# Electronic Supplementary Material (ESI) for Materials Horizons.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_ITIC
_database_code_depnum_ccdc_archive 'CCDC 1942946'
loop_
_audit_author_name
_audit_author_address
'Peter Horton'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2019-07-24 deposited with the CCDC.	2019-11-18 downloaded from the CCDC.
;

#2018ncs0666_1b

_audit_creation_date             2019-05-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C47 H41 N2 O S2)'
_chemical_formula_sum            'C94 H82 N4 O2 S4'
_chemical_formula_weight         1427.87
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C132 H166 N62 O6 S8 '
_chemical_oxdiff_usercomment     1:ITIC
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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                   14.9009(7)
_cell_length_b                   15.5043(4)
_cell_length_c                   18.1199(5)
_cell_angle_alpha                99.309(2)
_cell_angle_beta                 101.541(3)
_cell_angle_gamma                108.366(3)
_cell_volume                     3777.2(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9472
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.4890
_cell_measurement_theta_min      3.5040
_shelx_estimated_absorpt_T_max   0.984
_shelx_estimated_absorpt_T_min   0.558
_exptl_absorpt_coefficient_mu    1.572
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1508
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of Pet. ether and chloroform'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1294
_diffrn_reflns_av_unetI/netI     0.1064
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            61232
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.236
_diffrn_reflns_theta_min         2.565
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -89.00  89.00   0.50    3.00    --    0.00   0.00-180.00  356
  2  ω    -89.00  89.00   0.50    3.00    --    0.00  49.00  60.00  356
  3  ω   -179.00  -1.00   0.50   13.50    --  -90.00  54.00-101.42  356
  4  ω   -179.00  -1.00   0.50   13.50    --  -90.00  50.00  85.37  356
  5  ω   -179.00  -1.00   0.50   13.50    --  -90.00  59.00-148.87  356
  6  ω   -179.00 -23.00   0.50   13.50    --  -90.00  59.00  45.37  312
  7  ω   -179.00  -1.00   0.50   13.50    --  -90.00  59.00  22.18  356
  8  ω   -179.00 -23.00   0.50   13.50    --  -90.00  59.00  45.37  312
  9  ω   -140.00 -74.00   0.50   13.50    --  -90.00  58.00 -76.55  132
 10  ω   -178.00 -55.00   0.50   13.50    --  -90.00  59.00 114.60  246
 11  ω    -49.00 -22.00   0.50   13.50    --  -90.00  59.00 114.60   54
 12  ω   -178.00 -21.00   0.50   13.50    --  -90.00  59.00 -19.17  314
 13  ω   -178.00  -2.00   0.50   13.50    --  -90.00   0.00   0.00  352
 14  ω   -174.00-149.00   0.50   13.50    --  -90.00  59.00 174.53   50
 15  ω   -142.00 -92.00   0.50   13.50    --  -90.00  59.00 174.53  100
 16  ω    -63.00 -36.00   0.50   13.50    --  -90.00  59.00 174.53   54
 17  ω   -166.00-141.00   0.50   13.50    --  -90.00  59.00  65.22   50
 18  ω    -95.00 -68.00   0.50   13.50    --  -90.00  59.00  65.22   54
 19  ω   -177.00-112.00   0.50   13.50    --  -90.00  59.00 -54.33  130
 20  ω   -178.00 -31.00   0.50   13.50    --  -90.00  59.00 145.00  294
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter χ goniometer'
_diffrn_measurement_device_type  
'Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0255717000
_diffrn_orient_matrix_UB_12      -0.0241742000
_diffrn_orient_matrix_UB_13      -0.0893428000
_diffrn_orient_matrix_UB_21      0.1088527000
_diffrn_orient_matrix_UB_22      0.0186081000
_diffrn_orient_matrix_UB_23      0.0037566000
_diffrn_orient_matrix_UB_31      -0.0168163000
_diffrn_orient_matrix_UB_32      -0.1034938000
_diffrn_orient_matrix_UB_33      -0.0009935000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8924
_reflns_number_total             13714
_reflns_odcompleteness_completeness 99.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     941
_refine_ls_number_reflns         13714
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0718
_refine_ls_restrained_S_all      1.002
_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)+(0.1201P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1770
_refine_ls_wR_factor_ref         0.2080
_refine_special_details          ?
_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.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
 C46(H46A,H46B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B),
  C84(H84A,H84B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,
 H95B), C96(H96A,H96B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C15(H15), C23(H23), C25(H25),
 C26(H26), C28(H28), C29(H29), C37(H37), C38(H38), C40(H40), C41(H41), C56(H56),
  C57(H57), C58(H58), C59(H59), C63(H63), C65(H65), C73(H73), C75(H75),
 C76(H76), C78(H78), C79(H79), C87(H87), C88(H88), C90(H90), C91(H91)
2.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C47(H47A,H47B,H47C), C85(H85A,H85B,H85C), C97(H97A,H97B,
 H97C)
;
_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
S1 S 0.24146(7) 0.62259(5) 0.24998(5) 0.0316(2) Uani 1 1 d . . . . .
S2 S 0.49739(6) 0.72195(5) 0.43353(5) 0.0301(2) Uani 1 1 d . . . . .
O1 O 0.1214(2) 0.51297(16) 0.10617(16) 0.0468(7) Uani 1 1 d . . . . .
N1 N 0.2169(3) 0.2526(2) 0.3019(2) 0.0467(9) Uani 1 1 d . . . . .
N2 N 0.0507(3) 0.0405(2) 0.0975(2) 0.0619(11) Uani 1 1 d . . . . .
C1 C 0.1148(3) 0.4311(2) 0.0959(2) 0.0358(9) Uani 1 1 d . . . . .
C2 C 0.1615(3) 0.3878(2) 0.1508(2) 0.0337(9) Uani 1 1 d . . . . .
C3 C 0.1227(3) 0.2871(2) 0.1173(2) 0.0364(9) Uani 1 1 d . . . . .
C4 C 0.0625(3) 0.2703(2) 0.0374(2) 0.0359(9) Uani 1 1 d . . . . .
C5 C 0.0574(3) 0.3554(2) 0.0251(2) 0.0377(9) Uani 1 1 d . . . . .
C6 C 0.0013(3) 0.3615(3) -0.0432(2) 0.0473(11) Uani 1 1 d . . . . .
H6 H -0.001308 0.419988 -0.050852 0.057 Uiso 1 1 calc R . . . .
C7 C -0.0514(3) 0.2789(3) -0.1006(2) 0.0520(12) Uani 1 1 d . . . . .
H7 H -0.092326 0.280210 -0.147583 0.062 Uiso 1 1 calc R . . . .
C8 C -0.0440(3) 0.1947(3) -0.0891(3) 0.0493(11) Uani 1 1 d . . . . .
H8 H -0.078777 0.139401 -0.129370 0.059 Uiso 1 1 calc R . . . .
C9 C 0.0122(3) 0.1887(3) -0.0211(2) 0.0413(10) Uani 1 1 d . . . . .
H9 H 0.016511 0.130466 -0.014403 0.050 Uiso 1 1 calc R . . . .
C10 C 0.1302(3) 0.2192(2) 0.1559(2) 0.0398(10) Uani 1 1 d . . . . .
C11 C 0.1800(3) 0.2396(2) 0.2369(3) 0.0409(10) Uani 1 1 d . . . . .
C12 C 0.0855(3) 0.1207(2) 0.1210(3) 0.0465(11) Uani 1 1 d . . . . .
C13 C 0.2362(3) 0.4332(2) 0.2168(2) 0.0348(9) Uani 1 1 d . . . . .
H13 H 0.264134 0.392950 0.239046 0.042 Uiso 1 1 calc R . . . .
C14 C 0.2806(3) 0.5283(2) 0.2589(2) 0.0314(8) Uani 1 1 d . . . . .
C15 C 0.3650(3) 0.5543(2) 0.3193(2) 0.0306(8) Uani 1 1 d . . . . .
H15 H 0.396100 0.512321 0.333740 0.037 Uiso 1 1 calc R . . . .
C16 C 0.3989(3) 0.6497(2) 0.3565(2) 0.0290(8) Uani 1 1 d . . . . .
C17 C 0.3368(3) 0.6950(2) 0.3272(2) 0.0279(8) Uani 1 1 d . . . . .
C18 C 0.3706(3) 0.7902(2) 0.3691(2) 0.0284(8) Uani 1 1 d . . . . .
C19 C 0.4556(3) 0.8124(2) 0.4266(2) 0.0282(8) Uani 1 1 d . . . . .
C20 C 0.4878(3) 0.9089(2) 0.4706(2) 0.0272(8) Uani 1 1 d . . . . .
C21 C 0.4179(2) 0.9457(2) 0.4388(2) 0.0259(7) Uani 1 1 d . . . . .
C22 C 0.3345(3) 0.8719(2) 0.3723(2) 0.0278(8) Uani 1 1 d . . . . .
C23 C 0.5705(3) 0.9624(2) 0.5317(2) 0.0282(8) Uani 1 1 d . . . . .
H23 H 0.617099 0.936528 0.552285 0.034 Uiso 1 1 calc R . . . .
C24 C 0.3238(3) 0.9061(2) 0.2975(2) 0.0282(8) Uani 1 1 d . . . . .
C25 C 0.3539(3) 0.8708(2) 0.2352(2) 0.0304(8) Uani 1 1 d . . . . .
H25 H 0.384245 0.825601 0.239118 0.036 Uiso 1 1 calc R . . . .
C26 C 0.3400(3) 0.9013(2) 0.1670(2) 0.0356(9) Uani 1 1 d . . . . .
H26 H 0.360884 0.876085 0.125069 0.043 Uiso 1 1 calc R . . . .
C27 C 0.2961(3) 0.9678(2) 0.1586(2) 0.0356(9) Uani 1 1 d . . . . .
C28 C 0.2671(3) 1.0034(2) 0.2220(2) 0.0353(9) Uani 1 1 d . . . . .
H28 H 0.237964 1.049437 0.218488 0.042 Uiso 1 1 calc R . . . .
C29 C 0.2800(3) 0.9730(2) 0.2896(2) 0.0303(8) Uani 1 1 d . . . . .
H29 H 0.258728 0.997896 0.331479 0.036 Uiso 1 1 calc R . . . .
C30 C 0.2831(3) 0.9999(3) 0.0847(2) 0.0452(10) Uani 1 1 d . . . . .
H30A H 0.225821 1.020048 0.077629 0.054 Uiso 1 1 calc R . . . .
H30B H 0.269622 0.946921 0.040317 0.054 Uiso 1 1 calc R . . . .
C31 C 0.3743(4) 1.0812(3) 0.0851(3) 0.0485(11) Uani 1 1 d . . . . .
H31A H 0.433461 1.067768 0.106854 0.058 Uiso 1 1 calc R . . . .
H31B H 0.372833 1.085061 0.030929 0.058 Uiso 1 1 calc R . . . .
C32 C 0.3826(3) 1.1756(3) 0.1318(2) 0.0437(10) Uani 1 1 d . . . . .
H32A H 0.374379 1.169292 0.183751 0.052 Uiso 1 1 calc R . . . .
H32B H 0.328393 1.193294 0.105609 0.052 Uiso 1 1 calc R . . . .
C33 C 0.4802(3) 1.2541(3) 0.1416(3) 0.0473(10) Uani 1 1 d . . . . .
H33A H 0.533811 1.238318 0.171238 0.057 Uiso 1 1 calc R . . . .
H33B H 0.490703 1.256694 0.089651 0.057 Uiso 1 1 calc R . . . .
C34 C 0.4877(3) 1.3508(3) 0.1828(3) 0.0484(11) Uani 1 1 d . . . . .
H34A H 0.467337 1.346472 0.231225 0.058 Uiso 1 1 calc R . . . .
H34B H 0.557052 1.393452 0.197271 0.058 Uiso 1 1 calc R . . . .
C35 C 0.4251(4) 1.3925(3) 0.1340(3) 0.0531(12) Uani 1 1 d . . . . .
H35A H 0.444576 1.396859 0.085785 0.080 Uiso 1 1 calc GR . . . .
H35B H 0.434511 1.455145 0.163087 0.080 Uiso 1 1 calc GR . . . .
H35C H 0.355831 1.352361 0.121652 0.080 Uiso 1 1 calc GR . . . .
C36 C 0.2363(2) 0.8419(2) 0.3941(2) 0.0271(8) Uani 1 1 d . . . . .
C37 C 0.2325(3) 0.8477(2) 0.4705(2) 0.0332(8) Uani 1 1 d . . . . .
H37 H 0.291998 0.871416 0.510771 0.040 Uiso 1 1 calc R . . . .
C38 C 0.1438(3) 0.8198(2) 0.4892(2) 0.0367(9) Uani 1 1 d . . . . .
H38 H 0.143416 0.824524 0.542105 0.044 Uiso 1 1 calc R . . . .
C39 C 0.0549(3) 0.7847(2) 0.4318(2) 0.0359(9) Uani 1 1 d . . . . .
C40 C 0.0588(3) 0.7747(2) 0.3547(2) 0.0331(8) Uani 1 1 d . . . . .
H40 H -0.000499 0.748367 0.314201 0.040 Uiso 1 1 calc R . . . .
C41 C 0.1471(3) 0.8023(2) 0.3363(2) 0.0308(8) Uani 1 1 d . . . . .
H41 H 0.147539 0.794357 0.283307 0.037 Uiso 1 1 calc R . . . .
C42 C -0.0415(3) 0.7627(2) 0.4525(3) 0.0400(9) Uani 1 1 d . . . . .
H42A H -0.032681 0.749796 0.504705 0.048 Uiso 1 1 calc R . . . .
H42B H -0.090159 0.705264 0.415009 0.048 Uiso 1 1 calc R . . . .
C43 C -0.0815(3) 0.8422(2) 0.4522(3) 0.0424(10) Uani 1 1 d . . . . .
H43A H -0.033809 0.898952 0.491018 0.051 Uiso 1 1 calc R . . . .
H43B H -0.087925 0.856604 0.400553 0.051 Uiso 1 1 calc R . . . .
C44 C -0.1795(3) 0.8195(3) 0.4701(3) 0.0424(10) Uani 1 1 d . . . . .
H44A H -0.173509 0.802094 0.520598 0.051 Uiso 1 1 calc R . . . .
H44B H -0.227548 0.764137 0.429960 0.051 Uiso 1 1 calc R . . . .
C45 C -0.2200(3) 0.8992(3) 0.4737(3) 0.0498(11) Uani 1 1 d . . . . .
H45A H -0.281878 0.878834 0.489343 0.060 Uiso 1 1 calc R . . . .
H45B H -0.172642 0.953717 0.514986 0.060 Uiso 1 1 calc R . . . .
C46 C -0.2401(3) 0.9313(3) 0.3998(3) 0.0493(11) Uani 1 1 d . . . . .
H46A H -0.177576 0.956865 0.386030 0.059 Uiso 1 1 calc R . . . .
H46B H -0.265663 0.982663 0.409208 0.059 Uiso 1 1 calc R . . . .
C47 C -0.3127(4) 0.8545(3) 0.3320(3) 0.0568(12) Uani 1 1 d . . . . .
H47A H -0.332698 0.881956 0.289344 0.085 Uiso 1 1 calc GR . . . .
H47B H -0.370518 0.821351 0.348039 0.085 Uiso 1 1 calc GR . . . .
H47C H -0.282059 0.810437 0.314569 0.085 Uiso 1 1 calc GR . . . .
S51 S 0.29294(7) 0.74027(5) 0.66388(5) 0.0326(2) Uani 1 1 d . . . . .
S52 S 0.57627(7) 0.77632(5) 0.64113(5) 0.0309(2) Uani 1 1 d . . . . .
O51 O 0.13311(19) 0.78717(16) 0.67387(16) 0.0412(7) Uani 1 1 d . . . . .
N51 N 0.4829(3) 1.0941(3) 0.9182(2) 0.0561(10) Uani 1 1 d . . . . .
N52 N 0.2629(3) 1.2082(3) 0.9468(2) 0.0580(11) Uani 1 1 d . . . . .
C51 C 0.1543(3) 0.8674(2) 0.7116(2) 0.0360(9) Uani 1 1 d . . . . .
C52 C 0.2533(3) 0.9342(2) 0.7563(2) 0.0325(8) Uani 1 1 d . . . . .
C53 C 0.2385(3) 1.0139(2) 0.8013(2) 0.0341(9) Uani 1 1 d . . . . .
C54 C 0.1348(3) 1.0047(2) 0.7703(2) 0.0360(9) Uani 1 1 d . . . . .
C55 C 0.0856(3) 0.9170(2) 0.7179(2) 0.0380(9) Uani 1 1 d . . . . .
C56 C -0.0124(3) 0.8885(3) 0.6774(2) 0.0436(10) Uani 1 1 d . . . . .
H56 H -0.045711 0.828132 0.643258 0.052 Uiso 1 1 calc R . . . .
C57 C -0.0598(3) 0.9512(3) 0.6883(3) 0.0469(11) Uani 1 1 d . . . . .
H57 H -0.126629 0.934201 0.660773 0.056 Uiso 1 1 calc R . . . .
C58 C -0.0106(3) 1.0390(3) 0.7394(3) 0.0468(10) Uani 1 1 d . . . . .
H58 H -0.044524 1.081219 0.745428 0.056 Uiso 1 1 calc R . . . .
C59 C 0.0862(3) 1.0665(3) 0.7817(2) 0.0420(10) Uani 1 1 d . . . . .
H59 H 0.118256 1.125920 0.817532 0.050 Uiso 1 1 calc R . . . .
C60 C 0.3047(3) 1.0821(2) 0.8638(2) 0.0371(9) Uani 1 1 d . . . . .
C61 C 0.4030(3) 1.0873(3) 0.8933(2) 0.0418(10) Uani 1 1 d . . . . .
C62 C 0.2800(3) 1.1523(3) 0.9088(2) 0.0433(10) Uani 1 1 d . . . . .
C63 C 0.3404(3) 0.9291(2) 0.7488(2) 0.0347(9) Uani 1 1 d . . . . .
H63 H 0.394913 0.984429 0.776104 0.042 Uiso 1 1 calc R . . . .
C64 C 0.3676(3) 0.8582(2) 0.7086(2) 0.0329(8) Uani 1 1 d . . . . .
C65 C 0.4632(3) 0.8763(2) 0.7037(2) 0.0342(9) Uani 1 1 d . . . . .
H65 H 0.514068 0.935917 0.724257 0.041 Uiso 1 1 calc R . . . .
C66 C 0.4768(3) 0.7975(2) 0.6653(2) 0.0319(8) Uani 1 1 d . . . . .
C67 C 0.3907(3) 0.7179(2) 0.6415(2) 0.0327(8) Uani 1 1 d . . . . .
C68 C 0.4064(3) 0.6391(2) 0.6020(2) 0.0293(8) Uani 1 1 d . . . . .
C69 C 0.5015(3) 0.6614(2) 0.5973(2) 0.0282(8) Uani 1 1 d . . . . .
C70 C 0.5135(3) 0.5825(2) 0.5498(2) 0.0284(8) Uani 1 1 d . . . . .
C71 C 0.4214(3) 0.5092(2) 0.5265(2) 0.0286(8) Uani 1 1 d . . . . .
C72 C 0.3462(3) 0.5361(2) 0.5628(2) 0.0286(8) Uani 1 1 d . . . . .
C73 C 0.4066(3) 0.4250(2) 0.4758(2) 0.0288(8) Uani 1 1 d . . . . .
H73 H 0.344821 0.375040 0.459570 0.035 Uiso 1 1 calc R . . . .
C74 C 0.3229(3) 0.4858(2) 0.6270(2) 0.0293(8) Uani 1 1 d . . . . .
C75 C 0.3805(3) 0.4391(2) 0.6600(2) 0.0348(9) Uani 1 1 d . . . . .
H75 H 0.434674 0.435753 0.641113 0.042 Uiso 1 1 calc R . . . .
C76 C 0.3603(3) 0.3973(2) 0.7201(2) 0.0362(9) Uani 1 1 d . . . . .
H76 H 0.401628 0.367020 0.741928 0.043 Uiso 1 1 calc R . . . .
C77 C 0.2810(3) 0.3988(2) 0.7489(2) 0.0372(9) Uani 1 1 d . . . . .
C78 C 0.2245(3) 0.4467(2) 0.7164(2) 0.0374(9) Uani 1 1 d . . . . .
H78 H 0.170468 0.450124 0.735415 0.045 Uiso 1 1 calc R . . . .
C79 C 0.2449(3) 0.4894(2) 0.6569(2) 0.0339(8) Uani 1 1 d . . . . .
H79 H 0.204895 0.521524 0.636273 0.041 Uiso 1 1 calc R . . . .
C80 C 0.2547(3) 0.3480(3) 0.8109(3) 0.0469(10) Uani 1 1 d . . . . .
H80A H 0.306678 0.323286 0.828925 0.056 Uiso 1 1 calc R . . . .
H80B H 0.192877 0.293619 0.786803 0.056 Uiso 1 1 calc R . . . .
C81 C 0.2418(4) 0.4059(3) 0.8813(3) 0.0503(11) Uani 1 1 d . . . . .
H81A H 0.189584 0.430627 0.863873 0.060 Uiso 1 1 calc R . . . .
H81B H 0.219798 0.364770 0.915664 0.060 Uiso 1 1 calc R . . . .
C82 C 0.3343(3) 0.4870(3) 0.9275(3) 0.0500(11) Uani 1 1 d . . . . .
H82A H 0.350183 0.532928 0.895495 0.060 Uiso 1 1 calc R . . . .
H82B H 0.388979 0.463384 0.937228 0.060 Uiso 1 1 calc R . . . .
C83 C 0.3290(4) 0.5376(3) 1.0051(3) 0.0510(11) Uani 1 1 d . . . . .
H83A H 0.273499 0.560207 0.995740 0.061 Uiso 1 1 calc R . . . .
H83B H 0.315269 0.492459 1.037931 0.061 Uiso 1 1 calc R . . . .
C84 C 0.4214(4) 0.6194(3) 1.0483(3) 0.0573(12) Uani 1 1 d . . . . .
H84A H 0.433968 0.665090 1.015778 0.069 Uiso 1 1 calc R . . . .
H84B H 0.477035 0.596879 1.056006 0.069 Uiso 1 1 calc R . . . .
C85 C 0.4193(4) 0.6697(3) 1.1271(3) 0.0656(14) Uani 1 1 d . . . . .
H85A H 0.363928 0.691639 1.120473 0.098 Uiso 1 1 calc GR . . . .
H85B H 0.480741 0.723457 1.150211 0.098 Uiso 1 1 calc GR . . . .
H85C H 0.411847 0.626514 1.161291 0.098 Uiso 1 1 calc GR . . . .
C86 C 0.2525(3) 0.5195(2) 0.5002(2) 0.0297(8) Uani 1 1 d . . . . .
C87 C 0.2342(3) 0.5910(2) 0.4693(2) 0.0338(8) Uani 1 1 d . . . . .
H87 H 0.281636 0.652811 0.486653 0.041 Uiso 1 1 calc R . . . .
C88 C 0.1477(3) 0.5730(2) 0.4135(2) 0.0364(9) Uani 1 1 d . . . . .
H88 H 0.136287 0.622924 0.393939 0.044 Uiso 1 1 calc R . . . .
C89 C 0.0773(3) 0.4832(2) 0.3857(2) 0.0352(9) Uani 1 1 d . . . . .
C90 C 0.0968(3) 0.4112(2) 0.4155(2) 0.0376(9) Uani 1 1 d . . . . .
H90 H 0.050478 0.349001 0.396652 0.045 Uiso 1 1 calc R . . . .
C91 C 0.1822(3) 0.4291(2) 0.4717(2) 0.0334(8) Uani 1 1 d . . . . .
H91 H 0.193475 0.379169 0.491371 0.040 Uiso 1 1 calc R . . . .
C92 C -0.0181(3) 0.4614(3) 0.3265(2) 0.0455(10) Uani 1 1 d . . . . .
H92A H -0.026768 0.520959 0.321050 0.055 Uiso 1 1 calc R . . . .
H92B H -0.072399 0.425680 0.345939 0.055 Uiso 1 1 calc R . . . .
C93 C -0.0258(3) 0.4060(3) 0.2475(2) 0.0495(11) Uani 1 1 d . . . . .
H93A H -0.002894 0.353576 0.254112 0.059 Uiso 1 1 calc R . . . .
H93B H 0.018731 0.446888 0.223130 0.059 Uiso 1 1 calc R . . . .
C94 C -0.1287(3) 0.3663(3) 0.1929(3) 0.0538(12) Uani 1 1 d . . . . .
H94A H -0.173281 0.326150 0.217709 0.065 Uiso 1 1 calc R . . . .
H94B H -0.151179 0.418833 0.185934 0.065 Uiso 1 1 calc R . . . .
C95 C -0.1380(4) 0.3102(4) 0.1147(3) 0.0693(15) Uani 1 1 d . . . . .
H95A H -0.107345 0.263010 0.121924 0.083 Uiso 1 1 calc R . . . .
H95B H -0.100063 0.352567 0.087340 0.083 Uiso 1 1 calc R . . . .
C96 C -0.2419(4) 0.2598(3) 0.0627(3) 0.0619(13) Uani 1 1 d . . . . .
H96A H -0.275933 0.305213 0.060572 0.074 Uiso 1 1 calc R . . . .
H96B H -0.238571 0.236832 0.009395 0.074 Uiso 1 1 calc R . . . .
C97 C -0.3019(4) 0.1782(3) 0.0888(3) 0.0606(13) Uani 1 1 d . . . . .
H97A H -0.365333 0.145590 0.050108 0.091 Uiso 1 1 calc GR . . . .
H97B H -0.312600 0.201201 0.138758 0.091 Uiso 1 1 calc GR . . . .
H97C H -0.266686 0.134893 0.094611 0.091 Uiso 1 1 calc GR . . . .


_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 C14 1.755(3) . ?
S1 C17 1.711(3) . ?
S2 C16 1.731(3) . ?
S2 C19 1.717(3) . ?
O1 C1 1.221(4) . ?
N1 C11 1.151(5) . ?
N2 C12 1.153(5) . ?
C1 C2 1.470(5) . ?
C1 C5 1.481(5) . ?
C2 C3 1.457(4) . ?
C2 C13 1.367(5) . ?
C3 C4 1.477(5) . ?
C3 C10 1.375(5) . ?
C4 C5 1.396(5) . ?
C4 C9 1.392(5) . ?
C5 C6 1.384(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.395(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.390(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.378(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.439(6) . ?
C10 C12 1.433(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.419(4) . ?
C14 C15 1.389(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.402(4) . ?
C16 C17 1.403(4) . ?
C17 C18 1.423(4) . ?
C18 C19 1.375(5) . ?
C18 C22 1.521(4) . ?
C19 C20 1.453(4) . ?
C20 C21 1.408(4) . ?
C20 C23 1.395(5) . ?
C21 C22 1.538(4) . ?
C21 C23 1.381(4) 2_676 ?
C22 C24 1.530(5) . ?
C22 C36 1.542(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.392(5) . ?
C24 C29 1.399(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.393(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.397(5) . ?
C27 C28 1.398(5) . ?
C27 C30 1.500(5) . ?
C28 H28 0.9500 . ?
C28 C29 1.383(5) . ?
C29 H29 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.532(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.521(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.530(6) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.521(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.517(6) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.386(5) . ?
C36 C41 1.400(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.385(5) . ?
C38 H38 0.9500 . ?
C38 C39 1.395(5) . ?
C39 C40 1.395(5) . ?
C39 C42 1.506(6) . ?
C40 H40 0.9500 . ?
C40 C41 1.375(5) . ?
C41 H41 0.9500 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.530(5) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.504(6) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.536(5) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.510(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.510(6) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
S51 C64 1.765(3) . ?
S51 C67 1.708(4) . ?
S52 C66 1.736(4) . ?
S52 C69 1.728(3) . ?
O51 C51 1.227(4) . ?
N51 C61 1.151(5) . ?
N52 C62 1.144(5) . ?
C51 C52 1.481(5) . ?
C51 C55 1.472(5) . ?
C52 C53 1.469(5) . ?
C52 C63 1.357(5) . ?
C53 C54 1.486(5) . ?
C53 C60 1.372(5) . ?
C54 C55 1.401(5) . ?
C54 C59 1.387(5) . ?
C55 C56 1.388(6) . ?
C56 H56 0.9500 . ?
C56 C57 1.381(5) . ?
C57 H57 0.9500 . ?
C57 C58 1.393(6) . ?
C58 H58 0.9500 . ?
C58 C59 1.383(6) . ?
C59 H59 0.9500 . ?
C60 C61 1.427(6) . ?
C60 C62 1.437(5) . ?
C63 H63 0.9500 . ?
C63 C64 1.431(5) . ?
C64 C65 1.386(5) . ?
C65 H65 0.9500 . ?
C65 C66 1.398(5) . ?
C66 C67 1.402(5) . ?
C67 C68 1.422(5) . ?
C68 C69 1.373(5) . ?
C68 C72 1.529(4) . ?
C69 C70 1.458(4) . ?
C70 C71 1.409(5) . ?
C70 C73 1.392(5) 2_666 ?
C71 C72 1.537(5) . ?
C71 C73 1.394(4) . ?
C72 C74 1.538(5) . ?
C72 C86 1.532(5) . ?
C73 H73 0.9500 . ?
C74 C75 1.396(5) . ?
C74 C79 1.389(5) . ?
C75 H75 0.9500 . ?
C75 C76 1.389(5) . ?
C76 H76 0.9500 . ?
C76 C77 1.388(6) . ?
C77 C78 1.394(5) . ?
C77 C80 1.519(5) . ?
C78 H78 0.9500 . ?
C78 C79 1.389(5) . ?
C79 H79 0.9500 . ?
C80 H80A 0.9900 . ?
C80 H80B 0.9900 . ?
C80 C81 1.519(6) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C81 C82 1.512(6) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C82 C83 1.525(6) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C83 C84 1.506(7) . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?
C84 C85 1.523(6) . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C86 C87 1.396(5) . ?
C86 C91 1.397(5) . ?
C87 H87 0.9500 . ?
C87 C88 1.386(5) . ?
C88 H88 0.9500 . ?
C88 C89 1.390(5) . ?
C89 C90 1.399(5) . ?
C89 C92 1.502(5) . ?
C90 H90 0.9500 . ?
C90 C91 1.379(5) . ?
C91 H91 0.9500 . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C92 C93 1.508(6) . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
C93 C94 1.521(6) . ?
C94 H94A 0.9900 . ?
C94 H94B 0.9900 . ?
C94 C95 1.493(6) . ?
C95 H95A 0.9900 . ?
C95 H95B 0.9900 . ?
C95 C96 1.520(7) . ?
C96 H96A 0.9900 . ?
C96 H96B 0.9900 . ?
C96 C97 1.508(7) . ?
C97 H97A 0.9800 . ?
C97 H97B 0.9800 . ?
C97 H97C 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
C17 S1 C14 90.87(15) . . ?
C19 S2 C16 89.47(15) . . ?
O1 C1 C2 127.2(3) . . ?
O1 C1 C5 126.6(3) . . ?
C2 C1 C5 106.2(3) . . ?
C3 C2 C1 107.6(3) . . ?
C13 C2 C1 126.8(3) . . ?
C13 C2 C3 125.2(3) . . ?
C2 C3 C4 107.5(3) . . ?
C10 C3 C2 126.3(3) . . ?
C10 C3 C4 125.7(3) . . ?
C5 C4 C3 108.4(3) . . ?
C9 C4 C3 131.8(3) . . ?
C9 C4 C5 119.8(3) . . ?
C4 C5 C1 109.7(3) . . ?
C6 C5 C1 128.2(3) . . ?
C6 C5 C4 122.0(3) . . ?
C5 C6 H6 121.1 . . ?
C5 C6 C7 117.8(4) . . ?
C7 C6 H6 121.1 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0(4) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 H8 118.9 . . ?
C9 C8 C7 122.2(4) . . ?
C9 C8 H8 118.9 . . ?
C4 C9 H9 120.9 . . ?
C8 C9 C4 118.1(3) . . ?
C8 C9 H9 120.9 . . ?
C3 C10 C11 123.4(3) . . ?
C3 C10 C12 123.9(4) . . ?
C12 C10 C11 112.7(3) . . ?
N1 C11 C10 177.2(4) . . ?
N2 C12 C10 175.8(5) . . ?
C2 C13 H13 113.5 . . ?
C2 C13 C14 133.0(3) . . ?
C14 C13 H13 113.5 . . ?
C13 C14 S1 129.4(3) . . ?
C15 C14 S1 111.9(2) . . ?
C15 C14 C13 118.6(3) . . ?
C14 C15 H15 124.0 . . ?
C14 C15 C16 112.1(3) . . ?
C16 C15 H15 124.0 . . ?
C15 C16 S2 133.9(3) . . ?
C15 C16 C17 112.8(3) . . ?
C17 C16 S2 113.2(2) . . ?
C16 C17 S1 112.2(2) . . ?
C16 C17 C18 111.2(3) . . ?
C18 C17 S1 136.5(3) . . ?
C17 C18 C22 137.6(3) . . ?
C19 C18 C17 111.1(3) . . ?
C19 C18 C22 111.0(3) . . ?
C18 C19 S2 115.0(2) . . ?
C18 C19 C20 110.7(3) . . ?
C20 C19 S2 134.3(3) . . ?
C21 C20 C19 106.7(3) . . ?
C23 C20 C19 131.0(3) . . ?
C23 C20 C21 122.3(3) . . ?
C20 C21 C22 111.5(3) . . ?
C23 C21 C20 120.2(3) 2_676 . ?
C23 C21 C22 128.4(3) 2_676 . ?
C18 C22 C21 100.0(3) . . ?
C18 C22 C24 114.4(3) . . ?
C18 C22 C36 107.6(3) . . ?
C21 C22 C36 112.1(3) . . ?
C24 C22 C21 111.2(3) . . ?
C24 C22 C36 111.0(3) . . ?
C20 C23 H23 121.2 . . ?
C21 C23 C20 117.5(3) 2_676 . ?
C21 C23 H23 121.2 2_676 . ?
C25 C24 C22 122.0(3) . . ?
C25 C24 C29 118.1(3) . . ?
C29 C24 C22 119.9(3) . . ?
C24 C25 H25 119.8 . . ?
C24 C25 C26 120.4(3) . . ?
C26 C25 H25 119.8 . . ?
C25 C26 H26 119.1 . . ?
C25 C26 C27 121.9(4) . . ?
C27 C26 H26 119.1 . . ?
C26 C27 C28 117.1(3) . . ?
C26 C27 C30 120.5(3) . . ?
C28 C27 C30 122.4(3) . . ?
C27 C28 H28 119.3 . . ?
C29 C28 C27 121.5(3) . . ?
C29 C28 H28 119.3 . . ?
C24 C29 H29 119.5 . . ?
C28 C29 C24 121.1(3) . . ?
C28 C29 H29 119.5 . . ?
C27 C30 H30A 109.2 . . ?
C27 C30 H30B 109.2 . . ?
C27 C30 C31 111.9(3) . . ?
H30A C30 H30B 107.9 . . ?
C31 C30 H30A 109.2 . . ?
C31 C30 H30B 109.2 . . ?
C30 C31 H31A 108.8 . . ?
C30 C31 H31B 108.8 . . ?
H31A C31 H31B 107.7 . . ?
C32 C31 C30 113.8(4) . . ?
C32 C31 H31A 108.8 . . ?
C32 C31 H31B 108.8 . . ?
C31 C32 H32A 108.8 . . ?
C31 C32 H32B 108.8 . . ?
C31 C32 C33 113.7(4) . . ?
H32A C32 H32B 107.7 . . ?
C33 C32 H32A 108.8 . . ?
C33 C32 H32B 108.8 . . ?
C32 C33 H33A 108.6 . . ?
C32 C33 H33B 108.6 . . ?
H33A C33 H33B 107.5 . . ?
C34 C33 C32 114.9(4) . . ?
C34 C33 H33A 108.6 . . ?
C34 C33 H33B 108.6 . . ?
C33 C34 H34A 108.9 . . ?
C33 C34 H34B 108.9 . . ?
H34A C34 H34B 107.7 . . ?
C35 C34 C33 113.5(4) . . ?
C35 C34 H34A 108.9 . . ?
C35 C34 H34B 108.9 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 C22 121.8(3) . . ?
C37 C36 C41 117.4(3) . . ?
C41 C36 C22 120.6(3) . . ?
C36 C37 H37 119.4 . . ?
C38 C37 C36 121.3(3) . . ?
C38 C37 H37 119.4 . . ?
C37 C38 H38 119.5 . . ?
C37 C38 C39 121.1(4) . . ?
C39 C38 H38 119.5 . . ?
C38 C39 C40 117.6(4) . . ?
C38 C39 C42 121.0(4) . . ?
C40 C39 C42 121.3(3) . . ?
C39 C40 H40 119.4 . . ?
C41 C40 C39 121.1(3) . . ?
C41 C40 H40 119.4 . . ?
C36 C41 H41 119.3 . . ?
C40 C41 C36 121.4(3) . . ?
C40 C41 H41 119.3 . . ?
C39 C42 H42A 109.0 . . ?
C39 C42 H42B 109.0 . . ?
C39 C42 C43 112.9(3) . . ?
H42A C42 H42B 107.8 . . ?
C43 C42 H42A 109.0 . . ?
C43 C42 H42B 109.0 . . ?
C42 C43 H43A 108.9 . . ?
C42 C43 H43B 108.9 . . ?
H43A C43 H43B 107.7 . . ?
C44 C43 C42 113.2(3) . . ?
C44 C43 H43A 108.9 . . ?
C44 C43 H43B 108.9 . . ?
C43 C44 H44A 108.6 . . ?
C43 C44 H44B 108.6 . . ?
C43 C44 C45 114.7(3) . . ?
H44A C44 H44B 107.6 . . ?
C45 C44 H44A 108.6 . . ?
C45 C44 H44B 108.6 . . ?
C44 C45 H45A 108.2 . . ?
C44 C45 H45B 108.2 . . ?
H45A C45 H45B 107.4 . . ?
C46 C45 C44 116.2(4) . . ?
C46 C45 H45A 108.2 . . ?
C46 C45 H45B 108.2 . . ?
C45 C46 H46A 108.9 . . ?
C45 C46 H46B 108.9 . . ?
C45 C46 C47 113.6(4) . . ?
H46A C46 H46B 107.7 . . ?
C47 C46 H46A 108.9 . . ?
C47 C46 H46B 108.9 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C67 S51 C64 90.75(17) . . ?
C69 S52 C66 89.42(16) . . ?
O51 C51 C52 127.1(3) . . ?
O51 C51 C55 126.0(4) . . ?
C55 C51 C52 106.8(3) . . ?
C53 C52 C51 106.3(3) . . ?
C63 C52 C51 126.6(3) . . ?
C63 C52 C53 126.5(3) . . ?
C52 C53 C54 107.5(3) . . ?
C60 C53 C52 127.4(3) . . ?
C60 C53 C54 125.0(3) . . ?
C55 C54 C53 108.1(3) . . ?
C59 C54 C53 131.8(3) . . ?
C59 C54 C55 120.0(4) . . ?
C54 C55 C51 109.8(3) . . ?
C56 C55 C51 128.3(3) . . ?
C56 C55 C54 121.9(3) . . ?
C55 C56 H56 121.2 . . ?
C57 C56 C55 117.7(4) . . ?
C57 C56 H56 121.2 . . ?
C56 C57 H57 119.7 . . ?
C56 C57 C58 120.6(4) . . ?
C58 C57 H57 119.7 . . ?
C57 C58 H58 119.0 . . ?
C59 C58 C57 121.9(4) . . ?
C59 C58 H58 119.0 . . ?
C54 C59 H59 121.0 . . ?
C58 C59 C54 117.9(4) . . ?
C58 C59 H59 121.0 . . ?
C53 C60 C61 123.4(3) . . ?
C53 C60 C62 123.2(4) . . ?
C61 C60 C62 113.4(3) . . ?
N51 C61 C60 178.0(4) . . ?
N52 C62 C60 177.5(4) . . ?
C52 C63 H63 113.2 . . ?
C52 C63 C64 133.6(3) . . ?
C64 C63 H63 113.2 . . ?
C63 C64 S51 127.6(3) . . ?
C65 C64 S51 111.2(2) . . ?
C65 C64 C63 121.1(3) . . ?
C64 C65 H65 123.6 . . ?
C64 C65 C66 112.9(3) . . ?
C66 C65 H65 123.6 . . ?
C65 C66 S52 134.4(3) . . ?
C65 C66 C67 112.4(3) . . ?
C67 C66 S52 113.2(3) . . ?
C66 C67 S51 112.7(3) . . ?
C66 C67 C68 111.2(3) . . ?
C68 C67 S51 136.1(3) . . ?
C67 C68 C72 137.5(3) . . ?
C69 C68 C67 111.7(3) . . ?
C69 C68 C72 110.8(3) . . ?
C68 C69 S52 114.5(2) . . ?
C68 C69 C70 110.8(3) . . ?
C70 C69 S52 134.5(3) . . ?
C71 C70 C69 106.4(3) . . ?
C73 C70 C69 131.1(3) 2_666 . ?
C73 C70 C71 122.4(3) 2_666 . ?
C70 C71 C72 111.7(3) . . ?
C73 C71 C70 120.6(3) . . ?
C73 C71 C72 127.7(3) . . ?
C68 C72 C71 99.8(3) . . ?
C68 C72 C74 107.4(3) . . ?
C68 C72 C86 114.5(3) . . ?
C71 C72 C74 112.6(3) . . ?
C86 C72 C71 110.8(3) . . ?
C86 C72 C74 111.2(3) . . ?
C70 C73 C71 117.0(3) 2_666 . ?
C70 C73 H73 121.5 2_666 . ?
C71 C73 H73 121.5 . . ?
C75 C74 C72 122.4(3) . . ?
C79 C74 C72 120.3(3) . . ?
C79 C74 C75 117.3(3) . . ?
C74 C75 H75 119.3 . . ?
C76 C75 C74 121.3(4) . . ?
C76 C75 H75 119.3 . . ?
C75 C76 H76 119.2 . . ?
C77 C76 C75 121.6(3) . . ?
C77 C76 H76 119.2 . . ?
C76 C77 C78 116.9(4) . . ?
C76 C77 C80 121.8(3) . . ?
C78 C77 C80 121.3(4) . . ?
C77 C78 H78 119.1 . . ?
C79 C78 C77 121.8(4) . . ?
C79 C78 H78 119.1 . . ?
C74 C79 H79 119.4 . . ?
C78 C79 C74 121.1(3) . . ?
C78 C79 H79 119.4 . . ?
C77 C80 H80A 108.3 . . ?
C77 C80 H80B 108.3 . . ?
C77 C80 C81 115.9(3) . . ?
H80A C80 H80B 107.4 . . ?
C81 C80 H80A 108.3 . . ?
C81 C80 H80B 108.3 . . ?
C80 C81 H81A 108.9 . . ?
C80 C81 H81B 108.9 . . ?
H81A C81 H81B 107.7 . . ?
C82 C81 C80 113.5(4) . . ?
C82 C81 H81A 108.9 . . ?
C82 C81 H81B 108.9 . . ?
C81 C82 H82A 108.5 . . ?
C81 C82 H82B 108.5 . . ?
C81 C82 C83 115.0(4) . . ?
H82A C82 H82B 107.5 . . ?
C83 C82 H82A 108.5 . . ?
C83 C82 H82B 108.5 . . ?
C82 C83 H83A 108.9 . . ?
C82 C83 H83B 108.9 . . ?
H83A C83 H83B 107.7 . . ?
C84 C83 C82 113.5(4) . . ?
C84 C83 H83A 108.9 . . ?
C84 C83 H83B 108.9 . . ?
C83 C84 H84A 108.6 . . ?
C83 C84 H84B 108.6 . . ?
C83 C84 C85 114.7(4) . . ?
H84A C84 H84B 107.6 . . ?
C85 C84 H84A 108.6 . . ?
C85 C84 H84B 108.6 . . ?
C84 C85 H85A 109.5 . . ?
C84 C85 H85B 109.5 . . ?
C84 C85 H85C 109.5 . . ?
H85A C85 H85B 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
C87 C86 C72 122.8(3) . . ?
C87 C86 C91 117.9(3) . . ?
C91 C86 C72 119.3(3) . . ?
C86 C87 H87 119.6 . . ?
C88 C87 C86 120.8(3) . . ?
C88 C87 H87 119.6 . . ?
C87 C88 H88 119.3 . . ?
C87 C88 C89 121.3(3) . . ?
C89 C88 H88 119.3 . . ?
C88 C89 C90 117.8(3) . . ?
C88 C89 C92 122.8(3) . . ?
C90 C89 C92 119.4(3) . . ?
C89 C90 H90 119.5 . . ?
C91 C90 C89 121.0(3) . . ?
C91 C90 H90 119.5 . . ?
C86 C91 H91 119.4 . . ?
C90 C91 C86 121.1(3) . . ?
C90 C91 H91 119.4 . . ?
C89 C92 H92A 108.7 . . ?
C89 C92 H92B 108.7 . . ?
C89 C92 C93 114.3(3) . . ?
H92A C92 H92B 107.6 . . ?
C93 C92 H92A 108.7 . . ?
C93 C92 H92B 108.7 . . ?
C92 C93 H93A 108.7 . . ?
C92 C93 H93B 108.7 . . ?
C92 C93 C94 114.3(4) . . ?
H93A C93 H93B 107.6 . . ?
C94 C93 H93A 108.7 . . ?
C94 C93 H93B 108.7 . . ?
C93 C94 H94A 108.5 . . ?
C93 C94 H94B 108.5 . . ?
H94A C94 H94B 107.5 . . ?
C95 C94 C93 115.0(4) . . ?
C95 C94 H94A 108.5 . . ?
C95 C94 H94B 108.5 . . ?
C94 C95 H95A 108.3 . . ?
C94 C95 H95B 108.3 . . ?
C94 C95 C96 116.0(5) . . ?
H95A C95 H95B 107.4 . . ?
C96 C95 H95A 108.3 . . ?
C96 C95 H95B 108.3 . . ?
C95 C96 H96A 108.7 . . ?
C95 C96 H96B 108.7 . . ?
H96A C96 H96B 107.6 . . ?
C97 C96 C95 114.0(4) . . ?
C97 C96 H96A 108.7 . . ?
C97 C96 H96B 108.7 . . ?
C96 C97 H97A 109.5 . . ?
C96 C97 H97B 109.5 . . ?
C96 C97 H97C 109.5 . . ?
H97A C97 H97B 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 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 C14 C15 C16 -1.6(4) . . . . ?
S1 C17 C18 C19 -178.3(3) . . . . ?
S1 C17 C18 C22 7.9(7) . . . . ?
S2 C16 C17 S1 178.85(19) . . . . ?
S2 C16 C17 C18 -0.3(4) . . . . ?
S2 C19 C20 C21 -176.0(3) . . . . ?
S2 C19 C20 C23 5.3(7) . . . . ?
O1 C1 C2 C3 172.8(4) . . . . ?
O1 C1 C2 C13 -14.4(7) . . . . ?
O1 C1 C5 C4 -175.9(4) . . . . ?
O1 C1 C5 C6 0.8(7) . . . . ?
C1 C2 C3 C4 7.6(4) . . . . ?
C1 C2 C3 C10 -165.0(4) . . . . ?
C1 C2 C13 C14 11.1(8) . . . . ?
C1 C5 C6 C7 -176.1(4) . . . . ?
C2 C1 C5 C4 3.9(5) . . . . ?
C2 C1 C5 C6 -179.3(4) . . . . ?
C2 C3 C4 C5 -5.2(5) . . . . ?
C2 C3 C4 C9 177.1(4) . . . . ?
C2 C3 C10 C11 -0.6(7) . . . . ?
C2 C3 C10 C12 176.1(4) . . . . ?
C2 C13 C14 S1 11.9(7) . . . . ?
C2 C13 C14 C15 -171.6(4) . . . . ?
C3 C2 C13 C14 -177.3(4) . . . . ?
C3 C4 C5 C1 0.7(5) . . . . ?
C3 C4 C5 C6 -176.3(4) . . . . ?
C3 C4 C9 C8 175.5(4) . . . . ?
C4 C3 C10 C11 -171.9(4) . . . . ?
C4 C3 C10 C12 4.9(7) . . . . ?
C4 C5 C6 C7 0.3(7) . . . . ?
C5 C1 C2 C3 -7.0(5) . . . . ?
C5 C1 C2 C13 165.7(4) . . . . ?
C5 C4 C9 C8 -1.9(6) . . . . ?
C5 C6 C7 C8 -2.0(7) . . . . ?
C6 C7 C8 C9 1.9(7) . . . . ?
C7 C8 C9 C4 0.2(7) . . . . ?
C9 C4 C5 C1 178.7(4) . . . . ?
C9 C4 C5 C6 1.7(6) . . . . ?
C10 C3 C4 C5 167.4(4) . . . . ?
C10 C3 C4 C9 -10.3(7) . . . . ?
C13 C2 C3 C4 -165.4(4) . . . . ?
C13 C2 C3 C10 22.1(7) . . . . ?
C13 C14 C15 C16 -178.6(4) . . . . ?
C14 S1 C17 C16 2.7(3) . . . . ?
C14 S1 C17 C18 -178.4(4) . . . . ?
C14 C15 C16 S2 179.8(3) . . . . ?
C14 C15 C16 C17 3.6(5) . . . . ?
C15 C16 C17 S1 -4.1(4) . . . . ?
C15 C16 C17 C18 176.7(3) . . . . ?
C16 S2 C19 C18 0.4(3) . . . . ?
C16 S2 C19 C20 177.3(4) . . . . ?
C16 C17 C18 C19 0.6(5) . . . . ?
C16 C17 C18 C22 -173.1(4) . . . . ?
C17 S1 C14 C13 176.0(4) . . . . ?
C17 S1 C14 C15 -0.6(3) . . . . ?
C17 C18 C19 S2 -0.6(4) . . . . ?
C17 C18 C19 C20 -178.3(3) . . . . ?
C17 C18 C22 C21 176.9(4) . . . . ?
C17 C18 C22 C24 -64.1(6) . . . . ?
C17 C18 C22 C36 59.7(5) . . . . ?
C18 C19 C20 C21 1.0(4) . . . . ?
C18 C19 C20 C23 -177.7(4) . . . . ?
C18 C22 C24 C25 -6.0(5) . . . . ?
C18 C22 C24 C29 172.2(3) . . . . ?
C18 C22 C36 C37 83.0(4) . . . . ?
C18 C22 C36 C41 -93.2(3) . . . . ?
C19 S2 C16 C15 -176.2(4) . . . . ?
C19 S2 C16 C17 0.0(3) . . . . ?
C19 C18 C22 C21 3.2(4) . . . . ?
C19 C18 C22 C24 122.1(3) . . . . ?
C19 C18 C22 C36 -114.1(3) . . . . ?
C19 C20 C21 C22 1.1(4) . . . . ?
C19 C20 C21 C23 -179.2(3) . . . 2_676 ?
C19 C20 C23 C21 178.9(4) . . . 2_676 ?
C20 C21 C22 C18 -2.5(4) . . . . ?
C20 C21 C22 C24 -123.8(3) . . . . ?
C20 C21 C22 C36 111.2(3) . . . . ?
C21 C20 C23 C21 0.3(6) . . . 2_676 ?
C21 C22 C24 C25 106.4(3) . . . . ?
C21 C22 C24 C29 -75.4(4) . . . . ?
C21 C22 C36 C37 -26.1(4) . . . . ?
C21 C22 C36 C41 157.8(3) . . . . ?
C22 C18 C19 S2 174.9(3) . . . . ?
C22 C18 C19 C20 -2.8(4) . . . . ?
C22 C24 C25 C26 177.8(3) . . . . ?
C22 C24 C29 C28 -178.4(3) . . . . ?
C22 C36 C37 C38 -179.4(3) . . . . ?
C22 C36 C41 C40 179.6(3) . . . . ?
C23 C20 C21 C22 180.0(3) . . . . ?
C23 C20 C21 C23 -0.3(6) . . . 2_676 ?
C23 C21 C22 C18 177.8(4) 2_676 . . . ?
C23 C21 C22 C24 56.5(5) 2_676 . . . ?
C23 C21 C22 C36 -68.5(4) 2_676 . . . ?
C24 C22 C36 C37 -151.2(3) . . . . ?
C24 C22 C36 C41 32.7(4) . . . . ?
C24 C25 C26 C27 0.2(6) . . . . ?
C25 C24 C29 C28 -0.1(5) . . . . ?
C25 C26 C27 C28 0.4(6) . . . . ?
C25 C26 C27 C30 179.3(3) . . . . ?
C26 C27 C28 C29 -1.0(6) . . . . ?
C26 C27 C30 C31 -86.5(4) . . . . ?
C27 C28 C29 C24 0.8(5) . . . . ?
C27 C30 C31 C32 -78.6(4) . . . . ?
C28 C27 C30 C31 92.3(5) . . . . ?
C29 C24 C25 C26 -0.4(5) . . . . ?
C30 C27 C28 C29 -179.8(4) . . . . ?
C30 C31 C32 C33 171.9(3) . . . . ?
C31 C32 C33 C34 175.6(4) . . . . ?
C32 C33 C34 C35 -71.6(5) . . . . ?
C36 C22 C24 C25 -128.0(3) . . . . ?
C36 C22 C24 C29 50.2(4) . . . . ?
C36 C37 C38 C39 0.0(5) . . . . ?
C37 C36 C41 C40 3.3(5) . . . . ?
C37 C38 C39 C40 3.0(5) . . . . ?
C37 C38 C39 C42 -174.3(3) . . . . ?
C38 C39 C40 C41 -2.8(5) . . . . ?
C38 C39 C42 C43 96.5(4) . . . . ?
C39 C40 C41 C36 -0.4(5) . . . . ?
C39 C42 C43 C44 178.0(4) . . . . ?
C40 C39 C42 C43 -80.6(4) . . . . ?
C41 C36 C37 C38 -3.1(5) . . . . ?
C42 C39 C40 C41 174.4(3) . . . . ?
C42 C43 C44 C45 177.6(4) . . . . ?
C43 C44 C45 C46 62.0(5) . . . . ?
C44 C45 C46 C47 58.7(5) . . . . ?
S51 C64 C65 C66 -0.3(4) . . . . ?
S51 C67 C68 C69 177.1(3) . . . . ?
S51 C67 C68 C72 -2.4(7) . . . . ?
S52 C66 C67 S51 -178.75(19) . . . . ?
S52 C66 C67 C68 -0.8(4) . . . . ?
S52 C69 C70 C71 -175.1(3) . . . . ?
S52 C69 C70 C73 0.5(6) . . . 2_666 ?
O51 C51 C52 C53 -170.7(4) . . . . ?
O51 C51 C52 C63 17.7(6) . . . . ?
O51 C51 C55 C54 175.8(4) . . . . ?
O51 C51 C55 C56 -7.4(7) . . . . ?
C51 C52 C53 C54 -12.6(4) . . . . ?
C51 C52 C53 C60 163.7(4) . . . . ?
C51 C52 C63 C64 -10.6(7) . . . . ?
C51 C55 C56 C57 -174.3(4) . . . . ?
C52 C51 C55 C54 -6.7(4) . . . . ?
C52 C51 C55 C56 170.0(4) . . . . ?
C52 C53 C54 C55 8.7(4) . . . . ?
C52 C53 C54 C59 -167.8(4) . . . . ?
C52 C53 C60 C61 2.6(6) . . . . ?
C52 C53 C60 C62 -173.7(4) . . . . ?
C52 C63 C64 S51 -10.5(7) . . . . ?
C52 C63 C64 C65 172.4(4) . . . . ?
C53 C52 C63 C64 179.5(4) . . . . ?
C53 C54 C55 C51 -1.2(4) . . . . ?
C53 C54 C55 C56 -178.2(4) . . . . ?
C53 C54 C59 C58 175.4(4) . . . . ?
C54 C53 C60 C61 178.2(4) . . . . ?
C54 C53 C60 C62 1.9(6) . . . . ?
C54 C55 C56 C57 2.1(6) . . . . ?
C55 C51 C52 C53 11.8(4) . . . . ?
C55 C51 C52 C63 -159.7(4) . . . . ?
C55 C54 C59 C58 -0.8(6) . . . . ?
C55 C56 C57 C58 -1.0(7) . . . . ?
C56 C57 C58 C59 -0.9(7) . . . . ?
C57 C58 C59 C54 1.9(7) . . . . ?
C59 C54 C55 C51 175.8(4) . . . . ?
C59 C54 C55 C56 -1.2(6) . . . . ?
C60 C53 C54 C55 -167.7(4) . . . . ?
C60 C53 C54 C59 15.8(7) . . . . ?
C63 C52 C53 C54 158.9(4) . . . . ?
C63 C52 C53 C60 -24.8(6) . . . . ?
C63 C64 C65 C66 177.2(3) . . . . ?
C64 S51 C67 C66 -1.4(3) . . . . ?
C64 S51 C67 C68 -178.6(4) . . . . ?
C64 C65 C66 S52 179.6(3) . . . . ?
C64 C65 C66 C67 -0.8(5) . . . . ?
C65 C66 C67 S51 1.5(4) . . . . ?
C65 C66 C67 C68 179.5(3) . . . . ?
C66 S52 C69 C68 -1.3(3) . . . . ?
C66 S52 C69 C70 172.4(4) . . . . ?
C66 C67 C68 C69 -0.2(4) . . . . ?
C66 C67 C68 C72 -179.7(4) . . . . ?
C67 S51 C64 C63 -176.3(4) . . . . ?
C67 S51 C64 C65 0.9(3) . . . . ?
C67 C68 C69 S52 1.1(4) . . . . ?
C67 C68 C69 C70 -174.1(3) . . . . ?
C67 C68 C72 C71 172.4(4) . . . . ?
C67 C68 C72 C74 -69.9(5) . . . . ?
C67 C68 C72 C86 54.1(6) . . . . ?
C68 C69 C70 C71 -1.2(4) . . . . ?
C68 C69 C70 C73 174.4(3) . . . 2_666 ?
C68 C72 C74 C75 -94.9(4) . . . . ?
C68 C72 C74 C79 82.0(4) . . . . ?
C68 C72 C86 C87 13.6(5) . . . . ?
C68 C72 C86 C91 -167.2(3) . . . . ?
C69 S52 C66 C65 -179.1(4) . . . . ?
C69 S52 C66 C67 1.2(3) . . . . ?
C69 C68 C72 C71 -7.0(4) . . . . ?
C69 C68 C72 C74 110.6(3) . . . . ?
C69 C68 C72 C86 -125.4(3) . . . . ?
C69 C70 C71 C72 -3.6(4) . . . . ?
C69 C70 C71 C73 175.9(3) . . . . ?
C70 C71 C72 C68 6.3(4) . . . . ?
C70 C71 C72 C74 -107.3(3) . . . . ?
C70 C71 C72 C86 127.4(3) . . . . ?
C70 C71 C73 C70 0.1(5) . . . 2_666 ?
C71 C72 C74 C75 14.0(4) . . . . ?
C71 C72 C74 C79 -169.1(3) . . . . ?
C71 C72 C86 C87 -98.3(4) . . . . ?
C71 C72 C86 C91 80.9(4) . . . . ?
C72 C68 C69 S52 -179.3(2) . . . . ?
C72 C68 C69 C70 5.5(4) . . . . ?
C72 C71 C73 C70 179.5(3) . . . 2_666 ?
C72 C74 C75 C76 177.4(3) . . . . ?
C72 C74 C79 C78 -178.2(3) . . . . ?
C72 C86 C87 C88 -179.1(3) . . . . ?
C72 C86 C91 C90 179.9(4) . . . . ?
C73 C70 C71 C72 -179.6(3) 2_666 . . . ?
C73 C70 C71 C73 -0.2(6) 2_666 . . . ?
C73 C71 C72 C68 -173.1(3) . . . . ?
C73 C71 C72 C74 73.3(4) . . . . ?
C73 C71 C72 C86 -52.1(4) . . . . ?
C74 C72 C86 C87 135.5(3) . . . . ?
C74 C72 C86 C91 -45.2(4) . . . . ?
C74 C75 C76 C77 1.1(5) . . . . ?
C75 C74 C79 C78 -1.0(5) . . . . ?
C75 C76 C77 C78 -1.9(5) . . . . ?
C75 C76 C77 C80 176.0(3) . . . . ?
C76 C77 C78 C79 1.2(5) . . . . ?
C76 C77 C80 C81 128.5(4) . . . . ?
C77 C78 C79 C74 0.2(6) . . . . ?
C77 C80 C81 C82 -63.0(5) . . . . ?
C78 C77 C80 C81 -53.6(5) . . . . ?
C79 C74 C75 C76 0.4(5) . . . . ?
C80 C77 C78 C79 -176.7(3) . . . . ?
C80 C81 C82 C83 -171.0(4) . . . . ?
C81 C82 C83 C84 -178.5(4) . . . . ?
C82 C83 C84 C85 -178.4(4) . . . . ?
C86 C72 C74 C75 139.1(3) . . . . ?
C86 C72 C74 C79 -43.9(4) . . . . ?
C86 C87 C88 C89 -1.1(6) . . . . ?
C87 C86 C91 C90 -0.8(6) . . . . ?
C87 C88 C89 C90 -0.3(6) . . . . ?
C87 C88 C89 C92 178.7(4) . . . . ?
C88 C89 C90 C91 1.2(6) . . . . ?
C88 C89 C92 C93 109.4(5) . . . . ?
C89 C90 C91 C86 -0.6(6) . . . . ?
C89 C92 C93 C94 167.7(4) . . . . ?
C90 C89 C92 C93 -71.6(5) . . . . ?
C91 C86 C87 C88 1.7(6) . . . . ?
C92 C89 C90 C91 -177.9(4) . . . . ?
C92 C93 C94 C95 -179.3(4) . . . . ?
C93 C94 C95 C96 172.7(4) . . . . ?
C94 C95 C96 C97 -70.6(6) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id 'Sample #1:ITIC'
_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 2.947
_oxdiff_exptl_absorpt_empirical_full_min 0.424
####################################################################### 
# 
# 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_ICA
_database_code_depnum_ccdc_archive 'CCDC 1942952'
loop_
_audit_author_name
_audit_author_address
'Peter Horton'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2019-07-24 deposited with the CCDC.	2019-11-18 downloaded from the CCDC.
;

#2018ncs0776_1b

_audit_creation_date             2019-05-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C23 H20 N2 O S'
_chemical_formula_sum            'C23 H20 N2 O S'
_chemical_formula_weight         372.47
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C23 H20 N2 O S '
_chemical_oxdiff_usercomment     'Sample #23:OPN207'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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                   7.71450(10)
_cell_length_b                   10.8650(2)
_cell_length_c                   12.5062(3)
_cell_angle_alpha                110.002(2)
_cell_angle_beta                 96.063(2)
_cell_angle_gamma                104.290(2)
_cell_volume                     933.52(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14167
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.8630
_cell_measurement_theta_min      3.8520
_shelx_estimated_absorpt_T_max   0.879
_shelx_estimated_absorpt_T_min   0.655
_exptl_absorpt_coefficient_mu    1.650
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of Pet. ether and chloroform'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16421
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.234
_diffrn_reflns_theta_min         3.846
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -89.00  89.00   0.50    0.50    --    0.00  30.00-180.00  356
  2  ω    -84.00  94.00   0.50    0.50    --    5.00  39.00  30.00  356
  3  ω   -179.00  -1.00   0.50    0.50    --  -90.00  49.00 150.00  356
  4  ω   -179.00  -1.00   0.50    0.50    --  -90.00  59.00 -98.68  356
  5  ω   -179.00  -1.00   0.50    0.50    --  -90.00  49.00  30.00  356
  6  ω   -179.00  -1.00   0.50    0.50    --  -90.00  58.00-161.35  356
  7  ω   -179.00  -1.00   0.50    0.50    --  -90.00  59.00  64.44  356
  8  ω   -179.00  -1.00   0.50    0.50    --  -90.00  59.00 106.01  356
  9  ω   -179.00  -1.00   0.50    0.50    --  -90.00  59.00 106.01  356
 10  ω   -179.00  -1.00   0.50    0.50    --  -90.00  59.00 -47.44  356
 11  ω   -179.00  -1.00   0.50    0.50    --  -90.00  20.00 -30.00  356
 12  ω   -139.00 -17.00   0.50    0.50    --  -90.00  39.00-150.00  244
 13  ω   -177.00-105.00   0.50    0.50    --  -90.00  59.00 160.65  144
 14  ω   -178.00 -80.00   0.50    0.50    --  -90.00  58.00 -27.38  196
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter χ goniometer'
_diffrn_measurement_device_type  
'Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1492907000
_diffrn_orient_matrix_UB_12      -0.1402163000
_diffrn_orient_matrix_UB_13      -0.0455696000
_diffrn_orient_matrix_UB_21      -0.1166921000
_diffrn_orient_matrix_UB_22      0.0508869000
_diffrn_orient_matrix_UB_23      -0.0732527000
_diffrn_orient_matrix_UB_31      0.0921719000
_diffrn_orient_matrix_UB_32      -0.0530772000
_diffrn_orient_matrix_UB_33      -0.1025912000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3349
_reflns_number_total             3390
_reflns_odcompleteness_completeness 99.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3390
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0292
_refine_ls_restrained_S_all      1.047
_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)+(0.0383P)²+0.3991P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0761
_refine_special_details          ?
_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.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C15(H15), C16(H16)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C)
;
_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
S1 S 0.65598(4) 0.43014(3) 0.67312(2) 0.01760(10) Uani 1 1 d . . . . .
O1 O 0.73736(13) 0.61899(9) 0.57439(7) 0.0254(2) Uani 1 1 d . . . . .
N1 N 0.87375(16) 0.09799(11) 0.23494(10) 0.0282(3) Uani 1 1 d . . . . .
N2 N 0.98656(15) 0.34421(12) 0.03564(9) 0.0268(2) Uani 1 1 d . . . . .
C1 C 0.77764(15) 0.57747(12) 0.47951(10) 0.0187(2) Uani 1 1 d . . . . .
C2 C 0.78588(15) 0.43727(12) 0.41396(10) 0.0180(2) Uani 1 1 d . . . . .
C3 C 0.84664(15) 0.43739(12) 0.30652(10) 0.0175(2) Uani 1 1 d . . . . .
C4 C 0.86575(15) 0.57622(12) 0.30473(10) 0.0178(2) Uani 1 1 d . . . . .
C5 C 0.82755(15) 0.65845(12) 0.40733(10) 0.0186(2) Uani 1 1 d . . . . .
C6 C 0.83721(16) 0.79460(13) 0.43178(11) 0.0218(3) Uani 1 1 d . . . . .
H6 H 0.811707 0.848883 0.502305 0.026 Uiso 1 1 calc R . . . .
C7 C 0.88546(17) 0.84912(13) 0.34969(11) 0.0232(3) Uani 1 1 d . . . . .
H7 H 0.892865 0.942115 0.363851 0.028 Uiso 1 1 calc R . . . .
C8 C 0.92300(16) 0.76854(13) 0.24690(11) 0.0227(3) Uani 1 1 d . . . . .
H8 H 0.955254 0.807802 0.191850 0.027 Uiso 1 1 calc R . . . .
C9 C 0.91458(16) 0.63187(13) 0.22252(11) 0.0207(3) Uani 1 1 d . . . . .
H9 H 0.941186 0.578069 0.152227 0.025 Uiso 1 1 calc R . . . .
C10 C 0.88606(16) 0.33346(12) 0.22396(10) 0.0184(2) Uani 1 1 d . . . . .
C11 C 0.87864(16) 0.20321(13) 0.23164(10) 0.0210(3) Uani 1 1 d . . . . .
C12 C 0.94287(16) 0.34314(12) 0.12047(11) 0.0205(3) Uani 1 1 d . . . . .
C13 C 0.73926(16) 0.32742(12) 0.44651(10) 0.0191(2) Uani 1 1 d . . . . .
H13 H 0.744679 0.244579 0.389843 0.023 Uiso 1 1 calc R . . . .
C14 C 0.68426(16) 0.31057(12) 0.54728(10) 0.0187(2) Uani 1 1 d . . . . .
C15 C 0.65450(17) 0.18402(12) 0.55808(11) 0.0212(3) Uani 1 1 d . . . . .
H15 H 0.662579 0.104344 0.498603 0.025 Uiso 1 1 calc R . . . .
C16 C 0.61176(16) 0.18440(12) 0.66388(11) 0.0209(3) Uani 1 1 d . . . . .
H16 H 0.588038 0.105764 0.683717 0.025 Uiso 1 1 calc R . . . .
C17 C 0.60780(15) 0.31116(12) 0.73620(10) 0.0184(2) Uani 1 1 d . . . . .
C18 C 0.56905(17) 0.35330(12) 0.85656(10) 0.0201(3) Uani 1 1 d . . . . .
H18A H 0.469953 0.396615 0.858585 0.024 Uiso 1 1 calc R . . . .
H18B H 0.679730 0.423258 0.911831 0.024 Uiso 1 1 calc R . . . .
C19 C 0.51322(17) 0.23461(12) 0.89704(10) 0.0195(2) Uani 1 1 d . . . . .
H19A H 0.409787 0.160462 0.838210 0.023 Uiso 1 1 calc R . . . .
H19B H 0.616917 0.197184 0.903147 0.023 Uiso 1 1 calc R . . . .
C20 C 0.45701(17) 0.27837(12) 1.01423(10) 0.0199(3) Uani 1 1 d . . . . .
H20A H 0.557673 0.356472 1.071800 0.024 Uiso 1 1 calc R . . . .
H20B H 0.348635 0.310545 1.006729 0.024 Uiso 1 1 calc R . . . .
C21 C 0.41195(17) 0.16274(12) 1.05904(10) 0.0209(3) Uani 1 1 d . . . . .
H21A H 0.312024 0.084479 1.001011 0.025 Uiso 1 1 calc R . . . .
H21B H 0.520666 0.130993 1.066736 0.025 Uiso 1 1 calc R . . . .
C22 C 0.35439(18) 0.20442(13) 1.17574(11) 0.0222(3) Uani 1 1 d . . . . .
H22A H 0.239703 0.228735 1.166672 0.027 Uiso 1 1 calc R . . . .
H22B H 0.449827 0.287212 1.232391 0.027 Uiso 1 1 calc R . . . .
C23 C 0.3246(2) 0.09129(14) 1.22368(12) 0.0293(3) Uani 1 1 d . . . . .
H23A H 0.226903 0.010179 1.169407 0.044 Uiso 1 1 calc GR . . . .
H23B H 0.289897 0.123774 1.299202 0.044 Uiso 1 1 calc GR . . . .
H23C H 0.437910 0.067077 1.233311 0.044 Uiso 1 1 calc GR . . . .


_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 C14 1.7396(12) . ?
S1 C17 1.7187(12) . ?
O1 C1 1.2202(15) . ?
N1 C11 1.1495(17) . ?
N2 C12 1.1495(17) . ?
C1 C2 1.4835(16) . ?
C1 C5 1.4788(16) . ?
C2 C3 1.4693(16) . ?
C2 C13 1.3679(17) . ?
C3 C4 1.4871(16) . ?
C3 C10 1.3682(17) . ?
C4 C5 1.3990(17) . ?
C4 C9 1.3997(17) . ?
C5 C6 1.3851(17) . ?
C6 H6 0.9500 . ?
C6 C7 1.3898(17) . ?
C7 H7 0.9500 . ?
C7 C8 1.3918(19) . ?
C8 H8 0.9500 . ?
C8 C9 1.3930(17) . ?
C9 H9 0.9500 . ?
C10 C11 1.4385(16) . ?
C10 C12 1.4381(16) . ?
C13 H13 0.9500 . ?
C13 C14 1.4262(16) . ?
C14 C15 1.3925(17) . ?
C15 H15 0.9500 . ?
C15 C16 1.3959(17) . ?
C16 H16 0.9500 . ?
C16 C17 1.3748(17) . ?
C17 C18 1.5020(16) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.5242(16) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.5237(16) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.5233(16) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.5220(16) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.5222(17) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 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
C17 S1 C14 92.26(6) . . ?
O1 C1 C2 127.17(11) . . ?
O1 C1 C5 126.17(11) . . ?
C5 C1 C2 106.66(10) . . ?
C3 C2 C1 107.50(10) . . ?
C13 C2 C1 125.85(11) . . ?
C13 C2 C3 126.62(11) . . ?
C2 C3 C4 107.08(10) . . ?
C10 C3 C2 127.90(11) . . ?
C10 C3 C4 124.98(11) . . ?
C5 C4 C3 108.98(10) . . ?
C5 C4 C9 119.47(11) . . ?
C9 C4 C3 131.54(11) . . ?
C4 C5 C1 109.69(10) . . ?
C6 C5 C1 127.85(11) . . ?
C6 C5 C4 122.46(11) . . ?
C5 C6 H6 121.1 . . ?
C5 C6 C7 117.77(12) . . ?
C7 C6 H6 121.1 . . ?
C6 C7 H7 119.7 . . ?
C6 C7 C8 120.51(11) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 H8 119.1 . . ?
C7 C8 C9 121.79(11) . . ?
C9 C8 H8 119.1 . . ?
C4 C9 H9 121.0 . . ?
C8 C9 C4 118.00(11) . . ?
C8 C9 H9 121.0 . . ?
C3 C10 C11 123.96(11) . . ?
C3 C10 C12 123.70(11) . . ?
C12 C10 C11 112.33(10) . . ?
N1 C11 C10 178.21(13) . . ?
N2 C12 C10 176.74(13) . . ?
C2 C13 H13 113.1 . . ?
C2 C13 C14 133.75(11) . . ?
C14 C13 H13 113.1 . . ?
C13 C14 S1 130.23(9) . . ?
C15 C14 S1 109.35(9) . . ?
C15 C14 C13 120.32(11) . . ?
C14 C15 H15 122.9 . . ?
C14 C15 C16 114.17(11) . . ?
C16 C15 H15 122.9 . . ?
C15 C16 H16 123.7 . . ?
C17 C16 C15 112.54(11) . . ?
C17 C16 H16 123.7 . . ?
C16 C17 S1 111.67(9) . . ?
C16 C17 C18 128.62(11) . . ?
C18 C17 S1 119.71(9) . . ?
C17 C18 H18A 108.8 . . ?
C17 C18 H18B 108.8 . . ?
C17 C18 C19 113.78(10) . . ?
H18A C18 H18B 107.7 . . ?
C19 C18 H18A 108.8 . . ?
C19 C18 H18B 108.8 . . ?
C18 C19 H19A 109.1 . . ?
C18 C19 H19B 109.1 . . ?
H19A C19 H19B 107.9 . . ?
C20 C19 C18 112.32(10) . . ?
C20 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
C19 C20 H20A 109.0 . . ?
C19 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C21 C20 C19 112.79(10) . . ?
C21 C20 H20A 109.0 . . ?
C21 C20 H20B 109.0 . . ?
C20 C21 H21A 108.9 . . ?
C20 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
C22 C21 C20 113.51(10) . . ?
C22 C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
C21 C22 H22A 109.0 . . ?
C21 C22 H22B 109.0 . . ?
C21 C22 C23 112.74(10) . . ?
H22A C22 H22B 107.8 . . ?
C23 C22 H22A 109.0 . . ?
C23 C22 H22B 109.0 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 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 C14 C15 C16 -0.33(14) . . . . ?
S1 C17 C18 C19 175.19(8) . . . . ?
O1 C1 C2 C3 -178.08(11) . . . . ?
O1 C1 C2 C13 3.9(2) . . . . ?
O1 C1 C5 C4 179.69(11) . . . . ?
O1 C1 C5 C6 -0.5(2) . . . . ?
C1 C2 C3 C4 -2.85(12) . . . . ?
C1 C2 C3 C10 174.93(11) . . . . ?
C1 C2 C13 C14 -4.7(2) . . . . ?
C1 C5 C6 C7 -179.23(11) . . . . ?
C2 C1 C5 C4 -0.45(13) . . . . ?
C2 C1 C5 C6 179.35(11) . . . . ?
C2 C3 C4 C5 2.63(13) . . . . ?
C2 C3 C4 C9 -178.21(12) . . . . ?
C2 C3 C10 C11 -1.90(19) . . . . ?
C2 C3 C10 C12 179.25(11) . . . . ?
C2 C13 C14 S1 -0.5(2) . . . . ?
C2 C13 C14 C15 -176.47(13) . . . . ?
C3 C2 C13 C14 177.61(12) . . . . ?
C3 C4 C5 C1 -1.34(13) . . . . ?
C3 C4 C5 C6 178.85(11) . . . . ?
C3 C4 C9 C8 -179.11(11) . . . . ?
C4 C3 C10 C11 175.50(11) . . . . ?
C4 C3 C10 C12 -3.35(18) . . . . ?
C4 C5 C6 C7 0.54(18) . . . . ?
C5 C1 C2 C3 2.06(12) . . . . ?
C5 C1 C2 C13 -175.96(11) . . . . ?
C5 C4 C9 C8 -0.02(17) . . . . ?
C5 C6 C7 C8 -0.20(18) . . . . ?
C6 C7 C8 C9 -0.24(19) . . . . ?
C7 C8 C9 C4 0.35(18) . . . . ?
C9 C4 C5 C1 179.38(10) . . . . ?
C9 C4 C5 C6 -0.43(17) . . . . ?
C10 C3 C4 C5 -175.23(11) . . . . ?
C10 C3 C4 C9 3.9(2) . . . . ?
C13 C2 C3 C4 175.16(11) . . . . ?
C13 C2 C3 C10 -7.1(2) . . . . ?
C13 C14 C15 C16 176.44(11) . . . . ?
C14 S1 C17 C16 -0.40(10) . . . . ?
C14 S1 C17 C18 179.37(10) . . . . ?
C14 C15 C16 C17 0.04(16) . . . . ?
C15 C16 C17 S1 0.28(14) . . . . ?
C15 C16 C17 C18 -179.47(11) . . . . ?
C16 C17 C18 C19 -5.08(18) . . . . ?
C17 S1 C14 C13 -175.94(12) . . . . ?
C17 S1 C14 C15 0.41(9) . . . . ?
C17 C18 C19 C20 -174.38(10) . . . . ?
C18 C19 C20 C21 -176.53(10) . . . . ?
C19 C20 C21 C22 -179.65(10) . . . . ?
C20 C21 C22 C23 -175.43(11) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id 'Sample #23:OPN207'
_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 2.377
_oxdiff_exptl_absorpt_empirical_full_min 0.721
####################################################################### 
# 
# 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_IDIC
_database_code_depnum_ccdc_archive 'CCDC 1942951'
loop_
_audit_author_name
_audit_author_address
'Peter Horton'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2019-07-24 deposited with the CCDC.	2019-11-18 downloaded from the CCDC.
;

#2018ncs0658_1b

_audit_creation_date             2019-05-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H66 N4 O2 S2'
_chemical_formula_sum            'C66 H66 N4 O2 S2'
_chemical_formula_weight         1011.34
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C66 H66 N4 O2 S2 '
_chemical_oxdiff_usercomment     4:IDIC
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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                   8.6679(4)
_cell_length_b                   12.5073(7)
_cell_length_c                   13.5784(6)
_cell_angle_alpha                72.096(4)
_cell_angle_beta                 75.545(4)
_cell_angle_gamma                88.839(4)
_cell_volume                     1353.88(12)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7308
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.9060
_cell_measurement_theta_min      3.5270
_shelx_estimated_absorpt_T_max   0.975
_shelx_estimated_absorpt_T_min   0.883
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             538
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of Pet. ether and chloroform'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22142
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_min         3.538
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -84.00  94.00   0.50    0.75    --    5.00  50.00-129.00  356
  2  ω    -89.00  89.00   0.50    0.75    --    0.00   0.00-180.00  356
  3  ω    -89.00  89.00   0.50    0.75    --    0.00  50.00-129.00  356
  4  ω   -179.00  -1.00   0.50    3.00    --  -90.00  50.00-129.00  356
  5  ω   -179.00  -1.00   0.50    3.00    --  -90.00  52.00  -1.63  356
  6  ω   -179.00  -1.00   0.50    3.00    --  -90.00  59.00 117.15  356
  7  ω   -179.00  -1.00   0.50    3.00    --  -90.00  39.00  90.00  356
  8  ω   -179.00  -1.00   0.50    3.00    --  -90.00  59.00 -22.68  356
  9  ω   -179.00 -27.00   0.50    3.00    --  -90.00  59.00 -90.93  304
 10  ω    -53.00 -26.00   0.50    3.00    --  -90.00  59.00 166.97   54
 11  ω   -178.00 -98.00   0.50    3.00    --  -90.00  39.00-180.00  160
 12  ω    -60.00 -33.00   0.50    3.00    --  -90.00  39.00-180.00   54
 13  ω    -30.00  -2.00   0.50    3.00    --  -90.00  39.00-180.00   56
 14  ω   -139.00 -49.00   0.50    3.00    --  -90.00  57.00  61.10  180
 15  ω    -40.00 -15.00   0.50    3.00    --  -90.00  57.00  61.10   50
 16  ω   -178.00 -92.00   0.50    3.00    --  -90.00  59.00 166.97  172
 17  ω   -179.00 -19.00   0.50    3.00    --  -90.00  30.00 -30.00  320
 18  ω   -177.00 -21.00   0.50    3.00    --  -90.00  57.00  42.02  312
 19  ω   -178.00 -78.00   0.50    3.00    --  -90.00  59.00-132.34  200
 20  ω   -174.00-126.00   0.50    3.00    --  -90.00  59.00 112.91   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter χ goniometer'
_diffrn_measurement_device_type  
'Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0875332000
_diffrn_orient_matrix_UB_12      0.0331645000
_diffrn_orient_matrix_UB_13      0.0730581000
_diffrn_orient_matrix_UB_21      -0.0106615000
_diffrn_orient_matrix_UB_22      0.1253708000
_diffrn_orient_matrix_UB_23      -0.0595818000
_diffrn_orient_matrix_UB_31      -0.1613659000
_diffrn_orient_matrix_UB_32      0.0006484000
_diffrn_orient_matrix_UB_33      0.0795234000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4117
_reflns_number_total             4925
_reflns_odcompleteness_completeness 99.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         4925
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0545
_refine_ls_restrained_S_all      1.056
_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)+(0.0964P)²+0.2935P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1508
_refine_special_details          ?
_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.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,
 H26B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
 C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C15(H15), C21(H21)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C33(H33A,H33B,H33C)
;
_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
S1 S 0.37910(6) 0.51913(4) 0.72337(4) 0.02851(17) Uani 1 1 d . . . . .
O1 O 0.60105(17) 0.44050(13) 0.59247(12) 0.0353(4) Uani 1 1 d . . . . .
N1 N 0.7056(2) 0.96679(17) 0.38487(15) 0.0409(5) Uani 1 1 d . . . . .
N2 N 1.0525(2) 0.87085(17) 0.15430(16) 0.0438(5) Uani 1 1 d . . . . .
C1 C 0.6938(2) 0.51309(18) 0.52152(16) 0.0300(5) Uani 1 1 d . . . . .
C2 C 0.6863(2) 0.63645(18) 0.49482(16) 0.0284(4) Uani 1 1 d . . . . .
C3 C 0.8140(2) 0.68678(18) 0.39724(16) 0.0283(4) Uani 1 1 d . . . . .
C4 C 0.9062(2) 0.59399(18) 0.37153(16) 0.0301(4) Uani 1 1 d . . . . .
C5 C 0.8367(2) 0.49167(18) 0.44587(16) 0.0296(4) Uani 1 1 d . . . . .
C6 C 0.8994(3) 0.38948(19) 0.44469(17) 0.0329(5) Uani 1 1 d . . . . .
H6 H 0.849313 0.320993 0.495747 0.039 Uiso 1 1 calc R . . . .
C7 C 1.0381(3) 0.39004(19) 0.36648(17) 0.0348(5) Uani 1 1 d . . . . .
H7 H 1.084636 0.321151 0.364143 0.042 Uiso 1 1 calc R . . . .
C8 C 1.1090(3) 0.4907(2) 0.29176(17) 0.0361(5) Uani 1 1 d . . . . .
H8 H 1.203335 0.489251 0.238608 0.043 Uiso 1 1 calc R . . . .
C9 C 1.0457(3) 0.59342(19) 0.29261(17) 0.0333(5) Uani 1 1 d . . . . .
H9 H 1.095717 0.661643 0.241017 0.040 Uiso 1 1 calc R . . . .
C10 C 0.8451(2) 0.79794(18) 0.33722(16) 0.0300(5) Uani 1 1 d . . . . .
C11 C 0.7632(2) 0.88902(19) 0.36566(16) 0.0319(5) Uani 1 1 d . . . . .
C12 C 0.9628(3) 0.83599(18) 0.23632(17) 0.0341(5) Uani 1 1 d . . . . .
C13 C 0.5863(2) 0.69265(18) 0.55404(16) 0.0292(4) Uani 1 1 d . . . . .
H13 H 0.602164 0.772216 0.524605 0.035 Uiso 1 1 calc R . . . .
C14 C 0.4627(2) 0.65616(18) 0.65116(16) 0.0289(4) Uani 1 1 d . . . . .
C15 C 0.3915(2) 0.73344(18) 0.70152(16) 0.0291(4) Uani 1 1 d . . . . .
H15 H 0.419785 0.811957 0.674403 0.035 Uiso 1 1 calc R . . . .
C16 C 0.2749(2) 0.68328(18) 0.79546(16) 0.0284(4) Uani 1 1 d . . . . .
C17 C 0.2522(2) 0.56895(17) 0.81449(16) 0.0272(4) Uani 1 1 d . . . . .
C18 C 0.1241(2) 0.52021(18) 0.90973(15) 0.0277(4) Uani 1 1 d . . . . .
C19 C 0.0752(2) 0.60839(18) 0.95364(16) 0.0279(4) Uani 1 1 d . . . . .
C20 C 0.1737(2) 0.71861(17) 0.88757(16) 0.0280(4) Uani 1 1 d . . . . .
C21 C -0.0499(2) 0.58869(17) 1.04444(15) 0.0280(4) Uani 1 1 d . . . . .
H21 H -0.084505 0.646880 1.074743 0.034 Uiso 1 1 calc R . . . .
C22 C 0.2831(2) 0.75239(18) 0.94947(16) 0.0302(5) Uani 1 1 d . . . . .
H22A H 0.345975 0.822746 0.902295 0.036 Uiso 1 1 calc R . . . .
H22B H 0.214077 0.769507 1.012113 0.036 Uiso 1 1 calc R . . . .
C23 C 0.3986(3) 0.66645(19) 0.98902(17) 0.0343(5) Uani 1 1 d . . . . .
H23A H 0.454111 0.637759 0.929986 0.041 Uiso 1 1 calc R . . . .
H23B H 0.337226 0.602049 1.047884 0.041 Uiso 1 1 calc R . . . .
C24 C 0.5232(3) 0.7143(2) 1.02900(18) 0.0351(5) Uani 1 1 d . . . . .
H24A H 0.603130 0.657761 1.043014 0.042 Uiso 1 1 calc R . . . .
H24B H 0.579343 0.781744 0.971460 0.042 Uiso 1 1 calc R . . . .
C25 C 0.4558(3) 0.7468(2) 1.13017(18) 0.0373(5) Uani 1 1 d . . . . .
H25A H 0.403313 0.678804 1.188573 0.045 Uiso 1 1 calc R . . . .
H25B H 0.373021 0.801282 1.117141 0.045 Uiso 1 1 calc R . . . .
C26 C 0.5803(3) 0.7985(2) 1.16710(19) 0.0412(5) Uani 1 1 d . . . . .
H26A H 0.532498 0.800849 1.240611 0.049 Uiso 1 1 calc R . . . .
H26B H 0.671039 0.749229 1.169888 0.049 Uiso 1 1 calc R . . . .
C27 C 0.6433(4) 0.9163(2) 1.0957(2) 0.0552(7) Uani 1 1 d . . . . .
H27A H 0.696926 0.914137 1.023728 0.083 Uiso 1 1 calc GR . . . .
H27B H 0.719325 0.945202 1.125396 0.083 Uiso 1 1 calc GR . . . .
H27C H 0.554239 0.965629 1.091767 0.083 Uiso 1 1 calc GR . . . .
C28 C 0.0693(2) 0.81730(18) 0.85313(16) 0.0303(5) Uani 1 1 d . . . . .
H28A H -0.002043 0.828184 0.918249 0.036 Uiso 1 1 calc R . . . .
H28B H 0.139595 0.886685 0.815178 0.036 Uiso 1 1 calc R . . . .
C29 C -0.0325(3) 0.80266(18) 0.78125(17) 0.0335(5) Uani 1 1 d . . . . .
H29A H 0.038163 0.791851 0.715879 0.040 Uiso 1 1 calc R . . . .
H29B H -0.104006 0.733829 0.819079 0.040 Uiso 1 1 calc R . . . .
C30 C -0.1326(3) 0.90181(19) 0.74894(18) 0.0344(5) Uani 1 1 d . . . . .
H30A H -0.061517 0.971249 0.715053 0.041 Uiso 1 1 calc R . . . .
H30B H -0.207499 0.909787 0.814141 0.041 Uiso 1 1 calc R . . . .
C31 C -0.2278(3) 0.8910(2) 0.67176(19) 0.0383(5) Uani 1 1 d . . . . .
H31A H -0.152197 0.890101 0.604068 0.046 Uiso 1 1 calc R . . . .
H31B H -0.290873 0.817961 0.702829 0.046 Uiso 1 1 calc R . . . .
C32 C -0.3405(3) 0.9845(2) 0.6463(2) 0.0411(5) Uani 1 1 d . . . . .
H32A H -0.401269 0.968101 0.599204 0.049 Uiso 1 1 calc R . . . .
H32B H -0.418151 0.983958 0.713704 0.049 Uiso 1 1 calc R . . . .
C33 C -0.2588(3) 1.1010(2) 0.5924(2) 0.0530(7) Uani 1 1 d . . . . .
H33A H -0.181063 1.102537 0.525638 0.079 Uiso 1 1 calc GR . . . .
H33B H -0.203739 1.120182 0.640136 0.079 Uiso 1 1 calc GR . . . .
H33C H -0.338609 1.155878 0.576410 0.079 Uiso 1 1 calc GR . . . .


_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 C14 1.757(2) . ?
S1 C17 1.702(2) . ?
O1 C1 1.226(3) . ?
N1 C11 1.155(3) . ?
N2 C12 1.148(3) . ?
C1 C2 1.476(3) . ?
C1 C5 1.477(3) . ?
C2 C3 1.470(3) . ?
C2 C13 1.367(3) . ?
C3 C4 1.476(3) . ?
C3 C10 1.371(3) . ?
C4 C5 1.398(3) . ?
C4 C9 1.403(3) . ?
C5 C6 1.382(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.390(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.388(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.389(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.432(3) . ?
C10 C12 1.437(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.428(3) . ?
C14 C15 1.398(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.390(3) . ?
C16 C17 1.382(3) . ?
C16 C20 1.518(3) . ?
C17 C18 1.450(3) . ?
C18 C19 1.418(3) . ?
C18 C21 1.404(3) 2_567 ?
C19 C20 1.529(3) . ?
C19 C21 1.383(3) . ?
C20 C22 1.555(3) . ?
C20 C28 1.541(3) . ?
C21 H21 0.9500 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.522(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.529(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.525(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.527(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.516(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.520(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.515(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.523(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.521(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.514(3) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 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
C17 S1 C14 90.27(10) . . ?
O1 C1 C2 127.68(19) . . ?
O1 C1 C5 125.4(2) . . ?
C2 C1 C5 106.92(17) . . ?
C3 C2 C1 107.05(17) . . ?
C13 C2 C1 126.13(19) . . ?
C13 C2 C3 126.68(19) . . ?
C2 C3 C4 107.29(17) . . ?
C10 C3 C2 128.32(19) . . ?
C10 C3 C4 124.38(18) . . ?
C5 C4 C3 109.14(17) . . ?
C5 C4 C9 118.9(2) . . ?
C9 C4 C3 131.9(2) . . ?
C4 C5 C1 109.28(18) . . ?
C6 C5 C1 128.0(2) . . ?
C6 C5 C4 122.67(19) . . ?
C5 C6 H6 121.0 . . ?
C5 C6 C7 117.9(2) . . ?
C7 C6 H6 121.0 . . ?
C6 C7 H7 119.8 . . ?
C8 C7 C6 120.4(2) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 H8 119.1 . . ?
C7 C8 C9 121.8(2) . . ?
C9 C8 H8 119.1 . . ?
C4 C9 H9 120.8 . . ?
C8 C9 C4 118.4(2) . . ?
C8 C9 H9 120.8 . . ?
C3 C10 C11 124.58(18) . . ?
C3 C10 C12 123.23(19) . . ?
C11 C10 C12 112.17(18) . . ?
N1 C11 C10 175.7(2) . . ?
N2 C12 C10 176.6(2) . . ?
C2 C13 H13 113.5 . . ?
C2 C13 C14 133.1(2) . . ?
C14 C13 H13 113.5 . . ?
C13 C14 S1 128.52(17) . . ?
C15 C14 S1 110.88(15) . . ?
C15 C14 C13 120.60(19) . . ?
C14 C15 H15 123.6 . . ?
C16 C15 C14 112.89(19) . . ?
C16 C15 H15 123.6 . . ?
C15 C16 C20 137.01(19) . . ?
C17 C16 C15 111.97(19) . . ?
C17 C16 C20 110.82(17) . . ?
C16 C17 S1 113.89(15) . . ?
C16 C17 C18 110.65(18) . . ?
C18 C17 S1 135.46(16) . . ?
C19 C18 C17 106.21(18) . . ?
C21 C18 C17 131.52(19) 2_567 . ?
C21 C18 C19 122.24(18) 2_567 . ?
C18 C19 C20 111.69(17) . . ?
C21 C19 C18 120.03(19) . . ?
C21 C19 C20 128.27(19) . . ?
C16 C20 C19 100.10(16) . . ?
C16 C20 C22 109.72(16) . . ?
C16 C20 C28 114.10(16) . . ?
C19 C20 C22 111.68(16) . . ?
C19 C20 C28 112.68(16) . . ?
C28 C20 C22 108.42(16) . . ?
C18 C21 H21 121.1 2_567 . ?
C19 C21 C18 117.73(19) . 2_567 ?
C19 C21 H21 121.1 . . ?
C20 C22 H22A 108.1 . . ?
C20 C22 H22B 108.1 . . ?
H22A C22 H22B 107.3 . . ?
C23 C22 C20 116.72(18) . . ?
C23 C22 H22A 108.1 . . ?
C23 C22 H22B 108.1 . . ?
C22 C23 H23A 108.9 . . ?
C22 C23 H23B 108.9 . . ?
C22 C23 C24 113.22(19) . . ?
H23A C23 H23B 107.7 . . ?
C24 C23 H23A 108.9 . . ?
C24 C23 H23B 108.9 . . ?
C23 C24 H24A 108.6 . . ?
C23 C24 H24B 108.6 . . ?
H24A C24 H24B 107.6 . . ?
C25 C24 C23 114.64(18) . . ?
C25 C24 H24A 108.6 . . ?
C25 C24 H24B 108.6 . . ?
C24 C25 H25A 108.7 . . ?
C24 C25 H25B 108.7 . . ?
C24 C25 C26 114.21(19) . . ?
H25A C25 H25B 107.6 . . ?
C26 C25 H25A 108.7 . . ?
C26 C25 H25B 108.7 . . ?
C25 C26 H26A 108.8 . . ?
C25 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
C27 C26 C25 113.8(2) . . ?
C27 C26 H26A 108.8 . . ?
C27 C26 H26B 108.8 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C20 C28 H28A 108.5 . . ?
C20 C28 H28B 108.5 . . ?
H28A C28 H28B 107.5 . . ?
C29 C28 C20 115.00(18) . . ?
C29 C28 H28A 108.5 . . ?
C29 C28 H28B 108.5 . . ?
C28 C29 H29A 108.9 . . ?
C28 C29 H29B 108.9 . . ?
H29A C29 H29B 107.7 . . ?
C30 C29 C28 113.23(18) . . ?
C30 C29 H29A 108.9 . . ?
C30 C29 H29B 108.9 . . ?
C29 C30 H30A 108.8 . . ?
C29 C30 H30B 108.8 . . ?
C29 C30 C31 113.67(19) . . ?
H30A C30 H30B 107.7 . . ?
C31 C30 H30A 108.8 . . ?
C31 C30 H30B 108.8 . . ?
C30 C31 H31A 108.6 . . ?
C30 C31 H31B 108.6 . . ?
H31A C31 H31B 107.6 . . ?
C32 C31 C30 114.5(2) . . ?
C32 C31 H31A 108.6 . . ?
C32 C31 H31B 108.6 . . ?
C31 C32 H32A 108.7 . . ?
C31 C32 H32B 108.7 . . ?
H32A C32 H32B 107.6 . . ?
C33 C32 C31 114.4(2) . . ?
C33 C32 H32A 108.7 . . ?
C33 C32 H32B 108.7 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 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 C14 C15 C16 0.6(2) . . . . ?
S1 C17 C18 C19 175.42(18) . . . . ?
S1 C17 C18 C21 -6.4(4) . . . 2_567 ?
O1 C1 C2 C3 -174.3(2) . . . . ?
O1 C1 C2 C13 9.7(4) . . . . ?
O1 C1 C5 C4 175.5(2) . . . . ?
O1 C1 C5 C6 -5.1(4) . . . . ?
C1 C2 C3 C4 -4.9(2) . . . . ?
C1 C2 C3 C10 173.9(2) . . . . ?
C1 C2 C13 C14 -2.0(4) . . . . ?
C1 C5 C6 C7 -178.65(19) . . . . ?
C2 C1 C5 C4 -4.6(2) . . . . ?
C2 C1 C5 C6 174.8(2) . . . . ?
C2 C3 C4 C5 2.2(2) . . . . ?
C2 C3 C4 C9 -175.0(2) . . . . ?
C2 C3 C10 C11 5.9(3) . . . . ?
C2 C3 C10 C12 -172.7(2) . . . . ?
C2 C13 C14 S1 -7.9(4) . . . . ?
C2 C13 C14 C15 172.0(2) . . . . ?
C3 C2 C13 C14 -177.2(2) . . . . ?
C3 C4 C5 C1 1.5(2) . . . . ?
C3 C4 C5 C6 -177.87(19) . . . . ?
C3 C4 C9 C8 177.0(2) . . . . ?
C4 C3 C10 C11 -175.5(2) . . . . ?
C4 C3 C10 C12 5.9(3) . . . . ?
C4 C5 C6 C7 0.6(3) . . . . ?
C5 C1 C2 C3 5.8(2) . . . . ?
C5 C1 C2 C13 -170.2(2) . . . . ?
C5 C4 C9 C8 0.0(3) . . . . ?
C5 C6 C7 C8 -0.7(3) . . . . ?
C6 C7 C8 C9 0.5(3) . . . . ?
C7 C8 C9 C4 -0.1(3) . . . . ?
C9 C4 C5 C1 179.09(18) . . . . ?
C9 C4 C5 C6 -0.3(3) . . . . ?
C10 C3 C4 C5 -176.67(19) . . . . ?
C10 C3 C4 C9 6.2(4) . . . . ?
C13 C2 C3 C4 171.02(19) . . . . ?
C13 C2 C3 C10 -10.2(3) . . . . ?
C13 C14 C15 C16 -179.40(18) . . . . ?
C14 S1 C17 C16 -2.69(17) . . . . ?
C14 S1 C17 C18 177.9(2) . . . . ?
C14 C15 C16 C17 -2.6(3) . . . . ?
C14 C15 C16 C20 171.7(2) . . . . ?
C15 C16 C17 S1 3.5(2) . . . . ?
C15 C16 C17 C18 -176.89(17) . . . . ?
C15 C16 C20 C19 178.6(2) . . . . ?
C15 C16 C20 C22 -63.8(3) . . . . ?
C15 C16 C20 C28 58.1(3) . . . . ?
C16 C17 C18 C19 -4.0(2) . . . . ?
C16 C17 C18 C21 174.1(2) . . . 2_567 ?
C16 C20 C22 C23 -53.7(2) . . . . ?
C16 C20 C28 C29 51.2(2) . . . . ?
C17 S1 C14 C13 -178.9(2) . . . . ?
C17 S1 C14 C15 1.18(16) . . . . ?
C17 C16 C20 C19 -7.1(2) . . . . ?
C17 C16 C20 C22 110.46(19) . . . . ?
C17 C16 C20 C28 -127.67(19) . . . . ?
C17 C18 C19 C20 -0.7(2) . . . . ?
C17 C18 C19 C21 178.12(18) . . . . ?
C18 C19 C20 C16 4.6(2) . . . . ?
C18 C19 C20 C22 -111.47(19) . . . . ?
C18 C19 C20 C28 126.21(18) . . . . ?
C18 C19 C21 C18 0.3(3) . . . 2_567 ?
C19 C20 C22 C23 56.3(2) . . . . ?
C19 C20 C28 C29 -62.1(2) . . . . ?
C20 C16 C17 S1 -172.27(13) . . . . ?
C20 C16 C17 C18 7.3(2) . . . . ?
C20 C19 C21 C18 178.92(19) . . . 2_567 ?
C20 C22 C23 C24 168.63(17) . . . . ?
C20 C28 C29 C30 -179.73(17) . . . . ?
C21 C18 C19 C20 -179.14(18) 2_567 . . . ?
C21 C18 C19 C21 -0.3(3) 2_567 . . . ?
C21 C19 C20 C16 -174.1(2) . . . . ?
C21 C19 C20 C22 69.8(3) . . . . ?
C21 C19 C20 C28 -52.5(3) . . . . ?
C22 C20 C28 C29 173.78(17) . . . . ?
C22 C23 C24 C25 66.7(2) . . . . ?
C23 C24 C25 C26 -177.87(19) . . . . ?
C24 C25 C26 C27 71.3(3) . . . . ?
C28 C20 C22 C23 -178.96(17) . . . . ?
C28 C29 C30 C31 176.69(18) . . . . ?
C29 C30 C31 C32 174.71(18) . . . . ?
C30 C31 C32 C33 61.6(3) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id 'Sample #4: IDIC'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.721
_oxdiff_exptl_absorpt_empirical_full_min 0.731
####################################################################### 
# 
# 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_4TICO
_database_code_depnum_ccdc_archive 'CCDC 1942947'
loop_
_audit_author_name
_audit_author_address
'Peter Horton'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2019-07-24 deposited with the CCDC.	2019-11-18 downloaded from the CCDC.
;

#2018ncs0742r1_2b

_audit_creation_date             2019-05-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C49 H49 N2 O3 S2, C49 H48 N2 O3 S2, 2(C3 H6 O)'
_chemical_formula_sum            'C104 H109 N4 O8 S4'
_chemical_formula_weight         1671.19
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C98 H82 N4 O6 S4'
_chemical_oxdiff_usercomment     
'Sample #10: OPN018 Chloroform/Acetone recollection'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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                   15.2836(2)
_cell_length_b                   20.0101(5)
_cell_length_c                   29.3242(6)
_cell_angle_alpha                90
_cell_angle_beta                 89.997(2)
_cell_angle_gamma                90
_cell_volume                     8968.1(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8815
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.4000
_cell_measurement_theta_min      2.9900
_shelx_estimated_absorpt_T_max   0.972
_shelx_estimated_absorpt_T_min   0.751
_exptl_absorpt_coefficient_mu    1.446
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             3556
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of chloroform and acetone'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_av_unetI/netI     0.0847
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            62183
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        66.596
_diffrn_reflns_theta_max         66.596
_diffrn_reflns_theta_min         2.208
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -63.00 -20.00   0.50    5.00    --    0.00  20.00-180.00   86
  2  ω    -15.00  73.00   0.50    5.00    --    0.00  20.00-180.00  176
  3  ω   -100.00 -61.00   0.50   30.00    --  -90.00  59.00 -22.72   78
  4  ω   -179.00-122.00   0.50   30.00    --  -90.00  56.00  93.75  114
  5  ω   -136.00 -14.00   0.50   30.00    --  -90.00  58.00-177.24  244
  6  ω   -177.00-146.00   0.50   30.00    --  -90.00  59.00 122.03   62
  7  ω   -160.00  -4.00   0.50   30.00    --  -90.00  59.00-138.62  312
  8  ω    -50.00 -25.00   0.50   30.00    --  -90.00  59.00 163.27   50
  9  ω    -85.00  -1.00   0.50   30.00    --  -90.00  59.00 122.03  168
 10  ω    -38.00  -2.00   0.50   30.00    --  -90.00  56.00  93.75   72
 11  ω   -178.00 -22.00   0.50   30.00    --  -90.00  59.00-169.54  312
 12  ω   -178.00-145.00   0.50   30.00    --  -90.00  59.00 154.04   66
 13  ω   -162.00-134.00   0.50   30.00    --  -90.00  59.00 163.27   56
 14  ω   -123.00 -85.00   0.50   30.00    --  -90.00  59.00 163.27   76
 15  ω   -136.00-111.00   0.50   30.00    --  -90.00  59.00 -22.72   50
 16  ω   -135.00 -74.00   0.50   30.00    --  -90.00  58.00-119.97  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter χ goniometer'
_diffrn_measurement_device_type  
'Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0048336000
_diffrn_orient_matrix_UB_12      0.0615427000
_diffrn_orient_matrix_UB_13      0.0313809000
_diffrn_orient_matrix_UB_21      0.0151373000
_diffrn_orient_matrix_UB_22      -0.0460157000
_diffrn_orient_matrix_UB_23      0.0414341000
_diffrn_orient_matrix_UB_31      0.0995411000
_diffrn_orient_matrix_UB_32      0.0039173000
_diffrn_orient_matrix_UB_33      -0.0078460000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9046
_reflns_number_total             15523
_reflns_odcompleteness_completeness 97.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1174
_refine_ls_number_reflns         15523
_refine_ls_number_restraints     2209
_refine_ls_R_factor_all          0.1639
_refine_ls_R_factor_gt           0.0998
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1195P)²+19.4910P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2395
_refine_ls_wR_factor_ref         0.2842
_refine_special_details          
'The crystal used was a merohedral twin. The crystal was not of great quality, resulting in a poor structure. However, the overall connectivity especially of the core can be idenitfied. There is significant disorder observed especially in the longer alkyl chains (and solvent acetone) for which it was only possible to model one alkyl chain over two positions. Due to all the above, various geometrical (SADI, DFIX, BUMP) and displacement (SIMU, RIGU) restraints have been used'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.452(4)
 0.548(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C36-C35
 -1.4 with sigma of 0.02
 C99-C98 = C98-C97 = C97-C96 = C96-C95 = C95-C94 = C94-C93 = C93-C92
 1.5 with sigma of 0.03
 O201-C201 \\sim O211-C211
 with sigma of 0.02
 O211-C211 \\sim O216-C216
 with sigma of 0.02
 O52-C84 \\sim O3-C42 \\sim O2-C34 \\sim O53-C92
 with sigma of 0.02
 O52-C85 \\sim O3-C43 \\sim O2-C35 \\sim O53-C93
 with sigma of 0.02
 C25-C34 \\sim C31-C42 \\sim C75-C84 \\sim C81-C92
 with sigma of 0.02
 C93-C94 \\sim C93-C94A
 with sigma of 0.02
 C94-C95 \\sim C94A-C95A
 with sigma of 0.02
 C95-C96 \\sim C95A-C96A
 with sigma of 0.02
 C93-C95 \\sim C93-C95A
 with sigma of 0.04
 C94-C96 \\sim C94A-C96A
 with sigma of 0.04
 C96-C98 \\sim C96A-C98A
 with sigma of 0.04
 C94A-C92 \\sim C92-C94
 with sigma of 0.04
 C202-O201 \\sim C203-O201 \\sim C213-O211 \\sim O211-C212
 with sigma of 0.04
 C213-C211 \\sim C211-C212 \\sim C202-C201 \\sim C203-C201
 with sigma of 0.02
 C202-C203 \\sim C213-C212
 with sigma of 0.04
 C211-C212 \\sim C216-C217
 with sigma of 0.02
 C211-C213 \\sim C216-C218
 with sigma of 0.02
 O211-C212 \\sim O216-C217
 with sigma of 0.04
 O211-C213 \\sim O216-C218
 with sigma of 0.04
 C212-C213 \\sim C217-C218
 with sigma of 0.04
 C34-C35 \\sim C35-C36 \\sim C36-C37 \\sim C37-C38 \\sim C38-C39 \\sim C39-C40
\\sim C40-C41
 with sigma of 0.02
 C38-C40 \\sim C35-C37 \\sim C37-C39 \\sim C39-C41 \\sim C34-C36 \\sim C36-C38
 with sigma of 0.04
 C91-C90 \\sim C90-C89 \\sim C89-C88 \\sim C88-C87 \\sim C87-C86 \\sim C86-C85
\\sim C85-C84
 with sigma of 0.02
 C91-C89 \\sim C89-C87 \\sim C87-C85 \\sim C90-C88 \\sim C88-C86 \\sim C86-C84
 with sigma of 0.04
 C43-C44 \\sim C44-C45 \\sim C45-C46 \\sim C46-C47 \\sim C47-C48 \\sim C48-C49
\\sim C43-C42
 with sigma of 0.02
 C44-C46 \\sim C46-C48 \\sim C43-C45 \\sim C45-C47 \\sim C47-C49 \\sim C42-C44
 with sigma of 0.04
 C96-C97 \\sim C96A-C97A
 with sigma of 0.02
 C97-C98 \\sim C97A-C98A
 with sigma of 0.02
 C95-C97 \\sim C95A-C97A
 with sigma of 0.04
 C99-C98 \\sim C98-C97 \\sim C97-C96 \\sim C96-C95 \\sim C95-C94 \\sim C94-C93
\\sim C93-C92
 with sigma of 0.02
 C99-C97 \\sim C97-C95 \\sim C95-C93 \\sim C98-C96 \\sim C96-C94 \\sim C94-C92
 with sigma of 0.04
 C98-C99 \\sim C98A-C99A
 with sigma of 0.02
 C97-C99 \\sim C97A-C99A
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O216)=Sof(C216)=Sof(C217)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C218)=
 Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(O211)=Sof(C211)=Sof(C212)=Sof(H21G)=Sof(H21H)=Sof(H21I)=Sof(C213)=
 Sof(H21J)=Sof(H21K)=Sof(H21L)=FVAR(1)
 Sof(H93C)=Sof(H93D)=Sof(C94A)=Sof(H94C)=Sof(H94D)=Sof(C95A)=Sof(H95C)=
 Sof(H95D)=Sof(C96A)=Sof(H96C)=Sof(H96D)=Sof(C97A)=Sof(H97C)=Sof(H97D)=
 Sof(C98A)=Sof(H98C)=Sof(H98D)=Sof(C99A)=Sof(H99D)=Sof(H99E)=Sof(H99F)=1-FVAR(2)
 Sof(H93A)=Sof(H93B)=Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(C95)=Sof(H95A)=Sof(H95B)=
 Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(C98)=Sof(H98A)=
 Sof(H98B)=Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(H99C)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C65(H65A,H65B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,
 H87B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B), C92(H92A,H92B),
 C93(H93A,H93B), C93(H93C,H93D), C94(H94A,H94B), C95(H95A,H95B), C96(H96A,H96B),
  C97(H97A,H97B), C98(H98A,H98B), C94A(H94C,H94D), C95A(H95C,H95D), C96A(H96C,
 H96D), C97A(H97C,H97D), C98A(H98C,H98D), C34(H34A,H34B), C35(H35A,H35B),
 C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
  C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,
 H46B), C47(H47A,H47B), C48(H48A,H48B)
7.b Me refined with riding coordinates:
 C91(H91A,H91B,H91C), C99(H99A,H99B,H99C), C99A(H99D,H99E,H99F), C41(H41A,H41B,
 H41C), C49(H49A,H49B,H49C), C217(H21A,H21B,H21C), C218(H21D,H21E,H21F),
 C202(H20A,H20B,H20C), C203(H20D,H20E,H20F), C212(H21G,H21H,H21I), C213(H21J,
 H21K,H21L)
7.c Aromatic/amide H refined with riding coordinates:
 C56(H56), C57(H57), C58(H58), C59(H59), C63(H63), C73(H73), C74(H74),
 C76(H76), C77(H77), C79(H79), C80(H80), C82(H82), C83(H83), C6(H6), C7(H7),
 C8(H8), C9(H9), C13(H13), C15(H15), C23(H23), C24(H24), C26(H26), C27(H27),
 C29(H29), C30(H30), C32(H32), C33(H33)
;
_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
S51 S 0.21006(17) -0.10303(15) 0.56050(9) 0.0444(7) Uani 1 1 d . U . . .
S52 S 0.36886(17) -0.00380(13) 0.47778(10) 0.0430(7) Uani 1 1 d . U . . .
O51 O 0.0398(5) -0.1300(5) 0.5662(3) 0.063(3) Uani 1 1 d . U . . .
O52 O 0.5728(7) 0.0739(7) 0.7429(5) 0.140(4) Uani 1 1 d D U . . .
O53 O 0.6265(10) -0.3481(6) 0.5697(5) 0.145(5) Uani 1 1 d D U . . .
N51 N 0.1924(9) -0.2447(13) 0.7466(6) 0.178(10) Uani 1 1 d . U . . .
N52 N -0.0707(8) -0.2816(8) 0.7745(4) 0.090(4) Uani 1 1 d . U . . .
C51 C 0.0182(8) -0.1559(6) 0.6035(4) 0.050(3) Uani 1 1 d . U . . .
C52 C 0.0739(7) -0.1762(7) 0.6411(4) 0.049(3) Uani 1 1 d . U . . .
C53 C 0.0156(7) -0.2041(8) 0.6768(4) 0.066(4) Uani 1 1 d . U . . .
C54 C -0.0750(7) -0.1948(7) 0.6598(4) 0.053(3) Uani 1 1 d . U . . .
C55 C -0.0762(7) -0.1665(7) 0.6181(4) 0.052(3) Uani 1 1 d . U . . .
C56 C -0.1496(8) -0.1555(7) 0.5902(5) 0.068(4) Uani 1 1 d . U . . .
H56 H -0.146153 -0.137733 0.560238 0.081 Uiso 1 1 calc R . . . .
C57 C -0.2307(8) -0.1740(7) 0.6119(5) 0.071(4) Uani 1 1 d . U . . .
H57 H -0.284647 -0.168830 0.596184 0.085 Uiso 1 1 calc R . . . .
C58 C -0.2290(8) -0.1986(8) 0.6544(6) 0.085(4) Uani 1 1 d . U . . .
H58 H -0.283569 -0.208552 0.668388 0.102 Uiso 1 1 calc R . . . .
C59 C -0.1580(8) -0.2099(9) 0.6783(5) 0.083(4) Uani 1 1 d . U . . .
H59 H -0.162410 -0.228296 0.708025 0.099 Uiso 1 1 calc R . . . .
C60 C 0.0386(8) -0.2314(8) 0.7159(5) 0.076(4) Uani 1 1 d . U . . .
C61 C 0.1247(10) -0.2419(11) 0.7329(5) 0.102(6) Uani 1 1 d . U . . .
C62 C -0.0258(7) -0.2569(8) 0.7500(4) 0.079(5) Uani 1 1 d . U . . .
C63 C 0.1597(7) -0.1721(6) 0.6420(4) 0.049(3) Uani 1 1 d . U . . .
H63 H 0.184071 -0.192959 0.668223 0.059 Uiso 1 1 calc R . . . .
C64 C 0.2270(7) -0.1429(5) 0.6120(4) 0.045(3) Uani 1 1 d . U . . .
C65 C 0.3155(7) -0.1425(6) 0.6260(4) 0.046(3) Uani 1 1 d . U . . .
H65A H 0.336834 -0.188987 0.628993 0.055 Uiso 1 1 calc R . . . .
H65B H 0.320593 -0.120534 0.656127 0.055 Uiso 1 1 calc R . . . .
C66 C 0.3675(7) -0.1076(6) 0.5935(4) 0.044(2) Uani 1 1 d . U . . .
C67 C 0.3179(7) -0.0851(5) 0.5593(4) 0.042(2) Uani 1 1 d . U . . .
C68 C 0.3762(7) -0.0494(4) 0.5273(4) 0.041(2) Uani 1 1 d . U . . .
C69 C 0.4600(7) -0.0526(5) 0.5459(3) 0.039(2) Uani 1 1 d . U . . .
C70 C 0.4649(7) -0.0928(5) 0.5911(4) 0.043(2) Uani 1 1 d . U . . .
C71 C 0.5194(7) -0.0149(5) 0.5173(4) 0.035(2) Uani 1 1 d . U . . .
C72 C 0.4998(8) -0.0503(6) 0.6300(4) 0.050(2) Uani 1 1 d . U . . .
C73 C 0.5865(9) -0.0463(7) 0.6396(6) 0.083(4) Uani 1 1 d . U . . .
H73 H 0.628559 -0.068728 0.621304 0.100 Uiso 1 1 calc R . . . .
C74 C 0.6128(12) -0.0071(9) 0.6784(7) 0.110(5) Uani 1 1 d . U . . .
H74 H 0.672223 -0.007248 0.687791 0.132 Uiso 1 1 calc R . . . .
C75 C 0.5568(14) 0.0278(10) 0.7003(6) 0.110(5) Uani 1 1 d D U . . .
C76 C 0.4783(14) 0.0302(9) 0.6894(5) 0.096(4) Uani 1 1 d . U . . .
H76 H 0.440288 0.060714 0.704323 0.115 Uiso 1 1 calc R . . . .
C77 C 0.4462(11) -0.0108(7) 0.6562(5) 0.071(4) Uani 1 1 d . U . . .
H77 H 0.384898 -0.011980 0.650967 0.086 Uiso 1 1 calc R . . . .
C78 C 0.5153(7) -0.1568(6) 0.5851(4) 0.043(2) Uani 1 1 d . U . . .
C79 C 0.5447(8) -0.1813(7) 0.5405(4) 0.057(3) Uani 1 1 d . U . . .
H79 H 0.538496 -0.154365 0.514030 0.068 Uiso 1 1 calc R . . . .
C80 C 0.5817(10) -0.2447(8) 0.5377(5) 0.077(4) Uani 1 1 d . U . . .
H80 H 0.599477 -0.261235 0.508767 0.093 Uiso 1 1 calc R . . . .
C81 C 0.5928(11) -0.2823(7) 0.5740(6) 0.085(4) Uani 1 1 d D U . . .
C82 C 0.5636(9) -0.2611(7) 0.6161(5) 0.069(3) Uani 1 1 d . U . . .
H82 H 0.570006 -0.289498 0.641860 0.082 Uiso 1 1 calc R . . . .
C83 C 0.5249(8) -0.1987(6) 0.6215(4) 0.051(3) Uani 1 1 d . U . . .
H83 H 0.505001 -0.185079 0.650698 0.062 Uiso 1 1 calc R . . . .
C84 C 0.6393(14) 0.0668(10) 0.7580(7) 0.189(8) Uani 1 1 d D U . . .
H84A H 0.682224 0.077803 0.733927 0.227 Uiso 1 1 calc R . . . .
H84B H 0.645690 0.018408 0.764385 0.227 Uiso 1 1 calc R . . . .
C85 C 0.6679(11) 0.1032(9) 0.8005(6) 0.147(6) Uani 1 1 d D U . . .
H85A H 0.713937 0.073526 0.812883 0.176 Uiso 1 1 calc R . . . .
H85B H 0.699830 0.142186 0.788000 0.176 Uiso 1 1 calc R . . . .
C86 C 0.6283(11) 0.1301(10) 0.8412(5) 0.150(6) Uani 1 1 d D U . . .
H86A H 0.586969 0.096364 0.853172 0.180 Uiso 1 1 calc R . . . .
H86B H 0.593400 0.169711 0.832273 0.180 Uiso 1 1 calc R . . . .
C87 C 0.6880(11) 0.1505(7) 0.8795(5) 0.133(5) Uani 1 1 d D U . . .
H87A H 0.728321 0.184571 0.866888 0.159 Uiso 1 1 calc R . . . .
H87B H 0.724151 0.110940 0.886899 0.159 Uiso 1 1 calc R . . . .
C88 C 0.6546(9) 0.1777(9) 0.9241(5) 0.138(5) Uani 1 1 d D U . . .
H88A H 0.615155 0.215724 0.917579 0.166 Uiso 1 1 calc R . . . .
H88B H 0.619310 0.142546 0.939153 0.166 Uiso 1 1 calc R . . . .
C89 C 0.7233(10) 0.2006(9) 0.9567(5) 0.128(5) Uani 1 1 d D U . . .
H89A H 0.763754 0.231504 0.940893 0.153 Uiso 1 1 calc R . . . .
H89B H 0.757620 0.161599 0.967278 0.153 Uiso 1 1 calc R . . . .
C90 C 0.6833(10) 0.2362(8) 0.9981(5) 0.131(5) Uani 1 1 d D U . . .
H90A H 0.730880 0.253167 1.017905 0.157 Uiso 1 1 calc R . . . .
H90B H 0.648544 0.274961 0.987576 0.157 Uiso 1 1 calc R . . . .
C91 C 0.6254(17) 0.1899(14) 1.0254(10) 0.217(12) Uani 1 1 d D U . . .
H91A H 0.600945 0.214059 1.051469 0.325 Uiso 1 1 calc R . . . .
H91B H 0.577659 0.173618 1.005978 0.325 Uiso 1 1 calc R . . . .
H91C H 0.659934 0.151840 1.036285 0.325 Uiso 1 1 calc R . . . .
C92 C 0.6226(15) -0.3803(8) 0.5377(7) 0.203(8) Uani 1 1 d D U . . .
H92A H 0.668478 -0.363749 0.516691 0.243 Uiso 1 1 calc R . . . .
H92B H 0.565723 -0.370181 0.523118 0.243 Uiso 1 1 calc R . . . .
C93 C 0.6310(16) -0.4561(8) 0.5386(9) 0.248(11) Uani 1 1 d D U . . .
H93A H 0.687474 -0.467395 0.524006 0.298 Uiso 0.467(19) 1 calc R . P A 1
H93B H 0.584403 -0.474160 0.518647 0.298 Uiso 0.467(19) 1 calc R . P A 1
H93C H 0.680729 -0.467804 0.558728 0.298 Uiso 0.533(19) 1 calc R . P A 2
H93D H 0.646109 -0.471387 0.507494 0.298 Uiso 0.533(19) 1 calc R . P A 2
C94 C 0.627(2) -0.4952(18) 0.5834(12) 0.290(15) Uani 0.467(19) 1 d D U P A 1
H94A H 0.664055 -0.471878 0.605978 0.348 Uiso 0.467(19) 1 calc R . P A 1
H94B H 0.653023 -0.539771 0.578122 0.348 Uiso 0.467(19) 1 calc R . P A 1
C95 C 0.536(3) -0.505(3) 0.6048(19) 0.316(16) Uani 0.467(19) 1 d D U P A 1
H95A H 0.543517 -0.500464 0.638166 0.380 Uiso 0.467(19) 1 calc R . P A 1
H95B H 0.499284 -0.467653 0.594586 0.380 Uiso 0.467(19) 1 calc R . P A 1
C96 C 0.483(4) -0.569(4) 0.5972(17) 0.284(15) Uani 0.467(19) 1 d D U P A 1
H96A H 0.511928 -0.595531 0.573015 0.341 Uiso 0.467(19) 1 calc R . P A 1
H96B H 0.424554 -0.556009 0.585503 0.341 Uiso 0.467(19) 1 calc R . P A 1
C97 C 0.469(6) -0.615(3) 0.6386(17) 0.278(16) Uani 0.467(19) 1 d D U P A 1
H97A H 0.505124 -0.655395 0.634272 0.333 Uiso 0.467(19) 1 calc R . P A 1
H97B H 0.407230 -0.628719 0.639251 0.333 Uiso 0.467(19) 1 calc R . P A 1
C98 C 0.492(4) -0.585(4) 0.6853(17) 0.28(2) Uani 0.467(19) 1 d D U P A 1
H98A H 0.549605 -0.602578 0.694845 0.339 Uiso 0.467(19) 1 calc R . P A 1
H98B H 0.498668 -0.535765 0.681596 0.339 Uiso 0.467(19) 1 calc R . P A 1
C99 C 0.427(2) -0.5974(13) 0.7238(17) 0.27(3) Uani 0.467(19) 1 d D U P A 1
H99A H 0.447691 -0.576094 0.751799 0.405 Uiso 0.467(19) 1 calc R . P A 1
H99B H 0.369708 -0.578561 0.715421 0.405 Uiso 0.467(19) 1 calc R . P A 1
H99C H 0.420811 -0.645592 0.728713 0.405 Uiso 0.467(19) 1 calc R . P A 1
C94A C 0.5495(19) -0.4963(17) 0.555(3) 0.297(14) Uani 0.533(19) 1 d D U P A 2
H94C H 0.547456 -0.537746 0.536455 0.356 Uiso 0.533(19) 1 calc R . P A 2
H94D H 0.561061 -0.510135 0.586746 0.356 Uiso 0.533(19) 1 calc R . P A 2
C95A C 0.4573(18) -0.4661(13) 0.5540(11) 0.339(18) Uani 0.533(19) 1 d D U P A 2
H95C H 0.456855 -0.431795 0.529654 0.406 Uiso 0.533(19) 1 calc R . P A 2
H95D H 0.448926 -0.442330 0.583215 0.406 Uiso 0.533(19) 1 calc R . P A 2
C96A C 0.376(2) -0.5105(19) 0.5466(14) 0.333(18) Uani 0.533(19) 1 d D U P A 2
H96C H 0.323696 -0.484047 0.554875 0.400 Uiso 0.533(19) 1 calc R . P A 2
H96D H 0.371780 -0.520785 0.513664 0.400 Uiso 0.533(19) 1 calc R . P A 2
C97A C 0.372(4) -0.577(3) 0.5728(11) 0.302(16) Uani 0.533(19) 1 d D U P A 2
H97C H 0.361924 -0.612815 0.550434 0.363 Uiso 0.533(19) 1 calc R . P A 2
H97D H 0.320451 -0.575061 0.593106 0.363 Uiso 0.533(19) 1 calc R . P A 2
C98A C 0.452(4) -0.596(3) 0.6020(15) 0.277(15) Uani 0.533(19) 1 d D U P A 2
H98C H 0.459829 -0.645211 0.599213 0.333 Uiso 0.533(19) 1 calc R . P A 2
H98D H 0.504185 -0.574962 0.588340 0.333 Uiso 0.533(19) 1 calc R . P A 2
C99A C 0.451(4) -0.579(4) 0.6530(17) 0.260(19) Uani 0.533(19) 1 d D U P A 2
H99D H 0.505109 -0.594194 0.667196 0.389 Uiso 0.533(19) 1 calc R . P A 2
H99E H 0.445340 -0.530365 0.656669 0.389 Uiso 0.533(19) 1 calc R . P A 2
H99F H 0.400776 -0.600944 0.667593 0.389 Uiso 0.533(19) 1 calc R . P A 2
S1 S 0.28999(17) 0.10288(15) 0.56124(10) 0.0473(8) Uani 1 1 d . U . . .
S2 S 0.13096(17) 0.00338(14) 0.47818(9) 0.0418(7) Uani 1 1 d . U . . .
O1 O 0.4593(5) 0.1300(5) 0.5668(2) 0.053(2) Uani 1 1 d . U . . .
O2 O -0.1119(11) -0.0606(6) 0.7323(4) 0.190(6) Uani 1 1 d D U . . .
O3 O -0.1265(11) 0.3439(5) 0.5676(5) 0.136(5) Uani 1 1 d D U . . .
N1 N 0.3071(8) 0.2470(11) 0.7476(5) 0.149(8) Uani 1 1 d . U . . .
N2 N 0.5720(8) 0.2817(9) 0.7747(5) 0.106(5) Uani 1 1 d . U . . .
C1 C 0.4837(7) 0.1528(6) 0.6017(4) 0.044(3) Uani 1 1 d . U . . .
C2 C 0.4289(7) 0.1776(7) 0.6405(4) 0.050(3) Uani 1 1 d . U . . .
C3 C 0.4841(7) 0.2032(6) 0.6751(4) 0.044(2) Uani 1 1 d . U . . .
C4 C 0.5772(7) 0.1972(7) 0.6593(4) 0.056(3) Uani 1 1 d . U . . .
C5 C 0.5730(7) 0.1677(6) 0.6148(4) 0.042(2) Uani 1 1 d . U . . .
C6 C 0.6511(7) 0.1560(5) 0.5927(3) 0.046(3) Uani 1 1 d . U . . .
H6 H 0.649799 0.136303 0.563261 0.055 Uiso 1 1 calc R . . . .
C7 C 0.7274(8) 0.1709(7) 0.6107(4) 0.062(4) Uani 1 1 d . U . . .
H7 H 0.778964 0.163082 0.593439 0.074 Uiso 1 1 calc R . . . .
C8 C 0.7352(8) 0.1984(8) 0.6555(4) 0.071(4) Uani 1 1 d . U . . .
H8 H 0.790628 0.207868 0.668623 0.085 Uiso 1 1 calc R . . . .
C9 C 0.6556(7) 0.2110(7) 0.6795(4) 0.066(4) Uani 1 1 d . U . . .
H9 H 0.657190 0.229022 0.709420 0.079 Uiso 1 1 calc R . . . .
C10 C 0.4651(8) 0.2315(7) 0.7181(5) 0.066(4) Uani 1 1 d . U . . .
C11 C 0.3771(9) 0.2370(11) 0.7333(5) 0.101(6) Uani 1 1 d . U . . .
C12 C 0.5239(9) 0.2603(9) 0.7478(5) 0.084(5) Uani 1 1 d . U . . .
C13 C 0.3344(7) 0.1705(6) 0.6422(4) 0.052(3) Uani 1 1 d . U . . .
H13 H 0.309325 0.189393 0.668880 0.062 Uiso 1 1 calc R . . . .
C14 C 0.2749(7) 0.1433(7) 0.6143(4) 0.049(3) Uani 1 1 d . U . . .
C15 C 0.1858(7) 0.1423(6) 0.6259(4) 0.049(3) Uani 1 1 d . U . . .
H15 H 0.163349 0.162833 0.652697 0.058 Uiso 1 1 calc R . . . .
C16 C 0.1355(7) 0.1100(5) 0.5959(4) 0.042(2) Uani 1 1 d . U . . .
C17 C 0.1795(6) 0.0834(6) 0.5569(3) 0.040(2) Uani 1 1 d . U . . .
C18 C 0.1220(7) 0.0481(6) 0.5280(3) 0.044(2) Uani 1 1 d . U . . .
C19 C 0.0378(7) 0.0499(6) 0.5465(4) 0.043(2) Uani 1 1 d . U . . .
C20 C 0.0344(7) 0.0911(6) 0.5886(4) 0.044(2) Uani 1 1 d . U . . .
C21 C -0.0197(6) 0.0135(6) 0.5210(4) 0.039(2) Uani 1 1 d . U . . .
C22 C 0.0012(8) 0.0498(7) 0.6279(4) 0.053(3) Uani 1 1 d . U . . .
C23 C 0.0550(11) 0.0103(7) 0.6567(5) 0.074(4) Uani 1 1 d . U . . .
H23 H 0.116137 0.008439 0.651109 0.088 Uiso 1 1 calc R . . . .
C24 C 0.0201(14) -0.0259(10) 0.6930(6) 0.110(5) Uani 1 1 d . U . . .
H24 H 0.058256 -0.049376 0.712962 0.132 Uiso 1 1 calc R . . . .
C25 C -0.0706(14) -0.0282(10) 0.7006(6) 0.120(5) Uani 1 1 d D U . . .
C26 C -0.1262(14) 0.0089(9) 0.6689(7) 0.119(5) Uani 1 1 d . U . . .
H26 H -0.188083 0.004870 0.670622 0.143 Uiso 1 1 calc R . . . .
C27 C -0.0898(10) 0.0487(8) 0.6374(6) 0.098(5) Uani 1 1 d . U . . .
H27 H -0.126886 0.077756 0.620570 0.117 Uiso 1 1 calc R . . . .
C28 C -0.0140(7) 0.1593(6) 0.5826(5) 0.052(3) Uani 1 1 d . U . . .
C29 C -0.0444(8) 0.1790(7) 0.5429(5) 0.062(3) Uani 1 1 d . U . . .
H29 H -0.038922 0.149898 0.517513 0.074 Uiso 1 1 calc R . . . .
C30 C -0.0838(10) 0.2398(7) 0.5367(6) 0.080(4) Uani 1 1 d . U . . .
H30 H -0.108176 0.251044 0.507902 0.096 Uiso 1 1 calc R . . . .
C31 C -0.0882(10) 0.2865(6) 0.5738(6) 0.079(4) Uani 1 1 d D U . . .
C32 C -0.0598(9) 0.2645(7) 0.6169(6) 0.068(3) Uani 1 1 d . U . . .
H32 H -0.065406 0.292573 0.642855 0.082 Uiso 1 1 calc R . . . .
C33 C -0.0240(9) 0.2022(6) 0.6208(6) 0.062(3) Uani 1 1 d . U . . .
H33 H -0.005196 0.187203 0.649910 0.075 Uiso 1 1 calc R . . . .
C34 C -0.1680(15) -0.0739(11) 0.7524(7) 0.221(9) Uani 1 1 d D U . . .
H34A H -0.210759 -0.089159 0.729283 0.265 Uiso 1 1 calc R . . . .
H34B H -0.190304 -0.030124 0.763050 0.265 Uiso 1 1 calc R . . . .
C35 C -0.1844(16) -0.1175(11) 0.7906(5) 0.223(10) Uani 1 1 d D U . . .
H35A H -0.248270 -0.125743 0.790889 0.268 Uiso 1 1 calc R . . . .
H35B H -0.156406 -0.160691 0.783040 0.268 Uiso 1 1 calc R . . . .
C36 C -0.161(2) -0.1031(12) 0.8356(6) 0.249(11) Uani 1 1 d D U . . .
H36A H -0.186276 -0.059392 0.844257 0.298 Uiso 1 1 calc R . . . .
H36B H -0.096421 -0.099049 0.837393 0.298 Uiso 1 1 calc R . . . .
C37 C -0.191(2) -0.1548(12) 0.8692(6) 0.215(10) Uani 1 1 d D U . . .
H37A H -0.255158 -0.154131 0.871654 0.258 Uiso 1 1 calc R . . . .
H37B H -0.172414 -0.199795 0.858771 0.258 Uiso 1 1 calc R . . . .
C38 C -0.1516(19) -0.1402(12) 0.9131(6) 0.216(10) Uani 1 1 d D U . . .
H38A H -0.175094 -0.097038 0.924153 0.259 Uiso 1 1 calc R . . . .
H38B H -0.087712 -0.134610 0.908904 0.259 Uiso 1 1 calc R . . . .
C39 C -0.1662(18) -0.1911(10) 0.9488(6) 0.201(9) Uani 1 1 d D U . . .
H39A H -0.229539 -0.198863 0.953353 0.241 Uiso 1 1 calc R . . . .
H39B H -0.138213 -0.233930 0.940207 0.241 Uiso 1 1 calc R . . . .
C40 C -0.1262(16) -0.1640(11) 0.9907(5) 0.195(9) Uani 1 1 d D U . . .
H40A H -0.064112 -0.153329 0.984306 0.235 Uiso 1 1 calc R . . . .
H40B H -0.156103 -0.121768 0.998680 0.235 Uiso 1 1 calc R . . . .
C41 C -0.1300(15) -0.2078(10) 1.0288(6) 0.168(9) Uani 1 1 d D U . . .
H41A H -0.102207 -0.186398 1.055181 0.252 Uiso 1 1 calc R . . . .
H41B H -0.191203 -0.217806 1.036014 0.252 Uiso 1 1 calc R . . . .
H41C H -0.099070 -0.249415 1.021617 0.252 Uiso 1 1 calc R . . . .
C42 C -0.1327(14) 0.3917(7) 0.5909(7) 0.183(8) Uani 1 1 d D U . . .
H42A H -0.074416 0.403429 0.603211 0.219 Uiso 1 1 calc R . . . .
H42B H -0.171694 0.381620 0.616959 0.219 Uiso 1 1 calc R . . . .
C43 C -0.1714(15) 0.4548(7) 0.5631(10) 0.242(11) Uani 1 1 d D U . . .
H43A H -0.211438 0.481611 0.582358 0.291 Uiso 1 1 calc R . . . .
H43B H -0.202958 0.440193 0.535359 0.291 Uiso 1 1 calc R . . . .
C44 C -0.084(2) 0.4965(14) 0.5503(12) 0.333(14) Uani 1 1 d D U . . .
H44A H -0.034523 0.465160 0.547394 0.400 Uiso 1 1 calc R . . . .
H44B H -0.092891 0.518426 0.520352 0.400 Uiso 1 1 calc R . . . .
C45 C -0.061(2) 0.5523(13) 0.5877(13) 0.358(16) Uani 1 1 d D U . . .
H45A H -0.069317 0.534108 0.618848 0.430 Uiso 1 1 calc R . . . .
H45B H -0.099445 0.591703 0.584019 0.430 Uiso 1 1 calc R . . . .
C46 C 0.040(2) 0.573(2) 0.5800(12) 0.381(17) Uani 1 1 d D U . . .
H46A H 0.066436 0.546161 0.555340 0.458 Uiso 1 1 calc R . . . .
H46B H 0.044848 0.620975 0.572363 0.458 Uiso 1 1 calc R . . . .
C47 C 0.084(3) 0.5571(18) 0.6279(13) 0.358(17) Uani 1 1 d D U . . .
H47A H 0.148840 0.556055 0.625208 0.429 Uiso 1 1 calc R . . . .
H47B H 0.063675 0.513867 0.640297 0.429 Uiso 1 1 calc R . . . .
C48 C 0.053(4) 0.6186(15) 0.6592(15) 0.342(18) Uani 1 1 d D U . . .
H48A H 0.097049 0.654443 0.660516 0.411 Uiso 1 1 calc R . . . .
H48B H -0.003654 0.637377 0.648381 0.411 Uiso 1 1 calc R . . . .
C49 C 0.042(3) 0.5818(19) 0.7075(15) 0.34(2) Uani 1 1 d D U . . .
H49A H 0.022199 0.614141 0.730457 0.514 Uiso 1 1 calc R . . . .
H49B H -0.001587 0.545905 0.704835 0.514 Uiso 1 1 calc R . . . .
H49C H 0.098127 0.562803 0.716851 0.514 Uiso 1 1 calc R . . . .
O216 O 0.216(3) -0.090(2) 0.8235(16) 0.223(15) Uani 0.43(2) 1 d D U P B 2
C216 C 0.295(3) -0.075(3) 0.8071(16) 0.203(14) Uani 0.43(2) 1 d D U P B 2
C217 C 0.307(3) -0.0705(18) 0.7568(16) 0.175(16) Uani 0.43(2) 1 d D U P B 2
H21A H 0.368255 -0.059080 0.750162 0.263 Uiso 0.43(2) 1 calc R . P B 2
H21B H 0.292996 -0.113624 0.742786 0.263 Uiso 0.43(2) 1 calc R . P B 2
H21C H 0.268685 -0.035866 0.744315 0.263 Uiso 0.43(2) 1 calc R . P B 2
C218 C 0.374(3) -0.096(3) 0.833(2) 0.27(2) Uani 0.43(2) 1 d D U P B 2
H21D H 0.426729 -0.081846 0.817291 0.399 Uiso 0.43(2) 1 calc R . P B 2
H21E H 0.372602 -0.076141 0.863846 0.399 Uiso 0.43(2) 1 calc R . P B 2
H21F H 0.374201 -0.145173 0.836303 0.399 Uiso 0.43(2) 1 calc R . P B 2
O201 O 0.3565(19) 0.087(2) 0.7870(8) 0.337(17) Uani 1 1 d D U . . .
C201 C 0.270(2) 0.091(3) 0.7865(7) 0.331(18) Uani 1 1 d D U . . .
C202 C 0.217(2) 0.0946(14) 0.7438(7) 0.34(2) Uani 1 1 d D U . . .
H20A H 0.154873 0.097123 0.751624 0.516 Uiso 1 1 calc R . . . .
H20B H 0.233933 0.134529 0.726544 0.516 Uiso 1 1 calc R . . . .
H20C H 0.227842 0.054710 0.725272 0.516 Uiso 1 1 calc R . . . .
C203 C 0.222(2) 0.095(3) 0.8313(8) 0.39(2) Uani 1 1 d D U . . .
H20D H 0.158878 0.097845 0.825544 0.582 Uiso 1 1 calc R . . . .
H20E H 0.234798 0.055599 0.849658 0.582 Uiso 1 1 calc R . . . .
H20F H 0.240958 0.135386 0.847722 0.582 Uiso 1 1 calc R . . . .
O211 O 0.1387(14) -0.0891(17) 0.7860(11) 0.197(13) Uani 0.57(2) 1 d D U P B 1
C211 C 0.2223(19) -0.1004(19) 0.7853(10) 0.160(11) Uani 0.57(2) 1 d D U P B 1
C212 C 0.272(2) -0.0853(13) 0.7424(10) 0.143(12) Uani 0.57(2) 1 d D U P B 1
H21G H 0.333785 -0.096202 0.746794 0.214 Uiso 0.57(2) 1 calc R . P B 1
H21H H 0.248162 -0.112184 0.717336 0.214 Uiso 0.57(2) 1 calc R . P B 1
H21I H 0.265933 -0.037769 0.735056 0.214 Uiso 0.57(2) 1 calc R . P B 1
C213 C 0.279(2) -0.1204(17) 0.8247(10) 0.202(14) Uani 0.57(2) 1 d D U P B 1
H21J H 0.339638 -0.125497 0.814258 0.303 Uiso 0.57(2) 1 calc R . P B 1
H21K H 0.276440 -0.085896 0.848364 0.303 Uiso 0.57(2) 1 calc R . P B 1
H21L H 0.258273 -0.162946 0.837216 0.303 Uiso 0.57(2) 1 calc R . P B 1


_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
S51 C64 1.729(11) . ?
S51 C67 1.687(11) . ?
S52 C68 1.718(11) . ?
S52 C71 1.754(11) 3_656 ?
O51 C51 1.254(13) . ?
O52 C75 1.571(18) . ?
O52 C84 1.119(14) . ?
O53 C81 1.420(15) . ?
O53 C92 1.140(14) . ?
N51 C61 1.111(18) . ?
N52 C62 1.109(14) . ?
C51 C52 1.450(17) . ?
C51 C55 1.520(15) . ?
C52 C53 1.484(13) . ?
C52 C63 1.313(16) . ?
C53 C54 1.484(16) . ?
C53 C60 1.320(17) . ?
C54 C55 1.349(16) . ?
C54 C59 1.411(15) . ?
C55 C56 1.406(18) . ?
C56 H56 0.9500 . ?
C56 C57 1.440(16) . ?
C57 H57 0.9500 . ?
C57 C58 1.34(2) . ?
C58 H58 0.9500 . ?
C58 C59 1.310(19) . ?
C59 H59 0.9500 . ?
C60 C61 1.42(2) . ?
C60 C62 1.492(13) . ?
C63 H63 0.9500 . ?
C63 C64 1.475(13) . ?
C64 C65 1.412(16) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C65 C66 1.424(13) . ?
C66 C67 1.337(16) . ?
C66 C70 1.518(15) . ?
C67 C68 1.478(13) . ?
C68 C69 1.395(16) . ?
C69 C70 1.551(14) . ?
C69 C71 1.448(13) . ?
C70 C72 1.520(17) . ?
C70 C78 1.506(15) . ?
C71 C71 1.32(2) 3_656 ?
C72 C73 1.357(18) . ?
C72 C77 1.373(17) . ?
C73 H73 0.9500 . ?
C73 C74 1.44(2) . ?
C74 H74 0.9500 . ?
C74 C75 1.28(3) . ?
C75 C76 1.24(2) . ?
C76 H76 0.9500 . ?
C76 C77 1.36(2) . ?
C77 H77 0.9500 . ?
C78 C79 1.466(14) . ?
C78 C83 1.364(16) . ?
C79 H79 0.9500 . ?
C79 C80 1.391(19) . ?
C80 H80 0.9500 . ?
C80 C81 1.32(2) . ?
C81 C82 1.38(2) . ?
C82 H82 0.9500 . ?
C82 C83 1.389(18) . ?
C83 H83 0.9500 . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?
C84 C85 1.508(11) . ?
C85 H85A 0.9900 . ?
C85 H85B 0.9900 . ?
C85 C86 1.442(13) . ?
C86 H86A 0.9900 . ?
C86 H86B 0.9900 . ?
C86 C87 1.503(13) . ?
C87 H87A 0.9900 . ?
C87 H87B 0.9900 . ?
C87 C88 1.506(13) . ?
C88 H88A 0.9900 . ?
C88 H88B 0.9900 . ?
C88 C89 1.493(13) . ?
C89 H89A 0.9900 . ?
C89 H89B 0.9900 . ?
C89 C90 1.534(13) . ?
C90 H90A 0.9900 . ?
C90 H90B 0.9900 . ?
C90 C91 1.511(14) . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C92 C93 1.523(13) . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
C93 H93C 0.9900 . ?
C93 H93D 0.9900 . ?
C93 C94 1.530(15) . ?
C93 C94A 1.557(17) . ?
C94 H94A 0.9900 . ?
C94 H94B 0.9900 . ?
C94 C95 1.534(15) . ?
C95 H95A 0.9900 . ?
C95 H95B 0.9900 . ?
C95 C96 1.528(16) . ?
C96 H96A 0.9900 . ?
C96 H96B 0.9900 . ?
C96 C97 1.534(15) . ?
C97 H97A 0.9900 . ?
C97 H97B 0.9900 . ?
C97 C98 1.534(16) . ?
C98 H98A 0.9900 . ?
C98 H98B 0.9900 . ?
C98 C99 1.528(16) . ?
C99 H99A 0.9800 . ?
C99 H99B 0.9800 . ?
C99 H99C 0.9800 . ?
C94A H94C 0.9900 . ?
C94A H94D 0.9900 . ?
C94A C95A 1.533(17) . ?
C95A H95C 0.9900 . ?
C95A H95D 0.9900 . ?
C95A C96A 1.542(16) . ?
C96A H96C 0.9900 . ?
C96A H96D 0.9900 . ?
C96A C97A 1.530(17) . ?
C97A H97C 0.9900 . ?
C97A H97D 0.9900 . ?
C97A C98A 1.540(17) . ?
C98A H98C 0.9900 . ?
C98A H98D 0.9900 . ?
C98A C99A 1.536(18) . ?
C99A H99D 0.9800 . ?
C99A H99E 0.9800 . ?
C99A H99F 0.9800 . ?
S1 C14 1.769(11) . ?
S1 C17 1.738(10) . ?
S2 C18 1.719(11) . ?
S2 C21 1.734(10) 3_556 ?
O1 C1 1.181(13) . ?
O2 C25 1.298(12) . ?
O2 C34 1.073(14) . ?
O3 C31 1.300(14) . ?
O3 C42 1.181(14) . ?
N1 C11 1.167(16) . ?
N2 C12 1.160(17) . ?
C1 C2 1.496(14) . ?
C1 C5 1.449(16) . ?
C2 C3 1.417(16) . ?
C2 C13 1.453(15) . ?
C3 C4 1.501(14) . ?
C3 C10 1.411(15) . ?
C4 C5 1.434(15) . ?
C4 C9 1.364(16) . ?
C5 C6 1.379(14) . ?
C6 H6 0.9500 . ?
C6 C7 1.314(16) . ?
C7 H7 0.9500 . ?
C7 C8 1.428(15) . ?
C8 H8 0.9500 . ?
C8 C9 1.428(14) . ?
C9 H9 0.9500 . ?
C10 C11 1.421(17) . ?
C10 C12 1.378(19) . ?
C13 H13 0.9500 . ?
C13 C14 1.339(15) . ?
C14 C15 1.403(14) . ?
C15 H15 0.9500 . ?
C15 C16 1.337(16) . ?
C16 C17 1.429(13) . ?
C16 C20 1.605(14) . ?
C17 C18 1.410(15) . ?
C18 C19 1.397(14) . ?
C19 C20 1.487(15) . ?
C19 C21 1.363(15) . ?
C20 C22 1.506(15) . ?
C20 C28 1.563(17) . ?
C21 C21 1.48(2) 3_556 ?
C22 C23 1.419(19) . ?
C22 C27 1.419(18) . ?
C23 H23 0.9500 . ?
C23 C24 1.39(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.41(3) . ?
C25 C26 1.46(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.340(19) . ?
C27 H27 0.9500 . ?
C28 C29 1.312(18) . ?
C28 C33 1.421(19) . ?
C29 H29 0.9500 . ?
C29 C30 1.369(18) . ?
C30 H30 0.9500 . ?
C30 C31 1.43(2) . ?
C31 C32 1.41(2) . ?
C32 H32 0.9500 . ?
C32 C33 1.366(19) . ?
C33 H33 0.9500 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.442(12) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.398(13) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.498(16) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.451(17) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.477(16) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.474(17) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.423(15) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.614(18) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.61(2) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.61(2) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.61(2) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.59(2) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.61(2) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.61(2) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
O216 C216 1.33(3) . ?
C216 C217 1.49(2) . ?
C216 C218 1.50(2) . ?
C217 H21A 0.9800 . ?
C217 H21B 0.9800 . ?
C217 H21C 0.9800 . ?
C218 H21D 0.9800 . ?
C218 H21E 0.9800 . ?
C218 H21F 0.9800 . ?
O201 C201 1.32(3) . ?
C201 C202 1.491(19) . ?
C201 C203 1.51(2) . ?
C202 H20A 0.9800 . ?
C202 H20B 0.9800 . ?
C202 H20C 0.9800 . ?
C203 H20D 0.9800 . ?
C203 H20E 0.9800 . ?
C203 H20F 0.9800 . ?
O211 C211 1.30(3) . ?
C211 C212 1.498(19) . ?
C211 C213 1.50(2) . ?
C212 H21G 0.9800 . ?
C212 H21H 0.9800 . ?
C212 H21I 0.9800 . ?
C213 H21J 0.9800 . ?
C213 H21K 0.9800 . ?
C213 H21L 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
C67 S51 C64 88.3(5) . . ?
C68 S52 C71 88.9(5) . 3_656 ?
C84 O52 C75 112.5(13) . . ?
C92 O53 C81 125.4(16) . . ?
O51 C51 C52 128.6(10) . . ?
O51 C51 C55 123.5(11) . . ?
C52 C51 C55 107.7(9) . . ?
C51 C52 C53 106.8(10) . . ?
C63 C52 C51 125.8(10) . . ?
C63 C52 C53 127.4(11) . . ?
C54 C53 C52 106.1(10) . . ?
C60 C53 C52 127.6(11) . . ?
C60 C53 C54 126.3(10) . . ?
C55 C54 C53 111.6(9) . . ?
C55 C54 C59 115.2(12) . . ?
C59 C54 C53 133.1(11) . . ?
C54 C55 C51 107.6(11) . . ?
C54 C55 C56 127.1(11) . . ?
C56 C55 C51 125.0(11) . . ?
C55 C56 H56 123.5 . . ?
C55 C56 C57 113.0(12) . . ?
C57 C56 H56 123.5 . . ?
C56 C57 H57 120.4 . . ?
C58 C57 C56 119.2(13) . . ?
C58 C57 H57 120.4 . . ?
C57 C58 H58 117.5 . . ?
C59 C58 C57 125.1(12) . . ?
C59 C58 H58 117.5 . . ?
C54 C59 H59 119.9 . . ?
C58 C59 C54 120.2(12) . . ?
C58 C59 H59 119.9 . . ?
C53 C60 C61 127.7(10) . . ?
C53 C60 C62 123.3(11) . . ?
C61 C60 C62 109.0(10) . . ?
N51 C61 C60 175(3) . . ?
N52 C62 C60 173.5(18) . . ?
C52 C63 H63 112.5 . . ?
C52 C63 C64 135.1(11) . . ?
C64 C63 H63 112.5 . . ?
C63 C64 S51 126.8(9) . . ?
C65 C64 S51 113.2(8) . . ?
C65 C64 C63 119.8(10) . . ?
C64 C65 H65A 109.6 . . ?
C64 C65 H65B 109.6 . . ?
C64 C65 C66 110.1(10) . . ?
H65A C65 H65B 108.2 . . ?
C66 C65 H65A 109.6 . . ?
C66 C65 H65B 109.6 . . ?
C65 C66 C70 132.4(11) . . ?
C67 C66 C65 110.5(10) . . ?
C67 C66 C70 117.1(9) . . ?
C66 C67 S51 117.8(8) . . ?
C66 C67 C68 107.3(9) . . ?
C68 C67 S51 134.9(9) . . ?
C67 C68 S52 138.9(9) . . ?
C69 C68 S52 114.5(8) . . ?
C69 C68 C67 106.5(9) . . ?
C68 C69 C70 113.7(9) . . ?
C68 C69 C71 109.0(9) . . ?
C71 C69 C70 137.3(10) . . ?
C66 C70 C69 95.4(9) . . ?
C66 C70 C72 114.8(9) . . ?
C72 C70 C69 111.5(9) . . ?
C78 C70 C66 109.9(9) . . ?
C78 C70 C69 111.5(8) . . ?
C78 C70 C72 112.6(10) . . ?
C69 C71 S52 132.4(9) . 3_656 ?
C71 C71 S52 113.9(10) 3_656 3_656 ?
C71 C71 C69 113.6(12) 3_656 . ?
C73 C72 C70 122.2(12) . . ?
C73 C72 C77 115.6(14) . . ?
C77 C72 C70 122.1(13) . . ?
C72 C73 H73 121.0 . . ?
C72 C73 C74 118.0(14) . . ?
C74 C73 H73 121.0 . . ?
C73 C74 H74 119.7 . . ?
C75 C74 C73 120.6(16) . . ?
C75 C74 H74 119.7 . . ?
C74 C75 O52 128.0(17) . . ?
C76 C75 O52 109.4(18) . . ?
C76 C75 C74 122.5(18) . . ?
C75 C76 H76 119.7 . . ?
C75 C76 C77 120.5(17) . . ?
C77 C76 H76 119.7 . . ?
C72 C77 H77 119.0 . . ?
C76 C77 C72 122.1(17) . . ?
C76 C77 H77 119.0 . . ?
C79 C78 C70 123.0(10) . . ?
C83 C78 C70 119.1(9) . . ?
C83 C78 C79 117.3(11) . . ?
C78 C79 H79 120.6 . . ?
C80 C79 C78 118.8(11) . . ?
C80 C79 H79 120.6 . . ?
C79 C80 H80 119.2 . . ?
C81 C80 C79 121.7(12) . . ?
C81 C80 H80 119.2 . . ?
C80 C81 O53 120.2(14) . . ?
C80 C81 C82 120.5(12) . . ?
C82 C81 O53 118.9(15) . . ?
C81 C82 H82 119.5 . . ?
C81 C82 C83 120.9(13) . . ?
C83 C82 H82 119.5 . . ?
C78 C83 C82 120.6(12) . . ?
C78 C83 H83 119.7 . . ?
C82 C83 H83 119.7 . . ?
O52 C84 H84A 106.8 . . ?
O52 C84 H84B 106.8 . . ?
O52 C84 C85 122.1(17) . . ?
H84A C84 H84B 106.7 . . ?
C85 C84 H84A 106.8 . . ?
C85 C84 H84B 106.8 . . ?
C84 C85 H85A 102.6 . . ?
C84 C85 H85B 102.6 . . ?
H85A C85 H85B 105.0 . . ?
C86 C85 C84 137.9(15) . . ?
C86 C85 H85A 102.6 . . ?
C86 C85 H85B 102.6 . . ?
C85 C86 H86A 107.9 . . ?
C85 C86 H86B 107.9 . . ?
C85 C86 C87 117.7(13) . . ?
H86A C86 H86B 107.2 . . ?
C87 C86 H86A 107.9 . . ?
C87 C86 H86B 107.9 . . ?
C86 C87 H87A 106.6 . . ?
C86 C87 H87B 106.6 . . ?
C86 C87 C88 122.8(14) . . ?
H87A C87 H87B 106.6 . . ?
C88 C87 H87A 106.6 . . ?
C88 C87 H87B 106.6 . . ?
C87 C88 H88A 108.4 . . ?
C87 C88 H88B 108.4 . . ?
H88A C88 H88B 107.5 . . ?
C89 C88 C87 115.5(12) . . ?
C89 C88 H88A 108.4 . . ?
C89 C88 H88B 108.4 . . ?
C88 C89 H89A 109.3 . . ?
C88 C89 H89B 109.3 . . ?
C88 C89 C90 111.7(12) . . ?
H89A C89 H89B 107.9 . . ?
C90 C89 H89A 109.3 . . ?
C90 C89 H89B 109.3 . . ?
C89 C90 H90A 109.3 . . ?
C89 C90 H90B 109.3 . . ?
H90A C90 H90B 108.0 . . ?
C91 C90 C89 111.5(15) . . ?
C91 C90 H90A 109.3 . . ?
C91 C90 H90B 109.3 . . ?
C90 C91 H91A 109.5 . . ?
C90 C91 H91B 109.5 . . ?
C90 C91 H91C 109.5 . . ?
H91A C91 H91B 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
O53 C92 H92A 106.6 . . ?
O53 C92 H92B 106.6 . . ?
O53 C92 C93 123.0(16) . . ?
H92A C92 H92B 106.5 . . ?
C93 C92 H92A 106.6 . . ?
C93 C92 H92B 106.6 . . ?
C92 C93 H93A 107.0 . . ?
C92 C93 H93B 107.0 . . ?
C92 C93 H93C 108.1 . . ?
C92 C93 H93D 108.1 . . ?
C92 C93 C94 121.4(19) . . ?
C92 C93 C94A 116.9(16) . . ?
H93A C93 H93B 106.7 . . ?
H93C C93 H93D 107.3 . . ?
C94 C93 H93A 107.0 . . ?
C94 C93 H93B 107.0 . . ?
C94A C93 H93C 108.1 . . ?
C94A C93 H93D 108.1 . . ?
C93 C94 H94A 108.0 . . ?
C93 C94 H94B 108.0 . . ?
C93 C94 C95 117(2) . . ?
H94A C94 H94B 107.2 . . ?
C95 C94 H94A 108.0 . . ?
C95 C94 H94B 108.0 . . ?
C94 C95 H95A 106.8 . . ?
C94 C95 H95B 106.8 . . ?
H95A C95 H95B 106.6 . . ?
C96 C95 C94 122(3) . . ?
C96 C95 H95A 106.8 . . ?
C96 C95 H95B 106.8 . . ?
C95 C96 H96A 108.1 . . ?
C95 C96 H96B 108.1 . . ?
C95 C96 C97 117(2) . . ?
H96A C96 H96B 107.3 . . ?
C97 C96 H96A 108.1 . . ?
C97 C96 H96B 108.1 . . ?
C96 C97 H97A 108.2 . . ?
C96 C97 H97B 108.2 . . ?
C96 C97 C98 116(2) . . ?
H97A C97 H97B 107.4 . . ?
C98 C97 H97A 108.2 . . ?
C98 C97 H97B 108.2 . . ?
C97 C98 H98A 108.2 . . ?
C97 C98 H98B 108.2 . . ?
H98A C98 H98B 107.3 . . ?
C99 C98 C97 116(2) . . ?
C99 C98 H98A 108.2 . . ?
C99 C98 H98B 108.2 . . ?
C98 C99 H99A 109.5 . . ?
C98 C99 H99B 109.5 . . ?
C98 C99 H99C 109.5 . . ?
H99A C99 H99B 109.5 . . ?
H99A C99 H99C 109.5 . . ?
H99B C99 H99C 109.5 . . ?
C93 C94A H94C 106.9 . . ?
C93 C94A H94D 106.9 . . ?
H94C C94A H94D 106.7 . . ?
C95A C94A C93 122(2) . . ?
C95A C94A H94C 106.9 . . ?
C95A C94A H94D 106.9 . . ?
C94A C95A H95C 107.1 . . ?
C94A C95A H95D 107.1 . . ?
C94A C95A C96A 121.1(19) . . ?
H95C C95A H95D 106.8 . . ?
C96A C95A H95C 107.1 . . ?
C96A C95A H95D 107.1 . . ?
C95A C96A H96C 108.0 . . ?
C95A C96A H96D 108.0 . . ?
H96C C96A H96D 107.2 . . ?
C97A C96A C95A 117.3(19) . . ?
C97A C96A H96C 108.0 . . ?
C97A C96A H96D 108.0 . . ?
C96A C97A H97C 107.8 . . ?
C96A C97A H97D 107.8 . . ?
C96A C97A C98A 118(2) . . ?
H97C C97A H97D 107.2 . . ?
C98A C97A H97C 107.8 . . ?
C98A C97A H97D 107.8 . . ?
C97A C98A H98C 107.8 . . ?
C97A C98A H98D 107.8 . . ?
H98C C98A H98D 107.1 . . ?
C99A C98A C97A 118(2) . . ?
C99A C98A H98C 107.7 . . ?
C99A C98A H98D 107.7 . . ?
C98A C99A H99D 109.5 . . ?
C98A C99A H99E 109.5 . . ?
C98A C99A H99F 109.5 . . ?
H99D C99A H99E 109.5 . . ?
H99D C99A H99F 109.5 . . ?
H99E C99A H99F 109.5 . . ?
C17 S1 C14 92.3(5) . . ?
C18 S2 C21 90.7(5) . 3_556 ?
C34 O2 C25 155(2) . . ?
C42 O3 C31 132.3(17) . . ?
O1 C1 C2 127.6(11) . . ?
O1 C1 C5 127.3(10) . . ?
C5 C1 C2 104.9(10) . . ?
C3 C2 C1 109.4(9) . . ?
C3 C2 C13 127.0(10) . . ?
C13 C2 C1 123.4(11) . . ?
C2 C3 C4 108.3(9) . . ?
C10 C3 C2 131.6(11) . . ?
C10 C3 C4 120.2(11) . . ?
C5 C4 C3 105.8(10) . . ?
C9 C4 C3 133.0(9) . . ?
C9 C4 C5 121.2(9) . . ?
C4 C5 C1 111.6(9) . . ?
C6 C5 C1 131.1(10) . . ?
C6 C5 C4 117.3(10) . . ?
C5 C6 H6 118.6 . . ?
C7 C6 C5 122.8(9) . . ?
C7 C6 H6 118.6 . . ?
C6 C7 H7 119.0 . . ?
C6 C7 C8 122.1(10) . . ?
C8 C7 H7 119.0 . . ?
C7 C8 H8 121.6 . . ?
C7 C8 C9 116.7(11) . . ?
C9 C8 H8 121.6 . . ?
C4 C9 C8 119.9(10) . . ?
C4 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C3 C10 C11 120.4(12) . . ?
C12 C10 C3 126.8(11) . . ?
C12 C10 C11 112.7(10) . . ?
N1 C11 C10 173.8(19) . . ?
N2 C12 C10 175.9(19) . . ?
C2 C13 H13 113.0 . . ?
C14 C13 C2 134.0(9) . . ?
C14 C13 H13 113.0 . . ?
C13 C14 S1 129.4(8) . . ?
C13 C14 C15 121.1(10) . . ?
C15 C14 S1 109.5(9) . . ?
C14 C15 H15 123.0 . . ?
C16 C15 C14 113.9(10) . . ?
C16 C15 H15 123.0 . . ?
C15 C16 C17 115.8(9) . . ?
C15 C16 C20 139.1(9) . . ?
C17 C16 C20 105.1(9) . . ?
C16 C17 S1 108.4(8) . . ?
C18 C17 S1 139.6(8) . . ?
C18 C17 C16 111.9(9) . . ?
C17 C18 S2 136.2(8) . . ?
C19 C18 S2 114.6(9) . . ?
C19 C18 C17 109.2(9) . . ?
C18 C19 C20 111.6(10) . . ?
C21 C19 C18 111.7(10) . . ?
C21 C19 C20 136.7(9) . . ?
C19 C20 C16 101.9(8) . . ?
C19 C20 C22 110.1(10) . . ?
C19 C20 C28 114.0(10) . . ?
C22 C20 C16 110.6(10) . . ?
C22 C20 C28 114.0(9) . . ?
C28 C20 C16 105.4(9) . . ?
C19 C21 S2 136.9(9) . 3_556 ?
C19 C21 C21 112.9(10) . 3_556 ?
C21 C21 S2 109.9(11) 3_556 3_556 ?
C23 C22 C20 124.5(11) . . ?
C27 C22 C20 119.2(13) . . ?
C27 C22 C23 116.3(13) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 C22 121.5(16) . . ?
C24 C23 H23 119.2 . . ?
C23 C24 H24 119.5 . . ?
C23 C24 C25 121.0(19) . . ?
C25 C24 H24 119.5 . . ?
O2 C25 C24 128(2) . . ?
O2 C25 C26 115.3(18) . . ?
C24 C25 C26 117.2(12) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 C25 119.9(17) . . ?
C27 C26 H26 120.1 . . ?
C22 C27 H27 118.3 . . ?
C26 C27 C22 123.5(18) . . ?
C26 C27 H27 118.3 . . ?
C29 C28 C20 122.1(12) . . ?
C29 C28 C33 118.6(13) . . ?
C33 C28 C20 119.3(12) . . ?
C28 C29 H29 118.6 . . ?
C28 C29 C30 122.7(14) . . ?
C30 C29 H29 118.6 . . ?
C29 C30 H30 120.1 . . ?
C29 C30 C31 119.9(15) . . ?
C31 C30 H30 120.1 . . ?
O3 C31 C30 119.4(16) . . ?
O3 C31 C32 122.7(14) . . ?
C32 C31 C30 117.5(12) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 C31 119.0(14) . . ?
C33 C32 H32 120.5 . . ?
C28 C33 H33 119.1 . . ?
C32 C33 C28 121.9(15) . . ?
C32 C33 H33 119.1 . . ?
O2 C34 H34A 103.3 . . ?
O2 C34 H34B 103.3 . . ?
O2 C34 C35 136(2) . . ?
H34A C34 H34B 105.2 . . ?
C35 C34 H34A 103.3 . . ?
C35 C34 H34B 103.3 . . ?
C34 C35 H35A 106.2 . . ?
C34 C35 H35B 106.2 . . ?
H35A C35 H35B 106.4 . . ?
C36 C35 C34 124.4(18) . . ?
C36 C35 H35A 106.2 . . ?
C36 C35 H35B 106.2 . . ?
C35 C36 H36A 108.8 . . ?
C35 C36 H36B 108.8 . . ?
C35 C36 C37 113.6(17) . . ?
H36A C36 H36B 107.7 . . ?
C37 C36 H36A 108.8 . . ?
C37 C36 H36B 108.8 . . ?
C36 C37 H37A 109.9 . . ?
C36 C37 H37B 109.9 . . ?
H37A C37 H37B 108.3 . . ?
C38 C37 C36 108.7(19) . . ?
C38 C37 H37A 109.9 . . ?
C38 C37 H37B 109.9 . . ?
C37 C38 H38A 108.4 . . ?
C37 C38 H38B 108.4 . . ?
C37 C38 C39 115.4(19) . . ?
H38A C38 H38B 107.5 . . ?
C39 C38 H38A 108.4 . . ?
C39 C38 H38B 108.4 . . ?
C38 C39 H39A 110.6 . . ?
C38 C39 H39B 110.6 . . ?
H39A C39 H39B 108.7 . . ?
C40 C39 C38 105.9(18) . . ?
C40 C39 H39A 110.6 . . ?
C40 C39 H39B 110.6 . . ?
C39 C40 H40A 108.7 . . ?
C39 C40 H40B 108.7 . . ?
H40A C40 H40B 107.6 . . ?
C41 C40 C39 114.3(18) . . ?
C41 C40 H40A 108.7 . . ?
C41 C40 H40B 108.7 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O3 C42 H42A 109.2 . . ?
O3 C42 H42B 109.2 . . ?
O3 C42 C43 111.9(15) . . ?
H42A C42 H42B 107.9 . . ?
C43 C42 H42A 109.2 . . ?
C43 C42 H42B 109.2 . . ?
C42 C43 H43A 111.2 . . ?
C42 C43 H43B 111.2 . . ?
C42 C43 C44 102.7(16) . . ?
H43A C43 H43B 109.1 . . ?
C44 C43 H43A 111.2 . . ?
C44 C43 H43B 111.2 . . ?
C43 C44 H44A 109.1 . . ?
C43 C44 H44B 109.1 . . ?
H44A C44 H44B 107.8 . . ?
C45 C44 C43 112(2) . . ?
C45 C44 H44A 109.1 . . ?
C45 C44 H44B 109.1 . . ?
C44 C45 H45A 110.3 . . ?
C44 C45 H45B 110.3 . . ?
C44 C45 C46 107(2) . . ?
H45A C45 H45B 108.5 . . ?
C46 C45 H45A 110.3 . . ?
C46 C45 H45B 110.3 . . ?
C45 C46 H46A 111.0 . . ?
C45 C46 H46B 111.0 . . ?
H46A C46 H46B 109.0 . . ?
C47 C46 C45 104(2) . . ?
C47 C46 H46A 111.0 . . ?
C47 C46 H46B 111.0 . . ?
C46 C47 H47A 111.2 . . ?
C46 C47 H47B 111.2 . . ?
C46 C47 C48 103(2) . . ?
H47A C47 H47B 109.1 . . ?
C48 C47 H47A 111.2 . . ?
C48 C47 H47B 111.2 . . ?
C47 C48 H48A 111.6 . . ?
C47 C48 H48B 111.6 . . ?
H48A C48 H48B 109.4 . . ?
C49 C48 C47 101(2) . . ?
C49 C48 H48A 111.6 . . ?
C49 C48 H48B 111.6 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O216 C216 C217 119(3) . . ?
O216 C216 C218 119(3) . . ?
C217 C216 C218 115(3) . . ?
C216 C217 H21A 109.5 . . ?
C216 C217 H21B 109.5 . . ?
C216 C217 H21C 109.5 . . ?
H21A C217 H21B 109.5 . . ?
H21A C217 H21C 109.5 . . ?
H21B C217 H21C 109.5 . . ?
C216 C218 H21D 109.5 . . ?
C216 C218 H21E 109.5 . . ?
C216 C218 H21F 109.5 . . ?
H21D C218 H21E 109.5 . . ?
H21D C218 H21F 109.5 . . ?
H21E C218 H21F 109.5 . . ?
O201 C201 C202 124(2) . . ?
O201 C201 C203 118.7(19) . . ?
C202 C201 C203 118(2) . . ?
C201 C202 H20A 109.5 . . ?
C201 C202 H20B 109.5 . . ?
C201 C202 H20C 109.5 . . ?
H20A C202 H20B 109.5 . . ?
H20A C202 H20C 109.5 . . ?
H20B C202 H20C 109.5 . . ?
C201 C203 H20D 109.5 . . ?
C201 C203 H20E 109.5 . . ?
C201 C203 H20F 109.5 . . ?
H20D C203 H20E 109.5 . . ?
H20D C203 H20F 109.5 . . ?
H20E C203 H20F 109.5 . . ?
O211 C211 C212 118.4(19) . . ?
O211 C211 C213 127(2) . . ?
C212 C211 C213 114(2) . . ?
C211 C212 H21G 109.5 . . ?
C211 C212 H21H 109.5 . . ?
C211 C212 H21I 109.5 . . ?
H21G C212 H21H 109.5 . . ?
H21G C212 H21I 109.5 . . ?
H21H C212 H21I 109.5 . . ?
C211 C213 H21J 109.5 . . ?
C211 C213 H21K 109.5 . . ?
C211 C213 H21L 109.5 . . ?
H21J C213 H21K 109.5 . . ?
H21J C213 H21L 109.5 . . ?
H21K C213 H21L 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
S51 C64 C65 C66 1.1(13) . . . . ?
S51 C67 C68 S52 5.1(19) . . . . ?
S51 C67 C68 C69 -179.3(9) . . . . ?
S52 C68 C69 C70 178.8(7) . . . . ?
S52 C68 C69 C71 0.2(11) . . . . ?
O51 C51 C52 C53 -179.7(14) . . . . ?
O51 C51 C52 C63 -2(2) . . . . ?
O51 C51 C55 C54 -179.5(13) . . . . ?
O51 C51 C55 C56 7(2) . . . . ?
O52 C75 C76 C77 -173.4(14) . . . . ?
O52 C84 C85 C86 30(4) . . . . ?
O53 C81 C82 C83 -175.9(14) . . . . ?
O53 C92 C93 C94 12(3) . . . . ?
O53 C92 C93 C94A 77(4) . . . . ?
C51 C52 C53 C54 -3.9(16) . . . . ?
C51 C52 C53 C60 176.6(17) . . . . ?
C51 C52 C63 C64 7(3) . . . . ?
C51 C55 C56 C57 176.0(13) . . . . ?
C52 C51 C55 C54 -3.5(15) . . . . ?
C52 C51 C55 C56 -177.0(13) . . . . ?
C52 C53 C54 C55 1.8(17) . . . . ?
C52 C53 C54 C59 -178.9(16) . . . . ?
C52 C53 C60 C61 -1(3) . . . . ?
C52 C53 C60 C62 178.7(15) . . . . ?
C52 C63 C64 S51 -2(2) . . . . ?
C52 C63 C64 C65 174.2(15) . . . . ?
C53 C52 C63 C64 -175.3(13) . . . . ?
C53 C54 C55 C51 1.0(16) . . . . ?
C53 C54 C55 C56 174.3(14) . . . . ?
C53 C54 C59 C58 -176.9(18) . . . . ?
C54 C53 C60 C61 179.2(19) . . . . ?
C54 C53 C60 C62 -1(3) . . . . ?
C54 C55 C56 C57 4(2) . . . . ?
C55 C51 C52 C53 4.6(15) . . . . ?
C55 C51 C52 C63 -177.4(13) . . . . ?
C55 C54 C59 C58 2(2) . . . . ?
C55 C56 C57 C58 0(2) . . . . ?
C56 C57 C58 C59 -3(3) . . . . ?
C57 C58 C59 C54 1(3) . . . . ?
C59 C54 C55 C51 -178.4(13) . . . . ?
C59 C54 C55 C56 -5(2) . . . . ?
C60 C53 C54 C55 -178.8(16) . . . . ?
C60 C53 C54 C59 1(3) . . . . ?
C63 C52 C53 C54 178.1(14) . . . . ?
C63 C52 C53 C60 -1(3) . . . . ?
C63 C64 C65 C66 -175.7(10) . . . . ?
C64 S51 C67 C66 1.8(10) . . . . ?
C64 S51 C67 C68 -179.9(11) . . . . ?
C64 C65 C66 C67 0.2(14) . . . . ?
C64 C65 C66 C70 -179.4(11) . . . . ?
C65 C66 C67 S51 -1.5(13) . . . . ?
C65 C66 C67 C68 179.8(9) . . . . ?
C65 C66 C70 C69 -178.8(12) . . . . ?
C65 C66 C70 C72 -62.1(16) . . . . ?
C65 C66 C70 C78 66.0(16) . . . . ?
C66 C67 C68 S52 -176.4(10) . . . . ?
C66 C67 C68 C69 -0.9(12) . . . . ?
C66 C70 C72 C73 163.0(12) . . . . ?
C66 C70 C72 C77 -20.3(16) . . . . ?
C66 C70 C78 C79 96.6(13) . . . . ?
C66 C70 C78 C83 -74.7(14) . . . . ?
C67 S51 C64 C63 175.0(11) . . . . ?
C67 S51 C64 C65 -1.5(9) . . . . ?
C67 C66 C70 C69 1.6(12) . . . . ?
C67 C66 C70 C72 118.3(11) . . . . ?
C67 C66 C70 C78 -113.6(11) . . . . ?
C67 C68 C69 C70 2.0(12) . . . . ?
C67 C68 C69 C71 -176.6(8) . . . . ?
C68 C69 C70 C66 -2.1(11) . . . . ?
C68 C69 C70 C72 -121.5(10) . . . . ?
C68 C69 C70 C78 111.8(10) . . . . ?
C68 C69 C71 S52 177.2(8) . . . 3_656 ?
C68 C69 C71 C71 2.7(16) . . . 3_656 ?
C69 C70 C72 C73 -89.9(15) . . . . ?
C69 C70 C72 C77 86.8(13) . . . . ?
C69 C70 C78 C79 -7.9(16) . . . . ?
C69 C70 C78 C83 -179.2(11) . . . . ?
C70 C66 C67 S51 178.2(8) . . . . ?
C70 C66 C67 C68 -0.6(13) . . . . ?
C70 C69 C71 S52 -0.9(19) . . . 3_656 ?
C70 C69 C71 C71 -175.4(12) . . . 3_656 ?
C70 C72 C73 C74 -177.2(13) . . . . ?
C70 C72 C77 C76 -176.3(13) . . . . ?
C70 C78 C79 C80 -172.5(12) . . . . ?
C70 C78 C83 C82 173.7(12) . . . . ?
C71 S52 C68 C67 173.2(12) 3_656 . . . ?
C71 S52 C68 C69 -2.1(8) 3_656 . . . ?
C71 C69 C70 C66 175.9(12) . . . . ?
C71 C69 C70 C72 56.6(15) . . . . ?
C71 C69 C70 C78 -70.2(16) . . . . ?
C72 C70 C78 C79 -134.1(11) . . . . ?
C72 C70 C78 C83 54.6(14) . . . . ?
C72 C73 C74 C75 -7(3) . . . . ?
C73 C72 C77 C76 1(2) . . . . ?
C73 C74 C75 O52 -179.5(16) . . . . ?
C73 C74 C75 C76 0(3) . . . . ?
C74 C75 C76 C77 7(3) . . . . ?
C75 O52 C84 C85 -177.1(18) . . . . ?
C75 C76 C77 C72 -8(3) . . . . ?
C77 C72 C73 C74 6(2) . . . . ?
C78 C70 C72 C73 36.3(15) . . . . ?
C78 C70 C72 C77 -147.1(11) . . . . ?
C78 C79 C80 C81 -2(2) . . . . ?
C79 C78 C83 C82 1.9(18) . . . . ?
C79 C80 C81 O53 176.7(14) . . . . ?
C79 C80 C81 C82 3(3) . . . . ?
C80 C81 C82 C83 -2(3) . . . . ?
C81 O53 C92 C93 -158.8(19) . . . . ?
C81 C82 C83 C78 0(2) . . . . ?
C83 C78 C79 C80 -1.1(19) . . . . ?
C84 O52 C75 C74 -11(3) . . . . ?
C84 O52 C75 C76 170(2) . . . . ?
C84 C85 C86 C87 167(2) . . . . ?
C85 C86 C87 C88 -178.4(18) . . . . ?
C86 C87 C88 C89 -175.1(17) . . . . ?
C87 C88 C89 C90 172.1(15) . . . . ?
C88 C89 C90 C91 63(2) . . . . ?
C92 O53 C81 C80 -24(3) . . . . ?
C92 O53 C81 C82 149(2) . . . . ?
C92 C93 C94 C95 77(4) . . . . ?
C92 C93 C94A C95A 21(7) . . . . ?
C93 C94 C95 C96 96(5) . . . . ?
C93 C94A C95A C96A 149(4) . . . . ?
C94 C95 C96 C97 112(7) . . . . ?
C95 C96 C97 C98 13(9) . . . . ?
C96 C97 C98 C99 136(8) . . . . ?
C94A C95A C96A C97A 44(6) . . . . ?
C95A C96A C97A C98A -4(6) . . . . ?
C96A C97A C98A C99A 95(6) . . . . ?
S1 C14 C15 C16 2.3(14) . . . . ?
S1 C17 C18 S2 -1(2) . . . . ?
S1 C17 C18 C19 177.2(11) . . . . ?
S2 C18 C19 C20 -178.2(8) . . . . ?
S2 C18 C19 C21 1.6(14) . . . . ?
O1 C1 C2 C3 -177.8(13) . . . . ?
O1 C1 C2 C13 6(2) . . . . ?
O1 C1 C5 C4 178.0(13) . . . . ?
O1 C1 C5 C6 -5(2) . . . . ?
O2 C25 C26 C27 174.0(16) . . . . ?
O2 C34 C35 C36 76(4) . . . . ?
O3 C31 C32 C33 176.9(15) . . . . ?
O3 C42 C43 C44 -99(2) . . . . ?
C1 C2 C3 C4 1.1(15) . . . . ?
C1 C2 C3 C10 -179.4(13) . . . . ?
C1 C2 C13 C14 1(3) . . . . ?
C1 C5 C6 C7 -177.4(14) . . . . ?
C2 C1 C5 C4 2.3(14) . . . . ?
C2 C1 C5 C6 179.6(13) . . . . ?
C2 C3 C4 C5 0.2(15) . . . . ?
C2 C3 C4 C9 -176.6(17) . . . . ?
C2 C3 C10 C11 1(3) . . . . ?
C2 C3 C10 C12 -174.0(16) . . . . ?
C2 C13 C14 S1 0(2) . . . . ?
C2 C13 C14 C15 178.2(15) . . . . ?
C3 C2 C13 C14 -174.1(14) . . . . ?
C3 C4 C5 C1 -1.6(15) . . . . ?
C3 C4 C5 C6 -179.3(11) . . . . ?
C3 C4 C9 C8 178.7(16) . . . . ?
C4 C3 C10 C11 -179.7(16) . . . . ?
C4 C3 C10 C12 5(2) . . . . ?
C4 C5 C6 C7 -0.3(19) . . . . ?
C5 C1 C2 C3 -2.1(14) . . . . ?
C5 C1 C2 C13 -177.8(13) . . . . ?
C5 C4 C9 C8 2(2) . . . . ?
C5 C6 C7 C8 2(2) . . . . ?
C6 C7 C8 C9 -2(2) . . . . ?
C7 C8 C9 C4 0(2) . . . . ?
C9 C4 C5 C1 175.7(13) . . . . ?
C9 C4 C5 C6 -2(2) . . . . ?
C10 C3 C4 C5 -179.3(12) . . . . ?
C10 C3 C4 C9 4(2) . . . . ?
C13 C2 C3 C4 176.7(14) . . . . ?
C13 C2 C3 C10 -4(2) . . . . ?
C13 C14 C15 C16 -176.3(12) . . . . ?
C14 S1 C17 C16 1.2(9) . . . . ?
C14 S1 C17 C18 -175.9(14) . . . . ?
C14 C15 C16 C17 -1.4(16) . . . . ?
C14 C15 C16 C20 180.0(13) . . . . ?
C15 C16 C17 S1 -0.2(13) . . . . ?
C15 C16 C17 C18 177.8(11) . . . . ?
C15 C16 C20 C19 -176.6(14) . . . . ?
C15 C16 C20 C22 -59.6(19) . . . . ?
C15 C16 C20 C28 64.1(18) . . . . ?
C16 C17 C18 S2 -178.0(10) . . . . ?
C16 C17 C18 C19 0.1(14) . . . . ?
C16 C20 C22 C23 -24.1(17) . . . . ?
C16 C20 C22 C27 156.6(12) . . . . ?
C16 C20 C28 C29 107.6(12) . . . . ?
C16 C20 C28 C33 -71.0(12) . . . . ?
C17 S1 C14 C13 176.4(13) . . . . ?
C17 S1 C14 C15 -2.0(10) . . . . ?
C17 C16 C20 C19 4.7(11) . . . . ?
C17 C16 C20 C22 121.7(10) . . . . ?
C17 C16 C20 C28 -114.6(10) . . . . ?
C17 C18 C19 C20 3.3(14) . . . . ?
C17 C18 C19 C21 -176.9(10) . . . . ?
C18 C19 C20 C16 -4.9(13) . . . . ?
C18 C19 C20 C22 -122.3(11) . . . . ?
C18 C19 C20 C28 108.1(11) . . . . ?
C18 C19 C21 S2 -176.8(10) . . . 3_556 ?
C18 C19 C21 C21 -4.6(17) . . . 3_556 ?
C19 C20 C22 C23 87.8(15) . . . . ?
C19 C20 C22 C27 -91.5(15) . . . . ?
C19 C20 C28 C29 -3.3(15) . . . . ?
C19 C20 C28 C33 178.1(10) . . . . ?
C20 C16 C17 S1 178.9(7) . . . . ?
C20 C16 C17 C18 -3.1(12) . . . . ?
C20 C19 C21 S2 3(2) . . . 3_556 ?
C20 C19 C21 C21 175.1(13) . . . 3_556 ?
C20 C22 C23 C24 178.9(14) . . . . ?
C20 C22 C27 C26 173.7(16) . . . . ?
C20 C28 C29 C30 -177.3(11) . . . . ?
C20 C28 C33 C32 175.0(11) . . . . ?
C21 S2 C18 C17 179.5(13) 3_556 . . . ?
C21 S2 C18 C19 1.5(10) 3_556 . . . ?
C21 C19 C20 C16 175.4(14) . . . . ?
C21 C19 C20 C22 58.0(19) . . . . ?
C21 C19 C20 C28 -71.6(17) . . . . ?
C22 C20 C28 C29 -130.9(12) . . . . ?
C22 C20 C28 C33 50.4(14) . . . . ?
C22 C23 C24 C25 4(3) . . . . ?
C23 C22 C27 C26 -6(3) . . . . ?
C23 C24 C25 O2 178.8(18) . . . . ?
C23 C24 C25 C26 0(3) . . . . ?
C24 C25 C26 C27 -7(3) . . . . ?
C25 O2 C34 C35 -177(3) . . . . ?
C25 C26 C27 C22 10(3) . . . . ?
C27 C22 C23 C24 -2(2) . . . . ?
C28 C20 C22 C23 -142.6(13) . . . . ?
C28 C20 C22 C27 38.1(17) . . . . ?
C28 C29 C30 C31 4(2) . . . . ?
C29 C28 C33 C32 -3.7(19) . . . . ?
C29 C30 C31 O3 -179.4(14) . . . . ?
C29 C30 C31 C32 -7(2) . . . . ?
C30 C31 C32 C33 5(2) . . . . ?
C31 O3 C42 C43 169.0(19) . . . . ?
C31 C32 C33 C28 1(2) . . . . ?
C33 C28 C29 C30 1.4(19) . . . . ?
C34 O2 C25 C24 170(4) . . . . ?
C34 O2 C25 C26 -11(6) . . . . ?
C34 C35 C36 C37 176(2) . . . . ?
C35 C36 C37 C38 171(3) . . . . ?
C36 C37 C38 C39 -173(3) . . . . ?
C37 C38 C39 C40 -176(3) . . . . ?
C38 C39 C40 C41 -177(2) . . . . ?
C42 O3 C31 C30 -173(2) . . . . ?
C42 O3 C31 C32 14(3) . . . . ?
C42 C43 C44 C45 -92(2) . . . . ?
C43 C44 C45 C46 162(3) . . . . ?
C44 C45 C46 C47 -122(3) . . . . ?
C45 C46 C47 C48 -76(3) . . . . ?
C46 C47 C48 C49 145(4) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id 'Sample #10:OPN018'
_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 2.519
_oxdiff_exptl_absorpt_empirical_full_min 0.690
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.452(4)
2 0.548(4)

####################################################################### 
# 
# 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_m-4TICO
_database_code_depnum_ccdc_archive 'CCDC 1942948'
loop_
_audit_author_name
_audit_author_address
'Peter Horton'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2019-07-24 deposited with the CCDC.	2019-11-18 downloaded from the CCDC.
;

#2018ncs0778_2b

_audit_creation_date             2019-05-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C98 H96 N4 O6 S4, 2(C H Cl3)'
_chemical_formula_sum            'C100 H98 Cl6 N4 O6 S4'
_chemical_formula_weight         1792.76
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C98 H82 N4 O6 S4 CHCl3'
_chemical_oxdiff_usercomment     'Sample #17: OPN017 PE'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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                   8.6526(3)
_cell_length_b                   16.4878(8)
_cell_length_c                   18.0435(8)
_cell_angle_alpha                114.697(5)
_cell_angle_beta                 103.822(4)
_cell_angle_gamma                90.890(4)
_cell_volume                     2251.45(19)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    11203
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.9610
_cell_measurement_theta_min      2.7830
_shelx_estimated_absorpt_T_max   0.941
_shelx_estimated_absorpt_T_min   0.594
_exptl_absorpt_coefficient_mu    3.060
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       blade
_exptl_crystal_F_000             940
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of Pet. ether and chloroform'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38283
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.239
_diffrn_reflns_theta_min         2.800
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -89.00  89.00   0.50    2.50    --    0.00  20.00  30.00  356
  2  ω    -84.00  94.00   0.50    2.50    --    5.00  59.00 166.23  356
  3  ω   -179.00  -1.00   0.50   12.00    --  -90.00  56.00 -81.99  356
  4  ω   -179.00  -1.00   0.50   12.00    --  -90.00  59.00 169.00  356
  5  ω   -179.00  -1.00   0.50   12.00    --  -90.00  30.00   0.00  356
  6  ω   -179.00  -6.00   0.50   12.00    --  -90.00  56.00 112.89  346
  7  ω   -176.00-149.00   0.50   12.00    --  -90.00  59.00  68.94   54
  8  ω   -175.00-147.00   0.50   12.00    --  -90.00  53.00-134.95   56
  9  ω    -73.00 -30.00   0.50   12.00    --  -90.00  53.00-134.95   86
 10  ω   -177.00 -89.00   0.50   12.00    --  -90.00  59.00 -37.07  176
 11  ω    -61.00 -31.00   0.50   12.00    --  -90.00  59.00 -37.07   60
 12  ω   -173.00 -75.00   0.50   12.00    --  -90.00  10.00-150.00  196
 13  ω    -49.00 -22.00   0.50   12.00    --  -90.00  10.00-150.00   54
 14  ω   -146.00  -3.00   0.50   12.00    --  -90.00  59.00  68.94  286
 15  ω   -108.00 -83.00   0.50   12.00    --  -90.00  59.00-111.52   50
 16  ω   -178.00  -2.00   0.50   12.00    --  -90.00  59.00 130.42  352
 17  ω   -177.00 -63.00   0.50   12.00    --  -90.00  58.00  17.09  228
 18  ω    -48.00 -20.00   0.50   12.00    --  -90.00  58.00  17.09   56
 19  ω   -178.00-113.00   0.50   12.00    --  -90.00  59.00 -73.21  130
 20  ω    -86.00 -59.00   0.50   12.00    --  -90.00  59.00 -73.21   54
 21  ω    -51.00 -19.00   0.50   12.00    --  -90.00  59.00 -73.21   64
 22  ω   -178.00 -45.00   0.50   12.00    --  -90.00  59.00-152.53  266
 23  ω    -39.00 -12.00   0.50   12.00    --  -90.00   0.00-150.00   54
 24  ω   -160.00  -9.00   0.50   12.00    --  -90.00  59.00  37.38  302
 25  ω   -161.00 -84.00   0.50   12.00    --  -90.00  59.00-143.83  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter χ goniometer'
_diffrn_measurement_device_type  
'Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1772609000
_diffrn_orient_matrix_UB_12      0.0048791000
_diffrn_orient_matrix_UB_13      -0.0012295000
_diffrn_orient_matrix_UB_21      -0.0446113000
_diffrn_orient_matrix_UB_22      -0.0790866000
_diffrn_orient_matrix_UB_23      -0.0891951000
_diffrn_orient_matrix_UB_31      -0.0281484000
_diffrn_orient_matrix_UB_32      0.0669500000
_diffrn_orient_matrix_UB_33      -0.0396169000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6638
_reflns_number_total             8194
_reflns_odcompleteness_completeness 99.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         8194
_refine_ls_number_restraints     588
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0753
_refine_ls_restrained_S_all      1.044
_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)+(0.1197P)²+2.0232P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2089
_refine_ls_wR_factor_ref         0.2158
_refine_special_details          
'There is disorder in one alkyl chain and the solvent chloroform that have each been modelled over two positions. Due to this, various geometrical (SADI) and displacement (SIMU, RIGU) restraints have been used'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl51-C51 \\sim Cl63-C61
 with sigma of 0.02
 Cl52-C51 \\sim Cl61-C61
 with sigma of 0.02
 Cl53-C51 \\sim Cl62-C61
 with sigma of 0.02
 Cl51-Cl52 \\sim Cl63-Cl61
 with sigma of 0.04
 Cl51-Cl53 \\sim Cl63-Cl62
 with sigma of 0.04
 Cl52-Cl53 \\sim Cl61-Cl62
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl61 \\sim Cl62 \\sim Cl63 \\sim C61 \\sim Cl51 \\sim Cl52 \\sim Cl53 \\sim
C51: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H44C)=Sof(H44D)=Sof(C45B)=Sof(H45C)=Sof(H45D)=Sof(C46B)=Sof(H46C)=
 Sof(H46D)=Sof(C47B)=Sof(H47C)=Sof(H47D)=Sof(C48B)=Sof(H48C)=Sof(H48D)=
 Sof(C49B)=Sof(H49D)=Sof(H49E)=Sof(H49F)=1-FVAR(1)
 Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49A)=
 Sof(H49B)=Sof(H49C)=FVAR(1)
 Sof(Cl61)=Sof(Cl62)=Sof(Cl63)=Sof(C61)=Sof(H61)=1-FVAR(2)
 Sof(Cl51)=Sof(Cl52)=Sof(Cl53)=Sof(C51)=Sof(H51)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C61(H61), C51(H51)
6.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,
 H32B), C33(H33A,H33B), C34(H34A,H34B), C42(H42A,H42B), C43(H43A,H43B),
 C44(H44A,H44B), C44(H44C,H44D), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
  C48(H48A,H48B), C45B(H45C,H45D), C46B(H46C,H46D), C47B(H47C,H47D), C48B(H48C,
 H48D)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C15(H15), C23(H23), C25(H25),
 C26(H26), C27(H27), C37(H37), C39(H39), C40(H40), C41(H41)
6.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C49(H49A,H49B,H49C), C49B(H49D,H49E,H49F)
;
_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
S1 S 0.61382(10) 0.71062(6) 1.03913(6) 0.0428(2) Uani 1 1 d . U . . .
S2 S 0.48876(9) 0.95294(6) 1.09104(5) 0.0381(2) Uani 1 1 d . U . . .
O1 O 0.6186(4) 0.5945(2) 1.1036(2) 0.0633(8) Uani 1 1 d . U . . .
O2 O 0.1065(3) 0.77255(18) 0.68050(16) 0.0486(6) Uani 1 1 d . U . . .
O3 O 0.9299(3) 0.97238(18) 0.76826(16) 0.0470(6) Uani 1 1 d . U . . .
N1 N 0.9195(5) 0.4072(2) 0.8031(2) 0.0636(9) Uani 1 1 d . U . . .
N2 N 0.9713(4) 0.2118(2) 0.8999(2) 0.0598(9) Uani 1 1 d . U . . .
C1 C 0.6886(4) 0.5292(3) 1.0738(3) 0.0491(8) Uani 1 1 d . U . . .
C2 C 0.7481(4) 0.5034(2) 0.9984(2) 0.0448(8) Uani 1 1 d . U . . .
C3 C 0.8116(4) 0.4175(2) 0.9840(2) 0.0435(7) Uani 1 1 d . U . . .
C4 C 0.7997(4) 0.3961(2) 1.0549(2) 0.0443(8) Uani 1 1 d . U . . .
C5 C 0.7243(4) 0.4618(2) 1.1065(3) 0.0474(8) Uani 1 1 d . U . . .
C6 C 0.6956(5) 0.4603(3) 1.1786(3) 0.0528(9) Uani 1 1 d . U . . .
H6 H 0.644504 0.505917 1.213327 0.063 Uiso 1 1 calc R . . . .
C7 C 0.7435(5) 0.3905(3) 1.1979(3) 0.0550(9) Uani 1 1 d . U . . .
H7 H 0.723253 0.387053 1.246085 0.066 Uiso 1 1 calc R . . . .
C8 C 0.8209(5) 0.3255(3) 1.1480(3) 0.0562(10) Uani 1 1 d . U . . .
H8 H 0.855504 0.278976 1.163496 0.067 Uiso 1 1 calc R . . . .
C9 C 0.8493(4) 0.3264(3) 1.0759(3) 0.0499(8) Uani 1 1 d . U . . .
H9 H 0.901157 0.280764 1.041711 0.060 Uiso 1 1 calc R . . . .
C10 C 0.8738(4) 0.3649(3) 0.9188(2) 0.0479(8) Uani 1 1 d . U . . .
C11 C 0.8974(5) 0.3893(3) 0.8550(3) 0.0516(9) Uani 1 1 d . U . . .
C12 C 0.9275(5) 0.2802(3) 0.9103(3) 0.0511(9) Uani 1 1 d . U . . .
C13 C 0.7417(4) 0.5503(2) 0.9501(2) 0.0466(8) Uani 1 1 d . U . . .
H13 H 0.778972 0.520191 0.901200 0.056 Uiso 1 1 calc R . . . .
C14 C 0.6906(4) 0.6344(2) 0.9586(2) 0.0448(8) Uani 1 1 d . U . . .
C15 C 0.7001(4) 0.6682(2) 0.8998(2) 0.0441(8) Uani 1 1 d . U . . .
H15 H 0.737506 0.636504 0.851320 0.053 Uiso 1 1 calc R . . . .
C16 C 0.6498(4) 0.7520(2) 0.9195(2) 0.0399(7) Uani 1 1 d . U . . .
C17 C 0.6010(4) 0.7827(2) 0.9940(2) 0.0403(7) Uani 1 1 d . U . . .
C18 C 0.5506(4) 0.8699(2) 1.0106(2) 0.0382(7) Uani 1 1 d . U . . .
C19 C 0.5636(4) 0.8922(2) 0.9455(2) 0.0381(7) Uani 1 1 d . U . . .
C20 C 0.6300(4) 0.8195(2) 0.8805(2) 0.0381(7) Uani 1 1 d . U . . .
C21 C 0.5217(3) 0.9799(2) 0.9619(2) 0.0375(7) Uani 1 1 d . U . . .
C22 C 0.5158(4) 0.7741(2) 0.7913(2) 0.0394(7) Uani 1 1 d . U . . .
C23 C 0.3601(4) 0.7943(2) 0.7726(2) 0.0402(7) Uani 1 1 d . U . . .
H23 H 0.322631 0.839269 0.815572 0.048 Uiso 1 1 calc R . . . .
C24 C 0.2588(4) 0.7489(2) 0.6910(2) 0.0417(7) Uani 1 1 d . U . . .
C25 C 0.3123(4) 0.6839(3) 0.6265(2) 0.0462(8) Uani 1 1 d . U . . .
H25 H 0.243710 0.653994 0.570593 0.055 Uiso 1 1 calc R . . . .
C26 C 0.4680(4) 0.6639(3) 0.6458(2) 0.0476(8) Uani 1 1 d . U . . .
H26 H 0.505556 0.619237 0.602716 0.057 Uiso 1 1 calc R . . . .
C27 C 0.5694(4) 0.7082(2) 0.7269(2) 0.0444(8) Uani 1 1 d . U . . .
H27 H 0.675542 0.693755 0.738980 0.053 Uiso 1 1 calc R . . . .
C28 C 0.0015(4) 0.7333(3) 0.5968(2) 0.0487(8) Uani 1 1 d . U . . .
H28A H -0.003167 0.666888 0.571990 0.058 Uiso 1 1 calc R . . . .
H28B H 0.041555 0.755030 0.560488 0.058 Uiso 1 1 calc R . . . .
C29 C -0.1631(4) 0.7595(3) 0.6013(2) 0.0496(9) Uani 1 1 d . U . . .
H29A H -0.156150 0.825950 0.628194 0.060 Uiso 1 1 calc R . . . .
H29B H -0.202323 0.736729 0.637224 0.060 Uiso 1 1 calc R . . . .
C30 C -0.2826(4) 0.7218(3) 0.5136(2) 0.0490(8) Uani 1 1 d . U . . .
H30A H -0.272637 0.657343 0.482475 0.059 Uiso 1 1 calc R . . . .
H30B H -0.392853 0.725798 0.520419 0.059 Uiso 1 1 calc R . . . .
C31 C -0.2590(4) 0.7704(3) 0.4609(2) 0.0499(8) Uani 1 1 d . U . . .
H31A H -0.152768 0.761495 0.449378 0.060 Uiso 1 1 calc R . . . .
H31B H -0.258699 0.835788 0.494257 0.060 Uiso 1 1 calc R . . . .
C32 C -0.3876(5) 0.7384(3) 0.3772(2) 0.0507(9) Uani 1 1 d . U . . .
H32A H -0.494424 0.737015 0.387868 0.061 Uiso 1 1 calc R . . . .
H32B H -0.375127 0.676187 0.339790 0.061 Uiso 1 1 calc R . . . .
C33 C -0.3813(5) 0.7978(3) 0.3314(3) 0.0547(9) Uani 1 1 d . U . . .
H33A H -0.387942 0.860676 0.369997 0.066 Uiso 1 1 calc R . . . .
H33B H -0.276504 0.796694 0.318150 0.066 Uiso 1 1 calc R . . . .
C34 C -0.5143(5) 0.7691(3) 0.2501(3) 0.0550(9) Uani 1 1 d . U . . .
H34A H -0.498894 0.709787 0.208140 0.066 Uiso 1 1 calc R . . . .
H34B H -0.618838 0.762151 0.261562 0.066 Uiso 1 1 calc R . . . .
C35 C -0.5181(5) 0.8364(3) 0.2129(3) 0.0621(10) Uani 1 1 d . U . . .
H35A H -0.596413 0.811793 0.157127 0.093 Uiso 1 1 calc GR . . . .
H35B H -0.411479 0.848256 0.206931 0.093 Uiso 1 1 calc GR . . . .
H35C H -0.548890 0.892642 0.250536 0.093 Uiso 1 1 calc GR . . . .
C36 C 0.7909(4) 0.8606(2) 0.8804(2) 0.0383(7) Uani 1 1 d . U . . .
C37 C 0.7947(4) 0.8980(2) 0.8250(2) 0.0413(7) Uani 1 1 d . U . . .
H37 H 0.698531 0.895658 0.785076 0.050 Uiso 1 1 calc R . . . .
C38 C 0.9400(4) 0.9395(2) 0.8274(2) 0.0413(7) Uani 1 1 d . U . . .
C39 C 1.0795(4) 0.9444(2) 0.8862(2) 0.0420(7) Uani 1 1 d . U . . .
H39 H 1.177915 0.973058 0.888622 0.050 Uiso 1 1 calc R . . . .
C40 C 1.0745(4) 0.9070(2) 0.9421(2) 0.0418(7) Uani 1 1 d . U . . .
H40 H 1.170633 0.909987 0.982378 0.050 Uiso 1 1 calc R . . . .
C41 C 0.9327(4) 0.8655(2) 0.9400(2) 0.0402(7) Uani 1 1 d . U . . .
H41 H 0.931294 0.840481 0.978663 0.048 Uiso 1 1 calc R . . . .
C42 C 1.0784(4) 1.0045(3) 0.7603(3) 0.0495(9) Uani 1 1 d . U . . .
H42A H 1.155834 0.960519 0.758278 0.059 Uiso 1 1 calc R . . . .
H42B H 1.126216 1.062588 0.809606 0.059 Uiso 1 1 calc R . . . .
C43 C 1.0418(5) 1.0163(3) 0.6799(3) 0.0599(10) Uani 1 1 d . U . . .
H43A H 1.144334 1.028471 0.668777 0.072 Uiso 1 1 calc R . . . .
H43B H 0.983773 0.959166 0.632288 0.072 Uiso 1 1 calc R . . . .
C44 C 0.9436(6) 1.0906(4) 0.6817(4) 0.0793(15) Uani 1 1 d . U . . .
H44A H 1.008047 1.149773 0.720701 0.095 Uiso 0.709(11) 1 calc R . P A 1
H44B H 0.848379 1.085059 0.701421 0.095 Uiso 0.709(11) 1 calc R . P A 1
H44C H 0.988762 1.138921 0.739629 0.095 Uiso 0.291(11) 1 calc R . P A 2
H44D H 0.836973 1.067492 0.681228 0.095 Uiso 0.291(11) 1 calc R . P A 2
C45 C 0.8900(7) 1.0823(5) 0.5888(4) 0.0497(15) Uani 0.709(11) 1 d . U P A 1
H45A H 0.985525 1.084086 0.568038 0.060 Uiso 0.709(11) 1 calc R . P A 1
H45B H 0.821100 1.024353 0.550575 0.060 Uiso 0.709(11) 1 calc R . P A 1
C46 C 0.7972(8) 1.1606(4) 0.5891(4) 0.0567(18) Uani 0.709(11) 1 d . U P A 1
H46A H 0.705694 1.159770 0.613006 0.068 Uiso 0.709(11) 1 calc R . P A 1
H46B H 0.868479 1.217916 0.626845 0.068 Uiso 0.709(11) 1 calc R . P A 1
C47 C 0.7339(9) 1.1582(6) 0.5023(4) 0.0522(16) Uani 0.709(11) 1 d . U P A 1
H47A H 0.704202 1.218200 0.509252 0.063 Uiso 0.709(11) 1 calc R . P A 1
H47B H 0.820923 1.146162 0.473546 0.063 Uiso 0.709(11) 1 calc R . P A 1
C48 C 0.5898(12) 1.0881(7) 0.4462(7) 0.053(2) Uani 0.709(11) 1 d . U P A 1
H48A H 0.508041 1.096089 0.477922 0.064 Uiso 0.709(11) 1 calc R . P A 1
H48B H 0.623350 1.027800 0.434546 0.064 Uiso 0.709(11) 1 calc R . P A 1
C49 C 0.512(2) 1.0898(11) 0.3624(10) 0.056(3) Uani 0.709(11) 1 d . U P A 1
H49A H 0.584991 1.071323 0.325915 0.084 Uiso 0.709(11) 1 calc GR . P A 1
H49B H 0.489085 1.150988 0.372277 0.084 Uiso 0.709(11) 1 calc GR . P A 1
H49C H 0.411692 1.048334 0.334606 0.084 Uiso 0.709(11) 1 calc GR . P A 1
C45B C 0.9034(18) 1.1418(15) 0.6275(12) 0.058(4) Uani 0.291(11) 1 d . U P A 2
H45C H 0.886215 1.204326 0.661412 0.070 Uiso 0.291(11) 1 calc R . P A 2
H45D H 0.988840 1.142961 0.599797 0.070 Uiso 0.291(11) 1 calc R . P A 2
C46B C 0.7531(16) 1.0877(11) 0.5648(9) 0.052(4) Uani 0.291(11) 1 d . U P A 2
H46C H 0.666047 1.097476 0.593384 0.063 Uiso 0.291(11) 1 calc R . P A 2
H46D H 0.767132 1.023127 0.544041 0.063 Uiso 0.291(11) 1 calc R . P A 2
C47B C 0.701(2) 1.1097(15) 0.4878(11) 0.050(4) Uani 0.291(11) 1 d . U P A 2
H47C H 0.693622 1.175029 0.508809 0.060 Uiso 0.291(11) 1 calc R . P A 2
H47D H 0.785102 1.096301 0.457215 0.060 Uiso 0.291(11) 1 calc R . P A 2
C48B C 0.544(3) 1.0591(19) 0.4266(17) 0.057(6) Uani 0.291(11) 1 d . U P A 2
H48C H 0.454861 1.077402 0.453470 0.068 Uiso 0.291(11) 1 calc R . P A 2
H48D H 0.544754 0.993515 0.407628 0.068 Uiso 0.291(11) 1 calc R . P A 2
C49B C 0.522(7) 1.084(4) 0.348(3) 0.092(14) Uani 0.291(11) 1 d . U P A 2
H49D H 0.442156 1.038233 0.299135 0.138 Uiso 0.291(11) 1 calc GR . P A 2
H49E H 0.624613 1.084869 0.334831 0.138 Uiso 0.291(11) 1 calc GR . P A 2
H49F H 0.484921 1.142936 0.363160 0.138 Uiso 0.291(11) 1 calc GR . P A 2
Cl61 Cl 1.047(2) 0.4703(12) 0.5982(8) 0.168(8) Uani 0.158(3) 1 d D U P B 2
Cl62 Cl 0.8278(17) 0.3535(7) 0.5982(5) 0.116(5) Uani 0.158(3) 1 d D U P B 2
Cl63 Cl 0.809(3) 0.5430(16) 0.6776(12) 0.226(10) Uani 0.158(3) 1 d D U P B 2
C61 C 0.928(3) 0.4598(12) 0.6589(19) 0.085(12) Uani 0.158(3) 1 d D U P B 2
H61 H 0.996384 0.463885 0.713729 0.102 Uiso 0.158(3) 1 calc R . P B 2
Cl51 Cl 0.8900(2) 0.56882(14) 0.64131(16) 0.0974(7) Uani 0.842(3) 1 d D U P B 1
Cl52 Cl 0.9941(2) 0.39658(13) 0.61507(11) 0.0978(7) Uani 0.842(3) 1 d D U P B 1
Cl53 Cl 0.6774(2) 0.43229(16) 0.63450(18) 0.1218(9) Uani 0.842(3) 1 d D U P B 1
C51 C 0.8775(8) 0.4770(5) 0.6630(4) 0.0677(17) Uani 0.842(3) 1 d D U P B 1
H51 H 0.919605 0.498833 0.725657 0.081 Uiso 0.842(3) 1 calc R . P B 1


_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 C14 1.759(4) . ?
S1 C17 1.691(3) . ?
S2 C18 1.732(4) . ?
S2 C21 1.730(3) 2_677 ?
O1 C1 1.228(4) . ?
O2 C24 1.372(4) . ?
O2 C28 1.426(4) . ?
O3 C38 1.372(4) . ?
O3 C42 1.442(4) . ?
N1 C11 1.147(5) . ?
N2 C12 1.149(5) . ?
C1 C2 1.468(5) . ?
C1 C5 1.467(5) . ?
C2 C3 1.469(5) . ?
C2 C13 1.379(5) . ?
C3 C4 1.486(5) . ?
C3 C10 1.374(5) . ?
C4 C5 1.392(5) . ?
C4 C9 1.398(5) . ?
C5 C6 1.390(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.379(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.383(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.386(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.424(6) . ?
C10 C12 1.438(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.421(5) . ?
C14 C15 1.405(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.381(5) . ?
C16 C17 1.395(5) . ?
C16 C20 1.539(4) . ?
C17 C18 1.438(5) . ?
C18 C19 1.398(5) . ?
C19 C20 1.521(5) . ?
C19 C21 1.421(5) . ?
C20 C22 1.529(5) . ?
C20 C36 1.539(4) . ?
C21 C21 1.401(7) 2_677 ?
C22 C23 1.390(4) . ?
C22 C27 1.401(5) . ?
C23 H23 0.9500 . ?
C23 C24 1.392(5) . ?
C24 C25 1.395(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.390(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.385(5) . ?
C27 H27 0.9500 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.505(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.529(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.520(5) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.521(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.530(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.516(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.515(6) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.383(5) . ?
C36 C41 1.400(4) . ?
C37 H37 0.9500 . ?
C37 C38 1.404(5) . ?
C38 C39 1.379(5) . ?
C39 H39 0.9500 . ?
C39 C40 1.392(5) . ?
C40 H40 0.9500 . ?
C40 C41 1.380(5) . ?
C41 H41 0.9500 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.504(5) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.495(7) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 H44C 0.9900 . ?
C44 H44D 0.9900 . ?
C44 C45 1.574(8) . ?
C44 C45B 1.526(15) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.529(9) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.515(8) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.513(10) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.514(17) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C45B H45C 0.9900 . ?
C45B H45D 0.9900 . ?
C45B C46B 1.48(2) . ?
C46B H46C 0.9900 . ?
C46B H46D 0.9900 . ?
C46B C47B 1.55(2) . ?
C47B H47C 0.9900 . ?
C47B H47D 0.9900 . ?
C47B C48B 1.50(2) . ?
C48B H48C 0.9900 . ?
C48B H48D 0.9900 . ?
C48B C49B 1.59(5) . ?
C49B H49D 0.9800 . ?
C49B H49E 0.9800 . ?
C49B H49F 0.9800 . ?
Cl61 C61 1.73(2) . ?
Cl62 C61 1.71(2) . ?
Cl63 C61 1.694(19) . ?
C61 H61 1.0000 . ?
Cl51 C51 1.722(7) . ?
Cl52 C51 1.740(7) . ?
Cl53 C51 1.739(7) . ?
C51 H51 1.0000 . ?

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
C17 S1 C14 90.22(17) . . ?
C21 S2 C18 89.53(16) 2_677 . ?
C24 O2 C28 117.4(3) . . ?
C38 O3 C42 117.4(3) . . ?
O1 C1 C2 126.5(3) . . ?
O1 C1 C5 125.7(4) . . ?
C5 C1 C2 107.8(3) . . ?
C1 C2 C3 106.5(3) . . ?
C13 C2 C1 126.1(3) . . ?
C13 C2 C3 127.3(4) . . ?
C2 C3 C4 107.5(3) . . ?
C10 C3 C2 128.1(3) . . ?
C10 C3 C4 124.4(3) . . ?
C5 C4 C3 108.5(3) . . ?
C5 C4 C9 119.3(4) . . ?
C9 C4 C3 132.2(4) . . ?
C4 C5 C1 109.5(3) . . ?
C6 C5 C1 128.3(4) . . ?
C6 C5 C4 122.2(3) . . ?
C5 C6 H6 121.1 . . ?
C7 C6 C5 117.9(4) . . ?
C7 C6 H6 121.1 . . ?
C6 C7 H7 119.7 . . ?
C6 C7 C8 120.6(4) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 H8 119.1 . . ?
C7 C8 C9 121.8(4) . . ?
C9 C8 H8 119.1 . . ?
C4 C9 H9 120.9 . . ?
C8 C9 C4 118.3(4) . . ?
C8 C9 H9 120.9 . . ?
C3 C10 C11 124.2(3) . . ?
C3 C10 C12 122.8(4) . . ?
C11 C10 C12 113.0(3) . . ?
N1 C11 C10 178.0(4) . . ?
N2 C12 C10 176.9(4) . . ?
C2 C13 H13 113.5 . . ?
C2 C13 C14 133.0(4) . . ?
C14 C13 H13 113.5 . . ?
C13 C14 S1 128.0(3) . . ?
C15 C14 S1 110.6(3) . . ?
C15 C14 C13 121.4(3) . . ?
C14 C15 H15 123.3 . . ?
C16 C15 C14 113.4(3) . . ?
C16 C15 H15 123.3 . . ?
C15 C16 C17 111.2(3) . . ?
C15 C16 C20 137.0(3) . . ?
C17 C16 C20 111.7(3) . . ?
C16 C17 S1 114.5(3) . . ?
C16 C17 C18 108.3(3) . . ?
C18 C17 S1 137.2(3) . . ?
C17 C18 S2 136.5(3) . . ?
C19 C18 S2 114.4(3) . . ?
C19 C18 C17 109.0(3) . . ?
C18 C19 C20 111.7(3) . . ?
C18 C19 C21 110.6(3) . . ?
C21 C19 C20 137.5(3) . . ?
C16 C20 C36 113.1(2) . . ?
C19 C20 C16 99.3(3) . . ?
C19 C20 C22 114.8(3) . . ?
C19 C20 C36 108.2(3) . . ?
C22 C20 C16 109.4(3) . . ?
C22 C20 C36 111.6(3) . . ?
C19 C21 S2 134.5(3) . 2_677 ?
C21 C21 S2 113.4(3) 2_677 2_677 ?
C21 C21 C19 112.0(4) 2_677 . ?
C23 C22 C20 122.3(3) . . ?
C23 C22 C27 119.1(3) . . ?
C27 C22 C20 118.5(3) . . ?
C22 C23 H23 119.9 . . ?
C22 C23 C24 120.1(3) . . ?
C24 C23 H23 119.9 . . ?
O2 C24 C23 115.0(3) . . ?
O2 C24 C25 124.1(3) . . ?
C23 C24 C25 120.9(3) . . ?
C24 C25 H25 120.7 . . ?
C26 C25 C24 118.6(3) . . ?
C26 C25 H25 120.7 . . ?
C25 C26 H26 119.5 . . ?
C27 C26 C25 121.0(3) . . ?
C27 C26 H26 119.5 . . ?
C22 C27 H27 119.9 . . ?
C26 C27 C22 120.2(3) . . ?
C26 C27 H27 119.9 . . ?
O2 C28 H28A 110.0 . . ?
O2 C28 H28B 110.0 . . ?
O2 C28 C29 108.5(3) . . ?
H28A C28 H28B 108.4 . . ?
C29 C28 H28A 110.0 . . ?
C29 C28 H28B 110.0 . . ?
C28 C29 H29A 109.2 . . ?
C28 C29 H29B 109.2 . . ?
C28 C29 C30 111.9(3) . . ?
H29A C29 H29B 107.9 . . ?
C30 C29 H29A 109.2 . . ?
C30 C29 H29B 109.2 . . ?
C29 C30 H30A 108.8 . . ?
C29 C30 H30B 108.8 . . ?
H30A C30 H30B 107.7 . . ?
C31 C30 C29 113.7(3) . . ?
C31 C30 H30A 108.8 . . ?
C31 C30 H30B 108.8 . . ?
C30 C31 H31A 108.9 . . ?
C30 C31 H31B 108.9 . . ?
C30 C31 C32 113.4(3) . . ?
H31A C31 H31B 107.7 . . ?
C32 C31 H31A 108.9 . . ?
C32 C31 H31B 108.9 . . ?
C31 C32 H32A 108.9 . . ?
C31 C32 H32B 108.9 . . ?
C31 C32 C33 113.4(3) . . ?
H32A C32 H32B 107.7 . . ?
C33 C32 H32A 108.9 . . ?
C33 C32 H32B 108.9 . . ?
C32 C33 H33A 108.8 . . ?
C32 C33 H33B 108.8 . . ?
H33A C33 H33B 107.7 . . ?
C34 C33 C32 113.7(3) . . ?
C34 C33 H33A 108.8 . . ?
C34 C33 H33B 108.8 . . ?
C33 C34 H34A 109.2 . . ?
C33 C34 H34B 109.2 . . ?
H34A C34 H34B 107.9 . . ?
C35 C34 C33 112.2(4) . . ?
C35 C34 H34A 109.2 . . ?
C35 C34 H34B 109.2 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 C20 120.1(3) . . ?
C37 C36 C41 119.5(3) . . ?
C41 C36 C20 120.3(3) . . ?
C36 C37 H37 119.8 . . ?
C36 C37 C38 120.4(3) . . ?
C38 C37 H37 119.8 . . ?
O3 C38 C37 115.2(3) . . ?
O3 C38 C39 124.7(3) . . ?
C39 C38 C37 120.0(3) . . ?
C38 C39 H39 120.4 . . ?
C38 C39 C40 119.2(3) . . ?
C40 C39 H39 120.4 . . ?
C39 C40 H40 119.4 . . ?
C41 C40 C39 121.3(3) . . ?
C41 C40 H40 119.4 . . ?
C36 C41 H41 120.2 . . ?
C40 C41 C36 119.5(3) . . ?
C40 C41 H41 120.2 . . ?
O3 C42 H42A 110.1 . . ?
O3 C42 H42B 110.1 . . ?
O3 C42 C43 108.0(3) . . ?
H42A C42 H42B 108.4 . . ?
C43 C42 H42A 110.1 . . ?
C43 C42 H42B 110.1 . . ?
C42 C43 H43A 108.7 . . ?
C42 C43 H43B 108.7 . . ?
H43A C43 H43B 107.6 . . ?
C44 C43 C42 114.1(4) . . ?
C44 C43 H43A 108.7 . . ?
C44 C43 H43B 108.7 . . ?
C43 C44 H44A 110.2 . . ?
C43 C44 H44B 110.2 . . ?
C43 C44 H44C 103.5 . . ?
C43 C44 H44D 103.5 . . ?
C43 C44 C45 107.4(5) . . ?
C43 C44 C45B 134.9(8) . . ?
H44A C44 H44B 108.5 . . ?
H44C C44 H44D 105.3 . . ?
C45 C44 H44A 110.2 . . ?
C45 C44 H44B 110.2 . . ?
C45B C44 H44C 103.5 . . ?
C45B C44 H44D 103.5 . . ?
C44 C45 H45A 109.9 . . ?
C44 C45 H45B 109.9 . . ?
H45A C45 H45B 108.3 . . ?
C46 C45 C44 108.8(5) . . ?
C46 C45 H45A 109.9 . . ?
C46 C45 H45B 109.9 . . ?
C45 C46 H46A 108.8 . . ?
C45 C46 H46B 108.8 . . ?
H46A C46 H46B 107.7 . . ?
C47 C46 C45 113.8(5) . . ?
C47 C46 H46A 108.8 . . ?
C47 C46 H46B 108.8 . . ?
C46 C47 H47A 108.8 . . ?
C46 C47 H47B 108.8 . . ?
H47A C47 H47B 107.6 . . ?
C48 C47 C46 114.0(7) . . ?
C48 C47 H47A 108.8 . . ?
C48 C47 H47B 108.8 . . ?
C47 C48 H48A 108.4 . . ?
C47 C48 H48B 108.4 . . ?
C47 C48 C49 115.7(9) . . ?
H48A C48 H48B 107.4 . . ?
C49 C48 H48A 108.4 . . ?
C49 C48 H48B 108.4 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C44 C45B H45C 111.4 . . ?
C44 C45B H45D 111.4 . . ?
H45C C45B H45D 109.3 . . ?
C46B C45B C44 101.6(12) . . ?
C46B C45B H45C 111.4 . . ?
C46B C45B H45D 111.4 . . ?
C45B C46B H46C 108.7 . . ?
C45B C46B H46D 108.7 . . ?
C45B C46B C47B 114.2(12) . . ?
H46C C46B H46D 107.6 . . ?
C47B C46B H46C 108.7 . . ?
C47B C46B H46D 108.7 . . ?
C46B C47B H47C 108.6 . . ?
C46B C47B H47D 108.6 . . ?
H47C C47B H47D 107.6 . . ?
C48B C47B C46B 114.5(17) . . ?
C48B C47B H47C 108.6 . . ?
C48B C47B H47D 108.6 . . ?
C47B C48B H48C 110.5 . . ?
C47B C48B H48D 110.5 . . ?
C47B C48B C49B 106(3) . . ?
H48C C48B H48D 108.6 . . ?
C49B C48B H48C 110.5 . . ?
C49B C48B H48D 110.5 . . ?
C48B C49B H49D 109.5 . . ?
C48B C49B H49E 109.5 . . ?
C48B C49B H49F 109.5 . . ?
H49D C49B H49E 109.5 . . ?
H49D C49B H49F 109.5 . . ?
H49E C49B H49F 109.5 . . ?
Cl61 C61 H61 110.0 . . ?
Cl62 C61 Cl61 102.6(14) . . ?
Cl62 C61 H61 110.0 . . ?
Cl63 C61 Cl61 109.1(17) . . ?
Cl63 C61 Cl62 115.0(19) . . ?
Cl63 C61 H61 110.0 . . ?
Cl51 C51 Cl52 112.3(4) . . ?
Cl51 C51 Cl53 109.6(4) . . ?
Cl51 C51 H51 107.6 . . ?
Cl52 C51 H51 107.6 . . ?
Cl53 C51 Cl52 112.0(4) . . ?
Cl53 C51 H51 107.6 . . ?

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 C14 C15 C16 0.7(4) . . . . ?
S1 C17 C18 S2 6.0(6) . . . . ?
S1 C17 C18 C19 -177.5(3) . . . . ?
S2 C18 C19 C20 175.8(2) . . . . ?
S2 C18 C19 C21 0.0(4) . . . . ?
O1 C1 C2 C3 -175.8(4) . . . . ?
O1 C1 C2 C13 3.0(7) . . . . ?
O1 C1 C5 C4 177.9(4) . . . . ?
O1 C1 C5 C6 -3.9(7) . . . . ?
O2 C24 C25 C26 -178.0(3) . . . . ?
O2 C28 C29 C30 178.6(3) . . . . ?
O3 C38 C39 C40 -178.8(3) . . . . ?
O3 C42 C43 C44 67.7(5) . . . . ?
C1 C2 C3 C4 -4.0(4) . . . . ?
C1 C2 C3 C10 176.9(4) . . . . ?
C1 C2 C13 C14 4.6(7) . . . . ?
C1 C5 C6 C7 -178.4(4) . . . . ?
C2 C1 C5 C4 -0.8(4) . . . . ?
C2 C1 C5 C6 177.4(4) . . . . ?
C2 C3 C4 C5 3.5(4) . . . . ?
C2 C3 C4 C9 -176.1(4) . . . . ?
C2 C3 C10 C11 4.5(6) . . . . ?
C2 C3 C10 C12 -177.9(4) . . . . ?
C2 C13 C14 S1 -0.1(6) . . . . ?
C2 C13 C14 C15 178.6(4) . . . . ?
C3 C2 C13 C14 -176.9(4) . . . . ?
C3 C4 C5 C1 -1.7(4) . . . . ?
C3 C4 C5 C6 180.0(3) . . . . ?
C3 C4 C9 C8 179.7(4) . . . . ?
C4 C3 C10 C11 -174.5(3) . . . . ?
C4 C3 C10 C12 3.2(6) . . . . ?
C4 C5 C6 C7 -0.4(6) . . . . ?
C5 C1 C2 C3 3.0(4) . . . . ?
C5 C1 C2 C13 -178.3(4) . . . . ?
C5 C4 C9 C8 0.1(5) . . . . ?
C5 C6 C7 C8 1.4(6) . . . . ?
C6 C7 C8 C9 -1.7(7) . . . . ?
C7 C8 C9 C4 1.0(6) . . . . ?
C9 C4 C5 C1 178.0(3) . . . . ?
C9 C4 C5 C6 -0.3(6) . . . . ?
C10 C3 C4 C5 -177.3(3) . . . . ?
C10 C3 C4 C9 3.0(6) . . . . ?
C13 C2 C3 C4 177.3(3) . . . . ?
C13 C2 C3 C10 -1.8(6) . . . . ?
C13 C14 C15 C16 -178.1(3) . . . . ?
C14 S1 C17 C16 0.9(3) . . . . ?
C14 S1 C17 C18 -179.9(4) . . . . ?
C14 C15 C16 C17 -0.1(4) . . . . ?
C14 C15 C16 C20 -178.5(4) . . . . ?
C15 C16 C17 S1 -0.6(4) . . . . ?
C15 C16 C17 C18 179.9(3) . . . . ?
C15 C16 C20 C19 178.7(4) . . . . ?
C15 C16 C20 C22 58.1(5) . . . . ?
C15 C16 C20 C36 -66.9(5) . . . . ?
C16 C17 C18 S2 -174.8(3) . . . . ?
C16 C17 C18 C19 1.7(4) . . . . ?
C16 C20 C22 C23 107.0(3) . . . . ?
C16 C20 C22 C27 -71.3(4) . . . . ?
C16 C20 C36 C37 158.9(3) . . . . ?
C16 C20 C36 C41 -25.2(4) . . . . ?
C17 S1 C14 C13 177.9(3) . . . . ?
C17 S1 C14 C15 -0.9(3) . . . . ?
C17 C16 C20 C19 0.3(3) . . . . ?
C17 C16 C20 C22 -120.3(3) . . . . ?
C17 C16 C20 C36 114.7(3) . . . . ?
C17 C18 C19 C20 -1.6(4) . . . . ?
C17 C18 C19 C21 -177.3(3) . . . . ?
C18 C19 C20 C16 0.8(3) . . . . ?
C18 C19 C20 C22 117.3(3) . . . . ?
C18 C19 C20 C36 -117.4(3) . . . . ?
C18 C19 C21 S2 -179.8(3) . . . 2_677 ?
C18 C19 C21 C21 -0.2(5) . . . 2_677 ?
C19 C20 C22 C23 -3.6(4) . . . . ?
C19 C20 C22 C27 178.2(3) . . . . ?
C19 C20 C36 C37 -92.2(4) . . . . ?
C19 C20 C36 C41 83.7(4) . . . . ?
C20 C16 C17 S1 178.2(2) . . . . ?
C20 C16 C17 C18 -1.2(4) . . . . ?
C20 C19 C21 S2 6.1(6) . . . 2_677 ?
C20 C19 C21 C21 -174.4(4) . . . 2_677 ?
C20 C22 C23 C24 -177.7(3) . . . . ?
C20 C22 C27 C26 178.4(3) . . . . ?
C20 C36 C37 C38 176.9(3) . . . . ?
C20 C36 C41 C40 -176.5(3) . . . . ?
C21 S2 C18 C17 176.5(4) 2_677 . . . ?
C21 S2 C18 C19 0.2(3) 2_677 . . . ?
C21 C19 C20 C16 174.9(4) . . . . ?
C21 C19 C20 C22 -68.6(5) . . . . ?
C21 C19 C20 C36 56.7(5) . . . . ?
C22 C20 C36 C37 35.0(4) . . . . ?
C22 C20 C36 C41 -149.1(3) . . . . ?
C22 C23 C24 O2 178.2(3) . . . . ?
C22 C23 C24 C25 -1.3(5) . . . . ?
C23 C22 C27 C26 0.1(5) . . . . ?
C23 C24 C25 C26 1.4(5) . . . . ?
C24 O2 C28 C29 173.4(3) . . . . ?
C24 C25 C26 C27 -0.9(5) . . . . ?
C25 C26 C27 C22 0.1(5) . . . . ?
C27 C22 C23 C24 0.5(5) . . . . ?
C28 O2 C24 C23 175.3(3) . . . . ?
C28 O2 C24 C25 -5.3(5) . . . . ?
C28 C29 C30 C31 -74.1(4) . . . . ?
C29 C30 C31 C32 -174.6(3) . . . . ?
C30 C31 C32 C33 169.9(3) . . . . ?
C31 C32 C33 C34 -177.1(3) . . . . ?
C32 C33 C34 C35 172.1(4) . . . . ?
C36 C20 C22 C23 -127.1(3) . . . . ?
C36 C20 C22 C27 54.6(4) . . . . ?
C36 C37 C38 O3 178.5(3) . . . . ?
C36 C37 C38 C39 -1.1(5) . . . . ?
C37 C36 C41 C40 -0.5(5) . . . . ?
C37 C38 C39 C40 0.7(5) . . . . ?
C38 O3 C42 C43 166.9(3) . . . . ?
C38 C39 C40 C41 -0.4(5) . . . . ?
C39 C40 C41 C36 0.2(5) . . . . ?
C41 C36 C37 C38 0.9(5) . . . . ?
C42 O3 C38 C37 -171.7(3) . . . . ?
C42 O3 C38 C39 7.8(5) . . . . ?
C42 C43 C44 C45 -169.8(4) . . . . ?
C42 C43 C44 C45B 165.3(11) . . . . ?
C43 C44 C45 C46 -176.8(5) . . . . ?
C43 C44 C45B C46B 91.7(12) . . . . ?
C44 C45 C46 C47 -178.0(5) . . . . ?
C44 C45B C46B C47B -166.8(12) . . . . ?
C45 C46 C47 C48 74.7(8) . . . . ?
C46 C47 C48 C49 173.8(11) . . . . ?
C45B C46B C47B C48B -177(2) . . . . ?
C46B C47B C48B C49B -174(3) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id 'Sample #17:OPN017'
_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 4.624
_oxdiff_exptl_absorpt_empirical_full_min 0.621
####################################################################### 
# 
# 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_IEICO
_database_code_depnum_ccdc_archive 'CCDC 1942950'
loop_
_audit_author_name
_audit_author_address
'Peter Horton'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2019-07-24 deposited with the CCDC.	2019-11-18 downloaded from the CCDC.
;

#2018ncs0889_1b

_audit_creation_date             2019-05-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C57 H59 N2 O2 S2, C H Cl3'
_chemical_formula_sum            'C58 H60 Cl3 N2 O2 S2'
_chemical_formula_weight         987.55
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOS
_chemical_oxdiff_usercomment     'Sample #19:IEICO PE'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.1745(9)
_cell_length_b                   35.242(2)
_cell_length_c                   14.1841(9)
_cell_angle_alpha                90
_cell_angle_beta                 100.409(4)
_cell_angle_gamma                90
_cell_volume                     10410.5(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3649
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      48.6210
_cell_measurement_theta_min      3.6810
_shelx_estimated_absorpt_T_max   0.961
_shelx_estimated_absorpt_T_min   0.445
_exptl_absorpt_coefficient_mu    2.679
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             4168
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of Pet. ether and chloroform'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.015
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1045
_diffrn_reflns_av_unetI/netI     0.0841
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28791
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.235
_diffrn_reflns_theta_min         3.699
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     14.00  89.00   0.50    6.00    --    0.00  30.00 -90.00  150
  2  ω    -39.00   6.00   0.50    6.00    --    0.00  30.00 -90.00   90
  3  ω    -88.00 -61.00   0.50    6.00    --    0.00  30.00 -90.00   54
  4  ω    -35.00  -2.00   0.50   35.00    --  -90.00  57.00-119.31   66
  5  ω   -171.00-137.00   0.50   35.00    --  -90.00  59.00 -20.83   68
  6  ω   -172.00 -51.00   0.50   35.00    --  -90.00  59.00-125.08  242
  7  ω    -97.00 -13.00   0.50   35.00    --  -90.00  59.00-140.79  168
  8  ω   -168.00-102.00   0.50   35.00    --  -90.00  59.00-140.79  132
  9  ω   -175.00 -19.00   0.50   35.00    --  -90.00  56.00-174.03  312
 10  ω   -159.00 -31.00   0.50   35.00    --  -90.00  58.00 -85.61  256
 11  ω    -94.00 -47.00   0.50   35.00    --  -90.00  59.00 -36.47   94
 12  ω    -60.00 -34.00   0.50   35.00    --  -90.00  59.00 -20.83   52
 13  ω   -111.00 -85.00   0.50   35.00    --  -90.00  57.00-119.31   52
 14  ω   -162.00-136.00   0.50   35.00    --  -90.00  57.00-119.31   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter χ goniometer'
_diffrn_measurement_device_type  
'Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0053316000
_diffrn_orient_matrix_UB_12      0.0424430000
_diffrn_orient_matrix_UB_13      0.0231841000
_diffrn_orient_matrix_UB_21      -0.0121872000
_diffrn_orient_matrix_UB_22      -0.0102229000
_diffrn_orient_matrix_UB_23      0.1008758000
_diffrn_orient_matrix_UB_31      0.0727331000
_diffrn_orient_matrix_UB_32      0.0012941000
_diffrn_orient_matrix_UB_33      0.0388759000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4070
_reflns_number_total             9244
_reflns_odcompleteness_completeness 96.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.470
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         9244
_refine_ls_number_restraints     1314
_refine_ls_R_factor_all          0.2955
_refine_ls_R_factor_gt           0.1903
_refine_ls_restrained_S_all      1.391
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4321
_refine_ls_wR_factor_ref         0.4994
_refine_special_details          
'The crystal was not of great quality, resulting in a poor structure. However, the overall connectivity especially of the core can be idenitfied. There is significant disorder observed especially in the longer alkyl chains that have each been modelled over two positions. Due to all the above, various geometrical (SADI) and displacement (SIMU, RIGU) restraints have been used'
_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. Restrained distances
 C61-Cl63 \\sim C61-Cl61 \\sim C61-Cl62
 with sigma of 0.03
 Cl63-Cl61 \\sim Cl61-Cl62 \\sim Cl62-Cl63
 with sigma of 0.06
 C40-C41 \\sim C40B-C41B
 with sigma of 0.02
 C40-C37 \\sim C40B-C37
 with sigma of 0.02
 C41-C42 \\sim C41B-C42B
 with sigma of 0.02
 C42-C43 \\sim C42B-C43B
 with sigma of 0.02
 C43-C44 \\sim C43B-C44B
 with sigma of 0.02
 C40-C42 \\sim C40B-C42B
 with sigma of 0.04
 C41-C43 \\sim C41B-C43B
 with sigma of 0.04
 C41-C37 \\sim C41B-C37
 with sigma of 0.04
 C42-C44 \\sim C42B-C44B
 with sigma of 0.04
 C49-C52 \\sim C49-C52B
 with sigma of 0.02
 C56-C55 \\sim C56B-C55B
 with sigma of 0.02
 C55-C54 \\sim C55B-C54B
 with sigma of 0.02
 C54-C53 \\sim C54B-C53B
 with sigma of 0.02
 C53-C52 \\sim C53B-C52B
 with sigma of 0.02
 C49-C53 \\sim C49-C53B
 with sigma of 0.04
 C56-C54 \\sim C56B-C54B
 with sigma of 0.04
 C55-C53 \\sim C55B-C53B
 with sigma of 0.04
 C54-C52 \\sim C54B-C52B
 with sigma of 0.04
 C40-C41 \\sim C41-C42 \\sim C42-C43 \\sim C43-C44 \\sim C44-C45
 with sigma of 0.03
 C40-C42 \\sim C42-C44 \\sim C41-C43 \\sim C43-C45
 with sigma of 0.06
 C57-C56 \\sim C56-C55 \\sim C55-C54 \\sim C54-C53 \\sim C53-C52
 with sigma of 0.03
 C57-C55 \\sim C55-C53 \\sim C56-C54 \\sim C54-C52
 with sigma of 0.06
 C44-C45 \\sim C44B-C45B
 with sigma of 0.02
 C43-C45 \\sim C43B-C45B
 with sigma of 0.04
 C57-C56 \\sim C57B-C56B
 with sigma of 0.02
 C57-C55 \\sim C57B-C55B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(C40B)=Sof(H40C)=Sof(H40D)=Sof(C41B)=Sof(H41C)=Sof(H41D)=Sof(C42B)=
 Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43C)=Sof(H43D)=Sof(C44B)=Sof(H44C)=
 Sof(H44D)=Sof(C45B)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-FVAR(1)
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=
 Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=
 Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(1)
 Sof(C52B)=Sof(H52C)=Sof(H52D)=Sof(C53B)=Sof(H53C)=Sof(H53D)=Sof(C54B)=
 Sof(H54C)=Sof(H54D)=Sof(C55B)=Sof(H55C)=Sof(H55D)=Sof(C56B)=Sof(H56C)=
 Sof(H56D)=Sof(C57B)=Sof(H57D)=Sof(H57E)=Sof(H57F)=1-FVAR(2)
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(C55)=
 Sof(H55A)=Sof(H55B)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C53)=Sof(H53A)=Sof(H53B)=
 Sof(C52)=Sof(H52A)=Sof(H52B)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C27(H27), C61(H61)
6.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C26(H26A,H26B), C30(H30A,H30B), C28(H28A,H28B), C32(H32A,
 H32B), C56(H56A,H56B), C55(H55A,H55B), C54(H54A,H54B), C53(H53A,H53B),
 C52(H52A,H52B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
  C44(H44A,H44B), C40B(H40C,H40D), C41B(H41C,H41D), C42B(H42C,H42D), C43B(H43C,
 H43D), C44B(H44C,H44D), C52B(H52C,H52D), C53B(H53C,H53D), C54B(H54C,H54D),
 C55B(H55C,H55D), C56B(H56C,H56D)
6.c Me refined with riding coordinates:
 C57(H57A,H57B,H57C), C45(H45A,H45B,H45C), C45B(H45D,H45E,H45F), C57B(H57D,
 H57E,H57F)
6.d Aromatic/amide H refined with riding coordinates:
 C39(H39), C19(H19), C13(H13), C47(H47), C15(H15), C35(H35), C38(H38),
 C25(H25), C48(H48), C50(H50), C8(H8), C51(H51), C9(H9), C7(H7), C6(H6),
 C36(H36)
6.e Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C29(H29A,H29B,H29C)
;
_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
S1 S 0.46663(11) 0.43063(7) 0.60834(17) 0.0701(8) Uani 1 1 d . U . . .
S2 S 0.42982(10) 0.30951(8) 0.5648(2) 0.0805(9) Uani 1 1 d . U . . .
O2 O 0.5575(3) 0.3355(2) 0.6333(5) 0.0783(19) Uani 1 1 d . U . . .
O1 O 0.4497(4) 0.5055(2) 0.5847(6) 0.095(2) Uani 1 1 d . U . . .
C18 C 0.4228(4) 0.3580(3) 0.5833(7) 0.071(3) Uani 1 1 d . U . . .
C17 C 0.4759(4) 0.3830(3) 0.6085(6) 0.063(2) Uani 1 1 d . U . . .
C34 C 0.2238(4) 0.3410(3) 0.6361(8) 0.075(3) Uani 1 1 d . U . . .
C39 C 0.2095(4) 0.3160(3) 0.6986(9) 0.079(3) Uani 1 1 d . U . . .
H39 H 0.208346 0.289922 0.681424 0.095 Uiso 1 1 calc R . . . .
C16 C 0.5409(4) 0.3727(3) 0.6345(6) 0.064(2) Uani 1 1 d . U . . .
C14 C 0.5479(5) 0.4376(3) 0.6444(6) 0.070(3) Uani 1 1 d . U . . .
C19 C 0.3576(4) 0.3687(3) 0.5730(7) 0.072(3) Uani 1 1 d . U . . .
H19 H 0.343601 0.393832 0.581986 0.087 Uiso 1 1 calc R . . . .
C1 C 0.4964(8) 0.5242(4) 0.6196(8) 0.093(3) Uani 1 1 d . U . . .
C21 C 0.3477(4) 0.3046(3) 0.5437(9) 0.082(3) Uani 1 1 d . U . . .
C20 C 0.3160(4) 0.3381(3) 0.5482(8) 0.077(3) Uani 1 1 d . U . . .
C13 C 0.5810(6) 0.4730(4) 0.6715(7) 0.086(3) Uani 1 1 d . U . . .
H13 H 0.625190 0.469876 0.698249 0.103 Uiso 1 1 calc R . . . .
C47 C 0.2277(5) 0.3557(4) 0.3705(10) 0.094(3) Uani 1 1 d . U . . .
H47 H 0.270567 0.348224 0.368832 0.113 Uiso 1 1 calc R . . . .
C24 C 0.2439(4) 0.3307(3) 0.5402(8) 0.077(3) Uani 1 1 d . U . . .
C2 C 0.5618(6) 0.5088(4) 0.6661(8) 0.090(3) Uani 1 1 d . U . . .
C15 C 0.5808(5) 0.4038(3) 0.6569(7) 0.074(3) Uani 1 1 d . U . . .
H15 H 0.625908 0.401908 0.678390 0.088 Uiso 1 1 calc R . . . .
C46 C 0.2039(5) 0.3513(3) 0.4506(10) 0.088(3) Uani 1 1 d . U . . .
C35 C 0.2249(5) 0.3795(3) 0.6624(10) 0.092(3) Uani 1 1 d . U . . .
H35 H 0.235321 0.398508 0.620326 0.111 Uiso 1 1 calc R . . . .
C38 C 0.1961(5) 0.3256(4) 0.7875(10) 0.096(3) Uani 1 1 d . U . . .
H38 H 0.186950 0.306582 0.830555 0.115 Uiso 1 1 calc R . . . .
C23 C 0.2407(4) 0.2885(3) 0.5182(9) 0.082(3) Uani 1 1 d . U . . .
C25 C 0.3127(4) 0.2348(3) 0.5051(8) 0.081(3) Uani 1 1 d . U . . .
H25 H 0.354807 0.224592 0.511001 0.097 Uiso 1 1 calc R . . . .
C3 C 0.5996(8) 0.5420(4) 0.7043(9) 0.113(4) Uani 1 1 d . U . . .
C5 C 0.5002(10) 0.5652(4) 0.6235(9) 0.112(4) Uani 1 1 d . U . . .
C22 C 0.3036(4) 0.2732(3) 0.5197(9) 0.085(3) Uani 1 1 d . U . . .
C10 C 0.6611(9) 0.5404(5) 0.7670(11) 0.123(5) Uani 1 1 d . U . . .
C11 C 0.6968(11) 0.5081(7) 0.7915(14) 0.128(6) Uani 1 1 d . U . . .
C4 C 0.5599(10) 0.5760(4) 0.6709(8) 0.120(4) Uani 1 1 d . U . . .
C48 C 0.1906(6) 0.3711(4) 0.2905(12) 0.116(4) Uani 1 1 d . U . . .
H48 H 0.207674 0.373427 0.233322 0.139 Uiso 1 1 calc R . . . .
C31 C 0.6642(10) 0.2895(5) 0.4689(19) 0.162(6) Uani 1 1 d . U . . .
H31A H 0.669703 0.317304 0.475662 0.195 Uiso 1 1 calc R . . . .
H31B H 0.706639 0.277585 0.491334 0.195 Uiso 1 1 calc R . . . .
C50 C 0.1063(7) 0.3785(5) 0.3711(14) 0.136(5) Uani 1 1 d . U . . .
H50 H 0.063184 0.385755 0.371623 0.163 Uiso 1 1 calc R . . . .
C27 C 0.6317(7) 0.2847(5) 0.6352(15) 0.135(5) Uani 1 1 d . U . . .
H27 H 0.678283 0.278743 0.656155 0.161 Uiso 1 1 calc R . . . .
C8 C 0.5289(17) 0.6397(6) 0.6440(14) 0.178(8) Uani 1 1 d . U . . .
H8 H 0.536635 0.666063 0.653314 0.213 Uiso 1 1 calc R . . . .
C26 C 0.6246(5) 0.3255(4) 0.6557(11) 0.108(4) Uani 1 1 d . U . . .
H26A H 0.641545 0.330664 0.724223 0.130 Uiso 1 1 calc R . . . .
H26B H 0.649247 0.340902 0.616635 0.130 Uiso 1 1 calc R . . . .
C51 C 0.1437(5) 0.3633(4) 0.4539(12) 0.113(4) Uani 1 1 d . U . . .
H51 H 0.127106 0.361505 0.511655 0.136 Uiso 1 1 calc R . . . .
C30 C 0.6169(9) 0.2759(5) 0.5337(16) 0.145(5) Uani 1 1 d . U . . .
H30A H 0.574241 0.286851 0.507788 0.174 Uiso 1 1 calc R . . . .
H30B H 0.612884 0.248020 0.527126 0.174 Uiso 1 1 calc R . . . .
C49 C 0.1306(7) 0.3828(6) 0.2915(14) 0.138(5) Uani 1 1 d D U . . .
C9 C 0.5823(14) 0.6149(5) 0.6828(12) 0.161(7) Uani 1 1 d . U . . .
H9 H 0.624383 0.622824 0.710913 0.193 Uiso 1 1 calc R . . . .
C7 C 0.4715(15) 0.6305(5) 0.5979(11) 0.170(7) Uani 1 1 d . U . . .
H7 H 0.442602 0.649929 0.571155 0.204 Uiso 1 1 calc R . . . .
C28 C 0.5948(9) 0.2593(5) 0.6993(15) 0.157(6) Uani 1 1 d . U . . .
H28A H 0.598461 0.271243 0.763200 0.188 Uiso 1 1 calc R . . . .
H28B H 0.548704 0.258721 0.669831 0.188 Uiso 1 1 calc R . . . .
N2 N 0.7096(11) 0.6024(5) 0.8509(12) 0.200(9) Uani 1 1 d . U . . .
C12 C 0.6840(10) 0.5770(5) 0.8093(13) 0.153(6) Uani 1 1 d . U . . .
C6 C 0.4512(11) 0.5907(5) 0.5872(9) 0.143(5) Uani 1 1 d . U . . .
H6 H 0.409096 0.582995 0.558563 0.172 Uiso 1 1 calc R . . . .
C33 C 0.6884(14) 0.2904(5) 0.298(3) 0.228(12) Uani 1 1 d . U . . .
H33A H 0.679748 0.273497 0.242679 0.341 Uiso 1 1 calc GR . . . .
H33B H 0.733058 0.287272 0.330758 0.341 Uiso 1 1 calc GR . . . .
H33C H 0.681190 0.316763 0.277261 0.341 Uiso 1 1 calc GR . . . .
C32 C 0.6430(13) 0.2804(5) 0.369(2) 0.187(8) Uani 1 1 d . U . . .
H32A H 0.601607 0.293499 0.346442 0.224 Uiso 1 1 calc R . . . .
H32B H 0.634353 0.252766 0.363615 0.224 Uiso 1 1 calc R . . . .
N1 N 0.7274(8) 0.4811(7) 0.8162(16) 0.183(8) Uani 1 1 d . U . . .
C29 C 0.6185(15) 0.2202(8) 0.712(3) 0.253(14) Uani 1 1 d . U . . .
H29A H 0.599252 0.204991 0.655975 0.379 Uiso 1 1 calc GR . . . .
H29B H 0.606862 0.209364 0.769771 0.379 Uiso 1 1 calc GR . . . .
H29C H 0.665363 0.220081 0.717414 0.379 Uiso 1 1 calc GR . . . .
C57 C 0.040(3) 0.5723(14) 0.090(5) 0.32(3) Uani 0.62(2) 1 d D U P A 1
H57A H 0.001597 0.584788 0.053496 0.482 Uiso 0.62(2) 1 calc R . P A 1
H57B H 0.051785 0.584625 0.152469 0.482 Uiso 0.62(2) 1 calc R . P A 1
H57C H 0.075249 0.574307 0.054464 0.482 Uiso 0.62(2) 1 calc R . P A 1
C56 C 0.026(2) 0.5342(12) 0.103(5) 0.264(16) Uani 0.62(2) 1 d D U P A 1
H56A H -0.010844 0.532795 0.136648 0.316 Uiso 0.62(2) 1 calc R . P A 1
H56B H 0.012540 0.522512 0.038978 0.316 Uiso 0.62(2) 1 calc R . P A 1
C55 C 0.076(2) 0.5123(10) 0.154(4) 0.226(13) Uani 0.62(2) 1 d D U P A 1
H55A H 0.079519 0.518756 0.222353 0.272 Uiso 0.62(2) 1 calc R . P A 1
H55B H 0.116046 0.520377 0.133672 0.272 Uiso 0.62(2) 1 calc R . P A 1
C54 C 0.0717(19) 0.4726(9) 0.145(3) 0.204(11) Uani 0.62(2) 1 d D U P A 1
H54A H 0.083820 0.465354 0.083549 0.245 Uiso 0.62(2) 1 calc R . P A 1
H54B H 0.026235 0.465178 0.142019 0.245 Uiso 0.62(2) 1 calc R . P A 1
C53 C 0.110(2) 0.4505(10) 0.219(3) 0.193(11) Uani 0.62(2) 1 d D U P A 1
H53A H 0.155527 0.453556 0.214032 0.232 Uiso 0.62(2) 1 calc R . P A 1
H53B H 0.104396 0.460956 0.282096 0.232 Uiso 0.62(2) 1 calc R . P A 1
C52 C 0.0952(18) 0.4115(10) 0.217(3) 0.171(9) Uani 0.62(2) 1 d D U P A 1
H52A H 0.100182 0.402075 0.153462 0.205 Uiso 0.62(2) 1 calc R . P A 1
H52B H 0.049014 0.409470 0.220485 0.205 Uiso 0.62(2) 1 calc R . P A 1
C40 C 0.1877(13) 0.3747(15) 0.9147(19) 0.149(7) Uani 0.65(2) 1 d D U P B 1
H40A H 0.211906 0.356404 0.960468 0.179 Uiso 0.65(2) 1 calc R . P B 1
H40B H 0.206070 0.400236 0.930723 0.179 Uiso 0.65(2) 1 calc R . P B 1
C41 C 0.1216(14) 0.3746(9) 0.925(3) 0.169(9) Uani 0.65(2) 1 d D U P B 1
H41A H 0.097995 0.390565 0.873249 0.202 Uiso 0.65(2) 1 calc R . P B 1
H41B H 0.119541 0.387985 0.986245 0.202 Uiso 0.65(2) 1 calc R . P B 1
C42 C 0.0848(13) 0.3397(9) 0.926(3) 0.180(9) Uani 0.65(2) 1 d D U P B 1
H42A H 0.083527 0.327684 0.862829 0.216 Uiso 0.65(2) 1 calc R . P B 1
H42B H 0.110980 0.322755 0.973761 0.216 Uiso 0.65(2) 1 calc R . P B 1
C43 C 0.0198(13) 0.3378(9) 0.945(3) 0.197(10) Uani 0.65(2) 1 d D U P B 1
H43A H 0.020242 0.351995 1.005830 0.236 Uiso 0.65(2) 1 calc R . P B 1
H43B H -0.007076 0.352835 0.894205 0.236 Uiso 0.65(2) 1 calc R . P B 1
C44 C -0.0150(14) 0.3035(9) 0.954(3) 0.178(10) Uani 0.65(2) 1 d D U P B 1
H44A H 0.009995 0.289949 1.009611 0.214 Uiso 0.65(2) 1 calc R . P B 1
H44B H -0.055431 0.311537 0.973872 0.214 Uiso 0.65(2) 1 calc R . P B 1
C45 C -0.0333(15) 0.2751(11) 0.883(3) 0.173(12) Uani 0.65(2) 1 d D U P B 1
H45A H -0.056649 0.254803 0.908732 0.259 Uiso 0.65(2) 1 calc R . P B 1
H45B H -0.061018 0.286418 0.826818 0.259 Uiso 0.65(2) 1 calc R . P B 1
H45C H 0.005186 0.264574 0.862982 0.259 Uiso 0.65(2) 1 calc R . P B 1
C37 C 0.1963(6) 0.3642(4) 0.8126(11) 0.111(4) Uani 1 1 d D U . . .
C36 C 0.2108(6) 0.3889(4) 0.7489(12) 0.111(4) Uani 1 1 d . U . . .
H36 H 0.211247 0.415032 0.765126 0.134 Uiso 1 1 calc R . . . .
C61 C 0.2333(8) 0.4968(5) 0.424(3) 0.245(12) Uani 1 1 d D U . . .
H61 H 0.227972 0.502457 0.353996 0.294 Uiso 1 1 calc R . . . .
Cl63 Cl 0.1700(7) 0.5164(4) 0.4461(18) 0.421(11) Uani 1 1 d D U . . .
Cl61 Cl 0.2397(5) 0.4495(2) 0.4201(8) 0.263(4) Uani 1 1 d D U . . .
Cl62 Cl 0.2994(4) 0.5179(3) 0.4602(6) 0.252(4) Uani 1 1 d D U . . .
C40B C 0.175(2) 0.376(3) 0.906(3) 0.142(9) Uani 0.35(2) 1 d D U P B 2
H40C H 0.176842 0.352879 0.947652 0.171 Uiso 0.35(2) 1 calc R . P B 2
H40D H 0.206164 0.394263 0.939841 0.171 Uiso 0.35(2) 1 calc R . P B 2
C41B C 0.112(2) 0.3916(17) 0.895(5) 0.174(10) Uani 0.35(2) 1 d D U P B 2
H41C H 0.113009 0.415717 0.860009 0.209 Uiso 0.35(2) 1 calc R . P B 2
H41D H 0.105177 0.398439 0.960594 0.209 Uiso 0.35(2) 1 calc R . P B 2
C42B C 0.054(2) 0.3713(19) 0.849(4) 0.184(12) Uani 0.35(2) 1 d D U P B 2
H42C H 0.029247 0.389439 0.804164 0.221 Uiso 0.35(2) 1 calc R . P B 2
H42D H 0.069192 0.351215 0.809563 0.221 Uiso 0.35(2) 1 calc R . P B 2
C43B C 0.009(3) 0.3531(18) 0.901(4) 0.196(12) Uani 0.35(2) 1 d D U P B 2
H43C H 0.033377 0.344719 0.962985 0.235 Uiso 0.35(2) 1 calc R . P B 2
H43D H -0.020824 0.373311 0.914650 0.235 Uiso 0.35(2) 1 calc R . P B 2
C44B C -0.031(2) 0.3216(16) 0.862(5) 0.178(12) Uani 0.35(2) 1 d D U P B 2
H44C H -0.060590 0.316998 0.907710 0.213 Uiso 0.35(2) 1 calc R . P B 2
H44D H -0.057925 0.330869 0.802248 0.213 Uiso 0.35(2) 1 calc R . P B 2
C45B C -0.008(3) 0.2852(19) 0.840(6) 0.20(2) Uani 0.35(2) 1 d D U P B 2
H45D H -0.044220 0.268709 0.815312 0.304 Uiso 0.35(2) 1 calc R . P B 2
H45E H 0.019702 0.287984 0.792209 0.304 Uiso 0.35(2) 1 calc R . P B 2
H45F H 0.017010 0.273973 0.898732 0.304 Uiso 0.35(2) 1 calc R . P B 2
C52B C 0.083(3) 0.3932(14) 0.198(3) 0.163(12) Uani 0.38(2) 1 d D U P A 2
H52C H 0.090290 0.375334 0.147442 0.195 Uiso 0.38(2) 1 calc R . P A 2
H52D H 0.038940 0.388957 0.209870 0.195 Uiso 0.38(2) 1 calc R . P A 2
C53B C 0.087(3) 0.4306(13) 0.164(3) 0.191(11) Uani 0.38(2) 1 d D U P A 2
H53C H 0.048929 0.435164 0.113619 0.229 Uiso 0.38(2) 1 calc R . P A 2
H53D H 0.125347 0.432197 0.133064 0.229 Uiso 0.38(2) 1 calc R . P A 2
C54B C 0.091(4) 0.4604(14) 0.233(4) 0.195(12) Uani 0.38(2) 1 d D U P A 2
H54C H 0.054448 0.457605 0.267747 0.234 Uiso 0.38(2) 1 calc R . P A 2
H54D H 0.130880 0.456997 0.280827 0.234 Uiso 0.38(2) 1 calc R . P A 2
C55B C 0.090(3) 0.4978(14) 0.197(6) 0.221(13) Uani 0.38(2) 1 d D U P A 2
H55C H 0.131551 0.509659 0.225649 0.265 Uiso 0.38(2) 1 calc R . P A 2
H55D H 0.089477 0.495819 0.127368 0.265 Uiso 0.38(2) 1 calc R . P A 2
C56B C 0.042(4) 0.5231(18) 0.209(6) 0.238(15) Uani 0.38(2) 1 d D U P A 2
H56C H 0.044671 0.527470 0.278936 0.286 Uiso 0.38(2) 1 calc R . P A 2
H56D H 0.000053 0.511159 0.184843 0.286 Uiso 0.38(2) 1 calc R . P A 2
C57B C 0.044(4) 0.5581(18) 0.165(6) 0.25(2) Uani 0.38(2) 1 d D U P A 2
H57D H 0.008558 0.573978 0.177271 0.378 Uiso 0.38(2) 1 calc R . P A 2
H57E H 0.084998 0.570723 0.189656 0.378 Uiso 0.38(2) 1 calc R . P A 2
H57F H 0.040271 0.554372 0.095333 0.378 Uiso 0.38(2) 1 calc R . P A 2


_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 C17 1.689(10) . ?
S1 C14 1.722(10) . ?
S2 C18 1.740(10) . ?
S2 C21 1.720(9) . ?
O2 C16 1.358(12) . ?
O2 C26 1.442(13) . ?
O1 C1 1.215(15) . ?
C18 C17 1.423(11) . ?
C18 C19 1.413(13) . ?
C17 C16 1.406(13) . ?
C34 C39 1.324(15) . ?
C34 C24 1.540(15) . ?
C34 C35 1.405(15) . ?
C39 H39 0.9500 . ?
C39 C38 1.384(16) . ?
C16 C15 1.384(12) . ?
C14 C13 1.446(14) . ?
C14 C15 1.378(15) . ?
C19 H19 0.9500 . ?
C19 C20 1.398(12) . ?
C1 C2 1.52(2) . ?
C1 C5 1.446(19) . ?
C21 C20 1.365(14) . ?
C21 C22 1.446(13) . ?
C20 C24 1.531(12) . ?
C13 H13 0.9500 . ?
C13 C2 1.325(18) . ?
C47 H47 0.9500 . ?
C47 C46 1.333(17) . ?
C47 C48 1.369(19) . ?
C24 C46 1.571(17) . ?
C24 C23 1.516(14) . ?
C2 C3 1.465(17) . ?
C15 H15 0.9500 . ?
C46 C51 1.352(16) . ?
C35 H35 0.9500 . ?
C35 C36 1.356(18) . ?
C38 H38 0.9500 . ?
C38 C37 1.407(19) . ?
C23 C25 1.389(12) 7_556 ?
C23 C22 1.433(14) . ?
C25 H25 0.9500 . ?
C25 C22 1.390(15) . ?
C3 C10 1.44(2) . ?
C3 C4 1.49(2) . ?
C5 C4 1.37(2) . ?
C5 C6 1.40(2) . ?
C10 C11 1.37(3) . ?
C10 C12 1.47(2) . ?
C11 N1 1.17(3) . ?
C4 C9 1.45(2) . ?
C48 H48 0.9500 . ?
C48 C49 1.34(2) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C30 1.55(3) . ?
C31 C32 1.45(3) . ?
C50 H50 0.9500 . ?
C50 C51 1.40(2) . ?
C50 C49 1.33(2) . ?
C27 H27 1.0000 . ?
C27 C26 1.48(2) . ?
C27 C30 1.45(3) . ?
C27 C28 1.58(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.46(3) . ?
C8 C7 1.31(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C51 H51 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C49 C52 1.55(3) . ?
C49 C52B 1.55(3) . ?
C9 H9 0.9500 . ?
C7 H7 0.9500 . ?
C7 C6 1.47(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.47(3) . ?
N2 C12 1.154(17) . ?
C6 H6 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C33 C32 1.54(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C57 C56 1.39(3) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 C55 1.39(3) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 C54 1.41(3) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C54 C53 1.43(2) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C52 1.41(3) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.44(2) . ?
C40 C37 1.54(2) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.46(2) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.45(2) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.43(2) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.43(2) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C37 C36 1.33(2) . ?
C37 C40B 1.53(3) . ?
C36 H36 0.9500 . ?
C61 H61 1.0000 . ?
C61 Cl63 1.589(17) . ?
C61 Cl61 1.675(18) . ?
C61 Cl62 1.586(17) . ?
C40B H40C 0.9900 . ?
C40B H40D 0.9900 . ?
C40B C41B 1.43(3) . ?
C41B H41C 0.9900 . ?
C41B H41D 0.9900 . ?
C41B C42B 1.46(3) . ?
C42B H42C 0.9900 . ?
C42B H42D 0.9900 . ?
C42B C43B 1.46(3) . ?
C43B H43C 0.9900 . ?
C43B H43D 0.9900 . ?
C43B C44B 1.44(3) . ?
C44B H44C 0.9900 . ?
C44B H44D 0.9900 . ?
C44B C45B 1.43(3) . ?
C45B H45D 0.9800 . ?
C45B H45E 0.9800 . ?
C45B H45F 0.9800 . ?
C52B H52C 0.9900 . ?
C52B H52D 0.9900 . ?
C52B C53B 1.41(3) . ?
C53B H53C 0.9900 . ?
C53B H53D 0.9900 . ?
C53B C54B 1.43(3) . ?
C54B H54C 0.9900 . ?
C54B H54D 0.9900 . ?
C54B C55B 1.41(3) . ?
C55B H55C 0.9900 . ?
C55B H55D 0.9900 . ?
C55B C56B 1.39(3) . ?
C56B H56C 0.9900 . ?
C56B H56D 0.9900 . ?
C56B C57B 1.39(3) . ?
C57B H57D 0.9800 . ?
C57B H57E 0.9800 . ?
C57B H57F 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
C17 S1 C14 91.8(5) . . ?
C21 S2 C18 90.8(4) . . ?
C16 O2 C26 118.7(8) . . ?
C17 C18 S2 124.1(8) . . ?
C19 C18 S2 110.7(6) . . ?
C19 C18 C17 125.1(9) . . ?
C18 C17 S1 121.9(8) . . ?
C16 C17 S1 111.4(6) . . ?
C16 C17 C18 126.7(9) . . ?
C39 C34 C24 124.6(10) . . ?
C39 C34 C35 117.3(11) . . ?
C35 C34 C24 118.0(10) . . ?
C34 C39 H39 118.1 . . ?
C34 C39 C38 123.9(11) . . ?
C38 C39 H39 118.1 . . ?
O2 C16 C17 119.3(7) . . ?
O2 C16 C15 128.1(9) . . ?
C15 C16 C17 112.6(9) . . ?
C13 C14 S1 127.8(10) . . ?
C15 C14 S1 111.7(7) . . ?
C15 C14 C13 120.1(10) . . ?
C18 C19 H19 123.8 . . ?
C20 C19 C18 112.4(9) . . ?
C20 C19 H19 123.8 . . ?
O1 C1 C2 126.4(12) . . ?
O1 C1 C5 126.2(15) . . ?
C5 C1 C2 107.4(13) . . ?
C20 C21 S2 113.3(6) . . ?
C20 C21 C22 111.7(8) . . ?
C22 C21 S2 135.0(8) . . ?
C19 C20 C24 136.4(9) . . ?
C21 C20 C19 112.7(8) . . ?
C21 C20 C24 109.9(7) . . ?
C14 C13 H13 113.7 . . ?
C2 C13 C14 132.6(12) . . ?
C2 C13 H13 113.7 . . ?
C46 C47 H47 119.9 . . ?
C46 C47 C48 120.3(12) . . ?
C48 C47 H47 119.9 . . ?
C34 C24 C46 114.2(9) . . ?
C20 C24 C34 109.0(8) . . ?
C20 C24 C46 111.4(8) . . ?
C23 C24 C34 113.8(9) . . ?
C23 C24 C20 100.9(8) . . ?
C23 C24 C46 106.8(8) . . ?
C13 C2 C1 127.6(10) . . ?
C13 C2 C3 126.8(14) . . ?
C3 C2 C1 105.6(13) . . ?
C16 C15 H15 123.8 . . ?
C14 C15 C16 112.4(9) . . ?
C14 C15 H15 123.8 . . ?
C47 C46 C24 120.8(10) . . ?
C47 C46 C51 119.7(13) . . ?
C51 C46 C24 119.4(12) . . ?
C34 C35 H35 120.6 . . ?
C36 C35 C34 118.7(12) . . ?
C36 C35 H35 120.6 . . ?
C39 C38 H38 120.8 . . ?
C39 C38 C37 118.4(12) . . ?
C37 C38 H38 120.8 . . ?
C25 C23 C24 129.2(9) 7_556 . ?
C25 C23 C22 119.7(9) 7_556 . ?
C22 C23 C24 111.0(7) . . ?
C23 C25 H25 120.6 7_556 . ?
C23 C25 C22 118.9(9) 7_556 . ?
C22 C25 H25 120.6 . . ?
C2 C3 C4 106.6(14) . . ?
C10 C3 C2 124.7(16) . . ?
C10 C3 C4 128.6(13) . . ?
C4 C5 C1 109.6(16) . . ?
C4 C5 C6 123.9(15) . . ?
C6 C5 C1 126.6(18) . . ?
C23 C22 C21 105.9(9) . . ?
C25 C22 C21 132.7(9) . . ?
C25 C22 C23 121.2(8) . . ?
C3 C10 C12 114.4(19) . . ?
C11 C10 C3 125.7(13) . . ?
C11 C10 C12 119.8(16) . . ?
N1 C11 C10 177(2) . . ?
C5 C4 C3 110.5(13) . . ?
C5 C4 C9 124.8(19) . . ?
C9 C4 C3 124.6(19) . . ?
C47 C48 H48 119.4 . . ?
C49 C48 C47 121.1(15) . . ?
C49 C48 H48 119.4 . . ?
H31A C31 H31B 107.7 . . ?
C30 C31 H31A 108.9 . . ?
C30 C31 H31B 108.9 . . ?
C32 C31 H31A 108.9 . . ?
C32 C31 H31B 108.9 . . ?
C32 C31 C30 113.2(19) . . ?
C51 C50 H50 119.7 . . ?
C49 C50 H50 119.7 . . ?
C49 C50 C51 120.6(14) . . ?
C26 C27 H27 105.9 . . ?
C26 C27 C28 111.0(16) . . ?
C30 C27 H27 105.9 . . ?
C30 C27 C26 113.0(15) . . ?
C30 C27 C28 114.3(15) . . ?
C28 C27 H27 105.9 . . ?
C9 C8 H8 115.6 . . ?
C7 C8 H8 115.6 . . ?
C7 C8 C9 129(2) . . ?
O2 C26 C27 109.0(10) . . ?
O2 C26 H26A 109.9 . . ?
O2 C26 H26B 109.9 . . ?
C27 C26 H26A 109.9 . . ?
C27 C26 H26B 109.9 . . ?
H26A C26 H26B 108.3 . . ?
C46 C51 C50 119.0(14) . . ?
C46 C51 H51 120.5 . . ?
C50 C51 H51 120.5 . . ?
C31 C30 H30A 107.7 . . ?
C31 C30 H30B 107.7 . . ?
C27 C30 C31 118.4(16) . . ?
C27 C30 H30A 107.7 . . ?
C27 C30 H30B 107.7 . . ?
H30A C30 H30B 107.1 . . ?
C48 C49 C52 123(2) . . ?
C48 C49 C52B 122(3) . . ?
C50 C49 C48 119.1(16) . . ?
C50 C49 C52 116(2) . . ?
C50 C49 C52B 117(3) . . ?
C4 C9 C8 108(2) . . ?
C4 C9 H9 126.1 . . ?
C8 C9 H9 126.1 . . ?
C8 C7 H7 119.5 . . ?
C8 C7 C6 121(2) . . ?
C6 C7 H7 119.5 . . ?
C27 C28 H28A 108.8 . . ?
C27 C28 H28B 108.8 . . ?
H28A C28 H28B 107.6 . . ?
C29 C28 C27 114(2) . . ?
C29 C28 H28A 108.8 . . ?
C29 C28 H28B 108.8 . . ?
N2 C12 C10 169(3) . . ?
C5 C6 C7 113(2) . . ?
C5 C6 H6 123.4 . . ?
C7 C6 H6 123.4 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
C31 C32 C33 118(3) . . ?
C31 C32 H32A 107.9 . . ?
C31 C32 H32B 107.9 . . ?
C33 C32 H32A 107.9 . . ?
C33 C32 H32B 107.9 . . ?
H32A C32 H32B 107.2 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
C57 C56 H56A 108.1 . . ?
C57 C56 H56B 108.1 . . ?
H56A C56 H56B 107.3 . . ?
C55 C56 C57 117(4) . . ?
C55 C56 H56A 108.1 . . ?
C55 C56 H56B 108.1 . . ?
C56 C55 H55A 107.6 . . ?
C56 C55 H55B 107.6 . . ?
C56 C55 C54 119(4) . . ?
H55A C55 H55B 107.1 . . ?
C54 C55 H55A 107.6 . . ?
C54 C55 H55B 107.6 . . ?
C55 C54 H54A 107.9 . . ?
C55 C54 H54B 107.9 . . ?
C55 C54 C53 118(3) . . ?
H54A C54 H54B 107.2 . . ?
C53 C54 H54A 107.9 . . ?
C53 C54 H54B 107.9 . . ?
C54 C53 H53A 108.5 . . ?
C54 C53 H53B 108.5 . . ?
H53A C53 H53B 107.5 . . ?
C52 C53 C54 115(3) . . ?
C52 C53 H53A 108.5 . . ?
C52 C53 H53B 108.5 . . ?
C49 C52 H52A 106.5 . . ?
C49 C52 H52B 106.5 . . ?
C53 C52 C49 123(3) . . ?
C53 C52 H52A 106.5 . . ?
C53 C52 H52B 106.5 . . ?
H52A C52 H52B 106.5 . . ?
H40A C40 H40B 107.8 . . ?
C41 C40 H40A 109.1 . . ?
C41 C40 H40B 109.1 . . ?
C41 C40 C37 113(2) . . ?
C37 C40 H40A 109.1 . . ?
C37 C40 H40B 109.1 . . ?
C40 C41 H41A 106.7 . . ?
C40 C41 H41B 106.7 . . ?
C40 C41 C42 122(3) . . ?
H41A C41 H41B 106.6 . . ?
C42 C41 H41A 106.7 . . ?
C42 C41 H41B 106.7 . . ?
C41 C42 H42A 106.2 . . ?
C41 C42 H42B 106.2 . . ?
H42A C42 H42B 106.4 . . ?
C43 C42 C41 124(3) . . ?
C43 C42 H42A 106.2 . . ?
C43 C42 H42B 106.2 . . ?
C42 C43 H43A 106.1 . . ?
C42 C43 H43B 106.1 . . ?
H43A C43 H43B 106.3 . . ?
C44 C43 C42 125(2) . . ?
C44 C43 H43A 106.1 . . ?
C44 C43 H43B 106.1 . . ?
C43 C44 H44A 105.4 . . ?
C43 C44 H44B 105.4 . . ?
H44A C44 H44B 106.0 . . ?
C45 C44 C43 128(3) . . ?
C45 C44 H44A 105.4 . . ?
C45 C44 H44B 105.4 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C38 C37 C40 118(2) . . ?
C38 C37 C40B 119(4) . . ?
C36 C37 C38 116.8(13) . . ?
C36 C37 C40 124(2) . . ?
C36 C37 C40B 124(4) . . ?
C35 C36 H36 117.6 . . ?
C37 C36 C35 124.9(13) . . ?
C37 C36 H36 117.6 . . ?
Cl63 C61 H61 99.3 . . ?
Cl63 C61 Cl61 121.1(13) . . ?
Cl61 C61 H61 99.3 . . ?
Cl62 C61 H61 99.3 . . ?
Cl62 C61 Cl63 117.3(14) . . ?
Cl62 C61 Cl61 113.9(14) . . ?
C37 C40B H40C 108.5 . . ?
C37 C40B H40D 108.5 . . ?
H40C C40B H40D 107.5 . . ?
C41B C40B C37 115(3) . . ?
C41B C40B H40C 108.5 . . ?
C41B C40B H40D 108.5 . . ?
C40B C41B H41C 106.6 . . ?
C40B C41B H41D 106.6 . . ?
C40B C41B C42B 123(4) . . ?
H41C C41B H41D 106.6 . . ?
C42B C41B H41C 106.6 . . ?
C42B C41B H41D 106.6 . . ?
C41B C42B H42C 106.2 . . ?
C41B C42B H42D 106.2 . . ?
H42C C42B H42D 106.4 . . ?
C43B C42B C41B 125(4) . . ?
C43B C42B H42C 106.2 . . ?
C43B C42B H42D 106.2 . . ?
C42B C43B H43C 106.6 . . ?
C42B C43B H43D 106.6 . . ?
H43C C43B H43D 106.5 . . ?
C44B C43B C42B 123(4) . . ?
C44B C43B H43C 106.6 . . ?
C44B C43B H43D 106.6 . . ?
C43B C44B H44C 106.0 . . ?
C43B C44B H44D 106.0 . . ?
H44C C44B H44D 106.3 . . ?
C45B C44B C43B 125(4) . . ?
C45B C44B H44C 106.0 . . ?
C45B C44B H44D 106.0 . . ?
C44B C45B H45D 109.5 . . ?
C44B C45B H45E 109.5 . . ?
C44B C45B H45F 109.5 . . ?
H45D C45B H45E 109.5 . . ?
H45D C45B H45F 109.5 . . ?
H45E C45B H45F 109.5 . . ?
C49 C52B H52C 108.2 . . ?
C49 C52B H52D 108.2 . . ?
H52C C52B H52D 107.3 . . ?
C53B C52B C49 116(3) . . ?
C53B C52B H52C 108.2 . . ?
C53B C52B H52D 108.2 . . ?
C52B C53B H53C 108.2 . . ?
C52B C53B H53D 108.2 . . ?
C52B C53B C54B 117(4) . . ?
H53C C53B H53D 107.3 . . ?
C54B C53B H53C 108.2 . . ?
C54B C53B H53D 108.2 . . ?
C53B C54B H54C 108.3 . . ?
C53B C54B H54D 108.3 . . ?
H54C C54B H54D 107.4 . . ?
C55B C54B C53B 116(4) . . ?
C55B C54B H54C 108.3 . . ?
C55B C54B H54D 108.3 . . ?
C54B C55B H55C 107.1 . . ?
C54B C55B H55D 107.1 . . ?
H55C C55B H55D 106.8 . . ?
C56B C55B C54B 121(5) . . ?
C56B C55B H55C 107.1 . . ?
C56B C55B H55D 107.1 . . ?
C55B C56B H56C 108.4 . . ?
C55B C56B H56D 108.4 . . ?
C55B C56B C57B 115(5) . . ?
H56C C56B H56D 107.5 . . ?
C57B C56B H56C 108.4 . . ?
C57B C56B H56D 108.4 . . ?
C56B C57B H57D 109.5 . . ?
C56B C57B H57E 109.5 . . ?
C56B C57B H57F 109.5 . . ?
H57D C57B H57E 109.5 . . ?
H57D C57B H57F 109.5 . . ?
H57E C57B H57F 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 C17 C16 O2 -176.5(6) . . . . ?
S1 C17 C16 C15 2.3(10) . . . . ?
S1 C14 C13 C2 -9.1(16) . . . . ?
S1 C14 C15 C16 1.9(10) . . . . ?
S2 C18 C17 S1 170.1(5) . . . . ?
S2 C18 C17 C16 -8.7(14) . . . . ?
S2 C18 C19 C20 -1.7(11) . . . . ?
S2 C21 C20 C19 -2.6(14) . . . . ?
S2 C21 C20 C24 -173.5(8) . . . . ?
S2 C21 C22 C23 176.4(11) . . . . ?
S2 C21 C22 C25 0(2) . . . . ?
O2 C16 C15 C14 175.9(8) . . . . ?
O1 C1 C2 C13 4.9(17) . . . . ?
O1 C1 C2 C3 -175.1(10) . . . . ?
O1 C1 C5 C4 178.1(10) . . . . ?
O1 C1 C5 C6 -0.6(18) . . . . ?
C18 S2 C21 C20 1.4(10) . . . . ?
C18 S2 C21 C22 179.3(14) . . . . ?
C18 C17 C16 O2 2.5(13) . . . . ?
C18 C17 C16 C15 -178.8(9) . . . . ?
C18 C19 C20 C21 2.8(14) . . . . ?
C18 C19 C20 C24 170.4(12) . . . . ?
C17 S1 C14 C13 -173.2(8) . . . . ?
C17 S1 C14 C15 -0.5(7) . . . . ?
C17 C18 C19 C20 -179.7(10) . . . . ?
C17 C16 C15 C14 -2.7(11) . . . . ?
C34 C39 C38 C37 1.4(17) . . . . ?
C34 C24 C46 C47 157.2(9) . . . . ?
C34 C24 C46 C51 -25.3(13) . . . . ?
C34 C24 C23 C25 69.5(15) . . . 7_556 ?
C34 C24 C23 C22 -113.2(10) . . . . ?
C34 C35 C36 C37 1(2) . . . . ?
C39 C34 C24 C20 -106.8(10) . . . . ?
C39 C34 C24 C46 127.9(10) . . . . ?
C39 C34 C24 C23 4.9(13) . . . . ?
C39 C34 C35 C36 -0.6(16) . . . . ?
C39 C38 C37 C40 -174.3(15) . . . . ?
C39 C38 C37 C36 -1.3(19) . . . . ?
C39 C38 C37 C40B 174(2) . . . . ?
C16 O2 C26 C27 -171.2(12) . . . . ?
C14 S1 C17 C18 180.0(8) . . . . ?
C14 S1 C17 C16 -1.0(7) . . . . ?
C14 C13 C2 C1 -5.8(18) . . . . ?
C14 C13 C2 C3 174.1(10) . . . . ?
C19 C18 C17 S1 -12.2(14) . . . . ?
C19 C18 C17 C16 168.9(9) . . . . ?
C19 C20 C24 C34 -54.5(17) . . . . ?
C19 C20 C24 C46 72.4(16) . . . . ?
C19 C20 C24 C23 -174.6(13) . . . . ?
C1 C2 C3 C10 170.0(11) . . . . ?
C1 C2 C3 C4 -6.3(11) . . . . ?
C1 C5 C4 C3 -1.5(13) . . . . ?
C1 C5 C4 C9 175.7(11) . . . . ?
C1 C5 C6 C7 -176.8(10) . . . . ?
C21 S2 C18 C17 178.2(9) . . . . ?
C21 S2 C18 C19 0.2(8) . . . . ?
C21 C20 C24 C34 113.3(11) . . . . ?
C21 C20 C24 C46 -119.8(11) . . . . ?
C21 C20 C24 C23 -6.8(12) . . . . ?
C20 C21 C22 C23 -5.6(15) . . . . ?
C20 C21 C22 C25 178.3(13) . . . . ?
C20 C24 C46 C47 33.2(13) . . . . ?
C20 C24 C46 C51 -149.2(11) . . . . ?
C20 C24 C23 C25 -174.0(12) . . . 7_556 ?
C20 C24 C23 C22 3.4(12) . . . . ?
C13 C14 C15 C16 175.2(8) . . . . ?
C13 C2 C3 C10 -9.9(18) . . . . ?
C13 C2 C3 C4 173.7(10) . . . . ?
C47 C46 C51 C50 3(2) . . . . ?
C47 C48 C49 C50 -2(3) . . . . ?
C47 C48 C49 C52 160(2) . . . . ?
C47 C48 C49 C52B -168(2) . . . . ?
C24 C34 C39 C38 175.1(9) . . . . ?
C24 C34 C35 C36 -176.4(10) . . . . ?
C24 C46 C51 C50 -174.2(13) . . . . ?
C24 C23 C22 C21 0.9(14) . . . . ?
C24 C23 C22 C25 177.6(11) . . . . ?
C2 C1 C5 C4 -2.6(12) . . . . ?
C2 C1 C5 C6 178.7(10) . . . . ?
C2 C3 C10 C11 8(2) . . . . ?
C2 C3 C10 C12 -169.5(11) . . . . ?
C2 C3 C4 C5 5.1(12) . . . . ?
C2 C3 C4 C9 -172.1(11) . . . . ?
C15 C14 C13 C2 178.8(10) . . . . ?
C46 C47 C48 C49 2(2) . . . . ?
C46 C24 C23 C25 -57.4(15) . . . 7_556 ?
C46 C24 C23 C22 119.9(10) . . . . ?
C35 C34 C39 C38 -0.4(15) . . . . ?
C35 C34 C24 C20 68.6(12) . . . . ?
C35 C34 C24 C46 -56.7(11) . . . . ?
C35 C34 C24 C23 -179.6(9) . . . . ?
C38 C37 C36 C35 0(2) . . . . ?
C38 C37 C40B C41B -104(6) . . . . ?
C23 C24 C46 C47 -76.1(11) . . . . ?
C23 C24 C46 C51 101.4(12) . . . . ?
C23 C25 C22 C21 -179.6(13) 7_556 . . . ?
C23 C25 C22 C23 5(2) 7_556 . . . ?
C25 C23 C22 C21 178.5(11) 7_556 . . . ?
C25 C23 C22 C25 -5(2) 7_556 . . . ?
C3 C10 C12 N2 173(8) . . . . ?
C3 C4 C9 C8 -178.0(12) . . . . ?
C5 C1 C2 C13 -174.5(10) . . . . ?
C5 C1 C2 C3 5.6(11) . . . . ?
C5 C4 C9 C8 5.2(19) . . . . ?
C22 C21 C20 C19 178.9(10) . . . . ?
C22 C21 C20 C24 8.0(14) . . . . ?
C10 C3 C4 C5 -171.0(12) . . . . ?
C10 C3 C4 C9 12(2) . . . . ?
C11 C10 C12 N2 -5(9) . . . . ?
C4 C3 C10 C11 -176.7(14) . . . . ?
C4 C3 C10 C12 6.0(19) . . . . ?
C4 C5 C6 C7 4.7(17) . . . . ?
C48 C47 C46 C24 175.0(10) . . . . ?
C48 C47 C46 C51 -2.6(18) . . . . ?
C48 C49 C52 C53 -74(5) . . . . ?
C48 C49 C52B C53B -85(5) . . . . ?
C50 C49 C52 C53 88(5) . . . . ?
C50 C49 C52B C53B 109(5) . . . . ?
C8 C7 C6 C5 -5(2) . . . . ?
C26 O2 C16 C17 177.2(10) . . . . ?
C26 O2 C16 C15 -1.4(15) . . . . ?
C26 C27 C30 C31 70.6(19) . . . . ?
C26 C27 C28 C29 -157.6(19) . . . . ?
C51 C50 C49 C48 3(3) . . . . ?
C51 C50 C49 C52 -160(2) . . . . ?
C51 C50 C49 C52B 170(2) . . . . ?
C30 C31 C32 C33 -176.4(16) . . . . ?
C30 C27 C26 O2 68.3(18) . . . . ?
C30 C27 C28 C29 73(2) . . . . ?
C49 C50 C51 C46 -3(3) . . . . ?
C49 C52B C53B C54B -46(8) . . . . ?
C9 C8 C7 C6 6(3) . . . . ?
C7 C8 C9 C4 -6(3) . . . . ?
C28 C27 C26 O2 -61.5(16) . . . . ?
C28 C27 C30 C31 -161.2(15) . . . . ?
C6 C5 C4 C3 177.2(10) . . . . ?
C6 C5 C4 C9 -5.6(19) . . . . ?
C32 C31 C30 C27 -177.7(17) . . . . ?
C57 C56 C55 C54 -162(6) . . . . ?
C56 C55 C54 C53 -160(5) . . . . ?
C55 C54 C53 C52 169(5) . . . . ?
C54 C53 C52 C49 -180(4) . . . . ?
C40 C41 C42 C43 174(3) . . . . ?
C40 C37 C36 C35 172.8(18) . . . . ?
C41 C40 C37 C38 -82(4) . . . . ?
C41 C40 C37 C36 106(3) . . . . ?
C41 C42 C43 C44 -175(4) . . . . ?
C42 C43 C44 C45 -62(5) . . . . ?
C37 C40 C41 C42 72(5) . . . . ?
C37 C40B C41B C42B 59(7) . . . . ?
C36 C37 C40B C41B 71(6) . . . . ?
C40B C37 C36 C35 -175(2) . . . . ?
C40B C41B C42B C43B 103(8) . . . . ?
C41B C42B C43B C44B -154(6) . . . . ?
C42B C43B C44B C45B 63(11) . . . . ?
C52B C53B C54B C55B -176(6) . . . . ?
C53B C54B C55B C56B 120(9) . . . . ?
C54B C55B C56B C57B -176(7) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id 'Sample #19:IEICO'
_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 3.376
_oxdiff_exptl_absorpt_empirical_full_min 0.646


# start Validation Reply Form
_vrf_PLAT084_IEICO               
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.50 Report
RESPONSE: 
Poorly diffracting crystals, for which the modelling of the alkyl side-chains
was challenging and potentially inaccurate. However the data provides sufficient
information regarding the core of the structure.

;
# end Validation Reply Form


####################################################################### 
# 
# 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_IDT01
_database_code_depnum_ccdc_archive 'CCDC 1942954'
loop_
_audit_author_name
_audit_author_address
'Peter Horton'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2019-07-24 deposited with the CCDC.	2019-11-18 downloaded from the CCDC.
;

#2008com1125new

_audit_creation_date             2019-04-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C10 H9 S)'
_chemical_formula_sum            'C20 H18 S2'
_chemical_formula_weight         322.46
_chemical_compound_source        Merck
_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 0.0033 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'
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                   8.4290(2)
_cell_length_b                   9.7140(3)
_cell_length_c                   11.0760(3)
_cell_angle_alpha                82.096(2)
_cell_angle_beta                 69.206(2)
_cell_angle_gamma                76.828(2)
_cell_volume                     823.92(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7904
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  0.9511
_exptl_absorpt_correction_T_min  0.9293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_exptl_special_details           
;

;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19156
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.603
_diffrn_reflns_theta_min         3.066
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans to fill the asymmetric unit'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Bruker Nonius FR591 Rotating Anode'
_diffrn_special_details          ?
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2914
_reflns_number_total             3772
_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     >2σ(I)
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3789
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0466
_refine_ls_restrained_S_all      1.055
_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)+(0.0419P)²+0.4315P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1155
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C8(H8), C11(H11), C12(H12), C18(H18)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_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
S1 S 0.47105(7) 0.45851(6) 0.21234(5) 0.02440(15) Uani 1 1 d . . . . .
S2 S 1.04703(6) 0.82677(5) 0.34031(5) 0.02134(15) Uani 1 1 d . . . . .
C1 C 0.4423(3) 0.3772(2) 0.3657(2) 0.0274(5) Uani 1 1 d . . . . .
H1 H 0.333759 0.360466 0.424311 0.033 Uiso 1 1 calc R . . . .
C2 C 0.5923(3) 0.3398(2) 0.3933(2) 0.0247(5) Uani 1 1 d . . . . .
H2 H 0.600709 0.294549 0.473063 0.030 Uiso 1 1 calc R . . . .
C3 C 0.7342(3) 0.3768(2) 0.28804(19) 0.0200(4) Uani 1 1 d . . . . .
C4 C 0.9257(3) 0.3670(2) 0.26078(19) 0.0192(4) Uani 1 1 d . . . . .
C5 C 0.9807(3) 0.43354(19) 0.12233(19) 0.0176(4) Uani 1 1 d . . . . .
C6 C 0.8374(2) 0.47945(19) 0.07862(19) 0.0171(4) Uani 1 1 d . . . . .
C7 C 0.6884(2) 0.4414(2) 0.18378(19) 0.0193(4) Uani 1 1 d . . . . .
C8 C 0.8553(2) 0.5468(2) -0.04356(18) 0.0177(4) Uani 1 1 d . . . . .
H8 H 0.758481 0.578265 -0.072072 0.021 Uiso 1 1 calc R . . . .
C9 C 0.9558(3) 0.4561(2) 0.3526(2) 0.0259(5) Uani 1 1 d . . . . .
H9A H 1.079854 0.454501 0.328319 0.039 Uiso 1 1 calc GR . . . .
H9B H 0.912264 0.416404 0.441744 0.039 Uiso 1 1 calc GR . . . .
H9C H 0.894386 0.553949 0.346168 0.039 Uiso 1 1 calc GR . . . .
C10 C 1.0218(3) 0.2131(2) 0.2687(2) 0.0280(5) Uani 1 1 d . . . . .
H10A H 1.000797 0.157558 0.210405 0.042 Uiso 1 1 calc GR . . . .
H10B H 0.979880 0.172528 0.357640 0.042 Uiso 1 1 calc GR . . . .
H10C H 1.146174 0.211137 0.243096 0.042 Uiso 1 1 calc GR . . . .
C11 C 1.1126(3) 0.7889(2) 0.1798(2) 0.0243(5) Uani 1 1 d . . . . .
H11 H 1.228445 0.750051 0.130888 0.029 Uiso 1 1 calc R . . . .
C12 C 0.9799(3) 0.8207(2) 0.1309(2) 0.0231(5) Uani 1 1 d . . . . .
H12 H 0.992093 0.806292 0.044709 0.028 Uiso 1 1 calc R . . . .
C13 C 0.8217(3) 0.8778(2) 0.22520(19) 0.0193(4) Uani 1 1 d . . . . .
C14 C 0.6359(3) 0.9322(2) 0.23023(19) 0.0197(4) Uani 1 1 d . . . . .
C15 C 0.5498(2) 0.9710(2) 0.37078(18) 0.0176(4) Uani 1 1 d . . . . .
C16 C 0.6715(2) 0.94548(19) 0.43602(18) 0.0174(4) Uani 1 1 d . . . . .
C17 C 0.8376(2) 0.8867(2) 0.34224(19) 0.0183(4) Uani 1 1 d . . . . .
C18 C 0.6230(2) 0.9751(2) 0.56552(18) 0.0183(4) Uani 1 1 d . . . . .
H18 H 0.705758 0.958713 0.608479 0.022 Uiso 1 1 calc R . . . .
C19 C 0.5580(3) 0.8169(2) 0.2026(2) 0.0295(5) Uani 1 1 d . . . . .
H19A H 0.567607 0.734470 0.263268 0.044 Uiso 1 1 calc GR . . . .
H19B H 0.620774 0.788712 0.113770 0.044 Uiso 1 1 calc GR . . . .
H19C H 0.435882 0.853728 0.212948 0.044 Uiso 1 1 calc GR . . . .
C20 C 0.6213(3) 1.0623(2) 0.1359(2) 0.0288(5) Uani 1 1 d . . . . .
H20A H 0.499296 1.099049 0.145749 0.043 Uiso 1 1 calc GR . . . .
H20B H 0.685010 1.035129 0.046952 0.043 Uiso 1 1 calc GR . . . .
H20C H 0.670222 1.135742 0.154925 0.043 Uiso 1 1 calc GR . . . .


_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 C1 1.730(2) . ?
S1 C7 1.717(2) . ?
S2 C11 1.729(2) . ?
S2 C17 1.722(2) . ?
C1 H1 0.9500 . ?
C1 C2 1.363(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.417(3) . ?
C3 C4 1.516(3) . ?
C3 C7 1.372(3) . ?
C4 C5 1.531(3) . ?
C4 C9 1.540(3) . ?
C4 C10 1.536(3) . ?
C5 C6 1.414(3) . ?
C5 C8 1.388(3) 2_765 ?
C6 C7 1.458(3) . ?
C6 C8 1.392(3) . ?
C8 H8 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11 0.9500 . ?
C11 C12 1.366(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.418(3) . ?
C13 C14 1.518(3) . ?
C13 C17 1.366(3) . ?
C14 C15 1.525(3) . ?
C14 C19 1.533(3) . ?
C14 C20 1.537(3) . ?
C15 C16 1.414(3) . ?
C15 C18 1.385(3) 2_676 ?
C16 C17 1.460(3) . ?
C16 C18 1.397(3) . ?
C18 H18 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 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
C7 S1 C1 90.82(10) . . ?
C17 S2 C11 90.59(10) . . ?
S1 C1 H1 123.6 . . ?
C2 C1 S1 112.71(16) . . ?
C2 C1 H1 123.6 . . ?
C1 C2 H2 124.2 . . ?
C1 C2 C3 111.54(19) . . ?
C3 C2 H2 124.2 . . ?
C2 C3 C4 136.51(19) . . ?
C7 C3 C2 113.02(19) . . ?
C7 C3 C4 110.45(17) . . ?
C3 C4 C5 100.98(15) . . ?
C3 C4 C9 111.05(16) . . ?
C3 C4 C10 112.24(17) . . ?
C5 C4 C9 110.26(16) . . ?
C5 C4 C10 111.65(16) . . ?
C10 C4 C9 110.35(17) . . ?
C6 C5 C4 111.15(17) . . ?
C8 C5 C4 128.12(17) 2_765 . ?
C8 C5 C6 120.72(18) 2_765 . ?
C5 C6 C7 106.18(17) . . ?
C8 C6 C5 121.46(17) . . ?
C8 C6 C7 132.37(18) . . ?
C3 C7 S1 111.90(15) . . ?
C3 C7 C6 111.21(17) . . ?
C6 C7 S1 136.87(16) . . ?
C5 C8 C6 117.82(18) 2_765 . ?
C5 C8 H8 121.1 2_765 . ?
C6 C8 H8 121.1 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
S2 C11 H11 123.6 . . ?
C12 C11 S2 112.80(16) . . ?
C12 C11 H11 123.6 . . ?
C11 C12 H12 124.3 . . ?
C11 C12 C13 111.40(19) . . ?
C13 C12 H12 124.3 . . ?
C12 C13 C14 136.23(18) . . ?
C17 C13 C12 113.15(18) . . ?
C17 C13 C14 110.62(17) . . ?
C13 C14 C15 100.87(16) . . ?
C13 C14 C19 111.88(16) . . ?
C13 C14 C20 111.32(17) . . ?
C15 C14 C19 110.88(17) . . ?
C15 C14 C20 111.57(16) . . ?
C19 C14 C20 110.06(18) . . ?
C16 C15 C14 111.23(17) . . ?
C18 C15 C14 128.10(18) 2_676 . ?
C18 C15 C16 120.67(18) 2_676 . ?
C15 C16 C17 106.15(17) . . ?
C18 C16 C15 121.55(18) . . ?
C18 C16 C17 132.30(18) . . ?
C13 C17 S2 112.05(15) . . ?
C13 C17 C16 111.11(17) . . ?
C16 C17 S2 136.84(16) . . ?
C15 C18 C16 117.78(18) 2_676 . ?
C15 C18 H18 121.1 2_676 . ?
C16 C18 H18 121.1 . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C14 C20 H20A 109.5 . . ?
C14 C20 H20B 109.5 . . ?
C14 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 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 C1 C2 C3 -0.3(2) . . . . ?
S2 C11 C12 C13 0.4(2) . . . . ?
C1 S1 C7 C3 -0.27(16) . . . . ?
C1 S1 C7 C6 -178.9(2) . . . . ?
C1 C2 C3 C4 178.3(2) . . . . ?
C1 C2 C3 C7 0.1(3) . . . . ?
C2 C3 C4 C5 -179.5(2) . . . . ?
C2 C3 C4 C9 -62.6(3) . . . . ?
C2 C3 C4 C10 61.4(3) . . . . ?
C2 C3 C7 S1 0.1(2) . . . . ?
C2 C3 C7 C6 179.17(17) . . . . ?
C3 C4 C5 C6 1.8(2) . . . . ?
C3 C4 C5 C8 -179.35(19) . . . 2_765 ?
C4 C3 C7 S1 -178.50(13) . . . . ?
C4 C3 C7 C6 0.5(2) . . . . ?
C4 C5 C6 C7 -1.5(2) . . . . ?
C4 C5 C6 C8 178.31(17) . . . . ?
C5 C6 C7 S1 179.31(17) . . . . ?
C5 C6 C7 C3 0.6(2) . . . . ?
C5 C6 C8 C5 0.6(3) . . . 2_765 ?
C7 S1 C1 C2 0.34(17) . . . . ?
C7 C3 C4 C5 -1.3(2) . . . . ?
C7 C3 C4 C9 115.56(19) . . . . ?
C7 C3 C4 C10 -120.38(19) . . . . ?
C7 C6 C8 C5 -179.55(19) . . . 2_765 ?
C8 C5 C6 C7 179.49(17) 2_765 . . . ?
C8 C5 C6 C8 -0.7(3) 2_765 . . . ?
C8 C6 C7 S1 -0.5(4) . . . . ?
C8 C6 C7 C3 -179.2(2) . . . . ?
C9 C4 C5 C6 -115.73(18) . . . . ?
C9 C4 C5 C8 63.1(3) . . . 2_765 ?
C10 C4 C5 C6 121.22(18) . . . . ?
C10 C4 C5 C8 -59.9(3) . . . 2_765 ?
C11 S2 C17 C13 -0.29(16) . . . . ?
C11 S2 C17 C16 -179.8(2) . . . . ?
C11 C12 C13 C14 179.7(2) . . . . ?
C11 C12 C13 C17 -0.6(3) . . . . ?
C12 C13 C14 C15 178.9(2) . . . . ?
C12 C13 C14 C19 61.0(3) . . . . ?
C12 C13 C14 C20 -62.6(3) . . . . ?
C12 C13 C17 S2 0.6(2) . . . . ?
C12 C13 C17 C16 -179.77(17) . . . . ?
C13 C14 C15 C16 1.3(2) . . . . ?
C13 C14 C15 C18 -178.83(19) . . . 2_676 ?
C14 C13 C17 S2 -179.69(13) . . . . ?
C14 C13 C17 C16 0.0(2) . . . . ?
C14 C15 C16 C17 -1.4(2) . . . . ?
C14 C15 C16 C18 179.06(17) . . . . ?
C15 C16 C17 S2 -179.56(17) . . . . ?
C15 C16 C17 C13 0.9(2) . . . . ?
C15 C16 C18 C15 0.8(3) . . . 2_676 ?
C17 S2 C11 C12 -0.05(17) . . . . ?
C17 C13 C14 C15 -0.8(2) . . . . ?
C17 C13 C14 C19 -118.70(19) . . . . ?
C17 C13 C14 C20 117.70(19) . . . . ?
C17 C16 C18 C15 -178.64(19) . . . 2_676 ?
C18 C15 C16 C17 178.75(17) 2_676 . . . ?
C18 C15 C16 C18 -0.8(3) 2_676 . . . ?
C18 C16 C17 S2 -0.1(4) . . . . ?
C18 C16 C17 C13 -179.7(2) . . . . ?
C19 C14 C15 C16 119.99(18) . . . . ?
C19 C14 C15 C18 -60.2(3) . . . 2_676 ?
C20 C14 C15 C16 -116.95(19) . . . . ?
C20 C14 C15 C18 62.9(3) . . . 2_676 ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_ICNA
_database_code_depnum_ccdc_archive 'CCDC 1942953'
loop_
_audit_author_name
_audit_author_address
'Peter Horton'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2019-07-24 deposited with the CCDC.	2019-11-18 downloaded from the CCDC.
;

#2018ncs0777_1b

_audit_creation_date             2019-05-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H22 N2 O S'
_chemical_formula_sum            'C27 H22 N2 O S'
_chemical_formula_weight         422.52
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C27 H22 N2 S O'
_chemical_oxdiff_usercomment     'Sample #5: OPN216 PE'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   4.8299(2)
_cell_length_b                   24.0080(5)
_cell_length_c                   17.9904(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.295(2)
_cell_angle_gamma                90
_cell_volume                     2085.57(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8354
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.0660
_cell_measurement_theta_min      3.0440
_shelx_estimated_absorpt_T_max   0.955
_shelx_estimated_absorpt_T_min   0.727
_exptl_absorpt_coefficient_mu    1.546
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             888
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of Pet. ether and chloroform'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18627
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.233
_diffrn_reflns_theta_min         3.070
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -84.00  94.00   0.50    0.75    --    5.00  20.00 120.00  356
  2  ω   -179.00  -1.00   0.50    3.00    --  -90.00  58.00  55.21  356
  3  ω   -179.00  -1.00   0.50    3.00    --  -90.00  57.00  25.10  356
  4  ω   -179.00  -1.00   0.50    3.00    --  -90.00  59.00  81.10  356
  5  ω   -179.00  -1.00   0.50    3.00    --  -90.00  30.00 -60.00  356
  6  ω   -179.00  -1.00   0.50    3.00    --  -90.00  30.00   0.00  356
  7  ω   -179.00 -87.00   0.50    3.00    --  -90.00  30.00 150.00  184
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter χ goniometer'
_diffrn_measurement_device_type  
'Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0385294000
_diffrn_orient_matrix_UB_12      0.0625763000
_diffrn_orient_matrix_UB_13      0.0154408000
_diffrn_orient_matrix_UB_21      -0.1274530000
_diffrn_orient_matrix_UB_22      0.0076901000
_diffrn_orient_matrix_UB_23      -0.0785553000
_diffrn_orient_matrix_UB_31      -0.2902290000
_diffrn_orient_matrix_UB_32      -0.0118124000
_diffrn_orient_matrix_UB_33      0.0303412000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3260
_reflns_number_total             3805
_reflns_odcompleteness_completeness 99.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         3805
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0531
_refine_ls_restrained_S_all      1.098
_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)+(0.0726P)²+1.3123P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1478
_refine_special_details          
'Threre is disorder of the alkyl chain for which some geometrical restraints (SADI) have been used.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C25-C26 \\sim C25-C26B
 with sigma of 0.02
 C27-C26 \\sim C27B-C26B
 with sigma of 0.02
 C25-C27 \\sim C25-C27B
 with sigma of 0.04
3. Others
 Sof(H25C)=Sof(H25D)=Sof(C26B)=Sof(H26C)=Sof(H26D)=Sof(C27B)=Sof(H27D)=
 Sof(H27E)=Sof(H27F)=1-FVAR(1)
 Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=
 Sof(H27C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C25(H25C,
 H25D), C26(H26A,H26B), C26B(H26C,H26D)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C9(H9), C13(H13), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20),
 C21(H21)
4.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C27B(H27D,H27E,H27F)
;
_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
S1 S -0.02570(14) 0.44549(3) 0.77890(3) 0.0410(2) Uani 1 1 d . . . . .
O1 O 0.3248(4) 0.35824(7) 0.79693(8) 0.0430(4) Uani 1 1 d . . . . .
N1 N 0.5110(6) 0.43666(10) 0.46760(11) 0.0573(7) Uani 1 1 d . . . . .
N2 N 1.1119(5) 0.31086(10) 0.47852(11) 0.0503(6) Uani 1 1 d . . . . .
C1 C 0.4691(5) 0.34750(10) 0.74374(11) 0.0364(5) Uani 1 1 d . . . . .
C2 C 0.4609(5) 0.37622(9) 0.67015(11) 0.0349(5) Uani 1 1 d . . . . .
C3 C 0.6653(5) 0.34892(9) 0.62360(11) 0.0344(5) Uani 1 1 d . . . . .
C4 C 0.7975(5) 0.30416(9) 0.66810(11) 0.0355(5) Uani 1 1 d . . . . .
C5 C 0.6801(5) 0.30354(10) 0.74004(11) 0.0360(5) Uani 1 1 d . . . . .
C6 C 0.7633(5) 0.26647(10) 0.79370(12) 0.0389(5) Uani 1 1 d . . . . .
H6 H 0.683617 0.267515 0.841480 0.047 Uiso 1 1 calc R . . . .
C7 C 0.9683(5) 0.22663(10) 0.77768(11) 0.0372(5) Uani 1 1 d . . . . .
C8 C 1.0866(5) 0.22650(10) 0.70496(11) 0.0367(5) Uani 1 1 d . . . . .
C9 C 0.9987(5) 0.26577(10) 0.65129(11) 0.0381(5) Uani 1 1 d . . . . .
H9 H 1.078179 0.265796 0.603467 0.046 Uiso 1 1 calc R . . . .
C10 C 0.7317(5) 0.36113(10) 0.55139(11) 0.0363(5) Uani 1 1 d . . . . .
C11 C 0.6039(6) 0.40383(10) 0.50687(12) 0.0427(6) Uani 1 1 d . . . . .
C12 C 0.9428(6) 0.33240(10) 0.51218(12) 0.0401(6) Uani 1 1 d . . . . .
C13 C 0.2988(5) 0.42054(9) 0.65091(11) 0.0356(5) Uani 1 1 d . . . . .
H13 H 0.328295 0.433313 0.601737 0.043 Uiso 1 1 calc R . . . .
C14 C 0.0937(5) 0.45203(9) 0.68862(11) 0.0352(5) Uani 1 1 d . . . . .
C15 C -0.0413(5) 0.49611(10) 0.65361(12) 0.0386(5) Uani 1 1 d . . . . .
H15 H -0.007241 0.506583 0.603717 0.046 Uiso 1 1 calc R . . . .
C16 C -0.2312(5) 0.52379(10) 0.69766(12) 0.0403(6) Uani 1 1 d . . . . .
H16 H -0.340375 0.554464 0.681087 0.048 Uiso 1 1 calc R . . . .
C17 C -0.2418(6) 0.50139(11) 0.76814(12) 0.0427(6) Uani 1 1 d . . . . .
C18 C 1.0611(6) 0.18660(10) 0.82995(12) 0.0427(6) Uani 1 1 d . . . . .
H18 H 0.984348 0.186023 0.878101 0.051 Uiso 1 1 calc R . . . .
C19 C 1.2598(6) 0.14868(11) 0.81228(13) 0.0446(6) Uani 1 1 d . . . . .
H19 H 1.319901 0.122102 0.848286 0.053 Uiso 1 1 calc R . . . .
C20 C 1.3766(6) 0.14854(10) 0.74125(13) 0.0435(6) Uani 1 1 d . . . . .
H20 H 1.515034 0.122001 0.729697 0.052 Uiso 1 1 calc R . . . .
C21 C 1.2914(6) 0.18648(10) 0.68887(12) 0.0411(6) Uani 1 1 d . . . . .
H21 H 1.370871 0.185947 0.641046 0.049 Uiso 1 1 calc R . . . .
C22 C -0.4126(7) 0.52232(13) 0.83092(13) 0.0540(7) Uani 1 1 d . . . . .
H22A H -0.530314 0.491445 0.848435 0.065 Uiso 1 1 calc R . . . .
H22B H -0.537097 0.552017 0.811715 0.065 Uiso 1 1 calc R . . . .
C23 C -0.2466(7) 0.54515(12) 0.89688(14) 0.0543(7) Uani 1 1 d . . . . .
H23A H -0.113781 0.573319 0.879111 0.065 Uiso 1 1 calc R . . . .
H23B H -0.138895 0.514531 0.920394 0.065 Uiso 1 1 calc R . . . .
C24 C -0.4314(8) 0.57166(13) 0.95466(14) 0.0603(8) Uani 1 1 d . . . . .
H24A H -0.526204 0.604188 0.931814 0.072 Uiso 1 1 calc R . . . .
H24B H -0.575629 0.544433 0.968231 0.072 Uiso 1 1 calc R . . . .
C25 C -0.2804(8) 0.59070(15) 1.02539(16) 0.0711(10) Uani 1 1 d D . . . .
H25A H -0.424979 0.603099 1.059852 0.085 Uiso 0.693(9) 1 calc R . P A 1
H25B H -0.195102 0.556990 1.047829 0.085 Uiso 0.693(9) 1 calc R . P A 1
H25C H -0.101739 0.571447 1.034750 0.085 Uiso 0.307(9) 1 calc R . P A 2
H25D H -0.396409 0.589616 1.070040 0.085 Uiso 0.307(9) 1 calc R . P A 2
C26 C -0.0621(10) 0.63466(17) 1.0271(2) 0.0527(14) Uani 0.693(9) 1 d D . P A 1
H26A H 0.075301 0.626701 0.988510 0.063 Uiso 0.693(9) 1 calc R . P A 1
H26B H 0.035308 0.634294 1.076115 0.063 Uiso 0.693(9) 1 calc R . P A 1
C27 C -0.1891(14) 0.6920(2) 1.0134(3) 0.0568(16) Uani 0.693(9) 1 d D . P A 1
H27A H -0.284557 0.692389 0.964707 0.085 Uiso 0.693(9) 1 calc GR . P A 1
H27B H -0.042394 0.720196 1.014252 0.085 Uiso 0.693(9) 1 calc GR . P A 1
H27C H -0.321855 0.700214 1.052251 0.085 Uiso 0.693(9) 1 calc GR . P A 1
C26B C -0.246(3) 0.6556(5) 0.9886(6) 0.067(4) Uani 0.307(9) 1 d D . P A 2
H26C H -0.170484 0.652919 0.938035 0.081 Uiso 0.307(9) 1 calc R . P A 2
H26D H -0.429573 0.673905 0.984727 0.081 Uiso 0.307(9) 1 calc R . P A 2
C27B C -0.052(3) 0.6902(6) 1.0381(8) 0.068(4) Uani 0.307(9) 1 d D . P A 2
H27D H 0.116671 0.668867 1.049413 0.102 Uiso 0.307(9) 1 calc GR . P A 2
H27E H -0.144375 0.699445 1.084417 0.102 Uiso 0.307(9) 1 calc GR . P A 2
H27F H -0.003159 0.724671 1.012178 0.102 Uiso 0.307(9) 1 calc GR . P A 2


_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 C14 1.743(2) . ?
S1 C17 1.709(3) . ?
O1 C1 1.224(3) . ?
N1 C11 1.143(3) . ?
N2 C12 1.150(3) . ?
C1 C2 1.493(3) . ?
C1 C5 1.470(3) . ?
C2 C3 1.464(3) . ?
C2 C13 1.361(3) . ?
C3 C4 1.477(3) . ?
C3 C10 1.377(3) . ?
C4 C5 1.425(3) . ?
C4 C9 1.378(3) . ?
C5 C6 1.367(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.411(3) . ?
C7 C8 1.439(3) . ?
C7 C18 1.410(3) . ?
C8 C9 1.408(3) . ?
C8 C21 1.414(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.432(3) . ?
C10 C12 1.430(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.429(3) . ?
C14 C15 1.387(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.394(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.379(3) . ?
C17 C22 1.500(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.366(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.408(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.367(3) . ?
C21 H21 0.9500 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.519(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.525(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.522(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 H25C 0.9900 . ?
C25 H25D 0.9900 . ?
C25 C26 1.492(6) . ?
C25 C26B 1.703(11) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.525(6) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C26B H26C 0.9900 . ?
C26B H26D 0.9900 . ?
C26B C27B 1.524(13) . ?
C27B H27D 0.9800 . ?
C27B H27E 0.9800 . ?
C27B H27F 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
C17 S1 C14 92.16(11) . . ?
O1 C1 C2 126.3(2) . . ?
O1 C1 C5 126.5(2) . . ?
C5 C1 C2 107.22(18) . . ?
C3 C2 C1 107.21(19) . . ?
C13 C2 C1 126.2(2) . . ?
C13 C2 C3 126.59(19) . . ?
C2 C3 C4 107.74(18) . . ?
C10 C3 C2 128.2(2) . . ?
C10 C3 C4 124.0(2) . . ?
C5 C4 C3 108.9(2) . . ?
C9 C4 C3 131.78(19) . . ?
C9 C4 C5 119.3(2) . . ?
C4 C5 C1 108.93(19) . . ?
C6 C5 C1 129.0(2) . . ?
C6 C5 C4 122.1(2) . . ?
C5 C6 H6 120.2 . . ?
C5 C6 C7 119.6(2) . . ?
C7 C6 H6 120.2 . . ?
C6 C7 C8 118.8(2) . . ?
C18 C7 C6 122.6(2) . . ?
C18 C7 C8 118.5(2) . . ?
C9 C8 C7 120.1(2) . . ?
C9 C8 C21 121.1(2) . . ?
C21 C8 C7 118.8(2) . . ?
C4 C9 C8 120.0(2) . . ?
C4 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C3 C10 C11 125.0(2) . . ?
C3 C10 C12 123.1(2) . . ?
C12 C10 C11 111.87(19) . . ?
N1 C11 C10 175.7(3) . . ?
N2 C12 C10 177.3(2) . . ?
C2 C13 H13 113.0 . . ?
C2 C13 C14 133.9(2) . . ?
C14 C13 H13 113.0 . . ?
C13 C14 S1 129.95(17) . . ?
C15 C14 S1 109.26(17) . . ?
C15 C14 C13 120.8(2) . . ?
C14 C15 H15 122.8 . . ?
C14 C15 C16 114.5(2) . . ?
C16 C15 H15 122.8 . . ?
C15 C16 H16 124.0 . . ?
C17 C16 C15 112.1(2) . . ?
C17 C16 H16 124.0 . . ?
C16 C17 S1 112.03(19) . . ?
C16 C17 C22 126.4(2) . . ?
C22 C17 S1 121.51(19) . . ?
C7 C18 H18 119.6 . . ?
C19 C18 C7 120.9(2) . . ?
C19 C18 H18 119.6 . . ?
C18 C19 H19 119.6 . . ?
C18 C19 C20 120.7(2) . . ?
C20 C19 H19 119.6 . . ?
C19 C20 H20 119.9 . . ?
C21 C20 C19 120.2(2) . . ?
C21 C20 H20 119.9 . . ?
C8 C21 H21 119.6 . . ?
C20 C21 C8 120.8(2) . . ?
C20 C21 H21 119.6 . . ?
C17 C22 H22A 108.6 . . ?
C17 C22 H22B 108.6 . . ?
C17 C22 C23 114.8(3) . . ?
H22A C22 H22B 107.5 . . ?
C23 C22 H22A 108.6 . . ?
C23 C22 H22B 108.6 . . ?
C22 C23 H23A 109.2 . . ?
C22 C23 H23B 109.2 . . ?
C22 C23 C24 112.1(3) . . ?
H23A C23 H23B 107.9 . . ?
C24 C23 H23A 109.2 . . ?
C24 C23 H23B 109.2 . . ?
C23 C24 H24A 108.6 . . ?
C23 C24 H24B 108.6 . . ?
H24A C24 H24B 107.6 . . ?
C25 C24 C23 114.7(3) . . ?
C25 C24 H24A 108.6 . . ?
C25 C24 H24B 108.6 . . ?
C24 C25 H25A 106.4 . . ?
C24 C25 H25B 106.4 . . ?
C24 C25 H25C 113.7 . . ?
C24 C25 H25D 113.7 . . ?
C24 C25 C26B 89.9(4) . . ?
H25A C25 H25B 106.5 . . ?
H25C C25 H25D 110.9 . . ?
C26 C25 C24 123.7(3) . . ?
C26 C25 H25A 106.4 . . ?
C26 C25 H25B 106.4 . . ?
C26B C25 H25C 113.7 . . ?
C26B C25 H25D 113.7 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 C27 110.7(4) . . ?
H26A C26 H26B 108.1 . . ?
C27 C26 H26A 109.5 . . ?
C27 C26 H26B 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C26B H26C 109.7 . . ?
C25 C26B H26D 109.7 . . ?
H26C C26B H26D 108.2 . . ?
C27B C26B C25 109.6(9) . . ?
C27B C26B H26C 109.7 . . ?
C27B C26B H26D 109.7 . . ?
C26B C27B H27D 109.5 . . ?
C26B C27B H27E 109.5 . . ?
C26B C27B H27F 109.5 . . ?
H27D C27B H27E 109.5 . . ?
H27D C27B H27F 109.5 . . ?
H27E C27B H27F 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 C14 C15 C16 0.5(3) . . . . ?
S1 C17 C22 C23 64.4(3) . . . . ?
O1 C1 C2 C3 -179.0(2) . . . . ?
O1 C1 C2 C13 2.7(4) . . . . ?
O1 C1 C5 C4 179.0(2) . . . . ?
O1 C1 C5 C6 -1.1(4) . . . . ?
C1 C2 C3 C4 -0.1(3) . . . . ?
C1 C2 C3 C10 -179.8(2) . . . . ?
C1 C2 C13 C14 -1.6(4) . . . . ?
C1 C5 C6 C7 178.8(2) . . . . ?
C2 C1 C5 C4 -0.4(3) . . . . ?
C2 C1 C5 C6 179.6(2) . . . . ?
C2 C3 C4 C5 -0.1(3) . . . . ?
C2 C3 C4 C9 179.2(3) . . . . ?
C2 C3 C10 C11 -1.2(4) . . . . ?
C2 C3 C10 C12 178.0(2) . . . . ?
C2 C13 C14 S1 1.4(4) . . . . ?
C2 C13 C14 C15 -179.7(3) . . . . ?
C3 C2 C13 C14 -179.6(2) . . . . ?
C3 C4 C5 C1 0.3(3) . . . . ?
C3 C4 C5 C6 -179.7(2) . . . . ?
C3 C4 C9 C8 -179.2(2) . . . . ?
C4 C3 C10 C11 179.1(2) . . . . ?
C4 C3 C10 C12 -1.7(4) . . . . ?
C4 C5 C6 C7 -1.2(4) . . . . ?
C5 C1 C2 C3 0.3(3) . . . . ?
C5 C1 C2 C13 -178.0(2) . . . . ?
C5 C4 C9 C8 -0.1(4) . . . . ?
C5 C6 C7 C8 0.6(4) . . . . ?
C5 C6 C7 C18 -179.0(2) . . . . ?
C6 C7 C8 C9 0.3(4) . . . . ?
C6 C7 C8 C21 -179.8(2) . . . . ?
C6 C7 C18 C19 179.9(3) . . . . ?
C7 C8 C9 C4 -0.5(4) . . . . ?
C7 C8 C21 C20 -0.1(4) . . . . ?
C7 C18 C19 C20 -0.1(4) . . . . ?
C8 C7 C18 C19 0.3(4) . . . . ?
C9 C4 C5 C1 -179.1(2) . . . . ?
C9 C4 C5 C6 0.9(4) . . . . ?
C9 C8 C21 C20 179.8(2) . . . . ?
C10 C3 C4 C5 179.6(2) . . . . ?
C10 C3 C4 C9 -1.1(4) . . . . ?
C13 C2 C3 C4 178.2(2) . . . . ?
C13 C2 C3 C10 -1.5(4) . . . . ?
C13 C14 C15 C16 -178.6(2) . . . . ?
C14 S1 C17 C16 1.6(2) . . . . ?
C14 S1 C17 C22 -177.1(2) . . . . ?
C14 C15 C16 C17 0.7(3) . . . . ?
C15 C16 C17 S1 -1.6(3) . . . . ?
C15 C16 C17 C22 177.0(3) . . . . ?
C16 C17 C22 C23 -114.1(3) . . . . ?
C17 S1 C14 C13 177.8(2) . . . . ?
C17 S1 C14 C15 -1.2(2) . . . . ?
C17 C22 C23 C24 173.5(2) . . . . ?
C18 C7 C8 C9 179.9(2) . . . . ?
C18 C7 C8 C21 -0.2(4) . . . . ?
C18 C19 C20 C21 -0.2(4) . . . . ?
C19 C20 C21 C8 0.3(4) . . . . ?
C21 C8 C9 C4 179.6(2) . . . . ?
C22 C23 C24 C25 174.7(3) . . . . ?
C23 C24 C25 C26 62.7(4) . . . . ?
C23 C24 C25 C26B 93.4(5) . . . . ?
C24 C25 C26 C27 71.7(5) . . . . ?
C24 C25 C26B C27B -170.4(9) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id 'Sample #5:OPN216'
_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 2.930
_oxdiff_exptl_absorpt_empirical_full_min 0.718
####################################################################### 
# 
# 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_m-ITIC
_database_code_depnum_ccdc_archive 'CCDC 1942949'
loop_
_audit_author_name
_audit_author_address
'Peter Horton'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2019-07-24 deposited with the CCDC.	2019-11-18 downloaded from the CCDC.
;

#2018ncs0943_2b

_audit_creation_date             2019-05-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C47 H41 N2 O S2), C H Cl3'
_chemical_formula_sum            'C95 H83 Cl3 N4 O2 S4'
_chemical_formula_weight         1547.24
_chemical_melting_point          ?
_chemical_oxdiff_formula         C94H82N4O2S4
_chemical_oxdiff_usercomment     'Sample #21: m-ITIC'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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                   8.7454(13)
_cell_length_b                   18.872(2)
_cell_length_c                   25.2647(18)
_cell_angle_alpha                87.770(8)
_cell_angle_beta                 88.724(9)
_cell_angle_gamma                78.001(12)
_cell_volume                     4075.1(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2866
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.2090
_cell_measurement_theta_min      2.4540
_shelx_estimated_absorpt_T_max   0.954
_shelx_estimated_absorpt_T_min   0.717
_exptl_absorpt_coefficient_mu    2.380
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1624
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of Pet. ether and chloroform'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1316
_diffrn_reflns_av_unetI/netI     0.1258
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            43879
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        58.930
_diffrn_reflns_theta_max         58.930
_diffrn_reflns_theta_min         2.395
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -89.00  48.00   0.50   20.00    --    0.00  28.00  58.00  274
  2  ω    -88.00  88.00   0.50   20.00    --    0.00  10.00-150.00  352
  3  ω    -84.00  94.00   0.50   20.00    --    5.00  28.00  58.00  356
  4  ω   -179.00  -1.00   0.50  100.00    --  -90.00  28.00  58.00  356
  5  ω   -178.00-120.00   0.50  100.00    --  -90.00  59.00 171.21  116
  6  ω   -178.00-119.00   0.50  100.00    --  -90.00  59.00   5.82  118
  7  ω   -111.00 -84.00   0.50  100.00    --  -90.00  59.00   5.82   54
  8  ω    -53.00 -22.00   0.50  100.00    --  -90.00  59.00   5.82   62
  9  ω   -178.00-153.00   0.50  100.00    --  -90.00  58.00-134.21   50
 10  ω   -101.00 -74.00   0.50  100.00    --  -90.00  58.00  60.95   54
 11  ω   -135.00 -12.00   0.50  100.00    --  -90.00  58.00-134.21  246
 12  ω   -178.00-151.00   0.50  100.00    --  -90.00  59.00 -53.70   54
 13  ω   -148.00 -96.00   0.50  100.00    --  -90.00  59.00 -53.70  104
 14  ω    -87.00  -2.00   0.50  100.00    --  -90.00  59.00 -53.70  170
 15  ω   -179.00  -5.00   0.50  100.00    --  -90.00  59.00 108.53  348
 16  ω   -179.00-141.00   0.50  100.00    --  -90.00  58.00  60.95   76
 17  ω   -113.00  -2.00   0.50  100.00    --  -90.00  59.00 171.21  222
 18  ω   -177.00-102.00   0.50  100.00    --  -90.00   0.00 -30.00  150
 19  ω    -89.00 -39.00   0.50  100.00    --  -90.00   0.00 -30.00  100
 20  ω    -33.00  -2.00   0.50  100.00    --  -90.00   0.00 -30.00   62
 21  ω   -172.00-141.00   0.50  100.00    --  -90.00  59.00-113.29   62
 22  ω   -178.00-119.00   0.50  100.00    --  -90.00  49.00 120.00  118
 23  ω   -179.00 -23.00   0.50  100.00    --  -90.00  57.00 -87.97  312
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter χ goniometer'
_diffrn_measurement_device_type  
'Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0225117000
_diffrn_orient_matrix_UB_12      -0.0709938000
_diffrn_orient_matrix_UB_13      -0.0238099000
_diffrn_orient_matrix_UB_21      0.1681615000
_diffrn_orient_matrix_UB_22      -0.0367293000
_diffrn_orient_matrix_UB_23      0.0153029000
_diffrn_orient_matrix_UB_31      -0.0604563000
_diffrn_orient_matrix_UB_32      -0.0241722000
_diffrn_orient_matrix_UB_33      0.0540694000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4311
_reflns_number_total             11657
_reflns_odcompleteness_completeness 98.12
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.146
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.450
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         11657
_refine_ls_number_restraints     1813
_refine_ls_R_factor_all          0.3079
_refine_ls_R_factor_gt           0.1768
_refine_ls_restrained_S_all      1.408
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4418
_refine_ls_wR_factor_ref         0.5171
_refine_special_details          
'The crystal was not of great quality, resulting in a poor structure. However, the overall connectivity especially of the core can be idenitfied. There is likely to be disorder of the alkyl side arms but due to the poor quality of diffraction they could not be suitably modelled. Due to all the above, various geometrical (SADI, DFIX, BUMP) and displacement (SIMU, RIGU) restraints have been used'
_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. Restrained distances
 C42-C43 = C80-C81 = C30-C31 = C92-C93
 1.54 with sigma of 0.02
 C93-C94 \\sim C93A-C94A
 with sigma of 0.02
 C94-C95 \\sim C94A-C95A
 with sigma of 0.02
 C95-C96 \\sim C95A-C96A
 with sigma of 0.02
 C93-C95 \\sim C93A-C95A
 with sigma of 0.04
 C94-C96 \\sim C94A-C96A
 with sigma of 0.04
 C30-C26 \\sim C80-C76 \\sim C42-C38 \\sim C92-C88
 with sigma of 0.02
 C92-C93 \\sim C92A-C93A
 with sigma of 0.02
 C88-C93 \\sim C90-C93A
 with sigma of 0.04
 C92-C94 \\sim C92A-C94A
 with sigma of 0.04
 C92A-C90 \\sim C92-C88
 with sigma of 0.02
 C47-C46 \\sim C46-C45 \\sim C45-C44 \\sim C44-C43 \\sim C43-C42
 with sigma of 0.02
 C47-C45 \\sim C45-C43 \\sim C46-C44 \\sim C44-C42
 with sigma of 0.04
 C35-C34 \\sim C34-C33 \\sim C33-C32 \\sim C32-C31 \\sim C31-C30
 with sigma of 0.02
 C35-C33 \\sim C33-C31 \\sim C34-C32 \\sim C32-C30
 with sigma of 0.04
 C80-C81 \\sim C81-C82 \\sim C82-C83 \\sim C83-C84 \\sim C84-C85
 with sigma of 0.02
 C80-C82 \\sim C82-C84 \\sim C81-C83 \\sim C83-C85
 with sigma of 0.04
 C96-C97 \\sim C96A-C97A
 with sigma of 0.02
 C95-C97 \\sim C95A-C97A
 with sigma of 0.04
 C97-C96 \\sim C96-C95 \\sim C95-C94 \\sim C94-C93 \\sim C93-C92
 with sigma of 0.02
 C97-C95 \\sim C95-C93 \\sim C96-C94 \\sim C94-C92
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H88)=Sof(C92A)=Sof(H92C)=Sof(H92D)=Sof(C93A)=Sof(H93C)=Sof(H93D)=
 Sof(C94A)=Sof(H94C)=Sof(H94D)=Sof(C95A)=Sof(H95C)=Sof(H95D)=Sof(C96A)=
 Sof(H96C)=Sof(H96D)=Sof(C97A)=Sof(H97D)=Sof(H97E)=Sof(H97F)=1-FVAR(1)
 Sof(H90)=Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(C94)=
 Sof(H94A)=Sof(H94B)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(C96)=Sof(H96A)=Sof(H96B)=
 Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(H97C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C101(H101)
6.b Secondary CH2 refined with riding coordinates:
 C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,
 H84B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B),
 C96(H96A,H96B), C92A(H92C,H92D), C93A(H93C,H93D), C94A(H94C,H94D), C95A(H95C,
 H95D), C96A(H96C,H96D), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B),
 C33(H33A,H33B), C34(H34A,H34B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B),
  C45(H45A,H45B), C46(H46A,H46B)
6.c Me refined with riding coordinates:
 C85(H85A,H85B,H85C), C97(H97A,H97B,H97C), C97A(H97D,H97E,H97F), C35(H35A,H35B,
 H35C), C47(H47A,H47B,H47C)
6.d Aromatic/amide H refined with riding coordinates:
 C56(H56), C57(H57), C58(H58), C59(H59), C63(H63), C65(H65), C73(H73),
 C75(H75), C77(H77), C78(H78), C79(H79), C87(H87), C88(H88), C89(H89), C90(H90),
  C91(H91), C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C15(H15), C23(H23),
 C25(H25), C27(H27), C28(H28), C29(H29), C37(H37), C39(H39), C40(H40), C41(H41)
;
_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
S51 S 0.4103(4) 0.4348(2) 0.29284(11) 0.0898(12) Uani 1 1 d . U . . .
S52 S 0.0657(4) 0.6043(2) 0.34973(12) 0.0982(12) Uani 1 1 d . U . . .
O51 O 0.6053(10) 0.3530(5) 0.2262(3) 0.097(3) Uani 1 1 d . U . . .
N51 N 0.4698(17) 0.6613(7) 0.1178(5) 0.116(4) Uani 1 1 d . U . . .
N52 N 0.8479(14) 0.5703(6) 0.0201(4) 0.103(4) Uani 1 1 d . U . . .
C51 C 0.6489(15) 0.3860(8) 0.1883(4) 0.081(3) Uani 1 1 d . U . . .
C52 C 0.5921(14) 0.4627(8) 0.1719(4) 0.079(3) Uani 1 1 d . U . . .
C53 C 0.6786(14) 0.4800(7) 0.1253(4) 0.077(3) Uani 1 1 d . U . . .
C54 C 0.7873(13) 0.4111(7) 0.1122(4) 0.074(3) Uani 1 1 d . U . . .
C55 C 0.7758(15) 0.3550(8) 0.1491(4) 0.078(3) Uani 1 1 d . U . . .
C56 C 0.8574(16) 0.2864(8) 0.1474(5) 0.091(3) Uani 1 1 d . U . . .
H56 H 0.841087 0.250120 0.172709 0.109 Uiso 1 1 calc R . . . .
C57 C 0.9676(17) 0.2715(8) 0.1063(5) 0.096(4) Uani 1 1 d . U . . .
H57 H 1.030829 0.224177 0.104378 0.115 Uiso 1 1 calc R . . . .
C58 C 0.9867(15) 0.3239(8) 0.0684(5) 0.088(3) Uani 1 1 d . U . . .
H58 H 1.060137 0.311589 0.040273 0.105 Uiso 1 1 calc R . . . .
C59 C 0.9006(15) 0.3938(7) 0.0710(4) 0.084(3) Uani 1 1 d . U . . .
H59 H 0.916811 0.429904 0.045521 0.100 Uiso 1 1 calc R . . . .
C60 C 0.6709(15) 0.5419(8) 0.0988(5) 0.084(3) Uani 1 1 d . U . . .
C61 C 0.5644(18) 0.6090(9) 0.1090(5) 0.095(4) Uani 1 1 d . U . . .
C62 C 0.7734(14) 0.5574(7) 0.0544(5) 0.082(3) Uani 1 1 d . U . . .
C63 C 0.4794(15) 0.5100(8) 0.1981(5) 0.092(4) Uani 1 1 d . U . . .
H63 H 0.455287 0.556272 0.180550 0.111 Uiso 1 1 calc R . . . .
C64 C 0.3871(14) 0.5067(8) 0.2464(4) 0.089(3) Uani 1 1 d . U . . .
C65 C 0.2748(15) 0.5652(8) 0.2604(5) 0.093(4) Uani 1 1 d . U . . .
H65 H 0.247304 0.608644 0.239340 0.111 Uiso 1 1 calc R . . . .
C66 C 0.2056(16) 0.5534(8) 0.3094(5) 0.095(4) Uani 1 1 d . U . . .
C67 C 0.2687(14) 0.4868(8) 0.3317(5) 0.084(3) Uani 1 1 d . U . . .
C68 C 0.2073(15) 0.4742(8) 0.3845(5) 0.092(3) Uani 1 1 d . U . . .
C69 C 0.0954(15) 0.5332(9) 0.3961(5) 0.095(3) Uani 1 1 d . U . . .
C70 C 0.0334(15) 0.5242(9) 0.4495(5) 0.094(4) Uani 1 1 d . U . . .
C71 C 0.1087(14) 0.4556(9) 0.4674(5) 0.091(3) Uani 1 1 d . U . . .
C72 C 0.2295(15) 0.4182(8) 0.4284(5) 0.096(3) Uani 1 1 d . U . . .
C73 C -0.0781(14) 0.5705(8) 0.4798(5) 0.095(4) Uani 1 1 d . U . . .
H73 H -0.130784 0.616622 0.466240 0.114 Uiso 1 1 calc R . . . .
C74 C 0.3947(15) 0.4056(9) 0.4511(5) 0.100(4) Uani 1 1 d . U . . .
C75 C 0.4392(18) 0.3472(10) 0.4861(5) 0.118(4) Uani 1 1 d . U . . .
H75 H 0.369437 0.315674 0.493800 0.142 Uiso 1 1 calc R . . . .
C76 C 0.583(2) 0.3339(11) 0.5099(6) 0.134(5) Uani 1 1 d D U . . .
C77 C 0.6829(19) 0.3812(11) 0.4988(6) 0.133(5) Uani 1 1 d . U . . .
H77 H 0.779740 0.373759 0.516688 0.159 Uiso 1 1 calc R . . . .
C78 C 0.6472(19) 0.4362(12) 0.4643(6) 0.128(5) Uani 1 1 d . U . . .
H78 H 0.719956 0.466045 0.455645 0.153 Uiso 1 1 calc R . . . .
C79 C 0.4981(16) 0.4500(10) 0.4402(6) 0.115(4) Uani 1 1 d . U . . .
H79 H 0.469712 0.490378 0.416194 0.138 Uiso 1 1 calc R . . . .
C80 C 0.631(3) 0.2661(12) 0.5504(9) 0.206(8) Uani 1 1 d D U . . .
H80A H 0.582843 0.277550 0.585685 0.247 Uiso 1 1 calc R . . . .
H80B H 0.595133 0.223440 0.537412 0.247 Uiso 1 1 calc R . . . .
C81 C 0.805(3) 0.2509(16) 0.5534(16) 0.372(15) Uani 1 1 d D U . . .
H81A H 0.831375 0.262982 0.516336 0.446 Uiso 1 1 calc R . . . .
H81B H 0.818550 0.293360 0.573250 0.446 Uiso 1 1 calc R . . . .
C82 C 0.950(3) 0.199(2) 0.5682(19) 0.452(19) Uani 1 1 d D U . . .
H82A H 0.932562 0.150263 0.560807 0.542 Uiso 1 1 calc R . . . .
H82B H 0.958259 0.200719 0.607132 0.542 Uiso 1 1 calc R . . . .
C83 C 1.111(3) 0.202(2) 0.5454(15) 0.47(2) Uani 1 1 d D U . . .
H83A H 1.096490 0.247254 0.522766 0.561 Uiso 1 1 calc R . . . .
H83B H 1.174242 0.210508 0.575772 0.561 Uiso 1 1 calc R . . . .
C84 C 1.214(4) 0.144(2) 0.5139(18) 0.47(2) Uani 1 1 d D U . . .
H84A H 1.204648 0.097900 0.531993 0.570 Uiso 1 1 calc R . . . .
H84B H 1.161837 0.145443 0.479387 0.570 Uiso 1 1 calc R . . . .
C85 C 1.384(4) 0.1370(19) 0.5008(14) 0.43(3) Uani 1 1 d D U . . .
H85A H 1.419697 0.093914 0.479804 0.638 Uiso 1 1 calc R . . . .
H85B H 1.399956 0.180106 0.480434 0.638 Uiso 1 1 calc R . . . .
H85C H 1.443275 0.131999 0.533665 0.638 Uiso 1 1 calc R . . . .
C86 C 0.1928(16) 0.3479(8) 0.4069(5) 0.096(3) Uani 1 1 d . U . . .
C87 C 0.0520(17) 0.3287(9) 0.4131(5) 0.107(4) Uani 1 1 d . U . . .
H87 H -0.027308 0.358099 0.433605 0.128 Uiso 1 1 calc R . . . .
C88 C 0.020(2) 0.2678(10) 0.3904(7) 0.132(5) Uani 1 1 d D U . . .
H88 H -0.080915 0.256730 0.393717 0.158 Uiso 0.404(17) 1 calc R . P A 2
C89 C 0.143(2) 0.2218(10) 0.3619(7) 0.143(6) Uani 1 1 d . U . . .
H89 H 0.126532 0.178118 0.347793 0.171 Uiso 1 1 calc R . . . .
C90 C 0.290(2) 0.2422(11) 0.3551(7) 0.141(5) Uani 1 1 d D U . . .
H90 H 0.371991 0.212544 0.335938 0.169 Uiso 0.596(17) 1 calc R . P A 1
C91 C 0.3118(18) 0.3038(9) 0.3758(5) 0.117(5) Uani 1 1 d . U . . .
H91 H 0.408449 0.318366 0.369620 0.140 Uiso 1 1 calc R . . . .
C92 C -0.149(3) 0.2448(16) 0.3892(11) 0.150(9) Uani 0.596(17) 1 d D U P A 1
H92A H -0.230531 0.283905 0.403767 0.180 Uiso 0.596(17) 1 calc R . P A 1
H92B H -0.175814 0.237888 0.352139 0.180 Uiso 0.596(17) 1 calc R . P A 1
C93 C -0.144(3) 0.1759(17) 0.4213(15) 0.209(13) Uani 0.596(17) 1 d D U P A 1
H93A H -0.090694 0.135780 0.399057 0.250 Uiso 0.596(17) 1 calc R . P A 1
H93B H -0.074108 0.177062 0.451528 0.250 Uiso 0.596(17) 1 calc R . P A 1
C94 C -0.285(4) 0.155(2) 0.4433(14) 0.286(17) Uani 0.596(17) 1 d D U P A 1
H94A H -0.376625 0.189955 0.428919 0.343 Uiso 0.596(17) 1 calc R . P A 1
H94B H -0.286224 0.160793 0.482084 0.343 Uiso 0.596(17) 1 calc R . P A 1
C95 C -0.307(4) 0.0806(18) 0.4333(15) 0.33(2) Uani 0.596(17) 1 d D U P A 1
H95A H -0.339311 0.057901 0.466503 0.397 Uiso 0.596(17) 1 calc R . P A 1
H95B H -0.206832 0.050416 0.420865 0.397 Uiso 0.596(17) 1 calc R . P A 1
C96 C -0.431(4) 0.0854(19) 0.3915(12) 0.41(3) Uani 0.596(17) 1 d D U P A 1
H96A H -0.445612 0.036101 0.383912 0.490 Uiso 0.596(17) 1 calc R . P A 1
H96B H -0.532062 0.113667 0.404730 0.490 Uiso 0.596(17) 1 calc R . P A 1
C97 C -0.382(4) 0.1212(17) 0.3419(11) 0.51(4) Uani 0.596(17) 1 d D U P A 1
H97A H -0.462796 0.124202 0.314962 0.767 Uiso 0.596(17) 1 calc R . P A 1
H97B H -0.369409 0.170110 0.349441 0.767 Uiso 0.596(17) 1 calc R . P A 1
H97C H -0.283161 0.092724 0.328672 0.767 Uiso 0.596(17) 1 calc R . P A 1
C92A C 0.455(3) 0.200(2) 0.3320(15) 0.170(13) Uani 0.404(17) 1 d D U P A 2
H92C H 0.444211 0.149379 0.327927 0.204 Uiso 0.404(17) 1 calc R . P A 2
H92D H 0.464630 0.220691 0.295792 0.204 Uiso 0.404(17) 1 calc R . P A 2
C93A C 0.608(3) 0.196(2) 0.357(2) 0.224(17) Uani 0.404(17) 1 d D U P A 2
H93C H 0.688807 0.177746 0.330279 0.269 Uiso 0.404(17) 1 calc R . P A 2
H93D H 0.615799 0.246216 0.363991 0.269 Uiso 0.404(17) 1 calc R . P A 2
C94A C 0.652(5) 0.153(3) 0.4066(18) 0.225(19) Uani 0.404(17) 1 d D U P A 2
H94C H 0.593592 0.113078 0.408603 0.270 Uiso 0.404(17) 1 calc R . P A 2
H94D H 0.616071 0.184255 0.436718 0.270 Uiso 0.404(17) 1 calc R . P A 2
C95A C 0.820(6) 0.120(3) 0.414(3) 0.28(2) Uani 0.404(17) 1 d D U P A 2
H95C H 0.880396 0.157697 0.405005 0.330 Uiso 0.404(17) 1 calc R . P A 2
H95D H 0.834850 0.108246 0.452771 0.330 Uiso 0.404(17) 1 calc R . P A 2
C96A C 0.893(7) 0.054(3) 0.3858(19) 0.29(3) Uani 0.404(17) 1 d D U P A 2
H96C H 0.953620 0.069587 0.355431 0.344 Uiso 0.404(17) 1 calc R . P A 2
H96D H 0.807963 0.034139 0.370888 0.344 Uiso 0.404(17) 1 calc R . P A 2
C97A C 0.998(7) -0.006(3) 0.415(3) 0.35(4) Uani 0.404(17) 1 d D U P A 2
H97D H 1.037465 -0.045485 0.391000 0.518 Uiso 0.404(17) 1 calc R . P A 2
H97E H 1.086721 0.011693 0.428944 0.518 Uiso 0.404(17) 1 calc R . P A 2
H97F H 0.940303 -0.023940 0.444482 0.518 Uiso 0.404(17) 1 calc R . P A 2
S1 S 0.5044(5) -0.2346(3) 0.88629(17) 0.143(2) Uani 1 1 d . U . . .
S2 S 0.2298(5) -0.2241(3) 1.02493(19) 0.150(2) Uani 1 1 d . U . . .
O1 O 0.7171(18) -0.2832(10) 0.8106(5) 0.161(5) Uani 1 1 d . U . . .
N1 N 0.6962(18) -0.5583(8) 0.9570(6) 0.131(5) Uani 1 1 d . U . . .
N2 N 1.044(3) -0.6553(14) 0.8485(8) 0.202(9) Uani 1 1 d . U . . .
C1 C 0.780(3) -0.3465(14) 0.8155(7) 0.138(5) Uani 1 1 d . U . . .
C2 C 0.749(3) -0.3979(13) 0.8600(7) 0.139(5) Uani 1 1 d . U . . .
C3 C 0.857(2) -0.4707(14) 0.8485(7) 0.142(5) Uani 1 1 d . U . . .
C4 C 0.957(3) -0.4619(14) 0.8005(7) 0.150(5) Uani 1 1 d . U . . .
C5 C 0.911(2) -0.3895(14) 0.7805(7) 0.151(5) Uani 1 1 d . U . . .
C6 C 0.981(2) -0.3618(14) 0.7366(8) 0.159(6) Uani 1 1 d . U . . .
H6 H 0.948434 -0.312598 0.724990 0.191 Uiso 1 1 calc R . . . .
C7 C 1.095(3) -0.4068(16) 0.7112(8) 0.164(7) Uani 1 1 d . U . . .
H7 H 1.143111 -0.390066 0.680531 0.197 Uiso 1 1 calc R . . . .
C8 C 1.142(3) -0.4784(15) 0.7298(7) 0.164(6) Uani 1 1 d . U . . .
H8 H 1.224479 -0.509083 0.711348 0.197 Uiso 1 1 calc R . . . .
C9 C 1.077(3) -0.5065(14) 0.7732(7) 0.168(6) Uani 1 1 d . U . . .
H9 H 1.112600 -0.555723 0.784447 0.202 Uiso 1 1 calc R . . . .
C10 C 0.872(3) -0.5371(14) 0.8760(7) 0.142(5) Uani 1 1 d . U . . .
C11 C 0.770(2) -0.5490(10) 0.9226(7) 0.127(5) Uani 1 1 d . U . . .
C12 C 0.963(4) -0.6042(18) 0.8633(8) 0.168(7) Uani 1 1 d . U . . .
C13 C 0.651(2) -0.3812(11) 0.8999(7) 0.136(5) Uani 1 1 d . U . . .
H13 H 0.650808 -0.422259 0.922947 0.163 Uiso 1 1 calc R . . . .
C14 C 0.545(2) -0.3202(13) 0.9182(7) 0.138(5) Uani 1 1 d . U . . .
C15 C 0.459(2) -0.3208(13) 0.9667(7) 0.137(5) Uani 1 1 d . U . . .
H15 H 0.469011 -0.360726 0.991419 0.165 Uiso 1 1 calc R . . . .
C16 C 0.364(2) -0.2586(14) 0.9721(7) 0.139(5) Uani 1 1 d . U . . .
C17 C 0.375(2) -0.2064(13) 0.9353(7) 0.137(4) Uani 1 1 d . U . . .
C18 C 0.273(2) -0.1417(14) 0.9434(7) 0.142(5) Uani 1 1 d . U . . .
C19 C 0.1890(19) -0.1424(13) 0.9927(7) 0.141(5) Uani 1 1 d . U . . .
C20 C 0.083(2) -0.0709(13) 1.0005(8) 0.143(5) Uani 1 1 d . U . . .
C21 C 0.095(2) -0.0204(13) 0.9576(7) 0.137(5) Uani 1 1 d . U . . .
C22 C 0.2184(18) -0.0617(12) 0.9166(7) 0.147(4) Uani 1 1 d . U . . .
C23 C 0.019(2) 0.0463(13) 0.9539(7) 0.143(6) Uani 1 1 d . U . . .
H23 H 0.027257 0.076951 0.923708 0.172 Uiso 1 1 calc R . . . .
C24 C 0.3588(19) -0.0201(13) 0.9122(7) 0.160(6) Uani 1 1 d . U . . .
C25 C 0.343(2) 0.0377(13) 0.8799(8) 0.193(8) Uani 1 1 d . U . . .
H25 H 0.257591 0.047870 0.856168 0.232 Uiso 1 1 calc R . . . .
C26 C 0.454(2) 0.0868(13) 0.8800(10) 0.207(8) Uani 1 1 d D U . . .
C27 C 0.598(2) 0.0561(15) 0.9034(8) 0.197(8) Uani 1 1 d . U . . .
H27 H 0.684685 0.078612 0.897317 0.237 Uiso 1 1 calc R . . . .
C28 C 0.616(2) -0.0053(14) 0.9346(7) 0.168(7) Uani 1 1 d . U . . .
H28 H 0.709727 -0.020465 0.953849 0.202 Uiso 1 1 calc R . . . .
C29 C 0.5012(18) -0.0470(13) 0.9394(6) 0.149(6) Uani 1 1 d . U . . .
H29 H 0.517449 -0.091189 0.959859 0.179 Uiso 1 1 calc R . . . .
C30 C 0.415(2) 0.1712(12) 0.8592(9) 0.204(8) Uani 1 1 d D U . . .
H30A H 0.306181 0.195060 0.868621 0.245 Uiso 1 1 calc R . . . .
H30B H 0.488047 0.198710 0.873739 0.245 Uiso 1 1 calc R . . . .
C31 C 0.436(4) 0.1645(15) 0.8012(9) 0.259(11) Uani 1 1 d D U . . .
H31A H 0.545676 0.141026 0.793555 0.311 Uiso 1 1 calc R . . . .
H31B H 0.368581 0.132385 0.788947 0.311 Uiso 1 1 calc R . . . .
C32 C 0.398(5) 0.2341(17) 0.7707(10) 0.311(14) Uani 1 1 d D U . . .
H32A H 0.289877 0.256613 0.781495 0.374 Uiso 1 1 calc R . . . .
H32B H 0.465774 0.264507 0.785212 0.374 Uiso 1 1 calc R . . . .
C33 C 0.404(5) 0.2460(16) 0.7136(10) 0.307(14) Uani 1 1 d D U . . .
H33A H 0.508514 0.221796 0.700033 0.368 Uiso 1 1 calc R . . . .
H33B H 0.325056 0.223737 0.697110 0.368 Uiso 1 1 calc R . . . .
C34 C 0.377(5) 0.3224(17) 0.6982(14) 0.322(16) Uani 1 1 d D U . . .
H34A H 0.261468 0.339029 0.697883 0.386 Uiso 1 1 calc R . . . .
H34B H 0.413770 0.346537 0.727983 0.386 Uiso 1 1 calc R . . . .
C35 C 0.433(4) 0.3536(17) 0.6514(14) 0.37(2) Uani 1 1 d D U . . .
H35A H 0.396124 0.406357 0.651100 0.559 Uiso 1 1 calc R . . . .
H35B H 0.547152 0.341775 0.650704 0.559 Uiso 1 1 calc R . . . .
H35C H 0.393137 0.334182 0.620265 0.559 Uiso 1 1 calc R . . . .
C36 C 0.160(2) -0.0732(12) 0.8641(8) 0.151(5) Uani 1 1 d . U . . .
C37 C -0.0037(19) -0.0718(10) 0.8575(8) 0.133(5) Uani 1 1 d . U . . .
H37 H -0.076331 -0.056742 0.885380 0.160 Uiso 1 1 calc R . . . .
C38 C -0.054(2) -0.0925(12) 0.8101(11) 0.158(6) Uani 1 1 d D U . . .
C39 C 0.053(3) -0.1139(12) 0.7703(9) 0.161(6) Uani 1 1 d . U . . .
H39 H 0.019423 -0.129621 0.738057 0.193 Uiso 1 1 calc R . . . .
C40 C 0.206(3) -0.1128(14) 0.7766(8) 0.177(7) Uani 1 1 d . U . . .
H40 H 0.272442 -0.121584 0.746364 0.212 Uiso 1 1 calc R . . . .
C41 C 0.268(2) -0.1009(13) 0.8197(8) 0.171(7) Uani 1 1 d . U . . .
H41 H 0.378295 -0.109361 0.823374 0.205 Uiso 1 1 calc R . . . .
C42 C -0.232(2) -0.0911(12) 0.7986(11) 0.196(8) Uani 1 1 d D U . . .
H42A H -0.244661 -0.138400 0.785597 0.236 Uiso 1 1 calc R . . . .
H42B H -0.296712 -0.080639 0.831172 0.236 Uiso 1 1 calc R . . . .
C43 C -0.280(3) -0.0319(15) 0.7569(11) 0.255(11) Uani 1 1 d D U . . .
H43A H -0.301537 0.013823 0.776205 0.306 Uiso 1 1 calc R . . . .
H43B H -0.184873 -0.031273 0.735169 0.306 Uiso 1 1 calc R . . . .
C44 C -0.404(4) -0.0247(15) 0.7198(14) 0.341(15) Uani 1 1 d D U . . .
H44A H -0.490753 -0.040264 0.739834 0.410 Uiso 1 1 calc R . . . .
H44B H -0.366942 -0.062633 0.693783 0.410 Uiso 1 1 calc R . . . .
C45 C -0.478(4) 0.0389(18) 0.6883(14) 0.390(18) Uani 1 1 d D U . . .
H45A H -0.433460 0.033974 0.651956 0.468 Uiso 1 1 calc R . . . .
H45B H -0.448594 0.081775 0.703148 0.468 Uiso 1 1 calc R . . . .
C46 C -0.652(4) 0.0545(19) 0.6839(13) 0.44(2) Uani 1 1 d D U . . .
H46A H -0.682584 0.007565 0.691520 0.524 Uiso 1 1 calc R . . . .
H46B H -0.691318 0.085305 0.714136 0.524 Uiso 1 1 calc R . . . .
C47 C -0.744(5) 0.087(2) 0.6390(16) 0.52(3) Uani 1 1 d D U . . .
H47A H -0.855295 0.090716 0.647508 0.780 Uiso 1 1 calc R . . . .
H47B H -0.724229 0.135648 0.631057 0.780 Uiso 1 1 calc R . . . .
H47C H -0.715392 0.056986 0.608173 0.780 Uiso 1 1 calc R . . . .
Cl11 Cl -0.2143(8) 0.2405(4) 0.8243(3) 0.203(3) Uani 1 1 d . U . . .
Cl12 Cl -0.0638(12) 0.2318(5) 0.7236(3) 0.272(5) Uani 1 1 d . U . . .
Cl13 Cl -0.0247(9) 0.1081(4) 0.7953(3) 0.205(3) Uani 1 1 d . U . . .
C101 C -0.061(3) 0.2000(13) 0.7851(10) 0.211(11) Uani 1 1 d . U . . .
H101 H 0.032087 0.214586 0.800488 0.253 Uiso 1 1 calc R . . . .


_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
S51 O51 2.666(8) . ?
S51 C64 1.741(15) . ?
S51 C67 1.725(12) . ?
S52 C66 1.730(13) . ?
S52 C69 1.728(15) . ?
O51 C51 1.220(13) . ?
N51 C61 1.173(17) . ?
N52 C62 1.122(13) . ?
C51 C52 1.474(17) . ?
C51 C55 1.510(16) . ?
C52 C53 1.449(15) . ?
C52 C63 1.363(16) . ?
C53 C54 1.487(17) . ?
C53 C60 1.313(17) . ?
C54 C55 1.401(16) . ?
C54 C59 1.420(15) . ?
C55 C56 1.343(17) . ?
C56 H56 0.9500 . ?
C56 C57 1.396(17) . ?
C57 H57 0.9500 . ?
C57 C58 1.382(17) . ?
C58 H58 0.9500 . ?
C58 C59 1.380(17) . ?
C59 H59 0.9500 . ?
C60 C61 1.44(2) . ?
C60 C62 1.478(16) . ?
C63 H63 0.9500 . ?
C63 C64 1.455(15) . ?
C64 C65 1.368(18) . ?
C65 H65 0.9500 . ?
C65 C66 1.395(15) . ?
C66 C67 1.368(18) . ?
C67 C68 1.456(15) . ?
C68 C69 1.358(18) . ?
C68 C72 1.488(19) . ?
C69 C70 1.460(16) . ?
C70 C71 1.389(18) . ?
C70 C73 1.402(18) . ?
C71 C72 1.511(16) . ?
C71 C73 1.443(16) 2_566 ?
C72 C74 1.536(19) . ?
C72 C86 1.549(19) . ?
C73 H73 0.9500 . ?
C74 C75 1.38(2) . ?
C74 C79 1.37(2) . ?
C75 H75 0.9500 . ?
C75 C76 1.38(2) . ?
C76 C77 1.39(2) . ?
C76 C80 1.597(18) . ?
C77 H77 0.9500 . ?
C77 C78 1.32(2) . ?
C78 H78 0.9500 . ?
C78 C79 1.42(2) . ?
C79 H79 0.9500 . ?
C80 H80A 0.9900 . ?
C80 H80B 0.9900 . ?
C80 C81 1.493(13) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C81 C82 1.479(16) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C82 C83 1.521(18) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C83 C84 1.51(2) . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?
C84 C85 1.494(19) . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C86 C87 1.358(18) . ?
C86 C91 1.431(18) . ?
C87 H87 0.9500 . ?
C87 C88 1.39(2) . ?
C88 H88 0.9500 . ?
C88 C89 1.43(2) . ?
C88 C92 1.626(19) . ?
C89 H89 0.9500 . ?
C89 C90 1.42(2) . ?
C90 H90 0.9500 . ?
C90 C91 1.34(2) . ?
C90 C92A 1.60(2) . ?
C91 H91 0.9500 . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C92 C93 1.500(15) . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
C93 C94 1.464(17) . ?
C94 H94A 0.9900 . ?
C94 H94B 0.9900 . ?
C94 C95 1.489(19) . ?
C95 H95A 0.9900 . ?
C95 H95B 0.9900 . ?
C95 C96 1.522(19) . ?
C96 H96A 0.9900 . ?
C96 H96B 0.9900 . ?
C96 C97 1.497(19) . ?
C97 H97A 0.9800 . ?
C97 H97B 0.9800 . ?
C97 H97C 0.9800 . ?
C92A H92C 0.9900 . ?
C92A H92D 0.9900 . ?
C92A C93A 1.478(19) . ?
C93A H93C 0.9900 . ?
C93A H93D 0.9900 . ?
C93A C94A 1.48(2) . ?
C94A H94C 0.9900 . ?
C94A H94D 0.9900 . ?
C94A C95A 1.49(2) . ?
C95A H95C 0.9900 . ?
C95A H95D 0.9900 . ?
C95A C96A 1.48(2) . ?
C96A H96C 0.9900 . ?
C96A H96D 0.9900 . ?
C96A C97A 1.49(2) . ?
C97A H97D 0.9800 . ?
C97A H97E 0.9800 . ?
C97A H97F 0.9800 . ?
S1 O1 2.687(17) . ?
S1 C14 1.75(2) . ?
S1 C17 1.68(2) . ?
S2 C16 1.81(2) . ?
S2 C19 1.69(2) . ?
O1 C1 1.21(2) . ?
N1 C11 1.103(18) . ?
N2 C12 1.14(3) . ?
C1 C2 1.51(2) . ?
C1 C5 1.55(3) . ?
C2 C3 1.53(3) . ?
C2 C13 1.31(3) . ?
C3 C4 1.51(2) . ?
C3 C10 1.39(3) . ?
C4 C5 1.42(3) . ?
C4 C9 1.39(3) . ?
C5 C6 1.39(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.34(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.39(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.37(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.50(2) . ?
C10 C12 1.39(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.40(3) . ?
C14 C15 1.43(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.30(3) . ?
C16 C17 1.35(2) . ?
C17 C18 1.37(3) . ?
C18 C19 1.43(2) . ?
C18 C22 1.61(3) . ?
C19 C20 1.49(3) . ?
C20 C21 1.43(2) . ?
C20 C23 1.47(3) 2_557 ?
C21 C22 1.58(3) . ?
C21 C23 1.30(3) . ?
C22 C24 1.59(2) . ?
C22 C36 1.47(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.32(2) . ?
C24 C29 1.42(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.48(2) . ?
C26 C27 1.40(3) . ?
C26 C30 1.628(19) . ?
C27 H27 0.9500 . ?
C27 C28 1.36(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.40(2) . ?
C29 H29 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.478(15) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.477(19) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.454(19) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.45(2) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.422(19) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.44(2) . ?
C36 C41 1.49(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.38(3) . ?
C38 C39 1.37(3) . ?
C38 C42 1.583(18) . ?
C39 H39 0.9500 . ?
C39 C40 1.36(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.28(3) . ?
C41 H41 0.9500 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.507(14) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.430(17) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.457(17) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.49(2) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.449(19) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
Cl11 C101 1.72(2) . ?
Cl12 C101 1.64(2) . ?
Cl13 C101 1.71(2) . ?
C101 H101 1.0000 . ?

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
C64 S51 O51 89.7(5) . . ?
C67 S51 O51 174.0(5) . . ?
C67 S51 C64 88.5(7) . . ?
C69 S52 C66 88.9(7) . . ?
C51 O51 S51 114.8(8) . . ?
O51 C51 C52 127.7(11) . . ?
O51 C51 C55 125.5(13) . . ?
C52 C51 C55 106.7(10) . . ?
C53 C52 C51 109.5(10) . . ?
C63 C52 C51 124.7(10) . . ?
C63 C52 C53 125.8(13) . . ?
C52 C53 C54 105.3(11) . . ?
C60 C53 C52 130.2(13) . . ?
C60 C53 C54 124.5(11) . . ?
C55 C54 C53 111.9(10) . . ?
C55 C54 C59 116.3(12) . . ?
C59 C54 C53 131.8(11) . . ?
C54 C55 C51 106.6(12) . . ?
C56 C55 C51 127.7(12) . . ?
C56 C55 C54 125.6(11) . . ?
C55 C56 H56 121.8 . . ?
C55 C56 C57 116.3(13) . . ?
C57 C56 H56 121.8 . . ?
C56 C57 H57 119.2 . . ?
C58 C57 C56 121.6(14) . . ?
C58 C57 H57 119.2 . . ?
C57 C58 H58 119.6 . . ?
C59 C58 C57 120.8(12) . . ?
C59 C58 H58 119.6 . . ?
C54 C59 H59 120.4 . . ?
C58 C59 C54 119.3(12) . . ?
C58 C59 H59 120.4 . . ?
C53 C60 C61 126.3(11) . . ?
C53 C60 C62 127.3(13) . . ?
C61 C60 C62 106.3(11) . . ?
N51 C61 C60 175.6(14) . . ?
N52 C62 C60 178.3(16) . . ?
C52 C63 H63 112.3 . . ?
C52 C63 C64 135.5(14) . . ?
C64 C63 H63 112.3 . . ?
C63 C64 S51 126.1(11) . . ?
C65 C64 S51 113.6(9) . . ?
C65 C64 C63 120.3(13) . . ?
C64 C65 H65 124.1 . . ?
C64 C65 C66 111.8(14) . . ?
C66 C65 H65 124.1 . . ?
C65 C66 S52 135.2(13) . . ?
C67 C66 S52 112.6(9) . . ?
C67 C66 C65 112.1(12) . . ?
C66 C67 S51 113.9(9) . . ?
C66 C67 C68 113.9(11) . . ?
C68 C67 S51 132.1(12) . . ?
C67 C68 C72 140.1(13) . . ?
C69 C68 C67 107.6(13) . . ?
C69 C68 C72 112.3(10) . . ?
C68 C69 S52 116.9(9) . . ?
C68 C69 C70 109.7(13) . . ?
C70 C69 S52 133.1(12) . . ?
C71 C70 C69 105.4(11) . . ?
C71 C70 C73 123.3(11) . . ?
C73 C70 C69 131.3(15) . . ?
C70 C71 C72 112.8(11) . . ?
C70 C71 C73 120.3(11) . 2_566 ?
C73 C71 C72 126.6(14) 2_566 . ?
C68 C72 C71 99.6(12) . . ?
C68 C72 C74 111.8(11) . . ?
C68 C72 C86 107.9(11) . . ?
C71 C72 C74 111.2(10) . . ?
C71 C72 C86 113.8(10) . . ?
C74 C72 C86 111.9(12) . . ?
C70 C73 C71 116.4(12) . 2_566 ?
C70 C73 H73 121.8 . . ?
C71 C73 H73 121.8 2_566 . ?
C75 C74 C72 117.6(13) . . ?
C79 C74 C72 124.0(15) . . ?
C79 C74 C75 118.3(15) . . ?
C74 C75 H75 119.4 . . ?
C76 C75 C74 121.2(16) . . ?
C76 C75 H75 119.4 . . ?
C75 C76 C77 118.7(18) . . ?
C75 C76 C80 120.0(18) . . ?
C77 C76 C80 121.3(18) . . ?
C76 C77 H77 119.0 . . ?
C78 C77 C76 122.0(19) . . ?
C78 C77 H77 119.0 . . ?
C77 C78 H78 120.6 . . ?
C77 C78 C79 118.9(18) . . ?
C79 C78 H78 120.6 . . ?
C74 C79 C78 120.8(17) . . ?
C74 C79 H79 119.6 . . ?
C78 C79 H79 119.6 . . ?
C76 C80 H80A 110.5 . . ?
C76 C80 H80B 110.5 . . ?
H80A C80 H80B 108.7 . . ?
C81 C80 C76 106(2) . . ?
C81 C80 H80A 110.5 . . ?
C81 C80 H80B 110.5 . . ?
C80 C81 H81A 99.8 . . ?
C80 C81 H81B 99.8 . . ?
H81A C81 H81B 104.1 . . ?
C82 C81 C80 148(3) . . ?
C82 C81 H81A 99.8 . . ?
C82 C81 H81B 99.8 . . ?
C81 C82 H82A 106.3 . . ?
C81 C82 H82B 106.3 . . ?
C81 C82 C83 124(3) . . ?
H82A C82 H82B 106.4 . . ?
C83 C82 H82A 106.3 . . ?
C83 C82 H82B 106.3 . . ?
C82 C83 H83A 105.9 . . ?
C82 C83 H83B 105.9 . . ?
H83A C83 H83B 106.3 . . ?
C84 C83 C82 126(3) . . ?
C84 C83 H83A 105.9 . . ?
C84 C83 H83B 105.9 . . ?
C83 C84 H84A 105.4 . . ?
C83 C84 H84B 105.4 . . ?
H84A C84 H84B 106.0 . . ?
C85 C84 C83 128(3) . . ?
C85 C84 H84A 105.4 . . ?
C85 C84 H84B 105.4 . . ?
C84 C85 H85A 109.5 . . ?
C84 C85 H85B 109.5 . . ?
C84 C85 H85C 109.5 . . ?
H85A C85 H85B 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
C87 C86 C72 123.7(12) . . ?
C87 C86 C91 118.8(14) . . ?
C91 C86 C72 117.3(12) . . ?
C86 C87 H87 118.9 . . ?
C86 C87 C88 122.1(14) . . ?
C88 C87 H87 118.9 . . ?
C87 C88 H88 120.8 . . ?
C87 C88 C89 118.5(15) . . ?
C87 C88 C92 126.4(16) . . ?
C89 C88 H88 120.8 . . ?
C89 C88 C92 115.0(17) . . ?
C88 C89 H89 120.4 . . ?
C90 C89 C88 119.3(17) . . ?
C90 C89 H89 120.4 . . ?
C89 C90 H90 120.2 . . ?
C89 C90 C92A 132(2) . . ?
C91 C90 C89 119.6(15) . . ?
C91 C90 H90 120.2 . . ?
C91 C90 C92A 107.9(18) . . ?
C86 C91 H91 119.3 . . ?
C90 C91 C86 121.5(15) . . ?
C90 C91 H91 119.3 . . ?
C88 C92 H92A 109.7 . . ?
C88 C92 H92B 109.7 . . ?
H92A C92 H92B 108.2 . . ?
C93 C92 C88 109.8(19) . . ?
C93 C92 H92A 109.7 . . ?
C93 C92 H92B 109.7 . . ?
C92 C93 H93A 106.8 . . ?
C92 C93 H93B 106.8 . . ?
H93A C93 H93B 106.6 . . ?
C94 C93 C92 122(3) . . ?
C94 C93 H93A 106.8 . . ?
C94 C93 H93B 106.8 . . ?
C93 C94 H94A 108.0 . . ?
C93 C94 H94B 108.0 . . ?
C93 C94 C95 117(2) . . ?
H94A C94 H94B 107.2 . . ?
C95 C94 H94A 108.0 . . ?
C95 C94 H94B 108.0 . . ?
C94 C95 H95A 109.9 . . ?
C94 C95 H95B 109.9 . . ?
C94 C95 C96 109(2) . . ?
H95A C95 H95B 108.3 . . ?
C96 C95 H95A 109.9 . . ?
C96 C95 H95B 109.9 . . ?
C95 C96 H96A 109.8 . . ?
C95 C96 H96B 109.8 . . ?
H96A C96 H96B 108.2 . . ?
C97 C96 C95 110(2) . . ?
C97 C96 H96A 109.8 . . ?
C97 C96 H96B 109.8 . . ?
C96 C97 H97A 109.5 . . ?
C96 C97 H97B 109.5 . . ?
C96 C97 H97C 109.5 . . ?
H97A C97 H97B 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 109.5 . . ?
C90 C92A H92C 106.1 . . ?
C90 C92A H92D 106.1 . . ?
H92C C92A H92D 106.3 . . ?
C93A C92A C90 125(2) . . ?
C93A C92A H92C 106.1 . . ?
C93A C92A H92D 106.1 . . ?
C92A C93A H93C 106.8 . . ?
C92A C93A H93D 106.8 . . ?
H93C C93A H93D 106.6 . . ?
C94A C93A C92A 122(3) . . ?
C94A C93A H93C 106.8 . . ?
C94A C93A H93D 106.8 . . ?
C93A C94A H94C 107.8 . . ?
C93A C94A H94D 107.8 . . ?
C93A C94A C95A 118(3) . . ?
H94C C94A H94D 107.1 . . ?
C95A C94A H94C 107.8 . . ?
C95A C94A H94D 107.8 . . ?
C94A C95A H95C 107.4 . . ?
C94A C95A H95D 107.4 . . ?
H95C C95A H95D 106.9 . . ?
C96A C95A C94A 120(3) . . ?
C96A C95A H95C 107.4 . . ?
C96A C95A H95D 107.4 . . ?
C95A C96A H96C 107.6 . . ?
C95A C96A H96D 107.6 . . ?
C95A C96A C97A 119(3) . . ?
H96C C96A H96D 107.0 . . ?
C97A C96A H96C 107.6 . . ?
C97A C96A H96D 107.6 . . ?
C96A C97A H97D 109.5 . . ?
C96A C97A H97E 109.5 . . ?
C96A C97A H97F 109.5 . . ?
H97D C97A H97E 109.5 . . ?
H97D C97A H97F 109.5 . . ?
H97E C97A H97F 109.5 . . ?
C14 S1 O1 89.8(9) . . ?
C17 S1 O1 177.9(8) . . ?
C17 S1 C14 88.4(11) . . ?
C19 S2 C16 89.6(10) . . ?
C1 O1 S1 115.0(13) . . ?
O1 C1 C2 126(2) . . ?
O1 C1 C5 128(2) . . ?
C2 C1 C5 107(2) . . ?
C1 C2 C3 105(2) . . ?
C13 C2 C1 126(2) . . ?
C13 C2 C3 128.8(19) . . ?
C4 C3 C2 109(2) . . ?
C10 C3 C2 129(2) . . ?
C10 C3 C4 121(2) . . ?
C5 C4 C3 108(2) . . ?
C9 C4 C3 135(2) . . ?
C9 C4 C5 116.7(19) . . ?
C4 C5 C1 110.5(18) . . ?
C6 C5 C1 126(2) . . ?
C6 C5 C4 124(2) . . ?
C5 C6 H6 121.1 . . ?
C7 C6 C5 118(3) . . ?
C7 C6 H6 121.1 . . ?
C6 C7 H7 120.0 . . ?
C6 C7 C8 120(2) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 H8 118.3 . . ?
C9 C8 C7 123(3) . . ?
C9 C8 H8 118.3 . . ?
C4 C9 H9 120.7 . . ?
C8 C9 C4 119(3) . . ?
C8 C9 H9 120.7 . . ?
C3 C10 C11 123(2) . . ?
C3 C10 C12 129(2) . . ?
C12 C10 C11 107.8(19) . . ?
N1 C11 C10 179(2) . . ?
N2 C12 C10 173(2) . . ?
C2 C13 H13 110.9 . . ?
C2 C13 C14 138(2) . . ?
C14 C13 H13 110.9 . . ?
C13 C14 S1 125.6(15) . . ?
C13 C14 C15 123(2) . . ?
C15 C14 S1 111.4(19) . . ?
C14 C15 H15 125.1 . . ?
C16 C15 C14 110(2) . . ?
C16 C15 H15 125.1 . . ?
C15 C16 S2 131.5(16) . . ?
C15 C16 C17 117(2) . . ?
C17 C16 S2 111(2) . . ?
C16 C17 S1 113(2) . . ?
C16 C17 C18 114(2) . . ?
C18 C17 S1 132.4(16) . . ?
C17 C18 C19 112.2(19) . . ?
C17 C18 C22 141.1(18) . . ?
C19 C18 C22 107(2) . . ?
C18 C19 S2 112.5(19) . . ?
C18 C19 C20 110.5(17) . . ?
C20 C19 S2 136.9(15) . . ?
C21 C20 C19 112(2) . . ?
C21 C20 C23 119(2) . 2_557 ?
C23 C20 C19 129.1(17) 2_557 . ?
C20 C21 C22 107(2) . . ?
C23 C21 C20 126(2) . . ?
C23 C21 C22 127.5(17) . . ?
C21 C22 C18 104.2(14) . . ?
C21 C22 C24 107.2(17) . . ?
C24 C22 C18 111.4(13) . . ?
C36 C22 C18 105.3(18) . . ?
C36 C22 C21 116.9(15) . . ?
C36 C22 C24 111.7(13) . . ?
C20 C23 H23 122.4 2_557 . ?
C21 C23 C20 115.3(19) . 2_557 ?
C21 C23 H23 122.4 . . ?
C25 C24 C22 117.8(14) . . ?
C25 C24 C29 121.2(14) . . ?
C29 C24 C22 120.9(16) . . ?
C24 C25 H25 119.3 . . ?
C24 C25 C26 121.4(16) . . ?
C26 C25 H25 119.3 . . ?
C25 C26 C30 124.5(17) . . ?
C27 C26 C25 114.1(19) . . ?
C27 C26 C30 121.2(17) . . ?
C26 C27 H27 119.3 . . ?
C28 C27 C26 121.3(15) . . ?
C28 C27 H27 119.3 . . ?
C27 C28 H28 118.7 . . ?
C27 C28 C29 122.5(17) . . ?
C29 C28 H28 118.7 . . ?
C24 C29 H29 121.6 . . ?
C28 C29 C24 116.8(18) . . ?
C28 C29 H29 121.6 . . ?
C26 C30 H30A 111.4 . . ?
C26 C30 H30B 111.4 . . ?
H30A C30 H30B 109.3 . . ?
C31 C30 C26 101.9(19) . . ?
C31 C30 H30A 111.4 . . ?
C31 C30 H30B 111.4 . . ?
C30 C31 H31A 108.7 . . ?
C30 C31 H31B 108.7 . . ?
H31A C31 H31B 107.6 . . ?
C32 C31 C30 114(2) . . ?
C32 C31 H31A 108.7 . . ?
C32 C31 H31B 108.7 . . ?
C31 C32 H32A 105.3 . . ?
C31 C32 H32B 105.3 . . ?
H32A C32 H32B 106.0 . . ?
C33 C32 C31 128(3) . . ?
C33 C32 H32A 105.3 . . ?
C33 C32 H32B 105.3 . . ?
C32 C33 H33A 109.1 . . ?
C32 C33 H33B 109.1 . . ?
H33A C33 H33B 107.9 . . ?
C34 C33 C32 112(3) . . ?
C34 C33 H33A 109.1 . . ?
C34 C33 H33B 109.1 . . ?
C33 C34 H34A 105.6 . . ?
C33 C34 H34B 105.6 . . ?
H34A C34 H34B 106.1 . . ?
C35 C34 C33 127(3) . . ?
C35 C34 H34A 105.6 . . ?
C35 C34 H34B 105.6 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C22 C36 C41 121.6(16) . . ?
C37 C36 C22 120.0(18) . . ?
C37 C36 C41 117.3(18) . . ?
C36 C37 H37 120.2 . . ?
C38 C37 C36 120(2) . . ?
C38 C37 H37 120.2 . . ?
C37 C38 C42 123(2) . . ?
C39 C38 C37 119.1(18) . . ?
C39 C38 C42 118(2) . . ?
C38 C39 H39 119.7 . . ?
C40 C39 C38 121(2) . . ?
C40 C39 H39 119.7 . . ?
C39 C40 H40 117.2 . . ?
C41 C40 C39 126(2) . . ?
C41 C40 H40 117.2 . . ?
C36 C41 H41 121.6 . . ?
C40 C41 C36 117(2) . . ?
C40 C41 H41 121.6 . . ?
C38 C42 H42A 110.6 . . ?
C38 C42 H42B 110.6 . . ?
H42A C42 H42B 108.7 . . ?
C43 C42 C38 105.8(17) . . ?
C43 C42 H42A 110.6 . . ?
C43 C42 H42B 110.6 . . ?
C42 C43 H43A 105.4 . . ?
C42 C43 H43B 105.4 . . ?
H43A C43 H43B 106.0 . . ?
C44 C43 C42 128(3) . . ?
C44 C43 H43A 105.4 . . ?
C44 C43 H43B 105.4 . . ?
C43 C44 H44A 105.0 . . ?
C43 C44 H44B 105.0 . . ?
C43 C44 C45 129(2) . . ?
H44A C44 H44B 105.9 . . ?
C45 C44 H44A 105.0 . . ?
C45 C44 H44B 105.0 . . ?
C44 C45 H45A 107.8 . . ?
C44 C45 H45B 107.8 . . ?
C44 C45 C46 118(3) . . ?
H45A C45 H45B 107.1 . . ?
C46 C45 H45A 107.8 . . ?
C46 C45 H45B 107.8 . . ?
C45 C46 H46A 105.4 . . ?
C45 C46 H46B 105.4 . . ?
H46A C46 H46B 106.0 . . ?
C47 C46 C45 128(3) . . ?
C47 C46 H46A 105.4 . . ?
C47 C46 H46B 105.4 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
Cl11 C101 H101 104.0 . . ?
Cl12 C101 Cl11 115.0(15) . . ?
Cl12 C101 Cl13 117.6(17) . . ?
Cl12 C101 H101 104.0 . . ?
Cl13 C101 Cl11 110.4(10) . . ?
Cl13 C101 H101 104.0 . . ?

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
S51 O51 C51 C52 -8.3(15) . . . . ?
S51 O51 C51 C55 170.8(9) . . . . ?
S51 C64 C65 C66 0.5(14) . . . . ?
S51 C67 C68 C69 -179.6(10) . . . . ?
S51 C67 C68 C72 1(2) . . . . ?
S52 C66 C67 S51 -179.3(7) . . . . ?
S52 C66 C67 C68 -1.2(15) . . . . ?
S52 C69 C70 C71 -176.9(11) . . . . ?
S52 C69 C70 C73 3(2) . . . . ?
O51 S51 C64 C63 -10.4(10) . . . . ?
O51 S51 C64 C65 172.9(9) . . . . ?
O51 C51 C52 C53 178.7(11) . . . . ?
O51 C51 C52 C63 1(2) . . . . ?
O51 C51 C55 C54 179.7(11) . . . . ?
O51 C51 C55 C56 3(2) . . . . ?
C51 C52 C53 C54 1.8(12) . . . . ?
C51 C52 C53 C60 -177.2(12) . . . . ?
C51 C52 C63 C64 3(2) . . . . ?
C51 C55 C56 C57 179.1(11) . . . . ?
C52 C51 C55 C54 -1.0(12) . . . . ?
C52 C51 C55 C56 -177.7(12) . . . . ?
C52 C53 C54 C55 -2.6(12) . . . . ?
C52 C53 C54 C59 179.8(11) . . . . ?
C52 C53 C60 C61 -3(2) . . . . ?
C52 C53 C60 C62 173.7(11) . . . . ?
C52 C63 C64 S51 7(2) . . . . ?
C52 C63 C64 C65 -176.7(14) . . . . ?
C53 C52 C63 C64 -174.7(12) . . . . ?
C53 C54 C55 C51 2.2(12) . . . . ?
C53 C54 C55 C56 179.0(12) . . . . ?
C53 C54 C59 C58 179.9(11) . . . . ?
C54 C53 C60 C61 177.8(12) . . . . ?
C54 C53 C60 C62 -5(2) . . . . ?
C54 C55 C56 C57 3.0(19) . . . . ?
C55 C51 C52 C53 -0.6(12) . . . . ?
C55 C51 C52 C63 -178.4(11) . . . . ?
C55 C54 C59 C58 2.4(16) . . . . ?
C55 C56 C57 C58 -2.5(19) . . . . ?
C56 C57 C58 C59 2.2(19) . . . . ?
C57 C58 C59 C54 -2.1(18) . . . . ?
C59 C54 C55 C51 -179.8(10) . . . . ?
C59 C54 C55 C56 -3.0(17) . . . . ?
C60 C53 C54 C55 176.6(11) . . . . ?
C60 C53 C54 C59 -1(2) . . . . ?
C63 C52 C53 C54 179.6(11) . . . . ?
C63 C52 C53 C60 1(2) . . . . ?
C63 C64 C65 C66 -176.4(11) . . . . ?
C64 S51 C67 C66 2.0(11) . . . . ?
C64 S51 C67 C68 -175.7(12) . . . . ?
C64 C65 C66 S52 177.4(12) . . . . ?
C64 C65 C66 C67 1.0(17) . . . . ?
C65 C66 C67 S51 -2.1(15) . . . . ?
C65 C66 C67 C68 176.0(11) . . . . ?
C66 S52 C69 C68 2.2(11) . . . . ?
C66 S52 C69 C70 175.8(14) . . . . ?
C66 C67 C68 C69 2.7(16) . . . . ?
C66 C67 C68 C72 -176.9(15) . . . . ?
C67 S51 C64 C63 175.3(11) . . . . ?
C67 S51 C64 C65 -1.4(10) . . . . ?
C67 C68 C69 S52 -3.1(14) . . . . ?
C67 C68 C69 C70 -178.2(10) . . . . ?
C67 C68 C72 C71 180.0(15) . . . . ?
C67 C68 C72 C74 63(2) . . . . ?
C67 C68 C72 C86 -61.0(19) . . . . ?
C68 C69 C70 C71 -3.0(15) . . . . ?
C68 C69 C70 C73 177.5(14) . . . . ?
C68 C72 C74 C75 -169.8(12) . . . . ?
C68 C72 C74 C79 12.3(17) . . . . ?
C68 C72 C86 C87 -96.2(14) . . . . ?
C68 C72 C86 C91 79.2(15) . . . . ?
C69 S52 C66 C65 -176.8(15) . . . . ?
C69 S52 C66 C67 -0.4(11) . . . . ?
C69 C68 C72 C71 0.5(14) . . . . ?
C69 C68 C72 C74 -117.0(12) . . . . ?
C69 C68 C72 C86 119.5(12) . . . . ?
C69 C70 C71 C72 3.4(16) . . . . ?
C69 C70 C71 C73 178.1(11) . . . 2_566 ?
C69 C70 C73 C71 -178.3(13) . . . 2_566 ?
C70 C71 C72 C68 -2.5(15) . . . . ?
C70 C71 C72 C74 115.5(14) . . . . ?
C70 C71 C72 C86 -117.0(14) . . . . ?
C71 C70 C73 C71 2(2) . . . 2_566 ?
C71 C72 C74 C75 80.0(16) . . . . ?
C71 C72 C74 C79 -98.0(15) . . . . ?
C71 C72 C86 C87 13(2) . . . . ?
C71 C72 C86 C91 -171.3(13) . . . . ?
C72 C68 C69 S52 176.6(9) . . . . ?
C72 C68 C69 C70 1.5(16) . . . . ?
C72 C74 C75 C76 -177.4(12) . . . . ?
C72 C74 C79 C78 177.8(12) . . . . ?
C72 C86 C87 C88 175.7(15) . . . . ?
C72 C86 C91 C90 -179.3(15) . . . . ?
C73 C70 C71 C72 -177.0(13) . . . . ?
C73 C70 C71 C73 -2(2) . . . 2_566 ?
C73 C71 C72 C68 -176.8(12) 2_566 . . . ?
C73 C71 C72 C74 -58.8(18) 2_566 . . . ?
C73 C71 C72 C86 68.6(17) 2_566 . . . ?
C74 C72 C86 C87 140.4(13) . . . . ?
C74 C72 C86 C91 -44.2(16) . . . . ?
C74 C75 C76 C77 1(2) . . . . ?
C74 C75 C76 C80 179.7(15) . . . . ?
C75 C74 C79 C78 -0.1(19) . . . . ?
C75 C76 C77 C78 -3(2) . . . . ?
C75 C76 C80 C81 160(2) . . . . ?
C76 C77 C78 C79 4(2) . . . . ?
C76 C80 C81 C82 -162(7) . . . . ?
C77 C76 C80 C81 -21(3) . . . . ?
C77 C78 C79 C74 -2(2) . . . . ?
C79 C74 C75 C76 1(2) . . . . ?
C80 C76 C77 C78 177.9(16) . . . . ?
C80 C81 C82 C83 158(6) . . . . ?
C81 C82 C83 C84 -119(5) . . . . ?
C82 C83 C84 C85 -165(4) . . . . ?
C86 C72 C74 C75 -48.5(14) . . . . ?
C86 C72 C74 C79 133.5(13) . . . . ?
C86 C87 C88 C89 3(3) . . . . ?
C86 C87 C88 C92 -172.2(19) . . . . ?
C87 C86 C91 C90 -4(2) . . . . ?
C87 C88 C89 C90 -4(3) . . . . ?
C87 C88 C92 C93 -114(3) . . . . ?
C88 C89 C90 C91 1(3) . . . . ?
C88 C89 C90 C92A 172(3) . . . . ?
C88 C92 C93 C94 158(2) . . . . ?
C89 C88 C92 C93 70(3) . . . . ?
C89 C90 C91 C86 3(3) . . . . ?
C89 C90 C92A C93A -133(3) . . . . ?
C90 C92A C93A C94A 71(6) . . . . ?
C91 C86 C87 C88 0(2) . . . . ?
C91 C90 C92A C93A 38(4) . . . . ?
C92 C88 C89 C90 172.2(19) . . . . ?
C92 C93 C94 C95 130(3) . . . . ?
C93 C94 C95 C96 -105(4) . . . . ?
C94 C95 C96 C97 58(3) . . . . ?
C92A C90 C91 C86 -170(2) . . . . ?
C92A C93A C94A C95A 149(4) . . . . ?
C93A C94A C95A C96A -77(7) . . . . ?
C94A C95A C96A C97A -136(6) . . . . ?
S1 O1 C1 C2 -1(2) . . . . ?
S1 O1 C1 C5 -176.8(13) . . . . ?
S1 C14 C15 C16 4.7(19) . . . . ?
S1 C17 C18 C19 -178.1(11) . . . . ?
S1 C17 C18 C22 -1(4) . . . . ?
S2 C16 C17 S1 177.7(8) . . . . ?
S2 C16 C17 C18 -6(2) . . . . ?
S2 C19 C20 C21 -177.9(13) . . . . ?
S2 C19 C20 C23 7(3) . . . 2_557 ?
O1 S1 C14 C13 -2.3(15) . . . . ?
O1 S1 C14 C15 176.7(11) . . . . ?
O1 C1 C2 C3 -179.4(19) . . . . ?
O1 C1 C2 C13 0(3) . . . . ?
O1 C1 C5 C4 177.5(19) . . . . ?
O1 C1 C5 C6 0(3) . . . . ?
C1 C2 C3 C4 3.7(17) . . . . ?
C1 C2 C3 C10 -177.4(15) . . . . ?
C1 C2 C13 C14 0(3) . . . . ?
C1 C5 C6 C7 179.2(17) . . . . ?
C2 C1 C5 C4 1.1(19) . . . . ?
C2 C1 C5 C6 -176.6(15) . . . . ?
C2 C3 C4 C5 -3.2(18) . . . . ?
C2 C3 C4 C9 177(2) . . . . ?
C2 C3 C10 C11 4(3) . . . . ?
C2 C3 C10 C12 175.5(19) . . . . ?
C2 C13 C14 S1 2(3) . . . . ?
C2 C13 C14 C15 -176.6(17) . . . . ?
C3 C2 C13 C14 179.0(19) . . . . ?
C3 C4 C5 C1 1.3(19) . . . . ?
C3 C4 C5 C6 179.0(15) . . . . ?
C3 C4 C9 C8 -180.0(17) . . . . ?
C4 C3 C10 C11 -177.7(14) . . . . ?
C4 C3 C10 C12 -6(3) . . . . ?
C4 C5 C6 C7 2(3) . . . . ?
C5 C1 C2 C3 -2.9(16) . . . . ?
C5 C1 C2 C13 176.4(15) . . . . ?
C5 C4 C9 C8 1(3) . . . . ?
C5 C6 C7 C8 -2(3) . . . . ?
C6 C7 C8 C9 1(3) . . . . ?
C7 C8 C9 C4 0(3) . . . . ?
C9 C4 C5 C1 -179.1(15) . . . . ?
C9 C4 C5 C6 -1(3) . . . . ?
C10 C3 C4 C5 177.9(15) . . . . ?
C10 C3 C4 C9 -2(3) . . . . ?
C13 C2 C3 C4 -175.5(15) . . . . ?
C13 C2 C3 C10 3(3) . . . . ?
C13 C14 C15 C16 -176.3(17) . . . . ?
C14 S1 C17 C16 -0.8(13) . . . . ?
C14 S1 C17 C18 -176.6(19) . . . . ?
C14 C15 C16 S2 -177.7(12) . . . . ?
C14 C15 C16 C17 -6(2) . . . . ?
C15 C16 C17 S1 4(2) . . . . ?
C15 C16 C17 C18 -179.4(18) . . . . ?
C16 S2 C19 C18 0.5(12) . . . . ?
C16 S2 C19 C20 177.2(18) . . . . ?
C16 C17 C18 C19 6(2) . . . . ?
C16 C17 C18 C22 -176.8(18) . . . . ?
C17 S1 C14 C13 178.8(16) . . . . ?
C17 S1 C14 C15 -2.2(12) . . . . ?
C17 C18 C19 S2 -3.7(19) . . . . ?
C17 C18 C19 C20 178.7(15) . . . . ?
C17 C18 C22 C21 -177(2) . . . . ?
C17 C18 C22 C24 -62(3) . . . . ?
C17 C18 C22 C36 59(3) . . . . ?
C18 C19 C20 C21 -1.1(19) . . . . ?
C18 C19 C20 C23 -176.5(15) . . . 2_557 ?
C18 C22 C24 C25 164(2) . . . . ?
C18 C22 C24 C29 -12(3) . . . . ?
C18 C22 C36 C37 93(2) . . . . ?
C18 C22 C36 C41 -75(2) . . . . ?
C19 S2 C16 C15 175(2) . . . . ?
C19 S2 C16 C17 2.9(13) . . . . ?
C19 C18 C22 C21 0.1(16) . . . . ?
C19 C18 C22 C24 115.3(16) . . . . ?
C19 C18 C22 C36 -123.5(15) . . . . ?
C19 C20 C21 C22 1.1(17) . . . . ?
C19 C20 C21 C23 -179.2(17) . . . . ?
C20 C21 C22 C18 -0.7(15) . . . . ?
C20 C21 C22 C24 -118.8(14) . . . . ?
C20 C21 C22 C36 114.9(16) . . . . ?
C20 C21 C23 C20 3(3) . . . 2_557 ?
C21 C22 C24 C25 -83(2) . . . . ?
C21 C22 C24 C29 101(2) . . . . ?
C21 C22 C36 C37 -22(3) . . . . ?
C21 C22 C36 C41 170.4(17) . . . . ?
C22 C18 C19 S2 178.2(10) . . . . ?
C22 C18 C19 C20 0.6(17) . . . . ?
C22 C21 C23 C20 -177.2(13) . . . 2_557 ?
C22 C24 C25 C26 169(2) . . . . ?
C22 C24 C29 C28 -178(2) . . . . ?
C22 C36 C37 C38 -171.0(19) . . . . ?
C22 C36 C41 C40 176(2) . . . . ?
C23 C20 C21 C22 177.1(13) 2_557 . . . ?
C23 C20 C21 C23 -3(3) 2_557 . . . ?
C23 C21 C22 C18 179.6(17) . . . . ?
C23 C21 C22 C24 62(2) . . . . ?
C23 C21 C22 C36 -65(3) . . . . ?
C24 C22 C36 C37 -146.1(18) . . . . ?
C24 C22 C36 C41 46(3) . . . . ?
C24 C25 C26 C27 19(4) . . . . ?
C24 C25 C26 C30 -157(2) . . . . ?
C25 C24 C29 C28 6(3) . . . . ?
C25 C26 C27 C28 -16(4) . . . . ?
C25 C26 C30 C31 -81(3) . . . . ?
C26 C27 C28 C29 9(4) . . . . ?
C26 C30 C31 C32 177(3) . . . . ?
C27 C26 C30 C31 103(3) . . . . ?
C27 C28 C29 C24 -3(3) . . . . ?
C29 C24 C25 C26 -15(4) . . . . ?
C30 C26 C27 C28 160(2) . . . . ?
C30 C31 C32 C33 -179(4) . . . . ?
C31 C32 C33 C34 -173(4) . . . . ?
C32 C33 C34 C35 153(4) . . . . ?
C36 C22 C24 C25 46(3) . . . . ?
C36 C22 C24 C29 -130(2) . . . . ?
C36 C37 C38 C39 0(3) . . . . ?
C36 C37 C38 C42 -178.6(17) . . . . ?
C37 C36 C41 C40 9(3) . . . . ?
C37 C38 C39 C40 -2(3) . . . . ?
C37 C38 C42 C43 112(2) . . . . ?
C38 C39 C40 C41 8(4) . . . . ?
C38 C42 C43 C44 156(3) . . . . ?
C39 C38 C42 C43 -67(3) . . . . ?
C39 C40 C41 C36 -12(4) . . . . ?
C41 C36 C37 C38 -3(3) . . . . ?
C42 C38 C39 C40 176.6(18) . . . . ?
C42 C43 C44 C45 163(4) . . . . ?
C43 C44 C45 C46 -137(4) . . . . ?
C44 C45 C46 C47 -147(4) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id 'Sample #21: m-ITIC'
_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 2.046
_oxdiff_exptl_absorpt_empirical_full_min 0.503



# start Validation Reply Form
_vrf_PLAT084_m-ITIC              
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.52 Report
RESPONSE: 
Poorly diffracting crystals, for which the modelling of the alkyl side-chains
was challenging and potentially inaccurate. However the data provides sufficient
information regarding the core of the structure.

;
# end Validation Reply Form



