# Electronic Supplementary Material (ESI) for ChemComm.
# 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. 
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data_dfya53c
_database_code_depnum_ccdc_archive 'CCDC 1412209'
_audit_update_record             
;
2015-07-12 deposited with the CCDC.
2015-08-17 downloaded from the CCDC.
;
_audit_creation_date             2015-01-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H54 N2 O8, 2(C4 H8 O2)'
_chemical_formula_sum            'C80 H70 N2 O12'
_chemical_formula_weight         1251.38
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'

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

_cell_length_a                   16.978(2)
_cell_length_b                   16.7517(19)
_cell_length_c                   10.8751(13)
_cell_angle_alpha                90
_cell_angle_beta                 92.952(4)
_cell_angle_gamma                90
_cell_volume                     3088.8(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.014
_cell_measurement_theta_min      2.235
_shelx_estimated_absorpt_T_max   0.998
_shelx_estimated_absorpt_T_min   0.961
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1601 before and 0.0606 after correction.
The Ratio of minimum to maximum transmission is 0.9353.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            47356
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.067
_diffrn_reflns_theta_min         2.235
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON-100 area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_number_gt                4389
_reflns_number_total             5462
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         5462
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0487
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0501P)²+2.4484P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1239
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,
 H39B), C40(H40A,H40B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C18(H18), C19(H19), C24(H24),
 C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31)
2.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.27440(8) 0.42267(8) 0.58541(13) 0.0260(3) Uani 1 1 d . . . . .
O2 O 0.33820(8) 0.68543(8) 0.54976(14) 0.0295(4) Uani 1 1 d . . . . .
O3 O 0.18437(8) 0.53631(8) 0.40608(12) 0.0233(3) Uani 1 1 d . . . . .
O4 O 0.10510(8) 0.42849(9) 0.41365(15) 0.0344(4) Uani 1 1 d . . . . .
N1 N 0.30781(9) 0.55394(9) 0.57303(14) 0.0187(3) Uani 1 1 d . . . . .
C1 C 0.32471(11) 0.47192(11) 0.56655(17) 0.0186(4) Uani 1 1 d . . . . .
C2 C 0.40636(11) 0.45011(11) 0.53814(16) 0.0174(4) Uani 1 1 d . . . . .
C3 C 0.46107(11) 0.51069(11) 0.51351(16) 0.0157(4) Uani 1 1 d . . . . .
C4 C 0.43995(11) 0.59216(11) 0.51536(16) 0.0173(4) Uani 1 1 d . . . . .
C5 C 0.35934(11) 0.61631(11) 0.54624(17) 0.0201(4) Uani 1 1 d . . . . .
C6 C 0.42811(11) 0.37109(11) 0.53620(17) 0.0201(4) Uani 1 1 d . . . . .
H6 H 0.3908 0.3308 0.5531 0.024 Uiso 1 1 calc R . . . .
C7 C 0.49460(12) 0.65012(11) 0.49071(18) 0.0207(4) Uani 1 1 d . . . . .
H7 H 0.4799 0.7048 0.4919 0.025 Uiso 1 1 calc R . . . .
C8 C 0.22894(11) 0.57463(11) 0.60632(18) 0.0206(4) Uani 1 1 d . . . . .
C9 C 0.16622(11) 0.56090(11) 0.52415(17) 0.0201(4) Uani 1 1 d . . . . .
C10 C 0.09018(11) 0.57654(12) 0.55741(18) 0.0230(4) Uani 1 1 d . . . . .
H10 H 0.0466 0.5674 0.5008 0.028 Uiso 1 1 calc R . . . .
C11 C 0.07830(12) 0.60561(13) 0.67402(19) 0.0266(5) Uani 1 1 d . . . . .
H11 H 0.0260 0.6156 0.6969 0.032 Uiso 1 1 calc R . . . .
C12 C 0.14097(12) 0.62072(13) 0.75922(19) 0.0275(5) Uani 1 1 d . . . . .
C13 C 0.21662(12) 0.60520(12) 0.72161(18) 0.0254(5) Uani 1 1 d . . . . .
H13 H 0.2607 0.6159 0.7765 0.030 Uiso 1 1 calc R . . . .
C14 C 0.15082(12) 0.46779(13) 0.35991(19) 0.0259(5) Uani 1 1 d . . . . .
C15 C 0.17961(12) 0.45142(15) 0.2335(2) 0.0330(5) Uani 1 1 d . . . . .
H15A H 0.1741 0.5007 0.1836 0.040 Uiso 1 1 calc R . . . .
H15B H 0.1456 0.4101 0.1931 0.040 Uiso 1 1 calc R . . . .
C16 C 0.26523(12) 0.42350(13) 0.23454(18) 0.0262(5) Uani 1 1 d . . . . .
C17 C 0.32811(12) 0.47611(12) 0.21652(17) 0.0236(4) Uani 1 1 d . . . . .
C18 C 0.31956(13) 0.56153(13) 0.20756(19) 0.0301(5) Uani 1 1 d . . . . .
H18 H 0.2694 0.5847 0.2193 0.036 Uiso 1 1 calc R . . . .
C19 C 0.38052(14) 0.60959(13) 0.18298(19) 0.0321(5) Uani 1 1 d . . . . .
H19 H 0.3721 0.6656 0.1777 0.039 Uiso 1 1 calc R . . . .
C20 C 0.45778(13) 0.57845(12) 0.16463(18) 0.0274(5) Uani 1 1 d . . . . .
C21 C 0.46956(12) 0.49479(12) 0.17621(17) 0.0232(4) Uani 1 1 d . . . . .
C22 C 0.40544(12) 0.44405(12) 0.20401(17) 0.0221(4) Uani 1 1 d . . . . .
C23 C 0.41823(12) 0.36017(12) 0.21370(17) 0.0228(4) Uani 1 1 d . . . . .
C24 C 0.35477(13) 0.31091(12) 0.23753(19) 0.0271(5) Uani 1 1 d . . . . .
H24 H 0.3631 0.2552 0.2479 0.032 Uiso 1 1 calc R . . . .
C25 C 0.27956(13) 0.34205(13) 0.24635(19) 0.0289(5) Uani 1 1 d . . . . .
H25 H 0.2370 0.3070 0.2608 0.035 Uiso 1 1 calc R . . . .
C26 C 0.52071(15) 0.62663(13) 0.13287(19) 0.0339(5) Uani 1 1 d . . . . .
H26 H 0.5133 0.6827 0.1260 0.041 Uiso 1 1 calc R . . . .
C27 C 0.59379(14) 0.59404(14) 0.1111(2) 0.0349(5) Uani 1 1 d . . . . .
H27 H 0.6356 0.6277 0.0885 0.042 Uiso 1 1 calc R . . . .
C28 C 0.60595(13) 0.51280(14) 0.12234(19) 0.0313(5) Uani 1 1 d . . . . .
H28 H 0.6563 0.4911 0.1078 0.038 Uiso 1 1 calc R . . . .
C29 C 0.54484(12) 0.46205(12) 0.15488(17) 0.0240(4) Uani 1 1 d . . . . .
C30 C 0.55510(13) 0.37701(13) 0.16553(18) 0.0272(5) Uani 1 1 d . . . . .
H30 H 0.6051 0.3543 0.1516 0.033 Uiso 1 1 calc R . . . .
C31 C 0.49570(13) 0.32920(12) 0.19467(18) 0.0267(5) Uani 1 1 d . . . . .
H31 H 0.5049 0.2735 0.2030 0.032 Uiso 1 1 calc R . . . .
C32 C 0.12509(13) 0.65201(16) 0.8883(2) 0.0368(6) Uani 1 1 d . . . . .
C33 C 0.07676(19) 0.58779(16) 0.9556(2) 0.0549(8) Uani 1 1 d . . . . .
H33A H 0.0257 0.5799 0.9110 0.082 Uiso 1 1 calc GR . . . .
H33B H 0.0682 0.6057 1.0397 0.082 Uiso 1 1 calc GR . . . .
H33C H 0.1060 0.5373 0.9586 0.082 Uiso 1 1 calc GR . . . .
C34 C 0.20154(16) 0.6665(3) 0.9648(3) 0.0751(12) Uani 1 1 d . . . . .
H34A H 0.2330 0.6174 0.9682 0.113 Uiso 1 1 calc GR . . . .
H34B H 0.1893 0.6823 1.0484 0.113 Uiso 1 1 calc GR . . . .
H34C H 0.2316 0.7091 0.9269 0.113 Uiso 1 1 calc GR . . . .
C35 C 0.07615(14) 0.72856(13) 0.8778(2) 0.0341(5) Uani 1 1 d . . . . .
H35A H 0.0232 0.7154 0.8411 0.041 Uiso 1 1 calc R . . . .
H35B H 0.0693 0.7499 0.9615 0.041 Uiso 1 1 calc R . . . .
C36 C 0.1123(2) 0.79246(17) 0.8012(3) 0.0639(9) Uani 1 1 d . . . . .
H36A H 0.1657 0.8042 0.8345 0.096 Uiso 1 1 calc GR . . . .
H36B H 0.0801 0.8409 0.8031 0.096 Uiso 1 1 calc GR . . . .
H36C H 0.1146 0.7738 0.7160 0.096 Uiso 1 1 calc GR . . . .
O5 O 0.10857(9) 0.22211(10) 0.26275(14) 0.0361(4) Uani 1 1 d . . . . .
O6 O 0.16512(14) 0.11581(10) 0.44787(16) 0.0599(6) Uani 1 1 d . . . . .
C37 C 0.08826(15) 0.23068(14) 0.3874(2) 0.0401(6) Uani 1 1 d . . . . .
H37A H 0.0380 0.2025 0.3997 0.048 Uiso 1 1 calc R . . . .
H37B H 0.0805 0.2879 0.4059 0.048 Uiso 1 1 calc R . . . .
C38 C 0.15087(19) 0.19770(15) 0.4728(2) 0.0490(7) Uani 1 1 d . . . . .
H38A H 0.2001 0.2284 0.4645 0.059 Uiso 1 1 calc R . . . .
H38B H 0.1349 0.2035 0.5586 0.059 Uiso 1 1 calc R . . . .
C39 C 0.18435(17) 0.10689(16) 0.3229(2) 0.0451(6) Uani 1 1 d . . . . .
H39A H 0.1919 0.0496 0.3047 0.054 Uiso 1 1 calc R . . . .
H39B H 0.2345 0.1349 0.3096 0.054 Uiso 1 1 calc R . . . .
C40 C 0.12103(14) 0.13988(15) 0.2372(2) 0.0396(6) Uani 1 1 d . . . . .
H40A H 0.1363 0.1336 0.1512 0.047 Uiso 1 1 calc R . . . .
H40B H 0.0715 0.1099 0.2468 0.047 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.213(2) . ?
O2 C5 1.214(2) . ?
O3 C9 1.398(2) . ?
O3 C14 1.365(2) . ?
O4 C14 1.193(3) . ?
N1 C1 1.406(2) . ?
N1 C5 1.403(2) . ?
N1 C8 1.447(2) . ?
C1 C2 1.481(3) . ?
C2 C3 1.411(3) . ?
C2 C6 1.375(3) . ?
C3 C3 1.415(4) 3_666 ?
C3 C4 1.412(3) . ?
C4 C5 1.482(3) . ?
C4 C7 1.379(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.405(3) 3_666 ?
C7 C6 1.405(3) 3_666 ?
C7 H7 0.9500 . ?
C8 C9 1.374(3) . ?
C8 C13 1.380(3) . ?
C9 C10 1.384(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.383(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.398(3) . ?
C12 C13 1.392(3) . ?
C12 C32 1.535(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.508(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.526(3) . ?
C16 C17 1.406(3) . ?
C16 C25 1.391(3) . ?
C17 C18 1.441(3) . ?
C17 C22 1.431(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.349(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.435(3) . ?
C20 C21 1.420(3) . ?
C20 C26 1.397(3) . ?
C21 C22 1.426(3) . ?
C21 C29 1.421(3) . ?
C22 C23 1.425(3) . ?
C23 C24 1.392(3) . ?
C23 C31 1.439(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.387(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C26 C27 1.387(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.381(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.401(3) . ?
C29 C30 1.439(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.339(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.558(4) . ?
C32 C34 1.524(3) . ?
C32 C35 1.529(3) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.506(3) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
O5 C37 1.423(3) . ?
O5 C40 1.423(3) . ?
O6 C38 1.421(3) . ?
O6 C39 1.422(3) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.482(4) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.492(4) . ?
C40 H40A 0.9900 . ?
C40 H40B 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
C14 O3 C9 118.56(15) . . ?
C1 N1 C8 116.13(15) . . ?
C5 N1 C1 125.89(15) . . ?
C5 N1 C8 117.94(15) . . ?
O1 C1 N1 120.59(17) . . ?
O1 C1 C2 122.84(17) . . ?
N1 C1 C2 116.55(16) . . ?
C3 C2 C1 119.63(16) . . ?
C6 C2 C1 119.71(16) . . ?
C6 C2 C3 120.65(17) . . ?
C2 C3 C3 119.3(2) . 3_666 ?
C2 C3 C4 121.52(17) . . ?
C4 C3 C3 119.2(2) . 3_666 ?
C3 C4 C5 120.35(16) . . ?
C7 C4 C3 120.27(17) . . ?
C7 C4 C5 119.37(17) . . ?
O2 C5 N1 121.03(17) . . ?
O2 C5 C4 123.06(17) . . ?
N1 C5 C4 115.90(16) . . ?
C2 C6 H6 120.0 . . ?
C2 C6 C7 120.09(17) . 3_666 ?
C7 C6 H6 120.0 3_666 . ?
C4 C7 C6 120.50(17) . 3_666 ?
C4 C7 H7 119.7 . . ?
C6 C7 H7 119.7 3_666 . ?
C9 C8 N1 119.57(17) . . ?
C9 C8 C13 120.29(18) . . ?
C13 C8 N1 120.10(17) . . ?
C8 C9 O3 116.53(16) . . ?
C8 C9 C10 120.05(17) . . ?
C10 C9 O3 123.28(17) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 C9 119.24(18) . . ?
C11 C10 H10 120.4 . . ?
C10 C11 H11 119.0 . . ?
C10 C11 C12 121.99(18) . . ?
C12 C11 H11 119.0 . . ?
C11 C12 C32 120.30(18) . . ?
C13 C12 C11 116.99(18) . . ?
C13 C12 C32 122.71(19) . . ?
C8 C13 C12 121.42(19) . . ?
C8 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
O3 C14 C15 109.85(18) . . ?
O4 C14 O3 123.58(19) . . ?
O4 C14 C15 126.57(19) . . ?
C14 C15 H15A 108.8 . . ?
C14 C15 H15B 108.8 . . ?
C14 C15 C16 113.71(17) . . ?
H15A C15 H15B 107.7 . . ?
C16 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
C17 C16 C15 122.45(19) . . ?
C25 C16 C15 117.61(19) . . ?
C25 C16 C17 119.82(19) . . ?
C16 C17 C18 123.87(19) . . ?
C16 C17 C22 119.00(18) . . ?
C22 C17 C18 117.12(19) . . ?
C17 C18 H18 119.0 . . ?
C19 C18 C17 122.0(2) . . ?
C19 C18 H18 119.0 . . ?
C18 C19 H19 119.1 . . ?
C18 C19 C20 121.8(2) . . ?
C20 C19 H19 119.1 . . ?
C21 C20 C19 118.16(19) . . ?
C26 C20 C19 122.7(2) . . ?
C26 C20 C21 119.1(2) . . ?
C20 C21 C22 120.10(19) . . ?
C20 C21 C29 119.35(19) . . ?
C29 C21 C22 120.50(18) . . ?
C21 C22 C17 120.69(18) . . ?
C23 C22 C17 120.00(18) . . ?
C23 C22 C21 119.25(18) . . ?
C22 C23 C31 118.80(18) . . ?
C24 C23 C22 118.82(18) . . ?
C24 C23 C31 122.35(18) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 C23 120.92(19) . . ?
C25 C24 H24 119.5 . . ?
C16 C25 H25 119.3 . . ?
C24 C25 C16 121.3(2) . . ?
C24 C25 H25 119.3 . . ?
C20 C26 H26 119.4 . . ?
C27 C26 C20 121.1(2) . . ?
C27 C26 H26 119.4 . . ?
C26 C27 H27 119.9 . . ?
C28 C27 C26 120.3(2) . . ?
C28 C27 H27 119.9 . . ?
C27 C28 H28 119.6 . . ?
C27 C28 C29 120.7(2) . . ?
C29 C28 H28 119.6 . . ?
C21 C29 C30 118.37(18) . . ?
C28 C29 C21 119.42(19) . . ?
C28 C29 C30 122.2(2) . . ?
C29 C30 H30 119.3 . . ?
C31 C30 C29 121.45(19) . . ?
C31 C30 H30 119.3 . . ?
C23 C31 H31 119.2 . . ?
C30 C31 C23 121.59(19) . . ?
C30 C31 H31 119.2 . . ?
C12 C32 C33 108.4(2) . . ?
C34 C32 C12 111.63(18) . . ?
C34 C32 C33 107.9(2) . . ?
C34 C32 C35 110.6(2) . . ?
C35 C32 C12 109.77(19) . . ?
C35 C32 C33 108.47(18) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 108.8 . . ?
C32 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
C36 C35 C32 113.7(2) . . ?
C36 C35 H35A 108.8 . . ?
C36 C35 H35B 108.8 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C40 O5 C37 109.21(17) . . ?
C38 O6 C39 109.46(18) . . ?
O5 C37 H37A 109.4 . . ?
O5 C37 H37B 109.4 . . ?
O5 C37 C38 110.97(19) . . ?
H37A C37 H37B 108.0 . . ?
C38 C37 H37A 109.4 . . ?
C38 C37 H37B 109.4 . . ?
O6 C38 C37 111.4(2) . . ?
O6 C38 H38A 109.4 . . ?
O6 C38 H38B 109.4 . . ?
C37 C38 H38A 109.4 . . ?
C37 C38 H38B 109.4 . . ?
H38A C38 H38B 108.0 . . ?
O6 C39 H39A 109.4 . . ?
O6 C39 H39B 109.4 . . ?
O6 C39 C40 111.4(2) . . ?
H39A C39 H39B 108.0 . . ?
C40 C39 H39A 109.4 . . ?
C40 C39 H39B 109.4 . . ?
O5 C40 C39 110.3(2) . . ?
O5 C40 H40A 109.6 . . ?
O5 C40 H40B 109.6 . . ?
C39 C40 H40A 109.6 . . ?
C39 C40 H40B 109.6 . . ?
H40A C40 H40B 108.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 178.06(18) . . . . ?
O1 C1 C2 C6 -2.0(3) . . . . ?
O3 C9 C10 C11 -175.81(18) . . . . ?
O3 C14 C15 C16 72.4(2) . . . . ?
O4 C14 C15 C16 -108.3(2) . . . . ?
N1 C1 C2 C3 -3.0(2) . . . . ?
N1 C1 C2 C6 176.88(17) . . . . ?
N1 C8 C9 O3 -7.6(3) . . . . ?
N1 C8 C9 C10 176.61(17) . . . . ?
N1 C8 C13 C12 -175.70(19) . . . . ?
C1 N1 C5 O2 177.00(18) . . . . ?
C1 N1 C5 C4 -3.6(3) . . . . ?
C1 N1 C8 C9 -70.5(2) . . . . ?
C1 N1 C8 C13 107.1(2) . . . . ?
C1 C2 C3 C3 179.99(19) . . . 3_666 ?
C1 C2 C3 C4 0.1(3) . . . . ?
C1 C2 C6 C7 179.98(17) . . . 3_666 ?
C2 C3 C4 C5 1.3(3) . . . . ?
C2 C3 C4 C7 -179.88(17) . . . . ?
C3 C2 C6 C7 -0.1(3) . . . 3_666 ?
C3 C3 C4 C5 -178.57(19) 3_666 . . . ?
C3 C3 C4 C7 0.2(3) 3_666 . . . ?
C3 C4 C5 O2 179.62(18) . . . . ?
C3 C4 C5 N1 0.3(3) . . . . ?
C3 C4 C7 C6 -0.2(3) . . . 3_666 ?
C5 N1 C1 O1 -176.05(18) . . . . ?
C5 N1 C1 C2 5.0(3) . . . . ?
C5 N1 C8 C9 107.3(2) . . . . ?
C5 N1 C8 C13 -75.0(2) . . . . ?
C5 C4 C7 C6 178.62(17) . . . 3_666 ?
C6 C2 C3 C3 0.1(3) . . . 3_666 ?
C6 C2 C3 C4 -179.84(17) . . . . ?
C7 C4 C5 O2 0.8(3) . . . . ?
C7 C4 C5 N1 -178.51(17) . . . . ?
C8 N1 C1 O1 1.6(3) . . . . ?
C8 N1 C1 C2 -177.30(16) . . . . ?
C8 N1 C5 O2 -0.7(3) . . . . ?
C8 N1 C5 C4 178.70(16) . . . . ?
C8 C9 C10 C11 -0.3(3) . . . . ?
C9 O3 C14 O4 1.9(3) . . . . ?
C9 O3 C14 C15 -178.72(16) . . . . ?
C9 C8 C13 C12 1.9(3) . . . . ?
C9 C10 C11 C12 0.8(3) . . . . ?
C10 C11 C12 C13 0.0(3) . . . . ?
C10 C11 C12 C32 -179.2(2) . . . . ?
C11 C12 C13 C8 -1.4(3) . . . . ?
C11 C12 C32 C33 62.8(3) . . . . ?
C11 C12 C32 C34 -178.4(3) . . . . ?
C11 C12 C32 C35 -55.5(3) . . . . ?
C12 C32 C35 C36 -54.9(3) . . . . ?
C13 C8 C9 O3 174.76(18) . . . . ?
C13 C8 C9 C10 -1.0(3) . . . . ?
C13 C12 C32 C33 -116.4(2) . . . . ?
C13 C12 C32 C34 2.4(4) . . . . ?
C13 C12 C32 C35 125.3(2) . . . . ?
C14 O3 C9 C8 125.92(19) . . . . ?
C14 O3 C9 C10 -58.5(3) . . . . ?
C14 C15 C16 C17 -96.1(2) . . . . ?
C14 C15 C16 C25 88.0(2) . . . . ?
C15 C16 C17 C18 6.3(3) . . . . ?
C15 C16 C17 C22 -172.54(18) . . . . ?
C15 C16 C25 C24 174.38(19) . . . . ?
C16 C17 C18 C19 -176.0(2) . . . . ?
C16 C17 C22 C21 175.15(17) . . . . ?
C16 C17 C22 C23 -2.0(3) . . . . ?
C17 C16 C25 C24 -1.7(3) . . . . ?
C17 C18 C19 C20 -0.2(3) . . . . ?
C17 C22 C23 C24 -1.1(3) . . . . ?
C17 C22 C23 C31 176.95(17) . . . . ?
C18 C17 C22 C21 -3.8(3) . . . . ?
C18 C17 C22 C23 179.10(17) . . . . ?
C18 C19 C20 C21 -1.6(3) . . . . ?
C18 C19 C20 C26 176.6(2) . . . . ?
C19 C20 C21 C22 0.7(3) . . . . ?
C19 C20 C21 C29 178.11(17) . . . . ?
C19 C20 C26 C27 -177.4(2) . . . . ?
C20 C21 C22 C17 2.1(3) . . . . ?
C20 C21 C22 C23 179.21(17) . . . . ?
C20 C21 C29 C28 -0.2(3) . . . . ?
C20 C21 C29 C30 -179.18(18) . . . . ?
C20 C26 C27 C28 -0.9(3) . . . . ?
C21 C20 C26 C27 0.8(3) . . . . ?
C21 C22 C23 C24 -178.26(18) . . . . ?
C21 C22 C23 C31 -0.2(3) . . . . ?
C21 C29 C30 C31 0.1(3) . . . . ?
C22 C17 C18 C19 2.9(3) . . . . ?
C22 C21 C29 C28 177.17(18) . . . . ?
C22 C21 C29 C30 -1.8(3) . . . . ?
C22 C23 C24 C25 2.8(3) . . . . ?
C22 C23 C31 C30 -1.5(3) . . . . ?
C23 C24 C25 C16 -1.5(3) . . . . ?
C24 C23 C31 C30 176.47(19) . . . . ?
C25 C16 C17 C18 -177.77(19) . . . . ?
C25 C16 C17 C22 3.4(3) . . . . ?
C26 C20 C21 C22 -177.64(18) . . . . ?
C26 C20 C21 C29 -0.2(3) . . . . ?
C26 C27 C28 C29 0.4(3) . . . . ?
C27 C28 C29 C21 0.1(3) . . . . ?
C27 C28 C29 C30 179.03(19) . . . . ?
C28 C29 C30 C31 -178.85(19) . . . . ?
C29 C21 C22 C17 -175.32(17) . . . . ?
C29 C21 C22 C23 1.8(3) . . . . ?
C29 C30 C31 C23 1.6(3) . . . . ?
C31 C23 C24 C25 -175.15(19) . . . . ?
C32 C12 C13 C8 177.9(2) . . . . ?
C33 C32 C35 C36 -173.2(2) . . . . ?
C34 C32 C35 C36 68.6(3) . . . . ?
O5 C37 C38 O6 -58.0(3) . . . . ?
O6 C39 C40 O5 58.4(3) . . . . ?
C37 O5 C40 C39 -58.0(2) . . . . ?
C38 O6 C39 C40 -56.5(3) . . . . ?
C39 O6 C38 C37 56.2(3) . . . . ?
C40 O5 C37 C38 58.1(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_dfya53_dcm_0m
_database_code_depnum_ccdc_archive 'CCDC 1412210'
_audit_update_record             
;
2015-07-12 deposited with the CCDC.
2015-08-17 downloaded from the CCDC.
;
_audit_creation_date             2015-04-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H54 N2 O8, 2(C H2 Cl2)'
_chemical_formula_sum            'C74 H58 Cl4 N2 O8'
_chemical_formula_weight         1245.02
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Cl Cl 0.1484 0.1585 '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'

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

_cell_length_a                   17.1824(9)
_cell_length_b                   10.3899(5)
_cell_length_c                   17.8902(9)
_cell_angle_alpha                90
_cell_angle_beta                 113.491(2)
_cell_angle_gamma                90
_cell_volume                     2929.1(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9762
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.89
_cell_measurement_theta_min      2.32
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0707 before and 0.0583 after correction.
The Ratio of minimum to maximum transmission is 0.9637.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            142111
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.900
_diffrn_reflns_theta_max         27.919
_diffrn_reflns_theta_min         2.320
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON-100 area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_special_details          ?
_reflns_number_gt                6168
_reflns_number_total             7012
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.0024(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7012
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0371
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0447P)²+1.7845P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0971
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C16A, C16B}
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1S_1) = Uanis(Cl1S_2)
Uanis(C1S_1) = Uanis(C1S_2)
Uanis(Cl2S_1) = Uanis(Cl2S_2)
Uanis(C16A) = Uanis(C16B)
Uanis(C17A) = Uanis(C17B)
Uanis(C18A) = Uanis(C18B)
Uanis(C19A) = Uanis(C19B)
Uanis(C20A) = Uanis(C20B)
Uanis(C21A) = Uanis(C21B)
Uanis(C22A) = Uanis(C22B)
Uanis(C23A) = Uanis(C23B)
Uanis(C24A) = Uanis(C24B)
Uanis(C25A) = Uanis(C25B)
Uanis(C26A) = Uanis(C26B)
Uanis(C27A) = Uanis(C27B)
Uanis(C28A) = Uanis(C28B)
Uanis(C29A) = Uanis(C29B)
Uanis(C30A) = Uanis(C30B)
Uanis(C31A) = Uanis(C31B)
4. Same fragment restrains
{C16A, C17A, C18A, C19A, C20A, C21A, C22A, C23A, C24A, C25A, C26A, C27A, C28A,
C29A, C30A, C31A} sigma for 1-2: 0.01, 1-3: 0.04
as
{C16B, C17B, C18B, C19B, C20B, C21B, C22B, C23B, C24B, C25B, C26B, C27B, C28B,
C29B, C30B, C31B}
{C1S_1, Cl2S_1, Cl1S_1} sigma for 1-2: 0.01, 1-3: 0.04
as
{C1S_2, Cl2S_2, Cl1S_2}
5. Others
 Sof(H15C)=Sof(H15D)=Sof(C16B)=Sof(C17B)=Sof(C18B)=Sof(H18B)=Sof(C19B)=
 Sof(H19B)=Sof(C20B)=Sof(C21B)=Sof(C22B)=Sof(C23B)=Sof(C24B)=Sof(H24B)=
 Sof(C25B)=Sof(H25B)=Sof(C26B)=Sof(H26B)=Sof(C27B)=Sof(H27B)=Sof(C28B)=
 Sof(H28B)=Sof(C29B)=Sof(C30B)=Sof(H30B)=Sof(C31B)=Sof(H31B)=1-FVAR(1)
 Sof(H15A)=Sof(H15B)=Sof(C16A)=Sof(C17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=
 Sof(H19A)=Sof(C20A)=Sof(C21A)=Sof(C22A)=Sof(C23A)=Sof(C24A)=Sof(H24A)=
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=
 Sof(H28A)=Sof(C29A)=Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31A)=FVAR(1)
 Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(Cl2S)=Sof(Cl1S)=1-FVAR(2)
 Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(Cl2S)=Sof(Cl1S)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C15(H15C,H15D), C35(H35A,H35B), C1S(H1SA,H1SB), C1S(H1SA,H1SB)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C18A(H18A), C19A(H19A),
 C24A(H24A), C25A(H25A), C26A(H26A), C27A(H27A), C28A(H28A), C30A(H30A),
 C31A(H31A), C18B(H18B), C19B(H19B), C24B(H24B), C25B(H25B), C26B(H26B),
 C27B(H27B), C28B(H28B), C30B(H30B), C31B(H31B)
6.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.23846(5) 0.42254(10) 0.40083(5) 0.01848(19) Uani 1 1 d . . . . .
O2 O 0.39149(6) 0.47726(10) 0.67250(5) 0.0200(2) Uani 1 1 d . . . . .
O3 O 0.19983(5) 0.63327(8) 0.51330(5) 0.01556(18) Uani 1 1 d . . . . .
O4 O 0.09042(6) 0.61474(10) 0.38992(6) 0.0227(2) Uani 1 1 d . . . . .
N1 N 0.31690(6) 0.44037(10) 0.53703(6) 0.0119(2) Uani 1 1 d . . . . .
C1 C 0.30744(7) 0.44137(11) 0.45548(7) 0.0115(2) Uani 1 1 d . . . . .
C2 C 0.38535(7) 0.46456(11) 0.44106(7) 0.0102(2) Uani 1 1 d . . . . .
C3 C 0.46298(7) 0.48996(10) 0.50745(7) 0.0092(2) Uani 1 1 d . . . . .
C4 C 0.46825(7) 0.49635(11) 0.58822(7) 0.0107(2) Uani 1 1 d . . . . .
C5 C 0.39169(7) 0.47213(11) 0.60502(7) 0.0123(2) Uani 1 1 d . . . . .
C6 C 0.38165(7) 0.45925(11) 0.36264(7) 0.0124(2) Uani 1 1 d . . . . .
H6 H 0.3291 0.4427 0.3184 0.015 Uiso 1 1 calc R U . . .
C7 C 0.54469(7) 0.52172(12) 0.65203(7) 0.0128(2) Uani 1 1 d . . . . .
H7 H 0.5476 0.5264 0.7061 0.015 Uiso 1 1 calc R U . . .
C8 C 0.24192(7) 0.41671(12) 0.55277(7) 0.0123(2) Uani 1 1 d . . . . .
C9 C 0.18252(7) 0.51352(12) 0.53871(7) 0.0129(2) Uani 1 1 d . . . . .
C10 C 0.11189(7) 0.49448(12) 0.55595(7) 0.0154(2) Uani 1 1 d . . . . .
H10 H 0.0716 0.5616 0.5469 0.018 Uiso 1 1 calc R U . . .
C11 C 0.10006(7) 0.37623(12) 0.58662(8) 0.0156(2) Uani 1 1 d . . . . .
H11 H 0.0515 0.3638 0.5987 0.019 Uiso 1 1 calc R U . . .
C12 C 0.15793(7) 0.27563(12) 0.60007(7) 0.0144(2) Uani 1 1 d . . . . .
C13 C 0.22978(7) 0.29936(12) 0.58302(7) 0.0147(2) Uani 1 1 d . . . . .
H13 H 0.2709 0.2333 0.5925 0.018 Uiso 1 1 calc R U . . .
C14 C 0.14919(7) 0.67460(13) 0.43674(8) 0.0162(2) Uani 1 1 d . . . . .
C15 C 0.17865(8) 0.80566(13) 0.42234(9) 0.0196(3) Uani 1 1 d . . . . .
H15A H 0.1848 0.8624 0.4688 0.024 Uiso 0.760(3) 1 calc R U P A 1
H15B H 0.1347 0.8436 0.3727 0.024 Uiso 0.760(3) 1 calc R U P A 1
H15C H 0.1848 0.8624 0.4688 0.024 Uiso 0.240(3) 1 calc R U P A 2
H15D H 0.1347 0.8436 0.3727 0.024 Uiso 0.240(3) 1 calc R U P A 2
C16A C 0.26244(8) 0.80173(12) 0.41238(8) 0.0167(2) Uani 0.760(3) 1 d D . P A 1
C17A C 0.3426(2) 0.815(2) 0.4768(2) 0.0156(4) Uani 0.760(3) 1 d D . P A 1
C18A C 0.35526(17) 0.8262(7) 0.5607(2) 0.0191(6) Uani 0.760(3) 1 d D . P A 1
H18A H 0.3076 0.8226 0.5749 0.023 Uiso 0.760(3) 1 calc R U P A 1
C19A C 0.43388(15) 0.8422(3) 0.62037(16) 0.0226(5) Uani 0.760(3) 1 d D . P A 1
H19A H 0.4400 0.8491 0.6754 0.027 Uiso 0.760(3) 1 calc R U P A 1
C20A C 0.50773(13) 0.8488(2) 0.60221(14) 0.0208(5) Uani 0.760(3) 1 d D . P A 1
C21A C 0.49772(13) 0.8358(2) 0.52011(14) 0.0183(5) Uani 0.760(3) 1 d D . P A 1
C22A C 0.41525(17) 0.8173(4) 0.45681(13) 0.0162(5) Uani 0.760(3) 1 d D . P A 1
C23A C 0.40635(14) 0.8054(3) 0.37497(14) 0.0172(5) Uani 0.760(3) 1 d D . P A 1
C24A C 0.32551(14) 0.7908(3) 0.31320(14) 0.0187(5) Uani 0.760(3) 1 d D . P A 1
H24A H 0.3190 0.7812 0.2582 0.022 Uiso 0.760(3) 1 calc R U P A 1
C25A C 0.25444(14) 0.7904(5) 0.33215(15) 0.0183(5) Uani 0.760(3) 1 d D . P A 1
H25A H 0.1996 0.7824 0.2896 0.022 Uiso 0.760(3) 1 calc R U P A 1
C26A C 0.58907(13) 0.8709(2) 0.66290(15) 0.0290(5) Uani 0.760(3) 1 d D . P A 1
H26A H 0.5964 0.8806 0.7181 0.035 Uiso 0.760(3) 1 calc R U P A 1
C27A C 0.65880(13) 0.8786(2) 0.64214(19) 0.0326(7) Uani 0.760(3) 1 d D . P A 1
H27A H 0.7136 0.8927 0.6837 0.039 Uiso 0.760(3) 1 calc R U P A 1
C28A C 0.64998(12) 0.86605(19) 0.56257(19) 0.0306(6) Uani 0.760(3) 1 d D . P A
1
H28A H 0.6986 0.8718 0.5500 0.037 Uiso 0.760(3) 1 calc R U P A 1
C29A C 0.57004(12) 0.84488(19) 0.49976(18) 0.0224(5) Uani 0.760(3) 1 d D . P A
1
C30A C 0.55800(14) 0.83394(19) 0.41651(19) 0.0259(5) Uani 0.760(3) 1 d D . P A
1
H30A H 0.6057 0.8412 0.4026 0.031 Uiso 0.760(3) 1 calc R U P A 1
C31A C 0.48107(15) 0.8137(2) 0.35733(16) 0.0248(5) Uani 0.760(3) 1 d D . P A 1
H31A H 0.4757 0.8047 0.3026 0.030 Uiso 0.760(3) 1 calc R U P A 1
C16B C 0.26244(8) 0.80173(12) 0.41238(8) 0.0167(2) Uani 0.240(3) 1 d D . P A 2
C17B C 0.3393(6) 0.814(7) 0.4833(7) 0.0156(4) Uani 0.240(3) 1 d D . P A 2
C18B C 0.3406(7) 0.831(2) 0.5638(7) 0.0191(6) Uani 0.240(3) 1 d D . P A 2
H18B H 0.2888 0.8271 0.5708 0.023 Uiso 0.240(3) 1 calc R U P A 2
C19B C 0.4140(5) 0.8542(11) 0.6299(6) 0.0226(5) Uani 0.240(3) 1 d D . P A 2
H19B H 0.4114 0.8660 0.6815 0.027 Uiso 0.240(3) 1 calc R U P A 2
C20B C 0.4937(4) 0.8606(8) 0.6246(5) 0.0208(5) Uani 0.240(3) 1 d D . P A 2
C21B C 0.4973(5) 0.8441(9) 0.5480(5) 0.0183(5) Uani 0.240(3) 1 d D . P A 2
C22B C 0.4206(6) 0.8182(17) 0.4776(5) 0.0162(5) Uani 0.240(3) 1 d D . P A 2
C23B C 0.4246(5) 0.8051(11) 0.4009(5) 0.0172(5) Uani 0.240(3) 1 d D . P A 2
C24B C 0.3514(5) 0.7863(10) 0.3338(5) 0.0187(5) Uani 0.240(3) 1 d D . P A 2
H24B H 0.3539 0.7750 0.2821 0.022 Uiso 0.240(3) 1 calc R U P A 2
C25B C 0.2733(6) 0.7835(19) 0.3395(5) 0.0183(5) Uani 0.240(3) 1 d D . P A 2
H25B H 0.2242 0.7682 0.2912 0.022 Uiso 0.240(3) 1 calc R U P A 2
C26B C 0.5712(4) 0.8861(7) 0.6918(5) 0.0290(5) Uani 0.240(3) 1 d D . P A 2
H26B H 0.5718 0.8960 0.7449 0.035 Uiso 0.240(3) 1 calc R U P A 2
C27B C 0.6463(4) 0.8966(7) 0.6800(5) 0.0326(7) Uani 0.240(3) 1 d D . P A 2
H27B H 0.6974 0.9152 0.7257 0.039 Uiso 0.240(3) 1 calc R U P A 2
C28B C 0.6495(5) 0.8814(9) 0.6053(6) 0.0306(6) Uani 0.240(3) 1 d D . P A 2
H28B H 0.7020 0.8890 0.5997 0.037 Uiso 0.240(3) 1 calc R U P A 2
C29B C 0.5750(4) 0.8545(7) 0.5371(5) 0.0224(5) Uani 0.240(3) 1 d D . P A 2
C30B C 0.5746(5) 0.8400(7) 0.4584(6) 0.0259(5) Uani 0.240(3) 1 d D . P A 2
H30B H 0.6268 0.8489 0.4523 0.031 Uiso 0.240(3) 1 calc R U P A 2
C31B C 0.5051(5) 0.8148(8) 0.3928(5) 0.0248(5) Uani 0.240(3) 1 d D . P A 2
H31B H 0.5079 0.8033 0.3413 0.030 Uiso 0.240(3) 1 calc R U P A 2
C32 C 0.14735(8) 0.14429(12) 0.63419(8) 0.0178(3) Uani 1 1 d . . . . .
C33 C 0.06239(9) 0.13284(14) 0.64300(9) 0.0248(3) Uani 1 1 d . . . . .
H33A H 0.0585 0.2005 0.6795 0.037 Uiso 1 1 calc R U . . .
H33B H 0.0587 0.0483 0.6657 0.037 Uiso 1 1 calc R U . . .
H33C H 0.0157 0.1424 0.5894 0.037 Uiso 1 1 calc R U . . .
C34 C 0.15091(10) 0.03675(14) 0.57666(10) 0.0282(3) Uani 1 1 d . . . . .
H34A H 0.1051 0.0490 0.5228 0.042 Uiso 1 1 calc R U . . .
H34B H 0.1442 -0.0469 0.5987 0.042 Uiso 1 1 calc R U . . .
H34C H 0.2057 0.0396 0.5718 0.042 Uiso 1 1 calc R U . . .
C35 C 0.22132(9) 0.12303(14) 0.71826(9) 0.0237(3) Uani 1 1 d . . . . .
H35A H 0.2134 0.0386 0.7399 0.028 Uiso 1 1 calc R U . . .
H35B H 0.2751 0.1191 0.7103 0.028 Uiso 1 1 calc R U . . .
C36 C 0.22964(11) 0.22512(17) 0.78101(9) 0.0337(4) Uani 1 1 d . . . . .
H36A H 0.2363 0.3096 0.7599 0.050 Uiso 1 1 calc R U . . .
H36B H 0.2794 0.2068 0.8311 0.050 Uiso 1 1 calc R U . . .
H36C H 0.1786 0.2253 0.7928 0.050 Uiso 1 1 calc R U . . .
C1S_1 C 0.43202(11) 0.7836(2) 0.12585(13) 0.0261(5) Uani 0.861(3) 1 d D . P B 1
H1SA_1 H 0.4161 0.7967 0.0668 0.031 Uiso 0.861(3) 1 calc R U P B 1
H1SB_1 H 0.4109 0.8581 0.1468 0.031 Uiso 0.861(3) 1 calc R U P B 1
Cl2S_1 Cl 0.54342(3) 0.77581(13) 0.17595(5) 0.0386(2) Uani 0.861(3) 1 d D . P B
1
Cl1S_1 Cl 0.38365(6) 0.64047(10) 0.14112(7) 0.02654(16) Uani 0.861(3) 1 d D . P
B 1
C1S_2 C 0.4319(6) 0.8170(11) 0.1418(11) 0.0261(5) Uani 0.139(3) 1 d D . P B 2
H1SA_2 H 0.4145 0.8430 0.0842 0.031 Uiso 0.139(3) 1 calc R U P B 2
H1SB_2 H 0.4043 0.8758 0.1675 0.031 Uiso 0.139(3) 1 calc R U P B 2
Cl2S_2 Cl 0.5429(2) 0.8280(7) 0.1930(3) 0.0386(2) Uani 0.139(3) 1 d D . P B 2
Cl1S_2 Cl 0.3990(5) 0.6566(8) 0.1466(5) 0.02654(16) Uani 0.139(3) 1 d D . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.2145(15) . ?
O2 C5 1.2098(15) . ?
O3 C9 1.3968(14) . ?
O3 C14 1.3666(15) . ?
O4 C14 1.1974(16) . ?
N1 C1 1.4022(15) . ?
N1 C5 1.4120(15) . ?
N1 C8 1.4453(14) . ?
C1 C2 1.4805(15) . ?
C2 C3 1.4129(15) . ?
C2 C6 1.3800(16) . ?
C3 C3 1.415(2) 3_666 ?
C3 C4 1.4129(15) . ?
C4 C5 1.4831(15) . ?
C4 C7 1.3793(16) . ?
C6 H6 0.9500 . ?
C6 C7 1.4052(16) 3_666 ?
C7 C6 1.4052(16) 3_666 ?
C7 H7 0.9500 . ?
C8 C9 1.3827(17) . ?
C8 C13 1.3831(17) . ?
C9 C10 1.3803(16) . ?
C10 H10 0.9500 . ?
C10 C11 1.3931(18) . ?
C11 H11 0.9500 . ?
C11 C12 1.3959(17) . ?
C12 C13 1.4065(16) . ?
C12 C32 1.5350(17) . ?
C13 H13 0.9500 . ?
C14 C15 1.5102(18) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 H15C 0.9900 . ?
C15 H15D 0.9900 . ?
C15 C16A 1.5201(17) . ?
C15 C16B 1.5201(17) . ?
C16A C17A 1.406(3) . ?
C16A C25A 1.391(3) . ?
C17A C18A 1.434(3) . ?
C17A C22A 1.429(3) . ?
C18A H18A 0.9500 . ?
C18A C19A 1.357(3) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.431(3) . ?
C20A C21A 1.416(3) . ?
C20A C26A 1.405(3) . ?
C21A C22A 1.431(3) . ?
C21A C29A 1.431(3) . ?
C22A C23A 1.416(3) . ?
C23A C24A 1.396(3) . ?
C23A C31A 1.442(3) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.392(3) . ?
C25A H25A 0.9500 . ?
C26A H26A 0.9500 . ?
C26A C27A 1.391(4) . ?
C27A H27A 0.9500 . ?
C27A C28A 1.376(4) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.402(3) . ?
C29A C30A 1.424(3) . ?
C30A H30A 0.9500 . ?
C30A C31A 1.340(3) . ?
C31A H31A 0.9500 . ?
C16B C17B 1.427(7) . ?
C16B C25B 1.401(8) . ?
C17B C18B 1.441(8) . ?
C17B C22B 1.441(8) . ?
C18B H18B 0.9500 . ?
C18B C19B 1.362(8) . ?
C19B H19B 0.9500 . ?
C19B C20B 1.412(7) . ?
C20B C21B 1.406(7) . ?
C20B C26B 1.419(7) . ?
C21B C22B 1.440(8) . ?
C21B C29B 1.427(7) . ?
C22B C23B 1.408(7) . ?
C23B C24B 1.364(7) . ?
C23B C31B 1.451(8) . ?
C24B H24B 0.9500 . ?
C24B C25B 1.386(8) . ?
C25B H25B 0.9500 . ?
C26B H26B 0.9500 . ?
C26B C27B 1.393(8) . ?
C27B H27B 0.9500 . ?
C27B C28B 1.369(9) . ?
C28B H28B 0.9500 . ?
C28B C29B 1.399(8) . ?
C29B C30B 1.413(8) . ?
C30B H30B 0.9500 . ?
C30B C31B 1.325(8) . ?
C31B H31B 0.9500 . ?
C32 C33 1.5341(17) . ?
C32 C34 1.5367(19) . ?
C32 C35 1.5499(19) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.509(2) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C1S_1 H1SA_1 0.9900 . ?
C1S_1 H1SB_1 0.9900 . ?
C1S_1 Cl2S_1 1.7623(18) . ?
C1S_1 Cl1S_1 1.777(2) . ?
C1S_2 H1SA_2 0.9900 . ?
C1S_2 H1SB_2 0.9900 . ?
C1S_2 Cl2S_2 1.760(9) . ?
C1S_2 Cl1S_2 1.772(9) . ?

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
C14 O3 C9 118.23(10) . . ?
C1 N1 C5 125.65(9) . . ?
C1 N1 C8 117.48(9) . . ?
C5 N1 C8 116.60(9) . . ?
O1 C1 N1 120.50(10) . . ?
O1 C1 C2 123.10(11) . . ?
N1 C1 C2 116.40(10) . . ?
C3 C2 C1 120.01(10) . . ?
C6 C2 C1 119.48(10) . . ?
C6 C2 C3 120.51(10) . . ?
C2 C3 C3 119.17(13) . 3_666 ?
C4 C3 C2 121.51(10) . . ?
C4 C3 C3 119.32(13) . 3_666 ?
C3 C4 C5 119.92(10) . . ?
C7 C4 C3 120.47(10) . . ?
C7 C4 C5 119.58(10) . . ?
O2 C5 N1 120.42(10) . . ?
O2 C5 C4 123.39(11) . . ?
N1 C5 C4 116.19(10) . . ?
C2 C6 H6 119.9 . . ?
C2 C6 C7 120.29(10) . 3_666 ?
C7 C6 H6 119.9 3_666 . ?
C4 C7 C6 120.24(10) . 3_666 ?
C4 C7 H7 119.9 . . ?
C6 C7 H7 119.9 3_666 . ?
C9 C8 N1 119.44(11) . . ?
C9 C8 C13 119.80(10) . . ?
C13 C8 N1 120.75(10) . . ?
C8 C9 O3 118.02(10) . . ?
C10 C9 O3 121.37(11) . . ?
C10 C9 C8 120.40(11) . . ?
C9 C10 H10 120.2 . . ?
C9 C10 C11 119.59(11) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 H11 119.3 . . ?
C10 C11 C12 121.50(11) . . ?
C12 C11 H11 119.3 . . ?
C11 C12 C13 117.26(11) . . ?
C11 C12 C32 123.03(11) . . ?
C13 C12 C32 119.70(11) . . ?
C8 C13 C12 121.44(11) . . ?
C8 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
O3 C14 C15 109.36(11) . . ?
O4 C14 O3 124.08(12) . . ?
O4 C14 C15 126.55(12) . . ?
C14 C15 H15A 108.9 . . ?
C14 C15 H15B 108.9 . . ?
C14 C15 H15C 108.9 . . ?
C14 C15 H15D 108.9 . . ?
C14 C15 C16A 113.16(10) . . ?
C14 C15 C16B 113.16(10) . . ?
H15A C15 H15B 107.8 . . ?
H15C C15 H15D 107.8 . . ?
C16A C15 H15A 108.9 . . ?
C16A C15 H15B 108.9 . . ?
C16B C15 H15C 108.9 . . ?
C16B C15 H15D 108.9 . . ?
C17A C16A C15 124.45(18) . . ?
C25A C16A C15 114.49(14) . . ?
C25A C16A C17A 121.00(19) . . ?
C16A C17A C18A 123.8(3) . . ?
C16A C17A C22A 117.7(2) . . ?
C22A C17A C18A 118.5(2) . . ?
C17A C18A H18A 119.3 . . ?
C19A C18A C17A 121.5(2) . . ?
C19A C18A H18A 119.3 . . ?
C18A C19A H19A 119.3 . . ?
C18A C19A C20A 121.5(2) . . ?
C20A C19A H19A 119.3 . . ?
C21A C20A C19A 118.60(18) . . ?
C26A C20A C19A 122.1(2) . . ?
C26A C20A C21A 119.3(2) . . ?
C20A C21A C22A 120.43(18) . . ?
C20A C21A C29A 119.94(19) . . ?
C29A C21A C22A 119.6(2) . . ?
C17A C22A C21A 119.55(19) . . ?
C23A C22A C17A 120.8(2) . . ?
C23A C22A C21A 119.7(2) . . ?
C22A C23A C31A 118.85(19) . . ?
C24A C23A C22A 119.4(2) . . ?
C24A C23A C31A 121.7(2) . . ?
C23A C24A H24A 120.0 . . ?
C25A C24A C23A 120.0(2) . . ?
C25A C24A H24A 120.0 . . ?
C16A C25A C24A 121.0(2) . . ?
C16A C25A H25A 119.5 . . ?
C24A C25A H25A 119.5 . . ?
C20A C26A H26A 120.0 . . ?
C27A C26A C20A 120.0(2) . . ?
C27A C26A H26A 120.0 . . ?
C26A C27A H27A 119.4 . . ?
C28A C27A C26A 121.29(19) . . ?
C28A C27A H27A 119.4 . . ?
C27A C28A H28A 119.6 . . ?
C27A C28A C29A 120.8(2) . . ?
C29A C28A H28A 119.6 . . ?
C28A C29A C21A 118.6(2) . . ?
C28A C29A C30A 122.6(2) . . ?
C30A C29A C21A 118.81(17) . . ?
C29A C30A H30A 119.2 . . ?
C31A C30A C29A 121.67(18) . . ?
C31A C30A H30A 119.2 . . ?
C23A C31A H31A 119.3 . . ?
C30A C31A C23A 121.4(2) . . ?
C30A C31A H31A 119.3 . . ?
C17B C16B C15 118.5(5) . . ?
C25B C16B C15 126.6(4) . . ?
C25B C16B C17B 114.8(7) . . ?
C16B C17B C18B 122.7(9) . . ?
C16B C17B C22B 121.3(8) . . ?
C22B C17B C18B 115.9(8) . . ?
C17B C18B H18B 119.0 . . ?
C19B C18B C17B 122.0(10) . . ?
C19B C18B H18B 119.0 . . ?
C18B C19B H19B 118.8 . . ?
C18B C19B C20B 122.4(9) . . ?
C20B C19B H19B 118.8 . . ?
C19B C20B C26B 124.0(7) . . ?
C21B C20B C19B 118.8(7) . . ?
C21B C20B C26B 117.2(7) . . ?
C20B C21B C22B 119.6(7) . . ?
C20B C21B C29B 122.0(7) . . ?
C29B C21B C22B 118.4(7) . . ?
C21B C22B C17B 121.3(8) . . ?
C23B C22B C17B 119.5(8) . . ?
C23B C22B C21B 119.1(8) . . ?
C22B C23B C31B 120.7(7) . . ?
C24B C23B C22B 119.0(7) . . ?
C24B C23B C31B 120.3(7) . . ?
C23B C24B H24B 119.4 . . ?
C23B C24B C25B 121.3(9) . . ?
C25B C24B H24B 119.4 . . ?
C16B C25B H25B 118.1 . . ?
C24B C25B C16B 123.9(9) . . ?
C24B C25B H25B 118.1 . . ?
C20B C26B H26B 120.0 . . ?
C27B C26B C20B 119.9(7) . . ?
C27B C26B H26B 120.0 . . ?
C26B C27B H27B 118.7 . . ?
C28B C27B C26B 122.6(7) . . ?
C28B C27B H27B 118.7 . . ?
C27B C28B H28B 120.2 . . ?
C27B C28B C29B 119.7(8) . . ?
C29B C28B H28B 120.2 . . ?
C28B C29B C21B 118.5(7) . . ?
C28B C29B C30B 121.9(7) . . ?
C30B C29B C21B 119.6(6) . . ?
C29B C30B H30B 118.4 . . ?
C31B C30B C29B 123.3(7) . . ?
C31B C30B H30B 118.4 . . ?
C23B C31B H31B 120.5 . . ?
C30B C31B C23B 118.9(7) . . ?
C30B C31B H31B 120.5 . . ?
C12 C32 C34 109.72(10) . . ?
C12 C32 C35 109.34(10) . . ?
C33 C32 C12 112.22(11) . . ?
C33 C32 C34 107.82(11) . . ?
C33 C32 C35 109.57(11) . . ?
C34 C32 C35 108.07(11) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 108.6 . . ?
C32 C35 H35B 108.6 . . ?
H35A C35 H35B 107.5 . . ?
C36 C35 C32 114.81(12) . . ?
C36 C35 H35A 108.6 . . ?
C36 C35 H35B 108.6 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
H1SA_1 C1S_1 H1SB_1 108.0 . . ?
Cl2S_1 C1S_1 H1SA_1 109.4 . . ?
Cl2S_1 C1S_1 H1SB_1 109.4 . . ?
Cl2S_1 C1S_1 Cl1S_1 111.29(11) . . ?
Cl1S_1 C1S_1 H1SA_1 109.4 . . ?
Cl1S_1 C1S_1 H1SB_1 109.4 . . ?
H1SA_2 C1S_2 H1SB_2 108.2 . . ?
Cl2S_2 C1S_2 H1SA_2 109.7 . . ?
Cl2S_2 C1S_2 H1SB_2 109.7 . . ?
Cl2S_2 C1S_2 Cl1S_2 109.6(6) . . ?
Cl1S_2 C1S_2 H1SA_2 109.7 . . ?
Cl1S_2 C1S_2 H1SB_2 109.7 . . ?

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
O1 C1 C2 C3 177.92(11) . . . . ?
O1 C1 C2 C6 -3.03(18) . . . . ?
O3 C9 C10 C11 -175.48(11) . . . . ?
O3 C14 C15 C16A 71.46(14) . . . . ?
O3 C14 C15 C16B 71.46(14) . . . . ?
O4 C14 C15 C16A -109.29(15) . . . . ?
O4 C14 C15 C16B -109.29(15) . . . . ?
N1 C1 C2 C3 -2.87(16) . . . . ?
N1 C1 C2 C6 176.18(10) . . . . ?
N1 C8 C9 O3 -3.02(17) . . . . ?
N1 C8 C9 C10 -177.79(11) . . . . ?
N1 C8 C13 C12 178.81(11) . . . . ?
C1 N1 C5 O2 174.61(11) . . . . ?
C1 N1 C5 C4 -6.10(17) . . . . ?
C1 N1 C8 C9 -75.58(14) . . . . ?
C1 N1 C8 C13 105.57(13) . . . . ?
C1 C2 C3 C3 179.09(12) . . . 3_666 ?
C1 C2 C3 C4 -1.21(16) . . . . ?
C1 C2 C6 C7 -178.64(11) . . . 3_666 ?
C2 C3 C4 C5 1.90(17) . . . . ?
C2 C3 C4 C7 -179.78(11) . . . . ?
C3 C2 C6 C7 0.41(17) . . . 3_666 ?
C3 C3 C4 C5 -178.39(12) 3_666 . . . ?
C3 C3 C4 C7 -0.1(2) 3_666 . . . ?
C3 C4 C5 O2 -179.25(11) . . . . ?
C3 C4 C5 N1 1.49(16) . . . . ?
C3 C4 C7 C6 -0.39(18) . . . 3_666 ?
C5 N1 C1 O1 -173.99(11) . . . . ?
C5 N1 C1 C2 6.77(17) . . . . ?
C5 N1 C8 C9 98.78(13) . . . . ?
C5 N1 C8 C13 -80.06(14) . . . . ?
C5 C4 C7 C6 177.94(11) . . . 3_666 ?
C6 C2 C3 C3 0.05(19) . . . 3_666 ?
C6 C2 C3 C4 179.76(11) . . . . ?
C7 C4 C5 O2 2.41(18) . . . . ?
C7 C4 C5 N1 -176.85(11) . . . . ?
C8 N1 C1 O1 -0.19(17) . . . . ?
C8 N1 C1 C2 -179.43(10) . . . . ?
C8 N1 C5 O2 0.77(17) . . . . ?
C8 N1 C5 C4 -179.94(10) . . . . ?
C8 C9 C10 C11 -0.89(18) . . . . ?
C9 O3 C14 O4 0.34(18) . . . . ?
C9 O3 C14 C15 179.61(10) . . . . ?
C9 C8 C13 C12 -0.03(18) . . . . ?
C9 C10 C11 C12 -0.34(19) . . . . ?
C10 C11 C12 C13 1.33(18) . . . . ?
C10 C11 C12 C32 179.67(12) . . . . ?
C11 C12 C13 C8 -1.14(18) . . . . ?
C11 C12 C32 C33 5.89(18) . . . . ?
C11 C12 C32 C34 125.73(13) . . . . ?
C11 C12 C32 C35 -115.91(13) . . . . ?
C12 C32 C35 C36 57.59(15) . . . . ?
C13 C8 C9 O3 175.84(11) . . . . ?
C13 C8 C9 C10 1.07(18) . . . . ?
C13 C12 C32 C33 -175.80(12) . . . . ?
C13 C12 C32 C34 -55.96(16) . . . . ?
C13 C12 C32 C35 62.40(15) . . . . ?
C14 O3 C9 C8 114.10(12) . . . . ?
C14 O3 C9 C10 -71.19(15) . . . . ?
C14 C15 C16A C17A -90.6(11) . . . . ?
C14 C15 C16A C25A 92.4(3) . . . . ?
C14 C15 C16B C17B -90(3) . . . . ?
C14 C15 C16B C25B 88.4(10) . . . . ?
C15 C16A C17A C18A 3(2) . . . . ?
C15 C16A C17A C22A -175.9(9) . . . . ?
C15 C16A C25A C24A 177.4(3) . . . . ?
C15 C16B C17B C18B -1(7) . . . . ?
C15 C16B C17B C22B -177(4) . . . . ?
C15 C16B C25B C24B 177.1(11) . . . . ?
C16A C17A C18A C19A -178.0(12) . . . . ?
C16A C17A C22A C21A 177.3(10) . . . . ?
C16A C17A C22A C23A -1(2) . . . . ?
C17A C16A C25A C24A 0.3(12) . . . . ?
C17A C18A C19A C20A 0.4(13) . . . . ?
C17A C22A C23A C24A 0.0(12) . . . . ?
C17A C22A C23A C31A 177.6(11) . . . . ?
C18A C17A C22A C21A -2(2) . . . . ?
C18A C17A C22A C23A 179.6(11) . . . . ?
C18A C19A C20A C21A -1.3(5) . . . . ?
C18A C19A C20A C26A 177.2(4) . . . . ?
C19A C20A C21A C22A 0.5(4) . . . . ?
C19A C20A C21A C29A 178.6(2) . . . . ?
C19A C20A C26A C27A -179.0(2) . . . . ?
C20A C21A C22A C17A 1.2(11) . . . . ?
C20A C21A C22A C23A 179.5(3) . . . . ?
C20A C21A C29A C28A 0.4(3) . . . . ?
C20A C21A C29A C30A -178.76(19) . . . . ?
C20A C26A C27A C28A 0.6(3) . . . . ?
C21A C20A C26A C27A -0.6(3) . . . . ?
C21A C22A C23A C24A -178.3(3) . . . . ?
C21A C22A C23A C31A -0.7(5) . . . . ?
C21A C29A C30A C31A -0.9(3) . . . . ?
C22A C17A C18A C19A 1(2) . . . . ?
C22A C21A C29A C28A 178.5(3) . . . . ?
C22A C21A C29A C30A -0.6(4) . . . . ?
C22A C23A C24A C25A 1.2(5) . . . . ?
C22A C23A C31A C30A -0.8(4) . . . . ?
C23A C24A C25A C16A -1.4(6) . . . . ?
C24A C23A C31A C30A 176.7(2) . . . . ?
C25A C16A C17A C18A -179.8(12) . . . . ?
C25A C16A C17A C22A 1(2) . . . . ?
C26A C20A C21A C22A -178.0(3) . . . . ?
C26A C20A C21A C29A 0.1(3) . . . . ?
C26A C27A C28A C29A -0.1(3) . . . . ?
C27A C28A C29A C21A -0.4(3) . . . . ?
C27A C28A C29A C30A 178.73(19) . . . . ?
C28A C29A C30A C31A -180.0(2) . . . . ?
C29A C21A C22A C17A -176.9(11) . . . . ?
C29A C21A C22A C23A 1.4(5) . . . . ?
C29A C30A C31A C23A 1.6(3) . . . . ?
C31A C23A C24A C25A -176.3(3) . . . . ?
C16B C17B C18B C19B -174(4) . . . . ?
C16B C17B C22B C21B 173(4) . . . . ?
C16B C17B C22B C23B -2(7) . . . . ?
C17B C16B C25B C24B -5(4) . . . . ?
C17B C18B C19B C20B -1(4) . . . . ?
C17B C22B C23B C24B -1(4) . . . . ?
C17B C22B C23B C31B 177(3) . . . . ?
C18B C17B C22B C21B -3(7) . . . . ?
C18B C17B C22B C23B -178(3) . . . . ?
C18B C19B C20B C21B 1(2) . . . . ?
C18B C19B C20B C26B 178.9(15) . . . . ?
C19B C20B C21B C22B -1.4(15) . . . . ?
C19B C20B C21B C29B 177.4(8) . . . . ?
C19B C20B C26B C27B -177.0(8) . . . . ?
C20B C21B C22B C17B 3(4) . . . . ?
C20B C21B C22B C23B 178.4(11) . . . . ?
C20B C21B C29B C28B 0.3(13) . . . . ?
C20B C21B C29B C30B -178.4(8) . . . . ?
C20B C26B C27B C28B -1.0(12) . . . . ?
C21B C20B C26B C27B 1.4(12) . . . . ?
C21B C22B C23B C24B -177.1(12) . . . . ?
C21B C22B C23B C31B 1(2) . . . . ?
C21B C29B C30B C31B -1.2(13) . . . . ?
C22B C17B C18B C19B 2(7) . . . . ?
C22B C21B C29B C28B 179.1(11) . . . . ?
C22B C21B C29B C30B 0.4(14) . . . . ?
C22B C23B C24B C25B 2(2) . . . . ?
C22B C23B C31B C30B -1.9(16) . . . . ?
C23B C24B C25B C16B 1(2) . . . . ?
C24B C23B C31B C30B 176.4(10) . . . . ?
C25B C16B C17B C18B -179(4) . . . . ?
C25B C16B C17B C22B 5(7) . . . . ?
C26B C20B C21B C22B -179.9(10) . . . . ?
C26B C20B C21B C29B -1.1(13) . . . . ?
C26B C27B C28B C29B 0.2(13) . . . . ?
C27B C28B C29B C21B 0.2(13) . . . . ?
C27B C28B C29B C30B 178.9(8) . . . . ?
C28B C29B C30B C31B -179.9(8) . . . . ?
C29B C21B C22B C17B -176(4) . . . . ?
C29B C21B C22B C23B -0.5(19) . . . . ?
C29B C30B C31B C23B 1.9(13) . . . . ?
C31B C23B C24B C25B -176.6(13) . . . . ?
C32 C12 C13 C8 -179.55(11) . . . . ?
C33 C32 C35 C36 -65.80(15) . . . . ?
C34 C32 C35 C36 176.97(12) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_twin5a
_database_code_depnum_ccdc_archive 'CCDC 1412211'
_audit_update_record             
;
2015-07-12 deposited with the CCDC.
2015-08-17 downloaded from the CCDC.
;
_audit_creation_date             2015-03-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H54 N2 O8, 2(C2 H5 N O2)'
_chemical_formula_sum            'C76 H64 N4 O12'
_chemical_formula_weight         1225.31
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'

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

_cell_length_a                   10.3369(14)
_cell_length_b                   17.1080(18)
_cell_length_c                   18.463(2)
_cell_angle_alpha                115.858(3)
_cell_angle_beta                 90.538(4)
_cell_angle_gamma                92.053(4)
_cell_volume                     2935.1(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9437
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.382
_cell_measurement_theta_min      2.352
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.862013
_exptl_absorpt_correction_T_min  0.506782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1463 before and 0.1182 after correction.
 The Ratio of minimum to maximum transmission is 0.5879.
 The λ/2 correction factor is Not present
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9684
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        24.300
_diffrn_reflns_theta_max         24.407
_diffrn_reflns_theta_min         2.221
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON-100 area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_special_details          ?
_diffrn_standards_number         ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7851
_reflns_number_total             9684
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.0042(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         9684
_refine_ls_number_restraints     129
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0765
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1103P)²+3.5961P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1916
_refine_ls_wR_factor_ref         0.2059
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5220(19) 0.4780(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Shared sites
{C32B, C32D}
{C32A, C32C}
4. Restrained distances
 H11A-H35A
 2.1 with sigma of 0.015
 C32B-C33B \\sim C32B-C34B \\sim C32B-C35B \\sim C32D-C33D \\sim C32D-C34D
\\sim C32D-C35D
 with sigma of 0.015
 C35B-C36B \\sim C35D-C36D
 with sigma of 0.015
 C32B-C36B \\sim C32D-C36D
 with sigma of 0.015
 C33B-C34B \\sim C34B-C35B \\sim C35B-C33B \\sim C33D-C34D \\sim C34D-C35D
\\sim C35D-C33D
 with sigma of 0.02
 C32A-C35C \\sim C32A-C33C \\sim C32A-C35A \\sim C32C-C33A \\sim C32C-C34A
\\sim C32C-C34C
 with sigma of 0.015
 C35C-C33C \\sim C33C-C35A \\sim C35A-C35C \\sim C33A-C34A \\sim C34A-C34C
\\sim C34C-C33A
 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
Uanis(C8A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uiso(C35B) = Uiso(C35D)
Uiso(C36B) = Uiso(C36D)
Uiso(C32B) = Uiso(C32D)
Uiso(C34B) = Uiso(C34D)
Uiso(C33B) = Uiso(C33D)
Uiso(C32A) = Uiso(C32C)
Uiso(C35A) = Uiso(C34C)
Uiso(C34A) = Uiso(C33C)
6. Rigid body (RIGU) restrains
 C13B, C8B, C9B, N1B, C5B, C4B, C1B, C2B, C3B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7. Others
 Sof(C32D)=Sof(C33D)=Sof(H33J)=Sof(H33K)=Sof(H33L)=Sof(C34D)=Sof(H34J)=
 Sof(H34K)=Sof(H34L)=Sof(C35D)=Sof(H35G)=Sof(H35H)=Sof(C36D)=Sof(H36J)=
 Sof(H36K)=Sof(H36L)=1-FVAR(1)
 Sof(C32B)=Sof(C33B)=Sof(H33G)=Sof(H33H)=Sof(H33I)=Sof(C34B)=Sof(H34G)=
 Sof(H34H)=Sof(H34I)=Sof(C35B)=Sof(H35E)=Sof(H35F)=Sof(C36B)=Sof(H36G)=
 Sof(H36H)=Sof(H36I)=FVAR(1)
 Sof(C32C)=Sof(C33C)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34C)=Sof(H34D)=
 Sof(H34E)=Sof(H34F)=Sof(C35C)=Sof(H35C)=Sof(H35D)=Sof(C36C)=Sof(H36D)=
 Sof(H36E)=Sof(H36F)=1-FVAR(2)
 Sof(C32A)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34A)=Sof(H34A)=
 Sof(H34B)=Sof(H34C)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(C36A)=Sof(H36A)=
 Sof(H36B)=Sof(H36C)=FVAR(2)
8.a Secondary CH2 refined with riding coordinates:
 C15A(H15A,H15B), C35A(H35A,H35B), C35C(H35C,H35D), C15B(H15C,H15D), C35B(H35E,
 H35F), C35D(H35G,H35H), C3S(H3SA,H3SB), C1S(H1SA,H1SB)
8.b Aromatic/amide H refined with riding coordinates:
 C6A(H6A), C7A(H7A), C10A(H10A), C11A(H11A), C13A(H13A), C18A(H18A),
 C19A(H19A), C24A(H24A), C25A(H25A), C26A(H26A), C27A(H27A), C28A(H28A),
 C30A(H30A), C31A(H31A), C6B(H6B), C7B(H7B), C10B(H10B), C11B(H11B), C13B(H13B),
  C18B(H18B), C19B(H19B), C24B(H24B), C25B(H25B), C26B(H26B), C27B(H27B),
 C28B(H28B), C30B(H30B), C31B(H31B)
8.c Idealised Me refined with riding coordinates:
 C33A(H33A,H33B,H33C), C34A(H34A,H34B,H34C), C36A(H36A,H36B,H36C), C33C(H33D,
 H33E,H33F), C34C(H34D,H34E,H34F), C36C(H36D,H36E,H36F), C33B(H33G,H33H,H33I),
 C34B(H34G,H34H,H34I), C36B(H36G,H36H,H36I), C33D(H33J,H33K,H33L), C34D(H34J,
 H34K,H34L), C36D(H36J,H36K,H36L)
8.d Idealised Me refined as rotating group:
 C4S(H4SA,H4SB,H4SC), C2S(H2SA,H2SB,H2SC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1A C 0.0561(5) 0.1928(3) 0.0300(3) 0.0152(10) Uani 1 1 d . . . . .
C2A C 0.0335(4) 0.1196(3) 0.0510(3) 0.0119(9) Uani 1 1 d . . . . .
C3A C 0.0094(4) 0.0346(3) -0.0105(3) 0.0120(10) Uani 1 1 d . . . . .
C4A C 0.0078(5) 0.0173(3) -0.0927(3) 0.0151(10) Uani 1 1 d . . . . .
C5A C 0.0341(5) 0.0897(3) -0.1155(3) 0.0159(10) Uani 1 1 d . . . . .
C6A C 0.0373(5) 0.1348(3) 0.1304(3) 0.0132(10) Uani 1 1 d . . . . .
H6A H 0.0538 0.1921 0.1713 0.016 Uiso 1 1 calc R . . . .
C7A C -0.0168(5) -0.0660(3) -0.1512(3) 0.0170(11) Uani 1 1 d . . . . .
H7A H -0.0200 -0.0770 -0.2063 0.020 Uiso 1 1 calc R . . . .
C8A C 0.0776(5) 0.2448(3) -0.0725(3) 0.0170(11) Uani 1 1 d . U . . .
C9A C -0.0173(5) 0.3038(3) -0.0579(3) 0.0169(10) Uani 1 1 d . . . . .
C10A C 0.0029(5) 0.3749(3) -0.0745(3) 0.0251(12) Uani 1 1 d . . . . .
H10A H -0.0621 0.4161 -0.0639 0.030 Uiso 1 1 calc R . . . .
C11A C 0.1184(5) 0.3848(3) -0.1066(3) 0.0231(11) Uani 1 1 d . . . . .
H11A H 0.1327 0.4341 -0.1170 0.028 Uiso 1 1 calc DR . . . .
C12A C 0.2160(5) 0.3245(3) -0.1246(3) 0.0223(11) Uani 1 1 d . . . . .
C13A C 0.1923(5) 0.2544(3) -0.1061(3) 0.0177(10) Uani 1 1 d . . . . .
H13A H 0.2564 0.2125 -0.1168 0.021 Uiso 1 1 calc R . . . .
C14A C -0.1829(5) 0.3439(3) 0.0393(3) 0.0226(12) Uani 1 1 d . . . . .
C15A C -0.3140(5) 0.3118(3) 0.0508(3) 0.0249(12) Uani 1 1 d . . . . .
H15A H -0.3709 0.3023 0.0040 0.030 Uiso 1 1 calc R . . . .
H15B H -0.3519 0.3572 0.0994 0.030 Uiso 1 1 calc R . . . .
C16A C -0.3122(5) 0.2285(3) 0.0601(3) 0.0174(10) Uani 1 1 d . . . . .
C17A C -0.3239(5) 0.1455(3) -0.0060(3) 0.0168(10) Uani 1 1 d . . . . .
C18A C -0.3336(5) 0.1321(3) -0.0884(3) 0.0217(11) Uani 1 1 d . . . . .
H18A H -0.3296 0.1810 -0.1000 0.026 Uiso 1 1 calc R . . . .
C19A C -0.3481(5) 0.0522(3) -0.1492(3) 0.0231(11) Uani 1 1 d . . . . .
H19A H -0.3538 0.0462 -0.2028 0.028 Uiso 1 1 calc R . . . .
C20A C -0.3552(5) -0.0241(3) -0.1362(3) 0.0201(11) Uani 1 1 d . . . . .
C21A C -0.3426(5) -0.0144(3) -0.0562(3) 0.0166(10) Uani 1 1 d . . . . .
C22A C -0.3265(5) 0.0705(3) 0.0085(3) 0.0167(10) Uani 1 1 d . . . . .
C23A C -0.3155(5) 0.0797(3) 0.0889(3) 0.0190(11) Uani 1 1 d . . . . .
C24A C -0.3017(5) 0.1617(3) 0.1515(3) 0.0202(11) Uani 1 1 d . . . . .
H24A H -0.2914 0.1683 0.2051 0.024 Uiso 1 1 calc R . . . .
C25A C -0.3027(5) 0.2344(3) 0.1373(3) 0.0206(11) Uani 1 1 d . . . . .
H25A H -0.2966 0.2903 0.1818 0.025 Uiso 1 1 calc R . . . .
C26A C -0.3734(5) -0.1077(3) -0.1989(3) 0.0265(12) Uani 1 1 d . . . . .
H26A H -0.3812 -0.1152 -0.2529 0.032 Uiso 1 1 calc R . . . .
C27A C -0.3802(5) -0.1800(3) -0.1830(3) 0.0294(13) Uani 1 1 d . . . . .
H27A H -0.3923 -0.2365 -0.2263 0.035 Uiso 1 1 calc R . . . .
C28A C -0.3696(5) -0.1705(3) -0.1052(3) 0.0268(12) Uani 1 1 d . . . . .
H28A H -0.3744 -0.2205 -0.0953 0.032 Uiso 1 1 calc R . . . .
C29A C -0.3520(5) -0.0884(3) -0.0408(3) 0.0205(11) Uani 1 1 d . . . . .
C30A C -0.3412(5) -0.0760(3) 0.0410(3) 0.0234(12) Uani 1 1 d . . . . .
H30A H -0.3471 -0.1253 0.0520 0.028 Uiso 1 1 calc R . . . .
C31A C -0.3234(5) 0.0019(3) 0.1013(3) 0.0235(12) Uani 1 1 d . . . . .
H31A H -0.3156 0.0071 0.1545 0.028 Uiso 1 1 calc R . . . .
C32A C 0.3399(5) 0.3324(3) -0.1667(3) 0.0257(12) Uiso 0.508(10) 1 d D . P A 1
C33A C 0.4484(11) 0.2767(8) -0.1543(8) 0.038(3) Uiso 0.508(10) 1 d D . P A 1
H33A H 0.4663 0.2967 -0.0966 0.058 Uiso 0.508(10) 1 calc R . P A 1
H33B H 0.5275 0.2833 -0.1803 0.058 Uiso 0.508(10) 1 calc R . P A 1
H33C H 0.4188 0.2153 -0.1784 0.058 Uiso 0.508(10) 1 calc R . P A 1
C34A C 0.3018(13) 0.2879(7) -0.2573(5) 0.0262(16) Uiso 0.508(10) 1 d D . P A 1
H34A H 0.2754 0.2269 -0.2732 0.039 Uiso 0.508(10) 1 calc R . P A 1
H34B H 0.3761 0.2909 -0.2887 0.039 Uiso 0.508(10) 1 calc R . P A 1
H34C H 0.2297 0.3178 -0.2676 0.039 Uiso 0.508(10) 1 calc R . P A 1
C35A C 0.3667(11) 0.4276(5) -0.1573(7) 0.0307(18) Uiso 0.508(10) 1 d D . P A 1
H35A H 0.2870 0.4536 -0.1653 0.037 Uiso 0.508(10) 1 calc DR . P A 1
H35B H 0.4339 0.4302 -0.1941 0.037 Uiso 0.508(10) 1 calc R . P A 1
C36A C 0.4218(13) 0.4758(8) -0.0564(7) 0.042(3) Uiso 0.508(10) 1 d . . P A 1
H36A H 0.3567 0.4653 -0.0231 0.062 Uiso 0.508(10) 1 calc R . P A 1
H36B H 0.4362 0.5385 -0.0382 0.062 Uiso 0.508(10) 1 calc R . P A 1
H36C H 0.5031 0.4504 -0.0517 0.062 Uiso 0.508(10) 1 calc R . P A 1
C32C C 0.3399(5) 0.3324(3) -0.1667(3) 0.0257(12) Uiso 0.492(10) 1 d D . P A 2
C33C C 0.3279(13) 0.2748(7) -0.2579(5) 0.0262(16) Uiso 0.492(10) 1 d D . P A 2
H33D H 0.3163 0.2137 -0.2680 0.039 Uiso 0.492(10) 1 calc R . P A 2
H33E H 0.4066 0.2825 -0.2836 0.039 Uiso 0.492(10) 1 calc R . P A 2
H33F H 0.2530 0.2913 -0.2802 0.039 Uiso 0.492(10) 1 calc R . P A 2
C34C C 0.3904(12) 0.4240(5) -0.1415(7) 0.0307(18) Uiso 0.492(10) 1 d D . P A 2
H34D H 0.3241 0.4570 -0.1529 0.046 Uiso 0.492(10) 1 calc R . P A 2
H34E H 0.4683 0.4238 -0.1714 0.046 Uiso 0.492(10) 1 calc R . P A 2
H34F H 0.4117 0.4512 -0.0836 0.046 Uiso 0.492(10) 1 calc R . P A 2
C35C C 0.4555(10) 0.3105(8) -0.1286(7) 0.028(3) Uiso 0.492(10) 1 d D . P A 2
H35C H 0.4512 0.2473 -0.1439 0.034 Uiso 0.492(10) 1 calc R . P A 2
H35D H 0.4503 0.3414 -0.0693 0.034 Uiso 0.492(10) 1 calc R . P A 2
C36C C 0.5858(13) 0.3349(8) -0.1538(7) 0.041(3) Uiso 0.492(10) 1 d . . P A 2
H36D H 0.5916 0.3048 -0.2125 0.062 Uiso 0.492(10) 1 calc R . P A 2
H36E H 0.6562 0.3176 -0.1287 0.062 Uiso 0.492(10) 1 calc R . P A 2
H36F H 0.5928 0.3978 -0.1362 0.062 Uiso 0.492(10) 1 calc R . P A 2
N1A N 0.0550(4) 0.1728(2) -0.0522(2) 0.0141(8) Uani 1 1 d . . . . .
O1A O 0.0738(4) 0.2673(2) 0.08029(19) 0.0213(8) Uani 1 1 d . . . . .
O2A O 0.0374(4) 0.0781(2) -0.18499(19) 0.0232(8) Uani 1 1 d . . . . .
O3A O -0.1368(3) 0.2866(2) -0.03263(19) 0.0199(7) Uani 1 1 d . . . . .
O4A O -0.1244(4) 0.4094(2) 0.0840(2) 0.0291(9) Uani 1 1 d . . . . .
C1B C 0.5479(5) 0.3072(3) 0.4642(3) 0.0133(9) Uani 1 1 d . U . . .
C2B C 0.5300(4) 0.3825(3) 0.4465(3) 0.0126(9) Uani 1 1 d . U . . .
C3B C 0.5075(4) 0.4640(3) 0.5089(3) 0.0124(9) Uani 1 1 d . U . . .
C4B C 0.5015(5) 0.4777(3) 0.5899(3) 0.0132(9) Uani 1 1 d . U . . .
C5B C 0.5238(5) 0.4044(3) 0.6100(3) 0.0155(9) Uani 1 1 d . U . . .
C6B C 0.5379(5) 0.3713(3) 0.3677(3) 0.0161(10) Uani 1 1 d . . . . .
H6B H 0.5544 0.3158 0.3258 0.019 Uiso 1 1 calc R . . . .
C7B C 0.4785(5) 0.5577(3) 0.6500(3) 0.0125(10) Uani 1 1 d . . . . .
H7B H 0.4735 0.5653 0.7041 0.015 Uiso 1 1 calc R . . . .
C8B C 0.5641(5) 0.2509(3) 0.5640(3) 0.0138(8) Uani 1 1 d . U . . .
C9B C 0.4672(5) 0.1884(3) 0.5460(3) 0.0159(9) Uani 1 1 d . U . . .
C10B C 0.4859(5) 0.1172(3) 0.5616(3) 0.0199(11) Uani 1 1 d . . . . .
H10B H 0.4197 0.0728 0.5486 0.024 Uiso 1 1 calc R . . . .
C11B C 0.6022(5) 0.1117(3) 0.5965(3) 0.0193(11) Uani 1 1 d . . . . .
H11B H 0.6147 0.0628 0.6070 0.023 Uiso 1 1 calc R . . . .
C12B C 0.7016(5) 0.1752(3) 0.6167(3) 0.0156(10) Uani 1 1 d . . . . .
C13B C 0.6795(5) 0.2452(3) 0.5992(3) 0.0171(9) Uani 1 1 d . U . . .
H13B H 0.7453 0.2898 0.6116 0.020 Uiso 1 1 calc R . . . .
C14B C 0.3003(5) 0.1461(3) 0.4440(3) 0.0182(11) Uani 1 1 d . . . . .
C15B C 0.1710(5) 0.1744(3) 0.4293(3) 0.0238(12) Uani 1 1 d . . . . .
H15C H 0.1122 0.1775 0.4724 0.029 Uiso 1 1 calc R . . . .
H15D H 0.1334 0.1301 0.3774 0.029 Uiso 1 1 calc R . . . .
C16B C 0.1782(5) 0.2625(3) 0.4269(3) 0.0212(11) Uani 1 1 d . . . . .
C17B C 0.1699(5) 0.3417(3) 0.4962(3) 0.0155(10) Uani 1 1 d . . . . .
C18B C 0.1571(5) 0.3481(3) 0.5762(3) 0.0210(11) Uani 1 1 d . . . . .
H18B H 0.1566 0.2964 0.5835 0.025 Uiso 1 1 calc R . . . .
C19B C 0.1460(5) 0.4241(3) 0.6402(3) 0.0245(12) Uani 1 1 d . . . . .
H19B H 0.1387 0.4249 0.6918 0.029 Uiso 1 1 calc R . . . .
C20B C 0.1444(5) 0.5047(3) 0.6338(3) 0.0204(11) Uani 1 1 d . . . . .
C21B C 0.1567(5) 0.5012(3) 0.5555(3) 0.0170(10) Uani 1 1 d . . . . .
C22B C 0.1716(5) 0.4207(3) 0.4880(3) 0.0158(10) Uani 1 1 d . . . . .
C23B C 0.1846(5) 0.4190(3) 0.4105(3) 0.0186(11) Uani 1 1 d . . . . .
C24B C 0.1954(5) 0.3400(3) 0.3440(3) 0.0253(12) Uani 1 1 d . . . . .
H24B H 0.2059 0.3383 0.2922 0.030 Uiso 1 1 calc R . . . .
C25B C 0.1910(5) 0.2630(3) 0.3525(3) 0.0231(11) Uani 1 1 d . . . . .
H25B H 0.1969 0.2092 0.3060 0.028 Uiso 1 1 calc R . . . .
C26B C 0.1279(5) 0.5848(3) 0.6992(3) 0.0304(13) Uani 1 1 d . . . . .
H26B H 0.1201 0.5878 0.7515 0.036 Uiso 1 1 calc R . . . .
C27B C 0.1226(5) 0.6596(3) 0.6890(3) 0.0325(13) Uani 1 1 d . . . . .
H27B H 0.1109 0.7133 0.7345 0.039 Uiso 1 1 calc R . . . .
C28B C 0.1339(5) 0.6581(3) 0.6137(3) 0.0278(12) Uani 1 1 d . . . . .
H28B H 0.1297 0.7104 0.6077 0.033 Uiso 1 1 calc R . . . .
C29B C 0.1517(5) 0.5790(3) 0.5466(3) 0.0213(11) Uani 1 1 d . . . . .
C30B C 0.1646(5) 0.5750(3) 0.4675(3) 0.0251(12) Uani 1 1 d . . . . .
H30B H 0.1612 0.6268 0.4607 0.030 Uiso 1 1 calc R . . . .
C31B C 0.1811(5) 0.5001(3) 0.4042(3) 0.0227(12) Uani 1 1 d . . . . .
H31B H 0.1911 0.4996 0.3529 0.027 Uiso 1 1 calc R . . . .
C32B C 0.8280(5) 0.1681(3) 0.6566(3) 0.0219(11) Uiso 0.629(12) 1 d D . P B 1
C33B C 0.7942(9) 0.1355(7) 0.7210(5) 0.0292(18) Uiso 0.629(12) 1 d D . P B 1
H33G H 0.7420 0.1782 0.7626 0.044 Uiso 0.629(12) 1 calc R . P B 1
H33H H 0.8742 0.1280 0.7457 0.044 Uiso 0.629(12) 1 calc R . P B 1
H33I H 0.7449 0.0797 0.6954 0.044 Uiso 0.629(12) 1 calc R . P B 1
C34B C 0.9030(9) 0.2546(4) 0.6983(6) 0.0278(18) Uiso 0.629(12) 1 d D . P B 1
H34G H 0.9284 0.2753 0.6584 0.042 Uiso 0.629(12) 1 calc R . P B 1
H34H H 0.9808 0.2474 0.7252 0.042 Uiso 0.629(12) 1 calc R . P B 1
H34I H 0.8485 0.2971 0.7383 0.042 Uiso 0.629(12) 1 calc R . P B 1
C35B C 0.9080(8) 0.1002(6) 0.5912(4) 0.0270(17) Uiso 0.629(12) 1 d D . P B 1
H35E H 0.8569 0.0442 0.5678 0.032 Uiso 0.629(12) 1 calc R . P B 1
H35F H 0.9212 0.1185 0.5477 0.032 Uiso 0.629(12) 1 calc R . P B 1
C36B C 1.0399(9) 0.0850(7) 0.6192(6) 0.039(2) Uiso 0.629(12) 1 d D . P B 1
H36G H 1.0950 0.1383 0.6374 0.058 Uiso 0.629(12) 1 calc R . P B 1
H36H H 1.0807 0.0378 0.5745 0.058 Uiso 0.629(12) 1 calc R . P B 1
H36I H 1.0288 0.0690 0.6638 0.058 Uiso 0.629(12) 1 calc R . P B 1
C32D C 0.8280(5) 0.1681(3) 0.6566(3) 0.0219(11) Uiso 0.371(12) 1 d D . P B 2
C33D C 0.8051(15) 0.1730(11) 0.7396(7) 0.0292(18) Uiso 0.371(12) 1 d D . P B 2
H33J H 0.7784 0.2314 0.7759 0.044 Uiso 0.371(12) 1 calc R . P B 2
H33K H 0.8852 0.1608 0.7609 0.044 Uiso 0.371(12) 1 calc R . P B 2
H33L H 0.7368 0.1300 0.7358 0.044 Uiso 0.371(12) 1 calc R . P B 2
C34D C 0.9270(13) 0.2418(8) 0.6647(11) 0.0278(18) Uiso 0.371(12) 1 d D . P B 2
H34J H 0.9541 0.2330 0.6111 0.042 Uiso 0.371(12) 1 calc R . P B 2
H34K H 1.0028 0.2409 0.6966 0.042 Uiso 0.371(12) 1 calc R . P B 2
H34L H 0.8869 0.2980 0.6915 0.042 Uiso 0.371(12) 1 calc R . P B 2
C35D C 0.8796(14) 0.0812(7) 0.5974(7) 0.0270(17) Uiso 0.371(12) 1 d D . P B 2
H35G H 0.8141 0.0345 0.5903 0.032 Uiso 0.371(12) 1 calc R . P B 2
H35H H 0.8890 0.0822 0.5445 0.032 Uiso 0.371(12) 1 calc R . P B 2
C36D C 1.0086(15) 0.0576(11) 0.6215(10) 0.039(2) Uiso 0.371(12) 1 d D . P B 2
H36J H 1.0797 0.0821 0.6019 0.058 Uiso 0.371(12) 1 calc R . P B 2
H36K H 1.0133 -0.0058 0.5978 0.058 Uiso 0.371(12) 1 calc R . P B 2
H36L H 1.0158 0.0814 0.6803 0.058 Uiso 0.371(12) 1 calc R . P B 2
N1B N 0.5445(4) 0.3237(2) 0.5457(2) 0.0152(8) Uani 1 1 d . U . . .
O1B O 0.5637(4) 0.23464(19) 0.41262(19) 0.0216(8) Uani 1 1 d . . . . .
O2B O 0.5255(4) 0.4120(2) 0.67870(18) 0.0223(8) Uani 1 1 d . . . . .
O3B O 0.3472(3) 0.2021(2) 0.51891(19) 0.0202(7) Uani 1 1 d . . . . .
O4B O 0.3558(4) 0.0842(2) 0.3990(2) 0.0254(8) Uani 1 1 d . . . . .
C3S C 0.3083(5) 0.9436(3) 0.6201(3) 0.0268(12) Uani 1 1 d . . . . .
H3SA H 0.3827 0.9083 0.5934 0.032 Uiso 1 1 calc R . . . .
H3SB H 0.2755 0.9692 0.5850 0.032 Uiso 1 1 calc R . . . .
C4S C 0.3538(7) 1.0149(4) 0.6982(4) 0.0493(18) Uani 1 1 d . . . . .
H4SA H 0.2790 1.0439 0.7292 0.074 Uiso 1 1 calc GR . . . .
H4SB H 0.4088 1.0570 0.6884 0.074 Uiso 1 1 calc GR . . . .
H4SC H 0.4038 0.9908 0.7285 0.074 Uiso 1 1 calc GR . . . .
N2S N 0.2041(5) 0.8856(3) 0.6284(3) 0.0280(10) Uani 1 1 d . . . . .
O3S O 0.1883(4) 0.8848(2) 0.6938(2) 0.0374(10) Uani 1 1 d . . . . .
O4S O 0.1410(4) 0.8386(3) 0.5680(2) 0.0426(11) Uani 1 1 d . . . . .
C1S C 0.2114(6) 0.4496(3) 0.1199(3) 0.0284(13) Uani 1 1 d . . . . .
H1SA H 0.2495 0.4874 0.0967 0.034 Uiso 1 1 calc R . . . .
H1SB H 0.1446 0.4103 0.0810 0.034 Uiso 1 1 calc R . . . .
C2S C 0.1486(7) 0.5046(4) 0.1953(3) 0.0459(16) Uani 1 1 d . . . . .
H2SA H 0.1013 0.4676 0.2153 0.069 Uiso 1 1 calc GR . . . .
H2SB H 0.0880 0.5418 0.1853 0.069 Uiso 1 1 calc GR . . . .
H2SC H 0.2146 0.5409 0.2355 0.069 Uiso 1 1 calc GR . . . .
N1S N 0.3147(5) 0.3963(3) 0.1295(3) 0.0304(11) Uani 1 1 d . . . . .
O1S O 0.3236(4) 0.3903(2) 0.1935(2) 0.0414(11) Uani 1 1 d . . . . .
O2S O 0.3826(5) 0.3591(3) 0.0723(3) 0.0518(12) 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
C1A C2A 1.476(6) . ?
C1A N1A 1.402(6) . ?
C1A O1A 1.212(5) . ?
C2A C3A 1.412(6) . ?
C2A C6A 1.373(6) . ?
C3A C3A 1.405(8) 2 ?
C3A C4A 1.414(6) . ?
C4A C5A 1.487(6) . ?
C4A C7A 1.375(6) . ?
C5A N1A 1.400(6) . ?
C5A O2A 1.211(5) . ?
C6A H6A 0.9500 . ?
C6A C7A 1.397(6) 2 ?
C7A C6A 1.397(6) 2 ?
C7A H7A 0.9500 . ?
C8A C9A 1.375(7) . ?
C8A C13A 1.381(7) . ?
C8A N1A 1.449(5) . ?
C9A C10A 1.388(6) . ?
C9A O3A 1.391(6) . ?
C10A H10A 0.9500 . ?
C10A C11A 1.376(7) . ?
C11A H11A 0.9500 . ?
C11A C12A 1.405(7) . ?
C12A C13A 1.399(6) . ?
C12A C32A 1.535(7) . ?
C12A C32C 1.535(7) . ?
C13A H13A 0.9500 . ?
C14A C15A 1.497(7) . ?
C14A O3A 1.364(6) . ?
C14A O4A 1.199(6) . ?
C15A H15A 0.9900 . ?
C15A H15B 0.9900 . ?
C15A C16A 1.508(6) . ?
C16A C17A 1.412(7) . ?
C16A C25A 1.386(7) . ?
C17A C18A 1.438(7) . ?
C17A C22A 1.420(6) . ?
C18A H18A 0.9500 . ?
C18A C19A 1.339(7) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.425(7) . ?
C20A C21A 1.418(6) . ?
C20A C26A 1.398(7) . ?
C21A C22A 1.425(6) . ?
C21A C29A 1.413(6) . ?
C22A C23A 1.426(6) . ?
C23A C24A 1.376(7) . ?
C23A C31A 1.445(7) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.380(7) . ?
C25A H25A 0.9500 . ?
C26A H26A 0.9500 . ?
C26A C27A 1.390(7) . ?
C27A H27A 0.9500 . ?
C27A C28A 1.377(7) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.393(7) . ?
C29A C30A 1.432(7) . ?
C30A H30A 0.9500 . ?
C30A C31A 1.317(7) . ?
C31A H31A 0.9500 . ?
C32A C33A 1.575(9) . ?
C32A C34A 1.546(8) . ?
C32A C35A 1.575(8) . ?
C33A H33A 0.9800 . ?
C33A H33B 0.9800 . ?
C33A H33C 0.9800 . ?
C34A H34A 0.9800 . ?
C34A H34B 0.9800 . ?
C34A H34C 0.9800 . ?
C35A H35A 0.9900 . ?
C35A H35B 0.9900 . ?
C35A C36A 1.755(16) . ?
C36A H36A 0.9800 . ?
C36A H36B 0.9800 . ?
C36A H36C 0.9800 . ?
C32C C33C 1.536(8) . ?
C32C C34C 1.499(8) . ?
C32C C35C 1.520(8) . ?
C33C H33D 0.9800 . ?
C33C H33E 0.9800 . ?
C33C H33F 0.9800 . ?
C34C H34D 0.9800 . ?
C34C H34E 0.9800 . ?
C34C H34F 0.9800 . ?
C35C H35C 0.9900 . ?
C35C H35D 0.9900 . ?
C35C C36C 1.530(17) . ?
C36C H36D 0.9800 . ?
C36C H36E 0.9800 . ?
C36C H36F 0.9800 . ?
C1B C2B 1.477(6) . ?
C1B N1B 1.405(6) . ?
C1B O1B 1.209(5) . ?
C2B C3B 1.398(6) . ?
C2B C6B 1.386(6) . ?
C3B C3B 1.420(8) 2_666 ?
C3B C4B 1.410(6) . ?
C4B C5B 1.479(6) . ?
C4B C7B 1.366(6) . ?
C5B N1B 1.398(6) . ?
C5B O2B 1.218(5) . ?
C6B H6B 0.9500 . ?
C6B C7B 1.405(6) 2_666 ?
C7B C6B 1.405(6) 2_666 ?
C7B H7B 0.9500 . ?
C8B C9B 1.365(7) . ?
C8B C13B 1.379(7) . ?
C8B N1B 1.447(5) . ?
C9B C10B 1.389(6) . ?
C9B O3B 1.399(6) . ?
C10B H10B 0.9500 . ?
C10B C11B 1.384(7) . ?
C11B H11B 0.9500 . ?
C11B C12B 1.389(7) . ?
C12B C13B 1.396(6) . ?
C12B C32B 1.528(7) . ?
C12B C32D 1.528(7) . ?
C13B H13B 0.9500 . ?
C14B C15B 1.500(7) . ?
C14B O3B 1.366(6) . ?
C14B O4B 1.194(6) . ?
C15B H15C 0.9900 . ?
C15B H15D 0.9900 . ?
C15B C16B 1.527(6) . ?
C16B C17B 1.407(7) . ?
C16B C25B 1.384(7) . ?
C17B C18B 1.441(6) . ?
C17B C22B 1.422(6) . ?
C18B H18B 0.9500 . ?
C18B C19B 1.332(7) . ?
C19B H19B 0.9500 . ?
C19B C20B 1.435(7) . ?
C20B C21B 1.429(6) . ?
C20B C26B 1.394(7) . ?
C21B C22B 1.413(7) . ?
C21B C29B 1.413(6) . ?
C22B C23B 1.427(6) . ?
C23B C24B 1.383(7) . ?
C23B C31B 1.442(6) . ?
C24B H24B 0.9500 . ?
C24B C25B 1.394(7) . ?
C25B H25B 0.9500 . ?
C26B H26B 0.9500 . ?
C26B C27B 1.373(8) . ?
C27B H27B 0.9500 . ?
C27B C28B 1.386(8) . ?
C28B H28B 0.9500 . ?
C28B C29B 1.401(7) . ?
C29B C30B 1.438(7) . ?
C30B H30B 0.9500 . ?
C30B C31B 1.324(7) . ?
C31B H31B 0.9500 . ?
C32B C33B 1.556(7) . ?
C32B C34B 1.515(7) . ?
C32B C35B 1.535(7) . ?
C33B H33G 0.9800 . ?
C33B H33H 0.9800 . ?
C33B H33I 0.9800 . ?
C34B H34G 0.9800 . ?
C34B H34H 0.9800 . ?
C34B H34I 0.9800 . ?
C35B H35E 0.9900 . ?
C35B H35F 0.9900 . ?
C35B C36B 1.525(10) . ?
C36B H36G 0.9800 . ?
C36B H36H 0.9800 . ?
C36B H36I 0.9800 . ?
C32D C33D 1.520(9) . ?
C32D C34D 1.548(9) . ?
C32D C35D 1.530(9) . ?
C33D H33J 0.9800 . ?
C33D H33K 0.9800 . ?
C33D H33L 0.9800 . ?
C34D H34J 0.9800 . ?
C34D H34K 0.9800 . ?
C34D H34L 0.9800 . ?
C35D H35G 0.9900 . ?
C35D H35H 0.9900 . ?
C35D C36D 1.524(13) . ?
C36D H36J 0.9800 . ?
C36D H36K 0.9800 . ?
C36D H36L 0.9800 . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C3S C4S 1.483(8) . ?
C3S N2S 1.493(7) . ?
C4S H4SA 0.9800 . ?
C4S H4SB 0.9800 . ?
C4S H4SC 0.9800 . ?
N2S O3S 1.225(5) . ?
N2S O4S 1.218(6) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C1S C2S 1.471(8) . ?
C1S N1S 1.487(7) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
N1S O1S 1.233(5) . ?
N1S O2S 1.214(6) . ?

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
N1A C1A C2A 116.9(4) . . ?
O1A C1A C2A 122.8(4) . . ?
O1A C1A N1A 120.3(4) . . ?
C3A C2A C1A 119.9(4) . . ?
C6A C2A C1A 119.5(4) . . ?
C6A C2A C3A 120.6(4) . . ?
C2A C3A C4A 121.4(4) . . ?
C3A C3A C2A 119.1(5) 2 . ?
C3A C3A C4A 119.4(5) 2 . ?
C3A C4A C5A 119.6(4) . . ?
C7A C4A C3A 120.1(4) . . ?
C7A C4A C5A 120.3(4) . . ?
N1A C5A C4A 116.6(4) . . ?
O2A C5A C4A 122.4(4) . . ?
O2A C5A N1A 121.1(4) . . ?
C2A C6A H6A 119.9 . . ?
C2A C6A C7A 120.2(4) . 2 ?
C7A C6A H6A 119.9 2 . ?
C4A C7A C6A 120.6(4) . 2 ?
C4A C7A H7A 119.7 . . ?
C6A C7A H7A 119.7 2 . ?
C9A C8A C13A 120.3(4) . . ?
C9A C8A N1A 119.0(4) . . ?
C13A C8A N1A 120.7(4) . . ?
C8A C9A C10A 120.3(5) . . ?
C8A C9A O3A 118.5(4) . . ?
C10A C9A O3A 121.0(4) . . ?
C9A C10A H10A 120.5 . . ?
C11A C10A C9A 119.0(5) . . ?
C11A C10A H10A 120.5 . . ?
C10A C11A H11A 118.9 . . ?
C10A C11A C12A 122.3(4) . . ?
C12A C11A H11A 118.9 . . ?
C11A C12A C32A 121.7(4) . . ?
C11A C12A C32C 121.7(4) . . ?
C13A C12A C11A 116.8(5) . . ?
C13A C12A C32A 121.4(4) . . ?
C13A C12A C32C 121.4(4) . . ?
C8A C13A C12A 121.2(5) . . ?
C8A C13A H13A 119.4 . . ?
C12A C13A H13A 119.4 . . ?
O3A C14A C15A 109.2(4) . . ?
O4A C14A C15A 127.4(5) . . ?
O4A C14A O3A 123.4(5) . . ?
C14A C15A H15A 108.8 . . ?
C14A C15A H15B 108.8 . . ?
C14A C15A C16A 113.6(4) . . ?
H15A C15A H15B 107.7 . . ?
C16A C15A H15A 108.8 . . ?
C16A C15A H15B 108.8 . . ?
C17A C16A C15A 122.8(4) . . ?
C25A C16A C15A 118.1(4) . . ?
C25A C16A C17A 119.1(4) . . ?
C16A C17A C18A 123.6(4) . . ?
C16A C17A C22A 119.0(4) . . ?
C22A C17A C18A 117.4(4) . . ?
C17A C18A H18A 119.2 . . ?
C19A C18A C17A 121.6(4) . . ?
C19A C18A H18A 119.2 . . ?
C18A C19A H19A 118.9 . . ?
C18A C19A C20A 122.3(4) . . ?
C20A C19A H19A 118.9 . . ?
C21A C20A C19A 118.3(4) . . ?
C26A C20A C19A 122.9(4) . . ?
C26A C20A C21A 118.8(4) . . ?
C20A C21A C22A 119.4(4) . . ?
C29A C21A C20A 120.0(4) . . ?
C29A C21A C22A 120.6(4) . . ?
C17A C22A C21A 121.0(4) . . ?
C17A C22A C23A 120.0(4) . . ?
C21A C22A C23A 119.0(4) . . ?
C22A C23A C31A 118.3(4) . . ?
C24A C23A C22A 119.1(4) . . ?
C24A C23A C31A 122.6(4) . . ?
C23A C24A H24A 119.7 . . ?
C23A C24A C25A 120.7(4) . . ?
C25A C24A H24A 119.7 . . ?
C16A C25A H25A 119.0 . . ?
C24A C25A C16A 122.0(4) . . ?
C24A C25A H25A 119.0 . . ?
C20A C26A H26A 119.7 . . ?
C27A C26A C20A 120.6(5) . . ?
C27A C26A H26A 119.7 . . ?
C26A C27A H27A 119.7 . . ?
C28A C27A C26A 120.5(5) . . ?
C28A C27A H27A 119.7 . . ?
C27A C28A H28A 119.6 . . ?
C27A C28A C29A 120.8(5) . . ?
C29A C28A H28A 119.6 . . ?
C21A C29A C30A 118.4(4) . . ?
C28A C29A C21A 119.2(5) . . ?
C28A C29A C30A 122.4(4) . . ?
C29A C30A H30A 119.1 . . ?
C31A C30A C29A 121.8(4) . . ?
C31A C30A H30A 119.1 . . ?
C23A C31A H31A 119.0 . . ?
C30A C31A C23A 121.9(5) . . ?
C30A C31A H31A 119.0 . . ?
C12A C32A C33A 110.3(6) . . ?
C12A C32A C34A 104.3(6) . . ?
C12A C32A C35A 112.0(5) . . ?
C33A C32A C35A 123.0(7) . . ?
C34A C32A C33A 106.3(6) . . ?
C34A C32A C35A 98.4(7) . . ?
C32A C33A H33A 109.5 . . ?
C32A C33A H33B 109.5 . . ?
C32A C33A H33C 109.5 . . ?
H33A C33A H33B 109.5 . . ?
H33A C33A H33C 109.5 . . ?
H33B C33A H33C 109.5 . . ?
C32A C34A H34A 109.5 . . ?
C32A C34A H34B 109.5 . . ?
C32A C34A H34C 109.5 . . ?
H34A C34A H34B 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
C32A C35A H35A 112.1 . . ?
C32A C35A H35B 112.1 . . ?
C32A C35A C36A 98.1(7) . . ?
H35A C35A H35B 109.8 . . ?
C36A C35A H35A 112.1 . . ?
C36A C35A H35B 112.1 . . ?
C35A C36A H36A 109.5 . . ?
C35A C36A H36B 109.5 . . ?
C35A C36A H36C 109.5 . . ?
H36A C36A H36B 109.5 . . ?
H36A C36A H36C 109.5 . . ?
H36B C36A H36C 109.5 . . ?
C12A C32C C33C 111.0(6) . . ?
C34C C32C C12A 114.3(6) . . ?
C34C C32C C33C 116.0(8) . . ?
C34C C32C C35C 92.8(7) . . ?
C35C C32C C12A 109.5(5) . . ?
C35C C32C C33C 112.0(7) . . ?
C32C C33C H33D 109.5 . . ?
C32C C33C H33E 109.5 . . ?
C32C C33C H33F 109.5 . . ?
H33D C33C H33E 109.5 . . ?
H33D C33C H33F 109.5 . . ?
H33E C33C H33F 109.5 . . ?
C32C C34C H34D 109.5 . . ?
C32C C34C H34E 109.5 . . ?
C32C C34C H34F 109.5 . . ?
H34D C34C H34E 109.5 . . ?
H34D C34C H34F 109.5 . . ?
H34E C34C H34F 109.5 . . ?
C32C C35C H35C 108.9 . . ?
C32C C35C H35D 108.9 . . ?
C32C C35C C36C 113.3(8) . . ?
H35C C35C H35D 107.7 . . ?
C36C C35C H35C 108.9 . . ?
C36C C35C H35D 108.9 . . ?
C35C C36C H36D 109.5 . . ?
C35C C36C H36E 109.5 . . ?
C35C C36C H36F 109.5 . . ?
H36D C36C H36E 109.5 . . ?
H36D C36C H36F 109.5 . . ?
H36E C36C H36F 109.5 . . ?
C1A N1A C8A 116.7(3) . . ?
C5A N1A C1A 125.5(3) . . ?
C5A N1A C8A 117.8(4) . . ?
C14A O3A C9A 119.9(4) . . ?
N1B C1B C2B 116.3(4) . . ?
O1B C1B C2B 123.1(4) . . ?
O1B C1B N1B 120.6(4) . . ?
C3B C2B C1B 120.1(4) . . ?
C6B C2B C1B 119.1(4) . . ?
C6B C2B C3B 120.7(4) . . ?
C2B C3B C3B 119.4(5) . 2_666 ?
C2B C3B C4B 122.0(4) . . ?
C4B C3B C3B 118.6(5) . 2_666 ?
C3B C4B C5B 119.2(4) . . ?
C7B C4B C3B 121.2(4) . . ?
C7B C4B C5B 119.5(4) . . ?
N1B C5B C4B 116.9(4) . . ?
O2B C5B C4B 123.0(4) . . ?
O2B C5B N1B 120.1(4) . . ?
C2B C6B H6B 120.1 . . ?
C2B C6B C7B 119.8(4) . 2_666 ?
C7B C6B H6B 120.1 2_666 . ?
C4B C7B C6B 120.2(4) . 2_666 ?
C4B C7B H7B 119.9 . . ?
C6B C7B H7B 119.9 2_666 . ?
C9B C8B C13B 120.8(4) . . ?
C9B C8B N1B 119.1(4) . . ?
C13B C8B N1B 120.0(4) . . ?
C8B C9B C10B 119.7(5) . . ?
C8B C9B O3B 118.5(4) . . ?
C10B C9B O3B 121.5(4) . . ?
C9B C10B H10B 120.5 . . ?
C11B C10B C9B 119.0(4) . . ?
C11B C10B H10B 120.5 . . ?
C10B C11B H11B 118.8 . . ?
C10B C11B C12B 122.4(4) . . ?
C12B C11B H11B 118.8 . . ?
C11B C12B C13B 116.7(4) . . ?
C11B C12B C32B 121.2(4) . . ?
C11B C12B C32D 121.2(4) . . ?
C13B C12B C32B 122.1(4) . . ?
C13B C12B C32D 122.1(4) . . ?
C8B C13B C12B 121.2(4) . . ?
C8B C13B H13B 119.4 . . ?
C12B C13B H13B 119.4 . . ?
O3B C14B C15B 109.4(4) . . ?
O4B C14B C15B 126.8(5) . . ?
O4B C14B O3B 123.7(5) . . ?
C14B C15B H15C 108.9 . . ?
C14B C15B H15D 108.9 . . ?
C14B C15B C16B 113.2(4) . . ?
H15C C15B H15D 107.8 . . ?
C16B C15B H15C 108.9 . . ?
C16B C15B H15D 108.9 . . ?
C17B C16B C15B 122.8(4) . . ?
C25B C16B C15B 117.6(4) . . ?
C25B C16B C17B 119.5(4) . . ?
C16B C17B C18B 123.7(4) . . ?
C16B C17B C22B 119.1(4) . . ?
C22B C17B C18B 117.2(4) . . ?
C17B C18B H18B 119.0 . . ?
C19B C18B C17B 122.0(4) . . ?
C19B C18B H18B 119.0 . . ?
C18B C19B H19B 118.9 . . ?
C18B C19B C20B 122.2(4) . . ?
C20B C19B H19B 118.9 . . ?
C21B C20B C19B 117.5(4) . . ?
C26B C20B C19B 123.6(4) . . ?
C26B C20B C21B 118.9(4) . . ?
C22B C21B C20B 120.1(4) . . ?
C22B C21B C29B 120.8(4) . . ?
C29B C21B C20B 119.1(4) . . ?
C17B C22B C23B 120.0(4) . . ?
C21B C22B C17B 120.9(4) . . ?
C21B C22B C23B 119.0(4) . . ?
C22B C23B C31B 118.4(4) . . ?
C24B C23B C22B 119.2(4) . . ?
C24B C23B C31B 122.4(4) . . ?
C23B C24B H24B 119.8 . . ?
C23B C24B C25B 120.3(4) . . ?
C25B C24B H24B 119.8 . . ?
C16B C25B C24B 121.8(5) . . ?
C16B C25B H25B 119.1 . . ?
C24B C25B H25B 119.1 . . ?
C20B C26B H26B 119.5 . . ?
C27B C26B C20B 121.0(5) . . ?
C27B C26B H26B 119.5 . . ?
C26B C27B H27B 119.3 . . ?
C26B C27B C28B 121.3(5) . . ?
C28B C27B H27B 119.3 . . ?
C27B C28B H28B 120.3 . . ?
C27B C28B C29B 119.5(5) . . ?
C29B C28B H28B 120.3 . . ?
C21B C29B C30B 118.8(5) . . ?
C28B C29B C21B 120.2(5) . . ?
C28B C29B C30B 121.0(4) . . ?
C29B C30B H30B 119.6 . . ?
C31B C30B C29B 120.8(4) . . ?
C31B C30B H30B 119.6 . . ?
C23B C31B H31B 118.9 . . ?
C30B C31B C23B 122.2(5) . . ?
C30B C31B H31B 118.9 . . ?
C12B C32B C33B 108.1(5) . . ?
C12B C32B C35B 107.6(4) . . ?
C34B C32B C12B 112.5(5) . . ?
C34B C32B C33B 108.1(5) . . ?
C34B C32B C35B 111.4(5) . . ?
C35B C32B C33B 109.0(5) . . ?
C32B C33B H33G 109.5 . . ?
C32B C33B H33H 109.5 . . ?
C32B C33B H33I 109.5 . . ?
H33G C33B H33H 109.5 . . ?
H33G C33B H33I 109.5 . . ?
H33H C33B H33I 109.5 . . ?
C32B C34B H34G 109.5 . . ?
C32B C34B H34H 109.5 . . ?
C32B C34B H34I 109.5 . . ?
H34G C34B H34H 109.5 . . ?
H34G C34B H34I 109.5 . . ?
H34H C34B H34I 109.5 . . ?
C32B C35B H35E 108.4 . . ?
C32B C35B H35F 108.4 . . ?
H35E C35B H35F 107.5 . . ?
C36B C35B C32B 115.5(6) . . ?
C36B C35B H35E 108.4 . . ?
C36B C35B H35F 108.4 . . ?
C35B C36B H36G 109.5 . . ?
C35B C36B H36H 109.5 . . ?
C35B C36B H36I 109.5 . . ?
H36G C36B H36H 109.5 . . ?
H36G C36B H36I 109.5 . . ?
H36H C36B H36I 109.5 . . ?
C12B C32D C34D 110.7(6) . . ?
C12B C32D C35D 104.2(6) . . ?
C33D C32D C12B 111.2(7) . . ?
C33D C32D C34D 108.9(7) . . ?
C33D C32D C35D 113.2(7) . . ?
C35D C32D C34D 108.6(7) . . ?
C32D C33D H33J 109.5 . . ?
C32D C33D H33K 109.5 . . ?
C32D C33D H33L 109.5 . . ?
H33J C33D H33K 109.5 . . ?
H33J C33D H33L 109.5 . . ?
H33K C33D H33L 109.5 . . ?
C32D C34D H34J 109.5 . . ?
C32D C34D H34K 109.5 . . ?
C32D C34D H34L 109.5 . . ?
H34J C34D H34K 109.5 . . ?
H34J C34D H34L 109.5 . . ?
H34K C34D H34L 109.5 . . ?
C32D C35D H35G 108.4 . . ?
C32D C35D H35H 108.4 . . ?
H35G C35D H35H 107.4 . . ?
C36D C35D C32D 115.7(9) . . ?
C36D C35D H35G 108.4 . . ?
C36D C35D H35H 108.4 . . ?
C35D C36D H36J 109.5 . . ?
C35D C36D H36K 109.5 . . ?
C35D C36D H36L 109.5 . . ?
H36J C36D H36K 109.5 . . ?
H36J C36D H36L 109.5 . . ?
H36K C36D H36L 109.5 . . ?
C1B N1B C8B 116.8(4) . . ?
C5B N1B C1B 125.4(4) . . ?
C5B N1B C8B 117.7(4) . . ?
C14B O3B C9B 119.6(4) . . ?
H3SA C3S H3SB 107.7 . . ?
C4S C3S H3SA 108.9 . . ?
C4S C3S H3SB 108.9 . . ?
C4S C3S N2S 113.3(4) . . ?
N2S C3S H3SA 108.9 . . ?
N2S C3S H3SB 108.9 . . ?
C3S C4S H4SA 109.5 . . ?
C3S C4S H4SB 109.5 . . ?
C3S C4S H4SC 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?
O3S N2S C3S 119.7(5) . . ?
O4S N2S C3S 117.3(4) . . ?
O4S N2S O3S 122.9(5) . . ?
H1SA C1S H1SB 107.6 . . ?
C2S C1S H1SA 108.7 . . ?
C2S C1S H1SB 108.7 . . ?
C2S C1S N1S 114.1(5) . . ?
N1S C1S H1SA 108.7 . . ?
N1S C1S H1SB 108.7 . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
O1S N1S C1S 118.5(5) . . ?
O2S N1S C1S 117.4(4) . . ?
O2S N1S O1S 124.0(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
C1A C2A C3A C3A 178.7(5) . . . 2 ?
C1A C2A C3A C4A 0.8(7) . . . . ?
C1A C2A C6A C7A -179.6(4) . . . 2 ?
C2A C1A N1A C5A 0.2(7) . . . . ?
C2A C1A N1A C8A -179.8(4) . . . . ?
C2A C3A C4A C5A 1.0(7) . . . . ?
C2A C3A C4A C7A -179.6(4) . . . . ?
C3A C2A C6A C7A -0.2(7) . . . 2 ?
C3A C3A C4A C5A -176.9(5) 2 . . . ?
C3A C3A C4A C7A 2.5(8) 2 . . . ?
C3A C4A C5A N1A -2.1(7) . . . . ?
C3A C4A C5A O2A 178.0(5) . . . . ?
C3A C4A C7A C6A -1.6(7) . . . 2 ?
C4A C5A N1A C1A 1.5(7) . . . . ?
C4A C5A N1A C8A -178.4(4) . . . . ?
C5A C4A C7A C6A 177.8(4) . . . 2 ?
C6A C2A C3A C3A -0.7(8) . . . 2 ?
C6A C2A C3A C4A -178.7(4) . . . . ?
C7A C4A C5A N1A 178.5(4) . . . . ?
C7A C4A C5A O2A -1.5(8) . . . . ?
C8A C9A C10A C11A 0.7(7) . . . . ?
C8A C9A O3A C14A 121.0(5) . . . . ?
C9A C8A C13A C12A 1.2(7) . . . . ?
C9A C8A N1A C1A -71.4(6) . . . . ?
C9A C8A N1A C5A 108.5(5) . . . . ?
C9A C10A C11A C12A 1.2(8) . . . . ?
C10A C9A O3A C14A -64.4(6) . . . . ?
C10A C11A C12A C13A -1.9(7) . . . . ?
C10A C11A C12A C32A 175.0(4) . . . . ?
C10A C11A C12A C32C 175.0(4) . . . . ?
C11A C12A C13A C8A 0.7(7) . . . . ?
C11A C12A C32A C33A 161.8(6) . . . . ?
C11A C12A C32A C34A -84.4(7) . . . . ?
C11A C12A C32A C35A 21.0(7) . . . . ?
C11A C12A C32C C33C -96.4(7) . . . . ?
C11A C12A C32C C34C 37.1(8) . . . . ?
C11A C12A C32C C35C 139.5(7) . . . . ?
C12A C32A C35A C36A 75.1(7) . . . . ?
C12A C32C C35C C36C -167.8(8) . . . . ?
C13A C8A C9A C10A -1.9(7) . . . . ?
C13A C8A C9A O3A 172.8(4) . . . . ?
C13A C8A N1A C1A 108.7(5) . . . . ?
C13A C8A N1A C5A -71.4(6) . . . . ?
C13A C12A C32A C33A -21.4(7) . . . . ?
C13A C12A C32A C34A 92.4(6) . . . . ?
C13A C12A C32A C35A -162.2(6) . . . . ?
C13A C12A C32C C33C 80.4(7) . . . . ?
C13A C12A C32C C34C -146.2(6) . . . . ?
C13A C12A C32C C35C -43.7(7) . . . . ?
C14A C15A C16A C17A -89.2(6) . . . . ?
C14A C15A C16A C25A 92.8(6) . . . . ?
C15A C14A O3A C9A 178.3(4) . . . . ?
C15A C16A C17A C18A 2.5(8) . . . . ?
C15A C16A C17A C22A -177.5(5) . . . . ?
C15A C16A C25A C24A 179.3(5) . . . . ?
C16A C17A C18A C19A -178.1(5) . . . . ?
C16A C17A C22A C21A 177.8(4) . . . . ?
C16A C17A C22A C23A -0.9(7) . . . . ?
C17A C16A C25A C24A 1.3(8) . . . . ?
C17A C18A C19A C20A 0.2(8) . . . . ?
C17A C22A C23A C24A -0.4(7) . . . . ?
C17A C22A C23A C31A 177.7(4) . . . . ?
C18A C17A C22A C21A -2.2(7) . . . . ?
C18A C17A C22A C23A 179.2(4) . . . . ?
C18A C19A C20A C21A -1.9(8) . . . . ?
C18A C19A C20A C26A 178.4(5) . . . . ?
C19A C20A C21A C22A 1.5(7) . . . . ?
C19A C20A C21A C29A 178.6(4) . . . . ?
C19A C20A C26A C27A -179.8(5) . . . . ?
C20A C21A C22A C17A 0.5(7) . . . . ?
C20A C21A C22A C23A 179.2(4) . . . . ?
C20A C21A C29A C28A 2.0(7) . . . . ?
C20A C21A C29A C30A -178.8(4) . . . . ?
C20A C26A C27A C28A 0.2(8) . . . . ?
C21A C20A C26A C27A 0.6(8) . . . . ?
C21A C22A C23A C24A -179.1(4) . . . . ?
C21A C22A C23A C31A -1.0(7) . . . . ?
C21A C29A C30A C31A 0.2(7) . . . . ?
C22A C17A C18A C19A 1.8(7) . . . . ?
C22A C21A C29A C28A 179.1(4) . . . . ?
C22A C21A C29A C30A -1.7(7) . . . . ?
C22A C23A C24A C25A 2.1(7) . . . . ?
C22A C23A C31A C30A -0.5(8) . . . . ?
C23A C24A C25A C16A -2.6(8) . . . . ?
C24A C23A C31A C30A 177.5(5) . . . . ?
C25A C16A C17A C18A -179.6(5) . . . . ?
C25A C16A C17A C22A 0.4(7) . . . . ?
C26A C20A C21A C22A -178.8(4) . . . . ?
C26A C20A C21A C29A -1.7(7) . . . . ?
C26A C27A C28A C29A 0.0(8) . . . . ?
C27A C28A C29A C21A -1.2(8) . . . . ?
C27A C28A C29A C30A 179.7(5) . . . . ?
C28A C29A C30A C31A 179.4(5) . . . . ?
C29A C21A C22A C17A -176.6(4) . . . . ?
C29A C21A C22A C23A 2.1(7) . . . . ?
C29A C30A C31A C23A 0.9(8) . . . . ?
C31A C23A C24A C25A -175.9(5) . . . . ?
C32A C12A C13A C8A -176.2(4) . . . . ?
C33A C32A C35A C36A -60.0(10) . . . . ?
C34A C32A C35A C36A -175.7(8) . . . . ?
C32C C12A C13A C8A -176.2(4) . . . . ?
C33C C32C C35C C36C 68.7(11) . . . . ?
C34C C32C C35C C36C -50.8(11) . . . . ?
N1A C1A C2A C3A -1.4(7) . . . . ?
N1A C1A C2A C6A 178.1(4) . . . . ?
N1A C8A C9A C10A 178.2(4) . . . . ?
N1A C8A C9A O3A -7.2(6) . . . . ?
N1A C8A C13A C12A -178.9(4) . . . . ?
O1A C1A C2A C3A 178.0(4) . . . . ?
O1A C1A C2A C6A -2.5(7) . . . . ?
O1A C1A N1A C5A -179.2(4) . . . . ?
O1A C1A N1A C8A 0.7(7) . . . . ?
O2A C5A N1A C1A -178.5(5) . . . . ?
O2A C5A N1A C8A 1.5(7) . . . . ?
O3A C9A C10A C11A -173.8(4) . . . . ?
O3A C14A C15A C16A 66.0(5) . . . . ?
O4A C14A C15A C16A -114.4(5) . . . . ?
O4A C14A O3A C9A -1.3(6) . . . . ?
C1B C2B C3B C3B 179.1(5) . . . 2_666 ?
C1B C2B C3B C4B 0.2(7) . . . . ?
C1B C2B C6B C7B -179.8(4) . . . 2_666 ?
C2B C1B N1B C5B 1.0(7) . . . . ?
C2B C1B N1B C8B -179.0(4) . . . . ?
C2B C3B C4B C5B 2.0(7) . . . . ?
C2B C3B C4B C7B -179.5(4) . . . . ?
C3B C2B C6B C7B -0.9(7) . . . 2_666 ?
C3B C3B C4B C5B -176.9(5) 2_666 . . . ?
C3B C3B C4B C7B 1.6(8) 2_666 . . . ?
C3B C4B C5B N1B -2.6(7) . . . . ?
C3B C4B C5B O2B 176.9(5) . . . . ?
C3B C4B C7B C6B -0.9(7) . . . 2_666 ?
C4B C5B N1B C1B 1.1(7) . . . . ?
C4B C5B N1B C8B -178.9(4) . . . . ?
C5B C4B C7B C6B 177.6(4) . . . 2_666 ?
C6B C2B C3B C3B 0.2(8) . . . 2_666 ?
C6B C2B C3B C4B -178.7(4) . . . . ?
C7B C4B C5B N1B 178.9(4) . . . . ?
C7B C4B C5B O2B -1.7(7) . . . . ?
C8B C9B C10B C11B 1.1(7) . . . . ?
C8B C9B O3B C14B 118.4(5) . . . . ?
C9B C8B C13B C12B 0.7(7) . . . . ?
C9B C8B N1B C1B -73.6(6) . . . . ?
C9B C8B N1B C5B 106.4(5) . . . . ?
C9B C10B C11B C12B 0.1(7) . . . . ?
C10B C9B O3B C14B -67.4(5) . . . . ?
C10B C11B C12B C13B -0.9(7) . . . . ?
C10B C11B C12B C32B 178.8(4) . . . . ?
C10B C11B C12B C32D 178.8(4) . . . . ?
C11B C12B C13B C8B 0.5(6) . . . . ?
C11B C12B C32B C33B -41.5(7) . . . . ?
C11B C12B C32B C34B -160.8(6) . . . . ?
C11B C12B C32B C35B 76.1(6) . . . . ?
C11B C12B C32D C33D -64.6(9) . . . . ?
C11B C12B C32D C34D 174.2(8) . . . . ?
C11B C12B C32D C35D 57.7(8) . . . . ?
C12B C32B C35B C36B 179.0(6) . . . . ?
C12B C32D C35D C36D 178.9(10) . . . . ?
C13B C8B C9B C10B -1.4(7) . . . . ?
C13B C8B C9B O3B 172.9(4) . . . . ?
C13B C8B N1B C1B 106.4(5) . . . . ?
C13B C8B N1B C5B -73.6(6) . . . . ?
C13B C12B C32B C33B 138.2(6) . . . . ?
C13B C12B C32B C34B 18.9(7) . . . . ?
C13B C12B C32B C35B -104.2(6) . . . . ?
C13B C12B C32D C33D 115.1(8) . . . . ?
C13B C12B C32D C34D -6.1(9) . . . . ?
C13B C12B C32D C35D -122.6(8) . . . . ?
C14B C15B C16B C17B -88.1(6) . . . . ?
C14B C15B C16B C25B 93.2(6) . . . . ?
C15B C14B O3B C9B 179.9(4) . . . . ?
C15B C16B C17B C18B 1.6(8) . . . . ?
C15B C16B C17B C22B -177.2(4) . . . . ?
C15B C16B C25B C24B 178.5(5) . . . . ?
C16B C17B C18B C19B -178.1(5) . . . . ?
C16B C17B C22B C21B 176.6(5) . . . . ?
C16B C17B C22B C23B -1.4(7) . . . . ?
C17B C16B C25B C24B -0.3(8) . . . . ?
C17B C18B C19B C20B 0.7(8) . . . . ?
C17B C22B C23B C24B 0.0(7) . . . . ?
C17B C22B C23B C31B 177.8(4) . . . . ?
C18B C17B C22B C21B -2.2(7) . . . . ?
C18B C17B C22B C23B 179.8(4) . . . . ?
C18B C19B C20B C21B -0.6(8) . . . . ?
C18B C19B C20B C26B 177.4(5) . . . . ?
C19B C20B C21B C22B -1.0(7) . . . . ?
C19B C20B C21B C29B 178.1(4) . . . . ?
C19B C20B C26B C27B -177.6(5) . . . . ?
C20B C21B C22B C17B 2.4(7) . . . . ?
C20B C21B C22B C23B -179.5(4) . . . . ?
C20B C21B C29B C28B -0.6(7) . . . . ?
C20B C21B C29B C30B 179.8(4) . . . . ?
C20B C26B C27B C28B -0.2(9) . . . . ?
C21B C20B C26B C27B 0.3(8) . . . . ?
C21B C22B C23B C24B -178.1(5) . . . . ?
C21B C22B C23B C31B -0.3(7) . . . . ?
C21B C29B C30B C31B -0.2(7) . . . . ?
C22B C17B C18B C19B 0.7(7) . . . . ?
C22B C21B C29B C28B 178.6(5) . . . . ?
C22B C21B C29B C30B -1.1(7) . . . . ?
C22B C23B C24B C25B 1.3(8) . . . . ?
C22B C23B C31B C30B -1.0(7) . . . . ?
C23B C24B C25B C16B -1.2(8) . . . . ?
C24B C23B C31B C30B 176.7(5) . . . . ?
C25B C16B C17B C18B -179.7(5) . . . . ?
C25B C16B C17B C22B 1.5(7) . . . . ?
C26B C20B C21B C22B -179.1(5) . . . . ?
C26B C20B C21B C29B 0.1(7) . . . . ?
C26B C27B C28B C29B -0.3(8) . . . . ?
C27B C28B C29B C21B 0.7(8) . . . . ?
C27B C28B C29B C30B -179.7(5) . . . . ?
C28B C29B C30B C31B -179.9(5) . . . . ?
C29B C21B C22B C17B -176.7(4) . . . . ?
C29B C21B C22B C23B 1.3(7) . . . . ?
C29B C30B C31B C23B 1.2(8) . . . . ?
C31B C23B C24B C25B -176.4(5) . . . . ?
C32B C12B C13B C8B -179.2(4) . . . . ?
C33B C32B C35B C36B -64.0(8) . . . . ?
C34B C32B C35B C36B 55.2(8) . . . . ?
C32D C12B C13B C8B -179.2(4) . . . . ?
C33D C32D C35D C36D -60.2(14) . . . . ?
C34D C32D C35D C36D 60.9(13) . . . . ?
N1B C1B C2B C3B -1.7(6) . . . . ?
N1B C1B C2B C6B 177.2(4) . . . . ?
N1B C8B C9B C10B 178.6(4) . . . . ?
N1B C8B C9B O3B -7.1(6) . . . . ?
N1B C8B C13B C12B -179.3(4) . . . . ?
O1B C1B C2B C3B 177.7(5) . . . . ?
O1B C1B C2B C6B -3.4(7) . . . . ?
O1B C1B N1B C5B -178.4(5) . . . . ?
O1B C1B N1B C8B 1.6(7) . . . . ?
O2B C5B N1B C1B -178.4(4) . . . . ?
O2B C5B N1B C8B 1.6(7) . . . . ?
O3B C9B C10B C11B -173.1(4) . . . . ?
O3B C14B C15B C16B 64.7(5) . . . . ?
O4B C14B C15B C16B -116.0(5) . . . . ?
O4B C14B O3B C9B 0.6(6) . . . . ?
C4S C3S N2S O3S -19.0(7) . . . . ?
C4S C3S N2S O4S 163.6(5) . . . . ?
C2S C1S N1S O1S 12.5(7) . . . . ?
C2S C1S N1S O2S -169.8(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5220(19)
2 0.4780(19)

# start Validation Reply Form
_vrf_PLAT027_twin5a              
;
PROBLEM: _diffrn_reflns_theta_full (too) Low ............      24.30 Degree
RESPONSE: No diffraction intensity observed at higher angles because of low
crystal quality of the twinned and disordered material. Dataset truncated when
the mean I/sig(I) fell below 2.0 (from the SHELX XPrep output file).
;
_vrf_PLAT201_twin5a              
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         10 Report
RESPONSE: Atoms of two independent disordered -C(CH3)2(CH2CH3) groups were
refined isotropically.
;
####################################################################### 
# 
# 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_dfya53_meno2_0m
_database_code_depnum_ccdc_archive 'CCDC 1412212'
_audit_update_record             
;
2015-07-12 deposited with the CCDC.
2015-08-17 downloaded from the CCDC.
;
_audit_creation_date             2015-03-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H54 N2 O8, 2(C H3 N O2)'
_chemical_formula_sum            'C74 H60 N4 O12'
_chemical_formula_weight         1197.26
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'

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

_cell_length_a                   10.0093(4)
_cell_length_b                   10.5133(4)
_cell_length_c                   16.3672(7)
_cell_angle_alpha                71.388(2)
_cell_angle_beta                 89.742(2)
_cell_angle_gamma                62.504(2)
_cell_volume                     1426.83(10)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.551
_cell_measurement_theta_min      2.328
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.943
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1385 before and 0.0490 after correction.
The Ratio of minimum to maximum transmission is 0.9226.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27328
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        27.550
_diffrn_reflns_theta_max         27.551
_diffrn_reflns_theta_min         2.240
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON-100 area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_special_details          ?
_diffrn_standards_number         ?
_reflns_number_gt                5746
_reflns_number_total             6558
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0143(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         6558
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0419
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0582P)²+0.7907P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1187
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C35(H35A,H35B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C18(H18), C19(H19), C24(H24),
 C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31)
2.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.48271(11) 0.59558(12) 0.22934(6) 0.0191(2) Uani 1 1 d . . . . .
O2 O 0.92782(10) 0.35011(12) 0.41962(6) 0.0206(2) Uani 1 1 d . . . . .
O3 O 0.78751(11) 0.25167(10) 0.25704(6) 0.01534(19) Uani 1 1 d . . . . .
O4 O 0.63164(13) 0.32488(13) 0.13238(7) 0.0284(3) Uani 1 1 d . . . . .
N1 N 0.70383(12) 0.48123(12) 0.32497(7) 0.0120(2) Uani 1 1 d . . . . .
C1 C 0.54418(14) 0.54826(14) 0.30443(8) 0.0124(2) Uani 1 1 d . . . . .
C2 C 0.46018(14) 0.55808(14) 0.37874(8) 0.0112(2) Uani 1 1 d . . . . .
C3 C 0.54104(13) 0.49437(13) 0.46478(7) 0.0098(2) Uani 1 1 d . . . . .
C4 C 0.70259(13) 0.41882(13) 0.48267(8) 0.0115(2) Uani 1 1 d . . . . .
C5 C 0.78971(14) 0.41103(14) 0.40947(8) 0.0127(2) Uani 1 1 d . . . . .
C6 C 0.30256(14) 0.63190(15) 0.36317(8) 0.0142(2) Uani 1 1 d . . . . .
H6 H 0.2490 0.6750 0.3051 0.017 Uiso 1 1 calc R . . . .
C7 C 0.77907(14) 0.35639(15) 0.56721(8) 0.0148(2) Uani 1 1 d . . . . .
H7 H 0.8876 0.3051 0.5784 0.018 Uiso 1 1 calc R . . . .
C8 C 0.78974(13) 0.47842(14) 0.25391(8) 0.0122(2) Uani 1 1 d . . . . .
C9 C 0.82933(14) 0.36468(14) 0.21914(8) 0.0130(2) Uani 1 1 d . . . . .
C10 C 0.91749(15) 0.35895(15) 0.15345(8) 0.0163(3) Uani 1 1 d . . . . .
H10 H 0.9453 0.2808 0.1294 0.020 Uiso 1 1 calc R . . . .
C11 C 0.96481(15) 0.46801(15) 0.12309(8) 0.0161(3) Uani 1 1 d . . . . .
H11 H 1.0262 0.4625 0.0786 0.019 Uiso 1 1 calc R . . . .
C12 C 0.92450(14) 0.58634(14) 0.15629(8) 0.0130(2) Uani 1 1 d . . . . .
C13 C 0.83582(14) 0.58821(14) 0.22231(8) 0.0136(2) Uani 1 1 d . . . . .
H13 H 0.8062 0.6668 0.2462 0.016 Uiso 1 1 calc R . . . .
C14 C 0.68022(15) 0.24706(15) 0.20770(8) 0.0162(3) Uani 1 1 d . . . . .
C15 C 0.63855(16) 0.12938(15) 0.26266(8) 0.0170(3) Uani 1 1 d . . . . .
H15A H 0.7337 0.0324 0.2935 0.020 Uiso 1 1 calc R . . . .
H15B H 0.5823 0.1086 0.2236 0.020 Uiso 1 1 calc R . . . .
C16 C 0.54111(15) 0.17835(14) 0.32995(8) 0.0149(2) Uani 1 1 d . . . . .
C17 C 0.60517(14) 0.13636(14) 0.41721(8) 0.0135(2) Uani 1 1 d . . . . .
C18 C 0.76718(15) 0.05427(15) 0.44895(9) 0.0163(3) Uani 1 1 d . . . . .
H18 H 0.8358 0.0309 0.4090 0.020 Uiso 1 1 calc R . . . .
C19 C 0.82433(15) 0.00949(15) 0.53416(9) 0.0174(3) Uani 1 1 d . . . . .
H19 H 0.9320 -0.0443 0.5524 0.021 Uiso 1 1 calc R . . . .
C20 C 0.72694(15) 0.04107(14) 0.59735(8) 0.0153(3) Uani 1 1 d . . . . .
C21 C 0.56617(14) 0.12269(14) 0.56874(8) 0.0130(2) Uani 1 1 d . . . . .
C22 C 0.50507(14) 0.17145(14) 0.47880(8) 0.0126(2) Uani 1 1 d . . . . .
C23 C 0.34398(14) 0.25136(14) 0.45155(8) 0.0143(2) Uani 1 1 d . . . . .
C24 C 0.28501(15) 0.29577(15) 0.36384(9) 0.0172(3) Uani 1 1 d . . . . .
H24 H 0.1776 0.3518 0.3446 0.021 Uiso 1 1 calc R . . . .
C25 C 0.38270(15) 0.25835(15) 0.30473(9) 0.0169(3) Uani 1 1 d . . . . .
H25 H 0.3406 0.2880 0.2456 0.020 Uiso 1 1 calc R . . . .
C26 C 0.78463(16) -0.00740(15) 0.68611(9) 0.0191(3) Uani 1 1 d . . . . .
H26 H 0.8920 -0.0608 0.7054 0.023 Uiso 1 1 calc R . . . .
C27 C 0.68668(17) 0.02171(16) 0.74610(9) 0.0204(3) Uani 1 1 d . . . . .
H27 H 0.7274 -0.0128 0.8061 0.024 Uiso 1 1 calc R . . . .
C28 C 0.52969(16) 0.10088(15) 0.71893(9) 0.0175(3) Uani 1 1 d . . . . .
H28 H 0.4639 0.1203 0.7606 0.021 Uiso 1 1 calc R . . . .
C29 C 0.46652(15) 0.15270(14) 0.63068(8) 0.0143(2) Uani 1 1 d . . . . .
C30 C 0.30448(15) 0.23299(15) 0.60008(9) 0.0171(3) Uani 1 1 d . . . . .
H30 H 0.2367 0.2530 0.6408 0.020 Uiso 1 1 calc R . . . .
C31 C 0.24641(15) 0.28043(15) 0.51564(9) 0.0172(3) Uani 1 1 d . . . . .
H31 H 0.1387 0.3343 0.4978 0.021 Uiso 1 1 calc R . . . .
C32 C 0.97097(14) 0.71115(14) 0.11815(8) 0.0147(2) Uani 1 1 d . . . . .
C33 C 1.14157(16) 0.63730(17) 0.11063(11) 0.0254(3) Uani 1 1 d . . . . .
H33A H 1.2033 0.5759 0.1692 0.038 Uiso 1 1 calc GR . . . .
H33B H 1.1678 0.7180 0.0816 0.038 Uiso 1 1 calc GR . . . .
H33C H 1.1623 0.5710 0.0763 0.038 Uiso 1 1 calc GR . . . .
C34 C 0.87414(17) 0.81440(16) 0.02659(9) 0.0219(3) Uani 1 1 d . . . . .
H34A H 0.8902 0.7517 -0.0095 0.033 Uiso 1 1 calc GR . . . .
H34B H 0.9047 0.8923 -0.0007 0.033 Uiso 1 1 calc GR . . . .
H34C H 0.7658 0.8650 0.0317 0.033 Uiso 1 1 calc GR . . . .
C35 C 0.93987(16) 0.80843(16) 0.17681(9) 0.0184(3) Uani 1 1 d . . . . .
H35A H 0.8290 0.8584 0.1788 0.022 Uiso 1 1 calc R . . . .
H35B H 0.9938 0.7383 0.2370 0.022 Uiso 1 1 calc R . . . .
C36 C 0.98787(19) 0.93230(18) 0.14866(11) 0.0285(3) Uani 1 1 d . . . . .
H36A H 1.0976 0.8848 0.1466 0.043 Uiso 1 1 calc GR . . . .
H36B H 0.9662 0.9850 0.1908 0.043 Uiso 1 1 calc GR . . . .
H36C H 0.9306 1.0066 0.0906 0.043 Uiso 1 1 calc GR . . . .
O5 O 0.65961(13) 0.71901(15) -0.07691(8) 0.0345(3) Uani 1 1 d . . . . .
O6 O 0.46268(16) 0.92457(14) -0.07891(8) 0.0434(3) Uani 1 1 d . . . . .
N2 N 0.55043(14) 0.78699(14) -0.04559(8) 0.0230(3) Uani 1 1 d . . . . .
C37 C 0.5228(2) 0.7006(2) 0.03690(11) 0.0387(4) Uani 1 1 d . . . . .
H37A H 0.5725 0.5916 0.0445 0.058 Uiso 1 1 calc GR . . . .
H37B H 0.4126 0.7398 0.0351 0.058 Uiso 1 1 calc GR . . . .
H37C H 0.5649 0.7130 0.0860 0.058 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.2126(15) . ?
O2 C5 1.2106(15) . ?
O3 C9 1.3993(15) . ?
O3 C14 1.3743(16) . ?
O4 C14 1.1915(17) . ?
N1 C1 1.4061(15) . ?
N1 C5 1.4034(16) . ?
N1 C8 1.4431(15) . ?
C1 C2 1.4791(16) . ?
C2 C3 1.4122(16) . ?
C2 C6 1.3795(17) . ?
C3 C3 1.417(2) 2_666 ?
C3 C4 1.4147(16) . ?
C4 C5 1.4797(16) . ?
C4 C7 1.3774(17) . ?
C6 H6 0.9500 . ?
C6 C7 1.4033(17) 2_666 ?
C7 C6 1.4034(17) 2_666 ?
C7 H7 0.9500 . ?
C8 C9 1.3804(17) . ?
C8 C13 1.3860(17) . ?
C9 C10 1.3863(17) . ?
C10 H10 0.9500 . ?
C10 C11 1.3861(18) . ?
C11 H11 0.9500 . ?
C11 C12 1.4041(18) . ?
C12 C13 1.3945(17) . ?
C12 C32 1.5382(17) . ?
C13 H13 0.9500 . ?
C14 C15 1.5088(17) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.5224(17) . ?
C16 C17 1.4108(18) . ?
C16 C25 1.3946(18) . ?
C17 C18 1.4399(17) . ?
C17 C22 1.4293(17) . ?
C18 H18 0.9500 . ?
C18 C19 1.3541(19) . ?
C19 H19 0.9500 . ?
C19 C20 1.4287(18) . ?
C20 C21 1.4214(17) . ?
C20 C26 1.4024(18) . ?
C21 C22 1.4285(17) . ?
C21 C29 1.4236(17) . ?
C22 C23 1.4217(17) . ?
C23 C24 1.3973(18) . ?
C23 C31 1.4378(18) . ?
C24 H24 0.9500 . ?
C24 C25 1.3879(19) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C26 C27 1.387(2) . ?
C27 H27 0.9500 . ?
C27 C28 1.386(2) . ?
C28 H28 0.9500 . ?
C28 C29 1.4038(18) . ?
C29 C30 1.4378(18) . ?
C30 H30 0.9500 . ?
C30 C31 1.340(2) . ?
C31 H31 0.9500 . ?
C32 C33 1.5391(18) . ?
C32 C34 1.5385(18) . ?
C32 C35 1.5474(18) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.5270(19) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
O5 N2 1.2147(17) . ?
O6 N2 1.2201(17) . ?
N2 C37 1.473(2) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 O3 C9 117.90(10) . . ?
C1 N1 C8 118.03(10) . . ?
C5 N1 C1 125.84(10) . . ?
C5 N1 C8 116.09(10) . . ?
O1 C1 N1 120.29(11) . . ?
O1 C1 C2 123.68(11) . . ?
N1 C1 C2 116.03(10) . . ?
C3 C2 C1 120.09(10) . . ?
C6 C2 C1 119.52(11) . . ?
C6 C2 C3 120.38(11) . . ?
C2 C3 C3 119.44(13) . 2_666 ?
C2 C3 C4 121.64(11) . . ?
C4 C3 C3 118.92(13) . 2_666 ?
C3 C4 C5 119.53(11) . . ?
C7 C4 C3 120.62(11) . . ?
C7 C4 C5 119.82(11) . . ?
O2 C5 N1 120.13(11) . . ?
O2 C5 C4 123.26(11) . . ?
N1 C5 C4 116.60(10) . . ?
C2 C6 H6 119.8 . . ?
C2 C6 C7 120.31(11) . 2_666 ?
C7 C6 H6 119.8 2_666 . ?
C4 C7 C6 120.33(11) . 2_666 ?
C4 C7 H7 119.8 . . ?
C6 C7 H7 119.8 2_666 . ?
C9 C8 N1 120.23(11) . . ?
C9 C8 C13 120.15(11) . . ?
C13 C8 N1 119.60(11) . . ?
C8 C9 O3 117.66(11) . . ?
C8 C9 C10 119.85(11) . . ?
C10 C9 O3 122.31(11) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 C9 119.59(11) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 H11 119.1 . . ?
C10 C11 C12 121.86(11) . . ?
C12 C11 H11 119.1 . . ?
C11 C12 C32 120.94(11) . . ?
C13 C12 C11 116.86(11) . . ?
C13 C12 C32 122.15(11) . . ?
C8 C13 C12 121.68(11) . . ?
C8 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
O3 C14 C15 109.91(11) . . ?
O4 C14 O3 123.31(12) . . ?
O4 C14 C15 126.77(12) . . ?
C14 C15 H15A 108.8 . . ?
C14 C15 H15B 108.8 . . ?
C14 C15 C16 113.76(10) . . ?
H15A C15 H15B 107.7 . . ?
C16 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
C17 C16 C15 122.31(12) . . ?
C25 C16 C15 117.83(11) . . ?
C25 C16 C17 119.71(12) . . ?
C16 C17 C18 123.52(11) . . ?
C16 C17 C22 118.77(11) . . ?
C22 C17 C18 117.66(11) . . ?
C17 C18 H18 119.1 . . ?
C19 C18 C17 121.80(12) . . ?
C19 C18 H18 119.1 . . ?
C18 C19 H19 119.1 . . ?
C18 C19 C20 121.71(12) . . ?
C20 C19 H19 119.1 . . ?
C21 C20 C19 118.36(11) . . ?
C26 C20 C19 122.28(12) . . ?
C26 C20 C21 119.35(12) . . ?
C20 C21 C22 120.23(11) . . ?
C20 C21 C29 119.51(11) . . ?
C29 C21 C22 120.25(11) . . ?
C21 C22 C17 120.23(11) . . ?
C23 C22 C17 120.30(11) . . ?
C23 C22 C21 119.45(11) . . ?
C22 C23 C31 118.95(11) . . ?
C24 C23 C22 119.16(12) . . ?
C24 C23 C31 121.87(12) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 C23 120.30(12) . . ?
C25 C24 H24 119.9 . . ?
C16 C25 H25 119.1 . . ?
C24 C25 C16 121.70(12) . . ?
C24 C25 H25 119.1 . . ?
C20 C26 H26 119.6 . . ?
C27 C26 C20 120.76(12) . . ?
C27 C26 H26 119.6 . . ?
C26 C27 H27 119.8 . . ?
C28 C27 C26 120.36(12) . . ?
C28 C27 H27 119.8 . . ?
C27 C28 H28 119.5 . . ?
C27 C28 C29 120.97(12) . . ?
C29 C28 H28 119.5 . . ?
C21 C29 C30 118.25(11) . . ?
C28 C29 C21 119.05(12) . . ?
C28 C29 C30 122.69(12) . . ?
C29 C30 H30 119.1 . . ?
C31 C30 C29 121.80(12) . . ?
C31 C30 H30 119.1 . . ?
C23 C31 H31 119.4 . . ?
C30 C31 C23 121.30(12) . . ?
C30 C31 H31 119.4 . . ?
C12 C32 C33 110.22(10) . . ?
C12 C32 C34 107.47(10) . . ?
C12 C32 C35 110.42(10) . . ?
C33 C32 C35 109.54(11) . . ?
C34 C32 C33 109.55(11) . . ?
C34 C32 C35 109.62(11) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 108.3 . . ?
C32 C35 H35B 108.3 . . ?
H35A C35 H35B 107.4 . . ?
C36 C35 C32 115.87(11) . . ?
C36 C35 H35A 108.3 . . ?
C36 C35 H35B 108.3 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O5 N2 O6 123.01(14) . . ?
O5 N2 C37 118.89(14) . . ?
O6 N2 C37 118.10(14) . . ?
N2 C37 H37A 109.5 . . ?
N2 C37 H37B 109.5 . . ?
N2 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 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
O1 C1 C2 C3 177.37(12) . . . . ?
O1 C1 C2 C6 -3.64(19) . . . . ?
O3 C9 C10 C11 -175.17(11) . . . . ?
O3 C14 C15 C16 72.58(14) . . . . ?
O4 C14 C15 C16 -108.44(16) . . . . ?
N1 C1 C2 C3 -3.48(16) . . . . ?
N1 C1 C2 C6 175.51(11) . . . . ?
N1 C8 C9 O3 -1.99(17) . . . . ?
N1 C8 C9 C10 -177.22(11) . . . . ?
N1 C8 C13 C12 177.24(11) . . . . ?
C1 N1 C5 O2 176.29(12) . . . . ?
C1 N1 C5 C4 -4.74(17) . . . . ?
C1 N1 C8 C9 -82.64(15) . . . . ?
C1 N1 C8 C13 99.08(13) . . . . ?
C1 C2 C3 C3 179.56(13) . . . 2_666 ?
C1 C2 C3 C4 -0.65(17) . . . . ?
C1 C2 C6 C7 -179.39(11) . . . 2_666 ?
C2 C3 C4 C5 2.38(17) . . . . ?
C2 C3 C4 C7 -179.44(11) . . . . ?
C3 C2 C6 C7 -0.40(18) . . . 2_666 ?
C3 C3 C4 C5 -177.82(13) 2_666 . . . ?
C3 C3 C4 C7 0.4(2) 2_666 . . . ?
C3 C4 C5 O2 179.04(12) . . . . ?
C3 C4 C5 N1 0.10(16) . . . . ?
C3 C4 C7 C6 -0.55(19) . . . 2_666 ?
C5 N1 C1 O1 -174.43(12) . . . . ?
C5 N1 C1 C2 6.38(17) . . . . ?
C5 N1 C8 C9 95.27(14) . . . . ?
C5 N1 C8 C13 -83.01(14) . . . . ?
C5 C4 C7 C6 177.62(11) . . . 2_666 ?
C6 C2 C3 C3 0.6(2) . . . 2_666 ?
C6 C2 C3 C4 -179.63(11) . . . . ?
C7 C4 C5 O2 0.84(19) . . . . ?
C7 C4 C5 N1 -178.09(11) . . . . ?
C8 N1 C1 O1 3.25(17) . . . . ?
C8 N1 C1 C2 -175.93(10) . . . . ?
C8 N1 C5 O2 -1.43(17) . . . . ?
C8 N1 C5 C4 177.53(10) . . . . ?
C8 C9 C10 C11 -0.17(19) . . . . ?
C9 O3 C14 O4 6.89(19) . . . . ?
C9 O3 C14 C15 -174.08(10) . . . . ?
C9 C8 C13 C12 -1.04(19) . . . . ?
C9 C10 C11 C12 -0.8(2) . . . . ?
C10 C11 C12 C13 0.78(19) . . . . ?
C10 C11 C12 C32 -176.65(12) . . . . ?
C11 C12 C13 C8 0.12(18) . . . . ?
C11 C12 C32 C33 -48.19(16) . . . . ?
C11 C12 C32 C34 71.13(15) . . . . ?
C11 C12 C32 C35 -169.35(12) . . . . ?
C12 C32 C35 C36 177.27(12) . . . . ?
C13 C8 C9 O3 176.28(11) . . . . ?
C13 C8 C9 C10 1.06(19) . . . . ?
C13 C12 C32 C33 134.51(13) . . . . ?
C13 C12 C32 C34 -106.17(13) . . . . ?
C13 C12 C32 C35 13.36(16) . . . . ?
C14 O3 C9 C8 113.08(13) . . . . ?
C14 O3 C9 C10 -71.81(15) . . . . ?
C14 C15 C16 C17 -94.64(14) . . . . ?
C14 C15 C16 C25 89.88(14) . . . . ?
C15 C16 C17 C18 4.82(18) . . . . ?
C15 C16 C17 C22 -172.71(11) . . . . ?
C15 C16 C25 C24 174.33(12) . . . . ?
C16 C17 C18 C19 -176.76(12) . . . . ?
C16 C17 C22 C21 176.35(11) . . . . ?
C16 C17 C22 C23 -1.89(17) . . . . ?
C17 C16 C25 C24 -1.28(19) . . . . ?
C17 C18 C19 C20 0.1(2) . . . . ?
C17 C22 C23 C24 -0.36(18) . . . . ?
C17 C22 C23 C31 177.95(11) . . . . ?
C18 C17 C22 C21 -1.33(17) . . . . ?
C18 C17 C22 C23 -179.57(11) . . . . ?
C18 C19 C20 C21 -0.45(19) . . . . ?
C18 C19 C20 C26 178.66(12) . . . . ?
C19 C20 C21 C22 -0.10(18) . . . . ?
C19 C20 C21 C29 178.61(11) . . . . ?
C19 C20 C26 C27 -178.27(12) . . . . ?
C20 C21 C22 C17 1.01(18) . . . . ?
C20 C21 C22 C23 179.26(11) . . . . ?
C20 C21 C29 C28 0.06(17) . . . . ?
C20 C21 C29 C30 -178.86(11) . . . . ?
C20 C26 C27 C28 -0.7(2) . . . . ?
C21 C20 C26 C27 0.83(19) . . . . ?
C21 C22 C23 C24 -178.61(11) . . . . ?
C21 C22 C23 C31 -0.30(17) . . . . ?
C21 C29 C30 C31 -0.54(18) . . . . ?
C22 C17 C18 C19 0.80(18) . . . . ?
C22 C21 C29 C28 178.78(11) . . . . ?
C22 C21 C29 C30 -0.15(17) . . . . ?
C22 C23 C24 C25 1.83(18) . . . . ?
C22 C23 C31 C30 -0.38(18) . . . . ?
C23 C24 C25 C16 -1.04(19) . . . . ?
C24 C23 C31 C30 177.88(12) . . . . ?
C25 C16 C17 C18 -179.77(11) . . . . ?
C25 C16 C17 C22 2.69(18) . . . . ?
C26 C20 C21 C22 -179.24(11) . . . . ?
C26 C20 C21 C29 -0.52(18) . . . . ?
C26 C27 C28 C29 0.2(2) . . . . ?
C27 C28 C29 C21 0.10(18) . . . . ?
C27 C28 C29 C30 178.98(12) . . . . ?
C28 C29 C30 C31 -179.42(12) . . . . ?
C29 C21 C22 C17 -177.70(11) . . . . ?
C29 C21 C22 C23 0.55(17) . . . . ?
C29 C30 C31 C23 0.81(19) . . . . ?
C31 C23 C24 C25 -176.43(12) . . . . ?
C32 C12 C13 C8 177.52(11) . . . . ?
C33 C32 C35 C36 55.72(16) . . . . ?
C34 C32 C35 C36 -64.51(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_usca048_0m
_database_code_depnum_ccdc_archive 'CCDC 1412213'
_audit_update_record             
;
2015-07-12 deposited with the CCDC.
2015-08-17 downloaded from the CCDC.
;
_audit_creation_date             2014-11-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H54 N2 O8'
_chemical_formula_sum            'C72 H54 N2 O8'
_chemical_formula_weight         1075.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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 0.0080 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0140 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.4849(7)
_cell_length_b                   12.6610(11)
_cell_length_c                   13.7331(12)
_cell_angle_alpha                108.388(2)
_cell_angle_beta                 98.716(2)
_cell_angle_gamma                104.328(2)
_cell_volume                     1313.5(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7606
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.043
_cell_measurement_theta_min      2.790
_shelx_estimated_absorpt_T_max   0.999
_shelx_estimated_absorpt_T_min   0.993
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/4 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0886 before and 0.0484 after correction.
The Ratio of minimum to maximum transmission is 0.9041.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21985
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        29.200
_diffrn_reflns_theta_max         29.223
_diffrn_reflns_theta_min         2.089
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Si-<111> channel cut crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_source                   synchrotron
_diffrn_special_details          ?
_reflns_number_gt                3769
_reflns_number_total             5423
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         5423
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0518
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0398P)²+0.7072P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1266
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C32A, C32B}
3. Restrained distances
 C9-O3A \\sim C9-O3B
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O4A) \\sim Ueq, Uanis(O4B) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C17A) = Uanis(C17B)
Uanis(O4A) = Uanis(O4B)
Uanis(O3A) = Uanis(O3B)
Uanis(C14A) = Uanis(C14B)
Uanis(C31A) = Uanis(C26B)
Uanis(C15A) = Uanis(C15B)
Uanis(C32A) = Uanis(C32B)
Uanis(C36A) = Uanis(C36B)
5. Same fragment restrains
{O3A, O4A, C14A, C15A, C16A, C17A, C18A, C19A, C20A, C21A, C22A, C23A, C24A,
C25A, C26A, C27A, C28A, C29A, C30A, C31A}
as
{O3B, O4B, C14B, C15B, C16B, C17B, C18B, C19B, C20B, C21B, C22B, C23B, C24B,
C25B, C26B, C27B, C28B, C29B, C30B, C31B}
{C32A, C33A, C34A, C35A, C36A}
as
{C32B, C33B, C34B, C35B, C36B}
6. Others
 Sof(O3B)=Sof(O4B)=Sof(C14B)=Sof(C15B)=Sof(H15C)=Sof(H15D)=Sof(C16B)=Sof(C17B)=
 Sof(C18B)=Sof(H18B)=Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(C21B)=Sof(C22B)=
 Sof(C23B)=Sof(C24B)=Sof(H24B)=Sof(C25B)=Sof(H25B)=Sof(C26B)=Sof(H26B)=
 Sof(C27B)=Sof(H27B)=Sof(C28B)=Sof(H28B)=Sof(C29B)=Sof(C30B)=Sof(H30B)=
 Sof(C31B)=Sof(H31B)=1-FVAR(1)
 Sof(O3A)=Sof(O4A)=Sof(C14A)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(C16A)=Sof(C17A)=
 Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(C21A)=Sof(C22A)=
 Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=
 Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(C30A)=Sof(H30A)=
 Sof(C31A)=Sof(H31A)=FVAR(1)
 Sof(C32B)=Sof(C33B)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34B)=Sof(H34D)=
 Sof(H34E)=Sof(H34F)=Sof(C35B)=Sof(H35C)=Sof(H35D)=Sof(C36B)=Sof(H36D)=
 Sof(H36E)=Sof(H36F)=1-FVAR(2)
 Sof(C32A)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34A)=Sof(H34A)=
 Sof(H34B)=Sof(H34C)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(C36A)=Sof(H36A)=
 Sof(H36B)=Sof(H36C)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C15A(H15A,H15B), C15B(H15C,H15D), C35A(H35A,H35B), C35B(H35C,H35D)
7.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C18A(H18A), C19A(H19A),
 C24A(H24A), C25A(H25A), C26A(H26A), C27A(H27A), C28A(H28A), C30A(H30A),
 C31A(H31A), C18B(H18B), C19B(H19B), C24B(H24B), C25B(H25B), C26B(H26B),
 C27B(H27B), C28B(H28B), C30B(H30B), C31B(H31B)
7.c Idealised Me refined as rotating group:
 C33A(H33A,H33B,H33C), C34A(H34A,H34B,H34C), C36A(H36A,H36B,H36C), C33B(H33D,
 H33E,H33F), C34B(H34D,H34E,H34F), C36B(H36D,H36E,H36F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.34724(18) 0.19584(12) 0.22580(11) 0.0415(4) Uani 1 1 d . . . . .
O2 O -0.00255(18) 0.40173(12) 0.33499(11) 0.0428(4) Uani 1 1 d . . . . .
N1 N 0.17156(19) 0.29856(13) 0.28139(12) 0.0295(4) Uani 1 1 d . . . . .
C1 C 0.3292(2) 0.28020(16) 0.29028(15) 0.0318(4) Uani 1 1 d . . . . .
C2 C 0.4664(2) 0.36642(15) 0.38173(14) 0.0290(4) Uani 1 1 d . . . . .
C3 C 0.4351(2) 0.46072(15) 0.45553(14) 0.0271(4) Uani 1 1 d . . . . .
C4 C 0.2765(2) 0.47699(15) 0.44135(14) 0.0291(4) Uani 1 1 d . . . . .
C5 C 0.1372(2) 0.39317(16) 0.35016(15) 0.0312(4) Uani 1 1 d . . . . .
C6 C 0.6223(2) 0.35269(16) 0.39649(15) 0.0338(4) Uani 1 1 d . . . . .
H6 H 0.6432 0.2897 0.3463 0.041 Uiso 1 1 calc R . . . .
C7 C 0.2491(2) 0.56907(16) 0.51482(15) 0.0338(4) Uani 1 1 d . . . . .
H7 H 0.1416 0.5796 0.5052 0.041 Uiso 1 1 calc R . . . .
C8 C 0.0333(2) 0.20703(15) 0.20022(15) 0.0300(4) Uani 1 1 d . . . . .
C9 C 0.0140(2) 0.19213(16) 0.09532(15) 0.0338(5) Uani 1 1 d . . . . .
C10 C -0.1086(3) 0.09809(18) 0.01878(16) 0.0395(5) Uani 1 1 d . . . . .
H10 H -0.1197 0.0875 -0.0538 0.047 Uiso 1 1 calc R . . . .
C11 C -0.2167(3) 0.01820(17) 0.04768(16) 0.0400(5) Uani 1 1 d . . . . .
H11 H -0.2998 -0.0481 -0.0058 0.048 Uiso 1 1 calc R . . . .
C12 C -0.2055(2) 0.03352(17) 0.15366(16) 0.0364(5) Uani 1 1 d . . . . .
C13 C -0.0790(2) 0.12919(17) 0.22861(16) 0.0347(5) Uani 1 1 d . . . . .
H13 H -0.0688 0.1419 0.3016 0.042 Uiso 1 1 calc R . . . .
O3A O 0.1350(8) 0.2667(5) 0.0663(8) 0.0377(11) Uani 0.721(3) 1 d . . P A 1
O4A O -0.0388(5) 0.3715(4) 0.0535(5) 0.0829(15) Uani 0.721(3) 1 d . U P A 1
C14A C 0.0955(5) 0.3591(5) 0.0524(7) 0.0435(12) Uani 0.721(3) 1 d . . P A 1
C15A C 0.2410(4) 0.4355(3) 0.0298(3) 0.0409(9) Uani 0.721(3) 1 d . . P A 1
H15A H 0.2093 0.5012 0.0174 0.049 Uiso 0.721(3) 1 calc R . P A 1
H15B H 0.2654 0.3890 -0.0356 0.049 Uiso 0.721(3) 1 calc R . P A 1
C16A C 0.3978(4) 0.4845(2) 0.1199(2) 0.0380(8) Uani 0.721(3) 1 d . . P A 1
C17A C 0.4152(18) 0.5787(15) 0.2126(11) 0.0349(9) Uani 0.721(3) 1 d . . P A 1
C18A C 0.2821(4) 0.6293(2) 0.2302(2) 0.0397(8) Uani 0.721(3) 1 d . . P A 1
H18A H 0.1789 0.5986 0.1776 0.048 Uiso 0.721(3) 1 calc R . P A 1
C19A C 0.3026(7) 0.7196(6) 0.3205(5) 0.0408(15) Uani 0.721(3) 1 d . . P A 1
H19A H 0.2124 0.7504 0.3307 0.049 Uiso 0.721(3) 1 calc R . P A 1
C20A C 0.4557(6) 0.7701(4) 0.4012(4) 0.0376(9) Uani 0.721(3) 1 d . . P A 1
C21A C 0.5900(5) 0.7238(3) 0.3866(3) 0.0347(10) Uani 0.721(3) 1 d . . P A 1
C22A C 0.5671(4) 0.6257(3) 0.2932(3) 0.0341(7) Uani 0.721(3) 1 d . . P A 1
C23A C 0.7010(7) 0.5777(5) 0.2797(4) 0.0349(14) Uani 0.721(3) 1 d . . P A 1
C24A C 0.6763(8) 0.4808(5) 0.1885(5) 0.0425(13) Uani 0.721(3) 1 d . . P A 1
H24A H 0.7618 0.4448 0.1801 0.051 Uiso 0.721(3) 1 calc R . P A 1
C25A C 0.5283(4) 0.4366(3) 0.1101(3) 0.0415(8) Uani 0.721(3) 1 d . . P A 1
H25A H 0.5153 0.3717 0.0478 0.050 Uiso 0.721(3) 1 calc R . P A 1
C26A C 0.4788(6) 0.8651(4) 0.4939(4) 0.0423(10) Uani 0.721(3) 1 d . . P A 1
H26A H 0.3885 0.8951 0.5058 0.051 Uiso 0.721(3) 1 calc R . P A 1
C27A C 0.6319(5) 0.9163(3) 0.5691(3) 0.0472(8) Uani 0.721(3) 1 d . . P A 1
H27A H 0.6457 0.9812 0.6316 0.057 Uiso 0.721(3) 1 calc R . P A 1
C28A C 0.7636(4) 0.8732(3) 0.5534(2) 0.0428(8) Uani 0.721(3) 1 d . . P A 1
H28A H 0.8687 0.9104 0.6045 0.051 Uiso 0.721(3) 1 calc R . P A 1
C29A C 0.7458(10) 0.7758(6) 0.4635(5) 0.0349(14) Uani 0.721(3) 1 d . . P A 1
C30A C 0.8776(5) 0.7255(3) 0.4464(3) 0.0406(9) Uani 0.721(3) 1 d . . P A 1
H30A H 0.9837 0.7605 0.4965 0.049 Uiso 0.721(3) 1 calc R . P A 1
C31A C 0.8540(6) 0.6300(5) 0.3612(5) 0.0434(12) Uani 0.721(3) 1 d . . P A 1
H31A H 0.9417 0.5960 0.3546 0.052 Uiso 0.721(3) 1 calc R . P A 1
O3B O 0.118(2) 0.2841(16) 0.075(2) 0.0377(11) Uani 0.279(3) 1 d . . P A 2
O4B O -0.1002(15) 0.3397(13) 0.0223(15) 0.0829(15) Uani 0.279(3) 1 d . U P A 2
C14B C 0.0454(16) 0.3509(16) 0.035(2) 0.0435(12) Uani 0.279(3) 1 d . . P A 2
C15B C 0.1762(12) 0.4524(8) 0.0308(7) 0.0409(9) Uani 0.279(3) 1 d . . P A 2
H15C H 0.2665 0.4251 0.0038 0.049 Uiso 0.279(3) 1 calc R . P A 2
H15D H 0.1250 0.4838 -0.0189 0.049 Uiso 0.279(3) 1 calc R . P A 2
C16B C 0.2501(8) 0.5477(6) 0.1381(5) 0.0373(19) Uani 0.279(3) 1 d . . P A 2
C17B C 0.407(5) 0.563(4) 0.201(3) 0.0349(9) Uani 0.279(3) 1 d . . P A 2
C18B C 0.5142(11) 0.4942(7) 0.1656(7) 0.043(2) Uani 0.279(3) 1 d . . P A 2
H18B H 0.4740 0.4289 0.1004 0.051 Uiso 0.279(3) 1 calc R . P A 2
C19B C 0.6705(14) 0.5219(11) 0.2246(10) 0.037(3) Uani 0.279(3) 1 d . . P A 2
H19B H 0.7399 0.4767 0.1988 0.045 Uiso 0.279(3) 1 calc R . P A 2
C20B C 0.7358(18) 0.6159(13) 0.3241(10) 0.035(3) Uani 0.279(3) 1 d . . P A 2
C21B C 0.6353(11) 0.6879(8) 0.3613(8) 0.041(3) Uani 0.279(3) 1 d . . P A 2
C22B C 0.4721(9) 0.6600(6) 0.2995(5) 0.0355(19) Uani 0.279(3) 1 d . . P A 2
C23B C 0.3710(15) 0.7295(13) 0.3390(12) 0.032(3) Uani 0.279(3) 1 d . . P A 2
C24B C 0.2120(13) 0.7064(8) 0.2758(8) 0.048(3) Uani 0.279(3) 1 d . . P A 2
H24B H 0.1431 0.7523 0.3010 0.057 Uiso 0.279(3) 1 calc R . P A 2
C25B C 0.1535(9) 0.6170(6) 0.1765(6) 0.042(2) Uani 0.279(3) 1 d . . P A 2
H25B H 0.0455 0.6032 0.1343 0.051 Uiso 0.279(3) 1 calc R . P A 2
C26B C 0.902(2) 0.6537(16) 0.3787(15) 0.0434(12) Uani 0.279(3) 1 d . . P A 2
H26B H 0.9753 0.6129 0.3505 0.052 Uiso 0.279(3) 1 calc R . P A 2
C27B C 0.9672(14) 0.7508(9) 0.4748(9) 0.053(3) Uani 0.279(3) 1 d . . P A 2
H27B H 1.0800 0.7717 0.5138 0.064 Uiso 0.279(3) 1 calc R . P A 2
C28B C 0.8648(14) 0.8156(8) 0.5119(7) 0.049(2) Uani 0.279(3) 1 d . . P A 2
H28B H 0.9091 0.8821 0.5761 0.059 Uiso 0.279(3) 1 calc R . P A 2
C29B C 0.698(2) 0.7855(17) 0.4574(15) 0.038(5) Uani 0.279(3) 1 d . . P A 2
C30B C 0.5904(12) 0.8516(7) 0.4978(7) 0.045(2) Uani 0.279(3) 1 d . . P A 2
H30B H 0.6288 0.9144 0.5646 0.054 Uiso 0.279(3) 1 calc R . P A 2
C31B C 0.4370(14) 0.8220(11) 0.4389(9) 0.043(3) Uani 0.279(3) 1 d . . P A 2
H31B H 0.3662 0.8656 0.4653 0.051 Uiso 0.279(3) 1 calc R . P A 2
C32A C -0.3234(3) -0.05594(19) 0.18506(18) 0.0456(5) Uani 0.879(4) 1 d . . P B
1
C33A C -0.3154(4) -0.0071(2) 0.3050(2) 0.0547(8) Uani 0.879(4) 1 d . . P B 1
H33A H -0.2015 0.0086 0.3461 0.082 Uiso 0.879(4) 1 calc GR . P B 1
H33B H -0.3952 -0.0649 0.3222 0.082 Uiso 0.879(4) 1 calc GR . P B 1
H33C H -0.3444 0.0658 0.3227 0.082 Uiso 0.879(4) 1 calc GR . P B 1
C34A C -0.5042(3) -0.0839(3) 0.1267(3) 0.0635(9) Uani 0.879(4) 1 d . . P B 1
H34A H -0.5339 -0.0114 0.1416 0.095 Uiso 0.879(4) 1 calc GR . P B 1
H34B H -0.5784 -0.1379 0.1504 0.095 Uiso 0.879(4) 1 calc GR . P B 1
H34C H -0.5170 -0.1206 0.0503 0.095 Uiso 0.879(4) 1 calc GR . P B 1
C35A C -0.2726(3) -0.1666(2) 0.1589(2) 0.0479(7) Uani 0.879(4) 1 d . . P B 1
H35A H -0.2805 -0.1974 0.0819 0.058 Uiso 0.879(4) 1 calc R . P B 1
H35B H -0.3552 -0.2260 0.1738 0.058 Uiso 0.879(4) 1 calc R . P B 1
C36A C -0.0980(16) -0.1540(15) 0.2175(10) 0.0583(8) Uani 0.879(4) 1 d . . P B 1
H36A H -0.0149 -0.0909 0.2085 0.087 Uiso 0.879(4) 1 calc GR . P B 1
H36B H -0.0735 -0.2278 0.1887 0.087 Uiso 0.879(4) 1 calc GR . P B 1
H36C H -0.0930 -0.1352 0.2930 0.087 Uiso 0.879(4) 1 calc GR . P B 1
C32B C -0.3234(3) -0.05594(19) 0.18506(18) 0.0456(5) Uani 0.121(4) 1 d . . P B
2
C33B C -0.460(2) -0.002(2) 0.218(2) 0.078(8) Uiso 0.121(4) 1 d . . P B 2
H33D H -0.4121 0.0632 0.2870 0.117 Uiso 0.121(4) 1 calc GR . P B 2
H33E H -0.5530 -0.0615 0.2237 0.117 Uiso 0.121(4) 1 calc GR . P B 2
H33F H -0.5018 0.0280 0.1649 0.117 Uiso 0.121(4) 1 calc GR . P B 2
C34B C -0.422(3) -0.1634(15) 0.0811(12) 0.070(7) Uiso 0.121(4) 1 d . . P B 2
H34D H -0.4819 -0.1373 0.0311 0.105 Uiso 0.121(4) 1 calc GR . P B 2
H34E H -0.5028 -0.2212 0.0976 0.105 Uiso 0.121(4) 1 calc GR . P B 2
H34F H -0.3429 -0.1993 0.0493 0.105 Uiso 0.121(4) 1 calc GR . P B 2
C35B C -0.233(3) -0.0985(19) 0.2587(14) 0.066(7) Uiso 0.121(4) 1 d . . P B 2
H35C H -0.3169 -0.1557 0.2751 0.079 Uiso 0.121(4) 1 calc R . P B 2
H35D H -0.1738 -0.0312 0.3259 0.079 Uiso 0.121(4) 1 calc R . P B 2
C36B C -0.106(12) -0.156(11) 0.218(8) 0.0583(8) Uani 0.121(4) 1 d . . P B 2
H36D H -0.1583 -0.2143 0.1463 0.087 Uiso 0.121(4) 1 calc GR . P B 2
H36E H -0.0689 -0.1938 0.2651 0.087 Uiso 0.121(4) 1 calc GR . P B 2
H36F H -0.0091 -0.0957 0.2164 0.087 Uiso 0.121(4) 1 calc GR . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.214(2) . ?
O2 C5 1.210(2) . ?
N1 C1 1.407(2) . ?
N1 C5 1.398(2) . ?
N1 C8 1.442(2) . ?
C1 C2 1.479(3) . ?
C2 C3 1.413(2) . ?
C2 C6 1.370(3) . ?
C3 C3 1.406(4) 2_666 ?
C3 C4 1.405(3) . ?
C4 C5 1.478(3) . ?
C4 C7 1.376(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.399(3) 2_666 ?
C7 C6 1.399(3) 2_666 ?
C7 H7 0.9500 . ?
C8 C9 1.371(3) . ?
C8 C13 1.386(2) . ?
C9 C10 1.368(3) . ?
C9 O3A 1.409(4) . ?
C9 O3B 1.408(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.388(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.391(3) . ?
C12 C13 1.383(3) . ?
C12 C32A 1.532(3) . ?
C12 C32B 1.532(3) . ?
C13 H13 0.9500 . ?
O3A C14A 1.354(5) . ?
O4A C14A 1.190(5) . ?
C14A C15A 1.506(5) . ?
C15A H15A 0.9900 . ?
C15A H15B 0.9900 . ?
C15A C16A 1.514(5) . ?
C16A C17A 1.402(7) . ?
C16A C25A 1.392(4) . ?
C17A C18A 1.445(10) . ?
C17A C22A 1.418(6) . ?
C18A H18A 0.9500 . ?
C18A C19A 1.347(6) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.425(6) . ?
C20A C21A 1.417(5) . ?
C20A C26A 1.395(5) . ?
C21A C22A 1.423(4) . ?
C21A C29A 1.416(6) . ?
C22A C23A 1.425(6) . ?
C23A C24A 1.393(6) . ?
C23A C31A 1.430(7) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.383(7) . ?
C25A H25A 0.9500 . ?
C26A H26A 0.9500 . ?
C26A C27A 1.389(6) . ?
C27A H27A 0.9500 . ?
C27A C28A 1.376(4) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.399(6) . ?
C29A C30A 1.432(9) . ?
C30A H30A 0.9500 . ?
C30A C31A 1.337(7) . ?
C31A H31A 0.9500 . ?
O3B C14B 1.354(12) . ?
O4B C14B 1.187(11) . ?
C14B C15B 1.499(11) . ?
C15B H15C 0.9900 . ?
C15B H15D 0.9900 . ?
C15B C16B 1.498(10) . ?
C16B C17B 1.405(14) . ?
C16B C25B 1.384(9) . ?
C17B C18B 1.44(2) . ?
C17B C22B 1.425(12) . ?
C18B H18B 0.9500 . ?
C18B C19B 1.343(12) . ?
C19B H19B 0.9500 . ?
C19B C20B 1.417(11) . ?
C20B C21B 1.428(12) . ?
C20B C26B 1.381(13) . ?
C21B C22B 1.406(10) . ?
C21B C29B 1.409(12) . ?
C22B C23B 1.420(11) . ?
C23B C24B 1.396(11) . ?
C23B C31B 1.413(13) . ?
C24B H24B 0.9500 . ?
C24B C25B 1.389(10) . ?
C25B H25B 0.9500 . ?
C26B H26B 0.9500 . ?
C26B C27B 1.407(14) . ?
C27B H27B 0.9500 . ?
C27B C28B 1.382(11) . ?
C28B H28B 0.9500 . ?
C28B C29B 1.390(12) . ?
C29B C30B 1.445(15) . ?
C30B H30B 0.9500 . ?
C30B C31B 1.318(12) . ?
C31B H31B 0.9500 . ?
C32A C33A 1.551(3) . ?
C32A C34A 1.517(3) . ?
C32A C35A 1.518(3) . ?
C33A H33A 0.9800 . ?
C33A H33B 0.9800 . ?
C33A H33C 0.9800 . ?
C34A H34A 0.9800 . ?
C34A H34B 0.9800 . ?
C34A H34C 0.9800 . ?
C35A H35A 0.9900 . ?
C35A H35B 0.9900 . ?
C35A C36A 1.519(11) . ?
C36A H36A 0.9800 . ?
C36A H36B 0.9800 . ?
C36A H36C 0.9800 . ?
C32B C33B 1.544(10) . ?
C32B C34B 1.562(10) . ?
C32B C35B 1.488(10) . ?
C33B H33D 0.9800 . ?
C33B H33E 0.9800 . ?
C33B H33F 0.9800 . ?
C34B H34D 0.9800 . ?
C34B H34E 0.9800 . ?
C34B H34F 0.9800 . ?
C35B H35C 0.9900 . ?
C35B H35D 0.9900 . ?
C35B C36B 1.519(15) . ?
C36B H36D 0.9800 . ?
C36B H36E 0.9800 . ?
C36B H36F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C8 116.64(15) . . ?
C5 N1 C1 125.02(16) . . ?
C5 N1 C8 118.12(15) . . ?
O1 C1 N1 120.24(18) . . ?
O1 C1 C2 123.02(18) . . ?
N1 C1 C2 116.73(16) . . ?
C3 C2 C1 120.01(17) . . ?
C6 C2 C1 119.87(17) . . ?
C6 C2 C3 120.09(17) . . ?
C3 C3 C2 119.4(2) 2_666 . ?
C4 C3 C2 120.99(17) . . ?
C4 C3 C3 119.6(2) . 2_666 ?
C3 C4 C5 120.33(16) . . ?
C7 C4 C3 119.82(17) . . ?
C7 C4 C5 119.81(17) . . ?
O2 C5 N1 119.96(18) . . ?
O2 C5 C4 123.17(17) . . ?
N1 C5 C4 116.85(17) . . ?
C2 C6 H6 119.9 . . ?
C2 C6 C7 120.29(18) . 2_666 ?
C7 C6 H6 119.9 2_666 . ?
C4 C7 C6 120.79(18) . 2_666 ?
C4 C7 H7 119.6 . . ?
C6 C7 H7 119.6 2_666 . ?
C9 C8 N1 121.67(16) . . ?
C9 C8 C13 119.22(17) . . ?
C13 C8 N1 119.05(16) . . ?
C8 C9 O3A 118.9(4) . . ?
C8 C9 O3B 115.4(12) . . ?
C10 C9 C8 120.62(17) . . ?
C10 C9 O3A 120.0(4) . . ?
C10 C9 O3B 123.8(12) . . ?
C9 C10 H10 120.1 . . ?
C9 C10 C11 119.71(18) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 H11 119.4 . . ?
C10 C11 C12 121.15(19) . . ?
C12 C11 H11 119.4 . . ?
C11 C12 C32A 120.93(18) . . ?
C11 C12 C32B 120.93(18) . . ?
C13 C12 C11 117.34(17) . . ?
C13 C12 C32A 121.65(18) . . ?
C13 C12 C32B 121.65(18) . . ?
C8 C13 H13 119.1 . . ?
C12 C13 C8 121.83(18) . . ?
C12 C13 H13 119.1 . . ?
C14A O3A C9 115.8(4) . . ?
O3A C14A C15A 109.8(4) . . ?
O4A C14A O3A 123.0(5) . . ?
O4A C14A C15A 127.1(4) . . ?
C14A C15A H15A 109.1 . . ?
C14A C15A H15B 109.1 . . ?
C14A C15A C16A 112.3(3) . . ?
H15A C15A H15B 107.9 . . ?
C16A C15A H15A 109.1 . . ?
C16A C15A H15B 109.1 . . ?
C17A C16A C15A 121.1(4) . . ?
C25A C16A C15A 119.7(3) . . ?
C25A C16A C17A 119.2(5) . . ?
C16A C17A C18A 122.2(4) . . ?
C16A C17A C22A 119.5(7) . . ?
C22A C17A C18A 118.3(5) . . ?
C17A C18A H18A 119.6 . . ?
C19A C18A C17A 120.7(4) . . ?
C19A C18A H18A 119.6 . . ?
C18A C19A H19A 119.1 . . ?
C18A C19A C20A 121.9(5) . . ?
C20A C19A H19A 119.1 . . ?
C21A C20A C19A 119.2(5) . . ?
C26A C20A C19A 122.1(5) . . ?
C26A C20A C21A 118.7(5) . . ?
C20A C21A C22A 119.2(4) . . ?
C29A C21A C20A 120.2(5) . . ?
C29A C21A C22A 120.5(4) . . ?
C17A C22A C21A 120.6(4) . . ?
C17A C22A C23A 120.2(5) . . ?
C21A C22A C23A 119.2(4) . . ?
C22A C23A C31A 118.5(5) . . ?
C24A C23A C22A 118.7(5) . . ?
C24A C23A C31A 122.8(5) . . ?
C23A C24A H24A 119.8 . . ?
C25A C24A C23A 120.4(5) . . ?
C25A C24A H24A 119.8 . . ?
C16A C25A H25A 119.0 . . ?
C24A C25A C16A 121.9(4) . . ?
C24A C25A H25A 119.0 . . ?
C20A C26A H26A 119.5 . . ?
C27A C26A C20A 121.0(4) . . ?
C27A C26A H26A 119.5 . . ?
C26A C27A H27A 119.9 . . ?
C28A C27A C26A 120.2(3) . . ?
C28A C27A H27A 119.9 . . ?
C27A C28A H28A 119.4 . . ?
C27A C28A C29A 121.2(4) . . ?
C29A C28A H28A 119.4 . . ?
C21A C29A C30A 118.5(4) . . ?
C28A C29A C21A 118.6(6) . . ?
C28A C29A C30A 122.9(5) . . ?
C29A C30A H30A 119.4 . . ?
C31A C30A C29A 121.2(4) . . ?
C31A C30A H30A 119.4 . . ?
C23A C31A H31A 119.0 . . ?
C30A C31A C23A 122.1(5) . . ?
C30A C31A H31A 119.0 . . ?
C14B O3B C9 118.7(13) . . ?
O3B C14B C15B 110.9(10) . . ?
O4B C14B O3B 122.8(14) . . ?
O4B C14B C15B 125.2(13) . . ?
C14B C15B H15C 109.4 . . ?
C14B C15B H15D 109.4 . . ?
H15C C15B H15D 108.0 . . ?
C16B C15B C14B 111.1(12) . . ?
C16B C15B H15C 109.4 . . ?
C16B C15B H15D 109.4 . . ?
C17B C16B C15B 122.0(9) . . ?
C25B C16B C15B 117.5(7) . . ?
C25B C16B C17B 120.4(10) . . ?
C16B C17B C18B 123.2(12) . . ?
C16B C17B C22B 118.4(15) . . ?
C22B C17B C18B 118.1(12) . . ?
C17B C18B H18B 119.9 . . ?
C19B C18B C17B 120.2(10) . . ?
C19B C18B H18B 119.9 . . ?
C18B C19B H19B 118.7 . . ?
C18B C19B C20B 122.5(11) . . ?
C20B C19B H19B 118.7 . . ?
C19B C20B C21B 119.1(12) . . ?
C26B C20B C19B 122.5(12) . . ?
C26B C20B C21B 117.4(12) . . ?
C22B C21B C20B 118.6(9) . . ?
C22B C21B C29B 120.4(10) . . ?
C29B C21B C20B 120.9(9) . . ?
C21B C22B C17B 121.4(11) . . ?
C21B C22B C23B 118.2(8) . . ?
C23B C22B C17B 120.4(12) . . ?
C24B C23B C22B 118.6(11) . . ?
C24B C23B C31B 122.4(11) . . ?
C31B C23B C22B 118.9(11) . . ?
C23B C24B H24B 119.6 . . ?
C25B C24B C23B 120.7(11) . . ?
C25B C24B H24B 119.6 . . ?
C16B C25B C24B 121.0(7) . . ?
C16B C25B H25B 119.5 . . ?
C24B C25B H25B 119.5 . . ?
C20B C26B H26B 119.1 . . ?
C20B C26B C27B 121.8(15) . . ?
C27B C26B H26B 119.1 . . ?
C26B C27B H27B 120.4 . . ?
C28B C27B C26B 119.2(11) . . ?
C28B C27B H27B 120.4 . . ?
C27B C28B H28B 119.3 . . ?
C27B C28B C29B 121.5(10) . . ?
C29B C28B H28B 119.3 . . ?
C21B C29B C30B 120.0(11) . . ?
C28B C29B C21B 118.6(12) . . ?
C28B C29B C30B 121.3(11) . . ?
C29B C30B H30B 121.0 . . ?
C31B C30B C29B 117.9(10) . . ?
C31B C30B H30B 121.0 . . ?
C23B C31B H31B 117.9 . . ?
C30B C31B C23B 124.3(13) . . ?
C30B C31B H31B 117.9 . . ?
C12 C32A C33A 111.34(18) . . ?
C34A C32A C12 110.47(18) . . ?
C34A C32A C33A 106.6(2) . . ?
C34A C32A C35A 110.2(2) . . ?
C35A C32A C12 108.93(18) . . ?
C35A C32A C33A 109.3(2) . . ?
C32A C33A H33A 109.5 . . ?
C32A C33A H33B 109.5 . . ?
C32A C33A H33C 109.5 . . ?
H33A C33A H33B 109.5 . . ?
H33A C33A H33C 109.5 . . ?
H33B C33A H33C 109.5 . . ?
C32A C34A H34A 109.5 . . ?
C32A C34A H34B 109.5 . . ?
C32A C34A H34C 109.5 . . ?
H34A C34A H34B 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
C32A C35A H35A 108.2 . . ?
C32A C35A H35B 108.2 . . ?
C32A C35A C36A 116.4(6) . . ?
H35A C35A H35B 107.3 . . ?
C36A C35A H35A 108.2 . . ?
C36A C35A H35B 108.2 . . ?
C35A C36A H36A 109.5 . . ?
C35A C36A H36B 109.5 . . ?
C35A C36A H36C 109.5 . . ?
H36A C36A H36B 109.5 . . ?
H36A C36A H36C 109.5 . . ?
H36B C36A H36C 109.5 . . ?
C12 C32B C33B 105.6(10) . . ?
C12 C32B C34B 107.1(9) . . ?
C33B C32B C34B 103.3(12) . . ?
C35B C32B C12 113.2(9) . . ?
C35B C32B C33B 118.7(12) . . ?
C35B C32B C34B 108.1(12) . . ?
C32B C33B H33D 109.5 . . ?
C32B C33B H33E 109.5 . . ?
C32B C33B H33F 109.5 . . ?
H33D C33B H33E 109.5 . . ?
H33D C33B H33F 109.5 . . ?
H33E C33B H33F 109.5 . . ?
C32B C34B H34D 109.5 . . ?
C32B C34B H34E 109.5 . . ?
C32B C34B H34F 109.5 . . ?
H34D C34B H34E 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?
C32B C35B H35C 108.4 . . ?
C32B C35B H35D 108.4 . . ?
C32B C35B C36B 115(3) . . ?
H35C C35B H35D 107.5 . . ?
C36B C35B H35C 108.4 . . ?
C36B C35B H35D 108.4 . . ?
C35B C36B H36D 109.5 . . ?
C35B C36B H36E 109.5 . . ?
C35B C36B H36F 109.5 . . ?
H36D C36B H36E 109.5 . . ?
H36D C36B H36F 109.5 . . ?
H36E C36B H36F 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
O1 C1 C2 C3 -178.11(17) . . . . ?
O1 C1 C2 C6 -0.1(3) . . . . ?
N1 C1 C2 C3 0.7(2) . . . . ?
N1 C1 C2 C6 178.72(16) . . . . ?
N1 C8 C9 C10 173.69(18) . . . . ?
N1 C8 C9 O3A 1.5(4) . . . . ?
N1 C8 C9 O3B -11.6(8) . . . . ?
N1 C8 C13 C12 -174.27(18) . . . . ?
C1 N1 C5 O2 179.20(17) . . . . ?
C1 N1 C5 C4 -2.7(2) . . . . ?
C1 N1 C8 C9 -76.1(2) . . . . ?
C1 N1 C8 C13 101.2(2) . . . . ?
C1 C2 C3 C3 177.37(18) . . . 2_666 ?
C1 C2 C3 C4 -2.6(2) . . . . ?
C1 C2 C6 C7 -177.26(16) . . . 2_666 ?
C2 C3 C4 C5 1.9(2) . . . . ?
C2 C3 C4 C7 179.53(16) . . . . ?
C3 C2 C6 C7 0.8(3) . . . 2_666 ?
C3 C3 C4 C5 -178.05(18) 2_666 . . . ?
C3 C3 C4 C7 -0.4(3) 2_666 . . . ?
C3 C4 C5 O2 178.73(17) . . . . ?
C3 C4 C5 N1 0.7(2) . . . . ?
C3 C4 C7 C6 0.3(3) . . . 2_666 ?
C5 N1 C1 O1 -179.17(16) . . . . ?
C5 N1 C1 C2 2.0(2) . . . . ?
C5 N1 C8 C9 109.1(2) . . . . ?
C5 N1 C8 C13 -73.7(2) . . . . ?
C5 C4 C7 C6 177.97(17) . . . 2_666 ?
C6 C2 C3 C3 -0.6(3) . . . 2_666 ?
C6 C2 C3 C4 179.42(16) . . . . ?
C7 C4 C5 O2 1.1(3) . . . . ?
C7 C4 C5 N1 -176.99(15) . . . . ?
C8 N1 C1 O1 6.4(2) . . . . ?
C8 N1 C1 C2 -172.49(14) . . . . ?
C8 N1 C5 O2 -6.4(2) . . . . ?
C8 N1 C5 C4 171.75(15) . . . . ?
C8 C9 C10 C11 1.3(3) . . . . ?
C8 C9 O3A C14A -97.6(8) . . . . ?
C8 C9 O3B C14B -112(2) . . . . ?
C9 C8 C13 C12 3.1(3) . . . . ?
C9 C10 C11 C12 1.6(3) . . . . ?
C9 O3A C14A O4A -7.5(13) . . . . ?
C9 O3A C14A C15A 175.8(6) . . . . ?
C9 O3B C14B O4B 4(4) . . . . ?
C9 O3B C14B C15B 173.3(18) . . . . ?
C10 C9 O3A C14A 90.2(8) . . . . ?
C10 C9 O3B C14B 62(3) . . . . ?
C10 C11 C12 C13 -2.1(3) . . . . ?
C10 C11 C12 C32A -179.0(2) . . . . ?
C10 C11 C12 C32B -179.0(2) . . . . ?
C11 C12 C13 C8 -0.2(3) . . . . ?
C11 C12 C32A C33A -167.1(2) . . . . ?
C11 C12 C32A C34A -48.8(3) . . . . ?
C11 C12 C32A C35A 72.4(3) . . . . ?
C11 C12 C32B C33B -100.9(10) . . . . ?
C11 C12 C32B C34B 8.7(9) . . . . ?
C11 C12 C32B C35B 127.7(9) . . . . ?
C12 C32A C35A C36A 62.7(5) . . . . ?
C12 C32B C35B C36B -58(6) . . . . ?
C13 C8 C9 C10 -3.6(3) . . . . ?
C13 C8 C9 O3A -175.8(3) . . . . ?
C13 C8 C9 O3B 171.1(8) . . . . ?
C13 C12 C32A C33A 16.2(3) . . . . ?
C13 C12 C32A C34A 134.4(2) . . . . ?
C13 C12 C32A C35A -104.4(2) . . . . ?
C13 C12 C32B C33B 82.4(10) . . . . ?
C13 C12 C32B C34B -168.1(9) . . . . ?
C13 C12 C32B C35B -49.1(10) . . . . ?
O3A C9 C10 C11 173.4(3) . . . . ?
O3A C14A C15A C16A -60.8(8) . . . . ?
O4A C14A C15A C16A 122.7(7) . . . . ?
C14A C15A C16A C17A -77.0(15) . . . . ?
C14A C15A C16A C25A 104.0(4) . . . . ?
C15A C16A C17A C18A 4(3) . . . . ?
C15A C16A C17A C22A -177.1(13) . . . . ?
C15A C16A C25A C24A 177.8(4) . . . . ?
C16A C17A C18A C19A 179.7(15) . . . . ?
C16A C17A C22A C21A 177.9(14) . . . . ?
C16A C17A C22A C23A 0(3) . . . . ?
C17A C16A C25A C24A -1.3(14) . . . . ?
C17A C18A C19A C20A 1.1(16) . . . . ?
C17A C22A C23A C24A -3.0(15) . . . . ?
C17A C22A C23A C31A 178.0(14) . . . . ?
C18A C17A C22A C21A -3(3) . . . . ?
C18A C17A C22A C23A 179.3(13) . . . . ?
C18A C19A C20A C21A -0.5(8) . . . . ?
C18A C19A C20A C26A 178.7(4) . . . . ?
C19A C20A C21A C22A -1.8(6) . . . . ?
C19A C20A C21A C29A 177.2(6) . . . . ?
C19A C20A C26A C27A -177.0(4) . . . . ?
C20A C21A C22A C17A 3.5(14) . . . . ?
C20A C21A C22A C23A -178.7(3) . . . . ?
C20A C21A C29A C28A -0.1(10) . . . . ?
C20A C21A C29A C30A 179.3(6) . . . . ?
C20A C26A C27A C28A -0.4(5) . . . . ?
C21A C20A C26A C27A 2.2(5) . . . . ?
C21A C22A C23A C24A 179.2(4) . . . . ?
C21A C22A C23A C31A 0.2(6) . . . . ?
C21A C29A C30A C31A -1.5(11) . . . . ?
C22A C17A C18A C19A 1(3) . . . . ?
C22A C21A C29A C28A 179.0(5) . . . . ?
C22A C21A C29A C30A -1.7(10) . . . . ?
C22A C23A C24A C25A 3.7(7) . . . . ?
C22A C23A C31A C30A -3.3(9) . . . . ?
C23A C24A C25A C16A -1.6(7) . . . . ?
C24A C23A C31A C30A 177.7(5) . . . . ?
C25A C16A C17A C18A -177.1(15) . . . . ?
C25A C16A C17A C22A 2(3) . . . . ?
C26A C20A C21A C22A 179.0(3) . . . . ?
C26A C20A C21A C29A -2.0(7) . . . . ?
C26A C27A C28A C29A -1.7(7) . . . . ?
C27A C28A C29A C21A 1.9(10) . . . . ?
C27A C28A C29A C30A -177.3(6) . . . . ?
C28A C29A C30A C31A 177.8(7) . . . . ?
C29A C21A C22A C17A -175.6(15) . . . . ?
C29A C21A C22A C23A 2.3(7) . . . . ?
C29A C30A C31A C23A 4.0(10) . . . . ?
C31A C23A C24A C25A -177.3(5) . . . . ?
O3B C9 C10 C11 -172.9(9) . . . . ?
O3B C14B C15B C16B -78(2) . . . . ?
O4B C14B C15B C16B 91(3) . . . . ?
C14B C15B C16B C17B 101(4) . . . . ?
C14B C15B C16B C25B -75.4(11) . . . . ?
C15B C16B C17B C18B 4(8) . . . . ?
C15B C16B C17B C22B 177(3) . . . . ?
C15B C16B C25B C24B 179.3(8) . . . . ?
C16B C17B C18B C19B 173(4) . . . . ?
C16B C17B C22B C21B -174(4) . . . . ?
C16B C17B C22B C23B 8(7) . . . . ?
C17B C16B C25B C24B 3(4) . . . . ?
C17B C18B C19B C20B 2(4) . . . . ?
C17B C22B C23B C24B -4(4) . . . . ?
C17B C22B C23B C31B 178(4) . . . . ?
C18B C17B C22B C21B 0(7) . . . . ?
C18B C17B C22B C23B -179(4) . . . . ?
C18B C19B C20B C21B -3(2) . . . . ?
C18B C19B C20B C26B -171.7(16) . . . . ?
C19B C20B C21B C22B 2(2) . . . . ?
C19B C20B C21B C29B -177.1(18) . . . . ?
C19B C20B C26B C27B 176.8(16) . . . . ?
C20B C21B C22B C17B -1(4) . . . . ?
C20B C21B C22B C23B 177.8(13) . . . . ?
C20B C21B C29B C28B 4(3) . . . . ?
C20B C21B C29B C30B -175.2(17) . . . . ?
C20B C26B C27B C28B -5(3) . . . . ?
C21B C20B C26B C27B 8(3) . . . . ?
C21B C22B C23B C24B 176.7(13) . . . . ?
C21B C22B C23B C31B -1.1(19) . . . . ?
C21B C29B C30B C31B -4(3) . . . . ?
C22B C17B C18B C19B -1(7) . . . . ?
C22B C21B C29B C28B -175.0(16) . . . . ?
C22B C21B C29B C30B 5(3) . . . . ?
C22B C23B C24B C25B 0(2) . . . . ?
C22B C23B C31B C30B 2(2) . . . . ?
C23B C24B C25B C16B 0.7(17) . . . . ?
C24B C23B C31B C30B -175.3(13) . . . . ?
C25B C16B C17B C18B -180(4) . . . . ?
C25B C16B C17B C22B -7(7) . . . . ?
C26B C20B C21B C22B 171.7(15) . . . . ?
C26B C20B C21B C29B -8(3) . . . . ?
C26B C27B C28B C29B 1(2) . . . . ?
C27B C28B C29B C21B -1(3) . . . . ?
C27B C28B C29B C30B 178.4(15) . . . . ?
C28B C29B C30B C31B 176.3(17) . . . . ?
C29B C21B C22B C17B 178(4) . . . . ?
C29B C21B C22B C23B -2.8(19) . . . . ?
C29B C30B C31B C23B 0(2) . . . . ?
C31B C23B C24B C25B 177.9(10) . . . . ?
C32A C12 C13 C8 176.64(19) . . . . ?
C33A C32A C35A C36A -59.1(5) . . . . ?
C34A C32A C35A C36A -175.9(5) . . . . ?
C32B C12 C13 C8 176.64(19) . . . . ?
C33B C32B C35B C36B 177(6) . . . . ?
C34B C32B C35B C36B 60(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_btma25s
_database_code_depnum_ccdc_archive 'CCDC 1412214'
_audit_update_record             
;
2015-07-12 deposited with the CCDC.
2015-08-17 downloaded from the CCDC.
;
_audit_creation_date             2013-07-09
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C40 H38 N2 O8'
_chemical_formula_sum            'C40 H38 N2 O8'
_chemical_formula_weight         674.72
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   9.0743(16)
_cell_length_b                   15.186(3)
_cell_length_c                   12.460(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.575(3)
_cell_angle_gamma                90.00
_cell_volume                     1645.8(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7254
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.34
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.893069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0663 before and 0.0304 after correction.
The Ratio of minimum to maximum transmission is 0.8931.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.24
_exptl_special_details           
;
 The data collection nominally covered a full sphere of reciprocal space by
 a combination of 5 sets of ω and φ scans each set at different φ and/or
 ω angles and each scan (8 s exposure) covering -0.500° degrees.
 The crystal to detector distance was 4.956 cm.
;
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23130
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         2.17
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_target            Mo
_diffrn_source_voltage           45.0
_diffrn_special_details          ?
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                2933
_reflns_number_total             3402
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3402
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0458
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0699P)²+0.7587P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1263
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C10(H10), C11(H11), C13(H13)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.59026(13) 0.29513(7) 0.30137(9) 0.0281(3) Uani 1 1 d . . .
O2 O 0.29191(13) 0.53012(7) 0.15483(8) 0.0275(3) Uani 1 1 d . . .
O3 O 0.61860(12) 0.44308(7) 0.08850(9) 0.0255(3) Uani 1 1 d . . .
O4 O 0.79494(14) 0.33735(8) 0.09400(11) 0.0379(3) Uani 1 1 d . . .
N1 N 0.43605(14) 0.41108(8) 0.22969(9) 0.0206(3) Uani 1 1 d . . .
C1 C 0.53311(16) 0.36347(10) 0.31903(12) 0.0210(3) Uani 1 1 d . . .
C2 C 0.55488(16) 0.40068(10) 0.43284(11) 0.0196(3) Uani 1 1 d . . .
C3 C 0.48887(15) 0.48269(9) 0.44559(11) 0.0183(3) Uani 1 1 d . . .
C4 C 0.40089(16) 0.53105(9) 0.35186(11) 0.0196(3) Uani 1 1 d . . .
C5 C 0.37049(16) 0.49340(10) 0.23759(12) 0.0209(3) Uani 1 1 d . . .
C6 C 0.63780(17) 0.35384(10) 0.52536(12) 0.0223(3) Uani 1 1 d . . .
H6 H 0.6806 0.2983 0.5158 0.027 Uiso 1 1 calc R . .
C7 C 0.34081(17) 0.61214(10) 0.36648(12) 0.0228(3) Uani 1 1 d . . .
H7 H 0.2848 0.6451 0.3032 0.027 Uiso 1 1 calc R . .
C8 C 0.40133(17) 0.37043(10) 0.11992(12) 0.0213(3) Uani 1 1 d . . .
C9 C 0.49676(17) 0.38413(10) 0.05258(12) 0.0225(3) Uani 1 1 d . . .
C10 C 0.46232(17) 0.34487(10) -0.05178(12) 0.0244(3) Uani 1 1 d . . .
H10 H 0.5264 0.3545 -0.0991 0.029 Uiso 1 1 calc R . .
C11 C 0.33377(17) 0.29136(10) -0.08694(12) 0.0241(3) Uani 1 1 d . . .
H11 H 0.3113 0.2646 -0.1587 0.029 Uiso 1 1 calc R . .
C12 C 0.23619(16) 0.27552(10) -0.02017(12) 0.0220(3) Uani 1 1 d . . .
C13 C 0.27317(17) 0.31756(10) 0.08415(12) 0.0222(3) Uani 1 1 d . . .
H13 H 0.2085 0.3095 0.1313 0.027 Uiso 1 1 calc R . .
C14 C 0.76487(18) 0.41340(11) 0.09879(12) 0.0259(3) Uani 1 1 d . . .
C15 C 0.87435(18) 0.48877(11) 0.11534(13) 0.0284(4) Uani 1 1 d . . .
H15A H 0.8632 0.5257 0.1771 0.043 Uiso 1 1 calc R . .
H15B H 0.8520 0.5239 0.0466 0.043 Uiso 1 1 calc R . .
H15C H 0.9798 0.4663 0.1332 0.043 Uiso 1 1 calc R . .
C16 C 0.08973(17) 0.22049(11) -0.06132(12) 0.0261(3) Uani 1 1 d . . .
C17 C -0.0426(2) 0.28373(14) -0.11360(18) 0.0451(5) Uani 1 1 d . . .
H17A H -0.0206 0.3155 -0.1757 0.068 Uiso 1 1 calc R . .
H17B H -0.0537 0.3259 -0.0569 0.068 Uiso 1 1 calc R . .
H17C H -0.1382 0.2503 -0.1416 0.068 Uiso 1 1 calc R . .
C18 C 0.1014(2) 0.15422(14) -0.15136(16) 0.0421(5) Uani 1 1 d . . .
H18A H 0.1973 0.1207 -0.1248 0.063 Uiso 1 1 calc R . .
H18B H 0.1007 0.1858 -0.2201 0.063 Uiso 1 1 calc R . .
H18C H 0.0138 0.1137 -0.1668 0.063 Uiso 1 1 calc R . .
C19 C 0.0533(2) 0.16945(12) 0.03455(14) 0.0329(4) Uani 1 1 d . . .
H19A H 0.0388 0.2123 0.0905 0.039 Uiso 1 1 calc R . .
H19B H -0.0453 0.1379 0.0041 0.039 Uiso 1 1 calc R . .
C20 C 0.1750(3) 0.10313(15) 0.09380(19) 0.0540(6) Uani 1 1 d . . .
H20A H 0.2734 0.1334 0.1246 0.081 Uiso 1 1 calc R . .
H20B H 0.1862 0.0582 0.0403 0.081 Uiso 1 1 calc R . .
H20C H 0.1437 0.0751 0.1547 0.081 Uiso 1 1 calc R . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.2082(18) . ?
O2 C5 1.2097(17) . ?
O3 C9 1.3935(18) . ?
O3 C14 1.3727(19) . ?
O4 C14 1.192(2) . ?
N1 C1 1.4065(18) . ?
N1 C5 1.3999(19) . ?
N1 C8 1.4511(18) . ?
C1 C2 1.4865(19) . ?
C2 C3 1.410(2) . ?
C2 C6 1.381(2) . ?
C3 C3 1.414(3) 3_666 ?
C3 C4 1.4173(19) . ?
C4 C5 1.4854(19) . ?
C4 C7 1.380(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.404(2) 3_666 ?
C7 C6 1.404(2) 3_666 ?
C7 H7 0.9500 . ?
C8 C9 1.383(2) . ?
C8 C13 1.378(2) . ?
C9 C10 1.383(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.386(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.398(2) . ?
C12 C13 1.400(2) . ?
C12 C16 1.529(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.491(2) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.530(2) . ?
C16 C18 1.533(2) . ?
C16 C19 1.537(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.521(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 O3 C9 118.46(12) . . ?
C1 N1 C8 116.48(12) . . ?
C5 N1 C1 125.88(12) . . ?
C5 N1 C8 117.64(11) . . ?
O1 C1 N1 120.12(13) . . ?
O1 C1 C2 123.59(13) . . ?
N1 C1 C2 116.26(13) . . ?
C3 C2 C1 119.86(12) . . ?
C6 C2 C1 119.55(13) . . ?
C6 C2 C3 120.58(13) . . ?
C2 C3 C3 119.16(16) . 3_666 ?
C2 C3 C4 121.48(13) . . ?
C3 C3 C4 119.36(16) 3_666 . ?
C3 C4 C5 119.83(13) . . ?
C7 C4 C3 120.31(13) . . ?
C7 C4 C5 119.86(13) . . ?
O2 C5 N1 120.72(13) . . ?
O2 C5 C4 122.87(14) . . ?
N1 C5 C4 116.40(12) . . ?
C2 C6 H6 119.8 . . ?
C2 C6 C7 120.34(14) . 3_666 ?
C7 C6 H6 119.8 3_666 . ?
C4 C7 C6 120.23(13) . 3_666 ?
C4 C7 H7 119.9 . . ?
C6 C7 H7 119.9 3_666 . ?
C9 C8 N1 120.20(13) . . ?
C13 C8 N1 119.26(13) . . ?
C13 C8 C9 120.54(13) . . ?
C8 C9 O3 118.60(13) . . ?
C8 C9 C10 119.55(14) . . ?
C10 C9 O3 121.65(13) . . ?
C9 C10 H10 120.2 . . ?
C9 C10 C11 119.60(14) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 H11 118.9 . . ?
C10 C11 C12 122.11(13) . . ?
C12 C11 H11 118.9 . . ?
C11 C12 C13 116.69(14) . . ?
C11 C12 C16 122.14(13) . . ?
C13 C12 C16 121.03(13) . . ?
C8 C13 C12 121.49(14) . . ?
C8 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
O3 C14 C15 110.44(13) . . ?
O4 C14 O3 122.85(14) . . ?
O4 C14 C15 126.71(15) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C16 C17 107.52(13) . . ?
C12 C16 C18 111.66(13) . . ?
C12 C16 C19 111.96(12) . . ?
C17 C16 C18 108.07(15) . . ?
C17 C16 C19 109.31(14) . . ?
C18 C16 C19 108.23(14) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 108.5 . . ?
C16 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C20 C19 C16 115.08(15) . . ?
C20 C19 H19A 108.5 . . ?
C20 C19 H19B 108.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

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
O1 C1 C2 C3 177.49(14) . . . . ?
O1 C1 C2 C6 -3.5(2) . . . . ?
O3 C9 C10 C11 -175.60(13) . . . . ?
N1 C1 C2 C3 -4.5(2) . . . . ?
N1 C1 C2 C6 174.48(13) . . . . ?
N1 C8 C9 O3 -5.2(2) . . . . ?
N1 C8 C9 C10 179.92(13) . . . . ?
N1 C8 C13 C12 -178.81(13) . . . . ?
C1 N1 C5 O2 177.79(14) . . . . ?
C1 N1 C5 C4 -3.2(2) . . . . ?
C1 N1 C8 C9 -88.08(17) . . . . ?
C1 N1 C8 C13 91.37(16) . . . . ?
C1 C2 C3 C3 -179.77(15) . . . 3_666 ?
C1 C2 C3 C4 0.2(2) . . . . ?
C1 C2 C6 C7 -179.84(13) . . . 3_666 ?
C2 C3 C4 C5 2.9(2) . . . . ?
C2 C3 C4 C7 -178.37(13) . . . . ?
C3 C2 C6 C7 -0.8(2) . . . 3_666 ?
C3 C3 C4 C5 -177.09(15) 3_666 . . . ?
C3 C3 C4 C7 1.6(2) 3_666 . . . ?
C3 C4 C5 O2 177.40(14) . . . . ?
C3 C4 C5 N1 -1.6(2) . . . . ?
C3 C4 C7 C6 -2.0(2) . . . 3_666 ?
C5 N1 C1 O1 -175.75(13) . . . . ?
C5 N1 C1 C2 6.2(2) . . . . ?
C5 N1 C8 C9 92.04(17) . . . . ?
C5 N1 C8 C13 -88.51(17) . . . . ?
C5 C4 C7 C6 176.67(13) . . . 3_666 ?
C6 C2 C3 C3 1.2(2) . . . 3_666 ?
C6 C2 C3 C4 -178.79(13) . . . . ?
C7 C4 C5 O2 -1.3(2) . . . . ?
C7 C4 C5 N1 179.71(13) . . . . ?
C8 N1 C1 O1 4.4(2) . . . . ?
C8 N1 C1 C2 -173.67(12) . . . . ?
C8 N1 C5 O2 -2.3(2) . . . . ?
C8 N1 C5 C4 176.66(12) . . . . ?
C8 C9 C10 C11 -0.9(2) . . . . ?
C9 O3 C14 O4 -11.0(2) . . . . ?
C9 O3 C14 C15 168.60(12) . . . . ?
C9 C8 C13 C12 0.6(2) . . . . ?
C9 C10 C11 C12 0.1(2) . . . . ?
C10 C11 C12 C13 0.9(2) . . . . ?
C10 C11 C12 C16 176.68(14) . . . . ?
C11 C12 C13 C8 -1.3(2) . . . . ?
C11 C12 C16 C17 -92.26(18) . . . . ?
C11 C12 C16 C18 26.1(2) . . . . ?
C11 C12 C16 C19 147.66(15) . . . . ?
C12 C16 C19 C20 -61.5(2) . . . . ?
C13 C8 C9 O3 175.38(13) . . . . ?
C13 C8 C9 C10 0.5(2) . . . . ?
C13 C12 C16 C17 83.33(18) . . . . ?
C13 C12 C16 C18 -158.30(15) . . . . ?
C13 C12 C16 C19 -36.8(2) . . . . ?
C14 O3 C9 C8 123.15(15) . . . . ?
C14 O3 C9 C10 -62.06(18) . . . . ?
C16 C12 C13 C8 -177.12(14) . . . . ?
C17 C16 C19 C20 179.45(16) . . . . ?
C18 C16 C19 C20 61.97(19) . . . . ?

####################################################################### 
# 
# 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_dfya53m
_database_code_depnum_ccdc_archive 'CCDC 1412215'
_audit_update_record             
;
2015-07-12 deposited with the CCDC.
2015-08-17 downloaded from the CCDC.
;
_audit_creation_date             2013-11-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.13 svn.r2834 for OlexSys, GUI svn.r4705)
;
_shelxl_version_number           2013-4


# start Validation Reply Form
_vrf_PLAT201_dfya53m             
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          4 Report
RESPONSE: Disordered and fractionally occupied atoms of the disordered
acetonitrile / CH2Cl2 molecules and the -C(CH3)2CH2CH3 substituent were
refined isotropically.
;
# end Validation Reply Form

_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C72 H54 N2 O8, 1.36(C2 H3 N), 0.64(C H2 Cl2)'
_chemical_formula_sum            'C75.36 H59.36 Cl1.28 N3.36 O8'
_chemical_formula_weight         1185.35
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Cl Cl 0.1484 0.1585 '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'

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

_cell_length_a                   17.132(3)
_cell_length_b                   10.4771(16)
_cell_length_c                   17.718(3)
_cell_angle_alpha                90
_cell_angle_beta                 113.969(3)
_cell_angle_gamma                90
_cell_volume                     2906.0(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7671
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.878
_cell_measurement_theta_min      2.316
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1242
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.24
_exptl_special_details           
;
The data collection nominally covered a full sphere of reciprocal
space by a combination of 5 sets of ω and φ scans each set at
different φ and/or ω angles and each scan (10 s exposure) covering
-0.500\
egrees. The crystal to detector distance was 4.956 cm.
;
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32604
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.116
_diffrn_reflns_theta_min         2.146
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_source_current           37.0
_diffrn_source_power             1.739
_diffrn_source_voltage           47.0
_reflns_number_gt                3840
_reflns_number_total             5169
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.631 (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5169
_refine_ls_number_restraints     102
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0846
_refine_ls_restrained_S_all      1.139
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1244P)²+4.4388P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2333
_refine_ls_wR_factor_ref         0.2507
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C32A, C32B}
3. Restrained distances
 N1S-C1S
 1.13 with sigma of 0.02
 C1S-C2S
 1.445 with sigma of 0.02
 C3S-Cl1S = C3S-Cl2S
 1.76 with sigma of 0.02
 Cl1S-Cl2S
 2.93 with sigma of 0.02
 C4S-Cl3S = C4S-Cl4S
 1.76 with sigma of 0.02
 Cl3S-Cl4S
 2.93 with sigma of 0.02
 N1S-C2S
 0.02 with sigma of 2.57
 C32A-C33A \\sim C32A-C34A \\sim C32A-C35A \\sim C32B-C33B \\sim C32B-C34B
\\sim C32B-C35B
 with sigma of 0.01
 C33A-C34A \\sim C34A-C35A \\sim C35A-C33A \\sim C33B-C34B \\sim C34B-C35B
\\sim C35B-C33B
 with sigma of 0.02
 C35A-C36A \\sim C35B-C36B
 with sigma of 0.01
 C32A-C36A \\sim C32B-C36B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C32A) = Uanis(C32B)
Uiso(C33A) = Uiso(C33B)
Uiso(C2S) = Uiso(C3S) = Uiso(C4S)
5. Rigid body (RIGU) restrains
 C20, C26, C27, C28, C29, C30, C21, C19, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(N1S)+Sof(C1S)+Sof(C2S)+Sof(H2SA)+Sof(H2SB)+Sof(H2SC)]+1*[Sof(C3S)+
 Sof(H3SA)+Sof(H3SB)+Sof(Cl1S)+Sof(Cl2S)]+1*[Sof(C4S)+Sof(H4SA)+Sof(H4SB)+
 Sof(Cl3S)+Sof(Cl4S)]=1 with esd of 0.0001
 Sof(C32B)=Sof(C33B)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34B)=Sof(H34D)=
 Sof(H34E)=Sof(H34F)=Sof(C35B)=Sof(H35C)=Sof(H35D)=Sof(C36B)=Sof(H36D)=
 Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(C32A)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34A)=Sof(H34A)=
 Sof(H34B)=Sof(H34C)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(C36A)=Sof(H36A)=
 Sof(H36B)=Sof(H36C)=FVAR(1)
 Sof(N1S)=Sof(C1S)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(H2SC)=FVAR(2)
 Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(Cl1S)=Sof(Cl2S)=FVAR(3)
 Sof(C4S)=Sof(H4SA)=Sof(H4SB)=Sof(Cl3S)=Sof(Cl4S)=FVAR(4)
7.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C35A(H35A,H35B), C35B(H35C,H35D), C3S(H3SA,H3SB), C4S(H4SA,
 H4SB)
7.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C18(H18), C19(H19), C24(H24),
 C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31)
7.c Idealised Me refined with riding coordinates:
 C33A(H33A,H33B,H33C), C34A(H34A,H34B,H34C), C36A(H36A,H36B,H36C), C33B(H33D,
 H33E,H33F), C34B(H34D,H34E,H34F), C36B(H36D,H36E,H36F), C2S(H2SA,H2SB,H2SC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.23641(14) 0.4296(2) 0.40043(14) 0.0375(6) Uani 1 1 d . . . . .
O2 O 0.39664(15) 0.4562(3) 0.67610(14) 0.0451(7) Uani 1 1 d . . . . .
O3 O 0.20289(15) 0.6333(2) 0.51907(16) 0.0417(6) Uani 1 1 d . . . . .
O4 O 0.08992(16) 0.6237(3) 0.39574(19) 0.0543(8) Uani 1 1 d . . . . .
N1 N 0.31747(16) 0.4399(2) 0.53822(16) 0.0286(6) Uani 1 1 d . . . . .
C1 C 0.30645(19) 0.4446(3) 0.45540(19) 0.0278(7) Uani 1 1 d . . . . .
C2 C 0.38458(19) 0.4676(3) 0.44073(18) 0.0255(7) Uani 1 1 d . . . . .
C3 C 0.46342(18) 0.4891(3) 0.50787(18) 0.0231(6) Uani 1 1 d . . . . .
C4 C 0.47047(19) 0.4892(3) 0.59008(19) 0.0269(7) Uani 1 1 d . . . . .
C5 C 0.3947(2) 0.4616(3) 0.6073(2) 0.0302(7) Uani 1 1 d . . . . .
C6 C 0.3793(2) 0.4666(3) 0.36104(19) 0.0288(7) Uani 1 1 d . . . . .
H6 H 0.3259 0.4514 0.3162 0.035 Uiso 1 1 calc R . . . .
C7 C 0.5479(2) 0.5122(3) 0.65425(19) 0.0302(7) Uani 1 1 d . . . . .
H7 H 0.5520 0.5137 0.7094 0.036 Uiso 1 1 calc R . . . .
C8 C 0.2425(2) 0.4172(3) 0.5543(2) 0.0316(7) Uani 1 1 d . . . . .
C9 C 0.1847(2) 0.5134(3) 0.5429(2) 0.0343(8) Uani 1 1 d . . . . .
C10 C 0.1144(2) 0.4941(4) 0.5608(2) 0.0402(8) Uani 1 1 d . . . . .
H10 H 0.0737 0.5603 0.5517 0.048 Uiso 1 1 calc R . . . .
C11 C 0.1036(2) 0.3776(4) 0.5919(2) 0.0419(9) Uani 1 1 d . . . . .
H11 H 0.0557 0.3656 0.6053 0.050 Uiso 1 1 calc R . . . .
C12 C 0.1610(2) 0.2772(4) 0.6042(2) 0.0445(9) Uani 1 1 d . . . . .
C13 C 0.2308(2) 0.3003(3) 0.5845(2) 0.0390(8) Uani 1 1 d . . . . .
H13 H 0.2712 0.2341 0.5920 0.047 Uiso 1 1 calc R . . . .
C14 C 0.1507(2) 0.6797(4) 0.4430(3) 0.0464(10) Uani 1 1 d . . . . .
C15 C 0.1818(2) 0.8088(4) 0.4305(3) 0.0577(12) Uani 1 1 d . . . . .
H15A H 0.1889 0.8636 0.4783 0.069 Uiso 1 1 calc R . . . .
H15B H 0.1378 0.8485 0.3807 0.069 Uiso 1 1 calc R . . . .
C16 C 0.2659(2) 0.8050(3) 0.4205(2) 0.0425(9) Uani 1 1 d . . . . .
C17 C 0.3458(2) 0.8158(3) 0.4879(2) 0.0362(8) Uani 1 1 d . . . . .
C18 C 0.3565(3) 0.8241(4) 0.5717(3) 0.0522(10) Uani 1 1 d . . . . .
H18 H 0.3081 0.8180 0.5848 0.063 Uiso 1 1 calc R . . . .
C19 C 0.4360(4) 0.8409(4) 0.6337(3) 0.0688(13) Uani 1 1 d . . . . .
H19 H 0.4414 0.8476 0.6890 0.083 Uiso 1 1 calc R . . . .
C20 C 0.5109(3) 0.8485(4) 0.6174(4) 0.0708(13) Uani 1 1 d . . . . .
C21 C 0.5016(2) 0.8383(3) 0.5361(3) 0.0601(12) Uani 1 1 d . . . . .
C22 C 0.4204(2) 0.8209(3) 0.4715(3) 0.0422(9) Uani 1 1 d . . . . .
C23 C 0.4132(3) 0.8117(3) 0.3890(3) 0.0529(11) Uani 1 1 d . . . . .
C24 C 0.3321(3) 0.7986(4) 0.3250(3) 0.0585(11) Uani 1 1 d . . . . .
H24 H 0.3267 0.7910 0.2696 0.070 Uiso 1 1 calc R . . . .
C25 C 0.2614(3) 0.7966(4) 0.3410(3) 0.0524(10) Uani 1 1 d . . . . .
H25 H 0.2070 0.7892 0.2963 0.063 Uiso 1 1 calc R . . . .
C26 C 0.5920(4) 0.8698(5) 0.6800(5) 0.106(2) Uani 1 1 d . . . . .
H26 H 0.6005 0.8776 0.7362 0.127 Uiso 1 1 calc R . . . .
C27 C 0.6629(4) 0.8796(5) 0.6547(6) 0.107(2) Uani 1 1 d . . . . .
H27 H 0.7185 0.8941 0.6962 0.129 Uiso 1 1 calc R . . . .
C28 C 0.6540(3) 0.8692(5) 0.5754(6) 0.104(2) Uani 1 1 d . . . . .
H28 H 0.7028 0.8760 0.5629 0.125 Uiso 1 1 calc R . . . .
C29 C 0.5760(3) 0.8492(4) 0.5137(4) 0.0774(14) Uani 1 1 d . . . . .
C30 C 0.5614(4) 0.8401(4) 0.4289(5) 0.0860(16) Uani 1 1 d . . . . .
H30 H 0.6089 0.8473 0.4144 0.103 Uiso 1 1 calc R . . . .
C31 C 0.4878(4) 0.8229(4) 0.3718(4) 0.0789(15) Uani 1 1 d . . . . .
H31 H 0.4819 0.8173 0.3163 0.095 Uiso 1 1 calc R . . . .
C32A C 0.1523(2) 0.1492(4) 0.6419(3) 0.0674(14) Uani 0.565(9) 1 d . . P A 1
C33A C 0.0694(4) 0.1382(9) 0.6535(6) 0.0562(16) Uiso 0.565(9) 1 d . . P A 1
H33A H 0.0667 0.2064 0.6902 0.084 Uiso 0.565(9) 1 calc R . P A 1
H33B H 0.0673 0.0551 0.6780 0.084 Uiso 0.565(9) 1 calc R . P A 1
H33C H 0.0209 0.1459 0.5998 0.084 Uiso 0.565(9) 1 calc R . P A 1
C34A C 0.1497(6) 0.0408(8) 0.5782(5) 0.069(3) Uiso 0.565(9) 1 d . . P A 1
H34A H 0.1010 0.0554 0.5254 0.103 Uiso 0.565(9) 1 calc R . P A 1
H34B H 0.1437 -0.0427 0.6002 0.103 Uiso 0.565(9) 1 calc R . P A 1
H34C H 0.2027 0.0428 0.5697 0.103 Uiso 0.565(9) 1 calc R . P A 1
C35A C 0.2296(5) 0.1114(8) 0.7182(4) 0.066(3) Uiso 0.565(9) 1 d . . P A 1
H35A H 0.2222 0.0258 0.7381 0.079 Uiso 0.565(9) 1 calc R . P A 1
H35B H 0.2821 0.1118 0.7077 0.079 Uiso 0.565(9) 1 calc R . P A 1
C36A C 0.2325(7) 0.2132(10) 0.7786(6) 0.084(3) Uiso 0.565(9) 1 d . . P A 1
H36A H 0.2029 0.2896 0.7486 0.126 Uiso 0.565(9) 1 calc R . P A 1
H36B H 0.2921 0.2344 0.8134 0.126 Uiso 0.565(9) 1 calc R . P A 1
H36C H 0.2042 0.1824 0.8134 0.126 Uiso 0.565(9) 1 calc R . P A 1
C32B C 0.1523(2) 0.1492(4) 0.6419(3) 0.0674(14) Uani 0.435(9) 1 d . . P A 2
C33B C 0.0612(4) 0.1170(12) 0.6299(7) 0.0562(16) Uiso 0.435(9) 1 d . . P A 2
H33D H 0.0397 0.1835 0.6554 0.084 Uiso 0.435(9) 1 calc R . P A 2
H33E H 0.0607 0.0346 0.6559 0.084 Uiso 0.435(9) 1 calc R . P A 2
H33F H 0.0246 0.1122 0.5708 0.084 Uiso 0.435(9) 1 calc R . P A 2
C34B C 0.1977(8) 0.0380(10) 0.6253(8) 0.080(4) Uiso 0.435(9) 1 d . . P A 2
H34D H 0.1756 0.0230 0.5656 0.120 Uiso 0.435(9) 1 calc R . P A 2
H34E H 0.1882 -0.0381 0.6526 0.120 Uiso 0.435(9) 1 calc R . P A 2
H34F H 0.2590 0.0562 0.6467 0.120 Uiso 0.435(9) 1 calc R . P A 2
C35B C 0.2000(7) 0.1713(14) 0.7378(5) 0.087(4) Uiso 0.435(9) 1 d . . P A 2
H35C H 0.1756 0.2471 0.7538 0.104 Uiso 0.435(9) 1 calc R . P A 2
H35D H 0.1910 0.0964 0.7674 0.104 Uiso 0.435(9) 1 calc R . P A 2
C36B C 0.2938(8) 0.1908(19) 0.7626(10) 0.124(7) Uiso 0.435(9) 1 d . . P A 2
H36D H 0.3051 0.2030 0.7131 0.186 Uiso 0.435(9) 1 calc R . P A 2
H36E H 0.3251 0.1158 0.7930 0.186 Uiso 0.435(9) 1 calc R . P A 2
H36F H 0.3126 0.2665 0.7980 0.186 Uiso 0.435(9) 1 calc R . P A 2
N1S N 0.3730(4) 0.6070(7) 0.1422(4) 0.058(2) Uiso 0.680(3) 1 d D . P B 1
C1S C 0.4083(4) 0.6929(7) 0.1428(4) 0.0459(17) Uiso 0.680(3) 1 d D . P B 1
C2S C 0.4518(5) 0.8088(8) 0.1382(5) 0.0595(16) Uiso 0.680(3) 1 d D . P B 1
H2SA H 0.4096 0.8747 0.1093 0.089 Uiso 0.680(3) 1 calc R . P B 1
H2SB H 0.4876 0.7922 0.1081 0.089 Uiso 0.680(3) 1 calc R . P B 1
H2SC H 0.4876 0.8383 0.1942 0.089 Uiso 0.680(3) 1 calc R . P B 1
C3S C 0.4339(10) 0.7803(19) 0.1175(14) 0.0595(16) Uiso 0.242(3) 1 d D . P C 2
H3SA H 0.4259 0.7794 0.0590 0.071 Uiso 0.242(3) 1 calc R . P C 2
H3SB H 0.4066 0.8584 0.1270 0.071 Uiso 0.242(3) 1 calc R . P C 2
Cl1S Cl 0.3857(4) 0.6466(7) 0.1378(3) 0.0548(14) Uiso 0.242(3) 1 d D . P C 2
Cl2S Cl 0.5411(3) 0.7822(5) 0.1803(3) 0.0727(16) Uiso 0.242(3) 1 d D . P C 2
C4S C 0.453(2) 0.784(8) 0.127(4) 0.0595(16) Uiso 0.078(2) 1 d D . P D 3
H4SA H 0.4213 0.7212 0.1449 0.071 Uiso 0.078(2) 1 calc R . P D 3
H4SB H 0.4117 0.8416 0.0858 0.071 Uiso 0.078(2) 1 calc R . P D 3
Cl3S Cl 0.5129(10) 0.7040(15) 0.0813(9) 0.070(5) Uiso 0.078(2) 1 d D . P D 3
Cl4S Cl 0.5229(13) 0.8729(18) 0.2123(11) 0.086(6) Uiso 0.078(2) 1 d D . P D 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.210(4) . ?
O2 C5 1.208(4) . ?
O3 C9 1.401(4) . ?
O3 C14 1.368(5) . ?
O4 C14 1.193(5) . ?
N1 C1 1.402(4) . ?
N1 C5 1.408(4) . ?
N1 C8 1.444(4) . ?
C1 C2 1.483(4) . ?
C2 C3 1.409(4) . ?
C2 C6 1.378(4) . ?
C3 C3 1.409(6) 3_666 ?
C3 C4 1.412(4) . ?
C4 C5 1.478(4) . ?
C4 C7 1.373(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.397(4) 3_666 ?
C7 C6 1.397(4) 3_666 ?
C7 H7 0.9500 . ?
C8 C9 1.370(5) . ?
C8 C13 1.383(5) . ?
C9 C10 1.379(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.383(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.395(5) . ?
C12 C13 1.397(5) . ?
C12 C32A 1.531(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.503(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.522(5) . ?
C16 C17 1.408(5) . ?
C16 C25 1.381(6) . ?
C17 C18 1.423(6) . ?
C17 C22 1.422(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.369(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.428(8) . ?
C20 C21 1.387(8) . ?
C20 C26 1.399(7) . ?
C21 C22 1.410(5) . ?
C21 C29 1.485(7) . ?
C22 C23 1.420(6) . ?
C23 C24 1.398(6) . ?
C23 C31 1.433(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.353(6) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C26 C27 1.459(11) . ?
C27 H27 0.9500 . ?
C27 C28 1.354(11) . ?
C28 H28 0.9500 . ?
C28 C29 1.357(8) . ?
C29 C30 1.422(9) . ?
C30 H30 0.9500 . ?
C30 C31 1.269(9) . ?
C31 H31 0.9500 . ?
C32A C33A 1.520(6) . ?
C32A C34A 1.589(6) . ?
C32A C35A 1.512(6) . ?
C33A H33A 0.9800 . ?
C33A H33B 0.9800 . ?
C33A H33C 0.9800 . ?
C34A H34A 0.9800 . ?
C34A H34B 0.9800 . ?
C34A H34C 0.9800 . ?
C35A H35A 0.9900 . ?
C35A H35B 0.9900 . ?
C35A C36A 1.498(10) . ?
C36A H36A 0.9800 . ?
C36A H36B 0.9800 . ?
C36A H36C 0.9800 . ?
C33B H33D 0.9800 . ?
C33B H33E 0.9800 . ?
C33B H33F 0.9800 . ?
C34B H34D 0.9800 . ?
C34B H34E 0.9800 . ?
C34B H34F 0.9800 . ?
C35B H35C 0.9900 . ?
C35B H35D 0.9900 . ?
C35B C36B 1.499(11) . ?
C36B H36D 0.9800 . ?
C36B H36E 0.9800 . ?
C36B H36F 0.9800 . ?
N1S C1S 1.083(9) . ?
C1S C2S 1.444(10) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C3S Cl1S 1.736(17) . ?
C3S Cl2S 1.717(15) . ?
C4S H4SA 0.9900 . ?
C4S H4SB 0.9900 . ?
C4S Cl3S 1.75(2) . ?
C4S Cl4S 1.77(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 O3 C9 118.6(3) . . ?
C1 N1 C5 125.7(2) . . ?
C1 N1 C8 117.4(3) . . ?
C5 N1 C8 116.9(2) . . ?
O1 C1 N1 120.4(3) . . ?
O1 C1 C2 123.4(3) . . ?
N1 C1 C2 116.2(3) . . ?
C3 C2 C1 120.1(3) . . ?
C6 C2 C1 119.4(3) . . ?
C6 C2 C3 120.5(3) . . ?
C2 C3 C3 118.9(3) . 3_666 ?
C2 C3 C4 121.5(3) . . ?
C3 C3 C4 119.6(3) 3_666 . ?
C3 C4 C5 119.9(3) . . ?
C7 C4 C3 120.2(3) . . ?
C7 C4 C5 119.9(3) . . ?
O2 C5 N1 120.0(3) . . ?
O2 C5 C4 123.4(3) . . ?
N1 C5 C4 116.5(3) . . ?
C2 C6 H6 119.8 . . ?
C2 C6 C7 120.4(3) . 3_666 ?
C7 C6 H6 119.8 3_666 . ?
C4 C7 C6 120.4(3) . 3_666 ?
C4 C7 H7 119.8 . . ?
C6 C7 H7 119.8 3_666 . ?
C9 C8 N1 119.8(3) . . ?
C9 C8 C13 119.9(3) . . ?
C13 C8 N1 120.2(3) . . ?
C8 C9 O3 117.9(3) . . ?
C8 C9 C10 120.4(3) . . ?
C10 C9 O3 121.5(3) . . ?
C9 C10 H10 120.3 . . ?
C9 C10 C11 119.5(3) . . ?
C11 C10 H10 120.3 . . ?
C10 C11 H11 119.1 . . ?
C10 C11 C12 121.9(3) . . ?
C12 C11 H11 119.1 . . ?
C11 C12 C13 116.8(3) . . ?
C11 C12 C32A 122.8(3) . . ?
C13 C12 C32A 120.3(3) . . ?
C8 C13 C12 121.6(3) . . ?
C8 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
O3 C14 C15 109.7(3) . . ?
O4 C14 O3 123.5(3) . . ?
O4 C14 C15 126.8(4) . . ?
C14 C15 H15A 108.8 . . ?
C14 C15 H15B 108.8 . . ?
C14 C15 C16 113.8(3) . . ?
H15A C15 H15B 107.7 . . ?
C16 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
C17 C16 C15 122.6(4) . . ?
C25 C16 C15 117.1(4) . . ?
C25 C16 C17 120.2(3) . . ?
C16 C17 C18 124.0(3) . . ?
C16 C17 C22 118.3(3) . . ?
C22 C17 C18 117.7(3) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 C17 120.6(4) . . ?
C19 C18 H18 119.7 . . ?
C18 C19 H19 119.0 . . ?
C18 C19 C20 121.9(5) . . ?
C20 C19 H19 119.0 . . ?
C21 C20 C19 118.1(4) . . ?
C21 C20 C26 119.5(6) . . ?
C26 C20 C19 122.3(6) . . ?
C20 C21 C22 120.8(4) . . ?
C20 C21 C29 121.5(4) . . ?
C22 C21 C29 117.6(5) . . ?
C21 C22 C17 120.8(4) . . ?
C21 C22 C23 119.3(4) . . ?
C23 C22 C17 119.9(3) . . ?
C22 C23 C31 120.1(5) . . ?
C24 C23 C22 118.9(4) . . ?
C24 C23 C31 120.9(5) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 C23 120.7(4) . . ?
C25 C24 H24 119.6 . . ?
C16 C25 H25 119.0 . . ?
C24 C25 C16 121.9(4) . . ?
C24 C25 H25 119.0 . . ?
C20 C26 H26 121.6 . . ?
C20 C26 C27 116.8(7) . . ?
C27 C26 H26 121.6 . . ?
C26 C27 H27 118.1 . . ?
C28 C27 C26 123.8(6) . . ?
C28 C27 H27 118.1 . . ?
C27 C28 H28 119.8 . . ?
C27 C28 C29 120.4(7) . . ?
C29 C28 H28 119.8 . . ?
C28 C29 C21 117.9(7) . . ?
C28 C29 C30 123.6(6) . . ?
C30 C29 C21 118.5(4) . . ?
C29 C30 H30 118.6 . . ?
C31 C30 C29 122.8(5) . . ?
C31 C30 H30 118.6 . . ?
C23 C31 H31 119.1 . . ?
C30 C31 C23 121.7(6) . . ?
C30 C31 H31 119.1 . . ?
C12 C32A C34A 107.3(4) . . ?
C33A C32A C12 112.7(5) . . ?
C33A C32A C34A 106.5(5) . . ?
C35A C32A C12 114.5(5) . . ?
C35A C32A C33A 112.7(5) . . ?
C35A C32A C34A 102.1(5) . . ?
C32A C33A H33A 109.5 . . ?
C32A C33A H33B 109.5 . . ?
C32A C33A H33C 109.5 . . ?
H33A C33A H33B 109.5 . . ?
H33A C33A H33C 109.5 . . ?
H33B C33A H33C 109.5 . . ?
C32A C34A H34A 109.5 . . ?
C32A C34A H34B 109.5 . . ?
C32A C34A H34C 109.5 . . ?
H34A C34A H34B 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
C32A C35A H35A 111.3 . . ?
C32A C35A H35B 111.3 . . ?
H35A C35A H35B 109.2 . . ?
C36A C35A C32A 102.4(6) . . ?
C36A C35A H35A 111.3 . . ?
C36A C35A H35B 111.3 . . ?
C35A C36A H36A 109.5 . . ?
C35A C36A H36B 109.5 . . ?
C35A C36A H36C 109.5 . . ?
H36A C36A H36B 109.5 . . ?
H36A C36A H36C 109.5 . . ?
H36B C36A H36C 109.5 . . ?
H33D C33B H33E 109.5 . . ?
H33D C33B H33F 109.5 . . ?
H33E C33B H33F 109.5 . . ?
H34D C34B H34E 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?
H35C C35B H35D 108.0 . . ?
C36B C35B H35C 109.4 . . ?
C36B C35B H35D 109.4 . . ?
C35B C36B H36D 109.5 . . ?
C35B C36B H36E 109.5 . . ?
C35B C36B H36F 109.5 . . ?
H36D C36B H36E 109.5 . . ?
H36D C36B H36F 109.5 . . ?
H36E C36B H36F 109.5 . . ?
N1S C1S C2S 176.3(7) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
H3SA C3S H3SB 108.1 . . ?
Cl1S C3S H3SA 109.6 . . ?
Cl1S C3S H3SB 109.6 . . ?
Cl2S C3S H3SA 109.6 . . ?
Cl2S C3S H3SB 109.6 . . ?
Cl2S C3S Cl1S 110.4(11) . . ?
H4SA C4S H4SB 108.2 . . ?
Cl3S C4S H4SA 109.8 . . ?
Cl3S C4S H4SB 109.8 . . ?
Cl3S C4S Cl4S 109.4(16) . . ?
Cl4S C4S H4SA 109.8 . . ?
Cl4S C4S H4SB 109.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 177.6(3) . . . . ?
O1 C1 C2 C6 -2.9(4) . . . . ?
O3 C9 C10 C11 -173.6(3) . . . . ?
O3 C14 C15 C16 69.5(5) . . . . ?
O4 C14 C15 C16 -110.9(5) . . . . ?
N1 C1 C2 C3 -2.9(4) . . . . ?
N1 C1 C2 C6 176.6(3) . . . . ?
N1 C8 C9 O3 -2.7(5) . . . . ?
N1 C8 C9 C10 -177.8(3) . . . . ?
N1 C8 C13 C12 177.0(3) . . . . ?
C1 N1 C5 O2 179.3(3) . . . . ?
C1 N1 C5 C4 -1.2(4) . . . . ?
C1 N1 C8 C9 -75.7(4) . . . . ?
C1 N1 C8 C13 107.1(4) . . . . ?
C1 C2 C3 C3 -179.9(3) . . . 3_666 ?
C1 C2 C3 C4 0.1(4) . . . . ?
C1 C2 C6 C7 -179.9(3) . . . 3_666 ?
C2 C3 C4 C5 2.3(4) . . . . ?
C2 C3 C4 C7 -179.1(3) . . . . ?
C3 C2 C6 C7 -0.4(4) . . . 3_666 ?
C3 C3 C4 C5 -177.7(3) 3_666 . . . ?
C3 C3 C4 C7 0.9(5) 3_666 . . . ?
C3 C4 C5 O2 177.6(3) . . . . ?
C3 C4 C5 N1 -1.8(4) . . . . ?
C3 C4 C7 C6 -1.1(5) . . . 3_666 ?
C5 N1 C1 O1 -177.0(3) . . . . ?
C5 N1 C1 C2 3.5(4) . . . . ?
C5 N1 C8 C9 101.4(4) . . . . ?
C5 N1 C8 C13 -75.9(4) . . . . ?
C5 C4 C7 C6 177.5(3) . . . 3_666 ?
C6 C2 C3 C3 0.7(5) . . . 3_666 ?
C6 C2 C3 C4 -179.3(3) . . . . ?
C7 C4 C5 O2 -1.0(5) . . . . ?
C7 C4 C5 N1 179.6(3) . . . . ?
C8 N1 C1 O1 -0.2(4) . . . . ?
C8 N1 C1 C2 -179.7(3) . . . . ?
C8 N1 C5 O2 2.6(4) . . . . ?
C8 N1 C5 C4 -178.0(3) . . . . ?
C8 C9 C10 C11 1.3(5) . . . . ?
C9 O3 C14 O4 0.4(5) . . . . ?
C9 O3 C14 C15 180.0(3) . . . . ?
C9 C8 C13 C12 -0.2(5) . . . . ?
C9 C10 C11 C12 -1.5(6) . . . . ?
C10 C11 C12 C13 0.8(6) . . . . ?
C10 C11 C12 C32A 177.5(4) . . . . ?
C11 C12 C13 C8 0.1(6) . . . . ?
C11 C12 C32A C33A 7.4(7) . . . . ?
C11 C12 C32A C34A 124.3(5) . . . . ?
C11 C12 C32A C35A -123.2(5) . . . . ?
C12 C32A C35A C36A 64.5(7) . . . . ?
C13 C8 C9 O3 174.6(3) . . . . ?
C13 C8 C9 C10 -0.5(5) . . . . ?
C13 C12 C32A C33A -175.9(5) . . . . ?
C13 C12 C32A C34A -59.1(6) . . . . ?
C13 C12 C32A C35A 53.5(6) . . . . ?
C14 O3 C9 C8 114.9(4) . . . . ?
C14 O3 C9 C10 -70.1(4) . . . . ?
C14 C15 C16 C17 -90.7(5) . . . . ?
C14 C15 C16 C25 92.3(4) . . . . ?
C15 C16 C17 C18 3.6(5) . . . . ?
C15 C16 C17 C22 -175.3(3) . . . . ?
C15 C16 C25 C24 176.9(4) . . . . ?
C16 C17 C18 C19 -176.7(4) . . . . ?
C16 C17 C22 C21 176.7(3) . . . . ?
C16 C17 C22 C23 -1.7(5) . . . . ?
C17 C16 C25 C24 -0.1(6) . . . . ?
C17 C18 C19 C20 -1.1(6) . . . . ?
C17 C22 C23 C24 0.5(5) . . . . ?
C17 C22 C23 C31 177.0(3) . . . . ?
C18 C17 C22 C21 -2.3(5) . . . . ?
C18 C17 C22 C23 179.4(3) . . . . ?
C18 C19 C20 C21 0.0(6) . . . . ?
C18 C19 C20 C26 177.8(4) . . . . ?
C19 C20 C21 C22 -0.1(6) . . . . ?
C19 C20 C21 C29 178.1(3) . . . . ?
C19 C20 C26 C27 -178.1(4) . . . . ?
C20 C21 C22 C17 1.3(5) . . . . ?
C20 C21 C22 C23 179.6(3) . . . . ?
C20 C21 C29 C28 0.1(6) . . . . ?
C20 C21 C29 C30 -178.9(4) . . . . ?
C20 C26 C27 C28 0.0(8) . . . . ?
C21 C20 C26 C27 -0.3(6) . . . . ?
C21 C22 C23 C24 -177.9(3) . . . . ?
C21 C22 C23 C31 -1.4(5) . . . . ?
C21 C29 C30 C31 -0.2(7) . . . . ?
C22 C17 C18 C19 2.2(5) . . . . ?
C22 C21 C29 C28 178.4(4) . . . . ?
C22 C21 C29 C30 -0.6(5) . . . . ?
C22 C23 C24 C25 1.0(6) . . . . ?
C22 C23 C31 C30 0.6(6) . . . . ?
C23 C24 C25 C16 -1.2(6) . . . . ?
C24 C23 C31 C30 177.0(4) . . . . ?
C25 C16 C17 C18 -179.6(3) . . . . ?
C25 C16 C17 C22 1.5(5) . . . . ?
C26 C20 C21 C22 -178.0(4) . . . . ?
C26 C20 C21 C29 0.2(6) . . . . ?
C26 C27 C28 C29 0.4(8) . . . . ?
C27 C28 C29 C21 -0.4(7) . . . . ?
C27 C28 C29 C30 178.5(5) . . . . ?
C28 C29 C30 C31 -179.1(4) . . . . ?
C29 C21 C22 C17 -177.0(3) . . . . ?
C29 C21 C22 C23 1.4(5) . . . . ?
C29 C30 C31 C23 0.2(7) . . . . ?
C31 C23 C24 C25 -175.5(4) . . . . ?
C32A C12 C13 C8 -176.8(4) . . . . ?
C33A C32A C35A C36A -66.1(8) . . . . ?
C34A C32A C35A C36A -179.9(7) . . . . ?

