# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1030511'
_audit_update_record             
;
2014-10-22 deposited with the CCDC.
2014-12-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H18 N O5, C16 H36 N'
_chemical_formula_sum            'C38 H54 N2 O5'
_chemical_formula_weight         618.83

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'

_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                   13.654(3)
_cell_length_b                   17.014(3)
_cell_length_c                   16.235(3)
_cell_angle_alpha                90
_cell_angle_beta                 109.290(2)
_cell_angle_gamma                90
_cell_volume                     3559.8(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9498
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      27.5

_exptl_crystal_description       fragment
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_F_000             1344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.076
_shelx_estimated_absorpt_T_min   0.996
_shelx_estimated_absorpt_T_max   0.998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           'Mo K\a'
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Mitegen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_reflns_number            24283
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.658
_diffrn_reflns_theta_max         27.506
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8162
_reflns_number_gt                4856
_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       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_structure_solution    
'SUPERFLIP (Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  
'WinGX, ver.2013.3 (L.J. Farrugia, J.App.Cryst.(2012),45,849-854)'

_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)+(0.0444P)²+1.4684P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8162
_refine_ls_number_parameters     413
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.0592
_refine_ls_wR_factor_ref         0.1351
_refine_ls_wR_factor_gt          0.1122
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_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
C1 C 0.60060(14) 0.44291(12) 0.82114(14) 0.0224(5) Uani 1 1 d . . . . .
C1A C 0.78245(15) 0.42219(13) 0.92212(14) 0.0266(5) Uani 1 1 d . . . . .
H1AA H 0.8354 0.3829 0.9208 0.032 Uiso 1 1 calc R U . . .
H1AB H 0.7479 0.4028 0.9630 0.032 Uiso 1 1 calc R U . . .
C1S C 0.86418(14) 0.40676(11) 0.68511(14) 0.0220(5) Uani 1 1 d . . . . .
C2 C 0.55361(16) 0.45647(12) 0.88501(15) 0.0255(5) Uani 1 1 d . . . . .
H2 H 0.5929 0.4567 0.9454 0.031 Uiso 1 1 calc R U . . .
C2A C 0.83706(16) 0.49997(13) 0.95700(14) 0.0295(5) Uani 1 1 d . . . . .
H2AA H 0.9033 0.5025 0.9447 0.035 Uiso 1 1 calc R U . . .
H2AB H 0.7930 0.5442 0.9261 0.035 Uiso 1 1 calc R U . . .
C2S C 0.83125(15) 0.39323(12) 0.59096(14) 0.0243(5) Uani 1 1 d . . . . .
C3 C 0.44817(15) 0.46932(12) 0.85616(15) 0.0258(5) Uani 1 1 d . . . . .
H3 H 0.4147 0.4796 0.8978 0.031 Uiso 1 1 calc R U . . .
C3A C 0.85860(15) 0.50873(13) 1.05388(15) 0.0270(5) Uani 1 1 d . . . . .
C3S C 0.94392(15) 0.39357(12) 0.59563(15) 0.0253(5) Uani 1 1 d . . . . .
C4 C 0.38802(15) 0.46770(12) 0.76669(15) 0.0235(5) Uani 1 1 d . . . . .
C4S C 0.97129(15) 0.40601(11) 0.69148(14) 0.0221(5) Uani 1 1 d . . . . .
C5 C 0.43777(14) 0.45517(12) 0.70232(14) 0.0235(5) Uani 1 1 d . . . . .
C6 C 0.54687(14) 0.44330(12) 0.73302(14) 0.0217(4) Uani 1 1 d . . . . .
C7 C 0.62171(14) 0.42702(12) 0.68313(13) 0.0211(4) Uani 1 1 d . . . . .
C8 C 0.72607(14) 0.42206(12) 0.75801(14) 0.0221(5) Uani 1 1 d . . . . .
C9 C 0.62435(15) 0.49459(12) 0.62144(14) 0.0251(5) Uani 1 1 d . . . . .
H9A H 0.5547 0.5026 0.5793 0.038 Uiso 1 1 calc R U . . .
H9B H 0.6726 0.4816 0.5902 0.038 Uiso 1 1 calc R U . . .
H9C H 0.6475 0.5428 0.6553 0.038 Uiso 1 1 calc R U . . .
C10 C 0.59680(16) 0.34668(12) 0.63658(15) 0.0287(5) Uani 1 1 d . . . . .
H10A H 0.5974 0.3058 0.6793 0.043 Uiso 1 1 calc R U . . .
H10B H 0.6491 0.3345 0.6092 0.043 Uiso 1 1 calc R U . . .
H10C H 0.5281 0.3488 0.5917 0.043 Uiso 1 1 calc R U . . .
C11 C 0.82475(14) 0.41555(12) 0.75566(14) 0.0236(5) Uani 1 1 d . . . . .
H11 H 0.8769 0.4172 0.8115 0.028 Uiso 1 1 calc R U . . .
C12 C 0.27832(15) 0.47601(11) 0.73917(15) 0.0261(5) Uani 1 1 d . . . . .
H12 H 0.2451 0.4844 0.7814 0.031 Uiso 1 1 calc R U . . .
C13 C 0.22016(15) 0.47214(12) 0.65292(16) 0.0285(5) Uani 1 1 d . . . . .
H13 H 0.1467 0.4761 0.6356 0.034 Uiso 1 1 calc R U . . .
C14 C 0.26890(15) 0.46223(12) 0.58959(16) 0.0288(5) Uani 1 1 d . . . . .
H14 H 0.2281 0.4612 0.5295 0.035 Uiso 1 1 calc R U . . .
C15 C 0.37449(15) 0.45403(12) 0.61337(15) 0.0270(5) Uani 1 1 d . . . . .
H15 H 0.4057 0.4475 0.5695 0.032 Uiso 1 1 calc R U . . .
C16 C 0.68567(15) 0.31994(12) 0.33259(15) 0.0247(5) Uani 1 1 d . . . . .
H16A H 0.7177 0.3456 0.3899 0.030 Uiso 1 1 calc R U . . .
H16B H 0.6599 0.3620 0.2886 0.030 Uiso 1 1 calc R U . . .
C17 C 0.59354(15) 0.27212(12) 0.33627(15) 0.0272(5) Uani 1 1 d . . . . .
H17A H 0.6176 0.2289 0.3790 0.033 Uiso 1 1 calc R U . . .
H17B H 0.5573 0.2487 0.2784 0.033 Uiso 1 1 calc R U . . .
C18 C 0.51912(15) 0.32555(13) 0.36315(15) 0.0282(5) Uani 1 1 d . . . . .
H18A H 0.5573 0.3517 0.4190 0.034 Uiso 1 1 calc R U . . .
H18B H 0.4926 0.3669 0.3184 0.034 Uiso 1 1 calc R U . . .
C19 C 0.42775(17) 0.27992(14) 0.37358(19) 0.0418(6) Uani 1 1 d . . . . .
H19A H 0.3865 0.2575 0.3172 0.063 Uiso 1 1 calc R U . . .
H19B H 0.3843 0.3154 0.3942 0.063 Uiso 1 1 calc R U . . .
H19C H 0.4538 0.2375 0.4160 0.063 Uiso 1 1 calc R U . . .
C20 C 0.73007(15) 0.24196(12) 0.21803(14) 0.0255(5) Uani 1 1 d . . . . .
H20A H 0.6733 0.2044 0.2139 0.031 Uiso 1 1 calc R U . . .
H20B H 0.7869 0.2122 0.2072 0.031 Uiso 1 1 calc R U . . .
C21 C 0.69017(16) 0.30320(13) 0.14613(14) 0.0296(5) Uani 1 1 d . . . . .
H21A H 0.6241 0.3255 0.1483 0.035 Uiso 1 1 calc R U . . .
H21B H 0.7411 0.3465 0.1556 0.035 Uiso 1 1 calc R U . . .
C22 C 0.67277(19) 0.26651(14) 0.05688(16) 0.0367(6) Uani 1 1 d . . . . .
H22A H 0.6329 0.3037 0.0112 0.044 Uiso 1 1 calc R U . . .
H22B H 0.6305 0.2183 0.0517 0.044 Uiso 1 1 calc R U . . .
C23 C 0.7733(2) 0.24559(16) 0.04062(19) 0.0534(8) Uani 1 1 d . . . . .
H23A H 0.7575 0.2276 -0.0197 0.080 Uiso 1 1 calc R U . . .
H23B H 0.8089 0.2037 0.0807 0.080 Uiso 1 1 calc R U . . .
H23C H 0.8181 0.2921 0.0504 0.080 Uiso 1 1 calc R U . . .
C24 C 0.85850(15) 0.33238(12) 0.32229(16) 0.0283(5) Uani 1 1 d . . . . .
H24A H 0.8299 0.3797 0.2871 0.034 Uiso 1 1 calc R U . . .
H24B H 0.8840 0.3488 0.3843 0.034 Uiso 1 1 calc R U . . .
C25 C 0.95067(16) 0.30436(14) 0.29813(18) 0.0375(6) Uani 1 1 d . . . . .
H25A H 0.9280 0.2888 0.2359 0.045 Uiso 1 1 calc R U . . .
H25B H 0.9828 0.2582 0.3340 0.045 Uiso 1 1 calc R U . . .
C26 C 1.02924(18) 0.37170(15) 0.3145(2) 0.0495(8) Uani 1 1 d . . . . .
H26A H 0.9938 0.4192 0.2834 0.059 Uiso 1 1 calc R U . . .
H26B H 1.0551 0.3838 0.3777 0.059 Uiso 1 1 calc R U . . .
C27 C 1.1209(2) 0.35264(18) 0.2846(2) 0.0700(10) Uani 1 1 d . . . . .
H27A H 1.0965 0.3450 0.2212 0.105 Uiso 1 1 calc R U . . .
H27B H 1.1547 0.3045 0.3134 0.105 Uiso 1 1 calc R U . . .
H27C H 1.1707 0.3962 0.2999 0.105 Uiso 1 1 calc R U . . .
C28 C 0.80552(15) 0.20366(12) 0.37035(14) 0.0258(5) Uani 1 1 d . . . . .
H28A H 0.7484 0.1648 0.3565 0.031 Uiso 1 1 calc R U . . .
H28B H 0.8646 0.1787 0.3578 0.031 Uiso 1 1 calc R U . . .
C29 C 0.83868(17) 0.22234(13) 0.46711(15) 0.0317(5) Uani 1 1 d . . . . .
H29A H 0.7795 0.2458 0.4807 0.038 Uiso 1 1 calc R U . . .
H29B H 0.8954 0.2616 0.4816 0.038 Uiso 1 1 calc R U . . .
C30 C 0.87545(17) 0.14964(13) 0.52302(15) 0.0310(5) Uani 1 1 d . . . . .
H30A H 0.9424 0.1319 0.5181 0.037 Uiso 1 1 calc R U . . .
H30B H 0.8243 0.1068 0.5013 0.037 Uiso 1 1 calc R U . . .
C31 C 0.8891(2) 0.16608(15) 0.61872(16) 0.0413(6) Uani 1 1 d . . . . .
H31A H 0.8218 0.1797 0.6243 0.062 Uiso 1 1 calc R U . . .
H31B H 0.9375 0.2100 0.6396 0.062 Uiso 1 1 calc R U . . .
H31C H 0.9168 0.1192 0.6536 0.062 Uiso 1 1 calc R U . . .
N1 N 0.70605(12) 0.42784(10) 0.83573(11) 0.0244(4) Uani 1 1 d . . . . .
N2 N 0.76967(12) 0.27410(10) 0.31035(12) 0.0237(4) Uani 1 1 d . . . . .
O1A O 0.92604(11) 0.56412(10) 1.08943(10) 0.0341(4) Uani 1 1 d . . . . .
H1A H 0.9316 0.5690 1.1423 0.051 Uiso 1 1 calc R U . . .
O1S O 0.74911(10) 0.38325(9) 0.53072(10) 0.0312(4) Uani 1 1 d . . . . .
O2A O 0.81416(15) 0.47026(11) 1.09341(12) 0.0538(5) Uani 1 1 d . . . . .
O2S O 0.98962(11) 0.38536(10) 0.54281(10) 0.0345(4) Uani 1 1 d . . . . .
O3S O 1.05639(10) 0.41225(9) 0.75290(10) 0.0282(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.375(3) . ?
C1 N1 1.403(2) . ?
C1 C2 1.407(3) . ?
C1A N1 1.448(3) . ?
C1A C2A 1.533(3) . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C1S C11 1.425(3) . ?
C1S C4S 1.432(3) . ?
C1S C2S 1.462(3) . ?
C2 C3 1.376(3) . ?
C2 H2 0.9500 . ?
C2A C3A 1.509(3) . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C2S O1S 1.232(2) . ?
C2S C3S 1.515(3) . ?
C3 C4 1.413(3) . ?
C3 H3 0.9500 . ?
C3A O2A 1.211(3) . ?
C3A O1A 1.311(2) . ?
C3S O2S 1.224(3) . ?
C3S C4S 1.490(3) . ?
C4 C12 1.422(3) . ?
C4 C5 1.438(3) . ?
C4S O3S 1.261(2) . ?
C5 C15 1.417(3) . ?
C5 C6 1.420(3) . ?
C6 C7 1.524(3) . ?
C7 C9 1.533(3) . ?
C7 C8 1.540(3) . ?
C7 C10 1.545(3) . ?
C8 C11 1.365(3) . ?
C8 N1 1.380(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11 0.9500 . ?
C12 C13 1.364(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.407(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.371(3) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.516(3) . ?
C16 N2 1.526(2) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.530(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.526(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 N2 1.517(3) . ?
C20 C21 1.525(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.523(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.523(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.514(3) . ?
C24 N2 1.529(2) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.532(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.520(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.518(3) . ?
C28 N2 1.520(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.518(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.528(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
O1A H1A 0.8400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 N1 109.96(18) . . ?
C6 C1 C2 123.32(19) . . ?
N1 C1 C2 126.72(19) . . ?
N1 C1A C2A 114.04(18) . . ?
N1 C1A H1AA 108.7 . . ?
C2A C1A H1AA 108.7 . . ?
N1 C1A H1AB 108.7 . . ?
C2A C1A H1AB 108.7 . . ?
H1AA C1A H1AB 107.6 . . ?
C11 C1S C4S 126.22(18) . . ?
C11 C1S C2S 142.12(18) . . ?
C4S C1S C2S 91.61(16) . . ?
C3 C2 C1 117.1(2) . . ?
C3 C2 H2 121.4 . . ?
C1 C2 H2 121.4 . . ?
C3A C2A C1A 111.96(18) . . ?
C3A C2A H2AA 109.2 . . ?
C1A C2A H2AA 109.2 . . ?
C3A C2A H2AB 109.2 . . ?
C1A C2A H2AB 109.2 . . ?
H2AA C2A H2AB 107.9 . . ?
O1S C2S C1S 137.43(19) . . ?
O1S C2S C3S 133.1(2) . . ?
C1S C2S C3S 89.46(16) . . ?
C2 C3 C4 122.3(2) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
O2A C3A O1A 123.9(2) . . ?
O2A C3A C2A 122.7(2) . . ?
O1A C3A C2A 113.37(19) . . ?
O2S C3S C4S 137.54(19) . . ?
O2S C3S C2S 135.1(2) . . ?
C4S C3S C2S 87.31(16) . . ?
C3 C4 C12 121.0(2) . . ?
C3 C4 C5 119.74(18) . . ?
C12 C4 C5 119.2(2) . . ?
O3S C4S C1S 135.1(2) . . ?
O3S C4S C3S 133.25(18) . . ?
C1S C4S C3S 91.61(16) . . ?
C15 C5 C6 124.8(2) . . ?
C15 C5 C4 117.86(18) . . ?
C6 C5 C4 117.30(19) . . ?
C1 C6 C5 120.18(19) . . ?
C1 C6 C7 109.32(17) . . ?
C5 C6 C7 130.46(19) . . ?
C6 C7 C9 112.05(16) . . ?
C6 C7 C8 101.45(17) . . ?
C9 C7 C8 109.97(16) . . ?
C6 C7 C10 110.05(16) . . ?
C9 C7 C10 113.14(18) . . ?
C8 C7 C10 109.55(16) . . ?
C11 C8 N1 121.79(18) . . ?
C11 C8 C7 130.32(19) . . ?
N1 C8 C7 107.87(16) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 C1S 132.02(19) . . ?
C8 C11 H11 114.0 . . ?
C1S C11 H11 114.0 . . ?
C13 C12 C4 120.9(2) . . ?
C13 C12 H12 119.6 . . ?
C4 C12 H12 119.6 . . ?
C12 C13 C14 120.02(19) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15 C14 C13 120.9(2) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C14 C15 C5 121.1(2) . . ?
C14 C15 H15 119.5 . . ?
C5 C15 H15 119.5 . . ?
C17 C16 N2 115.69(16) . . ?
C17 C16 H16A 108.4 . . ?
N2 C16 H16A 108.4 . . ?
C17 C16 H16B 108.4 . . ?
N2 C16 H16B 108.4 . . ?
H16A C16 H16B 107.4 . . ?
C16 C17 C18 109.29(17) . . ?
C16 C17 H17A 109.8 . . ?
C18 C17 H17A 109.8 . . ?
C16 C17 H17B 109.8 . . ?
C18 C17 H17B 109.8 . . ?
H17A C17 H17B 108.3 . . ?
C19 C18 C17 111.94(18) . . ?
C19 C18 H18A 109.2 . . ?
C17 C18 H18A 109.2 . . ?
C19 C18 H18B 109.2 . . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C20 C21 115.51(17) . . ?
N2 C20 H20A 108.4 . . ?
C21 C20 H20A 108.4 . . ?
N2 C20 H20B 108.4 . . ?
C21 C20 H20B 108.4 . . ?
H20A C20 H20B 107.5 . . ?
C22 C21 C20 110.63(18) . . ?
C22 C21 H21A 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 108.1 . . ?
C21 C22 C23 113.2(2) . . ?
C21 C22 H22A 108.9 . . ?
C23 C22 H22A 108.9 . . ?
C21 C22 H22B 108.9 . . ?
C23 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 N2 117.11(17) . . ?
C25 C24 H24A 108.0 . . ?
N2 C24 H24A 108.0 . . ?
C25 C24 H24B 108.0 . . ?
N2 C24 H24B 108.0 . . ?
H24A C24 H24B 107.3 . . ?
C24 C25 C26 108.31(19) . . ?
C24 C25 H25A 110.0 . . ?
C26 C25 H25A 110.0 . . ?
C24 C25 H25B 110.0 . . ?
C26 C25 H25B 110.0 . . ?
H25A C25 H25B 108.4 . . ?
C27 C26 C25 112.9(2) . . ?
C27 C26 H26A 109.0 . . ?
C25 C26 H26A 109.0 . . ?
C27 C26 H26B 109.0 . . ?
C25 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 N2 114.90(17) . . ?
C29 C28 H28A 108.5 . . ?
N2 C28 H28A 108.5 . . ?
C29 C28 H28B 108.5 . . ?
N2 C28 H28B 108.5 . . ?
H28A C28 H28B 107.5 . . ?
C28 C29 C30 112.01(18) . . ?
C28 C29 H29A 109.2 . . ?
C30 C29 H29A 109.2 . . ?
C28 C29 H29B 109.2 . . ?
C30 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
C29 C30 C31 111.34(19) . . ?
C29 C30 H30A 109.4 . . ?
C31 C30 H30A 109.4 . . ?
C29 C30 H30B 109.4 . . ?
C31 C30 H30B 109.4 . . ?
H30A C30 H30B 108.0 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C8 N1 C1 111.15(16) . . ?
C8 N1 C1A 125.73(17) . . ?
C1 N1 C1A 123.09(18) . . ?
C20 N2 C28 106.45(15) . . ?
C20 N2 C16 111.56(15) . . ?
C28 N2 C16 111.07(16) . . ?
C20 N2 C24 111.59(17) . . ?
C28 N2 C24 110.87(15) . . ?
C16 N2 C24 105.39(15) . . ?
C3A O1A H1A 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
C6 C1 C2 C3 1.1(3) . . . . ?
N1 C1 C2 C3 -179.35(19) . . . . ?
N1 C1A C2A C3A 143.46(18) . . . . ?
C11 C1S C2S O1S 0.0(5) . . . . ?
C4S C1S C2S O1S 177.4(3) . . . . ?
C11 C1S C2S C3S -178.3(3) . . . . ?
C4S C1S C2S C3S -0.91(16) . . . . ?
C1 C2 C3 C4 1.2(3) . . . . ?
C1A C2A C3A O2A -18.4(3) . . . . ?
C1A C2A C3A O1A 164.52(18) . . . . ?
O1S C2S C3S O2S 1.1(4) . . . . ?
C1S C2S C3S O2S 179.5(3) . . . . ?
O1S C2S C3S C4S -177.5(2) . . . . ?
C1S C2S C3S C4S 0.87(15) . . . . ?
C2 C3 C4 C12 175.79(19) . . . . ?
C2 C3 C4 C5 -2.4(3) . . . . ?
C11 C1S C4S O3S -0.3(4) . . . . ?
C2S C1S C4S O3S -178.3(2) . . . . ?
C11 C1S C4S C3S 178.9(2) . . . . ?
C2S C1S C4S C3S 0.92(16) . . . . ?
O2S C3S C4S O3S -0.2(4) . . . . ?
C2S C3S C4S O3S 178.4(2) . . . . ?
O2S C3S C4S C1S -179.5(3) . . . . ?
C2S C3S C4S C1S -0.89(16) . . . . ?
C3 C4 C5 C15 -179.96(19) . . . . ?
C12 C4 C5 C15 1.8(3) . . . . ?
C3 C4 C5 C6 1.2(3) . . . . ?
C12 C4 C5 C6 -176.97(18) . . . . ?
N1 C1 C6 C5 178.19(17) . . . . ?
C2 C1 C6 C5 -2.2(3) . . . . ?
N1 C1 C6 C7 0.1(2) . . . . ?
C2 C1 C6 C7 179.70(18) . . . . ?
C15 C5 C6 C1 -177.8(2) . . . . ?
C4 C5 C6 C1 1.0(3) . . . . ?
C15 C5 C6 C7 -0.1(3) . . . . ?
C4 C5 C6 C7 178.59(19) . . . . ?
C1 C6 C7 C9 -120.16(19) . . . . ?
C5 C6 C7 C9 62.0(3) . . . . ?
C1 C6 C7 C8 -2.9(2) . . . . ?
C5 C6 C7 C8 179.3(2) . . . . ?
C1 C6 C7 C10 113.03(19) . . . . ?
C5 C6 C7 C10 -64.8(3) . . . . ?
C6 C7 C8 C11 -173.4(2) . . . . ?
C9 C7 C8 C11 -54.6(3) . . . . ?
C10 C7 C8 C11 70.3(3) . . . . ?
C6 C7 C8 N1 4.7(2) . . . . ?
C9 C7 C8 N1 123.50(18) . . . . ?
C10 C7 C8 N1 -111.56(19) . . . . ?
N1 C8 C11 C1S 178.0(2) . . . . ?
C7 C8 C11 C1S -4.1(4) . . . . ?
C4S C1S C11 C8 175.4(2) . . . . ?
C2S C1S C11 C8 -7.9(5) . . . . ?
C3 C4 C12 C13 -178.1(2) . . . . ?
C5 C4 C12 C13 0.1(3) . . . . ?
C4 C12 C13 C14 -2.0(3) . . . . ?
C12 C13 C14 C15 1.9(3) . . . . ?
C13 C14 C15 C5 0.1(3) . . . . ?
C6 C5 C15 C14 176.77(19) . . . . ?
C4 C5 C15 C14 -1.9(3) . . . . ?
N2 C16 C17 C18 177.51(18) . . . . ?
C16 C17 C18 C19 -176.5(2) . . . . ?
N2 C20 C21 C22 168.85(17) . . . . ?
C20 C21 C22 C23 -71.0(2) . . . . ?
N2 C24 C25 C26 179.6(2) . . . . ?
C24 C25 C26 C27 -174.7(3) . . . . ?
N2 C28 C29 C30 -178.87(17) . . . . ?
C28 C29 C30 C31 -169.34(19) . . . . ?
C11 C8 N1 C1 173.23(19) . . . . ?
C7 C8 N1 C1 -5.1(2) . . . . ?
C11 C8 N1 C1A -4.7(3) . . . . ?
C7 C8 N1 C1A 176.97(18) . . . . ?
C6 C1 N1 C8 3.2(2) . . . . ?
C2 C1 N1 C8 -176.3(2) . . . . ?
C6 C1 N1 C1A -178.76(19) . . . . ?
C2 C1 N1 C1A 1.7(3) . . . . ?
C2A C1A N1 C8 85.5(3) . . . . ?
C2A C1A N1 C1 -92.2(2) . . . . ?
C21 C20 N2 C28 -179.72(17) . . . . ?
C21 C20 N2 C16 59.0(2) . . . . ?
C21 C20 N2 C24 -58.6(2) . . . . ?
C29 C28 N2 C20 -174.34(17) . . . . ?
C29 C28 N2 C16 -52.7(2) . . . . ?
C29 C28 N2 C24 64.1(2) . . . . ?
C17 C16 N2 C20 65.8(2) . . . . ?
C17 C16 N2 C28 -52.8(2) . . . . ?
C17 C16 N2 C24 -172.91(19) . . . . ?
C25 C24 N2 C20 -54.4(2) . . . . ?
C25 C24 N2 C28 64.1(3) . . . . ?
C25 C24 N2 C16 -175.7(2) . . . . ?

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
O1A H1A O3S 0.84 1.69 2.523(2) 174.7 3_767

_refine_diff_density_max         0.271
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.050

_shelxl_version_number           2013-4


####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1030512'
_audit_update_record             
;
2014-10-22 deposited with the CCDC.
2014-12-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H41 N O5'
_chemical_formula_sum            'C30 H41 N O5'
_chemical_formula_weight         495.64

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'

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

_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                   9.8804(17)
_cell_length_b                   16.659(3)
_cell_length_c                   18.091(3)
_cell_angle_alpha                75.4470(10)
_cell_angle_beta                 81.260(11)
_cell_angle_gamma                74.709(9)
_cell_volume                     2768.4(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4858
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      27.5

_exptl_crystal_description       fragment
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_F_000             1072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.080
_shelx_estimated_absorpt_T_min   0.987
_shelx_estimated_absorpt_T_max   0.998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.263
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           'Mo K\a'
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Mitegen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_reflns_number            37607
_diffrn_reflns_av_unetI/netI     0.0931
_diffrn_reflns_av_R_equivalents  0.1004
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.146
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12648
_reflns_number_gt                7291
_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       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_structure_solution    
'SUPERFLIP (Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  
'WinGX, ver.2013.3 (L.J. Farrugia, J.App.Cryst.(2012),45,849-854)'

_refine_special_details          
;
In (7) disordered ethoxy group on one of two independent 
molecules present in the asymmetric unit was modelled 
over two sites with 68:32 ratio.
Vibrational restraints (SIMU/DELU) as well as distance 
restraints DFIX/DANG were used to maintain sensible molecular 
geometry and atomic displacement ellipsoids.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0760P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12648
_refine_ls_number_parameters     679
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0646
_refine_ls_wR_factor_ref         0.1746
_refine_ls_wR_factor_gt          0.1548
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_restrained_S_all      0.886
_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
C1 C 0.63372(19) 0.63140(12) 0.45546(11) 0.0209(4) Uani 1 1 d . . . . .
C1A C 0.70357(19) 0.47025(12) 0.48032(11) 0.0208(4) Uani 1 1 d . . . . .
H1AA H 0.6462 0.4290 0.4825 0.025 Uiso 1 1 calc R U . . .
H1AB H 0.7091 0.4738 0.5335 0.025 Uiso 1 1 calc R U . . .
C1S C 0.48654(19) 0.50030(12) 0.27969(11) 0.0208(4) Uani 1 1 d . . . . .
C2 C 0.6868(2) 0.64392(12) 0.51761(12) 0.0240(4) Uani 1 1 d . . . . .
H2 H 0.7356 0.5973 0.5535 0.029 Uiso 1 1 calc R U . . .
C2A C 0.85173(19) 0.43798(12) 0.44412(12) 0.0244(4) Uani 1 1 d . . . . .
H2AA H 0.9128 0.4746 0.4488 0.029 Uiso 1 1 calc R U . . .
H2AB H 0.8478 0.4424 0.3888 0.029 Uiso 1 1 calc R U . . .
C2S C 0.40227(19) 0.55475(13) 0.21447(11) 0.0219(4) Uani 1 1 d . . . . .
C3 C 0.6652(2) 0.72789(13) 0.52488(12) 0.0248(4) Uani 1 1 d . . . . .
H3 H 0.7003 0.7387 0.5666 0.030 Uiso 1 1 calc R U . . .
C3A C 0.9165(2) 0.34498(13) 0.48228(12) 0.0264(5) Uani 1 1 d . . . . .
H3AA H 1.0183 0.3313 0.4650 0.032 Uiso 1 1 calc R U . . .
H3AB H 0.9074 0.3393 0.5385 0.032 Uiso 1 1 calc R U . . .
C3S C 0.39682(19) 0.47424(13) 0.19128(12) 0.0231(4) Uani 1 1 d . . . . .
C4 C 0.5924(2) 0.79693(12) 0.47187(12) 0.0234(4) Uani 1 1 d . . . . .
C4A C 0.8490(2) 0.27998(12) 0.46472(12) 0.0260(5) Uani 1 1 d . . . . .
H4AA H 0.8559 0.2864 0.4085 0.031 Uiso 1 1 calc R U . . .
H4AB H 0.7478 0.2923 0.4834 0.031 Uiso 1 1 calc R U . . .
C4S C 0.47954(19) 0.42730(13) 0.25673(12) 0.0241(4) Uani 1 1 d . . . . .
C5 C 0.54301(19) 0.78169(12) 0.40897(11) 0.0231(4) Uani 1 1 d . . . . .
H5 H 0.4951 0.8280 0.3724 0.028 Uiso 1 1 calc R U . . .
C5A C 0.9180(2) 0.18771(13) 0.50162(13) 0.0317(5) Uani 1 1 d . . . . .
H5AA H 0.9145 0.1821 0.5576 0.038 Uiso 1 1 calc R U . . .
H5AB H 1.0185 0.1750 0.4815 0.038 Uiso 1 1 calc R U . . .
C6 C 0.56448(19) 0.69925(12) 0.40058(11) 0.0205(4) Uani 1 1 d . . . . .
C6A C 0.8490(2) 0.12143(14) 0.48733(13) 0.0332(5) Uani 1 1 d . . . . .
H6AA H 0.8968 0.0641 0.5151 0.040 Uiso 1 1 calc R U . . .
H6AB H 0.7494 0.1330 0.5090 0.040 Uiso 1 1 calc R U . . .
C7 C 0.51743(19) 0.66454(12) 0.34126(11) 0.0204(4) Uani 1 1 d . . . . .
C7A C 0.8536(2) 0.12032(14) 0.40264(13) 0.0334(5) Uani 1 1 d . . . . .
H7AA H 0.7969 0.1756 0.3761 0.040 Uiso 1 1 calc R U . . .
H7AB H 0.9521 0.1153 0.3796 0.040 Uiso 1 1 calc R U . . .
C8 C 0.56654(19) 0.56776(12) 0.37200(11) 0.0199(4) Uani 1 1 d . . . . .
C8A C 0.7993(2) 0.04849(14) 0.38788(13) 0.0341(5) Uani 1 1 d . . . . .
H8AA H 0.8555 -0.0069 0.4146 0.041 Uiso 1 1 calc R U . . .
H8AB H 0.7003 0.0537 0.4103 0.041 Uiso 1 1 calc R U . . .
C9 C 0.35565(19) 0.69487(12) 0.33963(12) 0.0240(4) Uani 1 1 d . . . . .
H9A H 0.3101 0.6786 0.3913 0.036 Uiso 1 1 calc R U . . .
H9B H 0.3248 0.6682 0.3047 0.036 Uiso 1 1 calc R U . . .
H9C H 0.3295 0.7571 0.3218 0.036 Uiso 1 1 calc R U . . .
C9A C 0.8060(2) 0.04832(14) 0.30303(13) 0.0340(5) Uani 1 1 d . . . . .
H9AA H 0.7510 0.1041 0.2763 0.041 Uiso 1 1 calc R U . . .
H9AB H 0.9052 0.0425 0.2809 0.041 Uiso 1 1 calc R U . . .
C10 C 0.5938(2) 0.68984(13) 0.26139(11) 0.0256(4) Uani 1 1 d . . . . .
H10A H 0.5752 0.7522 0.2454 0.038 Uiso 1 1 calc R U . . .
H10B H 0.5595 0.6675 0.2245 0.038 Uiso 1 1 calc R U . . .
H10C H 0.6954 0.6660 0.2634 0.038 Uiso 1 1 calc R U . . .
C10A C 0.7510(3) -0.02154(15) 0.28745(14) 0.0404(6) Uani 1 1 d . . . . .
H10D H 0.6477 -0.0093 0.3004 0.048 Uiso 1 1 calc R U . . .
H10E H 0.7926 -0.0761 0.3219 0.048 Uiso 1 1 calc R U . . .
C11 C 0.55440(19) 0.50161(12) 0.34343(11) 0.0216(4) Uani 1 1 d . . . . .
H11 H 0.5991 0.4468 0.3709 0.026 Uiso 1 1 calc R U . . .
C11A C 0.7824(3) -0.03257(16) 0.20444(14) 0.0433(6) Uani 1 1 d . . . . .
H11A H 0.8857 -0.0465 0.1916 0.052 Uiso 1 1 calc R U . . .
H11B H 0.7465 -0.0812 0.2001 0.052 Uiso 1 1 calc R U . . .
C11B C 0.19995(18) 0.47462(12) 0.97662(11) 0.0192(4) Uani 1 1 d . . . . .
H11C H 0.1529 0.4293 0.9757 0.023 Uiso 1 1 calc R U . . .
H11D H 0.2000 0.4767 1.0308 0.023 Uiso 1 1 calc R U . . .
C12 C 0.5592(2) 0.88485(13) 0.48326(12) 0.0263(5) Uani 1 1 d . . . . .
C12A C 0.7161(3) 0.04690(16) 0.14689(14) 0.0428(6) Uani 1 1 d . . . . .
H12A H 0.7333 0.0351 0.0954 0.064 Uiso 1 1 calc R U . . .
H12B H 0.7581 0.0939 0.1473 0.064 Uiso 1 1 calc R U . . .
H12C H 0.6144 0.0628 0.1609 0.064 Uiso 1 1 calc R U . . .
C12B C 0.35169(19) 0.45288(12) 0.94100(12) 0.0234(4) Uani 1 1 d . . . . .
H12D H 0.3996 0.4971 0.9439 0.028 Uiso 1 1 calc R U . . .
H12E H 0.3513 0.4535 0.8862 0.028 Uiso 1 1 calc R U . . .
C13B C 0.4343(2) 0.36524(13) 0.98141(12) 0.0259(5) Uani 1 1 d . . . . .
H13A H 0.5356 0.3594 0.9637 0.031 Uiso 1 1 calc R U . . .
H13B H 0.4236 0.3622 1.0373 0.031 Uiso 1 1 calc R U . . .
C14B C 0.3874(2) 0.29060(13) 0.96719(12) 0.0279(5) Uani 1 1 d . . . . .
H14A H 0.4058 0.2904 0.9119 0.033 Uiso 1 1 calc R U . . .
H14B H 0.2846 0.2986 0.9810 0.033 Uiso 1 1 calc R U . . .
C15B C 0.4630(2) 0.20465(13) 1.01321(12) 0.0316(5) Uani 1 1 d . . . . .
H15A H 0.4491 0.2063 1.0682 0.038 Uiso 1 1 calc R U . . .
H15B H 0.5653 0.1957 0.9973 0.038 Uiso 1 1 calc R U . . .
C16B C 0.4127(2) 0.12887(14) 1.00348(13) 0.0355(5) Uani 1 1 d . . . . .
H16A H 0.4630 0.0765 1.0374 0.043 Uiso 1 1 calc R U . . .
H16B H 0.3110 0.1373 1.0210 0.043 Uiso 1 1 calc R U . . .
C17B C 0.4342(2) 0.11477(14) 0.92208(13) 0.0336(5) Uani 1 1 d . . . . .
H17A H 0.3771 0.1650 0.8889 0.040 Uiso 1 1 calc R U . . .
H17B H 0.3983 0.0646 0.9222 0.040 Uiso 1 1 calc R U . . .
C18B C 0.5880(2) 0.10052(14) 0.88713(13) 0.0353(5) Uani 1 1 d . . . . .
H18A H 0.6173 0.1551 0.8756 0.042 Uiso 1 1 calc R U . . .
H18B H 0.6487 0.0593 0.9254 0.042 Uiso 1 1 calc R U . . .
C19B C 0.6113(2) 0.06712(14) 0.81396(13) 0.0341(5) Uani 1 1 d . . . . .
H19A H 0.5860 0.0112 0.8261 0.041 Uiso 1 1 calc R U . . .
H19B H 0.5470 0.1070 0.7768 0.041 Uiso 1 1 calc R U . . .
C20B C 0.7618(2) 0.05646(15) 0.77634(13) 0.0371(6) Uani 1 1 d . . . . .
H20A H 0.8250 0.0123 0.8116 0.044 Uiso 1 1 calc R U . . .
H20B H 0.7904 0.1108 0.7688 0.044 Uiso 1 1 calc R U . . .
C21B C 0.7822(2) 0.03111(16) 0.69900(14) 0.0459(7) Uani 1 1 d . . . . .
H21A H 0.7180 0.0748 0.6640 0.055 Uiso 1 1 calc R U . . .
H21B H 0.8800 0.0310 0.6764 0.055 Uiso 1 1 calc R U . . .
C21S C -0.01680(19) 0.49793(12) 0.77751(11) 0.0209(4) Uani 1 1 d . . . . .
C22B C 0.7548(3) -0.05602(18) 0.70393(17) 0.0575(8) Uani 1 1 d . . . . .
H22A H 0.7685 -0.0676 0.6525 0.086 Uiso 1 1 calc R U . . .
H22B H 0.6578 -0.0564 0.7256 0.086 Uiso 1 1 calc R U . . .
H22C H 0.8204 -0.1001 0.7368 0.086 Uiso 1 1 calc R U . . .
C22S C -0.09977(19) 0.55074(13) 0.71136(11) 0.0215(4) Uani 1 1 d . . . . .
C23S C -0.10423(19) 0.46858(12) 0.69014(11) 0.0216(4) Uani 1 1 d . . . . .
C24S C -0.02442(19) 0.42376(12) 0.75685(11) 0.0205(4) Uani 1 1 d . . . . .
C25S C -0.0114(2) 0.27754(13) 0.76365(13) 0.0300(5) Uani 1 1 d . . . . .
H25A H -0.1129 0.2955 0.7557 0.036 Uiso 1 1 calc R U . . .
H25B H 0.0039 0.2237 0.8033 0.036 Uiso 1 1 calc R U . . .
C26S C 0.0718(2) 0.26186(15) 0.69044(14) 0.0406(6) Uani 1 1 d . . . . .
H26A H 0.0593 0.3154 0.6515 0.061 Uiso 1 1 calc R U . . .
H26B H 0.0390 0.2198 0.6728 0.061 Uiso 1 1 calc R U . . .
H26C H 0.1718 0.2401 0.6990 0.061 Uiso 1 1 calc R U . . .
C101 C 0.11263(19) 0.63352(12) 0.95599(11) 0.0200(4) Uani 1 1 d . . . . .
C102 C 0.1648(2) 0.64569(12) 1.01852(11) 0.0230(4) Uani 1 1 d . . . . .
H102 H 0.2162 0.5991 1.0534 0.028 Uiso 1 1 calc R U . . .
C103 C 0.1385(2) 0.72881(12) 1.02786(11) 0.0238(4) Uani 1 1 d . . . . .
H103 H 0.1741 0.7396 1.0694 0.029 Uiso 1 1 calc R U . . .
C104 C 0.0603(2) 0.79728(12) 0.97680(12) 0.0240(4) Uani 1 1 d . . . . .
C105 C 0.0106(2) 0.78289(12) 0.91341(11) 0.0232(4) Uani 1 1 d . . . . .
H105 H -0.0410 0.8292 0.8783 0.028 Uiso 1 1 calc R U . . .
C106 C 0.03760(19) 0.70088(12) 0.90308(11) 0.0204(4) Uani 1 1 d . . . . .
C107 C -0.00415(19) 0.66592(12) 0.84213(11) 0.0201(4) Uani 1 1 d . . . . .
C108 C 0.05414(19) 0.56926(12) 0.87014(11) 0.0191(4) Uani 1 1 d . . . . .
C109 C -0.16529(19) 0.69051(12) 0.84065(11) 0.0228(4) Uani 1 1 d . . . . .
H10F H -0.2096 0.6713 0.8921 0.034 Uiso 1 1 calc R U . . .
H10G H -0.1916 0.6633 0.8046 0.034 Uiso 1 1 calc R U . . .
H10H H -0.1973 0.7526 0.8243 0.034 Uiso 1 1 calc R U . . .
C110 C 0.0680(2) 0.69746(13) 0.76221(11) 0.0260(4) Uani 1 1 d . . . . .
H11E H 0.0462 0.7600 0.7496 0.039 Uiso 1 1 calc R U . . .
H11F H 0.0334 0.6773 0.7238 0.039 Uiso 1 1 calc R U . . .
H11G H 0.1702 0.6751 0.7624 0.039 Uiso 1 1 calc R U . . .
C111 C 0.04894(19) 0.50210(12) 0.84061(11) 0.0203(4) Uani 1 1 d . . . . .
H111 H 0.0986 0.4482 0.8674 0.024 Uiso 1 1 calc R U . . .
C112 C 0.0306(2) 0.88492(13) 0.98876(12) 0.0263(5) Uani 1 1 d . . . . .
N1 N 0.63412(16) 0.55457(10) 0.43688(9) 0.0198(3) Uani 1 1 d . . . . .
N101 N 0.12102(15) 0.55682(10) 0.93520(9) 0.0187(3) Uani 1 1 d . . . . .
O1 O 0.60855(16) 0.89482(9) 0.54333(9) 0.0346(4) Uani 1 1 d . . . . .
H1 H 0.5823 0.9463 0.5462 0.052 Uiso 1 1 calc R U . . .
O1S O 0.35610(14) 0.63036(9) 0.18820(8) 0.0270(3) Uani 1 1 d . . . . .
O2 O 0.48587(14) 0.94513(9) 0.43983(8) 0.0285(3) Uani 1 1 d . . . . .
O2S O 0.34641(14) 0.45848(9) 0.14047(8) 0.0299(3) Uani 1 1 d . . . . .
O3S O 0.53494(15) 0.34683(9) 0.28869(10) 0.0366(4) Uani 1 1 d D U . . .
O21 O 0.08261(17) 0.89340(9) 1.04813(9) 0.0356(4) Uani 1 1 d . . . . .
H21 H 0.0679 0.9454 1.0480 0.053 Uiso 1 1 calc R U . . .
O21S O -0.14676(14) 0.62608(9) 0.68427(8) 0.0266(3) Uani 1 1 d . . . . .
O22 O -0.04109(16) 0.94651(9) 0.94459(9) 0.0336(4) Uani 1 1 d . . . . .
O22S O -0.15276(14) 0.45064(9) 0.63992(8) 0.0276(3) Uani 1 1 d . . . . .
O23S O 0.02755(14) 0.34336(8) 0.79130(8) 0.0255(3) Uani 1 1 d . . . . .
C51S C 0.4954(5) 0.2787(3) 0.2663(3) 0.0297(11) Uani 0.681(6) 1 d D U P A 1
H51A H 0.3931 0.2937 0.2608 0.036 Uiso 0.681(6) 1 calc R U P A 1
H51B H 0.5181 0.2249 0.3055 0.036 Uiso 0.681(6) 1 calc R U P A 1
C61S C 0.5787(4) 0.2685(2) 0.1902(2) 0.0402(11) Uani 0.681(6) 1 d D U P A 1
H61A H 0.5552 0.3222 0.1520 0.060 Uiso 0.681(6) 1 calc R U P A 1
H61B H 0.5550 0.2230 0.1730 0.060 Uiso 0.681(6) 1 calc R U P A 1
H61C H 0.6797 0.2537 0.1964 0.060 Uiso 0.681(6) 1 calc R U P A 1
C62S C 0.4703(7) 0.2190(5) 0.2837(4) 0.036(2) Uani 0.319(6) 1 d D U P A 2
H62A H 0.4731 0.1754 0.2554 0.055 Uiso 0.319(6) 1 calc R U P A 2
H62B H 0.3724 0.2429 0.3009 0.055 Uiso 0.319(6) 1 calc R U P A 2
H62C H 0.5248 0.1931 0.3282 0.055 Uiso 0.319(6) 1 calc R U P A 2
C52S C 0.5327(9) 0.2888(5) 0.2321(5) 0.023(2) Uani 0.319(6) 1 d D U P A 2
H52A H 0.4732 0.3208 0.1899 0.027 Uiso 0.319(6) 1 calc R U P A 2
H52B H 0.6290 0.2657 0.2101 0.027 Uiso 0.319(6) 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
C1 C2 1.392(3) . ?
C1 N1 1.401(2) . ?
C1 C6 1.402(2) . ?
C1A N1 1.471(2) . ?
C1A C2A 1.527(3) . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C1S C4S 1.401(3) . ?
C1S C11 1.427(3) . ?
C1S C2S 1.507(3) . ?
C2 C3 1.395(3) . ?
C2 H2 0.9500 . ?
C2A C3A 1.536(3) . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C2S O1S 1.218(2) . ?
C2S C3S 1.518(3) . ?
C3 C4 1.407(3) . ?
C3 H3 0.9500 . ?
C3A C4A 1.528(3) . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C3S O2S 1.221(2) . ?
C3S C4S 1.474(3) . ?
C4 C5 1.406(3) . ?
C4 C12 1.474(3) . ?
C4A C5A 1.531(3) . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
C4S O3S 1.323(2) . ?
C5 C6 1.377(3) . ?
C5 H5 0.9500 . ?
C5A C6A 1.532(3) . ?
C5A H5AA 0.9900 . ?
C5A H5AB 0.9900 . ?
C6 C7 1.519(3) . ?
C6A C7A 1.531(3) . ?
C6A H6AA 0.9900 . ?
C6A H6AB 0.9900 . ?
C7 C8 1.537(3) . ?
C7 C10 1.538(3) . ?
C7 C9 1.547(2) . ?
C7A C8A 1.528(3) . ?
C7A H7AA 0.9900 . ?
C7A H7AB 0.9900 . ?
C8 C11 1.368(3) . ?
C8 N1 1.379(2) . ?
C8A C9A 1.527(3) . ?
C8A H8AA 0.9900 . ?
C8A H8AB 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9A C10A 1.508(3) . ?
C9A H9AA 0.9900 . ?
C9A H9AB 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10A C11A 1.534(3) . ?
C10A H10D 0.9900 . ?
C10A H10E 0.9900 . ?
C11 H11 0.9500 . ?
C11A C12A 1.524(3) . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C11B N101 1.464(2) . ?
C11B C12B 1.527(2) . ?
C11B H11C 0.9900 . ?
C11B H11D 0.9900 . ?
C12 O2 1.242(2) . ?
C12 O1 1.319(2) . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
C12B C13B 1.532(3) . ?
C12B H12D 0.9900 . ?
C12B H12E 0.9900 . ?
C13B C14B 1.526(3) . ?
C13B H13A 0.9900 . ?
C13B H13B 0.9900 . ?
C14B C15B 1.526(3) . ?
C14B H14A 0.9900 . ?
C14B H14B 0.9900 . ?
C15B C16B 1.530(3) . ?
C15B H15A 0.9900 . ?
C15B H15B 0.9900 . ?
C16B C17B 1.524(3) . ?
C16B H16A 0.9900 . ?
C16B H16B 0.9900 . ?
C17B C18B 1.536(3) . ?
C17B H17A 0.9900 . ?
C17B H17B 0.9900 . ?
C18B C19B 1.525(3) . ?
C18B H18A 0.9900 . ?
C18B H18B 0.9900 . ?
C19B C20B 1.523(3) . ?
C19B H19A 0.9900 . ?
C19B H19B 0.9900 . ?
C20B C21B 1.531(3) . ?
C20B H20A 0.9900 . ?
C20B H20B 0.9900 . ?
C21B C22B 1.524(4) . ?
C21B H21A 0.9900 . ?
C21B H21B 0.9900 . ?
C21S C24S 1.401(3) . ?
C21S C111 1.421(2) . ?
C21S C22S 1.506(3) . ?
C22B H22A 0.9800 . ?
C22B H22B 0.9800 . ?
C22B H22C 0.9800 . ?
C22S O21S 1.218(2) . ?
C22S C23S 1.524(3) . ?
C23S O22S 1.220(2) . ?
C23S C24S 1.470(2) . ?
C24S O23S 1.327(2) . ?
C25S O23S 1.469(2) . ?
C25S C26S 1.493(3) . ?
C25S H25A 0.9900 . ?
C25S H25B 0.9900 . ?
C26S H26A 0.9800 . ?
C26S H26B 0.9800 . ?
C26S H26C 0.9800 . ?
C101 C102 1.390(3) . ?
C101 N101 1.399(2) . ?
C101 C106 1.401(2) . ?
C102 C103 1.389(3) . ?
C102 H102 0.9500 . ?
C103 C104 1.405(3) . ?
C103 H103 0.9500 . ?
C104 C105 1.409(3) . ?
C104 C112 1.476(3) . ?
C105 C106 1.376(3) . ?
C105 H105 0.9500 . ?
C106 C107 1.521(3) . ?
C107 C109 1.538(2) . ?
C107 C108 1.540(2) . ?
C107 C110 1.542(3) . ?
C108 C111 1.371(3) . ?
C108 N101 1.381(2) . ?
C109 H10F 0.9800 . ?
C109 H10G 0.9800 . ?
C109 H10H 0.9800 . ?
C110 H11E 0.9800 . ?
C110 H11F 0.9800 . ?
C110 H11G 0.9800 . ?
C111 H111 0.9500 . ?
C112 O22 1.253(2) . ?
C112 O21 1.312(2) . ?
O1 H1 0.8400 . ?
O3S C51S 1.454(4) . ?
O3S C52S 1.580(9) . ?
O21 H21 0.8400 . ?
C51S C61S 1.517(6) . ?
C51S H51A 0.9900 . ?
C51S H51B 0.9900 . ?
C61S H61A 0.9800 . ?
C61S H61B 0.9800 . ?
C61S H61C 0.9800 . ?
C62S C52S 1.503(10) . ?
C62S H62A 0.9800 . ?
C62S H62B 0.9800 . ?
C62S H62C 0.9800 . ?
C52S H52A 0.9900 . ?
C52S H52B 0.9900 . ?

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
C2 C1 N1 128.90(18) . . ?
C2 C1 C6 122.51(18) . . ?
N1 C1 C6 108.56(16) . . ?
N1 C1A C2A 111.89(16) . . ?
N1 C1A H1AA 109.2 . . ?
C2A C1A H1AA 109.2 . . ?
N1 C1A H1AB 109.2 . . ?
C2A C1A H1AB 109.2 . . ?
H1AA C1A H1AB 107.9 . . ?
C4S C1S C11 126.05(18) . . ?
C4S C1S C2S 89.30(16) . . ?
C11 C1S C2S 144.65(18) . . ?
C1 C2 C3 117.13(18) . . ?
C1 C2 H2 121.4 . . ?
C3 C2 H2 121.4 . . ?
C1A C2A C3A 112.05(17) . . ?
C1A C2A H2AA 109.2 . . ?
C3A C2A H2AA 109.2 . . ?
C1A C2A H2AB 109.2 . . ?
C3A C2A H2AB 109.2 . . ?
H2AA C2A H2AB 107.9 . . ?
O1S C2S C1S 137.73(18) . . ?
O1S C2S C3S 133.03(18) . . ?
C1S C2S C3S 89.24(15) . . ?
C2 C3 C4 121.45(18) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C4A C3A C2A 114.03(16) . . ?
C4A C3A H3AA 108.7 . . ?
C2A C3A H3AA 108.7 . . ?
C4A C3A H3AB 108.7 . . ?
C2A C3A H3AB 108.7 . . ?
H3AA C3A H3AB 107.6 . . ?
O2S C3S C4S 138.36(19) . . ?
O2S C3S C2S 135.44(19) . . ?
C4S C3S C2S 86.20(15) . . ?
C5 C4 C3 119.65(18) . . ?
C5 C4 C12 118.96(18) . . ?
C3 C4 C12 121.29(18) . . ?
C3A C4A C5A 112.99(16) . . ?
C3A C4A H4AA 109.0 . . ?
C5A C4A H4AA 109.0 . . ?
C3A C4A H4AB 109.0 . . ?
C5A C4A H4AB 109.0 . . ?
H4AA C4A H4AB 107.8 . . ?
O3S C4S C1S 127.32(18) . . ?
O3S C4S C3S 137.41(18) . . ?
C1S C4S C3S 95.26(16) . . ?
C6 C5 C4 119.64(18) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C4A C5A C6A 114.06(17) . . ?
C4A C5A H5AA 108.7 . . ?
C6A C5A H5AA 108.7 . . ?
C4A C5A H5AB 108.7 . . ?
C6A C5A H5AB 108.7 . . ?
H5AA C5A H5AB 107.6 . . ?
C5 C6 C1 119.57(18) . . ?
C5 C6 C7 130.67(17) . . ?
C1 C6 C7 109.66(16) . . ?
C7A C6A C5A 114.14(19) . . ?
C7A C6A H6AA 108.7 . . ?
C5A C6A H6AA 108.7 . . ?
C7A C6A H6AB 108.7 . . ?
C5A C6A H6AB 108.7 . . ?
H6AA C6A H6AB 107.6 . . ?
C6 C7 C8 101.59(15) . . ?
C6 C7 C10 111.71(16) . . ?
C8 C7 C10 109.32(15) . . ?
C6 C7 C9 109.78(15) . . ?
C8 C7 C9 112.70(16) . . ?
C10 C7 C9 111.37(15) . . ?
C8A C7A C6A 114.78(19) . . ?
C8A C7A H7AA 108.6 . . ?
C6A C7A H7AA 108.6 . . ?
C8A C7A H7AB 108.6 . . ?
C6A C7A H7AB 108.6 . . ?
H7AA C7A H7AB 107.5 . . ?
C11 C8 N1 122.08(17) . . ?
C11 C8 C7 129.88(17) . . ?
N1 C8 C7 108.01(15) . . ?
C9A C8A C7A 113.80(19) . . ?
C9A C8A H8AA 108.8 . . ?
C7A C8A H8AA 108.8 . . ?
C9A C8A H8AB 108.8 . . ?
C7A C8A H8AB 108.8 . . ?
H8AA C8A H8AB 107.7 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C10A C9A C8A 114.4(2) . . ?
C10A C9A H9AA 108.7 . . ?
C8A C9A H9AA 108.7 . . ?
C10A C9A H9AB 108.7 . . ?
C8A C9A H9AB 108.7 . . ?
H9AA C9A H9AB 107.6 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9A C10A C11A 114.6(2) . . ?
C9A C10A H10D 108.6 . . ?
C11A C10A H10D 108.6 . . ?
C9A C10A H10E 108.6 . . ?
C11A C10A H10E 108.6 . . ?
H10D C10A H10E 107.6 . . ?
C8 C11 C1S 131.46(18) . . ?
C8 C11 H11 114.3 . . ?
C1S C11 H11 114.3 . . ?
C12A C11A C10A 112.80(19) . . ?
C12A C11A H11A 109.0 . . ?
C10A C11A H11A 109.0 . . ?
C12A C11A H11B 109.0 . . ?
C10A C11A H11B 109.0 . . ?
H11A C11A H11B 107.8 . . ?
N101 C11B C12B 111.37(16) . . ?
N101 C11B H11C 109.4 . . ?
C12B C11B H11C 109.4 . . ?
N101 C11B H11D 109.4 . . ?
C12B C11B H11D 109.4 . . ?
H11C C11B H11D 108.0 . . ?
O2 C12 O1 122.45(18) . . ?
O2 C12 C4 121.57(19) . . ?
O1 C12 C4 115.96(17) . . ?
C11A C12A H12A 109.5 . . ?
C11A C12A H12B 109.5 . . ?
H12A C12A H12B 109.5 . . ?
C11A C12A H12C 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
C11B C12B C13B 112.16(17) . . ?
C11B C12B H12D 109.2 . . ?
C13B C12B H12D 109.2 . . ?
C11B C12B H12E 109.2 . . ?
C13B C12B H12E 109.2 . . ?
H12D C12B H12E 107.9 . . ?
C14B C13B C12B 113.77(16) . . ?
C14B C13B H13A 108.8 . . ?
C12B C13B H13A 108.8 . . ?
C14B C13B H13B 108.8 . . ?
C12B C13B H13B 108.8 . . ?
H13A C13B H13B 107.7 . . ?
C13B C14B C15B 112.60(17) . . ?
C13B C14B H14A 109.1 . . ?
C15B C14B H14A 109.1 . . ?
C13B C14B H14B 109.1 . . ?
C15B C14B H14B 109.1 . . ?
H14A C14B H14B 107.8 . . ?
C14B C15B C16B 113.87(18) . . ?
C14B C15B H15A 108.8 . . ?
C16B C15B H15A 108.8 . . ?
C14B C15B H15B 108.8 . . ?
C16B C15B H15B 108.8 . . ?
H15A C15B H15B 107.7 . . ?
C17B C16B C15B 115.2(2) . . ?
C17B C16B H16A 108.5 . . ?
C15B C16B H16A 108.5 . . ?
C17B C16B H16B 108.5 . . ?
C15B C16B H16B 108.5 . . ?
H16A C16B H16B 107.5 . . ?
C16B C17B C18B 114.40(19) . . ?
C16B C17B H17A 108.7 . . ?
C18B C17B H17A 108.7 . . ?
C16B C17B H17B 108.7 . . ?
C18B C17B H17B 108.7 . . ?
H17A C17B H17B 107.6 . . ?
C19B C18B C17B 113.17(18) . . ?
C19B C18B H18A 108.9 . . ?
C17B C18B H18A 108.9 . . ?
C19B C18B H18B 108.9 . . ?
C17B C18B H18B 108.9 . . ?
H18A C18B H18B 107.8 . . ?
C20B C19B C18B 114.01(19) . . ?
C20B C19B H19A 108.7 . . ?
C18B C19B H19A 108.7 . . ?
C20B C19B H19B 108.7 . . ?
C18B C19B H19B 108.7 . . ?
H19A C19B H19B 107.6 . . ?
C19B C20B C21B 114.0(2) . . ?
C19B C20B H20A 108.7 . . ?
C21B C20B H20A 108.7 . . ?
C19B C20B H20B 108.7 . . ?
C21B C20B H20B 108.7 . . ?
H20A C20B H20B 107.6 . . ?
C22B C21B C20B 114.0(2) . . ?
C22B C21B H21A 108.8 . . ?
C20B C21B H21A 108.8 . . ?
C22B C21B H21B 108.8 . . ?
C20B C21B H21B 108.8 . . ?
H21A C21B H21B 107.7 . . ?
C24S C21S C111 126.56(18) . . ?
C24S C21S C22S 89.43(15) . . ?
C111 C21S C22S 144.00(18) . . ?
C21B C22B H22A 109.5 . . ?
C21B C22B H22B 109.5 . . ?
H22A C22B H22B 109.5 . . ?
C21B C22B H22C 109.5 . . ?
H22A C22B H22C 109.5 . . ?
H22B C22B H22C 109.5 . . ?
O21S C22S C21S 137.49(18) . . ?
O21S C22S C23S 133.51(18) . . ?
C21S C22S C23S 88.99(15) . . ?
O22S C23S C24S 138.14(19) . . ?
O22S C23S C22S 135.68(18) . . ?
C24S C23S C22S 86.18(15) . . ?
O23S C24S C21S 127.78(18) . . ?
O23S C24S C23S 136.84(17) . . ?
C21S C24S C23S 95.38(16) . . ?
O23S C25S C26S 112.33(19) . . ?
O23S C25S H25A 109.1 . . ?
C26S C25S H25A 109.1 . . ?
O23S C25S H25B 109.1 . . ?
C26S C25S H25B 109.1 . . ?
H25A C25S H25B 107.9 . . ?
C25S C26S H26A 109.5 . . ?
C25S C26S H26B 109.5 . . ?
H26A C26S H26B 109.5 . . ?
C25S C26S H26C 109.5 . . ?
H26A C26S H26C 109.5 . . ?
H26B C26S H26C 109.5 . . ?
C102 C101 N101 128.41(17) . . ?
C102 C101 C106 122.85(18) . . ?
N101 C101 C106 108.73(16) . . ?
C103 C102 C101 117.24(18) . . ?
C103 C102 H102 121.4 . . ?
C101 C102 H102 121.4 . . ?
C102 C103 C104 121.07(18) . . ?
C102 C103 H103 119.5 . . ?
C104 C103 H103 119.5 . . ?
C103 C104 C105 120.25(18) . . ?
C103 C104 C112 120.29(18) . . ?
C105 C104 C112 119.46(18) . . ?
C106 C105 C104 119.10(18) . . ?
C106 C105 H105 120.5 . . ?
C104 C105 H105 120.5 . . ?
C105 C106 C101 119.46(18) . . ?
C105 C106 C107 130.96(17) . . ?
C101 C106 C107 109.56(16) . . ?
C106 C107 C109 110.17(15) . . ?
C106 C107 C108 101.62(14) . . ?
C109 C107 C108 112.68(16) . . ?
C106 C107 C110 111.65(16) . . ?
C109 C107 C110 110.48(15) . . ?
C108 C107 C110 109.97(15) . . ?
C111 C108 N101 121.51(17) . . ?
C111 C108 C107 130.69(17) . . ?
N101 C108 C107 107.79(15) . . ?
C107 C109 H10F 109.5 . . ?
C107 C109 H10G 109.5 . . ?
H10F C109 H10G 109.5 . . ?
C107 C109 H10H 109.5 . . ?
H10F C109 H10H 109.5 . . ?
H10G C109 H10H 109.5 . . ?
C107 C110 H11E 109.5 . . ?
C107 C110 H11F 109.5 . . ?
H11E C110 H11F 109.5 . . ?
C107 C110 H11G 109.5 . . ?
H11E C110 H11G 109.5 . . ?
H11F C110 H11G 109.5 . . ?
C108 C111 C21S 132.09(18) . . ?
C108 C111 H111 114.0 . . ?
C21S C111 H111 114.0 . . ?
O22 C112 O21 122.97(18) . . ?
O22 C112 C104 121.14(19) . . ?
O21 C112 C104 115.88(17) . . ?
C8 N1 C1 112.14(15) . . ?
C8 N1 C1A 124.41(15) . . ?
C1 N1 C1A 123.41(15) . . ?
C108 N101 C101 112.26(15) . . ?
C108 N101 C11B 125.38(15) . . ?
C101 N101 C11B 122.26(15) . . ?
C12 O1 H1 109.5 . . ?
C4S O3S C51S 119.6(2) . . ?
C4S O3S C52S 108.9(3) . . ?
C112 O21 H21 109.5 . . ?
C24S O23S C25S 116.44(15) . . ?
O3S C51S C61S 106.9(3) . . ?
O3S C51S H51A 110.3 . . ?
C61S C51S H51A 110.3 . . ?
O3S C51S H51B 110.3 . . ?
C61S C51S H51B 110.3 . . ?
H51A C51S H51B 108.6 . . ?
C51S C61S H61A 109.5 . . ?
C51S C61S H61B 109.5 . . ?
H61A C61S H61B 109.5 . . ?
C51S C61S H61C 109.5 . . ?
H61A C61S H61C 109.5 . . ?
H61B C61S H61C 109.5 . . ?
C52S C62S H62A 109.5 . . ?
C52S C62S H62B 109.5 . . ?
H62A C62S H62B 109.5 . . ?
C52S C62S H62C 109.5 . . ?
H62A C62S H62C 109.5 . . ?
H62B C62S H62C 109.5 . . ?
C62S C52S O3S 102.5(6) . . ?
C62S C52S H52A 111.3 . . ?
O3S C52S H52A 111.3 . . ?
C62S C52S H52B 111.3 . . ?
O3S C52S H52B 111.3 . . ?
H52A C52S H52B 109.2 . . ?

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
C1A H1AB O22S 0.99 2.42 3.314(2) 149.8 1_655
C2 H2 O22S 0.95 2.61 3.545(2) 168.3 1_655
C11B H11D O2S 0.99 2.54 3.413(2) 146.9 1_556
C25S H25A O1S 0.99 2.58 3.424(3) 143.3 2_566
C26S H26A O22S 0.98 2.63 3.338(3) 129.3 .
C102 H102 O2S 0.95 2.61 3.551(3) 172.6 1_556
O1 H1 O2 0.84 1.82 2.661(2) 174.7 2_676
O21 H21 O22 0.84 1.79 2.623(2) 175.3 2_577
C51S H51A O21S 0.99 2.63 3.475(5) 143.5 2_566
C61S H61A O2S 0.98 2.62 3.385(4) 134.8 .
C52S H52A O2S 0.99 2.33 3.155(8) 140.4 .

_refine_diff_density_max         0.446
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.071

_shelxl_version_number           2013-3


####################################################################### 
# 
# 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_8polymorph1
_database_code_depnum_ccdc_archive 'CCDC 1030513'
_audit_update_record             
;
2014-10-22 deposited with the CCDC.
2014-12-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H36 N3 O4, C6 H16 N'
_chemical_formula_sum            'C37 H52 N4 O4'
_chemical_formula_weight         616.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'

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

_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                   11.3712(6)
_cell_length_b                   12.1738(6)
_cell_length_c                   14.8030(10)
_cell_angle_alpha                105.290(7)
_cell_angle_beta                 92.938(7)
_cell_angle_gamma                113.173(8)
_cell_volume                     1789.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    23518
_cell_measurement_theta_min      3.2
_cell_measurement_theta_max      27.7

_exptl_crystal_description       fagment
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_F_000             668
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.074
_shelx_estimated_absorpt_T_min   0.989
_shelx_estimated_absorpt_T_max   0.998
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_process_details   'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           'Mo K\a'
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Mitegen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_reflns_number            31053
_diffrn_reflns_av_unetI/netI     0.0867
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.188
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8194
_reflns_number_gt                5922
_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       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'
_computing_cell_refinement       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'
_computing_data_reduction        'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'
_computing_structure_solution    
'SUPERFLIP (Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  
'WinGX, ver.2013.3 (L.J. Farrugia, J.App.Cryst.(2012),45,849-854)'

_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)+(0.0989P)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         8194
_refine_ls_number_parameters     417
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0617
_refine_ls_wR_factor_ref         0.1733
_refine_ls_wR_factor_gt          0.1573
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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
C1 C 0.26012(14) 0.32689(14) 0.90159(11) 0.0225(3) Uani 1 1 d . . . . .
C1A C 0.10999(15) 0.33247(14) 0.77457(12) 0.0250(3) Uani 1 1 d . . . . .
H1A1 H 0.0990 0.3064 0.7043 0.030 Uiso 1 1 calc R U . . .
H1A2 H 0.1599 0.4249 0.7984 0.030 Uiso 1 1 calc R U . . .
C1S C 0.07879(15) -0.04002(14) 0.62597(11) 0.0240(3) Uani 1 1 d . . . . .
C2 C 0.27669(14) 0.43543(14) 0.97063(12) 0.0252(4) Uani 1 1 d . . . . .
H2 H 0.2354 0.4864 0.9600 0.030 Uiso 1 1 calc R U . . .
C2A C -0.02312(15) 0.29818(15) 0.80330(12) 0.0280(4) Uani 1 1 d . . . . .
H2A1 H -0.0129 0.3215 0.8735 0.034 Uiso 1 1 calc R U . . .
H2A2 H -0.0749 0.2062 0.7772 0.034 Uiso 1 1 calc R U . . .
C2S C 0.15286(15) -0.11417(14) 0.59969(12) 0.0262(4) Uani 1 1 d . . . . .
C3 C 0.35649(15) 0.46721(14) 1.05656(11) 0.0259(4) Uani 1 1 d . . . . .
H3 H 0.3701 0.5415 1.1058 0.031 Uiso 1 1 calc R U . . .
C3A C -0.09545(15) 0.36442(15) 0.76750(13) 0.0290(4) Uani 1 1 d . . . . .
H3A1 H -0.1888 0.3206 0.7698 0.035 Uiso 1 1 calc R U . . .
H3A2 H -0.0873 0.3569 0.7001 0.035 Uiso 1 1 calc R U . . .
C3S C 0.03739(16) -0.21328(14) 0.52758(12) 0.0273(4) Uani 1 1 d . . . . .
C4 C 0.41665(14) 0.39228(14) 1.07171(11) 0.0255(4) Uani 1 1 d . . . . .
C4A C -0.04790(16) 0.50352(15) 0.82339(13) 0.0294(4) Uani 1 1 d . . . . .
H4A1 H -0.0621 0.5112 0.8898 0.035 Uiso 1 1 calc R U . . .
H4A2 H 0.0467 0.5468 0.8249 0.035 Uiso 1 1 calc R U . . .
C4S C -0.03176(15) -0.13278(14) 0.55660(11) 0.0253(4) Uani 1 1 d . . . . .
C5 C 0.39852(14) 0.28316(14) 0.99973(11) 0.0254(4) Uani 1 1 d . . . . .
H5 H 0.4399 0.2320 1.0097 0.030 Uiso 1 1 calc R U . . .
C5A C -0.11610(16) 0.56856(15) 0.78143(13) 0.0306(4) Uani 1 1 d . . . . .
H5A1 H -0.2112 0.5196 0.7732 0.037 Uiso 1 1 calc R U . . .
H5A2 H -0.0940 0.5689 0.7177 0.037 Uiso 1 1 calc R U . . .
C5S C -0.15539(15) -0.14652(14) 0.52683(12) 0.0266(4) Uani 1 1 d . . . . .
C6 C 0.32032(14) 0.25099(14) 0.91466(11) 0.0226(3) Uani 1 1 d . . . . .
C6A C -0.08032(17) 0.70308(15) 0.84215(14) 0.0327(4) Uani 1 1 d . . . . .
H6A1 H -0.0954 0.7035 0.9075 0.039 Uiso 1 1 calc R U . . .
H6A2 H 0.0135 0.7538 0.8458 0.039 Uiso 1 1 calc R U . . .
C6S C -0.20200(15) -0.05483(15) 0.56580(12) 0.0286(4) Uani 1 1 d . . . . .
C7 C 0.28600(14) 0.14289(13) 0.82404(11) 0.0232(3) Uani 1 1 d . . . . .
C7A C -0.15698(17) 0.76441(16) 0.80434(13) 0.0332(4) Uani 1 1 d . . . . .
H7A1 H -0.1279 0.7804 0.7453 0.040 Uiso 1 1 calc R U . . .
H7A2 H -0.2501 0.7053 0.7878 0.040 Uiso 1 1 calc R U . . .
C7S C -0.24172(15) -0.25490(15) 0.45270(12) 0.0273(4) Uani 1 1 d . . . . .
C9 C 0.23826(16) 0.01635(14) 0.84279(12) 0.0276(4) Uani 1 1 d . . . . .
H9B H 0.3080 0.0143 0.8830 0.041 Uiso 1 1 calc R U . . .
H9C H 0.2129 -0.0511 0.7822 0.041 Uiso 1 1 calc R U . . .
H9A H 0.1632 0.0047 0.8752 0.041 Uiso 1 1 calc R U . . .
C8A C -0.14214(16) 0.88720(15) 0.87437(14) 0.0328(4) Uani 1 1 d . . . . .
H8A1 H -0.1578 0.8738 0.9366 0.039 Uiso 1 1 calc R U . . .
H8A2 H -0.0514 0.9501 0.8832 0.039 Uiso 1 1 calc R U . . .
C10 C 0.40619(15) 0.16646(14) 0.77507(12) 0.0266(4) Uani 1 1 d . . . . .
H10A H 0.4362 0.2492 0.7655 0.040 Uiso 1 1 calc R U . . .
H10C H 0.3831 0.1014 0.7134 0.040 Uiso 1 1 calc R U . . .
H10B H 0.4756 0.1638 0.8152 0.040 Uiso 1 1 calc R U . . .
C9A C -0.23259(17) 0.94056(16) 0.84475(14) 0.0332(4) Uani 1 1 d . . . . .
H9A1 H -0.3236 0.8783 0.8360 0.040 Uiso 1 1 calc R U . . .
H9A2 H -0.2168 0.9551 0.7829 0.040 Uiso 1 1 calc R U . . .
C8 C 0.18216(14) 0.15889(13) 0.76590(11) 0.0221(3) Uani 1 1 d . . . . .
C10A C -0.21400(17) 1.06326(15) 0.91753(13) 0.0314(4) Uani 1 1 d . . . . .
H10E H -0.2257 1.0489 0.9799 0.038 Uiso 1 1 calc R U . . .
H10D H -0.1236 1.1258 0.9243 0.038 Uiso 1 1 calc R U . . .
C11 C 0.09411(15) 0.07874(14) 0.68554(11) 0.0246(3) Uani 1 1 d . . . . .
H11 H 0.0331 0.1072 0.6664 0.029 Uiso 1 1 calc R U . . .
C11A C -0.30589(17) 1.11784(16) 0.89304(14) 0.0348(4) Uani 1 1 d . . . . .
H11A H -0.3965 1.0570 0.8886 0.042 Uiso 1 1 calc R U . . .
H11B H -0.2961 1.1307 0.8300 0.042 Uiso 1 1 calc R U . . .
C12 C 0.50328(15) 0.42687(15) 1.16227(12) 0.0279(4) Uani 1 1 d . . . . .
C12A C -0.28079(19) 1.24215(17) 0.96637(16) 0.0421(5) Uani 1 1 d . . . . .
H12A H -0.2944 1.2292 1.0283 0.063 Uiso 1 1 calc R U . . .
H12B H -0.3407 1.2748 0.9467 0.063 Uiso 1 1 calc R U . . .
H12C H -0.1911 1.3026 0.9714 0.063 Uiso 1 1 calc R U . . .
C14 C 0.22396(16) 0.58532(15) 0.56414(13) 0.0330(4) Uani 1 1 d . . . . .
H14A H 0.1457 0.5579 0.5163 0.040 Uiso 1 1 calc R U . . .
H14B H 0.2545 0.5179 0.5503 0.040 Uiso 1 1 calc R U . . .
C17 C 0.52102(17) 0.66405(18) 0.60392(15) 0.0386(4) Uani 1 1 d . . . . .
H17A H 0.4646 0.5836 0.6120 0.058 Uiso 1 1 calc R U . . .
H17B H 0.6028 0.7021 0.6491 0.058 Uiso 1 1 calc R U . . .
H17C H 0.5391 0.6500 0.5389 0.058 Uiso 1 1 calc R U . . .
C15 C 0.18766(18) 0.60284(17) 0.66124(14) 0.0386(4) Uani 1 1 d . . . . .
H15A H 0.2594 0.6134 0.7073 0.058 Uiso 1 1 calc R U . . .
H15B H 0.1097 0.5289 0.6604 0.058 Uiso 1 1 calc R U . . .
H15C H 0.1702 0.6776 0.6795 0.058 Uiso 1 1 calc R U . . .
C16 C 0.45412(16) 0.75099(16) 0.62209(13) 0.0325(4) Uani 1 1 d . . . . .
H16A H 0.5137 0.8333 0.6170 0.039 Uiso 1 1 calc R U . . .
H16B H 0.4365 0.7647 0.6880 0.039 Uiso 1 1 calc R U . . .
C18 C 0.34336(18) 0.68664(17) 0.45289(13) 0.0360(4) Uani 1 1 d . . . . .
H18A H 0.2565 0.6522 0.4132 0.043 Uiso 1 1 calc R U . . .
H18B H 0.3805 0.6247 0.4325 0.043 Uiso 1 1 calc R U . . .
C19 C 0.42900(19) 0.80677(19) 0.43568(15) 0.0441(5) Uani 1 1 d . . . . .
H19A H 0.3986 0.8715 0.4622 0.066 Uiso 1 1 calc R U . . .
H19B H 0.4257 0.7928 0.3671 0.066 Uiso 1 1 calc R U . . .
H19C H 0.5186 0.8344 0.4665 0.066 Uiso 1 1 calc R U . . .
N1 N 0.18424(12) 0.27430(11) 0.81069(9) 0.0235(3) Uani 1 1 d . . . . .
N1S N -0.23996(15) 0.01893(14) 0.59785(12) 0.0394(4) Uani 1 1 d . . . . .
N2 N 0.32808(13) 0.70278(12) 0.55469(10) 0.0271(3) Uani 1 1 d . . . . .
N2S N -0.31410(13) -0.34307(13) 0.39365(11) 0.0329(3) Uani 1 1 d . . . . .
O1S O 0.26321(11) -0.10390(10) 0.62362(9) 0.0316(3) Uani 1 1 d . . . . .
O2 O 0.50576(12) 0.52851(10) 1.22705(8) 0.0335(3) Uani 1 1 d . . . . .
H2A H 0.5643 0.5517 1.2739 0.050 Uiso 1 1 calc R U . . .
O2S O 0.01341(12) -0.31453(10) 0.46955(9) 0.0347(3) Uani 1 1 d . . . . .
O1 O 0.56608(12) 0.37160(11) 1.17717(9) 0.0375(3) Uani 1 1 d . . . . .
H2N H 0.3006(18) 0.7689(16) 0.5752(13) 0.029(5) 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
C1 C2 1.378(2) . ?
C1 C6 1.392(2) . ?
C1 N1 1.3989(19) . ?
C1A N1 1.457(2) . ?
C1A C2A 1.519(2) . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
C1S C11 1.418(2) . ?
C1S C4S 1.431(2) . ?
C1S C2S 1.457(2) . ?
C2 C3 1.392(2) . ?
C2 H2 0.9500 . ?
C2A C3A 1.520(2) . ?
C2A H2A1 0.9900 . ?
C2A H2A2 0.9900 . ?
C2S O1S 1.2342(19) . ?
C2S C3S 1.500(2) . ?
C3 C4 1.391(2) . ?
C3 H3 0.9500 . ?
C3A C4A 1.529(2) . ?
C3A H3A1 0.9900 . ?
C3A H3A2 0.9900 . ?
C3S O2S 1.2184(19) . ?
C3S C4S 1.477(2) . ?
C4 C5 1.399(2) . ?
C4 C12 1.478(2) . ?
C4A C5A 1.519(2) . ?
C4A H4A1 0.9900 . ?
C4A H4A2 0.9900 . ?
C4S C5S 1.382(2) . ?
C5 C6 1.371(2) . ?
C5 H5 0.9500 . ?
C5A C6A 1.522(2) . ?
C5A H5A1 0.9900 . ?
C5A H5A2 0.9900 . ?
C5S C7S 1.420(2) . ?
C5S C6S 1.420(2) . ?
C6 C7 1.515(2) . ?
C6A C7A 1.521(2) . ?
C6A H6A1 0.9900 . ?
C6A H6A2 0.9900 . ?
C6S N1S 1.149(2) . ?
C7 C9 1.526(2) . ?
C7 C8 1.529(2) . ?
C7 C10 1.542(2) . ?
C7A C8A 1.518(2) . ?
C7A H7A1 0.9900 . ?
C7A H7A2 0.9900 . ?
C7S N2S 1.153(2) . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 H9A 0.9800 . ?
C8A C9A 1.517(2) . ?
C8A H8A1 0.9900 . ?
C8A H8A2 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10C 0.9800 . ?
C10 H10B 0.9800 . ?
C9A C10A 1.522(2) . ?
C9A H9A1 0.9900 . ?
C9A H9A2 0.9900 . ?
C8 C11 1.366(2) . ?
C8 N1 1.3766(19) . ?
C10A C11A 1.516(2) . ?
C10A H10E 0.9900 . ?
C10A H10D 0.9900 . ?
C11 H11 0.9500 . ?
C11A C12A 1.520(2) . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C12 O1 1.205(2) . ?
C12 O2 1.3399(19) . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
C14 C15 1.500(3) . ?
C14 N2 1.502(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C17 C16 1.509(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 N2 1.509(2) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C18 N2 1.496(2) . ?
C18 C19 1.501(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
N2 H2N 0.958(18) . ?
O2 H2A 0.8400 . ?

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
C2 C1 C6 122.76(14) . . ?
C2 C1 N1 128.06(15) . . ?
C6 C1 N1 109.19(13) . . ?
N1 C1A C2A 113.32(13) . . ?
N1 C1A H1A1 108.9 . . ?
C2A C1A H1A1 108.9 . . ?
N1 C1A H1A2 108.9 . . ?
C2A C1A H1A2 108.9 . . ?
H1A1 C1A H1A2 107.7 . . ?
C11 C1S C4S 127.80(15) . . ?
C11 C1S C2S 140.53(14) . . ?
C4S C1S C2S 91.46(13) . . ?
C1 C2 C3 117.13(15) . . ?
C1 C2 H2 121.4 . . ?
C3 C2 H2 121.4 . . ?
C1A C2A C3A 111.76(14) . . ?
C1A C2A H2A1 109.3 . . ?
C3A C2A H2A1 109.3 . . ?
C1A C2A H2A2 109.3 . . ?
C3A C2A H2A2 109.3 . . ?
H2A1 C2A H2A2 107.9 . . ?
O1S C2S C1S 137.11(14) . . ?
O1S C2S C3S 133.57(15) . . ?
C1S C2S C3S 89.32(12) . . ?
C4 C3 C2 121.21(15) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C2A C3A C4A 114.64(13) . . ?
C2A C3A H3A1 108.6 . . ?
C4A C3A H3A1 108.6 . . ?
C2A C3A H3A2 108.6 . . ?
C4A C3A H3A2 108.6 . . ?
H3A1 C3A H3A2 107.6 . . ?
O2S C3S C4S 136.51(15) . . ?
O2S C3S C2S 135.48(16) . . ?
C4S C3S C2S 88.00(12) . . ?
C3 C4 C5 120.15(15) . . ?
C3 C4 C12 121.36(15) . . ?
C5 C4 C12 118.47(15) . . ?
C5A C4A C3A 113.07(14) . . ?
C5A C4A H4A1 109.0 . . ?
C3A C4A H4A1 109.0 . . ?
C5A C4A H4A2 109.0 . . ?
C3A C4A H4A2 109.0 . . ?
H4A1 C4A H4A2 107.8 . . ?
C5S C4S C1S 135.95(15) . . ?
C5S C4S C3S 132.84(14) . . ?
C1S C4S C3S 91.20(13) . . ?
C6 C5 C4 119.19(15) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C4A C5A C6A 113.58(14) . . ?
C4A C5A H5A1 108.9 . . ?
C6A C5A H5A1 108.9 . . ?
C4A C5A H5A2 108.9 . . ?
C6A C5A H5A2 108.9 . . ?
H5A1 C5A H5A2 107.7 . . ?
C4S C5S C7S 120.19(15) . . ?
C4S C5S C6S 123.08(14) . . ?
C7S C5S C6S 116.72(14) . . ?
C5 C6 C1 119.56(14) . . ?
C5 C6 C7 131.23(14) . . ?
C1 C6 C7 109.19(13) . . ?
C7A C6A C5A 113.51(15) . . ?
C7A C6A H6A1 108.9 . . ?
C5A C6A H6A1 108.9 . . ?
C7A C6A H6A2 108.9 . . ?
C5A C6A H6A2 108.9 . . ?
H6A1 C6A H6A2 107.7 . . ?
N1S C6S C5S 179.5(2) . . ?
C6 C7 C9 112.08(13) . . ?
C6 C7 C8 101.18(12) . . ?
C9 C7 C8 113.84(12) . . ?
C6 C7 C10 108.54(12) . . ?
C9 C7 C10 111.19(13) . . ?
C8 C7 C10 109.49(13) . . ?
C8A C7A C6A 113.48(15) . . ?
C8A C7A H7A1 108.9 . . ?
C6A C7A H7A1 108.9 . . ?
C8A C7A H7A2 108.9 . . ?
C6A C7A H7A2 108.9 . . ?
H7A1 C7A H7A2 107.7 . . ?
N2S C7S C5S 178.44(19) . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
H9B C9 H9A 109.5 . . ?
H9C C9 H9A 109.5 . . ?
C9A C8A C7A 114.60(15) . . ?
C9A C8A H8A1 108.6 . . ?
C7A C8A H8A1 108.6 . . ?
C9A C8A H8A2 108.6 . . ?
C7A C8A H8A2 108.6 . . ?
H8A1 C8A H8A2 107.6 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10C C10 H10B 109.5 . . ?
C8A C9A C10A 112.42(15) . . ?
C8A C9A H9A1 109.1 . . ?
C10A C9A H9A1 109.1 . . ?
C8A C9A H9A2 109.1 . . ?
C10A C9A H9A2 109.1 . . ?
H9A1 C9A H9A2 107.9 . . ?
C11 C8 N1 121.18(14) . . ?
C11 C8 C7 130.73(14) . . ?
N1 C8 C7 108.05(12) . . ?
C11A C10A C9A 114.47(15) . . ?
C11A C10A H10E 108.6 . . ?
C9A C10A H10E 108.6 . . ?
C11A C10A H10D 108.6 . . ?
C9A C10A H10D 108.6 . . ?
H10E C10A H10D 107.6 . . ?
C8 C11 C1S 130.60(15) . . ?
C8 C11 H11 114.7 . . ?
C1S C11 H11 114.7 . . ?
C10A C11A C12A 112.42(15) . . ?
C10A C11A H11A 109.1 . . ?
C12A C11A H11A 109.1 . . ?
C10A C11A H11B 109.1 . . ?
C12A C11A H11B 109.1 . . ?
H11A C11A H11B 107.9 . . ?
O1 C12 O2 122.96(15) . . ?
O1 C12 C4 124.60(16) . . ?
O2 C12 C4 112.43(15) . . ?
C11A C12A H12A 109.5 . . ?
C11A C12A H12B 109.5 . . ?
H12A C12A H12B 109.5 . . ?
C11A C12A H12C 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
C15 C14 N2 112.88(14) . . ?
C15 C14 H14A 109.0 . . ?
N2 C14 H14A 109.0 . . ?
C15 C14 H14B 109.0 . . ?
N2 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N2 113.92(14) . . ?
C17 C16 H16A 108.8 . . ?
N2 C16 H16A 108.8 . . ?
C17 C16 H16B 108.8 . . ?
N2 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
N2 C18 C19 113.25(15) . . ?
N2 C18 H18A 108.9 . . ?
C19 C18 H18A 108.9 . . ?
N2 C18 H18B 108.9 . . ?
C19 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C8 N1 C1 110.92(13) . . ?
C8 N1 C1A 126.18(13) . . ?
C1 N1 C1A 122.70(13) . . ?
C18 N2 C14 110.39(13) . . ?
C18 N2 C16 113.85(13) . . ?
C14 N2 C16 113.72(13) . . ?
C18 N2 H2N 107.9(11) . . ?
C14 N2 H2N 107.5(11) . . ?
C16 N2 H2N 102.8(11) . . ?
C12 O2 H2A 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
C6 C1 C2 C3 -0.7(2) . . . . ?
N1 C1 C2 C3 179.09(15) . . . . ?
N1 C1A C2A C3A 177.85(13) . . . . ?
C11 C1S C2S O1S 4.2(4) . . . . ?
C4S C1S C2S O1S 178.8(2) . . . . ?
C11 C1S C2S C3S -175.3(2) . . . . ?
C4S C1S C2S C3S -0.76(13) . . . . ?
C1 C2 C3 C4 0.0(2) . . . . ?
C1A C2A C3A C4A -75.78(19) . . . . ?
O1S C2S C3S O2S -0.1(4) . . . . ?
C1S C2S C3S O2S 179.5(2) . . . . ?
O1S C2S C3S C4S -178.8(2) . . . . ?
C1S C2S C3S C4S 0.74(12) . . . . ?
C2 C3 C4 C5 0.5(2) . . . . ?
C2 C3 C4 C12 178.93(15) . . . . ?
C2A C3A C4A C5A 176.02(15) . . . . ?
C11 C1S C4S C5S -4.2(3) . . . . ?
C2S C1S C4S C5S -179.8(2) . . . . ?
C11 C1S C4S C3S 176.41(16) . . . . ?
C2S C1S C4S C3S 0.77(13) . . . . ?
O2S C3S C4S C5S 1.1(4) . . . . ?
C2S C3S C4S C5S 179.8(2) . . . . ?
O2S C3S C4S C1S -179.5(2) . . . . ?
C2S C3S C4S C1S -0.75(13) . . . . ?
C3 C4 C5 C6 -0.4(2) . . . . ?
C12 C4 C5 C6 -178.82(14) . . . . ?
C3A C4A C5A C6A 173.77(15) . . . . ?
C1S C4S C5S C7S 179.49(18) . . . . ?
C3S C4S C5S C7S -1.3(3) . . . . ?
C1S C4S C5S C6S 0.8(3) . . . . ?
C3S C4S C5S C6S 179.98(17) . . . . ?
C4 C5 C6 C1 -0.3(2) . . . . ?
C4 C5 C6 C7 177.87(15) . . . . ?
C2 C1 C6 C5 0.8(2) . . . . ?
N1 C1 C6 C5 -178.98(14) . . . . ?
C2 C1 C6 C7 -177.70(14) . . . . ?
N1 C1 C6 C7 2.50(17) . . . . ?
C4A C5A C6A C7A -175.18(15) . . . . ?
C5 C6 C7 C9 51.4(2) . . . . ?
C1 C6 C7 C9 -130.31(14) . . . . ?
C5 C6 C7 C8 173.06(16) . . . . ?
C1 C6 C7 C8 -8.65(16) . . . . ?
C5 C6 C7 C10 -71.8(2) . . . . ?
C1 C6 C7 C10 106.50(14) . . . . ?
C5A C6A C7A C8A 168.14(15) . . . . ?
C6A C7A C8A C9A -171.33(15) . . . . ?
C7A C8A C9A C10A 179.80(15) . . . . ?
C6 C7 C8 C11 -165.51(16) . . . . ?
C9 C7 C8 C11 -45.1(2) . . . . ?
C10 C7 C8 C11 80.0(2) . . . . ?
C6 C7 C8 N1 11.96(15) . . . . ?
C9 C7 C8 N1 132.37(14) . . . . ?
C10 C7 C8 N1 -102.48(14) . . . . ?
C8A C9A C10A C11A -177.72(15) . . . . ?
N1 C8 C11 C1S 176.46(16) . . . . ?
C7 C8 C11 C1S -6.3(3) . . . . ?
C4S C1S C11 C8 163.81(17) . . . . ?
C2S C1S C11 C8 -23.1(3) . . . . ?
C9A C10A C11A C12A -178.31(15) . . . . ?
C3 C4 C12 O1 -173.94(16) . . . . ?
C5 C4 C12 O1 4.5(3) . . . . ?
C3 C4 C12 O2 5.5(2) . . . . ?
C5 C4 C12 O2 -176.06(14) . . . . ?
C11 C8 N1 C1 166.29(15) . . . . ?
C7 C8 N1 C1 -11.47(17) . . . . ?
C11 C8 N1 C1A -8.6(2) . . . . ?
C7 C8 N1 C1A 173.62(14) . . . . ?
C2 C1 N1 C8 -174.01(15) . . . . ?
C6 C1 N1 C8 5.78(18) . . . . ?
C2 C1 N1 C1A 1.1(2) . . . . ?
C6 C1 N1 C1A -179.10(13) . . . . ?
C2A C1A N1 C8 89.19(18) . . . . ?
C2A C1A N1 C1 -85.16(17) . . . . ?
C19 C18 N2 C14 170.11(15) . . . . ?
C19 C18 N2 C16 -60.6(2) . . . . ?
C15 C14 N2 C18 -169.90(14) . . . . ?
C15 C14 N2 C16 60.71(19) . . . . ?
C17 C16 N2 C18 -62.42(19) . . . . ?
C17 C16 N2 C14 65.20(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
O2 H2A N2S 0.84 1.96 2.7660(18) 159.8 1_666
N2 H2N O1S 0.958(18) 1.748(18) 2.7021(18) 173.8(17) 1_565

_refine_diff_density_max         0.350
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.062

_shelxl_version_number           2013-4


####################################################################### 
# 
# 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_8polymorph2
_database_code_depnum_ccdc_archive 'CCDC 1030514'
_audit_update_record             
;
2014-10-22 deposited with the CCDC.
2014-12-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H36 N3 O4, C6 H16 N'
_chemical_formula_sum            'C37 H52 N4 O4'
_chemical_formula_weight         616.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'

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

_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                   8.358(3)
_cell_length_b                   10.369(4)
_cell_length_c                   22.108(8)
_cell_angle_alpha                98.940(6)
_cell_angle_beta                 91.829(5)
_cell_angle_gamma                111.105(7)
_cell_volume                     1757.7(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2886
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.5


_exptl_crystal_description       block
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_F_000             668
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.076
_shelx_estimated_absorpt_T_min   0.997
_shelx_estimated_absorpt_T_max   0.999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           'Mo K\a'
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Mitegen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_reflns_number            18323
_diffrn_reflns_av_unetI/netI     0.0937
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.076
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             6166
_reflns_number_gt                3532
_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       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_structure_solution    
'SUPERFLIP (Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  
'WinGX, ver.2013.3 (L.J. Farrugia, J.App.Cryst.(2012),45,849-854)'

_refine_special_details          
;
In (8polymorph2) aliphatic chain is badly disorder and modelled 
and constrained over two sites with 72:28 ratio. 
Vibrational restraints (SIMU/DELU) as well as distance/ange 
restraints DFIX/DANG were used to maintain sensible molecular 
geometry and atomic displacement ellipsoids. 
Some disordered atoms required 
EADP restraints to be used.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6166
_refine_ls_number_parameters     438
_refine_ls_number_restraints     575
_refine_ls_R_factor_all          0.1816
_refine_ls_R_factor_gt           0.1184
_refine_ls_wR_factor_ref         0.3751
_refine_ls_wR_factor_gt          0.3289
_refine_ls_goodness_of_fit_ref   1.263
_refine_ls_restrained_S_all      1.231
_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
C1 C 0.8422(7) 0.9162(5) 0.3458(2) 0.0318(12) Uani 1 1 d . U . . .
C1A C 0.8233(7) 0.6661(5) 0.3160(3) 0.0325(12) Uani 1 1 d . U . . .
H1AA H 0.7229 0.5784 0.3010 0.039 Uiso 1 1 calc R U . . .
H1AB H 0.8480 0.6723 0.3607 0.039 Uiso 1 1 calc R U . . .
C1S C 0.5177(6) 0.6510(5) 0.1512(2) 0.0309(12) Uani 1 1 d . U . . .
C2 C 0.9412(9) 0.9519(6) 0.4012(3) 0.0468(16) Uani 1 1 d . U . . .
H2 H 0.9826 0.8871 0.4158 0.056 Uiso 1 1 calc R U . . .
C2A C 0.9796(7) 0.6593(5) 0.2831(3) 0.0337(13) Uani 1 1 d D U . . .
H2AA H 0.9577 0.6582 0.2387 0.040 Uiso 1 1 calc R U . . .
H2AB H 1.0818 0.7444 0.2997 0.040 Uiso 1 1 calc R U . . .
C2S C 0.4268(7) 0.7154(5) 0.1156(3) 0.0310(12) Uani 1 1 d . U . . .
C3 C 0.9784(9) 1.0841(6) 0.4349(3) 0.0472(16) Uani 1 1 d . U . . .
H3 H 1.0424 1.1095 0.4741 0.057 Uiso 1 1 calc R U . . .
C3A C 1.0173(7) 0.5292(6) 0.2910(3) 0.0350(13) Uani 1 1 d D U . . .
H3AA H 1.0487 0.5342 0.3351 0.042 Uiso 1 1 calc R U . . .
H3AB H 0.9121 0.4445 0.2775 0.042 Uiso 1 1 calc R U . . .
C3S C 0.3680(6) 0.5826(5) 0.0671(3) 0.0305(12) Uani 1 1 d . U . . .
C4 C 0.9236(7) 1.1817(5) 0.4125(2) 0.0333(12) Uani 1 1 d . U . . .
C4A C 1.1631(8) 0.5167(6) 0.2540(3) 0.0427(14) Uani 1 1 d D U . . .
H4A1 H 1.1293 0.5103 0.2100 0.051 Uiso 1 1 calc R U . A 1
H4A2 H 1.2660 0.6037 0.2667 0.051 Uiso 1 1 calc R U . A 1
C4S C 0.4638(6) 0.5252(5) 0.1067(2) 0.0302(12) Uani 1 1 d . U . . .
C5 C 0.8279(7) 1.1447(5) 0.3546(2) 0.0313(12) Uani 1 1 d . U . . .
H5 H 0.7932 1.2112 0.3384 0.038 Uiso 1 1 calc R U . . .
C5S C 0.4779(6) 0.3953(5) 0.0999(3) 0.0306(12) Uani 1 1 d . U . . .
C6 C 0.7854(6) 1.0109(5) 0.3220(2) 0.0276(11) Uani 1 1 d . U . . .
C6S C 0.5661(7) 0.3556(5) 0.1461(2) 0.0305(12) Uani 1 1 d . U . . .
C7 C 0.6783(6) 0.9389(5) 0.2607(2) 0.0279(11) Uani 1 1 d . U . . .
C7S C 0.4030(6) 0.2954(5) 0.0453(3) 0.0309(12) Uani 1 1 d . U . . .
C8 C 0.6851(6) 0.7922(5) 0.2540(2) 0.0269(11) Uani 1 1 d . U . . .
C10 C 0.4928(7) 0.9338(6) 0.2654(3) 0.0353(13) Uani 1 1 d . U . . .
H10A H 0.4487 0.8956 0.3020 0.053 Uiso 1 1 calc R U . . .
H10C H 0.4195 0.8735 0.2287 0.053 Uiso 1 1 calc R U . . .
H10B H 0.4920 1.0289 0.2686 0.053 Uiso 1 1 calc R U . . .
C9 C 0.7590(7) 1.0135(6) 0.2084(3) 0.0354(13) Uani 1 1 d . U . . .
H9A H 0.7515 1.1067 0.2140 0.053 Uiso 1 1 calc R U . . .
H9B H 0.6969 0.9581 0.1690 0.053 Uiso 1 1 calc R U . . .
H9C H 0.8801 1.0234 0.2088 0.053 Uiso 1 1 calc R U . . .
C11 C 0.6200(6) 0.6784(5) 0.2083(2) 0.0288(12) Uani 1 1 d . U . . .
H11 H 0.6480 0.6009 0.2158 0.035 Uiso 1 1 calc R U . . .
C12 C 0.9609(7) 1.3221(6) 0.4494(2) 0.0315(12) Uani 1 1 d . U . . .
C13 C 0.9293(7) 0.2310(6) 1.0011(3) 0.0370(13) Uani 1 1 d . U . . .
H13A H 0.9613 0.3342 1.0086 0.044 Uiso 1 1 calc R U . . .
H13B H 1.0242 0.2108 1.0205 0.044 Uiso 1 1 calc R U . . .
C14 C 0.7669(7) 0.1649(6) 1.0311(3) 0.0394(14) Uani 1 1 d . U . . .
H14A H 0.6735 0.1874 1.0132 0.059 Uiso 1 1 calc R U . . .
H14B H 0.7867 0.2018 1.0754 0.059 Uiso 1 1 calc R U . . .
H14C H 0.7351 0.0628 1.0241 0.059 Uiso 1 1 calc R U . . .
C15 C 0.9027(7) 0.0294(5) 0.9187(3) 0.0373(13) Uani 1 1 d . U . . .
H15A H 0.8474 -0.0220 0.9513 0.045 Uiso 1 1 calc R U . . .
H15B H 1.0215 0.0302 0.9184 0.045 Uiso 1 1 calc R U . . .
C16 C 0.8038(7) -0.0461(6) 0.8574(3) 0.0417(14) Uani 1 1 d . U . . .
H16A H 0.8545 0.0073 0.8254 0.062 Uiso 1 1 calc R U . . .
H16B H 0.6833 -0.0547 0.8589 0.062 Uiso 1 1 calc R U . . .
H16C H 0.8091 -0.1399 0.8481 0.062 Uiso 1 1 calc R U . . .
C17 C 1.0527(7) 0.2727(6) 0.9021(3) 0.0383(13) Uani 1 1 d . U . . .
H17A H 1.1639 0.2972 0.9268 0.046 Uiso 1 1 calc R U . . .
H17B H 1.0589 0.2213 0.8612 0.046 Uiso 1 1 calc R U . . .
C18 C 1.0264(7) 0.4047(6) 0.8947(3) 0.0393(14) Uani 1 1 d . U . . .
H18A H 0.9184 0.3811 0.8691 0.059 Uiso 1 1 calc R U . . .
H18B H 1.1227 0.4632 0.8749 0.059 Uiso 1 1 calc R U . . .
H18C H 1.0210 0.4562 0.9351 0.059 Uiso 1 1 calc R U . . .
C5A C 1.2126(15) 0.3923(11) 0.2607(5) 0.062(2) Uani 0.717(6) 1 d D U P B 1
H5AA H 1.2888 0.3814 0.2285 0.074 Uiso 0.717(6) 1 calc R U P B 1
H5AB H 1.1071 0.3061 0.2536 0.074 Uiso 0.717(6) 1 calc R U P B 1
C6A C 1.3048(12) 0.4062(10) 0.3240(5) 0.072(3) Uani 0.717(6) 1 d D U P B 1
H6AA H 1.2293 0.4112 0.3571 0.087 Uiso 0.717(6) 1 calc R U P B 1
H6AB H 1.4121 0.4908 0.3324 0.087 Uiso 0.717(6) 1 calc R U P B 1
C7A C 1.3451(17) 0.2682(12) 0.3181(6) 0.101(3) Uani 0.717(6) 1 d D U P B 1
H7AA H 1.2376 0.1878 0.3201 0.122 Uiso 0.717(6) 1 calc R U P B 1
H7AB H 1.3877 0.2506 0.2775 0.122 Uiso 0.717(6) 1 calc R U P B 1
C8A C 1.4764(14) 0.2778(14) 0.3676(4) 0.087(3) Uani 0.717(6) 1 d D U P B 1
H8AA H 1.5849 0.3578 0.3661 0.105 Uiso 0.717(6) 1 calc R U P B 1
H8AB H 1.5013 0.1905 0.3621 0.105 Uiso 0.717(6) 1 calc R U P B 1
C9A C 1.4036(15) 0.2988(16) 0.4286(4) 0.086(3) Uani 0.717(6) 1 d D U P B 1
H9AA H 1.2850 0.2292 0.4270 0.103 Uiso 0.717(6) 1 calc R U P B 1
H9AB H 1.3996 0.3941 0.4376 0.103 Uiso 0.717(6) 1 calc R U P B 1
C10A C 1.5205(14) 0.2802(15) 0.4789(4) 0.083(3) Uani 0.717(6) 1 d D U P B 1
H10D H 1.5296 0.1871 0.4671 0.099 Uiso 0.717(6) 1 calc R U P B 1
H10E H 1.6373 0.3524 0.4802 0.099 Uiso 0.717(6) 1 calc R U P B 1
C11A C 1.4620(17) 0.2904(16) 0.5425(4) 0.094(3) Uani 0.717(6) 1 d D U P B 1
H11A H 1.3393 0.2285 0.5407 0.112 Uiso 0.717(6) 1 calc R U P B 1
H11B H 1.4711 0.3881 0.5575 0.112 Uiso 0.717(6) 1 calc R U P B 1
C12A C 1.569(2) 0.249(2) 0.5882(7) 0.130(6) Uani 0.717(6) 1 d D U P B 1
H12A H 1.5926 0.1674 0.5680 0.195 Uiso 0.717(6) 1 calc R U P B 1
H12B H 1.5036 0.2243 0.6236 0.195 Uiso 0.717(6) 1 calc R U P B 1
H12C H 1.6774 0.3276 0.6022 0.195 Uiso 0.717(6) 1 calc R U P B 1
C5B C 1.211(2) 0.394(2) 0.2683(15) 0.062(2) Uani 0.283(6) 1 d D U P B 2
H5BA H 1.1401 0.3061 0.2401 0.074 Uiso 0.283(6) 1 calc R U P B 2
H5BB H 1.1883 0.3803 0.3110 0.074 Uiso 0.283(6) 1 calc R U P B 2
C6B C 1.404(2) 0.426(3) 0.2604(9) 0.072(3) Uani 0.283(6) 1 d D U P B 2
H6BA H 1.4524 0.5117 0.2419 0.087 Uiso 0.283(6) 1 calc R U P B 2
H6BB H 1.4189 0.3469 0.2335 0.087 Uiso 0.283(6) 1 calc R U P B 2
C7B C 1.493(3) 0.450(3) 0.3255(11) 0.101(3) Uani 0.283(6) 1 d D U P B 2
H7BA H 1.5026 0.5417 0.3495 0.122 Uiso 0.283(6) 1 calc R U P B 2
H7BB H 1.6101 0.4474 0.3233 0.122 Uiso 0.283(6) 1 calc R U P B 2
C8B C 1.377(3) 0.328(3) 0.3556(11) 0.087(3) Uani 0.283(6) 1 d D U P B 2
H8BA H 1.2590 0.3282 0.3559 0.105 Uiso 0.283(6) 1 calc R U P B 2
H8BB H 1.3715 0.2365 0.3322 0.105 Uiso 0.283(6) 1 calc R U P B 2
C9B C 1.456(5) 0.349(3) 0.4213(10) 0.086(3) Uani 0.283(6) 1 d D U P B 2
H9BA H 1.3845 0.3794 0.4509 0.103 Uiso 0.283(6) 1 calc R U P B 2
H9BB H 1.5731 0.4236 0.4271 0.103 Uiso 0.283(6) 1 calc R U P B 2
C10B C 1.467(4) 0.209(3) 0.4328(9) 0.083(3) Uani 0.283(6) 1 d D U P B 2
H10F H 1.5419 0.1812 0.4042 0.099 Uiso 0.283(6) 1 calc R U P B 2
H10G H 1.3506 0.1346 0.4256 0.099 Uiso 0.283(6) 1 calc R U P B 2
C11B C 1.541(4) 0.229(3) 0.5000(11) 0.094(3) Uani 0.283(6) 1 d D U P B 2
H11C H 1.6432 0.2023 0.5009 0.112 Uiso 0.283(6) 1 calc R U P B 2
H11D H 1.5771 0.3292 0.5199 0.112 Uiso 0.283(6) 1 calc R U P B 2
C12B C 1.400(5) 0.136(5) 0.5349(15) 0.130(6) Uani 0.283(6) 1 d D U P B 2
H12D H 1.4454 0.1476 0.5776 0.195 Uiso 0.283(6) 1 calc R U P B 2
H12E H 1.3659 0.0375 0.5151 0.195 Uiso 0.283(6) 1 calc R U P B 2
H12F H 1.3000 0.1639 0.5340 0.195 Uiso 0.283(6) 1 calc R U P B 2
N1 N 0.7793(6) 0.7867(4) 0.30600(19) 0.0323(11) Uani 1 1 d . U . . .
N1S N 0.6394(6) 0.3267(5) 0.1830(2) 0.0405(12) Uani 1 1 d . U . . .
N2S N 0.3413(6) 0.2128(4) 0.0014(2) 0.0345(11) Uani 1 1 d . U . . .
N2 N 0.9097(6) 0.1781(4) 0.9333(2) 0.0335(11) Uani 1 1 d . U . . .
H2A H 0.7982 0.1793 0.9160 0.040 Uiso 1 1 calc R U . . .
O1 O 1.0374(6) 1.3429(4) 0.50466(18) 0.0507(12) Uani 1 1 d . U . . .
H1 H 1.0657 1.4277 0.5211 0.076 Uiso 1 1 calc R U . . .
O1S O 0.3977(5) 0.8245(4) 0.12074(17) 0.0383(10) Uani 1 1 d . U . . .
O2S O 0.2769(5) 0.5386(4) 0.01921(18) 0.0372(10) Uani 1 1 d . U . . .
O7 O 0.9209(5) 1.4104(4) 0.42969(17) 0.0387(10) Uani 1 1 d . 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
C1 C2 1.378(7) . ?
C1 N1 1.395(7) . ?
C1 C6 1.396(7) . ?
C1A N1 1.470(6) . ?
C1A C2A 1.534(8) . ?
C1S C4S 1.423(7) . ?
C1S C11 1.432(7) . ?
C1S C2S 1.461(7) . ?
C2 C3 1.375(8) . ?
C2A C3A 1.524(7) . ?
C2S O1S 1.230(6) . ?
C2S C3S 1.519(7) . ?
C3 C4 1.398(8) . ?
C3A C4A 1.522(8) . ?
C3S O2S 1.207(6) . ?
C3S C4S 1.491(7) . ?
C4 C5 1.409(7) . ?
C4 C12 1.474(7) . ?
C4A C5A 1.514(7) . ?
C4A C5B 1.539(10) . ?
C4S C5S 1.379(7) . ?
C5 C6 1.374(7) . ?
C5S C7S 1.421(7) . ?
C5S C6S 1.434(7) . ?
C6 C7 1.523(7) . ?
C6S N1S 1.143(6) . ?
C7 C8 1.528(7) . ?
C7 C9 1.531(8) . ?
C7 C10 1.539(7) . ?
C7S N2S 1.155(6) . ?
C8 C11 1.356(7) . ?
C8 N1 1.393(6) . ?
C12 O7 1.215(6) . ?
C12 O1 1.310(6) . ?
C13 N2 1.497(7) . ?
C13 C14 1.509(9) . ?
C15 N2 1.505(7) . ?
C15 C16 1.506(8) . ?
C17 C18 1.494(8) . ?
C17 N2 1.511(7) . ?
C5A C6A 1.537(9) . ?
C6A C7A 1.572(9) . ?
C7A C8A 1.492(8) . ?
C8A C9A 1.515(9) . ?
C9A C10A 1.537(9) . ?
C10A C11A 1.505(9) . ?
C11A C12A 1.535(9) . ?
C5B C6B 1.542(10) . ?
C6B C7B 1.543(10) . ?
C7B C8B 1.550(10) . ?
C8B C9B 1.526(10) . ?
C9B C10B 1.544(10) . ?
C10B C11B 1.545(10) . ?
C11B C12B 1.545(10) . ?

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
C2 C1 N1 128.3(5) . . ?
C2 C1 C6 122.3(5) . . ?
N1 C1 C6 109.4(4) . . ?
N1 C1A C2A 112.6(4) . . ?
C4S C1S C11 126.3(5) . . ?
C4S C1S C2S 92.6(4) . . ?
C11 C1S C2S 141.0(5) . . ?
C3 C2 C1 118.1(5) . . ?
C3A C2A C1A 111.9(5) . . ?
O1S C2S C1S 138.3(5) . . ?
O1S C2S C3S 133.0(5) . . ?
C1S C2S C3S 88.6(4) . . ?
C2 C3 C4 121.1(5) . . ?
C4A C3A C2A 111.6(5) . . ?
O2S C3S C4S 135.6(5) . . ?
O2S C3S C2S 136.7(5) . . ?
C4S C3S C2S 87.7(4) . . ?
C3 C4 C5 119.9(5) . . ?
C3 C4 C12 120.8(5) . . ?
C5 C4 C12 119.3(5) . . ?
C5A C4A C3A 115.2(6) . . ?
C3A C4A C5B 110.4(9) . . ?
C5S C4S C1S 137.8(5) . . ?
C5S C4S C3S 131.0(5) . . ?
C1S C4S C3S 91.2(4) . . ?
C6 C5 C4 119.0(5) . . ?
C4S C5S C7S 119.6(5) . . ?
C4S C5S C6S 122.7(5) . . ?
C7S C5S C6S 117.7(4) . . ?
C5 C6 C1 119.5(5) . . ?
C5 C6 C7 131.1(5) . . ?
C1 C6 C7 109.4(4) . . ?
N1S C6S C5S 178.5(6) . . ?
C6 C7 C8 101.7(4) . . ?
C6 C7 C9 111.1(4) . . ?
C8 C7 C9 111.6(4) . . ?
C6 C7 C10 109.7(4) . . ?
C8 C7 C10 111.3(4) . . ?
C9 C7 C10 111.0(4) . . ?
N2S C7S C5S 179.1(6) . . ?
C11 C8 N1 120.3(4) . . ?
C11 C8 C7 131.6(4) . . ?
N1 C8 C7 108.2(4) . . ?
C8 C11 C1S 133.2(5) . . ?
O7 C12 O1 123.2(5) . . ?
O7 C12 C4 121.7(5) . . ?
O1 C12 C4 115.0(5) . . ?
N2 C13 C14 112.6(4) . . ?
N2 C15 C16 111.7(4) . . ?
C18 C17 N2 112.3(5) . . ?
C4A C5A C6A 113.5(7) . . ?
C5A C6A C7A 103.2(7) . . ?
C8A C7A C6A 112.0(8) . . ?
C7A C8A C9A 107.6(8) . . ?
C8A C9A C10A 108.2(8) . . ?
C11A C10A C9A 115.4(8) . . ?
C10A C11A C12A 112.5(9) . . ?
C4A C5B C6B 109.3(12) . . ?
C5B C6B C7B 106.2(12) . . ?
C6B C7B C8B 105.5(11) . . ?
C9B C8B C7B 107.6(13) . . ?
C8B C9B C10B 108.5(13) . . ?
C9B C10B C11B 108.7(13) . . ?
C12B C11B C10B 108.5(10) . . ?
C8 N1 C1 111.3(4) . . ?
C8 N1 C1A 125.3(4) . . ?
C1 N1 C1A 123.1(4) . . ?
C13 N2 C15 112.0(4) . . ?
C13 N2 C17 111.1(4) . . ?
C15 N2 C17 110.1(4) . . ?

_refine_diff_density_max         2.159
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.110

_shelxl_version_number           2013-3



