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

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

data_2020jrh0001_res
_database_code_depnum_ccdc_archive 'CCDC 1997675'
loop_
_audit_author_name
_audit_author_address
'Jennifer Hiscock'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2020-04-17 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_audit_creation_date             2020-04-17
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C15 H12 N3 O4 S2), 4(C8 H18 N0.5), H2 O'
_chemical_formula_sum            'C62 H98 N8 O9 S4'
_chemical_formula_weight         1227.72
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H20N2O2S2
_chemical_oxdiff_usercomment     '100 K kira 1-15'
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           13
_space_group_name_H-M_alt        'P 1 2/n 1'
_space_group_name_Hall           '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   19.22676(16)
_cell_length_b                   13.73691(14)
_cell_length_c                   25.4779(2)
_cell_angle_alpha                90
_cell_angle_beta                 107.0098(10)
_cell_angle_gamma                90
_cell_volume                     6434.76(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    19085
_cell_measurement_temperature    148.47(10)
_cell_measurement_theta_max      72.8550
_cell_measurement_theta_min      3.6680
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.842
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2648
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 2 2 0.2510
5 -2 -2 0.2510
0 1 5 0.0411
0 -1 -5 0.0411
0 -1 0 0.0145
0 1 0 0.0145

_exptl_crystal_size_max          0.592
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.029
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.0065 1.9915 2.0071 0.0497 0.3906 0.2361
5.0065 -1.9915 -2.0071 -0.0497 -0.3906 -0.2361
-0.0054 0.9948 5.0087 0.0307 0.2173 -0.2539
0.0054 -0.9948 -5.0087 -0.0307 -0.2173 0.2539
0.0042 -0.9987 -0.0081 0.0846 -0.0734 -0.0028
-0.0042 0.9987 0.0081 -0.0846 0.0734 0.0028

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            42981
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.628
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      148.47(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -97.00 -18.00   1.00    8.00    --  -41.91 -57.00-150.00   79
  2  ω   -115.00 -16.00   1.00    8.00    --  -41.91 -47.00 -23.00   99
  3  ω    -66.00  32.00   1.00    8.00    --  -41.91  38.00 150.00   98
  4  ω    -68.00 -27.00   1.00    8.00    --  -41.91  57.00   0.00   41
  5  ω     38.00  81.00   1.00    8.00    --   41.91 -99.00 150.00   43
  6  ω     30.00 130.00   1.00   30.00    --  105.91 -77.00-180.00  100
  7  ω     81.00 173.00   1.00   30.00    --  105.91  45.00 -90.00   92
  8  ω     33.00  69.00   1.00   30.00    --  105.91-125.00  60.00   36
  9  ω     41.00 121.00   1.00   30.00    --  105.91-125.00-180.00   80
 10  ω     80.00 177.00   1.00   30.00    --  105.91  45.00   0.00   97
 11  ω     73.00 166.00   1.00   30.00    --  105.91  77.00 -60.00   93
 12  ω     35.00 115.00   1.00   30.00    --  105.91 -45.00   0.00   80
 13  ω     55.00 129.00   1.00   30.00    --  105.91 -77.00 -60.00   74
 14  ω     94.00 122.00   1.00   30.00    --  105.91 125.00-180.00   28
 15  ω     83.00 108.00   1.00   30.00    --  105.91 -94.00-120.00   25
 16  ω     90.00 115.00   1.00   30.00    --  105.91-125.00  60.00   25
 17  ω    151.00 178.00   1.00   30.00    --  105.91 125.00-150.00   27
 18  ω    134.00 166.00   1.00   30.00    --  105.91  45.00-120.00   32
 19  ω     81.00 117.00   1.00   30.00    --  105.91  45.00-120.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0345258000
_diffrn_orient_matrix_UB_12      -0.0850026000
_diffrn_orient_matrix_UB_13      0.0229839000
_diffrn_orient_matrix_UB_21      -0.0373770000
_diffrn_orient_matrix_UB_22      0.0731092000
_diffrn_orient_matrix_UB_23      0.0288191000
_diffrn_orient_matrix_UB_31      -0.0665801000
_diffrn_orient_matrix_UB_32      0.0029612000
_diffrn_orient_matrix_UB_33      -0.0513610000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9674
_reflns_number_total             11367
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         11367
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0379
_refine_ls_restrained_S_all      1.029
_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)+(0.0544P)²+2.0305P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1033
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O9(H9A,H9B)
2.b Secondary CH2 refined with riding coordinates:
 C60(H60A,H60B), C62(H62A,H62B), C58(H58A,H58B), C42(H42A,H42B), C50(H50A,
 H50B), C54(H54A,H54B), C48(H48A,H48B), C1(H1A,H1B), C38(H38A,H38B), C16(H16A,
 H16B), C34(H34A,H34B), C49(H49A,H49B), C41(H41A,H41B), C61(H61A,H61B),
 C46(H46A,H46B), C37(H37A,H37B), C40(H40A,H40B), C44(H44A,H44B), C45(H45A,H45B),
  C36(H36A,H36B), C56(H56A,H56B), C33(H33A,H33B), C57(H57A,H57B), C32(H32A,
 H32B), C52(H52A,H52B), C53(H53A,H53B)
2.c Aromatic/amide H refined with riding coordinates:
 N5(H5A), N2(H2), N1(H1), N4(H4A), C20(H20), C23(H23), C19(H19), C7(H7),
 C22(H22), C4(H4), C5(H5), C8(H8), C26(H26), C29(H29), C11(H11), C27(H27),
 C28(H28), C12(H12), C13(H13), C14(H14)
2.d Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C39(H39A,H39B,H39C), C47(H47A,H47B,H47C), C43(H43A,H43B,
 H43C), C55(H55A,H55B,H55C), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C), C51(H51A,
 H51B,H51C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.68156(2) 0.35542(3) 0.40397(2) 0.02067(10) Uani 1 1 d . . . . .
S3 S 0.84194(2) 0.33407(3) 0.60829(2) 0.01779(10) Uani 1 1 d . . . . .
S4 S 0.96683(2) -0.20065(3) 0.32445(2) 0.02040(10) Uani 1 1 d . . . . .
S2 S 0.52974(2) -0.22276(3) 0.65743(2) 0.02170(10) Uani 1 1 d . . . . .
O4 O 0.58273(6) 0.16507(9) 0.47739(5) 0.0213(3) Uani 1 1 d . . . . .
O5 O 0.77686(7) 0.39244(9) 0.58261(5) 0.0238(3) Uani 1 1 d . . . . .
O8 O 0.93407(6) 0.16054(10) 0.52529(5) 0.0241(3) Uani 1 1 d . . . . .
O6 O 0.88798(7) 0.37660(10) 0.65858(5) 0.0272(3) Uani 1 1 d . . . . .
O7 O 0.82229(7) 0.23277(9) 0.61327(5) 0.0252(3) Uani 1 1 d . . . . .
O3 O 0.74830(7) 0.40822(10) 0.43280(5) 0.0275(3) Uani 1 1 d . . . . .
O2 O 0.63494(7) 0.40965(11) 0.35845(5) 0.0304(3) Uani 1 1 d . . . . .
O1 O 0.69818(7) 0.25697(11) 0.39023(5) 0.0299(3) Uani 1 1 d . . . . .
N5 N 0.83919(8) 0.17238(11) 0.44585(6) 0.0196(3) Uani 1 1 d . . . . .
H5A H 0.7991 0.2030 0.4317 0.024 Uiso 1 1 calc R U . . .
N2 N 0.67847(8) 0.15745(11) 0.55664(6) 0.0190(3) Uani 1 1 d . . . . .
H2 H 0.7209 0.1815 0.5716 0.023 Uiso 1 1 calc R U . . .
N8 N 0.7500 -0.59093(15) 0.7500 0.0208(4) Uani 1 2 d S T P . .
N1 N 0.66512(8) 0.28907(11) 0.49957(6) 0.0204(3) Uani 1 1 d . . . . .
H1 H 0.7040 0.3109 0.5228 0.024 Uiso 1 1 calc R U . . .
N4 N 0.86073(8) 0.29452(11) 0.50944(6) 0.0221(3) Uani 1 1 d . . . . .
H4A H 0.8258 0.3248 0.4864 0.027 Uiso 1 1 calc R U . . .
N3 N 0.65078(8) -0.17154(11) 0.72949(6) 0.0203(3) Uani 1 1 d . . . . .
N7 N 0.74782(7) -0.13947(11) 0.49261(6) 0.0200(3) Uani 1 1 d . . . . .
N9 N 0.7500 -0.59160(15) 0.2500 0.0195(4) Uani 1 2 d S T P . .
N6 N 0.83796(7) -0.15175(11) 0.26298(6) 0.0202(3) Uani 1 1 d . . . . .
C21 C 0.87554(9) -0.05567(12) 0.34685(7) 0.0182(3) Uani 1 1 d . . . . .
C2 C 0.63762(9) 0.20128(12) 0.50841(7) 0.0172(3) Uani 1 1 d . . . . .
C18 C 0.85401(9) 0.09445(12) 0.41577(7) 0.0176(3) Uani 1 1 d . . . . .
C6 C 0.62546(9) -0.07476(12) 0.64584(7) 0.0178(3) Uani 1 1 d . . . . .
C3 C 0.65829(9) 0.07881(12) 0.58344(7) 0.0169(3) Uani 1 1 d . . . . .
O9 O 0.76416(13) -0.44322(12) 0.51364(9) 0.0606(5) Uani 1 1 d G . . . .
H9A H 0.7712 -0.4855 0.5390 0.091 Uiso 1 1 d G U . . .
H9B H 0.7565 -0.4717 0.4829 0.091 Uiso 1 1 d G U . . .
C20 C 0.81067(9) -0.00199(13) 0.33287(7) 0.0184(3) Uani 1 1 d . . . . .
H20 H 0.7744 -0.0162 0.3006 0.022 Uiso 1 1 calc R U . . .
C23 C 0.91806(9) 0.03904(13) 0.43070(7) 0.0185(3) Uani 1 1 d . . . . .
H23 H 0.9537 0.0516 0.4636 0.022 Uiso 1 1 calc R U . . .
C25 C 0.86141(9) -0.22719(13) 0.23652(7) 0.0196(3) Uani 1 1 d . . . . .
C19 C 0.80026(9) 0.07159(13) 0.36651(7) 0.0181(3) Uani 1 1 d . . . . .
H19 H 0.7570 0.1067 0.3565 0.022 Uiso 1 1 calc R U . . .
C7 C 0.57565(9) -0.04511(12) 0.59654(7) 0.0182(3) Uani 1 1 d . . . . .
H7 H 0.5310 -0.0766 0.5843 0.022 Uiso 1 1 calc R U . . .
C10 C 0.62220(9) -0.24787(12) 0.75220(7) 0.0202(3) Uani 1 1 d . . . . .
C22 C 0.92823(9) -0.03467(13) 0.39626(7) 0.0185(3) Uani 1 1 d . . . . .
H22 H 0.9710 -0.0707 0.4064 0.022 Uiso 1 1 calc R U . . .
C4 C 0.70907(9) 0.04750(13) 0.63250(7) 0.0188(3) Uani 1 1 d . . . . .
H4 H 0.7541 0.0781 0.6445 0.023 Uiso 1 1 calc R U . . .
C17 C 0.88211(9) 0.20569(13) 0.49604(7) 0.0189(3) Uani 1 1 d . . . . .
C5 C 0.69316(9) -0.02736(13) 0.66282(7) 0.0189(3) Uani 1 1 d . . . . .
H5 H 0.7276 -0.0469 0.6950 0.023 Uiso 1 1 calc R U . . .
C8 C 0.59124(9) 0.03005(12) 0.56541(7) 0.0183(3) Uani 1 1 d . . . . .
H8 H 0.5574 0.0482 0.5326 0.022 Uiso 1 1 calc R U . . .
C30 C 0.93099(9) -0.26377(13) 0.26345(7) 0.0201(3) Uani 1 1 d . . . . .
C15 C 0.55634(9) -0.28606(13) 0.71906(7) 0.0211(4) Uani 1 1 d . . . . .
C26 C 0.82078(10) -0.26889(14) 0.18679(7) 0.0235(4) Uani 1 1 d . . . . .
H26 H 0.7744 -0.2462 0.1688 0.028 Uiso 1 1 calc R U . . .
C60 C 0.59646(10) -0.78663(14) 0.20439(7) 0.0234(4) Uani 1 1 d . . . . .
H60A H 0.5571 -0.7411 0.2019 0.028 Uiso 1 1 calc R U . . .
H60B H 0.5821 -0.8288 0.1725 0.028 Uiso 1 1 calc R U . . .
C9 C 0.60913(9) -0.15117(12) 0.68040(7) 0.0188(3) Uani 1 1 d . . . . .
C62 C 0.68498(9) -0.65503(13) 0.24917(7) 0.0214(4) Uani 1 1 d . . . . .
H62A H 0.6434 -0.6131 0.2461 0.026 Uiso 1 1 calc R U . . .
H62B H 0.6953 -0.6889 0.2840 0.026 Uiso 1 1 calc R U . . .
C24 C 0.88621(9) -0.13090(12) 0.30942(7) 0.0179(3) Uani 1 1 d . . . . .
C58 C 0.76603(10) -0.52888(13) 0.30127(7) 0.0225(4) Uani 1 1 d . . . . .
H58A H 0.7814 -0.5710 0.3331 0.027 Uiso 1 1 calc R U . . .
H58B H 0.7213 -0.4973 0.3022 0.027 Uiso 1 1 calc R U . . .
C42 C 0.79045(10) -0.05985(13) 0.52937(7) 0.0235(4) Uani 1 1 d . . . . .
H42A H 0.7569 -0.0090 0.5324 0.028 Uiso 1 1 calc R U . . .
H42B H 0.8242 -0.0317 0.5118 0.028 Uiso 1 1 calc R U . . .
C50 C 0.68265(9) -0.65414(14) 0.74176(7) 0.0224(4) Uani 1 1 d . . . . .
H50A H 0.6871 -0.6898 0.7755 0.027 Uiso 1 1 calc R U . . .
H50B H 0.6406 -0.6118 0.7356 0.027 Uiso 1 1 calc R U . . .
C29 C 0.96136(10) -0.33990(13) 0.24150(8) 0.0236(4) Uani 1 1 d . . . . .
H29 H 1.0075 -0.3635 0.2595 0.028 Uiso 1 1 calc R U . . .
C54 C 0.74391(10) -0.52872(14) 0.69964(7) 0.0228(4) Uani 1 1 d . . . . .
H54A H 0.7346 -0.5712 0.6679 0.027 Uiso 1 1 calc R U . . .
H54B H 0.7905 -0.4974 0.7039 0.027 Uiso 1 1 calc R U . . .
C11 C 0.65415(11) -0.28774(14) 0.80413(7) 0.0259(4) Uani 1 1 d . . . . .
H11 H 0.6974 -0.2625 0.8268 0.031 Uiso 1 1 calc R U . . .
C48 C 0.60467(10) -0.79347(14) 0.69494(8) 0.0263(4) Uani 1 1 d . . . . .
H48A H 0.5624 -0.7538 0.6934 0.032 Uiso 1 1 calc R U . . .
H48B H 0.5929 -0.8337 0.6622 0.032 Uiso 1 1 calc R U . . .
C1 C 0.62964(9) 0.34536(13) 0.45181(7) 0.0201(3) Uani 1 1 d . . . . .
H1A H 0.6202 0.4102 0.4633 0.024 Uiso 1 1 calc R U . . .
H1B H 0.5831 0.3156 0.4335 0.024 Uiso 1 1 calc R U . . .
C38 C 0.79527(10) -0.22708(13) 0.49003(8) 0.0224(4) Uani 1 1 d . . . . .
H38A H 0.7662 -0.2733 0.4639 0.027 Uiso 1 1 calc R U . . .
H38B H 0.8093 -0.2583 0.5257 0.027 Uiso 1 1 calc R U . . .
C16 C 0.89598(9) 0.33787(13) 0.56160(7) 0.0210(4) Uani 1 1 d . . . . .
H16A H 0.9073 0.4052 0.5560 0.025 Uiso 1 1 calc R U . . .
H16B H 0.9415 0.3042 0.5780 0.025 Uiso 1 1 calc R U . . .
C34 C 0.71801(10) -0.09825(13) 0.43478(7) 0.0236(4) Uani 1 1 d . . . . .
H34A H 0.7587 -0.0792 0.4218 0.028 Uiso 1 1 calc R U . . .
H34B H 0.6920 -0.1496 0.4108 0.028 Uiso 1 1 calc R U . . .
C27 C 0.85102(10) -0.34430(14) 0.16510(7) 0.0244(4) Uani 1 1 d . . . . .
H27 H 0.8246 -0.3723 0.1320 0.029 Uiso 1 1 calc R U . . .
C28 C 0.92079(10) -0.37954(14) 0.19197(8) 0.0253(4) Uani 1 1 d . . . . .
H28 H 0.9401 -0.4301 0.1764 0.030 Uiso 1 1 calc R U . . .
C49 C 0.66833(10) -0.72672(14) 0.69480(8) 0.0270(4) Uani 1 1 d . . . . .
H49A H 0.7116 -0.7656 0.6984 0.032 Uiso 1 1 calc R U . . .
H49B H 0.6573 -0.6920 0.6602 0.032 Uiso 1 1 calc R U . . .
C41 C 0.83289(10) -0.09248(13) 0.58678(7) 0.0240(4) Uani 1 1 d . . . . .
H41A H 0.8584 -0.1526 0.5847 0.029 Uiso 1 1 calc R U . . .
H41B H 0.7996 -0.1047 0.6082 0.029 Uiso 1 1 calc R U . . .
C61 C 0.66425(11) -0.72989(14) 0.20330(8) 0.0266(4) Uani 1 1 d . . . . .
H61A H 0.7044 -0.7748 0.2071 0.032 Uiso 1 1 calc R U . . .
H61B H 0.6553 -0.6972 0.1682 0.032 Uiso 1 1 calc R U . . .
C46 C 0.68661(9) -0.17380(13) 0.51486(7) 0.0227(4) Uani 1 1 d . . . . .
H46A H 0.7081 -0.2040 0.5503 0.027 Uiso 1 1 calc R U . . .
H46B H 0.6597 -0.1172 0.5208 0.027 Uiso 1 1 calc R U . . .
C12 C 0.62037(11) -0.36532(14) 0.82122(8) 0.0272(4) Uani 1 1 d . . . . .
H12 H 0.6413 -0.3924 0.8557 0.033 Uiso 1 1 calc R U . . .
C37 C 0.86411(10) -0.20521(14) 0.47387(8) 0.0262(4) Uani 1 1 d . . . . .
H37A H 0.8861 -0.1457 0.4917 0.031 Uiso 1 1 calc R U . . .
H37B H 0.8516 -0.1955 0.4345 0.031 Uiso 1 1 calc R U . . .
C13 C 0.55521(11) -0.40358(14) 0.78746(8) 0.0281(4) Uani 1 1 d . . . . .
H13 H 0.5337 -0.4561 0.7997 0.034 Uiso 1 1 calc R U . . .
C40 C 0.88748(10) -0.01441(14) 0.61488(8) 0.0276(4) Uani 1 1 d . . . . .
H40A H 0.9199 -0.0010 0.5929 0.033 Uiso 1 1 calc R U . . .
H40B H 0.8618 0.0452 0.6177 0.033 Uiso 1 1 calc R U . . .
C14 C 0.52207(10) -0.36454(14) 0.73600(8) 0.0258(4) Uani 1 1 d . . . . .
H14 H 0.4786 -0.3897 0.7136 0.031 Uiso 1 1 calc R U . . .
C59 C 0.60771(11) -0.84823(15) 0.25594(8) 0.0300(4) Uani 1 1 d . . . . .
H59A H 0.6185 -0.8066 0.2875 0.045 Uiso 1 1 calc R U . . .
H59B H 0.6475 -0.8923 0.2592 0.045 Uiso 1 1 calc R U . . .
H59C H 0.5643 -0.8846 0.2536 0.045 Uiso 1 1 calc R U . . .
C39 C 0.93153(11) -0.04708(15) 0.67166(8) 0.0329(4) Uani 1 1 d . . . . .
H39A H 0.9547 -0.1080 0.6690 0.049 Uiso 1 1 calc R U . . .
H39B H 0.8999 -0.0549 0.6944 0.049 Uiso 1 1 calc R U . . .
H39C H 0.9679 0.0010 0.6875 0.049 Uiso 1 1 calc R U . . .
C44 C 0.56678(10) -0.25819(15) 0.49829(8) 0.0303(4) Uani 1 1 d . . . . .
H44A H 0.5439 -0.1954 0.4989 0.036 Uiso 1 1 calc R U . . .
H44B H 0.5814 -0.2836 0.5354 0.036 Uiso 1 1 calc R U . . .
C45 C 0.63332(10) -0.24519(15) 0.47878(8) 0.0278(4) Uani 1 1 d . . . . .
H45A H 0.6186 -0.2216 0.4413 0.033 Uiso 1 1 calc R U . . .
H45B H 0.6571 -0.3076 0.4793 0.033 Uiso 1 1 calc R U . . .
C36 C 0.91846(10) -0.28886(15) 0.49054(9) 0.0311(4) Uani 1 1 d . . . . .
H36A H 0.8925 -0.3500 0.4813 0.037 Uiso 1 1 calc R U . . .
H36B H 0.9529 -0.2846 0.4694 0.037 Uiso 1 1 calc R U . . .
C56 C 0.85845(11) -0.42206(14) 0.36595(8) 0.0295(4) Uani 1 1 d . . . . .
H56A H 0.8840 -0.3608 0.3673 0.035 Uiso 1 1 calc R U . . .
H56B H 0.8203 -0.4123 0.3833 0.035 Uiso 1 1 calc R U . . .
C47 C 0.62035(12) -0.85899(16) 0.74510(8) 0.0348(5) Uani 1 1 d . . . . .
H47A H 0.5817 -0.9054 0.7404 0.052 Uiso 1 1 calc R U . . .
H47B H 0.6239 -0.8202 0.7771 0.052 Uiso 1 1 calc R U . . .
H47C H 0.6654 -0.8928 0.7494 0.052 Uiso 1 1 calc R U . . .
C33 C 0.66742(10) -0.01132(14) 0.42935(8) 0.0284(4) Uani 1 1 d . . . . .
H33A H 0.6958 0.0465 0.4432 0.034 Uiso 1 1 calc R U . . .
H33B H 0.6345 -0.0223 0.4513 0.034 Uiso 1 1 calc R U . . .
C57 C 0.82397(11) -0.45085(15) 0.30594(8) 0.0315(4) Uani 1 1 d . . . . .
H57A H 0.8021 -0.3940 0.2849 0.038 Uiso 1 1 calc R U . . .
H57B H 0.8613 -0.4753 0.2907 0.038 Uiso 1 1 calc R U . . .
C32 C 0.62346(11) 0.00459(15) 0.36948(9) 0.0326(4) Uani 1 1 d . . . . .
H32A H 0.6031 0.0697 0.3659 0.039 Uiso 1 1 calc R U . . .
H32B H 0.6563 0.0013 0.3470 0.039 Uiso 1 1 calc R U . . .
C52 C 0.66942(11) -0.41464(14) 0.62883(8) 0.0311(4) Uani 1 1 d . . . . .
H52A H 0.6460 -0.3515 0.6258 0.037 Uiso 1 1 calc R U . . .
H52B H 0.7151 -0.4061 0.6204 0.037 Uiso 1 1 calc R U . . .
C53 C 0.68544(11) -0.45063(16) 0.68789(8) 0.0327(5) Uani 1 1 d . . . . .
H53A H 0.7016 -0.3966 0.7130 0.039 Uiso 1 1 calc R U . . .
H53B H 0.6414 -0.4770 0.6936 0.039 Uiso 1 1 calc R U . . .
C43 C 0.51209(11) -0.32736(17) 0.46124(9) 0.0357(5) Uani 1 1 d . . . . .
H43A H 0.4965 -0.3014 0.4247 0.054 Uiso 1 1 calc R U . . .
H43B H 0.4709 -0.3346 0.4749 0.054 Uiso 1 1 calc R U . . .
H43C H 0.5345 -0.3897 0.4608 0.054 Uiso 1 1 calc R U . . .
C55 C 0.91155(12) -0.49841(17) 0.39820(10) 0.0411(5) Uani 1 1 d . . . . .
H55A H 0.9348 -0.4745 0.4345 0.062 Uiso 1 1 calc R U . . .
H55B H 0.9477 -0.5116 0.3799 0.062 Uiso 1 1 calc R U . . .
H55C H 0.8856 -0.5572 0.4005 0.062 Uiso 1 1 calc R U . . .
C31 C 0.56201(11) -0.06737(17) 0.34705(10) 0.0394(5) Uani 1 1 d . . . . .
H31A H 0.5362 -0.0504 0.3099 0.059 Uiso 1 1 calc R U . . .
H31B H 0.5293 -0.0655 0.3691 0.059 Uiso 1 1 calc R U . . .
H31C H 0.5817 -0.1318 0.3479 0.059 Uiso 1 1 calc R U . . .
C35 C 0.96013(13) -0.28939(19) 0.55110(10) 0.0452(6) Uani 1 1 d . . . . .
H35A H 0.9953 -0.3411 0.5584 0.068 Uiso 1 1 calc R U . . .
H35B H 0.9269 -0.2992 0.5723 0.068 Uiso 1 1 calc R U . . .
H35C H 0.9846 -0.2282 0.5609 0.068 Uiso 1 1 calc R U . . .
C51 C 0.62141(13) -0.48244(18) 0.58678(10) 0.0469(6) Uani 1 1 d . . . . .
H51A H 0.6152 -0.4569 0.5506 0.070 Uiso 1 1 calc R U . . .
H51B H 0.5748 -0.4879 0.5932 0.070 Uiso 1 1 calc R U . . .
H51C H 0.6437 -0.5455 0.5898 0.070 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O3 1.4699(14) . ?
S1 O2 1.4474(13) . ?
S1 O1 1.4558(14) . ?
S1 C1 1.7926(17) . ?
S3 O5 1.4690(13) . ?
S3 O6 1.4500(13) . ?
S3 O7 1.4572(13) . ?
S3 C16 1.7945(17) . ?
S4 C30 1.7365(17) . ?
S4 C24 1.7663(17) . ?
S2 C15 1.7359(18) . ?
S2 C9 1.7655(17) . ?
O4 C2 1.224(2) . ?
O8 C17 1.226(2) . ?
N5 H5A 0.8600 . ?
N5 C18 1.394(2) . ?
N5 C17 1.381(2) . ?
N2 H2 0.8600 . ?
N2 C2 1.387(2) . ?
N2 C3 1.392(2) . ?
N8 C50 1.522(2) 2_656 ?
N8 C50 1.522(2) . ?
N8 C54 1.517(2) . ?
N8 C54 1.517(2) 2_656 ?
N1 H1 0.8600 . ?
N1 C2 1.362(2) . ?
N1 C1 1.435(2) . ?
N4 H4A 0.8600 . ?
N4 C17 1.363(2) . ?
N4 C16 1.433(2) . ?
N3 C10 1.387(2) . ?
N3 C9 1.303(2) . ?
N7 C42 1.515(2) . ?
N7 C38 1.523(2) . ?
N7 C34 1.525(2) . ?
N7 C46 1.523(2) . ?
N9 C62 1.519(2) 2_655 ?
N9 C62 1.519(2) . ?
N9 C58 1.519(2) 2_655 ?
N9 C58 1.519(2) . ?
N6 C25 1.382(2) . ?
N6 C24 1.304(2) . ?
C21 C20 1.402(2) . ?
C21 C22 1.396(2) . ?
C21 C24 1.461(2) . ?
C18 C23 1.402(2) . ?
C18 C19 1.408(2) . ?
C6 C7 1.399(2) . ?
C6 C5 1.406(2) . ?
C6 C9 1.462(2) . ?
C3 C4 1.409(2) . ?
C3 C8 1.406(2) . ?
O9 H9A 0.8502 . ?
O9 H9B 0.8498 . ?
C20 H20 0.9300 . ?
C20 C19 1.377(3) . ?
C23 H23 0.9300 . ?
C23 C22 1.391(3) . ?
C25 C30 1.406(2) . ?
C25 C26 1.402(2) . ?
C19 H19 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.387(2) . ?
C10 C15 1.402(3) . ?
C10 C11 1.397(3) . ?
C22 H22 0.9300 . ?
C4 H4 0.9300 . ?
C4 C5 1.373(3) . ?
C5 H5 0.9300 . ?
C8 H8 0.9300 . ?
C30 C29 1.392(3) . ?
C15 C14 1.396(3) . ?
C26 H26 0.9300 . ?
C26 C27 1.380(3) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C60 C61 1.526(3) . ?
C60 C59 1.523(3) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C62 C61 1.520(2) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C58 C57 1.525(3) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 C41 1.519(2) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C50 C49 1.519(3) . ?
C29 H29 0.9300 . ?
C29 C28 1.386(3) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C54 C53 1.519(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.383(3) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C48 C49 1.530(3) . ?
C48 C47 1.519(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C37 1.527(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C33 1.521(3) . ?
C27 H27 0.9300 . ?
C27 C28 1.402(3) . ?
C28 H28 0.9300 . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C40 1.525(3) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 C45 1.518(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.398(3) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C36 1.527(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.387(3) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 C39 1.515(3) . ?
C14 H14 0.9300 . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C44 C45 1.512(3) . ?
C44 C43 1.523(3) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C35 1.516(3) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C56 C57 1.530(3) . ?
C56 C55 1.525(3) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C32 1.528(3) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C31 1.518(3) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 C53 1.527(3) . ?
C52 C51 1.513(3) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?

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
O3 S1 C1 106.06(8) . . ?
O2 S1 O3 113.07(8) . . ?
O2 S1 O1 114.42(8) . . ?
O2 S1 C1 104.30(8) . . ?
O1 S1 O3 110.95(8) . . ?
O1 S1 C1 107.28(8) . . ?
O5 S3 C16 105.78(8) . . ?
O6 S3 O5 113.20(8) . . ?
O6 S3 O7 114.49(8) . . ?
O6 S3 C16 104.58(8) . . ?
O7 S3 O5 110.56(7) . . ?
O7 S3 C16 107.50(8) . . ?
C30 S4 C24 89.06(8) . . ?
C15 S2 C9 88.95(8) . . ?
C18 N5 H5A 116.5 . . ?
C17 N5 H5A 116.5 . . ?
C17 N5 C18 126.92(14) . . ?
C2 N2 H2 116.4 . . ?
C2 N2 C3 127.19(14) . . ?
C3 N2 H2 116.4 . . ?
C50 N8 C50 110.41(19) . 2_656 ?
C54 N8 C50 110.65(10) 2_656 2_656 ?
C54 N8 C50 106.86(9) . 2_656 ?
C54 N8 C50 106.86(9) 2_656 . ?
C54 N8 C50 110.65(10) . . ?
C54 N8 C54 111.5(2) . 2_656 ?
C2 N1 H1 119.8 . . ?
C2 N1 C1 120.42(14) . . ?
C1 N1 H1 119.8 . . ?
C17 N4 H4A 119.7 . . ?
C17 N4 C16 120.60(14) . . ?
C16 N4 H4A 119.7 . . ?
C9 N3 C10 110.83(15) . . ?
C42 N7 C38 111.99(13) . . ?
C42 N7 C34 108.16(13) . . ?
C42 N7 C46 109.30(14) . . ?
C38 N7 C34 108.20(13) . . ?
C46 N7 C38 108.01(13) . . ?
C46 N7 C34 111.20(13) . . ?
C62 N9 C62 109.99(19) 2_655 . ?
C62 N9 C58 110.74(10) 2_655 . ?
C62 N9 C58 110.75(10) . 2_655 ?
C62 N9 C58 107.24(9) . . ?
C62 N9 C58 107.24(9) 2_655 2_655 ?
C58 N9 C58 110.90(19) . 2_655 ?
C24 N6 C25 111.12(14) . . ?
C20 C21 C24 119.38(15) . . ?
C22 C21 C20 118.51(16) . . ?
C22 C21 C24 122.10(15) . . ?
O4 C2 N2 123.60(15) . . ?
O4 C2 N1 123.80(15) . . ?
N1 C2 N2 112.60(14) . . ?
N5 C18 C23 124.91(15) . . ?
N5 C18 C19 116.53(15) . . ?
C23 C18 C19 118.56(16) . . ?
C7 C6 C5 118.07(16) . . ?
C7 C6 C9 122.59(15) . . ?
C5 C6 C9 119.33(15) . . ?
N2 C3 C4 116.85(15) . . ?
N2 C3 C8 124.74(15) . . ?
C8 C3 C4 118.41(15) . . ?
H9A O9 H9B 109.5 . . ?
C21 C20 H20 119.7 . . ?
C19 C20 C21 120.55(15) . . ?
C19 C20 H20 119.7 . . ?
C18 C23 H23 120.1 . . ?
C22 C23 C18 119.89(15) . . ?
C22 C23 H23 120.1 . . ?
N6 C25 C30 115.44(15) . . ?
N6 C25 C26 124.91(16) . . ?
C26 C25 C30 119.63(17) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 C18 121.06(15) . . ?
C20 C19 H19 119.5 . . ?
C6 C7 H7 119.2 . . ?
C8 C7 C6 121.64(15) . . ?
C8 C7 H7 119.2 . . ?
N3 C10 C15 115.47(15) . . ?
N3 C10 C11 124.99(17) . . ?
C11 C10 C15 119.54(17) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 C21 121.38(15) . . ?
C23 C22 H22 119.3 . . ?
C3 C4 H4 119.4 . . ?
C5 C4 C3 121.11(16) . . ?
C5 C4 H4 119.4 . . ?
O8 C17 N5 123.71(16) . . ?
O8 C17 N4 123.56(16) . . ?
N4 C17 N5 112.73(14) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 C6 120.82(15) . . ?
C4 C5 H5 119.6 . . ?
C3 C8 H8 120.0 . . ?
C7 C8 C3 119.92(15) . . ?
C7 C8 H8 120.0 . . ?
C25 C30 S4 109.28(13) . . ?
C29 C30 S4 129.15(14) . . ?
C29 C30 C25 121.56(16) . . ?
C10 C15 S2 109.43(13) . . ?
C14 C15 S2 128.73(15) . . ?
C14 C15 C10 121.83(17) . . ?
C25 C26 H26 120.7 . . ?
C27 C26 C25 118.68(17) . . ?
C27 C26 H26 120.7 . . ?
H60A C60 H60B 107.8 . . ?
C61 C60 H60A 109.0 . . ?
C61 C60 H60B 109.0 . . ?
C59 C60 H60A 109.0 . . ?
C59 C60 H60B 109.0 . . ?
C59 C60 C61 113.13(15) . . ?
N3 C9 S2 115.32(13) . . ?
N3 C9 C6 123.52(16) . . ?
C6 C9 S2 121.16(12) . . ?
N9 C62 H62A 108.4 . . ?
N9 C62 H62B 108.4 . . ?
N9 C62 C61 115.38(14) . . ?
H62A C62 H62B 107.5 . . ?
C61 C62 H62A 108.4 . . ?
C61 C62 H62B 108.4 . . ?
N6 C24 S4 115.08(13) . . ?
N6 C24 C21 123.30(15) . . ?
C21 C24 S4 121.62(12) . . ?
N9 C58 H58A 108.5 . . ?
N9 C58 H58B 108.5 . . ?
N9 C58 C57 115.17(14) . . ?
H58A C58 H58B 107.5 . . ?
C57 C58 H58A 108.5 . . ?
C57 C58 H58B 108.5 . . ?
N7 C42 H42A 108.5 . . ?
N7 C42 H42B 108.5 . . ?
N7 C42 C41 115.04(14) . . ?
H42A C42 H42B 107.5 . . ?
C41 C42 H42A 108.5 . . ?
C41 C42 H42B 108.5 . . ?
N8 C50 H50A 108.4 . . ?
N8 C50 H50B 108.4 . . ?
H50A C50 H50B 107.4 . . ?
C49 C50 N8 115.72(14) . . ?
C49 C50 H50A 108.4 . . ?
C49 C50 H50B 108.4 . . ?
C30 C29 H29 121.0 . . ?
C28 C29 C30 118.06(17) . . ?
C28 C29 H29 121.0 . . ?
N8 C54 H54A 108.4 . . ?
N8 C54 H54B 108.4 . . ?
N8 C54 C53 115.71(14) . . ?
H54A C54 H54B 107.4 . . ?
C53 C54 H54A 108.4 . . ?
C53 C54 H54B 108.4 . . ?
C10 C11 H11 120.6 . . ?
C12 C11 C10 118.90(18) . . ?
C12 C11 H11 120.6 . . ?
H48A C48 H48B 107.7 . . ?
C49 C48 H48A 108.9 . . ?
C49 C48 H48B 108.9 . . ?
C47 C48 H48A 108.9 . . ?
C47 C48 H48B 108.9 . . ?
C47 C48 C49 113.26(16) . . ?
S1 C1 H1A 108.9 . . ?
S1 C1 H1B 108.9 . . ?
N1 C1 S1 113.39(12) . . ?
N1 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
N7 C38 H38A 108.4 . . ?
N7 C38 H38B 108.4 . . ?
N7 C38 C37 115.70(15) . . ?
H38A C38 H38B 107.4 . . ?
C37 C38 H38A 108.4 . . ?
C37 C38 H38B 108.4 . . ?
S3 C16 H16A 108.9 . . ?
S3 C16 H16B 108.9 . . ?
N4 C16 S3 113.22(12) . . ?
N4 C16 H16A 108.9 . . ?
N4 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
N7 C34 H34A 108.4 . . ?
N7 C34 H34B 108.4 . . ?
H34A C34 H34B 107.5 . . ?
C33 C34 N7 115.41(15) . . ?
C33 C34 H34A 108.4 . . ?
C33 C34 H34B 108.4 . . ?
C26 C27 H27 119.4 . . ?
C26 C27 C28 121.25(17) . . ?
C28 C27 H27 119.4 . . ?
C29 C28 C27 120.80(17) . . ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C50 C49 C48 110.62(15) . . ?
C50 C49 H49A 109.5 . . ?
C50 C49 H49B 109.5 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 108.1 . . ?
C42 C41 H41A 109.6 . . ?
C42 C41 H41B 109.6 . . ?
C42 C41 C40 110.28(15) . . ?
H41A C41 H41B 108.1 . . ?
C40 C41 H41A 109.6 . . ?
C40 C41 H41B 109.6 . . ?
C60 C61 H61A 109.3 . . ?
C60 C61 H61B 109.3 . . ?
C62 C61 C60 111.40(15) . . ?
C62 C61 H61A 109.3 . . ?
C62 C61 H61B 109.3 . . ?
H61A C61 H61B 108.0 . . ?
N7 C46 H46A 108.4 . . ?
N7 C46 H46B 108.4 . . ?
H46A C46 H46B 107.4 . . ?
C45 C46 N7 115.64(15) . . ?
C45 C46 H46A 108.4 . . ?
C45 C46 H46B 108.4 . . ?
C11 C12 H12 119.5 . . ?
C11 C12 C13 120.98(17) . . ?
C13 C12 H12 119.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
C38 C37 C36 110.71(15) . . ?
H37A C37 H37B 108.1 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C12 C13 H13 119.4 . . ?
C14 C13 C12 121.15(18) . . ?
C14 C13 H13 119.4 . . ?
C41 C40 H40A 109.5 . . ?
C41 C40 H40B 109.5 . . ?
H40A C40 H40B 108.1 . . ?
C39 C40 C41 110.84(16) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C15 C14 H14 121.2 . . ?
C13 C14 C15 117.58(18) . . ?
C13 C14 H14 121.2 . . ?
C60 C59 H59A 109.5 . . ?
C60 C59 H59B 109.5 . . ?
C60 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C40 C39 H39A 109.5 . . ?
C40 C39 H39B 109.5 . . ?
C40 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
H44A C44 H44B 108.0 . . ?
C45 C44 H44A 109.3 . . ?
C45 C44 H44B 109.3 . . ?
C45 C44 C43 111.54(17) . . ?
C43 C44 H44A 109.3 . . ?
C43 C44 H44B 109.3 . . ?
C46 C45 H45A 109.4 . . ?
C46 C45 H45B 109.4 . . ?
C44 C45 C46 111.29(16) . . ?
C44 C45 H45A 109.4 . . ?
C44 C45 H45B 109.4 . . ?
H45A C45 H45B 108.0 . . ?
C37 C36 H36A 108.8 . . ?
C37 C36 H36B 108.8 . . ?
H36A C36 H36B 107.7 . . ?
C35 C36 C37 113.66(18) . . ?
C35 C36 H36A 108.8 . . ?
C35 C36 H36B 108.8 . . ?
H56A C56 H56B 107.8 . . ?
C57 C56 H56A 109.0 . . ?
C57 C56 H56B 109.0 . . ?
C55 C56 H56A 109.0 . . ?
C55 C56 H56B 109.0 . . ?
C55 C56 C57 112.74(17) . . ?
C48 C47 H47A 109.5 . . ?
C48 C47 H47B 109.5 . . ?
C48 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C34 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
C34 C33 C32 110.82(17) . . ?
H33A C33 H33B 108.1 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C58 C57 C56 110.65(16) . . ?
C58 C57 H57A 109.5 . . ?
C58 C57 H57B 109.5 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 108.1 . . ?
C33 C32 H32A 108.5 . . ?
C33 C32 H32B 108.5 . . ?
H32A C32 H32B 107.5 . . ?
C31 C32 C33 115.15(18) . . ?
C31 C32 H32A 108.5 . . ?
C31 C32 H32B 108.5 . . ?
H52A C52 H52B 107.7 . . ?
C53 C52 H52A 108.8 . . ?
C53 C52 H52B 108.8 . . ?
C51 C52 H52A 108.8 . . ?
C51 C52 H52B 108.8 . . ?
C51 C52 C53 113.82(19) . . ?
C54 C53 C52 110.30(16) . . ?
C54 C53 H53A 109.6 . . ?
C54 C53 H53B 109.6 . . ?
C52 C53 H53A 109.6 . . ?
C52 C53 H53B 109.6 . . ?
H53A C53 H53B 108.1 . . ?
C44 C43 H43A 109.5 . . ?
C44 C43 H43B 109.5 . . ?
C44 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C56 C55 H55A 109.5 . . ?
C56 C55 H55B 109.5 . . ?
C56 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C36 C35 H35A 109.5 . . ?
C36 C35 H35B 109.5 . . ?
C36 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C52 C51 H51A 109.5 . . ?
C52 C51 H51B 109.5 . . ?
C52 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 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
S4 C30 C29 C28 178.92(14) . . . . ?
S2 C15 C14 C13 179.08(14) . . . . ?
O5 S3 C16 N4 -62.85(14) . . . . ?
O6 S3 C16 N4 177.38(13) . . . . ?
O7 S3 C16 N4 55.30(14) . . . . ?
O3 S1 C1 N1 -63.27(14) . . . . ?
O2 S1 C1 N1 177.11(13) . . . . ?
O1 S1 C1 N1 55.36(14) . . . . ?
N5 C18 C23 C22 -177.32(16) . . . . ?
N5 C18 C19 C20 177.80(15) . . . . ?
N2 C3 C4 C5 177.80(15) . . . . ?
N2 C3 C8 C7 -177.41(16) . . . . ?
N8 C50 C49 C48 173.45(15) . . . . ?
N8 C54 C53 C52 -163.07(16) . . . . ?
N3 C10 C15 S2 -0.32(19) . . . . ?
N3 C10 C15 C14 178.46(16) . . . . ?
N3 C10 C11 C12 -178.65(16) . . . . ?
N7 C42 C41 C40 166.06(15) . . . . ?
N7 C38 C37 C36 161.38(15) . . . . ?
N7 C34 C33 C32 -162.88(15) . . . . ?
N7 C46 C45 C44 -168.06(16) . . . . ?
N9 C62 C61 C60 -177.40(14) . . . . ?
N9 C58 C57 C56 -156.31(16) . . . . ?
N6 C25 C30 S4 0.55(19) . . . . ?
N6 C25 C30 C29 179.86(16) . . . . ?
N6 C25 C26 C27 -179.76(16) . . . . ?
C21 C20 C19 C18 -0.4(3) . . . . ?
C2 N2 C3 C4 -179.39(16) . . . . ?
C2 N2 C3 C8 -0.2(3) . . . . ?
C2 N1 C1 S1 -112.29(15) . . . . ?
C18 N5 C17 O8 -12.5(3) . . . . ?
C18 N5 C17 N4 167.09(16) . . . . ?
C18 C23 C22 C21 -0.5(3) . . . . ?
C6 C7 C8 C3 -0.4(3) . . . . ?
C3 N2 C2 O4 -13.8(3) . . . . ?
C3 N2 C2 N1 165.89(16) . . . . ?
C3 C4 C5 C6 -0.3(3) . . . . ?
C20 C21 C22 C23 -1.4(3) . . . . ?
C20 C21 C24 S4 179.70(13) . . . . ?
C20 C21 C24 N6 -0.3(3) . . . . ?
C23 C18 C19 C20 -1.5(2) . . . . ?
C25 N6 C24 S4 1.48(19) . . . . ?
C25 N6 C24 C21 -178.55(15) . . . . ?
C25 C30 C29 C28 -0.2(3) . . . . ?
C25 C26 C27 C28 0.3(3) . . . . ?
C19 C18 C23 C22 1.9(2) . . . . ?
C7 C6 C5 C4 1.6(2) . . . . ?
C7 C6 C9 S2 8.8(2) . . . . ?
C7 C6 C9 N3 -171.13(16) . . . . ?
C10 N3 C9 S2 0.83(19) . . . . ?
C10 N3 C9 C6 -179.26(15) . . . . ?
C10 C15 C14 C13 0.6(3) . . . . ?
C10 C11 C12 C13 -0.2(3) . . . . ?
C22 C21 C20 C19 1.8(2) . . . . ?
C22 C21 C24 S4 0.1(2) . . . . ?
C22 C21 C24 N6 -179.82(16) . . . . ?
C4 C3 C8 C7 1.8(2) . . . . ?
C17 N5 C18 C23 -3.4(3) . . . . ?
C17 N5 C18 C19 177.37(16) . . . . ?
C17 N4 C16 S3 -105.77(16) . . . . ?
C5 C6 C7 C8 -1.3(3) . . . . ?
C5 C6 C9 S2 -172.43(13) . . . . ?
C5 C6 C9 N3 7.7(3) . . . . ?
C8 C3 C4 C5 -1.5(3) . . . . ?
C30 S4 C24 N6 -1.01(14) . . . . ?
C30 S4 C24 C21 179.02(14) . . . . ?
C30 C25 C26 C27 -1.0(3) . . . . ?
C30 C29 C28 C27 -0.5(3) . . . . ?
C15 S2 C9 N3 -0.88(14) . . . . ?
C15 S2 C9 C6 179.22(14) . . . . ?
C15 C10 C11 C12 1.0(3) . . . . ?
C26 C25 C30 S4 -178.31(13) . . . . ?
C26 C25 C30 C29 1.0(3) . . . . ?
C26 C27 C28 C29 0.5(3) . . . . ?
C9 S2 C15 C10 0.62(13) . . . . ?
C9 S2 C15 C14 -178.05(18) . . . . ?
C9 N3 C10 C15 -0.3(2) . . . . ?
C9 N3 C10 C11 179.38(17) . . . . ?
C9 C6 C7 C8 177.53(16) . . . . ?
C9 C6 C5 C4 -177.24(16) . . . . ?
C62 N9 C62 C61 -54.40(13) 2_655 . . . ?
C62 N9 C58 C57 -172.79(16) . . . . ?
C62 N9 C58 C57 67.2(2) 2_655 . . . ?
C24 S4 C30 C25 0.22(13) . . . . ?
C24 S4 C30 C29 -179.02(17) . . . . ?
C24 N6 C25 C30 -1.3(2) . . . . ?
C24 N6 C25 C26 177.48(17) . . . . ?
C24 C21 C20 C19 -177.75(15) . . . . ?
C24 C21 C22 C23 178.17(15) . . . . ?
C58 N9 C62 C61 -174.90(15) . . . . ?
C58 N9 C62 C61 64.0(2) 2_655 . . . ?
C58 N9 C58 C57 -51.75(13) 2_655 . . . ?
C42 N7 C38 C37 -53.9(2) . . . . ?
C42 N7 C34 C33 -60.06(19) . . . . ?
C42 N7 C46 C45 173.02(15) . . . . ?
C42 C41 C40 C39 -178.56(16) . . . . ?
C50 N8 C50 C49 -56.49(13) 2_656 . . . ?
C50 N8 C54 C53 -172.66(16) 2_656 . . . ?
C50 N8 C54 C53 67.1(2) . . . . ?
C54 N8 C50 C49 -176.88(15) 2_656 . . . ?
C54 N8 C50 C49 61.6(2) . . . . ?
C54 N8 C54 C53 -51.66(14) 2_656 . . . ?
C11 C10 C15 S2 179.96(14) . . . . ?
C11 C10 C15 C14 -1.3(3) . . . . ?
C11 C12 C13 C14 -0.5(3) . . . . ?
C1 N1 C2 O4 0.2(3) . . . . ?
C1 N1 C2 N2 -179.54(15) . . . . ?
C38 N7 C42 C41 -52.63(19) . . . . ?
C38 N7 C34 C33 178.43(15) . . . . ?
C38 N7 C46 C45 -64.90(19) . . . . ?
C38 C37 C36 C35 -78.2(2) . . . . ?
C16 N4 C17 O8 -4.3(3) . . . . ?
C16 N4 C17 N5 176.01(15) . . . . ?
C34 N7 C42 C41 -171.77(14) . . . . ?
C34 N7 C38 C37 65.24(19) . . . . ?
C34 N7 C46 C45 53.7(2) . . . . ?
C34 C33 C32 C31 74.8(2) . . . . ?
C46 N7 C42 C41 67.02(18) . . . . ?
C46 N7 C38 C37 -174.29(15) . . . . ?
C46 N7 C34 C33 60.0(2) . . . . ?
C12 C13 C14 C15 0.3(3) . . . . ?
C59 C60 C61 C62 -64.4(2) . . . . ?
C47 C48 C49 C50 -65.4(2) . . . . ?
C43 C44 C45 C46 178.28(17) . . . . ?
C55 C56 C57 C58 75.3(2) . . . . ?
C51 C52 C53 C54 78.4(2) . . . . ?

_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 1.531
_oxdiff_exptl_absorpt_empirical_full_min 0.467
####################################################################### 
# 
# 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_jrh20200012a-hjs_ref
_database_code_depnum_ccdc_archive 'CCDC 2022536'
loop_
_audit_author_name
_audit_author_address
'Jennifer Hiscock'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2020-08-10 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_audit_creation_date             2020-08-10
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C10 H10 N3 O4 S2, 2(H2 O), C16 H36 N'
_chemical_formula_sum            'C26 H50 N4 O6 S2'
_chemical_formula_weight         578.82
_chemical_melting_point          ?
_chemical_oxdiff_formula         C26H50N4O6S2
_chemical_oxdiff_usercomment     '100 k'
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                   8.43220(10)
_cell_length_b                   16.2622(2)
_cell_length_c                   23.0023(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.4260(10)
_cell_angle_gamma                90
_cell_volume                     3102.14(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8816
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      71.8290
_cell_measurement_theta_min      4.7490
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.912
_exptl_absorpt_correction_T_max  0.509
_exptl_absorpt_correction_T_min  0.087
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 2 -3 0.1158
1 9 5 0.0295
5 -3 -6 0.1046
0 -4 13 0.0136
-5 4 4 0.0765
0 4 -13 0.0271
0 -8 -10 0.0186

_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.041
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5.3670 2.0320 -3.0329 0.1282 0.5301 0.8382
1.1262 9.3735 5.4827 0.2275 0.9520 -0.2048
4.9801 -3.4083 -6.2638 -0.0089 0.0009 1.0000
0.2135 -4.3574 13.2657 -0.9697 0.2322 -0.0754
-5.0072 4.0238 4.3797 0.1463 -0.0338 -0.9887
-0.2135 4.3574 -13.2657 0.9697 -0.2322 0.0754
-0.0107 -7.9869 -10.0219 0.0642 -0.9260 0.4208

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21823
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.103
_diffrn_reflns_theta_min         3.908
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -67.00  30.00   1.00    5.00    --  -41.91  42.00   2.00   97
  2  ω    -67.00  31.00   1.00    5.00    --  -41.91  57.00-150.00   98
  3  ω   -110.00 -19.00   1.00    5.00    --  -41.91 -57.00  60.00   91
  4  ω     55.00  87.00   1.00    5.00    --   41.91-125.00   0.00   32
  5  ω     27.00  74.00   1.00   10.00    --  103.72 -94.00 120.00   47
  6  ω     75.00 171.00   1.00   10.00    --  103.72  30.00   0.00   96
  7  ω     31.00 135.00   1.00   10.00    --  103.72 -77.00-150.00  104
  8  ω     35.00  65.00   1.00   10.00    --  103.72-125.00-150.00   30
  9  ω     97.00 135.00   1.00   10.00    --  103.72 125.00-180.00   38
 10  ω    101.00 176.00   1.00   10.00    --  103.72 125.00 -90.00   75
 11  ω     32.00  70.00   1.00   10.00    --  103.72 -45.00-120.00   38
 12  ω     93.00 119.00   1.00   10.00    --  103.72 -45.00-120.00   26
 13  ω     43.00 118.00   1.00   10.00    --  103.72-125.00-120.00   75
 14  ω     36.00 112.00   1.00   10.00    --  103.72-125.00 120.00   76
 15  ω     77.00 178.00   1.00   10.00    --  103.72  30.00 -90.00  101
 16  ω     77.00 102.00   1.00   10.00    --  103.72  61.00  60.00   25
 17  ω     32.00 118.00   1.00   10.00    --  103.72-125.00  60.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0285349000
_diffrn_orient_matrix_UB_12      0.0588782000
_diffrn_orient_matrix_UB_13      -0.0533031000
_diffrn_orient_matrix_UB_21      0.0947031000
_diffrn_orient_matrix_UB_22      0.0678096000
_diffrn_orient_matrix_UB_23      0.0382516000
_diffrn_orient_matrix_UB_31      0.1573599000
_diffrn_orient_matrix_UB_32      -0.0301602000
_diffrn_orient_matrix_UB_33      -0.0181198000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5113
_reflns_number_total             6021
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         6021
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0392
_refine_ls_restrained_S_all      1.020
_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)+(0.0559P)²+0.5186P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1069
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
2.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C18(H18A,H18B), C14(H14A,H14B), C16(H16A,H16B), C22(H22A,
 H22B), C1(H1A,H1B), C12(H12A,H12B), C13(H13A,H13B), C17(H17A,H17B), C25(H25A,
 H25B), C20(H20A,H20B), C24(H24A,H24B), C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C6(H6), C10(H10), C9(H9)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C11(H11A,H11B,H11C), C19(H19A,H19B,
 H19C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.82114(4) 0.37051(2) 0.50312(2) 0.02238(11) Uani 1 1 d . . . . .
S2 S 0.87910(5) 0.46283(2) 0.78367(2) 0.02440(11) Uani 1 1 d . . . . .
O2 O 0.86447(14) 0.30108(8) 0.46882(5) 0.0275(3) Uani 1 1 d . . . . .
O4 O 0.94402(14) 0.38472(7) 0.68413(5) 0.0261(3) Uani 1 1 d . . . . .
O5 O 0.89552(15) 0.63854(8) 0.58827(5) 0.0304(3) Uani 1 1 d G . . . .
H5A H 0.8134 0.6280 0.5620 0.046 Uiso 1 1 d G U . . .
H5B H 0.9778 0.6631 0.5653 0.046 Uiso 1 1 d G U . . .
O1 O 0.81850(14) 0.44850(7) 0.47156(5) 0.0276(3) Uani 1 1 d . . . . .
O3 O 0.67672(13) 0.35691(8) 0.52785(5) 0.0293(3) Uani 1 1 d . . . . .
N1 N 0.97229(16) 0.45056(9) 0.59852(6) 0.0245(3) Uani 1 1 d . . . . .
H1 H 0.9813 0.4978 0.5826 0.029 Uiso 1 1 calc R U . . .
N3 N 0.86906(16) 0.61610(9) 0.74847(6) 0.0240(3) Uani 1 1 d . . . . .
N4 N 0.35963(15) 0.68992(8) 0.70655(6) 0.0226(3) Uani 1 1 d . . . . .
N2 N 0.92173(16) 0.52505(9) 0.67681(6) 0.0244(3) Uani 1 1 d . . . . .
H2 H 0.9266 0.5663 0.6538 0.029 Uiso 1 1 calc R U . . .
O6 O 0.64391(17) 0.58549(10) 0.50705(9) 0.0552(5) Uani 1 1 d G . . . .
H6A H 0.6635 0.5383 0.4928 0.083 Uiso 1 1 d G U . . .
H6B H 0.5449 0.5979 0.4968 0.083 Uiso 1 1 d G U . . .
C2 C 0.94544(18) 0.44759(10) 0.65473(7) 0.0227(3) Uani 1 1 d . . . . .
C4 C 0.83993(18) 0.61627(10) 0.80632(8) 0.0240(3) Uani 1 1 d . . . . .
C26 C 0.40399(19) 0.68207(11) 0.77324(7) 0.0247(3) Uani 1 1 d . . . . .
H26A H 0.4333 0.7362 0.7894 0.030 Uiso 1 1 calc R U . . .
H26B H 0.4993 0.6477 0.7823 0.030 Uiso 1 1 calc R U . . .
C3 C 0.89128(18) 0.54142(10) 0.73200(7) 0.0230(3) Uani 1 1 d . . . . .
C18 C 0.50509(18) 0.72957(10) 0.68693(7) 0.0239(3) Uani 1 1 d . . . . .
H18A H 0.5272 0.7813 0.7078 0.029 Uiso 1 1 calc R U . . .
H18B H 0.5978 0.6942 0.6991 0.029 Uiso 1 1 calc R U . . .
C5 C 0.83878(19) 0.53871(10) 0.83298(8) 0.0245(3) Uani 1 1 d . . . . .
C14 C 0.32207(18) 0.60670(10) 0.67712(7) 0.0232(3) Uani 1 1 d . . . . .
H14A H 0.2345 0.5821 0.6932 0.028 Uiso 1 1 calc R U . . .
H14B H 0.2830 0.6160 0.6353 0.028 Uiso 1 1 calc R U . . .
C16 C 0.6449(2) 0.78587(11) 0.60996(8) 0.0276(4) Uani 1 1 d . . . . .
H16A H 0.6613 0.8374 0.6314 0.033 Uiso 1 1 calc R U . . .
H16B H 0.7350 0.7501 0.6251 0.033 Uiso 1 1 calc R U . . .
C22 C 0.20776(18) 0.74120(10) 0.68814(8) 0.0243(3) Uani 1 1 d . . . . .
H22A H 0.1856 0.7450 0.6453 0.029 Uiso 1 1 calc R U . . .
H22B H 0.1182 0.7123 0.7000 0.029 Uiso 1 1 calc R U . . .
C6 C 0.8105(2) 0.52954(11) 0.89011(8) 0.0270(4) Uani 1 1 d . . . . .
H6 H 0.8103 0.4776 0.9069 0.032 Uiso 1 1 calc R U . . .
C7 C 0.78241(19) 0.59923(12) 0.92205(8) 0.0284(4) Uani 1 1 d . . . . .
C1 C 0.98630(19) 0.37809(10) 0.56446(7) 0.0246(3) Uani 1 1 d . . . . .
H1A H 0.9875 0.3300 0.5894 0.030 Uiso 1 1 calc R U . . .
H1B H 1.0872 0.3796 0.5499 0.030 Uiso 1 1 calc R U . . .
C12 C 0.38796(19) 0.46259(10) 0.65847(8) 0.0265(3) Uani 1 1 d . . . . .
H12A H 0.3111 0.4437 0.6822 0.032 Uiso 1 1 calc R U . . .
H12B H 0.3298 0.4711 0.6185 0.032 Uiso 1 1 calc R U . . .
C10 C 0.81429(19) 0.68633(11) 0.83847(8) 0.0269(3) Uani 1 1 d . . . . .
H10 H 0.8157 0.7384 0.8218 0.032 Uiso 1 1 calc R U . . .
C13 C 0.45884(19) 0.54458(10) 0.68308(8) 0.0258(3) Uani 1 1 d . . . . .
H13A H 0.5088 0.5385 0.7243 0.031 Uiso 1 1 calc R U . . .
H13B H 0.5403 0.5630 0.6612 0.031 Uiso 1 1 calc R U . . .
C17 C 0.4898(2) 0.74619(12) 0.62141(8) 0.0298(4) Uani 1 1 d . . . . .
H17A H 0.3992 0.7826 0.6083 0.036 Uiso 1 1 calc R U . . .
H17B H 0.4708 0.6951 0.5995 0.036 Uiso 1 1 calc R U . . .
C25 C 0.27655(19) 0.64693(12) 0.80530(8) 0.0282(4) Uani 1 1 d . . . . .
H25A H 0.2389 0.5944 0.7881 0.034 Uiso 1 1 calc R U . . .
H25B H 0.1852 0.6840 0.8014 0.034 Uiso 1 1 calc R U . . .
C9 C 0.78670(19) 0.67685(11) 0.89574(8) 0.0288(4) Uani 1 1 d . . . . .
H9 H 0.7705 0.7234 0.9174 0.035 Uiso 1 1 calc R U . . .
C20 C 0.0677(2) 0.87746(12) 0.68299(9) 0.0317(4) Uani 1 1 d . . . . .
H20A H -0.0299 0.8478 0.6865 0.038 Uiso 1 1 calc R U . . .
H20B H 0.0656 0.9295 0.7034 0.038 Uiso 1 1 calc R U . . .
C24 C 0.3504(2) 0.63572(12) 0.87055(8) 0.0313(4) Uani 1 1 d . . . . .
H24A H 0.4403 0.5978 0.8738 0.038 Uiso 1 1 calc R U . . .
H24B H 0.3923 0.6882 0.8866 0.038 Uiso 1 1 calc R U . . .
C15 C 0.6429(2) 0.80219(12) 0.54468(8) 0.0317(4) Uani 1 1 d . . . . .
H15A H 0.6228 0.7517 0.5230 0.048 Uiso 1 1 calc R U . . .
H15B H 0.7453 0.8241 0.5397 0.048 Uiso 1 1 calc R U . . .
H15C H 0.5593 0.8411 0.5302 0.048 Uiso 1 1 calc R U . . .
C21 C 0.2138(2) 0.82771(11) 0.71333(8) 0.0302(4) Uani 1 1 d . . . . .
H21A H 0.3123 0.8547 0.7074 0.036 Uiso 1 1 calc R U . . .
H21B H 0.2143 0.8252 0.7555 0.036 Uiso 1 1 calc R U . . .
C23 C 0.2310(2) 0.60341(14) 0.90723(9) 0.0376(4) Uani 1 1 d . . . . .
H23A H 0.1846 0.5530 0.8903 0.056 Uiso 1 1 calc R U . . .
H23B H 0.1472 0.6433 0.9076 0.056 Uiso 1 1 calc R U . . .
H23C H 0.2858 0.5935 0.9470 0.056 Uiso 1 1 calc R U . . .
C11 C 0.5143(2) 0.39613(12) 0.65760(9) 0.0354(4) Uani 1 1 d . . . . .
H11A H 0.5862 0.4125 0.6318 0.053 Uiso 1 1 calc R U . . .
H11B H 0.4621 0.3456 0.6436 0.053 Uiso 1 1 calc R U . . .
H11C H 0.5743 0.3883 0.6968 0.053 Uiso 1 1 calc R U . . .
C19 C 0.0680(3) 0.89416(13) 0.61799(9) 0.0404(5) Uani 1 1 d . . . . .
H19A H 0.0523 0.8435 0.5963 0.061 Uiso 1 1 calc R U . . .
H19B H 0.1694 0.9179 0.6137 0.061 Uiso 1 1 calc R U . . .
H19C H -0.0177 0.9316 0.6029 0.061 Uiso 1 1 calc R U . . .
C8 C 0.7426(2) 0.59122(13) 0.98311(8) 0.0358(4) Uani 1 1 d . . . . .
H8A H 0.6368 0.5680 0.9804 0.054 Uiso 1 1 calc R U . . .
H8B H 0.7454 0.6445 1.0012 0.054 Uiso 1 1 calc R U . . .
H8C H 0.8203 0.5560 1.0067 0.054 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O2 1.4613(13) . ?
S1 O1 1.4594(12) . ?
S1 O3 1.4512(12) . ?
S1 C1 1.7985(17) . ?
S2 C3 1.7608(17) . ?
S2 C5 1.7506(17) . ?
O4 C2 1.227(2) . ?
O5 H5A 0.8501 . ?
O5 H5B 1.0266 . ?
N1 H1 0.8600 . ?
N1 C2 1.353(2) . ?
N1 C1 1.432(2) . ?
N3 C4 1.396(2) . ?
N3 C3 1.296(2) . ?
N4 C26 1.517(2) . ?
N4 C18 1.525(2) . ?
N4 C14 1.521(2) . ?
N4 C22 1.523(2) . ?
N2 H2 0.8600 . ?
N2 C2 1.386(2) . ?
N2 C3 1.366(2) . ?
O6 H6A 0.8631 . ?
O6 H6B 0.8500 . ?
C4 C5 1.403(2) . ?
C4 C10 1.396(2) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C25 1.520(2) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C17 1.513(2) . ?
C5 C6 1.385(2) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C13 1.521(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.523(2) . ?
C16 C15 1.522(2) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C21 1.519(2) . ?
C6 H6 0.9300 . ?
C6 C7 1.394(2) . ?
C7 C9 1.403(3) . ?
C7 C8 1.508(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.527(2) . ?
C12 C11 1.520(2) . ?
C10 H10 0.9300 . ?
C10 C9 1.387(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C24 1.528(2) . ?
C9 H9 0.9300 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.533(2) . ?
C20 C19 1.520(3) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C23 1.519(2) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?

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
O2 S1 C1 104.05(7) . . ?
O1 S1 O2 112.69(7) . . ?
O1 S1 C1 105.70(8) . . ?
O3 S1 O2 113.79(7) . . ?
O3 S1 O1 112.90(7) . . ?
O3 S1 C1 106.77(8) . . ?
C5 S2 C3 88.15(8) . . ?
H5A O5 H5B 104.6 . . ?
C2 N1 H1 118.7 . . ?
C2 N1 C1 122.55(14) . . ?
C1 N1 H1 118.7 . . ?
C3 N3 C4 109.89(14) . . ?
C26 N4 C18 105.70(12) . . ?
C26 N4 C14 111.64(13) . . ?
C26 N4 C22 111.62(12) . . ?
C14 N4 C18 111.01(12) . . ?
C14 N4 C22 105.46(12) . . ?
C22 N4 C18 111.54(12) . . ?
C2 N2 H2 117.2 . . ?
C3 N2 H2 117.2 . . ?
C3 N2 C2 125.54(14) . . ?
H6A O6 H6B 110.6 . . ?
O4 C2 N1 125.19(15) . . ?
O4 C2 N2 122.61(15) . . ?
N1 C2 N2 112.20(14) . . ?
N3 C4 C5 115.53(15) . . ?
N3 C4 C10 125.25(16) . . ?
C10 C4 C5 119.22(16) . . ?
N4 C26 H26A 108.0 . . ?
N4 C26 H26B 108.0 . . ?
N4 C26 C25 117.09(13) . . ?
H26A C26 H26B 107.3 . . ?
C25 C26 H26A 108.0 . . ?
C25 C26 H26B 108.0 . . ?
N3 C3 S2 116.98(13) . . ?
N3 C3 N2 121.04(15) . . ?
N2 C3 S2 121.98(12) . . ?
N4 C18 H18A 108.2 . . ?
N4 C18 H18B 108.2 . . ?
H18A C18 H18B 107.4 . . ?
C17 C18 N4 116.25(13) . . ?
C17 C18 H18A 108.2 . . ?
C17 C18 H18B 108.2 . . ?
C4 C5 S2 109.45(12) . . ?
C6 C5 S2 128.73(14) . . ?
C6 C5 C4 121.81(16) . . ?
N4 C14 H14A 108.0 . . ?
N4 C14 H14B 108.0 . . ?
H14A C14 H14B 107.2 . . ?
C13 C14 N4 117.24(13) . . ?
C13 C14 H14A 108.0 . . ?
C13 C14 H14B 108.0 . . ?
H16A C16 H16B 107.8 . . ?
C17 C16 H16A 109.0 . . ?
C17 C16 H16B 109.0 . . ?
C15 C16 H16A 109.0 . . ?
C15 C16 H16B 109.0 . . ?
C15 C16 C17 112.82(15) . . ?
N4 C22 H22A 108.4 . . ?
N4 C22 H22B 108.4 . . ?
H22A C22 H22B 107.4 . . ?
C21 C22 N4 115.63(13) . . ?
C21 C22 H22A 108.4 . . ?
C21 C22 H22B 108.4 . . ?
C5 C6 H6 120.4 . . ?
C5 C6 C7 119.16(17) . . ?
C7 C6 H6 120.4 . . ?
C6 C7 C9 118.94(16) . . ?
C6 C7 C8 120.57(17) . . ?
C9 C7 C8 120.46(16) . . ?
S1 C1 H1A 109.5 . . ?
S1 C1 H1B 109.5 . . ?
N1 C1 S1 110.90(11) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 108.0 . . ?
H12A C12 H12B 107.7 . . ?
C13 C12 H12A 108.9 . . ?
C13 C12 H12B 108.9 . . ?
C11 C12 H12A 108.9 . . ?
C11 C12 H12B 108.9 . . ?
C11 C12 C13 113.42(14) . . ?
C4 C10 H10 120.6 . . ?
C9 C10 C4 118.74(16) . . ?
C9 C10 H10 120.6 . . ?
C14 C13 C12 107.88(13) . . ?
C14 C13 H13A 110.1 . . ?
C14 C13 H13B 110.1 . . ?
C12 C13 H13A 110.1 . . ?
C12 C13 H13B 110.1 . . ?
H13A C13 H13B 108.4 . . ?
C18 C17 C16 109.07(14) . . ?
C18 C17 H17A 109.9 . . ?
C18 C17 H17B 109.9 . . ?
C16 C17 H17A 109.9 . . ?
C16 C17 H17B 109.9 . . ?
H17A C17 H17B 108.3 . . ?
C26 C25 H25A 109.9 . . ?
C26 C25 H25B 109.9 . . ?
C26 C25 C24 108.85(14) . . ?
H25A C25 H25B 108.3 . . ?
C24 C25 H25A 109.9 . . ?
C24 C25 H25B 109.9 . . ?
C7 C9 H9 119.0 . . ?
C10 C9 C7 122.10(16) . . ?
C10 C9 H9 119.0 . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C19 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
C19 C20 C21 113.45(15) . . ?
C25 C24 H24A 108.9 . . ?
C25 C24 H24B 108.9 . . ?
H24A C24 H24B 107.8 . . ?
C23 C24 C25 113.18(15) . . ?
C23 C24 H24A 108.9 . . ?
C23 C24 H24B 108.9 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C22 C21 C20 110.27(14) . . ?
C22 C21 H21A 109.6 . . ?
C22 C21 H21B 109.6 . . ?
C20 C21 H21A 109.6 . . ?
C20 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 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
S2 C5 C6 C7 179.29(13) . . . . ?
O2 S1 C1 N1 172.40(11) . . . . ?
O1 S1 C1 N1 53.49(13) . . . . ?
O3 S1 C1 N1 -66.96(13) . . . . ?
N3 C4 C5 S2 0.96(17) . . . . ?
N3 C4 C5 C6 -179.63(14) . . . . ?
N3 C4 C10 C9 179.98(15) . . . . ?
N4 C26 C25 C24 174.08(14) . . . . ?
N4 C18 C17 C16 179.82(14) . . . . ?
N4 C14 C13 C12 171.71(14) . . . . ?
N4 C22 C21 C20 169.80(14) . . . . ?
C2 N1 C1 S1 113.62(14) . . . . ?
C2 N2 C3 S2 0.3(2) . . . . ?
C2 N2 C3 N3 -179.27(14) . . . . ?
C4 N3 C3 S2 0.24(17) . . . . ?
C4 N3 C3 N2 179.86(13) . . . . ?
C4 C5 C6 C7 0.0(2) . . . . ?
C4 C10 C9 C7 -0.6(2) . . . . ?
C26 N4 C18 C17 -178.60(14) . . . . ?
C26 N4 C14 C13 -64.18(17) . . . . ?
C26 N4 C22 C21 57.34(18) . . . . ?
C26 C25 C24 C23 178.07(16) . . . . ?
C3 S2 C5 C4 -0.65(12) . . . . ?
C3 S2 C5 C6 180.00(16) . . . . ?
C3 N3 C4 C5 -0.79(19) . . . . ?
C3 N3 C4 C10 178.58(15) . . . . ?
C3 N2 C2 O4 -1.4(2) . . . . ?
C3 N2 C2 N1 179.64(14) . . . . ?
C18 N4 C26 C25 177.71(14) . . . . ?
C18 N4 C14 C13 53.47(18) . . . . ?
C18 N4 C22 C21 -60.66(18) . . . . ?
C5 S2 C3 N3 0.25(13) . . . . ?
C5 S2 C3 N2 -179.37(14) . . . . ?
C5 C4 C10 C9 -0.7(2) . . . . ?
C5 C6 C7 C9 -1.2(2) . . . . ?
C5 C6 C7 C8 176.77(15) . . . . ?
C14 N4 C26 C25 -61.49(18) . . . . ?
C14 N4 C18 C17 60.19(18) . . . . ?
C14 N4 C22 C21 178.74(14) . . . . ?
C22 N4 C26 C25 56.27(19) . . . . ?
C22 N4 C18 C17 -57.11(19) . . . . ?
C22 N4 C14 C13 174.42(14) . . . . ?
C6 C7 C9 C10 1.5(2) . . . . ?
C1 N1 C2 O4 6.6(2) . . . . ?
C1 N1 C2 N2 -174.49(13) . . . . ?
C10 C4 C5 S2 -178.44(12) . . . . ?
C10 C4 C5 C6 1.0(2) . . . . ?
C15 C16 C17 C18 178.00(15) . . . . ?
C11 C12 C13 C14 175.80(15) . . . . ?
C19 C20 C21 C22 -66.6(2) . . . . ?
C8 C7 C9 C10 -176.47(15) . . . . ?

_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 1.511
_oxdiff_exptl_absorpt_empirical_full_min 0.564
####################################################################### 
# 
# 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_2021jrh0004_res
_database_code_depnum_ccdc_archive 'CCDC 2106928'
loop_
_audit_author_name
_audit_author_address
'Jennifer Hiscock'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2021-09-01 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_audit_creation_date             2021-09-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H14 N3 O3 S, H2 O, C16 H36 N'
_chemical_formula_sum            'C33 H52 N4 O4 S'
_chemical_formula_weight         600.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H20N4O4S
_chemical_oxdiff_usercomment     '100 K lisa benzothazole carboxylate'
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                   9.1985(4)
_cell_length_b                   11.8652(4)
_cell_length_c                   16.6048(6)
_cell_angle_alpha                80.985(3)
_cell_angle_beta                 87.623(3)
_cell_angle_gamma                69.132(4)
_cell_volume                     1672.27(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5987
_cell_measurement_temperature    100.1(4)
_cell_measurement_theta_max      71.7890
_cell_measurement_theta_min      4.4610
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.181
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.623
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             652
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 5 1 0.0469
0 -5 -1 0.0469
4 2 5 0.0830
-4 -2 -5 0.0830
0 0 1 0.0327
0 0 -1 0.0327

_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.065
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0004 4.9982 0.9948 -0.0038 0.6943 -0.0227
0.0004 -4.9982 -0.9948 0.0038 -0.6943 0.0227
3.9951 2.0063 5.0042 0.0368 -0.0107 -0.7994
-3.9951 -2.0063 -5.0042 -0.0368 0.0107 0.7994
-0.0009 0.0013 1.0009 0.0810 -0.0027 -0.0477
0.0009 -0.0013 -1.0009 -0.0810 0.0027 0.0477

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11602
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.098
_diffrn_reflns_theta_min         4.034
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.1(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00  28.00   1.00    4.00    --  -41.91  57.00  30.00   96
  2  ω   -113.00 -20.00   1.00    4.00    --  -41.91 -57.00-120.00   93
  3  ω     62.00  88.00   1.00    4.00    --   41.91-125.00-180.00   26
  4  ω    -32.00  62.00   1.00    4.00    --   41.91 -38.00  90.00   94
  5  ω    106.00 132.00   1.00   15.00    --  103.72 -77.00 -30.00   26
  6  ω     36.00  62.00   1.00   15.00    --  103.72-125.00-120.00   26
  7  ω    121.00 173.00   1.00   15.00    --  103.72  61.00 -60.00   52
  8  ω     27.00 104.00   1.00   15.00    --  103.72 -94.00 -90.00   77
  9  ω     31.00 106.00   1.00   15.00    --  103.72 -77.00 150.00   75
 10  ω     42.00  71.00   1.00   15.00    --  103.72 -77.00 -30.00   29
 11  ω     77.00 173.00   1.00   15.00    --  103.72  30.00   0.00   96
 12  ω     33.00 118.00   1.00   15.00    --  103.72-125.00  90.00   85
 13  ω     95.00 177.00   1.00   15.00    --  103.72 125.00-120.00   82
 14  ω     91.00 116.00   1.00   15.00    --  103.72-125.00-120.00   25
 15  ω     31.00  69.00   1.00   15.00    --  103.72-125.00  60.00   38
 16  ω     90.00 116.00   1.00   15.00    --  103.72  61.00 -60.00   26
 17  ω    108.00 177.00   1.00   15.00    --  103.72  80.00  59.00   69
 18  ω     79.00 172.00   1.00   15.00    --  103.72  77.00-150.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0835964000
_diffrn_orient_matrix_UB_12      -0.0168668000
_diffrn_orient_matrix_UB_13      0.0808473000
_diffrn_orient_matrix_UB_21      -0.0690625000
_diffrn_orient_matrix_UB_22      0.1394843000
_diffrn_orient_matrix_UB_23      -0.0029191000
_diffrn_orient_matrix_UB_31      -0.1427448000
_diffrn_orient_matrix_UB_32      0.0049628000
_diffrn_orient_matrix_UB_33      -0.0477678000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5609
_reflns_number_total             6341
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    ?
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         6341
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0467
_refine_ls_restrained_S_all      1.028
_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)+(0.0720P)²+0.4190P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1281
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O4(H4A,H4B)
2.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C25(H25A,H25B), C28(H28A,H28B), C21(H21A,H21B), C33(H33A,
 H33B), C2(H2A,H2B), C24(H24A,H24B), C20(H20A,H20B), C27(H27A,H27B), C32(H32A,
 H32B), C19(H19A,H19B), C23(H23A,H23B), C31(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C8(H8), C5(H5), C6(H6), C9(H9), C16(H16), C12(H12), C15(H15)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C26(H26A,H26B,H26C), C22(H22A,H22B,H22C), C18(H18A,H18B,
 H18C), C30(H30A,H30B,H30C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.57208(5) 0.71528(3) 0.55158(2) 0.02690(12) Uani 1 1 d . . . . .
O3 O 0.39929(14) 0.40426(11) 0.25334(7) 0.0308(3) Uani 1 1 d . . . . .
O2 O 0.49695(17) 0.35937(12) -0.02732(7) 0.0393(3) Uani 1 1 d . . . . .
N3 N 0.64138(15) 0.86454(12) 0.43777(8) 0.0245(3) Uani 1 1 d . . . . .
O4 O 0.44151(19) 0.03885(13) -0.10946(8) 0.0452(3) Uani 1 1 d . . . . .
H4A H 0.4435 0.0896 -0.0791 0.068 Uiso 1 1 d G . . . .
H4B H 0.4827 -0.0333 -0.0842 0.068 Uiso 1 1 d G . . . .
N2 N 0.46363(16) 0.56608(12) 0.18835(8) 0.0275(3) Uani 1 1 d . . . . .
H2 H 0.4711 0.6048 0.1410 0.033 Uiso 1 1 calc R . . . .
N4 N -0.02361(15) 0.73828(12) 0.24445(8) 0.0259(3) Uani 1 1 d . . . . .
O1 O 0.4302(2) 0.19441(12) 0.00444(8) 0.0504(4) Uani 1 1 d . . . . .
N1 N 0.4268(2) 0.42992(14) 0.11639(9) 0.0360(3) Uani 1 1 d . . . . .
H1 H 0.4400 0.4772 0.0742 0.043 Uiso 1 1 calc R . . . .
C8 C 0.51401(18) 0.78810(14) 0.30440(9) 0.0246(3) Uani 1 1 d . . . . .
H8 H 0.5123 0.8679 0.2941 0.030 Uiso 1 1 calc R . . . .
C7 C 0.54653(17) 0.72317(14) 0.38368(9) 0.0235(3) Uani 1 1 d . . . . .
C17 C 0.67640(17) 0.88979(14) 0.51169(9) 0.0245(3) Uani 1 1 d . . . . .
C4 C 0.48738(17) 0.61490(14) 0.25512(9) 0.0237(3) Uani 1 1 d . . . . .
C5 C 0.51775(18) 0.54981(14) 0.33428(9) 0.0257(3) Uani 1 1 d . . . . .
H5 H 0.5188 0.4702 0.3447 0.031 Uiso 1 1 calc R . . . .
C3 C 0.42914(18) 0.46115(14) 0.19030(10) 0.0267(3) Uani 1 1 d . . . . .
C6 C 0.54612(18) 0.60352(14) 0.39677(9) 0.0250(3) Uani 1 1 d . . . . .
H6 H 0.5655 0.5593 0.4491 0.030 Uiso 1 1 calc R . . . .
C9 C 0.48451(18) 0.73581(14) 0.24137(9) 0.0251(3) Uani 1 1 d . . . . .
H9 H 0.4625 0.7808 0.1893 0.030 Uiso 1 1 calc R . . . .
C11 C 0.64712(18) 0.81728(14) 0.58159(10) 0.0256(3) Uani 1 1 d . . . . .
C16 C 0.74145(18) 0.97696(14) 0.52217(10) 0.0271(3) Uani 1 1 d . . . . .
H16 H 0.7631 1.0256 0.4772 0.033 Uiso 1 1 calc R . . . .
C12 C 0.67895(19) 0.83030(15) 0.66000(10) 0.0273(3) Uani 1 1 d . . . . .
H12 H 0.6578 0.7816 0.7051 0.033 Uiso 1 1 calc R . . . .
C10 C 0.58734(17) 0.77562(14) 0.44902(9) 0.0244(3) Uani 1 1 d . . . . .
C29 C -0.15831(18) 0.85519(14) 0.25434(10) 0.0260(3) Uani 1 1 d . . . . .
H29A H -0.2255 0.8786 0.2064 0.031 Uiso 1 1 calc R . . . .
H29B H -0.2184 0.8378 0.3009 0.031 Uiso 1 1 calc R . . . .
C15 C 0.77290(19) 0.98960(15) 0.59988(10) 0.0287(3) Uani 1 1 d . . . . .
H15 H 0.8155 1.0479 0.6066 0.034 Uiso 1 1 calc R . . . .
C25 C 0.08823(19) 0.69587(15) 0.31717(10) 0.0281(3) Uani 1 1 d . . . . .
H25A H 0.1632 0.6158 0.3118 0.034 Uiso 1 1 calc R . . . .
H25B H 0.1451 0.7511 0.3152 0.034 Uiso 1 1 calc R . . . .
C28 C -0.11429(19) 0.96328(15) 0.26613(10) 0.0290(3) Uani 1 1 d . . . . .
H28A H -0.0561 0.9837 0.2196 0.035 Uiso 1 1 calc R . . . .
H28B H -0.0491 0.9428 0.3146 0.035 Uiso 1 1 calc R . . . .
C13 C 0.74283(19) 0.91719(15) 0.66987(10) 0.0282(3) Uani 1 1 d . . . . .
C21 C -0.09669(19) 0.64399(15) 0.23623(10) 0.0288(3) Uani 1 1 d . . . . .
H21A H -0.1687 0.6752 0.1901 0.035 Uiso 1 1 calc R . . . .
H21B H -0.1570 0.6356 0.2846 0.035 Uiso 1 1 calc R . . . .
C33 C 0.0711(2) 0.75719(16) 0.16997(10) 0.0305(3) Uani 1 1 d . . . . .
H33A H 0.1153 0.8178 0.1778 0.037 Uiso 1 1 calc R . . . .
H33B H 0.1569 0.6813 0.1670 0.037 Uiso 1 1 calc R . . . .
C1 C 0.4482(2) 0.28842(15) 0.01962(10) 0.0327(4) Uani 1 1 d . . . . .
C2 C 0.4028(2) 0.31925(15) 0.10520(10) 0.0334(4) Uani 1 1 d . . . . .
H2A H 0.2942 0.3294 0.1139 0.040 Uiso 1 1 calc R . . . .
H2B H 0.4646 0.2523 0.1452 0.040 Uiso 1 1 calc R . . . .
C24 C 0.01366(19) 0.68860(16) 0.40017(10) 0.0315(4) Uani 1 1 d . . . . .
H24A H -0.0474 0.6363 0.4024 0.038 Uiso 1 1 calc R . . . .
H24B H -0.0560 0.7693 0.4082 0.038 Uiso 1 1 calc R . . . .
C14 C 0.7782(2) 0.93313(16) 0.75415(10) 0.0332(4) Uani 1 1 d . . . . .
H14A H 0.6981 0.9237 0.7906 0.050 Uiso 1 1 calc GR . . . .
H14B H 0.7823 1.0131 0.7528 0.050 Uiso 1 1 calc GR . . . .
H14C H 0.8767 0.8728 0.7729 0.050 Uiso 1 1 calc GR . . . .
C20 C 0.0155(2) 0.51760(16) 0.22480(12) 0.0356(4) Uani 1 1 d . . . . .
H20A H 0.0760 0.4785 0.2745 0.043 Uiso 1 1 calc R . . . .
H20B H 0.0869 0.5249 0.1813 0.043 Uiso 1 1 calc R . . . .
C27 C -0.2622(2) 1.07214(15) 0.27493(11) 0.0325(4) Uani 1 1 d . . . . .
H27A H -0.3246 1.0936 0.2254 0.039 Uiso 1 1 calc R . . . .
H27B H -0.3224 1.0490 0.3195 0.039 Uiso 1 1 calc R . . . .
C32 C -0.0155(2) 0.79742(18) 0.08883(11) 0.0375(4) Uani 1 1 d . . . . .
H32A H -0.0956 0.8772 0.0883 0.045 Uiso 1 1 calc R . . . .
H32B H -0.0653 0.7403 0.0808 0.045 Uiso 1 1 calc R . . . .
C19 C -0.0744(2) 0.43951(17) 0.20372(13) 0.0393(4) Uani 1 1 d . . . . .
H19A H -0.0062 0.3546 0.2120 0.047 Uiso 1 1 calc R . . . .
H19B H -0.1603 0.4475 0.2410 0.047 Uiso 1 1 calc R . . . .
C23 C 0.1363(2) 0.63842(19) 0.46787(11) 0.0399(4) Uani 1 1 d . . . . .
H23A H 0.2022 0.6872 0.4628 0.048 Uiso 1 1 calc R . . . .
H23B H 0.2012 0.5556 0.4618 0.048 Uiso 1 1 calc R . . . .
C26 C -0.2282(2) 1.18285(17) 0.29101(13) 0.0410(4) Uani 1 1 d . . . . .
H26A H -0.1734 1.2088 0.2457 0.061 Uiso 1 1 calc GR . . . .
H26B H -0.1654 1.1620 0.3397 0.061 Uiso 1 1 calc GR . . . .
H26C H -0.3243 1.2478 0.2978 0.061 Uiso 1 1 calc GR . . . .
C22 C 0.0650(2) 0.63863(19) 0.55221(11) 0.0433(5) Uani 1 1 d . . . . .
H22A H -0.0039 0.5933 0.5567 0.065 Uiso 1 1 calc GR . . . .
H22B H 0.0076 0.7211 0.5603 0.065 Uiso 1 1 calc GR . . . .
H22C H 0.1461 0.6016 0.5929 0.065 Uiso 1 1 calc GR . . . .
C31 C 0.0984(3) 0.8028(2) 0.02036(12) 0.0491(5) Uani 1 1 d . . . . .
H31A H 0.1503 0.8579 0.0299 0.059 Uiso 1 1 calc R . . . .
H31B H 0.1770 0.7223 0.0207 0.059 Uiso 1 1 calc R . . . .
C18 C -0.1380(3) 0.4733(2) 0.11711(14) 0.0509(5) Uani 1 1 d . . . . .
H18A H -0.0535 0.4636 0.0797 0.076 Uiso 1 1 calc GR . . . .
H18B H -0.2078 0.5566 0.1087 0.076 Uiso 1 1 calc GR . . . .
H18C H -0.1929 0.4210 0.1080 0.076 Uiso 1 1 calc GR . . . .
C30 C 0.0176(4) 0.8458(2) -0.06254(13) 0.0682(8) Uani 1 1 d . . . . .
H30A H 0.0929 0.8484 -0.1039 0.102 Uiso 1 1 calc GR . . . .
H30B H -0.0594 0.9259 -0.0634 0.102 Uiso 1 1 calc GR . . . .
H30C H -0.0317 0.7904 -0.0727 0.102 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 C11 1.7326(16) . ?
S1 C10 1.7613(15) . ?
O3 C3 1.230(2) . ?
O2 C1 1.246(2) . ?
N3 C17 1.385(2) . ?
N3 C10 1.304(2) . ?
O4 H4A 0.8499 . ?
O4 H4B 0.8501 . ?
N2 H2 0.8600 . ?
N2 C4 1.387(2) . ?
N2 C3 1.385(2) . ?
N4 C29 1.522(2) . ?
N4 C25 1.521(2) . ?
N4 C21 1.521(2) . ?
N4 C33 1.517(2) . ?
O1 C1 1.248(2) . ?
N1 H1 0.8600 . ?
N1 C3 1.340(2) . ?
N1 C2 1.447(2) . ?
C8 H8 0.9300 . ?
C8 C7 1.402(2) . ?
C8 C9 1.379(2) . ?
C7 C6 1.403(2) . ?
C7 C10 1.455(2) . ?
C17 C11 1.409(2) . ?
C17 C16 1.402(2) . ?
C4 C5 1.400(2) . ?
C4 C9 1.408(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.378(2) . ?
C6 H6 0.9300 . ?
C9 H9 0.9300 . ?
C11 C12 1.390(2) . ?
C16 H16 0.9300 . ?
C16 C15 1.376(2) . ?
C12 H12 0.9300 . ?
C12 C13 1.388(2) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C28 1.517(2) . ?
C15 H15 0.9300 . ?
C15 C13 1.412(2) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C24 1.518(2) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C27 1.527(2) . ?
C13 C14 1.505(2) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C20 1.523(2) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C32 1.515(2) . ?
C1 C2 1.527(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C23 1.519(2) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C19 1.529(2) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C26 1.518(2) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C31 1.523(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C18 1.514(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C22 1.522(3) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C30 1.517(3) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?

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
C11 S1 C10 89.28(7) . . ?
C10 N3 C17 110.69(13) . . ?
H4A O4 H4B 109.5 . . ?
C4 N2 H2 116.7 . . ?
C3 N2 H2 116.7 . . ?
C3 N2 C4 126.55(13) . . ?
C25 N4 C29 111.53(12) . . ?
C25 N4 C21 110.85(12) . . ?
C21 N4 C29 105.94(12) . . ?
C33 N4 C29 111.15(12) . . ?
C33 N4 C25 106.45(12) . . ?
C33 N4 C21 111.00(12) . . ?
C3 N1 H1 118.9 . . ?
C3 N1 C2 122.23(14) . . ?
C2 N1 H1 118.9 . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C9 C8 C7 121.22(14) . . ?
C8 C7 C6 117.61(14) . . ?
C8 C7 C10 121.16(14) . . ?
C6 C7 C10 121.15(14) . . ?
N3 C17 C11 115.62(14) . . ?
N3 C17 C16 125.93(14) . . ?
C16 C17 C11 118.42(14) . . ?
N2 C4 C5 123.73(14) . . ?
N2 C4 C9 117.56(14) . . ?
C5 C4 C9 118.69(14) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.12(14) . . ?
C6 C5 H5 119.9 . . ?
O3 C3 N2 123.38(15) . . ?
O3 C3 N1 123.30(15) . . ?
N1 C3 N2 113.29(14) . . ?
C7 C6 H6 119.1 . . ?
C5 C6 C7 121.82(14) . . ?
C5 C6 H6 119.1 . . ?
C8 C9 C4 120.53(14) . . ?
C8 C9 H9 119.7 . . ?
C4 C9 H9 119.7 . . ?
C17 C11 S1 109.02(12) . . ?
C12 C11 S1 128.66(12) . . ?
C12 C11 C17 122.31(15) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 C17 119.12(15) . . ?
C15 C16 H16 120.4 . . ?
C11 C12 H12 120.5 . . ?
C13 C12 C11 118.90(14) . . ?
C13 C12 H12 120.5 . . ?
N3 C10 S1 115.38(12) . . ?
N3 C10 C7 124.42(14) . . ?
C7 C10 S1 120.15(11) . . ?
N4 C29 H29A 108.3 . . ?
N4 C29 H29B 108.3 . . ?
H29A C29 H29B 107.4 . . ?
C28 C29 N4 115.98(13) . . ?
C28 C29 H29A 108.3 . . ?
C28 C29 H29B 108.3 . . ?
C16 C15 H15 118.8 . . ?
C16 C15 C13 122.36(15) . . ?
C13 C15 H15 118.8 . . ?
N4 C25 H25A 108.4 . . ?
N4 C25 H25B 108.4 . . ?
H25A C25 H25B 107.5 . . ?
C24 C25 N4 115.47(13) . . ?
C24 C25 H25A 108.4 . . ?
C24 C25 H25B 108.4 . . ?
C29 C28 H28A 109.9 . . ?
C29 C28 H28B 109.9 . . ?
C29 C28 C27 109.14(13) . . ?
H28A C28 H28B 108.3 . . ?
C27 C28 H28A 109.9 . . ?
C27 C28 H28B 109.9 . . ?
C12 C13 C15 118.88(15) . . ?
C12 C13 C14 119.91(15) . . ?
C15 C13 C14 121.21(15) . . ?
N4 C21 H21A 108.2 . . ?
N4 C21 H21B 108.2 . . ?
N4 C21 C20 116.18(13) . . ?
H21A C21 H21B 107.4 . . ?
C20 C21 H21A 108.2 . . ?
C20 C21 H21B 108.2 . . ?
N4 C33 H33A 108.2 . . ?
N4 C33 H33B 108.2 . . ?
H33A C33 H33B 107.4 . . ?
C32 C33 N4 116.26(14) . . ?
C32 C33 H33A 108.2 . . ?
C32 C33 H33B 108.2 . . ?
O2 C1 O1 127.23(17) . . ?
O2 C1 C2 117.25(15) . . ?
O1 C1 C2 115.51(15) . . ?
N1 C2 C1 111.18(14) . . ?
N1 C2 H2A 109.4 . . ?
N1 C2 H2B 109.4 . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C25 C24 H24A 109.4 . . ?
C25 C24 H24B 109.4 . . ?
C25 C24 C23 111.01(14) . . ?
H24A C24 H24B 108.0 . . ?
C23 C24 H24A 109.4 . . ?
C23 C24 H24B 109.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C21 C20 H20A 109.6 . . ?
C21 C20 H20B 109.6 . . ?
C21 C20 C19 110.19(15) . . ?
H20A C20 H20B 108.1 . . ?
C19 C20 H20A 109.6 . . ?
C19 C20 H20B 109.6 . . ?
C28 C27 H27A 109.1 . . ?
C28 C27 H27B 109.1 . . ?
H27A C27 H27B 107.8 . . ?
C26 C27 C28 112.57(15) . . ?
C26 C27 H27A 109.1 . . ?
C26 C27 H27B 109.1 . . ?
C33 C32 H32A 109.8 . . ?
C33 C32 H32B 109.8 . . ?
C33 C32 C31 109.46(16) . . ?
H32A C32 H32B 108.2 . . ?
C31 C32 H32A 109.8 . . ?
C31 C32 H32B 109.8 . . ?
C20 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C18 C19 C20 113.83(16) . . ?
C18 C19 H19A 108.8 . . ?
C18 C19 H19B 108.8 . . ?
C24 C23 H23A 109.1 . . ?
C24 C23 H23B 109.1 . . ?
C24 C23 C22 112.32(15) . . ?
H23A C23 H23B 107.9 . . ?
C22 C23 H23A 109.1 . . ?
C22 C23 H23B 109.1 . . ?
C27 C26 H26A 109.5 . . ?
C27 C26 H26B 109.5 . . ?
C27 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C32 C31 H31A 109.2 . . ?
C32 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
C30 C31 C32 111.9(2) . . ?
C30 C31 H31A 109.2 . . ?
C30 C31 H31B 109.2 . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C31 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
C31 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 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 C11 C12 C13 178.52(13) . . . . ?
O2 C1 C2 N1 -0.3(2) . . . . ?
N3 C17 C11 S1 -0.34(17) . . . . ?
N3 C17 C11 C12 178.81(14) . . . . ?
N3 C17 C16 C15 -178.55(15) . . . . ?
N2 C4 C5 C6 177.43(14) . . . . ?
N2 C4 C9 C8 -177.15(14) . . . . ?
N4 C29 C28 C27 179.97(13) . . . . ?
N4 C25 C24 C23 176.69(14) . . . . ?
N4 C21 C20 C19 -170.84(14) . . . . ?
N4 C33 C32 C31 -175.77(15) . . . . ?
O1 C1 C2 N1 -179.57(17) . . . . ?
C8 C7 C6 C5 1.1(2) . . . . ?
C8 C7 C10 S1 161.38(12) . . . . ?
C8 C7 C10 N3 -21.1(2) . . . . ?
C7 C8 C9 C4 -0.4(2) . . . . ?
C17 N3 C10 S1 0.68(17) . . . . ?
C17 N3 C10 C7 -176.94(14) . . . . ?
C17 C11 C12 C13 -0.5(2) . . . . ?
C17 C16 C15 C13 0.4(2) . . . . ?
C4 N2 C3 O3 7.8(3) . . . . ?
C4 N2 C3 N1 -174.13(15) . . . . ?
C4 C5 C6 C7 -0.3(2) . . . . ?
C5 C4 C9 C8 1.2(2) . . . . ?
C3 N2 C4 C5 16.5(2) . . . . ?
C3 N2 C4 C9 -165.26(15) . . . . ?
C3 N1 C2 C1 -164.73(16) . . . . ?
C6 C7 C10 S1 -21.9(2) . . . . ?
C6 C7 C10 N3 155.59(15) . . . . ?
C9 C8 C7 C6 -0.8(2) . . . . ?
C9 C8 C7 C10 176.05(14) . . . . ?
C9 C4 C5 C6 -0.8(2) . . . . ?
C11 S1 C10 N3 -0.76(13) . . . . ?
C11 S1 C10 C7 176.98(13) . . . . ?
C11 C17 C16 C15 -0.6(2) . . . . ?
C11 C12 C13 C15 0.2(2) . . . . ?
C11 C12 C13 C14 179.94(15) . . . . ?
C16 C17 C11 S1 -178.46(12) . . . . ?
C16 C17 C11 C12 0.7(2) . . . . ?
C16 C15 C13 C12 -0.1(2) . . . . ?
C16 C15 C13 C14 -179.91(15) . . . . ?
C10 S1 C11 C17 0.57(12) . . . . ?
C10 S1 C11 C12 -178.51(16) . . . . ?
C10 N3 C17 C11 -0.21(19) . . . . ?
C10 N3 C17 C16 177.74(15) . . . . ?
C10 C7 C6 C5 -175.66(14) . . . . ?
C29 N4 C25 C24 50.19(18) . . . . ?
C29 N4 C21 C20 179.54(14) . . . . ?
C29 N4 C33 C32 -59.63(18) . . . . ?
C29 C28 C27 C26 177.29(14) . . . . ?
C25 N4 C29 C28 57.68(17) . . . . ?
C25 N4 C21 C20 -59.31(18) . . . . ?
C25 N4 C33 C32 178.73(14) . . . . ?
C25 C24 C23 C22 175.82(16) . . . . ?
C21 N4 C29 C28 178.38(13) . . . . ?
C21 N4 C25 C24 -67.60(17) . . . . ?
C21 N4 C33 C32 58.01(18) . . . . ?
C21 C20 C19 C18 74.6(2) . . . . ?
C33 N4 C29 C28 -60.95(17) . . . . ?
C33 N4 C25 C24 171.59(14) . . . . ?
C33 N4 C21 C20 58.77(18) . . . . ?
C33 C32 C31 C30 -178.52(18) . . . . ?
C2 N1 C3 O3 -5.9(3) . . . . ?
C2 N1 C3 N2 176.07(16) . . . . ?

_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 1.375
_oxdiff_exptl_absorpt_empirical_full_min 0.834
####################################################################### 
# 
# 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_jrh20200019_res
_database_code_depnum_ccdc_archive 'CCDC 2033371'
loop_
_audit_author_name
_audit_author_address
'Jennifer Hiscock'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2020-09-22 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_audit_creation_date             2020-09-21
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C18 H18 N3 O4 S2, H2 O, C16 H36 N'
_chemical_formula_sum            'C34 H56 N4 O5 S2'
_chemical_formula_weight         664.94
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H20N2O2S2
_chemical_oxdiff_usercomment     '100 K nya 2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   9.2701(2)
_cell_length_b                   9.2791(3)
_cell_length_c                   21.7492(7)
_cell_angle_alpha                91.169(3)
_cell_angle_beta                 96.234(2)
_cell_angle_gamma                103.561(2)
_cell_volume                     1805.87(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5894
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      71.7540
_cell_measurement_theta_min      4.0660
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.688
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             720
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 1 -1 0.0534
-5 -1 1 0.0534
0 0 1 0.0128
0 0 -1 0.0128
2 -5 -1 0.0479
-2 5 1 0.0479

_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.026
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5.0028 0.9958 -0.9985 0.0144 -0.2079 -0.8869
-5.0028 -0.9958 0.9985 -0.0144 0.2079 0.8869
-0.0010 0.0001 1.0002 -0.0128 -0.0689 0.0131
0.0010 -0.0001 -1.0002 0.0128 0.0689 -0.0131
1.9950 -4.9992 -0.9980 -0.8151 0.2172 -0.0486
-1.9950 4.9992 0.9980 0.8151 -0.2172 0.0486

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12423
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.858
_diffrn_reflns_theta_min         4.094
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  30.00   1.00    2.94    --  -42.16  57.00 150.00   99
  2  ω    -90.00 -52.00   1.00    2.94    --  -42.16 125.00-150.00   38
  3  ω    -66.00  32.00   1.00    2.94    --  -42.16  38.00 -60.00   98
  4  ω   -110.00 -25.00   1.00    2.94    --  -42.16 -57.00   0.00   85
  5  ω     32.00  60.00   1.00   11.78    --  103.72 -61.00 -30.00   28
  6  ω     83.00 109.00   1.00   11.78    --  103.72 -61.00 -30.00   26
  7  ω     58.00 115.00   1.00   11.78    --  103.72 -77.00 120.00   57
  8  ω     38.00 118.00   1.00   11.78    --  103.72-125.00 150.00   80
  9  ω    115.00 176.00   1.00   11.78    --  103.72  61.00 -90.00   61
 10  ω     35.00 130.00   1.00   11.78    --  103.72 -45.00-150.00   95
 11  ω     33.00 119.00   1.00   11.78    --  103.72 -45.00 120.00   86
 12  ω     46.00 105.00   1.00   11.78    --  103.72 -94.00 -30.00   59
 13  ω     43.00 116.00   1.00   11.78    --  103.72 -45.00 -30.00   73
 14  ω     68.00 117.00   1.00   11.78    --  103.72-125.00 -60.00   49
 15  ω     17.00 164.00   1.00   11.78    --  103.72   0.00 -90.00  147
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0302470000
_diffrn_orient_matrix_UB_12      0.1535397000
_diffrn_orient_matrix_UB_13      -0.0128709000
_diffrn_orient_matrix_UB_21      -0.0457755000
_diffrn_orient_matrix_UB_22      -0.0479442000
_diffrn_orient_matrix_UB_23      -0.0689576000
_diffrn_orient_matrix_UB_31      -0.1631482000
_diffrn_orient_matrix_UB_32      -0.0579726000
_diffrn_orient_matrix_UB_33      0.0129555000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5940
_reflns_number_total             6885
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         6885
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0373
_refine_ls_restrained_S_all      1.033
_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)+(0.0393P)²+0.6599P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0950
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O5(H5A,H5B)
2.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C28(H28A,H28B), C23(H23A,H23B), C19(H19A,H19B), C32(H32A,
 H32B), C27(H27A,H27B), C33(H33A,H33B), C2(H2A,H2B), C3(H3A,H3B), C31(H31A,
 H31B), C25(H25A,H25B), C29(H29A,H29B), C1(H1A,H1B), C20(H20A,H20B), C21(H21A,
 H21B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C6(H6), C7(H7), C10(H10), C9(H9), C17(H17), C13(H13), C14(H14)
2.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C22(H22A,H22B,
 H22C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.75905(4) 0.11857(4) 0.63010(2) 0.01887(10) Uani 1 1 d . . . . .
S2 S -0.08618(5) 0.31721(5) 0.07262(2) 0.02704(11) Uani 1 1 d . . . . .
O1 O 0.60834(12) 0.03800(12) 0.64157(5) 0.0217(2) Uani 1 1 d . . . . .
O2 O 0.83701(12) 0.02384(13) 0.60006(5) 0.0250(2) Uani 1 1 d . . . . .
O4 O 0.48443(13) 0.48084(12) 0.38830(5) 0.0253(2) Uani 1 1 d . . . . .
O3 O 0.84452(14) 0.19930(13) 0.68570(6) 0.0300(3) Uani 1 1 d . . . . .
O5 O 0.91981(15) 0.12670(14) 0.81098(6) 0.0314(3) Uani 1 1 d G . . . .
H5A H 0.8924 0.1414 0.7735 0.047 Uiso 1 1 d G U . . .
H5B H 0.9255 0.2087 0.8303 0.047 Uiso 1 1 d G U . . .
N4 N 0.72184(13) 0.84057(14) 0.29086(6) 0.0171(3) Uani 1 1 d . . . . .
N1 N 0.52061(15) 0.25826(15) 0.41897(6) 0.0221(3) Uani 1 1 d . . . . .
H1 H 0.5018 0.1643 0.4105 0.027 Uiso 1 1 calc R U . . .
N2 N 0.37839(15) 0.26794(14) 0.32732(6) 0.0211(3) Uani 1 1 d . . . . .
H2 H 0.3761 0.1748 0.3246 0.025 Uiso 1 1 calc R U . . .
N3 N 0.00899(15) 0.58497(16) 0.12112(6) 0.0246(3) Uani 1 1 d . . . . .
C6 C 0.27826(17) 0.46605(17) 0.27657(7) 0.0207(3) Uani 1 1 d . . . . .
H6 H 0.3242 0.5356 0.3084 0.025 Uiso 1 1 calc R U . . .
C5 C 0.29724(16) 0.32063(17) 0.27876(7) 0.0191(3) Uani 1 1 d . . . . .
C24 C 0.66935(17) 0.56958(17) 0.25063(7) 0.0197(3) Uani 1 1 d . . . . .
H24A H 0.5771 0.5814 0.2280 0.024 Uiso 1 1 calc R U . . .
H24B H 0.6469 0.5284 0.2901 0.024 Uiso 1 1 calc R U . . .
C28 C 0.80136(17) 0.76917(17) 0.40013(7) 0.0205(3) Uani 1 1 d . . . . .
H28A H 0.8913 0.8469 0.3988 0.025 Uiso 1 1 calc R U . . .
H28B H 0.8227 0.6753 0.3888 0.025 Uiso 1 1 calc R U . . .
C23 C 0.78048(16) 0.71951(17) 0.26130(7) 0.0186(3) Uani 1 1 d . . . . .
H23A H 0.8678 0.7069 0.2875 0.022 Uiso 1 1 calc R U . . .
H23B H 0.8123 0.7521 0.2218 0.022 Uiso 1 1 calc R U . . .
C8 C 0.12054(17) 0.40500(18) 0.17836(7) 0.0211(3) Uani 1 1 d . . . . .
C4 C 0.46228(17) 0.34584(17) 0.37936(7) 0.0198(3) Uani 1 1 d . . . . .
C7 C 0.19122(17) 0.50619(17) 0.22712(7) 0.0214(3) Uani 1 1 d . . . . .
H7 H 0.1794 0.6030 0.2263 0.026 Uiso 1 1 calc R U . . .
C19 C 0.58415(16) 0.86517(17) 0.25172(7) 0.0197(3) Uani 1 1 d . . . . .
H19A H 0.5019 0.7800 0.2548 0.024 Uiso 1 1 calc R U . . .
H19B H 0.5577 0.9511 0.2693 0.024 Uiso 1 1 calc R U . . .
C32 C 0.82350(17) 1.10793(17) 0.33640(7) 0.0198(3) Uani 1 1 d . . . . .
H32A H 0.8337 1.0842 0.3796 0.024 Uiso 1 1 calc R U . . .
H32B H 0.7235 1.1217 0.3256 0.024 Uiso 1 1 calc R U . . .
C27 C 0.67661(16) 0.79840(17) 0.35433(7) 0.0185(3) Uani 1 1 d . . . . .
H27A H 0.5953 0.7100 0.3494 0.022 Uiso 1 1 calc R U . . .
H27B H 0.6391 0.8777 0.3716 0.022 Uiso 1 1 calc R U . . .
C33 C 0.93862(17) 1.25057(17) 0.32650(7) 0.0209(3) Uani 1 1 d . . . . .
H33A H 1.0378 1.2378 0.3402 0.025 Uiso 1 1 calc R U . . .
H33B H 0.9338 1.2682 0.2826 0.025 Uiso 1 1 calc R U . . .
C2 C 0.64133(17) 0.19593(17) 0.51665(7) 0.0210(3) Uani 1 1 d . . . . .
H2A H 0.6935 0.1346 0.4953 0.025 Uiso 1 1 calc R U . . .
H2B H 0.5461 0.1339 0.5247 0.025 Uiso 1 1 calc R U . . .
C10 C 0.22745(17) 0.21876(18) 0.22973(7) 0.0223(3) Uani 1 1 d . . . . .
H10 H 0.2400 0.1222 0.2302 0.027 Uiso 1 1 calc R U . . .
C3 C 0.61465(17) 0.32039(17) 0.47574(7) 0.0207(3) Uani 1 1 d . . . . .
H3A H 0.5664 0.3845 0.4977 0.025 Uiso 1 1 calc R U . . .
H3B H 0.7095 0.3796 0.4658 0.025 Uiso 1 1 calc R U . . .
C9 C 0.14031(17) 0.26007(18) 0.18074(7) 0.0228(3) Uani 1 1 d . . . . .
H9 H 0.0942 0.1907 0.1489 0.027 Uiso 1 1 calc R U . . .
C31 C 0.84750(16) 0.98117(16) 0.29621(7) 0.0186(3) Uani 1 1 d . . . . .
H31A H 0.9394 0.9561 0.3130 0.022 Uiso 1 1 calc R U . . .
H31B H 0.8608 1.0158 0.2550 0.022 Uiso 1 1 calc R U . . .
C11 C 0.02481(17) 0.45030(18) 0.12786(7) 0.0220(3) Uani 1 1 d . . . . .
C25 C 0.73640(17) 0.46489(18) 0.21378(7) 0.0221(3) Uani 1 1 d . . . . .
H25A H 0.7433 0.4988 0.1721 0.027 Uiso 1 1 calc R U . . .
H25B H 0.8368 0.4684 0.2328 0.027 Uiso 1 1 calc R U . . .
C29 C 0.75596(19) 0.7646(2) 0.46533(7) 0.0255(3) Uani 1 1 d . . . . .
H29A H 0.7386 0.8600 0.4770 0.031 Uiso 1 1 calc R U . . .
H29B H 0.6632 0.6902 0.4659 0.031 Uiso 1 1 calc R U . . .
C1 C 0.73338(17) 0.25831(17) 0.57778(7) 0.0215(3) Uani 1 1 d . . . . .
H1A H 0.6841 0.3253 0.5974 0.026 Uiso 1 1 calc R U . . .
H1B H 0.8305 0.3155 0.5694 0.026 Uiso 1 1 calc R U . . .
C20 C 0.59935(18) 0.88871(18) 0.18352(7) 0.0229(3) Uani 1 1 d . . . . .
H20A H 0.6222 0.8022 0.1647 0.028 Uiso 1 1 calc R U . . .
H20B H 0.6810 0.9738 0.1794 0.028 Uiso 1 1 calc R U . . .
C34 C 0.91415(18) 1.38538(18) 0.36122(8) 0.0246(3) Uani 1 1 d . . . . .
H34A H 0.9843 1.4728 0.3510 0.037 Uiso 1 1 calc R U . . .
H34B H 0.9285 1.3728 0.4050 0.037 Uiso 1 1 calc R U . . .
H34C H 0.8143 1.3955 0.3495 0.037 Uiso 1 1 calc R U . . .
C26 C 0.64443(19) 0.30494(18) 0.21056(8) 0.0263(3) Uani 1 1 d . . . . .
H26A H 0.6891 0.2443 0.1859 0.039 Uiso 1 1 calc R U . . .
H26B H 0.5445 0.3009 0.1922 0.039 Uiso 1 1 calc R U . . .
H26C H 0.6418 0.2689 0.2516 0.039 Uiso 1 1 calc R U . . .
C18 C -0.15987(19) 0.4554(2) 0.03854(8) 0.0279(4) Uani 1 1 d . . . . .
C12 C -0.09665(19) 0.5907(2) 0.07132(7) 0.0264(3) Uani 1 1 d . . . . .
C21 C 0.4547(2) 0.9145(2) 0.15015(8) 0.0305(4) Uani 1 1 d . . . . .
H21A H 0.3762 0.8247 0.1501 0.037 Uiso 1 1 calc R U . . .
H21B H 0.4255 0.9926 0.1725 0.037 Uiso 1 1 calc R U . . .
C17 C -0.2671(2) 0.4437(2) -0.01287(8) 0.0327(4) Uani 1 1 d . . . . .
H17 H -0.3057 0.3534 -0.0348 0.039 Uiso 1 1 calc R U . . .
C30 C 0.8749(2) 0.7285(2) 0.51215(8) 0.0332(4) Uani 1 1 d . . . . .
H30A H 0.8913 0.6334 0.5011 0.050 Uiso 1 1 calc R U . . .
H30B H 0.8423 0.7262 0.5526 0.050 Uiso 1 1 calc R U . . .
H30C H 0.9663 0.8032 0.5123 0.050 Uiso 1 1 calc R U . . .
C13 C -0.1448(2) 0.7176(2) 0.05329(8) 0.0332(4) Uani 1 1 d . . . . .
H13 H -0.1048 0.8086 0.0745 0.040 Uiso 1 1 calc R U . . .
C14 C -0.2535(2) 0.7039(2) 0.00300(9) 0.0375(4) Uani 1 1 d . . . . .
H14 H -0.2868 0.7874 -0.0089 0.045 Uiso 1 1 calc R U . . .
C15 C -0.3149(2) 0.5691(3) -0.03055(8) 0.0360(4) Uani 1 1 d . . . . .
C22 C 0.4710(3) 0.9579(2) 0.08353(9) 0.0415(5) Uani 1 1 d . . . . .
H22A H 0.5055 0.8836 0.0619 0.062 Uiso 1 1 calc R U . . .
H22B H 0.5418 1.0518 0.0835 0.062 Uiso 1 1 calc R U . . .
H22C H 0.3760 0.9656 0.0633 0.062 Uiso 1 1 calc R U . . .
C16 C -0.4323(2) 0.5596(3) -0.08544(9) 0.0453(5) Uani 1 1 d . . . . .
H16A H -0.3858 0.5656 -0.1230 0.068 Uiso 1 1 calc R U . . .
H16B H -0.4802 0.6402 -0.0822 0.068 Uiso 1 1 calc R U . . .
H16C H -0.5053 0.4670 -0.0860 0.068 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O1 1.4719(11) . ?
S1 O2 1.4487(12) . ?
S1 O3 1.4587(12) . ?
S1 C1 1.7830(16) . ?
S2 C11 1.7614(16) . ?
S2 C18 1.7320(18) . ?
O4 C4 1.229(2) . ?
O5 H5A 0.8500 . ?
O5 H5B 0.8495 . ?
N4 C23 1.5177(19) . ?
N4 C19 1.5214(18) . ?
N4 C27 1.5184(19) . ?
N4 C31 1.5245(19) . ?
N1 H1 0.8600 . ?
N1 C4 1.352(2) . ?
N1 C3 1.455(2) . ?
N2 H2 0.8600 . ?
N2 C5 1.393(2) . ?
N2 C4 1.386(2) . ?
N3 C11 1.301(2) . ?
N3 C12 1.390(2) . ?
C6 H6 0.9300 . ?
C6 C5 1.402(2) . ?
C6 C7 1.384(2) . ?
C5 C10 1.404(2) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C23 1.521(2) . ?
C24 C25 1.527(2) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C27 1.520(2) . ?
C28 C29 1.521(2) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C8 C7 1.398(2) . ?
C8 C9 1.400(2) . ?
C8 C11 1.467(2) . ?
C7 H7 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.521(2) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.528(2) . ?
C32 C31 1.523(2) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.522(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.521(2) . ?
C2 C1 1.524(2) . ?
C10 H10 0.9300 . ?
C10 C9 1.382(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C9 H9 0.9300 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.524(2) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.519(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.526(2) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C18 C12 1.398(3) . ?
C18 C17 1.397(2) . ?
C12 C13 1.402(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.525(3) . ?
C17 H17 0.9300 . ?
C17 C15 1.386(3) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C13 H13 0.9300 . ?
C13 C14 1.387(3) . ?
C14 H14 0.9300 . ?
C14 C15 1.400(3) . ?
C15 C16 1.512(3) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?

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
O1 S1 C1 106.10(7) . . ?
O2 S1 O1 112.07(7) . . ?
O2 S1 O3 113.62(7) . . ?
O2 S1 C1 107.29(7) . . ?
O3 S1 O1 112.00(7) . . ?
O3 S1 C1 105.10(7) . . ?
C18 S2 C11 89.29(8) . . ?
H5A O5 H5B 104.5 . . ?
C23 N4 C19 110.90(11) . . ?
C23 N4 C27 110.86(11) . . ?
C23 N4 C31 106.90(11) . . ?
C19 N4 C31 110.55(11) . . ?
C27 N4 C19 107.24(11) . . ?
C27 N4 C31 110.43(11) . . ?
C4 N1 H1 119.5 . . ?
C4 N1 C3 121.08(13) . . ?
C3 N1 H1 119.5 . . ?
C5 N2 H2 115.7 . . ?
C4 N2 H2 115.7 . . ?
C4 N2 C5 128.53(13) . . ?
C11 N3 C12 111.14(14) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C7 C6 C5 120.05(14) . . ?
N2 C5 C6 124.48(14) . . ?
N2 C5 C10 116.97(14) . . ?
C6 C5 C10 118.53(14) . . ?
H24A C24 H24B 108.3 . . ?
C23 C24 H24A 109.8 . . ?
C23 C24 H24B 109.8 . . ?
C23 C24 C25 109.20(12) . . ?
C25 C24 H24A 109.8 . . ?
C25 C24 H24B 109.8 . . ?
H28A C28 H28B 108.1 . . ?
C27 C28 H28A 109.6 . . ?
C27 C28 H28B 109.6 . . ?
C27 C28 C29 110.20(12) . . ?
C29 C28 H28A 109.6 . . ?
C29 C28 H28B 109.6 . . ?
N4 C23 C24 115.02(12) . . ?
N4 C23 H23A 108.5 . . ?
N4 C23 H23B 108.5 . . ?
C24 C23 H23A 108.5 . . ?
C24 C23 H23B 108.5 . . ?
H23A C23 H23B 107.5 . . ?
C7 C8 C9 117.96(14) . . ?
C7 C8 C11 120.08(15) . . ?
C9 C8 C11 121.93(14) . . ?
O4 C4 N1 123.16(14) . . ?
O4 C4 N2 123.85(14) . . ?
N1 C4 N2 112.98(14) . . ?
C6 C7 C8 121.70(15) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
N4 C19 H19A 108.3 . . ?
N4 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C20 C19 N4 115.85(12) . . ?
C20 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
H32A C32 H32B 108.2 . . ?
C33 C32 H32A 109.7 . . ?
C33 C32 H32B 109.7 . . ?
C31 C32 H32A 109.7 . . ?
C31 C32 H32B 109.7 . . ?
C31 C32 C33 109.61(12) . . ?
N4 C27 C28 114.67(12) . . ?
N4 C27 H27A 108.6 . . ?
N4 C27 H27B 108.6 . . ?
C28 C27 H27A 108.6 . . ?
C28 C27 H27B 108.6 . . ?
H27A C27 H27B 107.6 . . ?
C32 C33 H33A 109.0 . . ?
C32 C33 H33B 109.0 . . ?
H33A C33 H33B 107.8 . . ?
C34 C33 C32 112.77(13) . . ?
C34 C33 H33A 109.0 . . ?
C34 C33 H33B 109.0 . . ?
H2A C2 H2B 108.1 . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
C3 C2 C1 110.86(13) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C5 C10 H10 119.6 . . ?
C9 C10 C5 120.85(15) . . ?
C9 C10 H10 119.6 . . ?
N1 C3 C2 109.86(13) . . ?
N1 C3 H3A 109.7 . . ?
N1 C3 H3B 109.7 . . ?
C2 C3 H3A 109.7 . . ?
C2 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C8 C9 H9 119.6 . . ?
C10 C9 C8 120.90(15) . . ?
C10 C9 H9 119.6 . . ?
N4 C31 H31A 108.5 . . ?
N4 C31 H31B 108.5 . . ?
C32 C31 N4 115.24(12) . . ?
C32 C31 H31A 108.5 . . ?
C32 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?
N3 C11 S2 114.92(12) . . ?
N3 C11 C8 124.76(15) . . ?
C8 C11 S2 120.26(12) . . ?
C24 C25 H25A 109.1 . . ?
C24 C25 H25B 109.1 . . ?
H25A C25 H25B 107.8 . . ?
C26 C25 C24 112.61(13) . . ?
C26 C25 H25A 109.1 . . ?
C26 C25 H25B 109.1 . . ?
C28 C29 H29A 109.2 . . ?
C28 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
C30 C29 C28 111.84(14) . . ?
C30 C29 H29A 109.2 . . ?
C30 C29 H29B 109.2 . . ?
S1 C1 H1A 108.9 . . ?
S1 C1 H1B 108.9 . . ?
C2 C1 S1 113.30(11) . . ?
C2 C1 H1A 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
C19 C20 H20A 109.6 . . ?
C19 C20 H20B 109.6 . . ?
C19 C20 C21 110.34(13) . . ?
H20A C20 H20B 108.1 . . ?
C21 C20 H20A 109.6 . . ?
C21 C20 H20B 109.6 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C12 C18 S2 109.44(12) . . ?
C17 C18 S2 128.74(15) . . ?
C17 C18 C12 121.81(17) . . ?
N3 C12 C18 115.19(15) . . ?
N3 C12 C13 125.52(17) . . ?
C18 C12 C13 119.27(16) . . ?
C20 C21 H21A 109.2 . . ?
C20 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C22 C21 C20 112.15(16) . . ?
C22 C21 H21A 109.2 . . ?
C22 C21 H21B 109.2 . . ?
C18 C17 H17 120.6 . . ?
C15 C17 C18 118.85(19) . . ?
C15 C17 H17 120.6 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C12 C13 H13 120.8 . . ?
C14 C13 C12 118.38(19) . . ?
C14 C13 H13 120.8 . . ?
C13 C14 H14 118.8 . . ?
C13 C14 C15 122.39(18) . . ?
C15 C14 H14 118.8 . . ?
C17 C15 C14 119.28(17) . . ?
C17 C15 C16 120.1(2) . . ?
C14 C15 C16 120.62(19) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 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
S2 C18 C12 N3 1.17(18) . . . . ?
S2 C18 C12 C13 -177.42(14) . . . . ?
S2 C18 C17 C15 177.09(14) . . . . ?
O1 S1 C1 C2 -59.52(13) . . . . ?
O2 S1 C1 C2 60.44(13) . . . . ?
O3 S1 C1 C2 -178.32(12) . . . . ?
N4 C19 C20 C21 -179.03(13) . . . . ?
N2 C5 C10 C9 177.67(14) . . . . ?
N3 C12 C13 C14 -178.82(16) . . . . ?
C6 C5 C10 C9 -0.8(2) . . . . ?
C5 N2 C4 O4 -4.6(3) . . . . ?
C5 N2 C4 N1 176.80(14) . . . . ?
C5 C6 C7 C8 -0.1(2) . . . . ?
C5 C10 C9 C8 0.7(2) . . . . ?
C23 N4 C19 C20 -51.06(17) . . . . ?
C23 N4 C27 C28 58.76(16) . . . . ?
C23 N4 C31 C32 -168.12(12) . . . . ?
C23 C24 C25 C26 170.09(13) . . . . ?
C4 N1 C3 C2 169.85(14) . . . . ?
C4 N2 C5 C6 -4.7(2) . . . . ?
C4 N2 C5 C10 176.93(15) . . . . ?
C7 C6 C5 N2 -177.83(14) . . . . ?
C7 C6 C5 C10 0.6(2) . . . . ?
C7 C8 C9 C10 -0.2(2) . . . . ?
C7 C8 C11 S2 -170.52(12) . . . . ?
C7 C8 C11 N3 6.5(2) . . . . ?
C19 N4 C23 C24 -58.20(16) . . . . ?
C19 N4 C27 C28 179.95(12) . . . . ?
C19 N4 C31 C32 71.08(16) . . . . ?
C19 C20 C21 C22 172.82(15) . . . . ?
C27 N4 C23 C24 60.81(16) . . . . ?
C27 N4 C19 C20 -172.23(12) . . . . ?
C27 N4 C31 C32 -47.44(16) . . . . ?
C27 C28 C29 C30 177.38(14) . . . . ?
C33 C32 C31 N4 -167.68(12) . . . . ?
C3 N1 C4 O4 0.2(2) . . . . ?
C3 N1 C4 N2 178.75(13) . . . . ?
C3 C2 C1 S1 176.28(11) . . . . ?
C9 C8 C7 C6 -0.1(2) . . . . ?
C9 C8 C11 S2 7.3(2) . . . . ?
C9 C8 C11 N3 -175.72(15) . . . . ?
C31 N4 C23 C24 -178.78(12) . . . . ?
C31 N4 C19 C20 67.32(16) . . . . ?
C31 N4 C27 C28 -59.53(16) . . . . ?
C31 C32 C33 C34 175.39(12) . . . . ?
C11 S2 C18 C12 -0.40(12) . . . . ?
C11 S2 C18 C17 -179.52(17) . . . . ?
C11 N3 C12 C18 -1.5(2) . . . . ?
C11 N3 C12 C13 176.96(16) . . . . ?
C11 C8 C7 C6 177.80(14) . . . . ?
C11 C8 C9 C10 -178.03(14) . . . . ?
C25 C24 C23 N4 173.13(12) . . . . ?
C29 C28 C27 N4 166.51(13) . . . . ?
C1 C2 C3 N1 -177.27(13) . . . . ?
C18 S2 C11 N3 -0.46(13) . . . . ?
C18 S2 C11 C8 176.84(13) . . . . ?
C18 C12 C13 C14 -0.4(3) . . . . ?
C18 C17 C15 C14 0.7(3) . . . . ?
C18 C17 C15 C16 -179.18(16) . . . . ?
C12 N3 C11 S2 1.18(18) . . . . ?
C12 N3 C11 C8 -175.98(14) . . . . ?
C12 C18 C17 C15 -1.9(3) . . . . ?
C12 C13 C14 C15 -0.8(3) . . . . ?
C17 C18 C12 N3 -179.64(15) . . . . ?
C17 C18 C12 C13 1.8(3) . . . . ?
C13 C14 C15 C17 0.6(3) . . . . ?
C13 C14 C15 C16 -179.47(18) . . . . ?

_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 1.189
_oxdiff_exptl_absorpt_empirical_full_min 0.863
####################################################################### 
# 
# 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_jrh20200015_res
_database_code_depnum_ccdc_archive 'CCDC 2023004'
loop_
_audit_author_name
_audit_author_address
'jennifer Hiscock'
;University of kent
United Kingdom
;
_audit_update_record             
;
2020-08-12 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_audit_creation_date             2020-08-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C17 H16 N3 O4 S2, 2(C8 H18 N0.5)'
_chemical_formula_sum            'C33 H52 N4 O4 S2'
_chemical_formula_weight         632.90
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H20N2O2S2
_chemical_oxdiff_usercomment     'Nya ethyl linker 100 K'
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           13
_space_group_name_H-M_alt        'P 1 2/n 1'
_space_group_name_Hall           '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   16.4865(13)
_cell_length_b                   10.4507(7)
_cell_length_c                   20.0106(17)
_cell_angle_alpha                90
_cell_angle_beta                 94.596(7)
_cell_angle_gamma                90
_cell_volume                     3436.7(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2618
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      69.4100
_cell_measurement_theta_min      4.4020
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.728
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1368
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 5 0 0.0514
-2 -5 0 0.0514
-1 0 5 0.0073
1 0 -5 0.0073
5 0 1 0.0086
-5 0 -1 0.0086

_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.017
_exptl_crystal_size_min          0.015
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.9889 5.0051 0.0054 0.0101 0.0149 -0.7605
-1.9889 -5.0051 -0.0054 -0.0101 -0.0149 0.7605
-1.0556 0.0113 4.9891 -0.3213 -0.2216 0.0064
1.0556 -0.0113 -4.9891 0.3213 0.2216 -0.0064
4.9814 0.0076 1.0902 -0.2664 0.3841 -0.1133
-4.9814 -0.0076 -1.0902 0.2664 -0.3841 0.1133

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1112
_diffrn_reflns_av_unetI/netI     0.1299
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22331
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.619
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -56.00  10.00   1.00   10.00    --  -42.16  38.00  90.00   66
  2  ω    -68.00  29.00   1.00   10.00    --  -42.16  57.00 -90.00   97
  3  ω   -115.00 -19.00   1.00   10.00    --  -42.16 -57.00 120.00   96
  4  ω    -31.00  -1.00   1.00   10.00    --   42.16 -38.00 -30.00   30
  5  ω     16.00  82.00   1.00   10.00    --   42.16 -99.00   0.00   66
  6  ω     29.00 119.00   1.00   22.50    --  103.72 -30.00  30.00   90
  7  ω    102.00 169.00   1.00   22.50    --  103.72 125.00 -60.00   67
  8  ω     72.00 133.00   1.00   22.50    --  103.72 -61.00 150.00   61
  9  ω     85.00 118.00   1.00   22.50    --  103.72-125.00 -90.00   33
 10  ω     98.00 177.00   1.00   22.50    --  103.72  30.00  60.00   79
 11  ω     84.00 109.00   1.00   22.50    --  103.72 -94.00-120.00   25
 12  ω     92.00 118.00   1.00   22.50    --  103.72-125.00  30.00   26
 13  ω     47.00  73.00   1.00   22.50    --  103.72 -61.00  30.00   26
 14  ω     98.00 125.00   1.00   22.50    --  103.72 -61.00  30.00   27
 15  ω     21.00  47.00   1.00   22.50    --  103.72 -94.00-120.00   26
 16  ω     28.00 136.00   1.00   22.50    --  103.72 -77.00 -60.00  108
 17  ω     75.00 141.00   1.00   22.50    --  103.72  77.00   0.00   66
 18  ω    153.00 178.00   1.00   22.50    --  103.72  77.00   0.00   25
 19  ω     58.00 118.00   1.00   22.50    --  103.72-125.00 150.00   60
 20  ω     22.00 103.00   1.00   22.50    --  103.72 -15.00-120.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0376684000
_diffrn_orient_matrix_UB_12      0.0170742000
_diffrn_orient_matrix_UB_13      -0.0724063000
_diffrn_orient_matrix_UB_21      0.0830153000
_diffrn_orient_matrix_UB_22      -0.0299906000
_diffrn_orient_matrix_UB_23      -0.0267744000
_diffrn_orient_matrix_UB_31      -0.0218745000
_diffrn_orient_matrix_UB_32      -0.1432507000
_diffrn_orient_matrix_UB_33      -0.0030268000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3597
_reflns_number_total             6083
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    ?
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6083
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0622
_refine_ls_restrained_S_all      0.974
_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)+(0.0055P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1341
_refine_special_details          
;
 ?
;
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(H17C)=Sof(H17D)=1-FVAR(1)
 Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=FVAR(1)
 Sof(C30B)=Sof(H30C)=Sof(H30D)=Sof(C31B)=Sof(H31C)=Sof(H31D)=Sof(C26B)=
 Sof(H26C)=Sof(H26D)=Sof(C27B)=Sof(H27C)=Sof(H27D)=Sof(H32C)=Sof(H32D)=
 Sof(H28C)=Sof(H28D)=1-FVAR(2)
 Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(C31A)=
 Sof(H31A)=Sof(H31B)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H32A)=Sof(H32B)=
 Sof(H28B)=Sof(H28A)=FVAR(2)
 Sof(O2A)=Sof(O3A)=1-FVAR(3)
 Sof(O2B)=Sof(O3B)=FVAR(3)
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C22(H22A,H22B), C19(H19A,H19B), C23(H23A,H23B), C20(H20A,
 H20B), C24(H24A,H24B), C16(H16A,H16B), C16(H16C,H16D), C17A(H17A,H17B),
 C17B(H17C,H17D), C30A(H30A,H30B), C26A(H26A,H26B), C31A(H31A,H31B), C27A(H27A,
 H27B), C30B(H30C,H30D), C31B(H31C,H31D), C26B(H26C,H26D), C27B(H27C,H27D),
 C32(H32A,H32B), C32(H32C,H32D), C28(H28B,H28A), C28(H28C,H28D)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C4(H4), C11(H11), C10(H10), C3(H3A), C13(H13), C7(H7), C14(H14)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C25(H25A,H25B,H25C), C21(H21A,H21B,H21C), C33(H33A,H33B,
 H33C), C29(H29A,H29B,H29C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.32882(6) 0.56610(9) 0.54322(5) 0.0319(2) Uani 1 1 d . . . . .
S2 S 0.91390(6) -0.08292(10) 0.70268(5) 0.0377(3) Uani 1 1 d . . . . .
O4 O 0.85369(18) -0.0552(3) 0.75084(14) 0.0420(7) Uani 1 1 d . . . . .
O1 O 0.70225(18) 0.2150(3) 0.57333(15) 0.0441(8) Uani 1 1 d . . . . .
N1 N 0.29581(19) 0.4904(3) 0.66225(15) 0.0279(7) Uani 1 1 d . . . . .
N2 N 0.62338(19) 0.1514(3) 0.65742(16) 0.0305(7) Uani 1 1 d . . . . .
H2 H 0.6232 0.1023 0.6919 0.037 Uiso 1 1 calc R . . . .
N4 N 0.7500 0.5331(4) 0.7500 0.0340(11) Uani 1 2 d S T P . .
N3 N 0.7404(2) 0.0463(3) 0.63866(18) 0.0446(10) Uani 1 1 d . . . . .
H3 H 0.7305 -0.0004 0.6724 0.054 Uiso 1 1 calc R . . . .
C5 C 0.2349(2) 0.5762(3) 0.63970(18) 0.0265(8) Uani 1 1 d . . . . .
C9 C 0.4192(2) 0.3924(3) 0.62629(18) 0.0273(8) Uani 1 1 d . . . . .
C4 C 0.1692(2) 0.6134(3) 0.67543(19) 0.0308(9) Uani 1 1 d . . . . .
H4 H 0.1631 0.5798 0.7178 0.037 Uiso 1 1 calc R . . . .
C11 C 0.5063(2) 0.2542(3) 0.69687(19) 0.0290(8) Uani 1 1 d . . . . .
H11 H 0.5180 0.2139 0.7380 0.035 Uiso 1 1 calc R . . . .
C10 C 0.4395(2) 0.3338(3) 0.68806(19) 0.0295(9) Uani 1 1 d . . . . .
H10 H 0.4077 0.3485 0.7236 0.035 Uiso 1 1 calc R . . . .
C3 C 0.1136(2) 0.7004(4) 0.64722(19) 0.0306(9) Uani 1 1 d . . . . .
H3A H 0.0700 0.7250 0.6711 0.037 Uiso 1 1 calc R . . . .
C15 C 0.6894(2) 0.1421(4) 0.6195(2) 0.0326(9) Uani 1 1 d . . . . .
C8 C 0.3481(2) 0.4768(3) 0.61754(18) 0.0267(8) Uani 1 1 d . . . . .
C13 C 0.5370(2) 0.2914(4) 0.58268(19) 0.0308(9) Uani 1 1 d . . . . .
H13 H 0.5693 0.2781 0.5473 0.037 Uiso 1 1 calc R . . . .
C7 C 0.1866(2) 0.7155(4) 0.54723(19) 0.0317(9) Uani 1 1 d . . . . .
H7 H 0.1928 0.7484 0.5048 0.038 Uiso 1 1 calc R . . . .
C12 C 0.5565(2) 0.2333(3) 0.64495(19) 0.0294(8) Uani 1 1 d . . . . .
C6 C 0.2421(2) 0.6286(3) 0.57604(18) 0.0284(8) Uani 1 1 d . . . . .
C2 C 0.1213(2) 0.7530(4) 0.5827(2) 0.0333(9) Uani 1 1 d . . . . .
C14 C 0.4688(2) 0.3693(3) 0.57460(19) 0.0312(9) Uani 1 1 d . . . . .
H14 H 0.4558 0.4074 0.5331 0.037 Uiso 1 1 calc R . . . .
C18 C 0.6948(3) 0.6218(3) 0.70704(19) 0.0367(10) Uani 1 1 d . . . . .
H18A H 0.7288 0.6771 0.6821 0.044 Uiso 1 1 calc R . . . .
H18B H 0.6660 0.6759 0.7367 0.044 Uiso 1 1 calc R . . . .
C22 C 0.7020(3) 0.4454(3) 0.7926(2) 0.0373(10) Uani 1 1 d . . . . .
H22A H 0.7399 0.3871 0.8164 0.045 Uiso 1 1 calc R . . . .
H22B H 0.6657 0.3944 0.7628 0.045 Uiso 1 1 calc R . . . .
O2B O 0.9434(4) -0.2208(5) 0.7139(6) 0.037(2) Uani 0.59(2) 1 d . . . A 1
C19 C 0.6321(3) 0.5593(4) 0.6573(2) 0.0403(10) Uani 1 1 d . . . . .
H19A H 0.5971 0.5034 0.6810 0.048 Uiso 1 1 calc R . . . .
H19B H 0.6594 0.5081 0.6255 0.048 Uiso 1 1 calc R . . . .
C23 C 0.6518(3) 0.5095(4) 0.8436(2) 0.0463(12) Uani 1 1 d . . . . .
H23A H 0.6169 0.5742 0.8216 0.056 Uiso 1 1 calc R . . . .
H23B H 0.6875 0.5510 0.8778 0.056 Uiso 1 1 calc R . . . .
C1 C 0.0587(3) 0.8456(4) 0.5531(2) 0.0453(11) Uani 1 1 d . . . . .
H1A H 0.0078 0.8020 0.5437 0.068 Uiso 1 1 calc GR . . . .
H1B H 0.0763 0.8803 0.5122 0.068 Uiso 1 1 calc GR . . . .
H1C H 0.0519 0.9138 0.5843 0.068 Uiso 1 1 calc GR . . . .
C20 C 0.5810(3) 0.6629(4) 0.6202(2) 0.0499(12) Uani 1 1 d . . . . .
H20A H 0.5551 0.7145 0.6526 0.060 Uiso 1 1 calc R . . . .
H20B H 0.5384 0.6223 0.5913 0.060 Uiso 1 1 calc R . . . .
C24 C 0.6003(3) 0.4095(4) 0.8756(2) 0.0503(12) Uani 1 1 d . . . . .
H24A H 0.5633 0.3710 0.8411 0.060 Uiso 1 1 calc R . . . .
H24B H 0.6355 0.3425 0.8949 0.060 Uiso 1 1 calc R . . . .
C16 C 0.8120(3) 0.0208(5) 0.6030(3) 0.0598(15) Uani 1 1 d . . . . .
H16A H 0.8481 0.0940 0.6084 0.072 Uiso 0.577(8) 1 calc R . . A 1
H16B H 0.7952 0.0127 0.5556 0.072 Uiso 0.577(8) 1 calc R . . A 1
H16C H 0.8067 -0.0661 0.5862 0.072 Uiso 0.423(8) 1 calc R . . A 2
H16D H 0.8088 0.0766 0.5642 0.072 Uiso 0.423(8) 1 calc R . . A 2
C25 C 0.5514(3) 0.4651(5) 0.9299(2) 0.0607(14) Uani 1 1 d . . . . .
H25A H 0.5167 0.5320 0.9112 0.091 Uiso 1 1 calc GR . . . .
H25B H 0.5878 0.4994 0.9652 0.091 Uiso 1 1 calc GR . . . .
H25C H 0.5187 0.3991 0.9475 0.091 Uiso 1 1 calc GR . . . .
C21 C 0.6308(4) 0.7507(5) 0.5775(2) 0.0700(18) Uani 1 1 d . . . . .
H21A H 0.5945 0.7998 0.5476 0.105 Uiso 1 1 calc GR . . . .
H21B H 0.6656 0.6997 0.5520 0.105 Uiso 1 1 calc GR . . . .
H21C H 0.6633 0.8074 0.6063 0.105 Uiso 1 1 calc GR . . . .
C17A C 0.8577(4) -0.0939(6) 0.6246(3) 0.0318(19) Uani 0.577(8) 1 d . . . A 1
H17A H 0.8948 -0.1144 0.5909 0.038 Uiso 0.577(8) 1 calc R . . A 1
H17B H 0.8197 -0.1645 0.6262 0.038 Uiso 0.577(8) 1 calc R . . A 1
N5 N 0.7500 -0.0478(5) 0.2500 0.0436(13) Uani 1 2 d S T P . .
O3B O 0.9748(7) 0.0039(10) 0.7021(5) 0.041(2) Uani 0.59(2) 1 d . . . A 1
C17B C 0.8877(6) 0.0320(10) 0.6326(5) 0.044(3) Uani 0.423(8) 1 d . . . A 2
H17C H 0.8946 0.1184 0.6498 0.053 Uiso 0.423(8) 1 calc R . . A 2
H17D H 0.9260 0.0203 0.5988 0.053 Uiso 0.423(8) 1 calc R . . A 2
C30A C 0.8160(6) -0.0864(9) 0.2969(4) 0.039(2) Uani 0.498(8) 1 d . . . B 1
H30A H 0.8406 -0.0108 0.3181 0.047 Uiso 0.498(8) 1 calc R . . B 1
H30B H 0.8571 -0.1287 0.2727 0.047 Uiso 0.498(8) 1 calc R . . B 1
C26A C 0.7167(6) 0.0590(10) 0.2978(5) 0.051(3) Uani 0.498(8) 1 d . . . B 1
H26A H 0.7620 0.0926 0.3265 0.061 Uiso 0.498(8) 1 calc R . . B 1
H26B H 0.6941 0.1289 0.2704 0.061 Uiso 0.498(8) 1 calc R . . B 1
C31A C 0.7899(7) -0.1762(10) 0.3512(5) 0.050(3) Uani 0.498(8) 1 d . . . B 1
H31A H 0.7627 -0.2492 0.3295 0.060 Uiso 0.498(8) 1 calc R . . B 1
H31B H 0.7504 -0.1320 0.3762 0.060 Uiso 0.498(8) 1 calc R . . B 1
C27A C 0.6500(6) 0.0088(11) 0.3430(6) 0.066(4) Uani 0.498(8) 1 d . . . B 1
H27A H 0.6093 -0.0399 0.3161 0.079 Uiso 0.498(8) 1 calc R . . B 1
H27B H 0.6745 -0.0466 0.3778 0.079 Uiso 0.498(8) 1 calc R . . B 1
C30B C 0.7772(6) -0.1668(9) 0.2981(5) 0.044(3) Uani 0.502(8) 1 d . . . B 2
H30C H 0.7302 -0.1957 0.3201 0.053 Uiso 0.502(8) 1 calc R . . B 2
H30D H 0.7939 -0.2366 0.2703 0.053 Uiso 0.502(8) 1 calc R . . B 2
C31B C 0.8456(7) -0.1397(9) 0.3515(5) 0.050(3) Uani 0.502(8) 1 d . . . B 2
H31C H 0.8956 -0.1309 0.3294 0.060 Uiso 0.502(8) 1 calc R . . B 2
H31D H 0.8348 -0.0577 0.3716 0.060 Uiso 0.502(8) 1 calc R . . B 2
C26B C 0.6740(6) 0.0021(8) 0.2758(5) 0.041(3) Uani 0.502(8) 1 d . . . B 2
H26C H 0.6467 -0.0678 0.2967 0.049 Uiso 0.502(8) 1 calc R . . B 2
H26D H 0.6383 0.0317 0.2381 0.049 Uiso 0.502(8) 1 calc R . . B 2
C27B C 0.6863(7) 0.1090(9) 0.3254(6) 0.066(4) Uani 0.502(8) 1 d . . . B 2
H27C H 0.6908 0.1892 0.3016 0.080 Uiso 0.502(8) 1 calc R . . B 2
H27D H 0.7367 0.0954 0.3529 0.080 Uiso 0.502(8) 1 calc R . . B 2
C32 C 0.8588(4) -0.2263(7) 0.4015(3) 0.090(2) Uani 1 1 d . . . . .
H32A H 0.8878 -0.2963 0.3822 0.108 Uiso 0.498(8) 1 calc R . . B 1
H32B H 0.8972 -0.1586 0.4144 0.108 Uiso 0.498(8) 1 calc R . . B 1
H32C H 0.9122 -0.2026 0.4215 0.108 Uiso 0.502(8) 1 calc R . . B 2
H32D H 0.8673 -0.3051 0.3774 0.108 Uiso 0.502(8) 1 calc R . . B 2
C33 C 0.8186(6) -0.2683(7) 0.4569(3) 0.141(4) Uani 1 1 d . . . . .
H33A H 0.7882 -0.3444 0.4450 0.211 Uiso 1 1 calc GR . . . .
H33B H 0.7823 -0.2027 0.4699 0.211 Uiso 1 1 calc GR . . . .
H33C H 0.8580 -0.2866 0.4936 0.211 Uiso 1 1 calc GR . . . .
C29 C 0.5747(7) 0.0515(8) 0.4235(4) 0.180(6) Uani 1 1 d . . . . .
H29A H 0.6088 -0.0182 0.4396 0.269 Uiso 1 1 calc GR . . . .
H29B H 0.5231 0.0188 0.4054 0.269 Uiso 1 1 calc GR . . . .
H29C H 0.5665 0.1089 0.4598 0.269 Uiso 1 1 calc GR . . . .
C28 C 0.6127(4) 0.1181(6) 0.3726(4) 0.117(4) Uani 1 1 d . . . . .
H28B H 0.6526 0.1795 0.3909 0.140 Uiso 0.498(8) 1 calc R . . B 1
H28A H 0.5735 0.1605 0.3413 0.140 Uiso 0.498(8) 1 calc R . . B 1
H28C H 0.6228 0.2008 0.3936 0.140 Uiso 0.502(8) 1 calc R . . B 2
H28D H 0.5669 0.1326 0.3399 0.140 Uiso 0.502(8) 1 calc R . . B 2
O2A O 0.9136(8) -0.2008(8) 0.6728(9) 0.041(4) Uani 0.41(2) 1 d . . . A 2
O3A O 0.9980(8) -0.0270(15) 0.7248(9) 0.045(3) Uani 0.41(2) 1 d . . . 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 C8 1.763(4) . ?
S1 C6 1.747(4) . ?
S2 O4 1.467(3) . ?
S2 O2B 1.531(7) . ?
S2 C17A 1.756(7) . ?
S2 O3B 1.354(9) . ?
S2 C17B 1.871(10) . ?
S2 O2A 1.369(7) . ?
S2 O3A 1.536(14) . ?
O1 C15 1.230(5) . ?
N1 C5 1.394(5) . ?
N1 C8 1.299(5) . ?
N2 H2 0.8600 . ?
N2 C15 1.378(5) . ?
N2 C12 1.403(5) . ?
N4 C18 1.517(4) 2_656 ?
N4 C18 1.517(4) . ?
N4 C22 1.517(4) . ?
N4 C22 1.517(4) 2_656 ?
N3 H3 0.8600 . ?
N3 C15 1.343(5) . ?
N3 C16 1.451(5) . ?
C5 C4 1.400(5) . ?
C5 C6 1.400(5) . ?
C9 C10 1.396(5) . ?
C9 C8 1.465(5) . ?
C9 C14 1.391(5) . ?
C4 H4 0.9300 . ?
C4 C3 1.379(5) . ?
C11 H11 0.9300 . ?
C11 C10 1.380(5) . ?
C11 C12 1.397(5) . ?
C10 H10 0.9300 . ?
C3 H3A 0.9300 . ?
C3 C2 1.419(5) . ?
C13 H13 0.9300 . ?
C13 C12 1.401(5) . ?
C13 C14 1.386(5) . ?
C7 H7 0.9300 . ?
C7 C6 1.382(5) . ?
C7 C2 1.393(5) . ?
C2 C1 1.502(6) . ?
C14 H14 0.9300 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.523(5) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.520(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.527(6) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.520(6) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.535(6) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.519(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C16 H16D 0.9700 . ?
C16 C17A 1.462(8) . ?
C16 C17B 1.343(12) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C17A H17A 0.9700 . ?
C17A H17B 0.9700 . ?
N5 C30A 1.437(9) 2_655 ?
N5 C30A 1.437(9) . ?
N5 C26A 1.596(10) 2_655 ?
N5 C26A 1.596(10) . ?
N5 C30B 1.615(10) . ?
N5 C30B 1.615(10) 2_655 ?
N5 C26B 1.487(9) . ?
N5 C26B 1.487(9) 2_655 ?
C17B H17C 0.9700 . ?
C17B H17D 0.9700 . ?
C30A H30A 0.9700 . ?
C30A H30B 0.9700 . ?
C30A C31A 1.522(14) . ?
C26A H26A 0.9700 . ?
C26A H26B 0.9700 . ?
C26A C27A 1.569(15) . ?
C31A H31A 0.9700 . ?
C31A H31B 0.9700 . ?
C31A C32 1.547(12) . ?
C27A H27A 0.9700 . ?
C27A H27B 0.9700 . ?
C27A C28 1.447(11) . ?
C30B H30C 0.9700 . ?
C30B H30D 0.9700 . ?
C30B C31B 1.516(15) . ?
C31B H31C 0.9700 . ?
C31B H31D 0.9700 . ?
C31B C32 1.353(11) . ?
C26B H26C 0.9700 . ?
C26B H26D 0.9700 . ?
C26B C27B 1.497(13) . ?
C27B H27C 0.9700 . ?
C27B H27D 0.9700 . ?
C27B C28 1.600(12) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
C32 H32D 0.9700 . ?
C32 C33 1.408(8) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C29 C28 1.419(10) . ?
C28 H28B 0.9700 . ?
C28 H28A 0.9700 . ?
C28 H28C 0.9700 . ?
C28 H28D 0.9700 . ?

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
C6 S1 C8 88.78(18) . . ?
O4 S2 O2B 108.2(3) . . ?
O4 S2 C17A 105.1(3) . . ?
O4 S2 C17B 103.8(3) . . ?
O4 S2 O3A 112.2(6) . . ?
O2B S2 C17A 102.0(5) . . ?
O3B S2 O4 114.5(4) . . ?
O3B S2 O2B 113.9(5) . . ?
O3B S2 C17A 112.1(5) . . ?
O2A S2 O4 119.1(3) . . ?
O2A S2 C17B 104.9(9) . . ?
O2A S2 O3A 116.1(7) . . ?
O3A S2 C17B 96.9(7) . . ?
C8 N1 C5 110.4(3) . . ?
C15 N2 H2 116.9 . . ?
C15 N2 C12 126.1(3) . . ?
C12 N2 H2 116.9 . . ?
C18 N4 C18 104.7(4) 2_656 . ?
C22 N4 C18 111.8(2) . . ?
C22 N4 C18 111.5(2) . 2_656 ?
C22 N4 C18 111.8(2) 2_656 2_656 ?
C22 N4 C18 111.5(2) 2_656 . ?
C22 N4 C22 105.7(4) 2_656 . ?
C15 N3 H3 119.6 . . ?
C15 N3 C16 120.8(4) . . ?
C16 N3 H3 119.6 . . ?
N1 C5 C4 125.4(3) . . ?
N1 C5 C6 115.8(3) . . ?
C4 C5 C6 118.8(4) . . ?
C10 C9 C8 120.2(3) . . ?
C14 C9 C10 117.9(4) . . ?
C14 C9 C8 121.9(3) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 C5 119.3(3) . . ?
C3 C4 H4 120.3 . . ?
C10 C11 H11 119.5 . . ?
C10 C11 C12 120.9(4) . . ?
C12 C11 H11 119.5 . . ?
C9 C10 H10 119.7 . . ?
C11 C10 C9 120.7(3) . . ?
C11 C10 H10 119.7 . . ?
C4 C3 H3A 119.2 . . ?
C4 C3 C2 121.6(3) . . ?
C2 C3 H3A 119.2 . . ?
O1 C15 N2 124.1(4) . . ?
O1 C15 N3 122.3(4) . . ?
N3 C15 N2 113.6(3) . . ?
N1 C8 S1 116.0(3) . . ?
N1 C8 C9 123.5(3) . . ?
C9 C8 S1 120.5(3) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
C14 C13 C12 119.0(3) . . ?
C6 C7 H7 120.5 . . ?
C6 C7 C2 119.1(4) . . ?
C2 C7 H7 120.5 . . ?
C11 C12 N2 117.9(3) . . ?
C11 C12 C13 119.1(4) . . ?
C13 C12 N2 123.0(3) . . ?
C5 C6 S1 109.1(3) . . ?
C7 C6 S1 128.6(3) . . ?
C7 C6 C5 122.3(3) . . ?
C3 C2 C1 120.0(4) . . ?
C7 C2 C3 118.9(4) . . ?
C7 C2 C1 121.0(4) . . ?
C9 C14 H14 118.8 . . ?
C13 C14 C9 122.4(4) . . ?
C13 C14 H14 118.8 . . ?
N4 C18 H18A 108.1 . . ?
N4 C18 H18B 108.1 . . ?
N4 C18 C19 116.9(3) . . ?
H18A C18 H18B 107.3 . . ?
C19 C18 H18A 108.1 . . ?
C19 C18 H18B 108.1 . . ?
N4 C22 H22A 108.1 . . ?
N4 C22 H22B 108.1 . . ?
N4 C22 C23 116.6(3) . . ?
H22A C22 H22B 107.3 . . ?
C23 C22 H22A 108.1 . . ?
C23 C22 H22B 108.1 . . ?
C18 C19 H19A 109.8 . . ?
C18 C19 H19B 109.8 . . ?
C18 C19 C20 109.4(3) . . ?
H19A C19 H19B 108.2 . . ?
C20 C19 H19A 109.8 . . ?
C20 C19 H19B 109.8 . . ?
C22 C23 H23A 109.8 . . ?
C22 C23 H23B 109.8 . . ?
C22 C23 C24 109.4(3) . . ?
H23A C23 H23B 108.2 . . ?
C24 C23 H23A 109.8 . . ?
C24 C23 H23B 109.8 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C19 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
C19 C20 C21 113.4(4) . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C23 C24 H24A 109.1 . . ?
C23 C24 H24B 109.1 . . ?
H24A C24 H24B 107.8 . . ?
C25 C24 C23 112.6(4) . . ?
C25 C24 H24A 109.1 . . ?
C25 C24 H24B 109.1 . . ?
N3 C16 H16A 108.5 . . ?
N3 C16 H16B 108.5 . . ?
N3 C16 H16C 106.8 . . ?
N3 C16 H16D 106.8 . . ?
N3 C16 C17A 115.2(4) . . ?
H16A C16 H16B 107.5 . . ?
H16C C16 H16D 106.7 . . ?
C17A C16 H16A 108.5 . . ?
C17A C16 H16B 108.5 . . ?
C17B C16 N3 122.1(6) . . ?
C17B C16 H16C 106.8 . . ?
C17B C16 H16D 106.8 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
S2 C17A H17A 108.4 . . ?
S2 C17A H17B 108.4 . . ?
C16 C17A S2 115.6(5) . . ?
C16 C17A H17A 108.4 . . ?
C16 C17A H17B 108.4 . . ?
H17A C17A H17B 107.4 . . ?
C30A N5 C30A 147.3(9) 2_655 . ?
C30A N5 C26A 108.1(5) 2_655 . ?
C30A N5 C26A 94.8(5) 2_655 2_655 ?
C30A N5 C26A 94.8(5) . . ?
C30A N5 C26A 108.1(5) . 2_655 ?
C26A N5 C26A 91.3(8) 2_655 . ?
C30B N5 C30B 79.2(8) 2_655 . ?
C26B N5 C30B 106.0(5) . 2_655 ?
C26B N5 C30B 106.0(5) 2_655 . ?
C26B N5 C30B 105.4(5) . . ?
C26B N5 C30B 105.4(5) 2_655 2_655 ?
C26B N5 C26B 138.9(8) 2_655 . ?
S2 C17B H17C 108.5 . . ?
S2 C17B H17D 108.5 . . ?
C16 C17B S2 115.1(6) . . ?
C16 C17B H17C 108.5 . . ?
C16 C17B H17D 108.5 . . ?
H17C C17B H17D 107.5 . . ?
N5 C30A H30A 108.9 . . ?
N5 C30A H30B 108.9 . . ?
N5 C30A C31A 113.4(8) . . ?
H30A C30A H30B 107.7 . . ?
C31A C30A H30A 108.9 . . ?
C31A C30A H30B 108.9 . . ?
N5 C26A H26A 108.8 . . ?
N5 C26A H26B 108.8 . . ?
H26A C26A H26B 107.7 . . ?
C27A C26A N5 113.7(8) . . ?
C27A C26A H26A 108.8 . . ?
C27A C26A H26B 108.8 . . ?
C30A C31A H31A 108.3 . . ?
C30A C31A H31B 108.3 . . ?
C30A C31A C32 116.0(9) . . ?
H31A C31A H31B 107.4 . . ?
C32 C31A H31A 108.3 . . ?
C32 C31A H31B 108.3 . . ?
C26A C27A H27A 110.1 . . ?
C26A C27A H27B 110.1 . . ?
H27A C27A H27B 108.4 . . ?
C28 C27A C26A 108.2(9) . . ?
C28 C27A H27A 110.1 . . ?
C28 C27A H27B 110.1 . . ?
N5 C30B H30C 108.4 . . ?
N5 C30B H30D 108.4 . . ?
H30C C30B H30D 107.4 . . ?
C31B C30B N5 115.6(8) . . ?
C31B C30B H30C 108.4 . . ?
C31B C30B H30D 108.4 . . ?
C30B C31B H31C 107.9 . . ?
C30B C31B H31D 107.9 . . ?
H31C C31B H31D 107.2 . . ?
C32 C31B C30B 117.5(10) . . ?
C32 C31B H31C 107.9 . . ?
C32 C31B H31D 107.9 . . ?
N5 C26B H26C 108.6 . . ?
N5 C26B H26D 108.6 . . ?
N5 C26B C27B 114.8(8) . . ?
H26C C26B H26D 107.5 . . ?
C27B C26B H26C 108.6 . . ?
C27B C26B H26D 108.6 . . ?
C26B C27B H27C 109.3 . . ?
C26B C27B H27D 109.3 . . ?
C26B C27B C28 111.6(8) . . ?
H27C C27B H27D 108.0 . . ?
C28 C27B H27C 109.3 . . ?
C28 C27B H27D 109.3 . . ?
C31A C32 H32A 110.8 . . ?
C31A C32 H32B 110.8 . . ?
C31B C32 H32C 102.8 . . ?
C31B C32 H32D 102.8 . . ?
C31B C32 C33 137.2(9) . . ?
H32A C32 H32B 108.9 . . ?
H32C C32 H32D 105.0 . . ?
C33 C32 C31A 104.6(7) . . ?
C33 C32 H32A 110.8 . . ?
C33 C32 H32B 110.8 . . ?
C33 C32 H32C 102.8 . . ?
C33 C32 H32D 102.8 . . ?
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 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
C27A C28 H28B 112.2 . . ?
C27A C28 H28A 112.2 . . ?
C27B C28 H28C 101.3 . . ?
C27B C28 H28D 101.3 . . ?
C29 C28 C27A 97.7(8) . . ?
C29 C28 C27B 142.5(9) . . ?
C29 C28 H28B 112.2 . . ?
C29 C28 H28A 112.2 . . ?
C29 C28 H28C 101.3 . . ?
C29 C28 H28D 101.3 . . ?
H28B C28 H28A 109.8 . . ?
H28C C28 H28D 104.6 . . ?

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
O4 S2 C17A C16 59.6(5) . . . . ?
O4 S2 C17B C16 -59.3(8) . . . . ?
N1 C5 C4 C3 179.4(3) . . . . ?
N1 C5 C6 S1 0.4(4) . . . . ?
N1 C5 C6 C7 -179.7(3) . . . . ?
N4 C18 C19 C20 178.5(3) . . . . ?
N4 C22 C23 C24 173.3(3) . . . . ?
N3 C16 C17A S2 -72.8(6) . . . . ?
N3 C16 C17B S2 64.7(9) . . . . ?
C5 N1 C8 S1 -0.2(4) . . . . ?
C5 N1 C8 C9 -179.7(3) . . . . ?
C5 C4 C3 C2 0.1(6) . . . . ?
C4 C5 C6 S1 180.0(3) . . . . ?
C4 C5 C6 C7 -0.1(6) . . . . ?
C4 C3 C2 C7 0.1(6) . . . . ?
C4 C3 C2 C1 178.9(4) . . . . ?
C10 C9 C8 S1 172.4(3) . . . . ?
C10 C9 C8 N1 -8.1(6) . . . . ?
C10 C9 C14 C13 -0.3(6) . . . . ?
C10 C11 C12 N2 179.9(3) . . . . ?
C10 C11 C12 C13 -1.8(6) . . . . ?
C15 N2 C12 C11 -163.7(4) . . . . ?
C15 N2 C12 C13 18.0(6) . . . . ?
C15 N3 C16 C17A -174.0(5) . . . . ?
C15 N3 C16 C17B 116.7(7) . . . . ?
C8 S1 C6 C5 -0.4(3) . . . . ?
C8 S1 C6 C7 179.7(4) . . . . ?
C8 N1 C5 C4 -179.6(4) . . . . ?
C8 N1 C5 C6 -0.1(4) . . . . ?
C8 C9 C10 C11 -180.0(3) . . . . ?
C8 C9 C14 C13 178.8(4) . . . . ?
C12 N2 C15 O1 8.1(7) . . . . ?
C12 N2 C15 N3 -173.3(4) . . . . ?
C12 C11 C10 C9 1.9(6) . . . . ?
C12 C13 C14 C9 0.4(6) . . . . ?
C6 S1 C8 N1 0.4(3) . . . . ?
C6 S1 C8 C9 179.9(3) . . . . ?
C6 C5 C4 C3 -0.1(5) . . . . ?
C6 C7 C2 C3 -0.3(6) . . . . ?
C6 C7 C2 C1 -179.0(4) . . . . ?
C2 C7 C6 S1 -179.8(3) . . . . ?
C2 C7 C6 C5 0.3(6) . . . . ?
C14 C9 C10 C11 -0.8(5) . . . . ?
C14 C9 C8 S1 -6.7(5) . . . . ?
C14 C9 C8 N1 172.7(4) . . . . ?
C14 C13 C12 N2 178.9(4) . . . . ?
C14 C13 C12 C11 0.6(5) . . . . ?
C18 N4 C18 C19 179.4(4) 2_656 . . . ?
C18 N4 C22 C23 54.8(4) 2_656 . . . ?
C18 N4 C22 C23 -62.0(4) . . . . ?
C18 C19 C20 C21 63.2(5) . . . . ?
C22 N4 C18 C19 -59.7(4) . . . . ?
C22 N4 C18 C19 58.4(4) 2_656 . . . ?
C22 N4 C22 C23 176.5(5) 2_656 . . . ?
C22 C23 C24 C25 177.0(4) . . . . ?
O2B S2 C17A C16 172.4(5) . . . . ?
O2B S2 C17B C16 83.1(9) . . . . ?
C16 N3 C15 O1 -3.0(7) . . . . ?
C16 N3 C15 N2 178.4(4) . . . . ?
C17A S2 C17B C16 38.5(6) . . . . ?
C17A C16 C17B S2 -38.0(5) . . . . ?
N5 C30A C31A C32 177.3(7) . . . . ?
N5 C26A C27A C28 -167.8(8) . . . . ?
N5 C30B C31B C32 166.2(7) . . . . ?
N5 C26B C27B C28 -156.1(8) . . . . ?
O3B S2 C17A C16 -65.4(7) . . . . ?
O3B S2 C17B C16 -171.0(9) . . . . ?
C17B S2 C17A C16 -35.0(5) . . . . ?
C17B C16 C17A S2 41.2(6) . . . . ?
C30A N5 C30A C31A -55.0(7) 2_655 . . . ?
C30A N5 C26A C27A 64.8(10) 2_655 . . . ?
C30A N5 C26A C27A -91.6(9) . . . . ?
C30A N5 C30B C31B -178.8(8) 2_655 . . . ?
C30A N5 C30B C31B 15.6(7) . . . . ?
C30A N5 C26B C27B 52.6(11) . . . . ?
C30A N5 C26B C27B -160.5(9) 2_655 . . . ?
C30A C31A C32 C31B 9.4(9) . . . . ?
C30A C31A C32 C33 160.8(8) . . . . ?
C26A N5 C30A C31A 79.9(8) . . . . ?
C26A N5 C30A C31A 172.8(7) 2_655 . . . ?
C26A N5 C26A C27A 160.2(11) 2_655 . . . ?
C26A N5 C30B C31B 52.4(13) 2_655 . . . ?
C26A N5 C30B C31B -62.6(9) . . . . ?
C26A N5 C26B C27B -70.7(9) 2_655 . . . ?
C26A N5 C26B C27B -2.8(9) . . . . ?
C26A C27A C28 C27B -3.2(8) . . . . ?
C26A C27A C28 C29 -164.1(8) . . . . ?
C30B N5 C30A C31A -72.3(8) 2_655 . . . ?
C30B N5 C30A C31A -29.2(7) . . . . ?
C30B N5 C26A C27A -52.4(9) . . . . ?
C30B N5 C26A C27A 40.9(14) 2_655 . . . ?
C30B N5 C30B C31B 154.6(11) 2_655 . . . ?
C30B N5 C26B C27B 176.3(8) 2_655 . . . ?
C30B N5 C26B C27B 93.4(9) . . . . ?
C30B C31B C32 C31A -26.5(8) . . . . ?
C30B C31B C32 C33 -69.4(14) . . . . ?
C26B N5 C30A C31A -173.1(9) 2_655 . . . ?
C26B N5 C30A C31A 49.7(10) . . . . ?
C26B N5 C26A C27A 42.2(9) . . . . ?
C26B N5 C26A C27A -165.4(8) 2_655 . . . ?
C26B N5 C30B C31B -101.6(9) . . . . ?
C26B N5 C30B C31B 51.5(9) 2_655 . . . ?
C26B N5 C26B C27B -45.2(7) 2_655 . . . ?
C26B C27B C28 C27A 34.2(9) . . . . ?
C26B C27B C28 C29 66.5(16) . . . . ?
O2A S2 C17A C16 175.0(6) . . . . ?
O2A S2 C17B C16 66.3(9) . . . . ?
O3A S2 C17A C16 -82.2(9) . . . . ?
O3A S2 C17B C16 -174.3(9) . . . . ?

_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 1.273
_oxdiff_exptl_absorpt_empirical_full_min 0.462
