4 C43 H43B 107.9 . . ?
H43A C43 H43B 107.2 . . ?
C29 C44 S4 111.7(2) . . ?
C29 C44 H44A 109.3 . . ?
S4 C44 H44A 109.3 . . ?
C29 C44 H44B 109.3 . . ?
S4 C44 H44B 109.3 . . ?
H44A C44 H44B 107.9 . . ?
C50 C45 C46 117.4(3) . . ?
C50 C45 C52 119.2(3) . . ?
C46 C45 C52 123.0(3) . . ?
C47 C46 C45 120.0(3) . . ?
C47 C46 C51 117.5(3) . . ?
C45 C46 C51 122.5(3) . . ?
C46 C47 C48 122.1(3) . . ?
C46 C47 H47 119.0 . . ?
C48 C47 H47 119.0 . . ?
C47 C48 C49 116.9(3) . . ?
C47 C48 C65 121.6(3) . . ?
C49 C48 C65 121.3(3) . . ?
C50 C49 C48 120.4(3) . . ?
C50 C49 C66 117.8(3) . . ?
C48 C49 C66 121.7(3) . . ?
C45 C50 C49 121.9(3) . . ?
C45 C50 H50 119.0 . . ?
C49 C50 H50 119.0 . . ?
O3 C51 C46 126.2(4) . . ?
O3 C51 H51 116.9 . . ?
C46 C51 H51 116.9 . . ?
C45 C52 S5 110.8(2) . . ?
C45 C52 H52A 109.5 . . ?
S5 C52 H52A 109.5 . . ?
C45 C52 H52B 109.5 . . ?
S5 C52 H52B 109.5 . . ?
H52A C52 H52B 108.1 . . ?
C54 C53 S5 116.4(2) . . ?
C54 C53 H53A 108.2 . . ?
S5 C53 H53A 108.2 . . ?
C54 C53 H53B 108.2 . . ?
S5 C53 H53B 108.2 . . ?
H53A C53 H53B 107.4 . . ?
C55 C54 C60 108.5(3) . . ?
C55 C54 C59 109.0(3) . . ?
C60 C54 C59 107.7(3) . . ?
C55 C54 C53 111.1(3) . . ?
C60 C54 C53 109.2(3) . . ?
C59 C54 C53 111.2(3) . . ?
C56 C55 C54 110.4(3) . . ?
C56 C55 H55A 109.6 . . ?
C54 C55 H55A 109.6 . . ?
C56 C55 H55B 109.6 . . ?
C54 C55 H55B 109.6 . . ?
H55A C55 H55B 108.1 . . ?
C55 C56 C57 110.0(3) . . ?
C55 C56 C62 109.5(3) . . ?
C57 C56 C62 109.3(3) . . ?
C55 C56 H56 109.3 . . ?
C57 C56 H56 109.3 . . ?
C62 C56 H56 109.3 . . ?
C56 C57 C58 109.8(3) . . ?
C56 C57 H57A 109.7 . . ?
C58 C57 H57A 109.7 . . ?
C56 C57 H57B 109.7 . . ?
C58 C57 H57B 109.7 . . ?
H57A C57 H57B 108.2 . . ?
C59 C58 C63 109.1(3) . . ?
C59 C58 C64 111.2(3) . . ?
C63 C58 C64 112.1(3) . . ?
C59 C58 C57 108.0(3) . . ?
C63 C58 C57 108.9(3) . . ?
C64 C58 C57 107.4(3) . . ?
C58 C59 C54 111.8(3) . . ?
C58 C59 H59A 109.3 . . ?
C54 C59 H59A 109.3 . . ?
C58 C59 H59B 109.3 . . ?
C54 C59 H59B 109.3 . . ?
H59A C59 H59B 107.9 . . ?
C61 C60 C54 110.3(3) . . ?
C61 C60 H60A 109.6 . . ?
C54 C60 H60A 109.6 . . ?
C61 C60 H60B 109.6 . . ?
C54 C60 H60B 109.6 . . ?
H60A C60 H60B 108.1 . . ?
C63 C61 C62 110.2(3) . . ?
C63 C61 C60 109.3(3) . . ?
C62 C61 C60 109.8(3) . . ?
C63 C61 H61 109.1 . . ?
C62 C61 H61 109.1 . . ?
C60 C61 H61 109.1 . . ?
C61 C62 C56 108.7(3) . . ?
C61 C62 H62A 109.9 . . ?
C56 C62 H62A 109.9 . . ?
C61 C62 H62B 109.9 . . ?
C56 C62 H62B 109.9 . . ?
H62A C62 H62B 108.3 . . ?
C61 C63 C58 109.9(3) . . ?
C61 C63 H63A 109.7 . . ?
C58 C63 H63A 109.7 . . ?
C61 C63 H63B 109.7 . . ?
C58 C63 H63B 109.7 . . ?
H63A C63 H63B 108.2 . . ?
C58 C64 S6 116.4(2) . . ?
C58 C64 H64A 108.2 . . ?
S6 C64 H64A 108.2 . . ?
C58 C64 H64B 108.2 . . ?
S6 C64 H64B 108.2 . . ?
H64A C64 H64B 107.3 . . ?
C48 C65 S6 111.8(3) . . ?
C48 C65 H65A 109.3 . . ?
S6 C65 H65A 109.3 . . ?
C48 C65 H65B 109.3 . . ?
S6 C65 H65B 109.3 . . ?
H65A C65 H65B 107.9 . . ?
C66 C66 C49 174.9(5) 2_665 . ?

_refine_diff_density_max         0.411
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.066



