# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2018

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

data_c
_database_code_depnum_ccdc_archive 'CCDC 1839930'
_audit_update_record             
;
2018-04-26 deposited with the CCDC.
2018-08-29 downloaded from the CCDC.
;

_audit_creation_date             2017-03-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
decaaquodisodium 4-[2-(3-pyridyl)diazenyl]-benzoate 
 
;
_chemical_formula_moiety         'C12 H8 N3 O2, H10 Na O5'
_chemical_formula_sum            'C12 H18 N3 Na O7'
_chemical_formula_weight         339.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H72 N12 Na4 O28'
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'
Na Na 0.0362 0.0249 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   6.5197(6)
_cell_length_b                   35.222(3)
_cell_length_c                   7.2310(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.838(10)
_cell_angle_gamma                90.00
_cell_volume                     1619.0(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2519
_cell_measurement_temperature    119.99(14)
_cell_measurement_theta_max      30.4590
_cell_measurement_theta_min      3.3460
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11758
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.11
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -31.00   -4.00   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322  -57.0000   30.0000 90

#__ type_ start__ end____ width___ exp.time_
  2 omega  -57.00  -12.00   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -19.0000    0.0000 150

#__ type_ start__ end____ width___ exp.time_
  3 omega   11.00   36.50   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -57.0000  -90.0000 85

#__ type_ start__ end____ width___ exp.time_
  4 omega  -56.00   28.00   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -37.0000 -120.0000 280

#__ type_ start__ end____ width___ exp.time_
  5 omega  -81.00    4.50   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322  -61.0000  131.0315 285
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0371242000
_diffrn_orient_matrix_UB_12      -0.0183018000
_diffrn_orient_matrix_UB_13      0.0321873000
_diffrn_orient_matrix_UB_21      0.0749789000
_diffrn_orient_matrix_UB_22      0.0083890000
_diffrn_orient_matrix_UB_23      0.0750361000
_diffrn_orient_matrix_UB_31      -0.0738323000
_diffrn_orient_matrix_UB_32      -0.0006647000
_diffrn_orient_matrix_UB_33      0.0587060000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                3315
_reflns_number_total             4026
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    ?
_computing_publication_material  ?
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.259
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4026
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0911
_refine_ls_restrained_S_all      1.259
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0381P)²+2.1733P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1714
_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
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
C1 C 0.8560(6) 0.88557(8) 0.2102(5) 0.0228(7) Uani 1 d . . .
H1 H 0.8836 0.9115 0.2085 0.027 Uiso 1 calc . . R
C2 C 1.0254(5) 0.86081(9) 0.2450(5) 0.0212(7) Uani 1 d . . .
H2 H 1.1626 0.8699 0.2664 0.025 Uiso 1 calc . . R
C3 C 0.9857(5) 0.82225(9) 0.2471(4) 0.0201(7) Uani 1 d . . .
H3 H 1.0956 0.8048 0.2673 0.024 Uiso 1 calc . . R
C4 C 0.7783(5) 0.81012(8) 0.2183(4) 0.0167(6) Uani 1 d . . .
C5 C 0.6181(5) 0.83707(9) 0.1839(4) 0.0204(7) Uani 1 d . . .
H5 H 0.4796 0.8287 0.1635 0.024 Uiso 1 calc . . R
C6 C 0.5293(5) 0.72082(8) 0.2350(4) 0.0176(6) Uani 1 d . . .
C7 C 0.3217(5) 0.70890(9) 0.2065(4) 0.0196(7) Uani 1 d . . .
H7 H 0.2135 0.7267 0.1881 0.024 Uiso 1 calc . . R
C8 C 0.2760(5) 0.67040(8) 0.2055(4) 0.0183(6) Uani 1 d . . .
H8 H 0.1367 0.6624 0.1835 0.022 Uiso 1 calc . . R
C9 C 0.4372(5) 0.64356(8) 0.2373(4) 0.0140(6) Uani 1 d . . .
C10 C 0.6464(5) 0.65602(8) 0.2707(4) 0.0167(6) Uani 1 d . . .
H10 H 0.7550 0.6383 0.2934 0.020 Uiso 1 calc . . R
C11 C 0.6932(5) 0.69426(8) 0.2703(4) 0.0188(6) Uani 1 d . . .
H11 H 0.8324 0.7023 0.2932 0.023 Uiso 1 calc . . R
C12 C 0.3866(5) 0.60179(8) 0.2343(4) 0.0147(6) Uani 1 d . . .
N1 N 0.6540(5) 0.87433(7) 0.1788(4) 0.0235(6) Uani 1 d . . .
N2 N 0.7451(4) 0.77013(7) 0.2246(4) 0.0197(6) Uani 1 d . . .
N3 N 0.5610(4) 0.76099(7) 0.2286(4) 0.0194(6) Uani 1 d . . .
O1 O 0.5372(3) 0.57834(6) 0.2692(3) 0.0192(5) Uani 1 d . . .
O2 O 0.1975(3) 0.59233(6) 0.1952(3) 0.0242(5) Uani 1 d . . .
Na1 Na 1.32062(18) 0.97724(3) 0.31045(16) 0.0142(3) Uani 1 d . . .
O3 O 1.3532(4) 1.02781(6) 0.0945(3) 0.0159(5) Uani 1 d . . .
O4 O 1.3134(3) 1.02548(6) 0.5480(3) 0.0158(5) Uani 1 d . . .
O5 O 0.9518(3) 0.99576(6) 0.2155(3) 0.0150(4) Uani 1 d . . .
O6 O 1.2885(4) 0.92622(7) 0.5046(3) 0.0214(5) Uani 1 d . . .
O7 O 1.3611(4) 0.93398(6) 0.0749(3) 0.0174(5) Uani 1 d . . .
H5A H 0.956(6) 1.0210(12) 0.211(6) 0.034(11) Uiso 1 d . . .
H6A H 1.410(7) 0.9182(11) 0.560(6) 0.034(11) Uiso 1 d . . .
H7A H 1.438(6) 0.9127(11) 0.107(5) 0.023(9) Uiso 1 d . . .
H6B H 1.210(6) 0.9245(11) 0.583(6) 0.034(11) Uiso 1 d . . .
H3A H 1.451(7) 1.0362(12) 0.053(6) 0.039(12) Uiso 1 d . . .
H4A H 1.222(8) 1.0210(13) 0.607(7) 0.059(15) Uiso 1 d . . .
H7B H 1.260(7) 0.9289(11) -0.007(6) 0.032(12) Uiso 1 d . . .
H5B H 0.858(7) 0.9904(11) 0.105(6) 0.033(11) Uiso 1 d . . .
H4B H 1.276(6) 1.0459(11) 0.486(5) 0.025(10) Uiso 1 d . . .
H3B H 1.326(7) 1.0486(13) 0.156(6) 0.045(12) Uiso 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9300 . ?
C1 C2 1.386(5) . ?
C1 N1 1.346(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.383(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.389(4) . ?
C4 C5 1.392(4) . ?
C4 N2 1.427(4) . ?
C5 H5 0.9300 . ?
C5 N1 1.335(4) . ?
C6 C7 1.389(4) . ?
C6 C11 1.400(4) . ?
C6 N3 1.432(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.388(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.394(4) . ?
C9 C10 1.402(4) . ?
C9 C12 1.507(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.381(4) . ?
C11 H11 0.9300 . ?
C12 O1 1.265(4) . ?
C12 O2 1.248(4) . ?
N2 N3 1.249(4) . ?
Na1 Na1 3.565(2) 3_876 ?
Na1 O3 2.409(2) . ?
Na1 O4 2.380(3) 3_876 ?
Na1 O4 2.424(2) . ?
Na1 O5 2.438(2) . ?
Na1 O6 2.318(2) . ?
Na1 O7 2.344(2) . ?
O3 H3A 0.82(5) . ?
O3 H3B 0.90(5) . ?
O4 Na1 2.380(3) 3_876 ?
O4 H4A 0.82(5) . ?
O4 H4B 0.85(4) . ?
O5 H5A 0.89(4) . ?
O5 H5B 0.91(4) . ?
O6 H6A 0.85(5) . ?
O6 H6B 0.84(4) . ?
O7 H7A 0.90(4) . ?
O7 H7B 0.80(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 118.1 . . ?
N1 C1 H1 118.1 . . ?
N1 C1 C2 123.8(3) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 C1 118.4(3) . . ?
C3 C2 H2 120.8 . . ?
C2 C3 H3 120.7 . . ?
C2 C3 C4 118.6(3) . . ?
C4 C3 H3 120.7 . . ?
C3 C4 C5 118.9(3) . . ?
C3 C4 N2 116.6(3) . . ?
C5 C4 N2 124.4(3) . . ?
C4 C5 H5 118.4 . . ?
N1 C5 C4 123.1(3) . . ?
N1 C5 H5 118.4 . . ?
C7 C6 C11 120.3(3) . . ?
C7 C6 N3 115.9(3) . . ?
C11 C6 N3 123.8(3) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 C6 119.8(3) . . ?
C8 C7 H7 120.1 . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C9 120.6(3) . . ?
C9 C8 H8 119.7 . . ?
C8 C9 C10 119.0(3) . . ?
C8 C9 C12 120.3(3) . . ?
C10 C9 C12 120.6(3) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 C9 120.8(3) . . ?
C11 C10 H10 119.6 . . ?
C6 C11 H11 120.3 . . ?
C10 C11 C6 119.5(3) . . ?
C10 C11 H11 120.3 . . ?
O1 C12 C9 118.5(3) . . ?
O2 C12 C9 117.8(3) . . ?
O2 C12 O1 123.7(3) . . ?
C5 N1 C1 117.1(3) . . ?
N3 N2 C4 114.1(3) . . ?
N2 N3 C6 113.7(3) . . ?
O3 Na1 Na1 91.64(7) . 3_876 ?
O3 Na1 O4 87.68(8) . . ?
O3 Na1 O5 80.97(8) . . ?
O4 Na1 Na1 42.57(6) 3_876 3_876 ?
O4 Na1 Na1 41.63(6) . 3_876 ?
O4 Na1 O3 94.83(9) 3_876 . ?
O4 Na1 O4 84.20(8) 3_876 . ?
O4 Na1 O5 80.72(8) . . ?
O4 Na1 O5 164.48(9) 3_876 . ?
O5 Na1 Na1 122.26(7) . 3_876 ?
O6 Na1 Na1 90.86(8) . 3_876 ?
O6 Na1 O3 176.83(9) . . ?
O6 Na1 O4 85.70(9) . 3_876 ?
O6 Na1 O4 95.49(9) . . ?
O6 Na1 O5 99.31(9) . . ?
O6 Na1 O7 88.63(9) . . ?
O7 Na1 Na1 133.69(9) . 3_876 ?
O7 Na1 O3 88.23(8) . . ?
O7 Na1 O4 91.29(9) . 3_876 ?
O7 Na1 O4 173.63(9) . . ?
O7 Na1 O5 103.44(9) . . ?
Na1 O3 H3A 134(3) . . ?
Na1 O3 H3B 103(3) . . ?
H3A O3 H3B 98(4) . . ?
Na1 O4 Na1 95.80(8) 3_876 . ?
Na1 O4 H4A 111(3) . . ?
Na1 O4 H4A 123(3) 3_876 . ?
Na1 O4 H4B 114(3) 3_876 . ?
Na1 O4 H4B 105(2) . . ?
H4A O4 H4B 106(4) . . ?
Na1 O5 H5A 104(3) . . ?
Na1 O5 H5B 128(2) . . ?
H5A O5 H5B 101(3) . . ?
Na1 O6 H6A 110(3) . . ?
Na1 O6 H6B 128(3) . . ?
H6A O6 H6B 108(4) . . ?
Na1 O7 H7A 120(2) . . ?
Na1 O7 H7B 118(3) . . ?
H7A O7 H7B 109(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
C1 C2 C3 C4 -1.4(5) . . . . ?
C2 C1 N1 C5 0.7(5) . . . . ?
C2 C3 C4 C5 1.6(5) . . . . ?
C2 C3 C4 N2 -179.1(3) . . . . ?
C3 C4 C5 N1 -0.6(5) . . . . ?
C3 C4 N2 N3 169.1(3) . . . . ?
C4 C5 N1 C1 -0.5(5) . . . . ?
C4 N2 N3 C6 -180.0(2) . . . . ?
C5 C4 N2 N3 -11.6(4) . . . . ?
C6 C7 C8 C9 1.5(5) . . . . ?
C7 C6 C11 C10 2.0(5) . . . . ?
C7 C6 N3 N2 -169.2(3) . . . . ?
C7 C8 C9 C10 0.2(4) . . . . ?
C7 C8 C9 C12 -179.4(3) . . . . ?
C8 C9 C10 C11 -0.7(4) . . . . ?
C8 C9 C12 O1 -178.0(3) . . . . ?
C8 C9 C12 O2 2.9(4) . . . . ?
C9 C10 C11 C6 -0.4(5) . . . . ?
C10 C9 C12 O1 2.4(4) . . . . ?
C10 C9 C12 O2 -176.7(3) . . . . ?
C11 C6 C7 C8 -2.6(5) . . . . ?
C11 C6 N3 N2 11.7(4) . . . . ?
C12 C9 C10 C11 178.9(3) . . . . ?
N1 C1 C2 C3 0.2(5) . . . . ?
N2 C4 C5 N1 -180.0(3) . . . . ?
N3 C6 C7 C8 178.4(3) . . . . ?
N3 C6 C11 C10 -179.0(3) . . . . ?
O3 Na1 O4 Na1 -95.10(9) . . . 3_876 ?
O4 Na1 O4 Na1 0.0 3_876 . . 3_876 ?
O5 Na1 O4 Na1 -176.33(10) . . . 3_876 ?
O6 Na1 O4 Na1 85.10(10) . . . 3_876 ?
O7 Na1 O4 Na1 -45.0(9) . . . 3_876 ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 17 9 0.0686 -0.9913 16.9865 9.0025 -0.0579 0.7437 0.5904
1 -17 -9 0.0686 0.9913 -16.9865 -9.0025 0.0579 -0.7437 -0.5904
5 39 2 0.0912 5.0130 38.9757 1.9992 -0.4629 0.8528 -0.2787
-6 -31 6 0.1129 -6.0072 -30.9855 6.0034 0.5373 -0.2599 0.8166
1 38 -7 0.0478 1.0075 37.9958 -7.0044 -0.8834 -0.1313 -0.5108
8 -17 1 0.1354 7.9977 -17.0141 1.0018 0.6405 0.5321 -0.5204
1 -38 6 0.0737 0.9925 -37.9989 6.0042 0.9256 0.2062 0.3045
-1 -38 7 0.0742 -1.0075 -37.9958 7.0044 0.8834 0.1313 0.5108
-4 34 -5 0.1295 -3.9939 34.0054 -5.0038 -0.9317 -0.3897 -0.0215
-7 -26 6 0.1177 -7.0061 -25.9847 6.0030 0.4087 -0.2928 0.8870
0 -38 -6 0.0609 0.1749 -37.9675 -6.4414 0.4940 -0.7887 -0.3658
-1 38 7 0.0374 -0.9746 37.6014 6.6400 -0.5106 0.7406 0.4368
2 -48 -2 0.0592 1.9862 -47.9886 -1.9983 0.8877 -0.4036 -0.2321
0 48 -2 0.0318 0.0124 47.9891 -2.0031 -0.9423 0.2532 -0.1504
-2 46 3 0.0478 -1.9863 45.9879 2.9987 -0.8189 0.4619 0.2921
-1 -45 4 0.0756 -1.0109 -44.9902 4.0036 0.9147 -0.1528 0.3396
0 50 0 0.0230 0.0139 49.9861 -0.0024 -0.9144 0.4202 -0.0344
9 14 -4 0.1467 9.0041 13.9812 -4.0016 -0.0504 0.4921 -0.9090
-1 -49 -1 0.0656 -1.0143 -48.9829 -0.9981 0.8267 -0.5619 0.0489
-6 -39 1 0.1082 -6.0118 -38.9772 1.0019 0.5224 -0.7026 0.5286

_olex2_date_sample_data_collection 2015-05-21
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_C
_database_code_depnum_ccdc_archive 'CCDC 1859218'
_audit_update_record             
;
2018-07-30 deposited with the CCDC.
2018-08-29 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
;
2,7,12-Tris-(2-(4-pyridylazo)ethoxy)-3,8,13-trimethoxy-10,15-dihydro-2H-tribenzo[a,d,g]cyclononene nitromethane clathrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C65 H63 N11 O13'
_chemical_formula_weight         1206.26

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

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

_cell_length_a                   35.5103(7)
_cell_length_b                   9.6091(2)
_cell_length_c                   37.3391(8)
_cell_angle_alpha                90
_cell_angle_beta                 103.589(2)
_cell_angle_gamma                90
_cell_volume                     12384.3(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    13962
_cell_measurement_theta_min      4.7500
_cell_measurement_theta_max      63.4320

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_F_000             5072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    0.758
_shelx_estimated_absorpt_T_min   0.810
_shelx_estimated_absorpt_T_max   0.908
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41057
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         3.091
_diffrn_reflns_theta_max         63.826
_diffrn_reflns_theta_full        63.826
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             10085
_reflns_number_gt                7879
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

Two MeNO2 positions within L3.2(MeNO2) were each refined isotropically at 0.5 occupancy. Restraints
 were used for MeNO2 bond lengths and a FLAT restraint was employed for MeNO2
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10085
_refine_ls_number_parameters     804
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0959
_refine_ls_wR_factor_ref         0.3231
_refine_ls_wR_factor_gt          0.2991
_refine_ls_goodness_of_fit_ref   1.360
_refine_ls_restrained_S_all      1.365
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.43227(7) 0.8020(3) 0.13043(6) 0.0411(6) Uani 1 1 d . . . . .
O2 O 0.38869(7) 0.6863(2) 0.17286(6) 0.0377(6) Uani 1 1 d . . . . .
O3 O 0.31338(8) 0.6306(3) 0.13852(7) 0.0535(7) Uani 1 1 d . . . . .
O4 O 0.42451(7) 0.6389(3) 0.36382(7) 0.0435(6) Uani 1 1 d . . . . .
O5 O 0.49875(7) 0.6182(2) 0.39353(6) 0.0377(6) Uani 1 1 d . . . . .
O6 O 0.58407(8) 0.5243(3) 0.46082(7) 0.0475(7) Uani 1 1 d . . . . .
O7 O 0.62689(7) 0.6869(3) 0.28003(7) 0.0434(6) Uani 1 1 d . . . . .
O8 O 0.60937(7) 0.7731(3) 0.21155(7) 0.0433(6) Uani 1 1 d . . . . .
O9 O 0.56864(8) 0.6402(3) 0.13359(7) 0.0481(7) Uani 1 1 d . . . . .
O10 O 0.2847(4) 1.0272(15) 0.1205(4) 0.152(4) Uiso 0.5 1 d . . P . .
O11 O 0.2485(2) 1.0167(9) 0.0753(2) 0.087(2) Uiso 0.5 1 d . . P . .
O12 O 0.2890(4) 0.8610(13) 0.2028(4) 0.137(4) Uiso 0.5 1 d D . P . .
O13 O 0.2742(3) 1.0378(11) 0.2240(3) 0.104(3) Uiso 0.5 1 d D . P . .
O14 O 0.32316(14) 0.5459(5) 0.25716(13) 0.1049(15) Uani 1 1 d . . . . .
O15 O 0.31626(15) 0.4531(5) 0.30671(13) 0.1056(14) Uani 1 1 d . . . . .
N1 N 0.20807(12) 0.4113(6) 0.01852(12) 0.0789(13) Uani 1 1 d . . . . .
N2 N 0.19118(12) 0.4992(5) -0.00315(12) 0.0754(12) Uani 1 1 d . . . . .
N3 N 0.11721(13) 0.3357(6) -0.10112(12) 0.0840(15) Uani 1 1 d . . . . .
N4 N 0.65035(12) 0.1616(4) 0.57364(10) 0.0646(10) Uani 1 1 d . . . . .
N5 N 0.67795(12) 0.2065(4) 0.59656(11) 0.0655(10) Uani 1 1 d . . . . .
N6 N 0.72466(15) -0.0648(6) 0.68422(15) 0.0986(17) Uani 1 1 d . . . . .
N7 N 0.45327(10) 0.4109(3) 0.02256(8) 0.0466(8) Uani 1 1 d . . . . .
N8 N 0.46302(10) 0.3096(3) 0.00545(8) 0.0485(8) Uani 1 1 d . . . . .
N9 N 0.37669(14) 0.1407(5) -0.08121(11) 0.0728(12) Uani 1 1 d . . . . .
N10 N 0.2531(3) 1.0300(11) 0.1090(3) 0.083(3) Uiso 0.5 1 d . . P . .
N11 N 0.2915(2) 0.9328(9) 0.2303(2) 0.068(2) Uiso 0.5 1 d D . P . .
N12 N 0.31310(13) 0.4511(6) 0.27336(13) 0.0822(14) Uani 1 1 d . . . . .
C1 C 0.47024(10) 0.9895(3) 0.21792(8) 0.0325(7) Uani 1 1 d . . . . .
C2 C 0.46485(10) 0.9413(3) 0.18126(9) 0.0349(8) Uani 1 1 d . . . . .
H2 H 0.4811 0.9758 0.1664 0.042 Uiso 1 1 calc R U . . .
C3 C 0.43653(10) 0.8456(3) 0.16665(8) 0.0339(8) Uani 1 1 d . . . . .
C4 C 0.41396(10) 0.7892(3) 0.18888(9) 0.0336(8) Uani 1 1 d . . . . .
C5 C 0.41765(10) 0.8401(3) 0.22399(9) 0.0331(7) Uani 1 1 d . . . . .
H5 H 0.4012 0.8053 0.2387 0.040 Uiso 1 1 calc R U . . .
C6 C 0.44536(10) 0.9429(3) 0.23864(8) 0.0316(7) Uani 1 1 d . . . . .
C7 C 0.44487(10) 1.0007(3) 0.27640(9) 0.0343(8) Uani 1 1 d . . . . .
H7A H 0.4178 1.0228 0.2769 0.041 Uiso 1 1 calc R U . . .
H7B H 0.4597 1.0888 0.2801 0.041 Uiso 1 1 calc R U . . .
C8 C 0.46160(10) 0.9033(3) 0.30821(8) 0.0320(7) Uani 1 1 d . . . . .
C9 C 0.43569(10) 0.8154(3) 0.32075(9) 0.0341(8) Uani 1 1 d . . . . .
H9A H 0.4088 0.8201 0.3093 0.041 Uiso 1 1 calc R U . . .
C10 C 0.44815(10) 0.7231(3) 0.34915(9) 0.0356(8) Uani 1 1 d . . . . .
C11 C 0.48828(10) 0.7149(3) 0.36554(8) 0.0340(8) Uani 1 1 d . . . . .
C12 C 0.51337(10) 0.8028(3) 0.35410(8) 0.0332(8) Uani 1 1 d . . . . .
H12 H 0.5402 0.7986 0.3658 0.040 Uiso 1 1 calc R U . . .
C13 C 0.50051(10) 0.8991(3) 0.32556(8) 0.0317(7) Uani 1 1 d . . . . .
C14 C 0.53019(10) 0.9962(3) 0.31551(9) 0.0343(8) Uani 1 1 d . . . . .
H14A H 0.5506 1.0155 0.3380 0.041 Uiso 1 1 calc R U . . .
H14B H 0.5173 1.0857 0.3070 0.041 Uiso 1 1 calc R U . . .
C15 C 0.54946(10) 0.9416(3) 0.28579(8) 0.0318(7) Uani 1 1 d . . . . .
C16 C 0.57868(9) 0.8418(3) 0.29645(9) 0.0337(8) Uani 1 1 d . . . . .
H16 H 0.5855 0.8118 0.3214 0.040 Uiso 1 1 calc R U . . .
C17 C 0.59794(10) 0.7856(3) 0.27153(10) 0.0368(8) Uani 1 1 d . . . . .
C18 C 0.58874(10) 0.8325(4) 0.23499(10) 0.0374(8) Uani 1 1 d . . . . .
C19 C 0.56041(10) 0.9321(3) 0.22464(9) 0.0356(8) Uani 1 1 d . . . . .
H19 H 0.5546 0.9648 0.1999 0.043 Uiso 1 1 calc R U . . .
C20 C 0.53989(10) 0.9868(3) 0.24913(9) 0.0335(7) Uani 1 1 d . . . . .
C21 C 0.50571(10) 1.0814(3) 0.23314(9) 0.0358(8) Uani 1 1 d . . . . .
H21A H 0.5115 1.1394 0.2132 0.043 Uiso 1 1 calc R U . . .
H21B H 0.5005 1.1439 0.2525 0.043 Uiso 1 1 calc R U . . .
C22 C 0.39502(12) 0.8394(5) 0.10714(10) 0.0531(11) Uani 1 1 d . . . . .
H22A H 0.3747 0.7828 0.1138 0.080 Uiso 1 1 calc R U . . .
H22B H 0.3952 0.8226 0.0813 0.080 Uiso 1 1 calc R U . . .
H22C H 0.3899 0.9381 0.1106 0.080 Uiso 1 1 calc R U . . .
C23 C 0.36196(10) 0.6337(4) 0.19296(10) 0.0397(8) Uani 1 1 d . . . . .
H23A H 0.3477 0.7110 0.2013 0.048 Uiso 1 1 calc R U . . .
H23B H 0.3758 0.5806 0.2148 0.048 Uiso 1 1 calc R U . . .
C24 C 0.33489(11) 0.5414(4) 0.16704(10) 0.0445(9) Uani 1 1 d . . . . .
H24A H 0.3494 0.4707 0.1565 0.053 Uiso 1 1 calc R U . . .
H24B H 0.3172 0.4932 0.1799 0.053 Uiso 1 1 calc R U . . .
C25 C 0.28834(12) 0.5709(5) 0.10965(11) 0.0530(10) Uani 1 1 d . . . . .
C26 C 0.27922(13) 0.4301(5) 0.10667(13) 0.0585(11) Uani 1 1 d . . . . .
H26 H 0.2913 0.3668 0.1254 0.070 Uiso 1 1 calc R U . . .
C27 C 0.25215(14) 0.3832(6) 0.07583(14) 0.0693(13) Uani 1 1 d . . . . .
H27 H 0.2459 0.2871 0.0734 0.083 Uiso 1 1 calc R U . . .
C28 C 0.23442(13) 0.4745(6) 0.04883(13) 0.0652(13) Uani 1 1 d . . . . .
C29 C 0.24432(14) 0.6167(7) 0.05133(12) 0.0707(15) Uani 1 1 d . . . . .
H29 H 0.2326 0.6795 0.0323 0.085 Uiso 1 1 calc R U . . .
C30 C 0.27157(14) 0.6637(6) 0.08208(12) 0.0641(12) Uani 1 1 d . . . . .
H30 H 0.2787 0.7592 0.0842 0.077 Uiso 1 1 calc R U . . .
C31 C 0.16571(14) 0.4318(8) -0.03523(13) 0.0799(18) Uani 1 1 d . . . . .
C32 C 0.1647(2) 0.2909(9) -0.04508(17) 0.112(3) Uani 1 1 d . . . . .
H32 H 0.1803 0.2246 -0.0295 0.134 Uiso 1 1 calc R U . . .
C33 C 0.1402(2) 0.2503(8) -0.07824(19) 0.125(3) Uani 1 1 d . . . . .
H33 H 0.1401 0.1548 -0.0849 0.150 Uiso 1 1 calc R U . . .
C34 C 0.11870(15) 0.4680(8) -0.09091(14) 0.0809(17) Uani 1 1 d . . . . .
H34 H 0.1023 0.5316 -0.1068 0.097 Uiso 1 1 calc R U . . .
C35 C 0.14234(15) 0.5207(8) -0.05887(14) 0.0880(19) Uani 1 1 d . . . . .
H35 H 0.1422 0.6173 -0.0535 0.106 Uiso 1 1 calc R U . . .
C36 C 0.38359(12) 0.6699(5) 0.35314(12) 0.0532(10) Uani 1 1 d . . . . .
H36A H 0.3795 0.7687 0.3574 0.080 Uiso 1 1 calc R U . . .
H36B H 0.3698 0.6133 0.3678 0.080 Uiso 1 1 calc R U . . .
H36C H 0.3737 0.6485 0.3269 0.080 Uiso 1 1 calc R U . . .
C37 C 0.53883(11) 0.6200(4) 0.41197(9) 0.0396(8) Uani 1 1 d . . . . .
H37A H 0.5463 0.7129 0.4228 0.048 Uiso 1 1 calc R U . . .
H37B H 0.5551 0.5983 0.3945 0.048 Uiso 1 1 calc R U . . .
C38 C 0.54420(11) 0.5116(4) 0.44169(10) 0.0428(9) Uani 1 1 d . . . . .
H38A H 0.5269 0.5296 0.4585 0.051 Uiso 1 1 calc R U . . .
H38B H 0.5387 0.4174 0.4310 0.051 Uiso 1 1 calc R U . . .
C39 C 0.59939(12) 0.4309(4) 0.48740(9) 0.0443(9) Uani 1 1 d . . . . .
C40 C 0.57995(12) 0.3141(4) 0.49527(11) 0.0488(9) Uani 1 1 d . . . . .
H40 H 0.5542 0.2951 0.4819 0.059 Uiso 1 1 calc R U . . .
C41 C 0.59904(13) 0.2249(5) 0.52324(12) 0.0541(10) Uani 1 1 d . . . . .
H41 H 0.5866 0.1417 0.5280 0.065 Uiso 1 1 calc R U . . .
C42 C 0.63543(13) 0.2553(4) 0.54403(11) 0.0522(10) Uani 1 1 d . . . . .
C43 C 0.65514(13) 0.3724(5) 0.53521(12) 0.0598(12) Uani 1 1 d . . . . .
H43 H 0.6807 0.3926 0.5488 0.072 Uiso 1 1 calc R U . . .
C44 C 0.63714(13) 0.4572(5) 0.50682(12) 0.0576(11) Uani 1 1 d . . . . .
H44 H 0.6506 0.5351 0.5003 0.069 Uiso 1 1 calc R U . . .
C45 C 0.69173(15) 0.1093(6) 0.62657(13) 0.0667(13) Uani 1 1 d . . . . .
C46 C 0.67750(17) -0.0198(7) 0.62845(16) 0.0816(16) Uani 1 1 d . . . . .
H46 H 0.6560 -0.0521 0.6101 0.098 Uiso 1 1 calc R U . . .
C47 C 0.69474(18) -0.1042(7) 0.65759(18) 0.097(2) Uani 1 1 d . . . . .
H47 H 0.6847 -0.1953 0.6587 0.117 Uiso 1 1 calc R U . . .
C48 C 0.73772(16) 0.0661(7) 0.68209(16) 0.0795(16) Uani 1 1 d . . . . .
H48 H 0.7585 0.0983 0.7013 0.095 Uiso 1 1 calc R U . . .
C49 C 0.72244(15) 0.1552(6) 0.65348(14) 0.0733(14) Uani 1 1 d . . . . .
H49 H 0.7329 0.2457 0.6524 0.088 Uiso 1 1 calc R U . . .
C50 C 0.63524(12) 0.6328(4) 0.31676(11) 0.0469(9) Uani 1 1 d . . . . .
H50A H 0.6462 0.7068 0.3342 0.070 Uiso 1 1 calc R U . . .
H50B H 0.6539 0.5564 0.3189 0.070 Uiso 1 1 calc R U . . .
H50C H 0.6113 0.5983 0.3224 0.070 Uiso 1 1 calc R U . . .
C51 C 0.59929(13) 0.8194(4) 0.17392(10) 0.0499(10) Uani 1 1 d . . . . .
H51A H 0.6201 0.7908 0.1619 0.060 Uiso 1 1 calc R U . . .
H51B H 0.5983 0.9224 0.1737 0.060 Uiso 1 1 calc R U . . .
C52 C 0.56136(12) 0.7651(4) 0.15157(10) 0.0461(9) Uani 1 1 d . . . . .
H52A H 0.5436 0.7458 0.1678 0.055 Uiso 1 1 calc R U . . .
H52B H 0.5491 0.8352 0.1331 0.055 Uiso 1 1 calc R U . . .
C53 C 0.53934(12) 0.5854(4) 0.10742(10) 0.0436(9) Uani 1 1 d . . . . .
C54 C 0.50107(12) 0.6331(4) 0.10002(10) 0.0453(9) Uani 1 1 d . . . . .
H54 H 0.4940 0.7067 0.1141 0.054 Uiso 1 1 calc R U . . .
C55 C 0.47361(12) 0.5715(4) 0.07187(10) 0.0457(9) Uani 1 1 d . . . . .
H55 H 0.4476 0.6038 0.0666 0.055 Uiso 1 1 calc R U . . .
C56 C 0.48367(12) 0.4632(4) 0.05130(9) 0.0424(9) Uani 1 1 d . . . . .
C57 C 0.52158(12) 0.4136(4) 0.05962(10) 0.0459(9) Uani 1 1 d . . . . .
H57 H 0.5283 0.3372 0.0462 0.055 Uiso 1 1 calc R U . . .
C58 C 0.54946(12) 0.4744(4) 0.08714(10) 0.0445(9) Uani 1 1 d . . . . .
H58 H 0.5754 0.4413 0.0924 0.053 Uiso 1 1 calc R U . . .
C59 C 0.43244(13) 0.2584(4) -0.02344(10) 0.0492(10) Uani 1 1 d . . . . .
C60 C 0.39396(14) 0.3051(5) -0.03145(13) 0.0620(12) Uani 1 1 d . . . . .
H60 H 0.3860 0.3775 -0.0176 0.074 Uiso 1 1 calc R U . . .
C61 C 0.36814(16) 0.2421(6) -0.06029(15) 0.0745(14) Uani 1 1 d . . . . .
H61 H 0.3421 0.2738 -0.0656 0.089 Uiso 1 1 calc R U . . .
C62 C 0.41294(16) 0.0961(5) -0.07294(12) 0.0621(12) Uani 1 1 d . . . . .
H62 H 0.4199 0.0227 -0.0872 0.075 Uiso 1 1 calc R U . . .
C63 C 0.44142(14) 0.1519(5) -0.04434(11) 0.0558(11) Uani 1 1 d . . . . .
H63 H 0.4671 0.1160 -0.0393 0.067 Uiso 1 1 calc R U . . .
C64 C 0.2227(3) 1.0472(12) 0.1276(3) 0.074(3) Uiso 0.5 1 d . . P . .
H64A H 0.2335 1.0493 0.1542 0.111 Uiso 0.5 1 calc R U P . .
H64B H 0.2045 0.9693 0.1215 0.111 Uiso 0.5 1 calc R U P . .
H64C H 0.2090 1.1347 0.1198 0.111 Uiso 0.5 1 calc R U P . .
C65 C 0.3264(2) 0.9219(9) 0.2582(2) 0.053(2) Uiso 0.5 1 d . . P . .
H65A H 0.3306 0.8246 0.2660 0.080 Uiso 0.5 1 calc R U P . .
H65B H 0.3244 0.9792 0.2794 0.080 Uiso 0.5 1 calc R U P . .
H65C H 0.3482 0.9544 0.2485 0.080 Uiso 0.5 1 calc R U P . .
C66 C 0.29896(15) 0.3227(7) 0.25305(16) 0.0792(16) Uani 1 1 d . . . . .
H66A H 0.2796 0.3463 0.2305 0.119 Uiso 1 1 calc R U . . .
H66B H 0.2872 0.2622 0.2686 0.119 Uiso 1 1 calc R U . . .
H66C H 0.3207 0.2741 0.2466 0.119 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C3 1.390(4) . ?
O1 C22 1.447(4) . ?
O2 C4 1.374(4) . ?
O2 C23 1.433(4) . ?
O3 C25 1.353(5) . ?
O3 C24 1.439(4) . ?
O4 C10 1.369(4) . ?
O4 C36 1.444(5) . ?
O5 C11 1.382(4) . ?
O5 C37 1.428(4) . ?
O6 C39 1.354(4) . ?
O6 C38 1.433(4) . ?
O7 C17 1.380(4) . ?
O7 C50 1.431(5) . ?
O8 C18 1.389(4) . ?
O8 C51 1.437(5) . ?
O9 C53 1.355(5) . ?
O9 C52 1.428(5) . ?
O10 N10 1.103(15) . ?
O11 N10 1.236(12) . ?
O12 N11 1.223(13) . ?
O13 N11 1.176(11) . ?
O14 N12 1.193(6) . ?
O15 N12 1.224(6) . ?
N1 N2 1.225(6) . ?
N1 C28 1.424(6) . ?
N2 C31 1.470(7) . ?
N3 C33 1.320(8) . ?
N3 C34 1.325(8) . ?
N4 N5 1.219(5) . ?
N4 C42 1.428(5) . ?
N5 C45 1.453(6) . ?
N6 C47 1.328(8) . ?
N6 C48 1.349(8) . ?
N7 N8 1.257(5) . ?
N7 C56 1.423(5) . ?
N8 C59 1.426(5) . ?
N9 C62 1.322(7) . ?
N9 C61 1.328(7) . ?
N10 C64 1.425(15) . ?
N11 C65 1.423(12) . ?
N12 C66 1.474(8) . ?
C1 C6 1.379(5) . ?
C1 C2 1.415(5) . ?
C1 C21 1.534(5) . ?
C2 C3 1.377(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.392(5) . ?
C4 C5 1.377(5) . ?
C5 C6 1.411(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.519(5) . ?
C7 C8 1.519(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C13 1.382(5) . ?
C8 C9 1.408(5) . ?
C9 C10 1.374(5) . ?
C9 H9A 0.9500 . ?
C10 C11 1.415(5) . ?
C11 C12 1.367(5) . ?
C12 C13 1.405(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.519(5) . ?
C14 C15 1.527(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.400(5) . ?
C15 C20 1.400(4) . ?
C16 C17 1.387(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.401(5) . ?
C18 C19 1.376(5) . ?
C19 C20 1.399(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.522(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.487(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C30 1.386(6) . ?
C25 C26 1.390(7) . ?
C26 C27 1.390(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.372(8) . ?
C27 H27 0.9500 . ?
C28 C29 1.409(8) . ?
C29 C30 1.392(7) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C35 1.362(9) . ?
C31 C32 1.401(10) . ?
C32 C33 1.391(8) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C35 1.386(7) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.502(5) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.385(6) . ?
C39 C44 1.389(6) . ?
C40 C41 1.397(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.373(6) . ?
C41 H41 0.9500 . ?
C42 C43 1.405(7) . ?
C43 C44 1.371(6) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 C46 1.347(8) . ?
C45 C49 1.370(7) . ?
C46 C47 1.379(8) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 C49 1.377(7) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.501(6) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.399(6) . ?
C53 C58 1.403(6) . ?
C54 C55 1.387(5) . ?
C54 H54 0.9500 . ?
C55 C56 1.389(5) . ?
C55 H55 0.9500 . ?
C56 C57 1.392(6) . ?
C57 C58 1.378(5) . ?
C57 H57 0.9500 . ?
C58 H58 0.9500 . ?
C59 C63 1.369(6) . ?
C59 C60 1.402(6) . ?
C60 C61 1.380(6) . ?
C60 H60 0.9500 . ?
C61 H61 0.9500 . ?
C62 C63 1.394(6) . ?
C62 H62 0.9500 . ?
C63 H63 0.9500 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 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
C3 O1 C22 112.7(3) . . ?
C4 O2 C23 118.1(3) . . ?
C25 O3 C24 118.2(3) . . ?
C10 O4 C36 116.1(3) . . ?
C11 O5 C37 114.6(3) . . ?
C39 O6 C38 119.3(3) . . ?
C17 O7 C50 116.4(3) . . ?
C18 O8 C51 116.2(3) . . ?
C53 O9 C52 118.2(3) . . ?
N2 N1 C28 111.1(5) . . ?
N1 N2 C31 110.3(5) . . ?
C33 N3 C34 115.7(5) . . ?
N5 N4 C42 114.3(4) . . ?
N4 N5 C45 112.5(4) . . ?
C47 N6 C48 116.5(5) . . ?
N8 N7 C56 114.0(3) . . ?
N7 N8 C59 113.5(4) . . ?
C62 N9 C61 116.4(4) . . ?
O10 N10 O11 105.7(12) . . ?
O10 N10 C64 129.3(13) . . ?
O11 N10 C64 124.9(10) . . ?
O13 N11 O12 112.6(10) . . ?
O13 N11 C65 122.3(9) . . ?
O12 N11 C65 116.8(10) . . ?
O14 N12 O15 122.5(6) . . ?
O14 N12 C66 119.0(5) . . ?
O15 N12 C66 118.3(5) . . ?
C6 C1 C2 118.5(3) . . ?
C6 C1 C21 123.9(3) . . ?
C2 C1 C21 117.4(3) . . ?
C3 C2 C1 121.5(3) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C2 C3 O1 119.3(3) . . ?
C2 C3 C4 119.5(3) . . ?
O1 C3 C4 121.1(3) . . ?
C5 C4 O2 125.2(3) . . ?
C5 C4 C3 119.4(3) . . ?
O2 C4 C3 115.4(3) . . ?
C4 C5 C6 121.3(3) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C5 119.4(3) . . ?
C1 C6 C7 123.4(3) . . ?
C5 C6 C7 117.2(3) . . ?
C6 C7 C8 114.4(3) . . ?
C6 C7 H7A 108.7 . . ?
C8 C7 H7A 108.7 . . ?
C6 C7 H7B 108.7 . . ?
C8 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C13 C8 C9 119.1(3) . . ?
C13 C8 C7 123.3(3) . . ?
C9 C8 C7 117.6(3) . . ?
C10 C9 C8 121.8(3) . . ?
C10 C9 H9A 119.1 . . ?
C8 C9 H9A 119.1 . . ?
O4 C10 C9 125.0(3) . . ?
O4 C10 C11 116.4(3) . . ?
C9 C10 C11 118.6(3) . . ?
C12 C11 O5 124.9(3) . . ?
C12 C11 C10 119.6(3) . . ?
O5 C11 C10 115.4(3) . . ?
C11 C12 C13 121.7(3) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C8 C13 C12 119.0(3) . . ?
C8 C13 C14 122.8(3) . . ?
C12 C13 C14 118.1(3) . . ?
C13 C14 C15 115.1(3) . . ?
C13 C14 H14A 108.5 . . ?
C15 C14 H14A 108.5 . . ?
C13 C14 H14B 108.5 . . ?
C15 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
C16 C15 C20 119.0(3) . . ?
C16 C15 C14 117.2(3) . . ?
C20 C15 C14 123.8(3) . . ?
C17 C16 C15 121.7(3) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
O7 C17 C16 124.9(3) . . ?
O7 C17 C18 115.8(3) . . ?
C16 C17 C18 119.3(3) . . ?
C19 C18 O8 124.6(3) . . ?
C19 C18 C17 119.0(3) . . ?
O8 C18 C17 116.4(3) . . ?
C18 C19 C20 122.5(3) . . ?
C18 C19 H19 118.8 . . ?
C20 C19 H19 118.8 . . ?
C19 C20 C15 118.6(3) . . ?
C19 C20 C21 117.3(3) . . ?
C15 C20 C21 123.9(3) . . ?
C20 C21 C1 108.1(3) . . ?
C20 C21 H21A 110.1 . . ?
C1 C21 H21A 110.1 . . ?
C20 C21 H21B 110.1 . . ?
C1 C21 H21B 110.1 . . ?
H21A C21 H21B 108.4 . . ?
O1 C22 H22A 109.5 . . ?
O1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 C23 C24 106.0(3) . . ?
O2 C23 H23A 110.5 . . ?
C24 C23 H23A 110.5 . . ?
O2 C23 H23B 110.5 . . ?
C24 C23 H23B 110.5 . . ?
H23A C23 H23B 108.7 . . ?
O3 C24 C23 106.0(3) . . ?
O3 C24 H24A 110.5 . . ?
C23 C24 H24A 110.5 . . ?
O3 C24 H24B 110.5 . . ?
C23 C24 H24B 110.5 . . ?
H24A C24 H24B 108.7 . . ?
O3 C25 C30 113.9(4) . . ?
O3 C25 C26 125.0(4) . . ?
C30 C25 C26 121.0(4) . . ?
C27 C26 C25 119.0(5) . . ?
C27 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
C28 C27 C26 120.7(5) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C27 C28 C29 120.5(4) . . ?
C27 C28 N1 114.5(5) . . ?
C29 C28 N1 125.0(5) . . ?
C30 C29 C28 118.9(5) . . ?
C30 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
C25 C30 C29 119.9(5) . . ?
C25 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C35 C31 C32 117.5(5) . . ?
C35 C31 N2 114.6(6) . . ?
C32 C31 N2 127.8(5) . . ?
C33 C32 C31 118.5(6) . . ?
C33 C32 H32 120.8 . . ?
C31 C32 H32 120.8 . . ?
N3 C33 C32 124.4(8) . . ?
N3 C33 H33 117.8 . . ?
C32 C33 H33 117.8 . . ?
N3 C34 C35 125.1(6) . . ?
N3 C34 H34 117.5 . . ?
C35 C34 H34 117.5 . . ?
C31 C35 C34 118.9(7) . . ?
C31 C35 H35 120.5 . . ?
C34 C35 H35 120.5 . . ?
O4 C36 H36A 109.5 . . ?
O4 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
O4 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O5 C37 C38 106.7(3) . . ?
O5 C37 H37A 110.4 . . ?
C38 C37 H37A 110.4 . . ?
O5 C37 H37B 110.4 . . ?
C38 C37 H37B 110.4 . . ?
H37A C37 H37B 108.6 . . ?
O6 C38 C37 104.4(3) . . ?
O6 C38 H38A 110.9 . . ?
C37 C38 H38A 110.9 . . ?
O6 C38 H38B 110.9 . . ?
C37 C38 H38B 110.9 . . ?
H38A C38 H38B 108.9 . . ?
O6 C39 C40 123.9(4) . . ?
O6 C39 C44 115.7(4) . . ?
C40 C39 C44 120.4(4) . . ?
C39 C40 C41 118.5(4) . . ?
C39 C40 H40 120.8 . . ?
C41 C40 H40 120.8 . . ?
C42 C41 C40 121.3(4) . . ?
C42 C41 H41 119.4 . . ?
C40 C41 H41 119.4 . . ?
C41 C42 C43 119.5(4) . . ?
C41 C42 N4 115.6(4) . . ?
C43 C42 N4 124.9(4) . . ?
C44 C43 C42 119.4(4) . . ?
C44 C43 H43 120.3 . . ?
C42 C43 H43 120.3 . . ?
C43 C44 C39 120.8(4) . . ?
C43 C44 H44 119.6 . . ?
C39 C44 H44 119.6 . . ?
C46 C45 C49 120.1(5) . . ?
C46 C45 N5 124.7(5) . . ?
C49 C45 N5 115.1(5) . . ?
C45 C46 C47 118.7(5) . . ?
C45 C46 H46 120.7 . . ?
C47 C46 H46 120.7 . . ?
N6 C47 C46 123.5(6) . . ?
N6 C47 H47 118.3 . . ?
C46 C47 H47 118.3 . . ?
N6 C48 C49 123.2(5) . . ?
N6 C48 H48 118.4 . . ?
C49 C48 H48 118.4 . . ?
C45 C49 C48 118.0(6) . . ?
C45 C49 H49 121.0 . . ?
C48 C49 H49 121.0 . . ?
O7 C50 H50A 109.5 . . ?
O7 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
O7 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
O8 C51 C52 114.9(3) . . ?
O8 C51 H51A 108.5 . . ?
C52 C51 H51A 108.5 . . ?
O8 C51 H51B 108.5 . . ?
C52 C51 H51B 108.5 . . ?
H51A C51 H51B 107.5 . . ?
O9 C52 C51 108.4(3) . . ?
O9 C52 H52A 110.0 . . ?
C51 C52 H52A 110.0 . . ?
O9 C52 H52B 110.0 . . ?
C51 C52 H52B 110.0 . . ?
H52A C52 H52B 108.4 . . ?
O9 C53 C54 124.1(4) . . ?
O9 C53 C58 115.7(4) . . ?
C54 C53 C58 120.2(4) . . ?
C55 C54 C53 119.2(4) . . ?
C55 C54 H54 120.4 . . ?
C53 C54 H54 120.4 . . ?
C54 C55 C56 120.8(4) . . ?
C54 C55 H55 119.6 . . ?
C56 C55 H55 119.6 . . ?
C57 C56 C55 119.6(4) . . ?
C57 C56 N7 124.7(4) . . ?
C55 C56 N7 115.7(4) . . ?
C58 C57 C56 120.6(4) . . ?
C58 C57 H57 119.7 . . ?
C56 C57 H57 119.7 . . ?
C57 C58 C53 119.6(4) . . ?
C57 C58 H58 120.2 . . ?
C53 C58 H58 120.2 . . ?
C63 C59 C60 117.6(4) . . ?
C63 C59 N8 116.8(4) . . ?
C60 C59 N8 125.6(4) . . ?
C61 C60 C59 117.5(5) . . ?
C61 C60 H60 121.2 . . ?
C59 C60 H60 121.2 . . ?
N9 C61 C60 125.4(5) . . ?
N9 C61 H61 117.3 . . ?
C60 C61 H61 117.3 . . ?
N9 C62 C63 123.1(5) . . ?
N9 C62 H62 118.5 . . ?
C63 C62 H62 118.5 . . ?
C59 C63 C62 120.0(5) . . ?
C59 C63 H63 120.0 . . ?
C62 C63 H63 120.0 . . ?
N10 C64 H64A 109.5 . . ?
N10 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
N10 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N11 C65 H65A 109.5 . . ?
N11 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
N11 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
N12 C66 H66A 109.5 . . ?
N12 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
N12 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 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
C28 N1 N2 C31 176.9(4) . . . . ?
C42 N4 N5 C45 178.8(4) . . . . ?
C56 N7 N8 C59 -179.6(3) . . . . ?
C6 C1 C2 C3 -2.7(5) . . . . ?
C21 C1 C2 C3 172.4(3) . . . . ?
C1 C2 C3 O1 179.7(3) . . . . ?
C1 C2 C3 C4 -3.4(5) . . . . ?
C22 O1 C3 C2 -116.8(4) . . . . ?
C22 O1 C3 C4 66.3(4) . . . . ?
C23 O2 C4 C5 4.7(5) . . . . ?
C23 O2 C4 C3 -173.9(3) . . . . ?
C2 C3 C4 C5 6.5(5) . . . . ?
O1 C3 C4 C5 -176.7(3) . . . . ?
C2 C3 C4 O2 -174.8(3) . . . . ?
O1 C3 C4 O2 2.0(4) . . . . ?
O2 C4 C5 C6 177.9(3) . . . . ?
C3 C4 C5 C6 -3.6(5) . . . . ?
C2 C1 C6 C5 5.6(4) . . . . ?
C21 C1 C6 C5 -169.2(3) . . . . ?
C2 C1 C6 C7 -171.9(3) . . . . ?
C21 C1 C6 C7 13.4(5) . . . . ?
C4 C5 C6 C1 -2.5(5) . . . . ?
C4 C5 C6 C7 175.1(3) . . . . ?
C1 C6 C7 C8 -107.4(4) . . . . ?
C5 C6 C7 C8 75.1(4) . . . . ?
C6 C7 C8 C13 87.8(4) . . . . ?
C6 C7 C8 C9 -93.5(4) . . . . ?
C13 C8 C9 C10 -1.7(5) . . . . ?
C7 C8 C9 C10 179.5(3) . . . . ?
C36 O4 C10 C9 -12.3(5) . . . . ?
C36 O4 C10 C11 166.2(3) . . . . ?
C8 C9 C10 O4 177.1(3) . . . . ?
C8 C9 C10 C11 -1.3(5) . . . . ?
C37 O5 C11 C12 3.1(4) . . . . ?
C37 O5 C11 C10 -174.6(3) . . . . ?
O4 C10 C11 C12 -175.4(3) . . . . ?
C9 C10 C11 C12 3.1(5) . . . . ?
O4 C10 C11 O5 2.5(4) . . . . ?
C9 C10 C11 O5 -179.0(3) . . . . ?
O5 C11 C12 C13 -179.6(3) . . . . ?
C10 C11 C12 C13 -1.9(5) . . . . ?
C9 C8 C13 C12 3.0(4) . . . . ?
C7 C8 C13 C12 -178.3(3) . . . . ?
C9 C8 C13 C14 -176.1(3) . . . . ?
C7 C8 C13 C14 2.6(5) . . . . ?
C11 C12 C13 C8 -1.2(5) . . . . ?
C11 C12 C13 C14 177.9(3) . . . . ?
C8 C13 C14 C15 -90.7(4) . . . . ?
C12 C13 C14 C15 90.2(3) . . . . ?
C13 C14 C15 C16 -77.5(4) . . . . ?
C13 C14 C15 C20 103.3(4) . . . . ?
C20 C15 C16 C17 -0.8(5) . . . . ?
C14 C15 C16 C17 180.0(3) . . . . ?
C50 O7 C17 C16 4.6(5) . . . . ?
C50 O7 C17 C18 -176.9(3) . . . . ?
C15 C16 C17 O7 -179.8(3) . . . . ?
C15 C16 C17 C18 1.8(5) . . . . ?
C51 O8 C18 C19 -1.0(5) . . . . ?
C51 O8 C18 C17 178.8(3) . . . . ?
O7 C17 C18 C19 -179.4(3) . . . . ?
C16 C17 C18 C19 -0.8(5) . . . . ?
O7 C17 C18 O8 0.8(4) . . . . ?
C16 C17 C18 O8 179.4(3) . . . . ?
O8 C18 C19 C20 178.7(3) . . . . ?
C17 C18 C19 C20 -1.1(5) . . . . ?
C18 C19 C20 C15 2.1(5) . . . . ?
C18 C19 C20 C21 -172.0(3) . . . . ?
C16 C15 C20 C19 -1.1(4) . . . . ?
C14 C15 C20 C19 178.1(3) . . . . ?
C16 C15 C20 C21 172.5(3) . . . . ?
C14 C15 C20 C21 -8.3(5) . . . . ?
C19 C20 C21 C1 83.7(4) . . . . ?
C15 C20 C21 C1 -90.0(4) . . . . ?
C6 C1 C21 C20 87.8(4) . . . . ?
C2 C1 C21 C20 -87.0(3) . . . . ?
C4 O2 C23 C24 171.6(3) . . . . ?
C25 O3 C24 C23 175.4(3) . . . . ?
O2 C23 C24 O3 -66.2(4) . . . . ?
C24 O3 C25 C30 -174.6(4) . . . . ?
C24 O3 C25 C26 5.6(6) . . . . ?
O3 C25 C26 C27 178.3(4) . . . . ?
C30 C25 C26 C27 -1.5(7) . . . . ?
C25 C26 C27 C28 -0.5(8) . . . . ?
C26 C27 C28 C29 2.1(8) . . . . ?
C26 C27 C28 N1 178.6(5) . . . . ?
N2 N1 C28 C27 174.9(4) . . . . ?
N2 N1 C28 C29 -8.7(7) . . . . ?
C27 C28 C29 C30 -1.7(7) . . . . ?
N1 C28 C29 C30 -177.8(5) . . . . ?
O3 C25 C30 C29 -178.0(4) . . . . ?
C26 C25 C30 C29 1.9(7) . . . . ?
C28 C29 C30 C25 -0.3(7) . . . . ?
N1 N2 C31 C35 172.8(5) . . . . ?
N1 N2 C31 C32 -11.5(8) . . . . ?
C35 C31 C32 C33 0.4(10) . . . . ?
N2 C31 C32 C33 -175.2(6) . . . . ?
C34 N3 C33 C32 0.6(11) . . . . ?
C31 C32 C33 N3 -1.1(13) . . . . ?
C33 N3 C34 C35 0.5(9) . . . . ?
C32 C31 C35 C34 0.6(9) . . . . ?
N2 C31 C35 C34 176.8(5) . . . . ?
N3 C34 C35 C31 -1.1(9) . . . . ?
C11 O5 C37 C38 178.6(3) . . . . ?
C39 O6 C38 C37 -173.7(3) . . . . ?
O5 C37 C38 O6 -176.2(3) . . . . ?
C38 O6 C39 C40 6.4(5) . . . . ?
C38 O6 C39 C44 -174.6(4) . . . . ?
O6 C39 C40 C41 179.5(4) . . . . ?
C44 C39 C40 C41 0.5(6) . . . . ?
C39 C40 C41 C42 3.6(6) . . . . ?
C40 C41 C42 C43 -5.1(7) . . . . ?
C40 C41 C42 N4 175.0(4) . . . . ?
N5 N4 C42 C41 -163.7(4) . . . . ?
N5 N4 C42 C43 16.4(6) . . . . ?
C41 C42 C43 C44 2.3(7) . . . . ?
N4 C42 C43 C44 -177.8(4) . . . . ?
C42 C43 C44 C39 1.7(7) . . . . ?
O6 C39 C44 C43 177.7(4) . . . . ?
C40 C39 C44 C43 -3.2(7) . . . . ?
N4 N5 C45 C46 3.6(7) . . . . ?
N4 N5 C45 C49 -179.1(5) . . . . ?
C49 C45 C46 C47 -0.8(9) . . . . ?
N5 C45 C46 C47 176.4(6) . . . . ?
C48 N6 C47 C46 1.1(11) . . . . ?
C45 C46 C47 N6 0.4(11) . . . . ?
C47 N6 C48 C49 -2.3(10) . . . . ?
C46 C45 C49 C48 -0.4(8) . . . . ?
N5 C45 C49 C48 -177.9(5) . . . . ?
N6 C48 C49 C45 2.0(9) . . . . ?
C18 O8 C51 C52 -73.6(4) . . . . ?
C53 O9 C52 C51 -169.8(3) . . . . ?
O8 C51 C52 O9 -92.4(4) . . . . ?
C52 O9 C53 C54 -8.4(5) . . . . ?
C52 O9 C53 C58 171.5(3) . . . . ?
O9 C53 C54 C55 178.3(3) . . . . ?
C58 C53 C54 C55 -1.6(6) . . . . ?
C53 C54 C55 C56 0.4(6) . . . . ?
C54 C55 C56 C57 1.6(6) . . . . ?
C54 C55 C56 N7 -178.4(3) . . . . ?
N8 N7 C56 C57 2.6(5) . . . . ?
N8 N7 C56 C55 -177.4(3) . . . . ?
C55 C56 C57 C58 -2.4(6) . . . . ?
N7 C56 C57 C58 177.6(3) . . . . ?
C56 C57 C58 C53 1.3(6) . . . . ?
O9 C53 C58 C57 -179.1(3) . . . . ?
C54 C53 C58 C57 0.7(5) . . . . ?
N7 N8 C59 C63 177.2(3) . . . . ?
N7 N8 C59 C60 -4.8(6) . . . . ?
C63 C59 C60 C61 -1.2(7) . . . . ?
N8 C59 C60 C61 -179.2(4) . . . . ?
C62 N9 C61 C60 1.2(8) . . . . ?
C59 C60 C61 N9 -0.1(8) . . . . ?
C61 N9 C62 C63 -1.0(7) . . . . ?
C60 C59 C63 C62 1.5(6) . . . . ?
N8 C59 C63 C62 179.7(4) . . . . ?
N9 C62 C63 C59 -0.4(7) . . . . ?

_refine_diff_density_max         1.275
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.110


# start Validation Reply Form
_vrf_DIFF019_I                   
;
PROBLEM: _diffrn_standards_number is missing
RESPONSE: not applicable
;
_vrf_DIFF020_I                   
;
PROBLEM: _diffrn_standards_interval_count and
RESPONSE: not applicable
;
_vrf_DIFF022_I                   
;
PROBLEM: _diffrn_standards_decay_% is missing
RESPONSE: not applicable
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_C_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1859217'
_audit_update_record             
;
2018-07-30 deposited with the CCDC.
2018-08-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
;
octaaquodibis(4-[2-(4-pyridyl)diazenyl]-benzoate)sodium(I) 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H16 N3 Na O6'
_chemical_formula_weight         321.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.1765(4)
_cell_length_b                   7.0883(4)
_cell_length_c                   17.5927(6)
_cell_angle_alpha                88.175(4)
_cell_angle_beta                 83.629(5)
_cell_angle_gamma                69.716(6)
_cell_volume                     717.98(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5957
_cell_measurement_theta_min      5.1010
_cell_measurement_theta_max      73.7970

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_F_000             336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.274
_shelx_estimated_absorpt_T_min   0.794
_shelx_estimated_absorpt_T_max   0.951
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Agilent Supernova'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13098
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         5.059
_diffrn_reflns_theta_max         73.971
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measured_fraction_theta_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_point_group_measured_fraction_full 0.965
_reflns_number_total             2761
_reflns_number_gt                2329
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0570P)²+0.0305P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2761
_refine_ls_number_parameters     263
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.0973
_refine_ls_wR_factor_gt          0.0911
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Na2 Na 1.07261(8) 0.11831(7) 0.07641(3) 0.01649(16) Uani 1 1 d . . . . .
O4 O 1.32441(19) -0.17316(16) 0.12221(7) 0.0276(3) Uani 1 1 d . . . . .
O3 O 0.77309(18) 0.43012(15) 0.05168(6) 0.0190(2) Uani 1 1 d . . . . .
O6 O 0.77737(17) -0.02151(16) 0.05256(6) 0.0186(2) Uani 1 1 d . . . . .
O5 O 1.33154(17) 0.32516(15) 0.07651(6) 0.0188(2) Uani 1 1 d . . . . .
O1 O -0.12916(16) 0.43261(15) 0.79846(6) 0.0200(2) Uani 1 1 d . . . . .
O2 O 0.22806(16) 0.30868(14) 0.83542(6) 0.0190(2) Uani 1 1 d . . . . .
N3 N 0.4379(2) 0.25027(17) 0.46860(7) 0.0188(3) Uani 1 1 d . . . . .
N2 N 0.6486(2) 0.22781(17) 0.45174(7) 0.0186(3) Uani 1 1 d . . . . .
N1 N 0.8921(2) 0.16960(17) 0.21659(7) 0.0193(3) Uani 1 1 d . . . . .
C6 C 0.3649(2) 0.27076(19) 0.54866(8) 0.0165(3) Uani 1 1 d . . . . .
C7 C 0.5145(2) 0.2509(2) 0.60482(8) 0.0192(3) Uani 1 1 d . . . . .
C10 C 0.0408(2) 0.3416(2) 0.64586(8) 0.0178(3) Uani 1 1 d . . . . .
C9 C 0.1880(2) 0.32366(18) 0.70231(8) 0.0153(3) Uani 1 1 d . . . . .
C3 C 0.7192(2) 0.20916(18) 0.37143(8) 0.0165(3) Uani 1 1 d . . . . .
C12 C 0.0879(2) 0.35824(19) 0.78473(8) 0.0157(3) Uani 1 1 d . . . . .
C4 C 0.5704(2) 0.2378(2) 0.31503(9) 0.0201(3) Uani 1 1 d . . . . .
C11 C 0.1279(2) 0.3130(2) 0.56927(8) 0.0189(3) Uani 1 1 d . . . . .
C8 C 0.4267(2) 0.2764(2) 0.68098(8) 0.0179(3) Uani 1 1 d . . . . .
C2 C 0.9562(2) 0.1619(2) 0.34928(8) 0.0191(3) Uani 1 1 d . . . . .
C1 C 1.0322(2) 0.1424(2) 0.27176(8) 0.0195(3) Uani 1 1 d . . . . .
C5 C 0.6640(2) 0.2172(2) 0.23944(9) 0.0215(3) Uani 1 1 d . . . . .
H7 H 0.679(3) 0.219(3) 0.5913(11) 0.020(4) Uiso 1 1 d . . . . .
H8 H 0.526(3) 0.266(3) 0.7191(11) 0.023(4) Uiso 1 1 d . . . . .
H4 H 0.406(4) 0.269(3) 0.3289(12) 0.030(5) Uiso 1 1 d . . . . .
H10 H -0.121(3) 0.371(3) 0.6599(11) 0.022(4) Uiso 1 1 d . . . . .
H11 H 0.032(3) 0.321(3) 0.5304(11) 0.020(4) Uiso 1 1 d . . . . .
H2 H 1.061(3) 0.147(3) 0.3850(12) 0.028(5) Uiso 1 1 d . . . . .
H5 H 0.559(3) 0.238(3) 0.1987(12) 0.028(5) Uiso 1 1 d . . . . .
H1 H 1.199(3) 0.109(3) 0.2554(11) 0.023(4) Uiso 1 1 d . . . . .
H4A H 1.454(4) -0.203(3) 0.1395(13) 0.033(5) Uiso 1 1 d . . . . .
H3A H 0.650(4) 0.414(3) 0.0631(14) 0.036(6) Uiso 1 1 d . . . . .
H3B H 0.785(3) 0.503(3) 0.0843(12) 0.027(5) Uiso 1 1 d . . . . .
H5A H 1.287(4) 0.402(4) 0.0366(15) 0.044(6) Uiso 1 1 d . . . . .
H5B H 1.261(4) 0.410(3) 0.1155(14) 0.034(5) Uiso 1 1 d . . . . .
H4B H 1.253(4) -0.245(3) 0.1479(13) 0.034(5) Uiso 1 1 d . . . . .
H6A H 0.784(3) -0.115(3) 0.0844(13) 0.033(5) Uiso 1 1 d . . . . .
H6B H 0.647(4) 0.063(4) 0.0596(13) 0.038(6) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na2 O4 2.2980(12) . ?
Na2 O6 2.3810(11) 2_755 ?
Na2 O3 2.4039(11) . ?
Na2 O6 2.4358(11) . ?
Na2 O5 2.5168(11) . ?
Na2 N1 2.5734(13) . ?
Na2 Na2 3.5653(10) 2_755 ?
O6 Na2 2.3810(11) 2_755 ?
O1 C12 1.2570(17) . ?
O2 C12 1.2682(17) . ?
N3 N2 1.2571(17) . ?
N3 C6 1.4264(19) . ?
N2 C3 1.4278(19) . ?
N1 C1 1.3369(19) . ?
N1 C5 1.3464(19) . ?
C6 C11 1.3961(19) . ?
C6 C7 1.3978(19) . ?
C7 C8 1.381(2) . ?
C10 C11 1.388(2) . ?
C10 C9 1.3935(19) . ?
C9 C8 1.4034(19) . ?
C9 C12 1.505(2) . ?
C3 C4 1.389(2) . ?
C3 C2 1.3961(19) . ?
C4 C5 1.381(2) . ?
C2 C1 1.387(2) . ?

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
O4 Na2 O6 91.89(4) . 2_755 ?
O4 Na2 O3 169.54(5) . . ?
O6 Na2 O3 98.27(4) 2_755 . ?
O4 Na2 O6 96.03(4) . . ?
O6 Na2 O6 84.51(4) 2_755 . ?
O3 Na2 O6 82.52(4) . . ?
O4 Na2 O5 97.10(4) . . ?
O6 Na2 O5 89.48(4) 2_755 . ?
O3 Na2 O5 85.56(4) . . ?
O6 Na2 O5 165.73(4) . . ?
O4 Na2 N1 83.50(4) . . ?
O6 Na2 N1 170.41(4) 2_755 . ?
O3 Na2 N1 86.09(4) . . ?
O6 Na2 N1 87.61(4) . . ?
O5 Na2 N1 99.41(4) . . ?
O4 Na2 Na2 95.38(4) . 2_755 ?
O6 Na2 Na2 42.85(3) 2_755 2_755 ?
O3 Na2 Na2 90.40(3) . 2_755 ?
O6 Na2 Na2 41.66(3) . 2_755 ?
O5 Na2 Na2 131.00(4) . 2_755 ?
N1 Na2 Na2 129.05(4) . 2_755 ?
Na2 O6 Na2 95.49(4) 2_755 . ?
N2 N3 C6 113.95(12) . . ?
N3 N2 C3 113.43(12) . . ?
C1 N1 C5 116.51(13) . . ?
C1 N1 Na2 118.75(9) . . ?
C5 N1 Na2 124.71(10) . . ?
C11 C6 C7 120.31(13) . . ?
C11 C6 N3 115.65(12) . . ?
C7 C6 N3 124.03(12) . . ?
C8 C7 C6 119.79(12) . . ?
C11 C10 C9 120.73(12) . . ?
C10 C9 C8 119.25(13) . . ?
C10 C9 C12 119.46(12) . . ?
C8 C9 C12 121.28(12) . . ?
C4 C3 C2 118.65(13) . . ?
C4 C3 N2 125.02(12) . . ?
C2 C3 N2 116.31(12) . . ?
O1 C12 O2 124.64(13) . . ?
O1 C12 C9 117.58(12) . . ?
O2 C12 C9 117.78(11) . . ?
C5 C4 C3 118.43(13) . . ?
C10 C11 C6 119.45(13) . . ?
C7 C8 C9 120.44(13) . . ?
C1 C2 C3 118.19(13) . . ?
N1 C1 C2 124.11(13) . . ?
N1 C5 C4 124.09(13) . . ?

_refine_diff_density_max         0.249
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.052


# start Validation Reply Form
_vrf_DIFF019_I                   
;
PROBLEM: _diffrn_standards_number is missing
RESPONSE: not applicable
;
_vrf_DIFF020_I                   
;
PROBLEM: _diffrn_standards_interval_count and
RESPONSE: not applicable
;
_vrf_DIFF022_I                   
;
PROBLEM: _diffrn_standards_decay_% is missing
RESPONSE: not applicable
;
# end Validation Reply Form

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

data_c_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1839931'
_audit_update_record             
;
2018-04-26 deposited with the CCDC.
2018-08-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
2,7,12-trimethoxy-3,8,13-tris(4,3?-pyridyl-azophenylcarboxy)-10,15-dihydro-5H-tribenzo[a,d,g]cyclononene 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H30 N9 O9'
_chemical_formula_weight         1020.93

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

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

_cell_length_a                   9.6864(5)
_cell_length_b                   29.786(2)
_cell_length_c                   34.468(4)
_cell_angle_alpha                71.898(8)
_cell_angle_beta                 88.532(6)
_cell_angle_gamma                89.954(5)
_cell_volume                     9448.9(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    4571
_cell_measurement_theta_min      1.5460
_cell_measurement_theta_max      20.1510

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2100
_exptl_absorpt_coefficient_mu    0.050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.28437
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
 CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.68890
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_monochromator  synchrotron
_diffrn_measurement_device_type  'CCD plate'
_diffrn_measurement_method       'ω and π scans'
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -145.00   25.00   1.0000    0.0964
omega____ theta____ kappa____ phi______ frames
    -       30.0000    0.0000    0.0000 170

#__ type_ start__ end____ width___ exp.time_
  2 omega -145.00   25.00   1.0000    0.0964
omega____ theta____ kappa____ phi______ frames
    -       30.0000    0.0000  120.0000 170

#__ type_ start__ end____ width___ exp.time_
  3 omega -145.00   25.00   1.0000    0.0964
omega____ theta____ kappa____ phi______ frames
    -       30.0000    0.0000  240.0000 170

#__ type_ start__ end____ width___ exp.time_
  4 phi      0.00  180.00   1.0000    0.0964
omega____ theta____ kappa____ phi______ frames
   0.0000    0.0000    0.0000     -     180
;
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            60957
_diffrn_reflns_av_R_equivalents  0.1479
_diffrn_reflns_av_sigmaI/netI    0.1639
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.53
_diffrn_reflns_theta_max         20.00
_reflns_number_total             19323
_reflns_number_gt                5761
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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. 
Crystals were of poor quality due to extensive disorder and solvent-accessible voids. Refined isotropically due to poor parameter:observed data ratio
One azo-phenyl group modelled across two position at 0.65:0.35 occupancies and one azo-pyridine
 modelled across two positions each at 0.5 occupancy. Half of the aromatic ring groups of the
 structure were refine with a rigid body constraint (AFIX 66) and some additional restraints were placed 
on azo N-N and C-N distances (DFIX). Two pyridyl groups were refined each with one group
 displacement parameter. 
;

_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)+(0.1000P)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         19323
_refine_ls_number_parameters     390
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.3324
_refine_ls_R_factor_gt           0.2253
_refine_ls_wR_factor_ref         0.4885
_refine_ls_wR_factor_gt          0.4559
_refine_ls_goodness_of_fit_ref   1.711
_refine_ls_restrained_S_all      1.717
_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
O1 O 0.6687(11) 0.1675(4) 0.7511(4) 0.151(4) Uiso 1 1 d . . .
O2 O 0.6754(11) 0.1381(4) 0.8313(3) 0.150(4) Uiso 1 1 d . . .
O3 O 0.5082(16) 0.0845(5) 0.8450(4) 0.215(6) Uiso 1 1 d . . .
O4 O 0.6075(8) 0.3068(3) 0.9291(2) 0.103(3) Uiso 1 1 d . . .
O5 O 0.5237(8) 0.3974(3) 0.8922(3) 0.113(3) Uiso 1 1 d . . .
O6 O 0.4129(9) 0.3770(3) 0.9549(3) 0.136(3) Uiso 1 1 d . . .
O7 O 0.5222(10) 0.4693(4) 0.7013(3) 0.138(3) Uiso 1 1 d . . .
O8 O 0.5769(9) 0.4053(3) 0.6572(3) 0.133(3) Uiso 1 1 d . . .
O9 O 0.4185(12) 0.4594(4) 0.6218(3) 0.172(4) Uiso 1 1 d . . .
O10 O 1.1094(8) 0.2438(3) 0.9305(2) 0.114(3) Uiso 1 1 d . . .
O11 O 1.0242(8) 0.1802(3) 0.8928(2) 0.106(3) Uiso 1 1 d . . .
O12 O 0.9130(9) 0.1571(3) 0.9556(3) 0.126(3) Uiso 1 1 d . . .
O13 O 1.0233(10) 0.2476(3) 0.7025(3) 0.147(4) Uiso 1 1 d . . .
O14 O 1.0827(10) 0.3379(4) 0.6627(3) 0.152(4) Uiso 1 1 d . . .
O15 O 0.9303(12) 0.3168(4) 0.6239(4) 0.196(5) Uiso 1 1 d . . .
O16 O 1.1716(9) 0.5103(3) 0.7540(3) 0.143(4) Uiso 1 1 d . . .
O17 O 1.1745(9) 0.4833(3) 0.8329(3) 0.135(3) Uiso 1 1 d . . .
O18 O 1.0078(14) 0.5322(5) 0.8401(4) 0.213(5) Uiso 1 1 d . . .
N1 N 1.000(3) -0.0610(8) 0.9178(7) 0.314(11) Uiso 1 1 d D . .
N2 N 1.122(3) -0.0350(11) 0.8953(10) 0.424(17) Uiso 1 1 d D . .
N4 N 0.8525(10) 0.5352(4) 0.9674(3) 0.110(4) Uiso 1 1 d . . .
N5 N 0.8362(10) 0.5400(4) 1.0013(4) 0.110(4) Uiso 1 1 d . . .
N6 N 1.1256(13) 0.6246(5) 0.9942(4) 0.165(5) Uiso 1 1 d . . .
N7 N 0.9025(18) 0.4587(7) 0.4893(6) 0.217(7) Uiso 1 1 d . . .
N8 N 0.8839(19) 0.4848(7) 0.4558(7) 0.232(8) Uiso 1 1 d . . .
N10 N 1.3464(13) -0.0131(5) 0.9610(5) 0.072(5) Uiso 0.65 1 d PD A 2
N11 N 1.3351(11) -0.0396(4) 0.9949(4) 0.041(3) Uiso 0.65 1 d PD A 2
N13 N 1.405(3) 0.3842(10) 0.4839(8) 0.356(13) Uiso 1 1 d D . .
N14 N 1.533(4) 0.3696(14) 0.5023(10) 0.482(10) Uiso 1 1 d D . .
N16 N 1.525(2) 0.6136(9) 0.9121(7) 0.305(11) Uiso 1 1 d D . .
N17 N 1.453(4) 0.6491(14) 0.9227(11) 0.252(17) Uiso 0.50 1 d PD B 2
C1 C 0.3904(14) 0.2418(5) 0.7742(5) 0.105(4) Uiso 1 1 d . . .
C2 C 0.4824(14) 0.2248(5) 0.7494(5) 0.122(5) Uiso 1 1 d . . .
H2 H 0.4856 0.2363 0.7204 0.147 Uiso 1 1 calc R . .
C3 C 0.5726(17) 0.1873(6) 0.7738(6) 0.139(6) Uiso 1 1 d . . .
C4 C 0.5764(15) 0.1722(5) 0.8103(6) 0.116(5) Uiso 1 1 d . . .
C5 C 0.4926(14) 0.1890(5) 0.8381(5) 0.121(5) Uiso 1 1 d . . .
H5 H 0.4978 0.1781 0.8670 0.145 Uiso 1 1 calc R . .
C6 C 0.3991(14) 0.2252(5) 0.8151(5) 0.115(5) Uiso 1 1 d . . .
C7 C 0.3044(12) 0.2439(4) 0.8448(4) 0.096(4) Uiso 1 1 d . . .
H7A H 0.2863 0.2172 0.8700 0.115 Uiso 1 1 calc R . .
H7B H 0.2147 0.2531 0.8317 0.115 Uiso 1 1 calc R . .
C8 C 0.3600(12) 0.2875(5) 0.8582(4) 0.092(4) Uiso 1 1 d . . .
C9 C 0.4538(12) 0.2755(5) 0.8885(4) 0.097(4) Uiso 1 1 d . . .
H9 H 0.4782 0.2434 0.9008 0.117 Uiso 1 1 calc R . .
C10 C 0.5116(13) 0.3099(5) 0.9007(4) 0.099(4) Uiso 1 1 d . . .
C11 C 0.4657(14) 0.3567(5) 0.8843(4) 0.110(4) Uiso 1 1 d . . .
C12 C 0.3705(13) 0.3679(5) 0.8531(4) 0.112(5) Uiso 1 1 d . . .
H12 H 0.3420 0.3997 0.8416 0.134 Uiso 1 1 calc R . .
C13 C 0.3161(13) 0.3329(5) 0.8382(4) 0.097(4) Uiso 1 1 d . . .
C14 C 0.2283(13) 0.3501(5) 0.8008(4) 0.118(5) Uiso 1 1 d . . .
H14A H 0.1614 0.3250 0.8008 0.141 Uiso 1 1 calc R . .
H14B H 0.1752 0.3780 0.8022 0.141 Uiso 1 1 calc R . .
C15 C 0.3145(13) 0.3631(5) 0.7616(4) 0.108(4) Uiso 1 1 d . . .
C16 C 0.3710(13) 0.4097(5) 0.7512(4) 0.118(5) Uiso 1 1 d . . .
H16 H 0.3487 0.4304 0.7665 0.142 Uiso 1 1 calc R . .
C17 C 0.4661(15) 0.4238(6) 0.7152(5) 0.120(5) Uiso 1 1 d . . .
C18 C 0.4882(15) 0.3939(6) 0.6939(5) 0.119(5) Uiso 1 1 d . . .
C19 C 0.4331(14) 0.3494(5) 0.7048(5) 0.130(5) Uiso 1 1 d . . .
H19 H 0.4522 0.3294 0.6886 0.156 Uiso 1 1 calc R . .
C20 C 0.3476(13) 0.3334(5) 0.7402(4) 0.097(4) Uiso 1 1 d . . .
C21 C 0.2973(14) 0.2811(5) 0.7506(4) 0.130(5) Uiso 1 1 d . . .
H21A H 0.2089 0.2781 0.7663 0.156 Uiso 1 1 calc R . .
H21B H 0.2767 0.2753 0.7246 0.156 Uiso 1 1 calc R . .
C22 C 0.6728(17) 0.1891(6) 0.7079(5) 0.174(7) Uiso 1 1 d . . .
H22A H 0.5941 0.1780 0.6960 0.262 Uiso 1 1 calc R . .
H22B H 0.7590 0.1807 0.6964 0.262 Uiso 1 1 calc R . .
H22C H 0.6683 0.2235 0.7016 0.262 Uiso 1 1 calc R . .
C23 C 0.625(2) 0.0967(8) 0.8499(6) 0.184(8) Uiso 1 1 d . . .
C24 C 0.7343(19) 0.0582(7) 0.8626(4) 0.223(9) Uiso 1 1 d G . .
C25 C 0.6924(15) 0.0112(9) 0.8776(6) 0.323(14) Uiso 1 1 d G . .
H25 H 0.5983 0.0030 0.8762 0.387 Uiso 1 1 calc R . .
C26 C 0.788(3) -0.0237(5) 0.8947(5) 0.41(2) Uiso 1 1 d G . .
H26 H 0.7593 -0.0558 0.9050 0.495 Uiso 1 1 calc R . .
C27 C 0.926(2) -0.0116(7) 0.8968(5) 0.254(11) Uiso 1 1 d GD . .
C28 C 0.9675(13) 0.0354(8) 0.8817(5) 0.263(11) Uiso 1 1 d G . .
H28 H 1.0616 0.0437 0.8831 0.316 Uiso 1 1 calc R . .
C29 C 0.872(2) 0.0703(5) 0.8646(4) 0.212(8) Uiso 1 1 d G . .
H29 H 0.9006 0.1024 0.8544 0.254 Uiso 1 1 calc R . .
C30 C 1.2333(12) -0.0795(2) 0.9114(4) 0.463(10) Uiso 1 1 d GD . .
C31 C 1.3533(12) -0.0701(3) 0.8872(4) 0.463(10) Uiso 1 1 d G . .
H31 H 1.3638 -0.0409 0.8659 0.556 Uiso 1 1 calc R . .
C32 C 1.4581(12) -0.1033(3) 0.8941(4) 0.463(10) Uiso 1 1 d G . .
H32 H 1.5402 -0.0969 0.8775 0.556 Uiso 1 1 calc R . .
C33 C 1.4428(13) -0.1460(3) 0.9251(4) 0.463(10) Uiso 1 1 d G . .
H33 H 1.5143 -0.1688 0.9299 0.556 Uiso 1 1 calc R . .
N3 N 1.3227(13) -0.1554(3) 0.9493(4) 0.463(10) Uiso 1 1 d G . .
C34 C 1.2179(13) -0.1222(2) 0.9424(4) 0.463(10) Uiso 1 1 d G . .
H34 H 1.1359 -0.1286 0.9590 0.556 Uiso 1 1 calc R . .
C35 C 0.6613(5) 0.25829(13) 0.94944(16) 0.122(5) Uiso 1 1 d G . .
H35A H 0.5877 0.2387 0.9665 0.183 Uiso 1 1 calc R . .
H35B H 0.7389 0.2602 0.9665 0.183 Uiso 1 1 calc R . .
H35C H 0.6925 0.2442 0.9286 0.183 Uiso 1 1 calc R . .
C36 C 0.5028(4) 0.39786(14) 0.92832(15) 0.102(4) Uiso 1 1 d G . .
C37 C 0.5816(4) 0.43645(13) 0.94369(13) 0.097(4) Uiso 1 1 d G . .
C38 C 0.5648(4) 0.44669(14) 0.97835(13) 0.103(4) Uiso 1 1 d G . .
H38 H 0.4912 0.4316 0.9965 0.123 Uiso 1 1 calc R . .
C39 C 0.6484(4) 0.47811(13) 0.98969(12) 0.129(5) Uiso 1 1 d G . .
H39 H 0.6369 0.4859 1.0143 0.155 Uiso 1 1 calc R . .
C40 C 0.7587(4) 0.49789(12) 0.95806(12) 0.101(4) Uiso 1 1 d G . .
C41 C 0.7796(4) 0.49141(12) 0.92333(11) 0.116(5) Uiso 1 1 d G . .
H41 H 0.8507 0.5086 0.9054 0.139 Uiso 1 1 calc R . .
C42 C 0.6942(4) 0.45767(13) 0.91116(12) 0.122(5) Uiso 1 1 d G . .
H42 H 0.7070 0.4500 0.8865 0.146 Uiso 1 1 calc R . .
C43 C 0.9337(4) 0.57393(13) 1.00935(14) 0.107(4) Uiso 1 1 d G . .
C44 C 0.9173(5) 0.58525(14) 1.04506(14) 0.115(5) Uiso 1 1 d G . .
H44 H 0.8411 0.5714 1.0626 0.138 Uiso 1 1 calc R . .
C45 C 0.9966(6) 0.61301(15) 1.05671(16) 0.081(4) Uiso 1 1 d G . .
H45 H 0.9791 0.6207 1.0811 0.098 Uiso 1 1 calc R . .
C46 C 1.1053(5) 0.63011(16) 1.03190(18) 0.113(5) Uiso 1 1 d G . .
H46 H 1.1731 0.6473 1.0410 0.136 Uiso 1 1 calc R . .
C47 C 1.0434(4) 0.58758(14) 0.98150(15) 0.153(6) Uiso 1 1 d G . .
H47 H 1.0636 0.5763 0.9591 0.184 Uiso 1 1 calc R . .
C48 C 0.5309(8) 0.4940(2) 0.73036(14) 0.200(8) Uiso 1 1 d G . .
H48A H 0.4381 0.5030 0.7370 0.299 Uiso 1 1 calc R . .
H48B H 0.5878 0.5225 0.7189 0.299 Uiso 1 1 calc R . .
H48C H 0.5729 0.4737 0.7552 0.299 Uiso 1 1 calc R . .
C49 C 0.5316(12) 0.4384(3) 0.62243(16) 0.163(7) Uiso 1 1 d G . .
C50 C 0.6283(11) 0.4465(4) 0.5893(3) 0.132(5) Uiso 1 1 d G . .
C51 C 0.6028(10) 0.4803(4) 0.5521(4) 0.144(6) Uiso 1 1 d G . .
H51 H 0.5239 0.4999 0.5494 0.173 Uiso 1 1 calc R . .
C52 C 0.6928(14) 0.4855(4) 0.5189(3) 0.169(7) Uiso 1 1 d G . .
H52 H 0.6753 0.5086 0.4935 0.203 Uiso 1 1 calc R . .
C53 C 0.8082(12) 0.4568(5) 0.5229(4) 0.206(8) Uiso 1 1 d G . .
C54 C 0.8337(10) 0.4230(4) 0.5601(5) 0.195(8) Uiso 1 1 d G . .
H54 H 0.9126 0.4034 0.5629 0.234 Uiso 1 1 calc R . .
C55 C 0.7438(14) 0.4178(3) 0.5933(3) 0.162(6) Uiso 1 1 d G . .
H55 H 0.7612 0.3947 0.6187 0.195 Uiso 1 1 calc R . .
C56 C 0.9809(8) 0.4846(2) 0.42034(8) 0.201(8) Uiso 1 1 d G . .
C57 C 0.9525(9) 0.5155(2) 0.38199(8) 0.211(8) Uiso 1 1 d G . .
H57 H 0.8730 0.5349 0.3784 0.253 Uiso 1 1 calc R . .
N9 N 1.0405(9) 0.5180(3) 0.34887(8) 0.229(7) Uiso 1 1 d G . .
C59 C 1.1568(9) 0.4896(3) 0.35411(9) 0.227(9) Uiso 1 1 d G . .
H59 H 1.2169 0.4913 0.3315 0.273 Uiso 1 1 calc R . .
C58 C 1.1852(8) 0.4587(3) 0.39247(9) 0.257(11) Uiso 1 1 d G . .
H58 H 1.2647 0.4393 0.3960 0.308 Uiso 1 1 calc R . .
C60 C 1.0973(8) 0.4562(2) 0.42558(9) 0.222(9) Uiso 1 1 d G . .
H60 H 1.1167 0.4351 0.4518 0.267 Uiso 1 1 calc R . .
C61 C 0.8543(3) 0.31669(12) 0.85693(9) 0.095(4) Uiso 1 1 d G . .
C62 C 0.9557(3) 0.30555(13) 0.88838(8) 0.099(4) Uiso 1 1 d G . .
C63 C 1.0168(4) 0.25704(13) 0.90157(9) 0.098(4) Uiso 1 1 d G . .
C64 C 0.9651(4) 0.22767(12) 0.88473(9) 0.100(4) Uiso 1 1 d G . .
C65 C 0.8711(4) 0.23431(11) 0.85280(9) 0.121(5) Uiso 1 1 d G . .
C66 C 0.8204(3) 0.28410(12) 0.84040(9) 0.099(4) Uiso 1 1 d G . .
C67 C 0.7230(3) 0.29411(13) 0.80133(9) 0.113(5) Uiso 1 1 d G . .
H67A H 0.6673 0.2657 0.8029 0.136 Uiso 1 1 calc R . .
H67B H 0.6596 0.3206 0.8001 0.136 Uiso 1 1 calc R . .
C68 C 0.8171(3) 0.30629(11) 0.76491(9) 0.117(5) Uiso 1 1 d G . .
C69 C 0.8726(4) 0.27131(11) 0.75041(9) 0.122(5) Uiso 1 1 d G . .
C70 C 0.9645(4) 0.28450(11) 0.71591(9) 0.141(6) Uiso 1 1 d G . .
C71 C 0.9935(4) 0.32727(12) 0.69430(9) 0.143(6) Uiso 1 1 d G . .
C72 C 0.9387(3) 0.36307(11) 0.70500(8) 0.115(5) Uiso 1 1 d G . .
C73 C 0.8475(3) 0.35441(11) 0.74168(9) 0.099(4) Uiso 1 1 d G . .
C74 C 0.7919(3) 0.39897(12) 0.75137(9) 0.135(5) Uiso 1 1 d G . .
H74A H 0.7007 0.3914 0.7656 0.162 Uiso 1 1 calc R . .
H74B H 0.7785 0.4245 0.7254 0.162 Uiso 1 1 calc R . .
C75 C 0.8905(4) 0.41719(11) 0.77847(9) 0.110(4) Uiso 1 1 d G . .
C76 C 0.9838(4) 0.45483(10) 0.75049(10) 0.110(4) Uiso 1 1 d G . .
C77 C 1.0761(5) 0.47359(12) 0.77520(10) 0.117(5) Uiso 1 1 d G . .
C78 C 1.0748(5) 0.45922(12) 0.81447(10) 0.118(5) Uiso 1 1 d G . .
C79 C 0.9888(5) 0.42629(12) 0.83973(10) 0.107(4) Uiso 1 1 d G . .
C80 C 0.9015(4) 0.40533(11) 0.81887(9) 0.118(5) Uiso 1 1 d G . .
C81 C 0.7981(3) 0.36770(13) 0.84843(9) 0.104(4) Uiso 1 1 d G . .
H81A H 0.7860 0.3748 0.8745 0.125 Uiso 1 1 calc R . .
H81B H 0.7068 0.3700 0.8357 0.125 Uiso 1 1 calc R . .
C82 C 1.1601(4) 0.27754(17) 0.94788(9) 0.126(5) Uiso 1 1 d G . .
H82A H 1.1959 0.3051 0.9262 0.188 Uiso 1 1 calc R . .
H82B H 1.2344 0.2635 0.9665 0.188 Uiso 1 1 calc R . .
H82C H 1.0852 0.2873 0.9631 0.188 Uiso 1 1 calc R . .
C83 C 0.9973(6) 0.15234(13) 0.92867(11) 0.132(5) Uiso 1 1 d G . .
C84 C 1.0844(12) 0.1070(4) 0.9340(5) 0.080(7) Uiso 0.65 1 d PG A 2
C85 C 1.1906(14) 0.1045(4) 0.9069(4) 0.096(7) Uiso 0.65 1 d PG A 2
H85 H 1.2039 0.1293 0.8820 0.115 Uiso 0.65 1 calc PR A 2
C86 C 1.2773(12) 0.0656(5) 0.9163(4) 0.104(8) Uiso 0.65 1 d PG A 2
H86 H 1.3499 0.0638 0.8978 0.125 Uiso 0.65 1 calc PR A 2
C87 C 1.2579(12) 0.0293(4) 0.9529(5) 0.064(5) Uiso 0.65 1 d PGD A 2
C88 C 1.1517(14) 0.0318(4) 0.9800(3) 0.113(8) Uiso 0.65 1 d PG A 2
H88 H 1.1384 0.0070 1.0049 0.136 Uiso 0.65 1 calc PR A 2
C89 C 1.0649(11) 0.0707(5) 0.9706(4) 0.082(6) Uiso 0.65 1 d PG A 2
H89 H 0.9924 0.0725 0.9891 0.099 Uiso 0.65 1 calc PR A 2
C90 C 1.4330(6) -0.07961(19) 1.00985(15) 0.108(4) Uiso 1 1 d GD . .
C91 C 1.4107(7) -0.1159(2) 1.04623(15) 0.121(5) Uiso 1 1 d G A .
H91 H 1.3352 -0.1144 1.0639 0.145 Uiso 1 1 calc R . .
N12 N 1.4988(7) -0.15443(19) 1.05673(16) 0.131(4) Uiso 1 1 d G A .
C93 C 1.6093(7) -0.1566(2) 1.03086(17) 0.116(5) Uiso 1 1 d G A .
H93 H 1.6695 -0.1830 1.0380 0.139 Uiso 1 1 calc R . .
C92 C 1.6316(6) -0.1203(2) 0.99448(17) 0.151(6) Uiso 1 1 d G A .
H92 H 1.7071 -0.1218 0.9768 0.181 Uiso 1 1 calc R . .
C94 C 1.5435(6) -0.08182(18) 0.98398(16) 0.151(6) Uiso 1 1 d G A .
H94 H 1.5587 -0.0570 0.9591 0.181 Uiso 1 1 calc R . .
C95 C 1.0319(6) 0.2018(3) 0.7328(2) 0.186(7) Uiso 1 1 d G A .
H95A H 1.0903 0.2039 0.7550 0.278 Uiso 1 1 calc R . .
H95B H 1.0721 0.1792 0.7203 0.278 Uiso 1 1 calc R . .
H95C H 0.9392 0.1910 0.7438 0.278 Uiso 1 1 calc R . .
C96 C 1.0590(8) 0.3410(2) 0.6267(2) 0.169(7) Uiso 1 1 d G A .
C97 C 1.1322(8) 0.3451(2) 0.5902(2) 0.174(7) Uiso 1 1 d G A .
C98 C 1.2520(9) 0.3688(2) 0.5943(2) 0.190(8) Uiso 1 1 d G A .
H98 H 1.2686 0.3750 0.6192 0.228 Uiso 1 1 calc R . .
C99 C 1.3474(9) 0.3833(3) 0.5620(2) 0.223(9) Uiso 1 1 d G A .
H99 H 1.4292 0.3995 0.5648 0.267 Uiso 1 1 calc R . .
C100 C 1.3230(10) 0.3743(3) 0.5255(2) 0.244(10) Uiso 1 1 d GD A .
C101 C 1.2033(11) 0.3506(3) 0.5214(2) 0.262(11) Uiso 1 1 d G A .
H101 H 1.1866 0.3444 0.4965 0.314 Uiso 1 1 calc R . .
C102 C 1.1079(10) 0.3361(2) 0.5538(2) 0.232(9) Uiso 1 1 d G A .
H102 H 1.0261 0.3199 0.5510 0.278 Uiso 1 1 calc R . .
C103 C 1.6511(16) 0.3753(5) 0.4672(4) 0.482(10) Uiso 1 1 d GD . .
C104 C 1.6109(17) 0.4024(5) 0.4286(4) 0.482(10) Uiso 1 1 d G . .
H104 H 1.5213 0.4158 0.4250 0.579 Uiso 1 1 calc R . .
C105 C 1.7019(18) 0.4099(6) 0.3953(4) 0.482(10) Uiso 1 1 d G . .
H105 H 1.6744 0.4284 0.3689 0.579 Uiso 1 1 calc R . .
C106 C 1.8330(18) 0.3903(6) 0.4006(4) 0.482(10) Uiso 1 1 d G . .
H106 H 1.8952 0.3954 0.3779 0.579 Uiso 1 1 calc R . .
N15 N 1.8732(17) 0.3632(6) 0.4392(4) 0.482(10) Uiso 1 1 d G . .
C107 C 1.7822(16) 0.3557(5) 0.4725(4) 0.482(10) Uiso 1 1 d G . .
H107 H 1.8097 0.3372 0.4989 0.579 Uiso 1 1 calc R . .
C108 C 1.1690(8) 0.5239(4) 0.7116(3) 0.155(6) Uiso 1 1 d G . .
H10A H 1.2246 0.5020 0.7017 0.232 Uiso 1 1 calc R . .
H10B H 1.2069 0.5559 0.7002 0.232 Uiso 1 1 calc R . .
H10C H 1.0735 0.5233 0.7030 0.232 Uiso 1 1 calc R . .
C109 C 1.1203(10) 0.5116(3) 0.8535(2) 0.212(9) Uiso 1 1 d G . .
C110 C 1.2300(9) 0.5412(3) 0.8613(2) 0.212(8) Uiso 1 1 d G . .
C111 C 1.1870(10) 0.5756(3) 0.8783(2) 0.270(11) Uiso 1 1 d G B .
H111 H 1.0926 0.5845 0.8774 0.324 Uiso 1 1 calc R . .
C112 C 1.2820(11) 0.5971(3) 0.8966(2) 0.315(14) Uiso 1 1 d G . .
H112 H 1.2526 0.6206 0.9082 0.379 Uiso 1 1 calc R B .
C113 C 1.4200(10) 0.5840(4) 0.8978(2) 0.195(8) Uiso 1 1 d GD B .
C114 C 1.4631(10) 0.5496(4) 0.8808(2) 0.261(11) Uiso 1 1 d G . .
H114 H 1.5574 0.5406 0.8817 0.313 Uiso 1 1 calc R B .
C115 C 1.3680(9) 0.5281(3) 0.86252(19) 0.206(8) Uiso 1 1 d G B .
H115 H 1.3975 0.5046 0.8509 0.247 Uiso 1 1 calc R . .
C116 C 1.5528(19) 0.6724(4) 0.9401(5) 0.220(18) Uiso 0.50 1 d PGD B 2
C117 C 1.696(2) 0.6685(4) 0.9419(5) 0.27(3) Uiso 0.50 1 d PG B 2
H117 H 1.7406 0.6432 0.9356 0.323 Uiso 0.50 1 calc PR B 2
C118 C 1.773(2) 0.7017(5) 0.9530(7) 0.37(4) Uiso 0.50 1 d PG B 2
H118 H 1.8703 0.6991 0.9543 0.447 Uiso 0.50 1 calc PR B 2
C119 C 1.707(3) 0.7388(4) 0.9622(5) 0.31(3) Uiso 0.50 1 d PG B 2
H119 H 1.7595 0.7615 0.9698 0.372 Uiso 0.50 1 calc PR B 2
N18 N 1.564(3) 0.7426(4) 0.9604(5) 0.222(14) Uiso 0.50 1 d PG B 2
C120 C 1.487(2) 0.7094(4) 0.9493(6) 0.26(2) Uiso 0.50 1 d PG B 2
H120 H 1.3893 0.7120 0.9480 0.315 Uiso 0.50 1 calc PR B 2
N10B N 1.3669(15) -0.0032(4) 0.9775(6) 0.027(6) Uiso 0.35 1 d PGD A 1
N11B N 1.3328(18) -0.0348(4) 1.0164(6) 0.071(9) Uiso 0.35 1 d PGD A 1
N17B N 1.650(2) 0.6048(4) 0.8928(4) 0.192(12) Uiso 0.50 1 d PGD B 1
C16B C 1.747(3) 0.6424(8) 0.9047(9) 0.201(16) Uiso 0.50 1 d PGD B 1
C17B C 1.864(3) 0.6538(9) 0.8792(7) 0.234(19) Uiso 0.50 1 d PG B 1
H17B H 1.8711 0.6438 0.8556 0.281 Uiso 0.50 1 calc PR B 1
C18B C 1.971(2) 0.6799(9) 0.8882(8) 0.157(12) Uiso 0.50 1 d PG B 1
H18B H 2.0506 0.6877 0.8708 0.189 Uiso 0.50 1 calc PR B 1
C19B C 1.961(2) 0.6945(8) 0.9227(9) 0.194(15) Uiso 0.50 1 d PG B 1
H19B H 2.0334 0.7123 0.9289 0.232 Uiso 0.50 1 calc PR B 1
N18B N 1.844(3) 0.6831(10) 0.9482(6) 0.270(19) Uiso 0.50 1 d PG B 1
C20B C 1.737(2) 0.6571(10) 0.9392(8) 0.161(17) Uiso 0.50 1 d PG B 1
H20B H 1.6574 0.6493 0.9567 0.193 Uiso 0.50 1 calc PR B 1
C84B C 1.0908(16) 0.1078(5) 0.9529(6) 0.028(7) Uiso 0.35 1 d PG A 1
C85B C 1.1961(18) 0.1037(5) 0.9261(5) 0.065(10) Uiso 0.35 1 d PG A 1
H85B H 1.2118 0.1282 0.9011 0.078 Uiso 0.35 1 calc PR A 1
C86B C 1.2784(15) 0.0637(6) 0.9359(5) 0.015(6) Uiso 0.35 1 d PG A 1
H86B H 1.3504 0.0609 0.9176 0.018 Uiso 0.35 1 calc PR A 1
C87B C 1.2555(16) 0.0278(5) 0.9725(6) 0.047(9) Uiso 0.35 1 d PGD A 1
C88B C 1.1501(18) 0.0319(5) 0.9993(5) 0.028(7) Uiso 0.35 1 d PG A 1
H88B H 1.1344 0.0074 1.0243 0.034 Uiso 0.35 1 calc PR A 1
C89B C 1.0678(16) 0.0719(6) 0.9895(6) 0.064(10) Uiso 0.35 1 d PG A 1
H89B H 0.9958 0.0747 1.0079 0.076 Uiso 0.35 1 calc PR A 1

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C3 1.440(17) . ?
O1 C22 1.427(15) . ?
O2 C23 1.29(2) . ?
O2 C4 1.433(15) . ?
O3 C23 1.22(2) . ?
O4 C10 1.349(13) . ?
O4 C35 1.496(9) . ?
O5 C36 1.261(9) . ?
O5 C11 1.439(14) . ?
O6 C36 1.261(9) . ?
O7 C17 1.394(15) . ?
O7 C48 1.420(11) . ?
O8 C49 1.375(10) . ?
O8 C18 1.461(15) . ?
O9 C49 1.257(14) . ?
O10 C63 1.324(8) . ?
O10 C82 1.414(9) . ?
O11 C83 1.277(8) . ?
O11 C64 1.473(9) . ?
O12 C83 1.262(10) . ?
O13 C70 1.433(11) . ?
O13 C95 1.442(10) . ?
O14 C96 1.244(12) . ?
O14 C71 1.330(10) . ?
O15 C96 1.461(13) . ?
O16 C108 1.391(11) . ?
O16 C77 1.434(9) . ?
O17 C109 1.355(13) . ?
O17 C78 1.472(9) . ?
O18 C109 1.275(16) . ?
N1 N2 1.48(3) . ?
N1 C27 1.61(2) . ?
N2 C30 1.67(3) . ?
N4 N5 1.228(12) . ?
N4 C40 1.550(11) . ?
N5 C43 1.475(10) . ?
N6 C46 1.367(14) . ?
N6 C47 1.538(13) . ?
N7 N8 1.19(2) . ?
N7 C53 1.445(19) . ?
N8 C56 1.52(2) . ?
N10 N11 1.192(13) . ?
N10 C87 1.481(16) . ?
N11 C90 1.492(12) . ?
N13 N14 1.42(3) . ?
N13 C100 1.57(2) . ?
N14 C103 1.61(3) . ?
N16 N17 1.40(3) . ?
N16 N17B 1.43(3) . ?
N16 C113 1.53(2) . ?
N17 C116 1.44(3) . ?
C1 C6 1.345(16) . ?
C1 C2 1.418(17) . ?
C1 C21 1.513(16) . ?
C2 C3 1.473(18) . ?
C2 H2 0.9500 . ?
C3 C4 1.200(17) . ?
C4 C5 1.442(17) . ?
C5 C6 1.454(17) . ?
C5 H5 0.9500 . ?
C6 C7 1.585(16) . ?
C7 C8 1.603(15) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.364(14) . ?
C8 C13 1.386(15) . ?
C9 C10 1.351(14) . ?
C9 H9 0.9500 . ?
C10 C11 1.408(16) . ?
C11 C12 1.396(15) . ?
C12 C13 1.402(15) . ?
C12 H12 0.9500 . ?
C13 C14 1.513(15) . ?
C14 C15 1.515(16) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C20 1.350(16) . ?
C15 C16 1.428(15) . ?
C16 C17 1.478(17) . ?
C16 H16 0.9500 . ?
C17 C18 1.334(17) . ?
C18 C19 1.364(16) . ?
C19 C20 1.412(16) . ?
C19 H19 0.9500 . ?
C20 C21 1.561(16) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.53(2) . ?
C24 C25 1.3900 . ?
C24 C29 1.3900 . ?
C25 C26 1.3900 . ?
C25 H25 0.9500 . ?
C26 C27 1.3900 . ?
C26 H26 0.9500 . ?
C27 C28 1.3900 . ?
C28 C29 1.3900 . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C31 1.3900 . ?
C30 C34 1.3900 . ?
C31 C32 1.3900 . ?
C31 H31 0.9500 . ?
C32 C33 1.3900 . ?
C32 H32 0.9500 . ?
C33 N3 1.3900 . ?
C33 H33 0.9500 . ?
N3 C34 1.3900 . ?
C34 H34 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.6079 . ?
C37 C38 1.3280 . ?
C37 C42 1.5311 . ?
C38 C39 1.3889 . ?
C38 H38 0.9500 . ?
C39 C40 1.4897 . ?
C39 H39 0.9500 . ?
C40 C41 1.2814 . ?
C41 C42 1.4665 . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C44 1.3789 . ?
C43 C47 1.3864 . ?
C44 C45 1.2877 . ?
C44 H44 0.9500 . ?
C45 C46 1.3352 . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.418(12) . ?
C50 C51 1.3900 . ?
C50 C55 1.3900 . ?
C51 C52 1.3900 . ?
C51 H51 0.9500 . ?
C52 C53 1.3900 . ?
C52 H52 0.9500 . ?
C53 C54 1.3900 . ?
C54 C55 1.3900 . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 C57 1.3900 . ?
C56 C60 1.3900 . ?
C57 N9 1.3900 . ?
C57 H57 0.9500 . ?
N9 C59 1.3900 . ?
C59 C58 1.3900 . ?
C59 H59 0.9500 . ?
C58 C60 1.3900 . ?
C58 H58 0.9500 . ?
C60 H60 0.9500 . ?
C61 C66 1.3146 . ?
C61 C62 1.4423 . ?
C61 C81 1.5559 . ?
C62 C63 1.4997 . ?
C63 C64 1.2977 . ?
C64 C65 1.4124 . ?
C65 C66 1.4964 . ?
C66 C67 1.6152 . ?
C67 C68 1.4825 . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C68 C69 1.3903 . ?
C68 C73 1.4343 . ?
C69 C70 1.4204 . ?
C70 C71 1.2871 . ?
C71 C72 1.3375 . ?
C72 C73 1.4781 . ?
C73 C74 1.5584 . ?
C74 C75 1.5621 . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C75 C80 1.3330 . ?
C75 C76 1.5130 . ?
C76 C77 1.4737 . ?
C77 C78 1.2863 . ?
C78 C79 1.3594 . ?
C79 C80 1.3901 . ?
C80 C81 1.5928 . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 C84 1.555(11) . ?
C83 C84B 1.621(14) . ?
C84 C85 1.3900 . ?
C84 C89 1.3900 . ?
C85 C86 1.3900 . ?
C85 H85 0.9500 . ?
C86 C87 1.3900 . ?
C86 H86 0.9500 . ?
C87 C88 1.3900 . ?
C88 C89 1.3900 . ?
C88 H88 0.9500 . ?
C89 H89 0.9500 . ?
C90 C91 1.3900 . ?
C90 C94 1.3900 . ?
C90 N11B 1.716(16) . ?
C91 N12 1.3900 . ?
C91 H91 0.9500 . ?
N12 C93 1.3900 . ?
C93 C92 1.3900 . ?
C93 H93 0.9500 . ?
C92 C94 1.3900 . ?
C92 H92 0.9500 . ?
C94 H94 0.9500 . ?
C95 H95A 0.9800 . ?
C95 H95B 0.9800 . ?
C95 H95C 0.9800 . ?
C96 C97 1.3996 . ?
C97 C98 1.3900 . ?
C97 C102 1.3907 . ?
C98 C99 1.3902 . ?
C98 H98 0.9500 . ?
C99 C100 1.3902 . ?
C99 H99 0.9500 . ?
C100 C101 1.3902 . ?
C101 C102 1.3899 . ?
C101 H101 0.9500 . ?
C102 H102 0.9500 . ?
C103 C104 1.3900 . ?
C103 C107 1.3900 . ?
C104 C105 1.3900 . ?
C104 H104 0.9500 . ?
C105 C106 1.3900 . ?
C105 H105 0.9500 . ?
C106 N15 1.3900 . ?
C106 H106 0.9500 . ?
N15 C107 1.3900 . ?
C107 H107 0.9500 . ?
C108 H10A 0.9800 . ?
C108 H10B 0.9800 . ?
C108 H10C 0.9800 . ?
C109 C110 1.4634 . ?
C110 C111 1.3896 . ?
C110 C115 1.3901 . ?
C111 C112 1.3904 . ?
C111 H111 0.9500 . ?
C112 C113 1.3899 . ?
C112 H112 0.9500 . ?
C113 C114 1.3900 . ?
C114 C115 1.3903 . ?
C114 H114 0.9500 . ?
C115 H115 0.9500 . ?
C116 C117 1.3900 . ?
C116 C120 1.3900 . ?
C117 C118 1.3900 . ?
C117 H117 0.9500 . ?
C118 C119 1.3900 . ?
C118 H118 0.9500 . ?
C119 N18 1.3900 . ?
C119 H119 0.9500 . ?
N18 C120 1.3900 . ?
C120 H120 0.9500 . ?
N10B N11B 1.4103 . ?
N10B C87B 1.399(19) . ?
N17B C16B 1.62(2) . ?
C16B C17B 1.3900 . ?
C16B C20B 1.3900 . ?
C17B C18B 1.3900 . ?
C17B H17B 0.9500 . ?
C18B C19B 1.3900 . ?
C18B H18B 0.9500 . ?
C19B N18B 1.3900 . ?
C19B H19B 0.9500 . ?
N18B C20B 1.3900 . ?
C20B H20B 0.9500 . ?
C84B C85B 1.3900 . ?
C84B C89B 1.3900 . ?
C85B C86B 1.3900 . ?
C85B H85B 0.9500 . ?
C86B C87B 1.3900 . ?
C86B H86B 0.9500 . ?
C87B C88B 1.3900 . ?
C88B C89B 1.3900 . ?
C88B H88B 0.9500 . ?
C89B H89B 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 O1 C22 116.1(14) . . ?
C23 O2 C4 115.0(15) . . ?
C10 O4 C35 115.6(9) . . ?
C36 O5 C11 113.6(8) . . ?
C17 O7 C48 116.7(10) . . ?
C49 O8 C18 118.1(10) . . ?
C63 O10 C82 119.0(7) . . ?
C83 O11 C64 114.1(7) . . ?
C70 O13 C95 116.3(8) . . ?
C96 O14 C71 127.5(9) . . ?
C108 O16 C77 115.7(8) . . ?
C109 O17 C78 116.2(8) . . ?
N2 N1 C27 82.4(18) . . ?
N1 N2 C30 96(2) . . ?
N5 N4 C40 116.2(9) . . ?
N4 N5 C43 113.6(9) . . ?
C46 N6 C47 121.1(9) . . ?
N8 N7 C53 121(2) . . ?
N7 N8 C56 120(2) . . ?
N11 N10 C87 114.4(14) . . ?
N10 N11 C90 120.7(12) . . ?
N14 N13 C100 94(2) . . ?
N13 N14 C103 109(3) . . ?
N17 N16 N17B 143(3) . . ?
N17 N16 C113 108(2) . . ?
N17B N16 C113 101.6(19) . . ?
N16 N17 C116 106(3) . . ?
C6 C1 C2 119.5(15) . . ?
C6 C1 C21 126.0(16) . . ?
C2 C1 C21 114.3(14) . . ?
C1 C2 C3 112.2(15) . . ?
C1 C2 H2 123.9 . . ?
C3 C2 H2 123.9 . . ?
C4 C3 O1 116.8(19) . . ?
C4 C3 C2 127(2) . . ?
O1 C3 C2 116.0(17) . . ?
C3 C4 C5 125(2) . . ?
C3 C4 O2 122.9(19) . . ?
C5 C4 O2 112.1(15) . . ?
C4 C5 C6 109.7(15) . . ?
C4 C5 H5 125.2 . . ?
C6 C5 H5 125.2 . . ?
C1 C6 C5 126.6(16) . . ?
C1 C6 C7 122.6(14) . . ?
C5 C6 C7 110.8(14) . . ?
C6 C7 C8 118.1(9) . . ?
C6 C7 H7A 107.8 . . ?
C8 C7 H7A 107.8 . . ?
C6 C7 H7B 107.8 . . ?
C8 C7 H7B 107.8 . . ?
H7A C7 H7B 107.1 . . ?
C9 C8 C13 125.5(13) . . ?
C9 C8 C7 114.3(12) . . ?
C13 C8 C7 120.1(12) . . ?
C8 C9 C10 119.0(13) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
O4 C10 C9 129.6(13) . . ?
O4 C10 C11 111.0(13) . . ?
C9 C10 C11 119.3(14) . . ?
C12 C11 C10 119.9(14) . . ?
C12 C11 O5 113.7(13) . . ?
C10 C11 O5 125.6(13) . . ?
C11 C12 C13 121.2(14) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C8 C13 C12 114.6(13) . . ?
C8 C13 C14 128.8(13) . . ?
C12 C13 C14 116.3(13) . . ?
C15 C14 C13 112.1(11) . . ?
C15 C14 H14A 109.2 . . ?
C13 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C20 C15 C16 122.1(14) . . ?
C20 C15 C14 125.1(13) . . ?
C16 C15 C14 112.5(13) . . ?
C15 C16 C17 116.0(14) . . ?
C15 C16 H16 122.0 . . ?
C17 C16 H16 122.0 . . ?
C18 C17 O7 119.9(15) . . ?
C18 C17 C16 119.1(15) . . ?
O7 C17 C16 120.7(15) . . ?
C17 C18 C19 123.4(17) . . ?
C17 C18 O8 123.0(15) . . ?
C19 C18 O8 113.5(15) . . ?
C18 C19 C20 119.6(16) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C15 C20 C19 119.6(14) . . ?
C15 C20 C21 125.6(13) . . ?
C19 C20 C21 114.7(13) . . ?
C1 C21 C20 119.1(11) . . ?
C1 C21 H21A 107.5 . . ?
C20 C21 H21A 107.5 . . ?
C1 C21 H21B 107.5 . . ?
C20 C21 H21B 107.5 . . ?
H21A C21 H21B 107.0 . . ?
O1 C22 H22A 109.5 . . ?
O1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O3 C23 O2 123(2) . . ?
O3 C23 C24 117(2) . . ?
O2 C23 C24 114(2) . . ?
C25 C24 C29 120.0 . . ?
C25 C24 C23 119(2) . . ?
C29 C24 C23 120(2) . . ?
C26 C25 C24 120.0 . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 120.0 . . ?
C26 C27 N1 105(2) . . ?
C28 C27 N1 135(2) . . ?
C27 C28 C29 120.0 . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C28 C29 C24 120.0 . . ?
C28 C29 H29 120.0 . . ?
C24 C29 H29 120.0 . . ?
C31 C30 C34 120.0 . . ?
C31 C30 N2 110.1(12) . . ?
C34 C30 N2 129.8(12) . . ?
C32 C31 C30 120.0 . . ?
C32 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
C33 C32 C31 120.0 . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C33 N3 120.0 . . ?
C32 C33 H33 120.0 . . ?
N3 C33 H33 120.0 . . ?
C33 N3 C34 120.0 . . ?
N3 C34 C30 120.0 . . ?
N3 C34 H34 120.0 . . ?
C30 C34 H34 120.0 . . ?
O4 C35 H35A 109.5 . . ?
O4 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O4 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O5 C36 O6 130.8(6) . . ?
O5 C36 C37 119.2(4) . . ?
O6 C36 C37 109.2(5) . . ?
C38 C37 C42 124.7 . . ?
C38 C37 C36 129.5 . . ?
C42 C37 C36 105.6 . . ?
C37 C38 C39 123.9 . . ?
C37 C38 H38 118.1 . . ?
C39 C38 H38 118.1 . . ?
C38 C39 C40 110.8 . . ?
C38 C39 H39 124.6 . . ?
C40 C39 H39 124.6 . . ?
C41 C40 C39 129.5 . . ?
C41 C40 N4 116.2(5) . . ?
C39 C40 N4 114.0(5) . . ?
C40 C41 C42 120.4 . . ?
C40 C41 H41 119.8 . . ?
C42 C41 H41 119.8 . . ?
C41 C42 C37 110.5 . . ?
C41 C42 H42 124.7 . . ?
C37 C42 H42 124.7 . . ?
C44 C43 C47 125.9 . . ?
C44 C43 N5 118.6(5) . . ?
C47 C43 N5 115.1(5) . . ?
C45 C44 C43 125.6 . . ?
C45 C44 H44 117.2 . . ?
C43 C44 H44 117.2 . . ?
C44 C45 C46 114.9 . . ?
C44 C45 H45 122.5 . . ?
C46 C45 H45 122.5 . . ?
C45 C46 N6 124.4(6) . . ?
C45 C46 H46 117.8 . . ?
N6 C46 H46 117.8 . . ?
C43 C47 N6 106.2(5) . . ?
C43 C47 H47 126.9 . . ?
N6 C47 H47 126.9 . . ?
O7 C48 H48A 109.5 . . ?
O7 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
O7 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O9 C49 O8 122.0(10) . . ?
O9 C49 C50 125.7(9) . . ?
O8 C49 C50 112.2(11) . . ?
C51 C50 C55 120.0 . . ?
C51 C50 C49 120.4(11) . . ?
C55 C50 C49 119.4(11) . . ?
C52 C51 C50 120.0 . . ?
C52 C51 H51 120.0 . . ?
C50 C51 H51 120.0 . . ?
C51 C52 C53 120.0 . . ?
C51 C52 H52 120.0 . . ?
C53 C52 H52 120.0 . . ?
C52 C53 C54 120.0 . . ?
C52 C53 N7 123.0(14) . . ?
C54 C53 N7 117.0(14) . . ?
C55 C54 C53 120.0 . . ?
C55 C54 H54 120.0 . . ?
C53 C54 H54 120.0 . . ?
C54 C55 C50 120.0 . . ?
C54 C55 H55 120.0 . . ?
C50 C55 H55 120.0 . . ?
C57 C56 C60 120.0 . . ?
C57 C56 N8 117.6(8) . . ?
C60 C56 N8 122.3(8) . . ?
N9 C57 C56 120.0 . . ?
N9 C57 H57 120.0 . . ?
C56 C57 H57 120.0 . . ?
C57 N9 C59 120.0 . . ?
N9 C59 C58 120.0 . . ?
N9 C59 H59 120.0 . . ?
C58 C59 H59 120.0 . . ?
C60 C58 C59 120.0 . . ?
C60 C58 H58 120.0 . . ?
C59 C58 H58 120.0 . . ?
C58 C60 C56 120.0 . . ?
C58 C60 H60 120.0 . . ?
C56 C60 H60 120.0 . . ?
C66 C61 C62 118.7 . . ?
C66 C61 C81 129.4 . . ?
C62 C61 C81 111.9 . . ?
C61 C62 C63 118.9 . . ?
C64 C63 O10 122.0(4) . . ?
C64 C63 C62 115.1 . . ?
O10 C63 C62 122.7(4) . . ?
C63 C64 C65 131.5 . . ?
C63 C64 O11 120.0(4) . . ?
C65 C64 O11 107.6(4) . . ?
C64 C65 C66 109.3 . . ?
C61 C66 C65 126.1 . . ?
C61 C66 C67 123.3 . . ?
C65 C66 C67 110.5 . . ?
C68 C67 C66 106.2 . . ?
C68 C67 H67A 110.5 . . ?
C66 C67 H67A 110.5 . . ?
C68 C67 H67B 110.5 . . ?
C66 C67 H67B 110.5 . . ?
H67A C67 H67B 108.7 . . ?
C69 C68 C73 117.2 . . ?
C69 C68 C67 120.9 . . ?
C73 C68 C67 121.7 . . ?
C68 C69 C70 119.0 . . ?
C71 C70 C69 125.1 . . ?
C71 C70 O13 117.1(4) . . ?
C69 C70 O13 117.7(4) . . ?
C70 C71 C72 119.4 . . ?
C70 C71 O14 122.8(5) . . ?
C72 C71 O14 117.6(5) . . ?
C71 C72 C73 121.2 . . ?
C68 C73 C72 117.8 . . ?
C68 C73 C74 125.8 . . ?
C72 C73 C74 116.4 . . ?
C73 C74 C75 113.1 . . ?
C73 C74 H74A 109.0 . . ?
C75 C74 H74A 109.0 . . ?
C73 C74 H74B 109.0 . . ?
C75 C74 H74B 109.0 . . ?
H74A C74 H74B 107.8 . . ?
C80 C75 C76 120.5 . . ?
C80 C75 C74 131.5 . . ?
C76 C75 C74 108.1 . . ?
C77 C76 C75 109.4 . . ?
C78 C77 O16 118.5(4) . . ?
C78 C77 C76 123.8 . . ?
O16 C77 C76 117.7(4) . . ?
C77 C78 C79 127.0 . . ?
C77 C78 O17 114.7(4) . . ?
C79 C78 O17 118.2(4) . . ?
C78 C79 C80 113.0 . . ?
C75 C80 C79 126.2 . . ?
C75 C80 C81 120.5 . . ?
C79 C80 C81 113.0 . . ?
C61 C81 C80 110.8 . . ?
C61 C81 H81A 109.5 . . ?
C80 C81 H81A 109.5 . . ?
C61 C81 H81B 109.5 . . ?
C80 C81 H81B 109.5 . . ?
H81A C81 H81B 108.1 . . ?
O10 C82 H82A 109.5 . . ?
O10 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
O10 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
O11 C83 O12 129.7(7) . . ?
O11 C83 C84 107.2(8) . . ?
O12 C83 C84 123.1(7) . . ?
O11 C83 C84B 125.3(9) . . ?
O12 C83 C84B 103.9(8) . . ?
C84 C83 C84B 24.0(9) . . ?
C85 C84 C89 120.0 . . ?
C85 C84 C83 122.7(10) . . ?
C89 C84 C83 116.7(10) . . ?
C84 C85 C86 120.0 . . ?
C84 C85 H85 120.0 . . ?
C86 C85 H85 120.0 . . ?
C87 C86 C85 120.0 . . ?
C87 C86 H86 120.0 . . ?
C85 C86 H86 120.0 . . ?
C86 C87 C88 120.0 . . ?
C86 C87 N10 118.9(12) . . ?
C88 C87 N10 121.0(12) . . ?
C87 C88 C89 120.0 . . ?
C87 C88 H88 120.0 . . ?
C89 C88 H88 120.0 . . ?
C88 C89 C84 120.0 . . ?
C88 C89 H89 120.0 . . ?
C84 C89 H89 120.0 . . ?
C91 C90 C94 120.0 . . ?
C91 C90 N11 122.6(5) . . ?
C94 C90 N11 117.1(5) . . ?
C91 C90 N11B 103.0(6) . . ?
C94 C90 N11B 134.5(6) . . ?
N11 C90 N11B 27.6(8) . . ?
C90 C91 N12 120.0 . . ?
C90 C91 H91 120.0 . . ?
N12 C91 H91 120.0 . . ?
C91 N12 C93 120.0 . . ?
C92 C93 N12 120.0 . . ?
C92 C93 H93 120.0 . . ?
N12 C93 H93 120.0 . . ?
C94 C92 C93 120.0 . . ?
C94 C92 H92 120.0 . . ?
C93 C92 H92 120.0 . . ?
C92 C94 C90 120.0 . . ?
C92 C94 H94 120.0 . . ?
C90 C94 H94 120.0 . . ?
O13 C95 H95A 109.5 . . ?
O13 C95 H95B 109.5 . . ?
H95A C95 H95B 109.5 . . ?
O13 C95 H95C 109.5 . . ?
H95A C95 H95C 109.5 . . ?
H95B C95 H95C 109.5 . . ?
O14 C96 C97 138.9(7) . . ?
O14 C96 O15 111.2(9) . . ?
C97 C96 O15 105.2(6) . . ?
C98 C97 C102 120.0 . . ?
C98 C97 C96 102.8 . . ?
C102 C97 C96 136.9 . . ?
C97 C98 C99 120.0 . . ?
C97 C98 H98 120.0 . . ?
C99 C98 H98 120.0 . . ?
C98 C99 C100 120.0 . . ?
C98 C99 H99 120.0 . . ?
C100 C99 H99 120.0 . . ?
C101 C100 C99 120.0 . . ?
C101 C100 N13 105.5(12) . . ?
C99 C100 N13 134.5(12) . . ?
C102 C101 C100 120.0 . . ?
C102 C101 H101 120.0 . . ?
C100 C101 H101 120.0 . . ?
C101 C102 C97 120.0 . . ?
C101 C102 H102 120.0 . . ?
C97 C102 H102 120.0 . . ?
C104 C103 C107 120.0 . . ?
C104 C103 N14 113.8(15) . . ?
C107 C103 N14 126.2(15) . . ?
C105 C104 C103 120.0 . . ?
C105 C104 H104 120.0 . . ?
C103 C104 H104 120.0 . . ?
C104 C105 C106 120.0 . . ?
C104 C105 H105 120.0 . . ?
C106 C105 H105 120.0 . . ?
N15 C106 C105 120.0 . . ?
N15 C106 H106 120.0 . . ?
C105 C106 H106 120.0 . . ?
C106 N15 C107 120.0 . . ?
N15 C107 C103 120.0 . . ?
N15 C107 H107 120.0 . . ?
C103 C107 H107 120.0 . . ?
O16 C108 H10A 109.5 . . ?
O16 C108 H10B 109.5 . . ?
H10A C108 H10B 109.5 . . ?
O16 C108 H10C 109.5 . . ?
H10A C108 H10C 109.5 . . ?
H10B C108 H10C 109.5 . . ?
O18 C109 O17 116.1(10) . . ?
O18 C109 C110 116.6(8) . . ?
O17 C109 C110 109.3(5) . . ?
C111 C110 C115 120.0 . . ?
C111 C110 C109 115.6 . . ?
C115 C110 C109 122.1 . . ?
C110 C111 C112 120.0 . . ?
C110 C111 H111 120.0 . . ?
C112 C111 H111 120.0 . . ?
C113 C112 C111 120.0 . . ?
C113 C112 H112 120.0 . . ?
C111 C112 H112 120.0 . . ?
C112 C113 C114 120.0 . . ?
C112 C113 N16 118.3(12) . . ?
C114 C113 N16 121.0(12) . . ?
C113 C114 C115 120.0 . . ?
C113 C114 H114 120.0 . . ?
C115 C114 H114 120.0 . . ?
C110 C115 C114 120.0 . . ?
C110 C115 H115 120.0 . . ?
C114 C115 H115 120.0 . . ?
C117 C116 C120 120.0 . . ?
C117 C116 N17 131.2(17) . . ?
C120 C116 N17 107.7(17) . . ?
C116 C117 C118 120.0 . . ?
C116 C117 H117 120.0 . . ?
C118 C117 H117 120.0 . . ?
C117 C118 C119 120.0 . . ?
C117 C118 H118 120.0 . . ?
C119 C118 H118 120.0 . . ?
C118 C119 N18 120.0 . . ?
C118 C119 H119 120.0 . . ?
N18 C119 H119 120.0 . . ?
C120 N18 C119 120.0 . . ?
N18 C120 C116 120.0 . . ?
N18 C120 H120 120.0 . . ?
C116 C120 H120 120.0 . . ?
N11B N10B C87B 100.0(12) . . ?
N10B N11B C90 94.2(7) . . ?
N16 N17B C16B 97.5(18) . . ?
C17B C16B C20B 120.0 . . ?
C17B C16B N17B 111(2) . . ?
C20B C16B N17B 128(2) . . ?
C16B C17B C18B 120.0 . . ?
C16B C17B H17B 120.0 . . ?
C18B C17B H17B 120.0 . . ?
C19B C18B C17B 120.0 . . ?
C19B C18B H18B 120.0 . . ?
C17B C18B H18B 120.0 . . ?
C18B C19B N18B 120.0 . . ?
C18B C19B H19B 120.0 . . ?
N18B C19B H19B 120.0 . . ?
C20B N18B C19B 120.0 . . ?
N18B C20B C16B 120.0 . . ?
N18B C20B H20B 120.0 . . ?
C16B C20B H20B 120.0 . . ?
C85B C84B C89B 120.0 . . ?
C85B C84B C83 107.1(12) . . ?
C89B C84B C83 131.7(11) . . ?
C84B C85B C86B 120.0 . . ?
C84B C85B H85B 120.0 . . ?
C86B C85B H85B 120.0 . . ?
C85B C86B C87B 120.0 . . ?
C85B C86B H86B 120.0 . . ?
C87B C86B H86B 120.0 . . ?
C88B C87B C86B 120.0 . . ?
C88B C87B N10B 131.7(15) . . ?
C86B C87B N10B 107.3(14) . . ?
C87B C88B C89B 120.0 . . ?
C87B C88B H88B 120.0 . . ?
C89B C88B H88B 120.0 . . ?
C88B C89B C84B 120.0 . . ?
C88B C89B H89B 120.0 . . ?
C84B C89B H89B 120.0 . . ?

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
C27 N1 N2 C30 179.8(16) . . . . ?
C40 N4 N5 C43 176.6(6) . . . . ?
C53 N7 N8 C56 -177.1(11) . . . . ?
C87 N10 N11 C90 -170.1(9) . . . . ?
C100 N13 N14 C103 -179.6(19) . . . . ?
N17B N16 N17 C116 -46(6) . . . . ?
C113 N16 N17 C116 173.7(17) . . . . ?
C6 C1 C2 C3 3.9(18) . . . . ?
C21 C1 C2 C3 178.9(11) . . . . ?
C22 O1 C3 C4 -173.7(13) . . . . ?
C22 O1 C3 C2 4.8(18) . . . . ?
C1 C2 C3 C4 -2(2) . . . . ?
C1 C2 C3 O1 179.4(11) . . . . ?
O1 C3 C4 C5 177.2(11) . . . . ?
C2 C3 C4 C5 -1(3) . . . . ?
O1 C3 C4 O2 3(2) . . . . ?
C2 C3 C4 O2 -175.1(12) . . . . ?
C23 O2 C4 C3 -110.1(19) . . . . ?
C23 O2 C4 C5 75.3(18) . . . . ?
C3 C4 C5 C6 3(2) . . . . ?
O2 C4 C5 C6 177.1(11) . . . . ?
C2 C1 C6 C5 -3(2) . . . . ?
C21 C1 C6 C5 -176.9(12) . . . . ?
C2 C1 C6 C7 177.3(11) . . . . ?
C21 C1 C6 C7 3(2) . . . . ?
C4 C5 C6 C1 -0.8(19) . . . . ?
C4 C5 C6 C7 179.3(10) . . . . ?
C1 C6 C7 C8 -90.8(15) . . . . ?
C5 C6 C7 C8 89.1(14) . . . . ?
C6 C7 C8 C9 -79.5(14) . . . . ?
C6 C7 C8 C13 98.1(15) . . . . ?
C13 C8 C9 C10 0(2) . . . . ?
C7 C8 C9 C10 177.2(11) . . . . ?
C35 O4 C10 C9 1.9(18) . . . . ?
C35 O4 C10 C11 178.5(9) . . . . ?
C8 C9 C10 O4 -178.5(12) . . . . ?
C8 C9 C10 C11 5.0(19) . . . . ?
O4 C10 C11 C12 177.2(11) . . . . ?
C9 C10 C11 C12 -6(2) . . . . ?
O4 C10 C11 O5 7.6(18) . . . . ?
C9 C10 C11 O5 -175.3(11) . . . . ?
C36 O5 C11 C12 121.3(11) . . . . ?
C36 O5 C11 C10 -68.6(16) . . . . ?
C10 C11 C12 C13 2(2) . . . . ?
O5 C11 C12 C13 172.5(11) . . . . ?
C9 C8 C13 C12 -3.6(19) . . . . ?
C7 C8 C13 C12 179.1(10) . . . . ?
C9 C8 C13 C14 170.9(13) . . . . ?
C7 C8 C13 C14 -6(2) . . . . ?
C11 C12 C13 C8 2.7(19) . . . . ?
C11 C12 C13 C14 -172.5(12) . . . . ?
C8 C13 C14 C15 -88.3(16) . . . . ?
C12 C13 C14 C15 86.0(15) . . . . ?
C13 C14 C15 C20 90.9(17) . . . . ?
C13 C14 C15 C16 -82.8(15) . . . . ?
C20 C15 C16 C17 1(2) . . . . ?
C14 C15 C16 C17 175.0(11) . . . . ?
C48 O7 C17 C18 -161.7(12) . . . . ?
C48 O7 C17 C16 24.3(17) . . . . ?
C15 C16 C17 C18 3(2) . . . . ?
C15 C16 C17 O7 177.1(11) . . . . ?
O7 C17 C18 C19 -177.8(12) . . . . ?
C16 C17 C18 C19 -4(2) . . . . ?
O7 C17 C18 O8 4(2) . . . . ?
C16 C17 C18 O8 178.0(11) . . . . ?
C49 O8 C18 C17 -70.3(17) . . . . ?
C49 O8 C18 C19 111.2(13) . . . . ?
C17 C18 C19 C20 0(2) . . . . ?
O8 C18 C19 C20 178.7(11) . . . . ?
C16 C15 C20 C19 -5(2) . . . . ?
C14 C15 C20 C19 -177.7(12) . . . . ?
C16 C15 C20 C21 176.6(11) . . . . ?
C14 C15 C20 C21 3(2) . . . . ?
C18 C19 C20 C15 4(2) . . . . ?
C18 C19 C20 C21 -177.0(12) . . . . ?
C6 C1 C21 C20 85.3(18) . . . . ?
C2 C1 C21 C20 -89.3(16) . . . . ?
C15 C20 C21 C1 -97.2(18) . . . . ?
C19 C20 C21 C1 83.9(16) . . . . ?
C4 O2 C23 O3 12(3) . . . . ?
C4 O2 C23 C24 165.3(14) . . . . ?
O3 C23 C24 C25 -16(2) . . . . ?
O2 C23 C24 C25 -170.9(13) . . . . ?
O3 C23 C24 C29 173.5(15) . . . . ?
O2 C23 C24 C29 18(2) . . . . ?
C29 C24 C25 C26 0.0 . . . . ?
C23 C24 C25 C26 -170.8(15) . . . . ?
C24 C25 C26 C27 0.0 . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C25 C26 C27 N1 -179.7(15) . . . . ?
N2 N1 C27 C26 154.2(17) . . . . ?
N2 N1 C27 C28 -25(3) . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
N1 C27 C28 C29 180(2) . . . . ?
C27 C28 C29 C24 0.0 . . . . ?
C25 C24 C29 C28 0.0 . . . . ?
C23 C24 C29 C28 170.7(15) . . . . ?
N1 N2 C30 C31 164.8(16) . . . . ?
N1 N2 C30 C34 -12(3) . . . . ?
C34 C30 C31 C32 0.0 . . . . ?
N2 C30 C31 C32 -177.4(13) . . . . ?
C30 C31 C32 C33 0.0 . . . . ?
C31 C32 C33 N3 0.0 . . . . ?
C32 C33 N3 C34 0.0 . . . . ?
C33 N3 C34 C30 0.0 . . . . ?
C31 C30 C34 N3 0.0 . . . . ?
N2 C30 C34 N3 176.9(15) . . . . ?
C11 O5 C36 O6 -21.4(14) . . . . ?
C11 O5 C36 C37 170.2(7) . . . . ?
O5 C36 C37 C38 172.0(5) . . . . ?
O6 C36 C37 C38 1.3(5) . . . . ?
O5 C36 C37 C42 -12.9(5) . . . . ?
O6 C36 C37 C42 176.4(5) . . . . ?
C42 C37 C38 C39 -0.3 . . . . ?
C36 C37 C38 C39 173.9 . . . . ?
C37 C38 C39 C40 -0.6 . . . . ?
C38 C39 C40 C41 3.5 . . . . ?
C38 C39 C40 N4 177.2(4) . . . . ?
N5 N4 C40 C41 -177.2(9) . . . . ?
N5 N4 C40 C39 8.2(12) . . . . ?
C39 C40 C41 C42 -5.0 . . . . ?
N4 C40 C41 C42 -178.6(5) . . . . ?
C40 C41 C42 C37 3.3 . . . . ?
C38 C37 C42 C41 -0.9 . . . . ?
C36 C37 C42 C41 -176.3 . . . . ?
N4 N5 C43 C44 174.5(8) . . . . ?
N4 N5 C43 C47 -12.2(11) . . . . ?
C47 C43 C44 C45 5.1 . . . . ?
N5 C43 C44 C45 177.7(5) . . . . ?
C43 C44 C45 C46 -2.5 . . . . ?
C44 C45 C46 N6 8.2(7) . . . . ?
C47 N6 C46 C45 -15.7(14) . . . . ?
C44 C43 C47 N6 -10.4(6) . . . . ?
N5 C43 C47 N6 176.9(8) . . . . ?
C46 N6 C47 C43 15.1(12) . . . . ?
C18 O8 C49 O9 1.2(15) . . . . ?
C18 O8 C49 C50 179.2(10) . . . . ?
O9 C49 C50 C51 0.5(13) . . . . ?
O8 C49 C50 C51 -177.4(6) . . . . ?
O9 C49 C50 C55 -174.4(9) . . . . ?
O8 C49 C50 C55 7.7(10) . . . . ?
C55 C50 C51 C52 0.0 . . . . ?
C49 C50 C51 C52 -174.9(8) . . . . ?
C50 C51 C52 C53 0.0 . . . . ?
C51 C52 C53 C54 0.0 . . . . ?
C51 C52 C53 N7 177.1(12) . . . . ?
N8 N7 C53 C52 -1(2) . . . . ?
N8 N7 C53 C54 175.8(16) . . . . ?
C52 C53 C54 C55 0.0 . . . . ?
N7 C53 C54 C55 -177.3(11) . . . . ?
C53 C54 C55 C50 0.0 . . . . ?
C51 C50 C55 C54 0.0 . . . . ?
C49 C50 C55 C54 175.0(8) . . . . ?
N7 N8 C56 C57 179.2(15) . . . . ?
N7 N8 C56 C60 -3(2) . . . . ?
C60 C56 C57 N9 0.0 . . . . ?
N8 C56 C57 N9 177.7(8) . . . . ?
C56 C57 N9 C59 0.0 . . . . ?
C57 N9 C59 C58 0.0 . . . . ?
N9 C59 C58 C60 0.0 . . . . ?
C59 C58 C60 C56 0.0 . . . . ?
C57 C56 C60 C58 0.0 . . . . ?
N8 C56 C60 C58 -177.6(8) . . . . ?
C66 C61 C62 C63 -1.0 . . . . ?
C81 C61 C62 C63 177.7 . . . . ?
C82 O10 C63 C64 -179.2(4) . . . . ?
C82 O10 C63 C62 -4.3(9) . . . . ?
C61 C62 C63 C64 -4.2 . . . . ?
C61 C62 C63 O10 -179.4(5) . . . . ?
O10 C63 C64 C65 -177.0(5) . . . . ?
C62 C63 C64 C65 7.7 . . . . ?
O10 C63 C64 O11 -9.6(6) . . . . ?
C62 C63 C64 O11 175.2(4) . . . . ?
C83 O11 C64 C63 72.3(7) . . . . ?
C83 O11 C64 C65 -117.6(6) . . . . ?
C63 C64 C65 C66 -5.1 . . . . ?
O11 C64 C65 C66 -173.7(4) . . . . ?
C62 C61 C66 C65 4.0 . . . . ?
C81 C61 C66 C65 -174.5 . . . . ?
C62 C61 C66 C67 -172.2 . . . . ?
C81 C61 C66 C67 9.3 . . . . ?
C64 C65 C66 C61 -1.5 . . . . ?
C64 C65 C66 C67 175.1 . . . . ?
C61 C66 C67 C68 92.7 . . . . ?
C65 C66 C67 C68 -84.0 . . . . ?
C66 C67 C68 C69 87.5 . . . . ?
C66 C67 C68 C73 -96.7 . . . . ?
C73 C68 C69 C70 5.2 . . . . ?
C67 C68 C69 C70 -178.8 . . . . ?
C68 C69 C70 C71 -5.9 . . . . ?
C68 C69 C70 O13 178.1(5) . . . . ?
C95 O13 C70 C71 159.0(5) . . . . ?
C95 O13 C70 C69 -24.7(9) . . . . ?
C69 C70 C71 C72 2.5 . . . . ?
O13 C70 C71 C72 178.5(5) . . . . ?
C69 C70 C71 O14 178.5(6) . . . . ?
O13 C70 C71 O14 -5.5(7) . . . . ?
C96 O14 C71 C70 86.4(11) . . . . ?
C96 O14 C71 C72 -97.6(10) . . . . ?
C70 C71 C72 C73 1.3 . . . . ?
O14 C71 C72 C73 -175.0(5) . . . . ?
C69 C68 C73 C72 -1.9 . . . . ?
C67 C68 C73 C72 -177.9 . . . . ?
C69 C68 C73 C74 177.6 . . . . ?
C67 C68 C73 C74 1.6 . . . . ?
C71 C72 C73 C68 -1.5 . . . . ?
C71 C72 C73 C74 179.0 . . . . ?
C68 C73 C74 C75 92.3 . . . . ?
C72 C73 C74 C75 -88.3 . . . . ?
C73 C74 C75 C80 -86.7 . . . . ?
C73 C74 C75 C76 93.7 . . . . ?
C80 C75 C76 C77 -1.0 . . . . ?
C74 C75 C76 C77 178.7 . . . . ?
C108 O16 C77 C78 179.3(6) . . . . ?
C108 O16 C77 C76 -1.2(10) . . . . ?
C75 C76 C77 C78 0.2 . . . . ?
C75 C76 C77 O16 -179.2(5) . . . . ?
O16 C77 C78 C79 177.4(5) . . . . ?
C76 C77 C78 C79 -2.1 . . . . ?
O16 C77 C78 O17 0.3(6) . . . . ?
C76 C77 C78 O17 -179.2(5) . . . . ?
C109 O17 C78 C77 111.6(7) . . . . ?
C109 O17 C78 C79 -65.8(9) . . . . ?
C77 C78 C79 C80 4.2 . . . . ?
O17 C78 C79 C80 -178.8(5) . . . . ?
C76 C75 C80 C79 3.7 . . . . ?
C74 C75 C80 C79 -175.8 . . . . ?
C76 C75 C80 C81 176.7 . . . . ?
C74 C75 C80 C81 -2.8 . . . . ?
C78 C79 C80 C75 -5.1 . . . . ?
C78 C79 C80 C81 -178.5 . . . . ?
C66 C61 C81 C80 -100.0 . . . . ?
C62 C61 C81 C80 81.5 . . . . ?
C75 C80 C81 C61 88.6 . . . . ?
C79 C80 C81 C61 -97.5 . . . . ?
C64 O11 C83 O12 11.4(13) . . . . ?
C64 O11 C83 C84 -171.8(6) . . . . ?
C64 O11 C83 C84B -154.1(9) . . . . ?
O11 C83 C84 C85 12.2(10) . . . . ?
O12 C83 C84 C85 -170.7(8) . . . . ?
C84B C83 C84 C85 -130(2) . . . . ?
O11 C83 C84 C89 -176.7(7) . . . . ?
O12 C83 C84 C89 0.4(11) . . . . ?
C84B C83 C84 C89 41(2) . . . . ?
C89 C84 C85 C86 0.0 . . . . ?
C83 C84 C85 C86 170.8(11) . . . . ?
C84 C85 C86 C87 0.0 . . . . ?
C85 C86 C87 C88 0.0 . . . . ?
C85 C86 C87 N10 176.4(12) . . . . ?
N11 N10 C87 C86 170.9(10) . . . . ?
N11 N10 C87 C88 -12.7(18) . . . . ?
C86 C87 C88 C89 0.0 . . . . ?
N10 C87 C88 C89 -176.4(13) . . . . ?
C87 C88 C89 C84 0.0 . . . . ?
C85 C84 C89 C88 0.0 . . . . ?
C83 C84 C89 C88 -171.4(10) . . . . ?
N10 N11 C90 C91 -168.8(10) . . . . ?
N10 N11 C90 C94 5.5(14) . . . . ?
N10 N11 C90 N11B 142(2) . . . . ?
C94 C90 C91 N12 0.0 . . . . ?
N11 C90 C91 N12 174.1(6) . . . . ?
N11B C90 C91 N12 -164.6(7) . . . . ?
C90 C91 N12 C93 0.0 . . . . ?
C91 N12 C93 C92 0.0 . . . . ?
N12 C93 C92 C94 0.0 . . . . ?
C93 C92 C94 C90 0.0 . . . . ?
C91 C90 C94 C92 0.0 . . . . ?
N11 C90 C94 C92 -174.4(6) . . . . ?
N11B C90 C94 C92 158.8(9) . . . . ?
C71 O14 C96 C97 -169.4(5) . . . . ?
C71 O14 C96 O15 -18.8(14) . . . . ?
O14 C96 C97 C98 -29.0(9) . . . . ?
O15 C96 C97 C98 179.3(6) . . . . ?
O14 C96 C97 C102 158.2(9) . . . . ?
O15 C96 C97 C102 6.5(6) . . . . ?
C102 C97 C98 C99 0.0 . . . . ?
C96 C97 C98 C99 -174.3 . . . . ?
C97 C98 C99 C100 0.0 . . . . ?
C98 C99 C100 C101 0.0 . . . . ?
C98 C99 C100 N13 -179.0(16) . . . . ?
N14 N13 C100 C101 -135(2) . . . . ?
N14 N13 C100 C99 44(3) . . . . ?
C99 C100 C101 C102 0.0 . . . . ?
N13 C100 C101 C102 179.2(12) . . . . ?
C100 C101 C102 C97 0.0 . . . . ?
C98 C97 C102 C101 0.0 . . . . ?
C96 C97 C102 C101 171.9 . . . . ?
N13 N14 C103 C104 14(3) . . . . ?
N13 N14 C103 C107 -165(2) . . . . ?
C107 C103 C104 C105 0.0 . . . . ?
N14 C103 C104 C105 -179.4(16) . . . . ?
C103 C104 C105 C106 0.0 . . . . ?
C104 C105 C106 N15 0.0 . . . . ?
C105 C106 N15 C107 0.0 . . . . ?
C106 N15 C107 C103 0.0 . . . . ?
C104 C103 C107 N15 0.0 . . . . ?
N14 C103 C107 N15 179.3(18) . . . . ?
C78 O17 C109 O18 -32.0(13) . . . . ?
C78 O17 C109 C110 -166.5(5) . . . . ?
O18 C109 C110 C111 39.0(8) . . . . ?
O17 C109 C110 C111 173.3(6) . . . . ?
O18 C109 C110 C115 -158.1(8) . . . . ?
O17 C109 C110 C115 -23.8(6) . . . . ?
C115 C110 C111 C112 0.0 . . . . ?
C109 C110 C111 C112 163.2 . . . . ?
C110 C111 C112 C113 0.0 . . . . ?
C111 C112 C113 C114 0.0 . . . . ?
C111 C112 C113 N16 170.6(11) . . . . ?
N17 N16 C113 C112 2(3) . . . . ?
N17B N16 C113 C112 -155.1(11) . . . . ?
N17 N16 C113 C114 172(2) . . . . ?
N17B N16 C113 C114 15.5(19) . . . . ?
C112 C113 C114 C115 0.0 . . . . ?
N16 C113 C114 C115 -170.3(12) . . . . ?
C111 C110 C115 C114 0.0 . . . . ?
C109 C110 C115 C114 -162.1 . . . . ?
C113 C114 C115 C110 0.0 . . . . ?
N16 N17 C116 C117 9(4) . . . . ?
N16 N17 C116 C120 177(2) . . . . ?
C120 C116 C117 C118 0.0 . . . . ?
N17 C116 C117 C118 167(2) . . . . ?
C116 C117 C118 C119 0.0 . . . . ?
C117 C118 C119 N18 0.0 . . . . ?
C118 C119 N18 C120 0.0 . . . . ?
C119 N18 C120 C116 0.0 . . . . ?
C117 C116 C120 N18 0.0 . . . . ?
N17 C116 C120 N18 -169.6(18) . . . . ?
C87B N10B N11B C90 158.9(13) . . . . ?
C91 C90 N11B N10B -178.9(4) . . . . ?
C94 C90 N11B N10B 19.8(10) . . . . ?
N11 C90 N11B N10B -40.2(12) . . . . ?
N17 N16 N17B C16B 31(5) . . . . ?
C113 N16 N17B C16B 172.9(15) . . . . ?
N16 N17B C16B C17B -160.0(14) . . . . ?
N16 N17B C16B C20B 31(2) . . . . ?
C20B C16B C17B C18B 0.0 . . . . ?
N17B C16B C17B C18B -170(2) . . . . ?
C16B C17B C18B C19B 0.0 . . . . ?
C17B C18B C19B N18B 0.0 . . . . ?
C18B C19B N18B C20B 0.0 . . . . ?
C19B N18B C20B C16B 0.0 . . . . ?
C17B C16B C20B N18B 0.0 . . . . ?
N17B C16B C20B N18B 168(2) . . . . ?
O11 C83 C84B C85B -5.1(13) . . . . ?
O12 C83 C84B C85B -173.6(8) . . . . ?
C84 C83 C84B C85B 40.5(19) . . . . ?
O11 C83 C84B C89B -172.0(10) . . . . ?
O12 C83 C84B C89B 19.5(15) . . . . ?
C84 C83 C84B C89B -126(3) . . . . ?
C89B C84B C85B C86B 0.0 . . . . ?
C83 C84B C85B C86B -168.7(13) . . . . ?
C84B C85B C86B C87B 0.0 . . . . ?
C85B C86B C87B C88B 0.0 . . . . ?
C85B C86B C87B N10B -169.6(15) . . . . ?
N11B N10B C87B C88B 8.3(14) . . . . ?
N11B N10B C87B C86B 176.2(8) . . . . ?
C86B C87B C88B C89B 0.0 . . . . ?
N10B C87B C88B C89B 166.6(18) . . . . ?
C87B C88B C89B C84B 0.0 . . . . ?
C85B C84B C89B C88B 0.0 . . . . ?
C83 C84B C89B C88B 165.5(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        20.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.080
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.037 0.000 0.500 4564 758 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

# start Validation Reply Form
_vrf_ATOM007_I                   
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: Structure refined isotropically due to very weak data
;
_vrf_THETM01_I                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: ...Very weak data from poorly diffracting crystals
;
_vrf_PLAT023_I                   
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      20.00 Degree
RESPONSE: ...Very weak data from poorly diffracting crystals
;
_vrf_PLAT082_I                   
;
PROBLEM: High R1 Value ..................................       0.23 Report
RESPONSE: ...Data is weak and there is significant disorder
;
_vrf_PLAT084_I                   
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.49 Report
RESPONSE: ...Data is weak and there is significant disorder
;
_vrf_PLAT201_I                   
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......        149 Report
RESPONSE: ...Structure refined isotropically due to very weak data
;
# end Validation Reply Form
