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

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

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1031666'
_audit_update_record             
;
2014-10-30 deposited with the CCDC.
2015-03-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H92 N2 O4'
_chemical_formula_weight         1001.44

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           triclinic
_symmetry_space_group_name_H-M   p1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   8.2621(17)
_cell_length_b                   8.9309(18)
_cell_length_c                   21.084(4)
_cell_angle_alpha                81.69(3)
_cell_angle_beta                 85.17(3)
_cell_angle_gamma                82.15(3)
_cell_volume                     1521.7(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7590
_cell_measurement_theta_min      6.13
_cell_measurement_theta_max      54.90

_exptl_crystal_description       rod-like
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             546
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14465
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         27.46
_reflns_number_total             11016
_reflns_number_gt                5706
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0873P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2(2)
_refine_ls_number_reflns         11016
_refine_ls_number_parameters     671
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1278
_refine_ls_R_factor_gt           0.0591
_refine_ls_wR_factor_ref         0.1698
_refine_ls_wR_factor_gt          0.1381
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_restrained_S_all      0.964
_refine_ls_shift/su_max          0.629
_refine_ls_shift/su_mean         0.102

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
C1 C 0.2438(17) -1.2116(15) -0.1641(6) 0.158(5) Uani 1 1 d . . .
H1A H 0.1370 -1.2290 -0.1452 0.238 Uiso 1 1 calc R . .
H1B H 0.3011 -1.3051 -0.1763 0.238 Uiso 1 1 calc R . .
H1C H 0.2330 -1.1363 -0.2014 0.238 Uiso 1 1 calc R . .
C2 C 0.3346(14) -1.1578(12) -0.1180(5) 0.110(3) Uani 1 1 d . . .
H2A H 0.4476 -1.1582 -0.1347 0.132 Uiso 1 1 calc R . .
H2B H 0.3333 -1.2291 -0.0787 0.132 Uiso 1 1 calc R . .
C3 C 0.2731(12) -1.0050(9) -0.1023(4) 0.087(3) Uani 1 1 d . . .
H3A H 0.1595 -1.0044 -0.0862 0.104 Uiso 1 1 calc R . .
H3B H 0.2756 -0.9337 -0.1416 0.104 Uiso 1 1 calc R . .
C4 C 0.3666(9) -0.9473(9) -0.0529(4) 0.073(2) Uani 1 1 d . . .
H4A H 0.3628 -1.0182 -0.0135 0.087 Uiso 1 1 calc R . .
H4B H 0.4804 -0.9496 -0.0687 0.087 Uiso 1 1 calc R . .
C5 C 0.3086(11) -0.7960(10) -0.0375(4) 0.082(3) Uani 1 1 d . . .
H5A H 0.1951 -0.7938 -0.0212 0.098 Uiso 1 1 calc R . .
H5B H 0.3117 -0.7250 -0.0769 0.098 Uiso 1 1 calc R . .
C6 C 0.4035(9) -0.7402(8) 0.0111(3) 0.067(2) Uani 1 1 d . . .
H6A H 0.5174 -0.7455 -0.0049 0.081 Uiso 1 1 calc R . .
H6B H 0.3985 -0.8107 0.0506 0.081 Uiso 1 1 calc R . .
C7 C 0.3481(12) -0.5792(9) 0.0275(4) 0.078(2) Uani 1 1 d . . .
H7A H 0.3534 -0.5087 -0.0119 0.093 Uiso 1 1 calc R . .
H7B H 0.2341 -0.5739 0.0434 0.093 Uiso 1 1 calc R . .
C8 C 0.4406(10) -0.5255(8) 0.0750(3) 0.072(2) Uani 1 1 d . . .
H8A H 0.5540 -0.5281 0.0586 0.086 Uiso 1 1 calc R . .
H8B H 0.4377 -0.5974 0.1141 0.086 Uiso 1 1 calc R . .
C9 C 0.3814(11) -0.3654(8) 0.0925(4) 0.067(2) Uani 1 1 d . . .
H9A H 0.3775 -0.2929 0.0535 0.080 Uiso 1 1 calc R . .
H9B H 0.2711 -0.3636 0.1124 0.080 Uiso 1 1 calc R . .
C10 C 0.4920(9) -0.3159(8) 0.1381(3) 0.061(2) Uani 1 1 d . . .
H10A H 0.5049 -0.3928 0.1755 0.073 Uiso 1 1 calc R . .
H10B H 0.5993 -0.3063 0.1167 0.073 Uiso 1 1 calc R . .
C11 C 0.4179(10) -0.1635(8) 0.1594(3) 0.061(2) Uani 1 1 d . . .
H11A H 0.3091 -0.1725 0.1796 0.073 Uiso 1 1 calc R . .
H11B H 0.4080 -0.0862 0.1221 0.073 Uiso 1 1 calc R . .
C12 C 0.5265(8) -0.1141(7) 0.2076(3) 0.0490(16) Uani 1 1 d . . .
H12A H 0.5384 -0.1934 0.2441 0.059 Uiso 1 1 calc R . .
H12B H 0.6346 -0.1042 0.1869 0.059 Uiso 1 1 calc R . .
C13 C 0.4580(10) 0.0327(8) 0.2309(3) 0.070(2) Uani 1 1 d . . .
H13A H 0.3446 0.0288 0.2465 0.083 Uiso 1 1 calc R . .
H13B H 0.4615 0.1155 0.1958 0.083 Uiso 1 1 calc R . .
C14 C 0.5588(7) 0.0632(6) 0.2863(3) 0.0454(14) Uani 1 1 d . . .
H14A H 0.5683 -0.0264 0.3184 0.055 Uiso 1 1 calc R . .
H14B H 0.6683 0.0805 0.2691 0.055 Uiso 1 1 calc R . .
C15 C 0.4784(10) 0.2023(9) 0.3183(3) 0.077(2) Uani 1 1 d . . .
H15A H 0.3621 0.1962 0.3267 0.092 Uiso 1 1 calc R . .
H15B H 0.5253 0.2002 0.3591 0.092 Uiso 1 1 calc R . .
C16 C 0.5021(8) 0.3457(7) 0.2779(3) 0.0616(19) Uani 1 1 d . . .
H16A H 0.4638 0.3452 0.2357 0.074 Uiso 1 1 calc R . .
H16B H 0.6177 0.3573 0.2728 0.074 Uiso 1 1 calc R . .
C17 C 0.2516(8) 0.5463(7) 0.2914(3) 0.0463(16) Uani 1 1 d . . .
C18 C 0.1406(10) 0.5090(8) 0.2501(3) 0.061(2) Uani 1 1 d . . .
H18 H 0.1679 0.4250 0.2281 0.074 Uiso 1 1 calc R . .
C19 C -0.0038(10) 0.5959(8) 0.2432(4) 0.063(2) Uani 1 1 d . . .
H19 H -0.0782 0.5704 0.2170 0.076 Uiso 1 1 calc R . .
C20 C -0.0453(9) 0.7286(8) 0.2758(4) 0.072(2) Uani 1 1 d . . .
H20 H -0.1452 0.7891 0.2698 0.087 Uiso 1 1 calc R . .
C21 C 0.0581(8) 0.7652(8) 0.3143(3) 0.0557(19) Uani 1 1 d . . .
H21 H 0.0294 0.8500 0.3357 0.067 Uiso 1 1 calc R . .
C22 C 0.2110(7) 0.6760(6) 0.3230(3) 0.0387(14) Uani 1 1 d . . .
C23 C 0.3452(7) 0.6811(6) 0.3600(3) 0.0384(14) Uani 1 1 d . . .
C24 C 0.3793(7) 0.7852(6) 0.4017(3) 0.0371(14) Uani 1 1 d . . .
H24 H 0.3022 0.8665 0.4109 0.045 Uiso 1 1 calc R . .
C25 C 0.5293(7) 0.7606(7) 0.4274(3) 0.0398(15) Uani 1 1 d . . .
C26 C 0.6433(8) 0.6329(7) 0.4177(3) 0.0518(17) Uani 1 1 d . . .
H26 H 0.7401 0.6163 0.4387 0.062 Uiso 1 1 calc R . .
C27 C 0.6148(8) 0.5338(7) 0.3785(4) 0.0528(18) Uani 1 1 d . . .
H27 H 0.6931 0.4521 0.3707 0.063 Uiso 1 1 calc R . .
C28 C 0.4630(8) 0.5566(6) 0.3493(3) 0.0428(16) Uani 1 1 d . . .
C29 C 0.5713(7) 0.8778(6) 0.4669(3) 0.0357(14) Uani 1 1 d . . .
C30 C 0.7180(7) 0.9431(6) 0.4480(3) 0.0382(14) Uani 1 1 d . . .
H30 H 0.7886 0.9022 0.4164 0.046 Uiso 1 1 calc R . .
C31 C 0.7614(7) 1.0634(6) 0.4739(3) 0.0395(14) Uani 1 1 d . . .
C32 C 0.6621(7) 1.1207(6) 0.5253(3) 0.0373(14) Uani 1 1 d . . .
C33 C 0.5197(8) 1.0587(7) 0.5439(3) 0.0409(15) Uani 1 1 d . . .
H33 H 0.4517 1.0975 0.5767 0.049 Uiso 1 1 calc R . .
C34 C 0.4718(7) 0.9402(6) 0.5162(3) 0.0355(13) Uani 1 1 d . . .
C35 C 0.3195(7) 0.8773(7) 0.5470(3) 0.0398(14) Uani 1 1 d . . .
C36 C 0.9150(7) 1.1212(7) 0.4443(3) 0.0456(16) Uani 1 1 d . . .
C37 C 1.0547(8) 1.3396(7) 0.4171(3) 0.0509(18) Uani 1 1 d . . .
H37A H 1.0246 1.4481 0.4047 0.061 Uiso 1 1 calc R . .
H37B H 1.0943 1.2946 0.3786 0.061 Uiso 1 1 calc R . .
C38 C 1.1877(10) 1.3165(9) 0.4619(4) 0.076(2) Uani 1 1 d . . .
H38A H 1.1464 1.3529 0.5015 0.113 Uiso 1 1 calc R . .
H38B H 1.2756 1.3717 0.4430 0.113 Uiso 1 1 calc R . .
H38C H 1.2273 1.2098 0.4701 0.113 Uiso 1 1 calc R . .
C39 C 0.1791(9) 0.6594(8) 0.5732(4) 0.066(2) Uani 1 1 d . . .
H39A H 0.1359 0.7015 0.6120 0.079 Uiso 1 1 calc R . .
H39B H 0.2099 0.5506 0.5845 0.079 Uiso 1 1 calc R . .
C40 C 0.0494(8) 0.6859(9) 0.5255(4) 0.080(2) Uani 1 1 d . . .
H40A H 0.0108 0.7929 0.5177 0.120 Uiso 1 1 calc R . .
H40B H -0.0401 0.6307 0.5424 0.120 Uiso 1 1 calc R . .
H40C H 0.0947 0.6511 0.4860 0.120 Uiso 1 1 calc R . .
C41 C 0.7076(7) 1.2344(6) 0.5610(3) 0.0358(14) Uani 1 1 d . . .
C42 C 0.8542(7) 1.2153(6) 0.5922(3) 0.0372(14) Uani 1 1 d . . .
H42 H 0.9313 1.1314 0.5864 0.045 Uiso 1 1 calc R . .
C43 C 0.8861(7) 1.3142(6) 0.6300(3) 0.0362(13) Uani 1 1 d . . .
C44 C 0.7678(8) 1.4381(7) 0.6419(3) 0.0446(16) Uani 1 1 d . . .
C45 C 0.6250(9) 1.4659(8) 0.6130(4) 0.059(2) Uani 1 1 d . . .
H45 H 0.5498 1.5511 0.6188 0.070 Uiso 1 1 calc R . .
C46 C 0.5959(7) 1.3602(7) 0.5737(3) 0.0502(17) Uani 1 1 d . . .
H46 H 0.4961 1.3747 0.5549 0.060 Uiso 1 1 calc R . .
C47 C 1.0234(7) 1.3228(6) 0.6683(3) 0.0416(15) Uani 1 1 d . . .
C48 C 1.1691(8) 1.2341(8) 0.6774(3) 0.0521(17) Uani 1 1 d . . .
H48 H 1.1972 1.1467 0.6576 0.063 Uiso 1 1 calc R . .
C49 C 1.2765(8) 1.2790(9) 0.7179(4) 0.067(2) Uani 1 1 d . . .
H49 H 1.3786 1.2221 0.7233 0.080 Uiso 1 1 calc R . .
C50 C 1.2356(10) 1.3996(11) 0.7483(4) 0.075(2) Uani 1 1 d . . .
H50 H 1.3092 1.4232 0.7752 0.090 Uiso 1 1 calc R . .
C51 C 1.0848(9) 1.4941(8) 0.7414(3) 0.0578(19) Uani 1 1 d . . .
H51 H 1.0567 1.5790 0.7628 0.069 Uiso 1 1 calc R . .
C52 C 0.9829(8) 1.4519(7) 0.7011(3) 0.0468(16) Uani 1 1 d . . .
C53 C 0.7391(9) 1.6516(6) 0.7118(3) 0.067(2) Uani 1 1 d . . .
H53A H 0.7797 1.6563 0.7532 0.081 Uiso 1 1 calc R . .
H53B H 0.6251 1.6347 0.7193 0.081 Uiso 1 1 calc R . .
C54 C 0.7462(9) 1.8023(6) 0.6721(3) 0.0589(19) Uani 1 1 d . . .
H54A H 0.6913 1.8059 0.6329 0.071 Uiso 1 1 calc R . .
H54B H 0.8593 1.8180 0.6605 0.071 Uiso 1 1 calc R . .
C55 C 0.6597(10) 1.9313(7) 0.7116(4) 0.080(2) Uani 1 1 d . . .
H55A H 0.6220 2.0204 0.6820 0.096 Uiso 1 1 calc R . .
H55B H 0.5646 1.8958 0.7363 0.096 Uiso 1 1 calc R . .
C56 C 0.7693(9) 1.9756(7) 0.7558(3) 0.0578(18) Uani 1 1 d . . .
H56A H 0.8726 1.9927 0.7323 0.069 Uiso 1 1 calc R . .
H56B H 0.7915 1.8911 0.7896 0.069 Uiso 1 1 calc R . .
C57 C 0.7016(10) 2.1203(8) 0.7873(4) 0.064(2) Uani 1 1 d . . .
H57A H 0.6837 2.2054 0.7533 0.077 Uiso 1 1 calc R . .
H57B H 0.5957 2.1047 0.8089 0.077 Uiso 1 1 calc R . .
C58 C 0.8041(9) 2.1639(8) 0.8336(4) 0.0606(19) Uani 1 1 d . . .
H58A H 0.9144 2.1664 0.8140 0.073 Uiso 1 1 calc R . .
H58B H 0.8093 2.0857 0.8706 0.073 Uiso 1 1 calc R . .
C59 C 0.7455(9) 2.3166(8) 0.8564(3) 0.060(2) Uani 1 1 d . . .
H59A H 0.7367 2.3928 0.8187 0.072 Uiso 1 1 calc R . .
H59B H 0.6357 2.3118 0.8763 0.072 Uiso 1 1 calc R . .
C60 C 0.8425(10) 2.3736(8) 0.9022(4) 0.068(2) Uani 1 1 d . . .
H60A H 0.9550 2.3708 0.8846 0.081 Uiso 1 1 calc R . .
H60B H 0.8421 2.3040 0.9421 0.081 Uiso 1 1 calc R . .
C61 C 0.7841(10) 2.5314(8) 0.9173(4) 0.068(2) Uani 1 1 d . . .
H61A H 0.6710 2.5353 0.9344 0.081 Uiso 1 1 calc R . .
H61B H 0.7870 2.6019 0.8778 0.081 Uiso 1 1 calc R . .
C62 C 0.8861(11) 2.5846(9) 0.9661(4) 0.067(2) Uani 1 1 d . . .
H62A H 0.8810 2.5160 1.0061 0.081 Uiso 1 1 calc R . .
H62B H 0.9996 2.5791 0.9496 0.081 Uiso 1 1 calc R . .
C63 C 0.8272(10) 2.7432(8) 0.9789(4) 0.074(2) Uani 1 1 d . . .
H63A H 0.7123 2.7499 0.9935 0.089 Uiso 1 1 calc R . .
H63B H 0.8372 2.8125 0.9393 0.089 Uiso 1 1 calc R . .
C64 C 0.9217(9) 2.7924(9) 1.0288(4) 0.065(2) Uani 1 1 d . . .
H64A H 1.0363 2.7878 1.0137 0.078 Uiso 1 1 calc R . .
H64B H 0.9140 2.7214 1.0680 0.078 Uiso 1 1 calc R . .
C65 C 0.8587(11) 2.9572(8) 1.0440(4) 0.081(3) Uani 1 1 d . . .
H65A H 0.8650 3.0281 1.0047 0.098 Uiso 1 1 calc R . .
H65B H 0.7446 2.9615 1.0597 0.098 Uiso 1 1 calc R . .
C66 C 0.9550(11) 3.0064(9) 1.0932(4) 0.078(2) Uani 1 1 d . . .
H66A H 1.0678 3.0084 1.0764 0.094 Uiso 1 1 calc R . .
H66B H 0.9541 2.9325 1.1317 0.094 Uiso 1 1 calc R . .
C67 C 0.8845(14) 3.1655(10) 1.1106(5) 0.103(3) Uani 1 1 d . . .
H67A H 0.7715 3.1636 1.1270 0.123 Uiso 1 1 calc R . .
H67B H 0.8860 3.2394 1.0720 0.123 Uiso 1 1 calc R . .
C68 C 0.9850(13) 3.2179(16) 1.1627(7) 0.146(5) Uani 1 1 d . . .
H68A H 0.9720 3.1528 1.2028 0.219 Uiso 1 1 calc R . .
H68B H 0.9449 3.3214 1.1686 0.219 Uiso 1 1 calc R . .
H68C H 1.0989 3.2110 1.1484 0.219 Uiso 1 1 calc R . .
N1 N 0.4099(7) 0.4752(6) 0.3079(3) 0.0514(14) Uani 1 1 d . . .
N2 N 0.8301(7) 1.5196(5) 0.6857(3) 0.0511(14) Uani 1 1 d . . .
O1 O 0.2048(6) 0.9564(5) 0.5710(2) 0.0643(13) Uani 1 1 d . . .
O2 O 0.3237(5) 0.7306(5) 0.5466(2) 0.0483(11) Uani 1 1 d . . .
O3 O 1.0237(6) 1.0467(6) 0.4186(3) 0.0721(16) Uani 1 1 d . . .
O4 O 0.9112(5) 1.2720(4) 0.4457(2) 0.0508(11) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.447(13) . ?
C2 C3 1.463(11) . ?
C3 C4 1.532(10) . ?
C4 C5 1.443(10) . ?
C5 C6 1.518(10) . ?
C6 C7 1.528(10) . ?
C7 C8 1.478(10) . ?
C8 C9 1.533(8) . ?
C9 C10 1.529(10) . ?
C10 C11 1.526(8) . ?
C11 C12 1.557(9) . ?
C12 C13 1.490(8) . ?
C13 C14 1.564(9) . ?
C14 C15 1.543(8) . ?
C15 C16 1.460(10) . ?
C16 N1 1.485(7) . ?
C17 C22 1.405(7) . ?
C17 C18 1.419(9) . ?
C17 N1 1.421(8) . ?
C18 C19 1.339(10) . ?
C19 C20 1.443(8) . ?
C20 C21 1.329(10) . ?
C21 C22 1.409(8) . ?
C22 C23 1.418(8) . ?
C23 C28 1.405(7) . ?
C23 C24 1.436(7) . ?
C24 C25 1.373(8) . ?
C25 C26 1.404(7) . ?
C25 C29 1.519(7) . ?
C26 C27 1.352(9) . ?
C27 C28 1.420(9) . ?
C28 N1 1.348(8) . ?
C29 C34 1.403(7) . ?
C29 C30 1.418(8) . ?
C30 C31 1.375(8) . ?
C31 C32 1.415(7) . ?
C31 C36 1.489(9) . ?
C32 C33 1.372(8) . ?
C32 C41 1.452(8) . ?
C33 C34 1.396(8) . ?
C34 C35 1.507(9) . ?
C35 O1 1.221(6) . ?
C35 O2 1.308(7) . ?
C36 O3 1.185(6) . ?
C36 O4 1.348(7) . ?
C37 O4 1.451(8) . ?
C37 C38 1.483(11) . ?
C39 O2 1.462(8) . ?
C39 C40 1.502(11) . ?
C41 C46 1.396(7) . ?
C41 C42 1.406(8) . ?
C42 C43 1.336(7) . ?
C43 C44 1.410(7) . ?
C43 C47 1.464(8) . ?
C44 C45 1.350(10) . ?
C44 N2 1.422(8) . ?
C45 C46 1.398(8) . ?
C47 C48 1.359(9) . ?
C47 C52 1.417(8) . ?
C48 C49 1.414(9) . ?
C49 C50 1.322(10) . ?
C50 C51 1.412(10) . ?
C51 C52 1.369(9) . ?
C52 N2 1.368(8) . ?
C53 N2 1.461(6) . ?
C53 C54 1.485(9) . ?
C54 C55 1.577(7) . ?
C55 C56 1.480(10) . ?
C56 C57 1.552(8) . ?
C57 C58 1.470(10) . ?
C58 C59 1.516(8) . ?
C59 C60 1.489(9) . ?
C60 C61 1.496(9) . ?
C61 C62 1.546(10) . ?
C62 C63 1.489(9) . ?
C63 C64 1.507(9) . ?
C64 C65 1.562(9) . ?
C65 C66 1.505(11) . ?
C66 C67 1.544(11) . ?
C67 C68 1.590(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C2 C3 115.0(10) . . ?
C2 C3 C4 115.6(8) . . ?
C5 C4 C3 116.3(7) . . ?
C4 C5 C6 115.6(7) . . ?
C5 C6 C7 117.1(7) . . ?
C8 C7 C6 116.9(7) . . ?
C7 C8 C9 116.5(7) . . ?
C10 C9 C8 112.6(6) . . ?
C11 C10 C9 110.3(6) . . ?
C10 C11 C12 110.9(6) . . ?
C13 C12 C11 113.1(6) . . ?
C12 C13 C14 110.3(6) . . ?
C15 C14 C13 112.1(5) . . ?
C16 C15 C14 111.7(5) . . ?
C15 C16 N1 109.7(5) . . ?
C22 C17 C18 119.8(5) . . ?
C22 C17 N1 108.9(5) . . ?
C18 C17 N1 131.2(5) . . ?
C19 C18 C17 119.3(6) . . ?
C18 C19 C20 120.7(7) . . ?
C21 C20 C19 120.6(6) . . ?
C20 C21 C22 120.3(6) . . ?
C17 C22 C21 119.3(6) . . ?
C17 C22 C23 106.0(5) . . ?
C21 C22 C23 134.7(5) . . ?
C28 C23 C22 107.7(5) . . ?
C28 C23 C24 119.1(6) . . ?
C22 C23 C24 133.2(5) . . ?
C25 C24 C23 117.8(5) . . ?
C24 C25 C26 122.1(5) . . ?
C24 C25 C29 117.9(5) . . ?
C26 C25 C29 119.9(5) . . ?
C27 C26 C25 121.1(6) . . ?
C26 C27 C28 118.8(5) . . ?
N1 C28 C23 110.1(6) . . ?
N1 C28 C27 129.0(6) . . ?
C23 C28 C27 120.9(5) . . ?
C34 C29 C30 115.9(5) . . ?
C34 C29 C25 126.6(5) . . ?
C30 C29 C25 117.2(5) . . ?
C31 C30 C29 123.6(5) . . ?
C30 C31 C32 119.4(6) . . ?
C30 C31 C36 115.0(5) . . ?
C32 C31 C36 125.6(5) . . ?
C33 C32 C31 117.5(5) . . ?
C33 C32 C41 118.9(5) . . ?
C31 C32 C41 123.5(5) . . ?
C32 C33 C34 123.4(5) . . ?
C33 C34 C29 120.2(6) . . ?
C33 C34 C35 115.7(5) . . ?
C29 C34 C35 123.8(5) . . ?
O1 C35 O2 123.7(6) . . ?
O1 C35 C34 122.7(6) . . ?
O2 C35 C34 113.6(5) . . ?
O3 C36 O4 123.3(6) . . ?
O3 C36 C31 124.4(6) . . ?
O4 C36 C31 112.1(5) . . ?
O4 C37 C38 112.0(5) . . ?
O2 C39 C40 110.9(6) . . ?
C46 C41 C42 115.6(5) . . ?
C46 C41 C32 120.8(5) . . ?
C42 C41 C32 123.0(5) . . ?
C43 C42 C41 121.9(5) . . ?
C42 C43 C44 120.0(6) . . ?
C42 C43 C47 133.9(5) . . ?
C44 C43 C47 106.0(5) . . ?
C45 C44 C43 121.7(6) . . ?
C45 C44 N2 130.2(6) . . ?
C43 C44 N2 108.1(5) . . ?
C44 C45 C46 116.6(6) . . ?
C41 C46 C45 124.0(6) . . ?
C48 C47 C52 119.2(6) . . ?
C48 C47 C43 133.1(5) . . ?
C52 C47 C43 107.7(5) . . ?
C47 C48 C49 117.9(6) . . ?
C50 C49 C48 121.7(7) . . ?
C49 C50 C51 122.7(7) . . ?
C52 C51 C50 115.2(6) . . ?
C51 C52 N2 128.5(6) . . ?
C51 C52 C47 123.2(6) . . ?
N2 C52 C47 108.3(6) . . ?
N2 C53 C54 116.6(6) . . ?
C53 C54 C55 109.1(5) . . ?
C56 C55 C54 112.7(6) . . ?
C55 C56 C57 115.0(6) . . ?
C58 C57 C56 116.5(6) . . ?
C57 C58 C59 114.9(6) . . ?
C60 C59 C58 119.4(6) . . ?
C59 C60 C61 115.5(6) . . ?
C60 C61 C62 113.8(7) . . ?
C63 C62 C61 112.5(7) . . ?
C62 C63 C64 112.4(7) . . ?
C63 C64 C65 113.1(6) . . ?
C66 C65 C64 112.8(7) . . ?
C65 C66 C67 112.0(8) . . ?
C66 C67 C68 112.3(9) . . ?
C28 N1 C17 107.3(5) . . ?
C28 N1 C16 128.0(5) . . ?
C17 N1 C16 124.3(5) . . ?
C52 N2 C44 109.8(5) . . ?
C52 N2 C53 125.9(5) . . ?
C44 N2 C53 124.2(6) . . ?
C35 O2 C39 117.9(5) . . ?
C36 O4 C37 116.2(5) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.041
####################################################################### 
# 
# 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_boct
_database_code_depnum_ccdc_archive 'CCDC 1031667'
_audit_update_record             
;
2014-10-30 deposited with the CCDC.
2015-03-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H60 N2 O4'
_chemical_formula_weight         777.02

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   21.598(3)
_cell_length_b                   10.1507(6)
_cell_length_c                   22.926(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.388(18)
_cell_angle_gamma                90.00
_cell_volume                     4540.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9753
_cell_measurement_theta_min      3.25
_cell_measurement_theta_max      29.72

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1672
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25547
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0980
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.28
_diffrn_reflns_theta_max         30.02
_reflns_number_total             11529
_reflns_number_gt                3694
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1849P)²+0.0000P] 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     SHELXL
_refine_ls_extinction_coef       0.0053(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         11529
_refine_ls_number_parameters     536
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2474
_refine_ls_R_factor_gt           0.1113
_refine_ls_wR_factor_ref         0.4182
_refine_ls_wR_factor_gt          0.3136
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          4.588
_refine_ls_shift/su_mean         0.042

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
C1 C 0.22908(17) 0.8727(3) 0.20861(18) 0.0616(9) Uani 1 1 d . . .
C2 C 0.21172(16) 0.8656(3) 0.26110(17) 0.0564(9) Uani 1 1 d . . .
C3 C 0.32031(19) 0.5517(3) 0.21763(18) 0.0621(9) Uani 1 1 d . . .
C4 C 0.28471(16) 0.6585(3) 0.23498(17) 0.0556(9) Uani 1 1 d . . .
C5 C 0.23018(16) 0.7539(3) 0.29805(17) 0.0615(9) Uani 1 1 d . . .
H5A H 0.2177 0.7458 0.3320 0.074 Uiso 1 1 calc R . .
C6 C 0.0507(4) 1.1478(6) 0.0831(4) 0.193(4) Uani 1 1 d . . .
H6A H 0.0338 1.2217 0.0545 0.289 Uiso 1 1 calc R . .
H6B H 0.0466 1.1657 0.1224 0.289 Uiso 1 1 calc R . .
H6C H 0.0244 1.0708 0.0629 0.289 Uiso 1 1 calc R . .
C7 C 0.08716(17) 1.0510(3) 0.30646(16) 0.0580(9) Uani 1 1 d . . .
C8 C 0.41067(17) 0.4728(3) 0.19169(17) 0.0582(9) Uani 1 1 d . . .
C9 C 0.26575(17) 0.7704(3) 0.19716(17) 0.0627(10) Uani 1 1 d . . .
H9A H 0.2778 0.7779 0.1629 0.075 Uiso 1 1 calc R . .
C10 C 0.17589(18) 0.9731(3) 0.27803(17) 0.0613(9) Uani 1 1 d . . .
C11 C 0.1189(3) 1.1264(5) 0.0968(3) 0.1195(19) Uani 1 1 d . . .
H11A H 0.1458 1.2038 0.1171 0.143 Uiso 1 1 calc R . .
H11B H 0.1236 1.1087 0.0574 0.143 Uiso 1 1 calc R . .
C12 C 0.37851(17) 0.5755(3) 0.20836(16) 0.0588(9) Uani 1 1 d . . .
H12A H 0.3963 0.6603 0.2133 0.071 Uiso 1 1 calc R . .
C13 C 0.4437(4) 0.3682(6) 0.4088(4) 0.184(3) Uani 1 1 d . . .
H13A H 0.4596 0.2918 0.4358 0.276 Uiso 1 1 calc R . .
H13B H 0.4707 0.4432 0.4307 0.276 Uiso 1 1 calc R . .
H13C H 0.4479 0.3537 0.3693 0.276 Uiso 1 1 calc R . .
C14 C 0.3531(11) -0.4909(19) -0.0199(12) 0.294(11) Uani 1 1 d . . .
H14A H 0.343(8) -0.506(15) -0.065(6) 0.353 Uiso 1 1 calc . A 1
H14B H 0.401(9) -0.52(2) 0.003(11) 0.353 Uiso 1 1 calc . B 1
C15 C 0.02851(18) 1.0595(4) 0.32063(17) 0.0650(10) Uani 1 1 d . . .
C16 C 0.1356(8) 2.0279(10) 0.5212(6) 0.271(9) Uani 1 1 d . . .
H16A H 0.0887 2.0427 0.4900 0.325 Uiso 1 1 calc R . .
H16B H 0.1395 2.0567 0.5630 0.325 Uiso 1 1 calc R . .
C17 C 0.26687(17) 0.6518(3) 0.28694(18) 0.0597(9) Uani 1 1 d . . .
C18 C 0.11948(17) 0.9478(3) 0.28992(17) 0.0581(9) Uani 1 1 d . . .
H18A H 0.1030 0.8622 0.2869 0.070 Uiso 1 1 calc R . .
C19 C 0.2079(2) 0.9819(3) 0.1602(2) 0.0701(11) Uani 1 1 d . . .
C20 C 0.20001(19) 1.1047(3) 0.28308(18) 0.0702(11) Uani 1 1 d . . .
H20A H 0.2373 1.1218 0.2740 0.084 Uiso 1 1 calc R . .
C21 C 0.11318(19) 1.1800(3) 0.31185(18) 0.0670(10) Uani 1 1 d . . .
C22 C 0.1511(6) 1.8793(8) 0.5244(5) 0.214(4) Uani 1 1 d . . .
H22A H 0.1989 1.8667 0.5538 0.257 Uiso 1 1 calc R . .
H22B H 0.1240 1.8358 0.5433 0.257 Uiso 1 1 calc R . .
C23 C 0.2876(2) 0.5410(3) 0.3351(2) 0.0679(10) Uani 1 1 d . . .
C24 C 0.47163(19) 0.4642(4) 0.18064(18) 0.0667(10) Uani 1 1 d . . .
C25 C 0.38369(19) 0.3445(3) 0.18449(16) 0.0629(10) Uani 1 1 d . . .
C26 C 0.1704(2) 1.2077(3) 0.30084(19) 0.0744(11) Uani 1 1 d . . .
H26A H 0.1880 1.2926 0.3053 0.089 Uiso 1 1 calc R . .
C27 C 0.29538(19) 0.4206(3) 0.21092(19) 0.0712(11) Uani 1 1 d . . .
H27A H 0.2573 0.4037 0.2187 0.085 Uiso 1 1 calc R . .
C28 C 0.5202(2) 0.5560(4) 0.1822(2) 0.0791(11) Uani 1 1 d . . .
H28A H 0.5160 0.6445 0.1904 0.095 Uiso 1 1 calc R . .
C29 C 0.3250(2) 0.3177(3) 0.19338(19) 0.0727(11) Uani 1 1 d . . .
H29A H 0.3067 0.2332 0.1876 0.087 Uiso 1 1 calc R . .
C30 C 0.4789(2) 0.3325(4) 0.16769(18) 0.0720(11) Uani 1 1 d . . .
C31 C 0.0204(2) 1.1908(4) 0.33264(18) 0.0729(11) Uani 1 1 d . . .
C32 C -0.0182(2) 0.9666(4) 0.3221(2) 0.0801(11) Uani 1 1 d . . .
H32A H -0.0137 0.8780 0.3143 0.096 Uiso 1 1 calc R . .
C33 C -0.0323(2) 1.2342(5) 0.3468(2) 0.0917(14) Uani 1 1 d . . .
H33A H -0.0366 1.3225 0.3554 0.110 Uiso 1 1 calc R . .
C34 C 0.5332(3) 0.2877(5) 0.1558(2) 0.0947(14) Uani 1 1 d . . .
H34A H 0.5370 0.1997 0.1465 0.114 Uiso 1 1 calc R . .
C35 C 0.4128(2) 0.1190(4) 0.1569(2) 0.0925(14) Uani 1 1 d . . .
H35A H 0.4566 0.0743 0.1776 0.111 Uiso 1 1 calc R . .
H35B H 0.3846 0.0888 0.1777 0.111 Uiso 1 1 calc R . .
C36 C 0.5812(2) 0.3804(5) 0.1585(2) 0.0985(15) Uani 1 1 d . . .
H36A H 0.6187 0.3535 0.1516 0.118 Uiso 1 1 calc R . .
C37 C -0.0716(2) 1.0100(5) 0.3357(2) 0.1006(15) Uani 1 1 d . . .
H37A H -0.1034 0.9493 0.3367 0.121 Uiso 1 1 calc R . .
C38 C 0.5753(2) 0.5119(5) 0.1711(2) 0.1005(15) Uani 1 1 d . . .
H38A H 0.6085 0.5716 0.1722 0.121 Uiso 1 1 calc R . .
C39 C 0.0839(2) 1.4067(4) 0.3391(2) 0.0838(12) Uani 1 1 d . . .
H39A H 0.1114 1.4367 0.3175 0.101 Uiso 1 1 calc R . .
H39B H 0.0396 1.4494 0.3181 0.101 Uiso 1 1 calc R . .
C40 C 0.3804(3) 0.0779(5) 0.0902(3) 0.124(2) Uani 1 1 d . C .
H40A H 0.4070 0.1083 0.0677 0.149 Uiso 1 1 calc R . .
H40B H 0.3348 0.1154 0.0690 0.149 Uiso 1 1 calc R . .
C41 C -0.0786(2) 1.1401(6) 0.3476(2) 0.1037(16) Uani 1 1 d . . .
H41A H -0.1150 1.1659 0.3564 0.124 Uiso 1 1 calc R . .
C42 C 0.1165(3) 1.4521(4) 0.4059(2) 0.0950(14) Uani 1 1 d . . .
H42A H 0.1619 1.4135 0.4271 0.114 Uiso 1 1 calc R . .
H42B H 0.0899 1.4223 0.4283 0.114 Uiso 1 1 calc R . .
C43 C 0.3746(3) 0.3915(5) 0.3948(3) 0.1178(18) Uani 1 1 d . . .
H43A H 0.3698 0.4058 0.4345 0.141 Uiso 1 1 calc R . .
H43B H 0.3469 0.3160 0.3728 0.141 Uiso 1 1 calc R . .
C44 C 0.1226(3) 1.6025(4) 0.4103(3) 0.1102(17) Uani 1 1 d . . .
H44A H 0.1559 1.6290 0.3945 0.132 Uiso 1 1 calc R . .
H44B H 0.0788 1.6393 0.3811 0.132 Uiso 1 1 calc R . .
C45 C 0.3618(4) -0.2903(7) 0.0304(4) 0.159(3) Uani 1 1 d . . .
H45A H 0.4018 -0.3196 0.0681 0.191 Uiso 1 1 calc R C .
H45B H 0.3221 -0.3157 0.0373 0.191 Uiso 1 1 calc R . .
C46 C 0.3762(4) -0.0770(6) 0.0883(4) 0.159(3) Uani 1 1 d . . .
H46A H 0.4191 -0.1107 0.1209 0.190 Uiso 1 1 calc R C .
H46B H 0.3404 -0.1028 0.1008 0.190 Uiso 1 1 calc R . .
C47 C 0.3598(7) -0.3579(8) -0.0171(6) 0.237(5) Uani 1 1 d . C .
H47A H 0.4015 -0.3381 -0.0216 0.285 Uiso 1 1 calc R . .
H47B H 0.3222 -0.3233 -0.0554 0.285 Uiso 1 1 calc R . .
C48 C 0.3638(3) -0.1393(5) 0.0309(3) 0.133(2) Uani 1 1 d . C .
H48A H 0.3988 -0.1119 0.0177 0.159 Uiso 1 1 calc R . .
H48B H 0.3202 -0.1078 -0.0015 0.159 Uiso 1 1 calc R . .
C49 C 0.1424(3) 1.6627(5) 0.4736(3) 0.1266(19) Uani 1 1 d . . .
H49A H 0.1886 1.6351 0.5023 0.152 Uiso 1 1 calc R . .
H49B H 0.1118 1.6322 0.4918 0.152 Uiso 1 1 calc R . .
C50 C 0.1397(4) 1.8178(6) 0.4694(3) 0.142(2) Uani 1 1 d . . .
H50A H 0.1734 1.8475 0.4549 0.170 Uiso 1 1 calc R . .
H50B H 0.0949 1.8438 0.4370 0.170 Uiso 1 1 calc R . .
C51 C 0.3265(18) -0.5808(17) -0.0101(11) 0.33(2) Uani 0.50 1 d P C 1
H51E H 0.3389 -0.6587 -0.0264 0.490 Uiso 0.50 1 calc PR C 1
H51D H 0.2777 -0.5692 -0.0314 0.490 Uiso 0.50 1 calc PR C 1
H51F H 0.3408 -0.5898 0.0355 0.490 Uiso 0.50 1 calc PR C 1
C51' C 0.3949(18) -0.5660(17) -0.0085(11) 0.268(18) Uani 0.50 1 d PR C 2
H51A H 0.4251 -0.5109 -0.0186 0.401 Uiso 0.50 1 d PR C 2
H51B H 0.3767 -0.6340 -0.0405 0.401 Uiso 0.50 1 d PR C 2
H51C H 0.4197 -0.6053 0.0332 0.401 Uiso 0.50 1 d PR C 2
C52 C 0.1754(9) 2.0976(13) 0.5057(6) 0.292(8) Uani 1 1 d . . .
H52A H 0.1624 2.1886 0.5034 0.438 Uiso 1 1 calc R . .
H52B H 0.1719 2.0696 0.4644 0.438 Uiso 1 1 calc R . .
H52C H 0.2218 2.0871 0.5376 0.438 Uiso 1 1 calc R . .
N1 N 0.07345(17) 1.2649(3) 0.32839(15) 0.0752(9) Uani 1 1 d . . .
N2 N 0.42471(17) 0.2599(3) 0.16933(15) 0.0747(9) Uani 1 1 d . . .
O4 O 0.35210(15) 0.5078(3) 0.35382(14) 0.0877(9) Uani 1 1 d . . .
O3 O 0.24954(16) 0.4921(3) 0.35404(16) 0.0935(10) Uani 1 1 d . . .
O2 O 0.14290(15) 1.0129(3) 0.14065(15) 0.0863(9) Uani 1 1 d . . .
O1 O 0.24573(16) 1.0320(3) 0.14093(16) 0.0965(10) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C9 1.398(4) . ?
C1 C2 1.408(5) . ?
C1 C19 1.495(5) . ?
C2 C5 1.368(4) . ?
C2 C10 1.483(4) . ?
C3 C12 1.383(4) . ?
C3 C27 1.419(4) . ?
C3 C4 1.479(4) . ?
C4 C9 1.380(4) . ?
C4 C17 1.402(4) . ?
C5 C17 1.392(4) . ?
C6 C11 1.384(7) . ?
C7 C18 1.399(4) . ?
C7 C21 1.408(4) . ?
C7 C15 1.439(5) . ?
C8 C12 1.393(4) . ?
C8 C25 1.407(4) . ?
C8 C24 1.446(5) . ?
C10 C18 1.382(4) . ?
C10 C20 1.420(4) . ?
C11 O2 1.469(5) . ?
C13 C43 1.405(7) . ?
C14 C51 1.15(3) . ?
C14 C47 1.357(19) . ?
C15 C31 1.387(5) . ?
C15 C32 1.391(5) . ?
C16 C52 1.276(15) . ?
C16 C22 1.540(12) . ?
C17 C23 1.503(5) . ?
C19 O1 1.197(4) . ?
C19 O2 1.315(4) . ?
C20 C26 1.375(4) . ?
C21 N1 1.379(4) . ?
C21 C26 1.392(5) . ?
C22 C50 1.330(9) . ?
C23 O3 1.192(4) . ?
C23 O4 1.313(4) . ?
C24 C30 1.393(5) . ?
C24 C28 1.393(5) . ?
C25 N2 1.381(4) . ?
C25 C29 1.393(5) . ?
C27 C29 1.373(4) . ?
C28 C38 1.393(5) . ?
C30 C34 1.390(5) . ?
C30 N2 1.396(5) . ?
C31 C33 1.382(5) . ?
C31 N1 1.409(5) . ?
C32 C37 1.390(5) . ?
C33 C41 1.389(6) . ?
C34 C36 1.382(6) . ?
C35 C40 1.445(6) . ?
C35 N2 1.459(5) . ?
C36 C38 1.383(6) . ?
C37 C41 1.370(6) . ?
C39 C42 1.459(6) . ?
C39 N1 1.461(5) . ?
C40 C46 1.575(7) . ?
C42 C44 1.532(6) . ?
C43 O4 1.457(5) . ?
C44 C49 1.461(7) . ?
C45 C47 1.274(9) . ?
C45 C48 1.534(8) . ?
C46 C48 1.377(8) . ?
C49 C50 1.577(7) . ?

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
C9 C1 C2 120.1(3) . . ?
C9 C1 C19 115.5(3) . . ?
C2 C1 C19 124.3(3) . . ?
C5 C2 C1 117.3(3) . . ?
C5 C2 C10 119.6(3) . . ?
C1 C2 C10 123.1(3) . . ?
C12 C3 C27 118.3(3) . . ?
C12 C3 C4 121.7(3) . . ?
C27 C3 C4 120.0(3) . . ?
C9 C4 C17 117.3(3) . . ?
C9 C4 C3 118.9(3) . . ?
C17 C4 C3 123.8(3) . . ?
C2 C5 C17 122.7(3) . . ?
C18 C7 C21 119.6(3) . . ?
C18 C7 C15 134.1(3) . . ?
C21 C7 C15 106.4(3) . . ?
C12 C8 C25 119.6(3) . . ?
C12 C8 C24 133.7(3) . . ?
C25 C8 C24 106.6(3) . . ?
C4 C9 C1 122.2(3) . . ?
C18 C10 C20 118.9(3) . . ?
C18 C10 C2 121.2(3) . . ?
C20 C10 C2 120.0(3) . . ?
C6 C11 O2 108.0(4) . . ?
C3 C12 C8 120.3(3) . . ?
C51 C14 C47 146.6(19) . . ?
C31 C15 C32 119.4(3) . . ?
C31 C15 C7 107.5(3) . . ?
C32 C15 C7 133.0(3) . . ?
C52 C16 C22 113.4(14) . . ?
C5 C17 C4 120.3(3) . . ?
C5 C17 C23 115.9(3) . . ?
C4 C17 C23 123.8(3) . . ?
C10 C18 C7 119.9(3) . . ?
O1 C19 O2 124.8(4) . . ?
O1 C19 C1 123.3(4) . . ?
O2 C19 C1 111.9(3) . . ?
C26 C20 C10 122.6(3) . . ?
N1 C21 C26 129.0(3) . . ?
N1 C21 C7 109.5(3) . . ?
C26 C21 C7 121.6(3) . . ?
C50 C22 C16 117.8(8) . . ?
O3 C23 O4 125.1(4) . . ?
O3 C23 C17 123.0(4) . . ?
O4 C23 C17 112.0(3) . . ?
C30 C24 C28 119.7(3) . . ?
C30 C24 C8 106.8(3) . . ?
C28 C24 C8 133.5(3) . . ?
N2 C25 C29 129.5(3) . . ?
N2 C25 C8 109.1(3) . . ?
C29 C25 C8 121.4(3) . . ?
C20 C26 C21 117.5(3) . . ?
C29 C27 C3 122.8(3) . . ?
C38 C28 C24 118.3(4) . . ?
C27 C29 C25 117.5(3) . . ?
C34 C30 C24 122.5(4) . . ?
C34 C30 N2 128.3(4) . . ?
C24 C30 N2 109.2(3) . . ?
C33 C31 C15 122.7(4) . . ?
C33 C31 N1 128.4(4) . . ?
C15 C31 N1 108.8(3) . . ?
C37 C32 C15 118.1(4) . . ?
C31 C33 C41 116.9(4) . . ?
C36 C34 C30 116.7(4) . . ?
C40 C35 N2 117.0(4) . . ?
C34 C36 C38 122.1(4) . . ?
C41 C37 C32 121.6(4) . . ?
C36 C38 C28 120.7(4) . . ?
C42 C39 N1 117.2(4) . . ?
C35 C40 C46 108.3(5) . . ?
C37 C41 C33 121.3(4) . . ?
C39 C42 C44 111.9(4) . . ?
C13 C43 O4 108.1(5) . . ?
C49 C44 C42 117.5(5) . . ?
C47 C45 C48 122.3(7) . . ?
C48 C46 C40 118.0(6) . . ?
C45 C47 C14 122.6(12) . . ?
C46 C48 C45 117.3(6) . . ?
C44 C49 C50 111.7(5) . . ?
C22 C50 C49 115.1(6) . . ?
C21 N1 C31 107.8(3) . . ?
C21 N1 C39 126.3(3) . . ?
C31 N1 C39 125.9(3) . . ?
C25 N2 C30 108.3(3) . . ?
C25 N2 C35 125.4(3) . . ?
C30 N2 C35 126.3(3) . . ?
C23 O4 C43 115.7(3) . . ?
C19 O2 C11 115.7(3) . . ?

_diffrn_measured_fraction_theta_max 0.868
_diffrn_reflns_theta_full        30.02
_diffrn_measured_fraction_theta_full 0.868
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.054
####################################################################### 
# 
# 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_20140728-bect1
_database_code_depnum_ccdc_archive 'CCDC 1031692'
_audit_update_record             
;
2014-10-30 deposited with the CCDC.
2015-03-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H36 N2 O4'
_chemical_formula_weight         608.71

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   18.0254(6)
_cell_length_b                   9.4485(3)
_cell_length_c                   18.8799(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3215.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1655
_cell_measurement_theta_min      3.2305
_cell_measurement_theta_max      29.6506

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1288
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.988
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9753
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.25
_diffrn_reflns_theta_max         29.72
_reflns_number_total             4071
_reflns_number_gt                2927
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0445P)²+0.9351P] 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         4071
_refine_ls_number_parameters     210
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0533
_refine_ls_wR_factor_ref         0.1227
_refine_ls_wR_factor_gt          0.1101
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.15381(6) 0.25573(13) 0.46031(7) 0.0535(3) Uani 1 1 d . . .
O2 O 0.19726(6) 0.45501(12) 0.50864(7) 0.0504(3) Uani 1 1 d . . .
C3 C 0.01211(8) 0.36575(15) 0.53206(8) 0.0328(3) Uani 1 1 d . . .
C4 C 0.05700(8) 0.56811(16) 0.46628(8) 0.0352(3) Uani 1 1 d . . .
H4 H 0.0963 0.6137 0.4439 0.042 Uiso 1 1 calc R . .
N5 N 0.04960(8) -0.12269(13) 0.69816(8) 0.0434(3) Uani 1 1 d . . .
C6 C 0.14370(8) 0.36953(16) 0.48620(8) 0.0361(3) Uani 1 1 d . . .
C7 C 0.06923(7) 0.43664(15) 0.49686(8) 0.0333(3) Uani 1 1 d . . .
C8 C 0.08241(8) 0.21412(14) 0.61712(8) 0.0332(3) Uani 1 1 d . . .
H8 H 0.1180 0.2850 0.6213 0.040 Uiso 1 1 calc R . .
C9 C 0.02305(8) 0.23104(15) 0.57126(8) 0.0337(3) Uani 1 1 d . . .
C10 C 0.08867(8) 0.09084(14) 0.65692(8) 0.0329(3) Uani 1 1 d . . .
C11 C 0.03408(9) -0.01574(15) 0.65033(8) 0.0367(3) Uani 1 1 d . . .
C12 C 0.13874(9) 0.04517(15) 0.71193(8) 0.0366(3) Uani 1 1 d . . .
C13 C -0.02948(8) 0.12193(16) 0.56518(9) 0.0413(4) Uani 1 1 d . . .
H13 H -0.0689 0.1334 0.5340 0.050 Uiso 1 1 calc R . .
C14 C 0.11192(9) -0.08680(16) 0.73616(8) 0.0399(4) Uani 1 1 d . . .
C15 C -0.02466(9) -0.00144(16) 0.60383(10) 0.0441(4) Uani 1 1 d . . .
H15 H -0.0598 -0.0728 0.5988 0.053 Uiso 1 1 calc R . .
C16 C 0.14619(11) -0.15844(18) 0.79126(9) 0.0491(4) Uani 1 1 d . . .
H16 H 0.1276 -0.2443 0.8076 0.059 Uiso 1 1 calc R . .
C17 C 0.20168(10) 0.10218(18) 0.74287(10) 0.0491(4) Uani 1 1 d . . .
H17 H 0.2205 0.1885 0.7275 0.059 Uiso 1 1 calc R . .
C18 C 0.00772(11) -0.25318(18) 0.70726(11) 0.0580(5) Uani 1 1 d . . .
H18A H -0.0416 -0.2404 0.6877 0.070 Uiso 1 1 calc R . .
H18B H 0.0025 -0.2724 0.7575 0.070 Uiso 1 1 calc R . .
C19 C 0.23595(12) 0.0289(2) 0.79691(11) 0.0605(5) Uani 1 1 d . . .
H19 H 0.2785 0.0661 0.8176 0.073 Uiso 1 1 calc R . .
C20 C 0.27304(8) 0.4032(2) 0.50394(12) 0.0574(5) Uani 1 1 d . . .
H20A H 0.3069 0.4826 0.5005 0.069 Uiso 1 1 calc R . .
H20B H 0.2786 0.3460 0.4616 0.069 Uiso 1 1 calc R . .
C21 C 0.20802(12) -0.09945(19) 0.82091(10) 0.0572(5) Uani 1 1 d . . .
H21 H 0.2319 -0.1461 0.8578 0.069 Uiso 1 1 calc R . .
C22 C 0.29167(11) 0.3169(2) 0.56739(12) 0.0681(6) Uani 1 1 d . . .
H22A H 0.2610 0.2339 0.5684 0.102 Uiso 1 1 calc R . .
H22B H 0.2832 0.3718 0.6094 0.102 Uiso 1 1 calc R . .
H22C H 0.3429 0.2893 0.5653 0.102 Uiso 1 1 calc R . .
C23 C 0.04340(15) -0.3780(2) 0.67237(13) 0.0768(7) Uani 1 1 d . . .
H23A H 0.0472 -0.3611 0.6224 0.115 Uiso 1 1 calc R . .
H23B H 0.0138 -0.4609 0.6806 0.115 Uiso 1 1 calc R . .
H23C H 0.0921 -0.3920 0.6918 0.115 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 C6 1.1952(18) . ?
O2 C6 1.3281(18) . ?
O2 C20 1.4537(18) . ?
C3 C4 1.3939(19) 5_566 ?
C3 C7 1.397(2) . ?
C3 C9 1.485(2) . ?
C4 C7 1.387(2) . ?
C4 C3 1.3939(19) 5_566 ?
N5 C14 1.375(2) . ?
N5 C11 1.384(2) . ?
N5 C18 1.456(2) . ?
C6 C7 1.4983(19) . ?
C8 C9 1.386(2) . ?
C8 C10 1.391(2) . ?
C9 C13 1.405(2) . ?
C10 C11 1.413(2) . ?
C10 C12 1.442(2) . ?
C11 C15 1.382(2) . ?
C12 C17 1.385(2) . ?
C12 C14 1.414(2) . ?
C13 C15 1.378(2) . ?
C14 C16 1.386(2) . ?
C16 C21 1.366(3) . ?
C17 C19 1.379(2) . ?
C18 C23 1.496(3) . ?
C19 C21 1.389(3) . ?
C20 C22 1.488(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
C6 O2 C20 117.30(13) . . ?
C4 C3 C7 117.04(13) 5_566 . ?
C4 C3 C9 119.44(13) 5_566 . ?
C7 C3 C9 123.38(12) . . ?
C7 C4 C3 122.27(13) . 5_566 ?
C14 N5 C11 109.00(12) . . ?
C14 N5 C18 124.80(15) . . ?
C11 N5 C18 126.20(15) . . ?
O1 C6 O2 124.53(14) . . ?
O1 C6 C7 124.91(14) . . ?
O2 C6 C7 110.56(13) . . ?
C4 C7 C3 120.68(13) . . ?
C4 C7 C6 117.73(13) . . ?
C3 C7 C6 121.44(13) . . ?
C9 C8 C10 119.80(13) . . ?
C8 C9 C13 119.14(14) . . ?
C8 C9 C3 120.84(12) . . ?
C13 C9 C3 119.92(13) . . ?
C8 C10 C11 119.51(14) . . ?
C8 C10 C12 133.67(14) . . ?
C11 C10 C12 106.62(13) . . ?
C15 C11 N5 129.85(14) . . ?
C15 C11 C10 121.31(14) . . ?
N5 C11 C10 108.78(14) . . ?
C17 C12 C14 119.13(15) . . ?
C17 C12 C10 134.43(14) . . ?
C14 C12 C10 106.44(14) . . ?
C15 C13 C9 122.36(15) . . ?
N5 C14 C16 129.43(15) . . ?
N5 C14 C12 109.15(14) . . ?
C16 C14 C12 121.41(16) . . ?
C13 C15 C11 117.86(14) . . ?
C21 C16 C14 118.16(16) . . ?
C19 C17 C12 118.93(16) . . ?
N5 C18 C23 113.12(16) . . ?
C17 C19 C21 121.16(19) . . ?
O2 C20 C22 110.34(16) . . ?
C16 C21 C19 121.20(18) . . ?

_diffrn_measured_fraction_theta_max 0.891
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.042
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_preparation       Luminescent
