# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_compound_1
_database_code_depnum_ccdc_archive 'CCDC 1489604'
_audit_update_record             
;
2016-08-16 deposited with the CCDC.
2016-08-25 downloaded from the CCDC.
;
_audit_creation_date             2016-08-05
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2016.07.26 svn.r3321 for OlexSys, GUI svn.r5206)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C9 H11 N2 O5 S, C16 H36 N'
_chemical_formula_sum            'C25 H47 N3 O5 S'
_chemical_formula_weight         501.71
_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                   10.8520(3)
_cell_length_b                   14.2506(6)
_cell_length_c                   19.6911(8)
_cell_angle_alpha                96.202(3)
_cell_angle_beta                 103.112(3)
_cell_angle_gamma                94.223(3)
_cell_volume                     2933.22(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5898
_cell_measurement_temperature    300(1)
_cell_measurement_theta_max      72.2120
_cell_measurement_theta_min      3.1250
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.266
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0559
0 -1 0 0.0559
-5 0 1 0.1412
5 0 -1 0.1172
0 0 1 0.0184
0 0 -1 0.0144

_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.033
_exptl_special_details           
;
 Experiment performed at room temperature due to crystal shattering
 on cooling.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20872
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.536
_diffrn_reflns_theta_min         2.323
_diffrn_ambient_temperature      300(2)
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     50.00 115.00   1.00   35.00    --  105.19-111.00  90.00   65
  2  ω     62.00  96.00   1.00    5.00    --   40.62-125.00 120.00   34
  3  ω     35.00 117.00   1.00   35.00    --  105.19 -61.00  90.00   82
  4  ω     59.00 116.00   1.00   35.00    --  105.19-111.00 -60.00   57
  5  ω     90.00 124.00   1.00   35.00    --  105.19 -45.00 -90.00   34
  6  ω     73.00 100.00   1.00   35.00    --  105.19 -94.00-180.00   27
  7  ω     36.00  71.00   1.00   35.00    --  105.19 -45.00 -90.00   35
  8  ω     23.00  83.00   1.00   35.00    --  105.19 -94.00   0.00   60
  9  ω     24.00 152.00   1.00   35.00    --  105.19 -15.00   0.00  128
 10  ω    114.00 178.00   1.00   35.00    --  105.19 111.00  60.00   64
 11  ω    150.00 175.00   1.00   35.00    --  105.19 111.00   0.00   25
 12  ω    100.00 178.00   1.00   35.00    --  105.19  30.00-180.00   78
 13  ω     34.00 118.00   1.00   35.00    --  105.19 -30.00 150.00   84
 14  ω     22.00  58.00   1.00    5.00    --   40.62 -57.00  30.00   36
 15  ω     27.00  86.00   1.00   35.00    --  105.19 -94.00  90.00   59
 16  ω    -64.00  24.00   1.00    5.00    --  -40.62  38.00 -60.00   88
 17  ω    -40.00 -14.00   1.00    5.00    --  -40.62 -77.00 -90.00   26
 18  ω    -57.00  33.00   1.00    5.00    --  -40.62  57.00  30.00   90
 19  ω   -114.00 -17.00   1.00    5.00    --  -40.62 -38.00 120.00   97
;
_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                7615
_reflns_number_total             11353
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         11353
_refine_ls_number_restraints     549
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0564
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1075P)²+0.1544P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1675
_refine_ls_wR_factor_ref         0.1933
_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,
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1A-C1A
 1.4 with sigma of 0.02
 O1B-C1B
 1.4 with sigma of 0.02
 N1-C5A
 1.4 with sigma of 0.02
 N1-C5B
 1.4 with sigma of 0.02
 C49B-C50B
 1.5 with sigma of 0.02
 C49A-C50A
 1.5 with sigma of 0.02
 C48-C49B
 1.5 with sigma of 0.02
 C48-C49A
 1.5 with sigma of 0.02
 C32-C33A
 1.5 with sigma of 0.02
 C33A-C34A
 1.5 with sigma of 0.02
 C32-C33B
 1.5 with sigma of 0.02
 C33B-C34B
 1.5 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H48C)=Sof(H48D)=Sof(C49B)=Sof(H49C)=Sof(H49D)=Sof(C50B)=Sof(H50D)=
 Sof(H50E)=Sof(H50F)=1-FVAR(1)
 Sof(H48A)=Sof(H48B)=Sof(C49A)=Sof(H49A)=Sof(H49B)=Sof(C50A)=Sof(H50A)=
 Sof(H50B)=Sof(H50C)=FVAR(1)
 Sof(H32C)=Sof(H32D)=Sof(C33B)=Sof(H33C)=Sof(H33D)=Sof(C34B)=Sof(H34D)=
 Sof(H34E)=Sof(H34F)=1-FVAR(2)
 Sof(H32A)=Sof(H32B)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=
 Sof(H34B)=Sof(H34C)=FVAR(2)
 Sof(H29C)=Sof(H29D)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(3)
 Sof(H29A)=Sof(H29B)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(3)
 Sof(O1B)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C5B)=Sof(C6B)=Sof(H6B)=
 Sof(C7B)=Sof(H7B)=Sof(C2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=1-FVAR(4)
 Sof(O1A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C5A)=Sof(C4A)=Sof(H4A)=
 Sof(C3A)=Sof(H3A)=Sof(C2A)=Sof(C7A)=Sof(H7A)=Sof(C6A)=Sof(H6A)=FVAR(4)
 Fixed Sof: H1A(0.5) H1B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B),
 C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B), C29(H29C,H29D),
  C29(H29A,H29B), C31(H31A,H31B), C32(H32A,H32B), C32(H32C,H32D), C33A(H33A,
 H33B), C33B(H33C,H33D), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,H43B), C44(H44A,H44B),
  C45(H45A,H45B), C47(H47A,H47B), C48(H48A,H48B), C48(H48C,H48D), C49A(H49A,
 H49B), C49B(H49C,H49D), C18(H18A,H18B)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1A), N1(H1B), N2(H2), C4A(H4A), C3A(H3A), C7A(H7A), C6A(H6A), C6B(H6B),
 C7B(H7B), C3B(H3B), C4B(H4B), N3(H3), N4(H4), C12(H12), C13(H13), C15(H15),
 C16(H16)
5.c Fitted hexagon refined as free rotating group:
 C5A(C4A,C3A,C2A,C7A,C6A), C5B(C6B,C7B,C2B,C3B,C4B)
5.d Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C22(H22A,H22B,H22C), C26(H26A,H26B,
 H26C), C30A(H30A,H30B,H30C), C34A(H34A,H34B,H34C), C30B(H30D,H30E,H30F),
 C34B(H34D,H34E,H34F), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C46(H46A,H46B,
 H46C), C50A(H50A,H50B,H50C), C50B(H50D,H50E,H50F), C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.42682(5) 0.65223(5) 0.33708(3) 0.08181(18) Uani 1 1 d . U . . .
O2 O 0.43796(19) 0.6989(2) 0.13534(11) 0.1262(8) Uani 1 1 d . U . . .
O3 O 0.39975(18) 0.72934(14) 0.38409(9) 0.0994(5) Uani 1 1 d . U . . .
O4 O 0.51689(17) 0.59353(15) 0.37248(10) 0.1011(5) Uani 1 1 d . U . . .
O5 O 0.31183(15) 0.60006(14) 0.29366(11) 0.1005(5) Uani 1 1 d . U . . .
N1 N 0.3186(2) 0.8234(2) 0.14284(12) 0.1127(8) Uani 1 1 d D U . . .
H1A H 0.3044 0.8711 0.1696 0.135 Uiso 0.5 1 calc R . P A 1
H1B H 0.2997 0.8630 0.1741 0.135 Uiso 0.5 1 calc R . P B 2
N2 N 0.4320(2) 0.77257(19) 0.24186(12) 0.1026(6) Uani 1 1 d . U . . .
H2 H 0.4081 0.8201 0.2646 0.123 Uiso 1 1 calc R . . . .
C8 C 0.3986(2) 0.7603(3) 0.17067(15) 0.1011(8) Uani 1 1 d . U . . .
C9 C 0.5067(2) 0.7076(2) 0.28006(15) 0.1016(8) Uani 1 1 d . U . . .
H9A H 0.5861 0.7415 0.3076 0.122 Uiso 1 1 calc R . . . .
H9B H 0.5269 0.6591 0.2469 0.122 Uiso 1 1 calc R . . . .
O1A O 0.0620(14) 0.8063(10) -0.1400(6) 0.146(4) Uani 0.517(19) 1 d D U P C 1
C1A C -0.0137(14) 0.8752(13) -0.1653(13) 0.125(4) Uani 0.517(19) 1 d D U P C 1
H1AA H -0.0374 0.8641 -0.2158 0.187 Uiso 0.517(19) 1 calc GR . P C 1
H1AB H 0.0328 0.9367 -0.1504 0.187 Uiso 0.517(19) 1 calc GR . P C 1
H1AC H -0.0889 0.8723 -0.1473 0.187 Uiso 0.517(19) 1 calc GR . P C 1
C5A C 0.2576(8) 0.8105(7) 0.0686(3) 0.102(3) Uani 0.517(19) 1 d D U P C 1
C4A C 0.1759(11) 0.8798(7) 0.0525(4) 0.091(2) Uani 0.517(19) 1 d G U P C 1
H4A H 0.1655 0.9251 0.0880 0.109 Uiso 0.517(19) 1 calc R . P C 1
C3A C 0.1097(10) 0.8815(7) -0.0165(5) 0.101(2) Uani 0.517(19) 1 d G U P C 1
H3A H 0.0550 0.9279 -0.0273 0.121 Uiso 0.517(19) 1 calc R . P C 1
C2A C 0.1252(8) 0.8138(8) -0.0695(3) 0.123(3) Uani 0.517(19) 1 d G U P C 1
C7A C 0.2069(12) 0.7445(11) -0.0534(3) 0.142(4) Uani 0.517(19) 1 d G U P C 1
H7A H 0.2173 0.6992 -0.0888 0.171 Uiso 0.517(19) 1 calc R . P C 1
C6A C 0.2732(11) 0.7428(10) 0.0157(3) 0.136(4) Uani 0.517(19) 1 d G U P C 1
H6A H 0.3278 0.6965 0.0264 0.163 Uiso 0.517(19) 1 calc R . P C 1
O1B O 0.0964(15) 0.8482(13) -0.1366(6) 0.148(5) Uani 0.483(19) 1 d D U P C 2
C1B C -0.023(2) 0.886(2) -0.1514(16) 0.167(9) Uani 0.483(19) 1 d D U P C 2
H1BA H -0.0535 0.8842 -0.2013 0.251 Uiso 0.483(19) 1 calc GR . P C 2
H1BB H -0.0138 0.9502 -0.1293 0.251 Uiso 0.483(19) 1 calc GR . P C 2
H1BC H -0.0831 0.8485 -0.1335 0.251 Uiso 0.483(19) 1 calc GR . P C 2
C5B C 0.2608(8) 0.8368(9) 0.0735(3) 0.099(2) Uani 0.483(19) 1 d D U P C 2
C6B C 0.3180(9) 0.8040(13) 0.0204(4) 0.132(5) Uani 0.483(19) 1 d G U P C 2
H6B H 0.3961 0.7794 0.0316 0.159 Uiso 0.483(19) 1 calc R . P C 2
C7B C 0.2584(11) 0.8078(14) -0.0495(3) 0.141(5) Uani 0.483(19) 1 d G U P C 2
H7B H 0.2967 0.7858 -0.0851 0.169 Uiso 0.483(19) 1 calc R . P C 2
C2B C 0.1417(9) 0.8445(9) -0.0662(4) 0.121(3) Uani 0.483(19) 1 d G U P C 2
C3B C 0.0845(7) 0.8774(8) -0.0131(5) 0.102(3) Uani 0.483(19) 1 d G U P C 2
H3B H 0.0064 0.9020 -0.0243 0.122 Uiso 0.483(19) 1 calc R . P C 2
C4B C 0.1441(9) 0.8736(8) 0.0568(5) 0.089(2) Uani 0.483(19) 1 d G U P C 2
H4B H 0.1058 0.8956 0.0924 0.107 Uiso 0.483(19) 1 calc R . P C 2
N6 N 0.7864(2) 0.73580(17) 0.10522(12) 0.0958(6) Uani 1 1 d . U . . .
C19 C 0.9220(2) 0.7126(2) 0.13620(16) 0.1042(8) Uani 1 1 d . U . . .
H19A H 0.9773 0.7715 0.1495 0.125 Uiso 1 1 calc R . . . .
H19B H 0.9223 0.6838 0.1787 0.125 Uiso 1 1 calc R . . . .
C20 C 0.9762(3) 0.6477(3) 0.08808(17) 0.1138(9) Uani 1 1 d . U . . .
H20A H 0.9936 0.6808 0.0502 0.137 Uiso 1 1 calc R . . . .
H20B H 0.9149 0.5933 0.0675 0.137 Uiso 1 1 calc R . . . .
C21 C 1.0974(3) 0.6145(3) 0.1282(2) 0.1315(12) Uani 1 1 d . U . . .
H21A H 1.1585 0.6693 0.1477 0.158 Uiso 1 1 calc R . . . .
H21B H 1.0796 0.5841 0.1671 0.158 Uiso 1 1 calc R . . . .
C22 C 1.1559(4) 0.5462(5) 0.0839(3) 0.193(3) Uani 1 1 d . U . . .
H22A H 1.1606 0.5713 0.0411 0.289 Uiso 1 1 calc GR . . . .
H22B H 1.1045 0.4863 0.0729 0.289 Uiso 1 1 calc GR . . . .
H22C H 1.2399 0.5375 0.1094 0.289 Uiso 1 1 calc GR . . . .
C23 C 0.7856(4) 0.7880(3) 0.04387(19) 0.1239(10) Uani 1 1 d . U . . .
H23A H 0.8148 0.7477 0.0091 0.149 Uiso 1 1 calc R . . . .
H23B H 0.8471 0.8435 0.0591 0.149 Uiso 1 1 calc R . . . .
C24 C 0.6611(4) 0.8202(3) 0.0084(2) 0.1447(13) Uani 1 1 d . U . . .
H24A H 0.6012 0.7651 -0.0122 0.174 Uiso 1 1 calc R . . . .
H24B H 0.6268 0.8562 0.0433 0.174 Uiso 1 1 calc R . . . .
C25 C 0.6751(8) 0.8800(5) -0.0474(3) 0.220(3) Uani 1 1 d . U . . .
H25A H 0.7171 0.8457 -0.0794 0.263 Uiso 1 1 calc R . . . .
H25B H 0.7303 0.9371 -0.0256 0.263 Uiso 1 1 calc R . . . .
C26 C 0.5524(8) 0.9088(5) -0.0898(4) 0.254(4) Uani 1 1 d . U . . .
H26A H 0.5714 0.9552 -0.1189 0.381 Uiso 1 1 calc GR . . . .
H26B H 0.5043 0.9355 -0.0585 0.381 Uiso 1 1 calc GR . . . .
H26C H 0.5037 0.8541 -0.1189 0.381 Uiso 1 1 calc GR . . . .
C27 C 0.7427(3) 0.7945(3) 0.16358(18) 0.1170(10) Uani 1 1 d . U . . .
H27A H 0.6514 0.7959 0.1485 0.140 Uiso 1 1 calc R . . . .
H27B H 0.7585 0.7613 0.2047 0.140 Uiso 1 1 calc R . . . .
C28 C 0.8006(4) 0.8925(3) 0.1851(2) 0.1365(12) Uani 1 1 d . U . . .
H28A H 0.7813 0.9282 0.1454 0.164 Uiso 1 1 calc R . . . .
H28B H 0.8922 0.8930 0.1996 0.164 Uiso 1 1 calc R . . . .
C29 C 0.7517(5) 0.9399(4) 0.2454(3) 0.1695(19) Uani 1 1 d . U . . .
H29C H 0.7247 0.8925 0.2723 0.203 Uiso 0.408(9) 1 calc R . P D 2
H29D H 0.8184 0.9838 0.2765 0.203 Uiso 0.408(9) 1 calc R . P D 2
H29A H 0.6611 0.9431 0.2281 0.203 Uiso 0.592(9) 1 calc R . P D 1
H29B H 0.7614 0.8981 0.2816 0.203 Uiso 0.592(9) 1 calc R . P D 1
C31 C 0.6968(3) 0.6451(2) 0.08276(18) 0.1083(8) Uani 1 1 d . U . . .
H31A H 0.6107 0.6626 0.0697 0.130 Uiso 1 1 calc R . . . .
H31B H 0.7151 0.6127 0.0408 0.130 Uiso 1 1 calc R . . . .
C32 C 0.7002(4) 0.5768(3) 0.1345(2) 0.1368(12) Uani 1 1 d D U . . .
H32A H 0.7824 0.5520 0.1411 0.164 Uiso 0.557(13) 1 calc R . P E 1
H32B H 0.6982 0.6127 0.1789 0.164 Uiso 0.557(13) 1 calc R . P E 1
H32C H 0.6698 0.6021 0.1747 0.164 Uiso 0.443(13) 1 calc R . P E 2
H32D H 0.7850 0.5580 0.1505 0.164 Uiso 0.443(13) 1 calc R . P E 2
C30A C 0.8035(11) 1.0274(6) 0.2764(5) 0.184(4) Uani 0.592(9) 1 d . U P D 1
H30A H 0.8923 1.0341 0.2767 0.277 Uiso 0.592(9) 1 calc GR . P D 1
H30B H 0.7937 1.0361 0.3238 0.277 Uiso 0.592(9) 1 calc GR . P D 1
H30C H 0.7615 1.0742 0.2507 0.277 Uiso 0.592(9) 1 calc GR . P D 1
C33A C 0.6053(14) 0.4963(9) 0.1225(7) 0.169(5) Uani 0.557(13) 1 d D U P E 1
H33A H 0.6082 0.4691 0.1659 0.203 Uiso 0.557(13) 1 calc R . P E 1
H33B H 0.5212 0.5161 0.1063 0.203 Uiso 0.557(13) 1 calc R . P E 1
C34A C 0.6309(18) 0.4280(13) 0.0710(10) 0.284(11) Uani 0.557(13) 1 d D U P E 1
H34A H 0.6010 0.4467 0.0252 0.426 Uiso 0.557(13) 1 calc GR . P E 1
H34B H 0.5882 0.3674 0.0732 0.426 Uiso 0.557(13) 1 calc GR . P E 1
H34C H 0.7209 0.4237 0.0797 0.426 Uiso 0.557(13) 1 calc GR . P E 1
C30B C 0.6470(14) 0.9892(10) 0.2159(9) 0.192(6) Uani 0.408(9) 1 d . U P D 2
H30D H 0.6759 1.0387 0.1920 0.287 Uiso 0.408(9) 1 calc GR . P D 2
H30E H 0.6108 1.0165 0.2527 0.287 Uiso 0.408(9) 1 calc GR . P D 2
H30F H 0.5838 0.9458 0.1831 0.287 Uiso 0.408(9) 1 calc GR . P D 2
C33B C 0.6057(19) 0.4917(12) 0.0882(8) 0.165(6) Uani 0.443(13) 1 d D U P E 2
H33C H 0.5362 0.5179 0.0583 0.197 Uiso 0.443(13) 1 calc R . P E 2
H33D H 0.6503 0.4571 0.0577 0.197 Uiso 0.443(13) 1 calc R . P E 2
C34B C 0.554(2) 0.4277(13) 0.1260(8) 0.262(12) Uani 0.443(13) 1 d D U P E 2
H34D H 0.5193 0.3702 0.0955 0.392 Uiso 0.443(13) 1 calc GR . P E 2
H34E H 0.4888 0.4552 0.1445 0.392 Uiso 0.443(13) 1 calc GR . P E 2
H34F H 0.6203 0.4137 0.1641 0.392 Uiso 0.443(13) 1 calc GR . P E 2
N5 N 0.33047(16) 0.29673(13) 0.42054(10) 0.0766(4) Uani 1 1 d . U . . .
C35 C 0.2245(2) 0.23536(17) 0.43845(13) 0.0819(5) Uani 1 1 d . U . . .
H35A H 0.1451 0.2624 0.4226 0.098 Uiso 1 1 calc R . . . .
H35B H 0.2170 0.1728 0.4120 0.098 Uiso 1 1 calc R . . . .
C36 C 0.2404(3) 0.2240(2) 0.51473(15) 0.1013(7) Uani 1 1 d . U . . .
H36A H 0.2365 0.2847 0.5412 0.122 Uiso 1 1 calc R . . . .
H36B H 0.3230 0.2027 0.5328 0.122 Uiso 1 1 calc R . . . .
C37 C 0.1355(4) 0.1517(4) 0.5243(2) 0.1445(14) Uani 1 1 d . U . . .
H37A H 0.1486 0.0900 0.5026 0.173 Uiso 1 1 calc R . . . .
H37B H 0.1474 0.1481 0.5742 0.173 Uiso 1 1 calc R . . . .
C38 C 0.0072(5) 0.1674(5) 0.4974(3) 0.211(3) Uani 1 1 d . U . . .
H38A H -0.0113 0.1599 0.4470 0.317 Uiso 1 1 calc GR . . . .
H38B H -0.0062 0.2306 0.5145 0.317 Uiso 1 1 calc GR . . . .
H38C H -0.0479 0.1224 0.5125 0.317 Uiso 1 1 calc GR . . . .
C39 C 0.3469(2) 0.39714(16) 0.45853(14) 0.0854(6) Uani 1 1 d . U . . .
H39A H 0.3857 0.3950 0.5078 0.102 Uiso 1 1 calc R . . . .
H39B H 0.4067 0.4349 0.4400 0.102 Uiso 1 1 calc R . . . .
C40 C 0.2292(3) 0.44832(19) 0.45443(17) 0.0993(7) Uani 1 1 d . U . . .
H40A H 0.1688 0.4132 0.4742 0.119 Uiso 1 1 calc R . . . .
H40B H 0.1895 0.4528 0.4057 0.119 Uiso 1 1 calc R . . . .
C41 C 0.2649(3) 0.54642(19) 0.49476(17) 0.1030(8) Uani 1 1 d . U . . .
H41A H 0.3152 0.5411 0.5414 0.124 Uiso 1 1 calc R . . . .
H41B H 0.3180 0.5828 0.4713 0.124 Uiso 1 1 calc R . . . .
C42 C 0.1537(4) 0.5997(2) 0.5018(2) 0.1272(11) Uani 1 1 d . U . . .
H42A H 0.1000 0.6016 0.4561 0.191 Uiso 1 1 calc GR . . . .
H42B H 0.1835 0.6632 0.5239 0.191 Uiso 1 1 calc GR . . . .
H42C H 0.1062 0.5684 0.5300 0.191 Uiso 1 1 calc GR . . . .
C43 C 0.4575(2) 0.25736(18) 0.44334(15) 0.0891(6) Uani 1 1 d . U . . .
H43A H 0.5213 0.2968 0.4289 0.107 Uiso 1 1 calc R . . . .
H43B H 0.4801 0.2636 0.4943 0.107 Uiso 1 1 calc R . . . .
C44 C 0.4652(3) 0.1560(2) 0.41596(18) 0.1049(8) Uani 1 1 d . U . . .
H44A H 0.4431 0.1481 0.3650 0.126 Uiso 1 1 calc R . . . .
H44B H 0.4047 0.1150 0.4315 0.126 Uiso 1 1 calc R . . . .
C45 C 0.5983(3) 0.1280(3) 0.4420(2) 0.1323(12) Uani 1 1 d . U . . .
H45A H 0.6567 0.1654 0.4224 0.159 Uiso 1 1 calc R . . . .
H45B H 0.6233 0.1437 0.4928 0.159 Uiso 1 1 calc R . . . .
C46 C 0.6116(5) 0.0265(4) 0.4240(3) 0.174(2) Uani 1 1 d . U . . .
H46A H 0.5883 0.0103 0.3739 0.261 Uiso 1 1 calc GR . . . .
H46B H 0.5570 -0.0112 0.4449 0.261 Uiso 1 1 calc GR . . . .
H46C H 0.6983 0.0146 0.4416 0.261 Uiso 1 1 calc GR . . . .
C47 C 0.2927(2) 0.29602(18) 0.34175(13) 0.0863(6) Uani 1 1 d . U . . .
H47A H 0.2781 0.2305 0.3201 0.104 Uiso 1 1 calc R . . . .
H47B H 0.2123 0.3232 0.3302 0.104 Uiso 1 1 calc R . . . .
C48 C 0.3846(4) 0.3476(3) 0.30883(19) 0.1252(11) Uani 1 1 d D U . . .
H48A H 0.4707 0.3410 0.3341 0.150 Uiso 0.593(10) 1 calc R . P F 1
H48B H 0.3726 0.4146 0.3132 0.150 Uiso 0.593(10) 1 calc R . P F 1
H48C H 0.4050 0.4128 0.3310 0.150 Uiso 0.407(10) 1 calc R . P F 2
H48D H 0.4626 0.3171 0.3141 0.150 Uiso 0.407(10) 1 calc R . P F 2
C49A C 0.3666(10) 0.3072(9) 0.2247(5) 0.166(4) Uani 0.593(10) 1 d D U P F 1
H49A H 0.4397 0.3274 0.2073 0.199 Uiso 0.593(10) 1 calc R . P F 1
H49B H 0.3502 0.2386 0.2160 0.199 Uiso 0.593(10) 1 calc R . P F 1
C50A C 0.2581(10) 0.3523(8) 0.1958(6) 0.177(4) Uani 0.593(10) 1 d D U P F 1
H50A H 0.2413 0.3421 0.1454 0.266 Uiso 0.593(10) 1 calc GR . P F 1
H50B H 0.2734 0.4191 0.2117 0.266 Uiso 0.593(10) 1 calc GR . P F 1
H50C H 0.1860 0.3261 0.2107 0.266 Uiso 0.593(10) 1 calc GR . P F 1
C49B C 0.3209(12) 0.3443(10) 0.2328(5) 0.122(3) Uani 0.407(10) 1 d D U P F 2
H49C H 0.2914 0.2785 0.2147 0.146 Uiso 0.407(10) 1 calc R . P F 2
H49D H 0.2458 0.3780 0.2302 0.146 Uiso 0.407(10) 1 calc R . P F 2
C50B C 0.3901(15) 0.3814(11) 0.1849(7) 0.183(6) Uani 0.407(10) 1 d D U P F 2
H50D H 0.3326 0.4079 0.1491 0.274 Uiso 0.407(10) 1 calc GR . P F 2
H50E H 0.4281 0.3310 0.1634 0.274 Uiso 0.407(10) 1 calc GR . P F 2
H50F H 0.4554 0.4297 0.2104 0.274 Uiso 0.407(10) 1 calc GR . P F 2
S2 S 0.20674(7) 0.96392(4) 0.28452(4) 0.0968(2) Uani 1 1 d . U . . .
O6 O -0.2874(2) 0.3450(2) 0.29195(17) 0.1415(9) Uani 1 1 d . U . . .
O7 O -0.05659(18) 0.77700(14) 0.31456(11) 0.1011(5) Uani 1 1 d . U . . .
O8 O 0.3392(2) 0.94607(16) 0.29159(16) 0.1307(8) Uani 1 1 d . U . . .
O9 O 0.1898(2) 1.06251(13) 0.30124(12) 0.1225(7) Uani 1 1 d . U . . .
O10 O 0.1280(2) 0.91992(15) 0.21792(10) 0.1111(6) Uani 1 1 d . U . . .
N3 N 0.06730(18) 0.65498(14) 0.31557(12) 0.0868(5) Uani 1 1 d . U . . .
H3 H 0.1435 0.6418 0.3159 0.104 Uiso 1 1 calc R . . . .
N4 N 0.1580(2) 0.80759(15) 0.34280(13) 0.0950(6) Uani 1 1 d . U . . .
H4 H 0.2299 0.7840 0.3507 0.114 Uiso 1 1 calc R . . . .
C10 C -0.2590(5) 0.2532(3) 0.2729(3) 0.1698(19) Uani 1 1 d . U . . .
H10A H -0.2425 0.2485 0.2269 0.255 Uiso 1 1 calc GR . . . .
H10B H -0.3298 0.2085 0.2727 0.255 Uiso 1 1 calc GR . . . .
H10C H -0.1852 0.2394 0.3062 0.255 Uiso 1 1 calc GR . . . .
C11 C -0.1959(3) 0.4185(2) 0.29511(17) 0.1033(8) Uani 1 1 d . U . . .
C12 C -0.2245(3) 0.5066(2) 0.31961(16) 0.0999(7) Uani 1 1 d . U . . .
H12 H -0.3015 0.5127 0.3321 0.120 Uiso 1 1 calc R . . . .
C13 C -0.1411(2) 0.5842(2) 0.32553(14) 0.0898(6) Uani 1 1 d . U . . .
H13 H -0.1616 0.6431 0.3424 0.108 Uiso 1 1 calc R . . . .
C14 C -0.0255(2) 0.57769(18) 0.30696(13) 0.0810(5) Uani 1 1 d . U . . .
C15 C 0.0018(2) 0.48976(19) 0.28167(15) 0.0929(7) Uani 1 1 d . U . . .
H15 H 0.0779 0.4840 0.2681 0.112 Uiso 1 1 calc R . . . .
C16 C -0.0823(3) 0.4095(2) 0.27600(18) 0.1034(8) Uani 1 1 d . U . . .
H16 H -0.0622 0.3502 0.2595 0.124 Uiso 1 1 calc R . . . .
C17 C 0.0488(2) 0.74901(18) 0.32344(13) 0.0843(6) Uani 1 1 d . U . . .
C18 C 0.1555(3) 0.9075(2) 0.35022(15) 0.1027(8) Uani 1 1 d . U . . .
H18A H 0.2090 0.9342 0.3957 0.123 Uiso 1 1 calc R . . . .
H18B H 0.0693 0.9216 0.3498 0.123 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 O3 1.4498(19) . ?
S1 O4 1.4417(19) . ?
S1 O5 1.4432(18) . ?
S1 C9 1.779(3) . ?
O2 C8 1.221(4) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C8 1.367(4) . ?
N1 C5A 1.447(6) . ?
N1 C5B 1.407(7) . ?
N2 H2 0.8600 . ?
N2 C8 1.354(4) . ?
N2 C9 1.437(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
O1A C1A 1.387(13) . ?
O1A C2A 1.391(12) . ?
C1A H1AA 0.9600 . ?
C1A H1AB 0.9600 . ?
C1A H1AC 0.9600 . ?
C5A C4A 1.3900 . ?
C5A C6A 1.3900 . ?
C4A H4A 0.9300 . ?
C4A C3A 1.3900 . ?
C3A H3A 0.9300 . ?
C3A C2A 1.3900 . ?
C2A C7A 1.3900 . ?
C7A H7A 0.9300 . ?
C7A C6A 1.3900 . ?
C6A H6A 0.9300 . ?
O1B C1B 1.422(16) . ?
O1B C2B 1.370(12) . ?
C1B H1BA 0.9600 . ?
C1B H1BB 0.9600 . ?
C1B H1BC 0.9600 . ?
C5B C6B 1.3900 . ?
C5B C4B 1.3900 . ?
C6B H6B 0.9300 . ?
C6B C7B 1.3900 . ?
C7B H7B 0.9300 . ?
C7B C2B 1.3900 . ?
C2B C3B 1.3900 . ?
C3B H3B 0.9300 . ?
C3B C4B 1.3900 . ?
C4B H4B 0.9300 . ?
N6 C19 1.535(4) . ?
N6 C23 1.484(4) . ?
N6 C27 1.531(4) . ?
N6 C31 1.519(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.498(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.509(5) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.507(5) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.501(5) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.489(7) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.512(9) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.466(5) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.520(6) . ?
C29 H29C 0.9700 . ?
C29 H29D 0.9700 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30A 1.350(10) . ?
C29 C30B 1.424(14) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.480(5) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
C32 H32D 0.9700 . ?
C32 C33A 1.446(10) . ?
C32 C33B 1.583(12) . ?
C30A H30A 0.9600 . ?
C30A H30B 0.9600 . ?
C30A H30C 0.9600 . ?
C33A H33A 0.9700 . ?
C33A H33B 0.9700 . ?
C33A C34A 1.416(16) . ?
C34A H34A 0.9600 . ?
C34A H34B 0.9600 . ?
C34A H34C 0.9600 . ?
C30B H30D 0.9600 . ?
C30B H30E 0.9600 . ?
C30B H30F 0.9600 . ?
C33B H33C 0.9700 . ?
C33B H33D 0.9700 . ?
C33B C34B 1.399(15) . ?
C34B H34D 0.9600 . ?
C34B H34E 0.9600 . ?
C34B H34F 0.9600 . ?
N5 C35 1.521(3) . ?
N5 C39 1.520(3) . ?
N5 C43 1.518(3) . ?
N5 C47 1.511(3) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 C36 1.500(4) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C37 1.537(5) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.417(6) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.508(4) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 C41 1.509(4) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C42 1.497(4) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 C44 1.501(4) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C44 C45 1.518(4) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C45 C46 1.476(6) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C47 C48 1.497(4) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C48 H48C 0.9700 . ?
C48 H48D 0.9700 . ?
C48 C49A 1.656(10) . ?
C48 C49B 1.495(10) . ?
C49A H49A 0.9700 . ?
C49A H49B 0.9700 . ?
C49A C50A 1.418(12) . ?
C50A H50A 0.9600 . ?
C50A H50B 0.9600 . ?
C50A H50C 0.9600 . ?
C49B H49C 0.9700 . ?
C49B H49D 0.9700 . ?
C49B C50B 1.450(13) . ?
C50B H50D 0.9600 . ?
C50B H50E 0.9600 . ?
C50B H50F 0.9600 . ?
S2 O8 1.456(2) . ?
S2 O9 1.443(2) . ?
S2 O10 1.4416(19) . ?
S2 C18 1.765(3) . ?
O6 C10 1.398(5) . ?
O6 C11 1.375(4) . ?
O7 C17 1.221(3) . ?
N3 H3 0.8600 . ?
N3 C14 1.405(3) . ?
N3 C17 1.367(3) . ?
N4 H4 0.8600 . ?
N4 C17 1.352(3) . ?
N4 C18 1.419(3) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.378(4) . ?
C11 C16 1.379(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.354(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.391(3) . ?
C14 C15 1.376(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.388(4) . ?
C16 H16 0.9300 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 S1 C9 105.35(15) . . ?
O4 S1 O3 112.98(11) . . ?
O4 S1 O5 114.16(13) . . ?
O4 S1 C9 104.63(12) . . ?
O5 S1 O3 111.77(11) . . ?
O5 S1 C9 107.10(13) . . ?
C8 N1 H1A 119.8 . . ?
C8 N1 H1B 113.4 . . ?
C8 N1 C5A 120.5(4) . . ?
C8 N1 C5B 133.2(5) . . ?
C5A N1 H1A 119.8 . . ?
C5B N1 H1B 113.4 . . ?
C8 N2 H2 119.4 . . ?
C8 N2 C9 121.1(3) . . ?
C9 N2 H2 119.4 . . ?
O2 C8 N1 123.8(3) . . ?
O2 C8 N2 122.5(3) . . ?
N2 C8 N1 113.7(3) . . ?
S1 C9 H9A 109.1 . . ?
S1 C9 H9B 109.1 . . ?
N2 C9 S1 112.48(19) . . ?
N2 C9 H9A 109.1 . . ?
N2 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C1A O1A C2A 121.2(15) . . ?
O1A C1A H1AA 109.5 . . ?
O1A C1A H1AB 109.5 . . ?
O1A C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
C4A C5A N1 110.8(5) . . ?
C4A C5A C6A 120.0 . . ?
C6A C5A N1 129.2(5) . . ?
C5A C4A H4A 120.0 . . ?
C3A C4A C5A 120.0 . . ?
C3A C4A H4A 120.0 . . ?
C4A C3A H3A 120.0 . . ?
C4A C3A C2A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
C3A C2A O1A 125.5(8) . . ?
C7A C2A O1A 114.5(8) . . ?
C7A C2A C3A 120.0 . . ?
C2A C7A H7A 120.0 . . ?
C2A C7A C6A 120.0 . . ?
C6A C7A H7A 120.0 . . ?
C5A C6A H6A 120.0 . . ?
C7A C6A C5A 120.0 . . ?
C7A C6A H6A 120.0 . . ?
C2B O1B C1B 112.1(16) . . ?
O1B C1B H1BA 109.5 . . ?
O1B C1B H1BB 109.5 . . ?
O1B C1B H1BC 109.5 . . ?
H1BA C1B H1BB 109.5 . . ?
H1BA C1B H1BC 109.5 . . ?
H1BB C1B H1BC 109.5 . . ?
C6B C5B N1 117.9(5) . . ?
C6B C5B C4B 120.0 . . ?
C4B C5B N1 121.8(5) . . ?
C5B C6B H6B 120.0 . . ?
C5B C6B C7B 120.0 . . ?
C7B C6B H6B 120.0 . . ?
C6B C7B H7B 120.0 . . ?
C2B C7B C6B 120.0 . . ?
C2B C7B H7B 120.0 . . ?
O1B C2B C7B 114.0(8) . . ?
O1B C2B C3B 125.9(8) . . ?
C7B C2B C3B 120.0 . . ?
C2B C3B H3B 120.0 . . ?
C4B C3B C2B 120.0 . . ?
C4B C3B H3B 120.0 . . ?
C5B C4B H4B 120.0 . . ?
C3B C4B C5B 120.0 . . ?
C3B C4B H4B 120.0 . . ?
C23 N6 C19 109.6(2) . . ?
C23 N6 C27 111.9(3) . . ?
C23 N6 C31 109.9(2) . . ?
C27 N6 C19 107.5(2) . . ?
C31 N6 C19 110.2(2) . . ?
C31 N6 C27 107.7(2) . . ?
N6 C19 H19A 108.5 . . ?
N6 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C20 C19 N6 115.0(2) . . ?
C20 C19 H19A 108.5 . . ?
C20 C19 H19B 108.5 . . ?
C19 C20 H20A 109.6 . . ?
C19 C20 H20B 109.6 . . ?
C19 C20 C21 110.2(3) . . ?
H20A C20 H20B 108.1 . . ?
C21 C20 H20A 109.6 . . ?
C21 C20 H20B 109.6 . . ?
C20 C21 H21A 108.9 . . ?
C20 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
C22 C21 C20 113.5(3) . . ?
C22 C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N6 C23 H23A 108.0 . . ?
N6 C23 H23B 108.0 . . ?
N6 C23 C24 117.1(3) . . ?
H23A C23 H23B 107.3 . . ?
C24 C23 H23A 108.0 . . ?
C24 C23 H23B 108.0 . . ?
C23 C24 H24A 109.2 . . ?
C23 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
C25 C24 C23 112.0(5) . . ?
C25 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C24 C25 H25A 108.4 . . ?
C24 C25 H25B 108.4 . . ?
C24 C25 C26 115.4(7) . . ?
H25A C25 H25B 107.5 . . ?
C26 C25 H25A 108.4 . . ?
C26 C25 H25B 108.4 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N6 C27 H27A 107.9 . . ?
N6 C27 H27B 107.9 . . ?
H27A C27 H27B 107.2 . . ?
C28 C27 N6 117.5(3) . . ?
C28 C27 H27A 107.9 . . ?
C28 C27 H27B 107.9 . . ?
C27 C28 H28A 109.4 . . ?
C27 C28 H28B 109.4 . . ?
C27 C28 C29 111.2(4) . . ?
H28A C28 H28B 108.0 . . ?
C29 C28 H28A 109.4 . . ?
C29 C28 H28B 109.4 . . ?
C28 C29 H29C 110.2 . . ?
C28 C29 H29D 110.2 . . ?
C28 C29 H29A 107.5 . . ?
C28 C29 H29B 107.5 . . ?
H29C C29 H29D 108.5 . . ?
H29A C29 H29B 107.0 . . ?
C30A C29 C28 119.4(6) . . ?
C30A C29 H29A 107.5 . . ?
C30A C29 H29B 107.5 . . ?
C30B C29 C28 107.8(8) . . ?
C30B C29 H29C 110.2 . . ?
C30B C29 H29D 110.2 . . ?
N6 C31 H31A 108.0 . . ?
N6 C31 H31B 108.0 . . ?
H31A C31 H31B 107.2 . . ?
C32 C31 N6 117.3(3) . . ?
C32 C31 H31A 108.0 . . ?
C32 C31 H31B 108.0 . . ?
C31 C32 H32A 107.0 . . ?
C31 C32 H32B 107.0 . . ?
C31 C32 H32C 111.7 . . ?
C31 C32 H32D 111.7 . . ?
C31 C32 C33B 100.5(7) . . ?
H32A C32 H32B 106.8 . . ?
H32C C32 H32D 109.4 . . ?
C33A C32 C31 121.2(6) . . ?
C33A C32 H32A 107.0 . . ?
C33A C32 H32B 107.0 . . ?
C33B C32 H32C 111.7 . . ?
C33B C32 H32D 111.7 . . ?
C29 C30A H30A 109.5 . . ?
C29 C30A H30B 109.5 . . ?
C29 C30A H30C 109.5 . . ?
H30A C30A H30B 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
C32 C33A H33A 110.0 . . ?
C32 C33A H33B 110.0 . . ?
H33A C33A H33B 108.4 . . ?
C34A C33A C32 108.4(12) . . ?
C34A C33A H33A 110.0 . . ?
C34A C33A H33B 110.0 . . ?
C33A C34A H34A 109.5 . . ?
C33A C34A H34B 109.5 . . ?
C33A C34A H34C 109.5 . . ?
H34A C34A H34B 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
C29 C30B H30D 109.5 . . ?
C29 C30B H30E 109.5 . . ?
C29 C30B H30F 109.5 . . ?
H30D C30B H30E 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
C32 C33B H33C 108.5 . . ?
C32 C33B H33D 108.5 . . ?
H33C C33B H33D 107.5 . . ?
C34B C33B C32 115.2(12) . . ?
C34B C33B H33C 108.5 . . ?
C34B C33B H33D 108.5 . . ?
C33B C34B H34D 109.5 . . ?
C33B C34B H34E 109.5 . . ?
C33B C34B H34F 109.5 . . ?
H34D C34B H34E 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?
C39 N5 C35 111.93(18) . . ?
C43 N5 C35 110.92(19) . . ?
C43 N5 C39 105.97(16) . . ?
C47 N5 C35 105.46(17) . . ?
C47 N5 C39 111.25(18) . . ?
C47 N5 C43 111.44(19) . . ?
N5 C35 H35A 108.3 . . ?
N5 C35 H35B 108.3 . . ?
H35A C35 H35B 107.4 . . ?
C36 C35 N5 115.9(2) . . ?
C36 C35 H35A 108.3 . . ?
C36 C35 H35B 108.3 . . ?
C35 C36 H36A 109.6 . . ?
C35 C36 H36B 109.6 . . ?
C35 C36 C37 110.4(3) . . ?
H36A C36 H36B 108.1 . . ?
C37 C36 H36A 109.6 . . ?
C37 C36 H36B 109.6 . . ?
C36 C37 H37A 107.8 . . ?
C36 C37 H37B 107.8 . . ?
H37A C37 H37B 107.1 . . ?
C38 C37 C36 118.1(4) . . ?
C38 C37 H37A 107.8 . . ?
C38 C37 H37B 107.8 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N5 C39 H39A 108.0 . . ?
N5 C39 H39B 108.0 . . ?
H39A C39 H39B 107.2 . . ?
C40 C39 N5 117.4(2) . . ?
C40 C39 H39A 108.0 . . ?
C40 C39 H39B 108.0 . . ?
C39 C40 H40A 109.8 . . ?
C39 C40 H40B 109.8 . . ?
C39 C40 C41 109.5(2) . . ?
H40A C40 H40B 108.2 . . ?
C41 C40 H40A 109.8 . . ?
C41 C40 H40B 109.8 . . ?
C40 C41 H41A 108.7 . . ?
C40 C41 H41B 108.7 . . ?
H41A C41 H41B 107.6 . . ?
C42 C41 C40 114.2(3) . . ?
C42 C41 H41A 108.7 . . ?
C42 C41 H41B 108.7 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N5 C43 H43A 108.1 . . ?
N5 C43 H43B 108.1 . . ?
H43A C43 H43B 107.3 . . ?
C44 C43 N5 116.9(2) . . ?
C44 C43 H43A 108.1 . . ?
C44 C43 H43B 108.1 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 C45 110.6(3) . . ?
H44A C44 H44B 108.1 . . ?
C45 C44 H44A 109.5 . . ?
C45 C44 H44B 109.5 . . ?
C44 C45 H45A 108.7 . . ?
C44 C45 H45B 108.7 . . ?
H45A C45 H45B 107.6 . . ?
C46 C45 C44 114.4(3) . . ?
C46 C45 H45A 108.7 . . ?
C46 C45 H45B 108.7 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N5 C47 H47A 108.1 . . ?
N5 C47 H47B 108.1 . . ?
H47A C47 H47B 107.3 . . ?
C48 C47 N5 117.0(2) . . ?
C48 C47 H47A 108.1 . . ?
C48 C47 H47B 108.1 . . ?
C47 C48 H48A 109.1 . . ?
C47 C48 H48B 109.1 . . ?
C47 C48 H48C 110.4 . . ?
C47 C48 H48D 110.4 . . ?
C47 C48 C49A 112.4(5) . . ?
H48A C48 H48B 107.8 . . ?
H48C C48 H48D 108.6 . . ?
C49A C48 H48A 109.1 . . ?
C49A C48 H48B 109.1 . . ?
C49B C48 C47 106.7(5) . . ?
C49B C48 H48C 110.4 . . ?
C49B C48 H48D 110.4 . . ?
C48 C49A H49A 111.9 . . ?
C48 C49A H49B 111.9 . . ?
H49A C49A H49B 109.6 . . ?
C50A C49A C48 99.2(8) . . ?
C50A C49A H49A 111.9 . . ?
C50A C49A H49B 111.9 . . ?
C49A C50A H50A 109.5 . . ?
C49A C50A H50B 109.5 . . ?
C49A C50A H50C 109.5 . . ?
H50A C50A H50B 109.5 . . ?
H50A C50A H50C 109.5 . . ?
H50B C50A H50C 109.5 . . ?
C48 C49B H49C 107.3 . . ?
C48 C49B H49D 107.3 . . ?
H49C C49B H49D 106.9 . . ?
C50B C49B C48 120.1(11) . . ?
C50B C49B H49C 107.3 . . ?
C50B C49B H49D 107.3 . . ?
C49B C50B H50D 109.5 . . ?
C49B C50B H50E 109.5 . . ?
C49B C50B H50F 109.5 . . ?
H50D C50B H50E 109.5 . . ?
H50D C50B H50F 109.5 . . ?
H50E C50B H50F 109.5 . . ?
O8 S2 C18 105.73(16) . . ?
O9 S2 O8 113.62(14) . . ?
O9 S2 C18 104.25(15) . . ?
O10 S2 O8 111.60(15) . . ?
O10 S2 O9 113.97(13) . . ?
O10 S2 C18 106.78(14) . . ?
C11 O6 C10 117.5(3) . . ?
C14 N3 H3 116.7 . . ?
C17 N3 H3 116.7 . . ?
C17 N3 C14 126.6(2) . . ?
C17 N4 H4 119.6 . . ?
C17 N4 C18 120.7(2) . . ?
C18 N4 H4 119.6 . . ?
O6 C10 H10A 109.5 . . ?
O6 C10 H10B 109.5 . . ?
O6 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O6 C11 C12 115.0(3) . . ?
O6 C11 C16 125.1(3) . . ?
C12 C11 C16 119.9(3) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 C11 120.3(2) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 119.3 . . ?
C12 C13 C14 121.4(3) . . ?
C14 C13 H13 119.3 . . ?
C13 C14 N3 123.7(2) . . ?
C15 C14 N3 118.2(2) . . ?
C15 C14 C13 118.1(2) . . ?
C14 C15 H15 119.4 . . ?
C14 C15 C16 121.1(2) . . ?
C16 C15 H15 119.4 . . ?
C11 C16 C15 119.2(3) . . ?
C11 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
O7 C17 N3 122.9(3) . . ?
O7 C17 N4 123.4(2) . . ?
N4 C17 N3 113.7(2) . . ?
S2 C18 H18A 108.6 . . ?
S2 C18 H18B 108.6 . . ?
N4 C18 S2 114.6(2) . . ?
N4 C18 H18A 108.6 . . ?
N4 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 S1 C9 N2 -58.4(2) . . . . ?
O4 S1 C9 N2 -177.7(2) . . . . ?
O5 S1 C9 N2 60.7(3) . . . . ?
N1 C5A C4A C3A 178.6(7) . . . . ?
N1 C5A C6A C7A -178.3(8) . . . . ?
N1 C5B C6B C7B 174.2(8) . . . . ?
N1 C5B C4B C3B -173.9(9) . . . . ?
C8 N1 C5A C4A 177.0(6) . . . . ?
C8 N1 C5A C6A -4.5(9) . . . . ?
C8 N1 C5B C6B -23.7(9) . . . . ?
C8 N1 C5B C4B 150.3(7) . . . . ?
C8 N2 C9 S1 -120.2(3) . . . . ?
C9 N2 C8 O2 -6.0(5) . . . . ?
C9 N2 C8 N1 174.6(3) . . . . ?
O1A C2A C7A C6A -178.3(10) . . . . ?
C1A O1A C2A C3A 7.8(18) . . . . ?
C1A O1A C2A C7A -174.0(11) . . . . ?
C5A N1 C8 O2 10.8(6) . . . . ?
C5A N1 C8 N2 -169.9(5) . . . . ?
C5A C4A C3A C2A 0.0 . . . . ?
C4A C5A C6A C7A 0.0 . . . . ?
C4A C3A C2A O1A 178.1(11) . . . . ?
C4A C3A C2A C7A 0.0 . . . . ?
C3A C2A C7A C6A 0.0 . . . . ?
C2A C7A C6A C5A 0.0 . . . . ?
C6A C5A C4A C3A 0.0 . . . . ?
O1B C2B C3B C4B -176.8(11) . . . . ?
C1B O1B C2B C7B 179.8(15) . . . . ?
C1B O1B C2B C3B -3.3(19) . . . . ?
C5B N1 C8 O2 0.8(8) . . . . ?
C5B N1 C8 N2 -179.9(6) . . . . ?
C5B C6B C7B C2B 0.0 . . . . ?
C6B C5B C4B C3B 0.0 . . . . ?
C6B C7B C2B O1B 177.2(10) . . . . ?
C6B C7B C2B C3B 0.0 . . . . ?
C7B C2B C3B C4B 0.0 . . . . ?
C2B C3B C4B C5B 0.0 . . . . ?
C4B C5B C6B C7B 0.0 . . . . ?
N6 C19 C20 C21 -168.8(3) . . . . ?
N6 C23 C24 C25 174.1(4) . . . . ?
N6 C27 C28 C29 -177.6(3) . . . . ?
N6 C31 C32 C33A 170.0(8) . . . . ?
N6 C31 C32 C33B -174.8(8) . . . . ?
C19 N6 C23 C24 -177.6(3) . . . . ?
C19 N6 C27 C28 71.9(4) . . . . ?
C19 N6 C31 C32 49.9(4) . . . . ?
C19 C20 C21 C22 178.2(4) . . . . ?
C23 N6 C19 C20 -63.5(4) . . . . ?
C23 N6 C27 C28 -48.6(4) . . . . ?
C23 N6 C31 C32 170.8(3) . . . . ?
C23 C24 C25 C26 175.2(5) . . . . ?
C27 N6 C19 C20 174.7(3) . . . . ?
C27 N6 C23 C24 -58.4(4) . . . . ?
C27 N6 C31 C32 -67.1(4) . . . . ?
C27 C28 C29 C30A 173.8(7) . . . . ?
C27 C28 C29 C30B -93.9(8) . . . . ?
C31 N6 C19 C20 57.6(4) . . . . ?
C31 N6 C23 C24 61.1(4) . . . . ?
C31 N6 C27 C28 -169.4(3) . . . . ?
C31 C32 C33A C34A 74.6(16) . . . . ?
C31 C32 C33B C34B -160.0(19) . . . . ?
N5 C35 C36 C37 -173.5(3) . . . . ?
N5 C39 C40 C41 -179.7(2) . . . . ?
N5 C43 C44 C45 178.8(3) . . . . ?
N5 C47 C48 C49A 156.0(5) . . . . ?
N5 C47 C48 C49B -174.8(6) . . . . ?
C35 N5 C39 C40 -49.7(3) . . . . ?
C35 N5 C43 C44 55.2(3) . . . . ?
C35 N5 C47 C48 -176.9(3) . . . . ?
C35 C36 C37 C38 -55.6(6) . . . . ?
C39 N5 C35 C36 -59.4(3) . . . . ?
C39 N5 C43 C44 176.9(2) . . . . ?
C39 N5 C47 C48 61.5(3) . . . . ?
C39 C40 C41 C42 -172.9(3) . . . . ?
C43 N5 C35 C36 58.7(3) . . . . ?
C43 N5 C39 C40 -170.8(2) . . . . ?
C43 N5 C47 C48 -56.5(3) . . . . ?
C43 C44 C45 C46 173.8(4) . . . . ?
C47 N5 C35 C36 179.5(2) . . . . ?
C47 N5 C39 C40 68.0(3) . . . . ?
C47 N5 C43 C44 -62.0(3) . . . . ?
C47 C48 C49A C50A 78.1(8) . . . . ?
C47 C48 C49B C50B -174.7(11) . . . . ?
O6 C11 C12 C13 179.5(3) . . . . ?
O6 C11 C16 C15 179.9(3) . . . . ?
O8 S2 C18 N4 -62.6(3) . . . . ?
O9 S2 C18 N4 177.3(2) . . . . ?
O10 S2 C18 N4 56.3(3) . . . . ?
N3 C14 C15 C16 176.0(3) . . . . ?
C10 O6 C11 C12 -174.9(4) . . . . ?
C10 O6 C11 C16 5.1(6) . . . . ?
C11 C12 C13 C14 0.3(4) . . . . ?
C12 C11 C16 C15 -0.1(5) . . . . ?
C12 C13 C14 N3 -176.5(2) . . . . ?
C12 C13 C14 C15 0.5(4) . . . . ?
C13 C14 C15 C16 -1.2(4) . . . . ?
C14 N3 C17 O7 -10.0(4) . . . . ?
C14 N3 C17 N4 169.1(2) . . . . ?
C14 C15 C16 C11 1.0(5) . . . . ?
C16 C11 C12 C13 -0.5(5) . . . . ?
C17 N3 C14 C13 -19.8(4) . . . . ?
C17 N3 C14 C15 163.2(2) . . . . ?
C17 N4 C18 S2 -109.0(3) . . . . ?
C18 N4 C17 O7 -3.6(4) . . . . ?
C18 N4 C17 N3 177.2(2) . . . . ?

_shelx_SHELXL_version_number     2014/7
_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
;
####################################################################### 
# 
# 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_Compound_2
_database_code_depnum_ccdc_archive 'CCDC 1489605'
_audit_update_record             
;
2016-07-04 deposited with the CCDC.
2016-08-25 downloaded from the CCDC.
;
#-------------------------------------------------------------------------




_audit_creation_date             2016-05-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C8 H9 N2 O4 S, H2 O, C16 H36 N'
_chemical_formula_sum            'C24 H47 N3 O5 S'
_chemical_formula_weight         489.70
_chemical_absolute_configuration ?
_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      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   9.33311(13)
_cell_length_b                   18.8139(3)
_cell_length_c                   15.7107(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2758.68(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4380
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      72.8370
_cell_measurement_theta_min      3.6620
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 4 5 0.0266
0 -4 -5 0.0266
-5 -1 1 0.1784
5 1 -1 0.1784
0 -5 2 0.0234
0 5 -2 0.0234

_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.047
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0002 3.9994 4.9983 0.2823 0.5165 -0.0289
-0.0002 -3.9994 -4.9983 -0.2823 -0.5165 0.0289
-4.9980 -1.0010 1.0006 0.0764 0.0457 0.8303
4.9980 1.0010 -1.0006 -0.0764 -0.0457 -0.8303
-0.0010 -4.9967 1.9987 0.3628 -0.2685 0.0462
0.0010 4.9967 -1.9987 -0.3628 0.2685 -0.0462

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6432
_diffrn_reflns_point_group_measured_fraction_full 0.715
_diffrn_reflns_point_group_measured_fraction_max 0.690
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.024
_diffrn_reflns_theta_min         3.665
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_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  64.00   1.00    1.62    --   40.37 -38.00  30.00   39
  2  ω     52.00  77.00   1.00    1.62    --   40.37 -99.00   0.00   25
  3  ω     24.00 109.00   1.00    6.48    --  105.19 -94.00  60.00   85
  4  ω     58.00 176.00   1.00    6.48    --  105.19  15.00-180.00  118
  5  ω    141.00 167.00   1.00    6.48    --  105.19 111.00-120.00   26
  6  ω    132.00 159.00   1.00    6.48    --  105.19 111.00-150.00   27
  7  ω    -64.00  31.00   1.00    1.62    --  -40.37  38.00 -60.00   95
;
_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      0.0096845000
_diffrn_orient_matrix_UB_12      -0.0378978000
_diffrn_orient_matrix_UB_13      0.0867958000
_diffrn_orient_matrix_UB_21      -0.0144269000
_diffrn_orient_matrix_UB_22      0.0720237000
_diffrn_orient_matrix_UB_23      0.0457063000
_diffrn_orient_matrix_UB_31      -0.1641377000
_diffrn_orient_matrix_UB_32      -0.0087268000
_diffrn_orient_matrix_UB_33      0.0012103000
_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         0.361
_reflns_Friedel_fraction_full    0.408
_reflns_Friedel_fraction_max     0.380
_reflns_number_gt                3663
_reflns_number_total             3810
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 
;
 Flack x determined using 947 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.033(16)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         3810
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0300
_refine_ls_restrained_S_all      1.031
_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)+(0.0438P)²+0.3377P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0764
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H5A(0.055) H1(0.022) H2(0.02) H17A(0.022) H17B(0.022) H5(0.023)
 H21A(0.021) H21B(0.021) H9A(0.023) H9B(0.023) H13A(0.021) H13B(0.021)
 H23A(0.027) H23B(0.027) H2A(0.029) H18A(0.024) H18B(0.024) H3(0.025) H6(0.027)
 H11A(0.032) H11B(0.032) H22A(0.025) H22B(0.025) H19A(0.026) H19B(0.026)
 H10A(0.024) H10B(0.024) H8A(0.019) H8B(0.019) H1A(0.029) H14A(0.026)
 H14B(0.026) H20A(0.038) H20B(0.038) H20C(0.038) H12A(0.046) H12B(0.046)
 H12C(0.046) H24A(0.05) H24B(0.05) H24C(0.05) H16A(0.058) H16B(0.058)
 H16C(0.058) H15A(0.035) H15B(0.035)
 Fixed X: H5A(0.6727) H1(0.5873) H2(0.6097) H17A(0.1101) H17B(0.1913)
 H5(0.6286) H21A(0.1091) H21B(0.2653) H9A(0.4198) H9B(0.3542) H13A(0.3668)
 H13B(0.2155) H23A(0.1642) H23B(0.0134) H2A(0.1447) H18A(-0.0196) H18B(0.0481)
 H3(0.2305) H6(0.5406) H11A(0.6498) H11B(0.5873) H22A(0.2641) H22B(0.113) H19A(-
 0.0633) H19B(-0.1238) H10A(0.477) H10B(0.5512) H8A(0.4135) H8B(0.5679)
 H1A(0.2989) H14A(0.3068) H14B(0.4597) H20A(-0.3086) H20B(-0.2129) H20C(-
 0.2627) H12A(0.8285) H12B(0.736) H12C(0.801) H24A(0.0011) H24B(0.0246)
 H24C(0.1536) H16A(0.4416) H16B(0.579) H16C(0.4951) H15A(0.3015) H15B(0.4394)
 Fixed Y: H5A(0.3023) H1(0.1257) H2(0.2363) H17A(0.5226) H17B(0.5936)
 H5(0.005) H21A(0.449) H21B(0.4205) H9A(0.5486) H9B(0.4771) H13A(0.5231)
 H13B(0.5586) H23A(0.2979) H23B(0.3333) H2A(-0.0368) H18A(0.5415) H18B(0.6179)
 H3(0.0784) H6(-0.1098) H11A(0.4929) H11B(0.4167) H22A(0.3735) H22B(0.4071)
 H19A(0.6469) H19B(0.5694) H10A(0.4165) H10B(0.4887) H8A(0.3039) H8B(0.3329)
 H1A(-0.1316) H14A(0.6548) H14B(0.6198) H20A(0.6392) H20B(0.6704) H20C(0.5909)
 H12A(0.4063) H12B(0.3716) H12C(0.4477) H24A(0.2873) H24B(0.2247) H24C(0.2535)
 H16A(0.7598) H16B(0.7137) H16C(0.746) H15A(0.6714) H15B(0.625)
 Fixed Z: H5A(0.72) H1(0.5875) H2(0.5731) H17A(0.2545) H17B(0.2728) H5(0.5954)
 H21A(0.4085) H21B(0.42) H9A(0.2738) H9B(0.241) H13A(0.4616) H13B(0.4643)
 H23A(0.3863) H23B(0.3736) H2A(0.5545) H18A(0.3861) H18B(0.3886) H3(0.5496)
 H6(0.5995) H11A(0.2361) H11B(0.22) H22A(0.2829) H22B(0.2651) H19A(0.2595)
 H19B(0.2514) H10A(0.3528) H10B(0.377) H8A(0.4745) H8B(0.4928) H1A(0.5783)
 H14A(0.3823) H14B(0.3868) H20A(0.3003) H20B(0.3733) H20C(0.3769) H12A(0.2573)
 H12B(0.3295) H12C(0.3423) H24A(0.235) H24B(0.2993) H24C(0.2456) H16A(0.4617)
 H16B(0.4774) H16C(0.5548) H15A(0.5282) H15B(0.5407)
;
_atom_sites_solution_hydrogens   mixed
_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 0.41494(5) 0.36600(2) 0.60105(4) 0.01393(12) Uani 1 1 d . . . . .
O1 O 0.31827(16) 0.18851(9) 0.51047(12) 0.0204(3) Uani 1 1 d . . . . .
O003 O 0.27809(16) 0.33349(9) 0.62639(11) 0.0182(3) Uani 1 1 d . . . . .
O4 O 0.51878(17) 0.36596(8) 0.66957(11) 0.0190(3) Uani 1 1 d . . . . .
O2 O 0.39494(18) 0.43491(9) 0.56101(12) 0.0240(4) Uani 1 1 d . . . . .
O5 O 0.7551(2) 0.28990(11) 0.73773(15) 0.0364(5) Uani 1 1 d . . . . .
H5A H 0.6727 0.3023 0.7200 0.055 Uiso 1 1 d G . . . .
N3 N 0.25819(19) 0.51236(10) 0.34995(13) 0.0163(4) Uani 1 1 d . . . . .
N1 N 0.50078(19) 0.12230(10) 0.56906(14) 0.0179(4) Uani 1 1 d . . . . .
H1 H 0.5873 0.1257 0.5875 0.022 Uiso 1 1 calc R . . . .
N2 N 0.52742(18) 0.24153(10) 0.54925(13) 0.0166(4) Uani 1 1 d . . . . .
H2 H 0.6097 0.2363 0.5731 0.020 Uiso 1 1 calc R . . . .
C7 C 0.4380(2) 0.18424(12) 0.54126(15) 0.0162(4) Uani 1 1 d . . . . .
C4 C 0.4395(2) 0.05415(12) 0.57070(15) 0.0169(4) Uani 1 1 d . . . . .
C17 C 0.1455(2) 0.55312(12) 0.29950(16) 0.0182(4) Uani 1 1 d . . . . .
H17A H 0.1101 0.5226 0.2545 0.022 Uiso 1 1 calc R . . . .
H17B H 0.1913 0.5936 0.2728 0.022 Uiso 1 1 calc R . . . .
C5 C 0.5315(2) -0.00313(12) 0.58659(15) 0.0189(5) Uani 1 1 d . . . . .
H5 H 0.6286 0.0050 0.5954 0.023 Uiso 1 1 calc R . . . .
C21 C 0.1990(2) 0.44083(12) 0.37913(16) 0.0177(5) Uani 1 1 d . . . . .
H21A H 0.1091 0.4490 0.4085 0.021 Uiso 1 1 calc R . . . .
H21B H 0.2653 0.4205 0.4200 0.021 Uiso 1 1 calc R . . . .
C9 C 0.3858(2) 0.50218(12) 0.29156(16) 0.0190(5) Uani 1 1 d . . . . .
H9A H 0.4198 0.5486 0.2738 0.023 Uiso 1 1 calc R . . . .
H9B H 0.3542 0.4771 0.2410 0.023 Uiso 1 1 calc R . . . .
C13 C 0.3005(2) 0.55242(12) 0.42958(15) 0.0173(5) Uani 1 1 d . . . . .
H13A H 0.3668 0.5231 0.4616 0.021 Uiso 1 1 calc R . . . .
H13B H 0.2155 0.5586 0.4643 0.021 Uiso 1 1 calc R . . . .
C23 C 0.1013(3) 0.31985(13) 0.34480(18) 0.0226(5) Uani 1 1 d . . . . .
H23A H 0.1642 0.2979 0.3863 0.027 Uiso 1 1 calc R . . . .
H23B H 0.0134 0.3333 0.3736 0.027 Uiso 1 1 calc R . . . .
C2 C 0.2420(3) -0.02835(13) 0.56235(18) 0.0241(5) Uani 1 1 d . . . . .
H2A H 0.1447 -0.0368 0.5545 0.029 Uiso 1 1 calc R . . . .
C18 C 0.0177(2) 0.57980(13) 0.35118(17) 0.0201(5) Uani 1 1 d . . . . .
H18A H -0.0196 0.5415 0.3861 0.024 Uiso 1 1 calc R . . . .
H18B H 0.0481 0.6179 0.3886 0.024 Uiso 1 1 calc R . . . .
C3 C 0.2933(2) 0.04087(12) 0.55929(17) 0.0211(5) Uani 1 1 d . . . . .
H3 H 0.2305 0.0784 0.5496 0.025 Uiso 1 1 calc R . . . .
C6 C 0.4784(3) -0.07216(12) 0.58929(16) 0.0222(5) Uani 1 1 d . . . . .
H6 H 0.5406 -0.1098 0.5995 0.027 Uiso 1 1 calc R . . . .
C11 C 0.6252(3) 0.44828(15) 0.26328(19) 0.0266(5) Uani 1 1 d . . . . .
H11A H 0.6498 0.4929 0.2361 0.032 Uiso 1 1 calc R . . . .
H11B H 0.5873 0.4167 0.2200 0.032 Uiso 1 1 calc R . . . .
C22 C 0.1734(3) 0.38641(13) 0.30881(16) 0.0212(5) Uani 1 1 d . . . . .
H22A H 0.2641 0.3735 0.2829 0.025 Uiso 1 1 calc R . . . .
H22B H 0.1130 0.4071 0.2651 0.025 Uiso 1 1 calc R . . . .
C19 C -0.0993(2) 0.60665(13) 0.29154(17) 0.0220(5) Uani 1 1 d . . . . .
H19A H -0.0633 0.6469 0.2595 0.026 Uiso 1 1 calc R . . . .
H19B H -0.1238 0.5694 0.2514 0.026 Uiso 1 1 calc R . . . .
C10 C 0.5107(2) 0.46153(13) 0.33038(16) 0.0203(5) Uani 1 1 d . . . . .
H10A H 0.4770 0.4165 0.3528 0.024 Uiso 1 1 calc R . . . .
H10B H 0.5512 0.4887 0.3770 0.024 Uiso 1 1 calc R . . . .
C8 C 0.4856(2) 0.30985(12) 0.51838(15) 0.0161(4) Uani 1 1 d . . . . .
H8A H 0.4135 0.3039 0.4745 0.019 Uiso 1 1 calc R . . . .
H8B H 0.5679 0.3329 0.4928 0.019 Uiso 1 1 calc R . . . .
C1 C 0.3340(3) -0.08537(12) 0.57692(16) 0.0240(5) Uani 1 1 d . . . . .
H1A H 0.2989 -0.1316 0.5783 0.029 Uiso 1 1 calc R . . . .
C14 C 0.3691(3) 0.62499(12) 0.41647(17) 0.0218(5) Uani 1 1 d . . . . .
H14A H 0.3068 0.6548 0.3823 0.026 Uiso 1 1 calc R . . . .
H14B H 0.4597 0.6198 0.3868 0.026 Uiso 1 1 calc R . . . .
C20 C -0.2332(3) 0.62883(14) 0.33998(18) 0.0253(5) Uani 1 1 d . . . . .
H20A H -0.3086 0.6392 0.3003 0.038 Uiso 1 1 calc GR . . . .
H20B H -0.2129 0.6704 0.3733 0.038 Uiso 1 1 calc GR . . . .
H20C H -0.2627 0.5909 0.3769 0.038 Uiso 1 1 calc GR . . . .
C12 C 0.7602(3) 0.41540(15) 0.3016(2) 0.0307(6) Uani 1 1 d . . . . .
H12A H 0.8285 0.4063 0.2573 0.046 Uiso 1 1 calc GR . . . .
H12B H 0.7360 0.3716 0.3295 0.046 Uiso 1 1 calc GR . . . .
H12C H 0.8010 0.4477 0.3423 0.046 Uiso 1 1 calc GR . . . .
C24 C 0.0669(3) 0.26637(14) 0.2747(2) 0.0331(6) Uani 1 1 d . . . . .
H24A H 0.0011 0.2873 0.2350 0.050 Uiso 1 1 calc GR . . . .
H24B H 0.0246 0.2247 0.2993 0.050 Uiso 1 1 calc GR . . . .
H24C H 0.1536 0.2535 0.2456 0.050 Uiso 1 1 calc GR . . . .
C16 C 0.4858(3) 0.72584(15) 0.4989(2) 0.0386(7) Uani 1 1 d . . . . .
H16A H 0.4416 0.7598 0.4617 0.058 Uiso 1 1 calc GR . . . .
H16B H 0.5790 0.7137 0.4774 0.058 Uiso 1 1 calc GR . . . .
H16C H 0.4951 0.7460 0.5548 0.058 Uiso 1 1 calc GR . . . .
C15 C 0.3936(3) 0.65922(14) 0.5034(2) 0.0292(6) Uani 1 1 d . . . . .
H15A H 0.3015 0.6714 0.5282 0.035 Uiso 1 1 calc R . . . .
H15B H 0.4394 0.6250 0.5407 0.035 Uiso 1 1 calc R . . . .
H5B H 0.775(4) 0.258(2) 0.711(3) 0.038(10) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O003 1.4711(16) . ?
S1 O4 1.4485(17) . ?
S1 O2 1.4531(17) . ?
S1 C8 1.799(2) . ?
O1 C7 1.221(3) . ?
O5 H5A 0.8502 . ?
O5 H5B 0.75(4) . ?
N3 C17 1.524(3) . ?
N3 C21 1.525(3) . ?
N3 C9 1.516(3) . ?
N3 C13 1.513(3) . ?
N1 H1 0.8600 . ?
N1 C7 1.375(3) . ?
N1 C4 1.404(3) . ?
N2 H2 0.8600 . ?
N2 C7 1.369(3) . ?
N2 C8 1.428(3) . ?
C4 C5 1.400(3) . ?
C4 C3 1.399(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.528(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.391(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.525(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.522(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.522(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C22 1.530(3) . ?
C23 C24 1.526(4) . ?
C2 H2A 0.9300 . ?
C2 C3 1.388(3) . ?
C2 C1 1.393(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.525(3) . ?
C3 H3 0.9300 . ?
C6 H6 0.9300 . ?
C6 C1 1.384(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C10 1.522(3) . ?
C11 C12 1.527(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.522(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C1 H1A 0.9300 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.528(4) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 C15 1.522(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O003 S1 C8 105.63(10) . . ?
O4 S1 O003 112.31(10) . . ?
O4 S1 O2 114.09(10) . . ?
O4 S1 C8 106.92(10) . . ?
O2 S1 O003 112.13(10) . . ?
O2 S1 C8 104.98(11) . . ?
H5A O5 H5B 104.5 . . ?
C17 N3 C21 110.51(16) . . ?
C9 N3 C17 106.93(17) . . ?
C9 N3 C21 110.79(17) . . ?
C13 N3 C17 111.06(17) . . ?
C13 N3 C21 106.59(18) . . ?
C13 N3 C9 111.00(17) . . ?
C7 N1 H1 116.3 . . ?
C7 N1 C4 127.31(18) . . ?
C4 N1 H1 116.3 . . ?
C7 N2 H2 119.6 . . ?
C7 N2 C8 120.73(18) . . ?
C8 N2 H2 119.6 . . ?
O1 C7 N1 124.9(2) . . ?
O1 C7 N2 122.9(2) . . ?
N2 C7 N1 112.25(19) . . ?
C5 C4 N1 117.2(2) . . ?
C3 C4 N1 123.9(2) . . ?
C3 C4 C5 118.9(2) . . ?
N3 C17 H17A 108.4 . . ?
N3 C17 H17B 108.4 . . ?
N3 C17 C18 115.32(19) . . ?
H17A C17 H17B 107.5 . . ?
C18 C17 H17A 108.4 . . ?
C18 C17 H17B 108.4 . . ?
C4 C5 H5 119.8 . . ?
C6 C5 C4 120.4(2) . . ?
C6 C5 H5 119.8 . . ?
N3 C21 H21A 108.4 . . ?
N3 C21 H21B 108.4 . . ?
N3 C21 C22 115.6(2) . . ?
H21A C21 H21B 107.4 . . ?
C22 C21 H21A 108.4 . . ?
C22 C21 H21B 108.4 . . ?
N3 C9 H9A 108.5 . . ?
N3 C9 H9B 108.5 . . ?
N3 C9 C10 115.02(19) . . ?
H9A C9 H9B 107.5 . . ?
C10 C9 H9A 108.5 . . ?
C10 C9 H9B 108.5 . . ?
N3 C13 H13A 108.2 . . ?
N3 C13 H13B 108.2 . . ?
N3 C13 C14 116.40(19) . . ?
H13A C13 H13B 107.3 . . ?
C14 C13 H13A 108.2 . . ?
C14 C13 H13B 108.2 . . ?
H23A C23 H23B 108.0 . . ?
C22 C23 H23A 109.3 . . ?
C22 C23 H23B 109.3 . . ?
C24 C23 H23A 109.3 . . ?
C24 C23 H23B 109.3 . . ?
C24 C23 C22 111.4(2) . . ?
C3 C2 H2A 119.5 . . ?
C3 C2 C1 121.0(2) . . ?
C1 C2 H2A 119.5 . . ?
C17 C18 H18A 109.7 . . ?
C17 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
C19 C18 C17 110.0(2) . . ?
C19 C18 H18A 109.7 . . ?
C19 C18 H18B 109.7 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 C4 120.0(2) . . ?
C2 C3 H3 120.0 . . ?
C5 C6 H6 119.7 . . ?
C1 C6 C5 120.7(2) . . ?
C1 C6 H6 119.7 . . ?
H11A C11 H11B 107.9 . . ?
C10 C11 H11A 109.2 . . ?
C10 C11 H11B 109.2 . . ?
C10 C11 C12 111.9(2) . . ?
C12 C11 H11A 109.2 . . ?
C12 C11 H11B 109.2 . . ?
C21 C22 C23 110.5(2) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C18 C19 H19A 109.3 . . ?
C18 C19 H19B 109.3 . . ?
H19A C19 H19B 107.9 . . ?
C20 C19 C18 111.8(2) . . ?
C20 C19 H19A 109.3 . . ?
C20 C19 H19B 109.3 . . ?
C9 C10 C11 110.0(2) . . ?
C9 C10 H10A 109.7 . . ?
C9 C10 H10B 109.7 . . ?
C11 C10 H10A 109.7 . . ?
C11 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
S1 C8 H8A 109.1 . . ?
S1 C8 H8B 109.1 . . ?
N2 C8 S1 112.55(17) . . ?
N2 C8 H8A 109.1 . . ?
N2 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
C2 C1 H1A 120.5 . . ?
C6 C1 C2 119.0(2) . . ?
C6 C1 H1A 120.5 . . ?
C13 C14 H14A 110.0 . . ?
C13 C14 H14B 110.0 . . ?
C13 C14 C15 108.7(2) . . ?
H14A C14 H14B 108.3 . . ?
C15 C14 H14A 110.0 . . ?
C15 C14 H14B 110.0 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 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 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
C14 C15 H15A 109.0 . . ?
C14 C15 H15B 109.0 . . ?
C16 C15 C14 112.9(3) . . ?
C16 C15 H15A 109.0 . . ?
C16 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?

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
O003 S1 C8 N2 -68.08(16) . . . . ?
O4 S1 C8 N2 51.72(17) . . . . ?
O2 S1 C8 N2 173.25(14) . . . . ?
N3 C17 C18 C19 -169.15(19) . . . . ?
N3 C21 C22 C23 -174.70(18) . . . . ?
N3 C9 C10 C11 174.3(2) . . . . ?
N3 C13 C14 C15 175.79(19) . . . . ?
N1 C4 C5 C6 179.9(2) . . . . ?
N1 C4 C3 C2 -179.7(2) . . . . ?
C7 N1 C4 C5 168.4(2) . . . . ?
C7 N1 C4 C3 -13.0(4) . . . . ?
C7 N2 C8 S1 97.9(2) . . . . ?
C4 N1 C7 O1 -2.7(4) . . . . ?
C4 N1 C7 N2 179.4(2) . . . . ?
C4 C5 C6 C1 -0.4(4) . . . . ?
C17 N3 C21 C22 69.3(2) . . . . ?
C17 N3 C9 C10 -179.45(19) . . . . ?
C17 N3 C13 C14 -62.1(2) . . . . ?
C17 C18 C19 C20 175.9(2) . . . . ?
C5 C4 C3 C2 -1.1(4) . . . . ?
C5 C6 C1 C2 -0.5(4) . . . . ?
C21 N3 C17 C18 69.1(2) . . . . ?
C21 N3 C9 C10 -59.0(3) . . . . ?
C21 N3 C13 C14 177.47(18) . . . . ?
C9 N3 C17 C18 -170.26(19) . . . . ?
C9 N3 C21 C22 -49.0(3) . . . . ?
C9 N3 C13 C14 56.7(2) . . . . ?
C13 N3 C17 C18 -49.0(2) . . . . ?
C13 N3 C21 C22 -169.90(19) . . . . ?
C13 N3 C9 C10 59.3(2) . . . . ?
C13 C14 C15 C16 169.6(2) . . . . ?
C3 C4 C5 C6 1.2(4) . . . . ?
C3 C2 C1 C6 0.6(4) . . . . ?
C8 N2 C7 O1 -2.4(4) . . . . ?
C8 N2 C7 N1 175.6(2) . . . . ?
C1 C2 C3 C4 0.2(4) . . . . ?
C12 C11 C10 C9 173.3(2) . . . . ?
C24 C23 C22 C21 176.8(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.178
_oxdiff_exptl_absorpt_empirical_full_min 0.685
####################################################################### 
# 
# 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_Compound_3a
_database_code_depnum_ccdc_archive 'CCDC 1489606'
_audit_update_record             
;
2016-07-04 deposited with the CCDC.
2016-08-25 downloaded from the CCDC.
;
#-------------------------------------------------------------------


_audit_creation_date             2016-05-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C8 H8 N3 O6 S), 2(C16 H36 N), (H2 O)'
_chemical_formula_sum            'C48 H90 N8 O13 S2'
_chemical_formula_weight         1051.39
_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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.1853(5)
_cell_length_b                   16.9662(4)
_cell_length_c                   19.0342(5)
_cell_angle_alpha                90
_cell_angle_beta                 109.850(3)
_cell_angle_gamma                90
_cell_volume                     5827.5(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6355
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      72.4900
_cell_measurement_theta_min      3.5810
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.349
_exptl_absorpt_correction_T_max  0.272
_exptl_absorpt_correction_T_min  0.027
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2280
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 9 -6 0.1063
6 -9 -7 0.0282
9 2 5 0.1922
5 -9 -7 0.0366
9 3 -10 0.0566
-7 8 6 0.0461
6 -9 1 0.1172
-10 -1 10 0.0511
6 -9 -7 0.0308

_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.094
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.4959 9.2452 -6.1432 0.1972 0.8268 0.5268
6.1729 -8.5626 -6.5928 -0.4786 0.1133 -0.8707
9.0941 1.8549 4.6275 0.8598 -0.2051 -0.4677
5.2378 -8.6651 -7.0229 -0.5596 0.1350 -0.8177
9.4467 3.0409 -10.0275 0.2072 0.8689 -0.4496
-7.1014 8.3362 6.1256 0.3890 -0.0943 0.9164
6.2025 -9.0385 1.2163 -0.1095 -0.4514 -0.8856
-10.4408 -1.3662 9.6729 -0.1846 -0.7756 0.6036
5.7720 -8.6236 -6.7772 -0.5143 0.1219 -0.8489

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11139
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         73.098
_diffrn_reflns_theta_min         3.576
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      4.00  34.00   1.00    1.00    --   40.37 -57.00-120.00   30
  2  ω     36.00  72.00   1.00    1.00    --   40.37-125.00 -90.00   36
  3  ω      2.00  80.00   1.00    1.00    --   40.37 -99.00   0.00   78
  4  ω     34.00 116.00   1.00   10.00    --  105.19-111.00   0.00   82
  5  ω     46.00 131.00   1.00   10.00    --  105.19 -45.00 150.00   85
  6  ω     91.00 177.00   1.00   10.00    --  105.19  61.00 -60.00   86
  7  ω    145.00 176.00   1.00   10.00    --  105.19 111.00 -60.00   31
  8  ω    112.00 172.00   1.00   10.00    --  105.19  45.00-180.00   60
  9  ω     39.00 109.00   1.00   10.00    --  105.19 -45.00   0.00   70
 10  ω      8.00 117.00   1.00    1.00    --   40.37  77.00 120.00  109
;
_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      0.0569647000
_diffrn_orient_matrix_UB_12      0.0580094000
_diffrn_orient_matrix_UB_13      0.0505942000
_diffrn_orient_matrix_UB_21      0.0040597000
_diffrn_orient_matrix_UB_22      0.0433486000
_diffrn_orient_matrix_UB_23      -0.0696805000
_diffrn_orient_matrix_UB_31      -0.0634252000
_diffrn_orient_matrix_UB_32      0.0546792000
_diffrn_orient_matrix_UB_33      0.0016632000
_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                4888
_reflns_number_total             5674
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5674
_refine_ls_number_restraints     176
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0794
_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)+(0.1517P)²+3.6060P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2289
_refine_ls_wR_factor_ref         0.2406
_refine_special_details          
;
 Significant disorder was identified in the region of the TBA ion.  
 The ion was modelled over 2 distinct positions with relative occupancies 
 refined to c.a. 0.6 and 0.4.  The model required significant use of 
 restraints and constraints as detailed in the _olex2_refinement_description
 section.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N4-C13A \\sim N4-C13B \\sim N4-C17B \\sim N4-C17A \\sim N4-C9B \\sim N4-C9A
\\sim N4-C21B \\sim N4-C21A
 with sigma of 0.02
 C9A-C10A \\sim C10B-C9B \\sim C11B-C10B \\sim C11A-C10A \\sim C22B-C21B \\sim
C21A-C22A \\sim C23A-
 C22A \\sim C22B-C23B \\sim C13A-C14A \\sim C14B-C15B \\sim C15A-C14A \\sim
C14B-C13B \\sim C18B-C17B ~
 C17A-C18A \\sim C19A-C18A \\sim C19B-C18B
 with sigma of 0.02
 C19B-C20B \\sim C20A-C19A \\sim C11B-C12B \\sim C11A-C12A \\sim C15A-C16A
\\sim C16B-C15B \\sim C24B-
 C23B \\sim C23A-C24A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C17A) = Uanis(C17B)
Uanis(C21A) = Uanis(C21B)
Uanis(C9A) = Uanis(C9B)
Uanis(C13A) = Uanis(C13B)
Uanis(C10A) = Uanis(C10B)
Uanis(C18A) = Uanis(C18B)
Uanis(C14A) = Uanis(C14B)
Uanis(C22A) = Uanis(C22B)
Uanis(C23A) = Uanis(C23B)
Uanis(C19A) = Uanis(C19B)
Uanis(C11A) = Uanis(C11B)
Uanis(C15A) = Uanis(C15B)
Uanis(C12A) = Uanis(C12B)
Uanis(C16A) = Uanis(C16B)
Uanis(C20A) = Uanis(C20B)
Uanis(C24A) = Uanis(C24B)
4. Others
 Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C21B)=Sof(H21C)=Sof(H21D)=Sof(C9B)=
 Sof(H9BA)=Sof(H9BB)=Sof(C13B)=Sof(H13C)=Sof(H13D)=Sof(C10B)=Sof(H10C)=
 Sof(H10D)=Sof(C18B)=Sof(H18C)=Sof(H18D)=Sof(C14B)=Sof(H14C)=Sof(H14D)=
 Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(C19B)=
 Sof(H19C)=Sof(H19D)=Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C15B)=Sof(H15C)=
 Sof(H15D)=Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C16B)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=Sof(C20B)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C24B)=
 Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=
 Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C22A)=Sof(H22A)=Sof(H22B)=
 Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(C20A)=
 Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C24A)=
 Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(C23A)=
 Sof(H23A)=Sof(H23B)=FVAR(1)
 Fixed Sof: H7A(0.5) H7B(0.5)
5.a Free rotating group:
 O7(H7A,H7B)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C14A(H14A,H14B), C10A(H10A,H10B), C18A(H18A,H18B), C13A(H13A,
 H13B), C9A(H9AA,H9AB), C22A(H22A,H22B), C17A(H17A,H17B), C21A(H21A,H21B),
 C19A(H19A,H19B), C11A(H11A,H11B), C15A(H15A,H15B), C23A(H23A,H23B), C17B(H17C,
 H17D), C21B(H21C,H21D), C9B(H9BA,H9BB), C13B(H13C,H13D), C10B(H10C,H10D),
 C18B(H18C,H18D), C14B(H14C,H14D), C22B(H22C,H22D), C23B(H23C,H23D), C19B(H19C,
 H19D), C11B(H11C,H11D), C15B(H15C,H15D)
5.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N2(H2), C5(H5), C2(H2A), C6(H6), C3(H3A)
5.d Idealised Me refined as rotating group:
 C16A(H16A,H16B,H16C), C12A(H12A,H12B,H12C), C20A(H20A,H20B,H20C), C24A(H24A,
 H24B,H24C), C12B(H12D,H12E,H12F), C16B(H16D,H16E,H16F), C20B(H20D,H20E,H20F),
 C24B(H24D,H24E,H24F)
;
_atom_sites_solution_hydrogens   mixed
_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 0.44268(4) 0.08259(4) 0.60479(3) 0.0625(3) Uani 1 1 d . . . . .
O3 O 0.34731(9) 0.24897(13) 0.66788(12) 0.0719(6) Uani 1 1 d . . . . .
O4 O 0.46340(11) 0.16263(13) 0.59260(10) 0.0698(5) Uani 1 1 d . . . . .
O6 O 0.50514(10) 0.04100(12) 0.65753(10) 0.0653(5) Uani 1 1 d . . . . .
N3 N 0.40350(10) 0.13494(14) 0.71963(12) 0.0599(5) Uani 1 1 d . . . . .
H3 H 0.4285 0.1111 0.7603 0.072 Uiso 1 1 calc R . . . .
N4 N 0.35347(10) 0.15326(13) 0.34771(11) 0.0553(5) Uani 1 1 d D . . . .
O5 O 0.40538(15) 0.03869(14) 0.53801(12) 0.0865(7) Uani 1 1 d . . . . .
N2 N 0.43049(11) 0.24896(15) 0.78756(13) 0.0645(6) Uani 1 1 d . . . . .
H2 H 0.4541 0.2185 0.8239 0.077 Uiso 1 1 calc R . . . .
O2 O 0.43608(17) 0.61882(17) 0.80890(18) 0.1016(8) Uani 1 1 d . . . . .
C8 C 0.37564(13) 0.09131(17) 0.65105(16) 0.0639(7) Uani 1 1 d . . . . .
H8A H 0.3318 0.1174 0.6180 0.077 Uiso 1 1 calc R . . . .
H8B H 0.3613 0.0390 0.6616 0.077 Uiso 1 1 calc R . . . .
O1 O 0.49817(17) 0.58872(18) 0.92368(17) 0.1053(9) Uani 1 1 d . . . . .
N1 N 0.46379(16) 0.5699(2) 0.85867(19) 0.0896(9) Uani 1 1 d . . . . .
C7 C 0.39073(12) 0.21263(18) 0.72059(15) 0.0607(6) Uani 1 1 d . . . . .
C5 C 0.40857(13) 0.38680(19) 0.74721(16) 0.0653(7) Uani 1 1 d . . . . .
H5 H 0.3839 0.3723 0.6978 0.078 Uiso 1 1 calc R . . . .
C4 C 0.43602(12) 0.32870(19) 0.80184(15) 0.0645(7) Uani 1 1 d . . . . .
C2 C 0.48164(18) 0.4308(2) 0.89516(19) 0.0822(10) Uani 1 1 d . . . . .
H2A H 0.5059 0.4460 0.9444 0.099 Uiso 1 1 calc R . . . .
O7 O 0.5000 -0.0793(2) 0.7500 0.0962(11) Uani 1 2 d S T P . .
H7A H 0.5020 -0.0452 0.7180 0.144 Uiso 0.5 1 d G . . . .
H7B H 0.4884 -0.0569 0.7844 0.144 Uiso 0.5 1 d G . . . .
C6 C 0.41791(14) 0.4650(2) 0.76626(18) 0.0699(7) Uani 1 1 d . . . . .
H6 H 0.4000 0.5034 0.7297 0.084 Uiso 1 1 calc R . . . .
C1 C 0.45396(15) 0.4868(2) 0.83983(19) 0.0757(8) Uani 1 1 d . . . . .
C3 C 0.47282(16) 0.3526(2) 0.87652(17) 0.0750(8) Uani 1 1 d . . . . .
H3A H 0.4913 0.3146 0.9134 0.090 Uiso 1 1 calc R . . . .
C14A C 0.2868(4) 0.0244(4) 0.3599(6) 0.0733(18) Uani 0.6287(18) 1 d D . . A 1
H14A H 0.2718 0.0442 0.4004 0.088 Uiso 0.6287(18) 1 calc R . . A 1
H14B H 0.2475 0.0353 0.3131 0.088 Uiso 0.6287(18) 1 calc R . . A 1
C10A C 0.3397(3) 0.2829(3) 0.4107(3) 0.0613(10) Uani 0.6287(18) 1 d D . . A 1
H10A H 0.3072 0.3043 0.3638 0.074 Uiso 0.6287(18) 1 calc R . . A 1
H10B H 0.3901 0.2986 0.4169 0.074 Uiso 0.6287(18) 1 calc R . . A 1
C18A C 0.2916(3) 0.1216(3) 0.2068(3) 0.0674(11) Uani 0.6287(18) 1 d D . . A 1
H18A H 0.3394 0.1241 0.2000 0.081 Uiso 0.6287(18) 1 calc R . . A 1
H18B H 0.2824 0.0673 0.2168 0.081 Uiso 0.6287(18) 1 calc R . . A 1
C13A C 0.3581(2) 0.0651(3) 0.3609(2) 0.0606(8) Uani 0.6287(18) 1 d D . . A 1
H13A H 0.3960 0.0551 0.4089 0.073 Uiso 0.6287(18) 1 calc R . . A 1
H13B H 0.3745 0.0408 0.3230 0.073 Uiso 0.6287(18) 1 calc R . . A 1
C9A C 0.3342(2) 0.1938(2) 0.4089(2) 0.0562(7) Uani 0.6287(18) 1 d D . . A 1
H9AA H 0.3666 0.1737 0.4564 0.067 Uiso 0.6287(18) 1 calc R . . A 1
H9AB H 0.2839 0.1794 0.4043 0.067 Uiso 0.6287(18) 1 calc R . . A 1
C16A C 0.2350(9) -0.1125(8) 0.3641(13) 0.105(4) Uani 0.6287(18) 1 d D . . A 1
H16A H 0.2017 -0.1138 0.3133 0.158 Uiso 0.6287(18) 1 calc GR . . A 1
H16B H 0.2101 -0.0901 0.3955 0.158 Uiso 0.6287(18) 1 calc GR . . A 1
H16C H 0.2506 -0.1652 0.3804 0.158 Uiso 0.6287(18) 1 calc GR . . A 1
C22A C 0.4923(3) 0.1715(5) 0.4150(4) 0.0672(15) Uani 0.6287(18) 1 d D . . A 1
H22A H 0.5007 0.1157 0.4257 0.081 Uiso 0.6287(18) 1 calc R . . A 1
H22B H 0.4817 0.1959 0.4562 0.081 Uiso 0.6287(18) 1 calc R . . A 1
C17A C 0.2927(2) 0.1729(3) 0.2726(2) 0.0594(8) Uani 0.6287(18) 1 d D . . A 1
H17A H 0.2449 0.1687 0.2791 0.071 Uiso 0.6287(18) 1 calc R . . A 1
H17B H 0.2988 0.2274 0.2602 0.071 Uiso 0.6287(18) 1 calc R . . A 1
C12A C 0.3251(3) 0.4059(4) 0.4793(5) 0.090(2) Uani 0.6287(18) 1 d D . . A 1
H12A H 0.3154 0.4245 0.5227 0.135 Uiso 0.6287(18) 1 calc GR . . A 1
H12B H 0.2901 0.4289 0.4354 0.135 Uiso 0.6287(18) 1 calc GR . . A 1
H12C H 0.3744 0.4207 0.4826 0.135 Uiso 0.6287(18) 1 calc GR . . A 1
C21A C 0.4268(2) 0.1826(3) 0.3431(2) 0.0626(8) Uani 0.6287(18) 1 d D . . A 1
H21A H 0.4369 0.1550 0.3030 0.075 Uiso 0.6287(18) 1 calc R . . A 1
H21B H 0.4221 0.2382 0.3305 0.075 Uiso 0.6287(18) 1 calc R . . A 1
C19A C 0.2317(3) 0.1493(4) 0.1363(3) 0.0861(14) Uani 0.6287(18) 1 d D . . A 1
H19A H 0.1861 0.1568 0.1467 0.103 Uiso 0.6287(18) 1 calc R . . A 1
H19B H 0.2460 0.1999 0.1216 0.103 Uiso 0.6287(18) 1 calc R . . A 1
C20A C 0.2180(4) 0.0929(5) 0.0729(4) 0.1006(19) Uani 0.6287(18) 1 d D . . A 1
H20A H 0.1823 0.1149 0.0289 0.151 Uiso 0.6287(18) 1 calc GR . . A 1
H20B H 0.1993 0.0442 0.0852 0.151 Uiso 0.6287(18) 1 calc GR . . A 1
H20C H 0.2635 0.0832 0.0638 0.151 Uiso 0.6287(18) 1 calc GR . . A 1
C11A C 0.3178(2) 0.3159(3) 0.4750(3) 0.0688(10) Uani 0.6287(18) 1 d D . . A 1
H11A H 0.3494 0.2931 0.5217 0.083 Uiso 0.6287(18) 1 calc R . . A 1
H11B H 0.2671 0.3013 0.4680 0.083 Uiso 0.6287(18) 1 calc R . . A 1
C24A C 0.6266(3) 0.2050(7) 0.4775(4) 0.116(3) Uani 0.6287(18) 1 d D . . A 1
H24A H 0.6681 0.2318 0.4711 0.174 Uiso 0.6287(18) 1 calc GR . . A 1
H24B H 0.6395 0.1508 0.4902 0.174 Uiso 0.6287(18) 1 calc GR . . A 1
H24C H 0.6140 0.2297 0.5169 0.174 Uiso 0.6287(18) 1 calc GR . . A 1
C15A C 0.3007(4) -0.0637(3) 0.3687(4) 0.0868(15) Uani 0.6287(18) 1 d D . . A 1
H15A H 0.3199 -0.0812 0.3303 0.104 Uiso 0.6287(18) 1 calc R . . A 1
H15B H 0.3388 -0.0733 0.4166 0.104 Uiso 0.6287(18) 1 calc R . . A 1
C23A C 0.5620(3) 0.2089(4) 0.4066(3) 0.0876(14) Uani 0.6287(18) 1 d D . . A 1
H23A H 0.5743 0.1818 0.3675 0.105 Uiso 0.6287(18) 1 calc R . . A 1
H23B H 0.5518 0.2636 0.3918 0.105 Uiso 0.6287(18) 1 calc R . . A 1
C17B C 0.3487(3) 0.1415(5) 0.2684(3) 0.0594(8) Uani 0.3713(18) 1 d D . . A 2
H17C H 0.3680 0.0896 0.2639 0.071 Uiso 0.3713(18) 1 calc R . . A 2
H17D H 0.3804 0.1799 0.2565 0.071 Uiso 0.3713(18) 1 calc R . . A 2
C21B C 0.4345(3) 0.1360(5) 0.3997(4) 0.0626(8) Uani 0.3713(18) 1 d D . . A 2
H21C H 0.4352 0.1341 0.4509 0.075 Uiso 0.3713(18) 1 calc R . . A 2
H21D H 0.4484 0.0841 0.3876 0.075 Uiso 0.3713(18) 1 calc R . . A 2
C9B C 0.3336(3) 0.2377(4) 0.3590(4) 0.0562(7) Uani 0.3713(18) 1 d D . . A 2
H9BA H 0.3678 0.2721 0.3460 0.067 Uiso 0.3713(18) 1 calc R . . A 2
H9BB H 0.2844 0.2482 0.3238 0.067 Uiso 0.3713(18) 1 calc R . . A 2
C13B C 0.3037(4) 0.0981(4) 0.3714(4) 0.0606(8) Uani 0.3713(18) 1 d D . . A 2
H13C H 0.3160 0.1026 0.4250 0.073 Uiso 0.3713(18) 1 calc R . . A 2
H13D H 0.2529 0.1159 0.3484 0.073 Uiso 0.3713(18) 1 calc R . . A 2
C10B C 0.3344(5) 0.2599(5) 0.4354(5) 0.0613(10) Uani 0.3713(18) 1 d D . . A 2
H10C H 0.3783 0.2382 0.4725 0.074 Uiso 0.3713(18) 1 calc R . . A 2
H10D H 0.2914 0.2373 0.4437 0.074 Uiso 0.3713(18) 1 calc R . . A 2
C18B C 0.2715(5) 0.1485(7) 0.2113(5) 0.0674(11) Uani 0.3713(18) 1 d D . . A 2
H18C H 0.2384 0.1137 0.2254 0.081 Uiso 0.3713(18) 1 calc R . . A 2
H18D H 0.2540 0.2021 0.2117 0.081 Uiso 0.3713(18) 1 calc R . . A 2
C14B C 0.3071(9) 0.0132(7) 0.3527(11) 0.0733(18) Uani 0.3713(18) 1 d D . . A 2
H14C H 0.3583 -0.0040 0.3719 0.088 Uiso 0.3713(18) 1 calc R . . A 2
H14D H 0.2899 0.0075 0.2989 0.088 Uiso 0.3713(18) 1 calc R . . A 2
C22B C 0.4918(6) 0.1933(8) 0.3958(8) 0.0672(15) Uani 0.3713(18) 1 d D . . A 2
H22C H 0.4796 0.2451 0.4097 0.081 Uiso 0.3713(18) 1 calc R . . A 2
H22D H 0.4914 0.1961 0.3448 0.081 Uiso 0.3713(18) 1 calc R . . A 2
C23B C 0.5687(4) 0.1708(7) 0.4467(6) 0.0876(14) Uani 0.3713(18) 1 d D . . A 2
H23C H 0.5707 0.1725 0.4983 0.105 Uiso 0.3713(18) 1 calc R . . A 2
H23D H 0.5800 0.1175 0.4356 0.105 Uiso 0.3713(18) 1 calc R . . A 2
C19B C 0.2689(5) 0.1281(7) 0.1334(4) 0.0861(14) Uani 0.3713(18) 1 d D . . A 2
H19C H 0.3014 0.1643 0.1198 0.103 Uiso 0.3713(18) 1 calc R . . A 2
H19D H 0.2895 0.0756 0.1348 0.103 Uiso 0.3713(18) 1 calc R . . A 2
C11B C 0.3337(4) 0.3479(5) 0.4451(5) 0.0688(10) Uani 0.3713(18) 1 d D . . A 2
H11C H 0.3813 0.3687 0.4465 0.083 Uiso 0.3713(18) 1 calc R . . A 2
H11D H 0.2962 0.3702 0.4016 0.083 Uiso 0.3713(18) 1 calc R . . A 2
C15B C 0.2619(6) -0.0394(6) 0.3836(6) 0.0868(15) Uani 0.3713(18) 1 d D . . A 2
H15C H 0.2856 -0.0431 0.4374 0.104 Uiso 0.3713(18) 1 calc R . . A 2
H15D H 0.2133 -0.0162 0.3737 0.104 Uiso 0.3713(18) 1 calc R . . A 2
C12B C 0.3192(6) 0.3751(7) 0.5127(7) 0.090(2) Uani 0.3713(18) 1 d D . . A 2
H12D H 0.3250 0.4313 0.5170 0.135 Uiso 0.3713(18) 1 calc GR . . A 2
H12E H 0.3536 0.3505 0.5561 0.135 Uiso 0.3713(18) 1 calc GR . . A 2
H12F H 0.2695 0.3612 0.5089 0.135 Uiso 0.3713(18) 1 calc GR . . A 2
C16B C 0.2532(19) -0.1200(14) 0.351(2) 0.105(4) Uani 0.3713(18) 1 d D . . A 2
H16D H 0.2512 -0.1169 0.2999 0.158 Uiso 0.3713(18) 1 calc GR . . A 2
H16E H 0.2082 -0.1431 0.3529 0.158 Uiso 0.3713(18) 1 calc GR . . A 2
H16F H 0.2946 -0.1520 0.3789 0.158 Uiso 0.3713(18) 1 calc GR . . A 2
C20B C 0.1962(7) 0.1296(10) 0.0734(7) 0.1006(19) Uani 0.3713(18) 1 d D . . A 2
H20D H 0.2007 0.1075 0.0288 0.151 Uiso 0.3713(18) 1 calc GR . . A 2
H20E H 0.1791 0.1830 0.0641 0.151 Uiso 0.3713(18) 1 calc GR . . A 2
H20F H 0.1613 0.0992 0.0884 0.151 Uiso 0.3713(18) 1 calc GR . . A 2
C24B C 0.6238(6) 0.2259(10) 0.4360(8) 0.116(3) Uani 0.3713(18) 1 d D . . A 2
H24D H 0.6075 0.2437 0.3851 0.174 Uiso 0.3713(18) 1 calc GR . . A 2
H24E H 0.6706 0.1995 0.4473 0.174 Uiso 0.3713(18) 1 calc GR . . A 2
H24F H 0.6293 0.2704 0.4687 0.174 Uiso 0.3713(18) 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
S1 O4 1.456(2) . ?
S1 O6 1.458(2) . ?
S1 O5 1.437(2) . ?
S1 C8 1.795(3) . ?
O3 C7 1.230(3) . ?
N3 H3 0.8600 . ?
N3 C8 1.437(4) . ?
N3 C7 1.342(4) . ?
N4 C13A 1.514(5) . ?
N4 C9A 1.503(4) . ?
N4 C17A 1.544(4) . ?
N4 C21A 1.523(4) . ?
N4 C17B 1.494(7) . ?
N4 C21B 1.562(6) . ?
N4 C9B 1.515(6) . ?
N4 C13B 1.512(7) . ?
N2 H2 0.8600 . ?
N2 C7 1.388(3) . ?
N2 C4 1.377(4) . ?
O2 N1 1.236(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
O1 N1 1.231(4) . ?
N1 C1 1.451(5) . ?
C5 H5 0.9300 . ?
C5 C4 1.399(4) . ?
C5 C6 1.371(5) . ?
C4 C3 1.415(4) . ?
C2 H2A 0.9300 . ?
C2 C1 1.384(5) . ?
C2 C3 1.369(5) . ?
O7 H7A 0.8504 . ?
O7 H7B 0.8499 . ?
C6 H6 0.9300 . ?
C6 C1 1.385(4) . ?
C3 H3A 0.9300 . ?
C14A H14A 0.9700 . ?
C14A H14B 0.9700 . ?
C14A C13A 1.526(7) . ?
C14A C15A 1.518(8) . ?
C10A H10A 0.9700 . ?
C10A H10B 0.9700 . ?
C10A C9A 1.514(6) . ?
C10A C11A 1.527(6) . ?
C18A H18A 0.9700 . ?
C18A H18B 0.9700 . ?
C18A C17A 1.519(6) . ?
C18A C19A 1.515(6) . ?
C13A H13A 0.9700 . ?
C13A H13B 0.9700 . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C16A H16A 0.9600 . ?
C16A H16B 0.9600 . ?
C16A H16C 0.9600 . ?
C16A C15A 1.487(10) . ?
C22A H22A 0.9700 . ?
C22A H22B 0.9700 . ?
C22A C21A 1.523(7) . ?
C22A C23A 1.536(7) . ?
C17A H17A 0.9700 . ?
C17A H17B 0.9700 . ?
C12A H12A 0.9600 . ?
C12A H12B 0.9600 . ?
C12A H12C 0.9600 . ?
C12A C11A 1.533(7) . ?
C21A H21A 0.9700 . ?
C21A H21B 0.9700 . ?
C19A H19A 0.9700 . ?
C19A H19B 0.9700 . ?
C19A C20A 1.492(8) . ?
C20A H20A 0.9600 . ?
C20A H20B 0.9600 . ?
C20A H20C 0.9600 . ?
C11A H11A 0.9700 . ?
C11A H11B 0.9700 . ?
C24A H24A 0.9600 . ?
C24A H24B 0.9600 . ?
C24A H24C 0.9600 . ?
C24A C23A 1.492(7) . ?
C15A H15A 0.9700 . ?
C15A H15B 0.9700 . ?
C23A H23A 0.9700 . ?
C23A H23B 0.9700 . ?
C17B H17C 0.9700 . ?
C17B H17D 0.9700 . ?
C17B C18B 1.514(9) . ?
C21B H21C 0.9700 . ?
C21B H21D 0.9700 . ?
C21B C22B 1.488(11) . ?
C9B H9BA 0.9700 . ?
C9B H9BB 0.9700 . ?
C9B C10B 1.498(9) . ?
C13B H13C 0.9700 . ?
C13B H13D 0.9700 . ?
C13B C14B 1.490(12) . ?
C10B H10C 0.9700 . ?
C10B H10D 0.9700 . ?
C10B C11B 1.505(10) . ?
C18B H18C 0.9700 . ?
C18B H18D 0.9700 . ?
C18B C19B 1.507(10) . ?
C14B H14C 0.9700 . ?
C14B H14D 0.9700 . ?
C14B C15B 1.496(12) . ?
C22B H22C 0.9700 . ?
C22B H22D 0.9700 . ?
C22B C23B 1.512(11) . ?
C23B H23C 0.9700 . ?
C23B H23D 0.9700 . ?
C23B C24B 1.477(12) . ?
C19B H19C 0.9700 . ?
C19B H19D 0.9700 . ?
C19B C20B 1.473(11) . ?
C11B H11C 0.9700 . ?
C11B H11D 0.9700 . ?
C11B C12B 1.481(11) . ?
C15B H15C 0.9700 . ?
C15B H15D 0.9700 . ?
C15B C16B 1.489(14) . ?
C12B H12D 0.9600 . ?
C12B H12E 0.9600 . ?
C12B H12F 0.9600 . ?
C16B H16D 0.9600 . ?
C16B H16E 0.9600 . ?
C16B H16F 0.9600 . ?
C20B H20D 0.9600 . ?
C20B H20E 0.9600 . ?
C20B H20F 0.9600 . ?
C24B H24D 0.9600 . ?
C24B H24E 0.9600 . ?
C24B H24F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 S1 O6 110.87(12) . . ?
O4 S1 C8 106.33(13) . . ?
O6 S1 C8 105.10(12) . . ?
O5 S1 O4 115.07(13) . . ?
O5 S1 O6 113.85(14) . . ?
O5 S1 C8 104.60(15) . . ?
C8 N3 H3 119.8 . . ?
C7 N3 H3 119.8 . . ?
C7 N3 C8 120.3(2) . . ?
C13A N4 C17A 110.5(3) . . ?
C13A N4 C21A 109.2(3) . . ?
C9A N4 C13A 109.9(3) . . ?
C9A N4 C17A 108.2(2) . . ?
C9A N4 C21A 111.7(3) . . ?
C21A N4 C17A 107.3(2) . . ?
C17B N4 C21B 108.8(4) . . ?
C17B N4 C9B 109.7(4) . . ?
C17B N4 C13B 112.9(4) . . ?
C9B N4 C21B 109.4(4) . . ?
C13B N4 C21B 106.8(4) . . ?
C13B N4 C9B 109.1(4) . . ?
C7 N2 H2 116.6 . . ?
C4 N2 H2 116.6 . . ?
C4 N2 C7 126.8(2) . . ?
S1 C8 H8A 109.1 . . ?
S1 C8 H8B 109.1 . . ?
N3 C8 S1 112.39(17) . . ?
N3 C8 H8A 109.1 . . ?
N3 C8 H8B 109.1 . . ?
H8A C8 H8B 107.9 . . ?
O2 N1 C1 118.5(3) . . ?
O1 N1 O2 122.7(3) . . ?
O1 N1 C1 118.8(4) . . ?
O3 C7 N3 123.9(2) . . ?
O3 C7 N2 122.4(3) . . ?
N3 C7 N2 113.7(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C6 C5 C4 120.2(3) . . ?
N2 C4 C5 124.1(2) . . ?
N2 C4 C3 117.3(3) . . ?
C5 C4 C3 118.6(3) . . ?
C1 C2 H2A 120.4 . . ?
C3 C2 H2A 120.4 . . ?
C3 C2 C1 119.1(3) . . ?
H7A O7 H7B 109.4 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C1 120.1(3) . . ?
C1 C6 H6 120.0 . . ?
C2 C1 N1 119.7(3) . . ?
C2 C1 C6 121.1(3) . . ?
C6 C1 N1 119.2(3) . . ?
C4 C3 H3A 119.5 . . ?
C2 C3 C4 120.9(3) . . ?
C2 C3 H3A 119.5 . . ?
H14A C14A H14B 108.3 . . ?
C13A C14A H14A 109.9 . . ?
C13A C14A H14B 109.9 . . ?
C15A C14A H14A 109.9 . . ?
C15A C14A H14B 109.9 . . ?
C15A C14A C13A 108.7(5) . . ?
H10A C10A H10B 108.1 . . ?
C9A C10A H10A 109.6 . . ?
C9A C10A H10B 109.6 . . ?
C9A C10A C11A 110.4(4) . . ?
C11A C10A H10A 109.6 . . ?
C11A C10A H10B 109.6 . . ?
H18A C18A H18B 108.1 . . ?
C17A C18A H18A 109.6 . . ?
C17A C18A H18B 109.6 . . ?
C19A C18A H18A 109.6 . . ?
C19A C18A H18B 109.6 . . ?
C19A C18A C17A 110.3(4) . . ?
N4 C13A C14A 116.2(4) . . ?
N4 C13A H13A 108.2 . . ?
N4 C13A H13B 108.2 . . ?
C14A C13A H13A 108.2 . . ?
C14A C13A H13B 108.2 . . ?
H13A C13A H13B 107.4 . . ?
N4 C9A C10A 116.2(3) . . ?
N4 C9A H9AA 108.2 . . ?
N4 C9A H9AB 108.2 . . ?
C10A C9A H9AA 108.2 . . ?
C10A C9A H9AB 108.2 . . ?
H9AA C9A H9AB 107.4 . . ?
H16A C16A H16B 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
C15A C16A H16A 109.5 . . ?
C15A C16A H16B 109.5 . . ?
C15A C16A H16C 109.5 . . ?
H22A C22A H22B 108.2 . . ?
C21A C22A H22A 109.7 . . ?
C21A C22A H22B 109.7 . . ?
C21A C22A C23A 109.8(4) . . ?
C23A C22A H22A 109.7 . . ?
C23A C22A H22B 109.7 . . ?
N4 C17A H17A 108.3 . . ?
N4 C17A H17B 108.3 . . ?
C18A C17A N4 115.8(3) . . ?
C18A C17A H17A 108.3 . . ?
C18A C17A H17B 108.3 . . ?
H17A C17A H17B 107.4 . . ?
H12A C12A H12B 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
C11A C12A H12A 109.5 . . ?
C11A C12A H12B 109.5 . . ?
C11A C12A H12C 109.5 . . ?
N4 C21A H21A 108.8 . . ?
N4 C21A H21B 108.8 . . ?
C22A C21A N4 113.9(4) . . ?
C22A C21A H21A 108.8 . . ?
C22A C21A H21B 108.8 . . ?
H21A C21A H21B 107.7 . . ?
C18A C19A H19A 109.0 . . ?
C18A C19A H19B 109.0 . . ?
H19A C19A H19B 107.8 . . ?
C20A C19A C18A 113.0(5) . . ?
C20A C19A H19A 109.0 . . ?
C20A C19A H19B 109.0 . . ?
C19A C20A H20A 109.5 . . ?
C19A C20A H20B 109.5 . . ?
C19A C20A H20C 109.5 . . ?
H20A C20A H20B 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
C10A C11A C12A 111.3(5) . . ?
C10A C11A H11A 109.4 . . ?
C10A C11A H11B 109.4 . . ?
C12A C11A H11A 109.4 . . ?
C12A C11A H11B 109.4 . . ?
H11A C11A H11B 108.0 . . ?
H24A C24A H24B 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C23A C24A H24A 109.5 . . ?
C23A C24A H24B 109.5 . . ?
C23A C24A H24C 109.5 . . ?
C14A C15A H15A 108.4 . . ?
C14A C15A H15B 108.4 . . ?
C16A C15A C14A 115.4(9) . . ?
C16A C15A H15A 108.4 . . ?
C16A C15A H15B 108.4 . . ?
H15A C15A H15B 107.5 . . ?
C22A C23A H23A 109.2 . . ?
C22A C23A H23B 109.2 . . ?
C24A C23A C22A 111.9(6) . . ?
C24A C23A H23A 109.2 . . ?
C24A C23A H23B 109.2 . . ?
H23A C23A H23B 107.9 . . ?
N4 C17B H17C 108.5 . . ?
N4 C17B H17D 108.5 . . ?
N4 C17B C18B 115.1(5) . . ?
H17C C17B H17D 107.5 . . ?
C18B C17B H17C 108.5 . . ?
C18B C17B H17D 108.5 . . ?
N4 C21B H21C 108.3 . . ?
N4 C21B H21D 108.3 . . ?
H21C C21B H21D 107.4 . . ?
C22B C21B N4 116.0(6) . . ?
C22B C21B H21C 108.3 . . ?
C22B C21B H21D 108.3 . . ?
N4 C9B H9BA 108.0 . . ?
N4 C9B H9BB 108.0 . . ?
H9BA C9B H9BB 107.3 . . ?
C10B C9B N4 117.1(5) . . ?
C10B C9B H9BA 108.0 . . ?
C10B C9B H9BB 108.0 . . ?
N4 C13B H13C 108.2 . . ?
N4 C13B H13D 108.2 . . ?
H13C C13B H13D 107.3 . . ?
C14B C13B N4 116.4(7) . . ?
C14B C13B H13C 108.2 . . ?
C14B C13B H13D 108.2 . . ?
C9B C10B H10C 109.3 . . ?
C9B C10B H10D 109.3 . . ?
C9B C10B C11B 111.8(7) . . ?
H10C C10B H10D 107.9 . . ?
C11B C10B H10C 109.3 . . ?
C11B C10B H10D 109.3 . . ?
C17B C18B H18C 109.1 . . ?
C17B C18B H18D 109.1 . . ?
H18C C18B H18D 107.8 . . ?
C19B C18B C17B 112.7(7) . . ?
C19B C18B H18C 109.1 . . ?
C19B C18B H18D 109.1 . . ?
C13B C14B H14C 108.8 . . ?
C13B C14B H14D 108.8 . . ?
C13B C14B C15B 113.9(10) . . ?
H14C C14B H14D 107.7 . . ?
C15B C14B H14C 108.8 . . ?
C15B C14B H14D 108.8 . . ?
C21B C22B H22C 109.1 . . ?
C21B C22B H22D 109.1 . . ?
C21B C22B C23B 112.3(8) . . ?
H22C C22B H22D 107.9 . . ?
C23B C22B H22C 109.1 . . ?
C23B C22B H22D 109.1 . . ?
C22B C23B H23C 109.7 . . ?
C22B C23B H23D 109.7 . . ?
H23C C23B H23D 108.2 . . ?
C24B C23B C22B 109.9(10) . . ?
C24B C23B H23C 109.7 . . ?
C24B C23B H23D 109.7 . . ?
C18B C19B H19C 107.9 . . ?
C18B C19B H19D 107.9 . . ?
H19C C19B H19D 107.2 . . ?
C20B C19B C18B 117.7(9) . . ?
C20B C19B H19C 107.9 . . ?
C20B C19B H19D 107.9 . . ?
C10B C11B H11C 108.5 . . ?
C10B C11B H11D 108.4 . . ?
H11C C11B H11D 107.5 . . ?
C12B C11B C10B 115.3(8) . . ?
C12B C11B H11C 108.4 . . ?
C12B C11B H11D 108.4 . . ?
C14B C15B H15C 109.1 . . ?
C14B C15B H15D 109.1 . . ?
H15C C15B H15D 107.9 . . ?
C16B C15B C14B 112.4(16) . . ?
C16B C15B H15C 109.1 . . ?
C16B C15B H15D 109.1 . . ?
C11B C12B H12D 109.5 . . ?
C11B C12B H12E 109.5 . . ?
C11B C12B H12F 109.5 . . ?
H12D C12B H12E 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C15B C16B H16D 109.5 . . ?
C15B C16B H16E 109.5 . . ?
C15B C16B H16F 109.5 . . ?
H16D C16B H16E 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?
C19B C20B H20D 109.5 . . ?
C19B C20B H20E 109.5 . . ?
C19B C20B H20F 109.5 . . ?
H20D C20B H20E 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?
C23B C24B H24D 109.5 . . ?
C23B C24B H24E 109.5 . . ?
C23B C24B H24F 109.5 . . ?
H24D C24B H24E 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B 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
O4 S1 C8 N3 -57.2(2) . . . . ?
O6 S1 C8 N3 60.4(2) . . . . ?
N4 C17B C18B C19B -174.2(8) . . . . ?
N4 C21B C22B C23B -178.7(9) . . . . ?
N4 C9B C10B C11B 165.0(6) . . . . ?
N4 C13B C14B C15B 174.7(10) . . . . ?
O5 S1 C8 N3 -179.4(2) . . . . ?
N2 C4 C3 C2 179.0(3) . . . . ?
O2 N1 C1 C2 -177.2(3) . . . . ?
O2 N1 C1 C6 3.8(5) . . . . ?
C8 N3 C7 O3 10.5(4) . . . . ?
C8 N3 C7 N2 -170.4(2) . . . . ?
O1 N1 C1 C2 1.5(5) . . . . ?
O1 N1 C1 C6 -177.4(3) . . . . ?
C7 N3 C8 S1 94.3(2) . . . . ?
C7 N2 C4 C5 -7.8(4) . . . . ?
C7 N2 C4 C3 173.1(2) . . . . ?
C5 C4 C3 C2 -0.1(4) . . . . ?
C5 C6 C1 N1 179.5(3) . . . . ?
C5 C6 C1 C2 0.5(4) . . . . ?
C4 N2 C7 O3 -9.6(4) . . . . ?
C4 N2 C7 N3 171.3(2) . . . . ?
C4 C5 C6 C1 -0.6(4) . . . . ?
C6 C5 C4 N2 -178.6(2) . . . . ?
C6 C5 C4 C3 0.4(4) . . . . ?
C1 C2 C3 C4 0.0(5) . . . . ?
C3 C2 C1 N1 -179.2(3) . . . . ?
C3 C2 C1 C6 -0.2(5) . . . . ?
C13A N4 C9A C10A 170.4(3) . . . . ?
C13A N4 C17A C18A -44.8(4) . . . . ?
C13A N4 C21A C22A -63.2(5) . . . . ?
C13A N4 C17B C18B 101.4(7) . . . . ?
C13A N4 C21B C22B 153.8(10) . . . . ?
C13A N4 C9B C10B 31.7(11) . . . . ?
C13A N4 C13B C14B -21.8(9) . . . . ?
C13A C14A C15A C16A -176.4(11) . . . . ?
C9A N4 C13A C14A 62.6(6) . . . . ?
C9A N4 C17A C18A -165.2(4) . . . . ?
C9A N4 C21A C22A 58.5(5) . . . . ?
C9A N4 C17B C18B -41.8(12) . . . . ?
C9A N4 C21B C22B -96.3(9) . . . . ?
C9A N4 C9B C10B 13.4(5) . . . . ?
C9A N4 C13B C14B -159.1(10) . . . . ?
C9A C10A C11A C12A 178.4(4) . . . . ?
C17A N4 C13A C14A -56.7(6) . . . . ?
C17A N4 C9A C10A -68.9(4) . . . . ?
C17A N4 C21A C22A 176.9(5) . . . . ?
C17A N4 C17B C18B -16.1(6) . . . . ?
C17A N4 C21B C22B 50.1(14) . . . . ?
C17A N4 C9B C10B 143.8(6) . . . . ?
C17A N4 C13B C14B 92.8(10) . . . . ?
C17A C18A C19A C20A -169.1(6) . . . . ?
C21A N4 C13A C14A -174.6(5) . . . . ?
C21A N4 C9A C10A 49.0(4) . . . . ?
C21A N4 C17A C18A 74.2(4) . . . . ?
C21A N4 C17B C18B -148.9(8) . . . . ?
C21A N4 C21B C22B 20.0(9) . . . . ?
C21A N4 C9B C10B -108.2(6) . . . . ?
C21A N4 C13B C14B -54.2(14) . . . . ?
C21A C22A C23A C24A 175.7(7) . . . . ?
C19A C18A C17A N4 -177.6(4) . . . . ?
C11A C10A C9A N4 179.4(3) . . . . ?
C15A C14A C13A N4 176.2(5) . . . . ?
C23A C22A C21A N4 -175.4(5) . . . . ?
C17B N4 C13A C14A -101.1(6) . . . . ?
C17B N4 C9A C10A -49.2(9) . . . . ?
C17B N4 C17A C18A 26.5(5) . . . . ?
C17B N4 C21A C22A -148.5(6) . . . . ?
C17B N4 C21B C22B 68.5(10) . . . . ?
C17B N4 C9B C10B 179.1(6) . . . . ?
C17B N4 C13B C14B 48.2(11) . . . . ?
C17B C18B C19B C20B 177.5(11) . . . . ?
C21B N4 C13A C14A 149.6(6) . . . . ?
C21B N4 C9A C10A 96.7(4) . . . . ?
C21B N4 C17A C18A 50.4(10) . . . . ?
C21B N4 C21A C22A -16.1(6) . . . . ?
C21B N4 C17B C18B 174.5(7) . . . . ?
C21B N4 C9B C10B -61.6(7) . . . . ?
C21B N4 C13B C14B -71.4(10) . . . . ?
C21B C22B C23B C24B 175.4(12) . . . . ?
C9B N4 C13A C14A 48.5(10) . . . . ?
C9B N4 C9A C10A -17.4(4) . . . . ?
C9B N4 C17A C18A 158.9(5) . . . . ?
C9B N4 C21A C22A 100.6(5) . . . . ?
C9B N4 C17B C18B -65.9(8) . . . . ?
C9B N4 C21B C22B -51.3(10) . . . . ?
C9B N4 C13B C14B 170.5(10) . . . . ?
C9B C10B C11B C12B 168.1(7) . . . . ?
C13B N4 C13A C14A 19.0(6) . . . . ?
C13B N4 C9A C10A -156.5(4) . . . . ?
C13B N4 C17A C18A -92.1(5) . . . . ?
C13B N4 C21A C22A -37.7(11) . . . . ?
C13B N4 C17B C18B 56.1(8) . . . . ?
C13B N4 C21B C22B -169.3(9) . . . . ?
C13B N4 C9B C10B 54.9(7) . . . . ?
C13B C14B C15B C16B 168(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.424
_oxdiff_exptl_absorpt_empirical_full_min 0.217
####################################################################### 
# 
# 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_compound_4
_database_code_depnum_ccdc_archive 'CCDC 1489607'
_audit_update_record             
;
2016-08-16 deposited with the CCDC.
2016-08-25 downloaded from the CCDC.
;
_audit_creation_date             2016-08-05
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2016.07.26 svn.r3321 for OlexSys, GUI svn.r5206)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C9 H8 F3 N2 O4 S, C16 H36 N, H O0.5'
_chemical_formula_sum            'C25 H45 F3 N3 O4.50 S'
_chemical_formula_weight         548.70
_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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.4863(8)
_cell_length_b                   16.9500(6)
_cell_length_c                   19.0704(5)
_cell_angle_alpha                90
_cell_angle_beta                 110.145(4)
_cell_angle_gamma                90
_cell_volume                     5913.5(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4100
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      72.4260
_cell_measurement_theta_min      3.5450
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.438
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2360
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 1 7 0.1034
-10 -5 9 0.0362
-7 -1 -7 0.1025
9 5 -9 0.0331
3 11 1 0.0510
-4 10 3 0.0461
-13 -1 4 0.0769
4 -10 -3 0.0204
6 1 8 0.1038
-8 -1 -7 0.1017
9 5 -9 0.0323

_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.067
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9536
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         3.555
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00 -13.00   1.00    5.00    --  -40.62 -77.00  90.00   52
  2  ω   -112.00 -82.00   1.00    5.00    --  -40.62 -77.00  90.00   30
  3  ω     41.00  87.00   1.00    5.00    --   40.62-125.00   0.00   46
  4  ω      0.00  98.00   1.00    5.00    --   40.62  19.00   0.00   98
  5  ω     80.00 172.00   1.00   20.00    --  105.19  61.00 150.00   92
  6  ω     33.00 131.00   1.00   20.00    --  105.19 -61.00   0.00   98
  7  ω     60.00 159.00   1.00   20.00    --  105.19  15.00 120.00   99
  8  ω     32.00 108.00   1.00   20.00    --  105.19 -45.00-150.00   76
;
_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                4441
_reflns_number_total             5202
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (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         0.504
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         5202
_refine_ls_number_restraints     351
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0602
_refine_ls_restrained_S_all      1.037
_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)+(0.0620P)²+10.9899P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1558
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
C21B \\sim C21A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(C14B)=Sof(H14C)=Sof(H14D)=Sof(C10B)=
 Sof(H10C)=Sof(H10D)=Sof(C18B)=Sof(H18C)=Sof(H18D)=Sof(C15B)=Sof(H15C)=
 Sof(H15D)=Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C19B)=Sof(H19C)=Sof(H19D)=
 Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(C12B)=Sof(H12C)=Sof(H12D)=Sof(C16B)=
 Sof(H16C)=Sof(H16D)=Sof(C20B)=Sof(H20C)=Sof(H20D)=Sof(C24B)=Sof(H24C)=
 Sof(H24D)=Sof(C13B)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C17B)=Sof(H17D)=
 Sof(H17E)=Sof(H17F)=Sof(C21B)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C25B)=
 Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(C11A)=
 Sof(H11A)=Sof(H11B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(C10A)=Sof(H10A)=
 Sof(H10B)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C13A)=Sof(H13A)=Sof(H13B)=
 Sof(H13C)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(C18A)=Sof(H18A)=Sof(H18B)=
 Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C24A)=Sof(H24A)=Sof(H24B)=
 Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(H21C)=
 Sof(C20A)=Sof(H20A)=Sof(H20B)=FVAR(1)
5.a Free rotating group:
 O5(H5)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C15A(H15A,H15B), C23A(H23A,H23B), C11A(H11A,H11B), C22A(H22A,
 H22B), C10A(H10A,H10B), C14A(H14A,H14B), C19A(H19A,H19B), C18A(H18A,H18B),
 C16A(H16A,H16B), C24A(H24A,H24B), C12A(H12A,H12B), C20A(H20A,H20B), C22B(H22C,
 H22D), C14B(H14C,H14D), C10B(H10C,H10D), C18B(H18C,H18D), C15B(H15C,H15D),
 C11B(H11C,H11D), C19B(H19C,H19D), C23B(H23C,H23D), C12B(H12C,H12D), C16B(H16C,
 H16D), C20B(H20C,H20D), C24B(H24C,H24D)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C6(H6), C7(H7), C4(H4), C3(H3)
5.d Idealised Me refined as rotating group:
 C13A(H13A,H13B,H13C), C17A(H17A,H17B,H17C), C25A(H25A,H25B,H25C), C21A(H21A,
 H21B,H21C), C13B(H13D,H13E,H13F), C17B(H17D,H17E,H17F), C21B(H21D,H21E,H21F),
 C25B(H25D,H25E,H25F)
;
_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 0.43328(4) 0.91366(4) 0.10600(3) 0.0520(2) Uani 1 1 d . U . . .
O3 O 0.49765(10) 0.95653(12) 0.15468(10) 0.0533(5) Uani 1 1 d . U . . .
N3 N 0.15271(10) 0.64284(12) 0.15520(10) 0.0351(4) Uani 1 1 d . U . . .
O1 O 0.34776(9) 0.74612(12) 0.17818(11) 0.0565(5) Uani 1 1 d . U . . .
O4 O 0.45316(11) 0.83410(12) 0.09121(10) 0.0558(5) Uani 1 1 d . U . . .
O5 O 0.0000 0.5803(2) 0.2500 0.0761(10) Uani 1 2 d S TU P . .
H5 H 0.0025 0.5475 0.2859 0.114 Uiso 1 1 d G . . . .
O2 O 0.39022(14) 0.95708(14) 0.04055(11) 0.0747(7) Uani 1 1 d . U . . .
N1 N 0.43596(11) 0.74579(15) 0.29496(12) 0.0493(5) Uani 1 1 d . U . . .
H1 H 0.4606 0.7773 0.3316 0.059 Uiso 1 1 calc R . . . .
F1 F 0.49785(14) 0.40051(15) 0.43279(14) 0.1037(8) Uani 1 1 d . U . . .
N2 N 0.40619(11) 0.85979(14) 0.22675(12) 0.0473(5) Uani 1 1 d . U . . .
H2 H 0.4345 0.8841 0.2671 0.057 Uiso 1 1 calc R . . . .
C6 C 0.41232(13) 0.60667(18) 0.25615(16) 0.0504(7) Uani 1 1 d . U . . .
H6 H 0.3818 0.6211 0.2072 0.060 Uiso 1 1 calc R . . . .
F3 F 0.44034(15) 0.37197(14) 0.31873(14) 0.1061(8) Uani 1 1 d . U . . .
C8 C 0.39381(13) 0.78128(17) 0.22969(15) 0.0466(6) Uani 1 1 d . U . . .
C5 C 0.44380(13) 0.66499(18) 0.30927(15) 0.0500(7) Uani 1 1 d . U . . .
C9 C 0.37417(14) 0.90346(18) 0.15964(17) 0.0543(7) Uani 1 1 d . U . . .
H9A H 0.3609 0.9566 0.1723 0.065 Uiso 1 1 calc R . . . .
H9B H 0.3286 0.8768 0.1287 0.065 Uiso 1 1 calc R . . . .
F2 F 0.55392(15) 0.40103(16) 0.3554(2) 0.1275(11) Uani 1 1 d . U . . .
C7 C 0.42551(14) 0.52841(19) 0.27467(19) 0.0583(7) Uani 1 1 d . U . . .
H7 H 0.4033 0.4893 0.2382 0.070 Uiso 1 1 calc R . . . .
C2 C 0.47055(16) 0.5051(2) 0.34549(19) 0.0662(9) Uani 1 1 d . U . . .
C15A C 0.0152(5) 0.6843(6) 0.0999(7) 0.047(2) Uani 0.550(3) 1 d . U . A 1
H15A H 0.0150 0.6911 0.1514 0.056 Uiso 0.550(3) 1 calc R . . A 1
H15B H 0.0269 0.7359 0.0825 0.056 Uiso 0.550(3) 1 calc R . . A 1
C4 C 0.48787(17) 0.6416(2) 0.38114(17) 0.0650(9) Uani 1 1 d . U . . .
H4 H 0.5086 0.6804 0.4184 0.078 Uiso 1 1 calc R . . . .
C23A C 0.2316(3) 0.6367(4) 0.2901(4) 0.0414(14) Uani 0.550(3) 1 d . U . A 1
H23A H 0.2649 0.5999 0.2775 0.050 Uiso 0.550(3) 1 calc R . . A 1
H23B H 0.2500 0.6910 0.2889 0.050 Uiso 0.550(3) 1 calc R . . A 1
C3 C 0.50143(19) 0.5628(2) 0.3985(2) 0.0763(10) Uani 1 1 d . U . . .
H3 H 0.5322 0.5480 0.4472 0.092 Uiso 1 1 calc R . . . .
C11A C 0.1718(3) 0.7505(4) 0.0672(3) 0.0405(13) Uani 0.550(3) 1 d . U . A 1
H11A H 0.1279 0.7285 0.0286 0.049 Uiso 0.550(3) 1 calc R . . A 1
H11B H 0.2154 0.7281 0.0591 0.049 Uiso 0.550(3) 1 calc R . . A 1
C22A C 0.1559(2) 0.6296(3) 0.2321(2) 0.0375(10) Uani 0.550(3) 1 d . U . A 1
H22A H 0.1368 0.5762 0.2355 0.045 Uiso 0.550(3) 1 calc R . . A 1
H22B H 0.1233 0.6681 0.2440 0.045 Uiso 0.550(3) 1 calc R . . A 1
C10A C 0.1720(2) 0.7271(3) 0.1431(2) 0.0343(10) Uani 0.550(3) 1 d . U . A 1
H10A H 0.1375 0.7622 0.1560 0.041 Uiso 0.550(3) 1 calc R . . A 1
H10B H 0.2214 0.7381 0.1794 0.041 Uiso 0.550(3) 1 calc R . . A 1
C14A C 0.0728(2) 0.6246(3) 0.1000(2) 0.0377(10) Uani 0.550(3) 1 d . U . A 1
H14A H 0.0742 0.6209 0.0487 0.045 Uiso 0.550(3) 1 calc R . . A 1
H14B H 0.0579 0.5724 0.1129 0.045 Uiso 0.550(3) 1 calc R . . A 1
C13A C 0.1878(3) 0.8677(4) -0.0078(3) 0.0511(14) Uani 0.550(3) 1 d . U . A 1
H13A H 0.1537 0.8430 -0.0528 0.077 Uiso 0.550(3) 1 calc GR . . A 1
H13B H 0.2380 0.8540 -0.0030 0.077 Uiso 0.550(3) 1 calc GR . . A 1
H13C H 0.1818 0.9251 -0.0115 0.077 Uiso 0.550(3) 1 calc GR . . A 1
C19A C 0.1986(6) 0.5031(7) 0.1493(8) 0.054(3) Uani 0.550(3) 1 d . U . A 1
H19A H 0.1473 0.4849 0.1284 0.065 Uiso 0.550(3) 1 calc R . . A 1
H19B H 0.2149 0.4971 0.2043 0.065 Uiso 0.550(3) 1 calc R . . A 1
C18A C 0.2022(2) 0.5875(3) 0.1307(2) 0.0385(10) Uani 0.550(3) 1 d . U . A 1
H18A H 0.1893 0.5923 0.0759 0.046 Uiso 0.550(3) 1 calc R . . A 1
H18B H 0.2533 0.6057 0.1541 0.046 Uiso 0.550(3) 1 calc R . . A 1
C16A C -0.0593(3) 0.6576(4) 0.0497(4) 0.0546(13) Uani 0.550(3) 1 d . U . A 1
H16A H -0.0595 0.6532 -0.0022 0.066 Uiso 0.550(3) 1 calc R . . A 1
H16B H -0.0697 0.6048 0.0657 0.066 Uiso 0.550(3) 1 calc R . . A 1
C17A C -0.1181(5) 0.7141(8) 0.0515(8) 0.108(4) Uani 0.550(3) 1 d . U . A 1
H17A H -0.1661 0.6917 0.0236 0.163 Uiso 0.550(3) 1 calc GR . . A 1
H17B H -0.1121 0.7643 0.0287 0.163 Uiso 0.550(3) 1 calc GR . . A 1
H17C H -0.1144 0.7233 0.1034 0.163 Uiso 0.550(3) 1 calc GR . . A 1
C25A C 0.3058(4) 0.6206(5) 0.4269(4) 0.0703(18) Uani 0.550(3) 1 d . U . A 1
H25A H 0.3374 0.5810 0.4162 0.105 Uiso 0.550(3) 1 calc GR . . A 1
H25B H 0.3003 0.6087 0.4750 0.105 Uiso 0.550(3) 1 calc GR . . A 1
H25C H 0.3277 0.6730 0.4291 0.105 Uiso 0.550(3) 1 calc GR . . A 1
C24A C 0.2324(4) 0.6192(5) 0.3667(3) 0.082(2) Uani 0.550(3) 1 d . U . A 1
H24A H 0.2106 0.5664 0.3663 0.098 Uiso 0.550(3) 1 calc R . . A 1
H24B H 0.2007 0.6580 0.3795 0.098 Uiso 0.550(3) 1 calc R . . A 1
C12A C 0.1722(3) 0.8387(3) 0.0595(3) 0.0421(11) Uani 0.550(3) 1 d . U . A 1
H12A H 0.1239 0.8592 0.0573 0.051 Uiso 0.550(3) 1 calc R . . A 1
H12B H 0.2093 0.8608 0.1047 0.051 Uiso 0.550(3) 1 calc R . . A 1
C1 C 0.4905(2) 0.4209(2) 0.3621(2) 0.0844(11) Uani 1 1 d . U . . .
C21A C 0.2462(10) 0.3658(8) 0.1511(10) 0.142(7) Uani 0.550(3) 1 d . U . A 1
H21A H 0.2731 0.3300 0.1294 0.212 Uiso 0.550(3) 1 calc GR . . A 1
H21B H 0.1958 0.3472 0.1384 0.212 Uiso 0.550(3) 1 calc GR . . A 1
H21C H 0.2699 0.3668 0.2055 0.212 Uiso 0.550(3) 1 calc GR . . A 1
C20A C 0.2461(4) 0.4515(3) 0.1187(3) 0.0519(13) Uani 0.550(3) 1 d . U . A 1
H20A H 0.2966 0.4725 0.1345 0.062 Uiso 0.550(3) 1 calc R . . A 1
H20B H 0.2260 0.4504 0.0635 0.062 Uiso 0.550(3) 1 calc R . . A 1
C22B C 0.2138(3) 0.6620(3) 0.2343(3) 0.0357(12) Uani 0.450(3) 1 d . U . A 2
H22C H 0.2623 0.6582 0.2286 0.043 Uiso 0.450(3) 1 calc R . . A 2
H22D H 0.2073 0.7174 0.2473 0.043 Uiso 0.450(3) 1 calc R . . A 2
C14B C 0.0822(3) 0.6710(4) 0.1617(3) 0.0430(13) Uani 0.450(3) 1 d . U . A 2
H14C H 0.0731 0.6424 0.2029 0.052 Uiso 0.450(3) 1 calc R . . A 2
H14D H 0.0864 0.7279 0.1742 0.052 Uiso 0.450(3) 1 calc R . . A 2
C10B C 0.1747(3) 0.6857(3) 0.0984(3) 0.0357(12) Uani 0.450(3) 1 d . U . A 2
H10C H 0.1452 0.6650 0.0486 0.043 Uiso 0.450(3) 1 calc R . . A 2
H10D H 0.2264 0.6727 0.1067 0.043 Uiso 0.450(3) 1 calc R . . A 2
C18B C 0.1506(3) 0.5557(3) 0.1439(3) 0.0388(12) Uani 0.450(3) 1 d . U . A 2
H18C H 0.1124 0.5442 0.0952 0.047 Uiso 0.450(3) 1 calc R . . A 2
H18D H 0.1346 0.5314 0.1829 0.047 Uiso 0.450(3) 1 calc R . . A 2
C15B C 0.0196(7) 0.6587(7) 0.0917(8) 0.047(3) Uani 0.450(3) 1 d . U . A 2
H15C H 0.0115 0.6013 0.0827 0.056 Uiso 0.450(3) 1 calc R . . A 2
H15D H 0.0315 0.6812 0.0494 0.056 Uiso 0.450(3) 1 calc R . . A 2
C11B C 0.1672(4) 0.7745(4) 0.0963(5) 0.0467(17) Uani 0.450(3) 1 d . U . A 2
H11C H 0.1971 0.7969 0.1453 0.056 Uiso 0.450(3) 1 calc R . . A 2
H11D H 0.1155 0.7891 0.0866 0.056 Uiso 0.450(3) 1 calc R . . A 2
C19B C 0.2204(8) 0.5142(8) 0.1454(11) 0.057(3) Uani 0.450(3) 1 d . U . A 2
H19C H 0.2365 0.5351 0.1052 0.068 Uiso 0.450(3) 1 calc R . . A 2
H19D H 0.2597 0.5237 0.1939 0.068 Uiso 0.450(3) 1 calc R . . A 2
C23B C 0.2145(5) 0.6101(5) 0.2994(4) 0.0457(19) Uani 0.450(3) 1 d . U . A 2
H23C H 0.2235 0.5546 0.2888 0.055 Uiso 0.450(3) 1 calc R . . A 2
H23D H 0.1664 0.6128 0.3061 0.055 Uiso 0.450(3) 1 calc R . . A 2
C12B C 0.1923(3) 0.8083(5) 0.0352(4) 0.0507(16) Uani 0.450(3) 1 d . U . A 2
H12C H 0.1631 0.7849 -0.0134 0.061 Uiso 0.450(3) 1 calc R . . A 2
H12D H 0.2442 0.7943 0.0456 0.061 Uiso 0.450(3) 1 calc R . . A 2
C16B C -0.0506(4) 0.6966(6) 0.0942(5) 0.073(2) Uani 0.450(3) 1 d . U . A 2
H16C H -0.0635 0.6725 0.1353 0.087 Uiso 0.450(3) 1 calc R . . A 2
H16D H -0.0417 0.7535 0.1054 0.087 Uiso 0.450(3) 1 calc R . . A 2
C20B C 0.2051(5) 0.4275(5) 0.1344(6) 0.087(3) Uani 0.450(3) 1 d . U . A 2
H20C H 0.1826 0.4100 0.1710 0.105 Uiso 0.450(3) 1 calc R . . A 2
H20D H 0.1685 0.4197 0.0840 0.105 Uiso 0.450(3) 1 calc R . . A 2
C24B C 0.2742(5) 0.6374(4) 0.3708(4) 0.0514(16) Uani 0.450(3) 1 d . U . A 2
H24C H 0.2605 0.6893 0.3858 0.062 Uiso 0.450(3) 1 calc R . . A 2
H24D H 0.3205 0.6442 0.3608 0.062 Uiso 0.450(3) 1 calc R . . A 2
C13B C 0.1838(4) 0.8982(5) 0.0310(7) 0.085(3) Uani 0.450(3) 1 d . U . A 2
H13D H 0.1318 0.9118 0.0115 0.127 Uiso 0.450(3) 1 calc GR . . A 2
H13E H 0.2080 0.9195 -0.0021 0.127 Uiso 0.450(3) 1 calc GR . . A 2
H13F H 0.2062 0.9207 0.0811 0.127 Uiso 0.450(3) 1 calc GR . . A 2
C17B C -0.1150(6) 0.6873(8) 0.0213(8) 0.091(4) Uani 0.450(3) 1 d . U . A 2
H17D H -0.1234 0.6312 0.0092 0.137 Uiso 0.450(3) 1 calc GR . . A 2
H17E H -0.1041 0.7145 -0.0190 0.137 Uiso 0.450(3) 1 calc GR . . A 2
H17F H -0.1589 0.7104 0.0271 0.137 Uiso 0.450(3) 1 calc GR . . A 2
C21B C 0.2666(5) 0.3767(6) 0.1416(7) 0.053(2) Uani 0.450(3) 1 d . U . A 2
H21D H 0.2908 0.3940 0.1070 0.079 Uiso 0.450(3) 1 calc GR . . A 2
H21E H 0.2494 0.3223 0.1299 0.079 Uiso 0.450(3) 1 calc GR . . A 2
H21F H 0.3013 0.3792 0.1929 0.079 Uiso 0.450(3) 1 calc GR . . A 2
C25B C 0.2862(6) 0.5787(6) 0.4347(4) 0.076(3) Uani 0.450(3) 1 d . U . A 2
H25D H 0.2999 0.5273 0.4200 0.113 Uiso 0.450(3) 1 calc GR . . A 2
H25E H 0.2410 0.5733 0.4460 0.113 Uiso 0.450(3) 1 calc GR . . A 2
H25F H 0.3255 0.5978 0.4791 0.113 Uiso 0.450(3) 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
S1 O3 1.470(2) . ?
S1 O4 1.457(2) . ?
S1 O2 1.443(2) . ?
S1 C9 1.793(3) . ?
N3 C22A 1.463(4) . ?
N3 C10A 1.514(5) . ?
N3 C14A 1.581(4) . ?
N3 C18A 1.529(5) . ?
N3 C22B 1.600(5) . ?
N3 C14B 1.499(5) . ?
N3 C10B 1.484(5) . ?
N3 C18B 1.491(5) . ?
O1 C8 1.232(3) . ?
O5 H5 0.8703 . ?
N1 H1 0.8800 . ?
N1 C8 1.372(3) . ?
N1 C5 1.394(4) . ?
F1 C1 1.351(5) . ?
N2 H2 0.8800 . ?
N2 C8 1.357(4) . ?
N2 C9 1.423(4) . ?
C6 H6 0.9500 . ?
C6 C5 1.397(4) . ?
C6 C7 1.374(4) . ?
F3 C1 1.331(4) . ?
C5 C4 1.401(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
F2 C1 1.329(5) . ?
C7 H7 0.9500 . ?
C7 C2 1.391(4) . ?
C2 C3 1.386(5) . ?
C2 C1 1.485(5) . ?
C15A H15A 0.9900 . ?
C15A H15B 0.9900 . ?
C15A C14A 1.511(9) . ?
C15A C16A 1.506(11) . ?
C4 H4 0.9500 . ?
C4 C3 1.378(5) . ?
C23A H23A 0.9900 . ?
C23A H23B 0.9900 . ?
C23A C22A 1.513(7) . ?
C23A C24A 1.485(9) . ?
C3 H3 0.9500 . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C11A C10A 1.501(7) . ?
C11A C12A 1.502(8) . ?
C22A H22A 0.9900 . ?
C22A H22B 0.9900 . ?
C10A H10A 0.9900 . ?
C10A H10B 0.9900 . ?
C14A H14A 0.9900 . ?
C14A H14B 0.9900 . ?
C13A H13A 0.9800 . ?
C13A H13B 0.9800 . ?
C13A H13C 0.9800 . ?
C13A C12A 1.500(8) . ?
C19A H19A 0.9900 . ?
C19A H19B 0.9900 . ?
C19A C18A 1.482(12) . ?
C19A C20A 1.529(13) . ?
C18A H18A 0.9900 . ?
C18A H18B 0.9900 . ?
C16A H16A 0.9900 . ?
C16A H16B 0.9900 . ?
C16A C17A 1.504(11) . ?
C17A H17A 0.9800 . ?
C17A H17B 0.9800 . ?
C17A H17C 0.9800 . ?
C25A H25A 0.9800 . ?
C25A H25B 0.9800 . ?
C25A H25C 0.9800 . ?
C25A C24A 1.494(9) . ?
C24A H24A 0.9900 . ?
C24A H24B 0.9900 . ?
C12A H12A 0.9900 . ?
C12A H12B 0.9900 . ?
C21A H21A 0.9800 . ?
C21A H21B 0.9800 . ?
C21A H21C 0.9800 . ?
C21A C20A 1.578(14) . ?
C20A H20A 0.9900 . ?
C20A H20B 0.9900 . ?
C22B H22C 0.9900 . ?
C22B H22D 0.9900 . ?
C22B C23B 1.517(9) . ?
C14B H14C 0.9900 . ?
C14B H14D 0.9900 . ?
C14B C15B 1.481(14) . ?
C10B H10C 0.9900 . ?
C10B H10D 0.9900 . ?
C10B C11B 1.512(9) . ?
C18B H18C 0.9900 . ?
C18B H18D 0.9900 . ?
C18B C19B 1.523(15) . ?
C15B H15C 0.9900 . ?
C15B H15D 0.9900 . ?
C15B C16B 1.527(14) . ?
C11B H11C 0.9900 . ?
C11B H11D 0.9900 . ?
C11B C12B 1.523(11) . ?
C19B H19C 0.9900 . ?
C19B H19D 0.9900 . ?
C19B C20B 1.500(17) . ?
C23B H23C 0.9900 . ?
C23B H23D 0.9900 . ?
C23B C24B 1.526(10) . ?
C12B H12C 0.9900 . ?
C12B H12D 0.9900 . ?
C12B C13B 1.532(12) . ?
C16B H16C 0.9900 . ?
C16B H16D 0.9900 . ?
C16B C17B 1.526(14) . ?
C20B H20C 0.9900 . ?
C20B H20D 0.9900 . ?
C20B C21B 1.442(14) . ?
C24B H24C 0.9900 . ?
C24B H24D 0.9900 . ?
C24B C25B 1.528(11) . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9800 . ?
C13B H13F 0.9800 . ?
C17B H17D 0.9800 . ?
C17B H17E 0.9800 . ?
C17B H17F 0.9800 . ?
C21B H21D 0.9800 . ?
C21B H21E 0.9800 . ?
C21B H21F 0.9800 . ?
C25B H25D 0.9800 . ?
C25B H25E 0.9800 . ?
C25B H25F 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
O3 S1 C9 105.28(12) . . ?
O4 S1 O3 110.72(12) . . ?
O4 S1 C9 106.68(13) . . ?
O2 S1 O3 114.18(13) . . ?
O2 S1 O4 114.75(12) . . ?
O2 S1 C9 104.26(15) . . ?
C22A N3 C10A 111.7(3) . . ?
C22A N3 C14A 109.3(3) . . ?
C22A N3 C18A 113.5(3) . . ?
C10A N3 C14A 108.8(2) . . ?
C10A N3 C18A 108.4(3) . . ?
C18A N3 C14A 104.9(3) . . ?
C14B N3 C22B 105.2(3) . . ?
C10B N3 C22B 106.3(3) . . ?
C10B N3 C14B 114.0(3) . . ?
C10B N3 C18B 112.4(3) . . ?
C18B N3 C22B 108.2(3) . . ?
C18B N3 C14B 110.3(3) . . ?
C8 N1 H1 116.6 . . ?
C8 N1 C5 126.8(2) . . ?
C5 N1 H1 116.6 . . ?
C8 N2 H2 119.4 . . ?
C8 N2 C9 121.2(2) . . ?
C9 N2 H2 119.4 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C7 C6 C5 120.0(3) . . ?
O1 C8 N1 123.7(3) . . ?
O1 C8 N2 122.2(3) . . ?
N2 C8 N1 114.1(2) . . ?
N1 C5 C6 124.2(3) . . ?
N1 C5 C4 117.3(3) . . ?
C6 C5 C4 118.5(3) . . ?
S1 C9 H9A 108.9 . . ?
S1 C9 H9B 108.9 . . ?
N2 C9 S1 113.23(18) . . ?
N2 C9 H9A 108.9 . . ?
N2 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C6 C7 H7 119.2 . . ?
C6 C7 C2 121.6(3) . . ?
C2 C7 H7 119.2 . . ?
C7 C2 C1 120.8(3) . . ?
C3 C2 C7 118.5(3) . . ?
C3 C2 C1 120.5(3) . . ?
H15A C15A H15B 108.1 . . ?
C14A C15A H15A 109.5 . . ?
C14A C15A H15B 109.5 . . ?
C16A C15A H15A 109.5 . . ?
C16A C15A H15B 109.5 . . ?
C16A C15A C14A 110.6(7) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 C5 120.7(3) . . ?
C3 C4 H4 119.6 . . ?
H23A C23A H23B 107.8 . . ?
C22A C23A H23A 109.1 . . ?
C22A C23A H23B 109.1 . . ?
C24A C23A H23A 109.1 . . ?
C24A C23A H23B 109.1 . . ?
C24A C23A C22A 112.5(6) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.6(3) . . ?
C4 C3 H3 119.7 . . ?
H11A C11A H11B 108.0 . . ?
C10A C11A H11A 109.4 . . ?
C10A C11A H11B 109.4 . . ?
C10A C11A C12A 111.0(5) . . ?
C12A C11A H11A 109.4 . . ?
C12A C11A H11B 109.4 . . ?
N3 C22A C23A 114.5(4) . . ?
N3 C22A H22A 108.6 . . ?
N3 C22A H22B 108.6 . . ?
C23A C22A H22A 108.6 . . ?
C23A C22A H22B 108.6 . . ?
H22A C22A H22B 107.6 . . ?
N3 C10A H10A 107.7 . . ?
N3 C10A H10B 107.7 . . ?
C11A C10A N3 118.5(4) . . ?
C11A C10A H10A 107.7 . . ?
C11A C10A H10B 107.7 . . ?
H10A C10A H10B 107.1 . . ?
N3 C14A H14A 108.4 . . ?
N3 C14A H14B 108.4 . . ?
C15A C14A N3 115.5(5) . . ?
C15A C14A H14A 108.4 . . ?
C15A C14A H14B 108.4 . . ?
H14A C14A H14B 107.5 . . ?
H13A C13A H13B 109.5 . . ?
H13A C13A H13C 109.5 . . ?
H13B C13A H13C 109.5 . . ?
C12A C13A H13A 109.5 . . ?
C12A C13A H13B 109.5 . . ?
C12A C13A H13C 109.5 . . ?
H19A C19A H19B 107.9 . . ?
C18A C19A H19A 109.2 . . ?
C18A C19A H19B 109.2 . . ?
C18A C19A C20A 112.1(8) . . ?
C20A C19A H19A 109.2 . . ?
C20A C19A H19B 109.2 . . ?
N3 C18A H18A 108.4 . . ?
N3 C18A H18B 108.4 . . ?
C19A C18A N3 115.6(5) . . ?
C19A C18A H18A 108.4 . . ?
C19A C18A H18B 108.4 . . ?
H18A C18A H18B 107.4 . . ?
C15A C16A H16A 109.3 . . ?
C15A C16A H16B 109.3 . . ?
H16A C16A H16B 107.9 . . ?
C17A C16A C15A 111.7(7) . . ?
C17A C16A H16A 109.3 . . ?
C17A C16A H16B 109.3 . . ?
C16A C17A H17A 109.5 . . ?
C16A C17A H17B 109.5 . . ?
C16A C17A H17C 109.5 . . ?
H17A C17A H17B 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
H25A C25A H25B 109.5 . . ?
H25A C25A H25C 109.5 . . ?
H25B C25A H25C 109.5 . . ?
C24A C25A H25A 109.5 . . ?
C24A C25A H25B 109.5 . . ?
C24A C25A H25C 109.5 . . ?
C23A C24A C25A 115.9(7) . . ?
C23A C24A H24A 108.3 . . ?
C23A C24A H24B 108.3 . . ?
C25A C24A H24A 108.3 . . ?
C25A C24A H24B 108.3 . . ?
H24A C24A H24B 107.4 . . ?
C11A C12A H12A 108.6 . . ?
C11A C12A H12B 108.6 . . ?
C13A C12A C11A 114.8(6) . . ?
C13A C12A H12A 108.6 . . ?
C13A C12A H12B 108.6 . . ?
H12A C12A H12B 107.5 . . ?
F1 C1 C2 112.9(4) . . ?
F3 C1 F1 105.3(3) . . ?
F3 C1 C2 112.6(3) . . ?
F2 C1 F1 104.4(3) . . ?
F2 C1 F3 106.9(4) . . ?
F2 C1 C2 114.0(3) . . ?
H21A C21A H21B 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C20A C21A H21A 109.5 . . ?
C20A C21A H21B 109.5 . . ?
C20A C21A H21C 109.5 . . ?
C19A C20A C21A 107.3(9) . . ?
C19A C20A H20A 110.3 . . ?
C19A C20A H20B 110.3 . . ?
C21A C20A H20A 110.3 . . ?
C21A C20A H20B 110.3 . . ?
H20A C20A H20B 108.5 . . ?
N3 C22B H22C 108.1 . . ?
N3 C22B H22D 108.1 . . ?
H22C C22B H22D 107.3 . . ?
C23B C22B N3 116.6(4) . . ?
C23B C22B H22C 108.1 . . ?
C23B C22B H22D 108.1 . . ?
N3 C14B H14C 109.2 . . ?
N3 C14B H14D 109.2 . . ?
H14C C14B H14D 107.9 . . ?
C15B C14B N3 112.0(6) . . ?
C15B C14B H14C 109.2 . . ?
C15B C14B H14D 109.2 . . ?
N3 C10B H10C 108.0 . . ?
N3 C10B H10D 108.0 . . ?
N3 C10B C11B 117.2(5) . . ?
H10C C10B H10D 107.2 . . ?
C11B C10B H10C 108.0 . . ?
C11B C10B H10D 108.0 . . ?
N3 C18B H18C 107.7 . . ?
N3 C18B H18D 107.7 . . ?
N3 C18B C19B 118.3(6) . . ?
H18C C18B H18D 107.1 . . ?
C19B C18B H18C 107.7 . . ?
C19B C18B H18D 107.7 . . ?
C14B C15B H15C 109.1 . . ?
C14B C15B H15D 109.1 . . ?
C14B C15B C16B 112.4(9) . . ?
H15C C15B H15D 107.8 . . ?
C16B C15B H15C 109.1 . . ?
C16B C15B H15D 109.1 . . ?
C10B C11B H11C 109.7 . . ?
C10B C11B H11D 109.7 . . ?
C10B C11B C12B 110.0(7) . . ?
H11C C11B H11D 108.2 . . ?
C12B C11B H11C 109.7 . . ?
C12B C11B H11D 109.7 . . ?
C18B C19B H19C 110.0 . . ?
C18B C19B H19D 110.0 . . ?
H19C C19B H19D 108.4 . . ?
C20B C19B C18B 108.5(10) . . ?
C20B C19B H19C 110.0 . . ?
C20B C19B H19D 110.0 . . ?
C22B C23B H23C 109.6 . . ?
C22B C23B H23D 109.6 . . ?
C22B C23B C24B 110.1(6) . . ?
H23C C23B H23D 108.2 . . ?
C24B C23B H23C 109.6 . . ?
C24B C23B H23D 109.6 . . ?
C11B C12B H12C 109.5 . . ?
C11B C12B H12D 109.5 . . ?
C11B C12B C13B 110.9(9) . . ?
H12C C12B H12D 108.0 . . ?
C13B C12B H12C 109.5 . . ?
C13B C12B H12D 109.5 . . ?
C15B C16B H16C 109.0 . . ?
C15B C16B H16D 109.0 . . ?
H16C C16B H16D 107.8 . . ?
C17B C16B C15B 113.1(10) . . ?
C17B C16B H16C 109.0 . . ?
C17B C16B H16D 109.0 . . ?
C19B C20B H20C 108.0 . . ?
C19B C20B H20D 108.0 . . ?
H20C C20B H20D 107.3 . . ?
C21B C20B C19B 117.0(10) . . ?
C21B C20B H20C 108.0 . . ?
C21B C20B H20D 108.0 . . ?
C23B C24B H24C 109.2 . . ?
C23B C24B H24D 109.2 . . ?
C23B C24B C25B 112.0(7) . . ?
H24C C24B H24D 107.9 . . ?
C25B C24B H24C 109.2 . . ?
C25B C24B H24D 109.2 . . ?
C12B C13B H13D 109.5 . . ?
C12B C13B H13E 109.5 . . ?
C12B C13B H13F 109.5 . . ?
H13D C13B H13E 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C16B C17B H17D 109.5 . . ?
C16B C17B H17E 109.5 . . ?
C16B C17B H17F 109.5 . . ?
H17D C17B H17E 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
C20B C21B H21D 109.5 . . ?
C20B C21B H21E 109.5 . . ?
C20B C21B H21F 109.5 . . ?
H21D C21B H21E 109.5 . . ?
H21D C21B H21F 109.5 . . ?
H21E C21B H21F 109.5 . . ?
C24B C25B H25D 109.5 . . ?
C24B C25B H25E 109.5 . . ?
C24B C25B H25F 109.5 . . ?
H25D C25B H25E 109.5 . . ?
H25D C25B H25F 109.5 . . ?
H25E C25B H25F 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
O3 S1 C9 N2 -61.0(2) . . . . ?
N3 C22B C23B C24B -178.4(5) . . . . ?
N3 C14B C15B C16B -172.6(7) . . . . ?
N3 C10B C11B C12B 179.8(4) . . . . ?
N3 C18B C19B C20B 178.9(8) . . . . ?
O4 S1 C9 N2 56.6(2) . . . . ?
O2 S1 C9 N2 178.5(2) . . . . ?
N1 C5 C4 C3 -176.5(3) . . . . ?
C6 C5 C4 C3 1.7(4) . . . . ?
C6 C7 C2 C3 1.2(5) . . . . ?
C6 C7 C2 C1 -173.4(3) . . . . ?
C8 N1 C5 C6 4.1(4) . . . . ?
C8 N1 C5 C4 -177.8(2) . . . . ?
C8 N2 C9 S1 -95.3(3) . . . . ?
C5 N1 C8 O1 12.0(4) . . . . ?
C5 N1 C8 N2 -169.0(2) . . . . ?
C5 C6 C7 C2 -0.7(4) . . . . ?
C5 C4 C3 C2 -1.3(5) . . . . ?
C9 N2 C8 O1 -9.3(4) . . . . ?
C9 N2 C8 N1 171.8(2) . . . . ?
C7 C6 C5 N1 177.4(2) . . . . ?
C7 C6 C5 C4 -0.7(4) . . . . ?
C7 C2 C3 C4 -0.2(5) . . . . ?
C7 C2 C1 F1 -146.2(3) . . . . ?
C7 C2 C1 F3 -27.1(5) . . . . ?
C7 C2 C1 F2 94.9(4) . . . . ?
C3 C2 C1 F1 39.4(4) . . . . ?
C3 C2 C1 F3 158.4(3) . . . . ?
C3 C2 C1 F2 -79.6(5) . . . . ?
C22A N3 C10A C11A 179.6(4) . . . . ?
C22A N3 C14A C15A 72.0(7) . . . . ?
C22A N3 C18A C19A 46.3(8) . . . . ?
C22A C23A C24A C25A 176.7(6) . . . . ?
C10A N3 C22A C23A -65.6(5) . . . . ?
C10A N3 C14A C15A -50.2(7) . . . . ?
C10A N3 C18A C19A 171.1(7) . . . . ?
C10A C11A C12A C13A 167.8(4) . . . . ?
C14A N3 C22A C23A 173.9(4) . . . . ?
C14A N3 C10A C11A -59.7(4) . . . . ?
C14A N3 C18A C19A -72.8(7) . . . . ?
C14A C15A C16A C17A 177.3(9) . . . . ?
C18A N3 C22A C23A 57.3(5) . . . . ?
C18A N3 C10A C11A 53.8(5) . . . . ?
C18A N3 C14A C15A -166.1(6) . . . . ?
C18A C19A C20A C21A 172.5(10) . . . . ?
C16A C15A C14A N3 -175.8(6) . . . . ?
C24A C23A C22A N3 -177.4(5) . . . . ?
C12A C11A C10A N3 164.8(4) . . . . ?
C1 C2 C3 C4 174.4(3) . . . . ?
C20A C19A C18A N3 176.5(6) . . . . ?
C22B N3 C14B C15B 179.0(7) . . . . ?
C22B N3 C10B C11B -71.5(5) . . . . ?
C22B N3 C18B C19B -58.2(9) . . . . ?
C22B C23B C24B C25B -169.9(7) . . . . ?
C14B N3 C22B C23B 73.2(6) . . . . ?
C14B N3 C10B C11B 44.0(6) . . . . ?
C14B N3 C18B C19B -172.8(9) . . . . ?
C14B C15B C16B C17B 177.7(10) . . . . ?
C10B N3 C22B C23B -165.5(5) . . . . ?
C10B N3 C14B C15B 62.9(7) . . . . ?
C10B N3 C18B C19B 58.8(9) . . . . ?
C10B C11B C12B C13B 178.9(6) . . . . ?
C18B N3 C22B C23B -44.7(6) . . . . ?
C18B N3 C14B C15B -64.6(7) . . . . ?
C18B N3 C10B C11B 170.4(5) . . . . ?
C18B C19B C20B C21B -173.9(11) . . . . ?

_shelx_SHELXL_version_number     2014/7
_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
;
####################################################################### 
# 
# 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_Compound_5
_database_code_depnum_ccdc_archive 'CCDC 1489608'
_audit_update_record             
;
2016-07-04 deposited with the CCDC.
2016-08-25 downloaded from the CCDC.
;
#-------------------------------------------------------------------------

_audit_creation_date             2016-05-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'2(C9 H8 F3 N2 O3 S2), C2 H6 O S, H2 O, 2(C16 H36 N)'
_chemical_formula_sum            'C26 H48 F3 N3 O4 S2.5'
_chemical_formula_weight         603.82
_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'
F F 0.0727 0.0534 '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                   12.3465(7)
_cell_length_b                   13.2148(9)
_cell_length_c                   20.8662(10)
_cell_angle_alpha                78.866(5)
_cell_angle_beta                 76.851(4)
_cell_angle_gamma                82.631(5)
_cell_volume                     3240.1(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7738
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      72.7640
_cell_measurement_theta_min      3.4110
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.225
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 -5 0.0229
0 1 5 0.0229
-5 0 -2 0.0654
5 0 2 0.0654
0 5 -3 0.0085
0 -5 3 0.0085

_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.017
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0030 -1.0194 -4.9946 0.0265 0.2314 -0.3039
-0.0030 1.0194 4.9946 -0.0265 -0.2314 0.3039
-4.9942 0.0298 -2.0200 -0.1174 -0.4904 -0.3763
4.9942 -0.0298 2.0200 0.1174 0.4904 0.3763
0.0146 4.9827 -3.0520 -0.6494 0.1369 -0.1236
-0.0146 -4.9827 3.0520 0.6494 -0.1369 0.1236

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0942
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21922
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         2.206
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 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    -64.00  32.00   1.00    7.50    --  -40.37  38.00   0.00   96
  2  ω     13.00  72.00   1.00    7.50    --   40.37 -99.00  30.00   59
  3  ω     46.00 116.00   1.00   30.00    --  105.19-111.00 -30.00   70
  4  ω     83.00 126.00   1.00   30.00    --  105.19 -30.00-180.00   43
  5  ω     67.00 134.00   1.00   30.00    --  105.19  15.00 -60.00   67
  6  ω    149.00 176.00   1.00   30.00    --  105.19  15.00 -60.00   27
  7  ω    105.00 162.00   1.00   30.00    --  105.19 111.00 -60.00   57
  8  ω     88.00 173.00   1.00   30.00    --  105.19  45.00   0.00   85
  9  ω    103.00 130.00   1.00   30.00    --  105.19 -61.00 150.00   27
 10  ω     59.00  86.00   1.00   30.00    --  105.19 -61.00 150.00   27
 11  ω     46.00 104.00   1.00   30.00    --  105.19 -94.00  60.00   58
 12  ω     37.00 117.00   1.00   30.00    --  105.19 -30.00 -30.00   80
 13  ω     32.00  86.00   1.00    7.50    --   40.37-125.00-120.00   54
 14  ω     32.00 110.00   1.00   30.00    --  105.19-111.00-180.00   78
 15  ω     34.00  98.00   1.00   30.00    --  105.19 -61.00 -60.00   64
 16  ω     30.00  97.00   1.00   30.00    --  105.19 -94.00-120.00   67
 17  ω     57.00 124.00   1.00   30.00    --  105.19 178.00-150.00   67
 18  ω   -111.00 -23.00   1.00    7.50    --  -40.37 -57.00  90.00   88
 19  ω   -109.00 -16.00   1.00    7.50    --  -40.37 -38.00-180.00   93
;
_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      0.0151256000
_diffrn_orient_matrix_UB_12      -0.1187699000
_diffrn_orient_matrix_UB_13      0.0189463000
_diffrn_orient_matrix_UB_21      0.1168213000
_diffrn_orient_matrix_UB_22      -0.0010676000
_diffrn_orient_matrix_UB_23      -0.0460511000
_diffrn_orient_matrix_UB_31      0.0516899000
_diffrn_orient_matrix_UB_32      0.0109695000
_diffrn_orient_matrix_UB_33      0.0586458000
_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                8101
_reflns_number_total             11448
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         11448
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0543
_refine_ls_restrained_S_all      1.037
_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)+(0.0338P)²+0.6218P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1386
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H7A(0.059) H7B(0.059) H1(0.029) H2(0.031) H4(0.034) H3(0.037)
 H9A(0.03) H9B(0.03) H20A(0.03) H20B(0.03) H19A(0.027) H19B(0.027) H4A(0.033)
 H31A(0.029) H31B(0.029) H21A(0.034) H21B(0.034) H6(0.03) H27A(0.031)
 H27B(0.031) H25A(0.036) H25B(0.036) H3A(0.036) H15(0.035) H23A(0.028)
 H23B(0.028) H7(0.034) H18A(0.035) H18B(0.035) H48A(0.034) H48B(0.034)
 H32A(0.031) H32B(0.031) H24A(0.032) H24B(0.032) H33A(0.031) H33B(0.031)
 H43A(0.033) H43B(0.033) H16(0.036) H36A(0.039) H36B(0.039) H39A(0.035)
 H39B(0.035) H49A(0.036) H49B(0.036) H47A(0.032) H47B(0.032) H34A(0.048)
 H34B(0.048) H34C(0.048) H35A(0.034) H35B(0.034) H44A(0.037) H44B(0.037)
 H45A(0.045) H45B(0.045) H22A(0.051) H22B(0.051) H22C(0.051) H13(0.042)
 H28A(0.04) H28B(0.04) H12(0.044) H40A(0.046) H40B(0.046) H37A(0.041)
 H37B(0.041) H26A(0.065) H26B(0.065) H26C(0.065) H41A(0.05) H41B(0.05)
 H38A(0.07) H38B(0.07) H38C(0.07) H29A(0.056) H29B(0.056) H29C(0.056)
 H29D(0.056) H50A(0.065) H50B(0.065) H50C(0.065) H46A(0.074) H46B(0.074)
 H46C(0.074) H42A(0.081) H42B(0.081) H42C(0.081) H51A(0.101) H51B(0.101)
 H51C(0.101) H30A(0.077) H30B(0.077) H30C(0.077) H52A(0.091) H52B(0.091)
 H52C(0.091) H52D(0.091) H52E(0.091) H52F(0.091) H30D(0.077) H30E(0.077)
 H30F(0.077)
 Fixed X: H7A(0.3185) H7B(0.4318) H1(0.8915) H2(0.8297) H4(0.8291) H3(0.691)
 H9A(0.7101) H9B(0.6179) H20A(0.8961) H20B(0.9314) H19A(0.7322) H19B(0.7658)
 H4A(0.7161) H31A(0.7153) H31B(0.8297) H21A(0.91) H21B(0.9246) H6(1.0272)
 H27A(0.7648) H27B(0.6635) H25A(0.3671) H25B(0.427) H3A(0.772) H15(0.5346)
 H23A(0.6012) H23B(0.5516) H7(1.0806) H18A(1.0003) H18B(1.0325) H48A(0.3679)
 H48B(0.4057) H32A(0.735) H32B(0.8522) H24A(0.5538) H24B(0.4954) H33A(0.7982)
 H33B(0.9119) H43A(0.3856) H43B(0.3182) H16(0.4043) H36A(0.2465) H36B(0.3347)
 H39A(0.105) H39B(0.1203) H49A(0.2409) H49B(0.2871) H47A(0.2235) H47B(0.1842)
 H34A(0.847) H34B(0.9631) H34C(0.9323) H35A(0.4229) H35B(0.3623) H44A(0.2279)
 H44B(0.1715) H45A(0.3763) H45B(0.3272) H22A(1.1009) H22B(1.0978) H22C(1.0858)
 H13(0.7391) H28A(0.5377) H28B(0.6327) H12(0.6104) H40A(0.2002) H40B(0.1883)
 H37A(0.3874) H37B(0.476) H26A(0.2731) H26B(0.308) H26C(0.378) H41A(0.0079)
 H41B(0.0419) H38A(0.3857) H38B(0.4201) H38C(0.296) H29A(0.6139) H29B(0.7073)
 H29C(0.558) H29D(0.6642) H50A(0.3712) H50B(0.4121) H50C(0.463) H46A(0.2238)
 H46B(0.175) H46C(0.287) H42A(-0.0584) H42B(-0.0116) H42C(-0.1118) H51A(0.2204)
 H51B(0.2213) H51C(0.3305) H30A(0.5687) H30B(0.5773) H30C(0.4812) H52A(0.0675)
 H52B(0.0542) H52C(0.0497) H52D(0.3391) H52E(0.2295) H52F(0.2365) H30D(0.7774)
 H30E(0.6896) H30F(0.6819)
 Fixed Y: H7A(0.597) H7B(0.5987) H1(0.8814) H2(0.8134) H4(0.6374) H3(0.7067)
 H9A(0.8094) H9B(0.8696) H20A(0.2248) H20B(0.2899) H19A(0.1894) H19B(0.2657)
 H4A(1.038) H31A(0.4964) H31B(0.4309) H21A(0.0733) H21B(0.1348) H6(1.0028)
 H27A(0.306) H27B(0.2438) H25A(0.3584) H25B(0.3074) H3A(1.1614) H15(0.6497)
 H23A(0.3752) H23B(0.424) H7(1.129) H18A(0.5499) H18B(0.6153) H48A(0.7977)
 H48B(0.9071) H32A(0.4792) H32B(0.418) H24A(0.2095) H24B(0.2644) H33A(0.6288)
 H33B(0.5687) H43A(0.7311) H43B(0.7145) H16(0.7013) H36A(1.0403) H36B(1.0567)
 H39A(0.8165) H39B(0.934) H49A(0.8792) H49B(0.9857) H47A(0.9615) H47B(0.854)
 H34A(0.5996) H34B(0.5471) H34C(0.6654) H35A(0.8962) H35B(0.8823) H44A(0.6855)
 H44B(0.6575) H45A(0.5597) H45B(0.535) H22A(0.1756) H22B(0.0552) H22C(0.1221)
 H13(0.8545) H28A(0.381) H28B(0.4565) H12(0.9052) H40A(0.7854) H40B(0.9058)
 H37A(1.042) H37B(1.0575) H26A(0.2191) H26B(0.2014) H26C(0.1437) H41A(0.7811)
 H41B(0.8351) H38A(1.2209) H38B(1.2168) H38C(1.2053) H29A(0.2867) H29B(0.3632)
 H29C(0.3627) H29D(0.2879) H50A(0.9213) H50B(0.8175) H50C(0.9205) H46A(0.4913)
 H46B(0.4665) H46C(0.4074) H42A(0.9366) H42B(0.9973) H42C(0.9297) H51A(0.3992)
 H51B(0.347) H51C(0.3883) H30A(0.4959) H30B(0.4078) H30C(0.4132) H52A(0.6026)
 H52B(0.4839) H52C(0.5544) H52D(0.5133) H52E(0.4703) H52F(0.5901) H30D(0.4089)
 H30E(0.4327) H30F(0.4983)
 Fixed Z: H7A(0.6123) H7B(0.6091) H1(0.6918) H2(0.6292) H4(0.7188) H3(0.7757)
 H9A(0.5617) H9B(0.6091) H20A(0.6138) H20B(0.5421) H19A(0.582) H19B(0.5149)
 H4A(0.7883) H31A(0.5885) H31B(0.5901) H21A(0.5705) H21B(0.4972) H6(0.679)
 H27A(0.6799) H27B(0.6833) H25A(0.5892) H25B(0.5268) H3A(0.8362) H15(0.8659)
 H23A(0.5267) H23B(0.5911) H7(0.7252) H18A(0.7053) H18B(0.7524) H48A(0.6637)
 H48B(0.6631) H32A(0.4757) H32B(0.4779) H24A(0.5898) H24B(0.6507) H33A(0.4919)
 H33B(0.504) H43A(0.7689) H43B(0.8426) H16(0.9551) H36A(0.8169) H36B(0.7494)
 H39A(0.8279) H39B(0.8212) H49A(0.594) H49B(0.5905) H47A(0.7133) H47B(0.7127)
 H34A(0.3798) H34B(0.3927) H34C(0.3949) H35A(0.7724) H35B(0.8476) H44A(0.7352)
 H44B(0.8112) H45A(0.7494) H45B(0.8263) H22A(0.501) H22B(0.52) H22C(0.576)
 H13(0.8791) H28A(0.7089) H28B(0.6923) H12(0.9683) H40A(0.9206) H40B(0.9175)
 H37A(0.8765) H37B(0.8091) H26A(0.5781) H26B(0.6474) H26C(0.5904) H41A(0.9459)
 H41B(0.998) H38A(0.7773) H38B(0.8456) H38C(0.8441) H29A(0.8001) H29B(0.7838)
 H29C(0.8136) H29D(0.7915) H50A(0.4945) H50B(0.5363) H50C(0.5357) H46A(0.7284)
 H46B(0.8054) H46C(0.7741) H42A(0.8923) H42B(0.9361) H42C(0.9686) H51A(0.9378)
 H51B(1.0118) H51C(0.9649) H30A(0.81) H30B(0.8713) H30C(0.8325) H52A(1.0455)
 H52B(1.0552) H52C(0.9861) H52D(1.0543) H52E(1.0998) H52F(1.078) H30D(0.776)
 H30E(0.8397) H30F(0.7695)
;
_atom_sites_solution_hydrogens   mixed
_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
S4 S 1.04788(6) 0.70936(6) 0.64634(4) 0.02329(16) Uani 1 1 d . . . . .
S0AA S 0.63118(6) 0.69572(6) 0.65414(4) 0.02496(17) Uani 1 1 d . . . . .
S1 S 0.63327(6) 1.00750(6) 0.67980(4) 0.02727(17) Uani 1 1 d . . . . .
S3 S 0.91293(7) 0.70100(8) 0.85104(4) 0.0362(2) Uani 1 1 d . . . . .
S5 S 0.21382(14) 0.52064(12) 1.00134(8) 0.0823(5) Uani 1 1 d . . . . .
F6 F 0.33730(18) 0.92160(19) 1.00380(11) 0.0473(6) Uani 1 1 d . . . . .
O5 O 1.03971(18) 0.80821(18) 0.67029(11) 0.0290(5) Uani 1 1 d . . . . .
O6 O 1.16226(18) 0.66977(19) 0.62365(11) 0.0307(5) Uani 1 1 d . . . . .
O1 O 0.57322(18) 0.71659(19) 0.71981(11) 0.0305(5) Uani 1 1 d . . . . .
O4 O 0.97621(18) 0.71408(19) 0.59928(11) 0.0293(5) Uani 1 1 d . . . . .
O2 O 0.73121(18) 0.62479(18) 0.65753(12) 0.0306(5) Uani 1 1 d . . . . .
O3 O 0.55930(19) 0.6674(2) 0.61530(12) 0.0355(6) Uani 1 1 d . . . . .
F4 F 0.4500(2) 0.8809(2) 1.06970(12) 0.0613(8) Uani 1 1 d . . . . .
O7 O 0.38336(19) 0.5699(2) 0.59735(14) 0.0395(6) Uani 1 1 d . . . . .
H7A H 0.3185 0.5970 0.6123 0.059 Uiso 1 1 d G . . . .
H7B H 0.4318 0.5987 0.6091 0.059 Uiso 1 1 d G . . . .
N5 N 0.7036(2) 0.3417(2) 0.59443(12) 0.0219(5) Uani 1 1 d . . . . .
F5 F 0.3430(3) 0.7704(2) 1.06082(13) 0.0735(9) Uani 1 1 d . . . . .
N1 N 0.8409(2) 0.9323(2) 0.69569(13) 0.0242(5) Uani 1 1 d . . . . .
H1 H 0.8915 0.8814 0.6918 0.029 Uiso 1 1 calc R . . . .
N2 N 0.7649(2) 0.8472(2) 0.63558(13) 0.0256(6) Uani 1 1 d . . . . .
H2 H 0.8297 0.8134 0.6292 0.031 Uiso 1 1 calc R . . . .
N4 N 0.8756(2) 0.6470(2) 0.74166(13) 0.0281(6) Uani 1 1 d . . . . .
H4 H 0.8291 0.6374 0.7188 0.034 Uiso 1 1 calc R . . . .
F1 F 0.8980(3) 1.2603(3) 0.86984(14) 0.0744(9) Uani 1 1 d . . . . .
N6 N 0.2660(2) 0.8500(2) 0.78763(13) 0.0254(6) Uani 1 1 d . . . . .
N3 N 0.7221(2) 0.7124(2) 0.80765(13) 0.0306(6) Uani 1 1 d . . . . .
H3 H 0.6910 0.7067 0.7757 0.037 Uiso 1 1 calc R . . . .
F2 F 0.9728(4) 1.3293(2) 0.77440(16) 0.0957(12) Uani 1 1 d . . . . .
F3 F 1.0646(2) 1.2136(3) 0.8309(2) 0.1143(17) Uani 1 1 d . . . . .
C5 C 0.8646(2) 1.0101(2) 0.72662(15) 0.0217(6) Uani 1 1 d . . . . .
C9 C 0.6800(3) 0.8165(2) 0.60794(15) 0.0251(6) Uani 1 1 d . . . . .
H9A H 0.7101 0.8094 0.5617 0.030 Uiso 1 1 calc R . . . .
H9B H 0.6179 0.8696 0.6091 0.030 Uiso 1 1 calc R . . . .
C20 C 0.8907(2) 0.2319(2) 0.56744(16) 0.0249(6) Uani 1 1 d . . . . .
H20A H 0.8961 0.2248 0.6138 0.030 Uiso 1 1 calc R . . . .
H20B H 0.9314 0.2899 0.5421 0.030 Uiso 1 1 calc R . . . .
C19 C 0.7690(2) 0.2519(2) 0.56185(15) 0.0229(6) Uani 1 1 d . . . . .
H19A H 0.7322 0.1894 0.5820 0.027 Uiso 1 1 calc R . . . .
H19B H 0.7658 0.2657 0.5149 0.027 Uiso 1 1 calc R . . . .
C4 C 0.7891(3) 1.0564(3) 0.77510(15) 0.0277(7) Uani 1 1 d . . . . .
H4A H 0.7161 1.0380 0.7883 0.033 Uiso 1 1 calc R . . . .
C8 C 0.7501(2) 0.9259(2) 0.67110(15) 0.0227(6) Uani 1 1 d . . . . .
C31 C 0.7639(3) 0.4400(2) 0.57091(15) 0.0243(6) Uani 1 1 d . . . . .
H31A H 0.7153 0.4964 0.5885 0.029 Uiso 1 1 calc R . . . .
H31B H 0.8297 0.4309 0.5901 0.029 Uiso 1 1 calc R . . . .
C21 C 0.9422(3) 0.1326(2) 0.54050(17) 0.0284(7) Uani 1 1 d D . . . .
H21A H 0.9100 0.0733 0.5705 0.034 Uiso 1 1 calc R . . . .
H21B H 0.9246 0.1348 0.4972 0.034 Uiso 1 1 calc R . . . .
C17 C 0.8338(3) 0.6878(3) 0.79735(15) 0.0278(7) Uani 1 1 d . . . . .
C6 C 0.9750(2) 1.0361(2) 0.70961(16) 0.0247(6) Uani 1 1 d . . . . .
H6 H 1.0272 1.0028 0.6790 0.030 Uiso 1 1 calc R . . . .
C14 C 0.6502(3) 0.7460(3) 0.86361(15) 0.0270(7) Uani 1 1 d . . . . .
C27 C 0.6914(3) 0.3117(2) 0.66955(15) 0.0258(7) Uani 1 1 d . . . . .
H27A H 0.7648 0.3060 0.6799 0.031 Uiso 1 1 calc R . . . .
H27B H 0.6635 0.2438 0.6833 0.031 Uiso 1 1 calc R . . . .
C25 C 0.4080(3) 0.2958(3) 0.57526(17) 0.0299(7) Uani 1 1 d D . . . .
H25A H 0.3671 0.3584 0.5892 0.036 Uiso 1 1 calc R . . . .
H25B H 0.4270 0.3074 0.5268 0.036 Uiso 1 1 calc R . . . .
C3 C 0.8228(3) 1.1304(3) 0.80388(16) 0.0304(7) Uani 1 1 d . . . . .
H3A H 0.7720 1.1614 0.8362 0.036 Uiso 1 1 calc R . . . .
C15 C 0.5497(3) 0.7011(3) 0.88664(16) 0.0288(7) Uani 1 1 d . . . . .
H15 H 0.5346 0.6497 0.8659 0.035 Uiso 1 1 calc R . . . .
C23 C 0.5898(2) 0.3619(2) 0.57507(15) 0.0237(6) Uani 1 1 d . . . . .
H23A H 0.6012 0.3752 0.5267 0.028 Uiso 1 1 calc R . . . .
H23B H 0.5516 0.4240 0.5911 0.028 Uiso 1 1 calc R . . . .
C7 C 1.0075(3) 1.1108(3) 0.73788(16) 0.0283(7) Uani 1 1 d . . . . .
H7 H 1.0806 1.1290 0.7252 0.034 Uiso 1 1 calc R . . . .
C18 C 0.9917(3) 0.6182(3) 0.71741(16) 0.0288(7) Uani 1 1 d . . . . .
H18A H 1.0003 0.5499 0.7053 0.035 Uiso 1 1 calc R . . . .
H18B H 1.0325 0.6153 0.7524 0.035 Uiso 1 1 calc R . . . .
C48 C 0.3436(3) 0.8709(3) 0.66063(16) 0.0284(7) Uani 1 1 d . . . . .
H48A H 0.3679 0.7977 0.6637 0.034 Uiso 1 1 calc R . . . .
H48B H 0.4057 0.9071 0.6631 0.034 Uiso 1 1 calc R . . . .
C32 C 0.7996(3) 0.4716(2) 0.49597(15) 0.0255(7) Uani 1 1 d . . . . .
H32A H 0.7350 0.4792 0.4757 0.031 Uiso 1 1 calc R . . . .
H32B H 0.8522 0.4180 0.4779 0.031 Uiso 1 1 calc R . . . .
C24 C 0.5142(2) 0.2734(2) 0.60237(17) 0.0267(7) Uani 1 1 d . . . . .
H24A H 0.5538 0.2095 0.5898 0.032 Uiso 1 1 calc R . . . .
H24B H 0.4954 0.2644 0.6507 0.032 Uiso 1 1 calc R . . . .
O8 O 0.2679(4) 0.5998(3) 0.94569(18) 0.0766(11) Uani 1 1 d . . . . .
C33 C 0.8537(3) 0.5734(2) 0.47896(15) 0.0262(7) Uani 1 1 d D . . . .
H33A H 0.7982 0.6288 0.4919 0.031 Uiso 1 1 calc R . . . .
H33B H 0.9119 0.5687 0.5040 0.031 Uiso 1 1 calc R . . . .
C43 C 0.3112(3) 0.7365(3) 0.79653(16) 0.0279(7) Uani 1 1 d . . . . .
H43A H 0.3856 0.7311 0.7689 0.033 Uiso 1 1 calc R . . . .
H43B H 0.3182 0.7145 0.8426 0.033 Uiso 1 1 calc R . . . .
C16 C 0.4715(3) 0.7316(3) 0.94005(16) 0.0303(7) Uani 1 1 d . . . . .
H16 H 0.4043 0.7013 0.9551 0.036 Uiso 1 1 calc R . . . .
C36 C 0.3242(3) 1.0257(3) 0.79620(17) 0.0323(7) Uani 1 1 d . . . . .
H36A H 0.2465 1.0403 0.8169 0.039 Uiso 1 1 calc R . . . .
H36B H 0.3347 1.0567 0.7494 0.039 Uiso 1 1 calc R . . . .
C2 C 0.9314(3) 1.1584(3) 0.78484(17) 0.0305(7) Uani 1 1 d . . . . .
C39 C 0.1533(3) 0.8645(3) 0.83427(16) 0.0288(7) Uani 1 1 d . . . . .
H39A H 0.1050 0.8165 0.8279 0.035 Uiso 1 1 calc R . . . .
H39B H 0.1203 0.9340 0.8212 0.035 Uiso 1 1 calc R . . . .
C49 C 0.3069(3) 0.9116(3) 0.59421(16) 0.0304(7) Uani 1 1 d D . . . .
H49A H 0.2409 0.8792 0.5940 0.036 Uiso 1 1 calc R . . . .
H49B H 0.2871 0.9857 0.5905 0.036 Uiso 1 1 calc R . . . .
C47 C 0.2462(3) 0.8879(2) 0.71769(15) 0.0263(7) Uani 1 1 d . . . . .
H47A H 0.2235 0.9615 0.7133 0.032 Uiso 1 1 calc R . . . .
H47B H 0.1842 0.8540 0.7127 0.032 Uiso 1 1 calc R . . . .
C11 C 0.4949(3) 0.8084(3) 0.97086(16) 0.0314(7) Uani 1 1 d . . . . .
C34 C 0.9036(3) 0.5987(3) 0.40478(16) 0.0317(7) Uani 1 1 d D . . . .
H34A H 0.8470 0.5996 0.3798 0.048 Uiso 1 1 calc GR . . . .
H34B H 0.9631 0.5471 0.3927 0.048 Uiso 1 1 calc GR . . . .
H34C H 0.9323 0.6654 0.3949 0.048 Uiso 1 1 calc GR . . . .
C35 C 0.3522(3) 0.9094(3) 0.80250(16) 0.0279(7) Uani 1 1 d . . . . .
H35A H 0.4229 0.8962 0.7724 0.034 Uiso 1 1 calc R . . . .
H35B H 0.3623 0.8823 0.8476 0.034 Uiso 1 1 calc R . . . .
C44 C 0.2425(3) 0.6615(3) 0.77966(17) 0.0306(7) Uani 1 1 d . . . . .
H44A H 0.2279 0.6855 0.7352 0.037 Uiso 1 1 calc R . . . .
H44B H 0.1715 0.6575 0.8112 0.037 Uiso 1 1 calc R . . . .
C45 C 0.3075(3) 0.5553(3) 0.78293(19) 0.0373(8) Uani 1 1 d D . . . .
H45A H 0.3763 0.5597 0.7494 0.045 Uiso 1 1 calc R . . . .
H45B H 0.3272 0.5350 0.8263 0.045 Uiso 1 1 calc R . . . .
C22 C 1.0683(3) 0.1202(3) 0.53379(17) 0.0337(7) Uani 1 1 d D . . . .
H22A H 1.1009 0.1756 0.5010 0.051 Uiso 1 1 calc GR . . . .
H22B H 1.0978 0.0552 0.5200 0.051 Uiso 1 1 calc GR . . . .
H22C H 1.0858 0.1221 0.5760 0.051 Uiso 1 1 calc GR . . . .
C13 C 0.6724(3) 0.8235(3) 0.89446(18) 0.0348(8) Uani 1 1 d . . . . .
H13 H 0.7391 0.8545 0.8791 0.042 Uiso 1 1 calc R . . . .
C28 C 0.6147(3) 0.3860(3) 0.71052(16) 0.0336(7) Uani 1 1 d . . . . .
H28A H 0.5377 0.3810 0.7089 0.040 Uiso 1 1 calc R . . . .
H28B H 0.6327 0.4565 0.6923 0.040 Uiso 1 1 calc R . . . .
C12 C 0.5953(3) 0.8538(3) 0.94760(18) 0.0365(8) Uani 1 1 d . . . . .
H12 H 0.6104 0.9052 0.9683 0.044 Uiso 1 1 calc R . . . .
C10 C 0.4089(3) 0.8444(3) 1.02590(18) 0.0399(9) Uani 1 1 d . . . . .
C40 C 0.1548(3) 0.8488(3) 0.90870(18) 0.0381(8) Uani 1 1 d . . . . .
H40A H 0.2002 0.7854 0.9206 0.046 Uiso 1 1 calc R . . . .
H40B H 0.1883 0.9058 0.9175 0.046 Uiso 1 1 calc R . . . .
C37 C 0.3984(3) 1.0730(3) 0.82963(18) 0.0339(8) Uani 1 1 d D . . . .
H37A H 0.3874 1.0420 0.8765 0.041 Uiso 1 1 calc R . . . .
H37B H 0.4760 1.0575 0.8091 0.041 Uiso 1 1 calc R . . . .
C26 C 0.3351(3) 0.2069(3) 0.6000(2) 0.0431(9) Uani 1 1 d D . . . .
H26A H 0.2731 0.2191 0.5781 0.065 Uiso 1 1 calc GR . . . .
H26B H 0.3080 0.2014 0.6474 0.065 Uiso 1 1 calc GR . . . .
H26C H 0.3780 0.1437 0.5904 0.065 Uiso 1 1 calc GR . . . .
C1 C 0.9675(3) 1.2394(3) 0.8144(2) 0.0401(9) Uani 1 1 d . . . . .
C41 C 0.0374(3) 0.8428(3) 0.95146(18) 0.0415(9) Uani 1 1 d D . . . .
H41A H 0.0079 0.7811 0.9459 0.050 Uiso 1 1 calc R . . . .
H41B H 0.0419 0.8351 0.9980 0.050 Uiso 1 1 calc R . . . .
C38 C 0.3727(4) 1.1898(3) 0.8236(2) 0.0464(10) Uani 1 1 d D . . . .
H38A H 0.3857 1.2209 0.7773 0.070 Uiso 1 1 calc GR . . . .
H38B H 0.4201 1.2168 0.8456 0.070 Uiso 1 1 calc GR . . . .
H38C H 0.2960 1.2053 0.8441 0.070 Uiso 1 1 calc GR . . . .
C29 C 0.6298(4) 0.3581(3) 0.78312(18) 0.0466(10) Uani 1 1 d D . . . .
H29A H 0.6139 0.2867 0.8001 0.056 Uiso 0.797(6) 1 calc R . P A 1
H29B H 0.7073 0.3632 0.7838 0.056 Uiso 0.797(6) 1 calc R . P A 1
H29C H 0.5580 0.3627 0.8136 0.056 Uiso 0.203(6) 1 calc R . P A 2
H29D H 0.6642 0.2879 0.7915 0.056 Uiso 0.203(6) 1 calc R . P A 2
C50 C 0.3964(3) 0.8908(3) 0.53477(18) 0.0435(9) Uani 1 1 d D . . . .
H50A H 0.3712 0.9213 0.4945 0.065 Uiso 1 1 calc GR . . . .
H50B H 0.4121 0.8175 0.5363 0.065 Uiso 1 1 calc GR . . . .
H50C H 0.4630 0.9205 0.5357 0.065 Uiso 1 1 calc GR . . . .
C46 C 0.2423(4) 0.4725(3) 0.7717(2) 0.0494(10) Uani 1 1 d D . . . .
H46A H 0.2238 0.4913 0.7284 0.074 Uiso 1 1 calc GR . . . .
H46B H 0.1750 0.4665 0.8054 0.074 Uiso 1 1 calc GR . . . .
H46C H 0.2870 0.4074 0.7741 0.074 Uiso 1 1 calc GR . . . .
C42 C -0.0434(4) 0.9349(4) 0.9357(2) 0.0540(11) Uani 1 1 d D . . . .
H42A H -0.0584 0.9366 0.8923 0.081 Uiso 1 1 calc GR . . . .
H42B H -0.0116 0.9973 0.9361 0.081 Uiso 1 1 calc GR . . . .
H42C H -0.1118 0.9297 0.9686 0.081 Uiso 1 1 calc GR . . . .
C51 C 0.2506(5) 0.4002(4) 0.9761(2) 0.0673(14) Uani 1 1 d . . . . .
H51A H 0.2204 0.3992 0.9378 0.101 Uiso 1 1 calc GR . . . .
H51B H 0.2213 0.3470 1.0118 0.101 Uiso 1 1 calc GR . . . .
H51C H 0.3305 0.3883 0.9649 0.101 Uiso 1 1 calc GR . . . .
C30A C 0.5580(5) 0.4246(4) 0.8282(2) 0.0513(14) Uani 0.797(6) 1 d D . P A 1
H30A H 0.5687 0.4959 0.8100 0.077 Uiso 0.797(6) 1 calc GR . P A 1
H30B H 0.5773 0.4078 0.8713 0.077 Uiso 0.797(6) 1 calc GR . P A 1
H30C H 0.4812 0.4132 0.8325 0.077 Uiso 0.797(6) 1 calc GR . P A 1
C52A C 0.0836(9) 0.5425(8) 1.0243(5) 0.0608(17) Uani 0.484(6) 1 d . . P B 1
H52A H 0.0675 0.6026 1.0455 0.091 Uiso 0.484(6) 1 calc GR . P B 1
H52B H 0.0542 0.4839 1.0552 0.091 Uiso 0.484(6) 1 calc GR . P B 1
H52C H 0.0497 0.5544 0.9861 0.091 Uiso 0.484(6) 1 calc GR . P B 1
C52B C 0.2590(9) 0.5239(7) 1.0644(4) 0.0608(17) Uani 0.516(6) 1 d . . P B 2
H52D H 0.3391 0.5133 1.0543 0.091 Uiso 0.516(6) 1 calc GR . P B 2
H52E H 0.2295 0.4703 1.0998 0.091 Uiso 0.516(6) 1 calc GR . P B 2
H52F H 0.2365 0.5901 1.0780 0.091 Uiso 0.516(6) 1 calc GR . P B 2
C30B C 0.7006(16) 0.4306(14) 0.7929(9) 0.0513(14) Uani 0.203(6) 1 d D . P A 2
H30D H 0.7774 0.4089 0.7760 0.077 Uiso 0.203(6) 1 calc GR . P A 2
H30E H 0.6896 0.4327 0.8397 0.077 Uiso 0.203(6) 1 calc GR . P A 2
H30F H 0.6819 0.4983 0.7695 0.077 Uiso 0.203(6) 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
S4 O5 1.470(2) . ?
S4 O6 1.447(2) . ?
S4 O4 1.452(2) . ?
S4 C18 1.786(4) . ?
S0AA O1 1.454(2) . ?
S0AA O2 1.458(2) . ?
S0AA O3 1.454(2) . ?
S0AA C9 1.796(3) . ?
S1 C8 1.684(3) . ?
S3 C17 1.691(3) . ?
S5 O8 1.498(4) . ?
S5 C51 1.745(5) . ?
S5 C52A 1.575(11) . ?
S5 C52B 1.551(9) . ?
F6 C10 1.345(5) . ?
F4 C10 1.330(4) . ?
O7 H7A 0.8502 . ?
O7 H7B 0.8505 . ?
N5 C19 1.529(4) . ?
N5 C31 1.523(4) . ?
N5 C27 1.518(4) . ?
N5 C23 1.526(4) . ?
F5 C10 1.345(5) . ?
N1 H1 0.8600 . ?
N1 C5 1.407(4) . ?
N1 C8 1.352(4) . ?
N2 H2 0.8600 . ?
N2 C9 1.439(4) . ?
N2 C8 1.360(4) . ?
N4 H4 0.8600 . ?
N4 C17 1.343(4) . ?
N4 C18 1.435(4) . ?
F1 C1 1.327(5) . ?
N6 C43 1.524(4) . ?
N6 C39 1.519(4) . ?
N6 C47 1.513(4) . ?
N6 C35 1.517(4) . ?
N3 H3 0.8600 . ?
N3 C17 1.353(4) . ?
N3 C14 1.406(4) . ?
F2 C1 1.312(5) . ?
F3 C1 1.308(4) . ?
C5 C4 1.390(5) . ?
C5 C6 1.398(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C19 1.520(4) . ?
C20 C21 1.533(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C4 H4A 0.9300 . ?
C4 C3 1.391(5) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.515(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.522(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.385(4) . ?
C14 C15 1.389(5) . ?
C14 C13 1.395(5) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.519(5) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C24 1.517(4) . ?
C25 C26 1.511(4) . ?
C3 H3A 0.9300 . ?
C3 C2 1.386(5) . ?
C15 H15 0.9300 . ?
C15 C16 1.386(5) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.531(4) . ?
C7 H7 0.9300 . ?
C7 C2 1.381(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C48 C49 1.533(4) . ?
C48 C47 1.515(5) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.523(4) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.519(4) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 C44 1.520(4) . ?
C16 H16 0.9300 . ?
C16 C11 1.392(5) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C35 1.519(5) . ?
C36 C37 1.524(4) . ?
C2 C1 1.492(5) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.531(5) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C49 C50 1.505(5) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C11 C12 1.391(5) . ?
C11 C10 1.483(5) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C44 C45 1.523(5) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C45 C46 1.520(5) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C13 H13 0.9300 . ?
C13 C12 1.375(5) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.537(5) . ?
C12 H12 0.9300 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 C41 1.523(5) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.522(5) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C42 1.507(5) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 H29C 0.9700 . ?
C29 H29D 0.9700 . ?
C29 C30A 1.477(6) . ?
C29 C30B 1.447(13) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C30A H30A 0.9600 . ?
C30A H30B 0.9600 . ?
C30A H30C 0.9600 . ?
C52A H52A 0.9600 . ?
C52A H52B 0.9600 . ?
C52A H52C 0.9600 . ?
C52B H52D 0.9600 . ?
C52B H52E 0.9600 . ?
C52B H52F 0.9600 . ?
C30B H30D 0.9600 . ?
C30B H30E 0.9600 . ?
C30B H30F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 S4 C18 105.89(14) . . ?
O6 S4 O5 112.60(13) . . ?
O6 S4 O4 114.55(13) . . ?
O6 S4 C18 106.00(15) . . ?
O4 S4 O5 111.68(13) . . ?
O4 S4 C18 105.27(14) . . ?
O1 S0AA O2 111.77(14) . . ?
O1 S0AA C9 106.03(15) . . ?
O2 S0AA C9 105.59(15) . . ?
O3 S0AA O1 114.09(14) . . ?
O3 S0AA O2 113.79(14) . . ?
O3 S0AA C9 104.59(15) . . ?
O8 S5 C51 107.2(2) . . ?
O8 S5 C52A 114.7(4) . . ?
O8 S5 C52B 108.1(4) . . ?
C52A S5 C51 112.1(4) . . ?
C52B S5 C51 110.8(4) . . ?
H7A O7 H7B 109.5 . . ?
C31 N5 C19 111.4(2) . . ?
C31 N5 C23 108.7(2) . . ?
C27 N5 C19 108.4(2) . . ?
C27 N5 C31 108.8(2) . . ?
C27 N5 C23 111.2(2) . . ?
C23 N5 C19 108.4(2) . . ?
C5 N1 H1 115.3 . . ?
C8 N1 H1 115.3 . . ?
C8 N1 C5 129.5(3) . . ?
C9 N2 H2 117.6 . . ?
C8 N2 H2 117.6 . . ?
C8 N2 C9 124.7(3) . . ?
C17 N4 H4 117.5 . . ?
C17 N4 C18 125.1(2) . . ?
C18 N4 H4 117.5 . . ?
C39 N6 C43 110.5(3) . . ?
C47 N6 C43 111.1(2) . . ?
C47 N6 C39 106.0(2) . . ?
C47 N6 C35 111.4(2) . . ?
C35 N6 C43 106.3(2) . . ?
C35 N6 C39 111.5(2) . . ?
C17 N3 H3 115.7 . . ?
C17 N3 C14 128.6(3) . . ?
C14 N3 H3 115.7 . . ?
C4 C5 N1 124.8(3) . . ?
C4 C5 C6 119.0(3) . . ?
C6 C5 N1 116.1(3) . . ?
S0AA C9 H9A 109.5 . . ?
S0AA C9 H9B 109.5 . . ?
N2 C9 S0AA 110.9(2) . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
H20A C20 H20B 108.2 . . ?
C19 C20 H20A 109.7 . . ?
C19 C20 H20B 109.7 . . ?
C19 C20 C21 109.7(2) . . ?
C21 C20 H20A 109.7 . . ?
C21 C20 H20B 109.7 . . ?
N5 C19 H19A 108.5 . . ?
N5 C19 H19B 108.5 . . ?
C20 C19 N5 115.2(2) . . ?
C20 C19 H19A 108.5 . . ?
C20 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C5 C4 H4A 120.1 . . ?
C5 C4 C3 119.9(3) . . ?
C3 C4 H4A 120.1 . . ?
N1 C8 S1 124.9(2) . . ?
N1 C8 N2 112.2(3) . . ?
N2 C8 S1 122.8(2) . . ?
N5 C31 H31A 108.3 . . ?
N5 C31 H31B 108.3 . . ?
H31A C31 H31B 107.4 . . ?
C32 C31 N5 115.8(2) . . ?
C32 C31 H31A 108.3 . . ?
C32 C31 H31B 108.3 . . ?
C20 C21 H21A 109.4 . . ?
C20 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 C20 111.1(3) . . ?
C22 C21 H21A 109.4 . . ?
C22 C21 H21B 109.4 . . ?
N4 C17 S3 122.8(2) . . ?
N4 C17 N3 113.5(3) . . ?
N3 C17 S3 123.6(2) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.7(3) . . ?
C7 C6 H6 119.7 . . ?
C15 C14 N3 116.7(3) . . ?
C15 C14 C13 119.5(3) . . ?
C13 C14 N3 123.8(3) . . ?
N5 C27 H27A 108.4 . . ?
N5 C27 H27B 108.4 . . ?
N5 C27 C28 115.4(3) . . ?
H27A C27 H27B 107.5 . . ?
C28 C27 H27A 108.4 . . ?
C28 C27 H27B 108.4 . . ?
H25A C25 H25B 108.0 . . ?
C24 C25 H25A 109.4 . . ?
C24 C25 H25B 109.4 . . ?
C26 C25 H25A 109.4 . . ?
C26 C25 H25B 109.4 . . ?
C26 C25 C24 111.0(3) . . ?
C4 C3 H3A 119.7 . . ?
C2 C3 C4 120.7(3) . . ?
C2 C3 H3A 119.7 . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 121.0(3) . . ?
C16 C15 H15 119.5 . . ?
N5 C23 H23A 108.6 . . ?
N5 C23 H23B 108.6 . . ?
N5 C23 C24 114.5(2) . . ?
H23A C23 H23B 107.6 . . ?
C24 C23 H23A 108.6 . . ?
C24 C23 H23B 108.6 . . ?
C6 C7 H7 120.0 . . ?
C2 C7 C6 120.1(3) . . ?
C2 C7 H7 120.0 . . ?
S4 C18 H18A 109.5 . . ?
S4 C18 H18B 109.5 . . ?
N4 C18 S4 110.6(2) . . ?
N4 C18 H18A 109.5 . . ?
N4 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
H48A C48 H48B 108.3 . . ?
C49 C48 H48A 109.9 . . ?
C49 C48 H48B 109.9 . . ?
C47 C48 H48A 109.9 . . ?
C47 C48 H48B 109.9 . . ?
C47 C48 C49 109.1(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 C33 110.7(2) . . ?
H32A C32 H32B 108.1 . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
C25 C24 C23 110.8(3) . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
C32 C33 H33A 109.4 . . ?
C32 C33 H33B 109.4 . . ?
H33A C33 H33B 108.0 . . ?
C34 C33 C32 111.2(3) . . ?
C34 C33 H33A 109.4 . . ?
C34 C33 H33B 109.4 . . ?
N6 C43 H43A 108.2 . . ?
N6 C43 H43B 108.2 . . ?
H43A C43 H43B 107.4 . . ?
C44 C43 N6 116.3(2) . . ?
C44 C43 H43A 108.2 . . ?
C44 C43 H43B 108.2 . . ?
C15 C16 H16 120.5 . . ?
C15 C16 C11 119.0(3) . . ?
C11 C16 H16 120.5 . . ?
H36A C36 H36B 108.1 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 C37 110.6(3) . . ?
C37 C36 H36A 109.5 . . ?
C37 C36 H36B 109.5 . . ?
C3 C2 C1 121.0(3) . . ?
C7 C2 C3 119.7(3) . . ?
C7 C2 C1 119.4(3) . . ?
N6 C39 H39A 108.3 . . ?
N6 C39 H39B 108.3 . . ?
N6 C39 C40 115.9(3) . . ?
H39A C39 H39B 107.4 . . ?
C40 C39 H39A 108.3 . . ?
C40 C39 H39B 108.3 . . ?
C48 C49 H49A 109.1 . . ?
C48 C49 H49B 109.1 . . ?
H49A C49 H49B 107.8 . . ?
C50 C49 C48 112.6(3) . . ?
C50 C49 H49A 109.1 . . ?
C50 C49 H49B 109.1 . . ?
N6 C47 C48 116.8(2) . . ?
N6 C47 H47A 108.1 . . ?
N6 C47 H47B 108.1 . . ?
C48 C47 H47A 108.1 . . ?
C48 C47 H47B 108.1 . . ?
H47A C47 H47B 107.3 . . ?
C16 C11 C10 118.9(3) . . ?
C12 C11 C16 120.0(3) . . ?
C12 C11 C10 121.1(3) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N6 C35 C36 115.4(3) . . ?
N6 C35 H35A 108.4 . . ?
N6 C35 H35B 108.4 . . ?
C36 C35 H35A 108.4 . . ?
C36 C35 H35B 108.4 . . ?
H35A C35 H35B 107.5 . . ?
C43 C44 H44A 109.9 . . ?
C43 C44 H44B 109.9 . . ?
C43 C44 C45 108.7(3) . . ?
H44A C44 H44B 108.3 . . ?
C45 C44 H44A 109.9 . . ?
C45 C44 H44B 109.9 . . ?
C44 C45 H45A 109.0 . . ?
C44 C45 H45B 109.0 . . ?
H45A C45 H45B 107.8 . . ?
C46 C45 C44 112.9(3) . . ?
C46 C45 H45A 109.0 . . ?
C46 C45 H45B 109.0 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C14 C13 H13 120.1 . . ?
C12 C13 C14 119.7(3) . . ?
C12 C13 H13 120.1 . . ?
C27 C28 H28A 109.9 . . ?
C27 C28 H28B 109.9 . . ?
C27 C28 C29 109.1(3) . . ?
H28A C28 H28B 108.3 . . ?
C29 C28 H28A 109.9 . . ?
C29 C28 H28B 109.9 . . ?
C11 C12 H12 119.6 . . ?
C13 C12 C11 120.8(3) . . ?
C13 C12 H12 119.6 . . ?
F6 C10 F5 104.1(3) . . ?
F6 C10 C11 112.6(3) . . ?
F4 C10 F6 105.1(3) . . ?
F4 C10 F5 107.0(3) . . ?
F4 C10 C11 114.2(3) . . ?
F5 C10 C11 113.1(3) . . ?
C39 C40 H40A 109.4 . . ?
C39 C40 H40B 109.4 . . ?
H40A C40 H40B 108.0 . . ?
C41 C40 C39 111.3(3) . . ?
C41 C40 H40A 109.4 . . ?
C41 C40 H40B 109.4 . . ?
C36 C37 H37A 109.3 . . ?
C36 C37 H37B 109.3 . . ?
H37A C37 H37B 107.9 . . ?
C38 C37 C36 111.7(3) . . ?
C38 C37 H37A 109.3 . . ?
C38 C37 H37B 109.3 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
F1 C1 C2 113.6(3) . . ?
F2 C1 F1 104.0(3) . . ?
F2 C1 C2 112.7(3) . . ?
F3 C1 F1 105.1(3) . . ?
F3 C1 F2 107.8(4) . . ?
F3 C1 C2 112.9(3) . . ?
C40 C41 H41A 108.6 . . ?
C40 C41 H41B 108.6 . . ?
H41A C41 H41B 107.6 . . ?
C42 C41 C40 114.8(4) . . ?
C42 C41 H41A 108.6 . . ?
C42 C41 H41B 108.6 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C28 C29 H29A 108.8 . . ?
C28 C29 H29B 108.8 . . ?
C28 C29 H29C 110.2 . . ?
C28 C29 H29D 110.2 . . ?
H29A C29 H29B 107.7 . . ?
H29C C29 H29D 108.5 . . ?
C30A C29 C28 114.0(4) . . ?
C30A C29 H29A 108.8 . . ?
C30A C29 H29B 108.8 . . ?
C30B C29 C28 107.8(8) . . ?
C30B C29 H29C 110.2 . . ?
C30B C29 H29D 110.2 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
S5 C51 H51A 109.5 . . ?
S5 C51 H51B 109.5 . . ?
S5 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C29 C30A H30A 109.5 . . ?
C29 C30A H30B 109.5 . . ?
C29 C30A H30C 109.5 . . ?
H30A C30A H30B 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
S5 C52A H52A 109.5 . . ?
S5 C52A H52B 109.5 . . ?
S5 C52A H52C 109.5 . . ?
H52A C52A H52B 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
S5 C52B H52D 109.5 . . ?
S5 C52B H52E 109.5 . . ?
S5 C52B H52F 109.5 . . ?
H52D C52B H52E 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
C29 C30B H30D 109.5 . . ?
C29 C30B H30E 109.5 . . ?
C29 C30B H30F 109.5 . . ?
H30D C30B H30E 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 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
O5 S4 C18 N4 63.7(2) . . . . ?
O6 S4 C18 N4 -176.51(19) . . . . ?
O1 S0AA C9 N2 67.2(2) . . . . ?
O4 S4 C18 N4 -54.7(2) . . . . ?
O2 S0AA C9 N2 -51.6(2) . . . . ?
O3 S0AA C9 N2 -171.9(2) . . . . ?
N5 C31 C32 C33 177.3(2) . . . . ?
N5 C27 C28 C29 -168.3(3) . . . . ?
N5 C23 C24 C25 -174.5(3) . . . . ?
N1 C5 C4 C3 177.9(3) . . . . ?
N1 C5 C6 C7 -179.2(3) . . . . ?
N6 C43 C44 C45 172.8(3) . . . . ?
N6 C39 C40 C41 -168.1(3) . . . . ?
N3 C14 C15 C16 -177.7(3) . . . . ?
N3 C14 C13 C12 177.8(3) . . . . ?
C5 N1 C8 S1 -7.2(5) . . . . ?
C5 N1 C8 N2 170.3(3) . . . . ?
C5 C4 C3 C2 -0.2(5) . . . . ?
C5 C6 C7 C2 1.9(5) . . . . ?
C9 N2 C8 S1 -7.4(5) . . . . ?
C9 N2 C8 N1 174.9(3) . . . . ?
C19 N5 C31 C32 51.2(3) . . . . ?
C19 N5 C27 C28 -171.9(3) . . . . ?
C19 N5 C23 C24 65.2(3) . . . . ?
C19 C20 C21 C22 169.9(3) . . . . ?
C4 C5 C6 C7 -3.5(5) . . . . ?
C4 C3 C2 C7 -1.4(5) . . . . ?
C4 C3 C2 C1 178.6(3) . . . . ?
C8 N1 C5 C4 44.3(5) . . . . ?
C8 N1 C5 C6 -140.2(3) . . . . ?
C8 N2 C9 S0AA -107.3(3) . . . . ?
C31 N5 C19 C20 51.7(3) . . . . ?
C31 N5 C27 C28 66.8(3) . . . . ?
C31 N5 C23 C24 -173.5(2) . . . . ?
C31 C32 C33 C34 172.4(3) . . . . ?
C21 C20 C19 N5 173.2(3) . . . . ?
C17 N4 C18 S4 -106.0(3) . . . . ?
C17 N3 C14 C15 -135.9(4) . . . . ?
C17 N3 C14 C13 46.9(5) . . . . ?
C6 C5 C4 C3 2.6(5) . . . . ?
C6 C7 C2 C3 0.5(5) . . . . ?
C6 C7 C2 C1 -179.5(3) . . . . ?
C14 N3 C17 S3 -4.3(5) . . . . ?
C14 N3 C17 N4 172.8(3) . . . . ?
C14 C15 C16 C11 -0.2(5) . . . . ?
C14 C13 C12 C11 -0.3(5) . . . . ?
C27 N5 C19 C20 -68.0(3) . . . . ?
C27 N5 C31 C32 170.6(3) . . . . ?
C27 N5 C23 C24 -53.8(3) . . . . ?
C27 C28 C29 C30A -179.2(4) . . . . ?
C27 C28 C29 C30B 101.2(9) . . . . ?
C3 C2 C1 F1 16.2(5) . . . . ?
C3 C2 C1 F2 -101.8(4) . . . . ?
C3 C2 C1 F3 135.8(4) . . . . ?
C15 C14 C13 C12 0.7(5) . . . . ?
C15 C16 C11 C12 0.5(5) . . . . ?
C15 C16 C11 C10 177.2(3) . . . . ?
C23 N5 C19 C20 171.3(3) . . . . ?
C23 N5 C31 C32 -68.2(3) . . . . ?
C23 N5 C27 C28 -52.9(3) . . . . ?
C7 C2 C1 F1 -163.8(3) . . . . ?
C7 C2 C1 F2 78.3(4) . . . . ?
C7 C2 C1 F3 -44.1(5) . . . . ?
C18 N4 C17 S3 -5.7(5) . . . . ?
C18 N4 C17 N3 177.2(3) . . . . ?
C43 N6 C39 C40 69.4(3) . . . . ?
C43 N6 C47 C48 -53.3(3) . . . . ?
C43 N6 C35 C36 179.7(3) . . . . ?
C43 C44 C45 C46 175.9(3) . . . . ?
C16 C11 C12 C13 -0.3(5) . . . . ?
C16 C11 C10 F6 -87.5(4) . . . . ?
C16 C11 C10 F4 152.7(3) . . . . ?
C16 C11 C10 F5 30.1(5) . . . . ?
C39 N6 C43 C44 62.8(3) . . . . ?
C39 N6 C47 C48 -173.4(3) . . . . ?
C39 N6 C35 C36 -59.7(4) . . . . ?
C39 C40 C41 C42 -56.4(4) . . . . ?
C49 C48 C47 N6 178.6(3) . . . . ?
C47 N6 C43 C44 -54.6(4) . . . . ?
C47 N6 C39 C40 -170.1(3) . . . . ?
C47 N6 C35 C36 58.5(4) . . . . ?
C47 C48 C49 C50 -175.9(3) . . . . ?
C35 N6 C43 C44 -176.0(3) . . . . ?
C35 N6 C39 C40 -48.7(4) . . . . ?
C35 N6 C47 C48 65.1(3) . . . . ?
C35 C36 C37 C38 179.6(3) . . . . ?
C13 C14 C15 C16 -0.4(5) . . . . ?
C12 C11 C10 F6 89.1(4) . . . . ?
C12 C11 C10 F4 -30.6(5) . . . . ?
C12 C11 C10 F5 -153.3(4) . . . . ?
C10 C11 C12 C13 -176.8(3) . . . . ?
C37 C36 C35 N6 164.8(3) . . . . ?
C26 C25 C24 C23 177.9(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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.001
_oxdiff_exptl_absorpt_empirical_full_min 0.719
####################################################################### 
# 
# 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_Compound_6
_database_code_depnum_ccdc_archive 'CCDC 1489609'
_audit_update_record             
;
2016-07-04 deposited with the CCDC.
2016-08-25 downloaded from the CCDC.
;
#-------------------------------------------------------------------------


_audit_creation_date             2016-07-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C10 H7 F6 N2 O4 S), 2(C16 H36 N)'
_chemical_formula_sum            'C26 H43 F6 N3 O4 S'
_chemical_formula_weight         607.69
_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'
F F 0.0727 0.0534 '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                   13.3272(4)
_cell_length_b                   20.7771(6)
_cell_length_c                   22.3152(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.086(3)
_cell_angle_gamma                90
_cell_volume                     6175.0(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9782
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      72.6420
_cell_measurement_theta_min      2.9020
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.562
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 3 -5 0.0360
0 -3 5 0.0280
5 2 0 0.1992
-5 -2 0 0.1092
0 1 1 0.0131
0 -1 -1 0.0131

_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.026
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0014 3.0108 -4.9864 -0.2541 0.3201 -0.0385
-0.0014 -3.0108 4.9864 0.2541 -0.3201 0.0385
4.9929 1.9983 0.0094 -0.0304 -0.0144 -0.5961
-4.9929 -1.9983 -0.0094 0.0304 0.0144 0.5961
-0.0011 0.9944 1.0047 0.0876 0.0431 -0.0265
0.0011 -0.9944 -1.0047 -0.0876 -0.0431 0.0265

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25495
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.062
_diffrn_reflns_theta_min         2.907
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  33.00   1.00    7.50    --  -40.37  57.00 120.00  102
  2  ω    -95.00 -19.00   1.00    7.50    --  -40.37 -38.00 -60.00   76
  3  ω   -112.00 -74.00   1.00    7.50    --  -40.37 -57.00  60.00   38
  4  ω    100.00 154.00   1.00   30.00    --  105.19 111.00 -60.00   54
  5  ω    111.00 171.00   1.00   30.00    --  105.19  45.00 -90.00   60
  6  ω     81.00 108.00   1.00   30.00    --  105.19  45.00 -90.00   27
  7  ω     80.00 129.00   1.00   30.00    --  105.19 -30.00-150.00   49
  8  ω     52.00 109.00   1.00   30.00    --  105.19 -45.00-150.00   57
  9  ω     26.00  81.00   1.00   30.00    --  105.19 -94.00  30.00   55
 10  ω     49.00 138.00   1.00   30.00    --  105.19 -77.00 120.00   89
 11  ω     76.00 102.00   1.00   30.00    --  105.19  61.00  90.00   26
 12  ω     28.00 101.00   1.00   30.00    --  105.19 -94.00  60.00   73
;
_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      -0.0153185000
_diffrn_orient_matrix_UB_12      0.0227519000
_diffrn_orient_matrix_UB_13      0.0646984000
_diffrn_orient_matrix_UB_21      -0.0297273000
_diffrn_orient_matrix_UB_22      0.0671992000
_diffrn_orient_matrix_UB_23      -0.0236311000
_diffrn_orient_matrix_UB_31      -0.1107908000
_diffrn_orient_matrix_UB_32      -0.0214419000
_diffrn_orient_matrix_UB_33      -0.0052606000
_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'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9632
_reflns_number_total             12024
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         12024
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0446
_refine_ls_restrained_S_all      1.015
_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)+(0.0465P)²+1.7581P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1148
_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
 C52A-C51A \\sim C51B-C52B \\sim C40-C39 \\sim C48A-C47A \\sim C48B-C47B \\sim
C32-C31 \\sim C28-C27 ~
 C24-C23 \\sim C36-C35 \\sim C44-C43
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C46A) = Uanis(C46B)
Uanis(C47A) = Uanis(C47B)
Uanis(C48A) = Uanis(C48B)
Uanis(C51A) = Uanis(C51B)
Uanis(C52A) = Uanis(C52B)
4. Others
 Sof(H45C)=Sof(H45D)=Sof(C46B)=Sof(H46C)=Sof(H46D)=Sof(C47B)=Sof(H47C)=
 Sof(H47D)=Sof(C48B)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(1)
 Sof(H45A)=Sof(H45B)=Sof(C47A)=Sof(H47A)=Sof(H47B)=Sof(C46A)=Sof(H46A)=
 Sof(H46B)=Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(1)
 Sof(C51B)=Sof(H51C)=Sof(H51D)=Sof(C52B)=Sof(H52D)=Sof(H52E)=Sof(H52F)=1-FVAR(2)
 Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(H52C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C33(H33A,H33B), C21(H21A,H21B), C29(H29A,H29B), C20(H20A,
 H20B), C10(H10A,H10B), C26(H26A,H26B), C42(H42A,H42B), C35(H35A,H35B),
 C22(H22A,H22B), C30(H30A,H30B), C34(H34A,H34B), C37(H37A,H37B), C41(H41A,H41B),
  C23(H23A,H23B), C27(H27A,H27B), C39(H39A,H39B), C43(H43A,H43B), C38(H38A,
 H38B), C31(H31A,H31B), C45(H45A,H45B), C45(H45C,H45D), C49(H49A,H49B),
 C50(H50A,H50B), C47A(H47A,H47B), C51A(H51A,H51B), C46A(H46A,H46B), C46B(H46C,
 H46D), C47B(H47C,H47D), C51B(H51C,H51D)
5.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N1(H1), N3(H3), N2(H2), C6(H6), C7(H7), C17(H17), C1(H1A), C16(H16),
 C11(H11)
5.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C44(H44A,H44B,H44C), C36(H36A,H36B,H36C), C40(H40A,H40B,
 H40C), C32(H32A,H32B,H32C), C28(H28A,H28B,H28C), C48A(H48A,H48B,H48C),
 C52A(H52A,H52B,H52C), C48B(H48D,H48E,H48F), C52B(H52D,H52E,H52F)
;
_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
S2 S 0.15766(3) 0.53733(2) 0.33957(2) 0.02674(10) Uani 1 1 d . . . . .
S1 S 0.48874(3) 0.38787(2) 0.36018(2) 0.02819(10) Uani 1 1 d . . . . .
O1 O 0.54899(10) 0.55419(7) 0.43162(6) 0.0304(3) Uani 1 1 d . . . . .
O8 O 0.21948(10) 0.58985(6) 0.31776(6) 0.0293(3) Uani 1 1 d . . . . .
O5 O 0.26079(10) 0.52016(7) 0.18803(6) 0.0313(3) Uani 1 1 d . . . . .
O2 O 0.53696(10) 0.43251(7) 0.31948(6) 0.0321(3) Uani 1 1 d . . . . .
O6 O 0.19561(11) 0.51283(7) 0.39752(6) 0.0340(3) Uani 1 1 d . . . . .
O4 O 0.39223(11) 0.36516(7) 0.33523(7) 0.0342(3) Uani 1 1 d . . . . .
F2 F 0.70962(10) 0.77046(8) 0.42794(7) 0.0564(4) Uani 1 1 d . . . . .
O7 O 0.05103(10) 0.55207(7) 0.33749(7) 0.0355(3) Uani 1 1 d . . . . .
F10 F 0.52060(13) 0.59307(8) -0.01762(6) 0.0561(4) Uani 1 1 d . . . . .
F1 F 0.64082(12) 0.74733(8) 0.51003(6) 0.0590(4) Uani 1 1 d . . . . .
O3 O 0.55445(11) 0.33672(7) 0.38206(7) 0.0379(3) Uani 1 1 d . . . . .
F6 F 0.24419(13) 0.79129(7) 0.29895(8) 0.0648(5) Uani 1 1 d . . . . .
F9 F 0.79181(11) 0.48446(9) 0.17901(7) 0.0598(4) Uani 1 1 d . . . . .
F11 F 0.48476(14) 0.66073(7) 0.05050(7) 0.0612(4) Uani 1 1 d . . . . .
F12 F 0.37344(12) 0.59301(9) 0.01766(7) 0.0646(4) Uani 1 1 d . . . . .
F3 F 0.62102(12) 0.84102(7) 0.47130(8) 0.0626(4) Uani 1 1 d . . . . .
F5 F 0.27895(13) 0.86085(8) 0.36560(8) 0.0657(5) Uani 1 1 d . . . . .
N4 N 0.27312(12) 0.46001(8) 0.27341(7) 0.0287(3) Uani 1 1 d . . . . .
H4 H 0.3111 0.4349 0.2965 0.034 Uiso 1 1 calc R . . . .
N1 N 0.40899(12) 0.59982(8) 0.38589(7) 0.0286(3) Uani 1 1 d . . . . .
H1 H 0.3526 0.5902 0.3661 0.034 Uiso 1 1 calc R . . . .
N5 N 0.81116(11) 0.48361(7) 0.39230(7) 0.0261(3) Uani 1 1 d . . . . .
N3 N 0.41251(12) 0.47631(8) 0.21866(7) 0.0309(3) Uani 1 1 d . . . . .
H3 H 0.4427 0.4545 0.2479 0.037 Uiso 1 1 calc R . . . .
N2 N 0.40982(12) 0.49301(8) 0.41169(8) 0.0299(3) Uani 1 1 d . . . . .
H2 H 0.3448 0.4933 0.4032 0.036 Uiso 1 1 calc R . . . .
F8 F 0.79228(12) 0.48067(13) 0.08400(8) 0.0874(7) Uani 1 1 d . . . . .
F7 F 0.74287(13) 0.40080(9) 0.13402(12) 0.0858(7) Uani 1 1 d . . . . .
N6 N 0.46936(12) 0.16071(8) 0.32762(8) 0.0341(4) Uani 1 1 d . . . . .
F4 F 0.36901(14) 0.85503(11) 0.28985(10) 0.0927(8) Uani 1 1 d . . . . .
C19 C 0.31141(14) 0.48815(9) 0.22395(8) 0.0278(4) Uani 1 1 d . . . . .
C9 C 0.46280(14) 0.54905(9) 0.41120(8) 0.0270(4) Uani 1 1 d . . . . .
C8 C 0.43542(14) 0.66448(9) 0.38865(8) 0.0268(4) Uani 1 1 d . . . . .
C25 C 0.87911(14) 0.52554(9) 0.43225(9) 0.0289(4) Uani 1 1 d . . . . .
H25A H 0.9198 0.4971 0.4592 0.035 Uiso 1 1 calc R . . . .
H25B H 0.9260 0.5488 0.4066 0.035 Uiso 1 1 calc R . . . .
C6 C 0.37099(14) 0.70778(9) 0.35773(9) 0.0292(4) Uani 1 1 d . . . . .
H6 H 0.3148 0.6920 0.3348 0.035 Uiso 1 1 calc R . . . .
C5 C 0.53449(15) 0.75493(10) 0.42337(9) 0.0315(4) Uani 1 1 d . . . . .
C7 C 0.51806(14) 0.68879(10) 0.42155(8) 0.0295(4) Uani 1 1 d . . . . .
H7 H 0.5628 0.6604 0.4425 0.035 Uiso 1 1 calc R . . . .
C18 C 0.47185(14) 0.49548(9) 0.17147(9) 0.0296(4) Uani 1 1 d . . . . .
C33 C 0.87853(13) 0.44651(9) 0.35100(8) 0.0272(4) Uani 1 1 d . . . . .
H33A H 0.9346 0.4277 0.3755 0.033 Uiso 1 1 calc R . . . .
H33B H 0.9078 0.4773 0.3226 0.033 Uiso 1 1 calc R . . . .
C21 C 0.73638(14) 0.52424(9) 0.35594(9) 0.0291(4) Uani 1 1 d . . . . .
H21A H 0.6914 0.5460 0.3839 0.035 Uiso 1 1 calc R . . . .
H21B H 0.6945 0.4953 0.3302 0.035 Uiso 1 1 calc R . . . .
C4 C 0.38921(15) 0.77312(10) 0.36065(9) 0.0319(4) Uani 1 1 d . . . . .
C17 C 0.57045(15) 0.47279(10) 0.17265(9) 0.0327(4) Uani 1 1 d . . . . .
H17 H 0.5938 0.4455 0.2043 0.039 Uiso 1 1 calc R . . . .
C29 C 0.75076(14) 0.43822(9) 0.43062(9) 0.0295(4) Uani 1 1 d . . . . .
H29A H 0.7073 0.4641 0.4564 0.035 Uiso 1 1 calc R . . . .
H29B H 0.7065 0.4117 0.4039 0.035 Uiso 1 1 calc R . . . .
C20 C 0.17082(13) 0.47159(9) 0.28761(9) 0.0282(4) Uani 1 1 d . . . . .
H20A H 0.1426 0.4321 0.3052 0.034 Uiso 1 1 calc R . . . .
H20B H 0.1315 0.4813 0.2502 0.034 Uiso 1 1 calc R . . . .
C1 C 0.47153(16) 0.79788(10) 0.39325(9) 0.0333(4) Uani 1 1 d . . . . .
H1A H 0.4840 0.8429 0.3947 0.040 Uiso 1 1 calc R . . . .
C10 C 0.45966(15) 0.43357(9) 0.42606(9) 0.0309(4) Uani 1 1 d . . . . .
H10A H 0.4163 0.4074 0.4516 0.037 Uiso 1 1 calc R . . . .
H10B H 0.5226 0.4428 0.4494 0.037 Uiso 1 1 calc R . . . .
C15 C 0.63467(16) 0.49002(11) 0.12760(10) 0.0367(4) Uani 1 1 d . . . . .
C26 C 0.82584(15) 0.57456(10) 0.47049(9) 0.0317(4) Uani 1 1 d . . . . .
H26A H 0.7728 0.5531 0.4932 0.038 Uiso 1 1 calc R . . . .
H26B H 0.7939 0.6080 0.4446 0.038 Uiso 1 1 calc R . . . .
C42 C 0.28000(15) 0.18342(10) 0.31483(9) 0.0321(4) Uani 1 1 d . . . . .
H42A H 0.2661 0.1367 0.3170 0.039 Uiso 1 1 calc R . . . .
H42B H 0.2838 0.1956 0.2721 0.039 Uiso 1 1 calc R . . . .
C35 C 0.90212(16) 0.36077(10) 0.27433(9) 0.0348(4) Uani 1 1 d D . . . .
H35A H 0.9233 0.3923 0.2441 0.042 Uiso 1 1 calc R . . . .
H35B H 0.9624 0.3478 0.2986 0.042 Uiso 1 1 calc R . . . .
C22 C 0.78284(15) 0.57519(10) 0.31626(9) 0.0326(4) Uani 1 1 d . . . . .
H22A H 0.8001 0.5557 0.2775 0.039 Uiso 1 1 calc R . . . .
H22B H 0.8454 0.5917 0.3360 0.039 Uiso 1 1 calc R . . . .
C30 C 0.81475(16) 0.39380(11) 0.47018(9) 0.0354(4) Uani 1 1 d . . . . .
H30A H 0.8493 0.4194 0.5022 0.042 Uiso 1 1 calc R . . . .
H30B H 0.8667 0.3735 0.4459 0.042 Uiso 1 1 calc R . . . .
C16 C 0.43913(15) 0.53612(10) 0.12491(9) 0.0324(4) Uani 1 1 d . . . . .
H16 H 0.3723 0.5521 0.1235 0.039 Uiso 1 1 calc R . . . .
C34 C 0.82734(15) 0.39270(10) 0.31505(9) 0.0327(4) Uani 1 1 d . . . . .
H34A H 0.7705 0.4105 0.2905 0.039 Uiso 1 1 calc R . . . .
H34B H 0.8004 0.3603 0.3427 0.039 Uiso 1 1 calc R . . . .
C37 C 0.45292(15) 0.08912(10) 0.33568(10) 0.0356(4) Uani 1 1 d . . . . .
H37A H 0.5155 0.0665 0.3257 0.043 Uiso 1 1 calc R . . . .
H37B H 0.3999 0.0751 0.3063 0.043 Uiso 1 1 calc R . . . .
C14 C 0.50517(17) 0.55304(11) 0.08057(9) 0.0365(4) Uani 1 1 d . . . . .
C41 C 0.37875(15) 0.19863(10) 0.34789(9) 0.0325(4) Uani 1 1 d . . . . .
H41A H 0.3707 0.1905 0.3912 0.039 Uiso 1 1 calc R . . . .
H41B H 0.3929 0.2451 0.3431 0.039 Uiso 1 1 calc R . . . .
C23 C 0.70922(16) 0.63074(10) 0.30514(10) 0.0372(4) Uani 1 1 d D . . . .
H23A H 0.6908 0.6488 0.3443 0.045 Uiso 1 1 calc R . . . .
H23B H 0.7434 0.6651 0.2828 0.045 Uiso 1 1 calc R . . . .
C27 C 0.90280(17) 0.60536(11) 0.51379(10) 0.0398(5) Uani 1 1 d D . . . .
H27A H 0.9338 0.5714 0.5395 0.048 Uiso 1 1 calc R . . . .
H27B H 0.9566 0.6251 0.4905 0.048 Uiso 1 1 calc R . . . .
C3 C 0.62576(17) 0.77872(11) 0.45775(10) 0.0398(5) Uani 1 1 d . . . . .
C2 C 0.32001(17) 0.81924(10) 0.32823(11) 0.0395(5) Uani 1 1 d . . . . .
C39 C 0.42965(16) -0.00574(10) 0.40256(10) 0.0373(5) Uani 1 1 d D . . . .
H39A H 0.3972 -0.0253 0.3663 0.045 Uiso 1 1 calc R . . . .
H39B H 0.5011 -0.0190 0.4042 0.045 Uiso 1 1 calc R . . . .
C43 C 0.19627(15) 0.22097(11) 0.34367(10) 0.0378(5) Uani 1 1 d D . . . .
H43A H 0.2111 0.2676 0.3413 0.045 Uiso 1 1 calc R . . . .
H43B H 0.1943 0.2092 0.3866 0.045 Uiso 1 1 calc R . . . .
C11 C 0.60309(17) 0.53000(11) 0.08114(10) 0.0397(5) Uani 1 1 d . . . . .
H11 H 0.6472 0.5414 0.0504 0.048 Uiso 1 1 calc R . . . .
C38 C 0.42344(16) 0.06753(10) 0.39755(10) 0.0379(5) Uani 1 1 d . . . . .
H38A H 0.3541 0.0818 0.4049 0.045 Uiso 1 1 calc R . . . .
H38B H 0.4689 0.0875 0.4283 0.045 Uiso 1 1 calc R . . . .
C31 C 0.75212(17) 0.34152(11) 0.49868(10) 0.0393(5) Uani 1 1 d D . . . .
H31A H 0.7201 0.3144 0.4669 0.047 Uiso 1 1 calc R . . . .
H31B H 0.6983 0.3616 0.5217 0.047 Uiso 1 1 calc R . . . .
C45 C 0.55833(16) 0.18489(11) 0.36557(11) 0.0411(5) Uani 1 1 d . . . . .
H45A H 0.5484 0.1729 0.4079 0.049 Uiso 0.736(3) 1 calc R . P A 1
H45B H 0.5598 0.2325 0.3634 0.049 Uiso 0.736(3) 1 calc R . P A 1
H45C H 0.5337 0.1981 0.4050 0.049 Uiso 0.264(3) 1 calc R . P A 2
H45D H 0.5849 0.2239 0.3461 0.049 Uiso 0.264(3) 1 calc R . P A 2
C49 C 0.48546(16) 0.17067(11) 0.26131(10) 0.0399(5) Uani 1 1 d . . . . .
H49A H 0.5427 0.1435 0.2498 0.048 Uiso 1 1 calc R . . . .
H49B H 0.4251 0.1550 0.2386 0.048 Uiso 1 1 calc R . . . .
C24 C 0.61382(18) 0.61159(12) 0.27020(11) 0.0440(5) Uani 1 1 d D . . . .
H24A H 0.6310 0.5956 0.2305 0.066 Uiso 1 1 calc GR . . . .
H24B H 0.5697 0.6491 0.2656 0.066 Uiso 1 1 calc GR . . . .
H24C H 0.5793 0.5777 0.2919 0.066 Uiso 1 1 calc GR . . . .
C12 C 0.47062(19) 0.59958(12) 0.03292(10) 0.0450(5) Uani 1 1 d . . . . .
C44 C 0.09369(16) 0.20804(12) 0.31366(10) 0.0409(5) Uani 1 1 d D . . . .
H44A H 0.0935 0.2227 0.2719 0.061 Uiso 1 1 calc GR . . . .
H44B H 0.0420 0.2313 0.3351 0.061 Uiso 1 1 calc GR . . . .
H44C H 0.0795 0.1618 0.3146 0.061 Uiso 1 1 calc GR . . . .
C50 C 0.50577(18) 0.23919(12) 0.24177(11) 0.0447(5) Uani 1 1 d . . . . .
H50A H 0.4502 0.2678 0.2530 0.054 Uiso 1 1 calc R . . B 1
H50B H 0.5689 0.2552 0.2612 0.054 Uiso 1 1 calc R . . B 1
C13 C 0.73921(17) 0.46408(13) 0.13055(11) 0.0449(5) Uani 1 1 d . . . . .
C36 C 0.8583(2) 0.30186(13) 0.24239(12) 0.0524(6) Uani 1 1 d D . . . .
H36A H 0.9089 0.2830 0.2169 0.079 Uiso 1 1 calc GR . . . .
H36B H 0.7995 0.3146 0.2176 0.079 Uiso 1 1 calc GR . . . .
H36C H 0.8383 0.2701 0.2722 0.079 Uiso 1 1 calc GR . . . .
C40 C 0.37912(19) -0.03077(12) 0.45777(11) 0.0471(5) Uani 1 1 d D . . . .
H40A H 0.3069 -0.0219 0.4542 0.071 Uiso 1 1 calc GR . . . .
H40B H 0.4078 -0.0093 0.4935 0.071 Uiso 1 1 calc GR . . . .
H40C H 0.3900 -0.0773 0.4612 0.071 Uiso 1 1 calc GR . . . .
C32 C 0.8180(2) 0.29981(13) 0.54022(12) 0.0541(6) Uani 1 1 d D . . . .
H32A H 0.8742 0.2827 0.5180 0.081 Uiso 1 1 calc GR . . . .
H32B H 0.7781 0.2641 0.5554 0.081 Uiso 1 1 calc GR . . . .
H32C H 0.8439 0.3258 0.5740 0.081 Uiso 1 1 calc GR . . . .
C28 C 0.8580(2) 0.65629(13) 0.55340(12) 0.0542(6) Uani 1 1 d D . . . .
H28A H 0.8307 0.6914 0.5284 0.081 Uiso 1 1 calc GR . . . .
H28B H 0.9102 0.6732 0.5811 0.081 Uiso 1 1 calc GR . . . .
H28C H 0.8041 0.6372 0.5763 0.081 Uiso 1 1 calc GR . . . .
C47A C 0.7442(3) 0.18543(19) 0.38907(16) 0.0398(8) Uani 0.736(3) 1 d D . P A 1
H47A H 0.8097 0.1689 0.3762 0.048 Uiso 0.736(3) 1 calc R . P A 1
H47B H 0.7454 0.2329 0.3855 0.048 Uiso 0.736(3) 1 calc R . P A 1
C51A C 0.5142(3) 0.23771(17) 0.17441(15) 0.0493(8) Uani 0.814(5) 1 d D . P C 1
H51A H 0.4519 0.2196 0.1558 0.059 Uiso 0.814(5) 1 calc R . P C 1
H51B H 0.5707 0.2094 0.1639 0.059 Uiso 0.814(5) 1 calc R . P C 1
C46A C 0.6608(2) 0.15881(16) 0.34697(14) 0.0384(7) Uani 0.736(3) 1 d . . P A 1
H46A H 0.6607 0.1112 0.3488 0.046 Uiso 0.736(3) 1 calc R . P A 1
H46B H 0.6731 0.1718 0.3052 0.046 Uiso 0.736(3) 1 calc R . P A 1
C48A C 0.7314(2) 0.16742(17) 0.45466(15) 0.0456(7) Uani 0.736(3) 1 d D . P A 1
H48A H 0.7178 0.1212 0.4577 0.068 Uiso 0.736(3) 1 calc GR . P A 1
H48B H 0.6752 0.1917 0.4705 0.068 Uiso 0.736(3) 1 calc GR . P A 1
H48C H 0.7931 0.1778 0.4779 0.068 Uiso 0.736(3) 1 calc GR . P A 1
C52A C 0.5314(3) 0.30479(17) 0.14970(18) 0.0639(9) Uani 0.814(5) 1 d D . P C 1
H52A H 0.5380 0.3024 0.1062 0.096 Uiso 0.814(5) 1 calc GR . P C 1
H52B H 0.5930 0.3229 0.1682 0.096 Uiso 0.814(5) 1 calc GR . P C 1
H52C H 0.4743 0.3324 0.1588 0.096 Uiso 0.814(5) 1 calc GR . P C 1
C46B C 0.6485(6) 0.1362(5) 0.3768(4) 0.0384(7) Uani 0.264(3) 1 d . . P A 2
H46C H 0.6262 0.0989 0.4004 0.046 Uiso 0.264(3) 1 calc R . P A 2
H46D H 0.6728 0.1204 0.3381 0.046 Uiso 0.264(3) 1 calc R . P A 2
C47B C 0.7330(9) 0.1727(6) 0.4115(6) 0.0398(8) Uani 0.264(3) 1 d D . P A 2
H47C H 0.7049 0.1931 0.4473 0.048 Uiso 0.264(3) 1 calc R . P A 2
H47D H 0.7848 0.1414 0.4255 0.048 Uiso 0.264(3) 1 calc R . P A 2
C48B C 0.7821(7) 0.2240(5) 0.3744(4) 0.0456(7) Uani 0.264(3) 1 d D . P A 2
H48D H 0.8149 0.2038 0.3406 0.068 Uiso 0.264(3) 1 calc GR . P A 2
H48E H 0.8322 0.2470 0.3994 0.068 Uiso 0.264(3) 1 calc GR . P A 2
H48F H 0.7310 0.2543 0.3592 0.068 Uiso 0.264(3) 1 calc GR . P A 2
C51B C 0.4902(13) 0.2662(8) 0.1726(7) 0.0493(8) Uani 0.186(5) 1 d D . P C 2
H51C H 0.4203 0.2595 0.1575 0.059 Uiso 0.186(5) 1 calc R . P C 2
H51D H 0.5061 0.3127 0.1706 0.059 Uiso 0.186(5) 1 calc R . P C 2
C52B C 0.5632(12) 0.2271(7) 0.1363(8) 0.0639(9) Uani 0.186(5) 1 d D . P C 2
H52D H 0.5619 0.2429 0.0949 0.096 Uiso 0.186(5) 1 calc GR . P C 2
H52E H 0.5434 0.1817 0.1366 0.096 Uiso 0.186(5) 1 calc GR . P C 2
H52F H 0.6312 0.2316 0.1540 0.096 Uiso 0.186(5) 1 calc GR . P C 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 O8 1.4612(13) . ?
S2 O6 1.4629(15) . ?
S2 O7 1.4527(14) . ?
S2 C20 1.8045(19) . ?
S1 O2 1.4632(14) . ?
S1 O4 1.4611(15) . ?
S1 O3 1.4504(15) . ?
S1 C10 1.804(2) . ?
O1 C9 1.225(2) . ?
O5 C19 1.225(2) . ?
F2 C3 1.332(3) . ?
F10 C12 1.337(3) . ?
F1 C3 1.345(3) . ?
F6 C2 1.318(3) . ?
F9 C13 1.336(3) . ?
F11 C12 1.341(3) . ?
F12 C12 1.334(3) . ?
F3 C3 1.331(3) . ?
F5 C2 1.332(3) . ?
N4 H4 0.8800 . ?
N4 C19 1.364(3) . ?
N4 C20 1.431(2) . ?
N1 H1 0.8800 . ?
N1 C9 1.384(3) . ?
N1 C8 1.390(2) . ?
N5 C25 1.522(2) . ?
N5 C33 1.520(2) . ?
N5 C21 1.518(2) . ?
N5 C29 1.523(2) . ?
N3 H3 0.8800 . ?
N3 C19 1.379(2) . ?
N3 C18 1.398(3) . ?
N2 H2 0.8800 . ?
N2 C9 1.362(2) . ?
N2 C10 1.433(2) . ?
F8 C13 1.323(3) . ?
F7 C13 1.318(3) . ?
N6 C37 1.515(3) . ?
N6 C41 1.524(2) . ?
N6 C45 1.517(3) . ?
N6 C49 1.517(3) . ?
F4 C2 1.324(3) . ?
C8 C6 1.407(3) . ?
C8 C7 1.396(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.521(3) . ?
C6 H6 0.9500 . ?
C6 C4 1.380(3) . ?
C5 C7 1.392(3) . ?
C5 C1 1.382(3) . ?
C5 C3 1.498(3) . ?
C7 H7 0.9500 . ?
C18 C17 1.395(3) . ?
C18 C16 1.396(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.523(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.526(3) . ?
C4 C1 1.393(3) . ?
C4 C2 1.498(3) . ?
C17 H17 0.9500 . ?
C17 C15 1.391(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.518(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C1 H1A 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C15 C11 1.382(3) . ?
C15 C13 1.493(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.524(3) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C41 1.518(3) . ?
C42 C43 1.523(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C34 1.525(3) . ?
C35 C36 1.522(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.529(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.523(3) . ?
C16 H16 0.9500 . ?
C16 C14 1.393(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.517(3) . ?
C14 C11 1.390(3) . ?
C14 C12 1.497(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.520(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.515(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C38 1.528(3) . ?
C39 C40 1.517(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.524(3) . ?
C11 H11 0.9500 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.524(3) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 H45C 0.9900 . ?
C45 H45D 0.9900 . ?
C45 C46A 1.540(4) . ?
C45 C46B 1.583(9) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.516(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C50 C51A 1.512(4) . ?
C50 C51B 1.649(17) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C47A H47A 0.9900 . ?
C47A H47B 0.9900 . ?
C47A C46A 1.532(5) . ?
C47A C48A 1.526(5) . ?
C51A H51A 0.9900 . ?
C51A H51B 0.9900 . ?
C51A C52A 1.519(4) . ?
C46A H46A 0.9900 . ?
C46A H46B 0.9900 . ?
C48A H48A 0.9800 . ?
C48A H48B 0.9800 . ?
C48A H48C 0.9800 . ?
C52A H52A 0.9800 . ?
C52A H52B 0.9800 . ?
C52A H52C 0.9800 . ?
C46B H46C 0.9900 . ?
C46B H46D 0.9900 . ?
C46B C47B 1.542(15) . ?
C47B H47C 0.9900 . ?
C47B H47D 0.9900 . ?
C47B C48B 1.512(10) . ?
C48B H48D 0.9800 . ?
C48B H48E 0.9800 . ?
C48B H48F 0.9800 . ?
C51B H51C 0.9900 . ?
C51B H51D 0.9900 . ?
C51B C52B 1.523(13) . ?
C52B H52D 0.9800 . ?
C52B H52E 0.9800 . ?
C52B H52F 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
O8 S2 O6 111.92(8) . . ?
O8 S2 C20 106.39(8) . . ?
O6 S2 C20 105.43(9) . . ?
O7 S2 O8 113.26(8) . . ?
O7 S2 O6 114.07(9) . . ?
O7 S2 C20 104.89(9) . . ?
O2 S1 C10 106.52(9) . . ?
O4 S1 O2 111.63(8) . . ?
O4 S1 C10 105.57(9) . . ?
O3 S1 O2 113.58(9) . . ?
O3 S1 O4 113.83(8) . . ?
O3 S1 C10 104.85(9) . . ?
C19 N4 H4 120.2 . . ?
C19 N4 C20 119.62(16) . . ?
C20 N4 H4 120.2 . . ?
C9 N1 H1 116.9 . . ?
C9 N1 C8 126.29(16) . . ?
C8 N1 H1 116.9 . . ?
C25 N5 C29 109.94(14) . . ?
C33 N5 C25 107.07(13) . . ?
C33 N5 C29 111.25(14) . . ?
C21 N5 C25 111.10(14) . . ?
C21 N5 C33 110.41(14) . . ?
C21 N5 C29 107.11(14) . . ?
C19 N3 H3 116.7 . . ?
C19 N3 C18 126.52(17) . . ?
C18 N3 H3 116.7 . . ?
C9 N2 H2 119.9 . . ?
C9 N2 C10 120.15(16) . . ?
C10 N2 H2 119.9 . . ?
C37 N6 C41 110.65(16) . . ?
C37 N6 C45 111.85(17) . . ?
C37 N6 C49 106.02(15) . . ?
C45 N6 C41 105.94(15) . . ?
C49 N6 C41 111.14(17) . . ?
C49 N6 C45 111.34(17) . . ?
O5 C19 N4 123.28(17) . . ?
O5 C19 N3 123.88(18) . . ?
N4 C19 N3 112.84(16) . . ?
O1 C9 N1 123.38(17) . . ?
O1 C9 N2 123.44(18) . . ?
N2 C9 N1 113.18(16) . . ?
N1 C8 C6 116.57(17) . . ?
N1 C8 C7 124.54(18) . . ?
C7 C8 C6 118.84(17) . . ?
N5 C25 H25A 108.4 . . ?
N5 C25 H25B 108.4 . . ?
H25A C25 H25B 107.4 . . ?
C26 C25 N5 115.60(15) . . ?
C26 C25 H25A 108.4 . . ?
C26 C25 H25B 108.4 . . ?
C8 C6 H6 119.9 . . ?
C4 C6 C8 120.17(18) . . ?
C4 C6 H6 119.9 . . ?
C7 C5 C3 117.68(19) . . ?
C1 C5 C7 122.08(19) . . ?
C1 C5 C3 120.21(19) . . ?
C8 C7 H7 120.2 . . ?
C5 C7 C8 119.53(19) . . ?
C5 C7 H7 120.2 . . ?
C17 C18 N3 116.60(18) . . ?
C17 C18 C16 119.13(18) . . ?
C16 C18 N3 124.26(18) . . ?
N5 C33 H33A 108.4 . . ?
N5 C33 H33B 108.4 . . ?
N5 C33 C34 115.38(15) . . ?
H33A C33 H33B 107.5 . . ?
C34 C33 H33A 108.4 . . ?
C34 C33 H33B 108.4 . . ?
N5 C21 H21A 108.5 . . ?
N5 C21 H21B 108.5 . . ?
N5 C21 C22 115.05(15) . . ?
H21A C21 H21B 107.5 . . ?
C22 C21 H21A 108.5 . . ?
C22 C21 H21B 108.5 . . ?
C6 C4 C1 121.46(19) . . ?
C6 C4 C2 120.14(19) . . ?
C1 C4 C2 118.40(18) . . ?
C18 C17 H17 119.9 . . ?
C15 C17 C18 120.2(2) . . ?
C15 C17 H17 119.9 . . ?
N5 C29 H29A 108.8 . . ?
N5 C29 H29B 108.8 . . ?
H29A C29 H29B 107.7 . . ?
C30 C29 N5 113.95(15) . . ?
C30 C29 H29A 108.8 . . ?
C30 C29 H29B 108.8 . . ?
S2 C20 H20A 109.1 . . ?
S2 C20 H20B 109.1 . . ?
N4 C20 S2 112.65(13) . . ?
N4 C20 H20A 109.1 . . ?
N4 C20 H20B 109.1 . . ?
H20A C20 H20B 107.8 . . ?
C5 C1 C4 117.92(18) . . ?
C5 C1 H1A 121.0 . . ?
C4 C1 H1A 121.0 . . ?
S1 C10 H10A 109.1 . . ?
S1 C10 H10B 109.1 . . ?
N2 C10 S1 112.51(14) . . ?
N2 C10 H10A 109.1 . . ?
N2 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
C17 C15 C13 118.2(2) . . ?
C11 C15 C17 121.2(2) . . ?
C11 C15 C13 120.5(2) . . ?
C25 C26 H26A 110.0 . . ?
C25 C26 H26B 110.0 . . ?
C25 C26 C27 108.65(16) . . ?
H26A C26 H26B 108.3 . . ?
C27 C26 H26A 110.0 . . ?
C27 C26 H26B 110.0 . . ?
H42A C42 H42B 108.3 . . ?
C41 C42 H42A 109.9 . . ?
C41 C42 H42B 109.9 . . ?
C41 C42 C43 108.87(16) . . ?
C43 C42 H42A 109.9 . . ?
C43 C42 H42B 109.9 . . ?
H35A C35 H35B 107.9 . . ?
C34 C35 H35A 109.1 . . ?
C34 C35 H35B 109.1 . . ?
C36 C35 H35A 109.1 . . ?
C36 C35 H35B 109.1 . . ?
C36 C35 C34 112.39(18) . . ?
C21 C22 H22A 109.6 . . ?
C21 C22 H22B 109.6 . . ?
C21 C22 C23 110.26(16) . . ?
H22A C22 H22B 108.1 . . ?
C23 C22 H22A 109.6 . . ?
C23 C22 H22B 109.6 . . ?
C29 C30 H30A 109.3 . . ?
C29 C30 H30B 109.3 . . ?
C29 C30 C31 111.82(17) . . ?
H30A C30 H30B 107.9 . . ?
C31 C30 H30A 109.3 . . ?
C31 C30 H30B 109.3 . . ?
C18 C16 H16 120.2 . . ?
C14 C16 C18 119.53(19) . . ?
C14 C16 H16 120.2 . . ?
C33 C34 C35 110.08(16) . . ?
C33 C34 H34A 109.6 . . ?
C33 C34 H34B 109.6 . . ?
C35 C34 H34A 109.6 . . ?
C35 C34 H34B 109.6 . . ?
H34A C34 H34B 108.2 . . ?
N6 C37 H37A 108.2 . . ?
N6 C37 H37B 108.2 . . ?
N6 C37 C38 116.21(17) . . ?
H37A C37 H37B 107.4 . . ?
C38 C37 H37A 108.2 . . ?
C38 C37 H37B 108.2 . . ?
C16 C14 C12 118.8(2) . . ?
C11 C14 C16 121.6(2) . . ?
C11 C14 C12 119.6(2) . . ?
N6 C41 H41A 108.4 . . ?
N6 C41 H41B 108.4 . . ?
C42 C41 N6 115.48(16) . . ?
C42 C41 H41A 108.4 . . ?
C42 C41 H41B 108.4 . . ?
H41A C41 H41B 107.5 . . ?
C22 C23 H23A 108.8 . . ?
C22 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
C24 C23 C22 113.91(18) . . ?
C24 C23 H23A 108.8 . . ?
C24 C23 H23B 108.8 . . ?
C26 C27 H27A 109.0 . . ?
C26 C27 H27B 109.0 . . ?
H27A C27 H27B 107.8 . . ?
C28 C27 C26 113.12(18) . . ?
C28 C27 H27A 109.0 . . ?
C28 C27 H27B 109.0 . . ?
F2 C3 F1 105.6(2) . . ?
F2 C3 C5 112.45(18) . . ?
F1 C3 C5 112.15(18) . . ?
F3 C3 F2 106.63(19) . . ?
F3 C3 F1 106.34(18) . . ?
F3 C3 C5 113.1(2) . . ?
F6 C2 F5 105.73(19) . . ?
F6 C2 F4 108.3(2) . . ?
F6 C2 C4 113.90(18) . . ?
F5 C2 C4 111.87(19) . . ?
F4 C2 F5 105.3(2) . . ?
F4 C2 C4 111.23(19) . . ?
H39A C39 H39B 107.9 . . ?
C38 C39 H39A 109.2 . . ?
C38 C39 H39B 109.2 . . ?
C40 C39 H39A 109.2 . . ?
C40 C39 H39B 109.2 . . ?
C40 C39 C38 112.10(19) . . ?
C42 C43 H43A 109.1 . . ?
C42 C43 H43B 109.1 . . ?
C42 C43 C44 112.53(18) . . ?
H43A C43 H43B 107.8 . . ?
C44 C43 H43A 109.1 . . ?
C44 C43 H43B 109.1 . . ?
C15 C11 C14 118.3(2) . . ?
C15 C11 H11 120.9 . . ?
C14 C11 H11 120.9 . . ?
C37 C38 C39 110.23(17) . . ?
C37 C38 H38A 109.6 . . ?
C37 C38 H38B 109.6 . . ?
C39 C38 H38A 109.6 . . ?
C39 C38 H38B 109.6 . . ?
H38A C38 H38B 108.1 . . ?
C30 C31 H31A 109.6 . . ?
C30 C31 H31B 109.6 . . ?
C30 C31 C32 110.3(2) . . ?
H31A C31 H31B 108.1 . . ?
C32 C31 H31A 109.6 . . ?
C32 C31 H31B 109.6 . . ?
N6 C45 H45A 108.6 . . ?
N6 C45 H45B 108.6 . . ?
N6 C45 H45C 108.1 . . ?
N6 C45 H45D 108.1 . . ?
N6 C45 C46A 114.57(19) . . ?
N6 C45 C46B 116.7(3) . . ?
H45A C45 H45B 107.6 . . ?
H45C C45 H45D 107.3 . . ?
C46A C45 H45A 108.6 . . ?
C46A C45 H45B 108.6 . . ?
C46B C45 H45C 108.1 . . ?
C46B C45 H45D 108.1 . . ?
N6 C49 H49A 108.2 . . ?
N6 C49 H49B 108.2 . . ?
H49A C49 H49B 107.4 . . ?
C50 C49 N6 116.20(18) . . ?
C50 C49 H49A 108.2 . . ?
C50 C49 H49B 108.2 . . ?
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 . . ?
F10 C12 F11 105.9(2) . . ?
F10 C12 C14 112.6(2) . . ?
F11 C12 C14 111.6(2) . . ?
F12 C12 F10 106.4(2) . . ?
F12 C12 F11 107.2(2) . . ?
F12 C12 C14 112.7(2) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C49 C50 H50A 110.4 . . ?
C49 C50 H50B 110.4 . . ?
C49 C50 C51B 124.9(6) . . ?
H50A C50 H50B 108.6 . . ?
C51A C50 C49 106.7(2) . . ?
C51A C50 H50A 110.4 . . ?
C51A C50 H50B 110.4 . . ?
F9 C13 C15 112.50(19) . . ?
F8 C13 F9 105.9(2) . . ?
F8 C13 C15 113.3(2) . . ?
F7 C13 F9 104.6(2) . . ?
F7 C13 F8 106.6(2) . . ?
F7 C13 C15 113.3(2) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
H47A C47A H47B 107.7 . . ?
C46A C47A H47A 108.9 . . ?
C46A C47A H47B 108.9 . . ?
C48A C47A H47A 108.9 . . ?
C48A C47A H47B 108.9 . . ?
C48A C47A C46A 113.3(3) . . ?
C50 C51A H51A 109.4 . . ?
C50 C51A H51B 109.4 . . ?
C50 C51A C52A 111.1(3) . . ?
H51A C51A H51B 108.0 . . ?
C52A C51A H51A 109.4 . . ?
C52A C51A H51B 109.4 . . ?
C45 C46A H46A 109.7 . . ?
C45 C46A H46B 109.7 . . ?
C47A C46A C45 109.8(2) . . ?
C47A C46A H46A 109.7 . . ?
C47A C46A H46B 109.7 . . ?
H46A C46A H46B 108.2 . . ?
C47A C48A H48A 109.5 . . ?
C47A C48A H48B 109.5 . . ?
C47A C48A H48C 109.5 . . ?
H48A C48A H48B 109.5 . . ?
H48A C48A H48C 109.5 . . ?
H48B C48A H48C 109.5 . . ?
C51A C52A H52A 109.5 . . ?
C51A C52A H52B 109.5 . . ?
C51A C52A H52C 109.5 . . ?
H52A C52A H52B 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
C45 C46B H46C 110.2 . . ?
C45 C46B H46D 110.2 . . ?
H46C C46B H46D 108.5 . . ?
C47B C46B C45 107.6(7) . . ?
C47B C46B H46C 110.2 . . ?
C47B C46B H46D 110.2 . . ?
C46B C47B H47C 108.9 . . ?
C46B C47B H47D 108.9 . . ?
H47C C47B H47D 107.7 . . ?
C48B C47B C46B 113.3(9) . . ?
C48B C47B H47C 108.9 . . ?
C48B C47B H47D 108.9 . . ?
C47B C48B H48D 109.5 . . ?
C47B C48B H48E 109.5 . . ?
C47B C48B H48F 109.5 . . ?
H48D C48B H48E 109.5 . . ?
H48D C48B H48F 109.5 . . ?
H48E C48B H48F 109.5 . . ?
C50 C51B H51C 110.8 . . ?
C50 C51B H51D 110.8 . . ?
H51C C51B H51D 108.9 . . ?
C52B C51B C50 104.8(12) . . ?
C52B C51B H51C 110.8 . . ?
C52B C51B H51D 110.8 . . ?
C51B C52B H52D 109.5 . . ?
C51B C52B H52E 109.5 . . ?
C51B C52B H52F 109.5 . . ?
H52D C52B H52E 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 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
O8 S2 C20 N4 46.45(15) . . . . ?
O2 S1 C10 N2 48.79(16) . . . . ?
O6 S2 C20 N4 -72.55(15) . . . . ?
O4 S1 C10 N2 -70.02(15) . . . . ?
O7 S2 C20 N4 166.71(13) . . . . ?
O3 S1 C10 N2 169.47(14) . . . . ?
N1 C8 C6 C4 176.83(17) . . . . ?
N1 C8 C7 C5 -176.87(17) . . . . ?
N5 C25 C26 C27 171.99(17) . . . . ?
N5 C33 C34 C35 178.38(16) . . . . ?
N5 C21 C22 C23 -154.09(16) . . . . ?
N5 C29 C30 C31 -169.51(16) . . . . ?
N3 C18 C17 C15 -179.51(18) . . . . ?
N3 C18 C16 C14 178.94(19) . . . . ?
N6 C37 C38 C39 -168.89(17) . . . . ?
N6 C45 C46A C47A -178.9(2) . . . . ?
N6 C45 C46B C47B 175.3(5) . . . . ?
N6 C49 C50 C51A -177.4(2) . . . . ?
N6 C49 C50 C51B -159.6(7) . . . . ?
C19 N4 C20 S2 -93.78(18) . . . . ?
C19 N3 C18 C17 -173.96(18) . . . . ?
C19 N3 C18 C16 7.3(3) . . . . ?
C9 N1 C8 C6 177.82(17) . . . . ?
C9 N1 C8 C7 -4.8(3) . . . . ?
C9 N2 C10 S1 -98.96(18) . . . . ?
C8 N1 C9 O1 -11.7(3) . . . . ?
C8 N1 C9 N2 167.63(17) . . . . ?
C8 C6 C4 C1 0.8(3) . . . . ?
C8 C6 C4 C2 -179.38(18) . . . . ?
C25 N5 C33 C34 169.35(16) . . . . ?
C25 N5 C21 C22 57.4(2) . . . . ?
C25 N5 C29 C30 -59.1(2) . . . . ?
C25 C26 C27 C28 178.8(2) . . . . ?
C6 C8 C7 C5 0.4(3) . . . . ?
C6 C4 C1 C5 -0.7(3) . . . . ?
C6 C4 C2 F6 0.5(3) . . . . ?
C6 C4 C2 F5 120.3(2) . . . . ?
C6 C4 C2 F4 -122.2(2) . . . . ?
C7 C8 C6 C4 -0.7(3) . . . . ?
C7 C5 C1 C4 0.4(3) . . . . ?
C7 C5 C3 F2 76.9(2) . . . . ?
C7 C5 C3 F1 -41.9(3) . . . . ?
C7 C5 C3 F3 -162.20(19) . . . . ?
C18 N3 C19 O5 -3.2(3) . . . . ?
C18 N3 C19 N4 176.34(18) . . . . ?
C18 C17 C15 C11 0.4(3) . . . . ?
C18 C17 C15 C13 -179.49(19) . . . . ?
C18 C16 C14 C11 0.5(3) . . . . ?
C18 C16 C14 C12 -176.60(19) . . . . ?
C33 N5 C25 C26 170.81(16) . . . . ?
C33 N5 C21 C22 -61.2(2) . . . . ?
C33 N5 C29 C30 59.3(2) . . . . ?
C21 N5 C25 C26 50.2(2) . . . . ?
C21 N5 C33 C34 -69.6(2) . . . . ?
C21 N5 C29 C30 -179.93(16) . . . . ?
C21 C22 C23 C24 -64.2(2) . . . . ?
C17 C18 C16 C14 0.2(3) . . . . ?
C17 C15 C11 C14 0.3(3) . . . . ?
C17 C15 C13 F9 -63.3(3) . . . . ?
C17 C15 C13 F8 176.7(2) . . . . ?
C17 C15 C13 F7 55.0(3) . . . . ?
C29 N5 C25 C26 -68.2(2) . . . . ?
C29 N5 C33 C34 49.2(2) . . . . ?
C29 N5 C21 C22 177.51(16) . . . . ?
C29 C30 C31 C32 -177.43(19) . . . . ?
C20 N4 C19 O5 -4.9(3) . . . . ?
C20 N4 C19 N3 175.53(16) . . . . ?
C1 C5 C7 C8 -0.3(3) . . . . ?
C1 C5 C3 F2 -101.1(2) . . . . ?
C1 C5 C3 F1 140.1(2) . . . . ?
C1 C5 C3 F3 19.8(3) . . . . ?
C1 C4 C2 F6 -179.7(2) . . . . ?
C1 C4 C2 F5 -59.9(3) . . . . ?
C1 C4 C2 F4 57.6(3) . . . . ?
C10 N2 C9 O1 -12.1(3) . . . . ?
C10 N2 C9 N1 168.60(16) . . . . ?
C16 C18 C17 C15 -0.7(3) . . . . ?
C16 C14 C11 C15 -0.8(3) . . . . ?
C16 C14 C12 F10 -155.4(2) . . . . ?
C16 C14 C12 F11 85.8(3) . . . . ?
C16 C14 C12 F12 -35.0(3) . . . . ?
C37 N6 C41 C42 -59.8(2) . . . . ?
C37 N6 C45 C46A 66.6(3) . . . . ?
C37 N6 C45 C46B 32.2(5) . . . . ?
C37 N6 C49 C50 -178.86(18) . . . . ?
C41 N6 C37 C38 -52.8(2) . . . . ?
C41 N6 C45 C46A -172.7(2) . . . . ?
C41 N6 C45 C46B 152.9(5) . . . . ?
C41 N6 C49 C50 60.9(2) . . . . ?
C41 C42 C43 C44 -179.38(18) . . . . ?
C3 C5 C7 C8 -178.26(18) . . . . ?
C3 C5 C1 C4 178.31(18) . . . . ?
C2 C4 C1 C5 179.52(18) . . . . ?
C43 C42 C41 N6 175.39(18) . . . . ?
C11 C15 C13 F9 116.8(2) . . . . ?
C11 C15 C13 F8 -3.2(3) . . . . ?
C11 C15 C13 F7 -124.9(3) . . . . ?
C11 C14 C12 F10 27.4(3) . . . . ?
C11 C14 C12 F11 -91.4(3) . . . . ?
C11 C14 C12 F12 147.8(2) . . . . ?
C45 N6 C37 C38 65.0(2) . . . . ?
C45 N6 C41 C42 178.79(18) . . . . ?
C45 N6 C49 C50 -57.0(2) . . . . ?
C45 C46B C47B C48B -68.9(11) . . . . ?
C49 N6 C37 C38 -173.43(17) . . . . ?
C49 N6 C41 C42 57.7(2) . . . . ?
C49 N6 C45 C46A -51.8(3) . . . . ?
C49 N6 C45 C46B -86.2(5) . . . . ?
C49 C50 C51A C52A 178.2(3) . . . . ?
C49 C50 C51B C52B -62.2(13) . . . . ?
C12 C14 C11 C15 176.3(2) . . . . ?
C13 C15 C11 C14 -179.8(2) . . . . ?
C36 C35 C34 C33 173.68(19) . . . . ?
C40 C39 C38 C37 -167.14(18) . . . . ?
C51A C50 C51B C52B -16.5(10) . . . . ?
C46A C45 C46B C47B 81.6(8) . . . . ?
C48A C47A C46A C45 59.6(4) . . . . ?
C46B C45 C46A C47A -77.4(7) . . . . ?
C51B C50 C51A C52A 36.0(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.574
_oxdiff_exptl_absorpt_empirical_full_min 0.820
####################################################################### 
# 
# 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_compound_7
_database_code_depnum_ccdc_archive 'CCDC 1489610'
_audit_update_record             
;
2016-08-17 deposited with the CCDC.
2016-08-25 downloaded from the CCDC.
;
_audit_creation_date             2016-08-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C10 H7 F6 N2 O3 S2, C16 H36 N, H2 O'
_chemical_formula_sum            'C26 H43 F6 N3 O4 S2'
_chemical_formula_weight         639.75
_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'
F F 0.0727 0.0534 '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                   12.1225(5)
_cell_length_b                   13.1483(4)
_cell_length_c                   21.4144(11)
_cell_angle_alpha                74.424(4)
_cell_angle_beta                 87.100(4)
_cell_angle_gamma                84.476(3)
_cell_volume                     3271.5(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7166
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.4770
_cell_measurement_theta_min      3.4970
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.082
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.299
_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 0 0 0.0499
1 0 0 0.0499
0 -5 -1 0.1356
0 5 1 0.1356
1 0 5 0.0018
-1 0 -5 0.0018

_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.004
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21742
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         3.503
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -114.00 -16.00   1.00    7.50    --  -40.37 -38.00  30.00   98
  2  ω    -72.00  19.00   1.00    7.50    --  -40.37  77.00-180.00   91
  3  ω   -114.00 -23.00   1.00    7.50    --  -40.37 -38.00 -60.00   91
  4  ω      2.00  80.00   1.00    7.50    --   40.37 -99.00 -90.00   78
  5  ω     23.00  77.00   1.00    7.50    --   40.37-125.00 120.00   54
  6  ω     84.00 120.00   1.00   30.00    --  105.19  45.00  90.00   36
  7  ω     90.00 174.00   1.00   30.00    --  105.19  45.00 -90.00   84
  8  ω     71.00 105.00   1.00   30.00    --  105.19 -94.00 -60.00   34
  9  ω     35.00 112.00   1.00   30.00    --  105.19 -61.00 -30.00   77
 10  ω     37.00 130.00   1.00   30.00    --  105.19 -61.00-150.00   93
 11  ω     33.00 130.00   1.00   30.00    --  105.19 -30.00  90.00   97
 12  ω     81.00 116.00   1.00   30.00    --  105.19-111.00-150.00   35
 13  ω    145.00 170.00   1.00   30.00    --  105.19  45.00  90.00   25
 14  ω     79.00 116.00   1.00   30.00    --  105.19-111.00  60.00   37
 15  ω     31.00 135.00   1.00   30.00    --  105.19 -77.00  90.00  104
 16  ω     36.00  63.00   1.00   30.00    --  105.19 -94.00 -60.00   27
 17  ω     26.00 141.00   1.00   30.00    --  105.19 -15.00 -90.00  115
;
_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                8722
_reflns_number_total             11568
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         1.772
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     896
_refine_ls_number_reflns         11568
_refine_ls_number_restraints     898
_refine_ls_R_factor_all          0.1342
_refine_ls_R_factor_gt           0.1110
_refine_ls_restrained_S_all      1.246
_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)+(0.1841P)²+9.5549P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3006
_refine_ls_wR_factor_ref         0.3293
_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,
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C14B-C12B
 1.54 with sigma of 0.02
 F12B-C12B
 1.3 with sigma of 0.02
 C12B-F11B
 1.3 with sigma of 0.02
 C12B-F10B
 1.3 with sigma of 0.02
 F12B-F11B
 2 with sigma of 0.02
 F12B-F10B
 2 with sigma of 0.02
 F10B-F11B
 2 with sigma of 0.02
 F7B-F8B
 2 with sigma of 0.02
 F8B-F9B
 2 with sigma of 0.02
 F9B-F7B
 2 with sigma of 0.02
 F12A-F10A \\sim F10A-F11A \\sim F11A-F12A \\sim F8A-F9A \\sim F9A-F7A \\sim
F7A-F8A
 with sigma of 0.002
 C17A-C13A \\sim C17A-C16A
 with sigma of 0.02
 F12A-C12A \\sim F11A-C12A \\sim F10A-C12A \\sim F8A-C11A \\sim F7A-C11A \\sim
F9A-C11A \\sim F3-C2 ~
 F1-C2 \\sim F2-C2 \\sim F6-C3 \\sim F5-C3 \\sim F4-C3
 with sigma of 0.02
 C12A-C14A \\sim C16A-C11A \\sim C3-C5 \\sim C2-C4
 with sigma of 0.02
 C32-C31 \\sim C24-C23 \\sim C48_$1-C47_$1 \\sim C44_$1-C43_$1 \\sim
C51_$1-C52_$1
 with sigma of 0.02
 C31-C30 \\sim C46_$1-C47_$1 \\sim C39_$1-C38_$1 \\sim C51_$1-C50_$1 \\sim
C43_$1-C42_$1
 with sigma of 0.02
 C36-C35 \\sim C36A-C35A
 with sigma of 0.02
 C35-C34 \\sim C35A-C34
 with sigma of 0.02
3. Restrained planarity
 C13A, C14A, C12A, C15A
 with sigma of 0.1
 C17A, C16A, C15A, C11A
 with sigma of 0.1
 C13B, C14B, C12B, C15B
 with sigma of 0.1
 C17B, C16B, C15B, C11B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C14B) \\sim Ueq, Uanis(C12B) \\sim Ueq, Uanis(F12B) \\sim Ueq,
Uanis(F11B) \\sim Ueq, Uanis(F10B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.1
Uanis(C14A) \\sim Ueq, Uanis(C12A) \\sim Ueq, Uanis(F10A) \\sim Ueq,
Uanis(F12A) \\sim Ueq, Uanis(F11A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.1
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(H26C)=Sof(H26D)=Sof(C27B)=Sof(H27C)=Sof(H27D)=Sof(C28B)=Sof(H28D)=
 Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H26A)=Sof(H26B)=Sof(C28A)=Sof(H28A)=
 Sof(H28B)=Sof(H28C)=FVAR(1)
 Sof(H34C)=Sof(H34D)=Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C36A)=Sof(H36D)=
 Sof(H36E)=Sof(H36F)=1-FVAR(2)
 Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=FVAR(2)
 Sof(H3B)=Sof(C14B)=Sof(C13B)=Sof(H13B)=Sof(C18B)=Sof(C17B)=Sof(H17B)=
 Sof(C16B)=Sof(C15B)=Sof(H15B)=Sof(C11B)=Sof(F7B)=Sof(F9B)=Sof(F8B)=Sof(F10B)=
 Sof(F12B)=Sof(F11B)=Sof(C12B)=1-FVAR(3)
 Sof(H3A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(C11A)=Sof(C18A)=Sof(C13A)=Sof(H13A)=
 Sof(C14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(C17A)=Sof(H17A)=Sof(F11A)=
 Sof(F12A)=Sof(F10A)=Sof(C12A)=FVAR(3)
7.a Free rotating group:
 O8(H8A,H8B), O7(H7A,H7B)
7.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C45(H45A,H45B), C41(H41A,H41B), C49(H49A,H49B), C20(H20A,
 H20B), C42(H42A,H42B), C29(H29A,H29B), C50(H50A,H50B), C47(H47A,H47B),
 C37(H37A,H37B), C46(H46A,H46B), C30(H30A,H30B), C31(H31A,H31B), C21(H21A,H21B),
  C51(H51A,H51B), C43(H43A,H43B), C22(H22A,H22B), C38(H38A,H38B), C39(H39A,
 H39B), C23(H23A,H23B), C33(H33A,H33B), C34(H34A,H34B), C34(H34C,H34D),
 C35(H35A,H35B), C27A(H27A,H27B), C26(H26A,H26B), C26(H26C,H26D), C25(H25A,
 H25B), C27B(H27C,H27D), C35A(H35C,H35D)
7.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), N2(H2), N3(H3A), N3(H3B), C6(H6), C7(H7), C1(H1A), C13A(H13A),
  C15A(H15A), C17A(H17A), C13B(H13B), C17B(H17B), C15B(H15B)
7.d Fitted hexagon refined as free rotating group:
 C18A(C13A,C14A,C15A,C16A,C17A), C14B(C13B,C18B,C17B,C16B,C15B)
7.e Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C48(H48A,H48B,H48C), C32(H32A,H32B,H32C), C44(H44A,H44B,
 H44C), C24(H24A,H24B,H24C), C40(H40A,H40B,H40C), C36(H36A,H36B,H36C),
 C28A(H28A,H28B,H28C), C28B(H28D,H28E,H28F), C36A(H36D,H36E,H36F)
;
_atom_sites_solution_hydrogens   mixed
_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
S001 S 0.28982(10) 1.38723(9) 0.36530(6) 0.0370(3) Uani 1 1 d . U . . .
S1 S 0.07237(11) 1.82386(10) 0.26184(7) 0.0425(3) Uani 1 1 d . U . . .
S2 S 0.38574(12) 1.77182(12) 0.33471(7) 0.0478(4) Uani 1 1 d . U . . .
S3 S 0.40352(17) 1.45834(13) 0.17607(8) 0.0648(5) Uani 1 1 d . U . . .
O5 O 0.2724(3) 1.4627(3) 0.40448(17) 0.0394(7) Uani 1 1 d . U . . .
O4 O 0.2071(3) 1.4065(3) 0.31544(18) 0.0383(7) Uani 1 1 d . U . . .
O3 O 0.4470(3) 1.6683(4) 0.3542(2) 0.0531(8) Uani 1 1 d . U . . .
O1 O 0.3752(4) 1.8096(3) 0.26503(19) 0.0508(9) Uani 1 1 d . U . . .
O6 O 0.3010(3) 1.2783(3) 0.4041(2) 0.0494(9) Uani 1 1 d . U . . .
N1 N 0.1089(4) 1.6160(3) 0.2723(2) 0.0375(8) Uani 1 1 d . U . . .
H1 H 0.1443 1.5546 0.2911 0.045 Uiso 1 1 calc R . . . .
N6 N -0.2255(3) 0.7340(3) 0.3903(2) 0.0354(7) Uani 1 1 d . U . . .
N4 N 0.4204(4) 1.5179(4) 0.2840(2) 0.0449(9) Uani 1 1 d . U . . .
H4 H 0.4289 1.5682 0.3030 0.054 Uiso 1 1 calc R . . . .
N2 N 0.2006(3) 1.6746(3) 0.3430(2) 0.0347(8) Uani 1 1 d . U . . .
H2 H 0.2180 1.6070 0.3614 0.042 Uiso 1 1 calc R . . . .
O2 O 0.4264(4) 1.8482(4) 0.3639(2) 0.0686(12) Uani 1 1 d . U . . .
N3 N 0.3964(4) 1.6536(4) 0.1937(2) 0.0483(10) Uani 1 1 d . U . . .
H3A H 0.3985 1.6925 0.2212 0.058 Uiso 0.607(9) 1 calc R . P A 1
H3B H 0.3834 1.6882 0.2236 0.058 Uiso 0.393(9) 1 calc R . P A 2
O8 O 0.4833(4) 1.1302(4) 0.4257(3) 0.0703(13) Uani 1 1 d . U . . .
H8A H 0.4488 1.0753 0.4300 0.105 Uiso 1 1 d G . . . .
H8B H 0.4378 1.1852 0.4158 0.105 Uiso 1 1 d G . . . .
F7A F 0.1764(8) 1.9888(9) 0.0659(5) 0.096(3) Uani 0.607(9) 1 d D U P A 1
O7 O 0.6043(5) 1.0643(5) 0.5359(3) 0.0751(14) Uani 1 1 d . U . . .
H7A H 0.5410 1.0858 0.5197 0.113 Uiso 1 1 d G . . . .
H7B H 0.6545 1.0843 0.5072 0.113 Uiso 1 1 d G . . . .
N5 N 0.1720(5) 1.1748(4) 0.2277(2) 0.0561(9) Uani 1 1 d . U . . .
C9 C 0.1307(4) 1.7006(4) 0.2929(2) 0.0328(8) Uani 1 1 d . U . . .
C10 C 0.2483(5) 1.7517(4) 0.3679(3) 0.0432(10) Uani 1 1 d . U . . .
H10A H 0.2508 1.7267 0.4158 0.052 Uiso 1 1 calc R . . . .
H10B H 0.2014 1.8197 0.3565 0.052 Uiso 1 1 calc R . . . .
C45 C -0.1086(4) 0.7015(4) 0.4163(2) 0.0357(9) Uani 1 1 d . U . . .
H45A H -0.0824 0.6327 0.4077 0.043 Uiso 1 1 calc R . . . .
H45B H -0.0587 0.7546 0.3918 0.043 Uiso 1 1 calc R . . . .
C41 C -0.2706(4) 0.8390(4) 0.4027(3) 0.0382(9) Uani 1 1 d . U . . .
H41A H -0.3471 0.8556 0.3866 0.046 Uiso 1 1 calc R . . . .
H41B H -0.2750 0.8297 0.4501 0.046 Uiso 1 1 calc R . . . .
C8 C 0.0344(4) 1.6174(4) 0.2231(3) 0.0410(10) Uani 1 1 d . U . . .
C49 C -0.3069(4) 0.6540(4) 0.4236(3) 0.0373(9) Uani 1 1 d . U . . .
H49A H -0.3128 0.6529 0.4700 0.045 Uiso 1 1 calc R . . . .
H49B H -0.3807 0.6797 0.4049 0.045 Uiso 1 1 calc R . . . .
C20 C 0.4217(5) 1.4118(5) 0.3234(3) 0.0477(11) Uani 1 1 d . U . . .
H20A H 0.4809 1.3987 0.3555 0.057 Uiso 1 1 calc R . . . .
H20B H 0.4384 1.3622 0.2959 0.057 Uiso 1 1 calc R . . . .
C42 C -0.2055(5) 0.9336(4) 0.3723(3) 0.0470(12) Uani 1 1 d D U . . .
H42A H -0.2042 0.9479 0.3245 0.056 Uiso 1 1 calc R . . . .
H42B H -0.1281 0.9189 0.3871 0.056 Uiso 1 1 calc R . . . .
C29 C 0.1367(5) 1.1628(4) 0.2983(3) 0.0463(11) Uani 1 1 d . U . . .
H29A H 0.1817 1.2069 0.3161 0.056 Uiso 1 1 calc R . . . .
H29B H 0.0584 1.1916 0.2998 0.056 Uiso 1 1 calc R . . . .
C50 C -0.2805(4) 0.5416(4) 0.4192(3) 0.0437(11) Uani 1 1 d D U . . .
H50A H -0.2077 0.5135 0.4385 0.052 Uiso 1 1 calc R . . . .
H50B H -0.2761 0.5403 0.3731 0.052 Uiso 1 1 calc R . . . .
C47 C 0.0178(4) 0.6552(4) 0.5102(3) 0.0409(11) Uani 1 1 d D U . . .
H47A H 0.0404 0.5857 0.5017 0.049 Uiso 1 1 calc R . . . .
H47B H 0.0688 0.7066 0.4849 0.049 Uiso 1 1 calc R . . . .
F4 F -0.1010(6) 1.7637(5) 0.0116(3) 0.1235(18) Uani 1 1 d D U . . .
C6 C -0.0409(5) 1.5419(5) 0.2362(3) 0.0510(13) Uani 1 1 d . U . . .
H6 H -0.0422 1.4915 0.2773 0.061 Uiso 1 1 calc R . . . .
C19 C 0.4068(5) 1.5458(4) 0.2192(3) 0.0451(10) Uani 1 1 d . U . . .
C37 C -0.2135(4) 0.7441(5) 0.3178(3) 0.0417(10) Uani 1 1 d . U . . .
H37A H -0.1548 0.7920 0.2998 0.050 Uiso 1 1 calc R . . . .
H37B H -0.1875 0.6735 0.3118 0.050 Uiso 1 1 calc R . . . .
C46 C -0.0986(4) 0.6910(5) 0.4875(3) 0.0468(12) Uani 1 1 d D U . . .
H46A H -0.1495 0.6393 0.5123 0.056 Uiso 1 1 calc R . . . .
H46B H -0.1215 0.7602 0.4963 0.056 Uiso 1 1 calc R . . . .
C52 C -0.3493(5) 0.3589(5) 0.4516(3) 0.0518(13) Uani 1 1 d D U . . .
H52A H -0.3482 0.3565 0.4062 0.078 Uiso 1 1 calc GR . . . .
H52B H -0.4088 0.3181 0.4756 0.078 Uiso 1 1 calc GR . . . .
H52C H -0.2779 0.3283 0.4709 0.078 Uiso 1 1 calc GR . . . .
F8A F 0.2944(9) 2.0544(7) -0.0122(3) 0.094(2) Uani 0.607(9) 1 d D U P A 1
C30 C 0.1472(5) 1.0513(4) 0.3423(3) 0.0457(12) Uani 1 1 d D U . . .
H30A H 0.2231 1.0182 0.3382 0.055 Uiso 1 1 calc R . . . .
H30B H 0.0944 1.0082 0.3293 0.055 Uiso 1 1 calc R . . . .
C7 C 0.0408(5) 1.6892(5) 0.1624(3) 0.0508(12) Uani 1 1 d . U . . .
H7 H 0.0955 1.7387 0.1529 0.061 Uiso 1 1 calc R . . . .
F5 F -0.0373(7) 1.8661(5) 0.0551(3) 0.1244(17) Uani 1 1 d D U . . .
C31 C 0.1229(6) 1.0540(5) 0.4119(3) 0.0508(13) Uani 1 1 d D U . . .
H31A H 0.0517 1.0968 0.4143 0.061 Uiso 1 1 calc R . . . .
H31B H 0.1819 1.0889 0.4264 0.061 Uiso 1 1 calc R . . . .
C21 C 0.1564(6) 1.2933(5) 0.1947(3) 0.0550(13) Uani 1 1 d . U . . .
H21A H 0.0782 1.3181 0.2018 0.066 Uiso 1 1 calc R . . . .
H21B H 0.2030 1.3299 0.2169 0.066 Uiso 1 1 calc R . . . .
C51 C -0.3694(4) 0.4722(4) 0.4548(3) 0.0450(11) Uani 1 1 d D U . . .
H51A H -0.3729 0.4737 0.5009 0.054 Uiso 1 1 calc R . . . .
H51B H -0.4422 0.5020 0.4359 0.054 Uiso 1 1 calc R . . . .
C48 C 0.0285(5) 0.6457(6) 0.5810(3) 0.0575(15) Uani 1 1 d D U . . .
H48A H 0.0000 0.7125 0.5904 0.086 Uiso 1 1 calc GR . . . .
H48B H 0.1067 0.6301 0.5925 0.086 Uiso 1 1 calc GR . . . .
H48C H -0.0141 0.5883 0.6065 0.086 Uiso 1 1 calc GR . . . .
F1 F -0.2764(6) 1.4818(6) 0.2475(4) 0.1323(18) Uani 1 1 d D U . . .
F3 F -0.1572(6) 1.3645(6) 0.2390(4) 0.1394(19) Uani 1 1 d D U . . .
F9A F 0.3332(7) 2.0392(6) 0.0889(4) 0.094(2) Uani 0.607(9) 1 d D U P A 1
C32 C 0.1160(6) 0.9437(5) 0.4573(3) 0.0552(14) Uani 1 1 d D U . . .
H32A H 0.0624 0.9065 0.4410 0.083 Uiso 1 1 calc GR . . . .
H32B H 0.0921 0.9495 0.5007 0.083 Uiso 1 1 calc GR . . . .
H32C H 0.1891 0.9041 0.4595 0.083 Uiso 1 1 calc GR . . . .
F6 F 0.0781(7) 1.7706(6) 0.0253(3) 0.1362(18) Uani 1 1 d D U . . .
C4 C -0.1151(8) 1.5395(8) 0.1892(4) 0.0843(19) Uani 1 1 d D U . . .
C43 C -0.2606(6) 1.0295(5) 0.3924(4) 0.0585(15) Uani 1 1 d D U . . .
H43A H -0.3403 1.0381 0.3824 0.070 Uiso 1 1 calc R . . . .
H43B H -0.2546 1.0173 0.4398 0.070 Uiso 1 1 calc R . . . .
C5 C -0.0340(7) 1.6874(7) 0.1160(4) 0.0778(18) Uani 1 1 d D U . . .
C11A C 0.2842(12) 1.9937(11) 0.0481(6) 0.084(2) Uani 0.607(9) 1 d D U P A 1
C1 C -0.1125(7) 1.6142(7) 0.1293(4) 0.0738(19) Uani 1 1 d . U . . .
H1A H -0.1646 1.6149 0.0975 0.089 Uiso 1 1 calc R . . . .
F2 F -0.2541(7) 1.4539(7) 0.1574(3) 0.147(2) Uani 1 1 d D U . . .
C22 C 0.1832(9) 1.3282(6) 0.1228(3) 0.076(2) Uani 1 1 d . U . . .
H22A H 0.1476 1.2839 0.1003 0.091 Uiso 1 1 calc R . . . .
H22B H 0.2643 1.3192 0.1153 0.091 Uiso 1 1 calc R . . . .
C38 C -0.3150(6) 0.7844(8) 0.2786(3) 0.077(2) Uani 1 1 d D U . . .
H38A H -0.3445 0.8535 0.2855 0.093 Uiso 1 1 calc R . . . .
H38B H -0.3726 0.7341 0.2932 0.093 Uiso 1 1 calc R . . . .
C39 C -0.2888(7) 0.7974(8) 0.2074(3) 0.079(2) Uani 1 1 d D U . . .
H39A H -0.2251 0.8410 0.1948 0.095 Uiso 1 1 calc R . . . .
H39B H -0.2655 0.7267 0.2008 0.095 Uiso 1 1 calc R . . . .
C2 C -0.1979(8) 1.4595(9) 0.2050(5) 0.1166(17) Uani 1 1 d D U . . .
C23 C 0.1415(10) 1.4439(6) 0.0959(4) 0.088(3) Uani 1 1 d D U . . .
H23A H 0.0595 1.4506 0.0991 0.106 Uiso 1 1 calc R . . . .
H23B H 0.1690 1.4861 0.1229 0.106 Uiso 1 1 calc R . . . .
C33 C 0.1049(8) 1.1123(6) 0.1958(4) 0.0730(14) Uani 1 1 d . U . . .
H33A H 0.1375 1.1156 0.1520 0.088 Uiso 1 1 calc R . . . .
H33B H 0.1123 1.0371 0.2212 0.088 Uiso 1 1 calc R . . . .
C18A C 0.3822(14) 1.7101(9) 0.1261(4) 0.043(3) Uani 0.607(9) 1 d . U P A 1
C13A C 0.4221(12) 1.6756(6) 0.0726(4) 0.081(5) Uani 0.607(9) 1 d DG U P A 1
H13A H 0.4529 1.6046 0.0782 0.097 Uiso 0.607(9) 1 calc R . P A 1
C14A C 0.4169(12) 1.7450(9) 0.0109(4) 0.089(3) Uani 0.607(9) 1 d DG U P A 1
C15A C 0.3718(15) 1.8489(9) 0.0027(6) 0.074(5) Uani 0.607(9) 1 d G U P A 1
H15A H 0.3682 1.8964 -0.0394 0.089 Uiso 0.607(9) 1 calc R . P A 1
C16A C 0.3319(16) 1.8833(8) 0.0562(8) 0.068(2) Uani 0.607(9) 1 d DG U P A 1
C17A C 0.3371(15) 1.8139(10) 0.1179(6) 0.041(4) Uani 0.607(9) 1 d DG U P A 1
H17A H 0.3099 1.8375 0.1545 0.049 Uiso 0.607(9) 1 calc R . P A 1
C44 C -0.2078(8) 1.1304(6) 0.3578(5) 0.086(3) Uani 1 1 d D U . . .
H44A H -0.2154 1.1437 0.3109 0.129 Uiso 1 1 calc GR . . . .
H44B H -0.1291 1.1224 0.3680 0.129 Uiso 1 1 calc GR . . . .
H44C H -0.2449 1.1900 0.3722 0.129 Uiso 1 1 calc GR . . . .
C3 C -0.0254(9) 1.7641(8) 0.0512(4) 0.1110(16) Uani 1 1 d D U . . .
C34 C -0.0158(9) 1.1486(8) 0.1892(5) 0.092(2) Uani 1 1 d D U . . .
H34A H -0.0269 1.2246 0.1656 0.111 Uiso 0.709(14) 1 calc R . P B 1
H34B H -0.0538 1.1375 0.2323 0.111 Uiso 0.709(14) 1 calc R . P B 1
H34C H -0.0207 1.2116 0.1514 0.111 Uiso 0.291(14) 1 calc R . P B 2
H34D H -0.0372 1.1749 0.2278 0.111 Uiso 0.291(14) 1 calc R . P B 2
C24 C 0.1778(13) 1.4896(8) 0.0258(4) 0.125(5) Uani 1 1 d D U . . .
H24A H 0.1395 1.4574 -0.0023 0.187 Uiso 1 1 calc GR . . . .
H24B H 0.2580 1.4744 0.0211 0.187 Uiso 1 1 calc GR . . . .
H24C H 0.1592 1.5664 0.0135 0.187 Uiso 1 1 calc GR . . . .
C35 C -0.0589(12) 1.0776(10) 0.1499(5) 0.083(3) Uani 0.709(14) 1 d D U P B 1
H35A H -0.0199 1.0888 0.1071 0.099 Uiso 0.709(14) 1 calc R . P B 1
H35B H -0.0464 1.0018 0.1736 0.099 Uiso 0.709(14) 1 calc R . P B 1
C40 C -0.3800(9) 0.8463(14) 0.1638(5) 0.142(5) Uani 1 1 d . U . . .
H40A H -0.3936 0.7998 0.1366 0.212 Uiso 1 1 calc GR . . . .
H40B H -0.3601 0.9148 0.1361 0.212 Uiso 1 1 calc GR . . . .
H40C H -0.4472 0.8571 0.1895 0.212 Uiso 1 1 calc GR . . . .
C36 C -0.1799(14) 1.1093(14) 0.1415(8) 0.111(4) Uani 0.709(14) 1 d D U P B 1
H36A H -0.1909 1.1843 0.1178 0.166 Uiso 0.709(14) 1 calc GR . P B 1
H36B H -0.2172 1.0984 0.1842 0.166 Uiso 0.709(14) 1 calc GR . P B 1
H36C H -0.2112 1.0661 0.1171 0.166 Uiso 0.709(14) 1 calc GR . P B 1
F11A F 0.5432(9) 1.7762(7) -0.0790(4) 0.109(3) Uani 0.607(9) 1 d D U P A 1
F12A F 0.5308(9) 1.6100(6) -0.0258(4) 0.111(3) Uani 0.607(9) 1 d D U P A 1
F10A F 0.3890(8) 1.7022(9) -0.0799(5) 0.129(3) Uani 0.607(9) 1 d D U P A 1
C12A C 0.4730(11) 1.7070(10) -0.0432(7) 0.107(2) Uani 0.607(9) 1 d D U P A 1
C27A C 0.5062(17) 1.1531(13) 0.2501(7) 0.066(3) Uani 0.503(15) 1 d . U P C 1
H27A H 0.5317 1.2015 0.2091 0.079 Uiso 0.503(15) 1 calc R . P C 1
H27B H 0.5407 1.1705 0.2864 0.079 Uiso 0.503(15) 1 calc R . P C 1
C26 C 0.3743(7) 1.1706(6) 0.2571(4) 0.0710(15) Uani 1 1 d . U . . .
H26A H 0.3562 1.1427 0.3038 0.085 Uiso 0.503(15) 1 calc R . P C 1
H26B H 0.3563 1.2483 0.2469 0.085 Uiso 0.503(15) 1 calc R . P C 1
H26C H 0.3590 1.1528 0.3045 0.085 Uiso 0.497(15) 1 calc R . P C 2
H26D H 0.3794 1.2479 0.2400 0.085 Uiso 0.497(15) 1 calc R . P C 2
C28A C 0.5408(15) 1.0452(12) 0.2502(9) 0.076(4) Uani 0.503(15) 1 d . U P C 1
H28A H 0.5040 1.0269 0.2155 0.114 Uiso 0.503(15) 1 calc GR . P C 1
H28B H 0.5206 0.9977 0.2921 0.114 Uiso 0.503(15) 1 calc GR . P C 1
H28C H 0.6213 1.0374 0.2432 0.114 Uiso 0.503(15) 1 calc GR . P C 1
C25 C 0.2933(7) 1.1306(5) 0.2224(3) 0.0661(13) Uani 1 1 d . U . . .
H25A H 0.2972 1.0525 0.2390 0.079 Uiso 1 1 calc R . . . .
H25B H 0.3159 1.1471 0.1759 0.079 Uiso 1 1 calc R . . . .
C27B C 0.4799(12) 1.1036(15) 0.2383(8) 0.074(3) Uani 0.497(15) 1 d . U P C 2
H27C H 0.4809 1.0282 0.2630 0.088 Uiso 0.497(15) 1 calc R . P C 2
H27D H 0.4833 1.1086 0.1913 0.088 Uiso 0.497(15) 1 calc R . P C 2
C28B C 0.5758(19) 1.1574(16) 0.2577(10) 0.088(5) Uani 0.497(15) 1 d . U P C 2
H28D H 0.5775 1.2295 0.2294 0.133 Uiso 0.497(15) 1 calc GR . P C 2
H28E H 0.6463 1.1165 0.2532 0.133 Uiso 0.497(15) 1 calc GR . P C 2
H28F H 0.5644 1.1602 0.3029 0.133 Uiso 0.497(15) 1 calc GR . P C 2
C35A C -0.113(3) 1.079(3) 0.1814(15) 0.091(5) Uani 0.291(14) 1 d D U P B 2
H35C H -0.1121 1.0143 0.2182 0.109 Uiso 0.291(14) 1 calc R . P B 2
H35D H -0.1856 1.1201 0.1829 0.109 Uiso 0.291(14) 1 calc R . P B 2
C36A C -0.101(3) 1.048(3) 0.1198(14) 0.082(7) Uani 0.291(14) 1 d D U P B 2
H36D H -0.0777 0.9721 0.1287 0.123 Uiso 0.291(14) 1 calc GR . P B 2
H36E H -0.0458 1.0887 0.0915 0.123 Uiso 0.291(14) 1 calc GR . P B 2
H36F H -0.1727 1.0623 0.0982 0.123 Uiso 0.291(14) 1 calc GR . P B 2
C14B C 0.4500(18) 1.7450(14) 0.0200(6) 0.099(3) Uani 0.393(9) 1 d D U P A 2
C13B C 0.4560(16) 1.6827(10) 0.0837(7) 0.060(4) Uani 0.393(9) 1 d G U P A 2
H13B H 0.4973 1.6155 0.0933 0.072 Uiso 0.393(9) 1 calc R . P A 2
C18B C 0.401(2) 1.7189(15) 0.1333(6) 0.040(3) Uani 0.393(9) 1 d G U P A 2
C17B C 0.341(2) 1.8173(17) 0.1193(10) 0.041(6) Uani 0.393(9) 1 d G U P A 2
H17B H 0.3038 1.8420 0.1533 0.050 Uiso 0.393(9) 1 calc R . P A 2
C16B C 0.335(2) 1.8795(13) 0.0557(12) 0.058(3) Uani 0.393(9) 1 d G U P A 2
C15B C 0.390(2) 1.8434(15) 0.0061(8) 0.083(9) Uani 0.393(9) 1 d G U P A 2
H15B H 0.3855 1.8860 -0.0374 0.099 Uiso 0.393(9) 1 calc R . P A 2
C11B C 0.276(2) 1.983(2) 0.0424(12) 0.073(2) Uani 0.393(9) 1 d . U P A 2
F7B F 0.1844(12) 2.0052(15) 0.0783(7) 0.082(3) Uani 0.393(9) 1 d D U P A 2
F9B F 0.3314(10) 2.0576(10) 0.0540(7) 0.083(3) Uani 0.393(9) 1 d D U P A 2
F8B F 0.2428(12) 2.0223(11) -0.0163(5) 0.078(3) Uani 0.393(9) 1 d D U P A 2
F10B F 0.4831(17) 1.7605(13) -0.0945(7) 0.123(4) Uani 0.393(9) 1 d D U P A 2
F12B F 0.4471(16) 1.6139(12) -0.0413(7) 0.121(4) Uani 0.393(9) 1 d D U P A 2
F11B F 0.5919(14) 1.6861(15) -0.0249(7) 0.132(4) Uani 0.393(9) 1 d D U P A 2
C12B C 0.4897(19) 1.7014(16) -0.0361(9) 0.118(3) Uani 0.393(9) 1 d D U 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
S001 O5 1.457(4) . ?
S001 O4 1.457(4) . ?
S001 O6 1.447(4) . ?
S001 C20 1.806(6) . ?
S1 C9 1.679(5) . ?
S2 O3 1.453(5) . ?
S2 O1 1.449(4) . ?
S2 O2 1.452(4) . ?
S2 C10 1.794(6) . ?
S3 C19 1.662(6) . ?
N1 H1 0.8800 . ?
N1 C9 1.354(6) . ?
N1 C8 1.416(7) . ?
N6 C45 1.528(6) . ?
N6 C41 1.519(7) . ?
N6 C49 1.521(6) . ?
N6 C37 1.524(7) . ?
N4 H4 0.8800 . ?
N4 C20 1.422(7) . ?
N4 C19 1.352(7) . ?
N2 H2 0.8800 . ?
N2 C9 1.350(6) . ?
N2 C10 1.443(6) . ?
N3 H3A 0.8800 . ?
N3 H3B 0.8800 . ?
N3 C19 1.371(7) . ?
N3 C18A 1.449(10) . ?
N3 C18B 1.348(15) . ?
O8 H8A 0.8499 . ?
O8 H8B 0.8504 . ?
F7A C11A 1.345(13) . ?
O7 H7A 0.8495 . ?
O7 H7B 0.8512 . ?
N5 C29 1.521(7) . ?
N5 C21 1.525(8) . ?
N5 C33 1.514(9) . ?
N5 C25 1.539(10) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.503(7) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.516(7) . ?
C8 C6 1.377(8) . ?
C8 C7 1.391(8) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.508(8) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.524(7) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.512(8) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C50 C51 1.519(7) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C46 1.506(6) . ?
C47 C48 1.500(7) . ?
F4 C3 1.280(9) . ?
C6 H6 0.9500 . ?
C6 C4 1.391(9) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.496(9) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C52 C51 1.506(8) . ?
F8A C11A 1.331(12) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.514(7) . ?
C7 H7 0.9500 . ?
C7 C5 1.385(9) . ?
F5 C3 1.360(10) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.521(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.511(9) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
F1 C2 1.350(10) . ?
F3 C2 1.327(10) . ?
F9A C11A 1.369(12) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
F6 C3 1.347(10) . ?
C4 C1 1.392(11) . ?
C4 C2 1.485(10) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.518(9) . ?
C5 C1 1.383(11) . ?
C5 C3 1.487(10) . ?
C11A C16A 1.477(14) . ?
C1 H1A 0.9500 . ?
F2 C2 1.277(9) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.521(11) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.509(9) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.467(13) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.519(10) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.497(14) . ?
C18A C13A 1.3900 . ?
C18A C17A 1.3900 . ?
C13A H13A 0.9500 . ?
C13A C14A 1.3900 . ?
C14A C15A 1.3900 . ?
C14A C12A 1.490(13) . ?
C15A H15A 0.9500 . ?
C15A C16A 1.3900 . ?
C16A C17A 1.3900 . ?
C17A H17A 0.9500 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 H34C 0.9900 . ?
C34 H34D 0.9900 . ?
C34 C35 1.555(13) . ?
C34 C35A 1.60(2) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.493(18) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
F11A C12A 1.359(12) . ?
F12A C12A 1.362(12) . ?
F10A C12A 1.334(12) . ?
C27A H27A 0.9900 . ?
C27A H27B 0.9900 . ?
C27A C26 1.60(2) . ?
C27A C28A 1.44(2) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 H26C 0.9900 . ?
C26 H26D 0.9900 . ?
C26 C25 1.475(12) . ?
C26 C27B 1.580(17) . ?
C28A H28A 0.9800 . ?
C28A H28B 0.9800 . ?
C28A H28C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C27B H27C 0.9900 . ?
C27B H27D 0.9900 . ?
C27B C28B 1.55(3) . ?
C28B H28D 0.9800 . ?
C28B H28E 0.9800 . ?
C28B H28F 0.9800 . ?
C35A H35C 0.9900 . ?
C35A H35D 0.9900 . ?
C35A C36A 1.48(2) . ?
C36A H36D 0.9800 . ?
C36A H36E 0.9800 . ?
C36A H36F 0.9800 . ?
C14B C13B 1.3900 . ?
C14B C15B 1.3900 . ?
C14B C12B 1.504(16) . ?
C13B H13B 0.9500 . ?
C13B C18B 1.3900 . ?
C18B C17B 1.3900 . ?
C17B H17B 0.9500 . ?
C17B C16B 1.3900 . ?
C16B C15B 1.3900 . ?
C16B C11B 1.43(3) . ?
C15B H15B 0.9500 . ?
C11B F7B 1.37(3) . ?
C11B F9B 1.33(3) . ?
C11B F8B 1.29(3) . ?
F10B C12B 1.285(17) . ?
F12B C12B 1.339(17) . ?
F11B C12B 1.261(18) . ?

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
O5 S001 O4 111.9(2) . . ?
O5 S001 C20 105.7(3) . . ?
O4 S001 C20 106.6(3) . . ?
O6 S001 O5 112.7(2) . . ?
O6 S001 O4 113.1(2) . . ?
O6 S001 C20 106.2(3) . . ?
O3 S2 C10 105.1(3) . . ?
O1 S2 O3 112.3(3) . . ?
O1 S2 O2 113.7(3) . . ?
O1 S2 C10 106.4(3) . . ?
O2 S2 O3 112.7(3) . . ?
O2 S2 C10 105.7(3) . . ?
C9 N1 H1 117.0 . . ?
C9 N1 C8 126.0(4) . . ?
C8 N1 H1 117.0 . . ?
C41 N6 C45 110.9(4) . . ?
C41 N6 C49 106.2(4) . . ?
C41 N6 C37 110.6(4) . . ?
C49 N6 C45 112.0(4) . . ?
C49 N6 C37 112.0(4) . . ?
C37 N6 C45 105.2(4) . . ?
C20 N4 H4 118.1 . . ?
C19 N4 H4 118.1 . . ?
C19 N4 C20 123.8(5) . . ?
C9 N2 H2 118.2 . . ?
C9 N2 C10 123.6(4) . . ?
C10 N2 H2 118.2 . . ?
C19 N3 H3A 116.7 . . ?
C19 N3 H3B 112.6 . . ?
C19 N3 C18A 126.6(6) . . ?
C18A N3 H3A 116.7 . . ?
C18B N3 H3B 112.6 . . ?
C18B N3 C19 134.7(9) . . ?
H8A O8 H8B 109.5 . . ?
H7A O7 H7B 109.4 . . ?
C29 N5 C21 105.9(4) . . ?
C29 N5 C25 110.6(5) . . ?
C21 N5 C25 111.5(5) . . ?
C33 N5 C29 112.0(5) . . ?
C33 N5 C21 111.4(5) . . ?
C33 N5 C25 105.5(5) . . ?
N1 C9 S1 123.5(4) . . ?
N2 C9 S1 123.4(4) . . ?
N2 C9 N1 113.0(4) . . ?
S2 C10 H10A 109.6 . . ?
S2 C10 H10B 109.6 . . ?
N2 C10 S2 110.3(4) . . ?
N2 C10 H10A 109.6 . . ?
N2 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
N6 C45 H45A 108.5 . . ?
N6 C45 H45B 108.5 . . ?
H45A C45 H45B 107.5 . . ?
C46 C45 N6 115.0(4) . . ?
C46 C45 H45A 108.5 . . ?
C46 C45 H45B 108.5 . . ?
N6 C41 H41A 108.2 . . ?
N6 C41 H41B 108.2 . . ?
H41A C41 H41B 107.3 . . ?
C42 C41 N6 116.6(4) . . ?
C42 C41 H41A 108.1 . . ?
C42 C41 H41B 108.1 . . ?
C6 C8 N1 118.0(5) . . ?
C6 C8 C7 120.9(5) . . ?
C7 C8 N1 121.0(5) . . ?
N6 C49 H49A 108.0 . . ?
N6 C49 H49B 108.0 . . ?
H49A C49 H49B 107.3 . . ?
C50 C49 N6 117.1(4) . . ?
C50 C49 H49A 108.0 . . ?
C50 C49 H49B 108.0 . . ?
S001 C20 H20A 109.4 . . ?
S001 C20 H20B 109.4 . . ?
N4 C20 S001 111.0(4) . . ?
N4 C20 H20A 109.4 . . ?
N4 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
C41 C42 H42A 109.9 . . ?
C41 C42 H42B 109.9 . . ?
C41 C42 C43 108.7(5) . . ?
H42A C42 H42B 108.3 . . ?
C43 C42 H42A 109.9 . . ?
C43 C42 H42B 109.9 . . ?
N5 C29 H29A 108.2 . . ?
N5 C29 H29B 108.2 . . ?
H29A C29 H29B 107.4 . . ?
C30 C29 N5 116.2(4) . . ?
C30 C29 H29A 108.2 . . ?
C30 C29 H29B 108.2 . . ?
C49 C50 H50A 109.6 . . ?
C49 C50 H50B 109.6 . . ?
C49 C50 C51 110.4(5) . . ?
H50A C50 H50B 108.1 . . ?
C51 C50 H50A 109.6 . . ?
C51 C50 H50B 109.6 . . ?
H47A C47 H47B 107.9 . . ?
C46 C47 H47A 109.1 . . ?
C46 C47 H47B 109.1 . . ?
C48 C47 H47A 109.1 . . ?
C48 C47 H47B 109.1 . . ?
C48 C47 C46 112.4(5) . . ?
C8 C6 H6 119.9 . . ?
C8 C6 C4 120.1(6) . . ?
C4 C6 H6 119.9 . . ?
N4 C19 S3 123.2(4) . . ?
N4 C19 N3 112.3(5) . . ?
N3 C19 S3 124.4(5) . . ?
N6 C37 H37A 108.1 . . ?
N6 C37 H37B 108.1 . . ?
H37A C37 H37B 107.3 . . ?
C38 C37 N6 116.8(5) . . ?
C38 C37 H37A 108.1 . . ?
C38 C37 H37B 108.1 . . ?
C45 C46 C47 112.2(5) . . ?
C45 C46 H46A 109.2 . . ?
C45 C46 H46B 109.2 . . ?
C47 C46 H46A 109.2 . . ?
C47 C46 H46B 109.2 . . ?
H46A C46 H46B 107.9 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
C29 C30 H30A 109.7 . . ?
C29 C30 H30B 109.7 . . ?
C29 C30 C31 109.7(4) . . ?
H30A C30 H30B 108.2 . . ?
C31 C30 H30A 109.7 . . ?
C31 C30 H30B 109.7 . . ?
C8 C7 H7 120.6 . . ?
C5 C7 C8 118.8(6) . . ?
C5 C7 H7 120.6 . . ?
C30 C31 H31A 109.2 . . ?
C30 C31 H31B 109.2 . . ?
C30 C31 C32 112.2(5) . . ?
H31A C31 H31B 107.9 . . ?
C32 C31 H31A 109.2 . . ?
C32 C31 H31B 109.2 . . ?
N5 C21 H21A 108.0 . . ?
N5 C21 H21B 108.0 . . ?
H21A C21 H21B 107.2 . . ?
C22 C21 N5 117.3(5) . . ?
C22 C21 H21A 108.0 . . ?
C22 C21 H21B 108.0 . . ?
C50 C51 H51A 108.9 . . ?
C50 C51 H51B 108.9 . . ?
C52 C51 C50 113.3(5) . . ?
C52 C51 H51A 108.9 . . ?
C52 C51 H51B 108.9 . . ?
H51A C51 H51B 107.7 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C6 C4 C1 119.3(7) . . ?
C6 C4 C2 119.2(7) . . ?
C1 C4 C2 121.5(7) . . ?
C42 C43 H43A 109.3 . . ?
C42 C43 H43B 109.3 . . ?
H43A C43 H43B 107.9 . . ?
C44 C43 C42 111.8(6) . . ?
C44 C43 H43A 109.3 . . ?
C44 C43 H43B 109.3 . . ?
C7 C5 C3 118.2(7) . . ?
C1 C5 C7 120.7(7) . . ?
C1 C5 C3 121.1(7) . . ?
F7A C11A F9A 107.8(9) . . ?
F7A C11A C16A 106.6(12) . . ?
F8A C11A F7A 110.0(10) . . ?
F8A C11A F9A 108.5(9) . . ?
F8A C11A C16A 113.4(11) . . ?
F9A C11A C16A 110.4(12) . . ?
C4 C1 H1A 120.0 . . ?
C5 C1 C4 120.1(7) . . ?
C5 C1 H1A 120.0 . . ?
C21 C22 H22A 109.7 . . ?
C21 C22 H22B 109.7 . . ?
C21 C22 C23 109.8(6) . . ?
H22A C22 H22B 108.2 . . ?
C23 C22 H22A 109.7 . . ?
C23 C22 H22B 109.7 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 C39 110.8(6) . . ?
H38A C38 H38B 108.1 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
C38 C39 H39A 108.4 . . ?
C38 C39 H39B 108.4 . . ?
H39A C39 H39B 107.5 . . ?
C40 C39 C38 115.4(8) . . ?
C40 C39 H39A 108.4 . . ?
C40 C39 H39B 108.4 . . ?
F1 C2 C4 111.3(8) . . ?
F3 C2 F1 99.8(9) . . ?
F3 C2 C4 113.6(8) . . ?
F2 C2 F1 103.2(9) . . ?
F2 C2 F3 111.8(9) . . ?
F2 C2 C4 115.5(8) . . ?
C22 C23 H23A 108.9 . . ?
C22 C23 H23B 108.9 . . ?
H23A C23 H23B 107.7 . . ?
C24 C23 C22 113.2(8) . . ?
C24 C23 H23A 108.9 . . ?
C24 C23 H23B 108.9 . . ?
N5 C33 H33A 108.4 . . ?
N5 C33 H33B 108.4 . . ?
H33A C33 H33B 107.5 . . ?
C34 C33 N5 115.3(6) . . ?
C34 C33 H33A 108.4 . . ?
C34 C33 H33B 108.4 . . ?
C13A C18A N3 126.7(8) . . ?
C13A C18A C17A 120.0 . . ?
C17A C18A N3 112.6(8) . . ?
C18A C13A H13A 120.0 . . ?
C14A C13A C18A 120.0 . . ?
C14A C13A H13A 120.0 . . ?
C13A C14A C12A 117.1(8) . . ?
C15A C14A C13A 120.0 . . ?
C15A C14A C12A 122.5(8) . . ?
C14A C15A H15A 120.0 . . ?
C16A C15A C14A 120.0 . . ?
C16A C15A H15A 120.0 . . ?
C15A C16A C11A 120.5(11) . . ?
C15A C16A C17A 120.0 . . ?
C17A C16A C11A 119.5(11) . . ?
C18A C17A H17A 120.0 . . ?
C16A C17A C18A 120.0 . . ?
C16A C17A H17A 120.0 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
F4 C3 F5 102.2(8) . . ?
F4 C3 F6 115.3(9) . . ?
F4 C3 C5 115.5(8) . . ?
F5 C3 C5 111.8(8) . . ?
F6 C3 F5 94.4(8) . . ?
F6 C3 C5 114.6(8) . . ?
C33 C34 H34A 111.1 . . ?
C33 C34 H34B 111.1 . . ?
C33 C34 H34C 105.7 . . ?
C33 C34 H34D 105.7 . . ?
C33 C34 C35 103.3(9) . . ?
C33 C34 C35A 126.3(16) . . ?
H34A C34 H34B 109.1 . . ?
H34C C34 H34D 106.2 . . ?
C35 C34 H34A 111.1 . . ?
C35 C34 H34B 111.1 . . ?
C35A C34 H34C 105.7 . . ?
C35A C34 H34D 105.7 . . ?
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 . . ?
C34 C35 H35A 110.4 . . ?
C34 C35 H35B 110.4 . . ?
H35A C35 H35B 108.6 . . ?
C36 C35 C34 106.4(11) . . ?
C36 C35 H35A 110.4 . . ?
C36 C35 H35B 110.4 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
F11A C12A C14A 112.5(10) . . ?
F11A C12A F12A 107.3(9) . . ?
F12A C12A C14A 115.9(11) . . ?
F10A C12A C14A 103.2(11) . . ?
F10A C12A F11A 109.0(9) . . ?
F10A C12A F12A 108.8(9) . . ?
H27A C27A H27B 108.0 . . ?
C26 C27A H27A 109.5 . . ?
C26 C27A H27B 109.5 . . ?
C28A C27A H27A 109.5 . . ?
C28A C27A H27B 109.5 . . ?
C28A C27A C26 110.9(16) . . ?
C27A C26 H26A 105.9 . . ?
C27A C26 H26B 105.9 . . ?
H26A C26 H26B 106.2 . . ?
H26C C26 H26D 110.0 . . ?
C25 C26 C27A 125.8(9) . . ?
C25 C26 H26A 105.9 . . ?
C25 C26 H26B 105.9 . . ?
C25 C26 H26C 112.4 . . ?
C25 C26 H26D 112.4 . . ?
C25 C26 C27B 96.7(9) . . ?
C27B C26 H26C 112.4 . . ?
C27B C26 H26D 112.4 . . ?
C27A C28A H28A 109.5 . . ?
C27A C28A H28B 109.5 . . ?
C27A C28A H28C 109.5 . . ?
H28A C28A H28B 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
N5 C25 H25A 108.3 . . ?
N5 C25 H25B 108.3 . . ?
C26 C25 N5 115.8(6) . . ?
C26 C25 H25A 108.3 . . ?
C26 C25 H25B 108.3 . . ?
H25A C25 H25B 107.4 . . ?
C26 C27B H27C 111.3 . . ?
C26 C27B H27D 111.3 . . ?
H27C C27B H27D 109.2 . . ?
C28B C27B C26 102.2(15) . . ?
C28B C27B H27C 111.3 . . ?
C28B C27B H27D 111.3 . . ?
C27B C28B H28D 109.5 . . ?
C27B C28B H28E 109.5 . . ?
C27B C28B H28F 109.5 . . ?
H28D C28B H28E 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?
C34 C35A H35C 109.3 . . ?
C34 C35A H35D 109.3 . . ?
H35C C35A H35D 107.9 . . ?
C36A C35A C34 112(2) . . ?
C36A C35A H35C 109.3 . . ?
C36A C35A H35D 109.3 . . ?
C35A C36A H36D 109.5 . . ?
C35A C36A H36E 109.5 . . ?
C35A C36A H36F 109.5 . . ?
H36D C36A H36E 109.5 . . ?
H36D C36A H36F 109.5 . . ?
H36E C36A H36F 109.5 . . ?
C13B C14B C15B 120.0 . . ?
C13B C14B C12B 121.5(13) . . ?
C15B C14B C12B 117.6(13) . . ?
C14B C13B H13B 120.0 . . ?
C18B C13B C14B 120.0 . . ?
C18B C13B H13B 120.0 . . ?
N3 C18B C13B 119.8(13) . . ?
N3 C18B C17B 119.7(13) . . ?
C13B C18B C17B 120.0 . . ?
C18B C17B H17B 120.0 . . ?
C18B C17B C16B 120.0 . . ?
C16B C17B H17B 120.0 . . ?
C17B C16B C11B 119.3(19) . . ?
C15B C16B C17B 120.0 . . ?
C15B C16B C11B 120.6(19) . . ?
C14B C15B H15B 120.0 . . ?
C16B C15B C14B 120.0 . . ?
C16B C15B H15B 120.0 . . ?
F7B C11B C16B 123(2) . . ?
F9B C11B C16B 115(2) . . ?
F9B C11B F7B 93.4(18) . . ?
F8B C11B C16B 116(2) . . ?
F8B C11B F7B 102(2) . . ?
F8B C11B F9B 104(2) . . ?
F10B C12B C14B 120.3(17) . . ?
F10B C12B F12B 101.7(15) . . ?
F12B C12B C14B 117.8(16) . . ?
F11B C12B C14B 99.3(15) . . ?
F11B C12B F10B 105.1(16) . . ?
F11B C12B F12B 112.4(18) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O4 0.88 1.96 2.824(5) 165.5 .
N4 H4 O3 0.88 1.96 2.836(7) 173.7 .
N2 H2 O5 0.88 1.94 2.817(5) 173.4 .

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
O5 S001 C20 N4 -59.4(5) . . . . ?
O4 S001 C20 N4 59.8(5) . . . . ?
O3 S2 C10 N2 -59.3(4) . . . . ?
O1 S2 C10 N2 60.0(4) . . . . ?
O6 S001 C20 N4 -179.3(4) . . . . ?
N1 C8 C6 C4 -179.4(7) . . . . ?
N1 C8 C7 C5 -180.0(7) . . . . ?
N6 C45 C46 C47 178.1(4) . . . . ?
N6 C41 C42 C43 -177.6(5) . . . . ?
N6 C49 C50 C51 179.9(4) . . . . ?
N6 C37 C38 C39 176.0(6) . . . . ?
O2 S2 C10 N2 -178.8(4) . . . . ?
N3 C18A C13A C14A -170.0(14) . . . . ?
N3 C18A C17A C16A 171.3(12) . . . . ?
N3 C18B C17B C16B -172(2) . . . . ?
F7A C11A C16A C15A 115.0(11) . . . . ?
F7A C11A C16A C17A -65.2(13) . . . . ?
N5 C29 C30 C31 173.0(5) . . . . ?
N5 C21 C22 C23 168.8(7) . . . . ?
N5 C33 C34 C35 175.0(7) . . . . ?
N5 C33 C34 C35A -157.2(15) . . . . ?
C9 N1 C8 C6 -131.3(6) . . . . ?
C9 N1 C8 C7 51.8(8) . . . . ?
C9 N2 C10 S2 -98.0(5) . . . . ?
C10 N2 C9 S1 -11.3(7) . . . . ?
C10 N2 C9 N1 171.3(5) . . . . ?
C45 N6 C41 C42 60.0(6) . . . . ?
C45 N6 C49 C50 -58.2(6) . . . . ?
C45 N6 C37 C38 -175.0(6) . . . . ?
C41 N6 C45 C46 57.9(6) . . . . ?
C41 N6 C49 C50 -179.4(4) . . . . ?
C41 N6 C37 C38 -55.2(7) . . . . ?
C41 C42 C43 C44 -173.6(7) . . . . ?
C8 N1 C9 S1 -0.9(7) . . . . ?
C8 N1 C9 N2 176.4(5) . . . . ?
C8 C6 C4 C1 -0.3(13) . . . . ?
C8 C6 C4 C2 -178.2(8) . . . . ?
C8 C7 C5 C1 -1.1(13) . . . . ?
C8 C7 C5 C3 -179.4(8) . . . . ?
C49 N6 C45 C46 -60.6(6) . . . . ?
C49 N6 C41 C42 -178.0(5) . . . . ?
C49 N6 C37 C38 63.1(7) . . . . ?
C49 C50 C51 C52 179.1(5) . . . . ?
C20 N4 C19 S3 -6.9(8) . . . . ?
C20 N4 C19 N3 173.2(5) . . . . ?
C29 N5 C21 C22 -178.7(7) . . . . ?
C29 N5 C33 C34 65.3(8) . . . . ?
C29 N5 C25 C26 -51.8(7) . . . . ?
C29 C30 C31 C32 171.9(5) . . . . ?
C6 C8 C7 C5 3.3(10) . . . . ?
C6 C4 C1 C5 2.4(15) . . . . ?
C6 C4 C2 F1 70.7(13) . . . . ?
C6 C4 C2 F3 -41.0(14) . . . . ?
C6 C4 C2 F2 -172.0(10) . . . . ?
C19 N4 C20 S001 -100.7(6) . . . . ?
C19 N3 C18A C13A -30.0(15) . . . . ?
C19 N3 C18A C17A 159.4(7) . . . . ?
C19 N3 C18B C13B -21(2) . . . . ?
C19 N3 C18B C17B 151.0(11) . . . . ?
C37 N6 C45 C46 177.5(5) . . . . ?
C37 N6 C41 C42 -56.3(6) . . . . ?
C37 N6 C49 C50 59.7(6) . . . . ?
C37 C38 C39 C40 -174.3(10) . . . . ?
F8A C11A C16A C15A -6.2(15) . . . . ?
F8A C11A C16A C17A 173.6(10) . . . . ?
C7 C8 C6 C4 -2.6(10) . . . . ?
C7 C5 C1 C4 -1.7(15) . . . . ?
C7 C5 C3 F4 -175.5(9) . . . . ?
C7 C5 C3 F5 -59.2(12) . . . . ?
C7 C5 C3 F6 46.7(13) . . . . ?
C21 N5 C29 C30 -178.6(5) . . . . ?
C21 N5 C33 C34 -53.1(9) . . . . ?
C21 N5 C25 C26 65.8(7) . . . . ?
C21 C22 C23 C24 172.7(9) . . . . ?
C48 C47 C46 C45 179.4(5) . . . . ?
F9A C11A C16A C15A -128.1(11) . . . . ?
F9A C11A C16A C17A 51.6(14) . . . . ?
C11A C16A C17A C18A -179.7(15) . . . . ?
C1 C4 C2 F1 -107.1(11) . . . . ?
C1 C4 C2 F3 141.1(10) . . . . ?
C1 C4 C2 F2 10.1(17) . . . . ?
C1 C5 C3 F4 6.2(15) . . . . ?
C1 C5 C3 F5 122.5(10) . . . . ?
C1 C5 C3 F6 -131.6(10) . . . . ?
C2 C4 C1 C5 -179.7(10) . . . . ?
C33 N5 C29 C30 59.7(8) . . . . ?
C33 N5 C21 C22 -56.7(9) . . . . ?
C33 N5 C25 C26 -173.1(6) . . . . ?
C33 C34 C35 C36 179.9(10) . . . . ?
C33 C34 C35A C36A -65(3) . . . . ?
C18A N3 C19 S3 -0.8(11) . . . . ?
C18A N3 C19 N4 179.1(9) . . . . ?
C18A N3 C18B C13B -77(5) . . . . ?
C18A N3 C18B C17B 95(6) . . . . ?
C18A C13A C14A C15A 0.0 . . . . ?
C18A C13A C14A C12A 172.9(12) . . . . ?
C13A C18A C17A C16A 0.0 . . . . ?
C13A C14A C15A C16A 0.0 . . . . ?
C13A C14A C12A F11A -128.3(10) . . . . ?
C13A C14A C12A F12A -4.4(14) . . . . ?
C13A C14A C12A F10A 114.4(10) . . . . ?
C14A C15A C16A C11A 179.7(15) . . . . ?
C14A C15A C16A C17A 0.0 . . . . ?
C15A C14A C12A F11A 44.4(14) . . . . ?
C15A C14A C12A F12A 168.3(9) . . . . ?
C15A C14A C12A F10A -72.9(12) . . . . ?
C15A C16A C17A C18A 0.0 . . . . ?
C17A C18A C13A C14A 0.0 . . . . ?
C3 C5 C1 C4 176.5(10) . . . . ?
C35 C34 C35A C36A -10.6(18) . . . . ?
C12A C14A C15A C16A -172.5(13) . . . . ?
C27A C26 C25 N5 -169.2(8) . . . . ?
C27A C26 C27B C28B 5.3(15) . . . . ?
C28A C27A C26 C25 -44.0(16) . . . . ?
C28A C27A C26 C27B -21.1(15) . . . . ?
C25 N5 C29 C30 -57.7(7) . . . . ?
C25 N5 C21 C22 61.0(8) . . . . ?
C25 N5 C33 C34 -174.3(7) . . . . ?
C25 C26 C27B C28B 166.9(11) . . . . ?
C27B C26 C25 N5 179.2(7) . . . . ?
C35A C34 C35 C36 42(3) . . . . ?
C14B C13B C18B N3 172(2) . . . . ?
C14B C13B C18B C17B 0.0 . . . . ?
C13B C14B C15B C16B 0.0 . . . . ?
C13B C14B C12B F10B 179.9(18) . . . . ?
C13B C14B C12B F12B 55(2) . . . . ?
C13B C14B C12B F11B -66.5(19) . . . . ?
C13B C18B C17B C16B 0.0 . . . . ?
C18B N3 C19 S3 -14.2(17) . . . . ?
C18B N3 C19 N4 165.7(15) . . . . ?
C18B N3 C18A C13A 103(6) . . . . ?
C18B N3 C18A C17A -68(5) . . . . ?
C18B C17B C16B C15B 0.0 . . . . ?
C18B C17B C16B C11B -178(2) . . . . ?
C17B C16B C15B C14B 0.0 . . . . ?
C17B C16B C11B F7B -33(3) . . . . ?
C17B C16B C11B F9B 79(2) . . . . ?
C17B C16B C11B F8B -159(2) . . . . ?
C15B C14B C13B C18B 0.0 . . . . ?
C15B C14B C12B F10B 11(2) . . . . ?
C15B C14B C12B F12B -114.0(18) . . . . ?
C15B C14B C12B F11B 124.5(15) . . . . ?
C15B C16B C11B F7B 150(2) . . . . ?
C15B C16B C11B F9B -98(2) . . . . ?
C15B C16B C11B F8B 24(3) . . . . ?
C11B C16B C15B C14B 178(2) . . . . ?
C12B C14B C13B C18B -168.7(18) . . . . ?
C12B C14B C15B C16B 169.1(17) . . . . ?

_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
;
####################################################################### 
# 
# 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_Compound_9
_database_code_depnum_ccdc_archive 'CCDC 1489611'
_audit_update_record             
;
2016-07-04 deposited with the CCDC.
2016-08-25 downloaded from the CCDC.
;
#-------------------------------------------------------------------------


_audit_creation_date             2016-05-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C9 H10 F3 N2 Na O5 S'
_chemical_formula_sum            'C9 H10 F3 N2 Na O5 S'
_chemical_formula_weight         338.24
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C8 H9 N2 O5 F3 S Na'
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'
F F 0.0727 0.0534 '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'
Na Na 0.1353 0.1239 '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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   4.8741(3)
_cell_length_b                   6.3672(4)
_cell_length_c                   40.456(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1255.54(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5289
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      72.8710
_cell_measurement_theta_min      4.3580
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.277
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_correction_T_min  0.433
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             688
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 3 18 0.0422
0 -4 1 0.0566
-3 0 -14 0.2349
3 -1 14 0.2131
0 4 -2 0.0466
0 -3 21 0.0392
0 3 -20 0.0411
0 -2 -24 0.0445
0 2 24 0.0385

_exptl_crystal_size_max          0.596
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.087
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.1576 2.9969 18.0294 -0.2072 -0.8680 -0.4513
-0.1993 -4.1188 1.0506 -0.4762 0.8753 0.0840
-2.6439 0.2762 -14.3170 0.0563 -0.1059 0.9928
2.5707 -0.8837 14.2374 -0.1261 0.2342 -0.9640
0.0918 4.1206 -1.6279 0.4774 -0.8776 -0.0436
0.0082 -2.5526 20.6391 -0.8663 0.3066 -0.3943
0.1610 2.6261 -20.2205 0.8866 -0.3137 0.3399
0.0062 -1.7698 -23.7315 0.5240 0.6826 0.5095
-0.0724 1.7865 23.6738 -0.5304 -0.6911 -0.4909

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            7871
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.848
_diffrn_reflns_theta_min         2.184
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     23.00  49.00   1.00    1.00    --   40.62  77.00 -30.00   26
  2  ω     59.00 151.00   1.00    1.00    --  105.19  15.00 -30.00   92
  3  ω    103.00 163.00   1.00    1.00    --  105.19 111.00   0.00   60
  4  ω     79.00 143.00   1.00    1.00    --  105.19  45.00  90.00   64
  5  ω     59.00  86.00   1.00    1.00    --  105.19 178.00 -90.00   27
  6  ω    -62.00  30.00   1.00    1.00    --  -40.62  77.00 120.00   92
  7  ω     43.00 126.00   1.00    1.00    --  105.19 -30.00 -90.00   83
  8  ω     83.00 108.00   1.00    1.00    --  105.19 -94.00  30.00   25
  9  ω     87.00 116.00   1.00    1.00    --  105.19-111.00 150.00   29
 10  ω     45.00 131.00   1.00    1.00    --  105.19 -45.00  90.00   86
 11  ω     57.00  88.00   1.00    1.00    --   40.62-125.00 -30.00   31
 12  ω     37.00 101.00   1.00    1.00    --  105.19-111.00 -60.00   64
 13  ω     29.00 137.00   1.00    1.00    --  105.19 -77.00 -60.00  108
 14  ω     33.00  77.00   1.00    1.00    --  105.19 -94.00 120.00   44
 15  ω     31.00  56.00   1.00    1.00    --  105.19-111.00 150.00   25
 16  ω      1.00  78.00   1.00    1.00    --   40.62 -99.00-120.00   77
 17  ω   -112.00 -18.00   1.00    1.00    --  -40.62 -38.00 -30.00   94
 18  ω   -114.00 -87.00   1.00    1.00    --  -40.62 -57.00  90.00   27
;
_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      0.1493123000
_diffrn_orient_matrix_UB_12      0.1008511000
_diffrn_orient_matrix_UB_13      -0.0295605000
_diffrn_orient_matrix_UB_21      0.0840070000
_diffrn_orient_matrix_UB_22      -0.2197321000
_diffrn_orient_matrix_UB_23      -0.0123545000
_diffrn_orient_matrix_UB_31      -0.2653800000
_diffrn_orient_matrix_UB_32      -0.0127913000
_diffrn_orient_matrix_UB_33      -0.0205829000
_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         0.641
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2402
_reflns_number_total             2439
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin; batch scale factor refined to 0.34(2)
;
_refine_ls_abs_structure_Flack   0.34(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2439
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0279
_refine_ls_restrained_S_all      1.066
_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)+(0.0406P)²+0.3662P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0701
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H5A(0.033) H5B(0.033) H2(0.016) H1(0.019) H3(0.019) H4(0.018)
 H9A(0.015) H9B(0.015) H6(0.019) H7(0.019)
 Fixed X: H5A(1.1291) H5B(1.0725) H2(0.8152) H1(0.7682) H3(-0.036) H4(0.1578)
 H9A(0.6281) H9B(0.348) H6(0.7101) H7(0.5178)
 Fixed Y: H5A(0.6326) H5B(0.4205) H2(0.1372) H1(0.4059) H3(0.9127) H4(0.6376)
 H9A(-0.1747) H9B(-0.0574) H6(0.5517) H7(0.8277)
 Fixed Z: H5A(0.4452) H5B(0.4347) H2(0.391) H1(0.3598) H3(0.3466) H4(0.3761)
 H9A(0.4076) H9B(0.4122) H6(0.3032) H7(0.2742)
;
_atom_sites_solution_hydrogens   mixed
_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 0.62046(11) -0.00598(10) 0.45755(2) 0.01042(14) Uani 1 1 d . . . . .
Na1 Na 0.68756(18) 0.48986(16) 0.49054(2) 0.0129(2) Uani 1 1 d . . . . .
F1 F 0.0261(4) 1.0245(3) 0.25816(4) 0.0277(4) Uani 1 1 d . . . . .
F3 F 0.2970(4) 1.2314(3) 0.28404(4) 0.0296(4) Uani 1 1 d . . . . .
F2 F -0.1061(4) 1.1701(3) 0.30340(4) 0.0311(4) Uani 1 1 d . . . . .
O4 O 0.4868(4) 0.1883(3) 0.46802(4) 0.0144(4) Uani 1 1 d . . . . .
O3 O 0.4967(4) -0.1896(3) 0.47359(4) 0.0131(4) Uani 1 1 d . . . . .
O1 O 0.2137(4) 0.2544(3) 0.38375(4) 0.0172(4) Uani 1 1 d . . . . .
O2 O 0.9169(3) 0.0015(3) 0.46031(4) 0.0168(4) Uani 1 1 d . . . . .
O5 O 1.0273(4) 0.5201(3) 0.44896(4) 0.0223(4) Uani 1 1 d . . . . .
H5A H 1.1291 0.6326 0.4452 0.033 Uiso 1 1 d GR . . . .
H5B H 1.0725 0.4205 0.4347 0.033 Uiso 1 1 d GR . . . .
N2 N 0.6419(4) 0.1237(3) 0.39441(5) 0.0135(4) Uani 1 1 d . . . . .
H2 H 0.8152 0.1372 0.3910 0.016 Uiso 1 1 calc R . . . .
N1 N 0.5921(4) 0.4105(3) 0.36100(5) 0.0156(4) Uani 1 1 d . . . . .
H1 H 0.7682 0.4059 0.3598 0.019 Uiso 1 1 calc R . . . .
C8 C 0.4641(5) 0.2630(4) 0.38017(5) 0.0126(5) Uani 1 1 d . . . . .
C3 C 0.1145(5) 0.8409(4) 0.33807(6) 0.0156(5) Uani 1 1 d . . . . .
H3 H -0.0360 0.9127 0.3466 0.019 Uiso 1 1 calc R . . . .
C5 C 0.4570(5) 0.5694(4) 0.34303(6) 0.0138(5) Uani 1 1 d . . . . .
C2 C 0.2238(5) 0.8978(4) 0.30757(6) 0.0158(5) Uani 1 1 d . . . . .
C4 C 0.2307(5) 0.6764(4) 0.35579(6) 0.0146(5) Uani 1 1 d . . . . .
H4 H 0.1578 0.6376 0.3761 0.018 Uiso 1 1 calc R . . . .
C9 C 0.5449(5) -0.0443(4) 0.41487(5) 0.0127(5) Uani 1 1 d . . . . .
H9A H 0.6281 -0.1747 0.4076 0.015 Uiso 1 1 calc R . . . .
H9B H 0.3480 -0.0574 0.4122 0.015 Uiso 1 1 calc R . . . .
C6 C 0.5624(5) 0.6252(4) 0.31208(6) 0.0155(5) Uani 1 1 d . . . . .
H6 H 0.7101 0.5517 0.3032 0.019 Uiso 1 1 calc R . . . .
C7 C 0.4464(5) 0.7896(4) 0.29461(6) 0.0155(5) Uani 1 1 d . . . . .
H7 H 0.5178 0.8277 0.2742 0.019 Uiso 1 1 calc R . . . .
C1 C 0.1108(6) 1.0793(4) 0.28869(6) 0.0179(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 Na1 2.9787(10) 4_456 ?
S1 O4 1.4608(19) . ?
S1 O3 1.4668(18) . ?
S1 O2 1.4499(17) . ?
S1 C9 1.782(2) . ?
Na1 S1 2.9787(10) 4_556 ?
Na1 Na1 4.1832(17) 4_466 ?
Na1 Na1 3.9818(16) 4_456 ?
Na1 Na1 3.9818(16) 4_556 ?
Na1 Na1 4.1832(17) 4_566 ?
Na1 O4 2.495(2) 4_556 ?
Na1 O4 2.340(2) . ?
Na1 O3 2.3454(19) 1_565 ?
Na1 O3 2.449(2) 4_556 ?
Na1 O2 2.3868(18) 4_456 ?
Na1 O5 2.3685(19) . ?
F1 C1 1.348(3) . ?
F3 C1 1.341(3) . ?
F2 C1 1.344(3) . ?
O4 Na1 2.495(2) 4_456 ?
O3 Na1 2.3453(19) 1_545 ?
O3 Na1 2.448(2) 4_456 ?
O1 C8 1.230(3) . ?
O2 Na1 2.3869(17) 4_556 ?
O5 H5A 0.8842 . ?
O5 H5B 0.8848 . ?
N2 H2 0.8600 . ?
N2 C8 1.368(3) . ?
N2 C9 1.433(3) . ?
N1 H1 0.8600 . ?
N1 C8 1.368(3) . ?
N1 C5 1.409(3) . ?
C3 H3 0.9300 . ?
C3 C2 1.392(3) . ?
C3 C4 1.390(4) . ?
C5 C4 1.395(4) . ?
C5 C6 1.399(3) . ?
C2 C7 1.388(4) . ?
C2 C1 1.491(4) . ?
C4 H4 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C6 H6 0.9300 . ?
C6 C7 1.384(3) . ?
C7 H7 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
O4 S1 Na1 56.68(7) . 4_456 ?
O4 S1 O3 111.32(9) . . ?
O4 S1 C9 107.74(11) . . ?
O3 S1 Na1 54.86(7) . 4_456 ?
O3 S1 C9 103.56(10) . . ?
O2 S1 Na1 130.57(7) . 4_456 ?
O2 S1 O4 113.22(12) . . ?
O2 S1 O3 113.68(11) . . ?
O2 S1 C9 106.56(11) . . ?
C9 S1 Na1 122.78(9) . 4_456 ?
S1 Na1 Na1 108.93(4) 4_556 4_456 ?
S1 Na1 Na1 57.137(19) 4_556 4_556 ?
S1 Na1 Na1 104.86(4) 4_556 4_466 ?
S1 Na1 Na1 55.323(19) 4_556 4_566 ?
Na1 Na1 Na1 71.26(3) 4_466 4_566 ?
Na1 Na1 Na1 102.458(12) 4_556 4_566 ?
Na1 Na1 Na1 158.26(5) 4_456 4_566 ?
Na1 Na1 Na1 102.459(12) 4_456 4_466 ?
Na1 Na1 Na1 75.48(4) 4_456 4_556 ?
Na1 Na1 Na1 158.26(5) 4_556 4_466 ?
O4 Na1 S1 126.80(6) . 4_556 ?
O4 Na1 S1 29.29(4) 4_556 4_556 ?
O4 Na1 Na1 35.85(5) . 4_456 ?
O4 Na1 Na1 33.31(4) 4_556 4_556 ?
O4 Na1 Na1 164.74(6) . 4_566 ?
O4 Na1 Na1 72.62(6) . 4_556 ?
O4 Na1 Na1 125.29(6) 4_556 4_466 ?
O4 Na1 Na1 84.06(5) 4_556 4_566 ?
O4 Na1 Na1 118.52(5) . 4_466 ?
O4 Na1 Na1 83.10(6) 4_556 4_456 ?
O4 Na1 O4 97.65(6) . 4_556 ?
O4 Na1 O3 156.14(7) . 4_556 ?
O4 Na1 O3 115.74(7) . 1_565 ?
O4 Na1 O2 96.45(7) . 4_456 ?
O4 Na1 O5 94.73(7) . . ?
O3 Na1 S1 29.33(4) 4_556 4_556 ?
O3 Na1 S1 117.20(6) 1_565 4_556 ?
O3 Na1 Na1 28.55(4) 4_556 4_566 ?
O3 Na1 Na1 118.75(5) 1_565 4_456 ?
O3 Na1 Na1 84.71(5) 4_556 4_556 ?
O3 Na1 Na1 165.11(6) 1_565 4_556 ?
O3 Na1 Na1 131.39(6) 4_556 4_456 ?
O3 Na1 Na1 66.14(6) 1_565 4_566 ?
O3 Na1 Na1 29.93(4) 1_565 4_466 ?
O3 Na1 Na1 80.72(5) 4_556 4_466 ?
O3 Na1 O4 58.54(5) 4_556 4_556 ?
O3 Na1 O4 145.49(7) 1_565 4_556 ?
O3 Na1 O3 88.02(5) 1_565 4_556 ?
O3 Na1 O2 90.25(7) 1_565 4_456 ?
O3 Na1 O5 89.93(7) 1_565 . ?
O2 Na1 S1 78.67(5) 4_456 4_556 ?
O2 Na1 Na1 98.70(6) 4_456 4_566 ?
O2 Na1 Na1 61.27(5) 4_456 4_456 ?
O2 Na1 Na1 101.30(6) 4_456 4_556 ?
O2 Na1 Na1 60.48(5) 4_456 4_466 ?
O2 Na1 O4 76.93(6) 4_456 4_556 ?
O2 Na1 O3 80.47(6) 4_456 4_556 ?
O5 Na1 S1 90.16(5) . 4_556 ?
O5 Na1 Na1 70.02(5) . 4_566 ?
O5 Na1 Na1 76.76(5) . 4_556 ?
O5 Na1 Na1 118.22(7) . 4_466 ?
O5 Na1 Na1 128.82(7) . 4_456 ?
O5 Na1 O4 96.06(7) . 4_556 ?
O5 Na1 O3 87.05(7) . 4_556 ?
O5 Na1 O2 167.50(7) . 4_456 ?
S1 O4 Na1 94.04(9) . 4_456 ?
S1 O4 Na1 128.42(11) . . ?
Na1 O4 Na1 110.85(7) . 4_456 ?
S1 O3 Na1 131.30(11) . 1_545 ?
S1 O3 Na1 95.80(9) . 4_456 ?
Na1 O3 Na1 121.52(7) 1_545 4_456 ?
S1 O2 Na1 128.01(10) . 4_556 ?
Na1 O5 H5A 125.5 . . ?
Na1 O5 H5B 125.4 . . ?
H5A O5 H5B 109.2 . . ?
C8 N2 H2 119.4 . . ?
C8 N2 C9 121.2(2) . . ?
C9 N2 H2 119.4 . . ?
C8 N1 H1 117.6 . . ?
C8 N1 C5 124.9(2) . . ?
C5 N1 H1 117.6 . . ?
O1 C8 N2 123.4(2) . . ?
O1 C8 N1 123.3(2) . . ?
N2 C8 N1 113.3(2) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C4 C3 C2 119.8(2) . . ?
C4 C5 N1 121.9(2) . . ?
C4 C5 C6 119.8(2) . . ?
C6 C5 N1 118.2(2) . . ?
C3 C2 C1 121.0(2) . . ?
C7 C2 C3 120.3(2) . . ?
C7 C2 C1 118.7(2) . . ?
C3 C4 C5 119.9(2) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
S1 C9 H9A 109.0 . . ?
S1 C9 H9B 109.0 . . ?
N2 C9 S1 112.91(16) . . ?
N2 C9 H9A 109.0 . . ?
N2 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 C5 119.9(2) . . ?
C7 C6 H6 120.0 . . ?
C2 C7 H7 119.9 . . ?
C6 C7 C2 120.1(2) . . ?
C6 C7 H7 119.9 . . ?
F1 C1 C2 112.4(2) . . ?
F3 C1 F1 105.4(2) . . ?
F3 C1 F2 106.5(2) . . ?
F3 C1 C2 112.4(2) . . ?
F2 C1 F1 106.0(2) . . ?
F2 C1 C2 113.4(2) . . ?

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
Na1 S1 O4 Na1 120.75(14) 4_456 . . . ?
Na1 S1 O3 Na1 -142.06(15) 4_456 . . 1_545 ?
Na1 S1 O2 Na1 4.0(2) 4_456 . . 4_556 ?
Na1 S1 C9 N2 121.49(16) 4_456 . . . ?
O4 S1 O3 Na1 -5.25(10) . . . 4_456 ?
O4 S1 O3 Na1 -147.31(13) . . . 1_545 ?
O4 S1 O2 Na1 69.18(17) . . . 4_556 ?
O4 S1 C9 N2 60.2(2) . . . . ?
O3 S1 O4 Na1 5.13(10) . . . 4_456 ?
O3 S1 O4 Na1 125.89(12) . . . . ?
O3 S1 O2 Na1 -59.14(17) . . . 4_556 ?
O3 S1 C9 N2 178.20(17) . . . . ?
O2 S1 O4 Na1 -3.65(16) . . . . ?
O2 S1 O4 Na1 -124.40(9) . . . 4_456 ?
O2 S1 O3 Na1 -18.02(17) . . . 1_545 ?
O2 S1 O3 Na1 124.04(10) . . . 4_456 ?
O2 S1 C9 N2 -61.6(2) . . . . ?
N1 C5 C4 C3 176.0(2) . . . . ?
N1 C5 C6 C7 -175.8(2) . . . . ?
C8 N2 C9 S1 -108.4(2) . . . . ?
C8 N1 C5 C4 39.4(4) . . . . ?
C8 N1 C5 C6 -143.1(2) . . . . ?
C3 C2 C7 C6 -0.4(4) . . . . ?
C3 C2 C1 F1 -122.9(3) . . . . ?
C3 C2 C1 F3 118.3(3) . . . . ?
C3 C2 C1 F2 -2.6(4) . . . . ?
C5 N1 C8 O1 -0.1(4) . . . . ?
C5 N1 C8 N2 178.7(2) . . . . ?
C5 C6 C7 C2 -0.8(4) . . . . ?
C2 C3 C4 C5 0.2(4) . . . . ?
C4 C3 C2 C7 0.7(4) . . . . ?
C4 C3 C2 C1 -177.4(2) . . . . ?
C4 C5 C6 C7 1.7(4) . . . . ?
C9 S1 O4 Na1 118.04(10) . . . 4_456 ?
C9 S1 O4 Na1 -121.21(13) . . . . ?
C9 S1 O3 Na1 97.18(14) . . . 1_545 ?
C9 S1 O3 Na1 -120.75(10) . . . 4_456 ?
C9 S1 O2 Na1 -172.56(13) . . . 4_556 ?
C9 N2 C8 O1 -0.1(4) . . . . ?
C9 N2 C8 N1 -178.9(2) . . . . ?
C6 C5 C4 C3 -1.4(4) . . . . ?
C7 C2 C1 F1 58.9(3) . . . . ?
C7 C2 C1 F3 -59.9(3) . . . . ?
C7 C2 C1 F2 179.2(2) . . . . ?
C1 C2 C7 C6 177.7(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.415
_oxdiff_exptl_absorpt_empirical_full_min 0.429
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.66(2)
2 0.34(2)
####################################################################### 
# 
# 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_Compound_10
_database_code_depnum_ccdc_archive 'CCDC 1489612'
_audit_update_record             
;
2016-07-04 deposited with the CCDC.
2016-08-25 downloaded from the CCDC.
;
#-------------------------------------------------------------------------



_audit_creation_date             2016-05-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C9 H8 F3 N2 O4 S, C5 H6 N'
_chemical_formula_sum            'C14 H14 F3 N3 O4 S'
_chemical_formula_weight         377.34
_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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.1526(3)
_cell_length_b                   12.9487(5)
_cell_length_c                   13.3592(6)
_cell_angle_alpha                93.444(4)
_cell_angle_beta                 97.949(3)
_cell_angle_gamma                92.527(3)
_cell_volume                     1563.01(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7877
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      72.8510
_cell_measurement_theta_min      3.4090
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.423
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             776
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 5 1 0.0662
0 -5 -1 0.0662
-5 0 2 0.1473
5 0 -2 0.1473
0 0 -1 0.0705
0 0 1 0.0705

_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.132
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0009 4.9974 0.9929 0.0964 0.5797 0.1819
0.0009 -4.9974 -0.9929 -0.0964 -0.5797 -0.1819
-4.9949 0.0056 2.0024 0.0337 0.2428 -0.8130
4.9949 -0.0056 -2.0024 -0.0337 -0.2428 0.8130
0.0002 -0.0014 -0.9988 0.1048 -0.0506 0.0055
-0.0002 0.0014 0.9988 -0.1048 0.0506 -0.0055

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10664
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.983
_diffrn_reflns_theta_min         3.348
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     19.00  94.00   1.00    1.00    --   40.62  38.00  60.00   75
  2  ω     31.00 133.00   1.00    1.00    --  105.19 -30.00 120.00  102
  3  ω     94.00 178.00   1.00    1.00    --  105.19  30.00 150.00   84
  4  ω    107.00 138.00   1.00    1.00    --  105.19 -77.00  30.00   31
  5  ω     89.00 132.00   1.00    1.00    --  105.19 -77.00  90.00   43
  6  ω     82.00 115.00   1.00    1.00    --  105.19-111.00  90.00   33
  7  ω     74.00 100.00   1.00    1.00    --  105.19 -94.00 -30.00   26
  8  ω     49.00 133.00   1.00    1.00    --  105.19 -61.00-120.00   84
  9  ω     62.00  88.00   1.00    1.00    --   40.62-141.00 -54.00   26
 10  ω     48.00  92.00   1.00    1.00    --   40.62-125.00  90.00   44
 11  ω     31.00  82.00   1.00    1.00    --  105.19 -77.00  90.00   51
 12  ω     30.00  85.00   1.00    1.00    --  105.19 -77.00  30.00   55
 13  ω     24.00 143.00   1.00    1.00    --  105.19 -15.00 -30.00  119
 14  ω     45.00 112.00   1.00    1.00    --  105.19 -30.00-150.00   67
 15  ω     48.00 104.00   1.00    1.00    --  105.19 -94.00-120.00   56
 16  ω      5.00  43.00   1.00    1.00    --   40.62 -99.00 -30.00   38
 17  ω   -114.00 -12.00   1.00    1.00    --  -40.62 -57.00-150.00  102
 18  ω   -115.00 -16.00   1.00    1.00    --  -40.62 -38.00  90.00   99
;
_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      -0.0488045000
_diffrn_orient_matrix_UB_12      0.0401399000
_diffrn_orient_matrix_UB_13      -0.1050346000
_diffrn_orient_matrix_UB_21      -0.0282354000
_diffrn_orient_matrix_UB_22      0.1059536000
_diffrn_orient_matrix_UB_23      0.0505519000
_diffrn_orient_matrix_UB_31      0.1605797000
_diffrn_orient_matrix_UB_32      0.0375346000
_diffrn_orient_matrix_UB_33      -0.0055535000
_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                5708
_reflns_number_total             6036
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         6036
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0424
_refine_ls_restrained_S_all      1.128
_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)+(0.0329P)²+2.7186P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1113
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H5(0.018) H4A(0.019) H2(0.018) H1(0.019) H6A(0.022) H9A(0.017)
 H9B(0.017) H23A(0.017) H23B(0.017) H28(0.02) H24(0.024) H6(0.023) H27(0.023)
 H10(0.028) H20(0.023) H4(0.024) H26(0.025) H7(0.026) H13(0.026) H17(0.026)
 H25(0.026) H18(0.023) H11(0.028) H14(0.025) H21(0.025) H12(0.026) H3(0.026)
 Fixed X: H5(0.8544) H4A(0.8304) H2(0.3494) H1(0.347) H6A(0.7575) H9A(0.2608)
 H9B(0.1052) H23A(0.6215) H23B(0.7846) H28(0.5415) H24(0.9498) H6(0.0166)
 H27(0.5105) H10(-0.0276) H20(0.8273) H4(0.3747) H26(0.7065) H7(-0.0471)
 H13(0.4486) H17(0.3913) H25(0.9262) H18(0.4857) H11(0.1378) H14(0.2783)
 H21(0.7351) H12(0.3791) H3(0.3099)
 Fixed Y: H5(0.5796) H4A(0.4701) H2(0.6235) H1(0.7417) H6A(0.7504) H9A(0.4693)
 H9B(0.493) H23A(0.6119) H23B(0.6521) H28(0.6662) H24(0.7541) H6(0.703)
 H27(0.5737) H10(0.9146) H20(0.4023) H4(0.8964) H26(0.5686) H7(0.8001)
 H13(0.9215) H17(0.2183) H25(0.662) H18(0.3421) H11(1.0494) H14(0.7876)
 H21(0.2756) H12(1.0511) H3(0.9918)
 Fixed Z: H5(0.6352) H4A(0.7453) H2(0.6183) H1(0.5124) H6A(0.7923) H9A(0.6602)
 H9B(0.6039) H23A(0.4946) H23B(0.4904) H28(0.7948) H24(0.9156) H6(0.3474)
 H27(0.9337) H10(0.5944) H20(0.904) H4(0.4344) H26(1.0637) H7(0.2103)
 H13(0.7615) H17(0.7752) H25(1.0556) H18(0.6811) H11(0.5726) H14(0.7774)
 H21(0.9959) H12(0.6548) H3(0.2965)
;
_atom_sites_solution_hydrogens   mixed
_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
S001 S 0.13508(6) 0.56552(4) 0.76744(4) 0.01211(13) Uani 1 1 d . . . . .
S002 S 0.66931(6) 0.76980(4) 0.58492(4) 0.01287(13) Uani 1 1 d . . . . .
O6 O 0.53036(18) 0.75707(13) 0.62605(12) 0.0175(3) Uani 1 1 d . . . . .
O5 O 0.53386(17) 0.50495(13) 0.62418(12) 0.0162(3) Uani 1 1 d . . . . .
O2 O 0.03194(17) 0.64790(12) 0.74495(12) 0.0153(3) Uani 1 1 d . . . . .
F1 F 0.0713(2) 0.90300(13) 0.06089(11) 0.0346(4) Uani 1 1 d . . . . .
F6 F 0.5485(2) 0.05521(12) 0.91803(13) 0.0381(4) Uani 1 1 d . . . . .
O8 O 0.79181(17) 0.80039(13) 0.66669(12) 0.0164(3) Uani 1 1 d . . . . .
O4 O 0.06020(18) 0.47416(13) 0.80030(12) 0.0176(3) Uani 1 1 d . . . . .
O3 O 0.26776(18) 0.60350(13) 0.83450(12) 0.0176(3) Uani 1 1 d . . . . .
O1 O 0.04135(17) 0.63968(13) 0.50579(13) 0.0180(3) Uani 1 1 d . . . . .
F5 F 0.5422(2) 0.15788(13) 1.04904(12) 0.0422(5) Uani 1 1 d . . . . .
F3 F 0.1767(2) 1.04194(14) 0.13740(13) 0.0431(5) Uani 1 1 d . . . . .
O7 O 0.6620(2) 0.83622(14) 0.50139(13) 0.0224(4) Uani 1 1 d . . . . .
F4 F 0.3522(2) 0.13349(16) 0.93572(17) 0.0494(5) Uani 1 1 d . . . . .
F2 F -0.0508(2) 1.00356(18) 0.14664(14) 0.0515(6) Uani 1 1 d . . . . .
N5 N 0.7615(2) 0.57817(15) 0.61301(15) 0.0149(4) Uani 1 1 d . . . . .
H5 H 0.8544 0.5796 0.6352 0.018 Uiso 1 1 calc R . . . .
N4 N 0.7366(2) 0.45836(15) 0.72911(15) 0.0162(4) Uani 1 1 d . . . . .
H4A H 0.8304 0.4701 0.7453 0.019 Uiso 1 1 calc R . . . .
N2 N 0.2573(2) 0.60583(15) 0.60111(14) 0.0153(4) Uani 1 1 d . . . . .
H2 H 0.3494 0.6235 0.6183 0.018 Uiso 1 1 calc R . . . .
N1 N 0.2560(2) 0.73035(16) 0.48627(15) 0.0160(4) Uani 1 1 d . . . . .
H1 H 0.3470 0.7417 0.5124 0.019 Uiso 1 1 calc R . . . .
N6 N 0.7473(2) 0.71631(16) 0.84446(15) 0.0179(4) Uani 1 1 d . . . . .
H6A H 0.7575 0.7504 0.7923 0.022 Uiso 1 1 calc R . . . .
N3 N 0.1151(2) 0.84148(17) 0.68595(16) 0.0198(4) Uani 1 1 d . . . . .
C9 C 0.1908(2) 0.52298(18) 0.64889(17) 0.0144(4) Uani 1 1 d . . . . .
H9A H 0.2608 0.4693 0.6602 0.017 Uiso 1 1 calc R . . . .
H9B H 0.1052 0.4930 0.6039 0.017 Uiso 1 1 calc R . . . .
C22 C 0.6675(2) 0.51337(17) 0.65316(17) 0.0138(4) Uani 1 1 d . . . . .
C23 C 0.7099(2) 0.64421(18) 0.53475(17) 0.0140(4) Uani 1 1 d . . . . .
H23A H 0.6215 0.6119 0.4946 0.017 Uiso 1 1 calc R . . . .
H23B H 0.7846 0.6521 0.4904 0.017 Uiso 1 1 calc R . . . .
C5 C 0.2044(3) 0.78854(19) 0.40492(17) 0.0162(5) Uani 1 1 d . . . . .
C28 C 0.6185(3) 0.66461(18) 0.84799(18) 0.0169(5) Uani 1 1 d . . . . .
H28 H 0.5415 0.6662 0.7948 0.020 Uiso 1 1 calc R . . . .
C8 C 0.1750(2) 0.65666(18) 0.52856(17) 0.0146(4) Uani 1 1 d . . . . .
C16 C 0.5543(3) 0.23314(19) 0.89375(19) 0.0201(5) Uani 1 1 d . . . . .
C19 C 0.6681(3) 0.38477(18) 0.78260(18) 0.0156(5) Uani 1 1 d . . . . .
C24 C 0.8619(3) 0.7168(2) 0.92001(19) 0.0204(5) Uani 1 1 d . . . . .
H24 H 0.9498 0.7541 0.9156 0.024 Uiso 1 1 calc R . . . .
C2 C 0.1259(3) 0.90454(19) 0.23832(18) 0.0205(5) Uani 1 1 d . . . . .
C6 C 0.0761(3) 0.76046(19) 0.33718(18) 0.0190(5) Uani 1 1 d . . . . .
H6 H 0.0166 0.7030 0.3474 0.023 Uiso 1 1 calc R . . . .
C27 C 0.6000(3) 0.60920(19) 0.93031(18) 0.0196(5) Uani 1 1 d . . . . .
H27 H 0.5105 0.5737 0.9337 0.023 Uiso 1 1 calc R . . . .
C10 C 0.0694(3) 0.9165(2) 0.62670(19) 0.0237(5) Uani 1 1 d . . . . .
H10 H -0.0276 0.9146 0.5944 0.028 Uiso 1 1 calc R . . . .
C20 C 0.7404(3) 0.36444(19) 0.87752(18) 0.0194(5) Uani 1 1 d . . . . .
H20 H 0.8273 0.4023 0.9040 0.023 Uiso 1 1 calc R . . . .
C4 C 0.2904(3) 0.8764(2) 0.38895(19) 0.0198(5) Uani 1 1 d . . . . .
H4 H 0.3747 0.8964 0.4344 0.024 Uiso 1 1 calc R . . . .
C26 C 0.7166(3) 0.6070(2) 1.00824(19) 0.0210(5) Uani 1 1 d . . . . .
H26 H 0.7065 0.5686 1.0637 0.025 Uiso 1 1 calc R . . . .
C7 C 0.0383(3) 0.8187(2) 0.25507(19) 0.0216(5) Uani 1 1 d . . . . .
H7 H -0.0471 0.8001 0.2103 0.026 Uiso 1 1 calc R . . . .
C13 C 0.3534(3) 0.9203(2) 0.72644(19) 0.0219(5) Uani 1 1 d . . . . .
H13 H 0.4486 0.9215 0.7615 0.026 Uiso 1 1 calc R . . . .
C17 C 0.4801(3) 0.25463(19) 0.80033(19) 0.0216(5) Uani 1 1 d . . . . .
H17 H 0.3913 0.2183 0.7752 0.026 Uiso 1 1 calc R . . . .
C25 C 0.8480(3) 0.6621(2) 1.00312(19) 0.0214(5) Uani 1 1 d . . . . .
H25 H 0.9262 0.6620 1.0556 0.026 Uiso 1 1 calc R . . . .
C18 C 0.5357(3) 0.32904(19) 0.74410(19) 0.0190(5) Uani 1 1 d . . . . .
H18 H 0.4857 0.3421 0.6811 0.023 Uiso 1 1 calc R . . . .
C11 C 0.1674(3) 0.9968(2) 0.6140(2) 0.0236(5) Uani 1 1 d . . . . .
H11 H 0.1378 1.0494 0.5726 0.028 Uiso 1 1 calc R . . . .
C14 C 0.2518(3) 0.84104(19) 0.73614(19) 0.0211(5) Uani 1 1 d . . . . .
H14 H 0.2783 0.7876 0.7774 0.025 Uiso 1 1 calc R . . . .
C21 C 0.6852(3) 0.28899(19) 0.93291(19) 0.0211(5) Uani 1 1 d . . . . .
H21 H 0.7351 0.2756 0.9959 0.025 Uiso 1 1 calc R . . . .
C12 C 0.3112(3) 0.9980(2) 0.66373(19) 0.0219(5) Uani 1 1 d . . . . .
H12 H 0.3791 1.0511 0.6548 0.026 Uiso 1 1 calc R . . . .
C3 C 0.2517(3) 0.9336(2) 0.30644(19) 0.0217(5) Uani 1 1 d . . . . .
H3 H 0.3099 0.9918 0.2965 0.026 Uiso 1 1 calc R . . . .
C1 C 0.0817(3) 0.9631(2) 0.14699(19) 0.0249(6) Uani 1 1 d . . . . .
C15 C 0.4993(3) 0.1459(2) 0.9488(2) 0.0250(6) Uani 1 1 d . . . . .
H3A H 0.060(3) 0.795(2) 0.693(2) 0.021(8) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
S001 O2 1.4725(16) . ?
S001 O4 1.4615(17) . ?
S001 O3 1.4535(16) . ?
S001 C9 1.793(2) . ?
S002 O6 1.4602(17) . ?
S002 O8 1.4757(16) . ?
S002 O7 1.4452(17) . ?
S002 C23 1.795(2) . ?
O5 C22 1.229(3) . ?
F1 C1 1.339(3) . ?
F6 C15 1.338(3) . ?
O1 C8 1.226(3) . ?
F5 C15 1.341(3) . ?
F3 C1 1.335(3) . ?
F4 C15 1.334(3) . ?
F2 C1 1.341(3) . ?
N5 H5 0.8600 . ?
N5 C22 1.360(3) . ?
N5 C23 1.433(3) . ?
N4 H4A 0.8600 . ?
N4 C22 1.373(3) . ?
N4 C19 1.402(3) . ?
N2 H2 0.8600 . ?
N2 C9 1.436(3) . ?
N2 C8 1.363(3) . ?
N1 H1 0.8600 . ?
N1 C5 1.400(3) . ?
N1 C8 1.377(3) . ?
N6 H6A 0.8600 . ?
N6 C28 1.339(3) . ?
N6 C24 1.351(3) . ?
N3 C10 1.335(3) . ?
N3 C14 1.336(3) . ?
N3 H3A 0.78(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C5 C6 1.400(3) . ?
C5 C4 1.398(3) . ?
C28 H28 0.9300 . ?
C28 C27 1.374(3) . ?
C16 C17 1.386(4) . ?
C16 C21 1.391(4) . ?
C16 C15 1.490(3) . ?
C19 C20 1.392(3) . ?
C19 C18 1.400(3) . ?
C24 H24 0.9300 . ?
C24 C25 1.370(4) . ?
C2 C7 1.389(4) . ?
C2 C3 1.388(4) . ?
C2 C1 1.493(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.382(3) . ?
C27 H27 0.9300 . ?
C27 C26 1.386(3) . ?
C10 H10 0.9300 . ?
C10 C11 1.377(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.380(4) . ?
C4 H4 0.9300 . ?
C4 C3 1.380(4) . ?
C26 H26 0.9300 . ?
C26 C25 1.383(4) . ?
C7 H7 0.9300 . ?
C13 H13 0.9300 . ?
C13 C14 1.378(4) . ?
C13 C12 1.382(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.379(4) . ?
C25 H25 0.9300 . ?
C18 H18 0.9300 . ?
C11 H11 0.9300 . ?
C11 C12 1.389(4) . ?
C14 H14 0.9300 . ?
C21 H21 0.9300 . ?
C12 H12 0.9300 . ?
C3 H3 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
O2 S001 C9 106.14(10) . . ?
O4 S001 O2 111.38(10) . . ?
O4 S001 C9 104.64(10) . . ?
O3 S001 O2 112.20(10) . . ?
O3 S001 O4 114.50(10) . . ?
O3 S001 C9 107.25(10) . . ?
O6 S002 O8 110.54(10) . . ?
O6 S002 C23 106.85(10) . . ?
O8 S002 C23 105.66(10) . . ?
O7 S002 O6 113.82(10) . . ?
O7 S002 O8 113.25(10) . . ?
O7 S002 C23 106.06(11) . . ?
C22 N5 H5 119.1 . . ?
C22 N5 C23 121.78(19) . . ?
C23 N5 H5 119.1 . . ?
C22 N4 H4A 117.1 . . ?
C22 N4 C19 125.9(2) . . ?
C19 N4 H4A 117.1 . . ?
C9 N2 H2 119.8 . . ?
C8 N2 H2 119.8 . . ?
C8 N2 C9 120.31(19) . . ?
C5 N1 H1 116.9 . . ?
C8 N1 H1 116.9 . . ?
C8 N1 C5 126.3(2) . . ?
C28 N6 H6A 118.9 . . ?
C28 N6 C24 122.2(2) . . ?
C24 N6 H6A 118.9 . . ?
C10 N3 C14 123.2(2) . . ?
C10 N3 H3A 120(2) . . ?
C14 N3 H3A 117(2) . . ?
S001 C9 H9A 109.1 . . ?
S001 C9 H9B 109.1 . . ?
N2 C9 S001 112.39(16) . . ?
N2 C9 H9A 109.1 . . ?
N2 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
O5 C22 N5 123.2(2) . . ?
O5 C22 N4 123.4(2) . . ?
N5 C22 N4 113.4(2) . . ?
S002 C23 H23A 109.2 . . ?
S002 C23 H23B 109.2 . . ?
N5 C23 S002 112.18(16) . . ?
N5 C23 H23A 109.2 . . ?
N5 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C6 C5 N1 123.4(2) . . ?
C4 C5 N1 117.5(2) . . ?
C4 C5 C6 119.1(2) . . ?
N6 C28 H28 120.1 . . ?
N6 C28 C27 119.9(2) . . ?
C27 C28 H28 120.1 . . ?
O1 C8 N2 122.7(2) . . ?
O1 C8 N1 123.8(2) . . ?
N2 C8 N1 113.4(2) . . ?
C17 C16 C21 119.8(2) . . ?
C17 C16 C15 119.9(2) . . ?
C21 C16 C15 120.2(2) . . ?
C20 C19 N4 117.2(2) . . ?
C20 C19 C18 119.2(2) . . ?
C18 C19 N4 123.6(2) . . ?
N6 C24 H24 120.2 . . ?
N6 C24 C25 119.6(2) . . ?
C25 C24 H24 120.2 . . ?
C7 C2 C1 118.8(2) . . ?
C3 C2 C7 119.4(2) . . ?
C3 C2 C1 121.8(2) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 C5 119.5(2) . . ?
C7 C6 H6 120.2 . . ?
C28 C27 H27 120.4 . . ?
C28 C27 C26 119.2(2) . . ?
C26 C27 H27 120.4 . . ?
N3 C10 H10 120.4 . . ?
N3 C10 C11 119.2(2) . . ?
C11 C10 H10 120.4 . . ?
C19 C20 H20 119.5 . . ?
C21 C20 C19 121.0(2) . . ?
C21 C20 H20 119.5 . . ?
C5 C4 H4 119.6 . . ?
C3 C4 C5 120.7(2) . . ?
C3 C4 H4 119.6 . . ?
C27 C26 H26 120.1 . . ?
C25 C26 C27 119.7(2) . . ?
C25 C26 H26 120.1 . . ?
C2 C7 H7 119.4 . . ?
C6 C7 C2 121.1(2) . . ?
C6 C7 H7 119.4 . . ?
C14 C13 H13 120.6 . . ?
C14 C13 C12 118.9(2) . . ?
C12 C13 H13 120.6 . . ?
C16 C17 H17 119.5 . . ?
C18 C17 C16 121.0(2) . . ?
C18 C17 H17 119.5 . . ?
C24 C25 C26 119.4(2) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C19 C18 H18 120.2 . . ?
C17 C18 C19 119.5(2) . . ?
C17 C18 H18 120.2 . . ?
C10 C11 H11 120.4 . . ?
C10 C11 C12 119.1(2) . . ?
C12 C11 H11 120.4 . . ?
N3 C14 C13 119.6(2) . . ?
N3 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C16 C21 H21 120.3 . . ?
C20 C21 C16 119.5(2) . . ?
C20 C21 H21 120.3 . . ?
C13 C12 C11 119.9(2) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.1(2) . . ?
C4 C3 H3 120.0 . . ?
F1 C1 F2 105.6(2) . . ?
F1 C1 C2 112.2(2) . . ?
F3 C1 F1 106.1(2) . . ?
F3 C1 F2 106.2(2) . . ?
F3 C1 C2 113.3(2) . . ?
F2 C1 C2 112.8(2) . . ?
F6 C15 F5 106.2(2) . . ?
F6 C15 C16 111.9(2) . . ?
F5 C15 C16 112.7(2) . . ?
F4 C15 F6 106.0(2) . . ?
F4 C15 F5 106.3(2) . . ?
F4 C15 C16 113.1(2) . . ?

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
O6 S002 C23 N5 -74.81(17) . . . . ?
O2 S001 C9 N2 57.68(18) . . . . ?
O8 S002 C23 N5 42.94(18) . . . . ?
O4 S001 C9 N2 175.57(15) . . . . ?
O3 S001 C9 N2 -62.43(18) . . . . ?
O7 S002 C23 N5 163.43(16) . . . . ?
N4 C19 C20 C21 -176.3(2) . . . . ?
N4 C19 C18 C17 177.0(2) . . . . ?
N1 C5 C6 C7 -175.8(2) . . . . ?
N1 C5 C4 C3 175.7(2) . . . . ?
N6 C28 C27 C26 -0.7(4) . . . . ?
N6 C24 C25 C26 0.1(4) . . . . ?
N3 C10 C11 C12 -0.5(4) . . . . ?
C9 N2 C8 O1 5.0(3) . . . . ?
C9 N2 C8 N1 -176.81(19) . . . . ?
C22 N5 C23 S002 91.9(2) . . . . ?
C22 N4 C19 C20 -157.8(2) . . . . ?
C22 N4 C19 C18 24.7(4) . . . . ?
C23 N5 C22 O5 1.7(3) . . . . ?
C23 N5 C22 N4 -178.30(19) . . . . ?
C5 N1 C8 O1 -7.4(4) . . . . ?
C5 N1 C8 N2 174.5(2) . . . . ?
C5 C6 C7 C2 0.2(4) . . . . ?
C5 C4 C3 C2 0.2(4) . . . . ?
C28 N6 C24 C25 0.7(4) . . . . ?
C28 C27 C26 C25 1.4(4) . . . . ?
C8 N2 C9 S001 -96.5(2) . . . . ?
C8 N1 C5 C6 -18.5(4) . . . . ?
C8 N1 C5 C4 164.5(2) . . . . ?
C16 C17 C18 C19 -1.0(4) . . . . ?
C19 N4 C22 O5 1.2(4) . . . . ?
C19 N4 C22 N5 -178.7(2) . . . . ?
C19 C20 C21 C16 -0.7(4) . . . . ?
C24 N6 C28 C27 -0.4(4) . . . . ?
C6 C5 C4 C3 -1.4(4) . . . . ?
C27 C26 C25 C24 -1.1(4) . . . . ?
C10 N3 C14 C13 -0.9(4) . . . . ?
C10 C11 C12 C13 -1.2(4) . . . . ?
C20 C19 C18 C17 -0.5(4) . . . . ?
C4 C5 C6 C7 1.2(4) . . . . ?
C7 C2 C3 C4 1.2(4) . . . . ?
C7 C2 C1 F1 -58.0(3) . . . . ?
C7 C2 C1 F3 -178.1(2) . . . . ?
C7 C2 C1 F2 61.2(3) . . . . ?
C17 C16 C21 C20 -0.8(4) . . . . ?
C17 C16 C15 F6 84.5(3) . . . . ?
C17 C16 C15 F5 -155.8(2) . . . . ?
C17 C16 C15 F4 -35.2(3) . . . . ?
C18 C19 C20 C21 1.4(4) . . . . ?
C14 N3 C10 C11 1.6(4) . . . . ?
C14 C13 C12 C11 1.8(4) . . . . ?
C21 C16 C17 C18 1.6(4) . . . . ?
C21 C16 C15 F6 -91.5(3) . . . . ?
C21 C16 C15 F5 28.2(3) . . . . ?
C21 C16 C15 F4 148.8(2) . . . . ?
C12 C13 C14 N3 -0.7(4) . . . . ?
C3 C2 C7 C6 -1.4(4) . . . . ?
C3 C2 C1 F1 122.0(3) . . . . ?
C3 C2 C1 F3 1.9(4) . . . . ?
C3 C2 C1 F2 -118.9(3) . . . . ?
C1 C2 C7 C6 178.5(2) . . . . ?
C1 C2 C3 C4 -178.8(2) . . . . ?
C15 C16 C17 C18 -174.4(2) . . . . ?
C15 C16 C21 C20 175.3(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.192
_oxdiff_exptl_absorpt_empirical_full_min 0.754



# start Validation Reply Form
_vrf_PLAT230_Compound_1          
;
PROBLEM: Hirshfeld Test Diff for C36 -- C37 .. 8.3 s.u.
RESPONSE: Due to the room temperature collection a lot of thermal motion and disorder
 is present in the structure.  Where distinct sites could be identified for
 atoms they were modelled as such with relative occupancies refined, but 
 there is still residual unrefined disorder - as shown in checkCIF alerts 
 (level B).  Further refinement of this was not thought to be useful or
 necessary as it does not impact significantly on the structural information
 discussed in the manuscript.
;
_vrf_PLAT241_Compound_1          
;
PROBLEM: High ?MainMol? Ueq as Compared to Neighbors of O1 Check
RESPONSE: Due to the room temperature collection a lot of thermal motion and disorder
 is present in the structure.  Where distinct sites could be identified for
 atoms they were modelled as such with relative occupancies refined, but 
 there is still residual unrefined disorder - as shown in checkCIF alerts 
 (level B).  Further refinement of this was not thought to be useful or
 necessary as it does not impact significantly on the structural information
 discussed in the manuscript.
;
_vrf_PLAT915_Compound_2          
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage 38 %
RESPONSE: Flack Parameter refined to 0.033(16)
;
_vrf_DIFMX01_Compound_7          
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00
RESPONSE: There is significant residual electron density surrounding disordered
 CF3 groups.Where distinct sites could be identified for
 atoms they were modelled as such with relative occupancies refined, but 
 there is still residual unrefined disorder - as shown in checkCIF alerts 
 (level B).  Further refinement of this was not thought to be useful or
 necessary as it does not impact significantly on the structural information
 discussed in the manuscript.
;
_vrf_PLAT097_Compound_7          
;
PROBLEM: Large Reported Max. (Positive) Residual Density 2.00 eA-3
RESPONSE: There is significant residual electron density surrounding disordered
 CF3 groups. Where distinct sites could be identified for
 atoms they were modelled as such with relative occupancies refined, but 
 there is still residual unrefined disorder - as shown in checkCIF alerts 
 (level B).  Further refinement of this was not thought to be useful or
 necessary as it does not impact significantly on the structural information
 discussed in the manuscript.
;
_vrf_PLAT201_Compound_7          
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 4 Report
RESPONSE: There is significant residual electron density surrounding disordered
 CF3 groups, one of which was modelled using an isotropic model for the c and 
 3 F atoms.  An anisotropic model results in an unstable refinement.
;
_vrf_PLAT242_Compound_7          
;
PROBLEM: Low ?MainMol? Ueq as Compared to Neighbors of C39 Check
RESPONSE: C39 is part of a slightly disordered TBA ion.  Additional distinct 
 atomic positions could not be identified in the difference map, and as such 
 this disorder was not modelled.  This kind of disorder is common in these 
 highly flexible counter ions and does not affect the discussion in the 
 manuscript.
;
_vrf_PLAT306_Compound_7          
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O7 Check
RESPONSE: H atom positions could not be unambiguously identified in the 
 difference map.  The water channels are discussed in the manuscript.
;
_vrf_PLAT430_Compound_7          
;
PROBLEM: Short Inter D...A Contact O2 .. O7 .. 2.69 Ang.
RESPONSE: The water channels are discussed in the manuscript.
;
_vrf_PLAT987_Compound_9          
;
PROBLEM: The Flack x is >> 0 - Do a BASF/TWIN Refinement Please Check
RESPONSE: The flack parameter refined to 0.34(2)
;
# end Validation Reply Form
