# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_150K
_database_code_depnum_ccdc_archive 'CCDC 2015517'
loop_
_audit_author_name
_audit_author_address
'Leokadiya Zorina'
;Insitute of Solid State Physics RAS
Russia
;
_audit_update_record             
;
2020-07-10 deposited with the CCDC.	2020-10-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H21 Cl2 N5 O2 V, C2 H6 O, Cl'
_chemical_formula_sum            'C25 H27 Cl3 N5 O3 V'
_chemical_formula_weight         602.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

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'

_cell_length_a                   7.29023(8)
_cell_length_b                   15.38948(19)
_cell_length_c                   22.8617(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2564.92(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    11477
_cell_measurement_theta_min      2.2180
_cell_measurement_theta_max      32.7400

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_F_000             1240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.715
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.123
_exptl_absorpt_coefficient_mu    0.738
_shelx_estimated_absorpt_T_min   0.620
_shelx_estimated_absorpt_T_max   0.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87604
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.917
_oxdiff_exptl_absorpt_empirical_full_max 1.128
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;

_diffrn_ambient_temperature      150(1)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_detector_area_resol_mean 10.4566
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            21049
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.933
_diffrn_reflns_theta_max         32.885
_diffrn_reflns_theta_full        31.000
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             8631
_reflns_number_gt                8290
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.740
_reflns_Friedel_fraction_max     0.868
_reflns_Friedel_fraction_full    0.988

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'DIAMOND 3.1 (Crystal Impact GbR 2005)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0518P)²+0.9687P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3451 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.007(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8631
_refine_ls_number_parameters     340
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0840
_refine_ls_wR_factor_gt          0.0819
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000

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 0.83248(5) 0.99218(2) 0.76654(2) 0.01373(7) Uani 1 1 d . . . . .
Cl1 Cl 0.56697(7) 0.94605(3) 0.81704(2) 0.02013(10) Uani 1 1 d . . . . .
Cl2 Cl 1.10494(7) 1.03898(4) 0.71742(2) 0.02179(10) Uani 1 1 d . . . . .
C1 C 1.0136(3) 0.75021(14) 0.87995(9) 0.0191(4) Uani 1 1 d . . . . .
H1 H 0.9641 0.7437 0.8427 0.023 Uiso 1 1 calc R U . . .
C2 C 1.0540(4) 0.67754(15) 0.91348(11) 0.0241(4) Uani 1 1 d . . . . .
H2 H 1.0321 0.6223 0.8986 0.029 Uiso 1 1 calc R U . . .
C3 C 1.1270(4) 0.68713(16) 0.96931(11) 0.0275(5) Uani 1 1 d . . . . .
H3 H 1.1524 0.6383 0.9919 0.033 Uiso 1 1 calc R U . . .
C4 C 1.1618(4) 0.76947(16) 0.99127(10) 0.0257(4) Uani 1 1 d . . . . .
H4 H 1.2115 0.7756 1.0285 0.031 Uiso 1 1 calc R U . . .
C5 C 1.1233(3) 0.84316(15) 0.95811(10) 0.0226(4) Uani 1 1 d . . . . .
H5 H 1.1475 0.8983 0.9729 0.027 Uiso 1 1 calc R U . . .
C6 C 1.0477(3) 0.83335(13) 0.90235(9) 0.0162(3) Uani 1 1 d . . . . .
C7 C 1.0001(3) 0.90792(13) 0.86533(8) 0.0151(3) Uani 1 1 d . . . . .
C8 C 0.9568(3) 1.17027(14) 0.91715(9) 0.0183(4) Uani 1 1 d . . . . .
H8A H 1.0078 1.1275 0.9430 0.027 Uiso 1 1 calc R U . . .
H8B H 0.8503 1.1958 0.9349 0.027 Uiso 1 1 calc R U . . .
H8C H 1.0464 1.2146 0.9098 0.027 Uiso 1 1 calc R U . . .
C9 C 0.9040(3) 1.12832(12) 0.86109(8) 0.0149(3) Uani 1 1 d . . . . .
C10 C 0.8216(3) 1.17734(12) 0.81223(8) 0.0152(3) Uani 1 1 d . . . . .
C11 C 0.8030(3) 1.26737(13) 0.81096(9) 0.0183(4) Uani 1 1 d . . . . .
H11 H 0.8478 1.3014 0.8414 0.022 Uiso 1 1 calc R U . . .
C12 C 0.7160(3) 1.30530(13) 0.76334(10) 0.0194(4) Uani 1 1 d . . . . .
H12 H 0.7043 1.3654 0.7610 0.023 Uiso 1 1 calc R U . . .
C13 C 0.6466(3) 1.25258(13) 0.71918(9) 0.0181(4) Uani 1 1 d . . . . .
H13 H 0.5835 1.2765 0.6877 0.022 Uiso 1 1 calc R U . . .
C14 C 0.6735(3) 1.16302(12) 0.72302(8) 0.0156(3) Uani 1 1 d . . . . .
C15 C 0.6105(3) 1.09989(13) 0.67889(9) 0.0161(3) Uani 1 1 d . . . . .
C16 C 0.4903(3) 1.12553(14) 0.62925(9) 0.0215(4) Uani 1 1 d . . . . .
H16A H 0.4965 1.0821 0.5992 0.032 Uiso 1 1 calc R U . . .
H16B H 0.5307 1.1803 0.6138 0.032 Uiso 1 1 calc R U . . .
H16C H 0.3661 1.1308 0.6427 0.032 Uiso 1 1 calc R U . . .
C17 C 0.7055(3) 0.87890(13) 0.67354(8) 0.0155(3) Uani 1 1 d . . . . .
C18 C 0.6605(3) 0.79575(12) 0.64516(8) 0.0156(3) Uani 1 1 d . . . . .
C19 C 0.5830(3) 0.79067(13) 0.58919(9) 0.0179(3) Uani 1 1 d . . . . .
H19 H 0.5639 0.8408 0.5673 0.021 Uiso 1 1 calc R U . . .
C20 C 0.5349(3) 0.70998(15) 0.56669(10) 0.0210(4) Uani 1 1 d . . . . .
H20 H 0.4850 0.7061 0.5293 0.025 Uiso 1 1 calc R U . . .
C21 C 0.5609(3) 0.63481(14) 0.59960(10) 0.0215(4) Uani 1 1 d . . . . .
H21 H 0.5247 0.5812 0.5847 0.026 Uiso 1 1 calc R U . . .
C22 C 0.6414(3) 0.63996(13) 0.65499(10) 0.0195(4) Uani 1 1 d . . . . .
H22 H 0.6609 0.5897 0.6767 0.023 Uiso 1 1 calc R U . . .
C23 C 0.6920(3) 0.71997(13) 0.67754(9) 0.0168(3) Uani 1 1 d . . . . .
H23 H 0.7470 0.7234 0.7142 0.020 Uiso 1 1 calc R U . . .
N1 N 0.9798(2) 0.98783(11) 0.88902(7) 0.0157(3) Uani 1 1 d D . . . .
H1N H 0.955(4) 0.993(2) 0.9238(11) 0.019 Uiso 1 1 d D U . . .
N2 N 0.9167(2) 1.04677(11) 0.84836(7) 0.0144(3) Uani 1 1 d . . . . .
N3 N 0.7621(2) 1.12635(10) 0.76825(7) 0.0144(3) Uani 1 1 d . . . . .
N4 N 0.6695(3) 1.02265(10) 0.69073(7) 0.0159(3) Uani 1 1 d . . . . .
N5 N 0.6239(3) 0.95317(11) 0.65612(8) 0.0186(3) Uani 1 1 d D . . . .
H5N H 0.556(2) 0.95638(15) 0.6283(8) 0.022 Uiso 1 1 calc DR U . . .
O1 O 0.9761(2) 0.89849(10) 0.81162(6) 0.0179(3) Uani 1 1 d . . . . .
O2 O 0.8131(2) 0.88165(10) 0.71602(7) 0.0208(3) Uani 1 1 d . . . . .
Cl3 Cl 0.84243(10) 1.01353(4) 1.01428(2) 0.02938(13) Uani 1 1 d . . . . .
C1S C 0.4914(6) 0.6124(3) 0.4310(2) 0.0564(9) Uani 1 1 d . . . . .
H1SA H 0.3886 0.5869 0.4509 0.085 Uiso 1 1 calc R U . . .
H1SB H 0.4667 0.6149 0.3898 0.085 Uiso 1 1 calc R U . . .
H1SC H 0.5117 0.6701 0.4456 0.085 Uiso 1 1 calc R U . . .
C2S C 0.6602(5) 0.5579(2) 0.44163(13) 0.0393(6) Uani 1 1 d . . . . .
H2SA H 0.7317 0.5816 0.4736 0.047 Uiso 1 1 calc R U . . .
H2SB H 0.6261 0.4987 0.4513 0.047 Uiso 1 1 calc R U . . .
O1S O 0.7619(4) 0.5600(2) 0.38928(14) 0.0578(7) Uani 1 1 d . . . . .
H1S H 0.6943 0.5485 0.3617 0.087 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 2.0586(15) . ?
V1 O2 2.0609(15) . ?
V1 N3 2.1280(16) . ?
V1 N2 2.1404(17) . ?
V1 N4 2.1531(17) . ?
V1 Cl1 2.3629(6) . ?
V1 Cl2 2.3927(6) . ?
C1 C2 1.387(3) . ?
C1 C6 1.400(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.391(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.386(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.393(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.397(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.468(3) . ?
C7 O1 1.249(2) . ?
C7 N1 1.352(3) . ?
C8 C9 1.486(3) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N2 1.292(2) . ?
C9 C10 1.476(3) . ?
C10 N3 1.347(3) . ?
C10 C11 1.393(3) . ?
C11 C12 1.388(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.390(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.395(3) . ?
C13 H13 0.9300 . ?
C14 N3 1.343(3) . ?
C14 C15 1.474(3) . ?
C15 N4 1.293(2) . ?
C15 C16 1.487(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 O2 1.249(2) . ?
C17 N5 1.348(3) . ?
C17 C18 1.472(3) . ?
C18 C23 1.400(3) . ?
C18 C19 1.401(3) . ?
C19 C20 1.389(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.393(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.398(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.385(3) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
N1 N2 1.378(2) . ?
N1 H1N 0.82(2) . ?
N4 N5 1.371(2) . ?
N5 H5N 0.81(2) . ?
C1S C2S 1.509(6) . ?
C1S H1SA 0.9600 . ?
C1S H1SB 0.9600 . ?
C1S H1SC 0.9600 . ?
C2S O1S 1.408(4) . ?
C2S H2SA 0.9700 . ?
C2S H2SB 0.9700 . ?
O1S H1S 0.8200 . ?

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 74.78(6) . . ?
O1 V1 N3 142.48(6) . . ?
O2 V1 N3 142.62(7) . . ?
O1 V1 N2 72.03(6) . . ?
O2 V1 N2 146.45(6) . . ?
N3 V1 N2 70.87(6) . . ?
O1 V1 N4 146.75(6) . . ?
O2 V1 N4 71.98(6) . . ?
N3 V1 N4 70.75(6) . . ?
N2 V1 N4 140.92(6) . . ?
O1 V1 Cl1 87.80(5) . . ?
O2 V1 Cl1 88.25(5) . . ?
N3 V1 Cl1 94.88(5) . . ?
N2 V1 Cl1 85.75(5) . . ?
N4 V1 Cl1 90.38(5) . . ?
O1 V1 Cl2 91.35(5) . . ?
O2 V1 Cl2 92.43(5) . . ?
N3 V1 Cl2 85.23(5) . . ?
N2 V1 Cl2 93.09(5) . . ?
N4 V1 Cl2 90.84(5) . . ?
Cl1 V1 Cl2 178.73(2) . . ?
C2 C1 C6 119.8(2) . . ?
C2 C1 H1 120.1 . . ?
C6 C1 H1 120.1 . . ?
C1 C2 C3 120.2(2) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C4 C3 C2 120.0(2) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.7(2) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C6 119.2(2) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C5 C6 C1 120.16(19) . . ?
C5 C6 C7 122.35(19) . . ?
C1 C6 C7 117.48(18) . . ?
O1 C7 N1 118.97(18) . . ?
O1 C7 C6 120.62(18) . . ?
N1 C7 C6 120.40(17) . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 110.79(17) . . ?
N2 C9 C8 126.74(18) . . ?
C10 C9 C8 122.43(17) . . ?
N3 C10 C11 122.18(19) . . ?
N3 C10 C9 113.48(16) . . ?
C11 C10 C9 124.34(18) . . ?
C12 C11 C10 118.63(19) . . ?
C12 C11 H11 120.7 . . ?
C10 C11 H11 120.7 . . ?
C11 C12 C13 119.35(18) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C12 C13 C14 118.66(19) . . ?
C12 C13 H13 120.7 . . ?
C14 C13 H13 120.7 . . ?
N3 C14 C13 122.08(18) . . ?
N3 C14 C15 113.57(17) . . ?
C13 C14 C15 124.35(18) . . ?
N4 C15 C14 111.04(17) . . ?
N4 C15 C16 126.85(19) . . ?
C14 C15 C16 122.09(17) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O2 C17 N5 118.54(18) . . ?
O2 C17 C18 120.81(18) . . ?
N5 C17 C18 120.57(18) . . ?
C23 C18 C19 120.17(18) . . ?
C23 C18 C17 117.03(17) . . ?
C19 C18 C17 122.76(18) . . ?
C20 C19 C18 119.34(19) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C19 C20 C21 120.5(2) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C20 C21 C22 120.0(2) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C23 C22 C21 119.97(19) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C18 119.99(19) . . ?
C22 C23 H23 120.0 . . ?
C18 C23 H23 120.0 . . ?
C7 N1 N2 111.41(16) . . ?
C7 N1 H1N 120(2) . . ?
N2 N1 H1N 121(2) . . ?
C9 N2 N1 120.75(17) . . ?
C9 N2 V1 123.91(14) . . ?
N1 N2 V1 115.27(12) . . ?
C10 N3 C14 118.99(17) . . ?
C10 N3 V1 120.08(13) . . ?
C14 N3 V1 120.62(13) . . ?
C15 N4 N5 121.05(17) . . ?
C15 N4 V1 123.53(14) . . ?
N5 N4 V1 115.36(12) . . ?
C17 N5 N4 112.57(17) . . ?
C17 N5 H5N 123.7 . . ?
N4 N5 H5N 123.7 . . ?
C7 O1 V1 118.82(13) . . ?
C17 O2 V1 120.45(13) . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
O1S C2S C1S 106.3(3) . . ?
O1S C2S H2SA 110.5 . . ?
C1S C2S H2SA 110.5 . . ?
O1S C2S H2SB 110.5 . . ?
C1S C2S H2SB 110.5 . . ?
H2SA C2S H2SB 108.7 . . ?
C2S O1S H1S 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N Cl3 0.82(2) 2.25(2) 3.0595(17) 171(3) .
N5 H5N Cl3 0.81 2.75 3.2920(19) 126.1 2_674
N5 H5N O1S 0.81 2.19 2.843(4) 137.5 4_466
O1S H1S Cl2 0.82 2.35 3.095(3) 152.1 4_466
C3 H3 Cl3 0.93 2.72 3.485(2) 140.0 4_567
C8 H8A Cl3 0.96 2.68 3.383(2) 130.5 .
C11 H11 O1S 0.93 2.53 3.239(4) 133.5 2_675
C13 H13 Cl1 0.93 2.83 3.460(2) 125.9 3_656
C16 H16A Cl3 0.96 2.70 3.602(2) 156.0 2_674
C19 H19 Cl3 0.93 2.64 3.508(2) 156.0 2_674
C22 H22 Cl1 0.93 2.77 3.409(2) 126.9 3_646
C1S H1SA Cl3 0.96 2.18 3.131(5) 171.2 3_646
C1S H1SB O2 0.96 2.67 3.605(5) 166.0 4_466

_refine_diff_density_max         0.368
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.071

_shelxl_version_number           2013-2

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3_150K
_database_code_depnum_ccdc_archive 'CCDC 2015519'
loop_
_audit_author_name
_audit_author_address
'Leokadiya Zorina'
;Insitute of Solid State Physics RAS
Russia
;
_audit_update_record             
;
2020-07-10 deposited with the CCDC.	2020-10-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H27 N5 O4 V, C H4 O, Cl'
_chemical_formula_sum            'C26 H31 Cl N5 O5 V'
_chemical_formula_weight         579.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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'

_cell_length_a                   19.5934(3)
_cell_length_b                   7.49770(8)
_cell_length_c                   20.3843(3)
_cell_angle_alpha                90
_cell_angle_beta                 112.3819(18)
_cell_angle_gamma                90
_cell_volume                     2768.98(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    13692
_cell_measurement_theta_min      2.0280
_cell_measurement_theta_max      31.0730

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_F_000             1208
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    0.499
_shelx_estimated_absorpt_T_min   0.875
_shelx_estimated_absorpt_T_max   0.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.95977
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.930
_oxdiff_exptl_absorpt_empirical_full_max 1.071
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150(1)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_detector_area_resol_mean 10.4566
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            27429
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_av_R_equivalents  0.0149
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.021
_diffrn_reflns_theta_max         31.155
_diffrn_reflns_theta_full        29.000
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             8079
_reflns_number_gt                7041
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'DIAMOND 3.1 (Crystal Impact GbR 2005)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0416P)²+1.2810P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8079
_refine_ls_number_parameters     357
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0835
_refine_ls_wR_factor_gt          0.0789
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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 0.27743(2) 0.92173(2) 0.48998(2) 0.01461(5) Uani 1 1 d . . . . .
O1 O 0.18816(4) 0.88687(11) 0.40011(4) 0.01991(16) Uani 1 1 d . . . . .
O2 O 0.19257(4) 1.02729(12) 0.51006(4) 0.02055(16) Uani 1 1 d . . . . .
O3 O 0.29950(5) 1.16827(11) 0.45441(5) 0.02237(17) Uani 1 1 d . . . . .
H3A H 0.3200(10) 1.235(2) 0.4875(10) 0.034 Uiso 1 1 d . U . . .
O4 O 0.25954(5) 0.67560(12) 0.52577(5) 0.02265(18) Uani 1 1 d . . . . .
H4A H 0.2930(10) 0.604(2) 0.5381(10) 0.034 Uiso 1 1 d . U . . .
N1 N 0.25830(5) 0.74132(13) 0.34885(5) 0.01914(18) Uani 1 1 d . . . . .
N2 N 0.31135(5) 0.78850(12) 0.41386(5) 0.01728(18) Uani 1 1 d . . . . .
N3 N 0.39427(5) 0.87856(12) 0.53596(5) 0.01666(17) Uani 1 1 d . . . . .
N4 N 0.31920(5) 1.01683(13) 0.59744(5) 0.01729(18) Uani 1 1 d . . . . .
N5 N 0.27063(5) 1.09287(13) 0.62394(5) 0.01920(19) Uani 1 1 d . . . . .
C1 C 0.05985(6) 0.83496(16) 0.28450(6) 0.0203(2) Uani 1 1 d . . . . .
H1 H 0.058752 0.893119 0.325489 0.024 Uiso 1 1 calc R U . . .
C2 C -0.00478(7) 0.81518(17) 0.22531(7) 0.0236(2) Uani 1 1 d . . . . .
H2 H -0.049901 0.861103 0.225476 0.028 Uiso 1 1 calc R U . . .
C3 C -0.00343(7) 0.72809(17) 0.16575(7) 0.0253(2) Uani 1 1 d . . . . .
H3 H -0.047711 0.714477 0.125095 0.030 Uiso 1 1 calc R U . . .
C4 C 0.06252(7) 0.66071(18) 0.16541(7) 0.0263(2) Uani 1 1 d . . . . .
H4 H 0.063013 0.600019 0.124681 0.032 Uiso 1 1 calc R U . . .
C5 C 0.12774(7) 0.68166(16) 0.22434(6) 0.0226(2) Uani 1 1 d . . . . .
H5 H 0.172805 0.636243 0.223852 0.027 Uiso 1 1 calc R U . . .
C6 C 0.12664(6) 0.77004(14) 0.28440(6) 0.0178(2) Uani 1 1 d . . . . .
C7 C 0.19449(6) 0.80087(14) 0.34797(6) 0.0172(2) Uani 1 1 d . . . . .
C8 C 0.40520(7) 0.65054(17) 0.37619(7) 0.0238(2) Uani 1 1 d . . . . .
H8A H 0.364096 0.582662 0.342348 0.036 Uiso 1 1 calc R U . . .
H8B H 0.445289 0.568751 0.402557 0.036 Uiso 1 1 calc R U . . .
H8C H 0.423086 0.737252 0.350467 0.036 Uiso 1 1 calc R U . . .
C9 C 0.37951(6) 0.74639(14) 0.42674(6) 0.0180(2) Uani 1 1 d . . . . .
C10 C 0.42910(6) 0.80065(14) 0.49768(6) 0.0176(2) Uani 1 1 d . . . . .
C11 C 0.50555(6) 0.77633(16) 0.52531(7) 0.0218(2) Uani 1 1 d . . . . .
H11 H 0.529500 0.722890 0.497575 0.026 Uiso 1 1 calc R U . . .
C12 C 0.54573(6) 0.83216(16) 0.59432(7) 0.0235(2) Uani 1 1 d . . . . .
H12 H 0.597828 0.817919 0.614090 0.028 Uiso 1 1 calc R U . . .
C13 C 0.50996(6) 0.90868(16) 0.63446(7) 0.0213(2) Uani 1 1 d . . . . .
H13 H 0.536817 0.945661 0.681935 0.026 Uiso 1 1 calc R U . . .
C14 C 0.43356(6) 0.92988(14) 0.60329(6) 0.0175(2) Uani 1 1 d . . . . .
C15 C 0.38830(6) 1.00934(15) 0.63861(6) 0.0185(2) Uani 1 1 d . . . . .
C16 C 0.42051(7) 1.07498(18) 0.71321(7) 0.0263(3) Uani 1 1 d . . . . .
H16A H 0.381696 1.130565 0.725525 0.039 Uiso 1 1 calc R U . . .
H16B H 0.459084 1.162968 0.717926 0.039 Uiso 1 1 calc R U . . .
H16C H 0.441920 0.974552 0.745229 0.039 Uiso 1 1 calc R U . . .
C17 C 0.20518(6) 1.09242(14) 0.57213(6) 0.0175(2) Uani 1 1 d . . . . .
C18 C 0.14257(6) 1.17571(14) 0.58477(6) 0.0179(2) Uani 1 1 d . . . . .
C19 C 0.15254(7) 1.25817(17) 0.64918(7) 0.0239(2) Uani 1 1 d . . . . .
H19 H 0.199668 1.257373 0.686863 0.029 Uiso 1 1 calc R U . . .
C20 C 0.09316(8) 1.34145(18) 0.65793(8) 0.0297(3) Uani 1 1 d . . . . .
H20 H 0.099882 1.398589 0.701550 0.036 Uiso 1 1 calc R U . . .
C21 C 0.02425(8) 1.34144(18) 0.60328(8) 0.0310(3) Uani 1 1 d . . . . .
H21 H -0.016098 1.398811 0.609498 0.037 Uiso 1 1 calc R U . . .
C22 C 0.01404(7) 1.2582(2) 0.53975(7) 0.0305(3) Uani 1 1 d . . . . .
H22 H -0.033332 1.257815 0.502436 0.037 Uiso 1 1 calc R U . . .
C23 C 0.07327(7) 1.17496(17) 0.53049(7) 0.0233(2) Uani 1 1 d . . . . .
H23 H 0.066184 1.117447 0.486850 0.028 Uiso 1 1 calc R U . . .
C24 C 0.24634(9) 1.2646(2) 0.39648(9) 0.0385(3) Uani 1 1 d . . . . .
H24A H 0.237997 1.201816 0.351914 0.058 Uiso 1 1 calc R U . . .
H24B H 0.264992 1.384815 0.394309 0.058 Uiso 1 1 calc R U . . .
H24C H 0.199766 1.272836 0.403697 0.058 Uiso 1 1 calc R U . . .
C25 C 0.18994(7) 0.5958(2) 0.51518(9) 0.0350(3) Uani 1 1 d . . . . .
H25A H 0.176790 0.621701 0.556017 0.052 Uiso 1 1 calc R U . . .
H25B H 0.193238 0.466446 0.510184 0.052 Uiso 1 1 calc R U . . .
H25C H 0.152035 0.644552 0.472065 0.052 Uiso 1 1 calc R U . . .
Cl2 Cl 0.38675(2) 0.42512(4) 0.56775(2) 0.02395(7) Uani 1 1 d . . . . .
O1S O 0.39108(6) 0.60069(16) 0.71379(6) 0.0377(2) Uani 1 1 d . . . . .
C1S C 0.31630(9) 0.5860(3) 0.70492(9) 0.0435(4) Uani 1 1 d . . . . .
H1S1 H 0.312692 0.581542 0.751544 0.065 Uiso 1 1 calc R U . . .
H1S2 H 0.295339 0.476757 0.678558 0.065 Uiso 1 1 calc R U . . .
H1S3 H 0.288908 0.689542 0.678507 0.065 Uiso 1 1 calc R U . . .
H1S H 0.3943(13) 0.564(3) 0.6764(13) 0.065 Uiso 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 2.0109(8) . ?
V1 O2 2.0193(8) . ?
V1 O4 2.0629(9) . ?
V1 O3 2.0901(9) . ?
V1 N3 2.1424(9) . ?
V1 N4 2.1473(10) . ?
V1 N2 2.1524(9) . ?
O1 C7 1.2889(13) . ?
O2 C17 1.2892(14) . ?
O3 C24 1.4367(16) . ?
O3 H3A 0.811(19) . ?
O4 C25 1.4282(15) . ?
O4 H4A 0.810(19) . ?
N1 C7 1.3212(14) . ?
N1 N2 1.3831(14) . ?
N2 C9 1.2980(14) . ?
N3 C14 1.3491(15) . ?
N3 C10 1.3494(14) . ?
N4 C15 1.2943(15) . ?
N4 N5 1.3835(13) . ?
N5 C17 1.3147(15) . ?
C1 C2 1.3847(17) . ?
C1 C6 1.3970(16) . ?
C1 H1 0.9500 . ?
C2 C3 1.3876(17) . ?
C2 H2 0.9500 . ?
C3 C4 1.3899(18) . ?
C3 H3 0.9500 . ?
C4 C5 1.3899(18) . ?
C4 H4 0.9500 . ?
C5 C6 1.3994(16) . ?
C5 H5 0.9500 . ?
C6 C7 1.4793(16) . ?
C8 C9 1.4922(15) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.4597(16) . ?
C10 C11 1.3972(15) . ?
C11 C12 1.3894(18) . ?
C11 H11 0.9500 . ?
C12 C13 1.3880(17) . ?
C12 H12 0.9500 . ?
C13 C14 1.3947(16) . ?
C13 H13 0.9500 . ?
C14 C15 1.4648(15) . ?
C15 C16 1.4908(16) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.4839(15) . ?
C18 C23 1.3870(17) . ?
C18 C19 1.3962(16) . ?
C19 C20 1.3903(17) . ?
C19 H19 0.9500 . ?
C20 C21 1.385(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.3816(19) . ?
C21 H21 0.9500 . ?
C22 C23 1.3924(17) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
O1S C1S 1.4107(19) . ?
O1S H1S 0.84(2) . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?

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 74.80(3) . . ?
O1 V1 O4 89.99(4) . . ?
O2 V1 O4 90.86(4) . . ?
O1 V1 O3 91.26(4) . . ?
O2 V1 O3 91.07(4) . . ?
O4 V1 O3 177.92(3) . . ?
O1 V1 N3 142.45(4) . . ?
O2 V1 N3 142.73(4) . . ?
O4 V1 N3 90.42(3) . . ?
O3 V1 N3 87.57(4) . . ?
O1 V1 N4 146.50(3) . . ?
O2 V1 N4 71.73(3) . . ?
O4 V1 N4 89.22(4) . . ?
O3 V1 N4 90.65(4) . . ?
N3 V1 N4 71.05(4) . . ?
O1 V1 N2 71.53(3) . . ?
O2 V1 N2 146.33(4) . . ?
O4 V1 N2 88.88(4) . . ?
O3 V1 N2 89.94(4) . . ?
N3 V1 N2 70.94(4) . . ?
N4 V1 N2 141.92(4) . . ?
C7 O1 V1 119.52(7) . . ?
C17 O2 V1 118.84(7) . . ?
C24 O3 V1 123.28(8) . . ?
C24 O3 H3A 110.4(13) . . ?
V1 O3 H3A 111.0(13) . . ?
C25 O4 V1 127.04(8) . . ?
C25 O4 H4A 112.6(12) . . ?
V1 O4 H4A 118.3(12) . . ?
C7 N1 N2 106.78(9) . . ?
C9 N2 N1 118.14(9) . . ?
C9 N2 V1 122.91(8) . . ?
N1 N2 V1 118.93(7) . . ?
C14 N3 C10 119.57(10) . . ?
C14 N3 V1 120.18(7) . . ?
C10 N3 V1 120.26(8) . . ?
C15 N4 N5 118.03(10) . . ?
C15 N4 V1 123.04(8) . . ?
N5 N4 V1 118.92(7) . . ?
C17 N5 N4 106.91(9) . . ?
C2 C1 C6 120.51(11) . . ?
C2 C1 H1 119.7 . . ?
C6 C1 H1 119.7 . . ?
C1 C2 C3 119.80(11) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C2 C3 C4 120.20(12) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 120.34(11) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 119.62(11) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C5 119.52(11) . . ?
C1 C6 C7 118.31(10) . . ?
C5 C6 C7 122.16(10) . . ?
O1 C7 N1 123.07(10) . . ?
O1 C7 C6 117.64(10) . . ?
N1 C7 C6 119.29(10) . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 112.21(10) . . ?
N2 C9 C8 124.68(11) . . ?
C10 C9 C8 123.10(10) . . ?
N3 C10 C11 121.60(11) . . ?
N3 C10 C9 113.65(10) . . ?
C11 C10 C9 124.75(10) . . ?
C12 C11 C10 118.42(11) . . ?
C12 C11 H11 120.8 . . ?
C10 C11 H11 120.8 . . ?
C13 C12 C11 120.18(11) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 118.28(11) . . ?
C12 C13 H13 120.9 . . ?
C14 C13 H13 120.9 . . ?
N3 C14 C13 121.91(11) . . ?
N3 C14 C15 113.47(10) . . ?
C13 C14 C15 124.61(11) . . ?
N4 C15 C14 112.25(10) . . ?
N4 C15 C16 125.38(10) . . ?
C14 C15 C16 122.36(10) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O2 C17 N5 123.59(10) . . ?
O2 C17 C18 117.87(10) . . ?
N5 C17 C18 118.52(10) . . ?
C23 C18 C19 119.73(10) . . ?
C23 C18 C17 118.87(10) . . ?
C19 C18 C17 121.38(11) . . ?
C20 C19 C18 119.68(12) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C21 C20 C19 120.26(12) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C22 C21 C20 120.18(11) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C21 C22 C23 119.92(12) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C18 C23 C22 120.22(12) . . ?
C18 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
O3 C24 H24A 109.5 . . ?
O3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O4 C25 H25A 109.5 . . ?
O4 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O4 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C1S O1S H1S 107.1(17) . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?

_refine_diff_density_max         0.433
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.051

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2_150K
_database_code_depnum_ccdc_archive 'CCDC 2015518'
loop_
_audit_author_name
_audit_author_address
'Leokadiya Zorina'
;Insitute of Solid State Physics RAS
Russia
;
_audit_update_record             
;
2020-07-10 deposited with the CCDC.	2020-10-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H20 N7 O2 S2 V, 0.5(C2 H3 N), 0.5(C H4 O)'
_chemical_formula_sum            'C26.50 H23.50 N7.50 O2.50 S2 V'
_chemical_formula_weight         602.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

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'

_cell_length_a                   13.9738(2)
_cell_length_b                   14.3549(2)
_cell_length_c                   27.3124(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5478.66(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    13229
_cell_measurement_theta_min      1.5970
_cell_measurement_theta_max      30.8830

_exptl_crystal_description       stick
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_F_000             2480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.534
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.557
_shelx_estimated_absorpt_T_min   0.755
_shelx_estimated_absorpt_T_max   0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96320
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.950
_oxdiff_exptl_absorpt_empirical_full_max 1.079
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150(1)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_detector_area_resol_mean 10.4566
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            30256
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.603
_diffrn_reflns_theta_max         31.267
_diffrn_reflns_theta_full        29.500
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_point_group_measured_fraction_full 0.967
_reflns_number_total             15367
_reflns_number_gt                13382
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.747
_reflns_Friedel_fraction_max     0.807
_reflns_Friedel_fraction_full    0.940

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.1 (Crystal Impact GbR 2005)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0407P)²+1.5708P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 5144 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         15367
_refine_ls_number_parameters     785
_refine_ls_number_restraints     152
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.0868
_refine_ls_wR_factor_gt          0.0811
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.71156(3) 0.08363(3) 0.09644(2) 0.02674(10) Uani 1 1 d . . . . .
C24A C 0.7862(8) 0.2852(9) 0.1117(5) 0.030(2) Uani 0.7 1 d . U P A 1
S1A S 0.84634(11) 0.38365(12) 0.10728(6) 0.0389(3) Uani 0.7 1 d . . P A 1
C24B C 0.7702(17) 0.2999(19) 0.1138(12) 0.023(4) Uani 0.3 1 d . U P A 2
S1B S 0.8139(3) 0.4018(3) 0.12191(16) 0.0444(8) Uani 0.3 1 d . . P A 2
S2 S 0.64851(7) -0.24666(6) 0.08484(4) 0.0511(2) Uani 1 1 d . . . . .
C1 C 1.03593(18) 0.0813(2) 0.04738(10) 0.0305(6) Uani 1 1 d . . . . .
H1 H 1.019257 0.074451 0.080903 0.037 Uiso 1 1 calc R U . . .
C2 C 1.13149(19) 0.0757(2) 0.03296(11) 0.0351(6) Uani 1 1 d . . . . .
H2 H 1.180046 0.065580 0.056716 0.042 Uiso 1 1 calc R U . . .
C3 C 1.1555(2) 0.0847(2) -0.01578(12) 0.0401(7) Uani 1 1 d . . . . .
H3 H 1.220671 0.080979 -0.025507 0.048 Uiso 1 1 calc R U . . .
C4 C 1.0847(2) 0.0994(3) -0.05077(12) 0.0434(8) Uani 1 1 d . . . . .
H4 H 1.101347 0.104727 -0.084372 0.052 Uiso 1 1 calc R U . . .
C5 C 0.9896(2) 0.1062(2) -0.03640(11) 0.0367(6) Uani 1 1 d . . . . .
H5 H 0.941244 0.117117 -0.060154 0.044 Uiso 1 1 calc R U . . .
C6 C 0.96515(18) 0.09698(19) 0.01260(10) 0.0274(5) Uani 1 1 d . . . . .
C7 C 0.86399(18) 0.1000(2) 0.02852(10) 0.0280(5) Uani 1 1 d . . . . .
C8 C 0.6307(2) 0.1736(2) -0.05458(10) 0.0365(6) Uani 1 1 d . . . . .
H8A H 0.608264 0.238047 -0.057216 0.055 Uiso 1 1 calc R U . . .
H8B H 0.586608 0.132318 -0.072133 0.055 Uiso 1 1 calc R U . . .
H8C H 0.694761 0.168486 -0.068969 0.055 Uiso 1 1 calc R U . . .
C9 C 0.63458(19) 0.1460(2) -0.00212(10) 0.0287(5) Uani 1 1 d . . . . .
C10 C 0.54974(19) 0.1391(2) 0.02854(10) 0.0306(6) Uani 1 1 d . . . . .
C11 C 0.4564(2) 0.1600(2) 0.01337(12) 0.0378(6) Uani 1 1 d . . . . .
H11 H 0.443903 0.178413 -0.019419 0.045 Uiso 1 1 calc R U . . .
C12 C 0.3832(2) 0.1533(2) 0.04680(14) 0.0441(8) Uani 1 1 d . . . . .
H12 H 0.319642 0.168231 0.037297 0.053 Uiso 1 1 calc R U . . .
C13 C 0.40174(19) 0.1251(2) 0.09393(13) 0.0416(7) Uani 1 1 d . . . . .
H13 H 0.351376 0.119484 0.117108 0.050 Uiso 1 1 calc R U . . .
C14 C 0.49568(19) 0.1050(2) 0.10704(11) 0.0341(6) Uani 1 1 d . . . . .
C15 C 0.5265(2) 0.0770(2) 0.15669(11) 0.0367(6) Uani 1 1 d . . . . .
C16 C 0.4555(3) 0.0578(3) 0.19590(15) 0.0577(10) Uani 1 1 d . . . . .
H16A H 0.397847 0.030227 0.181453 0.087 Uiso 1 1 calc R U . . .
H16B H 0.438672 0.116117 0.212423 0.087 Uiso 1 1 calc R U . . .
H16C H 0.483068 0.014285 0.219688 0.087 Uiso 1 1 calc R U . . .
C17 C 0.7589(2) 0.0374(2) 0.19772(11) 0.0353(6) Uani 1 1 d . . . . .
C18 C 0.8216(2) 0.0145(2) 0.23937(11) 0.0385(7) Uani 1 1 d . . . . .
C19 C 0.7878(3) -0.0080(3) 0.28551(11) 0.0513(8) Uani 1 1 d . . . . .
H19 H 0.721002 -0.008138 0.291896 0.062 Uiso 1 1 calc R U . . .
C20 C 0.8525(4) -0.0304(3) 0.32260(13) 0.0646(12) Uani 1 1 d . . . . .
H20 H 0.829412 -0.046447 0.354208 0.078 Uiso 1 1 calc R U . . .
C21 C 0.9492(3) -0.0295(3) 0.31387(14) 0.0595(11) Uani 1 1 d . . . . .
H21 H 0.992635 -0.045155 0.339356 0.071 Uiso 1 1 calc R U . . .
C22 C 0.9837(3) -0.0059(3) 0.26796(14) 0.0566(10) Uani 1 1 d . . . . .
H22 H 1.050696 -0.004298 0.262040 0.068 Uiso 1 1 calc R U . . .
C23 C 0.9201(3) 0.0154(2) 0.23079(13) 0.0454(8) Uani 1 1 d . . . . .
H23 H 0.943651 0.030681 0.199169 0.054 Uiso 1 1 calc R U . . .
C25 C 0.66940(19) -0.1351(2) 0.08339(11) 0.0346(6) Uani 1 1 d . . . . .
N1 N 0.79894(15) 0.13381(17) -0.00144(8) 0.0286(5) Uani 1 1 d . . . . .
N2 N 0.71185(16) 0.12575(16) 0.02191(8) 0.0264(4) Uani 1 1 d . . . . .
N3 N 0.56803(15) 0.11326(16) 0.07498(8) 0.0291(5) Uani 1 1 d . . . . .
N4 N 0.61879(17) 0.07177(18) 0.15966(9) 0.0323(5) Uani 1 1 d . . . . .
N5 N 0.66365(19) 0.04931(19) 0.20307(9) 0.0369(6) Uani 1 1 d . . . . .
H5N H 0.634(3) 0.056(3) 0.2286(14) 0.044 Uiso 1 1 d . U . . .
N6 N 0.74084(16) 0.22028(18) 0.11249(8) 0.0318(5) Uani 1 1 d . . . . .
N7 N 0.68406(16) -0.05504(19) 0.08367(9) 0.0352(5) Uani 1 1 d . . . . .
O1 O 0.84440(13) 0.06801(15) 0.07121(7) 0.0331(4) Uani 1 1 d . . . . .
O2 O 0.79325(15) 0.04431(16) 0.15606(7) 0.0370(5) Uani 1 1 d . . . . .
V2 V 0.21498(3) 0.83802(3) 0.13857(2) 0.02432(9) Uani 1 1 d . . . . .
S11 S 0.16544(6) 1.16584(6) 0.17309(3) 0.04444(19) Uani 1 1 d . . . . .
S12 S 0.28018(6) 0.54658(7) 0.06120(3) 0.0497(2) Uani 1 1 d . . . . .
C31 C 0.46430(19) 0.8981(2) 0.01789(10) 0.0304(6) Uani 1 1 d . . . . .
H31 H 0.480074 0.896515 0.051716 0.036 Uiso 1 1 calc R U . . .
C32 C 0.53521(19) 0.9091(2) -0.01683(11) 0.0352(6) Uani 1 1 d . . . . .
H32 H 0.599872 0.915889 -0.006688 0.042 Uiso 1 1 calc R U . . .
C33 C 0.51321(19) 0.9104(2) -0.06619(10) 0.0321(6) Uani 1 1 d . . . . .
H33 H 0.562700 0.916610 -0.089815 0.039 Uiso 1 1 calc R U . . .
C34 C 0.4185(2) 0.9027(2) -0.08113(10) 0.0331(6) Uani 1 1 d . . . . .
H34 H 0.403328 0.903916 -0.115025 0.040 Uiso 1 1 calc R U . . .
C35 C 0.34623(19) 0.8931(2) -0.04689(10) 0.0321(6) Uani 1 1 d . . . . .
H35 H 0.281424 0.889235 -0.057198 0.038 Uiso 1 1 calc R U . . .
C36 C 0.36882(18) 0.88925(19) 0.00283(9) 0.0264(5) Uani 1 1 d . . . . .
C37 C 0.29566(18) 0.87637(19) 0.04119(9) 0.0269(5) Uani 1 1 d . . . . .
C38 C 0.00108(19) 0.8538(2) 0.01445(10) 0.0326(6) Uani 1 1 d . . . . .
H38A H 0.035960 0.896443 -0.007127 0.049 Uiso 1 1 calc R U . . .
H38B H -0.063423 0.878097 0.020347 0.049 Uiso 1 1 calc R U . . .
H38C H -0.003366 0.792372 -0.001079 0.049 Uiso 1 1 calc R U . . .
C39 C 0.05300(18) 0.8452(2) 0.06203(10) 0.0272(5) Uani 1 1 d . . . . .
C40 C 0.00406(17) 0.82941(19) 0.10872(9) 0.0275(5) Uani 1 1 d . . . . .
C41 C -0.09448(19) 0.8236(2) 0.11470(11) 0.0362(7) Uani 1 1 d . . . . .
H41 H -0.136241 0.835716 0.088004 0.043 Uiso 1 1 calc R U . . .
C42 C -0.1308(2) 0.8000(3) 0.16009(11) 0.0416(7) Uani 1 1 d . . . . .
H42 H -0.198022 0.795749 0.164808 0.050 Uiso 1 1 calc R U . . .
C43 C -0.06942(19) 0.7827(2) 0.19850(11) 0.0364(7) Uani 1 1 d . . . . .
H43 H -0.093468 0.764444 0.229586 0.044 Uiso 1 1 calc R U . . .
C44 C 0.02881(18) 0.79247(19) 0.19081(10) 0.0276(5) Uani 1 1 d . . . . .
C45 C 0.10260(18) 0.7804(2) 0.22834(10) 0.0275(5) Uani 1 1 d . . . . .
C46 C 0.0810(2) 0.7535(2) 0.27983(10) 0.0348(6) Uani 1 1 d . . . . .
H46A H 0.136842 0.722564 0.294174 0.052 Uiso 1 1 calc R U . . .
H46B H 0.026194 0.710947 0.280348 0.052 Uiso 1 1 calc R U . . .
H46C H 0.065707 0.809478 0.298862 0.052 Uiso 1 1 calc R U . . .
C47 C 0.34109(18) 0.8147(2) 0.21939(10) 0.0288(5) Uani 1 1 d . . . . .
C48 C 0.43323(18) 0.8136(2) 0.24614(10) 0.0300(6) Uani 1 1 d . . . . .
C49 C 0.4354(2) 0.8083(2) 0.29699(11) 0.0361(6) Uani 1 1 d . . . . .
H49 H 0.377212 0.804027 0.314843 0.043 Uiso 1 1 calc R U . . .
C50 C 0.5219(2) 0.8094(2) 0.32173(12) 0.0421(7) Uani 1 1 d . . . . .
H50 H 0.522720 0.807593 0.356498 0.051 Uiso 1 1 calc R U . . .
C51 C 0.6065(2) 0.8130(2) 0.29629(13) 0.0431(8) Uani 1 1 d . . . . .
H51 H 0.665601 0.812918 0.313466 0.052 Uiso 1 1 calc R U . . .
C52 C 0.6059(2) 0.8167(2) 0.24556(13) 0.0423(7) Uani 1 1 d . . . . .
H52 H 0.664520 0.818501 0.228004 0.051 Uiso 1 1 calc R U . . .
C53 C 0.51922(19) 0.8178(2) 0.22034(11) 0.0350(6) Uani 1 1 d . . . . .
H53 H 0.518725 0.821498 0.185607 0.042 Uiso 1 1 calc R U . . .
C54 C 0.17832(18) 1.0543(2) 0.16331(10) 0.0285(5) Uani 1 1 d . . . . .
C55 C 0.25662(18) 0.6386(2) 0.09358(11) 0.0335(6) Uani 1 1 d . . . . .
N11 N 0.20413(16) 0.85749(17) 0.02837(8) 0.0282(5) Uani 1 1 d . . . . .
H11N H 0.184(2) 0.839(2) 0.0012(12) 0.034 Uiso 1 1 d . U . . .
N12 N 0.14449(15) 0.84825(16) 0.06787(8) 0.0269(4) Uani 1 1 d . . . . .
N13 N 0.06426(14) 0.81554(15) 0.14661(8) 0.0261(4) Uani 1 1 d . . . . .
N14 N 0.18776(15) 0.79713(16) 0.21161(8) 0.0269(5) Uani 1 1 d . . . . .
N15 N 0.26375(15) 0.78958(18) 0.24348(8) 0.0305(5) Uani 1 1 d . . . . .
N16 N 0.18882(16) 0.97572(17) 0.15536(8) 0.0299(5) Uani 1 1 d . . . . .
N17 N 0.23901(15) 0.70403(18) 0.11719(9) 0.0313(5) Uani 1 1 d . . . . .
O11 O 0.31522(12) 0.88276(15) 0.08560(7) 0.0309(4) Uani 1 1 d . . . . .
O12 O 0.34035(13) 0.84047(15) 0.17445(6) 0.0318(4) Uani 1 1 d . . . . .
C2SA C 0.504(3) 0.0878(18) 0.3788(14) 0.126(7) Uani 0.5 1 d . U P B 1
H2S1 H 0.441883 0.056944 0.373540 0.189 Uiso 0.5 1 calc R U P B 1
H2S2 H 0.492973 0.149392 0.393265 0.189 Uiso 0.5 1 calc R U P B 1
H2S3 H 0.542815 0.050103 0.400993 0.189 Uiso 0.5 1 calc R U P B 1
C1SA C 0.5553(18) 0.099(2) 0.3298(10) 0.049(5) Uani 0.5 1 d . U P B 1
N1SA N 0.5927(5) 0.0915(8) 0.2975(4) 0.062(3) Uani 0.5 1 d . U P B 1
C2SB C 0.516(3) 0.1314(18) 0.3776(14) 0.126(7) Uani 0.5 1 d . U P C 2
H2S4 H 0.446142 0.130702 0.381788 0.189 Uiso 0.5 1 calc R U P C 2
H2S5 H 0.538277 0.195984 0.375967 0.189 Uiso 0.5 1 calc R U P C 2
H2S6 H 0.546048 0.099909 0.405422 0.189 Uiso 0.5 1 calc R U P C 2
C1SB C 0.540(2) 0.086(2) 0.3349(11) 0.047(4) Uani 0.5 1 d . U P C 2
N1SB N 0.5476(8) 0.0587(7) 0.2929(3) 0.067(3) Uani 0.5 1 d D U P C 2
C3SA C 0.2742(12) 0.0568(10) 0.2974(6) 0.090(4) Uani 0.7 1 d . U P D 1
H3S1 H 0.209338 0.081723 0.293887 0.134 Uiso 0.7 1 calc R U P D 1
H3S2 H 0.279453 -0.001983 0.279367 0.134 Uiso 0.7 1 calc R U P D 1
H3S3 H 0.320463 0.101673 0.284360 0.134 Uiso 0.7 1 calc R U P D 1
O1S O 0.2944(5) 0.0402(5) 0.3493(2) 0.117(2) Uani 0.7 1 d . U P D 1
H1S H 0.2668(10) -0.0130(18) 0.3587(4) 0.176 Uiso 0.7 1 calc DR U P D 1
C3SB C 0.276(3) 0.0870(19) 0.2971(12) 0.069(7) Uani 0.3 1 d . U P E 2
H3S4 H 0.254290 0.094418 0.263123 0.104 Uiso 0.3 1 calc R U P E 2
H3S5 H 0.310355 0.143004 0.307376 0.104 Uiso 0.3 1 calc R U P E 2
H3S6 H 0.220135 0.077585 0.318346 0.104 Uiso 0.3 1 calc R U P E 2
O2S O 0.3386(8) 0.0069(7) 0.3005(5) 0.084(4) Uani 0.3 1 d . U P E 2
H2S H 0.395(2) 0.0223(9) 0.2916(6) 0.127 Uiso 0.3 1 calc DR U P E 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.9926(19) . ?
V1 N6 2.051(3) . ?
V1 N7 2.057(3) . ?
V1 O2 2.067(2) . ?
V1 N2 2.123(2) . ?
V1 N3 2.132(2) . ?
V1 N4 2.166(2) . ?
C24A N6 1.127(13) . ?
C24A S1A 1.649(13) . ?
C24B N6 1.21(3) . ?
C24B S1B 1.60(3) . ?
S2 C25 1.628(3) . ?
C1 C6 1.390(4) . ?
C1 C2 1.395(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.379(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.392(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.480(3) . ?
C7 O1 1.282(3) . ?
C7 N1 1.316(3) . ?
C8 C9 1.487(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.297(3) . ?
C9 C10 1.455(4) . ?
C10 N3 1.346(4) . ?
C10 C11 1.401(4) . ?
C11 C12 1.374(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.374(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(4) . ?
C13 H13 0.9500 . ?
C14 N3 1.343(4) . ?
C14 C15 1.479(4) . ?
C15 N4 1.295(4) . ?
C15 C16 1.485(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 O2 1.239(3) . ?
C17 N5 1.350(4) . ?
C17 C18 1.473(4) . ?
C18 C19 1.384(4) . ?
C18 C23 1.397(5) . ?
C19 C20 1.396(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.372(7) . ?
C20 H20 0.9500 . ?
C21 C22 1.385(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.383(5) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C25 N7 1.167(4) . ?
N1 N2 1.379(3) . ?
N4 N5 1.379(3) . ?
N5 H5N 0.82(4) . ?
V2 O12 2.0077(18) . ?
V2 N17 2.038(3) . ?
V2 N16 2.062(3) . ?
V2 O11 2.1137(18) . ?
V2 N14 2.114(2) . ?
V2 N13 2.142(2) . ?
V2 N12 2.173(2) . ?
S11 C54 1.633(3) . ?
S12 C55 1.624(3) . ?
C31 C32 1.381(4) . ?
C31 C36 1.402(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.383(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.389(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.383(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.395(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.475(4) . ?
C37 O11 1.247(3) . ?
C37 N11 1.353(3) . ?
C38 C39 1.493(4) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 N12 1.289(3) . ?
C39 C40 1.465(4) . ?
C40 N13 1.348(3) . ?
C40 C41 1.389(4) . ?
C41 C42 1.382(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.378(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.396(4) . ?
C43 H43 0.9500 . ?
C44 N13 1.346(3) . ?
C44 C45 1.464(4) . ?
C45 N14 1.297(3) . ?
C45 C46 1.489(4) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 O12 1.282(3) . ?
C47 N15 1.316(3) . ?
C47 C48 1.480(4) . ?
C48 C49 1.391(4) . ?
C48 C53 1.395(4) . ?
C49 C50 1.385(4) . ?
C49 H49 0.9500 . ?
C50 C51 1.372(5) . ?
C50 H50 0.9500 . ?
C51 C52 1.387(5) . ?
C51 H51 0.9500 . ?
C52 C53 1.393(4) . ?
C52 H52 0.9500 . ?
C53 H53 0.9500 . ?
C54 N16 1.158(4) . ?
C55 N17 1.165(4) . ?
N11 N12 1.370(3) . ?
N11 H11N 0.83(3) . ?
N14 N15 1.377(3) . ?
C2SA C1SA 1.53(5) . ?
C2SA H2S1 0.9800 . ?
C2SA H2S2 0.9800 . ?
C2SA H2S3 0.9800 . ?
C1SA N1SA 1.03(3) . ?
C2SB C1SB 1.38(5) . ?
C2SB H2S4 0.9800 . ?
C2SB H2S5 0.9800 . ?
C2SB H2S6 0.9800 . ?
C1SB N1SB 1.22(3) . ?
C3SA O1S 1.464(16) . ?
C3SA H3S1 0.9800 . ?
C3SA H3S2 0.9800 . ?
C3SA H3S3 0.9800 . ?
O1S H1S 0.89(3) . ?
C3SB O2S 1.45(3) . ?
C3SB H3S4 0.9800 . ?
C3SB H3S5 0.9800 . ?
C3SB H3S6 0.9800 . ?
O2S H2S 0.85(3) . ?

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 N6 89.75(9) . . ?
O1 V1 N7 90.37(9) . . ?
N6 V1 N7 177.29(10) . . ?
O1 V1 O2 74.17(8) . . ?
N6 V1 O2 89.01(9) . . ?
N7 V1 O2 88.42(9) . . ?
O1 V1 N2 72.47(8) . . ?
N6 V1 N2 86.11(9) . . ?
N7 V1 N2 96.51(9) . . ?
O2 V1 N2 146.29(9) . . ?
O1 V1 N3 143.47(8) . . ?
N6 V1 N3 93.19(9) . . ?
N7 V1 N3 88.32(9) . . ?
O2 V1 N3 142.22(9) . . ?
N2 V1 N3 71.43(9) . . ?
O1 V1 N4 145.53(8) . . ?
N6 V1 N4 91.39(9) . . ?
N7 V1 N4 86.98(10) . . ?
O2 V1 N4 71.40(8) . . ?
N2 V1 N4 141.97(9) . . ?
N3 V1 N4 70.84(9) . . ?
N6 C24A S1A 175.4(11) . . ?
N6 C24B S1B 173(3) . . ?
C6 C1 C2 119.9(3) . . ?
C6 C1 H1 120.1 . . ?
C2 C1 H1 120.1 . . ?
C3 C2 C1 120.0(3) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 120.3(3) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 119.8(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C6 C5 C4 120.1(3) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C1 120.0(2) . . ?
C5 C6 C7 121.1(2) . . ?
C1 C6 C7 118.9(2) . . ?
O1 C7 N1 123.4(2) . . ?
O1 C7 C6 117.4(2) . . ?
N1 C7 C6 119.2(2) . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 111.8(2) . . ?
N2 C9 C8 125.3(3) . . ?
C10 C9 C8 122.9(2) . . ?
N3 C10 C11 121.0(3) . . ?
N3 C10 C9 114.0(2) . . ?
C11 C10 C9 125.0(3) . . ?
C12 C11 C10 118.8(3) . . ?
C12 C11 H11 120.6 . . ?
C10 C11 H11 120.6 . . ?
C13 C12 C11 120.2(3) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 118.7(3) . . ?
C12 C13 H13 120.7 . . ?
C14 C13 H13 120.7 . . ?
N3 C14 C13 121.6(3) . . ?
N3 C14 C15 113.8(2) . . ?
C13 C14 C15 124.6(3) . . ?
N4 C15 C14 111.3(2) . . ?
N4 C15 C16 127.6(3) . . ?
C14 C15 C16 121.2(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O2 C17 N5 118.1(3) . . ?
O2 C17 C18 119.8(3) . . ?
N5 C17 C18 122.1(3) . . ?
C19 C18 C23 119.4(3) . . ?
C19 C18 C17 123.6(3) . . ?
C23 C18 C17 117.0(3) . . ?
C18 C19 C20 119.6(4) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C21 C20 C19 120.6(4) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C20 C21 C22 120.1(3) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C23 C22 C21 119.7(4) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C22 C23 C18 120.5(3) . . ?
C22 C23 H23 119.7 . . ?
C18 C23 H23 119.7 . . ?
N7 C25 S2 178.2(3) . . ?
C7 N1 N2 106.9(2) . . ?
C9 N2 N1 118.8(2) . . ?
C9 N2 V1 123.20(19) . . ?
N1 N2 V1 117.96(16) . . ?
C14 N3 C10 119.7(2) . . ?
C14 N3 V1 120.76(19) . . ?
C10 N3 V1 119.51(18) . . ?
C15 N4 N5 121.3(3) . . ?
C15 N4 V1 122.8(2) . . ?
N5 N4 V1 115.57(18) . . ?
C17 N5 N4 112.6(2) . . ?
C17 N5 H5N 128(3) . . ?
N4 N5 H5N 118(3) . . ?
C24A N6 V1 154.0(6) . . ?
C24B N6 V1 166.8(14) . . ?
C25 N7 V1 170.6(2) . . ?
C7 O1 V1 118.23(17) . . ?
C17 O2 V1 122.1(2) . . ?
O12 V2 N17 90.73(9) . . ?
O12 V2 N16 91.68(9) . . ?
N17 V2 N16 176.15(9) . . ?
O12 V2 O11 75.56(7) . . ?
N17 V2 O11 88.94(9) . . ?
N16 V2 O11 88.76(9) . . ?
O12 V2 N14 72.62(8) . . ?
N17 V2 N14 92.18(9) . . ?
N16 V2 N14 91.41(9) . . ?
O11 V2 N14 148.17(8) . . ?
O12 V2 N13 144.16(8) . . ?
N17 V2 N13 92.82(9) . . ?
N16 V2 N13 86.98(9) . . ?
O11 V2 N13 140.13(8) . . ?
N14 V2 N13 71.61(8) . . ?
O12 V2 N12 145.92(8) . . ?
N17 V2 N12 83.33(9) . . ?
N16 V2 N12 93.00(9) . . ?
O11 V2 N12 70.82(8) . . ?
N14 V2 N12 140.88(8) . . ?
N13 V2 N12 69.84(8) . . ?
C32 C31 C36 119.5(2) . . ?
C32 C31 H31 120.3 . . ?
C36 C31 H31 120.3 . . ?
C31 C32 C33 120.8(3) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C32 C33 C34 119.8(3) . . ?
C32 C33 H33 120.1 . . ?
C34 C33 H33 120.1 . . ?
C35 C34 C33 120.3(2) . . ?
C35 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
C34 C35 C36 119.8(2) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C35 C36 C31 119.8(2) . . ?
C35 C36 C37 122.6(2) . . ?
C31 C36 C37 117.6(2) . . ?
O11 C37 N11 118.3(2) . . ?
O11 C37 C36 122.0(2) . . ?
N11 C37 C36 119.8(2) . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C39 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N12 C39 C40 111.1(2) . . ?
N12 C39 C38 125.9(2) . . ?
C40 C39 C38 122.9(2) . . ?
N13 C40 C41 121.3(3) . . ?
N13 C40 C39 113.6(2) . . ?
C41 C40 C39 125.1(2) . . ?
C42 C41 C40 119.0(3) . . ?
C42 C41 H41 120.5 . . ?
C40 C41 H41 120.5 . . ?
C43 C42 C41 119.9(3) . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C42 C43 C44 118.7(3) . . ?
C42 C43 H43 120.7 . . ?
C44 C43 H43 120.7 . . ?
N13 C44 C43 121.4(3) . . ?
N13 C44 C45 113.4(2) . . ?
C43 C44 C45 125.1(3) . . ?
N14 C45 C44 112.2(2) . . ?
N14 C45 C46 124.5(2) . . ?
C44 C45 C46 123.3(2) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O12 C47 N15 123.5(2) . . ?
O12 C47 C48 118.8(2) . . ?
N15 C47 C48 117.7(2) . . ?
C49 C48 C53 119.2(3) . . ?
C49 C48 C47 120.8(2) . . ?
C53 C48 C47 120.0(2) . . ?
C50 C49 C48 120.4(3) . . ?
C50 C49 H49 119.8 . . ?
C48 C49 H49 119.8 . . ?
C51 C50 C49 120.3(3) . . ?
C51 C50 H50 119.8 . . ?
C49 C50 H50 119.8 . . ?
C50 C51 C52 120.1(3) . . ?
C50 C51 H51 119.9 . . ?
C52 C51 H51 119.9 . . ?
C51 C52 C53 120.0(3) . . ?
C51 C52 H52 120.0 . . ?
C53 C52 H52 120.0 . . ?
C52 C53 C48 119.9(3) . . ?
C52 C53 H53 120.1 . . ?
C48 C53 H53 120.1 . . ?
N16 C54 S11 178.3(3) . . ?
N17 C55 S12 179.2(3) . . ?
C37 N11 N12 113.0(2) . . ?
C37 N11 H11N 128(2) . . ?
N12 N11 H11N 118(2) . . ?
C39 N12 N11 120.6(2) . . ?
C39 N12 V2 123.86(19) . . ?
N11 N12 V2 115.51(15) . . ?
C44 N13 C40 119.7(2) . . ?
C44 N13 V2 119.38(17) . . ?
C40 N13 V2 120.84(17) . . ?
C45 N14 N15 118.0(2) . . ?
C45 N14 V2 123.30(18) . . ?
N15 N14 V2 118.65(16) . . ?
C47 N15 N14 107.2(2) . . ?
C54 N16 V2 176.4(2) . . ?
C55 N17 V2 162.5(2) . . ?
C37 O11 V2 119.89(17) . . ?
C47 O12 V2 117.99(16) . . ?
C1SA C2SA H2S1 109.5 . . ?
C1SA C2SA H2S2 109.5 . . ?
H2S1 C2SA H2S2 109.5 . . ?
C1SA C2SA H2S3 109.5 . . ?
H2S1 C2SA H2S3 109.5 . . ?
H2S2 C2SA H2S3 109.5 . . ?
N1SA C1SA C2SA 168(3) . . ?
C1SB C2SB H2S4 109.5 . . ?
C1SB C2SB H2S5 109.5 . . ?
H2S4 C2SB H2S5 109.5 . . ?
C1SB C2SB H2S6 109.5 . . ?
H2S4 C2SB H2S6 109.5 . . ?
H2S5 C2SB H2S6 109.5 . . ?
N1SB C1SB C2SB 166(3) . . ?
O1S C3SA H3S1 109.5 . . ?
O1S C3SA H3S2 109.5 . . ?
H3S1 C3SA H3S2 109.5 . . ?
O1S C3SA H3S3 109.5 . . ?
H3S1 C3SA H3S3 109.5 . . ?
H3S2 C3SA H3S3 109.5 . . ?
C3SA O1S H1S 109.5 . . ?
O2S C3SB H3S4 109.5 . . ?
O2S C3SB H3S5 109.5 . . ?
H3S4 C3SB H3S5 109.5 . . ?
O2S C3SB H3S6 109.5 . . ?
H3S4 C3SB H3S6 109.5 . . ?
H3S5 C3SB H3S6 109.5 . . ?
C3SB O2S H2S 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5N N1SA 0.82(4) 2.03(4) 2.829(10) 164(4) .
N5 H5N N1SB 0.82(4) 2.13(4) 2.944(9) 173(4) .
N11 H11N S2 0.83(3) 2.75(3) 3.563(2) 167(3) 4_455
O1S H1S S1A 0.89 2.36 3.212(6) 160.1 3_645
O2S H2S N1SB 0.85 2.20 3.020(15) 162.3 .
C3 H3 S1A 0.95 2.89 3.683(3) 142.1 4
C3 H3 S1B 0.95 2.95 3.652(5) 132.0 4
C11 H11 S1A 0.95 2.90 3.690(3) 141.3 4_455
C16 H16C N1SB 0.98 2.28 2.945(10) 123.9 .
C19 H19 N1SA 0.95 2.30 3.096(8) 141.1 .
C19 H19 N1SB 0.95 2.61 3.497(11) 156.2 .
C21 H21 S1A 0.95 2.87 3.788(4) 163.1 3_745
C32 H32 S12 0.95 2.98 3.687(3) 132.7 4_565
C35 H35 S2 0.95 2.87 3.623(3) 137.6 4_455
C2SA H2S2 S2 0.98 2.55 3.34(3) 137.8 3_655
C2SA H2S3 S12 0.98 2.68 3.49(4) 139.9 3_645
C2SB H2S4 S2 0.98 2.38 3.06(3) 126.0 3_655
C2SB H2S6 S12 0.98 2.70 3.52(4) 141.2 3_645

_refine_diff_density_max         0.370
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.050

