# Supplementary Information (SI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2025

####################################################################### 
# 
# 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. 
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data_NpNDip91_LT
_database_code_depnum_ccdc_archive 'CCDC 2395322'
loop_
_audit_author_name
_audit_author_address
'Mikhail Grigoriev'
;Frumkin Institute of Physical Chemistry and Electrochemistry
Russia
;
_audit_update_record             
;
2024-11-01 deposited with the CCDC.	2025-02-05 downloaded from the CCDC.
;
_audit_creation_date             2024-09-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H34 N5 Np O7, N3 Np O11'
_chemical_formula_sum            'C32 H34 N8 Np2 O18'
_chemical_formula_weight         1292.67
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Np Np -11.4937 4.1493 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.9713(7)
_cell_length_b                   11.3635(5)
_cell_length_c                   22.5333(9)
_cell_angle_alpha                90
_cell_angle_beta                 98.939(1)
_cell_angle_gamma                90
_cell_volume                     4039.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.17
_cell_measurement_theta_min      2.47
_shelx_estimated_absorpt_T_max   0.530
_shelx_estimated_absorpt_T_min   0.287
_exptl_absorpt_coefficient_mu    5.201
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.125
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       bulk
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            75724
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         3.430
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  
'Bruker KAPPA APEX II area-detector diffractometer'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10342
_reflns_number_total             11748
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    ?
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         11748
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0194
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0124P)²+3.6776P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0365
_refine_ls_wR_factor_ref         0.0382
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C21(H21A,H21B), C23(H23A,H23B), C31(H31A,H31B)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C16(H16), C17(H17),
 C19(H19), C20(H20), C26(H26), C27(H27), C29(H29), C30(H30)
1.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C32(H32A,H32B,
 H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Np1 Np 0.38447(2) 0.44906(2) 0.85811(2) 0.00757(2) Uani 1 1 d . . . . .
Np2 Np -0.04531(2) 0.70300(2) 0.78767(2) 0.01251(2) Uani 1 1 d . . . . .
O1 O 0.36294(10) 0.59412(13) 0.87759(6) 0.0127(3) Uani 1 1 d . . . . .
O2 O 0.40703(10) 0.30438(14) 0.83875(7) 0.0147(3) Uani 1 1 d . . . . .
O3 O 0.27430(10) 0.44542(14) 0.77500(6) 0.0124(3) Uani 1 1 d . . . . .
O4 O 0.49179(10) 0.41417(14) 0.94301(7) 0.0134(3) Uani 1 1 d . . . . .
O5 O 0.23973(10) 0.39399(15) 0.87847(7) 0.0160(3) Uani 1 1 d . . . . .
O6 O 0.33773(10) 0.38746(15) 0.95541(7) 0.0145(3) Uani 1 1 d . . . . .
O7 O 0.20697(11) 0.34439(16) 0.96568(7) 0.0190(4) Uani 1 1 d . . . . .
O8 O -0.07053(11) 0.72859(17) 0.71054(7) 0.0223(4) Uani 1 1 d . . . . .
O9 O -0.02162(12) 0.67659(16) 0.86476(7) 0.0233(4) Uani 1 1 d . . . . .
O10 O -0.17399(11) 0.58420(16) 0.78460(8) 0.0228(4) Uani 1 1 d . . . . .
O11 O -0.06124(11) 0.48888(16) 0.77235(8) 0.0240(4) Uani 1 1 d . . . . .
O12 O -0.17773(12) 0.39238(16) 0.77822(8) 0.0265(4) Uani 1 1 d . . . . .
O13 O 0.08738(11) 0.60821(15) 0.77187(8) 0.0213(4) Uani 1 1 d . . . . .
O14 O 0.09565(10) 0.79256(14) 0.79515(7) 0.0169(3) Uani 1 1 d . . . . .
O15 O 0.20978(11) 0.69773(17) 0.78171(9) 0.0269(4) Uani 1 1 d . . . . .
O16 O -0.04660(12) 0.91590(16) 0.80331(8) 0.0245(4) Uani 1 1 d . . . . .
O17 O -0.16435(11) 0.82555(16) 0.80814(8) 0.0229(4) Uani 1 1 d . . . . .
O18 O -0.15845(13) 1.01688(17) 0.81714(9) 0.0316(5) Uani 1 1 d . . . . .
N1 N 0.21167(12) 0.46443(16) 0.67876(8) 0.0113(4) Uani 1 1 d . . . . .
N2 N 0.41200(11) 0.55500(16) 0.76139(7) 0.0094(3) Uani 1 1 d . . . . .
N3 N 0.53622(11) 0.52449(16) 0.85285(8) 0.0098(4) Uani 1 1 d . . . . .
N4 N 0.62232(12) 0.34231(17) 0.97504(8) 0.0119(4) Uani 1 1 d . . . . .
N5 N 0.25921(12) 0.37399(16) 0.93480(8) 0.0134(4) Uani 1 1 d . . . . .
N6 N -0.13975(14) 0.48442(19) 0.77840(9) 0.0200(4) Uani 1 1 d . . . . .
N7 N 0.13459(13) 0.69893(18) 0.78281(9) 0.0174(4) Uani 1 1 d . . . . .
N8 N -0.12486(14) 0.92393(19) 0.80986(9) 0.0219(5) Uani 1 1 d . . . . .
C1 C 0.27415(14) 0.48848(19) 0.72380(9) 0.0103(4) Uani 1 1 d . . . . .
C2 C 0.34566(14) 0.56958(18) 0.71697(9) 0.0099(4) Uani 1 1 d . . . . .
C3 C 0.34425(15) 0.6582(2) 0.67469(10) 0.0137(4) Uani 1 1 d . . . . .
H3 H 0.295914 0.668919 0.644808 0.016 Uiso 1 1 calc R U . . .
C4 C 0.41393(15) 0.7309(2) 0.67643(10) 0.0155(5) Uani 1 1 d . . . . .
H4 H 0.413313 0.793600 0.648505 0.019 Uiso 1 1 calc R U . . .
C5 C 0.48444(15) 0.7115(2) 0.71911(10) 0.0132(4) Uani 1 1 d . . . . .
H5 H 0.534113 0.757770 0.719737 0.016 Uiso 1 1 calc R U . . .
C6 C 0.48110(14) 0.62261(19) 0.76122(9) 0.0105(4) Uani 1 1 d . . . . .
C7 C 0.55238(14) 0.60064(19) 0.81022(9) 0.0104(4) Uani 1 1 d . . . . .
C8 C 0.63018(14) 0.6562(2) 0.81287(9) 0.0129(4) Uani 1 1 d . . . . .
H8 H 0.640305 0.707942 0.781638 0.016 Uiso 1 1 calc R U . . .
C9 C 0.69291(14) 0.6356(2) 0.86138(10) 0.0137(4) Uani 1 1 d . . . . .
H9 H 0.745655 0.675656 0.864803 0.016 Uiso 1 1 calc R U . . .
C10 C 0.67765(14) 0.5556(2) 0.90499(9) 0.0130(4) Uani 1 1 d . . . . .
H10 H 0.719848 0.538936 0.938504 0.016 Uiso 1 1 calc R U . . .
C11 C 0.59924(14) 0.50070(19) 0.89839(9) 0.0115(4) Uani 1 1 d . . . . .
C12 C 0.56982(14) 0.41567(19) 0.94127(9) 0.0119(4) Uani 1 1 d . . . . .
C13 C 0.14139(14) 0.3865(2) 0.69076(10) 0.0161(5) Uani 1 1 d . . . . .
H13A H 0.139361 0.386521 0.734453 0.019 Uiso 1 1 calc R U . . .
H13B H 0.153529 0.305084 0.679010 0.019 Uiso 1 1 calc R U . . .
C14 C 0.05551(15) 0.4228(2) 0.65766(10) 0.0197(5) Uani 1 1 d . . . . .
H14A H 0.044156 0.504731 0.667426 0.030 Uiso 1 1 calc R U . . .
H14B H 0.011672 0.371845 0.669827 0.030 Uiso 1 1 calc R U . . .
H14C H 0.055086 0.415340 0.614286 0.030 Uiso 1 1 calc R U . . .
C15 C 0.22003(14) 0.48823(19) 0.61697(9) 0.0112(4) Uani 1 1 d . . . . .
C16 C 0.17057(15) 0.5751(2) 0.58513(10) 0.0140(4) Uani 1 1 d . . . . .
H16 H 0.128827 0.615672 0.602985 0.017 Uiso 1 1 calc R U . . .
C17 C 0.18284(15) 0.6016(2) 0.52731(10) 0.0153(5) Uani 1 1 d . . . . .
H17 H 0.148937 0.660721 0.505555 0.018 Uiso 1 1 calc R U . . .
C18 C 0.24380(15) 0.5436(2) 0.50008(10) 0.0149(4) Uani 1 1 d . . . . .
C19 C 0.29091(15) 0.4545(2) 0.53226(10) 0.0158(5) Uani 1 1 d . . . . .
H19 H 0.331545 0.412173 0.514116 0.019 Uiso 1 1 calc R U . . .
C20 C 0.27914(15) 0.4268(2) 0.59066(10) 0.0145(5) Uani 1 1 d . . . . .
H20 H 0.311594 0.366045 0.612196 0.017 Uiso 1 1 calc R U . . .
C21 C 0.25924(16) 0.5778(2) 0.43792(10) 0.0187(5) Uani 1 1 d . . . . .
H21A H 0.307980 0.532132 0.427941 0.022 Uiso 1 1 calc R U . . .
H21B H 0.274643 0.662188 0.438006 0.022 Uiso 1 1 calc R U . . .
C22 C 0.18301(16) 0.5568(2) 0.38934(10) 0.0216(5) Uani 1 1 d . . . . .
H22A H 0.170921 0.472310 0.386066 0.032 Uiso 1 1 calc R U . . .
H22B H 0.195486 0.586319 0.350790 0.032 Uiso 1 1 calc R U . . .
H22C H 0.133611 0.598328 0.399925 0.032 Uiso 1 1 calc R U . . .
C23 C 0.58348(14) 0.2562(2) 1.01219(9) 0.0136(4) Uani 1 1 d . . . . .
H23A H 0.537262 0.294694 1.029603 0.016 Uiso 1 1 calc R U . . .
H23B H 0.626638 0.228754 1.045672 0.016 Uiso 1 1 calc R U . . .
C24 C 0.54841(16) 0.1520(2) 0.97440(11) 0.0199(5) Uani 1 1 d . . . . .
H24A H 0.505764 0.179314 0.941242 0.030 Uiso 1 1 calc R U . . .
H24B H 0.522250 0.096562 0.999353 0.030 Uiso 1 1 calc R U . . .
H24C H 0.594521 0.112623 0.958142 0.030 Uiso 1 1 calc R U . . .
C25 C 0.71049(14) 0.32833(19) 0.97053(9) 0.0120(4) Uani 1 1 d . . . . .
C26 C 0.73474(16) 0.2863(2) 0.91797(10) 0.0174(5) Uani 1 1 d . . . . .
H26 H 0.693210 0.264257 0.884978 0.021 Uiso 1 1 calc R U . . .
C27 C 0.82009(17) 0.2770(2) 0.91412(11) 0.0223(5) Uani 1 1 d . . . . .
H27 H 0.836764 0.248114 0.878150 0.027 Uiso 1 1 calc R U . . .
C28 C 0.88214(16) 0.3090(2) 0.96195(11) 0.0220(5) Uani 1 1 d . . . . .
C29 C 0.85624(15) 0.3476(2) 1.01491(11) 0.0184(5) Uani 1 1 d . . . . .
H29 H 0.897635 0.368163 1.048277 0.022 Uiso 1 1 calc R U . . .
C30 C 0.77089(15) 0.3565(2) 1.01966(10) 0.0141(4) Uani 1 1 d . . . . .
H30 H 0.753941 0.381623 1.056211 0.017 Uiso 1 1 calc R U . . .
C31 C 0.97543(17) 0.2982(3) 0.95767(14) 0.0331(7) Uani 1 1 d . . . . .
H31A H 0.984629 0.322885 0.917050 0.040 Uiso 1 1 calc R U . . .
H31B H 1.007876 0.352330 0.987086 0.040 Uiso 1 1 calc R U . . .
C32 C 1.0091(2) 0.1751(3) 0.96934(19) 0.0522(10) Uani 1 1 d . . . . .
H32A H 1.001147 0.150539 1.009787 0.078 Uiso 1 1 calc R U . . .
H32B H 1.069554 0.173551 0.966183 0.078 Uiso 1 1 calc R U . . .
H32C H 0.978349 0.121296 0.939662 0.078 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
Np1 O1 1.7537(15) . ?
Np1 O2 1.7527(16) . ?
Np1 O3 2.3624(14) . ?
Np1 O4 2.3949(15) . ?
Np1 O5 2.5051(16) . ?
Np1 O6 2.5225(15) . ?
Np1 N2 2.5865(17) . ?
Np1 N3 2.5907(18) . ?
Np1 N5 2.9648(19) . ?
Np2 O8 1.7462(16) . ?
Np2 O9 1.7454(16) . ?
Np2 O10 2.4509(18) . ?
Np2 O11 2.4651(18) . ?
Np2 O13 2.4520(17) . ?
Np2 O14 2.4525(17) . ?
Np2 O16 2.4454(18) . ?
Np2 O17 2.4574(18) . ?
Np2 N6 2.897(2) . ?
Np2 N7 2.893(2) . ?
Np2 N8 2.892(2) . ?
O3 C1 1.253(3) . ?
O4 C12 1.253(3) . ?
O5 N5 1.279(2) . ?
O6 N5 1.277(2) . ?
O7 N5 1.214(2) . ?
O10 N6 1.276(3) . ?
O11 N6 1.283(3) . ?
O12 N6 1.209(3) . ?
O13 N7 1.278(3) . ?
O14 N7 1.285(2) . ?
O15 N7 1.205(3) . ?
O16 N8 1.284(3) . ?
O17 N8 1.281(3) . ?
O18 N8 1.207(3) . ?
N1 C1 1.336(3) . ?
N1 C13 1.487(3) . ?
N1 C15 1.445(3) . ?
N2 C2 1.350(3) . ?
N2 C6 1.345(3) . ?
N3 C7 1.347(3) . ?
N3 C11 1.348(3) . ?
N4 C12 1.334(3) . ?
N4 C23 1.485(3) . ?
N4 C25 1.436(3) . ?
C1 C2 1.494(3) . ?
C2 C3 1.384(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.381(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.380(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(3) . ?
C6 C7 1.479(3) . ?
C7 C8 1.387(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.383(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.388(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.386(3) . ?
C11 C12 1.493(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.513(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.392(3) . ?
C15 C20 1.380(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.381(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.394(3) . ?
C18 C19 1.396(3) . ?
C18 C21 1.510(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.394(3) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.524(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.514(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.387(3) . ?
C25 C30 1.388(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.383(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.394(4) . ?
C28 C29 1.393(4) . ?
C28 C31 1.513(4) . ?
C29 H29 0.9500 . ?
C29 C30 1.387(3) . ?
C30 H30 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.506(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 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
O1 Np1 O3 93.67(6) . . ?
O1 Np1 O4 95.71(6) . . ?
O1 Np1 O5 88.08(7) . . ?
O1 Np1 O6 86.97(6) . . ?
O1 Np1 N2 80.74(6) . . ?
O1 Np1 N3 85.51(7) . . ?
O1 Np1 N5 87.03(6) . . ?
O2 Np1 O1 179.45(7) . . ?
O2 Np1 O3 86.73(6) . . ?
O2 Np1 O4 83.93(6) . . ?
O2 Np1 O5 92.44(7) . . ?
O2 Np1 O6 93.22(6) . . ?
O2 Np1 N2 99.11(6) . . ?
O2 Np1 N3 93.96(7) . . ?
O2 Np1 N5 93.36(6) . . ?
O3 Np1 O4 169.35(6) . . ?
O3 Np1 O5 63.00(5) . . ?
O3 Np1 O6 113.55(5) . . ?
O3 Np1 N2 62.83(5) . . ?
O3 Np1 N3 123.81(5) . . ?
O3 Np1 N5 88.29(5) . . ?
O4 Np1 O5 112.25(5) . . ?
O4 Np1 O6 62.06(5) . . ?
O4 Np1 N2 123.77(5) . . ?
O4 Np1 N3 62.15(5) . . ?
O4 Np1 N5 87.18(5) . . ?
O5 Np1 O6 50.61(5) . . ?
O5 Np1 N2 123.58(5) . . ?
O5 Np1 N3 170.92(5) . . ?
O5 Np1 N5 25.30(5) . . ?
O6 Np1 N2 166.79(5) . . ?
O6 Np1 N3 122.47(5) . . ?
O6 Np1 N5 25.30(5) . . ?
N2 Np1 N3 61.63(5) . . ?
N2 Np1 N5 147.51(5) . . ?
N3 Np1 N5 147.41(5) . . ?
O8 Np2 O9 179.15(8) . . ?
O8 Np2 O10 90.06(7) . . ?
O8 Np2 O11 91.27(8) . . ?
O8 Np2 O13 89.98(7) . . ?
O8 Np2 O14 93.82(7) . . ?
O8 Np2 O16 88.45(8) . . ?
O8 Np2 O17 91.54(7) . . ?
O8 Np2 N6 91.95(7) . . ?
O8 Np2 N7 92.40(7) . . ?
O8 Np2 N8 89.31(7) . . ?
O9 Np2 O10 89.11(8) . . ?
O9 Np2 O11 88.36(7) . . ?
O9 Np2 O13 90.59(7) . . ?
O9 Np2 O14 87.03(7) . . ?
O9 Np2 O16 91.83(7) . . ?
O9 Np2 O17 87.99(7) . . ?
O9 Np2 N6 87.38(7) . . ?
O9 Np2 N7 88.39(7) . . ?
O9 Np2 N8 90.59(7) . . ?
O10 Np2 O11 52.01(6) . . ?
O10 Np2 O13 119.59(6) . . ?
O10 Np2 O14 170.86(6) . . ?
O10 Np2 O17 69.37(6) . . ?
O10 Np2 N6 25.93(6) . . ?
O10 Np2 N7 145.45(6) . . ?
O10 Np2 N8 95.40(6) . . ?
O11 Np2 N6 26.14(6) . . ?
O11 Np2 N7 93.47(6) . . ?
O11 Np2 N8 147.40(6) . . ?
O13 Np2 O11 67.59(6) . . ?
O13 Np2 O14 52.22(5) . . ?
O13 Np2 O17 170.92(6) . . ?
O13 Np2 N6 93.73(6) . . ?
O13 Np2 N7 26.04(5) . . ?
O13 Np2 N8 145.00(6) . . ?
O14 Np2 O11 119.53(6) . . ?
O14 Np2 O17 118.72(6) . . ?
O14 Np2 N6 145.38(6) . . ?
O14 Np2 N7 26.19(5) . . ?
O14 Np2 N8 92.93(6) . . ?
O16 Np2 O10 121.55(6) . . ?
O16 Np2 O11 173.56(6) . . ?
O16 Np2 O13 118.84(6) . . ?
O16 Np2 O14 66.90(6) . . ?
O16 Np2 O17 52.28(6) . . ?
O16 Np2 N6 147.43(6) . . ?
O16 Np2 N7 92.98(6) . . ?
O16 Np2 N8 26.17(6) . . ?
O17 Np2 O11 121.31(6) . . ?
O17 Np2 N6 95.17(6) . . ?
O17 Np2 N7 144.90(6) . . ?
O17 Np2 N8 26.13(6) . . ?
N7 Np2 N6 119.52(6) . . ?
N8 Np2 N6 121.27(6) . . ?
N8 Np2 N7 119.08(6) . . ?
C1 O3 Np1 128.15(14) . . ?
C12 O4 Np1 124.38(13) . . ?
N5 O5 Np1 97.87(12) . . ?
N5 O6 Np1 97.10(11) . . ?
N6 O10 Np2 96.94(13) . . ?
N6 O11 Np2 96.05(14) . . ?
N7 O13 Np2 96.61(13) . . ?
N7 O14 Np2 96.41(13) . . ?
N8 O16 Np2 96.72(14) . . ?
N8 O17 Np2 96.24(13) . . ?
C1 N1 C13 118.64(18) . . ?
C1 N1 C15 121.58(19) . . ?
C15 N1 C13 118.17(17) . . ?
C2 N2 Np1 117.73(14) . . ?
C6 N2 Np1 121.01(13) . . ?
C6 N2 C2 118.53(18) . . ?
C7 N3 Np1 121.96(14) . . ?
C11 N3 Np1 119.47(14) . . ?
C11 N3 C7 117.92(19) . . ?
C12 N4 C23 116.93(19) . . ?
C12 N4 C25 124.41(19) . . ?
C25 N4 C23 117.85(18) . . ?
O5 N5 Np1 56.82(10) . . ?
O6 N5 Np1 57.60(10) . . ?
O6 N5 O5 114.42(18) . . ?
O7 N5 Np1 178.97(16) . . ?
O7 N5 O5 122.34(19) . . ?
O7 N5 O6 123.24(18) . . ?
O10 N6 Np2 57.13(11) . . ?
O10 N6 O11 114.8(2) . . ?
O11 N6 Np2 57.81(12) . . ?
O12 N6 Np2 176.06(16) . . ?
O12 N6 O10 123.1(2) . . ?
O12 N6 O11 122.1(2) . . ?
O13 N7 Np2 57.35(11) . . ?
O13 N7 O14 114.75(18) . . ?
O14 N7 Np2 57.41(11) . . ?
O15 N7 Np2 178.98(17) . . ?
O15 N7 O13 123.1(2) . . ?
O15 N7 O14 122.1(2) . . ?
O16 N8 Np2 57.11(12) . . ?
O17 N8 Np2 57.64(11) . . ?
O17 N8 O16 114.7(2) . . ?
O18 N8 Np2 177.87(17) . . ?
O18 N8 O16 122.6(2) . . ?
O18 N8 O17 122.7(2) . . ?
O3 C1 N1 120.9(2) . . ?
O3 C1 C2 116.35(18) . . ?
N1 C1 C2 122.71(19) . . ?
N2 C2 C1 111.86(18) . . ?
N2 C2 C3 121.8(2) . . ?
C3 C2 C1 126.07(19) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 C2 119.2(2) . . ?
C4 C3 H3 120.4 . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.4(2) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5 120.8 . . ?
C4 C5 C6 118.5(2) . . ?
C6 C5 H5 120.8 . . ?
N2 C6 C5 122.3(2) . . ?
N2 C6 C7 115.99(18) . . ?
C5 C6 C7 121.6(2) . . ?
N3 C7 C6 115.48(19) . . ?
N3 C7 C8 122.10(19) . . ?
C8 C7 C6 122.41(19) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 C7 119.4(2) . . ?
C9 C8 H8 120.3 . . ?
C8 C9 H9 120.5 . . ?
C8 C9 C10 119.0(2) . . ?
C10 C9 H9 120.5 . . ?
C9 C10 H10 120.9 . . ?
C11 C10 C9 118.3(2) . . ?
C11 C10 H10 120.9 . . ?
N3 C11 C10 123.1(2) . . ?
N3 C11 C12 110.45(19) . . ?
C10 C11 C12 126.28(19) . . ?
O4 C12 N4 120.9(2) . . ?
O4 C12 C11 116.33(19) . . ?
N4 C12 C11 122.7(2) . . ?
N1 C13 H13A 108.8 . . ?
N1 C13 H13B 108.8 . . ?
N1 C13 C14 113.59(19) . . ?
H13A C13 H13B 107.7 . . ?
C14 C13 H13A 108.8 . . ?
C14 C13 H13B 108.8 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 N1 120.0(2) . . ?
C20 C15 N1 119.42(19) . . ?
C20 C15 C16 120.6(2) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 C15 119.3(2) . . ?
C17 C16 H16 120.4 . . ?
C16 C17 H17 119.2 . . ?
C16 C17 C18 121.6(2) . . ?
C18 C17 H17 119.2 . . ?
C17 C18 C19 118.1(2) . . ?
C17 C18 C21 120.8(2) . . ?
C19 C18 C21 121.1(2) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 C18 120.9(2) . . ?
C20 C19 H19 119.5 . . ?
C15 C20 C19 119.5(2) . . ?
C15 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C18 C21 H21A 108.9 . . ?
C18 C21 H21B 108.9 . . ?
C18 C21 C22 113.5(2) . . ?
H21A C21 H21B 107.7 . . ?
C22 C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N4 C23 H23A 109.6 . . ?
N4 C23 H23B 109.6 . . ?
N4 C23 C24 110.42(18) . . ?
H23A C23 H23B 108.1 . . ?
C24 C23 H23A 109.6 . . ?
C24 C23 H23B 109.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 N4 120.37(19) . . ?
C26 C25 C30 120.6(2) . . ?
C30 C25 N4 119.1(2) . . ?
C25 C26 H26 120.4 . . ?
C27 C26 C25 119.3(2) . . ?
C27 C26 H26 120.4 . . ?
C26 C27 H27 119.3 . . ?
C26 C27 C28 121.4(2) . . ?
C28 C27 H27 119.3 . . ?
C27 C28 C31 121.2(2) . . ?
C29 C28 C27 118.3(2) . . ?
C29 C28 C31 120.4(2) . . ?
C28 C29 H29 119.5 . . ?
C30 C29 C28 121.0(2) . . ?
C30 C29 H29 119.5 . . ?
C25 C30 H30 120.3 . . ?
C29 C30 C25 119.4(2) . . ?
C29 C30 H30 120.3 . . ?
C28 C31 H31A 109.0 . . ?
C28 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
C32 C31 C28 113.1(3) . . ?
C32 C31 H31A 109.0 . . ?
C32 C31 H31B 109.0 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 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
Np1 O3 C1 N1 170.07(15) . . . . ?
Np1 O3 C1 C2 -11.6(3) . . . . ?
Np1 O4 C12 N4 -144.66(16) . . . . ?
Np1 O4 C12 C11 33.6(3) . . . . ?
Np1 O5 N5 O6 -0.91(19) . . . . ?
Np1 O5 N5 O7 179.27(18) . . . . ?
Np1 O6 N5 O5 0.90(19) . . . . ?
Np1 O6 N5 O7 -179.28(18) . . . . ?
Np1 N2 C2 C1 -18.3(2) . . . . ?
Np1 N2 C2 C3 155.90(17) . . . . ?
Np1 N2 C6 C5 -156.82(16) . . . . ?
Np1 N2 C6 C7 20.5(2) . . . . ?
Np1 N3 C7 C6 -9.7(2) . . . . ?
Np1 N3 C7 C8 169.09(16) . . . . ?
Np1 N3 C11 C10 -167.21(17) . . . . ?
Np1 N3 C11 C12 8.7(2) . . . . ?
Np2 O10 N6 O11 -4.6(2) . . . . ?
Np2 O10 N6 O12 175.31(19) . . . . ?
Np2 O11 N6 O10 4.6(2) . . . . ?
Np2 O11 N6 O12 -175.35(19) . . . . ?
Np2 O13 N7 O14 -1.11(19) . . . . ?
Np2 O13 N7 O15 178.9(2) . . . . ?
Np2 O14 N7 O13 1.10(19) . . . . ?
Np2 O14 N7 O15 -178.9(2) . . . . ?
Np2 O16 N8 O17 2.6(2) . . . . ?
Np2 O16 N8 O18 -177.5(2) . . . . ?
Np2 O17 N8 O16 -2.6(2) . . . . ?
Np2 O17 N8 O18 177.5(2) . . . . ?
O3 C1 C2 N2 19.3(3) . . . . ?
O3 C1 C2 C3 -154.6(2) . . . . ?
N1 C1 C2 N2 -162.4(2) . . . . ?
N1 C1 C2 C3 23.7(3) . . . . ?
N1 C15 C16 C17 176.2(2) . . . . ?
N1 C15 C20 C19 -176.2(2) . . . . ?
N2 C2 C3 C4 2.6(3) . . . . ?
N2 C6 C7 N3 -6.9(3) . . . . ?
N2 C6 C7 C8 174.3(2) . . . . ?
N3 C7 C8 C9 -1.6(3) . . . . ?
N3 C11 C12 O4 -25.7(3) . . . . ?
N3 C11 C12 N4 152.5(2) . . . . ?
N4 C25 C26 C27 178.1(2) . . . . ?
N4 C25 C30 C29 -177.5(2) . . . . ?
C1 N1 C13 C14 142.7(2) . . . . ?
C1 N1 C15 C16 -112.5(2) . . . . ?
C1 N1 C15 C20 65.5(3) . . . . ?
C1 C2 C3 C4 176.0(2) . . . . ?
C2 N2 C6 C5 4.0(3) . . . . ?
C2 N2 C6 C7 -178.64(18) . . . . ?
C2 C3 C4 C5 1.9(3) . . . . ?
C3 C4 C5 C6 -3.4(3) . . . . ?
C4 C5 C6 N2 0.4(3) . . . . ?
C4 C5 C6 C7 -176.8(2) . . . . ?
C5 C6 C7 N3 170.4(2) . . . . ?
C5 C6 C7 C8 -8.4(3) . . . . ?
C6 N2 C2 C1 -179.76(18) . . . . ?
C6 N2 C2 C3 -5.6(3) . . . . ?
C6 C7 C8 C9 177.1(2) . . . . ?
C7 N3 C11 C10 3.7(3) . . . . ?
C7 N3 C11 C12 179.65(18) . . . . ?
C7 C8 C9 C10 2.8(3) . . . . ?
C8 C9 C10 C11 -0.9(3) . . . . ?
C9 C10 C11 N3 -2.5(3) . . . . ?
C9 C10 C11 C12 -177.8(2) . . . . ?
C10 C11 C12 O4 150.1(2) . . . . ?
C10 C11 C12 N4 -31.7(3) . . . . ?
C11 N3 C7 C6 179.57(19) . . . . ?
C11 N3 C7 C8 -1.6(3) . . . . ?
C12 N4 C23 C24 80.7(2) . . . . ?
C12 N4 C25 C26 -63.0(3) . . . . ?
C12 N4 C25 C30 117.6(2) . . . . ?
C13 N1 C1 O3 0.8(3) . . . . ?
C13 N1 C1 C2 -177.4(2) . . . . ?
C13 N1 C15 C16 82.2(3) . . . . ?
C13 N1 C15 C20 -99.8(2) . . . . ?
C15 N1 C1 O3 -164.5(2) . . . . ?
C15 N1 C1 C2 17.3(3) . . . . ?
C15 N1 C13 C14 -51.5(3) . . . . ?
C15 C16 C17 C18 -0.2(3) . . . . ?
C16 C15 C20 C19 1.8(3) . . . . ?
C16 C17 C18 C19 2.0(3) . . . . ?
C16 C17 C18 C21 -177.0(2) . . . . ?
C17 C18 C19 C20 -2.0(3) . . . . ?
C17 C18 C21 C22 -63.7(3) . . . . ?
C18 C19 C20 C15 0.1(3) . . . . ?
C19 C18 C21 C22 117.3(3) . . . . ?
C20 C15 C16 C17 -1.8(3) . . . . ?
C21 C18 C19 C20 177.1(2) . . . . ?
C23 N4 C12 O4 2.7(3) . . . . ?
C23 N4 C12 C11 -175.40(19) . . . . ?
C23 N4 C25 C26 106.4(2) . . . . ?
C23 N4 C25 C30 -73.1(3) . . . . ?
C25 N4 C12 O4 172.1(2) . . . . ?
C25 N4 C12 C11 -6.0(3) . . . . ?
C25 N4 C23 C24 -89.4(2) . . . . ?
C25 C26 C27 C28 -0.1(4) . . . . ?
C26 C25 C30 C29 3.0(3) . . . . ?
C26 C27 C28 C29 1.9(4) . . . . ?
C26 C27 C28 C31 179.8(2) . . . . ?
C27 C28 C29 C30 -1.3(4) . . . . ?
C27 C28 C31 C32 -81.3(3) . . . . ?
C28 C29 C30 C25 -1.1(4) . . . . ?
C29 C28 C31 C32 96.5(3) . . . . ?
C30 C25 C26 C27 -2.5(3) . . . . ?
C31 C28 C29 C30 -179.2(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT910_NpNDip91_LT         
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 20 Note 
RESPONSE: Closed by beamstop.
;
####################################################################### 
# 
# 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_th3_0m
_database_code_depnum_ccdc_archive 'CCDC 2395348'
loop_
_audit_author_name
_audit_author_address
'Paulina Kalle'
;IGIC RAS
Russia
;
_audit_update_record             
;
2024-11-01 deposited with the CCDC.	2025-02-05 downloaded from the CCDC.
;
_audit_creation_date             2024-09-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H34 N8 O14 Th'
_chemical_formula_sum            'C32 H34 N8 O14 Th'
_chemical_formula_weight         986.71
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   51.304(4)
_cell_length_b                   8.5529(7)
_cell_length_c                   17.5571(14)
_cell_angle_alpha                90
_cell_angle_beta                 101.537(3)
_cell_angle_gamma                90
_cell_volume                     7548.3(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.510
_cell_measurement_theta_min      2.588
_shelx_estimated_absorpt_T_max   0.739
_shelx_estimated_absorpt_T_min   0.296
_exptl_absorpt_coefficient_mu    4.028
_exptl_absorpt_correction_T_max  0.4942
_exptl_absorpt_correction_T_min  0.2093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1636 before and 0.0806 after correction.
The Ratio of minimum to maximum transmission is 0.4235.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       65
_diffrn_reflns_limit_h_min       -65
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56261
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.995
_diffrn_reflns_theta_min         2.344
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6745
_reflns_number_total             8225
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.753
_refine_diff_density_min         -1.584
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         8225
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0330
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0254P)²+36.0115P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0763
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29A-C26 = C29-C26
 1.5 with sigma of 0.02
 C30A-C29A = C30-C29
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C29) = Uanis(C30) = Uanis(C29A) = Uanis(C30A)
4. Rigid body (RIGU) restrains
 C29, C30
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: C29(0.5) H29A(0.5) H29B(0.5) C30(0.5) H30A(0.5) H30B(0.5)
 H30C(0.5) C29A(0.5) H29C(0.5) H29D(0.5) C30A(0.5) H30D(0.5) H30E(0.5) H30F(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C20(H20A,H20B), C29(H29A,H29B), C31(H31A,H31B), C29A(H29C,H29D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C16(H16),
 C17(H17), C24(H24), C25(H25), C27(H27), C28(H28)
6.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C), C30A(H30D,H30E,H30F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Th1 Th 0.37078(2) 0.73480(2) 0.49353(2) 0.01402(5) Uani 1 1 d . . . . .
O1 O 0.35073(6) 0.9756(3) 0.52796(17) 0.0191(7) Uani 1 1 d . . . . .
O2 O 0.39012(6) 0.4924(3) 0.45458(17) 0.0192(7) Uani 1 1 d . . . . .
O3 O 0.31944(6) 0.7181(3) 0.48236(17) 0.0186(7) Uani 1 1 d . . . . .
O4 O 0.34003(6) 0.4998(3) 0.51486(17) 0.0187(7) Uani 1 1 d . . . . .
O5 O 0.29836(6) 0.5255(4) 0.5256(2) 0.0255(7) Uani 1 1 d . . . . .
O6 O 0.34272(6) 0.8653(3) 0.36873(18) 0.0225(7) Uani 1 1 d . . . . .
O7 O 0.34731(6) 0.6150(3) 0.36509(16) 0.0179(7) Uani 1 1 d . . . . .
O8 O 0.32772(7) 0.7390(4) 0.26095(18) 0.0304(8) Uani 1 1 d . . . . .
O9 O 0.39543(6) 0.7841(3) 0.38112(17) 0.0204(7) Uani 1 1 d . . . . .
O10 O 0.39263(6) 0.9859(3) 0.45292(17) 0.0224(7) Uani 1 1 d . . . . .
O11 O 0.41131(8) 1.0079(4) 0.3523(2) 0.0365(9) Uani 1 1 d . . . . .
O12 O 0.42224(6) 0.7248(3) 0.53273(17) 0.0200(7) Uani 1 1 d . . . . .
O13 O 0.40338(6) 0.8607(3) 0.61047(18) 0.0220(7) Uani 1 1 d . . . . .
O14 O 0.44605(7) 0.8140(5) 0.6405(2) 0.0458(10) Uani 1 1 d . . . . .
N1 N 0.35546(7) 0.7486(4) 0.62984(19) 0.0149(7) Uani 1 1 d . . . . .
N2 N 0.38878(7) 0.5213(4) 0.60278(19) 0.0151(7) Uani 1 1 d . . . . .
N3 N 0.31172(7) 1.0571(4) 0.5542(2) 0.0189(8) Uani 1 1 d . . . . .
N4 N 0.42783(7) 0.3511(4) 0.4786(2) 0.0190(8) Uani 1 1 d . . . . .
N5 N 0.31845(7) 0.5781(4) 0.5077(2) 0.0167(8) Uani 1 1 d . . . . .
N6 N 0.33882(7) 0.7402(4) 0.3290(2) 0.0186(8) Uani 1 1 d . . . . .
N7 N 0.40017(8) 0.9288(4) 0.3938(2) 0.0226(9) Uani 1 1 d . . . . .
N8 N 0.42464(8) 0.8012(5) 0.5962(2) 0.0245(9) Uani 1 1 d . . . . .
C1 C 0.34022(9) 0.8698(5) 0.6418(2) 0.0164(9) Uani 1 1 d . . . . .
C2 C 0.33426(9) 0.9037(5) 0.7134(3) 0.0199(10) Uani 1 1 d . . . . .
H2 H 0.323602 0.991527 0.720134 0.024 Uiso 1 1 calc R U . . .
C3 C 0.34438(9) 0.8050(5) 0.7753(3) 0.0228(10) Uani 1 1 d . . . . .
H3 H 0.340833 0.824964 0.825517 0.027 Uiso 1 1 calc R U . . .
C4 C 0.35962(9) 0.6778(5) 0.7631(3) 0.0220(10) Uani 1 1 d . . . . .
H4 H 0.366474 0.608933 0.804793 0.026 Uiso 1 1 calc R U . . .
C5 C 0.36488(9) 0.6512(5) 0.6894(2) 0.0162(9) Uani 1 1 d . . . . .
C6 C 0.38121(9) 0.5171(5) 0.6718(2) 0.0174(9) Uani 1 1 d . . . . .
C7 C 0.38725(9) 0.3904(5) 0.7221(3) 0.0224(10) Uani 1 1 d . . . . .
H7 H 0.381982 0.390284 0.771013 0.027 Uiso 1 1 calc R U . . .
C8 C 0.40094(10) 0.2655(5) 0.7001(3) 0.0267(11) Uani 1 1 d . . . . .
H8 H 0.405321 0.178437 0.733800 0.032 Uiso 1 1 calc R U . . .
C9 C 0.40831(9) 0.2674(5) 0.6283(3) 0.0235(10) Uani 1 1 d . . . . .
H9 H 0.417098 0.180407 0.611185 0.028 Uiso 1 1 calc R U . . .
C10 C 0.40254(8) 0.3995(5) 0.5822(2) 0.0175(9) Uani 1 1 d . . . . .
C11 C 0.33360(9) 0.9730(4) 0.5710(2) 0.0152(9) Uani 1 1 d . . . . .
C12 C 0.28905(9) 1.0368(5) 0.5907(3) 0.0184(9) Uani 1 1 d . . . . .
C13 C 0.27507(9) 0.8974(5) 0.5818(3) 0.0206(10) Uani 1 1 d . . . . .
H13 H 0.280799 0.812845 0.554150 0.025 Uiso 1 1 calc R U . . .
C14 C 0.25274(10) 0.8833(5) 0.6136(3) 0.0247(11) Uani 1 1 d . . . . .
H14 H 0.243186 0.787422 0.607567 0.030 Uiso 1 1 calc R U . . .
C15 C 0.24367(9) 1.0047(5) 0.6544(3) 0.0220(10) Uani 1 1 d . . . . .
C16 C 0.25844(9) 1.1435(5) 0.6626(3) 0.0228(10) Uani 1 1 d . . . . .
H16 H 0.253058 1.227561 0.691324 0.027 Uiso 1 1 calc R U . . .
C17 C 0.28063(9) 1.1612(5) 0.6300(3) 0.0228(10) Uani 1 1 d . . . . .
H17 H 0.290006 1.257598 0.634536 0.027 Uiso 1 1 calc R U . . .
C18 C 0.21849(9) 0.9870(6) 0.6857(3) 0.0268(11) Uani 1 1 d . . . . .
H18A H 0.214814 0.874080 0.689971 0.032 Uiso 1 1 calc R U . . .
H18B H 0.203586 1.032226 0.647443 0.032 Uiso 1 1 calc R U . . .
C19 C 0.21871(10) 1.0628(6) 0.7643(3) 0.0284(11) Uani 1 1 d . . . . .
H19A H 0.220240 1.176429 0.759702 0.043 Uiso 1 1 calc R U . . .
H19B H 0.233876 1.023174 0.802461 0.043 Uiso 1 1 calc R U . . .
H19C H 0.202145 1.037448 0.781379 0.043 Uiso 1 1 calc R U . . .
C20 C 0.30709(9) 1.1549(5) 0.4827(3) 0.0235(10) Uani 1 1 d . . . . .
H20A H 0.324431 1.186941 0.471084 0.028 Uiso 1 1 calc R U . . .
H20B H 0.297328 1.250770 0.491733 0.028 Uiso 1 1 calc R U . . .
C21 C 0.29125(10) 1.0672(6) 0.4134(3) 0.0308(12) Uani 1 1 d . . . . .
H21A H 0.288909 1.133996 0.367111 0.046 Uiso 1 1 calc R U . . .
H21B H 0.273785 1.039141 0.423833 0.046 Uiso 1 1 calc R U . . .
H21C H 0.300835 0.972055 0.404395 0.046 Uiso 1 1 calc R U . . .
C22 C 0.40717(8) 0.4152(5) 0.5009(2) 0.0155(9) Uani 1 1 d . . . . .
C23 C 0.45067(9) 0.2879(5) 0.5307(3) 0.0219(10) Uani 1 1 d . . . . .
C24 C 0.46646(10) 0.3831(6) 0.5847(3) 0.0317(12) Uani 1 1 d . . . . .
H24 H 0.461981 0.489976 0.589426 0.038 Uiso 1 1 calc R U . . .
C25 C 0.48887(11) 0.3205(8) 0.6317(3) 0.0426(15) Uani 1 1 d . . . . .
H25 H 0.499387 0.384929 0.670045 0.051 Uiso 1 1 calc R U . . .
C26 C 0.49643(12) 0.1669(8) 0.6246(3) 0.0475(16) Uani 1 1 d D . . . .
C27 C 0.48030(11) 0.0734(7) 0.5697(3) 0.0401(14) Uani 1 1 d . . . . .
H27 H 0.484993 -0.032916 0.564377 0.048 Uiso 1 1 calc R U . . .
C28 C 0.45745(10) 0.1327(6) 0.5224(3) 0.0288(11) Uani 1 1 d . . . . .
H28 H 0.446633 0.067823 0.484936 0.035 Uiso 1 1 calc R U . . .
C29 C 0.5202(4) 0.088(3) 0.6803(12) 0.058(4) Uani 0.5 1 d D . P A 1
H29A H 0.537003 0.131957 0.669998 0.069 Uiso 0.5 1 calc R U P A 1
H29B H 0.519230 0.114241 0.734566 0.069 Uiso 0.5 1 calc R U P A 1
C30 C 0.5212(4) -0.091(3) 0.6727(12) 0.058(4) Uani 0.5 1 d D . P A 1
H30A H 0.522172 -0.118766 0.619243 0.087 Uiso 0.5 1 calc R U P A 1
H30B H 0.505096 -0.136638 0.685699 0.087 Uiso 0.5 1 calc R U P A 1
H30C H 0.536888 -0.131515 0.708433 0.087 Uiso 0.5 1 calc R U P A 1
C31 C 0.43023(10) 0.3649(6) 0.3961(3) 0.0258(11) Uani 1 1 d . . . . .
H31A H 0.412282 0.376415 0.363132 0.031 Uiso 1 1 calc R U . . .
H31B H 0.438257 0.268074 0.380164 0.031 Uiso 1 1 calc R U . . .
C32 C 0.44715(12) 0.5034(7) 0.3835(3) 0.0422(14) Uani 1 1 d . . . . .
H32A H 0.448794 0.507087 0.328864 0.063 Uiso 1 1 calc R U . . .
H32B H 0.464860 0.493029 0.416647 0.063 Uiso 1 1 calc R U . . .
H32C H 0.438780 0.599915 0.396777 0.063 Uiso 1 1 calc R U . . .
C29A C 0.5238(4) 0.126(3) 0.6695(12) 0.058(4) Uani 0.5 1 d D . P A 2
H29C H 0.537167 0.162929 0.640001 0.069 Uiso 0.5 1 calc R U P A 2
H29D H 0.526984 0.181872 0.719762 0.069 Uiso 0.5 1 calc R U P A 2
C30A C 0.5282(3) -0.047(3) 0.6853(12) 0.058(4) Uani 0.5 1 d D . P A 2
H30D H 0.529791 -0.100252 0.637124 0.087 Uiso 0.5 1 calc R U P A 2
H30E H 0.513041 -0.089742 0.704681 0.087 Uiso 0.5 1 calc R U P A 2
H30F H 0.544521 -0.061913 0.724352 0.087 Uiso 0.5 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Th1 O1 2.432(3) . ?
Th1 O2 2.454(3) . ?
Th1 O3 2.605(3) . ?
Th1 O4 2.628(3) . ?
Th1 O6 2.618(3) . ?
Th1 O7 2.549(3) . ?
Th1 O9 2.583(3) . ?
Th1 O10 2.588(3) . ?
Th1 O12 2.593(3) . ?
Th1 O13 2.607(3) . ?
Th1 N1 2.667(3) . ?
Th1 N2 2.676(3) . ?
O1 C11 1.268(5) . ?
O2 C22 1.256(5) . ?
O3 N5 1.282(4) . ?
O4 N5 1.278(4) . ?
O5 N5 1.221(5) . ?
O6 N6 1.271(4) . ?
O7 N6 1.276(4) . ?
O8 N6 1.216(5) . ?
O9 N7 1.272(4) . ?
O10 N7 1.276(5) . ?
O11 N7 1.216(5) . ?
O12 N8 1.277(5) . ?
O13 N8 1.273(5) . ?
O14 N8 1.217(5) . ?
N1 C1 1.340(5) . ?
N1 C5 1.349(5) . ?
N2 C6 1.344(5) . ?
N2 C10 1.347(5) . ?
N3 C11 1.317(5) . ?
N3 C12 1.447(6) . ?
N3 C20 1.488(5) . ?
N4 C22 1.320(5) . ?
N4 C23 1.439(5) . ?
N4 C31 1.483(6) . ?
C1 C2 1.383(6) . ?
C1 C11 1.506(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.392(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.381(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.393(6) . ?
C5 C6 1.489(6) . ?
C6 C7 1.393(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.377(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.385(7) . ?
C9 H9 0.9500 . ?
C9 C10 1.388(6) . ?
C10 C22 1.499(6) . ?
C12 C13 1.384(6) . ?
C12 C17 1.383(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.377(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.393(6) . ?
C15 C16 1.400(6) . ?
C15 C18 1.510(7) . ?
C16 H16 0.9500 . ?
C16 C17 1.381(7) . ?
C17 H17 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.522(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.519(7) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C23 C24 1.383(7) . ?
C23 C28 1.387(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.382(7) . ?
C25 H25 0.9500 . ?
C25 C26 1.383(9) . ?
C26 C27 1.391(9) . ?
C26 C29 1.558(14) . ?
C26 C29A 1.510(15) . ?
C27 H27 0.9500 . ?
C27 C28 1.389(7) . ?
C28 H28 0.9500 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.536(16) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.511(7) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C29A H29C 0.9900 . ?
C29A H29D 0.9900 . ?
C29A C30A 1.507(15) . ?
C30A H30D 0.9800 . ?
C30A H30E 0.9800 . ?
C30A H30F 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
O1 Th1 O2 178.16(10) . . ?
O1 Th1 O3 66.02(9) . . ?
O1 Th1 O4 108.45(10) . . ?
O1 Th1 O6 70.00(10) . . ?
O1 Th1 O7 114.33(10) . . ?
O1 Th1 O9 110.35(10) . . ?
O1 Th1 O10 66.03(10) . . ?
O1 Th1 O12 114.89(10) . . ?
O1 Th1 O13 72.02(10) . . ?
O1 Th1 N1 61.58(10) . . ?
O1 Th1 N2 120.16(10) . . ?
O2 Th1 O3 113.07(9) . . ?
O2 Th1 O4 71.42(10) . . ?
O2 Th1 O6 108.19(10) . . ?
O2 Th1 O7 63.87(9) . . ?
O2 Th1 O9 68.77(9) . . ?
O2 Th1 O10 113.75(10) . . ?
O2 Th1 O12 66.36(10) . . ?
O2 Th1 O13 109.67(10) . . ?
O2 Th1 N1 119.72(10) . . ?
O2 Th1 N2 61.46(10) . . ?
O3 Th1 O4 48.87(9) . . ?
O3 Th1 O6 65.31(10) . . ?
O3 Th1 O13 124.16(10) . . ?
O3 Th1 N1 66.11(10) . . ?
O3 Th1 N2 102.44(10) . . ?
O4 Th1 N1 67.22(9) . . ?
O4 Th1 N2 60.44(10) . . ?
O6 Th1 O4 101.54(9) . . ?
O6 Th1 N1 121.38(10) . . ?
O6 Th1 N2 160.73(10) . . ?
O7 Th1 O3 67.67(9) . . ?
O7 Th1 O4 68.16(9) . . ?
O7 Th1 O6 49.29(9) . . ?
O7 Th1 O9 66.82(9) . . ?
O7 Th1 O10 104.11(9) . . ?
O7 Th1 O12 119.80(9) . . ?
O7 Th1 O13 167.84(10) . . ?
O7 Th1 N1 129.79(10) . . ?
O7 Th1 N2 113.20(9) . . ?
O9 Th1 O3 126.41(9) . . ?
O9 Th1 O4 129.31(9) . . ?
O9 Th1 O6 64.03(10) . . ?
O9 Th1 O10 49.36(9) . . ?
O9 Th1 O12 65.17(10) . . ?
O9 Th1 O13 101.49(10) . . ?
O9 Th1 N1 162.90(10) . . ?
O9 Th1 N2 120.51(10) . . ?
O10 Th1 O3 120.78(9) . . ?
O10 Th1 O4 168.38(10) . . ?
O10 Th1 O6 67.14(10) . . ?
O10 Th1 O12 68.06(10) . . ?
O10 Th1 O13 68.24(10) . . ?
O10 Th1 N1 115.61(10) . . ?
O10 Th1 N2 131.11(10) . . ?
O12 Th1 O3 168.05(9) . . ?
O12 Th1 O4 123.05(9) . . ?
O12 Th1 O6 126.59(10) . . ?
O12 Th1 O13 49.14(10) . . ?
O12 Th1 N1 103.33(10) . . ?
O12 Th1 N2 66.43(10) . . ?
O13 Th1 O4 120.83(9) . . ?
O13 Th1 O6 129.91(9) . . ?
O13 Th1 N1 62.16(10) . . ?
O13 Th1 N2 69.04(10) . . ?
N1 Th1 N2 60.55(10) . . ?
C11 O1 Th1 120.7(2) . . ?
C22 O2 Th1 122.1(3) . . ?
N5 O3 Th1 97.7(2) . . ?
N5 O4 Th1 96.8(2) . . ?
N6 O6 Th1 95.8(2) . . ?
N6 O7 Th1 99.0(2) . . ?
N7 O9 Th1 97.5(2) . . ?
N7 O10 Th1 97.2(2) . . ?
N8 O12 Th1 97.5(2) . . ?
N8 O13 Th1 96.9(2) . . ?
C1 N1 Th1 117.4(3) . . ?
C1 N1 C5 119.1(4) . . ?
C5 N1 Th1 123.0(3) . . ?
C6 N2 Th1 122.9(3) . . ?
C6 N2 C10 118.8(4) . . ?
C10 N2 Th1 117.3(3) . . ?
C11 N3 C12 124.0(4) . . ?
C11 N3 C20 118.8(4) . . ?
C12 N3 C20 115.8(3) . . ?
C22 N4 C23 124.6(4) . . ?
C22 N4 C31 119.0(4) . . ?
C23 N4 C31 115.7(4) . . ?
O4 N5 O3 115.4(3) . . ?
O5 N5 O3 121.8(4) . . ?
O5 N5 O4 122.7(3) . . ?
O6 N6 Th1 59.51(19) . . ?
O6 N6 O7 115.7(3) . . ?
O7 N6 Th1 56.39(19) . . ?
O8 N6 Th1 175.0(3) . . ?
O8 N6 O6 122.5(3) . . ?
O8 N6 O7 121.8(3) . . ?
O9 N7 Th1 57.8(2) . . ?
O9 N7 O10 115.8(3) . . ?
O10 N7 Th1 58.07(19) . . ?
O11 N7 Th1 178.2(3) . . ?
O11 N7 O9 122.2(4) . . ?
O11 N7 O10 122.0(4) . . ?
O12 N8 Th1 57.9(2) . . ?
O13 N8 Th1 58.5(2) . . ?
O13 N8 O12 116.1(3) . . ?
O14 N8 Th1 173.8(3) . . ?
O14 N8 O12 121.4(4) . . ?
O14 N8 O13 122.6(4) . . ?
N1 C1 C2 123.1(4) . . ?
N1 C1 C11 111.5(4) . . ?
C2 C1 C11 125.0(4) . . ?
C1 C2 H2 121.1 . . ?
C1 C2 C3 117.8(4) . . ?
C3 C2 H2 121.1 . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.4(4) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.6(4) . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 120.9(4) . . ?
N1 C5 C6 116.3(4) . . ?
C4 C5 C6 122.8(4) . . ?
N2 C6 C5 116.3(4) . . ?
N2 C6 C7 121.7(4) . . ?
C7 C6 C5 122.0(4) . . ?
C6 C7 H7 120.5 . . ?
C8 C7 C6 119.1(4) . . ?
C8 C7 H7 120.5 . . ?
C7 C8 H8 120.2 . . ?
C7 C8 C9 119.6(4) . . ?
C9 C8 H8 120.2 . . ?
C8 C9 H9 120.8 . . ?
C8 C9 C10 118.4(4) . . ?
C10 C9 H9 120.8 . . ?
N2 C10 C9 122.3(4) . . ?
N2 C10 C22 112.2(4) . . ?
C9 C10 C22 125.0(4) . . ?
O1 C11 N3 121.2(4) . . ?
O1 C11 C1 115.7(4) . . ?
N3 C11 C1 123.2(4) . . ?
C13 C12 N3 119.8(4) . . ?
C17 C12 N3 119.2(4) . . ?
C17 C12 C13 120.8(4) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 C12 119.0(4) . . ?
C14 C13 H13 120.5 . . ?
C13 C14 H14 118.9 . . ?
C13 C14 C15 122.2(4) . . ?
C15 C14 H14 118.9 . . ?
C14 C15 C16 117.1(4) . . ?
C14 C15 C18 120.7(4) . . ?
C16 C15 C18 122.1(4) . . ?
C15 C16 H16 119.2 . . ?
C17 C16 C15 121.6(4) . . ?
C17 C16 H16 119.2 . . ?
C12 C17 H17 120.4 . . ?
C16 C17 C12 119.2(4) . . ?
C16 C17 H17 120.4 . . ?
C15 C18 H18A 108.3 . . ?
C15 C18 H18B 108.3 . . ?
C15 C18 C19 115.9(4) . . ?
H18A C18 H18B 107.4 . . ?
C19 C18 H18A 108.3 . . ?
C19 C18 H18B 108.3 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 H20A 109.3 . . ?
N3 C20 H20B 109.3 . . ?
N3 C20 C21 111.6(4) . . ?
H20A C20 H20B 108.0 . . ?
C21 C20 H20A 109.3 . . ?
C21 C20 H20B 109.3 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O2 C22 N4 121.5(4) . . ?
O2 C22 C10 116.1(4) . . ?
N4 C22 C10 122.3(4) . . ?
C24 C23 N4 120.4(4) . . ?
C24 C23 C28 120.7(4) . . ?
C28 C23 N4 118.8(4) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 C23 119.0(5) . . ?
C25 C24 H24 120.5 . . ?
C24 C25 H25 119.0 . . ?
C24 C25 C26 122.0(5) . . ?
C26 C25 H25 119.0 . . ?
C25 C26 C27 118.0(5) . . ?
C25 C26 C29 123.7(13) . . ?
C25 C26 C29A 115.1(13) . . ?
C27 C26 C29 117.9(13) . . ?
C27 C26 C29A 126.2(13) . . ?
C26 C27 H27 119.4 . . ?
C28 C27 C26 121.2(5) . . ?
C28 C27 H27 119.4 . . ?
C23 C28 C27 119.1(5) . . ?
C23 C28 H28 120.5 . . ?
C27 C28 H28 120.5 . . ?
C26 C29 H29A 108.7 . . ?
C26 C29 H29B 108.7 . . ?
H29A C29 H29B 107.6 . . ?
C30 C29 C26 114(2) . . ?
C30 C29 H29A 108.7 . . ?
C30 C29 H29B 108.7 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N4 C31 H31A 109.3 . . ?
N4 C31 H31B 109.3 . . ?
N4 C31 C32 111.6(4) . . ?
H31A C31 H31B 108.0 . . ?
C32 C31 H31A 109.3 . . ?
C32 C31 H31B 109.3 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C26 C29A H29C 108.7 . . ?
C26 C29A H29D 108.7 . . ?
H29C C29A H29D 107.6 . . ?
C30A C29A C26 114.4(19) . . ?
C30A C29A H29C 108.7 . . ?
C30A C29A H29D 108.7 . . ?
C29A C30A H30D 109.5 . . ?
C29A C30A H30E 109.5 . . ?
C29A C30A H30F 109.5 . . ?
H30D C30A H30E 109.5 . . ?
H30D C30A H30F 109.5 . . ?
H30E C30A H30F 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
Th1 O1 C11 N3 -135.7(3) . . . . ?
Th1 O1 C11 C1 44.9(4) . . . . ?
Th1 O2 C22 N4 -139.5(3) . . . . ?
Th1 O2 C22 C10 40.9(5) . . . . ?
Th1 O3 N5 O4 -10.7(3) . . . . ?
Th1 O3 N5 O5 167.5(3) . . . . ?
Th1 O4 N5 O3 10.6(3) . . . . ?
Th1 O4 N5 O5 -167.6(3) . . . . ?
Th1 O6 N6 O7 5.3(4) . . . . ?
Th1 O6 N6 O8 -174.7(4) . . . . ?
Th1 O7 N6 O6 -5.5(4) . . . . ?
Th1 O7 N6 O8 174.5(4) . . . . ?
Th1 O9 N7 O10 2.5(4) . . . . ?
Th1 O9 N7 O11 -177.8(4) . . . . ?
Th1 O10 N7 O9 -2.5(4) . . . . ?
Th1 O10 N7 O11 177.8(4) . . . . ?
Th1 O12 N8 O13 -6.4(4) . . . . ?
Th1 O12 N8 O14 172.8(4) . . . . ?
Th1 O13 N8 O12 6.3(4) . . . . ?
Th1 O13 N8 O14 -172.8(4) . . . . ?
Th1 N1 C1 C2 -170.0(3) . . . . ?
Th1 N1 C1 C11 2.9(4) . . . . ?
Th1 N1 C5 C4 169.8(3) . . . . ?
Th1 N1 C5 C6 -9.5(5) . . . . ?
Th1 N2 C6 C5 -8.0(5) . . . . ?
Th1 N2 C6 C7 169.0(3) . . . . ?
Th1 N2 C10 C9 -167.1(3) . . . . ?
Th1 N2 C10 C22 4.9(4) . . . . ?
N1 C1 C2 C3 -0.9(7) . . . . ?
N1 C1 C11 O1 -29.0(5) . . . . ?
N1 C1 C11 N3 151.6(4) . . . . ?
N1 C5 C6 N2 11.2(6) . . . . ?
N1 C5 C6 C7 -165.8(4) . . . . ?
N2 C6 C7 C8 -1.0(7) . . . . ?
N2 C10 C22 O2 -28.0(5) . . . . ?
N2 C10 C22 N4 152.4(4) . . . . ?
N3 C12 C13 C14 -176.6(4) . . . . ?
N3 C12 C17 C16 177.7(4) . . . . ?
N4 C23 C24 C25 -177.4(5) . . . . ?
N4 C23 C28 C27 176.5(4) . . . . ?
C1 N1 C5 C4 -1.9(6) . . . . ?
C1 N1 C5 C6 178.8(4) . . . . ?
C1 C2 C3 C4 -0.5(7) . . . . ?
C2 C1 C11 O1 143.7(4) . . . . ?
C2 C1 C11 N3 -35.7(6) . . . . ?
C2 C3 C4 C5 0.7(7) . . . . ?
C3 C4 C5 N1 0.5(7) . . . . ?
C3 C4 C5 C6 179.8(4) . . . . ?
C4 C5 C6 N2 -168.1(4) . . . . ?
C4 C5 C6 C7 14.9(7) . . . . ?
C5 N1 C1 C2 2.1(6) . . . . ?
C5 N1 C1 C11 175.0(4) . . . . ?
C5 C6 C7 C8 175.8(4) . . . . ?
C6 N2 C10 C9 2.5(6) . . . . ?
C6 N2 C10 C22 174.5(4) . . . . ?
C6 C7 C8 C9 -0.4(7) . . . . ?
C7 C8 C9 C10 2.7(7) . . . . ?
C8 C9 C10 N2 -3.8(7) . . . . ?
C8 C9 C10 C22 -174.8(4) . . . . ?
C9 C10 C22 O2 143.8(4) . . . . ?
C9 C10 C22 N4 -35.8(7) . . . . ?
C10 N2 C6 C5 -177.0(4) . . . . ?
C10 N2 C6 C7 0.0(6) . . . . ?
C11 N3 C12 C13 -63.2(6) . . . . ?
C11 N3 C12 C17 121.0(5) . . . . ?
C11 N3 C20 C21 92.0(5) . . . . ?
C11 C1 C2 C3 -172.8(4) . . . . ?
C12 N3 C11 O1 166.9(4) . . . . ?
C12 N3 C11 C1 -13.7(6) . . . . ?
C12 N3 C20 C21 -75.3(5) . . . . ?
C12 C13 C14 C15 0.2(7) . . . . ?
C13 C12 C17 C16 2.0(7) . . . . ?
C13 C14 C15 C16 -0.6(7) . . . . ?
C13 C14 C15 C18 177.6(4) . . . . ?
C14 C15 C16 C17 1.7(7) . . . . ?
C14 C15 C18 C19 143.0(4) . . . . ?
C15 C16 C17 C12 -2.4(7) . . . . ?
C16 C15 C18 C19 -39.0(6) . . . . ?
C17 C12 C13 C14 -0.9(7) . . . . ?
C18 C15 C16 C17 -176.4(4) . . . . ?
C20 N3 C11 O1 0.8(6) . . . . ?
C20 N3 C11 C1 -179.9(4) . . . . ?
C20 N3 C12 C13 103.4(5) . . . . ?
C20 N3 C12 C17 -72.4(5) . . . . ?
C22 N4 C23 C24 -61.4(6) . . . . ?
C22 N4 C23 C28 122.5(5) . . . . ?
C22 N4 C31 C32 94.1(5) . . . . ?
C23 N4 C22 O2 167.3(4) . . . . ?
C23 N4 C22 C10 -13.1(6) . . . . ?
C23 N4 C31 C32 -76.8(5) . . . . ?
C23 C24 C25 C26 2.1(8) . . . . ?
C24 C23 C28 C27 0.5(7) . . . . ?
C24 C25 C26 C27 -1.9(9) . . . . ?
C24 C25 C26 C29 -175.1(9) . . . . ?
C24 C25 C26 C29A 169.1(9) . . . . ?
C25 C26 C27 C28 0.9(9) . . . . ?
C25 C26 C29 C30 167.2(13) . . . . ?
C25 C26 C29A C30A 159.2(15) . . . . ?
C26 C27 C28 C23 -0.2(8) . . . . ?
C27 C26 C29 C30 -6.0(16) . . . . ?
C27 C26 C29A C30A -30.7(19) . . . . ?
C28 C23 C24 C25 -1.4(8) . . . . ?
C29 C26 C27 C28 174.6(9) . . . . ?
C31 N4 C22 O2 -2.8(6) . . . . ?
C31 N4 C22 C10 176.8(4) . . . . ?
C31 N4 C23 C24 108.9(5) . . . . ?
C31 N4 C23 C28 -67.1(6) . . . . ?
C29A C26 C27 C28 -168.9(9) . . . . ?

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

data_yp
_database_code_depnum_ccdc_archive 'CCDC 2395323'
loop_
_audit_author_name
_audit_author_address
'Mikhail Grigoriev'
;Frumkin Institute of Physical Chemistry and Electrochemistry
Russia
;
_audit_update_record             
;
2024-11-01 deposited with the CCDC.	2025-02-05 downloaded from the CCDC.
;
_audit_creation_date             2024-09-13
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C56 H48 F4 N12 Np3 O22, 2[CH3CN]'
_chemical_formula_sum            'C60 H54 F4 N14 Np3 O22'
_chemical_formula_weight         2110.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Np Np -11.4937 4.1493 '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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1713(3)
_cell_length_b                   11.5817(4)
_cell_length_c                   13.7244(4)
_cell_angle_alpha                85.634(2)
_cell_angle_beta                 89.208(2)
_cell_angle_gamma                63.655(2)
_cell_volume                     1586.26(9)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    8555
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.499
_cell_measurement_theta_min      3.440
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.981
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.209
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1003
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20669
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         3.440
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  
'Bruker KAPPA APEX II area-detector diffractometer'
_diffrn_measurement_method       'ω- and φ-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6238
_reflns_number_total             7225
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 1998)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1998)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.455
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         7225
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0262
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0147P)²+3.5450P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0582
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F3-C19
 1.35 with sigma of 0.01
3. Others
 Fixed Sof: F1(0.8) H15(0.2) H19(0.8) F3(0.2)
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C21(H21A,H21B)
4.b Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C22(H22A,H22B,H22C)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C25(H25), C26(H26), C27(H27), C28(H28)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Np1 Np 0.23079(2) 0.93651(2) 0.24731(2) 0.01081(5) Uani 1 1 d . . . . .
Np2 Np 0.000000 1.000000 0.000000 0.01150(5) Uani 1 2 d S . P . .
F1 F -0.1112(3) 0.7353(3) 0.5899(2) 0.0263(7) Uani 0.8 1 d . . P A 1
F2 F 0.3386(4) 1.3578(3) 0.2565(2) 0.0424(8) Uani 1 1 d . . . . .
O1 O 0.2846(3) 0.9664(3) 0.3613(2) 0.0182(6) Uani 1 1 d . . . . .
O2 O 0.1638(3) 0.9161(3) 0.12844(19) 0.0148(6) Uani 1 1 d . . . . .
O3 O -0.0997(3) 1.1272(3) 0.0705(2) 0.0184(6) Uani 1 1 d . . . . .
O4 O 0.1325(3) 0.8081(3) 0.3356(2) 0.0191(6) Uani 1 1 d . . . . .
O5 O 0.3522(3) 1.0447(3) 0.1645(2) 0.0165(6) Uani 1 1 d . . . . .
O6 O 0.3912(3) 0.6984(3) 0.3053(2) 0.0273(7) Uani 1 1 d . . . . .
O7 O 0.4681(3) 0.7840(3) 0.1919(2) 0.0219(7) Uani 1 1 d . . . . .
O8 O 0.5923(4) 0.5881(4) 0.2532(3) 0.0472(11) Uani 1 1 d . . . . .
O9 O -0.0257(3) 0.8386(3) 0.1252(2) 0.0274(7) Uani 1 1 d . . . . .
O10 O -0.1690(3) 0.9131(3) 0.0065(2) 0.0205(6) Uani 1 1 d . . . . .
O11 O -0.1690(4) 0.7599(4) 0.1086(2) 0.0333(8) Uani 1 1 d . . . . .
N1 N -0.0148(3) 1.0575(3) 0.3094(2) 0.0128(7) Uani 1 1 d . . . . .
N2 N 0.1059(3) 1.1869(3) 0.2098(2) 0.0135(7) Uani 1 1 d . . . . .
N3 N -0.0260(4) 0.7640(4) 0.4072(3) 0.0195(8) Uani 1 1 d . . . . .
N4 N 0.3933(4) 1.2075(3) 0.1018(3) 0.0181(7) Uani 1 1 d . . . . .
N5 N 0.4878(4) 0.6871(4) 0.2510(3) 0.0255(8) Uani 1 1 d . . . . .
N6 N -0.1215(4) 0.8334(4) 0.0814(2) 0.0196(8) Uani 1 1 d . . . . .
C31 C -0.0627(4) 0.9908(4) 0.3705(3) 0.0142(8) Uani 1 1 d . . . . .
C2 C -0.1681(4) 1.0519(4) 0.4322(3) 0.0197(9) Uani 1 1 d . . . . .
H2 H -0.197132 1.002957 0.476559 0.024 Uiso 1 1 calc R U . . .
C3 C -0.2305(5) 1.1868(5) 0.4275(3) 0.0274(11) Uani 1 1 d . . . . .
H3 H -0.301164 1.231181 0.470107 0.033 Uiso 1 1 calc R U . . .
C4 C -0.1879(5) 1.2553(4) 0.3598(3) 0.0226(10) Uani 1 1 d . . . . .
H4 H -0.232420 1.347066 0.352591 0.027 Uiso 1 1 calc R U . . .
C5 C -0.0788(4) 1.1872(4) 0.3027(3) 0.0150(8) Uani 1 1 d . . . . .
C6 C -0.0228(4) 1.2544(4) 0.2336(3) 0.0139(8) Uani 1 1 d . . . . .
C7 C -0.0988(4) 1.3812(4) 0.1987(3) 0.0189(9) Uani 1 1 d . . . . .
H7 H -0.188467 1.427530 0.218410 0.023 Uiso 1 1 calc R U . . .
C8 C -0.0422(4) 1.4392(4) 0.1347(3) 0.0204(9) Uani 1 1 d . . . . .
H8 H -0.093949 1.525012 0.107234 0.024 Uiso 1 1 calc R U . . .
C9 C 0.0902(4) 1.3721(4) 0.1106(3) 0.0188(9) Uani 1 1 d . . . . .
H9 H 0.130513 1.411115 0.066665 0.023 Uiso 1 1 calc R U . . .
C10 C 0.1632(4) 1.2474(4) 0.1514(3) 0.0138(8) Uani 1 1 d . . . . .
C11 C 0.0185(4) 0.8479(4) 0.3694(3) 0.0157(8) Uani 1 1 d . . . . .
C12 C 0.0645(5) 0.6225(5) 0.4097(4) 0.0299(11) Uani 1 1 d . . . . .
H12A H 0.053757 0.579339 0.471960 0.036 Uiso 1 1 calc R U . . .
H12B H 0.158533 0.608622 0.406511 0.036 Uiso 1 1 calc R U . . .
C13 C 0.0334(6) 0.5645(5) 0.3257(4) 0.0410(14) Uani 1 1 d . . . . .
H13A H 0.093696 0.471776 0.328580 0.061 Uiso 1 1 calc R U . . .
H13B H -0.059278 0.577185 0.329508 0.061 Uiso 1 1 calc R U . . .
H13C H 0.045340 0.606424 0.264157 0.061 Uiso 1 1 calc R U . . .
C14 C -0.1637(4) 0.7964(4) 0.4243(3) 0.0179(9) Uani 1 1 d . . . . .
C15 C -0.2036(5) 0.7777(4) 0.5185(3) 0.0211(9) Uani 1 1 d . . . . .
H15 H -0.139351 0.745778 0.570710 0.025 Uiso 0.2 1 calc R U P A 2
C16 C -0.3339(5) 0.8047(5) 0.5373(3) 0.0266(10) Uani 1 1 d . . . . .
H16 H -0.359554 0.791617 0.601867 0.032 Uiso 1 1 calc R U . . .
C17 C -0.4272(5) 0.8508(5) 0.4621(4) 0.0283(11) Uani 1 1 d . . . . .
H17 H -0.517779 0.870465 0.474839 0.034 Uiso 1 1 calc R U . . .
C18 C -0.3895(5) 0.8685(5) 0.3676(3) 0.0262(10) Uani 1 1 d . . . . .
H18 H -0.454002 0.900184 0.315614 0.031 Uiso 1 1 calc R U . . .
C19 C -0.2577(5) 0.8400(5) 0.3493(3) 0.0225(9) Uani 1 1 d D . . . .
H19 H -0.231665 0.850610 0.284306 0.027 Uiso 0.8 1 calc R U P B 1
C20 C 0.3096(4) 1.1616(4) 0.1388(3) 0.0156(8) Uani 1 1 d . . . . .
C21 C 0.5367(4) 1.1172(4) 0.0912(3) 0.0233(10) Uani 1 1 d . . . . .
H21A H 0.568298 1.138823 0.027852 0.028 Uiso 1 1 calc R U . . .
H21B H 0.547218 1.027710 0.091551 0.028 Uiso 1 1 calc R U . . .
C22 C 0.6206(5) 1.1257(5) 0.1737(4) 0.0367(12) Uani 1 1 d . . . . .
H22A H 0.714606 1.065569 0.165324 0.055 Uiso 1 1 calc R U . . .
H22B H 0.611303 1.214033 0.172765 0.055 Uiso 1 1 calc R U . . .
H22C H 0.590251 1.103065 0.236380 0.055 Uiso 1 1 calc R U . . .
C23 C 0.3627(4) 1.3421(4) 0.0893(3) 0.0190(9) Uani 1 1 d . . . . .
C24 C 0.3380(5) 1.4144(5) 0.1683(3) 0.0251(10) Uani 1 1 d . . . . .
C25 C 0.3084(5) 1.5431(5) 0.1586(4) 0.0350(12) Uani 1 1 d . . . . .
H25 H 0.288366 1.592142 0.214140 0.042 Uiso 1 1 calc R U . . .
C26 C 0.3085(5) 1.5999(5) 0.0661(4) 0.0343(12) Uani 1 1 d . . . . .
H26 H 0.287832 1.688974 0.057910 0.041 Uiso 1 1 calc R U . . .
C27 C 0.3382(5) 1.5284(5) -0.0140(4) 0.0291(11) Uani 1 1 d . . . . .
H27 H 0.340394 1.568210 -0.076740 0.035 Uiso 1 1 calc R U . . .
C28 C 0.3652(4) 1.3983(5) -0.0047(4) 0.0249(10) Uani 1 1 d . . . . .
H28 H 0.384736 1.349217 -0.060213 0.030 Uiso 1 1 calc R U . . .
F3 F -0.2185(14) 0.8686(15) 0.2635(8) 0.036(4) Uani 0.2 1 d D . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Np1 O1 1.794(3) . ?
Np1 O2 1.878(3) . ?
Np1 O4 2.455(3) . ?
Np1 O5 2.439(3) . ?
Np1 O6 2.602(3) . ?
Np1 O7 2.592(3) . ?
Np1 N1 2.631(3) . ?
Np1 N2 2.612(3) . ?
Np2 O2 2.377(3) 2_575 ?
Np2 O2 2.377(3) . ?
Np2 O3 1.754(3) 2_575 ?
Np2 O3 1.754(3) . ?
Np2 O9 2.550(3) 2_575 ?
Np2 O9 2.550(3) . ?
Np2 O10 2.501(3) 2_575 ?
Np2 O10 2.501(3) . ?
Np2 N6 2.961(3) 2_575 ?
Np2 N6 2.961(3) . ?
F1 C15 1.331(5) . ?
F2 C24 1.331(5) . ?
O4 C11 1.242(5) . ?
O5 C20 1.243(5) . ?
O6 N5 1.267(5) . ?
O7 N5 1.270(5) . ?
O8 N5 1.219(5) . ?
O9 N6 1.261(5) . ?
O10 N6 1.276(4) . ?
O11 N6 1.221(4) . ?
N1 C31 1.356(5) . ?
N1 C5 1.343(5) . ?
N2 C6 1.347(5) . ?
N2 C10 1.358(5) . ?
N3 C11 1.345(5) . ?
N3 C12 1.493(6) . ?
N3 C14 1.433(5) . ?
N4 C20 1.342(5) . ?
N4 C21 1.486(6) . ?
N4 C23 1.437(5) . ?
C31 C2 1.388(6) . ?
C31 C11 1.495(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.397(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.390(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.391(6) . ?
C5 C6 1.483(5) . ?
C6 C7 1.380(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.377(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.381(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.381(6) . ?
C10 C20 1.506(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.496(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.394(6) . ?
C14 C19 1.378(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.372(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.374(7) . ?
C17 H17 0.9500 . ?
C17 C18 1.386(7) . ?
C18 H18 0.9500 . ?
C18 C19 1.382(6) . ?
C19 H19 0.9500 . ?
C19 F3 1.319(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.516(7) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.371(6) . ?
C23 C28 1.406(6) . ?
C24 C25 1.371(7) . ?
C25 H25 0.9500 . ?
C25 C26 1.385(8) . ?
C26 H26 0.9500 . ?
C26 C27 1.374(7) . ?
C27 H27 0.9500 . ?
C27 C28 1.395(7) . ?
C28 H28 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Np1 O2 176.04(13) . . ?
O1 Np1 O4 90.06(11) . . ?
O1 Np1 O5 87.99(11) . . ?
O1 Np1 O6 82.06(12) . . ?
O1 Np1 O7 95.54(12) . . ?
O1 Np1 N1 86.87(11) . . ?
O1 Np1 N2 87.34(12) . . ?
O2 Np1 O4 90.22(11) . . ?
O2 Np1 O5 92.14(11) . . ?
O2 Np1 O6 101.57(12) . . ?
O2 Np1 O7 88.09(11) . . ?
O2 Np1 N1 89.79(11) . . ?
O2 Np1 N2 89.23(11) . . ?
O4 Np1 O6 62.65(10) . . ?
O4 Np1 O7 109.42(10) . . ?
O4 Np1 N1 61.67(10) . . ?
O4 Np1 N2 124.02(10) . . ?
O5 Np1 O4 173.74(10) . . ?
O5 Np1 O6 111.17(10) . . ?
O5 Np1 O7 64.89(10) . . ?
O5 Np1 N1 124.11(10) . . ?
O5 Np1 N2 61.84(10) . . ?
O6 Np1 N1 123.03(10) . . ?
O6 Np1 N2 167.62(10) . . ?
O7 Np1 O6 48.94(9) . . ?
O7 Np1 N1 170.84(10) . . ?
O7 Np1 N2 126.50(10) . . ?
N2 Np1 N1 62.35(10) . . ?
O2 Np2 O2 180.0 . 2_575 ?
O2 Np2 O9 64.75(9) 2_575 2_575 ?
O2 Np2 O9 115.25(9) 2_575 . ?
O2 Np2 O9 64.75(9) . . ?
O2 Np2 O9 115.25(9) . 2_575 ?
O2 Np2 O10 114.95(9) 2_575 2_575 ?
O2 Np2 O10 65.05(9) . 2_575 ?
O2 Np2 O10 114.95(9) . . ?
O2 Np2 O10 65.05(9) 2_575 . ?
O2 Np2 N6 89.71(10) . . ?
O2 Np2 N6 89.71(10) 2_575 2_575 ?
O2 Np2 N6 90.29(10) . 2_575 ?
O2 Np2 N6 90.29(10) 2_575 . ?
O3 Np2 O2 90.49(12) 2_575 . ?
O3 Np2 O2 89.51(12) . . ?
O3 Np2 O2 89.51(12) 2_575 2_575 ?
O3 Np2 O2 90.49(12) . 2_575 ?
O3 Np2 O3 180.0 2_575 . ?
O3 Np2 O9 90.13(12) . . ?
O3 Np2 O9 89.87(12) . 2_575 ?
O3 Np2 O9 89.87(12) 2_575 . ?
O3 Np2 O9 90.13(12) 2_575 2_575 ?
O3 Np2 O10 88.41(12) . 2_575 ?
O3 Np2 O10 91.59(12) . . ?
O3 Np2 O10 91.58(12) 2_575 2_575 ?
O3 Np2 O10 88.42(12) 2_575 . ?
O3 Np2 N6 92.60(12) . . ?
O3 Np2 N6 87.40(12) 2_575 . ?
O3 Np2 N6 92.60(12) 2_575 2_575 ?
O3 Np2 N6 87.40(12) . 2_575 ?
O9 Np2 O9 180.00(11) 2_575 . ?
O9 Np2 N6 25.05(10) . . ?
O9 Np2 N6 154.95(10) 2_575 . ?
O9 Np2 N6 25.05(10) 2_575 2_575 ?
O9 Np2 N6 154.95(10) . 2_575 ?
O10 Np2 O9 129.79(10) 2_575 . ?
O10 Np2 O9 50.21(10) . . ?
O10 Np2 O9 50.21(10) 2_575 2_575 ?
O10 Np2 O9 129.79(10) . 2_575 ?
O10 Np2 O10 180.0 2_575 . ?
O10 Np2 N6 154.74(10) . 2_575 ?
O10 Np2 N6 25.26(10) 2_575 2_575 ?
O10 Np2 N6 25.26(10) . . ?
O10 Np2 N6 154.74(10) 2_575 . ?
N6 Np2 N6 180.0 2_575 . ?
Np1 O2 Np2 149.72(15) . . ?
C11 O4 Np1 127.4(3) . . ?
C20 O5 Np1 127.7(3) . . ?
N5 O6 Np1 97.3(2) . . ?
N5 O7 Np1 97.7(2) . . ?
N6 O9 Np2 96.0(2) . . ?
N6 O10 Np2 98.0(2) . . ?
C31 N1 Np1 118.6(3) . . ?
C5 N1 Np1 120.5(2) . . ?
C5 N1 C31 118.6(3) . . ?
C6 N2 Np1 121.1(2) . . ?
C6 N2 C10 118.5(4) . . ?
C10 N2 Np1 119.5(3) . . ?
C11 N3 C12 118.9(4) . . ?
C11 N3 C14 124.4(4) . . ?
C14 N3 C12 115.0(3) . . ?
C20 N4 C21 119.5(4) . . ?
C20 N4 C23 124.5(4) . . ?
C23 N4 C21 114.7(3) . . ?
O6 N5 O7 116.0(4) . . ?
O8 N5 O6 122.2(4) . . ?
O8 N5 O7 121.7(4) . . ?
O9 N6 Np2 58.9(2) . . ?
O9 N6 O10 115.4(3) . . ?
O10 N6 Np2 56.78(19) . . ?
O11 N6 Np2 175.1(3) . . ?
O11 N6 O9 123.5(4) . . ?
O11 N6 O10 121.2(4) . . ?
N1 C31 C2 122.2(4) . . ?
N1 C31 C11 112.2(3) . . ?
C2 C31 C11 125.3(4) . . ?
C31 C2 H2 120.7 . . ?
C31 C2 C3 118.5(4) . . ?
C3 C2 H2 120.7 . . ?
C2 C3 H3 120.4 . . ?
C4 C3 C2 119.2(4) . . ?
C4 C3 H3 120.4 . . ?
C3 C4 H4 120.6 . . ?
C3 C4 C5 118.8(4) . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 122.3(4) . . ?
N1 C5 C6 116.1(3) . . ?
C4 C5 C6 121.5(4) . . ?
N2 C6 C5 116.6(4) . . ?
N2 C6 C7 122.4(4) . . ?
C7 C6 C5 121.0(4) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 C6 118.8(4) . . ?
C8 C7 H7 120.6 . . ?
C7 C8 H8 120.2 . . ?
C7 C8 C9 119.6(4) . . ?
C9 C8 H8 120.2 . . ?
C8 C9 H9 120.5 . . ?
C8 C9 C10 119.1(4) . . ?
C10 C9 H9 120.5 . . ?
N2 C10 C9 121.5(4) . . ?
N2 C10 C20 111.5(4) . . ?
C9 C10 C20 127.0(4) . . ?
O4 C11 N3 120.4(4) . . ?
O4 C11 C31 117.5(3) . . ?
N3 C11 C31 122.0(4) . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
N3 C12 C13 110.6(4) . . ?
H12A C12 H12B 108.1 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N3 119.6(4) . . ?
C19 C14 N3 121.8(4) . . ?
C19 C14 C15 118.6(4) . . ?
F1 C15 C14 117.6(4) . . ?
F1 C15 C16 121.2(4) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 C14 121.2(4) . . ?
C16 C15 H15 119.4 . . ?
C15 C16 H16 120.2 . . ?
C15 C16 C17 119.7(4) . . ?
C17 C16 H16 120.2 . . ?
C16 C17 H17 119.9 . . ?
C16 C17 C18 120.1(4) . . ?
C18 C17 H17 119.9 . . ?
C17 C18 H18 120.1 . . ?
C19 C18 C17 119.8(4) . . ?
C19 C18 H18 120.1 . . ?
C14 C19 C18 120.6(4) . . ?
C14 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
F3 C19 C14 116.2(8) . . ?
F3 C19 C18 122.6(8) . . ?
O5 C20 N4 120.0(4) . . ?
O5 C20 C10 117.6(3) . . ?
N4 C20 C10 122.3(4) . . ?
N4 C21 H21A 109.5 . . ?
N4 C21 H21B 109.5 . . ?
N4 C21 C22 110.8(4) . . ?
H21A C21 H21B 108.1 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 N4 120.9(4) . . ?
C24 C23 C28 119.6(4) . . ?
C28 C23 N4 119.4(4) . . ?
F2 C24 C23 118.2(4) . . ?
F2 C24 C25 119.6(4) . . ?
C25 C24 C23 122.1(5) . . ?
C24 C25 H25 120.7 . . ?
C24 C25 C26 118.6(5) . . ?
C26 C25 H25 120.7 . . ?
C25 C26 H26 119.7 . . ?
C27 C26 C25 120.6(5) . . ?
C27 C26 H26 119.7 . . ?
C26 C27 H27 119.5 . . ?
C26 C27 C28 121.0(5) . . ?
C28 C27 H27 119.5 . . ?
C23 C28 H28 121.0 . . ?
C27 C28 C23 118.0(5) . . ?
C27 C28 H28 121.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Np1 O4 C11 N3 173.0(3) . . . . ?
Np1 O4 C11 C31 -9.9(5) . . . . ?
Np1 O5 C20 N4 173.9(3) . . . . ?
Np1 O5 C20 C10 -5.8(5) . . . . ?
Np1 O6 N5 O7 -3.2(4) . . . . ?
Np1 O6 N5 O8 178.7(4) . . . . ?
Np1 O7 N5 O6 3.2(4) . . . . ?
Np1 O7 N5 O8 -178.7(4) . . . . ?
Np1 N1 C31 C2 157.6(3) . . . . ?
Np1 N1 C31 C11 -17.2(4) . . . . ?
Np1 N1 C5 C4 -159.4(3) . . . . ?
Np1 N1 C5 C6 18.0(4) . . . . ?
Np1 N2 C6 C5 14.8(4) . . . . ?
Np1 N2 C6 C7 -167.3(3) . . . . ?
Np1 N2 C10 C9 164.3(3) . . . . ?
Np1 N2 C10 C20 -15.4(4) . . . . ?
Np2 O9 N6 O10 -6.5(4) . . . . ?
Np2 O9 N6 O11 174.9(4) . . . . ?
Np2 O10 N6 O9 6.7(4) . . . . ?
Np2 O10 N6 O11 -174.7(3) . . . . ?
F1 C15 C16 C17 178.8(4) . . . . ?
F2 C24 C25 C26 180.0(5) . . . . ?
O4 Np1 O2 Np2 100.5(3) . . . . ?
O5 Np1 O2 Np2 -85.3(3) . . . . ?
O6 Np1 O2 Np2 162.6(3) . . . . ?
O7 Np1 O2 Np2 -150.1(3) . . . . ?
N1 Np1 O2 Np2 38.8(3) . . . . ?
N1 C31 C2 C3 3.0(6) . . . . ?
N1 C31 C11 O4 17.7(5) . . . . ?
N1 C31 C11 N3 -165.3(4) . . . . ?
N1 C5 C6 N2 -21.4(5) . . . . ?
N1 C5 C6 C7 160.7(4) . . . . ?
N2 Np1 O2 Np2 -23.5(3) . . . . ?
N2 C6 C7 C8 2.2(6) . . . . ?
N2 C10 C20 O5 13.8(5) . . . . ?
N2 C10 C20 N4 -165.8(3) . . . . ?
N3 C14 C15 F1 3.0(6) . . . . ?
N3 C14 C15 C16 -178.4(4) . . . . ?
N3 C14 C19 C18 178.8(4) . . . . ?
N3 C14 C19 F3 -9.8(10) . . . . ?
N4 C23 C24 F2 -2.3(7) . . . . ?
N4 C23 C24 C25 -180.0(4) . . . . ?
N4 C23 C28 C27 -178.4(4) . . . . ?
C31 N1 C5 C4 3.5(6) . . . . ?
C31 N1 C5 C6 -179.2(3) . . . . ?
C31 C2 C3 C4 1.8(7) . . . . ?
C2 C31 C11 O4 -157.0(4) . . . . ?
C2 C31 C11 N3 20.0(6) . . . . ?
C2 C3 C4 C5 -3.9(7) . . . . ?
C3 C4 C5 N1 1.3(7) . . . . ?
C3 C4 C5 C6 -176.0(4) . . . . ?
C4 C5 C6 N2 156.0(4) . . . . ?
C4 C5 C6 C7 -21.9(6) . . . . ?
C5 N1 C31 C2 -5.6(6) . . . . ?
C5 N1 C31 C11 179.6(3) . . . . ?
C5 C6 C7 C8 -180.0(4) . . . . ?
C6 N2 C10 C9 -4.8(5) . . . . ?
C6 N2 C10 C20 175.4(3) . . . . ?
C6 C7 C8 C9 -3.1(6) . . . . ?
C7 C8 C9 C10 0.1(6) . . . . ?
C8 C9 C10 N2 3.9(6) . . . . ?
C8 C9 C10 C20 -176.4(4) . . . . ?
C9 C10 C20 O5 -165.9(4) . . . . ?
C9 C10 C20 N4 14.5(6) . . . . ?
C10 N2 C6 C5 -176.2(3) . . . . ?
C10 N2 C6 C7 1.7(5) . . . . ?
C11 N3 C12 C13 -98.7(5) . . . . ?
C11 N3 C14 C15 -121.6(5) . . . . ?
C11 N3 C14 C19 61.7(6) . . . . ?
C11 C31 C2 C3 177.1(4) . . . . ?
C12 N3 C11 O4 1.2(6) . . . . ?
C12 N3 C11 C31 -175.7(4) . . . . ?
C12 N3 C14 C15 73.5(5) . . . . ?
C12 N3 C14 C19 -103.2(5) . . . . ?
C14 N3 C11 O4 -163.1(4) . . . . ?
C14 N3 C11 C31 19.9(6) . . . . ?
C14 N3 C12 C13 67.1(5) . . . . ?
C14 C15 C16 C17 0.1(7) . . . . ?
C15 C14 C19 C18 2.0(7) . . . . ?
C15 C14 C19 F3 173.4(9) . . . . ?
C15 C16 C17 C18 0.7(7) . . . . ?
C16 C17 C18 C19 -0.1(8) . . . . ?
C17 C18 C19 C14 -1.3(7) . . . . ?
C17 C18 C19 F3 -172.1(9) . . . . ?
C19 C14 C15 F1 179.8(4) . . . . ?
C19 C14 C15 C16 -1.5(7) . . . . ?
C20 N4 C21 C22 -100.8(5) . . . . ?
C20 N4 C23 C24 63.1(6) . . . . ?
C20 N4 C23 C28 -120.4(5) . . . . ?
C21 N4 C20 O5 0.5(6) . . . . ?
C21 N4 C20 C10 -179.9(4) . . . . ?
C21 N4 C23 C24 -104.0(5) . . . . ?
C21 N4 C23 C28 72.5(5) . . . . ?
C23 N4 C20 O5 -166.1(4) . . . . ?
C23 N4 C20 C10 13.5(6) . . . . ?
C23 N4 C21 C22 67.0(5) . . . . ?
C23 C24 C25 C26 -2.4(8) . . . . ?
C24 C23 C28 C27 -1.9(7) . . . . ?
C24 C25 C26 C27 -0.3(8) . . . . ?
C25 C26 C27 C28 1.8(8) . . . . ?
C26 C27 C28 C23 -0.7(7) . . . . ?
C28 C23 C24 F2 -178.8(4) . . . . ?
C28 C23 C24 C25 3.5(7) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.500 0.500 103.0 58.7 '2 CH3CN'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT910_yp                  
;
RESPONSE: Data completeness is 99.3% which is enough for good refinement of data. 
Most of the missing reflections were excluded in order to avoid problems related to 
extinction and saturation common to low theta reflections.
;
####################################################################### 
# 
# 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_npn4721_lt
_database_code_depnum_ccdc_archive 'CCDC 2395325'
loop_
_audit_author_name
_audit_author_address
'Mikhail Grigoriev'
;Frumkin Institute of Physical Chemistry and Electrochemistry
Russia
;
_audit_update_record             
;
2025-01-31 deposited with the CCDC.	2025-02-05 downloaded from the CCDC.
;
_audit_creation_date             2024-09-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C30 H30 N5 Np O7), N4 Np O14'
_chemical_formula_sum            'C60 H60 N14 Np3 O28'
_chemical_formula_weight         2136.22
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Np Np -11.4937 4.1493 '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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.1227(13)
_cell_length_b                   17.534(3)
_cell_length_c                   25.389(4)
_cell_angle_alpha                106.001(7)
_cell_angle_beta                 92.587(7)
_cell_angle_gamma                94.446(7)
_cell_volume                     3457.1(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.30
_cell_measurement_theta_min      2.93
_shelx_estimated_absorpt_T_max   0.914
_shelx_estimated_absorpt_T_min   0.322
_exptl_absorpt_coefficient_mu    4.571
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.052
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             2042
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2227
_diffrn_reflns_av_unetI/netI     0.2785
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            36429
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         4.147
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  
'Bruker KAPPA APEX II area-detector diffractometer'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5346
_reflns_number_total             12103
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.453
_refine_diff_density_min         -2.347
_refine_diff_density_rms         0.263
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         12103
_refine_ls_number_restraints     255
_refine_ls_R_factor_all          0.2265
_refine_ls_R_factor_gt           0.0954
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0706P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.2159
_refine_special_details          
;
The data are of insufficient quality 
and can be used only to establish molecular connectivity/identity.
The precision of geometric parameters is low. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq: with sigma of 0.025 and sigma for terminal atoms of 0.05
Uanis(O9) \\sim Ueq: with sigma of 0.012 and sigma for terminal atoms of 0.024
Uanis(C7) = Uanis(C6)
Uanis(C54) = Uanis(C57)
Uanis(C19) = Uanis(C16)
Uanis(O10) = Uanis(C31)
Uanis(C35) = Uanis(C32)
Uanis(C34) = Uanis(N7)
Uanis(C48) = Uanis(C45)
Uanis(C42) = Uanis(N9)
3. Rigid body (RIGU) restrains
 C18, C19, C20, C15, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, C5, C4, C3, C2, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24, C29, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36, C35, C34, C33, C32, N7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C8, C9, C10, C11, N3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C45, C50, C49, C48, C47, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C55, C54, C59, C58, C57, C56
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O20, N12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C22(H22A,H22B), C43(H43A,H43B), C52(H52A,H52B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C17(H17), C18(H18),
 C19(H19), C20(H20), C26(H26), C27(H27), C28(H28), C29(H29), C33(H33), C34(H34),
  C35(H35), C38(H38), C39(H39), C40(H40), C47(H47), C48(H48), C49(H49),
 C50(H50), C56(H56), C57(H57), C58(H58), C59(H59)
4.c Fitted hexagon refined as free rotating group:
 C24(C25,C26,C27,C28,C29), C45(C46,C47,C48,C49,C50), C54(C55,C56,C57,C58,C59)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C30(H30A,H30B,
 H30C), C44(H44A,H44B,H44C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C60(H60A,
 H60B,H60C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Np1 Np 0.73844(11) 0.45749(6) 0.61398(4) 0.0303(3) Uani 1 1 d . . . . .
Np2 Np 0.14936(11) 0.56257(6) 0.86191(4) 0.0320(3) Uani 1 1 d . . . . .
Np3 Np 0.01752(13) -0.01327(7) 0.25122(5) 0.0567(4) Uani 1 1 d . . . . .
O1 O 0.6348(18) 0.4447(11) 0.5513(6) 0.060(5) Uani 1 1 d . U . . .
O2 O 0.8310(17) 0.4728(10) 0.6793(6) 0.041(4) Uani 1 1 d . . . . .
O3 O 0.7361(19) 0.5989(9) 0.6351(6) 0.039(4) Uani 1 1 d . . . . .
O4 O 0.768(2) 0.3200(11) 0.5938(7) 0.062(5) Uani 1 1 d . . . . .
O5 O 0.9671(19) 0.5322(10) 0.5822(7) 0.050(5) Uani 1 1 d . . . . .
O6 O 1.0001(18) 0.4114(9) 0.5740(6) 0.037(4) Uani 1 1 d . . . . .
O7 O 1.1983(17) 0.4848(9) 0.5546(6) 0.041(4) Uani 1 1 d . . . . .
O8 O 0.0593(16) 0.5228(10) 0.7965(5) 0.042(4) Uani 1 1 d . . . . .
O9 O 0.2413(19) 0.6035(11) 0.9276(5) 0.055(5) Uani 1 1 d . U . . .
O10 O 0.158(2) 0.4330(10) 0.8675(6) 0.050(4) Uani 1 1 d . . . . .
O11 O 0.1196(18) 0.6922(9) 0.8542(6) 0.039(4) Uani 1 1 d . . . . .
O12 O -0.0908(18) 0.5055(10) 0.9021(6) 0.042(4) Uani 1 1 d . . . . .
O13 O -0.1140(17) 0.6225(10) 0.8909(6) 0.039(4) Uani 1 1 d . . . . .
O14 O -0.3205(18) 0.5646(10) 0.9232(6) 0.044(5) Uani 1 1 d . . . . .
O15 O -0.1976(19) -0.0130(10) 0.2537(7) 0.059(5) Uani 1 1 d . . . . .
O16 O 0.2322(19) -0.0168(11) 0.2482(8) 0.079(7) Uani 1 1 d . . . . .
O17 O 0.066(2) 0.0716(11) 0.3486(8) 0.062(6) Uani 1 1 d . . . . .
O18 O 0.006(2) -0.0552(13) 0.3378(8) 0.072(6) Uani 1 1 d . . . . .
O19 O 0.047(2) 0.0294(13) 0.4208(9) 0.079(7) Uani 1 1 d . . . . .
O20 O 0.016(3) 0.0285(12) 0.1673(9) 0.086(7) Uani 1 1 d . . . . .
O21 O -0.016(2) -0.0944(12) 0.1534(8) 0.067(6) Uani 1 1 d . . . . .
O22 O -0.031(2) -0.0536(13) 0.0824(9) 0.080(7) Uani 1 1 d . . . . .
O23 O 0.054(2) 0.1269(12) 0.2669(8) 0.071(6) Uani 1 1 d . . . . .
O24 O -0.191(3) 0.1539(13) 0.2379(8) 0.083(7) Uani 1 1 d . . . . .
O25 O 0.012(3) 0.2474(13) 0.2659(9) 0.083(7) Uani 1 1 d . . . . .
O26 O -0.018(2) -0.1533(12) 0.2391(8) 0.085(7) Uani 1 1 d . . . . .
O27 O 0.215(2) -0.1812(10) 0.2649(8) 0.069(6) Uani 1 1 d . . . . .
O28 O 0.016(2) -0.2752(11) 0.2395(7) 0.052(5) Uani 1 1 d . . . . .
N1 N 0.601(2) 0.6982(12) 0.6220(8) 0.037(5) Uani 1 1 d . . . . .
N2 N 0.480(2) 0.5208(11) 0.6564(7) 0.032(4) Uani 1 1 d . . . . .
N3 N 0.504(2) 0.3632(11) 0.6398(7) 0.032(4) Uani 1 1 d . . . . .
N4 N 0.703(2) 0.1905(13) 0.5824(8) 0.042(5) Uani 1 1 d . . . . .
N5 N 1.062(2) 0.4780(14) 0.5693(8) 0.039(5) Uani 1 1 d . . . . .
N6 N 0.257(2) 0.3225(12) 0.8763(7) 0.035(5) Uani 1 1 d . . . . .
N7 N 0.410(2) 0.4857(12) 0.8287(7) 0.035(3) Uani 1 1 d . . . . .
N8 N 0.399(2) 0.6358(11) 0.8301(7) 0.031(5) Uani 1 1 d . . . . .
N9 N 0.238(2) 0.8149(12) 0.8903(8) 0.047(5) Uani 1 1 d . . . . .
N10 N -0.177(3) 0.5654(13) 0.9069(8) 0.038(5) Uani 1 1 d . . . . .
N11 N 0.044(3) 0.0159(18) 0.3716(12) 0.060(7) Uani 1 1 d . . . . .
N12 N -0.016(3) -0.0391(17) 0.1325(12) 0.073(8) Uani 1 1 d . . . . .
N13 N -0.040(3) 0.1765(13) 0.2548(8) 0.040(5) Uani 1 1 d . . . . .
N14 N 0.077(3) -0.2081(13) 0.2489(9) 0.044(6) Uani 1 1 d . . . . .
C1 C 0.603(3) 0.6360(15) 0.6382(10) 0.040(6) Uani 1 1 d . . . . .
C2 C 0.461(3) 0.5956(15) 0.6583(9) 0.035(5) Uani 1 1 d . . . . .
C3 C 0.328(3) 0.6364(13) 0.6805(8) 0.032(5) Uani 1 1 d . . . . .
H3 H 0.322194 0.691384 0.683828 0.039 Uiso 1 1 calc R U . . .
C4 C 0.202(3) 0.5904(13) 0.6977(8) 0.030(5) Uani 1 1 d . . . . .
H4 H 0.107684 0.614161 0.713244 0.036 Uiso 1 1 calc R U . . .
C5 C 0.216(2) 0.5145(12) 0.6921(8) 0.023(4) Uani 1 1 d . . . . .
H5 H 0.128794 0.483778 0.702716 0.027 Uiso 1 1 calc R U . . .
C6 C 0.351(2) 0.4784(13) 0.6716(8) 0.026(3) Uani 1 1 d . . . . .
C7 C 0.378(2) 0.3954(13) 0.6677(8) 0.026(3) Uani 1 1 d . . . . .
C8 C 0.276(3) 0.3527(13) 0.6943(9) 0.036(5) Uani 1 1 d . . . . .
H8 H 0.186466 0.375644 0.713606 0.043 Uiso 1 1 calc R U . . .
C9 C 0.310(3) 0.2760(13) 0.6916(9) 0.035(5) Uani 1 1 d . . . . .
H9 H 0.243447 0.245488 0.709812 0.042 Uiso 1 1 calc R U . . .
C10 C 0.442(2) 0.2424(14) 0.6619(9) 0.038(5) Uani 1 1 d . . . . .
H10 H 0.466038 0.189272 0.658897 0.045 Uiso 1 1 calc R U . . .
C11 C 0.533(3) 0.2900(14) 0.6378(10) 0.038(6) Uani 1 1 d . . . . .
C12 C 0.679(3) 0.2634(16) 0.6036(11) 0.042(6) Uani 1 1 d . . . . .
C13 C 0.761(2) 0.7302(15) 0.5997(9) 0.042(7) Uani 1 1 d . . . . .
H13A H 0.760987 0.787933 0.603710 0.050 Uiso 1 1 calc R U . . .
H13B H 0.861191 0.721548 0.620413 0.050 Uiso 1 1 calc R U . . .
C14 C 0.761(3) 0.6833(15) 0.5384(10) 0.051(7) Uani 1 1 d . . . . .
H14A H 0.654866 0.686279 0.519514 0.077 Uiso 1 1 calc R U . . .
H14B H 0.776918 0.627432 0.535367 0.077 Uiso 1 1 calc R U . . .
H14C H 0.851013 0.706441 0.521578 0.077 Uiso 1 1 calc R U . . .
C15 C 0.457(3) 0.7354(16) 0.6107(10) 0.049(6) Uani 1 1 d . . . . .
C16 C 0.425(3) 0.8041(16) 0.6436(10) 0.043(4) Uani 1 1 d . . . . .
C17 C 0.272(3) 0.8350(16) 0.6317(10) 0.047(6) Uani 1 1 d . . . . .
H17 H 0.245163 0.884885 0.654037 0.057 Uiso 1 1 calc R U . . .
C18 C 0.168(3) 0.7931(16) 0.5889(10) 0.051(6) Uani 1 1 d . . . . .
H18 H 0.069023 0.813622 0.580232 0.062 Uiso 1 1 calc R U . . .
C19 C 0.210(3) 0.7175(15) 0.5569(10) 0.043(4) Uani 1 1 d . . . . .
H19 H 0.136432 0.687992 0.526707 0.052 Uiso 1 1 calc R U . . .
C20 C 0.350(3) 0.6864(16) 0.5679(10) 0.046(5) Uani 1 1 d . . . . .
H20 H 0.373765 0.634579 0.548010 0.056 Uiso 1 1 calc R U . . .
C21 C 0.528(3) 0.8569(17) 0.6918(10) 0.071(9) Uani 1 1 d . . . . .
H21A H 0.559236 0.825826 0.716766 0.106 Uiso 1 1 calc R U . . .
H21B H 0.464804 0.900252 0.711086 0.106 Uiso 1 1 calc R U . . .
H21C H 0.628181 0.879249 0.679185 0.106 Uiso 1 1 calc R U . . .
C22 C 0.861(3) 0.1684(14) 0.5510(11) 0.055(8) Uani 1 1 d . . . . .
H22A H 0.857523 0.109937 0.535113 0.066 Uiso 1 1 calc R U . . .
H22B H 0.868803 0.193920 0.520807 0.066 Uiso 1 1 calc R U . . .
C23 C 1.000(4) 0.1967(19) 0.5903(14) 0.096(12) Uani 1 1 d . . . . .
H23A H 1.102485 0.192257 0.571219 0.145 Uiso 1 1 calc R U . . .
H23B H 1.000669 0.164712 0.616383 0.145 Uiso 1 1 calc R U . . .
H23C H 0.991431 0.252645 0.610088 0.145 Uiso 1 1 calc R U . . .
C24 C 0.5919(17) 0.1251(9) 0.5781(7) 0.057(7) Uani 1 1 d G . . . .
C25 C 0.4512(19) 0.1109(9) 0.5422(7) 0.049(7) Uani 1 1 d G . . . .
C26 C 0.3357(15) 0.0470(10) 0.5397(6) 0.043(7) Uani 1 1 d G . . . .
H26 H 0.239589 0.037242 0.515168 0.051 Uiso 1 1 calc R U . . .
C27 C 0.3608(18) -0.0027(8) 0.5730(7) 0.060(8) Uani 1 1 d G . . . .
H27 H 0.281776 -0.046356 0.571225 0.072 Uiso 1 1 calc R U . . .
C28 C 0.501(2) 0.0116(10) 0.6088(6) 0.060(7) Uani 1 1 d G . . . .
H28 H 0.518495 -0.022378 0.631580 0.072 Uiso 1 1 calc R U . . .
C29 C 0.6169(16) 0.0755(11) 0.6114(6) 0.056(7) Uani 1 1 d G . . . .
H29 H 0.713030 0.085200 0.635880 0.067 Uiso 1 1 calc R U . . .
C30 C 0.423(3) 0.1621(14) 0.5062(11) 0.059(8) Uani 1 1 d . . . . .
H30A H 0.322962 0.188965 0.515765 0.088 Uiso 1 1 calc R U . . .
H30B H 0.410214 0.129457 0.467902 0.088 Uiso 1 1 calc R U . . .
H30C H 0.518340 0.201996 0.511053 0.088 Uiso 1 1 calc R U . . .
C31 C 0.273(3) 0.3843(18) 0.8598(11) 0.050(4) Uani 1 1 d . . . . .
C32 C 0.414(3) 0.4104(15) 0.8312(8) 0.034(3) Uani 1 1 d . . . . .
C33 C 0.537(3) 0.3652(15) 0.8088(8) 0.036(5) Uani 1 1 d . . . . .
H33 H 0.535749 0.311044 0.809024 0.044 Uiso 1 1 calc R U . . .
C34 C 0.660(3) 0.3990(14) 0.7864(8) 0.035(3) Uani 1 1 d . . . . .
H34 H 0.746884 0.368209 0.771479 0.042 Uiso 1 1 calc R U . . .
C35 C 0.664(3) 0.4737(14) 0.7844(8) 0.034(3) Uani 1 1 d . . . . .
H35 H 0.751301 0.496860 0.768728 0.041 Uiso 1 1 calc R U . . .
C36 C 0.536(3) 0.5165(16) 0.8059(9) 0.036(5) Uani 1 1 d . . . . .
C37 C 0.531(3) 0.6021(17) 0.8076(9) 0.048(8) Uani 1 1 d . . . . .
C38 C 0.655(3) 0.6436(18) 0.7880(9) 0.047(7) Uani 1 1 d . . . . .
H38 H 0.745926 0.618149 0.771328 0.056 Uiso 1 1 calc R U . . .
C39 C 0.641(3) 0.7221(19) 0.7934(10) 0.053(8) Uani 1 1 d . . . . .
H39 H 0.725308 0.751393 0.780607 0.063 Uiso 1 1 calc R U . . .
C40 C 0.509(3) 0.7614(13) 0.8167(10) 0.040(6) Uani 1 1 d . . . . .
H40 H 0.498172 0.815923 0.819671 0.048 Uiso 1 1 calc R U . . .
C41 C 0.396(3) 0.7143(16) 0.8351(9) 0.040(6) Uani 1 1 d . . . . .
C42 C 0.239(3) 0.7445(16) 0.8615(11) 0.047(5) Uani 1 1 d . . . . .
C43 C 0.109(3) 0.3021(15) 0.8993(10) 0.054(8) Uani 1 1 d . . . . .
H43A H 0.093255 0.243540 0.892303 0.065 Uiso 1 1 calc R U . . .
H43B H 0.013748 0.318240 0.880410 0.065 Uiso 1 1 calc R U . . .
C44 C 0.107(3) 0.3410(18) 0.9610(10) 0.072(9) Uani 1 1 d . . . . .
H44A H 0.107347 0.398846 0.968006 0.107 Uiso 1 1 calc R U . . .
H44B H 0.205590 0.328996 0.979881 0.107 Uiso 1 1 calc R U . . .
H44C H 0.007506 0.320135 0.974753 0.107 Uiso 1 1 calc R U . . .
C45 C 0.3859(19) 0.2750(12) 0.8785(9) 0.075(6) Uani 1 1 d G . . . .
C46 C 0.526(2) 0.3008(10) 0.9146(7) 0.068(7) Uani 1 1 d G . . . .
C47 C 0.6556(18) 0.2529(12) 0.9115(8) 0.073(7) Uani 1 1 d G . . . .
H47 H 0.751221 0.270561 0.936111 0.088 Uiso 1 1 calc R U . . .
C48 C 0.6456(19) 0.1793(11) 0.8723(9) 0.075(6) Uani 1 1 d G . . . .
H48 H 0.734351 0.146547 0.870179 0.090 Uiso 1 1 calc R U . . .
C49 C 0.506(2) 0.1535(10) 0.8362(8) 0.091(9) Uani 1 1 d G . . . .
H49 H 0.498866 0.103139 0.809462 0.109 Uiso 1 1 calc R U . . .
C50 C 0.3759(19) 0.2014(13) 0.8393(8) 0.078(8) Uani 1 1 d G . . . .
H50 H 0.280250 0.183746 0.814677 0.094 Uiso 1 1 calc R U . . .
C51 C 0.542(4) 0.3822(19) 0.9536(12) 0.093(12) Uani 1 1 d . . . . .
H51A H 0.638635 0.413237 0.945492 0.140 Uiso 1 1 calc R U . . .
H51B H 0.557041 0.378324 0.991232 0.140 Uiso 1 1 calc R U . . .
H51C H 0.442280 0.408513 0.949622 0.140 Uiso 1 1 calc R U . . .
C52 C 0.080(3) 0.8409(15) 0.9148(13) 0.062(9) Uani 1 1 d . . . . .
H52A H -0.015235 0.813861 0.888662 0.074 Uiso 1 1 calc R U . . .
H52B H 0.078067 0.899026 0.920633 0.074 Uiso 1 1 calc R U . . .
C53 C 0.060(4) 0.8218(17) 0.9686(13) 0.081(10) Uani 1 1 d . . . . .
H53A H 0.024733 0.764980 0.961618 0.121 Uiso 1 1 calc R U . . .
H53B H -0.023133 0.853463 0.988741 0.121 Uiso 1 1 calc R U . . .
H53C H 0.166315 0.834545 0.990483 0.121 Uiso 1 1 calc R U . . .
C54 C 0.376(2) 0.8731(11) 0.9103(9) 0.086(7) Uani 1 1 d G . . . .
C55 C 0.503(3) 0.8640(11) 0.9461(9) 0.085(8) Uani 1 1 d G . . . .
C56 C 0.637(2) 0.9213(13) 0.9619(8) 0.088(8) Uani 1 1 d G . . . .
H56 H 0.723816 0.915054 0.986299 0.106 Uiso 1 1 calc R U . . .
C57 C 0.645(2) 0.9877(11) 0.9420(9) 0.086(7) Uani 1 1 d G . . . .
H57 H 0.736583 1.026870 0.952774 0.104 Uiso 1 1 calc R U . . .
C58 C 0.518(3) 0.9968(11) 0.9062(9) 0.111(11) Uani 1 1 d G . . . .
H58 H 0.522926 1.042219 0.892632 0.133 Uiso 1 1 calc R U . . .
C59 C 0.383(2) 0.9395(14) 0.8904(8) 0.085(8) Uani 1 1 d G . . . .
H59 H 0.296502 0.945751 0.866015 0.102 Uiso 1 1 calc R U . . .
C60 C 0.504(4) 0.7991(18) 0.9643(12) 0.087(11) Uani 1 1 d . . . . .
H60A H 0.397091 0.767269 0.954258 0.131 Uiso 1 1 calc R U . . .
H60B H 0.524998 0.815441 1.004317 0.131 Uiso 1 1 calc R U . . .
H60C H 0.592030 0.767115 0.947546 0.131 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
Np1 O1 1.716(14) . ?
Np1 O2 1.731(14) . ?
Np1 O3 2.390(16) . ?
Np1 O4 2.357(18) . ?
Np1 O5 2.482(16) . ?
Np1 O6 2.492(14) . ?
Np1 N2 2.591(17) . ?
Np1 N3 2.649(17) . ?
Np2 O8 1.718(13) . ?
Np2 O9 1.731(13) . ?
Np2 O10 2.321(17) . ?
Np2 O11 2.365(14) . ?
Np2 O12 2.508(15) . ?
Np2 O13 2.508(14) . ?
Np2 N7 2.643(18) . ?
Np2 N8 2.596(17) . ?
Np3 O15 1.751(15) . ?
Np3 O16 1.754(15) . ?
Np3 O17 2.505(18) . ?
Np3 O18 2.506(19) . ?
Np3 O20 2.44(2) . ?
Np3 O21 2.490(18) . ?
Np3 O23 2.37(2) . ?
Np3 O26 2.38(2) . ?
O3 C1 1.30(2) . ?
O4 C12 1.27(3) . ?
O5 N5 1.25(2) . ?
O6 N5 1.27(2) . ?
O7 N5 1.19(2) . ?
O10 C31 1.30(3) . ?
O11 C42 1.25(3) . ?
O12 N10 1.29(2) . ?
O13 N10 1.26(2) . ?
O14 N10 1.25(2) . ?
O17 N11 1.27(3) . ?
O18 N11 1.31(3) . ?
O19 N11 1.20(3) . ?
O20 N12 1.27(3) . ?
O21 N12 1.23(3) . ?
O22 N12 1.23(3) . ?
O23 N13 1.29(2) . ?
O24 N13 1.27(2) . ?
O25 N13 1.23(2) . ?
O26 N14 1.34(2) . ?
O27 N14 1.19(2) . ?
O28 N14 1.20(2) . ?
N1 C1 1.27(3) . ?
N1 C13 1.57(3) . ?
N1 C15 1.44(3) . ?
N2 C2 1.32(3) . ?
N2 C6 1.37(3) . ?
N3 C7 1.34(2) . ?
N3 C11 1.31(3) . ?
N4 C12 1.28(3) . ?
N4 C22 1.56(3) . ?
N4 C24 1.38(2) . ?
N6 C31 1.27(3) . ?
N6 C43 1.43(3) . ?
N6 C45 1.39(2) . ?
N7 C32 1.34(3) . ?
N7 C36 1.35(3) . ?
N8 C37 1.33(3) . ?
N8 C41 1.35(3) . ?
N9 C42 1.25(3) . ?
N9 C52 1.50(3) . ?
N9 C54 1.43(2) . ?
C1 C2 1.49(3) . ?
C2 C3 1.40(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.41(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.31(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.36(3) . ?
C6 C7 1.47(3) . ?
C7 C8 1.39(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.38(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.41(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.36(3) . ?
C11 C12 1.52(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.55(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.32(3) . ?
C15 C20 1.40(3) . ?
C16 C17 1.44(3) . ?
C16 C21 1.49(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.35(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.43(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.35(3) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.43(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.3900 . ?
C24 C29 1.3900 . ?
C25 C26 1.3900 . ?
C25 C30 1.47(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.3900 . ?
C27 H27 0.9500 . ?
C27 C28 1.3900 . ?
C28 H28 0.9500 . ?
C28 C29 1.3900 . ?
C29 H29 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.49(3) . ?
C32 C33 1.37(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.35(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.32(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.37(3) . ?
C36 C37 1.49(3) . ?
C37 C38 1.39(3) . ?
C38 H38 0.9500 . ?
C38 C39 1.36(3) . ?
C39 H39 0.9500 . ?
C39 C40 1.38(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.37(3) . ?
C41 C42 1.53(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.53(3) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.3900 . ?
C45 C50 1.3900 . ?
C46 C47 1.3900 . ?
C46 C51 1.49(3) . ?
C47 H47 0.9500 . ?
C47 C48 1.3900 . ?
C48 H48 0.9500 . ?
C48 C49 1.3900 . ?
C49 H49 0.9500 . ?
C49 C50 1.3900 . ?
C50 H50 0.9500 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52 C53 1.51(3) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C55 1.3900 . ?
C54 C59 1.3900 . ?
C55 C56 1.3900 . ?
C55 C60 1.34(3) . ?
C56 H56 0.9500 . ?
C56 C57 1.3900 . ?
C57 H57 0.9500 . ?
C57 C58 1.3900 . ?
C58 H58 0.9500 . ?
C58 C59 1.3900 . ?
C59 H59 0.9500 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 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
O1 Np1 O2 176.1(7) . . ?
O1 Np1 O3 91.3(7) . . ?
O1 Np1 O4 91.3(8) . . ?
O1 Np1 O5 87.7(7) . . ?
O1 Np1 O6 94.2(6) . . ?
O1 Np1 N2 86.3(6) . . ?
O1 Np1 N3 90.1(7) . . ?
O2 Np1 O3 87.2(6) . . ?
O2 Np1 O4 90.6(7) . . ?
O2 Np1 O5 94.8(6) . . ?
O2 Np1 O6 89.8(6) . . ?
O2 Np1 N2 89.8(6) . . ?
O2 Np1 N3 87.8(6) . . ?
O3 Np1 O5 62.5(5) . . ?
O3 Np1 O6 112.0(5) . . ?
O3 Np1 N2 61.8(6) . . ?
O3 Np1 N3 123.7(5) . . ?
O4 Np1 O3 174.7(6) . . ?
O4 Np1 O5 112.9(6) . . ?
O4 Np1 O6 63.1(6) . . ?
O4 Np1 N2 123.1(6) . . ?
O4 Np1 N3 61.0(5) . . ?
O5 Np1 O6 50.2(5) . . ?
O5 Np1 N2 123.7(6) . . ?
O5 Np1 N3 173.5(5) . . ?
O6 Np1 N2 173.8(6) . . ?
O6 Np1 N3 124.0(5) . . ?
N2 Np1 N3 62.1(6) . . ?
O8 Np2 O9 179.3(8) . . ?
O8 Np2 O10 87.6(7) . . ?
O8 Np2 O11 89.8(7) . . ?
O8 Np2 O12 91.4(6) . . ?
O8 Np2 O13 89.4(6) . . ?
O8 Np2 N7 87.7(6) . . ?
O8 Np2 N8 93.8(6) . . ?
O9 Np2 O10 93.0(7) . . ?
O9 Np2 O11 89.6(7) . . ?
O9 Np2 O12 89.2(6) . . ?
O9 Np2 O13 90.7(6) . . ?
O9 Np2 N7 92.2(6) . . ?
O9 Np2 N8 85.5(7) . . ?
O10 Np2 O11 175.8(6) . . ?
O10 Np2 O12 63.1(6) . . ?
O10 Np2 O13 114.2(6) . . ?
O10 Np2 N7 60.9(6) . . ?
O10 Np2 N8 121.0(6) . . ?
O11 Np2 O12 113.6(5) . . ?
O11 Np2 O13 62.4(5) . . ?
O11 Np2 N7 122.4(6) . . ?
O11 Np2 N8 62.5(6) . . ?
O12 Np2 N7 124.0(6) . . ?
O12 Np2 N8 173.4(6) . . ?
O13 Np2 O12 51.3(5) . . ?
O13 Np2 N7 174.4(6) . . ?
O13 Np2 N8 124.8(6) . . ?
N8 Np2 N7 60.3(6) . . ?
O15 Np3 O16 178.2(8) . . ?
O15 Np3 O17 92.0(7) . . ?
O15 Np3 O18 84.9(7) . . ?
O15 Np3 O20 92.5(8) . . ?
O15 Np3 O21 90.6(7) . . ?
O15 Np3 O23 92.1(7) . . ?
O15 Np3 O26 87.8(7) . . ?
O16 Np3 O17 88.9(7) . . ?
O16 Np3 O18 94.5(8) . . ?
O16 Np3 O20 88.1(9) . . ?
O16 Np3 O21 88.5(8) . . ?
O16 Np3 O23 89.7(8) . . ?
O16 Np3 O26 90.4(8) . . ?
O17 Np3 O18 51.5(6) . . ?
O20 Np3 O17 128.4(7) . . ?
O20 Np3 O18 177.4(7) . . ?
O20 Np3 O21 49.9(7) . . ?
O21 Np3 O17 176.9(7) . . ?
O21 Np3 O18 130.4(7) . . ?
O23 Np3 O17 62.2(7) . . ?
O23 Np3 O18 113.4(7) . . ?
O23 Np3 O20 66.2(7) . . ?
O23 Np3 O21 116.2(7) . . ?
O23 Np3 O26 177.8(7) . . ?
O26 Np3 O17 115.6(7) . . ?
O26 Np3 O18 64.4(7) . . ?
O26 Np3 O20 115.9(7) . . ?
O26 Np3 O21 66.0(7) . . ?
C1 O3 Np1 124.6(15) . . ?
C12 O4 Np1 131.5(16) . . ?
N5 O5 Np1 98.8(14) . . ?
N5 O6 Np1 97.7(12) . . ?
C31 O10 Np2 132.9(16) . . ?
C42 O11 Np2 122.7(15) . . ?
N10 O12 Np2 95.8(14) . . ?
N10 O13 Np2 96.6(13) . . ?
N11 O17 Np3 97.3(17) . . ?
N11 O18 Np3 96.2(17) . . ?
N12 O20 Np3 99.1(18) . . ?
N12 O21 Np3 97.7(18) . . ?
N13 O23 Np3 132.2(15) . . ?
N14 O26 Np3 135.6(15) . . ?
C1 N1 C13 119.1(19) . . ?
C1 N1 C15 127(2) . . ?
C15 N1 C13 113.1(18) . . ?
C2 N2 Np1 119.0(15) . . ?
C2 N2 C6 117.2(19) . . ?
C6 N2 Np1 123.4(14) . . ?
C7 N3 Np1 119.4(14) . . ?
C11 N3 Np1 118.8(14) . . ?
C11 N3 C7 119.6(19) . . ?
C12 N4 C22 121(2) . . ?
C12 N4 C24 126(2) . . ?
C24 N4 C22 112.7(18) . . ?
O5 N5 Np1 56.4(11) . . ?
O5 N5 O6 113.1(18) . . ?
O6 N5 Np1 56.9(10) . . ?
O7 N5 Np1 175.0(16) . . ?
O7 N5 O5 126(2) . . ?
O7 N5 O6 121(2) . . ?
C31 N6 C43 121(2) . . ?
C31 N6 C45 123(2) . . ?
C45 N6 C43 116(2) . . ?
C32 N7 Np2 119.3(15) . . ?
C32 N7 C36 117(2) . . ?
C36 N7 Np2 123.1(16) . . ?
C37 N8 Np2 125.7(17) . . ?
C37 N8 C41 116(2) . . ?
C41 N8 Np2 118.1(15) . . ?
C42 N9 C52 118(2) . . ?
C42 N9 C54 128(2) . . ?
C54 N9 C52 113.0(19) . . ?
O12 N10 Np2 58.3(11) . . ?
O13 N10 Np2 58.1(11) . . ?
O13 N10 O12 116(2) . . ?
O14 N10 Np2 176.5(14) . . ?
O14 N10 O12 122(2) . . ?
O14 N10 O13 122(2) . . ?
O17 N11 Np3 57.4(14) . . ?
O17 N11 O18 115(2) . . ?
O18 N11 Np3 57.6(14) . . ?
O19 N11 Np3 176.7(19) . . ?
O19 N11 O17 122(3) . . ?
O19 N11 O18 123(3) . . ?
O20 N12 Np3 55.5(15) . . ?
O21 N12 Np3 57.7(16) . . ?
O21 N12 O20 113(3) . . ?
O22 N12 Np3 177(2) . . ?
O22 N12 O20 127(3) . . ?
O22 N12 O21 119(3) . . ?
O24 N13 O23 120(2) . . ?
O25 N13 O23 119(2) . . ?
O25 N13 O24 121(2) . . ?
O27 N14 O26 113(2) . . ?
O27 N14 O28 129(2) . . ?
O28 N14 O26 118(2) . . ?
O3 C1 C2 114(2) . . ?
N1 C1 O3 120(2) . . ?
N1 C1 C2 126(2) . . ?
N2 C2 C1 114(2) . . ?
N2 C2 C3 124(2) . . ?
C3 C2 C1 122(2) . . ?
C2 C3 H3 122.2 . . ?
C2 C3 C4 116(2) . . ?
C4 C3 H3 122.2 . . ?
C3 C4 H4 120.2 . . ?
C5 C4 C3 120(2) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5 118.9 . . ?
C4 C5 C6 122(2) . . ?
C6 C5 H5 118.9 . . ?
N2 C6 C7 114.5(19) . . ?
C5 C6 N2 121(2) . . ?
C5 C6 C7 125(2) . . ?
N3 C7 C6 119(2) . . ?
N3 C7 C8 122(2) . . ?
C8 C7 C6 119(2) . . ?
C7 C8 H8 121.1 . . ?
C9 C8 C7 118(2) . . ?
C9 C8 H8 121.1 . . ?
C8 C9 H9 119.9 . . ?
C8 C9 C10 120(2) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 121.7 . . ?
C11 C10 C9 117(2) . . ?
C11 C10 H10 121.7 . . ?
N3 C11 C10 124(2) . . ?
N3 C11 C12 112(2) . . ?
C10 C11 C12 124(2) . . ?
O4 C12 N4 122(2) . . ?
O4 C12 C11 114(2) . . ?
N4 C12 C11 124(2) . . ?
N1 C13 H13A 110.4 . . ?
N1 C13 H13B 110.4 . . ?
H13A C13 H13B 108.6 . . ?
C14 C13 N1 106.8(18) . . ?
C14 C13 H13A 110.4 . . ?
C14 C13 H13B 110.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 N1 120(2) . . ?
C16 C15 C20 126(3) . . ?
C20 C15 N1 113(2) . . ?
C15 C16 C17 117(2) . . ?
C15 C16 C21 129(3) . . ?
C17 C16 C21 114(3) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 120(3) . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 120.5 . . ?
C17 C18 C19 119(3) . . ?
C19 C18 H18 120.5 . . ?
C18 C19 H19 118.9 . . ?
C20 C19 C18 122(2) . . ?
C20 C19 H19 118.9 . . ?
C15 C20 H20 122.2 . . ?
C19 C20 C15 116(3) . . ?
C19 C20 H20 122.2 . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N4 C22 H22A 110.4 . . ?
N4 C22 H22B 110.4 . . ?
H22A C22 H22B 108.6 . . ?
C23 C22 N4 107(2) . . ?
C23 C22 H22A 110.4 . . ?
C23 C22 H22B 110.4 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 C25 120.1(14) . . ?
N4 C24 C29 119.9(14) . . ?
C25 C24 C29 120.0 . . ?
C24 C25 C26 120.0 . . ?
C24 C25 C30 120.9(15) . . ?
C26 C25 C30 119.1(15) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C26 C27 H27 120.0 . . ?
C26 C27 C28 120.0 . . ?
C28 C27 H27 120.0 . . ?
C27 C28 H28 120.0 . . ?
C29 C28 C27 120.0 . . ?
C29 C28 H28 120.0 . . ?
C24 C29 H29 120.0 . . ?
C28 C29 C24 120.0 . . ?
C28 C29 H29 120.0 . . ?
C25 C30 H30A 109.5 . . ?
C25 C30 H30B 109.5 . . ?
C25 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O10 C31 C32 113(2) . . ?
N6 C31 O10 120(2) . . ?
N6 C31 C32 127(3) . . ?
N7 C32 C31 112(2) . . ?
N7 C32 C33 121(2) . . ?
C33 C32 C31 126(2) . . ?
C32 C33 H33 120.7 . . ?
C34 C33 C32 119(2) . . ?
C34 C33 H33 120.7 . . ?
C33 C34 H34 119.0 . . ?
C35 C34 C33 122(2) . . ?
C35 C34 H34 119.0 . . ?
C34 C35 H35 121.2 . . ?
C34 C35 C36 118(2) . . ?
C36 C35 H35 121.2 . . ?
N7 C36 C35 123(2) . . ?
N7 C36 C37 115(2) . . ?
C35 C36 C37 122(2) . . ?
N8 C37 C36 115(2) . . ?
N8 C37 C38 123(3) . . ?
C38 C37 C36 122(2) . . ?
C37 C38 H38 121.3 . . ?
C39 C38 C37 117(2) . . ?
C39 C38 H38 121.3 . . ?
C38 C39 H39 118.3 . . ?
C38 C39 C40 123(2) . . ?
C40 C39 H39 118.3 . . ?
C39 C40 H40 123.2 . . ?
C41 C40 C39 114(2) . . ?
C41 C40 H40 123.2 . . ?
N8 C41 C40 127(2) . . ?
N8 C41 C42 110(2) . . ?
C40 C41 C42 123(2) . . ?
O11 C42 C41 114(2) . . ?
N9 C42 O11 124(3) . . ?
N9 C42 C41 121(3) . . ?
N6 C43 H43A 108.8 . . ?
N6 C43 H43B 108.8 . . ?
N6 C43 C44 114(2) . . ?
H43A C43 H43B 107.7 . . ?
C44 C43 H43A 108.8 . . ?
C44 C43 H43B 108.8 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 N6 123.0(17) . . ?
C46 C45 C50 120.0 . . ?
C50 C45 N6 116.8(17) . . ?
C45 C46 C47 120.0 . . ?
C45 C46 C51 120.0(19) . . ?
C47 C46 C51 119.8(19) . . ?
C46 C47 H47 120.0 . . ?
C48 C47 C46 120.0 . . ?
C48 C47 H47 120.0 . . ?
C47 C48 H48 120.0 . . ?
C47 C48 C49 120.0 . . ?
C49 C48 H48 120.0 . . ?
C48 C49 H49 120.0 . . ?
C50 C49 C48 120.0 . . ?
C50 C49 H49 120.0 . . ?
C45 C50 H50 120.0 . . ?
C49 C50 C45 120.0 . . ?
C49 C50 H50 120.0 . . ?
C46 C51 H51A 109.5 . . ?
C46 C51 H51B 109.5 . . ?
C46 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N9 C52 H52A 109.3 . . ?
N9 C52 H52B 109.3 . . ?
N9 C52 C53 112(2) . . ?
H52A C52 H52B 107.9 . . ?
C53 C52 H52A 109.3 . . ?
C53 C52 H52B 109.3 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C55 C54 N9 123.0(19) . . ?
C55 C54 C59 120.0 . . ?
C59 C54 N9 116.9(19) . . ?
C56 C55 C54 120.0 . . ?
C60 C55 C54 122(2) . . ?
C60 C55 C56 118(2) . . ?
C55 C56 H56 120.0 . . ?
C57 C56 C55 120.0 . . ?
C57 C56 H56 120.0 . . ?
C56 C57 H57 120.0 . . ?
C56 C57 C58 120.0 . . ?
C58 C57 H57 120.0 . . ?
C57 C58 H58 120.0 . . ?
C59 C58 C57 120.0 . . ?
C59 C58 H58 120.0 . . ?
C54 C59 H59 120.0 . . ?
C58 C59 C54 120.0 . . ?
C58 C59 H59 120.0 . . ?
C55 C60 H60A 109.5 . . ?
C55 C60 H60B 109.5 . . ?
C55 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 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
Np1 O3 C1 N1 -144.1(19) . . . . ?
Np1 O3 C1 C2 32(3) . . . . ?
Np1 O4 C12 N4 169.8(16) . . . . ?
Np1 O4 C12 C11 -5(3) . . . . ?
Np1 O5 N5 O6 4.6(19) . . . . ?
Np1 O5 N5 O7 -175(2) . . . . ?
Np1 O6 N5 O5 -4.6(19) . . . . ?
Np1 O6 N5 O7 174.8(18) . . . . ?
Np1 N2 C2 C1 -4(2) . . . . ?
Np1 N2 C2 C3 -179.5(16) . . . . ?
Np1 N2 C6 C5 -178.0(14) . . . . ?
Np1 N2 C6 C7 6(2) . . . . ?
Np1 N3 C7 C6 15(2) . . . . ?
Np1 N3 C7 C8 -163.4(15) . . . . ?
Np1 N3 C11 C10 163.7(18) . . . . ?
Np1 N3 C11 C12 -18(3) . . . . ?
Np2 O10 C31 N6 165.5(16) . . . . ?
Np2 O10 C31 C32 -14(3) . . . . ?
Np2 O11 C42 N9 -133(2) . . . . ?
Np2 O11 C42 C41 43(3) . . . . ?
Np2 O12 N10 O13 0.3(18) . . . . ?
Np2 O12 N10 O14 175.9(16) . . . . ?
Np2 O13 N10 O12 -0.3(19) . . . . ?
Np2 O13 N10 O14 -175.9(16) . . . . ?
Np2 N7 C32 C31 -7(2) . . . . ?
Np2 N7 C32 C33 172.4(15) . . . . ?
Np2 N7 C36 C35 -174.1(15) . . . . ?
Np2 N7 C36 C37 8(2) . . . . ?
Np2 N8 C37 C36 -6(3) . . . . ?
Np2 N8 C37 C38 175.3(15) . . . . ?
Np2 N8 C41 C40 -174.3(19) . . . . ?
Np2 N8 C41 C42 2(2) . . . . ?
Np3 O17 N11 O18 -1(2) . . . . ?
Np3 O17 N11 O19 -176(2) . . . . ?
Np3 O18 N11 O17 1(2) . . . . ?
Np3 O18 N11 O19 176(2) . . . . ?
Np3 O20 N12 O21 -7(3) . . . . ?
Np3 O20 N12 O22 -180(3) . . . . ?
Np3 O21 N12 O20 7(3) . . . . ?
Np3 O21 N12 O22 -180(2) . . . . ?
Np3 O23 N13 O24 12(3) . . . . ?
Np3 O23 N13 O25 -177.0(16) . . . . ?
Np3 O26 N14 O27 -5(4) . . . . ?
Np3 O26 N14 O28 177.1(17) . . . . ?
O3 C1 C2 N2 -16(3) . . . . ?
O3 C1 C2 C3 160(2) . . . . ?
O10 C31 C32 N7 12(3) . . . . ?
O10 C31 C32 C33 -167(2) . . . . ?
N1 C1 C2 N2 160(2) . . . . ?
N1 C1 C2 C3 -24(4) . . . . ?
N1 C15 C16 C17 -176(2) . . . . ?
N1 C15 C16 C21 6(4) . . . . ?
N1 C15 C20 C19 178.1(19) . . . . ?
N2 C2 C3 C4 -5(3) . . . . ?
N2 C6 C7 N3 -14(3) . . . . ?
N2 C6 C7 C8 164.3(18) . . . . ?
N3 C7 C8 C9 1(3) . . . . ?
N3 C11 C12 O4 15(3) . . . . ?
N3 C11 C12 N4 -159(2) . . . . ?
N4 C24 C25 C26 -177.3(18) . . . . ?
N4 C24 C25 C30 3(2) . . . . ?
N4 C24 C29 C28 177.3(18) . . . . ?
N6 C31 C32 N7 -168(2) . . . . ?
N6 C31 C32 C33 13(4) . . . . ?
N6 C45 C46 C47 -174.6(19) . . . . ?
N6 C45 C46 C51 1(2) . . . . ?
N6 C45 C50 C49 175.0(17) . . . . ?
N7 C32 C33 C34 3(3) . . . . ?
N7 C36 C37 N8 -2(3) . . . . ?
N7 C36 C37 C38 177(2) . . . . ?
N8 C37 C38 C39 1(3) . . . . ?
N8 C41 C42 O11 -26(3) . . . . ?
N8 C41 C42 N9 150(2) . . . . ?
N9 C54 C55 C56 177(2) . . . . ?
N9 C54 C55 C60 0(2) . . . . ?
N9 C54 C59 C58 -177.1(18) . . . . ?
C1 N1 C13 C14 84(3) . . . . ?
C1 N1 C15 C16 109(3) . . . . ?
C1 N1 C15 C20 -62(3) . . . . ?
C1 C2 C3 C4 179.8(19) . . . . ?
C2 N2 C6 C5 -5(3) . . . . ?
C2 N2 C6 C7 179.2(17) . . . . ?
C2 C3 C4 C5 0(3) . . . . ?
C3 C4 C5 C6 2(3) . . . . ?
C4 C5 C6 N2 1(3) . . . . ?
C4 C5 C6 C7 175.8(18) . . . . ?
C5 C6 C7 N3 170.8(19) . . . . ?
C5 C6 C7 C8 -11(3) . . . . ?
C6 N2 C2 C1 -176.8(18) . . . . ?
C6 N2 C2 C3 7(3) . . . . ?
C6 C7 C8 C9 -177.4(18) . . . . ?
C7 N3 C11 C10 1(4) . . . . ?
C7 N3 C11 C12 179.1(19) . . . . ?
C7 C8 C9 C10 -1(3) . . . . ?
C8 C9 C10 C11 1(3) . . . . ?
C9 C10 C11 N3 -1(4) . . . . ?
C9 C10 C11 C12 -179(2) . . . . ?
C10 C11 C12 O4 -167(2) . . . . ?
C10 C11 C12 N4 19(4) . . . . ?
C11 N3 C7 C6 177.5(19) . . . . ?
C11 N3 C7 C8 -1(3) . . . . ?
C12 N4 C22 C23 64(3) . . . . ?
C12 N4 C24 C25 70(3) . . . . ?
C12 N4 C24 C29 -107(2) . . . . ?
C13 N1 C1 O3 -2(4) . . . . ?
C13 N1 C1 C2 -177(2) . . . . ?
C13 N1 C15 C16 -84(3) . . . . ?
C13 N1 C15 C20 104(2) . . . . ?
C15 N1 C1 O3 165(2) . . . . ?
C15 N1 C1 C2 -11(4) . . . . ?
C15 N1 C13 C14 -83(2) . . . . ?
C15 C16 C17 C18 1(3) . . . . ?
C16 C15 C20 C19 7(4) . . . . ?
C16 C17 C18 C19 2(4) . . . . ?
C17 C18 C19 C20 0(4) . . . . ?
C18 C19 C20 C15 -4(3) . . . . ?
C20 C15 C16 C17 -6(4) . . . . ?
C20 C15 C16 C21 176(2) . . . . ?
C21 C16 C17 C18 180(2) . . . . ?
C22 N4 C12 O4 10(4) . . . . ?
C22 N4 C12 C11 -176(2) . . . . ?
C22 N4 C24 C25 -102.4(18) . . . . ?
C22 N4 C24 C29 80.3(19) . . . . ?
C24 N4 C12 O4 -162(2) . . . . ?
C24 N4 C12 C11 12(4) . . . . ?
C24 N4 C22 C23 -124(2) . . . . ?
C24 C25 C26 C27 0.0 . . . . ?
C25 C24 C29 C28 0.0 . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C27 C28 C29 C24 0.0 . . . . ?
C29 C24 C25 C26 0.0 . . . . ?
C29 C24 C25 C30 -179.3(19) . . . . ?
C30 C25 C26 C27 179.3(18) . . . . ?
C31 N6 C43 C44 -87(3) . . . . ?
C31 N6 C45 C46 68(3) . . . . ?
C31 N6 C45 C50 -107(2) . . . . ?
C31 C32 C33 C34 -177(2) . . . . ?
C32 N7 C36 C35 2(3) . . . . ?
C32 N7 C36 C37 -176.0(18) . . . . ?
C32 C33 C34 C35 -1(3) . . . . ?
C33 C34 C35 C36 0(3) . . . . ?
C34 C35 C36 N7 0(3) . . . . ?
C34 C35 C36 C37 177.8(19) . . . . ?
C35 C36 C37 N8 -179(2) . . . . ?
C35 C36 C37 C38 0(3) . . . . ?
C36 N7 C32 C31 177.2(19) . . . . ?
C36 N7 C32 C33 -4(3) . . . . ?
C36 C37 C38 C39 -178(2) . . . . ?
C37 N8 C41 C40 4(3) . . . . ?
C37 N8 C41 C42 -180.0(19) . . . . ?
C37 C38 C39 C40 -1(4) . . . . ?
C38 C39 C40 C41 2(4) . . . . ?
C39 C40 C41 N8 -3(4) . . . . ?
C39 C40 C41 C42 -179(2) . . . . ?
C40 C41 C42 O11 150(2) . . . . ?
C40 C41 C42 N9 -34(4) . . . . ?
C41 N8 C37 C36 176.3(18) . . . . ?
C41 N8 C37 C38 -3(3) . . . . ?
C42 N9 C52 C53 86(3) . . . . ?
C42 N9 C54 C55 -62(3) . . . . ?
C42 N9 C54 C59 115(3) . . . . ?
C43 N6 C31 O10 5(4) . . . . ?
C43 N6 C31 C32 -175(2) . . . . ?
C43 N6 C45 C46 -106.2(19) . . . . ?
C43 N6 C45 C50 79(2) . . . . ?
C45 N6 C31 O10 -168(2) . . . . ?
C45 N6 C31 C32 11(4) . . . . ?
C45 N6 C43 C44 87(3) . . . . ?
C45 C46 C47 C48 0.0 . . . . ?
C46 C45 C50 C49 0.0 . . . . ?
C46 C47 C48 C49 0.0 . . . . ?
C47 C48 C49 C50 0.0 . . . . ?
C48 C49 C50 C45 0.0 . . . . ?
C50 C45 C46 C47 0.0 . . . . ?
C50 C45 C46 C51 175(2) . . . . ?
C51 C46 C47 C48 -175(2) . . . . ?
C52 N9 C42 O11 -5(4) . . . . ?
C52 N9 C42 C41 180(2) . . . . ?
C52 N9 C54 C55 108(2) . . . . ?
C52 N9 C54 C59 -75(2) . . . . ?
C54 N9 C42 O11 166(2) . . . . ?
C54 N9 C42 C41 -10(4) . . . . ?
C54 N9 C52 C53 -86(3) . . . . ?
C54 C55 C56 C57 0.0 . . . . ?
C55 C54 C59 C58 0.0 . . . . ?
C55 C56 C57 C58 0.0 . . . . ?
C56 C57 C58 C59 0.0 . . . . ?
C57 C58 C59 C54 0.0 . . . . ?
C59 C54 C55 C56 0.0 . . . . ?
C59 C54 C55 C60 -177(3) . . . . ?
C60 C55 C56 C57 177(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT020_npn4721_lt          
;
RESPONSE: The high RInt value is caused by poor diffraction 
due to low crystallinity.
;
_vrf_PLAT342_npn4721_lt          
;
RESPONSE: Low crystallinity leads to higher than expected errors 
in the determination of atomic positions.
;
_vrf_PLAT910_npn4721_lt          
;
RESPONSE: Closed by beamstop.
;
_vrf_PLAT972_npn4721_lt          
;
RESPONSE: Residual density close to the metal atom
 is caused by low crystallinity and poor diffraction data.
;
_vrf_PLAT973_npn4721_lt          
;
RESPONSE: Residual density close to the metal atom
 is caused by low crystallinity and poor diffraction data.
;
_vrf_RINTA01_npn4721_lt          
;
RESPONSE: The high RInt value is caused by poor diffraction 
due to low crystallinity.
;
####################################################################### 
# 
# 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_npn472_lt
_database_code_depnum_ccdc_archive 'CCDC 2395324'
loop_
_audit_author_name
_audit_author_address
'Mikhail Grigoriev'
;Frumkin Institute of Physical Chemistry and Electrochemistry
Russia
;
_audit_update_record             
;
2024-11-01 deposited with the CCDC.	2025-02-05 downloaded from the CCDC.
;
_audit_creation_date             2024-09-13
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H60 N12 Np3 O22, 2(C2 H3 N)'
_chemical_formula_sum            'C64 H66 N14 Np3 O22'
_chemical_formula_weight         2094.30
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Np Np -11.4937 4.1493 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.1405(18)
_cell_length_b                   13.4506(8)
_cell_length_c                   22.622(2)
_cell_angle_alpha                90
_cell_angle_beta                 123.760(2)
_cell_angle_gamma                90
_cell_volume                     7118.7(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4065
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.39
_cell_measurement_theta_min      2.67
_shelx_estimated_absorpt_T_max   0.666
_shelx_estimated_absorpt_T_min   0.537
_exptl_absorpt_coefficient_mu    4.432
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             4012
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1123
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            52580
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         4.095
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  
'Bruker KAPPA APEX II area-detector diffractometer'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6192
_reflns_number_total             8140
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.595
_refine_diff_density_min         -1.330
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         8140
_refine_ls_number_restraints     74
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0512
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0156P)²+96.6553P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0962
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29-C28 = C29A-C28A
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C31A) = Uanis(C31) = Uanis(C26) = Uanis(C25A)
Uanis(C25) = Uanis(C24) = Uanis(C28) = Uanis(C28A)
Uanis(C30) = Uanis(C30A) = Uanis(CXF) = Uanis(C26A)
Uanis(C29) = Uanis(C29A)
4. Rigid body (RIGU) restrains
 C31A, C30, C25, C26, CXF, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, C30A, C24, C25A, C26A, C28A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C31(0.5) C28A(0.5) C26A(0.5) H26A(0.5) C25A(0.5) H25A(0.5)
 C24(0.5) H24(0.5) C30A(0.5) H30A(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5)
 C31A(0.5) C28(0.5) CXF(0.5) HXF(0.5) C26(0.5) H26(0.5) C25(0.5) H25(0.5)
 C30(0.5) H30(0.5) C29A(0.5) H29D(0.5) H29E(0.5) H29F(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C22(H22A,H22B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C17(H17), C18(H18),
 C19(H19), C20(H20), C26A(H26A), C25A(H25A), C24(H24), C30A(H30A), CXF(HXF),
 C26(H26), C25(H25), C30(H30)
6.c Fitted hexagon refined as free rotating group:
 C31(C28A,C26A,C25A,C24,C30A), C31A(C28,CXF,C26,C25,C30)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C2S(H2SA,H2SB,
 H2SC), C29(H29A,H29B,H29C), C29A(H29D,H29E,H29F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Np1 Np 0.33528(2) 0.59460(2) 0.69419(2) 0.01670(8) Uani 1 1 d . . . . .
Np2 Np 0.250000 0.750000 0.500000 0.01916(10) Uani 1 2 d S . P . .
O1 O 0.2990(2) 0.6680(4) 0.6101(3) 0.0276(13) Uani 1 1 d . . . . .
O2 O 0.3698(2) 0.5208(4) 0.7738(3) 0.0234(12) Uani 1 1 d . . . . .
O3 O 0.3120(2) 0.7615(4) 0.5009(3) 0.0347(14) Uani 1 1 d . . . . .
O4 O 0.2627(2) 0.6415(4) 0.7171(3) 0.0366(15) Uani 1 1 d . . . . .
O5 O 0.4141(2) 0.5538(4) 0.6815(3) 0.0291(13) Uani 1 1 d . . . . .
O6 O 0.3542(2) 0.7532(4) 0.7687(3) 0.0263(12) Uani 1 1 d . . . . .
O7 O 0.4179(2) 0.7236(4) 0.7456(3) 0.0243(12) Uani 1 1 d . . . . .
O8 O 0.4267(2) 0.8544(4) 0.8090(3) 0.0320(14) Uani 1 1 d . . . . .
O9 O 0.2601(3) 0.5644(5) 0.4926(3) 0.0483(17) Uani 1 1 d . . . . .
O10 O 0.2030(3) 0.6349(4) 0.3921(3) 0.0347(14) Uani 1 1 d . . . . .
O11 O 0.2182(3) 0.4763(5) 0.3957(4) 0.062(2) Uani 1 1 d . . . . .
N1 N 0.2440(3) 0.4786(4) 0.6433(3) 0.0208(14) Uani 1 1 d . . . . .
N2 N 0.3275(3) 0.4294(4) 0.6251(3) 0.0193(13) Uani 1 1 d . . . . .
N3 N 0.1717(3) 0.6640(5) 0.6799(4) 0.0373(19) Uani 1 1 d . . . . .
N4 N 0.4434(3) 0.5032(4) 0.6126(3) 0.0198(14) Uani 1 1 d . . . . .
N5 N 0.4003(3) 0.7797(4) 0.7747(3) 0.0201(14) Uani 1 1 d . . . . .
N6 N 0.2264(3) 0.5555(6) 0.4254(4) 0.0408(19) Uani 1 1 d . . . . .
C1 C 0.2130(3) 0.6083(6) 0.6841(4) 0.031(2) Uani 1 1 d . . . . .
C2 C 0.2029(3) 0.5073(6) 0.6533(4) 0.0273(18) Uani 1 1 d . . . . .
C3 C 0.1597(3) 0.4431(6) 0.6411(4) 0.0297(19) Uani 1 1 d . . . . .
H3 H 0.132817 0.462898 0.651735 0.036 Uiso 1 1 calc R U . . .
C4 C 0.1565(4) 0.3507(6) 0.6135(4) 0.0294(19) Uani 1 1 d . . . . .
H4 H 0.126957 0.306026 0.604308 0.035 Uiso 1 1 calc R U . . .
C5 C 0.1961(3) 0.3231(6) 0.5994(4) 0.0261(18) Uani 1 1 d . . . . .
H5 H 0.192981 0.260902 0.577564 0.031 Uiso 1 1 calc R U . . .
C6 C 0.2410(3) 0.3879(5) 0.6175(4) 0.0215(16) Uani 1 1 d . . . . .
C7 C 0.2882(3) 0.3590(5) 0.6099(4) 0.0202(16) Uani 1 1 d . . . . .
C8 C 0.2938(4) 0.2641(5) 0.5905(4) 0.0260(18) Uani 1 1 d . . . . .
H8 H 0.266325 0.214710 0.581315 0.031 Uiso 1 1 calc R U . . .
C9 C 0.3386(4) 0.2401(6) 0.5844(4) 0.0299(19) Uani 1 1 d . . . . .
H9 H 0.342566 0.174852 0.571577 0.036 Uiso 1 1 calc R U . . .
C10 C 0.3775(3) 0.3135(5) 0.5973(4) 0.0234(17) Uani 1 1 d . . . . .
H10 H 0.408633 0.300425 0.592898 0.028 Uiso 1 1 calc R U . . .
C11 C 0.3699(3) 0.4074(5) 0.6170(4) 0.0226(16) Uani 1 1 d . . . . .
C12 C 0.4109(3) 0.4928(5) 0.6387(4) 0.0215(17) Uani 1 1 d . . . . .
C13 C 0.1877(4) 0.7641(7) 0.7122(6) 0.049(3) Uani 1 1 d . . . . .
H13A H 0.224482 0.759305 0.759096 0.059 Uiso 1 1 calc R U . . .
H13B H 0.158413 0.787021 0.720460 0.059 Uiso 1 1 calc R U . . .
C14 C 0.1935(5) 0.8401(7) 0.6683(6) 0.057(3) Uani 1 1 d . . . . .
H14A H 0.222881 0.818813 0.660528 0.085 Uiso 1 1 calc R U . . .
H14B H 0.204473 0.904079 0.693320 0.085 Uiso 1 1 calc R U . . .
H14C H 0.156875 0.847365 0.622413 0.085 Uiso 1 1 calc R U . . .
C15 C 0.1108(4) 0.6414(6) 0.6321(5) 0.037(2) Uani 1 1 d . . . . .
C16 C 0.0810(4) 0.6215(7) 0.6632(6) 0.048(3) Uani 1 1 d . . . . .
C17 C 0.0209(5) 0.6050(8) 0.6156(6) 0.057(3) Uani 1 1 d . . . . .
H17 H -0.001835 0.592464 0.633906 0.069 Uiso 1 1 calc R U . . .
C18 C -0.0040(5) 0.6074(7) 0.5433(6) 0.051(3) Uani 1 1 d . . . . .
H18 H -0.043828 0.594413 0.512392 0.061 Uiso 1 1 calc R U . . .
C19 C 0.0260(5) 0.6275(7) 0.5148(6) 0.058(3) Uani 1 1 d . . . . .
H19 H 0.006869 0.629145 0.464553 0.069 Uiso 1 1 calc R U . . .
C20 C 0.0858(4) 0.6462(6) 0.5582(5) 0.047(3) Uani 1 1 d . . . . .
H20 H 0.107393 0.661027 0.538709 0.057 Uiso 1 1 calc R U . . .
C21 C 0.1087(5) 0.6145(9) 0.7386(6) 0.069(4) Uani 1 1 d . . . . .
H21A H 0.141769 0.570034 0.758342 0.103 Uiso 1 1 calc R U . . .
H21B H 0.081795 0.587919 0.749200 0.103 Uiso 1 1 calc R U . . .
H21C H 0.121487 0.680617 0.759859 0.103 Uiso 1 1 calc R U . . .
C22 C 0.4823(3) 0.5889(5) 0.6372(4) 0.0233(17) Uani 1 1 d . . . . .
H22A H 0.515195 0.572764 0.634040 0.028 Uiso 1 1 calc R U . . .
H22B H 0.497299 0.602430 0.687666 0.028 Uiso 1 1 calc R U . . .
C23 C 0.4532(4) 0.6797(6) 0.5942(5) 0.039(2) Uani 1 1 d . . . . .
H23A H 0.421300 0.696965 0.598212 0.059 Uiso 1 1 calc R U . . .
H23B H 0.438745 0.666848 0.544254 0.059 Uiso 1 1 calc R U . . .
H23C H 0.480505 0.734962 0.611841 0.059 Uiso 1 1 calc R U . . .
N1S N 0.3755(5) 1.0128(7) 0.5467(6) 0.072(3) Uani 1 1 d . . . . .
C1S C 0.4000(4) 0.9657(8) 0.5963(6) 0.046(3) Uani 1 1 d . . . . .
C2S C 0.4304(5) 0.9028(8) 0.6601(6) 0.055(3) Uani 1 1 d . . . . .
H2SA H 0.413954 0.835758 0.648277 0.082 Uiso 1 1 calc R U . . .
H2SB H 0.426489 0.931281 0.697075 0.082 Uiso 1 1 calc R U . . .
H2SC H 0.470912 0.899370 0.677447 0.082 Uiso 1 1 calc R U . . .
C31 C 0.4330(11) 0.4536(17) 0.5498(7) 0.0353(19) Uani 0.5 1 d G . P A 2
C28A C 0.4777(8) 0.3995(16) 0.5562(5) 0.0388(19) Uani 0.5 1 d DG . P A 2
C26A C 0.4720(6) 0.3580(11) 0.4963(7) 0.039(2) Uani 0.5 1 d G . P A 2
H26A H 0.502560 0.321057 0.500700 0.047 Uiso 0.5 1 calc R U P A 2
C25A C 0.4214(6) 0.3705(9) 0.4299(5) 0.0353(19) Uani 0.5 1 d G . P A 2
H25A H 0.417485 0.342111 0.388957 0.042 Uiso 0.5 1 calc R U P A 2
C24 C 0.3767(5) 0.4245(10) 0.4235(7) 0.0388(19) Uani 0.5 1 d G . P A 2
H24 H 0.342134 0.433077 0.378118 0.047 Uiso 0.5 1 calc R U P A 2
C30A C 0.3824(8) 0.4661(13) 0.4834(10) 0.039(2) Uani 0.5 1 d G . P A 2
H30A H 0.351856 0.502990 0.479022 0.047 Uiso 0.5 1 calc R U P A 2
C29 C 0.5232(12) 0.388(6) 0.5973(19) 0.053(9) Uani 0.5 1 d D . P A 1
H29A H 0.548263 0.439327 0.598273 0.079 Uiso 0.5 1 calc R U P A 1
H29B H 0.536413 0.322281 0.593399 0.079 Uiso 0.5 1 calc R U P A 1
H29C H 0.524113 0.391036 0.641213 0.079 Uiso 0.5 1 calc R U P A 1
C31A C 0.4286(10) 0.4586(17) 0.5473(6) 0.0353(19) Uani 0.5 1 d G . P A 1
C28 C 0.4653(7) 0.4039(16) 0.5368(6) 0.0388(19) Uani 0.5 1 d DG . P A 1
CXF C 0.4463(5) 0.3677(11) 0.4696(7) 0.039(2) Uani 0.5 1 d G . P A 1
HXF H 0.471354 0.330364 0.462479 0.047 Uiso 0.5 1 calc R U P A 1
C26 C 0.3906(5) 0.3862(10) 0.4128(5) 0.0353(19) Uani 0.5 1 d G . P A 1
H26 H 0.377565 0.361462 0.366828 0.042 Uiso 0.5 1 calc R U P A 1
C25 C 0.3539(6) 0.4409(10) 0.4232(8) 0.0388(19) Uani 0.5 1 d G . P A 1
H25 H 0.315818 0.453503 0.384366 0.047 Uiso 0.5 1 calc R U P A 1
C30 C 0.3729(9) 0.4771(13) 0.4904(10) 0.039(2) Uani 0.5 1 d G . P A 1
H30 H 0.347859 0.514448 0.497557 0.047 Uiso 0.5 1 calc R U P A 1
C29A C 0.5295(13) 0.374(6) 0.6236(18) 0.053(9) Uani 0.5 1 d D . P A 2
H29D H 0.559215 0.422953 0.635524 0.079 Uiso 0.5 1 calc R U P A 2
H29E H 0.542528 0.307774 0.619898 0.079 Uiso 0.5 1 calc R U P A 2
H29F H 0.521790 0.372766 0.660800 0.079 Uiso 0.5 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Np1 O1 1.865(5) . ?
Np1 O2 1.797(5) . ?
Np1 O4 2.452(5) . ?
Np1 O5 2.451(5) . ?
Np1 O6 2.585(5) . ?
Np1 O7 2.601(5) . ?
Np1 N1 2.658(6) . ?
Np1 N2 2.655(6) . ?
Np2 O1 2.346(5) . ?
Np2 O1 2.346(5) 7_566 ?
Np2 O3 1.741(5) 7_566 ?
Np2 O3 1.741(5) . ?
Np2 O9 2.529(6) . ?
Np2 O9 2.529(6) 7_566 ?
Np2 O10 2.552(6) . ?
Np2 O10 2.552(6) 7_566 ?
O4 C1 1.246(9) . ?
O5 C12 1.235(8) . ?
O6 N5 1.278(7) . ?
O7 N5 1.270(7) . ?
O8 N5 1.235(7) . ?
O9 N6 1.274(9) . ?
O10 N6 1.261(9) . ?
O11 N6 1.211(9) . ?
N1 C2 1.351(9) . ?
N1 C6 1.335(9) . ?
N2 C7 1.347(9) . ?
N2 C11 1.338(9) . ?
N3 C1 1.341(10) . ?
N3 C13 1.477(11) . ?
N3 C15 1.462(11) . ?
N4 C12 1.342(9) . ?
N4 C22 1.470(9) . ?
N4 C31 1.445(10) . ?
N4 C31A 1.427(10) . ?
C1 C2 1.481(11) . ?
C2 C3 1.389(10) . ?
C3 H3 0.9500 . ?
C3 C4 1.371(11) . ?
C4 H4 0.9500 . ?
C4 C5 1.371(11) . ?
C5 H5 0.9500 . ?
C5 C6 1.397(10) . ?
C6 C7 1.482(10) . ?
C7 C8 1.387(10) . ?
C8 H8 0.9500 . ?
C8 C9 1.383(11) . ?
C9 H9 0.9500 . ?
C9 C10 1.379(11) . ?
C10 H10 0.9500 . ?
C10 C11 1.396(10) . ?
C11 C12 1.505(10) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.496(14) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.388(13) . ?
C15 C20 1.408(13) . ?
C16 C17 1.431(14) . ?
C16 C21 1.432(14) . ?
C17 H17 0.9500 . ?
C17 C18 1.377(14) . ?
C18 H18 0.9500 . ?
C18 C19 1.344(15) . ?
C19 H19 0.9500 . ?
C19 C20 1.422(13) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.491(11) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
N1S C1S 1.130(12) . ?
C1S C2S 1.468(14) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
C31 C28A 1.3900 . ?
C31 C30A 1.3900 . ?
C28A C26A 1.3900 . ?
C28A C29A 1.448(18) . ?
C26A H26A 0.9500 . ?
C26A C25A 1.3900 . ?
C25A H25A 0.9500 . ?
C25A C24 1.3900 . ?
C24 H24 0.9500 . ?
C24 C30A 1.3900 . ?
C30A H30A 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C29 C28 1.447(18) . ?
C31A C28 1.3900 . ?
C31A C30 1.3900 . ?
C28 CXF 1.3900 . ?
CXF HXF 0.9500 . ?
CXF C26 1.3900 . ?
C26 H26 0.9500 . ?
C26 C25 1.3900 . ?
C25 H25 0.9500 . ?
C25 C30 1.3900 . ?
C30 H30 0.9500 . ?
C29A H29D 0.9800 . ?
C29A H29E 0.9800 . ?
C29A H29F 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
O1 Np1 O4 91.8(2) . . ?
O1 Np1 O5 91.0(2) . . ?
O1 Np1 O6 91.5(2) . . ?
O1 Np1 O7 87.1(2) . . ?
O1 Np1 N1 91.1(2) . . ?
O1 Np1 N2 91.3(2) . . ?
O2 Np1 O1 178.4(2) . . ?
O2 Np1 O4 88.9(2) . . ?
O2 Np1 O5 88.5(2) . . ?
O2 Np1 O6 90.1(2) . . ?
O2 Np1 O7 94.0(2) . . ?
O2 Np1 N1 87.9(2) . . ?
O2 Np1 N2 87.1(2) . . ?
O4 Np1 O6 62.83(17) . . ?
O4 Np1 O7 112.13(17) . . ?
O4 Np1 N1 61.65(18) . . ?
O4 Np1 N2 122.27(18) . . ?
O5 Np1 O4 174.98(18) . . ?
O5 Np1 O6 112.92(17) . . ?
O5 Np1 O7 63.83(16) . . ?
O5 Np1 N1 122.48(18) . . ?
O5 Np1 N2 61.82(18) . . ?
O6 Np1 O7 49.40(15) . . ?
O6 Np1 N1 124.47(17) . . ?
O6 Np1 N2 174.07(17) . . ?
O7 Np1 N1 173.50(17) . . ?
O7 Np1 N2 125.60(17) . . ?
N2 Np1 N1 60.67(18) . . ?
O1 Np2 O1 180.0(2) 7_566 . ?
O1 Np2 O9 114.54(19) . 7_566 ?
O1 Np2 O9 114.55(19) 7_566 . ?
O1 Np2 O9 65.46(19) 7_566 7_566 ?
O1 Np2 O9 65.45(19) . . ?
O1 Np2 O10 114.60(17) . . ?
O1 Np2 O10 65.40(17) 7_566 . ?
O1 Np2 O10 114.60(17) 7_566 7_566 ?
O1 Np2 O10 65.40(17) . 7_566 ?
O3 Np2 O1 88.0(2) . 7_566 ?
O3 Np2 O1 92.0(2) 7_566 7_566 ?
O3 Np2 O1 88.0(2) 7_566 . ?
O3 Np2 O1 92.0(2) . . ?
O3 Np2 O3 180.0 . 7_566 ?
O3 Np2 O9 86.5(3) . . ?
O3 Np2 O9 93.5(3) . 7_566 ?
O3 Np2 O9 93.5(3) 7_566 . ?
O3 Np2 O9 86.5(3) 7_566 7_566 ?
O3 Np2 O10 92.7(2) 7_566 7_566 ?
O3 Np2 O10 87.3(2) . 7_566 ?
O3 Np2 O10 87.3(2) 7_566 . ?
O3 Np2 O10 92.7(2) . . ?
O9 Np2 O9 180.00(4) 7_566 . ?
O9 Np2 O10 130.14(18) . 7_566 ?
O9 Np2 O10 49.86(18) 7_566 7_566 ?
O9 Np2 O10 130.14(18) 7_566 . ?
O9 Np2 O10 49.86(18) . . ?
O10 Np2 O10 180.0 . 7_566 ?
Np1 O1 Np2 176.0(3) . . ?
C1 O4 Np1 124.8(5) . . ?
C12 O5 Np1 124.5(5) . . ?
N5 O6 Np1 97.3(4) . . ?
N5 O7 Np1 96.8(4) . . ?
N6 O9 Np2 97.8(5) . . ?
N6 O10 Np2 97.0(5) . . ?
C2 N1 Np1 118.1(5) . . ?
C6 N1 Np1 122.5(5) . . ?
C6 N1 C2 118.8(6) . . ?
C7 N2 Np1 121.7(5) . . ?
C11 N2 Np1 118.5(5) . . ?
C11 N2 C7 118.6(6) . . ?
C1 N3 C13 117.4(7) . . ?
C1 N3 C15 123.3(7) . . ?
C15 N3 C13 117.7(7) . . ?
C12 N4 C22 117.5(6) . . ?
C12 N4 C31 124.6(12) . . ?
C12 N4 C31A 122.3(12) . . ?
C31 N4 C22 115.8(11) . . ?
C31A N4 C22 116.6(11) . . ?
O7 N5 O6 116.5(6) . . ?
O8 N5 O6 120.9(6) . . ?
O8 N5 O7 122.6(6) . . ?
O10 N6 O9 115.3(7) . . ?
O11 N6 O9 122.0(8) . . ?
O11 N6 O10 122.6(8) . . ?
O4 C1 N3 118.8(8) . . ?
O4 C1 C2 117.9(7) . . ?
N3 C1 C2 123.3(7) . . ?
N1 C2 C1 112.5(7) . . ?
N1 C2 C3 121.8(7) . . ?
C3 C2 C1 125.5(7) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 C2 118.8(8) . . ?
C4 C3 H3 120.6 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.7(7) . . ?
C5 C4 H4 120.1 . . ?
C4 C5 H5 120.6 . . ?
C4 C5 C6 118.9(7) . . ?
C6 C5 H5 120.6 . . ?
N1 C6 C5 121.7(7) . . ?
N1 C6 C7 116.5(6) . . ?
C5 C6 C7 121.7(7) . . ?
N2 C7 C6 116.6(6) . . ?
N2 C7 C8 120.4(7) . . ?
C8 C7 C6 123.0(7) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 C7 121.1(7) . . ?
C9 C8 H8 119.5 . . ?
C8 C9 H9 120.9 . . ?
C10 C9 C8 118.3(7) . . ?
C10 C9 H9 120.9 . . ?
C9 C10 H10 121.0 . . ?
C9 C10 C11 118.1(7) . . ?
C11 C10 H10 121.0 . . ?
N2 C11 C10 123.4(7) . . ?
N2 C11 C12 111.6(6) . . ?
C10 C11 C12 124.7(7) . . ?
O5 C12 N4 120.4(7) . . ?
O5 C12 C11 118.0(7) . . ?
N4 C12 C11 121.5(7) . . ?
N3 C13 H13A 108.7 . . ?
N3 C13 H13B 108.7 . . ?
N3 C13 C14 114.2(8) . . ?
H13A C13 H13B 107.6 . . ?
C14 C13 H13A 108.7 . . ?
C14 C13 H13B 108.7 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 N3 117.0(9) . . ?
C16 C15 C20 124.4(9) . . ?
C20 C15 N3 118.5(8) . . ?
C15 C16 C17 116.4(10) . . ?
C15 C16 C21 122.3(10) . . ?
C17 C16 C21 121.2(10) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 C16 119.9(10) . . ?
C18 C17 H17 120.1 . . ?
C17 C18 H18 118.9 . . ?
C19 C18 C17 122.2(10) . . ?
C19 C18 H18 118.9 . . ?
C18 C19 H19 119.2 . . ?
C18 C19 C20 121.5(11) . . ?
C20 C19 H19 119.2 . . ?
C15 C20 C19 115.6(11) . . ?
C15 C20 H20 122.2 . . ?
C19 C20 H20 122.2 . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N4 C22 H22A 109.2 . . ?
N4 C22 H22B 109.2 . . ?
N4 C22 C23 111.8(6) . . ?
H22A C22 H22B 107.9 . . ?
C23 C22 H22A 109.2 . . ?
C23 C22 H22B 109.2 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N1S C1S C2S 178.4(12) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
C28A C31 N4 117.5(15) . . ?
C28A C31 C30A 120.0 . . ?
C30A C31 N4 122.2(14) . . ?
C31 C28A C26A 120.0 . . ?
C31 C28A C29A 124(3) . . ?
C26A C28A C29A 116(3) . . ?
C28A C26A H26A 120.0 . . ?
C28A C26A C25A 120.0 . . ?
C25A C26A H26A 120.0 . . ?
C26A C25A H25A 120.0 . . ?
C24 C25A C26A 120.0 . . ?
C24 C25A H25A 120.0 . . ?
C25A C24 H24 120.0 . . ?
C30A C24 C25A 120.0 . . ?
C30A C24 H24 120.0 . . ?
C31 C30A H30A 120.0 . . ?
C24 C30A C31 120.0 . . ?
C24 C30A H30A 120.0 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
C28 C31A N4 125.6(15) . . ?
C28 C31A C30 120.0 . . ?
C30 C31A N4 114.4(15) . . ?
C31A C28 C29 118(3) . . ?
CXF C28 C29 122(3) . . ?
CXF C28 C31A 120.0 . . ?
C28 CXF HXF 120.0 . . ?
C28 CXF C26 120.0 . . ?
C26 CXF HXF 120.0 . . ?
CXF C26 H26 120.0 . . ?
C25 C26 CXF 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C25 H25 120.0 . . ?
C26 C25 C30 120.0 . . ?
C30 C25 H25 120.0 . . ?
C31A C30 H30 120.0 . . ?
C25 C30 C31A 120.0 . . ?
C25 C30 H30 120.0 . . ?
C28A C29A H29D 109.5 . . ?
C28A C29A H29E 109.5 . . ?
C28A C29A H29F 109.5 . . ?
H29D C29A H29E 109.5 . . ?
H29D C29A H29F 109.5 . . ?
H29E C29A H29F 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
Np1 O4 C1 N3 -153.6(6) . . . . ?
Np1 O4 C1 C2 28.3(11) . . . . ?
Np1 O5 C12 N4 151.2(5) . . . . ?
Np1 O5 C12 C11 -28.9(9) . . . . ?
Np1 O6 N5 O7 -0.7(6) . . . . ?
Np1 O6 N5 O8 -178.5(6) . . . . ?
Np1 O7 N5 O6 0.7(6) . . . . ?
Np1 O7 N5 O8 178.5(6) . . . . ?
Np1 N1 C2 C1 7.5(9) . . . . ?
Np1 N1 C2 C3 -167.3(6) . . . . ?
Np1 N1 C6 C5 171.7(5) . . . . ?
Np1 N1 C6 C7 -7.6(9) . . . . ?
Np1 N2 C7 C6 14.3(8) . . . . ?
Np1 N2 C7 C8 -163.6(5) . . . . ?
Np1 N2 C11 C10 164.3(6) . . . . ?
Np1 N2 C11 C12 -10.0(8) . . . . ?
Np2 O9 N6 O10 -0.7(8) . . . . ?
Np2 O9 N6 O11 178.6(8) . . . . ?
Np2 O10 N6 O9 0.7(8) . . . . ?
Np2 O10 N6 O11 -178.6(8) . . . . ?
O4 C1 C2 N1 -22.1(11) . . . . ?
O4 C1 C2 C3 152.5(8) . . . . ?
N1 C2 C3 C4 -4.6(12) . . . . ?
N1 C6 C7 N2 -4.3(10) . . . . ?
N1 C6 C7 C8 173.4(7) . . . . ?
N2 C7 C8 C9 -2.0(11) . . . . ?
N2 C11 C12 O5 24.3(10) . . . . ?
N2 C11 C12 N4 -155.8(7) . . . . ?
N3 C1 C2 N1 159.9(8) . . . . ?
N3 C1 C2 C3 -25.5(14) . . . . ?
N3 C15 C16 C17 176.6(8) . . . . ?
N3 C15 C16 C21 -5.3(14) . . . . ?
N3 C15 C20 C19 -177.5(7) . . . . ?
N4 C31 C28A C26A -174.0(18) . . . . ?
N4 C31 C28A C29A 13(3) . . . . ?
N4 C31 C30A C24 173.7(19) . . . . ?
N4 C31A C28 C29 2(3) . . . . ?
N4 C31A C28 CXF -177(2) . . . . ?
N4 C31A C30 C25 177.6(18) . . . . ?
C1 N3 C13 C14 77.9(11) . . . . ?
C1 N3 C15 C16 118.1(10) . . . . ?
C1 N3 C15 C20 -65.1(12) . . . . ?
C1 C2 C3 C4 -178.7(8) . . . . ?
C2 N1 C6 C5 1.3(11) . . . . ?
C2 N1 C6 C7 -178.0(7) . . . . ?
C2 C3 C4 C5 0.7(12) . . . . ?
C3 C4 C5 C6 3.8(12) . . . . ?
C4 C5 C6 N1 -5.0(11) . . . . ?
C4 C5 C6 C7 174.2(7) . . . . ?
C5 C6 C7 N2 176.4(7) . . . . ?
C5 C6 C7 C8 -5.8(11) . . . . ?
C6 N1 C2 C1 178.3(7) . . . . ?
C6 N1 C2 C3 3.6(12) . . . . ?
C6 C7 C8 C9 -179.7(7) . . . . ?
C7 N2 C11 C10 -3.9(11) . . . . ?
C7 N2 C11 C12 -178.1(6) . . . . ?
C7 C8 C9 C10 -0.7(12) . . . . ?
C8 C9 C10 C11 1.0(11) . . . . ?
C9 C10 C11 N2 1.3(12) . . . . ?
C9 C10 C11 C12 174.7(7) . . . . ?
C10 C11 C12 O5 -149.9(8) . . . . ?
C10 C11 C12 N4 30.1(11) . . . . ?
C11 N2 C7 C6 -178.0(6) . . . . ?
C11 N2 C7 C8 4.1(10) . . . . ?
C12 N4 C22 C23 -85.7(8) . . . . ?
C12 N4 C31 C28A -126.7(10) . . . . ?
C12 N4 C31 C30A 59.5(17) . . . . ?
C12 N4 C31A C28 -132.0(11) . . . . ?
C12 N4 C31A C30 50.6(15) . . . . ?
C13 N3 C1 O4 2.8(13) . . . . ?
C13 N3 C1 C2 -179.2(8) . . . . ?
C13 N3 C15 C16 -76.7(11) . . . . ?
C13 N3 C15 C20 100.2(10) . . . . ?
C15 N3 C1 O4 168.1(8) . . . . ?
C15 N3 C1 C2 -13.9(14) . . . . ?
C15 N3 C13 C14 -88.2(10) . . . . ?
C15 C16 C17 C18 1.4(15) . . . . ?
C16 C15 C20 C19 -0.9(13) . . . . ?
C16 C17 C18 C19 -1.8(16) . . . . ?
C17 C18 C19 C20 0.8(16) . . . . ?
C18 C19 C20 C15 0.5(14) . . . . ?
C20 C15 C16 C17 0.0(14) . . . . ?
C20 C15 C16 C21 178.1(10) . . . . ?
C21 C16 C17 C18 -176.8(10) . . . . ?
C22 N4 C12 O5 0.1(11) . . . . ?
C22 N4 C12 C11 -179.8(6) . . . . ?
C22 N4 C31 C28A 70.1(12) . . . . ?
C22 N4 C31 C30A -103.7(13) . . . . ?
C22 N4 C31A C28 70.0(15) . . . . ?
C22 N4 C31A C30 -107.5(11) . . . . ?
C31 N4 C12 O5 -162.8(13) . . . . ?
C31 N4 C12 C11 17.2(15) . . . . ?
C31 N4 C22 C23 78.7(13) . . . . ?
C31 C28A C26A C25A 0.0 . . . . ?
C28A C31 C30A C24 0.0 . . . . ?
C28A C26A C25A C24 0.0 . . . . ?
C26A C25A C24 C30A 0.0 . . . . ?
C25A C24 C30A C31 0.0 . . . . ?
C30A C31 C28A C26A 0.0 . . . . ?
C30A C31 C28A C29A -173(4) . . . . ?
C29 C28 CXF C26 -179(3) . . . . ?
C31A N4 C12 O5 -157.8(13) . . . . ?
C31A N4 C12 C11 22.3(15) . . . . ?
C31A N4 C22 C23 73.4(13) . . . . ?
C31A C28 CXF C26 0.0 . . . . ?
C28 C31A C30 C25 0.0 . . . . ?
C28 CXF C26 C25 0.0 . . . . ?
CXF C26 C25 C30 0.0 . . . . ?
C26 C25 C30 C31A 0.0 . . . . ?
C30 C31A C28 C29 179(3) . . . . ?
C30 C31A C28 CXF 0.0 . . . . ?
C29A C28A C26A C25A 174(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT910_npn472_lt           
;
RESPONSE: Closed by beamstop.
;
