# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 2106164'
loop_
_audit_author_name
_audit_author_address
'jian zhou'
;Chongqing Normal University
China
;
_audit_update_record             
;
2021-08-29 deposited with the CCDC.	2021-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H34 N2 O16 V4'
_chemical_formula_sum            'C18 H34 N2 O16 V4'
_chemical_formula_weight         738.23

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.8770(16)
_cell_length_b                   10.9486(18)
_cell_length_c                   11.9696(17)
_cell_angle_alpha                90
_cell_angle_beta                 104.698(5)
_cell_angle_gamma                90
_cell_volume                     1378.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    15850
_cell_measurement_theta_min      2.6818
_cell_measurement_theta_max      27.9045

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_F_000             752
_exptl_transmission_factor_min   0.575
_exptl_transmission_factor_max   0.850
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.337
_exptl_crystal_size_min          0.116
_exptl_absorpt_coefficient_mu    1.390
_shelx_estimated_absorpt_T_min   0.600
_shelx_estimated_absorpt_T_max   0.855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11928
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.929
_diffrn_reflns_theta_max         25.095
_diffrn_reflns_theta_full        25.095
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2440
_reflns_number_gt                2155
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0239P)²+2.6009P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2440
_refine_ls_number_parameters     181
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0305
_refine_ls_wR_factor_ref         0.0785
_refine_ls_wR_factor_gt          0.0741
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.103
_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 0.61477(4) 0.71267(4) 0.43898(4) 0.01685(13) Uani 1 1 d . . . . .
V2 V 0.64815(4) 0.44021(4) 0.55112(4) 0.01493(13) Uani 1 1 d . . . . .
O1 O 0.67950(17) 0.61565(16) 0.58341(14) 0.0165(4) Uani 1 1 d . . . . .
O2 O 0.45618(16) 0.48682(16) 0.59577(14) 0.0158(4) Uani 1 1 d . . . . .
O3 O 0.7844(2) 0.5802(2) 0.93955(18) 0.0335(5) Uani 1 1 d . . . . .
H3A H 0.8051 0.5118 0.9653 0.050 Uiso 1 1 calc R U . . .
O4 O 0.78144(18) 0.38975(19) 0.53970(18) 0.0277(5) Uani 1 1 d . . . . .
O5 O 0.55164(17) 0.28540(16) 0.52458(16) 0.0195(4) Uani 1 1 d D . . . .
H5 H 0.5830 0.2159 0.4966 0.023 Uiso 1 1 calc DR U . . .
O6 O 0.6734(2) 0.84373(19) 0.48300(18) 0.0314(5) Uani 1 1 d . . . . .
O7 O 0.52297(18) 0.74780(18) 0.27633(16) 0.0231(4) Uani 1 1 d . . . . .
O8 O 0.75444(17) 0.64361(18) 0.37728(16) 0.0229(4) Uani 1 1 d . . . . .
N1 N 0.6797(2) 0.4397(2) 0.73345(18) 0.0176(5) Uani 1 1 d . . . . .
H1A H 0.6413 0.3764 0.7568 0.021 Uiso 1 1 calc R U . . .
H1B H 0.7624 0.4369 0.7681 0.021 Uiso 1 1 calc R U . . .
C1 C 0.6228(2) 0.5570(2) 0.7578(2) 0.0166(5) Uani 1 1 d . . . . .
C2 C 0.4796(3) 0.5456(2) 0.7049(2) 0.0186(6) Uani 1 1 d . . . . .
H2A H 0.4414 0.4988 0.7561 0.022 Uiso 1 1 calc R U . . .
H2B H 0.4413 0.6262 0.6957 0.022 Uiso 1 1 calc R U . . .
C3 C 0.6510(3) 0.5826(3) 0.8875(2) 0.0234(6) Uani 1 1 d . . . . .
H3B H 0.6172 0.6621 0.8998 0.028 Uiso 1 1 calc R U . . .
H3C H 0.6091 0.5217 0.9238 0.028 Uiso 1 1 calc R U . . .
C4 C 0.6814(3) 0.6551(2) 0.6967(2) 0.0195(6) Uani 1 1 d . . . . .
H4A H 0.6337 0.7305 0.6930 0.023 Uiso 1 1 calc R U . . .
H4B H 0.7683 0.6707 0.7398 0.023 Uiso 1 1 calc R U . . .
C5 C 0.4845(3) 0.8111(4) 0.0827(3) 0.0375(8) Uani 1 1 d . . . . .
H5A H 0.5285 0.8170 0.0228 0.056 Uiso 1 1 calc R U . . .
H5B H 0.4122 0.7582 0.0578 0.056 Uiso 1 1 calc R U . . .
H5C H 0.4565 0.8907 0.0989 0.056 Uiso 1 1 calc R U . . .
C6 C 0.5720(3) 0.7600(3) 0.1894(2) 0.0229(6) Uani 1 1 d . . . . .
C7 C 0.6933(3) 0.7236(3) 0.1888(2) 0.0281(7) Uani 1 1 d . . . . .
H7A H 0.7225 0.7427 0.1243 0.034 Uiso 1 1 calc R U . . .
C8 C 0.7749(3) 0.6603(3) 0.2785(2) 0.0218(6) Uani 1 1 d . . . . .
C9 C 0.8923(3) 0.6024(3) 0.2593(3) 0.0365(8) Uani 1 1 d . . . . .
H9A H 0.8987 0.6205 0.1825 0.055 Uiso 1 1 calc R U . . .
H9B H 0.9655 0.6340 0.3143 0.055 Uiso 1 1 calc R U . . .
H9C H 0.8880 0.5155 0.2686 0.055 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 O6 1.604(2) . ?
V1 O5 1.9666(19) 3_666 ?
V1 O7 1.9871(19) . ?
V1 O8 1.9986(19) . ?
V1 O1 1.9988(18) . ?
V1 O2 2.3186(18) 3_666 ?
V2 O4 1.5895(19) . ?
V2 O1 1.9719(19) . ?
V2 O5 1.9764(19) . ?
V2 O2 2.0013(18) 3_666 ?
V2 N1 2.121(2) . ?
V2 O2 2.3394(18) . ?
O1 C4 1.418(3) . ?
O2 C2 1.420(3) . ?
O2 V2 2.0013(18) 3_666 ?
O2 V1 2.3186(18) 3_666 ?
O3 C3 1.427(3) . ?
O3 H3A 0.8200 . ?
O5 V1 1.9667(19) 3_666 ?
O5 H5 0.9300 . ?
O7 C6 1.291(3) . ?
O8 C8 1.270(3) . ?
N1 C1 1.486(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
C1 C4 1.527(4) . ?
C1 C3 1.530(3) . ?
C1 C2 1.530(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3B 0.9700 . ?
C3 H3C 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.495(4) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.380(4) . ?
C7 C8 1.392(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.495(4) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?

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
O6 V1 O5 103.25(10) . 3_666 ?
O6 V1 O7 101.99(10) . . ?
O5 V1 O7 87.32(8) 3_666 . ?
O6 V1 O8 100.58(10) . . ?
O5 V1 O8 156.16(8) 3_666 . ?
O7 V1 O8 87.21(8) . . ?
O6 V1 O1 99.66(9) . . ?
O5 V1 O1 87.47(7) 3_666 . ?
O7 V1 O1 158.34(8) . . ?
O8 V1 O1 89.12(7) . . ?
O6 V1 O2 171.16(9) . 3_666 ?
O5 V1 O2 76.51(7) 3_666 3_666 ?
O7 V1 O2 86.84(7) . 3_666 ?
O8 V1 O2 80.04(7) . 3_666 ?
O1 V1 O2 71.50(7) . 3_666 ?
O4 V2 O1 103.85(9) . . ?
O4 V2 O5 98.45(9) . . ?
O1 V2 O5 157.70(8) . . ?
O4 V2 O2 112.92(9) . 3_666 ?
O1 V2 O2 79.32(7) . 3_666 ?
O5 V2 O2 92.38(8) . 3_666 ?
O4 V2 N1 100.06(10) . . ?
O1 V2 N1 79.99(8) . . ?
O5 V2 N1 95.95(8) . . ?
O2 V2 N1 144.34(8) 3_666 . ?
O4 V2 O2 169.11(9) . . ?
O1 V2 O2 82.11(7) . . ?
O5 V2 O2 75.84(7) . . ?
O2 V2 O2 76.91(7) 3_666 . ?
N1 V2 O2 71.72(7) . . ?
C4 O1 V2 116.36(15) . . ?
C4 O1 V1 125.56(16) . . ?
V2 O1 V1 110.04(8) . . ?
C2 O2 V2 123.82(16) . 3_666 ?
C2 O2 V1 124.48(15) . 3_666 ?
V2 O2 V1 97.45(7) 3_666 3_666 ?
C2 O2 V2 110.28(14) . . ?
V2 O2 V2 103.08(7) 3_666 . ?
V1 O2 V2 91.68(6) 3_666 . ?
C3 O3 H3A 109.5 . . ?
V1 O5 V2 115.87(9) 3_666 . ?
V1 O5 H5 122.1 3_666 . ?
V2 O5 H5 122.1 . . ?
C6 O7 V1 127.01(17) . . ?
C8 O8 V1 128.22(18) . . ?
C1 N1 V2 103.45(15) . . ?
C1 N1 H1A 111.1 . . ?
V2 N1 H1A 111.1 . . ?
C1 N1 H1B 111.1 . . ?
V2 N1 H1B 111.1 . . ?
H1A N1 H1B 109.0 . . ?
N1 C1 C4 105.6(2) . . ?
N1 C1 C3 111.8(2) . . ?
C4 C1 C3 110.9(2) . . ?
N1 C1 C2 106.2(2) . . ?
C4 C1 C2 111.3(2) . . ?
C3 C1 C2 110.8(2) . . ?
O2 C2 C1 110.1(2) . . ?
O2 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
O2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
O3 C3 C1 111.1(2) . . ?
O3 C3 H3B 109.4 . . ?
C1 C3 H3B 109.4 . . ?
O3 C3 H3C 109.4 . . ?
C1 C3 H3C 109.4 . . ?
H3B C3 H3C 108.0 . . ?
O1 C4 C1 109.7(2) . . ?
O1 C4 H4A 109.7 . . ?
C1 C4 H4A 109.7 . . ?
O1 C4 H4B 109.7 . . ?
C1 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O7 C6 C7 124.4(3) . . ?
O7 C6 C5 115.1(3) . . ?
C7 C6 C5 120.4(3) . . ?
C6 C7 C8 124.3(3) . . ?
C6 C7 H7A 117.9 . . ?
C8 C7 H7A 117.9 . . ?
O8 C8 C7 124.2(3) . . ?
O8 C8 C9 116.2(3) . . ?
C7 C8 C9 119.6(3) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 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
V2 N1 C1 C4 -51.8(2) . . . . ?
V2 N1 C1 C3 -172.50(18) . . . . ?
V2 N1 C1 C2 66.5(2) . . . . ?
V2 O2 C2 C1 -123.47(19) 3_666 . . . ?
V1 O2 C2 C1 106.0(2) 3_666 . . . ?
V2 O2 C2 C1 -0.9(2) . . . . ?
N1 C1 C2 O2 -40.9(3) . . . . ?
C4 C1 C2 O2 73.6(3) . . . . ?
C3 C1 C2 O2 -162.5(2) . . . . ?
N1 C1 C3 O3 55.5(3) . . . . ?
C4 C1 C3 O3 -62.1(3) . . . . ?
C2 C1 C3 O3 173.7(2) . . . . ?
V2 O1 C4 C1 -15.4(3) . . . . ?
V1 O1 C4 C1 130.17(19) . . . . ?
N1 C1 C4 O1 45.5(3) . . . . ?
C3 C1 C4 O1 166.8(2) . . . . ?
C2 C1 C4 O1 -69.3(3) . . . . ?
V1 O7 C6 C7 15.5(4) . . . . ?
V1 O7 C6 C5 -168.0(2) . . . . ?
O7 C6 C7 C8 5.4(5) . . . . ?
C5 C6 C7 C8 -170.9(3) . . . . ?
V1 O8 C8 C7 -6.3(4) . . . . ?
V1 O8 C8 C9 176.3(2) . . . . ?
C6 C7 C8 O8 -10.3(5) . . . . ?
C6 C7 C8 C9 167.0(3) . . . . ?

_refine_diff_density_max         0.778
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.076

####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 2106167'
loop_
_audit_author_name
_audit_author_address
'jian zhou'
;Chongqing Normal University
China
;
_audit_update_record             
;
2021-08-29 deposited with the CCDC.	2021-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H30 N2 O18 V4'
_chemical_formula_sum            'C16 H30 N2 O18 V4'
_chemical_formula_weight         742.18

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   8.266(5)
_cell_length_b                   8.933(6)
_cell_length_c                   9.866(6)
_cell_angle_alpha                65.414(10)
_cell_angle_beta                 76.7110(16)
_cell_angle_gamma                85.4870(12)
_cell_volume                     644.6(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    14768
_cell_measurement_theta_min      2.5493
_cell_measurement_theta_max      27.9086

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_F_000             376
_exptl_transmission_factor_min   0.903
_exptl_transmission_factor_max   0.922
_exptl_crystal_size_max          0.072
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.052
_exptl_absorpt_coefficient_mu    1.493
_shelx_estimated_absorpt_T_min   0.900
_shelx_estimated_absorpt_T_max   0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11631
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.044
_diffrn_reflns_theta_max         25.098
_diffrn_reflns_theta_full        25.098
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2290
_reflns_number_gt                1943
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0287P)²+1.5768P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2290
_refine_ls_number_parameters     184
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0849
_refine_ls_wR_factor_gt          0.0795
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_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 0.72087(7) 0.66487(7) 0.23290(6) 0.01873(16) Uani 1 1 d . . . . .
V2 V 0.36224(6) 0.66201(6) 0.45386(6) 0.01546(15) Uani 1 1 d . . . . .
O1 O 0.5243(3) 0.4666(2) 0.3759(2) 0.0159(5) Uani 1 1 d . . . . .
O9 O 0.8152(3) 0.4968(3) 0.1387(3) 0.0283(6) Uani 1 1 d . . . . .
H9A H 0.7457 0.4178 0.1711 0.042 Uiso 1 1 d R U . . .
H9B H 0.9060 0.4597 0.1654 0.042 Uiso 1 1 d R U . . .
O8 O 0.5616(3) 0.7375(3) 0.0886(3) 0.0257(5) Uani 1 1 d . . . . .
O7 O 0.3115(3) 0.7256(3) 0.2466(3) 0.0228(5) Uani 1 1 d . . . . .
O5 O 0.2576(3) 0.7973(3) 0.5056(3) 0.0256(5) Uani 1 1 d . . . . .
O2 O 0.2092(3) 0.4644(3) 0.5684(2) 0.0175(5) Uani 1 1 d . . . . .
O4 O 0.1328(4) 0.3791(3) 0.1810(3) 0.0388(7) Uani 1 1 d . . . . .
O3 O 0.4240(3) 0.2112(2) 0.6601(2) 0.0173(5) Uani 1 1 d . . . . .
O6 O 0.8718(3) 0.7966(3) 0.1423(3) 0.0327(6) Uani 1 1 d . . . . .
N1 N 0.2198(4) 0.1726(3) 0.3802(3) 0.0225(6) Uani 1 1 d . . . . .
H1 H 0.2250 0.0673 0.4260 0.027 Uiso 1 1 calc R U . . .
C1 C 0.2914(4) 0.2700(4) 0.4445(4) 0.0190(7) Uani 1 1 d . . . . .
C2 C 0.1544(4) 0.3782(4) 0.4910(4) 0.0197(7) Uani 1 1 d . . . . .
H2A H 0.1203 0.4578 0.4003 0.024 Uiso 1 1 calc R U . . .
H2B H 0.0585 0.3092 0.5576 0.024 Uiso 1 1 calc R U . . .
C3 C 0.3452(4) 0.1400(4) 0.5860(4) 0.0200(7) Uani 1 1 d . . . . .
H3A H 0.2484 0.0762 0.6575 0.024 Uiso 1 1 calc R U . . .
H3B H 0.4214 0.0654 0.5559 0.024 Uiso 1 1 calc R U . . .
C4 C 0.4435(4) 0.3698(4) 0.3235(4) 0.0180(7) Uani 1 1 d . . . . .
H4A H 0.5229 0.2945 0.2982 0.022 Uiso 1 1 calc R U . . .
H4B H 0.4074 0.4424 0.2313 0.022 Uiso 1 1 calc R U . . .
C5 C 0.1483(5) 0.2292(5) 0.2595(4) 0.0296(8) Uani 1 1 d . . . . .
C6 C 0.0840(6) 0.0977(6) 0.2242(5) 0.0474(11) Uani 1 1 d . . . . .
H6A H -0.0160 0.1345 0.1871 0.071 Uiso 1 1 calc R U . . .
H6B H 0.0609 -0.0022 0.3153 0.071 Uiso 1 1 calc R U . . .
H6C H 0.1665 0.0778 0.1477 0.071 Uiso 1 1 calc R U . . .
C7 C 0.4049(4) 0.7581(4) 0.1150(4) 0.0230(7) Uani 1 1 d . . . . .
C8 C 0.3231(5) 0.8218(5) -0.0173(4) 0.0399(10) Uani 1 1 d . . . . .
H8A H 0.3936 0.9041 -0.1034 0.060 Uiso 1 1 calc R U . . .
H8B H 0.2188 0.8695 0.0087 0.060 Uiso 1 1 calc R U . . .
H8C H 0.3040 0.7329 -0.0428 0.060 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 O6 1.607(3) . ?
V1 O3 1.989(2) 2_666 ?
V1 O2 2.010(2) 2_666 ?
V1 O8 2.035(2) . ?
V1 O9 2.090(3) . ?
V1 O1 2.255(2) . ?
V2 O5 1.617(2) . ?
V2 O1 1.992(2) 2_666 ?
V2 O3 2.003(2) 2_666 ?
V2 O2 2.007(2) . ?
V2 O7 2.017(3) . ?
V2 O1 2.389(2) . ?
O1 C4 1.443(4) . ?
O1 V2 1.992(2) 2_666 ?
O9 H9A 0.8500 . ?
O9 H9B 0.8501 . ?
O8 C7 1.275(4) . ?
O7 C7 1.276(4) . ?
O2 C2 1.444(4) . ?
O2 V1 2.010(2) 2_666 ?
O4 C5 1.251(4) . ?
O3 C3 1.427(4) . ?
O3 V1 1.989(2) 2_666 ?
O3 V2 2.003(2) 2_666 ?
N1 C5 1.340(4) . ?
N1 C1 1.492(4) . ?
N1 H1 0.8600 . ?
C1 C3 1.533(4) . ?
C1 C2 1.544(4) . ?
C1 C4 1.550(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.520(5) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.488(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?

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
O6 V1 O3 98.70(12) . 2_666 ?
O6 V1 O2 101.03(12) . 2_666 ?
O3 V1 O2 86.37(10) 2_666 2_666 ?
O6 V1 O8 103.08(12) . . ?
O3 V1 O8 85.49(10) 2_666 . ?
O2 V1 O8 155.45(10) 2_666 . ?
O6 V1 O9 96.18(13) . . ?
O3 V1 O9 164.66(10) 2_666 . ?
O2 V1 O9 94.46(10) 2_666 . ?
O8 V1 O9 87.54(10) . . ?
O6 V1 O1 174.56(11) . . ?
O3 V1 O1 82.46(10) 2_666 . ?
O2 V1 O1 73.70(9) 2_666 . ?
O8 V1 O1 82.28(10) . . ?
O9 V1 O1 83.08(10) . . ?
O5 V2 O1 104.35(11) . 2_666 ?
O5 V2 O3 99.52(12) . 2_666 ?
O1 V2 O3 87.72(10) 2_666 2_666 ?
O5 V2 O2 101.43(12) . . ?
O1 V2 O2 79.82(9) 2_666 . ?
O3 V2 O2 157.71(9) 2_666 . ?
O5 V2 O7 101.01(11) . . ?
O1 V2 O7 154.53(9) 2_666 . ?
O3 V2 O7 85.84(10) 2_666 . ?
O2 V2 O7 97.49(9) . . ?
O5 V2 O1 178.28(10) . . ?
O1 V2 O1 75.16(9) 2_666 . ?
O3 V2 O1 78.83(9) 2_666 . ?
O2 V2 O1 80.14(9) . . ?
O7 V2 O1 79.42(9) . . ?
C4 O1 V2 115.36(18) . 2_666 ?
C4 O1 V1 126.61(18) . . ?
V2 O1 V1 98.47(9) 2_666 . ?
C4 O1 V2 118.08(17) . . ?
V2 O1 V2 104.84(9) 2_666 . ?
V1 O1 V2 88.61(9) . . ?
V1 O9 H9A 109.5 . . ?
V1 O9 H9B 109.1 . . ?
H9A O9 H9B 109.5 . . ?
C7 O8 V1 130.2(2) . . ?
C7 O7 V2 132.3(2) . . ?
C2 O2 V2 121.44(19) . . ?
C2 O2 V1 119.51(19) . 2_666 ?
V2 O2 V1 106.65(10) . 2_666 ?
C3 O3 V1 116.48(19) . 2_666 ?
C3 O3 V2 118.67(19) . 2_666 ?
V1 O3 V2 108.80(11) 2_666 2_666 ?
C5 N1 C1 127.9(3) . . ?
C5 N1 H1 116.1 . . ?
C1 N1 H1 116.1 . . ?
N1 C1 C3 104.4(2) . . ?
N1 C1 C2 109.0(3) . . ?
C3 C1 C2 110.4(3) . . ?
N1 C1 C4 108.0(3) . . ?
C3 C1 C4 111.0(3) . . ?
C2 C1 C4 113.6(3) . . ?
O2 C2 C1 112.4(2) . . ?
O2 C2 H2A 109.1 . . ?
C1 C2 H2A 109.1 . . ?
O2 C2 H2B 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
O3 C3 C1 112.4(3) . . ?
O3 C3 H3A 109.1 . . ?
C1 C3 H3A 109.1 . . ?
O3 C3 H3B 109.1 . . ?
C1 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
O1 C4 C1 112.5(2) . . ?
O1 C4 H4A 109.1 . . ?
C1 C4 H4A 109.1 . . ?
O1 C4 H4B 109.1 . . ?
C1 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
O4 C5 N1 123.4(3) . . ?
O4 C5 C6 121.4(3) . . ?
N1 C5 C6 115.3(3) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O8 C7 O7 125.2(3) . . ?
O8 C7 C8 117.7(3) . . ?
O7 C7 C8 117.1(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 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
C5 N1 C1 C3 176.8(3) . . . . ?
C5 N1 C1 C2 58.8(4) . . . . ?
C5 N1 C1 C4 -65.1(4) . . . . ?
V2 O2 C2 C1 75.5(3) . . . . ?
V1 O2 C2 C1 -61.6(3) 2_666 . . . ?
N1 C1 C2 O2 174.2(2) . . . . ?
C3 C1 C2 O2 60.1(3) . . . . ?
C4 C1 C2 O2 -65.3(3) . . . . ?
V1 O3 C3 C1 70.1(3) 2_666 . . . ?
V2 O3 C3 C1 -63.0(3) 2_666 . . . ?
N1 C1 C3 O3 177.6(2) . . . . ?
C2 C1 C3 O3 -65.5(3) . . . . ?
C4 C1 C3 O3 61.5(3) . . . . ?
V2 O1 C4 C1 67.6(3) 2_666 . . . ?
V1 O1 C4 C1 -168.66(18) . . . . ?
V2 O1 C4 C1 -57.4(3) . . . . ?
N1 C1 C4 O1 -178.9(2) . . . . ?
C3 C1 C4 O1 -65.0(3) . . . . ?
C2 C1 C4 O1 60.1(3) . . . . ?
C1 N1 C5 O4 0.5(6) . . . . ?
C1 N1 C5 C6 -178.8(3) . . . . ?
V1 O8 C7 O7 -4.7(5) . . . . ?
V1 O8 C7 C8 176.7(2) . . . . ?
V2 O7 C7 O8 9.0(5) . . . . ?
V2 O7 C7 C8 -172.4(2) . . . . ?

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
O9 H9B O4 0.85 1.97 2.807(4) 167.6 1_655
N1 H1 O5 0.86 2.22 3.070(4) 170.4 1_545
C2 H2A O7 0.97 2.64 3.178(4) 114.9 .
C2 H2A O4 0.97 2.52 3.102(5) 118.6 .
C4 H4B O7 0.97 2.65 3.113(4) 110.0 .
C4 H4B O4 0.97 2.58 3.179(4) 119.9 .

_refine_diff_density_max         0.969
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.078

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 2106166'
loop_
_audit_author_name
_audit_author_address
'jian zhou'
;Chongqing Normal University
China
;
_audit_update_record             
;
2021-08-29 deposited with the CCDC.	2021-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H42 N2 O18 V4'
_chemical_formula_sum            'C22 H42 N2 O18 V4'
_chemical_formula_weight         826.34

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   8.642(6)
_cell_length_b                   8.842(6)
_cell_length_c                   11.429(8)
_cell_angle_alpha                70.10(2)
_cell_angle_beta                 68.447(19)
_cell_angle_gamma                84.306(18)
_cell_volume                     763.4(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    15976
_cell_measurement_theta_min      3.160
_cell_measurement_theta_max      27.517

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_F_000             424
_exptl_transmission_factor_min   0.702
_exptl_transmission_factor_max   0.905
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.078
_exptl_absorpt_coefficient_mu    1.271
_shelx_estimated_absorpt_T_min   0.673
_shelx_estimated_absorpt_T_max   0.908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15976
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.160
_diffrn_reflns_theta_max         27.517
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3506
_reflns_number_gt                2777
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0304P)²+1.0336P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         3506
_refine_ls_number_parameters     213
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0846
_refine_ls_wR_factor_gt          0.0759
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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 0.31636(5) 0.32187(5) 0.76983(4) 0.01901(11) Uani 1 1 d . . . . .
V2 V 0.42054(5) 0.66916(5) 0.53497(4) 0.01618(11) Uani 1 1 d . . . . .
O1 O 0.66229(19) 0.54539(19) 0.44734(16) 0.0169(3) Uani 1 1 d . . . . .
O2 O 0.43523(19) 0.5334(2) 0.70680(16) 0.0188(4) Uani 1 1 d . . . . .
O3 O 0.9570(3) 0.8204(3) 0.5132(2) 0.0425(6) Uani 1 1 d . . . . .
H3 H 1.036(5) 0.839(5) 0.524(4) 0.064 Uiso 1 1 d . U . . .
O4 O 0.4751(2) 0.7620(2) 0.33692(17) 0.0206(4) Uani 1 1 d . . . . .
O5 O 0.5616(3) 1.0963(3) 0.2357(2) 0.0396(5) Uani 1 1 d . . . . .
H5 H 0.6155 1.1772 0.1800 0.059 Uiso 1 1 calc R U . . .
O6 O 0.2647(2) 0.7805(2) 0.57342(19) 0.0280(4) Uani 1 1 d . . . . .
O7 O 0.1967(2) 0.1439(2) 0.76169(18) 0.0250(4) Uani 1 1 d . . . . .
O8 O 0.0932(2) 0.4226(2) 0.82367(19) 0.0271(4) Uani 1 1 d . . . . .
O9 O 0.3307(2) 0.2512(2) 0.91329(18) 0.0305(4) Uani 1 1 d . . . . .
N1 N 0.6177(2) 0.7900(2) 0.5396(2) 0.0199(4) Uani 1 1 d . . . . .
H1A H 0.6815 0.8485 0.4580 0.024 Uiso 1 1 calc R U . . .
H1B H 0.5789 0.8536 0.5894 0.024 Uiso 1 1 calc R U . . .
C1 C -0.0468(3) 0.3461(3) 0.8867(3) 0.0257(6) Uani 1 1 d . . . . .
C2 C -0.1849(3) 0.4296(4) 0.9651(3) 0.0362(7) Uani 1 1 d . . . . .
H2A H -0.1752 0.5432 0.9180 0.054 Uiso 1 1 calc R U . . .
H2B H -0.1771 0.4100 1.0507 0.054 Uiso 1 1 calc R U . . .
H2C H -0.2903 0.3889 0.9767 0.054 Uiso 1 1 calc R U . . .
C3 C -0.0761(3) 0.1934(4) 0.8867(3) 0.0304(6) Uani 1 1 d . . . . .
H3A H -0.1830 0.1485 0.9354 0.036 Uiso 1 1 calc R U . . .
C4 C 0.0403(3) 0.1039(3) 0.8207(2) 0.0243(5) Uani 1 1 d . . . . .
C5 C -0.0083(4) -0.0482(3) 0.8104(3) 0.0329(6) Uani 1 1 d . . . . .
H5A H -0.0158 -0.0263 0.7244 0.049 Uiso 1 1 calc R U . . .
H5B H -0.1143 -0.0879 0.8784 0.049 Uiso 1 1 calc R U . . .
H5C H 0.0741 -0.1274 0.8217 0.049 Uiso 1 1 calc R U . . .
C6 C 0.5808(3) 0.5527(3) 0.7306(2) 0.0215(5) Uani 1 1 d . . . . .
H6A H 0.6251 0.4483 0.7637 0.026 Uiso 1 1 calc R U . . .
H6B H 0.5540 0.6053 0.7973 0.026 Uiso 1 1 calc R U . . .
C7 C 0.7108(3) 0.6548(3) 0.6003(2) 0.0189(5) Uani 1 1 d . . . . .
C8 C 0.8494(3) 0.7105(3) 0.6300(3) 0.0242(5) Uani 1 1 d . . . . .
H8A H 0.8020 0.7614 0.6980 0.029 Uiso 1 1 calc R U . . .
H8B H 0.9111 0.6186 0.6632 0.029 Uiso 1 1 calc R U . . .
C9 C 0.3792(3) 0.8812(3) 0.2751(3) 0.0284(6) Uani 1 1 d . . . . .
H9A H 0.2886 0.9107 0.3435 0.034 Uiso 1 1 calc R U . . .
H9B H 0.3307 0.8352 0.2300 0.034 Uiso 1 1 calc R U . . .
C10 C 0.4794(4) 1.0297(3) 0.1767(3) 0.0336(6) Uani 1 1 d . . . . .
H10A H 0.5613 1.0033 0.1021 0.040 Uiso 1 1 calc R U . . .
H10B H 0.4067 1.1088 0.1429 0.040 Uiso 1 1 calc R U . . .
C11 C 0.7826(3) 0.5609(3) 0.5019(3) 0.0202(5) Uani 1 1 d . . . . .
H11A H 0.8819 0.6168 0.4305 0.024 Uiso 1 1 calc R U . . .
H11B H 0.8136 0.4549 0.5473 0.024 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 O9 1.591(2) . ?
V1 O2 1.998(2) . ?
V1 O4 2.005(2) 2_666 ?
V1 O7 2.012(2) . ?
V1 O8 2.013(2) . ?
V1 O1 2.301(2) 2_666 ?
V2 O6 1.6036(19) . ?
V2 O2 1.965(2) . ?
V2 O4 2.012(2) . ?
V2 O1 2.014(2) 2_666 ?
V2 N1 2.125(2) . ?
V2 O1 2.307(2) . ?
O1 C11 1.432(3) . ?
O1 V2 2.014(2) 2_666 ?
O1 V1 2.301(2) 2_666 ?
O2 C6 1.418(3) . ?
O3 C8 1.405(3) . ?
O3 H3 0.78(4) . ?
O4 C9 1.431(3) . ?
O4 V1 2.0054(19) 2_666 ?
O5 C10 1.418(4) . ?
O5 H5 0.8200 . ?
O7 C4 1.292(3) . ?
O8 C1 1.277(3) . ?
N1 C7 1.487(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
C1 C3 1.398(4) . ?
C1 C2 1.504(4) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.378(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.501(4) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.533(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.524(3) . ?
C7 C11 1.537(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.498(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?

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
O9 V1 O2 98.68(9) . . ?
O9 V1 O4 100.09(10) . 2_666 ?
O2 V1 O4 89.01(8) . 2_666 ?
O9 V1 O7 103.35(10) . . ?
O2 V1 O7 157.93(8) . . ?
O4 V1 O7 85.86(9) 2_666 . ?
O9 V1 O8 97.60(10) . . ?
O2 V1 O8 91.57(9) . . ?
O4 V1 O8 162.00(8) 2_666 . ?
O7 V1 O8 86.89(9) . . ?
O9 V1 O1 169.21(8) . 2_666 ?
O2 V1 O1 71.32(7) . 2_666 ?
O4 V1 O1 76.21(8) 2_666 2_666 ?
O7 V1 O1 86.62(8) . 2_666 ?
O8 V1 O1 86.94(7) . 2_666 ?
O6 V2 O2 104.51(9) . . ?
O6 V2 O4 95.78(9) . . ?
O2 V2 O4 159.70(7) . . ?
O6 V2 O1 109.22(10) . 2_666 ?
O2 V2 O1 78.52(8) . 2_666 ?
O4 V2 O1 94.98(7) . 2_666 ?
O6 V2 N1 103.05(10) . . ?
O2 V2 N1 79.34(8) . . ?
O4 V2 N1 96.27(8) . . ?
O1 V2 N1 144.45(8) 2_666 . ?
O6 V2 O1 170.35(8) . . ?
O2 V2 O1 83.82(7) . . ?
O4 V2 O1 75.96(7) . . ?
O1 V2 O1 76.90(8) 2_666 . ?
N1 V2 O1 73.36(8) . . ?
C11 O1 V2 122.84(15) . 2_666 ?
C11 O1 V1 124.00(14) . 2_666 ?
V2 O1 V1 97.79(7) 2_666 2_666 ?
C11 O1 V2 110.02(14) . . ?
V2 O1 V2 103.10(8) 2_666 . ?
V1 O1 V2 93.91(7) 2_666 . ?
C6 O2 V2 116.97(14) . . ?
C6 O2 V1 123.61(15) . . ?
V2 O2 V1 110.52(8) . . ?
C8 O3 H3 110(3) . . ?
C9 O4 V1 121.99(16) . 2_666 ?
C9 O4 V2 124.07(15) . . ?
V1 O4 V2 113.91(9) 2_666 . ?
C10 O5 H5 109.5 . . ?
C4 O7 V1 127.40(17) . . ?
C1 O8 V1 125.43(18) . . ?
C7 N1 V2 102.69(15) . . ?
C7 N1 H1A 111.2 . . ?
V2 N1 H1A 111.2 . . ?
C7 N1 H1B 111.2 . . ?
V2 N1 H1B 111.2 . . ?
H1A N1 H1B 109.1 . . ?
O8 C1 C3 124.1(2) . . ?
O8 C1 C2 116.0(3) . . ?
C3 C1 C2 119.9(2) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C1 125.4(2) . . ?
C4 C3 H3A 117.3 . . ?
C1 C3 H3A 117.3 . . ?
O7 C4 C3 123.6(2) . . ?
O7 C4 C5 115.0(2) . . ?
C3 C4 C5 121.5(2) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O2 C6 C7 109.2(2) . . ?
O2 C6 H6A 109.8 . . ?
C7 C6 H6A 109.8 . . ?
O2 C6 H6B 109.8 . . ?
C7 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
N1 C7 C8 113.2(2) . . ?
N1 C7 C6 105.37(19) . . ?
C8 C7 C6 109.7(2) . . ?
N1 C7 C11 106.8(2) . . ?
C8 C7 C11 110.4(2) . . ?
C6 C7 C11 111.3(2) . . ?
O3 C8 C7 109.6(2) . . ?
O3 C8 H8A 109.8 . . ?
C7 C8 H8A 109.8 . . ?
O3 C8 H8B 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
O4 C9 C10 113.1(2) . . ?
O4 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
O4 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
O5 C10 C9 111.3(2) . . ?
O5 C10 H10A 109.4 . . ?
C9 C10 H10A 109.4 . . ?
O5 C10 H10B 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
O1 C11 C7 110.27(18) . . ?
O1 C11 H11A 109.6 . . ?
C7 C11 H11A 109.6 . . ?
O1 C11 H11B 109.6 . . ?
C7 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?

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 O8 C1 C3 -24.2(4) . . . . ?
V1 O8 C1 C2 155.39(19) . . . . ?
O8 C1 C3 C4 0.5(5) . . . . ?
C2 C1 C3 C4 -179.0(3) . . . . ?
V1 O7 C4 C3 9.0(4) . . . . ?
V1 O7 C4 C5 -172.14(17) . . . . ?
C1 C3 C4 O7 7.7(5) . . . . ?
C1 C3 C4 C5 -171.1(3) . . . . ?
V2 O2 C6 C7 -11.6(2) . . . . ?
V1 O2 C6 C7 132.54(17) . . . . ?
V2 N1 C7 C8 -173.27(16) . . . . ?
V2 N1 C7 C6 -53.46(19) . . . . ?
V2 N1 C7 C11 65.04(18) . . . . ?
O2 C6 C7 N1 44.3(2) . . . . ?
O2 C6 C7 C8 166.4(2) . . . . ?
O2 C6 C7 C11 -71.1(2) . . . . ?
N1 C7 C8 O3 -55.2(3) . . . . ?
C6 C7 C8 O3 -172.6(2) . . . . ?
C11 C7 C8 O3 64.4(3) . . . . ?
V1 O4 C9 C10 -54.5(3) 2_666 . . . ?
V2 O4 C9 C10 123.3(2) . . . . ?
O4 C9 C10 O5 -55.0(3) . . . . ?
V2 O1 C11 C7 -121.54(18) 2_666 . . . ?
V1 O1 C11 C7 109.41(19) 2_666 . . . ?
V2 O1 C11 C7 -0.1(2) . . . . ?
N1 C7 C11 O1 -41.5(2) . . . . ?
C8 C7 C11 O1 -164.9(2) . . . . ?
C6 C7 C11 O1 73.0(3) . . . . ?

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
O3 H3 O6 0.78(4) 2.21(4) 2.943(3) 156(4) 1_655
N1 H1A O7 0.89 2.32 3.087(3) 144.7 2_666
N1 H1B O5 0.89 2.09 2.921(3) 154.4 2_676
C5 H5A O3 0.96 2.60 3.440(4) 146.4 2_666
C5 H5B O9 0.96 2.48 3.410(4) 161.8 2_557
C9 H9A O6 0.97 2.42 3.004(4) 118.3 .
C10 H10A O9 0.97 2.39 3.100(4) 129.9 2_666

_refine_diff_density_max         0.640
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.081

####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 2106170'
loop_
_audit_author_name
_audit_author_address
'jian zhou'
;Chongqing Normal University
China
;
_audit_update_record             
;
2021-08-29 deposited with the CCDC.	2021-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N3 O19 V6, 6(H2 O)'
_chemical_formula_sum            'C12 H41 N3 O25 V6'
_chemical_formula_weight         933.11

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'

_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                   17.0549(9)
_cell_length_b                   15.2858(8)
_cell_length_c                   12.0572(6)
_cell_angle_alpha                90
_cell_angle_beta                 99.7222(18)
_cell_angle_gamma                90
_cell_volume                     3098.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    23309
_cell_measurement_theta_min      2.3407
_cell_measurement_theta_max      28.2297

_exptl_crystal_description       flake
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.000
_exptl_crystal_F_000             1832
_exptl_transmission_factor_min   0.581
_exptl_transmission_factor_max   0.940
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.033
_exptl_absorpt_coefficient_mu    1.837
_shelx_estimated_absorpt_T_min   0.482
_shelx_estimated_absorpt_T_max   0.912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31788
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_av_R_equivalents  0.0791
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.766
_diffrn_reflns_theta_max         28.284
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7655
_reflns_number_gt                5892
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0630P)²+5.3029P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7655
_refine_ls_number_parameters     382
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0574
_refine_ls_wR_factor_ref         0.1744
_refine_ls_wR_factor_gt          0.1627
_refine_ls_goodness_of_fit_ref   1.270
_refine_ls_restrained_S_all      1.270
_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 0.37295(4) 0.37048(4) 0.58635(6) 0.01593(17) Uani 1 1 d . . . . .
V2 V 0.44186(4) 0.56610(4) 0.65894(6) 0.01608(17) Uani 1 1 d . . . . .
V3 V 0.26239(4) 0.63702(4) 0.66236(6) 0.01619(17) Uani 1 1 d . . . . .
V4 V 0.32966(4) 0.46558(4) 0.81150(6) 0.01622(17) Uani 1 1 d . . . . .
V5 V 0.30486(4) 0.54399(4) 0.43464(6) 0.01605(17) Uani 1 1 d . . . . .
V6 V 0.19412(4) 0.44435(4) 0.58942(6) 0.01643(17) Uani 1 1 d . . . . .
O1 O 0.19978(16) 0.48486(18) 0.4335(2) 0.0179(6) Uani 1 1 d . . . . .
O2 O 0.25899(17) 0.65029(18) 0.4960(2) 0.0180(6) Uani 1 1 d . . . . .
O3 O 0.16272(17) 0.56528(18) 0.6268(2) 0.0196(6) Uani 1 1 d . . . . .
O4 O 0.37285(17) 0.35657(18) 0.7508(2) 0.0182(6) Uani 1 1 d . . . . .
O5 O 0.22078(17) 0.41795(18) 0.7548(2) 0.0182(6) Uani 1 1 d . . . . .
O6 O 0.25747(17) 0.33755(17) 0.5616(2) 0.0177(6) Uani 1 1 d . . . . .
O7 O 0.28158(17) 0.58477(18) 0.8181(2) 0.0176(6) Uani 1 1 d . . . . .
O8 O 0.43516(17) 0.52487(18) 0.8149(2) 0.0174(6) Uani 1 1 d . . . . .
O9 O 0.37776(16) 0.67100(18) 0.6890(2) 0.0168(6) Uani 1 1 d . . . . .
O10 O 0.41240(19) 0.2795(2) 0.5583(3) 0.0270(7) Uani 1 1 d . . . . .
O11 O 0.2237(2) 0.7294(2) 0.6866(3) 0.0282(7) Uani 1 1 d . . . . .
O12 O 0.2985(2) 0.5710(2) 0.3043(3) 0.0287(7) Uani 1 1 d . . . . .
O13 O 0.3374(2) 0.4391(2) 0.9421(3) 0.0274(7) Uani 1 1 d . . . . .
O14 O 0.10697(18) 0.4003(2) 0.5654(3) 0.0267(7) Uani 1 1 d . . . . .
O15 O 0.52927(19) 0.6088(2) 0.6836(3) 0.0266(7) Uani 1 1 d . . . . .
O16 O 0.41182(17) 0.59305(18) 0.4965(2) 0.0190(6) Uani 1 1 d . . . . .
O17 O 0.31518(15) 0.50417(17) 0.6266(2) 0.0160(6) Uani 1 1 d . . . . .
O18 O 0.34960(17) 0.42284(18) 0.4325(2) 0.0183(6) Uani 1 1 d . . . . .
O19 O 0.47021(17) 0.44347(18) 0.6262(2) 0.0191(6) Uani 1 1 d . . . . .
C1 C 0.1160(3) 0.6174(3) 0.4340(4) 0.0267(10) Uani 1 1 d . . . . .
C2 C 0.1850(3) 0.6811(3) 0.4329(4) 0.0256(9) Uani 1 1 d . . . . .
H2A H 0.1917 0.6911 0.3556 0.031 Uiso 1 1 calc R U . . .
H2B H 0.1717 0.7366 0.4639 0.031 Uiso 1 1 calc R U . . .
C3 C 0.1314(3) 0.5307(3) 0.3772(4) 0.0277(10) Uani 1 1 d . . . . .
H3A H 0.0851 0.4934 0.3744 0.033 Uiso 1 1 calc R U . . .
H3B H 0.1383 0.5424 0.3004 0.033 Uiso 1 1 calc R U . . .
C4 C 0.0984(3) 0.6037(3) 0.5526(4) 0.0280(10) Uani 1 1 d . . . . .
H4A H 0.0857 0.6597 0.5830 0.034 Uiso 1 1 calc R U . . .
H4B H 0.0520 0.5664 0.5488 0.034 Uiso 1 1 calc R U . . .
C5 C 0.2549(3) 0.2628(3) 0.7417(4) 0.0213(9) Uani 1 1 d . . . . .
C6 C 0.2383(3) 0.2587(3) 0.6123(4) 0.0231(9) Uani 1 1 d . . . . .
H6A H 0.2690 0.2114 0.5875 0.028 Uiso 1 1 calc R U . . .
H6B H 0.1824 0.2458 0.5873 0.028 Uiso 1 1 calc R U . . .
C7 C 0.3439(3) 0.2757(3) 0.7866(4) 0.0211(9) Uani 1 1 d . . . . .
H7A H 0.3527 0.2740 0.8682 0.025 Uiso 1 1 calc R U . . .
H7B H 0.3736 0.2280 0.7607 0.025 Uiso 1 1 calc R U . . .
C8 C 0.2038(3) 0.3319(3) 0.7877(4) 0.0233(9) Uani 1 1 d . . . . .
H8A H 0.1481 0.3192 0.7610 0.028 Uiso 1 1 calc R U . . .
H8B H 0.2128 0.3285 0.8692 0.028 Uiso 1 1 calc R U . . .
C9 C 0.4031(3) 0.6658(3) 0.8953(3) 0.0201(8) Uani 1 1 d . . . . .
C10 C 0.4058(3) 0.7193(3) 0.7894(3) 0.0218(9) Uani 1 1 d . . . . .
H10A H 0.3734 0.7713 0.7908 0.026 Uiso 1 1 calc R U . . .
H10B H 0.4601 0.7380 0.7888 0.026 Uiso 1 1 calc R U . . .
C11 C 0.4590(3) 0.5861(3) 0.9037(3) 0.0219(9) Uani 1 1 d . . . . .
H11A H 0.5127 0.6058 0.9010 0.026 Uiso 1 1 calc R U . . .
H11B H 0.4594 0.5572 0.9755 0.026 Uiso 1 1 calc R U . . .
C12 C 0.3178(3) 0.6407(3) 0.9072(4) 0.0232(9) Uani 1 1 d . . . . .
H12A H 0.3185 0.6113 0.9786 0.028 Uiso 1 1 calc R U . . .
H12B H 0.2862 0.6935 0.9073 0.028 Uiso 1 1 calc R U . . .
N3 N 0.4350(2) 0.7226(2) 0.9940(3) 0.0256(8) Uani 1 1 d . . . . .
H3C H 0.4846 0.7384 0.9898 0.031 Uiso 1 1 calc R U . . .
H3D H 0.4345 0.6930 1.0575 0.031 Uiso 1 1 calc R U . . .
H3E H 0.4047 0.7701 0.9933 0.031 Uiso 1 1 calc R U . . .
N1 N 0.0451(3) 0.6588(3) 0.3660(4) 0.0374(10) Uani 1 1 d . . . . .
H1A H 0.0485 0.6548 0.2933 0.045 Uiso 1 1 calc R U . . .
H1B H 0.0429 0.7148 0.3852 0.045 Uiso 1 1 calc R U . . .
H1C H 0.0014 0.6314 0.3787 0.045 Uiso 1 1 calc R U . . .
N2 N 0.2324(2) 0.1751(2) 0.7844(3) 0.0281(9) Uani 1 1 d . . . . .
H2C H 0.2335 0.1348 0.7315 0.034 Uiso 1 1 calc R U . . .
H2D H 0.1836 0.1782 0.8012 0.034 Uiso 1 1 calc R U . . .
H2E H 0.2667 0.1607 0.8457 0.034 Uiso 1 1 calc R U . . .
O1W O 0.57881(17) 0.4065(2) 0.8287(3) 0.0506(11) Uani 1 1 d G . . . .
O2W O 0.0811(2) 0.1969(3) 0.8625(3) 0.0825(16) Uiso 1 1 d G . . . .
O3W O 0.2410(3) 0.04718(19) 0.6121(3) 0.123(3) Uiso 1 1 d G . . . .
O4W O 0.1528(3) 0.6100(3) 0.0926(3) 0.124(3) Uiso 1 1 d G . . . .
O5W O 0.1074(2) 0.5279(3) 0.8603(3) 0.170(4) Uiso 1 1 d G . . . .
O6W O 0.0026(3) 0.8411(3) 0.3490(5) 0.093(4) Uiso 0.5 1 d G . P . .
O7W O -0.0203(3) 0.6333(4) 0.1006(4) 0.117(5) Uiso 0.5 1 d G . P . .


_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 O10 1.606(3) . ?
V1 O19 1.990(3) . ?
V1 O4 1.995(3) . ?
V1 O18 1.997(3) . ?
V1 O6 2.006(3) . ?
V1 O17 2.355(3) . ?
V2 O15 1.608(3) . ?
V2 O16 1.982(3) . ?
V2 O19 1.992(3) . ?
V2 O8 2.005(3) . ?
V2 O9 2.008(3) . ?
V2 O17 2.331(3) . ?
V3 O11 1.607(3) . ?
V3 O2 2.007(3) . ?
V3 O3 2.007(3) . ?
V3 O9 2.008(3) . ?
V3 O7 2.016(3) . ?
V3 O17 2.292(3) . ?
V4 O13 1.610(3) . ?
V4 O5 2.004(3) . ?
V4 O7 2.005(3) . ?
V4 O8 2.009(3) . ?
V4 O4 2.009(3) . ?
V4 O17 2.279(3) . ?
V5 O12 1.610(3) . ?
V5 O16 1.997(3) . ?
V5 O2 1.999(3) . ?
V5 O18 2.005(3) . ?
V5 O1 2.005(3) . ?
V5 O17 2.371(3) . ?
V6 O14 1.613(3) . ?
V6 O3 1.997(3) . ?
V6 O1 1.997(3) . ?
V6 O5 2.010(3) . ?
V6 O6 2.017(3) . ?
V6 O17 2.233(3) . ?
O1 C3 1.429(5) . ?
O2 C2 1.439(5) . ?
O3 C4 1.421(5) . ?
O4 C7 1.425(5) . ?
O5 C8 1.418(5) . ?
O6 C6 1.414(5) . ?
O7 C12 1.429(5) . ?
O8 C11 1.428(5) . ?
O9 C10 1.430(5) . ?
C1 N1 1.482(6) . ?
C1 C4 1.525(7) . ?
C1 C2 1.528(6) . ?
C1 C3 1.535(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.509(5) . ?
C5 C8 1.532(6) . ?
C5 C7 1.535(6) . ?
C5 C6 1.539(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N3 1.499(5) . ?
C9 C10 1.523(6) . ?
C9 C12 1.535(6) . ?
C9 C11 1.539(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N3 H3E 0.8900 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?

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
O10 V1 O19 100.06(15) . . ?
O10 V1 O4 100.82(14) . . ?
O19 V1 O4 87.71(12) . . ?
O10 V1 O18 100.17(14) . . ?
O19 V1 O18 91.55(12) . . ?
O4 V1 O18 158.80(12) . . ?
O10 V1 O6 100.80(15) . . ?
O19 V1 O6 159.12(12) . . ?
O4 V1 O6 87.44(12) . . ?
O18 V1 O6 85.75(12) . . ?
O10 V1 O17 179.73(15) . . ?
O19 V1 O17 79.88(10) . . ?
O4 V1 O17 79.45(10) . . ?
O18 V1 O17 79.57(10) . . ?
O6 V1 O17 79.27(10) . . ?
O15 V2 O16 100.11(14) . . ?
O15 V2 O19 99.77(15) . . ?
O16 V2 O19 91.76(12) . . ?
O15 V2 O8 98.73(14) . . ?
O16 V2 O8 161.08(12) . . ?
O19 V2 O8 86.80(12) . . ?
O15 V2 O9 99.14(15) . . ?
O16 V2 O9 87.41(12) . . ?
O19 V2 O9 160.92(12) . . ?
O8 V2 O9 87.85(11) . . ?
O15 V2 O17 178.98(13) . . ?
O16 V2 O17 80.88(11) . . ?
O19 V2 O17 80.43(11) . . ?
O8 V2 O17 80.28(10) . . ?
O9 V2 O17 80.62(10) . . ?
O11 V3 O2 98.62(15) . . ?
O11 V3 O3 99.21(15) . . ?
O2 V3 O3 87.78(12) . . ?
O11 V3 O9 99.50(15) . . ?
O2 V3 O9 89.78(12) . . ?
O3 V3 O9 161.29(12) . . ?
O11 V3 O7 100.69(14) . . ?
O2 V3 O7 160.69(12) . . ?
O3 V3 O7 88.91(12) . . ?
O9 V3 O7 87.29(12) . . ?
O11 V3 O17 178.90(14) . . ?
O2 V3 O17 81.23(10) . . ?
O3 V3 O17 79.70(11) . . ?
O9 V3 O17 81.59(10) . . ?
O7 V3 O17 79.46(10) . . ?
O13 V4 O5 99.25(15) . . ?
O13 V4 O7 98.99(14) . . ?
O5 V4 O7 88.97(12) . . ?
O13 V4 O8 99.67(15) . . ?
O5 V4 O8 161.08(12) . . ?
O7 V4 O8 87.72(12) . . ?
O13 V4 O4 99.96(14) . . ?
O5 V4 O4 87.14(12) . . ?
O7 V4 O4 161.03(12) . . ?
O8 V4 O4 89.97(11) . . ?
O13 V4 O17 178.46(14) . . ?
O5 V4 O17 79.59(11) . . ?
O7 V4 O17 79.99(10) . . ?
O8 V4 O17 81.48(10) . . ?
O4 V4 O17 81.04(10) . . ?
O12 V5 O16 100.06(15) . . ?
O12 V5 O2 100.77(15) . . ?
O16 V5 O2 86.93(12) . . ?
O12 V5 O18 100.79(15) . . ?
O16 V5 O18 91.49(12) . . ?
O2 V5 O18 158.32(12) . . ?
O12 V5 O1 101.32(15) . . ?
O16 V5 O1 158.59(12) . . ?
O2 V5 O1 87.92(12) . . ?
O18 V5 O1 85.71(12) . . ?
O12 V5 O17 179.59(14) . . ?
O16 V5 O17 79.58(10) . . ?
O2 V5 O17 79.43(10) . . ?
O18 V5 O17 79.02(10) . . ?
O1 V5 O17 79.04(10) . . ?
O14 V6 O3 98.78(15) . . ?
O14 V6 O1 98.62(14) . . ?
O3 V6 O1 89.02(12) . . ?
O14 V6 O5 98.14(14) . . ?
O3 V6 O5 89.21(12) . . ?
O1 V6 O5 163.22(12) . . ?
O14 V6 O6 97.81(14) . . ?
O3 V6 O6 163.41(12) . . ?
O1 V6 O6 88.98(12) . . ?
O5 V6 O6 87.97(12) . . ?
O14 V6 O17 178.72(14) . . ?
O3 V6 O17 81.36(11) . . ?
O1 V6 O17 82.65(11) . . ?
O5 V6 O17 80.59(11) . . ?
O6 V6 O17 82.05(11) . . ?
C3 O1 V6 115.7(3) . . ?
C3 O1 V5 116.0(2) . . ?
V6 O1 V5 108.57(13) . . ?
C2 O2 V5 115.7(3) . . ?
C2 O2 V3 115.8(3) . . ?
V5 O2 V3 109.92(13) . . ?
C4 O3 V6 116.6(3) . . ?
C4 O3 V3 116.4(3) . . ?
V6 O3 V3 107.71(13) . . ?
C7 O4 V1 116.9(2) . . ?
C7 O4 V4 116.3(2) . . ?
V1 O4 V4 109.60(13) . . ?
C8 O5 V4 117.6(2) . . ?
C8 O5 V6 116.2(2) . . ?
V4 O5 V6 107.86(13) . . ?
C6 O6 V1 116.3(2) . . ?
C6 O6 V6 116.6(3) . . ?
V1 O6 V6 108.20(13) . . ?
C12 O7 V4 116.5(2) . . ?
C12 O7 V3 116.4(2) . . ?
V4 O7 V3 109.03(13) . . ?
C11 O8 V2 116.3(2) . . ?
C11 O8 V4 116.8(2) . . ?
V2 O8 V4 108.39(13) . . ?
C10 O9 V3 116.6(2) . . ?
C10 O9 V2 116.8(2) . . ?
V3 O9 V2 108.25(13) . . ?
V2 O16 V5 111.01(13) . . ?
V6 O17 V4 91.96(10) . . ?
V6 O17 V3 91.22(10) . . ?
V4 O17 V3 91.52(9) . . ?
V6 O17 V2 178.04(13) . . ?
V4 O17 V2 89.84(9) . . ?
V3 O17 V2 89.50(9) . . ?
V6 O17 V1 90.46(9) . . ?
V4 O17 V1 89.83(9) . . ?
V3 O17 V1 177.81(13) . . ?
V2 O17 V1 88.78(9) . . ?
V6 O17 V5 89.73(9) . . ?
V4 O17 V5 178.06(13) . . ?
V3 O17 V5 89.39(9) . . ?
V2 O17 V5 88.45(9) . . ?
V1 O17 V5 89.21(9) . . ?
V1 O18 V5 112.03(13) . . ?
V1 O19 V2 110.81(14) . . ?
N1 C1 C4 107.8(4) . . ?
N1 C1 C2 106.3(4) . . ?
C4 C1 C2 111.7(4) . . ?
N1 C1 C3 107.9(4) . . ?
C4 C1 C3 112.0(4) . . ?
C2 C1 C3 110.9(4) . . ?
O2 C2 C1 113.3(3) . . ?
O2 C2 H2A 108.9 . . ?
C1 C2 H2A 108.9 . . ?
O2 C2 H2B 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
O1 C3 C1 113.5(4) . . ?
O1 C3 H3A 108.9 . . ?
C1 C3 H3A 108.9 . . ?
O1 C3 H3B 108.9 . . ?
C1 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
O3 C4 C1 113.2(4) . . ?
O3 C4 H4A 108.9 . . ?
C1 C4 H4A 108.9 . . ?
O3 C4 H4B 108.9 . . ?
C1 C4 H4B 108.9 . . ?
H4A C4 H4B 107.8 . . ?
N2 C5 C8 107.1(3) . . ?
N2 C5 C7 106.7(3) . . ?
C8 C5 C7 111.9(4) . . ?
N2 C5 C6 107.2(3) . . ?
C8 C5 C6 112.1(3) . . ?
C7 C5 C6 111.4(4) . . ?
O6 C6 C5 112.8(3) . . ?
O6 C6 H6A 109.0 . . ?
C5 C6 H6A 109.0 . . ?
O6 C6 H6B 109.0 . . ?
C5 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
O4 C7 C5 112.1(3) . . ?
O4 C7 H7A 109.2 . . ?
C5 C7 H7A 109.2 . . ?
O4 C7 H7B 109.2 . . ?
C5 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
O5 C8 C5 112.4(3) . . ?
O5 C8 H8A 109.1 . . ?
C5 C8 H8A 109.1 . . ?
O5 C8 H8B 109.1 . . ?
C5 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
N3 C9 C10 107.2(3) . . ?
N3 C9 C12 107.0(3) . . ?
C10 C9 C12 112.0(4) . . ?
N3 C9 C11 105.6(3) . . ?
C10 C9 C11 112.0(3) . . ?
C12 C9 C11 112.5(3) . . ?
O9 C10 C9 112.2(3) . . ?
O9 C10 H10A 109.2 . . ?
C9 C10 H10A 109.2 . . ?
O9 C10 H10B 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
O8 C11 C9 112.0(3) . . ?
O8 C11 H11A 109.2 . . ?
C9 C11 H11A 109.2 . . ?
O8 C11 H11B 109.2 . . ?
C9 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
O7 C12 C9 112.1(3) . . ?
O7 C12 H12A 109.2 . . ?
C9 C12 H12A 109.2 . . ?
O7 C12 H12B 109.2 . . ?
C9 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
C9 N3 H3C 109.5 . . ?
C9 N3 H3D 109.5 . . ?
H3C N3 H3D 109.5 . . ?
C9 N3 H3E 109.5 . . ?
H3C N3 H3E 109.5 . . ?
H3D N3 H3E 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C5 N2 H2C 109.5 . . ?
C5 N2 H2D 109.5 . . ?
H2C N2 H2D 109.5 . . ?
C5 N2 H2E 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?

_refine_diff_density_max         1.842
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.150

####################################################################### 
# 
# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 2106168'
loop_
_audit_author_name
_audit_author_address
'jian zhou'
;Chongqing Normal University
China
;
_audit_update_record             
;
2021-08-29 deposited with the CCDC.	2021-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H42 N2 O16 V4'
_chemical_formula_sum            'C22 H42 N2 O16 V4'
_chemical_formula_weight         794.34

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   8.143(8)
_cell_length_b                   10.003(10)
_cell_length_c                   22.33(2)
_cell_angle_alpha                90.53(5)
_cell_angle_beta                 92.55(4)
_cell_angle_gamma                113.36(3)
_cell_volume                     1667(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    29200
_cell_measurement_theta_min      2.219
_cell_measurement_theta_max      25.099

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   0.823
_exptl_transmission_factor_max   0.951
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.043
_exptl_absorpt_coefficient_mu    1.156
_shelx_estimated_absorpt_T_min   0.831
_shelx_estimated_absorpt_T_max   0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35599
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_av_R_equivalents  0.0892
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.219
_diffrn_reflns_theta_max         27.929
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7939
_reflns_number_gt                6017
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0347P)²+6.9132P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7939
_refine_ls_number_parameters     424
_refine_ls_number_restraints     146
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0691
_refine_ls_wR_factor_ref         0.1689
_refine_ls_wR_factor_gt          0.1578
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.112
_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 0.67911(10) 0.45482(8) 0.49855(3) 0.02180(18) Uani 1 1 d . . . . .
V2 V 0.34573(10) 0.34252(9) 0.39145(3) 0.02635(19) Uani 1 1 d . . . . .
V3 V 0.31655(10) 1.03991(8) 0.00003(3) 0.02217(18) Uani 1 1 d . . . . .
V4 V 0.36999(11) 0.83192(9) 0.10183(4) 0.0285(2) Uani 1 1 d . . . . .
O1 O 0.5094(4) 0.5536(3) 0.44448(13) 0.0206(6) Uani 1 1 d . . . . .
O2 O 0.7864(4) 0.6502(3) 0.53610(13) 0.0258(7) Uani 1 1 d . . . . .
O3 O 0.9116(6) 0.9496(4) 0.3935(2) 0.0530(11) Uani 1 1 d . . . . .
H3 H 1.0025 1.0198 0.3857 0.079 Uiso 1 1 calc R U . . .
O4 O 0.7922(5) 0.3708(4) 0.52820(16) 0.0351(8) Uani 1 1 d . . . . .
O5 O 0.5191(5) 0.2930(4) 0.44241(15) 0.0328(7) Uani 1 1 d D U . . .
O6 O 0.2183(5) 0.1843(4) 0.36458(16) 0.0454(10) Uani 1 1 d . . . . .
O7 O 0.2296(5) 0.4639(4) 0.35173(15) 0.0396(9) Uani 1 1 d . . . . .
O8 O 0.5276(5) 0.4088(4) 0.32836(16) 0.0377(8) Uani 1 1 d . . . . .
O10 O 0.4809(4) 0.9507(3) -0.05712(13) 0.0219(6) Uani 1 1 d . . . . .
O9 O 0.2208(4) 0.8403(3) 0.02969(14) 0.0271(7) Uani 1 1 d . . . . .
O11 O 0.0754(6) 0.5569(5) -0.1282(2) 0.0690(14) Uani 1 1 d . U . . .
H11D H -0.0189 0.4849 -0.1268 0.104 Uiso 1 1 calc R U . . .
O12 O 0.2557(6) 0.6711(4) 0.12281(18) 0.0494(10) Uani 1 1 d . . . . .
O13 O 0.2529(5) 0.9440(4) 0.14494(15) 0.0395(9) Uani 1 1 d . . . . .
O14 O 0.5645(5) 0.9006(4) 0.16719(16) 0.0417(9) Uani 1 1 d . . . . .
O15 O 0.2068(5) 1.1196(4) 0.03295(16) 0.0344(8) Uani 1 1 d . . . . .
O16 O 0.4635(5) 1.2080(4) -0.04877(16) 0.0334(8) Uani 1 1 d D U . . .
N1 N 0.8358(5) 0.5715(4) 0.42797(17) 0.0260(8) Uani 1 1 d . . . . .
H1A H 0.9491 0.5815 0.4334 0.031 Uiso 1 1 calc R U . . .
H1B H 0.7917 0.5273 0.3926 0.031 Uiso 1 1 calc R U . . .
N2 N 0.1488(5) 0.9270(4) -0.07540(17) 0.0275(8) Uani 1 1 d . . . . .
H2A H 0.0356 0.9143 -0.0708 0.033 Uiso 1 1 calc R U . . .
H2B H 0.1857 0.9745 -0.1090 0.033 Uiso 1 1 calc R U . . .
C1 C 0.9430(7) 0.8230(5) 0.3894(2) 0.0327(11) Uani 1 1 d . . . . .
H1C H 1.0676 0.8437 0.4002 0.039 Uiso 1 1 calc R U . . .
H1D H 0.9163 0.7829 0.3487 0.039 Uiso 1 1 calc R U . . .
C2 C 0.8209(6) 0.7144(5) 0.4326(2) 0.0239(9) Uani 1 1 d . . . . .
C3 C 0.8760(6) 0.7670(5) 0.4979(2) 0.0279(10) Uani 1 1 d . . . . .
H3A H 1.0046 0.7991 0.5046 0.033 Uiso 1 1 calc R U . . .
H3B H 0.8441 0.8485 0.5066 0.033 Uiso 1 1 calc R U . . .
C4 C 0.6239(6) 0.6864(5) 0.4186(2) 0.0239(9) Uani 1 1 d . . . . .
H4A H 0.5995 0.7668 0.4344 0.029 Uiso 1 1 calc R U . . .
H4B H 0.5999 0.6802 0.3755 0.029 Uiso 1 1 calc R U . . .
C5 C 0.512(3) 0.050(2) 0.4330(11) 0.080(3) Uani 0.344(10) 1 d D U P A 1
H5A H 0.4073 0.0017 0.4068 0.121 Uiso 0.344(10) 1 calc R U P A 1
H5B H 0.4765 0.0465 0.4736 0.121 Uiso 0.344(10) 1 calc R U P A 1
H5C H 0.5916 0.0008 0.4298 0.121 Uiso 0.344(10) 1 calc R U P A 1
C6 C 0.605(3) 0.2051(18) 0.4156(11) 0.057(2) Uani 0.344(10) 1 d D U P A 1
H6A H 0.7298 0.2420 0.4293 0.069 Uiso 0.344(10) 1 calc R U P A 1
H6B H 0.5983 0.2111 0.3723 0.069 Uiso 0.344(10) 1 calc R U P A 1
C5' C 0.7122(17) 0.1989(13) 0.3936(6) 0.080(3) Uani 0.656(10) 1 d D U P A 2
H5'A H 0.6807 0.2214 0.3541 0.121 Uiso 0.656(10) 1 calc R U P A 2
H5'B H 0.7441 0.1164 0.3911 0.121 Uiso 0.656(10) 1 calc R U P A 2
H5'C H 0.8121 0.2813 0.4107 0.121 Uiso 0.656(10) 1 calc R U P A 2
C6' C 0.5547(16) 0.1639(9) 0.4325(6) 0.057(2) Uani 0.656(10) 1 d D U P A 2
H6'A H 0.4499 0.0877 0.4131 0.069 Uiso 0.656(10) 1 calc R U P A 2
H6'B H 0.5803 0.1287 0.4706 0.069 Uiso 0.656(10) 1 calc R U P A 2
C7 C 0.1321(11) 0.5919(10) 0.2806(3) 0.077(2) Uani 1 1 d . . . . .
H7A H 0.0102 0.5229 0.2750 0.116 Uiso 1 1 calc R U . . .
H7B H 0.1716 0.6393 0.2436 0.116 Uiso 1 1 calc R U . . .
H7C H 0.1398 0.6632 0.3109 0.116 Uiso 1 1 calc R U . . .
C8 C 0.2477(8) 0.5148(7) 0.2998(2) 0.0423(13) Uani 1 1 d . . . . .
C9 C 0.3727(9) 0.5029(8) 0.2602(2) 0.0526(16) Uani 1 1 d . . . . .
H9 H 0.3665 0.5312 0.2208 0.063 Uiso 1 1 calc R U . . .
C10 C 0.5023(8) 0.4525(7) 0.2759(2) 0.0430(13) Uani 1 1 d . . . . .
C11 C 0.6339(11) 0.4483(11) 0.2311(3) 0.083(3) Uani 1 1 d . . . . .
H11A H 0.7461 0.5299 0.2387 0.125 Uiso 1 1 calc R U . . .
H11B H 0.5874 0.4531 0.1912 0.125 Uiso 1 1 calc R U . . .
H11C H 0.6517 0.3594 0.2348 0.125 Uiso 1 1 calc R U . . .
C12 C 0.0417(7) 0.6799(6) -0.1246(2) 0.0367(12) Uani 1 1 d . U . . .
H12A H -0.0817 0.6544 -0.1147 0.044 Uiso 1 1 calc R U . . .
H12B H 0.0591 0.7265 -0.1630 0.044 Uiso 1 1 calc R U . . .
C13 C 0.1683(6) 0.7857(5) -0.0762(2) 0.0264(9) Uani 1 1 d . U . . .
C14 C 0.1249(6) 0.7265(5) -0.0135(2) 0.0314(11) Uani 1 1 d . . . . .
H14A H -0.0028 0.6926 -0.0085 0.038 Uiso 1 1 calc R U . . .
H14B H 0.1596 0.6450 -0.0079 0.038 Uiso 1 1 calc R U . . .
C15 C 0.3649(6) 0.8184(5) -0.0883(2) 0.0251(9) Uani 1 1 d . . . . .
H15A H 0.3948 0.7384 -0.0750 0.030 Uiso 1 1 calc R U . . .
H15B H 0.3816 0.8282 -0.1310 0.030 Uiso 1 1 calc R U . . .
C16 C 0.6950(12) 0.9480(13) 0.2658(3) 0.099(3) Uani 1 1 d . . . . .
H16A H 0.7314 0.8701 0.2568 0.149 Uiso 1 1 calc R U . . .
H16B H 0.6515 0.9377 0.3055 0.149 Uiso 1 1 calc R U . . .
H16C H 0.7954 1.0396 0.2636 0.149 Uiso 1 1 calc R U . . .
C17 C 0.5474(9) 0.9427(8) 0.2208(2) 0.0528(16) Uani 1 1 d . . . . .
C18 C 0.4203(9) 0.9906(9) 0.2368(3) 0.0614(19) Uani 1 1 d . . . . .
H18 H 0.4255 1.0230 0.2763 0.074 Uiso 1 1 calc R U . . .
C19 C 0.2821(8) 0.9945(8) 0.1981(2) 0.0489(15) Uani 1 1 d . . . . .
C20 C 0.1609(12) 1.0651(12) 0.2180(4) 0.093(3) Uani 1 1 d . . . . .
H20A H 0.1813 1.1509 0.1954 0.140 Uiso 1 1 calc R U . . .
H20B H 0.1856 1.0915 0.2599 0.140 Uiso 1 1 calc R U . . .
H20C H 0.0383 0.9980 0.2115 0.140 Uiso 1 1 calc R U . . .
C21 C 0.320(4) 1.355(3) -0.0861(12) 0.061(2) Uani 0.303(18) 1 d D U P B 1
H21A H 0.3118 1.4484 -0.0830 0.091 Uiso 0.303(18) 1 calc R U P B 1
H21B H 0.3512 1.3407 -0.1258 0.091 Uiso 0.303(18) 1 calc R U P B 1
H21C H 0.2060 1.2798 -0.0781 0.091 Uiso 0.303(18) 1 calc R U P B 1
C22 C 0.460(4) 1.3508(16) -0.0414(13) 0.049(4) Uani 0.303(18) 1 d D U P B 1
H22A H 0.5756 1.4263 -0.0490 0.059 Uiso 0.303(18) 1 calc R U P B 1
H22B H 0.4295 1.3651 -0.0010 0.059 Uiso 0.303(18) 1 calc R U P B 1
C21' C 0.2374(17) 1.2875(15) -0.0982(5) 0.061(2) Uani 0.697(18) 1 d D U P B 2
H21D H 0.2082 1.3711 -0.1023 0.091 Uiso 0.697(18) 1 calc R U P B 2
H21E H 0.2566 1.2559 -0.1370 0.091 Uiso 0.697(18) 1 calc R U P B 2
H21F H 0.1404 1.2103 -0.0807 0.091 Uiso 0.697(18) 1 calc R U P B 2
C22' C 0.4049(15) 1.3269(10) -0.0585(5) 0.046(2) Uani 0.697(18) 1 d D U P B 2
H22C H 0.5007 1.4069 -0.0761 0.055 Uiso 0.697(18) 1 calc R U P B 2
H22D H 0.3847 1.3614 -0.0199 0.055 Uiso 0.697(18) 1 calc R U P B 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 O4 1.601(4) . ?
V1 O2 1.959(4) . ?
V1 O5 2.008(4) . ?
V1 O1 2.014(3) 2_666 ?
V1 N1 2.123(4) . ?
V1 O1 2.302(3) . ?
V2 O6 1.602(4) . ?
V2 O5 1.989(4) . ?
V2 O2 1.999(3) 2_666 ?
V2 O7 2.003(4) . ?
V2 O8 2.011(4) . ?
V2 O1 2.284(4) . ?
V3 O15 1.609(3) . ?
V3 O9 1.967(4) . ?
V3 O16 2.000(4) . ?
V3 O10 2.010(3) 2_675 ?
V3 N2 2.125(4) . ?
V3 O10 2.301(3) . ?
V4 O12 1.594(4) . ?
V4 O16 1.991(4) 2_675 ?
V4 O9 1.997(4) . ?
V4 O13 2.001(4) . ?
V4 O14 2.006(4) . ?
V4 O10 2.293(4) 2_675 ?
O1 C4 1.431(5) . ?
O1 V1 2.014(3) 2_666 ?
O2 C3 1.422(5) . ?
O2 V2 1.999(3) 2_666 ?
O3 C1 1.391(7) . ?
O3 H3 0.8200 . ?
O5 C6' 1.449(7) . ?
O5 C6 1.459(9) . ?
O7 C8 1.261(6) . ?
O8 C10 1.290(7) . ?
O10 C15 1.435(5) . ?
O10 V3 2.011(3) 2_675 ?
O10 V4 2.293(4) 2_675 ?
O9 C14 1.429(6) . ?
O11 C12 1.365(7) . ?
O11 H11D 0.8200 . ?
O13 C19 1.260(6) . ?
O14 C17 1.297(7) . ?
O16 C22 1.449(10) . ?
O16 C22' 1.462(7) . ?
O16 V4 1.991(4) 2_675 ?
N1 C2 1.485(6) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 C13 1.483(6) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
C1 C2 1.532(6) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 C3 1.532(6) . ?
C2 C4 1.532(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.499(10) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C5' C6' 1.507(9) . ?
C5' H5'A 0.9600 . ?
C5' H5'B 0.9600 . ?
C5' H5'C 0.9600 . ?
C6' H6'A 0.9700 . ?
C6' H6'B 0.9700 . ?
C7 C8 1.487(8) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.418(8) . ?
C9 C10 1.373(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.510(8) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.538(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.526(7) . ?
C13 C15 1.539(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.515(9) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.361(9) . ?
C18 C19 1.402(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.502(9) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.496(10) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C21' C22' 1.504(8) . ?
C21' H21D 0.9600 . ?
C21' H21E 0.9600 . ?
C21' H21F 0.9600 . ?
C22' H22C 0.9700 . ?
C22' H22D 0.9700 . ?

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
O4 V1 O2 104.25(18) . . ?
O4 V1 O5 97.55(18) . . ?
O2 V1 O5 158.09(14) . . ?
O4 V1 O1 107.67(17) . 2_666 ?
O2 V1 O1 78.82(13) . 2_666 ?
O5 V1 O1 96.83(15) . 2_666 ?
O4 V1 N1 104.35(18) . . ?
O2 V1 N1 80.11(15) . . ?
O5 V1 N1 92.46(16) . . ?
O1 V1 N1 145.06(14) 2_666 . ?
O4 V1 O1 171.93(16) . . ?
O2 V1 O1 82.95(14) . . ?
O5 V1 O1 75.16(14) . . ?
O1 V1 O1 77.04(14) 2_666 . ?
N1 V1 O1 72.96(14) . . ?
O6 V2 O5 100.5(2) . . ?
O6 V2 O2 99.79(18) . 2_666 ?
O5 V2 O2 90.08(15) . 2_666 ?
O6 V2 O7 100.3(2) . . ?
O5 V2 O7 159.23(15) . . ?
O2 V2 O7 86.80(15) 2_666 . ?
O6 V2 O8 100.40(18) . . ?
O5 V2 O8 88.87(17) . . ?
O2 V2 O8 159.63(15) 2_666 . ?
O7 V2 O8 87.00(16) . . ?
O6 V2 O1 170.64(16) . . ?
O5 V2 O1 75.92(14) . . ?
O2 V2 O1 71.80(13) 2_666 . ?
O7 V2 O1 83.61(16) . . ?
O8 V2 O1 88.23(14) . . ?
O15 V3 O9 104.80(18) . . ?
O15 V3 O16 97.13(18) . . ?
O9 V3 O16 158.00(14) . . ?
O15 V3 O10 107.32(17) . 2_675 ?
O9 V3 O10 79.44(14) . 2_675 ?
O16 V3 O10 95.83(15) . 2_675 ?
O15 V3 N2 105.07(18) . . ?
O9 V3 N2 79.93(15) . . ?
O16 V3 N2 92.87(17) . . ?
O10 V3 N2 145.04(14) 2_675 . ?
O15 V3 O10 171.90(16) . . ?
O9 V3 O10 82.69(14) . . ?
O16 V3 O10 75.32(14) . . ?
O10 V3 O10 76.76(14) 2_675 . ?
N2 V3 O10 72.86(14) . . ?
O12 V4 O16 100.0(2) . 2_675 ?
O12 V4 O9 100.31(19) . . ?
O16 V4 O9 89.72(16) 2_675 . ?
O12 V4 O13 100.7(2) . . ?
O16 V4 O13 159.31(16) 2_675 . ?
O9 V4 O13 86.09(15) . . ?
O12 V4 O14 100.6(2) . . ?
O16 V4 O14 89.52(17) 2_675 . ?
O9 V4 O14 158.92(15) . . ?
O13 V4 O14 87.23(17) . . ?
O12 V4 O10 171.25(18) . 2_675 ?
O16 V4 O10 75.67(14) 2_675 2_675 ?
O9 V4 O10 72.31(13) . 2_675 ?
O13 V4 O10 83.76(16) . 2_675 ?
O14 V4 O10 87.11(15) . 2_675 ?
C4 O1 V1 122.5(3) . 2_666 ?
C4 O1 V2 124.7(3) . . ?
V1 O1 V2 97.41(13) 2_666 . ?
C4 O1 V1 109.9(2) . . ?
V1 O1 V1 102.96(14) 2_666 . ?
V2 O1 V1 94.29(13) . . ?
C3 O2 V1 116.6(3) . . ?
C3 O2 V2 127.1(3) . 2_666 ?
V1 O2 V2 109.62(15) . 2_666 ?
C1 O3 H3 109.5 . . ?
C6' O5 V2 123.4(6) . . ?
C6 O5 V2 118.3(11) . . ?
C6' O5 V1 120.9(6) . . ?
C6 O5 V1 115.2(10) . . ?
V2 O5 V1 114.53(17) . . ?
C8 O7 V2 129.3(4) . . ?
C10 O8 V2 125.6(4) . . ?
C15 O10 V3 122.5(3) . 2_675 ?
C15 O10 V4 124.8(3) . 2_675 ?
V3 O10 V4 96.90(13) 2_675 2_675 ?
C15 O10 V3 110.2(2) . . ?
V3 O10 V3 103.24(14) 2_675 . ?
V4 O10 V3 94.13(13) 2_675 . ?
C14 O9 V3 116.4(3) . . ?
C14 O9 V4 128.1(3) . . ?
V3 O9 V4 108.95(15) . . ?
C12 O11 H11D 109.5 . . ?
C19 O13 V4 129.1(4) . . ?
C17 O14 V4 125.2(4) . . ?
C22 O16 V4 123.1(12) . 2_675 ?
C22' O16 V4 122.9(5) . 2_675 ?
C22 O16 V3 121.9(12) . . ?
C22' O16 V3 119.1(5) . . ?
V4 O16 V3 114.83(17) 2_675 . ?
C2 N1 V1 102.6(3) . . ?
C2 N1 H1A 111.2 . . ?
V1 N1 H1A 111.2 . . ?
C2 N1 H1B 111.2 . . ?
V1 N1 H1B 111.2 . . ?
H1A N1 H1B 109.2 . . ?
C13 N2 V3 102.9(3) . . ?
C13 N2 H2A 111.2 . . ?
V3 N2 H2A 111.2 . . ?
C13 N2 H2B 111.2 . . ?
V3 N2 H2B 111.2 . . ?
H2A N2 H2B 109.1 . . ?
O3 C1 C2 107.5(4) . . ?
O3 C1 H1C 110.2 . . ?
C2 C1 H1C 110.2 . . ?
O3 C1 H1D 110.2 . . ?
C2 C1 H1D 110.2 . . ?
H1C C1 H1D 108.5 . . ?
N1 C2 C1 111.2(4) . . ?
N1 C2 C3 105.4(4) . . ?
C1 C2 C3 111.1(4) . . ?
N1 C2 C4 107.1(3) . . ?
C1 C2 C4 111.2(4) . . ?
C3 C2 C4 110.5(4) . . ?
O2 C3 C2 108.9(3) . . ?
O2 C3 H3A 109.9 . . ?
C2 C3 H3A 109.9 . . ?
O2 C3 H3B 109.9 . . ?
C2 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
O1 C4 C2 110.4(3) . . ?
O1 C4 H4A 109.6 . . ?
C2 C4 H4A 109.6 . . ?
O1 C4 H4B 109.6 . . ?
C2 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O5 C6 C5 109.7(13) . . ?
O5 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
O5 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C6' C5' H5'A 109.5 . . ?
C6' C5' H5'B 109.5 . . ?
H5'A C5' H5'B 109.5 . . ?
C6' C5' H5'C 109.5 . . ?
H5'A C5' H5'C 109.5 . . ?
H5'B C5' H5'C 109.5 . . ?
O5 C6' C5' 109.9(8) . . ?
O5 C6' H6'A 109.7 . . ?
C5' C6' H6'A 109.7 . . ?
O5 C6' H6'B 109.7 . . ?
C5' C6' H6'B 109.7 . . ?
H6'A C6' H6'B 108.2 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O7 C8 C9 123.2(5) . . ?
O7 C8 C7 117.3(5) . . ?
C9 C8 C7 119.5(5) . . ?
C10 C9 C8 124.3(5) . . ?
C10 C9 H9 117.8 . . ?
C8 C9 H9 117.8 . . ?
O8 C10 C9 125.3(5) . . ?
O8 C10 C11 114.1(6) . . ?
C9 C10 C11 120.6(6) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O11 C12 C13 109.9(5) . . ?
O11 C12 H12A 109.7 . . ?
C13 C12 H12A 109.7 . . ?
O11 C12 H12B 109.7 . . ?
C13 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
N2 C13 C14 105.5(4) . . ?
N2 C13 C12 111.4(4) . . ?
C14 C13 C12 111.5(4) . . ?
N2 C13 C15 107.1(4) . . ?
C14 C13 C15 110.6(4) . . ?
C12 C13 C15 110.6(4) . . ?
O9 C14 C13 108.7(4) . . ?
O9 C14 H14A 109.9 . . ?
C13 C14 H14A 109.9 . . ?
O9 C14 H14B 109.9 . . ?
C13 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
O10 C15 C13 110.0(3) . . ?
O10 C15 H15A 109.7 . . ?
C13 C15 H15A 109.7 . . ?
O10 C15 H15B 109.7 . . ?
C13 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O14 C17 C18 125.4(5) . . ?
O14 C17 C16 114.0(6) . . ?
C18 C17 C16 120.4(6) . . ?
C17 C18 C19 124.7(5) . . ?
C17 C18 H18 117.6 . . ?
C19 C18 H18 117.6 . . ?
O13 C19 C18 123.7(6) . . ?
O13 C19 C20 115.6(6) . . ?
C18 C19 C20 120.7(6) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O16 C22 C21 106.2(15) . . ?
O16 C22 H22A 110.5 . . ?
C21 C22 H22A 110.5 . . ?
O16 C22 H22B 110.5 . . ?
C21 C22 H22B 110.5 . . ?
H22A C22 H22B 108.7 . . ?
C22' C21' H21D 109.5 . . ?
C22' C21' H21E 109.5 . . ?
H21D C21' H21E 109.5 . . ?
C22' C21' H21F 109.5 . . ?
H21D C21' H21F 109.5 . . ?
H21E C21' H21F 109.5 . . ?
O16 C22' C21' 114.7(7) . . ?
O16 C22' H22C 108.6 . . ?
C21' C22' H22C 108.6 . . ?
O16 C22' H22D 108.6 . . ?
C21' C22' H22D 108.6 . . ?
H22C C22' H22D 107.6 . . ?

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 N1 C2 C1 173.7(3) . . . . ?
V1 N1 C2 C3 53.1(3) . . . . ?
V1 N1 C2 C4 -64.6(3) . . . . ?
O3 C1 C2 N1 175.9(4) . . . . ?
O3 C1 C2 C3 -67.0(5) . . . . ?
O3 C1 C2 C4 56.7(5) . . . . ?
V1 O2 C3 C2 15.7(5) . . . . ?
V2 O2 C3 C2 -132.4(3) 2_666 . . . ?
N1 C2 C3 O2 -46.7(5) . . . . ?
C1 C2 C3 O2 -167.4(4) . . . . ?
C4 C2 C3 O2 68.6(5) . . . . ?
V1 O1 C4 C2 123.8(3) 2_666 . . . ?
V2 O1 C4 C2 -107.3(3) . . . . ?
V1 O1 C4 C2 3.0(4) . . . . ?
N1 C2 C4 O1 39.1(5) . . . . ?
C1 C2 C4 O1 160.8(4) . . . . ?
C3 C2 C4 O1 -75.2(5) . . . . ?
V2 O5 C6 C5 -99.9(18) . . . . ?
V1 O5 C6 C5 119.5(17) . . . . ?
V2 O5 C6' C5' 93.0(10) . . . . ?
V1 O5 C6' C5' -74.3(10) . . . . ?
V2 O7 C8 C9 -5.5(9) . . . . ?
V2 O7 C8 C7 175.2(5) . . . . ?
O7 C8 C9 C10 -8.7(11) . . . . ?
C7 C8 C9 C10 170.6(7) . . . . ?
V2 O8 C10 C9 20.8(9) . . . . ?
V2 O8 C10 C11 -160.8(5) . . . . ?
C8 C9 C10 O8 0.3(11) . . . . ?
C8 C9 C10 C11 -178.0(7) . . . . ?
V3 N2 C13 C14 53.4(4) . . . . ?
V3 N2 C13 C12 174.5(3) . . . . ?
V3 N2 C13 C15 -64.5(4) . . . . ?
O11 C12 C13 N2 174.0(4) . . . . ?
O11 C12 C13 C14 -68.5(6) . . . . ?
O11 C12 C13 C15 55.0(6) . . . . ?
V3 O9 C14 C13 16.6(5) . . . . ?
V4 O9 C14 C13 -131.5(3) . . . . ?
N2 C13 C14 O9 -47.4(5) . . . . ?
C12 C13 C14 O9 -168.4(4) . . . . ?
C15 C13 C14 O9 68.1(5) . . . . ?
V3 O10 C15 C13 125.0(3) 2_675 . . . ?
V4 O10 C15 C13 -107.0(4) 2_675 . . . ?
V3 O10 C15 C13 3.5(4) . . . . ?
N2 C13 C15 O10 38.6(5) . . . . ?
C14 C13 C15 O10 -75.9(5) . . . . ?
C12 C13 C15 O10 160.1(4) . . . . ?
V4 O14 C17 C18 -21.7(10) . . . . ?
V4 O14 C17 C16 163.6(6) . . . . ?
O14 C17 C18 C19 3.5(13) . . . . ?
C16 C17 C18 C19 177.9(8) . . . . ?
V4 O13 C19 C18 5.8(10) . . . . ?
V4 O13 C19 C20 -175.9(6) . . . . ?
C17 C18 C19 O13 5.3(12) . . . . ?
C17 C18 C19 C20 -172.9(8) . . . . ?
V4 O16 C22 C21 93(2) 2_675 . . . ?
V3 O16 C22 C21 -93(2) . . . . ?
V4 O16 C22' C21' 89.7(9) 2_675 . . . ?
V3 O16 C22' C21' -69.1(10) . . . . ?

_refine_diff_density_max         1.311
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.112

####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 2106169'
loop_
_audit_author_name
_audit_author_address
'jian zhou'
;Chongqing Normal University
China
;
_audit_update_record             
;
2021-08-29 deposited with the CCDC.	2021-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H46 N2 O16 V4'
_chemical_formula_sum            'C32 H46 N2 O16 V4'
_chemical_formula_weight         918.47

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'
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'
N N 0.0061 0.0033 '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                   12.871(3)
_cell_length_b                   8.3842(17)
_cell_length_c                   17.948(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.56(3)
_cell_angle_gamma                90
_cell_volume                     1936.1(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11576
_cell_measurement_theta_min      2.7322
_cell_measurement_theta_max      27.4575

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_F_000             944
_exptl_transmission_factor_min   0.946
_exptl_transmission_factor_max   0.982
_exptl_crystal_size_max          0.054
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.019
_exptl_absorpt_coefficient_mu    1.008
_shelx_estimated_absorpt_T_min   0.948
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14479
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.732
_diffrn_reflns_theta_max         25.096
_diffrn_reflns_theta_full        25.096
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3440
_reflns_number_gt                2709
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0365P)²+1.1162P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0029(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3440
_refine_ls_number_parameters     247
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0294
_refine_ls_wR_factor_ref         0.0821
_refine_ls_wR_factor_gt          0.0713
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.000
_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 0.53156(3) 0.39884(4) 0.42280(2) 0.02169(14) Uani 1 1 d . . . . .
V2 V 0.71234(3) 0.54300(5) 0.54513(2) 0.02779(14) Uani 1 1 d . . . . .
O1 O 0.40427(13) 0.50633(18) 0.38733(8) 0.0238(4) Uani 1 1 d . . . . .
O2 O 0.55771(13) 0.63078(17) 0.48883(8) 0.0230(4) Uani 1 1 d . . . . .
O3 O 0.47323(16) 0.9617(2) 0.30319(10) 0.0387(5) Uani 1 1 d . . . . .
H3A H 0.4944 1.0402 0.3263 0.058 Uiso 1 1 calc R U . . .
O4 O 0.53088(15) 0.23321(19) 0.37816(10) 0.0338(4) Uani 1 1 d . . . . .
O5 O 0.72241(15) 0.7554(2) 0.59574(10) 0.0405(5) Uani 1 1 d . . . . .
O6 O 0.77890(15) 0.6448(2) 0.45787(10) 0.0389(5) Uani 1 1 d . . . . .
O7 O 0.80685(15) 0.4537(2) 0.58658(11) 0.0429(5) Uani 1 1 d . . . . .
O8 O 0.66511(13) 0.36312(18) 0.47878(9) 0.0280(4) Uani 1 1 d . . . . .
N1 N 0.59555(16) 0.5675(2) 0.34877(11) 0.0251(5) Uani 1 1 d . . . . .
H1A H 0.6617 0.5882 0.3609 0.030 Uiso 1 1 calc R U . . .
H1B H 0.5913 0.5332 0.3019 0.030 Uiso 1 1 calc R U . . .
C1 C 0.8400(2) 0.7666(3) 0.46036(17) 0.0391(7) Uani 1 1 d . . . . .
C2 C 0.9015(3) 0.7930(5) 0.3921(2) 0.0691(11) Uani 1 1 d . . . . .
H2 H 0.9551 0.7137 0.3896 0.104 Uiso 1 1 calc R U . . .
H1 H 0.9325 0.8971 0.3941 0.104 Uiso 1 1 calc R U . . .
H3 H 0.8565 0.7852 0.3487 0.104 Uiso 1 1 calc R U . . .
C3 C 0.8495(2) 0.8685(3) 0.52039(18) 0.0449(8) Uani 1 1 d . . . . .
H4 H 0.8995 0.9484 0.5182 0.054 Uiso 1 1 calc R U . . .
C4 C 0.7906(2) 0.8613(3) 0.58368(17) 0.0382(7) Uani 1 1 d . . . . .
C5 C 0.8037(3) 0.9835(4) 0.64416(19) 0.0558(9) Uani 1 1 d . . . . .
H5 H 0.7372 1.0085 0.6640 0.084 Uiso 1 1 calc R U . . .
H6 H 0.8339 1.0784 0.6241 0.084 Uiso 1 1 calc R U . . .
H7 H 0.8486 0.9420 0.6831 0.084 Uiso 1 1 calc R U . . .
C6 C 0.5493(2) 0.7661(3) 0.44012(13) 0.0267(6) Uani 1 1 d . . . . .
H13 H 0.6131 0.8275 0.4431 0.032 Uiso 1 1 calc R U . . .
H12 H 0.4929 0.8342 0.4556 0.032 Uiso 1 1 calc R U . . .
C7 C 0.5287(2) 0.7107(3) 0.35962(12) 0.0240(5) Uani 1 1 d . . . . .
C8 C 0.4169(2) 0.6524(3) 0.34817(13) 0.0270(6) Uani 1 1 d . . . . .
H8 H 0.3691 0.7317 0.3665 0.032 Uiso 1 1 calc R U . . .
H9 H 0.4018 0.6364 0.2955 0.032 Uiso 1 1 calc R U . . .
C9 C 0.5521(2) 0.8424(3) 0.30366(14) 0.0318(6) Uani 1 1 d . . . . .
H10 H 0.6187 0.8907 0.3166 0.038 Uiso 1 1 calc R U . . .
H11 H 0.5566 0.7966 0.2542 0.038 Uiso 1 1 calc R U . . .
C10 C 0.7299(2) 0.2265(3) 0.46664(15) 0.0365(7) Uani 1 1 d . . . . .
H20 H 0.6858 0.1349 0.4562 0.044 Uiso 1 1 calc R U . . .
H14 H 0.7698 0.2042 0.5121 0.044 Uiso 1 1 calc R U . . .
C11 C 0.8039(2) 0.2461(3) 0.40375(16) 0.0374(7) Uani 1 1 d . . . . .
C12 C 0.8995(3) 0.3163(4) 0.4152(2) 0.0574(9) Uani 1 1 d . . . . .
H15 H 0.9189 0.3527 0.4625 0.069 Uiso 1 1 calc R U . . .
C13 C 0.9673(3) 0.3335(5) 0.3573(3) 0.0721(11) Uani 1 1 d . . . . .
H19 H 1.0310 0.3838 0.3655 0.087 Uiso 1 1 calc R U . . .
C14 C 0.9406(3) 0.2764(6) 0.2879(2) 0.0790(13) Uani 1 1 d . . . . .
H16 H 0.9867 0.2870 0.2492 0.095 Uiso 1 1 calc R U . . .
C15 C 0.8469(3) 0.2041(5) 0.2753(2) 0.0717(11) Uani 1 1 d . . . . .
H18 H 0.8292 0.1640 0.2283 0.086 Uiso 1 1 calc R U . . .
C16 C 0.7785(3) 0.1909(4) 0.33302(17) 0.0537(8) Uani 1 1 d . . . . .
H17 H 0.7139 0.1438 0.3241 0.064 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 O4 1.6031(16) . ?
V1 O1 1.9608(17) . ?
V1 O8 1.9900(18) . ?
V1 O2 1.9992(17) 3_666 ?
V1 N1 2.122(2) . ?
V1 O2 2.2973(16) . ?
V2 O7 1.595(2) . ?
V2 O6 1.9969(19) . ?
V2 O1 1.9981(17) 3_666 ?
V2 O5 2.0020(18) . ?
V2 O8 2.0056(17) . ?
V2 O2 2.3268(18) . ?
O1 C8 1.424(3) . ?
O1 V2 1.9981(17) 3_666 ?
O2 C6 1.435(3) . ?
O2 V1 1.9993(17) 3_666 ?
O3 C9 1.425(3) . ?
O3 H3A 0.8200 . ?
O5 C4 1.271(3) . ?
O6 C1 1.289(3) . ?
O8 C10 1.437(3) . ?
N1 C7 1.493(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
C1 C3 1.378(4) . ?
C1 C2 1.493(4) . ?
C2 H2 0.9600 . ?
C2 H1 0.9600 . ?
C2 H3 0.9600 . ?
C3 C4 1.384(4) . ?
C3 H4 0.9300 . ?
C4 C5 1.499(4) . ?
C5 H5 0.9600 . ?
C5 H6 0.9600 . ?
C5 H7 0.9600 . ?
C6 C7 1.534(3) . ?
C6 H13 0.9700 . ?
C6 H12 0.9700 . ?
C7 C8 1.528(4) . ?
C7 C9 1.528(3) . ?
C8 H8 0.9700 . ?
C8 H9 0.9700 . ?
C9 H10 0.9700 . ?
C9 H11 0.9700 . ?
C10 C11 1.506(4) . ?
C10 H20 0.9700 . ?
C10 H14 0.9700 . ?
C11 C12 1.374(4) . ?
C11 C16 1.382(4) . ?
C12 C13 1.382(5) . ?
C12 H15 0.9300 . ?
C13 C14 1.370(6) . ?
C13 H19 0.9300 . ?
C14 C15 1.363(6) . ?
C14 H16 0.9300 . ?
C15 C16 1.383(5) . ?
C15 H18 0.9300 . ?
C16 H17 0.9300 . ?

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
O4 V1 O1 104.05(8) . . ?
O4 V1 O8 96.60(8) . . ?
O1 V1 O8 159.34(7) . . ?
O4 V1 O2 107.07(8) . 3_666 ?
O1 V1 O2 79.71(7) . 3_666 ?
O8 V1 O2 95.04(7) . 3_666 ?
O4 V1 N1 105.14(8) . . ?
O1 V1 N1 79.96(7) . . ?
O8 V1 N1 94.11(8) . . ?
O2 V1 N1 145.16(7) 3_666 . ?
O4 V1 O2 171.80(8) . . ?
O1 V1 O2 83.56(6) . . ?
O8 V1 O2 75.79(6) . . ?
O2 V1 O2 77.01(6) 3_666 . ?
N1 V1 O2 72.84(7) . . ?
O7 V2 O6 103.20(10) . . ?
O7 V2 O1 101.29(9) . 3_666 ?
O6 V2 O1 155.45(8) . 3_666 ?
O7 V2 O5 99.60(10) . . ?
O6 V2 O5 87.24(8) . . ?
O1 V2 O5 87.09(7) 3_666 . ?
O7 V2 O8 97.99(9) . . ?
O6 V2 O8 89.16(7) . . ?
O1 V2 O8 89.08(7) 3_666 . ?
O5 V2 O8 162.40(8) . . ?
O7 V2 O2 169.54(8) . . ?
O6 V2 O2 84.52(7) . . ?
O1 V2 O2 71.41(6) 3_666 . ?
O5 V2 O2 87.69(7) . . ?
O8 V2 O2 74.82(6) . . ?
C8 O1 V1 116.73(15) . . ?
C8 O1 V2 125.14(15) . 3_666 ?
V1 O1 V2 110.05(7) . 3_666 ?
C6 O2 V1 123.09(14) . 3_666 ?
C6 O2 V1 110.33(12) . . ?
V1 O2 V1 103.00(6) 3_666 . ?
C6 O2 V2 124.37(14) . . ?
V1 O2 V2 96.86(6) 3_666 . ?
V1 O2 V2 93.89(6) . . ?
C9 O3 H3A 109.5 . . ?
C4 O5 V2 125.50(19) . . ?
C1 O6 V2 125.85(18) . . ?
C10 O8 V1 122.70(15) . . ?
C10 O8 V2 121.44(16) . . ?
V1 O8 V2 115.49(8) . . ?
C7 N1 V1 102.67(14) . . ?
C7 N1 H1A 111.2 . . ?
V1 N1 H1A 111.2 . . ?
C7 N1 H1B 111.2 . . ?
V1 N1 H1B 111.2 . . ?
H1A N1 H1B 109.1 . . ?
O6 C1 C3 124.0(3) . . ?
O6 C1 C2 115.2(3) . . ?
C3 C1 C2 120.8(3) . . ?
C1 C2 H2 109.5 . . ?
C1 C2 H1 109.5 . . ?
H2 C2 H1 109.5 . . ?
C1 C2 H3 109.5 . . ?
H2 C2 H3 109.5 . . ?
H1 C2 H3 109.5 . . ?
C1 C3 C4 125.1(3) . . ?
C1 C3 H4 117.4 . . ?
C4 C3 H4 117.4 . . ?
O5 C4 C3 124.5(3) . . ?
O5 C4 C5 114.8(3) . . ?
C3 C4 C5 120.7(3) . . ?
C4 C5 H5 109.5 . . ?
C4 C5 H6 109.5 . . ?
H5 C5 H6 109.5 . . ?
C4 C5 H7 109.5 . . ?
H5 C5 H7 109.5 . . ?
H6 C5 H7 109.5 . . ?
O2 C6 C7 110.06(18) . . ?
O2 C6 H13 109.6 . . ?
C7 C6 H13 109.6 . . ?
O2 C6 H12 109.6 . . ?
C7 C6 H12 109.6 . . ?
H13 C6 H12 108.2 . . ?
N1 C7 C8 105.61(18) . . ?
N1 C7 C9 111.7(2) . . ?
C8 C7 C9 110.2(2) . . ?
N1 C7 C6 106.31(19) . . ?
C8 C7 C6 111.2(2) . . ?
C9 C7 C6 111.62(19) . . ?
O1 C8 C7 109.20(19) . . ?
O1 C8 H8 109.8 . . ?
C7 C8 H8 109.8 . . ?
O1 C8 H9 109.8 . . ?
C7 C8 H9 109.8 . . ?
H8 C8 H9 108.3 . . ?
O3 C9 C7 111.0(2) . . ?
O3 C9 H10 109.4 . . ?
C7 C9 H10 109.4 . . ?
O3 C9 H11 109.4 . . ?
C7 C9 H11 109.4 . . ?
H10 C9 H11 108.0 . . ?
O8 C10 C11 114.1(2) . . ?
O8 C10 H20 108.7 . . ?
C11 C10 H20 108.7 . . ?
O8 C10 H14 108.7 . . ?
C11 C10 H14 108.7 . . ?
H20 C10 H14 107.6 . . ?
C12 C11 C16 118.0(3) . . ?
C12 C11 C10 121.1(3) . . ?
C16 C11 C10 120.8(3) . . ?
C11 C12 C13 120.9(3) . . ?
C11 C12 H15 119.5 . . ?
C13 C12 H15 119.5 . . ?
C14 C13 C12 119.9(4) . . ?
C14 C13 H19 120.0 . . ?
C12 C13 H19 120.0 . . ?
C15 C14 C13 120.4(4) . . ?
C15 C14 H16 119.8 . . ?
C13 C14 H16 119.8 . . ?
C14 C15 C16 119.3(4) . . ?
C14 C15 H18 120.3 . . ?
C16 C15 H18 120.3 . . ?
C11 C16 C15 121.4(3) . . ?
C11 C16 H17 119.3 . . ?
C15 C16 H17 119.3 . . ?

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
V2 O6 C1 C3 -16.1(4) . . . . ?
V2 O6 C1 C2 164.2(2) . . . . ?
O6 C1 C3 C4 -4.7(5) . . . . ?
C2 C1 C3 C4 174.9(3) . . . . ?
V2 O5 C4 C3 19.5(4) . . . . ?
V2 O5 C4 C5 -160.8(2) . . . . ?
C1 C3 C4 O5 2.8(5) . . . . ?
C1 C3 C4 C5 -176.9(3) . . . . ?
V1 O2 C6 C7 -123.50(18) 3_666 . . . ?
V1 O2 C6 C7 -1.6(2) . . . . ?
V2 O2 C6 C7 108.30(19) . . . . ?
V1 N1 C7 C8 -52.80(18) . . . . ?
V1 N1 C7 C9 -172.59(16) . . . . ?
V1 N1 C7 C6 65.40(19) . . . . ?
O2 C6 C7 N1 -40.3(3) . . . . ?
O2 C6 C7 C8 74.1(3) . . . . ?
O2 C6 C7 C9 -162.4(2) . . . . ?
V1 O1 C8 C7 -13.6(2) . . . . ?
V2 O1 C8 C7 131.87(17) 3_666 . . . ?
N1 C7 C8 O1 45.1(2) . . . . ?
C9 C7 C8 O1 165.93(19) . . . . ?
C6 C7 C8 O1 -69.8(2) . . . . ?
N1 C7 C9 O3 166.72(19) . . . . ?
C8 C7 C9 O3 49.6(3) . . . . ?
C6 C7 C9 O3 -74.4(3) . . . . ?
V1 O8 C10 C11 85.5(3) . . . . ?
V2 O8 C10 C11 -87.2(2) . . . . ?
O8 C10 C11 C12 86.1(3) . . . . ?
O8 C10 C11 C16 -95.4(3) . . . . ?
C16 C11 C12 C13 1.1(5) . . . . ?
C10 C11 C12 C13 179.7(3) . . . . ?
C11 C12 C13 C14 -1.8(6) . . . . ?
C12 C13 C14 C15 0.7(6) . . . . ?
C13 C14 C15 C16 0.9(6) . . . . ?
C12 C11 C16 C15 0.5(5) . . . . ?
C10 C11 C16 C15 -178.1(3) . . . . ?
C14 C15 C16 C11 -1.5(6) . . . . ?

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
O3 H3A O4 0.82 1.92 2.737(2) 174.4 1_565
N1 H1A O6 0.89 2.32 3.094(3) 145.2 .
N1 H1B O3 0.89 2.13 2.979(3) 160.5 2_645
C6 H13 O6 0.97 2.63 3.134(3) 112.3 .
C9 H11 O4 0.97 2.66 3.527(3) 149.7 2_655
C10 H14 O7 0.97 2.52 3.021(3) 112.0 .

_refine_diff_density_max         0.293
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.057

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 2106165'
loop_
_audit_author_name
_audit_author_address
'jian zhou'
;Chongqing Normal University
China
;
_audit_update_record             
;
2021-08-29 deposited with the CCDC.	2021-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H38 N2 O16 V4'
_chemical_formula_weight         766.28

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'

_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                   8.1333(3)
_cell_length_b                   22.4738(8)
_cell_length_c                   8.8615(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.2050(13)
_cell_angle_gamma                90
_cell_volume                     1538.68(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    14376
_cell_measurement_theta_min      2.788
_cell_measurement_theta_max      25.088

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_F_000             784
_exptl_transmission_factor_min   0.821
_exptl_transmission_factor_max   0.915
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.069
_exptl_absorpt_coefficient_mu    1.249
_shelx_estimated_absorpt_T_min   0.733
_shelx_estimated_absorpt_T_max   0.919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14376
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.788
_diffrn_reflns_theta_max         25.088
_diffrn_reflns_theta_full        25.088
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2736
_reflns_number_gt                2325
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0376P)²+1.3271P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2736
_refine_ls_number_parameters     193
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0294
_refine_ls_wR_factor_ref         0.0787
_refine_ls_wR_factor_gt          0.0725
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.002
_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 0.32182(5) 0.50014(2) 0.55951(4) 0.01860(12) Uani 1 1 d . . . . .
V2 V 0.37133(5) 0.39511(2) 0.33031(5) 0.02336(13) Uani 1 1 d . . . . .
N1 N 0.1646(2) 0.57155(9) 0.4390(2) 0.0220(4) Uani 1 1 d . . . . .
H1A H 0.0545 0.5661 0.4336 0.026 Uiso 1 1 calc R U . . .
H1B H 0.2013 0.6061 0.4867 0.026 Uiso 1 1 calc R U . . .
C10 C 0.1435(3) 0.50554(10) 0.2208(3) 0.0241(5) Uani 1 1 d . . . . .
H13 H 0.0195 0.4990 0.1908 0.029 Uiso 1 1 calc R U . . .
H14 H 0.1807 0.4984 0.1285 0.029 Uiso 1 1 calc R U . . .
C1 C 0.2809(4) 0.30099(12) 0.5238(4) 0.0386(7) Uani 1 1 d . . . . .
C2 C 0.4159(4) 0.26464(13) 0.5154(4) 0.0456(8) Uani 1 1 d . . . . .
H4 H 0.4192 0.2260 0.5535 0.055 Uiso 1 1 calc R U . . .
C3 C 0.5449(4) 0.28155(12) 0.4550(3) 0.0364(7) Uani 1 1 d . . . . .
C4 C 0.6884(5) 0.23925(15) 0.4593(5) 0.0606(10) Uani 1 1 d . . . . .
H3 H 0.7804 0.2440 0.5575 0.091 Uiso 1 1 calc R U . . .
H1 H 0.7311 0.2475 0.3720 0.091 Uiso 1 1 calc R U . . .
H2 H 0.6457 0.1992 0.4511 0.091 Uiso 1 1 calc R U . . .
C5 C 0.1568(5) 0.27947(17) 0.6055(6) 0.0755(13) Uani 1 1 d . . . . .
H7 H 0.1916 0.2940 0.7127 0.113 Uiso 1 1 calc R U . . .
H6 H 0.1562 0.2368 0.6064 0.113 Uiso 1 1 calc R U . . .
H5 H 0.0427 0.2938 0.5498 0.113 Uiso 1 1 calc R U . . .
C6 C 0.5979(5) 0.42906(18) 0.1413(4) 0.0614(10) Uani 1 1 d . . . . .
H10 H 0.6559 0.4618 0.1099 0.092 Uiso 1 1 calc R U . . .
H9 H 0.5031 0.4162 0.0521 0.092 Uiso 1 1 calc R U . . .
H8 H 0.6778 0.3968 0.1775 0.092 Uiso 1 1 calc R U . . .
C7 C 0.1862(3) 0.56933(10) 0.2788(3) 0.0199(5) Uani 1 1 d . . . . .
C9 C 0.0661(3) 0.61367(11) 0.1669(3) 0.0269(5) Uani 1 1 d . . . . .
H16 H -0.0534 0.6039 0.1550 0.032 Uiso 1 1 calc R U . . .
H15 H 0.0889 0.6535 0.2108 0.032 Uiso 1 1 calc R U . . .
O1 O 0.48579(19) 0.55551(7) 0.44040(18) 0.0183(3) Uani 1 1 d . . . . .
O2 O 0.2307(2) 0.46598(7) 0.34585(18) 0.0224(4) Uani 1 1 d . . . . .
O3 O 0.0936(2) 0.61168(9) 0.0180(2) 0.0397(5) Uani 1 1 d . . . . .
H3A H 0.0012 0.6163 -0.0524 0.060 Uiso 1 1 calc R U . . .
O4 O 0.2085(2) 0.46970(8) 0.6564(2) 0.0327(4) Uani 1 1 d . . . . .
O5 O 0.2574(2) 0.37035(8) 0.1605(2) 0.0390(5) Uani 1 1 d . . . . .
O6 O 0.5338(2) 0.44760(7) 0.26653(18) 0.0257(4) Uani 1 1 d . . . . .
O7 O 0.5576(2) 0.33330(8) 0.3967(2) 0.0321(4) Uani 1 1 d . . . . .
O8 O 0.2547(2) 0.35306(8) 0.4678(2) 0.0350(4) Uani 1 1 d . . . . .
C8 C 0.3762(3) 0.58383(11) 0.3003(3) 0.0211(5) Uani 1 1 d . . . . .
H11 H 0.4062 0.5702 0.2084 0.025 Uiso 1 1 calc R U . . .
H12 H 0.3935 0.6266 0.3090 0.025 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 O4 1.5962(17) . ?
V1 O2 1.9613(16) . ?
V1 O6 2.0009(16) 3_666 ?
V1 O1 2.0030(15) 3_666 ?
V1 N1 2.1208(19) . ?
V1 O1 2.3067(16) . ?
V2 O5 1.6005(18) . ?
V2 O6 1.9809(17) . ?
V2 O2 1.9903(16) . ?
V2 O8 1.9997(19) . ?
V2 O7 2.0036(17) . ?
V2 O1 2.2880(15) 3_666 ?
N1 C7 1.485(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
C10 O2 1.425(3) . ?
C10 C7 1.526(3) . ?
C10 H13 0.9700 . ?
C10 H14 0.9700 . ?
C1 O8 1.263(3) . ?
C1 C2 1.389(4) . ?
C1 C5 1.495(4) . ?
C2 C3 1.371(4) . ?
C2 H4 0.9300 . ?
C3 O7 1.290(3) . ?
C3 C4 1.497(4) . ?
C4 H3 0.9600 . ?
C4 H1 0.9600 . ?
C4 H2 0.9600 . ?
C5 H7 0.9600 . ?
C5 H6 0.9600 . ?
C5 H5 0.9600 . ?
C6 O6 1.428(3) . ?
C6 H10 0.9600 . ?
C6 H9 0.9600 . ?
C6 H8 0.9600 . ?
C7 C9 1.525(3) . ?
C7 C8 1.532(3) . ?
C9 O3 1.406(3) . ?
C9 H16 0.9700 . ?
C9 H15 0.9700 . ?
O1 C8 1.431(3) . ?
O1 V1 2.0031(15) 3_666 ?
O1 V2 2.2880(15) 3_666 ?
O3 H3A 0.8200 . ?
O6 V1 2.0009(16) 3_666 ?
C8 H11 0.9700 . ?
C8 H12 0.9700 . ?

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
O4 V1 O2 104.12(8) . . ?
O4 V1 O6 97.80(8) . 3_666 ?
O2 V1 O6 158.02(7) . 3_666 ?
O4 V1 O1 108.31(8) . 3_666 ?
O2 V1 O1 79.36(6) . 3_666 ?
O6 V1 O1 95.50(7) 3_666 3_666 ?
O4 V1 N1 103.69(8) . . ?
O2 V1 N1 79.84(7) . . ?
O6 V1 N1 93.45(7) 3_666 . ?
O1 V1 N1 145.16(7) 3_666 . ?
O4 V1 O1 172.17(8) . . ?
O2 V1 O1 82.38(6) . . ?
O6 V1 O1 75.63(6) 3_666 . ?
O1 V1 O1 76.92(6) 3_666 . ?
N1 V1 O1 72.85(6) . . ?
O5 V2 O6 100.42(9) . . ?
O5 V2 O2 99.60(8) . . ?
O6 V2 O2 89.55(7) . . ?
O5 V2 O8 99.37(10) . . ?
O6 V2 O8 160.21(7) . . ?
O2 V2 O8 86.78(7) . . ?
O5 V2 O7 101.41(9) . . ?
O6 V2 O7 89.20(7) . . ?
O2 V2 O7 158.83(7) . . ?
O8 V2 O7 87.28(8) . . ?
O5 V2 O1 171.05(8) . 3_666 ?
O6 V2 O1 76.44(6) . 3_666 ?
O2 V2 O1 72.17(6) . 3_666 ?
O8 V2 O1 83.93(7) . 3_666 ?
O7 V2 O1 87.00(6) . 3_666 ?
C7 N1 V1 102.90(13) . . ?
C7 N1 H1A 111.2 . . ?
V1 N1 H1A 111.2 . . ?
C7 N1 H1B 111.2 . . ?
V1 N1 H1B 111.2 . . ?
H1A N1 H1B 109.1 . . ?
O2 C10 C7 108.58(18) . . ?
O2 C10 H13 110.0 . . ?
C7 C10 H13 110.0 . . ?
O2 C10 H14 110.0 . . ?
C7 C10 H14 110.0 . . ?
H13 C10 H14 108.4 . . ?
O8 C1 C2 124.2(3) . . ?
O8 C1 C5 115.7(3) . . ?
C2 C1 C5 120.1(3) . . ?
C3 C2 C1 124.9(3) . . ?
C3 C2 H4 117.6 . . ?
C1 C2 H4 117.6 . . ?
O7 C3 C2 125.0(3) . . ?
O7 C3 C4 115.0(3) . . ?
C2 C3 C4 120.0(3) . . ?
C3 C4 H3 109.5 . . ?
C3 C4 H1 109.5 . . ?
H3 C4 H1 109.5 . . ?
C3 C4 H2 109.5 . . ?
H3 C4 H2 109.5 . . ?
H1 C4 H2 109.5 . . ?
C1 C5 H7 109.5 . . ?
C1 C5 H6 109.5 . . ?
H7 C5 H6 109.5 . . ?
C1 C5 H5 109.5 . . ?
H7 C5 H5 109.5 . . ?
H6 C5 H5 109.5 . . ?
O6 C6 H10 109.5 . . ?
O6 C6 H9 109.5 . . ?
H10 C6 H9 109.5 . . ?
O6 C6 H8 109.5 . . ?
H10 C6 H8 109.5 . . ?
H9 C6 H8 109.5 . . ?
N1 C7 C9 110.89(19) . . ?
N1 C7 C10 105.73(18) . . ?
C9 C7 C10 111.28(19) . . ?
N1 C7 C8 106.85(17) . . ?
C9 C7 C8 111.00(19) . . ?
C10 C7 C8 110.88(19) . . ?
O3 C9 C7 109.4(2) . . ?
O3 C9 H16 109.8 . . ?
C7 C9 H16 109.8 . . ?
O3 C9 H15 109.8 . . ?
C7 C9 H15 109.8 . . ?
H16 C9 H15 108.2 . . ?
C8 O1 V1 123.55(14) . 3_666 ?
C8 O1 V2 124.08(13) . 3_666 ?
V1 O1 V2 97.04(6) 3_666 3_666 ?
C8 O1 V1 110.15(12) . . ?
V1 O1 V1 103.07(6) 3_666 . ?
V2 O1 V1 93.50(6) 3_666 . ?
C10 O2 V1 116.91(13) . . ?
C10 O2 V2 127.06(14) . . ?
V1 O2 V2 109.16(7) . . ?
C9 O3 H3A 109.5 . . ?
C6 O6 V2 119.08(18) . . ?
C6 O6 V1 120.09(18) . 3_666 ?
V2 O6 V1 114.39(8) . 3_666 ?
C3 O7 V2 126.49(18) . . ?
C1 O8 V2 128.57(19) . . ?
O1 C8 C7 110.12(18) . . ?
O1 C8 H11 109.6 . . ?
C7 C8 H11 109.6 . . ?
O1 C8 H12 109.6 . . ?
C7 C8 H12 109.6 . . ?
H11 C8 H12 108.2 . . ?

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
O8 C1 C2 C3 4.5(5) . . . . ?
C5 C1 C2 C3 -174.5(3) . . . . ?
C1 C2 C3 O7 -0.5(5) . . . . ?
C1 C2 C3 C4 177.1(3) . . . . ?
V1 N1 C7 C9 173.80(15) . . . . ?
V1 N1 C7 C10 53.06(18) . . . . ?
V1 N1 C7 C8 -65.12(18) . . . . ?
O2 C10 C7 N1 -46.3(2) . . . . ?
O2 C10 C7 C9 -166.81(19) . . . . ?
O2 C10 C7 C8 69.1(2) . . . . ?
N1 C7 C9 O3 178.23(19) . . . . ?
C10 C7 C9 O3 -64.4(3) . . . . ?
C8 C7 C9 O3 59.6(3) . . . . ?
C7 C10 O2 V1 15.4(2) . . . . ?
C7 C10 O2 V2 -132.17(17) . . . . ?
C2 C3 O7 V2 -15.7(4) . . . . ?
C4 C3 O7 V2 166.5(2) . . . . ?
C2 C1 O8 V2 8.6(4) . . . . ?
C5 C1 O8 V2 -172.4(3) . . . . ?
V1 O1 C8 C7 123.74(17) 3_666 . . . ?
V2 O1 C8 C7 -107.50(18) 3_666 . . . ?
V1 O1 C8 C7 1.6(2) . . . . ?
N1 C7 C8 O1 40.2(2) . . . . ?
C9 C7 C8 O1 161.22(19) . . . . ?
C10 C7 C8 O1 -74.5(2) . . . . ?

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 H1A O4 0.89 2.19 3.030(3) 157.3 3_566
N1 H1B O7 0.89 2.35 3.121(3) 145.7 3_666
C5 H6 O5 0.96 2.54 3.463(4) 161.3 4_566
C6 H10 O4 0.96 2.54 3.018(4) 110.8 3_666
O3 H3A O5 0.82 2.04 2.827(3) 160.1 3_565

_refine_diff_density_max         0.321
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.065

####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 2106171'
loop_
_audit_author_name
_audit_author_address
'jian zhou'
;Chongqing Normal University
China
;
_audit_update_record             
;
2021-08-29 deposited with the CCDC.	2021-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H75 N8 O46 V14, 2(H2 O)'
_chemical_formula_sum            'C35 H79 N8 O48 V14'
_chemical_formula_weight         2093.22

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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, -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                   18.8462(18)
_cell_length_b                   19.9961(18)
_cell_length_c                   18.8270(16)
_cell_angle_alpha                90
_cell_angle_beta                 99.460(4)
_cell_angle_gamma                90
_cell_volume                     6998.5(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    88077
_cell_measurement_theta_min      2.1911
_cell_measurement_theta_max      27.5120

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.987
_exptl_crystal_F_000             4204
_exptl_transmission_factor_min   0.777
_exptl_transmission_factor_max   0.853
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.084
_exptl_absorpt_coefficient_mu    1.884
_shelx_estimated_absorpt_T_min   0.702
_shelx_estimated_absorpt_T_max   0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            85127
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.992
_diffrn_reflns_theta_max         27.547
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8021
_reflns_number_gt                5971
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0214P)²+158.9745P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         8021
_refine_ls_number_parameters     508
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0727
_refine_ls_wR_factor_ref         0.1819
_refine_ls_wR_factor_gt          0.1519
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.000
_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 0.36450(6) 0.46026(6) 0.37935(6) 0.0336(3) Uani 1 1 d . . . . .
V2 V 0.27789(6) 0.35496(5) 0.47505(6) 0.0291(2) Uani 1 1 d . . . . .
V3 V 0.32648(7) 0.19667(6) 0.40398(6) 0.0355(3) Uani 1 1 d . . . . .
V4 V 0.23995(6) 0.34006(6) 0.32850(6) 0.0333(3) Uani 1 1 d . . . . .
V5 V 0.41602(6) 0.31372(6) 0.39323(7) 0.0359(3) Uani 1 1 d . . . . .
V6 V 0.23637(7) 0.50674(6) 0.46719(7) 0.0389(3) Uani 1 1 d . . . . .
V7 V 0.19874(7) 0.49455(6) 0.29547(7) 0.0418(3) Uani 1 1 d . . . . .
O1 O 0.4290(3) 0.2451(2) 0.4703(3) 0.0411(12) Uani 1 1 d . . . . .
O2 O 0.3938(3) 0.2296(2) 0.3344(3) 0.0396(11) Uani 1 1 d . . . . .
O3 O 0.5378(9) 0.0661(8) 0.4799(10) 0.162(7) Uani 0.723(15) 1 d D . P A 1
H3E H 0.5660 0.0348 0.4810 0.243 Uiso 0.723(15) 1 calc R U P A 1
O3B O 0.5860(17) 0.1296(17) 0.383(3) 0.162(7) Uani 0.277(15) 1 d D U P A 2
H3F H 0.6190 0.1030 0.3826 0.243 Uiso 0.277(15) 1 calc R U P A 2
O4 O 0.2828(3) 0.4352(2) 0.5335(2) 0.0359(10) Uani 1 1 d . . . . .
O5 O 0.3909(2) 0.3900(2) 0.4578(2) 0.0313(9) Uani 1 1 d . . . . .
O6 O 0.5014(4) 0.3298(4) 0.6522(4) 0.077(2) Uani 1 1 d . . . . .
H6C H 0.4953 0.2973 0.6770 0.116 Uiso 1 1 calc R U . . .
O7 O 0.3589(3) 0.3763(2) 0.3182(2) 0.0357(11) Uani 1 1 d . . . . .
O8 O 0.2158(3) 0.4075(2) 0.2524(2) 0.0398(11) Uani 1 1 d . . . . .
O9 O 0.3693(7) 0.2721(6) 0.1323(7) 0.071(4) Uani 0.563(16) 1 d . . P B 1
H9A H 0.4089 0.2871 0.1280 0.106 Uiso 0.563(16) 1 calc R U P B 1
O9B O 0.2586(10) 0.2973(8) 0.0753(8) 0.075(6) Uani 0.437(16) 1 d . . P B 2
H9B H 0.2381 0.3289 0.0529 0.112 Uiso 0.437(16) 1 calc R U P B 2
O10 O 0.2009(3) 0.5571(2) 0.3770(3) 0.0420(12) Uani 1 1 d . . . . .
O11 O 0.3361(3) 0.5263(2) 0.4502(3) 0.0376(11) Uani 1 1 d . . . . .
O12 O 0.3036(3) 0.5133(2) 0.3019(3) 0.0388(11) Uani 1 1 d . . . . .
O13 O 0.1122(3) 0.4549(3) 0.3301(3) 0.0533(14) Uani 1 1 d . . . . .
O14 O 0.1370(3) 0.4620(3) 0.4521(4) 0.0539(15) Uani 1 1 d . . . . .
O15 O 0.2227(4) 0.5624(3) 0.5238(3) 0.0596(16) Uani 1 1 d . . . . .
O16 O 0.1617(3) 0.5371(3) 0.2277(3) 0.0588(15) Uani 1 1 d . . . . .
O17 O 0.2628(3) 0.1653(3) 0.3481(3) 0.0496(13) Uani 1 1 d . . . . .
O18 O 0.4425(3) 0.4877(3) 0.3726(3) 0.0466(13) Uani 1 1 d . . . . .
O19 O 0.4970(3) 0.3303(3) 0.3833(3) 0.0564(15) Uani 1 1 d . . . . .
O20 O 0.1643(3) 0.3044(3) 0.3304(3) 0.0431(12) Uani 1 1 d . . . . .
O21 O 0.3043(2) 0.2918(2) 0.4045(2) 0.0298(9) Uani 1 1 d . . . . .
O22 O 0.2069(3) 0.3200(2) 0.5015(2) 0.0354(10) Uani 1 1 d . . . . .
O23 O 0.2541(2) 0.4183(2) 0.3943(2) 0.0293(9) Uani 1 1 d . . . . .
N1 N 0.3988(4) 0.1166(3) 0.4163(4) 0.0571(19) Uani 1 1 d . . . . .
H1A H 0.4018 0.0979 0.4596 0.069 Uiso 1 1 calc R U . . .
H1B H 0.3865 0.0856 0.3826 0.069 Uiso 1 1 calc R U . . .
N2 N 0.3550(3) 0.3238(3) 0.5631(3) 0.0380(13) Uani 1 1 d . . . . .
H2C H 0.3339 0.3076 0.5985 0.046 Uiso 1 1 calc R U . . .
H2D H 0.3840 0.2927 0.5498 0.046 Uiso 1 1 calc R U . . .
N3 N 0.2752(3) 0.2902(3) 0.2404(3) 0.0405(14) Uani 1 1 d . . . . .
H3C H 0.3100 0.2611 0.2559 0.049 Uiso 1 1 calc R U . . .
H3D H 0.2389 0.2687 0.2136 0.049 Uiso 1 1 calc R U . . .
N4 N 0.3317(4) 0.6921(4) 0.3559(4) 0.0563(18) Uani 1 1 d D . . . .
H4A H 0.338(5) 0.721(4) 0.393(3) 0.068 Uiso 1 1 d D U . . .
H4B H 0.375(2) 0.700(5) 0.345(5) 0.068 Uiso 1 1 d D U . . .
C1 C 0.4670(5) 0.1501(4) 0.4075(6) 0.060(2) Uani 1 1 d . . . . .
C2 C 0.4851(5) 0.1987(5) 0.4688(5) 0.060(2) Uani 1 1 d . . . . .
H2A H 0.4937 0.1744 0.5139 0.072 Uiso 1 1 calc R U . . .
H2B H 0.5288 0.2226 0.4637 0.072 Uiso 1 1 calc R U . . .
C3 C 0.4509(5) 0.1836(4) 0.3344(5) 0.056(2) Uani 1 1 d . . . . .
H3A H 0.4934 0.2069 0.3244 0.067 Uiso 1 1 calc R U . . .
H3B H 0.4376 0.1502 0.2972 0.067 Uiso 1 1 calc R U . . .
C4 C 0.5280(8) 0.0967(7) 0.4094(9) 0.108(5) Uani 1 1 d D . . . .
H4C H 0.5143 0.0633 0.3724 0.130 Uiso 0.723(15) 1 calc R U P A 1
H4D H 0.5722 0.1178 0.4011 0.130 Uiso 0.723(15) 1 calc R U P A 1
H4E H 0.5434 0.0808 0.4582 0.130 Uiso 0.277(15) 1 calc R U P A 2
H4F H 0.5111 0.0589 0.3790 0.130 Uiso 0.277(15) 1 calc R U P A 2
C5 C 0.3955(4) 0.3864(4) 0.5859(4) 0.0413(16) Uani 1 1 d . . . . .
C6 C 0.3403(4) 0.4404(4) 0.5929(4) 0.0397(16) Uani 1 1 d . . . . .
H6A H 0.3219 0.4348 0.6378 0.048 Uiso 1 1 calc R U . . .
H6B H 0.3625 0.4842 0.5932 0.048 Uiso 1 1 calc R U . . .
C7 C 0.4372(4) 0.4025(4) 0.5251(4) 0.0425(17) Uani 1 1 d . . . . .
H7A H 0.4522 0.4490 0.5278 0.051 Uiso 1 1 calc R U . . .
H7B H 0.4798 0.3746 0.5290 0.051 Uiso 1 1 calc R U . . .
C8 C 0.4472(5) 0.3784(5) 0.6575(4) 0.056(2) Uani 1 1 d . . . . .
H8A H 0.4699 0.4211 0.6712 0.067 Uiso 1 1 calc R U . . .
H8B H 0.4202 0.3651 0.6948 0.067 Uiso 1 1 calc R U . . .
C9 C 0.3022(5) 0.3456(4) 0.1989(4) 0.0463(18) Uani 1 1 d . . . . .
C10 C 0.3692(4) 0.3741(4) 0.2447(4) 0.0447(18) Uani 1 1 d . . . . .
H10A H 0.4104 0.3464 0.2403 0.054 Uiso 1 1 calc R U . . .
H10B H 0.3783 0.4188 0.2283 0.054 Uiso 1 1 calc R U . . .
C11 C 0.2420(5) 0.3972(4) 0.1865(4) 0.050(2) Uani 1 1 d . . . . .
H11A H 0.2599 0.4390 0.1702 0.061 Uiso 1 1 calc R U . . .
H11B H 0.2034 0.3814 0.1498 0.061 Uiso 1 1 calc R U . . .
C12 C 0.3211(6) 0.3221(5) 0.1263(5) 0.061(2) Uani 1 1 d . . . . .
H12A H 0.2773 0.3074 0.0957 0.073 Uiso 0.563(16) 1 calc R U P B 1
H12B H 0.3399 0.3597 0.1028 0.073 Uiso 0.563(16) 1 calc R U P B 1
H12C H 0.3427 0.3590 0.1042 0.073 Uiso 0.437(16) 1 calc R U P B 2
H12D H 0.3566 0.2867 0.1352 0.073 Uiso 0.437(16) 1 calc R U P B 2
C13 C 0.3101(4) 0.6216(4) 0.3663(4) 0.0427(17) Uani 1 1 d . . . . .
C14 C 0.2294(4) 0.6229(3) 0.3694(4) 0.0459(18) Uani 1 1 d . . . . .
H14A H 0.2211 0.6503 0.4097 0.055 Uiso 1 1 calc R U . . .
H14B H 0.2041 0.6432 0.3257 0.055 Uiso 1 1 calc R U . . .
C15 C 0.3523(4) 0.5944(3) 0.4353(4) 0.0427(17) Uani 1 1 d . . . . .
H15A H 0.4032 0.5978 0.4328 0.051 Uiso 1 1 calc R U . . .
H15B H 0.3430 0.6221 0.4750 0.051 Uiso 1 1 calc R U . . .
C16 C 0.3234(4) 0.5827(3) 0.3004(4) 0.0406(16) Uani 1 1 d . . . . .
H16A H 0.2964 0.6033 0.2577 0.049 Uiso 1 1 calc R U . . .
H16B H 0.3741 0.5857 0.2968 0.049 Uiso 1 1 calc R U . . .
C17 C 0.0988(5) 0.4468(4) 0.3936(7) 0.063(3) Uani 1 1 d D . . . .
H17A H 0.0549 0.4269 0.3969 0.075 Uiso 1 1 calc R U . C 1
O2W O -0.049(2) 0.379(2) 0.305(2) 0.30(2) Uani 0.5 1 d . U P D 1
H2E H -0.0207 0.4026 0.2878 0.449 Uiso 0.5 1 d R U P D 1
H2F H -0.0375 0.3393 0.3108 0.449 Uiso 0.5 1 d R U P D 1
C18 C 0.0200(13) 0.4181(19) 0.3824(18) 0.145(14) Uani 0.5 1 d D . P E 2
H18A H -0.0029 0.4311 0.4222 0.218 Uiso 0.5 1 calc R U P E 2
H18B H 0.0216 0.3702 0.3796 0.218 Uiso 0.5 1 calc R U P E 2
H18C H -0.0067 0.4357 0.3385 0.218 Uiso 0.5 1 calc R U P E 2
O1W O 0.4763(9) 0.2254(10) 0.7360(16) 0.132(8) Uani 0.5 1 d . . P . .
H1C H 0.4499 0.2110 0.7630 0.199 Uiso 0.5 1 d R U P . .
H1D H 0.4733 0.2066 0.6969 0.199 Uiso 0.5 1 d R U P . .


_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 O18 1.594(5) . ?
V1 O12 2.005(5) . ?
V1 O11 2.011(5) . ?
V1 O7 2.028(5) . ?
V1 O5 2.040(4) . ?
V1 O23 2.304(4) . ?
V1 V5 3.0845(16) . ?
V2 O22 1.657(4) . ?
V2 O4 1.940(5) . ?
V2 O21 1.955(4) . ?
V2 O23 1.973(4) . ?
V2 N2 2.111(6) . ?
V2 O5 2.315(4) . ?
V2 V4 2.7503(16) . ?
V3 O17 1.588(6) . ?
V3 O21 1.947(4) . ?
V3 O22 2.011(4) 7_556 ?
V3 O2 2.075(4) . ?
V3 N1 2.091(6) . ?
V3 O1 2.331(6) . ?
V3 V5 2.9119(17) . ?
V4 O20 1.599(5) . ?
V4 O8 1.966(5) . ?
V4 O21 1.970(5) . ?
V4 O23 1.986(4) . ?
V4 N3 2.132(6) . ?
V4 O7 2.394(5) . ?
V5 O19 1.602(5) . ?
V5 O1 1.982(5) . ?
V5 O2 2.020(5) . ?
V5 O5 2.053(5) . ?
V5 O7 2.055(5) . ?
V5 O21 2.196(4) . ?
V6 O15 1.591(5) . ?
V6 O10 1.994(5) . ?
V6 O11 1.997(5) . ?
V6 O4 2.003(5) . ?
V6 O14 2.053(7) . ?
V6 O23 2.297(4) . ?
V7 O16 1.595(6) . ?
V7 O8 1.970(5) . ?
V7 O10 1.975(5) . ?
V7 O12 1.996(5) . ?
V7 O13 2.017(6) . ?
O1 C2 1.410(9) . ?
O2 C3 1.415(9) . ?
O3 C4 1.445(18) . ?
O3 H3E 0.8200 . ?
O3B C4 1.43(2) . ?
O3B H3F 0.8200 . ?
O4 C6 1.427(8) . ?
O5 C7 1.438(8) . ?
O6 C8 1.424(11) . ?
O6 H6C 0.8200 . ?
O7 C10 1.429(7) . ?
O8 C11 1.423(8) . ?
O9 C12 1.344(14) . ?
O9 H9A 0.8200 . ?
O9B C12 1.477(19) . ?
O9B H9B 0.8200 . ?
O10 C14 1.436(8) . ?
O11 C15 1.433(8) . ?
O12 C16 1.437(8) . ?
O13 C17 1.271(11) . ?
O14 C17 1.251(12) . ?
O22 V3 2.011(4) 7_556 ?
N1 C1 1.482(11) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 C5 1.492(9) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N3 C9 1.494(9) . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N4 C13 1.490(9) . ?
N4 H4A 0.894(10) . ?
N4 H4B 0.891(10) . ?
C1 C2 1.504(14) . ?
C1 C3 1.516(13) . ?
C1 C4 1.565(12) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C4 H4E 0.9700 . ?
C4 H4F 0.9700 . ?
C5 C6 1.521(10) . ?
C5 C7 1.527(9) . ?
C5 C8 1.535(11) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.518(12) . ?
C9 C11 1.523(11) . ?
C9 C12 1.542(10) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C12 H12D 0.9700 . ?
C13 C15 1.509(11) . ?
C13 C16 1.520(10) . ?
C13 C14 1.531(11) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.573(17) . ?
C17 H17A 0.9300 . ?
O2W H2E 0.8200 . ?
O2W H2F 0.8200 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
O1W O1W 0.96(3) 2_656 ?
O1W H1C 0.8200 . ?
O1W H1D 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
O18 V1 O12 100.6(2) . . ?
O18 V1 O11 100.2(2) . . ?
O12 V1 O11 87.3(2) . . ?
O18 V1 O7 101.6(2) . . ?
O12 V1 O7 93.1(2) . . ?
O11 V1 O7 157.7(2) . . ?
O18 V1 O5 100.2(2) . . ?
O12 V1 O5 159.0(2) . . ?
O11 V1 O5 91.83(18) . . ?
O7 V1 O5 79.90(18) . . ?
O18 V1 O23 177.3(2) . . ?
O12 V1 O23 82.02(18) . . ?
O11 V1 O23 79.30(18) . . ?
O7 V1 O23 78.70(17) . . ?
O5 V1 O23 77.21(16) . . ?
O18 V1 V5 93.0(2) . . ?
O12 V1 V5 134.34(15) . . ?
O11 V1 V5 132.99(14) . . ?
O7 V1 V5 41.26(14) . . ?
O5 V1 V5 41.25(13) . . ?
O23 V1 V5 85.51(11) . . ?
O22 V2 O4 98.3(2) . . ?
O22 V2 O21 103.8(2) . . ?
O4 V2 O21 157.9(2) . . ?
O22 V2 O23 114.2(2) . . ?
O4 V2 O23 83.68(19) . . ?
O21 V2 O23 86.71(18) . . ?
O22 V2 N2 97.2(2) . . ?
O4 V2 N2 80.6(2) . . ?
O21 V2 N2 97.1(2) . . ?
O23 V2 N2 146.6(2) . . ?
O22 V2 O5 167.6(2) . . ?
O4 V2 O5 82.55(18) . . ?
O21 V2 O5 75.97(17) . . ?
O23 V2 O5 78.20(17) . . ?
N2 V2 O5 70.68(19) . . ?
O22 V2 V4 99.55(18) . . ?
O4 V2 V4 129.73(14) . . ?
O21 V2 V4 45.75(13) . . ?
O23 V2 V4 46.18(13) . . ?
N2 V2 V4 141.98(16) . . ?
O5 V2 V4 89.15(11) . . ?
O17 V3 O21 104.4(2) . . ?
O17 V3 O22 102.0(2) . 7_556 ?
O21 V3 O22 93.31(18) . 7_556 ?
O17 V3 O2 100.4(2) . . ?
O21 V3 O2 81.26(18) . . ?
O22 V3 O2 157.5(2) 7_556 . ?
O17 V3 N1 100.3(3) . . ?
O21 V3 N1 152.1(3) . . ?
O22 V3 N1 93.9(2) 7_556 . ?
O2 V3 N1 81.8(2) . . ?
O17 V3 O1 170.9(2) . . ?
O21 V3 O1 75.60(18) . . ?
O22 V3 O1 86.97(19) 7_556 . ?
O2 V3 O1 70.56(19) . . ?
N1 V3 O1 77.9(3) . . ?
O17 V3 V5 130.9(2) . . ?
O21 V3 V5 48.93(13) . . ?
O22 V3 V5 117.63(15) 7_556 . ?
O2 V3 V5 43.92(14) . . ?
N1 V3 V5 104.4(2) . . ?
O1 V3 V5 42.66(12) . . ?
O20 V4 O8 102.8(2) . . ?
O20 V4 O21 102.1(2) . . ?
O8 V4 O21 155.1(2) . . ?
O20 V4 O23 111.5(2) . . ?
O8 V4 O23 84.58(19) . . ?
O21 V4 O23 85.97(18) . . ?
O20 V4 N3 101.6(3) . . ?
O8 V4 N3 79.5(2) . . ?
O21 V4 N3 95.9(2) . . ?
O23 V4 N3 145.7(2) . . ?
O20 V4 O7 170.6(2) . . ?
O8 V4 O7 80.84(19) . . ?
O21 V4 O7 74.63(17) . . ?
O23 V4 O7 77.33(17) . . ?
N3 V4 O7 70.3(2) . . ?
O20 V4 V2 96.43(19) . . ?
O8 V4 V2 130.39(15) . . ?
O21 V4 V2 45.31(12) . . ?
O23 V4 V2 45.81(12) . . ?
N3 V4 V2 140.18(19) . . ?
O7 V4 V2 87.49(12) . . ?
O19 V5 O1 102.9(3) . . ?
O19 V5 O2 102.9(3) . . ?
O1 V5 O2 79.3(2) . . ?
O19 V5 O5 103.4(3) . . ?
O1 V5 O5 95.39(19) . . ?
O2 V5 O5 153.66(19) . . ?
O19 V5 O7 101.3(3) . . ?
O1 V5 O7 155.8(2) . . ?
O2 V5 O7 95.3(2) . . ?
O5 V5 O7 78.97(18) . . ?
O19 V5 O21 178.8(3) . . ?
O1 V5 O21 78.18(18) . . ?
O2 V5 O21 76.77(17) . . ?
O5 V5 O21 76.89(17) . . ?
O7 V5 O21 77.66(17) . . ?
O19 V5 V3 138.4(2) . . ?
O1 V5 V3 52.82(16) . . ?
O2 V5 V3 45.45(13) . . ?
O5 V5 V3 111.31(13) . . ?
O7 V5 V3 107.07(14) . . ?
O21 V5 V3 41.96(11) . . ?
O19 V5 V1 94.9(2) . . ?
O1 V5 V1 135.95(15) . . ?
O2 V5 V1 135.31(16) . . ?
O5 V5 V1 40.93(12) . . ?
O7 V5 V1 40.62(13) . . ?
O21 V5 V1 84.53(12) . . ?
V3 V5 V1 126.27(5) . . ?
O15 V6 O10 98.6(3) . . ?
O15 V6 O11 103.3(3) . . ?
O10 V6 O11 87.6(2) . . ?
O15 V6 O4 100.6(3) . . ?
O10 V6 O4 160.60(19) . . ?
O11 V6 O4 85.0(2) . . ?
O15 V6 O14 98.8(3) . . ?
O10 V6 O14 86.1(2) . . ?
O11 V6 O14 157.7(2) . . ?
O4 V6 O14 94.0(2) . . ?
O15 V6 O23 174.0(2) . . ?
O10 V6 O23 86.64(18) . . ?
O11 V6 O23 79.76(18) . . ?
O4 V6 O23 74.41(17) . . ?
O14 V6 O23 78.5(2) . . ?
O16 V7 O8 102.8(3) . . ?
O16 V7 O10 103.5(3) . . ?
O8 V7 O10 153.7(2) . . ?
O16 V7 O12 104.3(3) . . ?
O8 V7 O12 88.0(2) . . ?
O10 V7 O12 86.6(2) . . ?
O16 V7 O13 101.4(3) . . ?
O8 V7 O13 88.9(2) . . ?
O10 V7 O13 84.9(2) . . ?
O12 V7 O13 154.2(2) . . ?
C2 O1 V5 116.3(5) . . ?
C2 O1 V3 105.9(5) . . ?
V5 O1 V3 84.52(19) . . ?
C3 O2 V5 116.9(5) . . ?
C3 O2 V3 109.8(4) . . ?
V5 O2 V3 90.63(18) . . ?
C4 O3 H3E 109.5 . . ?
C4 O3B H3F 109.5 . . ?
C6 O4 V2 117.7(4) . . ?
C6 O4 V6 129.4(4) . . ?
V2 O4 V6 105.2(2) . . ?
C7 O5 V1 124.0(4) . . ?
C7 O5 V5 119.0(4) . . ?
V1 O5 V5 97.82(19) . . ?
C7 O5 V2 111.6(4) . . ?
V1 O5 V2 100.92(18) . . ?
V5 O5 V2 99.52(18) . . ?
C8 O6 H6C 109.5 . . ?
C10 O7 V1 124.9(4) . . ?
C10 O7 V5 120.5(4) . . ?
V1 O7 V5 98.1(2) . . ?
C10 O7 V4 110.3(4) . . ?
V1 O7 V4 99.59(18) . . ?
V5 O7 V4 98.70(17) . . ?
C11 O8 V4 117.7(4) . . ?
C11 O8 V7 126.2(5) . . ?
V4 O8 V7 109.9(2) . . ?
C12 O9 H9A 109.5 . . ?
C12 O9B H9B 109.5 . . ?
C14 O10 V7 117.6(4) . . ?
C14 O10 V6 118.0(5) . . ?
V7 O10 V6 107.6(2) . . ?
C15 O11 V6 117.0(4) . . ?
C15 O11 V1 113.9(4) . . ?
V6 O11 V1 109.7(2) . . ?
C16 O12 V7 116.0(4) . . ?
C16 O12 V1 113.9(4) . . ?
V7 O12 V1 112.8(2) . . ?
C17 O13 V7 130.5(6) . . ?
C17 O14 V6 127.4(5) . . ?
V3 O21 V2 135.5(2) . . ?
V3 O21 V4 125.6(2) . . ?
V2 O21 V4 88.95(17) . . ?
V3 O21 V5 89.11(17) . . ?
V2 O21 V5 107.0(2) . . ?
V4 O21 V5 108.47(19) . . ?
V2 O22 V3 136.2(3) . 7_556 ?
V2 O23 V4 88.01(17) . . ?
V2 O23 V6 94.04(17) . . ?
V4 O23 V6 164.1(2) . . ?
V2 O23 V1 103.42(19) . . ?
V4 O23 V1 104.01(18) . . ?
V6 O23 V1 90.87(16) . . ?
C1 N1 V3 101.7(5) . . ?
C1 N1 H1A 111.4 . . ?
V3 N1 H1A 111.4 . . ?
C1 N1 H1B 111.4 . . ?
V3 N1 H1B 111.4 . . ?
H1A N1 H1B 109.3 . . ?
C5 N2 V2 103.4(4) . . ?
C5 N2 H2C 111.1 . . ?
V2 N2 H2C 111.1 . . ?
C5 N2 H2D 111.1 . . ?
V2 N2 H2D 111.1 . . ?
H2C N2 H2D 109.0 . . ?
C9 N3 V4 103.7(4) . . ?
C9 N3 H3C 111.0 . . ?
V4 N3 H3C 111.0 . . ?
C9 N3 H3D 111.0 . . ?
V4 N3 H3D 111.0 . . ?
H3C N3 H3D 109.0 . . ?
C13 N4 H4A 121(6) . . ?
C13 N4 H4B 118(6) . . ?
H4A N4 H4B 93(8) . . ?
N1 C1 C2 107.4(7) . . ?
N1 C1 C3 104.7(8) . . ?
C2 C1 C3 113.4(7) . . ?
N1 C1 C4 109.6(8) . . ?
C2 C1 C4 110.6(10) . . ?
C3 C1 C4 111.0(8) . . ?
O1 C2 C1 111.4(7) . . ?
O1 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
O1 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
O2 C3 C1 109.0(6) . . ?
O2 C3 H3A 109.9 . . ?
C1 C3 H3A 109.9 . . ?
O2 C3 H3B 109.9 . . ?
C1 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
O3B C4 C1 106.2(16) . . ?
O3 C4 C1 107.0(10) . . ?
O3 C4 H4C 110.3 . . ?
C1 C4 H4C 110.3 . . ?
O3 C4 H4D 110.3 . . ?
C1 C4 H4D 110.3 . . ?
H4C C4 H4D 108.6 . . ?
O3B C4 H4E 110.5 . . ?
C1 C4 H4E 110.5 . . ?
O3B C4 H4F 110.5 . . ?
C1 C4 H4F 110.5 . . ?
H4E C4 H4F 108.7 . . ?
N2 C5 C6 107.2(6) . . ?
N2 C5 C7 105.2(6) . . ?
C6 C5 C7 111.1(6) . . ?
N2 C5 C8 112.7(6) . . ?
C6 C5 C8 110.1(6) . . ?
C7 C5 C8 110.5(6) . . ?
O4 C6 C5 108.8(6) . . ?
O4 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
O4 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
O5 C7 C5 108.2(6) . . ?
O5 C7 H7A 110.1 . . ?
C5 C7 H7A 110.1 . . ?
O5 C7 H7B 110.1 . . ?
C5 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
O6 C8 C5 111.7(7) . . ?
O6 C8 H8A 109.3 . . ?
C5 C8 H8A 109.3 . . ?
O6 C8 H8B 109.3 . . ?
C5 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
N3 C9 C10 107.8(6) . . ?
N3 C9 C11 105.8(6) . . ?
C10 C9 C11 111.3(7) . . ?
N3 C9 C12 112.6(7) . . ?
C10 C9 C12 109.1(7) . . ?
C11 C9 C12 110.2(7) . . ?
O7 C10 C9 109.2(6) . . ?
O7 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
O7 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
O8 C11 C9 108.7(6) . . ?
O8 C11 H11A 109.9 . . ?
C9 C11 H11A 109.9 . . ?
O8 C11 H11B 109.9 . . ?
C9 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
O9 C12 C9 113.9(9) . . ?
O9B C12 C9 113.9(9) . . ?
O9 C12 H12A 108.8 . . ?
C9 C12 H12A 108.8 . . ?
O9 C12 H12B 108.8 . . ?
C9 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
O9B C12 H12C 108.8 . . ?
C9 C12 H12C 108.8 . . ?
O9B C12 H12D 108.8 . . ?
C9 C12 H12D 108.8 . . ?
H12C C12 H12D 107.7 . . ?
N4 C13 C15 109.8(6) . . ?
N4 C13 C16 106.9(6) . . ?
C15 C13 C16 112.5(6) . . ?
N4 C13 C14 106.5(6) . . ?
C15 C13 C14 111.1(6) . . ?
C16 C13 C14 109.8(6) . . ?
O10 C14 C13 112.3(6) . . ?
O10 C14 H14A 109.2 . . ?
C13 C14 H14A 109.2 . . ?
O10 C14 H14B 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
O11 C15 C13 114.4(6) . . ?
O11 C15 H15A 108.7 . . ?
C13 C15 H15A 108.7 . . ?
O11 C15 H15B 108.7 . . ?
C13 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
O12 C16 C13 113.6(5) . . ?
O12 C16 H16A 108.9 . . ?
C13 C16 H16A 108.9 . . ?
O12 C16 H16B 108.9 . . ?
C13 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
O14 C17 O13 128.6(8) . . ?
O14 C17 C18 126.9(15) . . ?
O13 C17 C18 104.4(15) . . ?
O14 C17 H17A 115.7 . . ?
O13 C17 H17A 115.7 . . ?
H2E O2W H2F 115.9 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O1W O1W H1C 105.3 2_656 . ?
O1W O1W H1D 114.4 2_656 . ?
H1C O1W H1D 115.9 . . ?

_refine_diff_density_max         1.053
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.159

####################################################################### 
# 
# 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_3b
_database_code_depnum_ccdc_archive 'CCDC 2106172'
loop_
_audit_author_name
_audit_author_address
'jian zhou'
;Chongqing Normal University
China
;
_audit_update_record             
;
2021-08-29 deposited with the CCDC.	2021-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H42 N2 O16 V4'
_chemical_formula_sum            'C22 H42 N2 O16 V4'
_chemical_formula_weight         794.34

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   8.545(3)
_cell_length_b                   12.114(5)
_cell_length_c                   16.617(6)
_cell_angle_alpha                76.391(18)
_cell_angle_beta                 84.090(17)
_cell_angle_gamma                71.427(15)
_cell_volume                     1583.9(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    43719
_cell_measurement_theta_min      2.516
_cell_measurement_theta_max      25.096

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   0.755
_exptl_transmission_factor_max   0.928
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.217
_shelx_estimated_absorpt_T_min   0.767
_shelx_estimated_absorpt_T_max   0.931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43719
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.516
_diffrn_reflns_theta_max         25.096
_diffrn_reflns_theta_full        25.096
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5636
_reflns_number_gt                4768
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0298P)²+1.7532P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5636
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0827
_refine_ls_wR_factor_gt          0.0767
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_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 0.51746(5) 0.53556(4) 0.58862(3) 0.01822(11) Uani 1 1 d . . . . .
V2 V 0.32737(5) 0.74190(4) 0.42587(3) 0.02395(12) Uani 1 1 d . . . . .
V4 V 0.82609(6) 0.73338(4) 0.02712(3) 0.02545(12) Uani 1 1 d . . . . .
V3 V 1.03776(5) 0.55385(4) -0.10015(3) 0.01886(11) Uani 1 1 d . . . . .
O1 O 0.33597(19) 0.54888(15) 0.49393(10) 0.0180(4) Uani 1 1 d . . . . .
O2 O 0.5006(2) 0.37392(16) 0.63056(11) 0.0221(4) Uani 1 1 d . . . . .
O3 O -0.0699(2) 0.59857(18) 0.65765(12) 0.0312(5) Uani 1 1 d . . . . .
H3C H -0.1620 0.5930 0.6542 0.047 Uiso 1 1 calc R U . . .
O4 O 0.6430(2) 0.54624(19) 0.64962(11) 0.0299(4) Uani 1 1 d . . . . .
O5 O 0.3591(3) 0.86336(19) 0.37841(13) 0.0390(5) Uani 1 1 d . . . . .
O6 O 0.1541(2) 0.74323(18) 0.35170(12) 0.0327(5) Uani 1 1 d . . . . .
O7 O 0.1425(2) 0.79118(18) 0.50680(12) 0.0317(5) Uani 1 1 d . . . . .
O8 O 0.4817(2) 0.69880(16) 0.51858(11) 0.0251(4) Uani 1 1 d . . . . .
O9 O 1.0183(2) 0.39852(16) -0.10593(11) 0.0221(4) Uani 1 1 d . . . . .
O11 O 0.4609(3) 0.6401(2) -0.15777(15) 0.0440(6) Uani 1 1 d . . . . .
H10D H 0.3670 0.6387 -0.1623 0.066 Uiso 1 1 calc R U . . .
O10 O 0.83628(19) 0.55080(16) 0.00174(10) 0.0192(4) Uani 1 1 d . . . . .
O12 O 1.1714(2) 0.57535(18) -0.17342(11) 0.0275(4) Uani 1 1 d . . . . .
O13 O 0.9987(2) 0.70581(17) -0.06361(11) 0.0270(4) Uani 1 1 d . . . . .
O14 O 0.8571(3) 0.84534(19) 0.04893(14) 0.0411(5) Uani 1 1 d . . . . .
O15 O 0.6345(2) 0.72162(18) 0.10610(12) 0.0320(5) Uani 1 1 d . . . . .
O16 O 0.6615(2) 0.80552(19) -0.06192(12) 0.0341(5) Uani 1 1 d . . . . .
N1 N 0.2771(2) 0.57606(19) 0.64666(13) 0.0201(5) Uani 1 1 d . . . . .
H1C H 0.2826 0.5678 0.7010 0.024 Uiso 1 1 calc R U . . .
H1D H 0.2154 0.6497 0.6251 0.024 Uiso 1 1 calc R U . . .
N2 N 0.8090(3) 0.6093(2) -0.15947(13) 0.0225(5) Uani 1 1 d . . . . .
H2A H 0.7476 0.6811 -0.1522 0.027 Uiso 1 1 calc R U . . .
H2B H 0.8241 0.6108 -0.2135 0.027 Uiso 1 1 calc R U . . .
C1 C 0.0475(3) 0.4830(2) 0.67190(17) 0.0246(6) Uani 1 1 d . . . . .
H1A H 0.0052 0.4289 0.6524 0.029 Uiso 1 1 calc R U . . .
H1B H 0.0642 0.4536 0.7309 0.029 Uiso 1 1 calc R U . . .
C2 C 0.2120(3) 0.4854(2) 0.62742(15) 0.0197(5) Uani 1 1 d . . . . .
C3 C 0.1967(3) 0.5152(2) 0.53336(15) 0.0214(6) Uani 1 1 d . . . . .
H3A H 0.1903 0.4463 0.5152 0.026 Uiso 1 1 calc R U . . .
H3B H 0.0963 0.5801 0.5178 0.026 Uiso 1 1 calc R U . . .
C4 C 0.3410(3) 0.3647(2) 0.65689(17) 0.0255(6) Uani 1 1 d . . . . .
H4A H 0.3347 0.3413 0.7168 0.031 Uiso 1 1 calc R U . . .
H4B H 0.3196 0.3044 0.6340 0.031 Uiso 1 1 calc R U . . .
C5 C -0.1134(4) 0.8907(3) 0.5609(2) 0.0433(8) Uani 1 1 d . . . . .
H5A H -0.2254 0.9291 0.5440 0.065 Uiso 1 1 calc R U . . .
H5B H -0.1099 0.8257 0.6074 0.065 Uiso 1 1 calc R U . . .
H5C H -0.0712 0.9472 0.5763 0.065 Uiso 1 1 calc R U . . .
C6 C -0.0105(3) 0.8445(2) 0.49104(19) 0.0303(7) Uani 1 1 d . . . . .
C7 C -0.0780(4) 0.8597(3) 0.4157(2) 0.0378(8) Uani 1 1 d . . . . .
H7A H -0.1875 0.9065 0.4083 0.045 Uiso 1 1 calc R U . . .
C8 C 0.0057(3) 0.8099(3) 0.35004(19) 0.0308(7) Uani 1 1 d . . . . .
C9 C -0.0821(4) 0.8353(3) 0.2709(2) 0.0420(8) Uani 1 1 d . . . . .
H9A H -0.1929 0.8862 0.2762 0.063 Uiso 1 1 calc R U . . .
H9B H -0.0246 0.8740 0.2262 0.063 Uiso 1 1 calc R U . . .
H9C H -0.0850 0.7617 0.2597 0.063 Uiso 1 1 calc R U . . .
C10 C 0.4333(6) 0.8312(4) 0.6155(3) 0.0720(13) Uani 1 1 d . . . . .
H10A H 0.4730 0.8900 0.6292 0.108 Uiso 1 1 calc R U . . .
H10B H 0.3192 0.8660 0.6014 0.108 Uiso 1 1 calc R U . . .
H10C H 0.4439 0.7656 0.6623 0.108 Uiso 1 1 calc R U . . .
C11 C 0.5334(4) 0.7868(3) 0.5427(2) 0.0428(8) Uani 1 1 d . . . . .
H11A H 0.5241 0.8538 0.4960 0.051 Uiso 1 1 calc R U . . .
H11B H 0.6488 0.7534 0.5569 0.051 Uiso 1 1 calc R U . . .
C12 C 0.5734(3) 0.5251(3) -0.15535(17) 0.0295(6) Uani 1 1 d . . . . .
H12A H 0.5971 0.5110 -0.2111 0.035 Uiso 1 1 calc R U . . .
H12B H 0.5255 0.4654 -0.1230 0.035 Uiso 1 1 calc R U . . .
C13 C 0.7318(3) 0.5157(2) -0.11668(15) 0.0219(6) Uani 1 1 d . . . . .
C14 C 0.8603(3) 0.3967(3) -0.12321(17) 0.0250(6) Uani 1 1 d . . . . .
H14A H 0.8317 0.3323 -0.0841 0.030 Uiso 1 1 calc R U . . .
H14B H 0.8619 0.3830 -0.1785 0.030 Uiso 1 1 calc R U . . .
C15 C 0.6997(3) 0.5287(3) -0.02683(15) 0.0221(6) Uani 1 1 d . . . . .
H15A H 0.6002 0.5942 -0.0227 0.026 Uiso 1 1 calc R U . . .
H15B H 0.6833 0.4563 0.0076 0.026 Uiso 1 1 calc R U . . .
C16 C 0.4232(4) 0.9317(3) -0.1323(2) 0.0482(9) Uani 1 1 d . . . . .
H16A H 0.3098 0.9716 -0.1200 0.072 Uiso 1 1 calc R U . . .
H16B H 0.4767 0.9896 -0.1600 0.072 Uiso 1 1 calc R U . . .
H16C H 0.4283 0.8781 -0.1675 0.072 Uiso 1 1 calc R U . . .
C17 C 0.5085(4) 0.8629(3) -0.05347(19) 0.0321(7) Uani 1 1 d . . . . .
C18 C 0.4227(4) 0.8619(3) 0.0220(2) 0.0401(8) Uani 1 1 d . . . . .
H18A H 0.3148 0.9123 0.0226 0.048 Uiso 1 1 calc R U . . .
C19 C 0.4869(3) 0.7907(3) 0.09671(18) 0.0312(7) Uani 1 1 d . . . . .
C20 C 0.3777(4) 0.7930(3) 0.1733(2) 0.0433(8) Uani 1 1 d . . . . .
H20A H 0.2699 0.8475 0.1595 0.065 Uiso 1 1 calc R U . . .
H20B H 0.3690 0.7145 0.1962 0.065 Uiso 1 1 calc R U . . .
H20C H 0.4241 0.8184 0.2133 0.065 Uiso 1 1 calc R U . . .
C21 C 0.9614(7) 0.8574(4) -0.1943(3) 0.0959(18) Uani 1 1 d . . . . .
H21A H 1.0001 0.9221 -0.2244 0.144 Uiso 1 1 calc R U . . .
H21B H 0.9839 0.7975 -0.2265 0.144 Uiso 1 1 calc R U . . .
H21C H 0.8446 0.8864 -0.1835 0.144 Uiso 1 1 calc R U . . .
C22 C 1.0489(5) 0.8039(3) -0.1132(2) 0.0535(10) Uani 1 1 d . . . . .
H22A H 1.1670 0.7767 -0.1246 0.064 Uiso 1 1 calc R U . . .
H22B H 1.0277 0.8655 -0.0817 0.064 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 O4 1.6025(19) . ?
V1 O2 1.964(2) . ?
V1 O8 1.991(2) . ?
V1 O1 1.9968(18) 2_666 ?
V1 N1 2.136(2) . ?
V1 O1 2.2652(18) . ?
V2 O5 1.589(2) . ?
V2 O8 1.997(2) . ?
V2 O7 2.000(2) . ?
V2 O2 2.0075(19) 2_666 ?
V2 O6 2.015(2) . ?
V2 O1 2.327(2) . ?
V4 O14 1.588(2) . ?
V4 O16 1.992(2) . ?
V4 O13 2.0062(19) . ?
V4 O15 2.010(2) . ?
V4 O9 2.0141(19) 2_765 ?
V4 O10 2.321(2) . ?
V3 O12 1.6150(18) . ?
V3 O9 1.966(2) . ?
V3 O10 1.9893(18) 2_765 ?
V3 O13 1.990(2) . ?
V3 N2 2.119(2) . ?
V3 O10 2.2896(18) . ?
O1 C3 1.426(3) . ?
O1 V1 1.9967(18) 2_666 ?
O2 C4 1.420(3) . ?
O2 V2 2.0075(19) 2_666 ?
O3 C1 1.421(3) . ?
O3 H3C 0.8200 . ?
O6 C8 1.267(3) . ?
O7 C6 1.284(3) . ?
O8 C11 1.425(4) . ?
O9 C14 1.417(3) . ?
O9 V4 2.0140(19) 2_765 ?
O11 C12 1.412(4) . ?
O11 H10D 0.8200 . ?
O10 C15 1.425(3) . ?
O10 V3 1.9893(18) 2_765 ?
O13 C22 1.438(4) . ?
O15 C19 1.274(3) . ?
O16 C17 1.281(3) . ?
N1 C2 1.486(3) . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N2 C13 1.493(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
C1 C2 1.525(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.529(3) . ?
C2 C4 1.529(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.489(4) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.381(5) . ?
C7 C8 1.393(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.501(4) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.513(5) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.518(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C15 1.526(3) . ?
C13 C14 1.529(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.496(4) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.386(4) . ?
C18 C19 1.386(4) . ?
C18 H18A 0.9300 . ?
C19 C20 1.499(4) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.511(6) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?

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
O4 V1 O2 103.98(9) . . ?
O4 V1 O8 95.63(10) . . ?
O2 V1 O8 160.39(8) . . ?
O4 V1 O1 104.18(9) . 2_666 ?
O2 V1 O1 79.62(8) . 2_666 ?
O8 V1 O1 95.57(8) . 2_666 ?
O4 V1 N1 107.69(9) . . ?
O2 V1 N1 79.83(8) . . ?
O8 V1 N1 94.53(8) . . ?
O1 V1 N1 145.34(8) 2_666 . ?
O4 V1 O1 171.60(9) . . ?
O2 V1 O1 84.40(7) . . ?
O8 V1 O1 76.00(7) . . ?
O1 V1 O1 77.70(7) 2_666 . ?
N1 V1 O1 72.77(8) . . ?
O5 V2 O8 98.83(10) . . ?
O5 V2 O7 104.18(10) . . ?
O8 V2 O7 87.50(8) . . ?
O5 V2 O2 100.26(10) . 2_666 ?
O8 V2 O2 88.50(8) . 2_666 ?
O7 V2 O2 155.55(8) . 2_666 ?
O5 V2 O6 97.93(11) . . ?
O8 V2 O6 163.16(8) . . ?
O7 V2 O6 86.76(9) . . ?
O2 V2 O6 90.20(8) 2_666 . ?
O5 V2 O1 168.97(9) . . ?
O8 V2 O1 74.46(7) . . ?
O7 V2 O1 84.52(8) . . ?
O2 V2 O1 71.18(7) 2_666 . ?
O6 V2 O1 89.23(8) . . ?
O14 V4 O16 103.68(11) . . ?
O14 V4 O13 98.95(10) . . ?
O16 V4 O13 86.76(8) . . ?
O14 V4 O15 98.82(10) . . ?
O16 V4 O15 86.82(9) . . ?
O13 V4 O15 162.08(9) . . ?
O14 V4 O9 99.60(10) . 2_765 ?
O16 V4 O9 156.70(9) . 2_765 ?
O13 V4 O9 88.81(8) . 2_765 ?
O15 V4 O9 90.51(8) . 2_765 ?
O14 V4 O10 168.43(9) . . ?
O16 V4 O10 86.09(8) . . ?
O13 V4 O10 75.12(7) . . ?
O15 V4 O10 87.76(8) . . ?
O9 V4 O10 70.67(7) 2_765 . ?
O12 V3 O9 103.08(9) . . ?
O12 V3 O10 107.07(9) . 2_765 ?
O9 V3 O10 79.14(8) . 2_765 ?
O12 V3 O13 96.72(9) . . ?
O9 V3 O13 160.19(8) . . ?
O10 V3 O13 95.74(8) 2_765 . ?
O12 V3 N2 105.22(9) . . ?
O9 V3 N2 79.64(8) . . ?
O10 V3 N2 144.53(8) 2_765 . ?
O13 V3 N2 94.70(9) . . ?
O12 V3 O10 172.24(9) . . ?
O9 V3 O10 84.06(7) . . ?
O10 V3 O10 77.02(7) 2_765 . ?
O13 V3 O10 76.14(7) . . ?
N2 V3 O10 72.79(8) . . ?
C3 O1 V1 122.27(15) . 2_666 ?
C3 O1 V1 110.90(14) . . ?
V1 O1 V1 102.30(7) 2_666 . ?
C3 O1 V2 124.52(15) . . ?
V1 O1 V2 97.34(7) 2_666 . ?
V1 O1 V2 94.31(7) . . ?
C4 O2 V1 116.67(15) . . ?
C4 O2 V2 124.73(17) . 2_666 ?
V1 O2 V2 110.03(8) . 2_666 ?
C1 O3 H3C 109.5 . . ?
C8 O6 V2 125.1(2) . . ?
C6 O7 V2 127.25(19) . . ?
C11 O8 V1 122.19(18) . . ?
C11 O8 V2 121.32(18) . . ?
V1 O8 V2 115.22(9) . . ?
C14 O9 V3 116.67(15) . . ?
C14 O9 V4 123.58(16) . 2_765 ?
V3 O9 V4 110.21(9) . 2_765 ?
C12 O11 H10D 109.5 . . ?
C15 O10 V3 122.52(15) . 2_765 ?
C15 O10 V3 110.70(14) . . ?
V3 O10 V3 102.98(7) 2_765 . ?
C15 O10 V4 123.49(15) . . ?
V3 O10 V4 98.18(7) 2_765 . ?
V3 O10 V4 93.86(7) . . ?
C22 O13 V3 122.51(19) . . ?
C22 O13 V4 120.00(18) . . ?
V3 O13 V4 114.87(9) . . ?
C19 O15 V4 125.33(19) . . ?
C17 O16 V4 126.79(19) . . ?
C2 N1 V1 101.87(14) . . ?
C2 N1 H1C 111.4 . . ?
V1 N1 H1C 111.4 . . ?
C2 N1 H1D 111.4 . . ?
V1 N1 H1D 111.4 . . ?
H1C N1 H1D 109.3 . . ?
C13 N2 V3 102.63(15) . . ?
C13 N2 H2A 111.2 . . ?
V3 N2 H2A 111.2 . . ?
C13 N2 H2B 111.2 . . ?
V3 N2 H2B 111.2 . . ?
H2A N2 H2B 109.2 . . ?
O3 C1 C2 111.1(2) . . ?
O3 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
O3 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N1 C2 C1 113.1(2) . . ?
N1 C2 C3 106.0(2) . . ?
C1 C2 C3 111.5(2) . . ?
N1 C2 C4 106.1(2) . . ?
C1 C2 C4 108.6(2) . . ?
C3 C2 C4 111.5(2) . . ?
O1 C3 C2 110.1(2) . . ?
O1 C3 H3A 109.6 . . ?
C2 C3 H3A 109.6 . . ?
O1 C3 H3B 109.6 . . ?
C2 C3 H3B 109.6 . . ?
H3A C3 H3B 108.2 . . ?
O2 C4 C2 109.2(2) . . ?
O2 C4 H4A 109.8 . . ?
C2 C4 H4A 109.8 . . ?
O2 C4 H4B 109.8 . . ?
C2 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O7 C6 C7 123.9(3) . . ?
O7 C6 C5 114.8(3) . . ?
C7 C6 C5 121.3(3) . . ?
C6 C7 C8 124.8(3) . . ?
C6 C7 H7A 117.6 . . ?
C8 C7 H7A 117.6 . . ?
O6 C8 C7 124.5(3) . . ?
O6 C8 C9 116.2(3) . . ?
C7 C8 C9 119.3(3) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O8 C11 C10 112.9(3) . . ?
O8 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
O8 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
O11 C12 C13 109.3(2) . . ?
O11 C12 H12A 109.8 . . ?
C13 C12 H12A 109.8 . . ?
O11 C12 H12B 109.8 . . ?
C13 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
N2 C13 C12 113.6(2) . . ?
N2 C13 C15 106.2(2) . . ?
C12 C13 C15 110.8(2) . . ?
N2 C13 C14 105.6(2) . . ?
C12 C13 C14 109.2(2) . . ?
C15 C13 C14 111.3(2) . . ?
O9 C14 C13 109.6(2) . . ?
O9 C14 H14A 109.7 . . ?
C13 C14 H14A 109.7 . . ?
O9 C14 H14B 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
O10 C15 C13 110.0(2) . . ?
O10 C15 H15A 109.7 . . ?
C13 C15 H15A 109.7 . . ?
O10 C15 H15B 109.7 . . ?
C13 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O16 C17 C18 124.1(3) . . ?
O16 C17 C16 115.3(3) . . ?
C18 C17 C16 120.6(3) . . ?
C19 C18 C17 124.3(3) . . ?
C19 C18 H18A 117.8 . . ?
C17 C18 H18A 117.8 . . ?
O15 C19 C18 124.9(3) . . ?
O15 C19 C20 116.1(3) . . ?
C18 C19 C20 119.0(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O13 C22 C21 113.5(3) . . ?
O13 C22 H22A 108.9 . . ?
C21 C22 H22A 108.9 . . ?
O13 C22 H22B 108.9 . . ?
C21 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?

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 N1 C2 C1 172.30(17) . . . . ?
V1 N1 C2 C3 -65.28(19) . . . . ?
V1 N1 C2 C4 53.3(2) . . . . ?
O3 C1 C2 N1 52.7(3) . . . . ?
O3 C1 C2 C3 -66.6(3) . . . . ?
O3 C1 C2 C4 170.2(2) . . . . ?
V1 O1 C3 C2 122.84(18) 2_666 . . . ?
V1 O1 C3 C2 2.1(2) . . . . ?
V2 O1 C3 C2 -109.0(2) . . . . ?
N1 C2 C3 O1 40.6(3) . . . . ?
C1 C2 C3 O1 164.1(2) . . . . ?
C4 C2 C3 O1 -74.3(3) . . . . ?
V1 O2 C4 C2 12.7(3) . . . . ?
V2 O2 C4 C2 -131.82(19) 2_666 . . . ?
N1 C2 C4 O2 -45.4(3) . . . . ?
C1 C2 C4 O2 -167.3(2) . . . . ?
C3 C2 C4 O2 69.5(3) . . . . ?
V2 O7 C6 C7 11.2(4) . . . . ?
V2 O7 C6 C5 -168.6(2) . . . . ?
O7 C6 C7 C8 6.4(5) . . . . ?
C5 C6 C7 C8 -173.8(3) . . . . ?
V2 O6 C8 C7 -24.4(4) . . . . ?
V2 O6 C8 C9 155.5(2) . . . . ?
C6 C7 C8 O6 0.9(5) . . . . ?
C6 C7 C8 C9 -179.1(3) . . . . ?
V1 O8 C11 C10 -69.6(3) . . . . ?
V2 O8 C11 C10 97.0(3) . . . . ?
V3 N2 C13 C12 -172.48(18) . . . . ?
V3 N2 C13 C15 65.5(2) . . . . ?
V3 N2 C13 C14 -52.8(2) . . . . ?
O11 C12 C13 N2 -55.9(3) . . . . ?
O11 C12 C13 C15 63.5(3) . . . . ?
O11 C12 C13 C14 -173.5(2) . . . . ?
V3 O9 C14 C13 -11.1(3) . . . . ?
V4 O9 C14 C13 131.80(18) 2_765 . . . ?
N2 C13 C14 O9 43.6(3) . . . . ?
C12 C13 C14 O9 166.1(2) . . . . ?
C15 C13 C14 O9 -71.2(3) . . . . ?
V3 O10 C15 C13 -122.37(19) 2_765 . . . ?
V3 O10 C15 C13 -0.6(2) . . . . ?
V4 O10 C15 C13 109.0(2) . . . . ?
N2 C13 C15 O10 -41.1(3) . . . . ?
C12 C13 C15 O10 -164.9(2) . . . . ?
C14 C13 C15 O10 73.3(3) . . . . ?
V4 O16 C17 C18 -15.2(5) . . . . ?
V4 O16 C17 C16 166.1(2) . . . . ?
O16 C17 C18 C19 -6.0(6) . . . . ?
C16 C17 C18 C19 172.7(3) . . . . ?
V4 O15 C19 C18 19.6(4) . . . . ?
V4 O15 C19 C20 -160.5(2) . . . . ?
C17 C18 C19 O15 3.4(6) . . . . ?
C17 C18 C19 C20 -176.5(3) . . . . ?
V3 O13 C22 C21 64.0(4) . . . . ?
V4 O13 C22 C21 -96.7(3) . . . . ?

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
O3 H3C O4 0.82 1.94 2.746(3) 168.6 1_455
O11 H10D O12 0.82 2.09 2.875(3) 160.7 1_455
N1 H1C O12 0.89 2.21 3.032(3) 153.1 1_456
N1 H1D O7 0.89 2.27 3.050(3) 145.6 .
N2 H2A O16 0.89 2.28 3.058(3) 146.0 .
N2 H2B O3 0.89 2.26 3.127(3) 165.5 1_654
C1 H1B O9 0.97 2.65 3.596(3) 163.8 1_456
C5 H5B O3 0.96 2.60 3.443(4) 146.6 .
C11 H11A O5 0.97 2.49 3.049(4) 116.8 .
C12 H12A O4 0.97 2.27 3.199(4) 160.1 1_554
C21 H21B O12 0.96 2.65 3.267(6) 122.6 .
C21 H21C O16 0.96 2.62 3.319(6) 129.6 .
C22 H22A O11 0.97 2.62 3.547(4) 161.0 1_655
C22 H22B O14 0.97 2.49 3.066(4) 117.5 .

_refine_diff_density_max         0.318
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.065

