# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_POK2008
_database_code_depnum_ccdc_archive 'CCDC 2078088'
loop_
_audit_author_name
_audit_author_address
'Darina Ildarovna Nasyrova'
;N D Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences
Russia
;
_audit_update_record             
;
2021-04-16 deposited with the CCDC.	2021-12-15 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT430_POK2008             
;
PROBLEM: Short Inter D...A Contact  O13      ..O25      .       2.78 Ang.  
RESPONSE: This is due to the unique structure of the molecule.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H16 N24 O22, 2(C2 H3 N)'
_chemical_formula_sum            'C18 H22 N26 O22'
_chemical_formula_weight         954.61

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

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

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

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

_cell_length_a                   11.7431(2)
_cell_length_b                   15.9679(3)
_cell_length_c                   19.3734(4)
_cell_angle_alpha                89.4340(10)
_cell_angle_beta                 82.7850(10)
_cell_angle_gamma                73.8080(10)
_cell_volume                     3459.83(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9789
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      33.71

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_F_000             1952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    0.167
_shelx_estimated_absorpt_T_min   0.966
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7058
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_process_details   
'SADABS 2016/2 (Krause et al., J. Appl. Cryst. 2015, 48, 3-10)'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-Ray tube'
_diffrn_source_power             50
_diffrn_source_current           30
_diffrn_source_size              '0.6 mm, fine-focus'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS D8 QUEST, Photon III detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_detector_area_resol_mean 7.31
_diffrn_reflns_number            172779
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.986
_diffrn_reflns_theta_max         34.349
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             28977
_reflns_number_gt                19693
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 (Bruker, 2019)'
_computing_cell_refinement       'SAINT (Bruker, 2019)'
_computing_data_reduction        'SAINT (Bruker, 2019)'
_computing_structure_solution    
'SHELXT, SHELXS-2013 (Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_computing_structure_refinement  
'SHELXL-2018 (Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_molecular_graphics    
'SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)'
_computing_publication_material  
'SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)'
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0419P)²+1.3086P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         28977
_refine_ls_number_parameters     1194
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1187
_refine_ls_wR_factor_gt          0.0992
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.12229(12) 0.61118(7) 0.71243(6) 0.0310(3) Uani 1 1 d . . . . .
O2 O 0.31412(12) 0.59185(8) 0.71264(6) 0.0328(3) Uani 1 1 d . . . . .
O3 O 0.09143(11) 0.60399(7) 0.94511(6) 0.0288(3) Uani 1 1 d . . . . .
O4 O 0.27506(11) 0.60231(7) 0.90540(6) 0.0293(3) Uani 1 1 d . . . . .
O5 O 0.39350(10) 0.26014(7) 0.67911(6) 0.0278(2) Uani 1 1 d . . . . .
O6 O 0.51226(9) 0.33647(8) 0.70345(7) 0.0332(3) Uani 1 1 d . . . . .
O7 O 0.38035(10) 0.23634(7) 0.95781(5) 0.0230(2) Uani 1 1 d . . . . .
O8 O 0.46892(9) 0.33917(8) 0.95900(5) 0.0231(2) Uani 1 1 d . . . . .
O9 O -0.08466(10) 0.42370(9) 0.90426(7) 0.0314(3) Uani 1 1 d . . . . .
O10 O -0.09426(10) 0.46233(9) 0.79668(7) 0.0337(3) Uani 1 1 d . . . . .
O11 O 0.00134(9) 0.21932(7) 0.81368(6) 0.0213(2) Uani 1 1 d . . . . .
O12 O 0.00956(9) 0.12315(6) 0.89504(6) 0.0189(2) Uani 1 1 d . . . . .
O13 O 0.56660(11) 0.02215(8) 0.88613(7) 0.0304(3) Uani 1 1 d . . . . .
O14 O 0.64032(10) -0.09695(8) 0.93980(7) 0.0274(2) Uani 1 1 d . . . . .
O15 O 0.10802(9) 0.01895(7) 1.06932(5) 0.0209(2) Uani 1 1 d . . . . .
O16 O 0.22904(9) -0.09674(7) 1.10752(5) 0.0189(2) Uani 1 1 d . . . . .
O17 O 0.43341(9) -0.28837(7) 0.79344(5) 0.0193(2) Uani 1 1 d . . . . .
O18 O 0.50911(10) -0.31873(7) 0.89117(6) 0.0222(2) Uani 1 1 d . . . . .
O19 O 0.07354(9) -0.21500(7) 0.97000(6) 0.0199(2) Uani 1 1 d . . . . .
O20 O 0.21911(10) -0.27272(7) 1.03016(5) 0.0214(2) Uani 1 1 d . . . . .
O21 O 0.14679(10) -0.20433(8) 0.79230(6) 0.0263(2) Uani 1 1 d . . . . .
O22 O 0.27321(10) -0.16322(8) 0.71646(5) 0.0249(2) Uani 1 1 d . . . . .
N1 N 0.22095(11) 0.50941(8) 0.77979(6) 0.0163(2) Uani 1 1 d . . . . .
N2 N 0.22371(10) 0.47944(7) 0.91047(6) 0.0133(2) Uani 1 1 d . . . . .
N3 N 0.32765(10) 0.37007(8) 0.75388(6) 0.0180(2) Uani 1 1 d . . . . .
N4 N 0.33586(10) 0.34410(7) 0.88338(6) 0.0139(2) Uani 1 1 d . . . . .
N5 N 0.06255(10) 0.47235(7) 0.84776(6) 0.0142(2) Uani 1 1 d . . . . .
N6 N 0.18166(10) 0.31094(7) 0.82327(5) 0.01132(19) Uani 1 1 d . . . . .
N7 N 0.21936(14) 0.57496(8) 0.72966(6) 0.0234(3) Uani 1 1 d . . . . .
N8 N 0.19387(12) 0.56856(8) 0.92045(7) 0.0202(2) Uani 1 1 d . . . . .
N9 N 0.41610(10) 0.31952(8) 0.70912(6) 0.0178(2) Uani 1 1 d . . . . .
N10 N 0.39816(10) 0.30517(8) 0.93850(6) 0.0170(2) Uani 1 1 d . . . . .
N11 N -0.04648(11) 0.44993(9) 0.84962(7) 0.0222(3) Uani 1 1 d . . . . .
N12 N 0.16794(10) 0.17072(7) 0.86222(6) 0.0132(2) Uani 1 1 d . . . . .
N13 N 0.05270(10) 0.17111(7) 0.85642(6) 0.0147(2) Uani 1 1 d . . . . .
N14 N 0.25254(10) 0.01801(7) 0.88952(6) 0.0126(2) Uani 1 1 d . . . . .
N15 N 0.44782(10) -0.06187(7) 0.91992(6) 0.0128(2) Uani 1 1 d . . . . .
N16 N 0.25677(10) -0.06465(7) 0.99540(5) 0.01216(19) Uani 1 1 d . . . . .
N17 N 0.45428(10) -0.18139(7) 0.85921(6) 0.0132(2) Uani 1 1 d . . . . .
N18 N 0.25539(10) -0.19120(7) 0.93839(6) 0.01211(19) Uani 1 1 d . . . . .
N19 N 0.25337(10) -0.12035(7) 0.82758(6) 0.0134(2) Uani 1 1 d . . . . .
N20 N 0.56098(11) -0.04593(8) 0.91348(6) 0.0184(2) Uani 1 1 d . . . . .
N21 N 0.19227(10) -0.04740(7) 1.06196(6) 0.0141(2) Uani 1 1 d . . . . .
N22 N 0.46534(10) -0.26935(7) 0.84729(6) 0.0156(2) Uani 1 1 d . . . . .
N23 N 0.17528(10) -0.22859(7) 0.98388(6) 0.0148(2) Uani 1 1 d . . . . .
N24 N 0.22316(11) -0.16736(8) 0.77493(6) 0.0184(2) Uani 1 1 d . . . . .
C1 C 0.33548(12) 0.44801(9) 0.78846(7) 0.0162(2) Uani 1 1 d . . . . .
H1 H 0.404764 0.468429 0.767105 0.019 Uiso 1 1 calc R U . . .
C2 C 0.33603(12) 0.43337(9) 0.86946(7) 0.0141(2) Uani 1 1 d . . . . .
H2 H 0.405706 0.447369 0.886526 0.017 Uiso 1 1 calc R U . . .
C3 C 0.13228(12) 0.46068(8) 0.77904(7) 0.0136(2) Uani 1 1 d . . . . .
H3 H 0.079580 0.482258 0.742144 0.016 Uiso 1 1 calc R U . . .
C4 C 0.20531(11) 0.36263(8) 0.76431(6) 0.0117(2) Uani 1 1 d . . . . .
H4 H 0.184964 0.339804 0.720967 0.014 Uiso 1 1 calc R U . . .
C5 C 0.13165(11) 0.43604(8) 0.90463(7) 0.0126(2) Uani 1 1 d . . . . .
H5 H 0.078179 0.440075 0.949642 0.015 Uiso 1 1 calc R U . . .
C6 C 0.20881(11) 0.34012(8) 0.88748(7) 0.0123(2) Uani 1 1 d . . . . .
H6 H 0.191927 0.301370 0.925954 0.015 Uiso 1 1 calc R U . . .
C7 C 0.22473(11) 0.21611(8) 0.80939(7) 0.0130(2) Uani 1 1 d . . . . .
H7A H 0.206452 0.202369 0.763010 0.016 Uiso 1 1 calc R U . . .
H7B H 0.312525 0.196218 0.809158 0.016 Uiso 1 1 calc R U . . .
C8 C 0.23113(12) 0.10903(8) 0.91041(7) 0.0133(2) Uani 1 1 d . . . . .
H8A H 0.308859 0.120357 0.914135 0.016 Uiso 1 1 calc R U . . .
H8B H 0.183779 0.119367 0.957101 0.016 Uiso 1 1 calc R U . . .
C9 C 0.19270(11) -0.03228(8) 0.93467(6) 0.0116(2) Uani 1 1 d . . . . .
H9 H 0.109023 0.003037 0.950993 0.014 Uiso 1 1 calc R U . . .
C10 C 0.19150(11) -0.11843(8) 0.89658(6) 0.0125(2) Uani 1 1 d . . . . .
H10 H 0.107518 -0.120341 0.894793 0.015 Uiso 1 1 calc R U . . .
C11 C 0.32953(11) -0.15448(8) 0.97877(6) 0.0120(2) Uani 1 1 d . . . . .
H11 H 0.347257 -0.187923 1.021914 0.014 Uiso 1 1 calc R U . . .
C12 C 0.44819(11) -0.15217(8) 0.93127(6) 0.0123(2) Uani 1 1 d . . . . .
H12 H 0.520525 -0.185040 0.952443 0.015 Uiso 1 1 calc R U . . .
C13 C 0.37387(11) -0.11371(8) 0.82175(7) 0.0126(2) Uani 1 1 d . . . . .
H13 H 0.407789 -0.112592 0.771866 0.015 Uiso 1 1 calc R U . . .
C14 C 0.37295(11) -0.02865(8) 0.86246(7) 0.0125(2) Uani 1 1 d . . . . .
H14 H 0.410260 0.009301 0.831214 0.015 Uiso 1 1 calc R U . . .
O23 O 0.73131(11) -0.09704(7) 0.74625(7) 0.0323(3) Uani 1 1 d . . . . .
O24 O 0.91574(10) -0.10786(7) 0.76456(7) 0.0269(2) Uani 1 1 d . . . . .
O25 O 0.51265(9) 0.18122(7) 0.82032(6) 0.0217(2) Uani 1 1 d . . . . .
O26 O 0.62945(10) 0.26245(7) 0.83597(6) 0.0231(2) Uani 1 1 d . . . . .
O27 O 1.11742(9) 0.04980(8) 0.72877(6) 0.0239(2) Uani 1 1 d . . . . .
O28 O 1.11043(9) 0.08231(8) 0.61960(5) 0.0232(2) Uani 1 1 d . . . . .
O29 O 0.72441(10) -0.06067(7) 0.55597(6) 0.0223(2) Uani 1 1 d . . . . .
O30 O 0.91459(9) -0.07147(7) 0.53152(5) 0.0202(2) Uani 1 1 d . . . . .
O31 O 0.54953(9) 0.16744(7) 0.55935(5) 0.0192(2) Uani 1 1 d . . . . .
O32 O 0.65066(9) 0.26354(6) 0.54739(5) 0.0193(2) Uani 1 1 d . . . . .
O33 O 1.02075(9) 0.30512(7) 0.67949(6) 0.0212(2) Uani 1 1 d . . . . .
O36 O 1.00924(9) 0.38477(7) 0.58701(6) 0.0207(2) Uani 1 1 d . . . . .
O37 O 0.37005(9) 0.58448(7) 0.55292(6) 0.0202(2) Uani 1 1 d . . . . .
O38 O 0.46256(9) 0.46290(7) 0.59830(6) 0.0240(2) Uani 1 1 d . . . . .
O39 O 0.48717(10) 0.81916(7) 0.58784(6) 0.0246(2) Uani 1 1 d . . . . .
O40 O 0.56306(9) 0.79683(7) 0.68623(5) 0.0200(2) Uani 1 1 d . . . . .
O41 O 0.72629(10) 0.67741(8) 0.76855(5) 0.0258(2) Uani 1 1 d . . . . .
O42 O 0.86996(11) 0.70260(9) 0.69554(7) 0.0360(3) Uani 1 1 d . . . . .
O43 O 0.77261(10) 0.77394(7) 0.44920(6) 0.0218(2) Uani 1 1 d . . . . .
O44 O 0.90148(10) 0.74927(7) 0.52369(6) 0.0251(2) Uani 1 1 d . . . . .
O45 O 0.76800(9) 0.57296(7) 0.37772(5) 0.01671(19) Uani 1 1 d . . . . .
O46 O 0.89296(9) 0.46760(6) 0.42544(5) 0.01671(19) Uani 1 1 d . . . . .
N25 N 0.79003(10) 0.02151(7) 0.75392(6) 0.01229(19) Uani 1 1 d . . . . .
N26 N 0.68546(9) 0.15985(7) 0.75274(5) 0.01173(19) Uani 1 1 d . . . . .
N27 N 0.96043(9) 0.03894(7) 0.67841(6) 0.01157(19) Uani 1 1 d . . . . .
N28 N 0.80876(10) 0.01522(7) 0.62036(6) 0.01233(19) Uani 1 1 d . . . . .
N29 N 0.69802(9) 0.15853(7) 0.62299(6) 0.01198(19) Uani 1 1 d . . . . .
N30 N 0.84515(9) 0.20300(7) 0.68306(5) 0.01049(18) Uani 1 1 d . . . . .
N31 N 0.81441(11) -0.06738(8) 0.75442(7) 0.0200(2) Uani 1 1 d . . . . .
N32 N 0.60499(10) 0.20262(8) 0.80743(6) 0.0155(2) Uani 1 1 d . . . . .
N33 N 1.07043(10) 0.05991(8) 0.67529(6) 0.0155(2) Uani 1 1 d . . . . .
N34 N 0.81603(11) -0.04209(7) 0.56367(6) 0.0154(2) Uani 1 1 d . . . . .
N35 N 0.62904(10) 0.19772(7) 0.57236(6) 0.0143(2) Uani 1 1 d . . . . .
N38 N 0.85445(9) 0.33746(7) 0.62925(6) 0.01202(19) Uani 1 1 d . . . . .
N39 N 0.96821(10) 0.34262(7) 0.63272(6) 0.0148(2) Uani 1 1 d . . . . .
N40 N 0.76103(9) 0.48872(7) 0.60226(6) 0.01155(19) Uani 1 1 d . . . . .
N41 N 0.56372(9) 0.55935(7) 0.56915(6) 0.01252(19) Uani 1 1 d . . . . .
N42 N 0.54778(10) 0.68435(7) 0.62463(6) 0.0131(2) Uani 1 1 d . . . . .
N43 N 0.74862(10) 0.63381(7) 0.65759(6) 0.0132(2) Uani 1 1 d . . . . .
N44 N 0.74104(10) 0.69689(7) 0.54439(6) 0.0126(2) Uani 1 1 d . . . . .
N45 N 0.75271(10) 0.56486(7) 0.49309(5) 0.01162(19) Uani 1 1 d . . . . .
N46 N 0.45635(10) 0.53546(8) 0.57521(6) 0.0153(2) Uani 1 1 d . . . . .
N47 N 0.53257(10) 0.77322(7) 0.63341(6) 0.0166(2) Uani 1 1 d . . . . .
N48 N 0.78330(11) 0.67551(9) 0.71112(7) 0.0213(2) Uani 1 1 d . . . . .
N49 N 0.81213(11) 0.74259(7) 0.50145(6) 0.0168(2) Uani 1 1 d . . . . .
N50 N 0.80926(10) 0.53434(7) 0.42782(6) 0.01270(19) Uani 1 1 d . . . . .
C15 C 0.68139(11) 0.07511(8) 0.72925(7) 0.0120(2) Uani 1 1 d . . . . .
H15 H 0.608380 0.059781 0.751257 0.014 Uiso 1 1 calc R U . . .
C16 C 0.69201(11) 0.07318(8) 0.64682(7) 0.0123(2) Uani 1 1 d . . . . .
H16 H 0.625145 0.055527 0.629511 0.015 Uiso 1 1 calc R U . . .
C17 C 0.88449(11) 0.06419(8) 0.74538(6) 0.0112(2) Uani 1 1 d . . . . .
H17 H 0.933252 0.051567 0.784974 0.013 Uiso 1 1 calc R U . . .
C18 C 0.81113(11) 0.16290(8) 0.74663(6) 0.0107(2) Uani 1 1 d . . . . .
H18 H 0.824562 0.194231 0.787966 0.013 Uiso 1 1 calc R U . . .
C19 C 0.89744(11) 0.06406(8) 0.61734(6) 0.0111(2) Uani 1 1 d . . . . .
H19 H 0.954108 0.050122 0.573255 0.013 Uiso 1 1 calc R U . . .
C20 C 0.82309(11) 0.16290(8) 0.62152(6) 0.0110(2) Uani 1 1 d . . . . .
H20 H 0.846587 0.193366 0.579035 0.013 Uiso 1 1 calc R U . . .
C21 C 0.79988(11) 0.29878(8) 0.68778(7) 0.0123(2) Uani 1 1 d . . . . .
H21A H 0.711987 0.316478 0.688270 0.015 Uiso 1 1 calc R U . . .
H21B H 0.818008 0.320242 0.731742 0.015 Uiso 1 1 calc R U . . .
C22 C 0.78516(11) 0.39683(8) 0.58185(7) 0.0125(2) Uani 1 1 d . . . . .
H22A H 0.829551 0.386984 0.534346 0.015 Uiso 1 1 calc R U . . .
H22B H 0.708239 0.383182 0.580473 0.015 Uiso 1 1 calc R U . . .
C23 C 0.63837(11) 0.53298(8) 0.62746(6) 0.0118(2) Uani 1 1 d . . . . .
H23 H 0.603526 0.495301 0.660372 0.014 Uiso 1 1 calc R U . . .
C24 C 0.63065(11) 0.62185(8) 0.66467(7) 0.0127(2) Uani 1 1 d . . . . .
H24 H 0.596656 0.622922 0.714748 0.015 Uiso 1 1 calc R U . . .
C25 C 0.55551(11) 0.64987(8) 0.55387(7) 0.0124(2) Uani 1 1 d . . . . .
H25 H 0.481934 0.678187 0.532042 0.015 Uiso 1 1 calc R U . . .
C26 C 0.67341(11) 0.65335(8) 0.50482(7) 0.0120(2) Uani 1 1 d . . . . .
H26 H 0.654963 0.682933 0.460173 0.014 Uiso 1 1 calc R U . . .
C27 C 0.81011(11) 0.62961(8) 0.58853(7) 0.0120(2) Uani 1 1 d . . . . .
H27 H 0.892140 0.636162 0.589472 0.014 Uiso 1 1 calc R U . . .
C28 C 0.81664(11) 0.53940(8) 0.55431(6) 0.0106(2) Uani 1 1 d . . . . .
H28 H 0.901821 0.506472 0.539046 0.013 Uiso 1 1 calc R U . . .
N52 N 0.60638(12) -0.52175(9) 0.78645(7) 0.0242(3) Uani 1 1 d . . . . .
C31 C 0.63237(14) -0.51156(10) 0.91718(8) 0.0220(3) Uani 1 1 d . . . . .
H31A H 0.689164 -0.478135 0.922918 0.033 Uiso 1 1 calc R U . . .
H31B H 0.662080 -0.570419 0.934675 0.033 Uiso 1 1 calc R U . . .
H31C H 0.554574 -0.482346 0.943389 0.033 Uiso 1 1 calc R U . . .
C32 C 0.61939(12) -0.51719(9) 0.84361(8) 0.0178(3) Uani 1 1 d . . . . .
N51 N -0.19103(13) 0.63268(10) 0.94687(7) 0.0283(3) Uani 1 1 d . . . . .
C29 C -0.11052(17) 0.73976(12) 0.86599(9) 0.0316(4) Uani 1 1 d . . . . .
H29A H -0.049169 0.706956 0.829567 0.047 Uiso 1 1 calc R U . . .
H29B H -0.075694 0.774840 0.893789 0.047 Uiso 1 1 calc R U . . .
H29C H -0.176405 0.778236 0.844483 0.047 Uiso 1 1 calc R U . . .
C30 C -0.15559(14) 0.67914(11) 0.91077(8) 0.0233(3) Uani 1 1 d . . . . .
N53 N 0.81106(13) 0.10414(9) 0.46236(7) 0.0263(3) Uani 1 1 d . . . . .
C33 C 0.87817(17) 0.22203(12) 0.38772(9) 0.0304(4) Uani 1 1 d . . . . .
H33A H 0.926302 0.195700 0.344251 0.046 Uiso 1 1 calc R U . . .
H33B H 0.926066 0.247882 0.414395 0.046 Uiso 1 1 calc R U . . .
H33C H 0.807624 0.267482 0.377061 0.046 Uiso 1 1 calc R U . . .
C34 C 0.84035(14) 0.15527(10) 0.42849(8) 0.0213(3) Uani 1 1 d . . . . .
N54 N 0.42158(12) 1.04295(9) 0.71400(7) 0.0242(3) Uani 1 1 d . . . . .
C35 C 0.39044(13) 1.02219(10) 0.58550(8) 0.0211(3) Uani 1 1 d . . . . .
H35A H 0.358022 1.079431 0.565860 0.032 Uiso 1 1 calc R U . . .
H35B H 0.334870 0.986857 0.583001 0.032 Uiso 1 1 calc R U . . .
H35C H 0.467799 0.992739 0.558930 0.032 Uiso 1 1 calc R U . . .
C36 C 0.40623(12) 1.03342(9) 0.65782(8) 0.0176(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 N7 1.2121(18) . ?
O2 N7 1.2219(18) . ?
O3 N8 1.2153(17) . ?
O4 N8 1.2240(17) . ?
O5 N9 1.2238(16) . ?
O6 N9 1.2244(15) . ?
O7 N10 1.2214(16) . ?
O8 N10 1.2172(16) . ?
O9 N11 1.2139(17) . ?
O10 N11 1.2184(17) . ?
O11 N13 1.2231(14) . ?
O12 N13 1.2300(14) . ?
O13 N20 1.2193(16) . ?
O14 N20 1.2164(15) . ?
O15 N21 1.2266(15) . ?
O16 N21 1.2159(14) . ?
O17 N22 1.2204(15) . ?
O18 N22 1.2162(15) . ?
O19 N23 1.2173(15) . ?
O20 N23 1.2110(15) . ?
O21 N24 1.2171(16) . ?
O22 N24 1.2190(16) . ?
N1 N7 1.4187(16) . ?
N1 C1 1.4548(18) . ?
N1 C3 1.4648(17) . ?
N2 N8 1.3768(16) . ?
N2 C5 1.4531(17) . ?
N2 C2 1.4558(17) . ?
N3 N9 1.3426(16) . ?
N3 C1 1.4498(18) . ?
N3 C4 1.4631(16) . ?
N4 N10 1.4112(15) . ?
N4 C2 1.4486(17) . ?
N4 C6 1.5031(17) . ?
N5 N11 1.4187(16) . ?
N5 C3 1.4574(17) . ?
N5 C5 1.4690(17) . ?
N6 C6 1.4353(16) . ?
N6 C4 1.4467(16) . ?
N6 C7 1.4724(16) . ?
N12 N13 1.3702(15) . ?
N12 C7 1.4495(17) . ?
N12 C8 1.4631(16) . ?
N14 C9 1.4319(16) . ?
N14 C14 1.4365(16) . ?
N14 C8 1.4565(16) . ?
N15 N20 1.4115(16) . ?
N15 C12 1.4554(16) . ?
N15 C14 1.5058(16) . ?
N16 N21 1.3992(15) . ?
N16 C11 1.4656(16) . ?
N16 C9 1.4869(16) . ?
N17 N22 1.3929(15) . ?
N17 C12 1.4631(16) . ?
N17 C13 1.4743(16) . ?
N18 N23 1.4534(15) . ?
N18 C11 1.4760(16) . ?
N18 C10 1.4890(16) . ?
N19 N24 1.4086(16) . ?
N19 C10 1.4354(16) . ?
N19 C13 1.4387(17) . ?
C1 C2 1.5849(19) . ?
C1 H1 1.0000 . ?
C2 H2 1.0000 . ?
C3 C4 1.5705(18) . ?
C3 H3 1.0000 . ?
C4 H4 1.0000 . ?
C5 C6 1.5614(18) . ?
C5 H5 1.0000 . ?
C6 H6 1.0000 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.5719(18) . ?
C9 H9 1.0000 . ?
C10 H10 1.0000 . ?
C11 C12 1.5798(18) . ?
C11 H11 1.0000 . ?
C12 H12 1.0000 . ?
C13 C14 1.5741(18) . ?
C13 H13 1.0000 . ?
C14 H14 1.0000 . ?
O23 N31 1.2246(16) . ?
O24 N31 1.2246(16) . ?
O25 N32 1.2214(15) . ?
O26 N32 1.2266(15) . ?
O27 N33 1.2226(15) . ?
O28 N33 1.2131(15) . ?
O29 N34 1.2195(15) . ?
O30 N34 1.2122(15) . ?
O31 N35 1.2177(14) . ?
O32 N35 1.2291(15) . ?
O33 N39 1.2183(14) . ?
O36 N39 1.2374(15) . ?
O37 N46 1.2194(15) . ?
O38 N46 1.2243(15) . ?
O39 N47 1.2203(15) . ?
O40 N47 1.2216(15) . ?
O41 N48 1.2204(16) . ?
O42 N48 1.2164(17) . ?
O43 N49 1.2120(15) . ?
O44 N49 1.2143(15) . ?
O45 N50 1.2235(14) . ?
O46 N50 1.2286(14) . ?
N25 N31 1.3676(16) . ?
N25 C17 1.4476(16) . ?
N25 C15 1.4577(16) . ?
N26 N32 1.3729(15) . ?
N26 C15 1.4470(16) . ?
N26 C18 1.4801(16) . ?
N27 N33 1.4162(15) . ?
N27 C19 1.4673(16) . ?
N27 C17 1.4698(16) . ?
N28 N34 1.4155(15) . ?
N28 C16 1.4575(16) . ?
N28 C19 1.4605(16) . ?
N29 N35 1.3836(15) . ?
N29 C16 1.4521(16) . ?
N29 C20 1.4864(16) . ?
N30 C20 1.4435(16) . ?
N30 C18 1.4457(16) . ?
N30 C21 1.4722(16) . ?
N38 N39 1.3712(15) . ?
N38 C21 1.4499(16) . ?
N38 C22 1.4643(16) . ?
N40 C28 1.4393(16) . ?
N40 C23 1.4405(16) . ?
N40 C22 1.4633(16) . ?
N41 N46 1.4068(15) . ?
N41 C25 1.4516(16) . ?
N41 C23 1.5018(16) . ?
N42 N47 1.3894(15) . ?
N42 C25 1.4650(17) . ?
N42 C24 1.4757(16) . ?
N43 N48 1.3985(16) . ?
N43 C27 1.4311(16) . ?
N43 C24 1.4400(17) . ?
N44 N49 1.4404(15) . ?
N44 C26 1.4741(16) . ?
N44 C27 1.4878(16) . ?
N45 N50 1.3778(15) . ?
N45 C26 1.4611(16) . ?
N45 C28 1.4763(16) . ?
C15 C16 1.5859(18) . ?
C15 H15 1.0000 . ?
C16 H16 1.0000 . ?
C17 C18 1.5701(17) . ?
C17 H17 1.0000 . ?
C18 H18 1.0000 . ?
C19 C20 1.5736(17) . ?
C19 H19 1.0000 . ?
C20 H20 1.0000 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.5728(18) . ?
C23 H23 1.0000 . ?
C24 H24 1.0000 . ?
C25 C26 1.5920(18) . ?
C25 H25 1.0000 . ?
C26 H26 1.0000 . ?
C27 C28 1.5699(17) . ?
C27 H27 1.0000 . ?
C28 H28 1.0000 . ?
N52 C32 1.1425(19) . ?
C31 C32 1.459(2) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
N51 C30 1.141(2) . ?
C29 C30 1.457(2) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
N53 C34 1.142(2) . ?
C33 C34 1.455(2) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
N54 C36 1.1436(19) . ?
C35 C36 1.456(2) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 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 118.04(11) . . ?
N7 N1 C3 117.10(11) . . ?
C1 N1 C3 108.40(10) . . ?
N8 N2 C5 120.47(11) . . ?
N8 N2 C2 120.35(11) . . ?
C5 N2 C2 111.17(10) . . ?
N9 N3 C1 124.02(11) . . ?
N9 N3 C4 124.06(11) . . ?
C1 N3 C4 111.09(10) . . ?
N10 N4 C2 115.81(10) . . ?
N10 N4 C6 115.56(10) . . ?
C2 N4 C6 107.54(10) . . ?
N11 N5 C3 113.44(11) . . ?
N11 N5 C5 113.87(11) . . ?
C3 N5 C5 114.43(10) . . ?
C6 N6 C4 113.74(10) . . ?
C6 N6 C7 115.19(10) . . ?
C4 N6 C7 114.11(10) . . ?
O1 N7 O2 127.96(13) . . ?
O1 N7 N1 115.70(13) . . ?
O2 N7 N1 116.15(13) . . ?
O3 N8 O4 127.70(13) . . ?
O3 N8 N2 116.39(12) . . ?
O4 N8 N2 115.86(12) . . ?
O5 N9 O6 126.46(13) . . ?
O5 N9 N3 116.96(12) . . ?
O6 N9 N3 116.56(13) . . ?
O8 N10 O7 126.38(12) . . ?
O8 N10 N4 118.22(12) . . ?
O7 N10 N4 115.21(11) . . ?
O9 N11 O10 126.84(13) . . ?
O9 N11 N5 116.94(13) . . ?
O10 N11 N5 116.15(13) . . ?
N13 N12 C7 116.67(10) . . ?
N13 N12 C8 117.00(10) . . ?
C7 N12 C8 124.73(11) . . ?
O11 N13 O12 125.60(12) . . ?
O11 N13 N12 117.38(11) . . ?
O12 N13 N12 117.02(11) . . ?
C9 N14 C14 113.65(10) . . ?
C9 N14 C8 116.14(10) . . ?
C14 N14 C8 116.92(11) . . ?
N20 N15 C12 115.47(10) . . ?
N20 N15 C14 116.12(10) . . ?
C12 N15 C14 107.72(10) . . ?
N21 N16 C11 117.27(10) . . ?
N21 N16 C9 118.05(10) . . ?
C11 N16 C9 107.68(10) . . ?
N22 N17 C12 117.39(10) . . ?
N22 N17 C13 120.45(10) . . ?
C12 N17 C13 109.87(10) . . ?
N23 N18 C11 111.15(10) . . ?
N23 N18 C10 113.24(10) . . ?
C11 N18 C10 105.95(10) . . ?
N24 N19 C10 118.23(11) . . ?
N24 N19 C13 117.94(10) . . ?
C10 N19 C13 116.95(10) . . ?
O14 N20 O13 126.14(13) . . ?
O14 N20 N15 117.93(11) . . ?
O13 N20 N15 115.68(11) . . ?
O16 N21 O15 126.39(12) . . ?
O16 N21 N16 116.99(11) . . ?
O15 N21 N16 116.49(11) . . ?
O18 N22 O17 127.48(12) . . ?
O18 N22 N17 115.79(11) . . ?
O17 N22 N17 116.70(11) . . ?
O20 N23 O19 127.19(12) . . ?
O20 N23 N18 115.78(11) . . ?
O19 N23 N18 116.97(11) . . ?
O21 N24 O22 127.41(13) . . ?
O21 N24 N19 116.59(12) . . ?
O22 N24 N19 115.92(12) . . ?
N3 C1 N1 101.81(11) . . ?
N3 C1 C2 110.20(11) . . ?
N1 C1 C2 106.68(10) . . ?
N3 C1 H1 112.5 . . ?
N1 C1 H1 112.5 . . ?
C2 C1 H1 112.5 . . ?
N4 C2 N2 99.88(10) . . ?
N4 C2 C1 108.57(10) . . ?
N2 C2 C1 113.06(11) . . ?
N4 C2 H2 111.6 . . ?
N2 C2 H2 111.6 . . ?
C1 C2 H2 111.6 . . ?
N5 C3 N1 107.14(11) . . ?
N5 C3 C4 111.00(10) . . ?
N1 C3 C4 106.05(10) . . ?
N5 C3 H3 110.8 . . ?
N1 C3 H3 110.8 . . ?
C4 C3 H3 110.8 . . ?
N6 C4 N3 113.72(10) . . ?
N6 C4 C3 109.80(10) . . ?
N3 C4 C3 100.90(10) . . ?
N6 C4 H4 110.7 . . ?
N3 C4 H4 110.7 . . ?
C3 C4 H4 110.7 . . ?
N2 C5 N5 110.58(10) . . ?
N2 C5 C6 101.24(10) . . ?
N5 C5 C6 111.51(10) . . ?
N2 C5 H5 111.0 . . ?
N5 C5 H5 111.0 . . ?
C6 C5 H5 111.0 . . ?
N6 C6 N4 112.81(10) . . ?
N6 C6 C5 109.52(10) . . ?
N4 C6 C5 104.54(10) . . ?
N6 C6 H6 109.9 . . ?
N4 C6 H6 109.9 . . ?
C5 C6 H6 109.9 . . ?
N12 C7 N6 110.24(10) . . ?
N12 C7 H7A 109.6 . . ?
N6 C7 H7A 109.6 . . ?
N12 C7 H7B 109.6 . . ?
N6 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
N14 C8 N12 113.59(10) . . ?
N14 C8 H8A 108.8 . . ?
N12 C8 H8A 108.8 . . ?
N14 C8 H8B 108.8 . . ?
N12 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
N14 C9 N16 112.47(10) . . ?
N14 C9 C10 110.81(10) . . ?
N16 C9 C10 103.31(9) . . ?
N14 C9 H9 110.0 . . ?
N16 C9 H9 110.0 . . ?
C10 C9 H9 110.0 . . ?
N19 C10 N18 111.43(10) . . ?
N19 C10 C9 107.89(10) . . ?
N18 C10 C9 105.70(10) . . ?
N19 C10 H10 110.6 . . ?
N18 C10 H10 110.6 . . ?
C9 C10 H10 110.6 . . ?
N16 C11 N18 103.97(10) . . ?
N16 C11 C12 108.73(10) . . ?
N18 C11 C12 109.62(10) . . ?
N16 C11 H11 111.4 . . ?
N18 C11 H11 111.4 . . ?
C12 C11 H11 111.4 . . ?
N15 C12 N17 99.65(10) . . ?
N15 C12 C11 109.26(10) . . ?
N17 C12 C11 113.93(10) . . ?
N15 C12 H12 111.2 . . ?
N17 C12 H12 111.2 . . ?
C11 C12 H12 111.2 . . ?
N19 C13 N17 113.88(10) . . ?
N19 C13 C14 108.40(10) . . ?
N17 C13 C14 101.20(10) . . ?
N19 C13 H13 111.0 . . ?
N17 C13 H13 111.0 . . ?
C14 C13 H13 111.0 . . ?
N14 C14 N15 111.64(10) . . ?
N14 C14 C13 110.04(10) . . ?
N15 C14 C13 104.14(9) . . ?
N14 C14 H14 110.3 . . ?
N15 C14 H14 110.3 . . ?
C13 C14 H14 110.3 . . ?
N31 N25 C17 121.63(10) . . ?
N31 N25 C15 120.89(11) . . ?
C17 N25 C15 111.55(10) . . ?
N32 N26 C15 119.67(10) . . ?
N32 N26 C18 119.75(10) . . ?
C15 N26 C18 109.71(10) . . ?
N33 N27 C19 114.59(10) . . ?
N33 N27 C17 112.96(10) . . ?
C19 N27 C17 114.21(10) . . ?
N34 N28 C16 118.22(10) . . ?
N34 N28 C19 117.66(10) . . ?
C16 N28 C19 108.77(10) . . ?
N35 N29 C16 119.04(10) . . ?
N35 N29 C20 120.91(10) . . ?
C16 N29 C20 108.51(9) . . ?
C20 N30 C18 113.08(10) . . ?
C20 N30 C21 115.30(10) . . ?
C18 N30 C21 112.03(10) . . ?
O24 N31 O23 127.61(12) . . ?
O24 N31 N25 116.34(12) . . ?
O23 N31 N25 116.03(12) . . ?
O25 N32 O26 126.06(12) . . ?
O25 N32 N26 117.09(11) . . ?
O26 N32 N26 116.69(11) . . ?
O28 N33 O27 126.92(12) . . ?
O28 N33 N27 117.08(11) . . ?
O27 N33 N27 115.92(11) . . ?
O30 N34 O29 127.66(12) . . ?
O30 N34 N28 115.92(11) . . ?
O29 N34 N28 116.21(11) . . ?
O31 N35 O32 126.14(11) . . ?
O31 N35 N29 118.00(11) . . ?
O32 N35 N29 115.73(11) . . ?
N39 N38 C21 116.60(10) . . ?
N39 N38 C22 116.54(10) . . ?
C21 N38 C22 123.13(10) . . ?
O33 N39 O36 125.50(11) . . ?
O33 N39 N38 118.01(11) . . ?
O36 N39 N38 116.49(11) . . ?
C28 N40 C23 113.09(10) . . ?
C28 N40 C22 115.11(10) . . ?
C23 N40 C22 115.69(10) . . ?
N46 N41 C25 116.59(10) . . ?
N46 N41 C23 116.05(10) . . ?
C25 N41 C23 108.50(10) . . ?
N47 N42 C25 117.98(10) . . ?
N47 N42 C24 119.53(10) . . ?
C25 N42 C24 110.29(10) . . ?
N48 N43 C27 119.83(11) . . ?
N48 N43 C24 119.85(11) . . ?
C27 N43 C24 117.01(10) . . ?
N49 N44 C26 113.70(10) . . ?
N49 N44 C27 114.34(10) . . ?
C26 N44 C27 106.78(10) . . ?
N50 N45 C26 121.70(10) . . ?
N50 N45 C28 119.49(10) . . ?
C26 N45 C28 109.06(10) . . ?
O37 N46 O38 126.26(12) . . ?
O37 N46 N41 118.45(11) . . ?
O38 N46 N41 115.05(11) . . ?
O39 N47 O40 127.36(12) . . ?
O39 N47 N42 115.72(11) . . ?
O40 N47 N42 116.89(11) . . ?
O42 N48 O41 127.51(13) . . ?
O42 N48 N43 116.05(12) . . ?
O41 N48 N43 116.36(12) . . ?
O43 N49 O44 127.42(12) . . ?
O43 N49 N44 116.27(11) . . ?
O44 N49 N44 116.18(11) . . ?
O45 N50 O46 125.97(11) . . ?
O45 N50 N45 117.49(11) . . ?
O46 N50 N45 116.42(10) . . ?
N26 C15 N25 99.04(10) . . ?
N26 C15 C16 108.81(10) . . ?
N25 C15 C16 111.67(10) . . ?
N26 C15 H15 112.2 . . ?
N25 C15 H15 112.2 . . ?
C16 C15 H15 112.2 . . ?
N29 C16 N28 104.00(10) . . ?
N29 C16 C15 107.91(10) . . ?
N28 C16 C15 107.78(10) . . ?
N29 C16 H16 112.2 . . ?
N28 C16 H16 112.2 . . ?
C15 C16 H16 112.2 . . ?
N25 C17 N27 111.12(10) . . ?
N25 C17 C18 101.61(9) . . ?
N27 C17 C18 110.91(10) . . ?
N25 C17 H17 111.0 . . ?
N27 C17 H17 111.0 . . ?
C18 C17 H17 111.0 . . ?
N30 C18 N26 111.95(10) . . ?
N30 C18 C17 109.89(10) . . ?
N26 C18 C17 103.56(9) . . ?
N30 C18 H18 110.4 . . ?
N26 C18 H18 110.4 . . ?
C17 C18 H18 110.4 . . ?
N28 C19 N27 106.01(10) . . ?
N28 C19 C20 105.19(10) . . ?
N27 C19 C20 111.97(10) . . ?
N28 C19 H19 111.1 . . ?
N27 C19 H19 111.1 . . ?
C20 C19 H19 111.1 . . ?
N30 C20 N29 114.16(10) . . ?
N30 C20 C19 108.75(10) . . ?
N29 C20 C19 103.03(9) . . ?
N30 C20 H20 110.2 . . ?
N29 C20 H20 110.2 . . ?
C19 C20 H20 110.2 . . ?
N38 C21 N30 110.52(10) . . ?
N38 C21 H21A 109.5 . . ?
N30 C21 H21A 109.5 . . ?
N38 C21 H21B 109.5 . . ?
N30 C21 H21B 109.5 . . ?
H21A C21 H21B 108.1 . . ?
N40 C22 N38 112.89(10) . . ?
N40 C22 H22A 109.0 . . ?
N38 C22 H22A 109.0 . . ?
N40 C22 H22B 109.0 . . ?
N38 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
N40 C23 N41 112.03(10) . . ?
N40 C23 C24 109.96(10) . . ?
N41 C23 C24 104.07(9) . . ?
N40 C23 H23 110.2 . . ?
N41 C23 H23 110.2 . . ?
C24 C23 H23 110.2 . . ?
N43 C24 N42 113.24(10) . . ?
N43 C24 C23 108.44(10) . . ?
N42 C24 C23 101.22(10) . . ?
N43 C24 H24 111.2 . . ?
N42 C24 H24 111.2 . . ?
C23 C24 H24 111.2 . . ?
N41 C25 N42 99.53(10) . . ?
N41 C25 C26 108.44(10) . . ?
N42 C25 C26 113.82(10) . . ?
N41 C25 H25 111.5 . . ?
N42 C25 H25 111.5 . . ?
C26 C25 H25 111.5 . . ?
N45 C26 N44 103.28(10) . . ?
N45 C26 C25 109.02(10) . . ?
N44 C26 C25 107.94(10) . . ?
N45 C26 H26 112.1 . . ?
N44 C26 H26 112.1 . . ?
C25 C26 H26 112.1 . . ?
N43 C27 N44 111.00(10) . . ?
N43 C27 C28 107.99(10) . . ?
N44 C27 C28 105.64(10) . . ?
N43 C27 H27 110.7 . . ?
N44 C27 H27 110.7 . . ?
C28 C27 H27 110.7 . . ?
N40 C28 N45 112.76(10) . . ?
N40 C28 C27 110.74(10) . . ?
N45 C28 C27 102.93(9) . . ?
N40 C28 H28 110.1 . . ?
N45 C28 H28 110.1 . . ?
C27 C28 H28 110.1 . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N52 C32 C31 178.28(15) . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N51 C30 C29 178.72(18) . . ?
C34 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C34 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N53 C34 C33 177.84(17) . . ?
C36 C35 H35A 109.5 . . ?
C36 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C36 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N54 C36 C35 178.00(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N7 O1 163.45(12) . . . . ?
C3 N1 N7 O1 31.06(18) . . . . ?
C1 N1 N7 O2 -21.15(18) . . . . ?
C3 N1 N7 O2 -153.54(12) . . . . ?
C5 N2 N8 O3 22.15(18) . . . . ?
C2 N2 N8 O3 168.26(12) . . . . ?
C5 N2 N8 O4 -160.09(12) . . . . ?
C2 N2 N8 O4 -13.98(18) . . . . ?
C1 N3 N9 O5 -173.71(13) . . . . ?
C4 N3 N9 O5 -5.1(2) . . . . ?
C1 N3 N9 O6 7.7(2) . . . . ?
C4 N3 N9 O6 176.28(13) . . . . ?
C2 N4 N10 O8 -16.91(17) . . . . ?
C6 N4 N10 O8 -143.96(12) . . . . ?
C2 N4 N10 O7 167.71(11) . . . . ?
C6 N4 N10 O7 40.66(15) . . . . ?
C3 N5 N11 O9 150.92(13) . . . . ?
C5 N5 N11 O9 17.69(17) . . . . ?
C3 N5 N11 O10 -31.82(17) . . . . ?
C5 N5 N11 O10 -165.05(12) . . . . ?
C7 N12 N13 O11 -10.06(17) . . . . ?
C8 N12 N13 O11 -176.38(12) . . . . ?
C7 N12 N13 O12 170.32(11) . . . . ?
C8 N12 N13 O12 4.00(17) . . . . ?
C12 N15 N20 O14 -24.12(17) . . . . ?
C14 N15 N20 O14 -151.64(12) . . . . ?
C12 N15 N20 O13 161.21(12) . . . . ?
C14 N15 N20 O13 33.69(17) . . . . ?
C11 N16 N21 O16 23.76(16) . . . . ?
C9 N16 N21 O16 155.21(11) . . . . ?
C11 N16 N21 O15 -160.19(11) . . . . ?
C9 N16 N21 O15 -28.74(16) . . . . ?
C12 N17 N22 O18 -24.31(17) . . . . ?
C13 N17 N22 O18 -162.79(12) . . . . ?
C12 N17 N22 O17 157.69(11) . . . . ?
C13 N17 N22 O17 19.21(17) . . . . ?
C11 N18 N23 O20 -44.09(14) . . . . ?
C10 N18 N23 O20 -163.23(11) . . . . ?
C11 N18 N23 O19 138.50(11) . . . . ?
C10 N18 N23 O19 19.37(15) . . . . ?
C10 N19 N24 O21 -0.91(17) . . . . ?
C13 N19 N24 O21 149.20(12) . . . . ?
C10 N19 N24 O22 176.11(11) . . . . ?
C13 N19 N24 O22 -33.77(17) . . . . ?
N9 N3 C1 N1 134.71(13) . . . . ?
C4 N3 C1 N1 -35.19(14) . . . . ?
N9 N3 C1 C2 -112.38(14) . . . . ?
C4 N3 C1 C2 77.73(13) . . . . ?
N7 N1 C1 N3 -104.85(12) . . . . ?
C3 N1 C1 N3 31.29(13) . . . . ?
N7 N1 C1 C2 139.63(11) . . . . ?
C3 N1 C1 C2 -84.23(12) . . . . ?
N10 N4 C2 N2 -94.49(12) . . . . ?
C6 N4 C2 N2 36.48(12) . . . . ?
N10 N4 C2 C1 146.96(11) . . . . ?
C6 N4 C2 C1 -82.08(12) . . . . ?
N8 N2 C2 N4 171.10(11) . . . . ?
C5 N2 C2 N4 -39.92(12) . . . . ?
N8 N2 C2 C1 -73.73(15) . . . . ?
C5 N2 C2 C1 75.25(13) . . . . ?
N3 C1 C2 N4 3.46(14) . . . . ?
N1 C1 C2 N4 113.20(11) . . . . ?
N3 C1 C2 N2 -106.40(12) . . . . ?
N1 C1 C2 N2 3.34(14) . . . . ?
N11 N5 C3 N1 163.48(10) . . . . ?
C5 N5 C3 N1 -63.56(13) . . . . ?
N11 N5 C3 C4 -81.15(13) . . . . ?
C5 N5 C3 C4 51.81(14) . . . . ?
N7 N1 C3 N5 -122.16(12) . . . . ?
C1 N1 C3 N5 101.23(12) . . . . ?
N7 N1 C3 C4 119.22(12) . . . . ?
C1 N1 C3 C4 -17.39(13) . . . . ?
C6 N6 C4 N3 54.72(14) . . . . ?
C7 N6 C4 N3 -80.20(13) . . . . ?
C6 N6 C4 C3 -57.47(13) . . . . ?
C7 N6 C4 C3 167.61(10) . . . . ?
N9 N3 C4 N6 96.81(15) . . . . ?
C1 N3 C4 N6 -93.30(13) . . . . ?
N9 N3 C4 C3 -145.72(13) . . . . ?
C1 N3 C4 C3 24.17(13) . . . . ?
N5 C3 C4 N6 0.60(14) . . . . ?
N1 C3 C4 N6 116.63(11) . . . . ?
N5 C3 C4 N3 -119.71(11) . . . . ?
N1 C3 C4 N3 -3.68(12) . . . . ?
N8 N2 C5 N5 56.83(15) . . . . ?
C2 N2 C5 N5 -92.10(12) . . . . ?
N8 N2 C5 C6 175.12(11) . . . . ?
C2 N2 C5 C6 26.19(13) . . . . ?
N11 N5 C5 N2 -164.86(10) . . . . ?
C3 N5 C5 N2 62.38(14) . . . . ?
N11 N5 C5 C6 83.31(13) . . . . ?
C3 N5 C5 C6 -49.45(14) . . . . ?
C4 N6 C6 N4 -55.96(13) . . . . ?
C7 N6 C6 N4 78.46(13) . . . . ?
C4 N6 C6 C5 60.02(13) . . . . ?
C7 N6 C6 C5 -165.56(10) . . . . ?
N10 N4 C6 N6 -132.01(11) . . . . ?
C2 N4 C6 N6 96.89(12) . . . . ?
N10 N4 C6 C5 109.08(11) . . . . ?
C2 N4 C6 C5 -22.02(13) . . . . ?
N2 C5 C6 N6 -123.25(11) . . . . ?
N5 C5 C6 N6 -5.63(14) . . . . ?
N2 C5 C6 N4 -2.12(12) . . . . ?
N5 C5 C6 N4 115.49(11) . . . . ?
N13 N12 C7 N6 77.56(13) . . . . ?
C8 N12 C7 N6 -117.30(13) . . . . ?
C6 N6 C7 N12 62.68(14) . . . . ?
C4 N6 C7 N12 -163.07(10) . . . . ?
C9 N14 C8 N12 -114.95(12) . . . . ?
C14 N14 C8 N12 106.43(13) . . . . ?
N13 N12 C8 N14 65.55(15) . . . . ?
C7 N12 C8 N14 -99.55(14) . . . . ?
C14 N14 C9 N16 58.19(14) . . . . ?
C8 N14 C9 N16 -81.76(13) . . . . ?
C14 N14 C9 C10 -56.88(14) . . . . ?
C8 N14 C9 C10 163.17(10) . . . . ?
N21 N16 C9 N14 127.28(11) . . . . ?
C11 N16 C9 N14 -97.10(12) . . . . ?
N21 N16 C9 C10 -113.19(11) . . . . ?
C11 N16 C9 C10 22.43(12) . . . . ?
N24 N19 C10 N18 90.87(13) . . . . ?
C13 N19 C10 N18 -59.54(14) . . . . ?
N24 N19 C10 C9 -153.52(10) . . . . ?
C13 N19 C10 C9 56.07(14) . . . . ?
N23 N18 C10 N19 -142.17(10) . . . . ?
C11 N18 C10 N19 95.74(12) . . . . ?
N23 N18 C10 C9 100.89(11) . . . . ?
C11 N18 C10 C9 -21.20(12) . . . . ?
N14 C9 C10 N19 0.84(14) . . . . ?
N16 C9 C10 N19 -119.83(10) . . . . ?
N14 C9 C10 N18 120.15(11) . . . . ?
N16 C9 C10 N18 -0.52(12) . . . . ?
N21 N16 C11 N18 99.75(12) . . . . ?
C9 N16 C11 N18 -36.27(12) . . . . ?
N21 N16 C11 C12 -143.53(11) . . . . ?
C9 N16 C11 C12 80.45(12) . . . . ?
N23 N18 C11 N16 -88.19(11) . . . . ?
C10 N18 C11 N16 35.22(12) . . . . ?
N23 N18 C11 C12 155.71(10) . . . . ?
C10 N18 C11 C12 -80.88(12) . . . . ?
N20 N15 C12 N17 -93.28(12) . . . . ?
C14 N15 C12 N17 38.33(12) . . . . ?
N20 N15 C12 C11 147.03(11) . . . . ?
C14 N15 C12 C11 -81.36(12) . . . . ?
N22 N17 C12 N15 175.35(10) . . . . ?
C13 N17 C12 N15 -42.06(12) . . . . ?
N22 N17 C12 C11 -68.44(14) . . . . ?
C13 N17 C12 C11 74.15(13) . . . . ?
N16 C11 C12 N15 0.62(13) . . . . ?
N18 C11 C12 N15 113.66(11) . . . . ?
N16 C11 C12 N17 -109.83(11) . . . . ?
N18 C11 C12 N17 3.21(14) . . . . ?
N24 N19 C13 N17 -93.70(13) . . . . ?
C10 N19 C13 N17 56.79(15) . . . . ?
N24 N19 C13 C14 154.50(11) . . . . ?
C10 N19 C13 C14 -55.00(14) . . . . ?
N22 N17 C13 N19 53.38(15) . . . . ?
C12 N17 C13 N19 -87.88(13) . . . . ?
N22 N17 C13 C14 169.47(11) . . . . ?
C12 N17 C13 C14 28.20(13) . . . . ?
C9 N14 C14 N15 -57.26(14) . . . . ?
C8 N14 C14 N15 82.36(13) . . . . ?
C9 N14 C14 C13 57.85(13) . . . . ?
C8 N14 C14 C13 -162.53(10) . . . . ?
N20 N15 C14 N14 -132.35(11) . . . . ?
C12 N15 C14 N14 96.39(12) . . . . ?
N20 N15 C14 C13 108.95(12) . . . . ?
C12 N15 C14 C13 -22.31(12) . . . . ?
N19 C13 C14 N14 -2.97(13) . . . . ?
N17 C13 C14 N14 -123.03(11) . . . . ?
N19 C13 C14 N15 116.81(10) . . . . ?
N17 C13 C14 N15 -3.25(12) . . . . ?
C17 N25 N31 O24 17.43(19) . . . . ?
C15 N25 N31 O24 168.01(12) . . . . ?
C17 N25 N31 O23 -164.20(13) . . . . ?
C15 N25 N31 O23 -13.62(19) . . . . ?
C15 N26 N32 O25 -21.60(17) . . . . ?
C18 N26 N32 O25 -162.20(11) . . . . ?
C15 N26 N32 O26 162.77(11) . . . . ?
C18 N26 N32 O26 22.17(17) . . . . ?
C19 N27 N33 O28 -11.79(16) . . . . ?
C17 N27 N33 O28 -144.92(12) . . . . ?
C19 N27 N33 O27 171.18(11) . . . . ?
C17 N27 N33 O27 38.05(15) . . . . ?
C16 N28 N34 O30 160.92(11) . . . . ?
C19 N28 N34 O30 27.03(16) . . . . ?
C16 N28 N34 O29 -23.94(16) . . . . ?
C19 N28 N34 O29 -157.84(11) . . . . ?
C16 N29 N35 O31 13.85(17) . . . . ?
C20 N29 N35 O31 152.93(12) . . . . ?
C16 N29 N35 O32 -169.98(11) . . . . ?
C20 N29 N35 O32 -30.89(16) . . . . ?
C21 N38 N39 O33 9.07(17) . . . . ?
C22 N38 N39 O33 168.03(11) . . . . ?
C21 N38 N39 O36 -171.67(11) . . . . ?
C22 N38 N39 O36 -12.71(17) . . . . ?
C25 N41 N46 O37 15.79(17) . . . . ?
C23 N41 N46 O37 145.56(12) . . . . ?
C25 N41 N46 O38 -169.42(12) . . . . ?
C23 N41 N46 O38 -39.65(16) . . . . ?
C25 N42 N47 O39 24.06(17) . . . . ?
C24 N42 N47 O39 162.84(12) . . . . ?
C25 N42 N47 O40 -157.69(12) . . . . ?
C24 N42 N47 O40 -18.91(17) . . . . ?
C27 N43 N48 O42 -3.54(19) . . . . ?
C24 N43 N48 O42 -162.40(13) . . . . ?
C27 N43 N48 O41 179.32(12) . . . . ?
C24 N43 N48 O41 20.46(18) . . . . ?
C26 N44 N49 O43 32.12(15) . . . . ?
C27 N44 N49 O43 155.13(11) . . . . ?
C26 N44 N49 O44 -151.68(12) . . . . ?
C27 N44 N49 O44 -28.68(16) . . . . ?
C26 N45 N50 O45 -19.42(17) . . . . ?
C28 N45 N50 O45 -161.65(11) . . . . ?
C26 N45 N50 O46 164.44(11) . . . . ?
C28 N45 N50 O46 22.21(16) . . . . ?
N32 N26 C15 N25 -108.76(12) . . . . ?
C18 N26 C15 N25 35.41(12) . . . . ?
N32 N26 C15 C16 134.55(11) . . . . ?
C18 N26 C15 C16 -81.28(12) . . . . ?
N31 N25 C15 N26 168.50(11) . . . . ?
C17 N25 C15 N26 -38.23(12) . . . . ?
N31 N25 C15 C16 -77.02(14) . . . . ?
C17 N25 C15 C16 76.25(13) . . . . ?
N35 N29 C16 N28 110.99(12) . . . . ?
C20 N29 C16 N28 -32.67(12) . . . . ?
N35 N29 C16 C15 -134.72(11) . . . . ?
C20 N29 C16 C15 81.62(12) . . . . ?
N34 N28 C16 N29 -106.86(12) . . . . ?
C19 N28 C16 N29 30.76(12) . . . . ?
N34 N28 C16 C15 138.76(11) . . . . ?
C19 N28 C16 C15 -83.62(12) . . . . ?
N26 C15 C16 N29 -1.97(13) . . . . ?
N25 C15 C16 N29 -110.27(11) . . . . ?
N26 C15 C16 N28 109.78(11) . . . . ?
N25 C15 C16 N28 1.49(14) . . . . ?
N31 N25 C17 N27 60.66(15) . . . . ?
C15 N25 C17 N27 -92.39(12) . . . . ?
N31 N25 C17 C18 178.69(11) . . . . ?
C15 N25 C17 C18 25.64(13) . . . . ?
N33 N27 C17 N25 -164.36(10) . . . . ?
C19 N27 C17 N25 62.32(13) . . . . ?
N33 N27 C17 C18 83.39(12) . . . . ?
C19 N27 C17 C18 -49.93(13) . . . . ?
C20 N30 C18 N26 -54.08(13) . . . . ?
C21 N30 C18 N26 78.26(12) . . . . ?
C20 N30 C18 C17 60.42(13) . . . . ?
C21 N30 C18 C17 -167.24(10) . . . . ?
N32 N26 C18 N30 -118.88(12) . . . . ?
C15 N26 C18 N30 96.99(12) . . . . ?
N32 N26 C18 C17 122.79(11) . . . . ?
C15 N26 C18 C17 -21.35(12) . . . . ?
N25 C17 C18 N30 -122.12(10) . . . . ?
N27 C17 C18 N30 -3.94(14) . . . . ?
N25 C17 C18 N26 -2.37(12) . . . . ?
N27 C17 C18 N26 115.81(10) . . . . ?
N34 N28 C19 N27 -120.49(11) . . . . ?
C16 N28 C19 N27 101.62(11) . . . . ?
N34 N28 C19 C20 120.74(11) . . . . ?
C16 N28 C19 C20 -17.15(12) . . . . ?
N33 N27 C19 N28 163.42(10) . . . . ?
C17 N27 C19 N28 -64.03(12) . . . . ?
N33 N27 C19 C20 -82.39(12) . . . . ?
C17 N27 C19 C20 50.15(13) . . . . ?
C18 N30 C20 N29 54.34(13) . . . . ?
C21 N30 C20 N29 -76.38(13) . . . . ?
C18 N30 C20 C19 -60.06(13) . . . . ?
C21 N30 C20 C19 169.21(10) . . . . ?
N35 N29 C20 N30 121.20(12) . . . . ?
C16 N29 C20 N30 -95.94(12) . . . . ?
N35 N29 C20 C19 -121.06(11) . . . . ?
C16 N29 C20 C19 21.80(12) . . . . ?
N28 C19 C20 N30 118.75(10) . . . . ?
N27 C19 C20 N30 4.06(14) . . . . ?
N28 C19 C20 N29 -2.72(12) . . . . ?
N27 C19 C20 N29 -117.42(10) . . . . ?
N39 N38 C21 N30 -78.90(13) . . . . ?
C22 N38 C21 N30 123.65(12) . . . . ?
C20 N30 C21 N38 -60.00(13) . . . . ?
C18 N30 C21 N38 168.77(10) . . . . ?
C28 N40 C22 N38 114.66(12) . . . . ?
C23 N40 C22 N38 -110.43(12) . . . . ?
N39 N38 C22 N40 -64.07(14) . . . . ?
C21 N38 C22 N40 93.39(14) . . . . ?
C28 N40 C23 N41 56.73(13) . . . . ?
C22 N40 C23 N41 -79.08(13) . . . . ?
C28 N40 C23 C24 -58.49(13) . . . . ?
C22 N40 C23 C24 165.71(10) . . . . ?
N46 N41 C23 N40 129.58(11) . . . . ?
C25 N41 C23 N40 -96.87(12) . . . . ?
N46 N41 C23 C24 -111.67(11) . . . . ?
C25 N41 C23 C24 21.88(12) . . . . ?
N48 N43 C24 N42 102.63(13) . . . . ?
C27 N43 C24 N42 -56.81(14) . . . . ?
N48 N43 C24 C23 -145.88(11) . . . . ?
C27 N43 C24 C23 54.69(14) . . . . ?
N47 N42 C24 N43 -53.16(15) . . . . ?
C25 N42 C24 N43 88.49(13) . . . . ?
N47 N42 C24 C23 -169.01(11) . . . . ?
C25 N42 C24 C23 -27.36(12) . . . . ?
N40 C23 C24 N43 3.90(14) . . . . ?
N41 C23 C24 N43 -116.26(11) . . . . ?
N40 C23 C24 N42 123.25(10) . . . . ?
N41 C23 C24 N42 3.09(12) . . . . ?
N46 N41 C25 N42 95.95(12) . . . . ?
C23 N41 C25 N42 -37.31(12) . . . . ?
N46 N41 C25 C26 -144.86(10) . . . . ?
C23 N41 C25 C26 81.88(12) . . . . ?
N47 N42 C25 N41 -176.95(10) . . . . ?
C24 N42 C25 N41 40.73(12) . . . . ?
N47 N42 C25 C26 67.91(14) . . . . ?
C24 N42 C25 C26 -74.40(13) . . . . ?
N50 N45 C26 N44 -110.52(12) . . . . ?
C28 N45 C26 N44 35.14(12) . . . . ?
N50 N45 C26 C25 134.89(11) . . . . ?
C28 N45 C26 C25 -79.44(12) . . . . ?
N49 N44 C26 N45 93.70(11) . . . . ?
C27 N44 C26 N45 -33.35(12) . . . . ?
N49 N44 C26 C25 -150.94(10) . . . . ?
C27 N44 C26 C25 82.01(11) . . . . ?
N41 C25 C26 N45 -1.80(13) . . . . ?
N42 C25 C26 N45 107.96(11) . . . . ?
N41 C25 C26 N44 -113.32(11) . . . . ?
N42 C25 C26 N44 -3.56(14) . . . . ?
N48 N43 C27 N44 -100.37(13) . . . . ?
C24 N43 C27 N44 59.07(14) . . . . ?
N48 N43 C27 C28 144.27(11) . . . . ?
C24 N43 C27 C28 -56.29(13) . . . . ?
N49 N44 C27 N43 136.35(11) . . . . ?
C26 N44 C27 N43 -96.97(12) . . . . ?
N49 N44 C27 C28 -106.84(11) . . . . ?
C26 N44 C27 C28 19.83(12) . . . . ?
C23 N40 C28 N45 -57.73(13) . . . . ?
C22 N40 C28 N45 78.35(13) . . . . ?
C23 N40 C28 C27 57.01(13) . . . . ?
C22 N40 C28 C27 -166.92(10) . . . . ?
N50 N45 C28 N40 -116.50(12) . . . . ?
C26 N45 C28 N40 96.96(12) . . . . ?
N50 N45 C28 C27 124.13(11) . . . . ?
C26 N45 C28 C27 -22.41(12) . . . . ?
N43 C27 C28 N40 -0.69(13) . . . . ?
N44 C27 C28 N40 -119.52(11) . . . . ?
N43 C27 C28 N45 120.07(10) . . . . ?
N44 C27 C28 N45 1.24(12) . . . . ?

_refine_diff_density_max         0.462
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.074

####################################################################### 
# 
# 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_PVG2016
_database_code_depnum_ccdc_archive 'CCDC 2121216'
loop_
_audit_author_name
_audit_author_address
'Darina Ildarovna Nasyrova'
;N D Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences
Russia
;
_audit_update_record             
;
2021-11-09 deposited with the CCDC.	2021-12-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_PVG2016             
;
PROBLEM: Short Inter D...A Contact  O1       ..O28D     .       2.64 Ang.  
RESPONSE: These particular short contacts were expected from
 the chemical structure.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H15 N15 O14'
_chemical_formula_sum            'C10 H15 N15 O14'
_chemical_formula_weight         569.37

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   14.18150(10)
_cell_length_b                   13.83480(10)
_cell_length_c                   21.5145(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.9580(10)
_cell_angle_gamma                90
_cell_volume                     4211.04(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    36656
_cell_measurement_theta_min      3.1110
_cell_measurement_theta_max      79.1660

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_F_000             2336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    1.474
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75797
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            59336
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.124
_diffrn_reflns_theta_max         78.485
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9011
_reflns_number_gt                8476
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0747P)²+3.8374P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9011
_refine_ls_number_parameters     799
_refine_ls_number_restraints     71
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.1403
_refine_ls_wR_factor_gt          0.1384
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.96634(10) 0.75780(10) 0.64077(7) 0.0309(3) Uani 1 1 d . . . . .
C1 C 0.86578(12) 0.55487(12) 0.56168(8) 0.0181(3) Uani 1 1 d . . . . .
H1 H 0.919455 0.507961 0.561963 0.022 Uiso 1 1 calc R U . . .
N1 N 0.89845(10) 0.65383(11) 0.57340(7) 0.0182(3) Uani 1 1 d . . . . .
O2 O 0.97877(9) 0.60218(10) 0.65890(6) 0.0260(3) Uani 1 1 d . . . . .
C2 C 0.78871(12) 0.52321(12) 0.60741(8) 0.0177(3) Uani 1 1 d . . . . .
H2 H 0.806450 0.461956 0.629959 0.021 Uiso 1 1 calc R U . . .
N2 N 0.77273(10) 0.60244(10) 0.65023(6) 0.0171(3) Uani 1 1 d . . . . .
O3 O 0.71280(10) 0.63241(10) 0.74193(6) 0.0296(3) Uani 1 1 d . . . . .
C3 C 0.82720(11) 0.72438(12) 0.54910(7) 0.0177(3) Uani 1 1 d . . . . .
H3 H 0.857689 0.783356 0.532598 0.021 Uiso 1 1 calc R U . . .
N3 N 0.81960(10) 0.56706(10) 0.49959(6) 0.0180(3) Uani 1 1 d . . . . .
C4 C 0.77509(11) 0.66456(12) 0.49542(8) 0.0171(3) Uani 1 1 d . . . . .
H4 H 0.785278 0.694709 0.454174 0.020 Uiso 1 1 calc R U . . .
N4 N 0.69579(10) 0.51725(10) 0.57499(6) 0.0164(3) Uani 1 1 d . . . . .
O4 O 0.79023(11) 0.49896(11) 0.73013(6) 0.0325(3) Uani 1 1 d . . . . .
O5 O 0.84815(10) 0.57420(11) 0.39869(6) 0.0274(3) Uani 1 1 d . . . . .
C5 C 0.70571(11) 0.67129(12) 0.61839(7) 0.0163(3) Uani 1 1 d . . . . .
H5 H 0.659067 0.695896 0.647403 0.020 Uiso 1 1 calc R U . . .
N5 N 0.75798(10) 0.74957(10) 0.59286(6) 0.0177(3) Uani 1 1 d . . . . .
O6 O 0.92101(9) 0.46605(11) 0.45812(6) 0.0292(3) Uani 1 1 d . . . . .
C6 C 0.65483(11) 0.61439(11) 0.56217(7) 0.0158(3) Uani 1 1 d . . . . .
H6 H 0.584997 0.613195 0.566124 0.019 Uiso 1 1 calc R U . . .
N6 N 0.67586(10) 0.65835(10) 0.50420(6) 0.0164(3) Uani 1 1 d . . . . .
O7 O 0.59646(9) 0.44185(9) 0.50858(6) 0.0207(3) Uani 1 1 d . . . . .
C7 C 0.61592(12) 0.63294(12) 0.44849(8) 0.0177(3) Uani 1 1 d . . . . .
H7A H 0.643711 0.577465 0.427161 0.021 Uiso 1 1 calc R U . . .
H7B H 0.552371 0.613886 0.460475 0.021 Uiso 1 1 calc R U . . .
N7 N 0.95101(10) 0.67228(12) 0.62841(7) 0.0222(3) Uani 1 1 d . . . . .
O8 O 0.72655(10) 0.36955(9) 0.54465(6) 0.0250(3) Uani 1 1 d . . . . .
C8 C 0.64394(13) 0.71454(14) 0.34433(8) 0.0241(4) Uani 1 1 d . . . . .
H8A H 0.701029 0.673234 0.345327 0.029 Uiso 1 1 calc R U . . .
H8B H 0.663187 0.780962 0.333683 0.029 Uiso 1 1 calc R U . . .
N8 N 0.75523(11) 0.57490(11) 0.71174(7) 0.0224(3) Uani 1 1 d . . . . .
C9 C 0.57291(13) 0.67774(14) 0.29303(8) 0.0239(4) Uani 1 1 d . . . . .
H9A H 0.513895 0.715819 0.293763 0.029 Uiso 1 1 calc R U . . .
H9B H 0.599018 0.688016 0.252042 0.029 Uiso 1 1 calc R U . . .
N9 N 0.86862(10) 0.53501(12) 0.44844(7) 0.0220(3) Uani 1 1 d . . . . .
O9 O 0.81368(11) 0.89970(10) 0.60386(7) 0.0320(3) Uani 1 1 d . . . . .
N10 N 0.67164(10) 0.43870(10) 0.54026(7) 0.0180(3) Uani 1 1 d . . . . .
O10 O 0.73519(10) 0.83740(10) 0.67757(6) 0.0284(3) Uani 1 1 d . . . . .
C10 C 0.59020(15) 0.49994(16) 0.26150(10) 0.0319(4) Uani 1 1 d . . . . .
H10A H 0.542484 0.480052 0.228884 0.048 Uiso 1 1 calc R U . . .
H10B H 0.608670 0.444118 0.287616 0.048 Uiso 1 1 calc R U . . .
H10C H 0.645768 0.525262 0.242238 0.048 Uiso 1 1 calc R U . . .
N11 N 0.77065(11) 0.83451(11) 0.62766(7) 0.0213(3) Uani 1 1 d . . . . .
O11 O 0.53127(11) 0.85093(10) 0.38089(7) 0.0334(3) Uani 1 1 d . . . . .
C11 C 0.36404(13) 0.55809(12) 0.07796(8) 0.0207(3) Uani 1 1 d D . . . .
H11A H 0.419336 0.513290 0.083361 0.025 Uiso 0.734(4) 1 calc R U P A 1
H11B H 0.419763 0.514759 0.086928 0.025 Uiso 0.266(4) 1 calc R U P A 2
N12 N 0.60809(10) 0.71561(10) 0.40666(7) 0.0190(3) Uani 1 1 d . . . . .
O12 O 0.49988(10) 0.77439(10) 0.46620(6) 0.0269(3) Uani 1 1 d . . . . .
C12 C 0.27823(13) 0.52820(12) 0.11827(9) 0.0223(4) Uani 1 1 d D . . . .
H12A H 0.293146 0.469282 0.144025 0.027 Uiso 0.828(9) 1 calc R U P B 1
H12B H 0.288465 0.466340 0.141818 0.027 Uiso 0.172(9) 1 calc R U P B 2
N13 N 0.54226(11) 0.78365(11) 0.41862(7) 0.0231(3) Uani 1 1 d . . . . .
O13 O 0.43400(10) 0.61684(10) 0.35811(6) 0.0274(3) Uani 1 1 d . . . . .
C13 C 0.32404(12) 0.72388(12) 0.05660(7) 0.0171(3) Uani 1 1 d . . . . .
H13 H 0.358614 0.780797 0.040744 0.021 Uiso 1 1 calc R U . . .
N14 N 0.55083(11) 0.57532(12) 0.30003(7) 0.0239(3) Uani 1 1 d . . . . .
O14 O 0.44770(10) 0.46669(10) 0.32781(6) 0.0290(3) Uani 1 1 d . . . . .
C14 C 0.28035(13) 0.65938(12) 0.00190(8) 0.0207(3) Uani 1 1 d D . . . .
H14A H 0.297468 0.684862 -0.039338 0.025 Uiso 0.734(4) 1 calc R U P A 1
H14B H 0.293189 0.692256 -0.038043 0.025 Uiso 0.266(4) 1 calc R U P A 2
N16 N 0.38779(10) 0.65798(10) 0.09215(7) 0.0193(3) Uani 1 1 d . . . . .
O16 O 0.53166(10) 0.62342(11) 0.13305(7) 0.0343(3) Uani 1 1 d . . . . .
C16 C 0.14929(13) 0.61478(14) 0.06188(9) 0.0251(4) Uani 1 1 d D . . . .
H16 H 0.078696 0.613474 0.060789 0.030 Uiso 1 1 calc R U . B 1
N15 N 0.47342(11) 0.55201(12) 0.32982(7) 0.0234(3) Uani 1 1 d . . . . .
O15 O 0.49168(10) 0.77369(10) 0.11500(7) 0.0315(3) Uani 1 1 d . . . . .
C15 C 0.18992(12) 0.67825(13) 0.11767(8) 0.0213(3) Uani 1 1 d . . . . .
H15 H 0.138071 0.706023 0.141365 0.026 Uiso 1 1 calc R U . . .
O18 O 0.37462(9) 0.58841(10) 0.21830(6) 0.0260(3) Uani 1 1 d . . . . .
C18 C 0.15962(16) 0.7067(2) -0.15691(10) 0.0402(5) Uani 1 1 d D . . . .
H18A H 0.214376 0.662202 -0.154931 0.048 Uiso 0.824(2) 1 calc R U P C 1
H18B H 0.182957 0.771827 -0.167268 0.048 Uiso 0.824(2) 1 calc R U P C 1
H18C H 0.197832 0.647013 -0.158407 0.048 Uiso 0.0616(18) 1 calc R U P C 2
H18D H 0.203815 0.761766 -0.159468 0.048 Uiso 0.0616(18) 1 calc R U P C 2
H18E H 0.224670 0.680388 -0.153655 0.048 Uiso 0.0583(17) 1 calc R U P C 3
H18F H 0.161177 0.772256 -0.175326 0.048 Uiso 0.0583(17) 1 calc R U P C 3
H18G H 0.222012 0.674355 -0.154241 0.048 Uiso 0.056(2) 1 calc R U P C 4
H18H H 0.167372 0.772877 -0.173380 0.048 Uiso 0.056(2) 1 calc R U P C 4
N17 N 0.24677(10) 0.60806(11) 0.15584(7) 0.0210(3) Uani 1 1 d . . . . .
O17 O 0.28723(11) 0.71779(10) 0.22740(6) 0.0320(3) Uani 1 1 d . . . . .
C17 C 0.12449(14) 0.62819(13) -0.05324(9) 0.0249(4) Uani 1 1 d . . . . .
H17A H 0.153683 0.572147 -0.073128 0.030 Uiso 1 1 calc R U . . .
H17B H 0.059410 0.610088 -0.043927 0.030 Uiso 1 1 calc R U . . .
N20 N 0.24731(10) 0.75335(10) 0.09333(7) 0.0183(3) Uani 1 1 d . . . . .
N21 N 0.17944(11) 0.65324(11) 0.00441(7) 0.0237(3) Uani 1 1 d . . . . .
N22 N 0.47731(11) 0.68617(12) 0.11396(7) 0.0234(3) Uani 1 1 d . . . . .
N23 N 0.30697(11) 0.64031(11) 0.20333(7) 0.0230(3) Uani 1 1 d . . . . .
O23 O 0.30383(11) 0.90329(10) 0.10125(7) 0.0304(3) Uani 1 1 d . . . . .
O20A O 0.4261(2) 0.4556(2) -0.01761(11) 0.0610(10) Uani 0.734(4) 1 d D . P A 1
N24A N 0.3713(2) 0.5208(2) -0.03333(11) 0.0286(8) Uani 0.734(4) 1 d D . P A 1
O19A O 0.35012(18) 0.54795(19) -0.08647(10) 0.0265(5) Uani 0.734(4) 1 d D . P A
1
N18A N 0.32131(17) 0.56135(13) 0.01378(8) 0.0168(5) Uani 0.734(4) 1 d D . P A 1
O20B O 0.3669(7) 0.4223(6) -0.0079(3) 0.0610(10) Uani 0.266(4) 1 d D . P A 2
N24B N 0.3497(9) 0.5016(4) -0.0310(3) 0.0286(8) Uani 0.266(4) 1 d D . P A 2
O19B O 0.3249(6) 0.5217(6) -0.0848(3) 0.0265(5) Uani 0.266(4) 1 d D . P A 2
N18B N 0.3489(4) 0.5780(4) 0.01097(14) 0.0168(5) Uani 0.266(4) 1 d D . P A 2
O24 O 0.18242(11) 0.86411(11) 0.15232(7) 0.0338(3) Uani 1 1 d . . . . .
N19 N 0.18835(17) 0.51943(12) 0.08234(14) 0.0219(6) Uani 0.828(9) 1 d D . P B 1
N25 N 0.1680(3) 0.43823(17) 0.04824(17) 0.0209(6) Uani 0.828(9) 1 d D . P B 1
O21 O 0.0950(4) 0.4369(6) 0.0135(3) 0.0253(6) Uani 0.828(9) 1 d D . P B 1
O22 O 0.22407(18) 0.37150(18) 0.05788(15) 0.0300(6) Uani 0.828(9) 1 d D . P B 1
N19A N 0.2044(7) 0.5231(4) 0.0681(5) 0.0219(6) Uani 0.172(9) 1 d D . P B 2
N25A N 0.1720(16) 0.4310(5) 0.0599(12) 0.0209(6) Uani 0.172(9) 1 d D . P B 2
O21A O 0.107(2) 0.442(3) 0.0190(17) 0.0253(6) Uani 0.172(9) 1 d D . P B 2
O22A O 0.2036(9) 0.3529(8) 0.0784(7) 0.0300(6) Uani 0.172(9) 1 d D . P B 2
N28 N 0.0609(2) 0.78346(18) -0.08452(13) 0.0258(5) Uani 0.879(9) 1 d D . P D 1
O25 O 0.05595(15) 0.85052(14) -0.12258(18) 0.0381(7) Uani 0.879(9) 1 d D . P D
1
O26 O 0.01711(15) 0.77805(19) -0.03745(14) 0.0303(5) Uani 0.879(9) 1 d D . P D
1
N28A N 0.0651(19) 0.7772(12) -0.0702(10) 0.0258(5) Uani 0.121(9) 1 d D . P D 2
O25A O 0.0495(12) 0.8577(10) -0.0938(13) 0.0381(7) Uani 0.121(9) 1 d D . P D 2
O26A O 0.0301(13) 0.7583(15) -0.0210(7) 0.0303(5) Uani 0.121(9) 1 d D . P D 2
N26 N 0.24499(12) 0.84611(11) 0.11797(7) 0.0232(3) Uani 1 1 d . . . . .
N27 N 0.12167(11) 0.71059(12) -0.09540(7) 0.0245(3) Uani 1 1 d D . . . .
C19A C 0.0880(2) 0.6734(2) -0.20974(11) 0.0307(7) Uani 0.824(2) 1 d D . P C 1
H19A H 0.030085 0.713106 -0.208797 0.037 Uiso 0.824(2) 1 calc R U P C 1
H19B H 0.115279 0.684783 -0.250239 0.037 Uiso 0.824(2) 1 calc R U P C 1
N29A N 0.06189(16) 0.56981(18) -0.20541(10) 0.0337(5) Uani 0.824(2) 1 d D . P C
1
N30A N -0.01551(15) 0.54705(17) -0.17424(10) 0.0320(5) Uani 0.824(2) 1 d D . P
C 1
O28A O -0.03816(15) 0.46193(17) -0.17385(11) 0.0411(5) Uani 0.824(2) 1 d D . P
C 1
O27A O -0.05687(15) 0.61349(18) -0.14932(10) 0.0405(5) Uani 0.824(2) 1 d D . P
C 1
C20A C 0.1028(2) 0.4924(2) -0.24112(14) 0.0441(7) Uani 0.824(2) 1 d D . P C 1
H20A H 0.057016 0.471918 -0.274751 0.066 Uiso 0.824(2) 1 calc R U P C 1
H20B H 0.118563 0.437440 -0.213612 0.066 Uiso 0.824(2) 1 calc R U P C 1
H20C H 0.160246 0.515955 -0.258965 0.066 Uiso 0.824(2) 1 calc R U P C 1
C19B C 0.0926(12) 0.709(3) -0.2165(6) 0.0307(7) Uani 0.0616(18) 1 d D . P C 2
H19C H 0.107855 0.765398 -0.242078 0.037 Uiso 0.0616(18) 1 calc R U P C 2
H19D H 0.102297 0.649783 -0.241228 0.037 Uiso 0.0616(18) 1 calc R U P C 2
N29B N -0.0079(15) 0.7143(16) -0.2014(13) 0.0337(5) Uani 0.0616(18) 1 d D . P C
2
N30B N -0.0599(12) 0.7917(13) -0.2229(13) 0.0320(5) Uani 0.0616(18) 1 d D . P C
2
O28B O -0.1361(13) 0.7503(17) -0.2268(14) 0.0411(5) Uani 0.0616(18) 1 d D . P C
2
O27B O -0.0647(18) 0.8786(12) -0.2360(12) 0.0405(5) Uani 0.0616(18) 1 d D . P C
2
C20B C -0.052(2) 0.631(2) -0.174(2) 0.0441(7) Uani 0.0616(18) 1 d D . P C 2
H20D H -0.003914 0.582651 -0.161584 0.066 Uiso 0.0616(18) 1 calc R U P C 2
H20E H -0.085102 0.650917 -0.137790 0.066 Uiso 0.0616(18) 1 calc R U P C 2
H20F H -0.098070 0.601854 -0.205199 0.066 Uiso 0.0616(18) 1 calc R U P C 2
C19C C 0.0934(14) 0.6403(16) -0.1976(16) 0.0307(7) Uani 0.0583(17) 1 d D . P C
3
H19E H 0.120220 0.627342 -0.238025 0.037 Uiso 0.0583(17) 1 calc R U P C 3
H19F H 0.084227 0.577942 -0.176228 0.037 Uiso 0.0583(17) 1 calc R U P C 3
N29C N 0.0024(15) 0.693(2) -0.2070(13) 0.0337(5) Uani 0.0583(17) 1 d D . P C 3
N30C N -0.0818(12) 0.7118(15) -0.1824(12) 0.0320(5) Uani 0.0583(17) 1 d D . P C
3
O27C O -0.1380(17) 0.6502(16) -0.1661(12) 0.0405(5) Uani 0.0583(17) 1 d D . P C
3
O28C O -0.1281(17) 0.7817(16) -0.2011(14) 0.0411(5) Uani 0.0583(17) 1 d D . P C
3
C20C C 0.014(2) 0.772(3) -0.2508(17) 0.0441(7) Uani 0.0583(17) 1 d D . P C 3
H20G H 0.073783 0.764117 -0.270657 0.066 Uiso 0.0583(17) 1 calc R U P C 3
H20H H -0.038560 0.772280 -0.282689 0.066 Uiso 0.0583(17) 1 calc R U P C 3
H20I H 0.015274 0.834040 -0.228253 0.066 Uiso 0.0583(17) 1 calc R U P C 3
C19D C 0.088(3) 0.649(3) -0.1999(14) 0.0307(7) Uani 0.056(2) 1 d D . P C 4
H19G H 0.043050 0.699226 -0.215855 0.037 Uiso 0.056(2) 1 calc R U P C 4
H19H H 0.125306 0.632098 -0.235693 0.037 Uiso 0.056(2) 1 calc R U P C 4
N29D N 0.028(3) 0.5629(16) -0.1927(13) 0.0337(5) Uani 0.056(2) 1 d D . P C 4
N30D N 0.0192(19) 0.4690(16) -0.2115(11) 0.0320(5) Uani 0.056(2) 1 d D . P C 4
O28D O -0.038(2) 0.422(2) -0.1854(16) 0.0411(5) Uani 0.056(2) 1 d D . P C 4
O27D O 0.057(2) 0.425(2) -0.2533(12) 0.0405(5) Uani 0.056(2) 1 d D . P C 4
C20D C -0.021(3) 0.569(3) -0.1351(16) 0.0441(7) Uani 0.056(2) 1 d D . P C 4
H20K H -0.017460 0.635403 -0.119246 0.066 Uiso 0.056(2) 1 calc R U P C 4
H20L H -0.087485 0.550689 -0.143528 0.066 Uiso 0.056(2) 1 calc R U P C 4
H20M H 0.009067 0.525077 -0.104056 0.066 Uiso 0.056(2) 1 calc R U P C 4


_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(2) . ?
C1 N3 1.456(2) . ?
C1 N1 1.462(2) . ?
C1 C2 1.582(2) . ?
C1 H1 1.0000 . ?
N1 N7 1.378(2) . ?
N1 C3 1.475(2) . ?
O2 N7 1.221(2) . ?
C2 N4 1.450(2) . ?
C2 N2 1.460(2) . ?
C2 H2 1.0000 . ?
N2 N8 1.4154(19) . ?
N2 C5 1.480(2) . ?
O3 N8 1.213(2) . ?
C3 N5 1.449(2) . ?
C3 C4 1.564(2) . ?
C3 H3 1.0000 . ?
N3 N9 1.4131(19) . ?
N3 C4 1.489(2) . ?
C4 N6 1.435(2) . ?
C4 H4 1.0000 . ?
N4 N10 1.3495(19) . ?
N4 C6 1.482(2) . ?
O4 N8 1.216(2) . ?
O5 N9 1.217(2) . ?
C5 N5 1.442(2) . ?
C5 C6 1.576(2) . ?
C5 H5 1.0000 . ?
N5 N11 1.3983(19) . ?
O6 N9 1.218(2) . ?
C6 N6 1.437(2) . ?
C6 H6 1.0000 . ?
N6 C7 1.463(2) . ?
O7 N10 1.2259(19) . ?
C7 N12 1.455(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
O8 N10 1.2330(19) . ?
C8 N12 1.467(2) . ?
C8 C9 1.529(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 N14 1.461(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
O9 N11 1.221(2) . ?
O10 N11 1.217(2) . ?
C10 N14 1.467(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
O11 N13 1.238(2) . ?
C11 N16 1.450(2) . ?
C11 N18B 1.468(3) . ?
C11 N18A 1.470(2) . ?
C11 C12 1.597(3) . ?
C11 H11A 1.0000 . ?
C11 H11B 1.0000 . ?
N12 N13 1.363(2) . ?
O12 N13 1.229(2) . ?
C12 N19 1.449(2) . ?
C12 N19A 1.453(4) . ?
C12 N17 1.457(2) . ?
C12 H12A 1.0000 . ?
C12 H12B 1.0000 . ?
O13 N15 1.239(2) . ?
C13 N20 1.447(2) . ?
C13 N16 1.462(2) . ?
C13 C14 1.570(2) . ?
C13 H13 1.0000 . ?
N14 N15 1.348(2) . ?
O14 N15 1.235(2) . ?
C14 N21 1.438(2) . ?
C14 N18A 1.491(2) . ?
C14 N18B 1.492(3) . ?
C14 H14A 1.0000 . ?
C14 H14B 1.0000 . ?
N16 N22 1.379(2) . ?
O16 N22 1.214(2) . ?
C16 N21 1.438(2) . ?
C16 N19 1.486(2) . ?
C16 N19A 1.491(4) . ?
C16 C15 1.565(3) . ?
C16 H16 1.0000 . ?
O15 N22 1.228(2) . ?
C15 N20 1.440(2) . ?
C15 N17 1.475(2) . ?
C15 H15 1.0000 . ?
O18 N23 1.224(2) . ?
C18 N27 1.464(3) . ?
C18 C19A 1.542(3) . ?
C18 C19C 1.542(4) . ?
C18 C19B 1.542(4) . ?
C18 C19D 1.543(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 H18C 0.9900 . ?
C18 H18D 0.9900 . ?
C18 H18E 0.9900 . ?
C18 H18F 0.9900 . ?
C18 H18G 0.9900 . ?
C18 H18H 0.9900 . ?
N17 N23 1.361(2) . ?
O17 N23 1.231(2) . ?
C17 N27 1.456(2) . ?
C17 N21 1.460(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
N20 N26 1.390(2) . ?
O23 N26 1.222(2) . ?
O20A N24A 1.223(3) . ?
N24A O19A 1.221(3) . ?
N24A N18A 1.394(3) . ?
O20B N24B 1.222(4) . ?
N24B O19B 1.219(3) . ?
N24B N18B 1.391(4) . ?
O24 N26 1.219(2) . ?
N19 N25 1.362(3) . ?
N25 O22 1.227(3) . ?
N25 O21 1.234(3) . ?
N19A N25A 1.362(4) . ?
N25A O22A 1.227(4) . ?
N25A O21A 1.234(4) . ?
N28 O26 1.227(3) . ?
N28 O25 1.236(2) . ?
N28 N27 1.357(2) . ?
N28A O26A 1.228(4) . ?
N28A O25A 1.238(4) . ?
N28A N27 1.359(4) . ?
C19A N29A 1.484(4) . ?
C19A H19A 0.9900 . ?
C19A H19B 0.9900 . ?
N29A N30A 1.362(3) . ?
N29A C20A 1.461(4) . ?
N30A O28A 1.221(3) . ?
N30A O27A 1.233(3) . ?
C20A H20A 0.9800 . ?
C20A H20B 0.9800 . ?
C20A H20C 0.9800 . ?
C19B N29B 1.485(5) . ?
C19B H19C 0.9900 . ?
C19B H19D 0.9900 . ?
N29B N30B 1.363(4) . ?
N29B C20B 1.461(5) . ?
N30B O28B 1.222(4) . ?
N30B O27B 1.235(4) . ?
C20B H20D 0.9800 . ?
C20B H20E 0.9800 . ?
C20B H20F 0.9800 . ?
C19C N29C 1.485(5) . ?
C19C H19E 0.9900 . ?
C19C H19F 0.9900 . ?
N29C N30C 1.364(4) . ?
N29C C20C 1.463(5) . ?
N30C O28C 1.222(4) . ?
N30C O27C 1.234(4) . ?
C20C H20G 0.9800 . ?
C20C H20H 0.9800 . ?
C20C H20I 0.9800 . ?
C19D N29D 1.486(5) . ?
C19D H19G 0.9900 . ?
C19D H19H 0.9900 . ?
N29D N30D 1.364(4) . ?
N29D C20D 1.462(5) . ?
N30D O28D 1.21(4) . ?
N30D O27D 1.235(4) . ?
C20D H20K 0.9800 . ?
C20D H20L 0.9800 . ?
C20D H20M 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
N3 C1 N1 99.61(13) . . ?
N3 C1 C2 108.43(13) . . ?
N1 C1 C2 112.11(13) . . ?
N3 C1 H1 112.0 . . ?
N1 C1 H1 112.0 . . ?
C2 C1 H1 112.0 . . ?
N7 N1 C1 117.89(14) . . ?
N7 N1 C3 119.91(14) . . ?
C1 N1 C3 110.94(13) . . ?
N4 C2 N2 99.82(13) . . ?
N4 C2 C1 111.13(13) . . ?
N2 C2 C1 109.19(13) . . ?
N4 C2 H2 112.0 . . ?
N2 C2 H2 112.0 . . ?
C1 C2 H2 112.0 . . ?
N8 N2 C2 115.65(13) . . ?
N8 N2 C5 117.24(13) . . ?
C2 N2 C5 108.30(13) . . ?
N5 C3 N1 114.03(13) . . ?
N5 C3 C4 107.48(13) . . ?
N1 C3 C4 100.89(13) . . ?
N5 C3 H3 111.3 . . ?
N1 C3 H3 111.3 . . ?
C4 C3 H3 111.3 . . ?
N9 N3 C1 117.63(13) . . ?
N9 N3 C4 117.81(13) . . ?
C1 N3 C4 108.79(13) . . ?
N6 C4 N3 110.68(13) . . ?
N6 C4 C3 110.61(13) . . ?
N3 C4 C3 104.96(13) . . ?
N6 C4 H4 110.2 . . ?
N3 C4 H4 110.2 . . ?
C3 C4 H4 110.2 . . ?
N10 N4 C2 119.96(13) . . ?
N10 N4 C6 123.09(13) . . ?
C2 N4 C6 111.67(13) . . ?
N5 C5 N2 109.21(13) . . ?
N5 C5 C6 107.63(13) . . ?
N2 C5 C6 106.21(13) . . ?
N5 C5 H5 111.2 . . ?
N2 C5 H5 111.2 . . ?
C6 C5 H5 111.2 . . ?
N11 N5 C5 118.52(13) . . ?
N11 N5 C3 118.84(13) . . ?
C5 N5 C3 117.13(13) . . ?
N6 C6 N4 116.29(13) . . ?
N6 C6 C5 110.08(13) . . ?
N4 C6 C5 99.06(12) . . ?
N6 C6 H6 110.3 . . ?
N4 C6 H6 110.3 . . ?
C5 C6 H6 110.3 . . ?
C4 N6 C6 113.80(13) . . ?
C4 N6 C7 115.22(13) . . ?
C6 N6 C7 117.74(13) . . ?
N12 C7 N6 109.45(13) . . ?
N12 C7 H7A 109.8 . . ?
N6 C7 H7A 109.8 . . ?
N12 C7 H7B 109.8 . . ?
N6 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
O2 N7 O1 127.08(15) . . ?
O2 N7 N1 116.71(15) . . ?
O1 N7 N1 116.19(15) . . ?
N12 C8 C9 114.24(15) . . ?
N12 C8 H8A 108.7 . . ?
C9 C8 H8A 108.7 . . ?
N12 C8 H8B 108.7 . . ?
C9 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
O3 N8 O4 126.78(15) . . ?
O3 N8 N2 116.71(15) . . ?
O4 N8 N2 116.28(15) . . ?
N14 C9 C8 112.56(15) . . ?
N14 C9 H9A 109.1 . . ?
C8 C9 H9A 109.1 . . ?
N14 C9 H9B 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
O5 N9 O6 127.22(15) . . ?
O5 N9 N3 116.42(15) . . ?
O6 N9 N3 116.08(15) . . ?
O7 N10 O8 126.20(15) . . ?
O7 N10 N4 117.19(14) . . ?
O8 N10 N4 116.59(14) . . ?
N14 C10 H10A 109.5 . . ?
N14 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N14 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O10 N11 O9 126.47(15) . . ?
O10 N11 N5 117.02(14) . . ?
O9 N11 N5 116.46(15) . . ?
N16 C11 N18B 92.5(3) . . ?
N16 C11 N18A 104.08(14) . . ?
N16 C11 C12 107.88(14) . . ?
N18B C11 C12 121.1(3) . . ?
N18A C11 C12 103.77(16) . . ?
N16 C11 H11A 113.4 . . ?
N18A C11 H11A 113.4 . . ?
C12 C11 H11A 113.4 . . ?
N16 C11 H11B 111.2 . . ?
N18B C11 H11B 111.2 . . ?
C12 C11 H11B 111.2 . . ?
N13 N12 C7 116.76(14) . . ?
N13 N12 C8 117.70(14) . . ?
C7 N12 C8 122.76(14) . . ?
N19 C12 N17 93.89(16) . . ?
N19A C12 N17 102.5(3) . . ?
N19 C12 C11 114.02(19) . . ?
N19A C12 C11 98.4(6) . . ?
N17 C12 C11 112.27(14) . . ?
N19 C12 H12A 111.8 . . ?
N17 C12 H12A 111.8 . . ?
C11 C12 H12A 111.8 . . ?
N19A C12 H12B 114.0 . . ?
N17 C12 H12B 114.0 . . ?
C11 C12 H12B 114.0 . . ?
O12 N13 O11 125.31(16) . . ?
O12 N13 N12 117.77(14) . . ?
O11 N13 N12 116.90(16) . . ?
N20 C13 N16 110.55(13) . . ?
N20 C13 C14 107.27(13) . . ?
N16 C13 C14 103.63(13) . . ?
N20 C13 H13 111.7 . . ?
N16 C13 H13 111.7 . . ?
C14 C13 H13 111.7 . . ?
N15 N14 C9 117.93(16) . . ?
N15 N14 C10 116.93(16) . . ?
C9 N14 C10 122.60(15) . . ?
N21 C14 N18A 108.47(16) . . ?
N21 C14 N18B 126.3(3) . . ?
N21 C14 C13 110.34(14) . . ?
N18A C14 C13 105.04(14) . . ?
N18B C14 C13 96.4(2) . . ?
N21 C14 H14A 110.9 . . ?
N18A C14 H14A 110.9 . . ?
C13 C14 H14A 110.9 . . ?
N21 C14 H14B 107.4 . . ?
N18B C14 H14B 107.4 . . ?
C13 C14 H14B 107.4 . . ?
N22 N16 C11 122.43(14) . . ?
N22 N16 C13 121.54(14) . . ?
C11 N16 C13 110.97(13) . . ?
N21 C16 N19 117.2(2) . . ?
N21 C16 N19A 101.9(6) . . ?
N21 C16 C15 109.65(14) . . ?
N19 C16 C15 99.27(15) . . ?
N19A C16 C15 104.22(19) . . ?
N21 C16 H16 110.1 . . ?
N19 C16 H16 110.1 . . ?
C15 C16 H16 110.1 . . ?
O14 N15 O13 124.53(16) . . ?
O14 N15 N14 117.40(16) . . ?
O13 N15 N14 118.05(15) . . ?
N20 C15 N17 112.11(14) . . ?
N20 C15 C16 108.26(14) . . ?
N17 C15 C16 102.47(14) . . ?
N20 C15 H15 111.2 . . ?
N17 C15 H15 111.2 . . ?
C16 C15 H15 111.2 . . ?
N27 C18 C19A 114.39(18) . . ?
N27 C18 C19C 106.7(15) . . ?
N27 C18 C19B 120.4(8) . . ?
N27 C18 C19D 107.1(17) . . ?
N27 C18 H18A 108.7 . . ?
C19A C18 H18A 108.7 . . ?
N27 C18 H18B 108.7 . . ?
C19A C18 H18B 108.7 . . ?
H18A C18 H18B 107.6 . . ?
N27 C18 H18C 107.2 . . ?
C19B C18 H18C 107.2 . . ?
N27 C18 H18D 107.2 . . ?
C19B C18 H18D 107.2 . . ?
H18C C18 H18D 106.9 . . ?
N27 C18 H18E 110.4 . . ?
C19C C18 H18E 110.4 . . ?
N27 C18 H18F 110.4 . . ?
C19C C18 H18F 110.4 . . ?
H18E C18 H18F 108.6 . . ?
N27 C18 H18G 110.3 . . ?
C19D C18 H18G 110.3 . . ?
N27 C18 H18H 110.3 . . ?
C19D C18 H18H 110.3 . . ?
H18G C18 H18H 108.5 . . ?
N23 N17 C12 117.71(14) . . ?
N23 N17 C15 119.52(15) . . ?
C12 N17 C15 111.51(14) . . ?
N27 C17 N21 109.47(14) . . ?
N27 C17 H17A 109.8 . . ?
N21 C17 H17A 109.8 . . ?
N27 C17 H17B 109.8 . . ?
N21 C17 H17B 109.8 . . ?
H17A C17 H17B 108.2 . . ?
N26 N20 C15 119.90(14) . . ?
N26 N20 C13 120.47(14) . . ?
C15 N20 C13 117.41(14) . . ?
C16 N21 C14 114.19(14) . . ?
C16 N21 C17 118.01(15) . . ?
C14 N21 C17 117.14(15) . . ?
O16 N22 O15 126.76(16) . . ?
O16 N22 N16 117.46(15) . . ?
O15 N22 N16 115.65(15) . . ?
O18 N23 O17 126.67(16) . . ?
O18 N23 N17 116.43(15) . . ?
O17 N23 N17 116.89(15) . . ?
O19A N24A O20A 126.6(3) . . ?
O19A N24A N18A 116.9(2) . . ?
O20A N24A N18A 116.2(2) . . ?
N24A N18A C11 118.3(2) . . ?
N24A N18A C14 116.9(2) . . ?
C11 N18A C14 108.64(14) . . ?
O19B N24B O20B 128.9(7) . . ?
O19B N24B N18B 115.4(6) . . ?
O20B N24B N18B 115.4(6) . . ?
N24B N18B C11 119.2(4) . . ?
N24B N18B C14 121.5(5) . . ?
C11 N18B C14 108.6(2) . . ?
N25 N19 C12 120.1(2) . . ?
N25 N19 C16 120.8(2) . . ?
C12 N19 C16 112.32(15) . . ?
O22 N25 O21 126.7(5) . . ?
O22 N25 N19 114.8(2) . . ?
O21 N25 N19 118.4(5) . . ?
N25A N19A C12 111.2(10) . . ?
N25A N19A C16 127.9(8) . . ?
C12 N19A C16 111.8(3) . . ?
O22A N25A O21A 125(2) . . ?
O22A N25A N19A 132.1(16) . . ?
O21A N25A N19A 102(2) . . ?
O26 N28 O25 125.7(2) . . ?
O26 N28 N27 117.45(18) . . ?
O25 N28 N27 116.8(2) . . ?
O26A N28A O25A 118.3(13) . . ?
O26A N28A N27 119.0(12) . . ?
O25A N28A N27 122.7(14) . . ?
O24 N26 O23 125.92(16) . . ?
O24 N26 N20 117.21(15) . . ?
O23 N26 N20 116.80(15) . . ?
N28 N27 C17 117.71(18) . . ?
N28A N27 C17 105.9(6) . . ?
N28 N27 C18 117.4(2) . . ?
N28A N27 C18 130.5(7) . . ?
C17 N27 C18 122.61(18) . . ?
N29A C19A C18 113.4(2) . . ?
N29A C19A H19A 108.9 . . ?
C18 C19A H19A 108.9 . . ?
N29A C19A H19B 108.9 . . ?
C18 C19A H19B 108.9 . . ?
H19A C19A H19B 107.7 . . ?
N30A N29A C20A 116.9(2) . . ?
N30A N29A C19A 117.8(2) . . ?
C20A N29A C19A 124.4(2) . . ?
O28A N30A O27A 125.7(2) . . ?
O28A N30A N29A 116.6(2) . . ?
O27A N30A N29A 117.7(2) . . ?
N29A C20A H20A 109.5 . . ?
N29A C20A H20B 109.5 . . ?
H20A C20A H20B 109.5 . . ?
N29A C20A H20C 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
N29B C19B C18 111.4(16) . . ?
N29B C19B H19C 109.3 . . ?
C18 C19B H19C 109.3 . . ?
N29B C19B H19D 109.3 . . ?
C18 C19B H19D 109.3 . . ?
H19C C19B H19D 108.0 . . ?
N30B N29B C20B 121.4(17) . . ?
N30B N29B C19B 118(2) . . ?
C20B N29B C19B 119.6(19) . . ?
O28B N30B O27B 114.0(18) . . ?
O28B N30B N29B 96.3(17) . . ?
O27B N30B N29B 150(2) . . ?
N29B C20B H20D 109.5 . . ?
N29B C20B H20E 109.5 . . ?
H20D C20B H20E 109.5 . . ?
N29B C20B H20F 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?
N29C C19C C18 105.9(17) . . ?
N29C C19C H19E 110.6 . . ?
C18 C19C H19E 110.6 . . ?
N29C C19C H19F 110.6 . . ?
C18 C19C H19F 110.6 . . ?
H19E C19C H19F 108.7 . . ?
N30C N29C C20C 104.5(16) . . ?
N30C N29C C19C 145(2) . . ?
C20C N29C C19C 108.7(18) . . ?
O28C N30C O27C 107.2(18) . . ?
O28C N30C N29C 119.2(19) . . ?
O27C N30C N29C 125(2) . . ?
N29C C20C H20G 109.5 . . ?
N29C C20C H20H 109.5 . . ?
H20G C20C H20H 109.5 . . ?
N29C C20C H20I 109.5 . . ?
H20G C20C H20I 109.5 . . ?
H20H C20C H20I 109.5 . . ?
N29D C19D C18 135(3) . . ?
N29D C19D H19G 103.3 . . ?
C18 C19D H19G 103.3 . . ?
N29D C19D H19H 103.3 . . ?
C18 C19D H19H 103.3 . . ?
H19G C19D H19H 105.2 . . ?
N30D N29D C20D 105.6(17) . . ?
N30D N29D C19D 141(3) . . ?
C20D N29D C19D 111(2) . . ?
O28D N30D O27D 114(2) . . ?
O28D N30D N29D 115(2) . . ?
O27D N30D N29D 131(3) . . ?
N29D C20D H20K 109.5 . . ?
N29D C20D H20L 109.5 . . ?
H20K C20D H20L 109.5 . . ?
N29D C20D H20M 109.5 . . ?
H20K C20D H20M 109.5 . . ?
H20L C20D H20M 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
N3 C1 N1 N7 -177.20(13) . . . . ?
C2 C1 N1 N7 68.28(18) . . . . ?
N3 C1 N1 C3 39.02(16) . . . . ?
C2 C1 N1 C3 -75.50(16) . . . . ?
N3 C1 C2 N4 -0.97(18) . . . . ?
N1 C1 C2 N4 108.01(15) . . . . ?
N3 C1 C2 N2 -110.13(15) . . . . ?
N1 C1 C2 N2 -1.15(18) . . . . ?
N4 C2 N2 N8 99.62(15) . . . . ?
C1 C2 N2 N8 -143.79(14) . . . . ?
N4 C2 N2 C5 -34.29(15) . . . . ?
C1 C2 N2 C5 82.30(15) . . . . ?
N7 N1 C3 N5 -54.90(19) . . . . ?
C1 N1 C3 N5 88.05(16) . . . . ?
N7 N1 C3 C4 -169.78(14) . . . . ?
C1 N1 C3 C4 -26.83(16) . . . . ?
N1 C1 N3 N9 102.14(15) . . . . ?
C2 C1 N3 N9 -140.54(14) . . . . ?
N1 C1 N3 C4 -35.10(15) . . . . ?
C2 C1 N3 C4 82.22(15) . . . . ?
N9 N3 C4 N6 123.65(15) . . . . ?
C1 N3 C4 N6 -99.20(15) . . . . ?
N9 N3 C4 C3 -117.00(15) . . . . ?
C1 N3 C4 C3 20.16(16) . . . . ?
N5 C3 C4 N6 3.37(18) . . . . ?
N1 C3 C4 N6 123.06(14) . . . . ?
N5 C3 C4 N3 -116.04(14) . . . . ?
N1 C3 C4 N3 3.66(15) . . . . ?
N2 C2 N4 N10 -164.97(13) . . . . ?
C1 C2 N4 N10 79.90(18) . . . . ?
N2 C2 N4 C6 39.91(16) . . . . ?
C1 C2 N4 C6 -75.21(16) . . . . ?
N8 N2 C5 N5 129.63(14) . . . . ?
C2 N2 C5 N5 -97.30(15) . . . . ?
N8 N2 C5 C6 -114.57(15) . . . . ?
C2 N2 C5 C6 18.51(16) . . . . ?
N2 C5 N5 N11 -95.63(16) . . . . ?
C6 C5 N5 N11 149.48(14) . . . . ?
N2 C5 N5 C3 57.92(18) . . . . ?
C6 C5 N5 C3 -56.97(17) . . . . ?
N1 C3 N5 N11 97.93(17) . . . . ?
C4 C3 N5 N11 -151.14(14) . . . . ?
N1 C3 N5 C5 -55.53(19) . . . . ?
C4 C3 N5 C5 55.40(18) . . . . ?
N10 N4 C6 N6 -64.6(2) . . . . ?
C2 N4 C6 N6 89.57(16) . . . . ?
N10 N4 C6 C5 177.55(14) . . . . ?
C2 N4 C6 C5 -28.24(16) . . . . ?
N5 C5 C6 N6 -0.39(18) . . . . ?
N2 C5 C6 N6 -117.26(14) . . . . ?
N5 C5 C6 N4 122.01(13) . . . . ?
N2 C5 C6 N4 5.14(15) . . . . ?
N3 C4 N6 C6 57.06(17) . . . . ?
C3 C4 N6 C6 -58.83(17) . . . . ?
N3 C4 N6 C7 -83.29(16) . . . . ?
C3 C4 N6 C7 160.81(13) . . . . ?
N4 C6 N6 C4 -54.61(18) . . . . ?
C5 C6 N6 C4 56.95(17) . . . . ?
N4 C6 N6 C7 84.68(18) . . . . ?
C5 C6 N6 C7 -163.76(13) . . . . ?
C4 N6 C7 N12 -73.89(17) . . . . ?
C6 N6 C7 N12 147.38(14) . . . . ?
C1 N1 N7 O2 11.0(2) . . . . ?
C3 N1 N7 O2 151.42(15) . . . . ?
C1 N1 N7 O1 -170.41(15) . . . . ?
C3 N1 N7 O1 -30.0(2) . . . . ?
C2 N2 N8 O3 -156.87(15) . . . . ?
C5 N2 N8 O3 -27.2(2) . . . . ?
C2 N2 N8 O4 28.2(2) . . . . ?
C5 N2 N8 O4 157.87(15) . . . . ?
N12 C8 C9 N14 -66.8(2) . . . . ?
C1 N3 N9 O5 -154.62(15) . . . . ?
C4 N3 N9 O5 -21.2(2) . . . . ?
C1 N3 N9 O6 31.1(2) . . . . ?
C4 N3 N9 O6 164.45(14) . . . . ?
C2 N4 N10 O7 -172.35(14) . . . . ?
C6 N4 N10 O7 -20.2(2) . . . . ?
C2 N4 N10 O8 9.3(2) . . . . ?
C6 N4 N10 O8 161.51(14) . . . . ?
C5 N5 N11 O10 -0.9(2) . . . . ?
C3 N5 N11 O10 -154.03(15) . . . . ?
C5 N5 N11 O9 -178.60(15) . . . . ?
C3 N5 N11 O9 28.3(2) . . . . ?
N6 C7 N12 N13 -82.93(17) . . . . ?
N6 C7 N12 C8 116.40(16) . . . . ?
C9 C8 N12 N13 -71.9(2) . . . . ?
C9 C8 N12 C7 88.6(2) . . . . ?
N16 C11 C12 N19 106.72(17) . . . . ?
N18A C11 C12 N19 -3.29(19) . . . . ?
N16 C11 C12 N19A 108.8(2) . . . . ?
N18B C11 C12 N19A 4.4(3) . . . . ?
N16 C11 C12 N17 1.49(19) . . . . ?
N18B C11 C12 N17 -102.9(3) . . . . ?
N18A C11 C12 N17 -108.53(16) . . . . ?
C7 N12 N13 O12 5.6(2) . . . . ?
C8 N12 N13 O12 167.29(15) . . . . ?
C7 N12 N13 O11 -175.58(15) . . . . ?
C8 N12 N13 O11 -13.9(2) . . . . ?
C8 C9 N14 N15 95.23(19) . . . . ?
C8 C9 N14 C10 -103.4(2) . . . . ?
N20 C13 C14 N21 2.07(18) . . . . ?
N16 C13 C14 N21 119.05(14) . . . . ?
N20 C13 C14 N18A -114.65(16) . . . . ?
N16 C13 C14 N18A 2.33(18) . . . . ?
N20 C13 C14 N18B -130.5(3) . . . . ?
N16 C13 C14 N18B -13.5(3) . . . . ?
N18B C11 N16 N22 -112.7(2) . . . . ?
N18A C11 N16 N22 -126.81(17) . . . . ?
C12 C11 N16 N22 123.39(16) . . . . ?
N18B C11 N16 C13 42.4(2) . . . . ?
N18A C11 N16 C13 28.29(19) . . . . ?
C12 C11 N16 C13 -81.51(16) . . . . ?
N20 C13 N16 N22 -109.03(17) . . . . ?
C14 C13 N16 N22 136.31(15) . . . . ?
N20 C13 N16 C11 95.61(16) . . . . ?
C14 C13 N16 C11 -19.04(17) . . . . ?
C9 N14 N15 O14 169.92(15) . . . . ?
C10 N14 N15 O14 7.5(2) . . . . ?
C9 N14 N15 O13 -11.3(2) . . . . ?
C10 N14 N15 O13 -173.70(16) . . . . ?
N21 C16 C15 N20 -1.9(2) . . . . ?
N19 C16 C15 N20 121.47(18) . . . . ?
N19A C16 C15 N20 106.6(6) . . . . ?
N21 C16 C15 N17 -120.47(15) . . . . ?
N19 C16 C15 N17 2.9(2) . . . . ?
N19A C16 C15 N17 -12.0(6) . . . . ?
N19 C12 N17 N23 174.70(17) . . . . ?
N19A C12 N17 N23 -171.9(6) . . . . ?
C11 C12 N17 N23 -67.35(19) . . . . ?
N19 C12 N17 C15 -41.66(19) . . . . ?
N19A C12 N17 C15 -28.3(6) . . . . ?
C11 C12 N17 C15 76.29(17) . . . . ?
N20 C15 N17 N23 52.6(2) . . . . ?
C16 C15 N17 N23 168.43(14) . . . . ?
N20 C15 N17 C12 -90.33(17) . . . . ?
C16 C15 N17 C12 25.53(18) . . . . ?
N17 C15 N20 N26 -106.96(18) . . . . ?
C16 C15 N20 N26 140.75(15) . . . . ?
N17 C15 N20 C13 56.2(2) . . . . ?
C16 C15 N20 C13 -56.09(19) . . . . ?
N16 C13 N20 N26 106.42(16) . . . . ?
C14 C13 N20 N26 -141.24(14) . . . . ?
N16 C13 N20 C15 -56.64(19) . . . . ?
C14 C13 N20 C15 55.70(18) . . . . ?
N19 C16 N21 C14 -54.2(2) . . . . ?
N19A C16 N21 C14 -52.1(3) . . . . ?
C15 C16 N21 C14 57.9(2) . . . . ?
N19 C16 N21 C17 89.5(2) . . . . ?
N19A C16 N21 C17 91.5(3) . . . . ?
C15 C16 N21 C17 -158.48(15) . . . . ?
N18A C14 N21 C16 56.41(19) . . . . ?
N18B C14 N21 C16 56.6(3) . . . . ?
C13 C14 N21 C16 -58.15(19) . . . . ?
N18A C14 N21 C17 -87.56(18) . . . . ?
N18B C14 N21 C17 -87.4(3) . . . . ?
C13 C14 N21 C17 157.88(14) . . . . ?
N27 C17 N21 C16 143.84(17) . . . . ?
N27 C17 N21 C14 -73.6(2) . . . . ?
C11 N16 N22 O16 -14.6(2) . . . . ?
C13 N16 N22 O16 -167.10(15) . . . . ?
C11 N16 N22 O15 169.24(16) . . . . ?
C13 N16 N22 O15 16.7(2) . . . . ?
C12 N17 N23 O18 -13.6(2) . . . . ?
C15 N17 N23 O18 -154.28(15) . . . . ?
C12 N17 N23 O17 167.39(15) . . . . ?
C15 N17 N23 O17 26.7(2) . . . . ?
O19A N24A N18A C11 -159.1(2) . . . . ?
O20A N24A N18A C11 27.1(4) . . . . ?
O19A N24A N18A C14 -26.2(4) . . . . ?
O20A N24A N18A C14 159.9(3) . . . . ?
N16 C11 N18A N24A 110.5(2) . . . . ?
C12 C11 N18A N24A -136.7(2) . . . . ?
N16 C11 N18A C14 -25.9(2) . . . . ?
C12 C11 N18A C14 86.89(19) . . . . ?
N21 C14 N18A N24A 119.6(3) . . . . ?
C13 C14 N18A N24A -122.5(2) . . . . ?
N21 C14 N18A C11 -103.41(19) . . . . ?
C13 C14 N18A C11 14.6(2) . . . . ?
O19B N24B N18B C11 171.0(8) . . . . ?
O20B N24B N18B C11 -2.6(15) . . . . ?
O19B N24B N18B C14 30.5(14) . . . . ?
O20B N24B N18B C14 -143.2(9) . . . . ?
N16 C11 N18B N24B 161.6(8) . . . . ?
C12 C11 N18B N24B -85.8(8) . . . . ?
N16 C11 N18B C14 -53.3(4) . . . . ?
C12 C11 N18B C14 59.4(5) . . . . ?
N21 C14 N18B N24B 66.2(8) . . . . ?
C13 C14 N18B N24B -172.8(7) . . . . ?
N21 C14 N18B C11 -78.0(5) . . . . ?
C13 C14 N18B C11 43.1(4) . . . . ?
N17 C12 N19 N25 -163.9(4) . . . . ?
C11 C12 N19 N25 79.6(4) . . . . ?
N17 C12 N19 C16 44.6(3) . . . . ?
C11 C12 N19 C16 -71.9(3) . . . . ?
N21 C16 N19 N25 -64.6(4) . . . . ?
C15 C16 N19 N25 177.5(4) . . . . ?
N21 C16 N19 C12 86.6(3) . . . . ?
C15 C16 N19 C12 -31.2(3) . . . . ?
C12 N19 N25 O22 9.9(5) . . . . ?
C16 N19 N25 O22 158.9(3) . . . . ?
C12 N19 N25 O21 -173.1(5) . . . . ?
C16 N19 N25 O21 -24.0(8) . . . . ?
N17 C12 N19A N25A -130.4(14) . . . . ?
C11 C12 N19A N25A 114.5(15) . . . . ?
N17 C12 N19A C16 19.4(10) . . . . ?
C11 C12 N19A C16 -95.7(9) . . . . ?
N21 C16 N19A N25A -107.0(19) . . . . ?
C15 C16 N19A N25A 138.9(18) . . . . ?
N21 C16 N19A C12 109.5(9) . . . . ?
C15 C16 N19A C12 -4.6(11) . . . . ?
C12 N19A N25A O22A -15(4) . . . . ?
C16 N19A N25A O22A -158(3) . . . . ?
C12 N19A N25A O21A 176(3) . . . . ?
C16 N19A N25A O21A 32(4) . . . . ?
C15 N20 N26 O24 -12.0(2) . . . . ?
C13 N20 N26 O24 -174.61(15) . . . . ?
C15 N20 N26 O23 170.75(15) . . . . ?
C13 N20 N26 O23 8.1(2) . . . . ?
O26 N28 N27 C17 4.8(4) . . . . ?
O25 N28 N27 C17 -176.4(2) . . . . ?
O26 N28 N27 C18 168.2(2) . . . . ?
O25 N28 N27 C18 -13.1(4) . . . . ?
O26A N28A N27 C17 0(3) . . . . ?
O25A N28A N27 C17 178(3) . . . . ?
O26A N28A N27 C18 168.9(17) . . . . ?
O25A N28A N27 C18 -13(4) . . . . ?
N21 C17 N27 N28 -78.3(3) . . . . ?
N21 C17 N27 N28A -70.9(15) . . . . ?
N21 C17 N27 C18 119.33(19) . . . . ?
C19A C18 N27 N28 -73.2(3) . . . . ?
C19B C18 N27 N28A -57(3) . . . . ?
C19A C18 N27 C17 89.3(3) . . . . ?
C19C C18 N27 C17 69.8(9) . . . . ?
C19B C18 N27 C17 110.0(18) . . . . ?
C19D C18 N27 C17 76(2) . . . . ?
N27 C18 C19A N29A -69.3(3) . . . . ?
C18 C19A N29A N30A 92.3(3) . . . . ?
C18 C19A N29A C20A -98.9(3) . . . . ?
C20A N29A N30A O28A 7.0(3) . . . . ?
C19A N29A N30A O28A 176.6(2) . . . . ?
C20A N29A N30A O27A -172.5(2) . . . . ?
C19A N29A N30A O27A -2.9(3) . . . . ?
N27 C18 C19B N29B 0(3) . . . . ?
C18 C19B N29B N30B 120(3) . . . . ?
C18 C19B N29B C20B -71(4) . . . . ?
C20B N29B N30B O28B -18(4) . . . . ?
C19B N29B N30B O28B 151(3) . . . . ?
C20B N29B N30B O27B 156(5) . . . . ?
C19B N29B N30B O27B -35(7) . . . . ?
N27 C18 C19C N29C 68(2) . . . . ?
C18 C19C N29C N30C -86(5) . . . . ?
C18 C19C N29C C20C 73(4) . . . . ?
C20C N29C N30C O28C 2(4) . . . . ?
C19C N29C N30C O28C 162(4) . . . . ?
C20C N29C N30C O27C 147(3) . . . . ?
C19C N29C N30C O27C -54(6) . . . . ?
N27 C18 C19D N29D -38(6) . . . . ?
C18 C19D N29D N30D -111(6) . . . . ?
C18 C19D N29D C20D 45(7) . . . . ?
C20D N29D N30D O28D 14(5) . . . . ?
C19D N29D N30D O28D 170(4) . . . . ?
C20D N29D N30D O27D -171(4) . . . . ?
C19D N29D N30D O27D -14(8) . . . . ?

_refine_diff_density_max         0.624
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.070

####################################################################### 
# 
# 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_pgv2014
_database_code_depnum_ccdc_archive 'CCDC 2111284'
loop_
_audit_author_name
_audit_author_address
'Ivan Vladimirovich Fedyanin'
;A N Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences
Russia
;
_audit_update_record             
;
2021-09-22 deposited with the CCDC.	2021-12-15 downloaded from the CCDC.
;

_publ_contact_name               'Fedyanin, Ivan V.'
_publ_contact_email              octy@xrlab.ineos.ac.ru

_audit_creation_method           'Modified SHELXL output'
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H11 N13 O12'
_chemical_formula_sum            'C8 H11 N13 O12'
_chemical_formula_weight         481.30

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   8.7416(2)
_cell_length_b                   11.9374(3)
_cell_length_c                   16.2335(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.2070(10)
_cell_angle_gamma                90
_cell_volume                     1680.61(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9679
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      34.73

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_F_000             984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.177
_shelx_estimated_absorpt_T_min   0.944
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEX II diffractometer'
_diffrn_detector_type            'Bruker PHOTON II CPAD area detector'
_diffrn_measurement_method       'ο scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32903
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.124
_diffrn_reflns_theta_max         33.004
_diffrn_reflns_theta_full        33.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6342
_reflns_number_gt                4984
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0500P)²+0.3000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6342
_refine_ls_number_parameters     299
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.0916
_refine_ls_wR_factor_gt          0.0877
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 1.06738(8) 0.11236(6) 0.47372(5) 0.01840(15) Uani 1 1 d . . . . .
O2 O 1.07174(8) 0.26512(7) 0.54890(5) 0.02214(16) Uani 1 1 d . . . . .
O3 O 1.03738(9) 0.35732(6) 0.31095(5) 0.01975(15) Uani 1 1 d . . . . .
O4 O 1.01571(10) 0.48175(7) 0.40751(5) 0.02366(17) Uani 1 1 d . . . . .
O5 O 0.42999(8) 0.15914(7) 0.58976(5) 0.01985(15) Uani 1 1 d . . . . .
O6 O 0.61168(9) 0.25615(6) 0.66135(4) 0.01833(14) Uani 1 1 d . . . . .
O7 O 0.43989(10) 0.48969(7) 0.34513(6) 0.0308(2) Uani 1 1 d . . . . .
O8 O 0.60417(10) 0.56429(6) 0.44264(6) 0.02623(18) Uani 1 1 d . . . . .
O9 O 0.91450(10) 0.10613(7) 0.25604(5) 0.02313(16) Uani 1 1 d . . . . .
O10 O 0.88855(10) -0.02703(6) 0.34560(5) 0.02476(17) Uani 1 1 d . . . . .
O11 O 0.25697(9) -0.02316(7) 0.25114(5) 0.02364(16) Uani 1 1 d . . . . .
O12 O 0.31878(9) -0.00264(6) 0.38506(5) 0.02095(15) Uani 1 1 d . . . . .
N1 N 0.84945(9) 0.17815(7) 0.51229(5) 0.01182(14) Uani 1 1 d . . . . .
N2 N 0.86655(9) 0.32878(7) 0.39885(5) 0.01183(14) Uani 1 1 d . . . . .
N3 N 0.61123(9) 0.23783(7) 0.52408(5) 0.01179(14) Uani 1 1 d . . . . .
N4 N 0.62241(9) 0.38415(6) 0.41201(5) 0.01296(14) Uani 1 1 d . . . . .
N5 N 0.78714(9) 0.14118(6) 0.36362(5) 0.01151(14) Uani 1 1 d . . . . .
N6 N 0.51562(8) 0.19940(6) 0.37950(5) 0.01096(14) Uani 1 1 d . . . . .
N7 N 1.00679(9) 0.18580(7) 0.51138(5) 0.01441(15) Uani 1 1 d . . . . .
N8 N 0.97977(9) 0.39579(7) 0.36922(5) 0.01437(15) Uani 1 1 d . . . . .
N9 N 0.54883(9) 0.21411(7) 0.59753(5) 0.01426(15) Uani 1 1 d . . . . .
N10 N 0.55248(10) 0.48646(7) 0.39833(6) 0.01864(17) Uani 1 1 d . . . . .
N11 N 0.87104(10) 0.06822(7) 0.31910(5) 0.01596(16) Uani 1 1 d . . . . .
N12 N 0.26805(9) 0.14786(7) 0.30579(5) 0.01409(15) Uani 1 1 d . . . . .
N13 N 0.28276(9) 0.03503(7) 0.31429(5) 0.01565(15) Uani 1 1 d . . . . .
C1 C 0.76691(10) 0.28112(7) 0.53013(5) 0.01180(15) Uani 1 1 d . . . . .
H1 H 0.802833 0.311042 0.586796 0.014 Uiso 1 1 calc R U . . .
C2 C 0.77403(10) 0.37409(8) 0.45966(6) 0.01243(16) Uani 1 1 d . . . . .
H2 H 0.814227 0.447501 0.482852 0.015 Uiso 1 1 calc R U . . .
C3 C 0.75648(10) 0.11269(7) 0.44619(5) 0.01110(15) Uani 1 1 d . . . . .
H3 H 0.768284 0.030370 0.456507 0.013 Uiso 1 1 calc R U . . .
C4 C 0.58861(10) 0.15293(7) 0.45643(5) 0.01120(15) Uani 1 1 d . . . . .
H4 H 0.526530 0.088666 0.473709 0.013 Uiso 1 1 calc R U . . .
C5 C 0.76905(10) 0.25702(7) 0.33987(5) 0.01059(15) Uani 1 1 d . . . . .
H5 H 0.791721 0.269064 0.281651 0.013 Uiso 1 1 calc R U . . .
C6 C 0.59895(10) 0.29298(7) 0.35026(5) 0.01069(15) Uani 1 1 d . . . . .
H6 H 0.544828 0.321775 0.296503 0.013 Uiso 1 1 calc R U . . .
C7 C 0.34776(10) 0.21326(8) 0.37409(6) 0.01269(16) Uani 1 1 d . . . . .
H7A H 0.312624 0.189045 0.426944 0.015 Uiso 1 1 calc R U . . .
H7B H 0.321308 0.293439 0.365711 0.015 Uiso 1 1 calc R U . . .
C8 C 0.24860(12) 0.19054(9) 0.22073(6) 0.01932(19) Uani 1 1 d . . . . .
H8A H 0.341370 0.174163 0.194699 0.029 Uiso 1 1 calc R U . . .
H8B H 0.232108 0.271719 0.221446 0.029 Uiso 1 1 calc R U . . .
H8C H 0.159285 0.154361 0.189010 0.029 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 1.2264(11) . ?
O2 N7 1.2260(11) . ?
O3 N8 1.2160(11) . ?
O4 N8 1.2202(11) . ?
O5 N9 1.2218(11) . ?
O6 N9 1.2183(11) . ?
O7 N10 1.2259(12) . ?
O8 N10 1.2261(12) . ?
O9 N11 1.2226(11) . ?
O10 N11 1.2186(11) . ?
O11 N13 1.2354(11) . ?
O12 N13 1.2371(11) . ?
N1 N7 1.3803(11) . ?
N1 C1 1.4724(12) . ?
N1 C3 1.4845(12) . ?
N2 N8 1.4036(11) . ?
N2 C2 1.4565(12) . ?
N2 C5 1.4739(11) . ?
N3 N9 1.4011(11) . ?
N3 C1 1.4475(12) . ?
N3 C4 1.4892(12) . ?
N4 N10 1.3713(11) . ?
N4 C2 1.4534(12) . ?
N4 C6 1.4763(11) . ?
N5 N11 1.3971(11) . ?
N5 C5 1.4390(11) . ?
N5 C3 1.4402(11) . ?
N6 C4 1.4402(11) . ?
N6 C6 1.4459(11) . ?
N6 C7 1.4683(11) . ?
N12 N13 1.3584(11) . ?
N12 C7 1.4597(12) . ?
N12 C8 1.4616(13) . ?
C1 C2 1.6006(13) . ?
C1 H1 1.0000 . ?
C2 H2 1.0000 . ?
C3 C4 1.5726(12) . ?
C3 H3 1.0000 . ?
C4 H4 1.0000 . ?
C5 C6 1.5770(12) . ?
C5 H5 1.0000 . ?
C6 H6 1.0000 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 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 117.41(7) . . ?
N7 N1 C3 118.88(7) . . ?
C1 N1 C3 110.13(7) . . ?
N8 N2 C2 119.74(7) . . ?
N8 N2 C5 118.93(7) . . ?
C2 N2 C5 109.34(7) . . ?
N9 N3 C1 118.53(7) . . ?
N9 N3 C4 117.40(7) . . ?
C1 N3 C4 109.25(7) . . ?
N10 N4 C2 121.20(8) . . ?
N10 N4 C6 121.70(7) . . ?
C2 N4 C6 109.88(7) . . ?
N11 N5 C5 120.50(7) . . ?
N11 N5 C3 120.36(7) . . ?
C5 N5 C3 116.70(7) . . ?
C4 N6 C6 113.30(7) . . ?
C4 N6 C7 115.21(7) . . ?
C6 N6 C7 115.73(7) . . ?
O2 N7 O1 126.70(8) . . ?
O2 N7 N1 116.47(8) . . ?
O1 N7 N1 116.82(8) . . ?
O3 N8 O4 127.48(8) . . ?
O3 N8 N2 115.47(8) . . ?
O4 N8 N2 116.89(8) . . ?
O6 N9 O5 126.58(8) . . ?
O6 N9 N3 117.28(8) . . ?
O5 N9 N3 115.94(8) . . ?
O7 N10 O8 126.42(9) . . ?
O7 N10 N4 116.38(8) . . ?
O8 N10 N4 117.12(8) . . ?
O10 N11 O9 127.05(9) . . ?
O10 N11 N5 116.73(8) . . ?
O9 N11 N5 116.16(8) . . ?
N13 N12 C7 115.03(7) . . ?
N13 N12 C8 116.10(8) . . ?
C7 N12 C8 121.27(8) . . ?
O11 N13 O12 124.40(9) . . ?
O11 N13 N12 117.91(8) . . ?
O12 N13 N12 117.68(8) . . ?
N3 C1 N1 99.69(7) . . ?
N3 C1 C2 108.64(7) . . ?
N1 C1 C2 111.99(7) . . ?
N3 C1 H1 112.0 . . ?
N1 C1 H1 112.0 . . ?
C2 C1 H1 112.0 . . ?
N4 C2 N2 102.52(7) . . ?
N4 C2 C1 108.85(7) . . ?
N2 C2 C1 107.56(7) . . ?
N4 C2 H2 112.4 . . ?
N2 C2 H2 112.4 . . ?
C1 C2 H2 112.4 . . ?
N5 C3 N1 113.55(7) . . ?
N5 C3 C4 108.14(7) . . ?
N1 C3 C4 101.32(7) . . ?
N5 C3 H3 111.1 . . ?
N1 C3 H3 111.1 . . ?
C4 C3 H3 111.1 . . ?
N6 C4 N3 112.38(7) . . ?
N6 C4 C3 110.11(7) . . ?
N3 C4 C3 104.27(7) . . ?
N6 C4 H4 110.0 . . ?
N3 C4 H4 110.0 . . ?
C3 C4 H4 110.0 . . ?
N5 C5 N2 110.44(7) . . ?
N5 C5 C6 107.84(7) . . ?
N2 C5 C6 104.38(7) . . ?
N5 C5 H5 111.3 . . ?
N2 C5 H5 111.3 . . ?
C6 C5 H5 111.3 . . ?
N6 C6 N4 112.30(7) . . ?
N6 C6 C5 110.21(7) . . ?
N4 C6 C5 102.76(7) . . ?
N6 C6 H6 110.4 . . ?
N4 C6 H6 110.4 . . ?
C5 C6 H6 110.4 . . ?
N12 C7 N6 111.31(7) . . ?
N12 C7 H7A 109.4 . . ?
N6 C7 H7A 109.4 . . ?
N12 C7 H7B 109.4 . . ?
N6 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
N12 C8 H8A 109.5 . . ?
N12 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N12 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 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
C1 N1 N7 O2 21.40(11) . . . . ?
C3 N1 N7 O2 158.19(8) . . . . ?
C1 N1 N7 O1 -159.08(8) . . . . ?
C3 N1 N7 O1 -22.29(12) . . . . ?
C2 N2 N8 O3 -170.64(8) . . . . ?
C5 N2 N8 O3 -31.92(11) . . . . ?
C2 N2 N8 O4 13.70(12) . . . . ?
C5 N2 N8 O4 152.42(8) . . . . ?
C1 N3 N9 O6 17.81(11) . . . . ?
C4 N3 N9 O6 152.59(8) . . . . ?
C1 N3 N9 O5 -167.00(8) . . . . ?
C4 N3 N9 O5 -32.21(11) . . . . ?
C2 N4 N10 O7 166.58(9) . . . . ?
C6 N4 N10 O7 19.29(14) . . . . ?
C2 N4 N10 O8 -16.45(13) . . . . ?
C6 N4 N10 O8 -163.74(9) . . . . ?
C5 N5 N11 O10 176.08(8) . . . . ?
C3 N5 N11 O10 14.39(13) . . . . ?
C5 N5 N11 O9 -6.29(13) . . . . ?
C3 N5 N11 O9 -167.98(8) . . . . ?
C7 N12 N13 O11 -160.13(8) . . . . ?
C8 N12 N13 O11 -10.06(12) . . . . ?
C7 N12 N13 O12 20.98(12) . . . . ?
C8 N12 N13 O12 171.05(8) . . . . ?
N9 N3 C1 N1 101.38(8) . . . . ?
C4 N3 C1 N1 -36.75(8) . . . . ?
N9 N3 C1 C2 -141.33(7) . . . . ?
C4 N3 C1 C2 80.54(8) . . . . ?
N7 N1 C1 N3 179.27(7) . . . . ?
C3 N1 C1 N3 38.95(8) . . . . ?
N7 N1 C1 C2 64.52(10) . . . . ?
C3 N1 C1 C2 -75.79(9) . . . . ?
N10 N4 C2 N2 -117.28(9) . . . . ?
C6 N4 C2 N2 33.44(9) . . . . ?
N10 N4 C2 C1 129.00(9) . . . . ?
C6 N4 C2 C1 -80.28(9) . . . . ?
N8 N2 C2 N4 110.59(8) . . . . ?
C5 N2 C2 N4 -31.67(9) . . . . ?
N8 N2 C2 C1 -134.74(8) . . . . ?
C5 N2 C2 C1 82.99(8) . . . . ?
N3 C1 C2 N4 -0.52(9) . . . . ?
N1 C1 C2 N4 108.61(8) . . . . ?
N3 C1 C2 N2 -110.90(8) . . . . ?
N1 C1 C2 N2 -1.77(10) . . . . ?
N11 N5 C3 N1 106.52(9) . . . . ?
C5 N5 C3 N1 -55.84(10) . . . . ?
N11 N5 C3 C4 -141.89(8) . . . . ?
C5 N5 C3 C4 55.75(10) . . . . ?
N7 N1 C3 N5 -49.57(10) . . . . ?
C1 N1 C3 N5 90.09(9) . . . . ?
N7 N1 C3 C4 -165.26(7) . . . . ?
C1 N1 C3 C4 -25.61(9) . . . . ?
C6 N6 C4 N3 57.20(9) . . . . ?
C7 N6 C4 N3 -79.28(9) . . . . ?
C6 N6 C4 C3 -58.56(9) . . . . ?
C7 N6 C4 C3 164.96(7) . . . . ?
N9 N3 C4 N6 124.35(8) . . . . ?
C1 N3 C4 N6 -96.99(8) . . . . ?
N9 N3 C4 C3 -116.42(8) . . . . ?
C1 N3 C4 C3 22.24(9) . . . . ?
N5 C3 C4 N6 3.22(10) . . . . ?
N1 C3 C4 N6 122.84(7) . . . . ?
N5 C3 C4 N3 -117.54(7) . . . . ?
N1 C3 C4 N3 2.08(8) . . . . ?
N11 N5 C5 N2 -106.02(9) . . . . ?
C3 N5 C5 N2 56.31(10) . . . . ?
N11 N5 C5 C6 140.50(8) . . . . ?
C3 N5 C5 C6 -57.17(9) . . . . ?
N8 N2 C5 N5 120.16(8) . . . . ?
C2 N2 C5 N5 -97.23(8) . . . . ?
N8 N2 C5 C6 -124.18(8) . . . . ?
C2 N2 C5 C6 18.44(9) . . . . ?
C4 N6 C6 N4 -56.94(9) . . . . ?
C7 N6 C6 N4 79.31(9) . . . . ?
C4 N6 C6 C5 56.97(9) . . . . ?
C7 N6 C6 C5 -166.78(7) . . . . ?
N10 N4 C6 N6 -113.13(9) . . . . ?
C2 N4 C6 N6 96.32(8) . . . . ?
N10 N4 C6 C5 128.47(8) . . . . ?
C2 N4 C6 C5 -22.09(9) . . . . ?
N5 C5 C6 N6 -0.34(9) . . . . ?
N2 C5 C6 N6 -117.81(7) . . . . ?
N5 C5 C6 N4 119.53(7) . . . . ?
N2 C5 C6 N4 2.05(8) . . . . ?
N13 N12 C7 N6 65.30(10) . . . . ?
C8 N12 C7 N6 -83.08(10) . . . . ?
C4 N6 C7 N12 -119.51(8) . . . . ?
C6 N6 C7 N12 105.08(9) . . . . ?

_refine_diff_density_max         0.449
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.056

####################################################################### 
# 
# 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_POK2160
_database_code_depnum_ccdc_archive 'CCDC 2104897'
loop_
_audit_author_name
_audit_author_address
'Darina Ildarovna Nasyrova'
;N D Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences
Russia
;
_audit_update_record             
;
2021-09-22 deposited with the CCDC.	2021-12-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_POK2160             
;
PROBLEM: Short Inter D...A Contact
RESPONSE: This is due to the molecular structure.
;
_audit_creation_date             2021-09-22
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6394)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H13 N17 O14'
_chemical_formula_sum            'C9 H13 N17 O14'
_chemical_formula_weight         583.36
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C9 H13 N17 O14'
_chemical_oxdiff_usercomment     POK2160
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           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   17.7402(4)
_cell_length_b                   9.2797(4)
_cell_length_c                   12.2787(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2021.37(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9764
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      77.7610
_cell_measurement_theta_min      4.6840
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.106a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17943
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.343
_diffrn_reflns_theta_min         4.765
_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 0.992
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -64.00  24.00   0.50    2.50    --  -48.01  62.00 -21.00  176
  2  ω   -119.00 -32.00   0.50    2.50    --  -48.01 -62.00-158.00  174
  3  ω   -161.00 -74.00   0.50    2.50    --  -90.00 -62.00-158.00  174
  4  ω    -73.00 -18.00   0.50    2.50    --  -90.00  62.00 -21.00  110
  5  ω     96.00 178.00   0.50    2.50    --  111.50  62.00 -21.00  164
  6  ω     40.00  73.00   0.50    2.50    --  111.50 -62.00-158.00   66
  7  ω   -119.00 -73.00   0.50    2.50    --  -48.01-125.00 120.00   92
  8  ω   -119.00 -73.00   0.50    2.50    --  -48.01-125.00 -90.00   92
  9  ω    -23.00  64.00   0.50    2.50    --   48.01 -62.00-158.00  174
 10  ω     32.00 120.00   0.50    2.50    --   48.01  62.00 -21.00  176
 11  ω    -51.00 -18.00   0.50    2.50    --  -90.00  45.00 150.00   66
 12  ω    -51.00 -18.00   0.50    2.50    --  -90.00  45.00-180.00   66
 13  ω     40.00  71.00   0.50    2.50    --  111.50 -61.00-120.00   62
 14  ω    101.00 178.00   0.50    2.50    --  111.50  30.00  90.00  154
 15  ω     40.00  71.00   0.50    2.50    --  111.50 -61.00  60.00   62
 16  ω     40.00  71.00   0.50    2.50    --  111.50 -61.00  30.00   62
 17  ω     40.00 105.00   0.50    2.50    --  111.50 -95.00  30.00  130
 18  ω    101.00 178.00   0.50    2.50    --  111.50  45.00  60.00  154
 19  ω     40.00  71.00   0.50    2.50    --  111.50 -61.00 120.00   62
 20  ω     40.00 105.00   0.50    2.50    --  111.50 -77.00 -30.00  130
 21  ω    101.00 178.00   0.50    2.50    --  111.50  45.00 -60.00  154
 22  ω     40.00 105.00   0.50    2.50    --  111.50 -77.00  90.00  130
 23  ω    101.00 178.00   0.50    2.50    --  111.50  15.00-120.00  154
 24  ω    101.00 178.00   0.50    2.50    --  111.50  30.00 -90.00  154
 25  ω     40.00 105.00   0.50    2.50    --  111.50 -77.00-120.00  130
 26  ω     40.00 101.00   0.50    2.50    --  111.50 -77.00-180.00  122
 27  ω     48.00  74.00   0.50    2.50    --  111.50 -77.00 -60.00   52
 28  ω     43.00 100.00   0.50    2.50    --  111.50 -95.00-180.00  114
;
_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      -0.0575060000
_diffrn_orient_matrix_UB_12      -0.1244388000
_diffrn_orient_matrix_UB_13      0.0002981000
_diffrn_orient_matrix_UB_21      -0.0446696000
_diffrn_orient_matrix_UB_22      0.0748654000
_diffrn_orient_matrix_UB_23      -0.0915572000
_diffrn_orient_matrix_UB_31      0.0473503000
_diffrn_orient_matrix_UB_32      -0.0803930000
_diffrn_orient_matrix_UB_33      -0.0857731000
_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         0.752
_reflns_Friedel_fraction_full    0.881
_reflns_Friedel_fraction_max     0.804
_reflns_number_gt                3539
_reflns_number_total             3924
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_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         0.418
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.2(4)
_refine_ls_extinction_coef       0.0019(5)
_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   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         3924
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0521
_refine_ls_restrained_S_all      1.080
_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)+(0.0959P)²+0.9800P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1471
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 1.2(4)
 -0.2(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
;
_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 0.2583(2) 0.0873(5) 0.5989(3) 0.0422(9) Uani 1 1 d . . . . .
N1 N 0.3507(2) 0.2419(5) 0.5611(3) 0.0327(9) Uani 1 1 d . . . . .
C1 C 0.4150(3) 0.3148(6) 0.6071(4) 0.0327(10) Uani 1 1 d . . . . .
H1 H 0.440611 0.255481 0.664128 0.039 Uiso 1 1 calc R U . . .
O2 O 0.3636(2) 0.0681(5) 0.6886(3) 0.0444(9) Uani 1 1 d . . . . .
N2 N 0.4395(2) 0.3130(5) 0.4078(3) 0.0308(9) Uani 1 1 d . . . . .
C2 C 0.4712(2) 0.3586(6) 0.5108(4) 0.0307(10) Uani 1 1 d . . . . .
H2 H 0.523043 0.319003 0.522366 0.037 Uiso 1 1 calc R U . . .
N3 N 0.3768(2) 0.4392(5) 0.6534(3) 0.0316(9) Uani 1 1 d . . . . .
O3 O 0.4561(2) 0.2284(5) 0.2402(3) 0.0415(9) Uani 1 1 d . . . . .
C3 C 0.2976(3) 0.3520(6) 0.5193(4) 0.0308(10) Uani 1 1 d . . . . .
H3 H 0.244274 0.323402 0.534315 0.037 Uiso 1 1 calc R U . . .
N4 N 0.4711(2) 0.5142(5) 0.5052(4) 0.0304(9) Uani 1 1 d . . . . .
O4 O 0.5342(2) 0.1658(4) 0.3688(3) 0.0393(9) Uani 1 1 d . . . . .
C4 C 0.3176(3) 0.4947(6) 0.5791(4) 0.0307(10) Uani 1 1 d . . . . .
H4 H 0.273373 0.530495 0.621635 0.037 Uiso 1 1 calc R U . . .
O5 O 0.3751(2) 0.6286(5) 0.7590(4) 0.0495(11) Uani 1 1 d . . . . .
N5 N 0.3092(2) 0.3748(5) 0.4054(3) 0.0313(9) Uani 1 1 d . . . . .
C5 C 0.3847(2) 0.4186(6) 0.3724(4) 0.0286(10) Uani 1 1 d . . . . .
H5 H 0.387666 0.434969 0.291983 0.034 Uiso 1 1 calc R U . . .
O6 O 0.4706(2) 0.4790(5) 0.7657(4) 0.0465(10) Uani 1 1 d . . . . .
N6 N 0.3423(2) 0.6014(5) 0.5035(3) 0.0289(8) Uani 1 1 d . . . . .
C6 C 0.4054(2) 0.5575(6) 0.4369(4) 0.0301(10) Uani 1 1 d . . . . .
H6 H 0.420050 0.636614 0.385792 0.036 Uiso 1 1 calc R U . . .
N7 N 0.3217(3) 0.1253(5) 0.6224(4) 0.0358(10) Uani 1 1 d . . . . .
O7 O 0.5345(2) 0.7133(4) 0.4645(4) 0.0401(9) Uani 1 1 d . . . . .
C7 C 0.3395(3) 0.7521(6) 0.5340(4) 0.0306(10) Uani 1 1 d . . . . .
H7A H 0.390220 0.784560 0.557116 0.037 Uiso 1 1 calc R U . . .
H7B H 0.304546 0.765017 0.596083 0.037 Uiso 1 1 calc R U . . .
N8 N 0.4802(2) 0.2316(5) 0.3329(4) 0.0339(10) Uani 1 1 d . . . . .
O8 O 0.5970(2) 0.5223(5) 0.5171(4) 0.0483(10) Uani 1 1 d . . . . .
C8 C 0.2385(3) 0.8242(6) 0.3929(4) 0.0317(11) Uani 1 1 d . . . . .
H8A H 0.242901 0.835713 0.312997 0.038 Uiso 1 1 calc R U . . .
H8B H 0.219917 0.725392 0.407182 0.038 Uiso 1 1 calc R U . . .
O9 O 0.2783(2) 0.3249(4) 0.2346(3) 0.0367(8) Uani 1 1 d . . . . .
N9 N 0.4089(3) 0.5204(5) 0.7309(4) 0.0369(10) Uani 1 1 d . . . . .
C9 C 0.1470(3) 0.9076(6) 0.5274(4) 0.0323(11) Uani 1 1 d . . . . .
O10 O 0.20224(19) 0.2611(4) 0.3657(3) 0.0365(8) Uani 1 1 d . . . . .
N10 N 0.5394(2) 0.5873(5) 0.4921(4) 0.0357(10) Uani 1 1 d . . . . .
O11 O 0.3273(2) 1.0327(4) 0.3383(3) 0.0387(9) Uani 1 1 d . . . . .
N11 N 0.2612(2) 0.3139(5) 0.3308(4) 0.0321(9) Uani 1 1 d . . . . .
N12 N 0.3139(2) 0.8391(5) 0.4413(4) 0.0305(9) Uani 1 1 d . . . . .
O12 O 0.41766(19) 0.9740(4) 0.4495(4) 0.0389(8) Uani 1 1 d . . . . .
O13 O 0.07570(19) 0.8070(5) 0.7089(3) 0.0421(10) Uani 1 1 d . . . . .
N13 N 0.3552(2) 0.9542(5) 0.4078(4) 0.0322(9) Uani 1 1 d . . . . .
N14 N 0.1838(2) 0.9251(5) 0.4326(4) 0.0343(10) Uani 1 1 d . . . . .
H14 H 0.181(5) 1.002(10) 0.393(8) 0.06(2) Uiso 1 1 d . . . . .
O14 O 0.1658(2) 0.6491(5) 0.7236(3) 0.0399(9) Uani 1 1 d . . . . .
N15 N 0.0975(3) 1.0058(6) 0.5581(4) 0.0399(10) Uani 1 1 d . . . . .
H15A H 0.078(3) 0.990(6) 0.630(6) 0.032(15) Uiso 1 1 d . . . . .
H15B H 0.084(5) 1.076(9) 0.510(8) 0.06(2) Uiso 1 1 d . . . . .
N16 N 0.1685(2) 0.7868(5) 0.5801(4) 0.0328(9) Uani 1 1 d . . . . .
N17 N 0.1346(3) 0.7506(5) 0.6740(4) 0.0355(10) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 N7 1.214(6) . ?
N1 C1 1.442(7) . ?
N1 C3 1.481(7) . ?
N1 N7 1.415(6) . ?
C1 H1 1.0000 . ?
C1 C2 1.599(7) . ?
C1 N3 1.454(7) . ?
O2 N7 1.222(6) . ?
N2 C2 1.447(6) . ?
N2 C5 1.446(6) . ?
N2 N8 1.392(6) . ?
C2 H2 1.0000 . ?
C2 N4 1.446(7) . ?
N3 C4 1.483(6) . ?
N3 N9 1.341(6) . ?
O3 N8 1.217(6) . ?
C3 H3 1.0000 . ?
C3 C4 1.555(7) . ?
C3 N5 1.429(6) . ?
N4 C6 1.490(6) . ?
N4 N10 1.398(6) . ?
O4 N8 1.217(6) . ?
C4 H4 1.0000 . ?
C4 N6 1.426(7) . ?
O5 N9 1.220(6) . ?
N5 C5 1.459(6) . ?
N5 N11 1.372(6) . ?
C5 H5 1.0000 . ?
C5 C6 1.557(7) . ?
O6 N9 1.236(6) . ?
N6 C6 1.446(6) . ?
N6 C7 1.449(7) . ?
C6 H6 1.0000 . ?
O7 N10 1.220(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 N12 1.468(7) . ?
O8 N10 1.225(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 N12 1.469(6) . ?
C8 N14 1.435(7) . ?
O9 N11 1.223(6) . ?
C9 N14 1.344(7) . ?
C9 N15 1.321(7) . ?
C9 N16 1.350(7) . ?
O10 N11 1.232(6) . ?
O11 N13 1.226(6) . ?
N12 N13 1.359(6) . ?
O12 N13 1.236(6) . ?
O13 N17 1.245(6) . ?
N14 H14 0.86(9) . ?
O14 N17 1.251(6) . ?
N15 H15A 0.96(7) . ?
N15 H15B 0.91(9) . ?
N16 N17 1.342(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C3 108.4(4) . . ?
N7 N1 C1 116.0(4) . . ?
N7 N1 C3 118.8(4) . . ?
N1 C1 H1 112.0 . . ?
N1 C1 C2 108.9(4) . . ?
N1 C1 N3 99.0(4) . . ?
C2 C1 H1 112.0 . . ?
N3 C1 H1 112.0 . . ?
N3 C1 C2 112.2(4) . . ?
C5 N2 C2 109.0(4) . . ?
N8 N2 C2 122.2(4) . . ?
N8 N2 C5 121.2(4) . . ?
C1 C2 H2 112.0 . . ?
N2 C2 C1 109.3(4) . . ?
N2 C2 H2 112.0 . . ?
N4 C2 C1 106.7(4) . . ?
N4 C2 N2 104.5(4) . . ?
N4 C2 H2 112.0 . . ?
C1 N3 C4 111.4(4) . . ?
N9 N3 C1 121.7(4) . . ?
N9 N3 C4 122.8(4) . . ?
N1 C3 H3 110.8 . . ?
N1 C3 C4 106.2(4) . . ?
C4 C3 H3 110.8 . . ?
N5 C3 N1 110.5(4) . . ?
N5 C3 H3 110.8 . . ?
N5 C3 C4 107.6(4) . . ?
C2 N4 C6 107.3(4) . . ?
N10 N4 C2 119.3(4) . . ?
N10 N4 C6 118.8(4) . . ?
N3 C4 C3 99.0(4) . . ?
N3 C4 H4 110.5 . . ?
C3 C4 H4 110.5 . . ?
N6 C4 N3 115.1(4) . . ?
N6 C4 C3 110.7(4) . . ?
N6 C4 H4 110.5 . . ?
C3 N5 C5 116.4(4) . . ?
N11 N5 C3 120.2(4) . . ?
N11 N5 C5 119.9(4) . . ?
N2 C5 N5 110.2(4) . . ?
N2 C5 H5 111.4 . . ?
N2 C5 C6 104.4(4) . . ?
N5 C5 H5 111.4 . . ?
N5 C5 C6 107.8(4) . . ?
C6 C5 H5 111.4 . . ?
C4 N6 C6 114.2(4) . . ?
C4 N6 C7 119.4(4) . . ?
C6 N6 C7 116.4(4) . . ?
N4 C6 C5 104.3(4) . . ?
N4 C6 H6 110.4 . . ?
C5 C6 H6 110.4 . . ?
N6 C6 N4 111.3(4) . . ?
N6 C6 C5 109.8(4) . . ?
N6 C6 H6 110.4 . . ?
O1 N7 N1 115.6(5) . . ?
O1 N7 O2 126.6(5) . . ?
O2 N7 N1 117.7(4) . . ?
N6 C7 H7A 109.7 . . ?
N6 C7 H7B 109.7 . . ?
N6 C7 N12 109.9(4) . . ?
H7A C7 H7B 108.2 . . ?
N12 C7 H7A 109.7 . . ?
N12 C7 H7B 109.7 . . ?
O3 N8 N2 116.7(4) . . ?
O3 N8 O4 127.0(5) . . ?
O4 N8 N2 116.2(4) . . ?
H8A C8 H8B 107.6 . . ?
N12 C8 H8A 108.6 . . ?
N12 C8 H8B 108.6 . . ?
N14 C8 H8A 108.6 . . ?
N14 C8 H8B 108.6 . . ?
N14 C8 N12 114.7(4) . . ?
O5 N9 N3 117.0(4) . . ?
O5 N9 O6 126.4(5) . . ?
O6 N9 N3 116.6(5) . . ?
N14 C9 N16 112.3(4) . . ?
N15 C9 N14 119.1(5) . . ?
N15 C9 N16 128.6(5) . . ?
O7 N10 N4 115.8(4) . . ?
O7 N10 O8 127.0(4) . . ?
O8 N10 N4 117.0(4) . . ?
O9 N11 N5 117.2(4) . . ?
O9 N11 O10 125.3(4) . . ?
O10 N11 N5 117.3(4) . . ?
C7 N12 C8 122.9(4) . . ?
N13 N12 C7 120.0(4) . . ?
N13 N12 C8 116.2(4) . . ?
O11 N13 N12 117.4(4) . . ?
O11 N13 O12 124.2(4) . . ?
O12 N13 N12 118.3(4) . . ?
C8 N14 H14 112(6) . . ?
C9 N14 C8 122.9(5) . . ?
C9 N14 H14 124(6) . . ?
C9 N15 H15A 114(4) . . ?
C9 N15 H15B 119(6) . . ?
H15A N15 H15B 127(7) . . ?
N17 N16 C9 119.6(4) . . ?
O13 N17 O14 121.3(4) . . ?
O13 N17 N16 124.5(5) . . ?
O14 N17 N16 114.1(4) . . ?

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
N14 H14 O10 0.86(9) 2.46(9) 3.241(6) 151(8) 1_565 yes
N15 H15A O3 0.96(7) 2.66(6) 3.189(7) 115(4) 4_565 yes
N15 H15A O13 0.96(7) 1.96(6) 2.642(7) 126(5) . yes
N15 H15B O7 0.91(9) 2.22(9) 3.061(7) 154(8) 3_475 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 C1 C2 N2 0.7(6) . . . . ?
N1 C1 C2 N4 113.1(4) . . . . ?
N1 C1 N3 C4 -40.9(5) . . . . ?
N1 C1 N3 N9 161.2(4) . . . . ?
N1 C3 C4 N3 -4.0(5) . . . . ?
N1 C3 C4 N6 117.3(4) . . . . ?
N1 C3 N5 C5 -57.4(6) . . . . ?
N1 C3 N5 N11 101.7(5) . . . . ?
C1 N1 C3 C4 -20.7(5) . . . . ?
C1 N1 C3 N5 95.8(5) . . . . ?
C1 N1 N7 O1 162.7(4) . . . . ?
C1 N1 N7 O2 -21.3(7) . . . . ?
C1 C2 N4 C6 -84.5(4) . . . . ?
C1 C2 N4 N10 136.7(4) . . . . ?
C1 N3 C4 C3 28.1(5) . . . . ?
C1 N3 C4 N6 -89.9(5) . . . . ?
C1 N3 N9 O5 174.7(5) . . . . ?
C1 N3 N9 O6 -4.3(7) . . . . ?
N2 C2 N4 C6 31.2(5) . . . . ?
N2 C2 N4 N10 -107.7(4) . . . . ?
N2 C5 C6 N4 -0.7(4) . . . . ?
N2 C5 C6 N6 -120.1(4) . . . . ?
C2 C1 N3 C4 73.8(5) . . . . ?
C2 C1 N3 N9 -84.1(6) . . . . ?
C2 N2 C5 N5 -95.4(5) . . . . ?
C2 N2 C5 C6 20.2(5) . . . . ?
C2 N2 N8 O3 -162.8(5) . . . . ?
C2 N2 N8 O4 20.5(7) . . . . ?
C2 N4 C6 C5 -18.8(5) . . . . ?
C2 N4 C6 N6 99.6(5) . . . . ?
C2 N4 N10 O7 164.6(5) . . . . ?
C2 N4 N10 O8 -20.5(7) . . . . ?
N3 C1 C2 N2 -107.8(5) . . . . ?
N3 C1 C2 N4 4.6(5) . . . . ?
N3 C4 N6 C6 55.0(5) . . . . ?
N3 C4 N6 C7 -89.4(5) . . . . ?
C3 N1 C1 C2 -81.2(5) . . . . ?
C3 N1 C1 N3 36.1(5) . . . . ?
C3 N1 N7 O1 30.8(6) . . . . ?
C3 N1 N7 O2 -153.2(5) . . . . ?
C3 C4 N6 C6 -56.2(5) . . . . ?
C3 C4 N6 C7 159.4(4) . . . . ?
C3 N5 C5 N2 57.5(6) . . . . ?
C3 N5 C5 C6 -55.9(6) . . . . ?
C3 N5 N11 O9 -172.7(5) . . . . ?
C3 N5 N11 O10 12.0(7) . . . . ?
C4 N3 N9 O5 19.3(7) . . . . ?
C4 N3 N9 O6 -159.7(5) . . . . ?
C4 C3 N5 C5 58.1(6) . . . . ?
C4 C3 N5 N11 -142.7(4) . . . . ?
C4 N6 C6 N4 -56.9(5) . . . . ?
C4 N6 C6 C5 58.1(5) . . . . ?
C4 N6 C7 N12 -139.7(4) . . . . ?
N5 C3 C4 N3 -122.4(4) . . . . ?
N5 C3 C4 N6 -1.1(5) . . . . ?
N5 C5 C6 N4 116.5(4) . . . . ?
N5 C5 C6 N6 -2.9(5) . . . . ?
C5 N2 C2 C1 81.5(5) . . . . ?
C5 N2 C2 N4 -32.4(5) . . . . ?
C5 N2 N8 O3 -16.5(7) . . . . ?
C5 N2 N8 O4 166.8(4) . . . . ?
C5 N5 N11 O9 -14.3(7) . . . . ?
C5 N5 N11 O10 170.4(4) . . . . ?
N6 C7 N12 C8 63.7(5) . . . . ?
N6 C7 N12 N13 -127.2(4) . . . . ?
C6 N4 N10 O7 30.4(7) . . . . ?
C6 N4 N10 O8 -154.7(5) . . . . ?
C6 N6 C7 N12 76.6(5) . . . . ?
N7 N1 C1 C2 142.2(4) . . . . ?
N7 N1 C1 N3 -100.5(5) . . . . ?
N7 N1 C3 C4 114.5(4) . . . . ?
N7 N1 C3 N5 -129.1(4) . . . . ?
C7 N6 C6 N4 88.6(5) . . . . ?
C7 N6 C6 C5 -156.4(4) . . . . ?
C7 N12 N13 O11 -172.0(4) . . . . ?
C7 N12 N13 O12 7.4(7) . . . . ?
N8 N2 C2 C1 -128.6(4) . . . . ?
N8 N2 C2 N4 117.6(5) . . . . ?
N8 N2 C5 N5 114.3(5) . . . . ?
N8 N2 C5 C6 -130.1(4) . . . . ?
C8 N12 N13 O11 -2.2(6) . . . . ?
C8 N12 N13 O12 177.2(4) . . . . ?
N9 N3 C4 C3 -174.2(4) . . . . ?
N9 N3 C4 N6 67.7(6) . . . . ?
C9 N16 N17 O13 12.3(7) . . . . ?
C9 N16 N17 O14 -170.3(5) . . . . ?
N10 N4 C6 C5 120.3(4) . . . . ?
N10 N4 C6 N6 -121.4(5) . . . . ?
N11 N5 C5 N2 -101.7(5) . . . . ?
N11 N5 C5 C6 144.9(4) . . . . ?
N12 C8 N14 C9 -80.7(6) . . . . ?
N14 C8 N12 C7 95.9(6) . . . . ?
N14 C8 N12 N13 -73.6(6) . . . . ?
N14 C9 N16 N17 -177.1(4) . . . . ?
N15 C9 N14 C8 179.9(5) . . . . ?
N15 C9 N16 N17 4.0(8) . . . . ?
N16 C9 N14 C8 0.9(7) . . . . ?

_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 2.315
_oxdiff_exptl_absorpt_empirical_full_min 0.479
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.2(4)
2 -0.2(4)

