#------------------------------------------------------------------------------
#$Date: 2026-04-05 14:03:28 +0200 (Sun 05 de Apr de 2026) $
#$Revision: 305362 $
#$URL: svn://www.crystallography.net/cod/cif/7/72/02/7720203.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_7720203
loop_
_publ_author_name
'Topić, Edi'
'Sarjanović, Josipa'
'Kuzman, Dino'
'Cocut, Andrea'
'Hrenar, Tomica'
'Pisk, Jana'
'Vrdoljak, Višnja'
_publ_section_title
;
 Nicotinoyl hydrazone-directed vanadium assemblies: metallosupramolecular
 isomerism, polymorphism, and catalytic oxidation performance.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4237
_journal_page_last               4249
_journal_paper_doi               10.1039/d5dt03088a
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         '0.5(C34 H36 N6 O10 V2)'
_chemical_formula_sum            'C17 H18 N3 O5 V'
_chemical_formula_weight         395.28
_chemical_name_systematic
'oxo-n-propoxo-[N''-(2-oxo-3-methoxybenzylidene)nicotinoylhydrazonato]vanadium(v) polymer form alpha'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-09-08
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-12-22 deposited with the CCDC.	2026-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   15.7460(2)
_cell_length_b                   13.50300(10)
_cell_length_c                   34.1126(4)
_cell_measurement_reflns_used    12497
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.8820
_cell_measurement_theta_min      3.8190
_cell_volume                     7252.96(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -117.00 -45.00   0.50    2.50    --  -46.93 -51.00   4.00  144
  2  ω    -58.00 -33.00   0.50    9.00    --  -86.25  51.00 150.00   50
  3  ω   -145.00-120.00   0.50    9.00    --  -86.25-101.00 138.00   50
  4  ω     89.00 174.00   0.50    9.00    --  106.38  77.00  -4.00  170
  5  ω   -118.00 -92.00   0.50    2.50    --  -46.93-125.00-180.00   52
  6  ω     -4.00  26.00   0.50    2.50    --  -46.93  19.00 150.00   60
  7  ω    -22.00  21.00   0.50    2.50    --   46.93 -19.00-150.00   86
  8  ω    -40.00 -14.00   0.50    9.00    --  -86.25  38.00  90.00   52
  9  ω     89.00 162.00   0.50    9.00    --  106.38  77.00-120.00  146
 10  ω     34.00  68.00   0.50    9.00    --  106.38 -77.00-180.00   68
 11  ω     34.00  59.00   0.50    9.00    --  106.38 -57.00  30.00   50
 12  ω     34.00  72.00   0.50    9.00    --  106.38 -77.00 150.00   76
 13  ω     79.00 104.00   0.50    9.00    --  106.38 -77.00-180.00   50
 14  ω     34.00 105.00   0.50    9.00    --  106.38 -77.00  30.00  142
 15  ω     39.00  64.00   0.50    9.00    --  106.38 -57.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0118563000
_diffrn_orient_matrix_UB_12      0.0388396000
_diffrn_orient_matrix_UB_13      -0.0421107000
_diffrn_orient_matrix_UB_21      0.0619050000
_diffrn_orient_matrix_UB_22      -0.0856104000
_diffrn_orient_matrix_UB_23      -0.0086523000
_diffrn_orient_matrix_UB_31      -0.0748225000
_diffrn_orient_matrix_UB_32      -0.0646416000
_diffrn_orient_matrix_UB_33      -0.0138447000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            29109
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.337
_diffrn_reflns_theta_min         3.821
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.871
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.53a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7363
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0819P)²+2.4504P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1398
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6071
_reflns_number_total             7363
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt03088a2.cif
_cod_data_source_block           3alpha
_cod_depositor_comments
'Adding full bibliography for 7720194--7720204.cif.'
_cod_database_code               7720203
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'V C N O'
_chemical_oxdiff_usercomment     ' '
_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   0.868
_shelx_estimated_absorpt_t_min   0.793
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-C15
 1.5 with sigma of 0.02
 O4-C18
 1.5 with sigma of 0.02
 C19-O4
 2.3 with sigma of 0.02
 H17A-O4
 2.85 with sigma of 0.02
 C15-C17
 2.54 with sigma of 0.04
 C17A-C15A
 2.54 with sigma of 0.04
 C18-C20
 2.54 with sigma of 0.04
 C15-C16 \\sim C16-C17
 with sigma of 0.02
 C17A-C16A \\sim C16A-C15A
 with sigma of 0.02
 C18-C19 \\sim C19-C20
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C15 \\sim C16 \\sim C17: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C17A \\sim C16A \\sim C15A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C18 \\sim C19 \\sim C20: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C15, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17A, C16A, C15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C18, C19, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C15(0.5) H15A(0.5) H15B(0.5) C16(0.5) H16A(0.5) H16B(0.5) C17(0.5)
 H17A(0.5) H17B(0.5) H17C(0.5) C18(0.5) H18A(0.5) H18B(0.5) C19(0.5) H19A(0.5)
 H19B(0.5) C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5)
6.a Free rotating group:
 C15(C16,C17), C17A(C16A,C15A), C18(C19,C20)
6.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C16A(H16C,H16D), C15A(H15C,H15D), C18(H18A,
 H18B), C19(H19A,H19B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C13(H13), C10A(H10A), C10(H10), C11(H11), C8(H8), C12(H12),
 C13A(H13A), C11A(H11A), C6(H6), C7(H7), C2A(H2A), C12A(H12A), C8A(H8A),
 C7A(H7A), C6A(H6A)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C17(H17A,H17B,H17C), C17A(H17D,
 H17E,H17F), C20(H20A,H20B,H20C)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.259
_oxdiff_exptl_absorpt_empirical_full_min 0.772
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'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, 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
V1A V 0.85587(3) 0.64740(3) 0.66804(2) 0.04783(13) Uani 1 1 d . . . . .
V1 V 0.40012(3) 0.67718(4) 0.57309(2) 0.05007(14) Uani 1 1 d . . . . .
O1 O 0.52160(11) 0.66415(13) 0.58534(5) 0.0486(4) Uani 1 1 d . . . . .
O1A O 0.95060(10) 0.70864(12) 0.63941(5) 0.0508(4) Uani 1 1 d . . . . .
O2 O 0.30029(11) 0.63342(14) 0.54993(5) 0.0519(4) Uani 1 1 d . . . . .
O2A O 0.74306(12) 0.64405(15) 0.68379(6) 0.0587(5) Uani 1 1 d . . . . .
O4A O 0.87691(12) 0.52893(14) 0.64781(6) 0.0609(5) Uani 1 1 d . . . . .
N2 N 0.45663(12) 0.62774(15) 0.52089(5) 0.0436(4) Uani 1 1 d . . . . .
O3 O 0.13587(12) 0.62850(18) 0.53749(7) 0.0706(6) Uani 1 1 d . . . . .
N3 N 0.78527(12) 0.66071(15) 0.60446(6) 0.0471(4) Uani 1 1 d . . . . .
N1 N 0.54504(12) 0.62448(16) 0.52089(6) 0.0487(5) Uani 1 1 d . . . . .
N3A N 1.09475(12) 0.99217(16) 0.58871(6) 0.0482(4) Uani 1 1 d . . . . .
O5A O 0.89972(13) 0.64024(18) 0.70979(7) 0.0708(6) Uani 1 1 d . . . . .
O5 O 0.39959(15) 0.78963(16) 0.55884(8) 0.0768(6) Uani 1 1 d . . . . .
N2A N 0.83677(13) 0.80424(17) 0.67135(6) 0.0522(5) Uani 1 1 d . . . . .
N1A N 0.89695(13) 0.86322(16) 0.65225(7) 0.0551(5) Uani 1 1 d . . . . .
C9 C 0.66514(15) 0.65099(16) 0.56155(7) 0.0433(5) Uani 1 1 d . . . . .
O4 O 0.37071(16) 0.6842(2) 0.62237(6) 0.0891(8) Uani 1 1 d D . . . .
C1 C 0.57193(15) 0.64677(16) 0.55576(7) 0.0441(5) Uani 1 1 d . . . . .
C3 C 0.33074(15) 0.60791(17) 0.48187(7) 0.0451(5) Uani 1 1 d . . . . .
C4 C 0.27428(15) 0.62067(17) 0.51310(7) 0.0441(5) Uani 1 1 d . . . . .
C1A C 0.95411(14) 0.80493(18) 0.63762(7) 0.0461(5) Uani 1 1 d . . . . .
C2 C 0.42068(15) 0.60779(18) 0.48802(7) 0.0458(5) Uani 1 1 d . . . . .
H2 H 0.455359 0.592250 0.466828 0.055 Uiso 1 1 calc R U . . .
C13 C 0.71883(16) 0.64738(17) 0.52906(7) 0.0482(5) Uani 1 1 d . . . . .
H13 H 0.696621 0.643118 0.503853 0.058 Uiso 1 1 calc R U . . .
C10A C 1.02952(14) 0.94903(19) 0.60744(7) 0.0460(5) Uani 1 1 d . . . . .
H10A H 0.982916 0.987863 0.614087 0.055 Uiso 1 1 calc R U . . .
C9A C 1.02817(15) 0.84928(18) 0.61739(7) 0.0458(5) Uani 1 1 d . . . . .
C10 C 0.70107(14) 0.65852(17) 0.59848(7) 0.0447(5) Uani 1 1 d . . . . .
H10 H 0.665235 0.662228 0.620104 0.054 Uiso 1 1 calc R U . . .
C5 C 0.18582(16) 0.61722(18) 0.50552(8) 0.0511(6) Uani 1 1 d . . . . .
C11 C 0.83512(17) 0.65656(19) 0.57275(8) 0.0514(6) Uani 1 1 d . . . . .
H11 H 0.893619 0.658037 0.576460 0.062 Uiso 1 1 calc R U . . .
C8 C 0.29967(17) 0.59423(18) 0.44344(7) 0.0517(6) Uani 1 1 d . . . . .
H8 H 0.337274 0.585872 0.422685 0.062 Uiso 1 1 calc R U . . .
O3A O 0.62739(17) 0.5548(2) 0.72482(10) 0.1073(10) Uani 1 1 d . . . . .
C12 C 0.80496(17) 0.65023(19) 0.53494(8) 0.0515(6) Uani 1 1 d . . . . .
H12 H 0.842254 0.647938 0.513821 0.062 Uiso 1 1 calc R U . . .
C4A C 0.70285(16) 0.6988(2) 0.71017(9) 0.0612(7) Uani 1 1 d . . . . .
C13A C 1.09790(17) 0.7921(2) 0.60799(10) 0.0624(7) Uani 1 1 d . . . . .
H13A H 1.099172 0.725045 0.614168 0.075 Uiso 1 1 calc R U . . .
C11A C 1.16155(17) 0.9351(2) 0.58019(9) 0.0612(7) Uani 1 1 d . . . . .
H11A H 1.207526 0.964035 0.567459 0.073 Uiso 1 1 calc R U . . .
C6 C 0.15759(17) 0.6044(2) 0.46755(9) 0.0576(6) Uani 1 1 d . . . . .
H6 H 0.099533 0.603166 0.462558 0.069 Uiso 1 1 calc R U . . .
C7 C 0.21384(19) 0.5933(2) 0.43687(8) 0.0591(7) Uani 1 1 d . . . . .
H7 H 0.193337 0.585202 0.411511 0.071 Uiso 1 1 calc R U . . .
C2A C 0.78270(19) 0.8500(2) 0.69242(10) 0.0666(7) Uani 1 1 d . . . . .
H2A H 0.784115 0.918836 0.692903 0.080 Uiso 1 1 calc R U . . .
C3A C 0.71949(19) 0.7996(3) 0.71553(10) 0.0681(8) Uani 1 1 d . . . . .
C12A C 1.1660(2) 0.8365(2) 0.58915(12) 0.0743(9) Uani 1 1 d . . . . .
H12A H 1.214024 0.799767 0.582716 0.089 Uiso 1 1 calc R U . . .
C5A C 0.6383(2) 0.6536(3) 0.73243(12) 0.0781(9) Uani 1 1 d . . . . .
C8A C 0.6729(3) 0.8546(3) 0.74374(13) 0.0949(12) Uani 1 1 d . . . . .
H8A H 0.683742 0.921703 0.747406 0.114 Uiso 1 1 calc R U . . .
C7A C 0.6114(3) 0.8077(4) 0.76561(15) 0.1076(15) Uani 1 1 d . . . . .
H7A H 0.581800 0.842917 0.784634 0.129 Uiso 1 1 calc R U . . .
C6A C 0.5933(3) 0.7089(4) 0.75957(14) 0.1035(14) Uani 1 1 d . . . . .
H6A H 0.550241 0.678956 0.773977 0.124 Uiso 1 1 calc R U . . .
C14 C 0.0477(2) 0.6296(4) 0.53170(15) 0.1106(16) Uani 1 1 d . . . . .
H14A H 0.033389 0.680121 0.513046 0.166 Uiso 1 1 calc R U . . .
H14B H 0.019782 0.643042 0.556139 0.166 Uiso 1 1 calc R U . . .
H14C H 0.029624 0.566309 0.521953 0.166 Uiso 1 1 calc R U . . .
C14A C 0.5574(4) 0.5056(4) 0.7398(2) 0.161(3) Uani 1 1 d . . . . .
H14D H 0.555562 0.439609 0.729298 0.241 Uiso 1 1 calc R U . . .
H14E H 0.506637 0.540396 0.732505 0.241 Uiso 1 1 calc R U . . .
H14F H 0.561532 0.502596 0.767803 0.241 Uiso 1 1 calc R U . . .
C15 C 0.3980(7) 0.6593(9) 0.6598(2) 0.129(4) Uani 0.5 1 d DG U P A 1
H15A H 0.446296 0.699466 0.667405 0.155 Uiso 0.5 1 calc R U P A 1
H15B H 0.414201 0.590029 0.660961 0.155 Uiso 0.5 1 calc R U P A 1
C16 C 0.3221(10) 0.6794(12) 0.6867(3) 0.181(7) Uani 0.5 1 d DG U P A 1
H16A H 0.336294 0.659436 0.713183 0.217 Uiso 0.5 1 calc R U P A 1
H16B H 0.310438 0.749976 0.686974 0.217 Uiso 0.5 1 calc R U P A 1
C17 C 0.2423(9) 0.624(2) 0.6734(7) 0.337(17) Uani 0.5 1 d DG U P A 1
H17A H 0.207341 0.667415 0.658070 0.506 Uiso 0.5 1 calc DR U P A 1
H17B H 0.211176 0.602068 0.696013 0.506 Uiso 0.5 1 calc R U P A 1
H17C H 0.258409 0.567755 0.657907 0.506 Uiso 0.5 1 calc R U P A 1
C17A C 1.0725(3) 0.4929(5) 0.6320(3) 0.202(4) Uani 1 1 d DG U . B 2
H17D H 1.086456 0.519885 0.606791 0.302 Uiso 1 1 calc R U . B 2
H17E H 1.119913 0.455611 0.641807 0.302 Uiso 1 1 calc R U . B 2
H17F H 1.059755 0.545857 0.649853 0.302 Uiso 1 1 calc R U . B 2
C16A C 0.9952(3) 0.4249(4) 0.62823(15) 0.164(3) Uani 1 1 d DG U . B 2
H16C H 0.970609 0.432831 0.602336 0.197 Uiso 1 1 calc R U . B 2
H16D H 1.013271 0.356611 0.630898 0.197 Uiso 1 1 calc R U . B 2
C15A C 0.9275(3) 0.4474(3) 0.65916(13) 0.1005(13) Uani 1 1 d DG U . B 2
H15C H 0.891681 0.389699 0.662762 0.121 Uiso 1 1 calc R U . B 2
H15D H 0.954866 0.461898 0.683986 0.121 Uiso 1 1 calc R U . B 2
C18 C 0.3321(11) 0.7294(10) 0.6531(3) 0.179(6) Uani 0.5 1 d DG U P A 2
H18A H 0.271040 0.731348 0.649250 0.215 Uiso 0.5 1 calc R U P A 2
H18B H 0.352739 0.796620 0.656110 0.215 Uiso 0.5 1 calc R U P A 2
C19 C 0.3545(14) 0.6671(18) 0.6891(4) 0.309(13) Uani 0.5 1 d DG U P A 2
H19A H 0.413279 0.646233 0.687318 0.371 Uiso 0.5 1 calc R U P A 2
H19B H 0.348538 0.707460 0.712486 0.371 Uiso 0.5 1 calc R U P A 2
C20 C 0.2977(16) 0.5756(13) 0.6929(6) 0.250(11) Uani 0.5 1 d DG U P A 2
H20A H 0.248484 0.591796 0.708210 0.375 Uiso 0.5 1 calc R U P A 2
H20B H 0.328745 0.523424 0.705578 0.375 Uiso 0.5 1 calc R U P A 2
H20C H 0.280348 0.554142 0.667302 0.375 Uiso 0.5 1 calc R U P A 2
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
O1A V1A N3 82.72(7) . . ?
O1A V1A N2A 73.55(7) . . ?
O2A V1A O1A 151.69(8) . . ?
O2A V1A N3 79.83(8) . . ?
O2A V1A N2A 82.79(9) . . ?
O4A V1A O1A 92.54(8) . . ?
O4A V1A O2A 105.63(9) . . ?
O4A V1A N3 78.82(8) . . ?
O4A V1A N2A 159.82(9) . . ?
O5A V1A O1A 98.13(10) . . ?
O5A V1A O2A 98.93(10) . . ?
O5A V1A O4A 102.31(11) . . ?
O5A V1A N3 178.54(10) . . ?
O5A V1A N2A 94.24(11) . . ?
N2A V1A N3 84.85(8) . . ?
O1 V1 N2 74.90(7) . . ?
O2 V1 O1 152.40(8) . . ?
O2 V1 N2 84.07(8) . . ?
O5 V1 O1 98.92(10) . . ?
O5 V1 O2 99.73(10) . . ?
O5 V1 N2 92.67(11) . . ?
O5 V1 O4 103.90(14) . . ?
O4 V1 O1 93.34(10) . . ?
O4 V1 O2 101.68(11) . . ?
O4 V1 N2 161.11(11) . . ?
C1 O1 V1 116.28(15) . . ?
C1A O1A V1A 118.38(15) . . ?
C4 O2 V1 134.65(16) . . ?
C4A O2A V1A 129.80(18) . . ?
C15A O4A V1A 134.5(2) . . ?
N1 N2 V1 115.70(14) . . ?
C2 N2 V1 128.33(17) . . ?
C2 N2 N1 115.71(19) . . ?
C5 O3 C14 117.6(3) . . ?
C10 N3 V1A 125.65(16) . . ?
C11 N3 V1A 116.59(16) . . ?
C11 N3 C10 117.1(2) . . ?
C1 N1 N2 108.59(19) . . ?
C11A N3A C10A 117.1(2) . . ?
N1A N2A V1A 116.31(16) . . ?
C2A N2A V1A 127.1(2) . . ?
C2A N2A N1A 116.1(2) . . ?
C1A N1A N2A 107.7(2) . . ?
C13 C9 C1 119.5(2) . . ?
C10 C9 C1 121.9(2) . . ?
C10 C9 C13 118.6(2) . . ?
C15 O4 V1 142.2(4) . . ?
C18 O4 V1 152.5(6) . . ?
O1 C1 C9 119.4(2) . . ?
N1 C1 O1 123.5(2) . . ?
N1 C1 C9 117.0(2) . . ?
C4 C3 C2 121.2(2) . . ?
C4 C3 C8 120.2(2) . . ?
C8 C3 C2 118.6(2) . . ?
O2 C4 C3 122.6(2) . . ?
O2 C4 C5 118.6(2) . . ?
C3 C4 C5 118.8(2) . . ?
O1A C1A C9A 117.3(2) . . ?
N1A C1A O1A 124.0(2) . . ?
N1A C1A C9A 118.7(2) . . ?
N2 C2 C3 124.3(2) . . ?
N2 C2 H2 117.9 . . ?
C3 C2 H2 117.9 . . ?
C9 C13 H13 120.6 . . ?
C12 C13 C9 118.8(2) . . ?
C12 C13 H13 120.6 . . ?
N3A C10A H10A 118.4 . . ?
N3A C10A C9A 123.3(2) . . ?
C9A C10A H10A 118.4 . . ?
C10A C9A C1A 121.2(2) . . ?
C13A C9A C1A 120.6(2) . . ?
C13A C9A C10A 118.2(2) . . ?
N3 C10 C9 122.9(2) . . ?
N3 C10 H10 118.5 . . ?
C9 C10 H10 118.5 . . ?
O3 C5 C4 114.9(2) . . ?
O3 C5 C6 125.7(2) . . ?
C6 C5 C4 119.5(2) . . ?
N3 C11 H11 118.1 . . ?
N3 C11 C12 123.9(2) . . ?
C12 C11 H11 118.1 . . ?
C3 C8 H8 120.2 . . ?
C7 C8 C3 119.7(3) . . ?
C7 C8 H8 120.2 . . ?
C5A O3A C14A 119.8(4) . . ?
C13 C12 C11 118.7(2) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
O2A C4A C3A 122.8(3) . . ?
O2A C4A C5A 118.0(3) . . ?
C3A C4A C5A 119.1(3) . . ?
C9A C13A H13A 120.6 . . ?
C9A C13A C12A 118.8(3) . . ?
C12A C13A H13A 120.6 . . ?
N3A C11A H11A 118.2 . . ?
N3A C11A C12A 123.6(3) . . ?
C12A C11A H11A 118.2 . . ?
C5 C6 H6 119.4 . . ?
C7 C6 C5 121.2(2) . . ?
C7 C6 H6 119.4 . . ?
C8 C7 C6 120.6(2) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
N2A C2A H2A 118.6 . . ?
N2A C2A C3A 122.8(3) . . ?
C3A C2A H2A 118.6 . . ?
C4A C3A C2A 121.2(3) . . ?
C4A C3A C8A 120.1(3) . . ?
C8A C3A C2A 118.8(3) . . ?
C13A C12A H12A 120.5 . . ?
C11A C12A C13A 119.0(3) . . ?
C11A C12A H12A 120.5 . . ?
O3A C5A C4A 114.2(3) . . ?
O3A C5A C6A 126.0(3) . . ?
C6A C5A C4A 119.7(4) . . ?
C3A C8A H8A 120.3 . . ?
C7A C8A C3A 119.3(4) . . ?
C7A C8A H8A 120.3 . . ?
C8A C7A H7A 119.7 . . ?
C8A C7A C6A 120.6(4) . . ?
C6A C7A H7A 119.7 . . ?
C5A C6A H6A 119.5 . . ?
C7A C6A C5A 121.1(4) . . ?
C7A C6A H6A 119.5 . . ?
O3 C14 H14A 109.5 . . ?
O3 C14 H14B 109.5 . . ?
O3 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O3A C14A H14D 109.5 . . ?
O3A C14A H14E 109.5 . . ?
O3A C14A H14F 109.5 . . ?
H14D C14A H14E 109.5 . . ?
H14D C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
O4 C15 H15A 110.7 . . ?
O4 C15 H15B 110.7 . . ?
O4 C15 C16 105.4(6) . . ?
H15A C15 H15B 108.8 . . ?
C16 C15 H15A 110.7 . . ?
C16 C15 H15B 110.7 . . ?
C15 C16 H16A 109.2 . . ?
C15 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
C17 C16 C15 112.1 . . ?
C17 C16 H16A 109.2 . . ?
C17 C16 H16B 109.2 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
H17D C17A H17E 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
C16A C17A H17D 109.5 . . ?
C16A C17A H17E 109.5 . . ?
C16A C17A H17F 109.5 . . ?
C17A C16A H16C 109.2 . . ?
C17A C16A H16D 109.2 . . ?
H16C C16A H16D 107.9 . . ?
C15A C16A C17A 112.1 . . ?
C15A C16A H16C 109.2 . . ?
C15A C16A H16D 109.2 . . ?
O4A C15A C16A 111.0(3) . . ?
O4A C15A H15C 109.4 . . ?
O4A C15A H15D 109.4 . . ?
C16A C15A H15C 109.4 . . ?
C16A C15A H15D 109.4 . . ?
H15C C15A H15D 108.0 . . ?
O4 C18 H18A 110.6 . . ?
O4 C18 H18B 110.6 . . ?
O4 C18 C19 105.7(12) . . ?
H18A C18 H18B 108.7 . . ?
C19 C18 H18A 110.6 . . ?
C19 C18 H18B 110.6 . . ?
C18 C19 H19A 109.2 . . ?
C18 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C20 C19 C18 112.1 . . ?
C20 C19 H19A 109.2 . . ?
C20 C19 H19B 109.2 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
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
V1A O1A 1.9653(17) . ?
V1A O2A 1.8563(18) . ?
V1A O4A 1.773(2) . ?
V1A N3 2.444(2) . ?
V1A O5A 1.586(2) . ?
V1A N2A 2.142(2) . ?
V1 O1 1.9658(17) . ?
V1 O2 1.8558(18) . ?
V1 N2 2.0994(19) . ?
V1 O5 1.594(2) . ?
V1 O4 1.746(2) . ?
O1 C1 1.305(3) . ?
O1A C1A 1.303(3) . ?
O2 C4 1.333(3) . ?
O2A C4A 1.326(4) . ?
O4A C15A 1.413(4) . ?
N2 N1 1.393(3) . ?
N2 C2 1.285(3) . ?
O3 C5 1.353(3) . ?
O3 C14 1.402(4) . ?
N3 C10 1.342(3) . ?
N3 C11 1.338(3) . ?
N1 C1 1.298(3) . ?
N3A C10A 1.343(3) . ?
N3A C11A 1.336(3) . ?
N2A N1A 1.399(3) . ?
N2A C2A 1.274(4) . ?
N1A C1A 1.296(3) . ?
C9 C1 1.482(3) . ?
C9 C13 1.395(3) . ?
C9 C10 1.385(3) . ?
O4 C15 1.389(8) . ?
O4 C18 1.357(10) . ?
C3 C4 1.398(3) . ?
C3 C2 1.432(3) . ?
C3 C8 1.411(3) . ?
C4 C5 1.418(3) . ?
C1A C9A 1.481(3) . ?
C2 H2 0.9300 . ?
C13 H13 0.9300 . ?
C13 C12 1.372(4) . ?
C10A H10A 0.9300 . ?
C10A C9A 1.389(4) . ?
C9A C13A 1.380(4) . ?
C10 H10 0.9300 . ?
C5 C6 1.380(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.377(4) . ?
C8 H8 0.9300 . ?
C8 C7 1.370(4) . ?
O3A C5A 1.369(5) . ?
O3A C14A 1.384(5) . ?
C12 H12 0.9300 . ?
C4A C3A 1.399(5) . ?
C4A C5A 1.408(4) . ?
C13A H13A 0.9300 . ?
C13A C12A 1.387(4) . ?
C11A H11A 0.9300 . ?
C11A C12A 1.369(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.379(4) . ?
C7 H7 0.9300 . ?
C2A H2A 0.9300 . ?
C2A C3A 1.440(4) . ?
C3A C8A 1.420(5) . ?
C12A H12A 0.9300 . ?
C5A C6A 1.384(6) . ?
C8A H8A 0.9300 . ?
C8A C7A 1.376(6) . ?
C7A H7A 0.9300 . ?
C7A C6A 1.380(7) . ?
C6A H6A 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C14A H14D 0.9600 . ?
C14A H14E 0.9600 . ?
C14A H14F 0.9600 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.5307 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.5301 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17A H17D 0.9600 . ?
C17A H17E 0.9600 . ?
C17A H17F 0.9600 . ?
C17A C16A 1.5307 . ?
C16A H16C 0.9700 . ?
C16A H16D 0.9700 . ?
C16A C15A 1.5301 . ?
C15A H15C 0.9700 . ?
C15A H15D 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.5306 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.5300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
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
V1A O1A C1A N1A -2.9(3) . . . . ?
V1A O1A C1A C9A 177.34(16) . . . . ?
V1A O2A C4A C3A 37.5(4) . . . . ?
V1A O2A C4A C5A -145.2(2) . . . . ?
V1A O4A C15A C16A -119.3(3) . . . . ?
V1A N3 C10 C9 -169.70(17) . . . . ?
V1A N3 C11 C12 171.4(2) . . . . ?
V1A N2A N1A C1A -2.3(3) . . . . ?
V1A N2A C2A C3A -5.5(5) . . . . ?
V1 O1 C1 N1 -9.9(3) . . . . ?
V1 O1 C1 C9 170.84(15) . . . . ?
V1 O2 C4 C3 22.5(3) . . . . ?
V1 O2 C4 C5 -159.28(18) . . . . ?
V1 N2 N1 C1 5.0(2) . . . . ?
V1 N2 C2 C3 -5.7(4) . . . . ?
V1 O4 C15 C16 -170.6(8) . . . . ?
V1 O4 C18 C19 -174.6(12) . . . . ?
O1 V1 O2 C4 -65.8(3) . . . . ?
O1 V1 O4 C15 -22.8(10) . . . . ?
O1 V1 O4 C18 124.4(17) . . . . ?
O1A V1A O2A C4A -74.4(3) . . . . ?
O1A V1A O4A C15A 90.4(3) . . . . ?
O1A C1A C9A C10A 167.5(2) . . . . ?
O1A C1A C9A C13A -12.6(4) . . . . ?
O2 V1 O4 C15 133.9(10) . . . . ?
O2 V1 O4 C18 -78.8(17) . . . . ?
O2 C4 C5 O3 0.6(3) . . . . ?
O2 C4 C5 C6 179.8(2) . . . . ?
O2A V1A O4A C15A -111.6(3) . . . . ?
O2A C4A C3A C2A -0.4(5) . . . . ?
O2A C4A C3A C8A 178.6(3) . . . . ?
O2A C4A C5A O3A 2.6(5) . . . . ?
O2A C4A C5A C6A -178.4(4) . . . . ?
O4A V1A O2A C4A 157.6(2) . . . . ?
N2 V1 O2 C4 -25.7(2) . . . . ?
N2 V1 O4 C15 27.7(11) . . . . ?
N2 V1 O4 C18 175.0(17) . . . . ?
N2 N1 C1 O1 2.9(3) . . . . ?
N2 N1 C1 C9 -177.85(19) . . . . ?
O3 C5 C6 C7 -179.9(3) . . . . ?
N3 V1A O2A C4A -127.2(3) . . . . ?
N3 V1A O4A C15A 172.4(3) . . . . ?
N3 C11 C12 C13 -0.4(4) . . . . ?
N1 N2 C2 C3 -179.5(2) . . . . ?
N3A C10A C9A C1A -179.2(2) . . . . ?
N3A C10A C9A C13A 0.9(4) . . . . ?
N3A C11A C12A C13A 0.3(6) . . . . ?
O5A V1A O2A C4A 52.0(3) . . . . ?
O5A V1A O4A C15A -8.5(3) . . . . ?
O5 V1 O2 C4 66.0(2) . . . . ?
O5 V1 O4 C15 -122.9(10) . . . . ?
O5 V1 O4 C18 24.4(17) . . . . ?
N2A V1A O2A C4A -41.2(2) . . . . ?
N2A V1A O4A C15A 135.9(3) . . . . ?
N2A N1A C1A O1A 3.3(3) . . . . ?
N2A N1A C1A C9A -176.9(2) . . . . ?
N2A C2A C3A C4A -12.9(5) . . . . ?
N2A C2A C3A C8A 168.0(4) . . . . ?
N1A N2A C2A C3A -176.7(3) . . . . ?
N1A C1A C9A C10A -12.2(4) . . . . ?
N1A C1A C9A C13A 167.7(3) . . . . ?
C9 C13 C12 C11 0.0(4) . . . . ?
O4 V1 O2 C4 172.6(2) . . . . ?
O4 C15 C16 C17 55.4(17) . . . . ?
O4 C18 C19 C20 -81.1(19) . . . . ?
C1 C9 C13 C12 -179.3(2) . . . . ?
C1 C9 C10 N3 178.8(2) . . . . ?
C3 C4 C5 O3 178.9(2) . . . . ?
C3 C4 C5 C6 -1.9(4) . . . . ?
C3 C8 C7 C6 -0.8(4) . . . . ?
C4 C3 C2 N2 -6.5(4) . . . . ?
C4 C3 C8 C7 -0.1(4) . . . . ?
C4 C5 C6 C7 1.0(4) . . . . ?
C1A C9A C13A C12A -179.8(3) . . . . ?
C2 N2 N1 C1 179.6(2) . . . . ?
C2 C3 C4 O2 0.1(4) . . . . ?
C2 C3 C4 C5 -178.1(2) . . . . ?
C2 C3 C8 C7 179.5(2) . . . . ?
C13 C9 C1 O1 -170.3(2) . . . . ?
C13 C9 C1 N1 10.4(3) . . . . ?
C13 C9 C10 N3 -1.2(3) . . . . ?
C10A N3A C11A C12A 0.7(4) . . . . ?
C10A C9A C13A C12A 0.1(5) . . . . ?
C9A C13A C12A C11A -0.6(5) . . . . ?
C10 N3 C11 C12 0.0(4) . . . . ?
C10 C9 C1 O1 9.6(3) . . . . ?
C10 C9 C1 N1 -169.7(2) . . . . ?
C10 C9 C13 C12 0.8(3) . . . . ?
C5 C6 C7 C8 0.4(4) . . . . ?
C11 N3 C10 C9 0.9(3) . . . . ?
C8 C3 C4 O2 179.7(2) . . . . ?
C8 C3 C4 C5 1.5(3) . . . . ?
C8 C3 C2 N2 173.9(2) . . . . ?
O3A C5A C6A C7A 178.1(5) . . . . ?
C4A C3A C8A C7A 0.0(7) . . . . ?
C4A C5A C6A C7A -0.8(7) . . . . ?
C11A N3A C10A C9A -1.2(4) . . . . ?
C2A N2A N1A C1A 169.9(3) . . . . ?
C2A C3A C8A C7A 179.1(4) . . . . ?
C3A C4A C5A O3A 180.0(3) . . . . ?
C3A C4A C5A C6A -1.0(5) . . . . ?
C3A C8A C7A C6A -1.8(8) . . . . ?
C5A C4A C3A C2A -177.7(3) . . . . ?
C5A C4A C3A C8A 1.4(5) . . . . ?
C8A C7A C6A C5A 2.2(8) . . . . ?
C14 O3 C5 C4 177.6(3) . . . . ?
C14 O3 C5 C6 -1.5(5) . . . . ?
C14A O3A C5A C4A -169.3(5) . . . . ?
C14A O3A C5A C6A 11.7(8) . . . . ?
C17A C16A C15A O4A 81.3(6) . . . . ?
