# Electronic Supplementary Material (ESI) for Chemical Science.
# 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_1_kaj14pt1
_database_code_depnum_ccdc_archive 'CCDC 1457412'
_audit_update_record             
;
2016-03-03 deposited with the CCDC.
2016-04-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H32 N4 O6 S2'
_chemical_formula_weight         584.69

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.4474(5)
_cell_length_b                   8.6414(4)
_cell_length_c                   10.5047(6)
_cell_angle_alpha                101.755(4)
_cell_angle_beta                 103.383(5)
_cell_angle_gamma                98.623(4)
_cell_volume                     714.54(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    4050
_cell_measurement_theta_min      4.4460
_cell_measurement_theta_max      75.7860

_exptl_crystal_description       prismatic
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_F_000             308
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.063
_exptl_absorpt_coefficient_mu    2.098
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  CrysAlisPro, Agilent Technologies,
  Version 1.171.36.28
  Empirical absorption correction using spherical 
  harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;


_diffrn_crystal_treatment        
;
attached with Exxon Paratone N to a nylon loop and quenched 
in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. 
;


_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           'Cu K\a'
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.5861
_diffrn_reflns_number            6264
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         4.466
_diffrn_reflns_theta_max         76.143
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2933
_reflns_number_gt                2716
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;


_computing_data_collection       
;
  CrysAlisPro, Agilent Technologies,
;
_computing_cell_refinement       
;
  CrysAlisPro, Agilent Technologies,
;
_computing_data_reduction        
;
  CrysAlisPro, Agilent Technologies,
;
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
  ORTEP3 for Windows (Farrugia, L., 1997)
  ORTEPIII  (Burnett, N.M., Johnson,C.K., 1996). 
  WinGX (Farrugia, 1999)
  shelXle (Hï?1/2bschle,C.B., et al., 2011) 
;


_refine_special_details          
;
  Amine hydrogen sites located and modelled
  with isotropic displacement parameters.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.04P)²+0.1P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2933
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0902
_refine_ls_wR_factor_gt          0.0880
_refine_ls_goodness_of_fit_ref   1.323
_refine_ls_restrained_S_all      1.323
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
O1 O 0.29452(12) -0.06415(12) 0.12002(10) 0.0289(2) Uani 1 1 d . . . . .
O2 O 0.33645(13) 0.32176(12) 0.24828(10) 0.0303(2) Uani 1 1 d . . . . .
N1 N 0.29731(14) -0.13141(13) 0.41787(11) 0.0228(2) Uani 1 1 d . . . . .
H1N H 0.300(2) -0.113(2) 0.501(2) 0.030(4) Uiso 1 1 d . . . . .
N2 N 0.30268(14) 0.24257(13) 0.53642(11) 0.0226(2) Uani 1 1 d . . . . .
H2N H 0.304(2) 0.190(2) 0.5991(19) 0.027(4) Uiso 1 1 d . . . . .
C1 C 0.30419(14) -0.00487(14) 0.36485(12) 0.0190(2) Uani 1 1 d . . . . .
C2 C 0.30629(15) 0.02109(15) 0.23144(13) 0.0214(3) Uani 1 1 d . . . . .
C3 C 0.32123(15) 0.19906(15) 0.28939(13) 0.0215(3) Uani 1 1 d . . . . .
C4 C 0.31074(14) 0.16085(14) 0.41786(13) 0.0192(2) Uani 1 1 d . . . . .
C5 C 0.29037(17) 0.41286(15) 0.56327(14) 0.0259(3) Uani 1 1 d . . . . .
H5A H 0.2458 0.4407 0.4769 0.031 Uiso 1 1 calc R U . . .
H5B H 0.4025 0.4817 0.6070 0.031 Uiso 1 1 calc R U . . .
C6 C 0.17789(16) 0.44560(15) 0.65395(13) 0.0225(3) Uani 1 1 d . . . . .
C7 C 0.23561(17) 0.56652(16) 0.77301(15) 0.0289(3) Uani 1 1 d . . . . .
H7 H 0.3458 0.6284 0.7972 0.035 Uiso 1 1 calc R U . . .
C8 C 0.13260(19) 0.59743(18) 0.85701(15) 0.0342(3) Uani 1 1 d . . . . .
H8 H 0.1727 0.6801 0.9386 0.041 Uiso 1 1 calc R U . . .
C9 C -0.02851(18) 0.50791(17) 0.82194(14) 0.0284(3) Uani 1 1 d . . . . .
H9 H -0.0984 0.5297 0.8795 0.034 Uiso 1 1 calc R U . . .
C10 C -0.08860(16) 0.38602(14) 0.70262(13) 0.0220(3) Uani 1 1 d . . . . .
C11 C 0.01555(16) 0.35568(15) 0.61950(13) 0.0226(3) Uani 1 1 d . . . . .
H11 H -0.0243 0.2726 0.5382 0.027 Uiso 1 1 calc R U . . .
C12 C -0.26793(16) 0.29578(15) 0.66510(14) 0.0253(3) Uani 1 1 d . . . . .
H12A H -0.3010 0.2916 0.7490 0.030 Uiso 1 1 calc R U . . .
H12B H -0.3398 0.3569 0.6156 0.030 Uiso 1 1 calc R U . . .
S1 S 0.31176(4) 0.01174(4) 0.83345(3) 0.02669(11) Uani 1 1 d . . . . .
O3 O 0.31246(15) 0.01246(13) 0.68923(10) 0.0356(3) Uani 1 1 d . . . . .
C13 C 0.3889(2) 0.21646(19) 0.92736(15) 0.0362(3) Uani 1 1 d . . . . .
H13A H 0.3747 0.2279 1.0186 0.054 Uiso 1 1 calc R U . . .
H13B H 0.3273 0.2865 0.8821 0.054 Uiso 1 1 calc R U . . .
H13C H 0.5073 0.2476 0.9331 0.054 Uiso 1 1 calc R U . . .
C14 C 0.0998(2) 0.0011(3) 0.8349(2) 0.0516(5) Uani 1 1 d . . . . .
H14A H 0.0914 0.0132 0.9278 0.077 Uiso 1 1 calc R U . . .
H14B H 0.0331 -0.1037 0.7788 0.077 Uiso 1 1 calc R U . . .
H14C H 0.0585 0.0878 0.7989 0.077 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.2228(16) . ?
O2 C3 1.2242(17) . ?
N1 C1 1.3242(17) . ?
N1 C12 1.4590(16) 2_556 ?
N1 H1N 0.85(2) . ?
N2 C4 1.3228(17) . ?
N2 C5 1.4650(16) . ?
N2 H2N 0.872(19) . ?
C1 C4 1.4146(16) . ?
C1 C2 1.4674(17) . ?
C2 C3 1.5088(17) . ?
C3 C4 1.4718(17) . ?
C5 C6 1.5099(17) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.3879(18) . ?
C6 C11 1.3970(18) . ?
C7 C8 1.391(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.386(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.3947(18) . ?
C9 H9 0.9500 . ?
C10 C11 1.3917(18) . ?
C10 C12 1.5174(17) . ?
C11 H11 0.9500 . ?
C12 N1 1.4589(16) 2_556 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
S1 O3 1.5177(10) . ?
S1 C13 1.7813(16) . ?
S1 C14 1.7826(17) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 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
C1 N1 C12 121.74(11) . 2_556 ?
C1 N1 H1N 116.7(12) . . ?
C12 N1 H1N 121.3(12) 2_556 . ?
C4 N2 C5 122.60(12) . . ?
C4 N2 H2N 116.9(12) . . ?
C5 N2 H2N 120.5(12) . . ?
N1 C1 C4 132.92(12) . . ?
N1 C1 C2 135.29(11) . . ?
C4 C1 C2 91.79(10) . . ?
O1 C2 C1 136.17(12) . . ?
O1 C2 C3 135.45(13) . . ?
C1 C2 C3 88.33(10) . . ?
O2 C3 C4 135.87(12) . . ?
O2 C3 C2 136.18(12) . . ?
C4 C3 C2 87.95(10) . . ?
N2 C4 C1 132.29(12) . . ?
N2 C4 C3 135.82(12) . . ?
C1 C4 C3 91.83(10) . . ?
N2 C5 C6 110.67(11) . . ?
N2 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
C7 C6 C11 119.30(12) . . ?
C7 C6 C5 119.90(12) . . ?
C11 C6 C5 120.81(11) . . ?
C6 C7 C8 120.21(13) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C9 C8 C7 120.15(13) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 120.41(13) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C11 C10 C9 119.01(12) . . ?
C11 C10 C12 122.24(11) . . ?
C9 C10 C12 118.70(12) . . ?
C10 C11 C6 120.93(12) . . ?
C10 C11 H11 119.5 . . ?
C6 C11 H11 119.5 . . ?
N1 C12 C10 113.84(10) 2_556 . ?
N1 C12 H12A 108.8 2_556 . ?
C10 C12 H12A 108.8 . . ?
N1 C12 H12B 108.8 2_556 . ?
C10 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
O3 S1 C13 105.23(7) . . ?
O3 S1 C14 104.76(8) . . ?
C13 S1 C14 97.45(10) . . ?
S1 C13 H13A 109.5 . . ?
S1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
S1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
S1 C14 H14A 109.5 . . ?
S1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
S1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 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
C12 N1 C1 C4 171.21(12) 2_556 . . . ?
C12 N1 C1 C2 -8.0(2) 2_556 . . . ?
N1 C1 C2 O1 4.4(3) . . . . ?
C4 C1 C2 O1 -175.05(15) . . . . ?
N1 C1 C2 C3 -178.15(14) . . . . ?
C4 C1 C2 C3 2.43(9) . . . . ?
O1 C2 C3 O2 -5.2(3) . . . . ?
C1 C2 C3 O2 177.26(16) . . . . ?
O1 C2 C3 C4 175.18(15) . . . . ?
C1 C2 C3 C4 -2.34(9) . . . . ?
C5 N2 C4 C1 -171.74(12) . . . . ?
C5 N2 C4 C3 4.6(2) . . . . ?
N1 C1 C4 N2 -4.5(2) . . . . ?
C2 C1 C4 N2 174.97(13) . . . . ?
N1 C1 C4 C3 178.07(13) . . . . ?
C2 C1 C4 C3 -2.49(9) . . . . ?
O2 C3 C4 N2 5.5(3) . . . . ?
C2 C3 C4 N2 -174.89(14) . . . . ?
O2 C3 C4 C1 -177.18(15) . . . . ?
C2 C3 C4 C1 2.43(9) . . . . ?
C4 N2 C5 C6 142.83(12) . . . . ?
N2 C5 C6 C7 125.34(13) . . . . ?
N2 C5 C6 C11 -54.77(17) . . . . ?
C11 C6 C7 C8 0.1(2) . . . . ?
C5 C6 C7 C8 179.95(14) . . . . ?
C6 C7 C8 C9 -0.2(2) . . . . ?
C7 C8 C9 C10 0.2(2) . . . . ?
C8 C9 C10 C11 0.0(2) . . . . ?
C8 C9 C10 C12 -177.42(13) . . . . ?
C9 C10 C11 C6 -0.2(2) . . . . ?
C12 C10 C11 C6 177.17(12) . . . . ?
C7 C6 C11 C10 0.1(2) . . . . ?
C5 C6 C11 C10 -179.74(12) . . . . ?
C11 C10 C12 N1 30.13(18) . . . 2_556 ?
C9 C10 C12 N1 -152.50(13) . . . 2_556 ?

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 H1N O3 0.85(2) 2.02(2) 2.8332(15) 158.9(17) .
N2 H2N O3 0.872(19) 1.962(19) 2.7975(16) 160.0(17) .
C5 H5B O2 0.99 2.52 3.4942(17) 169.4 2_666
C12 H12A O1 0.99 2.62 3.3306(17) 128.9 2_556
C13 H13A O2 0.98 2.50 3.4572(18) 167.0 1_556
C13 H13C O1 0.98 2.55 3.2457(19) 128.1 2_656
C14 H14A O1 0.98 2.60 3.268(2) 125.5 1_556

_refine_diff_density_max         0.375
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.045


####################################################################### 
# 
# 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_3_kaj14mm_s1360
_database_code_depnum_ccdc_archive 'CCDC 1457413'
_audit_update_record             
;
2016-03-03 deposited with the CCDC.
2016-04-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H32 N4 O6 S2'
_chemical_formula_weight         584.69

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

_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.
;


loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.4511(2)
_cell_length_b                   8.5911(2)
_cell_length_c                   10.8922(2)
_cell_angle_alpha                73.717(2)
_cell_angle_beta                 84.157(2)
_cell_angle_gamma                69.545(2)
_cell_volume                     711.23(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    26314
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      76.28

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_F_000             308
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    2.108
_shelx_estimated_absorpt_T_min   0.743
_shelx_estimated_absorpt_T_max   0.866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
  CrysAlisPro, Agilent Technologies,
  Version 1.171.37.35
  Empirical absorption correction using spherical 
  harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_crystal_treatment        
;
attached with Exxon Paratone N to a nylon loop and quenched 
in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. 
;


_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           'Cu K\a'
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.5861
_diffrn_reflns_number            26314
_diffrn_reflns_av_unetI/netI     0.0085
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.228
_diffrn_reflns_theta_max         76.274
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2962
_reflns_number_gt                2896
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31d (release 11-02-2014 CrysAlis171 .NET)
(compiled Feb 11 2014,18:09:27)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31d (release 11-02-2014 CrysAlis171 .NET)
(compiled Feb 11 2014,18:09:27)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31d (release 11-02-2014 CrysAlis171 .NET)
(compiled Feb 11 2014,18:09:27)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
  ORTEP3 for Windows (Farrugia, L., 1997)
  ORTEPIII  (Burnett, N.M., Johnson,C.K., 1996). 
  WinGX (Farrugia, 1999)
  shelXle (Hï?1/2bschle,C.B., et al., 2011) 
;



_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.03P)²+0.3P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2962
_refine_ls_number_parameters     189
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0879
_refine_ls_wR_factor_gt          0.0875
_refine_ls_goodness_of_fit_ref   1.308
_refine_ls_restrained_S_all      1.308
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
O1 O 0.69329(14) -0.41901(13) 0.54331(10) 0.0291(2) Uani 1 1 d . . . . .
O2 O 0.79195(14) -0.07012(14) 0.40866(11) 0.0323(3) Uani 1 1 d . . . . .
N1 N 0.33947(16) -0.24816(16) 0.39421(11) 0.0231(3) Uani 1 1 d . . . . .
H1N H 0.352(2) -0.354(3) 0.4284(18) 0.032(5) Uiso 1 1 d . . . . .
N2 N 0.42320(16) 0.11257(15) 0.27087(11) 0.0221(2) Uani 1 1 d . . . . .
H2N H 0.329(3) 0.135(2) 0.2434(18) 0.029(5) Uiso 1 1 d . . . . .
C1 C 0.46622(18) -0.19364(17) 0.40220(12) 0.0206(3) Uani 1 1 d . . . . .
C2 C 0.62545(18) -0.27606(17) 0.47038(12) 0.0223(3) Uani 1 1 d . . . . .
C3 C 0.67054(18) -0.11599(18) 0.41006(13) 0.0228(3) Uani 1 1 d . . . . .
C4 C 0.50338(17) -0.03968(17) 0.34675(12) 0.0201(3) Uani 1 1 d . . . . .
C5 C 0.50891(19) 0.23767(17) 0.21265(13) 0.0233(3) Uani 1 1 d . . . . .
H5A H 0.6024 0.2197 0.2686 0.028 Uiso 1 1 calc R U . . .
H5B H 0.4283 0.3557 0.2047 0.028 Uiso 1 1 calc R U . . .
C6 C 0.57831(17) 0.21930(17) 0.08199(13) 0.0205(3) Uani 1 1 d . . . . .
C7 C 0.73165(19) 0.09396(19) 0.06935(14) 0.0278(3) Uani 1 1 d . . . . .
H7 H 0.7953 0.0212 0.1435 0.033 Uiso 1 1 calc R U . . .
C8 C 0.79295(19) 0.0738(2) -0.05024(14) 0.0273(3) Uani 1 1 d . . . . .
H8 H 0.8964 -0.0148 -0.0569 0.033 Uiso 1 1 calc R U . . .
C9 C 0.70470(17) 0.18173(17) -0.16046(13) 0.0201(3) Uani 1 1 d . . . . .
C10 C 0.55005(19) 0.30540(18) -0.14767(13) 0.0242(3) Uani 1 1 d . . . . .
H10 H 0.4870 0.3789 -0.2219 0.029 Uiso 1 1 calc R U . . .
C11 C 0.48669(18) 0.32272(18) -0.02757(14) 0.0240(3) Uani 1 1 d . . . . .
H11 H 0.3796 0.4062 -0.0204 0.029 Uiso 1 1 calc R U . . .
C12 C 0.78162(18) 0.16225(18) -0.28989(13) 0.0234(3) Uani 1 1 d . . . . .
H12A H 0.8750 0.2101 -0.3079 0.028 Uiso 1 1 calc R U . . .
H12B H 0.8302 0.0382 -0.2863 0.028 Uiso 1 1 calc R U . . .
S1 S -0.05660(5) 0.39395(5) 0.19015(4) 0.02892(12) Uani 1 1 d . . . . .
O3 O 0.10240(15) 0.27700(15) 0.14628(10) 0.0337(3) Uani 1 1 d . . . . .
C13 C -0.0736(3) 0.3048(3) 0.35548(19) 0.0574(6) Uani 1 1 d . . . . .
H13A H -0.1765 0.3773 0.3888 0.086 Uiso 1 1 calc R U . . .
H13B H -0.0788 0.1887 0.3704 0.086 Uiso 1 1 calc R U . . .
H13C H 0.0250 0.2987 0.3992 0.086 Uiso 1 1 calc R U . . .
C14 C -0.0123(3) 0.5789(3) 0.1967(2) 0.0540(5) Uani 1 1 d . . . . .
H14A H -0.1134 0.6598 0.2251 0.081 Uiso 1 1 calc R U . . .
H14B H 0.0799 0.5445 0.2570 0.081 Uiso 1 1 calc R U . . .
H14C H 0.0210 0.6345 0.1115 0.081 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.2335(17) . ?
O2 C3 1.2183(18) . ?
N1 C1 1.3293(19) . ?
N1 C12 1.4566(18) 2_655 ?
N1 H1N 0.86(2) . ?
N2 C4 1.3196(18) . ?
N2 C5 1.4663(17) . ?
N2 H2N 0.82(2) . ?
C1 C4 1.4200(18) . ?
C1 C2 1.451(2) . ?
C2 C3 1.5088(19) . ?
C3 C4 1.483(2) . ?
C5 C6 1.5118(18) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C11 1.3877(19) . ?
C6 C7 1.389(2) . ?
C7 C8 1.386(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.390(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.390(2) . ?
C9 C12 1.5192(19) . ?
C10 C11 1.390(2) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 N1 1.4565(18) 2_655 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
S1 O3 1.4961(11) . ?
S1 C13 1.761(2) . ?
S1 C14 1.7762(19) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 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
C1 N1 C12 121.26(12) . 2_655 ?
C1 N1 H1N 118.0(13) . . ?
C12 N1 H1N 115.5(13) 2_655 . ?
C4 N2 C5 121.70(13) . . ?
C4 N2 H2N 121.6(13) . . ?
C5 N2 H2N 115.8(13) . . ?
N1 C1 C4 135.22(13) . . ?
N1 C1 C2 132.48(13) . . ?
C4 C1 C2 92.28(11) . . ?
O1 C2 C1 134.31(13) . . ?
O1 C2 C3 136.73(14) . . ?
C1 C2 C3 88.93(11) . . ?
O2 C3 C4 135.52(13) . . ?
O2 C3 C2 136.84(14) . . ?
C4 C3 C2 87.58(11) . . ?
N2 C4 C1 135.39(14) . . ?
N2 C4 C3 133.44(13) . . ?
C1 C4 C3 91.17(11) . . ?
N2 C5 C6 111.00(11) . . ?
N2 C5 H5A 109.4 . . ?
C6 C5 H5A 109.4 . . ?
N2 C5 H5B 109.4 . . ?
C6 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
C11 C6 C7 118.60(13) . . ?
C11 C6 C5 120.60(12) . . ?
C7 C6 C5 120.75(12) . . ?
C8 C7 C6 120.76(13) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C7 C8 C9 120.74(13) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C10 C9 C8 118.44(13) . . ?
C10 C9 C12 122.54(12) . . ?
C8 C9 C12 119.01(12) . . ?
C11 C10 C9 120.74(13) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C6 C11 C10 120.64(13) . . ?
C6 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
N1 C12 C9 113.26(11) 2_655 . ?
N1 C12 H12A 108.9 2_655 . ?
C9 C12 H12A 108.9 . . ?
N1 C12 H12B 108.9 2_655 . ?
C9 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
O3 S1 C13 106.41(8) . . ?
O3 S1 C14 106.49(9) . . ?
C13 S1 C14 98.61(12) . . ?
S1 C13 H13A 109.5 . . ?
S1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
S1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
S1 C14 H14A 109.5 . . ?
S1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
S1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 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
C12 N1 C1 C4 17.0(2) 2_655 . . . ?
C12 N1 C1 C2 -160.48(13) 2_655 . . . ?
N1 C1 C2 O1 -1.4(3) . . . . ?
C4 C1 C2 O1 -179.66(16) . . . . ?
N1 C1 C2 C3 176.75(15) . . . . ?
C4 C1 C2 C3 -1.47(10) . . . . ?
O1 C2 C3 O2 2.2(3) . . . . ?
C1 C2 C3 O2 -175.96(18) . . . . ?
O1 C2 C3 C4 179.52(17) . . . . ?
C1 C2 C3 C4 1.41(10) . . . . ?
C5 N2 C4 C1 -169.60(14) . . . . ?
C5 N2 C4 C3 11.7(2) . . . . ?
N1 C1 C4 N2 4.3(3) . . . . ?
C2 C1 C4 N2 -177.60(16) . . . . ?
N1 C1 C4 C3 -176.64(15) . . . . ?
C2 C1 C4 C3 1.49(10) . . . . ?
O2 C3 C4 N2 -4.9(3) . . . . ?
C2 C3 C4 N2 177.69(15) . . . . ?
O2 C3 C4 C1 175.99(17) . . . . ?
C2 C3 C4 C1 -1.44(10) . . . . ?
C4 N2 C5 C6 92.38(15) . . . . ?
N2 C5 C6 C11 95.55(15) . . . . ?
N2 C5 C6 C7 -81.76(17) . . . . ?
C11 C6 C7 C8 0.7(2) . . . . ?
C5 C6 C7 C8 178.09(14) . . . . ?
C6 C7 C8 C9 1.9(2) . . . . ?
C7 C8 C9 C10 -2.8(2) . . . . ?
C7 C8 C9 C12 176.28(13) . . . . ?
C8 C9 C10 C11 1.2(2) . . . . ?
C12 C9 C10 C11 -177.86(13) . . . . ?
C7 C6 C11 C10 -2.3(2) . . . . ?
C5 C6 C11 C10 -179.71(13) . . . . ?
C9 C10 C11 C6 1.4(2) . . . . ?
C10 C9 C12 N1 -16.49(19) . . . 2_655 ?
C8 C9 C12 N1 164.49(13) . . . 2_655 ?

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 H1N O1 0.86(2) 2.05(2) 2.8530(16) 156.4(18) 2_646
N2 H2N O3 0.82(2) 2.08(2) 2.8608(17) 159.6(18) .
C5 H5A O2 0.99 2.58 3.2749(18) 126.9 .
C12 H12B O3 0.99 2.60 3.4734(18) 147.0 2_655
C13 H13A O1 0.98 2.65 3.512(2) 146.6 1_465
C13 H13C O2 0.98 2.62 3.364(3) 133.0 2_656

_refine_diff_density_max         0.302
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.061


####################################################################### 
# 
# 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_1+sulfate_kaj14mm_s1366
_database_code_depnum_ccdc_archive 'CCDC 1457414'
_audit_update_record             
;
2016-03-03 deposited with the CCDC.
2016-04-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H96 N6 O10 S'
_chemical_formula_weight         1045.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14


_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.3065(19)
_cell_length_b                   12.0238(10)
_cell_length_c                   25.441(2)
_cell_angle_alpha                90
_cell_angle_beta                 110.374(5)
_cell_angle_gamma                90
_cell_volume                     5823.1(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    18518
_cell_measurement_theta_min      2.797
_cell_measurement_theta_max      29.4135

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_F_000             2280
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
 SADABS (Sheldrick, 1996)
;

_diffrn_crystal_treatment        
;
attached with Exxon Paratone N to a nylon loop and quenched 
in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. 
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  APEXII-FR591
_diffrn_measurement_method       ω+φ
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            129874
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.670
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10639
_reflns_number_gt                8458
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'APEX (Bruker-AXS,2012)'
_computing_cell_refinement       'SAINT (Bruker-AXS,2012)'
_computing_data_reduction        'SAINT and XPREP (Bruker-AXS,2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
  ORTEP3 for Windows (Farrugia, L., 1997)
  ORTEPIII  (Burnett, N.M., Johnson,C.K., 1996). 
  WinGX (Farrugia, 1999)
  shelXle (Hï?1/2bschle,C.B., et al., 2011) 
;
_computing_publication_material  ?


_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.035P)²+4.0P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10639
_refine_ls_number_parameters     696
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.1182
_refine_ls_wR_factor_gt          0.1097
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_restrained_S_all      1.184
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
O1 O 0.43313(9) 1.04802(14) 0.13685(7) 0.0429(4) Uani 1 1 d . . . . .
O2 O 0.27301(9) 1.06237(13) 0.04447(6) 0.0378(4) Uani 1 1 d . . . . .
O3 O 0.10600(7) 1.11524(12) 0.33061(6) 0.0302(3) Uani 1 1 d . . . . .
O4 O 0.26490(7) 1.09045(12) 0.42398(6) 0.0302(3) Uani 1 1 d . . . . .
N1 N 0.38604(9) 0.83106(14) 0.19429(7) 0.0249(4) Uani 1 1 d . . . . .
H1N H 0.3650 0.7683 0.1968 0.030 Uiso 1 1 calc R U . . .
N2 N 0.22829(9) 0.84610(15) 0.10447(7) 0.0274(4) Uani 1 1 d . . . . .
H2N H 0.2321 0.7826 0.1225 0.033 Uiso 1 1 calc R U . . .
N3 N 0.13527(8) 0.89085(13) 0.26622(7) 0.0222(4) Uani 1 1 d . . . . .
H3N H 0.1539 0.8276 0.2610 0.027 Uiso 1 1 calc R U . . .
N4 N 0.28989(8) 0.86743(14) 0.35848(7) 0.0232(4) Uani 1 1 d . . . . .
H4N H 0.2801 0.8017 0.3425 0.028 Uiso 1 1 calc R U . . .
C1 C 0.35449(11) 0.90109(16) 0.15263(8) 0.0239(4) Uani 1 1 d . . . . .
C2 C 0.37775(12) 0.99731(18) 0.12761(9) 0.0299(5) Uani 1 1 d . . . . .
C3 C 0.30415(12) 1.00382(17) 0.08522(9) 0.0284(5) Uani 1 1 d . . . . .
C4 C 0.28555(11) 0.90811(17) 0.11307(8) 0.0250(4) Uani 1 1 d . . . . .
C5 C 0.15932(11) 0.88071(19) 0.06597(9) 0.0312(5) Uani 1 1 d . . . . .
H5A H 0.1325 0.8139 0.0479 0.037 Uiso 1 1 calc R U . . .
H5B H 0.1657 0.9276 0.0361 0.037 Uiso 1 1 calc R U . . .
C6 C 0.11707(11) 0.94495(17) 0.09449(8) 0.0270(5) Uani 1 1 d . . . . .
C7 C 0.08052(13) 1.03975(19) 0.06966(10) 0.0389(6) Uani 1 1 d . . . . .
H7 H 0.0833 1.0658 0.0352 0.047 Uiso 1 1 calc R U . . .
C8 C 0.04011(14) 1.0965(2) 0.09471(11) 0.0459(6) Uani 1 1 d . . . . .
H8 H 0.0147 1.1608 0.0772 0.055 Uiso 1 1 calc R U . . .
C9 C 0.03649(12) 1.05996(18) 0.14543(10) 0.0347(5) Uani 1 1 d . . . . .
H9 H 0.0092 1.0999 0.1627 0.042 Uiso 1 1 calc R U . . .
C10 C 0.07268(10) 0.96511(16) 0.17094(8) 0.0229(4) Uani 1 1 d . . . . .
C11 C 0.11240(10) 0.90784(17) 0.14503(8) 0.0243(4) Uani 1 1 d . . . . .
H11 H 0.1368 0.8424 0.1620 0.029 Uiso 1 1 calc R U . . .
C12 C 0.06725(10) 0.92363(17) 0.22542(8) 0.0242(4) Uani 1 1 d . . . . .
H12A H 0.0467 0.9830 0.2419 0.029 Uiso 1 1 calc R U . . .
H12B H 0.0350 0.8590 0.2175 0.029 Uiso 1 1 calc R U . . .
C13 C 0.17008(10) 0.95148(15) 0.31047(8) 0.0205(4) Uani 1 1 d . . . . .
C14 C 0.15597(10) 1.05144(16) 0.33847(8) 0.0221(4) Uani 1 1 d . . . . .
C15 C 0.22915(10) 1.04042(16) 0.38137(8) 0.0224(4) Uani 1 1 d . . . . .
C16 C 0.23852(10) 0.94159(15) 0.35092(8) 0.0201(4) Uani 1 1 d . . . . .
C17 C 0.36258(10) 0.89459(18) 0.39329(8) 0.0258(4) Uani 1 1 d . . . . .
H17A H 0.3872 0.8260 0.4113 0.031 Uiso 1 1 calc R U . . .
H17B H 0.3624 0.9470 0.4232 0.031 Uiso 1 1 calc R U . . .
C18 C 0.40133(10) 0.94631(17) 0.35830(8) 0.0230(4) Uani 1 1 d . . . . .
C19 C 0.42281(11) 1.05703(18) 0.36474(9) 0.0299(5) Uani 1 1 d . . . . .
H19 H 0.4141 1.1020 0.3924 0.036 Uiso 1 1 calc R U . . .
C20 C 0.45691(12) 1.10182(19) 0.33078(9) 0.0339(5) Uani 1 1 d . . . . .
H20 H 0.4721 1.1770 0.3358 0.041 Uiso 1 1 calc R U . . .
C21 C 0.46895(11) 1.03803(18) 0.28964(9) 0.0283(5) Uani 1 1 d . . . . .
H21 H 0.4920 1.0695 0.2665 0.034 Uiso 1 1 calc R U . . .
C22 C 0.44711(10) 0.92778(17) 0.28246(8) 0.0232(4) Uani 1 1 d . . . . .
C23 C 0.41377(10) 0.88295(17) 0.31715(8) 0.0234(4) Uani 1 1 d . . . . .
H23 H 0.3993 0.8074 0.3125 0.028 Uiso 1 1 calc R U . . .
C24 C 0.45533(10) 0.85641(18) 0.23615(8) 0.0272(5) Uani 1 1 d . . . . .
H24A H 0.4843 0.8961 0.2179 0.033 Uiso 1 1 calc R U . . .
H24B H 0.4796 0.7863 0.2522 0.033 Uiso 1 1 calc R U . . .
N5 N 0.30708(9) 0.41603(15) 0.09921(7) 0.0268(4) Uani 1 1 d . . . . .
C25 C 0.31764(12) 0.37297(19) 0.15806(8) 0.0311(5) Uani 1 1 d . . . . .
H25A H 0.3686 0.3631 0.1783 0.037 Uiso 1 1 calc R U . . .
H25B H 0.3009 0.4305 0.1783 0.037 Uiso 1 1 calc R U . . .
C26 C 0.28080(13) 0.26424(19) 0.16072(9) 0.0359(5) Uani 1 1 d . . . . .
H26A H 0.2941 0.2068 0.1384 0.043 Uiso 1 1 calc R U . . .
H26B H 0.2293 0.2748 0.1446 0.043 Uiso 1 1 calc R U . . .
C27 C 0.30146(14) 0.2260(2) 0.22131(10) 0.0437(6) Uani 1 1 d . . . . .
H27A H 0.2896 0.2854 0.2435 0.052 Uiso 1 1 calc R U . . .
H27B H 0.3530 0.2147 0.2367 0.052 Uiso 1 1 calc R U . . .
C28 C 0.26525(14) 0.1189(2) 0.22797(10) 0.0443(6) Uani 1 1 d . . . . .
H28A H 0.2806 0.0986 0.2677 0.066 Uiso 1 1 calc R U . . .
H28B H 0.2142 0.1298 0.2136 0.066 Uiso 1 1 calc R U . . .
H28C H 0.2776 0.0592 0.2068 0.066 Uiso 1 1 calc R U . . .
C29 C 0.33823(11) 0.33655(17) 0.06761(8) 0.0282(5) Uani 1 1 d . . . . .
H29A H 0.3310 0.3682 0.0301 0.034 Uiso 1 1 calc R U . . .
H29B H 0.3121 0.2654 0.0620 0.034 Uiso 1 1 calc R U . . .
C30 C 0.41616(12) 0.31235(18) 0.09642(8) 0.0312(5) Uani 1 1 d . . . . .
H30A H 0.4230 0.2645 0.1296 0.037 Uiso 1 1 calc R U . . .
H30B H 0.4418 0.3829 0.1094 0.037 Uiso 1 1 calc R U . . .
C31 C 0.44555(13) 0.25367(19) 0.05573(9) 0.0357(5) Uani 1 1 d . . . . .
H31A H 0.4928 0.2239 0.0771 0.043 Uiso 1 1 calc R U . . .
H31B H 0.4148 0.1899 0.0384 0.043 Uiso 1 1 calc R U . . .
C32 C 0.45101(13) 0.3293(2) 0.00969(9) 0.0377(5) Uani 1 1 d . . . . .
H32A H 0.4700 0.2873 -0.0148 0.056 Uiso 1 1 calc R U . . .
H32B H 0.4043 0.3577 -0.0123 0.056 Uiso 1 1 calc R U . . .
H32C H 0.4823 0.3918 0.0265 0.056 Uiso 1 1 calc R U . . .
C33 C 0.34261(10) 0.52927(17) 0.10714(8) 0.0258(5) Uani 1 1 d . . . . .
H33A H 0.3188 0.5788 0.1260 0.031 Uiso 1 1 calc R U . . .
H33B H 0.3918 0.5203 0.1327 0.031 Uiso 1 1 calc R U . . .
C34 C 0.34335(15) 0.5863(2) 0.05450(10) 0.0476(7) Uani 1 1 d . . . . .
H34A H 0.3719 0.5416 0.0377 0.057 Uiso 1 1 calc R U . . .
H34B H 0.2948 0.5893 0.0271 0.057 Uiso 1 1 calc R U . . .
C35 C 0.37165(17) 0.6984(2) 0.06460(11) 0.0567(8) Uani 1 1 d . . . . .
H35A H 0.4203 0.6921 0.0916 0.068 Uiso 1 1 calc R U . . .
H35B H 0.3444 0.7388 0.0841 0.068 Uiso 1 1 calc R U . . .
C36 C 0.37452(14) 0.7708(2) 0.01895(10) 0.0429(6) Uani 1 1 d . . . . .
H36A H 0.3953 0.8425 0.0344 0.064 Uiso 1 1 calc R U . . .
H36B H 0.4033 0.7355 -0.0003 0.064 Uiso 1 1 calc R U . . .
H36C H 0.3269 0.7827 -0.0078 0.064 Uiso 1 1 calc R U . . .
C37 C 0.22973(11) 0.4255(2) 0.06402(9) 0.0351(5) Uani 1 1 d . . . . .
H37A H 0.2252 0.4553 0.0267 0.042 Uiso 1 1 calc R U . A 1
H37B H 0.2086 0.3503 0.0585 0.042 Uiso 1 1 calc R U . A 1
C38A C 0.19059(19) 0.4971(4) 0.08912(17) 0.0315(9) Uani 0.65 1 d . . P B 1
H38A H 0.1997 0.5760 0.0829 0.038 Uiso 0.65 1 calc R U P B 1
H38B H 0.2067 0.4838 0.1301 0.038 Uiso 0.65 1 calc R U P B 1
C39A C 0.11245(17) 0.4736(3) 0.06345(16) 0.0367(9) Uani 0.65 1 d . . P B 1
H39A H 0.0980 0.4760 0.0221 0.044 Uiso 0.65 1 calc R U P B 1
H39B H 0.1028 0.3978 0.0742 0.044 Uiso 0.65 1 calc R U P B 1
C40A C 0.0699(2) 0.5566(3) 0.0824(2) 0.0536(11) Uani 0.65 1 d . . P B 1
H40A H 0.0198 0.5389 0.0651 0.080 Uiso 0.65 1 calc R U P B 1
H40B H 0.0835 0.5534 0.1233 0.080 Uiso 0.65 1 calc R U P B 1
H40C H 0.0787 0.6315 0.0712 0.080 Uiso 0.65 1 calc R U P B 1
C38B C 0.1874(4) 0.5362(7) 0.0763(3) 0.027(2) Uiso 0.35 1 d . . P B 2
H38C H 0.1953 0.5404 0.1169 0.032 Uiso 0.35 1 calc R U P B 2
H38D H 0.2070 0.6045 0.0658 0.032 Uiso 0.35 1 calc R U P B 2
C39B C 0.1064(4) 0.5318(7) 0.0429(3) 0.0434(18) Uiso 0.35 1 d . . P B 2
H39C H 0.0863 0.6074 0.0405 0.052 Uiso 0.35 1 calc R U P B 2
H39D H 0.0980 0.5053 0.0043 0.052 Uiso 0.35 1 calc R U P B 2
C40B C 0.0711(4) 0.4558(7) 0.0710(3) 0.0467(18) Uiso 0.35 1 d . . P B 2
H40D H 0.0206 0.4540 0.0496 0.070 Uiso 0.35 1 calc R U P B 2
H40E H 0.0906 0.3808 0.0728 0.070 Uiso 0.35 1 calc R U P B 2
H40F H 0.0788 0.4827 0.1090 0.070 Uiso 0.35 1 calc R U P B 2
N6 N 0.21274(8) 0.42959(13) 0.36131(7) 0.0241(4) Uani 1 1 d . . . . .
C41 C 0.18723(10) 0.36977(17) 0.30441(8) 0.0251(4) Uani 1 1 d . . . . .
H41A H 0.2127 0.4020 0.2812 0.030 Uiso 1 1 calc R U . . .
H41B H 0.2016 0.2908 0.3111 0.030 Uiso 1 1 calc R U . . .
C42 C 0.10930(10) 0.37245(18) 0.27002(8) 0.0265(4) Uani 1 1 d . . . . .
H42A H 0.0909 0.4486 0.2703 0.032 Uiso 1 1 calc R U . . .
H42B H 0.0838 0.3218 0.2869 0.032 Uiso 1 1 calc R U . . .
C43 C 0.09697(11) 0.3369(2) 0.20986(9) 0.0320(5) Uani 1 1 d . . . . .
H43A H 0.1117 0.2585 0.2095 0.038 Uiso 1 1 calc R U . . .
H43B H 0.1260 0.3834 0.1943 0.038 Uiso 1 1 calc R U . . .
C44 C 0.01957(11) 0.34876(19) 0.17321(9) 0.0339(5) Uani 1 1 d . . . . .
H44A H 0.0131 0.3254 0.1348 0.051 Uiso 1 1 calc R U . . .
H44B H -0.0092 0.3019 0.1883 0.051 Uiso 1 1 calc R U . . .
H44C H 0.0052 0.4266 0.1731 0.051 Uiso 1 1 calc R U . . .
C45 C 0.29139(11) 0.45137(17) 0.37627(9) 0.0292(5) Uani 1 1 d . . . . .
H45A H 0.2979 0.4989 0.3467 0.035 Uiso 1 1 calc R U . . .
H45B H 0.3081 0.4941 0.4117 0.035 Uiso 1 1 calc R U . . .
C46 C 0.33779(11) 0.34891(18) 0.38312(9) 0.0297(5) Uani 1 1 d . . . . .
H46A H 0.3165 0.2972 0.3514 0.036 Uiso 1 1 calc R U . . .
H46B H 0.3416 0.3098 0.4183 0.036 Uiso 1 1 calc R U . . .
C47 C 0.41131(12) 0.3841(2) 0.38472(10) 0.0381(6) Uani 1 1 d . . . . .
H47A H 0.4413 0.3170 0.3906 0.046 Uiso 1 1 calc R U . . .
H47B H 0.4072 0.4161 0.3478 0.046 Uiso 1 1 calc R U . . .
C48 C 0.44677(13) 0.4670(2) 0.42939(12) 0.0490(7) Uani 1 1 d . . . . .
H48A H 0.4931 0.4853 0.4278 0.073 Uiso 1 1 calc R U . . .
H48B H 0.4182 0.5346 0.4234 0.073 Uiso 1 1 calc R U . . .
H48C H 0.4523 0.4355 0.4662 0.073 Uiso 1 1 calc R U . . .
C49 C 0.17647(11) 0.54216(16) 0.35470(9) 0.0264(5) Uani 1 1 d . . . . .
H49A H 0.1256 0.5295 0.3458 0.032 Uiso 1 1 calc R U . . .
H49B H 0.1823 0.5807 0.3222 0.032 Uiso 1 1 calc R U . . .
C50 C 0.20261(11) 0.61904(17) 0.40535(9) 0.0290(5) Uani 1 1 d . . . . .
H50A H 0.2484 0.6517 0.4080 0.035 Uiso 1 1 calc R U . . .
H50B H 0.2091 0.5764 0.4401 0.035 Uiso 1 1 calc R U . . .
C51 C 0.14879(11) 0.71135(17) 0.39894(10) 0.0326(5) Uani 1 1 d . . . . .
H51A H 0.1386 0.7471 0.3619 0.039 Uiso 1 1 calc R U . . .
H51B H 0.1046 0.6778 0.3997 0.039 Uiso 1 1 calc R U . . .
C52 C 0.17248(12) 0.79984(18) 0.44407(10) 0.0368(5) Uani 1 1 d . . . . .
H52A H 0.1356 0.8562 0.4374 0.055 Uiso 1 1 calc R U . . .
H52B H 0.1816 0.7656 0.4809 0.055 Uiso 1 1 calc R U . . .
H52C H 0.2156 0.8349 0.4431 0.055 Uiso 1 1 calc R U . . .
C53 C 0.20195(11) 0.36063(17) 0.40776(8) 0.0260(4) Uani 1 1 d . . . . .
H53A H 0.2183 0.2839 0.4052 0.031 Uiso 1 1 calc R U . . .
H53B H 0.2321 0.3915 0.4443 0.031 Uiso 1 1 calc R U . . .
C54 C 0.12708(11) 0.35507(18) 0.40724(9) 0.0296(5) Uani 1 1 d . . . . .
H54A H 0.0956 0.3277 0.3703 0.036 Uiso 1 1 calc R U . . .
H54B H 0.1112 0.4304 0.4131 0.036 Uiso 1 1 calc R U . . .
C55 C 0.12292(12) 0.27739(19) 0.45330(9) 0.0339(5) Uani 1 1 d . . . . .
H55A H 0.1427 0.2039 0.4493 0.041 Uiso 1 1 calc R U . . .
H55B H 0.1512 0.3082 0.4904 0.041 Uiso 1 1 calc R U . . .
C56 C 0.04722(13) 0.2634(2) 0.44999(10) 0.0478(7) Uani 1 1 d . . . . .
H56A H 0.0455 0.2133 0.4799 0.072 Uiso 1 1 calc R U . . .
H56B H 0.0279 0.3360 0.4545 0.072 Uiso 1 1 calc R U . . .
H56C H 0.0194 0.2319 0.4135 0.072 Uiso 1 1 calc R U . . .
S1 S 0.24387(3) 0.64602(4) 0.23503(2) 0.02254(12) Uani 1 1 d . . . . .
O5 O 0.26870(7) 0.69994(12) 0.19287(6) 0.0288(3) Uani 1 1 d . . . . .
O6A O 0.17579(10) 0.68938(16) 0.23124(8) 0.0296(4) Uani 0.75 1 d . . P C 1
O7A O 0.24432(11) 0.52645(15) 0.22911(9) 0.0299(5) Uani 0.75 1 d . . P C 1
O8A O 0.29696(10) 0.67590(16) 0.29259(8) 0.0295(4) Uani 0.75 1 d . . P C 1
O6B O 0.1645(3) 0.6117(5) 0.2013(2) 0.0275(7) Uiso 0.25 1 d . U P C 2
O7B O 0.2831(3) 0.5477(5) 0.2579(3) 0.0275(7) Uiso 0.25 1 d . U P C 2
O8B O 0.2377(3) 0.7227(5) 0.2768(2) 0.0275(7) Uiso 0.25 1 d . U P C 2
O1W O 0.04198(10) 0.64687(14) 0.24164(7) 0.0389(4) Uani 1 1 d . . . . .
H1WA H 0.0027(19) 0.633(3) 0.2115(15) 0.082(11) Uiso 1 1 d . . . . .
H1WB H 0.0763(16) 0.649(2) 0.2264(12) 0.061(9) Uiso 1 1 d . . . . .
O2W O 0.42756(11) 0.60190(18) 0.28175(9) 0.0556(5) Uani 1 1 d . . . . .
H2WA H 0.466(2) 0.580(4) 0.3174(19) 0.132(17) Uiso 1 1 d . . . . .
H2WB H 0.384(2) 0.604(4) 0.2871(18) 0.128(16) 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
O1 C2 1.228(3) . ?
O2 C3 1.230(3) . ?
O3 C14 1.232(2) . ?
O4 C15 1.231(2) . ?
N1 C1 1.330(3) . ?
N1 C24 1.471(3) . ?
N1 H1N 0.8800 . ?
N2 C4 1.334(3) . ?
N2 C5 1.463(3) . ?
N2 H2N 0.8800 . ?
N3 C13 1.321(2) . ?
N3 C12 1.464(2) . ?
N3 H3N 0.8800 . ?
N4 C16 1.334(2) . ?
N4 C17 1.470(3) . ?
N4 H4N 0.8800 . ?
C1 C4 1.414(3) . ?
C1 C2 1.475(3) . ?
C2 C3 1.510(3) . ?
C3 C4 1.468(3) . ?
C5 C6 1.514(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.387(3) . ?
C6 C11 1.395(3) . ?
C7 C8 1.382(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.389(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.389(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.389(3) . ?
C10 C12 1.513(3) . ?
C11 H11 0.9500 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C16 1.417(3) . ?
C13 C14 1.475(3) . ?
C14 C15 1.513(3) . ?
C15 C16 1.467(3) . ?
C17 C18 1.512(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C23 1.387(3) . ?
C18 C19 1.393(3) . ?
C19 C20 1.390(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.386(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.390(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.394(3) . ?
C22 C24 1.513(3) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
N5 C37 1.517(3) . ?
N5 C33 1.521(3) . ?
N5 C29 1.521(3) . ?
N5 C25 1.527(3) . ?
C25 C26 1.519(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.521(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.522(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.523(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.535(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.517(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.509(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.453(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.469(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38A 1.461(4) . ?
C37 C38B 1.673(8) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38A C39A 1.517(5) . ?
C38A H38A 0.9900 . ?
C38A H38B 0.9900 . ?
C39A C40A 1.505(5) . ?
C39A H39A 0.9900 . ?
C39A H39B 0.9900 . ?
C40A H40A 0.9800 . ?
C40A H40B 0.9800 . ?
C40A H40C 0.9800 . ?
C38B C39B 1.567(11) . ?
C38B H38C 0.9900 . ?
C38B H38D 0.9900 . ?
C39B C40B 1.489(11) . ?
C39B H39C 0.9900 . ?
C39B H39D 0.9900 . ?
C40B H40D 0.9800 . ?
C40B H40E 0.9800 . ?
C40B H40F 0.9800 . ?
N6 C53 1.520(3) . ?
N6 C49 1.522(2) . ?
N6 C45 1.530(3) . ?
N6 C41 1.536(3) . ?
C41 C42 1.519(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.524(3) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.529(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.524(3) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.539(3) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.495(3) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.523(3) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.526(3) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.516(3) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.517(3) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.524(3) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.519(3) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
S1 O7B 1.431(6) . ?
S1 O8B 1.445(6) . ?
S1 O7A 1.4459(19) . ?
S1 O6A 1.4490(19) . ?
S1 O5 1.4838(14) . ?
S1 O8A 1.528(2) . ?
S1 O6B 1.594(6) . ?
O1W H1WA 0.91(4) . ?
O1W H1WB 0.91(3) . ?
O2W H2WA 1.00(5) . ?
O2W H2WB 0.95(5) . ?

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
C1 N1 C24 121.31(17) . . ?
C1 N1 H1N 119.3 . . ?
C24 N1 H1N 119.3 . . ?
C4 N2 C5 121.85(18) . . ?
C4 N2 H2N 119.1 . . ?
C5 N2 H2N 119.1 . . ?
C13 N3 C12 123.28(16) . . ?
C13 N3 H3N 118.4 . . ?
C12 N3 H3N 118.4 . . ?
C16 N4 C17 120.60(17) . . ?
C16 N4 H4N 119.7 . . ?
C17 N4 H4N 119.7 . . ?
N1 C1 C4 133.45(19) . . ?
N1 C1 C2 134.62(19) . . ?
C4 C1 C2 91.86(17) . . ?
O1 C2 C1 135.8(2) . . ?
O1 C2 C3 136.4(2) . . ?
C1 C2 C3 87.87(16) . . ?
O2 C3 C4 135.4(2) . . ?
O2 C3 C2 136.2(2) . . ?
C4 C3 C2 88.38(16) . . ?
N2 C4 C1 132.38(19) . . ?
N2 C4 C3 135.66(19) . . ?
C1 C4 C3 91.89(17) . . ?
N2 C5 C6 113.23(17) . . ?
N2 C5 H5A 108.9 . . ?
C6 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
C6 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
C7 C6 C11 119.0(2) . . ?
C7 C6 C5 120.25(19) . . ?
C11 C6 C5 120.67(19) . . ?
C8 C7 C6 120.4(2) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C9 120.3(2) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C8 C9 C10 120.2(2) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C9 C10 C11 119.05(19) . . ?
C9 C10 C12 120.20(18) . . ?
C11 C10 C12 120.73(18) . . ?
C10 C11 C6 121.05(19) . . ?
C10 C11 H11 119.5 . . ?
C6 C11 H11 119.5 . . ?
N3 C12 C10 112.75(15) . . ?
N3 C12 H12A 109.0 . . ?
C10 C12 H12A 109.0 . . ?
N3 C12 H12B 109.0 . . ?
C10 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
N3 C13 C16 132.16(18) . . ?
N3 C13 C14 136.47(18) . . ?
C16 C13 C14 91.37(15) . . ?
O3 C14 C13 135.78(19) . . ?
O3 C14 C15 135.95(18) . . ?
C13 C14 C15 88.27(15) . . ?
O4 C15 C16 135.70(19) . . ?
O4 C15 C14 136.25(18) . . ?
C16 C15 C14 88.02(15) . . ?
N4 C16 C13 132.87(18) . . ?
N4 C16 C15 134.75(18) . . ?
C13 C16 C15 92.34(15) . . ?
N4 C17 C18 110.86(16) . . ?
N4 C17 H17A 109.5 . . ?
C18 C17 H17A 109.5 . . ?
N4 C17 H17B 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 108.1 . . ?
C23 C18 C19 118.80(19) . . ?
C23 C18 C17 119.17(18) . . ?
C19 C18 C17 121.99(18) . . ?
C20 C19 C18 120.0(2) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C21 C20 C19 120.8(2) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C20 C21 C22 119.67(19) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
C21 C22 C23 119.25(19) . . ?
C21 C22 C24 121.79(18) . . ?
C23 C22 C24 118.89(18) . . ?
C18 C23 C22 121.44(19) . . ?
C18 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
N1 C24 C22 110.14(15) . . ?
N1 C24 H24A 109.6 . . ?
C22 C24 H24A 109.6 . . ?
N1 C24 H24B 109.6 . . ?
C22 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
C37 N5 C33 110.91(16) . . ?
C37 N5 C29 105.71(15) . . ?
C33 N5 C29 111.53(15) . . ?
C37 N5 C25 111.53(16) . . ?
C33 N5 C25 105.98(15) . . ?
C29 N5 C25 111.28(16) . . ?
C26 C25 N5 115.60(17) . . ?
C26 C25 H25A 108.4 . . ?
N5 C25 H25A 108.4 . . ?
C26 C25 H25B 108.4 . . ?
N5 C25 H25B 108.4 . . ?
H25A C25 H25B 107.4 . . ?
C25 C26 C27 109.80(19) . . ?
C25 C26 H26A 109.7 . . ?
C27 C26 H26A 109.7 . . ?
C25 C26 H26B 109.7 . . ?
C27 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
C26 C27 C28 113.3(2) . . ?
C26 C27 H27A 108.9 . . ?
C28 C27 H27A 108.9 . . ?
C26 C27 H27B 108.9 . . ?
C28 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N5 C29 C30 114.79(16) . . ?
N5 C29 H29A 108.6 . . ?
C30 C29 H29A 108.6 . . ?
N5 C29 H29B 108.6 . . ?
C30 C29 H29B 108.6 . . ?
H29A C29 H29B 107.5 . . ?
C29 C30 C31 110.26(17) . . ?
C29 C30 H30A 109.6 . . ?
C31 C30 H30A 109.6 . . ?
C29 C30 H30B 109.6 . . ?
C31 C30 H30B 109.6 . . ?
H30A C30 H30B 108.1 . . ?
C32 C31 C30 113.28(18) . . ?
C32 C31 H31A 108.9 . . ?
C30 C31 H31A 108.9 . . ?
C32 C31 H31B 108.9 . . ?
C30 C31 H31B 108.9 . . ?
H31A C31 H31B 107.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 N5 116.09(16) . . ?
C34 C33 H33A 108.3 . . ?
N5 C33 H33A 108.3 . . ?
C34 C33 H33B 108.3 . . ?
N5 C33 H33B 108.3 . . ?
H33A C33 H33B 107.4 . . ?
C35 C34 C33 113.0(2) . . ?
C35 C34 H34A 109.0 . . ?
C33 C34 H34A 109.0 . . ?
C35 C34 H34B 109.0 . . ?
C33 C34 H34B 109.0 . . ?
H34A C34 H34B 107.8 . . ?
C34 C35 C36 122.2(2) . . ?
C34 C35 H35A 106.8 . . ?
C36 C35 H35A 106.8 . . ?
C34 C35 H35B 106.8 . . ?
C36 C35 H35B 106.8 . . ?
H35A C35 H35B 106.6 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38A C37 N5 113.3(2) . . ?
N5 C37 C38B 116.3(3) . . ?
C38A C37 H37A 108.9 . . ?
N5 C37 H37A 108.9 . . ?
C38A C37 H37B 108.9 . . ?
N5 C37 H37B 108.9 . . ?
H37A C37 H37B 107.7 . . ?
C37 C38A C39A 110.4(3) . . ?
C37 C38A H38A 109.6 . . ?
C39A C38A H38A 109.6 . . ?
C37 C38A H38B 109.6 . . ?
C39A C38A H38B 109.6 . . ?
H38A C38A H38B 108.1 . . ?
C40A C39A C38A 111.7(3) . . ?
C40A C39A H39A 109.3 . . ?
C38A C39A H39A 109.3 . . ?
C40A C39A H39B 109.3 . . ?
C38A C39A H39B 109.3 . . ?
H39A C39A H39B 107.9 . . ?
C39A C40A H40A 109.5 . . ?
C39A C40A H40B 109.5 . . ?
H40A C40A H40B 109.5 . . ?
C39A C40A H40C 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
C39B C38B C37 112.4(6) . . ?
C39B C38B H38C 109.1 . . ?
C37 C38B H38C 109.1 . . ?
C39B C38B H38D 109.1 . . ?
C37 C38B H38D 109.1 . . ?
H38C C38B H38D 107.8 . . ?
C40B C39B C38B 110.5(7) . . ?
C40B C39B H39C 109.5 . . ?
C38B C39B H39C 109.5 . . ?
C40B C39B H39D 109.5 . . ?
C38B C39B H39D 109.5 . . ?
H39C C39B H39D 108.1 . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
H40D C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
C53 N6 C49 112.07(15) . . ?
C53 N6 C45 108.69(15) . . ?
C49 N6 C45 107.36(15) . . ?
C53 N6 C41 112.61(15) . . ?
C49 N6 C41 108.71(14) . . ?
C45 N6 C41 107.15(15) . . ?
C42 C41 N6 118.35(16) . . ?
C42 C41 H41A 107.7 . . ?
N6 C41 H41A 107.7 . . ?
C42 C41 H41B 107.7 . . ?
N6 C41 H41B 107.7 . . ?
H41A C41 H41B 107.1 . . ?
C41 C42 C43 110.29(17) . . ?
C41 C42 H42A 109.6 . . ?
C43 C42 H42A 109.6 . . ?
C41 C42 H42B 109.6 . . ?
C43 C42 H42B 109.6 . . ?
H42A C42 H42B 108.1 . . ?
C42 C43 C44 111.17(17) . . ?
C42 C43 H43A 109.4 . . ?
C44 C43 H43A 109.4 . . ?
C42 C43 H43B 109.4 . . ?
C44 C43 H43B 109.4 . . ?
H43A C43 H43B 108.0 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 N6 116.13(17) . . ?
C46 C45 H45A 108.3 . . ?
N6 C45 H45A 108.3 . . ?
C46 C45 H45B 108.3 . . ?
N6 C45 H45B 108.3 . . ?
H45A C45 H45B 107.4 . . ?
C45 C46 C47 109.66(18) . . ?
C45 C46 H46A 109.7 . . ?
C47 C46 H46A 109.7 . . ?
C45 C46 H46B 109.7 . . ?
C47 C46 H46B 109.7 . . ?
H46A C46 H46B 108.2 . . ?
C48 C47 C46 114.2(2) . . ?
C48 C47 H47A 108.7 . . ?
C46 C47 H47A 108.7 . . ?
C48 C47 H47B 108.7 . . ?
C46 C47 H47B 108.7 . . ?
H47A C47 H47B 107.6 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N6 C49 C50 115.69(16) . . ?
N6 C49 H49A 108.4 . . ?
C50 C49 H49A 108.4 . . ?
N6 C49 H49B 108.4 . . ?
C50 C49 H49B 108.4 . . ?
H49A C49 H49B 107.4 . . ?
C49 C50 C51 108.99(17) . . ?
C49 C50 H50A 109.9 . . ?
C51 C50 H50A 109.9 . . ?
C49 C50 H50B 109.9 . . ?
C51 C50 H50B 109.9 . . ?
H50A C50 H50B 108.3 . . ?
C52 C51 C50 113.77(18) . . ?
C52 C51 H51A 108.8 . . ?
C50 C51 H51A 108.8 . . ?
C52 C51 H51B 108.8 . . ?
C50 C51 H51B 108.8 . . ?
H51A C51 H51B 107.7 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C54 C53 N6 115.62(16) . . ?
C54 C53 H53A 108.4 . . ?
N6 C53 H53A 108.4 . . ?
C54 C53 H53B 108.4 . . ?
N6 C53 H53B 108.4 . . ?
H53A C53 H53B 107.4 . . ?
C53 C54 C55 110.12(17) . . ?
C53 C54 H54A 109.6 . . ?
C55 C54 H54A 109.6 . . ?
C53 C54 H54B 109.6 . . ?
C55 C54 H54B 109.6 . . ?
H54A C54 H54B 108.2 . . ?
C56 C55 C54 110.56(18) . . ?
C56 C55 H55A 109.5 . . ?
C54 C55 H55A 109.5 . . ?
C56 C55 H55B 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 108.1 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
O7B S1 O8B 114.0(3) . . ?
O7A S1 O6A 113.04(12) . . ?
O7B S1 O5 111.9(2) . . ?
O8B S1 O5 113.0(2) . . ?
O7A S1 O5 110.06(10) . . ?
O6A S1 O5 110.55(10) . . ?
O7A S1 O8A 107.80(12) . . ?
O6A S1 O8A 108.51(11) . . ?
O5 S1 O8A 106.62(10) . . ?
O7B S1 O6B 108.7(3) . . ?
O8B S1 O6B 103.3(3) . . ?
O5 S1 O6B 105.0(2) . . ?
H1WA O1W H1WB 103(3) . . ?
H2WA O2W H2WB 110(3) . . ?

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
C24 N1 C1 C4 -167.8(2) . . . . ?
C24 N1 C1 C2 16.1(3) . . . . ?
N1 C1 C2 O1 -2.0(4) . . . . ?
C4 C1 C2 O1 -179.2(3) . . . . ?
N1 C1 C2 C3 176.8(2) . . . . ?
C4 C1 C2 C3 -0.39(15) . . . . ?
O1 C2 C3 O2 0.1(5) . . . . ?
C1 C2 C3 O2 -178.7(3) . . . . ?
O1 C2 C3 C4 179.2(3) . . . . ?
C1 C2 C3 C4 0.38(15) . . . . ?
C5 N2 C4 C1 170.1(2) . . . . ?
C5 N2 C4 C3 -13.9(3) . . . . ?
N1 C1 C4 N2 0.4(4) . . . . ?
C2 C1 C4 N2 177.6(2) . . . . ?
N1 C1 C4 C3 -176.8(2) . . . . ?
C2 C1 C4 C3 0.41(16) . . . . ?
O2 C3 C4 N2 1.6(4) . . . . ?
C2 C3 C4 N2 -177.5(2) . . . . ?
O2 C3 C4 C1 178.7(2) . . . . ?
C2 C3 C4 C1 -0.40(15) . . . . ?
C4 N2 C5 C6 -92.6(2) . . . . ?
N2 C5 C6 C7 136.5(2) . . . . ?
N2 C5 C6 C11 -45.6(3) . . . . ?
C11 C6 C7 C8 0.0(3) . . . . ?
C5 C6 C7 C8 177.9(2) . . . . ?
C6 C7 C8 C9 0.9(4) . . . . ?
C7 C8 C9 C10 -0.9(4) . . . . ?
C8 C9 C10 C11 0.1(3) . . . . ?
C8 C9 C10 C12 -178.4(2) . . . . ?
C9 C10 C11 C6 0.8(3) . . . . ?
C12 C10 C11 C6 179.33(18) . . . . ?
C7 C6 C11 C10 -0.9(3) . . . . ?
C5 C6 C11 C10 -178.77(18) . . . . ?
C13 N3 C12 C10 104.9(2) . . . . ?
C9 C10 C12 N3 -135.97(19) . . . . ?
C11 C10 C12 N3 45.6(2) . . . . ?
C12 N3 C13 C16 -172.14(19) . . . . ?
C12 N3 C13 C14 9.0(3) . . . . ?
N3 C13 C14 O3 0.0(4) . . . . ?
C16 C13 C14 O3 -179.2(2) . . . . ?
N3 C13 C14 C15 179.3(2) . . . . ?
C16 C13 C14 C15 0.14(14) . . . . ?
O3 C14 C15 O4 0.7(4) . . . . ?
C13 C14 C15 O4 -178.6(2) . . . . ?
O3 C14 C15 C16 179.2(2) . . . . ?
C13 C14 C15 C16 -0.14(14) . . . . ?
C17 N4 C16 C13 161.40(19) . . . . ?
C17 N4 C16 C15 -21.4(3) . . . . ?
N3 C13 C16 N4 -1.4(4) . . . . ?
C14 C13 C16 N4 177.8(2) . . . . ?
N3 C13 C16 C15 -179.4(2) . . . . ?
C14 C13 C16 C15 -0.15(15) . . . . ?
O4 C15 C16 N4 0.7(4) . . . . ?
C14 C15 C16 N4 -177.8(2) . . . . ?
O4 C15 C16 C13 178.6(2) . . . . ?
C14 C15 C16 C13 0.15(14) . . . . ?
C16 N4 C17 C18 -90.0(2) . . . . ?
N4 C17 C18 C23 -65.2(2) . . . . ?
N4 C17 C18 C19 112.4(2) . . . . ?
C23 C18 C19 C20 -0.9(3) . . . . ?
C17 C18 C19 C20 -178.55(19) . . . . ?
C18 C19 C20 C21 1.1(3) . . . . ?
C19 C20 C21 C22 -0.4(3) . . . . ?
C20 C21 C22 C23 -0.4(3) . . . . ?
C20 C21 C22 C24 176.56(19) . . . . ?
C19 C18 C23 C22 0.0(3) . . . . ?
C17 C18 C23 C22 177.76(17) . . . . ?
C21 C22 C23 C18 0.6(3) . . . . ?
C24 C22 C23 C18 -176.44(17) . . . . ?
C1 N1 C24 C22 84.9(2) . . . . ?
C21 C22 C24 N1 -111.5(2) . . . . ?
C23 C22 C24 N1 65.5(2) . . . . ?
C37 N5 C25 C26 54.1(2) . . . . ?
C33 N5 C25 C26 174.87(18) . . . . ?
C29 N5 C25 C26 -63.7(2) . . . . ?
N5 C25 C26 C27 174.63(19) . . . . ?
C25 C26 C27 C28 178.4(2) . . . . ?
C37 N5 C29 C30 -178.58(18) . . . . ?
C33 N5 C29 C30 60.8(2) . . . . ?
C25 N5 C29 C30 -57.3(2) . . . . ?
N5 C29 C30 C31 -167.34(17) . . . . ?
C29 C30 C31 C32 71.0(3) . . . . ?
C37 N5 C33 C34 -62.6(2) . . . . ?
C29 N5 C33 C34 55.0(2) . . . . ?
C25 N5 C33 C34 176.2(2) . . . . ?
N5 C33 C34 C35 174.1(2) . . . . ?
C33 C34 C35 C36 -177.3(3) . . . . ?
C33 N5 C37 C38A -60.6(3) . . . . ?
C29 N5 C37 C38A 178.4(2) . . . . ?
C25 N5 C37 C38A 57.3(3) . . . . ?
C33 N5 C37 C38B -39.7(4) . . . . ?
C29 N5 C37 C38B -160.7(3) . . . . ?
C25 N5 C37 C38B 78.2(4) . . . . ?
N5 C37 C38A C39A -161.1(3) . . . . ?
C37 C38A C39A C40A -172.0(3) . . . . ?
N5 C37 C38B C39B -173.6(5) . . . . ?
C37 C38B C39B C40B 78.9(7) . . . . ?
C53 N6 C41 C42 81.0(2) . . . . ?
C49 N6 C41 C42 -43.8(2) . . . . ?
C45 N6 C41 C42 -159.50(17) . . . . ?
N6 C41 C42 C43 164.94(17) . . . . ?
C41 C42 C43 C44 -175.02(18) . . . . ?
C53 N6 C45 C46 60.4(2) . . . . ?
C49 N6 C45 C46 -178.20(17) . . . . ?
C41 N6 C45 C46 -61.6(2) . . . . ?
N6 C45 C46 C47 167.29(18) . . . . ?
C45 C46 C47 C48 56.4(3) . . . . ?
C53 N6 C49 C50 62.4(2) . . . . ?
C45 N6 C49 C50 -56.9(2) . . . . ?
C41 N6 C49 C50 -172.50(17) . . . . ?
N6 C49 C50 C51 -163.86(17) . . . . ?
C49 C50 C51 C52 -174.16(18) . . . . ?
C49 N6 C53 C54 47.1(2) . . . . ?
C45 N6 C53 C54 165.57(17) . . . . ?
C41 N6 C53 C54 -75.9(2) . . . . ?
N6 C53 C54 C55 176.15(17) . . . . ?
C53 C54 C55 C56 -175.13(19) . . . . ?

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 H1N O5 0.88 2.09 2.847(2) 143.4 .
N2 H2N O5 0.88 1.95 2.745(2) 148.7 .
N3 H3N O6A 0.88 1.94 2.801(2) 165.4 .
N3 H3N O8B 0.88 2.04 2.846(6) 151.2 .
N4 H4N O8A 0.88 2.08 2.881(2) 151.5 .
N4 H4N O8B 0.88 1.85 2.633(6) 146.8 .
C12 H12B O1W 0.99 2.62 3.414(3) 137.7 .
C17 H17B O4 0.99 2.63 3.342(3) 128.9 .
C25 H25B O7A 0.99 2.31 3.281(3) 164.8 .
C25 H25B O7B 0.99 2.59 3.549(6) 162.0 .
C29 H29A O4 0.99 2.61 3.543(2) 157.1 4_575
C29 H29B O2 0.99 2.56 3.525(3) 165.4 1_545
C30 H30A O1 0.99 2.61 3.321(3) 128.5 1_545
C38A H38B O7A 0.99 2.42 3.361(5) 158.5 .
C38B H38C O6B 0.99 2.58 3.490(10) 152.3 .
C41 H41A O7A 0.99 2.24 3.180(3) 158.9 .
C41 H41A O7B 0.99 2.46 3.372(6) 153.0 .
C42 H42A O1W 0.99 2.59 3.548(3) 163.6 .
C45 H45A O8A 0.99 2.53 3.464(3) 157.1 .
C45 H45A O7B 0.99 2.25 3.176(6) 155.2 .
C49 H49B S1 0.99 3.01 3.950(2) 160.0 .
C49 H49B O6A 0.99 2.62 3.601(3) 170.7 .
C49 H49B O8B 0.99 2.53 3.450(6) 153.7 .
C53 H53A O4 0.99 2.49 3.463(2) 165.9 1_545
C53 H53B O2 0.99 2.45 3.397(2) 159.2 4_576
O1W H1WA O3 0.91(4) 2.10(4) 2.951(2) 155(3) 2_545
O1W H1WB O6A 0.91(3) 2.04(3) 2.866(3) 151(3) .
O1W H1WB O6B 0.91(3) 2.15(3) 3.033(6) 165(3) .
O2W H2WA O1 1.00(5) 2.01(5) 2.938(3) 153(4) 2_645
O2W H2WB S1 0.95(5) 2.73(5) 3.538(2) 144(3) .
O2W H2WB O8A 0.95(5) 2.01(5) 2.900(3) 156(4) .
O2W H2WB O7B 0.95(5) 2.03(5) 2.856(7) 144(4) .

_refine_diff_density_max         0.517
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.045


####################################################################### 
# 
# 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_kaj15pt1_s1423
_database_code_depnum_ccdc_archive 'CCDC 1457415'
_audit_update_record             
;
2016-03-03 deposited with the CCDC.
2016-04-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H48 N4 O14'
_chemical_formula_weight         808.82

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'


_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.0434(3)
_cell_length_b                   8.9035(5)
_cell_length_c                   20.1417(10)
_cell_angle_alpha                101.174(5)
_cell_angle_beta                 91.268(4)
_cell_angle_gamma                107.342(5)
_cell_volume                     1011.20(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    5084
_cell_measurement_theta_min      4.4700
_cell_measurement_theta_max      75.0670

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_F_000             428
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  CrysAlisPro, Agilent Technologies,
  Version 1.171.37.35
  Empirical absorption correction using spherical 
  harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;


_diffrn_crystal_treatment        
;
attached with Exxon Paratone N to a nylon loop and quenched 
in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. 
;


_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.5861
_diffrn_reflns_number            9488
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         4.492
_diffrn_reflns_theta_max         76.288
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9488
_reflns_number_gt                4992
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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.
;

_computing_data_collection       
;
  CrysAlisPro, Agilent Technologies,
;
_computing_cell_refinement       
;
  CrysAlisPro, Agilent Technologies,
;
_computing_data_reduction        
;
  CrysAlisPro, Agilent Technologies,
;

_computing_structure_solution    'ShelxT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
  ORTEP3 for Windows (Farrugia, L., 1997)
  ORTEPIII  (Burnett, N.M., Johnson,C.K., 1996). 
  WinGX (Farrugia, 1999)
  shelXle (Hï?1/2bschle,C.B., et al., 2011) 
;
_computing_publication_material  ?

_cell_oxdiff_twin_number         2
loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 0.9948 -0.0101 0.0016 0.0191 0.9941 -0.0195 0.0220 0.1060 1.0089

_diffrn_orient_matrix_UB_11      -0.1780364000
_diffrn_orient_matrix_UB_12      -0.1636158000
_diffrn_orient_matrix_UB_13      -0.0325164000
_diffrn_orient_matrix_UB_21      0.0523146000
_diffrn_orient_matrix_UB_22      -0.0695655000
_diffrn_orient_matrix_UB_23      0.0607347000
_diffrn_orient_matrix_UB_31      -0.1934133000
_diffrn_orient_matrix_UB_32      0.0525825000
_diffrn_orient_matrix_UB_33      0.0371070000
_diffrn_oxdiff_twin_integration_method simultaneous
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.6560 16540 6349
2 0.3440 16245 6349


_refine_special_details          
;
 Refined as a 2-component twin/split crystal with
 a rotation of 2.6667 degrees around the following vectors: 
 Reciprocal space (hkl): 0.6691 -0.1944 0.7173
 Direct space (uvw)    : 0.9868 0.1223 0.1061
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.03P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9488
_refine_ls_number_parameters     301
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0509
_refine_ls_wR_factor_ref         0.1096
_refine_ls_wR_factor_gt          0.1016
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_restrained_S_all      1.176
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
O1 O 0.4846(3) 0.2381(2) -0.12894(9) 0.0397(4) Uani 1 1 d . . . . .
O2 O 0.4519(3) 0.1721(2) 0.02377(9) 0.0371(4) Uani 1 1 d . . . . .
O3 O 0.2280(3) 0.1375(2) 0.23827(9) 0.0415(4) Uani 1 1 d . . . . .
O4 O 0.3176(3) 0.3952(2) 0.29423(8) 0.0364(4) Uani 1 1 d . . . . .
O5 O 0.2352(4) 0.5494(3) 0.42773(10) 0.0634(7) Uani 1 1 d . . . . .
N1 N 1.0241(3) 0.2383(2) -0.12544(10) 0.0310(4) Uani 1 1 d . . . . .
H1N H 1.182(6) 0.235(4) -0.1086(15) 0.057(9) Uiso 1 1 d . . . . .
N2 N 1.0005(3) 0.1824(2) 0.03015(10) 0.0306(4) Uani 1 1 d . . . . .
H2N H 1.137(5) 0.184(3) 0.0172(14) 0.050(9) Uiso 1 1 d . . . . .
C1 C 0.8626(4) 0.2238(3) -0.08210(12) 0.0293(5) Uani 1 1 d . . . . .
C2 C 0.6208(4) 0.2231(3) -0.08533(13) 0.0329(5) Uani 1 1 d . . . . .
C3 C 0.6066(4) 0.1941(3) -0.01558(12) 0.0313(5) Uani 1 1 d . . . . .
C4 C 0.8501(4) 0.1974(3) -0.01477(12) 0.0289(5) Uani 1 1 d . . . . .
C5 C 0.9369(4) 0.1421(3) 0.09534(12) 0.0325(5) Uani 1 1 d . . . . .
H5A H 1.0737 0.1301 0.1192 0.039 Uiso 1 1 calc R U . . .
H5B H 0.8127 0.0371 0.0872 0.039 Uiso 1 1 calc R U . . .
C6 C 0.8530(4) 0.2665(3) 0.14064(11) 0.0303(5) Uani 1 1 d . . . . .
C7 C 0.6529(4) 0.2186(3) 0.17414(12) 0.0312(5) Uani 1 1 d . . . . .
H7 H 0.5712 0.1073 0.1690 0.037 Uiso 1 1 calc R U . . .
C8 C 0.5713(4) 0.3327(3) 0.21520(12) 0.0310(5) Uani 1 1 d . . . . .
C9 C 0.6887(4) 0.4965(3) 0.22162(12) 0.0312(5) Uani 1 1 d . . . . .
H9 H 0.6315 0.5744 0.2487 0.037 Uiso 1 1 calc R U . . .
C10 C 0.8884(4) 0.5457(3) 0.18871(12) 0.0300(5) Uani 1 1 d . . . . .
C11 C 0.9706(4) 0.4295(3) 0.14923(11) 0.0307(5) Uani 1 1 d . . . . .
H11 H 1.1101 0.4630 0.1278 0.037 Uiso 1 1 calc R U . . .
C12 C 1.0106(4) 0.7218(3) 0.19152(12) 0.0317(5) Uani 1 1 d . . . . .
H12A H 0.9485 0.7882 0.2269 0.038 Uiso 1 1 calc R U . . .
H12B H 1.1790 0.7463 0.2038 0.038 Uiso 1 1 calc R U . . .
C13 C 0.3557(4) 0.2753(3) 0.24925(12) 0.0331(5) Uani 1 1 d . . . . .
C14 C 0.1029(4) 0.3535(3) 0.32652(13) 0.0390(6) Uani 1 1 d . . . . .
H14A H 0.1051 0.2751 0.3551 0.047 Uiso 1 1 calc R U . . .
H14B H -0.0308 0.3044 0.2918 0.047 Uiso 1 1 calc R U . . .
C15 C 0.0816(5) 0.5035(4) 0.36898(14) 0.0505(7) Uani 1 1 d . . . . .
H15A H 0.1186 0.5902 0.3429 0.061 Uiso 1 1 calc R U . . .
H15B H -0.0801 0.4858 0.3817 0.061 Uiso 1 1 calc R U . . .
O6A O 0.3033(5) 0.8571(3) 0.57728(12) 0.0430(6) Uani 0.7 1 d . . P A 1
O7A O 0.4456(5) 1.1846(3) 0.67081(14) 0.0483(7) Uani 0.7 1 d . . P A 1
C16A C 0.1857(8) 0.6899(5) 0.46946(19) 0.0437(9) Uani 0.7 1 d . . P A 1
H16A H 0.0259 0.6597 0.4840 0.052 Uiso 0.7 1 calc R U P A 1
H16B H 0.2051 0.7774 0.4442 0.052 Uiso 0.7 1 calc R U P A 1
C17A C 0.3645(7) 0.7398(5) 0.52938(19) 0.0425(9) Uani 0.7 1 d . . P A 1
H17A H 0.3626 0.6460 0.5492 0.051 Uiso 0.7 1 calc R U P A 1
H17B H 0.5222 0.7858 0.5153 0.051 Uiso 0.7 1 calc R U P A 1
C18A C 0.4497(7) 0.9068(5) 0.63944(18) 0.0422(9) Uani 0.7 1 d . . P A 1
H18A H 0.6137 0.9513 0.6299 0.051 Uiso 0.7 1 calc R U P A 1
H18B H 0.4370 0.8125 0.6600 0.051 Uiso 0.7 1 calc R U P A 1
C19A C 0.3814(7) 1.0314(4) 0.68822(18) 0.0433(9) Uani 0.7 1 d . . P A 1
H19A H 0.2106 0.9941 0.6904 0.052 Uiso 0.7 1 calc R U P A 1
H19B H 0.4549 1.0423 0.7340 0.052 Uiso 0.7 1 calc R U P A 1
C20A C 0.2792(8) 1.2032(5) 0.6246(2) 0.0502(10) Uani 0.7 1 d . . P A 1
H20A H 0.2758 1.1337 0.5802 0.075 Uiso 0.7 1 calc R U P A 1
H20B H 0.3221 1.3156 0.6200 0.075 Uiso 0.7 1 calc R U P A 1
H20C H 0.1251 1.1729 0.6417 0.075 Uiso 0.7 1 calc R U P A 1
O6B O 0.4349(13) 0.7783(9) 0.6064(4) 0.0603(19) Uiso 0.3 1 d . . P A 2
O7B O 0.2484(17) 1.0286(11) 0.5773(5) 0.082(3) Uiso 0.3 1 d . . P A 2
C16B C 0.282(2) 0.6649(14) 0.4886(6) 0.053(3) Uiso 0.3 1 d . . P A 2
H16C H 0.1309 0.6551 0.5085 0.063 Uiso 0.3 1 calc R U P A 2
H16D H 0.3316 0.7714 0.4760 0.063 Uiso 0.3 1 calc R U P A 2
C17B C 0.458(2) 0.6717(13) 0.5464(5) 0.054(2) Uiso 0.3 1 d . . P A 2
H17C H 0.4307 0.5626 0.5556 0.065 Uiso 0.3 1 calc R U P A 2
H17D H 0.6178 0.7088 0.5325 0.065 Uiso 0.3 1 calc R U P A 2
C18B C 0.560(2) 0.9423(13) 0.6097(6) 0.059(3) Uiso 0.3 1 d . . P A 2
H18C H 0.6076 0.9566 0.5641 0.071 Uiso 0.3 1 calc R U P A 2
H18D H 0.7022 0.9729 0.6409 0.071 Uiso 0.3 1 calc R U P A 2
C19B C 0.417(2) 1.0521(16) 0.6343(6) 0.073(3) Uiso 0.3 1 d . . P A 2
H19C H 0.3364 1.0227 0.6744 0.088 Uiso 0.3 1 calc R U P A 2
H19D H 0.5164 1.1656 0.6467 0.088 Uiso 0.3 1 calc R U P A 2
C20B C 0.116(3) 1.134(2) 0.5911(9) 0.115(6) Uiso 0.3 1 d . . P A 2
H20D H 0.0680 1.1378 0.6374 0.172 Uiso 0.3 1 calc R U P A 2
H20E H -0.0218 1.0971 0.5587 0.172 Uiso 0.3 1 calc R U P A 2
H20F H 0.2101 1.2424 0.5870 0.172 Uiso 0.3 1 calc R 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
O1 C2 1.243(3) . ?
O2 C3 1.234(3) . ?
O3 C13 1.213(3) . ?
O4 C13 1.339(3) . ?
O4 C14 1.445(3) . ?
O5 C16B 1.401(12) . ?
O5 C15 1.403(4) . ?
O5 C16A 1.479(4) . ?
N1 C1 1.318(3) . ?
N1 C12 1.468(3) 2_765 ?
N1 H1N 1.02(3) . ?
N2 C4 1.321(3) . ?
N2 C5 1.457(3) . ?
N2 H2N 0.87(3) . ?
C1 C4 1.420(3) . ?
C1 C2 1.460(3) . ?
C2 C3 1.477(3) . ?
C3 C4 1.463(3) . ?
C5 C6 1.510(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C11 1.387(3) . ?
C6 C7 1.393(3) . ?
C7 C8 1.397(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.397(3) . ?
C8 C13 1.486(3) . ?
C9 C10 1.386(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.398(3) . ?
C10 C12 1.510(3) . ?
C11 H11 0.9500 . ?
C12 N1 1.468(3) 2_765 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C14 C15 1.482(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
O6A C17A 1.419(4) . ?
O6A C18A 1.431(4) . ?
O7A C19A 1.418(4) . ?
O7A C20A 1.422(5) . ?
C16A C17A 1.507(6) . ?
C16A H16A 0.9900 . ?
C16A H16B 0.9900 . ?
C17A H17A 0.9900 . ?
C17A H17B 0.9900 . ?
C18A C19A 1.495(5) . ?
C18A H18A 0.9900 . ?
C18A H18B 0.9900 . ?
C19A H19A 0.9900 . ?
C19A H19B 0.9900 . ?
C20A H20A 0.9800 . ?
C20A H20B 0.9800 . ?
C20A H20C 0.9800 . ?
O6B C18B 1.417(13) . ?
O6B C17B 1.421(12) . ?
O7B C20B 1.400(17) . ?
O7B C19B 1.458(15) . ?
C16B C17B 1.540(15) . ?
C16B H16C 0.9900 . ?
C16B H16D 0.9900 . ?
C17B H17C 0.9900 . ?
C17B H17D 0.9900 . ?
C18B C19B 1.511(16) . ?
C18B H18C 0.9900 . ?
C18B H18D 0.9900 . ?
C19B H19C 0.9900 . ?
C19B H19D 0.9900 . ?
C20B H20D 0.9800 . ?
C20B H20E 0.9800 . ?
C20B H20F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 O4 C14 115.69(19) . . ?
C16B O5 C15 137.4(6) . . ?
C15 O5 C16A 105.5(3) . . ?
C1 N1 C12 122.0(2) . 2_765 ?
C1 N1 H1N 116.6(16) . . ?
C12 N1 H1N 121.0(16) 2_765 . ?
C4 N2 C5 122.9(2) . . ?
C4 N2 H2N 117.0(19) . . ?
C5 N2 H2N 119.5(19) . . ?
N1 C1 C4 134.9(2) . . ?
N1 C1 C2 134.1(2) . . ?
C4 C1 C2 91.01(18) . . ?
O1 C2 C1 135.2(2) . . ?
O1 C2 C3 135.7(2) . . ?
C1 C2 C3 89.10(19) . . ?
O2 C3 C4 136.2(2) . . ?
O2 C3 C2 135.1(2) . . ?
C4 C3 C2 88.68(18) . . ?
N2 C4 C1 133.9(2) . . ?
N2 C4 C3 134.9(2) . . ?
C1 C4 C3 91.20(19) . . ?
N2 C5 C6 113.4(2) . . ?
N2 C5 H5A 108.9 . . ?
C6 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
C6 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
C11 C6 C7 118.8(2) . . ?
C11 C6 C5 121.2(2) . . ?
C7 C6 C5 120.0(2) . . ?
C6 C7 C8 120.6(2) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C7 C8 C9 119.7(2) . . ?
C7 C8 C13 118.4(2) . . ?
C9 C8 C13 121.8(2) . . ?
C10 C9 C8 120.3(2) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 119.1(2) . . ?
C9 C10 C12 121.3(2) . . ?
C11 C10 C12 119.5(2) . . ?
C6 C11 C10 121.5(2) . . ?
C6 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
N1 C12 C10 110.29(19) 2_765 . ?
N1 C12 H12A 109.6 2_765 . ?
C10 C12 H12A 109.6 . . ?
N1 C12 H12B 109.6 2_765 . ?
C10 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
O3 C13 O4 123.4(2) . . ?
O3 C13 C8 125.0(2) . . ?
O4 C13 C8 111.6(2) . . ?
O4 C14 C15 107.7(2) . . ?
O4 C14 H14A 110.2 . . ?
C15 C14 H14A 110.2 . . ?
O4 C14 H14B 110.2 . . ?
C15 C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?
O5 C15 C14 109.5(3) . . ?
O5 C15 H15A 109.8 . . ?
C14 C15 H15A 109.8 . . ?
O5 C15 H15B 109.8 . . ?
C14 C15 H15B 109.8 . . ?
H15A C15 H15B 108.2 . . ?
C17A O6A C18A 112.3(3) . . ?
C19A O7A C20A 113.6(3) . . ?
O5 C16A C17A 103.1(3) . . ?
O5 C16A H16A 111.1 . . ?
C17A C16A H16A 111.1 . . ?
O5 C16A H16B 111.1 . . ?
C17A C16A H16B 111.1 . . ?
H16A C16A H16B 109.1 . . ?
O6A C17A C16A 106.3(3) . . ?
O6A C17A H17A 110.5 . . ?
C16A C17A H17A 110.5 . . ?
O6A C17A H17B 110.5 . . ?
C16A C17A H17B 110.5 . . ?
H17A C17A H17B 108.7 . . ?
O6A C18A C19A 110.7(3) . . ?
O6A C18A H18A 109.5 . . ?
C19A C18A H18A 109.5 . . ?
O6A C18A H18B 109.5 . . ?
C19A C18A H18B 109.5 . . ?
H18A C18A H18B 108.1 . . ?
O7A C19A C18A 113.7(3) . . ?
O7A C19A H19A 108.8 . . ?
C18A C19A H19A 108.8 . . ?
O7A C19A H19B 108.8 . . ?
C18A C19A H19B 108.8 . . ?
H19A C19A H19B 107.7 . . ?
O7A C20A H20A 109.5 . . ?
O7A C20A H20B 109.5 . . ?
H20A C20A H20B 109.5 . . ?
O7A C20A H20C 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
C18B O6B C17B 114.5(9) . . ?
C20B O7B C19B 111.2(11) . . ?
O5 C16B C17B 123.0(9) . . ?
O5 C16B H16C 106.6 . . ?
C17B C16B H16C 106.6 . . ?
O5 C16B H16D 106.6 . . ?
C17B C16B H16D 106.6 . . ?
H16C C16B H16D 106.5 . . ?
O6B C17B C16B 110.4(9) . . ?
O6B C17B H17C 109.6 . . ?
C16B C17B H17C 109.6 . . ?
O6B C17B H17D 109.6 . . ?
C16B C17B H17D 109.6 . . ?
H17C C17B H17D 108.1 . . ?
O6B C18B C19B 112.1(11) . . ?
O6B C18B H18C 109.2 . . ?
C19B C18B H18C 109.2 . . ?
O6B C18B H18D 109.2 . . ?
C19B C18B H18D 109.2 . . ?
H18C C18B H18D 107.9 . . ?
O7B C19B C18B 105.1(10) . . ?
O7B C19B H19C 110.7 . . ?
C18B C19B H19C 110.7 . . ?
O7B C19B H19D 110.7 . . ?
C18B C19B H19D 110.7 . . ?
H19C C19B H19D 108.8 . . ?
O7B C20B H20D 109.5 . . ?
O7B C20B H20E 109.5 . . ?
H20D C20B H20E 109.5 . . ?
O7B C20B H20F 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 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
C12 N1 C1 C4 -175.2(2) 2_765 . . . ?
C12 N1 C1 C2 7.3(4) 2_765 . . . ?
N1 C1 C2 O1 -1.3(5) . . . . ?
C4 C1 C2 O1 -179.5(3) . . . . ?
N1 C1 C2 C3 177.7(3) . . . . ?
C4 C1 C2 C3 -0.52(19) . . . . ?
O1 C2 C3 O2 1.3(5) . . . . ?
C1 C2 C3 O2 -177.7(3) . . . . ?
O1 C2 C3 C4 179.5(3) . . . . ?
C1 C2 C3 C4 0.50(19) . . . . ?
C5 N2 C4 C1 -174.8(2) . . . . ?
C5 N2 C4 C3 5.3(4) . . . . ?
N1 C1 C4 N2 2.4(5) . . . . ?
C2 C1 C4 N2 -179.4(3) . . . . ?
N1 C1 C4 C3 -177.7(3) . . . . ?
C2 C1 C4 C3 0.5(2) . . . . ?
O2 C3 C4 N2 -2.4(5) . . . . ?
C2 C3 C4 N2 179.4(3) . . . . ?
O2 C3 C4 C1 177.7(3) . . . . ?
C2 C3 C4 C1 -0.52(19) . . . . ?
C4 N2 C5 C6 -62.4(3) . . . . ?
N2 C5 C6 C11 -45.4(3) . . . . ?
N2 C5 C6 C7 133.9(2) . . . . ?
C11 C6 C7 C8 0.5(4) . . . . ?
C5 C6 C7 C8 -178.8(2) . . . . ?
C6 C7 C8 C9 1.3(4) . . . . ?
C6 C7 C8 C13 179.4(2) . . . . ?
C7 C8 C9 C10 -1.5(4) . . . . ?
C13 C8 C9 C10 -179.5(2) . . . . ?
C8 C9 C10 C11 -0.1(4) . . . . ?
C8 C9 C10 C12 176.4(2) . . . . ?
C7 C6 C11 C10 -2.1(4) . . . . ?
C5 C6 C11 C10 177.2(2) . . . . ?
C9 C10 C11 C6 2.0(4) . . . . ?
C12 C10 C11 C6 -174.6(2) . . . . ?
C9 C10 C12 N1 -108.2(3) . . . 2_765 ?
C11 C10 C12 N1 68.3(3) . . . 2_765 ?
C14 O4 C13 O3 -4.2(4) . . . . ?
C14 O4 C13 C8 175.8(2) . . . . ?
C7 C8 C13 O3 -9.0(4) . . . . ?
C9 C8 C13 O3 169.0(3) . . . . ?
C7 C8 C13 O4 171.0(2) . . . . ?
C9 C8 C13 O4 -11.0(3) . . . . ?
C13 O4 C14 C15 -174.6(2) . . . . ?
C16B O5 C15 C14 -172.3(7) . . . . ?
C16A O5 C15 C14 -174.8(3) . . . . ?
O4 C14 C15 O5 -74.8(3) . . . . ?
C15 O5 C16A C17A -176.7(3) . . . . ?
C18A O6A C17A C16A 175.6(3) . . . . ?
O5 C16A C17A O6A -170.4(3) . . . . ?
C17A O6A C18A C19A 179.4(3) . . . . ?
C20A O7A C19A C18A 86.0(4) . . . . ?
O6A C18A C19A O7A -73.4(4) . . . . ?
C15 O5 C16B C17B 174.8(7) . . . . ?
C18B O6B C17B C16B -84.6(11) . . . . ?
O5 C16B C17B O6B -168.2(9) . . . . ?
C17B O6B C18B C19B 135.9(10) . . . . ?
C20B O7B C19B C18B -174.8(11) . . . . ?
O6B C18B C19B O7B -73.8(12) . . . . ?

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 H1N O1 1.02(3) 1.87(3) 2.786(3) 147(2) 1_655
N2 H2N O2 0.87(3) 1.94(3) 2.762(3) 157(3) 1_655
C5 H5A O3 0.99 2.54 3.354(3) 139.8 1_655
C12 H12B O1 0.99 2.54 3.274(3) 130.4 2_765
C20A H20A O6A 0.98 2.51 3.092(5) 118.1 .
C17B H17C O5 0.99 2.55 3.181(12) 121.8 2_666

_refine_diff_density_max         0.356
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.051



