# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_607_auto
_database_code_depnum_ccdc_archive 'CCDC 2154370'
loop_
_audit_author_name
_audit_author_address
'Zhao-Hui Zhou'
;Xiamen University
China
;
_audit_update_record             
;
2022-02-24 deposited with the CCDC.	2022-07-01 downloaded from the CCDC.
;
_audit_creation_date             2022-02-09
_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 H16 K2 N8 O24 V4, 2(H4 N)'
_chemical_formula_sum            'C20 H34 K2 N10 O29 V4'
_chemical_formula_weight         1160.53
_chemical_absolute_configuration ?
_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      trigonal
_space_group_IT_number           154
_space_group_name_H-M_alt        'P 32 2 1'
_space_group_name_Hall           'P 32 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'x-y, -y, -z+1/3'
'-x, -x+y, -z+2/3'

_cell_length_a                   18.11633(10)
_cell_length_b                   18.11633(10)
_cell_length_c                   11.42819(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3248.24(4)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    42550
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.9090
_cell_measurement_theta_min      2.7940
_shelx_estimated_absorpt_T_max   0.642
_shelx_estimated_absorpt_T_min   0.443
_exptl_absorpt_coefficient_mu    9.713
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (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 violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1758
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            48980
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.981
_diffrn_reflns_theta_min         2.816
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     95.00 177.00   0.50    0.07    --  105.19  45.00-150.00  164
  2  ω    100.00 178.00   0.50    0.07    --  105.19  30.00 -60.00  156
  3  ω    -16.00  19.00   0.50    0.05    --   47.87 -19.00-120.00   70
  4  ω    -25.00  27.00   0.50    0.05    --   47.87 -19.00-150.00  104
  5  ω    -24.00  28.00   0.50    0.05    --   47.87 -19.00  90.00  104
  6  ω     92.00 177.00   0.50    0.07    --  105.19  61.00 150.00  170
  7  ω     33.00  69.00   0.50    0.07    --  105.19 -95.00-150.00   72
  8  ω     53.00  79.00   0.50    0.07    --  105.19-125.00 -90.00   52
  9  ω     71.00 119.00   0.50    0.07    --  105.19-135.00-129.00   96
 10  ω     37.00 105.00   0.50    0.07    --  105.19 -95.00-120.00  136
 11  ω     54.00  80.00   0.50    0.05    --   47.87-135.00-129.00   52
 12  ω     69.00 112.00   0.50    0.07    --  105.19-125.00 -60.00   86
 13  ω     35.00  63.00   0.50    0.05    --   47.87-134.00  49.00   56
 14  ω     72.00 119.00   0.50    0.07    --  105.19-134.00  49.00   94
 15  ω     33.00 100.00   0.50    0.07    --  105.19 -95.00  30.00  134
 16  ω     33.00  84.00   0.50    0.07    --  105.19 -77.00  30.00  102
 17  ω     36.00  61.00   0.50    0.07    --  105.19 -61.00  90.00   50
 18  ω     38.00  67.00   0.50    0.07    --  105.19 -61.00  60.00   58
 19  ω     47.00  73.00   0.50    0.07    --  105.19 -61.00 -60.00   52
 20  ω     38.00  73.00   0.50    0.07    --  105.19 -61.00 -90.00   70
 21  ω     72.00  97.00   0.50    0.05    --   47.87 135.00 -64.00   50
 22  ω    100.00 125.00   0.50    0.07    --  105.19 135.00 -64.00   50
 23  ω     93.00 122.00   0.50    0.07    --  105.19 134.00 116.00   58
 24  ω     73.00  98.00   0.50    0.05    --   47.87 134.00 116.00   50
 25  ω    -24.00  27.00   0.50    0.05    --  -47.87  19.00-120.00  102
 26  ω    -53.00 -27.00   0.50    0.07    --  -99.00  61.00 -90.00   52
 27  ω   -103.00 -27.00   0.50    0.07    --  -99.00  77.00 -30.00  152
 28  ω    -20.00  27.00   0.50    0.05    --  -47.87  19.00  90.00   94
 29  ω    -54.00 -29.00   0.50    0.07    --  -99.00 125.00  60.00   50
 30  ω   -116.00 -28.00   0.50    0.07    --  -99.00 134.00 116.00  176
 31  ω   -126.00 -83.00   0.50    0.07    --  -99.00 144.00  75.29   86
 32  ω   -118.00 -65.00   0.50    0.07    --  -99.00 135.00 -64.00  106
 33  ω    -97.00 -20.00   0.50    0.05    --  -47.87 135.00 -64.00  154
 34  ω   -109.00 -63.00   0.50    0.07    --  -99.00 125.00  60.00   92
 35  ω    -97.00 -48.00   0.50    0.05    --  -47.87 134.00 116.00   98
 36  ω   -114.00 -89.00   0.50    0.07    --  -99.00 -15.00 -90.00   50
 37  ω   -169.00-144.00   0.50    0.07    --  -99.00 -15.00 -90.00   50
 38  ω   -170.00 -88.00   0.50    0.07    --  -99.00 -45.00  60.00  164
 39  ω   -102.00 -77.00   0.50    0.07    --  -99.00 -77.00 120.00   50
 40  ω   -171.00 -78.00   0.50    0.07    --  -99.00 -77.00 150.00  186
 41  ω   -171.00-123.00   0.50    0.07    --  -99.00 -77.00 120.00   96
 42  ω   -119.00 -92.00   0.50    0.05    --  -47.87-125.00   0.00   54
 43  ω   -110.00 -70.00   0.50    0.05    --  -47.87-134.00  49.00   80
 44  ω   -110.00 -76.00   0.50    0.05    --  -47.87-125.00  90.00   68
 45  ω    -99.00 -74.00   0.50    0.05    --  -47.87-135.00-129.00   50
 46  ω   -123.00 -92.00   0.50    0.07    --  -99.00-135.00-129.00   62
 47  ω   -144.00-119.00   0.50    0.07    --  -99.00-134.00  49.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                4419
_reflns_number_total             4498
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         1.332
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.018(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4498
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0472
_refine_ls_restrained_S_all      1.040
_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)+(0.0734P)²+7.3684P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1259
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.982(11)
 0.018(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H,H) groups
3. Restrained distances
 O6-H6
 0.85 with sigma of 0.02
 O5-H5
 0.85 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O7) = Uanis(C10) = Uanis(O8)
5.a Riding coordinates:
 N5(H5A,H5B,H5C), N5(H5D), O8(H6), O8(H5)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6A), C7(H7), C8(H8), C2(H2), C1(H1), C3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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 0.47076(6) 0.09207(5) 0.50006(7) 0.0175(2) Uani 1 1 d . . . . .
V3 V 0.56231(7) 0.000000 0.666667 0.0168(3) Uani 1 2 d S T P . .
V2 V 0.28829(7) 0.000000 0.666667 0.0218(3) Uani 1 2 d S T P . .
K1 K 0.72200(10) 0.23899(10) 0.57879(16) 0.0443(4) Uani 1 1 d . . . . .
O5 O 0.5393(2) 0.0917(2) 0.6311(3) 0.0183(7) Uani 1 1 d D . . . .
O6 O 0.3559(3) 0.0020(2) 0.5332(3) 0.0223(8) Uani 1 1 d D . . . .
O1 O 0.5747(2) 0.2021(2) 0.4425(3) 0.0211(7) Uani 1 1 d . . . . .
O9 O 0.6905(2) 0.0809(2) 0.6524(4) 0.0255(8) Uani 1 1 d . . . . .
O2 O 0.4328(3) 0.1089(3) 0.3387(3) 0.0274(9) Uani 1 1 d . . . . .
O4 O 0.4738(3) 0.1929(3) 0.1791(4) 0.0351(10) Uani 1 1 d . . . . .
O7 O 0.1942(5) -0.0141(5) 0.5550(9) 0.0875(17) Uani 1 1 d . . . . .
O3 O 0.6213(3) 0.3021(3) 0.3051(4) 0.0305(9) Uani 1 1 d . . . . .
O2W O 0.7677(3) 0.3799(3) 0.4355(4) 0.0353(10) Uani 1 1 d . . . . .
N2 N 0.5423(3) -0.0269(3) 0.4887(4) 0.0208(9) Uani 1 1 d . . . . .
N4 N 0.3600(3) 0.1332(3) 0.6534(4) 0.0227(9) Uani 1 1 d . . . . .
O10 O 0.8172(3) 0.0882(4) 0.6497(5) 0.0474(13) Uani 1 1 d . . . . .
N3 N 0.4335(3) 0.1696(3) 0.5897(4) 0.0190(9) Uani 1 1 d . . . . .
N1 N 0.5022(3) 0.0066(3) 0.4245(4) 0.0213(9) Uani 1 1 d . . . . .
O1W O 0.8812(3) 0.2637(3) 0.6366(4) 0.0463(13) Uani 1 1 d . . . . .
C4 C 0.5680(4) 0.2328(3) 0.3469(5) 0.0225(11) Uani 1 1 d . . . . .
C6 C 0.4698(4) 0.2545(3) 0.6009(5) 0.0232(11) Uani 1 1 d . . . . .
H6A H 0.521934 0.295251 0.565639 0.028 Uiso 1 1 calc R U . . .
C7 C 0.4191(4) 0.2737(4) 0.6726(6) 0.0291(13) Uani 1 1 d . . . . .
H7 H 0.429305 0.328428 0.695488 0.035 Uiso 1 1 calc R U . . .
C5 C 0.4846(4) 0.1745(4) 0.2786(5) 0.0245(11) Uani 1 1 d . . . . .
C9 C 0.7399(4) 0.0488(4) 0.6583(6) 0.0328(13) Uani 1 1 d . . . . .
C8 C 0.3511(4) 0.1957(4) 0.7025(6) 0.0292(12) Uani 1 1 d . . . . .
H8 H 0.304831 0.187183 0.750791 0.035 Uiso 1 1 calc R U . . .
N5 N 0.2611(4) 0.0493(6) 0.3288(7) 0.066(2) Uani 1 1 d . . . . .
H5A H 0.243782 0.043329 0.252960 0.079 Uiso 1 1 d R U . . .
H5B H 0.232902 -0.002091 0.365470 0.079 Uiso 1 1 d R U . . .
H5C H 0.249692 0.087019 0.365470 0.079 Uiso 1 1 d R U . . .
H5D H 0.318202 0.068929 0.331280 0.079 Uiso 1 1 d R U . . .
C2 C 0.5181(6) -0.0838(5) 0.3096(6) 0.0456(18) Uani 1 1 d . . . . .
H2 H 0.516370 -0.116229 0.243222 0.055 Uiso 1 1 calc R U . . .
C1 C 0.4877(5) -0.0286(4) 0.3179(5) 0.0346(14) Uani 1 1 d . . . . .
H1 H 0.459961 -0.016705 0.256325 0.042 Uiso 1 1 calc R U . . .
C3 C 0.5521(5) -0.0823(4) 0.4187(5) 0.0337(14) Uani 1 1 d . . . . .
H3 H 0.577992 -0.114614 0.441103 0.040 Uiso 1 1 calc R U . . .
C10 C 0.1331(7) -0.0090(8) 0.6017(13) 0.0875(17) Uani 1 1 d . . . . .
O8 O 0.0683(5) -0.0191(5) 0.5535(9) 0.0875(17) Uani 1 1 d . . . . .
H6 H 0.337204 -0.034229 0.480388 0.04(2) Uiso 1 1 d DR . . . .
H5 H 0.562564 0.134901 0.677278 0.06(3) Uiso 1 1 d DR . . . .


_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 O5 1.948(4) . ?
V1 O6 1.934(4) . ?
V1 O1 2.049(4) . ?
V1 O2 2.043(4) . ?
V1 N3 2.105(4) . ?
V1 N1 2.085(5) . ?
V3 O5 1.947(4) 5_556 ?
V3 O5 1.947(4) . ?
V3 O9 2.041(4) 5_556 ?
V3 O9 2.041(4) . ?
V3 N2 2.081(4) 5_556 ?
V3 N2 2.081(4) . ?
V2 O6 1.945(4) 5_556 ?
V2 O6 1.946(4) . ?
V2 O7 2.041(7) . ?
V2 O7 2.041(7) 5_556 ?
V2 N4 2.097(5) . ?
V2 N4 2.097(5) 5_556 ?
K1 O1 2.865(4) . ?
K1 O9 2.758(4) . ?
K1 O4 3.330(5) 2_655 ?
K1 O3 3.052(5) 3_665 ?
K1 O2W 2.907(5) 3_665 ?
K1 O2W 2.787(5) . ?
K1 O1W 2.768(6) . ?
K1 C7 3.241(6) 2_654 ?
K1 C8 3.537(6) 2_654 ?
K1 H5 2.7783 . ?
O5 H5 0.8598 . ?
O6 H6 0.8290 . ?
O1 C4 1.259(7) . ?
O9 C9 1.290(8) . ?
O2 C5 1.284(7) . ?
O4 C5 1.229(7) . ?
O7 C10 1.273(15) . ?
O3 C4 1.235(7) . ?
N2 N1 1.369(7) . ?
N2 C3 1.363(7) . ?
N4 N3 1.363(6) . ?
N4 C8 1.344(7) . ?
O10 C9 1.216(8) . ?
N3 C6 1.342(7) . ?
N1 C1 1.338(7) . ?
C4 C5 1.553(9) . ?
C6 H6A 0.9500 . ?
C6 C7 1.398(9) . ?
C7 H7 0.9500 . ?
C7 C8 1.375(9) . ?
C9 C9 1.542(13) 5_556 ?
C8 H8 0.9500 . ?
N5 H5A 0.9096 . ?
N5 H5B 0.9099 . ?
N5 H5C 0.9097 . ?
N5 H5D 0.9101 . ?
C2 H2 0.9500 . ?
C2 C1 1.366(11) . ?
C2 C3 1.385(10) . ?
C1 H1 0.9500 . ?
C3 H3 0.9500 . ?
C10 C10 1.51(3) 5_556 ?
C10 O8 1.225(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 V1 O1 88.46(15) . . ?
O5 V1 O2 163.16(17) . . ?
O5 V1 N3 92.64(16) . . ?
O5 V1 N1 84.53(17) . . ?
O6 V1 O5 105.36(16) . . ?
O6 V1 O1 164.04(17) . . ?
O6 V1 O2 90.14(16) . . ?
O6 V1 N3 84.21(17) . . ?
O6 V1 N1 91.85(17) . . ?
O1 V1 N3 87.28(16) . . ?
O1 V1 N1 97.47(16) . . ?
O2 V1 O1 77.24(16) . . ?
O2 V1 N3 95.48(17) . . ?
O2 V1 N1 88.52(17) . . ?
N1 V1 N3 174.38(17) . . ?
O5 V3 O5 100.3(2) 5_556 . ?
O5 V3 O9 91.34(15) . . ?
O5 V3 O9 91.34(15) 5_556 5_556 ?
O5 V3 O9 167.24(16) . 5_556 ?
O5 V3 O9 167.24(16) 5_556 . ?
O5 V3 N2 90.99(16) . 5_556 ?
O5 V3 N2 91.00(16) 5_556 . ?
O5 V3 N2 84.78(16) 5_556 5_556 ?
O5 V3 N2 84.78(16) . . ?
O9 V3 O9 77.6(2) 5_556 . ?
O9 V3 N2 95.33(17) . . ?
O9 V3 N2 89.81(17) . 5_556 ?
O9 V3 N2 95.33(17) 5_556 5_556 ?
O9 V3 N2 89.81(17) 5_556 . ?
N2 V3 N2 173.4(3) 5_556 . ?
O6 V2 O6 103.3(2) 5_556 . ?
O6 V2 O7 165.5(3) . 5_556 ?
O6 V2 O7 165.5(3) 5_556 . ?
O6 V2 O7 89.5(3) . . ?
O6 V2 O7 89.5(3) 5_556 5_556 ?
O6 V2 N4 84.23(17) . . ?
O6 V2 N4 84.23(17) 5_556 5_556 ?
O6 V2 N4 92.59(17) 5_556 . ?
O6 V2 N4 92.59(17) . 5_556 ?
O7 V2 O7 78.8(6) . 5_556 ?
O7 V2 N4 95.6(3) 5_556 5_556 ?
O7 V2 N4 88.4(3) 5_556 . ?
O7 V2 N4 95.6(3) . . ?
O7 V2 N4 88.4(3) . 5_556 ?
N4 V2 N4 174.9(3) . 5_556 ?
O1 K1 O4 145.29(13) . 2_655 ?
O1 K1 O3 74.31(12) . 3_665 ?
O1 K1 O2W 81.84(12) . 3_665 ?
O1 K1 C7 71.46(14) . 2_654 ?
O1 K1 C8 94.29(14) . 2_654 ?
O1 K1 H5 62.0 . . ?
O9 K1 O1 103.81(12) . . ?
O9 K1 O4 77.81(13) . 2_655 ?
O9 K1 O3 141.61(13) . 3_665 ?
O9 K1 O2W 160.55(13) . . ?
O9 K1 O2W 86.95(13) . 3_665 ?
O9 K1 O1W 75.67(14) . . ?
O9 K1 C7 76.17(15) . 2_654 ?
O9 K1 C8 71.02(13) . 2_654 ?
O9 K1 H5 64.3 . . ?
O4 K1 C8 118.15(15) 2_655 2_654 ?
O4 K1 H5 89.4 2_655 . ?
O3 K1 O4 83.31(13) 3_665 2_655 ?
O3 K1 C7 134.60(15) 3_665 2_654 ?
O3 K1 C8 146.75(14) 3_665 2_654 ?
O3 K1 H5 82.5 3_665 . ?
O2W K1 O1 73.15(13) . . ?
O2W K1 O4 63.53(12) 3_665 2_655 ?
O2W K1 O4 115.96(14) . 2_655 ?
O2W K1 O3 57.04(13) . 3_665 ?
O2W K1 O3 54.67(13) 3_665 3_665 ?
O2W K1 O2W 111.18(14) . 3_665 ?
O2W K1 C7 84.77(14) . 2_654 ?
O2W K1 C7 143.52(14) 3_665 2_654 ?
O2W K1 C8 156.12(14) 3_665 2_654 ?
O2W K1 C8 89.88(14) . 2_654 ?
O2W K1 H5 37.9 3_665 . ?
O2W K1 H5 126.3 . . ?
O1W K1 O1 160.19(14) . . ?
O1W K1 O4 54.45(14) . 2_655 ?
O1W K1 O3 118.67(15) . 3_665 ?
O1W K1 O2W 100.58(15) . . ?
O1W K1 O2W 117.69(14) . 3_665 ?
O1W K1 C7 89.44(15) . 2_654 ?
O1W K1 C8 66.57(15) . 2_654 ?
O1W K1 H5 131.2 . . ?
C7 K1 O4 139.77(15) 2_654 2_655 ?
C7 K1 C8 22.88(15) 2_654 2_654 ?
C7 K1 H5 106.0 2_654 . ?
C8 K1 H5 120.1 2_654 . ?
V1 O5 H5 119.4 . . ?
V3 O5 V1 124.93(18) . . ?
V3 O5 H5 115.6 . . ?
V1 O6 V2 124.82(18) . . ?
V1 O6 H6 111.5 . . ?
V2 O6 H6 123.5 . . ?
V1 O1 K1 110.39(15) . . ?
C4 O1 V1 117.6(4) . . ?
C4 O1 K1 130.8(4) . . ?
V3 O9 K1 109.88(16) . . ?
C9 O9 V3 118.0(4) . . ?
C9 O9 K1 130.9(4) . . ?
C5 O2 V1 118.4(4) . . ?
C5 O4 K1 160.4(4) . 3_664 ?
C10 O7 V2 115.5(8) . . ?
C4 O3 K1 170.1(4) . 2_654 ?
K1 O2W K1 159.8(2) . 2_654 ?
N1 N2 V3 119.3(3) . . ?
C3 N2 V3 132.4(4) . . ?
C3 N2 N1 107.8(5) . . ?
N3 N4 V2 119.3(3) . . ?
C8 N4 V2 132.3(4) . . ?
C8 N4 N3 108.3(5) . . ?
N4 N3 V1 119.9(3) . . ?
C6 N3 V1 132.4(4) . . ?
C6 N3 N4 107.7(4) . . ?
N2 N1 V1 120.6(3) . . ?
C1 N1 V1 132.0(4) . . ?
C1 N1 N2 107.3(5) . . ?
O1 C4 C5 114.3(5) . . ?
O3 C4 O1 125.9(6) . . ?
O3 C4 C5 119.8(5) . . ?
N3 C6 H6A 125.2 . . ?
N3 C6 C7 109.5(5) . . ?
C7 C6 H6A 125.2 . . ?
K1 C7 H7 85.6 3_665 . ?
C6 C7 K1 94.6(4) . 3_665 ?
C6 C7 H7 127.7 . . ?
C8 C7 K1 90.7(4) . 3_665 ?
C8 C7 C6 104.6(5) . . ?
C8 C7 H7 127.7 . . ?
O2 C5 C4 111.9(4) . . ?
O4 C5 O2 127.3(6) . . ?
O4 C5 C4 120.9(5) . . ?
O9 C9 C9 113.2(3) . 5_556 ?
O10 C9 O9 125.7(6) . . ?
O10 C9 C9 121.0(4) . 5_556 ?
K1 C8 H8 99.8 3_665 . ?
N4 C8 K1 101.8(4) . 3_665 ?
N4 C8 C7 109.8(5) . . ?
N4 C8 H8 125.1 . . ?
C7 C8 K1 66.4(3) . 3_665 ?
C7 C8 H8 125.1 . . ?
H5A N5 H5B 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5A N5 H5D 109.5 . . ?
H5B N5 H5C 109.5 . . ?
H5B N5 H5D 109.5 . . ?
H5C N5 H5D 109.5 . . ?
C1 C2 H2 127.4 . . ?
C1 C2 C3 105.1(5) . . ?
C3 C2 H2 127.4 . . ?
N1 C1 C2 111.0(6) . . ?
N1 C1 H1 124.5 . . ?
C2 C1 H1 124.5 . . ?
N2 C3 C2 108.8(6) . . ?
N2 C3 H3 125.6 . . ?
C2 C3 H3 125.6 . . ?
O7 C10 C10 115.1(7) . 5_556 ?
O8 C10 O7 127.1(13) . . ?
O8 C10 C10 117.8(9) . 5_556 ?

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 C4 O3 173.1(4) . . . . ?
V1 O1 C4 C5 -8.1(6) . . . . ?
V1 O2 C5 O4 177.1(5) . . . . ?
V1 O2 C5 C4 -2.8(6) . . . . ?
V1 N3 C6 C7 -178.9(4) . . . . ?
V1 N1 C1 C2 -177.9(5) . . . . ?
V3 O9 C9 O10 178.9(6) . . . . ?
V3 O9 C9 C9 0.3(9) . . . 5_556 ?
V3 N2 N1 V1 5.3(5) . . . . ?
V3 N2 N1 C1 -172.3(4) . . . . ?
V3 N2 C3 C2 171.4(5) . . . . ?
V2 O7 C10 C10 1.7(18) . . . 5_556 ?
V2 O7 C10 O8 -176.5(11) . . . . ?
V2 N4 N3 V1 2.7(5) . . . . ?
V2 N4 N3 C6 -176.1(3) . . . . ?
V2 N4 C8 K1 106.5(4) . . . 3_665 ?
V2 N4 C8 C7 175.5(4) . . . . ?
K1 O1 C4 O3 -21.0(8) . . . . ?
K1 O1 C4 C5 157.8(3) . . . . ?
K1 O9 C9 O10 13.2(10) . . . . ?
K1 O9 C9 C9 -165.4(5) . . . 5_556 ?
K1 O4 C5 O2 -154.8(9) 3_664 . . . ?
K1 O4 C5 C4 25.1(15) 3_664 . . . ?
K1 C7 C8 N4 -94.6(5) 3_665 . . . ?
O1 C4 C5 O2 7.1(7) . . . . ?
O1 C4 C5 O4 -172.8(5) . . . . ?
O3 C4 C5 O2 -174.0(5) . . . . ?
O3 C4 C5 O4 6.1(8) . . . . ?
N2 N1 C1 C2 -0.7(7) . . . . ?
N4 N3 C6 C7 -0.3(6) . . . . ?
N3 N4 C8 K1 -69.5(4) . . . 3_665 ?
N3 N4 C8 C7 -0.6(7) . . . . ?
N3 C6 C7 K1 91.8(4) . . . 3_665 ?
N3 C6 C7 C8 -0.1(7) . . . . ?
N1 N2 C3 C2 0.1(7) . . . . ?
C6 C7 C8 K1 95.0(4) . . . 3_665 ?
C6 C7 C8 N4 0.4(7) . . . . ?
C8 N4 N3 V1 179.4(4) . . . . ?
C8 N4 N3 C6 0.5(6) . . . . ?
C1 C2 C3 N2 -0.5(8) . . . . ?
C3 N2 N1 V1 178.0(4) . . . . ?
C3 N2 N1 C1 0.4(6) . . . . ?
C3 C2 C1 N1 0.7(9) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.060 435.5 155.0 '15 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
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.982(11)
2 0.018(11)

####################################################################### 
# 
# 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_246_auto
_database_code_depnum_ccdc_archive 'CCDC 2154371'
loop_
_audit_author_name
_audit_author_address
'Zhao-Hui Zhou'
;Xiamen University
China
;
_audit_update_record             
;
2022-02-24 deposited with the CCDC.	2022-07-01 downloaded from the CCDC.
;
_audit_creation_date             2022-02-09
_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         'C24 H24 N8 Na2 O21 V4, 2(H2 N)'
_chemical_formula_sum            'C24 H40 N10 Na2 O27 V4'
_chemical_formula_weight         1150.40
_chemical_absolute_configuration ?
_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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 '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      orthorhombic
_space_group_IT_number           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   12.6075(5)
_cell_length_b                   19.6716(6)
_cell_length_c                   19.2268(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4768.4(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4521
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      72.9670
_cell_measurement_theta_min      4.1390
_shelx_estimated_absorpt_T_max   0.708
_shelx_estimated_absorpt_T_min   0.524
_exptl_absorpt_coefficient_mu    7.416
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (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 violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9530
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        66.989
_diffrn_reflns_theta_max         66.989
_diffrn_reflns_theta_min         4.165
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     39.00  71.00   0.50    2.00    --  105.19 -61.00-150.00   64
  2  ω     44.00  71.00   0.50    2.00    --  105.19 -61.00 -90.00   54
  3  ω     33.00  58.00   0.50    2.00    --  105.19 -61.00 -30.00   50
  4  ω     33.00  58.00   0.50    2.00    --  105.19 -61.00  30.00   50
  5  ω    -25.00  27.00   0.50    0.50    --   47.87 -19.00 -30.00  104
  6  ω     42.00  68.00   0.50    2.00    --  105.19 -61.00 120.00   52
  7  ω    104.00 168.00   0.50    2.00    --  105.19  45.00  30.00  128
  8  ω   -155.00-107.00   0.50    2.00    --  -99.00 -47.00 143.00   96
  9  ω   -119.00 -46.00   0.50    0.50    --  -47.87 -47.00 143.00  146
 10  ω   -105.00 -74.00   0.50    0.50    --  -47.87-125.00  90.00   62
 11  ω   -108.00 -75.00   0.50    0.50    --  -47.87-125.00 -60.00   66
 12  ω   -104.00 -29.00   0.50    2.00    --  -99.00 120.00 159.00  150
 13  ω    -68.00 -42.00   0.50    2.00    --  -99.00  61.00 150.00   52
 14  ω    -88.00 -27.00   0.50    2.00    --  -99.00  74.00  87.00  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.701
_reflns_Friedel_fraction_full    0.873
_reflns_Friedel_fraction_max     0.872
_reflns_number_gt                3577
_reflns_number_total             4005
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (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         1.719
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.092(19)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4005
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0736
_refine_ls_restrained_S_all      1.048
_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)+(0.1590P)²+3.4443P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2013
_refine_ls_wR_factor_ref         0.2087
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.908(19)
 0.092(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O10-H10
 0.85 with sigma of 0.02
 H5-O5
 0.85 with sigma of 0.02
 H5-V1
 2.45 with sigma of 0.02
 V2-H5
 2.45 with sigma of 0.02
 H10-H10_$3
 3.1 with sigma of 0.02
 H5_$3-H5
 3.1 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: O1W(0.5)
6.a Riding coordinates:
 N5(H5A,H5B)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C1(H1), C2(H2), C9(H9)
6.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V 0.25098(10) 0.50656(6) 0.37416(7) 0.0352(4) Uani 1 1 d D . . . .
V1 V 0.24619(11) 0.37626(7) 0.49244(6) 0.0354(4) Uani 1 1 d D . . . .
Na1 Na -0.0300(3) 0.1514(2) 0.36222(19) 0.0495(9) Uani 1 1 d . . . . .
O10 O 0.3213(6) 0.5634(3) 0.4437(3) 0.0382(13) Uani 1 1 d D . . . .
O5 O 0.1760(5) 0.4406(3) 0.4322(3) 0.0378(13) Uani 1 1 d D . . . .
O7 O 0.3296(6) 0.5565(3) 0.2978(3) 0.0456(15) Uani 1 1 d . . . . .
O2 O 0.1702(6) 0.2979(3) 0.4444(3) 0.0443(15) Uani 1 1 d . . . . .
O6 O 0.1807(6) 0.4691(4) 0.2853(3) 0.0490(16) Uani 1 1 d . . . . .
O1 O 0.3181(6) 0.2925(3) 0.5347(3) 0.0472(15) Uani 1 1 d . . . . .
N4 N 0.1239(6) 0.6213(3) 0.4339(3) 0.0357(15) Uani 1 1 d . . . . .
N1 N 0.3747(6) 0.4351(4) 0.3760(3) 0.0365(15) Uani 1 1 d . . . . .
N2 N 0.3707(6) 0.3817(3) 0.4204(4) 0.0355(15) Uani 1 1 d . . . . .
N3 N 0.1263(6) 0.5769(3) 0.3817(4) 0.0343(14) Uani 1 1 d . . . . .
O3 O 0.3178(7) 0.1800(4) 0.5357(5) 0.066(2) Uani 1 1 d . . . . .
O8 O 0.1766(8) 0.4823(5) 0.1701(4) 0.075(3) Uani 1 1 d . . . . .
O4 O 0.1470(7) 0.1856(4) 0.4448(5) 0.073(2) Uani 1 1 d . . . . .
C3 C 0.5232(8) 0.3734(5) 0.3604(5) 0.049(2) Uani 1 1 d . . . . .
O9 O 0.3479(9) 0.5711(5) 0.1827(4) 0.083(3) Uani 1 1 d . . . . .
C10 C -0.0172(7) 0.6435(5) 0.3648(5) 0.042(2) Uani 1 1 d . . . . .
C11 C 0.0386(7) 0.6615(4) 0.4255(5) 0.0387(18) Uani 1 1 d . . . . .
H11 H 0.018790 0.697078 0.456225 0.046 Uiso 1 1 calc R U . . .
C5 C 0.2829(8) 0.2343(5) 0.5153(5) 0.049(2) Uani 1 1 d . . . . .
C7 C 0.2143(9) 0.4954(5) 0.2263(5) 0.053(3) Uani 1 1 d . . . . .
C1 C 0.4590(7) 0.3448(4) 0.4108(5) 0.0410(19) Uani 1 1 d . . . . .
H1 H 0.475321 0.304296 0.435438 0.049 Uiso 1 1 calc R U . . .
C6 C 0.1930(8) 0.2374(5) 0.4641(5) 0.051(2) Uani 1 1 d . . . . .
C8 C 0.3068(9) 0.5444(6) 0.2353(5) 0.057(3) Uani 1 1 d . . . . .
C2 C 0.4654(8) 0.4301(5) 0.3412(5) 0.043(2) Uani 1 1 d . . . . .
H2 H 0.487998 0.461865 0.307065 0.052 Uiso 1 1 calc R U . . .
C9 C 0.0427(7) 0.5883(5) 0.3412(4) 0.0407(19) Uani 1 1 d . . . . .
H9 H 0.025682 0.562178 0.301183 0.049 Uiso 1 1 calc R U . . .
C12 C -0.1127(9) 0.6754(5) 0.3345(6) 0.051(2) Uani 1 1 d . . . . .
H12A H -0.176172 0.651875 0.351407 0.077 Uiso 1 1 calc R U . . .
H12B H -0.109637 0.672273 0.283665 0.077 Uiso 1 1 calc R U . . .
H12C H -0.115676 0.723332 0.348343 0.077 Uiso 1 1 calc R U . . .
C4 C 0.6245(10) 0.3475(7) 0.3322(7) 0.070(3) Uani 1 1 d . . . . .
H4A H 0.682822 0.376669 0.347832 0.105 Uiso 1 1 calc R U . . .
H4B H 0.621594 0.347527 0.281296 0.105 Uiso 1 1 calc R U . . .
H4C H 0.636343 0.300973 0.348866 0.105 Uiso 1 1 calc R U . . .
N5 N -0.0372(9) 0.4526(8) 0.4452(7) 0.103(5) Uani 1 1 d . . . . .
H5A H -0.067308 0.454191 0.402239 0.124 Uiso 1 1 d R U . . .
H5B H -0.062798 0.416061 0.468899 0.124 Uiso 1 1 d R U . . .
H10 H 0.386(3) 0.554(4) 0.441(4) 0.06(4) Uiso 1 1 d D . . . .
H5 H 0.1104(16) 0.4488(12) 0.4388(11) 0.07(4) Uiso 1 1 d D . . . .
O1W O 0.5332(14) 0.5556(13) 0.4572(15) 0.119(8) Uani 0.5 1 d . 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
V2 O10 1.955(6) . ?
V2 O5 1.955(6) . ?
V2 O7 2.026(6) . ?
V2 O6 2.061(6) . ?
V2 N1 2.100(7) . ?
V2 N3 2.099(7) . ?
V1 O10 1.953(6) 4_566 ?
V1 O5 1.931(6) . ?
V1 O2 2.036(6) . ?
V1 O1 2.048(7) . ?
V1 N4 2.094(7) 4_566 ?
V1 N2 2.096(7) . ?
Na1 O7 2.855(8) 5_445 ?
Na1 O1 2.969(8) 8_456 ?
Na1 O4 2.820(10) . ?
Na1 O1W 2.74(3) 5_445 ?
O10 H10 0.84(3) . ?
O5 H5 0.852(19) . ?
O7 C8 1.258(12) . ?
O2 C6 1.282(12) . ?
O6 C7 1.315(13) . ?
O1 C5 1.284(13) . ?
N4 N3 1.331(10) . ?
N4 C11 1.343(11) . ?
N1 N2 1.354(10) . ?
N1 C2 1.328(12) . ?
N2 C1 1.343(11) . ?
N3 C9 1.330(11) . ?
O3 C5 1.219(12) . ?
O8 C7 1.209(12) . ?
O4 C6 1.229(13) . ?
C3 C1 1.381(13) . ?
C3 C2 1.383(14) . ?
C3 C4 1.478(15) . ?
O9 C8 1.253(14) . ?
C10 C11 1.409(13) . ?
C10 C9 1.397(13) . ?
C10 C12 1.478(13) . ?
C11 H11 0.9500 . ?
C5 C6 1.503(17) . ?
C7 C8 1.523(18) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C9 H9 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N5 H5A 0.9101 . ?
N5 H5B 0.9102 . ?

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
O10 V2 O7 89.8(3) . . ?
O10 V2 O6 165.0(3) . . ?
O10 V2 N1 92.0(3) . . ?
O10 V2 N3 85.1(3) . . ?
O5 V2 O10 102.0(3) . . ?
O5 V2 O7 166.5(3) . . ?
O5 V2 O6 91.7(3) . . ?
O5 V2 N1 84.6(3) . . ?
O5 V2 N3 92.1(3) . . ?
O7 V2 O6 77.4(3) . . ?
O7 V2 N1 88.5(3) . . ?
O7 V2 N3 95.6(3) . . ?
O6 V2 N1 95.4(3) . . ?
O6 V2 N3 88.3(3) . . ?
N3 V2 N1 175.0(3) . . ?
O10 V1 O2 166.7(3) 4_566 . ?
O10 V1 O1 91.4(3) 4_566 . ?
O10 V1 N4 85.3(3) 4_566 4_566 ?
O10 V1 N2 91.2(3) 4_566 . ?
O5 V1 O10 101.6(3) . 4_566 ?
O5 V1 O2 90.5(3) . . ?
O5 V1 O1 165.5(3) . . ?
O5 V1 N4 93.0(3) . 4_566 ?
O5 V1 N2 85.0(3) . . ?
O2 V1 O1 77.2(3) . . ?
O2 V1 N4 88.7(3) . 4_566 ?
O2 V1 N2 95.3(3) . . ?
O1 V1 N4 94.4(3) . 4_566 ?
O1 V1 N2 88.4(3) . . ?
N4 V1 N2 175.6(3) 4_566 . ?
O7 Na1 O1 97.6(2) 5_445 8_456 ?
O4 Na1 O7 153.0(3) . 5_445 ?
O4 Na1 O1 92.6(2) . 8_456 ?
O1W Na1 O7 91.1(4) 5_445 5_445 ?
O1W Na1 O1 89.9(5) 5_445 8_456 ?
O1W Na1 O4 63.9(4) 5_445 . ?
V2 O10 Na1 104.9(2) . 5 ?
V2 O10 H10 106(8) . . ?
V1 O10 V2 123.9(4) 4_566 . ?
V1 O10 Na1 106.3(2) 4_566 5 ?
V1 O10 H10 130(8) 4_566 . ?
Na1 O10 H10 59(2) 5 . ?
V2 O5 H5 115.4(19) . . ?
V1 O5 V2 123.8(4) . . ?
V1 O5 H5 118.6(19) . . ?
V2 O7 Na1 107.8(3) . 5 ?
C8 O7 V2 119.2(7) . . ?
C8 O7 Na1 132.9(7) . 5 ?
C6 O2 V1 117.7(7) . . ?
C7 O6 V2 115.8(7) . . ?
V1 O1 Na1 104.6(3) . 8_556 ?
C5 O1 V1 116.7(6) . . ?
C5 O1 Na1 138.4(6) . 8_556 ?
N3 N4 V1 120.5(5) . 4_566 ?
N3 N4 C11 108.3(6) . . ?
C11 N4 V1 131.1(6) . 4_566 ?
N2 N1 V2 120.1(5) . . ?
C2 N1 V2 132.9(6) . . ?
C2 N1 N2 107.0(7) . . ?
N1 N2 V1 119.0(5) . . ?
C1 N2 V1 133.2(6) . . ?
C1 N2 N1 107.6(6) . . ?
N4 N3 V2 120.1(5) . . ?
C9 N3 V2 131.7(6) . . ?
C9 N3 N4 108.2(7) . . ?
C6 O4 Na1 137.8(8) . . ?
C1 C3 C2 101.9(8) . . ?
C1 C3 C4 128.5(10) . . ?
C2 C3 C4 129.5(10) . . ?
C8 O9 Na1 142.4(9) . 7 ?
C11 C10 C12 128.8(9) . . ?
C9 C10 C11 101.2(8) . . ?
C9 C10 C12 130.0(9) . . ?
N4 C11 C10 110.6(8) . . ?
N4 C11 H11 124.7 . . ?
C10 C11 H11 124.7 . . ?
O1 C5 C6 114.5(8) . . ?
O3 C5 O1 124.3(11) . . ?
O3 C5 C6 121.3(10) . . ?
O6 C7 C8 113.4(8) . . ?
O8 C7 O6 124.0(12) . . ?
O8 C7 C8 122.5(10) . . ?
N2 C1 C3 111.3(8) . . ?
N2 C1 H1 124.4 . . ?
C3 C1 H1 124.4 . . ?
O2 C6 C5 113.6(9) . . ?
O4 C6 O2 125.1(11) . . ?
O4 C6 C5 121.4(9) . . ?
O7 C8 C7 113.8(9) . . ?
O9 C8 O7 126.7(13) . . ?
O9 C8 C7 119.4(10) . . ?
N1 C2 C3 112.3(8) . . ?
N1 C2 H2 123.9 . . ?
C3 C2 H2 123.9 . . ?
N3 C9 C10 111.7(8) . . ?
N3 C9 H9 124.1 . . ?
C10 C9 H9 124.1 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
H5A N5 H5B 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V2 O7 C8 O9 179.9(9) . . . . ?
V2 O7 C8 C7 4.1(10) . . . . ?
V2 O6 C7 O8 -175.0(8) . . . . ?
V2 O6 C7 C8 5.2(9) . . . . ?
V2 N1 N2 V1 -5.1(8) . . . . ?
V2 N1 N2 C1 -179.8(6) . . . . ?
V2 N1 C2 C3 179.6(6) . . . . ?
V2 N3 C9 C10 -176.7(6) . . . . ?
V1 O2 C6 O4 172.9(8) . . . . ?
V1 O2 C6 C5 -6.3(10) . . . . ?
V1 O1 C5 O3 179.7(8) . . . . ?
V1 O1 C5 C6 -0.2(10) . . . . ?
V1 N4 N3 V2 1.8(8) 4_566 . . . ?
V1 N4 N3 C9 -177.1(6) 4_566 . . . ?
V1 N4 C11 C10 175.1(6) 4_566 . . . ?
V1 N2 C1 C3 -173.1(6) . . . . ?
Na1 O7 C8 O9 4.3(15) 5 . . . ?
Na1 O7 C8 C7 -171.5(5) 5 . . . ?
Na1 O1 C5 O3 -7.4(15) 8_556 . . . ?
Na1 O1 C5 C6 172.7(6) 8_556 . . . ?
Na1 O4 C6 O2 -4.9(17) . . . . ?
Na1 O4 C6 C5 174.3(7) . . . . ?
Na1 O9 C8 O7 14.9(19) 7 . . . ?
Na1 O9 C8 C7 -169.5(8) 7 . . . ?
O6 C7 C8 O7 -6.1(12) . . . . ?
O6 C7 C8 O9 177.8(9) . . . . ?
O1 C5 C6 O2 4.3(12) . . . . ?
O1 C5 C6 O4 -175.0(9) . . . . ?
N4 N3 C9 C10 2.0(10) . . . . ?
N1 N2 C1 C3 0.5(10) . . . . ?
N2 N1 C2 C3 0.9(11) . . . . ?
N3 N4 C11 C10 -0.6(10) . . . . ?
O3 C5 C6 O2 -175.7(8) . . . . ?
O3 C5 C6 O4 5.1(16) . . . . ?
O8 C7 C8 O7 174.1(9) . . . . ?
O8 C7 C8 O9 -2.0(15) . . . . ?
C11 N4 N3 V2 178.1(6) . . . . ?
C11 N4 N3 C9 -0.8(9) . . . . ?
C11 C10 C9 N3 -2.3(10) . . . . ?
C1 C3 C2 N1 -0.6(11) . . . . ?
C2 N1 N2 V1 173.9(6) . . . . ?
C2 N1 N2 C1 -0.8(9) . . . . ?
C2 C3 C1 N2 0.0(11) . . . . ?
C9 C10 C11 N4 1.7(10) . . . . ?
C12 C10 C11 N4 -177.7(10) . . . . ?
C12 C10 C9 N3 177.1(10) . . . . ?
C4 C3 C1 N2 -177.1(11) . . . . ?
C4 C3 C2 N1 176.5(11) . . . . ?

_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 0.309 0.250 143.1 43.1 '4 H2O'
2 0.000 0.691 0.750 143.1 42.5 '4 H2O'
3 0.249 0.000 0.500 50.0 19.0 '2 H2O'
4 0.251 0.500 1.000 50.0 19.1 '2 H2O'
5 0.500 0.191 0.750 143.1 42.5 '4 H2O'
6 0.500 0.809 0.250 143.1 43.1 '4 H2O'
7 0.751 0.000 0.000 50.0 19.1 '2 H2O'
8 0.749 0.500 0.500 50.0 19.0 '2 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
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.908(19)
2 0.092(19)

####################################################################### 
# 
# 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_590_auto
_database_code_depnum_ccdc_archive 'CCDC 2154372'
loop_
_audit_author_name
_audit_author_address
'Zhao-Hui Zhou'
;Xiamen University
China
;
_audit_update_record             
;
2022-04-23 deposited with the CCDC.	2022-07-01 downloaded from the CCDC.
;
_audit_creation_date             2022-04-15
_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         
'C24 H40.5 K2 N30 O34.5 V6, 2(Cl), 1(O), 24[H2O]'
_chemical_formula_sum            'C24 H88.50 Cl2 K2 N30 O59.50 V6'
_chemical_formula_weight         2204.48
_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'
Cl Cl 0.3639 0.7018 '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      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'

_cell_length_a                   21.03400(10)
_cell_length_b                   21.03400(10)
_cell_length_c                   21.03400(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9306.06(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8145
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.8830
_cell_measurement_theta_min      4.2250
_shelx_estimated_absorpt_T_max   0.714
_shelx_estimated_absorpt_T_min   0.532
_exptl_absorpt_coefficient_mu    7.211
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (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 violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4514
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12070
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.694
_diffrn_reflns_theta_min         3.640
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -105.00 -40.00   0.50    0.80    --  -99.00 112.00 -72.00  130
  2  ω    -67.00 -29.00   0.50    0.80    --  -99.00  61.00-180.00   76
  3  ω   -112.00 -87.00   0.50    0.20    --  -47.87-125.00 150.00   50
  4  ω     43.00  73.00   0.50    0.80    --  105.19 -61.00-150.00   60
  5  ω     78.00 112.00   0.50    0.20    --   47.87 140.00-143.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2861
_reflns_number_total             3071
_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 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (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         0.992
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00037(6)
_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   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3071
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0524
_refine_ls_restrained_S_all      1.069
_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)+(0.0994P)²+12.6637P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1597
_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) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.02
3. Others
 Fixed Sof: K1(0.33333) O1W(0.75) H1W(0.75) O2W(0.16667)
4.a Rotating group:
 O1W(H1W)
4.b Aromatic/amide H refined with riding coordinates:
 N3(H3)
4.c X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N4(H4A,H4B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.49762(2) 0.11661(2) 0.61517(2) 0.0211(2) Uani 1 1 d . . . . .
Cl1 Cl 0.42802(3) -0.07198(3) 0.57198(3) 0.0256(3) Uani 1 3 d S T P . .
O5 O 0.52719(9) 0.02962(9) 0.61940(9) 0.0215(4) Uani 1 1 d D . . . .
O2 O 0.51711(11) 0.13195(10) 0.70874(10) 0.0317(5) Uani 1 1 d . . . . .
O1 O 0.47444(11) 0.20983(10) 0.62511(10) 0.0324(5) Uani 1 1 d . . . . .
N2 N 0.63790(11) 0.09449(11) 0.58615(12) 0.0258(5) Uani 1 1 d . . . . .
O4 O 0.51569(15) 0.20536(14) 0.78572(13) 0.0547(8) Uani 1 1 d . . . . .
N1 N 0.58976(11) 0.14140(11) 0.58607(12) 0.0255(5) Uani 1 1 d . . . . .
N3 N 0.67271(14) 0.17871(13) 0.53566(15) 0.0407(7) Uani 1 1 d . . . . .
H3 H 0.697824 0.204605 0.514462 0.049 Uiso 1 1 calc R U . . .
N5 N 0.74196(14) 0.09016(16) 0.54217(18) 0.0496(8) Uani 1 1 d . . . . .
H5A H 0.748625 0.050796 0.554663 0.060 Uiso 1 1 calc R U . . .
H5B H 0.771662 0.110729 0.521073 0.060 Uiso 1 1 calc R U . . .
O3 O 0.4769(2) 0.29147(14) 0.69248(15) 0.0749(11) Uani 1 1 d . . . . .
N4 N 0.58233(16) 0.24557(14) 0.5432(2) 0.0566(10) Uani 1 1 d . . . . .
H4A H 0.543056 0.251183 0.556526 0.068 Uiso 1 1 calc R U . . .
H4B H 0.601789 0.275961 0.522065 0.068 Uiso 1 1 calc R U . . .
C2 C 0.50742(17) 0.18807(17) 0.73046(16) 0.0378(8) Uani 1 1 d . . . . .
C4 C 0.68678(15) 0.11868(15) 0.55521(17) 0.0334(7) Uani 1 1 d . . . . .
C3 C 0.61240(15) 0.19093(15) 0.55520(17) 0.0347(7) Uani 1 1 d . . . . .
C1 C 0.48420(19) 0.23478(17) 0.67969(17) 0.0422(8) Uani 1 1 d . . . . .
H5 H 0.4983(14) 0.0016(14) 0.6151(19) 0.032(11) Uiso 1 1 d D . . . .
K1 K 0.60792(15) 0.11939(14) 0.81655(14) 0.0586(8) Uani 0.3333 1 d . . P . .
O1W O 0.6698(4) 0.1801(4) 0.7132(3) 0.112(2) Uani 0.75 1 d . . P . .
H1W H 0.713386 0.163482 0.704437 0.168 Uiso 0.75 1 d R U P . .
O2W O 0.8110(4) 0.1890(4) 0.6890(4) 0.097(5) Uani 0.5 3 d S T 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 O5 1.9345(19) . ?
V1 O5 1.9382(19) 23_655 ?
V1 O2 2.036(2) . ?
V1 O1 2.031(2) . ?
V1 N2 2.096(2) 23_655 ?
V1 N1 2.098(2) . ?
O5 H5 0.852(19) . ?
O2 C2 1.282(4) . ?
O2 K1 2.977(3) . ?
O1 C1 1.279(4) . ?
O1 K1 3.011(3) 23_655 ?
N2 N1 1.414(3) . ?
N2 C4 1.319(4) . ?
O4 C2 1.230(4) . ?
O4 K1 2.730(4) . ?
N1 C3 1.317(4) . ?
N3 H3 0.8800 . ?
N3 C4 1.361(4) . ?
N3 C3 1.358(4) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N5 C4 1.335(4) . ?
O3 C1 1.232(4) . ?
O3 K1 2.747(5) 23_655 ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
N4 C3 1.336(5) . ?
C2 C1 1.531(5) . ?
C1 K1 3.160(5) 23_655 ?
K1 O1W 2.837(8) . ?
O1W H1W 0.9988 . ?

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
O5 V1 O5 99.64(11) . 23_655 ?
O5 V1 O2 167.87(9) 23_655 . ?
O5 V1 O2 92.34(8) . . ?
O5 V1 O1 170.20(9) . . ?
O5 V1 O1 89.89(8) 23_655 . ?
O5 V1 N2 87.35(9) 23_655 23_655 ?
O5 V1 N2 89.86(9) . 23_655 ?
O5 V1 N1 89.25(9) 23_655 . ?
O5 V1 N1 87.22(9) . . ?
O2 V1 N2 90.81(9) . 23_655 ?
O2 V1 N1 93.25(10) . . ?
O1 V1 O2 78.22(9) . . ?
O1 V1 N2 92.85(10) . 23_655 ?
O1 V1 N1 90.68(9) . . ?
N2 V1 N1 175.10(10) 23_655 . ?
V1 O5 V1 125.82(10) . 20_566 ?
V1 O5 H5 115(3) . . ?
V1 O5 H5 118(3) 20_566 . ?
V1 O2 K1 148.38(11) . . ?
C2 O2 V1 117.3(2) . . ?
C2 O2 K1 84.97(19) . . ?
V1 O1 K1 149.85(12) . 23_655 ?
C1 O1 V1 116.7(2) . . ?
C1 O1 K1 84.7(2) . 23_655 ?
N1 N2 V1 118.83(17) . 20_566 ?
C4 N2 V1 133.3(2) . 20_566 ?
C4 N2 N1 106.8(2) . . ?
C2 O4 K1 97.4(2) . . ?
N2 N1 V1 119.19(17) . . ?
C3 N1 V1 132.4(2) . . ?
C3 N1 N2 107.1(2) . . ?
C4 N3 H3 126.7 . . ?
C3 N3 H3 126.7 . . ?
C3 N3 C4 106.7(3) . . ?
H5A N5 H5B 120.0 . . ?
C4 N5 H5A 120.0 . . ?
C4 N5 H5B 120.0 . . ?
C1 O3 K1 97.8(3) . 23_655 ?
H4A N4 H4B 120.0 . . ?
C3 N4 H4A 120.0 . . ?
C3 N4 H4B 120.0 . . ?
O2 C2 C1 113.1(3) . . ?
O4 C2 O2 125.9(3) . . ?
O4 C2 C1 121.0(3) . . ?
N2 C4 N3 109.7(3) . . ?
N2 C4 N5 127.3(3) . . ?
N5 C4 N3 123.0(3) . . ?
N1 C3 N3 109.7(3) . . ?
N1 C3 N4 127.0(3) . . ?
N4 C3 N3 123.2(3) . . ?
O1 C1 C2 114.5(3) . . ?
O1 C1 K1 71.6(2) . 23_655 ?
O3 C1 O1 125.0(4) . . ?
O3 C1 C2 120.6(3) . . ?
O3 C1 K1 59.4(2) . 23_655 ?
C2 C1 K1 154.5(3) . 23_655 ?
O2 K1 O1 64.36(8) . 20_566 ?
O2 K1 C1 87.31(10) . 20_566 ?
O1 K1 C1 23.76(8) 20_566 20_566 ?
O4 K1 O2 45.92(8) . . ?
O4 K1 O1 110.02(11) . 20_566 ?
O4 K1 O3 154.55(14) . 20_566 ?
O4 K1 C1 131.82(13) . 20_566 ?
O4 K1 O1W 81.1(2) . . ?
O3 K1 O2 109.56(11) 20_566 . ?
O3 K1 O1 45.23(8) 20_566 20_566 ?
O3 K1 C1 22.73(9) 20_566 20_566 ?
O3 K1 O1W 83.5(2) 20_566 . ?
O1W K1 O2 70.76(16) . . ?
O1W K1 O1 70.63(15) . 20_566 ?
O1W K1 C1 70.97(19) . 20_566 ?
K1 O1W H1W 113.9 . . ?

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 O2 C2 O4 178.8(3) . . . . ?
V1 O2 C2 C1 -1.8(4) . . . . ?
V1 O1 C1 O3 174.8(4) . . . . ?
V1 O1 C1 C2 -4.4(4) . . . . ?
V1 O1 C1 K1 -157.7(2) . . . 23_655 ?
V1 N2 N1 V1 -0.8(3) 20_566 . . . ?
V1 N2 N1 C3 -169.4(2) 20_566 . . . ?
V1 N2 C4 N3 167.5(2) 20_566 . . . ?
V1 N2 C4 N5 -10.7(5) 20_566 . . . ?
V1 N1 C3 N3 -166.8(2) . . . . ?
V1 N1 C3 N4 12.6(6) . . . . ?
O2 C2 C1 O1 4.1(5) . . . . ?
O2 C2 C1 O3 -175.2(4) . . . . ?
O2 C2 C1 K1 102.5(5) . . . 23_655 ?
N2 N1 C3 N3 -0.4(4) . . . . ?
N2 N1 C3 N4 179.1(4) . . . . ?
O4 C2 C1 O1 -176.5(4) . . . . ?
O4 C2 C1 O3 4.2(6) . . . . ?
O4 C2 C1 K1 -78.1(7) . . . 23_655 ?
N1 N2 C4 N3 0.4(3) . . . . ?
N1 N2 C4 N5 -177.8(3) . . . . ?
C4 N2 N1 V1 168.5(2) . . . . ?
C4 N2 N1 C3 0.0(3) . . . . ?
C4 N3 C3 N1 0.6(4) . . . . ?
C4 N3 C3 N4 -178.9(4) . . . . ?
C3 N3 C4 N2 -0.6(4) . . . . ?
C3 N3 C4 N5 177.7(3) . . . . ?
K1 O2 C2 O4 -24.8(4) . . . . ?
K1 O2 C2 C1 154.6(3) . . . . ?
K1 O1 C1 O3 -27.5(5) 23_655 . . . ?
K1 O1 C1 C2 153.3(3) 23_655 . . . ?
K1 O4 C2 O2 27.3(4) . . . . ?
K1 O4 C2 C1 -152.0(3) . . . . ?
K1 O3 C1 O1 30.5(5) 23_655 . . . ?
K1 O3 C1 C2 -150.3(3) 23_655 . . . ?

_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 -0.412 -0.484 0.073 2724.8 957.0 '96 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
;
####################################################################### 
# 
# 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_243_auto
_database_code_depnum_ccdc_archive 'CCDC 2154373'
loop_
_audit_author_name
_audit_author_address
'Zhao-Hui Zhou'
;Xiamen University
China
;
_audit_update_record             
;
2022-06-26 deposited with the CCDC.	2022-07-01 downloaded from the CCDC.
;
_audit_creation_date             2022-05-17
_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         'C16 H48 N40 O32 S8 V8, 38[H2O]'
_chemical_formula_sum            'C16 H124 N40 O70 S8 V8'
_chemical_formula_weight         2661.54
_chemical_absolute_configuration ?
_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'
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'
S S 0.3331 0.5567 '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      tetragonal
_space_group_IT_number           104
_space_group_name_H-M_alt        'P 4 n c'
_space_group_name_Hall           'P 4 -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   17.54950(10)
_cell_length_b                   17.54950(10)
_cell_length_c                   15.90610(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4898.84(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    37475
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9300
_cell_measurement_theta_min      3.5290
_shelx_estimated_absorpt_T_max   0.665
_shelx_estimated_absorpt_T_min   0.470
_exptl_absorpt_coefficient_mu    8.879
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (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 violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            69024
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.116
_diffrn_reflns_theta_min         3.562
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -85.00 -13.00   0.50    0.30    --  -47.87 113.00  66.00  144
  2  ω     28.00  54.00   0.50    0.30    --   47.87-113.00 -25.00   52
  3  ω   -102.00 -49.00   0.50    1.30    --  -99.00 113.00  66.00  106
  4  ω   -129.00-103.00   0.50    1.30    --  -99.00-113.00 -25.00   52
  5  ω    107.00 132.00   0.50    1.30    --  105.19 113.00  66.00   50
  6  ω     36.00 109.00   0.50    1.30    --  105.19-113.00 -25.00  146
  7  ω     -8.00  26.00   0.50    0.30    --  -47.87  19.00  60.00   68
  8  ω   -113.00 -76.00   0.50    0.30    --  -47.87-125.00-150.00   74
  9  ω    -22.00  22.00   0.50    0.30    --  -47.87  19.00 -30.00   88
 10  ω   -120.00 -92.00   0.50    0.30    --  -47.87-125.00  90.00   56
 11  ω     26.00 120.00   0.50    0.30    --   47.87  77.00-180.00  188
 12  ω     17.00  43.00   0.50    0.30    --   47.87 -38.00  60.00   52
 13  ω    -12.00  13.00   0.50    0.30    --   47.87 -38.00  60.00   50
 14  ω    -15.00  69.00   0.50    0.30    --   47.87 -77.00  60.00  168
 15  ω    -66.00 -40.00   0.50    1.30    --  -99.00  61.00 150.00   52
 16  ω    -58.00 -27.00   0.50    1.30    --  -99.00  61.00  60.00   62
 17  ω   -107.00 -29.00   0.50    1.30    --  -99.00 108.00 115.76  156
 18  ω   -166.00-139.00   0.50    1.30    --  -99.00 -95.00  30.00   54
 19  ω    -90.00 -38.00   0.50    1.30    --  -99.00  77.00  30.00  104
 20  ω   -170.00 -92.00   0.50    1.30    --  -99.00 -45.00-180.00  156
 21  ω    -57.00 -29.00   0.50    1.30    --  -99.00 112.00 153.94   56
 22  ω   -126.00 -74.00   0.50    1.30    --  -99.00 144.00 -33.66  104
 23  ω   -122.00 -96.00   0.50    1.30    --  -99.00 -61.00  60.00   52
 24  ω   -126.00 -99.00   0.50    1.30    --  -99.00 -95.00  30.00   54
 25  ω   -165.00-129.00   0.50    1.30    --  -99.00 -61.00  60.00   72
 26  ω    -67.00 -27.00   0.50    1.30    --  -99.00  61.00  90.00   80
 27  ω   -120.00 -27.00   0.50    1.30    --  -99.00 142.00   9.43  186
 28  ω   -108.00 -70.00   0.50    1.30    --  -99.00 112.00 153.94   76
 29  ω     67.00 101.00   0.50    1.30    --  105.19 -95.00-150.00   68
 30  ω     33.00  68.00   0.50    1.30    --  105.19 -61.00-120.00   70
 31  ω     57.00  82.00   0.50    1.30    --  105.19-125.00-180.00   50
 32  ω     46.00 111.00   0.50    1.30    --  105.19-125.00 -30.00  130
 33  ω     95.00 176.00   0.50    1.30    --  105.19  45.00   0.00  162
 34  ω    112.00 177.00   0.50    1.30    --  105.19  30.00-120.00  130
 35  ω     38.00  99.00   0.50    1.30    --  105.19 -95.00   0.00  122
 36  ω     34.00  64.00   0.50    1.30    --  105.19 -61.00 -60.00   60
 37  ω     45.00  71.00   0.50    1.30    --  105.19 -61.00-150.00   52
 38  ω     38.00  64.00   0.50    1.30    --  105.19 -61.00  90.00   52
 39  ω     47.00  72.00   0.50    1.30    --  105.19 -61.00  60.00   50
 40  ω     33.00  73.00   0.50    1.30    --  105.19 -61.00-180.00   80
 41  ω     41.00  91.00   0.50    1.30    --  105.19 -95.00-180.00  100
 42  ω     40.00  65.00   0.50    1.30    --  105.19-125.00  30.00   50
 43  ω     94.00 177.00   0.50    1.30    --  105.19  45.00  90.00  166
 44  ω     65.00 112.00   0.50    1.30    --  105.19-125.00-120.00   94
 45  ω     67.00 112.00   0.50    1.30    --  105.19-125.00 -60.00   90
 46  ω    120.00 173.00   0.50    1.30    --  105.19  45.00 -90.00  106
 47  ω     54.00  80.00   0.50    1.30    --  105.19 -95.00-120.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.942
_reflns_number_gt                4951
_reflns_number_total             5037
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (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         0.417
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.109(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5037
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0477
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0708P)²+11.8394P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1292
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.891(10)
 0.109(10)
2. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
3. Restrained distances
 O2-H2
 0.85 with sigma of 0.02
 O1-H1
 0.85 with sigma of 0.02
 V1-H1
 2.5 with sigma of 0.02
 V2_$2-H1
 2.5 with sigma of 0.02
 V1-H1 \\sim V2_$2-H1
 with sigma of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N8(H8)
4.b X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N10(H10A,H10B), N4(H4A,H4B), N9(H9A,H9B)
;
_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 0.43914(5) 0.24957(5) 0.49921(8) 0.0243(2) Uani 1 1 d . . . . .
V1 V 0.28500(5) 0.36983(5) 0.49492(7) 0.0255(2) Uani 1 1 d D . . . .
S1 S 0.26862(8) 0.19091(8) 0.46835(10) 0.0280(3) Uani 1 1 d . . . . .
S2 S 0.55781(8) 0.11185(8) 0.53568(12) 0.0313(3) Uani 1 1 d . . . . .
O1 O 0.3070(2) 0.4714(2) 0.5374(3) 0.0238(8) Uani 1 1 d D . . . .
O2 O 0.3888(2) 0.3435(2) 0.4580(3) 0.0255(8) Uani 1 1 d D . . . .
O6 O 0.4814(2) 0.1547(2) 0.5489(3) 0.0340(10) Uani 1 1 d . . . . .
O5 O 0.2333(3) 0.1411(2) 0.4024(3) 0.0322(9) Uani 1 1 d . . . . .
O4 O 0.3548(2) 0.1857(2) 0.4472(3) 0.0306(9) Uani 1 1 d . . . . .
O3 O 0.2486(2) 0.2728(2) 0.4382(3) 0.0325(10) Uani 1 1 d . . . . .
N7 N 0.2362(3) 0.5011(3) 0.3818(3) 0.0282(10) Uani 1 1 d . . . . .
O8 O 0.6175(3) 0.1748(2) 0.5271(3) 0.0362(10) Uani 1 1 d . . . . .
N1 N 0.3116(3) 0.3154(3) 0.6052(3) 0.0262(10) Uani 1 1 d . . . . .
O7 O 0.5718(3) 0.0778(3) 0.6188(4) 0.0442(12) Uani 1 1 d . . . . .
N6 N 0.2668(3) 0.4264(3) 0.3786(3) 0.0279(10) Uani 1 1 d . . . . .
N3 N 0.3351(3) 0.2848(3) 0.7360(3) 0.0309(11) Uani 1 1 d . . . . .
H3 H 0.331143 0.282020 0.791111 0.037 Uiso 1 1 calc R U . . .
N2 N 0.3776(3) 0.2680(3) 0.6087(4) 0.0282(11) Uani 1 1 d . . . . .
N5 N 0.4464(3) 0.2086(3) 0.7193(4) 0.0361(13) Uani 1 1 d . . . . .
H5A H 0.480380 0.188652 0.685131 0.043 Uiso 1 1 calc R U . . .
H5B H 0.449679 0.200516 0.773809 0.043 Uiso 1 1 calc R U . . .
N10 N 0.1995(3) 0.5897(3) 0.2751(4) 0.0371(13) Uani 1 1 d . . . . .
H10A H 0.187107 0.625328 0.311532 0.045 Uiso 1 1 calc R U . . .
H10B H 0.194651 0.598308 0.220843 0.045 Uiso 1 1 calc R U . . .
N4 N 0.2269(4) 0.3631(4) 0.7086(4) 0.0483(16) Uani 1 1 d . . . . .
H4A H 0.198534 0.387077 0.671411 0.058 Uiso 1 1 calc R U . . .
H4B H 0.215138 0.365209 0.762322 0.058 Uiso 1 1 calc R U . . .
C4 C 0.2258(4) 0.5223(4) 0.3022(4) 0.0323(13) Uani 1 1 d . . . . .
C1 C 0.2878(4) 0.3232(4) 0.6834(4) 0.0325(13) Uani 1 1 d . . . . .
N8 N 0.2492(4) 0.4659(4) 0.2496(4) 0.0419(14) Uani 1 1 d . . . . .
H8 H 0.248145 0.466478 0.194335 0.050 Uiso 1 1 calc R U . . .
C3 C 0.2746(4) 0.4085(4) 0.2993(4) 0.0331(14) Uani 1 1 d . . . . .
N9 N 0.3057(4) 0.3431(4) 0.2693(5) 0.0549(19) Uani 1 1 d . . . . .
H9A H 0.322733 0.308300 0.304360 0.066 Uiso 1 1 calc R U . . .
H9B H 0.308843 0.335573 0.214682 0.066 Uiso 1 1 calc R U . . .
C2 C 0.3891(4) 0.2516(4) 0.6882(4) 0.0293(12) Uani 1 1 d . . . . .
H2 H 0.416(8) 0.377(7) 0.433(9) 0.13(6) Uiso 1 1 d D . . . .
H1 H 0.329(8) 0.4752(18) 0.587(6) 0.25(12) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V2 O1 1.963(4) 3_655 ?
V2 O2 1.982(4) . ?
V2 O6 1.987(4) . ?
V2 O4 2.033(4) . ?
V2 N7 2.154(5) 3_655 ?
V2 N2 2.075(6) . ?
V1 O1 1.944(4) . ?
V1 O2 1.970(4) . ?
V1 O3 2.030(4) . ?
V1 O8 2.012(4) 4_565 ?
V1 N1 2.052(5) . ?
V1 N6 2.124(6) . ?
S1 O5 1.500(4) . ?
S1 O4 1.553(5) . ?
S1 O3 1.555(5) . ?
S2 O6 1.552(4) . ?
S2 O8 1.529(5) . ?
S2 O7 1.471(6) . ?
O1 H1 0.88(3) . ?
O2 H2 0.85(3) . ?
N7 N6 1.419(7) . ?
N7 C4 1.332(9) . ?
N1 N2 1.427(7) . ?
N1 C1 1.319(8) . ?
N6 C3 1.306(9) . ?
N3 H3 0.8800 . ?
N3 C1 1.358(9) . ?
N3 C2 1.348(9) . ?
N2 C2 1.311(9) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N5 C2 1.352(8) . ?
N10 H10A 0.8800 . ?
N10 H10B 0.8800 . ?
N10 C4 1.342(9) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
N4 C1 1.340(9) . ?
C4 N8 1.359(9) . ?
N8 H8 0.8800 . ?
N8 C3 1.355(9) . ?
C3 N9 1.358(9) . ?
N9 H9A 0.8800 . ?
N9 H9B 0.8800 . ?

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 O2 91.81(16) 3_655 . ?
O1 V2 O6 90.51(18) 3_655 . ?
O1 V2 O4 172.69(19) 3_655 . ?
O1 V2 N7 86.28(19) 3_655 3_655 ?
O1 V2 N2 94.4(2) 3_655 . ?
O2 V2 O6 174.33(19) . . ?
O2 V2 O4 89.99(18) . . ?
O2 V2 N7 91.2(2) . 3_655 ?
O2 V2 N2 85.20(19) . . ?
O6 V2 O4 88.34(19) . . ?
O6 V2 N7 94.1(2) . 3_655 ?
O6 V2 N2 89.5(2) . . ?
O4 V2 N7 86.61(19) . 3_655 ?
O4 V2 N2 92.8(2) . . ?
N2 V2 N7 176.3(2) . 3_655 ?
O1 V1 O2 97.75(16) . . ?
O1 V1 O3 170.27(18) . . ?
O1 V1 O8 90.10(18) . 4_565 ?
O1 V1 N1 94.86(19) . . ?
O1 V1 N6 84.52(19) . . ?
O2 V1 O3 87.79(18) . . ?
O2 V1 O8 172.15(18) . 4_565 ?
O2 V1 N1 86.29(19) . . ?
O2 V1 N6 89.4(2) . . ?
O3 V1 N1 93.5(2) . . ?
O3 V1 N6 87.6(2) . . ?
O8 V1 O3 84.44(19) 4_565 . ?
O8 V1 N1 93.0(2) 4_565 . ?
O8 V1 N6 91.4(2) 4_565 . ?
N1 V1 N6 175.5(2) . . ?
O5 S1 O4 102.5(3) . . ?
O5 S1 O3 103.2(3) . . ?
O4 S1 O3 102.0(2) . . ?
O8 S2 O6 104.8(2) . . ?
O7 S2 O6 102.7(3) . . ?
O7 S2 O8 105.1(3) . . ?
V2 O1 H1 116(2) 4_565 . ?
V1 O1 V2 121.6(2) . 4_565 ?
V1 O1 H1 118(2) . . ?
V2 O2 H2 118(10) . . ?
V1 O2 V2 120.6(2) . . ?
V1 O2 H2 120(10) . . ?
S2 O6 V2 132.4(3) . . ?
S1 O4 V2 126.0(3) . . ?
S1 O3 V1 124.6(3) . . ?
N6 N7 V2 116.1(4) . 4_565 ?
C4 N7 V2 134.7(5) . 4_565 ?
C4 N7 N6 105.9(5) . . ?
S2 O8 V1 142.4(3) . 3_655 ?
N2 N1 V1 119.3(4) . . ?
C1 N1 V1 133.3(4) . . ?
C1 N1 N2 106.3(5) . . ?
N7 N6 V1 117.2(4) . . ?
C3 N6 V1 135.5(5) . . ?
C3 N6 N7 107.2(5) . . ?
C1 N3 H3 126.4 . . ?
C2 N3 H3 126.4 . . ?
C2 N3 C1 107.1(5) . . ?
N1 N2 V2 118.7(4) . . ?
C2 N2 V2 134.0(4) . . ?
C2 N2 N1 106.9(5) . . ?
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 . . ?
H4A N4 H4B 120.0 . . ?
C1 N4 H4A 120.0 . . ?
C1 N4 H4B 120.0 . . ?
N7 C4 N10 126.7(7) . . ?
N7 C4 N8 110.0(6) . . ?
N10 C4 N8 123.3(7) . . ?
N1 C1 N3 109.7(5) . . ?
N1 C1 N4 126.1(7) . . ?
N4 C1 N3 124.2(6) . . ?
C4 N8 H8 126.8 . . ?
C3 N8 C4 106.3(6) . . ?
C3 N8 H8 126.8 . . ?
N6 C3 N8 110.5(6) . . ?
N6 C3 N9 125.8(7) . . ?
N8 C3 N9 123.7(7) . . ?
C3 N9 H9A 120.0 . . ?
C3 N9 H9B 120.0 . . ?
H9A N9 H9B 120.0 . . ?
N3 C2 N5 123.8(6) . . ?
N2 C2 N3 110.0(6) . . ?
N2 C2 N5 126.1(6) . . ?

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 N7 N6 V1 21.0(5) 4_565 . . . ?
V2 N7 N6 C3 -161.1(4) 4_565 . . . ?
V2 N7 C4 N10 -20.4(11) 4_565 . . . ?
V2 N7 C4 N8 156.9(5) 4_565 . . . ?
V2 N2 C2 N3 172.5(4) . . . . ?
V2 N2 C2 N5 -6.9(11) . . . . ?
V1 N1 N2 V2 -4.8(6) . . . . ?
V1 N1 N2 C2 168.9(4) . . . . ?
V1 N1 C1 N3 -166.7(4) . . . . ?
V1 N1 C1 N4 13.0(11) . . . . ?
V1 N6 C3 N8 175.8(5) . . . . ?
V1 N6 C3 N9 -6.1(11) . . . . ?
O6 S2 O8 V1 -24.3(6) . . . 3_655 ?
O5 S1 O4 V2 171.0(3) . . . . ?
O5 S1 O3 V1 -175.9(3) . . . . ?
O4 S1 O3 V1 -69.8(4) . . . . ?
O3 S1 O4 V2 64.4(4) . . . . ?
N7 N6 C3 N8 -1.7(7) . . . . ?
N7 N6 C3 N9 176.5(7) . . . . ?
N7 C4 N8 C3 0.1(8) . . . . ?
O8 S2 O6 V2 38.7(5) . . . . ?
N1 N2 C2 N3 0.2(7) . . . . ?
N1 N2 C2 N5 -179.3(6) . . . . ?
O7 S2 O6 V2 148.2(4) . . . . ?
O7 S2 O8 V1 -132.1(5) . . . 3_655 ?
N6 N7 C4 N10 -178.3(6) . . . . ?
N6 N7 C4 N8 -1.0(7) . . . . ?
N2 N1 C1 N3 0.8(7) . . . . ?
N2 N1 C1 N4 -179.6(7) . . . . ?
N10 C4 N8 C3 177.5(7) . . . . ?
C4 N7 N6 V1 -176.3(4) . . . . ?
C4 N7 N6 C3 1.6(7) . . . . ?
C4 N8 C3 N6 1.0(8) . . . . ?
C4 N8 C3 N9 -177.2(7) . . . . ?
C1 N1 N2 V2 -174.4(4) . . . . ?
C1 N1 N2 C2 -0.6(6) . . . . ?
C1 N3 C2 N2 0.3(7) . . . . ?
C1 N3 C2 N5 179.8(6) . . . . ?
C2 N3 C1 N1 -0.7(7) . . . . ?
C2 N3 C1 N4 179.7(7) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.111 -0.270 -0.262 2162.7 759.7 '76 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
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.891(10)
2 0.109(10)

# start Validation Reply Form
_vrf_PLAT420_exp_243_auto        
;
PROBLEM:  D-H Bond Without Acceptor O1 --H1        
RESPONSE: The solvent molecules are highly disordered, which supposed to 
form hydrogen bond with water molecules have been removed by the SQUEEZE 
routine in the PLATON software package.
;
# end Validation Reply Form
