# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2018

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1835198'
_audit_update_record             
;
2018-10-26 deposited with the CCDC.
2018-11-19 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            'C30 H40 N6 O12'
_chemical_formula_weight         676.68

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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+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                   27.337(3)
_cell_length_b                   6.1593(4)
_cell_length_c                   20.343(2)
_cell_angle_alpha                90
_cell_angle_beta                 106.22(1)
_cell_angle_gamma                90
_cell_volume                     3289.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    6943
_cell_measurement_theta_min      4.5240
_cell_measurement_theta_max      72.2830

_exptl_crystal_description       prismatic
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_F_000             1432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.901
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.68664
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 8.1241
_diffrn_reflns_number            13394
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.527
_diffrn_reflns_theta_max         66.569
_diffrn_reflns_theta_full        66.569
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2918
_reflns_number_gt                2426
_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 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_structure_solution    'SIR92 (Altomare 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury CSD 3.8'
_computing_publication_material  'PARST93 (Nardelli, 1993)'
_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)+(0.1283P)²+6.6781P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2918
_refine_ls_number_parameters     246
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1599
_refine_ls_wR_factor_gt          0.1386
_refine_ls_goodness_of_fit_ref   0.807
_refine_ls_restrained_S_all      0.807
_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
O3 O 0.14668(5) 0.3885(2) 0.41317(7) 0.0294(4) Uani 1 1 d . . . . .
O1 O 0.01030(6) 0.2641(3) 0.47863(10) 0.0423(4) Uani 1 1 d . . . . .
O5 O 0.10320(7) 0.1135(3) 0.20998(9) 0.0458(5) Uani 1 1 d . . . . .
O4 O 0.11994(7) 0.2901(3) 0.12509(8) 0.0488(5) Uani 1 1 d . . . . .
N3 N 0.24257(6) 0.0572(3) 0.46635(8) 0.0260(4) Uani 1 1 d . . . . .
N1 N 0.10504(6) 0.0724(3) 0.47565(8) 0.0245(4) Uani 1 1 d . . . . .
O2 O 0.11839(7) 0.1499(3) 0.33162(9) 0.0451(5) Uani 1 1 d . . . . .
N6 N 0.22994(6) 0.2912(3) 0.55302(9) 0.0264(4) Uani 1 1 d . . . . .
C13 C 0.18003(8) 0.5896(4) 0.20262(10) 0.0289(5) Uani 1 1 d . . . . .
H13 H 0.1768 0.5713 0.1562 0.035 Uiso 1 1 calc R U . . .
C10 C 0.19031(7) 0.6454(3) 0.33884(10) 0.0245(4) Uani 1 1 d . . . . .
H10 H 0.1941 0.6658 0.3853 0.029 Uiso 1 1 calc R U . . .
C1 C 0.22333(7) 0.1029(3) 0.51844(10) 0.0240(4) Uani 1 1 d . . . . .
C2 C 0.19244(7) -0.0705(3) 0.53970(10) 0.0272(5) Uani 1 1 d . . . . .
H2A H 0.1867 -0.0286 0.5829 0.033 Uiso 1 1 calc R U . . .
H2B H 0.2121 -0.2039 0.5474 0.033 Uiso 1 1 calc R U . . .
C7 C 0.09724(8) 0.1681(3) 0.53968(11) 0.0302(5) Uani 1 1 d . . . . .
H7A H 0.1291 0.2286 0.5675 0.036 Uiso 1 1 calc R U . . .
H7B H 0.0865 0.0556 0.5660 0.036 Uiso 1 1 calc R U . . .
C9 C 0.16147(7) 0.4694(3) 0.30603(10) 0.0235(4) Uani 1 1 d . . . . .
C11 C 0.21358(8) 0.7911(3) 0.30531(11) 0.0289(5) Uani 1 1 d . . . . .
H11 H 0.2321 0.9075 0.3288 0.035 Uiso 1 1 calc R U . . .
C12 C 0.20889(8) 0.7612(4) 0.23651(11) 0.0304(5) Uani 1 1 d . . . . .
H12 H 0.2249 0.8552 0.2133 0.036 Uiso 1 1 calc R U . . .
C5 C 0.01729(9) 0.1865(4) 0.41634(13) 0.0399(6) Uani 1 1 d . . . . .
H5A H 0.0298 0.3032 0.3934 0.048 Uiso 1 1 calc R U . . .
H5B H -0.0152 0.1384 0.3865 0.048 Uiso 1 1 calc R U . . .
C14 C 0.15548(7) 0.4426(3) 0.23497(10) 0.0261(4) Uani 1 1 d . . . . .
C3 C 0.14125(7) -0.1157(3) 0.48858(11) 0.0264(4) Uani 1 1 d . . . . .
H3A H 0.1470 -0.1590 0.4455 0.032 Uiso 1 1 calc R U . . .
H3B H 0.1254 -0.2370 0.5051 0.032 Uiso 1 1 calc R U . . .
C8 C 0.14047(8) 0.3269(3) 0.35287(10) 0.0271(5) Uani 1 1 d . . . . .
C15 C 0.12447(8) 0.2732(4) 0.18613(11) 0.0347(5) Uani 1 1 d . . . . .
C6 C 0.05722(9) 0.3441(4) 0.52159(14) 0.0401(6) Uani 1 1 d . . . . .
H6A H 0.0517 0.4022 0.5633 0.048 Uiso 1 1 calc R U . . .
H6B H 0.0693 0.4614 0.4984 0.048 Uiso 1 1 calc R U . . .
C4 C 0.05464(7) 0.0005(4) 0.42927(11) 0.0304(5) Uani 1 1 d . . . . .
H4A H 0.0414 -0.1190 0.4502 0.036 Uiso 1 1 calc R U . . .
H4B H 0.0592 -0.0499 0.3862 0.036 Uiso 1 1 calc R U . . .
OW1 O 0.03928(13) 0.2779(6) 0.68324(17) 0.0307(11) Uani 0.416(5) 1 d . . P . .
OW2 O 0.0184(3) -0.416(3) 0.2576(5) 0.082(5) Uani 0.318(11) 1 d . . P . .
OW3 O 0.0237(3) -0.2645(18) 0.2438(3) 0.036(3) Uani 0.268(11) 1 d . . P . .
H1 H 0.1204(11) 0.181(5) 0.4482(15) 0.052(8) Uiso 1 1 d . . . . .
H2 H 0.1112(14) 0.134(6) 0.2717(19) 0.074(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
O3 C8 1.249(2) . ?
O1 C5 1.416(3) . ?
O1 C6 1.423(3) . ?
O5 C15 1.303(3) . ?
O4 C15 1.217(3) . ?
N3 N6 1.325(2) 7_556 ?
N3 C1 1.338(3) . ?
N1 C7 1.498(3) . ?
N1 C4 1.503(2) . ?
N1 C3 1.498(2) . ?
O2 C8 1.263(3) . ?
N6 N3 1.325(2) 7_556 ?
N6 C1 1.343(3) . ?
C13 C12 1.382(3) . ?
C13 C14 1.396(3) . ?
C10 C11 1.385(3) . ?
C10 C9 1.396(3) . ?
C1 C2 1.498(3) . ?
C2 C3 1.518(3) . ?
C7 C6 1.511(3) . ?
C9 C14 1.418(3) . ?
C9 C8 1.521(3) . ?
C11 C12 1.382(3) . ?
C5 C4 1.508(3) . ?
C14 C15 1.525(3) . ?
OW1 OW3 1.415(7) 6_556 ?
OW2 OW2 0.964(18) 2 ?
OW2 OW3 0.994(12) . ?
OW2 OW3 1.472(8) 2 ?
OW3 OW3 1.384(13) 2 ?
OW3 OW1 1.415(7) 6 ?
OW3 OW2 1.472(8) 2 ?

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
C5 O1 C6 110.04(17) . . ?
N6 N3 C1 117.92(17) 7_556 . ?
C7 N1 C4 109.48(15) . . ?
C7 N1 C3 113.52(16) . . ?
C4 N1 C3 109.12(15) . . ?
N3 N6 C1 117.23(17) 7_556 . ?
C12 C13 C14 122.90(18) . . ?
C11 C10 C9 122.92(18) . . ?
N3 C1 N6 124.85(18) . . ?
N3 C1 C2 117.17(17) . . ?
N6 C1 C2 117.97(17) . . ?
C1 C2 C3 114.77(16) . . ?
N1 C7 C6 109.87(18) . . ?
C10 C9 C14 117.82(18) . . ?
C10 C9 C8 114.21(17) . . ?
C14 C9 C8 127.97(18) . . ?
C10 C11 C12 119.16(19) . . ?
C13 C12 C11 119.05(19) . . ?
O1 C5 C4 110.75(19) . . ?
C13 C14 C9 118.10(18) . . ?
C13 C14 C15 112.93(18) . . ?
C9 C14 C15 128.97(19) . . ?
N1 C3 C2 114.58(16) . . ?
O3 C8 O2 121.25(19) . . ?
O3 C8 C9 117.96(18) . . ?
O2 C8 C9 120.78(18) . . ?
O4 C15 O5 121.0(2) . . ?
O4 C15 C14 119.1(2) . . ?
O5 C15 C14 119.90(19) . . ?
O1 C6 C7 111.60(18) . . ?
N1 C4 C5 110.09(17) . . ?
OW2 OW2 OW3 97.5(7) 2 . ?
OW2 OW2 OW3 42.0(6) 2 2 ?
OW3 OW2 OW3 64.9(8) . 2 ?
OW2 OW3 OW3 74.5(7) . 2 ?
OW2 OW3 OW1 107.1(10) . 6 ?
OW3 OW3 OW1 133.0(7) 2 6 ?
OW2 OW3 OW2 40.5(9) . 2 ?
OW3 OW3 OW2 40.6(5) 2 2 ?
OW1 OW3 OW2 111.7(5) 6 2 ?

_refine_diff_density_max         0.497
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.068



#===END
####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1835199'
_audit_update_record             
;
2018-10-26 deposited with the CCDC.
2018-11-19 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            'C30 H36 N6 O10'
_chemical_formula_weight         640.65

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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   6.8698(1)
_cell_length_b                   14.4541(3)
_cell_length_c                   14.7842(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.204(2)
_cell_angle_gamma                90
_cell_volume                     1461.97(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    3512
_cell_measurement_theta_min      6.0050
_cell_measurement_theta_max      71.7010

_exptl_crystal_description       prismatic
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_F_000             676
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.930
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.68664
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 8.1241
_diffrn_reflns_number            7812
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.286
_diffrn_reflns_theta_max         72.351
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             2719
_reflns_number_gt                2148
_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 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_structure_solution    'SIR92 (Altomare 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury CSD 3.8'
_computing_publication_material  'PARST93 (Nardelli, 1993)'
_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)+(0.0888P)²+0.2900P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2719
_refine_ls_number_parameters     212
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1714
_refine_ls_wR_factor_gt          0.1411
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_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
O4 O 0.2141(2) 0.89413(11) 0.67705(11) 0.0264(4) Uani 1 1 d . . . . .
O1 O 0.1535(3) 0.61769(12) 0.62422(11) 0.0308(4) Uani 1 1 d . . . . .
O3 O 0.1764(3) 0.72630(13) 0.39089(12) 0.0324(4) Uani 1 1 d . . . . .
O5 O 0.4696(3) 0.87366(12) 0.77937(11) 0.0317(4) Uani 1 1 d . . . . .
O2 O 0.4430(3) 0.66451(13) 0.33928(11) 0.0351(5) Uani 1 1 d . . . . .
N3 N 0.4531(3) 0.53869(13) 0.74900(12) 0.0232(4) Uani 1 1 d . . . . .
H1 H 0.3892 0.4800 0.7614 0.028 Uiso 1 1 calc R U . . .
N1 N 0.9926(3) 0.54532(13) 0.91896(13) 0.0238(4) Uani 1 1 d . . . . .
N2 N 0.8375(3) 0.46399(12) 1.03225(13) 0.0226(4) Uani 1 1 d . . . . .
C9 C 0.4771(3) 0.74138(15) 0.48160(15) 0.0229(5) Uani 1 1 d . . . . .
C14 C 0.3820(3) 0.78567(14) 0.54920(15) 0.0222(5) Uani 1 1 d . . . . .
H14 H 0.2480 0.7961 0.5407 0.027 Uiso 1 1 calc R U . . .
C1 C 0.8338(3) 0.50935(15) 0.95325(15) 0.0219(5) Uani 1 1 d . . . . .
C7 C 0.3250(3) 0.61621(16) 0.77585(16) 0.0246(5) Uani 1 1 d . . . . .
H8B H 0.3884 0.6750 0.7670 0.030 Uiso 1 1 calc R U . . .
H8A H 0.3041 0.6106 0.8396 0.030 Uiso 1 1 calc R U . . .
C13 C 0.4875(3) 0.81418(15) 0.62921(15) 0.0225(5) Uani 1 1 d . . . . .
C8 C 0.3654(4) 0.70742(15) 0.39699(15) 0.0242(5) Uani 1 1 d . . . . .
C2 C 0.6388(3) 0.52182(17) 0.90167(16) 0.0257(5) Uani 1 1 d . . . . .
H2B H 0.5726 0.5735 0.9273 0.031 Uiso 1 1 calc R U . . .
H2A H 0.5607 0.4668 0.9089 0.031 Uiso 1 1 calc R U . . .
C12 C 0.6885(3) 0.79794(15) 0.64103(15) 0.0230(5) Uani 1 1 d . . . . .
H12 H 0.7593 0.8156 0.6949 0.028 Uiso 1 1 calc R U . . .
C10 C 0.6776(3) 0.72758(15) 0.49335(15) 0.0248(5) Uani 1 1 d . . . . .
H10 H 0.7412 0.6995 0.4477 0.030 Uiso 1 1 calc R U . . .
C11 C 0.7836(4) 0.75560(16) 0.57312(16) 0.0271(5) Uani 1 1 d . . . . .
H11 H 0.9180 0.7460 0.5810 0.032 Uiso 1 1 calc R U . . .
C5 C 0.2695(4) 0.54218(17) 0.59857(17) 0.0310(6) Uani 1 1 d . . . . .
H5B H 0.2811 0.5448 0.5337 0.037 Uiso 1 1 calc R U . . .
H5A H 0.2057 0.4845 0.6116 0.037 Uiso 1 1 calc R U . . .
C4 C 0.4707(4) 0.54461(17) 0.64885(15) 0.0275(5) Uani 1 1 d . . . . .
H4A H 0.5478 0.4931 0.6298 0.033 Uiso 1 1 calc R U . . .
H4B H 0.5365 0.6016 0.6350 0.033 Uiso 1 1 calc R U . . .
C6 C 0.1305(4) 0.61290(18) 0.71894(17) 0.0297(5) Uani 1 1 d . . . . .
H6A H 0.0635 0.5560 0.7317 0.036 Uiso 1 1 calc R U . . .
H7B H 0.0500 0.6642 0.7356 0.036 Uiso 1 1 calc R U . . .
C15 C 0.3817(3) 0.86363(15) 0.70083(15) 0.0233(5) Uani 1 1 d . . . . .
C3 C 0.6509(3) 0.53939(16) 0.80046(16) 0.0249(5) Uani 1 1 d . . . . .
H3B H 0.7125 0.5988 0.7924 0.030 Uiso 1 1 calc R U . . .
H3A H 0.7317 0.4921 0.7761 0.030 Uiso 1 1 calc R U . . .
H2 H 0.106(7) 0.689(3) 0.342(3) 0.083(14) 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
O4 C15 1.253(3) . ?
O1 C5 1.423(3) . ?
O1 C6 1.425(3) . ?
O3 C8 1.322(3) . ?
O5 C15 1.268(3) . ?
O2 C8 1.216(3) . ?
N3 C3 1.495(3) . ?
N3 C4 1.499(3) . ?
N3 C7 1.501(3) . ?
N1 N2 1.322(3) 3_767 ?
N1 C1 1.349(3) . ?
N2 N1 1.322(3) 3_767 ?
N2 C1 1.338(3) . ?
C9 C10 1.387(3) . ?
C9 C14 1.398(3) . ?
C9 C8 1.490(3) . ?
C14 C13 1.392(3) . ?
C1 C2 1.491(3) . ?
C7 C6 1.514(3) . ?
C13 C12 1.396(3) . ?
C13 C15 1.516(3) . ?
C2 C3 1.527(3) . ?
C12 C11 1.389(3) . ?
C10 C11 1.389(3) . ?
C5 C4 1.509(4) . ?

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
C5 O1 C6 109.83(18) . . ?
C3 N3 C4 110.56(17) . . ?
C3 N3 C7 112.83(17) . . ?
C4 N3 C7 108.69(17) . . ?
N2 N1 C1 117.40(19) 3_767 . ?
N1 N2 C1 118.17(19) 3_767 . ?
C10 C9 C14 120.0(2) . . ?
C10 C9 C8 119.2(2) . . ?
C14 C9 C8 120.9(2) . . ?
C13 C14 C9 120.1(2) . . ?
N2 C1 N1 124.4(2) . . ?
N2 C1 C2 116.80(19) . . ?
N1 C1 C2 118.8(2) . . ?
N3 C7 C6 109.81(19) . . ?
C14 C13 C12 119.3(2) . . ?
C14 C13 C15 119.2(2) . . ?
C12 C13 C15 121.5(2) . . ?
O2 C8 O3 123.2(2) . . ?
O2 C8 C9 122.1(2) . . ?
O3 C8 C9 114.65(19) . . ?
C1 C2 C3 113.26(19) . . ?
C11 C12 C13 120.6(2) . . ?
C9 C10 C11 120.2(2) . . ?
C12 C11 C10 119.8(2) . . ?
O1 C5 C4 111.2(2) . . ?
N3 C4 C5 109.44(19) . . ?
O1 C6 C7 111.96(19) . . ?
O4 C15 O5 124.5(2) . . ?
O4 C15 C13 117.1(2) . . ?
O5 C15 C13 118.4(2) . . ?
N3 C3 C2 111.69(18) . . ?

_refine_diff_density_max         0.311
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.096



#===END
####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1835200'
_audit_update_record             
;
2018-10-26 deposited with the CCDC.
2018-11-19 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            'C26 H38 N6 O9 S2'
_chemical_formula_weight         642.74

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      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   15.1627(5)
_cell_length_b                   6.4915(4)
_cell_length_c                   29.4057(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2894.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    12482
_cell_measurement_theta_min      5.8210
_cell_measurement_theta_max      72.3880

_exptl_crystal_description       prismatic
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_F_000             1360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    2.222
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.41285
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 8.1241
_diffrn_reflns_number            14957
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         5.836
_diffrn_reflns_theta_max         72.425
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.820
_diffrn_reflns_point_group_measured_fraction_full 0.841
_reflns_number_total             4695
_reflns_number_gt                4555
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.630
_reflns_Friedel_fraction_max     0.647
_reflns_Friedel_fraction_full    0.676

_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 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_structure_solution    'SIR92 (Altomare 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury CSD 3.8'
_computing_publication_material  'PARST93 (Nardelli, 1993)'
_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)+(0.0529P)²+0.5624P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1680 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4695
_refine_ls_number_parameters     396
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0755
_refine_ls_wR_factor_gt          0.0741
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_restrained_S_all      0.973
_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
N1 N 0.99304(15) 0.0685(3) 0.52512(8) 0.0194(4) Uani 1 1 d . . . . .
N2 N 1.00942(14) 0.2260(3) 0.55227(7) 0.0186(4) Uani 1 1 d . . . . .
N3 N 0.92677(16) 0.4444(3) 0.50354(8) 0.0214(5) Uani 1 1 d . . . . .
N4 N 0.91135(15) 0.2860(3) 0.47593(8) 0.0209(5) Uani 1 1 d . . . . .
C1 C 0.97450(16) 0.4085(4) 0.54079(9) 0.0173(5) Uani 1 1 d . . . . .
C2 C 0.99126(18) 0.5906(4) 0.57111(9) 0.0191(5) Uani 1 1 d . . . . .
H2A H 0.9391 0.6772 0.5717 0.023 Uiso 1 1 calc R U . . .
H2B H 1.0394 0.6713 0.5587 0.023 Uiso 1 1 calc R U . . .
C3 C 1.01407(16) 0.5267(4) 0.61923(9) 0.0173(5) Uani 1 1 d . . . . .
H3A H 0.9725 0.4229 0.6294 0.021 Uiso 1 1 calc R U . . .
H3B H 1.0726 0.4662 0.6196 0.021 Uiso 1 1 calc R U . . .
N5 N 1.01154(14) 0.7071(3) 0.65115(7) 0.0161(4) Uani 1 1 d . . . . .
H5 H 0.9522 0.7668 0.6498 0.019 Uiso 1 1 calc R U . . .
C4 C 1.02731(18) 0.6368(4) 0.69901(8) 0.0186(5) Uani 1 1 d . . . . .
H4B H 1.0852 0.5739 0.7013 0.022 Uiso 1 1 calc R U . . .
H4A H 0.9836 0.5347 0.7074 0.022 Uiso 1 1 calc R U . . .
C5 C 1.02157(18) 0.8200(4) 0.73097(9) 0.0220(5) Uani 1 1 d . . . . .
H5A H 0.9626 0.8775 0.7297 0.026 Uiso 1 1 calc R U . . .
H5B H 1.0321 0.7740 0.7619 0.026 Uiso 1 1 calc R U . . .
O1 O 1.08364(13) 0.9749(3) 0.71959(7) 0.0223(4) Uani 1 1 d . . . . .
C6 C 1.06815(18) 1.0466(4) 0.67462(10) 0.0213(5) Uani 1 1 d . . . . .
H6B H 1.1102 1.1544 0.6674 0.026 Uiso 1 1 calc R U . . .
H6A H 1.0094 1.1054 0.6729 0.026 Uiso 1 1 calc R U . . .
C7 C 1.07645(17) 0.8743(4) 0.63984(9) 0.0188(5) Uani 1 1 d . . . . .
H7A H 1.0647 0.9275 0.6096 0.023 Uiso 1 1 calc R U . . .
H7B H 1.1359 0.8192 0.6403 0.023 Uiso 1 1 calc R U . . .
C8 C 0.94341(16) 0.1028(4) 0.48797(8) 0.0170(5) Uani 1 1 d . . . . .
C9 C 0.92289(18) -0.0795(4) 0.45862(9) 0.0200(5) Uani 1 1 d . . . . .
H9A H 0.8783 -0.1634 0.4733 0.024 Uiso 1 1 calc R U . . .
H9B H 0.9756 -0.1628 0.4551 0.024 Uiso 1 1 calc R U . . .
C10 C 0.88997(18) -0.0132(3) 0.41206(9) 0.0179(5) Uani 1 1 d . . . . .
H10A H 0.8322 0.0495 0.4152 0.021 Uiso 1 1 calc R U . . .
H10B H 0.9297 0.0894 0.3996 0.021 Uiso 1 1 calc R U . . .
N6 N 0.88412(13) -0.1919(3) 0.37995(7) 0.0158(4) Uani 1 1 d . . . . .
H6 H 0.9422 -0.2578 0.3786 0.019 Uiso 1 1 calc R U . . .
C11 C 0.81801(17) -0.3515(4) 0.39453(9) 0.0194(5) Uani 1 1 d . . . . .
H11A H 0.7604 -0.2883 0.3980 0.023 Uiso 1 1 calc R U . . .
H11B H 0.8352 -0.4091 0.4236 0.023 Uiso 1 1 calc R U . . .
C12 C 0.81359(18) -0.5211(4) 0.35905(10) 0.0209(5) Uani 1 1 d . . . . .
H12A H 0.8707 -0.5875 0.3567 0.025 Uiso 1 1 calc R U . . .
H12B H 0.7710 -0.6241 0.3685 0.025 Uiso 1 1 calc R U . . .
O2 O 0.78893(13) -0.4410(3) 0.31583(7) 0.0236(4) Uani 1 1 d . . . . .
C14 C 0.86174(17) -0.1169(4) 0.33316(9) 0.0201(5) Uani 1 1 d . . . . .
H14B H 0.9074 -0.0240 0.3226 0.024 Uiso 1 1 calc R U . . .
H14A H 0.8065 -0.0414 0.3340 0.024 Uiso 1 1 calc R U . . .
C13 C 0.85352(19) -0.2969(4) 0.30061(9) 0.0232(5) Uani 1 1 d . . . . .
H13B H 0.8372 -0.2463 0.2707 0.028 Uiso 1 1 calc R U . . .
H13A H 0.9101 -0.3655 0.2980 0.028 Uiso 1 1 calc R U . . .
S1 S 1.08951(4) -0.52396(8) 0.35324(2) 0.01668(14) Uani 1 1 d . . . . .
O12 O 1.16386(12) -0.5861(3) 0.38121(6) 0.0220(4) Uani 1 1 d . . . . .
O13 O 1.05360(12) -0.3232(3) 0.36728(6) 0.0216(4) Uani 1 1 d . . . . .
O11 O 1.02224(12) -0.6822(3) 0.34975(7) 0.0241(4) Uani 1 1 d . . . . .
C15 C 1.13146(17) -0.4891(4) 0.29764(9) 0.0166(5) Uani 1 1 d . . . . .
C16 C 1.12331(16) -0.3015(4) 0.27530(9) 0.0195(5) Uani 1 1 d . . . . .
H16 H 1.0956 -0.1904 0.2893 0.023 Uiso 1 1 calc R U . . .
C17 C 1.15748(17) -0.2836(4) 0.23158(9) 0.0215(5) Uani 1 1 d . . . . .
H17 H 1.1530 -0.1586 0.2163 0.026 Uiso 1 1 calc R U . . .
C18 C 1.19805(18) -0.4489(4) 0.21053(9) 0.0231(6) Uani 1 1 d . . . . .
H18 H 1.2195 -0.4355 0.1811 0.028 Uiso 1 1 calc R U . . .
C19 C 1.20669(17) -0.6357(4) 0.23353(9) 0.0207(5) Uani 1 1 d . . . . .
H19 H 1.2346 -0.7467 0.2196 0.025 Uiso 1 1 calc R U . . .
C20 C 1.17358(16) -0.6550(4) 0.27715(9) 0.0181(5) Uani 1 1 d . . . . .
H20 H 1.1795 -0.7789 0.2928 0.022 Uiso 1 1 calc R U . . .
S2 S 0.79528(4) 0.01949(9) 0.62127(2) 0.01750(14) Uani 1 1 d . . . . .
O21 O 0.84523(14) -0.1633(3) 0.63510(7) 0.0330(5) Uani 1 1 d . . . . .
O22 O 0.71932(12) 0.0501(3) 0.65030(6) 0.0211(4) Uani 1 1 d . . . . .
O23 O 0.84933(15) 0.2001(4) 0.61572(8) 0.0376(5) Uani 1 1 d . . . . .
C21 C 0.75213(17) -0.0400(4) 0.56659(9) 0.0173(5) Uani 1 1 d . . . . .
C22 C 0.72618(18) 0.1209(4) 0.53860(9) 0.0220(5) Uani 1 1 d . . . . .
H22 H 0.7344 0.2566 0.5478 0.026 Uiso 1 1 calc R U . . .
C23 C 0.68799(19) 0.0787(4) 0.49695(9) 0.0240(5) Uani 1 1 d . . . . .
H23 H 0.6705 0.1864 0.4781 0.029 Uiso 1 1 calc R U . . .
C24 C 0.67561(17) -0.1231(4) 0.48315(9) 0.0225(5) Uani 1 1 d . . . . .
H24 H 0.6494 -0.1510 0.4552 0.027 Uiso 1 1 calc R U . . .
C25 C 0.70246(19) -0.2841(4) 0.51107(9) 0.0223(5) Uani 1 1 d . . . . .
H25 H 0.6943 -0.4196 0.5017 0.027 Uiso 1 1 calc R U . . .
C26 C 0.74139(17) -0.2432(4) 0.55286(9) 0.0187(5) Uani 1 1 d . . . . .
H26 H 0.7600 -0.3506 0.5714 0.022 Uiso 1 1 calc R U . . .
OW1 O 1.11831(16) 0.0179(3) 0.42100(8) 0.0303(5) Uani 1 1 d . . . . .
H1 H 1.098(3) -0.083(7) 0.3990(18) 0.053(12) Uiso 1 1 d . . . . .
H2 H 1.125(4) 0.143(8) 0.403(2) 0.070(15) 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
N1 N2 1.321(3) . ?
N1 C8 1.345(3) . ?
N2 C1 1.341(3) . ?
N3 N4 1.330(3) . ?
N3 C1 1.334(3) . ?
N4 C8 1.333(3) . ?
C1 C2 1.502(3) . ?
C2 C3 1.515(4) . ?
C3 N5 1.501(3) . ?
N5 C4 1.499(3) . ?
N5 C7 1.503(3) . ?
C4 C5 1.518(4) . ?
C5 O1 1.418(3) . ?
O1 C6 1.421(3) . ?
C6 C7 1.521(4) . ?
C8 C9 1.498(3) . ?
C9 C10 1.520(4) . ?
C10 N6 1.498(3) . ?
N6 C14 1.499(3) . ?
N6 C11 1.504(3) . ?
C11 C12 1.518(4) . ?
C12 O2 1.423(3) . ?
O2 C13 1.426(3) . ?
C14 C13 1.516(4) . ?
S1 O12 1.4528(19) . ?
S1 O11 1.4510(19) . ?
S1 O13 1.4716(18) . ?
S1 C15 1.769(3) . ?
C15 C16 1.389(4) . ?
C15 C20 1.390(3) . ?
C16 C17 1.391(4) . ?
C17 C18 1.383(4) . ?
C18 C19 1.395(4) . ?
C19 C20 1.383(4) . ?
S2 O23 1.440(2) . ?
S2 O22 1.4474(19) . ?
S2 O21 1.465(2) . ?
S2 C21 1.778(3) . ?
C21 C22 1.387(4) . ?
C21 C26 1.389(4) . ?
C22 C23 1.382(4) . ?
C23 C24 1.385(4) . ?
C24 C25 1.389(4) . ?
C25 C26 1.389(4) . ?

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
N2 N1 C8 117.9(2) . . ?
N1 N2 C1 117.2(2) . . ?
N4 N3 C1 117.5(2) . . ?
N3 N4 C8 117.6(2) . . ?
N3 C1 N2 125.2(2) . . ?
N3 C1 C2 116.2(2) . . ?
N2 C1 C2 118.6(2) . . ?
C1 C2 C3 112.2(2) . . ?
N5 C3 C2 111.39(19) . . ?
C4 N5 C7 108.85(19) . . ?
C4 N5 C3 110.23(19) . . ?
C7 N5 C3 114.11(19) . . ?
N5 C4 C5 109.5(2) . . ?
O1 C5 C4 111.8(2) . . ?
C5 O1 C6 110.0(2) . . ?
O1 C6 C7 111.8(2) . . ?
N5 C7 C6 109.2(2) . . ?
N4 C8 N1 124.6(2) . . ?
N4 C8 C9 118.5(2) . . ?
N1 C8 C9 117.0(2) . . ?
C8 C9 C10 111.3(2) . . ?
N6 C10 C9 111.58(19) . . ?
C14 N6 C10 109.89(18) . . ?
C14 N6 C11 109.55(19) . . ?
C10 N6 C11 113.16(19) . . ?
N6 C11 C12 109.5(2) . . ?
O2 C12 C11 111.1(2) . . ?
C13 O2 C12 109.8(2) . . ?
N6 C14 C13 110.3(2) . . ?
O2 C13 C14 111.3(2) . . ?
O12 S1 O11 112.88(11) . . ?
O12 S1 O13 111.98(11) . . ?
O11 S1 O13 112.75(11) . . ?
O12 S1 C15 106.24(11) . . ?
O11 S1 C15 106.14(12) . . ?
O13 S1 C15 106.22(11) . . ?
C16 C15 C20 121.0(2) . . ?
C16 C15 S1 121.1(2) . . ?
C20 C15 S1 117.84(19) . . ?
C15 C16 C17 118.5(2) . . ?
C18 C17 C16 120.9(2) . . ?
C17 C18 C19 120.0(2) . . ?
C20 C19 C18 119.6(2) . . ?
C19 C20 C15 119.9(2) . . ?
O23 S2 O22 114.10(13) . . ?
O23 S2 O21 113.37(14) . . ?
O22 S2 O21 111.02(12) . . ?
O23 S2 C21 106.48(13) . . ?
O22 S2 C21 105.68(11) . . ?
O21 S2 C21 105.39(12) . . ?
C22 C21 C26 120.6(2) . . ?
C22 C21 S2 118.5(2) . . ?
C26 C21 S2 120.8(2) . . ?
C23 C22 C21 119.7(2) . . ?
C22 C23 C24 120.3(2) . . ?
C23 C24 C25 119.9(2) . . ?
C24 C25 C26 120.2(2) . . ?
C25 C26 C21 119.2(2) . . ?

_refine_diff_density_max         0.249
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.050



#===END
