# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_Cage3_R_3(Et2O)_CH2Cl2_100K

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H84 N12, C H2 Cl2, 3(C4 H10 O)'
_chemical_formula_sum            'C85 H116 Cl2 N12 O3'
_chemical_formula_weight         1424.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R3

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

_cell_length_a                   25.629(3)
_cell_length_b                   25.629(3)
_cell_length_c                   11.1848(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6362.6(14)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8881
_cell_measurement_theta_min      2.457
_cell_measurement_theta_max      20.367

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.156
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2313
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4973
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  confocal
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            14584
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0906
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         23.25
_reflns_number_total             3644
_reflns_number_gt                3527
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.1 (Rigaku, 2011)'
_computing_cell_refinement       'Bruker AXS SAINT V7.68A'
_computing_data_reduction        'Bruker AXS SAINT V7.68A'
_computing_structure_solution    'SHELXD (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1535P)²+49.8181P] 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   0.2(9)
_refine_ls_number_reflns         3644
_refine_ls_number_parameters     319
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.1095
_refine_ls_wR_factor_ref         0.3020
_refine_ls_wR_factor_gt          0.3007
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_restrained_S_all      1.155
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.6338(8) 0.3459(8) 0.7214(9) 0.072(4) Uani 0.17 1 d PDU . 1
Cl3 Cl 0.6608(13) 0.3712(7) 0.8643(10) 0.157(7) Uiso 0.17 1 d PDU . 2
Cl2 Cl 0.666(3) 0.3180(18) 0.9525(10) 0.157(7) Uiso 0.17 1 d PDU . 1
Cl4 Cl 0.6667 0.3333 1.1051(9) 0.171(8) Uani 0.50 3 d SPDU . 2
O1 O 0.6175(4) 0.5141(3) 0.7322(8) 0.098(3) Uani 1 1 d DU A 2
N1 N 0.5022(3) 0.2794(3) 0.4418(6) 0.0375(15) Uani 1 1 d . . .
N2 N 0.4366(3) 0.2352(3) 0.6675(7) 0.0385(16) Uani 1 1 d . . .
N3 N 0.5220(3) 0.4029(3) 1.1346(6) 0.0358(15) Uani 1 1 d . . .
N4 N 0.6448(3) 0.4994(3) 1.1534(7) 0.0370(15) Uani 1 1 d . . .
C1 C 0.6316(3) 0.3607(3) 0.4258(8) 0.0338(17) Uani 1 1 d . . .
H1 H 0.6074 0.3792 0.4260 0.041 Uiso 1 1 calc R . .
C2 C 0.6028(3) 0.2970(3) 0.4256(7) 0.0312(17) Uani 1 1 d . . .
C3 C 0.5380(4) 0.2591(4) 0.4299(7) 0.0355(17) Uani 1 1 d . . .
H3 H 0.5213 0.2167 0.4233 0.043 Uiso 1 1 calc R . .
C4 C 0.4383(3) 0.2373(3) 0.4464(8) 0.0372(18) Uani 1 1 d . . .
H4 H 0.4315 0.1953 0.4432 0.045 Uiso 1 1 calc R . .
C5 C 0.4099(3) 0.2445(4) 0.5594(8) 0.043(2) Uani 1 1 d . . .
H5 H 0.4178 0.2869 0.5612 0.051 Uiso 1 1 calc R . .
C6 C 0.3420(4) 0.2029(5) 0.5602(9) 0.054(2) Uani 1 1 d . . .
H6A H 0.3250 0.2099 0.6339 0.064 Uiso 1 1 calc R . .
H6B H 0.3329 0.1605 0.5610 0.064 Uiso 1 1 calc R . .
C7 C 0.3124(4) 0.2130(6) 0.4518(9) 0.068(3) Uani 1 1 d . . .
H7A H 0.2686 0.1838 0.4530 0.082 Uiso 1 1 calc R . .
H7B H 0.3180 0.2541 0.4550 0.082 Uiso 1 1 calc R . .
C8 C 0.3397(4) 0.2055(5) 0.3370(8) 0.049(2) Uani 1 1 d . . .
H8A H 0.3218 0.2149 0.2675 0.059 Uiso 1 1 calc R . .
H8B H 0.3303 0.1632 0.3295 0.059 Uiso 1 1 calc R . .
C9 C 0.4084(4) 0.2477(4) 0.3371(9) 0.047(2) Uani 1 1 d . . .
H9A H 0.4175 0.2900 0.3368 0.056 Uiso 1 1 calc R . .
H9B H 0.4256 0.2409 0.2633 0.056 Uiso 1 1 calc R . .
C10 C 0.4528(4) 0.2736(4) 0.7448(9) 0.0402(18) Uani 1 1 d . . .
H10 H 0.4499 0.3084 0.7284 0.048 Uiso 1 1 calc R . .
C11 C 0.4773(3) 0.2695(3) 0.8653(8) 0.0340(17) Uani 1 1 d . . .
C12 C 0.4808(3) 0.2183(4) 0.8949(8) 0.0357(18) Uani 1 1 d . . .
H12 H 0.4717 0.1878 0.8371 0.043 Uiso 1 1 calc R . .
C13 C 0.4977(3) 0.2130(3) 1.0090(8) 0.0355(18) Uani 1 1 d . . .
C14 C 0.5148(3) 0.2593(3) 1.0911(8) 0.0293(16) Uani 1 1 d . . .
H14 H 0.5280 0.2558 1.1685 0.035 Uiso 1 1 calc R . .
C15 C 0.5129(3) 0.3105(3) 1.0610(8) 0.0356(18) Uani 1 1 d . . .
C16 C 0.4941(3) 0.3153(3) 0.9467(8) 0.0380(19) Uani 1 1 d . . .
H16 H 0.4930 0.3505 0.9248 0.046 Uiso 1 1 calc R . .
C17 C 0.5306(3) 0.3594(4) 1.1500(7) 0.0382(19) Uani 1 1 d . . .
H17 H 0.5493 0.3576 1.2219 0.046 Uiso 1 1 calc R . .
C18 C 0.5418(3) 0.4463(3) 1.2287(8) 0.0338(17) Uani 1 1 d . . .
H18 H 0.5559 0.4319 1.2979 0.041 Uiso 1 1 calc R . .
C19 C 0.5936(3) 0.5071(4) 1.1838(8) 0.0391(19) Uani 1 1 d . . .
H19 H 0.5802 0.5198 1.1110 0.047 Uiso 1 1 calc R . .
C20 C 0.6127(4) 0.5546(4) 1.2772(8) 0.045(2) Uani 1 1 d . . .
H20A H 0.6460 0.5928 1.2452 0.054 Uiso 1 1 calc R . .
H20B H 0.6284 0.5430 1.3469 0.054 Uiso 1 1 calc R . .
C21 C 0.5620(5) 0.5651(4) 1.3188(9) 0.052(2) Uani 1 1 d . . .
H21A H 0.5489 0.5813 1.2521 0.062 Uiso 1 1 calc R . .
H21B H 0.5763 0.5947 1.3850 0.062 Uiso 1 1 calc R . .
C22 C 0.5095(4) 0.5050(4) 1.3611(9) 0.050(2) Uani 1 1 d . . .
H22A H 0.5221 0.4921 1.4339 0.060 Uiso 1 1 calc R . .
H22B H 0.4755 0.5110 1.3833 0.060 Uiso 1 1 calc R . .
C23 C 0.4880(4) 0.4554(4) 1.2692(9) 0.048(2) Uani 1 1 d . . .
H23A H 0.4715 0.4659 1.1991 0.058 Uiso 1 1 calc R . .
H23B H 0.4555 0.4174 1.3037 0.058 Uiso 1 1 calc R . .
C24 C 0.6597(3) 0.5049(3) 1.0445(8) 0.0339(17) Uani 1 1 d . . .
H24 H 0.6363 0.5107 0.9857 0.041 Uiso 1 1 calc R . .
C25 C 0.6014(9) 0.4172(5) 0.7126(15) 0.113(6) Uani 1 1 d DU A 2
H25A H 0.6238 0.3983 0.6823 0.170 Uiso 1 1 calc R A 2
H25B H 0.5581 0.3900 0.6998 0.170 Uiso 1 1 calc R A 2
H25C H 0.6092 0.4252 0.7983 0.170 Uiso 1 1 calc R A 2
C26 C 0.6208(3) 0.4744(3) 0.6486(7) 0.0528(19) Uani 1 1 d DU A 2
H26A H 0.6625 0.4911 0.6187 0.063 Uiso 1 1 calc R A 2
H26B H 0.5939 0.4678 0.5797 0.063 Uiso 1 1 calc R A 2
C27 C 0.6499(6) 0.5679(4) 0.6639(9) 0.087(3) Uani 1 1 d DU A 2
H27A H 0.6300 0.5672 0.5877 0.104 Uiso 1 1 calc R A 2
H27B H 0.6926 0.5796 0.6501 0.104 Uiso 1 1 calc R A 2
C28 C 0.6421(4) 0.6031(4) 0.7573(9) 0.060(2) Uani 1 1 d DU A 2
H28A H 0.6353 0.6339 0.7206 0.091 Uiso 1 1 calc R A 2
H28B H 0.6783 0.6226 0.8072 0.091 Uiso 1 1 calc R A 2
H28C H 0.6073 0.5764 0.8070 0.091 Uiso 1 1 calc R A 2
C29 C 0.6608(13) 0.3712(7) 0.8643(10) 0.157(7) Uiso 0.17 1 d PDU B 1
H29A H 0.6339 0.3832 0.9042 0.189 Uiso 0.17 1 calc PR B 1
H29B H 0.7012 0.4075 0.8582 0.189 Uiso 0.17 1 calc PR B 1
C30 C 0.666(3) 0.3180(18) 0.9525(10) 0.157(7) Uiso 0.17 1 d PDU C 2
H30A H 0.7029 0.3173 0.9317 0.189 Uiso 0.17 1 calc PR C 2
H30B H 0.6310 0.2777 0.9353 0.189 Uiso 0.17 1 calc PR C 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
Cl1 Cl1 1.80(3) 3_665 ?
Cl1 Cl1 1.80(3) 2_655 ?
Cl1 C29 2.11(3) 2_655 ?
Cl3 C30 1.31(4) 3_665 ?
Cl3 C30 1.40(4) 2_655 ?
Cl3 Cl3 1.83(3) 2_655 ?
Cl3 Cl3 1.83(3) 3_665 ?
Cl2 Cl2 0.66(3) 2_655 ?
Cl2 Cl2 0.66(3) 3_665 ?
Cl2 C29 1.31(4) 2_655 ?
Cl2 C29 1.40(4) 3_665 ?
O1 C26 1.416(5) . ?
O1 C27 1.424(5) . ?
N1 C3 1.268(10) . ?
N1 C4 1.442(10) . ?
N2 C10 1.216(10) . ?
N2 C5 1.467(10) . ?
N3 C17 1.254(10) . ?
N3 C18 1.426(10) . ?
N4 C24 1.262(10) . ?
N4 C19 1.463(10) . ?
C1 C2 1.397(10) 3_665 ?
C1 C2 1.415(10) . ?
C2 C1 1.397(10) 2_655 ?
C2 C3 1.447(11) . ?
C4 C5 1.516(11) . ?
C4 C9 1.535(12) . ?
C5 C6 1.519(11) . ?
C6 C7 1.520(13) . ?
C7 C8 1.520(13) . ?
C8 C9 1.539(12) . ?
C10 C11 1.512(11) . ?
C11 C16 1.374(11) . ?
C11 C12 1.397(11) . ?
C12 C13 1.377(12) . ?
C13 C14 1.387(11) . ?
C13 C24 1.513(11) 2_655 ?
C14 C15 1.381(11) . ?
C15 C16 1.392(11) . ?
C15 C17 1.481(11) . ?
C18 C19 1.542(11) . ?
C18 C23 1.575(10) . ?
C19 C20 1.488(12) . ?
C20 C21 1.525(12) . ?
C21 C22 1.528(14) . ?
C22 C23 1.509(13) . ?
C24 C13 1.513(11) 3_665 ?
C25 C26 1.477(5) . ?
C27 C28 1.459(5) . ?

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
Cl1 Cl1 Cl1 60.000(1) 3_665 2_655 ?
Cl1 Cl1 C29 82.9(6) 3_665 2_655 ?
Cl1 Cl1 C29 51.8(7) 2_655 2_655 ?
C30 Cl3 C30 27.9(12) 3_665 2_655 ?
C30 Cl3 Cl3 50(3) 3_665 2_655 ?
C30 Cl3 Cl3 63.6(10) 2_655 2_655 ?
C30 Cl3 Cl3 64.9(15) 3_665 3_665 ?
C30 Cl3 Cl3 45.5(16) 2_655 3_665 ?
Cl3 Cl3 Cl3 60.000(2) 2_655 3_665 ?
Cl2 Cl2 Cl2 60.000(10) 2_655 3_665 ?
Cl2 Cl2 C29 120(3) 2_655 2_655 ?
Cl2 Cl2 C29 84(7) 3_665 2_655 ?
Cl2 Cl2 C29 68(7) 2_655 3_665 ?
Cl2 Cl2 C29 110(6) 3_665 3_665 ?
C29 Cl2 C29 84.7(16) 2_655 3_665 ?
C30 Cl4 C30 21.8(10) 2_655 3_665 ?
C26 O1 C27 97.3(7) . . ?
C3 N1 C4 118.7(7) . . ?
C10 N2 C5 116.9(7) . . ?
C17 N3 C18 116.1(7) . . ?
C24 N4 C19 116.8(7) . . ?
C2 C1 C2 122.2(7) 3_665 . ?
C1 C2 C1 117.8(7) 2_655 . ?
C1 C2 C3 119.8(7) 2_655 . ?
C1 C2 C3 122.4(6) . . ?
N1 C3 C2 123.5(7) . . ?
N1 C4 C5 111.9(6) . . ?
N1 C4 C9 108.7(6) . . ?
C5 C4 C9 109.3(7) . . ?
N2 C5 C6 110.1(7) . . ?
N2 C5 C4 112.0(6) . . ?
C6 C5 C4 111.7(7) . . ?
C5 C6 C7 111.7(7) . . ?
C8 C7 C6 110.6(8) . . ?
C7 C8 C9 110.4(7) . . ?
C8 C9 C4 112.0(7) . . ?
N2 C10 C11 124.3(8) . . ?
C16 C11 C12 120.3(7) . . ?
C16 C11 C10 119.7(7) . . ?
C12 C11 C10 120.0(7) . . ?
C13 C12 C11 118.9(7) . . ?
C12 C13 C14 120.6(7) . . ?
C12 C13 C24 118.7(7) . 2_655 ?
C14 C13 C24 120.6(7) . 2_655 ?
C13 C14 C15 120.4(7) . . ?
C14 C15 C16 119.0(7) . . ?
C14 C15 C17 119.9(7) . . ?
C16 C15 C17 121.1(7) . . ?
C11 C16 C15 120.6(7) . . ?
N3 C17 C15 123.0(7) . . ?
N3 C18 C19 109.8(6) . . ?
N3 C18 C23 109.3(6) . . ?
C19 C18 C23 108.6(6) . . ?
N4 C19 C20 108.9(7) . . ?
N4 C19 C18 108.4(6) . . ?
C20 C19 C18 111.3(7) . . ?
C19 C20 C21 113.4(7) . . ?
C20 C21 C22 108.3(7) . . ?
C23 C22 C21 113.9(7) . . ?
C22 C23 C18 110.1(7) . . ?
N4 C24 C13 119.1(7) . 3_665 ?
O1 C26 C25 106.4(8) . . ?
O1 C27 C28 91.1(7) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        23.25
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.099
_database_code_depnum_ccdc_archive 'CCDC 991214'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Cage3_R_11(N2)_100K_post_desolvation

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            cage3R
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H84 N12, 8(N2), 4(0.75(N2))'
_chemical_formula_sum            'C72 H84 N27'
_chemical_formula_weight         1327.66

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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'

_cell_length_a                   25.2558(11)
_cell_length_b                   25.2558(11)
_cell_length_c                   11.0068(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6080.1(5)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9946
_cell_measurement_theta_min      2.455
_cell_measurement_theta_max      23.217

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.156
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2115.0
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4491
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  confocal
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            41937
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         23.29
_reflns_number_total             9832
_reflns_number_gt                8425
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.1 (Rigaku, 2011)'
_computing_cell_refinement       'Bruker AXS SAINT V7.68A'
_computing_data_reduction        'Bruker AXS SAINT V7.68A'
_computing_structure_solution    'SHELXD (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1191P)²+2.5244P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_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   -1(3)
_refine_ls_number_reflns         9832
_refine_ls_number_parameters     833
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0642
_refine_ls_wR_factor_ref         0.1850
_refine_ls_wR_factor_gt          0.1723
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.49348(16) 0.69900(17) 1.3689(3) 0.0371(9) Uani 1 1 d . . .
N2 N 0.54893(17) 0.70021(17) 1.1360(3) 0.0380(9) Uani 1 1 d . . .
N3 N 0.43881(17) 0.55954(18) 0.6402(4) 0.0411(9) Uani 1 1 d . . .
N4 N 0.31317(17) 0.46926(17) 0.6697(4) 0.0400(9) Uani 1 1 d . . .
N5 N 0.63911(16) 0.46461(16) 0.8510(3) 0.0338(8) Uani 1 1 d . . .
N6 N 0.64932(16) 0.52898(17) 0.6236(4) 0.0370(9) Uani 1 1 d . . .
N7 N 0.50793(18) 0.38472(17) 0.1528(3) 0.0388(9) Uani 1 1 d . . .
N8 N 0.79913(17) 0.54455(17) 0.1358(4) 0.0403(9) Uani 1 1 d . . .
N9 N 0.24357(17) 0.12059(17) 0.4327(4) 0.0410(9) Uani 1 1 d . . .
N10 N 0.16972(16) 0.08769(16) 0.6523(3) 0.0364(9) Uani 1 1 d . . .
N11 N 0.16249(16) -0.03151(16) -0.0568(4) 0.0363(9) Uani 1 1 d . . .
N12 N 0.15495(17) 0.21607(17) -0.0340(3) 0.0374(9) Uani 1 1 d . . .
N13 N 0.2453(4) 0.3432(4) 0.1744(9) 0.123(3) Uiso 1 1 d . . .
N14 N 0.2258(4) 0.3168(4) 0.2433(9) 0.120(3) Uiso 1 1 d . . .
N15 N 0.5044(4) 0.3195(4) 0.5557(9) 0.138(3) Uiso 1 1 d D . .
N16 N 0.5007(5) 0.3287(5) 0.6413(10) 0.157(4) Uiso 1 1 d D . .
N17 N 0.3333 0.6667 0.6596(13) 0.102(4) Uiso 1 3 d S . .
N18 N 0.3333 0.6667 0.7540(15) 0.120(4) Uiso 1 3 d S . .
N19 N 0.6463(12) 0.3375(16) 0.5299(16) 0.156(8) Uiso 0.50 1 d P . .
N20 N 0.6667 0.3333 0.1505(14) 0.109(4) Uiso 1 3 d S . .
N21 N 0.6667 0.3333 0.2455(17) 0.138(5) Uiso 1 3 d S . .
N22 N 0.5147(4) 0.5272(3) 0.1845(7) 0.101(2) Uiso 1 1 d . . .
N23 N 0.5470(3) 0.5410(3) 0.2424(7) 0.0964(19) Uiso 1 1 d . . .
N24 N 0.3734(5) 0.5041(5) 0.0685(10) 0.164(4) Uiso 1 1 d D . .
N25 N 0.3673(5) 0.5115(5) 0.1542(10) 0.145(3) Uiso 1 1 d D . .
N26 N 0.3379(10) 0.6465(8) 0.0512(13) 0.117(5) Uiso 0.50 1 d P . .
N27 N 0.7533(4) 0.6590(3) 0.1668(8) 0.107(2) Uiso 1 1 d . . .
N28 N 0.7314(4) 0.6473(3) 0.2425(8) 0.105(2) Uiso 1 1 d . . .
N29 N 0.0000 0.0000 -0.0482(13) 0.104(4) Uiso 1 3 d SD . .
N30 N 0.0000 0.0000 0.0418(14) 0.193(9) Uiso 1 3 d SD . .
N31 N 0.8095(6) 0.9157(6) 0.4258(11) 0.090(4) Uiso 0.50 1 d PD . .
N32 N 0.8279(5) 0.9082(6) 0.3530(10) 0.083(3) Uiso 0.50 1 d PD . .
N33 N 0.0270(7) 0.0186(11) 0.3247(15) 0.139(7) Uiso 0.50 1 d P . .
C1 C 0.3280(2) 0.6093(2) 1.3632(4) 0.0367(10) Uani 1 1 d . . .
H1 H 0.3242 0.5699 1.3635 0.044 Uiso 1 1 calc R . .
C2 C 0.3856(2) 0.66071(19) 1.3630(4) 0.0345(10) Uani 1 1 d . . .
C3 C 0.4396(2) 0.6536(2) 1.3601(4) 0.0360(10) Uani 1 1 d . . .
H3 H 0.4342 0.6138 1.3514 0.043 Uiso 1 1 calc R . .
C4 C 0.5456(2) 0.6882(2) 1.3570(4) 0.0389(11) Uani 1 1 d . . .
H4 H 0.5300 0.6438 1.3412 0.047 Uiso 1 1 calc R . .
C5 C 0.5826(2) 0.7070(3) 1.4731(5) 0.0488(13) Uani 1 1 d . . .
H5A H 0.5580 0.6792 1.5396 0.059 Uiso 1 1 calc R . .
H5B H 0.5926 0.7489 1.4953 0.059 Uiso 1 1 calc R . .
C6 C 0.6422(2) 0.7050(3) 1.4590(5) 0.0520(13) Uani 1 1 d . . .
H6A H 0.6661 0.7192 1.5352 0.062 Uiso 1 1 calc R . .
H6B H 0.6323 0.6624 1.4441 0.062 Uiso 1 1 calc R . .
C7 C 0.6801(2) 0.7453(3) 1.3545(5) 0.0514(13) Uani 1 1 d . . .
H7A H 0.6923 0.7884 1.3712 0.062 Uiso 1 1 calc R . .
H7B H 0.7178 0.7426 1.3452 0.062 Uiso 1 1 calc R . .
C8 C 0.6430(2) 0.7243(2) 1.2394(5) 0.0468(12) Uani 1 1 d . . .
H8A H 0.6334 0.6820 1.2210 0.056 Uiso 1 1 calc R . .
H8B H 0.6678 0.7508 1.1715 0.056 Uiso 1 1 calc R . .
C9 C 0.5837(2) 0.7260(2) 1.2479(4) 0.0413(11) Uani 1 1 d . . .
H9 H 0.5932 0.7693 1.2571 0.050 Uiso 1 1 calc R . .
C10 C 0.5411(2) 0.7357(2) 1.0645(4) 0.0403(11) Uani 1 1 d . . .
H10 H 0.5540 0.7763 1.0902 0.048 Uiso 1 1 calc R . .
C11 C 0.5137(2) 0.7162(2) 0.9467(4) 0.0360(10) Uani 1 1 d . . .
C12 C 0.4884(2) 0.6551(2) 0.9075(4) 0.0392(11) Uani 1 1 d . . .
H12 H 0.4853 0.6251 0.9637 0.047 Uiso 1 1 calc R . .
C13 C 0.46815(19) 0.6376(2) 0.7910(4) 0.0347(10) Uani 1 1 d . . .
C14 C 0.47117(19) 0.6812(2) 0.7081(4) 0.0358(10) Uani 1 1 d . . .
H14 H 0.4568 0.6693 0.6273 0.043 Uiso 1 1 calc R . .
C15 C 0.4951(2) 0.7417(2) 0.7436(4) 0.0372(11) Uani 1 1 d . . .
C16 C 0.5154(2) 0.7584(2) 0.8621(4) 0.0370(10) Uani 1 1 d . . .
H16 H 0.5308 0.7997 0.8866 0.044 Uiso 1 1 calc R . .
C17 C 0.4464(2) 0.5742(2) 0.7510(4) 0.0378(11) Uani 1 1 d . . .
H17 H 0.4379 0.5436 0.8103 0.045 Uiso 1 1 calc R . .
C18 C 0.4159(2) 0.4941(2) 0.6110(5) 0.0401(11) Uani 1 1 d . . .
H18 H 0.4179 0.4724 0.6853 0.048 Uiso 1 1 calc R . .
C19 C 0.4545(2) 0.4892(2) 0.5121(5) 0.0502(13) Uani 1 1 d . . .
H19A H 0.4971 0.5070 0.5413 0.060 Uiso 1 1 calc R . .
H19B H 0.4547 0.5131 0.4407 0.060 Uiso 1 1 calc R . .
C20 C 0.4306(2) 0.4230(3) 0.4742(6) 0.0558(14) Uani 1 1 d . . .
H20A H 0.4342 0.3999 0.5432 0.067 Uiso 1 1 calc R . .
H20B H 0.4556 0.4217 0.4063 0.067 Uiso 1 1 calc R . .
C21 C 0.3637(3) 0.3931(3) 0.4345(6) 0.0601(15) Uani 1 1 d . . .
H21A H 0.3479 0.3493 0.4168 0.072 Uiso 1 1 calc R . .
H21B H 0.3607 0.4130 0.3592 0.072 Uiso 1 1 calc R . .
C22 C 0.3245(2) 0.3994(2) 0.5352(5) 0.0541(14) Uani 1 1 d . . .
H22A H 0.2819 0.3819 0.5064 0.065 Uiso 1 1 calc R . .
H22B H 0.3243 0.3761 0.6078 0.065 Uiso 1 1 calc R . .
C23 C 0.3495(2) 0.4659(2) 0.5697(5) 0.0434(12) Uani 1 1 d . . .
H23 H 0.3471 0.4890 0.4981 0.052 Uiso 1 1 calc R . .
C24 C 0.2860(2) 0.4994(2) 0.6518(4) 0.0408(11) Uani 1 1 d . . .
H24 H 0.2914 0.5193 0.5759 0.049 Uiso 1 1 calc R . .
C25 C 0.61571(19) 0.34089(19) 0.8499(4) 0.0308(9) Uani 1 1 d . . .
H25 H 0.5810 0.3461 0.8493 0.037 Uiso 1 1 calc R . .
C26 C 0.67435(19) 0.39226(19) 0.8504(4) 0.0309(9) Uani 1 1 d . . .
C27 C 0.6830(2) 0.4545(2) 0.8469(4) 0.0348(10) Uani 1 1 d . . .
H27 H 0.7233 0.4883 0.8413 0.042 Uiso 1 1 calc R . .
C28 C 0.6521(2) 0.52813(19) 0.8451(4) 0.0354(10) Uani 1 1 d . . .
H28 H 0.6972 0.5563 0.8372 0.043 Uiso 1 1 calc R . .
C29 C 0.6292(2) 0.5432(2) 0.9615(4) 0.0420(11) Uani 1 1 d . . .
H29A H 0.5859 0.5118 0.9753 0.050 Uiso 1 1 calc R . .
H29B H 0.6534 0.5423 1.0315 0.050 Uiso 1 1 calc R . .
C30 C 0.6346(2) 0.6060(2) 0.9538(5) 0.0466(12) Uani 1 1 d . . .
H30A H 0.6193 0.6144 1.0298 0.056 Uiso 1 1 calc R . .
H30B H 0.6781 0.6378 0.9442 0.056 Uiso 1 1 calc R . .
C31 C 0.5981(2) 0.6084(2) 0.8468(5) 0.0455(12) Uani 1 1 d . . .
H31A H 0.5544 0.5777 0.8580 0.055 Uiso 1 1 calc R . .
H31B H 0.6020 0.6493 0.8424 0.055 Uiso 1 1 calc R . .
C32 C 0.6211(2) 0.5955(2) 0.7300(5) 0.0403(11) Uani 1 1 d . . .
H32A H 0.6636 0.6287 0.7152 0.048 Uiso 1 1 calc R . .
H32B H 0.5956 0.5952 0.6616 0.048 Uiso 1 1 calc R . .
C33 C 0.6198(2) 0.5344(2) 0.7335(4) 0.0348(10) Uani 1 1 d . . .
H33 H 0.5762 0.5006 0.7343 0.042 Uiso 1 1 calc R . .
C34 C 0.6157(2) 0.4903(2) 0.5445(4) 0.0364(11) Uani 1 1 d . . .
H34 H 0.5737 0.4645 0.5635 0.044 Uiso 1 1 calc R . .
C35 C 0.6371(2) 0.48272(19) 0.4264(4) 0.0367(10) Uani 1 1 d . . .
C36 C 0.5940(2) 0.4451(2) 0.3410(4) 0.0388(11) Uani 1 1 d . . .
H36 H 0.5520 0.4232 0.3633 0.047 Uiso 1 1 calc R . .
C37 C 0.61051(19) 0.4388(2) 0.2247(4) 0.0349(10) Uani 1 1 d . . .
C38 C 0.6717(2) 0.4680(2) 0.1940(4) 0.0383(11) Uani 1 1 d . . .
H38 H 0.6835 0.4625 0.1152 0.046 Uiso 1 1 calc R . .
C39 C 0.7164(2) 0.5057(2) 0.2776(4) 0.0382(11) Uani 1 1 d . . .
C40 C 0.6987(2) 0.5125(2) 0.3934(4) 0.0381(11) Uani 1 1 d . . .
H40 H 0.7289 0.5377 0.4509 0.046 Uiso 1 1 calc R . .
C41 C 0.7814(2) 0.5403(2) 0.2428(5) 0.0369(11) Uani 1 1 d . . .
H41 H 0.8112 0.5603 0.3047 0.044 Uiso 1 1 calc R . .
C42 C 0.1908(2) 0.3008(2) -0.1781(5) 0.0426(11) Uani 1 1 d . . .
H42A H 0.2093 0.3291 -0.1086 0.051 Uiso 1 1 calc R . .
H42B H 0.2220 0.2921 -0.2117 0.051 Uiso 1 1 calc R . .
C43 C 0.5633(2) 0.4026(2) 0.1325(4) 0.0389(11) Uani 1 1 d . . .
H43 H 0.5750 0.3928 0.0575 0.047 Uiso 1 1 calc R . .
C44 C 0.4627(2) 0.3486(2) 0.0597(5) 0.0408(11) Uani 1 1 d . . .
H44 H 0.4841 0.3446 -0.0131 0.049 Uiso 1 1 calc R . .
C45 C 0.4203(2) 0.2857(2) 0.1114(5) 0.0415(11) Uani 1 1 d . . .
H45 H 0.4019 0.2898 0.1889 0.050 Uiso 1 1 calc R . .
C46 C 0.3689(2) 0.2476(2) 0.0198(5) 0.0506(13) Uani 1 1 d . . .
H46A H 0.3869 0.2404 -0.0538 0.061 Uiso 1 1 calc R . .
H46B H 0.3403 0.2074 0.0562 0.061 Uiso 1 1 calc R . .
C47 C 0.3342(2) 0.2795(3) -0.0156(6) 0.0606(15) Uani 1 1 d . . .
H47A H 0.3027 0.2545 -0.0767 0.073 Uiso 1 1 calc R . .
H47B H 0.3131 0.2835 0.0566 0.073 Uiso 1 1 calc R . .
C48 C 0.3763(3) 0.3420(3) -0.0675(6) 0.0630(16) Uani 1 1 d . . .
H48A H 0.3527 0.3627 -0.0862 0.076 Uiso 1 1 calc R . .
H48B H 0.3945 0.3380 -0.1441 0.076 Uiso 1 1 calc R . .
C49 C 0.4269(2) 0.3803(2) 0.0226(5) 0.0492(13) Uani 1 1 d . . .
H49A H 0.4087 0.3877 0.0958 0.059 Uiso 1 1 calc R . .
H49B H 0.4552 0.4205 -0.0144 0.059 Uiso 1 1 calc R . .
C50 C 0.0443(2) 0.0615(2) 0.6517(4) 0.0349(10) Uani 1 1 d . . .
H50 H 0.0749 0.1034 0.6509 0.042 Uiso 1 1 calc R . .
C51 C 0.0616(2) 0.01625(19) 0.6522(4) 0.0343(10) Uani 1 1 d . . .
C52 C 0.1269(2) 0.0335(2) 0.6482(4) 0.0354(10) Uani 1 1 d . . .
H52 H 0.1367 0.0019 0.6423 0.043 Uiso 1 1 calc R . .
C53 C 0.2324(2) 0.0988(2) 0.6483(4) 0.0367(10) Uani 1 1 d . . .
H53 H 0.2310 0.0597 0.6257 0.044 Uiso 1 1 calc R . .
C54 C 0.2609(2) 0.1179(2) 0.7729(4) 0.0415(11) Uani 1 1 d . . .
H54A H 0.2379 0.0841 0.8312 0.050 Uiso 1 1 calc R . .
H54B H 0.2584 0.1538 0.8006 0.050 Uiso 1 1 calc R . .
C55 C 0.3278(2) 0.1339(2) 0.7712(5) 0.0423(11) Uani 1 1 d . . .
H55A H 0.3302 0.0970 0.7501 0.051 Uiso 1 1 calc R . .
H55B H 0.3457 0.1475 0.8531 0.051 Uiso 1 1 calc R . .
C56 C 0.3647(2) 0.1845(2) 0.6790(5) 0.0456(12) Uani 1 1 d . . .
H56A H 0.3652 0.2224 0.7031 0.055 Uiso 1 1 calc R . .
H56B H 0.4075 0.1930 0.6771 0.055 Uiso 1 1 calc R . .
C57 C 0.3361(2) 0.1644(2) 0.5535(5) 0.0449(12) Uani 1 1 d . . .
H57A H 0.3590 0.1982 0.4952 0.054 Uiso 1 1 calc R . .
H57B H 0.3398 0.1290 0.5267 0.054 Uiso 1 1 calc R . .
C58 C 0.2687(2) 0.1468(2) 0.5504(4) 0.0368(10) Uani 1 1 d . . .
H58 H 0.2650 0.1839 0.5640 0.044 Uiso 1 1 calc R . .
C59 C 0.2258(2) 0.1480(2) 0.3619(4) 0.0386(11) Uani 1 1 d . . .
H59 H 0.2279 0.1849 0.3874 0.046 Uiso 1 1 calc R . .
C60 C 0.2019(2) 0.1232(2) 0.2403(4) 0.0372(11) Uani 1 1 d . . .
C61 C 0.1957(2) 0.0669(2) 0.2048(4) 0.0362(10) Uani 1 1 d . . .
H61 H 0.2063 0.0449 0.2601 0.043 Uiso 1 1 calc R . .
C62 C 0.1745(2) 0.04338(19) 0.0918(4) 0.0342(10) Uani 1 1 d . . .
C63 C 0.1580(2) 0.0756(2) 0.0092(4) 0.0345(10) Uani 1 1 d . . .
H63 H 0.1431 0.0593 -0.0692 0.041 Uiso 1 1 calc R . .
C64 C 0.1638(2) 0.1313(2) 0.0431(4) 0.0359(10) Uani 1 1 d . . .
C65 C 0.1858(2) 0.1551(2) 0.1571(4) 0.0382(11) Uani 1 1 d . . .
H65 H 0.1901 0.1933 0.1795 0.046 Uiso 1 1 calc R . .
C66 C 0.1734(2) -0.0132(2) 0.0520(4) 0.0349(10) Uani 1 1 d . . .
H66 H 0.1810 -0.0364 0.1100 0.042 Uiso 1 1 calc R . .
C67 C 0.1473(2) 0.1629(2) -0.0482(4) 0.0344(10) Uani 1 1 d . . .
H67 H 0.1299 0.1423 -0.1224 0.041 Uiso 1 1 calc R . .
C68 C 0.13634(19) 0.24133(19) -0.1332(4) 0.0347(10) Uani 1 1 d . . .
H68 H 0.1203 0.2112 -0.2016 0.042 Uiso 1 1 calc R . .
C69 C 0.0852(2) 0.25256(19) -0.0877(4) 0.0344(10) Uani 1 1 d . . .
H69 H 0.0996 0.2793 -0.0140 0.041 Uiso 1 1 calc R . .
C70 C 0.0669(2) 0.2829(2) -0.1860(5) 0.0409(11) Uani 1 1 d . . .
H70A H 0.0492 0.2548 -0.2560 0.049 Uiso 1 1 calc R . .
H70B H 0.0353 0.2914 -0.1538 0.049 Uiso 1 1 calc R . .
C71 C 0.1221(2) 0.3423(2) -0.2278(5) 0.0434(12) Uani 1 1 d . . .
H71A H 0.1096 0.3609 -0.2927 0.052 Uiso 1 1 calc R . .
H71B H 0.1381 0.3714 -0.1589 0.052 Uiso 1 1 calc R . .
C72 C 0.1723(2) 0.3314(2) -0.2752(5) 0.0460(12) Uani 1 1 d . . .
H72A H 0.1576 0.3050 -0.3482 0.055 Uiso 1 1 calc R . .
H72B H 0.2083 0.3708 -0.2988 0.055 Uiso 1 1 calc R . .
N34 N 0.8166(12) 0.8806(8) 0.4239(17) 0.186(9) Uiso 0.50 1 d PD . .


_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
N1 C3 1.271(6) . ?
N1 C4 1.479(6) . ?
N2 C10 1.280(6) . ?
N2 C9 1.463(6) . ?
N3 C17 1.261(6) . ?
N3 C18 1.489(6) . ?
N4 C24 1.268(6) . ?
N4 C23 1.462(6) . ?
N5 C27 1.255(5) . ?
N5 C28 1.469(5) . ?
N6 C34 1.266(6) . ?
N6 C33 1.464(6) . ?
N7 C43 1.256(6) . ?
N7 C44 1.465(6) . ?
N8 C41 1.245(6) . ?
N8 C45 1.476(6) 3_665 ?
N9 C59 1.265(6) . ?
N9 C58 1.449(6) . ?
N10 C52 1.250(5) . ?
N10 C53 1.465(6) . ?
N11 C66 1.263(6) . ?
N11 C69 1.462(6) 3 ?
N12 C67 1.268(6) . ?
N12 C68 1.457(6) . ?
N13 N14 0.966(10) . ?
N15 N16 0.987(5) . ?
N17 N18 1.039(16) . ?
N19 N19 1.00(3) 2_655 ?
N19 N19 1.00(3) 3_665 ?
N20 N21 1.046(18) . ?
N22 N23 0.954(8) . ?
N24 N25 0.988(5) . ?
N26 N26 1.00(2) 2_665 ?
N26 N26 1.00(2) 3_565 ?
N27 N28 0.960(9) . ?
N29 N30 0.991(5) . ?
N31 N34 0.990(5) . ?
N31 N32 0.991(5) . ?
N32 N34 0.990(5) . ?
N33 N33 1.05(3) 2 ?
N33 N33 1.05(3) 3 ?
C1 C2 1.382(6) . ?
C1 C2 1.405(6) 3_565 ?
C1 H1 0.9500 . ?
C2 C1 1.405(6) 2_665 ?
C2 C3 1.463(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.512(7) . ?
C4 C9 1.537(7) . ?
C4 H4 1.0000 . ?
C5 C6 1.537(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.517(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.505(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.524(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9 1.0000 . ?
C10 C11 1.437(7) . ?
C10 H10 0.9500 . ?
C11 C16 1.400(6) . ?
C11 C12 1.411(7) . ?
C12 C13 1.369(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.404(6) . ?
C13 C17 1.476(7) . ?
C14 C15 1.389(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(6) . ?
C15 C24 1.473(7) 2_665 ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.507(7) . ?
C18 C23 1.527(7) . ?
C18 H18 1.0000 . ?
C19 C20 1.526(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.531(8) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.546(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.518(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23 1.0000 . ?
C24 C15 1.473(7) 3_565 ?
C24 H24 0.9500 . ?
C25 C26 1.395(6) 2_655 ?
C25 C26 1.398(6) . ?
C25 H25 0.9500 . ?
C26 C25 1.395(6) 3_665 ?
C26 C27 1.476(6) . ?
C27 H27 0.9500 . ?
C28 C33 1.527(6) . ?
C28 C29 1.531(7) . ?
C28 H28 1.0000 . ?
C29 C30 1.524(6) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.515(7) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.512(7) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.525(6) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33 1.0000 . ?
C34 C35 1.457(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.392(7) . ?
C35 C40 1.396(6) . ?
C36 C37 1.380(7) . ?
C36 H36 0.9500 . ?
C37 C38 1.380(6) . ?
C37 C43 1.482(6) . ?
C38 C39 1.398(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.390(7) . ?
C39 C41 1.474(7) . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
C42 C72 1.522(7) . ?
C42 C68 1.525(6) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43 0.9500 . ?
C44 C45 1.514(7) . ?
C44 C49 1.534(7) . ?
C44 H44 1.0000 . ?
C45 N8 1.476(6) 2_655 ?
C45 C46 1.541(7) . ?
C45 H45 1.0000 . ?
C46 C47 1.509(8) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.508(8) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.521(7) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.372(6) 2 ?
C50 C51 1.412(6) . ?
C50 H50 0.9500 . ?
C51 C50 1.372(6) 3 ?
C51 C52 1.480(6) . ?
C52 H52 0.9500 . ?
C53 C54 1.511(7) . ?
C53 C58 1.536(6) . ?
C53 H53 1.0000 . ?
C54 C55 1.528(7) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.530(7) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C57 1.524(7) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C58 1.527(7) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58 1.0000 . ?
C59 C60 1.473(7) . ?
C59 H59 0.9500 . ?
C60 C65 1.406(6) . ?
C60 C61 1.405(6) . ?
C61 C62 1.366(6) . ?
C61 H61 0.9500 . ?
C62 C63 1.415(6) . ?
C62 C66 1.480(6) . ?
C63 C64 1.389(6) . ?
C63 H63 0.9500 . ?
C64 C65 1.382(6) . ?
C64 C67 1.467(6) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C67 H67 0.9500 . ?
C68 C69 1.538(6) . ?
C68 H68 1.0000 . ?
C69 N11 1.462(6) 2 ?
C69 C70 1.525(6) . ?
C69 H69 1.0000 . ?
C70 C71 1.522(6) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C71 C72 1.519(7) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 N1 C4 118.5(4) . . ?
C10 N2 C9 118.3(4) . . ?
C17 N3 C18 116.9(4) . . ?
C24 N4 C23 117.4(4) . . ?
C27 N5 C28 118.8(4) . . ?
C34 N6 C33 117.6(4) . . ?
C43 N7 C44 118.7(4) . . ?
C41 N8 C45 118.3(4) . 3_665 ?
C59 N9 C58 119.8(4) . . ?
C52 N10 C53 118.0(4) . . ?
C66 N11 C69 117.2(4) . 3 ?
C67 N12 C68 117.4(4) . . ?
N19 N19 N19 59.999(14) 2_655 3_665 ?
N26 N26 N26 60.005(10) 2_665 3_565 ?
N34 N31 N32 59.9(4) . . ?
N34 N32 N31 60.0(4) . . ?
N33 N33 N33 60.004(5) 2 3 ?
C2 C1 C2 120.9(4) . 3_565 ?
C2 C1 H1 119.5 . . ?
C2 C1 H1 119.5 3_565 . ?
C1 C2 C1 119.1(4) . 2_665 ?
C1 C2 C3 119.5(4) . . ?
C1 C2 C3 121.5(4) 2_665 . ?
N1 C3 C2 122.1(4) . . ?
N1 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
N1 C4 C5 109.6(4) . . ?
N1 C4 C9 107.0(4) . . ?
C5 C4 C9 111.6(4) . . ?
N1 C4 H4 109.5 . . ?
C5 C4 H4 109.5 . . ?
C9 C4 H4 109.5 . . ?
C4 C5 C6 111.5(4) . . ?
C4 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C7 C6 C5 110.8(4) . . ?
C7 C6 H6A 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C8 C7 C6 109.2(4) . . ?
C8 C7 H7A 109.8 . . ?
C6 C7 H7A 109.8 . . ?
C8 C7 H7B 109.8 . . ?
C6 C7 H7B 109.8 . . ?
H7A C7 H7B 108.3 . . ?
C7 C8 C9 112.8(4) . . ?
C7 C8 H8A 109.0 . . ?
C9 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
C9 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
N2 C9 C8 108.4(4) . . ?
N2 C9 C4 109.4(4) . . ?
C8 C9 C4 110.4(4) . . ?
N2 C9 H9 109.5 . . ?
C8 C9 H9 109.5 . . ?
C4 C9 H9 109.5 . . ?
N2 C10 C11 122.2(4) . . ?
N2 C10 H10 118.9 . . ?
C11 C10 H10 118.9 . . ?
C16 C11 C12 117.1(4) . . ?
C16 C11 C10 120.9(4) . . ?
C12 C11 C10 121.8(4) . . ?
C13 C12 C11 122.1(4) . . ?
C13 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
C12 C13 C14 119.4(4) . . ?
C12 C13 C17 120.4(4) . . ?
C14 C13 C17 120.1(4) . . ?
C15 C14 C13 120.2(4) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C16 C15 C14 119.4(4) . . ?
C16 C15 C24 122.1(4) . 2_665 ?
C14 C15 C24 118.4(4) . 2_665 ?
C15 C16 C11 121.8(4) . . ?
C15 C16 H16 119.1 . . ?
C11 C16 H16 119.1 . . ?
N3 C17 C13 121.8(4) . . ?
N3 C17 H17 119.1 . . ?
C13 C17 H17 119.1 . . ?
N3 C18 C19 109.7(4) . . ?
N3 C18 C23 107.9(4) . . ?
C19 C18 C23 110.6(4) . . ?
N3 C18 H18 109.5 . . ?
C19 C18 H18 109.5 . . ?
C23 C18 H18 109.5 . . ?
C18 C19 C20 111.7(4) . . ?
C18 C19 H19A 109.3 . . ?
C20 C19 H19A 109.3 . . ?
C18 C19 H19B 109.3 . . ?
C20 C19 H19B 109.3 . . ?
H19A C19 H19B 107.9 . . ?
C19 C20 C21 110.6(4) . . ?
C19 C20 H20A 109.5 . . ?
C21 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
C20 C21 C22 110.5(5) . . ?
C20 C21 H21A 109.6 . . ?
C22 C21 H21A 109.6 . . ?
C20 C21 H21B 109.6 . . ?
C22 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
C23 C22 C21 111.1(4) . . ?
C23 C22 H22A 109.4 . . ?
C21 C22 H22A 109.4 . . ?
C23 C22 H22B 109.4 . . ?
C21 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
N4 C23 C22 109.1(4) . . ?
N4 C23 C18 108.9(4) . . ?
C22 C23 C18 109.9(4) . . ?
N4 C23 H23 109.7 . . ?
C22 C23 H23 109.7 . . ?
C18 C23 H23 109.7 . . ?
N4 C24 C15 122.9(4) . 3_565 ?
N4 C24 H24 118.5 . . ?
C15 C24 H24 118.5 3_565 . ?
C26 C25 C26 120.6(4) 2_655 . ?
C26 C25 H25 119.7 2_655 . ?
C26 C25 H25 119.7 . . ?
C25 C26 C25 119.4(4) 3_665 . ?
C25 C26 C27 119.8(4) 3_665 . ?
C25 C26 C27 120.8(4) . . ?
N5 C27 C26 122.7(4) . . ?
N5 C27 H27 118.6 . . ?
C26 C27 H27 118.6 . . ?
N5 C28 C33 108.0(3) . . ?
N5 C28 C29 109.2(4) . . ?
C33 C28 C29 111.0(4) . . ?
N5 C28 H28 109.5 . . ?
C33 C28 H28 109.5 . . ?
C29 C28 H28 109.5 . . ?
C30 C29 C28 111.3(4) . . ?
C30 C29 H29A 109.4 . . ?
C28 C29 H29A 109.4 . . ?
C30 C29 H29B 109.4 . . ?
C28 C29 H29B 109.4 . . ?
H29A C29 H29B 108.0 . . ?
C31 C30 C29 110.2(4) . . ?
C31 C30 H30A 109.6 . . ?
C29 C30 H30A 109.6 . . ?
C31 C30 H30B 109.6 . . ?
C29 C30 H30B 109.6 . . ?
H30A C30 H30B 108.1 . . ?
C32 C31 C30 110.1(4) . . ?
C32 C31 H31A 109.6 . . ?
C30 C31 H31A 109.6 . . ?
C32 C31 H31B 109.6 . . ?
C30 C31 H31B 109.6 . . ?
H31A C31 H31B 108.1 . . ?
C31 C32 C33 112.3(4) . . ?
C31 C32 H32A 109.1 . . ?
C33 C32 H32A 109.1 . . ?
C31 C32 H32B 109.1 . . ?
C33 C32 H32B 109.1 . . ?
H32A C32 H32B 107.9 . . ?
N6 C33 C32 108.6(4) . . ?
N6 C33 C28 109.3(3) . . ?
C32 C33 C28 112.5(4) . . ?
N6 C33 H33 108.8 . . ?
C32 C33 H33 108.8 . . ?
C28 C33 H33 108.8 . . ?
N6 C34 C35 124.4(4) . . ?
N6 C34 H34 117.8 . . ?
C35 C34 H34 117.8 . . ?
C36 C35 C40 118.2(4) . . ?
C36 C35 C34 118.6(4) . . ?
C40 C35 C34 123.2(4) . . ?
C37 C36 C35 121.8(4) . . ?
C37 C36 H36 119.1 . . ?
C35 C36 H36 119.1 . . ?
C38 C37 C36 119.2(4) . . ?
C38 C37 C43 120.2(4) . . ?
C36 C37 C43 120.6(4) . . ?
C37 C38 C39 120.7(4) . . ?
C37 C38 H38 119.6 . . ?
C39 C38 H38 119.6 . . ?
C40 C39 C38 119.1(4) . . ?
C40 C39 C41 119.9(4) . . ?
C38 C39 C41 121.0(4) . . ?
C39 C40 C35 120.9(4) . . ?
C39 C40 H40 119.6 . . ?
C35 C40 H40 119.6 . . ?
N8 C41 C39 122.8(4) . . ?
N8 C41 H41 118.6 . . ?
C39 C41 H41 118.6 . . ?
C72 C42 C68 111.9(4) . . ?
C72 C42 H42A 109.2 . . ?
C68 C42 H42A 109.2 . . ?
C72 C42 H42B 109.2 . . ?
C68 C42 H42B 109.2 . . ?
H42A C42 H42B 107.9 . . ?
N7 C43 C37 120.5(4) . . ?
N7 C43 H43 119.7 . . ?
C37 C43 H43 119.7 . . ?
N7 C44 C45 108.2(4) . . ?
N7 C44 C49 110.0(4) . . ?
C45 C44 C49 110.8(4) . . ?
N7 C44 H44 109.3 . . ?
C45 C44 H44 109.3 . . ?
C49 C44 H44 109.3 . . ?
N8 C45 C44 109.2(4) 2_655 . ?
N8 C45 C46 109.2(4) 2_655 . ?
C44 C45 C46 110.0(4) . . ?
N8 C45 H45 109.5 2_655 . ?
C44 C45 H45 109.5 . . ?
C46 C45 H45 109.5 . . ?
C47 C46 C45 111.6(4) . . ?
C47 C46 H46A 109.3 . . ?
C45 C46 H46A 109.3 . . ?
C47 C46 H46B 109.3 . . ?
C45 C46 H46B 109.3 . . ?
H46A C46 H46B 108.0 . . ?
C48 C47 C46 111.3(5) . . ?
C48 C47 H47A 109.4 . . ?
C46 C47 H47A 109.4 . . ?
C48 C47 H47B 109.4 . . ?
C46 C47 H47B 109.4 . . ?
H47A C47 H47B 108.0 . . ?
C47 C48 C49 110.3(5) . . ?
C47 C48 H48A 109.6 . . ?
C49 C48 H48A 109.6 . . ?
C47 C48 H48B 109.6 . . ?
C49 C48 H48B 109.6 . . ?
H48A C48 H48B 108.1 . . ?
C48 C49 C44 111.6(4) . . ?
C48 C49 H49A 109.3 . . ?
C44 C49 H49A 109.3 . . ?
C48 C49 H49B 109.3 . . ?
C44 C49 H49B 109.3 . . ?
H49A C49 H49B 108.0 . . ?
C51 C50 C51 120.7(5) 2 . ?
C51 C50 H50 119.7 2 . ?
C51 C50 H50 119.7 . . ?
C50 C51 C50 119.3(5) 3 . ?
C50 C51 C52 119.9(4) 3 . ?
C50 C51 C52 120.7(4) . . ?
N10 C52 C51 123.3(4) . . ?
N10 C52 H52 118.4 . . ?
C51 C52 H52 118.4 . . ?
N10 C53 C54 109.3(4) . . ?
N10 C53 C58 109.5(4) . . ?
C54 C53 C58 112.6(4) . . ?
N10 C53 H53 108.4 . . ?
C54 C53 H53 108.4 . . ?
C58 C53 H53 108.4 . . ?
C53 C54 C55 111.2(4) . . ?
C53 C54 H54A 109.4 . . ?
C55 C54 H54A 109.4 . . ?
C53 C54 H54B 109.4 . . ?
C55 C54 H54B 109.4 . . ?
H54A C54 H54B 108.0 . . ?
C54 C55 C56 111.1(4) . . ?
C54 C55 H55A 109.4 . . ?
C56 C55 H55A 109.4 . . ?
C54 C55 H55B 109.4 . . ?
C56 C55 H55B 109.4 . . ?
H55A C55 H55B 108.0 . . ?
C57 C56 C55 109.5(4) . . ?
C57 C56 H56A 109.8 . . ?
C55 C56 H56A 109.8 . . ?
C57 C56 H56B 109.8 . . ?
C55 C56 H56B 109.8 . . ?
H56A C56 H56B 108.2 . . ?
C58 C57 C56 113.1(4) . . ?
C58 C57 H57A 109.0 . . ?
C56 C57 H57A 109.0 . . ?
C58 C57 H57B 109.0 . . ?
C56 C57 H57B 109.0 . . ?
H57A C57 H57B 107.8 . . ?
N9 C58 C57 108.9(4) . . ?
N9 C58 C53 108.3(4) . . ?
C57 C58 C53 110.7(4) . . ?
N9 C58 H58 109.6 . . ?
C57 C58 H58 109.6 . . ?
C53 C58 H58 109.6 . . ?
N9 C59 C60 120.7(4) . . ?
N9 C59 H59 119.7 . . ?
C60 C59 H59 119.7 . . ?
C65 C60 C61 118.6(4) . . ?
C65 C60 C59 121.5(4) . . ?
C61 C60 C59 119.8(4) . . ?
C62 C61 C60 121.0(4) . . ?
C62 C61 H61 119.5 . . ?
C60 C61 H61 119.5 . . ?
C61 C62 C63 119.8(4) . . ?
C61 C62 C66 120.3(4) . . ?
C63 C62 C66 119.7(4) . . ?
C64 C63 C62 119.8(4) . . ?
C64 C63 H63 120.1 . . ?
C62 C63 H63 120.1 . . ?
C65 C64 C63 120.0(4) . . ?
C65 C64 C67 123.1(4) . . ?
C63 C64 C67 116.9(4) . . ?
C64 C65 C60 120.7(4) . . ?
C64 C65 H65 119.7 . . ?
C60 C65 H65 119.7 . . ?
N11 C66 C62 122.1(4) . . ?
N11 C66 H66 119.0 . . ?
C62 C66 H66 119.0 . . ?
N12 C67 C64 123.9(4) . . ?
N12 C67 H67 118.0 . . ?
C64 C67 H67 118.0 . . ?
N12 C68 C42 110.2(4) . . ?
N12 C68 C69 108.7(4) . . ?
C42 C68 C69 110.5(3) . . ?
N12 C68 H68 109.1 . . ?
C42 C68 H68 109.1 . . ?
C69 C68 H68 109.1 . . ?
N11 C69 C70 108.2(4) 2 . ?
N11 C69 C68 109.2(3) 2 . ?
C70 C69 C68 110.8(4) . . ?
N11 C69 H69 109.5 2 . ?
C70 C69 H69 109.5 . . ?
C68 C69 H69 109.5 . . ?
C71 C70 C69 110.6(4) . . ?
C71 C70 H70A 109.5 . . ?
C69 C70 H70A 109.5 . . ?
C71 C70 H70B 109.5 . . ?
C69 C70 H70B 109.5 . . ?
H70A C70 H70B 108.1 . . ?
C72 C71 C70 111.2(4) . . ?
C72 C71 H71A 109.4 . . ?
C70 C71 H71A 109.4 . . ?
C72 C71 H71B 109.4 . . ?
C70 C71 H71B 109.4 . . ?
H71A C71 H71B 108.0 . . ?
C42 C72 C71 110.2(4) . . ?
C42 C72 H72A 109.6 . . ?
C71 C72 H72A 109.6 . . ?
C42 C72 H72B 109.6 . . ?
C71 C72 H72B 109.6 . . ?
H72A C72 H72B 108.1 . . ?
N32 N34 N31 60.1(4) . . ?

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
C2 C1 C2 C1 0.3(9) 3_565 . . 2_665 ?
C2 C1 C2 C3 -178.5(3) 3_565 . . . ?
C4 N1 C3 C2 -176.0(4) . . . . ?
C1 C2 C3 N1 -174.6(4) . . . . ?
C1 C2 C3 N1 6.6(7) 2_665 . . . ?
C3 N1 C4 C5 -119.1(5) . . . . ?
C3 N1 C4 C9 119.7(4) . . . . ?
N1 C4 C5 C6 -172.1(4) . . . . ?
C9 C4 C5 C6 -53.7(6) . . . . ?
C4 C5 C6 C7 56.8(6) . . . . ?
C5 C6 C7 C8 -57.9(6) . . . . ?
C6 C7 C8 C9 58.4(6) . . . . ?
C10 N2 C9 C8 -113.3(5) . . . . ?
C10 N2 C9 C4 126.3(4) . . . . ?
C7 C8 C9 N2 -175.4(4) . . . . ?
C7 C8 C9 C4 -55.6(6) . . . . ?
N1 C4 C9 N2 -68.4(4) . . . . ?
C5 C4 C9 N2 171.7(4) . . . . ?
N1 C4 C9 C8 172.3(4) . . . . ?
C5 C4 C9 C8 52.5(5) . . . . ?
C9 N2 C10 C11 172.9(4) . . . . ?
N2 C10 C11 C16 -168.7(4) . . . . ?
N2 C10 C11 C12 6.1(7) . . . . ?
C16 C11 C12 C13 2.2(6) . . . . ?
C10 C11 C12 C13 -172.8(4) . . . . ?
C11 C12 C13 C14 -1.5(6) . . . . ?
C11 C12 C13 C17 175.3(4) . . . . ?
C12 C13 C14 C15 0.7(6) . . . . ?
C17 C13 C14 C15 -176.0(4) . . . . ?
C13 C14 C15 C16 -0.7(6) . . . . ?
C13 C14 C15 C24 176.6(4) . . . 2_665 ?
C14 C15 C16 C11 1.5(6) . . . . ?
C24 C15 C16 C11 -175.7(4) 2_665 . . . ?
C12 C11 C16 C15 -2.2(6) . . . . ?
C10 C11 C16 C15 172.8(4) . . . . ?
C18 N3 C17 C13 -179.2(4) . . . . ?
C12 C13 C17 N3 -166.0(4) . . . . ?
C14 C13 C17 N3 10.8(6) . . . . ?
C17 N3 C18 C19 -131.8(5) . . . . ?
C17 N3 C18 C23 107.6(5) . . . . ?
N3 C18 C19 C20 -176.9(4) . . . . ?
C23 C18 C19 C20 -57.9(6) . . . . ?
C18 C19 C20 C21 56.2(6) . . . . ?
C19 C20 C21 C22 -54.5(7) . . . . ?
C20 C21 C22 C23 56.1(7) . . . . ?
C24 N4 C23 C22 -120.4(5) . . . . ?
C24 N4 C23 C18 119.7(5) . . . . ?
C21 C22 C23 N4 -176.8(5) . . . . ?
C21 C22 C23 C18 -57.5(6) . . . . ?
N3 C18 C23 N4 -62.3(5) . . . . ?
C19 C18 C23 N4 177.7(4) . . . . ?
N3 C18 C23 C22 178.3(4) . . . . ?
C19 C18 C23 C22 58.3(5) . . . . ?
C23 N4 C24 C15 178.2(4) . . . 3_565 ?
C26 C25 C26 C25 0.7(8) 2_655 . . 3_665 ?
C26 C25 C26 C27 178.5(3) 2_655 . . . ?
C28 N5 C27 C26 -179.1(4) . . . . ?
C25 C26 C27 N5 -177.7(4) 3_665 . . . ?
C25 C26 C27 N5 4.5(7) . . . . ?
C27 N5 C28 C33 119.9(4) . . . . ?
C27 N5 C28 C29 -119.2(4) . . . . ?
N5 C28 C29 C30 -173.2(4) . . . . ?
C33 C28 C29 C30 -54.1(5) . . . . ?
C28 C29 C30 C31 58.8(5) . . . . ?
C29 C30 C31 C32 -59.2(5) . . . . ?
C30 C31 C32 C33 56.2(5) . . . . ?
C34 N6 C33 C32 -109.6(4) . . . . ?
C34 N6 C33 C28 127.3(4) . . . . ?
C31 C32 C33 N6 -173.4(4) . . . . ?
C31 C32 C33 C28 -52.3(5) . . . . ?
N5 C28 C33 N6 -69.0(4) . . . . ?
C29 C28 C33 N6 171.3(3) . . . . ?
N5 C28 C33 C32 170.3(4) . . . . ?
C29 C28 C33 C32 50.6(5) . . . . ?
C33 N6 C34 C35 174.8(4) . . . . ?
N6 C34 C35 C36 -170.5(4) . . . . ?
N6 C34 C35 C40 7.9(7) . . . . ?
C40 C35 C36 C37 -2.7(6) . . . . ?
C34 C35 C36 C37 175.8(4) . . . . ?
C35 C36 C37 C38 3.4(7) . . . . ?
C35 C36 C37 C43 -174.8(4) . . . . ?
C36 C37 C38 C39 -2.7(7) . . . . ?
C43 C37 C38 C39 175.5(4) . . . . ?
C37 C38 C39 C40 1.4(6) . . . . ?
C37 C38 C39 C41 -175.8(4) . . . . ?
C38 C39 C40 C35 -0.7(6) . . . . ?
C41 C39 C40 C35 176.6(4) . . . . ?
C36 C35 C40 C39 1.3(6) . . . . ?
C34 C35 C40 C39 -177.1(4) . . . . ?
C45 N8 C41 C39 -179.2(4) 3_665 . . . ?
C40 C39 C41 N8 -167.4(4) . . . . ?
C38 C39 C41 N8 9.8(7) . . . . ?
C44 N7 C43 C37 -179.5(4) . . . . ?
C38 C37 C43 N7 -167.7(4) . . . . ?
C36 C37 C43 N7 10.5(7) . . . . ?
C43 N7 C44 C45 116.4(5) . . . . ?
C43 N7 C44 C49 -122.4(5) . . . . ?
N7 C44 C45 N8 -64.4(5) . . . 2_655 ?
C49 C44 C45 N8 175.0(4) . . . 2_655 ?
N7 C44 C45 C46 175.8(4) . . . . ?
C49 C44 C45 C46 55.2(5) . . . . ?
N8 C45 C46 C47 -175.9(4) 2_655 . . . ?
C44 C45 C46 C47 -56.1(6) . . . . ?
C45 C46 C47 C48 56.9(7) . . . . ?
C46 C47 C48 C49 -56.4(7) . . . . ?
C47 C48 C49 C44 56.2(7) . . . . ?
N7 C44 C49 C48 -176.0(5) . . . . ?
C45 C44 C49 C48 -56.4(6) . . . . ?
C51 C50 C51 C50 0.8(9) 2 . . 3 ?
C51 C50 C51 C52 178.3(3) 2 . . . ?
C53 N10 C52 C51 179.7(4) . . . . ?
C50 C51 C52 N10 -177.7(4) 3 . . . ?
C50 C51 C52 N10 4.9(7) . . . . ?
C52 N10 C53 C54 -106.7(5) . . . . ?
C52 N10 C53 C58 129.5(4) . . . . ?
N10 C53 C54 C55 -176.4(4) . . . . ?
C58 C53 C54 C55 -54.4(5) . . . . ?
C53 C54 C55 C56 57.2(5) . . . . ?
C54 C55 C56 C57 -57.2(5) . . . . ?
C55 C56 C57 C58 56.0(6) . . . . ?
C59 N9 C58 C57 -114.5(5) . . . . ?
C59 N9 C58 C53 125.0(4) . . . . ?
C56 C57 C58 N9 -172.2(4) . . . . ?
C56 C57 C58 C53 -53.2(5) . . . . ?
N10 C53 C58 N9 -66.9(4) . . . . ?
C54 C53 C58 N9 171.3(4) . . . . ?
N10 C53 C58 C57 173.8(4) . . . . ?
C54 C53 C58 C57 52.0(5) . . . . ?
C58 N9 C59 C60 178.1(4) . . . . ?
N9 C59 C60 C65 -175.6(4) . . . . ?
N9 C59 C60 C61 3.4(7) . . . . ?
C65 C60 C61 C62 0.0(7) . . . . ?
C59 C60 C61 C62 -179.0(4) . . . . ?
C60 C61 C62 C63 -0.5(7) . . . . ?
C60 C61 C62 C66 174.6(4) . . . . ?
C61 C62 C63 C64 0.4(6) . . . . ?
C66 C62 C63 C64 -174.8(4) . . . . ?
C62 C63 C64 C65 0.2(6) . . . . ?
C62 C63 C64 C67 178.5(4) . . . . ?
C63 C64 C65 C60 -0.7(6) . . . . ?
C67 C64 C65 C60 -178.9(4) . . . . ?
C61 C60 C65 C64 0.6(6) . . . . ?
C59 C60 C65 C64 179.5(4) . . . . ?
C69 N11 C66 C62 175.2(4) 3 . . . ?
C61 C62 C66 N11 -169.7(4) . . . . ?
C63 C62 C66 N11 5.4(7) . . . . ?
C68 N12 C67 C64 179.9(4) . . . . ?
C65 C64 C67 N12 4.3(7) . . . . ?
C63 C64 C67 N12 -174.0(4) . . . . ?
C67 N12 C68 C42 -121.0(4) . . . . ?
C67 N12 C68 C69 117.7(4) . . . . ?
C72 C42 C68 N12 -175.5(4) . . . . ?
C72 C42 C68 C69 -55.4(5) . . . . ?
N12 C68 C69 N11 -64.6(4) . . . 2 ?
C42 C68 C69 N11 174.4(4) . . . 2 ?
N12 C68 C69 C70 176.3(3) . . . . ?
C42 C68 C69 C70 55.3(5) . . . . ?
N11 C69 C70 C71 -176.3(4) 2 . . . ?
C68 C69 C70 C71 -56.7(5) . . . . ?
C69 C70 C71 C72 57.9(5) . . . . ?
C68 C42 C72 C71 56.2(5) . . . . ?
C70 C71 C72 C42 -57.1(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        23.29
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.055
_database_code_depnum_ccdc_archive 'CCDC 991215'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Cage3_R_beta_300K

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H84 N12'
_chemical_formula_sum            'C72 H84 N12'
_chemical_formula_weight         1117.51

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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'

_cell_length_a                   25.1483(15)
_cell_length_b                   25.1483(15)
_cell_length_c                   11.0268(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6039.4(6)
_cell_formula_units_Z            3
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    8881
_cell_measurement_theta_min      2.456
_cell_measurement_theta_max      20.367

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.156
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1800
_exptl_absorpt_coefficient_mu    0.055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4973
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  confocal
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            36665
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         0.93
_diffrn_reflns_theta_max         20.92
_reflns_number_total             7893
_reflns_number_gt                6054
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.1 (Rigaku, 2011)'
_computing_cell_refinement       'Bruker AXS SAINT V7.68A'
_computing_data_reduction        'Bruker AXS SAINT V7.68A'
_computing_structure_solution    'SHELXD (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1005P)²+1.7246P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_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   -1(3)
_refine_ls_number_reflns         7893
_refine_ls_number_parameters     757
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0689
_refine_ls_wR_factor_ref         0.1884
_refine_ls_wR_factor_gt          0.1683
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.4969(2) 0.2367(3) 1.3323(4) 0.0735(13) Uani 1 1 d . . .
N2 N 0.4248(2) 0.2035(3) 1.1118(5) 0.0795(15) Uani 1 1 d . . .
N3 N 0.5187(2) 0.1184(2) 0.6447(4) 0.0704(13) Uani 1 1 d . . .
N4 N 0.4992(2) 0.3582(2) 0.6219(5) 0.0685(13) Uani 1 1 d . . .
N5 N 0.3639(3) 0.5367(2) 1.0391(4) 0.0730(14) Uani 1 1 d . . .
N6 N 0.3662(3) 0.4818(3) 0.8111(5) 0.0810(15) Uani 1 1 d . . .
N7 N 0.5078(3) 0.6441(3) 0.3461(5) 0.0851(16) Uani 1 1 d . . .
N8 N 0.2234(3) 0.4526(2) 0.3184(5) 0.0802(15) Uani 1 1 d . . .
N9 N 0.1334(2) 0.1573(2) 0.5614(5) 0.0745(14) Uani 1 1 d . . .
N10 N 0.1991(3) 0.2166(2) 0.3414(6) 0.0840(15) Uani 1 1 d . . .
N11 N 0.2123(3) 0.0809(3) -0.1404(6) 0.0923(17) Uani 1 1 d . . .
N12 N 0.0496(3) 0.2102(3) -0.1242(5) 0.0893(16) Uani 1 1 d . . .
C1 C 0.6467(3) 0.3752(3) 1.3255(5) 0.0642(15) Uani 1 1 d . . .
H1 H 0.6335 0.4038 1.3263 0.077 Uiso 1 1 calc R . .
C2 C 0.6041(3) 0.3141(3) 1.3249(5) 0.0609(14) Uani 1 1 d . . .
C3 C 0.5385(3) 0.2928(3) 1.3239(5) 0.0662(15) Uani 1 1 d . . .
H3 H 0.5263 0.3220 1.3166 0.079 Uiso 1 1 calc R . .
C4 C 0.4323(3) 0.2216(3) 1.3268(5) 0.0746(17) Uani 1 1 d . . .
H4 H 0.4306 0.2587 1.3068 0.090 Uiso 1 1 calc R . .
C5 C 0.4000(3) 0.1741(3) 1.2293(5) 0.0784(18) Uani 1 1 d . . .
H5 H 0.4075 0.1397 1.2409 0.094 Uiso 1 1 calc R . .
C6 C 0.3314(3) 0.1506(4) 1.2272(7) 0.121(3) Uani 1 1 d . . .
H6A H 0.3118 0.1175 1.1688 0.145 Uiso 1 1 calc R . .
H6B H 0.3242 0.1834 1.2021 0.145 Uiso 1 1 calc R . .
C7 C 0.3029(4) 0.1272(5) 1.3537(10) 0.150(4) Uani 1 1 d . . .
H7A H 0.2596 0.1147 1.3519 0.180 Uiso 1 1 calc R . .
H7B H 0.3065 0.0919 1.3758 0.180 Uiso 1 1 calc R . .
C8 C 0.3347(4) 0.1764(6) 1.4443(8) 0.147(4) Uani 1 1 d . . .
H8A H 0.3166 0.1614 1.5235 0.177 Uiso 1 1 calc R . .
H8B H 0.3292 0.2109 1.4238 0.177 Uiso 1 1 calc R . .
C9 C 0.4034(3) 0.1981(4) 1.4497(6) 0.109(3) Uani 1 1 d . . .
H9A H 0.4231 0.2305 1.5095 0.131 Uiso 1 1 calc R . .
H9B H 0.4092 0.1642 1.4740 0.131 Uiso 1 1 calc R . .
C10 C 0.4458(3) 0.1805(3) 1.0396(7) 0.0803(18) Uani 1 1 d . . .
H10 H 0.4464 0.1452 1.0623 0.096 Uiso 1 1 calc R . .
C11 C 0.4699(3) 0.2077(3) 0.9191(5) 0.0703(16) Uani 1 1 d . . .
C12 C 0.4888(3) 0.1787(3) 0.8373(6) 0.0768(18) Uani 1 1 d . . .
H12 H 0.4874 0.1424 0.8601 0.092 Uiso 1 1 calc R . .
C13 C 0.5099(3) 0.2024(3) 0.7216(5) 0.0680(16) Uani 1 1 d . . .
C14 C 0.5121(3) 0.2568(3) 0.6913(5) 0.0696(16) Uani 1 1 d . . .
H14 H 0.5276 0.2744 0.6159 0.084 Uiso 1 1 calc R . .
C15 C 0.4919(3) 0.2860(3) 0.7703(5) 0.0701(16) Uani 1 1 d . . .
C16 C 0.4711(3) 0.2611(3) 0.8832(6) 0.0744(17) Uani 1 1 d . . .
H16 H 0.4576 0.2804 0.9367 0.089 Uiso 1 1 calc R . .
C17 C 0.5276(3) 0.1717(3) 0.6322(5) 0.0679(16) Uani 1 1 d . . .
H17 H 0.5465 0.1929 0.5615 0.082 Uiso 1 1 calc R . .
C18 C 0.5370(3) 0.0934(2) 0.5437(5) 0.0664(16) Uani 1 1 d . . .
H18 H 0.5530 0.1233 0.4774 0.080 Uiso 1 1 calc R . .
C19 C 0.4841(3) 0.0346(3) 0.4989(7) 0.093(2) Uani 1 1 d . . .
H19A H 0.4529 0.0427 0.4668 0.112 Uiso 1 1 calc R . .
H19B H 0.4663 0.0064 0.5664 0.112 Uiso 1 1 calc R . .
C20 C 0.4891(3) 0.3407(3) 0.7294(6) 0.0714(17) Uani 1 1 d . . .
H20 H 0.4796 0.3624 0.7852 0.086 Uiso 1 1 calc R . .
C21 C 0.4943(3) 0.4121(3) 0.5905(5) 0.0639(15) Uani 1 1 d . . .
H21 H 0.4820 0.4265 0.6620 0.077 Uiso 1 1 calc R . .
C22 C 0.4453(3) 0.3927(3) 0.4913(6) 0.0840(19) Uani 1 1 d . . .
H22A H 0.4559 0.3753 0.4233 0.101 Uiso 1 1 calc R . .
H22B H 0.4059 0.3615 0.5227 0.101 Uiso 1 1 calc R . .
C23 C 0.4408(4) 0.4478(4) 0.4488(7) 0.097(2) Uani 1 1 d . . .
H23A H 0.4099 0.4350 0.3858 0.116 Uiso 1 1 calc R . .
H23B H 0.4283 0.4639 0.5160 0.116 Uiso 1 1 calc R . .
C24 C 0.5016(4) 0.4972(4) 0.4004(7) 0.101(2) Uani 1 1 d . . .
H24A H 0.4984 0.5325 0.3759 0.121 Uiso 1 1 calc R . .
H24B H 0.5131 0.4821 0.3299 0.121 Uiso 1 1 calc R . .
C25 C 0.2083(3) 0.0934(3) -0.0331(8) 0.091(2) Uani 1 1 d . . .
H25 H 0.2279 0.0835 0.0268 0.109 Uiso 1 1 calc R . .
C26 C 0.1726(3) 0.1243(3) 0.0023(7) 0.0858(19) Uani 1 1 d . . .
C27 C 0.1333(3) 0.1287(3) -0.0793(6) 0.0860(19) Uani 1 1 d . . .
H27 H 0.1270 0.1100 -0.1549 0.103 Uiso 1 1 calc R . .
C28 C 0.1029(3) 0.1605(3) -0.0506(7) 0.0841(19) Uani 1 1 d . . .
C29 C 0.1100(3) 0.1843(3) 0.0650(7) 0.0881(19) Uani 1 1 d . . .
H29 H 0.0883 0.2037 0.0868 0.106 Uiso 1 1 calc R . .
C30 C 0.1487(3) 0.1800(3) 0.1500(6) 0.0839(19) Uani 1 1 d . . .
C31 C 0.1791(3) 0.1489(3) 0.1153(8) 0.092(2) Uani 1 1 d . . .
H31 H 0.2046 0.1447 0.1710 0.110 Uiso 1 1 calc R . .
C32 C 0.0131(3) 0.2179(3) -0.2177(6) 0.090(2) Uani 1 1 d . . .
H32 H 0.0088 0.1920 -0.2875 0.108 Uiso 1 1 calc R . .
C33 C -0.0501(4) 0.1973(3) -0.1638(7) 0.094(2) Uani 1 1 d . . .
H33 H -0.0453 0.2191 -0.0872 0.113 Uiso 1 1 calc R . .
C34 C -0.0894(4) 0.2114(4) -0.2521(9) 0.129(3) Uani 1 1 d . . .
H34A H -0.0990 0.1856 -0.3234 0.154 Uiso 1 1 calc R . .
H34B H -0.1278 0.2017 -0.2130 0.154 Uiso 1 1 calc R . .
C35 C -0.0562(6) 0.2776(5) -0.2896(11) 0.156(4) Uani 1 1 d . . .
H35A H -0.0813 0.2843 -0.3475 0.187 Uiso 1 1 calc R . .
H35B H -0.0506 0.3030 -0.2191 0.187 Uiso 1 1 calc R . .
C36 C 0.0049(6) 0.2968(5) -0.3452(10) 0.149(4) Uani 1 1 d . . .
H36A H 0.0254 0.3402 -0.3646 0.179 Uiso 1 1 calc R . .
H36B H -0.0006 0.2742 -0.4199 0.179 Uiso 1 1 calc R . .
C37 C 0.0442(4) 0.2844(4) -0.2576(8) 0.126(3) Uani 1 1 d . . .
H37A H 0.0829 0.2951 -0.2964 0.151 Uiso 1 1 calc R . .
H37B H 0.0530 0.3104 -0.1868 0.151 Uiso 1 1 calc R . .
C38 C 0.0663(3) 0.1712(3) -0.1399(6) 0.090(2) Uani 1 1 d . . .
H38 H 0.0549 0.1483 -0.2110 0.108 Uiso 1 1 calc R . .
C39 C 0.1570(4) 0.2094(3) 0.2663(7) 0.0850(19) Uani 1 1 d . . .
H39 H 0.1307 0.2239 0.2878 0.102 Uiso 1 1 calc R . .
C40 C 0.2040(3) 0.2486(3) 0.4527(6) 0.0758(17) Uani 1 1 d . . .
H40 H 0.1716 0.2594 0.4553 0.091 Uiso 1 1 calc R . .
C41 C 0.2669(3) 0.3075(3) 0.4564(7) 0.100(2) Uani 1 1 d . . .
H41A H 0.2693 0.3349 0.3921 0.120 Uiso 1 1 calc R . .
H41B H 0.2990 0.2974 0.4429 0.120 Uiso 1 1 calc R . .
C42 C 0.2773(4) 0.3401(4) 0.5798(10) 0.130(3) Uani 1 1 d . . .
H42A H 0.3175 0.3768 0.5804 0.156 Uiso 1 1 calc R . .
H42B H 0.2468 0.3526 0.5908 0.156 Uiso 1 1 calc R . .
C43 C 0.2730(4) 0.2990(5) 0.6827(8) 0.143(4) Uani 1 1 d . . .
H43A H 0.2792 0.3204 0.7592 0.171 Uiso 1 1 calc R . .
H43B H 0.3047 0.2880 0.6744 0.171 Uiso 1 1 calc R . .
C44 C 0.2102(4) 0.2414(4) 0.6816(7) 0.124(3) Uani 1 1 d . . .
H44A H 0.1790 0.2525 0.6966 0.149 Uiso 1 1 calc R . .
H44B H 0.2081 0.2144 0.7465 0.149 Uiso 1 1 calc R . .
C45 C 0.1968(3) 0.2073(3) 0.5614(6) 0.0765(18) Uani 1 1 d . . .
H45 H 0.2244 0.1906 0.5515 0.092 Uiso 1 1 calc R . .
C46 C 0.1226(3) 0.1027(3) 0.5548(6) 0.0741(17) Uani 1 1 d . . .
H46 H 0.1555 0.0957 0.5494 0.089 Uiso 1 1 calc R . .
C47 C 0.0602(3) 0.0501(3) 0.5554(5) 0.0628(15) Uani 1 1 d . . .
C48 C 0.0497(3) -0.0088(3) 0.5550(6) 0.0693(16) Uani 1 1 d . . .
H48 H 0.0831 -0.0151 0.5544 0.083 Uiso 1 1 calc R . .
C49 C 0.1521(4) 0.3666(4) 0.1902(8) 0.115(3) Uani 1 1 d . . .
H49A H 0.1752 0.3893 0.1194 0.139 Uiso 1 1 calc R . .
H49B H 0.1692 0.3417 0.2182 0.139 Uiso 1 1 calc R . .
C50 C 0.1590(3) 0.4121(3) 0.2905(6) 0.088(2) Uani 1 1 d . . .
H50 H 0.1376 0.3892 0.3636 0.105 Uiso 1 1 calc R . .
C51 C 0.2393(3) 0.4605(3) 0.4290(7) 0.0824(19) Uani 1 1 d . . .
H51 H 0.2097 0.4386 0.4876 0.099 Uiso 1 1 calc R . .
C52 C 0.3029(3) 0.5030(3) 0.4687(6) 0.0728(17) Uani 1 1 d . . .
C53 C 0.4065(3) 0.5798(3) 0.4205(5) 0.0661(16) Uani 1 1 d . . .
C54 C 0.3470(3) 0.5444(3) 0.3881(5) 0.0721(17) Uani 1 1 d . . .
H54 H 0.3351 0.5478 0.3100 0.087 Uiso 1 1 calc R . .
C55 C 0.4241(3) 0.5756(3) 0.5373(5) 0.0678(16) Uani 1 1 d . . .
H55 H 0.4650 0.5996 0.5600 0.081 Uiso 1 1 calc R . .
C56 C 0.3814(3) 0.5357(3) 0.6214(5) 0.0693(16) Uani 1 1 d . . .
C57 C 0.3205(3) 0.4994(3) 0.5855(6) 0.0737(17) Uani 1 1 d . . .
H57 H 0.2914 0.4726 0.6406 0.088 Uiso 1 1 calc R . .
C58 C 0.4512(3) 0.6191(3) 0.3304(6) 0.0742(17) Uani 1 1 d . . .
H58 H 0.4369 0.6260 0.2576 0.089 Uiso 1 1 calc R . .
C59 C 0.5499(3) 0.6804(3) 0.2481(6) 0.0864(19) Uani 1 1 d . . .
H59 H 0.5255 0.6790 0.1775 0.104 Uiso 1 1 calc R . .
C60 C 0.5900(4) 0.6540(4) 0.2124(9) 0.134(3) Uani 1 1 d . . .
H60A H 0.5645 0.6127 0.1812 0.161 Uiso 1 1 calc R . .
H60B H 0.6114 0.6515 0.2834 0.161 Uiso 1 1 calc R . .
C61 C 0.6373(5) 0.6939(5) 0.1148(10) 0.149(4) Uani 1 1 d . . .
H61A H 0.6647 0.6780 0.0992 0.179 Uiso 1 1 calc R . .
H61B H 0.6160 0.6916 0.0399 0.179 Uiso 1 1 calc R . .
C62 C 0.6747(4) 0.7607(5) 0.1551(10) 0.146(4) Uani 1 1 d . . .
H62A H 0.7002 0.7637 0.2238 0.175 Uiso 1 1 calc R . .
H62B H 0.7016 0.7852 0.0896 0.175 Uiso 1 1 calc R . .
C63 C 0.4015(3) 0.5256(3) 0.7415(6) 0.0818(18) Uani 1 1 d . . .
H63 H 0.4415 0.5523 0.7668 0.098 Uiso 1 1 calc R . .
C64 C 0.3918(3) 0.4734(3) 0.9221(5) 0.0767(18) Uani 1 1 d . . .
H64 H 0.4346 0.5060 0.9318 0.092 Uiso 1 1 calc R . .
C65 C 0.3522(3) 0.4741(3) 1.0280(5) 0.0740(17) Uani 1 1 d . . .
H65 H 0.3086 0.4461 1.0106 0.089 Uiso 1 1 calc R . .
C66 C 0.3702(4) 0.4549(3) 1.1459(6) 0.106(3) Uani 1 1 d . . .
H66A H 0.4121 0.4851 1.1667 0.127 Uiso 1 1 calc R . .
H66B H 0.3437 0.4538 1.2110 0.127 Uiso 1 1 calc R . .
C67 C 0.3647(5) 0.3926(4) 1.1333(7) 0.129(3) Uani 1 1 d . . .
H67A H 0.3764 0.3815 1.2091 0.155 Uiso 1 1 calc R . .
H67B H 0.3224 0.3620 1.1162 0.155 Uiso 1 1 calc R . .
C68 C 0.4054(5) 0.3929(4) 1.0329(7) 0.129(3) Uani 1 1 d . . .
H68A H 0.4011 0.3525 1.0252 0.155 Uiso 1 1 calc R . .
H68B H 0.4480 0.4221 1.0514 0.155 Uiso 1 1 calc R . .
C69 C 0.3873(5) 0.4104(4) 0.9153(6) 0.112(3) Uani 1 1 d . . .
H69A H 0.3455 0.3796 0.8953 0.135 Uiso 1 1 calc R . .
H69B H 0.4138 0.4109 0.8509 0.135 Uiso 1 1 calc R . .
C70 C 0.3196(3) 0.5467(3) 1.0268(5) 0.0711(16) Uani 1 1 d . . .
H70 H 0.2804 0.5133 1.0155 0.085 Uiso 1 1 calc R . .
C71 C 0.3267(3) 0.6083(3) 1.0294(5) 0.0638(15) Uani 1 1 d . . .
C72 C 0.2760(3) 0.6148(3) 1.0310(5) 0.0695(16) Uani 1 1 d . . .
H72 H 0.2372 0.5800 1.0332 0.083 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
N1 C3 1.271(7) . ?
N1 C4 1.472(7) . ?
N2 C10 1.246(7) . ?
N2 C5 1.467(7) . ?
N3 C17 1.254(7) . ?
N3 C18 1.462(7) . ?
N4 C20 1.246(7) . ?
N4 C21 1.461(7) . ?
N5 C70 1.268(7) . ?
N5 C65 1.456(8) . ?
N6 C63 1.269(8) . ?
N6 C64 1.447(7) . ?
N7 C58 1.249(8) . ?
N7 C59 1.469(8) . ?
N8 C51 1.268(8) . ?
N8 C50 1.452(8) . ?
N9 C46 1.261(7) . ?
N9 C45 1.457(7) . ?
N10 C39 1.285(8) . ?
N10 C40 1.439(8) . ?
N11 C25 1.241(8) . ?
N11 C33 1.459(9) 3 ?
N12 C38 1.255(8) . ?
N12 C32 1.458(8) . ?
C1 C2 1.364(8) . ?
C1 C2 1.407(7) 3_665 ?
C1 H1 0.9300 . ?
C2 C1 1.407(7) 2_655 ?
C2 C3 1.458(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.508(9) . ?
C4 C9 1.513(9) . ?
C4 H4 0.9800 . ?
C5 C6 1.521(9) . ?
C5 H5 0.9800 . ?
C6 C7 1.544(11) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.476(14) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.530(10) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.479(9) . ?
C10 H10 0.9300 . ?
C11 C16 1.385(8) . ?
C11 C12 1.385(8) . ?
C12 C13 1.395(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.383(8) . ?
C13 C17 1.451(8) . ?
C14 C15 1.389(8) . ?
C14 H14 0.9300 . ?
C15 C16 1.374(8) . ?
C15 C20 1.483(8) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.493(8) . ?
C18 C21 1.530(8) 2_655 ?
C18 H18 0.9800 . ?
C19 C24 1.528(9) 2_655 ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20 0.9300 . ?
C21 C18 1.530(8) 3_665 ?
C21 C22 1.534(8) . ?
C21 H21 0.9800 . ?
C22 C23 1.518(9) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.506(10) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C19 1.528(10) 3_665 ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.502(10) . ?
C25 H25 0.9300 . ?
C26 C31 1.364(9) . ?
C26 C27 1.383(9) . ?
C27 C28 1.392(9) . ?
C27 H27 0.9300 . ?
C28 C29 1.381(9) . ?
C28 C38 1.463(9) . ?
C29 C30 1.393(9) . ?
C29 H29 0.9300 . ?
C30 C31 1.393(9) . ?
C30 C39 1.443(9) . ?
C31 H31 0.9300 . ?
C32 C37 1.513(10) . ?
C32 C33 1.524(10) . ?
C32 H32 0.9800 . ?
C33 N11 1.459(9) 2 ?
C33 C34 1.548(10) . ?
C33 H33 0.9800 . ?
C34 C35 1.500(13) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.494(14) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C37 1.520(11) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 C41 1.535(9) . ?
C40 C45 1.537(9) . ?
C40 H40 0.9800 . ?
C41 C42 1.542(11) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.503(13) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.518(10) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 C45 1.522(9) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 H45 0.9800 . ?
C46 C47 1.462(8) . ?
C46 H46 0.9300 . ?
C47 C48 1.367(7) . ?
C47 C48 1.410(7) 2 ?
C48 C47 1.410(7) 3 ?
C48 H48 0.9300 . ?
C49 C62 1.505(11) 3_565 ?
C49 C50 1.539(9) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C50 C59 1.525(9) 3_565 ?
C50 H50 0.9800 . ?
C51 C52 1.477(9) . ?
C51 H51 0.9300 . ?
C52 C57 1.379(8) . ?
C52 C54 1.396(8) . ?
C53 C54 1.353(8) . ?
C53 C55 1.383(8) . ?
C53 C58 1.455(9) . ?
C54 H54 0.9300 . ?
C55 C56 1.394(8) . ?
C55 H55 0.9300 . ?
C56 C57 1.393(8) . ?
C56 C63 1.484(9) . ?
C57 H57 0.9300 . ?
C58 H58 0.9300 . ?
C59 C60 1.512(10) . ?
C59 C50 1.525(9) 2_665 ?
C59 H59 0.9800 . ?
C60 C61 1.544(11) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C61 C62 1.525(13) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C62 C49 1.505(11) 2_665 ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C63 H63 0.9300 . ?
C64 C69 1.531(9) . ?
C64 C65 1.541(8) . ?
C64 H64 0.9800 . ?
C65 C66 1.530(8) . ?
C65 H65 0.9800 . ?
C66 C67 1.511(10) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C67 C68 1.505(11) . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C68 C69 1.511(10) . ?
C68 H68A 0.9700 . ?
C68 H68B 0.9700 . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C70 C71 1.467(8) . ?
C70 H70 0.9300 . ?
C71 C72 1.364(8) . ?
C71 C72 1.406(8) 2_665 ?
C72 C71 1.407(8) 3_565 ?
C72 H72 0.9300 . ?

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
C3 N1 C4 118.2(5) . . ?
C10 N2 C5 120.1(6) . . ?
C17 N3 C18 116.8(5) . . ?
C20 N4 C21 117.2(5) . . ?
C70 N5 C65 119.0(5) . . ?
C63 N6 C64 118.0(6) . . ?
C58 N7 C59 119.7(6) . . ?
C51 N8 C50 117.8(6) . . ?
C46 N9 C45 119.1(5) . . ?
C39 N10 C40 117.4(6) . . ?
C25 N11 C33 116.7(6) . 3 ?
C38 N12 C32 119.1(6) . . ?
C2 C1 C2 121.4(6) . 3_665 ?
C2 C1 H1 119.3 . . ?
C2 C1 H1 119.3 3_665 . ?
C1 C2 C1 118.6(6) . 2_655 ?
C1 C2 C3 121.3(6) . . ?
C1 C2 C3 120.1(6) 2_655 . ?
N1 C3 C2 124.0(5) . . ?
N1 C3 H3 118.0 . . ?
C2 C3 H3 118.0 . . ?
N1 C4 C5 108.7(5) . . ?
N1 C4 C9 108.5(5) . . ?
C5 C4 C9 111.5(6) . . ?
N1 C4 H4 109.4 . . ?
C5 C4 H4 109.4 . . ?
C9 C4 H4 109.4 . . ?
N2 C5 C4 107.8(5) . . ?
N2 C5 C6 107.2(5) . . ?
C4 C5 C6 112.0(6) . . ?
N2 C5 H5 109.9 . . ?
C4 C5 H5 109.9 . . ?
C6 C5 H5 109.9 . . ?
C5 C6 C7 110.8(6) . . ?
C5 C6 H6A 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C8 C7 C6 109.8(8) . . ?
C8 C7 H7A 109.7 . . ?
C6 C7 H7A 109.7 . . ?
C8 C7 H7B 109.7 . . ?
C6 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
C7 C8 C9 111.6(8) . . ?
C7 C8 H8A 109.3 . . ?
C9 C8 H8A 109.3 . . ?
C7 C8 H8B 109.3 . . ?
C9 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
C4 C9 C8 109.9(6) . . ?
C4 C9 H9A 109.7 . . ?
C8 C9 H9A 109.7 . . ?
C4 C9 H9B 109.7 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N2 C10 C11 122.0(6) . . ?
N2 C10 H10 119.0 . . ?
C11 C10 H10 119.0 . . ?
C16 C11 C12 118.5(6) . . ?
C16 C11 C10 120.7(6) . . ?
C12 C11 C10 120.7(6) . . ?
C11 C12 C13 121.8(6) . . ?
C11 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
C14 C13 C12 117.6(5) . . ?
C14 C13 C17 119.3(5) . . ?
C12 C13 C17 123.1(6) . . ?
C13 C14 C15 121.8(6) . . ?
C13 C14 H14 119.1 . . ?
C15 C14 H14 119.1 . . ?
C16 C15 C14 118.9(5) . . ?
C16 C15 C20 121.1(6) . . ?
C14 C15 C20 119.9(6) . . ?
C15 C16 C11 121.4(5) . . ?
C15 C16 H16 119.3 . . ?
C11 C16 H16 119.3 . . ?
N3 C17 C13 123.8(6) . . ?
N3 C17 H17 118.1 . . ?
C13 C17 H17 118.1 . . ?
N3 C18 C19 111.2(5) . . ?
N3 C18 C21 107.0(5) . 2_655 ?
C19 C18 C21 110.1(5) . 2_655 ?
N3 C18 H18 109.5 . . ?
C19 C18 H18 109.5 . . ?
C21 C18 H18 109.5 2_655 . ?
C18 C19 C24 112.6(6) . 2_655 ?
C18 C19 H19A 109.1 . . ?
C24 C19 H19A 109.1 2_655 . ?
C18 C19 H19B 109.1 . . ?
C24 C19 H19B 109.1 2_655 . ?
H19A C19 H19B 107.8 . . ?
N4 C20 C15 121.5(5) . . ?
N4 C20 H20 119.3 . . ?
C15 C20 H20 119.3 . . ?
N4 C21 C18 109.4(4) . 3_665 ?
N4 C21 C22 107.5(5) . . ?
C18 C21 C22 110.2(5) 3_665 . ?
N4 C21 H21 109.9 . . ?
C18 C21 H21 109.9 3_665 . ?
C22 C21 H21 109.9 . . ?
C23 C22 C21 110.2(5) . . ?
C23 C22 H22A 109.6 . . ?
C21 C22 H22A 109.6 . . ?
C23 C22 H22B 109.6 . . ?
C21 C22 H22B 109.6 . . ?
H22A C22 H22B 108.1 . . ?
C24 C23 C22 110.7(6) . . ?
C24 C23 H23A 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 108.1 . . ?
C23 C24 C19 109.3(6) . 3_665 ?
C23 C24 H24A 109.8 . . ?
C19 C24 H24A 109.8 3_665 . ?
C23 C24 H24B 109.8 . . ?
C19 C24 H24B 109.8 3_665 . ?
H24A C24 H24B 108.3 . . ?
N11 C25 C26 121.5(7) . . ?
N11 C25 H25 119.2 . . ?
C26 C25 H25 119.2 . . ?
C31 C26 C27 119.1(7) . . ?
C31 C26 C25 120.3(7) . . ?
C27 C26 C25 120.6(7) . . ?
C26 C27 C28 121.2(7) . . ?
C26 C27 H27 119.4 . . ?
C28 C27 H27 119.4 . . ?
C29 C28 C27 118.0(6) . . ?
C29 C28 C38 119.9(7) . . ?
C27 C28 C38 122.0(7) . . ?
C28 C29 C30 122.2(7) . . ?
C28 C29 H29 118.9 . . ?
C30 C29 H29 118.9 . . ?
C29 C30 C31 117.3(6) . . ?
C29 C30 C39 119.1(7) . . ?
C31 C30 C39 123.6(7) . . ?
C26 C31 C30 122.1(6) . . ?
C26 C31 H31 118.9 . . ?
C30 C31 H31 118.9 . . ?
N12 C32 C37 109.9(6) . . ?
N12 C32 C33 107.4(6) . . ?
C37 C32 C33 111.4(6) . . ?
N12 C32 H32 109.4 . . ?
C37 C32 H32 109.4 . . ?
C33 C32 H32 109.4 . . ?
N11 C33 C32 109.0(6) 2 . ?
N11 C33 C34 109.5(6) 2 . ?
C32 C33 C34 110.6(7) . . ?
N11 C33 H33 109.2 2 . ?
C32 C33 H33 109.2 . . ?
C34 C33 H33 109.2 . . ?
C35 C34 C33 111.3(7) . . ?
C35 C34 H34A 109.4 . . ?
C33 C34 H34A 109.4 . . ?
C35 C34 H34B 109.4 . . ?
C33 C34 H34B 109.4 . . ?
H34A C34 H34B 108.0 . . ?
C36 C35 C34 112.5(8) . . ?
C36 C35 H35A 109.1 . . ?
C34 C35 H35A 109.1 . . ?
C36 C35 H35B 109.1 . . ?
C34 C35 H35B 109.1 . . ?
H35A C35 H35B 107.8 . . ?
C35 C36 C37 110.0(8) . . ?
C35 C36 H36A 109.7 . . ?
C37 C36 H36A 109.7 . . ?
C35 C36 H36B 109.7 . . ?
C37 C36 H36B 109.7 . . ?
H36A C36 H36B 108.2 . . ?
C32 C37 C36 112.4(8) . . ?
C32 C37 H37A 109.1 . . ?
C36 C37 H37A 109.1 . . ?
C32 C37 H37B 109.1 . . ?
C36 C37 H37B 109.1 . . ?
H37A C37 H37B 107.9 . . ?
N12 C38 C28 122.5(7) . . ?
N12 C38 H38 118.7 . . ?
C28 C38 H38 118.7 . . ?
N10 C39 C30 122.9(7) . . ?
N10 C39 H39 118.6 . . ?
C30 C39 H39 118.6 . . ?
N10 C40 C41 108.8(6) . . ?
N10 C40 C45 109.7(5) . . ?
C41 C40 C45 110.3(5) . . ?
N10 C40 H40 109.3 . . ?
C41 C40 H40 109.3 . . ?
C45 C40 H40 109.3 . . ?
C40 C41 C42 110.8(6) . . ?
C40 C41 H41A 109.5 . . ?
C42 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 108.1 . . ?
C43 C42 C41 111.4(7) . . ?
C43 C42 H42A 109.3 . . ?
C41 C42 H42A 109.3 . . ?
C43 C42 H42B 109.3 . . ?
C41 C42 H42B 109.3 . . ?
H42A C42 H42B 108.0 . . ?
C42 C43 C44 109.4(8) . . ?
C42 C43 H43A 109.8 . . ?
C44 C43 H43A 109.8 . . ?
C42 C43 H43B 109.8 . . ?
C44 C43 H43B 109.8 . . ?
H43A C43 H43B 108.2 . . ?
C43 C44 C45 112.1(6) . . ?
C43 C44 H44A 109.2 . . ?
C45 C44 H44A 109.2 . . ?
C43 C44 H44B 109.2 . . ?
C45 C44 H44B 109.2 . . ?
H44A C44 H44B 107.9 . . ?
N9 C45 C44 109.0(5) . . ?
N9 C45 C40 106.9(5) . . ?
C44 C45 C40 112.3(6) . . ?
N9 C45 H45 109.5 . . ?
C44 C45 H45 109.5 . . ?
C40 C45 H45 109.5 . . ?
N9 C46 C47 122.2(6) . . ?
N9 C46 H46 118.9 . . ?
C47 C46 H46 118.9 . . ?
C48 C47 C48 117.8(6) . 2 ?
C48 C47 C46 121.2(6) . . ?
C48 C47 C46 121.0(6) 2 . ?
C47 C48 C47 122.2(6) . 3 ?
C47 C48 H48 118.9 . . ?
C47 C48 H48 118.9 3 . ?
C62 C49 C50 111.9(7) 3_565 . ?
C62 C49 H49A 109.2 3_565 . ?
C50 C49 H49A 109.2 . . ?
C62 C49 H49B 109.2 3_565 . ?
C50 C49 H49B 109.2 . . ?
H49A C49 H49B 107.9 . . ?
N8 C50 C59 109.5(5) . 3_565 ?
N8 C50 C49 110.2(6) . . ?
C59 C50 C49 109.4(6) 3_565 . ?
N8 C50 H50 109.2 . . ?
C59 C50 H50 109.2 3_565 . ?
C49 C50 H50 109.2 . . ?
N8 C51 C52 122.7(6) . . ?
N8 C51 H51 118.6 . . ?
C52 C51 H51 118.6 . . ?
C57 C52 C54 118.9(6) . . ?
C57 C52 C51 119.7(6) . . ?
C54 C52 C51 121.3(6) . . ?
C54 C53 C55 119.1(5) . . ?
C54 C53 C58 119.4(6) . . ?
C55 C53 C58 121.4(6) . . ?
C53 C54 C52 121.9(6) . . ?
C53 C54 H54 119.1 . . ?
C52 C54 H54 119.1 . . ?
C53 C55 C56 121.0(6) . . ?
C53 C55 H55 119.5 . . ?
C56 C55 H55 119.5 . . ?
C57 C56 C55 118.8(5) . . ?
C57 C56 C63 119.9(6) . . ?
C55 C56 C63 120.8(6) . . ?
C52 C57 C56 120.4(6) . . ?
C52 C57 H57 119.8 . . ?
C56 C57 H57 119.8 . . ?
N7 C58 C53 123.1(6) . . ?
N7 C58 H58 118.5 . . ?
C53 C58 H58 118.5 . . ?
N7 C59 C60 110.4(6) . . ?
N7 C59 C50 108.5(5) . 2_665 ?
C60 C59 C50 111.8(6) . 2_665 ?
N7 C59 H59 108.7 . . ?
C60 C59 H59 108.7 . . ?
C50 C59 H59 108.7 2_665 . ?
C59 C60 C61 111.2(7) . . ?
C59 C60 H60A 109.4 . . ?
C61 C60 H60A 109.4 . . ?
C59 C60 H60B 109.4 . . ?
C61 C60 H60B 109.4 . . ?
H60A C60 H60B 108.0 . . ?
C62 C61 C60 111.3(8) . . ?
C62 C61 H61A 109.4 . . ?
C60 C61 H61A 109.4 . . ?
C62 C61 H61B 109.4 . . ?
C60 C61 H61B 109.4 . . ?
H61A C61 H61B 108.0 . . ?
C49 C62 C61 111.0(8) 2_665 . ?
C49 C62 H62A 109.4 2_665 . ?
C61 C62 H62A 109.4 . . ?
C49 C62 H62B 109.4 2_665 . ?
C61 C62 H62B 109.4 . . ?
H62A C62 H62B 108.0 . . ?
N6 C63 C56 122.5(6) . . ?
N6 C63 H63 118.7 . . ?
C56 C63 H63 118.7 . . ?
N6 C64 C69 107.6(5) . . ?
N6 C64 C65 107.6(5) . . ?
C69 C64 C65 109.5(5) . . ?
N6 C64 H64 110.7 . . ?
C69 C64 H64 110.7 . . ?
C65 C64 H64 110.7 . . ?
N5 C65 C66 109.7(5) . . ?
N5 C65 C64 107.1(5) . . ?
C66 C65 C64 110.3(5) . . ?
N5 C65 H65 109.9 . . ?
C66 C65 H65 109.9 . . ?
C64 C65 H65 109.9 . . ?
C67 C66 C65 111.1(6) . . ?
C67 C66 H66A 109.4 . . ?
C65 C66 H66A 109.4 . . ?
C67 C66 H66B 109.4 . . ?
C65 C66 H66B 109.4 . . ?
H66A C66 H66B 108.0 . . ?
C68 C67 C66 110.7(7) . . ?
C68 C67 H67A 109.5 . . ?
C66 C67 H67A 109.5 . . ?
C68 C67 H67B 109.5 . . ?
C66 C67 H67B 109.5 . . ?
H67A C67 H67B 108.1 . . ?
C67 C68 C69 109.3(7) . . ?
C67 C68 H68A 109.8 . . ?
C69 C68 H68A 109.8 . . ?
C67 C68 H68B 109.8 . . ?
C69 C68 H68B 109.8 . . ?
H68A C68 H68B 108.3 . . ?
C68 C69 C64 112.5(6) . . ?
C68 C69 H69A 109.1 . . ?
C64 C69 H69A 109.1 . . ?
C68 C69 H69B 109.1 . . ?
C64 C69 H69B 109.1 . . ?
H69A C69 H69B 107.8 . . ?
N5 C70 C71 123.6(6) . . ?
N5 C70 H70 118.2 . . ?
C71 C70 H70 118.2 . . ?
C72 C71 C72 119.0(6) . 2_665 ?
C72 C71 C70 119.9(6) . . ?
C72 C71 C70 121.1(6) 2_665 . ?
C71 C72 C71 120.9(6) . 3_565 ?
C71 C72 H72 119.5 . . ?
C71 C72 H72 119.5 3_565 . ?

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
C2 C1 C2 C1 0.9(10) 3_665 . . 2_655 ?
C2 C1 C2 C3 -179.2(4) 3_665 . . . ?
C4 N1 C3 C2 -178.4(5) . . . . ?
C1 C2 C3 N1 -174.6(5) . . . . ?
C1 C2 C3 N1 5.3(8) 2_655 . . . ?
C3 N1 C4 C5 126.3(6) . . . . ?
C3 N1 C4 C9 -112.4(7) . . . . ?
C10 N2 C5 C4 126.1(6) . . . . ?
C10 N2 C5 C6 -113.2(7) . . . . ?
N1 C4 C5 N2 -68.7(6) . . . . ?
C9 C4 C5 N2 171.7(5) . . . . ?
N1 C4 C5 C6 173.6(6) . . . . ?
C9 C4 C5 C6 54.0(8) . . . . ?
N2 C5 C6 C7 -171.8(8) . . . . ?
C4 C5 C6 C7 -53.8(10) . . . . ?
C5 C6 C7 C8 56.1(11) . . . . ?
C6 C7 C8 C9 -59.0(11) . . . . ?
N1 C4 C9 C8 -174.9(8) . . . . ?
C5 C4 C9 C8 -55.2(10) . . . . ?
C7 C8 C9 C4 59.0(11) . . . . ?
C5 N2 C10 C11 178.4(5) . . . . ?
N2 C10 C11 C16 1.6(10) . . . . ?
N2 C10 C11 C12 -175.3(6) . . . . ?
C16 C11 C12 C13 1.1(9) . . . . ?
C10 C11 C12 C13 178.0(6) . . . . ?
C11 C12 C13 C14 0.9(9) . . . . ?
C11 C12 C13 C17 -177.3(6) . . . . ?
C12 C13 C14 C15 -2.6(9) . . . . ?
C17 C13 C14 C15 175.6(5) . . . . ?
C13 C14 C15 C16 2.3(9) . . . . ?
C13 C14 C15 C20 -173.7(6) . . . . ?
C14 C15 C16 C11 -0.2(9) . . . . ?
C20 C15 C16 C11 175.7(6) . . . . ?
C12 C11 C16 C15 -1.4(9) . . . . ?
C10 C11 C16 C15 -178.3(6) . . . . ?
C18 N3 C17 C13 177.5(5) . . . . ?
C14 C13 C17 N3 -169.2(6) . . . . ?
C12 C13 C17 N3 8.9(9) . . . . ?
C17 N3 C18 C19 -123.0(6) . . . . ?
C17 N3 C18 C21 116.8(5) . . . 2_655 ?
N3 C18 C19 C24 -175.2(6) . . . 2_655 ?
C21 C18 C19 C24 -56.7(7) 2_655 . . 2_655 ?
C21 N4 C20 C15 179.0(5) . . . . ?
C16 C15 C20 N4 -169.3(6) . . . . ?
C14 C15 C20 N4 6.7(9) . . . . ?
C20 N4 C21 C18 119.0(6) . . . 3_665 ?
C20 N4 C21 C22 -121.2(6) . . . . ?
N4 C21 C22 C23 -176.4(6) . . . . ?
C18 C21 C22 C23 -57.3(7) 3_665 . . . ?
C21 C22 C23 C24 58.8(8) . . . . ?
C22 C23 C24 C19 -57.7(8) . . . 3_665 ?
C33 N11 C25 C26 -179.2(6) 3 . . . ?
N11 C25 C26 C31 -166.5(7) . . . . ?
N11 C25 C26 C27 12.9(10) . . . . ?
C31 C26 C27 C28 3.6(10) . . . . ?
C25 C26 C27 C28 -175.8(6) . . . . ?
C26 C27 C28 C29 -4.2(10) . . . . ?
C26 C27 C28 C38 173.4(6) . . . . ?
C27 C28 C29 C30 3.4(10) . . . . ?
C38 C28 C29 C30 -174.3(7) . . . . ?
C28 C29 C30 C31 -1.9(10) . . . . ?
C28 C29 C30 C39 175.9(6) . . . . ?
C27 C26 C31 C30 -2.0(10) . . . . ?
C25 C26 C31 C30 177.4(6) . . . . ?
C29 C30 C31 C26 1.2(10) . . . . ?
C39 C30 C31 C26 -176.5(7) . . . . ?
C38 N12 C32 C37 -124.6(8) . . . . ?
C38 N12 C32 C33 114.1(7) . . . . ?
N12 C32 C33 N11 -66.3(7) . . . 2 ?
C37 C32 C33 N11 173.3(6) . . . 2 ?
N12 C32 C33 C34 173.2(6) . . . . ?
C37 C32 C33 C34 52.8(8) . . . . ?
N11 C33 C34 C35 -173.6(8) 2 . . . ?
C32 C33 C34 C35 -53.4(10) . . . . ?
C33 C34 C35 C36 56.3(12) . . . . ?
C34 C35 C36 C37 -56.7(12) . . . . ?
N12 C32 C37 C36 -173.8(8) . . . . ?
C33 C32 C37 C36 -55.0(10) . . . . ?
C35 C36 C37 C32 55.9(12) . . . . ?
C32 N12 C38 C28 -179.9(6) . . . . ?
C29 C28 C38 N12 13.2(10) . . . . ?
C27 C28 C38 N12 -164.5(7) . . . . ?
C40 N10 C39 C30 177.9(6) . . . . ?
C29 C30 C39 N10 -168.0(7) . . . . ?
C31 C30 C39 N10 9.6(11) . . . . ?
C39 N10 C40 C41 -117.2(6) . . . . ?
C39 N10 C40 C45 122.1(6) . . . . ?
N10 C40 C41 C42 -173.9(7) . . . . ?
C45 C40 C41 C42 -53.5(8) . . . . ?
C40 C41 C42 C43 58.2(9) . . . . ?
C41 C42 C43 C44 -58.8(10) . . . . ?
C42 C43 C44 C45 57.0(11) . . . . ?
C46 N9 C45 C44 -116.7(7) . . . . ?
C46 N9 C45 C40 121.6(6) . . . . ?
C43 C44 C45 N9 -173.0(8) . . . . ?
C43 C44 C45 C40 -54.6(10) . . . . ?
N10 C40 C45 N9 -68.3(6) . . . . ?
C41 C40 C45 N9 171.8(5) . . . . ?
N10 C40 C45 C44 172.1(6) . . . . ?
C41 C40 C45 C44 52.3(8) . . . . ?
C45 N9 C46 C47 179.4(5) . . . . ?
N9 C46 C47 C48 -176.3(6) . . . . ?
N9 C46 C47 C48 4.4(9) . . . 2 ?
C48 C47 C48 C47 -0.6(12) 2 . . 3 ?
C46 C47 C48 C47 -179.9(4) . . . 3 ?
C51 N8 C50 C59 107.6(7) . . . 3_565 ?
C51 N8 C50 C49 -132.1(6) . . . . ?
C62 C49 C50 N8 -177.8(7) 3_565 . . . ?
C62 C49 C50 C59 -57.4(9) 3_565 . . 3_565 ?
C50 N8 C51 C52 -176.8(6) . . . . ?
N8 C51 C52 C57 -165.3(6) . . . . ?
N8 C51 C52 C54 10.7(9) . . . . ?
C55 C53 C54 C52 -1.0(9) . . . . ?
C58 C53 C54 C52 175.8(5) . . . . ?
C57 C52 C54 C53 1.8(9) . . . . ?
C51 C52 C54 C53 -174.2(6) . . . . ?
C54 C53 C55 C56 -0.3(8) . . . . ?
C58 C53 C55 C56 -177.0(5) . . . . ?
C53 C55 C56 C57 0.7(8) . . . . ?
C53 C55 C56 C63 172.5(5) . . . . ?
C54 C52 C57 C56 -1.3(9) . . . . ?
C51 C52 C57 C56 174.8(5) . . . . ?
C55 C56 C57 C52 0.1(9) . . . . ?
C63 C56 C57 C52 -171.7(5) . . . . ?
C59 N7 C58 C53 176.7(5) . . . . ?
C54 C53 C58 N7 -166.2(6) . . . . ?
C55 C53 C58 N7 10.5(9) . . . . ?
C58 N7 C59 C60 -120.6(8) . . . . ?
C58 N7 C59 C50 116.6(7) . . . 2_665 ?
N7 C59 C60 C61 -176.5(8) . . . . ?
C50 C59 C60 C61 -55.6(10) 2_665 . . . ?
C59 C60 C61 C62 53.9(12) . . . . ?
C60 C61 C62 C49 -54.4(12) . . . 2_665 ?
C64 N6 C63 C56 175.4(5) . . . . ?
C57 C56 C63 N6 5.2(9) . . . . ?
C55 C56 C63 N6 -166.5(6) . . . . ?
C63 N6 C64 C69 -117.1(7) . . . . ?
C63 N6 C64 C65 125.0(6) . . . . ?
C70 N5 C65 C66 -120.5(6) . . . . ?
C70 N5 C65 C64 119.9(6) . . . . ?
N6 C64 C65 N5 -69.9(6) . . . . ?
C69 C64 C65 N5 173.4(5) . . . . ?
N6 C64 C65 C66 170.8(6) . . . . ?
C69 C64 C65 C66 54.1(7) . . . . ?
N5 C65 C66 C67 -174.3(7) . . . . ?
C64 C65 C66 C67 -56.6(9) . . . . ?
C65 C66 C67 C68 59.2(10) . . . . ?
C66 C67 C68 C69 -58.8(10) . . . . ?
C67 C68 C69 C64 58.4(10) . . . . ?
N6 C64 C69 C68 -172.9(7) . . . . ?
C65 C64 C69 C68 -56.2(9) . . . . ?
C65 N5 C70 C71 -176.5(5) . . . . ?
N5 C70 C71 C72 -171.7(5) . . . . ?
N5 C70 C71 C72 8.0(8) . . . 2_665 ?
C72 C71 C72 C71 2.5(11) 2_665 . . 3_565 ?
C70 C71 C72 C71 -177.8(4) . . . 3_565 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        20.92
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.047
_database_code_depnum_ccdc_archive 'CCDC 991216'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Cage3_R_beta_400K

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H84 N12'
_chemical_formula_sum            'C72 H84 N12'
_chemical_formula_weight         1117.51

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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'

_cell_length_a                   25.2084(15)
_cell_length_b                   25.2084(15)
_cell_length_c                   11.0674(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6090.7(6)
_cell_formula_units_Z            3
_cell_measurement_temperature    400(2)
_cell_measurement_reflns_used    7684
_cell_measurement_theta_min      2.448
_cell_measurement_theta_max      19.414

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.156
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.914
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1800
_exptl_absorpt_coefficient_mu    0.055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5739
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      400(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  confocal
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            37467
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         20.81
_reflns_number_total             7895
_reflns_number_gt                5267
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.1 (Rigaku, 2011)'
_computing_cell_refinement       'Bruker AXS SAINT V7.68A'
_computing_data_reduction        'Bruker AXS SAINT V7.68A'
_computing_structure_solution    'SHELXD (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0953P)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    constr
_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   -3(3)
_refine_ls_number_reflns         7895
_refine_ls_number_parameters     757
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_ref         0.1637
_refine_ls_wR_factor_gt          0.1383
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N5 N 0.53286(18) 0.3558(2) 0.5333(4) 0.0982(13) Uani 1 1 d . . .
C4 C 0.4696(2) 0.3422(3) 0.5349(5) 0.0989(16) Uani 1 1 d . . .
H4 H 0.4416 0.2973 0.5467 0.119 Uiso 1 1 calc R . .
C2 C 0.6068(2) 0.3234(3) 0.5407(5) 0.0839(14) Uani 1 1 d . . .
N8 N 0.1669(2) 0.19197(18) 0.4738(4) 0.0940(12) Uani 1 1 d . . .
N4 N 0.4679(2) 0.3506(2) 0.7531(5) 0.1105(14) Uani 1 1 d . . .
C64 C 0.1944(3) 0.1234(3) 0.2135(5) 0.1006(16) Uani 1 1 d . . .
H64 H 0.2079 0.1567 0.1588 0.121 Uiso 1 1 calc R . .
C27 C 0.3199(3) 0.5303(3) 0.7072(5) 0.0970(16) Uani 1 1 d . . .
H27 H 0.3320 0.5451 0.7872 0.116 Uiso 1 1 calc R . .
N3 N 0.3003(2) 0.4490(2) 0.2871(4) 0.1060(14) Uani 1 1 d . . .
N12 N 0.3034(2) 0.5071(3) 0.0596(3) 0.0985(13) Uani 1 1 d . . .
C47 C 0.3398(3) 0.6153(3) 0.0685(4) 0.0874(14) Uani 1 1 d . . .
C30 C 0.2849(3) 0.4871(2) 0.4756(5) 0.0947(15) Uani 1 1 d . . .
N1 N 0.1594(3) 0.4694(3) 0.7494(4) 0.1137(15) Uani 1 1 d . . .
C14 C 0.5341(3) 0.3295(4) 1.1709(6) 0.1098(18) Uani 1 1 d . . .
H14 H 0.5406 0.3172 1.2481 0.132 Uiso 1 1 calc R . .
C1 C 0.6576(3) 0.3826(3) 0.5412(5) 0.0939(15) Uani 1 1 d . . .
H1 H 0.6511 0.4166 0.5420 0.113 Uiso 1 1 calc R . .
C32 C 0.2156(3) 0.5013(3) 0.7647(5) 0.1008(17) Uani 1 1 d . . .
H32 H 0.2299 0.5234 0.8383 0.121 Uiso 1 1 calc R . .
C28 C 0.2607(3) 0.5068(3) 0.6757(5) 0.0924(15) Uani 1 1 d . . .
C61 C 0.1556(2) 0.0259(3) 0.3758(5) 0.0919(15) Uani 1 1 d . . .
C59 C 0.1951(3) 0.0707(3) 0.1785(5) 0.0967(16) Uani 1 1 d . . .
C62 C 0.1537(2) 0.0782(3) 0.4048(5) 0.0930(15) Uani 1 1 d . . .
H62 H 0.1377 0.0804 0.4811 0.112 Uiso 1 1 calc R . .
C3 C 0.5445(2) 0.3134(3) 0.5422(5) 0.0962(16) Uani 1 1 d . . .
H3 H 0.5113 0.2727 0.5505 0.115 Uiso 1 1 calc R . .
C67 C 0.1716(2) 0.2503(2) 0.5062(5) 0.0895(15) Uani 1 1 d . . .
H67 H 0.1840 0.2777 0.4339 0.107 Uiso 1 1 calc R . .
N2 N 0.4431(3) 0.5634(2) 0.7760(5) 0.1083(14) Uani 1 1 d . . .
N10 N 0.2412(2) 0.1114(3) -0.0136(4) 0.1093(15) Uani 1 1 d . . .
C41 C 0.3142(3) 0.4558(3) 0.0710(5) 0.1010(17) Uani 1 1 d . . .
H41 H 0.3585 0.4716 0.0885 0.121 Uiso 1 1 calc R . .
C48 C 0.2814(3) 0.6089(3) 0.0685(4) 0.0926(15) Uani 1 1 d . . .
H48 H 0.2460 0.5693 0.0687 0.111 Uiso 1 1 calc R . .
C40 C 0.2754(3) 0.4153(3) 0.1758(5) 0.1052(17) Uani 1 1 d . . .
H40 H 0.2317 0.4044 0.1659 0.126 Uiso 1 1 calc R . .
C26 C 0.3638(3) 0.5336(2) 0.6266(5) 0.0953(15) Uani 1 1 d . . .
C9 C 0.4625(3) 0.3772(3) 0.6404(6) 0.0997(16) Uani 1 1 d . . .
H9 H 0.4953 0.4213 0.6362 0.120 Uiso 1 1 calc R . .
C65 C 0.1382(2) -0.0224(3) 0.4635(5) 0.0959(16) Uani 1 1 d . . .
H65 H 0.1184 -0.0205 0.5351 0.115 Uiso 1 1 calc R . .
C63 C 0.1744(3) 0.1274(3) 0.3266(5) 0.0960(15) Uani 1 1 d . . .
C39 C 0.2655(3) 0.4571(3) 0.3554(5) 0.1061(17) Uani 1 1 d . . .
H39 H 0.2247 0.4435 0.3294 0.127 Uiso 1 1 calc R . .
C12 C 0.5561(3) 0.4076(3) 1.0268(6) 0.1154(18) Uani 1 1 d . . .
H12 H 0.5773 0.4497 1.0050 0.139 Uiso 1 1 calc R . .
C66 C 0.1767(3) 0.1849(2) 0.3670(6) 0.0985(16) Uani 1 1 d . . .
H66 H 0.1858 0.2166 0.3101 0.118 Uiso 1 1 calc R . .
C18 C 0.6008(3) 0.4383(3) 1.2306(6) 0.1153(19) Uani 1 1 d . . .
H18 H 0.6121 0.4262 1.3030 0.138 Uiso 1 1 calc R . .
C13 C 0.5642(3) 0.3911(3) 1.1408(6) 0.1074(17) Uani 1 1 d . . .
C33 C 0.1179(3) 0.4644(3) 0.8469(6) 0.1156(19) Uani 1 1 d . . .
H33 H 0.1429 0.4882 0.9181 0.139 Uiso 1 1 calc R . .
N9 N 0.1472(2) -0.0666(2) 0.4523(4) 0.0950(12) Uani 1 1 d . . .
C50 C 0.0624(2) 0.0424(3) -0.2252(4) 0.0833(14) Uani 1 1 d . . .
C31 C 0.3460(3) 0.5119(3) 0.5106(5) 0.1021(16) Uani 1 1 d . . .
H31 H 0.3754 0.5138 0.4544 0.123 Uiso 1 1 calc R . .
C37 C 0.0345(3) 0.4862(4) 0.9037(7) 0.153(3) Uani 1 1 d . . .
H37A H 0.0574 0.5098 0.9759 0.184 Uiso 1 1 calc R . .
H37B H 0.0091 0.5035 0.8747 0.184 Uiso 1 1 calc R . .
C51 C 0.1280(3) 0.0869(2) -0.2241(5) 0.0939(15) Uani 1 1 d . . .
H51 H 0.1406 0.1291 -0.2164 0.113 Uiso 1 1 calc R . .
C25 C 0.4274(3) 0.5552(3) 0.6663(6) 0.1072(17) Uani 1 1 d . . .
H25 H 0.4577 0.5633 0.6068 0.129 Uiso 1 1 calc R . .
C5 C 0.4561(3) 0.3617(4) 0.4131(6) 0.156(3) Uani 1 1 d . . .
H5A H 0.4878 0.4046 0.3957 0.188 Uiso 1 1 calc R . .
H5B H 0.4577 0.3354 0.3483 0.188 Uiso 1 1 calc R . .
C52 C 0.2337(2) 0.1204(3) -0.2281(5) 0.0975(16) Uani 1 1 d . . .
H52 H 0.2363 0.1604 -0.2091 0.117 Uiso 1 1 calc R . .
N11 N 0.1691(2) 0.07193(19) -0.2329(4) 0.0955(12) Uani 1 1 d . . .
C42 C 0.2970(4) 0.4197(3) -0.0474(5) 0.142(3) Uani 1 1 d . . .
H42A H 0.2544 0.4079 -0.0694 0.170 Uiso 1 1 calc R . .
H42B H 0.3243 0.4460 -0.1127 0.170 Uiso 1 1 calc R . .
C15 C 0.4946(3) 0.2857(3) 1.0899(7) 0.1111(18) Uani 1 1 d . . .
C68 C 0.1095(3) 0.2385(2) 0.5528(5) 0.0928(15) Uani 1 1 d . . .
H68 H 0.0954 0.2079 0.6201 0.111 Uiso 1 1 calc R . .
C20 C 0.7168(4) 0.5796(3) 1.2556(6) 0.122(2) Uani 1 1 d . . .
H20 H 0.7118 0.5971 1.1782 0.146 Uiso 1 1 calc R . .
C45 C 0.2804(4) 0.3579(3) 0.1819(5) 0.145(3) Uani 1 1 d . . .
H45A H 0.2533 0.3310 0.2469 0.174 Uiso 1 1 calc R . .
H45B H 0.3230 0.3693 0.2027 0.174 Uiso 1 1 calc R . .
C19 C 0.6544(3) 0.5374(3) 1.3093(5) 0.1161(19) Uani 1 1 d . . .
H19 H 0.6588 0.5153 1.3801 0.139 Uiso 1 1 calc R . .
C49 C 0.0206(3) 0.0617(2) -0.2254(5) 0.0902(14) Uani 1 1 d . . .
H49 H 0.0345 0.1043 -0.2256 0.108 Uiso 1 1 calc R . .
C16 C 0.4878(3) 0.3033(4) 0.9772(7) 0.1162(18) Uani 1 1 d . . .
H16 H 0.4619 0.2730 0.9207 0.139 Uiso 1 1 calc R . .
C29 C 0.2428(3) 0.4846(2) 0.5586(5) 0.0959(15) Uani 1 1 d . . .
H29 H 0.2011 0.4675 0.5357 0.115 Uiso 1 1 calc R . .
C57 C 0.2652(2) 0.1051(3) -0.1305(5) 0.1051(17) Uani 1 1 d . . .
H57 H 0.2573 0.0623 -0.1410 0.126 Uiso 1 1 calc R . .
C46 C 0.3467(3) 0.5608(3) 0.0718(5) 0.0962(16) Uani 1 1 d . . .
H46 H 0.3867 0.5668 0.0839 0.115 Uiso 1 1 calc R . .
C38 C 0.0802(3) 0.4926(3) 0.8038(6) 0.1146(18) Uani 1 1 d . . .
H38 H 0.0570 0.4707 0.7295 0.138 Uiso 1 1 calc R . .
N7 N 0.6177(2) 0.4933(3) 1.2161(5) 0.1206(16) Uani 1 1 d . . .
C53 C 0.2620(3) 0.1243(3) -0.3501(5) 0.142(3) Uani 1 1 d . . .
H53A H 0.2421 0.1371 -0.4116 0.170 Uiso 1 1 calc R . .
H53B H 0.2553 0.0835 -0.3732 0.170 Uiso 1 1 calc R . .
C60 C 0.1760(3) 0.0228(3) 0.2595(6) 0.1046(16) Uani 1 1 d . . .
H60 H 0.1766 -0.0131 0.2358 0.125 Uiso 1 1 calc R . .
C8 C 0.3993(3) 0.3725(3) 0.6370(7) 0.134(2) Uani 1 1 d . . .
H8A H 0.3967 0.3982 0.7016 0.161 Uiso 1 1 calc R . .
H8B H 0.3669 0.3295 0.6512 0.161 Uiso 1 1 calc R . .
C10 C 0.5090(3) 0.3850(3) 0.8256(6) 0.1142(18) Uani 1 1 d . . .
H10 H 0.5355 0.4264 0.8028 0.137 Uiso 1 1 calc R . .
C56 C 0.3337(3) 0.1500(4) -0.1284(6) 0.157(3) Uani 1 1 d . . .
H56A H 0.3536 0.1368 -0.0678 0.189 Uiso 1 1 calc R . .
H56B H 0.3412 0.1911 -0.1051 0.189 Uiso 1 1 calc R . .
N6 N 0.4552(2) 0.2025(3) 1.2318(6) 0.1208(16) Uani 1 1 d . . .
C34 C 0.0779(4) 0.3981(4) 0.8839(8) 0.182(4) Uani 1 1 d . . .
H34A H 0.1039 0.3823 0.9169 0.219 Uiso 1 1 calc R . .
H34B H 0.0561 0.3732 0.8123 0.219 Uiso 1 1 calc R . .
C6 C 0.3941(4) 0.3564(6) 0.4139(8) 0.182(4) Uani 1 1 d . . .
H6A H 0.3869 0.3705 0.3353 0.218 Uiso 1 1 calc R . .
H6B H 0.3622 0.3130 0.4247 0.218 Uiso 1 1 calc R . .
C7 C 0.3895(3) 0.3939(4) 0.5135(10) 0.166(3) Uani 1 1 d . . .
H7A H 0.3485 0.3903 0.5114 0.199 Uiso 1 1 calc R . .
H7B H 0.4206 0.4375 0.5014 0.199 Uiso 1 1 calc R . .
C36 C -0.0068(4) 0.4193(5) 0.9379(9) 0.195(4) Uani 1 1 d . . .
H36A H -0.0352 0.4162 1.0029 0.234 Uiso 1 1 calc R . .
H36B H -0.0315 0.3962 0.8670 0.234 Uiso 1 1 calc R . .
C44 C 0.2628(5) 0.3228(3) 0.0637(8) 0.175(3) Uani 1 1 d . . .
H44A H 0.2675 0.2863 0.0711 0.210 Uiso 1 1 calc R . .
H44B H 0.2193 0.3088 0.0452 0.210 Uiso 1 1 calc R . .
C43 C 0.3023(5) 0.3625(4) -0.0366(7) 0.174(3) Uani 1 1 d . . .
H43A H 0.2897 0.3394 -0.1135 0.209 Uiso 1 1 calc R . .
H43B H 0.3455 0.3743 -0.0207 0.209 Uiso 1 1 calc R . .
C72 C 0.2201(3) 0.2797(3) 0.6056(6) 0.1167(19) Uani 1 1 d . . .
H72A H 0.2090 0.2512 0.6747 0.140 Uiso 1 1 calc R . .
H72B H 0.2603 0.2879 0.5742 0.140 Uiso 1 1 calc R . .
C21 C 0.7576(4) 0.6326(4) 1.3437(8) 0.168(3) Uani 1 1 d . . .
H21A H 0.7675 0.6159 1.4157 0.201 Uiso 1 1 calc R . .
H21B H 0.7965 0.6618 1.3032 0.201 Uiso 1 1 calc R . .
C71 C 0.2248(4) 0.3391(3) 0.6476(6) 0.131(2) Uani 1 1 d . . .
H71A H 0.2561 0.3575 0.7119 0.157 Uiso 1 1 calc R . .
H71B H 0.2378 0.3683 0.5793 0.157 Uiso 1 1 calc R . .
C24 C 0.6231(4) 0.5728(4) 1.3492(8) 0.160(3) Uani 1 1 d . . .
H24A H 0.6144 0.5907 1.2776 0.192 Uiso 1 1 calc R . .
H24B H 0.5836 0.5444 1.3884 0.192 Uiso 1 1 calc R . .
C11 C 0.5181(3) 0.3648(3) 0.9430(6) 0.1109(18) Uani 1 1 d . . .
C70 C 0.1638(4) 0.3276(3) 0.6953(7) 0.139(2) Uani 1 1 d . . .
H70A H 0.1670 0.3669 0.7198 0.166 Uiso 1 1 calc R . .
H70B H 0.1521 0.3007 0.7672 0.166 Uiso 1 1 calc R . .
C58 C 0.2195(3) 0.0673(3) 0.0576(6) 0.1065(17) Uani 1 1 d . . .
H58 H 0.2184 0.0305 0.0343 0.128 Uiso 1 1 calc R . .
C35 C 0.0309(5) 0.3921(5) 0.9803(9) 0.203(4) Uani 1 1 d . . .
H35A H 0.0036 0.3482 0.9995 0.244 Uiso 1 1 calc R . .
H35B H 0.0529 0.4131 1.0552 0.244 Uiso 1 1 calc R . .
C69 C 0.1151(3) 0.2973(3) 0.5976(6) 0.127(2) Uani 1 1 d . . .
H69A H 0.0751 0.2890 0.6302 0.152 Uiso 1 1 calc R . .
H69B H 0.1255 0.3260 0.5288 0.152 Uiso 1 1 calc R . .
C23 C 0.6629(6) 0.6232(5) 1.4366(9) 0.194(4) Uani 1 1 d . . .
H23A H 0.6421 0.6462 1.4594 0.233 Uiso 1 1 calc R . .
H23B H 0.6689 0.6050 1.5109 0.233 Uiso 1 1 calc R . .
C55 C 0.3613(3) 0.1532(5) -0.2536(9) 0.189(4) Uani 1 1 d . . .
H55A H 0.4055 0.1840 -0.2526 0.227 Uiso 1 1 calc R . .
H55B H 0.3569 0.1130 -0.2738 0.227 Uiso 1 1 calc R . .
C54 C 0.3302(4) 0.1701(5) -0.3466(7) 0.193(4) Uani 1 1 d . . .
H54A H 0.3484 0.1715 -0.4267 0.231 Uiso 1 1 calc R . .
H54B H 0.3367 0.2114 -0.3289 0.231 Uiso 1 1 calc R . .
C22 C 0.7234(6) 0.6659(4) 1.3824(10) 0.204(4) Uani 1 1 d . . .
H22A H 0.7485 0.6981 1.4419 0.244 Uiso 1 1 calc R . .
H22B H 0.7174 0.6861 1.3111 0.244 Uiso 1 1 calc R . .
C17 C 0.4600(3) 0.2198(3) 1.1252(8) 0.118(2) Uani 1 1 d . . .
H17 H 0.4410 0.1898 1.0636 0.141 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
N5 C3 1.243(6) . ?
N5 C4 1.455(6) . ?
C4 C9 1.527(7) . ?
C4 C5 1.529(8) . ?
C4 H4 1.0000 . ?
C2 C1 1.375(6) 2_655 ?
C2 C1 1.399(6) . ?
C2 C3 1.462(7) . ?
N8 C66 1.238(6) . ?
N8 C67 1.460(6) . ?
N4 C10 1.253(7) . ?
N4 C9 1.455(7) . ?
C64 C63 1.372(7) . ?
C64 C59 1.393(7) . ?
C64 H64 0.9500 . ?
C27 C28 1.347(7) . ?
C27 C26 1.392(7) . ?
C27 H27 0.9500 . ?
N3 C39 1.251(6) . ?
N3 C40 1.449(7) . ?
N12 C46 1.252(6) . ?
N12 C41 1.454(7) . ?
C47 C48 1.374(7) 2_665 ?
C47 C48 1.397(6) . ?
C47 C46 1.470(7) . ?
C30 C29 1.381(7) . ?
C30 C31 1.398(7) . ?
C30 C39 1.487(8) . ?
N1 C32 1.242(7) . ?
N1 C33 1.465(7) . ?
C14 C15 1.385(8) . ?
C14 C13 1.385(8) . ?
C14 H14 0.9500 . ?
C1 C2 1.374(6) 3_665 ?
C1 H1 0.9500 . ?
C32 C28 1.458(8) . ?
C32 H32 0.9500 . ?
C28 C29 1.394(7) . ?
C61 C62 1.379(7) . ?
C61 C60 1.403(7) . ?
C61 C65 1.444(7) . ?
C59 C60 1.381(7) . ?
C59 C58 1.492(8) . ?
C62 C63 1.384(7) . ?
C62 H62 0.9500 . ?
C3 H3 0.9500 . ?
C67 C68 1.529(7) . ?
C67 C72 1.533(7) . ?
C67 H67 1.0000 . ?
N2 C25 1.261(7) . ?
N2 C38 1.452(7) 2_665 ?
N10 C58 1.242(6) . ?
N10 C57 1.471(7) . ?
C41 C42 1.529(7) . ?
C41 C40 1.531(7) . ?
C41 H41 1.0000 . ?
C48 C47 1.374(7) 3_565 ?
C48 H48 0.9500 . ?
C40 C45 1.514(8) . ?
C40 H40 1.0000 . ?
C26 C31 1.379(7) . ?
C26 C25 1.478(8) . ?
C9 C8 1.536(8) . ?
C9 H9 1.0000 . ?
C65 N9 1.249(6) . ?
C65 H65 0.9500 . ?
C63 C66 1.489(7) . ?
C39 H39 0.9500 . ?
C12 C13 1.376(8) . ?
C12 C11 1.381(8) . ?
C12 H12 0.9500 . ?
C66 H66 0.9500 . ?
C18 N7 1.241(7) . ?
C18 C13 1.469(8) . ?
C18 H18 0.9500 . ?
C33 C34 1.515(9) . ?
C33 C38 1.518(8) . ?
C33 H33 1.0000 . ?
N9 C68 1.457(6) 3 ?
C50 C49 1.365(6) . ?
C50 C49 1.397(6) 3 ?
C50 C51 1.463(7) . ?
C31 H31 0.9500 . ?
C37 C36 1.523(10) . ?
C37 C38 1.546(8) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C51 N11 1.269(6) . ?
C51 H51 0.9500 . ?
C25 H25 0.9500 . ?
C5 C6 1.500(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C52 N11 1.469(6) . ?
C52 C57 1.503(7) . ?
C52 C53 1.508(7) . ?
C52 H52 1.0000 . ?
C42 C43 1.519(9) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C15 C16 1.362(8) . ?
C15 C17 1.491(9) . ?
C68 N9 1.457(6) 2 ?
C68 C69 1.502(7) . ?
C68 H68 1.0000 . ?
C20 N6 1.452(8) 3_665 ?
C20 C19 1.511(9) . ?
C20 C21 1.556(9) . ?
C20 H20 1.0000 . ?
C45 C44 1.516(9) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C19 N7 1.458(7) . ?
C19 C24 1.522(9) . ?
C19 H19 1.0000 . ?
C49 C50 1.397(6) 2 ?
C49 H49 0.9500 . ?
C16 C11 1.397(8) . ?
C16 H16 0.9500 . ?
C29 H29 0.9500 . ?
C57 C56 1.519(8) . ?
C57 H57 1.0000 . ?
C46 H46 0.9500 . ?
C38 N2 1.452(7) 3_565 ?
C38 H38 1.0000 . ?
C53 C54 1.519(9) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C60 H60 0.9500 . ?
C8 C7 1.535(10) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 C11 1.454(8) . ?
C10 H10 0.9500 . ?
C56 C55 1.534(10) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
N6 C17 1.243(7) . ?
N6 C20 1.452(8) 2_655 ?
C34 C35 1.544(10) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C6 C7 1.495(11) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C36 C35 1.500(12) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C44 C43 1.492(11) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C72 C71 1.514(8) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C21 C22 1.535(12) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C71 C70 1.512(9) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C24 C23 1.511(11) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C70 C69 1.524(9) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C58 H58 0.9500 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C23 C22 1.483(13) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C55 C54 1.478(12) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C17 H17 0.9500 . ?

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
C3 N5 C4 119.9(5) . . ?
N5 C4 C9 107.8(4) . . ?
N5 C4 C5 107.9(5) . . ?
C9 C4 C5 112.3(5) . . ?
N5 C4 H4 109.6 . . ?
C9 C4 H4 109.6 . . ?
C5 C4 H4 109.6 . . ?
C1 C2 C1 117.9(5) 2_655 . ?
C1 C2 C3 121.1(6) 2_655 . ?
C1 C2 C3 121.0(6) . . ?
C66 N8 C67 117.2(5) . . ?
C10 N4 C9 117.8(5) . . ?
C63 C64 C59 120.4(5) . . ?
C63 C64 H64 119.8 . . ?
C59 C64 H64 119.8 . . ?
C28 C27 C26 122.3(5) . . ?
C28 C27 H27 118.9 . . ?
C26 C27 H27 118.9 . . ?
C39 N3 C40 118.5(5) . . ?
C46 N12 C41 120.2(5) . . ?
C48 C47 C48 120.4(6) 2_665 . ?
C48 C47 C46 119.4(6) 2_665 . ?
C48 C47 C46 120.2(6) . . ?
C29 C30 C31 119.1(5) . . ?
C29 C30 C39 121.5(6) . . ?
C31 C30 C39 119.0(6) . . ?
C32 N1 C33 119.3(5) . . ?
C15 C14 C13 120.7(6) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C2 C1 C2 122.1(5) 3_665 . ?
C2 C1 H1 119.0 3_665 . ?
C2 C1 H1 119.0 . . ?
N1 C32 C28 123.5(6) . . ?
N1 C32 H32 118.2 . . ?
C28 C32 H32 118.2 . . ?
C27 C28 C29 118.8(5) . . ?
C27 C28 C32 120.5(6) . . ?
C29 C28 C32 120.6(6) . . ?
C62 C61 C60 117.0(5) . . ?
C62 C61 C65 120.5(5) . . ?
C60 C61 C65 122.4(5) . . ?
C60 C59 C64 119.1(5) . . ?
C60 C59 C58 120.5(6) . . ?
C64 C59 C58 120.3(6) . . ?
C61 C62 C63 122.3(5) . . ?
C61 C62 H62 118.8 . . ?
C63 C62 H62 118.8 . . ?
N5 C3 C2 123.0(5) . . ?
N5 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
N8 C67 C68 109.1(4) . . ?
N8 C67 C72 107.9(4) . . ?
C68 C67 C72 110.1(4) . . ?
N8 C67 H67 109.9 . . ?
C68 C67 H67 109.9 . . ?
C72 C67 H67 109.9 . . ?
C25 N2 C38 117.7(5) . 2_665 ?
C58 N10 C57 118.8(5) . . ?
N12 C41 C42 109.4(4) . . ?
N12 C41 C40 108.5(5) . . ?
C42 C41 C40 110.8(5) . . ?
N12 C41 H41 109.4 . . ?
C42 C41 H41 109.4 . . ?
C40 C41 H41 109.4 . . ?
C47 C48 C47 119.6(6) 3_565 . ?
C47 C48 H48 120.2 3_565 . ?
C47 C48 H48 120.2 . . ?
N3 C40 C45 107.7(5) . . ?
N3 C40 C41 107.9(5) . . ?
C45 C40 C41 109.9(5) . . ?
N3 C40 H40 110.4 . . ?
C45 C40 H40 110.4 . . ?
C41 C40 H40 110.4 . . ?
C31 C26 C27 118.7(6) . . ?
C31 C26 C25 120.0(6) . . ?
C27 C26 C25 121.0(6) . . ?
N4 C9 C4 108.9(5) . . ?
N4 C9 C8 108.6(5) . . ?
C4 C9 C8 110.6(5) . . ?
N4 C9 H9 109.6 . . ?
C4 C9 H9 109.6 . . ?
C8 C9 H9 109.6 . . ?
N9 C65 C61 124.8(5) . . ?
N9 C65 H65 117.6 . . ?
C61 C65 H65 117.6 . . ?
C64 C63 C62 119.4(5) . . ?
C64 C63 C66 120.6(5) . . ?
C62 C63 C66 119.9(5) . . ?
N3 C39 C30 123.0(6) . . ?
N3 C39 H39 118.5 . . ?
C30 C39 H39 118.5 . . ?
C13 C12 C11 122.0(6) . . ?
C13 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
N8 C66 C63 120.9(5) . . ?
N8 C66 H66 119.6 . . ?
C63 C66 H66 119.6 . . ?
N7 C18 C13 122.9(6) . . ?
N7 C18 H18 118.6 . . ?
C13 C18 H18 118.6 . . ?
C12 C13 C14 118.6(6) . . ?
C12 C13 C18 120.3(7) . . ?
C14 C13 C18 121.0(6) . . ?
N1 C33 C34 110.2(6) . . ?
N1 C33 C38 108.4(5) . . ?
C34 C33 C38 112.0(6) . . ?
N1 C33 H33 108.7 . . ?
C34 C33 H33 108.7 . . ?
C38 C33 H33 108.7 . . ?
C65 N9 C68 117.1(5) . 3 ?
C49 C50 C49 118.5(6) . 3 ?
C49 C50 C51 120.4(6) . . ?
C49 C50 C51 121.1(6) 3 . ?
C26 C31 C30 120.2(5) . . ?
C26 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C36 C37 C38 110.7(6) . . ?
C36 C37 H37A 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C38 C37 H37B 109.5 . . ?
H37A C37 H37B 108.1 . . ?
N11 C51 C50 123.2(5) . . ?
N11 C51 H51 118.4 . . ?
C50 C51 H51 118.4 . . ?
N2 C25 C26 122.6(6) . . ?
N2 C25 H25 118.7 . . ?
C26 C25 H25 118.7 . . ?
C6 C5 C4 110.8(5) . . ?
C6 C5 H5A 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N11 C52 C57 108.7(4) . . ?
N11 C52 C53 108.2(5) . . ?
C57 C52 C53 111.5(5) . . ?
N11 C52 H52 109.5 . . ?
C57 C52 H52 109.5 . . ?
C53 C52 H52 109.5 . . ?
C51 N11 C52 118.6(5) . . ?
C43 C42 C41 111.4(5) . . ?
C43 C42 H42A 109.4 . . ?
C41 C42 H42A 109.4 . . ?
C43 C42 H42B 109.4 . . ?
C41 C42 H42B 109.4 . . ?
H42A C42 H42B 108.0 . . ?
C16 C15 C14 119.4(7) . . ?
C16 C15 C17 120.3(7) . . ?
C14 C15 C17 120.3(7) . . ?
N9 C68 C69 111.0(5) 2 . ?
N9 C68 C67 107.1(4) 2 . ?
C69 C68 C67 109.7(4) . . ?
N9 C68 H68 109.7 2 . ?
C69 C68 H68 109.7 . . ?
C67 C68 H68 109.7 . . ?
N6 C20 C19 109.0(6) 3_665 . ?
N6 C20 C21 108.0(6) 3_665 . ?
C19 C20 C21 111.5(6) . . ?
N6 C20 H20 109.4 3_665 . ?
C19 C20 H20 109.4 . . ?
C21 C20 H20 109.4 . . ?
C40 C45 C44 112.3(5) . . ?
C40 C45 H45A 109.1 . . ?
C44 C45 H45A 109.1 . . ?
C40 C45 H45B 109.1 . . ?
C44 C45 H45B 109.1 . . ?
H45A C45 H45B 107.9 . . ?
N7 C19 C20 107.4(5) . . ?
N7 C19 C24 109.5(6) . . ?
C20 C19 C24 111.4(6) . . ?
N7 C19 H19 109.5 . . ?
C20 C19 H19 109.5 . . ?
C24 C19 H19 109.5 . . ?
C50 C49 C50 121.5(6) . 2 ?
C50 C49 H49 119.3 . . ?
C50 C49 H49 119.3 2 . ?
C15 C16 C11 121.5(6) . . ?
C15 C16 H16 119.3 . . ?
C11 C16 H16 119.3 . . ?
C30 C29 C28 120.9(5) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
N10 C57 C52 107.7(5) . . ?
N10 C57 C56 106.4(5) . . ?
C52 C57 C56 111.6(5) . . ?
N10 C57 H57 110.3 . . ?
C52 C57 H57 110.3 . . ?
C56 C57 H57 110.3 . . ?
N12 C46 C47 124.1(6) . . ?
N12 C46 H46 117.9 . . ?
C47 C46 H46 117.9 . . ?
N2 C38 C33 109.8(5) 3_565 . ?
N2 C38 C37 109.5(6) 3_565 . ?
C33 C38 C37 109.6(5) . . ?
N2 C38 H38 109.3 3_565 . ?
C33 C38 H38 109.3 . . ?
C37 C38 H38 109.3 . . ?
C18 N7 C19 119.5(5) . . ?
C52 C53 C54 110.2(5) . . ?
C52 C53 H53A 109.6 . . ?
C54 C53 H53A 109.6 . . ?
C52 C53 H53B 109.6 . . ?
C54 C53 H53B 109.6 . . ?
H53A C53 H53B 108.1 . . ?
C59 C60 C61 121.7(5) . . ?
C59 C60 H60 119.1 . . ?
C61 C60 H60 119.1 . . ?
C9 C8 C7 109.8(5) . . ?
C9 C8 H8A 109.7 . . ?
C7 C8 H8A 109.7 . . ?
C9 C8 H8B 109.7 . . ?
C7 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
N4 C10 C11 123.5(6) . . ?
N4 C10 H10 118.3 . . ?
C11 C10 H10 118.3 . . ?
C57 C56 C55 110.0(5) . . ?
C57 C56 H56A 109.7 . . ?
C55 C56 H56A 109.7 . . ?
C57 C56 H56B 109.7 . . ?
C55 C56 H56B 109.7 . . ?
H56A C56 H56B 108.2 . . ?
C17 N6 C20 117.8(6) . 2_655 ?
C33 C34 C35 110.5(7) . . ?
C33 C34 H34A 109.6 . . ?
C35 C34 H34A 109.6 . . ?
C33 C34 H34B 109.6 . . ?
C35 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
C7 C6 C5 110.9(7) . . ?
C7 C6 H6A 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C6 C7 C8 110.8(6) . . ?
C6 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C35 C36 C37 110.2(8) . . ?
C35 C36 H36A 109.6 . . ?
C37 C36 H36A 109.6 . . ?
C35 C36 H36B 109.6 . . ?
C37 C36 H36B 109.6 . . ?
H36A C36 H36B 108.1 . . ?
C43 C44 C45 110.4(6) . . ?
C43 C44 H44A 109.6 . . ?
C45 C44 H44A 109.6 . . ?
C43 C44 H44B 109.6 . . ?
C45 C44 H44B 109.6 . . ?
H44A C44 H44B 108.1 . . ?
C44 C43 C42 110.4(7) . . ?
C44 C43 H43A 109.6 . . ?
C42 C43 H43A 109.6 . . ?
C44 C43 H43B 109.6 . . ?
C42 C43 H43B 109.6 . . ?
H43A C43 H43B 108.1 . . ?
C71 C72 C67 110.4(5) . . ?
C71 C72 H72A 109.6 . . ?
C67 C72 H72A 109.6 . . ?
C71 C72 H72B 109.6 . . ?
C67 C72 H72B 109.6 . . ?
H72A C72 H72B 108.1 . . ?
C22 C21 C20 109.4(7) . . ?
C22 C21 H21A 109.8 . . ?
C20 C21 H21A 109.8 . . ?
C22 C21 H21B 109.8 . . ?
C20 C21 H21B 109.8 . . ?
H21A C21 H21B 108.2 . . ?
C70 C71 C72 110.4(5) . . ?
C70 C71 H71A 109.6 . . ?
C72 C71 H71A 109.6 . . ?
C70 C71 H71B 109.6 . . ?
C72 C71 H71B 109.6 . . ?
H71A C71 H71B 108.1 . . ?
C23 C24 C19 110.9(7) . . ?
C23 C24 H24A 109.5 . . ?
C19 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C19 C24 H24B 109.5 . . ?
H24A C24 H24B 108.0 . . ?
C12 C11 C16 117.8(6) . . ?
C12 C11 C10 119.8(7) . . ?
C16 C11 C10 122.4(6) . . ?
C71 C70 C69 109.6(5) . . ?
C71 C70 H70A 109.8 . . ?
C69 C70 H70A 109.8 . . ?
C71 C70 H70B 109.8 . . ?
C69 C70 H70B 109.8 . . ?
H70A C70 H70B 108.2 . . ?
N10 C58 C59 121.8(6) . . ?
N10 C58 H58 119.1 . . ?
C59 C58 H58 119.1 . . ?
C36 C35 C34 111.7(8) . . ?
C36 C35 H35A 109.3 . . ?
C34 C35 H35A 109.3 . . ?
C36 C35 H35B 109.3 . . ?
C34 C35 H35B 109.3 . . ?
H35A C35 H35B 107.9 . . ?
C68 C69 C70 112.5(5) . . ?
C68 C69 H69A 109.1 . . ?
C70 C69 H69A 109.1 . . ?
C68 C69 H69B 109.1 . . ?
C70 C69 H69B 109.1 . . ?
H69A C69 H69B 107.8 . . ?
C22 C23 C24 111.2(8) . . ?
C22 C23 H23A 109.4 . . ?
C24 C23 H23A 109.4 . . ?
C22 C23 H23B 109.4 . . ?
C24 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C54 C55 C56 110.6(7) . . ?
C54 C55 H55A 109.5 . . ?
C56 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
C56 C55 H55B 109.5 . . ?
H55A C55 H55B 108.1 . . ?
C55 C54 C53 111.1(7) . . ?
C55 C54 H54A 109.4 . . ?
C53 C54 H54A 109.4 . . ?
C55 C54 H54B 109.4 . . ?
C53 C54 H54B 109.4 . . ?
H54A C54 H54B 108.0 . . ?
C23 C22 C21 111.8(8) . . ?
C23 C22 H22A 109.3 . . ?
C21 C22 H22A 109.3 . . ?
C23 C22 H22B 109.3 . . ?
C21 C22 H22B 109.3 . . ?
H22A C22 H22B 107.9 . . ?
N6 C17 C15 122.6(6) . . ?
N6 C17 H17 118.7 . . ?
C15 C17 H17 118.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N5 C4 C9 121.3(6) . . . . ?
C3 N5 C4 C5 -117.2(6) . . . . ?
C1 C2 C1 C2 0.9(10) 2_655 . . 3_665 ?
C3 C2 C1 C2 179.5(4) . . . 3_665 ?
C33 N1 C32 C28 176.9(5) . . . . ?
C26 C27 C28 C29 0.6(8) . . . . ?
C26 C27 C28 C32 176.9(5) . . . . ?
N1 C32 C28 C27 -164.8(6) . . . . ?
N1 C32 C28 C29 11.4(9) . . . . ?
C63 C64 C59 C60 -0.7(8) . . . . ?
C63 C64 C59 C58 -177.3(5) . . . . ?
C60 C61 C62 C63 -3.9(8) . . . . ?
C65 C61 C62 C63 175.1(5) . . . . ?
C4 N5 C3 C2 179.6(5) . . . . ?
C1 C2 C3 N5 -174.8(5) 2_655 . . . ?
C1 C2 C3 N5 6.6(8) . . . . ?
C66 N8 C67 C68 118.6(5) . . . . ?
C66 N8 C67 C72 -121.8(5) . . . . ?
C46 N12 C41 C42 -119.7(6) . . . . ?
C46 N12 C41 C40 119.3(5) . . . . ?
C48 C47 C48 C47 0.1(10) 2_665 . . 3_565 ?
C46 C47 C48 C47 178.4(3) . . . 3_565 ?
C39 N3 C40 C45 -117.3(6) . . . . ?
C39 N3 C40 C41 124.0(6) . . . . ?
N12 C41 C40 N3 -68.7(6) . . . . ?
C42 C41 C40 N3 171.2(5) . . . . ?
N12 C41 C40 C45 174.0(5) . . . . ?
C42 C41 C40 C45 53.9(7) . . . . ?
C28 C27 C26 C31 -0.2(8) . . . . ?
C28 C27 C26 C25 -175.3(5) . . . . ?
C10 N4 C9 C4 122.0(6) . . . . ?
C10 N4 C9 C8 -117.5(6) . . . . ?
N5 C4 C9 N4 -68.8(6) . . . . ?
C5 C4 C9 N4 172.5(5) . . . . ?
N5 C4 C9 C8 172.0(5) . . . . ?
C5 C4 C9 C8 53.3(7) . . . . ?
C62 C61 C65 N9 -168.5(5) . . . . ?
C60 C61 C65 N9 10.5(8) . . . . ?
C59 C64 C63 C62 -1.2(8) . . . . ?
C59 C64 C63 C66 176.6(5) . . . . ?
C61 C62 C63 C64 3.6(8) . . . . ?
C61 C62 C63 C66 -174.2(5) . . . . ?
C40 N3 C39 C30 175.6(5) . . . . ?
C29 C30 C39 N3 -166.9(5) . . . . ?
C31 C30 C39 N3 5.2(8) . . . . ?
C67 N8 C66 C63 178.6(5) . . . . ?
C64 C63 C66 N8 -169.7(5) . . . . ?
C62 C63 C66 N8 8.1(8) . . . . ?
C11 C12 C13 C14 1.2(9) . . . . ?
C11 C12 C13 C18 -174.9(6) . . . . ?
C15 C14 C13 C12 -2.8(9) . . . . ?
C15 C14 C13 C18 173.3(6) . . . . ?
N7 C18 C13 C12 11.5(10) . . . . ?
N7 C18 C13 C14 -164.5(6) . . . . ?
C32 N1 C33 C34 -121.1(7) . . . . ?
C32 N1 C33 C38 115.9(6) . . . . ?
C61 C65 N9 C68 177.2(5) . . . 3 ?
C27 C26 C31 C30 0.0(8) . . . . ?
C25 C26 C31 C30 175.1(5) . . . . ?
C29 C30 C31 C26 -0.2(8) . . . . ?
C39 C30 C31 C26 -172.5(5) . . . . ?
C49 C50 C51 N11 -174.6(5) . . . . ?
C49 C50 C51 N11 5.8(7) 3 . . . ?
C38 N2 C25 C26 -177.0(5) 2_665 . . . ?
C31 C26 C25 N2 -164.9(5) . . . . ?
C27 C26 C25 N2 10.1(8) . . . . ?
N5 C4 C5 C6 -172.9(7) . . . . ?
C9 C4 C5 C6 -54.2(9) . . . . ?
C50 C51 N11 C52 -178.7(4) . . . . ?
C57 C52 N11 C51 125.5(5) . . . . ?
C53 C52 N11 C51 -113.3(6) . . . . ?
N12 C41 C42 C43 -175.2(7) . . . . ?
C40 C41 C42 C43 -55.5(8) . . . . ?
C13 C14 C15 C16 3.4(9) . . . . ?
C13 C14 C15 C17 -177.1(5) . . . . ?
N8 C67 C68 N9 -64.9(5) . . . 2 ?
C72 C67 C68 N9 176.9(4) . . . 2 ?
N8 C67 C68 C69 174.6(5) . . . . ?
C72 C67 C68 C69 56.4(6) . . . . ?
N3 C40 C45 C44 -173.0(7) . . . . ?
C41 C40 C45 C44 -55.6(8) . . . . ?
N6 C20 C19 N7 -66.5(6) 3_665 . . . ?
C21 C20 C19 N7 174.4(6) . . . . ?
N6 C20 C19 C24 173.6(5) 3_665 . . . ?
C21 C20 C19 C24 54.5(8) . . . . ?
C49 C50 C49 C50 0.3(9) 3 . . 2 ?
C51 C50 C49 C50 -179.3(3) . . . 2 ?
C14 C15 C16 C11 -2.4(9) . . . . ?
C17 C15 C16 C11 178.0(6) . . . . ?
C31 C30 C29 C28 0.5(8) . . . . ?
C39 C30 C29 C28 172.6(5) . . . . ?
C27 C28 C29 C30 -0.7(8) . . . . ?
C32 C28 C29 C30 -177.0(5) . . . . ?
C58 N10 C57 C52 125.6(6) . . . . ?
C58 N10 C57 C56 -114.5(6) . . . . ?
N11 C52 C57 N10 -69.1(6) . . . . ?
C53 C52 C57 N10 171.6(5) . . . . ?
N11 C52 C57 C56 174.4(5) . . . . ?
C53 C52 C57 C56 55.2(7) . . . . ?
C41 N12 C46 C47 -176.5(4) . . . . ?
C48 C47 C46 N12 -172.4(5) 2_665 . . . ?
C48 C47 C46 N12 9.3(8) . . . . ?
N1 C33 C38 N2 -61.4(7) . . . 3_565 ?
C34 C33 C38 N2 176.8(6) . . . 3_565 ?
N1 C33 C38 C37 178.3(6) . . . . ?
C34 C33 C38 C37 56.5(8) . . . . ?
C36 C37 C38 N2 -178.1(7) . . . 3_565 ?
C36 C37 C38 C33 -57.5(8) . . . . ?
C13 C18 N7 C19 -179.6(6) . . . . ?
C20 C19 N7 C18 114.6(7) . . . . ?
C24 C19 N7 C18 -124.4(7) . . . . ?
N11 C52 C53 C54 -175.1(7) . . . . ?
C57 C52 C53 C54 -55.6(9) . . . . ?
C64 C59 C60 C61 0.2(8) . . . . ?
C58 C59 C60 C61 176.9(5) . . . . ?
C62 C61 C60 C59 2.0(8) . . . . ?
C65 C61 C60 C59 -177.0(5) . . . . ?
N4 C9 C8 C7 -174.0(6) . . . . ?
C4 C9 C8 C7 -54.6(8) . . . . ?
C9 N4 C10 C11 177.9(5) . . . . ?
N10 C57 C56 C55 -172.0(7) . . . . ?
C52 C57 C56 C55 -54.8(9) . . . . ?
N1 C33 C34 C35 -176.0(8) . . . . ?
C38 C33 C34 C35 -55.1(9) . . . . ?
C4 C5 C6 C7 57.2(10) . . . . ?
C5 C6 C7 C8 -60.1(10) . . . . ?
C9 C8 C7 C6 58.5(9) . . . . ?
C38 C37 C36 C35 58.3(10) . . . . ?
C40 C45 C44 C43 58.0(10) . . . . ?
C45 C44 C43 C42 -57.8(9) . . . . ?
C41 C42 C43 C44 57.5(9) . . . . ?
N8 C67 C72 C71 -177.2(5) . . . . ?
C68 C67 C72 C71 -58.2(6) . . . . ?
N6 C20 C21 C22 -173.5(8) 3_665 . . . ?
C19 C20 C21 C22 -53.8(9) . . . . ?
C67 C72 C71 C70 59.0(7) . . . . ?
N7 C19 C24 C23 -174.3(8) . . . . ?
C20 C19 C24 C23 -55.7(9) . . . . ?
C13 C12 C11 C16 -0.3(9) . . . . ?
C13 C12 C11 C10 177.1(6) . . . . ?
C15 C16 C11 C12 0.9(9) . . . . ?
C15 C16 C11 C10 -176.5(6) . . . . ?
N4 C10 C11 C12 -167.5(6) . . . . ?
N4 C10 C11 C16 9.8(10) . . . . ?
C72 C71 C70 C69 -57.4(8) . . . . ?
C57 N10 C58 C59 179.0(5) . . . . ?
C60 C59 C58 N10 -174.7(6) . . . . ?
C64 C59 C58 N10 1.9(9) . . . . ?
C37 C36 C35 C34 -57.0(12) . . . . ?
C33 C34 C35 C36 55.3(12) . . . . ?
N9 C68 C69 C70 -174.9(5) 2 . . . ?
C67 C68 C69 C70 -56.8(7) . . . . ?
C71 C70 C69 C68 57.3(8) . . . . ?
C19 C24 C23 C22 57.5(11) . . . . ?
C57 C56 C55 C54 56.7(10) . . . . ?
C56 C55 C54 C53 -58.6(10) . . . . ?
C52 C53 C54 C55 57.9(10) . . . . ?
C24 C23 C22 C21 -58.4(12) . . . . ?
C20 C21 C22 C23 55.8(11) . . . . ?
C20 N6 C17 C15 180.0(6) 2_655 . . . ?
C16 C15 C17 N6 -165.8(7) . . . . ?
C14 C15 C17 N6 14.7(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        20.81
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.156
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.035
_database_code_depnum_ccdc_archive 'CCDC 991217'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_CC4_beta_350K
_audit_creation_date             2013-06-24
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C66 H72 N12'
_chemical_formula_sum            'C66 H72 N12'
_chemical_formula_weight         1033.36
_chemical_absolute_configuration unk
_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'

_space_group_crystal_system      cubic
_space_group_IT_number           210
_space_group_name_H-M_alt        'F 41 3 2'
_space_group_name_Hall           'F 4d 2 3'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y+1/4, x+1/4, z+1/4'
3 '-x, -y, z'
4 'y+1/4, -x+1/4, z+1/4'
5 'x+1/4, -z+1/4, y+1/4'
6 'x, -y, -z'
7 'x+1/4, z+1/4, -y+1/4'
8 'z+1/4, y+1/4, -x+1/4'
9 '-x, y, -z'
10 '-z+1/4, y+1/4, x+1/4'
11 'z, x, y'
12 'y, z, x'
13 '-y, -z, x'
14 'z, -x, -y'
15 '-y, z, -x'
16 '-z, -x, y'
17 '-z, x, -y'
18 'y, -z, -x'
19 'y+1/4, x+1/4, -z+1/4'
20 '-y+1/4, -x+1/4, -z+1/4'
21 '-x+1/4, z+1/4, y+1/4'
22 '-x+1/4, -z+1/4, -y+1/4'
23 'z+1/4, -y+1/4, x+1/4'
24 '-z+1/4, -y+1/4, -x+1/4'
25 'x, y+1/2, z+1/2'
26 '-y+1/4, x+3/4, z+3/4'
27 '-x, -y+1/2, z+1/2'
28 'y+1/4, -x+3/4, z+3/4'
29 'x+1/4, -z+3/4, y+3/4'
30 'x, -y+1/2, -z+1/2'
31 'x+1/4, z+3/4, -y+3/4'
32 'z+1/4, y+3/4, -x+3/4'
33 '-x, y+1/2, -z+1/2'
34 '-z+1/4, y+3/4, x+3/4'
35 'z, x+1/2, y+1/2'
36 'y, z+1/2, x+1/2'
37 '-y, -z+1/2, x+1/2'
38 'z, -x+1/2, -y+1/2'
39 '-y, z+1/2, -x+1/2'
40 '-z, -x+1/2, y+1/2'
41 '-z, x+1/2, -y+1/2'
42 'y, -z+1/2, -x+1/2'
43 'y+1/4, x+3/4, -z+3/4'
44 '-y+1/4, -x+3/4, -z+3/4'
45 '-x+1/4, z+3/4, y+3/4'
46 '-x+1/4, -z+3/4, -y+3/4'
47 'z+1/4, -y+3/4, x+3/4'
48 '-z+1/4, -y+3/4, -x+3/4'
49 'x+1/2, y, z+1/2'
50 '-y+3/4, x+1/4, z+3/4'
51 '-x+1/2, -y, z+1/2'
52 'y+3/4, -x+1/4, z+3/4'
53 'x+3/4, -z+1/4, y+3/4'
54 'x+1/2, -y, -z+1/2'
55 'x+3/4, z+1/4, -y+3/4'
56 'z+3/4, y+1/4, -x+3/4'
57 '-x+1/2, y, -z+1/2'
58 '-z+3/4, y+1/4, x+3/4'
59 'z+1/2, x, y+1/2'
60 'y+1/2, z, x+1/2'
61 '-y+1/2, -z, x+1/2'
62 'z+1/2, -x, -y+1/2'
63 '-y+1/2, z, -x+1/2'
64 '-z+1/2, -x, y+1/2'
65 '-z+1/2, x, -y+1/2'
66 'y+1/2, -z, -x+1/2'
67 'y+3/4, x+1/4, -z+3/4'
68 '-y+3/4, -x+1/4, -z+3/4'
69 '-x+3/4, z+1/4, y+3/4'
70 '-x+3/4, -z+1/4, -y+3/4'
71 'z+3/4, -y+1/4, x+3/4'
72 '-z+3/4, -y+1/4, -x+3/4'
73 'x+1/2, y+1/2, z'
74 '-y+3/4, x+3/4, z+1/4'
75 '-x+1/2, -y+1/2, z'
76 'y+3/4, -x+3/4, z+1/4'
77 'x+3/4, -z+3/4, y+1/4'
78 'x+1/2, -y+1/2, -z'
79 'x+3/4, z+3/4, -y+1/4'
80 'z+3/4, y+3/4, -x+1/4'
81 '-x+1/2, y+1/2, -z'
82 '-z+3/4, y+3/4, x+1/4'
83 'z+1/2, x+1/2, y'
84 'y+1/2, z+1/2, x'
85 '-y+1/2, -z+1/2, x'
86 'z+1/2, -x+1/2, -y'
87 '-y+1/2, z+1/2, -x'
88 '-z+1/2, -x+1/2, y'
89 '-z+1/2, x+1/2, -y'
90 'y+1/2, -z+1/2, -x'
91 'y+3/4, x+3/4, -z+1/4'
92 '-y+3/4, -x+3/4, -z+1/4'
93 '-x+3/4, z+3/4, y+1/4'
94 '-x+3/4, -z+3/4, -y+1/4'
95 'z+3/4, -y+3/4, x+1/4'
96 '-z+3/4, -y+3/4, -x+1/4'

_cell_length_a                   24.242(9)
_cell_length_b                   24.242(9)
_cell_length_c                   24.242(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     14246(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4531
_cell_measurement_temperature    350
_cell_measurement_theta_max      18.139
_cell_measurement_theta_min      2.377
_exptl_absorpt_coefficient_mu    0.058
_exptl_absorpt_correction_T_max  0.7443
_exptl_absorpt_correction_T_min  0.4251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1773 before and 0.1003 after correction.
The Ratio of minimum to maximum transmission is 0.5711.
The λ/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.964
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4416
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.1241
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26833
_diffrn_reflns_theta_full        18.81
_diffrn_reflns_theta_max         18.81
_diffrn_reflns_theta_min         1.45
_diffrn_ambient_temperature      350.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_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_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_number_gt                408
_reflns_number_total             480
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   10(10)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.338
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     60
_refine_ls_number_reflns         480
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.1146
_refine_ls_restrained_S_all      1.338
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2692
_refine_ls_wR_factor_ref         0.2904
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: H6A(0.5) H6B(0.5)
3.a Ternary CH refined with riding coordinates:
 C4(H4)
3.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
N1 N 0.4507(3) 0.2324(3) 0.5401(3) 0.108(2) Uani 1 1 d . . . .
C1 C 0.4415(3) 0.1172(4) 0.6356(4) 0.107(3) Uani 1 1 d . . . .
H1 H 0.4721 0.1261 0.6571 0.128 Uiso 1 1 calc . . R .
C4 C 0.4901(3) 0.2764(3) 0.5295(3) 0.100(3) Uani 1 1 d . . . .
H4 H 0.5219 0.2718 0.5541 0.120 Uiso 1 1 calc . . R .
C2 C 0.4284(3) 0.1494(3) 0.5904(4) 0.100(3) Uani 1 1 d . . . .
C3 C 0.4631(4) 0.1969(4) 0.5767(4) 0.104(3) Uani 1 1 d . . . .
H3 H 0.4960 0.2014 0.5958 0.125 Uiso 1 1 calc . . R .
C5 C 0.4669(4) 0.3331(3) 0.5369(4) 0.135(4) Uani 1 1 d . . . .
H5A H 0.4283 0.3340 0.5266 0.162 Uiso 1 1 calc . . R .
H5B H 0.4703 0.3449 0.5751 0.162 Uiso 1 1 calc . . R .
C6 C 0.5000 0.3697(6) 0.5000 0.176(7) Uani 1 2 d . . S T
H6A H 0.5242 0.3931 0.5217 0.211 Uiso 0.50 1 calc . . R .
H6B H 0.4758 0.3931 0.4783 0.211 Uiso 0.50 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
N1 C4 1.454(9) . ?
N1 C3 1.272(10) . ?
C1 H1 0.9300 . ?
C1 C2 1.392(9) 40_655 ?
C1 C2 1.382(9) . ?
C4 C4 1.510(14) 9_656 ?
C4 H4 0.9800 . ?
C4 C5 1.497(10) . ?
C2 C1 1.391(9) 87_546 ?
C2 C3 1.464(11) . ?
C3 H3 0.9300 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.494(11) . ?
C6 C5 1.494(11) 9_656 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?

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
C3 N1 C4 117.7(7) . . ?
C2 C1 H1 119.6 40_655 . ?
C2 C1 H1 119.6 . . ?
C2 C1 C2 120.8(8) . 40_655 ?
N1 C4 C4 112.1(6) . 9_656 ?
N1 C4 H4 109.1 . . ?
N1 C4 C5 113.9(7) . . ?
C4 C4 H4 109.1 9_656 . ?
C5 C4 C4 103.5(5) . 9_656 ?
C5 C4 H4 109.1 . . ?
C1 C2 C1 119.2(8) . 87_546 ?
C1 C2 C3 119.6(10) . . ?
C1 C2 C3 121.2(10) 87_546 . ?
N1 C3 C2 123.8(8) . . ?
N1 C3 H3 118.1 . . ?
C2 C3 H3 118.1 . . ?
C4 C5 H5A 110.6 . . ?
C4 C5 H5B 110.6 . . ?
H5A C5 H5B 108.7 . . ?
C6 C5 C4 105.8(8) . . ?
C6 C5 H5A 110.6 . . ?
C6 C5 H5B 110.6 . . ?
C5 C6 C5 107.2(10) . 9_656 ?
C5 C6 H6A 110.3 9_656 . ?
C5 C6 H6A 110.3 . . ?
C5 C6 H6B 110.3 9_656 . ?
C5 C6 H6B 110.3 . . ?
H6A C6 H6B 108.5 . . ?

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
N1 C4 C5 C6 -152.9(7) . . . . ?
C1 C2 C3 N1 -171.4(8) . . . . ?
C1 C2 C3 N1 9.3(12) 87_546 . . . ?
C4 N1 C3 C2 -177.8(7) . . . . ?
C4 C4 C5 C6 -31.0(9) 9_656 . . . ?
C4 C5 C6 C5 12.0(4) . . . 9_656 ?
C2 C1 C2 C1 -0.2(15) 40_655 . . 87_546 ?
C2 C1 C2 C3 -179.5(6) 40_655 . . . ?
C3 N1 C4 C4 120.1(9) . . . 9_656 ?
C3 N1 C4 C5 -122.8(8) . . . . ?

_database_code_depnum_ccdc_archive 'CCDC 991218'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_CC4_Para_Xylene_Solvate_100K
_audit_creation_date             2014-01-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '2(H2 O), C66 H72 N12, 3(C8 H10)'
_chemical_formula_sum            'C90 H106 N12 O2'
_chemical_formula_weight         1387.87
_chemical_absolute_configuration unk
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 'x+1/2, -y+1/2, -z'
4 '-x, y+1/2, -z+1/2'

_cell_length_a                   16.7488(15)
_cell_length_b                   19.2538(19)
_cell_length_c                   25.342(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8172.1(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9644
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.622
_cell_measurement_theta_min      2.263
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.4631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1250 before and 0.0745 after correction.
The Ratio of minimum to maximum transmission is 0.6215.
The λ/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.039
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            134283
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.61
_diffrn_ambient_temperature      100.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  Rigaku_AFC12K_724P_007HF_Mo
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_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_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                12428
_reflns_number_total             13923
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(2)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         13923
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0698
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1355P)²+5.3349P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1982
_refine_ls_wR_factor_ref         0.2088
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C83A, C83B}
{C84A, C84B}
{C86A, C86B}
{C87A, C87B}
{C85A, C85B}
{C88A, C88B}
3. Restrained distances
 C91-C84A = C89-C83A = C92-C87A = C86A-C90
 1.5 with sigma of 0.02
 C84A-C89 \\sim C88A-C89 \\sim C83A-C91 \\sim C85A-C91 \\sim C88A-C92 \\sim
C86A-C92 \\sim C85A-C90 ~
 C87A-C90
 with sigma of 0.02
4. Restrained planarity
 C91, C87A, C88A, C86A, C92, C83A, C85A, C90, C84A, C89
 with sigma of 0.001
5. Rigid bond restraints
 C81, C75, C76, C80, C77, C79, C78, C82
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
Uiso(C83A) = Uiso(C83B)
Uiso(C87A) = Uiso(C87B)
Uiso(C86A) = Uiso(C86B)
Uiso(C84A) = Uiso(C84B)
Uiso(C88A) = Uiso(C88B)
Uiso(C85A) = Uiso(C85B)
7. Others
 Fixed Sof: C87A(0.5) C88A(0.5) H88A(0.5) C83A(0.5) H83A(0.5) C84A(0.5)
 C85A(0.5) H85A(0.5) C86A(0.5) H86A(0.5) C89(0.5) H89A(0.5) H89B(0.5) H89C(0.5)
 C90(0.5) H90A(0.5) H90B(0.5) H90C(0.5) C91(0.5) H91A(0.5) H91B(0.5) H91C(0.5)
 C92(0.5) H92A(0.5) H92B(0.5) H92C(0.5) C83B(0.5) C84B(0.5) H84B(0.5) C86B(0.5)
 C87B(0.5) H87B(0.5) C85B(0.5) H85B(0.5) C88B(0.5) H88B(0.5)
8.a Ternary CH refined with riding coordinates:
 C37(H37), C41(H41), C42(H42), C46(H46), C47(H47), C51(H51), C52(H52),
 C56(H56), C57(H57), C58(H58), C62(H62), C66(H66)
8.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C43(H43A,H43B), C44(H44A,
 H44B), C45(H45A,H45B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B),
 C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C59(H59A,H59B), C60(H60A,H60B),
  C61(H61A,H61B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B)
8.c Me refined with riding coordinates:
 C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C92(H92A,H92B,
 H92C)
8.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C22(H22), C24(H24), C25(H25), C26(H26),
  C27(H27), C29(H29), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36),
 C68(H68), C69(H69), C71(H71), C72(H72), C76(H76), C77(H77), C79(H79), C80(H80),
  C88A(H88A), C83A(H83A), C85A(H85A), C86A(H86A), C84B(H84B), C87B(H87B),
 C85B(H85B), C88B(H88B)
8.e Fitted hexagon refined as free rotating group:
 C87A(C88A,C83A,C84A,C85A,C86A)
8.f Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C81(H81A,H81B,H81C), C82(H82A,H82B,
 H82C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
O1 O -0.6475(6) -0.5684(5) -0.6653(4) 0.206(4) Uiso 1 1 d . . . .
O2 O -0.4772(4) -0.1559(3) -0.8671(3) 0.1334(19) Uiso 1 1 d . . . .
N1 N -0.51814(17) -0.15707(17) -0.41602(12) 0.0408(7) Uani 1 1 d . . . .
N2 N -0.53746(17) -0.31548(17) -0.40524(11) 0.0385(7) Uani 1 1 d . . . .
N3 N -0.71455(17) -0.02270(14) -0.61494(12) 0.0375(7) Uani 1 1 d . . . .
N4 N -0.79736(17) -0.09384(15) -0.71275(12) 0.0363(6) Uani 1 1 d . . . .
N5 N -0.32868(17) -0.02670(16) -0.61132(12) 0.0386(7) Uani 1 1 d . . . .
N6 N -0.23009(16) -0.12541(15) -0.68151(11) 0.0340(6) Uani 1 1 d . . . .
N7 N -0.33379(17) -0.50851(17) -0.56388(12) 0.0394(7) Uani 1 1 d . . . .
N8 N -0.25107(16) -0.45534(15) -0.66510(11) 0.0348(6) Uani 1 1 d . . . .
N9 N -0.61503(18) -0.31131(15) -0.86624(11) 0.0352(6) Uani 1 1 d . . . .
N10 N -0.43141(18) -0.30108(16) -0.85815(11) 0.0380(7) Uani 1 1 d . . . .
N11 N -0.82030(17) -0.42009(16) -0.67348(12) 0.0372(6) Uani 1 1 d . . . .
N12 N -0.72022(16) -0.49230(16) -0.58249(12) 0.0378(7) Uani 1 1 d . . . .
C1 C -0.5811(2) -0.04457(18) -0.58102(15) 0.0380(8) Uani 1 1 d . . . .
C2 C -0.6037(2) -0.07481(18) -0.53326(15) 0.0375(8) Uani 1 1 d . . . .
H2 H -0.6587 -0.0799 -0.5250 0.045 Uiso 1 1 calc . . R .
C3 C -0.5458(2) -0.09766(19) -0.49756(15) 0.0384(8) Uani 1 1 d . . . .
C4 C -0.4647(2) -0.08808(19) -0.50956(15) 0.0395(8) Uani 1 1 d . . . .
H4 H -0.4251 -0.1022 -0.4850 0.047 Uiso 1 1 calc . . R .
C5 C -0.4418(2) -0.05812(18) -0.55703(15) 0.0368(8) Uani 1 1 d . . . .
C6 C -0.5002(2) -0.03598(17) -0.59201(15) 0.0373(8) Uani 1 1 d . . . .
H6 H -0.4846 -0.0145 -0.6242 0.045 Uiso 1 1 calc . . R .
C7 C -0.6396(2) -0.02066(17) -0.62102(16) 0.0374(8) Uani 1 1 d . . . .
H7 H -0.6195 -0.0026 -0.6533 0.045 Uiso 1 1 calc . . R .
C8 C -0.5687(2) -0.1340(2) -0.44892(15) 0.0406(8) Uani 1 1 d . . . .
H8 H -0.6238 -0.1405 -0.4418 0.049 Uiso 1 1 calc . . R .
C9 C -0.3557(2) -0.05480(19) -0.56976(15) 0.0378(8) Uani 1 1 d . . . .
H9 H -0.3189 -0.0747 -0.5456 0.045 Uiso 1 1 calc . . R .
C10 C -0.2852(2) -0.22073(18) -0.73040(13) 0.0345(7) Uani 1 1 d . . . .
C11 C -0.2563(2) -0.26953(19) -0.69479(13) 0.0366(8) Uani 1 1 d . . . .
H11 H -0.2236 -0.2547 -0.6663 0.044 Uiso 1 1 calc . . R .
C12 C -0.27461(19) -0.33989(19) -0.70015(13) 0.0344(7) Uani 1 1 d . . . .
C13 C -0.3229(2) -0.36033(19) -0.74273(13) 0.0353(7) Uani 1 1 d . . . .
H13 H -0.3359 -0.4080 -0.7471 0.042 Uiso 1 1 calc . . R .
C14 C -0.3517(2) -0.31186(19) -0.77840(13) 0.0355(7) Uani 1 1 d . . . .
C15 C -0.3331(2) -0.2421(2) -0.77218(14) 0.0379(8) Uani 1 1 d . . . .
H15 H -0.3531 -0.2089 -0.7965 0.045 Uiso 1 1 calc . . R .
C16 C -0.2680(2) -0.14590(19) -0.72186(13) 0.0366(8) Uani 1 1 d . . . .
H16 H -0.2856 -0.1128 -0.7471 0.044 Uiso 1 1 calc . . R .
C17 C -0.24523(19) -0.39009(18) -0.66072(13) 0.0335(7) Uani 1 1 d . . . .
H17 H -0.2202 -0.3722 -0.6299 0.040 Uiso 1 1 calc . . R .
C18 C -0.4039(2) -0.33812(18) -0.82094(13) 0.0342(7) Uani 1 1 d . . . .
H18 H -0.4179 -0.3859 -0.8204 0.041 Uiso 1 1 calc . . R .
C19 C -0.6089(2) -0.4501(2) -0.52982(14) 0.0379(8) Uani 1 1 d . . . .
C20 C -0.5490(2) -0.4876(2) -0.55635(15) 0.0402(8) Uani 1 1 d . . . .
H20 H -0.5628 -0.5174 -0.5848 0.048 Uiso 1 1 calc . . R .
C21 C -0.4699(2) -0.4810(2) -0.54092(14) 0.0386(8) Uani 1 1 d . . . .
C22 C -0.4497(2) -0.4382(2) -0.49854(13) 0.0371(8) Uani 1 1 d . . . .
H22 H -0.3955 -0.4341 -0.4879 0.044 Uiso 1 1 calc . . R .
C23 C -0.5086(2) -0.40162(19) -0.47192(14) 0.0365(8) Uani 1 1 d . . . .
C24 C -0.5889(2) -0.4086(2) -0.48784(14) 0.0373(8) Uani 1 1 d . . . .
H24 H -0.6296 -0.3842 -0.4693 0.045 Uiso 1 1 calc . . R .
C25 C -0.6933(2) -0.4527(2) -0.54678(14) 0.0378(8) Uani 1 1 d . . . .
H25 H -0.7300 -0.4224 -0.5297 0.045 Uiso 1 1 calc . . R .
C26 C -0.4080(2) -0.5188(2) -0.57122(15) 0.0386(8) Uani 1 1 d . . . .
H26 H -0.4243 -0.5517 -0.5970 0.046 Uiso 1 1 calc . . R .
C27 C -0.4865(2) -0.35310(18) -0.42925(13) 0.0347(7) Uani 1 1 d . . . .
H27 H -0.4320 -0.3498 -0.4193 0.042 Uiso 1 1 calc . . R .
C28 C -0.7030(2) -0.26565(18) -0.80103(13) 0.0340(7) Uani 1 1 d . . . .
C29 C -0.7175(2) -0.33185(19) -0.78018(14) 0.0379(8) Uani 1 1 d . . . .
H29 H -0.6945 -0.3715 -0.7965 0.045 Uiso 1 1 calc . . R .
C30 C -0.7651(2) -0.33976(18) -0.73593(13) 0.0352(7) Uani 1 1 d . . . .
C31 C -0.7979(2) -0.28161(19) -0.71221(14) 0.0350(7) Uani 1 1 d . . . .
H31 H -0.8311 -0.2871 -0.6821 0.042 Uiso 1 1 calc . . R .
C32 C -0.7832(2) -0.21597(19) -0.73131(14) 0.0350(7) Uani 1 1 d . . . .
C33 C -0.7358(2) -0.20822(18) -0.77669(13) 0.0353(7) Uani 1 1 d . . . .
H33 H -0.7264 -0.1632 -0.7907 0.042 Uiso 1 1 calc . . R .
C34 C -0.6475(2) -0.25864(17) -0.84641(13) 0.0338(7) Uani 1 1 d . . . .
H34 H -0.6366 -0.2140 -0.8606 0.041 Uiso 1 1 calc . . R .
C35 C -0.7756(2) -0.40949(18) -0.71273(13) 0.0373(8) Uani 1 1 d . . . .
H35 H -0.7478 -0.4476 -0.7279 0.045 Uiso 1 1 calc . . R .
C36 C -0.8126(2) -0.15538(18) -0.70111(14) 0.0354(7) Uani 1 1 d . . . .
H36 H -0.8451 -0.1638 -0.6711 0.042 Uiso 1 1 calc . . R .
C37 C -0.5089(2) -0.2674(2) -0.36586(13) 0.0390(8) Uani 1 1 d . . . .
H37 H -0.4496 -0.2629 -0.3687 0.047 Uiso 1 1 calc . . R .
C38 C -0.5315(2) -0.2882(2) -0.30928(14) 0.0441(9) Uani 1 1 d . . . .
H38A H -0.5856 -0.3089 -0.3084 0.053 Uiso 1 1 calc . . R .
H38B H -0.4929 -0.3223 -0.2950 0.053 Uiso 1 1 calc . . R .
C39 C -0.5292(3) -0.2209(2) -0.27747(15) 0.0519(10) Uani 1 1 d . . . .
H39A H -0.4815 -0.2198 -0.2544 0.062 Uiso 1 1 calc . . R .
H39B H -0.5775 -0.2167 -0.2551 0.062 Uiso 1 1 calc . . R .
C40 C -0.5260(2) -0.1618(2) -0.31814(15) 0.0467(9) Uani 1 1 d . . . .
H40A H -0.5650 -0.1249 -0.3092 0.056 Uiso 1 1 calc . . R .
H40B H -0.4719 -0.1411 -0.3196 0.056 Uiso 1 1 calc . . R .
C41 C -0.5473(2) -0.1962(2) -0.37067(14) 0.0413(8) Uani 1 1 d . . . .
H41 H -0.6065 -0.2015 -0.3733 0.050 Uiso 1 1 calc . . R .
C42 C -0.21764(19) -0.49763(19) -0.62270(14) 0.0367(8) Uani 1 1 d . . . .
H42 H -0.1950 -0.4664 -0.5949 0.044 Uiso 1 1 calc . . R .
C43 C -0.1527(2) -0.5471(2) -0.64178(17) 0.0453(9) Uani 1 1 d . . . .
H43A H -0.1002 -0.5234 -0.6427 0.054 Uiso 1 1 calc . . R .
H43B H -0.1651 -0.5646 -0.6776 0.054 Uiso 1 1 calc . . R .
C44 C -0.1520(3) -0.6069(3) -0.6014(2) 0.0802(18) Uani 1 1 d . . . .
H44A H -0.1547 -0.6524 -0.6196 0.096 Uiso 1 1 calc . . DR .
H44B H -0.1028 -0.6054 -0.5798 0.096 Uiso 1 1 calc . . R .
C45 C -0.2257(2) -0.5960(2) -0.56692(16) 0.0449(9) Uani 1 1 d . . . .
H45A H -0.2535 -0.6406 -0.5607 0.054 Uiso 1 1 calc . . R .
H45B H -0.2105 -0.5758 -0.5324 0.054 Uiso 1 1 calc . . R .
C46 C -0.27892(19) -0.54607(18) -0.59758(14) 0.0355(7) Uani 1 1 d . . . .
H46 H -0.3090 -0.5717 -0.6256 0.043 Uiso 1 1 calc . . R .
C47 C -0.4793(2) -0.33833(18) -0.89695(13) 0.0354(7) Uani 1 1 d . . . .
H47 H -0.4897 -0.3866 -0.8842 0.042 Uiso 1 1 calc . . R .
C48 C -0.4399(2) -0.3410(2) -0.95109(14) 0.0423(8) Uani 1 1 d . . . .
H48A H -0.3973 -0.3766 -0.9520 0.051 Uiso 1 1 calc . . R .
H48B H -0.4166 -0.2954 -0.9604 0.051 Uiso 1 1 calc . . R .
C49 C -0.5078(2) -0.3600(2) -0.98891(13) 0.0384(8) Uani 1 1 d . . . .
H49A H -0.5061 -0.4101 -0.9978 0.046 Uiso 1 1 calc . . R .
H49B H -0.5039 -0.3328 -1.0219 0.046 Uiso 1 1 calc . . R .
C50 C -0.5858(2) -0.3419(2) -0.95869(13) 0.0418(8) Uani 1 1 d . . . .
H50A H -0.6212 -0.3128 -0.9808 0.050 Uiso 1 1 calc . . R .
H50B H -0.6149 -0.3847 -0.9487 0.050 Uiso 1 1 calc . . R .
C51 C -0.5591(2) -0.30233(19) -0.90965(12) 0.0334(7) Uani 1 1 d . . . .
H51 H -0.5508 -0.2520 -0.9177 0.040 Uiso 1 1 calc . . R .
C52 C -0.8250(2) -0.4893(2) -0.65210(14) 0.0397(8) Uani 1 1 d . . . .
H52 H -0.7867 -0.5204 -0.6710 0.048 Uiso 1 1 calc . . R .
C53 C -0.9104(3) -0.5196(3) -0.65585(19) 0.0681(15) Uani 1 1 d . . . .
H53A H -0.9491 -0.4825 -0.6647 0.082 Uiso 1 1 calc . . R .
H53B H -0.9129 -0.5557 -0.6836 0.082 Uiso 1 1 calc . . R .
C54 C -0.9296(2) -0.5508(2) -0.60210(17) 0.0510(10) Uani 1 1 d . . . .
H54A H -0.9523 -0.5980 -0.6060 0.061 Uiso 1 1 calc . . R .
H54B H -0.9683 -0.5214 -0.5828 0.061 Uiso 1 1 calc . . R .
C55 C -0.8493(2) -0.5535(2) -0.57266(15) 0.0458(9) Uani 1 1 d . . . .
H55A H -0.8572 -0.5512 -0.5340 0.055 Uiso 1 1 calc . . R .
H55B H -0.8194 -0.5963 -0.5814 0.055 Uiso 1 1 calc . . R .
C56 C -0.8063(2) -0.4891(2) -0.59310(14) 0.0369(8) Uani 1 1 d . . . .
H56 H -0.8295 -0.4466 -0.5764 0.044 Uiso 1 1 calc . . R .
C57 C -0.2183(2) -0.05161(19) -0.67346(14) 0.0379(8) Uani 1 1 d . . . .
H57 H -0.2496 -0.0249 -0.7003 0.045 Uiso 1 1 calc . . R .
C58 C -0.2426(2) -0.02881(19) -0.61827(14) 0.0369(8) Uani 1 1 d . . . .
H58 H -0.2190 -0.0615 -0.5919 0.044 Uiso 1 1 calc . . R .
C59 C -0.2038(2) 0.0423(2) -0.61210(16) 0.0461(9) Uani 1 1 d . . . .
H59A H -0.1897 0.0509 -0.5747 0.055 Uiso 1 1 calc . . R .
H59B H -0.2405 0.0793 -0.6241 0.055 Uiso 1 1 calc . . R .
C60 C -0.1282(2) 0.0406(2) -0.64655(19) 0.0541(10) Uani 1 1 d . . . .
H60A H -0.0797 0.0442 -0.6244 0.065 Uiso 1 1 calc . . R .
H60B H -0.1284 0.0795 -0.6721 0.065 Uiso 1 1 calc . . R .
C61 C -0.1305(2) -0.0298(2) -0.67562(16) 0.0440(9) Uani 1 1 d . . . .
H61A H -0.1123 -0.0247 -0.7126 0.053 Uiso 1 1 calc . . R .
H61B H -0.0962 -0.0644 -0.6577 0.053 Uiso 1 1 calc . . R .
C62 C -0.8284(2) -0.04006(18) -0.67764(15) 0.0358(7) Uani 1 1 d . . . .
H62 H -0.8574 -0.0617 -0.6473 0.043 Uiso 1 1 calc . . R .
C63 C -0.8831(2) 0.0109(2) -0.70679(17) 0.0468(9) Uani 1 1 d . . . .
H63A H -0.8646 0.0177 -0.7436 0.056 Uiso 1 1 calc . . R .
H63B H -0.9386 -0.0066 -0.7075 0.056 Uiso 1 1 calc . . R .
C64 C -0.8783(3) 0.0786(2) -0.6762(2) 0.0622(12) Uani 1 1 d . . . .
H64A H -0.9285 0.0868 -0.6566 0.075 Uiso 1 1 calc . . R .
H64B H -0.8693 0.1180 -0.7005 0.075 Uiso 1 1 calc . . R .
C65 C -0.8081(2) 0.07147(19) -0.63779(17) 0.0473(9) Uani 1 1 d . . . .
H65A H -0.7739 0.1134 -0.6387 0.057 Uiso 1 1 calc . . R .
H65B H -0.8274 0.0643 -0.6013 0.057 Uiso 1 1 calc . . R .
C66 C -0.7622(2) 0.00786(17) -0.65733(15) 0.0374(8) Uani 1 1 d . . . .
H66 H -0.7265 0.0215 -0.6872 0.045 Uiso 1 1 calc . . R .
C67 C -0.8268(3) -0.2600(2) -0.4645(2) 0.0632(12) Uani 1 1 d . . . .
C68 C -0.8537(3) -0.2641(3) -0.5149(2) 0.0689(14) Uani 1 1 d . . . .
H68 H -0.9095 -0.2657 -0.5216 0.083 Uiso 1 1 calc . . R .
C69 C -0.8009(3) -0.2661(4) -0.5565(2) 0.0856(18) Uani 1 1 d . . . .
H69 H -0.8216 -0.2701 -0.5913 0.103 Uiso 1 1 calc . . R .
C70 C -0.7182(3) -0.2626(3) -0.5497(2) 0.0699(13) Uani 1 1 d . . . .
C71 C -0.6913(3) -0.2601(2) -0.4984(2) 0.0622(12) Uani 1 1 d . . . .
H71 H -0.6356 -0.2585 -0.4917 0.075 Uiso 1 1 calc . . R .
C72 C -0.7439(3) -0.2600(3) -0.4565(2) 0.0789(16) Uani 1 1 d . . . .
H72 H -0.7235 -0.2601 -0.4215 0.095 Uiso 1 1 calc . . R .
C73 C -0.8839(4) -0.2591(4) -0.4183(3) 0.0923(19) Uani 1 1 d . . . .
H73A H -0.8676 -0.2942 -0.3924 0.138 Uiso 1 1 calc . . GR .
H73B H -0.9380 -0.2693 -0.4307 0.138 Uiso 1 1 calc . . GR .
H73C H -0.8831 -0.2131 -0.4017 0.138 Uiso 1 1 calc . . GR .
C74 C -0.6610(4) -0.2629(5) -0.5948(3) 0.112(3) Uani 1 1 d . . . .
H74A H -0.6743 -0.2251 -0.6192 0.168 Uiso 1 1 calc . . GR .
H74B H -0.6645 -0.3075 -0.6133 0.168 Uiso 1 1 calc . . GR .
H74C H -0.6066 -0.2563 -0.5814 0.168 Uiso 1 1 calc . . GR .
C75 C -0.5209(3) -0.0985(5) -0.7364(3) 0.103(2) Uani 1 1 d . . . U
C76 C -0.5671(5) -0.0609(5) -0.7740(4) 0.131(3) Uani 1 1 d . . . U
H76 H -0.6137 -0.0830 -0.7872 0.157 Uiso 1 1 calc . . R .
C77 C -0.5507(4) 0.0034(5) -0.7927(3) 0.110(2) Uani 1 1 d . . . U
H77 H -0.5853 0.0250 -0.8174 0.132 Uiso 1 1 calc . . R .
C78 C -0.4841(3) 0.0365(5) -0.7756(2) 0.101(2) Uani 1 1 d . . . U
C79 C -0.4362(3) 0.0040(5) -0.7386(2) 0.114(3) Uani 1 1 d . . . U
H79 H -0.3909 0.0278 -0.7252 0.137 Uiso 1 1 calc . . R .
C80 C -0.4529(3) -0.0624(5) -0.7205(2) 0.099(2) Uani 1 1 d . . . U
H80 H -0.4169 -0.0840 -0.6967 0.119 Uiso 1 1 calc . . R .
C81 C -0.5392(6) -0.1703(7) -0.7158(5) 0.161(4) Uani 1 1 d . . . U
H81A H -0.5243 -0.2049 -0.7423 0.241 Uiso 1 1 calc . . GR .
H81B H -0.5964 -0.1740 -0.7082 0.241 Uiso 1 1 calc . . GR .
H81C H -0.5087 -0.1786 -0.6833 0.241 Uiso 1 1 calc . . GR .
C82 C -0.4650(4) 0.1055(6) -0.7965(4) 0.139(3) Uani 1 1 d . . . U
H82A H -0.4963 0.1139 -0.8285 0.209 Uiso 1 1 calc . . GR .
H82B H -0.4080 0.1078 -0.8049 0.209 Uiso 1 1 calc . . GR .
H82C H -0.4780 0.1408 -0.7700 0.209 Uiso 1 1 calc . . GR .
C87A C -0.4067(3) -0.7462(2) -0.38669(18) 0.113(2) Uiso 0.50 1 d A 1 D .
C88A C -0.4884(3) -0.7457(2) -0.37703(16) 0.104(2) Uiso 0.50 1 d A 1 G .
H88A H -0.5091 -0.7677 -0.3464 0.125 Uiso 0.50 1 calc A 1 R .
C83A C -0.5398(2) -0.7130(3) -0.41220(19) 0.115(2) Uiso 0.50 1 d A 1 DG .
H83A H -0.5956 -0.7127 -0.4056 0.138 Uiso 0.50 1 calc A 1 R .
C84A C -0.5095(3) -0.6808(2) -0.45702(17) 0.132(3) Uiso 0.50 1 d A 1 DG .
C85A C -0.4278(3) -0.6813(2) -0.46668(17) 0.135(3) Uiso 0.50 1 d A 1 G .
H85A H -0.4071 -0.6593 -0.4973 0.162 Uiso 0.50 1 calc A 1 R .
C86A C -0.3764(3) -0.7140(3) -0.4315(2) 0.131(3) Uiso 0.50 1 d A 1 DG .
H86A H -0.3206 -0.7144 -0.4381 0.158 Uiso 0.50 1 calc A 1 R .
C89 C -0.6283(4) -0.7099(5) -0.4049(5) 0.233(14) Uiso 0.50 1 d B 2 D .
H89A H -0.6503 -0.6722 -0.4265 0.350 Uiso 0.50 1 calc B 2 R .
H89B H -0.6406 -0.7014 -0.3677 0.350 Uiso 0.50 1 calc B 2 R .
H89C H -0.6521 -0.7542 -0.4159 0.350 Uiso 0.50 1 calc B 2 DR .
C90 C -0.2869(4) -0.7196(6) -0.4358(6) 0.188(10) Uiso 0.50 1 d B 2 D .
H90A H -0.2654 -0.7400 -0.4033 0.282 Uiso 0.50 1 calc B 2 R .
H90B H -0.2640 -0.6732 -0.4409 0.282 Uiso 0.50 1 calc B 2 R .
H90C H -0.2730 -0.7492 -0.4659 0.282 Uiso 0.50 1 calc B 2 R .
C91 C -0.5722(7) -0.6478(4) -0.4911(4) 0.123(5) Uiso 0.50 1 d A 1 D .
H91A H -0.6245 -0.6525 -0.4742 0.184 Uiso 0.50 1 calc A 1 R .
H91B H -0.5732 -0.6709 -0.5256 0.184 Uiso 0.50 1 calc A 1 R .
H91C H -0.5598 -0.5984 -0.4959 0.184 Uiso 0.50 1 calc A 1 R .
C92 C -0.3451(7) -0.7793(4) -0.3524(4) 0.123(5) Uiso 0.50 1 d A 1 D .
H92A H -0.3714 -0.8046 -0.3237 0.185 Uiso 0.50 1 calc A 1 R .
H92B H -0.3103 -0.7433 -0.3375 0.185 Uiso 0.50 1 calc A 1 R .
H92C H -0.3131 -0.8117 -0.3734 0.185 Uiso 0.50 1 calc A 1 R .
C83B C -0.5398(2) -0.7130(3) -0.41220(19) 0.115(2) Uiso 0.50 1 d B 2 . .
C84B C -0.5095(3) -0.6808(2) -0.45702(17) 0.132(3) Uiso 0.50 1 d B 2 . .
H84B H -0.5446 -0.6584 -0.4811 0.158 Uiso 0.50 1 calc B 2 R .
C86B C -0.3764(3) -0.7140(3) -0.4315(2) 0.131(3) Uiso 0.50 1 d B 2 . .
C87B C -0.4067(3) -0.7462(2) -0.38669(18) 0.113(2) Uiso 0.50 1 d B 2 . .
H87B H -0.3716 -0.7686 -0.3627 0.136 Uiso 0.50 1 calc B 2 R .
C85B C -0.4278(3) -0.6813(2) -0.46668(17) 0.135(3) Uiso 0.50 1 d B 2 . .
H85B H -0.4071 -0.6593 -0.4973 0.162 Uiso 0.50 1 calc B 2 R .
C88B C -0.4884(3) -0.7457(2) -0.37703(16) 0.104(2) Uiso 0.50 1 d B 2 . .
H88B H -0.5091 -0.7677 -0.3464 0.125 Uiso 0.50 1 calc B 2 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
N1 C8 1.268(5) . ?
N1 C41 1.458(5) . ?
N2 C27 1.274(5) . ?
N2 C37 1.443(5) . ?
N3 C7 1.265(5) . ?
N3 C66 1.462(5) . ?
N4 C36 1.247(5) . ?
N4 C62 1.461(4) . ?
N5 C9 1.268(5) . ?
N5 C58 1.453(4) . ?
N6 C16 1.266(4) . ?
N6 C57 1.449(5) . ?
N7 C26 1.273(5) . ?
N7 C46 1.448(5) . ?
N8 C17 1.265(5) . ?
N8 C42 1.460(4) . ?
N9 C34 1.256(4) . ?
N9 C51 1.456(4) . ?
N10 C18 1.269(5) . ?
N10 C47 1.457(4) . ?
N11 C35 1.261(5) . ?
N11 C52 1.441(5) . ?
N12 C25 1.267(5) . ?
N12 C56 1.468(4) . ?
C1 C2 1.395(6) . ?
C1 C6 1.393(5) . ?
C1 C7 1.484(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.397(5) . ?
C3 C4 1.404(5) . ?
C3 C8 1.468(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.388(5) . ?
C5 C6 1.387(5) . ?
C5 C9 1.479(5) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.390(5) . ?
C10 C15 1.390(5) . ?
C10 C16 1.485(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.396(5) . ?
C12 C13 1.405(5) . ?
C12 C17 1.475(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.386(5) . ?
C14 C15 1.387(5) . ?
C14 C18 1.478(5) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.407(5) . ?
C19 C24 1.372(5) . ?
C19 C25 1.479(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.387(5) . ?
C21 C22 1.396(5) . ?
C21 C26 1.481(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.388(5) . ?
C23 C24 1.410(5) . ?
C23 C27 1.476(5) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.401(5) . ?
C28 C33 1.381(5) . ?
C28 C34 1.484(5) . ?
C29 H29 0.9500 . ?
C29 C30 1.385(5) . ?
C30 C31 1.384(5) . ?
C30 C35 1.476(5) . ?
C31 H31 0.9500 . ?
C31 C32 1.375(5) . ?
C32 C33 1.405(5) . ?
C32 C36 1.480(5) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 H37 1.0000 . ?
C37 C38 1.536(5) . ?
C37 C41 1.520(6) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.527(6) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.537(6) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.529(5) . ?
C41 H41 1.0000 . ?
C42 H42 1.0000 . ?
C42 C43 1.525(5) . ?
C42 C46 1.526(5) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.541(6) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.526(6) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.524(5) . ?
C46 H46 1.0000 . ?
C47 H47 1.0000 . ?
C47 C48 1.523(5) . ?
C47 C51 1.539(5) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.531(5) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.554(5) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C50 C51 1.525(5) . ?
C51 H51 1.0000 . ?
C52 H52 1.0000 . ?
C52 C53 1.547(5) . ?
C52 C56 1.528(5) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.523(6) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C54 C55 1.538(5) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 C56 1.525(5) . ?
C56 H56 1.0000 . ?
C57 H57 1.0000 . ?
C57 C58 1.521(5) . ?
C57 C61 1.531(5) . ?
C58 H58 1.0000 . ?
C58 C59 1.523(5) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.538(6) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C60 C61 1.543(6) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62 1.0000 . ?
C62 C63 1.533(5) . ?
C62 C66 1.531(5) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.518(6) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C64 C65 1.532(6) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C65 C66 1.529(5) . ?
C66 H66 1.0000 . ?
C67 C68 1.357(7) . ?
C67 C72 1.404(7) . ?
C67 C73 1.512(8) . ?
C68 H68 0.9500 . ?
C68 C69 1.376(9) . ?
C69 H69 0.9500 . ?
C69 C70 1.397(8) . ?
C70 C71 1.379(7) . ?
C70 C74 1.490(9) . ?
C71 H71 0.9500 . ?
C71 C72 1.378(8) . ?
C72 H72 0.9500 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 C76 1.426(11) . ?
C75 C80 1.392(10) . ?
C75 C81 1.510(14) . ?
C76 H76 0.9500 . ?
C76 C77 1.352(13) . ?
C77 H77 0.9500 . ?
C77 C78 1.355(10) . ?
C78 C79 1.383(9) . ?
C78 C82 1.466(13) . ?
C79 H79 0.9500 . ?
C79 C80 1.387(12) . ?
C80 H80 0.9500 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C87A C88A 1.3900 . ?
C87A C86A 1.3900 . ?
C87A C92 1.492(5) . ?
C88A H88A 0.9500 . ?
C88A C83A 1.3900 . ?
C83A H83A 0.9500 . ?
C83A C84A 1.3900 . ?
C84A C85A 1.3900 . ?
C84A C91 1.502(5) . ?
C85A H85A 0.9500 . ?
C85A C86A 1.3900 . ?
C86A H86A 0.9500 . ?
C89 H89A 0.9800 . ?
C89 H89B 0.9800 . ?
C89 H89C 0.9800 . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 0.9800 . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 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
C8 N1 C41 118.4(3) . . ?
C27 N2 C37 118.2(3) . . ?
C7 N3 C66 116.1(3) . . ?
C36 N4 C62 117.2(3) . . ?
C9 N5 C58 116.3(3) . . ?
C16 N6 C57 119.2(3) . . ?
C26 N7 C46 117.1(3) . . ?
C17 N8 C42 117.4(3) . . ?
C34 N9 C51 119.0(3) . . ?
C18 N10 C47 115.1(3) . . ?
C35 N11 C52 118.6(3) . . ?
C25 N12 C56 117.1(3) . . ?
C2 C1 C7 122.9(3) . . ?
C6 C1 C2 119.1(3) . . ?
C6 C1 C7 118.0(3) . . ?
C1 C2 H2 119.8 . . ?
C1 C2 C3 120.3(3) . . ?
C3 C2 H2 119.8 . . ?
C2 C3 C4 119.3(4) . . ?
C2 C3 C8 120.9(3) . . ?
C4 C3 C8 119.8(3) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.6(3) . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C9 118.5(3) . . ?
C6 C5 C4 119.1(3) . . ?
C6 C5 C9 122.3(3) . . ?
C1 C6 H6 119.3 . . ?
C5 C6 C1 121.4(4) . . ?
C5 C6 H6 119.3 . . ?
N3 C7 C1 124.3(4) . . ?
N3 C7 H7 117.9 . . ?
C1 C7 H7 117.9 . . ?
N1 C8 C3 123.0(3) . . ?
N1 C8 H8 118.5 . . ?
C3 C8 H8 118.5 . . ?
N5 C9 C5 123.2(3) . . ?
N5 C9 H9 118.4 . . ?
C5 C9 H9 118.4 . . ?
C11 C10 C15 119.7(3) . . ?
C11 C10 C16 119.6(3) . . ?
C15 C10 C16 120.7(3) . . ?
C10 C11 H11 119.4 . . ?
C10 C11 C12 121.1(3) . . ?
C12 C11 H11 119.4 . . ?
C11 C12 C13 118.2(3) . . ?
C11 C12 C17 119.8(3) . . ?
C13 C12 C17 121.9(3) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 C12 120.8(3) . . ?
C14 C13 H13 119.6 . . ?
C13 C14 C15 120.0(3) . . ?
C13 C14 C18 116.8(3) . . ?
C15 C14 C18 123.2(3) . . ?
C10 C15 H15 119.9 . . ?
C14 C15 C10 120.2(3) . . ?
C14 C15 H15 119.9 . . ?
N6 C16 C10 121.2(3) . . ?
N6 C16 H16 119.4 . . ?
C10 C16 H16 119.4 . . ?
N8 C17 C12 124.5(3) . . ?
N8 C17 H17 117.8 . . ?
C12 C17 H17 117.8 . . ?
N10 C18 C14 124.4(3) . . ?
N10 C18 H18 117.8 . . ?
C14 C18 H18 117.8 . . ?
C20 C19 C25 121.7(3) . . ?
C24 C19 C20 119.8(3) . . ?
C24 C19 C25 118.5(3) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 C19 119.9(3) . . ?
C21 C20 H20 120.0 . . ?
C20 C21 C22 120.2(3) . . ?
C20 C21 C26 118.5(3) . . ?
C22 C21 C26 121.2(3) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 C21 120.1(3) . . ?
C23 C22 H22 120.0 . . ?
C22 C23 C24 119.4(3) . . ?
C22 C23 C27 120.0(3) . . ?
C24 C23 C27 120.6(3) . . ?
C19 C24 C23 120.6(3) . . ?
C19 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
N12 C25 C19 124.6(3) . . ?
N12 C25 H25 117.7 . . ?
C19 C25 H25 117.7 . . ?
N7 C26 C21 122.2(3) . . ?
N7 C26 H26 118.9 . . ?
C21 C26 H26 118.9 . . ?
N2 C27 C23 122.8(3) . . ?
N2 C27 H27 118.6 . . ?
C23 C27 H27 118.6 . . ?
C29 C28 C34 118.9(3) . . ?
C33 C28 C29 119.4(3) . . ?
C33 C28 C34 121.5(3) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 C28 120.4(3) . . ?
C30 C29 H29 119.8 . . ?
C29 C30 C35 119.4(3) . . ?
C31 C30 C29 119.4(3) . . ?
C31 C30 C35 121.0(3) . . ?
C30 C31 H31 119.3 . . ?
C32 C31 C30 121.3(3) . . ?
C32 C31 H31 119.3 . . ?
C31 C32 C33 119.1(3) . . ?
C31 C32 C36 118.9(3) . . ?
C33 C32 C36 121.8(3) . . ?
C28 C33 C32 120.4(3) . . ?
C28 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
N9 C34 C28 120.5(3) . . ?
N9 C34 H34 119.7 . . ?
C28 C34 H34 119.7 . . ?
N11 C35 C30 122.1(3) . . ?
N11 C35 H35 118.9 . . ?
C30 C35 H35 118.9 . . ?
N4 C36 C32 123.9(3) . . ?
N4 C36 H36 118.0 . . ?
C32 C36 H36 118.0 . . ?
N2 C37 H37 109.6 . . ?
N2 C37 C38 113.3(3) . . ?
N2 C37 C41 112.5(3) . . ?
C38 C37 H37 109.6 . . ?
C41 C37 H37 109.6 . . ?
C41 C37 C38 101.9(3) . . ?
C37 C38 H38A 110.7 . . ?
C37 C38 H38B 110.7 . . ?
H38A C38 H38B 108.8 . . ?
C39 C38 C37 105.4(3) . . ?
C39 C38 H38A 110.7 . . ?
C39 C38 H38B 110.7 . . ?
C38 C39 H39A 110.5 . . ?
C38 C39 H39B 110.5 . . ?
C38 C39 C40 106.0(3) . . ?
H39A C39 H39B 108.7 . . ?
C40 C39 H39A 110.5 . . ?
C40 C39 H39B 110.5 . . ?
C39 C40 H40A 110.8 . . ?
C39 C40 H40B 110.8 . . ?
H40A C40 H40B 108.9 . . ?
C41 C40 C39 104.8(3) . . ?
C41 C40 H40A 110.8 . . ?
C41 C40 H40B 110.8 . . ?
N1 C41 C37 112.8(3) . . ?
N1 C41 C40 112.6(3) . . ?
N1 C41 H41 109.4 . . ?
C37 C41 C40 102.8(3) . . ?
C37 C41 H41 109.4 . . ?
C40 C41 H41 109.4 . . ?
N8 C42 H42 109.2 . . ?
N8 C42 C43 112.9(3) . . ?
N8 C42 C46 113.0(3) . . ?
C43 C42 H42 109.2 . . ?
C43 C42 C46 103.4(3) . . ?
C46 C42 H42 109.2 . . ?
C42 C43 H43A 110.7 . . ?
C42 C43 H43B 110.7 . . ?
C42 C43 C44 105.2(3) . . ?
H43A C43 H43B 108.8 . . ?
C44 C43 H43A 110.7 . . ?
C44 C43 H43B 110.7 . . ?
C43 C44 H44A 110.6 . . ?
C43 C44 H44B 110.6 . . ?
H44A C44 H44B 108.7 . . ?
C45 C44 C43 105.7(3) . . ?
C45 C44 H44A 110.6 . . ?
C45 C44 H44B 110.6 . . ?
C44 C45 H45A 110.6 . . ?
C44 C45 H45B 110.6 . . ?
H45A C45 H45B 108.8 . . ?
C46 C45 C44 105.5(3) . . ?
C46 C45 H45A 110.6 . . ?
C46 C45 H45B 110.6 . . ?
N7 C46 C42 111.6(3) . . ?
N7 C46 C45 112.7(3) . . ?
N7 C46 H46 110.2 . . ?
C42 C46 H46 110.2 . . ?
C45 C46 C42 101.8(3) . . ?
C45 C46 H46 110.2 . . ?
N10 C47 H47 109.6 . . ?
N10 C47 C48 112.7(3) . . ?
N10 C47 C51 113.4(3) . . ?
C48 C47 H47 109.6 . . ?
C48 C47 C51 101.7(3) . . ?
C51 C47 H47 109.6 . . ?
C47 C48 H48A 110.8 . . ?
C47 C48 H48B 110.8 . . ?
C47 C48 C49 104.5(3) . . ?
H48A C48 H48B 108.9 . . ?
C49 C48 H48A 110.8 . . ?
C49 C48 H48B 110.8 . . ?
C48 C49 H49A 110.7 . . ?
C48 C49 H49B 110.7 . . ?
C48 C49 C50 105.2(3) . . ?
H49A C49 H49B 108.8 . . ?
C50 C49 H49A 110.7 . . ?
C50 C49 H49B 110.7 . . ?
C49 C50 H50A 110.7 . . ?
C49 C50 H50B 110.7 . . ?
H50A C50 H50B 108.8 . . ?
C51 C50 C49 105.5(3) . . ?
C51 C50 H50A 110.7 . . ?
C51 C50 H50B 110.7 . . ?
N9 C51 C47 110.3(3) . . ?
N9 C51 C50 111.5(3) . . ?
N9 C51 H51 111.0 . . ?
C47 C51 H51 111.0 . . ?
C50 C51 C47 101.6(3) . . ?
C50 C51 H51 111.0 . . ?
N11 C52 H52 109.8 . . ?
N11 C52 C53 112.1(3) . . ?
N11 C52 C56 110.7(3) . . ?
C53 C52 H52 109.8 . . ?
C56 C52 H52 109.8 . . ?
C56 C52 C53 104.5(3) . . ?
C52 C53 H53A 110.4 . . ?
C52 C53 H53B 110.4 . . ?
H53A C53 H53B 108.6 . . ?
C54 C53 C52 106.8(3) . . ?
C54 C53 H53A 110.4 . . ?
C54 C53 H53B 110.4 . . ?
C53 C54 H54A 110.7 . . ?
C53 C54 H54B 110.7 . . ?
C53 C54 C55 105.2(3) . . ?
H54A C54 H54B 108.8 . . ?
C55 C54 H54A 110.7 . . ?
C55 C54 H54B 110.7 . . ?
C54 C55 H55A 111.2 . . ?
C54 C55 H55B 111.2 . . ?
H55A C55 H55B 109.1 . . ?
C56 C55 C54 102.8(3) . . ?
C56 C55 H55A 111.2 . . ?
C56 C55 H55B 111.2 . . ?
N12 C56 C52 112.4(3) . . ?
N12 C56 C55 111.6(3) . . ?
N12 C56 H56 109.7 . . ?
C52 C56 H56 109.7 . . ?
C55 C56 C52 103.5(3) . . ?
C55 C56 H56 109.7 . . ?
N6 C57 H57 109.7 . . ?
N6 C57 C58 112.1(3) . . ?
N6 C57 C61 113.2(3) . . ?
C58 C57 H57 109.7 . . ?
C58 C57 C61 102.1(3) . . ?
C61 C57 H57 109.7 . . ?
N5 C58 C57 112.6(3) . . ?
N5 C58 H58 109.2 . . ?
N5 C58 C59 112.7(3) . . ?
C57 C58 H58 109.2 . . ?
C57 C58 C59 103.9(3) . . ?
C59 C58 H58 109.2 . . ?
C58 C59 H59A 110.6 . . ?
C58 C59 H59B 110.6 . . ?
C58 C59 C60 105.9(3) . . ?
H59A C59 H59B 108.7 . . ?
C60 C59 H59A 110.6 . . ?
C60 C59 H59B 110.6 . . ?
C59 C60 H60A 110.6 . . ?
C59 C60 H60B 110.6 . . ?
C59 C60 C61 105.6(3) . . ?
H60A C60 H60B 108.8 . . ?
C61 C60 H60A 110.6 . . ?
C61 C60 H60B 110.6 . . ?
C57 C61 C60 104.3(3) . . ?
C57 C61 H61A 110.9 . . ?
C57 C61 H61B 110.9 . . ?
C60 C61 H61A 110.9 . . ?
C60 C61 H61B 110.9 . . ?
H61A C61 H61B 108.9 . . ?
N4 C62 H62 110.2 . . ?
N4 C62 C63 111.9(3) . . ?
N4 C62 C66 112.0(3) . . ?
C63 C62 H62 110.2 . . ?
C66 C62 H62 110.2 . . ?
C66 C62 C63 102.0(3) . . ?
C62 C63 H63A 110.6 . . ?
C62 C63 H63B 110.6 . . ?
H63A C63 H63B 108.7 . . ?
C64 C63 C62 105.8(3) . . ?
C64 C63 H63A 110.6 . . ?
C64 C63 H63B 110.6 . . ?
C63 C64 H64A 110.4 . . ?
C63 C64 H64B 110.4 . . ?
C63 C64 C65 106.8(3) . . ?
H64A C64 H64B 108.6 . . ?
C65 C64 H64A 110.4 . . ?
C65 C64 H64B 110.4 . . ?
C64 C65 H65A 110.8 . . ?
C64 C65 H65B 110.8 . . ?
H65A C65 H65B 108.9 . . ?
C66 C65 C64 104.6(3) . . ?
C66 C65 H65A 110.8 . . ?
C66 C65 H65B 110.8 . . ?
N3 C66 C62 113.5(3) . . ?
N3 C66 C65 111.0(3) . . ?
N3 C66 H66 109.6 . . ?
C62 C66 H66 109.6 . . ?
C65 C66 C62 103.1(3) . . ?
C65 C66 H66 109.6 . . ?
C68 C67 C72 117.6(5) . . ?
C68 C67 C73 121.4(5) . . ?
C72 C67 C73 120.9(5) . . ?
C67 C68 H68 119.7 . . ?
C67 C68 C69 120.6(5) . . ?
C69 C68 H68 119.7 . . ?
C68 C69 H69 118.6 . . ?
C68 C69 C70 122.8(5) . . ?
C70 C69 H69 118.6 . . ?
C69 C70 C74 122.9(5) . . ?
C71 C70 C69 116.2(5) . . ?
C71 C70 C74 120.9(5) . . ?
C70 C71 H71 119.4 . . ?
C72 C71 C70 121.2(5) . . ?
C72 C71 H71 119.4 . . ?
C67 C72 H72 119.3 . . ?
C71 C72 C67 121.4(5) . . ?
C71 C72 H72 119.3 . . ?
C67 C73 H73A 109.5 . . ?
C67 C73 H73B 109.5 . . ?
C67 C73 H73C 109.5 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C70 C74 H74A 109.5 . . ?
C70 C74 H74B 109.5 . . ?
C70 C74 H74C 109.5 . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C76 C75 C81 125.9(7) . . ?
C80 C75 C76 112.5(9) . . ?
C80 C75 C81 121.5(7) . . ?
C75 C76 H76 117.0 . . ?
C77 C76 C75 126.0(7) . . ?
C77 C76 H76 117.0 . . ?
C76 C77 H77 120.5 . . ?
C76 C77 C78 119.0(7) . . ?
C78 C77 H77 120.5 . . ?
C77 C78 C79 118.8(9) . . ?
C77 C78 C82 119.4(7) . . ?
C79 C78 C82 121.9(7) . . ?
C78 C79 H79 119.2 . . ?
C78 C79 C80 121.6(7) . . ?
C80 C79 H79 119.2 . . ?
C75 C80 H80 119.0 . . ?
C79 C80 C75 122.0(6) . . ?
C79 C80 H80 119.0 . . ?
C75 C81 H81A 109.5 . . ?
C75 C81 H81B 109.5 . . ?
C75 C81 H81C 109.5 . . ?
H81A C81 H81B 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C78 C82 H82A 109.5 . . ?
C78 C82 H82B 109.5 . . ?
C78 C82 H82C 109.5 . . ?
H82A C82 H82B 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C88A C87A C86A 120.0 . . ?
C88A C87A C92 125.5(6) . . ?
C86A C87A C92 114.5(6) . . ?
C87A C88A H88A 120.0 . . ?
C87A C88A C83A 120.0 . . ?
C83A C88A H88A 120.0 . . ?
C88A C83A H83A 120.0 . . ?
C88A C83A C84A 120.0 . . ?
C84A C83A H83A 120.0 . . ?
C83A C84A C91 113.8(6) . . ?
C85A C84A C83A 120.0 . . ?
C85A C84A C91 126.2(6) . . ?
C84A C85A H85A 120.0 . . ?
C86A C85A C84A 120.0 . . ?
C86A C85A H85A 120.0 . . ?
C87A C86A H86A 120.0 . . ?
C85A C86A C87A 120.0 . . ?
C85A C86A H86A 120.0 . . ?
H89A C89 H89B 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
H90A C90 H90B 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
C84A C91 H91A 109.5 . . ?
C84A C91 H91B 109.5 . . ?
C84A C91 H91C 109.5 . . ?
H91A C91 H91B 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
C87A C92 H92A 109.5 . . ?
C87A C92 H92B 109.5 . . ?
C87A C92 H92C 109.5 . . ?
H92A C92 H92B 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 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
N2 C37 C38 C39 -156.7(3) . . . . ?
N2 C37 C41 N1 -72.8(4) . . . . ?
N2 C37 C41 C40 165.6(3) . . . . ?
N4 C62 C63 C64 -153.5(3) . . . . ?
N4 C62 C66 N3 -77.7(4) . . . . ?
N4 C62 C66 C65 162.1(3) . . . . ?
N5 C58 C59 C60 -151.6(3) . . . . ?
N6 C57 C58 N5 -74.0(4) . . . . ?
N6 C57 C58 C59 163.7(3) . . . . ?
N6 C57 C61 C60 -159.6(3) . . . . ?
N8 C42 C43 C44 -155.1(4) . . . . ?
N8 C42 C46 N7 -74.3(4) . . . . ?
N8 C42 C46 C45 165.3(3) . . . . ?
N10 C47 C48 C49 -162.5(3) . . . . ?
N10 C47 C51 N9 -74.2(4) . . . . ?
N10 C47 C51 C50 167.5(3) . . . . ?
N11 C52 C53 C54 -132.9(4) . . . . ?
N11 C52 C56 N12 -84.6(4) . . . . ?
N11 C52 C56 C55 154.8(3) . . . . ?
C1 C2 C3 C4 1.8(5) . . . . ?
C1 C2 C3 C8 -175.7(3) . . . . ?
C2 C1 C6 C5 1.4(5) . . . . ?
C2 C1 C7 N3 3.0(5) . . . . ?
C2 C3 C4 C5 -1.9(5) . . . . ?
C2 C3 C8 N1 178.3(3) . . . . ?
C3 C4 C5 C6 1.7(5) . . . . ?
C3 C4 C5 C9 -174.7(3) . . . . ?
C4 C3 C8 N1 0.8(5) . . . . ?
C4 C5 C6 C1 -1.4(5) . . . . ?
C4 C5 C9 N5 -177.9(3) . . . . ?
C6 C1 C2 C3 -1.5(5) . . . . ?
C6 C1 C7 N3 -176.8(3) . . . . ?
C6 C5 C9 N5 5.8(5) . . . . ?
C7 N3 C66 C62 129.2(3) . . . . ?
C7 N3 C66 C65 -115.1(4) . . . . ?
C7 C1 C2 C3 178.7(3) . . . . ?
C7 C1 C6 C5 -178.8(3) . . . . ?
C8 N1 C41 C37 125.2(3) . . . . ?
C8 N1 C41 C40 -118.9(4) . . . . ?
C8 C3 C4 C5 175.6(3) . . . . ?
C9 N5 C58 C57 133.1(3) . . . . ?
C9 N5 C58 C59 -109.8(4) . . . . ?
C9 C5 C6 C1 174.9(3) . . . . ?
C10 C11 C12 C13 0.3(5) . . . . ?
C10 C11 C12 C17 -178.0(3) . . . . ?
C11 C10 C15 C14 -0.2(5) . . . . ?
C11 C10 C16 N6 -2.9(5) . . . . ?
C11 C12 C13 C14 -0.1(5) . . . . ?
C11 C12 C17 N8 -171.9(3) . . . . ?
C12 C13 C14 C15 -0.2(5) . . . . ?
C12 C13 C14 C18 -178.2(3) . . . . ?
C13 C12 C17 N8 9.9(5) . . . . ?
C13 C14 C15 C10 0.3(5) . . . . ?
C13 C14 C18 N10 -176.0(3) . . . . ?
C15 C10 C11 C12 -0.1(5) . . . . ?
C15 C10 C16 N6 174.0(3) . . . . ?
C15 C14 C18 N10 6.0(5) . . . . ?
C16 N6 C57 C58 129.6(3) . . . . ?
C16 N6 C57 C61 -115.5(4) . . . . ?
C16 C10 C11 C12 176.9(3) . . . . ?
C16 C10 C15 C14 -177.1(3) . . . . ?
C17 N8 C42 C43 -120.4(4) . . . . ?
C17 N8 C42 C46 122.8(3) . . . . ?
C17 C12 C13 C14 178.1(3) . . . . ?
C18 N10 C47 C48 -113.2(4) . . . . ?
C18 N10 C47 C51 131.9(3) . . . . ?
C18 C14 C15 C10 178.3(3) . . . . ?
C19 C20 C21 C22 1.1(6) . . . . ?
C19 C20 C21 C26 -177.3(4) . . . . ?
C20 C19 C24 C23 1.8(6) . . . . ?
C20 C19 C25 N12 6.5(6) . . . . ?
C20 C21 C22 C23 -0.5(6) . . . . ?
C20 C21 C26 N7 170.8(4) . . . . ?
C21 C22 C23 C24 0.5(5) . . . . ?
C21 C22 C23 C27 -176.3(3) . . . . ?
C22 C21 C26 N7 -7.5(6) . . . . ?
C22 C23 C24 C19 -1.1(5) . . . . ?
C22 C23 C27 N2 176.3(3) . . . . ?
C24 C19 C20 C21 -1.8(6) . . . . ?
C24 C19 C25 N12 -175.0(4) . . . . ?
C24 C23 C27 N2 -0.4(5) . . . . ?
C25 N12 C56 C52 136.8(4) . . . . ?
C25 N12 C56 C55 -107.4(4) . . . . ?
C25 C19 C20 C21 176.7(4) . . . . ?
C25 C19 C24 C23 -176.7(3) . . . . ?
C26 N7 C46 C42 129.2(4) . . . . ?
C26 N7 C46 C45 -117.0(4) . . . . ?
C26 C21 C22 C23 177.8(3) . . . . ?
C27 N2 C37 C38 -109.9(4) . . . . ?
C27 N2 C37 C41 135.1(3) . . . . ?
C27 C23 C24 C19 175.6(3) . . . . ?
C28 C29 C30 C31 -0.5(5) . . . . ?
C28 C29 C30 C35 -176.3(3) . . . . ?
C29 C28 C33 C32 0.2(5) . . . . ?
C29 C28 C34 N9 1.0(5) . . . . ?
C29 C30 C31 C32 -0.8(5) . . . . ?
C29 C30 C35 N11 -177.7(3) . . . . ?
C30 C31 C32 C33 1.8(5) . . . . ?
C30 C31 C32 C36 -173.5(3) . . . . ?
C31 C30 C35 N11 6.5(5) . . . . ?
C31 C32 C33 C28 -1.5(5) . . . . ?
C31 C32 C36 N4 174.3(3) . . . . ?
C33 C28 C29 C30 0.8(5) . . . . ?
C33 C28 C34 N9 176.3(3) . . . . ?
C33 C32 C36 N4 -0.9(5) . . . . ?
C34 N9 C51 C47 126.5(3) . . . . ?
C34 N9 C51 C50 -121.4(4) . . . . ?
C34 C28 C29 C30 176.2(3) . . . . ?
C34 C28 C33 C32 -175.1(3) . . . . ?
C35 N11 C52 C53 -117.9(4) . . . . ?
C35 N11 C52 C56 125.8(3) . . . . ?
C35 C30 C31 C32 174.9(3) . . . . ?
C36 N4 C62 C63 -121.3(4) . . . . ?
C36 N4 C62 C66 124.8(3) . . . . ?
C36 C32 C33 C28 173.7(3) . . . . ?
C37 N2 C27 C23 -177.1(3) . . . . ?
C37 C38 C39 C40 13.6(4) . . . . ?
C38 C37 C41 N1 165.5(3) . . . . ?
C38 C37 C41 C40 43.9(3) . . . . ?
C38 C39 C40 C41 13.6(4) . . . . ?
C39 C40 C41 N1 -157.6(3) . . . . ?
C39 C40 C41 C37 -35.8(4) . . . . ?
C41 N1 C8 C3 -176.2(3) . . . . ?
C41 C37 C38 C39 -35.6(4) . . . . ?
C42 N8 C17 C12 179.1(3) . . . . ?
C42 C43 C44 C45 9.8(5) . . . . ?
C43 C42 C46 N7 163.4(3) . . . . ?
C43 C42 C46 C45 42.9(4) . . . . ?
C43 C44 C45 C46 17.0(5) . . . . ?
C44 C45 C46 N7 -156.7(4) . . . . ?
C44 C45 C46 C42 -37.0(4) . . . . ?
C46 N7 C26 C21 -177.2(3) . . . . ?
C46 C42 C43 C44 -32.8(4) . . . . ?
C47 N10 C18 C14 177.8(3) . . . . ?
C47 C48 C49 C50 19.4(4) . . . . ?
C48 C47 C51 N9 164.6(3) . . . . ?
C48 C47 C51 C50 46.2(3) . . . . ?
C48 C49 C50 C51 9.5(4) . . . . ?
C49 C50 C51 N9 -151.7(3) . . . . ?
C49 C50 C51 C47 -34.2(4) . . . . ?
C51 N9 C34 C28 -178.1(3) . . . . ?
C51 C47 C48 C49 -40.7(4) . . . . ?
C52 N11 C35 C30 -177.8(3) . . . . ?
C52 C53 C54 C55 -12.8(5) . . . . ?
C53 C52 C56 N12 154.5(4) . . . . ?
C53 C52 C56 C55 34.0(4) . . . . ?
C53 C54 C55 C56 33.8(5) . . . . ?
C54 C55 C56 N12 -163.0(3) . . . . ?
C54 C55 C56 C52 -42.0(4) . . . . ?
C56 N12 C25 C19 178.4(3) . . . . ?
C56 C52 C53 C54 -12.9(5) . . . . ?
C57 N6 C16 C10 -176.8(3) . . . . ?
C57 C58 C59 C60 -29.4(4) . . . . ?
C58 N5 C9 C5 -179.1(3) . . . . ?
C58 C57 C61 C60 -38.8(4) . . . . ?
C58 C59 C60 C61 5.1(4) . . . . ?
C59 C60 C61 C57 20.8(4) . . . . ?
C61 C57 C58 N5 164.4(3) . . . . ?
C61 C57 C58 C59 42.2(3) . . . . ?
C62 N4 C36 C32 -177.6(3) . . . . ?
C62 C63 C64 C65 12.3(5) . . . . ?
C63 C62 C66 N3 162.5(3) . . . . ?
C63 C62 C66 C65 42.2(4) . . . . ?
C63 C64 C65 C66 14.0(5) . . . . ?
C64 C65 C66 N3 -156.9(3) . . . . ?
C64 C65 C66 C62 -35.0(4) . . . . ?
C66 N3 C7 C1 175.8(3) . . . . ?
C66 C62 C63 C64 -33.6(4) . . . . ?
C67 C68 C69 C70 -1.4(10) . . . . ?
C68 C67 C72 C71 3.8(8) . . . . ?
C68 C69 C70 C71 2.9(9) . . . . ?
C68 C69 C70 C74 -178.4(7) . . . . ?
C69 C70 C71 C72 -1.1(8) . . . . ?
C70 C71 C72 C67 -2.3(9) . . . . ?
C72 C67 C68 C69 -2.0(8) . . . . ?
C73 C67 C68 C69 -178.9(6) . . . . ?
C73 C67 C72 C71 -179.3(6) . . . . ?
C74 C70 C71 C72 -179.8(7) . . . . ?
C75 C76 C77 C78 1.0(13) . . . . ?
C76 C75 C80 C79 2.7(9) . . . . ?
C76 C77 C78 C79 -1.6(10) . . . . ?
C76 C77 C78 C82 178.7(8) . . . . ?
C77 C78 C79 C80 2.9(10) . . . . ?
C78 C79 C80 C75 -3.6(10) . . . . ?
C80 C75 C76 C77 -1.5(11) . . . . ?
C81 C75 C76 C77 -179.8(9) . . . . ?
C81 C75 C80 C79 -178.9(8) . . . . ?
C82 C78 C79 C80 -177.4(7) . . . . ?
C87A C88A C83A C84A 0.0 . . . . ?
C88A C87A C86A C85A 0.0 . . . . ?
C88A C83A C84A C85A 0.0 . . . . ?
C88A C83A C84A C91 180.0 . . . . ?
C83A C84A C85A C86A 0.0 . . . . ?
C84A C85A C86A C87A 0.0 . . . . ?
C86A C87A C88A C83A 0.0 . . . . ?
C91 C84A C85A C86A 180.0 . . . . ?
C92 C87A C88A C83A 180.0 . . . . ?
C92 C87A C86A C85A 180.0 . . . . ?

_database_code_depnum_ccdc_archive 'CCDC 991219'
