# 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. 
# 
#######################################################################

data_1
_audit_block_doi                 10.5517/ccdc.csd.cc2kqj83
_database_code_depnum_ccdc_archive 'CCDC 2375135'
loop_
_audit_author_name
_audit_author_address
'Mingze Meng'
;ou University
China
;
_audit_update_record             
;
2024-08-01 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_audit_creation_date             2024-07-31
_audit_creation_method           
;
FinalCif V119 by Daniel Kratzert, Freiburg 2024,
https://dkratzert.de/finalcif.html
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C6 H24 N6 Ni), B28 H12 O74 V10'
_chemical_formula_sum            'C12 H66 B28 N12 Ni2 O74 V10'
_chemical_formula_weight         2492.26
_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'
B B 0.0013 0.0007 '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'
Ni Ni 0.3393 1.1124 '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'
V V 0.3005 0.5294 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   20.0146(19)
_cell_length_b                   25.470(2)
_cell_length_c                   12.7134(12)
_cell_angle_alpha                90
_cell_angle_beta                 122.660(2)
_cell_angle_gamma                90
_cell_volume                     5456.2(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      2.49
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.252
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5553
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction:
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    1.517
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       blcok
_exptl_crystal_F_000             2480
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26044
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.091
_diffrn_reflns_theta_max         25.091
_diffrn_reflns_theta_min         2.417
_diffrn_ambient_environment      ?
_diffrn_ambient_temperature      293
_diffrn_detector                 ?
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_ambient_temperature_device_make ?
_diffrn_measurement_device       ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_measurement_specimen_support ?
_diffrn_radiation_monochromator  ?
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              ?
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4354
_reflns_number_total             4915
_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 V8.38A (Bruker, 2018)'
_computing_data_collection       
'Bruker BIS 8.5.0.27 Release/2023-03-20 && APEX5 2023.9-2'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.774
_refine_diff_density_min         -1.671
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4915
_refine_ls_number_restraints     537
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0938
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0586P)²+195.3011P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2198
_refine_ls_wR_factor_ref         0.2245
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 O17-B8
 1.45 with sigma of 0.01
2. Rigid bond restraints
 C3, C3
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.04
 C1, C2
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.04
 C2, C1
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.04
 O17, B8
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.04
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2: within 2A with sigma of 0.007 and sigma for terminal atoms of
0.001 within 2A
All non-hydrogen atoms have similar U: within 2A with sigma of 0.1 and sigma
for terminal atoms of 0.2 within 2A
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O17
\\sim O18 \\sim O19 \\sim O20: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3.8A
Uanis(O17) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O16) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O15) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
Uanis(C3) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), C1(H1C,H1D), C2(H2C,H2D), C3(H3C,H3D)
4.b Tetrahedral OH refined with riding coordinates:
 O17(H17)
4.c Idealised tetrahedral OH refined as rotating group:
 O16(H16), O20(H20)
;
_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
Ni1 Ni 0.500000 0.81749(6) 1.000000 0.0321(4) Uani 1 2 d S T P . .
N1 N 0.4858(6) 0.7612(4) 0.8653(9) 0.053(2) Uani 1 1 d . U . . .
H1A H 0.481324 0.729043 0.888178 0.063 Uiso 1 1 calc R U . . .
H1B H 0.442523 0.768220 0.790941 0.063 Uiso 1 1 calc R U . . .
N2 N 0.6196(5) 0.8130(3) 1.0543(8) 0.043(2) Uani 1 1 d . U . . .
H2A H 0.633552 0.842789 1.034641 0.052 Uiso 1 1 calc R U . . .
H2B H 0.650385 0.808757 1.136672 0.052 Uiso 1 1 calc R U . . .
N3 N 0.5238(5) 0.8798(3) 1.1251(8) 0.046(2) Uani 1 1 d . U . . .
H3A H 0.484724 0.882787 1.138542 0.055 Uiso 1 1 calc R U . . .
H3B H 0.568883 0.873814 1.197852 0.055 Uiso 1 1 calc R U . . .
C1 C 0.5578(7) 0.7651(5) 0.8597(11) 0.061(3) Uani 1 1 d . U . . .
H1C H 0.553988 0.795730 0.811356 0.073 Uiso 1 1 calc R U . . .
H1D H 0.562108 0.734246 0.819130 0.073 Uiso 1 1 calc R U . . .
C2 C 0.6314(7) 0.7696(5) 0.9928(11) 0.059(3) Uani 1 1 d . U . . .
H2C H 0.638855 0.737353 1.038428 0.070 Uiso 1 1 calc R U . . .
H2D H 0.678214 0.775651 0.989969 0.070 Uiso 1 1 calc R U . . .
C3 C 0.5303(7) 0.9276(4) 1.0681(10) 0.054(3) Uani 1 1 d . U . . .
H3C H 0.582910 0.929836 1.082088 0.065 Uiso 1 1 calc R U . . .
H3D H 0.522719 0.958002 1.106600 0.065 Uiso 1 1 calc R U . . .
V1 V 0.25679(8) 0.56054(5) 0.12459(12) 0.0201(3) Uani 1 1 d . U . . .
V2 V 0.34819(8) 0.65228(5) 0.26890(11) 0.0188(3) Uani 1 1 d . U . . .
V3 V 0.500000 0.68720(7) 0.500000 0.0216(4) Uani 1 2 d S TU P . .
O1 O 0.1770(3) 0.5777(2) 0.0004(5) 0.0295(13) Uani 1 1 d . U . . .
O2 O 0.3033(3) 0.7053(2) 0.2006(5) 0.0263(12) Uani 1 1 d . U . . .
O3 O 0.500000 0.7505(3) 0.500000 0.0329(19) Uani 1 2 d S TU P . .
O4 O 0.2337(5) 0.500000 0.1985(7) 0.0244(15) Uani 1 2 d S TU P . .
O5 O 0.2085(3) 0.5457(2) 0.3373(5) 0.0250(11) Uani 1 1 d . U . . .
O6 O 0.2729(3) 0.6023(2) 0.2616(5) 0.0211(10) Uani 1 1 d . U . . .
O7 O 0.3185(3) 0.5990(2) 0.4803(5) 0.0234(11) Uani 1 1 d . U . . .
O8 O 0.3959(3) 0.6614(2) 0.4490(5) 0.0221(10) Uani 1 1 d . U . . .
O9 O 0.4151(3) 0.6498(2) 0.6536(5) 0.0267(11) Uani 1 1 d . U . . .
O10 O 0.5372(3) 0.6609(2) 0.6681(5) 0.0235(11) Uani 1 1 d . U . . .
O11 O 0.5309(4) 0.6230(3) 0.8343(6) 0.0361(13) Uani 1 1 d . U . . .
O12 O 0.6014(4) 0.5454(3) 0.9362(6) 0.0369(13) Uani 1 1 d . U . . .
O13 O 0.6579(3) 0.6032(2) 0.8547(5) 0.0269(11) Uani 1 1 d . U . . .
O14 O 0.6959(5) 0.500000 0.9110(7) 0.0250(16) Uani 1 2 d S TU P . .
O15 O 0.6541(4) 0.6282(3) 1.0363(6) 0.0481(15) Uani 1 1 d . U . . .
O16 O 0.6584(5) 0.6580(4) 1.2138(8) 0.066(2) Uani 1 1 d . U . . .
H16 H 0.633625 0.654807 1.247933 0.098 Uiso 1 1 calc R U . . .
O17 O 0.5503(6) 0.5992(5) 1.0726(11) 0.110(3) Uani 1 1 d D U . . .
H17 H 0.540345 0.602565 1.126922 0.166 Uiso 1 1 calc R U . . .
O18 O 0.1919(3) 0.6380(2) 0.3313(5) 0.0208(10) Uani 1 1 d . U . . .
O19 O 0.2974(3) 0.6915(2) 0.4916(5) 0.0237(11) Uani 1 1 d . U . . .
O20 O 0.1620(3) 0.7196(2) 0.3768(6) 0.0359(15) Uani 1 1 d . U . . .
H20 H 0.180746 0.742080 0.431581 0.054 Uiso 1 1 calc R U . . .
B1 B 0.2152(7) 0.500000 0.2879(13) 0.020(3) Uani 1 2 d S TU P . .
B2 B 0.2473(6) 0.5956(4) 0.3516(9) 0.027(2) Uani 1 1 d . U . . .
B3 B 0.2191(6) 0.6830(3) 0.4022(8) 0.0229(19) Uani 1 1 d . U . . .
B4 B 0.3590(5) 0.6498(3) 0.5204(8) 0.0212(18) Uani 1 1 d . U . . .
B5 B 0.4948(6) 0.6439(4) 0.7182(8) 0.025(2) Uani 1 1 d . U . . .
B6 B 0.6115(7) 0.5998(4) 0.9124(9) 0.034(2) Uani 1 1 d . U . . .
B7 B 0.6313(9) 0.500000 0.9250(12) 0.025(3) Uani 1 2 d S TU P . .
B8 B 0.6223(7) 0.6304(5) 1.1071(10) 0.046(3) Uani 1 1 d D 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
Ni1 N1 2.132(9) 2_657 ?
Ni1 N1 2.132(9) . ?
Ni1 N2 2.107(8) . ?
Ni1 N2 2.107(8) 2_657 ?
Ni1 N3 2.110(8) . ?
Ni1 N3 2.110(8) 2_657 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.483(14) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C2 1.443(14) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C3 1.459(14) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.535(16) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 C3 1.49(2) 2_657 ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
V1 V1 3.084(3) 6_565 ?
V1 V2 2.9241(18) . ?
V1 O1 1.585(6) . ?
V1 O4 1.986(5) . ?
V1 O6 1.914(5) . ?
V1 O13 1.919(5) 2_656 ?
V1 O14 1.985(5) 5_666 ?
V2 V3 3.0034(14) . ?
V2 O2 1.595(6) . ?
V2 O6 1.935(5) . ?
V2 O8 1.962(5) . ?
V2 O10 1.992(5) 2_656 ?
V2 O13 1.960(5) 2_656 ?
V3 O3 1.612(9) . ?
V3 O8 1.933(5) 2_656 ?
V3 O8 1.933(5) . ?
V3 O10 1.963(5) 2_656 ?
V3 O10 1.963(5) . ?
O4 B1 1.372(14) . ?
O5 B1 1.364(8) . ?
O5 B2 1.450(10) . ?
O6 B2 1.495(10) . ?
O7 B2 1.482(12) . ?
O7 B4 1.465(10) . ?
O8 B4 1.476(10) . ?
O9 B4 1.441(10) . ?
O9 B5 1.351(11) . ?
O10 B5 1.379(10) . ?
O11 B5 1.353(11) . ?
O11 B6 1.486(13) . ?
O12 B6 1.455(12) . ?
O12 B7 1.346(9) . ?
O13 B6 1.463(11) . ?
O14 B7 1.397(15) . ?
O15 B6 1.510(12) . ?
O15 B8 1.355(12) . ?
O16 H16 0.8200 . ?
O16 B8 1.342(14) . ?
O17 H17 0.8200 . ?
O17 B8 1.489(9) . ?
O18 B2 1.467(11) . ?
O18 B3 1.377(10) . ?
O19 B3 1.368(11) . ?
O19 B4 1.515(10) . ?
O20 H20 0.8200 . ?
O20 B3 1.370(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 95.5(5) . 2_657 ?
N2 Ni1 N1 82.0(3) . . ?
N2 Ni1 N1 93.7(3) . 2_657 ?
N2 Ni1 N1 82.0(3) 2_657 2_657 ?
N2 Ni1 N1 93.7(3) 2_657 . ?
N2 Ni1 N2 173.7(5) . 2_657 ?
N2 Ni1 N3 92.4(4) . 2_657 ?
N2 Ni1 N3 92.3(3) 2_657 2_657 ?
N2 Ni1 N3 92.3(3) . . ?
N2 Ni1 N3 92.4(3) 2_657 . ?
N3 Ni1 N1 91.3(4) 2_657 . ?
N3 Ni1 N1 171.4(4) . . ?
N3 Ni1 N1 91.3(4) . 2_657 ?
N3 Ni1 N1 171.4(4) 2_657 2_657 ?
N3 Ni1 N3 82.6(5) 2_657 . ?
Ni1 N1 H1A 110.5 . . ?
Ni1 N1 H1B 110.5 . . ?
H1A N1 H1B 108.7 . . ?
C1 N1 Ni1 106.3(7) . . ?
C1 N1 H1A 110.5 . . ?
C1 N1 H1B 110.5 . . ?
Ni1 N2 H2A 109.5 . . ?
Ni1 N2 H2B 109.5 . . ?
H2A N2 H2B 108.1 . . ?
C2 N2 Ni1 110.7(7) . . ?
C2 N2 H2A 109.5 . . ?
C2 N2 H2B 109.5 . . ?
Ni1 N3 H3A 110.2 . . ?
Ni1 N3 H3B 110.2 . . ?
H3A N3 H3B 108.5 . . ?
C3 N3 Ni1 107.4(6) . . ?
C3 N3 H3A 110.2 . . ?
C3 N3 H3B 110.2 . . ?
N1 C1 H1C 109.8 . . ?
N1 C1 H1D 109.8 . . ?
N1 C1 C2 109.3(10) . . ?
H1C C1 H1D 108.3 . . ?
C2 C1 H1C 109.8 . . ?
C2 C1 H1D 109.8 . . ?
N2 C2 C1 108.3(10) . . ?
N2 C2 H2C 110.0 . . ?
N2 C2 H2D 110.0 . . ?
C1 C2 H2C 110.0 . . ?
C1 C2 H2D 110.0 . . ?
H2C C2 H2D 108.4 . . ?
N3 C3 C3 110.1(7) . 2_657 ?
N3 C3 H3C 109.6 . . ?
N3 C3 H3D 109.6 . . ?
C3 C3 H3C 109.6 2_657 . ?
C3 C3 H3D 109.6 2_657 . ?
H3C C3 H3D 108.2 . . ?
V2 V1 V1 143.05(4) . 6_565 ?
O1 V1 V1 106.0(2) . 6_565 ?
O1 V1 V2 111.0(2) . . ?
O1 V1 O4 108.5(3) . . ?
O1 V1 O6 109.7(3) . . ?
O1 V1 O13 108.9(3) . 2_656 ?
O1 V1 O14 109.6(3) . 5_666 ?
O4 V1 V1 39.06(17) . 6_565 ?
O4 V1 V2 123.4(2) . . ?
O6 V1 V1 123.78(16) . 6_565 ?
O6 V1 V2 40.84(15) . . ?
O6 V1 O4 88.2(2) . . ?
O6 V1 O13 81.9(2) . 2_656 ?
O6 V1 O14 140.5(3) . 5_666 ?
O13 V1 V1 124.48(18) 2_656 6_565 ?
O13 V1 V2 41.62(16) 2_656 . ?
O13 V1 O4 142.4(3) 2_656 . ?
O13 V1 O14 88.4(2) 2_656 5_666 ?
O14 V1 V1 39.02(17) 5_666 6_565 ?
O14 V1 V2 123.4(2) 5_666 . ?
O14 V1 O4 76.5(2) 5_666 . ?
V1 V2 V3 144.15(6) . . ?
O2 V2 V1 110.9(2) . . ?
O2 V2 V3 104.9(2) . . ?
O2 V2 O6 109.6(3) . . ?
O2 V2 O8 108.2(3) . . ?
O2 V2 O10 108.2(3) . 2_656 ?
O2 V2 O13 109.3(3) . 2_656 ?
O6 V2 V1 40.29(15) . . ?
O6 V2 V3 126.30(16) . . ?
O6 V2 O8 90.6(2) . . ?
O6 V2 O10 142.1(2) . 2_656 ?
O6 V2 O13 80.3(2) . 2_656 ?
O8 V2 V1 124.91(17) . . ?
O8 V2 V3 39.21(15) . . ?
O8 V2 O10 77.8(2) . 2_656 ?
O10 V2 V1 122.36(17) 2_656 . ?
O10 V2 V3 40.22(15) 2_656 . ?
O13 V2 V1 40.55(16) 2_656 . ?
O13 V2 V3 124.43(18) 2_656 . ?
O13 V2 O8 142.4(2) 2_656 . ?
O13 V2 O10 87.3(2) 2_656 2_656 ?
V2 V3 V2 145.55(8) . 2_656 ?
O3 V3 V2 107.23(4) . 2_656 ?
O3 V3 V2 107.22(4) . . ?
O3 V3 O8 109.88(17) . . ?
O3 V3 O8 109.88(17) . 2_656 ?
O3 V3 O10 109.95(17) . . ?
O3 V3 O10 109.95(17) . 2_656 ?
O8 V3 V2 124.45(17) 2_656 . ?
O8 V3 V2 39.90(15) 2_656 2_656 ?
O8 V3 V2 124.45(17) . 2_656 ?
O8 V3 V2 39.91(15) . . ?
O8 V3 O8 140.2(3) 2_656 . ?
O8 V3 O10 79.2(2) . 2_656 ?
O8 V3 O10 79.1(2) 2_656 . ?
O8 V3 O10 87.5(2) 2_656 2_656 ?
O8 V3 O10 87.5(2) . . ?
O10 V3 V2 40.94(15) . 2_656 ?
O10 V3 V2 123.60(17) 2_656 2_656 ?
O10 V3 V2 40.94(15) 2_656 . ?
O10 V3 V2 123.60(17) . . ?
O10 V3 O10 140.1(3) 2_656 . ?
V1 O4 V1 101.9(3) . 6_565 ?
B1 O4 V1 128.89(18) . . ?
B1 O4 V1 128.89(18) . 6_565 ?
B1 O5 B2 128.8(7) . . ?
V1 O6 V2 98.9(2) . . ?
B2 O6 V1 132.4(5) . . ?
B2 O6 V2 128.1(5) . . ?
B4 O7 B2 117.2(6) . . ?
V3 O8 V2 100.9(2) . . ?
B4 O8 V2 127.2(5) . . ?
B4 O8 V3 131.9(5) . . ?
B5 O9 B4 129.1(6) . . ?
V3 O10 V2 98.8(2) . 2_656 ?
B5 O10 V2 130.0(5) . 2_656 ?
B5 O10 V3 130.1(5) . . ?
B5 O11 B6 129.3(6) . . ?
B7 O12 B6 132.6(7) . . ?
V1 O13 V2 97.8(2) 2_656 2_656 ?
B6 O13 V1 131.1(5) . 2_656 ?
B6 O13 V2 131.1(5) . 2_656 ?
V1 O14 V1 102.0(3) 2_656 5_666 ?
B7 O14 V1 128.1(2) . 5_666 ?
B7 O14 V1 128.1(2) . 2_656 ?
B8 O15 B6 120.6(9) . . ?
B8 O16 H16 109.5 . . ?
B8 O17 H17 109.5 . . ?
B3 O18 B2 120.2(6) . . ?
B3 O19 B4 120.6(6) . . ?
B3 O20 H20 109.5 . . ?
O5 B1 O4 121.3(5) 6_565 . ?
O5 B1 O4 121.3(5) . . ?
O5 B1 O5 117.3(10) . 6_565 ?
O5 B2 O6 112.7(6) . . ?
O5 B2 O7 108.6(7) . . ?
O5 B2 O18 108.6(7) . . ?
O7 B2 O6 108.4(7) . . ?
O18 B2 O6 108.7(7) . . ?
O18 B2 O7 109.7(6) . . ?
O19 B3 O18 123.1(7) . . ?
O20 B3 O18 115.3(7) . . ?
O20 B3 O19 121.6(7) . . ?
O7 B4 O8 109.2(6) . . ?
O7 B4 O19 108.0(6) . . ?
O8 B4 O19 108.8(6) . . ?
O9 B4 O7 110.1(7) . . ?
O9 B4 O8 113.0(6) . . ?
O9 B4 O19 107.5(6) . . ?
O9 B5 O10 120.2(7) . . ?
O9 B5 O11 117.9(7) . . ?
O11 B5 O10 121.9(8) . . ?
O11 B6 O15 107.8(7) . . ?
O12 B6 O11 107.1(8) . . ?
O12 B6 O13 110.9(7) . . ?
O12 B6 O15 107.5(7) . . ?
O13 B6 O11 113.3(7) . . ?
O13 B6 O15 109.9(9) . . ?
O12 B7 O12 118.7(11) 6_565 . ?
O12 B7 O14 120.6(5) 6_565 . ?
O12 B7 O14 120.6(5) . . ?
O15 B8 O17 120.6(10) . . ?
O16 B8 O15 120.3(10) . . ?
O16 B8 O17 119.0(9) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O16 H16 O9 0.82 1.96 2.780(9) 173.7 2_657 yes
O17 H17 O11 0.82 1.82 2.546(14) 147.2 2_657 yes
O20 H20 O19 0.82 1.88 2.669(8) 160.1 7_566 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N1 C1 C2 43.0(11) . . . . ?
Ni1 N2 C2 C1 36.6(11) . . . . ?
Ni1 N3 C3 C3 39.5(13) . . . 2_657 ?
N1 C1 C2 N2 -54.2(13) . . . . ?
V1 O4 B1 O5 -1.6(16) 6_565 . . 6_565 ?
V1 O4 B1 O5 1.6(16) . . . . ?
V1 O4 B1 O5 173.5(7) 6_565 . . . ?
V1 O4 B1 O5 -173.5(7) . . . 6_565 ?
V1 O6 B2 O5 5.8(11) . . . . ?
V1 O6 B2 O7 126.1(6) . . . . ?
V1 O6 B2 O18 -114.7(6) . . . . ?
V1 O13 B6 O11 -153.8(6) 2_656 . . . ?
V1 O13 B6 O12 -33.3(12) 2_656 . . . ?
V1 O13 B6 O15 85.5(9) 2_656 . . . ?
V1 O14 B7 O12 -11.6(17) 2_656 . . . ?
V1 O14 B7 O12 11.6(17) 5_666 . . 6_565 ?
V1 O14 B7 O12 -173.1(7) 5_666 . . . ?
V1 O14 B7 O12 173.1(7) 2_656 . . 6_565 ?
V2 O6 B2 O5 -163.4(5) . . . . ?
V2 O6 B2 O7 -43.0(9) . . . . ?
V2 O6 B2 O18 76.2(8) . . . . ?
V2 O8 B4 O7 44.2(8) . . . . ?
V2 O8 B4 O9 167.1(5) . . . . ?
V2 O8 B4 O19 -73.5(7) . . . . ?
V2 O10 B5 O9 -173.7(5) 2_656 . . . ?
V2 O10 B5 O11 9.1(12) 2_656 . . . ?
V2 O13 B6 O11 25.6(12) 2_656 . . . ?
V2 O13 B6 O12 146.1(6) 2_656 . . . ?
V2 O13 B6 O15 -95.1(9) 2_656 . . . ?
V3 O8 B4 O7 -134.3(5) . . . . ?
V3 O8 B4 O9 -11.4(10) . . . . ?
V3 O8 B4 O19 107.9(6) . . . . ?
V3 O10 B5 O9 -8.1(12) . . . . ?
V3 O10 B5 O11 174.6(6) . . . . ?
B1 O5 B2 O6 23.8(14) . . . . ?
B1 O5 B2 O7 -96.4(10) . . . . ?
B1 O5 B2 O18 144.3(9) . . . . ?
B2 O5 B1 O4 -28.0(17) . . . . ?
B2 O5 B1 O5 147.4(8) . . . 6_565 ?
B2 O7 B4 O8 -67.9(8) . . . . ?
B2 O7 B4 O9 167.4(6) . . . . ?
B2 O7 B4 O19 50.3(8) . . . . ?
B2 O18 B3 O19 1.4(11) . . . . ?
B2 O18 B3 O20 -178.9(7) . . . . ?
B3 O18 B2 O5 142.3(7) . . . . ?
B3 O18 B2 O6 -94.7(8) . . . . ?
B3 O18 B2 O7 23.7(9) . . . . ?
B3 O19 B4 O7 -22.5(9) . . . . ?
B3 O19 B4 O8 96.0(8) . . . . ?
B3 O19 B4 O9 -141.3(7) . . . . ?
B4 O7 B2 O5 -170.4(6) . . . . ?
B4 O7 B2 O6 66.8(8) . . . . ?
B4 O7 B2 O18 -51.8(9) . . . . ?
B4 O9 B5 O10 30.8(13) . . . . ?
B4 O9 B5 O11 -151.9(8) . . . . ?
B4 O19 B3 O18 -2.1(11) . . . . ?
B4 O19 B3 O20 178.3(7) . . . . ?
B5 O9 B4 O7 101.6(9) . . . . ?
B5 O9 B4 O8 -20.8(12) . . . . ?
B5 O9 B4 O19 -140.9(8) . . . . ?
B5 O11 B6 O12 -119.4(9) . . . . ?
B5 O11 B6 O13 3.3(14) . . . . ?
B5 O11 B6 O15 125.2(9) . . . . ?
B6 O11 B5 O9 162.9(8) . . . . ?
B6 O11 B5 O10 -19.8(14) . . . . ?
B6 O12 B7 O12 -169.9(8) . . . 6_565 ?
B6 O12 B7 O14 14.7(19) . . . . ?
B6 O15 B8 O16 -176.4(9) . . . . ?
B6 O15 B8 O17 8.0(14) . . . . ?
B7 O12 B6 O11 130.4(11) . . . . ?
B7 O12 B6 O13 6.3(16) . . . . ?
B7 O12 B6 O15 -114.0(12) . . . . ?
B8 O15 B6 O11 56.0(11) . . . . ?
B8 O15 B6 O12 -59.2(11) . . . . ?
B8 O15 B6 O13 180.0(8) . . . . ?

_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 -0.012 0.000 0.500 879.1 214.6 ?
2 0.244 0.500 0.500 879.1 214.6 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT341_1                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0165 Ang.  
RESPONSE: The C-C bonds are located in the free [Ni(en)3]2+ cation and disorder
can account for the low bond precisi on.
;
####################################################################### 
# 
# 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_1_CCDC1
_audit_block_doi                 10.5517/ccdc.csd.cc2kqjb5
_database_code_depnum_ccdc_archive 'CCDC 2375137'
loop_
_audit_author_name
_audit_author_address
'Mingze Meng'
;fuzhou university
China
;
_audit_update_record             
;
2024-08-01 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_audit_creation_date             2024-07-31
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C6 H25 B26 Li2 N4 O70 V10, C3 H12 N2, 2(C2 H9 N2)'
_chemical_formula_sum            'C13 H78 B26 Li2 N10 O70 V10'
_chemical_formula_weight         2299.19
_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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   26.4843(12)
_cell_length_b                   16.0720(7)
_cell_length_c                   20.8945(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8893.9(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9865
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.033
_cell_measurement_theta_min      2.54
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4608
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55544
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.774
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_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                5294
_reflns_number_total             7855
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.815
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.251
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         7855
_refine_ls_number_restraints     470
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0722
_refine_ls_restrained_S_all      1.093
_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)+(0.1736P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2244
_refine_ls_wR_factor_ref         0.2566
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 H28-O28
 0.82 with sigma of 0.01
2. Rigid bond restraints
 N5, C3
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.04
3. Uiso/Uaniso restraints and constraints
C6 \\sim C5: within 2A with sigma of 0.007 and sigma for terminal atoms of
0.001 within 2A
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(N7) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
4. Others
 Fixed Sof: H23(0.5) H2A(0.5) H2B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C7(H7A,H7B), C3(H3A,H3B), C2(H2A,H2B), C1(H1D,H1E), C6(H6C,H6D),
 C5(H5D,H5E)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3)
5.c Tetrahedral OH refined with riding coordinates:
 O23(H23)
5.d X=CH2 refined with riding coordinates:
 N6(H6A,H6B)
5.e Idealised Me refined as rotating group:
 N5(H5A,H5B,H5C), N1(H1A,H1B,H1C), N7(H7C,H7D,H7E)
5.f Idealised tetrahedral OH refined as rotating group:
 O6(H6)
;
_atom_sites_solution_hydrogens   mixed
_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
V1 V 0.500000 0.61044(9) 0.250000 0.0189(4) Uani 1 2 d S TU P . .
V2 V 0.59302(4) 0.54287(6) 0.18746(5) 0.0198(3) Uani 1 1 d . U . . .
V3 V 0.64347(4) 0.38606(6) 0.15231(5) 0.0199(3) Uani 1 1 d . U . . .
V4 V 0.59640(4) 0.04689(6) 0.19077(5) 0.0210(3) Uani 1 1 d . U . . .
V5 V 0.500000 -0.01934(9) 0.250000 0.0215(4) Uani 1 2 d S TU P . .
V6 V 0.35408(4) 0.20089(6) 0.34665(5) 0.0179(3) Uani 1 1 d . U . . .
O1 O 0.47743(16) 0.5667(3) 0.3313(2) 0.0221(9) Uani 1 1 d . U . . .
O2 O 0.500000 0.7109(4) 0.250000 0.0336(17) Uani 1 2 d S TU P . .
O3 O 0.56869(16) 0.5778(3) 0.2714(2) 0.0235(9) Uani 1 1 d . U . . .
O4 O 0.55690(16) 0.5763(3) 0.38724(19) 0.0226(9) Uani 1 1 d . U . . .
O5 O 0.63480(17) 0.6158(3) 0.3472(2) 0.0242(10) Uani 1 1 d . U . . .
O6 O 0.72050(19) 0.6437(3) 0.3481(3) 0.0419(13) Uani 1 1 d . U . . .
H6 H 0.746582 0.617570 0.354521 0.063 Uiso 1 1 calc R U . . .
O7 O 0.69245(17) 0.5148(3) 0.3051(2) 0.0273(10) Uani 1 1 d . U . . .
O35 O 0.45767(16) 0.2205(3) 0.4352(2) 0.0255(10) Uani 1 1 d . U . . .
O8 O 0.60861(17) 0.4724(3) 0.3350(2) 0.0232(10) Uani 1 1 d . U . . .
O9 O 0.6272(2) 0.6149(3) 0.1566(2) 0.0370(12) Uani 1 1 d . U . . .
O36 O 0.63529(18) 0.4577(3) 0.2255(2) 0.0256(10) Uani 1 1 d . U . . .
O11 O 0.69403(19) 0.4154(3) 0.1152(2) 0.0362(12) Uani 1 1 d . U . . .
O12 O 0.67062(18) 0.3701(2) 0.31005(19) 0.0249(10) Uani 1 1 d . U . . .
O13 O 0.65760(18) 0.2954(2) 0.2125(2) 0.0229(10) Uani 1 1 d . U . . .
O14 O 0.67080(18) 0.2257(3) 0.3122(2) 0.0277(11) Uani 1 1 d . U . . .
O15 O 0.63583(17) 0.1343(3) 0.2291(2) 0.0244(10) Uani 1 1 d . U . . .
O16 O 0.69092(17) 0.0805(3) 0.3108(2) 0.0262(10) Uani 1 1 d . U . . .
O17 O 0.71604(19) -0.0521(3) 0.3468(3) 0.0395(13) Uani 1 1 d . U . . .
O18 O 0.63129(17) -0.0186(3) 0.3502(2) 0.0286(11) Uani 1 1 d . U . . .
O19 O 0.60715(17) 0.1254(3) 0.3379(2) 0.0269(10) Uani 1 1 d . U . . .
O20 O 0.6332(2) -0.0280(3) 0.1706(3) 0.0422(13) Uani 1 1 d . U . . .
O21 O 0.56614(17) 0.0209(3) 0.2736(2) 0.0288(10) Uani 1 1 d . U . . .
O22 O 0.55178(19) 0.0314(4) 0.3895(2) 0.0436(13) Uani 1 1 d . U . . .
O23 O 0.500000 -0.1200(4) 0.250000 0.050(2) Uani 1 2 d S TU P . .
H23 H 0.500000 -0.137009 0.287000 0.075 Uiso 0.5 1 calc R U P . .
O24 O 0.47421(16) 0.0203(3) 0.3321(2) 0.0232(10) Uani 1 1 d . U . . .
O25 O 0.4785(2) 0.0769(3) 0.4378(2) 0.0430(13) Uani 1 1 d . U . . .
O26 O 0.40464(17) 0.1258(3) 0.3785(2) 0.0256(10) Uani 1 1 d . U . . .
O27 O 0.40643(18) 0.1235(3) 0.4939(2) 0.0272(10) Uani 1 1 d . U . . .
O28 O 0.3690(2) 0.1751(3) 0.5881(2) 0.0379(12) Uani 1 1 d D U . . .
H28 H 0.369(3) 0.128(2) 0.603(4) 0.057 Uiso 1 1 d D U . . .
O29 O 0.39450(16) 0.2689(3) 0.5083(2) 0.0230(10) Uani 1 1 d . U . . .
O30 O 0.38581(17) 0.2926(2) 0.3930(2) 0.0215(10) Uani 1 1 d . U . . .
O31 O 0.30041(18) 0.1772(3) 0.3789(3) 0.0378(12) Uani 1 1 d . U . . .
O32 O 0.44972(18) 0.3640(3) 0.4557(2) 0.0306(11) Uani 1 1 d . U . . .
O33 O 0.41307(17) 0.4533(3) 0.3781(2) 0.0260(10) Uani 1 1 d . U . . .
O34 O 0.49236(16) 0.4836(3) 0.4257(2) 0.0249(10) Uani 1 1 d . U . . .
N3 N 0.4811(2) 0.6342(3) 0.4379(2) 0.0252(12) Uani 1 1 d . U . . .
H3 H 0.468720 0.622401 0.474893 0.030 Uiso 1 1 calc R U . . .
C4 C 0.4503(3) 0.7798(4) 0.4553(4) 0.0410(18) Uani 1 1 d . U . . .
H4A H 0.415193 0.763060 0.452341 0.049 Uiso 1 1 calc R U . . .
H4B H 0.460567 0.775072 0.499728 0.049 Uiso 1 1 calc R U . . .
N5 N 0.4242(4) 0.9260(5) 0.4813(4) 0.079(3) Uani 1 1 d . U . . .
H5A H 0.427798 0.978865 0.469485 0.094 Uiso 1 1 calc R U . . .
H5B H 0.435707 0.919550 0.521021 0.094 Uiso 1 1 calc R U . . .
H5C H 0.391752 0.912009 0.479784 0.094 Uiso 1 1 calc R U . . .
C7 C 0.4828(3) 0.7212(4) 0.4141(4) 0.0353(16) Uani 1 1 d . U . . .
H7A H 0.470800 0.722725 0.370249 0.042 Uiso 1 1 calc R U . . .
H7B H 0.517491 0.740618 0.414358 0.042 Uiso 1 1 calc R U . . .
C3 C 0.4553(3) 0.8683(4) 0.4344(4) 0.049(2) Uani 1 1 d . U . . .
H3A H 0.442592 0.874445 0.391083 0.059 Uiso 1 1 calc R U . . .
H3B H 0.490558 0.884558 0.434713 0.059 Uiso 1 1 calc R U . . .
B2 B 0.5903(3) 0.5574(4) 0.3352(4) 0.0217(14) Uani 1 1 d . U . . .
B3 B 0.6820(3) 0.5893(4) 0.3337(4) 0.0229(15) Uani 1 1 d . U . . .
B4 B 0.6508(3) 0.4530(4) 0.2943(4) 0.0235(14) Uani 1 1 d . U . . .
B5 B 0.6661(3) 0.2975(4) 0.2780(4) 0.0226(15) Uani 1 1 d . U . . .
B6 B 0.6497(3) 0.1415(4) 0.2973(4) 0.0238(14) Uani 1 1 d . U . . .
B7 B 0.6793(3) 0.0042(5) 0.3366(4) 0.0271(16) Uani 1 1 d . U . . .
B8 B 0.5887(3) 0.0416(5) 0.3379(4) 0.0291(15) Uani 1 1 d . U . . .
B9 B 0.5021(3) 0.0397(6) 0.3860(4) 0.0355(17) Uani 1 1 d . U . . .
B10 B 0.4370(3) 0.1366(5) 0.4355(4) 0.0268(15) Uani 1 1 d . U . . .
B11 B 0.3906(3) 0.1886(5) 0.5282(4) 0.0260(16) Uani 1 1 d . U . . .
B12 B 0.4229(3) 0.2863(4) 0.4463(3) 0.0218(14) Uani 1 1 d . U . . .
B13 B 0.4515(3) 0.4342(4) 0.4196(3) 0.0224(15) Uani 1 1 d . U . . .
B14 B 0.5035(3) 0.5620(4) 0.3912(3) 0.0211(14) Uani 1 1 d . U . . .
Li1 Li 0.6108(5) 0.6264(8) 0.4412(6) 0.039(3) Uani 1 1 d . U . . .
N1 N 0.5399(2) 0.2560(3) 0.3594(3) 0.0302(13) Uani 1 1 d . U . . .
H1A H 0.559613 0.213906 0.347510 0.036 Uiso 1 1 calc R U . . .
H1B H 0.513188 0.236213 0.380390 0.036 Uiso 1 1 calc R U . . .
H1C H 0.557121 0.290091 0.384848 0.036 Uiso 1 1 calc R U . . .
C2 C 0.500000 0.2482(6) 0.250000 0.041(2) Uani 1 2 d S TU P . .
H2A H 0.474054 0.212835 0.268281 0.049 Uiso 0.5 1 calc R U P . .
H2B H 0.525947 0.212837 0.231718 0.049 Uiso 0.5 1 calc R U P . .
C1 C 0.5225(3) 0.3026(4) 0.3013(4) 0.0380(18) Uani 1 1 d . U . . .
H1D H 0.550992 0.332485 0.283387 0.046 Uiso 1 1 calc R U . . .
H1E H 0.497515 0.343370 0.314236 0.046 Uiso 1 1 calc R U . . .
N6 N 0.5941(3) 0.7802(6) 0.2878(4) 0.078(3) Uani 1 1 d . U . . .
H6A H 0.608436 0.765485 0.322925 0.094 Uiso 1 1 calc R U . . .
H6B H 0.561746 0.784505 0.285969 0.094 Uiso 1 1 calc R U . . .
N7 N 0.7044(6) 0.7960(8) 0.1724(8) 0.152(5) Uani 1 1 d . U . . .
H7C H 0.736633 0.780915 0.175927 0.182 Uiso 1 1 calc R U . . .
H7D H 0.702675 0.848333 0.158714 0.182 Uiso 1 1 calc R U . . .
H7E H 0.688922 0.762755 0.144527 0.182 Uiso 1 1 calc R U . . .
C6 C 0.6231(4) 0.7969(6) 0.2341(5) 0.062(2) Uani 1 1 d . U . . .
H6C H 0.615741 0.853429 0.220588 0.074 Uiso 1 1 calc R U . . .
H6D H 0.611883 0.760253 0.200046 0.074 Uiso 1 1 calc R U . . .
C5 C 0.6779(4) 0.7887(6) 0.2397(6) 0.071(3) Uani 1 1 d . U . . .
H5D H 0.685915 0.735209 0.258628 0.086 Uiso 1 1 calc R U . . .
H5E H 0.690687 0.831801 0.267827 0.086 Uiso 1 1 calc R U . . .
O10 O 0.6491(3) 0.5360(6) 0.4845(3) 0.096(3) Uani 1 1 d . 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
V1 V2 2.9926(12) . ?
V1 V2 2.9926(12) 3_655 ?
V1 O1 1.934(4) . ?
V1 O1 1.934(4) 3_655 ?
V1 O2 1.615(6) . ?
V1 O3 1.946(4) 3_655 ?
V1 O3 1.946(4) . ?
V2 V3 2.9456(14) . ?
V2 O1 1.945(4) 3_655 ?
V2 O3 1.952(4) . ?
V2 O9 1.604(5) . ?
V2 O36 1.939(4) . ?
V2 O33 1.994(4) 3_655 ?
V3 V6 2.9768(14) 3_655 ?
V3 O36 1.926(4) . ?
V3 O11 1.618(5) . ?
V3 O13 1.961(4) . ?
V3 O30 1.938(4) 3_655 ?
V3 O33 1.952(4) 3_655 ?
V4 V5 3.0304(12) . ?
V4 V6 2.9081(14) 3_655 ?
V4 O15 1.924(4) . ?
V4 O20 1.605(5) . ?
V4 O21 1.953(5) . ?
V4 O24 1.977(4) 3_655 ?
V4 O26 1.924(4) 3_655 ?
V5 O21 1.932(4) . ?
V5 O21 1.932(4) 3_655 ?
V5 O23 1.618(7) . ?
V5 H23 2.043(7) 3_655 ?
V5 O24 1.953(4) . ?
V5 O24 1.953(4) 3_655 ?
V6 O13 1.982(4) 3_655 ?
V6 O15 1.929(4) 3_655 ?
V6 O26 1.922(4) . ?
V6 O30 1.953(4) . ?
V6 O31 1.619(5) . ?
O1 B14 1.430(8) . ?
O3 B2 1.486(9) . ?
O4 B2 1.435(9) . ?
O4 B14 1.434(8) . ?
O4 Li1 1.989(13) . ?
O5 B2 1.528(8) . ?
O5 B3 1.351(9) . ?
O5 Li1 2.072(13) . ?
O6 H6 0.8200 . ?
O6 B3 1.376(9) . ?
O7 B3 1.366(8) . ?
O7 B4 1.501(8) . ?
O35 B10 1.455(9) . ?
O35 B12 1.422(9) . ?
O8 B2 1.449(8) . ?
O8 B4 1.440(9) . ?
O36 B4 1.497(9) . ?
O12 B4 1.468(8) . ?
O12 B5 1.350(8) . ?
O13 B5 1.388(9) . ?
O14 B5 1.363(8) . ?
O14 B6 1.497(8) . ?
O15 B6 1.477(8) . ?
O16 B6 1.494(8) . ?
O16 B7 1.375(9) . ?
O17 B7 1.347(9) . ?
O18 B7 1.352(9) . ?
O18 B8 1.508(9) . ?
O19 B6 1.433(9) . ?
O19 B8 1.433(9) . ?
O21 B8 1.506(9) . ?
O22 B8 1.466(10) . ?
O22 B9 1.326(10) . ?
O23 H23 0.8200 . ?
O23 H23 0.8200 3_655 ?
O24 B9 1.382(9) . ?
O25 B9 1.383(10) . ?
O25 B10 1.462(9) . ?
O26 B10 1.477(9) . ?
O27 B10 1.479(9) . ?
O27 B11 1.337(9) . ?
O28 H28 0.818(10) . ?
O28 B11 1.392(9) . ?
O29 B11 1.359(8) . ?
O29 B12 1.523(8) . ?
O29 Li1 1.990(13) 5_666 ?
O30 B12 1.489(9) . ?
O32 B12 1.450(8) . ?
O32 B13 1.357(8) . ?
O33 B13 1.371(8) . ?
O34 B13 1.349(8) . ?
O34 B14 1.482(8) . ?
N3 H3 0.8600 . ?
N3 C7 1.485(8) . ?
N3 B14 1.630(9) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C7 1.540(11) . ?
C4 C3 1.494(10) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N5 H5C 0.8900 . ?
N5 C3 1.579(12) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
Li1 O10 1.989(15) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.499(9) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.506(9) 3_655 ?
C2 C1 1.506(9) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
N6 H6A 0.8600 . ?
N6 H6B 0.8600 . ?
N6 C6 1.386(13) . ?
N7 H7C 0.8900 . ?
N7 H7D 0.8900 . ?
N7 H7E 0.8900 . ?
N7 C5 1.577(18) . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C6 C5 1.462(15) . ?
C5 H5D 0.9700 . ?
C5 H5E 0.9700 . ?

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
V2 V1 V2 137.45(6) . 3_655 ?
O1 V1 V2 39.64(13) 3_655 . ?
O1 V1 V2 120.41(14) 3_655 3_655 ?
O1 V1 V2 39.64(13) . 3_655 ?
O1 V1 V2 120.41(14) . . ?
O1 V1 O1 137.3(3) 3_655 . ?
O1 V1 O3 89.34(18) 3_655 3_655 ?
O1 V1 O3 79.35(18) 3_655 . ?
O1 V1 O3 79.35(18) . 3_655 ?
O1 V1 O3 89.34(18) . . ?
O2 V1 V2 111.28(3) . . ?
O2 V1 V2 111.28(3) . 3_655 ?
O2 V1 O1 111.32(13) . 3_655 ?
O2 V1 O1 111.33(13) . . ?
O2 V1 O3 105.66(13) . . ?
O2 V1 O3 105.66(13) . 3_655 ?
O3 V1 V2 124.83(13) 3_655 . ?
O3 V1 V2 124.83(13) . 3_655 ?
O3 V1 V2 39.91(12) . . ?
O3 V1 V2 39.91(12) 3_655 3_655 ?
O3 V1 O3 148.7(3) 3_655 . ?
V3 V2 V1 142.44(5) . . ?
O1 V2 V1 39.38(12) 3_655 . ?
O1 V2 V3 123.59(13) 3_655 . ?
O1 V2 O3 78.95(18) 3_655 . ?
O1 V2 O33 85.75(18) 3_655 3_655 ?
O3 V2 V1 39.77(12) . . ?
O3 V2 V3 128.30(13) . . ?
O3 V2 O33 142.98(19) . 3_655 ?
O9 V2 V1 112.21(19) . . ?
O9 V2 V3 105.14(19) . . ?
O9 V2 O1 108.6(2) . 3_655 ?
O9 V2 O3 109.9(2) . . ?
O9 V2 O36 110.4(2) . . ?
O9 V2 O33 106.9(2) . 3_655 ?
O36 V2 V1 123.55(14) . . ?
O36 V2 V3 40.19(12) . . ?
O36 V2 O1 140.87(19) . 3_655 ?
O36 V2 O3 91.44(18) . . ?
O36 V2 O33 79.51(17) . 3_655 ?
O33 V2 V1 119.70(14) 3_655 . ?
O33 V2 V3 41.18(12) 3_655 . ?
V2 V3 V6 149.71(5) . 3_655 ?
O36 V3 V2 40.51(13) . . ?
O36 V3 V6 126.46(14) . 3_655 ?
O36 V3 O13 87.54(18) . . ?
O36 V3 O30 143.7(2) . 3_655 ?
O36 V3 O33 80.87(18) . 3_655 ?
O11 V3 V2 104.21(18) . . ?
O11 V3 V6 106.08(18) . 3_655 ?
O11 V3 O36 107.4(2) . . ?
O11 V3 O13 111.5(2) . . ?
O11 V3 O30 108.8(2) . 3_655 ?
O11 V3 O33 108.5(2) . 3_655 ?
O13 V3 V2 124.25(14) . . ?
O13 V3 V6 41.23(12) . 3_655 ?
O30 V3 V2 127.14(14) 3_655 . ?
O30 V3 V6 40.27(12) 3_655 3_655 ?
O30 V3 O13 79.22(17) 3_655 . ?
O30 V3 O33 87.89(18) 3_655 3_655 ?
O33 V3 V2 42.26(12) 3_655 . ?
O33 V3 V6 124.90(14) 3_655 3_655 ?
O33 V3 O13 140.0(2) 3_655 . ?
V6 V4 V5 142.06(5) 3_655 . ?
O15 V4 V5 122.92(14) . . ?
O15 V4 V6 41.08(12) . 3_655 ?
O15 V4 O21 90.56(19) . . ?
O15 V4 O24 140.49(19) . 3_655 ?
O20 V4 V5 110.84(19) . . ?
O20 V4 V6 107.06(19) . 3_655 ?
O20 V4 O15 109.1(2) . . ?
O20 V4 O21 108.8(2) . . ?
O20 V4 O24 110.5(2) . 3_655 ?
O20 V4 O26 107.8(2) . 3_655 ?
O21 V4 V5 38.47(13) . . ?
O21 V4 V6 127.25(14) . 3_655 ?
O21 V4 O24 77.28(18) . 3_655 ?
O24 V4 V5 39.27(12) 3_655 . ?
O24 V4 V6 123.06(13) 3_655 3_655 ?
O26 V4 V5 121.77(14) 3_655 . ?
O26 V4 V6 40.85(12) 3_655 3_655 ?
O26 V4 O15 80.80(17) 3_655 . ?
O26 V4 O21 143.3(2) 3_655 . ?
O26 V4 O24 86.96(18) 3_655 3_655 ?
V4 V5 V4 138.87(6) 3_655 . ?
V4 V5 H23 118.66(4) 3_655 3_655 ?
V4 V5 H23 99.82(4) . 3_655 ?
O21 V5 V4 122.82(15) 3_655 . ?
O21 V5 V4 38.98(14) . . ?
O21 V5 V4 122.82(15) . 3_655 ?
O21 V5 V4 38.98(14) 3_655 3_655 ?
O21 V5 O21 140.8(3) 3_655 . ?
O21 V5 H23 102.32(13) 3_655 3_655 ?
O21 V5 H23 114.01(14) . 3_655 ?
O21 V5 O24 78.34(18) 3_655 . ?
O21 V5 O24 78.35(18) . 3_655 ?
O21 V5 O24 89.05(19) 3_655 3_655 ?
O21 V5 O24 89.05(19) . . ?
O23 V5 V4 110.56(3) . 3_655 ?
O23 V5 V4 110.56(3) . . ?
O23 V5 O21 109.58(14) . 3_655 ?
O23 V5 O21 109.58(14) . . ?
O23 V5 H23 22.23(7) . 3_655 ?
O23 V5 O24 109.05(13) . 3_655 ?
O23 V5 O24 109.05(13) . . ?
O24 V5 V4 39.84(13) 3_655 . ?
O24 V5 V4 122.59(14) 3_655 3_655 ?
O24 V5 V4 122.59(14) . . ?
O24 V5 V4 39.84(13) . 3_655 ?
O24 V5 H23 88.27(14) 3_655 3_655 ?
O24 V5 H23 129.37(15) . 3_655 ?
O24 V5 O24 141.9(3) 3_655 . ?
V4 V6 V3 147.46(5) 3_655 3_655 ?
O13 V6 V3 40.70(12) 3_655 3_655 ?
O13 V6 V4 123.71(14) 3_655 3_655 ?
O15 V6 V3 123.90(13) 3_655 3_655 ?
O15 V6 V4 40.95(13) 3_655 3_655 ?
O15 V6 O13 86.31(18) 3_655 3_655 ?
O15 V6 O30 140.0(2) 3_655 . ?
O26 V6 V3 127.61(14) . 3_655 ?
O26 V6 V4 40.91(13) . 3_655 ?
O26 V6 O13 143.7(2) . 3_655 ?
O26 V6 O15 80.73(18) . 3_655 ?
O26 V6 O30 90.14(19) . . ?
O30 V6 V3 39.90(12) . 3_655 ?
O30 V6 V4 125.54(14) . 3_655 ?
O30 V6 O13 78.35(17) . 3_655 ?
O31 V6 V3 104.54(18) . 3_655 ?
O31 V6 V4 107.95(19) . 3_655 ?
O31 V6 O13 107.6(2) . 3_655 ?
O31 V6 O15 109.4(2) . 3_655 ?
O31 V6 O26 108.7(2) . . ?
O31 V6 O30 110.4(2) . . ?
V1 O1 V2 100.99(19) . 3_655 ?
B14 O1 V1 129.6(4) . . ?
B14 O1 V2 129.0(4) . 3_655 ?
V1 O3 V2 100.32(19) . . ?
B2 O3 V1 128.8(4) . . ?
B2 O3 V2 128.0(4) . . ?
B2 O4 Li1 94.2(5) . . ?
B14 O4 B2 128.1(5) . . ?
B14 O4 Li1 137.7(5) . . ?
B2 O5 Li1 88.3(5) . . ?
B3 O5 B2 119.1(5) . . ?
B3 O5 Li1 120.6(5) . . ?
B3 O6 H6 109.5 . . ?
B3 O7 B4 119.9(5) . . ?
B12 O35 B10 116.4(5) . . ?
B4 O8 B2 117.8(5) . . ?
V3 O36 V2 99.3(2) . . ?
B4 O36 V2 126.0(4) . . ?
B4 O36 V3 134.5(4) . . ?
B5 O12 B4 129.9(5) . . ?
V3 O13 V6 98.1(2) . 3_655 ?
B5 O13 V3 130.1(4) . . ?
B5 O13 V6 131.2(4) . 3_655 ?
B5 O14 B6 128.6(5) . . ?
V4 O15 V6 97.97(19) . 3_655 ?
B6 O15 V4 126.4(4) . . ?
B6 O15 V6 135.5(4) . 3_655 ?
B7 O16 B6 119.7(6) . . ?
B7 O18 B8 119.6(5) . . ?
B6 O19 B8 116.0(5) . . ?
V5 O21 V4 102.5(2) . . ?
B8 O21 V4 125.5(4) . . ?
B8 O21 V5 131.4(4) . . ?
B9 O22 B8 127.6(6) . . ?
V5 O23 H23 109.471(1) . 3_655 ?
V5 O23 H23 109.5 . . ?
H23 O23 H23 141.1 . 3_655 ?
V5 O24 V4 100.89(19) . 3_655 ?
B9 O24 V4 130.8(4) . 3_655 ?
B9 O24 V5 127.1(5) . . ?
B9 O25 B10 126.7(6) . . ?
V6 O26 V4 98.24(19) . 3_655 ?
B10 O26 V4 133.8(4) . 3_655 ?
B10 O26 V6 127.5(4) . . ?
B11 O27 B10 120.2(5) . . ?
B11 O28 H28 118(6) . . ?
B11 O29 B12 118.2(5) . . ?
B11 O29 Li1 129.4(6) . 5_666 ?
B12 O29 Li1 109.2(5) . 5_666 ?
V3 O30 V6 99.83(19) 3_655 . ?
B12 O30 V3 133.0(3) . 3_655 ?
B12 O30 V6 127.2(3) . . ?
B13 O32 B12 131.1(5) . . ?
V3 O33 V2 96.56(19) 3_655 3_655 ?
B13 O33 V2 131.0(4) . 3_655 ?
B13 O33 V3 130.6(4) . 3_655 ?
B13 O34 B14 127.9(5) . . ?
C7 N3 H3 121.4 . . ?
C7 N3 B14 117.3(5) . . ?
B14 N3 H3 121.4 . . ?
H4A C4 H4B 107.9 . . ?
C7 C4 H4A 109.3 . . ?
C7 C4 H4B 109.3 . . ?
C3 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
C3 C4 C7 111.7(7) . . ?
H5A N5 H5B 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
C3 N5 H5A 109.5 . . ?
C3 N5 H5B 109.5 . . ?
C3 N5 H5C 109.5 . . ?
N3 C7 C4 111.8(6) . . ?
N3 C7 H7A 109.3 . . ?
N3 C7 H7B 109.3 . . ?
C4 C7 H7A 109.3 . . ?
C4 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
C4 C3 N5 109.3(7) . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
N5 C3 H3A 109.8 . . ?
N5 C3 H3B 109.8 . . ?
H3A C3 H3B 108.3 . . ?
O3 B2 O5 108.0(5) . . ?
O4 B2 O3 113.3(5) . . ?
O4 B2 O5 102.7(5) . . ?
O4 B2 O8 114.1(6) . . ?
O8 B2 O3 109.6(5) . . ?
O8 B2 O5 108.7(5) . . ?
O5 B3 O6 116.1(6) . . ?
O5 B3 O7 123.7(6) . . ?
O7 B3 O6 120.2(6) . . ?
O8 B4 O7 109.7(5) . . ?
O8 B4 O36 110.0(5) . . ?
O8 B4 O12 110.0(6) . . ?
O36 B4 O7 108.2(5) . . ?
O12 B4 O7 107.8(5) . . ?
O12 B4 O36 111.1(5) . . ?
O12 B5 O13 121.7(6) . . ?
O12 B5 O14 117.7(6) . . ?
O14 B5 O13 120.7(5) . . ?
O14 B6 O16 106.3(5) . . ?
O15 B6 O14 111.3(5) . . ?
O15 B6 O16 108.1(5) . . ?
O19 B6 O14 109.6(5) . . ?
O19 B6 O15 111.2(6) . . ?
O19 B6 O16 110.2(5) . . ?
O17 B7 O16 120.0(7) . . ?
O17 B7 O18 117.7(6) . . ?
O18 B7 O16 122.3(6) . . ?
O19 B8 O18 110.3(6) . . ?
O19 B8 O21 110.0(6) . . ?
O19 B8 O22 109.4(6) . . ?
O21 B8 O18 107.9(6) . . ?
O22 B8 O18 107.6(5) . . ?
O22 B8 O21 111.5(6) . . ?
O22 B9 O24 123.6(7) . . ?
O22 B9 O25 116.6(7) . . ?
O24 B9 O25 119.6(7) . . ?
O35 B10 O25 109.0(6) . . ?
O35 B10 O26 108.9(5) . . ?
O35 B10 O27 110.0(5) . . ?
O25 B10 O26 112.7(5) . . ?
O25 B10 O27 106.9(6) . . ?
O26 B10 O27 109.3(6) . . ?
O27 B11 O28 119.2(6) . . ?
O27 B11 O29 123.7(6) . . ?
O29 B11 O28 117.1(6) . . ?
O35 B12 O29 108.8(5) . . ?
O35 B12 O30 110.8(5) . . ?
O35 B12 O32 110.2(6) . . ?
O30 B12 O29 108.9(5) . . ?
O32 B12 O29 106.6(5) . . ?
O32 B12 O30 111.5(5) . . ?
O32 B13 O33 120.8(6) . . ?
O34 B13 O32 117.6(6) . . ?
O34 B13 O33 121.6(6) . . ?
O1 B14 O4 114.7(5) . . ?
O1 B14 O34 112.0(5) . . ?
O1 B14 N3 108.1(5) . . ?
O4 B14 O34 111.2(5) . . ?
O4 B14 N3 106.3(5) . . ?
O34 B14 N3 103.9(5) . . ?
O4 Li1 O5 69.5(4) . . ?
O4 Li1 O29 126.3(7) . 5_666 ?
O4 Li1 O10 109.1(7) . . ?
O29 Li1 O5 126.4(7) 5_666 . ?
O29 Li1 O10 114.4(6) 5_666 . ?
O10 Li1 O5 102.3(6) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H2A C2 H2B 108.3 . . ?
C1 C2 H2A 109.9 3_655 . ?
C1 C2 H2A 109.9 . . ?
C1 C2 H2B 109.9 3_655 . ?
C1 C2 H2B 109.9 . . ?
C1 C2 C1 109.0(8) . 3_655 ?
N1 C1 C2 114.1(6) . . ?
N1 C1 H1D 108.7 . . ?
N1 C1 H1E 108.7 . . ?
C2 C1 H1D 108.7 . . ?
C2 C1 H1E 108.7 . . ?
H1D C1 H1E 107.6 . . ?
H6A N6 H6B 120.0 . . ?
C6 N6 H6A 120.0 . . ?
C6 N6 H6B 120.0 . . ?
H7C N7 H7D 109.5 . . ?
H7C N7 H7E 109.5 . . ?
H7D N7 H7E 109.5 . . ?
C5 N7 H7C 109.5 . . ?
C5 N7 H7D 109.5 . . ?
C5 N7 H7E 109.5 . . ?
N6 C6 H6C 107.8 . . ?
N6 C6 H6D 107.8 . . ?
N6 C6 C5 117.8(9) . . ?
H6C C6 H6D 107.2 . . ?
C5 C6 H6C 107.8 . . ?
C5 C6 H6D 107.8 . . ?
N7 C5 H5D 109.4 . . ?
N7 C5 H5E 109.4 . . ?
C6 C5 N7 111.4(10) . . ?
C6 C5 H5D 109.4 . . ?
C6 C5 H5E 109.4 . . ?
H5D C5 H5E 108.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O6 H6 O16 0.82 1.98 2.673(7) 141.4 8_765 yes
O28 H28 O18 0.818(10) 2.014(17) 2.826(7) 172(9) 5_656 yes
N5 H5B O22 0.89 2.06 2.856(10) 149.2 5_666 yes
N1 H1A O19 0.89 1.91 2.790(7) 169.2 . yes
N1 H1B O35 0.89 1.88 2.751(7) 165.6 . yes
N6 H6A O28 0.86 2.17 2.863(10) 136.9 5_666 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 O1 B14 O4 -13.8(8) . . . . ?
V1 O1 B14 O34 -141.7(4) . . . . ?
V1 O1 B14 N3 104.5(5) . . . . ?
V1 O3 B2 O4 -9.5(8) . . . . ?
V1 O3 B2 O5 -122.6(5) . . . . ?
V1 O3 B2 O8 119.1(5) . . . . ?
V2 O1 B14 O4 174.4(4) 3_655 . . . ?
V2 O1 B14 O34 46.5(7) 3_655 . . . ?
V2 O1 B14 N3 -67.4(6) 3_655 . . . ?
V2 O3 B2 O4 -166.1(4) . . . . ?
V2 O3 B2 O5 80.8(6) . . . . ?
V2 O3 B2 O8 -37.5(7) . . . . ?
V2 O36 B4 O7 -77.5(6) . . . . ?
V2 O36 B4 O8 42.3(7) . . . . ?
V2 O36 B4 O12 164.4(4) . . . . ?
V2 O33 B13 O32 -172.7(4) 3_655 . . . ?
V2 O33 B13 O34 6.7(10) 3_655 . . . ?
V3 O36 B4 O7 108.4(5) . . . . ?
V3 O36 B4 O8 -131.7(5) . . . . ?
V3 O36 B4 O12 -9.7(9) . . . . ?
V3 O13 B5 O12 -6.8(10) . . . . ?
V3 O13 B5 O14 174.0(5) . . . . ?
V3 O30 B12 O35 -138.7(4) 3_655 . . . ?
V3 O30 B12 O29 101.7(6) 3_655 . . . ?
V3 O30 B12 O32 -15.7(9) 3_655 . . . ?
V3 O33 B13 O32 -11.9(10) 3_655 . . . ?
V3 O33 B13 O34 167.5(4) 3_655 . . . ?
V4 O15 B6 O14 -167.8(4) . . . . ?
V4 O15 B6 O16 75.7(7) . . . . ?
V4 O15 B6 O19 -45.3(7) . . . . ?
V4 O21 B8 O18 -75.3(6) . . . . ?
V4 O21 B8 O19 45.2(8) . . . . ?
V4 O21 B8 O22 166.8(4) . . . . ?
V4 O24 B9 O22 -166.6(6) 3_655 . . . ?
V4 O24 B9 O25 7.2(11) 3_655 . . . ?
V4 O26 B10 O35 124.6(5) 3_655 . . . ?
V4 O26 B10 O25 3.6(9) 3_655 . . . ?
V4 O26 B10 O27 -115.2(6) 3_655 . . . ?
V5 O21 B8 O18 115.2(5) . . . . ?
V5 O21 B8 O19 -124.4(5) . . . . ?
V5 O21 B8 O22 -2.8(9) . . . . ?
V5 O24 B9 O22 -1.8(11) . . . . ?
V5 O24 B9 O25 171.9(5) . . . . ?
V6 O13 B5 O12 -176.4(5) 3_655 . . . ?
V6 O13 B5 O14 4.3(10) 3_655 . . . ?
V6 O15 B6 O14 9.4(9) 3_655 . . . ?
V6 O15 B6 O16 -107.0(6) 3_655 . . . ?
V6 O15 B6 O19 131.9(5) 3_655 . . . ?
V6 O26 B10 O35 -46.3(8) . . . . ?
V6 O26 B10 O25 -167.3(4) . . . . ?
V6 O26 B10 O27 74.0(7) . . . . ?
V6 O30 B12 O35 39.2(7) . . . . ?
V6 O30 B12 O29 -80.4(6) . . . . ?
V6 O30 B12 O32 162.2(4) . . . . ?
C7 N3 B14 O1 -56.2(7) . . . . ?
C7 N3 B14 O4 67.3(7) . . . . ?
C7 N3 B14 O34 -175.3(5) . . . . ?
C7 C4 C3 N5 -176.0(7) . . . . ?
C3 C4 C7 N3 175.6(6) . . . . ?
B2 O4 B14 O1 -31.3(9) . . . . ?
B2 O4 B14 O34 97.0(7) . . . . ?
B2 O4 B14 N3 -150.6(6) . . . . ?
B2 O5 B3 O6 -177.5(6) . . . . ?
B2 O5 B3 O7 5.1(10) . . . . ?
B2 O8 B4 O7 49.9(7) . . . . ?
B2 O8 B4 O36 -69.0(7) . . . . ?
B2 O8 B4 O12 168.3(5) . . . . ?
B3 O5 B2 O3 -96.1(6) . . . . ?
B3 O5 B2 O4 143.9(6) . . . . ?
B3 O5 B2 O8 22.7(8) . . . . ?
B3 O7 B4 O8 -18.6(8) . . . . ?
B3 O7 B4 O36 101.5(7) . . . . ?
B3 O7 B4 O12 -138.3(6) . . . . ?
B4 O7 B3 O5 -7.5(10) . . . . ?
B4 O7 B3 O6 175.2(6) . . . . ?
B4 O8 B2 O3 66.0(7) . . . . ?
B4 O8 B2 O4 -165.8(5) . . . . ?
B4 O8 B2 O5 -51.8(7) . . . . ?
B4 O12 B5 O13 24.8(11) . . . . ?
B4 O12 B5 O14 -155.9(6) . . . . ?
B5 O12 B4 O7 -134.9(7) . . . . ?
B5 O12 B4 O8 105.5(8) . . . . ?
B5 O12 B4 O36 -16.5(10) . . . . ?
B5 O14 B6 O15 19.1(10) . . . . ?
B5 O14 B6 O16 136.6(7) . . . . ?
B5 O14 B6 O19 -104.3(8) . . . . ?
B6 O14 B5 O12 154.9(6) . . . . ?
B6 O14 B5 O13 -25.8(11) . . . . ?
B6 O16 B7 O17 177.7(6) . . . . ?
B6 O16 B7 O18 0.4(10) . . . . ?
B6 O19 B8 O18 51.6(7) . . . . ?
B6 O19 B8 O21 -67.4(7) . . . . ?
B6 O19 B8 O22 169.8(5) . . . . ?
B7 O16 B6 O14 143.5(6) . . . . ?
B7 O16 B6 O15 -96.8(7) . . . . ?
B7 O16 B6 O19 24.8(8) . . . . ?
B7 O18 B8 O19 -23.8(8) . . . . ?
B7 O18 B8 O21 96.4(7) . . . . ?
B7 O18 B8 O22 -143.1(6) . . . . ?
B8 O18 B7 O16 -0.9(10) . . . . ?
B8 O18 B7 O17 -178.3(6) . . . . ?
B8 O19 B6 O14 -168.8(5) . . . . ?
B8 O19 B6 O15 67.8(7) . . . . ?
B8 O19 B6 O16 -52.1(7) . . . . ?
B8 O22 B9 O24 32.4(13) . . . . ?
B8 O22 B9 O25 -141.5(8) . . . . ?
B9 O22 B8 O18 -146.9(7) . . . . ?
B9 O22 B8 O19 93.2(9) . . . . ?
B9 O22 B8 O21 -28.8(11) . . . . ?
B9 O25 B10 O35 -92.5(8) . . . . ?
B9 O25 B10 O26 28.5(11) . . . . ?
B9 O25 B10 O27 148.6(7) . . . . ?
B10 O35 B12 O29 53.6(7) . . . . ?
B10 O35 B12 O30 -66.1(7) . . . . ?
B10 O35 B12 O32 170.1(5) . . . . ?
B10 O25 B9 O22 139.9(8) . . . . ?
B10 O25 B9 O24 -34.3(12) . . . . ?
B10 O27 B11 O28 -169.7(6) . . . . ?
B10 O27 B11 O29 9.7(10) . . . . ?
B11 O27 B10 O35 17.0(8) . . . . ?
B11 O27 B10 O25 135.3(6) . . . . ?
B11 O27 B10 O26 -102.5(7) . . . . ?
B11 O29 B12 O35 -24.7(8) . . . . ?
B11 O29 B12 O30 96.1(6) . . . . ?
B11 O29 B12 O32 -143.5(6) . . . . ?
B12 O35 B10 O25 -167.4(5) . . . . ?
B12 O35 B10 O26 69.3(7) . . . . ?
B12 O35 B10 O27 -50.5(7) . . . . ?
B12 O29 B11 O27 -5.8(10) . . . . ?
B12 O29 B11 O28 173.6(6) . . . . ?
B12 O32 B13 O33 23.7(11) . . . . ?
B12 O32 B13 O34 -155.7(7) . . . . ?
B13 O32 B12 O35 113.2(8) . . . . ?
B13 O32 B12 O29 -129.0(7) . . . . ?
B13 O32 B12 O30 -10.2(10) . . . . ?
B13 O34 B14 O1 -23.7(9) . . . . ?
B13 O34 B14 O4 -153.5(6) . . . . ?
B13 O34 B14 N3 92.6(7) . . . . ?
B14 O4 B2 O3 42.1(8) . . . . ?
B14 O4 B2 O5 158.3(5) . . . . ?
B14 O4 B2 O8 -84.2(8) . . . . ?
B14 O34 B13 O32 178.8(6) . . . . ?
B14 O34 B13 O33 -0.6(11) . . . . ?
B14 N3 C7 C4 167.3(6) . . . . ?
Li1 O4 B2 O3 -136.6(6) . . . . ?
Li1 O4 B2 O5 -20.4(6) . . . . ?
Li1 O4 B2 O8 97.1(6) . . . . ?
Li1 O4 B14 O1 146.8(7) . . . . ?
Li1 O4 B14 O34 -84.9(9) . . . . ?
Li1 O4 B14 N3 27.5(10) . . . . ?
Li1 O5 B2 O3 139.5(6) . . . . ?
Li1 O5 B2 O4 19.5(6) . . . . ?
Li1 O5 B2 O8 -101.7(6) . . . . ?
Li1 O5 B3 O6 -70.7(8) . . . . ?
Li1 O5 B3 O7 111.9(8) . . . . ?
Li1 O29 B11 O27 -163.4(7) 5_666 . . . ?
Li1 O29 B11 O28 16.0(11) 5_666 . . . ?
Li1 O29 B12 O35 137.1(6) 5_666 . . . ?
Li1 O29 B12 O30 -102.1(6) 5_666 . . . ?
Li1 O29 B12 O32 18.3(7) 5_666 . . . ?
C1 C2 C1 N1 172.1(8) 3_655 . . . ?
N6 C6 C5 N7 171.0(9) . . . . ?

_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 0.250 -0.276 0.484 418.9 236.9 ?
2 0.250 -0.396 -0.016 418.9 236.9 ?
3 0.750 -0.384 0.516 418.9 236.9 ?
4 0.750 -0.128 0.016 418.9 236.9 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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_1_CCDC2
_audit_block_doi                 10.5517/ccdc.csd.cc2kqj94
_database_code_depnum_ccdc_archive 'CCDC 2375136'
loop_
_audit_author_name
_audit_author_address
'Mingze Meng'
;fuzhou university
China
;
_audit_update_record             
;
2024-08-01 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_audit_creation_date             2024-08-01
_audit_creation_method           
;
FinalCif V119 by Daniel Kratzert, Freiburg 2024,
https://dkratzert.de/finalcif.html
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C6 H28 B26 N4 O68 V10, 2(H O), 5(C3 H12 N2), 2(C3 H11 N2)'
_chemical_formula_sum            'C27 H110 B26 N18 O70 V10'
_chemical_formula_weight         2597.78
_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'
B B 0.0013 0.0007 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   27.2018(13)
_cell_length_b                   16.3281(7)
_cell_length_c                   21.6011(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9594.2(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.54
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       blcok
_exptl_crystal_F_000             5272
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1467
_diffrn_reflns_av_unetI/netI     0.0867
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            53314
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.382
_diffrn_ambient_environment      ?
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 ?
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_ambient_temperature_device_make ?
_diffrn_measurement_device       ?
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_measurement_specimen_support ?
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           ?
_diffrn_source_type              ?
_diffrn_source_voltage           ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5616
_reflns_number_total             8462
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         8462
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0685
_refine_ls_restrained_S_all      1.039
_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)+(0.1191P)²+7.6488P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1771
_refine_ls_wR_factor_ref         0.2023
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 H9B_$6-H5C
 2.2 with sigma of 0.02
 O30-H30
 0.85 with sigma of 0.01
 O1-H1
 0.82 with sigma of 0.01
2. Others
 Fixed Sof: H5D(0.5) H5E(0.5)
3.a Free rotating group:
 O1W(H1W)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1B,H1C), C2(H2D,H2E), C3(H3A,H3B), C4(H4D,H4E), C5(H5D,H5E), C10(H10A,
 H10B), C11(H11A,H11B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1A), C9(H9)
3.d X=CH2 refined with riding coordinates:
 O18(H18A,H18B)
3.e Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N3(H3C,H3D,H3E), N6(H6C,H6D,H6E), N7(H7C,H7D,H7E), N4(H4A,
 H4B,H4C), N5(H5A,H5B,H5C), N8(H8C,H8D,H8E), N9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_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
V1 V 0.500000 -0.03606(8) 0.750000 0.0184(3) Uani 1 2 d S T P . .
V2 V 0.40876(4) 0.02715(5) 0.68478(4) 0.0172(3) Uani 1 1 d . . . . .
V3 V 0.36313(4) 0.18281(5) 0.64325(4) 0.0169(2) Uani 1 1 d . . . . .
V4 V 0.36846(4) 0.36324(5) 0.64438(4) 0.0175(3) Uani 1 1 d . . . . .
V5 V 0.41360(4) 0.51723(5) 0.68263(4) 0.0150(2) Uani 1 1 d . . . . .
V6 V 0.500000 0.58737(7) 0.750000 0.0143(3) Uani 1 2 d S T P . .
O1 O 0.71387(18) -0.0688(3) 0.6638(2) 0.0344(11) Uani 1 1 d D . . . .
H1 H 0.7407(14) -0.055(5) 0.677(4) 0.052 Uiso 1 1 d D U . . .
O2 O 0.63109(16) -0.0319(2) 0.6623(2) 0.0289(10) Uani 1 1 d . . . . .
O3 O 0.68989(14) 0.0596(2) 0.70710(18) 0.0188(9) Uani 1 1 d . . . . .
O4 O 0.61035(15) 0.1108(2) 0.67682(18) 0.0226(9) Uani 1 1 d . . . . .
O5 O 0.63432(15) 0.1125(2) 0.78437(17) 0.0197(9) Uani 1 1 d . . . . .
O6 O 0.56515(14) 0.0070(2) 0.73223(18) 0.0217(9) Uani 1 1 d . . . . .
O7 O 0.55770(17) 0.0232(3) 0.62040(19) 0.0379(12) Uani 1 1 d . . . . .
O8 O 0.500000 -0.1339(3) 0.750000 0.0388(17) Uani 1 2 d S T P . .
O9 O 0.47941(15) 0.0027(2) 0.66846(18) 0.0228(9) Uani 1 1 d . . . . .
O10 O 0.37566(17) -0.0498(2) 0.6656(2) 0.0313(11) Uani 1 1 d . . . . .
O11 O 0.48605(16) 0.0536(2) 0.56630(18) 0.0270(10) Uani 1 1 d . . . . .
O12 O 0.41213(15) 0.1038(2) 0.61660(17) 0.0217(9) Uani 1 1 d . . . . .
O13 O 0.31410(16) 0.1706(3) 0.6032(2) 0.0316(11) Uani 1 1 d . . . . .
O14 O 0.42179(16) 0.1066(2) 0.50547(17) 0.0229(9) Uani 1 1 d . . . . .
O15 O 0.47100(15) 0.1961(2) 0.57025(17) 0.0205(9) Uani 1 1 d . . . . .
O16 O 0.40042(16) 0.2714(2) 0.60575(18) 0.0210(9) Uani 1 1 d . . . . .
O17 O 0.41468(17) 0.2512(2) 0.49544(19) 0.0262(10) Uani 1 1 d . . . . .
O18 O 0.39511(19) 0.1660(2) 0.41149(19) 0.0343(11) Uani 1 1 d . . . . .
H18A H 0.391237 0.114467 0.393774 0.051 Uiso 1 1 calc R U . . .
H18B H 0.388010 0.212734 0.388592 0.051 Uiso 1 1 calc R U . . .
O19 O 0.46766(16) 0.3399(2) 0.55263(18) 0.0257(10) Uani 1 1 d . . . . .
O20 O 0.42568(16) 0.4289(2) 0.62286(17) 0.0229(9) Uani 1 1 d . . . . .
O21 O 0.50275(15) 0.4651(2) 0.57874(17) 0.0206(9) Uani 1 1 d . . . . .
O22 O 0.48260(15) 0.5453(2) 0.66961(17) 0.0176(9) Uani 1 1 d . . . . .
O23 O 0.56279(14) 0.5562(2) 0.62214(16) 0.0174(8) Uani 1 1 d . . . . .
O24 O 0.56742(15) 0.5526(2) 0.73475(16) 0.0179(8) Uani 1 1 d . . . . .
O25 O 0.500000 0.6861(3) 0.750000 0.0216(13) Uani 1 2 d S T P . .
O26 O 0.38061(17) 0.5851(2) 0.6489(2) 0.0290(10) Uani 1 1 d . . . . .
O27 O 0.63716(15) 0.5908(2) 0.67193(18) 0.0202(9) Uani 1 1 d . . . . .
O28 O 0.61009(15) 0.4500(2) 0.67522(16) 0.0169(9) Uani 1 1 d . . . . .
O29 O 0.62911(15) 0.4338(2) 0.78310(17) 0.0184(9) Uani 1 1 d . . . . .
O30 O 0.71960(17) 0.6191(3) 0.6838(3) 0.0453(14) Uani 1 1 d D . . . .
H30 H 0.743(2) 0.598(5) 0.705(4) 0.068 Uiso 1 1 d D U . . .
O31 O 0.69054(14) 0.4867(2) 0.71294(18) 0.0198(9) Uani 1 1 d . . . . .
O32 O 0.66688(16) 0.3459(2) 0.70526(17) 0.0218(9) Uani 1 1 d . . . . .
O33 O 0.65051(17) 0.2750(2) 0.79935(17) 0.0223(9) Uani 1 1 d . . . . .
O34 O 0.32366(18) 0.3878(3) 0.6006(2) 0.0355(11) Uani 1 1 d . . . . .
O35 O 0.67316(16) 0.2034(2) 0.70845(18) 0.0241(10) Uani 1 1 d . . . . .
N1 N 0.48907(19) 0.6126(3) 0.5679(2) 0.0207(11) Uani 1 1 d . . . . .
H1A H 0.479341 0.601063 0.531074 0.025 Uiso 1 1 calc R U . . .
N2 N 0.4430(2) 0.9009(3) 0.5221(3) 0.0391(15) Uani 1 1 d . . . . .
H2A H 0.464858 0.902629 0.491508 0.047 Uiso 1 1 calc R U . . .
H2B H 0.439650 0.950694 0.538403 0.047 Uiso 1 1 calc R U . . .
H2C H 0.414144 0.884104 0.507393 0.047 Uiso 1 1 calc R U . . .
C1 C 0.4857(3) 0.6978(4) 0.5921(3) 0.0290(15) Uani 1 1 d . . . . .
H1B H 0.518684 0.718897 0.598284 0.035 Uiso 1 1 calc R U . . .
H1C H 0.469479 0.696737 0.632066 0.035 Uiso 1 1 calc R U . . .
C2 C 0.4580(3) 0.7551(4) 0.5496(3) 0.0285(15) Uani 1 1 d . . . . .
H2D H 0.471774 0.751369 0.508288 0.034 Uiso 1 1 calc R U . . .
H2E H 0.423917 0.738033 0.547484 0.034 Uiso 1 1 calc R U . . .
C3 C 0.4603(3) 0.8426(4) 0.5711(3) 0.0350(16) Uani 1 1 d . . . . .
H3A H 0.440104 0.848879 0.607768 0.042 Uiso 1 1 calc R U . . .
H3B H 0.493941 0.855882 0.582282 0.042 Uiso 1 1 calc R U . . .
B1 B 0.6773(3) -0.0127(4) 0.6778(3) 0.0211(15) Uani 1 1 d . . . . .
B2 B 0.5905(3) 0.0270(4) 0.6728(3) 0.0247(16) Uani 1 1 d . . . . .
B3 B 0.5082(3) 0.0261(4) 0.6192(3) 0.0221(15) Uani 1 1 d . . . . .
B4 B 0.4471(3) 0.1159(4) 0.5649(3) 0.0207(15) Uani 1 1 d . . . . .
B5 B 0.4115(3) 0.1731(4) 0.4720(3) 0.0224(15) Uani 1 1 d . . . . .
B6 B 0.4386(3) 0.2646(4) 0.5567(3) 0.0212(15) Uani 1 1 d . . . . .
B7 B 0.4652(3) 0.4116(4) 0.5845(3) 0.0185(14) Uani 1 1 d . . . . .
B8 B 0.5120(3) 0.5405(4) 0.6137(3) 0.0168(14) Uani 1 1 d . . . . .
B9 B 0.5934(2) 0.5356(4) 0.6746(3) 0.0157(14) Uani 1 1 d . . . . .
B10 B 0.6818(3) 0.5644(4) 0.6905(3) 0.0236(15) Uani 1 1 d . . . . .
B11 B 0.6484(3) 0.4283(4) 0.7188(3) 0.0187(14) Uani 1 1 d . . . . .
B12 B 0.6633(2) 0.2757(4) 0.7377(3) 0.0194(14) Uani 1 1 d . . . . .
B13 B 0.6511(3) 0.1221(4) 0.7197(3) 0.0205(15) Uani 1 1 d . . . . .
O1W O 0.6449(3) 0.1173(5) 0.5484(3) 0.076(2) Uani 1 1 d G . . . .
H1W H 0.622325 0.090663 0.530110 0.115 Uiso 1 1 d G U . . .
N3 N 0.5457(2) 0.2384(3) 0.6483(3) 0.0370(14) Uani 1 1 d . . . . .
H3C H 0.560882 0.272884 0.622714 0.044 Uiso 1 1 calc R U . . .
H3D H 0.521289 0.213574 0.628291 0.044 Uiso 1 1 calc R U . . .
H3E H 0.567042 0.201100 0.661733 0.044 Uiso 1 1 calc R U . . .
C4 C 0.5254(3) 0.2850(4) 0.7023(3) 0.0409(19) Uani 1 1 d . . . . .
H4D H 0.502053 0.325202 0.687187 0.049 Uiso 1 1 calc R U . . .
H4E H 0.551992 0.314333 0.722336 0.049 Uiso 1 1 calc R U . . .
C5 C 0.500000 0.2312(6) 0.750000 0.042(3) Uani 1 2 d S T P . .
H5D H 0.524001 0.196397 0.770258 0.051 Uiso 0.5 1 calc R U P . .
H5E H 0.475999 0.196396 0.729742 0.051 Uiso 0.5 1 calc R U P . .
N6 N 0.6951(4) 0.2525(5) 0.5880(4) 0.082(3) Uani 1 1 d . . . . .
H6C H 0.687347 0.208097 0.566208 0.098 Uiso 1 1 calc R U . . .
H6D H 0.669410 0.286257 0.589146 0.098 Uiso 1 1 calc R U . . .
H6E H 0.703176 0.237958 0.626374 0.098 Uiso 1 1 calc R U . . .
N7 N 0.8450(3) 0.1403(4) 0.5427(3) 0.0528(18) Uani 1 1 d . . . . .
H7C H 0.847236 0.093386 0.521926 0.063 Uiso 1 1 calc R U . . .
H7D H 0.850833 0.131135 0.582689 0.063 Uiso 1 1 calc R U . . .
H7E H 0.866976 0.175693 0.528107 0.063 Uiso 1 1 calc R U . . .
C9 C 0.7351(4) 0.2924(7) 0.5600(6) 0.083(3) Uani 1 1 d . . . . .
H9 H 0.730831 0.339683 0.536642 0.100 Uiso 1 1 calc R U . . .
C10 C 0.7862(5) 0.2544(7) 0.5697(7) 0.096(4) Uani 1 1 d . . . . .
H10A H 0.811138 0.292939 0.556240 0.116 Uiso 1 1 calc R U . . .
H10B H 0.791186 0.243954 0.613447 0.116 Uiso 1 1 calc R U . . .
C11 C 0.7919(4) 0.1767(8) 0.5348(5) 0.088(3) Uani 1 1 d . . . . .
H11A H 0.785597 0.186544 0.491255 0.106 Uiso 1 1 calc R U . . .
H11B H 0.767928 0.137208 0.549501 0.106 Uiso 1 1 calc R U . . .
N4 N 0.5911(3) 0.7493(4) 0.7049(3) 0.0496(17) Uani 1 1 d . . . . .
H4A H 0.599455 0.789518 0.679233 0.060 Uiso 1 1 calc R U . . .
H4B H 0.558452 0.745361 0.706560 0.060 Uiso 1 1 calc R U . . .
H4C H 0.603621 0.702253 0.691407 0.060 Uiso 1 1 calc R U . . .
N5 N 0.7348(3) 0.7906(6) 0.8310(5) 0.089(3) Uani 1 1 d . . . . .
H5A H 0.752078 0.757940 0.855812 0.107 Uiso 1 1 calc R U . . .
H5B H 0.738950 0.842441 0.842629 0.107 Uiso 1 1 calc R U . . .
H5C H 0.745194 0.784478 0.792177 0.107 Uiso 1 1 calc DR U . . .
C6 C 0.6104(3) 0.7671(5) 0.7674(4) 0.055(2) Uani 1 1 d . . . . .
H6A H 0.595432 0.817018 0.782818 0.066 Uiso 1 1 calc R U . . .
H6B H 0.601457 0.722883 0.795199 0.066 Uiso 1 1 calc R U . . .
C7 C 0.6632(4) 0.7764(5) 0.7672(5) 0.068(3) Uani 1 1 d . . . . .
H7A H 0.671769 0.829267 0.749707 0.082 Uiso 1 1 calc R U . . .
H7B H 0.677804 0.734274 0.741457 0.082 Uiso 1 1 calc R U . . .
C8 C 0.6846(4) 0.7700(6) 0.8347(5) 0.068(3) Uani 1 1 d . . . . .
H8A H 0.667551 0.807371 0.862161 0.081 Uiso 1 1 calc R U . . .
H8B H 0.680732 0.714714 0.850448 0.081 Uiso 1 1 calc R U . . .
N8 N 0.6875(3) -0.0284(5) 0.5208(4) 0.076(2) Uani 1 1 d . . . . .
H8C H 0.661872 -0.053170 0.503414 0.091 Uiso 1 1 calc R U . . .
H8D H 0.680330 0.024008 0.527564 0.091 Uiso 1 1 calc R U . . .
H8E H 0.694570 -0.052686 0.556624 0.091 Uiso 1 1 calc R U . . .
N9 N 0.7412(3) 0.0339(4) 0.3135(3) 0.057(2) Uani 1 1 d . . . . .
H9A H 0.760747 0.018254 0.282611 0.069 Uiso 1 1 calc R U . . .
H9B H 0.746764 0.086315 0.322236 0.069 Uiso 1 1 calc R U . . .
H9C H 0.709942 0.027498 0.302232 0.069 Uiso 1 1 calc R U . . .
C12 C 0.7298(4) -0.0339(5) 0.4796(4) 0.067(3) Uani 1 1 d . . . . .
H12A H 0.736610 -0.090801 0.469920 0.081 Uiso 1 1 calc R U . . .
H12B H 0.758590 -0.010800 0.499592 0.081 Uiso 1 1 calc R U . . .
C13 C 0.7185(4) 0.0123(5) 0.4218(4) 0.056(2) Uani 1 1 d . . . . .
H13A H 0.723550 0.070326 0.428891 0.068 Uiso 1 1 calc R U . . .
H13B H 0.684252 0.004105 0.410875 0.068 Uiso 1 1 calc R U . . .
C14 C 0.7512(3) -0.0160(5) 0.3680(4) 0.051(2) Uani 1 1 d . . . . .
H14A H 0.785529 -0.010770 0.379492 0.062 Uiso 1 1 calc R U . . .
H14B H 0.744683 -0.073112 0.358818 0.062 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
V1 V2 3.0347(11) 3_656 ?
V1 V2 3.0347(11) . ?
V1 O6 1.945(4) . ?
V1 O6 1.945(4) 3_656 ?
V1 O8 1.597(6) . ?
V1 O9 1.954(4) . ?
V1 O9 1.954(4) 3_656 ?
V2 V3 2.9673(13) . ?
V2 O5 1.939(4) 3_656 ?
V2 O6 1.956(4) 3_656 ?
V2 O9 1.994(4) . ?
V2 O10 1.601(4) . ?
V2 O12 1.935(4) . ?
V3 V4 2.9497(13) . ?
V3 O5 1.941(4) 3_656 ?
V3 O12 1.942(4) . ?
V3 O13 1.602(4) . ?
V3 O16 1.944(4) . ?
V3 O33 1.985(4) 3_656 ?
V4 V5 2.9177(13) . ?
V4 O16 1.923(4) . ?
V4 O20 1.946(4) . ?
V4 O29 1.946(4) 3_656 ?
V4 O33 1.954(4) 3_656 ?
V4 O34 1.595(4) . ?
V5 V6 2.9922(11) . ?
V5 O20 1.964(4) . ?
V5 O22 1.953(4) . ?
V5 O24 1.945(4) 3_656 ?
V5 O26 1.601(4) . ?
V5 O29 1.938(4) 3_656 ?
V6 O22 1.927(4) 3_656 ?
V6 O22 1.927(4) . ?
V6 O24 1.948(4) . ?
V6 O24 1.948(4) 3_656 ?
V6 O25 1.613(5) . ?
O1 H1 0.818(10) . ?
O1 B1 1.385(8) . ?
O2 B1 1.338(8) . ?
O2 B2 1.482(8) . ?
O3 B1 1.383(8) . ?
O3 B13 1.492(8) . ?
O4 B2 1.474(8) . ?
O4 B13 1.456(8) . ?
O5 B13 1.479(8) . ?
O6 B2 1.492(8) . ?
O7 B2 1.443(9) . ?
O7 B3 1.347(8) . ?
O9 B3 1.376(8) . ?
O11 B3 1.368(8) . ?
O11 B4 1.470(8) . ?
O12 B4 1.479(8) . ?
O14 B4 1.465(8) . ?
O14 B5 1.334(8) . ?
O15 B4 1.466(8) . ?
O15 B6 1.454(8) . ?
O16 B6 1.487(8) . ?
O17 B5 1.375(8) . ?
O17 B6 1.491(8) . ?
O18 H18A 0.9300 . ?
O18 H18B 0.9300 . ?
O18 B5 1.386(8) . ?
O19 B6 1.464(8) . ?
O19 B7 1.360(7) . ?
O20 B7 1.387(8) . ?
O21 B7 1.349(8) . ?
O21 B8 1.465(7) . ?
O22 B8 1.451(7) . ?
O23 B8 1.417(8) . ?
O23 B9 1.446(8) . ?
O24 B9 1.504(7) . ?
O27 B9 1.495(8) . ?
O27 B10 1.351(8) . ?
O28 B9 1.469(7) . ?
O28 B11 1.448(8) . ?
O29 B11 1.488(7) . ?
O30 H30 0.847(10) . ?
O30 B10 1.370(9) . ?
O31 B10 1.379(8) . ?
O31 B11 1.495(8) . ?
O32 B11 1.467(7) . ?
O32 B12 1.347(7) . ?
O33 B12 1.377(8) . ?
O35 B12 1.364(8) . ?
O35 B13 1.477(8) . ?
N1 H1A 0.8600 . ?
N1 C1 1.488(7) . ?
N1 B8 1.659(7) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C3 1.500(8) . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C1 C2 1.512(9) . ?
C2 H2D 0.9700 . ?
C2 H2E 0.9700 . ?
C2 C3 1.503(8) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
O1W H1W 0.8504 . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N3 H3E 0.8900 . ?
N3 C4 1.499(9) . ?
C4 H4D 0.9700 . ?
C4 H4E 0.9700 . ?
C4 C5 1.519(9) . ?
C5 H5D 0.9700 . ?
C5 H5E 0.9700 . ?
N6 H6C 0.8900 . ?
N6 H6D 0.8900 . ?
N6 H6E 0.8900 . ?
N6 C9 1.405(14) . ?
N7 H7C 0.8900 . ?
N7 H7D 0.8900 . ?
N7 H7E 0.8900 . ?
N7 C11 1.571(13) . ?
C9 H9 0.9300 . ?
C9 C10 1.537(16) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.484(15) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8900 . ?
N4 C6 1.477(11) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N5 H5C 0.8900 . ?
N5 C8 1.409(13) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.445(13) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.572(14) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
N8 H8C 0.8900 . ?
N8 H8D 0.8900 . ?
N8 H8E 0.8900 . ?
N8 C12 1.457(12) . ?
N9 H9A 0.8900 . ?
N9 H9B 0.8900 . ?
N9 H9C 0.8900 . ?
N9 C14 1.458(11) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.492(12) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.534(12) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?

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
V2 V1 V2 140.23(6) 3_656 . ?
O6 V1 V2 39.05(11) 3_656 . ?
O6 V1 V2 122.05(13) 3_656 3_656 ?
O6 V1 V2 122.05(13) . . ?
O6 V1 V2 39.05(11) . 3_656 ?
O6 V1 O6 137.6(2) 3_656 . ?
O6 V1 O9 78.43(16) . 3_656 ?
O6 V1 O9 78.43(16) 3_656 . ?
O6 V1 O9 88.07(17) . . ?
O6 V1 O9 88.07(17) 3_656 3_656 ?
O8 V1 V2 109.89(3) . . ?
O8 V1 V2 109.89(3) . 3_656 ?
O8 V1 O6 111.19(12) . . ?
O8 V1 O6 111.19(12) . 3_656 ?
O8 V1 O9 108.90(12) . . ?
O8 V1 O9 108.90(12) . 3_656 ?
O9 V1 V2 122.88(13) . 3_656 ?
O9 V1 V2 40.25(12) . . ?
O9 V1 V2 122.88(12) 3_656 . ?
O9 V1 V2 40.25(12) 3_656 3_656 ?
O9 V1 O9 142.2(2) . 3_656 ?
V3 V2 V1 140.69(4) . . ?
O5 V2 V1 125.39(12) 3_656 . ?
O5 V2 V3 40.13(11) 3_656 . ?
O5 V2 O6 91.45(17) 3_656 3_656 ?
O5 V2 O9 141.92(17) 3_656 . ?
O6 V2 V1 38.79(12) 3_656 . ?
O6 V2 V3 124.96(12) 3_656 . ?
O6 V2 O9 77.21(17) 3_656 . ?
O9 V2 V1 39.27(11) . . ?
O9 V2 V3 121.42(12) . . ?
O10 V2 V1 108.25(16) . . ?
O10 V2 V3 111.04(16) . . ?
O10 V2 O5 108.3(2) . 3_656 ?
O10 V2 O6 108.0(2) . 3_656 ?
O10 V2 O9 109.8(2) . . ?
O10 V2 O12 109.7(2) . . ?
O12 V2 V1 122.32(13) . . ?
O12 V2 V3 40.15(12) . . ?
O12 V2 O5 79.94(16) . 3_656 ?
O12 V2 O6 142.13(17) . 3_656 ?
O12 V2 O9 87.10(17) . . ?
V4 V3 V2 146.35(4) . . ?
O5 V3 V2 40.10(11) 3_656 . ?
O5 V3 V4 125.61(12) 3_656 . ?
O5 V3 O12 79.72(16) 3_656 . ?
O5 V3 O16 139.23(18) 3_656 . ?
O5 V3 O33 87.24(15) 3_656 3_656 ?
O12 V3 V2 39.97(11) . . ?
O12 V3 V4 129.21(12) . . ?
O12 V3 O16 90.74(17) . . ?
O12 V3 O33 144.79(19) . 3_656 ?
O13 V3 V2 113.89(16) . . ?
O13 V3 V4 99.76(16) . . ?
O13 V3 O5 113.0(2) . 3_656 ?
O13 V3 O12 109.2(2) . . ?
O13 V3 O16 107.6(2) . . ?
O13 V3 O33 106.0(2) . 3_656 ?
O16 V3 V2 123.05(13) . . ?
O16 V3 V4 40.04(11) . . ?
O16 V3 O33 78.08(16) . 3_656 ?
O33 V3 V2 122.60(12) 3_656 . ?
O33 V3 V4 41.12(11) 3_656 . ?
V5 V4 V3 152.09(5) . . ?
O16 V4 V3 40.55(12) . . ?
O16 V4 V5 127.18(13) . . ?
O16 V4 O20 87.94(17) . . ?
O16 V4 O29 142.69(18) . 3_656 ?
O16 V4 O33 79.31(16) . 3_656 ?
O20 V4 V3 125.96(12) . . ?
O20 V4 V5 41.97(11) . . ?
O20 V4 O33 139.96(19) . 3_656 ?
O29 V4 V3 126.84(11) 3_656 . ?
O29 V4 V5 41.19(11) 3_656 . ?
O29 V4 O20 80.74(16) 3_656 . ?
O29 V4 O33 86.83(15) 3_656 3_656 ?
O33 V4 V3 41.91(11) 3_656 . ?
O33 V4 V5 124.77(12) 3_656 . ?
O34 V4 V3 102.08(16) . . ?
O34 V4 V5 105.82(16) . . ?
O34 V4 O16 106.5(2) . . ?
O34 V4 O20 109.3(2) . . ?
O34 V4 O29 110.8(2) . 3_656 ?
O34 V4 O33 110.7(2) . 3_656 ?
V4 V5 V6 142.96(4) . . ?
O20 V5 V4 41.50(12) . . ?
O20 V5 V6 118.01(13) . . ?
O22 V5 V4 124.47(11) . . ?
O22 V5 V6 39.21(11) . . ?
O22 V5 O20 85.23(16) . . ?
O24 V5 V4 128.83(11) 3_656 . ?
O24 V5 V6 39.82(12) 3_656 . ?
O24 V5 O20 140.95(17) 3_656 . ?
O24 V5 O22 78.90(16) 3_656 . ?
O26 V5 V4 103.37(16) . . ?
O26 V5 V6 113.39(16) . . ?
O26 V5 O20 107.6(2) . . ?
O26 V5 O22 108.1(2) . . ?
O26 V5 O24 111.19(19) . 3_656 ?
O26 V5 O29 108.9(2) . 3_656 ?
O29 V5 V4 41.40(11) 3_656 . ?
O29 V5 V6 123.66(12) 3_656 . ?
O29 V5 O20 80.49(16) 3_656 . ?
O29 V5 O22 142.80(16) 3_656 . ?
O29 V5 O24 90.97(16) 3_656 3_656 ?
V5 V6 V5 134.99(5) . 3_656 ?
O22 V6 V5 119.66(12) 3_656 . ?
O22 V6 V5 39.84(12) . . ?
O22 V6 V5 119.66(12) . 3_656 ?
O22 V6 V5 39.84(12) 3_656 3_656 ?
O22 V6 O22 138.2(2) 3_656 . ?
O22 V6 O24 79.46(16) 3_656 . ?
O22 V6 O24 88.55(16) . . ?
O22 V6 O24 79.46(16) . 3_656 ?
O22 V6 O24 88.55(16) 3_656 3_656 ?
O24 V6 V5 123.06(11) 3_656 3_656 ?
O24 V6 V5 123.06(11) . . ?
O24 V6 V5 39.74(11) . 3_656 ?
O24 V6 V5 39.75(11) 3_656 . ?
O24 V6 O24 146.1(2) . 3_656 ?
O25 V6 V5 112.50(3) . 3_656 ?
O25 V6 V5 112.50(3) . . ?
O25 V6 O22 110.89(11) . . ?
O25 V6 O22 110.89(11) . 3_656 ?
O25 V6 O24 106.97(11) . 3_656 ?
O25 V6 O24 106.97(11) . . ?
B1 O1 H1 112(6) . . ?
B1 O2 B2 120.7(5) . . ?
B1 O3 B13 119.5(5) . . ?
B13 O4 B2 115.7(4) . . ?
V2 O5 V3 99.77(17) 3_656 3_656 ?
B13 O5 V2 126.0(3) . 3_656 ?
B13 O5 V3 133.5(3) . 3_656 ?
V1 O6 V2 102.16(18) . 3_656 ?
B2 O6 V1 132.0(4) . . ?
B2 O6 V2 125.7(4) . 3_656 ?
B3 O7 B2 129.1(5) . . ?
V1 O9 V2 100.48(18) . . ?
B3 O9 V1 128.6(4) . . ?
B3 O9 V2 129.0(4) . . ?
B3 O11 B4 124.2(5) . . ?
V2 O12 V3 99.88(17) . . ?
B4 O12 V2 133.7(3) . . ?
B4 O12 V3 125.1(3) . . ?
B5 O14 B4 119.3(5) . . ?
B6 O15 B4 113.7(5) . . ?
V4 O16 V3 99.41(19) . . ?
B6 O16 V3 127.3(3) . . ?
B6 O16 V4 133.0(3) . . ?
B5 O17 B6 119.4(5) . . ?
H18A O18 H18B 120.0 . . ?
B5 O18 H18A 120.0 . . ?
B5 O18 H18B 120.0 . . ?
B7 O19 B6 131.7(5) . . ?
V4 O20 V5 96.53(17) . . ?
B7 O20 V4 130.6(3) . . ?
B7 O20 V5 132.2(4) . . ?
B7 O21 B8 128.8(5) . . ?
V6 O22 V5 100.95(17) . . ?
B8 O22 V5 129.6(4) . . ?
B8 O22 V6 129.4(4) . . ?
B8 O23 B9 128.3(4) . . ?
V5 O24 V6 100.45(17) 3_656 . ?
B9 O24 V5 127.8(3) . 3_656 ?
B9 O24 V6 129.9(3) . . ?
B10 O27 B9 120.8(5) . . ?
B11 O28 B9 117.4(4) . . ?
V5 O29 V4 97.41(16) 3_656 3_656 ?
B11 O29 V4 134.8(3) . 3_656 ?
B11 O29 V5 127.6(3) . 3_656 ?
B10 O30 H30 104(6) . . ?
B10 O31 B11 118.9(5) . . ?
B12 O32 B11 130.8(5) . . ?
V4 O33 V3 96.97(17) 3_656 3_656 ?
B12 O33 V3 131.1(3) . 3_656 ?
B12 O33 V4 131.5(3) . 3_656 ?
B12 O35 B13 128.4(5) . . ?
C1 N1 H1A 120.7 . . ?
C1 N1 B8 118.5(4) . . ?
B8 N1 H1A 120.7 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C3 N2 H2A 109.5 . . ?
C3 N2 H2B 109.5 . . ?
C3 N2 H2C 109.5 . . ?
N1 C1 H1B 108.9 . . ?
N1 C1 H1C 108.9 . . ?
N1 C1 C2 113.3(5) . . ?
H1B C1 H1C 107.7 . . ?
C2 C1 H1B 108.9 . . ?
C2 C1 H1C 108.9 . . ?
C1 C2 H2D 109.1 . . ?
C1 C2 H2E 109.1 . . ?
H2D C2 H2E 107.9 . . ?
C3 C2 C1 112.3(6) . . ?
C3 C2 H2D 109.1 . . ?
C3 C2 H2E 109.1 . . ?
N2 C3 C2 111.9(6) . . ?
N2 C3 H3A 109.2 . . ?
N2 C3 H3B 109.2 . . ?
C2 C3 H3A 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
O2 B1 O1 117.7(5) . . ?
O2 B1 O3 123.2(6) . . ?
O3 B1 O1 119.1(6) . . ?
O2 B2 O6 109.6(5) . . ?
O4 B2 O2 109.7(5) . . ?
O4 B2 O6 108.8(5) . . ?
O7 B2 O2 108.2(5) . . ?
O7 B2 O4 108.1(5) . . ?
O7 B2 O6 112.4(5) . . ?
O7 B3 O9 123.0(6) . . ?
O7 B3 O11 117.9(6) . . ?
O11 B3 O9 119.1(6) . . ?
O11 B4 O12 110.8(5) . . ?
O14 B4 O11 106.5(5) . . ?
O14 B4 O12 110.2(5) . . ?
O14 B4 O15 111.7(5) . . ?
O15 B4 O11 107.3(5) . . ?
O15 B4 O12 110.2(5) . . ?
O14 B5 O17 122.9(6) . . ?
O14 B5 O18 120.7(5) . . ?
O17 B5 O18 116.4(5) . . ?
O15 B6 O16 109.7(5) . . ?
O15 B6 O17 109.2(4) . . ?
O15 B6 O19 109.3(6) . . ?
O16 B6 O17 109.8(5) . . ?
O19 B6 O16 111.0(4) . . ?
O19 B6 O17 107.8(5) . . ?
O19 B7 O20 121.0(5) . . ?
O21 B7 O19 118.3(5) . . ?
O21 B7 O20 120.7(5) . . ?
O21 B8 N1 103.0(4) . . ?
O22 B8 O21 112.3(5) . . ?
O22 B8 N1 104.5(4) . . ?
O23 B8 O21 112.7(5) . . ?
O23 B8 O22 114.9(5) . . ?
O23 B8 N1 108.4(4) . . ?
O23 B9 O24 111.4(5) . . ?
O23 B9 O27 106.7(4) . . ?
O23 B9 O28 114.0(4) . . ?
O27 B9 O24 107.2(4) . . ?
O28 B9 O24 108.2(4) . . ?
O28 B9 O27 109.1(5) . . ?
O27 B10 O30 115.7(5) . . ?
O27 B10 O31 123.6(6) . . ?
O30 B10 O31 120.6(6) . . ?
O28 B11 O29 109.8(5) . . ?
O28 B11 O31 110.0(4) . . ?
O28 B11 O32 110.0(5) . . ?
O29 B11 O31 108.1(5) . . ?
O32 B11 O29 111.2(4) . . ?
O32 B11 O31 107.8(5) . . ?
O32 B12 O33 121.9(5) . . ?
O32 B12 O35 118.7(6) . . ?
O35 B12 O33 119.4(5) . . ?
O4 B13 O3 109.7(5) . . ?
O4 B13 O5 110.6(5) . . ?
O4 B13 O35 108.6(5) . . ?
O5 B13 O3 108.5(5) . . ?
O35 B13 O3 107.3(5) . . ?
O35 B13 O5 112.0(5) . . ?
H3C N3 H3D 109.5 . . ?
H3C N3 H3E 109.5 . . ?
H3D N3 H3E 109.5 . . ?
C4 N3 H3C 109.5 . . ?
C4 N3 H3D 109.5 . . ?
C4 N3 H3E 109.5 . . ?
N3 C4 H4D 108.8 . . ?
N3 C4 H4E 108.8 . . ?
N3 C4 C5 113.7(6) . . ?
H4D C4 H4E 107.7 . . ?
C5 C4 H4D 108.8 . . ?
C5 C4 H4E 108.8 . . ?
C4 C5 C4 109.4(8) . 3_656 ?
C4 C5 H5D 109.8 . . ?
C4 C5 H5D 109.8 3_656 . ?
C4 C5 H5E 109.8 . . ?
C4 C5 H5E 109.8 3_656 . ?
H5D C5 H5E 108.2 . . ?
H6C N6 H6D 109.5 . . ?
H6C N6 H6E 109.5 . . ?
H6D N6 H6E 109.5 . . ?
C9 N6 H6C 109.5 . . ?
C9 N6 H6D 109.5 . . ?
C9 N6 H6E 109.5 . . ?
H7C N7 H7D 109.5 . . ?
H7C N7 H7E 109.5 . . ?
H7D N7 H7E 109.5 . . ?
C11 N7 H7C 109.5 . . ?
C11 N7 H7D 109.5 . . ?
C11 N7 H7E 109.5 . . ?
N6 C9 H9 121.5 . . ?
N6 C9 C10 117.1(10) . . ?
C10 C9 H9 121.5 . . ?
C9 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 107.9 . . ?
C11 C10 C9 111.8(10) . . ?
C11 C10 H10A 109.3 . . ?
C11 C10 H10B 109.3 . . ?
N7 C11 H11A 109.4 . . ?
N7 C11 H11B 109.4 . . ?
C10 C11 N7 111.4(9) . . ?
C10 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
H4A N4 H4B 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
C6 N4 H4A 109.5 . . ?
C6 N4 H4B 109.5 . . ?
C6 N4 H4C 109.5 . . ?
H5A N5 H5B 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
C8 N5 H5A 109.5 . . ?
C8 N5 H5B 109.5 . . ?
C8 N5 H5C 109.5 . . ?
N4 C6 H6A 109.2 . . ?
N4 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
C7 C6 N4 111.9(8) . . ?
C7 C6 H6A 109.2 . . ?
C7 C6 H6B 109.2 . . ?
C6 C7 H7A 109.4 . . ?
C6 C7 H7B 109.4 . . ?
C6 C7 C8 111.0(9) . . ?
H7A C7 H7B 108.0 . . ?
C8 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
N5 C8 C7 106.8(9) . . ?
N5 C8 H8A 110.4 . . ?
N5 C8 H8B 110.4 . . ?
C7 C8 H8A 110.4 . . ?
C7 C8 H8B 110.4 . . ?
H8A C8 H8B 108.6 . . ?
H8C N8 H8D 109.5 . . ?
H8C N8 H8E 109.5 . . ?
H8D N8 H8E 109.5 . . ?
C12 N8 H8C 109.5 . . ?
C12 N8 H8D 109.5 . . ?
C12 N8 H8E 109.5 . . ?
H9A N9 H9B 109.5 . . ?
H9A N9 H9C 109.5 . . ?
H9B N9 H9C 109.5 . . ?
C14 N9 H9A 109.5 . . ?
C14 N9 H9B 109.5 . . ?
C14 N9 H9C 109.5 . . ?
N8 C12 H12A 110.0 . . ?
N8 C12 H12B 110.0 . . ?
N8 C12 C13 108.5(9) . . ?
H12A C12 H12B 108.4 . . ?
C13 C12 H12A 110.0 . . ?
C13 C12 H12B 110.0 . . ?
C12 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
C12 C13 C14 111.3(8) . . ?
H13A C13 H13B 108.0 . . ?
C14 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
N9 C14 C13 109.6(7) . . ?
N9 C14 H14A 109.7 . . ?
N9 C14 H14B 109.7 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O18 H18A O2 0.93 1.91 2.800(6) 159.2 5_656 yes
O18 H18B N4 0.93 2.19 2.895(8) 132.0 5_666 yes
O30 H30 O3 0.847(10) 1.94(5) 2.694(6) 148(9) 8_765 yes
N2 H2A O11 0.89 1.96 2.815(7) 159.8 5_666 yes
N2 H2C O1W 0.89 2.01 2.851(9) 157.4 5_666 yes
N3 H3D O15 0.89 1.88 2.729(7) 159.6 . yes
N3 H3E O4 0.89 1.92 2.795(7) 169.6 . yes
N6 H6C O1W 0.89 1.92 2.733(12) 151.5 . yes
N6 H6E O35 0.89 2.03 2.787(8) 142.0 . yes
N7 H7E O17 0.89 1.83 2.723(8) 175.1 4_556 yes
N4 H4A O18 0.89 2.10 2.895(8) 149.1 5_666 yes
N4 H4B O25 0.89 2.08 2.854(7) 144.2 . yes
N5 H5B N9 0.89 2.12 2.896(11) 145.8 7_566 yes
N8 H8D O1W 0.89 1.86 2.712(12) 160.5 . yes
N9 H9A O31 0.89 2.01 2.877(8) 165.4 2_654 yes
N9 H9B N5 0.89 2.04 2.896(11) 159.8 7_565 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 O6 B2 O2 -111.0(5) . . . . ?
V1 O6 B2 O4 129.0(4) . . . . ?
V1 O6 B2 O7 9.3(8) . . . . ?
V1 O9 B3 O7 1.8(9) . . . . ?
V1 O9 B3 O11 -178.3(4) . . . . ?
V2 O5 B13 O3 -75.8(6) 3_656 . . . ?
V2 O5 B13 O4 44.6(6) 3_656 . . . ?
V2 O5 B13 O35 165.9(4) 3_656 . . . ?
V2 O6 B2 O2 73.6(6) 3_656 . . . ?
V2 O6 B2 O4 -46.3(7) 3_656 . . . ?
V2 O6 B2 O7 -166.1(4) 3_656 . . . ?
V2 O9 B3 O7 163.1(4) . . . . ?
V2 O9 B3 O11 -16.9(8) . . . . ?
V2 O12 B4 O11 2.3(8) . . . . ?
V2 O12 B4 O14 120.0(5) . . . . ?
V2 O12 B4 O15 -116.2(5) . . . . ?
V3 O5 B13 O3 116.5(5) 3_656 . . . ?
V3 O5 B13 O4 -123.2(4) 3_656 . . . ?
V3 O5 B13 O35 -1.9(8) 3_656 . . . ?
V3 O12 B4 O11 166.9(3) . . . . ?
V3 O12 B4 O14 -75.5(5) . . . . ?
V3 O12 B4 O15 48.3(6) . . . . ?
V3 O16 B6 O15 -43.4(7) . . . . ?
V3 O16 B6 O17 76.7(6) . . . . ?
V3 O16 B6 O19 -164.3(4) . . . . ?
V3 O33 B12 O32 174.1(4) 3_656 . . . ?
V3 O33 B12 O35 -6.5(9) 3_656 . . . ?
V4 O16 B6 O15 143.9(4) . . . . ?
V4 O16 B6 O17 -96.0(5) . . . . ?
V4 O16 B6 O19 23.1(8) . . . . ?
V4 O20 B7 O19 2.6(9) . . . . ?
V4 O20 B7 O21 -176.4(4) . . . . ?
V4 O29 B11 O28 132.8(4) 3_656 . . . ?
V4 O29 B11 O31 -107.2(5) 3_656 . . . ?
V4 O29 B11 O32 10.9(8) 3_656 . . . ?
V4 O33 B12 O32 3.4(9) 3_656 . . . ?
V4 O33 B12 O35 -177.3(4) 3_656 . . . ?
V5 O20 B7 O19 171.3(4) . . . . ?
V5 O20 B7 O21 -7.7(9) . . . . ?
V5 O22 B8 O21 -42.0(6) . . . . ?
V5 O22 B8 O23 -172.5(3) . . . . ?
V5 O22 B8 N1 68.9(5) . . . . ?
V5 O24 B9 O23 167.3(3) 3_656 . . . ?
V5 O24 B9 O27 -76.3(5) 3_656 . . . ?
V5 O24 B9 O28 41.3(6) 3_656 . . . ?
V5 O29 B11 O28 -41.1(6) 3_656 . . . ?
V5 O29 B11 O31 78.8(6) 3_656 . . . ?
V5 O29 B11 O32 -163.0(3) 3_656 . . . ?
V6 O22 B8 O21 142.2(4) . . . . ?
V6 O22 B8 O23 11.7(7) . . . . ?
V6 O22 B8 N1 -106.9(5) . . . . ?
V6 O24 B9 O23 5.8(6) . . . . ?
V6 O24 B9 O27 122.2(4) . . . . ?
V6 O24 B9 O28 -120.2(4) . . . . ?
N1 C1 C2 C3 -173.1(6) . . . . ?
C1 N1 B8 O21 171.9(5) . . . . ?
C1 N1 B8 O22 54.4(7) . . . . ?
C1 N1 B8 O23 -68.6(6) . . . . ?
C1 C2 C3 N2 167.1(6) . . . . ?
B1 O2 B2 O4 22.4(8) . . . . ?
B1 O2 B2 O6 -97.0(6) . . . . ?
B1 O2 B2 O7 140.2(6) . . . . ?
B1 O3 B13 O4 -23.3(7) . . . . ?
B1 O3 B13 O5 97.6(6) . . . . ?
B1 O3 B13 O35 -141.1(5) . . . . ?
B2 O2 B1 O1 -176.8(5) . . . . ?
B2 O2 B1 O3 3.5(9) . . . . ?
B2 O4 B13 O3 51.2(6) . . . . ?
B2 O4 B13 O5 -68.5(6) . . . . ?
B2 O4 B13 O35 168.2(5) . . . . ?
B2 O7 B3 O9 -25.5(10) . . . . ?
B2 O7 B3 O11 154.6(6) . . . . ?
B3 O7 B2 O2 140.3(6) . . . . ?
B3 O7 B2 O4 -100.9(7) . . . . ?
B3 O7 B2 O6 19.2(9) . . . . ?
B3 O11 B4 O12 -40.2(8) . . . . ?
B3 O11 B4 O14 -160.1(5) . . . . ?
B3 O11 B4 O15 80.2(7) . . . . ?
B4 O11 B3 O7 -131.2(6) . . . . ?
B4 O11 B3 O9 48.8(8) . . . . ?
B4 O14 B5 O17 -12.9(9) . . . . ?
B4 O14 B5 O18 169.2(6) . . . . ?
B4 O15 B6 O16 68.0(6) . . . . ?
B4 O15 B6 O17 -52.4(6) . . . . ?
B4 O15 B6 O19 -170.1(4) . . . . ?
B5 O14 B4 O11 -134.6(5) . . . . ?
B5 O14 B4 O12 105.1(6) . . . . ?
B5 O14 B4 O15 -17.8(8) . . . . ?
B5 O17 B6 O15 21.9(8) . . . . ?
B5 O17 B6 O16 -98.4(6) . . . . ?
B5 O17 B6 O19 140.6(5) . . . . ?
B6 O15 B4 O11 167.9(4) . . . . ?
B6 O15 B4 O12 -71.4(6) . . . . ?
B6 O15 B4 O14 51.5(6) . . . . ?
B6 O17 B5 O14 10.7(9) . . . . ?
B6 O17 B5 O18 -171.4(6) . . . . ?
B6 O19 B7 O20 -11.2(10) . . . . ?
B6 O19 B7 O21 167.8(6) . . . . ?
B7 O19 B6 O15 -121.7(6) . . . . ?
B7 O19 B6 O16 -0.5(9) . . . . ?
B7 O19 B6 O17 119.7(6) . . . . ?
B7 O21 B8 O22 15.0(8) . . . . ?
B7 O21 B8 O23 146.6(5) . . . . ?
B7 O21 B8 N1 -96.8(6) . . . . ?
B8 O21 B7 O19 -171.3(5) . . . . ?
B8 O21 B7 O20 7.7(9) . . . . ?
B8 O23 B9 O24 -42.5(7) . . . . ?
B8 O23 B9 O27 -159.2(5) . . . . ?
B8 O23 B9 O28 80.3(7) . . . . ?
B8 N1 C1 C2 -172.1(5) . . . . ?
B9 O23 B8 O21 -95.4(6) . . . . ?
B9 O23 B8 O22 34.9(7) . . . . ?
B9 O23 B8 N1 151.3(5) . . . . ?
B9 O27 B10 O30 177.6(5) . . . . ?
B9 O27 B10 O31 -0.1(9) . . . . ?
B9 O28 B11 O29 67.9(6) . . . . ?
B9 O28 B11 O31 -50.9(6) . . . . ?
B9 O28 B11 O32 -169.4(4) . . . . ?
B10 O27 B9 O23 -145.5(5) . . . . ?
B10 O27 B9 O24 95.1(6) . . . . ?
B10 O27 B9 O28 -21.9(7) . . . . ?
B10 O31 B11 O28 25.5(7) . . . . ?
B10 O31 B11 O29 -94.3(6) . . . . ?
B10 O31 B11 O32 145.4(5) . . . . ?
B11 O28 B9 O23 168.0(5) . . . . ?
B11 O28 B9 O24 -67.5(6) . . . . ?
B11 O28 B9 O27 48.9(6) . . . . ?
B11 O31 B10 O27 -1.5(9) . . . . ?
B11 O31 B10 O30 -179.1(6) . . . . ?
B11 O32 B12 O33 -16.4(10) . . . . ?
B11 O32 B12 O35 164.3(6) . . . . ?
B12 O32 B11 O28 -112.4(6) . . . . ?
B12 O32 B11 O29 9.4(9) . . . . ?
B12 O32 B11 O31 127.8(6) . . . . ?
B12 O35 B13 O3 -147.2(6) . . . . ?
B12 O35 B13 O4 94.3(7) . . . . ?
B12 O35 B13 O5 -28.2(9) . . . . ?
B13 O3 B1 O1 177.1(5) . . . . ?
B13 O3 B1 O2 -3.2(9) . . . . ?
B13 O4 B2 O2 -50.9(6) . . . . ?
B13 O4 B2 O6 68.9(6) . . . . ?
B13 O4 B2 O7 -168.8(5) . . . . ?
B13 O35 B12 O32 -147.7(6) . . . . ?
B13 O35 B12 O33 32.9(9) . . . . ?
N3 C4 C5 C4 -172.0(8) . . . 3_656 ?
N6 C9 C10 C11 71.3(15) . . . . ?
C9 C10 C11 N7 177.6(9) . . . . ?
N4 C6 C7 C8 -163.7(7) . . . . ?
C6 C7 C8 N5 -172.3(8) . . . . ?
N8 C12 C13 C14 -158.7(7) . . . . ?
C12 C13 C14 N9 -176.5(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 0.137 0.094 0.494 65.5 48.7 ?
2 0.137 0.906 0.994 65.5 48.8 ?
3 0.363 0.406 -0.006 65.5 48.8 ?
4 0.363 0.594 0.494 65.5 49.0 ?
5 0.637 0.406 0.506 65.5 48.7 ?
6 0.637 0.594 0.006 65.5 48.9 ?
7 0.863 0.094 0.006 65.5 48.9 ?
8 0.863 0.906 0.506 65.5 49.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT417_1                   
;
PROBLEM: Short Inter D-H..H-D       H4A      ..H18B     .       1.50 Ang.  
RESPONSE: All &#8220;417&#8221; warnings stem from the fact that there are three
protonated 1,3dap which are disordered in the structure and are not connected to
clusters, and therefore cannot be positioned, which results in short contacts
between other H atoms
;
_vrf_RINTA01_1                   
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: The high R1 value is caused by the poor crystal data quality. 
;
