# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_2016jrh0053_res
_database_code_depnum_ccdc_archive 'CCDC 1562758'
_audit_update_record             
;
2017-09-04 deposited with the CCDC.
2017-09-21 downloaded from the CCDC.
;
_audit_creation_date             2017-09-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C16 H13 N2 O4 S, C16 H11 N2 O6 S, 2(C16 H36 N)'
_chemical_formula_sum            'C64 H96 N6 O10 S2'
_chemical_formula_weight         1173.58
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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                   11.2916(13)
_cell_length_b                   12.5010(13)
_cell_length_c                   23.9203(16)
_cell_angle_alpha                88.359(8)
_cell_angle_beta                 86.588(8)
_cell_angle_gamma                76.689(10)
_cell_volume                     3279.6(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3098
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      66.1440
_cell_measurement_theta_min      3.6090
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1268
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-7 -1 -1 0.0616
-4 -7 5 0.0395
7 -1 3 0.0139
1 7 -6 0.0096
-4 -7 -3 0.0465
1 -1 15 0.0082
4 7 4 0.0125
-1 2 -15 0.0148

_exptl_crystal_size_max          0.107
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.025
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1754
_diffrn_reflns_av_unetI/netI     0.1246
_diffrn_reflns_Laue_measured_fraction_full 0.578
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37401
_diffrn_reflns_point_group_measured_fraction_full 0.578
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         50.435
_diffrn_reflns_theta_min         3.634
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.578
_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     -9.00  16.00   1.00   10.00    --   34.00 102.00  98.42   25
  2  ω      0.00  25.00   1.00   10.00    --   38.00  93.00 -31.67   25
  3  ω   -113.00 -13.00   1.00   10.00    --  -40.62 -57.00  90.00  100
  4  ω   -115.00 -30.00   1.00   10.00    --  -40.62 -38.00   0.00   85
  5  ω    -94.00 -18.00   1.00   10.00    --  -40.62 -38.00-180.00   76
  6  ω    -68.00  29.00   1.00   10.00    --  -40.62  57.00  60.00   97
  7  ω   -112.00 -25.00   1.00   10.00    --  -40.62 -38.00 -90.00   87
  8  ω     23.00  86.00   1.00   10.00    --   40.62-125.00-180.00   63
  9  ω     23.00  83.00   1.00   10.00    --   40.62-125.00 -60.00   60
 10  ω     12.00  37.00   1.00   10.00    --   46.00  83.00-123.06   25
 11  ω     16.00  41.00   1.00   10.00    --   50.00  82.00 157.87   25
 12  ω     16.00  41.00   1.00   10.00    --   50.00  82.00  63.22   25
 13  ω     21.00  46.00   1.00   10.00    --   54.00  79.00 -23.57   25
 14  ω     20.00  45.00   1.00   10.00    --   54.00  81.00 -77.67   25
 15  ω     20.00  45.00   1.00   10.00    --   54.00  81.00  -0.17   25
 16  ω     21.00  46.00   1.00   10.00    --   54.00  79.00 176.49   25
 17  ω     20.00  46.00   1.00   10.00    --   54.00  81.00  91.90   26
 18  ω     33.00  79.00   1.00   10.00    --   66.00  77.00-153.30   46
 19  ω     35.00  60.00   1.00   10.00    --   66.00  76.00-110.99   25
 20  ω     33.00  59.00   1.00   10.00    --   66.00  77.00 -69.87   26
 21  ω    100.00 126.00   1.00   10.00    --   66.00  77.00 -69.87   26
 22  ω     34.00  61.00   1.00   10.00    --   66.00  76.00 124.95   27
 23  ω    100.00 137.00   1.00   10.00    --   70.00  76.00  95.68   37
 24  ω     38.00  71.00   1.00   10.00    --   70.00  76.00  95.68   33
 25  ω     39.00  69.00   1.00   10.00    --   70.00  76.00 -47.88   30
 26  ω     38.00  96.00   1.00   10.00    --   70.00  76.00 162.48   58
 27  ω    110.00 143.00   1.00   10.00    --   70.00  77.00   1.68   33
 28  ω     37.00  64.00   1.00   10.00    --   70.00  77.00   1.68   27
 29  ω     41.00  73.00   1.00   20.00    --   74.00  77.00  34.15   32
 30  ω    102.00 128.00   1.00   20.00    --   74.00  77.00  34.15   26
 31  ω     73.00 148.00   1.00   20.00    --  105.19  77.00 -90.00   75
 32  ω     32.00 116.00   1.00   20.00    --  105.19-111.00-120.00   84
 33  ω     53.00 112.00   1.00   20.00    --  105.19-111.00  60.00   59
 34  ω     76.00 107.00   1.00   20.00    --  105.19  61.00-120.00   31
 35  ω     55.00  98.00   1.00   20.00    --  105.19 -94.00 -30.00   43
 36  ω     77.00 111.00   1.00   20.00    --  105.19  61.00 120.00   34
 37  ω     76.00 103.00   1.00   20.00    --  105.19  61.00 -60.00   27
 38  ω     29.00 100.00   1.00   20.00    --  105.19 -94.00 150.00   71
 39  ω     73.00 143.00   1.00   20.00    --  105.19  77.00  30.00   70
 40  ω    109.00 178.00   1.00   20.00    --  105.19  77.00 -60.00   69
 41  ω     73.00 100.00   1.00   20.00    --  105.19  77.00 -60.00   27
 42  ω     73.00 177.00   1.00   20.00    --  105.19  77.00   0.00  104
 43  ω     76.00 103.00   1.00   20.00    --  105.19  61.00 -30.00   27
 44  ω     73.00 176.00   1.00   20.00    --  105.19  77.00 120.00  103
 45  ω     73.00 147.00   1.00   20.00    --  105.19  77.00 -30.00   74
 46  ω     73.00 175.00   1.00   20.00    --  105.19  77.00 150.00  102
 47  ω     73.00 178.00   1.00   20.00    --  105.19  77.00  60.00  105
 48  ω     73.00 177.00   1.00   20.00    --  105.19  77.00-120.00  104
 49  ω     79.00 106.00   1.00   20.00    --  105.19  61.00-150.00   27
 50  ω    127.00 153.00   1.00   20.00    --  105.19  61.00-150.00   26
 51  ω    110.00 160.00   1.00   20.00    --  105.19  77.00-180.00   50
 52  ω     23.00  94.00   1.00   20.00    --  105.19 -94.00  90.00   71
 53  ω     73.00  98.00   1.00   20.00    --  105.19  77.00-180.00   25
 54  ω     31.00  95.00   1.00   20.00    --  105.19 -94.00 -90.00   64
 55  ω    115.00 175.00   1.00   20.00    --  105.19  77.00  90.00   60
 56  ω     73.00  99.00   1.00   20.00    --  105.19  77.00  90.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3357
_reflns_number_total             6864
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.460
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         6864
_refine_ls_number_restraints     223
_refine_ls_R_factor_all          0.2097
_refine_ls_R_factor_gt           0.1405
_refine_ls_restrained_S_all      1.476
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3336
_refine_ls_wR_factor_ref         0.3767
_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. Restrained distances
 N5-C33 \\sim N5-C45 \\sim N5-C37 \\sim N5-C41 \\sim N62_$1-C49_$1 \\sim
N62_$1-C53_$1 \\sim N62_$1-
 C57_$1 \\sim N62_$1-C61_$1
 with sigma of 0.002
 C58-C57 \\sim C59-C58 \\sim C49-C50 \\sim C51-C50 \\sim C53-C54 \\sim C55-C54
\\sim C63A-C62A \\sim C63B-
 C62B \\sim C61-C62B \\sim C61-C62A
 with sigma of 0.002
 C64A-C63A \\sim C55-C56 \\sim C44-C43 \\sim C36-C35 \\sim C60-C59 \\sim
C48-C47 \\sim C51-C52 \\sim C39-
 C40 \\sim C63B-C64B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C56 \\sim N62 \\sim C49 \\sim C53 \\sim C61 \\sim C57 \\sim C50 \\sim C54 \\sim
C62A \\sim C62B \\sim C58 \\sim C51 \\sim C55 \\sim C63A \\sim C63B \\sim C59
\\sim C52 \\sim C64A \\sim C64B \\sim C60: within 2A with sigma of 0.008 and
sigma for terminal atoms of 0.004
Uanis(C62A) = Uanis(C62B)
Uanis(C63A) = Uanis(C64B)
Uanis(C64A) = Uanis(C63B)
4. Others
 Sof(H61A)=Sof(H61B)=Sof(C62B)=Sof(H62C)=Sof(H62D)=Sof(C64B)=Sof(H64D)=
 Sof(H64E)=Sof(H64F)=Sof(C63B)=Sof(H63C)=Sof(H63D)=1-FVAR(1)
 Sof(H61C)=Sof(H61D)=Sof(C63A)=Sof(H63A)=Sof(H63B)=Sof(C64A)=Sof(H64A)=
 Sof(H64B)=Sof(H64C)=Sof(C62A)=Sof(H62A)=Sof(H62B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C17(H17A,H17B), C45(H45A,H45B), C34(H34A,H34B), C33(H33A,H33B),
 C37(H37A,H37B), C35(H35A,H35B), C41(H41A,H41B), C42(H42A,H42B), C47(H47A,H47B),
  C38(H38A,H38B), C46(H46A,H46B), C43(H43A,H43B), C39(H39A,H39B), C54(H54A,
 H54B), C50(H50A,H50B), C49(H49A,H49B), C55(H55A,H55B), C51(H51A,H51B),
 C53(H53A,H53B), C61(H61C,H61D), C61(H61A,H61B), C58(H58A,H58B), C59(H59A,H59B),
  C57(H57A,H57B), C63A(H63A,H63B), C62A(H62A,H62B), C62B(H62C,H62D), C63B(H63C,
 H63D)
5.b Me refined with riding coordinates:
 C52(H52A,H52B,H52C), C56(H56A,H56B,H56C), C64A(H64A,H64B,H64C), C64B(H64D,
 H64E,H64F), C60(H60A,H60B,H60C)
5.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C4(H4), N4(H4A), C9(H9), N3(H3), C24(H24), C10(H10), C8(H8),
 C15(H15), C21(H21), C16(H16), C7(H7), C20(H20), C13(H13), C14(H14), C29(H29),
 C31(H31), C32(H32), C30(H30)
5.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C44(H44A,H44B,H44C), C48(H48A,H48B,H48C), C40(H40A,H40B,
 H40C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.9271(3) 0.3961(3) 0.32960(14) 0.0743(10) Uani 1 1 d . . . . .
S2 S 0.6719(3) 0.1116(4) 0.38157(17) 0.0983(13) Uani 1 1 d . . . . .
O1 O 0.6948(7) 0.4452(6) 0.2201(3) 0.070(2) Uani 1 1 d . . . . .
O4 O 0.9652(6) 0.3519(6) 0.2732(3) 0.071(2) Uani 1 1 d . . . . .
N2 N 0.6308(8) 0.2859(7) 0.2401(4) 0.064(3) Uani 1 1 d . . . . .
H2 H 0.6157 0.2432 0.2671 0.077 Uiso 1 1 calc R . . . .
O3 O 0.9796(7) 0.4866(6) 0.3428(3) 0.084(3) Uani 1 1 d . . . . .
O9 O 0.6183(7) 0.1185(7) 0.3275(4) 0.094(3) Uani 1 1 d . . . . .
O2 O 0.9418(7) 0.3076(7) 0.3722(3) 0.080(2) Uani 1 1 d . . . . .
N1 N 0.7032(8) 0.3739(7) 0.3103(4) 0.064(3) Uani 1 1 d . . . . .
H1 H 0.6802 0.3282 0.3337 0.077 Uiso 1 1 calc R . . . .
O10 O 0.6694(8) 0.2224(8) 0.4036(4) 0.096(3) Uani 1 1 d . . . . .
C2 C 0.6784(10) 0.3720(10) 0.2545(6) 0.066(3) Uani 1 1 d . . . . .
C6 C 0.5354(9) 0.1884(9) 0.0850(5) 0.062(3) Uani 1 1 d . . . . .
C3 C 0.6037(9) 0.2590(9) 0.1864(5) 0.056(3) Uani 1 1 d . . . . .
C4 C 0.6082(9) 0.3208(8) 0.1396(5) 0.061(3) Uani 1 1 d . . . . .
H4 H 0.6307 0.3875 0.1418 0.073 Uiso 1 1 calc R . . . .
N4 N 0.9219(8) 0.1512(8) 0.2357(6) 0.082(3) Uani 1 1 d . . . . .
H4A H 0.9532 0.2012 0.2488 0.098 Uiso 1 1 calc R . . . .
C9 C 0.5067(9) 0.1553(9) 0.0321(6) 0.071(4) Uani 1 1 d . . . . .
H9 H 0.4801 0.0905 0.0301 0.085 Uiso 1 1 calc R . . . .
N3 N 0.8867(9) 0.1046(9) 0.3303(6) 0.094(4) Uani 1 1 d . . . . .
H3 H 0.9228 0.1543 0.3398 0.113 Uiso 1 1 calc R . . . .
C5 C 0.5791(9) 0.2867(8) 0.0866(6) 0.064(3) Uani 1 1 d . . . . .
C12 C 0.5169(10) 0.2159(11) -0.0169(5) 0.068(3) Uani 1 1 d . . . . .
C23 C 0.8675(10) 0.0855(10) 0.0898(7) 0.073(4) Uani 1 1 d . . . . .
O5 O 0.8623(8) -0.0073(7) 0.2596(4) 0.099(3) Uani 1 1 d . . . . .
C25 C 0.8260(11) 0.0023(11) 0.0607(8) 0.086(4) Uani 1 1 d . . . . .
C22 C 0.8902(10) 0.1778(10) 0.0633(6) 0.074(4) Uani 1 1 d . . . . .
C24 C 0.8776(10) 0.0753(10) 0.1473(8) 0.088(5) Uani 1 1 d . . . . .
H24 H 0.8606 0.0138 0.1660 0.106 Uiso 1 1 calc R . . . .
C19 C 0.9126(10) 0.1545(10) 0.1777(7) 0.073(4) Uani 1 1 d . . . . .
C10 C 0.5903(10) 0.3463(9) 0.0367(5) 0.068(3) Uani 1 1 d . . . . .
H10 H 0.6183 0.4105 0.0381 0.082 Uiso 1 1 calc R . . . .
C11 C 0.5614(10) 0.3135(9) -0.0143(5) 0.062(3) Uani 1 1 d . . . . .
C8 C 0.5610(10) 0.1604(9) 0.1839(6) 0.069(3) Uani 1 1 d . . . . .
H8 H 0.5532 0.1197 0.2165 0.083 Uiso 1 1 calc R . . . .
C1 C 0.7662(9) 0.4508(9) 0.3293(5) 0.067(3) Uani 1 1 d . . . . .
H1A H 0.7353 0.4729 0.3669 0.081 Uiso 1 1 calc R . . . .
H1B H 0.7504 0.5157 0.3053 0.081 Uiso 1 1 calc R . . . .
O6 O 0.7982(10) -0.0794(8) 0.0889(5) 0.127(4) Uani 1 1 d . . . . .
C26 C 0.8758(11) 0.1899(11) 0.0025(7) 0.082(4) Uani 1 1 d . . . . .
O7 O 0.8927(9) 0.2737(9) -0.0239(4) 0.111(3) Uani 1 1 d . . . . .
C15 C 0.5394(12) 0.3421(13) -0.1143(6) 0.092(4) Uani 1 1 d . . . . .
H15 H 0.5488 0.3833 -0.1466 0.110 Uiso 1 1 calc R . . . .
C21 C 0.9270(11) 0.2545(10) 0.0942(7) 0.081(4) Uani 1 1 d . . . . .
H21 H 0.9449 0.3158 0.0757 0.097 Uiso 1 1 calc R . . . .
C27 C 0.8392(11) 0.1049(11) -0.0288(8) 0.086(5) Uani 1 1 d . . . . .
C28 C 0.8195(11) 0.0107(11) 0.0004(8) 0.087(5) Uani 1 1 d . . . . .
C16 C 0.5715(11) 0.3729(11) -0.0639(6) 0.084(4) Uani 1 1 d . . . . .
H16 H 0.6014 0.4362 -0.0627 0.101 Uiso 1 1 calc R . . . .
C7 C 0.5323(10) 0.1259(9) 0.1353(6) 0.079(4) Uani 1 1 d . . . . .
H7 H 0.5095 0.0591 0.1344 0.094 Uiso 1 1 calc R . . . .
C20 C 0.9382(11) 0.2445(10) 0.1496(6) 0.078(4) Uani 1 1 d . . . . .
H20 H 0.9631 0.2982 0.1689 0.093 Uiso 1 1 calc R . . . .
C18 C 0.8881(11) 0.0788(11) 0.2753(8) 0.084(4) Uani 1 1 d . . . . .
O8 O 0.6280(9) 0.0379(9) 0.4209(4) 0.125(4) Uani 1 1 d . . . . .
C13 C 0.4799(11) 0.1885(12) -0.0699(7) 0.087(4) Uani 1 1 d . . . . .
H13 H 0.4462 0.1275 -0.0718 0.104 Uiso 1 1 calc R . . . .
C14 C 0.4916(13) 0.2469(12) -0.1170(6) 0.091(4) Uani 1 1 d . . . . .
H14 H 0.4687 0.2254 -0.1508 0.109 Uiso 1 1 calc R . . . .
C29 C 0.7863(12) -0.0697(12) -0.0304(9) 0.110(6) Uani 1 1 d . . . . .
H29 H 0.7712 -0.1320 -0.0118 0.132 Uiso 1 1 calc R . . . .
C31 C 0.7948(13) 0.0338(15) -0.1173(8) 0.117(6) Uani 1 1 d . . . . .
H31 H 0.7862 0.0423 -0.1557 0.141 Uiso 1 1 calc R . . . .
C32 C 0.8282(13) 0.1131(13) -0.0851(8) 0.104(5) Uani 1 1 d . . . . .
H32 H 0.8438 0.1753 -0.1035 0.125 Uiso 1 1 calc R . . . .
C30 C 0.7753(12) -0.0602(13) -0.0869(8) 0.102(6) Uani 1 1 d . . . . .
H30 H 0.7545 -0.1166 -0.1059 0.123 Uiso 1 1 calc R . . . .
C17 C 0.8251(11) 0.0493(10) 0.3732(6) 0.096(5) Uani 1 1 d . . . . .
H17A H 0.8630 0.0500 0.4085 0.116 Uiso 1 1 calc R . . . .
H17B H 0.8341 -0.0268 0.3629 0.116 Uiso 1 1 calc R . . . .
N62 N 0.2863(12) 0.2778(13) 0.4356(6) 0.182(4) Uani 1 1 d D U . . .
N5 N -0.0410(6) 0.6542(5) 0.1869(3) 0.068(3) Uani 1 1 d D . . . .
C45 C 0.0432(10) 0.5422(7) 0.1947(5) 0.073(3) Uani 1 1 d D . . . .
H45A H -0.0008 0.4863 0.1874 0.088 Uiso 1 1 calc R . . . .
H45B H 0.0647 0.5337 0.2335 0.088 Uiso 1 1 calc R . . . .
C34 C -0.2480(9) 0.7675(8) 0.2258(5) 0.061(3) Uani 1 1 d . . . . .
H34A H -0.2116 0.8248 0.2388 0.073 Uiso 1 1 calc R . . . .
H34B H -0.2742 0.7872 0.1883 0.073 Uiso 1 1 calc R . . . .
C33 C -0.1544(8) 0.6593(8) 0.2247(4) 0.064(3) Uani 1 1 d D . . . .
H33A H -0.1937 0.6027 0.2133 0.077 Uiso 1 1 calc R . . . .
H33B H -0.1295 0.6413 0.2626 0.077 Uiso 1 1 calc R . . . .
C37 C 0.0224(11) 0.7441(9) 0.1999(7) 0.094(5) Uani 1 1 d D . . . .
H37A H 0.0980 0.7336 0.1771 0.113 Uiso 1 1 calc R . . . .
H37B H -0.0286 0.8143 0.1891 0.113 Uiso 1 1 calc R . . . .
C35 C -0.3554(11) 0.7592(8) 0.2637(5) 0.079(4) Uani 1 1 d D . . . .
H35A H -0.3270 0.7345 0.3004 0.095 Uiso 1 1 calc R . . . .
H35B H -0.3925 0.7035 0.2495 0.095 Uiso 1 1 calc R . . . .
C41 C -0.0771(12) 0.6779(10) 0.1271(4) 0.082(4) Uani 1 1 d D . . . .
H41A H -0.1327 0.7496 0.1255 0.098 Uiso 1 1 calc R . . . .
H41B H -0.0047 0.6819 0.1039 0.098 Uiso 1 1 calc R . . . .
C42 C -0.1348(13) 0.5976(11) 0.1030(5) 0.091(4) Uani 1 1 d . . . . .
H42A H -0.2110 0.5957 0.1235 0.110 Uiso 1 1 calc R . . . .
H42B H -0.0816 0.5247 0.1039 0.110 Uiso 1 1 calc R . . . .
C47 C 0.2351(14) 0.4013(11) 0.1629(6) 0.104(5) Uani 1 1 d D . . . .
H47A H 0.1841 0.3495 0.1591 0.125 Uiso 1 1 calc R . . . .
H47B H 0.3017 0.3864 0.1346 0.125 Uiso 1 1 calc R . . . .
C36 C -0.4513(12) 0.8641(10) 0.2703(6) 0.107(5) Uani 1 1 d D . . . .
H36A H -0.4849 0.8864 0.2347 0.160 Uiso 1 1 calc GR . . . .
H36B H -0.4154 0.9205 0.2836 0.160 Uiso 1 1 calc GR . . . .
H36C H -0.5148 0.8526 0.2966 0.160 Uiso 1 1 calc GR . . . .
C38 C 0.0499(13) 0.7490(10) 0.2587(7) 0.109(5) Uani 1 1 d . . . . .
H38A H 0.0843 0.6749 0.2718 0.131 Uiso 1 1 calc R . . . .
H38B H -0.0262 0.7755 0.2803 0.131 Uiso 1 1 calc R . . . .
C46 C 0.1595(12) 0.5217(11) 0.1575(6) 0.103(5) Uani 1 1 d . . . . .
H46A H 0.2088 0.5716 0.1676 0.124 Uiso 1 1 calc R . . . .
H46B H 0.1391 0.5371 0.1188 0.124 Uiso 1 1 calc R . . . .
C43 C -0.1575(14) 0.6383(12) 0.0412(7) 0.119(6) Uani 1 1 d D . . . .
H43A H -0.2044 0.7138 0.0412 0.142 Uiso 1 1 calc R . . . .
H43B H -0.0799 0.6364 0.0210 0.142 Uiso 1 1 calc R . . . .
C44 C -0.2231(15) 0.5695(11) 0.0128(7) 0.135(6) Uani 1 1 d D . . . .
H44A H -0.2321 0.5936 -0.0255 0.203 Uiso 1 1 calc GR . . . .
H44B H -0.3022 0.5754 0.0312 0.203 Uiso 1 1 calc GR . . . .
H44C H -0.1782 0.4943 0.0140 0.203 Uiso 1 1 calc GR . . . .
C39 C 0.1391(15) 0.8228(13) 0.2717(9) 0.171(10) Uani 1 1 d D . . . .
H39A H 0.2186 0.7888 0.2548 0.206 Uiso 1 1 calc R . . . .
H39B H 0.1118 0.8929 0.2526 0.206 Uiso 1 1 calc R . . . .
C48 C 0.2819(17) 0.3940(17) 0.2198(7) 0.186(10) Uani 1 1 d D . . . .
H48A H 0.3304 0.4471 0.2230 0.279 Uiso 1 1 calc GR . . . .
H48B H 0.3310 0.3215 0.2262 0.279 Uiso 1 1 calc GR . . . .
H48C H 0.2146 0.4087 0.2471 0.279 Uiso 1 1 calc GR . . . .
C40 C 0.1565(18) 0.8468(16) 0.3329(9) 0.217(13) Uani 1 1 d D . . . .
H40A H 0.2332 0.8665 0.3355 0.326 Uiso 1 1 calc GR . . . .
H40B H 0.1553 0.7824 0.3556 0.326 Uiso 1 1 calc GR . . . .
H40C H 0.0917 0.9064 0.3459 0.326 Uiso 1 1 calc GR . . . .
C54 C 0.2470(12) 0.1912(14) 0.3458(6) 0.145(4) Uani 1 1 d D U . . .
H54A H 0.1734 0.1711 0.3610 0.174 Uiso 1 1 calc R . . . .
H54B H 0.2250 0.2630 0.3278 0.174 Uiso 1 1 calc R . . . .
C50 C 0.3600(14) 0.4181(14) 0.3749(8) 0.173(5) Uani 1 1 d D U . . .
H50A H 0.4335 0.4077 0.3954 0.208 Uiso 1 1 calc R . . . .
H50B H 0.3761 0.3702 0.3428 0.208 Uiso 1 1 calc R . . . .
C49 C 0.2540(14) 0.3945(14) 0.4129(8) 0.171(4) Uani 1 1 d D U . . .
H49A H 0.2366 0.4456 0.4437 0.205 Uiso 1 1 calc R . . . .
H49B H 0.1815 0.4050 0.3916 0.205 Uiso 1 1 calc R . . . .
C55 C 0.3172(13) 0.1049(14) 0.3040(7) 0.149(4) Uani 1 1 d D U . . .
H55A H 0.3939 0.1228 0.2917 0.179 Uiso 1 1 calc R . . . .
H55B H 0.3350 0.0330 0.3221 0.179 Uiso 1 1 calc R . . . .
C51 C 0.3166(16) 0.5388(15) 0.3564(9) 0.187(5) Uani 1 1 d D U . . .
H51A H 0.2430 0.5470 0.3361 0.224 Uiso 1 1 calc R . . . .
H51B H 0.2967 0.5845 0.3893 0.224 Uiso 1 1 calc R . . . .
C53 C 0.3359(14) 0.1911(15) 0.3920(6) 0.161(4) Uani 1 1 d D U . . .
H53A H 0.3535 0.1193 0.4102 0.193 Uiso 1 1 calc R . . . .
H53B H 0.4118 0.2037 0.3751 0.193 Uiso 1 1 calc R . . . .
C61 C 0.1709(15) 0.2657(17) 0.4682(8) 0.193(5) Uani 1 1 d D U . . .
H61C H 0.1858 0.1946 0.4871 0.231 Uiso 0.548(8) 1 calc R . P A -1
H61D H 0.1074 0.2681 0.4423 0.231 Uiso 0.548(8) 1 calc R . P A -1
H61A H 0.1017 0.3026 0.4473 0.231 Uiso 0.452(8) 1 calc R . P A -2
H61B H 0.1656 0.3037 0.5034 0.231 Uiso 0.452(8) 1 calc R . P A -2
C52 C 0.4122(15) 0.5781(16) 0.3194(9) 0.190(5) Uani 1 1 d D U . . .
H52A H 0.4058 0.5592 0.2813 0.284 Uiso 1 1 calc R . . . .
H52B H 0.4918 0.5436 0.3314 0.284 Uiso 1 1 calc R . . . .
H52C H 0.3995 0.6564 0.3221 0.284 Uiso 1 1 calc R . . . .
C58 C 0.3708(19) 0.289(2) 0.5370(8) 0.254(6) Uani 1 1 d D U . . .
H58A H 0.3283 0.2363 0.5540 0.305 Uiso 1 1 calc R . . . .
H58B H 0.3165 0.3614 0.5413 0.305 Uiso 1 1 calc R . . . .
C56 C 0.2410(13) 0.1031(14) 0.2539(7) 0.150(4) Uani 1 1 d D U . . .
H56A H 0.2902 0.0599 0.2249 0.225 Uiso 1 1 calc R . . . .
H56B H 0.2114 0.1769 0.2403 0.225 Uiso 1 1 calc R . . . .
H56C H 0.1732 0.0715 0.2650 0.225 Uiso 1 1 calc R . . . .
C59 C 0.483(2) 0.287(2) 0.5711(11) 0.276(6) Uani 1 1 d D U . . .
H59A H 0.5189 0.3472 0.5585 0.331 Uiso 1 1 calc R . . . .
H59B H 0.4560 0.2986 0.6102 0.331 Uiso 1 1 calc R . . . .
C57 C 0.3905(15) 0.266(2) 0.4740(7) 0.219(5) Uani 1 1 d D U . . .
H57A H 0.4421 0.3128 0.4585 0.262 Uiso 1 1 calc R . . . .
H57B H 0.4379 0.1908 0.4706 0.262 Uiso 1 1 calc R . . . .
C63A C 0.030(3) 0.378(3) 0.5607(13) 0.199(6) Uani 0.548(8) 1 d D U P A -1
H63A H 0.0347 0.4415 0.5819 0.239 Uiso 0.548(8) 1 calc R . P A -1
H63B H -0.0522 0.3878 0.5478 0.239 Uiso 0.548(8) 1 calc R . P A -1
C64A C 0.066(3) 0.273(3) 0.5941(16) 0.199(6) Uani 0.548(8) 1 d D U P A -1
H64A H 0.0396 0.2156 0.5764 0.299 Uiso 0.548(8) 1 calc R . P A -1
H64B H 0.0289 0.2836 0.6313 0.299 Uiso 0.548(8) 1 calc R . P A -1
H64C H 0.1531 0.2539 0.5959 0.299 Uiso 0.548(8) 1 calc R . P A -1
C62A C 0.126(3) 0.356(3) 0.5118(11) 0.199(5) Uani 0.548(8) 1 d D U P A -1
H62A H 0.2005 0.3603 0.5293 0.238 Uiso 0.548(8) 1 calc R . P A -1
H62B H 0.1057 0.4226 0.4890 0.238 Uiso 0.548(8) 1 calc R . P A -1
C62B C 0.159(3) 0.1473(19) 0.481(2) 0.199(5) Uani 0.452(8) 1 d D U P A -2
H62C H 0.1972 0.1075 0.4480 0.238 Uiso 0.452(8) 1 calc R . P A -2
H62D H 0.2160 0.1230 0.5104 0.238 Uiso 0.452(8) 1 calc R . P A -2
C64B C 0.069(4) -0.030(3) 0.492(2) 0.199(6) Uani 0.452(8) 1 d D U P A -2
H64D H 0.1384 -0.0572 0.4670 0.298 Uiso 0.452(8) 1 calc R . P A -2
H64E H -0.0025 -0.0444 0.4775 0.298 Uiso 0.452(8) 1 calc R . P A -2
H64F H 0.0825 -0.0648 0.5281 0.298 Uiso 0.452(8) 1 calc R . P A -2
C63B C 0.053(3) 0.093(3) 0.498(2) 0.199(6) Uani 0.452(8) 1 d D U P A -2
H63C H 0.0293 0.1104 0.5369 0.239 Uiso 0.452(8) 1 calc R . P A -2
H63D H -0.0151 0.1287 0.4762 0.239 Uiso 0.452(8) 1 calc R . P A -2
C60 C 0.578(2) 0.181(2) 0.5662(11) 0.279(7) Uani 1 1 d D U . . .
H60A H 0.5387 0.1210 0.5648 0.418 Uiso 1 1 calc R . . . .
H60B H 0.6271 0.1722 0.5980 0.418 Uiso 1 1 calc R . . . .
H60C H 0.6281 0.1835 0.5326 0.418 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O4 1.474(8) . ?
S1 O3 1.443(7) . ?
S1 O2 1.470(8) . ?
S1 C1 1.788(11) . ?
S2 O9 1.452(9) . ?
S2 O10 1.490(10) . ?
S2 O8 1.444(9) . ?
S2 C17 1.729(13) . ?
O1 C2 1.251(13) . ?
N2 C2 1.370(13) . ?
N2 C3 1.405(13) . ?
N1 C2 1.383(14) . ?
N1 C1 1.420(13) . ?
C6 C9 1.421(16) . ?
C6 C5 1.428(14) . ?
C6 C7 1.419(16) . ?
C3 C4 1.347(14) . ?
C3 C8 1.428(14) . ?
C4 C5 1.428(15) . ?
N4 C19 1.395(15) . ?
N4 C18 1.390(16) . ?
C9 C12 1.390(16) . ?
N3 C18 1.361(17) . ?
N3 C17 1.453(15) . ?
C5 C10 1.405(15) . ?
C12 C11 1.427(15) . ?
C12 C13 1.433(17) . ?
C23 C25 1.445(17) . ?
C23 C22 1.368(16) . ?
C23 C24 1.389(17) . ?
O5 C18 1.252(15) . ?
C25 O6 1.296(17) . ?
C25 C28 1.447(19) . ?
C22 C26 1.474(18) . ?
C22 C21 1.378(16) . ?
C24 C19 1.386(17) . ?
C19 C20 1.373(16) . ?
C10 C11 1.377(15) . ?
C11 C16 1.396(16) . ?
C8 C7 1.334(16) . ?
C26 O7 1.254(15) . ?
C26 C27 1.464(17) . ?
C15 C16 1.370(16) . ?
C15 C14 1.420(17) . ?
C21 C20 1.338(17) . ?
C27 C28 1.407(19) . ?
C27 C32 1.359(19) . ?
C28 C29 1.394(18) . ?
C13 C14 1.340(17) . ?
C29 C30 1.36(2) . ?
C31 C32 1.402(18) . ?
C31 C30 1.42(2) . ?
N62 C49 1.514(5) . ?
N62 C53 1.514(5) . ?
N62 C61 1.514(5) . ?
N62 C57 1.514(5) . ?
N5 C45 1.514(5) . ?
N5 C33 1.513(5) . ?
N5 C37 1.513(5) . ?
N5 C41 1.514(5) . ?
C45 C46 1.517(15) . ?
C34 C33 1.512(13) . ?
C34 C35 1.492(14) . ?
C37 C38 1.463(18) . ?
C35 C36 1.502(12) . ?
C41 C42 1.463(16) . ?
C42 C43 1.567(17) . ?
C47 C46 1.556(17) . ?
C47 C48 1.482(14) . ?
C38 C39 1.564(18) . ?
C43 C44 1.463(13) . ?
C39 C40 1.535(15) . ?
C54 C55 1.536(7) . ?
C54 C53 1.537(7) . ?
C50 C49 1.537(7) . ?
C50 C51 1.537(7) . ?
C55 C56 1.521(13) . ?
C51 C52 1.514(14) . ?
C61 C62A 1.537(7) . ?
C61 C62B 1.537(7) . ?
C58 C59 1.537(7) . ?
C58 C57 1.536(7) . ?
C59 C60 1.500(16) . ?
C63A C64A 1.499(17) . ?
C63A C62A 1.537(7) . ?
C62B C63B 1.537(8) . ?
C64B C63B 1.511(17) . ?

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
O4 S1 C1 106.1(5) . . ?
O3 S1 O4 113.4(5) . . ?
O3 S1 O2 114.4(5) . . ?
O3 S1 C1 106.0(5) . . ?
O2 S1 O4 111.2(5) . . ?
O2 S1 C1 104.7(5) . . ?
O9 S2 O10 111.9(6) . . ?
O9 S2 C17 108.8(7) . . ?
O10 S2 C17 104.4(6) . . ?
O8 S2 O9 113.6(6) . . ?
O8 S2 O10 115.0(7) . . ?
O8 S2 C17 102.0(6) . . ?
C2 N2 C3 127.6(10) . . ?
C2 N1 C1 120.5(10) . . ?
O1 C2 N2 122.5(12) . . ?
O1 C2 N1 122.6(11) . . ?
N2 C2 N1 114.9(11) . . ?
C9 C6 C5 117.6(12) . . ?
C7 C6 C9 124.2(11) . . ?
C7 C6 C5 118.0(11) . . ?
N2 C3 C8 114.9(10) . . ?
C4 C3 N2 125.7(10) . . ?
C4 C3 C8 119.3(11) . . ?
C3 C4 C5 121.8(10) . . ?
C18 N4 C19 129.4(12) . . ?
C12 C9 C6 122.6(11) . . ?
C18 N3 C17 120.9(12) . . ?
C4 C5 C6 118.1(12) . . ?
C10 C5 C6 119.1(11) . . ?
C10 C5 C4 122.8(10) . . ?
C9 C12 C11 118.7(11) . . ?
C9 C12 C13 123.5(13) . . ?
C11 C12 C13 117.7(12) . . ?
C22 C23 C25 122.5(16) . . ?
C22 C23 C24 118.3(12) . . ?
C24 C23 C25 119.0(14) . . ?
C23 C25 C28 119.1(14) . . ?
O6 C25 C23 119.4(16) . . ?
O6 C25 C28 121.4(12) . . ?
C23 C22 C26 118.2(12) . . ?
C23 C22 C21 119.0(14) . . ?
C21 C22 C26 122.7(13) . . ?
C19 C24 C23 121.6(14) . . ?
C24 C19 N4 124.8(13) . . ?
C20 C19 N4 116.7(12) . . ?
C20 C19 C24 118.5(15) . . ?
C11 C10 C5 122.6(10) . . ?
C10 C11 C12 119.3(11) . . ?
C10 C11 C16 122.8(11) . . ?
C16 C11 C12 117.9(11) . . ?
C7 C8 C3 120.7(12) . . ?
N1 C1 S1 112.5(7) . . ?
O7 C26 C22 121.2(12) . . ?
O7 C26 C27 118.0(16) . . ?
C27 C26 C22 120.8(13) . . ?
C16 C15 C14 119.5(13) . . ?
C20 C21 C22 122.8(13) . . ?
C28 C27 C26 118.5(16) . . ?
C32 C27 C26 121.8(15) . . ?
C32 C27 C28 119.6(14) . . ?
C27 C28 C25 120.5(13) . . ?
C29 C28 C25 121.9(16) . . ?
C29 C28 C27 117.4(17) . . ?
C15 C16 C11 122.9(13) . . ?
C8 C7 C6 121.9(11) . . ?
C21 C20 C19 119.7(12) . . ?
N3 C18 N4 117.8(13) . . ?
O5 C18 N4 119.5(16) . . ?
O5 C18 N3 122.8(13) . . ?
C14 C13 C12 122.9(13) . . ?
C13 C14 C15 119.1(13) . . ?
C30 C29 C28 122.2(17) . . ?
C32 C31 C30 114.9(17) . . ?
C27 C32 C31 124.4(16) . . ?
C29 C30 C31 121.4(15) . . ?
N3 C17 S2 111.7(8) . . ?
C49 N62 C53 114.8(15) . . ?
C49 N62 C61 103.5(12) . . ?
C49 N62 C57 109.3(16) . . ?
C61 N62 C53 115.5(15) . . ?
C61 N62 C57 110.8(15) . . ?
C57 N62 C53 103.0(12) . . ?
C33 N5 C45 108.1(7) . . ?
C33 N5 C41 109.2(8) . . ?
C37 N5 C45 110.5(8) . . ?
C37 N5 C33 111.5(8) . . ?
C37 N5 C41 104.5(9) . . ?
C41 N5 C45 113.1(8) . . ?
N5 C45 C46 114.7(9) . . ?
C35 C34 C33 110.5(8) . . ?
C34 C33 N5 116.7(8) . . ?
C38 C37 N5 114.9(11) . . ?
C34 C35 C36 114.9(10) . . ?
C42 C41 N5 115.2(9) . . ?
C41 C42 C43 104.9(11) . . ?
C48 C47 C46 104.5(13) . . ?
C37 C38 C39 116.4(14) . . ?
C45 C46 C47 112.1(11) . . ?
C44 C43 C42 111.1(14) . . ?
C40 C39 C38 119.3(17) . . ?
C55 C54 C53 104.7(11) . . ?
C51 C50 C49 104.6(13) . . ?
N62 C49 C50 110.2(14) . . ?
C56 C55 C54 109.5(12) . . ?
C52 C51 C50 112.1(15) . . ?
N62 C53 C54 112.8(12) . . ?
N62 C61 C62A 112.6(18) . . ?
N62 C61 C62B 116(2) . . ?
C57 C58 C59 118.6(19) . . ?
C60 C59 C58 114(2) . . ?
N62 C57 C58 122.8(16) . . ?
C64A C63A C62A 101(3) . . ?
C63A C62A C61 136(3) . . ?
C63B C62B C61 135(3) . . ?
C64B C63B C62B 120(3) . . ?

_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
;
# start Validation Reply Form
_vrf_THETM01_2016jrh0053_res     
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystals were very poorly diffracting;  cutting the data at a resolution
 of 1 Ang. is required to obtain an average I/sig of 3.  This is the result of significant 
 disorder in the TBA ions.
;
_vrf_PLAT410_2016jrh0053_res     
;
PROBLEM: Short Intra H...H Contact   H58B   ..  H62A    .       1.36 Ang.  
RESPONSE: These short contacts are from disordered arms of a TBA ion; it is not expected 
that both orientations would be simultaneously present.
;





_vrf_PLAT084_2016jrh0053_res     
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.38 Report
RESPONSE: The crystals were very poorly diffracting; this is the result of significant 
 disorder in the TBA ions.  A large number of restraints and constraints were required
 in the refinement and as a consequence all structural parameters should be interpreted
 with caution.
;


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

data_2017jrh0007_res
_database_code_depnum_ccdc_archive 'CCDC 1562760'
_audit_update_record             
;
2017-07-20 deposited with the CCDC.
2017-09-21 downloaded from the CCDC.
;
_audit_creation_date             2017-07-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C15 H12 N3 O4 S2, C16 H36 N'
_chemical_formula_sum            'C31 H48 N4 O4 S2'
_chemical_formula_weight         604.85
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H20N2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.8269(16)
_cell_length_b                   14.5451(15)
_cell_length_c                   16.5512(16)
_cell_angle_alpha                90
_cell_angle_beta                 103.927(11)
_cell_angle_gamma                90
_cell_volume                     3230.8(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5919
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      72.5510
_cell_measurement_theta_min      4.3820
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.816
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -4 -10 0.0750
-2 4 10 0.0750
0 -9 3 0.0704
0 9 -3 0.0704
-9 1 2 0.0182
9 -1 -2 0.0182

_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.036
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
1.9877 -4.0132 -9.9689 0.0441 0.0187 -1.0197
-1.9877 4.0132 9.9689 -0.0441 -0.0187 1.0197
-0.0237 -9.0161 3.0344 -0.6334 -0.7497 -0.1802
0.0237 9.0161 -3.0344 0.6334 0.7497 0.1802
-9.0008 1.0222 1.9969 -0.7012 0.7004 0.1947
9.0008 -1.0222 -1.9969 0.7012 -0.7004 -0.1947

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12954
_diffrn_reflns_point_group_measured_fraction_full 0.977
_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         4.100
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2774
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.977
_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     25.00  80.00   1.00    5.54    --   41.22-125.00-120.00   55
  2  ω     31.00 108.00   1.00   22.16    --  104.59-111.00  30.00   77
  3  ω     33.00 107.00   1.00   22.16    --  104.59 -94.00  60.00   74
  4  ω     32.00 102.00   1.00   22.16    --  104.59 -61.00 150.00   70
  5  ω     80.00 170.00   1.00   22.16    --  104.59  45.00 -30.00   90
  6  ω    140.00 177.00   1.00   22.16    --  104.59  45.00 -60.00   37
  7  ω    116.00 178.00   1.00   22.16    --  104.59 111.00  30.00   62
  8  ω    105.00 146.00   1.00   22.16    --  104.59 111.00 150.00   41
  9  ω     86.00 112.00   1.00   22.16    --  104.59  45.00 -60.00   26
 10  ω   -117.00  -9.00   1.00    5.54    --  -41.22 -77.00-120.00  108
 11  ω   -115.00 -38.00   1.00    5.54    --  -41.22 -38.00 -30.00   77
;
_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      0.0821373000
_diffrn_orient_matrix_UB_12      0.0652237000
_diffrn_orient_matrix_UB_13      -0.0143024000
_diffrn_orient_matrix_UB_21      -0.0801212000
_diffrn_orient_matrix_UB_22      0.0681237000
_diffrn_orient_matrix_UB_23      -0.0452732000
_diffrn_orient_matrix_UB_31      0.0023316000
_diffrn_orient_matrix_UB_32      0.0480540000
_diffrn_orient_matrix_UB_33      0.0834040000
_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                4604
_reflns_number_total             5716
_reflns_odcompleteness_completeness 99.92
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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         0.571
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5716
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0463
_refine_ls_restrained_S_all      1.036
_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)+(0.0670P)²+0.6730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1308
_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. Uiso/Uaniso restraints and constraints
Uanis(C24) = Uanis(C24A)
3. Others
 Sof(H25A)=Sof(H25B)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(H25C)=Sof(H25D)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C27(H27A,H27B), C31(H31A,H31B), C23(H23A,H23B), C15(H15A,
 H15B), C25(H25C,H25D), C25(H25A,H25B), C17(H17A,H17B), C30(H30A,H30B),
 C18(H18A,H18B), C22(H22A,H22B), C21(H21A,H21B), C26(H26A,H26B), C29(H29A,H29B)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C12(H12), C9(H9), C11(H11), C2(H2A), C5(H5), C10(H10),
 C3(H3A), C4(H4)
4.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C24(H24A,H24B,
 H24C), C24A(H24D,H24E,H24F)
;
_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
S2 S 0.59207(4) 0.57750(4) 0.40607(3) 0.02667(15) Uani 1 1 d . . . . .
S1 S 1.04579(4) 0.53297(4) 0.35837(3) 0.03542(16) Uani 1 1 d . . . . .
O2 O 0.62974(11) 0.54178(10) 0.33778(9) 0.0300(3) Uani 1 1 d . . . . .
O1 O 0.70644(12) 0.28329(11) 0.50990(10) 0.0334(4) Uani 1 1 d . . . . .
O4 O 0.49055(12) 0.54839(12) 0.40253(10) 0.0370(4) Uani 1 1 d . . . . .
O3 O 0.60737(13) 0.67589(11) 0.41875(10) 0.0376(4) Uani 1 1 d . . . . .
N2 N 0.79427(13) 0.39096(12) 0.45500(10) 0.0257(4) Uani 1 1 d . . . . .
H2 H 0.7883 0.4463 0.4329 0.031 Uiso 1 1 calc R . . . .
N4 N 0.61092(13) 0.32358(13) 0.21356(10) 0.0269(4) Uani 1 1 d . . . . .
N1 N 0.87485(14) 0.53760(13) 0.39591(11) 0.0301(4) Uani 1 1 d . . . . .
N3 N 0.65818(14) 0.43061(13) 0.50560(11) 0.0289(4) Uani 1 1 d . . . . .
H3 H 0.6044 0.4119 0.5205 0.035 Uiso 1 1 calc R . . . .
C8 C 0.95526(16) 0.38623(16) 0.42035(12) 0.0282(4) Uani 1 1 d . . . . .
C13 C 0.87872(16) 0.34135(15) 0.44915(12) 0.0262(4) Uani 1 1 d . . . . .
C7 C 0.94862(15) 0.48321(16) 0.39529(12) 0.0276(4) Uani 1 1 d . . . . .
C19 C 0.64171(16) 0.22758(15) 0.19511(13) 0.0282(4) Uani 1 1 d . . . . .
H19A H 0.5832 0.1865 0.1882 0.034 Uiso 1 1 calc R . . . .
H19B H 0.6615 0.2287 0.1415 0.034 Uiso 1 1 calc R . . . .
C14 C 0.71929(16) 0.36349(15) 0.49127(12) 0.0265(4) Uani 1 1 d . . . . .
C12 C 0.89227(18) 0.24839(16) 0.47162(14) 0.0325(5) Uani 1 1 d . . . . .
H12 H 0.8424 0.2168 0.4913 0.039 Uiso 1 1 calc R . . . .
C1 C 0.88895(18) 0.62383(16) 0.36491(13) 0.0323(5) Uani 1 1 d . . . . .
C27 C 0.53011(16) 0.35266(15) 0.13846(12) 0.0288(4) Uani 1 1 d . . . . .
H27A H 0.5566 0.3477 0.0881 0.035 Uiso 1 1 calc R . . . .
H27B H 0.4735 0.3094 0.1318 0.035 Uiso 1 1 calc R . . . .
C9 C 1.03954(18) 0.33670(18) 0.41466(14) 0.0371(5) Uani 1 1 d . . . . .
H9 H 1.0903 0.3668 0.3949 0.044 Uiso 1 1 calc R . . . .
C6 C 0.97901(18) 0.63458(17) 0.34133(13) 0.0344(5) Uani 1 1 d . . . . .
C31 C 0.57230(17) 0.32499(16) 0.29288(13) 0.0304(5) Uani 1 1 d . . . . .
H31A H 0.6259 0.3021 0.3395 0.036 Uiso 1 1 calc R . . . .
H31B H 0.5589 0.3896 0.3054 0.036 Uiso 1 1 calc R . . . .
C23 C 0.69902(16) 0.38900(16) 0.22807(13) 0.0305(5) Uani 1 1 d . . . . .
H23A H 0.7513 0.3658 0.2755 0.037 Uiso 1 1 calc R . . . .
H23B H 0.6773 0.4497 0.2443 0.037 Uiso 1 1 calc R . . . .
C15 C 0.66890(16) 0.52858(15) 0.49987(13) 0.0284(4) Uani 1 1 d . . . . .
H15A H 0.7395 0.5430 0.5024 0.034 Uiso 1 1 calc R . . . .
H15B H 0.6516 0.5578 0.5485 0.034 Uiso 1 1 calc R . . . .
C11 C 0.9775(2) 0.20245(17) 0.46532(15) 0.0396(5) Uani 1 1 d . . . . .
H11 H 0.9853 0.1395 0.4810 0.048 Uiso 1 1 calc R . . . .
C25 C 0.40353(18) 0.46919(17) 0.07142(15) 0.0368(5) Uani 1 1 d . . . . .
H25C H 0.3465 0.4298 0.0755 0.044 Uiso 0.724(5) 1 calc R . P A -1
H25D H 0.4211 0.4554 0.0181 0.044 Uiso 0.724(5) 1 calc R . P A -1
H25A H 0.4284 0.4708 0.0201 0.044 Uiso 0.276(5) 1 calc R . P A -2
H25B H 0.3796 0.5318 0.0796 0.044 Uiso 0.276(5) 1 calc R . P A -2
C17 C 0.74463(19) 0.08801(17) 0.23903(16) 0.0380(5) Uani 1 1 d . . . . .
H17A H 0.6830 0.0518 0.2348 0.046 Uiso 1 1 calc R . . . .
H17B H 0.7614 0.0862 0.1842 0.046 Uiso 1 1 calc R . . . .
C30 C 0.47946(19) 0.2695(2) 0.29027(14) 0.0396(6) Uani 1 1 d . . . . .
H30A H 0.4917 0.2039 0.2800 0.048 Uiso 1 1 calc R . . . .
H30B H 0.4243 0.2917 0.2446 0.048 Uiso 1 1 calc R . . . .
C18 C 0.72630(18) 0.18718(17) 0.26081(15) 0.0370(5) Uani 1 1 d . . . . .
H18A H 0.7096 0.1894 0.3157 0.044 Uiso 1 1 calc R . . . .
H18B H 0.7875 0.2239 0.2645 0.044 Uiso 1 1 calc R . . . .
C22 C 0.74464(19) 0.40235(18) 0.15410(14) 0.0366(5) Uani 1 1 d . . . . .
H22A H 0.7668 0.3423 0.1370 0.044 Uiso 1 1 calc R . . . .
H22B H 0.6939 0.4277 0.1066 0.044 Uiso 1 1 calc R . . . .
C2 C 0.8222(2) 0.69688(18) 0.35651(16) 0.0412(6) Uani 1 1 d . . . . .
H2A H 0.7610 0.6908 0.3726 0.049 Uiso 1 1 calc R . . . .
C21 C 0.83242(19) 0.46726(18) 0.17629(15) 0.0406(6) Uani 1 1 d . . . . .
H21A H 0.8098 0.5264 0.1950 0.049 Uiso 1 1 calc R . . . .
H21B H 0.8828 0.4410 0.2235 0.049 Uiso 1 1 calc R . . . .
C5 C 1.0033(2) 0.7172(2) 0.30833(16) 0.0463(6) Uani 1 1 d . . . . .
H5 H 1.0643 0.7241 0.2921 0.056 Uiso 1 1 calc R . . . .
C26 C 0.4921(2) 0.44927(17) 0.14381(15) 0.0389(5) Uani 1 1 d . . . . .
H26A H 0.5461 0.4937 0.1431 0.047 Uiso 1 1 calc R . . . .
H26B H 0.4721 0.4570 0.1969 0.047 Uiso 1 1 calc R . . . .
C10 C 1.0515(2) 0.24577(19) 0.43678(16) 0.0426(6) Uani 1 1 d . . . . .
H10 H 1.1097 0.2133 0.4325 0.051 Uiso 1 1 calc R . . . .
C3 C 0.8474(2) 0.77799(19) 0.32419(17) 0.0475(6) Uani 1 1 d . . . . .
H3A H 0.8027 0.8286 0.3181 0.057 Uiso 1 1 calc R . . . .
C4 C 0.9367(2) 0.7879(2) 0.30012(17) 0.0498(7) Uani 1 1 d . . . . .
H4 H 0.9515 0.8449 0.2776 0.060 Uiso 1 1 calc R . . . .
C16 C 0.8291(2) 0.04511(19) 0.30433(17) 0.0438(6) Uani 1 1 d . . . . .
H16A H 0.8427 -0.0168 0.2865 0.066 Uiso 1 1 calc GR . . . .
H16B H 0.8099 0.0414 0.3575 0.066 Uiso 1 1 calc GR . . . .
H16C H 0.8890 0.0831 0.3111 0.066 Uiso 1 1 calc GR . . . .
C29 C 0.4514(2) 0.2800(2) 0.37409(16) 0.0476(7) Uani 1 1 d . . . . .
H29A H 0.5080 0.2594 0.4193 0.057 Uiso 1 1 calc R . . . .
H29B H 0.4394 0.3458 0.3835 0.057 Uiso 1 1 calc R . . . .
C20 C 0.8807(3) 0.4856(2) 0.10546(19) 0.0605(9) Uani 1 1 d . . . . .
H20A H 0.8334 0.5175 0.0606 0.091 Uiso 1 1 calc GR . . . .
H20B H 0.9002 0.4271 0.0845 0.091 Uiso 1 1 calc GR . . . .
H20C H 0.9399 0.5240 0.1252 0.091 Uiso 1 1 calc GR . . . .
C28 C 0.3593(2) 0.2252(3) 0.37808(19) 0.0624(9) Uani 1 1 d . . . . .
H28A H 0.3012 0.2505 0.3381 0.094 Uiso 1 1 calc GR . . . .
H28B H 0.3485 0.2290 0.4344 0.094 Uiso 1 1 calc GR . . . .
H28C H 0.3686 0.1608 0.3643 0.094 Uiso 1 1 calc GR . . . .
C24 C 0.3749(3) 0.5703(3) 0.0738(2) 0.0460(8) Uani 0.724(5) 1 d . . P A -1
H24A H 0.3686 0.5861 0.1299 0.069 Uiso 0.724(5) 1 calc GR . P A -1
H24B H 0.3112 0.5811 0.0337 0.069 Uiso 0.724(5) 1 calc GR . P A -1
H24C H 0.4266 0.6087 0.0594 0.069 Uiso 0.724(5) 1 calc GR . P A -1
C24A C 0.3125(8) 0.4045(7) 0.0550(6) 0.0460(8) Uani 0.276(5) 1 d . . P A -2
H24D H 0.3320 0.3436 0.0391 0.069 Uiso 0.276(5) 1 calc GR . P A -2
H24E H 0.2598 0.4295 0.0098 0.069 Uiso 0.276(5) 1 calc GR . P A -2
H24F H 0.2879 0.3992 0.1056 0.069 Uiso 0.276(5) 1 calc GR . P A -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S2 O2 1.4499(15) . ?
S2 O4 1.4537(17) . ?
S2 O3 1.4544(17) . ?
S2 C15 1.803(2) . ?
S1 C7 1.760(2) . ?
S1 C6 1.729(3) . ?
O1 C14 1.230(3) . ?
N2 H2 0.8800 . ?
N2 C13 1.396(3) . ?
N2 C14 1.376(3) . ?
N4 C19 1.512(3) . ?
N4 C27 1.518(3) . ?
N4 C31 1.532(3) . ?
N4 C23 1.519(3) . ?
N1 C7 1.293(3) . ?
N1 C1 1.387(3) . ?
N3 H3 0.8800 . ?
N3 C14 1.349(3) . ?
N3 C15 1.438(3) . ?
C8 C13 1.420(3) . ?
C8 C7 1.467(3) . ?
C8 C9 1.392(3) . ?
C13 C12 1.403(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C18 1.511(3) . ?
C12 H12 0.9500 . ?
C12 C11 1.380(3) . ?
C1 C6 1.400(3) . ?
C1 C2 1.393(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C26 1.510(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.372(4) . ?
C6 C5 1.394(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C30 1.508(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C22 1.519(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C11 H11 0.9500 . ?
C11 C10 1.378(4) . ?
C25 H25C 0.9900 . ?
C25 H25D 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.521(3) . ?
C25 C24 1.527(4) . ?
C25 C24A 1.542(11) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.523(3) . ?
C17 C16 1.521(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C29 1.535(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C21 1.511(3) . ?
C2 H2A 0.9500 . ?
C2 C3 1.374(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C20 1.506(4) . ?
C5 H5 0.9500 . ?
C5 C4 1.365(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C10 H10 0.9500 . ?
C3 H3A 0.9500 . ?
C3 C4 1.394(4) . ?
C4 H4 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C28 1.517(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 S2 O4 112.88(10) . . ?
O2 S2 O3 113.45(9) . . ?
O2 S2 C15 106.38(9) . . ?
O4 S2 O3 113.45(10) . . ?
O4 S2 C15 106.43(10) . . ?
O3 S2 C15 103.24(10) . . ?
C6 S1 C7 89.19(11) . . ?
C13 N2 H2 116.2 . . ?
C14 N2 H2 116.2 . . ?
C14 N2 C13 127.65(18) . . ?
C19 N4 C27 106.23(15) . . ?
C19 N4 C31 111.02(17) . . ?
C19 N4 C23 110.88(17) . . ?
C27 N4 C31 111.00(16) . . ?
C27 N4 C23 111.05(17) . . ?
C23 N4 C31 106.73(15) . . ?
C7 N1 C1 111.65(19) . . ?
C14 N3 H3 115.6 . . ?
C14 N3 C15 128.80(18) . . ?
C15 N3 H3 115.6 . . ?
C13 C8 C7 122.41(19) . . ?
C9 C8 C13 119.2(2) . . ?
C9 C8 C7 118.4(2) . . ?
N2 C13 C8 119.29(19) . . ?
N2 C13 C12 122.7(2) . . ?
C12 C13 C8 118.0(2) . . ?
N1 C7 S1 114.89(17) . . ?
N1 C7 C8 125.6(2) . . ?
C8 C7 S1 119.50(16) . . ?
N4 C19 H19A 108.6 . . ?
N4 C19 H19B 108.6 . . ?
H19A C19 H19B 107.5 . . ?
C18 C19 N4 114.86(17) . . ?
C18 C19 H19A 108.6 . . ?
C18 C19 H19B 108.6 . . ?
O1 C14 N2 123.63(19) . . ?
O1 C14 N3 120.52(19) . . ?
N3 C14 N2 115.85(19) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 C13 120.6(2) . . ?
C11 C12 H12 119.7 . . ?
N1 C1 C6 114.7(2) . . ?
N1 C1 C2 125.3(2) . . ?
C2 C1 C6 120.0(2) . . ?
N4 C27 H27A 108.7 . . ?
N4 C27 H27B 108.7 . . ?
H27A C27 H27B 107.6 . . ?
C26 C27 N4 114.15(17) . . ?
C26 C27 H27A 108.7 . . ?
C26 C27 H27B 108.7 . . ?
C8 C9 H9 119.0 . . ?
C10 C9 C8 122.0(2) . . ?
C10 C9 H9 119.0 . . ?
C1 C6 S1 109.56(18) . . ?
C5 C6 S1 129.1(2) . . ?
C5 C6 C1 121.3(2) . . ?
N4 C31 H31A 108.3 . . ?
N4 C31 H31B 108.3 . . ?
H31A C31 H31B 107.4 . . ?
C30 C31 N4 115.99(17) . . ?
C30 C31 H31A 108.3 . . ?
C30 C31 H31B 108.3 . . ?
N4 C23 H23A 108.5 . . ?
N4 C23 H23B 108.5 . . ?
N4 C23 C22 115.19(17) . . ?
H23A C23 H23B 107.5 . . ?
C22 C23 H23A 108.5 . . ?
C22 C23 H23B 108.5 . . ?
S2 C15 H15A 108.9 . . ?
S2 C15 H15B 108.9 . . ?
N3 C15 S2 113.52(15) . . ?
N3 C15 H15A 108.9 . . ?
N3 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C12 C11 H11 119.3 . . ?
C10 C11 C12 121.5(2) . . ?
C10 C11 H11 119.3 . . ?
H25C C25 H25D 108.3 . . ?
H25A C25 H25B 107.0 . . ?
C26 C25 H25C 109.9 . . ?
C26 C25 H25D 109.9 . . ?
C26 C25 H25A 107.5 . . ?
C26 C25 H25B 107.5 . . ?
C26 C25 C24 109.1(2) . . ?
C26 C25 C24A 119.4(4) . . ?
C24 C25 H25C 109.9 . . ?
C24 C25 H25D 109.9 . . ?
C24A C25 H25A 107.5 . . ?
C24A C25 H25B 107.5 . . ?
H17A C17 H17B 108.0 . . ?
C18 C17 H17A 109.4 . . ?
C18 C17 H17B 109.4 . . ?
C16 C17 H17A 109.4 . . ?
C16 C17 H17B 109.4 . . ?
C16 C17 C18 111.3(2) . . ?
C31 C30 H30A 110.0 . . ?
C31 C30 H30B 110.0 . . ?
C31 C30 C29 108.6(2) . . ?
H30A C30 H30B 108.3 . . ?
C29 C30 H30A 110.0 . . ?
C29 C30 H30B 110.0 . . ?
C19 C18 C17 110.00(19) . . ?
C19 C18 H18A 109.7 . . ?
C19 C18 H18B 109.7 . . ?
C17 C18 H18A 109.7 . . ?
C17 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
C23 C22 H22A 109.6 . . ?
C23 C22 H22B 109.6 . . ?
H22A C22 H22B 108.1 . . ?
C21 C22 C23 110.44(19) . . ?
C21 C22 H22A 109.6 . . ?
C21 C22 H22B 109.6 . . ?
C1 C2 H2A 121.0 . . ?
C3 C2 C1 118.0(2) . . ?
C3 C2 H2A 121.0 . . ?
C22 C21 H21A 108.8 . . ?
C22 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C20 C21 C22 113.7(2) . . ?
C20 C21 H21A 108.8 . . ?
C20 C21 H21B 108.8 . . ?
C6 C5 H5 121.0 . . ?
C4 C5 C6 117.9(3) . . ?
C4 C5 H5 121.0 . . ?
C27 C26 C25 110.89(19) . . ?
C27 C26 H26A 109.5 . . ?
C27 C26 H26B 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 108.0 . . ?
C9 C10 C11 118.7(2) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C2 C3 H3A 119.2 . . ?
C2 C3 C4 121.7(3) . . ?
C4 C3 H3A 119.2 . . ?
C5 C4 C3 121.1(2) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C30 C29 H29A 109.1 . . ?
C30 C29 H29B 109.1 . . ?
H29A C29 H29B 107.8 . . ?
C28 C29 C30 112.6(2) . . ?
C28 C29 H29A 109.1 . . ?
C28 C29 H29B 109.1 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C29 C28 H28A 109.5 . . ?
C29 C28 H28B 109.5 . . ?
C29 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C25 C24A H24D 109.5 . . ?
C25 C24A H24E 109.5 . . ?
C25 C24A H24F 109.5 . . ?
H24D C24A H24E 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 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 C6 C5 C4 179.2(2) . . . . ?
O2 S2 C15 N3 -66.26(17) . . . . ?
O4 S2 C15 N3 54.34(17) . . . . ?
O3 S2 C15 N3 174.05(15) . . . . ?
N2 C13 C12 C11 -179.5(2) . . . . ?
N4 C19 C18 C17 175.23(18) . . . . ?
N4 C27 C26 C25 -173.38(19) . . . . ?
N4 C31 C30 C29 -179.3(2) . . . . ?
N4 C23 C22 C21 -179.0(2) . . . . ?
N1 C1 C6 S1 0.4(2) . . . . ?
N1 C1 C6 C5 179.4(2) . . . . ?
N1 C1 C2 C3 -179.7(2) . . . . ?
C8 C13 C12 C11 -0.3(3) . . . . ?
C8 C9 C10 C11 0.1(4) . . . . ?
C13 N2 C14 O1 -14.8(3) . . . . ?
C13 N2 C14 N3 165.52(19) . . . . ?
C13 C8 C7 S1 -178.76(15) . . . . ?
C13 C8 C7 N1 -0.4(3) . . . . ?
C13 C8 C9 C10 -0.6(3) . . . . ?
C13 C12 C11 C10 -0.2(4) . . . . ?
C7 S1 C6 C1 0.25(17) . . . . ?
C7 S1 C6 C5 -178.6(2) . . . . ?
C7 N1 C1 C6 -1.1(3) . . . . ?
C7 N1 C1 C2 179.1(2) . . . . ?
C7 C8 C13 N2 -0.8(3) . . . . ?
C7 C8 C13 C12 180.00(19) . . . . ?
C7 C8 C9 C10 -180.0(2) . . . . ?
C19 N4 C27 C26 -177.78(19) . . . . ?
C19 N4 C31 C30 -63.2(3) . . . . ?
C19 N4 C23 C22 62.7(2) . . . . ?
C14 N2 C13 C8 -170.73(19) . . . . ?
C14 N2 C13 C12 8.5(3) . . . . ?
C14 N3 C15 S2 102.0(2) . . . . ?
C12 C11 C10 C9 0.3(4) . . . . ?
C1 N1 C7 S1 1.3(2) . . . . ?
C1 N1 C7 C8 -177.14(19) . . . . ?
C1 C6 C5 C4 0.4(4) . . . . ?
C1 C2 C3 C4 0.1(4) . . . . ?
C27 N4 C19 C18 176.89(18) . . . . ?
C27 N4 C31 C30 54.7(3) . . . . ?
C27 N4 C23 C22 -55.2(3) . . . . ?
C9 C8 C13 N2 179.90(19) . . . . ?
C9 C8 C13 C12 0.7(3) . . . . ?
C9 C8 C7 S1 0.6(3) . . . . ?
C9 C8 C7 N1 179.0(2) . . . . ?
C6 S1 C7 N1 -0.94(17) . . . . ?
C6 S1 C7 C8 177.63(17) . . . . ?
C6 C1 C2 C3 0.5(4) . . . . ?
C6 C5 C4 C3 0.2(4) . . . . ?
C31 N4 C19 C18 -62.3(2) . . . . ?
C31 N4 C27 C26 61.4(2) . . . . ?
C31 N4 C23 C22 -176.3(2) . . . . ?
C31 C30 C29 C28 -179.1(3) . . . . ?
C23 N4 C19 C18 56.1(2) . . . . ?
C23 N4 C27 C26 -57.1(2) . . . . ?
C23 N4 C31 C30 175.8(2) . . . . ?
C23 C22 C21 C20 -178.9(3) . . . . ?
C15 N3 C14 O1 170.0(2) . . . . ?
C15 N3 C14 N2 -10.3(3) . . . . ?
C2 C1 C6 S1 -179.76(19) . . . . ?
C2 C1 C6 C5 -0.8(4) . . . . ?
C2 C3 C4 C5 -0.5(4) . . . . ?
C16 C17 C18 C19 -179.7(2) . . . . ?
C24 C25 C26 C27 -173.8(2) . . . . ?
C24A C25 C26 C27 54.5(5) . . . . ?

_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 1.549
_oxdiff_exptl_absorpt_empirical_full_min 0.771
# start Validation Reply Form
_vrf_PLAT413_2017jrh0007_res     
;
PROBLEM: Short Inter XH3 .. XHn H20A .. H24E .. 1.70 Ang.
RESPONSE: This alert corresponds to a close contact steric clash between
the arms of one one tetrabutylammonium arm and a second which is the minor
componant in a disordered terminal methyl group.
;
####################################################################### 
# 
# 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_2017jrh0018_res
_database_code_depnum_ccdc_archive 'CCDC 1562761'
_audit_update_record             
;
2017-07-17 deposited with the CCDC.
2017-09-21 downloaded from the CCDC.
;
_audit_creation_date             2017-07-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C12 H11 N2 O4 S, C16 H36 N, H2 O'
_chemical_formula_sum            'C28 H49 N3 O5 S'
_chemical_formula_weight         539.76
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H20N4O4S2
_chemical_oxdiff_usercomment     naphalene
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                   13.1121(18)
_cell_length_b                   16.3159(14)
_cell_length_c                   13.6871(16)
_cell_angle_alpha                90
_cell_angle_beta                 90.027(11)
_cell_angle_gamma                90
_cell_volume                     2928.2(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5572
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      72.3010
_cell_measurement_theta_min      4.1150
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.306
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 0 -6 0.0828
0 -10 -2 0.0343
6 -1 6 0.0811
-1 10 1 0.0223
-6 -1 6 0.0108
6 -1 -6 0.0108

_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.03
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
-6.1425 -0.3283 -6.1433 0.0100 0.3400 0.9404
0.4331 -10.2407 -2.2203 -0.0215 -0.8709 0.4911
6.2888 -1.1392 5.9081 -0.0133 -0.4699 -0.8826
-1.3663 10.3327 1.3237 0.0233 0.9342 -0.3559
-6.0930 -1.3289 6.1053 0.9968 0.0791 0.0089
6.4586 -0.8043 -5.7520 -0.9586 -0.2847 0.0093

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20834
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.195
_diffrn_reflns_theta_min         4.216
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2774
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -71.00  25.00   1.00   10.00    --  -41.47  77.00  30.00   96
  2  ω   -115.00 -17.00   1.00   10.00    --  -41.47 -38.00 120.00   98
  3  ω    -66.00  28.00   1.00   10.00    --  -41.47  38.00 -60.00   94
  4  ω     60.00  94.00   1.00   10.00    --   41.47-125.00-120.00   34
  5  ω     41.00  68.00   1.00   10.00    --   41.47-125.00-180.00   27
  6  ω     47.00 106.00   1.00   30.00    --  104.59 -94.00-180.00   59
  7  ω     30.00 137.00   1.00   30.00    --  104.59 -77.00 -30.00  107
  8  ω     53.00  84.00   1.00   30.00    --  104.59 -61.00-180.00   31
  9  ω     63.00 111.00   1.00   30.00    --  104.59 178.00 -60.00   48
 10  ω     30.00 103.00   1.00   30.00    --  104.59-111.00 -60.00   73
 11  ω    116.00 178.00   1.00   30.00    --  104.59  30.00  90.00   62
 12  ω    140.00 169.00   1.00   30.00    --  104.59  61.00  30.00   29
 13  ω     68.00 115.00   1.00   30.00    --  104.59-111.00   0.00   47
 14  ω     30.00 122.00   1.00   30.00    --  104.59 -30.00  60.00   92
 15  ω    109.00 134.00   1.00   30.00    --  104.59 -61.00-180.00   25
 16  ω     41.00 118.00   1.00   30.00    --  104.59 -45.00 -30.00   77
 17  ω     23.00 145.00   1.00   30.00    --  104.59 -15.00 -90.00  122
 18  ω     52.00 110.00   1.00   30.00    --  104.59-111.00 150.00   58
;
_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      -0.0800307000
_diffrn_orient_matrix_UB_12      -0.0184960000
_diffrn_orient_matrix_UB_13      0.0793759000
_diffrn_orient_matrix_UB_21      -0.0458840000
_diffrn_orient_matrix_UB_22      0.0861509000
_diffrn_orient_matrix_UB_23      -0.0140782000
_diffrn_orient_matrix_UB_31      -0.0727354000
_diffrn_orient_matrix_UB_32      -0.0340025000
_diffrn_orient_matrix_UB_33      -0.0785274000
_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                4527
_reflns_number_total             5754
_reflns_odcompleteness_completeness 99.94
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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         0.278
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         5754
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0504
_refine_ls_restrained_S_all      1.038
_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)+(0.0760P)²+0.7220P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1479
_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, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N1-C10A \\sim N1-C10
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(C2A)
Uanis(C1) = Uanis(C1A)
Uanis(C10) = Uanis(C10A)
Uanis(C9) = Uanis(C9A)
Uanis(C8) = Uanis(C8A)
Uanis(C7) = Uanis(C7A)
Uanis(C6) = Uanis(C6A)
Uanis(C5) = Uanis(C5A)
Uanis(C4) = Uanis(C4A)
Uanis(C3) = Uanis(C3A)
4. Others
 Sof(H1B)=Sof(C2A)=Sof(H2AA)=Sof(C1A)=Sof(C10A)=Sof(C9A)=Sof(H9A)=Sof(C8A)=
 Sof(H8A)=Sof(C7A)=Sof(H7A)=Sof(C6A)=Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(H4A)=
 Sof(C3A)=Sof(H3A)=1-FVAR(1)
 Sof(H1A)=Sof(C1)=Sof(C10)=Sof(C2)=Sof(H2A)=Sof(C3)=Sof(H3)=Sof(C6)=Sof(C9)=
 Sof(H9)=Sof(C4)=Sof(H4)=Sof(C7)=Sof(H7)=Sof(C5)=Sof(H5)=Sof(C8)=Sof(H8)=FVAR(1)
5.a Free rotating group:
 O5(H5B,H5C)
5.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C24(H24A,H24B), C20(H20A,H20B), C18(H18A,H18B), C23(H23A,
 H23B), C28(H28A,H28B), C19(H19A,H19B), C15(H15A,H15B), C27(H27A,H27B),
 C26(H26A,H26B), C14(H14A,H14B), C22(H22A,H22B), C12(H12A,H12B)
5.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1A), N1(H1B), C2(H2A), C3(H3), C9(H9), C4(H4), C7(H7), C5(H5),
 C8(H8), C2A(H2AA), C9A(H9A), C8A(H8A), C7A(H7A), C5A(H5A), C4A(H4A), C3A(H3A)
5.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C17(H17A,H17B,
 H17C)
;
_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 0.69688(4) 0.54612(3) 0.56716(4) 0.03270(15) Uani 1 1 d . . . . .
O3 O 0.63894(13) 0.54505(11) 0.47576(12) 0.0459(4) Uani 1 1 d . . . . .
N3 N 0.29615(12) 0.72050(9) 0.88158(11) 0.0224(3) Uani 1 1 d . . . . .
O4 O 0.80369(12) 0.52737(11) 0.55419(13) 0.0447(4) Uani 1 1 d . . . . .
O1 O 0.54031(13) 0.46634(12) 0.81251(13) 0.0480(4) Uani 1 1 d . . . . .
O2 O 0.67710(14) 0.61991(10) 0.62250(15) 0.0501(4) Uani 1 1 d . . . . .
N2 N 0.53764(14) 0.46513(10) 0.64693(14) 0.0343(4) Uani 1 1 d . . . . .
H2 H 0.5002 0.4671 0.5954 0.041 Uiso 1 1 calc R . . . .
N1 N 0.38741(14) 0.46195(10) 0.73134(14) 0.0333(4) Uani 1 1 d D . . . .
H1A H 0.3619 0.4664 0.6737 0.040 Uiso 0.830(11) 1 calc R . P A 1
H1B H 0.3537 0.4628 0.6775 0.040 Uiso 0.170(11) 1 calc R . P A 2
C16 C 0.27846(14) 0.65857(11) 0.96267(14) 0.0240(4) Uani 1 1 d . . . . .
H16A H 0.3435 0.6349 0.9812 0.029 Uiso 1 1 calc R . . . .
H16B H 0.2360 0.6146 0.9376 0.029 Uiso 1 1 calc R . . . .
C24 C 0.34313(14) 0.67439(11) 0.79587(14) 0.0245(4) Uani 1 1 d . . . . .
H24A H 0.4069 0.6503 0.8175 0.029 Uiso 1 1 calc R . . . .
H24B H 0.2979 0.6297 0.7783 0.029 Uiso 1 1 calc R . . . .
C20 C 0.19694(14) 0.76157(11) 0.85145(14) 0.0245(4) Uani 1 1 d . . . . .
H20A H 0.2116 0.7997 0.7989 0.029 Uiso 1 1 calc R . . . .
H20B H 0.1720 0.7933 0.9064 0.029 Uiso 1 1 calc R . . . .
C18 C 0.02412(15) 0.75519(12) 0.77525(14) 0.0285(4) Uani 1 1 d . . . . .
H18A H 0.0038 0.7964 0.8225 0.034 Uiso 1 1 calc R . . . .
H18B H 0.0479 0.7834 0.7172 0.034 Uiso 1 1 calc R . . . .
C23 C 0.36398(15) 0.72484(11) 0.70485(14) 0.0274(4) Uani 1 1 d . . . . .
H23A H 0.4086 0.7703 0.7209 0.033 Uiso 1 1 calc R . . . .
H23B H 0.3005 0.7470 0.6798 0.033 Uiso 1 1 calc R . . . .
C28 C 0.36689(15) 0.78880(11) 0.91565(14) 0.0260(4) Uani 1 1 d . . . . .
H28A H 0.3783 0.8258 0.8613 0.031 Uiso 1 1 calc R . . . .
H28B H 0.3324 0.8196 0.9665 0.031 Uiso 1 1 calc R . . . .
C19 C 0.11194(14) 0.70443(11) 0.81794(14) 0.0263(4) Uani 1 1 d . . . . .
H19A H 0.0875 0.6724 0.8728 0.032 Uiso 1 1 calc R . . . .
H19B H 0.1378 0.6670 0.7688 0.032 Uiso 1 1 calc R . . . .
C1 C 0.2091(3) 0.4674(2) 0.7871(3) 0.0263(8) Uani 0.830(11) 1 d . . P A 1
O5 O 0.6107(2) 0.62969(14) 0.81757(17) 0.0675(6) Uani 1 1 d . . . . .
H5B H 0.5886 0.5809 0.8235 0.101 Uiso 1 1 d G . . . .
H5C H 0.6263 0.6386 0.7582 0.101 Uiso 1 1 d G . . . .
C15 C 0.22811(16) 0.69419(12) 1.05319(14) 0.0302(4) Uani 1 1 d . . . . .
H15A H 0.2651 0.7428 1.0735 0.036 Uiso 1 1 calc R . . . .
H15B H 0.1589 0.7104 1.0373 0.036 Uiso 1 1 calc R . . . .
C27 C 0.47014(15) 0.76136(12) 0.95469(16) 0.0306(4) Uani 1 1 d . . . . .
H27A H 0.5041 0.7272 0.9067 0.037 Uiso 1 1 calc R . . . .
H27B H 0.4609 0.7294 1.0138 0.037 Uiso 1 1 calc R . . . .
C26 C 0.53510(15) 0.83660(13) 0.97645(16) 0.0314(4) Uani 1 1 d . . . . .
H26A H 0.5003 0.8706 1.0241 0.038 Uiso 1 1 calc R . . . .
H26B H 0.5431 0.8685 0.9171 0.038 Uiso 1 1 calc R . . . .
C14 C 0.22578(16) 0.63340(13) 1.13699(15) 0.0323(4) Uani 1 1 d . . . . .
H14A H 0.2950 0.6183 1.1543 0.039 Uiso 1 1 calc R . . . .
H14B H 0.1904 0.5841 1.1164 0.039 Uiso 1 1 calc R . . . .
C11 C 0.49185(17) 0.46484(12) 0.73573(17) 0.0346(5) Uani 1 1 d . . . . .
C22 C 0.41405(16) 0.67113(13) 0.62729(15) 0.0313(4) Uani 1 1 d . . . . .
H22A H 0.4770 0.6487 0.6533 0.038 Uiso 1 1 calc R . . . .
H22B H 0.3691 0.6257 0.6119 0.038 Uiso 1 1 calc R . . . .
C10 C 0.3157(3) 0.4528(2) 0.8073(3) 0.0265(8) Uani 0.830(11) 1 d D . P A 1
C21 C 0.43728(17) 0.71840(14) 0.53422(16) 0.0362(5) Uani 1 1 d . . . . .
H21A H 0.4755 0.6842 0.4905 0.054 Uiso 1 1 calc GR . . . .
H21B H 0.4764 0.7664 0.5499 0.054 Uiso 1 1 calc GR . . . .
H21C H 0.3745 0.7345 0.5035 0.054 Uiso 1 1 calc GR . . . .
C13 C 0.17240(16) 0.66924(14) 1.22619(15) 0.0345(5) Uani 1 1 d . . . . .
H13A H 0.1033 0.6828 1.2096 0.052 Uiso 1 1 calc GR . . . .
H13B H 0.2076 0.7178 1.2470 0.052 Uiso 1 1 calc GR . . . .
H13C H 0.1727 0.6297 1.2781 0.052 Uiso 1 1 calc GR . . . .
C2 C 0.1733(3) 0.4900(2) 0.6922(3) 0.0275(8) Uani 0.830(11) 1 d . . P A 1
H2A H 0.2193 0.4965 0.6411 0.033 Uiso 0.830(11) 1 calc R . P A 1
C12 C 0.64631(17) 0.46227(13) 0.63602(17) 0.0356(5) Uani 1 1 d . . . . .
H12A H 0.6648 0.4114 0.6039 0.043 Uiso 1 1 calc R . . . .
H12B H 0.6774 0.4622 0.7003 0.043 Uiso 1 1 calc R . . . .
C3 C 0.0701(3) 0.5020(2) 0.6768(3) 0.0344(8) Uani 0.830(11) 1 d . . P A 1
H3 H 0.0472 0.5172 0.6150 0.041 Uiso 0.830(11) 1 calc R . P A 1
C25 C 0.64007(17) 0.81365(14) 1.01566(17) 0.0383(5) Uani 1 1 d . . . . .
H25A H 0.6753 0.7808 0.9682 0.057 Uiso 1 1 calc GR . . . .
H25B H 0.6326 0.7831 1.0752 0.057 Uiso 1 1 calc GR . . . .
H25C H 0.6785 0.8626 1.0283 0.057 Uiso 1 1 calc GR . . . .
C6 C 0.1375(3) 0.45705(17) 0.8630(3) 0.0291(8) Uani 0.830(11) 1 d . . P A 1
C9 C 0.3446(3) 0.4300(2) 0.9000(3) 0.0329(8) Uani 0.830(11) 1 d . . P A 1
H9 H 0.4132 0.4213 0.9137 0.039 Uiso 0.830(11) 1 calc R . P A 1
C17 C -0.06810(17) 0.70331(15) 0.74888(18) 0.0394(5) Uani 1 1 d . . . . .
H17A H -0.0486 0.6624 0.7021 0.059 Uiso 1 1 calc GR . . . .
H17B H -0.1201 0.7377 0.7212 0.059 Uiso 1 1 calc GR . . . .
H17C H -0.0939 0.6771 0.8066 0.059 Uiso 1 1 calc GR . . . .
C4 C -0.0001(3) 0.4918(2) 0.7520(4) 0.0371(9) Uani 0.830(11) 1 d . . P A 1
H4 H -0.0692 0.4998 0.7401 0.045 Uiso 0.830(11) 1 calc R . P A 1
C7 C 0.1707(3) 0.4331(2) 0.9571(4) 0.0351(9) Uani 0.830(11) 1 d . . P A 1
H7 H 0.1237 0.4264 1.0073 0.042 Uiso 0.830(11) 1 calc R . P A 1
C5 C 0.0320(3) 0.4702(2) 0.8433(4) 0.0368(11) Uani 0.830(11) 1 d . . P A 1
H5 H -0.0154 0.4639 0.8932 0.044 Uiso 0.830(11) 1 calc R . P A 1
C8 C 0.2717(3) 0.4198(2) 0.9742(3) 0.0350(8) Uani 0.830(11) 1 d . . P A 1
H8 H 0.2929 0.4036 1.0361 0.042 Uiso 0.830(11) 1 calc R . P A 1
C2A C 0.1899(19) 0.4870(15) 0.720(2) 0.0275(8) Uani 0.170(11) 1 d . . P A 2
H2AA H 0.2342 0.5005 0.6693 0.033 Uiso 0.170(11) 1 calc R . P A 2
C1A C 0.2374(18) 0.4638(13) 0.803(2) 0.0263(8) Uani 0.170(11) 1 d . . P A 2
C10A C 0.3395(17) 0.4574(15) 0.8270(12) 0.0265(8) Uani 0.170(11) 1 d D . P A 2
C9A C 0.3726(17) 0.4401(13) 0.9192(17) 0.0329(8) Uani 0.170(11) 1 d . . P A 2
H9A H 0.4418 0.4325 0.9310 0.039 Uiso 0.170(11) 1 calc R . P A 2
C8A C 0.2987(16) 0.4332(12) 1.0006(15) 0.0350(8) Uani 0.170(11) 1 d . . P A 2
H8A H 0.3217 0.4257 1.0643 0.042 Uiso 0.170(11) 1 calc R . P A 2
C7A C 0.2008(19) 0.4378(13) 0.9824(17) 0.0351(9) Uani 0.170(11) 1 d . . P A 2
H7A H 0.1555 0.4289 1.0336 0.042 Uiso 0.170(11) 1 calc R . P A 2
C6A C 0.1626(17) 0.4546(11) 0.8940(19) 0.0291(8) Uani 0.170(11) 1 d . . P A 2
C5A C 0.0613(18) 0.4649(13) 0.8688(19) 0.0368(11) Uani 0.170(11) 1 d . . P A 2
H5A H 0.0150 0.4554 0.9190 0.044 Uiso 0.170(11) 1 calc R . P A 2
C4A C 0.0209(19) 0.4859(14) 0.786(2) 0.0371(9) Uani 0.170(11) 1 d . . P A 2
H4A H -0.0487 0.4956 0.7800 0.045 Uiso 0.170(11) 1 calc R . P A 2
C3A C 0.0943(19) 0.4941(14) 0.697(2) 0.0344(8) Uani 0.170(11) 1 d . . P A 2
H3A H 0.0716 0.5033 0.6337 0.041 Uiso 0.170(11) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O3 1.4635(18) . ?
S1 O4 1.4446(17) . ?
S1 O2 1.4459(18) . ?
S1 C12 1.789(2) . ?
N3 C16 1.519(2) . ?
N3 C24 1.524(2) . ?
N3 C20 1.520(2) . ?
N3 C28 1.523(2) . ?
O1 C11 1.228(3) . ?
N2 H2 0.8600 . ?
N2 C11 1.356(3) . ?
N2 C12 1.433(3) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C11 1.372(3) . ?
N1 C10 1.410(4) . ?
N1 C10A 1.455(16) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C15 1.520(3) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C23 1.518(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C19 1.524(3) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.534(2) . ?
C18 C17 1.519(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C22 1.525(3) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C27 1.523(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C1 C10 1.444(4) . ?
C1 C2 1.429(4) . ?
C1 C6 1.410(5) . ?
O5 H5B 0.8503 . ?
O5 H5C 0.8501 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C14 1.517(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C26 1.523(3) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C25 1.524(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C13 1.524(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C21 1.520(3) . ?
C10 C9 1.376(5) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C2 H2A 0.9300 . ?
C2 C3 1.384(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C3 H3 0.9300 . ?
C3 C4 1.392(6) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C6 C7 1.416(4) . ?
C6 C5 1.424(4) . ?
C9 H9 0.9300 . ?
C9 C8 1.404(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C4 H4 0.9300 . ?
C4 C5 1.365(5) . ?
C7 H7 0.9300 . ?
C7 C8 1.362(5) . ?
C5 H5 0.9300 . ?
C8 H8 0.9300 . ?
C2A H2AA 0.9300 . ?
C2A C1A 1.35(3) . ?
C2A C3A 1.30(3) . ?
C1A C10A 1.38(2) . ?
C1A C6A 1.59(4) . ?
C10A C9A 1.36(3) . ?
C9A H9A 0.9300 . ?
C9A C8A 1.48(3) . ?
C8A H8A 0.9300 . ?
C8A C7A 1.31(3) . ?
C7A H7A 0.9300 . ?
C7A C6A 1.34(3) . ?
C6A C5A 1.38(2) . ?
C5A H5A 0.9300 . ?
C5A C4A 1.30(3) . ?
C4A H4A 0.9300 . ?
C4A C3A 1.56(4) . ?
C3A H3A 0.9300 . ?

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 C12 104.41(11) . . ?
O4 S1 O3 113.29(11) . . ?
O4 S1 O2 114.51(11) . . ?
O4 S1 C12 105.21(10) . . ?
O2 S1 O3 111.38(11) . . ?
O2 S1 C12 107.11(11) . . ?
C16 N3 C24 107.21(13) . . ?
C16 N3 C20 111.13(14) . . ?
C16 N3 C28 110.87(14) . . ?
C20 N3 C24 110.79(13) . . ?
C20 N3 C28 106.35(13) . . ?
C28 N3 C24 110.52(14) . . ?
C11 N2 H2 118.9 . . ?
C11 N2 C12 122.27(19) . . ?
C12 N2 H2 118.9 . . ?
C11 N1 H1A 115.2 . . ?
C11 N1 H1B 123.4 . . ?
C11 N1 C10 129.6(3) . . ?
C11 N1 C10A 113.2(9) . . ?
C10 N1 H1A 115.2 . . ?
C10A N1 H1B 123.4 . . ?
N3 C16 H16A 108.7 . . ?
N3 C16 H16B 108.7 . . ?
N3 C16 C15 114.07(15) . . ?
H16A C16 H16B 107.6 . . ?
C15 C16 H16A 108.7 . . ?
C15 C16 H16B 108.7 . . ?
N3 C24 H24A 108.3 . . ?
N3 C24 H24B 108.3 . . ?
H24A C24 H24B 107.4 . . ?
C23 C24 N3 115.91(15) . . ?
C23 C24 H24A 108.3 . . ?
C23 C24 H24B 108.3 . . ?
N3 C20 H20A 108.3 . . ?
N3 C20 H20B 108.3 . . ?
N3 C20 C19 115.96(14) . . ?
H20A C20 H20B 107.4 . . ?
C19 C20 H20A 108.3 . . ?
C19 C20 H20B 108.3 . . ?
H18A C18 H18B 107.8 . . ?
C19 C18 H18A 109.0 . . ?
C19 C18 H18B 109.0 . . ?
C17 C18 H18A 109.0 . . ?
C17 C18 H18B 109.0 . . ?
C17 C18 C19 112.76(17) . . ?
C24 C23 H23A 109.7 . . ?
C24 C23 H23B 109.7 . . ?
C24 C23 C22 109.71(16) . . ?
H23A C23 H23B 108.2 . . ?
C22 C23 H23A 109.7 . . ?
C22 C23 H23B 109.7 . . ?
N3 C28 H28A 108.4 . . ?
N3 C28 H28B 108.4 . . ?
H28A C28 H28B 107.4 . . ?
C27 C28 N3 115.70(15) . . ?
C27 C28 H28A 108.4 . . ?
C27 C28 H28B 108.4 . . ?
C20 C19 C18 109.46(15) . . ?
C20 C19 H19A 109.8 . . ?
C20 C19 H19B 109.8 . . ?
C18 C19 H19A 109.8 . . ?
C18 C19 H19B 109.8 . . ?
H19A C19 H19B 108.2 . . ?
C2 C1 C10 122.2(3) . . ?
C6 C1 C10 119.0(3) . . ?
C6 C1 C2 118.8(3) . . ?
H5B O5 H5C 109.4 . . ?
C16 C15 H15A 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C14 C15 C16 112.04(16) . . ?
C14 C15 H15A 109.2 . . ?
C14 C15 H15B 109.2 . . ?
C28 C27 H27A 109.8 . . ?
C28 C27 H27B 109.8 . . ?
C28 C27 C26 109.18(16) . . ?
H27A C27 H27B 108.3 . . ?
C26 C27 H27A 109.8 . . ?
C26 C27 H27B 109.8 . . ?
C27 C26 H26A 109.2 . . ?
C27 C26 H26B 109.2 . . ?
C27 C26 C25 112.06(17) . . ?
H26A C26 H26B 107.9 . . ?
C25 C26 H26A 109.2 . . ?
C25 C26 H26B 109.2 . . ?
C15 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
C15 C14 C13 111.36(17) . . ?
H14A C14 H14B 108.0 . . ?
C13 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
O1 C11 N2 122.5(2) . . ?
O1 C11 N1 123.7(2) . . ?
N2 C11 N1 113.8(2) . . ?
C23 C22 H22A 109.2 . . ?
C23 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
C21 C22 C23 112.23(17) . . ?
C21 C22 H22A 109.2 . . ?
C21 C22 H22B 109.2 . . ?
N1 C10 C1 119.2(3) . . ?
C9 C10 N1 121.7(3) . . ?
C9 C10 C1 119.1(3) . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C1 C2 H2A 120.1 . . ?
C3 C2 C1 119.7(3) . . ?
C3 C2 H2A 120.1 . . ?
S1 C12 H12A 108.9 . . ?
S1 C12 H12B 108.9 . . ?
N2 C12 S1 113.50(14) . . ?
N2 C12 H12A 108.9 . . ?
N2 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
C2 C3 H3 119.5 . . ?
C2 C3 C4 121.1(3) . . ?
C4 C3 H3 119.5 . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
C26 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C1 C6 C7 119.9(3) . . ?
C1 C6 C5 119.3(3) . . ?
C7 C6 C5 120.8(3) . . ?
C10 C9 H9 119.6 . . ?
C10 C9 C8 120.8(3) . . ?
C8 C9 H9 119.6 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.3(3) . . ?
C5 C4 H4 119.8 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0(3) . . ?
C8 C7 H7 120.0 . . ?
C6 C5 H5 119.6 . . ?
C4 C5 C6 120.7(3) . . ?
C4 C5 H5 119.6 . . ?
C9 C8 H8 119.4 . . ?
C7 C8 C9 121.3(3) . . ?
C7 C8 H8 119.4 . . ?
C1A C2A H2AA 113.9 . . ?
C3A C2A H2AA 113.9 . . ?
C3A C2A C1A 132(3) . . ?
C2A C1A C10A 132(2) . . ?
C2A C1A C6A 114(2) . . ?
C10A C1A C6A 113.8(19) . . ?
C1A C10A N1 101.6(18) . . ?
C9A C10A N1 134.9(19) . . ?
C9A C10A C1A 122.9(18) . . ?
C10A C9A H9A 119.9 . . ?
C10A C9A C8A 120.2(18) . . ?
C8A C9A H9A 119.9 . . ?
C9A C8A H8A 120.2 . . ?
C7A C8A C9A 119.6(18) . . ?
C7A C8A H8A 120.2 . . ?
C8A C7A H7A 118.3 . . ?
C8A C7A C6A 123(2) . . ?
C6A C7A H7A 118.3 . . ?
C7A C6A C1A 119.8(18) . . ?
C7A C6A C5A 128(2) . . ?
C5A C6A C1A 112.7(19) . . ?
C6A C5A H5A 115.0 . . ?
C4A C5A C6A 130(2) . . ?
C4A C5A H5A 115.0 . . ?
C5A C4A H4A 121.5 . . ?
C5A C4A C3A 117(2) . . ?
C3A C4A H4A 121.5 . . ?
C2A C3A C4A 114(2) . . ?
C2A C3A H3A 123.1 . . ?
C4A C3A H3A 123.1 . . ?

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
O3 S1 C12 N2 -53.74(19) . . . . ?
N3 C16 C15 C14 -171.85(16) . . . . ?
N3 C24 C23 C22 178.06(15) . . . . ?
N3 C20 C19 C18 -171.18(15) . . . . ?
N3 C28 C27 C26 174.68(16) . . . . ?
O4 S1 C12 N2 -173.27(17) . . . . ?
O2 S1 C12 N2 64.49(19) . . . . ?
N1 C10 C9 C8 -178.8(3) . . . . ?
N1 C10A C9A C8A -174.1(19) . . . . ?
C16 N3 C24 C23 178.07(15) . . . . ?
C16 N3 C20 C19 -57.0(2) . . . . ?
C16 N3 C28 C27 56.0(2) . . . . ?
C16 C15 C14 C13 -178.39(17) . . . . ?
C24 N3 C16 C15 -178.00(15) . . . . ?
C24 N3 C20 C19 62.1(2) . . . . ?
C24 N3 C28 C27 -62.7(2) . . . . ?
C24 C23 C22 C21 -179.77(17) . . . . ?
C20 N3 C16 C15 -56.79(19) . . . . ?
C20 N3 C24 C23 56.6(2) . . . . ?
C20 N3 C28 C27 176.96(16) . . . . ?
C28 N3 C16 C15 61.3(2) . . . . ?
C28 N3 C24 C23 -60.99(19) . . . . ?
C28 N3 C20 C19 -177.75(16) . . . . ?
C28 C27 C26 C25 -179.83(18) . . . . ?
C1 C10 C9 C8 0.9(5) . . . . ?
C1 C2 C3 C4 -0.6(6) . . . . ?
C1 C6 C7 C8 -0.2(5) . . . . ?
C1 C6 C5 C4 0.6(5) . . . . ?
C11 N2 C12 S1 -123.36(19) . . . . ?
C11 N1 C10 C1 168.0(3) . . . . ?
C11 N1 C10 C9 -12.2(5) . . . . ?
C11 N1 C10A C1A 174.1(12) . . . . ?
C11 N1 C10A C9A -15(3) . . . . ?
C10 N1 C11 O1 -6.3(4) . . . . ?
C10 N1 C11 N2 173.1(3) . . . . ?
C10 N1 C10A C1A -16(3) . . . . ?
C10 N1 C10A C9A 155(6) . . . . ?
C10 C1 C2 C3 179.1(3) . . . . ?
C10 C1 C6 C7 0.3(5) . . . . ?
C10 C1 C6 C5 -179.1(3) . . . . ?
C10 C9 C8 C7 -0.9(5) . . . . ?
C2 C1 C10 N1 0.8(5) . . . . ?
C2 C1 C10 C9 -179.0(3) . . . . ?
C2 C1 C6 C7 178.7(3) . . . . ?
C2 C1 C6 C5 -0.7(5) . . . . ?
C2 C3 C4 C5 0.5(6) . . . . ?
C12 N2 C11 O1 3.8(3) . . . . ?
C12 N2 C11 N1 -175.60(17) . . . . ?
C3 C4 C5 C6 -0.5(5) . . . . ?
C6 C1 C10 N1 179.1(3) . . . . ?
C6 C1 C10 C9 -0.6(5) . . . . ?
C6 C1 C2 C3 0.7(5) . . . . ?
C6 C7 C8 C9 0.5(5) . . . . ?
C17 C18 C19 C20 -174.55(17) . . . . ?
C7 C6 C5 C4 -178.8(3) . . . . ?
C5 C6 C7 C8 179.2(3) . . . . ?
C2A C1A C10A N1 -14(3) . . . . ?
C2A C1A C10A C9A 173(3) . . . . ?
C2A C1A C6A C7A -175(2) . . . . ?
C2A C1A C6A C5A 6(3) . . . . ?
C1A C2A C3A C4A 10(4) . . . . ?
C1A C10A C9A C8A -5(3) . . . . ?
C1A C6A C5A C4A -5(4) . . . . ?
C10A N1 C11 O1 -2.4(11) . . . . ?
C10A N1 C11 N2 177.0(11) . . . . ?
C10A N1 C10 C1 155(4) . . . . ?
C10A N1 C10 C9 -25(4) . . . . ?
C10A C1A C6A C7A -3(3) . . . . ?
C10A C1A C6A C5A 177.2(19) . . . . ?
C10A C9A C8A C7A 5(3) . . . . ?
C9A C8A C7A C6A -5(3) . . . . ?
C8A C7A C6A C1A 4(3) . . . . ?
C8A C7A C6A C5A -176(2) . . . . ?
C7A C6A C5A C4A 175(2) . . . . ?
C6A C1A C10A N1 176.0(15) . . . . ?
C6A C1A C10A C9A 4(3) . . . . ?
C6A C5A C4A C3A 6(4) . . . . ?
C5A C4A C3A C2A -7(3) . . . . ?
C3A C2A C1A C10A -179(3) . . . . ?
C3A C2A C1A C6A -9(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.198
_oxdiff_exptl_absorpt_empirical_full_min 0.756
# start Validation Reply Form
_vrf_PLAT415_2017jrh0018_res     
;
PROBLEM: Short Inter D-H..H-X H5B .. H8A .. 1.94 Ang.
RESPONSE: This alert corresconds to a close contact steric clash between
the OH of a water molecule and a CH which is the minor componant in a 
disordered naphthalene functionaility.
;
####################################################################### 
# 
# 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_2017jrh0006_res
_database_code_depnum_ccdc_archive 'CCDC 1562759'
_audit_update_record             
;
2017-09-04 deposited with the CCDC.
2017-09-21 downloaded from the CCDC.
;
_audit_creation_date             2017-08-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C16 H14 N3 O4 S2, 2(C8 H18 N0.5), 0.5(O)'
_chemical_formula_sum            'C32 H50 N4 O4.50 S2'
_chemical_formula_weight         626.88
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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                   12.706(3)
_cell_length_b                   13.689(4)
_cell_length_c                   19.969(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.12(3)
_cell_angle_gamma                90
_cell_volume                     3319.3(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1635
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      72.8630
_cell_measurement_theta_min      3.9180
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.797
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 11 0.0212
8 -1 -7 0.0145
-1 1 -12 0.0280
-3 -8 2 0.0009
3 8 -1 0.0009

_exptl_crystal_size_max          0.064
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.004
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1197
_diffrn_reflns_av_unetI/netI     0.1660
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12807
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         3.695
_diffrn_ambient_temperature      100.0(4)
_diffrn_detector_area_resol_mean 5.2774
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -62.00  33.00   1.00   10.00    --  -41.59  38.00 -60.00   95
  2  ω    -66.00  32.00   1.00   10.00    --  -41.59  38.00-150.00   98
  3  ω     29.00  60.00   1.00   10.00    --   41.59-125.00-180.00   31
  4  ω     64.00  90.00   1.00   10.00    --   41.59-125.00-180.00   26
  5  ω     35.00 109.00   1.00   30.00    --  104.59 -94.00 -90.00   74
  6  ω     86.00 115.00   1.00   30.00    --  104.59-111.00-180.00   29
  7  ω     56.00 129.00   1.00   30.00    --  104.59 -45.00-120.00   73
  8  ω     97.00 177.00   1.00   30.00    --  104.59  45.00  30.00   80
  9  ω    100.00 175.00   1.00   30.00    --  104.59 111.00-150.00   75
 10  ω     88.00 123.00   1.00   30.00    --  104.59 178.00 -90.00   35
 11  ω     82.00 121.00   1.00   30.00    --  104.59 178.00 150.00   39
 12  ω     74.00 109.00   1.00   30.00    --  104.59 -94.00  30.00   35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3279
_reflns_number_total             5872
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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         0.436
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         5872
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1212
_refine_ls_R_factor_gt           0.0673
_refine_ls_restrained_S_all      0.933
_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)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1610
_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. Uiso/Uaniso restraints and constraints
Uanis(C31B) = Uanis(C31A)
Uanis(C29B) = Uanis(C29A)
Uanis(C28B) = Uanis(C28A)
Uanis(C27B) = Uanis(C27A)
Uanis(C30B) = Uanis(C30A)
Uanis(C32B) = Uanis(C32A)
3. Others
 Fixed Sof: C28B(0.5) H28A(0.5) H28B(0.5) C27B(0.5) H27A(0.5) H27B(0.5)
 C28A(0.5) H28C(0.5) H28D(0.5) C27A(0.5) H27C(0.5) H27D(0.5) C29B(0.5)
 H29A(0.5) H29B(0.5) C29A(0.5) H29C(0.5) H29D(0.5) H26C(0.5) H26D(0.5)
 H26A(0.5) H26B(0.5) C30B(0.5) H30A(0.5) H30B(0.5) C31B(0.5) H31A(0.5)
 H31B(0.5) C31A(0.5) H31C(0.5) H31D(0.5) C32B(0.5) H32A(0.5) H32B(0.5)
 H32C(0.5) C30A(0.5) H30C(0.5) H30D(0.5) C32A(0.5) H32D(0.5) H32E(0.5) H32F(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C16(H16A,H16B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C28B(H28A,H28B), C27B(H27A,H27B),
 C28A(H28C,H28D), C27A(H27C,H27D), C29B(H29A,H29B), C29A(H29C,H29D), C26(H26C,
 H26D), C26(H26A,H26B), C30B(H30A,H30B), C31B(H31A,H31B), C31A(H31C,H31D),
 C30A(H30C,H30D)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C11(H11), C10(H10), C13(H13), C3(H3A), C14(H14), C6(H6),
 C2(H2A)
4.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C32B(H32A,H32B,H32C), C32A(H32D,H32E,H32F)
;
_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
S2 S 0.38417(8) 1.32937(10) 0.17342(5) 0.0316(3) Uani 1 1 d . . . . .
S1 S -0.30828(9) 0.79907(10) 0.03030(5) 0.0337(3) Uani 1 1 d . . . . .
O1 O 0.1385(2) 1.1518(3) 0.07881(13) 0.0340(8) Uani 1 1 d . . . . .
O2 O 0.4149(3) 1.2275(3) 0.19156(15) 0.0388(8) Uani 1 1 d . . . . .
O4 O 0.3880(2) 1.3864(3) 0.23642(14) 0.0357(8) Uani 1 1 d . . . . .
O3 O 0.4425(2) 1.3747(3) 0.12999(15) 0.0433(9) Uani 1 1 d . . . . .
N2 N 0.0649(3) 1.1549(3) 0.17079(16) 0.0341(9) Uani 1 1 d . . . . .
H2 H 0.0728 1.1835 0.2114 0.041 Uiso 1 1 calc R . . . .
N4 N 0.2500 0.5942(5) -0.2500 0.0307(12) Uani 1 2 d S T P . .
N1 N -0.3045(3) 0.8285(3) 0.15943(16) 0.0316(9) Uani 1 1 d . . . . .
N3 N 0.1723(3) 1.2814(3) 0.15431(16) 0.0337(9) Uani 1 1 d . . . . .
H3 H 0.1582 1.3090 0.1905 0.040 Uiso 1 1 calc R . . . .
N5 N 0.2500 0.8587(5) 0.2500 0.0411(14) Uani 1 2 d S T P . .
C12 C -0.0095(3) 1.0769(4) 0.1537(2) 0.0291(10) Uani 1 1 d . . . . .
C9 C -0.1691(3) 0.9282(4) 0.12679(19) 0.0280(10) Uani 1 1 d . . . . .
C11 C -0.0565(3) 1.0474(4) 0.20521(19) 0.0302(10) Uani 1 1 d . . . . .
H11 H -0.0350 1.0786 0.2497 0.036 Uiso 1 1 calc R . . . .
C10 C -0.1345(3) 0.9731(4) 0.19264(19) 0.0302(10) Uani 1 1 d . . . . .
H10 H -0.1643 0.9527 0.2288 0.036 Uiso 1 1 calc R . . . .
C15 C 0.1260(3) 1.1907(4) 0.13077(19) 0.0291(10) Uani 1 1 d . . . . .
C18 C 0.2176(3) 0.7959(4) -0.3931(2) 0.0324(10) Uani 1 1 d . . . . .
H18A H 0.1815 0.7534 -0.4334 0.039 Uiso 1 1 calc R . . . .
H18B H 0.2715 0.8374 -0.4069 0.039 Uiso 1 1 calc R . . . .
C13 C -0.0420(4) 1.0296(4) 0.0883(2) 0.0326(10) Uani 1 1 d . . . . .
H13 H -0.0097 1.0475 0.0528 0.039 Uiso 1 1 calc R . . . .
C3 C -0.5337(4) 0.6518(4) 0.1327(2) 0.0356(11) Uani 1 1 d . . . . .
H3A H -0.5795 0.6227 0.1572 0.043 Uiso 1 1 calc R . . . .
C19 C 0.2791(3) 0.7320(4) -0.3316(2) 0.0353(11) Uani 1 1 d . . . . .
H19A H 0.3120 0.7735 -0.2901 0.042 Uiso 1 1 calc R . . . .
H19B H 0.3395 0.6971 -0.3434 0.042 Uiso 1 1 calc R . . . .
C14 C -0.1214(4) 0.9566(4) 0.07575(19) 0.0340(11) Uani 1 1 d . . . . .
H14 H -0.1435 0.9255 0.0313 0.041 Uiso 1 1 calc R . . . .
C1 C -0.3866(3) 0.7600(4) 0.1322(2) 0.0325(11) Uani 1 1 d . . . . .
C4 C -0.5505(4) 0.6278(4) 0.0618(2) 0.0343(11) Uani 1 1 d . . . . .
C7 C -0.4016(4) 0.7351(4) 0.0615(2) 0.0324(10) Uani 1 1 d . . . . .
C8 C -0.2570(3) 0.8546(4) 0.11366(19) 0.0300(10) Uani 1 1 d . . . . .
C20 C 0.2010(3) 0.6579(4) -0.3142(2) 0.0316(10) Uani 1 1 d . . . . .
H20A H 0.1375 0.6938 -0.3072 0.038 Uiso 1 1 calc R . . . .
H20B H 0.1725 0.6146 -0.3553 0.038 Uiso 1 1 calc R . . . .
C6 C -0.4824(4) 0.6698(4) 0.0267(2) 0.0329(10) Uani 1 1 d . . . . .
H6 H -0.4912 0.6538 -0.0209 0.039 Uiso 1 1 calc R . . . .
C16 C 0.2419(3) 1.3299(4) 0.12063(19) 0.0309(10) Uani 1 1 d . . . . .
H16A H 0.2169 1.3982 0.1106 0.037 Uiso 1 1 calc R . . . .
H16B H 0.2357 1.2973 0.0754 0.037 Uiso 1 1 calc R . . . .
C21 C 0.1576(3) 0.5311(4) -0.2402(2) 0.0338(11) Uani 1 1 d . . . . .
H21A H 0.1210 0.4984 -0.2853 0.041 Uiso 1 1 calc R . . . .
H21B H 0.1024 0.5743 -0.2292 0.041 Uiso 1 1 calc R . . . .
C5 C -0.6425(4) 0.5588(4) 0.0244(2) 0.0402(12) Uani 1 1 d . . . . .
H5A H -0.6476 0.5055 0.0560 0.060 Uiso 1 1 calc GR . . . .
H5B H -0.6268 0.5318 -0.0172 0.060 Uiso 1 1 calc GR . . . .
H5C H -0.7124 0.5945 0.0100 0.060 Uiso 1 1 calc GR . . . .
C22 C 0.1911(4) 0.4531(4) -0.1834(2) 0.0388(11) Uani 1 1 d . . . . .
H22A H 0.2223 0.3961 -0.2015 0.047 Uiso 1 1 calc R . . . .
H22B H 0.2487 0.4795 -0.1426 0.047 Uiso 1 1 calc R . . . .
C2 C -0.4528(4) 0.7164(4) 0.1677(2) 0.0377(11) Uani 1 1 d . . . . .
H2A H -0.4426 0.7308 0.2158 0.045 Uiso 1 1 calc R . . . .
C23 C 0.0927(4) 0.4205(4) -0.1604(2) 0.0432(13) Uani 1 1 d . . . . .
H23A H 0.0296 0.4087 -0.2026 0.052 Uiso 1 1 calc R . . . .
H23B H 0.1108 0.3579 -0.1348 0.052 Uiso 1 1 calc R . . . .
C17 C 0.1303(4) 0.8617(4) -0.3773(2) 0.0429(12) Uani 1 1 d . . . . .
H17A H 0.1016 0.9073 -0.4162 0.064 Uiso 1 1 calc GR . . . .
H17B H 0.1634 0.8986 -0.3341 0.064 Uiso 1 1 calc GR . . . .
H17C H 0.0699 0.8214 -0.3714 0.064 Uiso 1 1 calc GR . . . .
C24 C 0.0588(5) 0.4938(5) -0.1142(2) 0.0570(16) Uani 1 1 d . . . . .
H24A H 0.0360 0.5547 -0.1402 0.086 Uiso 1 1 calc GR . . . .
H24B H 0.1211 0.5068 -0.0727 0.086 Uiso 1 1 calc GR . . . .
H24C H -0.0029 0.4674 -0.0997 0.086 Uiso 1 1 calc GR . . . .
C28B C 0.3378(7) 0.8895(8) 0.2120(4) 0.0345(16) Uani 0.5 1 d . . . A -1
H28A H 0.4092 0.8993 0.2484 0.041 Uiso 0.5 1 calc R . . A -1
H28B H 0.3472 0.8340 0.1825 0.041 Uiso 0.5 1 calc R . . A -1
C27B C 0.3137(7) 0.9810(8) 0.1660(4) 0.0344(15) Uani 0.5 1 d . . . A -1
H27A H 0.2345 0.9814 0.1395 0.041 Uiso 0.5 1 calc R . . A -1
H27B H 0.3283 1.0392 0.1968 0.041 Uiso 0.5 1 calc R . . A -1
C28A C 0.2811(7) 0.9393(8) 0.2142(4) 0.0345(16) Uani 0.5 1 d . . . A -2
H28C H 0.3201 0.9883 0.2491 0.041 Uiso 0.5 1 calc R . . A -2
H28D H 0.2137 0.9705 0.1837 0.041 Uiso 0.5 1 calc R . . A -2
C27A C 0.3546(7) 0.9102(8) 0.1698(4) 0.0344(15) Uani 0.5 1 d . . . A -2
H27C H 0.3220 0.8521 0.1418 0.041 Uiso 0.5 1 calc R . . A -2
H27D H 0.4271 0.8904 0.2016 0.041 Uiso 0.5 1 calc R . . A -2
C29B C 0.1401(7) 0.8345(8) 0.1812(4) 0.0298(14) Uani 0.5 1 d . . . A -1
H29A H 0.0818 0.8079 0.1997 0.036 Uiso 0.5 1 calc R . . A -1
H29B H 0.1128 0.8974 0.1582 0.036 Uiso 0.5 1 calc R . . A -1
C29A C 0.2222(7) 0.7646(7) 0.2180(4) 0.0298(14) Uani 0.5 1 d . . . A -2
H29C H 0.1981 0.7207 0.2500 0.036 Uiso 0.5 1 calc R . . A -2
H29D H 0.2876 0.7352 0.2085 0.036 Uiso 0.5 1 calc R . . A -2
C26 C 0.3739(7) 0.9887(5) 0.1194(3) 0.068(2) Uani 1 1 d . . . . .
H26C H 0.4490 0.9996 0.1513 0.082 Uiso 0.5 1 calc R . . A -1
H26D H 0.3503 1.0534 0.0982 0.082 Uiso 0.5 1 calc R . . A -1
H26A H 0.3076 1.0301 0.1019 0.082 Uiso 0.5 1 calc R . . A -2
H26B H 0.4368 1.0309 0.1437 0.082 Uiso 0.5 1 calc R . . A -2
C30B C 0.1527(11) 0.7658(11) 0.1256(5) 0.035(2) Uani 0.5 1 d . . . A -1
H30A H 0.2145 0.7885 0.1088 0.042 Uiso 0.5 1 calc R . . A -1
H30B H 0.1721 0.7003 0.1465 0.042 Uiso 0.5 1 calc R . . A -1
C25 C 0.3966(7) 0.9383(7) 0.0629(3) 0.092(3) Uani 1 1 d . . . . .
H25A H 0.4741 0.9183 0.0768 0.138 Uiso 1 1 calc GR . . . .
H25B H 0.3819 0.9816 0.0221 0.138 Uiso 1 1 calc GR . . . .
H25C H 0.3495 0.8804 0.0510 0.138 Uiso 1 1 calc GR . . . .
C31B C 0.0530(8) 0.7572(9) 0.0649(5) 0.0400(17) Uani 0.5 1 d . . . A -1
H31A H 0.0309 0.8232 0.0454 0.048 Uiso 0.5 1 calc R . . A -1
H31B H -0.0078 0.7306 0.0810 0.048 Uiso 0.5 1 calc R . . A -1
C31A C 0.1345(8) 0.6919(9) 0.0996(4) 0.0400(17) Uani 0.5 1 d . . . A -2
H31C H 0.2079 0.6907 0.0918 0.048 Uiso 0.5 1 calc R . . A -2
H31D H 0.1240 0.6292 0.1215 0.048 Uiso 0.5 1 calc R . . A -2
C32B C 0.0699(15) 0.6907(15) 0.0062(7) 0.050(3) Uani 0.5 1 d . . . A -1
H32A H 0.0002 0.6844 -0.0313 0.075 Uiso 0.5 1 calc GR . . A -1
H32B H 0.0945 0.6260 0.0255 0.075 Uiso 0.5 1 calc GR . . A -1
H32C H 0.1257 0.7196 -0.0128 0.075 Uiso 0.5 1 calc GR . . A -1
O5 O 0.2500 0.5424(5) 0.2500 0.107(3) Uani 1 2 d S T P . .
C30A C 0.1300(11) 0.7767(11) 0.1498(5) 0.035(2) Uani 0.5 1 d . . . A -2
H30C H 0.1383 0.8398 0.1277 0.042 Uiso 0.5 1 calc R . . A -2
H30D H 0.0579 0.7767 0.1594 0.042 Uiso 0.5 1 calc R . . A -2
C32A C 0.0459(15) 0.7027(15) 0.0294(7) 0.050(3) Uani 0.5 1 d . . . A -2
H32D H 0.0541 0.6506 -0.0023 0.075 Uiso 0.5 1 calc GR . . A -2
H32E H 0.0537 0.7663 0.0089 0.075 Uiso 0.5 1 calc GR . . A -2
H32F H -0.0270 0.6982 0.0366 0.075 Uiso 0.5 1 calc GR . . 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
S2 O2 1.465(4) . ?
S2 O4 1.469(3) . ?
S2 O3 1.437(3) . ?
S2 C16 1.805(4) . ?
S1 C7 1.731(5) . ?
S1 C8 1.770(4) . ?
O1 C15 1.218(5) . ?
N2 H2 0.8800 . ?
N2 C12 1.399(6) . ?
N2 C15 1.359(6) . ?
N4 C20 1.524(6) 2_554 ?
N4 C20 1.524(6) . ?
N4 C21 1.516(6) 2_554 ?
N4 C21 1.516(6) . ?
N1 C1 1.388(6) . ?
N1 C8 1.285(6) . ?
N3 H3 0.8800 . ?
N3 C15 1.394(7) . ?
N3 C16 1.424(6) . ?
N5 C28B 1.579(10) . ?
N5 C28A 1.432(11) . ?
N5 C29B 1.678(8) . ?
N5 C29A 1.435(11) . ?
C12 C11 1.393(6) . ?
C12 C13 1.406(6) . ?
C9 C10 1.400(6) . ?
C9 C14 1.386(6) . ?
C9 C8 1.470(7) . ?
C11 H11 0.9500 . ?
C11 C10 1.391(7) . ?
C10 H10 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.523(6) . ?
C18 C17 1.533(7) . ?
C13 H13 0.9500 . ?
C13 C14 1.390(7) . ?
C3 H3A 0.9500 . ?
C3 C4 1.407(6) . ?
C3 C2 1.379(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.528(6) . ?
C14 H14 0.9500 . ?
C1 C7 1.410(6) . ?
C1 C2 1.386(7) . ?
C4 C6 1.388(7) . ?
C4 C5 1.518(7) . ?
C7 C6 1.384(7) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C6 H6 0.9500 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.525(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.519(7) . ?
C2 H2A 0.9500 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.509(8) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C28B H28A 0.9900 . ?
C28B H28B 0.9900 . ?
C28B C27B 1.530(14) . ?
C27B H27A 0.9900 . ?
C27B H27B 0.9900 . ?
C27B C26 1.371(11) . ?
C28A H28C 0.9900 . ?
C28A H28D 0.9900 . ?
C28A C27A 1.518(13) . ?
C27A H27C 0.9900 . ?
C27A H27D 0.9900 . ?
C27A C26 1.539(11) . ?
C29B H29A 0.9900 . ?
C29B H29B 0.9900 . ?
C29B C30B 1.499(13) . ?
C29A H29C 0.9900 . ?
C29A H29D 0.9900 . ?
C29A C30A 1.522(14) . ?
C26 H26C 0.9900 . ?
C26 H26D 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C25 1.423(9) . ?
C30B H30A 0.9900 . ?
C30B H30B 0.9900 . ?
C30B C31B 1.477(14) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C31B H31A 0.9900 . ?
C31B H31B 0.9900 . ?
C31B C32B 1.550(15) . ?
C31A H31C 0.9900 . ?
C31A H31D 0.9900 . ?
C31A C30A 1.544(15) . ?
C31A C32A 1.525(17) . ?
C32B H32A 0.9800 . ?
C32B H32B 0.9800 . ?
C32B H32C 0.9800 . ?
C30A H30C 0.9900 . ?
C30A H30D 0.9900 . ?
C32A H32D 0.9800 . ?
C32A H32E 0.9800 . ?
C32A H32F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 S2 O4 110.80(18) . . ?
O2 S2 C16 107.2(2) . . ?
O4 S2 C16 105.9(2) . . ?
O3 S2 O2 114.4(2) . . ?
O3 S2 O4 113.2(2) . . ?
O3 S2 C16 104.58(18) . . ?
C7 S1 C8 88.9(2) . . ?
C12 N2 H2 116.8 . . ?
C15 N2 H2 116.8 . . ?
C15 N2 C12 126.4(4) . . ?
C20 N4 C20 110.2(5) . 2_554 ?
C21 N4 C20 111.0(2) . 2_554 ?
C21 N4 C20 107.1(2) 2_554 2_554 ?
C21 N4 C20 107.1(2) . . ?
C21 N4 C20 111.0(2) 2_554 . ?
C21 N4 C21 110.5(6) . 2_554 ?
C8 N1 C1 111.4(4) . . ?
C15 N3 H3 119.5 . . ?
C15 N3 C16 121.0(4) . . ?
C16 N3 H3 119.5 . . ?
C28B N5 C29B 101.2(4) . . ?
C28A N5 C29A 122.4(5) . . ?
N2 C12 C13 124.8(4) . . ?
C11 C12 N2 116.5(4) . . ?
C11 C12 C13 118.7(4) . . ?
C10 C9 C8 118.7(4) . . ?
C14 C9 C10 118.9(4) . . ?
C14 C9 C8 122.3(4) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 C12 121.1(4) . . ?
C10 C11 H11 119.5 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.0(4) . . ?
C11 C10 H10 120.0 . . ?
O1 C15 N2 125.7(5) . . ?
O1 C15 N3 121.9(4) . . ?
N2 C15 N3 112.3(4) . . ?
H18A C18 H18B 107.7 . . ?
C19 C18 H18A 108.8 . . ?
C19 C18 H18B 108.8 . . ?
C19 C18 C17 113.7(4) . . ?
C17 C18 H18A 108.8 . . ?
C17 C18 H18B 108.8 . . ?
C12 C13 H13 120.1 . . ?
C14 C13 C12 119.8(4) . . ?
C14 C13 H13 120.1 . . ?
C4 C3 H3A 119.0 . . ?
C2 C3 H3A 119.0 . . ?
C2 C3 C4 121.9(4) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 C20 110.6(3) . . ?
H19A C19 H19B 108.1 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
C9 C14 C13 121.4(4) . . ?
C9 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
N1 C1 C7 114.8(4) . . ?
C2 C1 N1 126.1(4) . . ?
C2 C1 C7 119.0(4) . . ?
C3 C4 C5 120.5(4) . . ?
C6 C4 C3 118.6(4) . . ?
C6 C4 C5 120.8(4) . . ?
C1 C7 S1 109.4(4) . . ?
C6 C7 S1 129.2(3) . . ?
C6 C7 C1 121.4(4) . . ?
N1 C8 S1 115.4(4) . . ?
N1 C8 C9 123.7(4) . . ?
C9 C8 S1 120.8(3) . . ?
N4 C20 C19 116.1(3) . . ?
N4 C20 H20A 108.3 . . ?
N4 C20 H20B 108.3 . . ?
C19 C20 H20A 108.3 . . ?
C19 C20 H20B 108.3 . . ?
H20A C20 H20B 107.4 . . ?
C4 C6 H6 120.2 . . ?
C7 C6 C4 119.6(4) . . ?
C7 C6 H6 120.2 . . ?
S2 C16 H16A 109.2 . . ?
S2 C16 H16B 109.2 . . ?
N3 C16 S2 112.2(3) . . ?
N3 C16 H16A 109.2 . . ?
N3 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
N4 C21 H21A 108.3 . . ?
N4 C21 H21B 108.3 . . ?
N4 C21 C22 116.0(3) . . ?
H21A C21 H21B 107.4 . . ?
C22 C21 H21A 108.3 . . ?
C22 C21 H21B 108.3 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C23 C22 C21 110.9(4) . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
C3 C2 C1 119.4(4) . . ?
C3 C2 H2A 120.3 . . ?
C1 C2 H2A 120.3 . . ?
C22 C23 H23A 108.9 . . ?
C22 C23 H23B 108.9 . . ?
H23A C23 H23B 107.7 . . ?
C24 C23 C22 113.5(5) . . ?
C24 C23 H23A 108.9 . . ?
C24 C23 H23B 108.9 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N5 C28B H28A 107.9 . . ?
N5 C28B H28B 107.9 . . ?
H28A C28B H28B 107.2 . . ?
C27B C28B N5 117.5(8) . . ?
C27B C28B H28A 107.9 . . ?
C27B C28B H28B 107.9 . . ?
C28B C27B H27A 108.6 . . ?
C28B C27B H27B 108.6 . . ?
H27A C27B H27B 107.6 . . ?
C26 C27B C28B 114.7(8) . . ?
C26 C27B H27A 108.6 . . ?
C26 C27B H27B 108.6 . . ?
N5 C28A H28C 108.9 . . ?
N5 C28A H28D 108.9 . . ?
N5 C28A C27A 113.4(9) . . ?
H28C C28A H28D 107.7 . . ?
C27A C28A H28C 108.9 . . ?
C27A C28A H28D 108.9 . . ?
C28A C27A H27C 108.2 . . ?
C28A C27A H27D 108.2 . . ?
C28A C27A C26 116.2(8) . . ?
H27C C27A H27D 107.4 . . ?
C26 C27A H27C 108.2 . . ?
C26 C27A H27D 108.2 . . ?
N5 C29B H29A 107.5 . . ?
N5 C29B H29B 107.5 . . ?
H29A C29B H29B 107.0 . . ?
C30B C29B N5 119.1(8) . . ?
C30B C29B H29A 107.5 . . ?
C30B C29B H29B 107.5 . . ?
N5 C29A H29C 109.9 . . ?
N5 C29A H29D 109.9 . . ?
N5 C29A C30A 108.9(9) . . ?
H29C C29A H29D 108.3 . . ?
C30A C29A H29C 109.9 . . ?
C30A C29A H29D 109.9 . . ?
C27B C26 H26C 101.6 . . ?
C27B C26 H26D 101.6 . . ?
C27B C26 C25 141.7(9) . . ?
C27A C26 H26A 110.4 . . ?
C27A C26 H26B 110.4 . . ?
H26C C26 H26D 104.6 . . ?
H26A C26 H26B 108.6 . . ?
C25 C26 C27A 106.8(7) . . ?
C25 C26 H26C 101.6 . . ?
C25 C26 H26D 101.6 . . ?
C25 C26 H26A 110.4 . . ?
C25 C26 H26B 110.4 . . ?
C29B C30B H30A 108.8 . . ?
C29B C30B H30B 108.8 . . ?
H30A C30B H30B 107.7 . . ?
C31B C30B C29B 113.9(10) . . ?
C31B C30B H30A 108.8 . . ?
C31B C30B H30B 108.8 . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
C26 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C30B C31B H31A 109.0 . . ?
C30B C31B H31B 109.0 . . ?
C30B C31B C32B 113.0(11) . . ?
H31A C31B H31B 107.8 . . ?
C32B C31B H31A 109.0 . . ?
C32B C31B H31B 109.0 . . ?
H31C C31A H31D 108.0 . . ?
C30A C31A H31C 109.3 . . ?
C30A C31A H31D 109.3 . . ?
C32A C31A H31C 109.3 . . ?
C32A C31A H31D 109.3 . . ?
C32A C31A C30A 111.4(10) . . ?
C31B C32B H32A 109.5 . . ?
C31B C32B H32B 109.5 . . ?
C31B C32B H32C 109.5 . . ?
H32A C32B H32B 109.5 . . ?
H32A C32B H32C 109.5 . . ?
H32B C32B H32C 109.5 . . ?
C29A C30A C31A 109.5(10) . . ?
C29A C30A H30C 109.8 . . ?
C29A C30A H30D 109.8 . . ?
C31A C30A H30C 109.8 . . ?
C31A C30A H30D 109.8 . . ?
H30C C30A H30D 108.2 . . ?
C31A C32A H32D 109.5 . . ?
C31A C32A H32E 109.5 . . ?
C31A C32A H32F 109.5 . . ?
H32D C32A H32E 109.5 . . ?
H32D C32A H32F 109.5 . . ?
H32E C32A H32F 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 C7 C6 C4 -178.7(4) . . . . ?
O2 S2 C16 N3 54.4(4) . . . . ?
O4 S2 C16 N3 -63.9(4) . . . . ?
O3 S2 C16 N3 176.3(4) . . . . ?
N2 C12 C11 C10 177.6(4) . . . . ?
N2 C12 C13 C14 -176.2(4) . . . . ?
N4 C21 C22 C23 159.6(4) . . . . ?
N1 C1 C7 S1 0.9(5) . . . . ?
N1 C1 C7 C6 -178.2(4) . . . . ?
N1 C1 C2 C3 177.7(5) . . . . ?
N5 C28B C27B C26 -162.2(7) . . . . ?
N5 C28A C27A C26 169.2(6) . . . . ?
N5 C29B C30B C31B -174.8(9) . . . . ?
N5 C29A C30A C31A 154.3(8) . . . . ?
C12 N2 C15 O1 -11.9(7) . . . . ?
C12 N2 C15 N3 166.2(4) . . . . ?
C12 C11 C10 C9 -1.6(7) . . . . ?
C12 C13 C14 C9 -0.7(7) . . . . ?
C11 C12 C13 C14 1.5(7) . . . . ?
C10 C9 C14 C13 -1.2(7) . . . . ?
C10 C9 C8 S1 177.3(3) . . . . ?
C10 C9 C8 N1 -0.1(7) . . . . ?
C15 N2 C12 C11 174.9(4) . . . . ?
C15 N2 C12 C13 -7.4(7) . . . . ?
C15 N3 C16 S2 -108.3(4) . . . . ?
C18 C19 C20 N4 -175.5(4) . . . . ?
C13 C12 C11 C10 -0.3(7) . . . . ?
C3 C4 C6 C7 -1.2(7) . . . . ?
C14 C9 C10 C11 2.4(7) . . . . ?
C14 C9 C8 S1 -0.9(6) . . . . ?
C14 C9 C8 N1 -178.3(5) . . . . ?
C1 N1 C8 S1 0.7(5) . . . . ?
C1 N1 C8 C9 178.2(4) . . . . ?
C1 C7 C6 C4 0.2(7) . . . . ?
C4 C3 C2 C1 0.7(8) . . . . ?
C7 S1 C8 N1 -0.2(4) . . . . ?
C7 S1 C8 C9 -177.8(4) . . . . ?
C7 C1 C2 C3 -1.7(7) . . . . ?
C8 S1 C7 C1 -0.4(4) . . . . ?
C8 S1 C7 C6 178.6(5) . . . . ?
C8 N1 C1 C7 -1.0(6) . . . . ?
C8 N1 C1 C2 179.5(5) . . . . ?
C8 C9 C10 C11 -175.9(4) . . . . ?
C8 C9 C14 C13 177.0(4) . . . . ?
C20 N4 C20 C19 56.0(3) 2_554 . . . ?
C20 N4 C21 C22 173.4(4) . . . . ?
C20 N4 C21 C22 -66.3(6) 2_554 . . . ?
C16 N3 C15 O1 -3.7(6) . . . . ?
C16 N3 C15 N2 178.1(4) . . . . ?
C21 N4 C20 C19 -62.5(6) 2_554 . . . ?
C21 N4 C20 C19 176.8(4) . . . . ?
C21 N4 C21 C22 52.4(4) 2_554 . . . ?
C21 C22 C23 C24 -75.2(5) . . . . ?
C5 C4 C6 C7 177.8(4) . . . . ?
C2 C3 C4 C6 0.7(7) . . . . ?
C2 C3 C4 C5 -178.2(5) . . . . ?
C2 C1 C7 S1 -179.6(4) . . . . ?
C2 C1 C7 C6 1.3(7) . . . . ?
C17 C18 C19 C20 65.5(5) . . . . ?
C28B N5 C28A C27A 18.2(7) . . . . ?
C28B N5 C29B C30B 52.0(11) . . . . ?
C28B N5 C29A C30A -87.7(8) . . . . ?
C28B C27B C26 C27A 8.9(7) . . . . ?
C28B C27B C26 C25 57.9(14) . . . . ?
C28A N5 C28B C27B -15.0(7) . . . . ?
C28A N5 C29B C30B 89.5(10) . . . . ?
C28A N5 C29A C30A -55.5(9) . . . . ?
C28A C27A C26 C27B -2.4(8) . . . . ?
C28A C27A C26 C25 -153.2(7) . . . . ?
C29B N5 C28B C27B 63.3(9) . . . . ?
C29B N5 C28A C27A -87.8(7) . . . . ?
C29B N5 C29A C30A 10.4(6) . . . . ?
C29B C30B C31B C32B 176.6(12) . . . . ?
C29A N5 C28B C27B 118.8(8) . . . . ?
C29A N5 C28A C27A -39.7(9) . . . . ?
C29A N5 C29B C30B -40.1(9) . . . . ?
C32A C31A C30A C29A -178.0(11) . . . . ?

_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
;
