# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_ivan_1m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            
;
 (1,4,8,11,14,18,23,27-octa-azoniadiaza-6(2,5)-furana-16,25(1,4)-dibenzena
 bicyclo[9.9.9]nonacosaphane nitrate clathrate) heptanitrate trihydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H60 N8 O, 8(N O3), 3(H2 O)'
_chemical_formula_sum            'C34 H66 N16 O28'
_chemical_formula_weight         1146.98

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2


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

_cell_length_a                   12.5559(13)
_cell_length_b                   12.7718(13)
_cell_length_c                   17.8881(18)
_cell_angle_alpha                110.689(2)
_cell_angle_beta                 91.837(2)
_cell_angle_gamma                102.914(2)
_cell_volume                     2596.2(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2002
_cell_measurement_theta_min      2
_cell_measurement_theta_max      17

_exptl_crystal_description       irregular
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1202
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Axs Smart-Apex CCD'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_decay_%        0
_diffrn_reflns_number            17958
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.23
_diffrn_reflns_theta_max         23.03
_reflns_number_total             7234
_reflns_number_gt                3387
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'SMART (Bruker-Axs Inc)'
_computing_cell_refinement       'SAINT (Bruker-Axs Inc)'
_computing_data_reduction        'SAINT (Bruker-Axs Inc)'
_computing_structure_solution    'SIR2011 (Burla et al., 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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 > 2σ(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.
 Positional disorder affects two of the eight nitrate counterions.
 The nitrate ion formed by the N15, O20, O21 and O22 atoms is disordered over
 two alternative positions (A and B) mutually exclusive and half populated.
 A half populated O4w atom site is placed near the O22B atom site;
 O4w hosts a water molecule when the O22B site is empty. The nitrate ion
 formed by the N16, O23, O24 and O25 atoms shows two alternative positions
 for the O25 site (A and B), mutually exclusive and half populated.
 Soft restraints on the geometrical features and on the Uij components
 have been applied to the refinement of the atom sites of the disordered
 nitrate ions. Positions for water proton remain undetermined.
;

_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)+(0.2000P)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_number_reflns         7234
_refine_ls_number_parameters     754
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.1808
_refine_ls_R_factor_gt           0.1131
_refine_ls_wR_factor_ref         0.3669
_refine_ls_wR_factor_gt          0.3090
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.125
_refine_ls_shift/su_max          0.008
_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
C1 C 0.3984(6) 0.1410(6) 0.1288(4) 0.086(2) Uani 1 1 d . . .
H1A H 0.4117 0.1486 0.0776 0.104 Uiso 1 1 calc R . .
H1B H 0.3864 0.0600 0.1211 0.104 Uiso 1 1 calc R . .
C2 C 0.4990(6) 0.2118(7) 0.1909(4) 0.091(2) Uani 1 1 d . . .
H2A H 0.4995 0.2930 0.2098 0.109 Uiso 1 1 calc R . .
H2B H 0.4952 0.1879 0.2368 0.109 Uiso 1 1 calc R . .
C3 C 0.6976(6) 0.2487(6) 0.2170(6) 0.115(3) Uani 1 1 d . . .
H3A H 0.6860 0.2205 0.2607 0.138 Uiso 1 1 calc R . .
H3B H 0.7607 0.2255 0.1927 0.138 Uiso 1 1 calc R . .
C4 C 0.7211(6) 0.3767(7) 0.2500(5) 0.088(2) Uani 1 1 d . . .
C5 C 0.6850(6) 0.4359(7) 0.3199(6) 0.098(2) Uani 1 1 d . . .
H5 H 0.6440 0.3949 0.3477 0.118 Uiso 1 1 calc R . .
C6 C 0.7079(6) 0.5559(8) 0.3506(4) 0.097(2) Uani 1 1 d . . .
H6 H 0.6813 0.5942 0.3978 0.117 Uiso 1 1 calc R . .
C7 C 0.7712(6) 0.6191(6) 0.3101(5) 0.0817(19) Uani 1 1 d . . .
C8 C 0.8079(5) 0.5597(6) 0.2406(5) 0.087(2) Uani 1 1 d . . .
H8 H 0.8495 0.6004 0.2129 0.105 Uiso 1 1 calc R . .
C9 C 0.7843(6) 0.4396(7) 0.2102(5) 0.094(2) Uani 1 1 d . . .
H9 H 0.8109 0.4011 0.1630 0.113 Uiso 1 1 calc R . .
C10 C 0.7970(6) 0.7507(6) 0.3407(5) 0.094(2) Uani 1 1 d . . .
H10A H 0.7986 0.7806 0.3988 0.112 Uiso 1 1 calc R . .
H10B H 0.8695 0.7801 0.3283 0.112 Uiso 1 1 calc R . .
C11 C 0.6030(5) 0.7612(6) 0.3239(4) 0.0850(19) Uani 1 1 d . . .
H11A H 0.6016 0.7924 0.3817 0.102 Uiso 1 1 calc R . .
H11B H 0.5774 0.6777 0.3051 0.102 Uiso 1 1 calc R . .
C12 C 0.5282(6) 0.8080(6) 0.2834(4) 0.086(2) Uani 1 1 d . . .
H12A H 0.5415 0.7903 0.2277 0.103 Uiso 1 1 calc R . .
H12B H 0.5446 0.8914 0.3099 0.103 Uiso 1 1 calc R . .
C13 C 0.2553(6) 0.1343(6) 0.2175(4) 0.086(2) Uani 1 1 d . . .
H13A H 0.3158 0.1462 0.2571 0.104 Uiso 1 1 calc R . .
H13B H 0.2230 0.0518 0.1919 0.104 Uiso 1 1 calc R . .
C14 C 0.1693(6) 0.1933(7) 0.2594(4) 0.097(2) Uani 1 1 d . . .
H14A H 0.1934 0.2758 0.2715 0.116 Uiso 1 1 calc R . .
H14B H 0.1004 0.1635 0.2240 0.116 Uiso 1 1 calc R . .
C15 C 0.0660(8) 0.2221(9) 0.3765(5) 0.121(3) Uani 1 1 d . . .
H15A H 0.0597 0.2056 0.4253 0.145 Uiso 1 1 calc R . .
H15B H -0.0038 0.1849 0.3425 0.145 Uiso 1 1 calc R . .
C16 C 0.0882(8) 0.3512(9) 0.3982(5) 0.103(3) Uani 1 1 d . . .
C17 C 0.0193(8) 0.3987(12) 0.3672(6) 0.129(3) Uani 1 1 d . . .
H17 H -0.0399 0.3508 0.3289 0.155 Uiso 1 1 calc R . .
C18 C 0.0362(8) 0.5139(11) 0.3916(6) 0.121(3) Uani 1 1 d . . .
H18 H -0.0143 0.5425 0.3703 0.145 Uiso 1 1 calc R . .
C19 C 0.1222(9) 0.5920(10) 0.4454(6) 0.115(3) Uani 1 1 d . . .
C20 C 0.1930(10) 0.5498(10) 0.4748(6) 0.127(3) Uani 1 1 d . . .
H20 H 0.2542 0.5998 0.5103 0.152 Uiso 1 1 calc R . .
C21 C 0.1765(9) 0.4298(11) 0.4528(6) 0.126(3) Uani 1 1 d . . .
H21 H 0.2262 0.4021 0.4755 0.151 Uiso 1 1 calc R . .
C22 C 0.1347(8) 0.7228(9) 0.4750(6) 0.132(3) Uani 1 1 d . . .
H22A H 0.0738 0.7375 0.4489 0.159 Uiso 1 1 calc R . .
H22B H 0.1303 0.7517 0.5325 0.159 Uiso 1 1 calc R . .
C23 C 0.2585(7) 0.7499(7) 0.3737(4) 0.099(2) Uani 1 1 d . . .
H23A H 0.1997 0.7602 0.3426 0.119 Uiso 1 1 calc R . .
H23B H 0.2569 0.6684 0.3537 0.119 Uiso 1 1 calc R . .
C24 C 0.3695(7) 0.8191(6) 0.3625(4) 0.097(2) Uani 1 1 d . . .
H24A H 0.3619 0.8929 0.3623 0.116 Uiso 1 1 calc R . .
H24B H 0.4236 0.8341 0.4074 0.116 Uiso 1 1 calc R . .
C25 C 0.2120(6) 0.1472(6) 0.0854(4) 0.0827(19) Uani 1 1 d . . .
H25A H 0.1423 0.1560 0.1052 0.099 Uiso 1 1 calc R . .
H25B H 0.2030 0.0665 0.0520 0.099 Uiso 1 1 calc R . .
C26 C 0.2424(6) 0.2202(7) 0.0354(4) 0.091(2) Uani 1 1 d . . .
H26A H 0.2527 0.3010 0.0692 0.110 Uiso 1 1 calc R . .
H26B H 0.3117 0.2105 0.0152 0.110 Uiso 1 1 calc R . .
C27 C 0.0489(6) 0.2040(7) -0.0159(5) 0.098(2) Uani 1 1 d . . .
H27A H 0.0125 0.1462 0.0047 0.117 Uiso 1 1 calc R . .
H27B H 0.0060 0.1918 -0.0657 0.117 Uiso 1 1 calc R . .
C28 C 0.0535(6) 0.3209(7) 0.0434(6) 0.091(2) Uani 1 1 d . . .
C29 C 0.0274(7) 0.3613(8) 0.1162(6) 0.102(2) Uani 1 1 d . . .
H29 H -0.0041 0.3185 0.1461 0.123 Uiso 1 1 calc R . .
C30 C 0.0566(7) 0.4836(8) 0.1408(6) 0.106(2) Uani 1 1 d . . .
H30 H 0.0459 0.5362 0.1897 0.127 Uiso 1 1 calc R . .
C31 C 0.1034(6) 0.5099(7) 0.0795(6) 0.097(2) Uani 1 1 d . . .
C32 C 0.1544(6) 0.6181(7) 0.0692(5) 0.097(2) Uani 1 1 d . . .
H32A H 0.1401 0.6828 0.1126 0.116 Uiso 1 1 calc R . .
H32B H 0.1227 0.6173 0.0188 0.116 Uiso 1 1 calc R . .
C33 C 0.3393(6) 0.6391(6) 0.1427(4) 0.090(2) Uani 1 1 d . . .
H33A H 0.4151 0.6394 0.1336 0.108 Uiso 1 1 calc R . .
H33B H 0.3079 0.5716 0.1554 0.108 Uiso 1 1 calc R . .
C34 C 0.3361(6) 0.7483(6) 0.2133(4) 0.090(2) Uani 1 1 d . . .
H34A H 0.2610 0.7457 0.2253 0.108 Uiso 1 1 calc R . .
H34B H 0.3633 0.8158 0.1997 0.108 Uiso 1 1 calc R . .
N1 N 0.2984(4) 0.1809(4) 0.1555(3) 0.0746(14) Uani 1 1 d . . .
H1N H 0.3181 0.2594 0.1788 0.089 Uiso 1 1 calc R . .
N2 N 0.5987(5) 0.1954(5) 0.1558(4) 0.0935(18) Uani 1 1 d . . .
H2NA H 0.6066 0.2269 0.1180 0.112 Uiso 1 1 calc R . .
H2NB H 0.5932 0.1192 0.1316 0.112 Uiso 1 1 calc R . .
N3 N 0.7156(5) 0.7936(4) 0.3052(3) 0.0842(16) Uani 1 1 d . . .
H3NA H 0.7380 0.8713 0.3228 0.101 Uiso 1 1 calc R . .
H3NB H 0.7150 0.7662 0.2513 0.101 Uiso 1 1 calc R . .
N4 N 0.1526(6) 0.1722(6) 0.3342(4) 0.111(2) Uani 1 1 d . . .
H4NA H 0.2163 0.2025 0.3673 0.134 Uiso 1 1 calc R . .
H4NB H 0.1343 0.0954 0.3227 0.134 Uiso 1 1 calc R . .
N5 N 0.2405(7) 0.7878(6) 0.4589(4) 0.119(2) Uani 1 1 d . . .
H5NA H 0.2417 0.8634 0.4767 0.143 Uiso 1 1 calc R . .
H5NB H 0.2966 0.7800 0.4874 0.143 Uiso 1 1 calc R . .
N6 N 0.1594(6) 0.1904(5) -0.0320(4) 0.0981(18) Uani 1 1 d . . .
H6NA H 0.1529 0.1160 -0.0634 0.118 Uiso 1 1 calc R . .
H6NB H 0.1853 0.2334 -0.0611 0.118 Uiso 1 1 calc R . .
N7 N 0.2770(5) 0.6325(5) 0.0692(3) 0.0946(17) Uani 1 1 d . . .
H7NA H 0.2883 0.5728 0.0276 0.114 Uiso 1 1 calc R . .
H7NB H 0.3054 0.6973 0.0599 0.114 Uiso 1 1 calc R . .
N8 N 0.4082(4) 0.7560(4) 0.2867(3) 0.0772(15) Uani 1 1 d . . .
H8N H 0.4022 0.6826 0.2843 0.093 Uiso 1 1 calc R . .
O1 O 0.1005(4) 0.4091(5) 0.0175(3) 0.0942(15) Uani 1 1 d . . .
N9 N 0.3760(7) 0.4700(8) 0.2937(6) 0.118(2) Uani 1 1 d D . .
O2 O 0.3916(5) 0.3932(5) 0.3183(4) 0.133(2) Uani 1 1 d D . .
O3 O 0.3249(8) 0.4391(8) 0.2292(5) 0.182(4) Uani 1 1 d D . .
O4 O 0.4103(6) 0.5726(6) 0.3395(5) 0.156(3) Uani 1 1 d D . .
N10 N 0.6592(7) 0.6164(7) 0.1016(5) 0.108(2) Uani 1 1 d . . .
O5 O 0.5882(6) 0.5835(5) 0.1419(4) 0.1219(19) Uani 1 1 d . . .
O6 O 0.6554(6) 0.5608(6) 0.0284(4) 0.139(2) Uani 1 1 d . . .
O7 O 0.7318(5) 0.7127(6) 0.1359(3) 0.1218(19) Uani 1 1 d . . .
N11 N 0.5375(6) -0.1026(7) 0.1049(5) 0.0969(18) Uani 1 1 d . . .
O8 O 0.5262(6) -0.0405(6) 0.1728(4) 0.136(2) Uani 1 1 d . . .
O9 O 0.5279(6) -0.2074(5) 0.0867(4) 0.131(2) Uani 1 1 d . . .
O10 O 0.5612(6) -0.0559(5) 0.0579(4) 0.137(2) Uani 1 1 d . . .
N12 N 0.1025(7) -0.0745(7) -0.1548(5) 0.1007(19) Uani 1 1 d . . .
O11 O 0.1848(5) -0.0053(6) -0.1590(4) 0.1216(19) Uani 1 1 d . . .
O12 O 0.0808(5) -0.1754(6) -0.2063(5) 0.149(2) Uani 1 1 d . . .
O13 O 0.0435(5) -0.0488(5) -0.1035(4) 0.1202(19) Uani 1 1 d . . .
N13 N 0.7472(6) 0.1600(7) -0.0063(6) 0.107(2) Uani 1 1 d . . .
O14 O 0.7666(7) 0.1362(5) -0.0764(5) 0.150(3) Uani 1 1 d . . .
O15 O 0.7032(6) 0.2404(6) 0.0258(5) 0.145(2) Uani 1 1 d . . .
O16 O 0.7687(8) 0.1071(7) 0.0303(5) 0.167(3) Uani 1 1 d . . .
N14 N 0.0679(10) -0.1313(10) 0.2510(6) 0.140(3) Uani 1 1 d . . .
O17 O 0.0470(7) -0.2314(8) 0.2397(7) 0.202(4) Uani 1 1 d . . .
O18 O 0.0089(8) -0.0667(8) 0.2546(7) 0.215(5) Uani 1 1 d . . .
O19 O 0.1619(11) -0.0791(10) 0.2778(10) 0.242(6) Uani 1 1 d . . .
O1W O 0.5131(6) 0.3434(6) 0.0794(5) 0.159(3) Uani 1 1 d . . .
O2W O 0.5000 0.5000 0.5000 0.253(7) Uani 1 2 d S . .
O3W O 0.7782(6) 1.0292(5) 0.3203(5) 0.170(3) Uani 1 1 d . . .
N15A N 0.0960(17) -0.0081(16) 0.4736(13) 0.181(9) Uani 0.50 1 d PD A 1
O20A O 0.1963(15) 0.0011(14) 0.4920(12) 0.151(6) Uani 0.50 1 d PD A 1
O21A O 0.072(2) 0.0762(15) 0.4715(13) 0.238(13) Uani 0.50 1 d PD A 1
O22A O 0.0290(17) -0.1035(14) 0.4558(15) 0.263(16) Uani 0.50 1 d PD A 1
O4W O 0.326(2) 0.250(2) 0.4494(11) 0.243(15) Uani 0.50 1 d P B 1
N15B N 0.2640(17) 0.0718(13) 0.4634(10) 0.148(6) Uani 0.50 1 d PDU C 2
O20B O 0.3025(18) 0.0373(12) 0.5138(8) 0.162(6) Uani 0.50 1 d PD C 2
O21B O 0.2184(18) -0.0019(13) 0.4013(10) 0.212(10) Uani 0.50 1 d PD C 2
O22B O 0.2909(17) 0.1771(10) 0.4737(11) 0.162(7) Uani 0.50 1 d PD C 2
N16 N 0.4617(11) 0.8415(15) 0.5968(8) 0.222(7) Uani 1 1 d DU . .
O23 O 0.3639(12) 0.8119(14) 0.6056(10) 0.291(7) Uani 1 1 d D D .
O24 O 0.5395(10) 0.8833(15) 0.6512(6) 0.280(8) Uani 1 1 d D D .
O25A O 0.469(2) 0.794(3) 0.5228(8) 0.293(17) Uani 0.50 1 d PD D .
O25B O 0.4476(17) 0.9218(12) 0.5763(12) 0.233(11) Uani 0.50 1 d PD D 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.489(8) . ?
C1 C2 1.529(10) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.442(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.483(10) . ?
C3 N2 1.488(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.365(11) . ?
C4 C9 1.391(10) . ?
C5 C6 1.390(11) . ?
C5 H5 0.9300 . ?
C6 C7 1.403(10) . ?
C6 H6 0.9300 . ?
C7 C8 1.364(10) . ?
C7 C10 1.524(10) . ?
C8 C9 1.390(10) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 N3 1.485(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N3 1.467(8) . ?
C11 C12 1.509(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N8 1.517(8) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N1 1.495(8) . ?
C13 C14 1.520(10) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 N4 1.469(9) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N4 1.477(11) . ?
C15 C16 1.510(12) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.365(13) . ?
C16 C21 1.389(13) . ?
C17 C18 1.342(14) . ?
C17 H17 0.9300 . ?
C18 C19 1.364(13) . ?
C18 H18 0.9300 . ?
C19 C20 1.320(13) . ?
C19 C22 1.533(13) . ?
C20 C21 1.404(13) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 N5 1.496(11) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 N5 1.470(9) . ?
C23 C24 1.534(10) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 N8 1.473(9) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 N1 1.502(8) . ?
C25 C26 1.506(9) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 N6 1.449(9) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 N6 1.462(9) . ?
C27 C28 1.482(11) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.304(11) . ?
C28 O1 1.386(8) . ?
C29 C30 1.420(11) . ?
C29 H29 0.9300 . ?
C30 C31 1.369(11) . ?
C30 H30 0.9300 . ?
C31 O1 1.362(9) . ?
C31 C32 1.466(11) . ?
C32 N7 1.508(9) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 N7 1.476(8) . ?
C33 C34 1.525(9) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 N8 1.530(8) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
N1 H1N 0.9100 . ?
N2 H2NA 0.9000 . ?
N2 H2NB 0.9000 . ?
N3 H3NA 0.9000 . ?
N3 H3NB 0.9000 . ?
N4 H4NA 0.9000 . ?
N4 H4NB 0.9000 . ?
N5 H5NA 0.9000 . ?
N5 H5NB 0.9000 . ?
N6 H6NA 0.9000 . ?
N6 H6NB 0.9000 . ?
N7 H7NA 0.9000 . ?
N7 H7NB 0.9000 . ?
N8 H8N 0.9100 . ?
N9 O3 1.191(9) . ?
N9 O4 1.241(9) . ?
N9 O2 1.257(8) . ?
N10 O6 1.243(8) . ?
N10 O5 1.257(9) . ?
N10 O7 1.285(9) . ?
N11 O10 1.201(8) . ?
N11 O8 1.227(8) . ?
N11 O9 1.236(8) . ?
N12 O13 1.199(8) . ?
N12 O11 1.225(8) . ?
N12 O12 1.254(8) . ?
N13 O16 1.158(9) . ?
N13 O14 1.227(9) . ?
N13 O15 1.243(10) . ?
N14 O17 1.187(11) . ?
N14 O19 1.205(12) . ?
N14 O18 1.214(11) . ?
N15A O21A 1.194(11) . ?
N15A O22A 1.243(12) . ?
N15A O20A 1.260(11) . ?
N15B O21B 1.195(11) . ?
N15B O22B 1.255(12) . ?
N15B O20B 1.260(11) . ?
N16 O23 1.234(9) . ?
N16 O24 1.235(9) . ?
N16 O25B 1.249(10) . ?
N16 O25A 1.264(10) . ?
O23 O25B 1.80(3) . ?
O25A O25B 1.66(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 110.9(6) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.0 . . ?
N2 C2 C1 110.3(6) . . ?
N2 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C4 C3 N2 111.7(6) . . ?
C4 C3 H3A 109.3 . . ?
N2 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
N2 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
C5 C4 C9 118.4(7) . . ?
C5 C4 C3 121.9(8) . . ?
C9 C4 C3 119.7(8) . . ?
C4 C5 C6 121.6(8) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C7 119.9(7) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C8 C7 C6 118.3(7) . . ?
C8 C7 C10 119.9(7) . . ?
C6 C7 C10 121.8(7) . . ?
C7 C8 C9 121.4(7) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 H8 119.3 . . ?
C8 C9 C4 120.4(7) . . ?
C8 C9 H9 119.8 . . ?
C4 C9 H9 119.8 . . ?
N3 C10 C7 113.0(5) . . ?
N3 C10 H10A 109.0 . . ?
C7 C10 H10A 109.0 . . ?
N3 C10 H10B 109.0 . . ?
C7 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
N3 C11 C12 109.6(6) . . ?
N3 C11 H11A 109.8 . . ?
C12 C11 H11A 109.8 . . ?
N3 C11 H11B 109.8 . . ?
C12 C11 H11B 109.8 . . ?
H11A C11 H11B 108.2 . . ?
C11 C12 N8 111.1(5) . . ?
C11 C12 H12A 109.4 . . ?
N8 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
N8 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
N1 C13 C14 111.4(6) . . ?
N1 C13 H13A 109.4 . . ?
C14 C13 H13A 109.4 . . ?
N1 C13 H13B 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
N4 C14 C13 110.0(6) . . ?
N4 C14 H14A 109.7 . . ?
C13 C14 H14A 109.7 . . ?
N4 C14 H14B 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
N4 C15 C16 113.3(7) . . ?
N4 C15 H15A 108.9 . . ?
C16 C15 H15A 108.9 . . ?
N4 C15 H15B 108.9 . . ?
C16 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C17 C16 C21 115.4(10) . . ?
C17 C16 C15 121.6(10) . . ?
C21 C16 C15 123.0(11) . . ?
C18 C17 C16 120.7(9) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C19 124.5(10) . . ?
C17 C18 H18 117.8 . . ?
C19 C18 H18 117.8 . . ?
C20 C19 C18 116.9(11) . . ?
C20 C19 C22 120.4(11) . . ?
C18 C19 C22 122.7(11) . . ?
C19 C20 C21 120.4(10) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C16 C21 C20 122.1(10) . . ?
C16 C21 H21 118.9 . . ?
C20 C21 H21 118.9 . . ?
N5 C22 C19 113.4(7) . . ?
N5 C22 H22A 108.9 . . ?
C19 C22 H22A 108.9 . . ?
N5 C22 H22B 108.9 . . ?
C19 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
N5 C23 C24 111.1(6) . . ?
N5 C23 H23A 109.4 . . ?
C24 C23 H23A 109.4 . . ?
N5 C23 H23B 109.4 . . ?
C24 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
N8 C24 C23 111.3(6) . . ?
N8 C24 H24A 109.4 . . ?
C23 C24 H24A 109.4 . . ?
N8 C24 H24B 109.4 . . ?
C23 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
N1 C25 C26 111.6(6) . . ?
N1 C25 H25A 109.3 . . ?
C26 C25 H25A 109.3 . . ?
N1 C25 H25B 109.3 . . ?
C26 C25 H25B 109.3 . . ?
H25A C25 H25B 108.0 . . ?
N6 C26 C25 112.6(6) . . ?
N6 C26 H26A 109.1 . . ?
C25 C26 H26A 109.1 . . ?
N6 C26 H26B 109.1 . . ?
C25 C26 H26B 109.1 . . ?
H26A C26 H26B 107.8 . . ?
N6 C27 C28 110.9(6) . . ?
N6 C27 H27A 109.5 . . ?
C28 C27 H27A 109.5 . . ?
N6 C27 H27B 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 108.0 . . ?
C29 C28 O1 111.6(7) . . ?
C29 C28 C27 134.9(8) . . ?
O1 C28 C27 113.4(8) . . ?
C28 C29 C30 106.3(8) . . ?
C28 C29 H29 126.8 . . ?
C30 C29 H29 126.8 . . ?
C31 C30 C29 107.4(8) . . ?
C31 C30 H30 126.3 . . ?
C29 C30 H30 126.3 . . ?
O1 C31 C30 108.4(7) . . ?
O1 C31 C32 117.5(8) . . ?
C30 C31 C32 134.1(9) . . ?
C31 C32 N7 110.1(6) . . ?
C31 C32 H32A 109.6 . . ?
N7 C32 H32A 109.6 . . ?
C31 C32 H32B 109.6 . . ?
N7 C32 H32B 109.6 . . ?
H32A C32 H32B 108.2 . . ?
N7 C33 C34 110.5(6) . . ?
N7 C33 H33A 109.5 . . ?
C34 C33 H33A 109.5 . . ?
N7 C33 H33B 109.5 . . ?
C34 C33 H33B 109.5 . . ?
H33A C33 H33B 108.1 . . ?
C33 C34 N8 108.8(5) . . ?
C33 C34 H34A 109.9 . . ?
N8 C34 H34A 109.9 . . ?
C33 C34 H34B 109.9 . . ?
N8 C34 H34B 109.9 . . ?
H34A C34 H34B 108.3 . . ?
C1 N1 C13 109.8(5) . . ?
C1 N1 C25 111.2(5) . . ?
C13 N1 C25 111.5(5) . . ?
C1 N1 H1N 108.0 . . ?
C13 N1 H1N 108.0 . . ?
C25 N1 H1N 108.0 . . ?
C2 N2 C3 112.1(6) . . ?
C2 N2 H2NA 109.2 . . ?
C3 N2 H2NA 109.2 . . ?
C2 N2 H2NB 109.2 . . ?
C3 N2 H2NB 109.2 . . ?
H2NA N2 H2NB 107.9 . . ?
C11 N3 C10 114.6(5) . . ?
C11 N3 H3NA 108.6 . . ?
C10 N3 H3NA 108.6 . . ?
C11 N3 H3NB 108.6 . . ?
C10 N3 H3NB 108.6 . . ?
H3NA N3 H3NB 107.6 . . ?
C14 N4 C15 113.2(7) . . ?
C14 N4 H4NA 108.9 . . ?
C15 N4 H4NA 108.9 . . ?
C14 N4 H4NB 108.9 . . ?
C15 N4 H4NB 108.9 . . ?
H4NA N4 H4NB 107.7 . . ?
C23 N5 C22 114.3(7) . . ?
C23 N5 H5NA 108.7 . . ?
C22 N5 H5NA 108.7 . . ?
C23 N5 H5NB 108.7 . . ?
C22 N5 H5NB 108.7 . . ?
H5NA N5 H5NB 107.6 . . ?
C26 N6 C27 118.9(6) . . ?
C26 N6 H6NA 107.6 . . ?
C27 N6 H6NA 107.6 . . ?
C26 N6 H6NB 107.6 . . ?
C27 N6 H6NB 107.6 . . ?
H6NA N6 H6NB 107.0 . . ?
C33 N7 C32 117.0(6) . . ?
C33 N7 H7NA 108.1 . . ?
C32 N7 H7NA 108.1 . . ?
C33 N7 H7NB 108.1 . . ?
C32 N7 H7NB 108.1 . . ?
H7NA N7 H7NB 107.3 . . ?
C24 N8 C12 112.2(5) . . ?
C24 N8 C34 111.6(5) . . ?
C12 N8 C34 110.6(5) . . ?
C24 N8 H8N 107.4 . . ?
C12 N8 H8N 107.4 . . ?
C34 N8 H8N 107.4 . . ?
C31 O1 C28 106.2(6) . . ?
O3 N9 O4 124.2(9) . . ?
O3 N9 O2 117.6(9) . . ?
O4 N9 O2 118.1(9) . . ?
O6 N10 O5 120.8(8) . . ?
O6 N10 O7 120.1(9) . . ?
O5 N10 O7 118.9(8) . . ?
O10 N11 O8 116.6(7) . . ?
O10 N11 O9 121.9(8) . . ?
O8 N11 O9 121.5(8) . . ?
O13 N12 O11 122.3(8) . . ?
O13 N12 O12 120.0(9) . . ?
O11 N12 O12 117.8(9) . . ?
O16 N13 O14 120.3(11) . . ?
O16 N13 O15 119.4(10) . . ?
O14 N13 O15 120.3(8) . . ?
O17 N14 O19 115.2(12) . . ?
O17 N14 O18 131.4(12) . . ?
O19 N14 O18 111.9(11) . . ?
O21A N15A O22A 123.8(12) . . ?
O21A N15A O20A 116.9(13) . . ?
O22A N15A O20A 119.2(13) . . ?
O21B N15B O22B 122.9(12) . . ?
O21B N15B O20B 116.0(12) . . ?
O22B N15B O20B 119.9(13) . . ?
O23 N16 O24 125.5(15) . . ?
O23 N16 O25B 93.0(17) . . ?
O24 N16 O25B 107.0(17) . . ?
O23 N16 O25A 107(2) . . ?
O24 N16 O25A 125.3(16) . . ?
O25B N16 O25A 83.0(17) . . ?
N16 O23 O25B 43.8(9) . . ?
N16 O25A O25B 48.1(9) . . ?
N16 O25B O25A 48.9(9) . . ?
N16 O25B O23 43.1(9) . . ?
O25A O25B O23 70.5(15) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        23.03
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.100
_database_code_depnum_ccdc_archive 'CCDC 992963'
