#------------------------------------------------------------------------------
#$Date: 2022-07-03 01:52:28 +0300 (Sun, 03 Jul 2022) $
#$Revision: 276501 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/06/7710670.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7710670
loop_
_publ_author_name
'Xie, Zhenlang'
'An, Dongli'
'Weng, Weizheng'
'Zhou, Zhao-Hui'
_publ_section_title
;
 Successive constructions of regular tetra-, hexa- and octanuclear
 microporous polyoxovanadates(III) for gas adsorptions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01360F
_journal_year                    2022
_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
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-02-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2022-02-24 deposited with the CCDC.	2022-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.11633(10)
_cell_length_b                   18.11633(10)
_cell_length_c                   11.42819(6)
_cell_measurement_reflns_used    42550
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.9090
_cell_measurement_theta_min      2.7940
_cell_volume                     3248.24(3)
_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)'
_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_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
_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_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_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
_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_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_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0472
_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
_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_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01360f2.cif
_cod_data_source_block           exp_607_auto
_cod_original_cell_volume        3248.24(4)
_cod_database_code               7710670
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_max   0.642
_shelx_estimated_absorpt_t_min   0.443
_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)
;
_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_
_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'
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 . . . .
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'
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_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_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) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.982(11)
2 0.018(11)
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'
