# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1537243'
_audit_update_record             
;
2018-03-29 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H50 N2 O8'
_chemical_formula_weight         734.86

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   11.8540(13)
_cell_length_b                   22.738(2)
_cell_length_c                   14.8160(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.020(3)
_cell_angle_gamma                90.00
_cell_volume                     3932.5(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    13259
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1568
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9832
_exptl_absorpt_correction_T_max  0.9882
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  multilayer
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean 5.814
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            50193
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0120
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         27.52
_reflns_number_total             9008
_reflns_number_gt                8075
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b42'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b42'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0759P)²+3.1432P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9008
_refine_ls_number_parameters     497
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0539
_refine_ls_wR_factor_ref         0.1515
_refine_ls_wR_factor_gt          0.1481
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.175
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.09858(10) 0.90527(5) 0.89307(8) 0.0200(3) Uani 1 1 d . . .
O2 O -0.03084(12) 0.87673(6) 0.77214(9) 0.0271(3) Uani 1 1 d . . .
O3 O -0.21165(10) 1.02891(6) 0.75061(8) 0.0215(3) Uani 1 1 d . . .
O4 O -0.21429(9) 1.01051(6) 0.60055(8) 0.0189(2) Uani 1 1 d . . .
O5 O 0.11421(11) 1.13508(5) 0.50620(8) 0.0201(3) Uani 1 1 d . . .
O6 O 0.23203(12) 1.17351(6) 0.62748(9) 0.0306(3) Uani 1 1 d . . .
O7 O 0.42318(11) 1.02570(7) 0.65466(9) 0.0300(3) Uani 1 1 d . . .
O8 O 0.42510(10) 1.03469(6) 0.80614(8) 0.0209(3) Uani 1 1 d . . .
N1 N 0.11725(11) 1.06943(6) 0.81229(8) 0.0134(3) Uani 1 1 d . . .
N2 N 0.09080(11) 0.98052(6) 0.58962(9) 0.0162(3) Uani 1 1 d D . .
H2 H 0.0499(16) 0.9873(9) 0.5351(9) 0.019 Uiso 1 1 d D . .
C1 C 0.03538(12) 1.02240(7) 0.78817(10) 0.0130(3) Uani 1 1 d . . .
H1 H -0.0146 1.0166 0.8353 0.016 Uiso 1 1 calc R . .
C2 C 0.08687(13) 0.96175(7) 0.75852(10) 0.0137(3) Uani 1 1 d . . .
C3 C 0.02053(13) 0.97054(7) 0.65920(10) 0.0138(3) Uani 1 1 d . . .
H3 H -0.0377 0.9390 0.6410 0.017 Uiso 1 1 calc R . .
C4 C -0.03511(13) 1.02857(7) 0.68989(10) 0.0131(3) Uani 1 1 d . . .
C5 C -0.00675(13) 1.08218(7) 0.63381(10) 0.0136(3) Uani 1 1 d . . .
H5 H -0.0345 1.0719 0.5681 0.016 Uiso 1 1 calc R . .
C6 C 0.12429(13) 1.08537(7) 0.64521(10) 0.0137(3) Uani 1 1 d . . .
C7 C 0.19032(13) 1.07772(7) 0.74422(10) 0.0135(3) Uani 1 1 d . . .
H7 H 0.2481 1.1096 0.7619 0.016 Uiso 1 1 calc R . .
C8 C 0.24673(13) 1.01923(7) 0.71472(10) 0.0140(3) Uani 1 1 d . . .
C9 C 0.17640(13) 1.02557(7) 0.61641(10) 0.0146(3) Uani 1 1 d . . .
H9 H 0.2265 1.0315 0.5694 0.018 Uiso 1 1 calc R . .
C10 C 0.21822(13) 0.96525(7) 0.77051(10) 0.0139(3) Uani 1 1 d . . .
H10 H 0.2464 0.9748 0.8365 0.017 Uiso 1 1 calc R . .
C11 C 0.28041(13) 0.90938(7) 0.75024(11) 0.0165(3) Uani 1 1 d . . .
C12 C 0.38088(17) 0.89418(9) 0.80889(14) 0.0314(4) Uani 1 1 d . . .
H12 H 0.4056 0.9173 0.8620 0.038 Uiso 1 1 calc R . .
C13 C 0.44601(17) 0.84598(9) 0.79182(16) 0.0350(5) Uani 1 1 d . . .
H13 H 0.5142 0.8371 0.8336 0.042 Uiso 1 1 calc R . .
C14 C 0.41427(16) 0.81039(8) 0.71535(14) 0.0267(4) Uani 1 1 d . . .
C15 C 0.3115(2) 0.82396(9) 0.65958(14) 0.0360(5) Uani 1 1 d . . .
H15 H 0.2850 0.7997 0.6080 0.043 Uiso 1 1 calc R . .
C16 C 0.24541(18) 0.87221(9) 0.67679(14) 0.0314(4) Uani 1 1 d . . .
H16 H 0.1748 0.8797 0.6371 0.038 Uiso 1 1 calc R . .
C17 C 0.49001(19) 0.75782(9) 0.69835(17) 0.0382(5) Uani 1 1 d . . .
C18 C 0.4573(4) 0.7311(2) 0.6072(3) 0.0923(11) Uani 1 1 d U . .
H18A H 0.5123 0.7002 0.5992 0.138 Uiso 1 1 calc R . .
H18B H 0.4573 0.7613 0.5600 0.138 Uiso 1 1 calc R . .
H18C H 0.3805 0.7140 0.6017 0.138 Uiso 1 1 calc R . .
C19 C 0.4900(3) 0.71227(14) 0.7736(3) 0.0860(13) Uani 1 1 d . . .
H19A H 0.4147 0.6933 0.7662 0.129 Uiso 1 1 calc R . .
H19B H 0.5064 0.7316 0.8336 0.129 Uiso 1 1 calc R . .
H19C H 0.5488 0.6826 0.7696 0.129 Uiso 1 1 calc R . .
C20 C 0.6177(2) 0.77729(12) 0.7110(3) 0.0661(9) Uani 1 1 d . . .
H20A H 0.6657 0.7432 0.7036 0.099 Uiso 1 1 calc R . .
H20B H 0.6410 0.7939 0.7725 0.099 Uiso 1 1 calc R . .
H20C H 0.6266 0.8071 0.6650 0.099 Uiso 1 1 calc R . .
C21 C 0.04448(13) 0.90940(7) 0.80639(11) 0.0161(3) Uani 1 1 d . . .
C22 C 0.06053(15) 0.85817(8) 0.94812(12) 0.0221(3) Uani 1 1 d . . .
H22A H 0.0707 0.8194 0.9203 0.026 Uiso 1 1 calc R . .
H22B H -0.0215 0.8632 0.9519 0.026 Uiso 1 1 calc R . .
C23 C 0.1328(2) 0.86219(12) 1.04178(15) 0.0454(6) Uani 1 1 d . . .
H23A H 0.2134 0.8562 1.0371 0.068 Uiso 1 1 calc R . .
H23B H 0.1088 0.8319 1.0815 0.068 Uiso 1 1 calc R . .
H23C H 0.1233 0.9011 1.0679 0.068 Uiso 1 1 calc R . .
C24 C -0.16285(13) 1.02306(7) 0.68617(11) 0.0147(3) Uani 1 1 d . . .
C25 C -0.33853(13) 1.00217(8) 0.58623(12) 0.0215(3) Uani 1 1 d . . .
H25A H -0.3722 1.0126 0.5224 0.026 Uiso 1 1 calc R . .
H25B H -0.3722 1.0284 0.6279 0.026 Uiso 1 1 calc R . .
C26 C -0.36637(17) 0.93917(9) 0.60454(17) 0.0364(5) Uani 1 1 d . . .
H26A H -0.3348 0.9134 0.5621 0.055 Uiso 1 1 calc R . .
H26B H -0.4497 0.9342 0.5957 0.055 Uiso 1 1 calc R . .
H26C H -0.3327 0.9289 0.6677 0.055 Uiso 1 1 calc R . .
C27 C -0.06731(13) 1.13910(7) 0.65071(11) 0.0162(3) Uani 1 1 d . . .
C28 C -0.17254(15) 1.15088(8) 0.59571(13) 0.0245(4) Uani 1 1 d . . .
H28 H -0.2040 1.1234 0.5498 0.029 Uiso 1 1 calc R . .
C29 C -0.23242(17) 1.20222(9) 0.60685(15) 0.0324(4) Uani 1 1 d . . .
H29 H -0.3049 1.2091 0.5695 0.039 Uiso 1 1 calc R . .
C30 C -0.18692(18) 1.24324(9) 0.67204(15) 0.0319(4) Uani 1 1 d . . .
H30 H -0.2276 1.2784 0.6796 0.038 Uiso 1 1 calc R . .
C31 C -0.08177(19) 1.23258(8) 0.72604(14) 0.0310(4) Uani 1 1 d . . .
H31 H -0.0494 1.2609 0.7702 0.037 Uiso 1 1 calc R . .
C32 C -0.02261(16) 1.18063(8) 0.71629(12) 0.0232(4) Uani 1 1 d . . .
H32 H 0.0489 1.1735 0.7548 0.028 Uiso 1 1 calc R . .
C33 C 0.16376(13) 1.13699(7) 0.59479(11) 0.0166(3) Uani 1 1 d . . .
C34 C 0.13654(17) 1.18497(8) 0.44993(12) 0.0245(4) Uani 1 1 d . . .
H34A H 0.1223 1.1736 0.3844 0.029 Uiso 1 1 calc R . .
H34B H 0.2176 1.1973 0.4668 0.029 Uiso 1 1 calc R . .
C35 C 0.0590(2) 1.23509(9) 0.46500(15) 0.0356(5) Uani 1 1 d . . .
H35A H -0.0208 1.2219 0.4520 0.053 Uiso 1 1 calc R . .
H35B H 0.0696 1.2677 0.4240 0.053 Uiso 1 1 calc R . .
H35C H 0.0779 1.2483 0.5288 0.053 Uiso 1 1 calc R . .
C36 C 0.16493(13) 1.07990(7) 0.90528(10) 0.0148(3) Uani 1 1 d . . .
C37 C 0.22692(15) 1.13167(8) 0.92910(11) 0.0213(3) Uani 1 1 d . . .
H37 H 0.2385 1.1586 0.8826 0.026 Uiso 1 1 calc R . .
C38 C 0.27158(17) 1.14398(9) 1.01989(13) 0.0276(4) Uani 1 1 d . . .
H38 H 0.3139 1.1792 1.0349 0.033 Uiso 1 1 calc R . .
C39 C 0.25522(16) 1.10549(9) 1.08919(12) 0.0277(4) Uani 1 1 d . . .
H39 H 0.2856 1.1142 1.1514 0.033 Uiso 1 1 calc R . .
C40 C 0.19400(15) 1.05425(8) 1.06636(11) 0.0231(4) Uani 1 1 d . . .
H40 H 0.1825 1.0276 1.1133 0.028 Uiso 1 1 calc R . .
C41 C 0.14908(14) 1.04120(7) 0.97542(11) 0.0180(3) Uani 1 1 d . . .
H41 H 0.1074 1.0058 0.9609 0.022 Uiso 1 1 calc R . .
C42 C 0.37424(13) 1.02632(7) 0.71931(11) 0.0170(3) Uani 1 1 d . . .
C43 C 0.54917(14) 1.04131(9) 0.82204(13) 0.0243(4) Uani 1 1 d . . .
H43A H 0.5713 1.0758 0.7883 0.029 Uiso 1 1 calc R . .
H43B H 0.5857 1.0058 0.8013 0.029 Uiso 1 1 calc R . .
C44 C 0.58552(17) 1.04972(10) 0.92341(14) 0.0340(4) Uani 1 1 d . . .
H44A H 0.5435 1.0829 0.9438 0.051 Uiso 1 1 calc R . .
H44B H 0.6679 1.0578 0.9371 0.051 Uiso 1 1 calc R . .
H44C H 0.5689 1.0139 0.9555 0.051 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 C21 1.3351(19) . ?
O1 C22 1.4640(19) . ?
O2 C21 1.204(2) . ?
O3 C24 1.2067(19) . ?
O4 C24 1.3391(19) . ?
O4 C25 1.4632(18) . ?
O5 C33 1.3422(19) . ?
O5 C34 1.4591(19) . ?
O6 C33 1.201(2) . ?
O7 C42 1.203(2) . ?
O8 C42 1.336(2) . ?
O8 C43 1.4563(19) . ?
N1 C36 1.4154(19) . ?
N1 C1 1.4465(19) . ?
N1 C7 1.4515(19) . ?
N2 C9 1.448(2) . ?
N2 C3 1.4514(19) . ?
N2 H2 0.880(10) . ?
C1 C4 1.554(2) . ?
C1 C2 1.600(2) . ?
C1 H1 1.0000 . ?
C2 C21 1.516(2) . ?
C2 C10 1.538(2) . ?
C2 C3 1.556(2) . ?
C3 C4 1.577(2) . ?
C3 H3 1.0000 . ?
C4 C24 1.511(2) . ?
C4 C5 1.545(2) . ?
C5 C27 1.522(2) . ?
C5 C6 1.535(2) . ?
C5 H5 1.0000 . ?
C6 C33 1.509(2) . ?
C6 C7 1.548(2) . ?
C6 C9 1.582(2) . ?
C7 C8 1.584(2) . ?
C7 H7 1.0000 . ?
C8 C42 1.510(2) . ?
C8 C10 1.550(2) . ?
C8 C9 1.554(2) . ?
C9 H9 1.0000 . ?
C10 C11 1.525(2) . ?
C10 H10 1.0000 . ?
C11 C16 1.383(2) . ?
C11 C12 1.390(2) . ?
C12 C13 1.389(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.390(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.383(3) . ?
C14 C17 1.542(3) . ?
C15 C16 1.397(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.469(5) . ?
C17 C19 1.522(4) . ?
C17 C20 1.556(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C22 C23 1.501(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C25 C26 1.505(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C32 1.392(2) . ?
C27 C28 1.392(2) . ?
C28 C29 1.391(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.383(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.380(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.394(3) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C34 C35 1.505(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C41 1.399(2) . ?
C36 C37 1.400(2) . ?
C37 C38 1.386(2) . ?
C37 H37 0.9500 . ?
C38 C39 1.388(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.383(3) . ?
C39 H39 0.9500 . ?
C40 C41 1.392(2) . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
C43 C44 1.501(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 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
C21 O1 C22 116.38(13) . . ?
C24 O4 C25 116.48(12) . . ?
C33 O5 C34 116.21(13) . . ?
C42 O8 C43 116.38(13) . . ?
C36 N1 C1 120.13(12) . . ?
C36 N1 C7 117.96(12) . . ?
C1 N1 C7 112.35(12) . . ?
C9 N2 C3 112.17(12) . . ?
C9 N2 H2 112.1(14) . . ?
C3 N2 H2 112.7(14) . . ?
N1 C1 C4 113.13(12) . . ?
N1 C1 C2 115.68(12) . . ?
C4 C1 C2 89.38(11) . . ?
N1 C1 H1 112.3 . . ?
C4 C1 H1 112.3 . . ?
C2 C1 H1 112.3 . . ?
C21 C2 C10 113.45(12) . . ?
C21 C2 C3 112.92(12) . . ?
C10 C2 C3 115.94(12) . . ?
C21 C2 C1 112.03(12) . . ?
C10 C2 C1 110.52(12) . . ?
C3 C2 C1 89.71(11) . . ?
N2 C3 C2 115.70(12) . . ?
N2 C3 C4 113.24(12) . . ?
C2 C3 C4 90.15(11) . . ?
N2 C3 H3 112.0 . . ?
C2 C3 H3 112.0 . . ?
C4 C3 H3 112.0 . . ?
C24 C4 C5 110.88(12) . . ?
C24 C4 C1 113.50(12) . . ?
C5 C4 C1 116.33(12) . . ?
C24 C4 C3 112.75(12) . . ?
C5 C4 C3 111.35(12) . . ?
C1 C4 C3 90.63(11) . . ?
C27 C5 C6 116.05(13) . . ?
C27 C5 C4 115.43(12) . . ?
C6 C5 C4 106.79(12) . . ?
C27 C5 H5 105.9 . . ?
C6 C5 H5 105.9 . . ?
C4 C5 H5 105.9 . . ?
C33 C6 C5 112.17(13) . . ?
C33 C6 C7 114.05(13) . . ?
C5 C6 C7 115.75(12) . . ?
C33 C6 C9 111.45(12) . . ?
C5 C6 C9 111.40(12) . . ?
C7 C6 C9 90.13(11) . . ?
N1 C7 C6 114.11(12) . . ?
N1 C7 C8 114.48(12) . . ?
C6 C7 C8 90.06(11) . . ?
N1 C7 H7 112.2 . . ?
C6 C7 H7 112.2 . . ?
C8 C7 H7 112.2 . . ?
C42 C8 C10 111.72(12) . . ?
C42 C8 C9 113.70(12) . . ?
C10 C8 C9 116.25(12) . . ?
C42 C8 C7 111.43(12) . . ?
C10 C8 C7 112.09(12) . . ?
C9 C8 C7 89.85(11) . . ?
N2 C9 C8 115.30(13) . . ?
N2 C9 C6 113.21(12) . . ?
C8 C9 C6 89.88(11) . . ?
N2 C9 H9 112.2 . . ?
C8 C9 H9 112.2 . . ?
C6 C9 H9 112.2 . . ?
C11 C10 C2 116.66(13) . . ?
C11 C10 C8 113.39(12) . . ?
C2 C10 C8 106.84(12) . . ?
C11 C10 H10 106.4 . . ?
C2 C10 H10 106.4 . . ?
C8 C10 H10 106.4 . . ?
C16 C11 C12 116.54(16) . . ?
C16 C11 C10 125.10(15) . . ?
C12 C11 C10 118.36(15) . . ?
C13 C12 C11 121.68(18) . . ?
C13 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
C12 C13 C14 121.85(18) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C15 C14 C13 116.27(17) . . ?
C15 C14 C17 123.57(18) . . ?
C13 C14 C17 120.12(18) . . ?
C14 C15 C16 122.00(18) . . ?
C14 C15 H15 119.0 . . ?
C16 C15 H15 119.0 . . ?
C11 C16 C15 121.50(17) . . ?
C11 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C18 C17 C19 111.0(3) . . ?
C18 C17 C14 113.7(2) . . ?
C19 C17 C14 109.5(2) . . ?
C18 C17 C20 108.9(3) . . ?
C19 C17 C20 103.3(2) . . ?
C14 C17 C20 109.96(18) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O2 C21 O1 123.99(15) . . ?
O2 C21 C2 124.71(15) . . ?
O1 C21 C2 111.26(13) . . ?
O1 C22 C23 106.79(14) . . ?
O1 C22 H22A 110.4 . . ?
C23 C22 H22A 110.4 . . ?
O1 C22 H22B 110.4 . . ?
C23 C22 H22B 110.4 . . ?
H22A C22 H22B 108.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O3 C24 O4 124.82(14) . . ?
O3 C24 C4 125.27(14) . . ?
O4 C24 C4 109.91(12) . . ?
O4 C25 C26 110.12(15) . . ?
O4 C25 H25A 109.6 . . ?
C26 C25 H25A 109.6 . . ?
O4 C25 H25B 109.6 . . ?
C26 C25 H25B 109.6 . . ?
H25A C25 H25B 108.2 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C32 C27 C28 118.15(15) . . ?
C32 C27 C5 123.96(14) . . ?
C28 C27 C5 117.87(15) . . ?
C29 C28 C27 121.04(18) . . ?
C29 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
C30 C29 C28 120.26(18) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C31 C30 C29 119.31(17) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
C30 C31 C32 120.56(18) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C27 C32 C31 120.66(17) . . ?
C27 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
O6 C33 O5 124.49(15) . . ?
O6 C33 C6 125.69(15) . . ?
O5 C33 C6 109.78(13) . . ?
O5 C34 C35 109.14(15) . . ?
O5 C34 H34A 109.9 . . ?
C35 C34 H34A 109.9 . . ?
O5 C34 H34B 109.9 . . ?
C35 C34 H34B 109.9 . . ?
H34A C34 H34B 108.3 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C41 C36 C37 118.29(14) . . ?
C41 C36 N1 122.33(14) . . ?
C37 C36 N1 119.34(14) . . ?
C38 C37 C36 120.64(16) . . ?
C38 C37 H37 119.7 . . ?
C36 C37 H37 119.7 . . ?
C37 C38 C39 120.78(17) . . ?
C37 C38 H38 119.6 . . ?
C39 C38 H38 119.6 . . ?
C40 C39 C38 119.02(16) . . ?
C40 C39 H39 120.5 . . ?
C38 C39 H39 120.5 . . ?
C39 C40 C41 120.82(16) . . ?
C39 C40 H40 119.6 . . ?
C41 C40 H40 119.6 . . ?
C40 C41 C36 120.45(16) . . ?
C40 C41 H41 119.8 . . ?
C36 C41 H41 119.8 . . ?
O7 C42 O8 124.68(15) . . ?
O7 C42 C8 125.49(15) . . ?
O8 C42 C8 109.82(13) . . ?
O8 C43 C44 106.32(14) . . ?
O8 C43 H43A 110.5 . . ?
C44 C43 H43A 110.5 . . ?
O8 C43 H43B 110.5 . . ?
C44 C43 H43B 110.5 . . ?
H43A C43 H43B 108.7 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

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
C36 N1 C1 C4 162.43(13) . . . . ?
C7 N1 C1 C4 -52.01(16) . . . . ?
C36 N1 C1 C2 -96.48(16) . . . . ?
C7 N1 C1 C2 49.08(17) . . . . ?
N1 C1 C2 C21 132.59(13) . . . . ?
C4 C1 C2 C21 -111.90(13) . . . . ?
N1 C1 C2 C10 5.02(17) . . . . ?
C4 C1 C2 C10 120.54(12) . . . . ?
N1 C1 C2 C3 -112.70(13) . . . . ?
C4 C1 C2 C3 2.81(11) . . . . ?
C9 N2 C3 C2 -49.07(17) . . . . ?
C9 N2 C3 C4 53.04(17) . . . . ?
C21 C2 C3 N2 -132.83(14) . . . . ?
C10 C2 C3 N2 0.49(19) . . . . ?
C1 C2 C3 N2 113.28(13) . . . . ?
C21 C2 C3 C4 111.12(13) . . . . ?
C10 C2 C3 C4 -115.56(13) . . . . ?
C1 C2 C3 C4 -2.77(11) . . . . ?
N1 C1 C4 C24 -129.71(13) . . . . ?
C2 C1 C4 C24 112.48(13) . . . . ?
N1 C1 C4 C5 0.74(18) . . . . ?
C2 C1 C4 C5 -117.08(13) . . . . ?
N1 C1 C4 C3 115.04(13) . . . . ?
C2 C1 C4 C3 -2.77(11) . . . . ?
N2 C3 C4 C24 128.71(13) . . . . ?
C2 C3 C4 C24 -113.06(13) . . . . ?
N2 C3 C4 C5 3.34(17) . . . . ?
C2 C3 C4 C5 121.57(12) . . . . ?
N2 C3 C4 C1 -115.38(13) . . . . ?
C2 C3 C4 C1 2.85(11) . . . . ?
C24 C4 C5 C27 47.04(17) . . . . ?
C1 C4 C5 C27 -84.63(16) . . . . ?
C3 C4 C5 C27 173.45(12) . . . . ?
C24 C4 C5 C6 177.69(12) . . . . ?
C1 C4 C5 C6 46.01(16) . . . . ?
C3 C4 C5 C6 -55.90(15) . . . . ?
C27 C5 C6 C33 -48.62(17) . . . . ?
C4 C5 C6 C33 -178.92(12) . . . . ?
C27 C5 C6 C7 84.62(16) . . . . ?
C4 C5 C6 C7 -45.68(16) . . . . ?
C27 C5 C6 C9 -174.33(12) . . . . ?
C4 C5 C6 C9 55.37(15) . . . . ?
C36 N1 C7 C6 -161.07(13) . . . . ?
C1 N1 C7 C6 52.56(17) . . . . ?
C36 N1 C7 C8 97.10(16) . . . . ?
C1 N1 C7 C8 -49.27(16) . . . . ?
C33 C6 C7 N1 131.52(14) . . . . ?
C5 C6 C7 N1 -0.86(18) . . . . ?
C9 C6 C7 N1 -114.82(13) . . . . ?
C33 C6 C7 C8 -111.45(13) . . . . ?
C5 C6 C7 C8 116.17(13) . . . . ?
C9 C6 C7 C8 2.22(11) . . . . ?
N1 C7 C8 C42 -130.04(13) . . . . ?
C6 C7 C8 C42 113.26(13) . . . . ?
N1 C7 C8 C10 -3.99(17) . . . . ?
C6 C7 C8 C10 -120.70(12) . . . . ?
N1 C7 C8 C9 114.45(13) . . . . ?
C6 C7 C8 C9 -2.26(11) . . . . ?
C3 N2 C9 C8 47.95(17) . . . . ?
C3 N2 C9 C6 -53.59(17) . . . . ?
C42 C8 C9 N2 132.99(14) . . . . ?
C10 C8 C9 N2 1.14(18) . . . . ?
C7 C8 C9 N2 -113.57(13) . . . . ?
C42 C8 C9 C6 -111.23(13) . . . . ?
C10 C8 C9 C6 116.92(13) . . . . ?
C7 C8 C9 C6 2.21(11) . . . . ?
C33 C6 C9 N2 -128.59(14) . . . . ?
C5 C6 C9 N2 -2.47(17) . . . . ?
C7 C6 C9 N2 115.39(13) . . . . ?
C33 C6 C9 C8 113.76(13) . . . . ?
C5 C6 C9 C8 -120.12(12) . . . . ?
C7 C6 C9 C8 -2.26(11) . . . . ?
C21 C2 C10 C11 49.76(18) . . . . ?
C3 C2 C10 C11 -83.32(16) . . . . ?
C1 C2 C10 C11 176.54(12) . . . . ?
C21 C2 C10 C8 177.78(12) . . . . ?
C3 C2 C10 C8 44.70(16) . . . . ?
C1 C2 C10 C8 -55.43(15) . . . . ?
C42 C8 C10 C11 -48.61(17) . . . . ?
C9 C8 C10 C11 84.15(16) . . . . ?
C7 C8 C10 C11 -174.50(12) . . . . ?
C42 C8 C10 C2 -178.52(12) . . . . ?
C9 C8 C10 C2 -45.76(16) . . . . ?
C7 C8 C10 C2 55.59(15) . . . . ?
C2 C10 C11 C16 42.5(2) . . . . ?
C8 C10 C11 C16 -82.3(2) . . . . ?
C2 C10 C11 C12 -138.18(17) . . . . ?
C8 C10 C11 C12 97.05(19) . . . . ?
C16 C11 C12 C13 3.4(3) . . . . ?
C10 C11 C12 C13 -175.99(19) . . . . ?
C11 C12 C13 C14 0.0(4) . . . . ?
C12 C13 C14 C15 -3.0(3) . . . . ?
C12 C13 C14 C17 179.2(2) . . . . ?
C13 C14 C15 C16 2.6(3) . . . . ?
C17 C14 C15 C16 -179.6(2) . . . . ?
C12 C11 C16 C15 -3.8(3) . . . . ?
C10 C11 C16 C15 175.60(19) . . . . ?
C14 C15 C16 C11 0.8(4) . . . . ?
C15 C14 C17 C18 12.9(4) . . . . ?
C13 C14 C17 C18 -169.4(3) . . . . ?
C15 C14 C17 C19 -111.9(3) . . . . ?
C13 C14 C17 C19 65.8(3) . . . . ?
C15 C14 C17 C20 135.3(3) . . . . ?
C13 C14 C17 C20 -47.0(3) . . . . ?
C22 O1 C21 O2 -1.0(2) . . . . ?
C22 O1 C21 C2 176.74(13) . . . . ?
C10 C2 C21 O2 -133.15(17) . . . . ?
C3 C2 C21 O2 1.4(2) . . . . ?
C1 C2 C21 O2 100.86(19) . . . . ?
C10 C2 C21 O1 49.18(17) . . . . ?
C3 C2 C21 O1 -176.31(12) . . . . ?
C1 C2 C21 O1 -76.81(16) . . . . ?
C21 O1 C22 C23 -179.99(17) . . . . ?
C25 O4 C24 O3 -1.5(2) . . . . ?
C25 O4 C24 C4 178.38(13) . . . . ?
C5 C4 C24 O3 -114.14(17) . . . . ?
C1 C4 C24 O3 19.0(2) . . . . ?
C3 C4 C24 O3 120.24(17) . . . . ?
C5 C4 C24 O4 66.02(16) . . . . ?
C1 C4 C24 O4 -160.86(13) . . . . ?
C3 C4 C24 O4 -59.60(16) . . . . ?
C24 O4 C25 C26 -87.05(18) . . . . ?
C6 C5 C27 C32 -35.1(2) . . . . ?
C4 C5 C27 C32 90.91(19) . . . . ?
C6 C5 C27 C28 143.30(15) . . . . ?
C4 C5 C27 C28 -90.66(18) . . . . ?
C32 C27 C28 C29 -1.0(3) . . . . ?
C5 C27 C28 C29 -179.58(17) . . . . ?
C27 C28 C29 C30 1.3(3) . . . . ?
C28 C29 C30 C31 -0.2(3) . . . . ?
C29 C30 C31 C32 -1.1(3) . . . . ?
C28 C27 C32 C31 -0.3(3) . . . . ?
C5 C27 C32 C31 178.18(16) . . . . ?
C30 C31 C32 C27 1.3(3) . . . . ?
C34 O5 C33 O6 -7.2(2) . . . . ?
C34 O5 C33 C6 175.01(13) . . . . ?
C5 C6 C33 O6 127.22(18) . . . . ?
C7 C6 C33 O6 -6.8(2) . . . . ?
C9 C6 C33 O6 -107.10(19) . . . . ?
C5 C6 C33 O5 -55.04(17) . . . . ?
C7 C6 C33 O5 170.89(12) . . . . ?
C9 C6 C33 O5 70.64(16) . . . . ?
C33 O5 C34 C35 -80.51(19) . . . . ?
C1 N1 C36 C41 9.5(2) . . . . ?
C7 N1 C36 C41 -134.21(15) . . . . ?
C1 N1 C36 C37 -168.23(14) . . . . ?
C7 N1 C36 C37 48.1(2) . . . . ?
C41 C36 C37 C38 0.2(3) . . . . ?
N1 C36 C37 C38 177.99(16) . . . . ?
C36 C37 C38 C39 -0.4(3) . . . . ?
C37 C38 C39 C40 0.4(3) . . . . ?
C38 C39 C40 C41 -0.1(3) . . . . ?
C39 C40 C41 C36 -0.2(3) . . . . ?
C37 C36 C41 C40 0.1(2) . . . . ?
N1 C36 C41 C40 -177.64(15) . . . . ?
C43 O8 C42 O7 -2.3(2) . . . . ?
C43 O8 C42 C8 178.99(14) . . . . ?
C10 C8 C42 O7 120.21(18) . . . . ?
C9 C8 C42 O7 -13.8(2) . . . . ?
C7 C8 C42 O7 -113.54(19) . . . . ?
C10 C8 C42 O8 -61.08(17) . . . . ?
C9 C8 C42 O8 164.90(13) . . . . ?
C7 C8 C42 O8 65.17(16) . . . . ?
C42 O8 C43 C44 -179.70(15) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 N2 0.880(10) 2.379(12) 3.238(3) 165.1(19) 3_576

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.352
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.058
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1537245'
_audit_update_record             
;
2018-03-29 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H44 N2 O11'
_chemical_formula_weight         692.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   7.0677(17)
_cell_length_b                   38.091(8)
_cell_length_c                   12.609(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.486(5)
_cell_angle_gamma                90.00
_cell_volume                     3379.0(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    4494
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.4

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1472
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9802
_exptl_absorpt_correction_T_max  0.9880
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  multilayer
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean 5.814
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            41837
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         27.50
_reflns_number_total             7675
_reflns_number_gt                5169
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b42'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b42'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0424P)²+3.7309P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7675
_refine_ls_number_parameters     464
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0572
_refine_ls_wR_factor_ref         0.1372
_refine_ls_wR_factor_gt          0.1149
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.5929(2) 0.17738(5) 0.21594(13) 0.0325(4) Uani 1 1 d . . .
O2 O 0.3425(2) 0.17001(4) 0.09535(12) 0.0246(4) Uani 1 1 d . . .
O3 O -0.1307(3) 0.12517(4) 0.06315(13) 0.0320(4) Uani 1 1 d . . .
O4 O 0.1070(2) 0.08601(4) 0.07774(12) 0.0225(4) Uani 1 1 d . . .
O5 O -0.2946(2) 0.09543(4) 0.48013(13) 0.0238(4) Uani 1 1 d . . .
O6 O -0.0464(2) 0.10877(4) 0.59837(12) 0.0231(4) Uani 1 1 d . . .
O7 O 0.4127(3) 0.15082(4) 0.63469(13) 0.0311(4) Uani 1 1 d . . .
O8 O 0.1941(3) 0.19345(4) 0.60667(12) 0.0270(4) Uani 1 1 d . . .
O9 O 0.1083(2) -0.02097(4) 0.36403(14) 0.0289(4) Uani 1 1 d . . .
O10 O -0.1919(2) -0.04204(4) 0.23728(13) 0.0245(4) Uani 1 1 d . . .
O11 O -0.4478(2) 0.00457(4) 0.14862(14) 0.0309(4) Uani 1 1 d . . .
N1 N -0.0216(3) 0.17730(4) 0.32793(14) 0.0159(4) Uani 1 1 d D . .
H1 H -0.1475(15) 0.1783(6) 0.3087(18) 0.019 Uiso 1 1 d D . .
N2 N 0.3168(3) 0.09889(5) 0.36566(14) 0.0172(4) Uani 1 1 d D . .
H2 H 0.4422(15) 0.0977(6) 0.3835(19) 0.021 Uiso 1 1 d D . .
C1 C 0.2786(3) 0.11764(5) 0.26651(17) 0.0170(4) Uani 1 1 d . . .
H1A H 0.3520 0.1079 0.2093 0.020 Uiso 1 1 calc R . .
C2 C 0.2964(3) 0.15962(5) 0.27499(17) 0.0164(4) Uani 1 1 d . . .
C3 C 0.0774(3) 0.16252(5) 0.24329(17) 0.0165(4) Uani 1 1 d . . .
H3 H 0.0476 0.1752 0.1743 0.020 Uiso 1 1 calc R . .
C4 C 0.0634(3) 0.12131(5) 0.22914(17) 0.0163(4) Uani 1 1 d . . .
C5 C -0.0728(3) 0.10464(5) 0.30516(16) 0.0163(4) Uani 1 1 d . . .
H5 H -0.1997 0.1159 0.2876 0.020 Uiso 1 1 calc R . .
C6 C -0.0032(3) 0.11637(5) 0.41837(16) 0.0156(4) Uani 1 1 d . . .
C7 C 0.2157(3) 0.11366(5) 0.45003(17) 0.0166(4) Uani 1 1 d . . .
H7 H 0.2453 0.1010 0.5190 0.020 Uiso 1 1 calc R . .
C8 C 0.2293(3) 0.15455(5) 0.46453(17) 0.0176(5) Uani 1 1 d . . .
C9 C 0.0144(3) 0.15837(5) 0.42677(17) 0.0161(4) Uani 1 1 d . . .
H9 H -0.0594 0.1681 0.4839 0.019 Uiso 1 1 calc R . .
C10 C 0.3662(3) 0.17092(5) 0.38889(16) 0.0169(4) Uani 1 1 d . . .
H10 H 0.4916 0.1591 0.4062 0.020 Uiso 1 1 calc R . .
C11 C 0.4023(3) 0.21000(6) 0.40674(17) 0.0183(5) Uani 1 1 d . . .
C12 C 0.5572(3) 0.22004(6) 0.47700(18) 0.0233(5) Uani 1 1 d . . .
H12 H 0.6397 0.2026 0.5091 0.028 Uiso 1 1 calc R . .
C13 C 0.5930(4) 0.25519(6) 0.5009(2) 0.0290(6) Uani 1 1 d . . .
H13 H 0.6984 0.2615 0.5496 0.035 Uiso 1 1 calc R . .
C14 C 0.4750(4) 0.28096(6) 0.4537(2) 0.0298(6) Uani 1 1 d . . .
H14 H 0.4984 0.3050 0.4701 0.036 Uiso 1 1 calc R . .
C15 C 0.3231(4) 0.27136(6) 0.3827(2) 0.0279(6) Uani 1 1 d . . .
H15 H 0.2430 0.2890 0.3494 0.033 Uiso 1 1 calc R . .
C16 C 0.2857(3) 0.23615(6) 0.35915(19) 0.0229(5) Uani 1 1 d . . .
H16 H 0.1801 0.2300 0.3104 0.027 Uiso 1 1 calc R . .
C17 C 0.4270(3) 0.17112(5) 0.19507(17) 0.0187(5) Uani 1 1 d . . .
C18 C 0.4625(4) 0.17360(7) 0.00736(18) 0.0269(5) Uani 1 1 d . . .
H18A H 0.5984 0.1731 0.0349 0.032 Uiso 1 1 calc R . .
H18B H 0.4360 0.1962 -0.0300 0.032 Uiso 1 1 calc R . .
C19 C 0.4183(4) 0.14369(8) -0.0672(2) 0.0394(7) Uani 1 1 d . . .
H19A H 0.4653 0.1218 -0.0333 0.059 Uiso 1 1 calc R . .
H19B H 0.4802 0.1475 -0.1326 0.059 Uiso 1 1 calc R . .
H19C H 0.2805 0.1421 -0.0847 0.059 Uiso 1 1 calc R . .
C20 C 0.0010(3) 0.11142(5) 0.11474(17) 0.0192(5) Uani 1 1 d . . .
C21 C 0.0550(4) 0.07476(6) -0.03188(18) 0.0261(5) Uani 1 1 d . . .
H21A H 0.1661 0.0635 -0.0600 0.031 Uiso 1 1 calc R . .
H21B H 0.0201 0.0956 -0.0765 0.031 Uiso 1 1 calc R . .
C22 C -0.1080(4) 0.04951(7) -0.0394(2) 0.0367(7) Uani 1 1 d . . .
H22A H -0.0827 0.0308 0.0135 0.055 Uiso 1 1 calc R . .
H22B H -0.1235 0.0392 -0.1110 0.055 Uiso 1 1 calc R . .
H22C H -0.2246 0.0620 -0.0258 0.055 Uiso 1 1 calc R . .
C23 C -0.1314(3) 0.10460(5) 0.49977(17) 0.0176(5) Uani 1 1 d . . .
C24 C -0.1607(4) 0.10520(6) 0.68851(18) 0.0248(5) Uani 1 1 d . . .
H24A H -0.1184 0.0845 0.7321 0.030 Uiso 1 1 calc R . .
H24B H -0.2964 0.1021 0.6628 0.030 Uiso 1 1 calc R . .
C25 C -0.1345(4) 0.13804(7) 0.7534(2) 0.0335(6) Uani 1 1 d . . .
H25A H 0.0015 0.1422 0.7721 0.050 Uiso 1 1 calc R . .
H25B H -0.1983 0.1355 0.8186 0.050 Uiso 1 1 calc R . .
H25C H -0.1895 0.1579 0.7120 0.050 Uiso 1 1 calc R . .
C26 C 0.2893(3) 0.16529(6) 0.57823(18) 0.0207(5) Uani 1 1 d . . .
C27 C 0.2622(5) 0.20928(7) 0.7086(2) 0.0436(8) Uani 1 1 d . . .
H27A H 0.2052 0.1972 0.7673 0.052 Uiso 1 1 calc R . .
H27B H 0.4021 0.2071 0.7208 0.052 Uiso 1 1 calc R . .
C28 C 0.2082(6) 0.24606(8) 0.7058(3) 0.0549(9) Uani 1 1 d . . .
H28A H 0.2620 0.2577 0.6462 0.082 Uiso 1 1 calc R . .
H28B H 0.2568 0.2573 0.7728 0.082 Uiso 1 1 calc R . .
H28C H 0.0693 0.2480 0.6967 0.082 Uiso 1 1 calc R . .
C29 C -0.1036(3) 0.06521(5) 0.29107(17) 0.0180(5) Uani 1 1 d . . .
C30 C 0.0245(3) 0.04053(5) 0.33724(18) 0.0201(5) Uani 1 1 d . . .
H30 H 0.1350 0.0481 0.3800 0.024 Uiso 1 1 calc R . .
C31 C -0.0090(3) 0.00484(6) 0.32093(18) 0.0203(5) Uani 1 1 d . . .
C32 C -0.1688(3) -0.00669(5) 0.25775(18) 0.0200(5) Uani 1 1 d . . .
C33 C -0.2969(3) 0.01805(6) 0.21167(18) 0.0217(5) Uani 1 1 d . . .
C34 C -0.2653(3) 0.05383(6) 0.22955(17) 0.0205(5) Uani 1 1 d . . .
H34 H -0.3551 0.0705 0.1995 0.025 Uiso 1 1 calc R . .
C35 C 0.2716(4) -0.01014(6) 0.4317(2) 0.0306(6) Uani 1 1 d . . .
H35A H 0.3539 0.0042 0.3909 0.046 Uiso 1 1 calc R . .
H35B H 0.3418 -0.0309 0.4596 0.046 Uiso 1 1 calc R . .
H35C H 0.2312 0.0037 0.4912 0.046 Uiso 1 1 calc R . .
C36 C -0.3431(4) -0.05816(6) 0.2873(2) 0.0329(6) Uani 1 1 d . . .
H36A H -0.3292 -0.0527 0.3636 0.049 Uiso 1 1 calc R . .
H36B H -0.3383 -0.0837 0.2775 0.049 Uiso 1 1 calc R . .
H36C H -0.4652 -0.0492 0.2552 0.049 Uiso 1 1 calc R . .
C37 C -0.5928(4) 0.02869(7) 0.1109(3) 0.0414(7) Uani 1 1 d . . .
H37A H -0.6430 0.0403 0.1716 0.062 Uiso 1 1 calc R . .
H37B H -0.6956 0.0160 0.0695 0.062 Uiso 1 1 calc R . .
H37C H -0.5396 0.0463 0.0655 0.062 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 C17 1.201(3) . ?
O2 C17 1.340(3) . ?
O2 C18 1.466(3) . ?
O3 C20 1.203(3) . ?
O4 C20 1.335(3) . ?
O4 C21 1.460(3) . ?
O5 C23 1.208(3) . ?
O6 C23 1.337(3) . ?
O6 C24 1.462(3) . ?
O7 C26 1.205(3) . ?
O8 C26 1.334(3) . ?
O8 C27 1.459(3) . ?
O9 C31 1.365(3) . ?
O9 C35 1.430(3) . ?
O10 C32 1.378(2) . ?
O10 C36 1.430(3) . ?
O11 C33 1.368(3) . ?
O11 C37 1.424(3) . ?
N1 C9 1.441(3) . ?
N1 C3 1.445(3) . ?
N2 C1 1.443(3) . ?
N2 C7 1.450(3) . ?
C1 C4 1.555(3) . ?
C1 C2 1.607(3) . ?
C2 C17 1.496(3) . ?
C2 C10 1.535(3) . ?
C2 C3 1.565(3) . ?
C3 C4 1.582(3) . ?
C4 C20 1.515(3) . ?
C4 C5 1.557(3) . ?
C5 C29 1.525(3) . ?
C5 C6 1.531(3) . ?
C6 C23 1.501(3) . ?
C6 C7 1.564(3) . ?
C6 C9 1.607(3) . ?
C7 C8 1.570(3) . ?
C8 C26 1.512(3) . ?
C8 C10 1.553(3) . ?
C8 C9 1.555(3) . ?
C10 C11 1.523(3) . ?
C11 C16 1.392(3) . ?
C11 C12 1.394(3) . ?
C12 C13 1.391(3) . ?
C13 C14 1.385(4) . ?
C14 C15 1.380(4) . ?
C15 C16 1.393(3) . ?
C18 C19 1.491(4) . ?
C21 C22 1.497(4) . ?
C24 C25 1.496(3) . ?
C27 C28 1.452(4) . ?
C29 C34 1.388(3) . ?
C29 C30 1.393(3) . ?
C30 C31 1.392(3) . ?
C31 C32 1.389(3) . ?
C32 C33 1.394(3) . ?
C33 C34 1.396(3) . ?

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
C17 O2 C18 117.97(18) . . ?
C20 O4 C21 116.39(17) . . ?
C23 O6 C24 118.64(18) . . ?
C26 O8 C27 115.9(2) . . ?
C31 O9 C35 117.05(17) . . ?
C32 O10 C36 114.65(18) . . ?
C33 O11 C37 116.64(18) . . ?
C9 N1 C3 112.71(17) . . ?
C1 N2 C7 112.28(17) . . ?
N2 C1 C4 113.80(18) . . ?
N2 C1 C2 115.34(17) . . ?
C4 C1 C2 89.93(15) . . ?
C17 C2 C10 112.62(18) . . ?
C17 C2 C3 117.79(18) . . ?
C10 C2 C3 116.14(18) . . ?
C17 C2 C1 107.23(17) . . ?
C10 C2 C1 110.95(16) . . ?
C3 C2 C1 89.08(15) . . ?
N1 C3 C2 112.07(17) . . ?
N1 C3 C4 116.13(17) . . ?
C2 C3 C4 90.49(15) . . ?
C20 C4 C1 116.95(18) . . ?
C20 C4 C5 110.11(17) . . ?
C1 C4 C5 114.90(17) . . ?
C20 C4 C3 111.33(17) . . ?
C1 C4 C3 90.36(15) . . ?
C5 C4 C3 111.78(17) . . ?
C29 C5 C6 115.17(17) . . ?
C29 C5 C4 114.80(17) . . ?
C6 C5 C4 106.99(17) . . ?
C23 C6 C5 112.88(18) . . ?
C23 C6 C7 116.93(17) . . ?
C5 C6 C7 116.15(18) . . ?
C23 C6 C9 107.46(17) . . ?
C5 C6 C9 111.57(16) . . ?
C7 C6 C9 88.90(15) . . ?
N2 C7 C6 112.52(17) . . ?
N2 C7 C8 116.17(18) . . ?
C6 C7 C8 90.71(15) . . ?
C26 C8 C10 109.83(17) . . ?
C26 C8 C9 116.23(18) . . ?
C10 C8 C9 114.97(17) . . ?
C26 C8 C7 112.79(17) . . ?
C10 C8 C7 111.21(17) . . ?
C9 C8 C7 90.58(15) . . ?
N1 C9 C8 113.45(18) . . ?
N1 C9 C6 115.77(16) . . ?
C8 C9 C6 89.64(15) . . ?
C11 C10 C2 116.52(17) . . ?
C11 C10 C8 114.02(17) . . ?
C2 C10 C8 107.39(17) . . ?
C16 C11 C12 118.3(2) . . ?
C16 C11 C10 123.5(2) . . ?
C12 C11 C10 118.2(2) . . ?
C13 C12 C11 121.2(2) . . ?
C14 C13 C12 119.9(2) . . ?
C15 C14 C13 119.4(2) . . ?
C14 C15 C16 120.9(2) . . ?
C11 C16 C15 120.3(2) . . ?
O1 C17 O2 123.4(2) . . ?
O1 C17 C2 124.3(2) . . ?
O2 C17 C2 112.00(19) . . ?
O2 C18 C19 107.7(2) . . ?
O3 C20 O4 123.9(2) . . ?
O3 C20 C4 123.1(2) . . ?
O4 C20 C4 113.02(18) . . ?
O4 C21 C22 111.8(2) . . ?
O5 C23 O6 124.1(2) . . ?
O5 C23 C6 124.98(19) . . ?
O6 C23 C6 110.69(18) . . ?
O6 C24 C25 107.39(19) . . ?
O7 C26 O8 124.3(2) . . ?
O7 C26 C8 123.9(2) . . ?
O8 C26 C8 111.70(19) . . ?
C28 C27 O8 108.3(2) . . ?
C34 C29 C30 119.35(19) . . ?
C34 C29 C5 118.24(19) . . ?
C30 C29 C5 122.41(19) . . ?
C31 C30 C29 120.2(2) . . ?
O9 C31 C32 115.47(19) . . ?
O9 C31 C30 123.8(2) . . ?
C32 C31 C30 120.7(2) . . ?
O10 C32 C31 119.4(2) . . ?
O10 C32 C33 121.5(2) . . ?
C31 C32 C33 119.01(19) . . ?
O11 C33 C32 115.31(19) . . ?
O11 C33 C34 124.3(2) . . ?
C32 C33 C34 120.4(2) . . ?
C29 C34 C33 120.4(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O1 0.901(10) 2.079(12) 2.946(3) 161(2) 1_455
N2 H2 O5 0.894(10) 2.126(13) 2.981(2) 160(2) 1_655

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.060
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_sq
_database_code_depnum_ccdc_archive 'CCDC 1537244'
_audit_update_record             
;
2018-03-29 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;
_audit_creation_date             16-05-26
_audit_creation_method           
;
Rigaku CrystalClear-SM Expert 2.1 b42
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C37 H42 N2 O11'
_chemical_formula_sum            'C37 H42 N2 O11'
_chemical_formula_weight         690.72
_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'

_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                   10.9132(13)
_cell_length_b                   16.828(2)
_cell_length_c                   21.963(3)
_cell_angle_alpha                88.088(9)
_cell_angle_beta                 75.632(7)
_cell_angle_gamma                76.611(7)
_cell_volume                     3799.9(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5787
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_shelx_estimated_absorpt_T_max   0.984
_shelx_estimated_absorpt_T_min   0.980
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1464
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            48769
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.539
_diffrn_reflns_theta_min         3.060
_diffrn_ambient_temperature      113
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
scan:
	Number of images: 360
	           Slice: -105.0000 - 75.0000
	     Image width: 0.5000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.0040
	          2theta: -15.0627
scan:
	Number of images: 360
	           Slice: -105.0000 - 75.0000
	     Image width: 0.5000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.0040
	          2theta: -15.0627
scan:
	Number of images: 360
	           Slice: -105.0000 - 75.0000
	     Image width: 0.5000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.0040
	          2theta: -15.0627
;
_diffrn_measurement_device       
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.078108
_diffrn_orient_matrix_UB_12      0.057411
_diffrn_orient_matrix_UB_13      0.007294
_diffrn_orient_matrix_UB_21      -0.004568
_diffrn_orient_matrix_UB_22      -0.024722
_diffrn_orient_matrix_UB_23      0.055693
_diffrn_orient_matrix_UB_31      0.017094
_diffrn_orient_matrix_UB_32      -0.040977
_diffrn_orient_matrix_UB_33      -0.015469
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11650
_reflns_number_total             17104
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         17104
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0783
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0830P)²+5.3487P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1892
_refine_ls_wR_factor_ref         0.2147
_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
{C73, C73'}
3. Restrained distances
 C73-C74 = C73'-C74'
 1.54 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C73 \\sim C74 \\sim C73' \\sim C74': within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C73') \\sim Ueq, Uanis(C74')
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C73) = Uanis(C73')
5. Others
 Sof(C73')=Sof(H73C)=Sof(H73D)=Sof(C74')=Sof(H74D)=Sof(H74E)=Sof(H74F)=1-FVAR(1)
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C40(H40), C42(H42), C44(H44), C47(H47)
6.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C21(H21A,H21B), C33(H33A,H33B), C36(H36A,H36B), C55(H55A,
 H55B), C58(H58A,H58B), C70(H70A,H70B), C73(H73A,H73B), C73'(H73C,H73D)
6.c Me refined with riding coordinates:
 C74(H74A,H74B,H74C), C74'(H74D,H74E,H74F)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C24(H24),
 C28(H28), C38(H38), C45(H45), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53),
  C61(H61), C65(H65)
6.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C37(H37A,H37B,H37C), C56(H56A,
 H56B,H56C), C59(H59A,H59B,H59C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C),
 C68(H68A,H68B,H68C), C71(H71A,H71B,H71C)
;
_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 0.78003(19) -0.15801(11) 0.84417(9) 0.0281(4) Uani 1 1 d . . . . .
O2 O 0.8918(2) -0.10579(13) 0.75834(10) 0.0372(5) Uani 1 1 d . . . . .
O3 O 0.6613(2) -0.10340(13) 0.69021(11) 0.0421(5) Uani 1 1 d . . . . .
O4 O 0.6759(2) 0.01814(13) 0.64635(9) 0.0353(5) Uani 1 1 d . . . . .
O5 O 0.2559(2) -0.11917(13) 0.69630(12) 0.0440(6) Uani 1 1 d . . . . .
O6 O 0.1714(2) -0.02381(15) 0.60668(11) 0.0453(6) Uani 1 1 d . . . . .
O7 O 0.2052(2) 0.12809(15) 0.59103(11) 0.0473(6) Uani 1 1 d . . . . .
O8 O 0.3192(2) 0.25543(12) 0.77819(10) 0.0369(5) Uani 1 1 d . . . . .
O9 O 0.2499(2) 0.22865(13) 0.88036(10) 0.0432(6) Uani 1 1 d . . . . .
O10 O 0.5338(2) 0.19844(12) 0.98523(9) 0.0349(5) Uani 1 1 d . . . . .
O11 O 0.5809(2) 0.06914(12) 1.01732(9) 0.0410(6) Uani 1 1 d . . . . .
O12 O 0.81833(18) 0.32376(11) 0.35542(9) 0.0277(4) Uani 1 1 d . . . . .
O13 O 0.9422(2) 0.37181(12) 0.27105(10) 0.0345(5) Uani 1 1 d . . . . .
O14 O 0.6949(2) 0.36273(12) 0.20152(10) 0.0357(5) Uani 1 1 d . . . . .
O15 O 0.7373(2) 0.47446(13) 0.14997(9) 0.0318(5) Uani 1 1 d . . . . .
O16 O 0.2835(2) 0.35715(13) 0.21163(10) 0.0379(5) Uani 1 1 d . . . . .
O17 O 0.2543(2) 0.42272(14) 0.10188(10) 0.0388(5) Uani 1 1 d . . . . .
O18 O 0.3535(3) 0.55041(17) 0.05803(12) 0.0598(8) Uani 1 1 d . . . . .
O19 O 0.3585(2) 0.72360(13) 0.26264(10) 0.0399(5) Uani 1 1 d . . . . .
O20 O 0.2788(2) 0.70789(13) 0.36621(10) 0.0400(5) Uani 1 1 d . . . . .
O21 O 0.5351(2) 0.69227(12) 0.47229(10) 0.0364(5) Uani 1 1 d . . . . .
O22 O 0.5915(2) 0.56962(13) 0.51398(9) 0.0406(5) Uani 1 1 d . . . . .
N1 N 0.6745(2) 0.12877(13) 0.80060(11) 0.0267(5) Uani 1 1 d . . . . .
N2 N 0.4526(2) -0.00449(14) 0.86288(11) 0.0291(5) Uani 1 1 d . . . . .
N3 N 0.4968(2) 0.47966(14) 0.36653(10) 0.0257(5) Uani 1 1 d . . . . .
N4 N 0.7238(2) 0.60614(13) 0.29515(10) 0.0252(5) Uani 1 1 d . . . . .
C1 C 0.3816(3) 0.07293(17) 0.86412(13) 0.0266(6) Uani 1 1 d . . . . .
H1 H 0.3228 0.0941 0.9027 0.032 Uiso 1 1 calc R . . . .
C2 C 0.3885(3) 0.12254(16) 0.81406(12) 0.0247(6) Uani 1 1 d . . . . .
C3 C 0.4694(3) 0.08996(16) 0.74964(12) 0.0246(6) Uani 1 1 d . . . . .
H3 H 0.5029 0.1357 0.7263 0.029 Uiso 1 1 calc R . . . .
C4 C 0.5886(3) 0.02067(16) 0.75553(13) 0.0259(6) Uani 1 1 d . . . . .
C5 C 0.5693(3) -0.03408(16) 0.81393(13) 0.0258(6) Uani 1 1 d . . . . .
H5 H 0.5782 -0.0922 0.8015 0.031 Uiso 1 1 calc R . . . .
C6 C 0.6998(3) -0.02048(16) 0.82685(13) 0.0243(6) Uani 1 1 d . . . . .
C7 C 0.7038(3) 0.04605(16) 0.77632(13) 0.0247(6) Uani 1 1 d . . . . .
H7 H 0.7866 0.0333 0.7426 0.030 Uiso 1 1 calc R . . . .
C8 C 0.6309(3) 0.14766(16) 0.86257(13) 0.0250(6) Uani 1 1 d . . . . .
H8 H 0.5949 0.2036 0.8745 0.030 Uiso 1 1 calc R . . . .
C9 C 0.6345(3) 0.09283(16) 0.90917(13) 0.0257(6) Uani 1 1 d . . . . .
C10 C 0.6996(3) 0.00346(16) 0.89459(12) 0.0247(6) Uani 1 1 d . . . . .
H10 H 0.6485 -0.0299 0.9247 0.030 Uiso 1 1 calc R . . . .
C11 C 0.8375(3) -0.01486(17) 0.90408(14) 0.0311(6) Uani 1 1 d . . . . .
C12 C 0.8701(4) -0.0659(2) 0.95129(16) 0.0443(8) Uani 1 1 d . . . . .
H12 H 0.8060 -0.0889 0.9787 0.053 Uiso 1 1 calc R . . . .
C13 C 0.9980(5) -0.0838(2) 0.9586(2) 0.0620(12) Uani 1 1 d . . . . .
H13 H 1.0202 -0.1191 0.9908 0.074 Uiso 1 1 calc R . . . .
C14 C 1.0922(4) -0.0500(3) 0.9189(2) 0.0639(12) Uani 1 1 d . . . . .
H14 H 1.1782 -0.0618 0.9243 0.077 Uiso 1 1 calc R . . . .
C15 C 1.0616(4) -0.0002(3) 0.8724(2) 0.0585(11) Uani 1 1 d . . . . .
H15 H 1.1261 0.0222 0.8448 0.070 Uiso 1 1 calc R . . . .
C16 C 0.9340(3) 0.0177(2) 0.86544(17) 0.0445(8) Uani 1 1 d . . . . .
H16 H 0.9128 0.0534 0.8332 0.053 Uiso 1 1 calc R . . . .
C17 C 0.8037(3) -0.09804(17) 0.80475(13) 0.0269(6) Uani 1 1 d . . . . .
C18 C 0.8707(3) -0.23762(16) 0.82971(15) 0.0328(7) Uani 1 1 d . . . . .
H18A H 0.8956 -0.2481 0.7837 0.039 Uiso 1 1 calc R . . . .
H18B H 0.8274 -0.2808 0.8498 0.039 Uiso 1 1 calc R . . . .
C19 C 0.9907(3) -0.2415(2) 0.85249(17) 0.0450(8) Uani 1 1 d . . . . .
H19A H 1.0308 -0.1968 0.8346 0.068 Uiso 1 1 calc GR . . . .
H19B H 1.0523 -0.2940 0.8392 0.068 Uiso 1 1 calc GR . . . .
H19C H 0.9672 -0.2364 0.8985 0.068 Uiso 1 1 calc GR . . . .
C20 C 0.6441(3) -0.03021(18) 0.69486(14) 0.0298(6) Uani 1 1 d . . . . .
C21 C 0.7217(4) -0.0196(2) 0.58316(15) 0.0457(8) Uani 1 1 d . . . . .
H21A H 0.7780 0.0124 0.5556 0.055 Uiso 1 1 calc R . . . .
H21B H 0.7744 -0.0756 0.5852 0.055 Uiso 1 1 calc R . . . .
C22 C 0.6136(5) -0.0232(4) 0.5562(2) 0.0789(15) Uani 1 1 d . . . . .
H22A H 0.5584 -0.0555 0.5830 0.118 Uiso 1 1 calc GR . . . .
H22B H 0.6475 -0.0488 0.5141 0.118 Uiso 1 1 calc GR . . . .
H22C H 0.5622 0.0322 0.5533 0.118 Uiso 1 1 calc GR . . . .
C23 C 0.3854(3) 0.06084(16) 0.71306(13) 0.0263(6) Uani 1 1 d . . . . .
C24 C 0.3556(3) -0.01543(17) 0.72498(14) 0.0314(6) Uani 1 1 d . . . . .
H24 H 0.3845 -0.0480 0.7571 0.038 Uiso 1 1 calc R . . . .
C25 C 0.2838(3) -0.04380(18) 0.68987(15) 0.0328(7) Uani 1 1 d . . . . .
C26 C 0.2372(3) 0.0053(2) 0.64411(14) 0.0343(7) Uani 1 1 d . . . . .
C27 C 0.2606(3) 0.08370(19) 0.63460(14) 0.0325(7) Uani 1 1 d . . . . .
C28 C 0.3367(3) 0.11045(18) 0.66821(14) 0.0303(6) Uani 1 1 d . . . . .
H28 H 0.3556 0.1628 0.6606 0.036 Uiso 1 1 calc R . . . .
C29 C 0.3019(4) -0.1706(2) 0.7431(2) 0.0562(10) Uani 1 1 d . . . . .
H29A H 0.3970 -0.1816 0.7333 0.084 Uiso 1 1 calc GR . . . .
H29B H 0.2748 -0.2223 0.7436 0.084 Uiso 1 1 calc GR . . . .
H29C H 0.2654 -0.1431 0.7845 0.084 Uiso 1 1 calc GR . . . .
C30 C 0.0362(3) -0.0118(2) 0.6350(2) 0.0515(9) Uani 1 1 d . . . . .
H30A H 0.0235 -0.0395 0.6753 0.077 Uiso 1 1 calc GR . . . .
H30B H -0.0055 -0.0344 0.6071 0.077 Uiso 1 1 calc GR . . . .
H30C H -0.0027 0.0468 0.6421 0.077 Uiso 1 1 calc GR . . . .
C31 C 0.2284(5) 0.2071(3) 0.5790(2) 0.0731(15) Uani 1 1 d . . . . .
H31A H 0.1870 0.2423 0.6166 0.110 Uiso 1 1 calc GR . . . .
H31B H 0.1922 0.2303 0.5440 0.110 Uiso 1 1 calc GR . . . .
H31C H 0.3223 0.2035 0.5681 0.110 Uiso 1 1 calc GR . . . .
C32 C 0.3177(3) 0.20694(17) 0.82074(13) 0.0288(6) Uani 1 1 d . . . . .
C33 C 0.1802(4) 0.3124(2) 0.89325(19) 0.0560(10) Uani 1 1 d . . . . .
H33A H 0.1180 0.3287 0.8666 0.067 Uiso 1 1 calc R . . . .
H33B H 0.2410 0.3493 0.8854 0.067 Uiso 1 1 calc R . . . .
C34 C 0.1090(5) 0.3157(3) 0.9621(2) 0.0871(17) Uani 1 1 d . . . . .
H34A H 0.0483 0.2797 0.9688 0.131 Uiso 1 1 calc GR . . . .
H34B H 0.0608 0.3718 0.9746 0.131 Uiso 1 1 calc GR . . . .
H34C H 0.1720 0.2977 0.9876 0.131 Uiso 1 1 calc GR . . . .
C35 C 0.5821(3) 0.11776(17) 0.97471(13) 0.0289(6) Uani 1 1 d . . . . .
C36 C 0.4673(4) 0.2251(2) 1.04999(16) 0.0482(9) Uani 1 1 d . . . . .
H36A H 0.4124 0.1869 1.0688 0.058 Uiso 1 1 calc R . . . .
H36B H 0.4093 0.2799 1.0499 0.058 Uiso 1 1 calc R . . . .
C37 C 0.5587(5) 0.2288(2) 1.08947(19) 0.0691(13) Uani 1 1 d . . . . .
H37A H 0.6045 0.1733 1.0966 0.104 Uiso 1 1 calc GR . . . .
H37B H 0.5099 0.2559 1.1299 0.104 Uiso 1 1 calc GR . . . .
H37C H 0.6219 0.2598 1.0679 0.104 Uiso 1 1 calc GR . . . .
C38 C 0.4231(3) 0.55505(16) 0.36198(13) 0.0249(6) Uani 1 1 d . . . . .
H38 H 0.3597 0.5790 0.3985 0.030 Uiso 1 1 calc R . . . .
C39 C 0.4337(3) 0.59870(16) 0.30867(13) 0.0249(6) Uani 1 1 d . . . . .
C40 C 0.5226(3) 0.56122(16) 0.24675(12) 0.0235(5) Uani 1 1 d . . . . .
H40 H 0.5588 0.6051 0.2220 0.028 Uiso 1 1 calc R . . . .
C41 C 0.6378(3) 0.49325(16) 0.25787(12) 0.0229(5) Uani 1 1 d . . . . .
C42 C 0.6144(3) 0.44534(16) 0.31953(12) 0.0229(5) Uani 1 1 d . . . . .
H42 H 0.6220 0.3862 0.3109 0.027 Uiso 1 1 calc R . . . .
C43 C 0.7442(3) 0.46043(16) 0.33164(12) 0.0234(5) Uani 1 1 d . . . . .
C44 C 0.7534(3) 0.52087(16) 0.27636(12) 0.0240(6) Uani 1 1 d . . . . .
H44 H 0.8371 0.5046 0.2435 0.029 Uiso 1 1 calc R . . . .
C45 C 0.6673(3) 0.63174(16) 0.35509(12) 0.0240(6) Uani 1 1 d . . . . .
H45 H 0.6251 0.6879 0.3626 0.029 Uiso 1 1 calc R . . . .
C46 C 0.6665(3) 0.58285(15) 0.40550(12) 0.0231(5) Uani 1 1 d . . . . .
C47 C 0.7390(3) 0.49400(16) 0.39735(12) 0.0241(6) Uani 1 1 d . . . . .
H47 H 0.6898 0.4622 0.4298 0.029 Uiso 1 1 calc R . . . .
C48 C 0.8764(3) 0.48190(17) 0.40717(13) 0.0291(6) Uani 1 1 d . . . . .
C49 C 0.9646(3) 0.5238(2) 0.37165(16) 0.0414(8) Uani 1 1 d . . . . .
H49 H 0.9374 0.5629 0.3426 0.050 Uiso 1 1 calc R . . . .
C50 C 1.0919(4) 0.5098(3) 0.37785(18) 0.0524(9) Uani 1 1 d . . . . .
H50 H 1.1507 0.5385 0.3527 0.063 Uiso 1 1 calc R . . . .
C51 C 1.1325(4) 0.4544(2) 0.42031(18) 0.0502(9) Uani 1 1 d . . . . .
H51 H 1.2189 0.4450 0.4249 0.060 Uiso 1 1 calc R . . . .
C52 C 1.0464(4) 0.4128(2) 0.45594(18) 0.0493(9) Uani 1 1 d . . . . .
H52 H 1.0738 0.3745 0.4854 0.059 Uiso 1 1 calc R . . . .
C53 C 0.9189(3) 0.42603(19) 0.44946(15) 0.0383(7) Uani 1 1 d . . . . .
H53 H 0.8609 0.3964 0.4743 0.046 Uiso 1 1 calc R . . . .
C54 C 0.8486(3) 0.38155(16) 0.31503(12) 0.0244(6) Uani 1 1 d . . . . .
C55 C 0.9064(3) 0.24226(17) 0.34406(15) 0.0341(7) Uani 1 1 d . . . . .
H55A H 0.9382 0.2310 0.2982 0.041 Uiso 1 1 calc R . . . .
H55B H 0.8578 0.2007 0.3624 0.041 Uiso 1 1 calc R . . . .
C56 C 1.0197(3) 0.2352(2) 0.37191(18) 0.0458(8) Uani 1 1 d . . . . .
H56A H 1.0645 0.2788 0.3562 0.069 Uiso 1 1 calc GR . . . .
H56B H 1.0799 0.1820 0.3600 0.069 Uiso 1 1 calc GR . . . .
H56C H 0.9893 0.2403 0.4178 0.069 Uiso 1 1 calc GR . . . .
C57 C 0.6923(3) 0.43461(17) 0.20124(13) 0.0269(6) Uani 1 1 d . . . . .
C58 C 0.7697(3) 0.4290(2) 0.09051(14) 0.0408(8) Uani 1 1 d . . . . .
H58A H 0.6931 0.4107 0.0851 0.049 Uiso 1 1 calc R . . . .
H58B H 0.8410 0.3802 0.0900 0.049 Uiso 1 1 calc R . . . .
C59 C 0.8107(4) 0.4838(3) 0.03908(16) 0.0500(9) Uani 1 1 d . . . . .
H59A H 0.7423 0.5338 0.0420 0.075 Uiso 1 1 calc GR . . . .
H59B H 0.8260 0.4560 -0.0016 0.075 Uiso 1 1 calc GR . . . .
H59C H 0.8910 0.4976 0.0428 0.075 Uiso 1 1 calc GR . . . .
C60 C 0.4458(3) 0.52689(17) 0.20885(13) 0.0259(6) Uani 1 1 d . . . . .
C61 C 0.3931(3) 0.46079(17) 0.23141(13) 0.0285(6) Uani 1 1 d . . . . .
H61 H 0.3995 0.4399 0.2715 0.034 Uiso 1 1 calc R . . . .
C62 C 0.3311(3) 0.42528(17) 0.19544(14) 0.0293(6) Uani 1 1 d . . . . .
C63 C 0.3172(3) 0.45787(18) 0.13751(14) 0.0316(6) Uani 1 1 d . . . . .
C64 C 0.3699(3) 0.5238(2) 0.11508(14) 0.0361(7) Uani 1 1 d . . . . .
C65 C 0.4358(3) 0.55771(18) 0.15076(14) 0.0332(7) Uani 1 1 d . . . . .
H65 H 0.4738 0.6020 0.1350 0.040 Uiso 1 1 calc R . . . .
C66 C 0.3105(4) 0.3161(2) 0.26638(17) 0.0478(9) Uani 1 1 d . . . . .
H66A H 0.4046 0.3020 0.2621 0.072 Uiso 1 1 calc GR . . . .
H66B H 0.2778 0.2661 0.2711 0.072 Uiso 1 1 calc GR . . . .
H66C H 0.2676 0.3520 0.3035 0.072 Uiso 1 1 calc GR . . . .
C67 C 0.1163(3) 0.4489(2) 0.12246(17) 0.0425(8) Uani 1 1 d . . . . .
H67A H 0.0877 0.4339 0.1663 0.064 Uiso 1 1 calc GR . . . .
H67B H 0.0761 0.4224 0.0961 0.064 Uiso 1 1 calc GR . . . .
H67C H 0.0903 0.5083 0.1191 0.064 Uiso 1 1 calc GR . . . .
C68 C 0.4152(7) 0.6145(4) 0.0322(2) 0.112(3) Uani 1 1 d . . . . .
H68A H 0.3704 0.6654 0.0563 0.168 Uiso 1 1 calc GR . . . .
H68B H 0.4112 0.6218 -0.0118 0.168 Uiso 1 1 calc GR . . . .
H68C H 0.5062 0.6002 0.0344 0.168 Uiso 1 1 calc GR . . . .
C69 C 0.3561(3) 0.68101(17) 0.30906(14) 0.0298(6) Uani 1 1 d . . . . .
C70 C 0.1978(4) 0.7895(2) 0.37125(18) 0.0506(9) Uani 1 1 d . . . . .
H70A H 0.1427 0.7963 0.3409 0.061 Uiso 1 1 calc R . . . .
H70B H 0.2518 0.8303 0.3625 0.061 Uiso 1 1 calc R . . . .
C71 C 0.1147(4) 0.8002(3) 0.4376(2) 0.0631(11) Uani 1 1 d . . . . .
H71A H 0.0662 0.7571 0.4464 0.095 Uiso 1 1 calc GR . . . .
H71B H 0.0536 0.8537 0.4427 0.095 Uiso 1 1 calc GR . . . .
H71C H 0.1703 0.7968 0.4669 0.095 Uiso 1 1 calc GR . . . .
C72 C 0.5963(3) 0.61270(16) 0.46809(13) 0.0271(6) Uani 1 1 d . . . . .
C73 C 0.4580(4) 0.7240(2) 0.53381(17) 0.0544(10) Uani 0.590(9) 1 d D U P A 1
H73A H 0.5119 0.7147 0.5647 0.065 Uiso 0.590(9) 1 calc R . P A 1
H73B H 0.3848 0.6969 0.5484 0.065 Uiso 0.590(9) 1 calc R . P A 1
C74 C 0.4086(7) 0.8134(3) 0.5263(4) 0.065(2) Uani 0.590(9) 1 d D U P A 1
H74A H 0.3553 0.8382 0.5668 0.098 Uiso 0.590(9) 1 calc R . P A 1
H74B H 0.4823 0.8391 0.5117 0.098 Uiso 0.590(9) 1 calc R . P A 1
H74C H 0.3558 0.8214 0.4954 0.098 Uiso 0.590(9) 1 calc R . P A 1
C73' C 0.4580(4) 0.7240(2) 0.53381(17) 0.0544(10) Uani 0.410(9) 1 d D U P A 2
H73C H 0.4068 0.6840 0.5529 0.065 Uiso 0.410(9) 1 calc R . P A 2
H73D H 0.3954 0.7748 0.5280 0.065 Uiso 0.410(9) 1 calc R . P A 2
C74' C 0.5298(11) 0.7426(7) 0.5802(4) 0.069(3) Uani 0.410(9) 1 d D U P A 2
H74D H 0.4673 0.7635 0.6198 0.103 Uiso 0.410(9) 1 calc R . P A 2
H74E H 0.5901 0.6925 0.5880 0.103 Uiso 0.410(9) 1 calc R . P A 2
H74F H 0.5787 0.7837 0.5630 0.103 Uiso 0.410(9) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C17 1.337(3) . ?
O1 C18 1.461(3) . ?
O2 C17 1.202(3) . ?
O3 C20 1.206(3) . ?
O4 C20 1.344(4) . ?
O4 C21 1.465(4) . ?
O5 C25 1.367(3) . ?
O5 C29 1.433(4) . ?
O6 C26 1.383(4) . ?
O6 C30 1.421(4) . ?
O7 C27 1.367(4) . ?
O7 C31 1.415(4) . ?
O8 C32 1.219(3) . ?
O9 C32 1.350(3) . ?
O9 C33 1.439(4) . ?
O10 C35 1.343(3) . ?
O10 C36 1.459(4) . ?
O11 C35 1.222(3) . ?
O12 C54 1.337(3) . ?
O12 C55 1.470(3) . ?
O13 C54 1.202(3) . ?
O14 C57 1.203(3) . ?
O15 C57 1.337(3) . ?
O15 C58 1.459(3) . ?
O16 C62 1.367(3) . ?
O16 C66 1.427(4) . ?
O17 C63 1.385(3) . ?
O17 C67 1.426(4) . ?
O18 C64 1.356(4) . ?
O18 C68 1.430(5) . ?
O19 C69 1.225(3) . ?
O20 C69 1.352(4) . ?
O20 C70 1.442(4) . ?
O21 C72 1.346(3) . ?
O21 C73 1.447(4) . ?
O21 C73' 1.447(4) . ?
O22 C72 1.219(3) . ?
N1 C7 1.443(3) . ?
N1 C8 1.348(3) . ?
N2 C1 1.350(4) . ?
N2 C5 1.445(4) . ?
N3 C38 1.351(3) . ?
N3 C42 1.443(3) . ?
N4 C44 1.446(3) . ?
N4 C45 1.346(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.356(4) . ?
C2 C3 1.513(4) . ?
C2 C32 1.444(4) . ?
C3 H3 1.0000 . ?
C3 C4 1.562(4) . ?
C3 C23 1.525(4) . ?
C4 C5 1.554(4) . ?
C4 C7 1.586(4) . ?
C4 C20 1.520(4) . ?
C5 H5 1.0000 . ?
C5 C6 1.586(4) . ?
C6 C7 1.550(4) . ?
C6 C10 1.553(4) . ?
C6 C17 1.519(4) . ?
C7 H7 1.0000 . ?
C8 H8 0.9500 . ?
C8 C9 1.357(4) . ?
C9 C10 1.514(4) . ?
C9 C35 1.448(4) . ?
C10 H10 1.0000 . ?
C10 C11 1.530(4) . ?
C11 C12 1.387(4) . ?
C11 C16 1.387(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.407(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.390(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.355(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.401(5) . ?
C16 H16 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.500(5) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.459(6) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.396(4) . ?
C23 C28 1.396(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.391(4) . ?
C25 C26 1.399(4) . ?
C26 C27 1.400(4) . ?
C27 C28 1.391(4) . ?
C28 H28 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.516(6) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.488(6) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38 0.9500 . ?
C38 C39 1.356(4) . ?
C39 C40 1.519(4) . ?
C39 C69 1.446(4) . ?
C40 H40 1.0000 . ?
C40 C41 1.555(4) . ?
C40 C60 1.528(4) . ?
C41 C42 1.549(4) . ?
C41 C44 1.585(4) . ?
C41 C57 1.522(4) . ?
C42 H42 1.0000 . ?
C42 C43 1.582(4) . ?
C43 C44 1.557(4) . ?
C43 C47 1.550(4) . ?
C43 C54 1.523(4) . ?
C44 H44 1.0000 . ?
C45 H45 0.9500 . ?
C45 C46 1.357(4) . ?
C46 C47 1.514(4) . ?
C46 C72 1.440(4) . ?
C47 H47 1.0000 . ?
C47 C48 1.534(4) . ?
C48 C49 1.392(4) . ?
C48 C53 1.384(4) . ?
C49 H49 0.9500 . ?
C49 C50 1.394(5) . ?
C50 H50 0.9500 . ?
C50 C51 1.375(5) . ?
C51 H51 0.9500 . ?
C51 C52 1.374(6) . ?
C52 H52 0.9500 . ?
C52 C53 1.400(5) . ?
C53 H53 0.9500 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 C56 1.490(5) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C59 1.482(5) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 C61 1.390(4) . ?
C60 C65 1.381(4) . ?
C61 H61 0.9500 . ?
C61 C62 1.386(4) . ?
C62 C63 1.398(4) . ?
C63 C64 1.387(4) . ?
C64 C65 1.398(4) . ?
C65 H65 0.9500 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C70 C71 1.504(5) . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C73 C74 1.495(6) . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C73' H73C 0.9900 . ?
C73' H73D 0.9900 . ?
C73' C74' 1.511(8) . ?
C74' H74D 0.9800 . ?
C74' H74E 0.9800 . ?
C74' H74F 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
C17 O1 C18 116.6(2) . . ?
C20 O4 C21 117.6(2) . . ?
C25 O5 C29 117.2(3) . . ?
C26 O6 C30 112.7(3) . . ?
C27 O7 C31 117.1(3) . . ?
C32 O9 C33 117.9(3) . . ?
C35 O10 C36 116.6(2) . . ?
C54 O12 C55 116.7(2) . . ?
C57 O15 C58 115.5(2) . . ?
C62 O16 C66 117.1(2) . . ?
C63 O17 C67 112.3(2) . . ?
C64 O18 C68 116.3(3) . . ?
C69 O20 C70 117.7(2) . . ?
C72 O21 C73 116.7(2) . . ?
C72 O21 C73' 116.7(2) . . ?
C8 N1 C7 122.4(2) . . ?
C1 N2 C5 121.6(2) . . ?
C38 N3 C42 122.4(2) . . ?
C45 N4 C44 121.7(2) . . ?
N2 C1 H1 117.7 . . ?
N2 C1 C2 124.5(3) . . ?
C2 C1 H1 117.7 . . ?
C1 C2 C3 120.4(2) . . ?
C1 C2 C32 121.0(3) . . ?
C32 C2 C3 118.6(2) . . ?
C2 C3 H3 108.1 . . ?
C2 C3 C4 110.5(2) . . ?
C2 C3 C23 110.2(2) . . ?
C4 C3 H3 108.1 . . ?
C23 C3 H3 108.1 . . ?
C23 C3 C4 111.8(2) . . ?
C3 C4 C7 117.8(2) . . ?
C5 C4 C3 116.9(2) . . ?
C5 C4 C7 89.6(2) . . ?
C20 C4 C3 110.4(2) . . ?
C20 C4 C5 111.6(2) . . ?
C20 C4 C7 108.9(2) . . ?
N2 C5 C4 115.4(2) . . ?
N2 C5 H5 111.5 . . ?
N2 C5 C6 115.7(2) . . ?
C4 C5 H5 111.5 . . ?
C4 C5 C6 89.5(2) . . ?
C6 C5 H5 111.5 . . ?
C7 C6 C5 89.7(2) . . ?
C7 C6 C10 118.2(2) . . ?
C10 C6 C5 118.7(2) . . ?
C17 C6 C5 106.9(2) . . ?
C17 C6 C7 111.9(2) . . ?
C17 C6 C10 109.7(2) . . ?
N1 C7 C4 115.0(2) . . ?
N1 C7 C6 115.0(2) . . ?
N1 C7 H7 111.8 . . ?
C4 C7 H7 111.8 . . ?
C6 C7 C4 89.64(19) . . ?
C6 C7 H7 111.8 . . ?
N1 C8 H8 117.5 . . ?
N1 C8 C9 124.9(2) . . ?
C9 C8 H8 117.5 . . ?
C8 C9 C10 121.0(2) . . ?
C8 C9 C35 121.6(2) . . ?
C35 C9 C10 117.4(2) . . ?
C6 C10 H10 108.1 . . ?
C9 C10 C6 110.8(2) . . ?
C9 C10 H10 108.1 . . ?
C9 C10 C11 110.2(2) . . ?
C11 C10 C6 111.4(2) . . ?
C11 C10 H10 108.1 . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 C16 118.0(3) . . ?
C16 C11 C10 121.4(3) . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.0(4) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 119.9 . . ?
C14 C13 C12 120.3(4) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 H14 119.9 . . ?
C15 C14 C13 120.2(4) . . ?
C15 C14 H14 119.9 . . ?
C14 C15 H15 120.3 . . ?
C14 C15 C16 119.4(4) . . ?
C16 C15 H15 120.3 . . ?
C11 C16 C15 122.1(4) . . ?
C11 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?
O1 C17 C6 109.3(2) . . ?
O2 C17 O1 124.7(3) . . ?
O2 C17 C6 126.0(3) . . ?
O1 C18 H18A 109.3 . . ?
O1 C18 H18B 109.3 . . ?
O1 C18 C19 111.5(2) . . ?
H18A C18 H18B 108.0 . . ?
C19 C18 H18A 109.3 . . ?
C19 C18 H18B 109.3 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O3 C20 O4 124.1(3) . . ?
O3 C20 C4 125.9(3) . . ?
O4 C20 C4 110.0(2) . . ?
O4 C21 H21A 109.3 . . ?
O4 C21 H21B 109.3 . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 O4 111.6(3) . . ?
C22 C21 H21A 109.3 . . ?
C22 C21 H21B 109.3 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C3 119.9(2) . . ?
C24 C23 C28 119.8(3) . . ?
C28 C23 C3 120.4(2) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 C23 120.1(3) . . ?
C25 C24 H24 120.0 . . ?
O5 C25 C24 123.9(3) . . ?
O5 C25 C26 116.0(3) . . ?
C24 C25 C26 120.0(3) . . ?
O6 C26 C25 120.6(3) . . ?
O6 C26 C27 119.5(3) . . ?
C25 C26 C27 119.9(3) . . ?
O7 C27 C26 115.1(3) . . ?
O7 C27 C28 125.1(3) . . ?
C28 C27 C26 119.7(3) . . ?
C23 C28 H28 119.8 . . ?
C27 C28 C23 120.4(3) . . ?
C27 C28 H28 119.8 . . ?
O5 C29 H29A 109.5 . . ?
O5 C29 H29B 109.5 . . ?
O5 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O6 C30 H30A 109.5 . . ?
O6 C30 H30B 109.5 . . ?
O6 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O7 C31 H31A 109.5 . . ?
O7 C31 H31B 109.5 . . ?
O7 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O8 C32 O9 122.1(3) . . ?
O8 C32 C2 124.9(3) . . ?
O9 C32 C2 112.9(2) . . ?
O9 C33 H33A 110.7 . . ?
O9 C33 H33B 110.7 . . ?
O9 C33 C34 105.0(3) . . ?
H33A C33 H33B 108.8 . . ?
C34 C33 H33A 110.7 . . ?
C34 C33 H33B 110.7 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O10 C35 C9 115.0(2) . . ?
O11 C35 O10 122.4(3) . . ?
O11 C35 C9 122.7(3) . . ?
O10 C36 H36A 109.0 . . ?
O10 C36 H36B 109.0 . . ?
O10 C36 C37 112.8(3) . . ?
H36A C36 H36B 107.8 . . ?
C37 C36 H36A 109.0 . . ?
C37 C36 H36B 109.0 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N3 C38 H38 117.9 . . ?
N3 C38 C39 124.3(3) . . ?
C39 C38 H38 117.9 . . ?
C38 C39 C40 121.0(2) . . ?
C38 C39 C69 120.5(3) . . ?
C69 C39 C40 118.5(2) . . ?
C39 C40 H40 108.4 . . ?
C39 C40 C41 111.1(2) . . ?
C39 C40 C60 110.2(2) . . ?
C41 C40 H40 108.4 . . ?
C60 C40 H40 108.4 . . ?
C60 C40 C41 110.4(2) . . ?
C40 C41 C44 117.7(2) . . ?
C42 C41 C40 117.5(2) . . ?
C42 C41 C44 90.07(19) . . ?
C57 C41 C40 110.1(2) . . ?
C57 C41 C42 110.5(2) . . ?
C57 C41 C44 109.4(2) . . ?
N3 C42 C41 115.6(2) . . ?
N3 C42 H42 111.5 . . ?
N3 C42 C43 115.7(2) . . ?
C41 C42 H42 111.5 . . ?
C41 C42 C43 89.45(19) . . ?
C43 C42 H42 111.5 . . ?
C44 C43 C42 89.91(19) . . ?
C47 C43 C42 117.9(2) . . ?
C47 C43 C44 117.2(2) . . ?
C54 C43 C42 108.0(2) . . ?
C54 C43 C44 111.4(2) . . ?
C54 C43 C47 110.7(2) . . ?
N4 C44 C41 114.0(2) . . ?
N4 C44 C43 114.9(2) . . ?
N4 C44 H44 112.3 . . ?
C41 C44 H44 112.3 . . ?
C43 C44 C41 89.07(19) . . ?
C43 C44 H44 112.3 . . ?
N4 C45 H45 117.8 . . ?
N4 C45 C46 124.4(2) . . ?
C46 C45 H45 117.8 . . ?
C45 C46 C47 120.6(2) . . ?
C45 C46 C72 121.7(2) . . ?
C72 C46 C47 117.7(2) . . ?
C43 C47 H47 108.0 . . ?
C46 C47 C43 110.3(2) . . ?
C46 C47 H47 108.0 . . ?
C46 C47 C48 111.8(2) . . ?
C48 C47 C43 110.6(2) . . ?
C48 C47 H47 108.0 . . ?
C49 C48 C47 121.1(3) . . ?
C53 C48 C47 121.1(3) . . ?
C53 C48 C49 117.8(3) . . ?
C48 C49 H49 119.3 . . ?
C48 C49 C50 121.4(3) . . ?
C50 C49 H49 119.3 . . ?
C49 C50 H50 119.9 . . ?
C51 C50 C49 120.2(4) . . ?
C51 C50 H50 119.9 . . ?
C50 C51 H51 120.4 . . ?
C52 C51 C50 119.1(3) . . ?
C52 C51 H51 120.4 . . ?
C51 C52 H52 119.5 . . ?
C51 C52 C53 121.0(3) . . ?
C53 C52 H52 119.5 . . ?
C48 C53 C52 120.5(3) . . ?
C48 C53 H53 119.7 . . ?
C52 C53 H53 119.7 . . ?
O12 C54 C43 109.8(2) . . ?
O13 C54 O12 125.0(3) . . ?
O13 C54 C43 125.2(2) . . ?
O12 C55 H55A 109.2 . . ?
O12 C55 H55B 109.2 . . ?
O12 C55 C56 112.0(2) . . ?
H55A C55 H55B 107.9 . . ?
C56 C55 H55A 109.2 . . ?
C56 C55 H55B 109.2 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
O14 C57 O15 124.0(3) . . ?
O14 C57 C41 125.8(3) . . ?
O15 C57 C41 110.2(2) . . ?
O15 C58 H58A 110.1 . . ?
O15 C58 H58B 110.1 . . ?
O15 C58 C59 108.0(3) . . ?
H58A C58 H58B 108.4 . . ?
C59 C58 H58A 110.1 . . ?
C59 C58 H58B 110.1 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C61 C60 C40 119.4(2) . . ?
C65 C60 C40 120.3(2) . . ?
C65 C60 C61 120.1(3) . . ?
C60 C61 H61 120.0 . . ?
C62 C61 C60 120.0(3) . . ?
C62 C61 H61 120.0 . . ?
O16 C62 C61 124.5(3) . . ?
O16 C62 C63 115.5(2) . . ?
C61 C62 C63 120.0(3) . . ?
O17 C63 C62 120.0(3) . . ?
O17 C63 C64 120.3(3) . . ?
C64 C63 C62 119.7(3) . . ?
O18 C64 C63 115.6(3) . . ?
O18 C64 C65 124.5(3) . . ?
C63 C64 C65 119.8(3) . . ?
C60 C65 C64 120.1(3) . . ?
C60 C65 H65 119.9 . . ?
C64 C65 H65 119.9 . . ?
O16 C66 H66A 109.5 . . ?
O16 C66 H66B 109.5 . . ?
O16 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
O17 C67 H67A 109.5 . . ?
O17 C67 H67B 109.5 . . ?
O17 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
O18 C68 H68A 109.5 . . ?
O18 C68 H68B 109.5 . . ?
O18 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
O19 C69 O20 122.0(3) . . ?
O19 C69 C39 124.3(3) . . ?
O20 C69 C39 113.7(2) . . ?
O20 C70 H70A 110.5 . . ?
O20 C70 H70B 110.5 . . ?
O20 C70 C71 106.3(3) . . ?
H70A C70 H70B 108.7 . . ?
C71 C70 H70A 110.5 . . ?
C71 C70 H70B 110.5 . . ?
C70 C71 H71A 109.5 . . ?
C70 C71 H71B 109.5 . . ?
C70 C71 H71C 109.5 . . ?
H71A C71 H71B 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
O21 C72 C46 114.8(2) . . ?
O22 C72 O21 122.1(3) . . ?
O22 C72 C46 123.1(3) . . ?
O21 C73 H73A 110.6 . . ?
O21 C73 H73B 110.6 . . ?
O21 C73 C74 105.9(4) . . ?
H73A C73 H73B 108.7 . . ?
C74 C73 H73A 110.6 . . ?
C74 C73 H73B 110.6 . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
O21 C73' H73C 108.0 . . ?
O21 C73' H73D 108.0 . . ?
O21 C73' C74' 117.3(5) . . ?
H73C C73' H73D 107.2 . . ?
C74' C73' H73C 108.0 . . ?
C74' C73' H73D 108.0 . . ?
C73' C74' H74D 109.5 . . ?
C73' C74' H74E 109.5 . . ?
C73' C74' H74F 109.5 . . ?
H74D C74' H74E 109.5 . . ?
H74D C74' H74F 109.5 . . ?
H74E C74' H74F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 C25 C26 O6 -2.4(4) . . . . ?
O5 C25 C26 C27 179.6(3) . . . . ?
O6 C26 C27 O7 5.2(4) . . . . ?
O6 C26 C27 C28 -174.2(3) . . . . ?
O7 C27 C28 C23 178.1(3) . . . . ?
O16 C62 C63 O17 2.2(4) . . . . ?
O16 C62 C63 C64 -175.8(3) . . . . ?
O17 C63 C64 O18 0.9(5) . . . . ?
O17 C63 C64 C65 -178.5(3) . . . . ?
O18 C64 C65 C60 179.1(3) . . . . ?
N1 C8 C9 C10 4.8(4) . . . . ?
N1 C8 C9 C35 -178.1(3) . . . . ?
N2 C1 C2 C3 6.4(4) . . . . ?
N2 C1 C2 C32 -174.4(3) . . . . ?
N2 C5 C6 C7 -108.4(2) . . . . ?
N2 C5 C6 C10 14.1(3) . . . . ?
N2 C5 C6 C17 138.7(2) . . . . ?
N3 C38 C39 C40 6.5(4) . . . . ?
N3 C38 C39 C69 -176.2(3) . . . . ?
N3 C42 C43 C44 -109.1(2) . . . . ?
N3 C42 C43 C47 12.1(3) . . . . ?
N3 C42 C43 C54 138.4(2) . . . . ?
N4 C45 C46 C47 3.8(4) . . . . ?
N4 C45 C46 C72 -175.5(3) . . . . ?
C1 N2 C5 C4 -14.2(4) . . . . ?
C1 N2 C5 C6 88.4(3) . . . . ?
C1 C2 C3 C4 -30.9(3) . . . . ?
C1 C2 C3 C23 93.1(3) . . . . ?
C1 C2 C32 O8 179.7(3) . . . . ?
C1 C2 C32 O9 1.1(4) . . . . ?
C2 C3 C4 C5 32.7(3) . . . . ?
C2 C3 C4 C7 -72.3(3) . . . . ?
C2 C3 C4 C20 161.6(2) . . . . ?
C2 C3 C23 C24 -79.6(3) . . . . ?
C2 C3 C23 C28 99.6(3) . . . . ?
C3 C2 C32 O8 -1.2(4) . . . . ?
C3 C2 C32 O9 -179.7(2) . . . . ?
C3 C4 C5 N2 -12.4(3) . . . . ?
C3 C4 C5 C6 -130.8(2) . . . . ?
C3 C4 C7 N1 12.6(3) . . . . ?
C3 C4 C7 C6 130.2(2) . . . . ?
C3 C4 C20 O3 -125.5(3) . . . . ?
C3 C4 C20 O4 56.5(3) . . . . ?
C3 C23 C24 C25 -177.2(3) . . . . ?
C3 C23 C28 C27 179.7(3) . . . . ?
C4 C3 C23 C24 43.6(3) . . . . ?
C4 C3 C23 C28 -137.1(3) . . . . ?
C4 C5 C6 C7 9.7(2) . . . . ?
C4 C5 C6 C10 132.2(2) . . . . ?
C4 C5 C6 C17 -103.2(2) . . . . ?
C5 N2 C1 C2 18.7(4) . . . . ?
C5 C4 C7 N1 -107.9(2) . . . . ?
C5 C4 C7 C6 9.7(2) . . . . ?
C5 C4 C20 O3 6.3(4) . . . . ?
C5 C4 C20 O4 -171.7(2) . . . . ?
C5 C6 C7 N1 108.1(2) . . . . ?
C5 C6 C7 C4 -9.53(19) . . . . ?
C5 C6 C10 C9 -76.9(3) . . . . ?
C5 C6 C10 C11 160.1(2) . . . . ?
C5 C6 C17 O1 -71.2(3) . . . . ?
C5 C6 C17 O2 107.0(3) . . . . ?
C6 C10 C11 C12 -122.6(3) . . . . ?
C6 C10 C11 C16 56.3(3) . . . . ?
C7 N1 C8 C9 14.2(4) . . . . ?
C7 C4 C5 N2 108.9(2) . . . . ?
C7 C4 C5 C6 -9.51(19) . . . . ?
C7 C4 C20 O3 103.6(3) . . . . ?
C7 C4 C20 O4 -74.4(3) . . . . ?
C7 C6 C10 C9 29.8(3) . . . . ?
C7 C6 C10 C11 -93.2(3) . . . . ?
C7 C6 C17 O1 -167.8(2) . . . . ?
C7 C6 C17 O2 10.3(4) . . . . ?
C8 N1 C7 C4 94.0(3) . . . . ?
C8 N1 C7 C6 -8.1(4) . . . . ?
C8 C9 C10 C6 -25.7(4) . . . . ?
C8 C9 C10 C11 97.9(3) . . . . ?
C8 C9 C35 O10 -1.7(4) . . . . ?
C8 C9 C35 O11 177.8(3) . . . . ?
C9 C10 C11 C12 114.0(3) . . . . ?
C9 C10 C11 C16 -67.0(3) . . . . ?
C10 C6 C7 N1 -14.7(4) . . . . ?
C10 C6 C7 C4 -132.4(2) . . . . ?
C10 C6 C17 O1 58.8(3) . . . . ?
C10 C6 C17 O2 -123.1(3) . . . . ?
C10 C9 C35 O10 175.5(2) . . . . ?
C10 C9 C35 O11 -5.0(4) . . . . ?
C10 C11 C12 C13 178.5(3) . . . . ?
C10 C11 C16 C15 -178.2(3) . . . . ?
C11 C12 C13 C14 0.4(5) . . . . ?
C12 C11 C16 C15 0.8(5) . . . . ?
C12 C13 C14 C15 -0.7(6) . . . . ?
C13 C14 C15 C16 1.0(6) . . . . ?
C14 C15 C16 C11 -1.1(6) . . . . ?
C16 C11 C12 C13 -0.5(5) . . . . ?
C17 O1 C18 C19 81.8(3) . . . . ?
C17 C6 C7 N1 -143.8(2) . . . . ?
C17 C6 C7 C4 98.6(2) . . . . ?
C17 C6 C10 C9 159.9(2) . . . . ?
C17 C6 C10 C11 36.8(3) . . . . ?
C18 O1 C17 O2 1.6(4) . . . . ?
C18 O1 C17 C6 179.7(2) . . . . ?
C20 O4 C21 C22 84.9(4) . . . . ?
C20 C4 C5 N2 -140.8(2) . . . . ?
C20 C4 C5 C6 100.7(2) . . . . ?
C20 C4 C7 N1 139.4(2) . . . . ?
C20 C4 C7 C6 -103.0(2) . . . . ?
C21 O4 C20 O3 6.6(4) . . . . ?
C21 O4 C20 C4 -175.4(2) . . . . ?
C23 C3 C4 C5 -90.4(3) . . . . ?
C23 C3 C4 C7 164.6(2) . . . . ?
C23 C3 C4 C20 38.6(3) . . . . ?
C23 C24 C25 O5 176.7(3) . . . . ?
C23 C24 C25 C26 -2.4(5) . . . . ?
C24 C23 C28 C27 -1.1(4) . . . . ?
C24 C25 C26 O6 176.7(3) . . . . ?
C24 C25 C26 C27 -1.3(5) . . . . ?
C25 C26 C27 O7 -176.8(3) . . . . ?
C25 C26 C27 C28 3.7(5) . . . . ?
C26 C27 C28 C23 -2.5(4) . . . . ?
C28 C23 C24 C25 3.6(4) . . . . ?
C29 O5 C25 C24 1.3(5) . . . . ?
C29 O5 C25 C26 -179.6(3) . . . . ?
C30 O6 C26 C25 86.3(4) . . . . ?
C30 O6 C26 C27 -95.7(3) . . . . ?
C31 O7 C27 C26 -178.8(3) . . . . ?
C31 O7 C27 C28 0.6(5) . . . . ?
C32 O9 C33 C34 176.7(4) . . . . ?
C32 C2 C3 C4 149.9(2) . . . . ?
C32 C2 C3 C23 -86.1(3) . . . . ?
C33 O9 C32 O8 -1.3(5) . . . . ?
C33 O9 C32 C2 177.3(3) . . . . ?
C35 O10 C36 C37 79.6(4) . . . . ?
C35 C9 C10 C6 157.1(2) . . . . ?
C35 C9 C10 C11 -79.2(3) . . . . ?
C36 O10 C35 O11 -6.0(4) . . . . ?
C36 O10 C35 C9 173.5(3) . . . . ?
C38 N3 C42 C41 -10.6(4) . . . . ?
C38 N3 C42 C43 92.0(3) . . . . ?
C38 C39 C40 C41 -27.6(3) . . . . ?
C38 C39 C40 C60 95.1(3) . . . . ?
C38 C39 C69 O19 -178.5(3) . . . . ?
C38 C39 C69 O20 1.4(4) . . . . ?
C39 C40 C41 C42 29.4(3) . . . . ?
C39 C40 C41 C44 -76.6(3) . . . . ?
C39 C40 C41 C57 157.1(2) . . . . ?
C39 C40 C60 C61 -66.0(3) . . . . ?
C39 C40 C60 C65 118.1(3) . . . . ?
C40 C39 C69 O19 -1.2(4) . . . . ?
C40 C39 C69 O20 178.8(2) . . . . ?
C40 C41 C42 N3 -12.4(3) . . . . ?
C40 C41 C42 C43 -130.9(2) . . . . ?
C40 C41 C44 N4 13.9(3) . . . . ?
C40 C41 C44 C43 130.8(2) . . . . ?
C40 C41 C57 O14 -118.4(3) . . . . ?
C40 C41 C57 O15 61.3(3) . . . . ?
C40 C60 C61 C62 -175.4(3) . . . . ?
C40 C60 C65 C64 177.3(3) . . . . ?
C41 C40 C60 C61 57.0(3) . . . . ?
C41 C40 C60 C65 -118.8(3) . . . . ?
C41 C42 C43 C44 9.34(19) . . . . ?
C41 C42 C43 C47 130.5(2) . . . . ?
C41 C42 C43 C54 -103.2(2) . . . . ?
C42 N3 C38 C39 14.7(4) . . . . ?
C42 C41 C44 N4 -107.6(2) . . . . ?
C42 C41 C44 C43 9.3(2) . . . . ?
C42 C41 C57 O14 13.1(4) . . . . ?
C42 C41 C57 O15 -167.2(2) . . . . ?
C42 C43 C44 N4 107.1(2) . . . . ?
C42 C43 C44 C41 -9.13(19) . . . . ?
C42 C43 C47 C46 -72.0(3) . . . . ?
C42 C43 C47 C48 163.8(2) . . . . ?
C42 C43 C54 O12 -66.7(3) . . . . ?
C42 C43 C54 O13 111.2(3) . . . . ?
C43 C47 C48 C49 66.8(3) . . . . ?
C43 C47 C48 C53 -110.1(3) . . . . ?
C44 N4 C45 C46 19.9(4) . . . . ?
C44 C41 C42 N3 109.3(2) . . . . ?
C44 C41 C42 C43 -9.17(19) . . . . ?
C44 C41 C57 O14 110.7(3) . . . . ?
C44 C41 C57 O15 -69.6(3) . . . . ?
C44 C43 C47 C46 33.7(3) . . . . ?
C44 C43 C47 C48 -90.4(3) . . . . ?
C44 C43 C54 O12 -163.9(2) . . . . ?
C44 C43 C54 O13 14.0(4) . . . . ?
C45 N4 C44 C41 87.8(3) . . . . ?
C45 N4 C44 C43 -13.0(4) . . . . ?
C45 C46 C47 C43 -29.6(3) . . . . ?
C45 C46 C47 C48 93.9(3) . . . . ?
C45 C46 C72 O21 -1.3(4) . . . . ?
C45 C46 C72 O22 178.3(3) . . . . ?
C46 C47 C48 C49 -56.6(4) . . . . ?
C46 C47 C48 C53 126.6(3) . . . . ?
C47 C43 C44 N4 -14.7(3) . . . . ?
C47 C43 C44 C41 -130.9(2) . . . . ?
C47 C43 C54 O12 63.8(3) . . . . ?
C47 C43 C54 O13 -118.3(3) . . . . ?
C47 C46 C72 O21 179.3(2) . . . . ?
C47 C46 C72 O22 -1.1(4) . . . . ?
C47 C48 C49 C50 -176.4(3) . . . . ?
C47 C48 C53 C52 177.1(3) . . . . ?
C48 C49 C50 C51 -0.9(6) . . . . ?
C49 C48 C53 C52 0.1(4) . . . . ?
C49 C50 C51 C52 0.6(6) . . . . ?
C50 C51 C52 C53 0.1(5) . . . . ?
C51 C52 C53 C48 -0.5(5) . . . . ?
C53 C48 C49 C50 0.6(5) . . . . ?
C54 O12 C55 C56 84.5(3) . . . . ?
C54 C43 C44 N4 -143.6(2) . . . . ?
C54 C43 C44 C41 100.2(2) . . . . ?
C54 C43 C47 C46 163.0(2) . . . . ?
C54 C43 C47 C48 38.8(3) . . . . ?
C55 O12 C54 O13 -0.7(4) . . . . ?
C55 O12 C54 C43 177.1(2) . . . . ?
C57 O15 C58 C59 176.9(3) . . . . ?
C57 C41 C42 N3 -140.0(2) . . . . ?
C57 C41 C42 C43 101.6(2) . . . . ?
C57 C41 C44 N4 140.5(2) . . . . ?
C57 C41 C44 C43 -102.5(2) . . . . ?
C58 O15 C57 O14 10.7(4) . . . . ?
C58 O15 C57 C41 -169.0(2) . . . . ?
C60 C40 C41 C42 -93.1(3) . . . . ?
C60 C40 C41 C44 160.9(2) . . . . ?
C60 C40 C41 C57 34.6(3) . . . . ?
C60 C61 C62 O16 175.7(3) . . . . ?
C60 C61 C62 C63 -2.5(4) . . . . ?
C61 C60 C65 C64 1.6(5) . . . . ?
C61 C62 C63 O17 -179.5(3) . . . . ?
C61 C62 C63 C64 2.5(5) . . . . ?
C62 C63 C64 O18 178.9(3) . . . . ?
C62 C63 C64 C65 -0.5(5) . . . . ?
C63 C64 C65 C60 -1.5(5) . . . . ?
C65 C60 C61 C62 0.4(4) . . . . ?
C66 O16 C62 C61 -6.0(4) . . . . ?
C66 O16 C62 C63 172.3(3) . . . . ?
C67 O17 C63 C62 81.3(4) . . . . ?
C67 O17 C63 C64 -100.7(3) . . . . ?
C68 O18 C64 C63 -175.7(4) . . . . ?
C68 O18 C64 C65 3.7(6) . . . . ?
C69 O20 C70 C71 175.1(3) . . . . ?
C69 C39 C40 C41 155.1(2) . . . . ?
C69 C39 C40 C60 -82.3(3) . . . . ?
C70 O20 C69 O19 -0.1(4) . . . . ?
C70 O20 C69 C39 179.9(3) . . . . ?
C72 O21 C73 C74 176.4(4) . . . . ?
C72 O21 C73' C74' 77.8(6) . . . . ?
C72 C46 C47 C43 149.7(2) . . . . ?
C72 C46 C47 C48 -86.8(3) . . . . ?
C73 O21 C72 O22 -2.6(4) . . . . ?
C73 O21 C72 C46 177.0(3) . . . . ?
C73' O21 C72 O22 -2.6(4) . . . . ?
C73' O21 C72 C46 177.0(3) . . . . ?

_shelx_SHELXL_version_number     2014/8
_olex2_submission_special_instructions 'No special instructions were received'
