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

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

data_110k
_database_code_depnum_ccdc_archive 'CCDC 2004615'
loop_
_audit_author_name
_audit_author_address
'zhiyuan Yao'
;Nanjing Tech university
China
;
_audit_update_record             
;
2020-05-19 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_audit_creation_date             2019-11-28
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'O8 V3, 0.5(H16 N4)'
_chemical_formula_sum            'H8 N2 O8 V3'
_chemical_formula_weight         316.90
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   8.8551(3)
_cell_length_b                   8.8551(3)
_cell_length_c                   5.5652(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     436.38(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2547
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      27.517
_cell_measurement_theta_min      4.604
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.164
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1216 before and 0.0788 after correction. The Ratio of minimum to maximum transmission is 0.7347. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.412
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             310
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4284
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.575
_diffrn_reflns_theta_min         3.254
_diffrn_ambient_temperature      110.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                532
_reflns_number_total             556
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 
;
 Flack x determined using 217 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         556
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0335
_refine_ls_restrained_S_all      1.141
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+1.3754P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0685
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.79(9)
 0.21(9)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H,H) groups
3. Restrained distances
 N1-H1C \\sim N1-H1B \\sim N1-H1A
 with sigma of 0.02
4. Others
 Fixed Sof: H1B(0.5) H1C(0.5)
5.a Riding coordinates:
 N1(H1A,H1B,H1C), N1(H1D)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V -0.13323(8) -0.63323(8) -0.8584(3) 0.0095(3) Uani 1 2 d S T P . .
V1 V 0.0000 -1.0000 -0.8618(5) 0.0126(4) Uani 1 4 d S T P . .
O1 O 0.0000 -1.0000 -0.5740(16) 0.0217(18) Uani 1 4 d S T P . .
O3 O 0.0000 -0.5000 -0.9731(15) 0.023(2) Uani 1 4 d S T P . .
O2 O -0.0853(5) -0.8068(5) -0.9660(9) 0.0267(10) Uani 1 1 d . . . . .
O4 O -0.1301(4) -0.6301(4) -0.5643(10) 0.0143(11) Uani 1 2 d S T P . .
N1 N -0.3291(5) -0.8291(5) -0.3273(14) 0.0163(15) Uani 1 2 d DS T P . .
H1A H -0.3825 -0.8825 -0.4383 0.020 Uiso 1 2 d DR U P . .
H1B H -0.2753 -0.8940 -0.2337 0.020 Uiso 0.5 1 d DR U P . .
H1C H -0.3939 -0.7754 -0.2337 0.020 Uiso 0.5 1 d DR U P . .
H1D H -0.2634 -0.7634 -0.4049 0.020 Uiso 1 2 d R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V2 0.0092(3) 0.0092(3) 0.0102(5) -0.0024(6) -0.0024(6) 0.0018(4)
V1 0.0085(4) 0.0085(4) 0.0208(8) 0.000 0.000 0.000
O1 0.023(3) 0.023(3) 0.020(4) 0.000 0.000 0.000
O3 0.028(3) 0.028(3) 0.014(4) 0.000 0.000 -0.010(4)
O2 0.036(3) 0.016(2) 0.028(2) -0.0100(18) -0.017(2) 0.015(2)
O4 0.0178(18) 0.0178(18) 0.007(2) -0.0006(15) -0.0006(15) -0.005(2)
N1 0.0192(18) 0.0192(18) 0.010(4) 0.002(2) 0.002(2) -0.007(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
V2 O3 1.786(3) . ?
V2 O2 1.703(4) . ?
V2 O2 1.703(4) 8_545 ?
V2 O4 1.637(6) . ?
V1 O1 1.602(9) . ?
V1 O2 1.958(4) 2_535 ?
V1 O2 1.958(4) 3_445 ?
V1 O2 1.958(4) . ?
V1 O2 1.958(4) 4_645 ?
O3 V2 1.786(3) 2_545 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9106 . ?
N1 H1C 0.9095 . ?
N1 H1D 0.9289 . ?

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
O2 V2 O3 107.8(3) 8_545 . ?
O2 V2 O3 107.8(3) . . ?
O2 V2 O2 109.0(3) . 8_545 ?
O4 V2 O3 109.5(3) . . ?
O4 V2 O2 111.3(2) . 8_545 ?
O4 V2 O2 111.3(2) . . ?
O1 V1 O2 107.23(16) . 3_445 ?
O1 V1 O2 107.23(16) . . ?
O1 V1 O2 107.23(16) . 2_535 ?
O1 V1 O2 107.23(16) . 4_645 ?
O2 V1 O2 84.97(9) 3_445 2_535 ?
O2 V1 O2 145.5(3) 2_535 . ?
O2 V1 O2 84.97(9) 4_645 . ?
O2 V1 O2 145.5(3) 3_445 4_645 ?
O2 V1 O2 84.97(9) 3_445 . ?
O2 V1 O2 84.97(9) 4_645 2_535 ?
V2 O3 V2 138.1(5) . 2_545 ?
V2 O2 V1 141.3(3) . . ?
H1A N1 H1B 109.4 . . ?
H1A N1 H1C 109.4 . . ?
H1A N1 H1D 109.5 . . ?
H1B N1 H1C 109.5 . . ?
H1B N1 H1D 109.5 . . ?
H1C N1 H1D 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
O3 V2 O2 V1 108.5(5) . . . . ?
O2 V2 O3 V2 -121.22(19) . . . 2_545 ?
O2 V2 O3 V2 121.22(19) 8_545 . . 2_545 ?
O2 V2 O2 V1 -134.7(3) 8_545 . . . ?
O4 V2 O3 V2 0.000(1) . . . 2_545 ?
O4 V2 O2 V1 -11.6(6) . . . . ?

_shelx_res_file                  
;
    110k.res created by SHELXL-2014/7

TITL 110K in P4bm
CELL 0.71073 8.8551 8.8551 5.5652 90 90 90
ZERR 2 0.0003 0.0003 0.0005 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,+Z
SYMM 0.5-Y,0.5-X,+Z
SYMM 0.5+Y,0.5+X,+Z
SFAC H N O V
UNIT 16 4 16 6
SADI N1 H1c N1 H1b N1 H1a

L.S. 10
PLAN  1
TEMP -163.15
CONF
MORE -1
BOND $H
fmap 2
acta
TWIN 1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%110K.hkl">
REM </olex2.extras>

WGHT    0.000000    1.375400
BASF   0.20817
FVAR       0.78143
V2    4   -0.133232   -0.633232   -0.858429    10.50000    0.00917    0.00917 =
         0.01019   -0.00240   -0.00240    0.00176
V1    4    0.000000   -1.000000   -0.861801    10.25000    0.00852    0.00852 =
         0.02082    0.00000    0.00000    0.00000
O1    3    0.000000   -1.000000   -0.573952    10.25000    0.02268    0.02268 =
         0.01975    0.00000    0.00000    0.00000
O3    3    0.000000   -0.500000   -0.973107    10.25000    0.02795    0.02795 =
         0.01362    0.00000    0.00000   -0.00968
O2    3   -0.085330   -0.806771   -0.966022    11.00000    0.03630    0.01615 =
         0.02764   -0.01004   -0.01676    0.01511
O4    3   -0.130076   -0.630076   -0.564286    10.50000    0.01778    0.01778 =
         0.00744   -0.00059   -0.00059   -0.00538
N1    2   -0.329101   -0.829101   -0.327326    10.50000    0.01924    0.01924 =
         0.01041    0.00151    0.00151   -0.00652
AFIX   3
H1A   1   -0.382451   -0.882450   -0.438336    10.50000   -1.20000
H1B   1   -0.275251   -0.894020   -0.233716    10.50000   -1.20000
H1C   1   -0.393911   -0.775360   -0.233716    10.50000   -1.20000
AFIX   3
H1D   1   -0.263421   -0.763420   -0.404906    10.50000   -1.20000
AFIX   0
HKLF 4

REM  110K in P4bm
REM R1 =  0.0335 for     532 Fo > 4sig(Fo)  and  0.0362 for all     556 data
REM     39 parameters refined using      4 restraints

END

WGHT      0.0000      1.3754

REM Highest difference peak  0.501,  deepest hole -0.426,  1-sigma level  0.102
Q1    1  -0.0428 -0.6453 -0.8576  11.00000  0.05    0.50
;
_shelx_res_checksum              97881
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.79(9)
2 0.21(9)

####################################################################### 
# 
# 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_300k-1
_database_code_depnum_ccdc_archive 'CCDC 2004938'
loop_
_audit_author_name
_audit_author_address
'zhiyuan Yao'
;Nanjing Tech university
China
;
_audit_update_record             
;
2020-05-20 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_audit_creation_date             2019-11-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'O8 V3, 0.5(H16 N4)'
_chemical_formula_sum            'H8 N2 O8 V3'
_chemical_formula_weight         316.90
_chemical_absolute_configuration rmad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   8.8895(4)
_cell_length_b                   8.8895(4)
_cell_length_c                   5.5731(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     440.40(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2541
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      27.418
_cell_measurement_theta_min      4.586
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.135
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1208 before and 0.0775 after correction. The Ratio of minimum to maximum transmission is 0.7614. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.390
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             310
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4245
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.416
_diffrn_reflns_theta_min         3.241
_diffrn_ambient_temperature      300.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                526
_reflns_number_total             556
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 
;
 Flack x determined using 222 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.30(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         556
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0338
_refine_ls_restrained_S_all      1.112
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0147P)²+1.4411P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0725
_refine_special_details          
;
 Refined as a 2-component perfect twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H,H) groups
2. Others
 Fixed Sof: H1B(0.5) H1C(0.5)
3.a Riding coordinates:
 N1(H1A,H1B,H1C), N1(H1D)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V 0.63349(8) 0.13349(8) 0.2186(4) 0.0113(3) Uani 1 2 d S T P . .
N1 N 0.8301(5) 0.3301(5) 0.7485(17) 0.0286(19) Uani 1 2 d S T P . .
H1A H 0.8820 0.3820 0.6401 0.034 Uiso 1 2 d R U P . .
H1B H 0.7776 0.3931 0.8399 0.034 Uiso 0.5 1 d R U P . .
H1C H 0.8932 0.2775 0.8399 0.034 Uiso 0.5 1 d R U P . .
H1D H 0.7660 0.2660 0.6724 0.034 Uiso 1 2 d R U P . .
O4 O 0.6305(5) 0.1305(5) 0.5117(11) 0.0225(13) Uani 1 2 d S T P . .
V1 V 1.0000 0.0000 0.2153(5) 0.0123(4) Uani 1 4 d S T P . .
O3 O 0.5000 0.0000 0.1039(15) 0.0190(18) Uani 1 4 d S T P . .
O1 O 1.0000 0.0000 0.5021(16) 0.029(2) Uani 1 4 d S T P . .
O2 O 0.8069(5) 0.0855(5) 0.1120(9) 0.0226(9) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V2 0.0085(3) 0.0085(3) 0.0169(5) -0.0001(7) -0.0001(7) 0.0004(4)
N1 0.034(2) 0.034(2) 0.017(5) -0.003(2) -0.003(2) -0.015(3)
O4 0.027(2) 0.027(2) 0.013(3) -0.0017(18) -0.0017(18) -0.004(3)
V1 0.0090(4) 0.0090(4) 0.0190(8) 0.000 0.000 0.000
O3 0.016(3) 0.016(3) 0.024(5) 0.000 0.000 -0.007(3)
O1 0.035(3) 0.035(3) 0.017(5) 0.000 0.000 0.000
O2 0.012(2) 0.020(2) 0.037(2) 0.0029(19) 0.0025(18) 0.0054(17)

_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
V2 O4 1.634(6) . ?
V2 O3 1.796(3) . ?
V2 O2 1.707(4) . ?
V2 O2 1.707(4) 8_545 ?
N1 H1A 0.8899 . ?
N1 H1B 0.8894 . ?
N1 H1C 0.8905 . ?
N1 H1D 0.9101 . ?
V1 O1 1.599(9) . ?
V1 O2 1.963(4) . ?
V1 O2 1.963(4) 2_755 ?
V1 O2 1.963(4) 3_645 ?
V1 O2 1.963(4) 4_665 ?
O3 V2 1.796(3) 2_655 ?

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 V2 O3 109.5(3) . . ?
O4 V2 O2 111.0(2) . . ?
O4 V2 O2 111.0(2) . 8_545 ?
O2 V2 O3 107.9(2) . . ?
O2 V2 O3 107.9(2) 8_545 . ?
O2 V2 O2 109.3(3) . 8_545 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1A N1 H1D 109.5 . . ?
H1B N1 H1C 109.5 . . ?
H1B N1 H1D 109.4 . . ?
H1C N1 H1D 109.4 . . ?
O1 V1 O2 107.05(16) . 3_645 ?
O1 V1 O2 107.04(16) . . ?
O1 V1 O2 107.05(16) . 4_665 ?
O1 V1 O2 107.05(16) . 2_755 ?
O2 V1 O2 145.9(3) 2_755 . ?
O2 V1 O2 85.07(9) 3_645 . ?
O2 V1 O2 85.07(9) 4_665 . ?
O2 V1 O2 145.9(3) 3_645 4_665 ?
O2 V1 O2 85.07(9) 3_645 2_755 ?
O2 V1 O2 85.07(9) 4_665 2_755 ?
V2 O3 V2 138.3(5) . 2_655 ?
V2 O2 V1 141.7(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
O4 V2 O3 V2 0.000(1) . . . 2_655 ?
O4 V2 O2 V1 11.8(5) . . . . ?
O3 V2 O2 V1 -108.2(5) . . . . ?
O2 V2 O3 V2 121.0(2) . . . 2_655 ?
O2 V2 O3 V2 -121.0(2) 8_545 . . 2_655 ?
O2 V2 O2 V1 134.6(3) 8_545 . . . ?

_shelx_res_file                  
;
    300k-1.res created by SHELXL-2014/7

TITL 300K-1 in P4bm
CELL 0.71073 8.8895 8.8895 5.5731 90 90 90
ZERR 2 0.0004 0.0004 0.0006 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,+Z
SYMM 0.5-Y,0.5-X,+Z
SYMM 0.5+Y,0.5+X,+Z
SFAC H N O V
UNIT 16 4 16 6

L.S. 4
PLAN  1
TEMP 26.85
CONF
BOND
fmap 2
acta
MORE -1
BOND $H
TWIN 1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\300K-1.hkl">
REM </olex2.extras>

WGHT    0.014700    1.441100
FVAR       0.84229
V2    4    0.633485    0.133485    0.218601    10.50000    0.00848    0.00848 =
         0.01688   -0.00010   -0.00010    0.00037
N1    2    0.830074    0.330074    0.748492    10.50000    0.03437    0.03437 =
         0.01714   -0.00325   -0.00325   -0.01513
AFIX   3
H1A   1    0.882034    0.382030    0.640052    10.50000   -1.20000
H1B   1    0.777594    0.393090    0.839902    10.50000   -1.20000
H1C   1    0.893204    0.277480    0.839902    10.50000   -1.20000
AFIX   3
H1D   1    0.766014    0.266010    0.672432    10.50000   -1.20000
AFIX   0

O4    3    0.630462    0.130462    0.511726    10.50000    0.02746    0.02746 =
         0.01261   -0.00170   -0.00170   -0.00362
V1    4    1.000000    0.000000    0.215267    10.25000    0.00902    0.00902 =
         0.01898    0.00000    0.00000    0.00000
O3    3    0.500000    0.000000    0.103944    10.25000    0.01629    0.01629 =
         0.02447    0.00000    0.00000   -0.00724
O1    3    1.000000    0.000000    0.502103    10.25000    0.03489    0.03489 =
         0.01728    0.00000    0.00000    0.00000
O2    3    0.806947    0.085518    0.112011    11.00000    0.01156    0.01960 =
         0.03654    0.00286    0.00248    0.00540
HKLF 4

REM  300K-1 in P4bm
REM R1 =  0.0338 for     526 Fo > 4sig(Fo)  and  0.0379 for all     556 data
REM     38 parameters refined using      1 restraints

END

WGHT      0.0147      1.4411

REM Highest difference peak  0.504,  deepest hole -0.437,  1-sigma level  0.101
Q1    1   0.6349  0.2238  0.2191  11.00000  0.05    0.50
;
_shelx_res_checksum              33080
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_130k
_database_code_depnum_ccdc_archive 'CCDC 2005049'
loop_
_audit_author_name
_audit_author_address
'zhiyuan Yao'
;Nanjing Tech university
China
;
_audit_update_record             
;
2020-05-21 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_audit_creation_date             2019-11-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'O8 V3, 0.5(H16 N4)'
_chemical_formula_sum            'H8 N2 O8 V3'
_chemical_formula_weight         316.90
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   8.8599(4)
_cell_length_b                   8.8599(4)
_cell_length_c                   5.5653(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     436.86(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2544
_cell_measurement_temperature    130.0
_cell_measurement_theta_max      27.502
_cell_measurement_theta_min      4.601
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.161
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1227 before and 0.0797 after correction. The Ratio of minimum to maximum transmission is 0.7363. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.409
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             310
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4261
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.574
_diffrn_reflns_theta_min         3.252
_diffrn_ambient_temperature      130.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                526
_reflns_number_total             555
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 
;
 Flack x determined using 217 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         555
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0318
_refine_ls_restrained_S_all      1.166
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+1.2543P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0671
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.81(9)
 0.19(9)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
3. Restrained distances
 N1-H1D
 0.9 with sigma of 0.02
4. Others
 Fixed Sof: H1B(0.5) H1C(0.5)
5.a Riding coordinates:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V -0.36669(8) -0.13331(8) -0.4957(3) 0.0096(3) Uani 1 2 d S T P . .
V1 V 0.0000 0.0000 -0.4988(5) 0.0118(3) Uani 1 4 d S T P . .
O4 O -0.3701(4) -0.1299(4) -0.2012(10) 0.0146(11) Uani 1 2 d S T P . .
O1 O 0.0000 0.0000 -0.2109(16) 0.0228(19) Uani 1 4 d S T P . .
O3 O -0.5000 0.0000 -0.6105(14) 0.0221(19) Uani 1 4 d S T P . .
O2 O -0.1933(5) -0.0852(5) -0.6030(9) 0.0256(9) Uani 1 1 d . . . . .
N1 N -0.1708(5) -0.3292(5) 0.0348(15) 0.0174(15) Uani 1 2 d DS T P . .
H1A H -0.1174 -0.3826 -0.0761 0.021 Uiso 1 2 d R U P . .
H1B H -0.1060 -0.2752 0.1285 0.021 Uiso 0.5 1 d R U P . .
H1C H -0.2246 -0.3938 0.1285 0.021 Uiso 0.5 1 d R U P . .
H1D H -0.232(6) -0.268(6) -0.05(2) 0.06(4) Uiso 1 2 d DS . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V2 0.0091(3) 0.0091(3) 0.0107(5) -0.0020(6) 0.0020(6) -0.0015(4)
V1 0.0084(4) 0.0084(4) 0.0188(8) 0.000 0.000 0.000
O4 0.0181(18) 0.0181(18) 0.008(2) 0.0008(15) -0.0008(15) 0.005(2)
O1 0.026(3) 0.026(3) 0.016(4) 0.000 0.000 0.000
O3 0.027(3) 0.027(3) 0.011(4) 0.000 0.000 0.010(4)
O2 0.014(2) 0.034(3) 0.029(2) -0.014(2) 0.0080(18) -0.0135(19)
N1 0.0212(18) 0.0212(18) 0.010(4) 0.000(2) 0.000(2) 0.008(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
V2 O4 1.639(6) . ?
V2 O3 1.788(3) . ?
V2 O2 1.702(4) . ?
V2 O2 1.702(4) 7_445 ?
V1 O1 1.603(9) . ?
V1 O2 1.960(4) . ?
V1 O2 1.960(4) 4 ?
V1 O2 1.960(4) 3 ?
V1 O2 1.960(4) 2 ?
O3 V2 1.788(3) 2_455 ?
N1 H1A 0.9103 . ?
N1 H1B 0.9106 . ?
N1 H1C 0.9093 . ?
N1 H1D 0.90(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 V2 O3 109.4(3) . . ?
O4 V2 O2 111.3(2) . 7_445 ?
O4 V2 O2 111.3(2) . . ?
O2 V2 O3 107.8(2) . . ?
O2 V2 O3 107.8(2) 7_445 . ?
O2 V2 O2 109.2(3) 7_445 . ?
O1 V1 O2 107.21(16) . 3 ?
O1 V1 O2 107.21(16) . 4 ?
O1 V1 O2 107.21(16) . . ?
O1 V1 O2 107.21(16) . 2 ?
O2 V1 O2 84.98(9) . 3 ?
O2 V1 O2 145.6(3) 3 4 ?
O2 V1 O2 84.98(9) 2 4 ?
O2 V1 O2 145.6(3) . 2 ?
O2 V1 O2 84.98(9) . 4 ?
O2 V1 O2 84.98(9) 2 3 ?
V2 O3 V2 138.1(5) 2_455 . ?
V2 O2 V1 141.4(3) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1A N1 H1D 105.2 . . ?
H1B N1 H1C 109.5 . . ?
H1B N1 H1D 111.5 . . ?
H1C N1 H1D 111.6 . . ?

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
O4 V2 O3 V2 0.000(1) . . . 2_455 ?
O4 V2 O2 V1 -11.4(6) . . . . ?
O3 V2 O2 V1 108.6(5) . . . . ?
O2 V2 O3 V2 121.14(19) 7_445 . . 2_455 ?
O2 V2 O3 V2 -121.14(19) . . . 2_455 ?
O2 V2 O2 V1 -134.6(3) 7_445 . . . ?

_shelx_res_file                  
;
    130k.res created by SHELXL-2014/7

TITL 130K in P4bm
CELL 0.71073 8.8599 8.8599 5.5653 90 90 90
ZERR 2 0.0004 0.0004 0.0006 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,+Z
SYMM 0.5-Y,0.5-X,+Z
SYMM 0.5+Y,0.5+X,+Z
SFAC H N O V
UNIT 16 4 16 6
DFIX 0.9 N1 H1d

L.S. 20
PLAN  1
TEMP -143.15
CONF
MORE -1
BOND $H
fmap 2
acta
TWIN 1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%130K.hkl">
REM </olex2.extras>

WGHT    0.000000    1.254300
BASF   0.19279
FVAR       0.24699
V2    4   -0.366694   -0.133306   -0.495670    10.50000    0.00908    0.00908 =
         0.01066   -0.00195    0.00195   -0.00154
V1    4    0.000000    0.000000   -0.498841    10.25000    0.00836    0.00836 =
         0.01879    0.00000    0.00000    0.00000
O4    3   -0.370108   -0.129892   -0.201228    10.50000    0.01808    0.01808 =
         0.00776    0.00078   -0.00078    0.00508
O1    3    0.000000    0.000000   -0.210860    10.25000    0.02606    0.02606 =
         0.01638    0.00000    0.00000    0.00000
O3    3   -0.500000    0.000000   -0.610458    10.25000    0.02743    0.02743 =
         0.01143    0.00000    0.00000    0.01040
O2    3   -0.193315   -0.085228   -0.603017    11.00000    0.01444    0.03351 =
         0.02883   -0.01436    0.00803   -0.01354
N1    2   -0.170784   -0.329216    0.034844    10.50000    0.02122    0.02122 =
         0.00986    0.00025   -0.00025    0.00775
AFIX   3
H1A   1   -0.117403   -0.382600   -0.076096    10.50000   -1.20000
H1B   1   -0.106043   -0.275220    0.128454    10.50000   -1.20000
H1C   1   -0.224643   -0.393820    0.128454    10.50000   -1.20000
AFIX   0
H1D   1   -0.231683   -0.268317   -0.051247    10.50000    0.06404
HKLF 4

REM  130K in P4bm
REM R1 =  0.0318 for     526 Fo > 4sig(Fo)  and  0.0358 for all     555 data
REM     42 parameters refined using      2 restraints

END

WGHT      0.0000      1.2543

REM Highest difference peak  0.514,  deepest hole -0.427,  1-sigma level  0.102
Q1    1  -0.3693 -0.0430 -0.4952  11.00000  0.05    0.51
;
_shelx_res_checksum              11966
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.81(9)
2 0.19(9)

####################################################################### 
# 
# 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_k-1
_database_code_depnum_ccdc_archive 'CCDC 2004937'
loop_
_audit_author_name
_audit_author_address
'zhiyuan Yao'
;Nanjing Tech university
China
;
_audit_update_record             
;
2020-05-21 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_audit_creation_date             2019-11-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'O8 V3, 0.5(H16 N4)'
_chemical_formula_sum            'H8 N2 O8 V3'
_chemical_formula_weight         316.90
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   8.8761(4)
_cell_length_b                   8.8761(4)
_cell_length_c                   5.5632(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     438.30(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2634
_cell_measurement_temperature    190.0
_cell_measurement_theta_max      27.470
_cell_measurement_theta_min      4.593
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.150
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1208 before and 0.0784 after correction. The Ratio of minimum to maximum transmission is 0.7523. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.401
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             310
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4307
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.581
_diffrn_reflns_theta_min         3.246
_diffrn_ambient_temperature      190.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                528
_reflns_number_total             555
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 
;
 Flack x determined using 222 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         555
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0283
_refine_ls_restrained_S_all      1.146
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+0.9522P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0605
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.78(8)
 0.22(8)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
3. Others
 Fixed Sof: H1B(0.5) H1C(0.5)
4.a Riding coordinates:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V -0.13337(7) -0.36663(7) -0.2262(3) 0.0093(2) Uani 1 2 d S T P . .
V1 V 0.0000 0.0000 -0.2299(4) 0.0108(3) Uani 1 4 d S T P . .
O4 O -0.1302(4) -0.3698(4) 0.0687(9) 0.0166(10) Uani 1 2 d S T P . .
O3 O 0.0000 -0.5000 -0.3410(13) 0.0189(16) Uani 1 4 d S T P . .
O2 O -0.0852(4) -0.1933(4) -0.3338(8) 0.0217(8) Uani 1 1 d . . . . .
O1 O 0.0000 0.0000 0.0576(14) 0.0232(17) Uani 1 4 d S T P . .
N1 N -0.3298(5) -0.1702(5) 0.3044(13) 0.0200(14) Uani 1 2 d S T P . .
H1A H -0.3829 -0.1171 0.1931 0.024 Uiso 1 2 d R U P . .
H1B H -0.3945 -0.2239 0.3980 0.024 Uiso 0.5 1 d R U P . .
H1C H -0.2761 -0.1055 0.3980 0.024 Uiso 0.5 1 d R U P . .
H1D H -0.269(10) -0.231(10) 0.23(3) 0.06(4) Uiso 1 2 d S . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V2 0.0080(3) 0.0080(3) 0.0119(4) 0.0009(6) -0.0009(6) -0.0009(3)
V1 0.0079(4) 0.0079(4) 0.0165(7) 0.000 0.000 0.000
O4 0.0199(16) 0.0199(16) 0.010(2) -0.0015(14) 0.0015(14) 0.003(2)
O3 0.021(2) 0.021(2) 0.015(4) 0.000 0.000 0.008(3)
O2 0.025(2) 0.0122(18) 0.0282(18) 0.0046(15) -0.0077(16) -0.0084(16)
O1 0.027(3) 0.027(3) 0.015(4) 0.000 0.000 0.000
N1 0.0250(17) 0.0250(17) 0.010(4) -0.0008(18) 0.0008(18) 0.009(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
V2 O4 1.641(5) . ?
V2 O3 1.792(3) . ?
V2 O2 1.706(4) . ?
V2 O2 1.706(4) 7_445 ?
V1 O2 1.962(4) 4 ?
V1 O2 1.962(4) 3 ?
V1 O2 1.962(4) 2 ?
V1 O2 1.962(4) . ?
V1 O1 1.600(8) . ?
O3 V2 1.792(3) 2_545 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9102 . ?
N1 H1C 0.9097 . ?
N1 H1D 0.88(14) . ?

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 V2 O3 109.5(3) . . ?
O4 V2 O2 111.23(19) . 7_445 ?
O4 V2 O2 111.23(19) . . ?
O2 V2 O3 107.8(2) 7_445 . ?
O2 V2 O3 107.8(2) . . ?
O2 V2 O2 109.2(3) 7_445 . ?
O2 V1 O2 85.02(8) 2 3 ?
O2 V1 O2 85.02(8) 2 4 ?
O2 V1 O2 85.02(8) . 4 ?
O2 V1 O2 85.02(8) . 3 ?
O2 V1 O2 145.7(3) 2 . ?
O2 V1 O2 145.7(3) 4 3 ?
O1 V1 O2 107.14(14) . 3 ?
O1 V1 O2 107.14(14) . 4 ?
O1 V1 O2 107.14(14) . 2 ?
O1 V1 O2 107.14(14) . . ?
V2 O3 V2 138.2(4) 2_545 . ?
V2 O2 V1 141.4(3) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1A N1 H1D 107.4 . . ?
H1B N1 H1C 109.5 . . ?
H1B N1 H1D 110.5 . . ?
H1C N1 H1D 110.5 . . ?

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
O4 V2 O3 V2 0.000(1) . . . 2_545 ?
O4 V2 O2 V1 11.4(5) . . . . ?
O3 V2 O2 V1 -108.6(4) . . . . ?
O2 V2 O3 V2 -121.13(17) 7_445 . . 2_545 ?
O2 V2 O3 V2 121.13(17) . . . 2_545 ?
O2 V2 O2 V1 134.6(2) 7_445 . . . ?

_shelx_res_file                  
;
    k-1.res created by SHELXL-2014/7

TITL K-1 in P4bm
CELL 0.71073 8.8761 8.8761 5.5632 90 90 90
ZERR 2 0.0004 0.0004 0.0006 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,+Z
SYMM 0.5-Y,0.5-X,+Z
SYMM 0.5+Y,0.5+X,+Z
SFAC H N O V
UNIT 16 4 16 6

L.S. 4
PLAN  1
TEMP -83.15
CONF
BOND
fmap 2
acta
MORE -1
BOND $H
TWIN 1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\K-1.hkl">
REM </olex2.extras>

WGHT    0.000000    0.952200
BASF   0.21673
FVAR       0.24677
V2    4   -0.133368   -0.366632   -0.226161    10.50000    0.00804    0.00804 =
         0.01187    0.00087   -0.00087   -0.00088
V1    4    0.000000    0.000000   -0.229922    10.25000    0.00790    0.00790 =
         0.01646    0.00000    0.00000    0.00000
O4    3   -0.130232   -0.369768    0.068665    10.50000    0.01992    0.01992 =
         0.01009   -0.00155    0.00155    0.00265
O3    3    0.000000   -0.500000   -0.341034    10.25000    0.02062    0.02062 =
         0.01543    0.00000    0.00000    0.00844
O2    3   -0.085191   -0.193284   -0.333847    11.00000    0.02478    0.01223 =
         0.02824    0.00463   -0.00765   -0.00839
O1    3    0.000000    0.000000    0.057595    10.25000    0.02727    0.02727 =
         0.01508    0.00000    0.00000    0.00000
N1    2   -0.329774   -0.170226    0.304358    10.50000    0.02499    0.02499 =
         0.01005   -0.00082    0.00082    0.00938
AFIX   3
H1A   1   -0.382915   -0.117090    0.193078    10.50000   -1.20000
H1B   1   -0.394504   -0.223920    0.397958    10.50000   -1.20000
H1C   1   -0.276134   -0.105540    0.397958    10.50000   -1.20000
AFIX   0
H1D   1   -0.268617   -0.231383    0.225418    10.50000    0.06373
HKLF 4

REM  K-1 in P4bm
REM R1 =  0.0283 for     528 Fo > 4sig(Fo)  and  0.0313 for all     555 data
REM     42 parameters refined using      1 restraints

END

WGHT      0.0000      0.9529

REM Highest difference peak  0.433,  deepest hole -0.376,  1-sigma level  0.089
Q1    1  -0.0420 -0.3598 -0.2235  11.00000  0.05    0.43
;
_shelx_res_checksum              90281
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.78(8)
2 0.22(8)

####################################################################### 
# 
# 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_160k
_database_code_depnum_ccdc_archive 'CCDC 2004936'
loop_
_audit_author_name
_audit_author_address
'zhiyuan Yao'
;Nanjing Tech university
China
;
_audit_update_record             
;
2020-05-21 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_audit_creation_date             2019-11-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'O8 V3, 0.5(H16 N4)'
_chemical_formula_sum            'H8 N2 O8 V3'
_chemical_formula_weight         316.90
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   8.8669(4)
_cell_length_b                   8.8669(4)
_cell_length_c                   5.5650(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     437.53(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2564
_cell_measurement_temperature    160.0
_cell_measurement_theta_max      27.479
_cell_measurement_theta_min      4.598
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.156
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1235 before and 0.0796 after correction. The Ratio of minimum to maximum transmission is 0.7445. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.405
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             310
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4267
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.574
_diffrn_reflns_theta_min         3.249
_diffrn_ambient_temperature      160.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                527
_reflns_number_total             556
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 
;
 Flack x determined using 220 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         556
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0316
_refine_ls_restrained_S_all      1.156
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+1.2178P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0672
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.80(9)
 0.20(9)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
3. Restrained distances
 N1-H1D
 0.9 with sigma of 0.02
4. Others
 Fixed Sof: H1B(0.5) H1C(0.5)
5.a Riding coordinates:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V 0.36665(8) -0.13335(8) 0.7297(3) 0.0097(3) Uani 1 2 d S T P . .
V1 V 0.0000 0.0000 0.7262(5) 0.0113(3) Uani 1 4 d S T P . .
O4 O 0.3700(4) -0.1300(4) 1.0237(10) 0.0159(11) Uani 1 2 d S T P . .
O1 O 0.0000 0.0000 1.0135(15) 0.0235(19) Uani 1 4 d S T P . .
O3 O 0.5000 0.0000 0.6150(14) 0.0207(18) Uani 1 4 d S T P . .
O2 O 0.1930(5) -0.0853(5) 0.6222(9) 0.0236(9) Uani 1 1 d . . . . .
N1 N 0.1704(5) -0.3296(5) 1.2598(15) 0.0196(15) Uani 1 2 d DS T P . .
H1A H 0.1172 -0.3828 1.1487 0.024 Uiso 1 2 d R U P . .
H1B H 0.2241 -0.3942 1.3534 0.024 Uiso 0.5 1 d R U P . .
H1C H 0.1056 -0.2757 1.3534 0.024 Uiso 0.5 1 d R U P . .
H1D H 0.234(6) -0.266(6) 1.18(2) 0.07(4) Uiso 1 2 d DS . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V2 0.0089(3) 0.0089(3) 0.0113(5) -0.0016(6) -0.0016(6) 0.0013(4)
V1 0.0080(4) 0.0080(4) 0.0177(8) 0.000 0.000 0.000
O4 0.0193(18) 0.0193(18) 0.009(2) 0.0008(15) 0.0008(15) -0.004(2)
O1 0.027(3) 0.027(3) 0.017(4) 0.000 0.000 0.000
O3 0.025(3) 0.025(3) 0.013(4) 0.000 0.000 -0.009(4)
O2 0.013(2) 0.030(2) 0.028(2) -0.0119(19) -0.0066(17) 0.0102(18)
N1 0.0240(19) 0.0240(19) 0.011(4) 0.001(2) 0.001(2) -0.008(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
V2 O4 1.637(6) . ?
V2 O3 1.790(3) . ?
V2 O2 1.706(4) . ?
V2 O2 1.706(4) 8_545 ?
V1 O1 1.599(9) . ?
V1 O2 1.959(4) . ?
V1 O2 1.959(4) 2 ?
V1 O2 1.959(4) 3 ?
V1 O2 1.959(4) 4 ?
O3 V2 1.790(3) 2_655 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9089 . ?
N1 H1C 0.9109 . ?
N1 H1D 0.90(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 V2 O3 109.4(3) . . ?
O4 V2 O2 111.2(2) . 8_545 ?
O4 V2 O2 111.2(2) . . ?
O2 V2 O3 107.8(2) . . ?
O2 V2 O3 107.8(2) 8_545 . ?
O2 V2 O2 109.2(3) 8_545 . ?
O1 V1 O2 107.18(16) . 3 ?
O1 V1 O2 107.18(16) . 2 ?
O1 V1 O2 107.18(16) . . ?
O1 V1 O2 107.18(16) . 4 ?
O2 V1 O2 85.00(9) . 3 ?
O2 V1 O2 84.99(9) 3 2 ?
O2 V1 O2 84.99(9) 4 2 ?
O2 V1 O2 84.99(9) . 4 ?
O2 V1 O2 145.6(3) . 2 ?
O2 V1 O2 145.6(3) 4 3 ?
V2 O3 V2 138.2(5) 2_655 . ?
V2 O2 V1 141.4(3) . . ?
H1A N1 H1B 109.6 . . ?
H1A N1 H1C 109.5 . . ?
H1A N1 H1D 108.7 . . ?
H1B N1 H1C 109.5 . . ?
H1B N1 H1D 109.8 . . ?
H1C N1 H1D 109.7 . . ?

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
O4 V2 O3 V2 0.000(0) . . . 2_655 ?
O4 V2 O2 V1 11.5(5) . . . . ?
O3 V2 O2 V1 -108.5(5) . . . . ?
O2 V2 O3 V2 -121.12(18) 8_545 . . 2_655 ?
O2 V2 O3 V2 121.12(18) . . . 2_655 ?
O2 V2 O2 V1 134.6(3) 8_545 . . . ?

_shelx_res_file                  
;
    160k.res created by SHELXL-2014/7

TITL 160K in P4bm
CELL 0.71073 8.8669 8.8669 5.565 90 90 90
ZERR 2 0.0004 0.0004 0.0006 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,+Z
SYMM 0.5-Y,0.5-X,+Z
SYMM 0.5+Y,0.5+X,+Z
SFAC H N O V
UNIT 16 4 16 6
DFIX 0.9 N1 H1d

L.S. 20
PLAN  1
TEMP -113.15
CONF
MORE -1
BOND $H
fmap 2
acta
TWIN 1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\160K.hkl">
REM </olex2.extras>

WGHT    0.000000    1.217800
BASF   0.20110
FVAR       0.78154
V2    4    0.366646   -0.133354    0.729661    10.50000    0.00885    0.00885 =
         0.01135   -0.00159   -0.00159    0.00131
V1    4    0.000000    0.000000    0.726189    10.25000    0.00805    0.00805 =
         0.01769    0.00000    0.00000    0.00000
O4    3    0.369992   -0.130008    1.023719    10.50000    0.01934    0.01934 =
         0.00912    0.00084    0.00084   -0.00386
O1    3    0.000000    0.000000    1.013466    10.25000    0.02673    0.02673 =
         0.01702    0.00000    0.00000    0.00000
O3    3    0.500000    0.000000    0.614970    10.25000    0.02475    0.02475 =
         0.01267    0.00000    0.00000   -0.00903
O2    3    0.193030   -0.085289    0.622230    11.00000    0.01276    0.03013 =
         0.02804   -0.01186   -0.00657    0.01024
N1    2    0.170398   -0.329602    1.259826    10.50000    0.02396    0.02396 =
         0.01092    0.00096    0.00096   -0.00829
AFIX   3
H1A   1    0.117178   -0.382820    1.148656    10.50000   -1.20000
H1B   1    0.224138   -0.394180    1.353406    10.50000   -1.20000
H1C   1    0.105628   -0.275670    1.353406    10.50000   -1.20000
AFIX   0
H1D   1    0.233620   -0.266380    1.182685    10.50000    0.07487
HKLF 4

REM  160K in P4bm
REM R1 =  0.0316 for     527 Fo > 4sig(Fo)  and  0.0349 for all     556 data
REM     42 parameters refined using      2 restraints

END

WGHT      0.0000      1.2178

REM Highest difference peak  0.528,  deepest hole -0.410,  1-sigma level  0.099
Q1    1   0.3622 -0.0409  0.7326  11.00000  0.05    0.53
;
_shelx_res_checksum              77423
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.80(9)
2 0.20(9)

####################################################################### 
# 
# 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_200k-1
_database_code_depnum_ccdc_archive 'CCDC 2005052'
loop_
_audit_author_name
_audit_author_address
'zhiyuan Yao'
;Nanjing Tech university
China
;
_audit_update_record             
;
2020-05-21 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_audit_creation_date             2019-11-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'O8 V3, 0.5(H16 N4)'
_chemical_formula_sum            'H8 N2 O8 V3'
_chemical_formula_weight         316.90
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   8.8776(4)
_cell_length_b                   8.8776(4)
_cell_length_c                   5.5610(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     438.27(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2666
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      27.480
_cell_measurement_theta_min      4.592
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.151
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1208 before and 0.0781 after correction. The Ratio of minimum to maximum transmission is 0.7598. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.401
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             310
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4316
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.591
_diffrn_reflns_theta_min         3.245
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                525
_reflns_number_total             555
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 
;
 Flack x determined using 224 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         555
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0288
_refine_ls_restrained_S_all      1.140
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+1.1105P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0628
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.80(9)
 0.20(9)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
3. Restrained distances
 N1-H1D
 0.9 with sigma of 0.02
4. Others
 Fixed Sof: H1B(0.5) H1C(0.5)
5.a Riding coordinates:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V -0.13341(7) -0.36659(7) -0.7708(3) 0.0090(2) Uani 1 2 d S T P . .
V1 V 0.0000 0.0000 -0.7744(4) 0.0104(3) Uani 1 4 d S T P . .
N1 N -0.3297(5) -0.1703(5) -0.2406(15) 0.0208(15) Uani 1 2 d DS T P . .
H1A H -0.3827 -0.1172 -0.3522 0.025 Uiso 1 2 d R U P . .
H1B H -0.3945 -0.2228 -0.1470 0.025 Uiso 0.5 1 d R U P . .
H1C H -0.2761 -0.1044 -0.1470 0.025 Uiso 0.5 1 d R U P . .
O2 O -0.0854(4) -0.1931(4) -0.8784(8) 0.0205(8) Uani 1 1 d . . . . .
O1 O 0.0000 0.0000 -0.4872(14) 0.0228(17) Uani 1 4 d S T P . .
O4 O -0.1302(4) -0.3698(4) -0.4763(9) 0.0170(11) Uani 1 2 d S T P . .
O3 O 0.0000 -0.5000 -0.8852(13) 0.0166(15) Uani 1 4 d S T P . .
H1D H -0.268(6) -0.232(6) -0.32(2) 0.06(4) Uiso 1 2 d DS . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V2 0.0075(3) 0.0075(3) 0.0122(5) 0.0009(6) -0.0009(6) -0.0007(3)
V1 0.0078(4) 0.0078(4) 0.0155(7) 0.000 0.000 0.000
N1 0.0247(18) 0.0247(18) 0.013(4) -0.0017(19) 0.0017(19) 0.010(2)
O2 0.022(2) 0.0111(18) 0.0283(19) 0.0038(16) -0.0076(16) -0.0072(16)
O1 0.027(3) 0.027(3) 0.014(4) 0.000 0.000 0.000
O4 0.0204(17) 0.0204(17) 0.010(2) -0.0010(15) 0.0010(15) 0.004(2)
O3 0.018(2) 0.018(2) 0.014(4) 0.000 0.000 0.007(3)

_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
V2 O2 1.706(4) . ?
V2 O2 1.706(4) 7_445 ?
V2 O4 1.638(5) . ?
V2 O3 1.792(3) . ?
V1 O2 1.961(4) 2 ?
V1 O2 1.961(4) . ?
V1 O2 1.961(4) 3 ?
V1 O2 1.961(4) 4 ?
V1 O1 1.597(8) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9050 . ?
N1 H1C 0.9162 . ?
N1 H1D 0.90(3) . ?
O3 V2 1.792(3) 2_545 ?

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
O2 V2 O2 109.2(3) 7_445 . ?
O2 V2 O3 107.9(2) 7_445 . ?
O2 V2 O3 107.9(2) . . ?
O4 V2 O2 111.2(2) . . ?
O4 V2 O2 111.2(2) . 7_445 ?
O4 V2 O3 109.4(3) . . ?
O2 V1 O2 85.02(8) 2 4 ?
O2 V1 O2 145.7(3) 4 3 ?
O2 V1 O2 85.02(8) 2 3 ?
O2 V1 O2 145.7(3) 2 . ?
O2 V1 O2 85.02(8) 4 . ?
O2 V1 O2 85.02(8) 3 . ?
O1 V1 O2 107.14(14) . . ?
O1 V1 O2 107.14(14) . 3 ?
O1 V1 O2 107.14(14) . 2 ?
O1 V1 O2 107.14(14) . 4 ?
H1A N1 H1B 109.3 . . ?
H1A N1 H1C 109.0 . . ?
H1A N1 H1D 106.3 . . ?
H1B N1 H1C 109.4 . . ?
H1B N1 H1D 111.5 . . ?
H1C N1 H1D 111.3 . . ?
V2 O2 V1 141.5(3) . . ?
V2 O3 V2 138.4(4) 2_545 . ?

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
O2 V2 O2 V1 134.7(2) 7_445 . . . ?
O2 V2 O3 V2 121.09(17) . . . 2_545 ?
O2 V2 O3 V2 -121.09(17) 7_445 . . 2_545 ?
O4 V2 O2 V1 11.6(5) . . . . ?
O4 V2 O3 V2 0.000(2) . . . 2_545 ?
O3 V2 O2 V1 -108.4(4) . . . . ?

_shelx_res_file                  
;
    200k-1.res created by SHELXL-2014/7

TITL 200K-1 in P4bm
CELL 0.71073 8.8776 8.8776 5.561 90 90 90
ZERR 2 0.0004 0.0004 0.0006 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,+Z
SYMM 0.5-Y,0.5-X,+Z
SYMM 0.5+Y,0.5+X,+Z
SFAC H N O V
UNIT 16 4 16 6
DFIX 0.9 N1 H1d

L.S. 4
PLAN  1
TEMP -73.15
CONF
BOND
MORE -1
BOND $H
fmap 2
acta
TWIN 1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\200K-1.hkl">
REM </olex2.extras>

WGHT    0.000000    1.110500
BASF   0.20193
FVAR       0.82948
V2    4   -0.133412   -0.366588   -0.770808    10.50000    0.00747    0.00747 =
         0.01217    0.00090   -0.00090   -0.00070
V1    4    0.000000    0.000000   -0.774422    10.25000    0.00778    0.00778 =
         0.01552    0.00000    0.00000    0.00000
N1    2   -0.329716   -0.170284   -0.240624    10.50000    0.02471    0.02471 =
         0.01282   -0.00172    0.00172    0.01013
AFIX   3
H1A   1   -0.382746   -0.117250   -0.352164    10.50000   -1.20000
H1B   1   -0.394506   -0.222760   -0.146994    10.50000   -1.20000
H1C   1   -0.276146   -0.104400   -0.146994    10.50000   -1.20000
AFIX   0

O2    3   -0.085362   -0.193103   -0.878363    11.00000    0.02203    0.01110 =
         0.02827    0.00384   -0.00762   -0.00724
O1    3    0.000000    0.000000   -0.487211    10.25000    0.02725    0.02725 =
         0.01390    0.00000    0.00000    0.00000
O4    3   -0.130229   -0.369771   -0.476289    10.50000    0.02036    0.02036 =
         0.01034   -0.00102    0.00102    0.00377
O3    3    0.000000   -0.500000   -0.885184    10.25000    0.01778    0.01778 =
         0.01420    0.00000    0.00000    0.00723
H1D   1   -0.268069   -0.231931   -0.323241    10.50000    0.06347
HKLF 4

REM  200K-1 in P4bm
REM R1 =  0.0288 for     525 Fo > 4sig(Fo)  and  0.0330 for all     555 data
REM     42 parameters refined using      2 restraints

END

WGHT      0.0000      1.1105

REM Highest difference peak  0.478,  deepest hole -0.493,  1-sigma level  0.093
Q1    1  -0.0397 -0.3777 -0.7668  11.00000  0.05    0.48
;
_shelx_res_checksum              2388
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.80(9)
2 0.20(9)

####################################################################### 
# 
# 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_120k
_database_code_depnum_ccdc_archive 'CCDC 2004673'
loop_
_audit_author_name
_audit_author_address
'zhiyuan Yao'
;Nanjing Tech university
China
;
_audit_update_record             
;
2020-05-19 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_audit_creation_date             2019-11-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'O8 V3, 0.5(H16 N4)'
_chemical_formula_sum            'H8 N2 O8 V3'
_chemical_formula_weight         316.90
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   8.8572(3)
_cell_length_b                   8.8572(3)
_cell_length_c                   5.5653(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     436.60(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2549
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.511
_cell_measurement_theta_min      4.603
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.163
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1228 before and 0.0802 after correction. The Ratio of minimum to maximum transmission is 0.7359. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.411
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             310
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4273
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.574
_diffrn_reflns_theta_min         3.253
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                531
_reflns_number_total             555
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 
;
 Flack x determined using 217 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         555
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0335
_refine_ls_restrained_S_all      1.179
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+1.2576P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0692
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.20(9)
 0.80(9)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
3. Restrained distances
 N1-H1D
 0.9 with sigma of 0.02
4. Others
 Fixed Sof: H1B(0.5) H1C(0.5)
5.a Riding coordinates:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V -0.13335(8) -0.36665(8) -0.4618(3) 0.0096(3) Uani 1 2 d S T P . .
V1 V 0.0000 0.0000 -0.4586(5) 0.0122(4) Uani 1 4 d S T P . .
O2 O -0.0856(5) -0.1929(5) -0.3547(9) 0.0263(10) Uani 1 1 d . . . . .
O4 O -0.1297(4) -0.3703(4) -0.7562(10) 0.0146(11) Uani 1 2 d S T P . .
O1 O 0.0000 0.0000 -0.7440(17) 0.0236(19) Uani 1 4 d S T P . .
O3 O 0.0000 -0.5000 -0.3476(14) 0.022(2) Uani 1 4 d S T P . .
N1 N -0.3297(5) -0.1703(5) -0.9915(17) 0.0184(16) Uani 1 2 d DS T P . .
H1A H -0.3192 -0.1808 -1.1533 0.022 Uiso 1 2 d R U P . .
H1B H -0.4264 -0.1929 -0.9488 0.022 Uiso 0.5 1 d R U P . .
H1C H -0.3078 -0.0743 -0.9488 0.022 Uiso 0.5 1 d R U P . .
H1D H -0.260(4) -0.240(4) -0.96(4) 0.09(4) Uiso 1 2 d DS . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V2 0.0092(3) 0.0092(3) 0.0105(5) -0.0025(7) 0.0025(7) -0.0019(4)
V1 0.0086(4) 0.0086(4) 0.0195(8) 0.000 0.000 0.000
O2 0.037(3) 0.016(2) 0.027(2) -0.0077(18) 0.014(2) -0.014(2)
O4 0.0180(18) 0.0180(18) 0.008(2) 0.0000(15) 0.0000(15) 0.008(2)
O1 0.026(3) 0.026(3) 0.019(5) 0.000 0.000 0.000
O3 0.028(3) 0.028(3) 0.010(4) 0.000 0.000 0.008(4)
N1 0.0214(19) 0.0214(19) 0.012(4) -0.003(2) 0.003(2) 0.005(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
V2 O2 1.703(4) . ?
V2 O2 1.703(4) 7_445 ?
V2 O4 1.639(6) . ?
V2 O3 1.787(3) . ?
V1 O2 1.957(4) . ?
V1 O2 1.957(4) 4 ?
V1 O2 1.957(4) 3 ?
V1 O2 1.957(4) 2 ?
V1 O1 1.589(9) . ?
O3 V2 1.787(3) 2_545 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9113 . ?
N1 H1C 0.9039 . ?
N1 H1D 0.90(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 V2 O2 109.0(3) 7_445 . ?
O2 V2 O3 108.0(2) 7_445 . ?
O2 V2 O3 108.0(2) . . ?
O4 V2 O2 111.3(2) . . ?
O4 V2 O2 111.3(2) . 7_445 ?
O4 V2 O3 109.2(3) . . ?
O2 V1 O2 145.6(3) . 2 ?
O2 V1 O2 84.99(9) 2 3 ?
O2 V1 O2 84.99(9) . 3 ?
O2 V1 O2 84.99(9) . 4 ?
O2 V1 O2 84.99(9) 2 4 ?
O2 V1 O2 145.6(3) 3 4 ?
O1 V1 O2 107.18(17) . 4 ?
O1 V1 O2 107.18(16) . 3 ?
O1 V1 O2 107.18(17) . . ?
O1 V1 O2 107.18(17) . 2 ?
V2 O2 V1 141.4(3) . . ?
V2 O3 V2 138.3(5) 2_545 . ?
H1A N1 H1B 109.4 . . ?
H1A N1 H1C 109.6 . . ?
H1A N1 H1D 94.4 . . ?
H1B N1 H1C 109.9 . . ?
H1B N1 H1D 116.0 . . ?
H1C N1 H1D 116.2 . . ?

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
O2 V2 O2 V1 -134.8(3) 7_445 . . . ?
O2 V2 O3 V2 -121.14(19) . . . 2_545 ?
O2 V2 O3 V2 121.14(19) 7_445 . . 2_545 ?
O4 V2 O2 V1 -11.7(6) . . . . ?
O4 V2 O3 V2 0.000(1) . . . 2_545 ?
O3 V2 O2 V1 108.1(5) . . . . ?

_shelx_res_file                  
;
    120k.res created by SHELXL-2014/7

TITL 120K in P4bm
CELL 0.71073 8.8572 8.8572 5.5653 90 90 90
ZERR 2 0.0003 0.0003 0.0005 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,+Z
SYMM 0.5-Y,0.5-X,+Z
SYMM 0.5+Y,0.5+X,+Z
SFAC H N O V
UNIT 16 4 16 6
DFIX 0.9 N1 H1d

L.S. 20
PLAN  1
TEMP -153.15
CONF
MORE -1
BOND $H
fmap 2
acta
TWIN 1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%120K.hkl">
REM </olex2.extras>

WGHT    0.000000    1.257600
BASF   0.79626
FVAR       0.24763
V2    4   -0.133351   -0.366649   -0.461809    10.50000    0.00916    0.00916 =
         0.01053   -0.00249    0.00249   -0.00185
V1    4    0.000000    0.000000   -0.458552    10.25000    0.00863    0.00863 =
         0.01948    0.00000    0.00000    0.00000
O2    3   -0.085640   -0.192927   -0.354666    11.00000    0.03666    0.01559 =
         0.02677   -0.00768    0.01352   -0.01372
O4    3   -0.129713   -0.370287   -0.756234    10.50000    0.01802    0.01802 =
         0.00771   -0.00002    0.00002    0.00787
O1    3    0.000000    0.000000   -0.743988    10.25000    0.02607    0.02607 =
         0.01871    0.00000    0.00000    0.00000
O3    3    0.000000   -0.500000   -0.347634    10.25000    0.02826    0.02826 =
         0.01013    0.00000    0.00000    0.00789
N1    2   -0.329732   -0.170268   -0.991546    10.50000    0.02137    0.02137 =
         0.01248   -0.00294    0.00294    0.00514
AFIX   3
H1A   1   -0.319222   -0.180780   -1.153346    10.50000   -1.20000
H1B   1   -0.426432   -0.192920   -0.948776    10.50000   -1.20000
H1C   1   -0.307812   -0.074290   -0.948776    10.50000   -1.20000
AFIX   0
H1D   1   -0.259584   -0.240416   -0.955774    10.50000    0.09103
HKLF 4

REM  120K in P4bm
REM R1 =  0.0335 for     531 Fo > 4sig(Fo)  and  0.0367 for all     555 data
REM     42 parameters refined using      2 restraints

END

WGHT      0.0000      1.2576

REM Highest difference peak  0.515,  deepest hole -0.530,  1-sigma level  0.103
Q1    1  -0.0353 -0.3820 -0.4615  11.00000  0.05    0.51
;
_shelx_res_checksum              24415
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.20(9)
2 0.80(9)

####################################################################### 
# 
# 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_140k
_database_code_depnum_ccdc_archive 'CCDC 2004617'
loop_
_audit_author_name
_audit_author_address
'zhiyuan Yao'
;Nanjing Tech university
China
;
_audit_update_record             
;
2020-05-20 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_audit_creation_date             2019-11-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'O8 V3, 0.5(H16 N4)'
_chemical_formula_sum            'H8 N2 O8 V3'
_chemical_formula_weight         316.90
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   8.8620(4)
_cell_length_b                   8.8620(4)
_cell_length_c                   5.5652(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     437.06(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2541
_cell_measurement_temperature    140.0
_cell_measurement_theta_max      27.494
_cell_measurement_theta_min      4.600
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.159
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1229 before and 0.0792 after correction. The Ratio of minimum to maximum transmission is 0.7389. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.408
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             310
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4273
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.574
_diffrn_reflns_theta_min         3.251
_diffrn_ambient_temperature      140.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                526
_reflns_number_total             555
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 
;
 Flack x determined using 219 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         555
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0311
_refine_ls_restrained_S_all      1.163
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+1.1358P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0657
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.78(9)
 0.22(9)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
3. Restrained distances
 N1-H1D
 0.9 with sigma of 0.02
4. Others
 Fixed Sof: H1B(0.5) H1C(0.5)
5.a Riding coordinates:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V -0.36674(8) -0.13326(8) -0.6259(3) 0.0095(3) Uani 1 2 d S T P . .
V1 V 0.0000 0.0000 -0.6294(5) 0.0117(3) Uani 1 4 d S T P . .
N1 N -0.1703(5) -0.3297(5) -0.0954(15) 0.0177(15) Uani 1 2 d DS T P . .
H1A H -0.1170 -0.3830 -0.2065 0.021 Uiso 1 2 d R U P . .
H1B H -0.1055 -0.2760 -0.0018 0.021 Uiso 0.5 1 d R U P . .
H1C H -0.2240 -0.3946 -0.0018 0.021 Uiso 0.5 1 d R U P . .
O4 O -0.3700(4) -0.1300(4) -0.3313(10) 0.0152(11) Uani 1 2 d S T P . .
O1 O 0.0000 0.0000 -0.3419(15) 0.0224(18) Uani 1 4 d S T P . .
O3 O -0.5000 0.0000 -0.7407(14) 0.0215(18) Uani 1 4 d S T P . .
O2 O -0.1933(5) -0.0853(5) -0.7337(9) 0.0247(9) Uani 1 1 d . . . . .
H1D H -0.232(5) -0.268(5) -0.180(19) 0.05(4) Uiso 1 2 d DS . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V2 0.0090(3) 0.0090(3) 0.0107(5) -0.0021(6) 0.0021(6) -0.0013(4)
V1 0.0084(4) 0.0084(4) 0.0183(8) 0.000 0.000 0.000
N1 0.0206(18) 0.0206(18) 0.012(4) -0.0004(19) 0.0004(19) 0.008(2)
O4 0.0187(17) 0.0187(17) 0.008(2) -0.0004(15) 0.0004(15) 0.004(2)
O1 0.025(3) 0.025(3) 0.017(4) 0.000 0.000 0.000
O3 0.027(3) 0.027(3) 0.011(4) 0.000 0.000 0.008(4)
O2 0.014(2) 0.032(2) 0.028(2) -0.0141(19) 0.0082(17) -0.0126(19)

_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
V2 O4 1.640(5) . ?
V2 O3 1.788(3) . ?
V2 O2 1.704(4) 7_445 ?
V2 O2 1.704(4) . ?
V1 O1 1.600(8) . ?
V1 O2 1.960(4) 2 ?
V1 O2 1.960(4) . ?
V1 O2 1.960(4) 4 ?
V1 O2 1.960(4) 3 ?
N1 H1A 0.9101 . ?
N1 H1B 0.9099 . ?
N1 H1C 0.9100 . ?
N1 H1D 0.90(3) . ?
O3 V2 1.788(3) 2_455 ?

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 V2 O3 109.5(3) . . ?
O4 V2 O2 111.3(2) . . ?
O4 V2 O2 111.3(2) . 7_445 ?
O2 V2 O3 107.8(2) 7_445 . ?
O2 V2 O3 107.8(2) . . ?
O2 V2 O2 109.0(3) . 7_445 ?
O1 V1 O2 107.23(15) . 4 ?
O1 V1 O2 107.23(15) . . ?
O1 V1 O2 107.23(15) . 2 ?
O1 V1 O2 107.23(15) . 3 ?
O2 V1 O2 84.97(9) 2 4 ?
O2 V1 O2 84.97(9) 4 . ?
O2 V1 O2 84.97(9) 3 . ?
O2 V1 O2 84.97(9) 2 3 ?
O2 V1 O2 145.5(3) 2 . ?
O2 V1 O2 145.5(3) 3 4 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1A N1 H1D 105.8 . . ?
H1B N1 H1C 109.5 . . ?
H1B N1 H1D 111.3 . . ?
H1C N1 H1D 111.3 . . ?
V2 O3 V2 138.1(5) . 2_455 ?
V2 O2 V1 141.3(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
O4 V2 O3 V2 0.000(2) . . . 2_455 ?
O4 V2 O2 V1 -11.5(5) . . . . ?
O3 V2 O2 V1 108.6(5) . . . . ?
O2 V2 O3 V2 -121.24(18) . . . 2_455 ?
O2 V2 O3 V2 121.24(18) 7_445 . . 2_455 ?
O2 V2 O2 V1 -134.7(3) 7_445 . . . ?

_shelx_res_file                  
;
    140k.res created by SHELXL-2014/7

TITL 140K in P4bm
CELL 0.71073 8.862 8.862 5.5652 90 90 90
ZERR 2 0.0004 0.0004 0.0006 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,+Z
SYMM 0.5-Y,0.5-X,+Z
SYMM 0.5+Y,0.5+X,+Z
SFAC H N O V
UNIT 16 4 16 6
DFIX 0.9 N1 H1d

L.S. 20
PLAN  1
TEMP -133.15
CONF
BOND
MORE -1
BOND $H
fmap 2
acta
TWIN 1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\140K.hkl">
REM </olex2.extras>

WGHT    0.000000    1.135800
BASF   0.22338
FVAR       0.24757
V2    4   -0.366738   -0.133262   -0.625851    10.50000    0.00896    0.00896 =
         0.01071   -0.00215    0.00215   -0.00132
V1    4    0.000000    0.000000   -0.629368    10.25000    0.00843    0.00843 =
         0.01829    0.00000    0.00000    0.00000
N1    2   -0.170251   -0.329749   -0.095354    10.50000    0.02061    0.02061 =
         0.01192   -0.00037    0.00037    0.00850
AFIX   3
H1A   1   -0.116971   -0.383030   -0.206474    10.50000   -1.20000
H1B   1   -0.105461   -0.275980   -0.001774    10.50000   -1.20000
H1C   1   -0.224031   -0.394550   -0.001774    10.50000   -1.20000
AFIX   0

O4    3   -0.369985   -0.130015   -0.331330    10.50000    0.01866    0.01866 =
         0.00814   -0.00043    0.00043    0.00443
O1    3    0.000000    0.000000   -0.341923    10.25000    0.02505    0.02505 =
         0.01713    0.00000    0.00000    0.00000
O3    3   -0.500000    0.000000   -0.740692    10.25000    0.02654    0.02654 =
         0.01148    0.00000    0.00000    0.00779
O2    3   -0.193274   -0.085305   -0.733685    11.00000    0.01429    0.03219 =
         0.02763   -0.01407    0.00816   -0.01255
H1D   1   -0.231574   -0.268426   -0.179756    10.50000    0.05418
HKLF 4

REM  140K in P4bm
REM R1 =  0.0311 for     526 Fo > 4sig(Fo)  and  0.0353 for all     555 data
REM     42 parameters refined using      2 restraints

END

WGHT      0.0000      1.1358

REM Highest difference peak  0.477,  deepest hole -0.423,  1-sigma level  0.097
Q1    1  -0.3632 -0.0418 -0.6239  11.00000  0.05    0.48
;
_shelx_res_checksum              37948
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.78(9)
2 0.22(9)

####################################################################### 
# 
# 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_270k-1
_database_code_depnum_ccdc_archive 'CCDC 2004953'
loop_
_audit_author_name
_audit_author_address
'zhiyuan Yao'
;Nanjing Tech university
China
;
_audit_update_record             
;
2020-05-20 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(O16 V6), H8 N2'
_chemical_formula_sum            'H8 N2 O8 V3'
_chemical_formula_weight         316.90
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   8.8891(3)
_cell_length_b                   8.8891(3)
_cell_length_c                   5.5691(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     440.05(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2583
_cell_measurement_temperature    270(2)
_cell_measurement_theta_max      27.438
_cell_measurement_theta_min      4.586
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.138
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1195 before and 0.0769 after correction. The Ratio of minimum to maximum transmission is 0.7659. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.392
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             310
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4274
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.436
_diffrn_reflns_theta_min         3.241
_diffrn_ambient_temperature      270.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                527
_reflns_number_total             556
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 
;
 Flack x determined using 224 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         556
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0325
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+1.7111P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0697
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.17(10)
 0.83(10)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H,H) groups
3. Restrained distances
 N1-H1D
 0.9 with sigma of 0.02
4. Others
 Fixed Sof: H1B(0.5) H1C(0.5)
5.a Riding coordinates:
 N1(H1A,H1B,H1C), N1(H1D)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V -0.63352(8) -0.13352(8) -0.2142(4) 0.0105(3) Uani 1 2 d S T P . .
O4 O -0.6303(5) -0.1303(5) -0.5079(11) 0.0200(13) Uani 1 2 d S T P . .
O3 O -0.5000 0.0000 -0.1000(14) 0.0168(17) Uani 1 4 d S T P . .
O2 O -0.8071(5) -0.0857(5) -0.1071(9) 0.0210(9) Uani 1 1 d . . . . .
V1 V -1.0000 0.0000 -0.2106(5) 0.0118(3) Uani 1 4 d S T P . .
O1 O -1.0000 0.0000 -0.4968(17) 0.028(2) Uani 1 4 d S T P . .
N1 N -0.8306(5) -0.3306(5) -0.7443(18) 0.0277(19) Uani 1 2 d DS T P . .
H1A H -0.8206 -0.3205 -0.9025 0.033 Uiso 1 2 d RS T P . .
H1B H -0.8092 -0.4241 -0.7022 0.033 Uiso 0.5 1 d R . . . .
H1C H -0.9248 -0.3085 -0.7022 0.033 Uiso 0.5 1 d R . . . .
H1D H -0.7665 -0.2664 -0.6685 0.033 Uiso 1 2 d DRS T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V2 0.0080(3) 0.0080(3) 0.0155(5) 0.0006(7) 0.0006(7) 0.0004(4)
O4 0.024(2) 0.024(2) 0.012(3) -0.0020(17) -0.0020(17) -0.006(3)
O3 0.016(2) 0.016(2) 0.019(4) 0.000 0.000 -0.006(3)
O2 0.011(2) 0.018(2) 0.034(2) 0.0027(18) 0.0020(18) 0.0054(17)
V1 0.0089(4) 0.0089(4) 0.0175(8) 0.000 0.000 0.000
O1 0.034(3) 0.034(3) 0.017(5) 0.000 0.000 0.000
N1 0.032(2) 0.032(2) 0.019(5) 0.000(2) 0.000(2) -0.012(3)

_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
V2 O4 1.636(6) . ?
V2 O3 1.795(3) . ?
V2 O2 1.708(4) 8_455 ?
V2 O2 1.708(4) . ?
O3 V2 1.795(3) 2_455 ?
O2 V1 1.963(4) . ?
V1 O2 1.963(4) 4_445 ?
V1 O2 1.963(4) 2_355 ?
V1 O2 1.963(4) 3_465 ?
V1 O1 1.594(9) . ?
N1 H1A 0.8901 . ?
N1 H1B 0.8840 . ?
N1 H1C 0.8913 . ?
N1 H1D 0.9105 . ?

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 V2 O3 109.3(3) . . ?
O4 V2 O2 111.1(2) . 8_455 ?
O4 V2 O2 111.1(2) . . ?
O2 V2 O3 108.0(2) . . ?
O2 V2 O3 108.0(2) 8_455 . ?
O2 V2 O2 109.1(3) . 8_455 ?
V2 O3 V2 138.5(5) . 2_455 ?
V2 O2 V1 141.5(3) . . ?
O2 V1 O2 85.05(9) 4_445 . ?
O2 V1 O2 85.05(9) 4_445 2_355 ?
O2 V1 O2 145.8(3) 3_465 4_445 ?
O2 V1 O2 145.8(3) 2_355 . ?
O2 V1 O2 85.05(9) 3_465 2_355 ?
O2 V1 O2 85.05(9) 3_465 . ?
O1 V1 O2 107.09(16) . . ?
O1 V1 O2 107.09(16) . 4_445 ?
O1 V1 O2 107.09(16) . 3_465 ?
O1 V1 O2 107.09(16) . 2_355 ?
H1A N1 H1B 109.6 . . ?
H1A N1 H1C 109.4 . . ?
H1A N1 H1D 109.4 . . ?
H1B N1 H1C 109.9 . . ?
H1B N1 H1D 109.4 . . ?
H1C N1 H1D 109.1 . . ?

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
O4 V2 O3 V2 0.000(0) . . . 2_455 ?
O4 V2 O2 V1 -11.9(5) . . . . ?
O3 V2 O2 V1 108.0(5) . . . . ?
O2 V2 O3 V2 -121.0(2) . . . 2_455 ?
O2 V2 O3 V2 121.0(2) 8_455 . . 2_455 ?
O2 V2 O2 V1 -134.8(3) 8_455 . . . ?

_shelx_res_file                  
;
    270k-1.res created by SHELXL-2014/7

TITL 270K-1 in P4bm
CELL 0.71073 8.8891 8.8891 5.5691 90 90 90
ZERR 2 0.0003 0.0003 0.0005 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,+Z
SYMM 0.5-Y,0.5-X,+Z
SYMM 0.5+Y,0.5+X,+Z
SFAC H N O V
UNIT 16 4 16 6
DFIX 0.9 N1 H1d

L.S. 4
PLAN  1
TEMP -3.15
CONF
MORE -1
BOND $H
fmap 2
acta
TWIN 1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\270K-1.hkl">
REM </olex2.extras>

WGHT    0.000000    1.711100
BASF   0.83252
FVAR       0.26554
V2    4   -0.633518   -0.133518   -0.214158    10.50000    0.00804    0.00804 =
         0.01545    0.00063    0.00063    0.00039
O4    3   -0.630335   -0.130335   -0.507868    10.50000    0.02407    0.02407 =
         0.01181   -0.00198   -0.00198   -0.00598
O3    3   -0.500000    0.000000   -0.099988    10.25000    0.01594    0.01594 =
         0.01864    0.00000    0.00000   -0.00624
O2    3   -0.807083   -0.085683   -0.107065    11.00000    0.01076    0.01845 =
         0.03388    0.00274    0.00204    0.00545
V1    4   -1.000000    0.000000   -0.210635    10.25000    0.00889    0.00889 =
         0.01753    0.00000    0.00000    0.00000
O1    3   -1.000000    0.000000   -0.496810    10.25000    0.03435    0.03435 =
         0.01660    0.00000    0.00000    0.00000
N1    2   -0.830601   -0.330601   -0.744279    10.50000    0.03176    0.03176 =
         0.01944   -0.00042   -0.00042   -0.01202
AFIX   3
H1A   1   -0.820571   -0.320470   -0.902479    10.50000   -1.20000
H1B   1   -0.809171   -0.424070   -0.702229    10.50000   -1.20000
H1C   1   -0.924781   -0.308460   -0.702229    10.50000   -1.20000
AFIX   3
H1D   1   -0.766461   -0.266360   -0.668539    10.50000   -1.20000
AFIX   0
HKLF 4

REM  270K-1 in P4bm
REM R1 =  0.0325 for     527 Fo > 4sig(Fo)  and  0.0358 for all     556 data
REM     39 parameters refined using      2 restraints

END

WGHT      0.0000      1.4949

REM Highest difference peak  0.509,  deepest hole -0.491,  1-sigma level  0.101
Q1    1  -0.6121 -0.0356 -0.2131  11.00000  0.05    0.51
;
_shelx_res_checksum              57183
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.17(10)
2 0.83(10)

####################################################################### 
# 
# 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_220k-1
_database_code_depnum_ccdc_archive 'CCDC 2004952'
loop_
_audit_author_name
_audit_author_address
'zhiyuan Yao'
;Nanjing Tech university
China
;
_audit_update_record             
;
2020-05-21 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(O16 V6), H8 N2'
_chemical_formula_sum            'H8 N2 O8 V3'
_chemical_formula_weight         316.90
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   8.8868(3)
_cell_length_b                   8.8868(3)
_cell_length_c                   5.5606(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     439.15(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2705
_cell_measurement_temperature    220.0
_cell_measurement_theta_max      27.481
_cell_measurement_theta_min      4.588
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.144
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1185 before and 0.0766 after correction.
The Ratio of minimum to maximum transmission is 0.7712.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic blackish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.397
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             310
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4353
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         3.242
_diffrn_ambient_temperature      220.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                532
_reflns_number_total             556
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 
;
 Flack x determined using 225 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         556
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0269
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+0.8337P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0558
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.79(7)
 0.21(7)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
3. Restrained distances
 N1-H1D
 0.9 with sigma of 0.02
4. Others
 Fixed Sof: H1B(0.5) H1C(0.5)
5.a Riding coordinates:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V 0.13345(6) 0.36655(6) 0.5001(3) 0.0090(2) Uani 1 2 d S T P . .
V1 V 0.0000 0.0000 0.4960(4) 0.0100(3) Uani 1 4 d S T P . .
O4 O 0.1304(4) 0.3696(4) 0.7949(8) 0.0182(10) Uani 1 2 d S T P . .
O3 O 0.0000 0.5000 0.3859(11) 0.0153(13) Uani 1 4 d S T P . .
O2 O 0.0852(4) 0.1932(4) 0.3923(7) 0.0188(6) Uani 1 1 d . . . . .
O1 O 0.0000 0.0000 0.7835(12) 0.0229(15) Uani 1 4 d S T P . .
N1 N 0.3299(4) 0.1701(4) 1.0307(13) 0.0223(13) Uani 1 2 d DS T P . .
H1A H 0.3823 0.1177 0.9204 0.027 Uiso 1 2 d RS T P . .
H1B H 0.3939 0.2231 1.1233 0.027 Uiso 0.5 1 d R . . . .
H1C H 0.2769 0.1062 1.1233 0.027 Uiso 0.5 1 d R . . . .
H1D H 0.269(5) 0.231(5) 0.944(17) 0.07(3) Uiso 1 2 d DS T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V2 0.0071(3) 0.0071(3) 0.0127(4) -0.0003(5) 0.0003(5) -0.0005(3)
V1 0.0075(3) 0.0075(3) 0.0150(6) 0.000 0.000 0.000
O4 0.0212(15) 0.0212(15) 0.012(2) 0.0018(13) -0.0018(13) 0.0025(19)
O3 0.0153(19) 0.0153(19) 0.015(3) 0.000 0.000 0.007(2)
O2 0.0177(16) 0.0099(15) 0.0288(16) -0.0025(13) 0.0039(14) -0.0047(13)
O1 0.026(2) 0.026(2) 0.016(4) 0.000 0.000 0.000
N1 0.0270(17) 0.0270(17) 0.013(4) 0.0017(17) -0.0017(17) 0.012(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
V2 O4 1.640(5) . ?
V2 O3 1.793(2) . ?
V2 O2 1.707(3) . ?
V2 O2 1.707(3) 7 ?
V1 O2 1.963(3) 3 ?
V1 O2 1.963(3) 2 ?
V1 O2 1.963(3) 4 ?
V1 O2 1.963(3) . ?
V1 O1 1.598(7) . ?
O3 V2 1.793(2) 2_565 ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N1 H1C 0.9000 . ?
N1 H1D 0.90(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 V2 O3 109.4(2) . . ?
O4 V2 O2 111.21(17) . 7 ?
O4 V2 O2 111.21(17) . . ?
O2 V2 O3 107.84(17) 7 . ?
O2 V2 O3 107.84(18) . . ?
O2 V2 O2 109.2(2) 7 . ?
O2 V1 O2 85.05(7) . 4 ?
O2 V1 O2 145.8(2) . 2 ?
O2 V1 O2 85.05(7) 2 4 ?
O2 V1 O2 85.05(7) . 3 ?
O2 V1 O2 85.05(7) 2 3 ?
O2 V1 O2 145.8(2) 3 4 ?
O1 V1 O2 107.08(12) . 4 ?
O1 V1 O2 107.08(12) . 2 ?
O1 V1 O2 107.08(12) . 3 ?
O1 V1 O2 107.08(12) . . ?
V2 O3 V2 138.5(4) . 2_565 ?
V2 O2 V1 141.5(2) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1A N1 H1D 104.7 . . ?
H1B N1 H1C 109.5 . . ?
H1B N1 H1D 111.8 . . ?
H1C N1 H1D 111.8 . . ?

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
O4 V2 O3 V2 0.000(1) . . . 2_565 ?
O4 V2 O2 V1 11.5(4) . . . . ?
O3 V2 O2 V1 -108.4(4) . . . . ?
O2 V2 O3 V2 -121.07(15) 7 . . 2_565 ?
O2 V2 O3 V2 121.07(15) . . . 2_565 ?
O2 V2 O2 V1 134.6(2) 7 . . . ?

_shelx_res_file                  
;
    220k-1.res created by SHELXL-2014/7

TITL 220K-1 in P4bm
CELL 0.71073 8.8868 8.8868 5.5606 90 90 90
ZERR 2 0.0003 0.0003 0.0005 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,+Z
SYMM 0.5-Y,0.5-X,+Z
SYMM 0.5+Y,0.5+X,+Z
SFAC H N O V
UNIT 16 4 16 6
DFIX 0.9 N1 H1d

L.S. 15
PLAN  1
TEMP -53.15
CONF
BOND
MORE -1
BOND $H
fmap 2
acta
TWIN 1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\220K-1.hkl">
REM </olex2.extras>

WGHT    0.000000    0.833700
BASF   0.20905
FVAR       0.26303
V2    4    0.133455    0.366545    0.500080    10.50000    0.00712    0.00712 =
         0.01267   -0.00027    0.00027   -0.00045
V1    4    0.000000    0.000000    0.496012    10.25000    0.00747    0.00747 =
         0.01495    0.00000    0.00000    0.00000
O4    3    0.130385    0.369615    0.794883    10.50000    0.02121    0.02121 =
         0.01214    0.00179   -0.00179    0.00246
O3    3    0.000000    0.500000    0.385895    10.25000    0.01533    0.01533 =
         0.01523    0.00000    0.00000    0.00702
O2    3    0.085236    0.193224    0.392305    11.00000    0.01774    0.00993 =
         0.02876   -0.00250    0.00392   -0.00470
O1    3    0.000000    0.000000    0.783456    10.25000    0.02618    0.02618 =
         0.01625    0.00000    0.00000    0.00000
N1    2    0.329857    0.170143    1.030677    10.50000    0.02698    0.02698 =
         0.01291    0.00174   -0.00174    0.01211
AFIX   3
H1A   1    0.382267    0.117730    0.920397    10.50000   -1.20000
H1B   1    0.393857    0.223090    1.123287    10.50000   -1.20000
H1C   1    0.276917    0.106150    1.123287    10.50000   -1.20000
AFIX   0
H1D   1    0.269374    0.230626    0.943980    10.50000    0.06729
HKLF 4

REM  220K-1 in P4bm
REM R1 =  0.0269 for     532 Fo > 4sig(Fo)  and  0.0289 for all     556 data
REM     42 parameters refined using      2 restraints

END

WGHT      0.0000      0.8336

REM Highest difference peak  0.344,  deepest hole -0.391,  1-sigma level  0.081
Q1    1   0.0432  0.3473  0.5017  11.00000  0.05    0.34
;
_shelx_res_checksum              9278
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.79(7)
2 0.21(7)

####################################################################### 
# 
# 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_170k-1
_database_code_depnum_ccdc_archive 'CCDC 2005050'
loop_
_audit_author_name
_audit_author_address
'zhiyuan Yao'
;Nanjing Tech university
China
;
_audit_update_record             
;
2020-05-21 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(O16 V6), H8 N2'
_chemical_formula_sum            'H8 N2 O8 V3'
_chemical_formula_weight         316.90
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   8.8700(4)
_cell_length_b                   8.8700(4)
_cell_length_c                   5.5649(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     437.83(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2586
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      27.468
_cell_measurement_theta_min      4.596
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.154
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1229 before and 0.0793 after correction. The Ratio of minimum to maximum transmission is 0.7379. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.404
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             310
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4269
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.573
_diffrn_reflns_theta_min         3.248
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                527
_reflns_number_total             553
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 
;
 Flack x determined using 219 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         553
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0316
_refine_ls_restrained_S_all      1.166
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+1.2988P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0673
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.20(9)
 0.80(9)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
3. Restrained distances
 N1-H1D
 0.9 with sigma of 0.02
4. Others
 Fixed Sof: H1B(0.5) H1C(0.5)
5.a Riding coordinates:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V -1.0000 0.0000 -0.4016(5) 0.0112(3) Uani 1 4 d S T P . .
V2 V -1.36661(8) 0.13339(8) -0.4052(3) 0.0096(3) Uani 1 2 d S T P . .
O4 O -1.3699(4) 0.1301(4) -0.7000(10) 0.0156(11) Uani 1 2 d S T P . .
O1 O -1.0000 0.0000 -0.6880(16) 0.0242(19) Uani 1 4 d S T P . .
N1 N -1.1701(5) 0.3299(5) -0.9349(17) 0.0208(16) Uani 1 2 d DS T P . .
H1A H -1.1806 0.3194 -1.0967 0.025 Uiso 1 2 d RS T P . .
H1B H -1.1921 0.4257 -0.8921 0.025 Uiso 0.5 1 d R . . . .
H1C H -1.0736 0.3073 -0.8921 0.025 Uiso 0.5 1 d R . . . .
O3 O -1.5000 0.0000 -0.2909(14) 0.0196(18) Uani 1 4 d S T P . .
O2 O -1.1926(5) 0.0856(5) -0.2979(9) 0.0231(9) Uani 1 1 d . . . . .
H1D H -1.238(6) 0.262(6) -0.88(4) 0.10(5) Uiso 1 2 d DS T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0081(4) 0.0081(4) 0.0175(8) 0.000 0.000 0.000
V2 0.0087(3) 0.0087(3) 0.0115(5) -0.0015(7) -0.0015(7) 0.0013(4)
O4 0.0186(18) 0.0186(18) 0.010(2) 0.0010(15) 0.0010(15) -0.007(2)
O1 0.028(3) 0.028(3) 0.016(4) 0.000 0.000 0.000
N1 0.024(2) 0.024(2) 0.014(4) -0.001(2) -0.001(2) -0.008(2)
O3 0.021(3) 0.021(3) 0.017(4) 0.000 0.000 -0.007(3)
O2 0.012(2) 0.029(2) 0.028(2) -0.0089(19) -0.0059(17) 0.0104(18)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.594(9) . ?
V1 O2 1.957(4) 4_445 ?
V1 O2 1.957(4) 2_355 ?
V1 O2 1.957(4) 3_465 ?
V1 O2 1.957(4) . ?
V2 O4 1.641(6) . ?
V2 O3 1.790(3) . ?
V2 O2 1.708(4) 8_365 ?
V2 O2 1.708(4) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9042 . ?
N1 H1C 0.9113 . ?
N1 H1D 0.90(3) . ?
O3 V2 1.790(3) 2_255 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O2 107.16(16) . 4_445 ?
O1 V1 O2 107.16(16) . 3_465 ?
O1 V1 O2 107.16(16) . . ?
O1 V1 O2 107.16(16) . 2_355 ?
O2 V1 O2 85.01(9) 3_465 2_355 ?
O2 V1 O2 145.7(3) 4_445 3_465 ?
O2 V1 O2 85.01(9) 4_445 2_355 ?
O2 V1 O2 85.01(9) 3_465 . ?
O2 V1 O2 145.7(3) 2_355 . ?
O2 V1 O2 85.01(9) 4_445 . ?
O4 V2 O3 109.4(3) . . ?
O4 V2 O2 111.2(2) . 8_365 ?
O4 V2 O2 111.2(2) . . ?
O2 V2 O3 108.0(2) . . ?
O2 V2 O3 108.0(2) 8_365 . ?
O2 V2 O2 109.0(3) . 8_365 ?
H1A N1 H1B 109.6 . . ?
H1A N1 H1C 109.4 . . ?
H1A N1 H1D 100.3 . . ?
H1B N1 H1C 109.9 . . ?
H1B N1 H1D 113.7 . . ?
H1C N1 H1D 113.5 . . ?
V2 O3 V2 138.4(5) . 2_255 ?
V2 O2 V1 141.4(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
O4 V2 O3 V2 0.000(1) . . . 2_255 ?
O4 V2 O2 V1 -11.9(5) . . . . ?
O3 V2 O2 V1 108.0(5) . . . . ?
O2 V2 O3 V2 -121.12(19) . . . 2_255 ?
O2 V2 O3 V2 121.12(19) 8_365 . . 2_255 ?
O2 V2 O2 V1 -134.8(3) 8_365 . . . ?

_shelx_res_file                  
;
    170k-1.res created by SHELXL-2014/7

TITL 170K-1 in P4bm
CELL 0.71073 8.87 8.87 5.5649 90 90 90
ZERR 2 0.0004 0.0004 0.0006 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,+Z
SYMM 0.5-Y,0.5-X,+Z
SYMM 0.5+Y,0.5+X,+Z
SFAC H N O V
UNIT 16 4 16 6
DFIX 0.9 N1 H1d

L.S. 20
PLAN  6
TEMP -103.15
CONF
MORE -1
BOND $H
fmap 2
acta
TWIN 1 0 0 0 -1 0 0 0 -1 2
OMIT -3 -1 -1
OMIT 3 1 1
OMIT -3 -2 -1
OMIT 3 2 1
OMIT 0 0 3
OMIT 0 0 -3
REM <olex2.extras>
REM <HklSrc "%.\\170K-1.hkl">
REM </olex2.extras>

WGHT    0.000000    1.298800
BASF   0.79970
FVAR       0.24731
V1    4   -1.000000    0.000000   -0.401613    10.25000    0.00808    0.00808 =
         0.01753    0.00000    0.00000    0.00000
V2    4   -1.366609    0.133391   -0.405183    10.50000    0.00869    0.00869 =
         0.01154   -0.00149   -0.00149    0.00126
O4    3   -1.369949    0.130051   -0.700007    10.50000    0.01856    0.01856 =
         0.00969    0.00099    0.00099   -0.00682
O1    3   -1.000000    0.000000   -0.688034    10.25000    0.02830    0.02830 =
         0.01591    0.00000    0.00000    0.00000
N1    2   -1.170144    0.329856   -0.934901    10.50000    0.02415    0.02415 =
         0.01400   -0.00088   -0.00088   -0.00790
AFIX   3
H1A   1   -1.180584    0.319420   -1.096721    10.50000   -1.20000
H1B   1   -1.192054    0.425710   -0.892051    10.50000   -1.20000
H1C   1   -1.073594    0.307250   -0.892051    10.50000   -1.20000
AFIX   0

O3    3   -1.500000    0.000000   -0.290867    10.25000    0.02070    0.02070 =
         0.01729    0.00000    0.00000   -0.00703
O2    3   -1.192603    0.085647   -0.297871    11.00000    0.01247    0.02872 =
         0.02819   -0.00890   -0.00594    0.01038
H1D   1   -1.238281    0.261719   -0.883375    10.50000    0.09622
HKLF 4

REM  170K-1 in P4bm
REM R1 =  0.0316 for     527 Fo > 4sig(Fo)  and  0.0351 for all     553 data
REM     42 parameters refined using      2 restraints

END

WGHT      0.0000      1.3001

REM Highest difference peak  0.499,  deepest hole -0.465,  1-sigma level  0.100
Q1    1  -1.3865  0.0353 -0.4052  11.00000  0.05    0.50
Q2    1  -0.9902  0.1047 -0.4020  11.00000  0.05    0.37
Q3    1  -1.2179  0.0305 -0.4023  11.00000  0.05    0.35
Q4    1  -1.2350  0.3870 -1.0705  11.00000  0.05    0.35
Q5    1  -1.2931  0.0531 -0.2590  11.00000  0.05    0.34
Q6    1  -1.3681  0.2204 -0.4023  11.00000  0.05    0.33
;
_shelx_res_checksum              61842
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.20(9)
2 0.80(9)

####################################################################### 
# 
# 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_240k-1
_database_code_depnum_ccdc_archive 'CCDC 2005051'
loop_
_audit_author_name
_audit_author_address
'zhiyuan Yao'
;Nanjing Tech university
China
;
_audit_update_record             
;
2020-05-21 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(O16 V6), H8 N2'
_chemical_formula_sum            'H8 N2 O8 V3'
_chemical_formula_weight         316.90
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   8.8884(3)
_cell_length_b                   8.8884(3)
_cell_length_c                   5.5625(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     439.46(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2675
_cell_measurement_temperature    240.0
_cell_measurement_theta_max      27.471
_cell_measurement_theta_min      4.587
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.142
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1184 before and 0.0756 after correction. The Ratio of minimum to maximum transmission is 0.7565. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.395
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             310
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4362
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.470
_diffrn_reflns_theta_min         3.241
_diffrn_ambient_temperature      240.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                525
_reflns_number_total             555
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 
;
 Flack x determined using 224 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         555
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0279
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+0.9736P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0588
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.17(8)
 0.83(8)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H,H) groups
3. Others
 Fixed Sof: H1B(0.5) H1C(0.5)
4.a Riding coordinates:
 N1(H1A,H1B,H1C), N1(H1D)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V -0.13351(7) -0.63351(7) -0.4056(3) 0.0094(2) Uani 1 2 d S T P . .
N1 N -0.3306(4) -0.8306(4) -0.9354(14) 0.0245(15) Uani 1 2 d S T P . .
H1A H -0.3282 -0.8282 -1.0971 0.029 Uiso 1 2 d RS T P . .
H1B H -0.3066 -0.9250 -0.8839 0.029 Uiso 0.5 1 d R . . . .
H1C H -0.4235 -0.8081 -0.8839 0.029 Uiso 0.5 1 d R . . . .
H1D H -0.2624 -0.7624 -0.8752 0.029 Uiso 1 2 d RS T P . .
O4 O -0.1305(4) -0.6305(4) -0.7001(9) 0.0189(10) Uani 1 2 d S T P . .
V1 V 0.0000 -1.0000 -0.4015(4) 0.0105(3) Uani 1 4 d S T P . .
O1 O 0.0000 -1.0000 -0.6875(14) 0.0263(17) Uani 1 4 d S T P . .
O3 O 0.0000 -0.5000 -0.2916(12) 0.0158(14) Uani 1 4 d S T P . .
O2 O -0.0856(4) -0.8071(4) -0.2983(8) 0.0192(7) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V2 0.0073(3) 0.0073(3) 0.0136(4) 0.0009(5) 0.0009(5) 0.0005(3)
N1 0.0289(18) 0.0289(18) 0.016(4) 0.0003(19) 0.0003(19) -0.012(2)
O4 0.0221(16) 0.0221(16) 0.012(2) -0.0010(14) -0.0010(14) -0.005(2)
V1 0.0080(4) 0.0080(4) 0.0157(6) 0.000 0.000 0.000
O1 0.031(3) 0.031(3) 0.016(4) 0.000 0.000 0.000
O3 0.016(2) 0.016(2) 0.016(3) 0.000 0.000 -0.005(3)
O2 0.0174(17) 0.0103(16) 0.0300(17) 0.0016(14) 0.0021(15) 0.0053(14)

_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
V2 O4 1.639(5) . ?
V2 O3 1.794(3) . ?
V2 O2 1.708(3) 8_545 ?
V2 O2 1.708(3) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9121 . ?
N1 H1C 0.8971 . ?
N1 H1D 0.9205 . ?
V1 O1 1.591(8) . ?
V1 O2 1.961(3) 2_535 ?
V1 O2 1.961(3) 3_445 ?
V1 O2 1.961(3) . ?
V1 O2 1.961(3) 4_645 ?
O3 V2 1.794(3) 2_545 ?

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 V2 O3 109.4(3) . . ?
O4 V2 O2 111.09(18) . 8_545 ?
O4 V2 O2 111.09(18) . . ?
O2 V2 O3 108.01(18) 8_545 . ?
O2 V2 O3 108.01(19) . . ?
O2 V2 O2 109.2(2) 8_545 . ?
H1A N1 H1B 109.2 . . ?
H1A N1 H1C 109.6 . . ?
H1A N1 H1D 109.5 . . ?
H1B N1 H1C 108.7 . . ?
H1B N1 H1D 109.8 . . ?
H1C N1 H1D 110.1 . . ?
O1 V1 O2 107.01(13) . . ?
O1 V1 O2 107.01(13) . 2_535 ?
O1 V1 O2 107.01(13) . 4_645 ?
O1 V1 O2 107.01(13) . 3_445 ?
O2 V1 O2 85.09(7) 3_445 2_535 ?
O2 V1 O2 146.0(3) . 2_535 ?
O2 V1 O2 85.09(7) 4_645 2_535 ?
O2 V1 O2 85.09(8) . 4_645 ?
O2 V1 O2 85.09(8) . 3_445 ?
O2 V1 O2 146.0(3) 4_645 3_445 ?
V2 O3 V2 138.6(4) 2_545 . ?
V2 O2 V1 141.6(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
O4 V2 O3 V2 0.000(1) . . . 2_545 ?
O4 V2 O2 V1 11.9(4) . . . . ?
O3 V2 O2 V1 -108.0(4) . . . . ?
O2 V2 O3 V2 -121.02(16) 8_545 . . 2_545 ?
O2 V2 O3 V2 121.02(16) . . . 2_545 ?
O2 V2 O2 V1 134.8(2) 8_545 . . . ?

_shelx_res_file                  
;
    240k-1.res created by SHELXL-2014/7

TITL 240K-1 in P4bm
CELL 0.71073 8.8884 8.8884 5.5625 90 90 90
ZERR 2 0.0003 0.0003 0.0005 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,+Z
SYMM 0.5-Y,0.5-X,+Z
SYMM 0.5+Y,0.5+X,+Z
SFAC H N O V
UNIT 16 4 16 6

L.S. 20
PLAN  1
TEMP -33.15
CONF
MORE -1
BOND $H
fmap 2
acta
TWIN 1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\240K-1.hkl">
REM </olex2.extras>

WGHT    0.000000    0.973600
BASF   0.82673
FVAR       0.26288
V2    4   -0.133511   -0.633510   -0.405561    10.50000    0.00732    0.00732 =
         0.01356    0.00088    0.00088    0.00053
N1    2   -0.330568   -0.830568   -0.935359    10.50000    0.02887    0.02887 =
         0.01591    0.00029    0.00029   -0.01185
AFIX   3
H1A   1   -0.328238   -0.828240   -1.097069    10.50000   -1.20000
H1B   1   -0.306628   -0.925020   -0.883938    10.50000   -1.20000
H1C   1   -0.423548   -0.808100   -0.883938    10.50000   -1.20000
AFIX   3
H1D   1   -0.262358   -0.762360   -0.875158    10.50000   -1.20000
AFIX   0

O4    3   -0.130497   -0.630497   -0.700090    10.50000    0.02212    0.02212 =
         0.01248   -0.00097   -0.00097   -0.00534
V1    4    0.000000   -1.000000   -0.401459    10.25000    0.00796    0.00796 =
         0.01570    0.00000    0.00000    0.00000
O1    3    0.000000   -1.000000   -0.687519    10.25000    0.03129    0.03129 =
         0.01630    0.00000    0.00000    0.00000
O3    3    0.000000   -0.500000   -0.291609    10.25000    0.01593    0.01593 =
         0.01566    0.00000    0.00000   -0.00454
O2    3   -0.085597   -0.807132   -0.298306    11.00000    0.01736    0.01035 =
         0.03000    0.00160    0.00205    0.00525
HKLF 4

REM  240K-1 in P4bm
REM R1 =  0.0279 for     525 Fo > 4sig(Fo)  and  0.0302 for all     555 data
REM     39 parameters refined using      1 restraints

END

WGHT      0.0000      0.9734

REM Highest difference peak  0.414,  deepest hole -0.491,  1-sigma level  0.088
Q1    1  -0.0443 -0.6364 -0.4042  11.00000  0.05    0.41
;
_shelx_res_checksum              62099
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.17(8)
2 0.83(8)

