#------------------------------------------------------------------------------
#$Date: 2026-04-05 14:03:28 +0200 (Sun 05 de Apr de 2026) $
#$Revision: 305362 $
#$URL: svn://www.crystallography.net/cod/cif/7/72/02/7720202.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_7720202
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         'C16 H16 N3 O5 V'
_chemical_formula_sum            'C16 H16 N3 O5 V'
_chemical_formula_weight         381.26
_chemical_name_systematic
'oxo-ethoxo-[N''-(2-oxo-3-methoxybenzylidene)nicotinoylhydrazonato]vanadium(v) polymer'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 93.011(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.8838(3)
_cell_length_b                   10.7455(3)
_cell_length_c                   26.4644(7)
_cell_measurement_reflns_used    17778
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      77.4980
_cell_measurement_theta_min      3.3460
_cell_volume                     3374.77(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      169.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     94.00 120.00   0.50    1.43    --  107.75  61.00  90.00   52
  2  ω    134.00 160.00   0.50    1.43    --  107.75  61.00  90.00   52
  3  ω    145.00 172.00   0.50    1.43    --  107.75  45.00  60.00   54
  4  ω    113.00 138.00   0.50    1.43    --  107.75  45.00  60.00   50
  5  ω    147.00 173.00   0.50    1.43    --  107.75  61.00-150.00   52
  6  ω    103.00 162.00   0.50    1.43    --  107.75  45.00-180.00  118
  7  ω     92.00 123.00   0.50    1.43    --  107.75  61.00-150.00   62
  8  ω    133.00 175.00   0.50    1.43    --  107.75  44.00-166.00   84
  9  ω     42.00 119.00   0.50    0.36    --   47.03  44.00-166.00  154
 10  ω     95.00 131.00   0.50    1.43    --  107.75  30.00 -30.00   72
 11  ω    135.00 161.00   0.50    1.43    --  107.75  30.00 -30.00   52
 12  ω     99.00 170.00   0.50    1.43    --  107.75  15.00 120.00  142
 13  ω    -22.00  28.00   0.50    0.36    --  -47.03  19.00   0.00  100
 14  ω    -49.00 -17.00   0.50    1.43    --  -86.25  45.00   0.00   64
 15  ω    -85.00 -60.00   0.50    0.36    --  -47.03 125.00  30.00   50
 16  ω    -49.00 -24.00   0.50    1.43    --  -86.25  44.00-166.00   50
 17  ω    -36.00  20.00   0.50    0.36    --  -47.03  44.00-166.00  112
 18  ω      5.00  31.00   0.50    0.36    --   47.03 -44.00  42.00   52
 19  ω    144.00 170.00   0.50    1.43    --  107.75 125.00  60.00   52
 20  ω    100.00 126.00   0.50    1.43    --  107.75 125.00  60.00   52
 21  ω     40.00  66.00   0.50    1.43    --  107.75 -77.00  30.00   52
 22  ω     36.00  71.00   0.50    1.43    --  107.75 -77.00 120.00   70
 23  ω     76.00 104.00   0.50    1.43    --  107.75 -77.00 120.00   56
 24  ω     39.00 101.00   0.50    1.43    --  107.75 -77.00 150.00  124
 25  ω     80.00 105.00   0.50    1.43    --  107.75 -77.00  30.00   50
 26  ω     36.00  67.00   0.50    1.43    --  107.75 -61.00 120.00   62
 27  ω     36.00  67.00   0.50    1.43    --  107.75 -61.00 -90.00   62
 28  ω     79.00 105.00   0.50    1.43    --  107.75 -77.00-180.00   52
 29  ω     44.00  70.00   0.50    1.43    --  107.75 -77.00-180.00   52
 30  ω     36.00  66.00   0.50    1.43    --  107.75 -61.00-180.00   60
 31  ω     36.00  67.00   0.50    1.43    --  107.75 -61.00-150.00   62
 32  ω     41.00  66.00   0.50    1.43    --  107.75 -61.00-120.00   50
 33  ω     39.00  67.00   0.50    1.43    --  107.75 -61.00  90.00   56
 34  ω     56.00 103.00   0.50    1.43    --  107.75-125.00   0.00   94
 35  ω     35.00  94.00   0.50    1.43    --  107.75 -95.00  30.00  118
 36  ω     37.00  63.00   0.50    1.43    --  107.75 -95.00   0.00   52
 37  ω     64.00 105.00   0.50    1.43    --  107.75 -95.00   0.00   82
 38  ω   -100.00 -34.00   0.50    0.36    --  -47.03 -44.00  42.00  132
 39  ω   -140.00-115.00   0.50    1.43    --  -86.25 -44.00  42.00   50
 40  ω   -119.00 -73.00   0.50    0.36    --  -47.03-125.00   0.00   92
;
_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      -0.0175672000
_diffrn_orient_matrix_UB_12      0.0358364000
_diffrn_orient_matrix_UB_13      0.0554347000
_diffrn_orient_matrix_UB_21      0.1086500000
_diffrn_orient_matrix_UB_22      -0.0698552000
_diffrn_orient_matrix_UB_23      0.0167801000
_diffrn_orient_matrix_UB_31      0.0687243000
_diffrn_orient_matrix_UB_32      0.1199646000
_diffrn_orient_matrix_UB_33      -0.0067770000
_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  0.0563
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31106
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.528
_diffrn_reflns_theta_min         3.345
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.212
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.409
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.822
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         7066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0476
_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)+(0.0716P)²+3.4969P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6333
_reflns_number_total             7066
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt03088a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7720194--7720204.cif.'
_cod_database_code               7720202
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'V2 O10 N6 C32'
_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   0.681
_shelx_estimated_absorpt_t_min   0.368
_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.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C15A(H15C,H15D)
2.b Aromatic/amide H refined with riding coordinates:
 C10A(H10A), C10(H10), C12A(H12A), C2(H2), C13(H13), C11(H11), C12(H12),
 C2A(H2A), C13A(H13A), C7(H7), C11A(H11A), C8(H8), C7A(H7A), C8A(H8A), C6(H6),
 C6A(H6A)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C14(H14A,H14B,H14C), C16A(H16D,H16E,H16F), C14A(H14D,
 H14E,H14F)
;
_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 1.582
_oxdiff_exptl_absorpt_empirical_full_min 0.627
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.42441(4) 0.47885(4) 0.37981(2) 0.02173(12) Uani 1 1 d . . . . .
V1A V 0.08536(4) -0.10877(4) 0.34638(2) 0.02512(13) Uani 1 1 d . . . . .
O1 O 0.36391(15) 0.31184(16) 0.39289(7) 0.0241(4) Uani 1 1 d . . . . .
O4 O 0.32977(16) 0.49428(16) 0.32589(7) 0.0257(4) Uani 1 1 d . . . . .
O1A O 0.20697(16) -0.17359(16) 0.30722(7) 0.0278(4) Uani 1 1 d . . . . .
O2 O 0.54397(16) 0.58707(17) 0.37022(7) 0.0273(4) Uani 1 1 d . . . . .
O4A O 0.08703(17) -0.23250(17) 0.39129(7) 0.0296(4) Uani 1 1 d . . . . .
O5 O 0.36033(16) 0.55554(17) 0.42119(7) 0.0285(4) Uani 1 1 d . . . . .
O2A O 0.02426(18) 0.01910(18) 0.38295(8) 0.0330(4) Uani 1 1 d . . . . .
O5A O -0.01956(18) -0.1463(2) 0.30992(8) 0.0357(5) Uani 1 1 d . . . . .
O3 O 0.6207(2) 0.8092(2) 0.34977(8) 0.0405(5) Uani 1 1 d . . . . .
N2 N 0.53979(18) 0.39483(19) 0.43285(8) 0.0227(4) Uani 1 1 d . . . . .
N3A N 0.48167(18) -0.1388(2) 0.18323(8) 0.0233(4) Uani 1 1 d . . . . .
N1 N 0.52241(19) 0.26927(19) 0.44366(8) 0.0253(4) Uani 1 1 d . . . . .
O3A O -0.1331(2) 0.1003(2) 0.44065(9) 0.0468(6) Uani 1 1 d . . . . .
N3 N 0.25280(19) -0.0479(2) 0.39550(9) 0.0266(5) Uani 1 1 d . . . . .
N2A N 0.13637(19) 0.0419(2) 0.29923(8) 0.0249(4) Uani 1 1 d . . . . .
N1A N 0.22491(19) 0.0162(2) 0.26790(9) 0.0272(5) Uani 1 1 d . . . . .
C9 C 0.3927(2) 0.1041(2) 0.42088(9) 0.0238(5) Uani 1 1 d . . . . .
C10A C 0.3904(2) -0.0980(2) 0.20597(10) 0.0236(5) Uani 1 1 d . . . . .
H10A H 0.349601 -0.029843 0.191278 0.028 Uiso 1 1 calc R U . . .
C1 C 0.4282(2) 0.2355(2) 0.41982(9) 0.0236(5) Uani 1 1 d . . . . .
C3A C 0.0058(2) 0.1953(2) 0.32751(10) 0.0272(5) Uani 1 1 d . . . . .
C4 C 0.6148(2) 0.6398(2) 0.40487(10) 0.0256(5) Uani 1 1 d . . . . .
C3 C 0.6515(2) 0.5785(3) 0.44969(10) 0.0266(5) Uani 1 1 d . . . . .
C1A C 0.2552(2) -0.0993(2) 0.27575(10) 0.0253(5) Uani 1 1 d . . . . .
C9A C 0.3527(2) -0.1506(2) 0.25008(10) 0.0248(5) Uani 1 1 d . . . . .
C10 C 0.2883(2) 0.0704(2) 0.39955(10) 0.0256(5) Uani 1 1 d . . . . .
H10 H 0.239118 0.134382 0.387110 0.031 Uiso 1 1 calc R U . . .
C12A C 0.5053(3) -0.2945(3) 0.24799(12) 0.0345(6) Uani 1 1 d . . . . .
H12A H 0.546339 -0.363836 0.261499 0.041 Uiso 1 1 calc R U . . .
C4A C -0.0249(2) 0.1262(2) 0.36979(11) 0.0273(5) Uani 1 1 d . . . . .
C2 C 0.6179(2) 0.4513(2) 0.45910(9) 0.0253(5) Uani 1 1 d . . . . .
H2 H 0.655667 0.407393 0.486147 0.030 Uiso 1 1 calc R U . . .
C13 C 0.4644(2) 0.0103(3) 0.44014(11) 0.0292(6) Uani 1 1 d . . . . .
H13 H 0.536998 0.029779 0.454714 0.035 Uiso 1 1 calc R U . . .
C11 C 0.3226(2) -0.1367(2) 0.41437(11) 0.0296(6) Uani 1 1 d . . . . .
H11 H 0.298974 -0.220989 0.411691 0.035 Uiso 1 1 calc R U . . .
C5A C -0.1067(2) 0.1741(3) 0.40100(11) 0.0319(6) Uani 1 1 d . . . . .
C15 C 0.2130(2) 0.5238(3) 0.32608(11) 0.0304(6) Uani 1 1 d . . . . .
H15A H 0.202822 0.602165 0.344970 0.036 Uiso 1 1 calc R U . . .
H15B H 0.172571 0.456755 0.343288 0.036 Uiso 1 1 calc R U . . .
C12 C 0.4270(3) -0.1115(2) 0.43747(11) 0.0313(6) Uani 1 1 d . . . . .
H12 H 0.472607 -0.177010 0.451339 0.038 Uiso 1 1 calc R U . . .
C2A C 0.0928(2) 0.1518(2) 0.29542(10) 0.0271(5) Uani 1 1 d . . . . .
H2A H 0.119011 0.206692 0.270452 0.032 Uiso 1 1 calc R U . . .
C13A C 0.4116(2) -0.2506(3) 0.27139(10) 0.0300(6) Uani 1 1 d . . . . .
H13A H 0.388159 -0.288428 0.301530 0.036 Uiso 1 1 calc R U . . .
C7 C 0.7654(3) 0.7556(3) 0.47483(12) 0.0363(7) Uani 1 1 d . . . . .
H7 H 0.814831 0.796092 0.498945 0.044 Uiso 1 1 calc R U . . .
C11A C 0.5382(2) -0.2359(2) 0.20469(10) 0.0283(5) Uani 1 1 d . . . . .
H11A H 0.603671 -0.265265 0.189328 0.034 Uiso 1 1 calc R U . . .
C8 C 0.7266(2) 0.6382(3) 0.48455(11) 0.0322(6) Uani 1 1 d . . . . .
H8 H 0.750668 0.597056 0.515000 0.039 Uiso 1 1 calc R U . . .
C7A C -0.1247(3) 0.3569(3) 0.34817(12) 0.0369(7) Uani 1 1 d . . . . .
H7A H -0.158826 0.435374 0.341029 0.044 Uiso 1 1 calc R U . . .
C15A C 0.0063(3) -0.3306(3) 0.39471(13) 0.0371(7) Uani 1 1 d . . . . .
H15C H 0.003684 -0.380280 0.363173 0.045 Uiso 1 1 calc R U . . .
H15D H -0.069453 -0.294585 0.398639 0.045 Uiso 1 1 calc R U . . .
C5 C 0.6590(2) 0.7590(3) 0.39472(11) 0.0309(6) Uani 1 1 d . . . . .
C8A C -0.0450(2) 0.3113(3) 0.31735(11) 0.0320(6) Uani 1 1 d . . . . .
H8A H -0.024117 0.358464 0.288959 0.038 Uiso 1 1 calc R U . . .
C6 C 0.7326(3) 0.8159(3) 0.42982(12) 0.0361(6) Uani 1 1 d . . . . .
H6 H 0.760979 0.896634 0.423176 0.043 Uiso 1 1 calc R U . . .
C16 C 0.1646(3) 0.5382(3) 0.27263(12) 0.0392(7) Uani 1 1 d . . . . .
H16A H 0.171840 0.459375 0.254452 0.059 Uiso 1 1 calc R U . . .
H16B H 0.205681 0.603539 0.255494 0.059 Uiso 1 1 calc R U . . .
H16C H 0.084844 0.560998 0.273191 0.059 Uiso 1 1 calc R U . . .
C6A C -0.1557(3) 0.2880(3) 0.39011(13) 0.0386(7) Uani 1 1 d . . . . .
H6A H -0.210958 0.320030 0.411280 0.046 Uiso 1 1 calc R U . . .
C14 C 0.6669(4) 0.9271(4) 0.33634(16) 0.0564(10) Uani 1 1 d . . . . .
H14A H 0.640692 0.948554 0.301697 0.085 Uiso 1 1 calc R U . . .
H14B H 0.749324 0.922263 0.338461 0.085 Uiso 1 1 calc R U . . .
H14C H 0.642127 0.991154 0.359672 0.085 Uiso 1 1 calc R U . . .
C16A C 0.0371(4) -0.4128(4) 0.43887(15) 0.0544(9) Uani 1 1 d . . . . .
H16D H 0.113669 -0.444770 0.435842 0.082 Uiso 1 1 calc R U . . .
H16E H -0.015901 -0.482673 0.439419 0.082 Uiso 1 1 calc R U . . .
H16F H 0.033613 -0.365014 0.470276 0.082 Uiso 1 1 calc R U . . .
C14A C -0.2015(5) 0.1428(5) 0.47647(19) 0.0751(14) Uani 1 1 d . . . . .
H14D H -0.276335 0.160533 0.460826 0.113 Uiso 1 1 calc R U . . .
H14E H -0.169547 0.219006 0.491628 0.113 Uiso 1 1 calc R U . . .
H14F H -0.207858 0.079329 0.502774 0.113 Uiso 1 1 calc R U . . .
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 4 7 0.0500
-5 -5 -5 0.0637
-4 4 -8 0.0793
4 -4 8 0.0715
0 0 17 0.0325
0 0 -17 0.0460
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 N2 73.99(8) . . ?
O1 V1 N3A 80.24(7) . 2_655 ?
O4 V1 O1 90.27(8) . . ?
O4 V1 O2 106.69(8) . . ?
O4 V1 N2 159.13(8) . . ?
O4 V1 N3A 77.88(8) . 2_655 ?
O2 V1 O1 151.64(8) . . ?
O2 V1 N2 83.36(8) . . ?
O2 V1 N3A 81.33(8) . 2_655 ?
O5 V1 O1 99.09(9) . . ?
O5 V1 O4 101.43(9) . . ?
O5 V1 O2 99.55(9) . . ?
O5 V1 N2 94.65(9) . . ?
O5 V1 N3A 179.02(9) . 2_655 ?
N2 V1 N3A 85.86(8) . 2_655 ?
O1A V1A N3 76.68(8) . . ?
O1A V1A N2A 73.82(8) . . ?
O4A V1A O1A 96.04(8) . . ?
O4A V1A O2A 101.31(9) . . ?
O4A V1A N3 82.12(8) . . ?
O4A V1A N2A 162.68(9) . . ?
O2A V1A O1A 149.86(9) . . ?
O2A V1A N3 81.48(9) . . ?
O2A V1A N2A 82.80(9) . . ?
O5A V1A O1A 99.58(10) . . ?
O5A V1A O4A 101.34(10) . . ?
O5A V1A O2A 100.91(11) . . ?
O5A V1A N3 175.24(9) . . ?
O5A V1A N2A 94.29(10) . . ?
N2A V1A N3 81.87(8) . . ?
C1 O1 V1 117.32(16) . . ?
C15 O4 V1 126.41(17) . . ?
C1A O1A V1A 118.80(16) . . ?
C4 O2 V1 128.89(16) . . ?
C15A O4A V1A 127.38(19) . . ?
C4A O2A V1A 133.24(18) . . ?
C5 O3 C14 116.9(3) . . ?
N1 N2 V1 116.81(16) . . ?
C2 N2 V1 125.73(18) . . ?
C2 N2 N1 117.2(2) . . ?
C10A N3A V1 123.54(17) . 2_645 ?
C10A N3A C11A 117.4(2) . . ?
C11A N3A V1 117.22(17) . 2_645 ?
C1 N1 N2 107.5(2) . . ?
C14A O3A C5A 120.8(3) . . ?
C10 N3 V1A 123.20(18) . . ?
C10 N3 C11 117.2(2) . . ?
C11 N3 V1A 118.95(18) . . ?
N1A N2A V1A 116.00(15) . . ?
C2A N2A V1A 127.58(18) . . ?
C2A N2A N1A 116.4(2) . . ?
C1A N1A N2A 107.6(2) . . ?
C10 C9 C1 119.6(2) . . ?
C10 C9 C13 118.4(2) . . ?
C13 C9 C1 121.9(2) . . ?
N3A C10A H10A 118.4 . . ?
N3A C10A C9A 123.1(2) . . ?
C9A C10A H10A 118.4 . . ?
O1 C1 N1 123.4(2) . . ?
O1 C1 C9 116.9(2) . . ?
N1 C1 C9 119.7(2) . . ?
C4A C3A C2A 121.2(2) . . ?
C8A C3A C4A 119.6(3) . . ?
C8A C3A C2A 119.1(3) . . ?
O2 C4 C3 122.4(2) . . ?
O2 C4 C5 118.7(2) . . ?
C3 C4 C5 118.8(2) . . ?
C4 C3 C2 120.7(2) . . ?
C8 C3 C4 119.9(3) . . ?
C8 C3 C2 119.3(3) . . ?
O1A C1A C9A 116.4(2) . . ?
N1A C1A O1A 123.8(2) . . ?
N1A C1A C9A 119.8(2) . . ?
C10A C9A C1A 121.8(2) . . ?
C13A C9A C10A 118.6(2) . . ?
C13A C9A C1A 119.6(2) . . ?
N3 C10 C9 123.5(2) . . ?
N3 C10 H10 118.2 . . ?
C9 C10 H10 118.2 . . ?
C13A C12A H12A 120.5 . . ?
C11A C12A H12A 120.5 . . ?
C11A C12A C13A 119.0(3) . . ?
O2A C4A C3A 122.5(2) . . ?
O2A C4A C5A 118.1(3) . . ?
C5A C4A C3A 119.3(2) . . ?
N2 C2 C3 123.4(2) . . ?
N2 C2 H2 118.3 . . ?
C3 C2 H2 118.3 . . ?
C9 C13 H13 120.8 . . ?
C12 C13 C9 118.4(3) . . ?
C12 C13 H13 120.8 . . ?
N3 C11 H11 118.4 . . ?
N3 C11 C12 123.3(2) . . ?
C12 C11 H11 118.4 . . ?
O3A C5A C4A 115.7(3) . . ?
O3A C5A C6A 124.4(3) . . ?
C6A C5A C4A 120.0(3) . . ?
O4 C15 H15A 109.6 . . ?
O4 C15 H15B 109.6 . . ?
O4 C15 C16 110.1(2) . . ?
H15A C15 H15B 108.2 . . ?
C16 C15 H15A 109.6 . . ?
C16 C15 H15B 109.6 . . ?
C13 C12 H12 120.4 . . ?
C11 C12 C13 119.1(3) . . ?
C11 C12 H12 120.4 . . ?
N2A C2A C3A 123.0(2) . . ?
N2A C2A H2A 118.5 . . ?
C3A C2A H2A 118.5 . . ?
C9A C13A H13A 120.6 . . ?
C12A C13A C9A 118.9(2) . . ?
C12A C13A H13A 120.6 . . ?
C8 C7 H7 119.8 . . ?
C8 C7 C6 120.4(3) . . ?
C6 C7 H7 119.8 . . ?
N3A C11A C12A 123.0(2) . . ?
N3A C11A H11A 118.5 . . ?
C12A C11A H11A 118.5 . . ?
C3 C8 H8 119.8 . . ?
C7 C8 C3 120.3(3) . . ?
C7 C8 H8 119.8 . . ?
C8A C7A H7A 120.0 . . ?
C8A C7A C6A 120.1(3) . . ?
C6A C7A H7A 120.0 . . ?
O4A C15A H15C 109.6 . . ?
O4A C15A H15D 109.6 . . ?
O4A C15A C16A 110.3(3) . . ?
H15C C15A H15D 108.1 . . ?
C16A C15A H15C 109.6 . . ?
C16A C15A H15D 109.6 . . ?
O3 C5 C4 114.4(3) . . ?
O3 C5 C6 125.5(3) . . ?
C6 C5 C4 120.0(3) . . ?
C3A C8A H8A 119.8 . . ?
C7A C8A C3A 120.4(3) . . ?
C7A C8A H8A 119.8 . . ?
C7 C6 H6 119.8 . . ?
C5 C6 C7 120.4(3) . . ?
C5 C6 H6 119.8 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C5A C6A C7A 120.6(3) . . ?
C5A C6A H6A 119.7 . . ?
C7A C6A H6A 119.7 . . ?
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 . . ?
C15A C16A H16D 109.5 . . ?
C15A C16A H16E 109.5 . . ?
C15A C16A H16F 109.5 . . ?
H16D C16A H16E 109.5 . . ?
H16D C16A H16F 109.5 . . ?
H16E C16A H16F 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 . . ?
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 1.9706(18) . ?
V1 O4 1.7777(19) . ?
V1 O2 1.8637(19) . ?
V1 O5 1.5956(19) . ?
V1 N2 2.113(2) . ?
V1 N3A 2.413(2) 2_655 ?
V1A O1A 1.9507(19) . ?
V1A O4A 1.7828(19) . ?
V1A O2A 1.851(2) . ?
V1A O5A 1.588(2) . ?
V1A N3 2.409(2) . ?
V1A N2A 2.151(2) . ?
O1 C1 1.307(3) . ?
O4 C15 1.424(3) . ?
O1A C1A 1.308(3) . ?
O2 C4 1.337(3) . ?
O4A C15A 1.431(3) . ?
O2A C4A 1.329(3) . ?
O3 C5 1.363(4) . ?
O3 C14 1.433(4) . ?
N2 N1 1.397(3) . ?
N2 C2 1.282(3) . ?
N3A C10A 1.341(3) . ?
N3A C11A 1.350(3) . ?
N1 C1 1.307(3) . ?
O3A C5A 1.365(4) . ?
O3A C14A 1.359(5) . ?
N3 C10 1.341(3) . ?
N3 C11 1.343(4) . ?
N2A N1A 1.401(3) . ?
N2A C2A 1.291(4) . ?
N1A C1A 1.306(3) . ?
C9 C1 1.474(3) . ?
C9 C10 1.385(4) . ?
C9 C13 1.398(4) . ?
C10A H10A 0.9500 . ?
C10A C9A 1.393(4) . ?
C3A C4A 1.407(4) . ?
C3A C2A 1.450(4) . ?
C3A C8A 1.405(4) . ?
C4 C3 1.406(4) . ?
C4 C5 1.415(4) . ?
C3 C2 1.450(4) . ?
C3 C8 1.405(4) . ?
C1A C9A 1.481(4) . ?
C9A C13A 1.386(4) . ?
C10 H10 0.9500 . ?
C12A H12A 0.9500 . ?
C12A C13A 1.385(4) . ?
C12A C11A 1.382(4) . ?
C4A C5A 1.406(4) . ?
C2 H2 0.9500 . ?
C13 H13 0.9500 . ?
C13 C12 1.383(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.381(4) . ?
C5A C6A 1.380(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.506(4) . ?
C12 H12 0.9500 . ?
C2A H2A 0.9500 . ?
C13A H13A 0.9500 . ?
C7 H7 0.9500 . ?
C7 C8 1.373(4) . ?
C7 C6 1.393(5) . ?
C11A H11A 0.9500 . ?
C8 H8 0.9500 . ?
C7A H7A 0.9500 . ?
C7A C8A 1.372(4) . ?
C7A C6A 1.400(5) . ?
C15A H15C 0.9900 . ?
C15A H15D 0.9900 . ?
C15A C16A 1.495(5) . ?
C5 C6 1.385(4) . ?
C8A H8A 0.9500 . ?
C6 H6 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C6A H6A 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C16A H16D 0.9800 . ?
C16A H16E 0.9800 . ?
C16A H16F 0.9800 . ?
C14A H14D 0.9800 . ?
C14A H14E 0.9800 . ?
C14A H14F 0.9800 . ?
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 C1 N1 9.3(3) . . . . ?
V1 O1 C1 C9 -168.09(17) . . . . ?
V1 O4 C15 C16 175.52(19) . . . . ?
V1 O2 C4 C3 34.9(4) . . . . ?
V1 O2 C4 C5 -148.5(2) . . . . ?
V1 N2 N1 C1 -5.2(3) . . . . ?
V1 N2 C2 C3 -11.4(4) . . . . ?
V1 N3A C10A C9A -164.16(19) 2_645 . . . ?
V1 N3A C11A C12A 166.2(2) 2_645 . . . ?
V1A O1A C1A N1A -1.7(4) . . . . ?
V1A O1A C1A C9A 175.36(17) . . . . ?
V1A O4A C15A C16A -178.2(2) . . . . ?
V1A O2A C4A C3A -32.7(4) . . . . ?
V1A O2A C4A C5A 150.4(2) . . . . ?
V1A N3 C10 C9 -169.50(19) . . . . ?
V1A N3 C11 C12 171.7(2) . . . . ?
V1A N2A N1A C1A 0.2(3) . . . . ?
V1A N2A C2A C3A 6.3(4) . . . . ?
O1 V1 O4 C15 78.1(2) . . . . ?
O1 V1 O2 C4 -79.9(3) . . . . ?
O4 V1 O2 C4 155.7(2) . . . . ?
O1A V1A O4A C15A -106.5(2) . . . . ?
O1A V1A O2A C4A 75.0(3) . . . . ?
O1A C1A C9A C10A 160.8(2) . . . . ?
O1A C1A C9A C13A -21.9(4) . . . . ?
O2 V1 O4 C15 -124.9(2) . . . . ?
O2 C4 C3 C2 3.2(4) . . . . ?
O2 C4 C3 C8 179.5(2) . . . . ?
O2 C4 C5 O3 1.6(4) . . . . ?
O2 C4 C5 C6 -179.9(3) . . . . ?
O4A V1A O2A C4A -161.1(3) . . . . ?
O5 V1 O4 C15 -21.2(2) . . . . ?
O5 V1 O2 C4 50.6(2) . . . . ?
O2A V1A O4A C15A 98.2(2) . . . . ?
O2A C4A C5A O3A -4.1(4) . . . . ?
O2A C4A C5A C6A 176.8(3) . . . . ?
O5A V1A O4A C15A -5.5(2) . . . . ?
O5A V1A O2A C4A -57.0(3) . . . . ?
O3 C5 C6 C7 179.5(3) . . . . ?
N2 V1 O4 C15 118.5(3) . . . . ?
N2 V1 O2 C4 -43.1(2) . . . . ?
N2 N1 C1 O1 -2.3(3) . . . . ?
N2 N1 C1 C9 175.1(2) . . . . ?
N3A V1 O4 C15 158.1(2) 2_655 . . . ?
N3A V1 O2 C4 -129.9(2) 2_655 . . . ?
N3A C10A C9A C1A 176.8(2) . . . . ?
N3A C10A C9A C13A -0.5(4) . . . . ?
N1 N2 C2 C3 175.1(2) . . . . ?
O3A C5A C6A C7A -179.0(3) . . . . ?
N3 V1A O4A C15A 177.9(2) . . . . ?
N3 V1A O2A C4A 118.8(3) . . . . ?
N3 C11 C12 C13 -2.2(4) . . . . ?
N2A V1A O4A C15A -159.5(3) . . . . ?
N2A V1A O2A C4A 36.0(3) . . . . ?
N2A N1A C1A O1A 0.9(4) . . . . ?
N2A N1A C1A C9A -176.0(2) . . . . ?
N1A N2A C2A C3A -175.8(2) . . . . ?
N1A C1A C9A C10A -22.0(4) . . . . ?
N1A C1A C9A C13A 155.2(3) . . . . ?
C9 C13 C12 C11 2.3(4) . . . . ?
C10A N3A C11A C12A 0.9(4) . . . . ?
C10A C9A C13A C12A -0.2(4) . . . . ?
C1 C9 C10 N3 174.9(2) . . . . ?
C1 C9 C13 C12 -176.7(3) . . . . ?
C3A C4A C5A O3A 178.8(3) . . . . ?
C3A C4A C5A C6A -0.2(4) . . . . ?
C4 C3 C2 N2 -12.4(4) . . . . ?
C4 C3 C8 C7 -0.7(4) . . . . ?
C4 C5 C6 C7 1.2(5) . . . . ?
C3 C4 C5 O3 178.3(2) . . . . ?
C3 C4 C5 C6 -3.3(4) . . . . ?
C1A C9A C13A C12A -177.5(3) . . . . ?
C10 N3 C11 C12 0.3(4) . . . . ?
C10 C9 C1 O1 -8.3(3) . . . . ?
C10 C9 C1 N1 174.2(2) . . . . ?
C10 C9 C13 C12 -0.7(4) . . . . ?
C4A C3A C2A N2A 9.4(4) . . . . ?
C4A C3A C8A C7A -0.4(4) . . . . ?
C4A C5A C6A C7A 0.0(5) . . . . ?
C2 N2 N1 C1 168.9(2) . . . . ?
C2 C3 C8 C7 175.7(3) . . . . ?
C13 C9 C1 O1 167.7(2) . . . . ?
C13 C9 C1 N1 -9.8(4) . . . . ?
C13 C9 C10 N3 -1.3(4) . . . . ?
C11 N3 C10 C9 1.5(4) . . . . ?
C2A N2A N1A C1A -177.9(2) . . . . ?
C2A C3A C4A O2A 0.7(4) . . . . ?
C2A C3A C4A C5A 177.6(3) . . . . ?
C2A C3A C8A C7A -177.6(3) . . . . ?
C13A C12A C11A N3A -1.5(5) . . . . ?
C11A N3A C10A C9A 0.2(4) . . . . ?
C11A C12A C13A C9A 1.1(5) . . . . ?
C8 C3 C2 N2 171.2(3) . . . . ?
C8 C7 C6 C5 1.1(5) . . . . ?
C5 C4 C3 C2 -173.4(2) . . . . ?
C5 C4 C3 C8 3.0(4) . . . . ?
C8A C3A C4A O2A -176.4(3) . . . . ?
C8A C3A C4A C5A 0.5(4) . . . . ?
C8A C3A C2A N2A -173.4(3) . . . . ?
C8A C7A C6A C5A 0.1(5) . . . . ?
C6 C7 C8 C3 -1.4(5) . . . . ?
C6A C7A C8A C3A 0.1(5) . . . . ?
C14 O3 C5 C4 -177.0(3) . . . . ?
C14 O3 C5 C6 4.6(5) . . . . ?
C14A O3A C5A C4A 172.6(4) . . . . ?
C14A O3A C5A C6A -8.4(5) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4.8066 4.4174 7.3117 0.4792 0.3363 0.8107
-4.8200 -4.9448 -5.0391 -0.3719 -0.2628 -0.8903
-4.4829 4.4230 -8.2637 -0.2208 -0.9347 0.2785
4.4544 -4.4474 8.2640 0.2205 0.9333 -0.2834
-0.0707 -0.0397 17.1556 0.9508 0.2830 -0.1259
0.1010 0.0821 -17.1574 -0.9499 -0.2827 0.1331
