#------------------------------------------------------------------------------
#$Date: 2023-10-21 01:04:12 +0200 (Sat 21 de Oct de 2023) $
#$Revision: 287066 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/42/7714265.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_7714265
loop_
_publ_author_name
'Zhu, Shuang-Shuang'
'Xie, Zhenlang'
'Deng, Lan'
'Wang, Si-Yuan'
'Ni, Lubin'
'Zhou, Zhao-Hui'
_publ_section_title
;
 Protonated and deprotonated vanadyl imidazole tartrates for the mimics of
 the vanadium coordination in FeV-cofactor of V-nitrogenase
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02903D
_journal_year                    2023
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C22 H26 N12 O8 V2, 4(H2 O)'
_chemical_formula_sum            'C22 H34 N12 O12 V2'
_chemical_formula_weight         760.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-25 deposited with the CCDC.	2023-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.4050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.16620(10)
_cell_length_b                   13.61250(10)
_cell_length_c                   12.80470(10)
_cell_measurement_reflns_used    19341
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.4960
_cell_measurement_theta_min      4.5920
_cell_volume                     1671.35(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -56.00  24.00   0.50    0.10    --  -47.96  57.00  30.00  160
  2  ω    -59.00  25.00   0.50    0.10    --  -47.96  57.00 150.00  168
  3  ω    -60.00  22.00   0.50    0.10    --  -47.96  57.00 -90.00  164
  4  ω   -115.00 -85.00   0.50    0.10    --  -47.96-125.00 150.00   60
  5  ω     49.00  78.00   0.50    0.10    --   47.96  57.00 -30.00   58
  6  ω     80.00 120.00   0.50    0.10    --   47.96  57.00 -30.00   80
  7  ω     14.00  55.00   0.50    0.10    --   47.96 -19.00  30.00   82
  8  ω   -113.00 -87.00   0.50    0.39    --  -86.25 -94.00-120.00   52
  9  ω   -130.00 -91.00   0.50    0.39    --  -86.25-125.00  60.00   78
 10  ω     38.00  64.00   0.50    0.39    --  107.75-125.00-150.00   52
 11  ω     92.00 165.00   0.50    0.39    --  107.75  61.00-150.00  146
 12  ω     38.00 112.00   0.50    0.39    --  107.75 -77.00 150.00  148
 13  ω     35.00  65.00   0.50    0.39    --  107.75-125.00  90.00   60
 14  ω    115.00 167.00   0.50    0.39    --  107.75  15.00  90.00  104
 15  ω    102.00 170.00   0.50    0.39    --  107.75 125.00  90.00  136
 16  ω     83.00 109.00   0.50    0.39    --  107.75 -94.00   0.00   52
 17  ω     89.00 121.00   0.50    0.39    --  107.75 -15.00-120.00   64
 18  ω     37.00  63.00   0.50    0.39    --  107.75 -94.00   0.00   52
 19  ω     92.00 162.00   0.50    0.39    --  107.75 125.00  30.00  140
 20  ω     35.00  68.00   0.50    0.39    --  107.75 -61.00   0.00   66
 21  ω     77.00 122.00   0.50    0.39    --  107.75 -61.00   0.00   90
 22  ω     35.00 114.00   0.50    0.39    --  107.75 -30.00 150.00  158
 23  ω     35.00  65.00   0.50    0.39    --  107.75 -15.00-120.00   60
 24  ω     81.00 117.00   0.50    0.39    --  107.75-125.00-180.00   72
 25  ω     96.00 168.00   0.50    0.39    --  107.75  15.00 150.00  144
 26  ω     68.00 117.00   0.50    0.39    --  107.75-125.00   0.00   98
 27  ω     39.00  64.00   0.50    0.39    --  107.75-125.00-180.00   50
 28  ω     77.00 106.00   0.50    0.39    --  107.75-125.00  90.00   58
 29  ω     56.00  83.00   0.50    0.39    --  107.75-125.00 -30.00   54
 30  ω     92.00 121.00   0.50    0.39    --  107.75 125.00 120.00   58
 31  ω    136.00 174.00   0.50    0.39    --  107.75 125.00 120.00   76
 32  ω     38.00  81.00   0.50    0.39    --  107.75 -94.00-120.00   86
 33  ω     88.00 117.00   0.50    0.39    --  107.75-125.00 -30.00   58
 34  ω     77.00 102.00   0.50    0.39    --  107.75 -94.00  90.00   50
 35  ω    100.00 125.00   0.50    0.39    --  107.75  61.00-180.00   50
 36  ω    143.00 170.00   0.50    0.39    --  107.75  61.00-180.00   54
 37  ω     82.00 116.00   0.50    0.39    --  107.75-125.00-150.00   68
 38  ω     39.00  70.00   0.50    0.39    --  107.75 -94.00 150.00   62
 39  ω     83.00 116.00   0.50    0.39    --  107.75-125.00 -60.00   66
 40  ω     99.00 124.00   0.50    0.39    --  107.75  61.00 -60.00   50
 41  ω    148.00 173.00   0.50    0.39    --  107.75  61.00 -60.00   50
 42  ω     79.00 108.00   0.50    0.39    --  107.75 -94.00  60.00   58
 43  ω     45.00 121.00   0.50    0.39    --  107.75 -45.00   0.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0490683000
_diffrn_orient_matrix_UB_12      -0.1048780000
_diffrn_orient_matrix_UB_13      -0.0134726000
_diffrn_orient_matrix_UB_21      -0.1127018000
_diffrn_orient_matrix_UB_22      -0.0424005000
_diffrn_orient_matrix_UB_23      0.0431872000
_diffrn_orient_matrix_UB_31      -0.1034435000
_diffrn_orient_matrix_UB_32      -0.0035623000
_diffrn_orient_matrix_UB_33      -0.1192663000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22233
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.854
_diffrn_reflns_theta_min         3.660
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.352
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 2992 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0019(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6846
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0257
_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)+(0.0317P)²+1.0622P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0695
_reflns_Friedel_coverage         0.863
_reflns_Friedel_fraction_full    0.965
_reflns_Friedel_fraction_max     0.929
_reflns_number_gt                6676
_reflns_number_total             6846
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt02903d2.cif
_cod_data_source_block           exp_673
_cod_database_code               7714265
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C46 H64 N22 O24 V4 '
_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   0.617
_shelx_estimated_absorpt_t_min   0.617
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O3W-H3WB
 0.85 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C12(H12A), C1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 N6(H6), N10(H10), N8(H8), N4(H4), N12(H12), C17(H17), C6(H6A), C20(H20),
 C9(H9), C14(H14), C22(H22), C11(H11), C21(H21), C10(H10A), C3(H3), C8(H8A),
 C5(H5), C19(H19), C4(H4A), C18(H18), C7(H7), C16(H16), C15(H15)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.695
_oxdiff_exptl_absorpt_empirical_full_min 0.715
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
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 0.29130(5) 0.29926(3) 0.22814(3) 0.01400(10) Uani 1 1 d . . . . .
V2 V 0.24257(4) 0.73271(3) 0.25749(3) 0.01398(10) Uani 1 1 d . . . . .
O3 O 0.3084(2) 0.47813(16) -0.02871(15) 0.0180(4) Uani 1 1 d . . . . .
O6 O 0.44803(19) 0.68424(15) 0.34125(15) 0.0166(4) Uani 1 1 d . . . . .
O5 O 0.25585(19) 0.61723(14) 0.16797(15) 0.0148(4) Uani 1 1 d . . . . .
O7 O 0.6218(2) 0.60329(15) 0.31007(16) 0.0182(4) Uani 1 1 d . . . . .
O1 O 0.38575(19) 0.42803(14) 0.25920(15) 0.0149(4) Uani 1 1 d . . . . .
O2 O 0.2402(2) 0.36254(15) 0.06485(16) 0.0186(4) Uani 1 1 d . . . . .
O4 O 0.3349(2) 0.25159(15) 0.34976(16) 0.0193(4) Uani 1 1 d . . . . .
O8 O 0.0874(2) 0.77334(15) 0.19189(16) 0.0195(4) Uani 1 1 d . . . . .
O1W O 0.7458(3) 0.6263(2) 0.1534(2) 0.0302(5) Uani 1 1 d . . . . .
O4W O 0.2091(2) 0.19938(19) 0.5062(2) 0.0279(5) Uani 1 1 d . . . . .
O2W O 0.1687(3) 0.3293(2) 0.8122(2) 0.0366(6) Uani 1 1 d . . . . .
N6 N -0.0653(3) 0.4685(2) 0.2177(2) 0.0230(5) Uani 1 1 d . . . . .
H6 H -0.1137 0.5217 0.2024 0.028 Uiso 1 1 calc R . . . .
O3W O 0.2217(3) 0.3694(2) 0.6181(2) 0.0391(6) Uani 1 1 d D . . . .
N3 N 0.1605(3) 0.18436(18) 0.1419(2) 0.0189(5) Uani 1 1 d . . . . .
N9 N 0.2938(2) 0.83893(18) 0.38384(19) 0.0179(5) Uani 1 1 d . . . . .
N11 N 0.1804(2) 0.64580(19) 0.3686(2) 0.0177(5) Uani 1 1 d . . . . .
N10 N 0.3995(3) 0.91202(19) 0.5421(2) 0.0196(5) Uani 1 1 d . . . . .
H10 H 0.4638 0.9284 0.6026 0.024 Uiso 1 1 calc R . . . .
N1 N 0.4640(2) 0.2328(2) 0.1943(2) 0.0197(5) Uani 1 1 d . . . . .
N7 N 0.3349(2) 0.82039(18) 0.16349(19) 0.0184(5) Uani 1 1 d . . . . .
N5 N 0.1048(3) 0.36313(19) 0.2359(2) 0.0185(5) Uani 1 1 d . . . . .
N2 N 0.5911(3) 0.1439(2) 0.1207(2) 0.0260(6) Uani 1 1 d . . . . .
N8 N 0.4820(3) 0.9038(2) 0.1064(3) 0.0301(6) Uani 1 1 d . . . . .
H8 H 0.5586 0.9301 0.1056 0.036 Uiso 1 1 calc R . . . .
N4 N -0.0277(3) 0.1171(2) 0.0259(2) 0.0233(5) Uani 1 1 d . . . . .
H4 H -0.1017 0.1095 -0.0307 0.028 Uiso 1 1 calc R . . . .
N12 N 0.1708(3) 0.5319(2) 0.4868(2) 0.0244(5) Uani 1 1 d . . . . .
H12 H 0.1898 0.4794 0.5265 0.029 Uiso 1 1 calc R . . . .
C12 C 0.3917(3) 0.5888(2) 0.1771(2) 0.0143(5) Uani 1 1 d . . . . .
H12A H 0.4143 0.6185 0.1155 0.017 Uiso 1 1 calc R . . . .
C13 C 0.4963(3) 0.6271(2) 0.2848(2) 0.0150(5) Uani 1 1 d . . . . .
C2 C 0.3109(3) 0.4374(2) 0.0602(2) 0.0151(5) Uani 1 1 d . . . . .
C17 C 0.4112(3) 0.8456(2) 0.4685(2) 0.0187(5) Uani 1 1 d . . . . .
H17 H 0.4912 0.8091 0.4760 0.022 Uiso 1 1 calc R . . . .
C6 C 0.0563(3) 0.1954(2) 0.0482(2) 0.0186(6) Uani 1 1 d . . . . .
H6A H 0.0429 0.2507 0.0033 0.022 Uiso 1 1 calc R . . . .
C1 C 0.4079(3) 0.4770(2) 0.1705(2) 0.0140(5) Uani 1 1 d . . . . .
H1 H 0.5040 0.4637 0.1739 0.017 Uiso 1 1 calc R . . . .
C20 C 0.2354(3) 0.5622(2) 0.4175(3) 0.0212(6) Uani 1 1 d . . . . .
H20 H 0.3090 0.5294 0.4051 0.025 Uiso 1 1 calc R . . . .
C9 C 0.0580(3) 0.4528(2) 0.2046(2) 0.0194(6) Uani 1 1 d . . . . .
H9 H 0.1051 0.4992 0.1770 0.023 Uiso 1 1 calc R . . . .
C14 C 0.4649(3) 0.8498(2) 0.1881(3) 0.0253(6) Uani 1 1 d . . . . .
H14 H 0.5357 0.8349 0.2538 0.030 Uiso 1 1 calc R . . . .
C22 C 0.0751(3) 0.6687(2) 0.4108(3) 0.0222(6) Uani 1 1 d . . . . .
H22 H 0.0177 0.7236 0.3918 0.027 Uiso 1 1 calc R . . . .
C11 C 0.0051(3) 0.3191(3) 0.2713(3) 0.0309(7) Uani 1 1 d . . . . .
H11 H 0.0093 0.2554 0.2984 0.037 Uiso 1 1 calc R . . . .
C21 C 0.0687(3) 0.5988(3) 0.4840(3) 0.0255(6) Uani 1 1 d . . . . .
H21 H 0.0076 0.5965 0.5242 0.031 Uiso 1 1 calc R . . . .
C10 C -0.1002(4) 0.3836(3) 0.2602(3) 0.0344(8) Uani 1 1 d . . . . .
H10A H -0.1806 0.3725 0.2780 0.041 Uiso 1 1 calc R . . . .
C3 C 0.4679(3) 0.1889(3) 0.1042(3) 0.0266(7) Uani 1 1 d . . . . .
H3 H 0.3947 0.1889 0.0372 0.032 Uiso 1 1 calc R . . . .
C8 C 0.1424(4) 0.0941(3) 0.1811(3) 0.0464(11) Uani 1 1 d . . . . .
H8A H 0.2004 0.0660 0.2464 0.056 Uiso 1 1 calc R . . . .
C5 C 0.5909(4) 0.2130(3) 0.2732(3) 0.0368(9) Uani 1 1 d . . . . .
H5 H 0.6183 0.2338 0.3465 0.044 Uiso 1 1 calc R . . . .
C19 C 0.2015(3) 0.9040(2) 0.4057(3) 0.0251(6) Uani 1 1 d . . . . .
H19 H 0.1100 0.9149 0.3604 0.030 Uiso 1 1 calc R . . . .
C4 C 0.6702(4) 0.1585(3) 0.2282(3) 0.0373(8) Uani 1 1 d . . . . .
H4A H 0.7604 0.1358 0.2637 0.045 Uiso 1 1 calc R . . . .
C18 C 0.2664(3) 0.9494(2) 0.5039(3) 0.0260(7) Uani 1 1 d . . . . .
H18 H 0.2283 0.9963 0.5383 0.031 Uiso 1 1 calc R . . . .
C7 C 0.0260(5) 0.0516(3) 0.1096(4) 0.0506(12) Uani 1 1 d . . . . .
H7 H -0.0097 -0.0100 0.1165 0.061 Uiso 1 1 calc R . . . .
C16 C 0.2672(4) 0.8578(4) 0.0612(4) 0.0497(12) Uani 1 1 d . . . . .
H16 H 0.1730 0.8491 0.0219 0.060 Uiso 1 1 calc R . . . .
C15 C 0.3570(5) 0.9095(4) 0.0253(4) 0.0584(15) Uani 1 1 d . . . . .
H15 H 0.3369 0.9424 -0.0418 0.070 Uiso 1 1 calc R . . . .
H2 H 0.618(5) 0.110(3) 0.075(4) 0.031(11) Uiso 1 1 d . . . . .
H3WA H 0.181(6) 0.367(4) 0.664(5) 0.048(15) Uiso 1 1 d . . . . .
H4WA H 0.271(5) 0.170(4) 0.561(4) 0.042(13) Uiso 1 1 d . . . . .
H4WB H 0.247(5) 0.209(4) 0.459(4) 0.041(13) Uiso 1 1 d . . . . .
H1WA H 0.711(5) 0.621(4) 0.204(4) 0.043(13) Uiso 1 1 d . . . . .
H1WB H 0.774(6) 0.685(5) 0.160(5) 0.064(18) Uiso 1 1 d . . . . .
H3WB H 0.199(6) 0.317(2) 0.580(4) 0.059(16) Uiso 1 1 d D . . . .
H2WA H 0.200(5) 0.367(4) 0.857(4) 0.036(12) Uiso 1 1 d . . . . .
H2WB H 0.095(5) 0.319(4) 0.808(4) 0.039(13) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O2 77.61(8) . . ?
O1 V1 N3 160.48(9) . . ?
O1 V1 N1 92.24(9) . . ?
O1 V1 N5 90.52(9) . . ?
O4 V1 O1 101.77(9) . . ?
O4 V1 O2 177.97(10) . . ?
O4 V1 N3 97.51(10) . . ?
O4 V1 N1 92.55(10) . . ?
O4 V1 N5 94.79(10) . . ?
N3 V1 O2 83.22(9) . . ?
N3 V1 N1 89.87(10) . . ?
N3 V1 N5 84.87(10) . . ?
N1 V1 O2 85.56(9) . . ?
N5 V1 O2 87.15(9) . . ?
N5 V1 N1 171.47(9) . . ?
O6 V2 N7 85.11(9) . . ?
O5 V2 O6 78.43(8) . . ?
O5 V2 N9 161.11(9) . . ?
O5 V2 N11 92.22(9) . . ?
O5 V2 N7 89.43(9) . . ?
O8 V2 O6 177.94(10) . . ?
O8 V2 O5 102.32(9) . . ?
O8 V2 N9 96.55(10) . . ?
O8 V2 N11 94.76(10) . . ?
O8 V2 N7 92.97(10) . . ?
N9 V2 O6 82.74(9) . . ?
N9 V2 N11 85.39(10) . . ?
N9 V2 N7 90.37(10) . . ?
N11 V2 O6 87.12(9) . . ?
N11 V2 N7 171.56(10) . . ?
C13 O6 V2 114.05(17) . . ?
C12 O5 V2 115.27(16) . . ?
C1 O1 V1 117.27(16) . . ?
C2 O2 V1 114.24(17) . . ?
C9 N6 C10 107.0(3) . . ?
C6 N3 V1 124.6(2) . . ?
C6 N3 C8 105.8(3) . . ?
C8 N3 V1 127.9(2) . . ?
C17 N9 V2 127.1(2) . . ?
C17 N9 C19 106.1(2) . . ?
C19 N9 V2 125.7(2) . . ?
C20 N11 V2 128.8(2) . . ?
C20 N11 C22 105.5(2) . . ?
C22 N11 V2 125.6(2) . . ?
C17 N10 C18 107.8(2) . . ?
C3 N1 V1 129.5(2) . . ?
C3 N1 C5 105.2(3) . . ?
C5 N1 V1 124.5(2) . . ?
C14 N7 V2 129.3(2) . . ?
C14 N7 C16 105.3(3) . . ?
C16 N7 V2 125.4(2) . . ?
C9 N5 V1 127.0(2) . . ?
C9 N5 C11 105.7(3) . . ?
C11 N5 V1 127.2(2) . . ?
C3 N2 C4 107.4(3) . . ?
C14 N8 C15 107.5(3) . . ?
C6 N4 C7 107.0(3) . . ?
C20 N12 C21 108.2(3) . . ?
O5 C12 C13 110.6(2) . . ?
O5 C12 C1 113.0(2) . . ?
C13 C12 C1 109.5(2) . . ?
O6 C13 C12 116.1(2) . . ?
O7 C13 O6 124.5(3) . . ?
O7 C13 C12 119.4(2) . . ?
O3 C2 O2 123.9(3) . . ?
O3 C2 C1 119.6(2) . . ?
O2 C2 C1 116.5(2) . . ?
N9 C17 N10 110.9(3) . . ?
N3 C6 N4 111.5(3) . . ?
O1 C1 C12 112.2(2) . . ?
O1 C1 C2 110.7(2) . . ?
C2 C1 C12 110.7(2) . . ?
N11 C20 N12 110.9(3) . . ?
N5 C9 N6 111.6(3) . . ?
N7 C14 N8 111.2(3) . . ?
C21 C22 N11 109.5(3) . . ?
C10 C11 N5 109.1(3) . . ?
C22 C21 N12 106.0(3) . . ?
C11 C10 N6 106.7(3) . . ?
N1 C3 N2 111.6(3) . . ?
C7 C8 N3 109.2(3) . . ?
C4 C5 N1 109.9(3) . . ?
C18 C19 N9 108.9(3) . . ?
C5 C4 N2 105.9(3) . . ?
C19 C18 N10 106.2(3) . . ?
N4 C7 C8 106.5(3) . . ?
C15 C16 N7 109.9(3) . . ?
C16 C15 N8 106.2(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.975(2) . ?
V1 O2 2.159(2) . ?
V1 O4 1.608(2) . ?
V1 N3 2.111(2) . ?
V1 N1 2.143(2) . ?
V1 N5 2.118(3) . ?
V2 O6 2.1118(19) . ?
V2 O5 1.976(2) . ?
V2 O8 1.618(2) . ?
V2 N9 2.102(2) . ?
V2 N11 2.103(2) . ?
V2 N7 2.122(2) . ?
O3 C2 1.260(3) . ?
O6 C13 1.267(3) . ?
O5 C12 1.402(3) . ?
O7 C13 1.250(3) . ?
O1 C1 1.398(3) . ?
O2 C2 1.260(4) . ?
N6 C9 1.337(4) . ?
N6 C10 1.374(5) . ?
N3 C6 1.319(4) . ?
N3 C8 1.362(4) . ?
N9 C17 1.322(4) . ?
N9 C19 1.385(4) . ?
N11 C20 1.329(4) . ?
N11 C22 1.386(4) . ?
N10 C17 1.340(4) . ?
N10 C18 1.375(4) . ?
N1 C3 1.312(4) . ?
N1 C5 1.376(4) . ?
N7 C14 1.315(4) . ?
N7 C16 1.360(4) . ?
N5 C9 1.323(4) . ?
N5 C11 1.378(4) . ?
N2 C3 1.346(4) . ?
N2 C4 1.359(5) . ?
N8 C14 1.337(4) . ?
N8 C15 1.349(5) . ?
N4 C6 1.335(4) . ?
N4 C7 1.361(5) . ?
N12 C20 1.333(4) . ?
N12 C21 1.372(4) . ?
C12 C13 1.526(4) . ?
C12 C1 1.536(4) . ?
C2 C1 1.527(4) . ?
C22 C21 1.352(5) . ?
C11 C10 1.355(5) . ?
C8 C7 1.362(5) . ?
C5 C4 1.357(5) . ?
C19 C18 1.359(4) . ?
C16 C15 1.349(6) . ?
