# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

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

data_exp_9805_auto
_database_code_depnum_ccdc_archive 'CCDC 2262727'
loop_
_audit_author_name
_audit_author_address
'Xie Zhen-Lang'
;Xiamen University
China
;
_audit_update_record             
;
2023-11-11 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_audit_creation_date             2023-11-11
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C12 H19 N15 O9 V2, 5(H2 O)'
_chemical_formula_sum            'C12 H29 N15 O14 V2'
_chemical_formula_weight         709.38
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N V '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.3068(2)
_cell_length_b                   16.4045(2)
_cell_length_c                   16.7884(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.654(2)
_cell_angle_gamma                90
_cell_volume                     2719.48(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11378
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.1040
_cell_measurement_theta_min      3.8470
_shelx_estimated_absorpt_T_max   0.437
_shelx_estimated_absorpt_T_min   0.351
_exptl_absorpt_coefficient_mu    6.611
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17071
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.374
_diffrn_reflns_theta_min         3.849
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     44.00  69.00   0.50    0.33    --   43.34  27.00 -15.00   50
  2  ω     54.00  80.00   0.50    1.31    --  108.01  15.00 120.00   52
  3  ω     93.00 177.00   0.50    1.31    --  108.01  15.00 120.00  168
  4  ω     91.00 141.00   0.50    1.31    --  108.01  27.00 -15.00  100
  5  ω    101.00 178.00   0.50    1.31    --  108.01 125.00-180.00  154
  6  ω     53.00 100.00   0.50    1.31    --  108.01 -77.00  60.00   94
  7  ω     49.00  99.00   0.50    1.31    --  108.01 -77.00 -30.00  100
  8  ω     33.00  58.00   0.50    1.31    --  108.01 -61.00 -90.00   50
  9  ω     35.00  70.00   0.50    1.31    --  108.01 -61.00-150.00   70
 10  ω    -26.00  -1.00   0.50    0.33    --   43.34 -27.00-177.00   50
 11  ω    -33.00  37.00   0.50    0.33    --  -43.34  27.00 -15.00  140
 12  ω    -64.00 -28.00   0.50    1.31    --  -96.00  61.00 -90.00   72
 13  ω    -70.00 -22.00   0.50    1.31    --  -96.00  61.00-180.00   96
 14  ω    -71.00 -46.00   0.50    1.31    --  -96.00  61.00-150.00   50
 15  ω    -65.00 -22.00   0.50    1.31    --  -96.00  61.00 -60.00   86
 16  ω     32.00  98.00   0.50    0.33    --   43.34-125.00  90.00  132
 17  ω    -48.00 -22.00   0.50    1.31    --  -96.00  45.00  60.00   52
 18  ω    -66.00 -22.00   0.50    1.31    --  -96.00  61.00  90.00   88
 19  ω    -70.00 -33.00   0.50    1.31    --  -96.00  61.00 150.00   74
 20  ω    -55.00 -29.00   0.50    1.31    --  -96.00 125.00  60.00   52
 21  ω   -124.00 -14.00   0.50    0.33    --  -43.34 -27.00-177.00  220
 22  ω   -169.00 -77.00   0.50    1.31    --  -96.00 -27.00-177.00  184
 23  ω   -118.00 -92.00   0.50    0.33    --  -43.34-125.00 -30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0303643000
_diffrn_orient_matrix_UB_12      0.0039022000
_diffrn_orient_matrix_UB_13      0.0952692000
_diffrn_orient_matrix_UB_21      0.1425429000
_diffrn_orient_matrix_UB_22      0.0333962000
_diffrn_orient_matrix_UB_23      0.0070388000
_diffrn_orient_matrix_UB_31      -0.0556510000
_diffrn_orient_matrix_UB_32      0.0876923000
_diffrn_orient_matrix_UB_33      -0.0069369000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4799
_reflns_number_total             5267
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_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         0.392
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         5267
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0326
_refine_ls_restrained_S_all      7.160
_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)+(0.0482P)²+1.1967P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0866
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O3W-H = O3W-HA_$1
 0.87 with sigma of 0.02
 O4W-HG = O4W-HH
 0.87 with sigma of 0.02
 HG-HH
 1.38 with sigma of 0.04
 H-HA_$1
 1.38 with sigma of 0.04
 O3A-C4 \\sim O3-C4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O5WA \\sim O5W: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O2W \\sim O2WA: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O3A \\sim O3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
4. Others
 Sof(O5WA)=Sof(H5WC)=Sof(H5WD)=Sof(O2WA)=Sof(H2WA)=Sof(H2WB)=Sof(O3A)=1-FVAR(1)
 Sof(O3)=Sof(O2W)=Sof(H2WC)=Sof(H2WD)=Sof(O5W)=Sof(H5WA)=Sof(H5WB)=FVAR(1)
5.a Riding coordinates:
 O3W(H,HA), O1W(HB,HC), O4W(HG,HH)
5.b Free rotating group:
 O2W(H2WC,H2WD), O5W(H5WA,H5WB), O5WA(H5WC,H5WD), O2WA(H2WA,H2WB)
5.c Rotating group:
 N14(HI,HJ), N4(HO,HP)
5.d Secondary CH2 refined with riding coordinates:
 C5(HU,HV), C2(HW,HX)
5.e Aromatic/amide H refined with riding coordinates:
 N8(HD), N12(HE), N3(HF)
5.f X=CH2 refined with riding coordinates:
 N9(HK,HL), N10(HM,HN), N5(HQ,HR), N15(HS,HT)
;
_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 0.67009(3) 0.47957(2) 0.22253(2) 0.01139(9) Uani 1 1 d . . . . .
V2 V 0.66718(3) 0.69284(2) 0.23672(2) 0.01126(9) Uani 1 1 d . . . . .
O1 O 0.71515(13) 0.59078(7) 0.17712(8) 0.0119(3) Uani 1 1 d . . . . .
O4 O 0.62364(14) 0.44287(8) 0.10279(8) 0.0164(3) Uani 1 1 d . . . . .
O6 O 0.85721(13) 0.73061(8) 0.24562(8) 0.0155(3) Uani 1 1 d . . . . .
O2 O 0.86748(14) 0.46438(8) 0.22717(9) 0.0160(3) Uani 1 1 d . . . . .
O8 O 0.63093(14) 0.39469(8) 0.25929(9) 0.0182(3) Uani 1 1 d . . . . .
O9 O 0.62514(14) 0.76710(8) 0.28746(9) 0.0175(3) Uani 1 1 d . . . . .
O5 O 0.65072(16) 0.42420(9) -0.02177(9) 0.0209(3) Uani 1 1 d . . . . .
O3 O 1.0312(3) 0.5096(2) 0.17579(19) 0.0190(6) Uani 0.897(5) 1 d D U P A 1
O7 O 1.06590(15) 0.70451(9) 0.24282(9) 0.0228(3) Uani 1 1 d . . . . .
O3W O 0.94127(16) 0.84865(9) 0.36347(10) 0.0278(3) Uani 1 1 d D . . . .
H H 0.921072 0.813735 0.321839 0.042 Uiso 1 1 d DR U . . .
HA H 0.982042 0.890265 0.349169 0.042 Uiso 1 1 d R U . . .
N1 N 0.75009(16) 0.62138(9) 0.34379(10) 0.0144(3) Uani 1 1 d . . . . .
N2 N 0.73612(17) 0.53617(9) 0.33840(10) 0.0147(3) Uani 1 1 d . . . . .
O1W O 0.93327(17) 0.89339(11) 0.13059(9) 0.0286(3) Uani 1 1 d . . . . .
HB H 0.857154 0.903206 0.141501 0.043 Uiso 1 1 d R U . . .
HC H 0.994554 0.915906 0.171391 0.043 Uiso 1 1 d R U . . .
N8 N 0.28056(16) 0.58000(9) 0.18869(10) 0.0143(3) Uani 1 1 d . . . . .
HD H 0.192239 0.578671 0.180025 0.017 Uiso 1 1 calc R U . . .
N11 N 0.58968(16) 0.74768(9) 0.12023(10) 0.0151(3) Uani 1 1 d . . . . .
N6 N 0.48843(16) 0.62565(9) 0.21476(10) 0.0124(3) Uani 1 1 d . . . . .
N12 N 0.52719(17) 0.70466(10) 0.04833(10) 0.0173(3) Uani 1 1 d . . . . .
HE H 0.508781 0.652174 0.045272 0.021 Uiso 1 1 calc R U . . .
N7 N 0.48923(16) 0.54011(9) 0.20521(10) 0.0131(3) Uani 1 1 d . . . . .
N3 N 0.83777(18) 0.56874(11) 0.46744(10) 0.0197(4) Uani 1 1 d . . . . .
HF H 0.878439 0.564581 0.521063 0.024 Uiso 1 1 calc R U . . .
O2W O 1.1517(2) 0.65477(12) 0.40920(12) 0.0312(6) Uani 0.897(5) 1 d G U P A 1
H2WC H 1.118518 0.667575 0.356979 0.047 Uiso 0.897(5) 1 d G U P A 1
H2WD H 1.161191 0.701241 0.435261 0.047 Uiso 0.897(5) 1 d G U P A 1
N13 N 0.54564(19) 0.83176(10) 0.00963(11) 0.0206(4) Uani 1 1 d . . . . .
O4W O 0.1389(2) 0.70339(12) 0.00402(12) 0.0414(5) Uani 1 1 d D . . . .
HG H 0.199393 0.665705 0.023072 0.062 Uiso 1 1 d DR U . . .
HH H 0.080073 0.680395 -0.039318 0.062 Uiso 1 1 d DR U . . .
N14 N 0.66041(18) 0.88559(10) 0.14320(11) 0.0196(4) Uani 1 1 d . . . . .
HI H 0.623565 0.932818 0.123137 0.023 Uiso 1 1 d R U . . .
HJ H 0.651131 0.878867 0.193666 0.023 Uiso 1 1 d R U . . .
N9 N 0.31551(17) 0.72291(10) 0.20704(11) 0.0190(4) Uani 1 1 d . . . . .
HK H 0.371928 0.764433 0.216262 0.023 Uiso 1 1 calc R U . . .
HL H 0.228458 0.731257 0.199444 0.023 Uiso 1 1 calc R U . . .
N10 N 0.32183(17) 0.43786(10) 0.17521(11) 0.0191(3) Uani 1 1 d . . . . .
HM H 0.381020 0.398794 0.176759 0.023 Uiso 1 1 calc R U . . .
HN H 0.235256 0.426049 0.164642 0.023 Uiso 1 1 calc R U . . .
N4 N 0.84090(19) 0.71344(11) 0.45639(11) 0.0220(4) Uani 1 1 d . . . . .
HO H 0.830642 0.750086 0.416758 0.026 Uiso 1 1 d R U . . .
HP H 0.910962 0.709596 0.500959 0.026 Uiso 1 1 d R U . . .
O5W O 0.3793(3) 0.55687(13) 0.39301(14) 0.0322(6) Uani 0.897(5) 1 d G U P A 1
H5WA H 0.445336 0.577057 0.432696 0.048 Uiso 0.897(5) 1 d G U P A 1
H5WB H 0.307517 0.582050 0.397586 0.048 Uiso 0.897(5) 1 d G U P A 1
N5 N 0.7996(2) 0.42746(11) 0.43478(12) 0.0252(4) Uani 1 1 d . . . . .
HQ H 0.769453 0.389765 0.396659 0.030 Uiso 1 1 calc R U . . .
HR H 0.836651 0.413300 0.486915 0.030 Uiso 1 1 calc R U . . .
C7 C 0.36196(19) 0.64730(11) 0.20459(11) 0.0131(4) Uani 1 1 d . . . . .
C8 C 0.36356(19) 0.51540(11) 0.18896(12) 0.0140(4) Uani 1 1 d . . . . .
N15 N 0.4343(2) 0.73506(11) -0.09328(12) 0.0279(4) Uani 1 1 d . . . . .
HS H 0.407024 0.684404 -0.104443 0.033 Uiso 1 1 calc R U . . .
HT H 0.418449 0.771468 -0.133417 0.033 Uiso 1 1 calc R U . . .
C4 C 0.9159(2) 0.51498(11) 0.18466(13) 0.0160(4) Uani 1 1 d D . . . .
C1 C 0.67005(19) 0.46472(11) 0.04313(12) 0.0155(4) Uani 1 1 d . . . . .
C3 C 0.81453(19) 0.57946(11) 0.13582(12) 0.0143(4) Uani 1 1 d . . . . .
C9 C 0.7889(2) 0.50670(12) 0.41336(12) 0.0174(4) Uani 1 1 d . . . . .
C5 C 0.88545(19) 0.66003(12) 0.12716(12) 0.0156(4) Uani 1 1 d . . . . .
HU H 0.959616 0.649092 0.102002 0.019 Uiso 1 1 calc R U . . .
HV H 0.819808 0.696999 0.089502 0.019 Uiso 1 1 calc R U . . .
C6 C 0.9424(2) 0.70103(11) 0.20996(12) 0.0157(4) Uani 1 1 d . . . . .
C2 C 0.7501(2) 0.54364(12) 0.04846(12) 0.0174(4) Uani 1 1 d . . . . .
HW H 0.688926 0.585370 0.014854 0.021 Uiso 1 1 calc R U . . .
HX H 0.823246 0.534133 0.022121 0.021 Uiso 1 1 calc R U . . .
C10 C 0.8110(2) 0.63850(12) 0.42183(12) 0.0172(4) Uani 1 1 d . . . . .
C15 C 0.4999(2) 0.75669(12) -0.01534(13) 0.0193(4) Uani 1 1 d . . . . .
C11 C 0.5982(2) 0.82301(12) 0.09272(13) 0.0166(4) Uani 1 1 d . . . . .
O5WA O 0.448(3) 0.5519(13) 0.3923(13) 0.033(4) Uani 0.103(5) 1 d G U P A 2
H5WC H 0.530357 0.533283 0.401274 0.049 Uiso 0.103(5) 1 d G U P A 2
H5WD H 0.426717 0.540191 0.437390 0.049 Uiso 0.103(5) 1 d G U P A 2
O2WA O 1.162(2) 0.5982(15) 0.3885(13) 0.051(5) Uani 0.103(5) 1 d G U P A 2
H2WA H 1.163544 0.617152 0.340393 0.076 Uiso 0.103(5) 1 d G U P A 2
H2WB H 1.084978 0.614372 0.394182 0.076 Uiso 0.103(5) 1 d G U P A 2
O3A O 1.0425(18) 0.517(2) 0.2050(18) 0.026(6) Uani 0.103(5) 1 d D U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 2.0804(12) . ?
V1 O4 2.0203(14) . ?
V1 O2 2.0288(14) . ?
V1 O8 1.6202(14) . ?
V1 N2 2.0857(17) . ?
V1 N7 2.0579(16) . ?
V2 O1 2.0813(13) . ?
V2 O6 2.0186(13) . ?
V2 O9 1.6153(14) . ?
V2 N1 2.1107(16) . ?
V2 N11 2.0921(16) . ?
V2 N6 2.0870(16) . ?
O1 C3 1.404(2) . ?
O4 C1 1.279(2) . ?
O6 C6 1.291(2) . ?
O2 C4 1.285(2) . ?
O5 C1 1.243(2) . ?
O3 C4 1.243(3) . ?
O7 C6 1.235(3) . ?
O3W H 0.8811 . ?
O3W HA 0.8707 . ?
N1 N2 1.406(2) . ?
N1 C10 1.311(3) . ?
N2 C9 1.312(3) . ?
O1W HB 0.8703 . ?
O1W HC 0.8698 . ?
N8 HD 0.8800 . ?
N8 C7 1.366(2) . ?
N8 C8 1.361(2) . ?
N11 N12 1.387(2) . ?
N11 C11 1.331(3) . ?
N6 N7 1.413(2) . ?
N6 C7 1.314(2) . ?
N12 HE 0.8800 . ?
N12 C15 1.333(3) . ?
N7 C8 1.309(3) . ?
N3 HF 0.8800 . ?
N3 C9 1.361(3) . ?
N3 C10 1.360(3) . ?
O2W H2WC 0.8705 . ?
O2W H2WD 0.8704 . ?
N13 C15 1.342(3) . ?
N13 C11 1.352(3) . ?
O4W HG 0.8710 . ?
O4W HH 0.8870 . ?
N14 HI 0.8858 . ?
N14 HJ 0.8864 . ?
N14 C11 1.368(3) . ?
N9 HK 0.8800 . ?
N9 HL 0.8800 . ?
N9 C7 1.334(3) . ?
N10 HM 0.8800 . ?
N10 HN 0.8800 . ?
N10 C8 1.341(3) . ?
N4 HO 0.8803 . ?
N4 HP 0.8807 . ?
N4 C10 1.356(3) . ?
O5W H5WA 0.8700 . ?
O5W H5WB 0.8698 . ?
N5 HQ 0.8800 . ?
N5 HR 0.8800 . ?
N5 C9 1.345(3) . ?
N15 HS 0.8800 . ?
N15 HT 0.8800 . ?
N15 C15 1.337(3) . ?
C4 C3 1.546(3) . ?
C4 O3A 1.251(17) . ?
C1 C2 1.524(3) . ?
C3 C5 1.537(3) . ?
C3 C2 1.542(3) . ?
C5 HU 0.9900 . ?
C5 HV 0.9900 . ?
C5 C6 1.504(3) . ?
C2 HW 0.9900 . ?
C2 HX 0.9900 . ?
O5WA H5WC 0.8701 . ?
O5WA H5WD 0.8697 . ?
O2WA H2WA 0.8695 . ?
O2WA H2WB 0.8702 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 N2 84.49(6) . . ?
O4 V1 O1 84.89(5) . . ?
O4 V1 O2 87.17(6) . . ?
O4 V1 N2 169.01(6) . . ?
O4 V1 N7 93.24(6) . . ?
O2 V1 O1 78.18(5) . . ?
O2 V1 N2 87.90(6) . . ?
O2 V1 N7 157.29(6) . . ?
O8 V1 O1 177.86(6) . . ?
O8 V1 O4 96.25(6) . . ?
O8 V1 O2 103.67(6) . . ?
O8 V1 N2 94.46(7) . . ?
O8 V1 N7 98.86(7) . . ?
N7 V1 O1 79.24(6) . . ?
N7 V1 N2 87.55(6) . . ?
O1 V2 N1 82.46(6) . . ?
O1 V2 N11 88.64(6) . . ?
O1 V2 N6 79.02(6) . . ?
O6 V2 O1 85.60(5) . . ?
O6 V2 N1 87.71(6) . . ?
O6 V2 N11 92.27(6) . . ?
O6 V2 N6 164.55(6) . . ?
O9 V2 O1 175.39(6) . . ?
O9 V2 O6 97.51(6) . . ?
O9 V2 N1 94.25(7) . . ?
O9 V2 N11 94.61(7) . . ?
O9 V2 N6 97.75(7) . . ?
N11 V2 N1 171.07(6) . . ?
N6 V2 N1 88.77(6) . . ?
N6 V2 N11 88.90(6) . . ?
V1 O1 V2 114.87(6) . . ?
C3 O1 V1 109.63(10) . . ?
C3 O1 V2 130.64(10) . . ?
C1 O4 V1 131.35(12) . . ?
C6 O6 V2 128.67(12) . . ?
C4 O2 V1 116.35(12) . . ?
H O3W HA 108.3 . . ?
N2 N1 V2 119.24(11) . . ?
C10 N1 V2 133.90(13) . . ?
C10 N1 N2 106.76(15) . . ?
N1 N2 V1 120.19(11) . . ?
C9 N2 V1 131.71(14) . . ?
C9 N2 N1 107.34(16) . . ?
HB O1W HC 104.5 . . ?
C7 N8 HD 126.9 . . ?
C8 N8 HD 126.9 . . ?
C8 N8 C7 106.16(16) . . ?
N12 N11 V2 123.53(12) . . ?
C11 N11 V2 132.70(14) . . ?
C11 N11 N12 103.35(16) . . ?
N7 N6 V2 120.74(11) . . ?
C7 N6 V2 132.28(12) . . ?
C7 N6 N7 106.95(15) . . ?
N11 N12 HE 126.0 . . ?
C15 N12 N11 108.10(15) . . ?
C15 N12 HE 126.0 . . ?
N6 N7 V1 119.85(11) . . ?
C8 N7 V1 133.01(13) . . ?
C8 N7 N6 107.08(15) . . ?
C9 N3 HF 127.0 . . ?
C10 N3 HF 127.0 . . ?
C10 N3 C9 106.09(17) . . ?
H2WC O2W H2WD 104.5 . . ?
C15 N13 C11 103.07(17) . . ?
HG O4W HH 104.4 . . ?
HI N14 HJ 108.7 . . ?
C11 N14 HI 110.3 . . ?
C11 N14 HJ 109.8 . . ?
HK N9 HL 120.0 . . ?
C7 N9 HK 120.0 . . ?
C7 N9 HL 120.0 . . ?
HM N10 HN 120.0 . . ?
C8 N10 HM 120.0 . . ?
C8 N10 HN 120.0 . . ?
HO N4 HP 125.6 . . ?
C10 N4 HO 109.4 . . ?
C10 N4 HP 109.2 . . ?
H5WA O5W H5WB 104.5 . . ?
HQ N5 HR 120.0 . . ?
C9 N5 HQ 120.0 . . ?
C9 N5 HR 120.0 . . ?
N6 C7 N8 109.74(16) . . ?
N6 C7 N9 126.76(17) . . ?
N9 C7 N8 123.48(17) . . ?
N7 C8 N8 110.06(16) . . ?
N7 C8 N10 125.37(18) . . ?
N10 C8 N8 124.57(18) . . ?
HS N15 HT 120.0 . . ?
C15 N15 HS 120.0 . . ?
C15 N15 HT 120.0 . . ?
O2 C4 C3 115.20(16) . . ?
O3 C4 O2 123.9(3) . . ?
O3 C4 C3 120.6(2) . . ?
O3A C4 O2 113.8(16) . . ?
O3A C4 C3 128.4(17) . . ?
O4 C1 C2 120.66(17) . . ?
O5 C1 O4 122.32(18) . . ?
O5 C1 C2 117.00(17) . . ?
O1 C3 C4 107.82(15) . . ?
O1 C3 C5 111.52(15) . . ?
O1 C3 C2 110.09(15) . . ?
C5 C3 C4 111.78(16) . . ?
C5 C3 C2 108.94(15) . . ?
C2 C3 C4 106.56(15) . . ?
N2 C9 N3 109.68(17) . . ?
N2 C9 N5 126.33(19) . . ?
N5 C9 N3 123.94(19) . . ?
C3 C5 HU 109.3 . . ?
C3 C5 HV 109.3 . . ?
HU C5 HV 108.0 . . ?
C6 C5 C3 111.56(15) . . ?
C6 C5 HU 109.3 . . ?
C6 C5 HV 109.3 . . ?
O6 C6 C5 117.35(17) . . ?
O7 C6 O6 121.76(19) . . ?
O7 C6 C5 120.87(18) . . ?
C1 C2 C3 117.25(16) . . ?
C1 C2 HW 108.0 . . ?
C1 C2 HX 108.0 . . ?
C3 C2 HW 108.0 . . ?
C3 C2 HX 108.0 . . ?
HW C2 HX 107.2 . . ?
N1 C10 N3 110.12(17) . . ?
N1 C10 N4 127.34(19) . . ?
N4 C10 N3 122.48(18) . . ?
N12 C15 N13 111.24(18) . . ?
N12 C15 N15 123.09(19) . . ?
N15 C15 N13 125.66(19) . . ?
N11 C11 N13 114.19(17) . . ?
N11 C11 N14 123.21(18) . . ?
N13 C11 N14 122.54(18) . . ?
H5WC O5WA H5WD 104.5 . . ?
H2WA O2WA H2WB 104.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 O1 C3 C4 -37.73(16) . . . . ?
V1 O1 C3 C5 -160.80(12) . . . . ?
V1 O1 C3 C2 78.15(15) . . . . ?
V1 O4 C1 O5 164.52(14) . . . . ?
V1 O4 C1 C2 -16.7(3) . . . . ?
V1 O2 C4 O3 -173.9(2) . . . . ?
V1 O2 C4 C3 -0.5(2) . . . . ?
V1 O2 C4 O3A 163.1(17) . . . . ?
V1 N2 C9 N3 169.23(14) . . . . ?
V1 N2 C9 N5 -8.2(3) . . . . ?
V1 N7 C8 N8 175.99(13) . . . . ?
V1 N7 C8 N10 -3.5(3) . . . . ?
V2 O1 C3 C4 115.71(14) . . . . ?
V2 O1 C3 C5 -7.4(2) . . . . ?
V2 O1 C3 C2 -128.41(14) . . . . ?
V2 O6 C6 O7 -149.55(15) . . . . ?
V2 O6 C6 C5 29.0(2) . . . . ?
V2 N1 N2 V1 12.30(18) . . . . ?
V2 N1 N2 C9 -176.55(13) . . . . ?
V2 N1 C10 N3 176.24(13) . . . . ?
V2 N1 C10 N4 -1.3(3) . . . . ?
V2 N11 N12 C15 -175.06(13) . . . . ?
V2 N11 C11 N13 172.91(14) . . . . ?
V2 N11 C11 N14 -4.2(3) . . . . ?
V2 N6 N7 V1 5.06(18) . . . . ?
V2 N6 N7 C8 -177.47(12) . . . . ?
V2 N6 C7 N8 177.74(13) . . . . ?
V2 N6 C7 N9 -0.8(3) . . . . ?
O1 C3 C5 C6 54.4(2) . . . . ?
O1 C3 C2 C1 -55.3(2) . . . . ?
O4 C1 C2 C3 20.7(3) . . . . ?
O2 C4 C3 O1 26.1(2) . . . . ?
O2 C4 C3 C5 149.05(17) . . . . ?
O2 C4 C3 C2 -92.03(19) . . . . ?
O5 C1 C2 C3 -160.50(17) . . . . ?
O3 C4 C3 O1 -160.2(2) . . . . ?
O3 C4 C3 C5 -37.2(3) . . . . ?
O3 C4 C3 C2 81.7(3) . . . . ?
N1 N2 C9 N3 -0.5(2) . . . . ?
N1 N2 C9 N5 -177.9(2) . . . . ?
N2 N1 C10 N3 0.2(2) . . . . ?
N2 N1 C10 N4 -177.34(19) . . . . ?
N11 N12 C15 N13 2.5(2) . . . . ?
N11 N12 C15 N15 -177.1(2) . . . . ?
N6 N7 C8 N8 -1.0(2) . . . . ?
N6 N7 C8 N10 179.53(18) . . . . ?
N12 N11 C11 N13 0.5(2) . . . . ?
N12 N11 C11 N14 -176.58(18) . . . . ?
N7 N6 C7 N8 -0.2(2) . . . . ?
N7 N6 C7 N9 -178.73(18) . . . . ?
C7 N8 C8 N7 0.9(2) . . . . ?
C7 N8 C8 N10 -179.62(18) . . . . ?
C7 N6 N7 V1 -176.75(12) . . . . ?
C7 N6 N7 C8 0.7(2) . . . . ?
C8 N8 C7 N6 -0.4(2) . . . . ?
C8 N8 C7 N9 178.20(18) . . . . ?
C4 C3 C5 C6 -66.4(2) . . . . ?
C4 C3 C2 C1 61.3(2) . . . . ?
C3 C5 C6 O6 -69.1(2) . . . . ?
C3 C5 C6 O7 109.5(2) . . . . ?
C9 N3 C10 N1 -0.5(2) . . . . ?
C9 N3 C10 N4 177.18(19) . . . . ?
C5 C3 C2 C1 -177.90(16) . . . . ?
C2 C3 C5 C6 176.12(16) . . . . ?
C10 N1 N2 V1 -170.94(13) . . . . ?
C10 N1 N2 C9 0.2(2) . . . . ?
C10 N3 C9 N2 0.6(2) . . . . ?
C10 N3 C9 N5 178.1(2) . . . . ?
C15 N13 C11 N11 0.9(2) . . . . ?
C15 N13 C11 N14 178.02(19) . . . . ?
C11 N11 N12 C15 -1.7(2) . . . . ?
C11 N13 C15 N12 -2.1(2) . . . . ?
C11 N13 C15 N15 177.5(2) . . . . ?
O3A C4 C3 O1 -134.6(19) . . . . ?
O3A C4 C3 C5 -11.7(19) . . . . ?
O3A C4 C3 C2 107.3(19) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.176
_oxdiff_exptl_absorpt_empirical_full_min 0.847
####################################################################### 
# 
# 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_exp_12327_auto
_database_code_depnum_ccdc_archive 'CCDC 2262730'
loop_
_audit_author_name
_audit_author_address
'Xie Zhen-Lang'
;Xiamen University
China
;
_audit_update_record             
;
2023-11-11 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_audit_creation_date             2023-04-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H11 N10 O8 V3, 0.5(H2 O), 4[H2O]'
_chemical_formula_sum            'C4 H20 N10 O12.50 V3'
_chemical_formula_weight         561.12
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N V Cl'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.3231(2)
_cell_length_b                   17.2111(3)
_cell_length_c                   10.4223(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.788(2)
_cell_angle_gamma                90
_cell_volume                     1812.70(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6488
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.3320
_cell_measurement_theta_min      5.0180
_shelx_estimated_absorpt_T_max   0.344
_shelx_estimated_absorpt_T_min   0.236
_exptl_absorpt_coefficient_mu    13.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.056
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10675
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.006
_diffrn_reflns_theta_min         5.039
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -51.00 -20.00   0.50    0.12    --  -98.00  45.00 150.00   62
  2  ω    -49.00 -20.00   0.50    0.12    --  -98.00  45.00 120.00   58
  3  ω    -51.00 -20.00   0.50    0.12    --  -98.00  45.00 -60.00   62
  4  ω    -47.00 -22.00   0.50    0.12    --  -98.00  45.00-180.00   50
  5  ω    -57.00 -31.00   0.50    0.12    --  -98.00  61.00 -90.00   52
  6  ω    -46.00 -21.00   0.50    0.12    --  -98.00  45.00 -90.00   50
  7  ω    -49.00 -21.00   0.50    0.12    --  -98.00  45.00 -30.00   56
  8  ω    -26.00  42.00   0.50    0.05    --  -40.63  19.00 -90.00  136
  9  ω    -51.00 -21.00   0.50    0.12    --  -98.00  45.00   0.00   60
 10  ω    -50.00 -25.00   0.50    0.12    --  -98.00  45.00  30.00   50
 11  ω    -51.00 -21.00   0.50    0.12    --  -98.00  45.00  90.00   60
 12  ω    -67.00  -3.00   0.50    0.05    --  -40.63 110.00 153.00  128
 13  ω    -77.00 -52.00   0.50    0.12    --  -98.00 110.00 153.00   50
 14  ω    -87.00 -25.00   0.50    0.12    --  -98.00 125.00-180.00  124
 15  ω   -149.00 -79.00   0.50    0.12    --  -98.00-110.00  58.00  140
 16  ω   -115.00 -62.00   0.50    0.05    --  -40.63 -38.00 -60.00  106
 17  ω    -58.00 -14.00   0.50    0.05    --  -40.63 -38.00 -60.00   88
 18  ω    -40.00  -8.00   0.50    0.05    --   40.63 -19.00  30.00   64
 19  ω     61.00  87.00   0.50    0.12    --  110.43 -77.00  60.00   52
 20  ω     46.00  71.00   0.50    0.12    --  110.43 -61.00  30.00   50
 21  ω     37.00  69.00   0.50    0.12    --  110.43 -61.00  60.00   64
 22  ω     36.00 102.00   0.50    0.12    --  110.43 -77.00 120.00  132
 23  ω     75.00 113.00   0.50    0.12    --  110.43-125.00 150.00   76
 24  ω     48.00 103.00   0.50    0.12    --  110.43-110.00  58.00  110
 25  ω     31.00  87.00   0.50    0.05    --   40.63-110.00  58.00  112
 26  ω     90.00 115.00   0.50    0.12    --  110.43  61.00  60.00   50
 27  ω    133.00 165.00   0.50    0.12    --  110.43  61.00  60.00   64
 28  ω    109.00 143.00   0.50    0.12    --  110.43 110.00 153.00   68
 29  ω     68.00  93.00   0.50    0.05    --   40.63 178.00 -30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1007082000
_diffrn_orient_matrix_UB_12      -0.0244339000
_diffrn_orient_matrix_UB_13      -0.1236890000
_diffrn_orient_matrix_UB_21      -0.0033065000
_diffrn_orient_matrix_UB_22      0.0840348000
_diffrn_orient_matrix_UB_23      -0.0514979000
_diffrn_orient_matrix_UB_31      0.1143779000
_diffrn_orient_matrix_UB_32      -0.0189772000
_diffrn_orient_matrix_UB_33      -0.0694746000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3203
_reflns_number_total             3504
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.238
_refine_diff_density_min         -1.315
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3504
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0537
_refine_ls_restrained_S_all      1.072
_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)+(0.0912P)²+4.0553P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1536
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5)
3.a Riding coordinates:
 O1W(H1WA,H1WB)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N8(H8)
3.c X=CH2 refined with riding coordinates:
 N9(H9A,H9B), N4(H4A,H4B), N5(H5A,H5B), N10(H10A,H10B)
;
_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 1.80843(6) 0.56835(4) -0.67640(6) 0.01417(19) Uani 1 1 d . . . . .
V3 V 1.66487(6) 0.54000(4) -0.39603(6) 0.01498(19) Uani 1 1 d . . . . .
V2 V 1.68279(6) 0.71248(4) -0.58398(7) 0.0163(2) Uani 1 1 d . . . . .
O7 O 1.7164(3) 0.60170(16) -0.5369(3) 0.0162(5) Uani 1 1 d . . . . .
O8 O 1.7884(3) 0.67891(16) -0.7080(3) 0.0208(6) Uani 1 1 d . . . . .
O1 O 1.9619(3) 0.56242(16) -0.6954(3) 0.0206(6) Uani 1 1 d . . . . .
O2 O 1.7117(3) 0.53427(17) -0.8094(3) 0.0240(7) Uani 1 1 d . . . . .
O5 O 1.5469(3) 0.48384(17) -0.3600(3) 0.0227(6) Uani 1 1 d . . . . .
O6 O 1.7789(3) 0.54449(18) -0.2634(3) 0.0228(6) Uani 1 1 d . . . . .
O3 O 1.5454(3) 0.73285(19) -0.6873(3) 0.0252(6) Uani 1 1 d . . . . .
O4 O 1.7623(3) 0.79363(17) -0.5408(3) 0.0274(7) Uani 1 1 d . . . . .
N6 N 1.6046(3) 0.70988(19) -0.4178(3) 0.0167(7) Uani 1 1 d . . . . .
N2 N 1.7439(3) 0.45008(19) -0.4856(3) 0.0157(7) Uani 1 1 d . . . . .
N3 N 1.8394(3) 0.34192(19) -0.5273(3) 0.0175(7) Uani 1 1 d . . . . .
H3 H 1.861681 0.292567 -0.527234 0.021 Uiso 1 1 calc R U . . .
N7 N 1.5656(3) 0.64020(19) -0.3683(3) 0.0150(6) Uani 1 1 d . . . . .
N8 N 1.4732(3) 0.73845(19) -0.2792(3) 0.0157(7) Uani 1 1 d . . . . .
H8 H 1.427299 0.764886 -0.231564 0.019 Uiso 1 1 calc R U . . .
N9 N 1.5445(3) 0.84241(19) -0.3984(3) 0.0192(7) Uani 1 1 d . . . . .
H9A H 1.585769 0.857517 -0.460095 0.023 Uiso 1 1 calc R U . . .
H9B H 1.502941 0.876656 -0.358792 0.023 Uiso 1 1 calc R U . . .
N4 N 1.9714(4) 0.3897(2) -0.6719(4) 0.0241(8) Uani 1 1 d . . . . .
H4A H 1.997256 0.429329 -0.713786 0.029 Uiso 1 1 calc R U . . .
H4B H 2.003011 0.342965 -0.680750 0.029 Uiso 1 1 calc R U . . .
N1 N 1.8283(3) 0.46594(19) -0.5717(3) 0.0158(6) Uani 1 1 d . . . . .
N5 N 1.6932(4) 0.3349(2) -0.3779(4) 0.0225(7) Uani 1 1 d . . . . .
H5A H 1.640481 0.359308 -0.334816 0.027 Uiso 1 1 calc R U . . .
H5B H 1.706067 0.284528 -0.367303 0.027 Uiso 1 1 calc R U . . .
N10 N 1.4340(3) 0.6102(2) -0.2106(3) 0.0183(7) Uani 1 1 d . . . . .
H10A H 1.448366 0.559991 -0.215449 0.022 Uiso 1 1 calc R U . . .
H10B H 1.384229 0.627764 -0.157755 0.022 Uiso 1 1 calc R U . . .
C2 C 1.7541(4) 0.3745(2) -0.4602(4) 0.0164(8) Uani 1 1 d . . . . .
C4 C 1.4888(4) 0.6608(2) -0.2851(4) 0.0153(7) Uani 1 1 d . . . . .
C3 C 1.5450(4) 0.7658(2) -0.3641(4) 0.0161(7) Uani 1 1 d . . . . .
C1 C 1.8841(4) 0.4005(2) -0.5949(4) 0.0172(8) Uani 1 1 d . . . . .
O1W O 1.5836(11) 0.5759(6) -0.9998(12) 0.070(3) Uani 0.5 1 d . . P . .
H1WA H 1.589662 0.536921 -1.051502 0.106 Uiso 0.5 1 d R U P . .
H1WB H 1.592862 0.555081 -0.922291 0.106 Uiso 0.5 1 d R U P . .


_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 3.0453(9) . ?
V1 O7 1.978(3) . ?
V1 O8 1.935(3) . ?
V1 O1 1.639(3) . ?
V1 O2 1.642(3) . ?
V1 N1 2.061(3) . ?
V3 O7 1.971(3) . ?
V3 O5 1.656(3) . ?
V3 O6 1.624(3) . ?
V3 N2 2.060(3) . ?
V3 N7 2.056(3) . ?
V2 O7 1.982(3) . ?
V2 O8 1.942(3) . ?
V2 O3 1.634(3) . ?
V2 O4 1.636(3) . ?
V2 N6 2.056(3) . ?
N6 N7 1.396(4) . ?
N6 C3 1.325(5) . ?
N2 N1 1.400(5) . ?
N2 C2 1.327(5) . ?
N3 H3 0.8800 . ?
N3 C2 1.353(5) . ?
N3 C1 1.363(5) . ?
N7 C4 1.337(5) . ?
N8 H8 0.8800 . ?
N8 C4 1.349(5) . ?
N8 C3 1.349(5) . ?
N9 H9A 0.8800 . ?
N9 H9B 0.8800 . ?
N9 C3 1.366(5) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
N4 C1 1.337(6) . ?
N1 C1 1.310(5) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N5 C2 1.348(5) . ?
N10 H10A 0.8800 . ?
N10 H10B 0.8800 . ?
N10 C4 1.364(5) . ?
O1W H1WA 0.8703 . ?
O1W H1WB 0.8702 . ?

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
O7 V1 V2 39.77(8) . . ?
O7 V1 N1 82.51(12) . . ?
O8 V1 V2 38.31(8) . . ?
O8 V1 O7 77.84(12) . . ?
O8 V1 N1 157.94(14) . . ?
O1 V1 V2 124.99(11) . . ?
O1 V1 O7 136.73(14) . . ?
O1 V1 O8 96.47(13) . . ?
O1 V1 O2 108.19(16) . . ?
O1 V1 N1 90.96(13) . . ?
O2 V1 V2 109.45(11) . . ?
O2 V1 O7 115.04(14) . . ?
O2 V1 O8 100.49(14) . . ?
O2 V1 N1 96.83(14) . . ?
N1 V1 V2 122.13(10) . . ?
O7 V3 N2 82.83(12) . . ?
O7 V3 N7 82.56(12) . . ?
O5 V3 O7 143.67(14) . . ?
O5 V3 N2 92.39(14) . . ?
O5 V3 N7 92.71(14) . . ?
O6 V3 O7 110.45(14) . . ?
O6 V3 O5 105.88(16) . . ?
O6 V3 N2 97.83(14) . . ?
O6 V3 N7 97.81(14) . . ?
N7 V3 N2 161.54(13) . . ?
O7 V2 V1 39.68(8) . . ?
O7 V2 N6 81.33(12) . . ?
O8 V2 V1 38.15(9) . . ?
O8 V2 O7 77.59(12) . . ?
O8 V2 N6 157.70(13) . . ?
O3 V2 V1 109.57(12) . . ?
O3 V2 O7 117.01(14) . . ?
O3 V2 O8 98.93(15) . . ?
O3 V2 O4 108.49(17) . . ?
O3 V2 N6 97.03(14) . . ?
O4 V2 V1 124.07(12) . . ?
O4 V2 O7 134.50(15) . . ?
O4 V2 O8 96.80(14) . . ?
O4 V2 N6 92.77(15) . . ?
N6 V2 V1 120.98(9) . . ?
V1 O7 V2 100.54(12) . . ?
V3 O7 V1 129.38(14) . . ?
V3 O7 V2 130.01(14) . . ?
V1 O8 V2 103.53(13) . . ?
N7 N6 V2 121.5(2) . . ?
C3 N6 V2 129.5(3) . . ?
C3 N6 N7 105.9(3) . . ?
N1 N2 V3 120.0(2) . . ?
C2 N2 V3 132.0(3) . . ?
C2 N2 N1 106.5(3) . . ?
C2 N3 H3 126.7 . . ?
C2 N3 C1 106.5(3) . . ?
C1 N3 H3 126.7 . . ?
N6 N7 V3 118.6(2) . . ?
C4 N7 V3 133.8(3) . . ?
C4 N7 N6 105.4(3) . . ?
C4 N8 H8 128.4 . . ?
C4 N8 C3 103.2(3) . . ?
C3 N8 H8 128.4 . . ?
H9A N9 H9B 120.0 . . ?
C3 N9 H9A 120.0 . . ?
C3 N9 H9B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C1 N4 H4A 120.0 . . ?
C1 N4 H4B 120.0 . . ?
N2 N1 V1 119.9(2) . . ?
C1 N1 V1 129.6(3) . . ?
C1 N1 N2 107.8(3) . . ?
H5A N5 H5B 120.0 . . ?
C2 N5 H5A 120.0 . . ?
C2 N5 H5B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
C4 N10 H10A 120.0 . . ?
C4 N10 H10B 120.0 . . ?
N2 C2 N3 109.7(3) . . ?
N2 C2 N5 126.5(4) . . ?
N5 C2 N3 123.8(4) . . ?
N7 C4 N8 112.6(3) . . ?
N7 C4 N10 124.7(4) . . ?
N8 C4 N10 122.6(4) . . ?
N6 C3 N8 112.8(4) . . ?
N6 C3 N9 124.6(4) . . ?
N8 C3 N9 122.3(4) . . ?
N4 C1 N3 123.2(4) . . ?
N1 C1 N3 109.4(4) . . ?
N1 C1 N4 127.3(4) . . ?
H1WA O1W H1WB 104.5 . . ?

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
N8 H8 O8 0.88 1.79 2.606(4) 153.7 4_576 yes
N9 H9A O4 0.88 2.42 3.054(5) 129.1 . yes
N9 H9B O1 0.88 2.12 2.937(4) 155.1 4_576 yes
N4 H4A O1 0.88 2.33 2.983(5) 130.7 . yes
N5 H5A O5 0.88 2.34 3.001(5) 131.6 . yes
N10 H10A O5 0.88 2.38 3.042(5) 132.6 . yes
O1W H1WB O2 0.87 1.56 2.264(14) 135.7 . 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 N1 C1 N3 -160.9(3) . . . . ?
V1 N1 C1 N4 19.0(6) . . . . ?
V3 N2 N1 V1 -28.8(4) . . . . ?
V3 N2 N1 C1 168.0(3) . . . . ?
V3 N2 C2 N3 -166.3(3) . . . . ?
V3 N2 C2 N5 12.0(6) . . . . ?
V3 N7 C4 N8 163.5(3) . . . . ?
V3 N7 C4 N10 -14.8(6) . . . . ?
V2 N6 N7 V3 30.8(4) . . . . ?
V2 N6 N7 C4 -163.7(2) . . . . ?
V2 N6 C3 N8 161.9(3) . . . . ?
V2 N6 C3 N9 -12.3(6) . . . . ?
N6 N7 C4 N8 1.2(4) . . . . ?
N6 N7 C4 N10 -177.1(3) . . . . ?
N2 N1 C1 N3 0.1(4) . . . . ?
N2 N1 C1 N4 180.0(4) . . . . ?
N7 N6 C3 N8 2.2(4) . . . . ?
N7 N6 C3 N9 -172.0(4) . . . . ?
N1 N2 C2 N3 -0.8(4) . . . . ?
N1 N2 C2 N5 177.5(4) . . . . ?
C2 N2 N1 V1 163.6(2) . . . . ?
C2 N2 N1 C1 0.4(4) . . . . ?
C2 N3 C1 N4 179.5(4) . . . . ?
C2 N3 C1 N1 -0.5(4) . . . . ?
C4 N8 C3 N6 -1.4(4) . . . . ?
C4 N8 C3 N9 172.9(4) . . . . ?
C3 N6 N7 V3 -167.5(2) . . . . ?
C3 N6 N7 C4 -2.0(4) . . . . ?
C3 N8 C4 N7 0.0(4) . . . . ?
C3 N8 C4 N10 178.4(3) . . . . ?
C1 N3 C2 N2 0.8(4) . . . . ?
C1 N3 C2 N5 -177.5(4) . . . . ?

_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 -0.027 0.000 0.500 163.5 76.7 '8 H2O'
2 -0.997 0.500 0.000 163.5 76.7 '8 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 7.500
_oxdiff_exptl_absorpt_empirical_full_min 0.527
# start Validation Reply Form
_vrf_PLAT420_exp_12327_auto      
;
PROBLEM: D-H Without Acceptor       O1W      --H1WA.
RESPONSE: The solvent molecules are highly disordered, which supposed to 
form hydrogen bond with water molecules have been removed by the Mask
routine in the PLATON software package.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_18883_vs-cit-hdatrz_auto
_database_code_depnum_ccdc_archive 'CCDC 2280842'
loop_
_audit_author_name
_audit_author_address
'Xie Zhen-Lang'
;Xiamen University
China
;
_audit_update_record             
;
2023-07-24 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_audit_creation_date             2023-07-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C12 H19 N15 O9 V2, C6 H4 O8 V, 2(C2 H6 N5), 0.5(O), 9[H2O]'
_chemical_formula_sum            'C22 H53 N25 O26.50 V3'
_chemical_formula_weight         1244.71
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N V K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.4466(4)
_cell_length_b                   10.7317(4)
_cell_length_c                   22.6402(6)
_cell_angle_alpha                82.025(2)
_cell_angle_beta                 89.802(3)
_cell_angle_gamma                78.306(3)
_cell_volume                     2460.67(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7022
_cell_measurement_temperature    233.00(10)
_cell_measurement_theta_max      68.5520
_cell_measurement_theta_min      3.9320
_shelx_estimated_absorpt_T_max   0.600
_shelx_estimated_absorpt_T_min   0.483
_exptl_absorpt_coefficient_mu    5.681
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1282
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16902
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.908
_diffrn_reflns_theta_min         3.944
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      233.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -76.00  -7.00   1.00    1.00    --  -40.50 125.00 120.00   69
  2  ω   -113.00 -22.00   1.00    1.00    --  -40.50 -37.00 -60.00   91
  3  ω   -110.00 -18.00   1.00    1.00    --  -40.50 -37.00  30.00   92
  4  ω     43.00  79.00   1.00    1.00    --   42.91-125.00   0.00   36
  5  ω     57.00 112.00   1.00    2.50    --   95.91-125.00 150.00   55
  6  ω    129.00 156.00   1.00    2.50    --   95.91 125.00   0.00   27
  7  ω     19.00  46.00   1.00    2.50    --   95.91 -94.00-150.00   27
  8  ω     29.00 116.00   1.00    2.50    --   95.91 -61.00 120.00   87
  9  ω     77.00 165.00   1.00    2.50    --   95.91  30.00-180.00   88
 10  ω     46.00 118.00   1.00    2.50    --   95.91 -30.00   0.00   72
 11  ω     97.00 137.00   1.00    2.50    --   95.91 125.00  90.00   40
 12  ω     32.00 100.00   1.00    2.50    --   95.91 -94.00 -60.00   68
 13  ω    108.00 161.00   1.00    2.50    --   95.91  77.00-180.00   53
 14  ω     85.00 112.00   1.00    2.50    --   95.91-125.00  60.00   27
 15  ω     69.00 103.00   1.00    2.50    --   95.91 -94.00-150.00   34
 16  ω     28.00 107.00   1.00    2.50    --   95.91 -61.00 -30.00   79
 17  ω     18.00 104.00   1.00    2.50    --   95.91 -15.00-180.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1463702000
_diffrn_orient_matrix_UB_12      0.0045792000
_diffrn_orient_matrix_UB_13      0.0110481000
_diffrn_orient_matrix_UB_21      0.0248555000
_diffrn_orient_matrix_UB_22      -0.1477718000
_diffrn_orient_matrix_UB_23      0.0062695000
_diffrn_orient_matrix_UB_31      0.0255311000
_diffrn_orient_matrix_UB_32      -0.0082739000
_diffrn_orient_matrix_UB_33      0.0675480000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7295
_reflns_number_total             8843
_reflns_odcompleteness_completeness 97.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         8843
_refine_ls_number_restraints     289
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0608
_refine_ls_restrained_S_all      1.083
_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)+(0.0456P)²+6.4511P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1502
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 N21-N22
 1.4 with sigma of 0.02
 C14-C13 = C023-C01W
 2.2 with sigma of 0.02
 N23-C023 = N23-C01W
 1.344 with sigma of 0.02
 N21-C023 = N22-C01W
 1.3 with sigma of 0.02
 N21-N22 = N22A-N21A
 1.4 with sigma of 0.02
 N24-C023 = N24A-C16 = N25-C01W = N25A-C15
 1.31 with sigma of 0.02
 N23-C023 = N23A-C16 = N21-C023 = N21A-C16 = N22-C01W = N22A-C15 = N23-C01W =
 N23A-C15
 1.34 with sigma of 0.02
 N24A-N25A
 4.68 with sigma of 0.02
 C023-C01W
 2.2 with sigma of 0.02
 C16-C15
 2.2 with sigma of 0.02
 N24-N25
 4.68 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N25A \\sim C15 \\sim N22A \\sim N23A \\sim N21A \\sim C16 \\sim N24A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N25 \\sim N22 \\sim N21 \\sim C01W \\sim C023 \\sim N23 \\sim N24: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(N25) \\sim Ueq, Uanis(N22) \\sim Ueq, Uanis(N21) \\sim Ueq, Uanis(C01W)
\\sim Ueq, Uanis(C023) \\sim Ueq, Uanis(N23) \\sim Ueq, Uanis(N24) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N25A) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(N22A) \\sim Ueq, Uanis(N23A)
\\sim Ueq, Uanis(N21A) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(N24A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N25A) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(N23A) \\sim Ueq, Uanis(N22A)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(N21A) \\sim Ueq, Uanis(N24A) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 N23A, N25A, C15, N22A, N21A, C16, N24A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C01W, N22, N21, C023, N25, N23, N24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(N25A)=Sof(H25C)=Sof(H25D)=Sof(N22A)=Sof(N21A)=Sof(H21C)=Sof(C15)=Sof(C16)=
 Sof(N23A)=Sof(H23A)=Sof(N24A)=Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(N22)=Sof(N21)=Sof(H21)=Sof(C023)=Sof(N23)=Sof(H23)=Sof(C01W)=Sof(N25)=
 Sof(H25A)=Sof(H25B)=Sof(N24)=Sof(H24A)=Sof(H24B)=FVAR(1)
 Fixed Sof: O1W(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C5(H5C,H5D), C18(H18A,H18B), C21(H21A,H21B), C2(H2A,H2B)
6.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N8(H8), N12(H12), N18(H18), N17(H17), N21(H21), N23(H23), N21A(H21C),
 N23A(H23A)
6.c Fitted pentagon refined as free rotating group:
 N22(N21,C023,N23,C01W)
6.d X=CH2 refined with riding coordinates:
 N14(H14A,H14B), N9(H9A,H9B), N4(H4A,H4B), N10(H10A,H10B), N5(H5A,H5B),
 N15(H15A,H15B), N19(H19A,H19B), N20(H20A,H20B), N25(H25A,H25B), N24(H24A,H24B),
  N25A(H25C,H25D), N24A(H24C,H24D)
;
_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
V2 V 0.89111(7) 0.99876(7) 0.29482(3) 0.01778(16) Uani 1 1 d . . . . .
V1 V 0.99367(7) 0.73867(7) 0.40746(3) 0.01941(17) Uani 1 1 d . . . . .
V3 V 1.05606(8) 1.41443(7) -0.05331(3) 0.02363(18) Uani 1 1 d . . . . .
O3 O 0.8597(3) 0.9055(3) 0.37889(12) 0.0188(6) Uani 1 1 d . . . . .
O1 O 0.7016(3) 1.0020(3) 0.27768(13) 0.0246(6) Uani 1 1 d . . . . .
O12 O 1.0354(3) 1.3940(3) 0.03385(12) 0.0213(6) Uani 1 1 d . . . . .
O6 O 0.9745(3) 0.8001(3) 0.48777(13) 0.0270(7) Uani 1 1 d . . . . .
O4 O 0.8234(3) 0.6796(3) 0.42261(14) 0.0277(7) Uani 1 1 d . . . . .
O10 O 0.8971(3) 1.3332(3) -0.05871(13) 0.0280(7) Uani 1 1 d . . . . .
O15 O 0.9870(3) 1.4938(3) 0.13777(13) 0.0307(7) Uani 1 1 d . . . . .
O8 O 0.9250(3) 1.0588(3) 0.22900(13) 0.0274(7) Uani 1 1 d . . . . .
O9 O 1.0999(3) 0.6079(3) 0.42915(13) 0.0298(7) Uani 1 1 d . . . . .
O13 O 0.7909(3) 1.4928(3) 0.04826(14) 0.0294(7) Uani 1 1 d . . . . .
N6 N 1.0786(3) 0.9625(3) 0.33262(15) 0.0197(7) Uani 1 1 d . . . . .
O17 O 1.1602(3) 1.2888(3) -0.06596(14) 0.0313(7) Uani 1 1 d . . . . .
N7 N 1.1214(3) 0.8583(3) 0.37803(15) 0.0210(7) Uani 1 1 d . . . . .
O2 O 0.5184(3) 0.9355(3) 0.29708(15) 0.0340(8) Uani 1 1 d . . . . .
O16 O 1.0306(4) 1.3486(3) 0.21793(14) 0.0398(9) Uani 1 1 d . . . . .
N2 N 0.9815(3) 0.7059(3) 0.31943(16) 0.0225(7) Uani 1 1 d . . . . .
O7 O 0.8789(3) 0.8840(4) 0.56428(14) 0.0418(9) Uani 1 1 d . . . . .
N13 N 0.7455(4) 1.3820(4) 0.33480(17) 0.0298(9) Uani 1 1 d . . . . .
O14 O 0.7347(4) 1.3079(4) 0.07896(19) 0.0468(10) Uani 1 1 d . . . . .
O11 O 0.8520(4) 1.1394(4) -0.04896(16) 0.0490(10) Uani 1 1 d . . . . .
N3 N 0.9708(4) 0.6354(4) 0.23389(16) 0.0267(8) Uani 1 1 d . . . . .
H3 H 0.978002 0.583448 0.207220 0.032 Uiso 1 1 calc R U . . .
N11 N 0.8425(4) 1.1780(3) 0.32561(16) 0.0243(8) Uani 1 1 d . . . . .
O5 O 0.6105(3) 0.7453(4) 0.43376(19) 0.0469(10) Uani 1 1 d . . . . .
N8 N 1.2898(3) 0.9409(4) 0.34928(16) 0.0244(8) Uani 1 1 d . . . . .
H8 H 1.369045 0.954669 0.347135 0.029 Uiso 1 1 calc R U . . .
N12 N 0.8824(4) 1.2105(4) 0.37942(16) 0.0265(8) Uani 1 1 d . . . . .
H12 H 0.935086 1.160019 0.406288 0.032 Uiso 1 1 calc R U . . .
N1 N 0.9304(3) 0.8104(3) 0.27538(15) 0.0220(7) Uani 1 1 d . . . . .
N14 N 0.6934(4) 1.2941(4) 0.24916(18) 0.0357(10) Uani 1 1 d . . . . .
H14A H 0.701415 1.228133 0.230011 0.043 Uiso 1 1 calc R U . . .
H14B H 0.641653 1.366250 0.235023 0.043 Uiso 1 1 calc R U . . .
N18 N 1.2433(4) 0.6863(4) 0.16654(18) 0.0344(9) Uani 1 1 d . . . . .
H18 H 1.217074 0.688019 0.129944 0.041 Uiso 1 1 calc R U . . .
N17 N 1.3208(4) 0.6224(4) 0.25480(18) 0.0388(10) Uani 1 1 d . . . . .
H17 H 1.355106 0.571856 0.286646 0.047 Uiso 1 1 calc R U . . .
N9 N 1.1902(4) 1.1046(4) 0.27202(18) 0.0337(9) Uani 1 1 d . . . . .
H9A H 1.120281 1.142960 0.250942 0.040 Uiso 1 1 calc R U . . .
H9B H 1.264117 1.128338 0.264486 0.040 Uiso 1 1 calc R U . . .
N4 N 0.8813(5) 0.8304(4) 0.17174(17) 0.0383(10) Uani 1 1 d . . . . .
H4A H 0.855207 0.913456 0.167948 0.046 Uiso 1 1 calc R U . . .
H4B H 0.880204 0.790398 0.140901 0.046 Uiso 1 1 calc R U . . .
C9 C 1.0053(4) 0.6034(4) 0.2928(2) 0.0250(9) Uani 1 1 d . . . . .
N10 N 1.3263(4) 0.7610(4) 0.42567(19) 0.0382(10) Uani 1 1 d . . . . .
H10A H 1.294527 0.704148 0.449178 0.046 Uiso 1 1 calc R U . . .
H10B H 1.409250 0.761900 0.427680 0.046 Uiso 1 1 calc R U . . .
N16 N 1.2867(4) 0.7559(5) 0.25115(18) 0.0399(10) Uani 1 1 d . . . . .
N5 N 1.0573(5) 0.4833(4) 0.31775(19) 0.0398(10) Uani 1 1 d . . . . .
H5A H 1.078905 0.467632 0.355531 0.048 Uiso 1 1 calc R U . . .
H5B H 1.069574 0.421023 0.296208 0.048 Uiso 1 1 calc R U . . .
C8 C 1.2474(4) 0.8473(4) 0.38637(19) 0.0231(9) Uani 1 1 d . . . . .
C20 C 0.8189(5) 1.3724(5) 0.0637(2) 0.0293(10) Uani 1 1 d . . . . .
C10 C 0.9229(4) 0.7643(4) 0.22482(19) 0.0247(9) Uani 1 1 d . . . . .
C4 C 0.7194(4) 0.7689(4) 0.4222(2) 0.0270(10) Uani 1 1 d . . . . .
N15 N 0.8446(5) 1.3935(4) 0.4283(2) 0.0443(11) Uani 1 1 d . . . . .
H15A H 0.896019 1.353533 0.458118 0.053 Uiso 1 1 calc R U . . .
H15B H 0.805479 1.473204 0.428319 0.053 Uiso 1 1 calc R U . . .
N19 N 1.1953(5) 0.9114(5) 0.1699(2) 0.0511(12) Uani 1 1 d . . . . .
H19A H 1.197129 0.975163 0.189540 0.061 Uiso 1 1 calc R U . . .
H19B H 1.165179 0.926235 0.133253 0.061 Uiso 1 1 calc R U . . .
C3 C 0.7438(4) 0.9059(4) 0.41101(19) 0.0233(9) Uani 1 1 d . . . . .
C12 C 0.8257(5) 1.3322(4) 0.3823(2) 0.0272(10) Uani 1 1 d . . . . .
C6 C 0.6132(4) 0.9770(4) 0.31382(19) 0.0223(9) Uani 1 1 d . . . . .
C1 C 0.8781(4) 0.8728(4) 0.5102(2) 0.0274(10) Uani 1 1 d . . . . .
N20 N 1.3151(5) 0.4617(5) 0.1937(2) 0.0529(13) Uani 1 1 d . . . . .
H20A H 1.348537 0.398998 0.221373 0.064 Uiso 1 1 calc R U . . .
H20B H 1.294597 0.445419 0.158765 0.064 Uiso 1 1 calc R U . . .
C11 C 0.7618(4) 1.2844(4) 0.3012(2) 0.0255(9) Uani 1 1 d . . . . .
C7 C 1.1841(4) 1.0081(4) 0.31644(19) 0.0235(9) Uani 1 1 d . . . . .
C19 C 0.9628(4) 1.3054(4) 0.06268(19) 0.0239(9) Uani 1 1 d . . . . .
N22 N 0.6414(9) 0.5455(6) 0.1853(3) 0.045(3) Uani 0.508(10) 1 d DG U P A 1
N21 N 0.5988(8) 0.5718(7) 0.1246(3) 0.048(2) Uani 0.508(10) 1 d DG U P A 1
H21 H 0.605029 0.515982 0.099728 0.058 Uiso 0.508(10) 1 calc R U P A 1
C023 C 0.5441(7) 0.7052(8) 0.1115(3) 0.042(2) Uani 0.508(10) 1 d DG U P A 1
N23 N 0.5529(7) 0.7614(5) 0.1642(4) 0.033(2) Uani 0.508(10) 1 d DG U P A 1
H23 H 0.526207 0.842071 0.167828 0.040 Uiso 0.508(10) 1 calc R U P A 1
C01W C 0.6131(8) 0.6626(7) 0.2098(3) 0.030(2) Uani 0.508(10) 1 d DG U P A 1
C17 C 0.9030(5) 1.2196(5) -0.0295(2) 0.0293(10) Uani 1 1 d . . . . .
C5 C 0.6267(4) 0.9998(5) 0.3782(2) 0.0268(10) Uani 1 1 d . . . . .
H5C H 0.546427 0.989646 0.399154 0.032 Uiso 1 1 calc R U . . .
H5D H 0.637789 1.088147 0.378751 0.032 Uiso 1 1 calc R U . . .
C18 C 0.9722(5) 1.1876(4) 0.03096(19) 0.0278(10) Uani 1 1 d . . . . .
H18A H 1.064553 1.149983 0.025880 0.033 Uiso 1 1 calc R U . . .
H18B H 0.933737 1.123142 0.055859 0.033 Uiso 1 1 calc R U . . .
C22 C 1.0102(5) 1.3760(4) 0.1632(2) 0.0282(10) Uani 1 1 d . . . . .
C13 C 1.2388(5) 0.7905(5) 0.1960(2) 0.0356(11) Uani 1 1 d D . . . .
C14 C 1.2955(5) 0.5811(5) 0.2047(2) 0.0328(11) Uani 1 1 d D . . . .
C21 C 1.0146(5) 1.2657(4) 0.12729(19) 0.0278(10) Uani 1 1 d . . . . .
H21A H 0.963479 1.206373 0.147743 0.033 Uiso 1 1 calc R U . . .
H21B H 1.105383 1.218854 0.126780 0.033 Uiso 1 1 calc R U . . .
C2 C 0.7633(5) 0.9490(5) 0.4724(2) 0.0296(10) Uani 1 1 d . . . . .
H2A H 0.772372 1.038979 0.465484 0.036 Uiso 1 1 calc R U . . .
H2B H 0.683827 0.945712 0.495166 0.036 Uiso 1 1 calc R U . . .
N25 N 0.6392(12) 0.6788(11) 0.2621(5) 0.039(3) Uani 0.508(10) 1 d D U P A 1
H25A H 0.678735 0.613986 0.287346 0.047 Uiso 0.508(10) 1 calc R U P A 1
H25B H 0.617758 0.754807 0.272894 0.047 Uiso 0.508(10) 1 calc R U P A 1
N24 N 0.5008(10) 0.7662(12) 0.0610(4) 0.059(3) Uani 0.508(10) 1 d D U P A 1
H24A H 0.503036 0.725720 0.030149 0.071 Uiso 0.508(10) 1 calc R U P A 1
H24B H 0.468865 0.848403 0.057285 0.071 Uiso 0.508(10) 1 calc R U P A 1
N25A N 0.6594(15) 0.6586(15) 0.2820(5) 0.047(4) Uani 0.492(10) 1 d D U P A 2
H25C H 0.696996 0.583919 0.300744 0.057 Uiso 0.492(10) 1 calc R U P A 2
H25D H 0.638731 0.724192 0.301316 0.057 Uiso 0.492(10) 1 calc R U P A 2
N22A N 0.6593(11) 0.5832(11) 0.1893(4) 0.033(2) Uani 0.492(10) 1 d D U P A 2
N21A N 0.6086(9) 0.6398(10) 0.1321(4) 0.038(2) Uani 0.492(10) 1 d D U P A 2
H21C H 0.613805 0.602631 0.100159 0.045 Uiso 0.492(10) 1 calc R U P A 2
C15 C 0.6340(17) 0.6725(13) 0.2245(6) 0.046(3) Uani 0.492(10) 1 d D U P A 2
C16 C 0.5519(12) 0.7597(11) 0.1362(5) 0.037(3) Uani 0.492(10) 1 d D U P A 2
N23A N 0.5615(10) 0.7844(9) 0.1935(5) 0.040(2) Uani 0.492(10) 1 d D U P A 2
H23A H 0.528981 0.855361 0.207424 0.048 Uiso 0.492(10) 1 calc R U P A 2
N24A N 0.4964(11) 0.8492(11) 0.0913(5) 0.061(3) Uani 0.492(10) 1 d D U P A 2
H24C H 0.495679 0.830141 0.055178 0.073 Uiso 0.492(10) 1 calc R U P A 2
H24D H 0.461146 0.926272 0.098240 0.073 Uiso 0.492(10) 1 calc R U P A 2
O1W O 0.4803(13) 0.6836(12) 0.0035(5) 0.094(4) Uani 0.5 1 d . . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V2 O3 2.082(3) . ?
V2 O1 2.012(3) . ?
V2 O8 1.608(3) . ?
V2 N6 2.081(3) . ?
V2 N11 2.101(4) . ?
V2 N1 2.087(4) . ?
V1 O3 2.062(3) . ?
V1 O6 2.014(3) . ?
V1 O4 2.019(3) . ?
V1 O9 1.620(3) . ?
V1 N7 2.080(3) . ?
V1 N2 2.080(4) . ?
V3 O12 2.188(3) 2_785 ?
V3 O12 1.971(3) . ?
V3 O10 2.037(3) . ?
V3 O15 2.033(3) 2_785 ?
V3 O13 2.059(3) 2_785 ?
V3 O17 1.611(3) . ?
O3 C3 1.409(5) . ?
O1 C6 1.276(5) . ?
O12 C19 1.421(5) . ?
O6 C1 1.292(5) . ?
O4 C4 1.294(6) . ?
O10 C17 1.293(6) . ?
O15 C22 1.290(6) . ?
O13 C20 1.264(6) . ?
N6 N7 1.410(5) . ?
N6 C7 1.324(5) . ?
N7 C8 1.310(5) . ?
O2 C6 1.246(5) . ?
O16 C22 1.242(5) . ?
N2 N1 1.410(5) . ?
N2 C9 1.308(6) . ?
O7 C1 1.248(5) . ?
N13 C12 1.344(6) . ?
N13 C11 1.361(6) . ?
O14 C20 1.246(6) . ?
O11 C17 1.229(6) . ?
N3 H3 0.8700 . ?
N3 C9 1.360(6) . ?
N3 C10 1.360(6) . ?
N11 N12 1.400(5) . ?
N11 C11 1.326(6) . ?
O5 C4 1.234(5) . ?
N8 H8 0.8700 . ?
N8 C8 1.361(6) . ?
N8 C7 1.352(6) . ?
N12 H12 0.8700 . ?
N12 C12 1.331(6) . ?
N1 C10 1.317(5) . ?
N14 H14A 0.8700 . ?
N14 H14B 0.8700 . ?
N14 C11 1.361(6) . ?
N18 H18 0.8700 . ?
N18 C13 1.372(6) . ?
N18 C14 1.341(6) . ?
N17 H17 0.8700 . ?
N17 N16 1.395(6) . ?
N17 C14 1.320(6) . ?
N9 H9A 0.8700 . ?
N9 H9B 0.8700 . ?
N9 C7 1.351(6) . ?
N4 H4A 0.8700 . ?
N4 H4B 0.8700 . ?
N4 C10 1.333(6) . ?
C9 N5 1.338(6) . ?
N10 H10A 0.8700 . ?
N10 H10B 0.8700 . ?
N10 C8 1.340(6) . ?
N16 C13 1.322(7) . ?
N5 H5A 0.8700 . ?
N5 H5B 0.8700 . ?
C20 C19 1.531(7) . ?
C4 C3 1.529(6) . ?
N15 H15A 0.8700 . ?
N15 H15B 0.8700 . ?
N15 C12 1.343(6) . ?
N19 H19A 0.8700 . ?
N19 H19B 0.8700 . ?
N19 C13 1.338(7) . ?
C3 C5 1.537(6) . ?
C3 C2 1.551(6) . ?
C6 C5 1.522(6) . ?
C1 C2 1.502(6) . ?
N20 H20A 0.8700 . ?
N20 H20B 0.8700 . ?
N20 C14 1.314(7) . ?
C19 C18 1.525(6) . ?
C19 C21 1.534(6) . ?
N22 N21 1.4200 . ?
N22 C01W 1.4200 . ?
N21 H21 0.8700 . ?
N21 C023 1.4200 . ?
C023 N23 1.4200 . ?
C023 N24 1.271(9) . ?
N23 H23 0.8700 . ?
N23 C01W 1.4200 . ?
C01W N25 1.258(11) . ?
C17 C18 1.513(6) . ?
C5 H5C 0.9800 . ?
C5 H5D 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C22 C21 1.520(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
N25 H25A 0.8700 . ?
N25 H25B 0.8700 . ?
N24 H24A 0.8700 . ?
N24 H24B 0.8700 . ?
N24 O1W 1.709(17) . ?
N25A H25C 0.8700 . ?
N25A H25D 0.8700 . ?
N25A C15 1.311(13) . ?
N22A N21A 1.407(11) . ?
N22A C15 1.315(14) . ?
N21A H21C 0.8700 . ?
N21A C16 1.319(12) . ?
C15 N23A 1.382(13) . ?
C16 N23A 1.366(12) . ?
C16 N24A 1.342(12) . ?
N23A H23A 0.8700 . ?
N24A H24C 0.8700 . ?
N24A H24D 0.8700 . ?

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
O3 V2 N11 90.65(13) . . ?
O3 V2 N1 81.62(12) . . ?
O1 V2 O3 85.52(11) . . ?
O1 V2 N6 164.69(13) . . ?
O1 V2 N11 91.04(13) . . ?
O1 V2 N1 87.12(13) . . ?
O8 V2 O3 174.65(15) . . ?
O8 V2 O1 96.92(14) . . ?
O8 V2 N6 97.83(15) . . ?
O8 V2 N11 94.06(15) . . ?
O8 V2 N1 93.72(15) . . ?
N6 V2 O3 79.44(12) . . ?
N6 V2 N11 91.98(14) . . ?
N6 V2 N1 87.87(14) . . ?
N1 V2 N11 172.17(14) . . ?
O3 V1 N7 80.59(12) . . ?
O3 V1 N2 84.13(13) . . ?
O6 V1 O3 84.36(12) . . ?
O6 V1 O4 87.05(13) . . ?
O6 V1 N7 93.20(13) . . ?
O6 V1 N2 168.35(13) . . ?
O4 V1 O3 78.75(11) . . ?
O4 V1 N7 159.22(13) . . ?
O4 V1 N2 88.91(14) . . ?
O9 V1 O3 179.29(14) . . ?
O9 V1 O6 96.19(14) . . ?
O9 V1 O4 101.71(15) . . ?
O9 V1 N7 98.92(15) . . ?
O9 V1 N2 95.33(15) . . ?
N7 V1 N2 86.73(14) . . ?
O12 V3 O12 74.96(12) . 2_785 ?
O12 V3 O10 87.50(12) . . ?
O12 V3 O15 153.61(13) . 2_785 ?
O12 V3 O13 92.46(13) . 2_785 ?
O10 V3 O12 101.31(12) . 2_785 ?
O10 V3 O13 176.52(13) . 2_785 ?
O15 V3 O12 80.24(11) 2_785 2_785 ?
O15 V3 O10 88.66(13) 2_785 . ?
O15 V3 O13 89.84(13) 2_785 2_785 ?
O13 V3 O12 75.33(12) 2_785 2_785 ?
O17 V3 O12 105.47(14) . . ?
O17 V3 O12 163.86(15) . 2_785 ?
O17 V3 O10 94.82(15) . . ?
O17 V3 O15 100.87(15) . 2_785 ?
O17 V3 O13 88.55(15) . 2_785 ?
V1 O3 V2 115.45(13) . . ?
C3 O3 V2 130.7(2) . . ?
C3 O3 V1 109.5(2) . . ?
C6 O1 V2 129.0(3) . . ?
V3 O12 V3 105.04(12) . 2_785 ?
C19 O12 V3 107.8(2) . 2_785 ?
C19 O12 V3 121.2(2) . . ?
C1 O6 V1 131.0(3) . . ?
C4 O4 V1 116.4(3) . . ?
C17 O10 V3 117.5(3) . . ?
C22 O15 V3 135.8(3) . 2_785 ?
C20 O13 V3 115.2(3) . 2_785 ?
N7 N6 V2 121.5(2) . . ?
C7 N6 V2 131.9(3) . . ?
C7 N6 N7 105.7(3) . . ?
N6 N7 V1 119.0(2) . . ?
C8 N7 V1 132.3(3) . . ?
C8 N7 N6 107.8(3) . . ?
N1 N2 V1 118.8(2) . . ?
C9 N2 V1 134.3(3) . . ?
C9 N2 N1 106.7(3) . . ?
C12 N13 C11 103.0(4) . . ?
C9 N3 H3 126.7 . . ?
C10 N3 H3 126.7 . . ?
C10 N3 C9 106.7(4) . . ?
N12 N11 V2 127.6(3) . . ?
C11 N11 V2 129.1(3) . . ?
C11 N11 N12 103.2(3) . . ?
C8 N8 H8 126.9 . . ?
C7 N8 H8 126.9 . . ?
C7 N8 C8 106.2(3) . . ?
N11 N12 H12 126.0 . . ?
C12 N12 N11 108.1(3) . . ?
C12 N12 H12 126.0 . . ?
N2 N1 V2 121.2(2) . . ?
C10 N1 V2 131.2(3) . . ?
C10 N1 N2 107.5(3) . . ?
H14A N14 H14B 120.0 . . ?
C11 N14 H14A 120.0 . . ?
C11 N14 H14B 120.0 . . ?
C13 N18 H18 126.4 . . ?
C14 N18 H18 126.4 . . ?
C14 N18 C13 107.3(4) . . ?
N16 N17 H17 123.7 . . ?
C14 N17 H17 123.7 . . ?
C14 N17 N16 112.7(4) . . ?
H9A N9 H9B 120.0 . . ?
C7 N9 H9A 120.0 . . ?
C7 N9 H9B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C10 N4 H4A 120.0 . . ?
C10 N4 H4B 120.0 . . ?
N2 C9 N3 110.0(4) . . ?
N2 C9 N5 126.7(4) . . ?
N5 C9 N3 123.3(4) . . ?
H10A N10 H10B 120.0 . . ?
C8 N10 H10A 120.0 . . ?
C8 N10 H10B 120.0 . . ?
C13 N16 N17 102.2(4) . . ?
C9 N5 H5A 120.0 . . ?
C9 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
N7 C8 N8 109.6(4) . . ?
N7 C8 N10 127.2(4) . . ?
N10 C8 N8 123.1(4) . . ?
O13 C20 C19 117.5(4) . . ?
O14 C20 O13 122.7(5) . . ?
O14 C20 C19 119.7(4) . . ?
N1 C10 N3 109.1(4) . . ?
N1 C10 N4 127.3(4) . . ?
N4 C10 N3 123.6(4) . . ?
O4 C4 C3 114.6(4) . . ?
O5 C4 O4 122.6(4) . . ?
O5 C4 C3 122.6(4) . . ?
H15A N15 H15B 120.0 . . ?
C12 N15 H15A 120.0 . . ?
C12 N15 H15B 120.0 . . ?
H19A N19 H19B 120.0 . . ?
C13 N19 H19A 120.0 . . ?
C13 N19 H19B 120.0 . . ?
O3 C3 C4 108.9(3) . . ?
O3 C3 C5 111.6(3) . . ?
O3 C3 C2 108.5(3) . . ?
C4 C3 C5 111.4(4) . . ?
C4 C3 C2 108.0(4) . . ?
C5 C3 C2 108.3(4) . . ?
N12 C12 N13 111.3(4) . . ?
N12 C12 N15 123.1(4) . . ?
N15 C12 N13 125.5(4) . . ?
O1 C6 C5 118.0(4) . . ?
O2 C6 O1 121.2(4) . . ?
O2 C6 C5 120.8(4) . . ?
O6 C1 C2 121.8(4) . . ?
O7 C1 O6 120.6(4) . . ?
O7 C1 C2 117.6(4) . . ?
H20A N20 H20B 120.0 . . ?
C14 N20 H20A 120.0 . . ?
C14 N20 H20B 120.0 . . ?
N13 C11 N14 122.0(4) . . ?
N11 C11 N13 114.2(4) . . ?
N11 C11 N14 123.6(4) . . ?
N6 C7 N8 110.6(4) . . ?
N6 C7 N9 126.3(4) . . ?
N9 C7 N8 123.1(4) . . ?
O12 C19 C20 109.0(3) . . ?
O12 C19 C18 112.1(4) . . ?
O12 C19 C21 108.1(3) . . ?
C20 C19 C21 108.4(4) . . ?
C18 C19 C20 108.6(4) . . ?
C18 C19 C21 110.6(4) . . ?
N21 N22 C01W 108.0 . . ?
N22 N21 H21 126.0 . . ?
N22 N21 C023 108.0 . . ?
C023 N21 H21 126.0 . . ?
N21 C023 N23 108.0 . . ?
N24 C023 N21 126.6(8) . . ?
N24 C023 N23 125.3(8) . . ?
C023 N23 H23 126.0 . . ?
C023 N23 C01W 108.0 . . ?
C01W N23 H23 126.0 . . ?
N22 C01W N23 108.0 . . ?
N25 C01W N22 126.8(7) . . ?
N25 C01W N23 125.1(7) . . ?
O10 C17 C18 118.2(4) . . ?
O11 C17 O10 121.9(4) . . ?
O11 C17 C18 119.9(4) . . ?
C3 C5 H5C 109.3 . . ?
C3 C5 H5D 109.3 . . ?
C6 C5 C3 111.8(4) . . ?
C6 C5 H5C 109.3 . . ?
C6 C5 H5D 109.3 . . ?
H5C C5 H5D 107.9 . . ?
C19 C18 H18A 109.1 . . ?
C19 C18 H18B 109.1 . . ?
C17 C18 C19 112.3(4) . . ?
C17 C18 H18A 109.1 . . ?
C17 C18 H18B 109.1 . . ?
H18A C18 H18B 107.9 . . ?
O15 C22 C21 121.2(4) . . ?
O16 C22 O15 121.2(4) . . ?
O16 C22 C21 117.6(4) . . ?
N16 C13 N18 111.7(5) . . ?
N16 C13 N19 125.6(5) . . ?
N19 C13 N18 122.7(5) . . ?
N17 C14 N18 106.1(4) . . ?
N20 C14 N18 126.1(5) . . ?
N20 C14 N17 127.7(5) . . ?
C19 C21 H21A 108.5 . . ?
C19 C21 H21B 108.5 . . ?
C22 C21 C19 115.1(4) . . ?
C22 C21 H21A 108.5 . . ?
C22 C21 H21B 108.5 . . ?
H21A C21 H21B 107.5 . . ?
C3 C2 H2A 108.2 . . ?
C3 C2 H2B 108.2 . . ?
C1 C2 C3 116.4(4) . . ?
C1 C2 H2A 108.2 . . ?
C1 C2 H2B 108.2 . . ?
H2A C2 H2B 107.3 . . ?
C01W N25 H25A 120.0 . . ?
C01W N25 H25B 120.0 . . ?
H25A N25 H25B 120.0 . . ?
C023 N24 H24A 120.0 . . ?
C023 N24 H24B 120.0 . . ?
C023 N24 O1W 119.9(10) . . ?
H24A N24 H24B 120.0 . . ?
O1W N24 H24A 9.3 . . ?
O1W N24 H24B 119.3 . . ?
H25C N25A H25D 120.0 . . ?
C15 N25A H25C 120.0 . . ?
C15 N25A H25D 120.0 . . ?
C15 N22A N21A 107.3(10) . . ?
N22A N21A H21C 126.5 . . ?
C16 N21A N22A 107.0(9) . . ?
C16 N21A H21C 126.5 . . ?
N25A C15 N22A 127.1(13) . . ?
N25A C15 N23A 122.7(13) . . ?
N22A C15 N23A 109.9(11) . . ?
N21A C16 N23A 110.4(9) . . ?
N21A C16 N24A 126.5(11) . . ?
N24A C16 N23A 123.1(11) . . ?
C15 N23A H23A 127.4 . . ?
C16 N23A C15 105.3(9) . . ?
C16 N23A H23A 127.4 . . ?
C16 N24A H24C 120.0 . . ?
C16 N24A H24D 120.0 . . ?
H24C N24A H24D 120.0 . . ?

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
N3 H3 O15 0.87 1.95 2.808(5) 170.2 1_545 yes
N8 H8 O2 0.87 1.92 2.654(5) 141.3 1_655 yes
N12 H12 O7 0.87 2.00 2.741(5) 142.6 2_776 yes
N14 H14B N22 0.87 2.09 2.827(7) 142.2 1_565 yes
N18 H18 O10 0.87 2.07 2.906(5) 159.8 2_775 yes
N9 H9A O16 0.87 2.24 2.914(5) 134.2 . yes
N4 H4B O17 0.87 2.08 2.939(5) 169.0 2_775 yes
N10 H10B O5 0.87 2.08 2.945(5) 174.6 1_655 yes
N5 H5B O16 0.87 2.10 2.890(5) 149.9 1_545 yes
N15 H15A O6 0.87 2.14 2.972(5) 159.1 2_776 yes
N19 H19B O11 0.87 2.14 2.927(6) 149.5 2_775 yes
N25A H25C N13 0.87 2.15 2.999(15) 163.6 1_545 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
V2 O3 C3 C4 118.5(3) . . . . ?
V2 O3 C3 C5 -4.9(5) . . . . ?
V2 O3 C3 C2 -124.1(3) . . . . ?
V2 O1 C6 O2 -152.2(3) . . . . ?
V2 O1 C6 C5 27.9(6) . . . . ?
V2 N6 N7 V1 0.1(4) . . . . ?
V2 N6 N7 C8 170.3(3) . . . . ?
V2 N6 C7 N8 -169.9(3) . . . . ?
V2 N6 C7 N9 7.6(7) . . . . ?
V2 N11 N12 C12 -177.8(3) . . . . ?
V2 N11 C11 N13 175.9(3) . . . . ?
V2 N11 C11 N14 0.3(7) . . . . ?
V2 N1 C10 N3 174.2(3) . . . . ?
V2 N1 C10 N4 -3.0(7) . . . . ?
V1 O3 C3 C4 -36.5(4) . . . . ?
V1 O3 C3 C5 -159.9(3) . . . . ?
V1 O3 C3 C2 80.8(3) . . . . ?
V1 O6 C1 O7 169.3(3) . . . . ?
V1 O6 C1 C2 -12.3(6) . . . . ?
V1 O4 C4 O5 -176.4(4) . . . . ?
V1 O4 C4 C3 -0.8(5) . . . . ?
V1 N7 C8 N8 169.4(3) . . . . ?
V1 N7 C8 N10 -12.1(7) . . . . ?
V1 N2 N1 V2 8.3(4) . . . . ?
V1 N2 N1 C10 -175.1(3) . . . . ?
V1 N2 C9 N3 175.2(3) . . . . ?
V1 N2 C9 N5 -5.5(7) . . . . ?
V3 O12 C19 C20 32.6(4) 2_785 . . . ?
V3 O12 C19 C20 -88.2(4) . . . . ?
V3 O12 C19 C18 152.9(3) 2_785 . . . ?
V3 O12 C19 C18 32.1(5) . . . . ?
V3 O12 C19 C21 -85.0(3) 2_785 . . . ?
V3 O12 C19 C21 154.2(3) . . . . ?
V3 O10 C17 O11 -144.3(4) . . . . ?
V3 O10 C17 C18 37.1(5) . . . . ?
V3 O15 C22 O16 -177.9(3) 2_785 . . . ?
V3 O15 C22 C21 2.6(7) 2_785 . . . ?
V3 O13 C20 O14 159.6(4) 2_785 . . . ?
V3 O13 C20 C19 -20.9(5) 2_785 . . . ?
O3 C3 C5 C6 51.9(5) . . . . ?
O3 C3 C2 C1 -55.7(5) . . . . ?
O1 C6 C5 C3 -67.6(5) . . . . ?
O12 C19 C18 C17 -68.4(5) . . . . ?
O12 C19 C21 C22 56.8(5) . . . . ?
O6 C1 C2 C3 18.5(6) . . . . ?
O4 C4 C3 O3 25.4(5) . . . . ?
O4 C4 C3 C5 148.9(4) . . . . ?
O4 C4 C3 C2 -92.3(4) . . . . ?
O10 C17 C18 C19 30.1(6) . . . . ?
O15 C22 C21 C19 -11.9(6) . . . . ?
O13 C20 C19 O12 -10.0(5) . . . . ?
O13 C20 C19 C18 -132.5(4) . . . . ?
O13 C20 C19 C21 107.4(4) . . . . ?
N6 N7 C8 N8 1.1(5) . . . . ?
N6 N7 C8 N10 179.6(4) . . . . ?
N7 N6 C7 N8 -1.0(5) . . . . ?
N7 N6 C7 N9 176.5(4) . . . . ?
O2 C6 C5 C3 112.5(5) . . . . ?
O16 C22 C21 C19 168.5(4) . . . . ?
N2 N1 C10 N3 -2.0(5) . . . . ?
N2 N1 C10 N4 -179.2(4) . . . . ?
O7 C1 C2 C3 -163.1(4) . . . . ?
O14 C20 C19 O12 169.6(4) . . . . ?
O14 C20 C19 C18 47.1(6) . . . . ?
O14 C20 C19 C21 -73.0(5) . . . . ?
O11 C17 C18 C19 -148.5(5) . . . . ?
N11 N12 C12 N13 2.6(5) . . . . ?
N11 N12 C12 N15 -179.5(4) . . . . ?
O5 C4 C3 O3 -159.0(4) . . . . ?
O5 C4 C3 C5 -35.5(6) . . . . ?
O5 C4 C3 C2 83.3(5) . . . . ?
N12 N11 C11 N13 -0.5(5) . . . . ?
N12 N11 C11 N14 -176.2(4) . . . . ?
N1 N2 C9 N3 -0.8(5) . . . . ?
N1 N2 C9 N5 178.4(4) . . . . ?
N17 N16 C13 N18 -0.4(5) . . . . ?
N17 N16 C13 N19 -178.0(5) . . . . ?
C9 N2 N1 V2 -174.9(3) . . . . ?
C9 N2 N1 C10 1.7(4) . . . . ?
C9 N3 C10 N1 1.5(5) . . . . ?
C9 N3 C10 N4 178.8(4) . . . . ?
N16 N17 C14 N18 -0.3(6) . . . . ?
N16 N17 C14 N20 -179.5(5) . . . . ?
C8 N8 C7 N6 1.6(5) . . . . ?
C8 N8 C7 N9 -176.0(4) . . . . ?
C20 C19 C18 C17 52.1(5) . . . . ?
C20 C19 C21 C22 -61.2(5) . . . . ?
C10 N3 C9 N2 -0.3(5) . . . . ?
C10 N3 C9 N5 -179.6(4) . . . . ?
C4 C3 C5 C6 -70.1(4) . . . . ?
C4 C3 C2 C1 62.2(5) . . . . ?
C12 N13 C11 N11 2.0(5) . . . . ?
C12 N13 C11 N14 177.8(4) . . . . ?
C11 N13 C12 N12 -2.8(5) . . . . ?
C11 N13 C12 N15 179.3(5) . . . . ?
C11 N11 N12 C12 -1.2(5) . . . . ?
C7 N6 N7 V1 -170.2(3) . . . . ?
C7 N6 N7 C8 -0.1(4) . . . . ?
C7 N8 C8 N7 -1.6(5) . . . . ?
C7 N8 C8 N10 179.7(4) . . . . ?
N22 N21 C023 N23 0.0 . . . . ?
N22 N21 C023 N24 176.6(10) . . . . ?
N21 N22 C01W N23 0.0 . . . . ?
N21 N22 C01W N25 -178.2(11) . . . . ?
N21 C023 N23 C01W 0.0 . . . . ?
N21 C023 N24 O1W 10.7(14) . . . . ?
C023 N23 C01W N22 0.0 . . . . ?
C023 N23 C01W N25 178.2(11) . . . . ?
N23 C023 N24 O1W -173.3(7) . . . . ?
C01W N22 N21 C023 0.0 . . . . ?
C5 C3 C2 C1 -177.0(4) . . . . ?
C18 C19 C21 C22 179.8(4) . . . . ?
C13 N18 C14 N17 0.0(5) . . . . ?
C13 N18 C14 N20 179.2(5) . . . . ?
C14 N18 C13 N16 0.3(6) . . . . ?
C14 N18 C13 N19 178.0(5) . . . . ?
C14 N17 N16 C13 0.4(6) . . . . ?
C21 C19 C18 C17 171.0(4) . . . . ?
C2 C3 C5 C6 171.3(4) . . . . ?
N24 C023 N23 C01W -176.7(10) . . . . ?
N25A C15 N23A C16 -177.5(17) . . . . ?
N22A N21A C16 N23A -0.7(14) . . . . ?
N22A N21A C16 N24A 176.8(12) . . . . ?
N22A C15 N23A C16 -3.9(16) . . . . ?
N21A N22A C15 N25A 176.8(18) . . . . ?
N21A N22A C15 N23A 3.6(16) . . . . ?
N21A C16 N23A C15 2.7(15) . . . . ?
C15 N22A N21A C16 -1.8(14) . . . . ?
N24A C16 N23A C15 -174.8(13) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 -0.432 -0.149 550.7 176.5 '18 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.425
_oxdiff_exptl_absorpt_empirical_full_min 0.741
####################################################################### 
# 
# 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_exp_13142_k2v8_auto
_database_code_depnum_ccdc_archive 'CCDC 2262729'
loop_
_audit_author_name
_audit_author_address
'Xie Zhen-Lang'
;Xiamen University
China
;
_audit_update_record             
;
2023-07-24 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_audit_creation_date             2023-07-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H59 K2 N40 O43.5 V8, 20[H2O]'
_chemical_formula_sum            'C40 H99 K2 N40 O63.50 V8'
_chemical_formula_weight         2642.31
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   20.30450(10)
_cell_length_b                   18.4546(2)
_cell_length_c                   26.9082(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.6380(10)
_cell_angle_gamma                90
_cell_volume                     10062.49(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    31273
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      69.2920
_cell_measurement_theta_min      2.8160
_shelx_estimated_absorpt_T_max   0.509
_shelx_estimated_absorpt_T_min   0.304
_exptl_absorpt_coefficient_mu    7.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5396
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            71737
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.730
_diffrn_reflns_theta_min         2.647
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -114.00 -69.00   0.50    0.60    --  -42.99-147.00-117.00   90
  2  ω    -92.00 -46.00   0.50    0.60    --  -42.99 125.00 125.00   92
  3  ω    -98.00 -71.00   0.50    0.60    --  -42.99-125.00  47.00   54
  4  ω     54.00  80.00   0.50    0.60    --   45.49-125.00  47.00   52
  5  ω     54.00  79.00   0.50    0.60    --   45.49-147.00-117.00   50
  6  ω    -81.00 -56.00   0.50    2.40    --  -95.46 125.00 125.00   50
  7  ω    -96.00 -61.00   0.50    2.40    --  -95.46-147.00-117.00   70
  8  ω   -143.00-118.00   0.50    2.40    --  -95.46-125.00  47.00   50
  9  ω     46.00 132.00   0.50    2.40    --   97.96-147.00-117.00  172
 10  ω     31.00 108.00   0.50    2.40    --   97.96-125.00  47.00  154
 11  ω    -17.00  15.00   0.50    0.60    --  -42.99  19.00-120.00   64
 12  ω    -25.00  38.00   0.50    0.60    --  -42.99  19.00 -30.00  126
 13  ω   -116.00 -76.00   0.50    0.60    --  -42.99-125.00 120.00   80
 14  ω    -24.00  17.00   0.50    0.60    --  -42.99  19.00-150.00   82
 15  ω    -51.00 -26.00   0.50    2.40    --  -95.46  45.00  60.00   50
 16  ω   -105.00 -74.00   0.50    2.40    --  -95.46  77.00 120.00   62
 17  ω    -86.00 -22.00   0.50    2.40    --  -95.46 125.00  90.00  128
 18  ω    -50.00 -22.00   0.50    2.40    --  -95.46 125.00-120.00   56
 19  ω    -51.00 -26.00   0.50    2.40    --  -95.46  45.00 -30.00   50
 20  ω    -51.00 -26.00   0.50    2.40    --  -95.46  45.00 -60.00   50
 21  ω    -67.00 -30.00   0.50    2.40    --  -95.46  77.00 120.00   74
 22  ω    -91.00 -57.00   0.50    2.40    --  -95.46 125.00-120.00   68
 23  ω   -167.00 -80.00   0.50    2.40    --  -95.46 -95.00-180.00  174
 24  ω     21.00  99.00   0.50    2.40    --   97.96 -95.00  60.00  156
 25  ω     25.00  51.00   0.50    2.40    --   97.96 -45.00-150.00   52
 26  ω     38.00  63.00   0.50    2.40    --   97.96 -61.00-180.00   50
 27  ω     80.00 171.00   0.50    2.40    --   97.96  45.00 -60.00  182
 28  ω     23.00  48.00   0.50    2.40    --   97.96 -45.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0536972000
_diffrn_orient_matrix_UB_12      0.0049892000
_diffrn_orient_matrix_UB_13      -0.0429801000
_diffrn_orient_matrix_UB_21      0.0073765000
_diffrn_orient_matrix_UB_22      0.0830940000
_diffrn_orient_matrix_UB_23      -0.0003235000
_diffrn_orient_matrix_UB_31      0.0533099000
_diffrn_orient_matrix_UB_32      -0.0064170000
_diffrn_orient_matrix_UB_33      -0.0379900000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15885
_reflns_number_total             18443
_reflns_odcompleteness_completeness 98.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1256
_refine_ls_number_reflns         18443
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0483
_refine_ls_restrained_S_all      1.058
_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)+(0.0785P)²+16.6432P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1424
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups, All O(H,H,H,H) groups
2. Restrained distances
 K2A-O31 \\sim K2-O31
 with sigma of 0.02
 O22A-C40 \\sim O22-C40
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O9W \\sim O9WA: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
K2 \\sim K2A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
O22 \\sim O22A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(O2W) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O3W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O10W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(K2) \\sim Ueq, Uanis(K2A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O9W) \\sim Ueq, Uanis(O9WA) \\sim Ueq, Uanis(O8W) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 K2A, O31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 K2, O31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(K2)=Sof(H6WC)=Sof(H6WD)=Sof(O9WA)=Sof(O22)=1-FVAR(1)
 Sof(K2A)=Sof(H6WA)=Sof(H6WB)=Sof(O9W)=Sof(O22A)=FVAR(1)
 Fixed Sof: O2W(0.5) H2WA(0.5) H2WB(0.5) O3W(0.25) O5W(0.25) O8W(0.5)
6.a Riding coordinates:
 O6W(H6WA,H6WB), O6W(H6WC,H6WD)
6.b Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O10W(H10C,H10D)
6.c Secondary CH2 refined with riding coordinates:
 C15(H15C,H15D), C18(H18A,H18B), C23(H23A,H23B), C30(H30C,H30D), C32(H32A,
 H32B), C34(H34C,H34D), C37(H37A,H37B), C39(H39C,H39D)
6.d Aromatic/amide H refined with riding coordinates:
 N3(H3), N13(H13), N23(H23), N33(H33)
6.e X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N5(H5A,H5B), N9(H9A,H9B), N10(H10A,H10B), N14(H14A,H14B),
 N15(H15A,H15B), N19(H19A,H19B), N20(H20A,H20B), N24(H24A,H24B), N25(H25A,H25B),
  N29(H29A,H29B), N30(H30A,H30B), N34(H34A,H34B), N35(H35A,H35B), N39(H39A,
 H39B), N40(H40A,H40B)
;
_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
V2 V 0.20198(3) 0.82490(3) 0.70846(2) 0.02107(13) Uani 1 1 d . . . . .
V1 V 0.13153(3) 0.65157(3) 0.71623(2) 0.02429(13) Uani 1 1 d . . . . .
V4 V 0.13881(3) 0.71622(3) 0.48894(2) 0.02174(13) Uani 1 1 d . . . . .
V3 V 0.13359(3) 0.88366(3) 0.42695(2) 0.02337(13) Uani 1 1 d . . . . .
V6 V 0.42153(3) 0.80747(3) 0.44669(2) 0.01922(12) Uani 1 1 d . . . . .
V5 V 0.47127(3) 0.62700(3) 0.43928(2) 0.02151(13) Uani 1 1 d . . . . .
V8 V 0.47430(3) 0.70218(3) 0.66608(2) 0.01748(12) Uani 1 1 d . . . . .
V7 V 0.49877(3) 0.87065(3) 0.72377(2) 0.01982(12) Uani 1 1 d . . . . .
K1 K 0.30862(4) 0.60773(5) 0.92587(3) 0.0399(2) Uani 1 1 d . . . . .
K2 K 0.80177(14) 0.8913(2) 0.72375(12) 0.0816(10) Uani 0.552(4) 1 d D U P A 2
K2A K 0.81619(19) 0.8461(3) 0.70952(16) 0.0837(10) Uani 0.448(4) 1 d D U P A 1
O16 O 0.17582(12) 0.63845(14) 0.49119(9) 0.0307(5) Uani 1 1 d . . . . .
O1 O 0.23794(11) 0.85043(14) 0.77735(8) 0.0268(5) Uani 1 1 d . . . . .
O1W O 0.31415(12) 0.75621(16) 0.94075(10) 0.0368(6) Uani 1 1 d . . . . .
H1WA H 0.301527 0.778311 0.913046 0.055 Uiso 1 1 d R U . . .
H1WB H 0.355040 0.769462 0.946634 0.055 Uiso 1 1 d R U . . .
O2 O 0.26568(13) 0.82859(15) 0.85635(9) 0.0328(6) Uani 1 1 d . . . . .
O2W O 0.2983(4) 0.5805(4) 1.0343(3) 0.069(2) Uani 0.5 1 d . U P . .
H2WA H 0.337777 0.582931 1.050149 0.104 Uiso 0.5 1 d R U P . .
H2WB H 0.285659 0.535177 1.038929 0.104 Uiso 0.5 1 d R U P . .
O3 O 0.21506(11) 0.71706(13) 0.73098(8) 0.0221(5) Uani 1 1 d . . . . .
O3W O 0.2108(8) 0.6231(9) 0.9822(7) 0.073(4) Uani 0.25 1 d . U P . .
O4 O 0.15063(11) 0.63351(14) 0.78963(9) 0.0278(5) Uani 1 1 d . . . . .
O4W O 0.23853(14) 0.48441(15) 0.88992(10) 0.0392(6) Uani 1 1 d . . . . .
O5 O 0.22023(12) 0.65828(14) 0.85422(9) 0.0289(5) Uani 1 1 d . . . . .
O5W O 0.7359(11) 0.9297(12) 0.7801(8) 0.103(6) Uani 0.25 1 d . U P . .
O6 O 0.20033(12) 0.57596(14) 0.70288(9) 0.0291(5) Uani 1 1 d . . . . .
O6W O 0.80083(19) 0.7091(3) 0.70783(15) 0.0942(17) Uani 1 1 d . . . . .
H6WA H 0.812072 0.691367 0.737089 0.141 Uiso 0.448(4) 1 d R U P A 1
H6WB H 0.759092 0.698957 0.703009 0.141 Uiso 0.448(4) 1 d R U P A 1
H6WC H 0.812322 0.688097 0.735989 0.141 Uiso 0.552(4) 1 d R U P A 2
H6WD H 0.760632 0.694467 0.700639 0.141 Uiso 0.552(4) 1 d R U P A 2
O7 O 0.29357(16) 0.51753(19) 0.70528(17) 0.0693(12) Uani 1 1 d . . . . .
O7W O 0.8873(2) 0.9974(4) 0.71581(18) 0.111(2) Uani 1 1 d . . . . .
O8 O 0.18564(11) 0.90613(13) 0.68933(9) 0.0272(5) Uani 1 1 d . . . . .
O8W O 0.8449(5) 0.8765(6) 0.6254(4) 0.098(3) Uani 0.5 1 d . U P . .
O9 O 0.06630(12) 0.60366(15) 0.70284(10) 0.0349(6) Uani 1 1 d . . . . .
O9W O 0.7332(4) 1.0114(6) 0.6799(3) 0.069(3) Uani 0.448(4) 1 d . U P A 1
O9WA O 0.7573(5) 0.9524(7) 0.6478(5) 0.126(4) Uani 0.552(4) 1 d . U P A 2
O10 O -0.05977(13) 0.68041(16) 0.46349(11) 0.0411(7) Uani 1 1 d . . . . .
O11 O 0.09469(10) 0.81553(13) 0.47992(8) 0.0216(5) Uani 1 1 d . . . . .
O12 O 0.12173(12) 0.95965(14) 0.47843(9) 0.0297(5) Uani 1 1 d . . . . .
O13 O 0.09088(14) 1.01081(15) 0.54697(10) 0.0359(6) Uani 1 1 d . . . . .
O14 O 0.03711(11) 0.89235(14) 0.40769(8) 0.0278(5) Uani 1 1 d . . . . .
O15 O -0.05824(11) 0.84046(14) 0.42139(9) 0.0265(5) Uani 1 1 d . . . . .
O35 O 0.38637(11) 0.83832(14) 0.37859(8) 0.0270(5) Uani 1 1 d . . . . .
O36 O 0.33910(15) 0.8347(2) 0.30336(10) 0.0513(8) Uani 1 1 d . . . . .
O18 O 0.39561(11) 0.70263(13) 0.42412(8) 0.0222(5) Uani 1 1 d . . . . .
O17 O 0.16601(13) 0.93276(15) 0.38496(10) 0.0357(6) Uani 1 1 d . . . . .
O19 O 0.44992(12) 0.61192(14) 0.36500(8) 0.0274(5) Uani 1 1 d . . . . .
O20 O 0.38988(12) 0.65492(15) 0.29975(9) 0.0307(6) Uani 1 1 d . . . . .
O21 O 0.39589(13) 0.55915(14) 0.45044(9) 0.0319(6) Uani 1 1 d . . . . .
O22 O 0.3131(7) 0.4921(6) 0.4196(5) 0.062(3) Uani 0.552(4) 1 d D U P A 2
O22A O 0.2987(7) 0.5067(7) 0.4373(7) 0.060(4) Uani 0.448(4) 1 d D U P A 1
O23 O 0.44664(11) 0.88549(13) 0.46738(8) 0.0250(5) Uani 1 1 d . . . . .
O24 O 0.53090(12) 0.57132(13) 0.45378(9) 0.0293(5) Uani 1 1 d . . . . .
O25 O 0.56175(11) 0.64969(13) 0.66756(9) 0.0252(5) Uani 1 1 d . . . . .
O26 O 0.66882(16) 0.6477(2) 0.68462(19) 0.0791(14) Uani 1 1 d . . . . .
O27 O 0.52735(10) 0.79669(12) 0.67050(8) 0.0199(4) Uani 1 1 d . . . . .
O28 O 0.51767(12) 0.94370(13) 0.67118(8) 0.0249(5) Uani 1 1 d . . . . .
O29 O 0.55446(14) 0.99239(14) 0.60355(9) 0.0341(6) Uani 1 1 d . . . . .
O30 O 0.59690(12) 0.86292(13) 0.74051(8) 0.0268(5) Uani 1 1 d . . . . .
O31 O 0.68959(15) 0.8170(2) 0.71728(13) 0.0645(11) Uani 1 1 d D . . . .
O32 O 0.42882(11) 0.63016(12) 0.66669(8) 0.0226(5) Uani 1 1 d . . . . .
O33 O 0.47567(13) 0.92676(13) 0.76531(9) 0.0291(5) Uani 1 1 d . . . . .
O34 O 0.04641(12) 0.67459(14) 0.48563(9) 0.0291(5) Uani 1 1 d . . . . .
N1 N 0.11164(14) 0.81109(17) 0.73927(11) 0.0267(6) Uani 1 1 d . . . . .
N2 N 0.07960(14) 0.74379(18) 0.73685(11) 0.0292(6) Uani 1 1 d . . . . .
N3 N 0.01403(16) 0.8243(2) 0.76701(12) 0.0372(8) Uani 1 1 d . . . . .
H3 H -0.021032 0.844045 0.779079 0.045 Uiso 1 1 calc R U . . .
N4 N 0.08281(17) 0.92889(19) 0.76591(13) 0.0396(8) Uani 1 1 d . . . . .
H4A H 0.120685 0.947985 0.758532 0.048 Uiso 1 1 calc R U . . .
H4B H 0.052530 0.956195 0.778565 0.048 Uiso 1 1 calc R U . . .
N5 N -0.02551(18) 0.7036(2) 0.75831(15) 0.0515(10) Uani 1 1 d . . . . .
H5A H -0.018238 0.658621 0.749178 0.062 Uiso 1 1 calc R U . . .
H5B H -0.063430 0.715285 0.770255 0.062 Uiso 1 1 calc R U . . .
N6 N 0.16426(13) 0.77120(15) 0.64494(10) 0.0220(6) Uani 1 1 d . . . . .
N7 N 0.14023(13) 0.69984(16) 0.64705(10) 0.0238(6) Uani 1 1 d . . . . .
N8 N 0.14024(13) 0.73186(16) 0.56710(10) 0.0226(6) Uani 1 1 d . . . . .
N9 N 0.18208(14) 0.85214(16) 0.57927(10) 0.0247(6) Uani 1 1 d . . . . .
H9A H 0.195201 0.886591 0.600234 0.030 Uiso 1 1 calc R U . . .
H9B H 0.180919 0.860116 0.546984 0.030 Uiso 1 1 calc R U . . .
N10 N 0.10145(16) 0.61400(18) 0.58687(12) 0.0357(7) Uani 1 1 d . . . . .
H10A H 0.093806 0.581608 0.609802 0.043 Uiso 1 1 calc R U . . .
H10B H 0.093037 0.603644 0.555177 0.043 Uiso 1 1 calc R U . . .
N11 N 0.13520(14) 0.78706(17) 0.38628(10) 0.0271(6) Uani 1 1 d . . . . .
N12 N 0.13294(14) 0.71998(17) 0.41064(10) 0.0280(6) Uani 1 1 d . . . . .
N13 N 0.13710(15) 0.7001(2) 0.33109(12) 0.0377(8) Uani 1 1 d . . . . .
H13 H 0.138623 0.677245 0.302477 0.045 Uiso 1 1 calc R U . . .
N14 N 0.13853(18) 0.8222(2) 0.30139(12) 0.0455(9) Uani 1 1 d . . . . .
H14A H 0.137515 0.868684 0.308481 0.055 Uiso 1 1 calc R U . . .
H14B H 0.140159 0.807942 0.270277 0.055 Uiso 1 1 calc R U . . .
N15 N 0.13193(18) 0.5977(2) 0.38348(14) 0.0449(9) Uani 1 1 d . . . . .
H15A H 0.129863 0.579999 0.413709 0.054 Uiso 1 1 calc R U . . .
H15B H 0.132769 0.568215 0.357826 0.054 Uiso 1 1 calc R U . . .
N16 N 0.22096(13) 0.84877(15) 0.46313(10) 0.0227(6) Uani 1 1 d . . . . .
N17 N 0.22347(13) 0.77887(15) 0.48449(10) 0.0216(6) Uani 1 1 d . . . . .
N18 N 0.32607(13) 0.81448(16) 0.47242(10) 0.0228(6) Uani 1 1 d . . . . .
N19 N 0.30191(14) 0.93322(16) 0.44048(11) 0.0286(6) Uani 1 1 d . . . . .
H19A H 0.272096 0.966779 0.433077 0.034 Uiso 1 1 calc R U . . .
H19B H 0.343947 0.942363 0.437178 0.034 Uiso 1 1 calc R U . . .
N20 N 0.30983(14) 0.70032(16) 0.51193(10) 0.0251(6) Uani 1 1 d . . . . .
H20A H 0.282052 0.669021 0.523683 0.030 Uiso 1 1 calc R U . . .
H20B H 0.352504 0.691518 0.514577 0.030 Uiso 1 1 calc R U . . .
N21 N 0.50923(13) 0.78241(15) 0.41498(10) 0.0227(6) Uani 1 1 d . . . . .
N22 N 0.53359(13) 0.71063(15) 0.41854(10) 0.0224(6) Uani 1 1 d . . . . .
N23 N 0.60813(14) 0.78019(16) 0.38718(10) 0.0257(6) Uani 1 1 d . . . . .
H23 H 0.645174 0.794697 0.375088 0.031 Uiso 1 1 calc R U . . .
N24 N 0.55265(15) 0.89344(17) 0.38667(12) 0.0316(7) Uani 1 1 d . . . . .
H24A H 0.517691 0.918813 0.393589 0.038 Uiso 1 1 calc R U . . .
H24B H 0.586228 0.914923 0.373683 0.038 Uiso 1 1 calc R U . . .
N25 N 0.63340(16) 0.65458(18) 0.39626(12) 0.0337(7) Uani 1 1 d . . . . .
H25A H 0.621290 0.611086 0.405508 0.040 Uiso 1 1 calc R U . . .
H25B H 0.672127 0.660912 0.383958 0.040 Uiso 1 1 calc R U . . .
N26 N 0.45255(13) 0.75005(14) 0.50976(9) 0.0190(5) Uani 1 1 d . . . . .
N27 N 0.46747(13) 0.67537(15) 0.50825(10) 0.0206(5) Uani 1 1 d . . . . .
N28 N 0.47192(13) 0.71068(14) 0.58768(10) 0.0203(5) Uani 1 1 d . . . . .
N29 N 0.44513(14) 0.83586(15) 0.57391(10) 0.0228(6) Uani 1 1 d . . . . .
H29A H 0.435956 0.871005 0.552473 0.027 Uiso 1 1 calc R U . . .
H29B H 0.447604 0.844981 0.606069 0.027 Uiso 1 1 calc R U . . .
N30 N 0.49319(18) 0.58637(16) 0.56967(11) 0.0354(8) Uani 1 1 d . . . . .
H30A H 0.495623 0.552006 0.547184 0.042 Uiso 1 1 calc R U . . .
H30B H 0.500190 0.576032 0.601488 0.042 Uiso 1 1 calc R U . . .
N31 N 0.48543(13) 0.77826(15) 0.76761(10) 0.0212(5) Uani 1 1 d . . . . .
N32 N 0.48280(13) 0.70944(15) 0.74465(10) 0.0210(5) Uani 1 1 d . . . . .
N33 N 0.46482(14) 0.69634(16) 0.82359(10) 0.0233(6) Uani 1 1 d . . . . .
H33 H 0.456429 0.676180 0.852146 0.028 Uiso 1 1 calc R U . . .
N34 N 0.47227(16) 0.81867(17) 0.85022(11) 0.0320(7) Uani 1 1 d . . . . .
H34A H 0.479062 0.864446 0.842935 0.038 Uiso 1 1 calc R U . . .
H34B H 0.464262 0.806226 0.880827 0.038 Uiso 1 1 calc R U . . .
N35 N 0.46625(15) 0.58983(16) 0.77444(11) 0.0279(6) Uani 1 1 d . . . . .
H35A H 0.471136 0.569573 0.745297 0.033 Uiso 1 1 calc R U . . .
H35B H 0.458205 0.562758 0.800283 0.033 Uiso 1 1 calc R U . . .
N36 N 0.39657(13) 0.77564(14) 0.66984(9) 0.0180(5) Uani 1 1 d . . . . .
N37 N 0.40630(13) 0.84490(14) 0.69117(9) 0.0197(5) Uani 1 1 d . . . . .
N38 N 0.29827(13) 0.82193(15) 0.68414(9) 0.0198(5) Uani 1 1 d . . . . .
N39 N 0.30283(13) 0.70666(15) 0.64355(10) 0.0219(6) Uani 1 1 d . . . . .
H39A H 0.327189 0.672761 0.630836 0.026 Uiso 1 1 calc R U . . .
H39B H 0.259581 0.702434 0.641822 0.026 Uiso 1 1 calc R U . . .
N40 N 0.33435(15) 0.93646(16) 0.71735(11) 0.0275(6) Uani 1 1 d . . . . .
H40A H 0.367304 0.966307 0.724821 0.033 Uiso 1 1 calc R U . . .
H40B H 0.293573 0.949976 0.721772 0.033 Uiso 1 1 calc R U . . .
C1 C 0.33176(15) 0.76502(17) 0.66564(11) 0.0188(6) Uani 1 1 d . . . . .
C2 C 0.47105(15) 0.66180(19) 0.77945(12) 0.0223(7) Uani 1 1 d . . . . .
C3 C 0.47863(16) 0.65545(17) 0.55523(12) 0.0210(6) Uani 1 1 d . . . . .
C4 C 0.12607(16) 0.67951(19) 0.60029(12) 0.0245(7) Uani 1 1 d . . . . .
C5 C 0.34641(16) 0.86965(17) 0.69900(11) 0.0203(6) Uani 1 1 d . . . . .
C6 C 0.47410(15) 0.76824(19) 0.81493(12) 0.0216(6) Uani 1 1 d . . . . .
C7 C 0.45536(15) 0.76834(18) 0.55754(11) 0.0197(6) Uani 1 1 d . . . . .
C8 C 0.25336(16) 0.68727(19) 0.77138(12) 0.0238(7) Uani 1 1 d . . . . .
C9 C 0.35472(17) 0.6798(2) 0.38276(12) 0.0255(7) Uani 1 1 d . . . . .
C10 C 0.28298(16) 0.86706(18) 0.45708(12) 0.0225(7) Uani 1 1 d . . . . .
C11 C -0.00169(16) 0.85881(19) 0.43551(12) 0.0243(7) Uani 1 1 d . . . . .
C12 C 0.26595(16) 0.8111(2) 0.81155(12) 0.0258(7) Uani 1 1 d . . . . .
C13 C 0.20541(16) 0.65740(19) 0.80876(12) 0.0234(7) Uani 1 1 d . . . . .
C14 C 0.28707(15) 0.76162(18) 0.48993(11) 0.0208(6) Uani 1 1 d . . . . .
C15 C 0.31135(17) 0.7405(2) 0.35960(13) 0.0307(8) Uani 1 1 d . . . . .
H15C H 0.287337 0.721515 0.329184 0.037 Uiso 1 1 calc R U . . .
H15D H 0.278048 0.753801 0.383342 0.037 Uiso 1 1 calc R U . . .
C16 C 0.55474(16) 0.82219(19) 0.39590(12) 0.0248(7) Uani 1 1 d . . . . .
C17 C 0.16393(15) 0.78770(18) 0.59646(12) 0.0206(6) Uani 1 1 d . . . . .
C18 C 0.30059(16) 0.7432(2) 0.79629(12) 0.0274(7) Uani 1 1 d . . . . .
H18A H 0.323543 0.721134 0.826110 0.033 Uiso 1 1 calc R U . . .
H18B H 0.334405 0.756294 0.772909 0.033 Uiso 1 1 calc R U . . .
C19 C 0.55314(17) 0.94171(19) 0.63325(12) 0.0261(7) Uani 1 1 d . . . . .
C20 C 0.26085(18) 0.5687(2) 0.71871(14) 0.0312(8) Uani 1 1 d . . . . .
C21 C 0.08526(17) 0.9617(2) 0.51597(13) 0.0280(7) Uani 1 1 d . . . . .
C22 C 0.59283(17) 0.7112(2) 0.40090(12) 0.0253(7) Uani 1 1 d . . . . .
C23 C 0.29464(17) 0.6225(2) 0.75388(13) 0.0270(7) Uani 1 1 d . . . . .
H23A H 0.333151 0.642323 0.737628 0.032 Uiso 1 1 calc R U . . .
H23B H 0.311885 0.595786 0.783850 0.032 Uiso 1 1 calc R U . . .
C24 C 0.63124(17) 0.8310(2) 0.70858(14) 0.0303(8) Uani 1 1 d . . . . .
C25 C 0.59340(16) 0.81123(19) 0.65920(12) 0.0230(7) Uani 1 1 d . . . . .
C26 C -0.00951(17) 0.7076(2) 0.48484(13) 0.0287(7) Uani 1 1 d . . . . .
C27 C 0.40050(16) 0.6477(2) 0.34508(12) 0.0257(7) Uani 1 1 d . . . . .
C28 C 0.34782(17) 0.8085(2) 0.34597(13) 0.0303(8) Uani 1 1 d . . . . .
C29 C 0.02970(16) 0.83885(19) 0.48790(12) 0.0237(7) Uani 1 1 d . . . . .
C30 C 0.03302(17) 0.9048(2) 0.52266(12) 0.0262(7) Uani 1 1 d . . . . .
H30C H -0.010466 0.929231 0.519386 0.031 Uiso 1 1 calc R U . . .
H30D H 0.038988 0.886651 0.557263 0.031 Uiso 1 1 calc R U . . .
C31 C 0.07138(18) 0.8591(2) 0.75796(13) 0.0328(8) Uani 1 1 d . . . . .
C32 C -0.01108(16) 0.7792(2) 0.51157(13) 0.0275(7) Uani 1 1 d . . . . .
H32A H 0.005904 0.772170 0.546542 0.033 Uiso 1 1 calc R U . . .
H32B H -0.057466 0.795608 0.511977 0.033 Uiso 1 1 calc R U . . .
C33 C 0.62011(18) 0.6763(2) 0.66422(15) 0.0340(8) Uani 1 1 d . . . . .
C34 C 0.59574(17) 0.87589(19) 0.62390(13) 0.0273(7) Uani 1 1 d . . . . .
H34C H 0.642139 0.892445 0.624199 0.033 Uiso 1 1 calc R U . . .
H34D H 0.583424 0.858244 0.589824 0.033 Uiso 1 1 calc R U . . .
C35 C 0.13381(18) 0.6692(2) 0.37655(14) 0.0339(8) Uani 1 1 d . . . . .
C36 C 0.13760(17) 0.7728(2) 0.33812(13) 0.0332(9) Uani 1 1 d . . . . .
C37 C 0.62539(17) 0.7460(2) 0.63477(14) 0.0291(8) Uani 1 1 d . . . . .
H37A H 0.604010 0.738876 0.601031 0.035 Uiso 1 1 calc R U . . .
H37B H 0.672584 0.756811 0.631038 0.035 Uiso 1 1 calc R U . . .
C38 C 0.02081(18) 0.7537(2) 0.75405(14) 0.0352(9) Uani 1 1 d . . . . .
C39 C 0.30880(17) 0.6174(2) 0.39811(13) 0.0313(8) Uani 1 1 d . . . . .
H39C H 0.274992 0.638648 0.418719 0.038 Uiso 1 1 calc R U . . .
H39D H 0.285429 0.598386 0.367442 0.038 Uiso 1 1 calc R U . . .
C40 C 0.3395(2) 0.5545(2) 0.42612(16) 0.0426(10) Uani 1 1 d D . . . .
O10W O 0.10762(18) 1.02294(19) 0.64876(11) 0.0553(9) Uani 1 1 d . U . . .
H10C H 0.131660 0.988926 0.663211 0.083 Uiso 1 1 d R U . . .
H10D H 0.075900 0.999837 0.632231 0.083 Uiso 1 1 d 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
V2 O1 2.005(2) . ?
V2 O3 2.092(2) . ?
V2 O8 1.613(2) . ?
V2 N1 2.076(3) . ?
V2 N6 2.079(3) . ?
V2 N38 2.101(3) . ?
V1 O3 2.100(2) . ?
V1 O4 2.016(2) . ?
V1 O6 2.023(3) . ?
V1 O9 1.614(3) . ?
V1 N2 2.095(3) . ?
V1 N7 2.081(3) . ?
V4 O16 1.619(3) . ?
V4 O11 2.048(2) . ?
V4 O34 2.024(2) . ?
V4 N8 2.121(3) . ?
V4 N12 2.104(3) . ?
V4 N17 2.081(3) . ?
V3 O11 2.093(2) . ?
V3 O12 1.996(3) . ?
V3 O14 2.001(2) . ?
V3 O17 1.620(3) . ?
V3 N11 2.093(3) . ?
V3 N16 2.071(3) . ?
V6 O35 2.006(2) . ?
V6 O18 2.085(2) . ?
V6 O23 1.615(2) . ?
V6 N18 2.103(3) . ?
V6 N21 2.075(3) . ?
V6 N26 2.065(3) . ?
V5 O18 2.096(2) . ?
V5 O19 2.037(2) . ?
V5 O21 2.015(2) . ?
V5 O24 1.617(3) . ?
V5 N22 2.094(3) . ?
V5 N27 2.065(3) . ?
V8 O25 2.021(2) . ?
V8 O27 2.049(2) . ?
V8 O32 1.619(2) . ?
V8 N28 2.113(3) . ?
V8 N32 2.114(3) . ?
V8 N36 2.088(3) . ?
V7 O27 2.088(2) . ?
V7 O28 2.009(2) . ?
V7 O30 2.020(2) . ?
V7 O33 1.615(2) . ?
V7 N31 2.101(3) . ?
V7 N37 2.076(3) . ?
K1 O1W 2.771(3) . ?
K1 O2W 2.981(9) . ?
K1 O3W 2.589(13) . ?
K1 O4W 2.822(3) . ?
K1 O5 2.714(2) . ?
K1 O13 2.777(3) 2_546 ?
K1 O15 2.877(2) 4_676 ?
K1 O10W 3.132(4) 2_546 ?
K2 O5W 2.20(2) . ?
K2 O6W 3.389(7) . ?
K2 O7W 2.634(6) . ?
K2 O8W 2.852(12) . ?
K2 O9WA 2.456(10) . ?
K2 O20 2.765(4) 4_676 ?
K2 O31 2.655(5) . ?
K2A O5W 3.007(19) . ?
K2A O6W 2.547(8) . ?
K2A H6WA 2.9524 . ?
K2A H6WB 2.9531 . ?
K2A O7W 3.143(8) . ?
K2A O8W 2.437(11) . ?
K2A O20 2.770(4) 4_676 ?
K2A O31 2.647(5) . ?
O1 C12 1.277(4) . ?
O1W H1WA 0.8737 . ?
O1W H1WB 0.8704 . ?
O2 C12 1.248(4) . ?
O2W H2WA 0.8855 . ?
O2W H2WB 0.8858 . ?
O3 C8 1.408(4) . ?
O4 C13 1.274(4) . ?
O5 C13 1.241(4) . ?
O6 C20 1.282(5) . ?
O6W H6WA 0.8698 . ?
O6W H6WB 0.8697 . ?
O6W H6WC 0.8699 . ?
O6W H6WD 0.8700 . ?
O7 C20 1.222(5) . ?
O10 C26 1.245(4) . ?
O11 C29 1.417(4) . ?
O12 C21 1.290(4) . ?
O13 C21 1.232(4) . ?
O14 C11 1.280(4) . ?
O15 C11 1.234(4) . ?
O35 C28 1.265(5) . ?
O36 C28 1.247(4) . ?
O18 C9 1.410(4) . ?
O19 C27 1.289(4) . ?
O20 C27 1.233(4) . ?
O21 C40 1.285(5) . ?
O22 C40 1.276(10) . ?
O22A C40 1.259(11) . ?
O25 C33 1.291(5) . ?
O26 C33 1.220(5) . ?
O27 C25 1.420(4) . ?
O28 C19 1.286(4) . ?
O29 C19 1.232(4) . ?
O30 C24 1.283(5) . ?
O31 C24 1.221(5) . ?
O34 C26 1.288(4) . ?
N1 N2 1.402(5) . ?
N1 C31 1.326(5) . ?
N2 C38 1.320(5) . ?
N3 H3 0.8800 . ?
N3 C31 1.365(5) . ?
N3 C38 1.357(6) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
N4 C31 1.324(6) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N5 C38 1.330(6) . ?
N6 N7 1.407(4) . ?
N6 C17 1.339(4) . ?
N7 C4 1.327(4) . ?
N8 C4 1.359(4) . ?
N8 C17 1.367(4) . ?
N9 H9A 0.8800 . ?
N9 H9B 0.8800 . ?
N9 C17 1.336(4) . ?
N10 H10A 0.8800 . ?
N10 H10B 0.8800 . ?
N10 C4 1.349(5) . ?
N11 N12 1.403(4) . ?
N11 C36 1.326(5) . ?
N12 C35 1.312(5) . ?
N13 H13 0.8800 . ?
N13 C35 1.354(5) . ?
N13 C36 1.355(6) . ?
N14 H14A 0.8800 . ?
N14 H14B 0.8800 . ?
N14 C36 1.345(6) . ?
N15 H15A 0.8800 . ?
N15 H15B 0.8800 . ?
N15 C35 1.334(6) . ?
N16 N17 1.412(4) . ?
N16 C10 1.324(4) . ?
N17 C14 1.329(4) . ?
N18 C10 1.353(4) . ?
N18 C14 1.360(4) . ?
N19 H19A 0.8800 . ?
N19 H19B 0.8800 . ?
N19 C10 1.364(5) . ?
N20 H20A 0.8800 . ?
N20 H20B 0.8800 . ?
N20 C14 1.345(4) . ?
N21 N22 1.415(4) . ?
N21 C16 1.310(4) . ?
N22 C22 1.321(4) . ?
N23 H23 0.8800 . ?
N23 C16 1.365(5) . ?
N23 C22 1.366(5) . ?
N24 H24A 0.8800 . ?
N24 H24B 0.8800 . ?
N24 C16 1.338(5) . ?
N25 H25A 0.8800 . ?
N25 H25B 0.8800 . ?
N25 C22 1.342(5) . ?
N26 N27 1.412(4) . ?
N26 C7 1.327(4) . ?
N27 C3 1.322(4) . ?
N28 C3 1.354(4) . ?
N28 C7 1.367(4) . ?
N29 H29A 0.8800 . ?
N29 H29B 0.8800 . ?
N29 C7 1.342(4) . ?
N30 H30A 0.8800 . ?
N30 H30B 0.8800 . ?
N30 C3 1.360(4) . ?
N31 N32 1.412(4) . ?
N31 C6 1.321(4) . ?
N32 C2 1.317(4) . ?
N33 H33 0.8800 . ?
N33 C2 1.361(4) . ?
N33 C6 1.362(4) . ?
N34 H34A 0.8800 . ?
N34 H34B 0.8800 . ?
N34 C6 1.332(5) . ?
N35 H35A 0.8800 . ?
N35 H35B 0.8800 . ?
N35 C2 1.338(5) . ?
N36 N37 1.410(4) . ?
N36 C1 1.328(4) . ?
N37 C5 1.328(4) . ?
N38 C1 1.362(4) . ?
N38 C5 1.357(4) . ?
N39 H39A 0.8800 . ?
N39 H39B 0.8800 . ?
N39 C1 1.347(4) . ?
N40 H40A 0.8800 . ?
N40 H40B 0.8800 . ?
N40 C5 1.356(4) . ?
C8 C13 1.545(5) . ?
C8 C18 1.534(5) . ?
C8 C23 1.550(5) . ?
C9 C15 1.534(5) . ?
C9 C27 1.537(5) . ?
C9 C39 1.553(5) . ?
C11 C29 1.554(5) . ?
C12 C18 1.506(5) . ?
C15 H15C 0.9900 . ?
C15 H15D 0.9900 . ?
C15 C28 1.513(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C34 1.521(5) . ?
C20 C23 1.507(5) . ?
C21 C30 1.511(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.536(5) . ?
C25 C34 1.528(5) . ?
C25 C37 1.535(5) . ?
C26 C32 1.505(5) . ?
C29 C30 1.534(5) . ?
C29 C32 1.540(5) . ?
C30 H30C 0.9900 . ?
C30 H30D 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C37 1.519(5) . ?
C34 H34C 0.9900 . ?
C34 H34D 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C39 H39C 0.9900 . ?
C39 H39D 0.9900 . ?
C39 C40 1.499(6) . ?
O10W H10C 0.8714 . ?
O10W H10D 0.8707 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V2 O3 85.63(10) . . ?
O1 V2 N1 86.49(11) . . ?
O1 V2 N6 164.91(11) . . ?
O1 V2 N38 90.15(10) . . ?
O3 V2 N38 87.81(10) . . ?
O8 V2 O1 97.59(12) . . ?
O8 V2 O3 175.12(11) . . ?
O8 V2 N1 94.15(12) . . ?
O8 V2 N6 97.07(12) . . ?
O8 V2 N38 95.83(11) . . ?
N1 V2 O3 82.34(10) . . ?
N1 V2 N6 88.91(11) . . ?
N1 V2 N38 169.81(11) . . ?
N6 V2 O3 79.52(10) . . ?
N6 V2 N38 91.89(10) . . ?
O4 V1 O3 78.88(9) . . ?
O4 V1 O6 88.15(10) . . ?
O4 V1 N2 86.76(11) . . ?
O4 V1 N7 157.65(11) . . ?
O6 V1 O3 82.64(10) . . ?
O6 V1 N2 166.45(12) . . ?
O6 V1 N7 92.16(11) . . ?
O9 V1 O3 177.41(12) . . ?
O9 V1 O4 103.43(12) . . ?
O9 V1 O6 98.55(13) . . ?
O9 V1 N2 94.85(13) . . ?
O9 V1 N7 98.62(12) . . ?
N2 V1 O3 84.05(11) . . ?
N7 V1 O3 79.00(10) . . ?
N7 V1 N2 87.82(11) . . ?
O16 V4 O11 175.00(11) . . ?
O16 V4 O34 95.27(12) . . ?
O16 V4 N8 96.10(12) . . ?
O16 V4 N12 93.64(13) . . ?
O16 V4 N17 96.40(12) . . ?
O11 V4 N8 88.51(10) . . ?
O11 V4 N12 81.68(11) . . ?
O11 V4 N17 81.53(10) . . ?
O34 V4 O11 86.40(10) . . ?
O34 V4 N8 92.84(10) . . ?
O34 V4 N12 88.57(11) . . ?
O34 V4 N17 167.14(11) . . ?
N12 V4 N8 169.99(12) . . ?
N17 V4 N8 91.26(10) . . ?
N17 V4 N12 85.33(11) . . ?
O11 V3 N11 82.15(10) . . ?
O12 V3 O11 83.22(10) . . ?
O12 V3 O14 87.95(10) . . ?
O12 V3 N11 165.37(11) . . ?
O12 V3 N16 91.70(11) . . ?
O14 V3 O11 79.56(9) . . ?
O14 V3 N11 88.88(11) . . ?
O14 V3 N16 160.38(11) . . ?
O17 V3 O11 176.92(12) . . ?
O17 V3 O12 99.40(13) . . ?
O17 V3 O14 102.07(12) . . ?
O17 V3 N11 95.23(13) . . ?
O17 V3 N16 97.35(12) . . ?
N16 V3 O11 80.91(10) . . ?
N16 V3 N11 86.54(11) . . ?
O35 V6 O18 85.92(10) . . ?
O35 V6 N18 90.08(10) . . ?
O35 V6 N21 87.28(10) . . ?
O35 V6 N26 165.59(11) . . ?
O18 V6 N18 86.11(10) . . ?
O23 V6 O35 98.52(11) . . ?
O23 V6 O18 174.95(11) . . ?
O23 V6 N18 96.26(12) . . ?
O23 V6 N21 94.59(12) . . ?
O23 V6 N26 95.79(11) . . ?
N21 V6 O18 83.16(10) . . ?
N21 V6 N18 169.10(12) . . ?
N26 V6 O18 79.71(10) . . ?
N26 V6 N18 90.03(10) . . ?
N26 V6 N21 89.92(10) . . ?
O19 V5 O18 78.02(9) . . ?
O19 V5 N22 86.20(10) . . ?
O19 V5 N27 157.36(11) . . ?
O21 V5 O18 83.60(10) . . ?
O21 V5 O19 86.84(10) . . ?
O21 V5 N22 167.29(11) . . ?
O21 V5 N27 93.60(10) . . ?
O24 V5 O18 176.73(11) . . ?
O24 V5 O19 105.03(11) . . ?
O24 V5 O21 97.67(12) . . ?
O24 V5 N22 94.40(12) . . ?
O24 V5 N27 97.35(12) . . ?
N22 V5 O18 84.56(10) . . ?
N27 V5 O18 79.54(10) . . ?
N27 V5 N22 88.77(11) . . ?
O25 V8 O27 87.07(9) . . ?
O25 V8 N28 91.13(10) . . ?
O25 V8 N32 89.70(10) . . ?
O25 V8 N36 167.48(11) . . ?
O27 V8 N28 88.47(10) . . ?
O27 V8 N32 83.04(10) . . ?
O27 V8 N36 80.83(10) . . ?
O32 V8 O25 96.16(11) . . ?
O32 V8 O27 174.89(10) . . ?
O32 V8 N28 95.40(11) . . ?
O32 V8 N32 93.00(11) . . ?
O32 V8 N36 95.69(11) . . ?
N28 V8 N32 171.42(11) . . ?
N36 V8 N28 91.76(10) . . ?
N36 V8 N32 85.66(10) . . ?
O27 V7 N31 84.63(10) . . ?
O28 V7 O27 83.18(9) . . ?
O28 V7 O30 88.55(10) . . ?
O28 V7 N31 167.81(10) . . ?
O28 V7 N37 93.67(10) . . ?
O30 V7 O27 78.10(9) . . ?
O30 V7 N31 88.74(10) . . ?
O30 V7 N37 158.57(11) . . ?
O33 V7 O27 178.92(11) . . ?
O33 V7 O28 97.70(11) . . ?
O33 V7 O30 102.51(12) . . ?
O33 V7 N31 94.49(12) . . ?
O33 V7 N37 98.31(12) . . ?
N37 V7 O27 81.00(9) . . ?
N37 V7 N31 84.61(11) . . ?
O1W K1 O2W 91.72(16) . . ?
O1W K1 O4W 149.54(9) . . ?
O1W K1 O13 125.22(8) . 2_546 ?
O1W K1 O15 69.38(8) . 4_676 ?
O1W K1 O10W 124.62(8) . 2_546 ?
O2W K1 O10W 128.19(13) . 2_546 ?
O3W K1 O1W 80.4(4) . . ?
O3W K1 O2W 48.8(5) . . ?
O3W K1 O4W 84.3(4) . . ?
O3W K1 O5 83.2(4) . . ?
O3W K1 O13 119.7(4) . 2_546 ?
O3W K1 O15 138.2(4) . 4_676 ?
O3W K1 O10W 153.9(4) . 2_546 ?
O4W K1 O2W 97.71(18) . . ?
O4W K1 O15 135.10(8) . 4_676 ?
O4W K1 O10W 70.12(8) . 2_546 ?
O5 K1 O1W 77.39(8) . . ?
O5 K1 O2W 131.95(14) . . ?
O5 K1 O4W 74.78(8) . . ?
O5 K1 O13 148.23(9) . 2_546 ?
O5 K1 O15 115.89(8) . 4_676 ?
O5 K1 O10W 94.46(9) . 2_546 ?
O13 K1 O2W 74.33(13) 2_546 . ?
O13 K1 O4W 85.24(8) 2_546 . ?
O13 K1 O15 63.14(8) 2_546 4_676 ?
O13 K1 O10W 55.04(9) 2_546 2_546 ?
O15 K1 O2W 102.81(17) 4_676 . ?
O15 K1 O10W 65.75(8) 4_676 2_546 ?
O5W K2 O6W 114.0(7) . . ?
O5W K2 O7W 104.4(7) . . ?
O5W K2 O8W 154.9(7) . . ?
O5W K2 O9WA 102.6(7) . . ?
O5W K2 O20 89.0(6) . 4_676 ?
O5W K2 O31 69.8(6) . . ?
O7W K2 O6W 136.5(2) . . ?
O7W K2 O8W 75.7(2) . . ?
O7W K2 O20 83.72(15) . 4_676 ?
O7W K2 O31 161.0(2) . . ?
O8W K2 O6W 77.7(2) . . ?
O9WA K2 O6W 110.6(4) . . ?
O9WA K2 O7W 78.5(3) . . ?
O9WA K2 O8W 52.4(4) . . ?
O9WA K2 O20 160.7(3) . 4_676 ?
O9WA K2 O31 85.1(3) . . ?
O20 K2 O6W 77.61(13) 4_676 . ?
O20 K2 O8W 115.7(3) 4_676 . ?
O31 K2 O6W 58.76(13) . . ?
O31 K2 O8W 101.6(2) . . ?
O31 K2 O20 113.65(14) . 4_676 ?
O5W K2A H6WA 108.2 . . ?
O5W K2A H6WB 106.4 . . ?
O5W K2A O7W 77.0(5) . . ?
O6W K2A O5W 116.7(5) . . ?
O6W K2A H6WA 16.1 . . ?
O6W K2A H6WB 16.1 . . ?
O6W K2A O7W 159.7(2) . . ?
O6W K2A O20 93.89(17) . 4_676 ?
O6W K2A O31 71.44(16) . . ?
H6WA K2A H6WB 26.9 . . ?
O7W K2A H6WA 150.0 . . ?
O7W K2A H6WB 175.8 . . ?
O8W K2A O5W 129.7(6) . . ?
O8W K2A O6W 104.4(4) . . ?
O8W K2A H6WA 117.9 . . ?
O8W K2A H6WB 105.8 . . ?
O8W K2A O7W 73.1(3) . . ?
O8W K2A O20 131.9(3) . 4_676 ?
O8W K2A O31 114.2(3) . . ?
O20 K2A O5W 74.6(5) 4_676 . ?
O20 K2A H6WA 78.2 4_676 . ?
O20 K2A H6WB 103.5 4_676 . ?
O20 K2A O7W 74.82(15) 4_676 . ?
O31 K2A O5W 59.1(5) . . ?
O31 K2A H6WA 75.0 . . ?
O31 K2A H6WB 55.9 . . ?
O31 K2A O7W 128.4(3) . . ?
O31 K2A O20 113.75(18) . 4_676 ?
C12 O1 V2 130.7(2) . . ?
K1 O1W H1WA 109.4 . . ?
K1 O1W H1WB 109.5 . . ?
H1WA O1W H1WB 104.4 . . ?
K1 O2W H2WA 110.2 . . ?
K1 O2W H2WB 109.6 . . ?
H2WA O2W H2WB 104.0 . . ?
V2 O3 V1 113.99(10) . . ?
C8 O3 V2 130.5(2) . . ?
C8 O3 V1 108.73(19) . . ?
C13 O4 V1 116.6(2) . . ?
C13 O5 K1 143.5(2) . . ?
C20 O6 V1 132.2(2) . . ?
K2 O6W H6WC 109.5 . . ?
K2 O6W H6WD 109.5 . . ?
K2A O6W H6WA 109.4 . . ?
K2A O6W H6WB 109.5 . . ?
H6WA O6W H6WB 104.5 . . ?
H6WC O6W H6WD 104.5 . . ?
V4 O11 V3 115.93(10) . . ?
C29 O11 V4 131.2(2) . . ?
C29 O11 V3 108.42(19) . . ?
C21 O12 V3 131.6(2) . . ?
C21 O13 K1 133.4(3) . 2_556 ?
C11 O14 V3 116.0(2) . . ?
C11 O15 K1 139.0(2) . 4_575 ?
C28 O35 V6 132.7(2) . . ?
V6 O18 V5 113.13(10) . . ?
C9 O18 V6 129.2(2) . . ?
C9 O18 V5 110.0(2) . . ?
C27 O19 V5 116.7(2) . . ?
C27 O20 K2 139.7(2) . 4_575 ?
C27 O20 K2A 156.6(2) . 4_575 ?
C40 O21 V5 128.8(3) . . ?
C33 O25 V8 128.7(2) . . ?
V8 O27 V7 115.36(10) . . ?
C25 O27 V8 130.4(2) . . ?
C25 O27 V7 109.33(19) . . ?
C19 O28 V7 132.9(2) . . ?
C24 O30 V7 117.0(2) . . ?
C24 O31 K2 136.1(4) . . ?
C24 O31 K2A 151.3(4) . . ?
C26 O34 V4 129.4(2) . . ?
N2 N1 V2 120.6(2) . . ?
C31 N1 V2 130.6(3) . . ?
C31 N1 N2 108.3(3) . . ?
N1 N2 V1 119.5(2) . . ?
C38 N2 V1 133.4(3) . . ?
C38 N2 N1 106.7(3) . . ?
C31 N3 H3 126.2 . . ?
C38 N3 H3 126.2 . . ?
C38 N3 C31 107.7(3) . . ?
H4A N4 H4B 120.0 . . ?
C31 N4 H4A 120.0 . . ?
C31 N4 H4B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C38 N5 H5A 120.0 . . ?
C38 N5 H5B 120.0 . . ?
N7 N6 V2 121.6(2) . . ?
C17 N6 V2 132.2(2) . . ?
C17 N6 N7 105.8(3) . . ?
N6 N7 V1 119.1(2) . . ?
C4 N7 V1 134.5(2) . . ?
C4 N7 N6 106.3(3) . . ?
C4 N8 V4 124.4(2) . . ?
C4 N8 C17 103.7(3) . . ?
C17 N8 V4 131.1(2) . . ?
H9A N9 H9B 120.0 . . ?
C17 N9 H9A 120.0 . . ?
C17 N9 H9B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
C4 N10 H10A 120.0 . . ?
C4 N10 H10B 120.0 . . ?
N12 N11 V3 120.4(2) . . ?
C36 N11 V3 133.1(3) . . ?
C36 N11 N12 106.6(3) . . ?
N11 N12 V4 119.7(2) . . ?
C35 N12 V4 132.4(3) . . ?
C35 N12 N11 107.5(3) . . ?
C35 N13 H13 126.6 . . ?
C35 N13 C36 106.9(3) . . ?
C36 N13 H13 126.6 . . ?
H14A N14 H14B 120.0 . . ?
C36 N14 H14A 120.0 . . ?
C36 N14 H14B 120.0 . . ?
H15A N15 H15B 120.0 . . ?
C35 N15 H15A 120.0 . . ?
C35 N15 H15B 120.0 . . ?
N17 N16 V3 118.9(2) . . ?
C10 N16 V3 131.0(2) . . ?
C10 N16 N17 105.8(3) . . ?
N16 N17 V4 121.5(2) . . ?
C14 N17 V4 131.4(2) . . ?
C14 N17 N16 105.9(3) . . ?
C10 N18 V6 122.4(2) . . ?
C10 N18 C14 103.9(3) . . ?
C14 N18 V6 129.7(2) . . ?
H19A N19 H19B 120.0 . . ?
C10 N19 H19A 120.0 . . ?
C10 N19 H19B 120.0 . . ?
H20A N20 H20B 120.0 . . ?
C14 N20 H20A 120.0 . . ?
C14 N20 H20B 120.0 . . ?
N22 N21 V6 119.09(19) . . ?
C16 N21 V6 132.9(2) . . ?
C16 N21 N22 107.4(3) . . ?
N21 N22 V5 119.56(19) . . ?
C22 N22 V5 133.0(2) . . ?
C22 N22 N21 106.9(3) . . ?
C16 N23 H23 126.7 . . ?
C16 N23 C22 106.6(3) . . ?
C22 N23 H23 126.7 . . ?
H24A N24 H24B 120.0 . . ?
C16 N24 H24A 120.0 . . ?
C16 N24 H24B 120.0 . . ?
H25A N25 H25B 120.0 . . ?
C22 N25 H25A 120.0 . . ?
C22 N25 H25B 120.0 . . ?
N27 N26 V6 122.14(19) . . ?
C7 N26 V6 131.1(2) . . ?
C7 N26 N27 106.3(2) . . ?
N26 N27 V5 117.90(19) . . ?
C3 N27 V5 136.5(2) . . ?
C3 N27 N26 105.5(2) . . ?
C3 N28 V8 126.2(2) . . ?
C3 N28 C7 103.6(3) . . ?
C7 N28 V8 129.7(2) . . ?
H29A N29 H29B 120.0 . . ?
C7 N29 H29A 120.0 . . ?
C7 N29 H29B 120.0 . . ?
H30A N30 H30B 120.0 . . ?
C3 N30 H30A 120.0 . . ?
C3 N30 H30B 120.0 . . ?
N32 N31 V7 119.14(19) . . ?
C6 N31 V7 133.7(2) . . ?
C6 N31 N32 107.0(3) . . ?
N31 N32 V8 119.54(19) . . ?
C2 N32 V8 131.4(2) . . ?
C2 N32 N31 107.0(3) . . ?
C2 N33 H33 126.7 . . ?
C2 N33 C6 106.6(3) . . ?
C6 N33 H33 126.7 . . ?
H34A N34 H34B 120.0 . . ?
C6 N34 H34A 120.0 . . ?
C6 N34 H34B 120.0 . . ?
H35A N35 H35B 120.0 . . ?
C2 N35 H35A 120.0 . . ?
C2 N35 H35B 120.0 . . ?
N37 N36 V8 121.43(19) . . ?
C1 N36 V8 130.4(2) . . ?
C1 N36 N37 106.3(2) . . ?
N36 N37 V7 118.62(19) . . ?
C5 N37 V7 131.8(2) . . ?
C5 N37 N36 105.7(3) . . ?
C1 N38 V2 129.0(2) . . ?
C5 N38 V2 123.9(2) . . ?
C5 N38 C1 103.9(3) . . ?
H39A N39 H39B 120.0 . . ?
C1 N39 H39A 120.0 . . ?
C1 N39 H39B 120.0 . . ?
H40A N40 H40B 120.0 . . ?
C5 N40 H40A 120.0 . . ?
C5 N40 H40B 120.0 . . ?
N36 C1 N38 111.7(3) . . ?
N36 C1 N39 123.9(3) . . ?
N39 C1 N38 124.3(3) . . ?
N32 C2 N33 109.8(3) . . ?
N32 C2 N35 127.3(3) . . ?
N35 C2 N33 122.9(3) . . ?
N27 C3 N28 112.9(3) . . ?
N27 C3 N30 123.7(3) . . ?
N28 C3 N30 123.4(3) . . ?
N7 C4 N8 112.3(3) . . ?
N7 C4 N10 124.2(3) . . ?
N10 C4 N8 123.5(3) . . ?
N37 C5 N38 112.3(3) . . ?
N37 C5 N40 124.0(3) . . ?
N40 C5 N38 123.6(3) . . ?
N31 C6 N33 109.6(3) . . ?
N31 C6 N34 127.1(3) . . ?
N34 C6 N33 123.2(3) . . ?
N26 C7 N28 111.8(3) . . ?
N26 C7 N29 123.8(3) . . ?
N29 C7 N28 124.4(3) . . ?
O3 C8 C13 107.6(3) . . ?
O3 C8 C18 111.9(3) . . ?
O3 C8 C23 110.5(3) . . ?
C13 C8 C23 107.3(3) . . ?
C18 C8 C13 111.0(3) . . ?
C18 C8 C23 108.5(3) . . ?
O18 C9 C15 113.3(3) . . ?
O18 C9 C27 106.6(3) . . ?
O18 C9 C39 110.2(3) . . ?
C15 C9 C27 111.7(3) . . ?
C15 C9 C39 108.1(3) . . ?
C27 C9 C39 106.7(3) . . ?
N16 C10 N18 112.4(3) . . ?
N16 C10 N19 124.0(3) . . ?
N18 C10 N19 123.5(3) . . ?
O14 C11 C29 114.4(3) . . ?
O15 C11 O14 123.2(3) . . ?
O15 C11 C29 122.3(3) . . ?
O1 C12 C18 118.1(3) . . ?
O2 C12 O1 121.3(3) . . ?
O2 C12 C18 120.6(3) . . ?
O4 C13 C8 115.5(3) . . ?
O5 C13 O4 123.6(3) . . ?
O5 C13 C8 120.9(3) . . ?
N17 C14 N18 111.9(3) . . ?
N17 C14 N20 123.7(3) . . ?
N20 C14 N18 124.4(3) . . ?
C9 C15 H15C 108.5 . . ?
C9 C15 H15D 108.5 . . ?
H15C C15 H15D 107.5 . . ?
C28 C15 C9 115.3(3) . . ?
C28 C15 H15C 108.5 . . ?
C28 C15 H15D 108.5 . . ?
N21 C16 N23 109.7(3) . . ?
N21 C16 N24 127.5(3) . . ?
N24 C16 N23 122.8(3) . . ?
N6 C17 N8 111.8(3) . . ?
N9 C17 N6 123.7(3) . . ?
N9 C17 N8 124.4(3) . . ?
C8 C18 H18A 109.0 . . ?
C8 C18 H18B 109.0 . . ?
C12 C18 C8 112.9(3) . . ?
C12 C18 H18A 109.0 . . ?
C12 C18 H18B 109.0 . . ?
H18A C18 H18B 107.8 . . ?
O28 C19 C34 120.5(3) . . ?
O29 C19 O28 122.0(3) . . ?
O29 C19 C34 117.6(3) . . ?
O6 C20 C23 121.9(3) . . ?
O7 C20 O6 120.7(4) . . ?
O7 C20 C23 117.4(3) . . ?
O12 C21 C30 121.0(3) . . ?
O13 C21 O12 121.2(4) . . ?
O13 C21 C30 117.8(3) . . ?
N22 C22 N23 109.4(3) . . ?
N22 C22 N25 127.3(3) . . ?
N25 C22 N23 123.3(3) . . ?
C8 C23 H23A 107.9 . . ?
C8 C23 H23B 107.9 . . ?
C20 C23 C8 117.7(3) . . ?
C20 C23 H23A 107.9 . . ?
C20 C23 H23B 107.9 . . ?
H23A C23 H23B 107.2 . . ?
O30 C24 C25 115.2(3) . . ?
O31 C24 O30 122.1(4) . . ?
O31 C24 C25 122.8(4) . . ?
O27 C25 C24 106.7(3) . . ?
O27 C25 C34 110.3(3) . . ?
O27 C25 C37 112.0(3) . . ?
C34 C25 C24 108.6(3) . . ?
C34 C25 C37 108.4(3) . . ?
C37 C25 C24 110.8(3) . . ?
O10 C26 O34 120.8(4) . . ?
O10 C26 C32 122.2(3) . . ?
O34 C26 C32 116.9(3) . . ?
O19 C27 C9 114.2(3) . . ?
O20 C27 O19 123.4(3) . . ?
O20 C27 C9 122.4(3) . . ?
O35 C28 C15 118.9(3) . . ?
O36 C28 O35 121.0(4) . . ?
O36 C28 C15 120.1(3) . . ?
O11 C29 C11 105.5(2) . . ?
O11 C29 C30 109.1(3) . . ?
O11 C29 C32 112.1(3) . . ?
C30 C29 C11 111.4(3) . . ?
C30 C29 C32 108.6(3) . . ?
C32 C29 C11 110.1(3) . . ?
C21 C30 C29 118.9(3) . . ?
C21 C30 H30C 107.6 . . ?
C21 C30 H30D 107.6 . . ?
C29 C30 H30C 107.6 . . ?
C29 C30 H30D 107.6 . . ?
H30C C30 H30D 107.0 . . ?
N1 C31 N3 107.8(4) . . ?
N4 C31 N1 127.3(4) . . ?
N4 C31 N3 124.9(3) . . ?
C26 C32 C29 113.7(3) . . ?
C26 C32 H32A 108.8 . . ?
C26 C32 H32B 108.8 . . ?
C29 C32 H32A 108.8 . . ?
C29 C32 H32B 108.8 . . ?
H32A C32 H32B 107.7 . . ?
O25 C33 C37 117.0(3) . . ?
O26 C33 O25 121.7(4) . . ?
O26 C33 C37 121.3(4) . . ?
C19 C34 C25 118.7(3) . . ?
C19 C34 H34C 107.6 . . ?
C19 C34 H34D 107.6 . . ?
C25 C34 H34C 107.6 . . ?
C25 C34 H34D 107.6 . . ?
H34C C34 H34D 107.1 . . ?
N12 C35 N13 109.6(4) . . ?
N12 C35 N15 127.4(4) . . ?
N15 C35 N13 123.0(3) . . ?
N11 C36 N13 109.4(4) . . ?
N11 C36 N14 125.9(4) . . ?
N14 C36 N13 124.7(3) . . ?
C25 C37 H37A 108.9 . . ?
C25 C37 H37B 108.9 . . ?
C33 C37 C25 113.3(3) . . ?
C33 C37 H37A 108.9 . . ?
C33 C37 H37B 108.9 . . ?
H37A C37 H37B 107.7 . . ?
N2 C38 N3 109.4(4) . . ?
N2 C38 N5 126.4(4) . . ?
N5 C38 N3 124.2(3) . . ?
C9 C39 H39C 107.8 . . ?
C9 C39 H39D 107.8 . . ?
H39C C39 H39D 107.1 . . ?
C40 C39 C9 118.1(3) . . ?
C40 C39 H39C 107.8 . . ?
C40 C39 H39D 107.8 . . ?
O21 C40 C39 122.2(3) . . ?
O22 C40 O21 118.9(8) . . ?
O22 C40 C39 118.2(8) . . ?
O22A C40 O21 120.3(10) . . ?
O22A C40 C39 113.8(9) . . ?
K1 O10W H10C 109.5 2_556 . ?
K1 O10W H10D 109.3 2_556 . ?
H10C O10W H10D 104.5 . . ?

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
O1W H1WA O2 0.87 1.89 2.762(4) 173.8 . yes
O1W H1WB O10 0.87 1.99 2.846(4) 168.0 4_676 yes
O6W H6WA O36 0.87 1.89 2.759(5) 172.5 4_676 yes
O6W H6WD O26 0.87 2.08 2.941(6) 173.5 . yes
N3 H3 O20 0.88 1.93 2.749(4) 155.1 4_576 yes
N4 H4A O7 0.88 2.33 3.055(5) 140.2 2_556 yes
N4 H4A O8 0.88 2.47 3.054(4) 124.1 . yes
N5 H5A O9 0.88 2.41 3.075(5) 132.8 . yes
N5 H5B O36 0.88 2.41 3.154(5) 143.2 4_576 yes
N9 H9A O4W 0.88 2.26 3.012(4) 143.8 2_556 yes
N9 H9A O8 0.88 2.44 3.121(4) 134.1 . yes
N9 H9B O11 0.88 2.57 3.186(3) 127.9 . yes
N9 H9B N17 0.88 2.45 3.051(4) 125.9 . yes
N10 H10B O16 0.88 2.56 3.099(4) 120.1 . yes
N10 H10B O34 0.88 2.43 3.088(4) 132.3 . yes
N13 H13 O30 0.88 1.97 2.776(4) 152.3 4_575 yes
N14 H14A O17 0.88 2.41 3.062(5) 131.0 . yes
N15 H15A O16 0.88 2.48 3.071(4) 125.4 . yes
N19 H19B O23 0.88 2.43 3.109(4) 134.5 . yes
N20 H20A O16 0.88 2.34 2.971(4) 128.3 . yes
N20 H20B N26 0.88 2.31 3.044(4) 140.7 . yes
N23 H23 O5 0.88 1.87 2.741(4) 169.7 4_675 yes
N24 H24A O23 0.88 2.60 3.157(4) 122.0 . yes
N24 H24A O29 0.88 2.20 3.051(4) 161.9 3_676 yes
N25 H25A O24 0.88 2.43 3.082(4) 131.4 . yes
N25 H25B O2 0.88 2.09 2.971(4) 177.3 4_675 yes
N29 H29A O23 0.88 2.33 3.011(3) 134.4 . yes
N29 H29B O27 0.88 2.46 3.085(3) 128.1 . yes
N29 H29B N36 0.88 2.43 3.032(4) 126.5 . yes
N30 H30A O24 0.88 2.34 3.011(4) 133.3 3_666 yes
N30 H30B O25 0.88 2.51 3.127(4) 127.9 . yes
N30 H30B O32 0.88 2.55 3.100(4) 121.4 . yes
N33 H33 O14 0.88 2.49 3.088(4) 125.6 4_676 yes
N33 H33 O15 0.88 1.93 2.786(4) 163.8 4_676 yes
N34 H34A O33 0.88 2.38 3.037(4) 131.5 . yes
N34 H34B O10 0.88 2.32 3.157(4) 158.7 4_676 yes
N35 H35A O32 0.88 2.50 3.043(4) 120.8 . yes
N35 H35B O10W 0.88 2.11 2.905(4) 150.4 2_546 yes
N39 H39A O32 0.88 2.36 2.953(4) 125.2 . yes
N39 H39B N6 0.88 2.32 3.058(4) 141.4 . yes
N40 H40A O33 0.88 2.50 3.076(4) 123.5 . yes
N40 H40B O8 0.88 2.44 3.116(4) 133.4 . yes
O10W H10C O8 0.87 1.98 2.851(4) 174.0 . 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
V2 O1 C12 O2 -155.9(3) . . . . ?
V2 O1 C12 C18 25.2(4) . . . . ?
V2 O3 C8 C13 110.8(3) . . . . ?
V2 O3 C8 C18 -11.3(4) . . . . ?
V2 O3 C8 C23 -132.3(2) . . . . ?
V2 N1 N2 V1 13.3(3) . . . . ?
V2 N1 N2 C38 -172.9(2) . . . . ?
V2 N1 C31 N3 171.5(2) . . . . ?
V2 N1 C31 N4 -7.2(6) . . . . ?
V2 N6 N7 V1 7.6(3) . . . . ?
V2 N6 N7 C4 -174.1(2) . . . . ?
V2 N6 C17 N8 172.7(2) . . . . ?
V2 N6 C17 N9 -9.9(5) . . . . ?
V2 N38 C1 N36 -158.8(2) . . . . ?
V2 N38 C1 N39 24.2(4) . . . . ?
V2 N38 C5 N37 161.0(2) . . . . ?
V2 N38 C5 N40 -22.2(4) . . . . ?
V1 O3 C8 C13 -37.7(3) . . . . ?
V1 O3 C8 C18 -159.9(2) . . . . ?
V1 O3 C8 C23 79.1(3) . . . . ?
V1 O4 C13 O5 170.8(3) . . . . ?
V1 O4 C13 C8 -8.2(4) . . . . ?
V1 O6 C20 O7 180.0(3) . . . . ?
V1 O6 C20 C23 -0.6(5) . . . . ?
V1 N2 C38 N3 172.9(3) . . . . ?
V1 N2 C38 N5 -7.3(6) . . . . ?
V1 N7 C4 N8 179.1(2) . . . . ?
V1 N7 C4 N10 -2.0(5) . . . . ?
V4 O11 C29 C11 -114.0(3) . . . . ?
V4 O11 C29 C30 126.2(3) . . . . ?
V4 O11 C29 C32 5.9(4) . . . . ?
V4 O34 C26 O10 150.7(3) . . . . ?
V4 O34 C26 C32 -30.4(4) . . . . ?
V4 N8 C4 N7 170.3(2) . . . . ?
V4 N8 C4 N10 -8.6(5) . . . . ?
V4 N8 C17 N6 -170.4(2) . . . . ?
V4 N8 C17 N9 12.2(5) . . . . ?
V4 N12 C35 N13 -172.2(2) . . . . ?
V4 N12 C35 N15 7.7(6) . . . . ?
V4 N17 C14 N18 165.2(2) . . . . ?
V4 N17 C14 N20 -17.2(5) . . . . ?
V3 O11 C29 C11 40.6(3) . . . . ?
V3 O11 C29 C30 -79.1(3) . . . . ?
V3 O11 C29 C32 160.5(2) . . . . ?
V3 O12 C21 O13 171.4(2) . . . . ?
V3 O12 C21 C30 -10.1(5) . . . . ?
V3 O14 C11 O15 -157.4(3) . . . . ?
V3 O14 C11 C29 19.1(4) . . . . ?
V3 N11 N12 V4 -6.9(3) . . . . ?
V3 N11 N12 C35 179.3(2) . . . . ?
V3 N11 C36 N13 -179.5(2) . . . . ?
V3 N11 C36 N14 -1.3(6) . . . . ?
V3 N16 N17 V4 -8.5(3) . . . . ?
V3 N16 N17 C14 160.0(2) . . . . ?
V3 N16 C10 N18 -155.3(2) . . . . ?
V3 N16 C10 N19 28.9(5) . . . . ?
V6 O35 C28 O36 -171.3(3) . . . . ?
V6 O35 C28 C15 9.6(5) . . . . ?
V6 O18 C9 C15 -16.3(4) . . . . ?
V6 O18 C9 C27 107.0(3) . . . . ?
V6 O18 C9 C39 -137.5(2) . . . . ?
V6 N18 C10 N16 158.1(2) . . . . ?
V6 N18 C10 N19 -26.1(4) . . . . ?
V6 N18 C14 N17 -155.5(2) . . . . ?
V6 N18 C14 N20 26.9(5) . . . . ?
V6 N21 N22 V5 15.0(3) . . . . ?
V6 N21 N22 C22 -172.8(2) . . . . ?
V6 N21 C16 N23 170.3(2) . . . . ?
V6 N21 C16 N24 -8.2(6) . . . . ?
V6 N26 N27 V5 9.1(3) . . . . ?
V6 N26 N27 C3 -173.6(2) . . . . ?
V6 N26 C7 N28 172.8(2) . . . . ?
V6 N26 C7 N29 -9.1(5) . . . . ?
V5 O18 C9 C15 -163.0(2) . . . . ?
V5 O18 C9 C27 -39.8(3) . . . . ?
V5 O18 C9 C39 75.7(3) . . . . ?
V5 O19 C27 O20 165.4(3) . . . . ?
V5 O19 C27 C9 -15.6(4) . . . . ?
V5 O21 C40 O22 144.2(6) . . . . ?
V5 O21 C40 O22A 177.6(8) . . . . ?
V5 O21 C40 C39 -25.6(6) . . . . ?
V5 N22 C22 N23 172.0(2) . . . . ?
V5 N22 C22 N25 -7.8(6) . . . . ?
V5 N27 C3 N28 176.8(2) . . . . ?
V5 N27 C3 N30 -5.2(5) . . . . ?
V8 O25 C33 O26 149.8(4) . . . . ?
V8 O25 C33 C37 -28.7(5) . . . . ?
V8 O27 C25 C24 -114.2(3) . . . . ?
V8 O27 C25 C34 128.1(3) . . . . ?
V8 O27 C25 C37 7.2(4) . . . . ?
V8 N28 C3 N27 172.6(2) . . . . ?
V8 N28 C3 N30 -5.4(5) . . . . ?
V8 N28 C7 N26 -172.7(2) . . . . ?
V8 N28 C7 N29 9.3(5) . . . . ?
V8 N32 C2 N33 -162.2(2) . . . . ?
V8 N32 C2 N35 18.5(5) . . . . ?
V8 N36 N37 V7 -4.3(3) . . . . ?
V8 N36 N37 C5 -164.7(2) . . . . ?
V8 N36 C1 N38 162.5(2) . . . . ?
V8 N36 C1 N39 -20.6(4) . . . . ?
V7 O27 C25 C24 39.3(3) . . . . ?
V7 O27 C25 C34 -78.4(3) . . . . ?
V7 O27 C25 C37 160.8(2) . . . . ?
V7 O28 C19 O29 175.3(2) . . . . ?
V7 O28 C19 C34 -5.2(5) . . . . ?
V7 O30 C24 O31 -172.4(3) . . . . ?
V7 O30 C24 C25 6.9(4) . . . . ?
V7 N31 N32 V8 -11.4(3) . . . . ?
V7 N31 N32 C2 -177.0(2) . . . . ?
V7 N31 C6 N33 175.8(2) . . . . ?
V7 N31 C6 N34 -4.9(5) . . . . ?
V7 N37 C5 N38 -157.1(2) . . . . ?
V7 N37 C5 N40 26.1(5) . . . . ?
K1 O5 C13 O4 119.5(4) . . . . ?
K1 O5 C13 C8 -61.6(5) . . . . ?
K1 O13 C21 O12 -21.0(5) 2_556 . . . ?
K1 O13 C21 C30 160.4(2) 2_556 . . . ?
K1 O15 C11 O14 -96.8(4) 4_575 . . . ?
K1 O15 C11 C29 86.9(4) 4_575 . . . ?
K2 O20 C27 O19 109.5(4) 4_575 . . . ?
K2 O20 C27 C9 -69.4(5) 4_575 . . . ?
K2 O31 C24 O30 -73.9(5) . . . . ?
K2 O31 C24 C25 106.9(5) . . . . ?
K2A O20 C27 O19 131.4(6) 4_575 . . . ?
K2A O20 C27 C9 -47.5(8) 4_575 . . . ?
K2A O31 C24 O30 -99.3(7) . . . . ?
K2A O31 C24 C25 81.5(8) . . . . ?
O1 C12 C18 C8 -64.3(4) . . . . ?
O2 C12 C18 C8 116.7(4) . . . . ?
O3 C8 C13 O4 31.7(4) . . . . ?
O3 C8 C13 O5 -147.3(3) . . . . ?
O3 C8 C18 C12 53.8(4) . . . . ?
O3 C8 C23 C20 -43.9(4) . . . . ?
O6 C20 C23 C8 1.0(5) . . . . ?
O7 C20 C23 C8 -179.6(4) . . . . ?
O10 C26 C32 C29 -115.2(4) . . . . ?
O11 C29 C30 C21 40.1(4) . . . . ?
O11 C29 C32 C26 -50.7(4) . . . . ?
O12 C21 C30 C29 7.8(5) . . . . ?
O13 C21 C30 C29 -173.7(3) . . . . ?
O14 C11 C29 O11 -40.7(4) . . . . ?
O14 C11 C29 C30 77.6(4) . . . . ?
O14 C11 C29 C32 -161.8(3) . . . . ?
O15 C11 C29 O11 135.9(3) . . . . ?
O15 C11 C29 C30 -105.8(4) . . . . ?
O15 C11 C29 C32 14.7(4) . . . . ?
O18 C9 C15 C28 53.1(4) . . . . ?
O18 C9 C27 O19 37.2(4) . . . . ?
O18 C9 C27 O20 -143.8(3) . . . . ?
O18 C9 C39 C40 -50.0(4) . . . . ?
O25 C33 C37 C25 66.5(5) . . . . ?
O26 C33 C37 C25 -112.0(5) . . . . ?
O27 C25 C34 C19 42.5(4) . . . . ?
O27 C25 C37 C33 -52.5(4) . . . . ?
O28 C19 C34 C25 2.4(5) . . . . ?
O29 C19 C34 C25 -178.1(3) . . . . ?
O30 C24 C25 O27 -31.4(4) . . . . ?
O30 C24 C25 C34 87.5(4) . . . . ?
O30 C24 C25 C37 -153.6(3) . . . . ?
O31 C24 C25 O27 147.8(4) . . . . ?
O31 C24 C25 C34 -93.2(5) . . . . ?
O31 C24 C25 C37 25.7(5) . . . . ?
O34 C26 C32 C29 65.9(4) . . . . ?
N1 N2 C38 N3 0.3(4) . . . . ?
N1 N2 C38 N5 -179.9(4) . . . . ?
N2 N1 C31 N3 -0.7(4) . . . . ?
N2 N1 C31 N4 -179.5(4) . . . . ?
N6 N7 C4 N8 1.2(4) . . . . ?
N6 N7 C4 N10 -179.8(3) . . . . ?
N7 N6 C17 N8 0.9(3) . . . . ?
N7 N6 C17 N9 178.4(3) . . . . ?
N11 N12 C35 N13 0.5(4) . . . . ?
N11 N12 C35 N15 -179.6(4) . . . . ?
N12 N11 C36 N13 -0.1(4) . . . . ?
N12 N11 C36 N14 178.1(3) . . . . ?
N16 N17 C14 N18 -1.6(3) . . . . ?
N16 N17 C14 N20 176.0(3) . . . . ?
N17 N16 C10 N18 0.5(4) . . . . ?
N17 N16 C10 N19 -175.3(3) . . . . ?
N21 N22 C22 N23 1.2(4) . . . . ?
N21 N22 C22 N25 -178.5(3) . . . . ?
N22 N21 C16 N23 -0.6(4) . . . . ?
N22 N21 C16 N24 -179.1(3) . . . . ?
N26 N27 C3 N28 0.4(4) . . . . ?
N26 N27 C3 N30 178.4(3) . . . . ?
N27 N26 C7 N28 0.7(3) . . . . ?
N27 N26 C7 N29 178.8(3) . . . . ?
N31 N32 C2 N33 1.0(3) . . . . ?
N31 N32 C2 N35 -178.2(3) . . . . ?
N32 N31 C6 N33 0.4(3) . . . . ?
N32 N31 C6 N34 179.8(3) . . . . ?
N36 N37 C5 N38 -0.3(3) . . . . ?
N36 N37 C5 N40 -177.1(3) . . . . ?
N37 N36 C1 N38 -1.8(3) . . . . ?
N37 N36 C1 N39 175.2(3) . . . . ?
C1 N36 N37 V7 161.65(19) . . . . ?
C1 N36 N37 C5 1.3(3) . . . . ?
C1 N38 C5 N37 -0.7(3) . . . . ?
C1 N38 C5 N40 176.1(3) . . . . ?
C2 N33 C6 N31 0.2(4) . . . . ?
C2 N33 C6 N34 -179.2(3) . . . . ?
C3 N28 C7 N26 -0.5(3) . . . . ?
C3 N28 C7 N29 -178.5(3) . . . . ?
C4 N8 C17 N6 -0.2(3) . . . . ?
C4 N8 C17 N9 -177.6(3) . . . . ?
C5 N38 C1 N36 1.5(3) . . . . ?
C5 N38 C1 N39 -175.4(3) . . . . ?
C6 N31 N32 V8 164.7(2) . . . . ?
C6 N31 N32 C2 -0.9(3) . . . . ?
C6 N33 C2 N32 -0.8(4) . . . . ?
C6 N33 C2 N35 178.5(3) . . . . ?
C7 N26 N27 V5 -177.9(2) . . . . ?
C7 N26 N27 C3 -0.6(3) . . . . ?
C7 N28 C3 N27 0.0(4) . . . . ?
C7 N28 C3 N30 -178.0(3) . . . . ?
C9 C15 C28 O35 -52.3(5) . . . . ?
C9 C15 C28 O36 128.6(4) . . . . ?
C9 C39 C40 O21 21.4(6) . . . . ?
C9 C39 C40 O22 -148.4(7) . . . . ?
C9 C39 C40 O22A 179.6(8) . . . . ?
C10 N16 N17 V4 -167.8(2) . . . . ?
C10 N16 N17 C14 0.7(3) . . . . ?
C10 N18 C14 N17 1.9(4) . . . . ?
C10 N18 C14 N20 -175.7(3) . . . . ?
C11 C29 C30 C21 -76.0(4) . . . . ?
C11 C29 C32 C26 66.4(4) . . . . ?
C13 C8 C18 C12 -66.4(4) . . . . ?
C13 C8 C23 C20 73.1(4) . . . . ?
C14 N18 C10 N16 -1.4(4) . . . . ?
C14 N18 C10 N19 174.4(3) . . . . ?
C15 C9 C27 O19 161.5(3) . . . . ?
C15 C9 C27 O20 -19.5(5) . . . . ?
C15 C9 C39 C40 -174.3(3) . . . . ?
C16 N21 N22 V5 -172.6(2) . . . . ?
C16 N21 N22 C22 -0.4(4) . . . . ?
C16 N23 C22 N22 -1.6(4) . . . . ?
C16 N23 C22 N25 178.2(3) . . . . ?
C17 N6 N7 V1 -179.5(2) . . . . ?
C17 N6 N7 C4 -1.3(3) . . . . ?
C17 N8 C4 N7 -0.7(4) . . . . ?
C17 N8 C4 N10 -179.6(3) . . . . ?
C18 C8 C13 O4 154.5(3) . . . . ?
C18 C8 C13 O5 -24.5(4) . . . . ?
C18 C8 C23 C20 -166.9(3) . . . . ?
C22 N23 C16 N21 1.3(4) . . . . ?
C22 N23 C16 N24 179.9(3) . . . . ?
C23 C8 C13 O4 -87.2(3) . . . . ?
C23 C8 C13 O5 93.8(4) . . . . ?
C23 C8 C18 C12 176.0(3) . . . . ?
C24 C25 C34 C19 -74.1(4) . . . . ?
C24 C25 C37 C33 66.6(4) . . . . ?
C27 C9 C15 C28 -67.3(4) . . . . ?
C27 C9 C39 C40 65.4(4) . . . . ?
C30 C29 C32 C26 -171.4(3) . . . . ?
C31 N1 N2 V1 -173.6(2) . . . . ?
C31 N1 N2 C38 0.3(4) . . . . ?
C31 N3 C38 N2 -0.7(4) . . . . ?
C31 N3 C38 N5 179.4(4) . . . . ?
C32 C29 C30 C21 162.6(3) . . . . ?
C34 C25 C37 C33 -174.4(3) . . . . ?
C35 N13 C36 N11 0.4(4) . . . . ?
C35 N13 C36 N14 -177.9(3) . . . . ?
C36 N11 N12 V4 173.6(2) . . . . ?
C36 N11 N12 C35 -0.2(4) . . . . ?
C36 N13 C35 N12 -0.6(4) . . . . ?
C36 N13 C35 N15 179.5(4) . . . . ?
C37 C25 C34 C19 165.5(3) . . . . ?
C38 N3 C31 N1 0.9(4) . . . . ?
C38 N3 C31 N4 179.7(4) . . . . ?
C39 C9 C15 C28 175.5(3) . . . . ?
C39 C9 C27 O19 -80.6(3) . . . . ?
C39 C9 C27 O20 98.5(4) . . . . ?

_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 0.474 0.000 0.000 1201.2 397.8 '40 H2O'
2 -0.775 -0.002 0.500 1201.2 397.8 '40 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.339
_oxdiff_exptl_absorpt_empirical_full_min 0.768
# start Validation Reply Form
_vrf_PLAT220_exp_13142_k2v8_auto 
;
PROBLEM: Non Solvent Resd 1  O   Ueq(max) / Ueq(min) Range        6.3 Ratio
RESPONSE: This alert is due to the disordered O atoms O22 and O9w.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_9808_auto
_database_code_depnum_ccdc_archive 'CCDC 2262728'
loop_
_audit_author_name
_audit_author_address
'Xie Zhen-Lang'
;Xiamen University
China
;
_audit_update_record             
;
2023-05-13 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_audit_creation_date             2023-04-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C20 H28 N20 O22 V6, 4[H2O]'
_chemical_formula_sum            'C20 H36 N20 O26 V6'
_chemical_formula_weight         1278.33
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N V'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.60453(18)
_cell_length_b                   18.2772(3)
_cell_length_c                   11.2855(2)
_cell_angle_alpha                90
_cell_angle_beta                 106.3481(18)
_cell_angle_gamma                90
_cell_volume                     2098.93(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8909
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      73.7480
_cell_measurement_theta_min      4.7150
_shelx_estimated_absorpt_T_max   0.384
_shelx_estimated_absorpt_T_min   0.270
_exptl_absorpt_coefficient_mu    11.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.023
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13873
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.943
_diffrn_reflns_theta_min         4.746
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -71.00  33.00   0.50    0.12    --  -43.34  95.00 125.00  208
  2  ω     13.00  55.00   0.50    0.12    --   43.34 -95.00  15.00   84
  3  ω   -129.00 -83.00   0.50    0.48    --  -96.00 -95.00  15.00   92
  4  ω    -80.00 -19.00   0.50    0.48    --  -96.00  95.00 125.00  122
  5  ω     63.00 108.00   0.50    0.48    --  108.01 -95.00  15.00   90
  6  ω    105.00 157.00   0.50    0.48    --  108.01  95.00 125.00  104
  7  ω   -117.00 -73.00   0.50    0.12    --  -43.34-125.00-180.00   88
  8  ω   -108.00 -70.00   0.50    0.12    --  -43.34-125.00 -90.00   76
  9  ω    -26.00  25.00   0.50    0.12    --  -43.34  19.00-120.00  102
 10  ω   -116.00 -85.00   0.50    0.12    --  -43.34-125.00 150.00   62
 11  ω    -50.00 -22.00   0.50    0.48    --  -96.00  45.00-150.00   56
 12  ω    -70.00 -22.00   0.50    0.48    --  -96.00  61.00 -60.00   96
 13  ω    -90.00 -65.00   0.50    0.48    --  -96.00 125.00  30.00   50
 14  ω    -51.00 -23.00   0.50    0.48    --  -96.00  45.00 120.00   56
 15  ω    -50.00 -19.00   0.50    0.48    --  -96.00  45.00-120.00   62
 16  ω    -50.00 -25.00   0.50    0.48    --  -96.00  45.00   0.00   50
 17  ω    -69.00 -25.00   0.50    0.48    --  -96.00  61.00 -90.00   88
 18  ω    -56.00 -29.00   0.50    0.48    --  -96.00  61.00 -30.00   54
 19  ω    -50.00 -21.00   0.50    0.48    --  -96.00  45.00 150.00   58
 20  ω    -51.00 -25.00   0.50    0.48    --  -96.00  45.00  90.00   52
 21  ω     78.00 103.00   0.50    0.48    --  108.01 -77.00  30.00   50
 22  ω     33.00  63.00   0.50    0.48    --  108.01 -77.00  30.00   60
 23  ω     41.00  67.00   0.50    0.48    --  108.01 -61.00-180.00   52
 24  ω     39.00  71.00   0.50    0.48    --  108.01 -61.00 150.00   64
 25  ω     35.00 105.00   0.50    0.48    --  108.01 -77.00 -60.00  140
 26  ω     41.00  67.00   0.50    0.48    --  108.01 -61.00  90.00   52
 27  ω     35.00  61.00   0.50    0.48    --  108.01 -61.00  30.00   52
 28  ω     71.00 101.00   0.50    0.48    --  108.01 -77.00-120.00   60
 29  ω     45.00  70.00   0.50    0.48    --  108.01 -77.00-120.00   50
 30  ω     34.00  62.00   0.50    0.48    --  108.01 -61.00  60.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0849251000
_diffrn_orient_matrix_UB_12      0.0259764000
_diffrn_orient_matrix_UB_13      -0.0824763000
_diffrn_orient_matrix_UB_21      0.0205277000
_diffrn_orient_matrix_UB_22      0.0743029000
_diffrn_orient_matrix_UB_23      0.0671702000
_diffrn_orient_matrix_UB_31      0.1235581000
_diffrn_orient_matrix_UB_32      -0.0301795000
_diffrn_orient_matrix_UB_33      0.0945022000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3819
_reflns_number_total             4055
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_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         0.380
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00034(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4055
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0311
_refine_ls_restrained_S_all      1.056
_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)+(0.0383P)²+1.7543P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0811
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4C,H4D)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N8(H8)
2.c X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N4(H4A,H4B), N10(H10A,H10B), N9(H9A,H9B)
;
_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
V1 V 0.63787(4) 0.57978(2) 0.76453(3) 0.01484(11) Uani 1 1 d . . . . .
V3 V 0.77986(4) 0.48200(2) 0.57251(3) 0.01583(11) Uani 1 1 d . . . . .
V2 V 0.60435(4) 0.42493(2) 0.77099(3) 0.01786(11) Uani 1 1 d . . . . .
O3 O 0.52972(15) 0.51139(8) 0.83407(14) 0.0171(3) Uani 1 1 d . . . . .
O1 O 0.49961(15) 0.65565(9) 0.74739(14) 0.0188(3) Uani 1 1 d . . . . .
O10 O 0.69511(15) 0.49387(8) 0.69776(14) 0.0169(3) Uani 1 1 d . . . . .
O7 O 0.21797(15) 0.52772(9) 0.60904(14) 0.0194(3) Uani 1 1 d . . . . .
O8 O 0.75167(16) 0.60451(9) 0.88332(15) 0.0216(3) Uani 1 1 d . . . . .
O2 O 0.39295(17) 0.72151(9) 0.85381(16) 0.0239(4) Uani 1 1 d . . . . .
O4 O 0.43998(17) 0.37045(9) 0.76568(16) 0.0251(4) Uani 1 1 d . . . . .
O6 O 0.41902(15) 0.50766(9) 0.59859(15) 0.0215(3) Uani 1 1 d . . . . .
O11 O 0.93456(16) 0.47348(10) 0.63588(16) 0.0262(4) Uani 1 1 d . . . . .
O9 O 0.70893(17) 0.39250(10) 0.89074(15) 0.0253(4) Uani 1 1 d . . . . .
O5 O 0.2921(2) 0.33302(10) 0.85724(18) 0.0340(4) Uani 1 1 d . . . . .
N2 N 0.76510(18) 0.59433(10) 0.55784(17) 0.0171(4) Uani 1 1 d . . . . .
N1 N 0.68945(18) 0.63298(10) 0.62283(17) 0.0164(4) Uani 1 1 d . . . . .
N3 N 0.76822(18) 0.71114(10) 0.51408(18) 0.0186(4) Uani 1 1 d . . . . .
H3 H 0.785610 0.752403 0.481691 0.022 Uiso 1 1 calc R U . . .
N7 N 0.71588(19) 0.37443(10) 0.56663(17) 0.0196(4) Uani 1 1 d . . . . .
N5 N 0.6349(2) 0.75780(11) 0.63518(19) 0.0226(4) Uani 1 1 d . . . . .
H5A H 0.587950 0.748989 0.686677 0.027 Uiso 1 1 calc R U . . .
H5B H 0.643044 0.802876 0.610933 0.027 Uiso 1 1 calc R U . . .
N6 N 0.6310(2) 0.35400(11) 0.63791(17) 0.0206(4) Uani 1 1 d . . . . .
N4 N 0.8873(2) 0.63034(11) 0.4207(2) 0.0247(4) Uani 1 1 d . . . . .
H4A H 0.912891 0.585526 0.410643 0.030 Uiso 1 1 calc R U . . .
H4B H 0.912331 0.667061 0.382144 0.030 Uiso 1 1 calc R U . . .
N8 N 0.6798(2) 0.25675(11) 0.54593(19) 0.0244(4) Uani 1 1 d . . . . .
H8 H 0.682498 0.211125 0.521868 0.029 Uiso 1 1 calc R U . . .
N10 N 0.8170(2) 0.31061(12) 0.43529(19) 0.0266(4) Uani 1 1 d . . . . .
H10A H 0.854800 0.350089 0.416515 0.032 Uiso 1 1 calc R U . . .
H10B H 0.828553 0.268076 0.403350 0.032 Uiso 1 1 calc R U . . .
N9 N 0.5413(2) 0.24169(12) 0.6788(2) 0.0306(5) Uani 1 1 d . . . . .
H9A H 0.501411 0.262036 0.729108 0.037 Uiso 1 1 calc R U . . .
H9B H 0.534014 0.194320 0.664589 0.037 Uiso 1 1 calc R U . . .
C1 C 0.4210(2) 0.66212(13) 0.8171(2) 0.0181(4) Uani 1 1 d . . . . .
C8 C 0.8106(2) 0.64263(12) 0.4943(2) 0.0182(4) Uani 1 1 d . . . . .
C3 C 0.3906(2) 0.52136(12) 0.8017(2) 0.0178(4) Uani 1 1 d . . . . .
C6 C 0.3406(2) 0.51885(12) 0.6606(2) 0.0173(4) Uani 1 1 d . . . . .
C2 C 0.3589(2) 0.59417(13) 0.8528(2) 0.0203(5) Uani 1 1 d . . . . .
H2A H 0.262318 0.600736 0.825838 0.024 Uiso 1 1 calc R U . . .
H2B H 0.385689 0.590772 0.944016 0.024 Uiso 1 1 calc R U . . .
C7 C 0.6938(2) 0.70274(12) 0.5938(2) 0.0179(4) Uani 1 1 d . . . . .
C5 C 0.3544(2) 0.38254(13) 0.8256(2) 0.0221(5) Uani 1 1 d . . . . .
C10 C 0.7419(2) 0.31526(13) 0.5123(2) 0.0205(5) Uani 1 1 d . . . . .
C9 C 0.6128(2) 0.28270(13) 0.6240(2) 0.0229(5) Uani 1 1 d . . . . .
C4 C 0.3273(2) 0.46032(13) 0.8575(2) 0.0217(5) Uani 1 1 d . . . . .
H4C H 0.356949 0.465475 0.948473 0.026 Uiso 1 1 calc R U . . .
H4D H 0.230982 0.467955 0.831223 0.026 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 2.8560(5) . ?
V1 O3 2.0001(16) . ?
V1 O1 1.9875(16) . ?
V1 O10 1.9130(15) . ?
V1 O8 1.5960(16) . ?
V1 N1 2.0723(18) . ?
V3 O10 1.8888(16) . ?
V3 O7 2.0632(16) 3_666 ?
V3 O6 2.4330(16) 3_666 ?
V3 O11 1.6020(17) . ?
V3 N2 2.0621(19) . ?
V3 N7 2.075(2) . ?
V2 O3 1.9868(16) . ?
V2 O10 1.9092(16) . ?
V2 O4 1.9936(17) . ?
V2 O9 1.6012(17) . ?
V2 N6 2.063(2) . ?
O3 C3 1.428(3) . ?
O1 C1 1.303(3) . ?
O7 C6 1.277(3) . ?
O2 C1 1.228(3) . ?
O4 C5 1.294(3) . ?
O6 C6 1.246(3) . ?
O5 C5 1.231(3) . ?
N2 N1 1.418(2) . ?
N2 C8 1.312(3) . ?
N1 C7 1.320(3) . ?
N3 H3 0.8800 . ?
N3 C8 1.370(3) . ?
N3 C7 1.362(3) . ?
N7 N6 1.416(3) . ?
N7 C10 1.310(3) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N5 C7 1.336(3) . ?
N6 C9 1.320(3) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
N4 C8 1.336(3) . ?
N8 H8 0.8800 . ?
N8 C10 1.364(3) . ?
N8 C9 1.364(3) . ?
N10 H10A 0.8800 . ?
N10 H10B 0.8800 . ?
N10 C10 1.337(3) . ?
N9 H9A 0.8800 . ?
N9 H9B 0.8800 . ?
N9 C9 1.335(3) . ?
C1 C2 1.512(3) . ?
C3 C6 1.531(3) . ?
C3 C2 1.525(3) . ?
C3 C4 1.526(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C5 C4 1.514(3) . ?
C4 H4C 0.9900 . ?
C4 H4D 0.9900 . ?

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
O3 V1 V2 44.06(4) . . ?
O3 V1 N1 154.30(7) . . ?
O1 V1 V2 126.88(5) . . ?
O1 V1 O3 89.17(6) . . ?
O1 V1 N1 86.86(7) . . ?
O10 V1 V2 41.60(5) . . ?
O10 V1 O3 85.54(6) . . ?
O10 V1 O1 147.30(7) . . ?
O10 V1 N1 84.21(7) . . ?
O8 V1 V2 109.23(6) . . ?
O8 V1 O3 103.23(8) . . ?
O8 V1 O1 104.29(8) . . ?
O8 V1 O10 108.34(8) . . ?
O8 V1 N1 102.35(8) . . ?
N1 V1 V2 123.12(5) . . ?
O10 V3 O7 153.34(7) . 3_666 ?
O10 V3 O6 95.52(6) . 3_666 ?
O10 V3 N2 84.51(7) . . ?
O10 V3 N7 84.99(7) . . ?
O7 V3 O6 57.86(6) 3_666 3_666 ?
O7 V3 N7 88.94(7) 3_666 . ?
O11 V3 O10 108.68(8) . . ?
O11 V3 O7 97.97(8) . 3_666 ?
O11 V3 O6 155.76(8) . 3_666 ?
O11 V3 N2 100.24(9) . . ?
O11 V3 N7 101.93(9) . . ?
N2 V3 O7 91.60(7) . 3_666 ?
N2 V3 O6 80.20(7) . 3_666 ?
N2 V3 N7 157.54(8) . . ?
N7 V3 O6 81.12(7) . 3_666 ?
O3 V2 V1 44.43(4) . . ?
O3 V2 O4 88.56(7) . . ?
O3 V2 N6 155.61(7) . . ?
O10 V2 V1 41.70(5) . . ?
O10 V2 O3 86.01(6) . . ?
O10 V2 O4 149.28(7) . . ?
O10 V2 N6 84.87(7) . . ?
O4 V2 V1 127.46(5) . . ?
O4 V2 N6 87.82(8) . . ?
O9 V2 V1 109.07(7) . . ?
O9 V2 O3 104.07(8) . . ?
O9 V2 O10 107.21(8) . . ?
O9 V2 O4 103.45(8) . . ?
O9 V2 N6 100.23(8) . . ?
N6 V2 V1 124.11(6) . . ?
V2 O3 V1 91.50(6) . . ?
C3 O3 V1 119.02(13) . . ?
C3 O3 V2 119.80(13) . . ?
C1 O1 V1 125.75(14) . . ?
V3 O10 V1 131.27(8) . . ?
V3 O10 V2 130.71(8) . . ?
V2 O10 V1 96.70(7) . . ?
C6 O7 V3 98.48(13) . 3_666 ?
C5 O4 V2 129.41(15) . . ?
C6 O6 V3 82.33(13) . 3_666 ?
N1 N2 V3 119.70(13) . . ?
C8 N2 V3 133.04(15) . . ?
C8 N2 N1 107.23(18) . . ?
N2 N1 V1 118.42(13) . . ?
C7 N1 V1 132.82(15) . . ?
C7 N1 N2 106.76(17) . . ?
C8 N3 H3 126.8 . . ?
C7 N3 H3 126.8 . . ?
C7 N3 C8 106.40(18) . . ?
N6 N7 V3 119.09(14) . . ?
C10 N7 V3 133.41(17) . . ?
C10 N7 N6 107.41(19) . . ?
H5A N5 H5B 120.0 . . ?
C7 N5 H5A 120.0 . . ?
C7 N5 H5B 120.0 . . ?
N7 N6 V2 119.16(14) . . ?
C9 N6 V2 131.39(16) . . ?
C9 N6 N7 106.75(19) . . ?
H4A N4 H4B 120.0 . . ?
C8 N4 H4A 120.0 . . ?
C8 N4 H4B 120.0 . . ?
C10 N8 H8 126.7 . . ?
C9 N8 H8 126.7 . . ?
C9 N8 C10 106.69(19) . . ?
H10A N10 H10B 120.0 . . ?
C10 N10 H10A 120.0 . . ?
C10 N10 H10B 120.0 . . ?
H9A N9 H9B 120.0 . . ?
C9 N9 H9A 120.0 . . ?
C9 N9 H9B 120.0 . . ?
O1 C1 C2 119.12(19) . . ?
O2 C1 O1 122.7(2) . . ?
O2 C1 C2 118.14(19) . . ?
N2 C8 N3 109.74(19) . . ?
N2 C8 N4 127.5(2) . . ?
N4 C8 N3 122.7(2) . . ?
O3 C3 C6 107.02(17) . . ?
O3 C3 C2 109.68(18) . . ?
O3 C3 C4 110.12(18) . . ?
C2 C3 C6 111.75(18) . . ?
C2 C3 C4 108.22(18) . . ?
C4 C3 C6 110.07(18) . . ?
O7 C6 C3 118.75(19) . . ?
O6 C6 O7 121.3(2) . . ?
O6 C6 C3 119.9(2) . . ?
C1 C2 C3 117.21(18) . . ?
C1 C2 H2A 108.0 . . ?
C1 C2 H2B 108.0 . . ?
C3 C2 H2A 108.0 . . ?
C3 C2 H2B 108.0 . . ?
H2A C2 H2B 107.2 . . ?
N1 C7 N3 109.86(19) . . ?
N1 C7 N5 126.0(2) . . ?
N5 C7 N3 124.1(2) . . ?
O4 C5 C4 119.5(2) . . ?
O5 C5 O4 122.6(2) . . ?
O5 C5 C4 117.9(2) . . ?
N7 C10 N8 109.6(2) . . ?
N7 C10 N10 126.8(2) . . ?
N10 C10 N8 123.6(2) . . ?
N6 C9 N8 109.5(2) . . ?
N6 C9 N9 125.6(2) . . ?
N9 C9 N8 124.8(2) . . ?
C3 C4 H4C 108.1 . . ?
C3 C4 H4D 108.1 . . ?
C5 C4 C3 116.96(19) . . ?
C5 C4 H4C 108.1 . . ?
C5 C4 H4D 108.1 . . ?
H4C C4 H4D 107.3 . . ?

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
N3 H3 O2 0.88 2.13 2.808(2) 133.5 4_675 yes
N5 H5A O1 0.88 2.15 2.858(3) 137.2 . yes
N5 H5B O9 0.88 2.27 3.027(3) 143.7 2_656 yes
N4 H4A O7 0.88 2.47 3.081(3) 127.4 3_666 yes
N4 H4A O11 0.88 2.13 2.873(3) 141.8 3_766 yes
N4 H4B O2 0.88 2.06 2.816(3) 143.0 4_675 yes
N8 H8 O8 0.88 2.24 2.929(3) 135.3 2_646 yes
N8 H8 O5 0.88 2.58 3.174(3) 125.3 4_665 yes
N10 H10A O7 0.88 2.35 3.002(3) 130.7 3_666 yes
N10 H10B O5 0.88 1.93 2.758(3) 156.4 4_665 yes
N9 H9A O4 0.88 2.16 2.872(3) 137.4 . yes
C2 H2B O9 0.99 2.37 3.182(3) 138.4 3_667 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 O3 C3 C6 56.4(2) . . . . ?
V1 O3 C3 C2 -65.0(2) . . . . ?
V1 O3 C3 C4 176.06(13) . . . . ?
V1 O1 C1 O2 138.35(19) . . . . ?
V1 O1 C1 C2 -43.0(3) . . . . ?
V1 N1 C7 N3 162.93(15) . . . . ?
V1 N1 C7 N5 -17.1(4) . . . . ?
V3 O7 C6 O6 -0.5(2) 3_666 . . . ?
V3 O7 C6 C3 -179.88(16) 3_666 . . . ?
V3 O6 C6 O7 0.4(2) 3_666 . . . ?
V3 O6 C6 C3 179.79(19) 3_666 . . . ?
V3 N2 N1 V1 16.0(2) . . . . ?
V3 N2 N1 C7 -178.07(14) . . . . ?
V3 N2 C8 N3 177.76(15) . . . . ?
V3 N2 C8 N4 -2.5(4) . . . . ?
V3 N7 N6 V2 -12.5(2) . . . . ?
V3 N7 N6 C9 -175.91(15) . . . . ?
V3 N7 C10 N8 175.62(15) . . . . ?
V3 N7 C10 N10 -4.4(4) . . . . ?
V2 O3 C3 C6 -54.2(2) . . . . ?
V2 O3 C3 C2 -175.58(13) . . . . ?
V2 O3 C3 C4 65.4(2) . . . . ?
V2 O4 C5 O5 -148.05(19) . . . . ?
V2 O4 C5 C4 32.7(3) . . . . ?
V2 N6 C9 N8 -161.67(16) . . . . ?
V2 N6 C9 N9 17.6(4) . . . . ?
O3 C3 C6 O7 -178.92(18) . . . . ?
O3 C3 C6 O6 1.7(3) . . . . ?
O3 C3 C2 C1 55.3(3) . . . . ?
O3 C3 C4 C5 -56.1(3) . . . . ?
O1 C1 C2 C3 -1.2(3) . . . . ?
O7 V3 O10 V1 -84.19(18) 3_666 . . . ?
O7 V3 O10 V2 79.51(18) 3_666 . . . ?
O2 C1 C2 C3 177.5(2) . . . . ?
O4 C5 C4 C3 7.8(3) . . . . ?
O6 V3 O10 V1 -81.16(11) 3_666 . . . ?
O6 V3 O10 V2 82.54(11) 3_666 . . . ?
O11 V3 O10 V1 97.37(12) . . . . ?
O11 V3 O10 V2 -98.92(12) . . . . ?
O5 C5 C4 C3 -171.5(2) . . . . ?
N2 V3 O10 V1 -1.60(11) . . . . ?
N2 V3 O10 V2 162.10(12) . . . . ?
N2 N1 C7 N3 -0.1(2) . . . . ?
N2 N1 C7 N5 179.8(2) . . . . ?
N1 N2 C8 N3 -0.2(2) . . . . ?
N1 N2 C8 N4 179.5(2) . . . . ?
N7 V3 O10 V1 -161.71(12) . . . . ?
N7 V3 O10 V2 1.99(11) . . . . ?
N7 N6 C9 N8 -1.0(2) . . . . ?
N7 N6 C9 N9 178.2(2) . . . . ?
N6 N7 C10 N8 -0.9(2) . . . . ?
N6 N7 C10 N10 179.0(2) . . . . ?
C8 N2 N1 V1 -165.74(14) . . . . ?
C8 N2 N1 C7 0.2(2) . . . . ?
C8 N3 C7 N1 0.0(2) . . . . ?
C8 N3 C7 N5 -180.0(2) . . . . ?
C6 C3 C2 C1 -63.2(3) . . . . ?
C6 C3 C4 C5 61.6(3) . . . . ?
C2 C3 C6 O7 -58.8(3) . . . . ?
C2 C3 C6 O6 121.8(2) . . . . ?
C2 C3 C4 C5 -176.00(19) . . . . ?
C7 N3 C8 N2 0.1(2) . . . . ?
C7 N3 C8 N4 -179.6(2) . . . . ?
C10 N7 N6 V2 164.65(15) . . . . ?
C10 N7 N6 C9 1.2(2) . . . . ?
C10 N8 C9 N6 0.5(3) . . . . ?
C10 N8 C9 N9 -178.7(2) . . . . ?
C9 N8 C10 N7 0.3(3) . . . . ?
C9 N8 C10 N10 -179.6(2) . . . . ?
C4 C3 C6 O7 61.4(3) . . . . ?
C4 C3 C6 O6 -117.9(2) . . . . ?
C4 C3 C2 C1 175.42(19) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 1.000 96.1 40.8 '4 H2O'
2 0.500 0.000 0.500 96.1 40.8 '4 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.863
_oxdiff_exptl_absorpt_empirical_full_min 0.673
