# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_337MGL17
_database_code_depnum_ccdc_archive 'CCDC 1844998'
_audit_update_record             
;
2018-05-24 deposited with the CCDC.
2019-01-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H164 N20 O18'
_chemical_formula_weight         2174.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   27.0176(6)
_cell_length_b                   36.9735(8)
_cell_length_c                   14.7072(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14691.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9809
_cell_measurement_theta_min      3.62
_cell_measurement_theta_max      68.21

_exptl_crystal_description       Prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.983
_exptl_crystal_F_000             4672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.289
_exptl_crystal_size_min          0.179
_exptl_absorpt_coefficient_mu    0.540
_shelx_estimated_absorpt_T_min   0.842
_shelx_estimated_absorpt_T_max   0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6681
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_process_details   
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  
'Bruker D8 Venture κ-geometry diffractometer 208039-01'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 0.83
_diffrn_reflns_number            27876
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.624
_diffrn_reflns_theta_max         68.386
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.968
_reflns_number_total             6518
_reflns_number_gt                4835
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_max     0.931
_reflns_Friedel_fraction_full    0.933

_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. 
;

_computing_data_collection       'APEX3 v2016.1 (Bruker, 2014)'
_computing_cell_refinement       'APEX3 v2016.1 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.37A  (Bruker, 2014)'
_computing_structure_solution    'SHELXS-2014 (Bruker, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0956P)²+11.8017P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1626 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.15(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6518
_refine_ls_number_parameters     414
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0701
_refine_ls_wR_factor_ref         0.1927
_refine_ls_wR_factor_gt          0.1767
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.122
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001

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 -0.06567(15) 0.21035(10) 0.3676(4) 0.0964(15) Uani 1 1 d . . . . .
O2 O 0.13431(13) 0.00265(9) 0.3005(3) 0.0841(12) Uani 1 1 d . . . . .
O3 O 0.03808(17) 0.21738(10) 0.2528(3) 0.0818(11) Uani 1 1 d . . . . .
O4 O 0.22266(14) 0.06968(10) 0.2183(3) 0.0723(9) Uani 1 1 d . . . . .
N1 N 0.00677(14) 0.18950(10) 0.4191(3) 0.0566(9) Uani 1 1 d . . . . .
C2 C -0.04113(18) 0.18424(13) 0.3930(4) 0.0648(13) Uani 1 1 d . . . . .
C3 C -0.06370(17) 0.14758(13) 0.3991(4) 0.0634(12) Uani 1 1 d . . . . .
C4 C -0.04838(17) 0.11871(12) 0.3456(4) 0.0614(12) Uani 1 1 d . . . . .
H4 H -0.0205 0.1213 0.3090 0.074 Uiso 1 1 calc R U . . .
C5 C -0.07397(16) 0.08607(12) 0.3458(4) 0.0624(12) Uani 1 1 d . . . . .
C6 C -0.1149(2) 0.08277(16) 0.4036(5) 0.0819(16) Uani 1 1 d . . . . .
H6 H -0.1318 0.0609 0.4070 0.098 Uiso 1 1 calc R U . . .
C7 C -0.1301(3) 0.1112(2) 0.4547(6) 0.103(2) Uani 1 1 d . . . . .
H7 H -0.1577 0.1087 0.4921 0.124 Uiso 1 1 calc R U . . .
C8 C -0.1052(2) 0.14397(18) 0.4519(5) 0.094(2) Uani 1 1 d . . . . .
H8 H -0.1166 0.1635 0.4859 0.113 Uiso 1 1 calc R U . . .
N9 N -0.06193(15) 0.05734(12) 0.2896(5) 0.0884(17) Uani 1 1 d D . . . .
H9 H -0.0840 0.0408 0.2820 0.106 Uiso 1 1 calc DR U . . .
C10 C -0.01632(18) 0.05293(12) 0.2438(5) 0.0736(16) Uani 1 1 d . . . . .
C11 C 0.02785(17) 0.04852(13) 0.2923(4) 0.0662(13) Uani 1 1 d . . . . .
H11 H 0.0276 0.0503 0.3554 0.079 Uiso 1 1 calc R U . . .
C12 C 0.07148(18) 0.04162(12) 0.2478(4) 0.0628(12) Uani 1 1 d . . . . .
C13 C 0.0715(2) 0.0388(2) 0.1546(5) 0.0948(19) Uani 1 1 d . . . . .
H13 H 0.1006 0.0331 0.1240 0.114 Uiso 1 1 calc R U . . .
C14 C 0.0286(3) 0.0444(3) 0.1065(6) 0.121(3) Uani 1 1 d . . . . .
H14 H 0.0292 0.0437 0.0433 0.145 Uiso 1 1 calc R U . . .
C15 C -0.0150(3) 0.0509(2) 0.1506(6) 0.100(2) Uani 1 1 d . . . . .
H15 H -0.0439 0.0540 0.1173 0.120 Uiso 1 1 calc R U . . .
C16 C 0.11890(16) 0.03433(11) 0.2950(4) 0.0597(12) Uani 1 1 d . . . . .
N17 N 0.14486(14) 0.06183(10) 0.3308(3) 0.0629(10) Uani 1 1 d . . . . .
C18 C 0.03976(17) 0.16107(12) 0.4501(4) 0.0587(11) Uani 1 1 d . . . . .
H18A H 0.0203 0.1401 0.4671 0.070 Uiso 1 1 calc R U . . .
H18B H 0.0572 0.1693 0.5039 0.070 Uiso 1 1 calc R U . . .
C19 C 0.07710(19) 0.15013(12) 0.3786(4) 0.0670(13) Uani 1 1 d . . . . .
H19A H 0.1021 0.1689 0.3732 0.080 Uiso 1 1 calc R U . . .
H19B H 0.0605 0.1480 0.3203 0.080 Uiso 1 1 calc R U . . .
C20 C 0.10228(19) 0.11415(13) 0.4016(4) 0.0688(13) Uani 1 1 d . . . . .
H20A H 0.1256 0.1178 0.4508 0.083 Uiso 1 1 calc R U . . .
H20B H 0.0776 0.0969 0.4217 0.083 Uiso 1 1 calc R U . . .
C21 C 0.12903(18) 0.09937(12) 0.3197(4) 0.0655(13) Uani 1 1 d . . . . .
H21A H 0.1074 0.1010 0.2672 0.079 Uiso 1 1 calc R U . . .
H21B H 0.1579 0.1143 0.3077 0.079 Uiso 1 1 calc R U . . .
C22 C 0.02582(17) 0.22619(11) 0.4136(3) 0.0569(11) Uani 1 1 d . . . . .
H22A H 0.0566 0.2276 0.4475 0.068 Uiso 1 1 calc R U . . .
H22B H 0.0024 0.2425 0.4422 0.068 Uiso 1 1 calc R U . . .
C23 C 0.03516(16) 0.23889(12) 0.3167(3) 0.0573(11) Uani 1 1 d . . . . .
N24 N 0.04157(16) 0.27426(11) 0.3088(3) 0.0632(10) Uani 1 1 d D . . . .
H24 H 0.036(2) 0.2862(14) 0.360(2) 0.076 Uiso 1 1 d D U . . .
C25 C 0.0490(2) 0.29457(15) 0.2241(4) 0.0748(13) Uani 1 1 d . U . . .
C26 C 0.0121(9) 0.2851(8) 0.152(2) 0.085(5) Uani 0.52(5) 1 d . U P A 1
H26A H 0.0112 0.3039 0.1070 0.127 Uiso 0.52(5) 1 calc R U P A 1
H26B H -0.0201 0.2825 0.1788 0.127 Uiso 0.52(5) 1 calc R U P A 1
H26C H 0.0215 0.2627 0.1234 0.127 Uiso 0.52(5) 1 calc R U P A 1
C27 C 0.1018(8) 0.2895(9) 0.189(2) 0.099(5) Uani 0.52(5) 1 d . U P A 1
H27A H 0.1067 0.3042 0.1360 0.148 Uiso 0.52(5) 1 calc R U P A 1
H27B H 0.1070 0.2646 0.1736 0.148 Uiso 0.52(5) 1 calc R U P A 1
H27C H 0.1249 0.2965 0.2353 0.148 Uiso 0.52(5) 1 calc R U P A 1
C28 C 0.0609(12) 0.3332(6) 0.2575(16) 0.087(5) Uani 0.52(5) 1 d . U P A 1
H28A H 0.0714 0.3478 0.2069 0.131 Uiso 0.52(5) 1 calc R U P A 1
H28B H 0.0869 0.3322 0.3020 0.131 Uiso 0.52(5) 1 calc R U P A 1
H28C H 0.0318 0.3437 0.2842 0.131 Uiso 0.52(5) 1 calc R U P A 1
C26A C -0.0004(12) 0.2936(10) 0.172(3) 0.103(7) Uani 0.48(5) 1 d . U P A 2
H26D H 0.0042 0.3039 0.1123 0.155 Uiso 0.48(5) 1 calc R U P A 2
H26E H -0.0248 0.3074 0.2042 0.155 Uiso 0.48(5) 1 calc R U P A 2
H26F H -0.0113 0.2691 0.1658 0.155 Uiso 0.48(5) 1 calc R U P A 2
C27A C 0.0935(11) 0.2776(8) 0.170(2) 0.097(5) Uani 0.48(5) 1 d . U P A 2
H27D H 0.1112 0.2964 0.1389 0.145 Uiso 0.48(5) 1 calc R U P A 2
H27E H 0.0811 0.2605 0.1264 0.145 Uiso 0.48(5) 1 calc R U P A 2
H27F H 0.1154 0.2655 0.2115 0.145 Uiso 0.48(5) 1 calc R U P A 2
C28A C 0.0410(14) 0.3370(6) 0.246(2) 0.095(6) Uani 0.48(5) 1 d . U P A 2
H28D H 0.0414 0.3505 0.1905 0.143 Uiso 0.48(5) 1 calc R U P A 2
H28E H 0.0672 0.3454 0.2850 0.143 Uiso 0.48(5) 1 calc R U P A 2
H28F H 0.0098 0.3403 0.2761 0.143 Uiso 0.48(5) 1 calc R U P A 2
C29 C 0.19365(18) 0.05590(13) 0.3683(4) 0.0635(12) Uani 1 1 d . . . . .
H29A H 0.1969 0.0308 0.3865 0.076 Uiso 1 1 calc R U . . .
H29B H 0.1980 0.0708 0.4219 0.076 Uiso 1 1 calc R U . . .
C30 C 0.23343(18) 0.06504(11) 0.2989(4) 0.0594(12) Uani 1 1 d . . . . .
N31 N 0.27852(16) 0.06798(12) 0.3322(3) 0.0681(11) Uani 1 1 d D . . . .
H31 H 0.280(2) 0.0625(16) 0.3920(14) 0.082 Uiso 1 1 d D U . . .
C32 C 0.3239(2) 0.07792(16) 0.2800(4) 0.0801(16) Uani 1 1 d . . . . .
C33 C 0.3656(3) 0.0804(3) 0.3489(6) 0.119(3) Uani 1 1 d . . . . .
H33A H 0.3957 0.0870 0.3184 0.178 Uiso 1 1 calc R U . . .
H33B H 0.3698 0.0575 0.3783 0.178 Uiso 1 1 calc R U . . .
H33C H 0.3577 0.0985 0.3935 0.178 Uiso 1 1 calc R U . . .
C34 C 0.3158(4) 0.1143(2) 0.2332(7) 0.127(3) Uani 1 1 d . . . . .
H34A H 0.3452 0.1210 0.2008 0.190 Uiso 1 1 calc R U . . .
H34B H 0.3084 0.1324 0.2781 0.190 Uiso 1 1 calc R U . . .
H34C H 0.2886 0.1124 0.1914 0.190 Uiso 1 1 calc R U . . .
C35 C 0.3353(3) 0.0491(2) 0.2111(7) 0.115(3) Uani 1 1 d . . . . .
H35A H 0.3649 0.0554 0.1789 0.173 Uiso 1 1 calc R U . . .
H35B H 0.3083 0.0472 0.1690 0.173 Uiso 1 1 calc R U . . .
H35C H 0.3399 0.0264 0.2415 0.173 Uiso 1 1 calc R U . . .
O5 O -0.1691(6) 0.2455(6) 0.2860(13) 0.088(8) Uani 0.253(17) 1 d . . P B 1
O5A O -0.1625(8) 0.2154(8) 0.296(2) 0.133(12) Uani 0.247(17) 1 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 C2 1.229(6) . ?
O2 C16 1.246(5) . ?
O3 C23 1.233(6) . ?
O4 C30 1.234(6) . ?
N1 C2 1.364(6) . ?
N1 C18 1.452(6) . ?
N1 C22 1.453(6) . ?
C2 C3 1.489(7) . ?
C3 C8 1.370(8) . ?
C3 C4 1.389(7) . ?
C4 C5 1.391(6) . ?
C4 H4 0.9300 . ?
C5 N9 1.384(7) . ?
C5 C6 1.401(8) . ?
C6 C7 1.356(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.386(9) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
N9 C10 1.414(7) . ?
N9 H9 0.8600 . ?
C10 C15 1.373(10) . ?
C10 C11 1.400(8) . ?
C11 C12 1.373(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.374(9) . ?
C12 C16 1.482(7) . ?
C13 C14 1.373(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.366(11) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 N17 1.342(6) . ?
N17 C29 1.446(6) . ?
N17 C21 1.461(6) . ?
C18 C19 1.513(7) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.532(6) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.508(8) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.523(7) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 N24 1.324(6) . ?
N24 C25 1.468(7) . ?
N24 H24 0.890(14) . ?
C25 C26 1.50(2) . ?
C25 C27 1.53(2) . ?
C25 C26A 1.54(3) . ?
C25 C28 1.55(2) . ?
C25 C27A 1.57(3) . ?
C25 C28A 1.62(2) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C26A H26D 0.9600 . ?
C26A H26E 0.9600 . ?
C26A H26F 0.9600 . ?
C27A H27D 0.9600 . ?
C27A H27E 0.9600 . ?
C27A H27F 0.9600 . ?
C28A H28D 0.9600 . ?
C28A H28E 0.9600 . ?
C28A H28F 0.9600 . ?
C29 C30 1.520(7) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 N31 1.317(7) . ?
N31 C32 1.492(7) . ?
N31 H31 0.902(14) . ?
C32 C35 1.502(10) . ?
C32 C33 1.519(10) . ?
C32 C34 1.526(10) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C18 124.6(4) . . ?
C2 N1 C22 117.0(4) . . ?
C18 N1 C22 118.4(4) . . ?
O1 C2 N1 119.0(4) . . ?
O1 C2 C3 120.8(4) . . ?
N1 C2 C3 120.1(4) . . ?
C8 C3 C4 119.4(5) . . ?
C8 C3 C2 117.2(5) . . ?
C4 C3 C2 122.9(5) . . ?
C3 C4 C5 121.1(5) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
N9 C5 C4 123.2(5) . . ?
N9 C5 C6 118.7(4) . . ?
C4 C5 C6 118.0(5) . . ?
C7 C6 C5 120.5(5) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C6 C7 C8 121.0(6) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C3 C8 C7 120.0(6) . . ?
C3 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C5 N9 C10 125.3(4) . . ?
C5 N9 H9 117.4 . . ?
C10 N9 H9 117.4 . . ?
C15 C10 C11 118.7(6) . . ?
C15 C10 N9 120.3(6) . . ?
C11 C10 N9 120.9(6) . . ?
C12 C11 C10 120.7(6) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 119.4(6) . . ?
C11 C12 C16 123.5(5) . . ?
C13 C12 C16 117.0(5) . . ?
C14 C13 C12 120.1(7) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C15 C14 C13 120.6(8) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C10 120.4(7) . . ?
C14 C15 H15 119.8 . . ?
C10 C15 H15 119.8 . . ?
O2 C16 N17 120.8(5) . . ?
O2 C16 C12 119.3(4) . . ?
N17 C16 C12 119.8(4) . . ?
C16 N17 C29 120.7(4) . . ?
C16 N17 C21 121.5(4) . . ?
C29 N17 C21 117.0(4) . . ?
N1 C18 C19 112.6(4) . . ?
N1 C18 H18A 109.1 . . ?
C19 C18 H18A 109.1 . . ?
N1 C18 H18B 109.1 . . ?
C19 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
C18 C19 C20 112.0(4) . . ?
C18 C19 H19A 109.2 . . ?
C20 C19 H19A 109.2 . . ?
C18 C19 H19B 109.2 . . ?
C20 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C21 C20 C19 110.5(5) . . ?
C21 C20 H20A 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
N17 C21 C20 113.3(4) . . ?
N17 C21 H21A 108.9 . . ?
C20 C21 H21A 108.9 . . ?
N17 C21 H21B 108.9 . . ?
C20 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
N1 C22 C23 113.5(4) . . ?
N1 C22 H22A 108.9 . . ?
C23 C22 H22A 108.9 . . ?
N1 C22 H22B 108.9 . . ?
C23 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
O3 C23 N24 124.2(5) . . ?
O3 C23 C22 121.6(4) . . ?
N24 C23 C22 114.1(4) . . ?
C23 N24 C25 126.7(4) . . ?
C23 N24 H24 113(4) . . ?
C25 N24 H24 119(4) . . ?
N24 C25 C26 113.0(13) . . ?
N24 C25 C27 110.6(12) . . ?
C26 C25 C27 110.7(13) . . ?
N24 C25 C26A 107.1(16) . . ?
N24 C25 C28 103.4(10) . . ?
C26 C25 C28 125.4(19) . . ?
C27 C25 C28 92(2) . . ?
N24 C25 C27A 109.3(12) . . ?
C26A C25 C27A 113.6(15) . . ?
N24 C25 C28A 107.9(12) . . ?
C26A C25 C28A 90(2) . . ?
C27A C25 C28A 126(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 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C26A H26D 109.5 . . ?
C25 C26A H26E 109.5 . . ?
H26D C26A H26E 109.5 . . ?
C25 C26A H26F 109.5 . . ?
H26D C26A H26F 109.5 . . ?
H26E C26A H26F 109.5 . . ?
C25 C27A H27D 109.5 . . ?
C25 C27A H27E 109.5 . . ?
H27D C27A H27E 109.5 . . ?
C25 C27A H27F 109.5 . . ?
H27D C27A H27F 109.5 . . ?
H27E C27A H27F 109.5 . . ?
C25 C28A H28D 109.5 . . ?
C25 C28A H28E 109.5 . . ?
H28D C28A H28E 109.5 . . ?
C25 C28A H28F 109.5 . . ?
H28D C28A H28F 109.5 . . ?
H28E C28A H28F 109.5 . . ?
N17 C29 C30 110.8(4) . . ?
N17 C29 H29A 109.5 . . ?
C30 C29 H29A 109.5 . . ?
N17 C29 H29B 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 108.1 . . ?
O4 C30 N31 124.3(5) . . ?
O4 C30 C29 120.6(5) . . ?
N31 C30 C29 115.0(5) . . ?
C30 N31 C32 126.0(5) . . ?
C30 N31 H31 112(4) . . ?
C32 N31 H31 122(4) . . ?
N31 C32 C35 110.0(5) . . ?
N31 C32 C33 106.4(5) . . ?
C35 C32 C33 109.9(7) . . ?
N31 C32 C34 109.4(6) . . ?
C35 C32 C34 110.5(7) . . ?
C33 C32 C34 110.7(6) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

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
N9 H9 O2 0.86 2.12 2.961(5) 164.6 2
N24 H24 O4 0.890(14) 2.027(18) 2.910(6) 172(6) 4
N31 H31 O3 0.902(14) 1.98(3) 2.841(6) 158(5) 3

_refine_diff_density_max         0.430
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.050



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol'
_chemical_properties_physical    Heat-sensitive
