# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2023

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 2208926'
loop_
_audit_author_name
_audit_author_address
'Aida I Samigullina'
;N D Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences 
Russia
;
_audit_update_record             
;
2022-09-22 deposited with the CCDC.	2022-12-09 downloaded from the CCDC.
;
_audit_creation_date             2022-06-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2018/3
# start Validation Reply Form
_vrf_PLAT430_4                   
;
PROBLEM: Short Inter D...A Contact  O8       ..N20      .       2.74 Ang.  
RESPONSE: These intermolecular interactions are expected for this structure.
;
_vrf_PLAT089_4                   
;
PROBLEM: Poor Data / Parameter Ratio (Zmax < 18) ........       6.26 Note  
RESPONSE: The small size and weak reflectivity of the crystal do not 
allow the use of Mo-radiation. More reflections on Cu-radiation cannot be
obtained.
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C13 H16 N20 O16'
_chemical_formula_sum            'C13 H16 N20 O16'
_chemical_formula_weight         708.46
_chemical_absolute_configuration unk
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     PGV-2022
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.06669(19)
_cell_length_b                   13.5410(3)
_cell_length_c                   11.9398(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.3951(19)
_cell_angle_gamma                90
_cell_volume                     1278.49(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18074
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.4680
_cell_measurement_theta_min      3.2480
_shelx_estimated_absorpt_T_max   0.971
_shelx_estimated_absorpt_T_min   0.755
_exptl_absorpt_coefficient_mu    1.487
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.57a (Rigaku Oxford Diffraction, 2022)
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   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             724
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0637
0 -1 0 0.0693
0 0 1 0.0157
0 0 -1 0.0061
3 -4 4 0.0415
-1 -1 -1 0.0522
-1 0 1 0.1023
1 1 1 0.0659

_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
loop_
_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
0.0008 0.9998 -0.0026 0.0793 -0.0796 -0.0178
-0.0008 -0.9998 0.0026 -0.0793 0.0796 0.0178
0.0006 -0.0000 0.9980 0.0708 0.0486 0.0994
-0.0006 0.0000 -0.9980 -0.0708 -0.0486 -0.0994
3.4402 -3.6288 3.7916 -0.2569 0.1196 0.9590
-1.0007 -1.0003 -1.0003 -0.0815 0.1334 -0.2326
-0.9987 -0.0006 0.9930 0.1394 0.1511 -0.0515
1.0007 1.0003 1.0003 0.0815 -0.1334 0.2326

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24639
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.802
_diffrn_reflns_theta_min         3.777
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     58.00  92.00   0.50    0.81    --  107.75-165.00 123.00   68
  2  ω     97.00 138.00   0.50    0.81    --  107.75-165.00 123.00   82
  3  ω     69.00  95.00   0.50    0.81    --  107.75-125.00  30.00   52
  4  ω     38.00  66.00   0.50    0.81    --  107.75-125.00  30.00   56
  5  ω     46.00  81.00   0.50    0.20    --   48.45-116.00 -88.00   70
  6  ω     39.00  67.00   0.50    0.81    --  107.75-125.00-150.00   56
  7  ω     75.00 102.00   0.50    0.81    --  107.75-125.00-150.00   54
  8  ω     80.00 105.00   0.50    0.81    --  107.75-116.00 -88.00   50
  9  ω     76.00 105.00   0.50    0.81    --  107.75 -95.00 -90.00   58
 10  ω     43.00  69.00   0.50    0.81    --  107.75 -95.00 -90.00   52
 11  ω     73.00  99.00   0.50    0.81    --  107.75 -95.00 -60.00   52
 12  ω     88.00 114.00   0.50    0.81    --  107.75 -87.00-135.98   52
 13  ω     64.00 103.00   0.50    0.81    --  107.75 -95.00 -30.00   78
 14  ω     83.00 108.00   0.50    0.81    --  107.75-107.00  68.32   50
 15  ω     61.00  87.00   0.50    0.81    --  107.75 -88.00 151.88   52
 16  ω    103.00 128.00   0.50    0.81    --  107.75 -88.00 151.88   50
 17  ω     44.00  80.00   0.50    0.81    --  107.75 -87.00-135.98   72
 18  ω     78.00 103.00   0.50    0.81    --  107.75 -77.00 -90.00   50
 19  ω     37.00  69.00   0.50    0.81    --  107.75 -77.00-120.00   64
 20  ω     41.00  66.00   0.50    0.81    --  107.75 -72.00-119.61   50
 21  ω     37.00  69.00   0.50    0.81    --  107.75 -77.00 -90.00   64
 22  ω     39.00  64.00   0.50    0.81    --  107.75 -61.00 -60.00   50
 23  ω     39.00  71.00   0.50    0.81    --  107.75 -61.00 -90.00   64
 24  ω     40.00  65.00   0.50    0.81    --  107.75 -61.00 -30.00   50
 25  ω     40.00  70.00   0.50    0.81    --  107.75 -61.00   0.00   60
 26  ω     36.00  61.00   0.50    0.81    --  107.75 -61.00  60.00   50
 27  ω     45.00  71.00   0.50    0.81    --  107.75 -61.00  90.00   52
 28  ω    -24.00  25.00   0.50    0.20    --   48.45 -19.00-120.00   98
 29  ω    -23.00  42.00   0.50    0.20    --   48.45 -38.00   0.00  130
 30  ω    103.00 147.00   0.50    0.81    --  107.75  61.00 150.00   88
 31  ω    109.00 135.00   0.50    0.81    --  107.75  45.00  90.00   52
 32  ω    106.00 136.00   0.50    0.81    --  107.75  45.00  60.00   60
 33  ω    145.00 177.00   0.50    0.81    --  107.75  45.00  60.00   64
 34  ω    107.00 177.00   0.50    0.81    --  107.75  45.00   0.00  140
 35  ω     99.00 124.00   0.50    0.81    --  107.75  30.00 -60.00   50
 36  ω    143.00 171.00   0.50    0.81    --  107.75  30.00 -60.00   56
 37  ω    148.00 175.00   0.50    0.81    --  107.75  35.00 -90.64   54
 38  ω    130.00 165.00   0.50    0.81    --  107.75  45.00-120.00   70
 39  ω    101.00 126.00   0.50    0.81    --  107.75  45.00-120.00   50
 40  ω    115.00 140.00   0.50    0.81    --  107.75 116.00  -0.00   50
 41  ω     96.00 139.00   0.50    0.81    --  107.75 125.00  90.00   86
 42  ω     98.00 123.00   0.50    0.81    --  107.75 125.00 120.00   50
 43  ω     70.00 113.00   0.50    0.81    --  107.75 165.00 146.00   86
 44  ω    143.00 169.00   0.50    0.81    --  107.75 125.00 120.00   52
 45  ω    146.00 172.00   0.50    0.81    --  107.75 125.00  90.00   52
 46  ω    -24.00   2.00   0.50    0.20    --  -48.45  19.00-150.00   52
 47  ω    -83.00 -19.00   0.50    0.20    --  -48.45 116.00  -0.00  128
 48  ω    -50.00 -15.00   0.50    0.81    --  -86.25  45.00-150.00   70
 49  ω   -119.00 -75.00   0.50    0.20    --  -48.45-125.00 120.00   88
 50  ω   -120.00 -47.00   0.50    0.20    --  -48.45-165.00 123.00  146
 51  ω   -120.00 -74.00   0.50    0.20    --  -48.45-125.00 -30.00   92
 52  ω   -119.00 -91.00   0.50    0.81    --  -86.25-116.00 -88.00   56
 53  ω     81.00 107.00   0.50    0.81    --  107.75-116.00 -88.00   52
 54  ω    -68.00 -37.00   0.50    0.20    --  -48.70 -57.00  30.00   62
 55  ω   -108.00 -82.00   0.50    0.20    --  -48.70 -57.00  30.00   52
 56  ω   -111.00 -75.00   0.50    0.20    --  -48.70-125.00-150.00   72
 57  ω    -23.00  26.00   0.50    0.20    --  -48.70  19.00 -30.00   98
 58  ω    -17.00   9.00   0.50    0.20    --   48.70 -19.00 -90.00   52
 59  ω    -49.00 -14.00   0.50    0.81    --  -86.25  45.00-180.00   70
 60  ω    -63.00 -36.00   0.50    0.81    --  -86.25  61.00  60.00   54
 61  ω     42.00  68.00   0.50    0.81    --  107.75 -61.00 120.00   52
 62  ω     44.00  82.00   0.50    0.81    --  107.75 -77.00 120.00   76
 63  ω     36.00  61.00   0.50    0.81    --  107.75 -56.00 -60.77   50
 64  ω    110.00 136.00   0.50    0.81    --  107.75 125.00 -90.00   52
 65  ω     43.00  69.00   0.50    0.81    --  107.75 -77.00   0.00   52
 66  ω    111.00 137.00   0.50    0.81    --  107.75  45.00 150.00   52
 67  ω    142.00 178.00   0.50    0.81    --  107.75  45.00 150.00   72
 68  ω     81.00 107.00   0.50    0.81    --  107.75-105.00 -32.81   52
 69  ω     62.00 106.00   0.50    0.81    --  107.75-125.00-120.00   88
 70  ω     73.00 108.00   0.50    0.81    --  107.75-109.00-142.50   70
 71  ω     71.00  96.00   0.50    0.81    --  107.75 -95.00   0.00   50
 72  ω     74.00 106.00   0.50    0.81    --  107.75-101.00  75.63   64
 73  ω     53.00 103.00   0.50    0.81    --  107.75-125.00 -60.00  100
 74  ω    104.00 130.00   0.50    0.81    --  107.75  30.00-150.00   52
 75  ω    139.00 165.00   0.50    0.81    --  107.75 125.00 -90.00   52
 76  ω     38.00  64.00   0.50    0.81    --  107.75-105.00 -32.81   52
 77  ω     38.00  64.00   0.50    0.81    --  107.75 -95.00   0.00   52
 78  ω     36.00  61.00   0.50    0.81    --  107.75 -61.00-150.00   50
 79  ω     41.00  67.00   0.50    0.81    --  107.75 -77.00  30.00   52
 80  ω     71.00  97.00   0.50    0.81    --  107.75 -77.00  30.00   52
 81  ω     92.00 151.00   0.50    0.81    --  107.75  77.00-120.00  118
 82  ω    103.00 129.00   0.50    0.81    --  107.75  15.00-150.00   52
 83  ω    138.00 164.00   0.50    0.81    --  107.75  15.00-150.00   52
 84  ω     74.00  99.00   0.50    0.81    --  107.75 -95.00 150.00   50
 85  ω    101.00 136.00   0.50    0.81    --  107.75  31.00-141.81   70
 86  ω     65.00  91.00   0.50    0.81    --  107.75-103.00 -42.87   52
 87  ω    101.00 128.00   0.50    0.81    --  107.75  30.00 150.00   54
 88  ω    153.00 178.00   0.50    0.81    --  107.75  15.00  30.00   50
 89  ω     94.00 119.00   0.50    0.81    --  107.75  61.00   0.00   50
 90  ω     37.00  63.00   0.50    0.81    --  107.75 -95.00  90.00   52
 91  ω     69.00  94.00   0.50    0.81    --  107.75 -77.00 -30.00   50
 92  ω     80.00 105.00   0.50    0.81    --  107.75 -95.00-150.00   50
 93  ω     77.00 110.00   0.50    0.81    --  107.75-125.00  90.00   66
 94  ω     40.00 105.00   0.50    0.81    --  107.75-125.00 150.00  130
 95  ω    152.00 177.00   0.50    0.81    --  107.75  30.00-180.00   50
 96  ω    149.00 174.00   0.50    0.81    --  107.75  15.00 120.00   50
 97  ω    130.00 156.00   0.50    0.81    --  107.75  30.00-120.00   52
 98  ω    128.00 154.00   0.50    0.81    --  107.75  15.00  90.00   52
 99  ω     83.00 108.00   0.50    0.81    --  107.75 -79.00 138.36   50
100  ω     63.00 103.00   0.50    0.81    --  107.75-101.00 127.57   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0690478000
_diffrn_orient_matrix_UB_12      0.0795305000
_diffrn_orient_matrix_UB_13      0.0710003000
_diffrn_orient_matrix_UB_21      -0.1027378000
_diffrn_orient_matrix_UB_22      -0.0793777000
_diffrn_orient_matrix_UB_23      0.0487838000
_diffrn_orient_matrix_UB_31      0.1505244000
_diffrn_orient_matrix_UB_32      -0.0176092000
_diffrn_orient_matrix_UB_33      0.0995033000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.879
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.950
_reflns_number_gt                5119
_reflns_number_total             5296
_reflns_odcompleteness_completeness 92.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     86.18
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 
;
 Flack x determined using 2321 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.06(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         5296
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0310
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0478P)²+0.3294P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0827
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4), C6(H6), C3(H3), C5(H5A), C1(H1), C2(H2), C10(H10), C9(H9), C8(H8),
 C7(H7), C12(H12), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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_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 0.8112(3) 0.42228(15) 0.62080(16) 0.0213(4) Uani 1 1 d . . . . .
O2 O 1.0043(2) 0.40544(16) 0.77485(17) 0.0225(4) Uani 1 1 d . . . . .
O5 O 0.6506(3) 0.71799(15) 0.73758(16) 0.0245(4) Uani 1 1 d . . . . .
O6 O 0.8834(3) 0.68549(16) 0.86012(18) 0.0250(4) Uani 1 1 d . . . . .
O3 O 0.8296(3) 0.35357(17) 1.10409(17) 0.0260(4) Uani 1 1 d . . . . .
O4 O 0.6003(3) 0.26658(17) 1.04331(19) 0.0276(5) Uani 1 1 d . . . . .
O7 O 0.7161(3) 0.62394(17) 1.16892(17) 0.0250(4) Uani 1 1 d . . . . .
O8 O 0.4531(3) 0.58304(16) 1.15433(17) 0.0235(4) Uani 1 1 d . . . . .
O13 O 0.4737(3) 0.70234(15) 0.37897(17) 0.0241(4) Uani 1 1 d . . . . .
O14 O 0.2375(3) 0.73325(15) 0.25959(17) 0.0238(4) Uani 1 1 d . . . . .
O16 O 0.2610(3) 0.39382(15) 0.11654(16) 0.0233(4) Uani 1 1 d . . . . .
O15 O 0.1030(2) 0.52451(16) 0.07869(16) 0.0212(4) Uani 1 1 d . . . . .
O11 O -0.3124(3) 0.42949(18) 0.3261(2) 0.0317(5) Uani 1 1 d . . . . .
O12 O -0.1923(3) 0.29456(16) 0.4047(2) 0.0308(5) Uani 1 1 d . . . . .
O10 O -0.1675(3) 0.64416(16) 0.5203(2) 0.0267(4) Uani 1 1 d . . . . .
O9 O 0.0243(3) 0.60619(16) 0.66980(17) 0.0244(4) Uani 1 1 d . . . . .
N1 N 0.7480(3) 0.46623(16) 0.78661(18) 0.0146(4) Uani 1 1 d . . . . .
N3 N 0.6406(3) 0.62065(16) 0.88342(18) 0.0152(4) Uani 1 1 d . . . . .
N2 N 0.6923(3) 0.36752(16) 0.92481(18) 0.0156(4) Uani 1 1 d . . . . .
N4 N 0.5937(3) 0.52450(17) 1.02448(18) 0.0146(4) Uani 1 1 d . . . . .
N5 N 0.3940(3) 0.41989(16) 0.89650(18) 0.0159(4) Uani 1 1 d . . . . .
N6 N 0.4592(3) 0.52291(16) 0.73198(18) 0.0141(4) Uani 1 1 d . . . . .
N7 N 0.8625(3) 0.42637(17) 0.72400(19) 0.0172(4) Uani 1 1 d . . . . .
N9 N 0.7320(3) 0.67754(16) 0.82244(19) 0.0181(5) Uani 1 1 d . . . . .
N8 N 0.7082(3) 0.32765(17) 1.0311(2) 0.0199(5) Uani 1 1 d . . . . .
N10 N 0.5870(3) 0.58285(17) 1.12091(18) 0.0172(4) Uani 1 1 d . . . . .
N13 N 0.2600(3) 0.59774(16) 0.36621(18) 0.0146(4) Uani 1 1 d . . . . .
N14 N 0.1608(3) 0.46513(17) 0.25651(18) 0.0161(4) Uani 1 1 d . . . . .
N11 N 0.0613(3) 0.56004(16) 0.49818(18) 0.0152(4) Uani 1 1 d . . . . .
N12 N -0.0363(3) 0.42568(17) 0.39173(19) 0.0175(4) Uani 1 1 d . . . . .
N15 N 0.2417(3) 0.35078(17) 0.41660(19) 0.0150(4) Uani 1 1 d . . . . .
N16 N 0.3507(3) 0.49941(16) 0.53722(18) 0.0136(4) Uani 1 1 d . . . . .
N19 N 0.3299(3) 0.68232(16) 0.33188(19) 0.0173(4) Uani 1 1 d . . . . .
N20 N 0.1781(3) 0.46187(17) 0.14448(19) 0.0169(4) Uani 1 1 d . . . . .
N18 N -0.1896(3) 0.38078(19) 0.3745(2) 0.0218(5) Uani 1 1 d . . . . .
N17 N -0.0355(3) 0.60478(16) 0.5682(2) 0.0193(5) Uani 1 1 d . . . . .
C4 C 0.5647(3) 0.43741(18) 0.7485(2) 0.0141(5) Uani 1 1 d . . . . .
H4 H 0.549227 0.397827 0.676446 0.017 Uiso 1 1 calc R U . . .
C6 C 0.4694(3) 0.58334(18) 0.8315(2) 0.0143(5) Uani 1 1 d . . . . .
H6 H 0.387348 0.639367 0.815400 0.017 Uiso 1 1 calc R U . . .
C3 C 0.5224(3) 0.37324(19) 0.8479(2) 0.0152(5) Uani 1 1 d . . . . .
H3 H 0.484540 0.305933 0.819226 0.018 Uiso 1 1 calc R U . . .
C5 C 0.4320(3) 0.51916(19) 0.9334(2) 0.0150(5) Uani 1 1 d . . . . .
H5A H 0.335349 0.548050 0.963348 0.018 Uiso 1 1 calc R U . . .
C1 C 0.7912(3) 0.45530(19) 0.9100(2) 0.0152(5) Uani 1 1 d . . . . .
H1 H 0.915098 0.443721 0.937024 0.018 Uiso 1 1 calc R U . . .
C2 C 0.7298(3) 0.55098(19) 0.9663(2) 0.0145(5) Uani 1 1 d . . . . .
H2 H 0.825352 0.583509 1.019584 0.017 Uiso 1 1 calc R U . . .
C13 C 0.4385(3) 0.57014(19) 0.6204(2) 0.0146(5) Uani 1 1 d . . . . .
H13A H 0.550104 0.587057 0.603025 0.017 Uiso 1 1 calc R U . . .
H13B H 0.371322 0.631492 0.618880 0.017 Uiso 1 1 calc R U . . .
C10 C 0.3684(3) 0.51564(18) 0.4216(2) 0.0132(5) Uani 1 1 d . . . . .
H10 H 0.489468 0.528297 0.418387 0.016 Uiso 1 1 calc R U . . .
C9 C 0.3006(3) 0.42306(19) 0.3469(2) 0.0138(5) Uani 1 1 d . . . . .
H9 H 0.391894 0.394736 0.310893 0.017 Uiso 1 1 calc R U . . .
C8 C 0.1049(3) 0.55748(19) 0.2994(2) 0.0152(5) Uani 1 1 d . . . . .
H8 H 0.052133 0.602789 0.236213 0.018 Uiso 1 1 calc R U . . .
C7 C -0.0208(3) 0.53197(19) 0.3829(2) 0.0165(5) Uani 1 1 d . . . . .
H7 H -0.133219 0.564754 0.358627 0.020 Uiso 1 1 calc R U . . .
C12 C 0.1790(3) 0.47863(18) 0.5467(2) 0.0142(5) Uani 1 1 d . . . . .
H12 H 0.172502 0.466847 0.628437 0.017 Uiso 1 1 calc R U . . .
C11 C 0.1131(3) 0.38573(19) 0.4727(2) 0.0151(5) Uani 1 1 d . . . . .
H11 H 0.077890 0.332680 0.521414 0.018 Uiso 1 1 calc R U . . .
H5 H 0.348(5) 0.383(3) 0.947(3) 0.024(9) Uiso 1 1 d . . . . .
H15 H 0.229(5) 0.291(3) 0.389(4) 0.031(10) 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
O1 N7 1.221(3) . ?
O2 N7 1.217(3) . ?
O5 N9 1.223(3) . ?
O6 N9 1.220(3) . ?
O3 N8 1.226(3) . ?
O4 N8 1.230(3) . ?
O7 N10 1.219(3) . ?
O8 N10 1.223(3) . ?
O13 N19 1.215(3) . ?
O14 N19 1.234(3) . ?
O16 N20 1.223(3) . ?
O15 N20 1.231(3) . ?
O11 N18 1.234(3) . ?
O12 N18 1.223(3) . ?
O10 N17 1.227(3) . ?
O9 N17 1.214(3) . ?
N1 N7 1.406(3) . ?
N1 C4 1.510(3) . ?
N1 C1 1.453(3) . ?
N3 N9 1.371(3) . ?
N3 C6 1.486(3) . ?
N3 C2 1.451(3) . ?
N2 N8 1.362(3) . ?
N2 C3 1.493(3) . ?
N2 C1 1.462(3) . ?
N4 N10 1.406(3) . ?
N4 C5 1.526(3) . ?
N4 C2 1.455(3) . ?
N5 C3 1.431(3) . ?
N5 C5 1.429(3) . ?
N5 H5 0.92(4) . ?
N6 C4 1.427(3) . ?
N6 C6 1.431(3) . ?
N6 C13 1.457(3) . ?
N13 N19 1.374(3) . ?
N13 C10 1.486(3) . ?
N13 C8 1.451(3) . ?
N14 N20 1.373(3) . ?
N14 C9 1.510(3) . ?
N14 C8 1.456(3) . ?
N11 N17 1.391(3) . ?
N11 C7 1.455(3) . ?
N11 C12 1.495(3) . ?
N12 N18 1.357(3) . ?
N12 C7 1.450(3) . ?
N12 C11 1.490(3) . ?
N15 C9 1.425(3) . ?
N15 C11 1.423(3) . ?
N15 H15 0.87(5) . ?
N16 C13 1.458(3) . ?
N16 C10 1.432(3) . ?
N16 C12 1.440(3) . ?
C4 H4 1.0000 . ?
C4 C3 1.562(3) . ?
C6 H6 1.0000 . ?
C6 C5 1.572(3) . ?
C3 H3 1.0000 . ?
C5 H5A 1.0000 . ?
C1 H1 1.0000 . ?
C1 C2 1.584(3) . ?
C2 H2 1.0000 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C10 H10 1.0000 . ?
C10 C9 1.573(3) . ?
C9 H9 1.0000 . ?
C8 H8 1.0000 . ?
C8 C7 1.594(4) . ?
C7 H7 1.0000 . ?
C12 H12 1.0000 . ?
C12 C11 1.568(3) . ?
C11 H11 1.0000 . ?

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
N7 N1 C4 116.6(2) . . ?
N7 N1 C1 116.7(2) . . ?
C1 N1 C4 107.7(2) . . ?
N9 N3 C6 121.5(2) . . ?
N9 N3 C2 118.8(2) . . ?
C2 N3 C6 111.0(2) . . ?
N8 N2 C3 120.0(2) . . ?
N8 N2 C1 118.8(2) . . ?
C1 N2 C3 109.87(19) . . ?
N10 N4 C5 116.4(2) . . ?
N10 N4 C2 114.0(2) . . ?
C2 N4 C5 106.86(19) . . ?
C3 N5 H5 117(2) . . ?
C5 N5 C3 114.3(2) . . ?
C5 N5 H5 113(2) . . ?
C4 N6 C6 114.48(19) . . ?
C4 N6 C13 116.1(2) . . ?
C6 N6 C13 119.0(2) . . ?
O1 N7 N1 115.2(2) . . ?
O2 N7 O1 126.2(2) . . ?
O2 N7 N1 118.4(2) . . ?
O5 N9 N3 115.8(2) . . ?
O6 N9 O5 126.9(2) . . ?
O6 N9 N3 117.3(2) . . ?
O3 N8 O4 126.4(2) . . ?
O3 N8 N2 117.6(2) . . ?
O4 N8 N2 116.0(2) . . ?
O7 N10 O8 125.0(2) . . ?
O7 N10 N4 118.3(2) . . ?
O8 N10 N4 116.6(2) . . ?
N19 N13 C10 121.1(2) . . ?
N19 N13 C8 120.6(2) . . ?
C8 N13 C10 109.3(2) . . ?
N20 N14 C9 118.6(2) . . ?
N20 N14 C8 117.9(2) . . ?
C8 N14 C9 108.17(19) . . ?
N17 N11 C7 118.5(2) . . ?
N17 N11 C12 118.5(2) . . ?
C7 N11 C12 108.0(2) . . ?
N18 N12 C7 121.5(2) . . ?
N18 N12 C11 122.1(2) . . ?
C7 N12 C11 109.7(2) . . ?
C9 N15 H15 116(3) . . ?
C11 N15 C9 113.9(2) . . ?
C11 N15 H15 117(3) . . ?
C10 N16 C13 115.4(2) . . ?
C10 N16 C12 112.7(2) . . ?
C12 N16 C13 114.8(2) . . ?
O13 N19 O14 126.0(2) . . ?
O13 N19 N13 117.3(2) . . ?
O14 N19 N13 116.6(2) . . ?
O16 N20 O15 124.9(2) . . ?
O16 N20 N14 117.2(2) . . ?
O15 N20 N14 117.9(2) . . ?
O11 N18 N12 117.0(2) . . ?
O12 N18 O11 126.1(2) . . ?
O12 N18 N12 116.9(2) . . ?
O10 N17 N11 116.6(2) . . ?
O9 N17 O10 126.6(2) . . ?
O9 N17 N11 116.6(2) . . ?
N1 C4 H4 110.3 . . ?
N1 C4 C3 105.21(19) . . ?
N6 C4 N1 110.7(2) . . ?
N6 C4 H4 110.3 . . ?
N6 C4 C3 110.0(2) . . ?
C3 C4 H4 110.3 . . ?
N3 C6 H6 110.3 . . ?
N3 C6 C5 99.74(19) . . ?
N6 C6 N3 115.9(2) . . ?
N6 C6 H6 110.3 . . ?
N6 C6 C5 109.7(2) . . ?
C5 C6 H6 110.3 . . ?
N2 C3 C4 100.63(19) . . ?
N2 C3 H3 110.2 . . ?
N5 C3 N2 115.1(2) . . ?
N5 C3 C4 110.3(2) . . ?
N5 C3 H3 110.2 . . ?
C4 C3 H3 110.2 . . ?
N4 C5 C6 104.96(19) . . ?
N4 C5 H5A 110.1 . . ?
N5 C5 N4 111.4(2) . . ?
N5 C5 C6 110.1(2) . . ?
N5 C5 H5A 110.1 . . ?
C6 C5 H5A 110.1 . . ?
N1 C1 N2 100.27(19) . . ?
N1 C1 H1 111.6 . . ?
N1 C1 C2 108.3(2) . . ?
N2 C1 H1 111.6 . . ?
N2 C1 C2 112.9(2) . . ?
C2 C1 H1 111.6 . . ?
N3 C2 N4 99.59(19) . . ?
N3 C2 C1 113.4(2) . . ?
N3 C2 H2 111.3 . . ?
N4 C2 C1 109.3(2) . . ?
N4 C2 H2 111.3 . . ?
C1 C2 H2 111.3 . . ?
N6 C13 N16 106.7(2) . . ?
N6 C13 H13A 110.4 . . ?
N6 C13 H13B 110.4 . . ?
N16 C13 H13A 110.4 . . ?
N16 C13 H13B 110.4 . . ?
H13A C13 H13B 108.6 . . ?
N13 C10 H10 110.3 . . ?
N13 C10 C9 103.63(18) . . ?
N16 C10 N13 112.5(2) . . ?
N16 C10 H10 110.3 . . ?
N16 C10 C9 109.5(2) . . ?
C9 C10 H10 110.3 . . ?
N14 C9 C10 103.4(2) . . ?
N14 C9 H9 110.3 . . ?
N15 C9 N14 112.8(2) . . ?
N15 C9 C10 109.57(19) . . ?
N15 C9 H9 110.3 . . ?
C10 C9 H9 110.3 . . ?
N13 C8 N14 102.9(2) . . ?
N13 C8 H8 112.1 . . ?
N13 C8 C7 108.9(2) . . ?
N14 C8 H8 112.1 . . ?
N14 C8 C7 108.3(2) . . ?
C7 C8 H8 112.1 . . ?
N11 C7 C8 107.9(2) . . ?
N11 C7 H7 112.0 . . ?
N12 C7 N11 102.7(2) . . ?
N12 C7 C8 109.6(2) . . ?
N12 C7 H7 112.0 . . ?
C8 C7 H7 112.0 . . ?
N11 C12 H12 110.2 . . ?
N11 C12 C11 104.75(19) . . ?
N16 C12 N11 111.9(2) . . ?
N16 C12 H12 110.2 . . ?
N16 C12 C11 109.7(2) . . ?
C11 C12 H12 110.2 . . ?
N12 C11 C12 102.4(2) . . ?
N12 C11 H11 110.6 . . ?
N15 C11 N12 112.7(2) . . ?
N15 C11 C12 109.6(2) . . ?
N15 C11 H11 110.6 . . ?
C12 C11 H11 110.6 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N5 H5 O16 0.92(4) 2.27(4) 3.048(3) 142(3) 1_556 yes
N15 H15 O5 0.87(5) 2.19(4) 2.830(3) 130(4) 2_646 yes
N15 H15 O10 0.87(5) 2.36(4) 2.988(3) 129(4) 2_546 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C4 C3 N2 -4.5(2) . . . . ?
N1 C4 C3 N5 117.4(2) . . . . ?
N1 C1 C2 N3 3.1(3) . . . . ?
N1 C1 C2 N4 113.2(2) . . . . ?
N3 C6 C5 N4 -3.8(2) . . . . ?
N3 C6 C5 N5 -123.9(2) . . . . ?
N2 C1 C2 N3 -107.0(2) . . . . ?
N2 C1 C2 N4 3.1(3) . . . . ?
N6 C4 C3 N2 -123.8(2) . . . . ?
N6 C4 C3 N5 -1.8(3) . . . . ?
N6 C6 C5 N4 118.4(2) . . . . ?
N6 C6 C5 N5 -1.7(3) . . . . ?
N7 N1 C4 N6 -128.1(2) . . . . ?
N7 N1 C4 C3 113.1(2) . . . . ?
N7 N1 C1 N2 -96.8(2) . . . . ?
N7 N1 C1 C2 144.7(2) . . . . ?
N9 N3 C6 N6 58.7(3) . . . . ?
N9 N3 C6 C5 176.3(2) . . . . ?
N9 N3 C2 N4 168.7(2) . . . . ?
N9 N3 C2 C1 -75.4(3) . . . . ?
N8 N2 C3 N5 53.0(3) . . . . ?
N8 N2 C3 C4 171.5(2) . . . . ?
N8 N2 C1 N1 175.2(2) . . . . ?
N8 N2 C1 C2 -69.7(3) . . . . ?
N10 N4 C5 N5 -133.8(2) . . . . ?
N10 N4 C5 C6 107.0(2) . . . . ?
N10 N4 C2 N3 -92.0(2) . . . . ?
N10 N4 C2 C1 149.0(2) . . . . ?
N13 C10 C9 N14 0.4(2) . . . . ?
N13 C10 C9 N15 -120.2(2) . . . . ?
N13 C8 C7 N11 1.4(3) . . . . ?
N13 C8 C7 N12 -109.8(2) . . . . ?
N14 C8 C7 N11 112.5(2) . . . . ?
N14 C8 C7 N12 1.4(3) . . . . ?
N11 C12 C11 N12 -0.8(2) . . . . ?
N11 C12 C11 N15 119.1(2) . . . . ?
N16 C10 C9 N14 120.6(2) . . . . ?
N16 C10 C9 N15 0.1(3) . . . . ?
N16 C12 C11 N12 -120.9(2) . . . . ?
N16 C12 C11 N15 -1.1(3) . . . . ?
N19 N13 C10 N16 115.7(2) . . . . ?
N19 N13 C10 C9 -126.1(2) . . . . ?
N19 N13 C8 N14 112.7(2) . . . . ?
N19 N13 C8 C7 -132.6(2) . . . . ?
N20 N14 C9 N15 -125.6(2) . . . . ?
N20 N14 C9 C10 116.2(2) . . . . ?
N20 N14 C8 N13 -103.5(2) . . . . ?
N20 N14 C8 C7 141.4(2) . . . . ?
N18 N12 C7 N11 116.9(2) . . . . ?
N18 N12 C7 C8 -128.5(2) . . . . ?
N18 N12 C11 N15 112.7(3) . . . . ?
N18 N12 C11 C12 -129.6(2) . . . . ?
N17 N11 C7 N12 -104.6(2) . . . . ?
N17 N11 C7 C8 139.6(2) . . . . ?
N17 N11 C12 N16 -123.3(2) . . . . ?
N17 N11 C12 C11 118.0(2) . . . . ?
C4 N1 N7 O1 39.6(3) . . . . ?
C4 N1 N7 O2 -145.0(2) . . . . ?
C4 N1 C1 N2 36.5(2) . . . . ?
C4 N1 C1 C2 -82.0(2) . . . . ?
C4 N6 C6 N3 57.3(3) . . . . ?
C4 N6 C6 C5 -54.7(3) . . . . ?
C4 N6 C13 N16 64.6(3) . . . . ?
C6 N3 N9 O5 19.7(3) . . . . ?
C6 N3 N9 O6 -162.9(2) . . . . ?
C6 N3 C2 N4 -43.3(2) . . . . ?
C6 N3 C2 C1 72.7(3) . . . . ?
C6 N6 C4 N1 -59.1(3) . . . . ?
C6 N6 C4 C3 56.7(3) . . . . ?
C6 N6 C13 N16 -152.3(2) . . . . ?
C3 N2 N8 O3 -155.3(2) . . . . ?
C3 N2 N8 O4 26.6(3) . . . . ?
C3 N2 C1 N1 -41.2(2) . . . . ?
C3 N2 C1 C2 73.9(3) . . . . ?
C3 N5 C5 N4 -59.9(3) . . . . ?
C3 N5 C5 C6 56.2(3) . . . . ?
C5 N4 N10 O7 -149.0(2) . . . . ?
C5 N4 N10 O8 35.6(3) . . . . ?
C5 N4 C2 N3 38.1(2) . . . . ?
C5 N4 C2 C1 -81.0(2) . . . . ?
C5 N5 C3 N2 58.6(3) . . . . ?
C5 N5 C3 C4 -54.4(3) . . . . ?
C1 N1 N7 O1 168.7(2) . . . . ?
C1 N1 N7 O2 -15.8(3) . . . . ?
C1 N1 C4 N6 98.5(2) . . . . ?
C1 N1 C4 C3 -20.3(3) . . . . ?
C1 N2 N8 O3 -15.4(4) . . . . ?
C1 N2 N8 O4 166.5(2) . . . . ?
C1 N2 C3 N5 -90.2(3) . . . . ?
C1 N2 C3 C4 28.4(2) . . . . ?
C2 N3 N9 O5 164.3(2) . . . . ?
C2 N3 N9 O6 -18.3(3) . . . . ?
C2 N3 C6 N6 -88.4(2) . . . . ?
C2 N3 C6 C5 29.3(2) . . . . ?
C2 N4 N10 O7 -23.9(3) . . . . ?
C2 N4 N10 O8 160.7(2) . . . . ?
C2 N4 C5 N5 97.4(2) . . . . ?
C2 N4 C5 C6 -21.8(2) . . . . ?
C13 N6 C4 N1 85.6(3) . . . . ?
C13 N6 C4 C3 -158.6(2) . . . . ?
C13 N6 C6 N3 -86.3(3) . . . . ?
C13 N6 C6 C5 161.7(2) . . . . ?
C13 N16 C10 N13 -77.0(3) . . . . ?
C13 N16 C10 C9 168.3(2) . . . . ?
C13 N16 C12 N11 76.9(3) . . . . ?
C13 N16 C12 C11 -167.35(19) . . . . ?
C10 N13 N19 O13 -23.3(3) . . . . ?
C10 N13 N19 O14 159.9(2) . . . . ?
C10 N13 C8 N14 -34.8(3) . . . . ?
C10 N13 C8 C7 79.9(2) . . . . ?
C10 N16 C13 N6 -159.4(2) . . . . ?
C10 N16 C12 N11 -57.9(3) . . . . ?
C10 N16 C12 C11 57.8(3) . . . . ?
C9 N14 N20 O16 29.6(3) . . . . ?
C9 N14 N20 O15 -153.8(2) . . . . ?
C9 N14 C8 N13 34.7(2) . . . . ?
C9 N14 C8 C7 -80.5(2) . . . . ?
C9 N15 C11 N12 56.6(3) . . . . ?
C9 N15 C11 C12 -56.8(3) . . . . ?
C8 N13 N19 O13 -167.0(2) . . . . ?
C8 N13 N19 O14 16.2(3) . . . . ?
C8 N13 C10 N16 -97.0(2) . . . . ?
C8 N13 C10 C9 21.2(3) . . . . ?
C8 N14 N20 O16 163.3(2) . . . . ?
C8 N14 N20 O15 -20.0(3) . . . . ?
C8 N14 C9 N15 96.6(2) . . . . ?
C8 N14 C9 C10 -21.7(3) . . . . ?
C7 N11 N17 O10 -21.1(3) . . . . ?
C7 N11 N17 O9 163.3(2) . . . . ?
C7 N11 C12 N16 98.2(2) . . . . ?
C7 N11 C12 C11 -20.5(3) . . . . ?
C7 N12 N18 O11 16.2(4) . . . . ?
C7 N12 N18 O12 -166.4(2) . . . . ?
C7 N12 C11 N15 -95.5(3) . . . . ?
C7 N12 C11 C12 22.1(3) . . . . ?
C12 N11 N17 O10 -155.3(2) . . . . ?
C12 N11 N17 O9 29.1(3) . . . . ?
C12 N11 C7 N12 33.8(3) . . . . ?
C12 N11 C7 C8 -82.0(2) . . . . ?
C12 N16 C13 N6 67.0(3) . . . . ?
C12 N16 C10 N13 57.6(3) . . . . ?
C12 N16 C10 C9 -57.1(3) . . . . ?
C11 N12 N18 O11 164.7(2) . . . . ?
C11 N12 N18 O12 -17.9(4) . . . . ?
C11 N12 C7 N11 -35.0(3) . . . . ?
C11 N12 C7 C8 79.5(2) . . . . ?
C11 N15 C9 N14 -57.2(3) . . . . ?
C11 N15 C9 C10 57.4(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.293
_oxdiff_exptl_absorpt_empirical_full_min 0.655
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 2208927'
loop_
_audit_author_name
_audit_author_address
'Aida I Samigullina'
;N D Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences 
Russia
;
_audit_update_record             
;
2022-09-22 deposited with the CCDC.	2022-12-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_9                   
;
PROBLEM: Short Inter D...A Contact  O7       ..N21      .       2.77 Ang.  
RESPONSE: This is due to the unique chemical structure
 of this particular energetic compound.
;
# end Validation Reply Form
_audit_creation_date             2022-05-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H18 N26 O16, C2 H3 N'
_chemical_formula_sum            'C17 H21 N27 O16'
_chemical_formula_weight         859.61
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     SNV7039
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   8.0773(2)
_cell_length_b                   24.2356(5)
_cell_length_c                   31.9915(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6262.6(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    18398
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      78.7930
_cell_measurement_theta_min      3.9000
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.415
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            42994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.199
_diffrn_reflns_theta_min         3.648
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00 -22.00   0.50   12.00    --  -48.76  66.00 149.00   86
  2  ω    -63.00 -38.00   0.50   35.00    --  -90.00  55.00 -37.00   50
  3  ω     40.00  65.00   0.50   35.00    --  111.50 -66.00  14.00   50
  4  ω     41.00  77.00   0.50   35.00    --  111.50-122.00 -53.00   72
  5  ω     65.00  97.00   0.50   35.00    --  111.50-151.00 145.00   64
  6  ω    131.00 158.00   0.50   35.00    --  111.50  66.00 149.00   54
  7  ω    114.00 139.00   0.50   35.00    --  111.50  55.00 -37.00   50
  8  ω   -114.00 -83.00   0.50   12.00    --  -48.76-125.00 120.00   62
  9  ω   -121.00 -39.00   0.50   12.00    --  -48.76 -38.00  30.00  164
 10  ω   -112.00 -74.00   0.50   12.00    --  -48.76-125.00  90.00   76
 11  ω    -51.00 -26.00   0.50   35.00    --  -90.00  45.00-120.00   50
 12  ω     41.00  89.00   0.50   35.00    --  111.50 -78.00 167.15   96
 13  ω    140.00 175.00   0.50   35.00    --  111.50  30.00  60.00   70
 14  ω     54.00 103.00   0.50   35.00    --  111.50 -95.00 -60.00   98
 15  ω    124.00 155.00   0.50   35.00    --  111.50  77.00  60.00   62
 16  ω    143.00 178.00   0.50   35.00    --  111.50  29.00 -48.34   70
 17  ω    100.00 157.00   0.50   35.00    --  111.50  52.00  89.77  114
 18  ω     43.00  68.00   0.50   35.00    --  111.50 -95.00 -90.00   50
 19  ω     43.00  72.00   0.50   35.00    --  111.50 -78.00   9.92   58
 20  ω     48.00  84.00   0.50   35.00    --  111.50-125.00-120.00   72
 21  ω    135.00 161.00   0.50   35.00    --  111.50  30.00 -30.00   52
 22  ω     79.00 105.00   0.50   35.00    --  111.50 -77.00  60.00   52
 23  ω     40.00  74.00   0.50   35.00    --  111.50 -77.00  60.00   68
 24  ω     40.00  96.00   0.50   35.00    --  111.50 -95.00 150.00  112
 25  ω    101.00 129.00   0.50   35.00    --  111.50  29.00 -48.34   56
 26  ω    108.00 134.00   0.50   35.00    --  111.50  30.00 -30.00   52
 27  ω     40.00  66.00   0.50   35.00    --  111.50 -61.00  30.00   52
 28  ω     44.00  69.00   0.50   35.00    --  111.50 -61.00-150.00   50
 29  ω     45.00  71.00   0.50   35.00    --  111.50 -77.00-120.00   52
 30  ω     74.00  99.00   0.50   35.00    --  111.50 -95.00 -30.00   50
 31  ω    102.00 128.00   0.50   35.00    --  111.50  45.00 -30.00   52
 32  ω     98.00 124.00   0.50   35.00    --  111.50 125.00  60.00   52
 33  ω     57.00  83.00   0.50   35.00    --  111.50 -95.00   0.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0417331000
_diffrn_orient_matrix_UB_12      -0.0617038000
_diffrn_orient_matrix_UB_13      -0.0049690000
_diffrn_orient_matrix_UB_21      0.1192379000
_diffrn_orient_matrix_UB_22      0.0139742000
_diffrn_orient_matrix_UB_23      -0.0360659000
_diffrn_orient_matrix_UB_31      0.1428963000
_diffrn_orient_matrix_UB_32      0.0063314000
_diffrn_orient_matrix_UB_33      0.0315025000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5719
_reflns_number_total             6726
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         6726
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0591
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0928P)²+5.2137P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1639
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10),
 C11(H11), C12(H12), C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C15(H15A,H15B)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.2966(2) 0.86124(6) 0.32361(5) 0.0292(4) Uani 1 1 d . . . . .
O2 O 0.5594(2) 0.84565(7) 0.33525(6) 0.0306(4) Uani 1 1 d . . . . .
O3 O 0.1960(3) 0.77145(7) 0.24489(6) 0.0390(4) Uani 1 1 d . . . . .
O4 O 0.3822(3) 0.71050(8) 0.22791(6) 0.0404(5) Uani 1 1 d . . . . .
O5 O 0.2487(2) 0.72206(9) 0.47048(6) 0.0389(4) Uani 1 1 d . . . . .
O6 O 0.0157(2) 0.73965(8) 0.43904(6) 0.0381(4) Uani 1 1 d . . . . .
O7 O 0.0476(2) 0.57708(7) 0.37190(6) 0.0314(4) Uani 1 1 d . . . . .
O8 O -0.1101(2) 0.64969(8) 0.37609(6) 0.0370(4) Uani 1 1 d . . . . .
O9 O 0.2993(2) 0.44665(7) 0.25700(5) 0.0278(4) Uani 1 1 d . . . . .
O10 O 0.4833(2) 0.38100(7) 0.25826(5) 0.0308(4) Uani 1 1 d . . . . .
O11 O 0.8604(2) 0.59334(6) 0.29267(5) 0.0306(4) Uani 1 1 d . . . . .
O12 O 1.0091(2) 0.51817(7) 0.29009(5) 0.0296(4) Uani 1 1 d . . . . .
O13 O 0.3948(2) 0.35265(7) 0.40137(6) 0.0347(4) Uani 1 1 d . . . . .
O14 O 0.5743(2) 0.32149(7) 0.35608(6) 0.0316(4) Uani 1 1 d . . . . .
O15 O 1.0451(2) 0.44524(9) 0.38862(6) 0.0406(5) Uani 1 1 d . . . . .
O16 O 0.9238(2) 0.48973(8) 0.43928(5) 0.0346(4) Uani 1 1 d . . . . .
N1 N 0.3812(2) 0.77653(7) 0.34019(6) 0.0248(4) Uani 1 1 d . . . . .
N2 N 0.2881(2) 0.71203(7) 0.29401(6) 0.0254(4) Uani 1 1 d . . . . .
N3 N 0.2468(2) 0.72604(8) 0.40083(6) 0.0248(4) Uani 1 1 d . . . . .
N4 N 0.1548(2) 0.65915(7) 0.35539(6) 0.0234(4) Uani 1 1 d . . . . .
N5 N 0.5360(2) 0.71135(8) 0.38189(6) 0.0240(4) Uani 1 1 d . . . . .
N6 N 0.4305(2) 0.63811(7) 0.33106(6) 0.0230(4) Uani 1 1 d . . . . .
N7 N 0.4153(2) 0.83137(7) 0.33179(6) 0.0242(4) Uani 1 1 d . . . . .
N8 N 0.2919(3) 0.73376(8) 0.25305(7) 0.0315(5) Uani 1 1 d . . . . .
N9 N 0.1628(3) 0.72841(8) 0.43943(7) 0.0301(4) Uani 1 1 d . . . . .
N10 N 0.0224(2) 0.62711(8) 0.36964(7) 0.0271(4) Uani 1 1 d . . . . .
N11 N 0.5599(3) 0.79416(9) 0.42382(7) 0.0335(5) Uani 1 1 d . . . . .
N12 N 0.6617(3) 0.82969(9) 0.43454(7) 0.0338(5) Uani 1 1 d . . . . .
N13 N 0.7419(3) 0.86537(10) 0.44485(8) 0.0426(6) Uani 1 1 d . . . . .
N14 N 0.5122(2) 0.45419(7) 0.30088(6) 0.0202(4) Uani 1 1 d . . . . .
N15 N 0.7560(2) 0.51618(7) 0.31872(6) 0.0202(4) Uani 1 1 d . . . . .
N16 N 0.5416(2) 0.41159(7) 0.36371(6) 0.0219(4) Uani 1 1 d . . . . .
N17 N 0.7846(2) 0.47223(8) 0.38111(6) 0.0224(4) Uani 1 1 d . . . . .
N18 N 0.5047(2) 0.49613(8) 0.40348(6) 0.0243(4) Uani 1 1 d . . . . .
N19 N 0.4746(2) 0.54371(7) 0.33385(6) 0.0212(4) Uani 1 1 d . . . . .
N20 N 0.4243(2) 0.42449(8) 0.27051(6) 0.0229(4) Uani 1 1 d . . . . .
N21 N 0.8849(2) 0.54409(8) 0.30001(6) 0.0247(4) Uani 1 1 d . . . . .
N22 N 0.4986(2) 0.35867(8) 0.37388(6) 0.0266(4) Uani 1 1 d . . . . .
N23 N 0.9281(2) 0.46990(8) 0.40406(7) 0.0281(4) Uani 1 1 d . . . . .
N24 N 0.3228(3) 0.48679(9) 0.46267(7) 0.0335(5) Uani 1 1 d . . . . .
N25 N 0.2714(3) 0.53502(10) 0.45979(7) 0.0336(5) Uani 1 1 d . . . . .
N26 N 0.2094(3) 0.57754(11) 0.45825(8) 0.0426(6) Uani 1 1 d . . . . .
N27 N 0.3944(3) 0.38821(10) 0.53832(8) 0.0437(6) Uani 1 1 d . . . . .
C1 C 0.2297(3) 0.75099(9) 0.32594(7) 0.0250(5) Uani 1 1 d . . . . .
H1 H 0.152336 0.778870 0.313707 0.030 Uiso 1 1 calc R U . . .
C2 C 0.1456(3) 0.71859(9) 0.36348(8) 0.0250(5) Uani 1 1 d . . . . .
H2 H 0.028953 0.730950 0.368155 0.030 Uiso 1 1 calc R U . . .
C3 C 0.4502(3) 0.68939(9) 0.30989(7) 0.0245(4) Uani 1 1 d . . . . .
H3 H 0.529951 0.685104 0.286201 0.029 Uiso 1 1 calc R U . . .
C4 C 0.3254(3) 0.64105(9) 0.36697(7) 0.0236(4) Uani 1 1 d . . . . .
H4 H 0.321243 0.604417 0.381311 0.028 Uiso 1 1 calc R U . . .
C5 C 0.5149(3) 0.73480(9) 0.34132(8) 0.0241(4) Uani 1 1 d . . . . .
H5 H 0.621344 0.751022 0.331133 0.029 Uiso 1 1 calc R U . . .
C6 C 0.3886(3) 0.68659(9) 0.39805(7) 0.0237(4) Uani 1 1 d . . . . .
H6 H 0.410991 0.669946 0.426087 0.028 Uiso 1 1 calc R U . . .
C7 C 0.6386(3) 0.74114(9) 0.41066(8) 0.0285(5) Uani 1 1 d . . . . .
H7A H 0.746645 0.749016 0.397335 0.034 Uiso 1 1 calc R U . . .
H7B H 0.659177 0.718033 0.435638 0.034 Uiso 1 1 calc R U . . .
C8 C 0.7858(3) 0.46183(8) 0.33643(7) 0.0212(4) Uani 1 1 d . . . . .
H8 H 0.893188 0.445732 0.326797 0.025 Uiso 1 1 calc R U . . .
C9 C 0.6329(3) 0.42321(8) 0.32548(7) 0.0207(4) Uani 1 1 d . . . . .
H9 H 0.668451 0.388629 0.310994 0.025 Uiso 1 1 calc R U . . .
C10 C 0.6423(3) 0.54656(8) 0.34727(7) 0.0209(4) Uani 1 1 d . . . . .
H10 H 0.677868 0.585950 0.349748 0.025 Uiso 1 1 calc R U . . .
C11 C 0.6631(3) 0.51660(9) 0.39015(7) 0.0228(4) Uani 1 1 d . . . . .
H11 H 0.708978 0.542638 0.411457 0.027 Uiso 1 1 calc R U . . .
C12 C 0.4122(3) 0.48873(8) 0.33032(7) 0.0214(4) Uani 1 1 d . . . . .
H12 H 0.293429 0.489271 0.321533 0.026 Uiso 1 1 calc R U . . .
C13 C 0.4313(3) 0.45888(9) 0.37363(7) 0.0227(4) Uani 1 1 d . . . . .
H13 H 0.321454 0.445474 0.383862 0.027 Uiso 1 1 calc R U . . .
C14 C 0.4922(3) 0.47931(10) 0.44669(7) 0.0287(5) Uani 1 1 d . . . . .
H14A H 0.570070 0.501367 0.463786 0.034 Uiso 1 1 calc R U . . .
H14B H 0.524126 0.440006 0.449230 0.034 Uiso 1 1 calc R U . . .
C15 C 0.4177(3) 0.58741(9) 0.30651(7) 0.0234(4) Uani 1 1 d . . . . .
H15A H 0.301690 0.580862 0.297822 0.028 Uiso 1 1 calc R U . . .
H15B H 0.487907 0.589669 0.281203 0.028 Uiso 1 1 calc R U . . .
C16 C 0.2857(4) 0.37944(11) 0.51656(9) 0.0360(6) Uani 1 1 d . . . . .
C17 C 0.1468(4) 0.36865(15) 0.48925(10) 0.0481(7) Uani 1 1 d . . . . .
H17A H 0.097900 0.332850 0.496338 0.072 Uiso 1 1 calc R U . . .
H17B H 0.184871 0.368065 0.460165 0.072 Uiso 1 1 calc R U . . .
H17C H 0.063616 0.397712 0.492733 0.072 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 N7 1.229(3) . ?
O2 N7 1.219(3) . ?
O3 N8 1.226(3) . ?
O4 N8 1.223(3) . ?
O5 N9 1.221(3) . ?
O6 N9 1.219(3) . ?
O7 N10 1.232(3) . ?
O8 N10 1.220(3) . ?
O9 N20 1.223(3) . ?
O10 N20 1.221(3) . ?
O11 N21 1.232(3) . ?
O12 N21 1.226(3) . ?
O13 N22 1.224(3) . ?
O14 N22 1.229(3) . ?
O15 N23 1.223(3) . ?
O16 N23 1.225(3) . ?
N1 N7 1.383(2) . ?
N1 C1 1.445(3) . ?
N1 C5 1.480(3) . ?
N2 N8 1.413(3) . ?
N2 C1 1.469(3) . ?
N2 C3 1.508(3) . ?
N3 N9 1.410(3) . ?
N3 C2 1.459(3) . ?
N3 C6 1.495(3) . ?
N4 N10 1.397(3) . ?
N4 C2 1.466(3) . ?
N4 C4 1.493(3) . ?
N5 C5 1.427(3) . ?
N5 C6 1.430(3) . ?
N5 C7 1.434(3) . ?
N6 C3 1.424(3) . ?
N6 C4 1.430(3) . ?
N6 C15 1.462(3) . ?
N11 N12 1.239(3) . ?
N11 C7 1.494(3) . ?
N12 N13 1.130(3) . ?
N14 N20 1.402(3) . ?
N14 C9 1.460(3) . ?
N14 C12 1.497(3) . ?
N15 N21 1.378(3) . ?
N15 C8 1.454(3) . ?
N15 C10 1.490(3) . ?
N16 N22 1.368(3) . ?
N16 C9 1.456(3) . ?
N16 C13 1.486(3) . ?
N17 N23 1.373(3) . ?
N17 C8 1.452(3) . ?
N17 C11 1.484(3) . ?
N18 C11 1.437(3) . ?
N18 C13 1.442(3) . ?
N18 C14 1.445(3) . ?
N19 C10 1.423(3) . ?
N19 C12 1.429(3) . ?
N19 C15 1.448(3) . ?
N24 N25 1.244(3) . ?
N24 C14 1.472(3) . ?
N25 N26 1.147(3) . ?
N27 C16 1.141(4) . ?
C1 H1 1.0000 . ?
C1 C2 1.587(3) . ?
C2 H2 1.0000 . ?
C3 H3 1.0000 . ?
C3 C5 1.580(3) . ?
C4 H4 1.0000 . ?
C4 C6 1.571(3) . ?
C5 H5 1.0000 . ?
C6 H6 1.0000 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8 1.0000 . ?
C8 C9 1.588(3) . ?
C9 H9 1.0000 . ?
C10 H10 1.0000 . ?
C10 C11 1.561(3) . ?
C11 H11 1.0000 . ?
C12 H12 1.0000 . ?
C12 C13 1.571(3) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.445(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 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
N7 N1 C1 121.25(18) . . ?
N7 N1 C5 121.07(18) . . ?
C1 N1 C5 109.45(17) . . ?
N8 N2 C1 114.36(17) . . ?
N8 N2 C3 115.43(19) . . ?
C1 N2 C3 106.18(17) . . ?
N9 N3 C2 116.93(18) . . ?
N9 N3 C6 116.53(18) . . ?
C2 N3 C6 107.55(17) . . ?
N10 N4 C2 116.76(18) . . ?
N10 N4 C4 117.50(17) . . ?
C2 N4 C4 106.95(17) . . ?
C5 N5 C6 113.38(18) . . ?
C5 N5 C7 116.88(18) . . ?
C6 N5 C7 117.42(19) . . ?
C3 N6 C4 113.88(17) . . ?
C3 N6 C15 119.07(18) . . ?
C4 N6 C15 115.56(18) . . ?
O1 N7 N1 116.86(18) . . ?
O2 N7 O1 126.63(19) . . ?
O2 N7 N1 116.42(18) . . ?
O3 N8 N2 117.5(2) . . ?
O4 N8 O3 125.5(2) . . ?
O4 N8 N2 116.8(2) . . ?
O5 N9 N3 115.7(2) . . ?
O6 N9 O5 126.1(2) . . ?
O6 N9 N3 118.0(2) . . ?
O7 N10 N4 116.11(19) . . ?
O8 N10 O7 125.2(2) . . ?
O8 N10 N4 118.49(19) . . ?
N12 N11 C7 113.2(2) . . ?
N13 N12 N11 173.4(3) . . ?
N20 N14 C9 116.58(16) . . ?
N20 N14 C12 116.74(17) . . ?
C9 N14 C12 107.97(16) . . ?
N21 N15 C8 119.28(17) . . ?
N21 N15 C10 119.29(16) . . ?
C8 N15 C10 108.10(17) . . ?
N22 N16 C9 120.66(18) . . ?
N22 N16 C13 121.36(18) . . ?
C9 N16 C13 109.51(16) . . ?
N23 N17 C8 120.93(18) . . ?
N23 N17 C11 118.91(18) . . ?
C8 N17 C11 108.79(17) . . ?
C11 N18 C13 112.68(18) . . ?
C11 N18 C14 116.31(19) . . ?
C13 N18 C14 115.37(19) . . ?
C10 N19 C12 113.87(17) . . ?
C10 N19 C15 116.66(17) . . ?
C12 N19 C15 121.49(18) . . ?
O9 N20 N14 115.95(17) . . ?
O10 N20 O9 125.98(19) . . ?
O10 N20 N14 117.92(18) . . ?
O11 N21 N15 115.91(19) . . ?
O12 N21 O11 125.33(19) . . ?
O12 N21 N15 118.64(18) . . ?
O13 N22 O14 125.9(2) . . ?
O13 N22 N16 117.16(19) . . ?
O14 N22 N16 116.81(19) . . ?
O15 N23 O16 125.8(2) . . ?
O15 N23 N17 117.2(2) . . ?
O16 N23 N17 116.9(2) . . ?
N25 N24 C14 113.6(2) . . ?
N26 N25 N24 173.4(3) . . ?
N1 C1 N2 102.86(18) . . ?
N1 C1 H1 111.3 . . ?
N1 C1 C2 109.60(19) . . ?
N2 C1 H1 111.3 . . ?
N2 C1 C2 110.22(17) . . ?
C2 C1 H1 111.3 . . ?
N3 C2 N4 103.76(17) . . ?
N3 C2 C1 108.59(18) . . ?
N3 C2 H2 111.6 . . ?
N4 C2 C1 109.34(18) . . ?
N4 C2 H2 111.6 . . ?
C1 C2 H2 111.6 . . ?
N2 C3 H3 110.0 . . ?
N2 C3 C5 104.37(17) . . ?
N6 C3 N2 112.36(18) . . ?
N6 C3 H3 110.0 . . ?
N6 C3 C5 110.02(19) . . ?
C5 C3 H3 110.0 . . ?
N4 C4 H4 110.1 . . ?
N4 C4 C6 104.52(17) . . ?
N6 C4 N4 111.31(18) . . ?
N6 C4 H4 110.1 . . ?
N6 C4 C6 110.51(18) . . ?
C6 C4 H4 110.1 . . ?
N1 C5 C3 102.65(17) . . ?
N1 C5 H5 110.5 . . ?
N5 C5 N1 112.43(19) . . ?
N5 C5 C3 109.93(17) . . ?
N5 C5 H5 110.5 . . ?
C3 C5 H5 110.5 . . ?
N3 C6 C4 103.76(17) . . ?
N3 C6 H6 110.1 . . ?
N5 C6 N3 113.02(18) . . ?
N5 C6 C4 109.68(18) . . ?
N5 C6 H6 110.1 . . ?
C4 C6 H6 110.1 . . ?
N5 C7 N11 111.60(19) . . ?
N5 C7 H7A 109.3 . . ?
N5 C7 H7B 109.3 . . ?
N11 C7 H7A 109.3 . . ?
N11 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
N15 C8 H8 112.1 . . ?
N15 C8 C9 108.63(17) . . ?
N17 C8 N15 103.02(17) . . ?
N17 C8 H8 112.1 . . ?
N17 C8 C9 108.32(17) . . ?
C9 C8 H8 112.1 . . ?
N14 C9 C8 109.55(16) . . ?
N14 C9 H9 111.9 . . ?
N16 C9 N14 102.36(16) . . ?
N16 C9 C8 108.83(17) . . ?
N16 C9 H9 111.9 . . ?
C8 C9 H9 111.9 . . ?
N15 C10 H10 110.1 . . ?
N15 C10 C11 104.04(16) . . ?
N19 C10 N15 112.21(17) . . ?
N19 C10 H10 110.1 . . ?
N19 C10 C11 110.18(17) . . ?
C11 C10 H10 110.1 . . ?
N17 C11 C10 103.70(16) . . ?
N17 C11 H11 110.2 . . ?
N18 C11 N17 113.35(18) . . ?
N18 C11 C10 109.00(17) . . ?
N18 C11 H11 110.2 . . ?
C10 C11 H11 110.2 . . ?
N14 C12 H12 110.4 . . ?
N14 C12 C13 104.15(16) . . ?
N19 C12 N14 112.40(17) . . ?
N19 C12 H12 110.4 . . ?
N19 C12 C13 108.99(17) . . ?
C13 C12 H12 110.4 . . ?
N16 C13 C12 103.05(17) . . ?
N16 C13 H13 110.6 . . ?
N18 C13 N16 112.22(18) . . ?
N18 C13 C12 109.64(17) . . ?
N18 C13 H13 110.6 . . ?
C12 C13 H13 110.6 . . ?
N18 C14 N24 111.2(2) . . ?
N18 C14 H14A 109.4 . . ?
N18 C14 H14B 109.4 . . ?
N24 C14 H14A 109.4 . . ?
N24 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
N6 C15 H15A 110.6 . . ?
N6 C15 H15B 110.6 . . ?
N19 C15 N6 105.53(17) . . ?
N19 C15 H15A 110.6 . . ?
N19 C15 H15B 110.6 . . ?
H15A C15 H15B 108.8 . . ?
N27 C16 C17 179.4(4) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 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
N1 C1 C2 N3 1.3(2) . . . . ?
N1 C1 C2 N4 -111.3(2) . . . . ?
N2 C1 C2 N3 113.80(19) . . . . ?
N2 C1 C2 N4 1.2(2) . . . . ?
N2 C3 C5 N1 1.3(2) . . . . ?
N2 C3 C5 N5 121.09(18) . . . . ?
N4 C4 C6 N3 -0.1(2) . . . . ?
N4 C4 C6 N5 -121.11(19) . . . . ?
N6 C3 C5 N1 -119.49(19) . . . . ?
N6 C3 C5 N5 0.3(2) . . . . ?
N6 C4 C6 N3 119.74(19) . . . . ?
N6 C4 C6 N5 -1.3(2) . . . . ?
N7 N1 C1 N2 111.3(2) . . . . ?
N7 N1 C1 C2 -131.4(2) . . . . ?
N7 N1 C5 N5 115.3(2) . . . . ?
N7 N1 C5 C3 -126.6(2) . . . . ?
N8 N2 C1 N1 -91.5(2) . . . . ?
N8 N2 C1 C2 151.73(19) . . . . ?
N8 N2 C3 N6 -136.45(19) . . . . ?
N8 N2 C3 C5 104.4(2) . . . . ?
N9 N3 C2 N4 -97.4(2) . . . . ?
N9 N3 C2 C1 146.39(18) . . . . ?
N9 N3 C6 N5 -129.6(2) . . . . ?
N9 N3 C6 C4 111.6(2) . . . . ?
N10 N4 C2 N3 98.2(2) . . . . ?
N10 N4 C2 C1 -146.14(19) . . . . ?
N10 N4 C4 N6 129.03(19) . . . . ?
N10 N4 C4 C6 -111.7(2) . . . . ?
N12 N11 C7 N5 -153.7(2) . . . . ?
N14 C12 C13 N16 0.8(2) . . . . ?
N14 C12 C13 N18 120.47(18) . . . . ?
N15 C8 C9 N14 0.6(2) . . . . ?
N15 C8 C9 N16 -110.62(19) . . . . ?
N15 C10 C11 N17 -0.6(2) . . . . ?
N15 C10 C11 N18 -121.64(18) . . . . ?
N17 C8 C9 N14 111.78(19) . . . . ?
N17 C8 C9 N16 0.6(2) . . . . ?
N19 C10 C11 N17 119.84(18) . . . . ?
N19 C10 C11 N18 -1.2(2) . . . . ?
N19 C12 C13 N16 -119.35(18) . . . . ?
N19 C12 C13 N18 0.3(2) . . . . ?
N20 N14 C9 N16 -98.59(19) . . . . ?
N20 N14 C9 C8 146.04(18) . . . . ?
N20 N14 C12 N19 -130.88(19) . . . . ?
N20 N14 C12 C13 111.29(19) . . . . ?
N21 N15 C8 N17 106.2(2) . . . . ?
N21 N15 C8 C9 -139.06(18) . . . . ?
N21 N15 C10 N19 121.9(2) . . . . ?
N21 N15 C10 C11 -118.99(19) . . . . ?
N22 N16 C9 N14 113.3(2) . . . . ?
N22 N16 C9 C8 -130.8(2) . . . . ?
N22 N16 C13 N18 115.2(2) . . . . ?
N22 N16 C13 C12 -126.9(2) . . . . ?
N23 N17 C8 N15 -108.8(2) . . . . ?
N23 N17 C8 C9 136.24(19) . . . . ?
N23 N17 C11 N18 -118.8(2) . . . . ?
N23 N17 C11 C10 123.2(2) . . . . ?
N25 N24 C14 N18 -57.6(3) . . . . ?
C1 N1 N7 O1 21.5(3) . . . . ?
C1 N1 N7 O2 -161.9(2) . . . . ?
C1 N1 C5 N5 -95.9(2) . . . . ?
C1 N1 C5 C3 22.1(2) . . . . ?
C1 N2 N8 O3 -26.3(3) . . . . ?
C1 N2 N8 O4 159.0(2) . . . . ?
C1 N2 C3 N6 95.7(2) . . . . ?
C1 N2 C3 C5 -23.5(2) . . . . ?
C2 N3 N9 O5 164.0(2) . . . . ?
C2 N3 N9 O6 -20.2(3) . . . . ?
C2 N3 C6 N5 96.8(2) . . . . ?
C2 N3 C6 C4 -21.9(2) . . . . ?
C2 N4 N10 O7 -163.2(2) . . . . ?
C2 N4 N10 O8 21.6(3) . . . . ?
C2 N4 C4 N6 -97.4(2) . . . . ?
C2 N4 C4 C6 21.9(2) . . . . ?
C3 N2 N8 O3 -149.9(2) . . . . ?
C3 N2 N8 O4 35.3(3) . . . . ?
C3 N2 C1 N1 37.0(2) . . . . ?
C3 N2 C1 C2 -79.8(2) . . . . ?
C3 N6 C4 N4 60.6(2) . . . . ?
C3 N6 C4 C6 -55.1(2) . . . . ?
C3 N6 C15 N19 154.42(19) . . . . ?
C4 N4 N10 O7 -34.1(3) . . . . ?
C4 N4 N10 O8 150.7(2) . . . . ?
C4 N4 C2 N3 -35.8(2) . . . . ?
C4 N4 C2 C1 79.9(2) . . . . ?
C4 N6 C3 N2 -60.5(3) . . . . ?
C4 N6 C3 C5 55.4(2) . . . . ?
C4 N6 C15 N19 -64.4(2) . . . . ?
C5 N1 N7 O1 166.6(2) . . . . ?
C5 N1 N7 O2 -16.8(3) . . . . ?
C5 N1 C1 N2 -37.4(2) . . . . ?
C5 N1 C1 C2 79.9(2) . . . . ?
C5 N5 C6 N3 -58.0(2) . . . . ?
C5 N5 C6 C4 57.2(2) . . . . ?
C5 N5 C7 N11 68.5(3) . . . . ?
C6 N3 N9 O5 34.9(3) . . . . ?
C6 N3 N9 O6 -149.3(2) . . . . ?
C6 N3 C2 N4 36.0(2) . . . . ?
C6 N3 C2 C1 -80.3(2) . . . . ?
C6 N5 C5 N1 56.9(2) . . . . ?
C6 N5 C5 C3 -56.8(2) . . . . ?
C6 N5 C7 N11 -71.3(3) . . . . ?
C7 N5 C5 N1 -84.5(2) . . . . ?
C7 N5 C5 C3 161.82(18) . . . . ?
C7 N5 C6 N3 83.2(2) . . . . ?
C7 N5 C6 C4 -161.61(18) . . . . ?
C8 N15 N21 O11 -167.01(19) . . . . ?
C8 N15 N21 O12 16.7(3) . . . . ?
C8 N15 C10 N19 -97.4(2) . . . . ?
C8 N15 C10 C11 21.7(2) . . . . ?
C8 N17 N23 O15 -18.8(3) . . . . ?
C8 N17 N23 O16 165.68(19) . . . . ?
C8 N17 C11 N18 97.3(2) . . . . ?
C8 N17 C11 C10 -20.7(2) . . . . ?
C9 N14 N20 O9 163.65(18) . . . . ?
C9 N14 N20 O10 -20.5(3) . . . . ?
C9 N14 C12 N19 95.5(2) . . . . ?
C9 N14 C12 C13 -22.3(2) . . . . ?
C9 N16 N22 O13 -165.5(2) . . . . ?
C9 N16 N22 O14 18.1(3) . . . . ?
C9 N16 C13 N18 -96.6(2) . . . . ?
C9 N16 C13 C12 21.2(2) . . . . ?
C10 N15 N21 O11 -30.7(3) . . . . ?
C10 N15 N21 O12 153.02(19) . . . . ?
C10 N15 C8 N17 -34.5(2) . . . . ?
C10 N15 C8 C9 80.3(2) . . . . ?
C10 N19 C12 N14 -57.8(2) . . . . ?
C10 N19 C12 C13 57.2(2) . . . . ?
C10 N19 C15 N6 -63.1(2) . . . . ?
C11 N17 N23 O15 -158.2(2) . . . . ?
C11 N17 N23 O16 26.2(3) . . . . ?
C11 N17 C8 N15 34.3(2) . . . . ?
C11 N17 C8 C9 -80.7(2) . . . . ?
C11 N18 C13 N16 56.1(2) . . . . ?
C11 N18 C13 C12 -57.8(2) . . . . ?
C11 N18 C14 N24 150.6(2) . . . . ?
C12 N14 N20 O9 34.0(3) . . . . ?
C12 N14 N20 O10 -150.15(19) . . . . ?
C12 N14 C9 N16 35.1(2) . . . . ?
C12 N14 C9 C8 -80.2(2) . . . . ?
C12 N19 C10 N15 58.3(2) . . . . ?
C12 N19 C10 C11 -57.1(2) . . . . ?
C12 N19 C15 N6 149.96(19) . . . . ?
C13 N16 N22 O13 -20.9(3) . . . . ?
C13 N16 N22 O14 162.8(2) . . . . ?
C13 N16 C9 N14 -35.1(2) . . . . ?
C13 N16 C9 C8 80.8(2) . . . . ?
C13 N18 C11 N17 -56.8(2) . . . . ?
C13 N18 C11 C10 58.1(2) . . . . ?
C13 N18 C14 N24 -74.1(3) . . . . ?
C14 N18 C11 N17 79.7(2) . . . . ?
C14 N18 C11 C10 -165.42(18) . . . . ?
C14 N18 C13 N16 -80.8(2) . . . . ?
C14 N18 C13 C12 165.32(19) . . . . ?
C15 N6 C3 N2 81.4(2) . . . . ?
C15 N6 C3 C5 -162.82(18) . . . . ?
C15 N6 C4 N4 -82.6(2) . . . . ?
C15 N6 C4 C6 161.72(18) . . . . ?
C15 N19 C10 N15 -91.2(2) . . . . ?
C15 N19 C10 C11 153.41(18) . . . . ?
C15 N19 C12 N14 90.1(2) . . . . ?
C15 N19 C12 C13 -155.00(19) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.863
_oxdiff_exptl_absorpt_empirical_full_min 0.403
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 2208928'
loop_
_audit_author_name
_audit_author_address
'Aida I Samigullina'
;N D Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences 
Russia
;
_audit_update_record             
;
2022-09-22 deposited with the CCDC.	2022-12-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_7                   
;
PROBLEM: Short Inter D...A Contact  O6       ..O20      .       2.79 Ang.  
RESPONSE: These intermolecular interactions are expected for this structure.
;
_vrf_PLAT230_7                   
;
PROBLEM: Hirshfeld Test Diff for    O12      --N18      .        6.0 s.u.  
RESPONSE: These intermolecular interactions are expected for this structure.
;
# end Validation Reply Form
_audit_creation_date             2022-09-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C13 H14 N22 O18'
_chemical_formula_sum            'C13 H14 N22 O18'
_chemical_formula_weight         766.46
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     PGV2037
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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   21.46514(4)
_cell_length_b                   21.46514(4)
_cell_length_c                   26.19638(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     12070.04(7)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    62530
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.5950
_cell_measurement_theta_min      2.6430
_shelx_estimated_absorpt_T_max   0.885
_shelx_estimated_absorpt_T_min   0.741
_exptl_absorpt_coefficient_mu    1.386
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.58a (Rigaku Oxford Diffraction, 2022)
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   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6240
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.1300
0 0 -1 0.0986
0 -1 0 0.0494
0 1 0 0.0494
1 -1 0 0.0519
-1 1 0 0.0422
1 0 0 0.0522
-1 0 0 0.0444
1 1 0 0.0494
0 1 1 0.0715
-1 0 1 0.0914

_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
loop_
_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
-0.0000 -0.0002 0.9996 -0.0004 -0.0245 0.0534
0.0000 0.0002 -0.9996 0.0004 0.0245 -0.0534
-0.0003 -0.9997 0.0001 -0.0293 0.0596 0.0272
0.0003 0.9997 -0.0001 0.0293 -0.0596 -0.0272
0.9994 -0.9998 0.0001 -0.0948 0.0331 0.0145
-0.9994 0.9998 -0.0001 0.0948 -0.0331 -0.0145
0.9997 -0.0002 0.0001 -0.0655 -0.0265 -0.0126
-0.9997 0.0002 -0.0001 0.0655 0.0265 0.0126
1.0000 0.9995 -0.0000 -0.0362 -0.0861 -0.0398
0.0003 0.9995 0.9995 0.0289 -0.0841 0.0263
-0.9997 -0.0001 0.9995 0.0650 0.0020 0.0661

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            104285
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.881
_diffrn_reflns_theta_min         2.661
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -121.00 -37.00   0.50    1.10    --  -48.68 -32.00   9.00  168
  2  ω    -24.00  37.00   0.50    1.10    --   48.68 -32.00   9.00  122
  3  ω   -159.00 -75.00   0.50    4.00    --  -86.25 -32.00   9.00  168
  4  ω     97.00 178.00   0.50    4.00    --  107.75  32.00 168.00  162
  5  ω    -37.00  24.00   0.50    1.10    --  -48.68  32.00 168.00  122
  6  ω    -26.00  26.00   0.50    1.10    --  -48.68  19.00 -60.00  104
  7  ω     27.00 120.00   0.50    1.10    --   48.68  77.00 -90.00  186
  8  ω     35.00 120.00   0.50    1.10    --   48.68  57.00 -90.00  170
  9  ω     39.00 121.00   0.50    1.10    --   48.68  38.00-150.00  164
 10  ω   -158.00 -64.00   0.50    4.00    --  -86.25 -77.00 -90.00  188
 11  ω   -158.00 -67.00   0.50    4.00    --  -86.25 -71.00-109.35  182
 12  ω   -158.00 -65.00   0.50    4.00    --  -86.25 -75.00 -82.21  186
 13  ω   -158.00 -71.00   0.50    4.00    --  -86.25 -61.00 -90.00  174
 14  ω     97.00 178.00   0.50    4.00    --  107.75  30.00 120.00  162
 15  ω     86.00 178.00   0.50    4.00    --  107.75  77.00-150.00  184
 16  ω     93.00 178.00   0.50    4.00    --  107.75  61.00 -60.00  170
 17  ω     97.00 178.00   0.50    4.00    --  107.75  15.00-150.00  162
 18  ω     36.00  71.00   0.50    4.00    --  107.75 -61.00   0.00   70
 19  ω     36.00  71.00   0.50    4.00    --  107.75 -61.00 -30.00   70
 20  ω     86.00 178.00   0.50    4.00    --  107.75  77.00 -90.00  184
 21  ω     95.00 178.00   0.50    4.00    --  107.75 125.00  30.00  166
 22  ω     93.00 178.00   0.50    4.00    --  107.75  61.00-120.00  170
 23  ω     95.00 178.00   0.50    4.00    --  107.75 125.00  60.00  166
 24  ω     36.00  71.00   0.50    4.00    --  107.75 -61.00-120.00   70
 25  ω     97.00 178.00   0.50    4.00    --  107.75  15.00  60.00  162
 26  ω     95.00 178.00   0.50    4.00    --  107.75  61.00  60.00  166
 27  ω    118.00 160.00   0.50    4.00    --  107.75  77.00-120.00   84
 28  ω     93.00 167.00   0.50    4.00    --  107.75  61.00 -90.00  148
 29  ω     93.00 141.00   0.50    4.00    --  107.75  77.00 -60.00   96
 30  ω     87.00 113.00   0.50    4.00    --  107.75  77.00-120.00   52
 31  ω     37.00  64.00   0.50    4.00    --  107.75 -77.00 -60.00   54
 32  ω     77.00 102.00   0.50    4.00    --  107.75 -77.00 -60.00   50
 33  ω     42.00  68.00   0.50    4.00    --  107.75 -77.00   0.00   52
 34  ω     63.00  88.00   0.50    4.00    --  107.75 -77.00  30.00   50
 35  ω     37.00  66.00   0.50    4.00    --  107.75-125.00-180.00   58
 36  ω     97.00 128.00   0.50    4.00    --  107.75  45.00 -60.00   62
 37  ω    127.00 178.00   0.50    4.00    --  107.75 125.00   0.00  102
 38  ω    135.00 161.00   0.50    4.00    --  107.75  15.00 -90.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0654815000
_diffrn_orient_matrix_UB_12      0.0293472000
_diffrn_orient_matrix_UB_13      -0.0004313000
_diffrn_orient_matrix_UB_21      -0.0265011000
_diffrn_orient_matrix_UB_22      -0.0595912000
_diffrn_orient_matrix_UB_23      -0.0245201000
_diffrn_orient_matrix_UB_31      -0.0126598000
_diffrn_orient_matrix_UB_32      -0.0271523000
_diffrn_orient_matrix_UB_33      0.0534632000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6055
_reflns_number_total             6421
_reflns_odcompleteness_completeness 98.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     78.52
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         6421
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0435
_refine_ls_restrained_S_all      1.137
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0528P)²+20.4205P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1119
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N5-O9 \\sim N5-O9A
 with sigma of 0.04
 N7B-N1 \\sim N1-N7 \\sim N1-N7B
 with sigma of 0.02
 N5-N11 \\sim N5-N11A
 with sigma of 0.02
 O9-N11 \\sim O9A-N11A
 with sigma of 0.02
 N2-N8 \\sim N2-N8A
 with sigma of 0.02
 N13-N19 \\sim N13-N19A
 with sigma of 0.02
 N16-O20 \\sim N16-O20A
 with sigma of 0.04
 N16-N22 \\sim N16-N22A \\sim N16-N22B
 with sigma of 0.02
 N22-O20 \\sim N22A-O20A \\sim N22B-O20B
 with sigma of 0.02
 O3-N8 \\sim O3A-N8A
 with sigma of 0.02
 O3-N2 \\sim O3A-N2
 with sigma of 0.04
 O4-N8 \\sim O4A-N8A
 with sigma of 0.02
 O3-O4 \\sim O3A-O4A
 with sigma of 0.04
 O4-N2 \\sim O4A-N2
 with sigma of 0.04
 N1-O1 \\sim N1-O1A
 with sigma of 0.04
 N7B-O1B \\sim N7-O1 \\sim N7A-O1A
 with sigma of 0.02
 N1-O2 \\sim N1-O2A
 with sigma of 0.04
 O2B-N7B \\sim O2-N7 \\sim O2A-N7A
 with sigma of 0.02
 O2-O1 \\sim O2A-O1A
 with sigma of 0.04
 O13-N19 \\sim O13A-N19A
 with sigma of 0.02
 O13-N13 \\sim O13A-N13
 with sigma of 0.04
 N19-O14 \\sim N19A-O14A
 with sigma of 0.02
 O13-O14 \\sim O13A-O14A
 with sigma of 0.04
 N13-O14 \\sim N13-O14A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq: with sigma of 0.0008 and sigma for terminal atoms of 0.0016
Uanis(O4A) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O1A) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O1B) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O2B) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O14A) \\sim Ueq, Uanis(O14) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O9) = Uanis(O9A)
Uanis(N7) = Uanis(N7A) = Uanis(N7B)
Uanis(N11A) = Uanis(N11)
Uanis(N8A) = Uanis(N8)
Uanis(N19A) = Uanis(N19)
Uanis(O20A) = Uanis(O20B) = Uanis(O20)
Uanis(N22) = Uanis(N22A) = Uanis(N22B)
Uanis(O3A) = Uanis(O3)
Uanis(O4) = Uanis(O4A)
Uanis(O1) = Uanis(O1B) = Uanis(O1A)
Uanis(O2) = Uanis(O2A) = Uanis(O2B)
Uanis(O13A) = Uanis(O13)
Uanis(O14A) = Uanis(O14)
4. Others
 1*[Sof(O1)+Sof(O2)+Sof(N7)]+1*[Sof(O1A)+Sof(O2A)+Sof(N7A)]+1*[Sof(O1B)+
 Sof(O2B)+Sof(N7B)]=1 with esd of 0.0001
 1*[Sof(O20)+Sof(N22)]+1*[Sof(O20A)+Sof(N22A)]+1*[Sof(O20B)+Sof(N22B)]=1 with
 esd of 0.0001
 Sof(O1)=Sof(O2)=Sof(N7)=FVAR(1)
 Sof(O9A)=Sof(N11A)=1-FVAR(2)
 Sof(O9)=Sof(N11)=FVAR(2)
 Sof(O20)=Sof(N22)=FVAR(3)
 Sof(O1A)=Sof(O2A)=Sof(N7A)=FVAR(4)
 Sof(O1B)=Sof(O2B)=Sof(N7B)=FVAR(5)
 Sof(O3A)=Sof(O4A)=Sof(N8A)=1-FVAR(6)
 Sof(O3)=Sof(O4)=Sof(N8)=FVAR(6)
 Sof(O13A)=Sof(O14A)=Sof(N19A)=1-FVAR(7)
 Sof(O13)=Sof(O14)=Sof(N19)=FVAR(7)
 Sof(O20A)=Sof(N22A)=FVAR(8)
 Sof(O20B)=Sof(N22B)=FVAR(9)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10),
 C11(H11), C12(H12), C13(H13)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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_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 0.34591(17) 0.23153(15) 0.72030(15) 0.0434(7) Uani 0.537(3) 1 d D U P A 1
O1A O 0.3108(3) 0.2187(3) 0.7105(3) 0.0434(7) Uani 0.233(2) 1 d D U P A 2
O1B O 0.3641(4) 0.2410(4) 0.7147(4) 0.0434(7) Uani 0.230(3) 1 d D U P A 3
O2 O 0.30411(18) 0.29595(14) 0.77470(11) 0.0372(6) Uani 0.537(3) 1 d D U P A 1
O2A O 0.2771(3) 0.2867(3) 0.7672(2) 0.0372(6) Uani 0.233(2) 1 d D U P A 2
O2B O 0.3287(4) 0.3076(3) 0.7731(3) 0.0372(6) Uani 0.230(3) 1 d D U P A 3
O3 O 0.15945(12) 0.21432(10) 0.60618(18) 0.0395(7) Uani 0.874(13) 1 d D . P B 1
O3A O 0.1595(10) 0.2132(8) 0.6234(10) 0.0395(7) Uani 0.126(13) 1 d D . P B 2
O4 O 0.09887(10) 0.27352(9) 0.6519(2) 0.0401(8) Uani 0.874(13) 1 d D U P B 1
O4A O 0.1067(7) 0.2777(7) 0.6734(11) 0.0401(8) Uani 0.126(13) 1 d D U P B 2
O5 O 0.43525(6) 0.31978(6) 0.62082(6) 0.0435(3) Uani 1 1 d . . . . .
O6 O 0.42993(6) 0.42066(6) 0.62517(7) 0.0506(4) Uani 1 1 d . . . . .
O7 O 0.28362(9) 0.31622(7) 0.50971(6) 0.0565(4) Uani 1 1 d . U . . .
O8 O 0.24963(7) 0.41224(6) 0.50930(5) 0.0383(3) Uani 1 1 d . . . . .
O9 O 0.20097(10) 0.40809(8) 0.77812(8) 0.0445(5) Uani 0.795(3) 1 d D . P C 1
O9A O 0.1411(4) 0.4035(3) 0.7516(3) 0.0445(5) Uani 0.205(3) 1 d D . P C 2
O11 O 0.38748(6) 0.76899(6) 0.64048(5) 0.0355(3) Uani 1 1 d . . . . .
O12 O 0.30430(5) 0.80603(5) 0.60360(5) 0.0288(3) Uani 1 1 d . . . . .
O13 O 0.2211(5) 0.6899(6) 0.7774(4) 0.0325(6) Uani 0.235(7) 1 d D . P D 1
O13A O 0.20460(15) 0.68076(15) 0.78039(11) 0.0325(6) Uani 0.765(7) 1 d D . P D
2
O14 O 0.1627(5) 0.7414(5) 0.7255(3) 0.0475(6) Uani 0.235(7) 1 d D U P D 1
O14A O 0.13929(16) 0.72220(15) 0.72613(9) 0.0475(6) Uani 0.765(7) 1 d D U P D 2
O15 O 0.30007(7) 0.60150(6) 0.50283(5) 0.0358(3) Uani 1 1 d . . . . .
O16 O 0.24348(7) 0.68630(6) 0.50340(5) 0.0405(3) Uani 1 1 d . . . . .
O17 O 0.12266(6) 0.52163(6) 0.63976(5) 0.0332(3) Uani 1 1 d . . . . .
O18 O 0.08409(6) 0.61545(7) 0.63807(6) 0.0406(3) Uani 1 1 d . . . . .
O20 O 0.34854(11) 0.64142(12) 0.77482(9) 0.0375(5) Uani 0.579(2) 1 d D . P E 1
O20A O 0.4139(3) 0.6611(3) 0.7241(2) 0.0375(5) Uani 0.228(3) 1 d D . P E 2
O20B O 0.4050(4) 0.6529(4) 0.7395(3) 0.0375(5) Uani 0.193(3) 1 d D . P E 3
N1 N 0.30081(8) 0.31693(7) 0.69206(6) 0.0323(3) Uani 1 1 d D . . . .
N2 N 0.19883(6) 0.30048(6) 0.64277(6) 0.0267(3) Uani 1 1 d D . . . .
N3 N 0.34110(6) 0.36667(6) 0.62333(6) 0.0258(3) Uani 1 1 d . . . . .
N4 N 0.23523(7) 0.35234(6) 0.57624(5) 0.0283(3) Uani 1 1 d . . . . .
N5 N 0.21403(7) 0.38521(6) 0.69949(5) 0.0289(3) Uani 1 1 d D . . . .
N6 N 0.26007(6) 0.44587(5) 0.62642(5) 0.0200(3) Uani 1 1 d . . . . .
N7 N 0.31736(19) 0.27851(17) 0.7318(2) 0.0341(19) Uani 0.537(3) 1 d D . P A 1
N7A N 0.2967(5) 0.2717(5) 0.7250(4) 0.0341(19) Uani 0.233(2) 1 d D . P A 2
N7B N 0.3337(8) 0.2870(6) 0.7291(4) 0.0341(19) Uani 0.230(3) 1 d D . P A 3
N8 N 0.14823(11) 0.26014(11) 0.63169(16) 0.0306(6) Uani 0.874(13) 1 d D . P B 1
N8A N 0.1486(8) 0.2607(8) 0.6469(10) 0.0306(6) Uani 0.126(13) 1 d D . P B 2
N9 N 0.40717(7) 0.36891(7) 0.62403(7) 0.0358(4) Uani 1 1 d . . . . .
N10 N 0.25794(8) 0.36048(7) 0.52878(6) 0.0334(3) Uani 1 1 d . . . . .
N11 N 0.17376(12) 0.39608(10) 0.73811(9) 0.0344(5) Uani 0.795(3) 1 d D . P C 1
N11A N 0.1985(5) 0.4055(5) 0.7498(4) 0.0344(5) Uani 0.205(3) 1 d D . P C 2
N12 N 0.30299(6) 0.71013(6) 0.63524(6) 0.0241(3) Uani 1 1 d . . . . .
N13 N 0.22132(7) 0.67051(7) 0.69712(5) 0.0303(3) Uani 1 1 d D . . . .
N15 N 0.18734(6) 0.60235(6) 0.63628(5) 0.0225(3) Uani 1 1 d . . . . .
N16 N 0.32501(6) 0.63164(6) 0.69578(5) 0.0261(3) Uani 1 1 d D . . . .
N17 N 0.28944(6) 0.55176(5) 0.63065(5) 0.0193(2) Uani 1 1 d . . . . .
N18 N 0.33404(6) 0.76520(6) 0.62480(5) 0.0247(3) Uani 1 1 d . . . . .
N19 N 0.1975(7) 0.7000(7) 0.7363(5) 0.0288(8) Uani 0.235(7) 1 d D . P D 1
N19A N 0.18577(17) 0.69193(18) 0.73718(15) 0.0288(8) Uani 0.765(7) 1 d D . P D
2
N20 N 0.27193(7) 0.64417(6) 0.52433(5) 0.0277(3) Uani 1 1 d . . . . .
N21 N 0.12702(6) 0.57820(7) 0.63917(5) 0.0273(3) Uani 1 1 d . . . . .
N22 N 0.3679(4) 0.6492(4) 0.7313(3) 0.0313(10) Uani 0.579(2) 1 d D . P E 1
N22A N 0.3634(10) 0.6397(12) 0.7367(7) 0.0313(10) Uani 0.228(3) 1 d D . P E 2
N22B N 0.3515(5) 0.6284(5) 0.7456(4) 0.0313(10) Uani 0.193(3) 1 d D . P E 3
N14 N 0.26937(6) 0.64094(6) 0.57608(5) 0.0206(3) Uani 1 1 d . . . . .
C1 C 0.31378(7) 0.30701(7) 0.63837(6) 0.0241(3) Uani 1 1 d . . . . .
H1 H 0.343205 0.271538 0.632817 0.029 Uiso 1 1 calc R U . . .
C2 C 0.25076(7) 0.29835(7) 0.60734(6) 0.0233(3) Uani 1 1 d . . . . .
H2 H 0.250860 0.259049 0.586835 0.028 Uiso 1 1 calc R U . . .
C3 C 0.28128(8) 0.38071(7) 0.70100(6) 0.0267(3) Uani 1 1 d . . . . .
H3 H 0.298308 0.397071 0.733905 0.032 Uiso 1 1 calc R U . . .
C4 C 0.30918(7) 0.41627(7) 0.65417(6) 0.0217(3) Uani 1 1 d . . . . .
H4 H 0.340162 0.447959 0.665943 0.026 Uiso 1 1 calc R U . . .
C5 C 0.18404(7) 0.36661(7) 0.65316(7) 0.0262(3) Uani 1 1 d . . . . .
H5 H 0.137994 0.373241 0.655246 0.031 Uiso 1 1 calc R U . . .
C6 C 0.21294(7) 0.40442(7) 0.60773(6) 0.0229(3) Uani 1 1 d . . . . .
H6 H 0.179808 0.428232 0.589305 0.028 Uiso 1 1 calc R U . . .
C7 C 0.27694(8) 0.49975(7) 0.59591(6) 0.0231(3) Uani 1 1 d . . . . .
H7A H 0.242470 0.510618 0.572426 0.028 Uiso 1 1 calc R U . . .
H7B H 0.314449 0.490481 0.575270 0.028 Uiso 1 1 calc R U . . .
C8 C 0.19604(7) 0.66853(7) 0.64563(6) 0.0223(3) Uani 1 1 d . . . . .
H8 H 0.156126 0.692299 0.642712 0.027 Uiso 1 1 calc R U . . .
C9 C 0.24769(7) 0.69329(7) 0.60662(6) 0.0209(3) Uani 1 1 d . . . . .
H9 H 0.232058 0.728417 0.585058 0.025 Uiso 1 1 calc R U . . .
C10 C 0.26092(7) 0.61540(8) 0.70508(6) 0.0254(3) Uani 1 1 d . . . . .
H10 H 0.255309 0.597984 0.740187 0.031 Uiso 1 1 calc R U . . .
C11 C 0.23821(7) 0.56809(7) 0.66336(6) 0.0212(3) Uani 1 1 d . . . . .
H11 H 0.221054 0.529842 0.680011 0.025 Uiso 1 1 calc R U . . .
C12 C 0.33955(7) 0.65377(7) 0.64560(6) 0.0232(3) Uani 1 1 d . . . . .
H12 H 0.385192 0.661891 0.641825 0.028 Uiso 1 1 calc R U . . .
C13 C 0.31634(7) 0.60519(6) 0.60540(6) 0.0198(3) Uani 1 1 d . . . . .
H13 H 0.351386 0.592047 0.582676 0.024 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 N7 1.218(5) . ?
O1A N7A 1.238(10) . ?
O1B N7B 1.241(11) . ?
O2 N7 1.218(5) . ?
O2A N7A 1.227(11) . ?
O2B N7B 1.239(12) . ?
O3 N8 1.213(3) . ?
O3A N8A 1.214(16) . ?
O4 N8 1.218(3) . ?
O4A N8A 1.193(15) . ?
O5 N9 1.218(2) . ?
O6 N9 1.214(2) . ?
O7 N10 1.207(2) . ?
O8 N10 1.236(2) . ?
O9 N11 1.227(3) . ?
O9A N11A 1.233(11) . ?
O11 N18 1.2211(18) . ?
O12 N18 1.2182(18) . ?
O13 N19 1.209(13) . ?
O13A N19A 1.226(4) . ?
O14 N19 1.195(13) . ?
O14A N19A 1.225(4) . ?
O15 N20 1.2331(18) . ?
O16 N20 1.2213(19) . ?
O17 N21 1.2180(19) . ?
O18 N21 1.221(2) . ?
O20 N22 1.226(8) . ?
O20A N22A 1.224(15) . ?
O20B N22B 1.273(11) . ?
N1 N7 1.375(5) . ?
N1 N7A 1.301(13) . ?
N1 N7B 1.361(12) . ?
N1 C1 1.450(2) . ?
N1 C3 1.451(2) . ?
N2 N8 1.419(3) . ?
N2 N8A 1.380(15) . ?
N2 C2 1.451(2) . ?
N2 C5 1.4798(19) . ?
N3 N9 1.4192(19) . ?
N3 C1 1.4625(19) . ?
N3 C4 1.5018(19) . ?
N4 N10 1.347(2) . ?
N4 C2 1.4552(19) . ?
N4 C6 1.469(2) . ?
N5 N11 1.351(3) . ?
N5 N11A 1.427(11) . ?
N5 C3 1.447(2) . ?
N5 C5 1.431(2) . ?
N6 C4 1.4296(19) . ?
N6 C6 1.4334(19) . ?
N6 C7 1.4520(18) . ?
N12 N18 1.3844(18) . ?
N12 C9 1.4497(19) . ?
N12 C12 1.4674(19) . ?
N13 N19 1.309(13) . ?
N13 N19A 1.377(4) . ?
N13 C8 1.454(2) . ?
N13 C10 1.472(2) . ?
N15 N21 1.3968(18) . ?
N15 C8 1.4537(19) . ?
N15 C11 1.4955(19) . ?
N16 N22 1.362(6) . ?
N16 N22A 1.363(13) . ?
N16 N22B 1.424(10) . ?
N16 C10 1.440(2) . ?
N16 C12 1.432(2) . ?
N17 C7 1.4653(18) . ?
N17 C11 1.4374(18) . ?
N17 C13 1.4443(18) . ?
N20 N14 1.3585(19) . ?
N14 C9 1.4557(18) . ?
N14 C13 1.4816(19) . ?
C1 H1 1.0000 . ?
C1 C2 1.589(2) . ?
C2 H2 1.0000 . ?
C3 H3 1.0000 . ?
C3 C4 1.564(2) . ?
C4 H4 1.0000 . ?
C5 H5 1.0000 . ?
C5 C6 1.568(2) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8 1.0000 . ?
C8 C9 1.599(2) . ?
C9 H9 1.0000 . ?
C10 H10 1.0000 . ?
C10 C11 1.570(2) . ?
C11 H11 1.0000 . ?
C12 H12 1.0000 . ?
C12 C13 1.563(2) . ?
C13 H13 1.0000 . ?

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
N7 N1 C1 126.7(2) . . ?
N7 N1 C3 121.2(2) . . ?
N7A N1 C1 123.1(4) . . ?
N7A N1 C3 125.3(4) . . ?
N7B N1 C1 121.5(5) . . ?
N7B N1 C3 118.7(6) . . ?
C1 N1 C3 110.52(12) . . ?
N8 N2 C2 115.96(19) . . ?
N8 N2 C5 117.30(15) . . ?
N8A N2 C2 129.1(9) . . ?
N8A N2 C5 114.3(8) . . ?
C2 N2 C5 108.23(12) . . ?
N9 N3 C1 115.28(13) . . ?
N9 N3 C4 115.14(12) . . ?
C1 N3 C4 107.03(12) . . ?
N10 N4 C2 122.49(14) . . ?
N10 N4 C6 122.50(13) . . ?
C2 N4 C6 111.49(12) . . ?
N11 N5 C3 129.00(17) . . ?
N11 N5 C5 113.30(16) . . ?
N11A N5 C3 103.2(4) . . ?
N11A N5 C5 139.8(4) . . ?
C5 N5 C3 116.96(13) . . ?
C4 N6 C6 114.73(12) . . ?
C4 N6 C7 116.75(13) . . ?
C6 N6 C7 118.84(12) . . ?
O1 N7 O2 126.9(5) . . ?
O1 N7 N1 116.1(4) . . ?
O2 N7 N1 117.0(3) . . ?
O1A N7A N1 117.8(9) . . ?
O2A N7A O1A 127.0(12) . . ?
O2A N7A N1 115.2(8) . . ?
O1B N7B N1 115.5(10) . . ?
O2B N7B O1B 127.8(11) . . ?
O2B N7B N1 116.7(9) . . ?
O3 N8 O4 127.1(2) . . ?
O3 N8 N2 117.1(2) . . ?
O4 N8 N2 115.67(19) . . ?
O3A N8A N2 109.2(15) . . ?
O4A N8A O3A 134.3(18) . . ?
O4A N8A N2 116.4(14) . . ?
O5 N9 N3 117.67(14) . . ?
O6 N9 O5 126.52(15) . . ?
O6 N9 N3 115.69(14) . . ?
O7 N10 O8 127.08(16) . . ?
O7 N10 N4 116.44(15) . . ?
O8 N10 N4 116.47(14) . . ?
O9 N11 N5 111.8(2) . . ?
O9A N11A N5 104.9(9) . . ?
N18 N12 C9 120.32(13) . . ?
N18 N12 C12 118.88(12) . . ?
C9 N12 C12 109.15(11) . . ?
N19 N13 C8 126.6(6) . . ?
N19 N13 C10 120.2(6) . . ?
N19A N13 C8 120.7(2) . . ?
N19A N13 C10 118.7(2) . . ?
C8 N13 C10 108.87(12) . . ?
N21 N15 C8 118.20(12) . . ?
N21 N15 C11 117.94(12) . . ?
C8 N15 C11 107.87(12) . . ?
N22 N16 C10 126.7(4) . . ?
N22 N16 C12 112.8(3) . . ?
N22A N16 C10 118.3(9) . . ?
N22A N16 C12 123.3(7) . . ?
N22B N16 C10 102.4(4) . . ?
N22B N16 C12 140.3(4) . . ?
C12 N16 C10 116.35(13) . . ?
C11 N17 C7 114.57(12) . . ?
C11 N17 C13 112.66(11) . . ?
C13 N17 C7 113.19(12) . . ?
O11 N18 N12 116.28(13) . . ?
O12 N18 O11 126.69(14) . . ?
O12 N18 N12 116.89(13) . . ?
O13 N19 N13 116.7(12) . . ?
O14 N19 O13 127.3(13) . . ?
O14 N19 N13 114.7(11) . . ?
O13A N19A N13 117.1(3) . . ?
O14A N19A O13A 126.2(3) . . ?
O14A N19A N13 116.6(3) . . ?
O15 N20 N14 115.96(13) . . ?
O16 N20 O15 126.13(15) . . ?
O16 N20 N14 117.76(13) . . ?
O17 N21 O18 126.55(14) . . ?
O17 N21 N15 116.22(13) . . ?
O18 N21 N15 117.09(14) . . ?
O20 N22 N16 111.6(5) . . ?
O20A N22A N16 111.7(14) . . ?
O20B N22B N16 103.0(7) . . ?
N20 N14 C9 121.46(12) . . ?
N20 N14 C13 121.08(12) . . ?
C9 N14 C13 109.42(12) . . ?
N1 C1 N3 102.11(13) . . ?
N1 C1 H1 112.0 . . ?
N1 C1 C2 110.50(13) . . ?
N3 C1 H1 112.0 . . ?
N3 C1 C2 107.82(12) . . ?
C2 C1 H1 112.0 . . ?
N2 C2 N4 99.03(12) . . ?
N2 C2 C1 108.83(13) . . ?
N2 C2 H2 111.8 . . ?
N4 C2 C1 112.84(12) . . ?
N4 C2 H2 111.8 . . ?
C1 C2 H2 111.8 . . ?
N1 C3 H3 111.4 . . ?
N1 C3 C4 102.90(13) . . ?
N5 C3 N1 110.29(14) . . ?
N5 C3 H3 111.4 . . ?
N5 C3 C4 109.15(12) . . ?
C4 C3 H3 111.4 . . ?
N3 C4 C3 104.52(12) . . ?
N3 C4 H4 110.2 . . ?
N6 C4 N3 112.20(12) . . ?
N6 C4 C3 109.46(12) . . ?
N6 C4 H4 110.2 . . ?
C3 C4 H4 110.2 . . ?
N2 C5 H5 111.0 . . ?
N2 C5 C6 105.78(13) . . ?
N5 C5 N2 109.10(13) . . ?
N5 C5 H5 111.0 . . ?
N5 C5 C6 108.74(13) . . ?
C6 C5 H5 111.0 . . ?
N4 C6 C5 99.27(12) . . ?
N4 C6 H6 110.5 . . ?
N6 C6 N4 115.73(13) . . ?
N6 C6 C5 109.95(13) . . ?
N6 C6 H6 110.5 . . ?
C5 C6 H6 110.5 . . ?
N6 C7 N17 108.10(12) . . ?
N6 C7 H7A 110.1 . . ?
N6 C7 H7B 110.1 . . ?
N17 C7 H7A 110.1 . . ?
N17 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
N13 C8 H8 112.1 . . ?
N13 C8 C9 108.93(12) . . ?
N15 C8 N13 103.46(13) . . ?
N15 C8 H8 112.1 . . ?
N15 C8 C9 107.83(11) . . ?
C9 C8 H8 112.1 . . ?
N12 C9 N14 102.41(11) . . ?
N12 C9 C8 108.66(12) . . ?
N12 C9 H9 112.3 . . ?
N14 C9 C8 108.44(11) . . ?
N14 C9 H9 112.3 . . ?
C8 C9 H9 112.3 . . ?
N13 C10 H10 111.2 . . ?
N13 C10 C11 104.01(12) . . ?
N16 C10 N13 109.47(14) . . ?
N16 C10 H10 111.2 . . ?
N16 C10 C11 109.60(12) . . ?
C11 C10 H10 111.2 . . ?
N15 C11 C10 103.82(12) . . ?
N15 C11 H11 110.0 . . ?
N17 C11 N15 113.32(12) . . ?
N17 C11 C10 109.59(12) . . ?
N17 C11 H11 110.0 . . ?
C10 C11 H11 110.0 . . ?
N12 C12 H12 111.2 . . ?
N12 C12 C13 104.77(12) . . ?
N16 C12 N12 109.06(13) . . ?
N16 C12 H12 111.2 . . ?
N16 C12 C13 109.12(12) . . ?
C13 C12 H12 111.2 . . ?
N17 C13 N14 112.13(12) . . ?
N17 C13 C12 110.40(12) . . ?
N17 C13 H13 110.4 . . ?
N14 C13 C12 102.74(11) . . ?
N14 C13 H13 110.4 . . ?
C12 C13 H13 110.4 . . ?

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
O15 N20 N14 C9 168.81(14) . . . . ?
O15 N20 N14 C13 23.3(2) . . . . ?
O16 N20 N14 C9 -15.4(2) . . . . ?
O16 N20 N14 C13 -160.89(14) . . . . ?
N1 C1 C2 N2 -2.30(16) . . . . ?
N1 C1 C2 N4 106.58(15) . . . . ?
N1 C3 C4 N3 0.83(16) . . . . ?
N1 C3 C4 N6 121.20(13) . . . . ?
N2 C5 C6 N4 4.58(15) . . . . ?
N2 C5 C6 N6 -117.23(14) . . . . ?
N3 C1 C2 N2 -113.12(13) . . . . ?
N3 C1 C2 N4 -4.25(18) . . . . ?
N5 C3 C4 N3 -116.31(13) . . . . ?
N5 C3 C4 N6 4.06(17) . . . . ?
N5 C5 C6 N4 121.63(13) . . . . ?
N5 C5 C6 N6 -0.18(17) . . . . ?
N7 N1 C1 N3 -129.6(3) . . . . ?
N7 N1 C1 C2 115.9(3) . . . . ?
N7 N1 C3 N5 -100.0(3) . . . . ?
N7 N1 C3 C4 143.7(2) . . . . ?
N7A N1 C1 N3 -155.4(6) . . . . ?
N7A N1 C1 C2 90.2(6) . . . . ?
N7A N1 C3 N5 -74.8(6) . . . . ?
N7A N1 C3 C4 168.8(6) . . . . ?
N7B N1 C1 N3 -110.2(9) . . . . ?
N7B N1 C1 C2 135.4(9) . . . . ?
N7B N1 C3 N5 -119.3(8) . . . . ?
N7B N1 C3 C4 124.4(8) . . . . ?
N8 N2 C2 N4 98.25(19) . . . . ?
N8 N2 C2 C1 -143.75(18) . . . . ?
N8 N2 C5 N5 129.9(2) . . . . ?
N8 N2 C5 C6 -113.3(2) . . . . ?
N8A N2 C2 N4 109.7(14) . . . . ?
N8A N2 C2 C1 -132.3(14) . . . . ?
N8A N2 C5 N5 112.1(12) . . . . ?
N8A N2 C5 C6 -131.1(12) . . . . ?
N9 N3 C1 N1 95.51(15) . . . . ?
N9 N3 C1 C2 -148.06(14) . . . . ?
N9 N3 C4 N6 132.65(15) . . . . ?
N9 N3 C4 C3 -108.82(15) . . . . ?
N10 N4 C2 N2 -159.45(15) . . . . ?
N10 N4 C2 C1 85.62(18) . . . . ?
N10 N4 C6 N6 -70.48(19) . . . . ?
N10 N4 C6 C5 171.98(15) . . . . ?
N11 N5 C3 N1 110.10(19) . . . . ?
N11 N5 C3 C4 -137.55(18) . . . . ?
N11 N5 C5 N2 -111.02(16) . . . . ?
N11 N5 C5 C6 134.06(15) . . . . ?
N11A N5 C3 N1 117.7(4) . . . . ?
N11A N5 C3 C4 -129.9(4) . . . . ?
N11A N5 C5 N2 -115.5(7) . . . . ?
N11A N5 C5 C6 129.6(7) . . . . ?
N12 C12 C13 N17 -118.80(13) . . . . ?
N12 C12 C13 N14 0.95(15) . . . . ?
N13 C8 C9 N12 -0.37(16) . . . . ?
N13 C8 C9 N14 110.22(13) . . . . ?
N13 C10 C11 N15 -0.24(15) . . . . ?
N13 C10 C11 N17 121.11(13) . . . . ?
N15 C8 C9 N12 -112.01(13) . . . . ?
N15 C8 C9 N14 -1.41(16) . . . . ?
N16 C10 C11 N15 -117.20(13) . . . . ?
N16 C10 C11 N17 4.14(17) . . . . ?
N16 C12 C13 N17 -2.13(16) . . . . ?
N16 C12 C13 N14 117.61(12) . . . . ?
N18 N12 C9 N14 109.98(14) . . . . ?
N18 N12 C9 C8 -135.42(13) . . . . ?
N18 N12 C12 N16 119.84(15) . . . . ?
N18 N12 C12 C13 -123.45(14) . . . . ?
N19 N13 C8 N15 -122.1(9) . . . . ?
N19 N13 C8 C9 123.3(9) . . . . ?
N19 N13 C10 N16 -105.7(9) . . . . ?
N19 N13 C10 C11 137.2(9) . . . . ?
N19A N13 C8 N15 -108.5(2) . . . . ?
N19A N13 C8 C9 137.0(2) . . . . ?
N19A N13 C10 N16 -120.3(2) . . . . ?
N19A N13 C10 C11 122.6(2) . . . . ?
N20 N14 C9 N12 -115.47(15) . . . . ?
N20 N14 C9 C8 129.78(14) . . . . ?
N20 N14 C13 N17 -113.72(14) . . . . ?
N20 N14 C13 C12 127.74(14) . . . . ?
N21 N15 C8 N13 103.24(15) . . . . ?
N21 N15 C8 C9 -141.46(13) . . . . ?
N21 N15 C11 N17 125.02(14) . . . . ?
N21 N15 C11 C10 -116.16(14) . . . . ?
N22 N16 C10 N13 95.0(6) . . . . ?
N22 N16 C10 C11 -151.6(6) . . . . ?
N22 N16 C12 N12 -98.8(6) . . . . ?
N22 N16 C12 C13 147.3(6) . . . . ?
N22A N16 C10 N13 104.0(14) . . . . ?
N22A N16 C10 C11 -142.5(14) . . . . ?
N22A N16 C12 N12 -103.5(16) . . . . ?
N22A N16 C12 C13 142.6(16) . . . . ?
N22B N16 C10 N13 110.9(5) . . . . ?
N22B N16 C10 C11 -135.7(5) . . . . ?
N22B N16 C12 N12 -106.5(8) . . . . ?
N22B N16 C12 C13 139.6(8) . . . . ?
C1 N1 N7 O1 0.1(5) . . . . ?
C1 N1 N7 O2 177.5(3) . . . . ?
C1 N1 N7A O1A 7.6(12) . . . . ?
C1 N1 N7A O2A -170.4(6) . . . . ?
C1 N1 N7B O1B -16.5(17) . . . . ?
C1 N1 N7B O2B 165.4(9) . . . . ?
C1 N1 C3 N5 93.48(16) . . . . ?
C1 N1 C3 C4 -22.85(17) . . . . ?
C1 N3 N9 O5 22.5(2) . . . . ?
C1 N3 N9 O6 -161.09(17) . . . . ?
C1 N3 C4 N6 -97.77(15) . . . . ?
C1 N3 C4 C3 20.75(15) . . . . ?
C2 N2 N8 O3 24.3(3) . . . . ?
C2 N2 N8 O4 -160.35(18) . . . . ?
C2 N2 N8A O3A 15(3) . . . . ?
C2 N2 N8A O4A -168.1(14) . . . . ?
C2 N2 C5 N5 -96.62(15) . . . . ?
C2 N2 C5 C6 20.20(17) . . . . ?
C2 N4 N10 O7 11.8(2) . . . . ?
C2 N4 N10 O8 -168.91(15) . . . . ?
C2 N4 C6 N6 88.80(16) . . . . ?
C2 N4 C6 C5 -28.74(16) . . . . ?
C3 N1 N7 O1 -164.1(3) . . . . ?
C3 N1 N7 O2 13.2(4) . . . . ?
C3 N1 N7A O1A 174.5(6) . . . . ?
C3 N1 N7A O2A -3.5(11) . . . . ?
C3 N1 N7B O1B -160.0(10) . . . . ?
C3 N1 N7B O2B 21.8(17) . . . . ?
C3 N1 C1 N3 36.04(17) . . . . ?
C3 N1 C1 C2 -78.44(16) . . . . ?
C3 N5 N11 O9 6.0(3) . . . . ?
C3 N5 N11A O9A -173.1(6) . . . . ?
C3 N5 C5 N2 59.98(17) . . . . ?
C3 N5 C5 C6 -54.93(17) . . . . ?
C4 N3 N9 O5 147.95(17) . . . . ?
C4 N3 N9 O6 -35.7(2) . . . . ?
C4 N3 C1 N1 -33.99(15) . . . . ?
C4 N3 C1 C2 82.45(15) . . . . ?
C4 N6 C6 N4 -54.56(18) . . . . ?
C4 N6 C6 C5 56.86(17) . . . . ?
C4 N6 C7 N17 -72.72(16) . . . . ?
C5 N2 N8 O3 154.27(19) . . . . ?
C5 N2 N8 O4 -30.4(3) . . . . ?
C5 N2 N8A O3A 159.4(15) . . . . ?
C5 N2 N8A O4A -24(2) . . . . ?
C5 N2 C2 N4 -35.97(15) . . . . ?
C5 N2 C2 C1 82.03(15) . . . . ?
C5 N5 N11 O9 175.71(16) . . . . ?
C5 N5 N11A O9A 2.7(12) . . . . ?
C5 N5 C3 N1 -59.25(18) . . . . ?
C5 N5 C3 C4 53.10(17) . . . . ?
C6 N4 N10 O7 168.86(17) . . . . ?
C6 N4 N10 O8 -11.9(2) . . . . ?
C6 N4 C2 N2 41.27(16) . . . . ?
C6 N4 C2 C1 -73.66(17) . . . . ?
C6 N6 C4 N3 56.84(17) . . . . ?
C6 N6 C4 C3 -58.72(16) . . . . ?
C6 N6 C7 N17 142.95(13) . . . . ?
C7 N6 C4 N3 -88.94(15) . . . . ?
C7 N6 C4 C3 155.50(12) . . . . ?
C7 N6 C6 N4 90.46(16) . . . . ?
C7 N6 C6 C5 -158.13(13) . . . . ?
C7 N17 C11 N15 -74.84(16) . . . . ?
C7 N17 C11 C10 169.72(12) . . . . ?
C7 N17 C13 N14 76.39(15) . . . . ?
C7 N17 C13 C12 -169.71(12) . . . . ?
C8 N13 N19 O13 171.1(9) . . . . ?
C8 N13 N19 O14 -21.3(18) . . . . ?
C8 N13 N19A O13A 165.5(2) . . . . ?
C8 N13 N19A O14A -16.8(4) . . . . ?
C8 N13 C10 N16 96.36(15) . . . . ?
C8 N13 C10 C11 -20.70(17) . . . . ?
C8 N15 N21 O17 -167.98(14) . . . . ?
C8 N15 N21 O18 15.9(2) . . . . ?
C8 N15 C11 N17 -97.83(14) . . . . ?
C8 N15 C11 C10 20.99(15) . . . . ?
C9 N12 N18 O11 -162.01(14) . . . . ?
C9 N12 N18 O12 22.0(2) . . . . ?
C9 N12 C12 N16 -96.86(15) . . . . ?
C9 N12 C12 C13 19.85(16) . . . . ?
C9 N14 C13 N17 97.12(14) . . . . ?
C9 N14 C13 C12 -21.42(14) . . . . ?
C10 N13 N19 O13 17.4(17) . . . . ?
C10 N13 N19 O14 -175.1(10) . . . . ?
C10 N13 N19A O13A 26.6(4) . . . . ?
C10 N13 N19A O14A -155.7(3) . . . . ?
C10 N13 C8 N15 34.00(16) . . . . ?
C10 N13 C8 C9 -80.50(15) . . . . ?
C10 N16 N22 O20 9.8(11) . . . . ?
C10 N16 N22A O20A -171.2(14) . . . . ?
C10 N16 N22B O20B -169.2(7) . . . . ?
C10 N16 C12 N12 59.87(16) . . . . ?
C10 N16 C12 C13 -54.03(16) . . . . ?
C11 N15 N21 O17 -35.24(19) . . . . ?
C11 N15 N21 O18 148.61(15) . . . . ?
C11 N15 C8 N13 -33.78(14) . . . . ?
C11 N15 C8 C9 81.52(14) . . . . ?
C11 N17 C7 N6 -58.32(16) . . . . ?
C11 N17 C13 N14 -55.60(16) . . . . ?
C11 N17 C13 C12 58.30(15) . . . . ?
C12 N12 N18 O11 -22.9(2) . . . . ?
C12 N12 N18 O12 161.20(14) . . . . ?
C12 N12 C9 N14 -32.70(16) . . . . ?
C12 N12 C9 C8 81.90(14) . . . . ?
C12 N16 N22 O20 165.8(6) . . . . ?
C12 N16 N22A O20A -8(3) . . . . ?
C12 N16 N22B O20B -1.7(13) . . . . ?
C12 N16 C10 N13 -60.29(17) . . . . ?
C12 N16 C10 C11 53.19(17) . . . . ?
C13 N17 C7 N6 170.64(12) . . . . ?
C13 N17 C11 N15 56.46(16) . . . . ?
C13 N17 C11 C10 -58.98(16) . . . . ?
C13 N14 C9 N12 33.56(15) . . . . ?
C13 N14 C9 C8 -81.20(14) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.250 0.760 123.6 43.8 '2 C2H3N1'
2 0.000 0.250 0.247 72.3 28.9 '1 C2H5N1O1'
3 0.000 0.250 0.003 72.3 28.9 '2 C2H3N1'
4 0.000 0.250 0.490 123.6 43.8 '1 C2H5N1O1'
5 0.000 0.750 0.240 123.6 43.8 '2 C2H3N1'
6 0.000 0.750 0.753 72.3 28.9 '1 C2H5N1O1'
7 0.000 0.750 0.510 123.6 43.8 '2 C2H3N1'
8 0.000 0.750 0.997 72.3 28.9 '1 C2H5N1O1'
9 0.500 0.250 0.010 123.6 43.8 '2 C2H3N1'
10 0.500 0.750 0.990 123.6 43.8 '2 C2H3N1'
11 0.500 0.250 0.497 72.3 28.9 '1 C2H5N1O1'
12 0.500 0.750 0.503 72.3 28.9 '1 C2H5N1O1'
13 0.500 0.250 0.740 123.6 43.8 '2 C2H3N1'
14 0.500 0.750 0.260 123.6 43.8 '2 C2H3N1'
15 0.500 0.250 0.253 72.3 28.9 '1 C2H5N1O1'
16 0.500 0.750 0.747 72.3 28.9 '1 C2H5N1O1'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.445
_oxdiff_exptl_absorpt_empirical_full_min 0.880
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_14
_database_code_depnum_ccdc_archive 'CCDC 2208929'
loop_
_audit_author_name
_audit_author_address
'Aida I Samigullina'
;N D Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences 
Russia
;
_audit_update_record             
;
2022-09-27 deposited with the CCDC.	2022-12-09 downloaded from the CCDC.
;
_audit_creation_date             2022-09-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2018/3
# start Validation Reply Form
_vrf_PLAT430_14                  
;
PROBLEM: Short Inter D...A Contact  O7       ..O20A     .       2.64 Ang.  
RESPONSE: These intermolecular interactions are expected for this structure
;
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C13 H14 N22 O19'
_chemical_formula_sum            'C13 H14 N22 O19'
_chemical_formula_weight         782.46
_chemical_melting_point          ?
_chemical_oxdiff_formula         C15H17N23O18
_chemical_oxdiff_usercomment     PGV2040-needle
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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   21.53830(10)
_cell_length_b                   21.53830(10)
_cell_length_c                   26.3607(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     12228.68(15)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    41236
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      77.6180
_cell_measurement_theta_min      2.5970
_shelx_estimated_absorpt_T_max   0.946
_shelx_estimated_absorpt_T_min   0.738
_exptl_absorpt_coefficient_mu    1.408
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.58a (Rigaku Oxford Diffraction, 2022)
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   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             6368
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.1664
0 0 -1 0.0627
1 0 0 0.0209
-1 0 0 0.0190
0 1 0 0.0198
0 -1 0 0.0157

_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
loop_
_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
-0.0041 0.0013 0.9976 -0.0137 0.0058 0.0564
0.0041 -0.0013 -0.9976 0.0137 -0.0058 -0.0564
0.9998 -0.0044 0.0059 0.0343 0.0627 0.0019
-0.9998 0.0044 -0.0059 -0.0343 -0.0627 -0.0019
0.0045 1.0002 -0.0029 -0.0604 0.0337 -0.0182
-0.0045 -1.0002 0.0029 0.0604 -0.0337 0.0182

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            80393
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.086
_diffrn_reflns_theta_min         2.649
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -119.00 -94.00   0.50    5.00    --  -48.68-133.00-152.00   50
  2  ω    -91.00 -21.00   0.50    5.00    --  -48.68 137.00  92.00  140
  3  ω    -81.00 -45.00   0.50    5.00    --  -48.68 -19.00-108.00   72
  4  ω    -24.00   1.00   0.50    5.00    --  -48.68  19.00  58.00   50
  5  ω     57.00  82.00   0.50    5.00    --   48.68  19.00  58.00   50
  6  ω    -81.00 -56.00   0.50   18.00    --  -86.25 137.00  92.00   50
  7  ω   -137.00-112.00   0.50   18.00    --  -86.25-133.00-152.00   50
  8  ω   -118.00 -93.00   0.50   18.00    --  -86.25 -19.00-108.00   50
  9  ω   -145.00-120.00   0.50   18.00    --  -86.25-106.00 101.00   50
 10  ω     43.00  70.00   0.50   18.00    --  107.75-133.00-152.00   54
 11  ω     71.00  96.00   0.50   18.00    --  107.75-106.00 101.00   50
 12  ω    103.00 133.00   0.50   18.00    --  107.75 137.00  92.00   60
 13  ω    113.00 138.00   0.50   18.00    --  107.75  19.00  58.00   50
 14  ω     80.00 105.00   0.50   18.00    --  107.75-137.00  29.00   50
 15  ω     80.00 117.00   0.50   18.00    --  107.75-133.00-152.00   74
 16  ω    -64.00 -35.00   0.50    5.00    --  -48.68 -57.00 150.00   58
 17  ω    -69.00 -37.00   0.50    5.00    --  -48.68 -57.00 120.00   64
 18  ω    -59.00 -27.00   0.50    5.00    --  -48.68 -77.00 120.00   64
 19  ω     40.00  94.00   0.50    5.00    --   48.68  19.00 150.00  108
 20  ω     39.00 118.00   0.50    5.00    --   48.68  38.00-180.00  158
 21  ω    -90.00 -64.00   0.50   18.00    --  -86.25 -77.00 120.00   52
 22  ω    -96.00 -69.00   0.50   18.00    --  -86.25 -66.00 176.72   54
 23  ω    -89.00 -64.00   0.50   18.00    --  -86.25 -77.00 150.00   50
 24  ω    -94.00 -65.00   0.50   18.00    --  -86.25 -77.00 137.01   58
 25  ω    -90.00 -64.00   0.50   18.00    --  -86.25 -77.00-180.00   52
 26  ω   -108.00 -66.00   0.50   18.00    --  -86.25 -72.00 159.78   84
 27  ω    125.00 151.00   0.50   18.00    --  107.75  61.00 150.00   52
 28  ω     86.00 166.00   0.50   18.00    --  107.75  77.00-180.00  160
 29  ω     37.00  62.00   0.50   18.00    --  107.75 -61.00 120.00   50
 30  ω     93.00 124.00   0.50   18.00    --  107.75  61.00 150.00   62
 31  ω    140.00 166.00   0.50   18.00    --  107.75  45.00 120.00   52
 32  ω    122.00 167.00   0.50   18.00    --  107.75  77.00 150.00   90
 33  ω     38.00  70.00   0.50   18.00    --  107.75 -61.00   0.00   64
 34  ω     37.00  69.00   0.50   18.00    --  107.75 -61.00  30.00   64
 35  ω     48.00  74.00   0.50   18.00    --  107.75 -95.00-180.00   52
 36  ω     92.00 129.00   0.50   18.00    --  107.75  77.00 120.00   74
 37  ω     95.00 168.00   0.50   18.00    --  107.75  61.00 -90.00  146
 38  ω     63.00 101.00   0.50   18.00    --  107.75 -95.00  30.00   76
 39  ω     98.00 157.00   0.50   18.00    --  107.75  15.00-120.00  118
 40  ω     95.00 143.00   0.50   18.00    --  107.75  74.00-133.05   96
 41  ω    153.00 178.00   0.50   18.00    --  107.75  74.00-133.05   50
 42  ω     64.00 103.00   0.50   18.00    --  107.75 -77.00-150.00   78
 43  ω     94.00 120.00   0.50   18.00    --  107.75  75.00  57.42   52
 44  ω    133.00 159.00   0.50   18.00    --  107.75  75.00  57.42   52
 45  ω     37.00  75.00   0.50   18.00    --  107.75 -67.00 -11.90   76
 46  ω     88.00 116.00   0.50   18.00    --  107.75  77.00 150.00   56
 47  ω     70.00 110.00   0.50   18.00    --  107.75   4.00  43.81   80
 48  ω     38.00  70.00   0.50   18.00    --  107.75 -61.00 -60.00   64
 49  ω     79.00 104.00   0.50   18.00    --  107.75 -77.00  90.00   50
 50  ω     93.00 156.00   0.50   18.00    --  107.75  61.00-180.00  126
 51  ω    106.00 132.00   0.50   18.00    --  107.75  30.00-180.00   52
 52  ω     95.00 121.00   0.50   18.00    --  107.75 -86.00 132.30   52
 53  ω     38.00  74.00   0.50   18.00    --  107.75 -77.00  90.00   72
 54  ω    110.00 135.00   0.50   18.00    --  107.75 133.00 -84.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0341463000
_diffrn_orient_matrix_UB_12      -0.0606024000
_diffrn_orient_matrix_UB_13      -0.0135032000
_diffrn_orient_matrix_UB_21      0.0628390000
_diffrn_orient_matrix_UB_22      0.0334564000
_diffrn_orient_matrix_UB_23      0.0060571000
_diffrn_orient_matrix_UB_31      0.0014807000
_diffrn_orient_matrix_UB_32      -0.0180615000
_diffrn_orient_matrix_UB_33      0.0565354000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6047
_reflns_number_total             6509
_reflns_odcompleteness_completeness 98.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     78.52
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.000058(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         6509
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0482
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0534P)²+23.8467P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1210
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N13-O13 \\sim N13-O13A
 with sigma of 0.04
 N13-N19 \\sim N13-N19A \\sim N13-N19B
 with sigma of 0.02
 O13-N19 \\sim O13A-N19A \\sim O13B-N19B
 with sigma of 0.02
 N13-O14 \\sim N13-O14A
 with sigma of 0.04
 O13-O14 \\sim O13A-O14A
 with sigma of 0.04
 N19-O14 \\sim N19A-O14A \\sim N19B-O14B
 with sigma of 0.02
 O1-N7 \\sim O1A-N7A
 with sigma of 0.02
 N1-N7 \\sim N1-N7A
 with sigma of 0.02
 N7-O2 \\sim N7A-O2A
 with sigma of 0.02
 O1-N1 \\sim O1A-N1
 with sigma of 0.04
 O1-O2 \\sim O1A-O2A
 with sigma of 0.04
 N1-O2 \\sim N1-O2A
 with sigma of 0.04
 N11B-O10B \\sim O10A-N11A
 with sigma of 0.02
 O20A-N22A \\sim N22-O20
 with sigma of 0.02
 N11B-N5 \\sim N16-N22B
 with sigma of 0.02
 N5-N11A \\sim N5-N11 \\sim N22-N16 \\sim N16-N22A
 with sigma of 0.02
 N11-O9 \\sim N11-O10 \\sim N22B-O21B \\sim N22B-O20B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(O2A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N19A) = Uanis(N19) = Uanis(N19B)
Uanis(O13A) = Uanis(O13) = Uanis(O14A) = Uanis(O14) = Uanis(O13B) = Uanis(O14B)
Uanis(O1A) = Uanis(O1)
Uanis(N7) = Uanis(N7A)
Uanis(O2) = Uanis(O2A)
Uanis(O20A) = Uanis(O20)
Uanis(N22A) = Uanis(N22)
Uanis(O10) = Uanis(O10A)
Uanis(O10B) = Uanis(O9)
Uanis(N11) = Uanis(N11A) = Uanis(N11B)
Uanis(O20) = Uanis(O20B)
Uanis(O20B) = Uanis(O21B)
Uanis(N22A) = Uanis(N22) = Uanis(N22B)
4. Others
 1*[Sof(N11)+Sof(O10)+Sof(O9)]+1*[Sof(N11A)+Sof(O10A)]+1*[Sof(O10B)+Sof(N11B)]=
 1 with esd of 0.0001
 1*[Sof(O20)+Sof(N22)]+1*[Sof(N22A)+Sof(O20A)]+1*[Sof(O21B)+Sof(O20B)+
 Sof(N22B)]=1 with esd of 0.0001
 1*[Sof(O13)+Sof(N19)+Sof(O14)]+1*[Sof(N19A)+Sof(O14A)+Sof(O13A)]+1*[Sof(O14B)+
 Sof(N19B)+Sof(O13B)]=1 with esd of 0.0001
 1*[Sof(N11)+Sof(O10)+Sof(O9)]+1*[Sof(O21B)+Sof(O20B)+Sof(N22B)]=1 with esd of
 0.0001
 1*[Sof(O20)+Sof(N22)]+1*[Sof(N11A)+Sof(O10A)]+1*[Sof(O10B)+Sof(N11B)]+1*
 [Sof(N22A)+Sof(O20A)]=1 with esd of 0.0001
 Sof(O13)=Sof(N19)=Sof(O14)=FVAR(1)
 Sof(O20)=Sof(N22)=FVAR(2)
 Sof(N11)=Sof(O10)=Sof(O9)=FVAR(3)
 Sof(N11A)=Sof(O10A)=FVAR(4)
 Sof(O10B)=Sof(N11B)=FVAR(5)
 Sof(N22A)=Sof(O20A)=FVAR(6)
 Sof(O21B)=Sof(O20B)=Sof(N22B)=FVAR(7)
 Sof(N19A)=Sof(O14A)=Sof(O13A)=FVAR(8)
 Sof(O14B)=Sof(N19B)=Sof(O13B)=FVAR(9)
 Sof(O2A)=Sof(N7A)=Sof(O1A)=1-FVAR(10)
 Sof(O1)=Sof(N7)=Sof(O2)=FVAR(10)
5.a Ternary CH refined with riding coordinates:
 C4(H4), C6(H6), C2(H2), C11(H11), C8(H8), C13(H13), C5(H5), C1(H1), C3(H3),
 C9(H9), C10(H10), C12(H12)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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_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
O4 O 0.19591(6) 0.80509(6) 0.39785(5) 0.0311(3) Uani 1 1 d . . . . .
O8 O 0.19984(7) 0.60080(6) 0.49793(5) 0.0355(3) Uani 1 1 d . . . . .
O6 O 0.37606(7) 0.52107(7) 0.36010(5) 0.0351(3) Uani 1 1 d . . . . .
O3 O 0.11342(6) 0.76878(6) 0.36054(6) 0.0364(3) Uani 1 1 d . . . . .
O15 O 0.24740(8) 0.41058(7) 0.48934(5) 0.0376(3) Uani 1 1 d . . . . .
O7 O 0.25220(8) 0.68778(7) 0.49749(6) 0.0413(4) Uani 1 1 d . . . . .
N6 N 0.21042(7) 0.55161(6) 0.37034(5) 0.0206(3) Uani 1 1 d . . . . .
O5 O 0.41510(6) 0.61414(8) 0.36461(7) 0.0434(4) Uani 1 1 d . . . . .
O18 O 0.06430(7) 0.32094(7) 0.37684(7) 0.0435(4) Uani 1 1 d . . . . .
N3 N 0.31216(6) 0.60176(7) 0.36446(6) 0.0235(3) Uani 1 1 d . . . . .
N17 N 0.23928(7) 0.44596(6) 0.37397(5) 0.0215(3) Uani 1 1 d . . . . .
N4 N 0.23101(7) 0.63999(6) 0.42498(5) 0.0217(3) Uani 1 1 d . . . . .
N2 N 0.19714(7) 0.70943(6) 0.36640(6) 0.0242(3) Uani 1 1 d . . . . .
N14 N 0.26400(8) 0.35162(7) 0.42251(6) 0.0270(3) Uani 1 1 d . . . . .
N8 N 0.16636(7) 0.76455(7) 0.37659(6) 0.0264(3) Uani 1 1 d . . . . .
O1 O 0.2986(2) 0.6799(3) 0.2222(2) 0.0343(9) Uani 0.664(8) 1 d D . P A 1
N15 N 0.15802(7) 0.36731(7) 0.37520(6) 0.0254(3) Uani 1 1 d . . . . .
N12 N 0.30011(7) 0.30136(7) 0.35519(6) 0.0283(3) Uani 1 1 d . . . . .
O17 O 0.06966(7) 0.42131(7) 0.37315(7) 0.0458(4) Uani 1 1 d . . . . .
O12 O 0.33940(8) 0.21507(7) 0.39032(8) 0.0512(4) Uani 1 1 d . . . . .
N5 N 0.17456(7) 0.63058(7) 0.30624(6) 0.0259(3) Uani 1 1 d D . . . .
N16 N 0.28507(8) 0.38786(8) 0.30031(6) 0.0308(4) Uani 1 1 d D . . . .
N10 N 0.22672(8) 0.64410(7) 0.47659(6) 0.0284(3) Uani 1 1 d . . . . .
N9 N 0.37201(7) 0.57739(8) 0.36183(6) 0.0292(3) Uani 1 1 d . . . . .
N1 N 0.27815(7) 0.67069(8) 0.30471(6) 0.0298(3) Uani 1 1 d D . . . .
O11 O 0.39973(7) 0.27552(8) 0.34623(9) 0.0571(5) Uani 1 1 d . . . . .
N13 N 0.19832(8) 0.31931(7) 0.30629(6) 0.0320(4) Uani 1 1 d D . . . .
N20 N 0.23836(9) 0.35973(8) 0.46872(6) 0.0341(4) Uani 1 1 d . . . . .
O16 O 0.20941(10) 0.31617(7) 0.48598(7) 0.0568(5) Uani 1 1 d . . . . .
N21 N 0.09228(8) 0.36979(8) 0.37411(7) 0.0337(4) Uani 1 1 d . . . . .
N7 N 0.3164(3) 0.6907(4) 0.2656(2) 0.0309(14) Uani 0.664(8) 1 d D . P A 1
N18 N 0.35059(8) 0.26142(8) 0.36551(8) 0.0403(4) Uani 1 1 d . . . . .
N11 N 0.1375(6) 0.6503(14) 0.2671(4) 0.0309(15) Uani 0.6340(15) 1 d D . P B 1
O10 O 0.1557(7) 0.6448(6) 0.2236(4) 0.0434(14) Uani 0.6340(15) 1 d D . P B 1
C4 C 0.26129(8) 0.56799(8) 0.33771(6) 0.0218(3) Uani 1 1 d . . . . .
H4 H 0.278193 0.529937 0.320932 0.026 Uiso 1 1 calc R U . . .
O20 O 0.3019(2) 0.4087(3) 0.2214(3) 0.0433(8) Uani 0.531(2) 1 d D . P C 1
C6 C 0.18404(8) 0.60465(7) 0.39570(7) 0.0211(3) Uani 1 1 d . . . . .
H6 H 0.149229 0.591415 0.418351 0.025 Uiso 1 1 calc R U . . .
O2 O 0.3642(2) 0.71846(19) 0.27760(13) 0.0450(7) Uani 0.664(8) 1 d D U P A 1
C2 C 0.25224(8) 0.69248(8) 0.39468(7) 0.0217(3) Uani 1 1 d . . . . .
H2 H 0.267932 0.727389 0.416155 0.026 Uiso 1 1 calc R U . . .
C7 C 0.22258(9) 0.49940(7) 0.40450(7) 0.0240(4) Uani 1 1 d . . . . .
H7A H 0.256882 0.509874 0.427986 0.029 Uiso 1 1 calc R U . . .
H7B H 0.185092 0.490102 0.424864 0.029 Uiso 1 1 calc R U . . .
C11 C 0.28634(8) 0.40419(8) 0.39177(7) 0.0236(3) Uani 1 1 d . . . . .
H11 H 0.319410 0.427506 0.410372 0.028 Uiso 1 1 calc R U . . .
C8 C 0.24820(8) 0.29862(8) 0.39048(7) 0.0251(4) Uani 1 1 d . . . . .
H8 H 0.247871 0.258903 0.410116 0.030 Uiso 1 1 calc R U . . .
C13 C 0.19035(8) 0.41746(8) 0.34557(7) 0.0232(3) Uani 1 1 d . . . . .
H13 H 0.159727 0.449518 0.334301 0.028 Uiso 1 1 calc R U . . .
C5 C 0.16053(8) 0.65343(8) 0.35613(7) 0.0234(3) Uani 1 1 d . . . . .
H5 H 0.115077 0.661530 0.360166 0.028 Uiso 1 1 calc R U . . .
N22 N 0.3278(3) 0.3956(7) 0.2621(4) 0.0313(13) Uani 0.531(2) 1 d D . P C 1
C1 C 0.30346(8) 0.66795(8) 0.35583(7) 0.0236(3) Uani 1 1 d . . . . .
H1 H 0.343290 0.691525 0.358834 0.028 Uiso 1 1 calc R U . . .
C3 C 0.23879(8) 0.61541(8) 0.29659(7) 0.0249(4) Uani 1 1 d . . . . .
H3 H 0.244385 0.598327 0.261615 0.030 Uiso 1 1 calc R U . . .
C9 C 0.18550(8) 0.30835(8) 0.35970(7) 0.0260(4) Uani 1 1 d . . . . .
H9 H 0.156114 0.272927 0.364655 0.031 Uiso 1 1 calc R U . . .
C10 C 0.31503(9) 0.36760(8) 0.34608(7) 0.0266(4) Uani 1 1 d . . . . .
H10 H 0.360931 0.374147 0.344137 0.032 Uiso 1 1 calc R U . . .
C12 C 0.21812(9) 0.38289(8) 0.29850(7) 0.0274(4) Uani 1 1 d . . . . .
H12 H 0.201239 0.400030 0.266059 0.033 Uiso 1 1 calc R U . . .
O9 O 0.08644(12) 0.67021(14) 0.27896(11) 0.0442(6) Uani 0.6340(15) 1 d D . P B
1
O13 O 0.2253(4) 0.2921(3) 0.2314(2) 0.0486(10) Uani 0.291(2) 1 d D . P D 1
N19 N 0.2053(4) 0.2745(3) 0.2728(3) 0.0347(13) Uani 0.291(2) 1 d D . P D 1
O14 O 0.1906(4) 0.2223(3) 0.2858(2) 0.0486(10) Uani 0.291(2) 1 d D . P D 1
N19A N 0.1830(3) 0.2798(3) 0.2669(2) 0.0347(13) Uani 0.386(3) 1 d D . P D 2
O14A O 0.1530(4) 0.2334(2) 0.2756(3) 0.0486(10) Uani 0.386(3) 1 d D . P D 2
O13A O 0.1952(3) 0.2970(3) 0.2235(2) 0.0486(10) Uani 0.386(3) 1 d D . P D 2
N22A N 0.3000(8) 0.4042(12) 0.2503(7) 0.0313(13) Uani 0.103(2) 1 d D . P C 2
O20A O 0.3586(9) 0.4041(9) 0.2429(7) 0.0433(8) Uani 0.103(2) 1 d D . P C 2
N11A N 0.1313(15) 0.648(3) 0.2703(10) 0.0309(15) Uani 0.268(2) 1 d D . P B 3
O10A O 0.1549(19) 0.6361(17) 0.2308(12) 0.0434(14) Uani 0.268(2) 1 d D . P B 3
O10B O 0.0988(9) 0.6504(10) 0.2582(8) 0.0442(6) Uani 0.0977(19) 1 d D . P B 2
N11B N 0.1490(10) 0.6278(10) 0.2571(8) 0.0309(15) Uani 0.0977(19) 1 d D . P B 2
O21B O 0.3699(3) 0.3900(2) 0.25726(19) 0.0433(8) Uani 0.3660(15) 1 d D . P C 3
O20B O 0.2833(3) 0.4029(5) 0.2178(4) 0.0433(8) Uani 0.3660(15) 1 d D . P C 3
N22B N 0.3138(5) 0.3948(11) 0.2546(5) 0.0313(13) Uani 0.3660(15) 1 d D . P C 3
O14B O 0.1367(4) 0.2444(3) 0.2833(3) 0.0486(10) Uani 0.323(3) 1 d D . P D 3
N19B N 0.1651(3) 0.2910(4) 0.2686(3) 0.0347(13) Uani 0.323(3) 1 d D . P D 3
O13B O 0.1722(3) 0.3118(3) 0.2255(2) 0.0486(10) Uani 0.323(3) 1 d D . P D 3
O2A O 0.3428(4) 0.7353(4) 0.2738(3) 0.0450(7) Uani 0.336(8) 1 d D U P A 2
N7A N 0.3041(7) 0.6969(8) 0.2639(5) 0.0309(14) Uani 0.336(8) 1 d D . P A 2
O1A O 0.2822(5) 0.6865(7) 0.2226(5) 0.0343(9) Uani 0.336(8) 1 d D . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O4 N8 1.217(2) . ?
O8 N10 1.233(2) . ?
O6 N9 1.217(2) . ?
O3 N8 1.220(2) . ?
O15 N20 1.238(2) . ?
O7 N10 1.221(2) . ?
N6 C4 1.437(2) . ?
N6 C6 1.440(2) . ?
N6 C7 1.464(2) . ?
O5 N9 1.222(2) . ?
O18 N21 1.215(2) . ?
N3 N9 1.394(2) . ?
N3 C4 1.492(2) . ?
N3 C1 1.456(2) . ?
N17 C7 1.450(2) . ?
N17 C11 1.434(2) . ?
N17 C13 1.431(2) . ?
N4 N10 1.366(2) . ?
N4 C6 1.483(2) . ?
N4 C2 1.458(2) . ?
N2 N8 1.386(2) . ?
N2 C2 1.448(2) . ?
N2 C5 1.466(2) . ?
N14 N20 1.349(2) . ?
N14 C11 1.473(2) . ?
N14 C8 1.460(2) . ?
O1 N7 1.229(6) . ?
N15 N21 1.417(2) . ?
N15 C13 1.504(2) . ?
N15 C9 1.459(2) . ?
N12 N18 1.413(2) . ?
N12 C8 1.456(2) . ?
N12 C10 1.482(2) . ?
O17 N21 1.212(2) . ?
O12 N18 1.217(2) . ?
N5 N11 1.372(7) . ?
N5 C5 1.437(2) . ?
N5 C3 1.444(2) . ?
N5 N11A 1.379(14) . ?
N5 N11B 1.409(19) . ?
N16 N22 1.374(10) . ?
N16 C10 1.436(3) . ?
N16 C12 1.447(3) . ?
N16 N22A 1.403(15) . ?
N16 N22B 1.362(16) . ?
N1 N7 1.389(6) . ?
N1 C1 1.455(2) . ?
N1 C3 1.477(2) . ?
N1 N7A 1.337(12) . ?
O11 N18 1.213(2) . ?
N13 C9 1.454(2) . ?
N13 C12 1.449(2) . ?
N13 N19 1.317(7) . ?
N13 N19A 1.384(6) . ?
N13 N19B 1.367(8) . ?
N20 O16 1.215(2) . ?
N7 O2 1.230(6) . ?
N11 O10 1.219(9) . ?
N11 O9 1.220(11) . ?
C4 H4 1.0000 . ?
C4 C3 1.566(2) . ?
O20 N22 1.242(9) . ?
C6 H6 1.0000 . ?
C6 C5 1.565(2) . ?
C2 H2 1.0000 . ?
C2 C1 1.595(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C11 H11 1.0000 . ?
C11 C10 1.566(2) . ?
C8 H8 1.0000 . ?
C8 C9 1.589(3) . ?
C13 H13 1.0000 . ?
C13 C12 1.566(2) . ?
C5 H5 1.0000 . ?
C1 H1 1.0000 . ?
C3 H3 1.0000 . ?
C9 H9 1.0000 . ?
C10 H10 1.0000 . ?
C12 H12 1.0000 . ?
O13 N19 1.234(9) . ?
N19 O14 1.216(9) . ?
N19A O14A 1.210(7) . ?
N19A O13A 1.231(7) . ?
N22A O20A 1.277(19) . ?
N11A O10A 1.19(3) . ?
O10B N11B 1.19(2) . ?
O21B N22B 1.213(11) . ?
O20B N22B 1.186(13) . ?
O14B N19B 1.238(9) . ?
N19B O13B 1.230(9) . ?
O2A N7A 1.201(12) . ?
N7A O1A 1.209(12) . ?

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
C4 N6 C6 112.57(13) . . ?
C4 N6 C7 114.86(14) . . ?
C6 N6 C7 113.23(13) . . ?
N9 N3 C4 118.17(14) . . ?
N9 N3 C1 118.70(14) . . ?
C1 N3 C4 107.99(13) . . ?
C11 N17 C7 119.45(14) . . ?
C13 N17 C7 116.62(14) . . ?
C13 N17 C11 114.99(13) . . ?
N10 N4 C6 120.37(14) . . ?
N10 N4 C2 121.11(14) . . ?
C2 N4 C6 109.07(13) . . ?
N8 N2 C2 120.54(14) . . ?
N8 N2 C5 118.90(14) . . ?
C2 N2 C5 109.17(13) . . ?
N20 N14 C11 122.07(14) . . ?
N20 N14 C8 121.88(15) . . ?
C8 N14 C11 111.03(14) . . ?
O4 N8 O3 126.52(15) . . ?
O4 N8 N2 116.97(15) . . ?
O3 N8 N2 116.35(15) . . ?
N21 N15 C13 115.14(14) . . ?
N21 N15 C9 115.61(14) . . ?
C9 N15 C13 106.96(14) . . ?
N18 N12 C8 116.32(16) . . ?
N18 N12 C10 116.78(15) . . ?
C8 N12 C10 108.01(14) . . ?
N11 N5 C5 117.3(8) . . ?
N11 N5 C3 119.7(5) . . ?
C5 N5 C3 116.12(14) . . ?
N11A N5 C5 113.3(18) . . ?
N11A N5 C3 126.0(13) . . ?
N11B N5 C5 140.8(9) . . ?
N11B N5 C3 101.7(10) . . ?
N22 N16 C10 110.6(3) . . ?
N22 N16 C12 130.8(3) . . ?
C10 N16 C12 116.93(15) . . ?
N22A N16 C10 139.8(8) . . ?
N22A N16 C12 102.5(8) . . ?
N22B N16 C10 124.9(5) . . ?
N22B N16 C12 115.6(4) . . ?
O8 N10 N4 115.91(15) . . ?
O7 N10 O8 126.00(17) . . ?
O7 N10 N4 117.97(15) . . ?
O6 N9 O5 126.41(16) . . ?
O6 N9 N3 116.34(15) . . ?
O5 N9 N3 117.09(16) . . ?
N7 N1 C1 118.5(3) . . ?
N7 N1 C3 118.9(3) . . ?
C1 N1 C3 108.46(14) . . ?
N7A N1 C1 127.2(6) . . ?
N7A N1 C3 117.7(6) . . ?
C12 N13 C9 110.28(14) . . ?
N19 N13 C9 123.5(4) . . ?
N19 N13 C12 124.4(4) . . ?
N19A N13 C9 125.6(3) . . ?
N19A N13 C12 123.1(3) . . ?
N19B N13 C9 122.1(4) . . ?
N19B N13 C12 118.2(4) . . ?
O15 N20 N14 116.53(16) . . ?
O16 N20 O15 126.83(18) . . ?
O16 N20 N14 116.63(17) . . ?
O18 N21 N15 117.50(16) . . ?
O17 N21 O18 126.50(18) . . ?
O17 N21 N15 115.88(16) . . ?
O1 N7 N1 116.5(5) . . ?
O1 N7 O2 126.3(6) . . ?
O2 N7 N1 117.2(5) . . ?
O12 N18 N12 116.76(17) . . ?
O11 N18 N12 116.00(18) . . ?
O11 N18 O12 127.11(19) . . ?
O10 N11 N5 119.3(10) . . ?
O10 N11 O9 124.4(8) . . ?
O9 N11 N5 116.2(8) . . ?
N6 C4 N3 113.37(14) . . ?
N6 C4 H4 109.9 . . ?
N6 C4 C3 109.79(14) . . ?
N3 C4 H4 109.9 . . ?
N3 C4 C3 103.68(13) . . ?
C3 C4 H4 109.9 . . ?
N6 C6 N4 112.31(14) . . ?
N6 C6 H6 110.3 . . ?
N6 C6 C5 110.55(14) . . ?
N4 C6 H6 110.3 . . ?
N4 C6 C5 102.89(13) . . ?
C5 C6 H6 110.3 . . ?
N4 C2 H2 112.3 . . ?
N4 C2 C1 108.18(13) . . ?
N2 C2 N4 102.73(13) . . ?
N2 C2 H2 112.3 . . ?
N2 C2 C1 108.65(14) . . ?
C1 C2 H2 112.3 . . ?
N6 C7 H7A 110.1 . . ?
N6 C7 H7B 110.1 . . ?
N17 C7 N6 108.22(14) . . ?
N17 C7 H7A 110.1 . . ?
N17 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
N17 C11 N14 115.56(15) . . ?
N17 C11 H11 110.4 . . ?
N17 C11 C10 110.05(14) . . ?
N14 C11 H11 110.4 . . ?
N14 C11 C10 99.50(13) . . ?
C10 C11 H11 110.4 . . ?
N14 C8 H8 111.8 . . ?
N14 C8 C9 112.97(14) . . ?
N12 C8 N14 99.14(14) . . ?
N12 C8 H8 111.8 . . ?
N12 C8 C9 108.73(15) . . ?
C9 C8 H8 111.8 . . ?
N17 C13 N15 112.17(14) . . ?
N17 C13 H13 110.2 . . ?
N17 C13 C12 109.70(14) . . ?
N15 C13 H13 110.2 . . ?
N15 C13 C12 104.29(13) . . ?
C12 C13 H13 110.2 . . ?
N2 C5 C6 104.79(14) . . ?
N2 C5 H5 111.3 . . ?
N5 C5 N2 109.73(14) . . ?
N5 C5 C6 108.19(13) . . ?
N5 C5 H5 111.3 . . ?
C6 C5 H5 111.3 . . ?
O20 N22 N16 111.1(6) . . ?
N3 C1 C2 108.24(13) . . ?
N3 C1 H1 112.0 . . ?
N1 C1 N3 103.45(14) . . ?
N1 C1 C2 108.79(14) . . ?
N1 C1 H1 112.0 . . ?
C2 C1 H1 112.0 . . ?
N5 C3 N1 109.99(15) . . ?
N5 C3 C4 108.79(14) . . ?
N5 C3 H3 111.2 . . ?
N1 C3 C4 104.35(14) . . ?
N1 C3 H3 111.2 . . ?
C4 C3 H3 111.2 . . ?
N15 C9 C8 108.44(14) . . ?
N15 C9 H9 111.8 . . ?
N13 C9 N15 101.94(14) . . ?
N13 C9 C8 110.76(15) . . ?
N13 C9 H9 111.8 . . ?
C8 C9 H9 111.8 . . ?
N12 C10 C11 105.91(14) . . ?
N12 C10 H10 111.0 . . ?
N16 C10 N12 109.35(15) . . ?
N16 C10 C11 108.42(14) . . ?
N16 C10 H10 111.0 . . ?
C11 C10 H10 111.0 . . ?
N16 C12 N13 111.02(16) . . ?
N16 C12 C13 108.63(14) . . ?
N16 C12 H12 111.3 . . ?
N13 C12 C13 102.99(14) . . ?
N13 C12 H12 111.3 . . ?
C13 C12 H12 111.3 . . ?
O13 N19 N13 114.0(6) . . ?
O14 N19 N13 117.3(7) . . ?
O14 N19 O13 128.6(7) . . ?
O14A N19A N13 119.4(5) . . ?
O14A N19A O13A 122.7(7) . . ?
O13A N19A N13 117.4(5) . . ?
O20A N22A N16 111.6(15) . . ?
O10A N11A N5 105(3) . . ?
O10B N11B N5 108(2) . . ?
O21B N22B N16 113.1(9) . . ?
O20B N22B N16 119.2(10) . . ?
O20B N22B O21B 127.7(14) . . ?
O14B N19B N13 113.1(7) . . ?
O13B N19B N13 116.3(6) . . ?
O13B N19B O14B 130.2(8) . . ?
O2A N7A N1 114.0(11) . . ?
O2A N7A O1A 126.4(13) . . ?
O1A N7A N1 118.9(12) . . ?

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
N6 C4 C3 N5 3.29(19) . . . . ?
N6 C4 C3 N1 120.66(15) . . . . ?
N6 C6 C5 N2 -118.81(15) . . . . ?
N6 C6 C5 N5 -1.79(18) . . . . ?
N3 C4 C3 N5 -118.14(15) . . . . ?
N3 C4 C3 N1 -0.77(17) . . . . ?
N17 C11 C10 N12 -116.97(16) . . . . ?
N17 C11 C10 N16 0.29(19) . . . . ?
N17 C13 C12 N16 3.20(19) . . . . ?
N17 C13 C12 N13 120.99(15) . . . . ?
N4 C6 C5 N2 1.30(16) . . . . ?
N4 C6 C5 N5 118.32(14) . . . . ?
N4 C2 C1 N3 -0.87(18) . . . . ?
N4 C2 C1 N1 110.90(15) . . . . ?
N2 C2 C1 N3 -111.70(15) . . . . ?
N2 C2 C1 N1 0.07(18) . . . . ?
N14 C11 C10 N12 4.81(17) . . . . ?
N14 C11 C10 N16 122.07(15) . . . . ?
N14 C8 C9 N15 -4.2(2) . . . . ?
N14 C8 C9 N13 106.92(17) . . . . ?
N8 N2 C2 N4 110.63(16) . . . . ?
N8 N2 C2 C1 -134.93(15) . . . . ?
N8 N2 C5 N5 119.70(17) . . . . ?
N8 N2 C5 C6 -124.33(16) . . . . ?
N15 C13 C12 N16 -117.12(15) . . . . ?
N15 C13 C12 N13 0.67(18) . . . . ?
N12 C8 C9 N15 -113.18(15) . . . . ?
N12 C8 C9 N13 -2.10(19) . . . . ?
N10 N4 C6 N6 -115.85(16) . . . . ?
N10 N4 C6 C5 125.26(15) . . . . ?
N10 N4 C2 N2 -113.04(17) . . . . ?
N10 N4 C2 C1 132.17(16) . . . . ?
N9 N3 C4 N6 124.24(16) . . . . ?
N9 N3 C4 C3 -116.77(16) . . . . ?
N9 N3 C1 N1 103.83(17) . . . . ?
N9 N3 C1 C2 -140.85(15) . . . . ?
N20 N14 C11 N17 -66.6(2) . . . . ?
N20 N14 C11 C10 175.72(16) . . . . ?
N20 N14 C8 N12 -163.17(16) . . . . ?
N20 N14 C8 C9 81.9(2) . . . . ?
N21 N15 C13 N17 132.83(16) . . . . ?
N21 N15 C13 C12 -108.52(17) . . . . ?
N21 N15 C9 N13 94.84(17) . . . . ?
N21 N15 C9 C8 -148.26(15) . . . . ?
N7 N1 C1 N3 -105.8(4) . . . . ?
N7 N1 C1 C2 139.2(4) . . . . ?
N7 N1 C3 N5 -124.3(4) . . . . ?
N7 N1 C3 C4 119.2(4) . . . . ?
N18 N12 C8 N14 97.46(17) . . . . ?
N18 N12 C8 C9 -144.38(15) . . . . ?
N18 N12 C10 N16 130.16(18) . . . . ?
N18 N12 C10 C11 -113.21(18) . . . . ?
N11 N5 C5 N2 -92.9(13) . . . . ?
N11 N5 C5 C6 153.4(13) . . . . ?
N11 N5 C3 N1 91.7(15) . . . . ?
N11 N5 C3 C4 -154.6(15) . . . . ?
C4 N6 C6 N4 -55.81(18) . . . . ?
C4 N6 C6 C5 58.49(18) . . . . ?
C4 N6 C7 N17 -57.89(19) . . . . ?
C4 N3 N9 O6 -33.3(2) . . . . ?
C4 N3 N9 O5 151.05(17) . . . . ?
C4 N3 C1 N1 -34.21(16) . . . . ?
C4 N3 C1 C2 81.10(16) . . . . ?
C6 N6 C4 N3 56.47(18) . . . . ?
C6 N6 C4 C3 -58.95(18) . . . . ?
C6 N6 C7 N17 170.87(14) . . . . ?
C6 N4 N10 O8 27.0(2) . . . . ?
C6 N4 N10 O7 -156.78(16) . . . . ?
C6 N4 C2 N2 33.40(17) . . . . ?
C6 N4 C2 C1 -81.39(16) . . . . ?
C2 N4 N10 O8 169.70(15) . . . . ?
C2 N4 N10 O7 -14.0(2) . . . . ?
C2 N4 C6 N6 97.42(16) . . . . ?
C2 N4 C6 C5 -21.47(16) . . . . ?
C2 N2 N8 O4 21.3(2) . . . . ?
C2 N2 N8 O3 -162.98(16) . . . . ?
C2 N2 C5 N5 -96.56(17) . . . . ?
C2 N2 C5 C6 19.40(18) . . . . ?
C7 N6 C4 N3 -75.09(18) . . . . ?
C7 N6 C4 C3 169.49(14) . . . . ?
C7 N6 C6 N4 76.56(17) . . . . ?
C7 N6 C6 C5 -169.14(14) . . . . ?
C7 N17 C11 N14 90.85(18) . . . . ?
C7 N17 C11 C10 -157.49(15) . . . . ?
C7 N17 C13 N15 -89.85(17) . . . . ?
C7 N17 C13 C12 154.75(14) . . . . ?
C11 N17 C7 N6 142.44(15) . . . . ?
C11 N17 C13 N15 57.35(19) . . . . ?
C11 N17 C13 C12 -58.06(19) . . . . ?
C11 N14 N20 O15 -16.5(3) . . . . ?
C11 N14 N20 O16 164.28(19) . . . . ?
C11 N14 C8 N12 41.47(18) . . . . ?
C11 N14 C8 C9 -73.45(19) . . . . ?
C8 N14 N20 O15 -169.17(17) . . . . ?
C8 N14 N20 O16 11.6(3) . . . . ?
C8 N14 C11 N17 88.75(18) . . . . ?
C8 N14 C11 C10 -28.98(18) . . . . ?
C8 N12 N18 O12 24.5(3) . . . . ?
C8 N12 N18 O11 -159.36(19) . . . . ?
C8 N12 C10 N16 -96.51(17) . . . . ?
C8 N12 C10 C11 20.13(19) . . . . ?
C13 N17 C7 N6 -71.89(18) . . . . ?
C13 N17 C11 N14 -55.4(2) . . . . ?
C13 N17 C11 C10 56.31(19) . . . . ?
C13 N15 N21 O18 148.74(18) . . . . ?
C13 N15 N21 O17 -34.9(2) . . . . ?
C13 N15 C9 N13 -34.87(17) . . . . ?
C13 N15 C9 C8 82.03(17) . . . . ?
C5 N2 N8 O4 160.86(16) . . . . ?
C5 N2 N8 O3 -23.4(2) . . . . ?
C5 N2 C2 N4 -32.41(18) . . . . ?
C5 N2 C2 C1 82.03(16) . . . . ?
C5 N5 N11 O10 162(2) . . . . ?
C5 N5 N11 O9 -21(3) . . . . ?
C5 N5 C3 N1 -58.69(19) . . . . ?
C5 N5 C3 C4 55.04(19) . . . . ?
C5 N5 N11A O10A 167(4) . . . . ?
C5 N5 N11B O10B -3(3) . . . . ?
N22 N16 C10 N12 -107.5(7) . . . . ?
N22 N16 C10 C11 137.5(7) . . . . ?
N22 N16 C12 N13 104.9(9) . . . . ?
N22 N16 C12 C13 -142.5(9) . . . . ?
C1 N3 N9 O6 -167.15(16) . . . . ?
C1 N3 N9 O5 17.2(2) . . . . ?
C1 N3 C4 N6 -97.46(16) . . . . ?
C1 N3 C4 C3 21.54(17) . . . . ?
C1 N1 N7 O1 164.7(5) . . . . ?
C1 N1 N7 O2 -16.5(8) . . . . ?
C1 N1 C3 N5 96.24(17) . . . . ?
C1 N1 C3 C4 -20.31(18) . . . . ?
C1 N1 N7A O2A -21(2) . . . . ?
C1 N1 N7A O1A 167.9(11) . . . . ?
C3 N5 N11 O10 12(3) . . . . ?
C3 N5 N11 O9 -170.5(16) . . . . ?
C3 N5 C5 N2 58.21(19) . . . . ?
C3 N5 C5 C6 -55.58(18) . . . . ?
C3 N5 N11A O10A 12(7) . . . . ?
C3 N5 N11B O10B -167.3(17) . . . . ?
C3 N1 N7 O1 29.2(8) . . . . ?
C3 N1 N7 O2 -151.9(5) . . . . ?
C3 N1 C1 N3 33.82(18) . . . . ?
C3 N1 C1 C2 -81.10(17) . . . . ?
C3 N1 N7A O2A -169.1(11) . . . . ?
C3 N1 N7A O1A 20(2) . . . . ?
C9 N15 N21 O18 23.1(3) . . . . ?
C9 N15 N21 O17 -160.54(18) . . . . ?
C9 N15 C13 N17 -97.20(17) . . . . ?
C9 N15 C13 C12 21.45(18) . . . . ?
C9 N13 C12 N16 92.95(18) . . . . ?
C9 N13 C12 C13 -23.1(2) . . . . ?
C9 N13 N19 O13 -169.4(5) . . . . ?
C9 N13 N19 O14 12.0(9) . . . . ?
C9 N13 N19A O14A 4.9(8) . . . . ?
C9 N13 N19A O13A 177.5(5) . . . . ?
C9 N13 N19B O14B -18.8(8) . . . . ?
C9 N13 N19B O13B 167.3(5) . . . . ?
C10 N12 N18 O12 153.99(19) . . . . ?
C10 N12 N18 O11 -29.9(3) . . . . ?
C10 N12 C8 N14 -36.12(18) . . . . ?
C10 N12 C8 C9 82.04(17) . . . . ?
C10 N16 N22 O20 175.0(9) . . . . ?
C10 N16 C12 N13 -58.4(2) . . . . ?
C10 N16 C12 C13 54.2(2) . . . . ?
C10 N16 N22A O20A -4(3) . . . . ?
C10 N16 N22B O21B -9(2) . . . . ?
C10 N16 N22B O20B 168.9(13) . . . . ?
C12 N16 N22 O20 10.9(17) . . . . ?
C12 N16 C10 N12 59.1(2) . . . . ?
C12 N16 C10 C11 -55.94(19) . . . . ?
C12 N16 N22A O20A -172.7(18) . . . . ?
C12 N16 N22B O21B -170.2(12) . . . . ?
C12 N16 N22B O20B 8(2) . . . . ?
C12 N13 C9 N15 36.79(19) . . . . ?
C12 N13 C9 C8 -78.43(19) . . . . ?
C12 N13 N19 O13 -6.6(9) . . . . ?
C12 N13 N19 O14 174.8(6) . . . . ?
C12 N13 N19A O14A -162.2(6) . . . . ?
C12 N13 N19A O13A 10.4(7) . . . . ?
C12 N13 N19B O14B -162.0(5) . . . . ?
C12 N13 N19B O13B 24.1(8) . . . . ?
N19 N13 C9 N15 -158.3(4) . . . . ?
N19 N13 C9 C8 86.5(5) . . . . ?
N19 N13 C12 N16 -71.8(5) . . . . ?
N19 N13 C12 C13 172.1(5) . . . . ?
N19A N13 C9 N15 -131.7(4) . . . . ?
N19A N13 C9 C8 113.1(4) . . . . ?
N19A N13 C12 N16 -98.3(4) . . . . ?
N19A N13 C12 C13 145.6(4) . . . . ?
N22A N16 C10 N12 -108.3(17) . . . . ?
N22A N16 C10 C11 136.7(17) . . . . ?
N22A N16 C12 N13 113.3(11) . . . . ?
N22A N16 C12 C13 -134.1(11) . . . . ?
N11A N5 C5 N2 -99(3) . . . . ?
N11A N5 C5 C6 147(3) . . . . ?
N11A N5 C3 N1 95(4) . . . . ?
N11A N5 C3 C4 -151(4) . . . . ?
N11B N5 C5 N2 -104.9(16) . . . . ?
N11B N5 C5 C6 141.3(15) . . . . ?
N11B N5 C3 N1 110.5(10) . . . . ?
N11B N5 C3 C4 -135.8(10) . . . . ?
N22B N16 C10 N12 -101.8(12) . . . . ?
N22B N16 C10 C11 143.1(12) . . . . ?
N22B N16 C12 N13 104.3(11) . . . . ?
N22B N16 C12 C13 -143.1(11) . . . . ?
N19B N13 C9 N15 -108.9(4) . . . . ?
N19B N13 C9 C8 135.8(4) . . . . ?
N19B N13 C12 N16 -119.8(4) . . . . ?
N19B N13 C12 C13 124.1(4) . . . . ?
N7A N1 C1 N3 -116.5(11) . . . . ?
N7A N1 C1 C2 128.6(11) . . . . ?
N7A N1 C3 N5 -110.2(10) . . . . ?
N7A N1 C3 C4 133.2(10) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.250 0.257 129.4 45.3 '2 C2H3N1'
2 0.000 0.250 0.755 67.2 31.5 '1.5 C2H3N1'
3 0.000 0.250 -0.007 129.4 45.2 '2 C2H3N1'
4 0.000 0.250 0.495 67.2 31.5 '1.5 C2H3N1'
5 0.000 0.750 0.743 129.4 45.2 '2 C2H3N1'
6 0.000 0.750 0.245 67.2 31.5 '1.5 C2H3N1'
7 0.000 0.750 0.007 129.4 45.3 '2 C2H3N1'
8 0.000 0.750 0.505 67.2 31.5 '1.5 C2H3N1'
9 0.500 0.250 0.507 129.4 45.3 '2 C2H3N1'
10 0.500 0.750 0.493 129.4 45.2 '2 C2H3N1'
11 0.500 0.250 0.005 67.2 31.5 '1.5 C2H3N1'
12 0.500 0.750 -0.005 67.2 31.5 '1.5 C2H3N1'
13 0.500 0.250 0.243 129.4 45.2 '2 C2H3N1'
14 0.500 0.750 0.757 129.4 45.3 '2 C2H3N1'
15 0.500 0.250 0.745 67.2 31.5 '1.5 C2H3N1'
16 0.500 0.750 0.255 67.2 31.5 '1.5 C2H3N1'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.771
_oxdiff_exptl_absorpt_empirical_full_min 0.701
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_13
_database_code_depnum_ccdc_archive 'CCDC 2208931'
loop_
_audit_author_name
_audit_author_address
'Aida I Samigullina'
;N D Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences 
Russia
;
_audit_update_record             
;
2022-09-22 deposited with the CCDC.	2022-12-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_13                  
;
PROBLEM: Short Inter D...A Contact  O2       ..O23      .       2.83 Ang.  
RESPONSE: These intermolecular interactions are expected for this structure.
;
_vrf_PLAT041_13                  
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check 
RESPONSE: Crystal contains partially occupated water molecules, the hydrogen 
atoms of which are not located.
;
# end Validation Reply Form
_audit_creation_date             2022-08-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C13 H14 N22 O20, 3.93(C2 H3 N), 0.094(H2 O)'
_chemical_formula_sum            'C20.86 H25.98 N25.93 O20.09'
_chemical_formula_weight         961.51
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     SNI7061-1
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   19.26767(13)
_cell_length_b                   25.25063(19)
_cell_length_c                   15.55504(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.9403(6)
_cell_angle_gamma                90
_cell_volume                     7549.96(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    50379
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.0500
_cell_measurement_theta_min      2.9050
_shelx_estimated_absorpt_T_max   0.913
_shelx_estimated_absorpt_T_min   0.806
_exptl_absorpt_coefficient_mu    1.323
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
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   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3947
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 1 0.0506
-1 -1 -1 0.0453
1 0 0 0.0418
-1 0 0 0.0324
0 -1 1 0.0579
0 1 -1 0.0567
1 -1 0 0.0592
-1 1 0 0.0645
0 1 1 0.0649
0 -1 -1 0.0580
-1 0 -1 0.0466
1 0 1 0.0484
0 -1 0 0.0787
0 1 0 0.0903
1 -1 -1 0.0513
1 1 0 0.0564

_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
loop_
_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
0.9996 0.9996 1.0005 0.0588 -0.0539 0.1214
-0.9996 -0.9996 -1.0005 -0.0588 0.0539 -0.1214
0.9998 -0.0007 0.0004 -0.0390 -0.0344 0.0610
-0.9998 0.0007 -0.0004 0.0390 0.0344 -0.0610
-0.0002 -0.9985 0.9994 0.0323 0.0821 0.0760
0.0002 0.9985 -0.9994 -0.0323 -0.0821 -0.0760
0.9998 -1.0001 0.0001 -0.0717 0.0165 0.0688
-0.9998 1.0001 -0.0001 0.0717 -0.0165 -0.0688
-0.0002 1.0003 1.0000 0.0978 -0.0196 0.0603
0.0002 -1.0003 -1.0000 -0.0978 0.0196 -0.0603
-0.9996 -0.0002 -1.0002 -0.0261 0.0031 -0.1292
0.9996 0.0002 1.0002 0.0261 -0.0031 0.1292
0.0000 -0.9994 -0.0003 -0.0327 0.0508 0.0078
-0.0000 0.9994 0.0003 0.0327 -0.0508 -0.0078
1.0000 -1.0010 -0.9996 -0.1367 -0.0148 0.0007
0.9998 0.9987 0.0007 -0.0062 -0.0852 0.0532

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            108627
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.542
_diffrn_reflns_theta_min         2.299
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -84.00 -25.00   0.50    1.25    --  -48.76 119.00 -14.00  118
  2  ω   -121.00 -53.00   0.50    1.25    --  -48.76-158.00 105.00  136
  3  ω     59.00  84.00   0.50    1.25    --   48.76-158.00 105.00   50
  4  ω     47.00  73.00   0.50    1.25    --   48.76-119.00-100.00   52
  5  ω     73.00  98.00   0.50    1.25    --   48.76 158.00 139.00   50
  6  ω    -75.00 -50.00   0.50    5.01    --  -90.00 119.00 -14.00   50
  7  ω    -93.00 -68.00   0.50    5.01    --  -90.00 158.00 139.00   50
  8  ω   -143.00-118.00   0.50    5.01    --  -90.00-119.00-100.00   50
  9  ω    114.00 139.00   0.50    5.01    --  111.50 119.00 -14.00   50
 10  ω    107.00 132.00   0.50    5.01    --  111.50 158.00 139.00   50
 11  ω    104.00 130.00   0.50    5.01    --  111.50-158.00 105.00   52
 12  ω     49.00 109.00   0.50    5.01    --  111.50-119.00-100.00  120
 13  ω    -25.00  23.00   0.50    1.25    --  -48.76  19.00-180.00   96
 14  ω   -115.00 -88.00   0.50    1.25    --  -48.76-125.00 150.00   54
 15  ω    -22.00  24.00   0.50    1.25    --  -48.76  19.00 -30.00   92
 16  ω    -26.00  26.00   0.50    1.25    --  -48.76  19.00 -60.00  104
 17  ω   -121.00 -73.00   0.50    1.25    --  -48.76-125.00 -60.00   96
 18  ω   -117.00 -75.00   0.50    1.25    --  -48.76-125.00  30.00   84
 19  ω    101.00 177.00   0.50    5.01    --  111.50  15.00  60.00  152
 20  ω     79.00 109.00   0.50    5.01    --  111.50-117.00 -46.72   60
 21  ω     41.00  70.00   0.50    5.01    --  111.50 -61.00 -90.00   58
 22  ω     56.00  82.00   0.50    5.01    --  111.50 -95.00 120.00   52
 23  ω     45.00  75.00   0.50    5.01    --  111.50 -95.00  90.00   60
 24  ω     43.00  70.00   0.50    5.01    --  111.50 -61.00  30.00   54
 25  ω     98.00 124.00   0.50    5.01    --  111.50 -84.00-118.78   52
 26  ω     48.00 108.00   0.50    5.01    --  111.50-111.00 -25.77  120
 27  ω     44.00  74.00   0.50    5.01    --  111.50-117.00 -46.72   60
 28  ω     77.00 107.00   0.50    5.01    --  111.50-103.00 -93.05   60
 29  ω     46.00  73.00   0.50    5.01    --  111.50-103.00 -93.05   54
 30  ω     41.00  86.00   0.50    5.01    --  111.50 -84.00-118.78   90
 31  ω     44.00  70.00   0.50    5.01    --  111.50 -81.00  77.20   52
 32  ω     94.00 133.00   0.50    5.01    --  111.50 -81.00  77.20   78
 33  ω    104.00 152.00   0.50    5.01    --  111.50  45.00 -90.00   96
 34  ω    115.00 177.00   0.50    5.01    --  111.50  30.00 -30.00  124
 35  ω    110.00 174.00   0.50    5.01    --  111.50  79.00-113.18  128
 36  ω     51.00  76.00   0.50    5.01    --  111.50 -87.00-107.09   50
 37  ω     93.00 123.00   0.50    5.01    --  111.50 -87.00-107.09   60
 38  ω    109.00 152.00   0.50    5.01    --  111.50  30.00   0.00   86
 39  ω     70.00 105.00   0.50    5.01    --  111.50-111.00  23.50   70
 40  ω     43.00  70.00   0.50    5.01    --  111.50 -61.00-180.00   54
 41  ω     94.00 148.00   0.50    5.01    --  111.50  77.00  60.00  108
 42  ω     67.00  92.00   0.50    5.01    --  111.50-125.00  60.00   50
 43  ω    102.00 176.00   0.50    5.01    --  111.50  30.00-150.00  148
 44  ω    105.00 131.00   0.50    5.01    --  111.50  15.00  90.00   52
 45  ω     41.00  75.00   0.50    5.01    --  111.50 -77.00  30.00   68
 46  ω     76.00 102.00   0.50    5.01    --  111.50 -95.00-120.00   52
 47  ω    127.00 158.00   0.50    5.01    --  111.50  45.00-120.00   62
 48  ω    104.00 178.00   0.50    5.01    --  111.50  30.00 -60.00  148
 49  ω    116.00 145.00   0.50    5.01    --  111.50  61.00  90.00   58
 50  ω    132.00 175.00   0.50    5.01    --  111.50 125.00-150.00   86
 51  ω     46.00  72.00   0.50    5.01    --  111.50 -77.00 -90.00   52
 52  ω     69.00  95.00   0.50    5.01    --  111.50 -77.00 -60.00   52
 53  ω     68.00  96.00   0.50    5.01    --  111.50 -77.00 120.00   56
 54  ω     43.00  69.00   0.50    5.01    --  111.50 -95.00 -90.00   52
 55  ω     43.00  70.00   0.50    5.01    --  111.50 -61.00 -30.00   54
 56  ω     41.00  70.00   0.50    5.01    --  111.50 -61.00 -60.00   58
 57  ω    107.00 133.00   0.50    5.01    --  111.50  77.00 -90.00   52
 58  ω    136.00 173.00   0.50    5.01    --  111.50  77.00 -90.00   74
 59  ω     40.00  70.00   0.50    5.01    --  111.50 -61.00-120.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0389647000
_diffrn_orient_matrix_UB_12      0.0327293000
_diffrn_orient_matrix_UB_13      0.0650327000
_diffrn_orient_matrix_UB_21      -0.0344147000
_diffrn_orient_matrix_UB_22      -0.0508731000
_diffrn_orient_matrix_UB_23      0.0312903000
_diffrn_orient_matrix_UB_31      0.0610090000
_diffrn_orient_matrix_UB_32      -0.0078352000
_diffrn_orient_matrix_UB_33      0.0681887000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14493
_reflns_number_total             16231
_reflns_odcompleteness_completeness 97.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.50
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1229
_refine_ls_number_reflns         16231
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0458
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0620P)²+5.9131P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1239
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O28-N27 \\sim O28A-N27
 with sigma of 0.04
 N27-O27 \\sim N27-O27A
 with sigma of 0.04
 O28-O27 \\sim O28A-O27A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C51) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O27) = Uanis(O28)
Uanis(O28) = Uanis(O28A) = Uanis(O27A) = Uanis(O27)
4. Others
 Sof(O27A)=Sof(O28A)=1-FVAR(1)
 Sof(O27)=Sof(O28)=Sof(N51)=Sof(C52)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=
 FVAR(1)
 Sof(O41)=Sof(H41A)=Sof(H41B)=FVAR(2)
5.a Free rotating group:
 O41(H41A,H41B)
5.b Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10),
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
  C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
5.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C26(H26A,H26B)
5.d Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C57(H57A,H57B,
 H57C), C59(H59A,H59B,H59C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C65(H65A,
 H65B,H65C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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_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 0.58499(8) 0.47597(6) 1.09868(9) 0.0337(3) Uani 1 1 d . . . . .
O2 O 0.66779(8) 0.41778(6) 1.12359(9) 0.0360(3) Uani 1 1 d . . . . .
O3 O 0.47825(7) 0.39748(5) 0.94119(8) 0.0289(3) Uani 1 1 d . . . . .
O4 O 0.53719(7) 0.32396(5) 0.93027(8) 0.0278(3) Uani 1 1 d . . . . .
O5 O 0.65399(7) 0.57017(5) 0.98666(8) 0.0263(3) Uani 1 1 d . . . . .
O6 O 0.75211(6) 0.56098(5) 0.92594(9) 0.0281(3) Uani 1 1 d . . . . .
O7 O 0.50359(7) 0.47854(6) 0.69350(9) 0.0320(3) Uani 1 1 d . . . . .
O8 O 0.60012(8) 0.46764(6) 0.62985(8) 0.0336(3) Uani 1 1 d . . . . .
O9 O 0.71315(8) 0.31425(6) 1.01602(9) 0.0366(3) Uani 1 1 d . . . . .
O10 O 0.67246(7) 0.27727(5) 0.89647(9) 0.0313(3) Uani 1 1 d . . . . .
O11 O 0.75893(7) 0.58733(6) 0.60748(9) 0.0333(3) Uani 1 1 d . . . . .
O12 O 0.85544(8) 0.59711(6) 0.54407(10) 0.0352(3) Uani 1 1 d . . . . .
O13 O 0.91071(9) 0.43471(6) 0.83854(9) 0.0373(3) Uani 1 1 d . . . . .
O14 O 1.00185(7) 0.45379(6) 0.76869(10) 0.0365(3) Uani 1 1 d . . . . .
O15 O 0.89253(9) 0.51932(7) 0.38672(9) 0.0438(4) Uani 1 1 d . . . . .
O16 O 0.79574(9) 0.47677(8) 0.35350(9) 0.0478(4) Uani 1 1 d . . . . .
O17 O 0.98704(7) 0.41189(6) 0.48203(9) 0.0324(3) Uani 1 1 d . . . . .
O18 O 0.91237(7) 0.34707(5) 0.46840(8) 0.0293(3) Uani 1 1 d . . . . .
O19 O 0.72959(11) 0.36535(7) 0.42421(12) 0.0582(5) Uani 1 1 d . . . . .
O20 O 0.77782(8) 0.30582(6) 0.50916(10) 0.0370(3) Uani 1 1 d . . . . .
N1 N 0.62871(8) 0.43389(6) 0.98705(9) 0.0221(3) Uani 1 1 d . . . . .
N2 N 0.56257(7) 0.39386(6) 0.85230(9) 0.0210(3) Uani 1 1 d . . . . .
N3 N 0.66960(7) 0.49992(6) 0.90141(9) 0.0213(3) Uani 1 1 d . . . . .
N4 N 0.60250(7) 0.45844(6) 0.77201(9) 0.0211(3) Uani 1 1 d . . . . .
N5 N 0.67855(8) 0.36524(6) 0.90427(9) 0.0227(3) Uani 1 1 d . . . . .
N6 N 0.72320(7) 0.43628(6) 0.80817(9) 0.0214(3) Uani 1 1 d . . . . .
N7 N 0.62855(8) 0.44425(6) 1.07683(9) 0.0268(3) Uani 1 1 d . . . . .
N8 N 0.52414(7) 0.37013(6) 0.91211(9) 0.0230(3) Uani 1 1 d . . . . .
N9 N 0.69405(7) 0.54623(6) 0.94274(9) 0.0218(3) Uani 1 1 d . . . . .
N10 N 0.56519(8) 0.46776(6) 0.69279(10) 0.0260(3) Uani 1 1 d . . . . .
N11 N 0.68757(8) 0.31535(6) 0.94205(10) 0.0263(3) Uani 1 1 d . . . . .
N12 N 0.83119(8) 0.51832(6) 0.60288(9) 0.0229(3) Uani 1 1 d . . . . .
N13 N 0.89650(8) 0.44937(6) 0.69759(9) 0.0232(3) Uani 1 1 d . . . . .
N14 N 0.84850(8) 0.46602(6) 0.48457(9) 0.0236(3) Uani 1 1 d . . . . .
N15 N 0.91519(7) 0.39834(6) 0.58474(9) 0.0222(3) Uani 1 1 d . . . . .
N16 N 0.79111(8) 0.39133(6) 0.54206(10) 0.0236(3) Uani 1 1 d . . . . .
N17 N 0.77202(8) 0.44664(6) 0.67388(9) 0.0227(3) Uani 1 1 d . . . . .
N18 N 0.81341(8) 0.57113(6) 0.58124(10) 0.0264(3) Uani 1 1 d . . . . .
N19 N 0.94028(9) 0.44472(6) 0.77307(10) 0.0291(3) Uani 1 1 d . . . . .
N20 N 0.84443(9) 0.49020(7) 0.40238(10) 0.0332(4) Uani 1 1 d . . . . .
N21 N 0.93923(8) 0.38498(6) 0.50617(9) 0.0248(3) Uani 1 1 d . . . . .
N22 N 0.76569(9) 0.35117(7) 0.48735(12) 0.0345(4) Uani 1 1 d . . . . .
C1 C 0.60535(9) 0.47686(7) 0.92897(11) 0.0216(3) Uani 1 1 d . . . . .
H1 H 0.576725 0.503478 0.958381 0.026 Uiso 1 1 calc R U . . .
C2 C 0.56359(9) 0.45141(7) 0.84729(11) 0.0210(3) Uani 1 1 d . . . . .
H2 H 0.515582 0.466388 0.838466 0.025 Uiso 1 1 calc R U . . .
C3 C 0.72081(9) 0.45581(7) 0.89464(11) 0.0219(3) Uani 1 1 d . . . . .
H3 H 0.768158 0.467774 0.916914 0.026 Uiso 1 1 calc R U . . .
C4 C 0.69335(9) 0.41179(7) 0.95549(11) 0.0225(3) Uani 1 1 d . . . . .
H4 H 0.728280 0.404032 1.004421 0.027 Uiso 1 1 calc R U . . .
C5 C 0.65712(9) 0.41634(7) 0.77241(11) 0.0212(3) Uani 1 1 d . . . . .
H5 H 0.661732 0.402963 0.712564 0.025 Uiso 1 1 calc R U . . .
C6 C 0.62970(9) 0.37129(7) 0.83014(11) 0.0216(3) Uani 1 1 d . . . . .
H6 H 0.623143 0.337345 0.797462 0.026 Uiso 1 1 calc R U . . .
C7 C 0.75336(9) 0.47460(7) 0.75096(11) 0.0235(3) Uani 1 1 d . . . . .
H7A H 0.719252 0.502891 0.735230 0.028 Uiso 1 1 calc R U . . .
H7B H 0.795190 0.491084 0.780255 0.028 Uiso 1 1 calc R U . . .
C8 C 0.92747(9) 0.45243(7) 0.61569(11) 0.0231(3) Uani 1 1 d . . . . .
H8 H 0.978258 0.460804 0.623053 0.028 Uiso 1 1 calc R U . . .
C9 C 0.88616(9) 0.49472(7) 0.55544(11) 0.0228(3) Uani 1 1 d . . . . .
H9 H 0.917952 0.522202 0.533669 0.027 Uiso 1 1 calc R U . . .
C10 C 0.83394(9) 0.41509(7) 0.68812(11) 0.0224(3) Uani 1 1 d . . . . .
H10 H 0.830838 0.392431 0.740440 0.027 Uiso 1 1 calc R U . . .
C11 C 0.84582(9) 0.37983(7) 0.60741(11) 0.0225(3) Uani 1 1 d . . . . .
H11 H 0.846692 0.341357 0.622674 0.027 Uiso 1 1 calc R U . . .
C12 C 0.77197(9) 0.47968(7) 0.59894(11) 0.0227(3) Uani 1 1 d . . . . .
H12 H 0.726821 0.499199 0.591142 0.027 Uiso 1 1 calc R U . . .
C13 C 0.78316(9) 0.44578(7) 0.51663(11) 0.0240(3) Uani 1 1 d . . . . .
H13 H 0.743414 0.450224 0.472398 0.029 Uiso 1 1 calc R U . . .
O21 O 0.60762(8) 0.74389(6) 1.10718(8) 0.0336(3) Uani 1 1 d . . . . .
O22 O 0.61781(7) 0.81931(5) 1.04140(9) 0.0299(3) Uani 1 1 d . . . . .
O23 O 0.43255(7) 0.66404(6) 0.87274(10) 0.0376(3) Uani 1 1 d . . . . .
O24 O 0.43389(7) 0.73045(6) 0.78270(10) 0.0375(3) Uani 1 1 d . . . . .
O25 O 0.73078(7) 0.65950(5) 1.07693(8) 0.0290(3) Uani 1 1 d . . . . .
O26 O 0.80799(6) 0.67873(5) 0.98582(8) 0.0258(3) Uani 1 1 d . . . . .
O27 O 0.54183(11) 0.82573(7) 0.73095(12) 0.0377(4) Uani 0.860(3) 1 d D . P A 1
O27A O 0.5114(7) 0.8193(4) 0.7614(8) 0.0377(4) Uani 0.140(3) 1 d D . P A 2
O28 O 0.59612(16) 0.85953(10) 0.84786(14) 0.0377(4) Uani 0.860(3) 1 d D . P A 1
O28A O 0.5940(11) 0.8637(6) 0.8288(9) 0.0377(4) Uani 0.140(3) 1 d D . P A 2
O29 O 0.93339(8) 0.85340(6) 0.61948(9) 0.0344(3) Uani 1 1 d . . . . .
O30 O 0.97573(8) 0.79474(6) 0.53447(9) 0.0365(3) Uani 1 1 d . . . . .
O31 O 1.08243(8) 0.70706(7) 0.86918(10) 0.0406(4) Uani 1 1 d . . . . .
O32 O 1.09956(7) 0.66674(7) 0.74858(11) 0.0430(4) Uani 1 1 d . . . . .
O33 O 0.75200(6) 0.71922(5) 0.55100(8) 0.0260(3) Uani 1 1 d . . . . .
O34 O 0.84535(7) 0.70712(5) 0.48186(8) 0.0268(3) Uani 1 1 d . . . . .
O35 O 0.88050(7) 0.56704(5) 0.79073(9) 0.0302(3) Uani 1 1 d . . . . .
O36 O 0.96609(7) 0.56690(5) 0.70561(9) 0.0309(3) Uani 1 1 d . . . . .
O37 O 0.98800(7) 0.79993(6) 0.91558(9) 0.0334(3) Uani 1 1 d . . . . .
O38 O 0.93825(8) 0.85525(6) 0.82347(9) 0.0353(3) Uani 1 1 d . . . . .
O39 O 0.61880(7) 0.58015(5) 0.72125(8) 0.0259(3) Uani 1 1 d . . . . .
O40 O 0.54858(6) 0.56640(5) 0.82337(8) 0.0243(2) Uani 1 1 d . . . . .
N23 N 0.61212(7) 0.74488(6) 0.96409(9) 0.0212(3) Uani 1 1 d . . . . .
N24 N 0.53282(7) 0.70294(6) 0.84816(9) 0.0230(3) Uani 1 1 d . . . . .
N25 N 0.69584(7) 0.68263(6) 0.94132(8) 0.0186(3) Uani 1 1 d . . . . .
N26 N 0.61460(7) 0.63971(6) 0.82591(8) 0.0198(3) Uani 1 1 d . . . . .
N27 N 0.60838(8) 0.77435(6) 0.81671(9) 0.0218(3) Uani 1 1 d D . . . .
N28 N 0.69999(7) 0.70584(6) 0.79047(8) 0.0182(3) Uani 1 1 d . . . . .
N29 N 0.61371(8) 0.77123(6) 1.04361(9) 0.0240(3) Uani 1 1 d . . . . .
N30 N 0.46169(8) 0.69817(7) 0.83226(10) 0.0289(3) Uani 1 1 d . . . . .
N31 N 0.74795(8) 0.67369(6) 1.00670(9) 0.0223(3) Uani 1 1 d . . . . .
N32 N 0.59125(7) 0.59288(6) 0.78663(9) 0.0210(3) Uani 1 1 d . . . . .
N33 N 0.57841(10) 0.82319(7) 0.79830(11) 0.0351(4) Uani 1 1 d . . . . .
N34 N 0.93787(8) 0.76844(6) 0.65947(9) 0.0239(3) Uani 1 1 d . . . . .
N35 N 0.99682(7) 0.70332(6) 0.76583(9) 0.0246(3) Uani 1 1 d . . . . .
N36 N 0.85276(7) 0.70715(6) 0.62642(9) 0.0208(3) Uani 1 1 d . . . . .
N37 N 0.91151(7) 0.64278(6) 0.73231(9) 0.0220(3) Uani 1 1 d . . . . .
N38 N 0.91544(8) 0.76867(6) 0.80963(9) 0.0238(3) Uani 1 1 d . . . . .
N39 N 0.82045(7) 0.70210(6) 0.77422(9) 0.0199(3) Uani 1 1 d . . . . .
N40 N 0.94835(8) 0.80852(7) 0.59940(10) 0.0284(3) Uani 1 1 d . . . . .
N41 N 1.06391(8) 0.69077(7) 0.79765(11) 0.0322(4) Uani 1 1 d . . . . .
N42 N 0.81500(8) 0.71221(6) 0.54746(9) 0.0218(3) Uani 1 1 d . . . . .
N43 N 0.92132(8) 0.58897(6) 0.74486(9) 0.0238(3) Uani 1 1 d . . . . .
N44 N 0.95062(8) 0.81116(6) 0.85172(10) 0.0275(3) Uani 1 1 d . . . . .
C14 C 0.62446(8) 0.68786(7) 0.96546(10) 0.0203(3) Uani 1 1 d . . . . .
H14 H 0.618274 0.672331 1.023579 0.024 Uiso 1 1 calc R U . . .
C15 C 0.57339(8) 0.66154(7) 0.89297(10) 0.0209(3) Uani 1 1 d . . . . .
H15 H 0.542961 0.634067 0.917389 0.025 Uiso 1 1 calc R U . . .
C16 C 0.65197(8) 0.76814(7) 0.89513(10) 0.0200(3) Uani 1 1 d . . . . .
H16 H 0.673980 0.802488 0.913869 0.024 Uiso 1 1 calc R U . . .
C17 C 0.70824(8) 0.72538(6) 0.87790(10) 0.0188(3) Uani 1 1 d . . . . .
H17 H 0.755905 0.740533 0.889636 0.023 Uiso 1 1 calc R U . . .
C18 C 0.57442(9) 0.72715(7) 0.78293(10) 0.0212(3) Uani 1 1 d . . . . .
H18 H 0.545427 0.734678 0.728496 0.025 Uiso 1 1 calc R U . . .
C19 C 0.63201(8) 0.68461(7) 0.76811(10) 0.0195(3) Uani 1 1 d . . . . .
H19 H 0.628537 0.672723 0.706638 0.023 Uiso 1 1 calc R U . . .
C20 C 0.96494(9) 0.67362(7) 0.69345(11) 0.0232(3) Uani 1 1 d . . . . .
H20 H 0.999295 0.650619 0.665787 0.028 Uiso 1 1 calc R U . . .
C21 C 0.92789(9) 0.71433(7) 0.62695(11) 0.0224(3) Uani 1 1 d . . . . .
H21 H 0.944870 0.710260 0.567993 0.027 Uiso 1 1 calc R U . . .
C22 C 0.94342(9) 0.71614(7) 0.82558(11) 0.0236(3) Uani 1 1 d . . . . .
H22 H 0.961971 0.712132 0.886869 0.028 Uiso 1 1 calc R U . . .
C23 C 0.88331(8) 0.67500(7) 0.80226(10) 0.0208(3) Uani 1 1 d . . . . .
H23 H 0.875454 0.652156 0.853202 0.025 Uiso 1 1 calc R U . . .
C24 C 0.88613(9) 0.77850(7) 0.72300(11) 0.0228(3) Uani 1 1 d . . . . .
H24 H 0.867317 0.815331 0.717281 0.027 Uiso 1 1 calc R U . . .
C25 C 0.82746(9) 0.73653(7) 0.70202(10) 0.0208(3) Uani 1 1 d . . . . .
H25 H 0.782266 0.754547 0.685589 0.025 Uiso 1 1 calc R U . . .
C26 C 0.75680(8) 0.67070(7) 0.76963(11) 0.0204(3) Uani 1 1 d . . . . .
H26A H 0.761182 0.641022 0.811234 0.025 Uiso 1 1 calc R U . . .
H26B H 0.747702 0.655869 0.711017 0.025 Uiso 1 1 calc R U . . .
O41 O 0.8508(5) 0.3834(6) 0.9857(9) 0.077(5) Uani 0.189(7) 1 d G . P . .
H41A H 0.876819 0.395258 0.946414 0.115 Uiso 0.189(7) 1 d G U P . .
H41B H 0.878617 0.363854 1.018837 0.115 Uiso 0.189(7) 1 d G U P . .
N50 N 0.08762(11) 0.81200(9) 0.73019(13) 0.0458(5) Uani 1 1 d . . . . .
C50 C 0.10955(11) 0.79904(10) 0.66837(16) 0.0413(5) Uani 1 1 d . . . . .
C51 C 0.13710(17) 0.7819(2) 0.5878(3) 0.0892(13) Uani 1 1 d . U . . .
H51A H 0.143094 0.812689 0.550769 0.134 Uiso 1 1 calc R U . . .
H51B H 0.104560 0.756911 0.558389 0.134 Uiso 1 1 calc R U . . .
H51C H 0.182144 0.764471 0.600239 0.134 Uiso 1 1 calc R U . . .
N51 N 0.43780(12) 0.64468(9) 0.36352(15) 0.0407(5) Uani 0.860(3) 1 d . . P A 1
C52 C 0.42562(12) 0.67388(9) 0.41651(15) 0.0322(5) Uani 0.860(3) 1 d . . P A 1
C53 C 0.40997(17) 0.71088(11) 0.48267(17) 0.0436(6) Uani 0.860(3) 1 d . . P A 1
H53A H 0.367135 0.730045 0.464915 0.065 Uiso 0.860(3) 1 calc R U P A 1
H53B H 0.448408 0.736110 0.491856 0.065 Uiso 0.860(3) 1 calc R U P A 1
H53C H 0.403692 0.691698 0.536357 0.065 Uiso 0.860(3) 1 calc R U P A 1
N52 N 0.48457(10) 0.64335(8) 0.66892(13) 0.0426(4) Uani 1 1 d . . . . .
C54 C 0.44233(12) 0.61172(9) 0.67481(13) 0.0367(5) Uani 1 1 d . . . . .
C55 C 0.38944(12) 0.57098(10) 0.68367(15) 0.0420(5) Uani 1 1 d . . . . .
H55A H 0.383596 0.550413 0.630232 0.063 Uiso 1 1 calc R U . . .
H55B H 0.345180 0.587801 0.695136 0.063 Uiso 1 1 calc R U . . .
H55C H 0.404075 0.547404 0.731577 0.063 Uiso 1 1 calc R U . . .
N53 N 0.32718(14) 0.46664(10) 0.54758(14) 0.0563(6) Uani 1 1 d . . . . .
C56 C 0.37935(14) 0.45128(9) 0.52517(14) 0.0422(5) Uani 1 1 d . . . . .
C57 C 0.44426(13) 0.43229(9) 0.49584(15) 0.0392(5) Uani 1 1 d . . . . .
H57A H 0.434913 0.409098 0.445872 0.059 Uiso 1 1 calc R U . . .
H57B H 0.469456 0.412436 0.542263 0.059 Uiso 1 1 calc R U . . .
H57C H 0.472517 0.462455 0.479455 0.059 Uiso 1 1 calc R U . . .
N54 N 0.73120(11) 0.18877(8) 0.20449(14) 0.0458(5) Uani 1 1 d . . . . .
C58 C 0.73195(10) 0.23378(9) 0.21284(14) 0.0346(4) Uani 1 1 d . . . . .
C59 C 0.73380(12) 0.29068(9) 0.22443(16) 0.0399(5) Uani 1 1 d . . . . .
H59A H 0.700063 0.307319 0.182811 0.060 Uiso 1 1 calc R U . . .
H59B H 0.780570 0.303843 0.215261 0.060 Uiso 1 1 calc R U . . .
H59C H 0.722034 0.299397 0.283080 0.060 Uiso 1 1 calc R U . . .
N55 N 0.77867(12) 0.48879(9) 0.07856(13) 0.0492(5) Uani 1 1 d . . . . .
C60 C 0.82138(13) 0.47454(10) 0.12814(15) 0.0432(5) Uani 1 1 d . . . . .
C61 C 0.87582(15) 0.45640(14) 0.19007(19) 0.0613(7) Uani 1 1 d . . . . .
H61A H 0.914669 0.442409 0.159490 0.092 Uiso 1 1 calc R U . . .
H61B H 0.857503 0.428439 0.225899 0.092 Uiso 1 1 calc R U . . .
H61C H 0.892099 0.486071 0.226729 0.092 Uiso 1 1 calc R U . . .
N56 N 0.75571(11) 0.66169(8) 0.29060(13) 0.0421(4) Uani 1 1 d . . . . .
C62 C 0.73188(13) 0.62266(10) 0.26530(14) 0.0415(5) Uani 1 1 d . . . . .
C63 C 0.69920(19) 0.57360(10) 0.23198(17) 0.0585(7) Uani 1 1 d . . . . .
H63A H 0.725428 0.559749 0.185093 0.088 Uiso 1 1 calc R U . . .
H63B H 0.651222 0.580963 0.210241 0.088 Uiso 1 1 calc R U . . .
H63C H 0.699125 0.547344 0.278367 0.088 Uiso 1 1 calc R U . . .
N57 N 1.00076(11) 0.60600(8) 0.91173(13) 0.0432(4) Uani 1 1 d . . . . .
C64 C 0.96985(12) 0.57961(10) 0.95354(15) 0.0415(5) Uani 1 1 d . . . . .
C65 C 0.92706(14) 0.54585(11) 1.00548(17) 0.0494(6) Uani 1 1 d . . . . .
H65A H 0.920832 0.511164 0.977736 0.074 Uiso 1 1 calc R U . . .
H65B H 0.881529 0.562468 1.010302 0.074 Uiso 1 1 calc R U . . .
H65C H 0.950218 0.541346 1.063096 0.074 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 N7 1.225(2) . ?
O2 N7 1.213(2) . ?
O3 N8 1.232(2) . ?
O4 N8 1.222(2) . ?
O5 N9 1.225(2) . ?
O6 N9 1.2242(19) . ?
O7 N10 1.218(2) . ?
O8 N10 1.226(2) . ?
O9 N11 1.220(2) . ?
O10 N11 1.218(2) . ?
O11 N18 1.223(2) . ?
O12 N18 1.218(2) . ?
O13 N19 1.227(2) . ?
O14 N19 1.215(2) . ?
O15 N20 1.221(2) . ?
O16 N20 1.215(2) . ?
O17 N21 1.224(2) . ?
O18 N21 1.220(2) . ?
O19 N22 1.218(2) . ?
O20 N22 1.212(2) . ?
N1 N7 1.421(2) . ?
N1 C1 1.463(2) . ?
N1 C4 1.479(2) . ?
N2 N8 1.366(2) . ?
N2 C2 1.456(2) . ?
N2 C6 1.476(2) . ?
N3 N9 1.400(2) . ?
N3 C1 1.459(2) . ?
N3 C3 1.497(2) . ?
N4 N10 1.403(2) . ?
N4 C2 1.444(2) . ?
N4 C5 1.496(2) . ?
N5 N11 1.396(2) . ?
N5 C4 1.438(2) . ?
N5 C6 1.445(2) . ?
N6 C3 1.436(2) . ?
N6 C5 1.445(2) . ?
N6 C7 1.462(2) . ?
N12 N18 1.412(2) . ?
N12 C9 1.459(2) . ?
N12 C12 1.499(2) . ?
N13 N19 1.403(2) . ?
N13 C8 1.446(2) . ?
N13 C10 1.483(2) . ?
N14 N20 1.414(2) . ?
N14 C9 1.469(2) . ?
N14 C13 1.477(2) . ?
N15 N21 1.378(2) . ?
N15 C8 1.462(2) . ?
N15 C11 1.481(2) . ?
N16 N22 1.391(2) . ?
N16 C11 1.443(2) . ?
N16 C13 1.436(2) . ?
N17 C7 1.457(2) . ?
N17 C10 1.439(2) . ?
N17 C12 1.433(2) . ?
C1 H1 1.0000 . ?
C1 C2 1.592(2) . ?
C2 H2 1.0000 . ?
C3 H3 1.0000 . ?
C3 C4 1.575(2) . ?
C4 H4 1.0000 . ?
C5 H5 1.0000 . ?
C5 C6 1.564(2) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8 1.0000 . ?
C8 C9 1.597(2) . ?
C9 H9 1.0000 . ?
C10 H10 1.0000 . ?
C10 C11 1.569(2) . ?
C11 H11 1.0000 . ?
C12 H12 1.0000 . ?
C12 C13 1.567(2) . ?
C13 H13 1.0000 . ?
O21 N29 1.218(2) . ?
O22 N29 1.217(2) . ?
O23 N30 1.226(2) . ?
O24 N30 1.220(2) . ?
O25 N31 1.217(2) . ?
O26 N31 1.229(2) . ?
O27 N33 1.224(2) . ?
O27A N33 1.380(12) . ?
O28 N33 1.232(3) . ?
O28A N33 1.160(17) . ?
O29 N40 1.215(2) . ?
O30 N40 1.222(2) . ?
O31 N41 1.217(2) . ?
O32 N41 1.222(2) . ?
O33 N42 1.232(2) . ?
O34 N42 1.217(2) . ?
O35 N43 1.229(2) . ?
O36 N43 1.225(2) . ?
O37 N44 1.219(2) . ?
O38 N44 1.214(2) . ?
O39 N32 1.2221(19) . ?
O40 N32 1.2305(19) . ?
N23 N29 1.4030(19) . ?
N23 C14 1.459(2) . ?
N23 C16 1.483(2) . ?
N24 N30 1.381(2) . ?
N24 C15 1.454(2) . ?
N24 C18 1.469(2) . ?
N25 N31 1.3976(19) . ?
N25 C14 1.456(2) . ?
N25 C17 1.493(2) . ?
N26 N32 1.392(2) . ?
N26 C15 1.462(2) . ?
N26 C19 1.499(2) . ?
N27 N33 1.383(2) . ?
N27 C16 1.441(2) . ?
N27 C18 1.441(2) . ?
N28 C17 1.445(2) . ?
N28 C19 1.436(2) . ?
N28 C26 1.463(2) . ?
N34 N40 1.402(2) . ?
N34 C21 1.465(2) . ?
N34 C24 1.473(2) . ?
N35 N41 1.389(2) . ?
N35 C20 1.453(2) . ?
N35 C22 1.469(2) . ?
N36 N42 1.3897(19) . ?
N36 C21 1.458(2) . ?
N36 C25 1.500(2) . ?
N37 N43 1.384(2) . ?
N37 C20 1.455(2) . ?
N37 C23 1.491(2) . ?
N38 N44 1.407(2) . ?
N38 C22 1.447(2) . ?
N38 C24 1.446(2) . ?
N39 C23 1.433(2) . ?
N39 C25 1.434(2) . ?
N39 C26 1.458(2) . ?
C14 H14 1.0000 . ?
C14 C15 1.590(2) . ?
C15 H15 1.0000 . ?
C16 H16 1.0000 . ?
C16 C17 1.566(2) . ?
C17 H17 1.0000 . ?
C18 H18 1.0000 . ?
C18 C19 1.573(2) . ?
C19 H19 1.0000 . ?
C20 H20 1.0000 . ?
C20 C21 1.592(2) . ?
C21 H21 1.0000 . ?
C22 H22 1.0000 . ?
C22 C23 1.579(2) . ?
C23 H23 1.0000 . ?
C24 H24 1.0000 . ?
C24 C25 1.567(2) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
O41 H41A 0.8700 . ?
O41 H41B 0.8700 . ?
N50 C50 1.125(3) . ?
C50 C51 1.460(4) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
N51 C52 1.142(3) . ?
C52 C53 1.437(4) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
N52 C54 1.148(3) . ?
C54 C55 1.461(3) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
N53 C56 1.153(4) . ?
C56 C57 1.442(4) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
N54 C58 1.144(3) . ?
C58 C59 1.448(3) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
N55 C60 1.147(3) . ?
C60 C61 1.449(4) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
N56 C62 1.145(3) . ?
C62 C63 1.468(4) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
N57 C64 1.129(3) . ?
C64 C65 1.467(4) . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 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
N7 N1 C1 116.68(14) . . ?
N7 N1 C4 117.02(13) . . ?
C1 N1 C4 107.78(13) . . ?
N8 N2 C2 118.95(14) . . ?
N8 N2 C6 120.95(14) . . ?
C2 N2 C6 110.96(13) . . ?
N9 N3 C1 117.64(13) . . ?
N9 N3 C3 116.82(13) . . ?
C1 N3 C3 107.49(13) . . ?
N10 N4 C2 118.00(14) . . ?
N10 N4 C5 116.15(13) . . ?
C2 N4 C5 108.29(13) . . ?
N11 N5 C4 119.35(14) . . ?
N11 N5 C6 119.12(14) . . ?
C4 N5 C6 116.70(14) . . ?
C3 N6 C5 113.34(13) . . ?
C3 N6 C7 112.49(14) . . ?
C5 N6 C7 111.90(14) . . ?
O1 N7 N1 116.16(15) . . ?
O2 N7 O1 127.19(16) . . ?
O2 N7 N1 116.39(15) . . ?
O3 N8 N2 116.12(14) . . ?
O4 N8 O3 126.26(15) . . ?
O4 N8 N2 117.60(14) . . ?
O5 N9 N3 117.60(14) . . ?
O6 N9 O5 126.09(15) . . ?
O6 N9 N3 116.07(14) . . ?
O7 N10 O8 126.62(15) . . ?
O7 N10 N4 118.05(15) . . ?
O8 N10 N4 115.13(15) . . ?
O9 N11 N5 116.62(15) . . ?
O10 N11 O9 126.55(16) . . ?
O10 N11 N5 116.71(14) . . ?
N18 N12 C9 115.98(14) . . ?
N18 N12 C12 115.69(13) . . ?
C9 N12 C12 106.88(13) . . ?
N19 N13 C8 118.77(14) . . ?
N19 N13 C10 118.18(14) . . ?
C8 N13 C10 109.00(13) . . ?
N20 N14 C9 117.36(15) . . ?
N20 N14 C13 117.33(14) . . ?
C9 N14 C13 107.81(13) . . ?
N21 N15 C8 117.64(14) . . ?
N21 N15 C11 119.84(14) . . ?
C8 N15 C11 110.16(13) . . ?
N22 N16 C11 119.60(15) . . ?
N22 N16 C13 120.20(15) . . ?
C13 N16 C11 116.47(14) . . ?
C10 N17 C7 112.97(14) . . ?
C12 N17 C7 113.63(14) . . ?
C12 N17 C10 113.67(13) . . ?
O11 N18 N12 115.86(15) . . ?
O12 N18 O11 126.32(16) . . ?
O12 N18 N12 117.60(15) . . ?
O13 N19 N13 115.15(16) . . ?
O14 N19 O13 126.62(16) . . ?
O14 N19 N13 118.08(16) . . ?
O15 N20 N14 116.41(16) . . ?
O16 N20 O15 127.42(17) . . ?
O16 N20 N14 115.97(17) . . ?
O17 N21 N15 116.23(15) . . ?
O18 N21 O17 126.24(15) . . ?
O18 N21 N15 117.51(15) . . ?
O19 N22 N16 115.88(17) . . ?
O20 N22 O19 126.30(18) . . ?
O20 N22 N16 117.66(16) . . ?
N1 C1 H1 111.8 . . ?
N1 C1 C2 108.10(13) . . ?
N3 C1 N1 104.26(13) . . ?
N3 C1 H1 111.8 . . ?
N3 C1 C2 108.61(13) . . ?
C2 C1 H1 111.8 . . ?
N2 C2 C1 111.61(13) . . ?
N2 C2 H2 111.7 . . ?
N4 C2 N2 100.12(13) . . ?
N4 C2 C1 109.60(13) . . ?
N4 C2 H2 111.7 . . ?
C1 C2 H2 111.7 . . ?
N3 C3 H3 109.9 . . ?
N3 C3 C4 103.45(13) . . ?
N6 C3 N3 112.65(13) . . ?
N6 C3 H3 109.9 . . ?
N6 C3 C4 110.75(14) . . ?
C4 C3 H3 109.9 . . ?
N1 C4 C3 104.98(13) . . ?
N1 C4 H4 111.1 . . ?
N5 C4 N1 110.66(14) . . ?
N5 C4 C3 107.82(13) . . ?
N5 C4 H4 111.1 . . ?
C3 C4 H4 111.1 . . ?
N4 C5 H5 110.1 . . ?
N4 C5 C6 104.72(13) . . ?
N6 C5 N4 110.81(13) . . ?
N6 C5 H5 110.1 . . ?
N6 C5 C6 110.86(13) . . ?
C6 C5 H5 110.1 . . ?
N2 C6 C5 100.91(13) . . ?
N2 C6 H6 111.6 . . ?
N5 C6 N2 112.80(14) . . ?
N5 C6 C5 107.93(13) . . ?
N5 C6 H6 111.6 . . ?
C5 C6 H6 111.6 . . ?
N6 C7 H7A 110.1 . . ?
N6 C7 H7B 110.1 . . ?
N17 C7 N6 108.13(14) . . ?
N17 C7 H7A 110.1 . . ?
N17 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
N13 C8 N15 99.96(14) . . ?
N13 C8 H8 111.7 . . ?
N13 C8 C9 109.49(14) . . ?
N15 C8 H8 111.7 . . ?
N15 C8 C9 111.63(13) . . ?
C9 C8 H8 111.7 . . ?
N12 C9 N14 104.05(14) . . ?
N12 C9 C8 109.04(13) . . ?
N12 C9 H9 111.8 . . ?
N14 C9 C8 108.14(14) . . ?
N14 C9 H9 111.8 . . ?
C8 C9 H9 111.8 . . ?
N13 C10 H10 110.3 . . ?
N13 C10 C11 104.38(13) . . ?
N17 C10 N13 110.60(14) . . ?
N17 C10 H10 110.3 . . ?
N17 C10 C11 110.86(14) . . ?
C11 C10 H10 110.3 . . ?
N15 C11 C10 101.25(13) . . ?
N15 C11 H11 111.2 . . ?
N16 C11 N15 113.35(14) . . ?
N16 C11 C10 108.06(13) . . ?
N16 C11 H11 111.2 . . ?
C10 C11 H11 111.2 . . ?
N12 C12 H12 109.7 . . ?
N12 C12 C13 103.99(13) . . ?
N17 C12 N12 112.80(14) . . ?
N17 C12 H12 109.7 . . ?
N17 C12 C13 110.74(14) . . ?
C13 C12 H12 109.7 . . ?
N14 C13 C12 104.78(14) . . ?
N14 C13 H13 111.0 . . ?
N16 C13 N14 110.31(14) . . ?
N16 C13 C12 108.42(14) . . ?
N16 C13 H13 111.0 . . ?
C12 C13 H13 111.0 . . ?
N29 N23 C14 117.48(13) . . ?
N29 N23 C16 117.96(13) . . ?
C14 N23 C16 108.03(13) . . ?
N30 N24 C15 121.15(15) . . ?
N30 N24 C18 119.63(14) . . ?
C15 N24 C18 109.23(13) . . ?
N31 N25 C14 118.10(13) . . ?
N31 N25 C17 117.26(13) . . ?
C14 N25 C17 107.56(12) . . ?
N32 N26 C15 117.31(13) . . ?
N32 N26 C19 117.27(12) . . ?
C15 N26 C19 107.32(13) . . ?
N33 N27 C16 118.87(14) . . ?
N33 N27 C18 119.29(14) . . ?
C16 N27 C18 116.23(13) . . ?
C17 N28 C26 112.34(13) . . ?
C19 N28 C17 113.27(13) . . ?
C19 N28 C26 113.82(13) . . ?
O21 N29 N23 116.70(15) . . ?
O22 N29 O21 126.75(15) . . ?
O22 N29 N23 116.46(14) . . ?
O23 N30 N24 116.94(15) . . ?
O24 N30 O23 126.69(16) . . ?
O24 N30 N24 116.24(16) . . ?
O25 N31 O26 125.90(14) . . ?
O25 N31 N25 118.34(14) . . ?
O26 N31 N25 115.67(14) . . ?
O39 N32 O40 125.87(15) . . ?
O39 N32 N26 116.30(14) . . ?
O40 N32 N26 117.64(13) . . ?
O27 N33 O28 127.97(18) . . ?
O27 N33 N27 115.58(16) . . ?
O27A N33 N27 112.8(5) . . ?
O28 N33 N27 116.17(16) . . ?
O28A N33 O27A 116.2(10) . . ?
O28A N33 N27 127.6(8) . . ?
N40 N34 C21 117.70(14) . . ?
N40 N34 C24 117.25(14) . . ?
C21 N34 C24 108.27(13) . . ?
N41 N35 C20 119.46(15) . . ?
N41 N35 C22 120.00(14) . . ?
C20 N35 C22 109.06(13) . . ?
N42 N36 C21 116.93(13) . . ?
N42 N36 C25 117.96(13) . . ?
C21 N36 C25 108.05(13) . . ?
N43 N37 C20 119.37(14) . . ?
N43 N37 C23 119.09(13) . . ?
C20 N37 C23 108.35(13) . . ?
N44 N38 C22 117.23(14) . . ?
N44 N38 C24 116.59(14) . . ?
C24 N38 C22 115.73(14) . . ?
C23 N39 C25 113.89(13) . . ?
C23 N39 C26 116.48(13) . . ?
C25 N39 C26 114.55(13) . . ?
O29 N40 O30 126.99(17) . . ?
O29 N40 N34 117.02(15) . . ?
O30 N40 N34 115.82(16) . . ?
O31 N41 O32 126.64(17) . . ?
O31 N41 N35 117.13(17) . . ?
O32 N41 N35 116.11(16) . . ?
O33 N42 N36 115.56(14) . . ?
O34 N42 O33 125.76(14) . . ?
O34 N42 N36 118.60(14) . . ?
O35 N43 N37 115.94(14) . . ?
O36 N43 O35 125.81(16) . . ?
O36 N43 N37 118.07(14) . . ?
O37 N44 N38 116.14(15) . . ?
O38 N44 O37 126.73(16) . . ?
O38 N44 N38 117.03(15) . . ?
N23 C14 H14 111.8 . . ?
N23 C14 C15 108.04(13) . . ?
N25 C14 N23 103.98(13) . . ?
N25 C14 H14 111.8 . . ?
N25 C14 C15 109.17(13) . . ?
C15 C14 H14 111.8 . . ?
N24 C15 N26 103.27(13) . . ?
N24 C15 C14 108.99(14) . . ?
N24 C15 H15 111.8 . . ?
N26 C15 C14 108.88(13) . . ?
N26 C15 H15 111.8 . . ?
C14 C15 H15 111.8 . . ?
N23 C16 H16 111.3 . . ?
N23 C16 C17 104.47(13) . . ?
N27 C16 N23 110.78(13) . . ?
N27 C16 H16 111.3 . . ?
N27 C16 C17 107.46(13) . . ?
C17 C16 H16 111.3 . . ?
N25 C17 C16 103.96(12) . . ?
N25 C17 H17 110.0 . . ?
N28 C17 N25 111.27(13) . . ?
N28 C17 C16 111.33(13) . . ?
N28 C17 H17 110.0 . . ?
C16 C17 H17 110.0 . . ?
N24 C18 H18 111.4 . . ?
N24 C18 C19 103.95(13) . . ?
N27 C18 N24 110.36(13) . . ?
N27 C18 H18 111.4 . . ?
N27 C18 C19 108.12(13) . . ?
C19 C18 H18 111.4 . . ?
N26 C19 C18 103.85(13) . . ?
N26 C19 H19 110.1 . . ?
N28 C19 N26 112.02(13) . . ?
N28 C19 C18 110.52(13) . . ?
N28 C19 H19 110.1 . . ?
C18 C19 H19 110.1 . . ?
N35 C20 N37 103.17(13) . . ?
N35 C20 H20 112.1 . . ?
N35 C20 C21 108.48(14) . . ?
N37 C20 H20 112.1 . . ?
N37 C20 C21 108.49(13) . . ?
C21 C20 H20 112.1 . . ?
N34 C21 C20 109.60(14) . . ?
N34 C21 H21 111.7 . . ?
N36 C21 N34 102.98(14) . . ?
N36 C21 C20 108.91(13) . . ?
N36 C21 H21 111.7 . . ?
C20 C21 H21 111.7 . . ?
N35 C22 H22 111.2 . . ?
N35 C22 C23 104.14(13) . . ?
N38 C22 N35 111.25(14) . . ?
N38 C22 H22 111.2 . . ?
N38 C22 C23 107.75(13) . . ?
C23 C22 H22 111.2 . . ?
N37 C23 C22 103.20(13) . . ?
N37 C23 H23 110.2 . . ?
N39 C23 N37 112.41(13) . . ?
N39 C23 C22 110.31(14) . . ?
N39 C23 H23 110.2 . . ?
C22 C23 H23 110.2 . . ?
N34 C24 H24 111.0 . . ?
N34 C24 C25 104.80(13) . . ?
N38 C24 N34 110.89(14) . . ?
N38 C24 H24 111.0 . . ?
N38 C24 C25 107.93(14) . . ?
C25 C24 H24 111.0 . . ?
N36 C25 C24 103.25(13) . . ?
N36 C25 H25 110.4 . . ?
N39 C25 N36 111.55(14) . . ?
N39 C25 C24 110.63(13) . . ?
N39 C25 H25 110.4 . . ?
C24 C25 H25 110.4 . . ?
N28 C26 H26A 110.2 . . ?
N28 C26 H26B 110.2 . . ?
N39 C26 N28 107.41(13) . . ?
N39 C26 H26A 110.2 . . ?
N39 C26 H26B 110.2 . . ?
H26A C26 H26B 108.5 . . ?
H41A O41 H41B 104.5 . . ?
N50 C50 C51 179.2(3) . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N51 C52 C53 179.5(3) . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N52 C54 C55 178.9(2) . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
N53 C56 C57 179.1(2) . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
N54 C58 C59 179.1(3) . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
N55 C60 C61 179.4(3) . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
N56 C62 C63 178.1(3) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
N57 C64 C65 177.6(3) . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 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
N1 C1 C2 N2 -1.84(18) . . . . ?
N1 C1 C2 N4 -111.82(15) . . . . ?
N3 C1 C2 N2 110.71(15) . . . . ?
N3 C1 C2 N4 0.73(18) . . . . ?
N3 C3 C4 N1 2.47(16) . . . . ?
N3 C3 C4 N5 120.48(14) . . . . ?
N4 C5 C6 N2 1.37(15) . . . . ?
N4 C5 C6 N5 -117.13(14) . . . . ?
N6 C3 C4 N1 -118.47(14) . . . . ?
N6 C3 C4 N5 -0.46(18) . . . . ?
N6 C5 C6 N2 120.93(14) . . . . ?
N6 C5 C6 N5 2.42(18) . . . . ?
N7 N1 C1 N3 100.91(15) . . . . ?
N7 N1 C1 C2 -143.65(14) . . . . ?
N7 N1 C4 N5 128.70(15) . . . . ?
N7 N1 C4 C3 -115.23(15) . . . . ?
N8 N2 C2 N4 -173.96(13) . . . . ?
N8 N2 C2 C1 70.11(18) . . . . ?
N8 N2 C6 N5 -56.6(2) . . . . ?
N8 N2 C6 C5 -171.51(14) . . . . ?
N9 N3 C1 N1 -99.53(16) . . . . ?
N9 N3 C1 C2 145.40(14) . . . . ?
N9 N3 C3 N6 -128.39(15) . . . . ?
N9 N3 C3 C4 111.97(15) . . . . ?
N10 N4 C2 N2 98.20(16) . . . . ?
N10 N4 C2 C1 -144.37(14) . . . . ?
N10 N4 C5 N6 127.25(15) . . . . ?
N10 N4 C5 C6 -113.16(15) . . . . ?
N11 N5 C4 N1 -97.84(17) . . . . ?
N11 N5 C4 C3 147.87(14) . . . . ?
N11 N5 C6 N2 100.55(17) . . . . ?
N11 N5 C6 C5 -148.86(14) . . . . ?
N12 C12 C13 N14 2.84(17) . . . . ?
N12 C12 C13 N16 120.62(14) . . . . ?
N13 C8 C9 N12 1.70(19) . . . . ?
N13 C8 C9 N14 -110.84(15) . . . . ?
N13 C10 C11 N15 1.85(16) . . . . ?
N13 C10 C11 N16 -117.49(14) . . . . ?
N15 C8 C9 N12 111.43(15) . . . . ?
N15 C8 C9 N14 -1.11(18) . . . . ?
N17 C10 C11 N15 120.95(14) . . . . ?
N17 C10 C11 N16 1.62(19) . . . . ?
N17 C12 C13 N14 -118.59(15) . . . . ?
N17 C12 C13 N16 -0.81(19) . . . . ?
N18 N12 C9 N14 -95.36(16) . . . . ?
N18 N12 C9 C8 149.44(14) . . . . ?
N18 N12 C12 N17 -132.59(15) . . . . ?
N18 N12 C12 C13 107.37(15) . . . . ?
N19 N13 C8 N15 102.62(16) . . . . ?
N19 N13 C8 C9 -140.05(15) . . . . ?
N19 N13 C10 N17 123.34(15) . . . . ?
N19 N13 C10 C11 -117.38(15) . . . . ?
N20 N14 C9 N12 101.53(16) . . . . ?
N20 N14 C9 C8 -142.63(15) . . . . ?
N20 N14 C13 N16 126.99(16) . . . . ?
N20 N14 C13 C12 -116.51(16) . . . . ?
N21 N15 C8 N13 -178.91(13) . . . . ?
N21 N15 C8 C9 65.36(18) . . . . ?
N21 N15 C11 N16 -51.2(2) . . . . ?
N21 N15 C11 C10 -166.69(14) . . . . ?
N22 N16 C11 N15 102.61(18) . . . . ?
N22 N16 C11 C10 -146.03(16) . . . . ?
N22 N16 C13 N14 -100.21(18) . . . . ?
N22 N16 C13 C12 145.59(16) . . . . ?
C1 N1 N7 O1 29.3(2) . . . . ?
C1 N1 N7 O2 -156.12(16) . . . . ?
C1 N1 C4 N5 -97.45(16) . . . . ?
C1 N1 C4 C3 18.62(17) . . . . ?
C1 N3 N9 O5 -14.0(2) . . . . ?
C1 N3 N9 O6 171.31(14) . . . . ?
C1 N3 C3 N6 96.84(16) . . . . ?
C1 N3 C3 C4 -22.80(16) . . . . ?
C2 N2 N8 O3 19.5(2) . . . . ?
C2 N2 N8 O4 -162.02(14) . . . . ?
C2 N2 C6 N5 89.94(16) . . . . ?
C2 N2 C6 C5 -24.97(16) . . . . ?
C2 N4 N10 O7 12.5(2) . . . . ?
C2 N4 N10 O8 -172.36(15) . . . . ?
C2 N4 C5 N6 -97.25(15) . . . . ?
C2 N4 C5 C6 22.33(17) . . . . ?
C3 N3 N9 O5 -144.18(15) . . . . ?
C3 N3 N9 O6 41.2(2) . . . . ?
C3 N3 C1 N1 34.82(16) . . . . ?
C3 N3 C1 C2 -80.26(16) . . . . ?
C3 N6 C5 N4 58.48(18) . . . . ?
C3 N6 C5 C6 -57.35(18) . . . . ?
C3 N6 C7 N17 163.80(14) . . . . ?
C4 N1 N7 O1 159.12(15) . . . . ?
C4 N1 N7 O2 -26.3(2) . . . . ?
C4 N1 C1 N3 -33.12(16) . . . . ?
C4 N1 C1 C2 82.32(15) . . . . ?
C4 N5 N11 O9 -5.6(2) . . . . ?
C4 N5 N11 O10 178.03(15) . . . . ?
C4 N5 C6 N2 -54.73(19) . . . . ?
C4 N5 C6 C5 55.87(18) . . . . ?
C5 N4 N10 O7 143.54(16) . . . . ?
C5 N4 N10 O8 -41.3(2) . . . . ?
C5 N4 C2 N2 -36.35(16) . . . . ?
C5 N4 C2 C1 81.08(16) . . . . ?
C5 N6 C3 N3 -59.19(18) . . . . ?
C5 N6 C3 C4 56.13(18) . . . . ?
C5 N6 C7 N17 -67.26(17) . . . . ?
C6 N2 N8 O3 163.49(14) . . . . ?
C6 N2 N8 O4 -18.1(2) . . . . ?
C6 N2 C2 N4 38.74(16) . . . . ?
C6 N2 C2 C1 -77.19(16) . . . . ?
C6 N5 N11 O9 -160.23(16) . . . . ?
C6 N5 N11 O10 23.4(2) . . . . ?
C6 N5 C4 N1 57.37(19) . . . . ?
C6 N5 C4 C3 -56.91(18) . . . . ?
C7 N6 C3 N3 69.01(18) . . . . ?
C7 N6 C3 C4 -175.67(13) . . . . ?
C7 N6 C5 N4 -70.02(17) . . . . ?
C7 N6 C5 C6 174.15(13) . . . . ?
C7 N17 C10 N13 -72.66(17) . . . . ?
C7 N17 C10 C11 172.05(14) . . . . ?
C7 N17 C12 N12 71.06(18) . . . . ?
C7 N17 C12 C13 -172.85(14) . . . . ?
C8 N13 N19 O13 -169.99(16) . . . . ?
C8 N13 N19 O14 14.2(2) . . . . ?
C8 N13 C10 N17 -97.03(16) . . . . ?
C8 N13 C10 C11 22.26(17) . . . . ?
C8 N15 N21 O17 23.1(2) . . . . ?
C8 N15 N21 O18 -158.53(15) . . . . ?
C8 N15 C11 N16 90.09(17) . . . . ?
C8 N15 C11 C10 -25.39(17) . . . . ?
C9 N12 N18 O11 165.79(15) . . . . ?
C9 N12 N18 O12 -19.2(2) . . . . ?
C9 N12 C12 N17 96.58(16) . . . . ?
C9 N12 C12 C13 -23.46(16) . . . . ?
C9 N14 N20 O15 29.2(2) . . . . ?
C9 N14 N20 O16 -155.56(18) . . . . ?
C9 N14 C13 N16 -97.83(16) . . . . ?
C9 N14 C13 C12 18.67(17) . . . . ?
C10 N13 N19 O13 -34.3(2) . . . . ?
C10 N13 N19 O14 149.84(16) . . . . ?
C10 N13 C8 N15 -36.74(16) . . . . ?
C10 N13 C8 C9 80.59(16) . . . . ?
C10 N17 C7 N6 -75.34(17) . . . . ?
C10 N17 C12 N12 -60.00(19) . . . . ?
C10 N17 C12 C13 56.09(19) . . . . ?
C11 N15 N21 O17 161.64(15) . . . . ?
C11 N15 N21 O18 -20.0(2) . . . . ?
C11 N15 C8 N13 38.84(16) . . . . ?
C11 N15 C8 C9 -76.89(16) . . . . ?
C11 N16 N22 O19 -166.61(19) . . . . ?
C11 N16 N22 O20 17.6(3) . . . . ?
C11 N16 C13 N14 57.94(19) . . . . ?
C11 N16 C13 C12 -56.26(19) . . . . ?
C12 N12 N18 O11 39.4(2) . . . . ?
C12 N12 N18 O12 -145.58(16) . . . . ?
C12 N12 C9 N14 35.31(16) . . . . ?
C12 N12 C9 C8 -79.89(16) . . . . ?
C12 N17 C7 N6 153.26(14) . . . . ?
C12 N17 C10 N13 58.72(18) . . . . ?
C12 N17 C10 C11 -56.56(19) . . . . ?
C13 N14 N20 O15 160.11(17) . . . . ?
C13 N14 N20 O16 -24.6(2) . . . . ?
C13 N14 C9 N12 -33.64(17) . . . . ?
C13 N14 C9 C8 82.21(16) . . . . ?
C13 N16 N22 O19 -9.1(3) . . . . ?
C13 N16 N22 O20 175.11(17) . . . . ?
C13 N16 C11 N15 -55.68(19) . . . . ?
C13 N16 C11 C10 55.68(19) . . . . ?
N23 C14 C15 N24 1.42(17) . . . . ?
N23 C14 C15 N26 113.41(14) . . . . ?
N23 C16 C17 N25 -1.73(15) . . . . ?
N23 C16 C17 N28 118.16(14) . . . . ?
N24 C18 C19 N26 1.68(15) . . . . ?
N24 C18 C19 N28 -118.63(14) . . . . ?
N25 C14 C15 N24 -111.05(15) . . . . ?
N25 C14 C15 N26 0.93(18) . . . . ?
N27 C16 C17 N25 -119.46(14) . . . . ?
N27 C16 C17 N28 0.43(18) . . . . ?
N27 C18 C19 N26 118.96(13) . . . . ?
N27 C18 C19 N28 -1.35(17) . . . . ?
N29 N23 C14 N25 -103.09(15) . . . . ?
N29 N23 C14 C15 140.99(14) . . . . ?
N29 N23 C16 N27 -127.65(15) . . . . ?
N29 N23 C16 C17 116.92(15) . . . . ?
N30 N24 C15 N26 111.23(16) . . . . ?
N30 N24 C15 C14 -133.12(15) . . . . ?
N30 N24 C18 N27 118.22(16) . . . . ?
N30 N24 C18 C19 -126.06(16) . . . . ?
N31 N25 C14 N23 101.07(15) . . . . ?
N31 N25 C14 C15 -143.81(14) . . . . ?
N31 N25 C17 N28 126.32(14) . . . . ?
N31 N25 C17 C16 -113.75(14) . . . . ?
N32 N26 C15 N24 -99.87(15) . . . . ?
N32 N26 C15 C14 144.40(14) . . . . ?
N32 N26 C19 N28 -128.59(14) . . . . ?
N32 N26 C19 C18 112.12(14) . . . . ?
N33 N27 C16 N23 97.15(18) . . . . ?
N33 N27 C16 C17 -149.30(16) . . . . ?
N33 N27 C18 N24 -97.30(18) . . . . ?
N33 N27 C18 C19 149.62(15) . . . . ?
N34 C24 C25 N36 -0.70(16) . . . . ?
N34 C24 C25 N39 118.76(15) . . . . ?
N35 C20 C21 N34 0.21(18) . . . . ?
N35 C20 C21 N36 -111.75(15) . . . . ?
N35 C22 C23 N37 1.22(16) . . . . ?
N35 C22 C23 N39 -119.07(14) . . . . ?
N37 C20 C21 N34 111.62(15) . . . . ?
N37 C20 C21 N36 -0.34(19) . . . . ?
N38 C22 C23 N37 119.45(14) . . . . ?
N38 C22 C23 N39 -0.84(18) . . . . ?
N38 C24 C25 N36 -118.93(14) . . . . ?
N38 C24 C25 N39 0.52(19) . . . . ?
N40 N34 C21 N36 -101.37(16) . . . . ?
N40 N34 C21 C20 142.85(14) . . . . ?
N40 N34 C24 N38 -128.49(15) . . . . ?
N40 N34 C24 C25 115.31(15) . . . . ?
N41 N35 C20 N37 109.68(16) . . . . ?
N41 N35 C20 C21 -135.39(15) . . . . ?
N41 N35 C22 N38 121.02(17) . . . . ?
N41 N35 C22 C23 -123.18(16) . . . . ?
N42 N36 C21 N34 101.02(15) . . . . ?
N42 N36 C21 C20 -142.69(14) . . . . ?
N42 N36 C25 N39 127.83(15) . . . . ?
N42 N36 C25 C24 -113.35(15) . . . . ?
N43 N37 C20 N35 -106.38(16) . . . . ?
N43 N37 C20 C21 138.69(15) . . . . ?
N43 N37 C23 N39 -122.23(15) . . . . ?
N43 N37 C23 C22 118.93(15) . . . . ?
N44 N38 C22 N35 -87.28(17) . . . . ?
N44 N38 C22 C23 159.17(14) . . . . ?
N44 N38 C24 N34 87.08(18) . . . . ?
N44 N38 C24 C25 -158.66(14) . . . . ?
C14 N23 N29 O21 -18.0(2) . . . . ?
C14 N23 N29 O22 165.26(14) . . . . ?
C14 N23 C16 N27 96.12(15) . . . . ?
C14 N23 C16 C17 -19.31(16) . . . . ?
C14 N25 N31 O25 15.5(2) . . . . ?
C14 N25 N31 O26 -167.79(14) . . . . ?
C14 N25 C17 N28 -97.72(15) . . . . ?
C14 N25 C17 C16 22.21(16) . . . . ?
C15 N24 N30 O23 15.3(2) . . . . ?
C15 N24 N30 O24 -168.60(16) . . . . ?
C15 N24 C18 N27 -95.81(16) . . . . ?
C15 N24 C18 C19 19.91(16) . . . . ?
C15 N26 N32 O39 167.65(14) . . . . ?
C15 N26 N32 O40 -17.1(2) . . . . ?
C15 N26 C19 N28 96.87(15) . . . . ?
C15 N26 C19 C18 -22.41(15) . . . . ?
C16 N23 N29 O21 -150.18(15) . . . . ?
C16 N23 N29 O22 33.1(2) . . . . ?
C16 N23 C14 N25 33.38(16) . . . . ?
C16 N23 C14 C15 -82.54(15) . . . . ?
C16 N27 N33 O27 -179.7(2) . . . . ?
C16 N27 N33 O27A -141.5(7) . . . . ?
C16 N27 N33 O28 5.8(3) . . . . ?
C16 N27 N33 O28A 16.8(13) . . . . ?
C16 N27 C18 N24 56.03(19) . . . . ?
C16 N27 C18 C19 -57.04(18) . . . . ?
C17 N25 N31 O25 146.79(15) . . . . ?
C17 N25 N31 O26 -36.5(2) . . . . ?
C17 N25 C14 N23 -34.46(15) . . . . ?
C17 N25 C14 C15 80.66(15) . . . . ?
C17 N28 C19 N26 -58.91(18) . . . . ?
C17 N28 C19 C18 56.37(17) . . . . ?
C17 N28 C26 N39 -64.26(16) . . . . ?
C18 N24 N30 O23 157.18(16) . . . . ?
C18 N24 N30 O24 -26.7(2) . . . . ?
C18 N24 C15 N26 -34.13(16) . . . . ?
C18 N24 C15 C14 81.52(15) . . . . ?
C18 N27 N33 O27 -27.1(3) . . . . ?
C18 N27 N33 O27A 11.2(7) . . . . ?
C18 N27 N33 O28 158.4(2) . . . . ?
C18 N27 N33 O28A 169.4(13) . . . . ?
C18 N27 C16 N23 -56.30(19) . . . . ?
C18 N27 C16 C17 57.25(18) . . . . ?
C19 N26 N32 O39 37.6(2) . . . . ?
C19 N26 N32 O40 -147.08(14) . . . . ?
C19 N26 C15 N24 34.65(16) . . . . ?
C19 N26 C15 C14 -81.08(15) . . . . ?
C19 N28 C17 N25 59.22(17) . . . . ?
C19 N28 C17 C16 -56.24(17) . . . . ?
C19 N28 C26 N39 165.32(13) . . . . ?
C20 N35 N41 O31 -162.86(17) . . . . ?
C20 N35 N41 O32 20.9(2) . . . . ?
C20 N35 C22 N38 -95.81(16) . . . . ?
C20 N35 C22 C23 19.99(18) . . . . ?
C20 N37 N43 O35 168.06(14) . . . . ?
C20 N37 N43 O36 -16.6(2) . . . . ?
C20 N37 C23 N39 96.89(16) . . . . ?
C20 N37 C23 C22 -21.95(16) . . . . ?
C21 N34 N40 O29 155.77(16) . . . . ?
C21 N34 N40 O30 -28.6(2) . . . . ?
C21 N34 C24 N38 95.40(16) . . . . ?
C21 N34 C24 C25 -20.81(17) . . . . ?
C21 N36 N42 O33 -162.57(15) . . . . ?
C21 N36 N42 O34 20.6(2) . . . . ?
C21 N36 C25 N39 -96.75(16) . . . . ?
C21 N36 C25 C24 22.07(16) . . . . ?
C22 N35 N41 O31 -23.5(3) . . . . ?
C22 N35 N41 O32 160.31(18) . . . . ?
C22 N35 C20 N37 -33.72(18) . . . . ?
C22 N35 C20 C21 81.21(16) . . . . ?
C22 N38 N44 O37 -20.7(2) . . . . ?
C22 N38 N44 O38 162.66(16) . . . . ?
C22 N38 C24 N34 -56.94(19) . . . . ?
C22 N38 C24 C25 57.31(18) . . . . ?
C23 N37 N43 O35 31.5(2) . . . . ?
C23 N37 N43 O36 -153.15(15) . . . . ?
C23 N37 C20 N35 34.37(17) . . . . ?
C23 N37 C20 C21 -80.56(16) . . . . ?
C23 N39 C25 N36 57.30(18) . . . . ?
C23 N39 C25 C24 -57.03(18) . . . . ?
C23 N39 C26 N28 147.29(13) . . . . ?
C24 N34 N40 O29 23.8(2) . . . . ?
C24 N34 N40 O30 -160.58(15) . . . . ?
C24 N34 C21 N36 34.53(16) . . . . ?
C24 N34 C21 C20 -81.26(16) . . . . ?
C24 N38 N44 O37 -164.21(16) . . . . ?
C24 N38 N44 O38 19.2(2) . . . . ?
C24 N38 C22 N35 56.51(19) . . . . ?
C24 N38 C22 C23 -57.04(18) . . . . ?
C25 N36 N42 O33 -31.0(2) . . . . ?
C25 N36 N42 O34 152.17(15) . . . . ?
C25 N36 C21 N34 -34.93(16) . . . . ?
C25 N36 C21 C20 81.36(16) . . . . ?
C25 N39 C23 N37 -57.55(18) . . . . ?
C25 N39 C23 C22 57.03(17) . . . . ?
C25 N39 C26 N28 -76.24(16) . . . . ?
C26 N28 C17 N25 -71.48(16) . . . . ?
C26 N28 C17 C16 173.06(13) . . . . ?
C26 N28 C19 N26 71.04(17) . . . . ?
C26 N28 C19 C18 -173.67(13) . . . . ?
C26 N39 C23 N37 79.21(17) . . . . ?
C26 N39 C23 C22 -166.21(13) . . . . ?
C26 N39 C25 N36 -80.31(17) . . . . ?
C26 N39 C25 C24 165.37(13) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.349
_oxdiff_exptl_absorpt_empirical_full_min 0.845
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_11
_database_code_depnum_ccdc_archive 'CCDC 2208930'
loop_
_audit_author_name
_audit_author_address
'Aida I Samigullina'
;N D Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences 
Russia
;
_audit_update_record             
;
2022-09-22 deposited with the CCDC.	2022-12-09 downloaded from the CCDC.
;
_audit_creation_date             2022-09-22
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
# start Validation Reply Form
_vrf_PLAT430_11                  
;
PROBLEM: Short Inter D...A Contact  O15      ..O42      .       2.71 Ang.  
RESPONSE: These intermolecular interactions are expected for this structure.
;
# end Validation Reply Form

_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H18 N26 O28, 5(C2 H3 N)'
_chemical_formula_sum            'C27 H33 N31 O28'
_chemical_formula_weight         1239.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         C12H12N12O12
_chemical_oxdiff_usercomment     NSV2022
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/c 1'
_space_group_name_Hall           '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   26.0971(2)
_cell_length_b                   11.66535(8)
_cell_length_c                   36.7954(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.7058(8)
_cell_angle_gamma                90
_cell_volume                     10882.72(14)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    72632
_cell_measurement_temperature    100.1(1)
_cell_measurement_theta_max      77.8210
_cell_measurement_theta_min      2.4130
_shelx_estimated_absorpt_T_max   0.921
_shelx_estimated_absorpt_T_min   0.770
_exptl_absorpt_coefficient_mu    1.200
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5088
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            150991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.807
_diffrn_reflns_theta_min         2.472
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.1(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -63.00  23.00   0.50    0.30    --  -48.70  63.00 -22.00  172
  2  ω   -114.00 -33.00   0.50    0.30    --  -48.70 -63.00-159.00  162
  3  ω     41.00  68.00   0.50    0.30    --   48.70  63.00 -22.00   54
  4  ω      7.00  38.00   0.50    0.30    --   48.70 -63.00-159.00   62
  5  ω   -138.00-113.00   0.50    1.00    --  -86.25 -63.00-159.00   50
  6  ω    -68.00 -43.00   0.50    1.00    --  -86.25  63.00 -22.00   50
  7  ω     93.00 123.00   0.50    1.00    --  107.75  63.00 -22.00   60
  8  ω     37.00  62.00   0.50    1.00    --  107.75 -63.00-159.00   50
  9  ω   -107.00 -77.00   0.50    0.30    --  -48.70-125.00 -90.00   60
 10  ω    -25.00  22.00   0.50    0.30    --  -48.70  19.00 120.00   94
 11  ω    -46.00 -20.00   0.50    1.00    --  -86.25  45.00-180.00   52
 12  ω    -51.00 -26.00   0.50    1.00    --  -86.25  45.00 120.00   50
 13  ω     36.00  61.00   0.50    1.00    --  107.75 -61.00-120.00   50
 14  ω     97.00 133.00   0.50    1.00    --  107.75  44.00  88.45   72
 15  ω    146.00 178.00   0.50    1.00    --  107.75  15.00 -90.00   64
 16  ω     47.00 107.00   0.50    1.00    --  107.75-105.00  67.39  120
 17  ω     42.00 102.00   0.50    1.00    --  107.75 -95.00  30.00  120
 18  ω     47.00  90.00   0.50    1.00    --  107.75 -77.00-120.00   86
 19  ω    104.00 150.00   0.50    1.00    --  107.75  45.00 -30.00   92
 20  ω    121.00 168.00   0.50    1.00    --  107.75 125.00-150.00   94
 21  ω     40.00  71.00   0.50    1.00    --  107.75-108.00 106.23   62
 22  ω    119.00 178.00   0.50    1.00    --  107.75  15.00  60.00  118
 23  ω    126.00 178.00   0.50    1.00    --  107.75  61.00 -90.00  104
 24  ω     44.00  70.00   0.50    1.00    --  107.75 -61.00 -90.00   52
 25  ω     97.00 123.00   0.50    1.00    --  107.75  61.00 -90.00   52
 26  ω     40.00 109.00   0.50    1.00    --  107.75-114.00 -45.37  138
 27  ω     36.00  96.00   0.50    1.00    --  107.75 -93.00-116.93  120
 28  ω     36.00  69.00   0.50    1.00    --  107.75 -77.00 -60.00   66
 29  ω     72.00  98.00   0.50    1.00    --  107.75 -77.00 -60.00   52
 30  ω     99.00 124.00   0.50    1.00    --  107.75  15.00-120.00   50
 31  ω    120.00 157.00   0.50    1.00    --  107.75 101.00 128.85   74
 32  ω     51.00  93.00   0.50    1.00    --  107.75-127.00 -12.71   84
 33  ω     86.00 124.00   0.50    1.00    --  107.75  77.00 150.00   76
 34  ω    136.00 162.00   0.50    1.00    --  107.75  77.00 150.00   52
 35  ω     40.00  92.00   0.50    1.00    --  107.75 -95.00   0.00  104
 36  ω     77.00 104.00   0.50    1.00    --  107.75-108.00 106.23   54
 37  ω     88.00 121.00   0.50    1.00    --  107.75  77.00-180.00   66
 38  ω     41.00  80.00   0.50    1.00    --  107.75 -77.00  30.00   78
 39  ω     38.00  63.00   0.50    1.00    --  107.75 -61.00-180.00   50
 40  ω    134.00 160.00   0.50    1.00    --  107.75  44.00  88.45   52
 41  ω     98.00 175.00   0.50    1.00    --  107.75  30.00-180.00  154
 42  ω    134.00 161.00   0.50    1.00    --  107.75 125.00  30.00   54
 43  ω     51.00  77.00   0.50    1.00    --  107.75 -77.00  60.00   52
 44  ω     39.00  89.00   0.50    1.00    --  107.75 -77.00 150.00  100
 45  ω     45.00  71.00   0.50    1.00    --  107.75 -95.00  90.00   52
 46  ω     41.00  67.00   0.50    1.00    --  107.75-112.00   4.33   52
 47  ω     36.00  66.00   0.50    1.00    --  107.75 -61.00  30.00   60
 48  ω     40.00  66.00   0.50    1.00    --  107.75-125.00 -60.00   52
 49  ω    135.00 175.00   0.50    1.00    --  107.75  45.00-150.00   80
 50  ω    139.00 175.00   0.50    1.00    --  107.75  45.00 120.00   72
 51  ω    149.00 176.00   0.50    1.00    --  107.75 125.00 -30.00   54
 52  ω     95.00 121.00   0.50    1.00    --  107.75  77.00-150.00   52
 53  ω     43.00  69.00   0.50    1.00    --  107.75 -87.00 146.33   52
 54  ω    112.00 138.00   0.50    1.00    --  107.75  15.00 -90.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0423772000
_diffrn_orient_matrix_UB_12      0.0010744000
_diffrn_orient_matrix_UB_13      -0.0371250000
_diffrn_orient_matrix_UB_21      -0.0292022000
_diffrn_orient_matrix_UB_22      0.0972989000
_diffrn_orient_matrix_UB_23      0.0150090000
_diffrn_orient_matrix_UB_31      0.0323047000
_diffrn_orient_matrix_UB_32      0.0892670000
_diffrn_orient_matrix_UB_33      -0.0159339000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                20188
_reflns_number_total             23017
_reflns_odcompleteness_completeness 93.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     86.18
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1559
_refine_ls_number_reflns         23017
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0519
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0700P)²+9.4340P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1456
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10),
 C11(H11), C12(H12), C13(H13), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C16(H16A,H16B), C24(H24A,H24B), C31(H31A,H31B),
 C33(H33A,H33B)
2.c Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C67(H67A,H67B,
 H67C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C73(H73A,H73B,H73C), C74(H74A,
 H74B,H74C), C79(H79A,H79B,H79C), C81(H81A,H81B,H81C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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_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 0.80560(5) 0.60646(13) 0.36414(4) 0.0290(3) Uani 1 1 d . . . . .
O2 O 0.78536(5) 0.52330(12) 0.30948(4) 0.0277(3) Uani 1 1 d . . . . .
O3 O 0.79026(6) 0.91653(14) 0.31660(4) 0.0338(3) Uani 1 1 d . . . . .
O4 O 0.78008(5) 0.79429(13) 0.27029(4) 0.0305(3) Uani 1 1 d . . . . .
O5 O 0.59780(5) 0.45897(12) 0.31807(4) 0.0292(3) Uani 1 1 d . . . . .
O6 O 0.65190(6) 0.42279(12) 0.28251(4) 0.0311(3) Uani 1 1 d . . . . .
O7 O 0.56307(6) 0.91531(14) 0.24287(4) 0.0357(3) Uani 1 1 d . . . . .
O8 O 0.62009(6) 0.86156(13) 0.21172(4) 0.0318(3) Uani 1 1 d . . . . .
O9 O 0.47258(6) 0.82541(14) 0.46842(4) 0.0344(3) Uani 1 1 d . . . . .
O10 O 0.40655(6) 0.89919(14) 0.42731(5) 0.0377(4) Uani 1 1 d . . . . .
O11 O 0.42120(6) 0.47657(13) 0.42301(4) 0.0323(3) Uani 1 1 d . . . . .
O12 O 0.36268(6) 0.60415(14) 0.39667(5) 0.0344(3) Uani 1 1 d . . . . .
O13 O 0.43928(6) 1.01319(12) 0.35149(5) 0.0349(3) Uani 1 1 d . . . . .
O14 O 0.51976(6) 0.99646(13) 0.34492(5) 0.0356(3) Uani 1 1 d . . . . .
O15 O 0.38114(5) 0.58489(14) 0.28188(4) 0.0307(3) Uani 1 1 d . . . . .
O16 O 0.45920(6) 0.55526(15) 0.27261(4) 0.0340(3) Uani 1 1 d . . . . .
O17 O 0.74215(9) 1.06941(16) 0.45523(5) 0.0532(5) Uani 1 1 d . . . . .
O18 O 0.81404(7) 0.98856(18) 0.44756(5) 0.0478(4) Uani 1 1 d . . . . .
O19 O 0.74727(8) 0.82146(17) 0.48270(5) 0.0470(4) Uani 1 1 d . . . . .
O20 O 0.75209(6) 0.70148(14) 0.43861(4) 0.0357(3) Uani 1 1 d . . . . .
O21 O 0.65041(6) 0.85718(15) 0.42705(5) 0.0412(4) Uani 1 1 d . . . . .
O22 O 0.66436(7) 1.00094(15) 0.39326(5) 0.0405(4) Uani 1 1 d . . . . .
O23 O 0.65295(7) 0.60648(16) 0.43444(5) 0.0474(4) Uani 1 1 d . . . . .
O24 O 0.60502(6) 0.46001(14) 0.41132(4) 0.0355(3) Uani 1 1 d . . . . .
O25 O 0.65578(7) 0.60036(17) 0.51818(5) 0.0524(5) Uani 1 1 d . . . . .
O26 O 0.59998(7) 0.72395(15) 0.48823(5) 0.0494(5) Uani 1 1 d . . . . .
O27 O 0.64046(7) 0.36774(16) 0.48321(6) 0.0484(4) Uani 1 1 d . . . . .
O28 O 0.57393(7) 0.40415(16) 0.50791(5) 0.0433(4) Uani 1 1 d . . . . .
N1 N 0.73191(6) 0.65491(14) 0.32410(4) 0.0223(3) Uani 1 1 d . . . . .
N2 N 0.71070(6) 0.84849(14) 0.29087(4) 0.0228(3) Uani 1 1 d . . . . .
N3 N 0.64555(6) 0.60144(13) 0.30372(4) 0.0211(3) Uani 1 1 d . . . . .
N4 N 0.62710(6) 0.79478(13) 0.27032(4) 0.0223(3) Uani 1 1 d . . . . .
N5 N 0.71171(6) 0.81894(13) 0.35784(4) 0.0225(3) Uani 1 1 d . . . . .
N6 N 0.61471(6) 0.76457(13) 0.33332(4) 0.0212(3) Uani 1 1 d . . . . .
N7 N 0.77660(6) 0.58907(14) 0.33326(5) 0.0234(3) Uani 1 1 d . . . . .
N8 N 0.76384(6) 0.85241(14) 0.29302(5) 0.0258(3) Uani 1 1 d . . . . .
N9 N 0.63179(6) 0.48531(14) 0.30166(5) 0.0245(3) Uani 1 1 d . . . . .
N10 N 0.60245(6) 0.86417(14) 0.23967(5) 0.0259(3) Uani 1 1 d . . . . .
N11 N 0.45713(6) 0.76518(14) 0.40935(5) 0.0242(3) Uani 1 1 d . . . . .
N12 N 0.43257(6) 0.57444(14) 0.37403(4) 0.0232(3) Uani 1 1 d . . . . .
N13 N 0.47786(6) 0.84037(13) 0.35666(5) 0.0234(3) Uani 1 1 d . . . . .
N14 N 0.45210(6) 0.65083(14) 0.32363(4) 0.0224(3) Uani 1 1 d . . . . .
N15 N 0.52083(6) 0.61275(13) 0.41480(4) 0.0228(3) Uani 1 1 d . . . . .
N16 N 0.54246(6) 0.69204(13) 0.35502(4) 0.0218(3) Uani 1 1 d . . . . .
N17 N 0.44518(7) 0.83722(15) 0.43683(5) 0.0292(4) Uani 1 1 d . . . . .
N18 N 0.40405(6) 0.55049(15) 0.39990(5) 0.0270(3) Uani 1 1 d . . . . .
N19 N 0.47915(7) 0.95905(14) 0.35154(5) 0.0288(3) Uani 1 1 d . . . . .
N20 N 0.42900(6) 0.59015(14) 0.29079(4) 0.0251(3) Uani 1 1 d . . . . .
N21 N 0.76675(8) 0.99511(17) 0.44360(5) 0.0372(4) Uani 1 1 d . . . . .
N22 N 0.74657(7) 0.79587(17) 0.45071(5) 0.0313(4) Uani 1 1 d . . . . .
N23 N 0.67823(7) 0.92018(15) 0.41392(5) 0.0304(4) Uani 1 1 d . . . . .
N24 N 0.61984(7) 0.53376(15) 0.43464(5) 0.0298(4) Uani 1 1 d . . . . .
N25 N 0.61841(7) 0.62889(17) 0.49363(5) 0.0353(4) Uani 1 1 d . . . . .
N26 N 0.60349(7) 0.42423(17) 0.48761(5) 0.0350(4) Uani 1 1 d . . . . .
C1 C 0.69136(7) 0.63511(16) 0.29015(5) 0.0213(3) Uani 1 1 d . . . . .
H1 H 0.701810 0.575328 0.273809 0.026 Uiso 1 1 calc R U . . .
C2 C 0.67976(7) 0.75562(16) 0.26975(5) 0.0219(3) Uani 1 1 d . . . . .
H2 H 0.684621 0.751971 0.243618 0.026 Uiso 1 1 calc R U . . .
C3 C 0.68948(7) 0.88070(16) 0.32390(5) 0.0226(4) Uani 1 1 d . . . . .
H3 H 0.692562 0.965247 0.328375 0.027 Uiso 1 1 calc R U . . .
C4 C 0.63019(7) 0.84555(16) 0.30864(5) 0.0219(3) Uani 1 1 d . . . . .
H4 H 0.607261 0.915147 0.306267 0.026 Uiso 1 1 calc R U . . .
C5 C 0.70729(7) 0.69762(16) 0.35393(5) 0.0218(3) Uani 1 1 d . . . . .
H5 H 0.722970 0.658805 0.378259 0.026 Uiso 1 1 calc R U . . .
C6 C 0.64773(7) 0.66311(15) 0.33925(5) 0.0210(3) Uani 1 1 d . . . . .
H6 H 0.636721 0.610941 0.357589 0.025 Uiso 1 1 calc R U . . .
C7 C 0.55872(7) 0.73467(16) 0.32213(5) 0.0225(4) Uani 1 1 d . . . . .
H7A H 0.537652 0.803002 0.311973 0.027 Uiso 1 1 calc R U . . .
H7B H 0.552936 0.674977 0.302453 0.027 Uiso 1 1 calc R U . . .
C8 C 0.43446(7) 0.79140(16) 0.37004(5) 0.0246(4) Uani 1 1 d . . . . .
H8 H 0.403830 0.845092 0.366727 0.029 Uiso 1 1 calc R U . . .
C9 C 0.41849(7) 0.67238(16) 0.34930(5) 0.0232(4) Uani 1 1 d . . . . .
H9 H 0.380306 0.670891 0.336085 0.028 Uiso 1 1 calc R U . . .
C10 C 0.52737(7) 0.78350(16) 0.37698(5) 0.0225(3) Uani 1 1 d . . . . .
H10 H 0.556456 0.841075 0.383780 0.027 Uiso 1 1 calc R U . . .
C11 C 0.51357(7) 0.73461(16) 0.41333(5) 0.0233(4) Uani 1 1 d . . . . .
H11 H 0.536055 0.771557 0.436121 0.028 Uiso 1 1 calc R U . . .
C12 C 0.50327(7) 0.60346(16) 0.34602(5) 0.0212(3) Uani 1 1 d . . . . .
H12 H 0.515871 0.540820 0.331746 0.025 Uiso 1 1 calc R U . . .
C13 C 0.49061(7) 0.55365(16) 0.38259(5) 0.0221(3) Uani 1 1 d . . . . .
H13 H 0.498218 0.469574 0.384634 0.026 Uiso 1 1 calc R U . . .
C14 C 0.75426(7) 0.86974(17) 0.38590(5) 0.0253(4) Uani 1 1 d . . . . .
H14A H 0.765533 0.942134 0.376102 0.030 Uiso 1 1 calc R U . . .
H14B H 0.784813 0.816898 0.391294 0.030 Uiso 1 1 calc R U . . .
C15 C 0.73678(8) 0.89435(17) 0.42227(6) 0.0273(4) Uani 1 1 d . . . . .
C16 C 0.53194(7) 0.55477(17) 0.45062(5) 0.0247(4) Uani 1 1 d . . . . .
H16A H 0.513777 0.479650 0.447780 0.030 Uiso 1 1 calc R U . . .
H16B H 0.517891 0.600929 0.468652 0.030 Uiso 1 1 calc R U . . .
C17 C 0.59167(8) 0.53603(17) 0.46619(5) 0.0264(4) Uani 1 1 d . . . . .
O31 O 1.08845(5) 0.73918(12) 0.57423(4) 0.0277(3) Uani 1 1 d . . . . .
O32 O 1.14719(5) 0.61630(13) 0.60364(4) 0.0300(3) Uani 1 1 d . . . . .
O33 O 1.09726(6) 0.32739(13) 0.57559(4) 0.0303(3) Uani 1 1 d . . . . .
O34 O 1.03446(6) 0.41085(13) 0.53428(4) 0.0293(3) Uani 1 1 d . . . . .
O35 O 1.13180(5) 0.65450(12) 0.71789(4) 0.0253(3) Uani 1 1 d . . . . .
O36 O 1.05500(5) 0.69369(12) 0.72833(4) 0.0252(3) Uani 1 1 d . . . . .
O37 O 1.06069(6) 0.22287(11) 0.65238(4) 0.0285(3) Uani 1 1 d . . . . .
O38 O 0.98088(6) 0.25198(12) 0.65901(4) 0.0279(3) Uani 1 1 d . . . . .
O39 O 0.70094(6) 0.63196(14) 0.62747(4) 0.0350(3) Uani 1 1 d . . . . .
O40 O 0.71446(6) 0.70611(14) 0.68335(4) 0.0375(4) Uani 1 1 d . . . . .
O41 O 0.72015(6) 0.29665(14) 0.67861(4) 0.0325(3) Uani 1 1 d . . . . .
O42 O 0.72290(5) 0.43416(14) 0.71936(4) 0.0315(3) Uani 1 1 d . . . . .
O43 O 0.90127(6) 0.78951(12) 0.68457(4) 0.0309(3) Uani 1 1 d . . . . .
O44 O 0.84144(6) 0.81591(12) 0.71633(4) 0.0331(3) Uani 1 1 d . . . . .
O45 O 0.94192(5) 0.33158(12) 0.75768(4) 0.0286(3) Uani 1 1 d . . . . .
O46 O 0.88069(5) 0.37708(12) 0.78618(4) 0.0256(3) Uani 1 1 d . . . . .
O47 O 0.93074(6) 0.83682(13) 0.49463(4) 0.0350(3) Uani 1 1 d . . . . .
O48 O 0.86714(7) 0.87468(16) 0.52233(5) 0.0463(4) Uani 1 1 d . . . . .
O49 O 0.90212(6) 0.51519(13) 0.51765(4) 0.0310(3) Uani 1 1 d . . . . .
O50 O 0.84757(6) 0.64265(16) 0.48762(4) 0.0405(4) Uani 1 1 d . . . . .
O51 O 0.90892(6) 0.78232(13) 0.59410(4) 0.0321(3) Uani 1 1 d . . . . .
O52 O 0.85612(6) 0.64091(15) 0.57203(4) 0.0381(4) Uani 1 1 d . . . . .
O53 O 0.86031(7) 0.38444(16) 0.57008(5) 0.0439(4) Uani 1 1 d . . . . .
O54 O 0.84960(7) 0.23794(15) 0.60397(5) 0.0409(4) Uani 1 1 d . . . . .
O55 O 0.75770(6) 0.52918(15) 0.55756(4) 0.0375(3) Uani 1 1 d . . . . .
O56 O 0.76097(9) 0.40787(19) 0.51361(5) 0.0567(5) Uani 1 1 d . . . . .
O57 O 0.77216(10) 0.16258(18) 0.54256(6) 0.0628(6) Uani 1 1 d . . . . .
O58 O 0.69911(8) 0.23581(18) 0.55121(5) 0.0515(5) Uani 1 1 d . . . . .
N31 N 1.07819(6) 0.65759(12) 0.62634(4) 0.0182(3) Uani 1 1 d . . . . .
N32 N 1.04885(6) 0.46564(13) 0.59329(4) 0.0190(3) Uani 1 1 d . . . . .
N33 N 1.05818(6) 0.59135(12) 0.67786(4) 0.0176(3) Uani 1 1 d . . . . .
N34 N 1.02678(6) 0.40088(12) 0.64657(4) 0.0178(3) Uani 1 1 d . . . . .
N35 N 0.98898(6) 0.62621(12) 0.58653(4) 0.0182(3) Uani 1 1 d . . . . .
N36 N 0.96622(6) 0.55832(12) 0.64692(4) 0.0170(3) Uani 1 1 d . . . . .
N37 N 1.10621(6) 0.67105(13) 0.59951(4) 0.0221(3) Uani 1 1 d . . . . .
N38 N 1.06057(6) 0.39425(14) 0.56616(4) 0.0234(3) Uani 1 1 d . . . . .
N39 N 1.08350(6) 0.65311(13) 0.70980(4) 0.0198(3) Uani 1 1 d . . . . .
N40 N 1.02243(6) 0.28309(13) 0.65222(4) 0.0221(3) Uani 1 1 d . . . . .
N41 N 0.77050(6) 0.57523(14) 0.67095(4) 0.0228(3) Uani 1 1 d . . . . .
N42 N 0.79604(6) 0.38153(14) 0.70420(4) 0.0213(3) Uani 1 1 d . . . . .
N43 N 0.85458(6) 0.63988(13) 0.69543(4) 0.0205(3) Uani 1 1 d . . . . .
N44 N 0.87676(6) 0.44742(13) 0.72842(4) 0.0190(3) Uani 1 1 d . . . . .
N45 N 0.79943(6) 0.41647(14) 0.63863(4) 0.0212(3) Uani 1 1 d . . . . .
N46 N 0.89364(6) 0.48489(13) 0.66732(4) 0.0185(3) Uani 1 1 d . . . . .
N47 N 0.72610(6) 0.64462(15) 0.65968(5) 0.0281(3) Uani 1 1 d . . . . .
N48 N 0.74323(6) 0.37083(15) 0.70020(4) 0.0259(3) Uani 1 1 d . . . . .
N49 N 0.86565(7) 0.75770(14) 0.69844(5) 0.0257(3) Uani 1 1 d . . . . .
N50 N 0.90071(6) 0.37800(13) 0.75949(4) 0.0210(3) Uani 1 1 d . . . . .
N51 N 0.90332(7) 0.81658(16) 0.51627(5) 0.0316(4) Uani 1 1 d . . . . .
N52 N 0.88555(6) 0.61230(16) 0.51161(4) 0.0276(3) Uani 1 1 d . . . . .
N53 N 0.89058(6) 0.71013(15) 0.57083(5) 0.0267(3) Uani 1 1 d . . . . .
N54 N 0.83388(7) 0.31749(16) 0.58302(5) 0.0327(4) Uani 1 1 d . . . . .
N55 N 0.76305(7) 0.43555(17) 0.54589(5) 0.0328(4) Uani 1 1 d . . . . .
N56 N 0.74617(9) 0.23414(18) 0.55411(5) 0.0413(5) Uani 1 1 d . . . . .
C18 C 1.07124(7) 0.44162(15) 0.63267(5) 0.0182(3) Uani 1 1 d . . . . .
H18 H 1.100429 0.384097 0.636383 0.022 Uiso 1 1 calc R U . . .
C19 C 1.09036(7) 0.56095(14) 0.65207(5) 0.0178(3) Uani 1 1 d . . . . .
H19 H 1.128677 0.558972 0.664924 0.021 Uiso 1 1 calc R U . . .
C20 C 0.99335(7) 0.50444(15) 0.58897(5) 0.0184(3) Uani 1 1 d . . . . .
H20 H 0.969781 0.467721 0.566593 0.022 Uiso 1 1 calc R U . . .
C21 C 0.97894(7) 0.46235(15) 0.62575(5) 0.0182(3) Uani 1 1 d . . . . .
H21 H 0.948406 0.408214 0.619503 0.022 Uiso 1 1 calc R U . . .
C22 C 1.02090(7) 0.68522(14) 0.61812(5) 0.0175(3) Uani 1 1 d . . . . .
H22 H 1.015376 0.769888 0.615307 0.021 Uiso 1 1 calc R U . . .
C23 C 1.00755(6) 0.64239(14) 0.65523(5) 0.0169(3) Uani 1 1 d . . . . .
H23 H 0.996581 0.708460 0.668971 0.020 Uiso 1 1 calc R U . . .
C24 C 0.94859(7) 0.52138(15) 0.67991(5) 0.0187(3) Uani 1 1 d . . . . .
H24A H 0.951484 0.585387 0.697946 0.022 Uiso 1 1 calc R U . . .
H24B H 0.970655 0.457054 0.692379 0.022 Uiso 1 1 calc R U . . .
C25 C 0.80800(7) 0.59750(16) 0.70618(5) 0.0215(3) Uani 1 1 d . . . . .
H25 H 0.794137 0.653688 0.722018 0.026 Uiso 1 1 calc R U . . .
C26 C 0.82229(7) 0.47775(16) 0.72661(5) 0.0205(3) Uani 1 1 d . . . . .
H26 H 0.814876 0.478185 0.752056 0.025 Uiso 1 1 calc R U . . .
C27 C 0.85769(7) 0.58109(15) 0.66020(5) 0.0191(3) Uani 1 1 d . . . . .
H27 H 0.868907 0.636578 0.642864 0.023 Uiso 1 1 calc R U . . .
C28 C 0.79994(7) 0.53880(16) 0.64289(5) 0.0212(3) Uani 1 1 d . . . . .
H28 H 0.785285 0.576944 0.618279 0.025 Uiso 1 1 calc R U . . .
C29 C 0.87877(7) 0.39907(15) 0.69061(5) 0.0187(3) Uani 1 1 d . . . . .
H29 H 0.904047 0.333343 0.693817 0.022 Uiso 1 1 calc R U . . .
C30 C 0.82131(7) 0.35613(16) 0.67270(5) 0.0204(3) Uani 1 1 d . . . . .
H30 H 0.821291 0.271710 0.667983 0.024 Uiso 1 1 calc R U . . .
C31 C 0.97554(7) 0.68274(16) 0.55052(5) 0.0205(3) Uani 1 1 d . . . . .
H31A H 0.986873 0.634304 0.531758 0.025 Uiso 1 1 calc R U . . .
H31B H 0.994701 0.756509 0.552161 0.025 Uiso 1 1 calc R U . . .
C32 C 0.91575(7) 0.70520(16) 0.53766(5) 0.0234(4) Uani 1 1 d . . . . .
C33 C 0.75765(7) 0.36232(18) 0.61090(5) 0.0245(4) Uani 1 1 d . . . . .
H33A H 0.726393 0.413167 0.605289 0.029 Uiso 1 1 calc R U . . .
H33B H 0.747395 0.289680 0.621158 0.029 Uiso 1 1 calc R U . . .
C34 C 0.77504(8) 0.33724(18) 0.57455(5) 0.0284(4) Uani 1 1 d . . . . .
N60 N -0.00407(10) -0.04447(17) 0.56783(7) 0.0489(5) Uani 1 1 d . . . . .
C60 C 0.03755(10) -0.00908(18) 0.57990(7) 0.0360(5) Uani 1 1 d . . . . .
C61 C 0.08994(10) 0.03525(19) 0.59488(7) 0.0388(5) Uani 1 1 d . . . . .
H61A H 0.096753 0.098665 0.579196 0.058 Uiso 1 1 calc R U . . .
H61B H 0.115867 -0.025720 0.595179 0.058 Uiso 1 1 calc R U . . .
H61C H 0.092762 0.062919 0.620425 0.058 Uiso 1 1 calc R U . . .
N61 N 0.93895(11) -0.10914(18) 0.82928(6) 0.0525(6) Uani 1 1 d . . . . .
C62 C 0.92547(11) -0.04251(19) 0.80653(7) 0.0408(5) Uani 1 1 d . . . . .
C63 C 0.90808(14) 0.0415(2) 0.77727(7) 0.0558(7) Uani 1 1 d . . . . .
H63A H 0.880870 0.090268 0.783606 0.084 Uiso 1 1 calc R U . . .
H63B H 0.893513 0.002237 0.753530 0.084 Uiso 1 1 calc R U . . .
H63C H 0.938094 0.088975 0.774871 0.084 Uiso 1 1 calc R U . . .
N62 N 0.22486(14) 0.8601(2) 0.62671(8) 0.0683(8) Uani 1 1 d . . . . .
C64 C 0.23079(12) 0.8173(2) 0.65545(9) 0.0481(6) Uani 1 1 d . . . . .
C65 C 0.23882(15) 0.7631(3) 0.69179(10) 0.0647(8) Uani 1 1 d . . . . .
H65A H 0.235390 0.679799 0.688615 0.097 Uiso 1 1 calc R U . . .
H65B H 0.212344 0.791131 0.704583 0.097 Uiso 1 1 calc R U . . .
H65C H 0.274172 0.781640 0.706754 0.097 Uiso 1 1 calc R U . . .
N63 N 0.97207(8) 0.24803(15) 0.57227(5) 0.0341(4) Uani 1 1 d . . . . .
C66 C 0.94697(9) 0.20620(17) 0.54621(6) 0.0302(4) Uani 1 1 d . . . . .
C67 C 0.91499(15) 0.1524(3) 0.51274(8) 0.0626(9) Uani 1 1 d . . . . .
H67A H 0.902263 0.211044 0.493673 0.094 Uiso 1 1 calc R U . . .
H67B H 0.884821 0.113650 0.518916 0.094 Uiso 1 1 calc R U . . .
H67C H 0.936364 0.096188 0.503090 0.094 Uiso 1 1 calc R U . . .
N64 N 0.87965(9) 0.11696(17) 0.68985(6) 0.0412(5) Uani 1 1 d . . . . .
C68 C 0.89637(9) 0.07169(18) 0.66779(6) 0.0343(5) Uani 1 1 d . . . . .
C69 C 0.91730(11) 0.0152(2) 0.63909(7) 0.0426(5) Uani 1 1 d . . . . .
H69A H 0.924366 0.072637 0.621444 0.064 Uiso 1 1 calc R U . . .
H69B H 0.891494 -0.040362 0.625677 0.064 Uiso 1 1 calc R U . . .
H69C H 0.950131 -0.024524 0.650826 0.064 Uiso 1 1 calc R U . . .
N65 N 0.74070(17) 0.0874(2) 0.62380(9) 0.0864(11) Uani 1 1 d . . . . .
C70 C 0.74277(14) 0.0528(2) 0.65319(9) 0.0589(8) Uani 1 1 d . . . . .
C71 C 0.74619(15) 0.0096(3) 0.69047(10) 0.0629(8) Uani 1 1 d . . . . .
H71A H 0.750448 -0.073841 0.690629 0.094 Uiso 1 1 calc R U . . .
H71B H 0.713859 0.029139 0.698267 0.094 Uiso 1 1 calc R U . . .
H71C H 0.776575 0.044328 0.707826 0.094 Uiso 1 1 calc R U . . .
N66 N 0.71271(7) 0.43837(16) 0.36775(6) 0.0357(4) Uani 1 1 d . . . . .
C72 C 0.73154(9) 0.40054(19) 0.39629(6) 0.0326(4) Uani 1 1 d . . . . .
C73 C 0.75548(12) 0.3555(3) 0.43308(7) 0.0526(7) Uani 1 1 d . . . . .
H73A H 0.779990 0.293721 0.430832 0.079 Uiso 1 1 calc R U . . .
H73B H 0.727932 0.325459 0.444527 0.079 Uiso 1 1 calc R U . . .
H73C H 0.774718 0.416841 0.448784 0.079 Uiso 1 1 calc R U . . .
N67 N 0.53441(8) -0.01159(17) 0.43162(6) 0.0395(4) Uani 1 1 d . . . . .
C74 C 0.61138(10) 0.0810(3) 0.48050(8) 0.0480(6) Uani 1 1 d . . . . .
H74A H 0.643312 0.080388 0.470862 0.072 Uiso 1 1 calc R U . . .
H74B H 0.617756 0.037677 0.503960 0.072 Uiso 1 1 calc R U . . .
H74C H 0.602161 0.160296 0.485062 0.072 Uiso 1 1 calc R U . . .
C75 C 0.56836(9) 0.02882(18) 0.45332(6) 0.0324(4) Uani 1 1 d . . . . .
N69 N 0.79226(9) 0.80038(18) 0.62664(6) 0.0444(5) Uani 1 1 d . . . . .
C78 C 0.76754(11) 0.8332(2) 0.59918(7) 0.0398(5) Uani 1 1 d . . . . .
C79 C 0.7345(2) 0.8749(3) 0.56428(8) 0.0849(13) Uani 1 1 d . . . . .
H79A H 0.715507 0.810495 0.550107 0.127 Uiso 1 1 calc R U . . .
H79B H 0.756574 0.911985 0.549552 0.127 Uiso 1 1 calc R U . . .
H79C H 0.709085 0.930538 0.569611 0.127 Uiso 1 1 calc R U . . .
N70 N 0.48250(11) 0.71897(19) 0.56571(8) 0.0599(7) Uani 1 1 d . . . . .
C80 C 0.52397(12) 0.7569(2) 0.57331(8) 0.0480(6) Uani 1 1 d . . . . .
C81 C 0.57690(14) 0.8040(3) 0.58391(12) 0.0707(10) Uani 1 1 d . . . . .
H81A H 0.595160 0.789290 0.563971 0.106 Uiso 1 1 calc R U . . .
H81B H 0.596328 0.767577 0.607104 0.106 Uiso 1 1 calc R U . . .
H81C H 0.574954 0.886791 0.587820 0.106 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 N7 1.224(2) . ?
O2 N7 1.225(2) . ?
O3 N8 1.227(2) . ?
O4 N8 1.227(2) . ?
O5 N9 1.225(2) . ?
O6 N9 1.216(2) . ?
O7 N10 1.218(2) . ?
O8 N10 1.223(2) . ?
O9 N17 1.220(2) . ?
O10 N17 1.223(2) . ?
O11 N18 1.219(2) . ?
O12 N18 1.229(2) . ?
O13 N19 1.217(2) . ?
O14 N19 1.223(2) . ?
O15 N20 1.215(2) . ?
O16 N20 1.218(2) . ?
O17 N21 1.215(3) . ?
O18 N21 1.210(3) . ?
O19 N22 1.210(2) . ?
O20 N22 1.209(2) . ?
O21 N23 1.211(2) . ?
O22 N23 1.211(2) . ?
O23 N24 1.212(2) . ?
O24 N24 1.212(2) . ?
O25 N25 1.208(3) . ?
O26 N25 1.206(3) . ?
O27 N26 1.210(3) . ?
O28 N26 1.217(3) . ?
N1 N7 1.370(2) . ?
N1 C1 1.451(2) . ?
N1 C5 1.483(2) . ?
N2 N8 1.371(2) . ?
N2 C2 1.460(2) . ?
N2 C3 1.498(2) . ?
N3 N9 1.399(2) . ?
N3 C1 1.454(2) . ?
N3 C6 1.482(2) . ?
N4 N10 1.413(2) . ?
N4 C2 1.453(2) . ?
N4 C4 1.514(2) . ?
N5 C3 1.440(2) . ?
N5 C5 1.425(2) . ?
N5 C14 1.451(2) . ?
N6 C4 1.433(2) . ?
N6 C6 1.450(2) . ?
N6 C7 1.463(2) . ?
N11 N17 1.405(2) . ?
N11 C8 1.459(3) . ?
N11 C11 1.488(2) . ?
N12 N18 1.369(2) . ?
N12 C9 1.453(2) . ?
N12 C13 1.492(2) . ?
N13 N19 1.399(2) . ?
N13 C8 1.454(2) . ?
N13 C10 1.487(2) . ?
N14 N20 1.407(2) . ?
N14 C9 1.455(2) . ?
N14 C12 1.499(2) . ?
N15 C11 1.433(2) . ?
N15 C13 1.435(2) . ?
N15 C16 1.448(2) . ?
N16 C7 1.461(2) . ?
N16 C10 1.448(2) . ?
N16 C12 1.436(2) . ?
N21 C15 1.523(3) . ?
N22 C15 1.534(3) . ?
N23 C15 1.516(3) . ?
N24 C17 1.514(3) . ?
N25 C17 1.532(3) . ?
N26 C17 1.517(3) . ?
C1 H1 1.0000 . ?
C1 C2 1.589(3) . ?
C2 H2 1.0000 . ?
C3 H3 1.0000 . ?
C3 C4 1.570(2) . ?
C4 H4 1.0000 . ?
C5 H5 1.0000 . ?
C5 C6 1.572(2) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8 1.0000 . ?
C8 C9 1.592(3) . ?
C9 H9 1.0000 . ?
C10 H10 1.0000 . ?
C10 C11 1.573(3) . ?
C11 H11 1.0000 . ?
C12 H12 1.0000 . ?
C12 C13 1.571(3) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.540(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.544(3) . ?
O31 N37 1.228(2) . ?
O32 N37 1.224(2) . ?
O33 N38 1.220(2) . ?
O34 N38 1.224(2) . ?
O35 N39 1.225(2) . ?
O36 N39 1.217(2) . ?
O37 N40 1.220(2) . ?
O38 N40 1.224(2) . ?
O39 N47 1.220(2) . ?
O40 N47 1.221(2) . ?
O41 N48 1.231(2) . ?
O42 N48 1.225(2) . ?
O43 N49 1.219(2) . ?
O44 N49 1.221(2) . ?
O45 N50 1.220(2) . ?
O46 N50 1.217(2) . ?
O47 N51 1.213(2) . ?
O48 N51 1.225(3) . ?
O49 N52 1.214(2) . ?
O50 N52 1.213(2) . ?
O51 N53 1.215(2) . ?
O52 N53 1.217(2) . ?
O53 N54 1.212(3) . ?
O54 N54 1.214(2) . ?
O55 N55 1.194(3) . ?
O56 N55 1.219(2) . ?
O57 N56 1.214(3) . ?
O58 N56 1.208(3) . ?
N31 N37 1.369(2) . ?
N31 C19 1.458(2) . ?
N31 C22 1.489(2) . ?
N32 N38 1.389(2) . ?
N32 C18 1.456(2) . ?
N32 C20 1.490(2) . ?
N33 N39 1.403(2) . ?
N33 C19 1.452(2) . ?
N33 C23 1.507(2) . ?
N34 N40 1.398(2) . ?
N34 C18 1.454(2) . ?
N34 C21 1.485(2) . ?
N35 C20 1.426(2) . ?
N35 C22 1.435(2) . ?
N35 C31 1.447(2) . ?
N36 C21 1.447(2) . ?
N36 C23 1.436(2) . ?
N36 C24 1.461(2) . ?
N41 N47 1.394(2) . ?
N41 C25 1.451(2) . ?
N41 C28 1.487(2) . ?
N42 N48 1.356(2) . ?
N42 C26 1.463(2) . ?
N42 C30 1.493(2) . ?
N43 N49 1.403(2) . ?
N43 C25 1.451(2) . ?
N43 C27 1.486(2) . ?
N44 N50 1.419(2) . ?
N44 C26 1.451(2) . ?
N44 C29 1.514(2) . ?
N45 C28 1.435(2) . ?
N45 C30 1.433(2) . ?
N45 C33 1.450(2) . ?
N46 C24 1.462(2) . ?
N46 C27 1.446(2) . ?
N46 C29 1.430(2) . ?
N51 C32 1.514(2) . ?
N52 C32 1.535(3) . ?
N53 C32 1.518(2) . ?
N54 C34 1.511(3) . ?
N55 C34 1.539(3) . ?
N56 C34 1.520(3) . ?
C18 H18 1.0000 . ?
C18 C19 1.590(2) . ?
C19 H19 1.0000 . ?
C20 H20 1.0000 . ?
C20 C21 1.567(2) . ?
C21 H21 1.0000 . ?
C22 H22 1.0000 . ?
C22 C23 1.569(2) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25 1.0000 . ?
C25 C26 1.588(3) . ?
C26 H26 1.0000 . ?
C27 H27 1.0000 . ?
C27 C28 1.570(2) . ?
C28 H28 1.0000 . ?
C29 H29 1.0000 . ?
C29 C30 1.570(2) . ?
C30 H30 1.0000 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.542(2) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.539(3) . ?
N60 C60 1.148(3) . ?
C60 C61 1.443(4) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
N61 C62 1.136(3) . ?
C62 C63 1.447(3) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
N62 C64 1.146(4) . ?
C64 C65 1.449(4) . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
N63 C66 1.135(3) . ?
C66 C67 1.456(3) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
N64 C68 1.138(3) . ?
C68 C69 1.456(3) . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
N65 C70 1.144(4) . ?
C70 C71 1.444(5) . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
N66 C72 1.138(3) . ?
C72 C73 1.449(4) . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
N67 C75 1.144(3) . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C74 C75 1.449(3) . ?
N69 C78 1.129(3) . ?
C78 C79 1.451(4) . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
N70 C80 1.141(4) . ?
C80 C81 1.451(4) . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 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
N7 N1 C1 121.80(15) . . ?
N7 N1 C5 119.92(15) . . ?
C1 N1 C5 109.58(14) . . ?
N8 N2 C2 118.66(15) . . ?
N8 N2 C3 120.55(15) . . ?
C2 N2 C3 110.73(14) . . ?
N9 N3 C1 117.66(14) . . ?
N9 N3 C6 118.27(14) . . ?
C1 N3 C6 107.99(14) . . ?
N10 N4 C2 114.95(14) . . ?
N10 N4 C4 115.65(14) . . ?
C2 N4 C4 107.14(14) . . ?
C3 N5 C14 119.74(15) . . ?
C5 N5 C3 113.78(15) . . ?
C5 N5 C14 120.50(15) . . ?
C4 N6 C6 112.75(14) . . ?
C4 N6 C7 113.05(14) . . ?
C6 N6 C7 111.48(15) . . ?
O1 N7 O2 126.01(16) . . ?
O1 N7 N1 116.02(15) . . ?
O2 N7 N1 117.85(15) . . ?
O3 N8 O4 126.29(16) . . ?
O3 N8 N2 116.90(16) . . ?
O4 N8 N2 116.76(16) . . ?
O5 N9 N3 115.02(15) . . ?
O6 N9 O5 126.70(16) . . ?
O6 N9 N3 118.14(15) . . ?
O7 N10 O8 126.02(17) . . ?
O7 N10 N4 116.00(16) . . ?
O8 N10 N4 117.78(15) . . ?
N17 N11 C8 118.73(15) . . ?
N17 N11 C11 117.09(15) . . ?
C8 N11 C11 107.89(14) . . ?
N18 N12 C9 119.84(15) . . ?
N18 N12 C13 120.80(15) . . ?
C9 N12 C13 110.71(14) . . ?
N19 N13 C8 118.67(15) . . ?
N19 N13 C10 117.62(15) . . ?
C8 N13 C10 107.95(14) . . ?
N20 N14 C9 116.28(14) . . ?
N20 N14 C12 115.55(14) . . ?
C9 N14 C12 107.61(14) . . ?
C11 N15 C13 113.79(15) . . ?
C11 N15 C16 119.58(15) . . ?
C13 N15 C16 118.65(15) . . ?
C10 N16 C7 112.46(15) . . ?
C12 N16 C7 112.63(14) . . ?
C12 N16 C10 112.67(14) . . ?
O9 N17 O10 126.68(17) . . ?
O9 N17 N11 115.99(16) . . ?
O10 N17 N11 117.13(17) . . ?
O11 N18 O12 126.61(17) . . ?
O11 N18 N12 117.33(16) . . ?
O12 N18 N12 116.02(17) . . ?
O13 N19 O14 126.55(17) . . ?
O13 N19 N13 117.78(16) . . ?
O14 N19 N13 115.45(16) . . ?
O15 N20 O16 126.32(17) . . ?
O15 N20 N14 117.45(15) . . ?
O16 N20 N14 115.99(15) . . ?
O17 N21 C15 118.84(19) . . ?
O18 N21 O17 127.7(2) . . ?
O18 N21 C15 113.45(19) . . ?
O19 N22 C15 116.12(18) . . ?
O20 N22 O19 127.39(19) . . ?
O20 N22 C15 116.49(16) . . ?
O21 N23 C15 117.98(17) . . ?
O22 N23 O21 127.18(19) . . ?
O22 N23 C15 114.78(17) . . ?
O23 N24 C17 117.95(18) . . ?
O24 N24 O23 126.92(19) . . ?
O24 N24 C17 115.08(17) . . ?
O25 N25 C17 117.32(19) . . ?
O26 N25 O25 126.6(2) . . ?
O26 N25 C17 116.10(17) . . ?
O27 N26 O28 128.2(2) . . ?
O27 N26 C17 117.97(18) . . ?
O28 N26 C17 113.82(18) . . ?
N1 C1 N3 103.80(14) . . ?
N1 C1 H1 112.4 . . ?
N1 C1 C2 106.52(14) . . ?
N3 C1 H1 112.4 . . ?
N3 C1 C2 108.72(14) . . ?
C2 C1 H1 112.4 . . ?
N2 C2 C1 112.67(15) . . ?
N2 C2 H2 111.3 . . ?
N4 C2 N2 99.47(14) . . ?
N4 C2 C1 110.27(14) . . ?
N4 C2 H2 111.3 . . ?
C1 C2 H2 111.3 . . ?
N2 C3 H3 110.5 . . ?
N2 C3 C4 99.60(14) . . ?
N5 C3 N2 115.34(15) . . ?
N5 C3 H3 110.5 . . ?
N5 C3 C4 109.87(15) . . ?
C4 C3 H3 110.5 . . ?
N4 C4 C3 105.41(14) . . ?
N4 C4 H4 109.7 . . ?
N6 C4 N4 111.81(15) . . ?
N6 C4 C3 110.33(15) . . ?
N6 C4 H4 109.7 . . ?
C3 C4 H4 109.7 . . ?
N1 C5 H5 110.7 . . ?
N1 C5 C6 103.06(14) . . ?
N5 C5 N1 111.68(15) . . ?
N5 C5 H5 110.7 . . ?
N5 C5 C6 109.81(14) . . ?
C6 C5 H5 110.7 . . ?
N3 C6 C5 104.81(13) . . ?
N3 C6 H6 110.0 . . ?
N6 C6 N3 111.49(15) . . ?
N6 C6 C5 110.29(14) . . ?
N6 C6 H6 110.0 . . ?
C5 C6 H6 110.0 . . ?
N6 C7 H7A 110.0 . . ?
N6 C7 H7B 110.0 . . ?
N16 C7 N6 108.34(14) . . ?
N16 C7 H7A 110.0 . . ?
N16 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
N11 C8 H8 112.1 . . ?
N11 C8 C9 106.92(15) . . ?
N13 C8 N11 104.62(15) . . ?
N13 C8 H8 112.1 . . ?
N13 C8 C9 108.46(15) . . ?
C9 C8 H8 112.1 . . ?
N12 C9 N14 99.71(14) . . ?
N12 C9 C8 112.77(15) . . ?
N12 C9 H9 111.5 . . ?
N14 C9 C8 109.41(14) . . ?
N14 C9 H9 111.5 . . ?
C8 C9 H9 111.5 . . ?
N13 C10 H10 110.1 . . ?
N13 C10 C11 104.04(14) . . ?
N16 C10 N13 111.54(15) . . ?
N16 C10 H10 110.1 . . ?
N16 C10 C11 110.79(15) . . ?
C11 C10 H10 110.1 . . ?
N11 C11 C10 104.48(15) . . ?
N11 C11 H11 110.5 . . ?
N15 C11 N11 111.12(15) . . ?
N15 C11 C10 109.68(15) . . ?
N15 C11 H11 110.5 . . ?
C10 C11 H11 110.5 . . ?
N14 C12 H12 110.0 . . ?
N14 C12 C13 105.46(13) . . ?
N16 C12 N14 110.76(15) . . ?
N16 C12 H12 110.0 . . ?
N16 C12 C13 110.58(15) . . ?
C13 C12 H12 110.0 . . ?
N12 C13 C12 99.66(14) . . ?
N12 C13 H13 110.4 . . ?
N15 C13 N12 115.36(15) . . ?
N15 C13 C12 110.11(15) . . ?
N15 C13 H13 110.4 . . ?
C12 C13 H13 110.4 . . ?
N5 C14 H14A 109.4 . . ?
N5 C14 H14B 109.4 . . ?
N5 C14 C15 111.10(15) . . ?
H14A C14 H14B 108.0 . . ?
C15 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
N21 C15 N22 104.15(16) . . ?
N21 C15 C14 111.71(16) . . ?
N22 C15 C14 114.67(17) . . ?
N23 C15 N21 108.73(17) . . ?
N23 C15 N22 106.53(15) . . ?
N23 C15 C14 110.66(16) . . ?
N15 C16 H16A 109.3 . . ?
N15 C16 H16B 109.3 . . ?
N15 C16 C17 111.77(15) . . ?
H16A C16 H16B 107.9 . . ?
C17 C16 H16A 109.3 . . ?
C17 C16 H16B 109.3 . . ?
N24 C17 N25 106.83(16) . . ?
N24 C17 N26 107.89(16) . . ?
N24 C17 C16 110.41(15) . . ?
N25 C17 C16 114.01(16) . . ?
N26 C17 N25 105.11(16) . . ?
N26 C17 C16 112.19(16) . . ?
N37 N31 C19 119.03(14) . . ?
N37 N31 C22 120.71(14) . . ?
C19 N31 C22 110.68(13) . . ?
N38 N32 C18 119.70(14) . . ?
N38 N32 C20 118.68(14) . . ?
C18 N32 C20 108.39(13) . . ?
N39 N33 C19 116.25(13) . . ?
N39 N33 C23 115.91(13) . . ?
C19 N33 C23 107.61(13) . . ?
N40 N34 C18 118.23(14) . . ?
N40 N34 C21 117.59(14) . . ?
C18 N34 C21 107.70(13) . . ?
C20 N35 C22 113.85(14) . . ?
C20 N35 C31 120.66(14) . . ?
C22 N35 C31 119.43(14) . . ?
C21 N36 C24 112.12(13) . . ?
C23 N36 C21 112.75(13) . . ?
C23 N36 C24 113.13(13) . . ?
O31 N37 N31 116.76(15) . . ?
O32 N37 O31 126.41(15) . . ?
O32 N37 N31 116.80(15) . . ?
O33 N38 O34 126.50(16) . . ?
O33 N38 N32 118.08(15) . . ?
O34 N38 N32 115.25(15) . . ?
O35 N39 N33 117.61(14) . . ?
O36 N39 O35 126.08(15) . . ?
O36 N39 N33 116.09(14) . . ?
O37 N40 O38 126.30(16) . . ?
O37 N40 N34 118.13(15) . . ?
O38 N40 N34 115.39(15) . . ?
N47 N41 C25 119.95(15) . . ?
N47 N41 C28 119.28(14) . . ?
C25 N41 C28 108.76(14) . . ?
N48 N42 C26 117.37(15) . . ?
N48 N42 C30 121.45(14) . . ?
C26 N42 C30 110.84(13) . . ?
N49 N43 C25 118.83(14) . . ?
N49 N43 C27 117.90(14) . . ?
C25 N43 C27 107.64(14) . . ?
N50 N44 C26 114.57(13) . . ?
N50 N44 C29 115.03(13) . . ?
C26 N44 C29 107.19(13) . . ?
C28 N45 C33 119.74(15) . . ?
C30 N45 C28 113.66(14) . . ?
C30 N45 C33 118.62(15) . . ?
C27 N46 C24 112.14(14) . . ?
C29 N46 C24 113.52(14) . . ?
C29 N46 C27 113.29(14) . . ?
O39 N47 O40 126.62(17) . . ?
O39 N47 N41 115.91(16) . . ?
O40 N47 N41 117.30(16) . . ?
O41 N48 N42 117.63(16) . . ?
O42 N48 O41 125.63(16) . . ?
O42 N48 N42 116.70(16) . . ?
O43 N49 O44 126.84(17) . . ?
O43 N49 N43 115.35(15) . . ?
O44 N49 N43 117.64(16) . . ?
O45 N50 N44 115.78(14) . . ?
O46 N50 O45 126.36(16) . . ?
O46 N50 N44 117.63(14) . . ?
O47 N51 O48 127.72(18) . . ?
O47 N51 C32 114.92(17) . . ?
O48 N51 C32 117.36(17) . . ?
O49 N52 C32 115.89(15) . . ?
O50 N52 O49 126.84(18) . . ?
O50 N52 C32 117.27(17) . . ?
O51 N53 O52 127.24(17) . . ?
O51 N53 C32 114.80(16) . . ?
O52 N53 C32 117.91(16) . . ?
O53 N54 O54 127.2(2) . . ?
O53 N54 C34 117.79(18) . . ?
O54 N54 C34 114.94(18) . . ?
O55 N55 O56 127.6(2) . . ?
O55 N55 C34 117.21(16) . . ?
O56 N55 C34 115.15(19) . . ?
O57 N56 C34 117.7(2) . . ?
O58 N56 O57 128.4(2) . . ?
O58 N56 C34 113.9(2) . . ?
N32 C18 H18 112.2 . . ?
N32 C18 C19 106.71(13) . . ?
N34 C18 N32 104.33(14) . . ?
N34 C18 H18 112.2 . . ?
N34 C18 C19 108.67(13) . . ?
C19 C18 H18 112.2 . . ?
N31 C19 C18 112.87(13) . . ?
N31 C19 H19 111.4 . . ?
N33 C19 N31 99.48(13) . . ?
N33 C19 C18 109.78(13) . . ?
N33 C19 H19 111.4 . . ?
C18 C19 H19 111.4 . . ?
N32 C20 H20 110.5 . . ?
N32 C20 C21 103.82(13) . . ?
N35 C20 N32 111.75(14) . . ?
N35 C20 H20 110.5 . . ?
N35 C20 C21 109.55(14) . . ?
C21 C20 H20 110.5 . . ?
N34 C21 C20 104.62(13) . . ?
N34 C21 H21 109.9 . . ?
N36 C21 N34 111.59(14) . . ?
N36 C21 C20 110.80(14) . . ?
N36 C21 H21 109.9 . . ?
C20 C21 H21 109.9 . . ?
N31 C22 H22 110.4 . . ?
N31 C22 C23 100.01(13) . . ?
N35 C22 N31 115.02(14) . . ?
N35 C22 H22 110.4 . . ?
N35 C22 C23 110.25(13) . . ?
C23 C22 H22 110.4 . . ?
N33 C23 C22 105.07(13) . . ?
N33 C23 H23 110.1 . . ?
N36 C23 N33 111.33(13) . . ?
N36 C23 C22 110.03(13) . . ?
N36 C23 H23 110.1 . . ?
C22 C23 H23 110.1 . . ?
N36 C24 N46 107.52(13) . . ?
N36 C24 H24A 110.2 . . ?
N36 C24 H24B 110.2 . . ?
N46 C24 H24A 110.2 . . ?
N46 C24 H24B 110.2 . . ?
H24A C24 H24B 108.5 . . ?
N41 C25 N43 104.40(14) . . ?
N41 C25 H25 112.2 . . ?
N41 C25 C26 107.36(15) . . ?
N43 C25 H25 112.2 . . ?
N43 C25 C26 108.10(14) . . ?
C26 C25 H25 112.2 . . ?
N42 C26 C25 112.46(14) . . ?
N42 C26 H26 111.3 . . ?
N44 C26 N42 99.30(14) . . ?
N44 C26 C25 110.72(14) . . ?
N44 C26 H26 111.3 . . ?
C25 C26 H26 111.3 . . ?
N43 C27 H27 110.0 . . ?
N43 C27 C28 104.67(13) . . ?
N46 C27 N43 111.55(14) . . ?
N46 C27 H27 110.0 . . ?
N46 C27 C28 110.41(14) . . ?
C28 C27 H27 110.0 . . ?
N41 C28 C27 103.45(14) . . ?
N41 C28 H28 110.6 . . ?
N45 C28 N41 111.52(15) . . ?
N45 C28 C27 109.86(14) . . ?
N45 C28 H28 110.6 . . ?
C27 C28 H28 110.6 . . ?
N44 C29 H29 110.0 . . ?
N44 C29 C30 105.47(13) . . ?
N46 C29 N44 111.31(14) . . ?
N46 C29 H29 110.0 . . ?
N46 C29 C30 109.86(14) . . ?
C30 C29 H29 110.0 . . ?
N42 C30 C29 99.48(13) . . ?
N42 C30 H30 110.4 . . ?
N45 C30 N42 115.09(15) . . ?
N45 C30 C29 110.69(14) . . ?
N45 C30 H30 110.4 . . ?
C29 C30 H30 110.4 . . ?
N35 C31 H31A 109.3 . . ?
N35 C31 H31B 109.3 . . ?
N35 C31 C32 111.52(14) . . ?
H31A C31 H31B 108.0 . . ?
C32 C31 H31A 109.3 . . ?
C32 C31 H31B 109.3 . . ?
N51 C32 N52 105.45(14) . . ?
N51 C32 N53 107.78(15) . . ?
N51 C32 C31 112.45(15) . . ?
N52 C32 C31 113.84(15) . . ?
N53 C32 N52 105.83(14) . . ?
N53 C32 C31 111.02(14) . . ?
N45 C33 H33A 109.3 . . ?
N45 C33 H33B 109.3 . . ?
N45 C33 C34 111.54(15) . . ?
H33A C33 H33B 108.0 . . ?
C34 C33 H33A 109.3 . . ?
C34 C33 H33B 109.3 . . ?
N54 C34 N55 106.65(16) . . ?
N54 C34 N56 109.99(18) . . ?
N54 C34 C33 110.14(15) . . ?
N56 C34 N55 104.72(15) . . ?
N56 C34 C33 111.52(16) . . ?
C33 C34 N55 113.58(17) . . ?
N60 C60 C61 179.7(3) . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
N61 C62 C63 179.5(3) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
N62 C64 C65 179.4(4) . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
N63 C66 C67 179.7(3) . . ?
C66 C67 H67A 109.5 . . ?
C66 C67 H67B 109.5 . . ?
C66 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
N64 C68 C69 179.0(3) . . ?
C68 C69 H69A 109.5 . . ?
C68 C69 H69B 109.5 . . ?
C68 C69 H69C 109.5 . . ?
H69A C69 H69B 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
N65 C70 C71 179.1(4) . . ?
C70 C71 H71A 109.5 . . ?
C70 C71 H71B 109.5 . . ?
C70 C71 H71C 109.5 . . ?
H71A C71 H71B 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
N66 C72 C73 178.4(3) . . ?
C72 C73 H73A 109.5 . . ?
C72 C73 H73B 109.5 . . ?
C72 C73 H73C 109.5 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C75 C74 H74A 109.5 . . ?
C75 C74 H74B 109.5 . . ?
C75 C74 H74C 109.5 . . ?
N67 C75 C74 179.4(3) . . ?
N69 C78 C79 178.4(3) . . ?
C78 C79 H79A 109.5 . . ?
C78 C79 H79B 109.5 . . ?
C78 C79 H79C 109.5 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
N70 C80 C81 178.6(4) . . ?
C80 C81 H81A 109.5 . . ?
C80 C81 H81B 109.5 . . ?
C80 C81 H81C 109.5 . . ?
H81A C81 H81B 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 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
O17 N21 C15 N22 -103.1(2) . . . . ?
O17 N21 C15 N23 10.2(3) . . . . ?
O17 N21 C15 C14 132.6(2) . . . . ?
O18 N21 C15 N22 75.2(2) . . . . ?
O18 N21 C15 N23 -171.51(18) . . . . ?
O18 N21 C15 C14 -49.1(2) . . . . ?
O19 N22 C15 N21 37.9(2) . . . . ?
O19 N22 C15 N23 -76.9(2) . . . . ?
O19 N22 C15 C14 160.32(18) . . . . ?
O20 N22 C15 N21 -142.92(18) . . . . ?
O20 N22 C15 N23 102.23(19) . . . . ?
O20 N22 C15 C14 -20.5(2) . . . . ?
O21 N23 C15 N21 -118.2(2) . . . . ?
O21 N23 C15 N22 -6.5(2) . . . . ?
O21 N23 C15 C14 118.7(2) . . . . ?
O22 N23 C15 N21 64.4(2) . . . . ?
O22 N23 C15 N22 176.14(17) . . . . ?
O22 N23 C15 C14 -58.6(2) . . . . ?
O23 N24 C17 N25 -6.1(2) . . . . ?
O23 N24 C17 N26 -118.7(2) . . . . ?
O23 N24 C17 C16 118.4(2) . . . . ?
O24 N24 C17 N25 176.34(16) . . . . ?
O24 N24 C17 N26 63.8(2) . . . . ?
O24 N24 C17 C16 -59.2(2) . . . . ?
O25 N25 C17 N24 -88.8(2) . . . . ?
O25 N25 C17 N26 25.6(3) . . . . ?
O25 N25 C17 C16 148.9(2) . . . . ?
O26 N25 C17 N24 90.6(2) . . . . ?
O26 N25 C17 N26 -154.9(2) . . . . ?
O26 N25 C17 C16 -31.6(3) . . . . ?
O27 N26 C17 N24 17.1(3) . . . . ?
O27 N26 C17 N25 -96.6(2) . . . . ?
O27 N26 C17 C16 139.0(2) . . . . ?
O28 N26 C17 N24 -163.93(17) . . . . ?
O28 N26 C17 N25 82.3(2) . . . . ?
O28 N26 C17 C16 -42.1(2) . . . . ?
N1 C1 C2 N2 -1.94(19) . . . . ?
N1 C1 C2 N4 -112.08(16) . . . . ?
N1 C5 C6 N3 2.00(17) . . . . ?
N1 C5 C6 N6 -118.11(15) . . . . ?
N2 C3 C4 N4 2.21(17) . . . . ?
N2 C3 C4 N6 123.08(15) . . . . ?
N3 C1 C2 N2 109.36(16) . . . . ?
N3 C1 C2 N4 -0.8(2) . . . . ?
N5 C3 C4 N4 -119.30(15) . . . . ?
N5 C3 C4 N6 1.6(2) . . . . ?
N5 C5 C6 N3 121.12(15) . . . . ?
N5 C5 C6 N6 1.0(2) . . . . ?
N5 C14 C15 N21 -151.48(17) . . . . ?
N5 C14 C15 N22 90.33(19) . . . . ?
N5 C14 C15 N23 -30.2(2) . . . . ?
N7 N1 C1 N3 115.82(17) . . . . ?
N7 N1 C1 C2 -129.50(16) . . . . ?
N7 N1 C5 N5 112.16(18) . . . . ?
N7 N1 C5 C6 -130.02(16) . . . . ?
N8 N2 C2 N4 -171.93(15) . . . . ?
N8 N2 C2 C1 71.3(2) . . . . ?
N8 N2 C3 N5 -55.1(2) . . . . ?
N8 N2 C3 C4 -172.62(15) . . . . ?
N9 N3 C1 N1 -104.50(17) . . . . ?
N9 N3 C1 C2 142.39(15) . . . . ?
N9 N3 C6 N6 -125.25(16) . . . . ?
N9 N3 C6 C5 115.43(16) . . . . ?
N10 N4 C2 N2 91.29(17) . . . . ?
N10 N4 C2 C1 -150.14(15) . . . . ?
N10 N4 C4 N6 133.77(15) . . . . ?
N10 N4 C4 C3 -106.34(16) . . . . ?
N11 C8 C9 N12 -2.49(19) . . . . ?
N11 C8 C9 N14 -112.49(16) . . . . ?
N13 C8 C9 N12 109.82(17) . . . . ?
N13 C8 C9 N14 -0.2(2) . . . . ?
N13 C10 C11 N11 1.88(18) . . . . ?
N13 C10 C11 N15 121.05(15) . . . . ?
N14 C12 C13 N12 3.37(17) . . . . ?
N14 C12 C13 N15 -118.30(15) . . . . ?
N15 C16 C17 N24 -24.8(2) . . . . ?
N15 C16 C17 N25 95.44(19) . . . . ?
N15 C16 C17 N26 -145.23(16) . . . . ?
N16 C10 C11 N11 -118.10(15) . . . . ?
N16 C10 C11 N15 1.1(2) . . . . ?
N16 C12 C13 N12 123.15(15) . . . . ?
N16 C12 C13 N15 1.5(2) . . . . ?
N17 N11 C8 N13 104.37(17) . . . . ?
N17 N11 C8 C9 -140.70(16) . . . . ?
N17 N11 C11 N15 122.96(17) . . . . ?
N17 N11 C11 C10 -118.84(17) . . . . ?
N18 N12 C9 N14 -170.34(15) . . . . ?
N18 N12 C9 C8 73.7(2) . . . . ?
N18 N12 C13 N15 -57.9(2) . . . . ?
N18 N12 C13 C12 -175.72(15) . . . . ?
N19 N13 C8 N11 -103.82(18) . . . . ?
N19 N13 C8 C9 142.34(16) . . . . ?
N19 N13 C10 N16 -124.39(17) . . . . ?
N19 N13 C10 C11 116.14(17) . . . . ?
N20 N14 C9 N12 93.95(17) . . . . ?
N20 N14 C9 C8 -147.58(15) . . . . ?
N20 N14 C12 N16 130.14(16) . . . . ?
N20 N14 C12 C13 -110.20(16) . . . . ?
C1 N1 N7 O1 -173.36(16) . . . . ?
C1 N1 N7 O2 10.4(2) . . . . ?
C1 N1 C5 N5 -99.62(17) . . . . ?
C1 N1 C5 C6 18.19(18) . . . . ?
C1 N3 N9 O5 170.23(16) . . . . ?
C1 N3 N9 O6 -13.8(2) . . . . ?
C1 N3 C6 N6 97.95(16) . . . . ?
C1 N3 C6 C5 -21.37(18) . . . . ?
C2 N2 N8 O3 -165.99(16) . . . . ?
C2 N2 N8 O4 16.4(2) . . . . ?
C2 N2 C3 N5 89.83(18) . . . . ?
C2 N2 C3 C4 -27.66(18) . . . . ?
C2 N4 N10 O7 -166.71(16) . . . . ?
C2 N4 N10 O8 18.1(2) . . . . ?
C2 N4 C4 N6 -96.60(17) . . . . ?
C2 N4 C4 C3 23.29(18) . . . . ?
C3 N2 N8 O3 -23.7(2) . . . . ?
C3 N2 N8 O4 158.65(16) . . . . ?
C3 N2 C2 N4 42.37(17) . . . . ?
C3 N2 C2 C1 -74.39(18) . . . . ?
C3 N5 C5 N1 56.70(19) . . . . ?
C3 N5 C5 C6 -56.99(19) . . . . ?
C3 N5 C14 C15 114.87(18) . . . . ?
C4 N4 N10 O7 -41.0(2) . . . . ?
C4 N4 N10 O8 143.83(16) . . . . ?
C4 N4 C2 N2 -38.73(17) . . . . ?
C4 N4 C2 C1 79.83(17) . . . . ?
C4 N6 C6 N3 -60.46(19) . . . . ?
C4 N6 C6 C5 55.55(19) . . . . ?
C4 N6 C7 N16 -157.45(15) . . . . ?
C5 N1 N7 O1 -29.1(2) . . . . ?
C5 N1 N7 O2 154.66(16) . . . . ?
C5 N1 C1 N3 -31.69(18) . . . . ?
C5 N1 C1 C2 83.00(16) . . . . ?
C5 N5 C3 N2 -55.6(2) . . . . ?
C5 N5 C3 C4 55.94(19) . . . . ?
C5 N5 C14 C15 -94.0(2) . . . . ?
C6 N3 N9 O5 37.5(2) . . . . ?
C6 N3 N9 O6 -146.48(17) . . . . ?
C6 N3 C1 N1 32.60(18) . . . . ?
C6 N3 C1 C2 -80.51(17) . . . . ?
C6 N6 C4 N4 60.30(19) . . . . ?
C6 N6 C4 C3 -56.66(19) . . . . ?
C6 N6 C7 N16 74.31(18) . . . . ?
C7 N6 C4 N4 -67.28(18) . . . . ?
C7 N6 C4 C3 175.76(14) . . . . ?
C7 N6 C6 N3 67.94(18) . . . . ?
C7 N6 C6 C5 -176.05(14) . . . . ?
C7 N16 C10 N13 68.13(18) . . . . ?
C7 N16 C10 C11 -176.48(14) . . . . ?
C7 N16 C12 N14 -68.13(18) . . . . ?
C7 N16 C12 C13 175.33(14) . . . . ?
C8 N11 N17 O9 -166.36(17) . . . . ?
C8 N11 N17 O10 18.5(2) . . . . ?
C8 N11 C11 N15 -99.96(17) . . . . ?
C8 N11 C11 C10 18.24(18) . . . . ?
C8 N13 N19 O13 -13.9(3) . . . . ?
C8 N13 N19 O14 171.03(17) . . . . ?
C8 N13 C10 N16 97.99(17) . . . . ?
C8 N13 C10 C11 -21.48(18) . . . . ?
C9 N12 N18 O11 -171.09(16) . . . . ?
C9 N12 N18 O12 10.9(2) . . . . ?
C9 N12 C13 N15 89.73(19) . . . . ?
C9 N12 C13 C12 -28.09(18) . . . . ?
C9 N14 N20 O15 17.4(2) . . . . ?
C9 N14 N20 O16 -167.90(17) . . . . ?
C9 N14 C12 N16 -98.06(17) . . . . ?
C9 N14 C12 C13 21.60(18) . . . . ?
C10 N13 N19 O13 -146.99(18) . . . . ?
C10 N13 N19 O14 38.0(2) . . . . ?
C10 N13 C8 N11 33.28(18) . . . . ?
C10 N13 C8 C9 -80.55(18) . . . . ?
C10 N16 C7 N6 85.60(17) . . . . ?
C10 N16 C12 N14 60.39(19) . . . . ?
C10 N16 C12 C13 -56.15(19) . . . . ?
C11 N11 N17 O9 -34.0(2) . . . . ?
C11 N11 N17 O10 150.84(17) . . . . ?
C11 N11 C8 N13 -31.90(18) . . . . ?
C11 N11 C8 C9 83.03(17) . . . . ?
C11 N15 C13 N12 -56.2(2) . . . . ?
C11 N15 C13 C12 55.64(19) . . . . ?
C11 N15 C16 C17 -95.99(19) . . . . ?
C12 N14 N20 O15 144.98(17) . . . . ?
C12 N14 N20 O16 -40.3(2) . . . . ?
C12 N14 C9 N12 -37.46(17) . . . . ?
C12 N14 C9 C8 81.01(17) . . . . ?
C12 N16 C7 N6 -145.77(15) . . . . ?
C12 N16 C10 N13 -60.5(2) . . . . ?
C12 N16 C10 C11 54.92(19) . . . . ?
C13 N12 N18 O11 -26.4(2) . . . . ?
C13 N12 N18 O12 155.61(17) . . . . ?
C13 N12 C9 N14 41.68(18) . . . . ?
C13 N12 C9 C8 -74.26(18) . . . . ?
C13 N15 C11 N11 58.3(2) . . . . ?
C13 N15 C11 C10 -56.75(19) . . . . ?
C13 N15 C16 C17 116.99(18) . . . . ?
C14 N5 C3 N2 97.30(19) . . . . ?
C14 N5 C3 C4 -151.15(15) . . . . ?
C14 N5 C5 N1 -95.99(19) . . . . ?
C14 N5 C5 C6 150.32(15) . . . . ?
C16 N15 C11 N11 -90.27(19) . . . . ?
C16 N15 C11 C10 154.73(15) . . . . ?
C16 N15 C13 N12 92.7(2) . . . . ?
C16 N15 C13 C12 -155.52(15) . . . . ?
O47 N51 C32 N52 -84.1(2) . . . . ?
O47 N51 C32 N53 163.15(16) . . . . ?
O47 N51 C32 C31 40.5(2) . . . . ?
O48 N51 C32 N52 95.2(2) . . . . ?
O48 N51 C32 N53 -17.5(2) . . . . ?
O48 N51 C32 C31 -140.16(19) . . . . ?
O49 N52 C32 N51 157.77(16) . . . . ?
O49 N52 C32 N53 -88.16(19) . . . . ?
O49 N52 C32 C31 34.0(2) . . . . ?
O50 N52 C32 N51 -23.1(2) . . . . ?
O50 N52 C32 N53 90.97(19) . . . . ?
O50 N52 C32 C31 -146.83(17) . . . . ?
O51 N53 C32 N51 -65.6(2) . . . . ?
O51 N53 C32 N52 -178.08(15) . . . . ?
O51 N53 C32 C31 57.9(2) . . . . ?
O52 N53 C32 N51 116.56(19) . . . . ?
O52 N53 C32 N52 4.1(2) . . . . ?
O52 N53 C32 C31 -119.87(19) . . . . ?
O53 N54 C34 N55 7.1(2) . . . . ?
O53 N54 C34 N56 120.2(2) . . . . ?
O53 N54 C34 C33 -116.5(2) . . . . ?
O54 N54 C34 N55 -176.43(17) . . . . ?
O54 N54 C34 N56 -63.4(2) . . . . ?
O54 N54 C34 C33 59.9(2) . . . . ?
O55 N55 C34 N54 -99.1(2) . . . . ?
O55 N55 C34 N56 144.36(19) . . . . ?
O55 N55 C34 C33 22.5(2) . . . . ?
O56 N55 C34 N54 79.9(2) . . . . ?
O56 N55 C34 N56 -36.7(2) . . . . ?
O56 N55 C34 C33 -158.62(19) . . . . ?
O57 N56 C34 N54 -11.1(3) . . . . ?
O57 N56 C34 N55 103.1(2) . . . . ?
O57 N56 C34 C33 -133.6(2) . . . . ?
O58 N56 C34 N54 169.67(18) . . . . ?
O58 N56 C34 N55 -76.1(2) . . . . ?
O58 N56 C34 C33 47.2(3) . . . . ?
N31 C22 C23 N33 -3.01(15) . . . . ?
N31 C22 C23 N36 -122.95(14) . . . . ?
N32 C18 C19 N31 2.75(18) . . . . ?
N32 C18 C19 N33 112.74(15) . . . . ?
N32 C20 C21 N34 -1.80(16) . . . . ?
N32 C20 C21 N36 118.59(14) . . . . ?
N34 C18 C19 N31 -109.23(15) . . . . ?
N34 C18 C19 N33 0.76(18) . . . . ?
N35 C20 C21 N34 -121.30(14) . . . . ?
N35 C20 C21 N36 -0.91(19) . . . . ?
N35 C22 C23 N33 118.52(14) . . . . ?
N35 C22 C23 N36 -1.43(19) . . . . ?
N35 C31 C32 N51 144.82(15) . . . . ?
N35 C31 C32 N52 -95.33(17) . . . . ?
N35 C31 C32 N53 24.0(2) . . . . ?
N37 N31 C19 N33 171.59(14) . . . . ?
N37 N31 C19 C18 -72.12(19) . . . . ?
N37 N31 C22 N35 55.8(2) . . . . ?
N37 N31 C22 C23 173.83(14) . . . . ?
N38 N32 C18 N34 -108.30(16) . . . . ?
N38 N32 C18 C19 136.76(15) . . . . ?
N38 N32 C20 N35 -119.57(16) . . . . ?
N38 N32 C20 C21 122.45(15) . . . . ?
N39 N33 C19 N31 -93.95(15) . . . . ?
N39 N33 C19 C18 147.44(14) . . . . ?
N39 N33 C23 N36 -131.11(14) . . . . ?
N39 N33 C23 C22 109.81(15) . . . . ?
N40 N34 C18 N32 103.04(16) . . . . ?
N40 N34 C18 C19 -143.41(14) . . . . ?
N40 N34 C21 N36 125.02(15) . . . . ?
N40 N34 C21 C20 -115.12(15) . . . . ?
N41 C25 C26 N42 2.16(19) . . . . ?
N41 C25 C26 N44 112.24(15) . . . . ?
N43 C25 C26 N42 -109.94(16) . . . . ?
N43 C25 C26 N44 0.14(19) . . . . ?
N43 C27 C28 N41 -1.71(17) . . . . ?
N43 C27 C28 N45 -120.89(15) . . . . ?
N44 C29 C30 N42 -2.77(16) . . . . ?
N44 C29 C30 N45 118.73(15) . . . . ?
N45 C33 C34 N54 29.0(2) . . . . ?
N45 C33 C34 N55 -90.50(19) . . . . ?
N45 C33 C34 N56 151.45(18) . . . . ?
N46 C27 C28 N41 118.45(15) . . . . ?
N46 C27 C28 N45 -0.72(19) . . . . ?
N46 C29 C30 N42 -122.83(14) . . . . ?
N46 C29 C30 N45 -1.33(19) . . . . ?
N47 N41 C25 N43 -110.07(17) . . . . ?
N47 N41 C25 C26 135.33(16) . . . . ?
N47 N41 C28 N45 -117.92(18) . . . . ?
N47 N41 C28 C27 124.05(17) . . . . ?
N48 N42 C26 N44 171.70(14) . . . . ?
N48 N42 C26 C25 -71.20(19) . . . . ?
N48 N42 C30 N45 53.9(2) . . . . ?
N48 N42 C30 C29 172.20(16) . . . . ?
N49 N43 C25 N41 104.22(17) . . . . ?
N49 N43 C25 C26 -141.69(15) . . . . ?
N49 N43 C27 N46 124.13(16) . . . . ?
N49 N43 C27 C28 -116.46(16) . . . . ?
N50 N44 C26 N42 -90.45(16) . . . . ?
N50 N44 C26 C25 151.14(14) . . . . ?
N50 N44 C29 N46 -135.11(15) . . . . ?
N50 N44 C29 C30 105.79(15) . . . . ?
C18 N32 N38 O33 -14.4(2) . . . . ?
C18 N32 N38 O34 170.10(15) . . . . ?
C18 N32 C20 N35 99.46(16) . . . . ?
C18 N32 C20 C21 -18.52(17) . . . . ?
C18 N34 N40 O37 14.1(2) . . . . ?
C18 N34 N40 O38 -170.50(15) . . . . ?
C18 N34 C21 N36 -98.35(15) . . . . ?
C18 N34 C21 C20 21.51(17) . . . . ?
C19 N31 N37 O31 166.48(15) . . . . ?
C19 N31 N37 O32 -15.4(2) . . . . ?
C19 N31 C22 N35 -90.07(17) . . . . ?
C19 N31 C22 C23 27.98(16) . . . . ?
C19 N33 N39 O35 -15.9(2) . . . . ?
C19 N33 N39 O36 169.07(14) . . . . ?
C19 N33 C23 N36 96.81(15) . . . . ?
C19 N33 C23 C22 -22.27(16) . . . . ?
C20 N32 N38 O33 -150.93(16) . . . . ?
C20 N32 N38 O34 33.6(2) . . . . ?
C20 N32 C18 N34 32.21(17) . . . . ?
C20 N32 C18 C19 -82.73(15) . . . . ?
C20 N35 C22 N31 56.22(19) . . . . ?
C20 N35 C22 C23 -55.91(18) . . . . ?
C20 N35 C31 C32 94.41(19) . . . . ?
C21 N34 N40 O37 146.15(16) . . . . ?
C21 N34 N40 O38 -38.4(2) . . . . ?
C21 N34 C18 N32 -33.28(17) . . . . ?
C21 N34 C18 C19 80.28(16) . . . . ?
C21 N36 C23 N33 -59.81(17) . . . . ?
C21 N36 C23 C22 56.26(18) . . . . ?
C21 N36 C24 N46 -78.49(17) . . . . ?
C22 N31 N37 O31 23.4(2) . . . . ?
C22 N31 N37 O32 -158.49(16) . . . . ?
C22 N31 C19 N33 -41.92(16) . . . . ?
C22 N31 C19 C18 74.37(17) . . . . ?
C22 N35 C20 N32 -57.73(18) . . . . ?
C22 N35 C20 C21 56.76(18) . . . . ?
C22 N35 C31 C32 -114.64(17) . . . . ?
C23 N33 N39 O35 -143.84(15) . . . . ?
C23 N33 N39 O36 41.1(2) . . . . ?
C23 N33 C19 N31 37.94(16) . . . . ?
C23 N33 C19 C18 -80.67(16) . . . . ?
C23 N36 C21 N34 60.71(18) . . . . ?
C23 N36 C21 C20 -55.44(18) . . . . ?
C23 N36 C24 N46 152.64(14) . . . . ?
C24 N36 C21 N34 -68.36(17) . . . . ?
C24 N36 C21 C20 175.49(13) . . . . ?
C24 N36 C23 N33 68.74(17) . . . . ?
C24 N36 C23 C22 -175.19(13) . . . . ?
C24 N46 C27 N43 -69.84(17) . . . . ?
C24 N46 C27 C28 174.22(13) . . . . ?
C24 N46 C29 N44 69.47(18) . . . . ?
C24 N46 C29 C30 -174.09(14) . . . . ?
C25 N41 N47 O39 169.11(17) . . . . ?
C25 N41 N47 O40 -15.3(3) . . . . ?
C25 N41 C28 N45 99.44(17) . . . . ?
C25 N41 C28 C27 -18.59(18) . . . . ?
C25 N43 N49 O43 -171.02(16) . . . . ?
C25 N43 N49 O44 13.4(2) . . . . ?
C25 N43 C27 N46 -98.06(16) . . . . ?
C25 N43 C27 C28 21.35(17) . . . . ?
C26 N42 N48 O41 173.39(16) . . . . ?
C26 N42 N48 O42 -8.6(2) . . . . ?
C26 N42 C30 N45 -90.11(18) . . . . ?
C26 N42 C30 C29 28.16(17) . . . . ?
C26 N44 N50 O45 165.15(15) . . . . ?
C26 N44 N50 O46 -20.1(2) . . . . ?
C26 N44 C29 N46 96.21(16) . . . . ?
C26 N44 C29 C30 -22.89(17) . . . . ?
C27 N43 N49 O43 -37.9(2) . . . . ?
C27 N43 N49 O44 146.43(16) . . . . ?
C27 N43 C25 N41 -33.13(18) . . . . ?
C27 N43 C25 C26 80.95(16) . . . . ?
C27 N46 C24 N36 -78.62(17) . . . . ?
C27 N46 C29 N44 -59.95(18) . . . . ?
C27 N46 C29 C30 56.50(18) . . . . ?
C28 N41 N47 O39 30.7(3) . . . . ?
C28 N41 N47 O40 -153.79(18) . . . . ?
C28 N41 C25 N43 32.28(18) . . . . ?
C28 N41 C25 C26 -82.33(17) . . . . ?
C28 N45 C30 N42 56.5(2) . . . . ?
C28 N45 C30 C29 -55.29(19) . . . . ?
C28 N45 C33 C34 97.45(19) . . . . ?
C29 N44 N50 O45 40.2(2) . . . . ?
C29 N44 N50 O46 -144.98(15) . . . . ?
C29 N44 C26 N42 38.50(16) . . . . ?
C29 N44 C26 C25 -79.91(16) . . . . ?
C29 N46 C24 N36 151.39(14) . . . . ?
C29 N46 C27 N43 60.27(19) . . . . ?
C29 N46 C27 C28 -55.67(18) . . . . ?
C30 N42 N48 O41 31.6(2) . . . . ?
C30 N42 N48 O42 -150.46(17) . . . . ?
C30 N42 C26 N44 -42.64(17) . . . . ?
C30 N42 C26 C25 74.46(17) . . . . ?
C30 N45 C28 N41 -58.13(19) . . . . ?
C30 N45 C28 C27 55.97(18) . . . . ?
C30 N45 C33 C34 -115.59(18) . . . . ?
C31 N35 C20 N32 94.73(18) . . . . ?
C31 N35 C20 C21 -150.78(15) . . . . ?
C31 N35 C22 N31 -96.61(18) . . . . ?
C31 N35 C22 C23 151.27(14) . . . . ?
C33 N45 C28 N41 90.36(18) . . . . ?
C33 N45 C28 C27 -155.54(15) . . . . ?
C33 N45 C30 N42 -92.37(19) . . . . ?
C33 N45 C30 C29 155.84(15) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.069 0.250 26.7 0.0 ?
2 0.000 -0.069 0.750 26.7 0.0 ?
3 0.500 0.219 0.250 406.9 102.3 '5 C2H3N'
4 0.500 0.781 0.750 406.9 102.2 '5 C2H3N'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.475
_oxdiff_exptl_absorpt_empirical_full_min 0.597
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
