# Supplementary Information (SI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2024

####################################################################### 
# 
# 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_voc2o4
_database_code_depnum_ccdc_archive 'CCDC 2364915'
loop_
_audit_author_name
_audit_author_address
"Sofiya Vorob'eva"
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2024-08-09 deposited with the CCDC.	2024-08-16 downloaded from the CCDC.
;
_audit_creation_date             2024-06-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 O9 V, 2(C16 H36 N)'
_chemical_formula_sum            'C36 H72 N2 O9 V'
_chemical_formula_weight         727.89
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.9092(19)
_cell_length_b                   13.9416(12)
_cell_length_c                   18.272(3)
_cell_angle_alpha                90
_cell_angle_beta                 120.899(3)
_cell_angle_gamma                90
_cell_volume                     4133.4(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4100
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.81
_cell_measurement_theta_min      2.51
_shelx_estimated_absorpt_T_max   0.980
_shelx_estimated_absorpt_T_min   0.974
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1588
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25901
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_min         2.511
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
'Data collection was performed by Kochelakov D.V. in XRD Facility of NIIC SB RAS'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3772
_reflns_number_total             5125
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         5125
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0449
_refine_ls_restrained_S_all      1.040
_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)+(0.0400P)²+2.5035P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1156
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B)
1.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.500000 0.24420(3) 0.250000 0.02617(12) Uani 1 2 d S T P . .
O1 O 0.500000 0.13044(14) 0.250000 0.0503(6) Uani 1 2 d S T P . .
O11 O 0.38505(7) 0.29065(9) 0.19762(8) 0.0314(3) Uani 1 1 d . . . . .
O12 O 0.50328(8) 0.29140(9) 0.35317(7) 0.0314(3) Uani 1 1 d . . . . .
O13 O 0.29840(8) 0.36529(10) 0.22811(8) 0.0376(3) Uani 1 1 d . . . . .
O14 O 0.42596(8) 0.35553(10) 0.40043(8) 0.0365(3) Uani 1 1 d . . . . .
C1 C 0.36479(11) 0.32945(12) 0.24890(11) 0.0262(4) Uani 1 1 d . . . . .
C2 C 0.43562(11) 0.32601(12) 0.34344(11) 0.0261(4) Uani 1 1 d . . . . .
N1 N 0.30603(8) 0.58200(10) 0.40931(9) 0.0229(3) Uani 1 1 d . . . . .
C3 C 0.32181(11) 0.57889(12) 0.33567(11) 0.0261(4) Uani 1 1 d . . . . .
H3A H 0.374267 0.612625 0.353421 0.031 Uiso 1 1 calc R U . . .
H3B H 0.329114 0.511083 0.324821 0.031 Uiso 1 1 calc R U . . .
C4 C 0.25496(12) 0.62285(14) 0.25262(11) 0.0321(4) Uani 1 1 d . . . . .
H4A H 0.246448 0.690631 0.262365 0.039 Uiso 1 1 calc R U . . .
H4B H 0.202506 0.588026 0.232493 0.039 Uiso 1 1 calc R U . . .
C5 C 0.27880(14) 0.61779(16) 0.18499(13) 0.0431(5) Uani 1 1 d . . . . .
H5A H 0.289810 0.550198 0.177410 0.052 Uiso 1 1 calc R U . . .
H5B H 0.330136 0.654758 0.204442 0.052 Uiso 1 1 calc R U . . .
C6 C 0.21132(15) 0.65758(16) 0.09980(13) 0.0469(5) Uani 1 1 d . . . . .
H6A H 0.230242 0.656892 0.058923 0.070 Uiso 1 1 calc R U . . .
H6B H 0.198539 0.723572 0.107571 0.070 Uiso 1 1 calc R U . . .
H6C H 0.161750 0.617870 0.078068 0.070 Uiso 1 1 calc R U . . .
C7 C 0.37826(10) 0.53048(12) 0.48374(10) 0.0256(4) Uani 1 1 d . . . . .
H7A H 0.384367 0.466661 0.463856 0.031 Uiso 1 1 calc R U . . .
H7B H 0.429186 0.567202 0.500501 0.031 Uiso 1 1 calc R U . . .
C8 C 0.37125(12) 0.51668(14) 0.56235(11) 0.0313(4) Uani 1 1 d . . . . .
H8A H 0.318842 0.483632 0.546091 0.038 Uiso 1 1 calc R U . . .
H8B H 0.370707 0.580017 0.586548 0.038 Uiso 1 1 calc R U . . .
C9 C 0.44373(12) 0.45726(15) 0.62954(12) 0.0389(5) Uani 1 1 d . . . . .
H9A H 0.495675 0.487431 0.640485 0.047 Uiso 1 1 calc R U . . .
H9B H 0.443197 0.459424 0.683410 0.047 Uiso 1 1 calc R U . . .
C10 C 0.44356(15) 0.35304(16) 0.60536(15) 0.0491(6) Uani 1 1 d . . . . .
H10A H 0.451315 0.349638 0.556356 0.074 Uiso 1 1 calc R U . . .
H10B H 0.390783 0.323479 0.590392 0.074 Uiso 1 1 calc R U . . .
H10C H 0.488487 0.318739 0.653733 0.074 Uiso 1 1 calc R U . . .
C11 C 0.22555(10) 0.53209(12) 0.38479(11) 0.0268(4) Uani 1 1 d . . . . .
H11A H 0.180766 0.562907 0.332684 0.032 Uiso 1 1 calc R U . . .
H11B H 0.213547 0.542115 0.430980 0.032 Uiso 1 1 calc R U . . .
C12 C 0.22426(12) 0.42443(13) 0.36840(13) 0.0352(4) Uani 1 1 d . . . . .
H12A H 0.257059 0.390341 0.423393 0.042 Uiso 1 1 calc R U . . .
H12B H 0.249672 0.411977 0.333577 0.042 Uiso 1 1 calc R U . . .
C13 C 0.13587(14) 0.38634(17) 0.32184(15) 0.0484(6) Uani 1 1 d . . . . .
H13A H 0.137143 0.315825 0.328782 0.058 Uiso 1 1 calc R U . . .
H13B H 0.106140 0.413939 0.348410 0.058 Uiso 1 1 calc R U . . .
C14 C 0.08938(15) 0.4102(2) 0.22797(16) 0.0620(7) Uani 1 1 d . . . . .
H14A H 0.038232 0.372839 0.199071 0.093 Uiso 1 1 calc R U . . .
H14B H 0.123482 0.394358 0.203501 0.093 Uiso 1 1 calc R U . . .
H14C H 0.076218 0.478763 0.220358 0.093 Uiso 1 1 calc R U . . .
C15 C 0.29913(11) 0.68461(12) 0.43325(11) 0.0256(4) Uani 1 1 d . . . . .
H15A H 0.245794 0.711187 0.388138 0.031 Uiso 1 1 calc R U . . .
H15B H 0.297866 0.683148 0.486735 0.031 Uiso 1 1 calc R U . . .
C16 C 0.36725(11) 0.75265(12) 0.44567(11) 0.0265(4) Uani 1 1 d . . . . .
H16A H 0.360922 0.768310 0.389766 0.032 Uiso 1 1 calc R U . . .
H16B H 0.421615 0.721746 0.481562 0.032 Uiso 1 1 calc R U . . .
C17 C 0.36238(12) 0.84436(13) 0.48875(12) 0.0326(4) Uani 1 1 d . . . . .
H17A H 0.308750 0.876069 0.451178 0.039 Uiso 1 1 calc R U . . .
H17B H 0.364968 0.827390 0.542691 0.039 Uiso 1 1 calc R U . . .
C18 C 0.43148(15) 0.91408(15) 0.50784(15) 0.0503(6) Uani 1 1 d . . . . .
H18A H 0.428387 0.932358 0.454479 0.075 Uiso 1 1 calc R U . . .
H18B H 0.484720 0.883440 0.545860 0.075 Uiso 1 1 calc R U . . .
H18C H 0.425918 0.971443 0.535487 0.075 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 1.5860(19) . ?
V1 O11 1.9808(13) 2_655 ?
V1 O11 1.9808(13) . ?
V1 O12 1.9674(12) 2_655 ?
V1 O12 1.9674(12) . ?
O11 C1 1.299(2) . ?
O12 C2 1.291(2) . ?
O13 C1 1.217(2) . ?
O14 C2 1.218(2) . ?
C1 C2 1.551(2) . ?
N1 C3 1.521(2) . ?
N1 C7 1.524(2) . ?
N1 C11 1.517(2) . ?
N1 C15 1.521(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.519(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.519(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.523(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.521(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.531(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.518(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.528(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.529(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.509(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.520(2) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.529(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.518(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 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 O11 109.09(4) . . ?
O1 V1 O11 109.09(4) . 2_655 ?
O1 V1 O12 109.54(4) . . ?
O1 V1 O12 109.54(4) . 2_655 ?
O11 V1 O11 141.83(8) . 2_655 ?
O12 V1 O11 86.60(5) 2_655 . ?
O12 V1 O11 86.60(5) . 2_655 ?
O12 V1 O11 80.82(5) . . ?
O12 V1 O11 80.82(5) 2_655 2_655 ?
O12 V1 O12 140.92(8) . 2_655 ?
C1 O11 V1 116.40(11) . . ?
C2 O12 V1 116.84(10) . . ?
O11 C1 C2 112.64(15) . . ?
O13 C1 O11 125.82(16) . . ?
O13 C1 C2 121.54(15) . . ?
O12 C2 C1 113.14(14) . . ?
O14 C2 O12 125.57(16) . . ?
O14 C2 C1 121.27(16) . . ?
C3 N1 C7 106.44(12) . . ?
C3 N1 C15 111.47(12) . . ?
C11 N1 C3 110.39(13) . . ?
C11 N1 C7 110.54(13) . . ?
C11 N1 C15 107.16(12) . . ?
C15 N1 C7 110.88(12) . . ?
N1 C3 H3A 108.4 . . ?
N1 C3 H3B 108.4 . . ?
H3A C3 H3B 107.4 . . ?
C4 C3 N1 115.58(14) . . ?
C4 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 C5 110.60(15) . . ?
H4A C4 H4B 108.1 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C4 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
C4 C5 C6 111.83(17) . . ?
H5A C5 H5B 107.9 . . ?
C6 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 H7A 108.4 . . ?
N1 C7 H7B 108.4 . . ?
H7A C7 H7B 107.5 . . ?
C8 C7 N1 115.44(14) . . ?
C8 C7 H7A 108.4 . . ?
C8 C7 H7B 108.4 . . ?
C7 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
C7 C8 C9 110.46(15) . . ?
H8A C8 H8B 108.1 . . ?
C9 C8 H8A 109.6 . . ?
C9 C8 H8B 109.6 . . ?
C8 C9 H9A 108.6 . . ?
C8 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
C10 C9 C8 114.66(17) . . ?
C10 C9 H9A 108.6 . . ?
C10 C9 H9B 108.6 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 H11A 108.5 . . ?
N1 C11 H11B 108.5 . . ?
N1 C11 C12 114.90(14) . . ?
H11A C11 H11B 107.5 . . ?
C12 C11 H11A 108.5 . . ?
C12 C11 H11B 108.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 C13 110.67(16) . . ?
H12A C12 H12B 108.1 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
C12 C13 H13A 109.0 . . ?
C12 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
C14 C13 C12 112.85(19) . . ?
C14 C13 H13A 109.0 . . ?
C14 C13 H13B 109.0 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 H15A 108.3 . . ?
N1 C15 H15B 108.3 . . ?
H15A C15 H15B 107.4 . . ?
C16 C15 N1 116.01(13) . . ?
C16 C15 H15A 108.3 . . ?
C16 C15 H15B 108.3 . . ?
C15 C16 H16A 109.8 . . ?
C15 C16 H16B 109.8 . . ?
C15 C16 C17 109.17(14) . . ?
H16A C16 H16B 108.3 . . ?
C17 C16 H16A 109.8 . . ?
C17 C16 H16B 109.8 . . ?
C16 C17 H17A 109.1 . . ?
C16 C17 H17B 109.1 . . ?
H17A C17 H17B 107.9 . . ?
C18 C17 C16 112.42(17) . . ?
C18 C17 H17A 109.1 . . ?
C18 C17 H17B 109.1 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

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 O11 C1 O13 176.93(14) . . . . ?
V1 O11 C1 C2 -3.15(17) . . . . ?
V1 O12 C2 O14 177.65(14) . . . . ?
V1 O12 C2 C1 -3.74(18) . . . . ?
O11 C1 C2 O12 4.5(2) . . . . ?
O11 C1 C2 O14 -176.82(16) . . . . ?
O13 C1 C2 O12 -175.57(16) . . . . ?
O13 C1 C2 O14 3.1(3) . . . . ?
N1 C3 C4 C5 178.49(15) . . . . ?
N1 C7 C8 C9 175.41(15) . . . . ?
N1 C11 C12 C13 -164.83(15) . . . . ?
N1 C15 C16 C17 -167.09(14) . . . . ?
C3 N1 C7 C8 -174.43(14) . . . . ?
C3 N1 C11 C12 65.15(18) . . . . ?
C3 N1 C15 C16 -49.17(18) . . . . ?
C3 C4 C5 C6 177.61(18) . . . . ?
C7 N1 C3 C4 177.48(15) . . . . ?
C7 N1 C11 C12 -52.35(18) . . . . ?
C7 N1 C15 C16 69.22(18) . . . . ?
C7 C8 C9 C10 -68.6(2) . . . . ?
C11 N1 C3 C4 57.48(19) . . . . ?
C11 N1 C7 C8 -54.53(18) . . . . ?
C11 N1 C15 C16 -170.06(14) . . . . ?
C11 C12 C13 C14 77.3(2) . . . . ?
C15 N1 C3 C4 -61.50(19) . . . . ?
C15 N1 C7 C8 64.17(18) . . . . ?
C15 N1 C11 C12 -173.29(14) . . . . ?
C15 C16 C17 C18 176.88(16) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_p3-1
_database_code_depnum_ccdc_archive 'CCDC 2364916'
loop_
_audit_author_name
_audit_author_address
"Sofiya Vorob'eva"
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2024-06-24 deposited with the CCDC.	2024-08-16 downloaded from the CCDC.
;
_audit_creation_date             2024-06-05
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 O6 V, C16 H36 N'
_chemical_formula_sum            'C18 H36 N O6 V'
_chemical_formula_weight         413.42
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.8694(5)
_cell_length_b                   14.9160(6)
_cell_length_c                   16.6499(7)
_cell_angle_alpha                90
_cell_angle_beta                 103.309(2)
_cell_angle_gamma                90
_cell_volume                     2143.56(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2806
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.40
_shelx_estimated_absorpt_T_max   0.976
_shelx_estimated_absorpt_T_min   0.957
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1072 before and 0.0664 after correction.
The Ratio of minimum to maximum transmission is 0.9020.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23280
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         2.405
_diffrn_ambient_temperature      150.0
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_details      
'Data collection was performed by Sukhikh T.S. in XRD Facility of NIIC SB RAS'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         .
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3554
_reflns_number_total             4914
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4914
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0473
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0273P)²+1.2275P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1098
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B), C14(H14A,H14B), C9(H9A,H9B), C15(H15A,H15B), C6(H6A,
 H6B), C13(H13A,H13B), C12(H12A,H12B), C4(H4A,H4B), C5(H5A,H5B), C18(H18A,H18B),
  C16(H16A,H16B)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C3(H3A,H3B,H3C), C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.70938(5) 0.44198(2) 0.40800(2) 0.01965(12) Uani 1 1 d . . . . .
O5 O 0.51781(18) 0.51825(10) 0.39914(9) 0.0194(3) Uani 1 1 d . . . . .
O3 O 0.92618(18) 0.39664(10) 0.46007(10) 0.0222(4) Uani 1 1 d . . . . .
O6 O 0.33844(18) 0.56655(10) 0.46459(9) 0.0210(3) Uani 1 1 d . . . . .
O2 O 0.63461(19) 0.34299(11) 0.38583(10) 0.0254(4) Uani 1 1 d . . . . .
O4 O 1.16777(18) 0.43703(10) 0.52303(9) 0.0215(3) Uani 1 1 d . . . . .
O1 O 0.7452(2) 0.47917(11) 0.32189(10) 0.0279(4) Uani 1 1 d . . . . .
N1 N 0.6336(2) 0.74739(12) 0.28281(11) 0.0222(4) Uani 1 1 d . . . . .
C8 C 0.6352(3) 0.79633(16) 0.43186(15) 0.0285(6) Uani 1 1 d . . . . .
H8A H 0.572259 0.849936 0.411327 0.034 Uiso 1 1 calc R U . . .
H8B H 0.745888 0.813584 0.443429 0.034 Uiso 1 1 calc R U . . .
C7 C 0.6037(3) 0.72324(15) 0.36680(14) 0.0235(5) Uani 1 1 d . . . . .
H7A H 0.494003 0.704716 0.358614 0.028 Uiso 1 1 calc R U . . .
H7B H 0.668450 0.670659 0.388502 0.028 Uiso 1 1 calc R U . . .
C14 C 0.5426(3) 0.82996(15) 0.24670(15) 0.0245(5) Uani 1 1 d . . . . .
H14A H 0.581167 0.881951 0.282526 0.029 Uiso 1 1 calc R U . . .
H14B H 0.563463 0.842071 0.191798 0.029 Uiso 1 1 calc R U . . .
C9 C 0.5948(3) 0.76281(18) 0.51067(15) 0.0322(6) Uani 1 1 d . . . . .
H9A H 0.488402 0.738080 0.497095 0.039 Uiso 1 1 calc R U . . .
H9B H 0.666512 0.713656 0.534158 0.039 Uiso 1 1 calc R U . . .
C1 C 0.4575(3) 0.52459(14) 0.46107(13) 0.0177(5) Uani 1 1 d . . . . .
C2 C 1.0285(3) 0.45236(14) 0.49531(13) 0.0195(5) Uani 1 1 d . . . . .
C15 C 0.8032(3) 0.77058(16) 0.29023(15) 0.0249(5) Uani 1 1 d . . . . .
H15A H 0.816436 0.789452 0.235262 0.030 Uiso 1 1 calc R U . . .
H15B H 0.829589 0.822591 0.327773 0.030 Uiso 1 1 calc R U . . .
C6 C 0.5860(3) 0.66598(15) 0.22844(15) 0.0274(6) Uani 1 1 d . . . . .
H6A H 0.479587 0.648851 0.231511 0.033 Uiso 1 1 calc R U . . .
H6B H 0.655311 0.615633 0.251370 0.033 Uiso 1 1 calc R U . . .
C13 C 0.3693(3) 0.82288(16) 0.23731(17) 0.0305(6) Uani 1 1 d . . . . .
H13A H 0.346990 0.812024 0.292097 0.037 Uiso 1 1 calc R U . . .
H13B H 0.329451 0.771067 0.201522 0.037 Uiso 1 1 calc R U . . .
C12 C 0.2856(3) 0.90773(17) 0.19997(17) 0.0346(6) Uani 1 1 d . . . . .
H12A H 0.315237 0.920880 0.147381 0.042 Uiso 1 1 calc R U . . .
H12B H 0.172577 0.896549 0.187084 0.042 Uiso 1 1 calc R U . . .
C4 C 0.5625(4) 0.58678(18) 0.09352(17) 0.0411(7) Uani 1 1 d . . . . .
H4A H 0.475936 0.555513 0.110044 0.049 Uiso 1 1 calc R U . . .
H4B H 0.531418 0.597467 0.033279 0.049 Uiso 1 1 calc R U . . .
C5 C 0.5891(4) 0.67725(17) 0.13796(16) 0.0372(7) Uani 1 1 d . . . . .
H5A H 0.690472 0.702031 0.133706 0.045 Uiso 1 1 calc R U . . .
H5B H 0.507323 0.719970 0.111348 0.045 Uiso 1 1 calc R U . . .
C10 C 0.6048(4) 0.8359(2) 0.57486(17) 0.0445(7) Uani 1 1 d . . . . .
H10A H 0.534634 0.885031 0.551829 0.067 Uiso 1 1 calc R U . . .
H10B H 0.711225 0.858557 0.590681 0.067 Uiso 1 1 calc R U . . .
H10C H 0.574837 0.811505 0.623582 0.067 Uiso 1 1 calc R U . . .
C18 C 1.0832(3) 0.7303(2) 0.33373(18) 0.0395(7) Uani 1 1 d . . . . .
H18A H 1.154828 0.678419 0.342367 0.047 Uiso 1 1 calc R U . . .
H18B H 1.093713 0.761042 0.282604 0.047 Uiso 1 1 calc R U . . .
C16 C 0.9179(3) 0.69584(19) 0.3217(2) 0.0414(7) Uani 1 1 d . . . . .
H16A H 0.900939 0.645739 0.281625 0.050 Uiso 1 1 calc R U . . .
H16B H 0.901307 0.672964 0.374820 0.050 Uiso 1 1 calc R U . . .
C17 C 1.1317(4) 0.7941(2) 0.40542(19) 0.0536(9) Uani 1 1 d . . . . .
H17A H 1.066797 0.847969 0.395419 0.080 Uiso 1 1 calc R U . . .
H17B H 1.240484 0.810933 0.411171 0.080 Uiso 1 1 calc R U . . .
H17C H 1.119297 0.764860 0.456211 0.080 Uiso 1 1 calc R U . . .
C3 C 0.7016(4) 0.5275(2) 0.1115(2) 0.0551(9) Uani 1 1 d . . . . .
H3A H 0.678883 0.472105 0.079389 0.083 Uiso 1 1 calc R U . . .
H3B H 0.728795 0.513025 0.170510 0.083 Uiso 1 1 calc R U . . .
H3C H 0.788663 0.558470 0.096503 0.083 Uiso 1 1 calc R U . . .
C11 C 0.3204(4) 0.9890(2) 0.2553(2) 0.0630(11) Uani 1 1 d . . . . .
H11A H 0.254342 1.039034 0.230311 0.094 Uiso 1 1 calc R U . . .
H11B H 0.429485 1.005795 0.262198 0.094 Uiso 1 1 calc R U . . .
H11C H 0.299968 0.975027 0.309330 0.094 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 O5 2.0217(16) . ?
V1 O3 2.0344(16) . ?
V1 O6 2.2606(16) 3_666 ?
V1 O2 1.6259(16) . ?
V1 O4 2.2775(16) 3_766 ?
V1 O1 1.6353(16) . ?
O5 C1 1.270(3) . ?
O3 C2 1.270(3) . ?
O6 C1 1.241(3) . ?
O4 C2 1.236(3) . ?
N1 C7 1.525(3) . ?
N1 C14 1.519(3) . ?
N1 C15 1.520(3) . ?
N1 C6 1.516(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C7 1.517(3) . ?
C8 C9 1.522(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.513(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.515(4) . ?
C1 C1 1.529(4) 3_666 ?
C2 C2 1.529(4) 3_766 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.519(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C5 1.522(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C12 1.525(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.511(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.531(4) . ?
C4 C3 1.491(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C16 1.523(4) . ?
C18 C17 1.510(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 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
O5 V1 O3 156.09(6) . . ?
O5 V1 O6 76.36(6) . 3_666 ?
O5 V1 O4 83.54(6) . 3_766 ?
O3 V1 O6 86.82(6) . 3_666 ?
O3 V1 O4 75.70(6) . 3_766 ?
O6 V1 O4 75.10(6) 3_666 3_766 ?
O2 V1 O5 101.68(7) . . ?
O2 V1 O3 95.22(7) . . ?
O2 V1 O6 90.41(7) . 3_666 ?
O2 V1 O4 163.12(7) . 3_766 ?
O2 V1 O1 105.10(8) . . ?
O1 V1 O5 94.28(7) . . ?
O1 V1 O3 97.53(8) . . ?
O1 V1 O6 163.36(7) . 3_666 ?
O1 V1 O4 90.36(7) . 3_766 ?
C1 O5 V1 119.11(14) . . ?
C2 O3 V1 118.96(14) . . ?
C1 O6 V1 111.20(13) . 3_666 ?
C2 O4 V1 111.26(13) . 3_766 ?
C14 N1 C7 111.44(18) . . ?
C14 N1 C15 105.86(17) . . ?
C15 N1 C7 110.92(17) . . ?
C6 N1 C7 105.95(17) . . ?
C6 N1 C14 111.31(18) . . ?
C6 N1 C15 111.45(19) . . ?
H8A C8 H8B 108.2 . . ?
C7 C8 H8A 109.7 . . ?
C7 C8 H8B 109.7 . . ?
C7 C8 C9 109.8(2) . . ?
C9 C8 H8A 109.7 . . ?
C9 C8 H8B 109.7 . . ?
N1 C7 H7A 108.2 . . ?
N1 C7 H7B 108.2 . . ?
C8 C7 N1 116.27(18) . . ?
C8 C7 H7A 108.2 . . ?
C8 C7 H7B 108.2 . . ?
H7A C7 H7B 107.4 . . ?
N1 C14 H14A 108.6 . . ?
N1 C14 H14B 108.6 . . ?
H14A C14 H14B 107.5 . . ?
C13 C14 N1 114.78(19) . . ?
C13 C14 H14A 108.6 . . ?
C13 C14 H14B 108.6 . . ?
C8 C9 H9A 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C10 C9 C8 112.6(2) . . ?
C10 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
O5 C1 C1 115.8(2) . 3_666 ?
O6 C1 O5 126.7(2) . . ?
O6 C1 C1 117.4(2) . 3_666 ?
O3 C2 C2 115.9(3) . 3_766 ?
O4 C2 O3 126.7(2) . . ?
O4 C2 C2 117.4(2) . 3_766 ?
N1 C15 H15A 108.4 . . ?
N1 C15 H15B 108.4 . . ?
H15A C15 H15B 107.4 . . ?
C16 C15 N1 115.63(19) . . ?
C16 C15 H15A 108.4 . . ?
C16 C15 H15B 108.4 . . ?
N1 C6 H6A 108.3 . . ?
N1 C6 H6B 108.3 . . ?
N1 C6 C5 115.89(19) . . ?
H6A C6 H6B 107.4 . . ?
C5 C6 H6A 108.3 . . ?
C5 C6 H6B 108.3 . . ?
C14 C13 H13A 109.3 . . ?
C14 C13 H13B 109.3 . . ?
C14 C13 C12 111.8(2) . . ?
H13A C13 H13B 107.9 . . ?
C12 C13 H13A 109.3 . . ?
C12 C13 H13B 109.3 . . ?
C13 C12 H12A 108.8 . . ?
C13 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
C11 C12 C13 113.9(2) . . ?
C11 C12 H12A 108.8 . . ?
C11 C12 H12B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C5 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
C3 C4 C5 113.4(3) . . ?
C6 C5 C4 110.2(2) . . ?
C6 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
C4 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
H18A C18 H18B 107.6 . . ?
C16 C18 H18A 108.8 . . ?
C16 C18 H18B 108.8 . . ?
C17 C18 H18A 108.8 . . ?
C17 C18 H18B 108.8 . . ?
C17 C18 C16 114.0(3) . . ?
C15 C16 C18 110.2(2) . . ?
C15 C16 H16A 109.6 . . ?
C15 C16 H16B 109.6 . . ?
C18 C16 H16A 109.6 . . ?
C18 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

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 O5 C1 O6 -177.96(17) . . . . ?
V1 O5 C1 C1 2.4(3) . . . 3_666 ?
V1 O3 C2 O4 -173.00(17) . . . . ?
V1 O3 C2 C2 7.7(3) . . . 3_766 ?
V1 O6 C1 O5 -178.07(18) 3_666 . . . ?
V1 O6 C1 C1 1.6(3) 3_666 . . 3_666 ?
V1 O4 C2 O3 -173.70(18) 3_766 . . . ?
V1 O4 C2 C2 5.6(3) 3_766 . . 3_766 ?
N1 C14 C13 C12 -179.4(2) . . . . ?
N1 C15 C16 C18 -174.8(2) . . . . ?
N1 C6 C5 C4 171.5(2) . . . . ?
C7 N1 C14 C13 -56.8(3) . . . . ?
C7 N1 C15 C16 61.7(3) . . . . ?
C7 N1 C6 C5 173.7(2) . . . . ?
C7 C8 C9 C10 -173.0(2) . . . . ?
C14 N1 C7 C8 -55.9(3) . . . . ?
C14 N1 C15 C16 -177.3(2) . . . . ?
C14 N1 C6 C5 52.4(3) . . . . ?
C14 C13 C12 C11 -67.1(3) . . . . ?
C9 C8 C7 N1 178.2(2) . . . . ?
C15 N1 C7 C8 61.8(3) . . . . ?
C15 N1 C14 C13 -177.5(2) . . . . ?
C15 N1 C6 C5 -65.5(3) . . . . ?
C6 N1 C7 C8 -177.1(2) . . . . ?
C6 N1 C14 C13 61.2(3) . . . . ?
C6 N1 C15 C16 -56.1(3) . . . . ?
C17 C18 C16 C15 70.6(3) . . . . ?
C3 C4 C5 C6 -76.7(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_rzv-7
_database_code_depnum_ccdc_archive 'CCDC 2364917'
loop_
_audit_author_name
_audit_author_address
"Sofiya Vorob'eva"
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2024-08-09 deposited with the CCDC.	2024-08-16 downloaded from the CCDC.
;
_audit_creation_date             2024-06-10
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(H6 N2 Pt0.5), C4 H2 O10 V, 2(H2 O)'
_chemical_formula_sum            'C4 H18 N4 O12 Pt V'
_chemical_formula_weight         560.25
_chemical_melting_point          ?
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'
Pt Pt -1.7033 8.3905 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.27950(10)
_cell_length_b                   8.24340(10)
_cell_length_c                   12.9863(2)
_cell_angle_alpha                108.1350(10)
_cell_angle_beta                 97.3040(10)
_cell_angle_gamma                95.7430(10)
_cell_volume                     726.455(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      33.12
_cell_measurement_theta_min      2.61
_shelx_estimated_absorpt_T_max   0.683
_shelx_estimated_absorpt_T_min   0.425
_exptl_absorpt_coefficient_mu    10.331
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0681 before and 0.0359 after correction.
The Ratio of minimum to maximum transmission is 0.8040.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light blue'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.561
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             534
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15497
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.132
_diffrn_reflns_theta_min         1.674
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_measurement_details      
'Data collection was performed by Sukhikh A.S. in XRD Facility of NIIC SB RAS'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4682
_reflns_number_total             5492
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.611
_refine_diff_density_min         -1.578
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         5492
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0192
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0143P)²+0.3056P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0414
_refine_ls_wR_factor_ref         0.0433
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O4(H4D,H4E), O5(H5A,H5B)
2.b Rotating group:
 O2(H2A,H2B)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2C,H2D,H2E), N3(H3A,H3B,H3C), N4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Pt1 Pt 1.000000 1.000000 0.500000 0.01062(3) Uani 1 2 d S . P . .
N1 N 1.0053(3) 0.7568(2) 0.50907(15) 0.0163(4) Uani 1 1 d . . . . .
H1A H 1.098572 0.709701 0.475108 0.020 Uiso 1 1 calc R U . . .
H1B H 0.893473 0.689937 0.475315 0.020 Uiso 1 1 calc R U . . .
H1C H 1.026356 0.762704 0.580829 0.020 Uiso 1 1 calc R U . . .
N2 N 0.9024(3) 1.0761(3) 0.64637(16) 0.0197(4) Uani 1 1 d . . . . .
H2C H 0.775011 1.062418 0.633198 0.024 Uiso 1 1 calc R U . . .
H2D H 0.948164 1.189156 0.683272 0.024 Uiso 1 1 calc R U . . .
H2E H 0.940559 1.010630 0.687620 0.024 Uiso 1 1 calc R U . . .
Pt2 Pt 0.500000 1.000000 1.000000 0.01358(3) Uani 1 2 d S . P . .
N3 N 0.6789(3) 1.0525(2) 0.90135(17) 0.0194(4) Uani 1 1 d . . . . .
H3A H 0.619662 1.013203 0.830246 0.023 Uiso 1 1 calc R U . . .
H3B H 0.781251 0.999176 0.907732 0.023 Uiso 1 1 calc R U . . .
H3C H 0.715325 1.168524 0.922182 0.023 Uiso 1 1 calc R U . . .
N4 N 0.2923(3) 0.8922(3) 0.86798(17) 0.0234(4) Uani 1 1 d . . . . .
H4A H 0.343502 0.854264 0.805974 0.028 Uiso 1 1 calc R U . . .
H4B H 0.218264 0.972355 0.861625 0.028 Uiso 1 1 calc R U . . .
H4C H 0.222133 0.801597 0.877287 0.028 Uiso 1 1 calc R U . . .
V1 V 0.81360(5) 0.60867(5) 0.76397(3) 0.01133(7) Uani 1 1 d . . . . .
O1 O 0.9015(2) 0.7563(2) 0.72006(13) 0.0180(3) Uani 1 1 d . . . . .
O2 O 1.0436(2) 0.4873(2) 0.76959(13) 0.0155(3) Uani 1 1 d . . . . .
H2A H 1.122268 0.521470 0.732526 0.023 Uiso 1 1 d R U . . .
H2B H 1.104137 0.521259 0.836836 0.023 Uiso 1 1 d R U . . .
O11 O 0.5459(2) 0.6466(2) 0.75061(12) 0.0154(3) Uani 1 1 d . . . . .
O12 O 0.7088(2) 0.4104(2) 0.62901(12) 0.0153(3) Uani 1 1 d . . . . .
O13 O 0.2708(2) 0.5510(2) 0.63802(13) 0.0189(3) Uani 1 1 d . . . . .
O14 O 0.4446(2) 0.2966(2) 0.50672(14) 0.0226(4) Uani 1 1 d . . . . .
O21 O 0.8897(2) 0.76538(19) 0.92351(12) 0.0142(3) Uani 1 1 d . . . . .
O22 O 0.7303(2) 0.44678(19) 0.85906(12) 0.0150(3) Uani 1 1 d . . . . .
O23 O 0.8926(2) 0.7908(2) 1.10065(13) 0.0178(3) Uani 1 1 d . . . . .
O24 O 0.7640(2) 0.4381(2) 1.03029(13) 0.0195(3) Uani 1 1 d . . . . .
C00K C 0.5335(3) 0.4025(3) 0.59054(17) 0.0143(4) Uani 1 1 d . . . . .
C00L C 0.8603(3) 0.7078(3) 1.00168(17) 0.0124(4) Uani 1 1 d . . . . .
C00M C 0.7770(3) 0.5142(3) 0.96226(17) 0.0127(4) Uani 1 1 d . . . . .
C00N C 0.4389(3) 0.5446(3) 0.66396(17) 0.0144(4) Uani 1 1 d . . . . .
O4 O 0.3632(3) 0.2685(2) 0.76107(15) 0.0260(4) Uani 1 1 d G . . . .
H4D H 0.279519 0.248409 0.799546 0.039 Uiso 1 1 d G U . . .
H4E H 0.467648 0.320090 0.804864 0.039 Uiso 1 1 d G U . . .
O5 O 0.4934(4) -0.0330(3) 0.66993(18) 0.0523(7) Uani 1 1 d G . . . .
H5A H 0.429141 0.048365 0.664751 0.078 Uiso 1 1 d G U . . .
H5B H 0.489541 -0.107028 0.604844 0.078 Uiso 1 1 d G 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
Pt1 N1 2.0485(18) . ?
Pt1 N1 2.0485(18) 2_776 ?
Pt1 N2 2.0500(18) . ?
Pt1 N2 2.0500(18) 2_776 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N2 H2C 0.9100 . ?
N2 H2D 0.9100 . ?
N2 H2E 0.9100 . ?
Pt2 N3 2.0446(19) 2_677 ?
Pt2 N3 2.0446(19) . ?
Pt2 N4 2.0345(19) . ?
Pt2 N4 2.035(2) 2_677 ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N4 H4C 0.9100 . ?
V1 O1 1.6080(16) . ?
V1 O2 2.0395(15) . ?
V1 O11 1.9985(15) . ?
V1 O12 1.9881(16) . ?
V1 O21 2.0413(15) . ?
V1 O22 2.1743(15) . ?
O2 H2A 0.8724 . ?
O2 H2B 0.8720 . ?
O11 C00N 1.279(3) . ?
O12 C00K 1.297(3) . ?
O13 C00N 1.238(3) . ?
O14 C00K 1.217(3) . ?
O21 C00L 1.279(2) . ?
O22 C00M 1.266(2) . ?
O23 C00L 1.232(2) . ?
O24 C00M 1.240(2) . ?
C00K C00N 1.546(3) . ?
C00L C00M 1.548(3) . ?
O4 H4D 0.8701 . ?
O4 H4E 0.8700 . ?
O5 H5A 0.8698 . ?
O5 H5B 0.8700 . ?

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
N1 Pt1 N1 180.0 . 2_776 ?
N1 Pt1 N2 90.58(8) 2_776 2_776 ?
N1 Pt1 N2 90.58(8) . . ?
N1 Pt1 N2 89.42(8) . 2_776 ?
N1 Pt1 N2 89.42(8) 2_776 . ?
N2 Pt1 N2 180.0 . 2_776 ?
Pt1 N1 H1A 109.5 . . ?
Pt1 N1 H1B 109.5 . . ?
Pt1 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
Pt1 N2 H2C 109.5 . . ?
Pt1 N2 H2D 109.5 . . ?
Pt1 N2 H2E 109.5 . . ?
H2C N2 H2D 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
N3 Pt2 N3 180.0 2_677 . ?
N4 Pt2 N3 89.14(9) 2_677 . ?
N4 Pt2 N3 90.86(8) 2_677 2_677 ?
N4 Pt2 N3 89.14(9) . 2_677 ?
N4 Pt2 N3 90.86(8) . . ?
N4 Pt2 N4 180.0 . 2_677 ?
Pt2 N3 H3A 109.5 . . ?
Pt2 N3 H3B 109.5 . . ?
Pt2 N3 H3C 109.5 . . ?
H3A N3 H3B 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
Pt2 N4 H4A 109.5 . . ?
Pt2 N4 H4B 109.5 . . ?
Pt2 N4 H4C 109.5 . . ?
H4A N4 H4B 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
O1 V1 O2 97.32(7) . . ?
O1 V1 O11 99.97(8) . . ?
O1 V1 O12 104.86(8) . . ?
O1 V1 O21 91.55(7) . . ?
O1 V1 O22 166.99(7) . . ?
O2 V1 O21 92.83(6) . . ?
O2 V1 O22 80.51(6) . . ?
O11 V1 O2 160.46(7) . . ?
O11 V1 O21 95.73(6) . . ?
O11 V1 O22 84.60(6) . . ?
O12 V1 O2 85.77(6) . . ?
O12 V1 O11 81.07(6) . . ?
O12 V1 O21 163.59(6) . . ?
O12 V1 O22 87.83(6) . . ?
O21 V1 O22 75.82(6) . . ?
V1 O2 H2A 109.5 . . ?
V1 O2 H2B 109.5 . . ?
H2A O2 H2B 104.4 . . ?
C00N O11 V1 114.99(13) . . ?
C00K O12 V1 115.72(13) . . ?
C00L O21 V1 120.06(13) . . ?
C00M O22 V1 115.36(13) . . ?
O12 C00K C00N 113.02(18) . . ?
O14 C00K O12 126.3(2) . . ?
O14 C00K C00N 120.7(2) . . ?
O21 C00L C00M 113.76(18) . . ?
O23 C00L O21 126.3(2) . . ?
O23 C00L C00M 119.90(18) . . ?
O22 C00M C00L 114.47(18) . . ?
O24 C00M O22 125.7(2) . . ?
O24 C00M C00L 119.80(19) . . ?
O11 C00N C00K 114.84(18) . . ?
O13 C00N O11 125.1(2) . . ?
O13 C00N C00K 120.0(2) . . ?
H4D O4 H4E 109.4 . . ?
H5A O5 H5B 109.5 . . ?

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 O11 C00N O13 -176.96(17) . . . . ?
V1 O11 C00N C00K 4.5(2) . . . . ?
V1 O12 C00K O14 176.68(18) . . . . ?
V1 O12 C00K C00N -4.1(2) . . . . ?
V1 O21 C00L O23 -176.86(17) . . . . ?
V1 O21 C00L C00M 3.4(2) . . . . ?
V1 O22 C00M O24 -170.63(17) . . . . ?
V1 O22 C00M C00L 8.0(2) . . . . ?
O12 C00K C00N O11 -0.3(3) . . . . ?
O12 C00K C00N O13 -178.93(19) . . . . ?
O14 C00K C00N O11 179.0(2) . . . . ?
O14 C00K C00N O13 0.4(3) . . . . ?
O21 C00L C00M O22 -7.7(3) . . . . ?
O21 C00L C00M O24 171.01(19) . . . . ?
O23 C00L C00M O22 172.56(19) . . . . ?
O23 C00L C00M O24 -8.7(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_bch-337-2
_database_code_depnum_ccdc_archive 'CCDC 2364932'
loop_
_audit_author_name
_audit_author_address
"Sofiya Vorob'eva"
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2024-08-09 deposited with the CCDC.	2024-08-16 downloaded from the CCDC.
;
_audit_creation_date             2024-06-10
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(H6 N2 Pt0.5), C4 O9 V'
_chemical_formula_sum            'C4 H12 N4 O9 Pt V'
_chemical_formula_weight         506.21
_chemical_melting_point          ?
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'
Pt Pt -1.7033 8.3905 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.603(8)
_cell_length_b                   7.945(3)
_cell_length_c                   15.358(6)
_cell_angle_alpha                90
_cell_angle_beta                 97.242(13)
_cell_angle_gamma                90
_cell_volume                     2372.8(16)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    175
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      17.27
_cell_measurement_theta_min      2.67
_shelx_estimated_absorpt_T_max   0.884
_shelx_estimated_absorpt_T_min   0.571
_exptl_absorpt_coefficient_mu    12.618
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.5846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0868 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.7848.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.834
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1196
_diffrn_reflns_av_unetI/netI     0.1500
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4516
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        23.261
_diffrn_reflns_theta_max         23.261
_diffrn_reflns_theta_min         2.674
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_measurement_details      
'Data collection was performed by Kochelakov D. in XRD Facility of NIIC SB RAS'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1070
_reflns_number_total             1703
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.332
_refine_diff_density_min         -1.555
_refine_diff_density_rms         0.369
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         1703
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0561
_refine_ls_restrained_S_all      0.930
_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)+(0.0188P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1190
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 O11, O12, O13, O14, C1, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O21, O22, O23, O24, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N3(H3A,H3B,H3C), N4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Pt1 Pt 0.500000 0.000000 0.500000 0.0159(3) Uani 1 2 d S . P . .
N1 N 0.4695(7) 0.2370(19) 0.5322(10) 0.017(4) Uani 1 1 d . . . . .
H1A H 0.442592 0.282598 0.485507 0.021 Uiso 1 1 calc R U . . .
H1B H 0.507245 0.302895 0.546411 0.021 Uiso 1 1 calc R U . . .
H1C H 0.445251 0.230388 0.578787 0.021 Uiso 1 1 calc R U . . .
N2 N 0.4714(8) 0.050(2) 0.3695(11) 0.025(5) Uani 1 1 d . U . . .
H2A H 0.497332 -0.012551 0.336599 0.030 Uiso 1 1 calc R U . . .
H2B H 0.477984 0.161475 0.359131 0.030 Uiso 1 1 calc R U . . .
H2C H 0.426203 0.024160 0.354989 0.030 Uiso 1 1 calc R U . . .
Pt2 Pt 0.250000 0.250000 0.000000 0.0180(3) Uani 1 2 d S . P . .
N3 N 0.3275(8) 0.101(2) 0.0593(12) 0.027(5) Uani 1 1 d . . . . .
H3A H 0.363421 0.102983 0.027188 0.033 Uiso 1 1 calc R U . . .
H3B H 0.311948 -0.005934 0.062951 0.033 Uiso 1 1 calc R U . . .
H3C H 0.341508 0.141261 0.114219 0.033 Uiso 1 1 calc R U . . .
N4 N 0.3225(8) 0.4343(19) -0.0117(11) 0.023(4) Uani 1 1 d . U . . .
H4A H 0.303714 0.516230 -0.048580 0.028 Uiso 1 1 calc R U . . .
H4B H 0.359244 0.388271 -0.033584 0.028 Uiso 1 1 calc R U . . .
H4C H 0.336393 0.479605 0.042067 0.028 Uiso 1 1 calc R U . . .
V1 V 0.34882(16) 0.7461(5) 0.2253(2) 0.0216(9) Uani 1 1 d . . . . .
O1 O 0.4048(6) 0.8617(18) 0.1866(9) 0.025(4) Uani 1 1 d . . . . .
O11 O 0.3713(6) 0.5241(16) 0.1722(9) 0.019(3) Uani 1 1 d . . . . .
O12 O 0.4051(7) 0.6468(17) 0.3287(10) 0.033(4) Uani 1 1 d . . . . .
O13 O 0.4058(7) 0.2645(18) 0.2136(10) 0.034(4) Uani 1 1 d . . . . .
O14 O 0.4656(8) 0.4194(18) 0.3714(11) 0.041(5) Uani 1 1 d . . . . .
O21 O 0.2337(7) 1.0849(19) 0.2348(10) 0.026(4) Uani 1 1 d . . . . .
O22 O 0.3204(6) 0.9264(16) 0.3042(9) 0.023(3) Uani 1 1 d . . . . .
O23 O 0.2279(7) 1.2751(17) 0.3722(9) 0.027(4) Uani 1 1 d . . . . .
O24 O 0.3335(7) 1.1864(16) 0.4284(10) 0.028(4) Uani 1 1 d . . . . .
C1 C 0.4270(10) 0.496(3) 0.3177(14) 0.025(4) Uani 1 1 d . . . . .
C2 C 0.4004(11) 0.417(3) 0.2229(16) 0.027(5) Uani 1 1 d . . . . .
C3 C 0.2773(11) 1.050(3) 0.2959(16) 0.028(5) Uani 1 1 d . . . . .
C4 C 0.2834(10) 1.176(3) 0.3752(15) 0.026(5) Uani 1 1 d . . . . .


_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
Pt1 N1 2.054(15) . ?
Pt1 N1 2.054(15) 5_656 ?
Pt1 N2 2.051(16) . ?
Pt1 N2 2.051(16) 5_656 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
Pt2 N3 2.044(15) . ?
Pt2 N3 2.044(15) 7 ?
Pt2 N4 2.063(14) 7 ?
Pt2 N4 2.063(14) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N4 H4C 0.9100 . ?
V1 O1 1.601(14) . ?
V1 O11 2.015(13) . ?
V1 O12 1.979(14) . ?
V1 O21 2.210(14) 4_545 ?
V1 O22 2.000(14) . ?
V1 O23 1.997(13) 4_545 ?
O11 C2 1.24(2) . ?
O12 C1 1.29(3) . ?
O13 C2 1.23(2) . ?
O14 C1 1.21(2) . ?
O21 C3 1.22(2) . ?
O22 C3 1.29(2) . ?
O23 C4 1.34(2) . ?
O24 C4 1.20(2) . ?
C1 C2 1.61(3) . ?
C3 C4 1.57(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
N1 Pt1 N1 180.0 . 5_656 ?
N2 Pt1 N1 89.7(6) 5_656 . ?
N2 Pt1 N1 89.7(6) . 5_656 ?
N2 Pt1 N1 90.3(6) . . ?
N2 Pt1 N1 90.3(6) 5_656 5_656 ?
N2 Pt1 N2 180.0(9) . 5_656 ?
Pt1 N1 H1A 109.5 . . ?
Pt1 N1 H1B 109.5 . . ?
Pt1 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
Pt1 N2 H2A 109.5 . . ?
Pt1 N2 H2B 109.5 . . ?
Pt1 N2 H2C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
N3 Pt2 N3 180.0(6) 7 . ?
N3 Pt2 N4 88.1(6) 7 7 ?
N3 Pt2 N4 91.9(6) . 7 ?
N3 Pt2 N4 91.9(6) 7 . ?
N3 Pt2 N4 88.1(6) . . ?
N4 Pt2 N4 180.0(10) . 7 ?
Pt2 N3 H3A 109.5 . . ?
Pt2 N3 H3B 109.5 . . ?
Pt2 N3 H3C 109.5 . . ?
H3A N3 H3B 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
Pt2 N4 H4A 109.5 . . ?
Pt2 N4 H4B 109.5 . . ?
Pt2 N4 H4C 109.5 . . ?
H4A N4 H4B 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
O1 V1 O11 99.0(7) . . ?
O1 V1 O12 100.9(6) . . ?
O1 V1 O21 174.3(6) . 4_545 ?
O1 V1 O22 94.0(7) . . ?
O1 V1 O23 98.1(7) . 4_545 ?
O11 V1 O21 79.0(5) . 4_545 ?
O12 V1 O11 81.3(6) . . ?
O12 V1 O21 84.3(6) . 4_545 ?
O12 V1 O22 88.2(6) . . ?
O12 V1 O23 159.7(6) . 4_545 ?
O22 V1 O11 164.5(6) . . ?
O22 V1 O21 88.7(6) . 4_545 ?
O23 V1 O11 88.8(6) 4_545 . ?
O23 V1 O21 76.5(6) 4_545 4_545 ?
O23 V1 O22 97.5(6) 4_545 . ?
C2 O11 V1 116.8(14) . . ?
C1 O12 V1 115.2(14) . . ?
C3 O21 V1 112.6(15) . 4 ?
C3 O22 V1 135.5(14) . . ?
C4 O23 V1 119.3(13) . 4 ?
O12 C1 C2 113.8(18) . . ?
O14 C1 O12 125(2) . . ?
O14 C1 C2 122(2) . . ?
O11 C2 C1 111.9(18) . . ?
O13 C2 O11 130(2) . . ?
O13 C2 C1 118(2) . . ?
O21 C3 O22 129(2) . . ?
O21 C3 C4 116(2) . . ?
O22 C3 C4 114.9(19) . . ?
O23 C4 C3 111.4(18) . . ?
O24 C4 O23 125(2) . . ?
O24 C4 C3 124(2) . . ?

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 O11 C2 O13 162(2) . . . . ?
V1 O11 C2 C1 -11(2) . . . . ?
V1 O12 C1 O14 175.0(17) . . . . ?
V1 O12 C1 C2 -3(2) . . . . ?
V1 O21 C3 O22 158(2) 4 . . . ?
V1 O21 C3 C4 -23(2) 4 . . . ?
V1 O22 C3 O21 8(4) . . . . ?
V1 O22 C3 C4 -170.1(13) . . . . ?
V1 O23 C4 O24 176.8(17) 4 . . . ?
V1 O23 C4 C3 1(2) 4 . . . ?
O12 C1 C2 O11 10(3) . . . . ?
O12 C1 C2 O13 -164(2) . . . . ?
O14 C1 C2 O11 -168.4(19) . . . . ?
O14 C1 C2 O13 18(3) . . . . ?
O21 C3 C4 O23 16(3) . . . . ?
O21 C3 C4 O24 -160(2) . . . . ?
O22 C3 C4 O23 -165.0(18) . . . . ?
O22 C3 C4 O24 19(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_THETM01_bch-337-2           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
Calculated sin(theta_max)/wavelength = 0.5557
RESPONSE: Compound precipitates as a fine crystalline powder, 
after numerous attempts we succeeded in obtaining a small crystal.
The quality of the XRD data is enought for solving reasonable structure,
but there is no diffraction below d<0.9 Ang.
;
