# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# 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_nr20002
_database_code_depnum_ccdc_archive 'CCDC 2235428'
loop_
_audit_author_name
_audit_author_address
'Gary Stephen Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-01-10 deposited with the CCDC.	2023-03-19 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT410_nr20002             
;
PROBLEM: Short Intra H...H Contact  H26      ..H29A     .       1.89 Ang.
RESPONSE: H atoms added using HFIX
;
_vrf_PLAT910_nr20002             
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         11 Note
RESPONSE: Noted, but no action taken
;
_vrf_PLAT042_nr20002             
;
PROBLEM: Calc. and Reported MoietyFormula Strings  Differ     Please Check
RESPONSE: This is because of a fractionally occuped Br
;
_vrf_PLAT077_nr20002             
;
PROBLEM: Unitcell Contains Non-integer Number of Atoms ..     Please Check
RESPONSE: This is because of a fractionally occuped Br
;
_vrf_PLAT410_nr20002_2           
;
PROBLEM: Short Intra H...H Contact  H22      ..H31A     .       1.95 Ang.
RESPONSE: H atoms added using HFIX
;
_vrf_PLAT906_nr20002             
;
PROBLEM: Large K Value in the Analysis of Variance ......      7.220 Check
RESPONSE: Noted, but no action taken
;
# Added during the CSD deposition process: Tuesday 10 January 2023 03:12 PM
# end Validation Reply Form

_audit_creation_date             2020-09-07
_audit_creation_method           
;
Olex2 1.3-beta
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
g.s.nichol@ed.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H29.959 Br2.041 S'
_chemical_formula_sum            'C34 H29.96 Br2.04 S'
_chemical_formula_weight         633.61
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C68 H60 S2 Br4 '
_chemical_oxdiff_usercomment     '@ 120 K BrTxS'
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'
Br Br -0.2901 2.4595 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.3239(2)
_cell_length_b                   9.5641(4)
_cell_length_c                   20.1031(8)
_cell_angle_alpha                77.186(3)
_cell_angle_beta                 84.695(3)
_cell_angle_gamma                81.803(3)
_cell_volume                     1356.35(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7102
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      28.8590
_cell_measurement_theta_min      4.1030
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.147
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.397
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             643
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 13 7 0.2435
-10 1 0 0.0793
1 -13 -7 0.2208
10 0 1 0.0913
-1 -1 -28 0.0132
1 1 28 0.0132
8 10 4 0.1783

_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of ethanol and dichloromethane  by solvent layering'
_exptl_crystal_size_max          0.512
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.026
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.1531 13.0379 6.7043 0.1649 -0.3925 0.9048
-10.1257 0.6733 -0.3318 0.3798 -0.9154 -0.1332
1.0501 -13.0715 -6.7288 -0.1614 0.3841 -0.9091
10.1938 -0.1635 0.6016 -0.3775 0.9101 0.1706
-0.7883 -1.3864 -28.1360 -0.9155 -0.3799 -0.1328
0.7883 1.3864 28.1360 0.9155 0.3799 0.1328
8.0284 9.8445 4.0223 -0.2595 0.4746 0.8411

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23435
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         3.336
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      9.00  70.00   1.00   15.00    --   10.76-131.00 164.00   61
  2  ω    -36.00  61.00   1.00   15.00    --   -9.35  57.00   0.00   97
  3  ω    -80.00  17.00   1.00   15.00    --   -9.35 -57.00-150.00   97
  4  ω    -42.00  22.00   1.00   15.00    --   -9.35 -77.00  60.00   64
  5  ω    -41.00  21.00   1.00   15.00    --   -9.35  77.00 120.00   62
  6  ω    -15.00  31.00   1.00   15.00    --   -9.35 -99.00  30.00   46
  7  ω    -41.00  21.00   1.00   15.00    --   -9.35  77.00  30.00   62
  8  ω     13.00  73.00   1.00   15.00    --   10.76-138.00 -10.00   60
  9  ω    -82.00 -10.00   1.00   15.00    --   -9.35 -38.00 -60.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0391793000
_diffrn_orient_matrix_UB_12      -0.0083225000
_diffrn_orient_matrix_UB_13      0.0340446000
_diffrn_orient_matrix_UB_21      0.0880874000
_diffrn_orient_matrix_UB_22      -0.0287170000
_diffrn_orient_matrix_UB_23      0.0124480000
_diffrn_orient_matrix_UB_31      0.0178276000
_diffrn_orient_matrix_UB_32      0.0705953000
_diffrn_orient_matrix_UB_33      0.0007427000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4928
_reflns_number_total             6479
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         6479
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0542
_refine_ls_restrained_S_all      1.109
_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/[σ²(Fo²)+(0.0324P)²+1.8245P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1102
_refine_special_details          
;
A residual peak close to C25 was modelled as a small (ca 5%) amount of a tribrominated compound.

#===============================================================================
#>>> The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text

410_ALERT_2_B Short Intra H...H Contact  H26      ..H29A     .       1.89 Ang.
                                                      x,y,z  =      1_555 Check

H atoms added using HFIX

910_ALERT_3_B Missing # of FCF Reflection(s) Below Theta(Min).         11 Note

Noted

#===============================================================================
077_ALERT_4_C Unitcell Contains Non-integer Number of Atoms ..     Please Check

Disorder, see above.

410_ALERT_2_C Short Intra H...H Contact  H22      ..H31A     .       1.95 Ang.
                                                      x,y,z  =      1_555 Check

H atoms added using HFIX


906_ALERT_3_C Large K Value in the Analysis of Variance ......      7.232 Check
#===============================================================================
;
_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. Shared sites
{C25, C25A}
3. Uiso/Uaniso restraints and constraints
Uanis(C25) = Uanis(C25A)
4. Others
 Sof(Br3A)=Sof(C25A)=1-FVAR(1)
 Sof(C25)=Sof(H25)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B), C33(H33A,H33B)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26)
5.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Br1 Br 0.95191(6) 0.73475(4) 0.36291(2) 0.02515(12) Uani 1 1 d . . . . .
Br2 Br 0.76359(6) 1.13288(4) 0.94640(2) 0.02667(12) Uani 1 1 d . . . . .
Br3A Br 0.1302(15) 0.2225(11) 0.9847(5) 0.029(4) Uani 0.0408(19) 1 d . . P A 2
S1 S 0.50856(13) 0.35680(10) 0.68677(5) 0.0190(2) Uani 1 1 d . . . . .
C1 C 0.7149(5) 0.7312(4) 0.68214(19) 0.0148(8) Uani 1 1 d . . . . .
C2 C 0.6674(5) 0.6112(4) 0.66163(19) 0.0150(8) Uani 1 1 d . . . . .
C3 C 0.5781(5) 0.5074(4) 0.70814(19) 0.0157(8) Uani 1 1 d . . . . .
C4 C 0.5276(5) 0.5188(4) 0.77625(19) 0.0172(8) Uani 1 1 d . . . . .
C5 C 0.5780(5) 0.6397(4) 0.79693(19) 0.0152(8) Uani 1 1 d . . . . .
C6 C 0.6703(5) 0.7450(4) 0.74984(19) 0.0157(8) Uani 1 1 d . . . . .
C7 C 0.8134(5) 0.8260(4) 0.62185(18) 0.0152(8) Uani 1 1 d . . . . .
C8 C 0.8113(5) 0.7429(4) 0.56580(19) 0.0153(8) Uani 1 1 d . . . . .
C9 C 0.7230(5) 0.6191(4) 0.58920(19) 0.0150(8) Uani 1 1 d . . . . .
C10 C 0.5482(5) 0.6785(4) 0.86712(19) 0.0175(8) Uani 1 1 d . . . . .
C11 C 0.6349(5) 0.8177(4) 0.85395(19) 0.0161(8) Uani 1 1 d . . . . .
C12 C 0.7028(5) 0.8569(4) 0.7865(2) 0.0160(8) Uani 1 1 d . . . . .
C13 C 0.4074(5) 0.3047(4) 0.76866(19) 0.0172(8) Uani 1 1 d . . . . .
C14 C 0.4255(5) 0.3987(4) 0.81164(19) 0.0164(8) Uani 1 1 d . . . . .
C15 C 0.8826(5) 0.7775(4) 0.49901(19) 0.0161(8) Uani 1 1 d . . . . .
H15 H 0.946620 0.859553 0.483490 0.019 Uiso 1 1 calc R U . . .
C16 C 0.8582(5) 0.6894(4) 0.45530(19) 0.0169(8) Uani 1 1 d . . . . .
C17 C 0.7682(5) 0.5675(4) 0.4773(2) 0.0201(8) Uani 1 1 d . . . . .
H17 H 0.752815 0.509019 0.446196 0.024 Uiso 1 1 calc R U . . .
C18 C 0.7013(5) 0.5316(4) 0.54442(19) 0.0182(8) Uani 1 1 d . . . . .
H18 H 0.640874 0.447677 0.559996 0.022 Uiso 1 1 calc R U . . .
C19 C 0.6497(5) 0.8986(4) 0.9020(2) 0.0183(8) Uani 1 1 d . . . . .
H19 H 0.604119 0.869302 0.948115 0.022 Uiso 1 1 calc R U . . .
C20 C 0.7334(5) 1.0241(4) 0.8806(2) 0.0194(8) Uani 1 1 d . . . . .
C21 C 0.7977(5) 1.0688(4) 0.8137(2) 0.0184(8) Uani 1 1 d . . . . .
H21 H 0.852565 1.155828 0.800112 0.022 Uiso 1 1 calc R U . . .
C22 C 0.7818(5) 0.9860(4) 0.7663(2) 0.0186(8) Uani 1 1 d . . . . .
H22 H 0.824768 1.017077 0.720019 0.022 Uiso 1 1 calc R U . . .
C23 C 0.3172(5) 0.1821(4) 0.7902(2) 0.0210(8) Uani 1 1 d . . . . .
H23 H 0.308987 0.120091 0.759980 0.025 Uiso 1 1 calc R U . . .
C24 C 0.2408(5) 0.1526(4) 0.8557(2) 0.0217(9) Uani 1 1 d . . . . .
H24 H 0.178541 0.069579 0.871219 0.026 Uiso 1 1 calc R U . A 1
C25 C 0.2541(5) 0.2439(4) 0.8995(2) 0.0220(9) Uani 0.9592(19) 1 d . . P A 1
H25 H 0.200114 0.222978 0.944854 0.026 Uiso 0.9592(19) 1 calc R U P A 1
C25A C 0.2541(5) 0.2439(4) 0.8995(2) 0.0220(9) Uani 0.0408(19) 1 d . . P A 2
C26 C 0.3451(5) 0.3651(4) 0.8779(2) 0.0208(8) Uani 1 1 d . . . . .
H26 H 0.352832 0.426097 0.908653 0.025 Uiso 1 1 calc R U . A 1
C27 C 0.6518(5) 0.5652(4) 0.9232(2) 0.0199(8) Uani 1 1 d . . . . .
H27A H 0.631178 0.599754 0.966527 0.024 Uiso 1 1 calc R U . . .
H27B H 0.597009 0.473796 0.930356 0.024 Uiso 1 1 calc R U . . .
C28 C 0.8601(6) 0.5336(5) 0.9074(2) 0.0316(10) Uani 1 1 d . . . . .
H28A H 0.882651 0.497762 0.864992 0.047 Uiso 1 1 calc R U . . .
H28B H 0.914048 0.460234 0.945058 0.047 Uiso 1 1 calc R U . . .
H28C H 0.917120 0.622385 0.902224 0.047 Uiso 1 1 calc R U . . .
C29 C 0.3409(5) 0.7135(4) 0.8910(2) 0.0216(9) Uani 1 1 d . . . . .
H29A H 0.293144 0.622268 0.914473 0.026 Uiso 1 1 calc R U . . .
H29B H 0.332909 0.776034 0.924625 0.026 Uiso 1 1 calc R U . . .
C30 C 0.2182(5) 0.7885(4) 0.8329(2) 0.0268(10) Uani 1 1 d . . . . .
H30A H 0.278239 0.867318 0.803449 0.040 Uiso 1 1 calc R U . . .
H30B H 0.098795 0.827836 0.851930 0.040 Uiso 1 1 calc R U . . .
H30C H 0.198697 0.718666 0.806042 0.040 Uiso 1 1 calc R U . . .
C31 C 0.7071(5) 0.9790(4) 0.5987(2) 0.0194(8) Uani 1 1 d . . . . .
H31A H 0.728130 1.039497 0.630635 0.023 Uiso 1 1 calc R U . . .
H31B H 0.759145 1.023186 0.552862 0.023 Uiso 1 1 calc R U . . .
C32 C 0.4993(6) 0.9816(5) 0.5954(2) 0.0314(10) Uani 1 1 d . . . . .
H32A H 0.476656 0.916184 0.566665 0.047 Uiso 1 1 calc R U . . .
H32B H 0.444325 1.080059 0.575847 0.047 Uiso 1 1 calc R U . . .
H32C H 0.443530 0.950237 0.641588 0.047 Uiso 1 1 calc R U . . .
C33 C 1.0174(5) 0.8349(4) 0.6351(2) 0.0192(8) Uani 1 1 d . . . . .
H33A H 1.079464 0.883303 0.592006 0.023 Uiso 1 1 calc R U . . .
H33B H 1.017265 0.895837 0.668994 0.023 Uiso 1 1 calc R U . . .
C34 C 1.1281(6) 0.6902(4) 0.6607(2) 0.0272(10) Uani 1 1 d . . . . .
H34A H 1.125658 0.627724 0.628321 0.041 Uiso 1 1 calc R U . . .
H34B H 1.074220 0.645044 0.705440 0.041 Uiso 1 1 calc R U . . .
H34C H 1.256120 0.703972 0.665128 0.041 Uiso 1 1 calc R U . . .


_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.
;
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
Br1 C16 1.898(4) . ?
Br2 C20 1.900(3) . ?
Br3A C25A 1.847(10) . ?
S1 C3 1.745(3) . ?
S1 C13 1.739(4) . ?
C1 C2 1.400(5) . ?
C1 C6 1.400(5) . ?
C1 C7 1.533(5) . ?
C2 C3 1.395(5) . ?
C2 C9 1.463(5) . ?
C3 C4 1.409(5) . ?
C4 C5 1.417(5) . ?
C4 C14 1.472(5) . ?
C5 C6 1.422(5) . ?
C5 C10 1.526(5) . ?
C6 C12 1.482(5) . ?
C7 C8 1.518(5) . ?
C7 C31 1.550(5) . ?
C7 C33 1.559(5) . ?
C8 C9 1.399(5) . ?
C8 C15 1.381(5) . ?
C9 C18 1.391(5) . ?
C10 C11 1.517(5) . ?
C10 C27 1.549(6) . ?
C10 C29 1.561(5) . ?
C11 C12 1.390(5) . ?
C11 C19 1.385(5) . ?
C12 C22 1.401(5) . ?
C13 C14 1.405(5) . ?
C13 C23 1.393(5) . ?
C14 C26 1.394(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.384(5) . ?
C16 C17 1.387(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.378(5) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C19 C20 1.390(5) . ?
C20 C21 1.378(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.390(5) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C23 C24 1.367(5) . ?
C24 H24 0.9500 . ?
C24 C25 1.389(5) . ?
C24 C25A 1.389(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.386(5) . ?
C25A C26 1.386(5) . ?
C26 H26 0.9500 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.530(5) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.525(6) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.526(5) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.510(6) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?

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
C13 S1 C3 90.93(17) . . ?
C2 C1 C6 118.7(3) . . ?
C2 C1 C7 109.5(3) . . ?
C6 C1 C7 131.7(3) . . ?
C1 C2 C9 109.9(3) . . ?
C3 C2 C1 120.3(3) . . ?
C3 C2 C9 129.9(3) . . ?
C2 C3 S1 123.5(3) . . ?
C2 C3 C4 122.7(3) . . ?
C4 C3 S1 113.7(3) . . ?
C3 C4 C5 116.7(3) . . ?
C3 C4 C14 110.4(3) . . ?
C5 C4 C14 132.8(3) . . ?
C4 C5 C6 120.7(3) . . ?
C4 C5 C10 128.8(3) . . ?
C6 C5 C10 110.5(3) . . ?
C1 C6 C5 120.8(3) . . ?
C1 C6 C12 131.4(3) . . ?
C5 C6 C12 107.8(3) . . ?
C1 C7 C31 113.5(3) . . ?
C1 C7 C33 112.5(3) . . ?
C8 C7 C1 101.5(3) . . ?
C8 C7 C31 108.4(3) . . ?
C8 C7 C33 109.3(3) . . ?
C31 C7 C33 111.0(3) . . ?
C9 C8 C7 111.4(3) . . ?
C15 C8 C7 127.8(3) . . ?
C15 C8 C9 120.8(3) . . ?
C8 C9 C2 107.6(3) . . ?
C18 C9 C2 132.5(3) . . ?
C18 C9 C8 119.9(3) . . ?
C5 C10 C27 113.1(3) . . ?
C5 C10 C29 114.3(3) . . ?
C11 C10 C5 101.4(3) . . ?
C11 C10 C27 109.1(3) . . ?
C11 C10 C29 107.6(3) . . ?
C27 C10 C29 110.8(3) . . ?
C12 C11 C10 111.9(3) . . ?
C19 C11 C10 125.7(3) . . ?
C19 C11 C12 122.3(3) . . ?
C11 C12 C6 108.3(3) . . ?
C11 C12 C22 118.3(3) . . ?
C22 C12 C6 133.4(4) . . ?
C14 C13 S1 113.3(3) . . ?
C23 C13 S1 123.9(3) . . ?
C23 C13 C14 122.8(4) . . ?
C13 C14 C4 111.7(3) . . ?
C26 C14 C4 131.8(3) . . ?
C26 C14 C13 116.5(3) . . ?
C8 C15 H15 120.9 . . ?
C8 C15 C16 118.2(3) . . ?
C16 C15 H15 120.9 . . ?
C15 C16 Br1 119.4(3) . . ?
C15 C16 C17 121.8(3) . . ?
C17 C16 Br1 118.9(3) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 C16 119.7(3) . . ?
C18 C17 H17 120.1 . . ?
C9 C18 H18 120.2 . . ?
C17 C18 C9 119.5(3) . . ?
C17 C18 H18 120.2 . . ?
C11 C19 H19 121.1 . . ?
C11 C19 C20 117.8(4) . . ?
C20 C19 H19 121.1 . . ?
C19 C20 Br2 118.5(3) . . ?
C21 C20 Br2 119.8(3) . . ?
C21 C20 C19 121.7(3) . . ?
C20 C21 H21 120.2 . . ?
C20 C21 C22 119.6(3) . . ?
C22 C21 H21 120.2 . . ?
C12 C22 H22 119.9 . . ?
C21 C22 C12 120.3(4) . . ?
C21 C22 H22 119.9 . . ?
C13 C23 H23 120.6 . . ?
C24 C23 C13 118.9(3) . . ?
C24 C23 H23 120.6 . . ?
C23 C24 H24 120.0 . . ?
C23 C24 C25 120.0(3) . . ?
C23 C24 C25A 120.0(3) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 119.6 . . ?
C26 C25 C24 120.8(4) . . ?
C26 C25 H25 119.6 . . ?
C24 C25A Br3A 122.0(4) . . ?
C26 C25A Br3A 116.8(4) . . ?
C26 C25A C24 120.8(4) . . ?
C14 C26 H26 119.5 . . ?
C25 C26 C14 120.9(3) . . ?
C25 C26 H26 119.5 . . ?
C25A C26 C14 120.9(3) . . ?
C10 C27 H27A 108.5 . . ?
C10 C27 H27B 108.5 . . ?
H27A C27 H27B 107.5 . . ?
C28 C27 C10 114.9(3) . . ?
C28 C27 H27A 108.5 . . ?
C28 C27 H27B 108.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C10 C29 H29A 108.8 . . ?
C10 C29 H29B 108.8 . . ?
H29A C29 H29B 107.7 . . ?
C30 C29 C10 113.8(3) . . ?
C30 C29 H29A 108.8 . . ?
C30 C29 H29B 108.8 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C7 C31 H31A 108.7 . . ?
C7 C31 H31B 108.7 . . ?
H31A C31 H31B 107.6 . . ?
C32 C31 C7 114.4(3) . . ?
C32 C31 H31A 108.7 . . ?
C32 C31 H31B 108.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C7 C33 H33A 108.7 . . ?
C7 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
C34 C33 C7 114.2(3) . . ?
C34 C33 H33A 108.7 . . ?
C34 C33 H33B 108.7 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 C16 C17 C18 179.1(3) . . . . ?
Br2 C20 C21 C22 177.5(3) . . . . ?
Br3A C25A C26 C14 -173.0(5) . . . . ?
S1 C3 C4 C5 -179.3(3) . . . . ?
S1 C3 C4 C14 -0.7(4) . . . . ?
S1 C13 C14 C4 -0.3(4) . . . . ?
S1 C13 C14 C26 179.0(3) . . . . ?
S1 C13 C23 C24 -179.2(3) . . . . ?
C1 C2 C3 S1 178.4(3) . . . . ?
C1 C2 C3 C4 1.6(6) . . . . ?
C1 C2 C9 C8 2.1(4) . . . . ?
C1 C2 C9 C18 -177.1(4) . . . . ?
C1 C6 C12 C11 -178.6(4) . . . . ?
C1 C6 C12 C22 2.3(7) . . . . ?
C1 C7 C8 C9 0.7(4) . . . . ?
C1 C7 C8 C15 -179.8(4) . . . . ?
C1 C7 C31 C32 -42.9(4) . . . . ?
C1 C7 C33 C34 49.1(4) . . . . ?
C2 C1 C6 C5 -0.2(5) . . . . ?
C2 C1 C6 C12 179.4(4) . . . . ?
C2 C1 C7 C8 0.6(4) . . . . ?
C2 C1 C7 C31 116.7(3) . . . . ?
C2 C1 C7 C33 -116.1(3) . . . . ?
C2 C3 C4 C5 -2.2(6) . . . . ?
C2 C3 C4 C14 176.4(3) . . . . ?
C2 C9 C18 C17 179.4(4) . . . . ?
C3 S1 C13 C14 -0.1(3) . . . . ?
C3 S1 C13 C23 -180.0(4) . . . . ?
C3 C2 C9 C8 -178.8(4) . . . . ?
C3 C2 C9 C18 2.0(7) . . . . ?
C3 C4 C5 C6 1.7(5) . . . . ?
C3 C4 C5 C10 -178.0(4) . . . . ?
C3 C4 C14 C13 0.6(5) . . . . ?
C3 C4 C14 C26 -178.6(4) . . . . ?
C4 C5 C6 C1 -0.5(6) . . . . ?
C4 C5 C6 C12 179.7(3) . . . . ?
C4 C5 C10 C11 179.5(4) . . . . ?
C4 C5 C10 C27 62.9(5) . . . . ?
C4 C5 C10 C29 -65.0(5) . . . . ?
C4 C14 C26 C25 179.7(4) . . . . ?
C4 C14 C26 C25A 179.7(4) . . . . ?
C5 C4 C14 C13 179.0(4) . . . . ?
C5 C4 C14 C26 -0.2(7) . . . . ?
C5 C6 C12 C11 1.1(4) . . . . ?
C5 C6 C12 C22 -178.0(4) . . . . ?
C5 C10 C11 C12 0.9(4) . . . . ?
C5 C10 C11 C19 -178.4(4) . . . . ?
C5 C10 C27 C28 55.6(4) . . . . ?
C5 C10 C29 C30 -34.2(4) . . . . ?
C6 C1 C2 C3 -0.3(5) . . . . ?
C6 C1 C2 C9 179.0(3) . . . . ?
C6 C1 C7 C8 179.9(4) . . . . ?
C6 C1 C7 C31 -64.0(5) . . . . ?
C6 C1 C7 C33 63.2(5) . . . . ?
C6 C5 C10 C11 -0.1(4) . . . . ?
C6 C5 C10 C27 -116.8(3) . . . . ?
C6 C5 C10 C29 115.3(3) . . . . ?
C6 C12 C22 C21 -178.4(4) . . . . ?
C7 C1 C2 C3 179.1(3) . . . . ?
C7 C1 C2 C9 -1.6(4) . . . . ?
C7 C1 C6 C5 -179.5(4) . . . . ?
C7 C1 C6 C12 0.2(7) . . . . ?
C7 C8 C9 C2 -1.7(4) . . . . ?
C7 C8 C9 C18 177.6(3) . . . . ?
C7 C8 C15 C16 -177.1(4) . . . . ?
C8 C7 C31 C32 69.1(4) . . . . ?
C8 C7 C33 C34 -62.9(4) . . . . ?
C8 C9 C18 C17 0.3(6) . . . . ?
C8 C15 C16 Br1 179.3(3) . . . . ?
C8 C15 C16 C17 -1.3(6) . . . . ?
C9 C2 C3 S1 -0.7(6) . . . . ?
C9 C2 C3 C4 -177.5(4) . . . . ?
C9 C8 C15 C16 2.4(5) . . . . ?
C10 C5 C6 C1 179.2(3) . . . . ?
C10 C5 C6 C12 -0.6(4) . . . . ?
C10 C11 C12 C6 -1.2(4) . . . . ?
C10 C11 C12 C22 178.0(3) . . . . ?
C10 C11 C19 C20 -179.9(4) . . . . ?
C11 C10 C27 C28 -56.5(4) . . . . ?
C11 C10 C29 C30 77.5(4) . . . . ?
C11 C12 C22 C21 2.5(5) . . . . ?
C11 C19 C20 Br2 -177.7(3) . . . . ?
C11 C19 C20 C21 0.9(6) . . . . ?
C12 C11 C19 C20 1.0(6) . . . . ?
C13 S1 C3 C2 -176.6(3) . . . . ?
C13 S1 C3 C4 0.5(3) . . . . ?
C13 C14 C26 C25 0.6(6) . . . . ?
C13 C14 C26 C25A 0.6(6) . . . . ?
C13 C23 C24 C25 -0.2(6) . . . . ?
C13 C23 C24 C25A -0.2(6) . . . . ?
C14 C4 C5 C6 -176.5(4) . . . . ?
C14 C4 C5 C10 3.8(7) . . . . ?
C14 C13 C23 C24 0.9(6) . . . . ?
C15 C8 C9 C2 178.8(3) . . . . ?
C15 C8 C9 C18 -1.9(5) . . . . ?
C15 C16 C17 C18 -0.3(6) . . . . ?
C16 C17 C18 C9 0.7(6) . . . . ?
C19 C11 C12 C6 178.0(3) . . . . ?
C19 C11 C12 C22 -2.7(6) . . . . ?
C19 C20 C21 C22 -1.1(6) . . . . ?
C20 C21 C22 C12 -0.7(6) . . . . ?
C23 C13 C14 C4 179.6(3) . . . . ?
C23 C13 C14 C26 -1.1(6) . . . . ?
C23 C24 C25 C26 -0.3(6) . . . . ?
C23 C24 C25A Br3A 172.4(5) . . . . ?
C23 C24 C25A C26 -0.3(6) . . . . ?
C24 C25 C26 C14 0.1(6) . . . . ?
C24 C25A C26 C14 0.1(6) . . . . ?
C27 C10 C11 C12 120.4(3) . . . . ?
C27 C10 C11 C19 -58.9(5) . . . . ?
C27 C10 C29 C30 -163.3(3) . . . . ?
C29 C10 C11 C12 -119.4(3) . . . . ?
C29 C10 C11 C19 61.4(5) . . . . ?
C29 C10 C27 C28 -174.7(3) . . . . ?
C31 C7 C8 C9 -119.1(3) . . . . ?
C31 C7 C8 C15 60.4(5) . . . . ?
C31 C7 C33 C34 177.6(3) . . . . ?
C33 C7 C8 C9 119.7(3) . . . . ?
C33 C7 C8 C15 -60.7(5) . . . . ?
C33 C7 C31 C32 -170.9(3) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil.'
_olex2_submission_original_sample_id BrTxS
_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 3.530
_oxdiff_exptl_absorpt_empirical_full_min 0.538
####################################################################### 
# 
# 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_nr20003
_database_code_depnum_ccdc_archive 'CCDC 2235429'
loop_
_audit_author_name
_audit_author_address
'Gary Stephen Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-01-10 deposited with the CCDC.	2023-03-19 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_nr20003             
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Synchrotron data, weak, cut at 1.2 A resolution.
;
_vrf_PLAT088_nr20003             
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.05 Note
RESPONSE: Synchrotron data, weak, cut at 1.2 A resolution.
;
_vrf_PLAT340_nr20003             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01676 Ang.
RESPONSE: Consequence of weak data.
;
_vrf_PLAT410_nr20003             
;
PROBLEM: Short Intra H...H Contact  H22      ..H31A     .       1.89 Ang.
RESPONSE: H atoms were added according to geometry of the parent atom.
;
_vrf_PLAT220_nr20003             
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        3.4 Ratio
RESPONSE: Synchrotron data, weak, cut at 1.2 A resolution.
;
_vrf_PLAT234_nr20003             
;
PROBLEM: Large Hirshfeld Difference O1       --C59      .       0.24 Ang.
RESPONSE: Synchrotron data, weak, cut at 1.2 A resolution.
;
_vrf_PLAT241_nr20003             
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         N1 Check
RESPONSE: Synchrotron data, weak, cut at 1.2 A resolution.
;
_vrf_PLAT242_nr20003             
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C27 Check
RESPONSE: Synchrotron data, weak, cut at 1.2 A resolution.
;
_vrf_PLAT260_nr20003             
;
PROBLEM: Large Average Ueq of Residue Including        S1      0.102 Check
RESPONSE: Synchrotron data, weak, cut at 1.2 A resolution.
;
_vrf_PLAT410_nr20003_2           
;
PROBLEM: Short Intra H...H Contact  H26      ..H27B     .       1.96 Ang.
RESPONSE: Synchrotron data, weak, cut at 1.2 A resolution.
;
_vrf_PLAT906_nr20003             
;
PROBLEM: Large K Value in the Analysis of Variance ......      5.396 Check
RESPONSE: Synchrotron data, weak, cut at 1.2 A resolution.
;
_vrf_PLAT911_nr20003             
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.419         27 Report
RESPONSE: Synchrotron data, weak, cut at 1.2 A resolution.
;
# Added during the CSD deposition process: Tuesday 10 January 2023 03:12 PM
# end Validation Reply Form

_audit_creation_date             2020-10-19
_audit_creation_method           
;
Olex2 1.3-beta
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
g.s.nichol@ed.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C62 H58 N2 O4 S, 1[CH2Cl2]'
_chemical_formula_sum            'C63 H60 Cl2 N2 O4 S'
_chemical_formula_weight         1012.09
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0032 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1418 0.1507 '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'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0108 0.0057 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1181 0.1169 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.771(3)
_cell_length_b                   25.909(4)
_cell_length_c                   11.8177(17)
_cell_angle_alpha                90
_cell_angle_beta                 106.224(3)
_cell_angle_gamma                90
_cell_volume                     5224.6(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8427
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      16.715
_cell_measurement_theta_min      2.313
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.5626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1694 before and 0.1151 after correction.
The Ratio of minimum to maximum transmission is 0.7562.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2136
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of ethanol and dichloromethane  by solvent layering'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.012
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            25408
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        16.770
_diffrn_reflns_theta_max         16.770
_diffrn_reflns_theta_min         1.157
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS_2M_S_N_24_0107_Diamond
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Diamond Light Source I-19 EH1'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_source                   Synchrotron
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2347
_reflns_number_total             3183
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         3183
_refine_ls_number_restraints     588
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0889
_refine_ls_restrained_S_all      0.980
_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)+(0.1522P)²+10.2651P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2415
_refine_ls_wR_factor_ref         0.2544
_refine_special_details          
;
The data set was cut at 1.2 A during integration due to rising values of R(merge) at higher resolution.  One molecule of solvent dichloromethane was handled using the solvent masking routine of Olex2.


#===============================================================================
#>>> The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text

023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6]..       0.42 Ang-1
088_ALERT_3_A Poor Data / Parameter Ratio ....................       5.05 Note

Weak data from a synchrotron source, cut at 1.2 A resolution.

#===============================================================================
340_ALERT_3_B Low Bond Precision on  C-C Bonds ...............    0.01676 Ang.

Consequence of weak data.

410_ALERT_2_B Short Intra H...H Contact  H22      ..H31A     .       1.89 Ang.
                                                      x,y,z  =      1_555 Check

H atoms were added according to geometry of the parent atom.

#===============================================================================
220_ALERT_2_C NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        3.4 Ratio
234_ALERT_4_C Large Hirshfeld Difference O1       --C59      .       0.24 Ang.
234_ALERT_4_C Large Hirshfeld Difference O2       --C60      .       0.19 Ang.
241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of         N1 Check
241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of        C44 Check
241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of        C48 Check
242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        C27 Check
242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        C35 Check
242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        C36 Check
242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        C45 Check
260_ALERT_2_C Large Average Ueq of Residue Including        S1      0.102 Check
410_ALERT_2_C Short Intra H...H Contact  H26      ..H27B     .       1.96 Ang.
                                                      x,y,z  =      1_555 Check
906_ALERT_3_C Large K Value in the Analysis of Variance ......      5.396 Check
911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.419         27 Report

Most of these are a consequence of the weak data.  A global RIGU was applied.

#===============================================================================
;
_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 body (RIGU) restrains
 S1, C3, C13, C2, C4, C14, C23, C1, C9, C5, C26, C24, C6, C7, C8, C18, C10,
 C25, C12, C31, C33, C15, C17, C11, C27, C29, C22, C32, C34, C16, C19, C28, C30,
  C21, N2, C20, C37, C38, N1, C49, C53, C54, C58, C35, C36, C50, C52, C55, C57,
 C44, C48, C39, C43, C51, C56, C45, C47, C40, C42, O3, O4, C46, C41, C61, C62,
 O2, O1, C60, C59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B), C33(H33A,H33B)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44),
  C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53),
 C54(H54), C55(H55), C57(H57), C58(H58)
3.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,
 H62B,H62C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.04945(15) 0.44018(9) 0.1213(2) 0.0734(9) Uani 1 1 d . . . . .
O1 O 0.5090(8) 0.0573(5) 0.2835(12) 0.198(5) Uani 1 1 d . . . . .
O2 O 0.8383(6) 0.3230(4) 0.7469(10) 0.152(3) Uani 1 1 d . . . . .
O3 O 0.2211(5) 0.5815(3) 1.1228(8) 0.126(3) Uani 1 1 d . . . . .
O4 O -0.0573(4) 0.7577(2) 0.4224(6) 0.092(2) Uani 1 1 d . . . . .
N1 N 0.5528(6) 0.2545(4) 0.4597(10) 0.129(4) Uani 1 1 d . . . . .
N2 N 0.1017(5) 0.5818(3) 0.6354(7) 0.082(3) Uani 1 1 d . . . . .
C1 C 0.2384(6) 0.4134(4) 0.3984(9) 0.074(3) Uani 1 1 d . . . . .
C2 C 0.1669(6) 0.4331(3) 0.3301(9) 0.063(2) Uani 1 1 d . . . . .
C3 C 0.1377(5) 0.4181(3) 0.2113(8) 0.060(2) Uani 1 1 d . . . . .
C4 C 0.1777(6) 0.3834(3) 0.1584(8) 0.063(2) Uani 1 1 d . . . . .
C5 C 0.2488(6) 0.3631(3) 0.2270(9) 0.069(3) Uani 1 1 d . . . . .
C6 C 0.2787(6) 0.3774(4) 0.3475(9) 0.076(3) Uani 1 1 d . . . . .
C7 C 0.2567(7) 0.4366(4) 0.5264(9) 0.086(3) Uani 1 1 d . . . . .
C8 C 0.1904(6) 0.4752(4) 0.5086(9) 0.077(3) Uani 1 1 d . . . . .
C9 C 0.1370(6) 0.4701(4) 0.3960(8) 0.069(3) Uani 1 1 d . . . . .
C10 C 0.3045(6) 0.3253(4) 0.1935(9) 0.077(3) Uani 1 1 d . . . . .
C11 C 0.3685(7) 0.3197(4) 0.3078(10) 0.088(3) Uani 1 1 d . . . . .
C12 C 0.3532(6) 0.3498(4) 0.3955(10) 0.093(3) Uani 1 1 d . . . . .
C13 C 0.0639(6) 0.4057(3) 0.0048(8) 0.062(3) Uani 1 1 d . . . . .
C14 C 0.1313(6) 0.3762(3) 0.0308(8) 0.063(2) Uani 1 1 d . . . . .
C15 C 0.1791(6) 0.5113(4) 0.5868(8) 0.079(3) Uani 1 1 d . . . . .
H15 H 0.216613 0.515257 0.661341 0.095 Uiso 1 1 calc R U . . .
C16 C 0.1130(7) 0.5420(4) 0.5572(9) 0.075(3) Uani 1 1 d . . . . .
C17 C 0.0577(6) 0.5358(3) 0.4491(8) 0.072(3) Uani 1 1 d . . . . .
H17 H 0.010974 0.555707 0.431042 0.086 Uiso 1 1 calc R U . . .
C18 C 0.0700(6) 0.5010(3) 0.3674(8) 0.069(3) Uani 1 1 d . . . . .
H18 H 0.032966 0.498142 0.292182 0.083 Uiso 1 1 calc R U . . .
C19 C 0.4330(7) 0.2880(5) 0.3266(11) 0.115(4) Uani 1 1 d . . . . .
H19 H 0.441362 0.267903 0.264055 0.137 Uiso 1 1 calc R U . . .
C20 C 0.4863(8) 0.2858(5) 0.4395(12) 0.121(4) Uani 1 1 d . . . . .
C21 C 0.4688(8) 0.3133(5) 0.5272(11) 0.127(5) Uani 1 1 d . . . . .
H21 H 0.501934 0.309299 0.605118 0.152 Uiso 1 1 calc R U . . .
C22 C 0.4063(7) 0.3463(5) 0.5099(11) 0.119(4) Uani 1 1 d . . . . .
H22 H 0.398791 0.366445 0.573001 0.143 Uiso 1 1 calc R U . . .
C23 C 0.0127(6) 0.4076(4) -0.1088(9) 0.076(3) Uani 1 1 d . . . . .
H23 H -0.031762 0.429671 -0.125778 0.091 Uiso 1 1 calc R U . . .
C24 C 0.0274(7) 0.3773(4) -0.1960(9) 0.092(3) Uani 1 1 d . . . . .
H24 H -0.009051 0.376126 -0.272017 0.110 Uiso 1 1 calc R U . . .
C25 C 0.0957(7) 0.3486(4) -0.1722(9) 0.090(3) Uani 1 1 d . . . . .
H25 H 0.108074 0.329594 -0.233456 0.108 Uiso 1 1 calc R U . . .
C26 C 0.1456(6) 0.3475(3) -0.0597(9) 0.079(3) Uani 1 1 d . . . . .
H26 H 0.191098 0.326375 -0.043709 0.094 Uiso 1 1 calc R U . . .
C27 C 0.3407(6) 0.3479(4) 0.0986(9) 0.092(3) Uani 1 1 d . . . . .
H27A H 0.381058 0.323674 0.087017 0.111 Uiso 1 1 calc R U . . .
H27B H 0.299194 0.350458 0.022873 0.111 Uiso 1 1 calc R U . . .
C28 C 0.3773(8) 0.4000(4) 0.1297(13) 0.141(5) Uani 1 1 d . . . . .
H28A H 0.405947 0.409587 0.073112 0.212 Uiso 1 1 calc R U . . .
H28B H 0.413547 0.398875 0.209219 0.212 Uiso 1 1 calc R U . . .
H28C H 0.336183 0.425535 0.127278 0.212 Uiso 1 1 calc R U . . .
C29 C 0.2663(6) 0.2715(3) 0.1585(9) 0.080(3) Uani 1 1 d . . . . .
H29A H 0.220116 0.275714 0.089268 0.097 Uiso 1 1 calc R U . . .
H29B H 0.304288 0.249054 0.134655 0.097 Uiso 1 1 calc R U . . .
C30 C 0.2406(7) 0.2448(4) 0.2562(10) 0.107(4) Uani 1 1 d . . . . .
H30A H 0.218001 0.211002 0.228360 0.160 Uiso 1 1 calc R U . . .
H30B H 0.201178 0.265959 0.278133 0.160 Uiso 1 1 calc R U . . .
H30C H 0.285980 0.240085 0.325027 0.160 Uiso 1 1 calc R U . . .
C31 C 0.3329(7) 0.4636(4) 0.5643(10) 0.103(3) Uani 1 1 d . . . . .
H31A H 0.374874 0.437213 0.580549 0.124 Uiso 1 1 calc R U . . .
H31B H 0.336060 0.481456 0.639491 0.124 Uiso 1 1 calc R U . . .
C32 C 0.3494(7) 0.5019(4) 0.4808(10) 0.109(4) Uani 1 1 d . . . . .
H32A H 0.362960 0.483761 0.416342 0.164 Uiso 1 1 calc R U . . .
H32B H 0.393382 0.523836 0.522342 0.164 Uiso 1 1 calc R U . . .
H32C H 0.302914 0.523290 0.448653 0.164 Uiso 1 1 calc R U . . .
C33 C 0.2448(6) 0.3914(4) 0.6121(8) 0.091(3) Uani 1 1 d . . . . .
H33A H 0.190774 0.377815 0.582728 0.109 Uiso 1 1 calc R U . . .
H33B H 0.281386 0.362878 0.609679 0.109 Uiso 1 1 calc R U . . .
C34 C 0.2587(8) 0.4090(4) 0.7403(9) 0.117(4) Uani 1 1 d . . . . .
H34A H 0.216461 0.432324 0.745780 0.176 Uiso 1 1 calc R U . . .
H34B H 0.309042 0.427007 0.766457 0.176 Uiso 1 1 calc R U . . .
H34C H 0.259404 0.378787 0.790604 0.176 Uiso 1 1 calc R U . . .
C35 C 0.6249(8) 0.2714(6) 0.5382(13) 0.118(4) Uani 1 1 d . . . . .
C36 C 0.5444(7) 0.2054(5) 0.4118(11) 0.098(3) Uani 1 1 d . . . . .
C37 C 0.1320(6) 0.5782(4) 0.7561(9) 0.074(3) Uani 1 1 d . . . . .
C38 C 0.0629(7) 0.6276(4) 0.5820(8) 0.074(3) Uani 1 1 d . . . . .
C39 C 0.4811(9) 0.1739(7) 0.4048(12) 0.133(5) Uani 1 1 d . . . . .
H39 H 0.440668 0.187631 0.434202 0.160 Uiso 1 1 calc R U . . .
C40 C 0.4705(10) 0.1272(7) 0.3618(15) 0.149(5) Uani 1 1 d . . . . .
H40 H 0.424716 0.107564 0.357966 0.179 Uiso 1 1 calc R U . . .
C41 C 0.5303(13) 0.1091(8) 0.3234(16) 0.164(6) Uani 1 1 d . . . . .
C42 C 0.5989(9) 0.1352(6) 0.3221(13) 0.144(5) Uani 1 1 d . . . . .
H42 H 0.638221 0.119925 0.292575 0.173 Uiso 1 1 calc R U . . .
C43 C 0.6053(7) 0.1850(5) 0.3671(12) 0.127(4) Uani 1 1 d . . . . .
H43 H 0.649806 0.205456 0.368112 0.153 Uiso 1 1 calc R U . . .
C44 C 0.6672(9) 0.2398(6) 0.6272(14) 0.149(5) Uani 1 1 d . . . . .
H44 H 0.647527 0.206527 0.637242 0.179 Uiso 1 1 calc R U . . .
C45 C 0.7393(8) 0.2563(5) 0.7038(12) 0.122(4) Uani 1 1 d . . . . .
H45 H 0.769197 0.235990 0.767583 0.147 Uiso 1 1 calc R U . . .
C46 C 0.7624(10) 0.3047(7) 0.6769(15) 0.134(5) Uani 1 1 d . . . . .
C47 C 0.7218(10) 0.3359(6) 0.5942(16) 0.139(5) Uani 1 1 d . . . . .
H47 H 0.742330 0.369047 0.585387 0.167 Uiso 1 1 calc R U . . .
C48 C 0.6523(10) 0.3219(7) 0.5221(16) 0.155(5) Uani 1 1 d . . . . .
H48 H 0.622696 0.344572 0.463121 0.186 Uiso 1 1 calc R U . . .
C49 C 0.1361(5) 0.5321(4) 0.8189(9) 0.082(3) Uani 1 1 d . . . . .
H49 H 0.118858 0.500978 0.777265 0.098 Uiso 1 1 calc R U . . .
C50 C 0.1649(6) 0.5307(4) 0.9408(10) 0.094(3) Uani 1 1 d . . . . .
H50 H 0.168450 0.499151 0.982845 0.112 Uiso 1 1 calc R U . . .
C51 C 0.1884(7) 0.5773(5) 0.9999(12) 0.106(4) Uani 1 1 d . . . . .
C52 C 0.1857(7) 0.6224(5) 0.9405(11) 0.099(4) Uani 1 1 d . . . . .
H52 H 0.204540 0.653431 0.981556 0.119 Uiso 1 1 calc R U . . .
C53 C 0.1565(6) 0.6226(4) 0.8249(10) 0.087(3) Uani 1 1 d . . . . .
H53 H 0.151664 0.654917 0.785498 0.104 Uiso 1 1 calc R U . . .
C54 C -0.0094(6) 0.6426(4) 0.5994(8) 0.076(3) Uani 1 1 d . . . . .
H54 H -0.033165 0.622480 0.647223 0.091 Uiso 1 1 calc R U . . .
C55 C -0.0447(6) 0.6869(4) 0.5456(8) 0.077(3) Uani 1 1 d . . . . .
H55 H -0.092365 0.697667 0.559829 0.093 Uiso 1 1 calc R U . . .
C56 C -0.0150(7) 0.7156(4) 0.4743(8) 0.070(3) Uani 1 1 d . . . . .
C57 C 0.0558(6) 0.7003(4) 0.4552(9) 0.081(3) Uani 1 1 d . . . . .
H57 H 0.077871 0.720004 0.404601 0.097 Uiso 1 1 calc R U . . .
C58 C 0.0939(6) 0.6564(4) 0.5099(8) 0.083(3) Uani 1 1 d . . . . .
H58 H 0.142239 0.646390 0.496897 0.100 Uiso 1 1 calc R U . . .
C59 C 0.5590(10) 0.0407(8) 0.2357(14) 0.203(8) Uani 1 1 d . . . . .
H59A H 0.573477 0.068270 0.189029 0.304 Uiso 1 1 calc R U . . .
H59B H 0.536832 0.011612 0.184080 0.304 Uiso 1 1 calc R U . . .
H59C H 0.605600 0.029197 0.296594 0.304 Uiso 1 1 calc R U . . .
C60 C 0.8786(9) 0.2910(6) 0.8421(11) 0.155(6) Uani 1 1 d . . . . .
H60A H 0.890535 0.257758 0.811510 0.232 Uiso 1 1 calc R U . . .
H60B H 0.845572 0.285334 0.894932 0.232 Uiso 1 1 calc R U . . .
H60C H 0.927498 0.307839 0.885644 0.232 Uiso 1 1 calc R U . . .
C61 C 0.2153(8) 0.5390(5) 1.1846(12) 0.136(5) Uani 1 1 d . . . . .
H61A H 0.256035 0.514313 1.179675 0.204 Uiso 1 1 calc R U . . .
H61B H 0.163579 0.523332 1.152020 0.204 Uiso 1 1 calc R U . . .
H61C H 0.222029 0.548328 1.267200 0.204 Uiso 1 1 calc R U . . .
C62 C -0.0255(7) 0.7867(4) 0.3437(9) 0.102(4) Uani 1 1 d . . . . .
H62A H -0.020602 0.764342 0.279183 0.154 Uiso 1 1 calc R U . . .
H62B H 0.026272 0.799907 0.386501 0.154 Uiso 1 1 calc R U . . .
H62C H -0.060383 0.815628 0.311426 0.154 Uiso 1 1 calc R U . . .


_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.
;
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 C3 1.728(10) . ?
S1 C13 1.720(9) . ?
O1 C41 1.44(2) . ?
O1 C59 1.254(15) . ?
O2 C46 1.450(18) . ?
O2 C60 1.419(14) . ?
O3 C51 1.411(14) . ?
O3 C61 1.341(12) . ?
O4 C56 1.370(11) . ?
O4 C62 1.429(11) . ?
N1 C20 1.397(14) . ?
N1 C35 1.424(16) . ?
N1 C36 1.385(14) . ?
N2 C16 1.436(11) . ?
N2 C37 1.380(12) . ?
N2 C38 1.429(11) . ?
C1 C2 1.397(12) . ?
C1 C6 1.408(12) . ?
C1 C7 1.575(13) . ?
C2 C3 1.409(12) . ?
C2 C9 1.427(12) . ?
C3 C4 1.398(11) . ?
C4 C5 1.398(12) . ?
C4 C14 1.515(12) . ?
C5 C6 1.424(12) . ?
C5 C10 1.521(12) . ?
C6 C12 1.472(13) . ?
C7 C8 1.514(13) . ?
C7 C31 1.477(14) . ?
C7 C33 1.601(13) . ?
C8 C9 1.408(12) . ?
C8 C15 1.370(12) . ?
C9 C18 1.396(12) . ?
C10 C11 1.510(13) . ?
C10 C27 1.554(13) . ?
C10 C29 1.555(13) . ?
C11 C12 1.384(13) . ?
C11 C19 1.376(13) . ?
C12 C22 1.418(14) . ?
C13 C14 1.380(12) . ?
C13 C23 1.396(12) . ?
C14 C26 1.385(12) . ?
C15 H15 0.9500 . ?
C15 C16 1.379(13) . ?
C16 C17 1.385(13) . ?
C17 H17 0.9500 . ?
C17 C18 1.382(11) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C19 C20 1.405(15) . ?
C20 C21 1.363(15) . ?
C21 H21 0.9500 . ?
C21 C22 1.371(14) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C23 C24 1.379(12) . ?
C24 H24 0.9500 . ?
C24 C25 1.383(13) . ?
C25 H25 0.9500 . ?
C25 C26 1.378(13) . ?
C26 H26 0.9500 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.499(13) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.523(12) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.486(13) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.534(13) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C44 1.378(18) . ?
C35 C48 1.429(19) . ?
C36 C39 1.372(16) . ?
C36 C43 1.431(15) . ?
C37 C49 1.398(13) . ?
C37 C53 1.406(13) . ?
C38 C54 1.411(13) . ?
C38 C58 1.360(12) . ?
C39 H39 0.9500 . ?
C39 C40 1.307(19) . ?
C40 H40 0.9500 . ?
C40 C41 1.35(2) . ?
C41 C42 1.40(2) . ?
C42 H42 0.9500 . ?
C42 C43 1.389(16) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C44 C45 1.413(17) . ?
C45 H45 0.9500 . ?
C45 C46 1.386(19) . ?
C46 C47 1.316(19) . ?
C47 H47 0.9500 . ?
C47 C48 1.339(18) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C49 C50 1.388(13) . ?
C50 H50 0.9500 . ?
C50 C51 1.399(15) . ?
C51 C52 1.357(15) . ?
C52 H52 0.9500 . ?
C52 C53 1.318(13) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C54 C55 1.376(12) . ?
C55 H55 0.9500 . ?
C55 C56 1.338(12) . ?
C56 C57 1.395(13) . ?
C57 H57 0.9500 . ?
C57 C58 1.388(12) . ?
C58 H58 0.9500 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?

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
C13 S1 C3 90.5(5) . . ?
C59 O1 C41 108.3(18) . . ?
C60 O2 C46 116.4(13) . . ?
C61 O3 C51 115.2(11) . . ?
C56 O4 C62 116.2(8) . . ?
C20 N1 C35 119.8(10) . . ?
C36 N1 C20 118.3(11) . . ?
C36 N1 C35 121.5(11) . . ?
C37 N2 C16 122.2(8) . . ?
C37 N2 C38 120.9(8) . . ?
C38 N2 C16 116.8(8) . . ?
C2 C1 C6 119.0(9) . . ?
C2 C1 C7 108.9(8) . . ?
C6 C1 C7 132.0(9) . . ?
C1 C2 C3 119.8(9) . . ?
C1 C2 C9 110.4(9) . . ?
C3 C2 C9 129.7(9) . . ?
C2 C3 S1 122.8(7) . . ?
C4 C3 S1 115.2(7) . . ?
C4 C3 C2 122.1(9) . . ?
C3 C4 C5 118.3(8) . . ?
C3 C4 C14 108.7(9) . . ?
C5 C4 C14 133.1(9) . . ?
C4 C5 C6 120.3(9) . . ?
C4 C5 C10 129.8(9) . . ?
C6 C5 C10 109.9(9) . . ?
C1 C6 C5 120.5(9) . . ?
C1 C6 C12 131.9(9) . . ?
C5 C6 C12 107.6(9) . . ?
C1 C7 C33 107.4(7) . . ?
C8 C7 C1 100.1(8) . . ?
C8 C7 C33 109.6(8) . . ?
C31 C7 C1 113.4(9) . . ?
C31 C7 C8 110.0(8) . . ?
C31 C7 C33 115.2(9) . . ?
C9 C8 C7 111.2(9) . . ?
C15 C8 C7 127.8(9) . . ?
C15 C8 C9 121.0(9) . . ?
C8 C9 C2 108.8(9) . . ?
C18 C9 C2 132.5(9) . . ?
C18 C9 C8 118.6(9) . . ?
C5 C10 C27 112.2(8) . . ?
C5 C10 C29 112.2(8) . . ?
C11 C10 C5 102.2(8) . . ?
C11 C10 C27 108.8(9) . . ?
C11 C10 C29 108.3(8) . . ?
C27 C10 C29 112.5(8) . . ?
C12 C11 C10 111.0(9) . . ?
C19 C11 C10 126.0(10) . . ?
C19 C11 C12 122.9(11) . . ?
C11 C12 C6 109.2(10) . . ?
C11 C12 C22 117.4(10) . . ?
C22 C12 C6 133.3(10) . . ?
C14 C13 S1 115.0(7) . . ?
C14 C13 C23 121.7(9) . . ?
C23 C13 S1 123.2(8) . . ?
C13 C14 C4 110.6(8) . . ?
C13 C14 C26 117.4(9) . . ?
C26 C14 C4 131.9(9) . . ?
C8 C15 H15 120.1 . . ?
C8 C15 C16 119.8(10) . . ?
C16 C15 H15 120.1 . . ?
C15 C16 N2 120.8(10) . . ?
C15 C16 C17 120.1(9) . . ?
C17 C16 N2 119.0(9) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 C16 120.6(9) . . ?
C18 C17 H17 119.7 . . ?
C9 C18 H18 120.1 . . ?
C17 C18 C9 119.7(9) . . ?
C17 C18 H18 120.1 . . ?
C11 C19 H19 120.4 . . ?
C11 C19 C20 119.2(11) . . ?
C20 C19 H19 120.4 . . ?
N1 C20 C19 120.0(11) . . ?
C21 C20 N1 122.3(12) . . ?
C21 C20 C19 117.6(11) . . ?
C20 C21 H21 118.0 . . ?
C20 C21 C22 124.0(12) . . ?
C22 C21 H21 118.0 . . ?
C12 C22 H22 120.7 . . ?
C21 C22 C12 118.5(11) . . ?
C21 C22 H22 120.7 . . ?
C13 C23 H23 120.3 . . ?
C24 C23 C13 119.3(9) . . ?
C24 C23 H23 120.3 . . ?
C23 C24 H24 120.2 . . ?
C23 C24 C25 119.6(10) . . ?
C25 C24 H24 120.2 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 C24 119.9(10) . . ?
C26 C25 H25 120.0 . . ?
C14 C26 H26 119.1 . . ?
C25 C26 C14 121.8(10) . . ?
C25 C26 H26 119.1 . . ?
C10 C27 H27A 108.9 . . ?
C10 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
C28 C27 C10 113.5(9) . . ?
C28 C27 H27A 108.9 . . ?
C28 C27 H27B 108.9 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C10 C29 H29A 108.7 . . ?
C10 C29 H29B 108.7 . . ?
H29A C29 H29B 107.6 . . ?
C30 C29 C10 114.1(8) . . ?
C30 C29 H29A 108.7 . . ?
C30 C29 H29B 108.7 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C7 C31 H31A 108.1 . . ?
C7 C31 H31B 108.1 . . ?
C7 C31 C32 116.7(10) . . ?
H31A C31 H31B 107.3 . . ?
C32 C31 H31A 108.1 . . ?
C32 C31 H31B 108.1 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C7 C33 H33A 108.9 . . ?
C7 C33 H33B 108.9 . . ?
H33A C33 H33B 107.7 . . ?
C34 C33 C7 113.2(8) . . ?
C34 C33 H33A 108.9 . . ?
C34 C33 H33B 108.9 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N1 C35 C48 118.2(16) . . ?
C44 C35 N1 121.0(15) . . ?
C44 C35 C48 120.8(16) . . ?
N1 C36 C43 119.0(12) . . ?
C39 C36 N1 124.3(13) . . ?
C39 C36 C43 116.8(13) . . ?
N2 C37 C49 123.7(10) . . ?
N2 C37 C53 120.7(9) . . ?
C49 C37 C53 115.5(10) . . ?
C54 C38 N2 120.7(10) . . ?
C58 C38 N2 120.1(10) . . ?
C58 C38 C54 119.1(10) . . ?
C36 C39 H39 116.6 . . ?
C40 C39 C36 126.8(17) . . ?
C40 C39 H39 116.6 . . ?
C39 C40 H40 122.8 . . ?
C39 C40 C41 114(2) . . ?
C41 C40 H40 122.8 . . ?
C40 C41 O1 106(2) . . ?
C40 C41 C42 127(2) . . ?
C42 C41 O1 127(2) . . ?
C41 C42 H42 122.5 . . ?
C43 C42 C41 115.1(15) . . ?
C43 C42 H42 122.5 . . ?
C36 C43 H43 120.2 . . ?
C42 C43 C36 119.7(13) . . ?
C42 C43 H43 120.2 . . ?
C35 C44 H44 119.6 . . ?
C35 C44 C45 120.9(16) . . ?
C45 C44 H44 119.6 . . ?
C44 C45 H45 123.2 . . ?
C46 C45 C44 113.6(15) . . ?
C46 C45 H45 123.2 . . ?
C45 C46 O2 116.9(16) . . ?
C47 C46 O2 117.0(18) . . ?
C47 C46 C45 126.2(19) . . ?
C46 C47 H47 119.2 . . ?
C46 C47 C48 121.5(19) . . ?
C48 C47 H47 119.2 . . ?
C35 C48 H48 121.6 . . ?
C47 C48 C35 116.8(18) . . ?
C47 C48 H48 121.6 . . ?
C37 C49 H49 119.2 . . ?
C50 C49 C37 121.5(10) . . ?
C50 C49 H49 119.2 . . ?
C49 C50 H50 121.1 . . ?
C49 C50 C51 117.9(11) . . ?
C51 C50 H50 121.1 . . ?
C50 C51 O3 124.1(12) . . ?
C52 C51 O3 114.3(12) . . ?
C52 C51 C50 121.5(12) . . ?
C51 C52 H52 120.5 . . ?
C53 C52 C51 119.1(12) . . ?
C53 C52 H52 120.5 . . ?
C37 C53 H53 117.8 . . ?
C52 C53 C37 124.4(11) . . ?
C52 C53 H53 117.8 . . ?
C38 C54 H54 120.7 . . ?
C55 C54 C38 118.6(10) . . ?
C55 C54 H54 120.7 . . ?
C54 C55 H55 118.5 . . ?
C56 C55 C54 123.0(10) . . ?
C56 C55 H55 118.5 . . ?
O4 C56 C57 124.1(10) . . ?
C55 C56 O4 117.4(10) . . ?
C55 C56 C57 118.5(10) . . ?
C56 C57 H57 120.0 . . ?
C58 C57 C56 120.1(10) . . ?
C58 C57 H57 120.0 . . ?
C38 C58 C57 120.7(10) . . ?
C38 C58 H58 119.6 . . ?
C57 C58 H58 119.6 . . ?
O1 C59 H59A 109.5 . . ?
O1 C59 H59B 109.5 . . ?
O1 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
O2 C60 H60A 109.5 . . ?
O2 C60 H60B 109.5 . . ?
O2 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
O3 C61 H61A 109.5 . . ?
O3 C61 H61B 109.5 . . ?
O3 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
O4 C62 H62A 109.5 . . ?
O4 C62 H62B 109.5 . . ?
O4 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C3 C4 C5 -178.6(7) . . . . ?
S1 C3 C4 C14 1.8(9) . . . . ?
S1 C13 C14 C4 -1.8(9) . . . . ?
S1 C13 C14 C26 179.7(6) . . . . ?
S1 C13 C23 C24 -177.7(7) . . . . ?
O1 C41 C42 C43 -179.4(15) . . . . ?
O2 C46 C47 C48 177.6(13) . . . . ?
O3 C51 C52 C53 179.6(10) . . . . ?
O4 C56 C57 C58 -178.7(8) . . . . ?
N1 C20 C21 C22 176.7(13) . . . . ?
N1 C35 C44 C45 178.9(12) . . . . ?
N1 C35 C48 C47 -177.3(13) . . . . ?
N1 C36 C39 C40 -179.2(15) . . . . ?
N1 C36 C43 C42 178.0(12) . . . . ?
N2 C16 C17 C18 174.3(8) . . . . ?
N2 C37 C49 C50 -178.0(9) . . . . ?
N2 C37 C53 C52 179.7(10) . . . . ?
N2 C38 C54 C55 -179.7(8) . . . . ?
N2 C38 C58 C57 178.3(8) . . . . ?
C1 C2 C3 S1 179.3(7) . . . . ?
C1 C2 C3 C4 0.4(13) . . . . ?
C1 C2 C9 C8 0.9(11) . . . . ?
C1 C2 C9 C18 178.3(10) . . . . ?
C1 C6 C12 C11 -178.1(10) . . . . ?
C1 C6 C12 C22 6(2) . . . . ?
C1 C7 C8 C9 7.2(10) . . . . ?
C1 C7 C8 C15 -173.1(10) . . . . ?
C1 C7 C31 C32 49.3(13) . . . . ?
C1 C7 C33 C34 -178.5(9) . . . . ?
C2 C1 C6 C5 2.6(13) . . . . ?
C2 C1 C6 C12 -179.4(10) . . . . ?
C2 C1 C7 C8 -6.5(10) . . . . ?
C2 C1 C7 C31 -123.7(10) . . . . ?
C2 C1 C7 C33 107.9(9) . . . . ?
C2 C3 C4 C5 0.4(12) . . . . ?
C2 C3 C4 C14 -179.2(7) . . . . ?
C2 C9 C18 C17 -176.8(9) . . . . ?
C3 S1 C13 C14 2.4(7) . . . . ?
C3 S1 C13 C23 -176.4(8) . . . . ?
C3 C2 C9 C8 -174.6(9) . . . . ?
C3 C2 C9 C18 2.8(16) . . . . ?
C3 C4 C5 C6 0.3(13) . . . . ?
C3 C4 C5 C10 -179.6(9) . . . . ?
C3 C4 C14 C13 0.0(10) . . . . ?
C3 C4 C14 C26 178.3(9) . . . . ?
C4 C5 C6 C1 -1.8(14) . . . . ?
C4 C5 C6 C12 179.7(8) . . . . ?
C4 C5 C10 C11 -179.7(9) . . . . ?
C4 C5 C10 C27 63.9(13) . . . . ?
C4 C5 C10 C29 -63.9(13) . . . . ?
C4 C14 C26 C25 -177.1(9) . . . . ?
C5 C4 C14 C13 -179.6(9) . . . . ?
C5 C4 C14 C26 -1.3(16) . . . . ?
C5 C6 C12 C11 0.1(12) . . . . ?
C5 C6 C12 C22 -175.8(12) . . . . ?
C5 C10 C11 C12 -0.3(11) . . . . ?
C5 C10 C11 C19 177.7(10) . . . . ?
C5 C10 C27 C28 51.9(12) . . . . ?
C5 C10 C29 C30 -60.6(11) . . . . ?
C6 C1 C2 C3 -1.9(13) . . . . ?
C6 C1 C2 C9 -177.9(8) . . . . ?
C6 C1 C7 C8 175.5(10) . . . . ?
C6 C1 C7 C31 58.4(14) . . . . ?
C6 C1 C7 C33 -70.0(13) . . . . ?
C6 C5 C10 C11 0.4(10) . . . . ?
C6 C5 C10 C27 -116.0(9) . . . . ?
C6 C5 C10 C29 116.2(9) . . . . ?
C6 C12 C22 C21 175.0(12) . . . . ?
C7 C1 C2 C3 179.8(8) . . . . ?
C7 C1 C2 C9 3.8(10) . . . . ?
C7 C1 C6 C5 -179.6(9) . . . . ?
C7 C1 C6 C12 -1.6(18) . . . . ?
C7 C8 C9 C2 -5.5(11) . . . . ?
C7 C8 C9 C18 176.6(8) . . . . ?
C7 C8 C15 C16 -177.2(9) . . . . ?
C8 C7 C31 C32 -61.8(12) . . . . ?
C8 C7 C33 C34 -70.6(11) . . . . ?
C8 C9 C18 C17 0.4(13) . . . . ?
C8 C15 C16 N2 -177.0(8) . . . . ?
C8 C15 C16 C17 0.8(14) . . . . ?
C9 C2 C3 S1 -5.5(13) . . . . ?
C9 C2 C3 C4 175.6(8) . . . . ?
C9 C8 C15 C16 2.5(14) . . . . ?
C10 C5 C6 C1 178.1(8) . . . . ?
C10 C5 C6 C12 -0.4(11) . . . . ?
C10 C11 C12 C6 0.1(12) . . . . ?
C10 C11 C12 C22 176.8(10) . . . . ?
C10 C11 C19 C20 -178.0(12) . . . . ?
C11 C10 C27 C28 -60.5(12) . . . . ?
C11 C10 C29 C30 51.4(11) . . . . ?
C11 C12 C22 C21 -0.7(18) . . . . ?
C11 C19 C20 N1 -179.0(11) . . . . ?
C11 C19 C20 C21 4(2) . . . . ?
C12 C11 C19 C20 -0.2(19) . . . . ?
C13 S1 C3 C2 178.6(7) . . . . ?
C13 S1 C3 C4 -2.4(7) . . . . ?
C13 C14 C26 C25 1.1(13) . . . . ?
C13 C23 C24 C25 -5.1(14) . . . . ?
C14 C4 C5 C6 179.8(9) . . . . ?
C14 C4 C5 C10 -0.1(17) . . . . ?
C14 C13 C23 C24 3.6(14) . . . . ?
C15 C8 C9 C2 174.8(8) . . . . ?
C15 C8 C9 C18 -3.1(14) . . . . ?
C15 C16 C17 C18 -3.5(14) . . . . ?
C16 N2 C37 C49 -36.9(14) . . . . ?
C16 N2 C37 C53 147.2(10) . . . . ?
C16 N2 C38 C54 117.8(10) . . . . ?
C16 N2 C38 C58 -59.7(12) . . . . ?
C16 C17 C18 C9 2.9(13) . . . . ?
C19 C11 C12 C6 -178.0(10) . . . . ?
C19 C11 C12 C22 -1.4(17) . . . . ?
C19 C20 C21 C22 -6(2) . . . . ?
C20 N1 C35 C44 129.6(14) . . . . ?
C20 N1 C35 C48 -50.5(18) . . . . ?
C20 N1 C36 C39 -38.1(18) . . . . ?
C20 N1 C36 C43 142.5(12) . . . . ?
C20 C21 C22 C12 5(2) . . . . ?
C23 C13 C14 C4 177.0(8) . . . . ?
C23 C13 C14 C26 -1.5(13) . . . . ?
C23 C24 C25 C26 4.7(15) . . . . ?
C24 C25 C26 C14 -2.7(15) . . . . ?
C27 C10 C11 C12 118.5(10) . . . . ?
C27 C10 C11 C19 -63.4(14) . . . . ?
C27 C10 C29 C30 171.7(8) . . . . ?
C29 C10 C11 C12 -118.9(9) . . . . ?
C29 C10 C11 C19 59.2(14) . . . . ?
C29 C10 C27 C28 179.5(9) . . . . ?
C31 C7 C8 C9 126.9(9) . . . . ?
C31 C7 C8 C15 -53.5(14) . . . . ?
C31 C7 C33 C34 54.1(12) . . . . ?
C33 C7 C8 C9 -105.5(9) . . . . ?
C33 C7 C8 C15 74.2(13) . . . . ?
C33 C7 C31 C32 173.6(9) . . . . ?
C35 N1 C20 C19 143.3(14) . . . . ?
C35 N1 C20 C21 -40(2) . . . . ?
C35 N1 C36 C39 135.2(14) . . . . ?
C35 N1 C36 C43 -44.2(17) . . . . ?
C35 C44 C45 C46 -2(2) . . . . ?
C36 N1 C20 C19 -43.2(19) . . . . ?
C36 N1 C20 C21 133.9(14) . . . . ?
C36 N1 C35 C44 -43.6(19) . . . . ?
C36 N1 C35 C48 136.3(13) . . . . ?
C36 C39 C40 C41 1(3) . . . . ?
C37 N2 C16 C15 -29.5(14) . . . . ?
C37 N2 C16 C17 152.7(9) . . . . ?
C37 N2 C38 C54 -67.2(12) . . . . ?
C37 N2 C38 C58 115.4(11) . . . . ?
C37 C49 C50 C51 1.2(16) . . . . ?
C38 N2 C16 C15 145.5(9) . . . . ?
C38 N2 C16 C17 -32.3(13) . . . . ?
C38 N2 C37 C49 148.3(10) . . . . ?
C38 N2 C37 C53 -27.6(14) . . . . ?
C38 C54 C55 C56 2.4(14) . . . . ?
C39 C36 C43 C42 -1.5(19) . . . . ?
C39 C40 C41 O1 178.3(14) . . . . ?
C39 C40 C41 C42 -2(3) . . . . ?
C40 C41 C42 C43 1(3) . . . . ?
C41 C42 C43 C36 1(2) . . . . ?
C43 C36 C39 C40 0(2) . . . . ?
C44 C35 C48 C47 3(2) . . . . ?
C44 C45 C46 O2 -176.2(11) . . . . ?
C44 C45 C46 C47 4(2) . . . . ?
C45 C46 C47 C48 -3(3) . . . . ?
C46 C47 C48 C35 -1(2) . . . . ?
C48 C35 C44 C45 -1(2) . . . . ?
C49 C37 C53 C52 3.5(16) . . . . ?
C49 C50 C51 O3 -177.8(10) . . . . ?
C49 C50 C51 C52 -1.9(18) . . . . ?
C50 C51 C52 C53 3.4(19) . . . . ?
C51 C52 C53 C37 -4.3(18) . . . . ?
C53 C37 C49 C50 -1.9(14) . . . . ?
C54 C38 C58 C57 0.8(14) . . . . ?
C54 C55 C56 O4 177.4(8) . . . . ?
C54 C55 C56 C57 -1.2(14) . . . . ?
C55 C56 C57 C58 -0.3(14) . . . . ?
C56 C57 C58 C38 0.4(15) . . . . ?
C58 C38 C54 C55 -2.1(14) . . . . ?
C59 O1 C41 C40 173.3(15) . . . . ?
C59 O1 C41 C42 -7(2) . . . . ?
C60 O2 C46 C45 -4.9(17) . . . . ?
C60 O2 C46 C47 174.9(12) . . . . ?
C61 O3 C51 C50 -12.0(17) . . . . ?
C61 O3 C51 C52 171.9(11) . . . . ?
C62 O4 C56 C55 -178.1(9) . . . . ?
C62 O4 C56 C57 0.4(13) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.500 1.000 295.9 83.2 '2 DCM'
2 0.500 0.000 0.500 295.9 83.2 '2 DCM'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 800'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id TxSDPA
_olex2_submission_special_instructions 'No special instructions were received'
