# Electronic Supplementary Material (ESI) for Molecular Systems Design & Engineering.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_[C4H12N2][(VO)3(SeO3)(HSeO3)4]-H2O-compound-4
_database_code_depnum_ccdc_archive 'CCDC 1588069'
_audit_update_record             
;
2017-11-28 deposited with the CCDC.
2018-02-01 downloaded from the CCDC.
;

_cell_length_a                   10.0027(6)
_cell_length_b                   10.4765(6)
_cell_length_c                   12.2924(7)
_cell_angle_alpha                74.478(3)
_cell_angle_beta                 72.643(3)
_cell_angle_gamma                79.707(3)
_cell_volume                     1177.80(7)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Se -0.0929 2.2259 17.0006 2.4098 5.8196 0.2726 3.9731 15.2372 4.3543 43.8163
2.8409 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
V 0.3005 0.5294 10.2971 6.8657 7.3511 0.4385 2.0703 26.8938 2.0571 102.4780
1.2199 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C6 O22 Se6 V3 
# Dc =      2.96 Fooo =   1010.00 Mu =    105.36 M =   1050.64
# Found Formula = C4 H18 N2 O22 Se6 V3 
# Dc =      3.02 FOOO =   1010.00 Mu =    105.40 M =   1072.77

_chemical_formula_sum            'C4 H18 N2 O22 Se6 V3'
_chemical_formula_moiety         'C4 H18 N2 O22 Se6 V3'
_chemical_compound_source        ?
_chemical_formula_weight         1072.77


_cell_measurement_reflns_used    9915
_cell_measurement_theta_min      2.3761
_cell_measurement_theta_max      32.1290
_cell_measurement_temperature    100

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_min          0.080
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_max          0.190

_exptl_crystal_density_diffrn    3.025
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1010
_exptl_absorpt_coefficient_mu    10.540

# Sheldrick geometric approximatio 0.23 0.43 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.23
_exptl_absorpt_correction_T_max  0.43
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      100
_diffrn_reflns_number            46237
_reflns_number_total             7940
_diffrn_reflns_av_R_equivalents  0.021
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 7940 
# Theoretical number of reflections is about 16756 


_diffrn_reflns_theta_min         1.783
_diffrn_reflns_theta_max         32.288
_diffrn_measured_fraction_theta_max 0.948

_diffrn_reflns_theta_full        29.059
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_reflns_limit_h_min              -14
_reflns_limit_h_max              14
_reflns_limit_k_min              -14
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              18

_oxford_diffrn_Wilson_B_factor   0.32
_oxford_diffrn_Wilson_scale      87.69

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.92
_refine_diff_density_max         3.36


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         7940
_refine_ls_number_restraints     20
_refine_ls_number_parameters     365
_oxford_refine_ls_R_factor_ref   0.0222
_refine_ls_wR_factor_ref         0.0412
_refine_ls_goodness_of_fit_ref   0.9390
_refine_ls_shift/su_max          0.0012870
_refine_ls_shift/su_mean         0.0000574


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        7940
_refine_ls_R_factor_all          0.0222
_refine_ls_wR_factor_all         0.0412

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7071
_refine_ls_R_factor_gt           0.0180
_refine_ls_wR_factor_gt          0.0396

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.01P)² + 3.32P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
V1 V 0.26605(3) 0.99567(3) 0.24756(3) 0.0041 1.0000 Uani . . . . . .
V2 V 0.25311(3) 0.49428(3) 0.26014(3) 0.0041 1.0000 Uani . . . . . .
V3 V 0.79135(3) 0.72685(3) 0.21670(3) 0.0066 1.0000 Uani . . . . . .
Se1 Se 0.072291(17) 0.777662(16) 0.249501(14) 0.0041 1.0000 Uani . . . . . .
Se2 Se 0.135526(17) 0.216285(17) 0.397984(15) 0.0044 1.0000 Uani . . . . . .
Se3 Se 0.367427(17) 1.276711(17) 0.112546(15) 0.0043 1.0000 Uani . . . . . .
Se4 Se 0.458371(17) 0.713159(16) 0.248429(15) 0.0043 1.0000 Uani . . . . . .
Se5 Se 0.215000(18) 0.483786(17) 0.539930(15) 0.0056 1.0000 Uani . . . . . .
Se6 Se 0.288940(17) 1.016489(17) -0.032917(15) 0.0048 1.0000 Uani . . . . . .
O1 O 0.31730(14) 0.95058(13) 0.36640(12) 0.0091 1.0000 Uani . . . . . .
O2 O 0.08677(13) 0.90519(12) 0.30832(11) 0.0059 1.0000 Uani . . . . . .
O3 O 0.14468(13) 1.16596(12) 0.27513(11) 0.0057 1.0000 Uani . . . . . .
O4 O 0.42016(13) 1.11271(12) 0.14607(11) 0.0068 1.0000 Uani . . . . . .
O5 O 0.36494(13) 0.84175(12) 0.17496(11) 0.0064 1.0000 Uani . . . . . .
O6 O 0.18617(13) 1.05497(13) 0.09110(11) 0.0071 1.0000 Uani . . . . . .
O7 O 0.21112(14) 0.53984(13) 0.13795(12) 0.0088 1.0000 Uani . . . . . .
O8 O 0.37484(13) 0.32318(13) 0.23283(11) 0.0062 1.0000 Uani . . . . . .
O9 O 0.09434(13) 0.38120(12) 0.35700(12) 0.0070 1.0000 Uani . . . . . .
O10 O 0.15103(13) 0.64697(12) 0.33269(11) 0.0062 1.0000 Uani . . . . . .
O11 O 0.43602(13) 0.58245(13) 0.19837(11) 0.0065 1.0000 Uani . . . . . .
O12 O 0.32613(14) 0.43624(13) 0.42353(12) 0.0085 1.0000 Uani . . . . . .
O13 O 0.90586(14) 0.64263(15) 0.13374(13) 0.0123 1.0000 Uani . . . . . .
O14 O 0.62263(13) 0.73877(13) 0.15958(11) 0.0071 1.0000 Uani . . . . . .
O15 O 0.70208(14) 0.59220(14) 0.35365(12) 0.0104 1.0000 Uani . . . . . .
O16 O 0.89972(13) 0.75977(13) 0.31782(12) 0.0076 1.0000 Uani . . . . . .
O17 O 0.80830(14) 0.91306(13) 0.12940(11) 0.0083 1.0000 Uani . . . . . .
O18 O 0.53022(14) 1.33027(13) 0.02412(11) 0.0077 1.0000 Uani D . . . . .
O19 O 0.24138(14) 0.85570(13) -0.01827(12) 0.0082 1.0000 Uani D . . . . .
O20 O -0.03401(13) 0.17291(13) 0.47302(11) 0.0076 1.0000 Uani D . . . . .
O21 O 0.26909(15) 0.64203(13) 0.52844(12) 0.0099 1.0000 Uani D . . . . .
O22 O 0.60249(19) 0.8581(2) 0.37996(19) 0.0286 1.0000 Uani D . . . . .
N1 N 0.64660(18) 0.33096(17) 0.27633(16) 0.0126 1.0000 Uani D . . . . .
N2 N 0.89877(18) 0.17525(18) 0.17475(17) 0.0149 1.0000 Uani D . . . . .
C1 C 0.6555(2) 0.1817(2) 0.30148(18) 0.0136 1.0000 Uani D . . . . .
C2 C 0.8060(2) 0.1182(2) 0.29169(19) 0.0151 1.0000 Uani D . . . . .
C3 C 0.8937(2) 0.3236(2) 0.15289(19) 0.0152 1.0000 Uani D . . . . .
C4 C 0.7435(2) 0.3877(2) 0.16071(18) 0.0132 1.0000 Uani D . . . . .
H1 H 0.529(3) 1.361(2) -0.0443(15) 0.0093 1.0000 Uiso D . . . . .
H2 H 0.306(2) 0.798(2) -0.010(2) 0.0098 1.0000 Uiso D . . . . .
H3 H -0.041(3) 0.143(2) 0.5431(15) 0.0091 1.0000 Uiso D . . . . .
H4 H 0.204(2) 0.700(2) 0.516(2) 0.0119 1.0000 Uiso D . . . . .
H5 H 0.599(4) 0.784(2) 0.433(2) 0.0339 1.0000 Uiso D . . . . .
H6 H 0.517(2) 0.893(3) 0.391(3) 0.0339 1.0000 Uiso D . . . . .
H7 H 0.668(2) 0.3537(19) 0.3336(15) 0.0149 1.0000 Uiso D . . . . .
H8 H 0.5594(18) 0.3662(18) 0.2762(17) 0.0149 1.0000 Uiso D . . . . .
H9 H 0.6008 0.1512 0.3799 0.0168 1.0000 Uiso . . . . . .
H10 H 0.6176 0.1571 0.2475 0.0173 1.0000 Uiso . . . . . .
H11 H 0.8404 0.1345 0.3523 0.0181 1.0000 Uiso . . . . . .
H12 H 0.8083 0.0227 0.3015 0.0186 1.0000 Uiso . . . . . .
H13 H 0.9858(18) 0.1369(18) 0.1710(17) 0.0179 1.0000 Uiso D . . . . .
H14 H 0.868(2) 0.1547(19) 0.1211(16) 0.0179 1.0000 Uiso D . . . . .
H15 H 0.9287 0.3444 0.2117 0.0188 1.0000 Uiso . . . . . .
H16 H 0.9520 0.3565 0.0735 0.0192 1.0000 Uiso . . . . . .
H17 H 0.7389 0.4835 0.1518 0.0158 1.0000 Uiso . . . . . .
H18 H 0.7099 0.3696 0.0997 0.0158 1.0000 Uiso . . . . . .

_refine_ls_extinction_coef       2.8(5)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.087586(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 . Se2 1_565 3.1991(4) yes
V1 . Se1 . 3.2401(4) yes
V1 . Se3 . 3.1463(4) yes
V1 . Se4 . 3.2282(4) yes
V1 . O1 . 1.6159(14) yes
V1 . O2 . 2.0252(13) yes
V1 . O3 . 2.0188(13) yes
V1 . O4 . 2.0361(13) yes
V1 . O5 . 2.0121(13) yes
V1 . O6 . 2.1961(13) yes
V2 . Se3 1_545 3.1367(4) yes
V2 . Se1 . 3.1807(4) yes
V2 . Se2 . 3.1828(4) yes
V2 . Se4 . 3.2900(4) yes
V2 . O7 . 1.6066(14) yes
V2 . O8 . 2.0265(13) yes
V2 . O9 . 2.0328(13) yes
V2 . O10 . 2.0083(13) yes
V2 . O11 . 2.0438(13) yes
V2 . O12 . 2.2361(14) yes
V3 . Se1 1_655 3.1094(4) yes
V3 . Se6 2_675 3.1683(4) yes
V3 . Se5 2_666 3.1979(4) yes
V3 . O13 . 1.5982(14) yes
V3 . O14 . 1.9853(13) yes
V3 . O15 . 1.9758(14) yes
V3 . O16 . 2.0015(13) yes
V3 . O17 . 1.9686(13) yes
Se1 . O16 1_455 1.6990(13) yes
Se1 . O2 . 1.7256(13) yes
Se1 . O10 . 1.6990(12) yes
Se2 . O3 1_545 1.7010(13) yes
Se2 . O9 . 1.6770(13) yes
Se2 . O20 . 1.7467(13) yes
Se3 . O8 1_565 1.7008(13) yes
Se3 . O4 . 1.6814(13) yes
Se3 . O18 . 1.7584(13) yes
Se4 . O5 . 1.7048(12) yes
Se4 . O11 . 1.7165(13) yes
Se4 . O14 . 1.7013(13) yes
Se5 . O15 2_666 1.6991(13) yes
Se5 . O12 . 1.6630(13) yes
Se5 . O21 . 1.7919(14) yes
Se6 . O17 2_675 1.6914(13) yes
Se6 . O6 . 1.6701(13) yes
Se6 . O19 . 1.7803(13) yes
O18 . H1 . 0.819(16) no
O19 . H2 . 0.814(16) no
O20 . H3 . 0.821(16) no
O21 . H4 . 0.825(16) no
O22 . H5 . 0.872(17) no
O22 . H6 . 0.855(17) no
N1 . C1 . 1.503(3) yes
N1 . C4 . 1.498(3) yes
N1 . H7 . 0.892(16) no
N1 . H8 . 0.885(16) no
N2 . C2 . 1.492(3) yes
N2 . C3 . 1.498(3) yes
N2 . H13 . 0.884(16) no
N2 . H14 . 0.892(16) no
C1 . C2 . 1.517(3) yes
C1 . H9 . 0.956 no
C1 . H10 . 0.963 no
C2 . H11 . 0.972 no
C2 . H12 . 0.972 no
C3 . C4 . 1.519(3) yes
C3 . H15 . 0.977 no
C3 . H16 . 0.982 no
C4 . H17 . 0.974 no
C4 . H18 . 0.980 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Se2 1_565 V1 . Se1 . 119.892(10) yes
Se2 1_565 V1 . Se3 . 67.938(9) yes
Se1 . V1 . Se3 . 143.203(11) yes
Se2 1_565 V1 . Se4 . 143.005(11) yes
Se1 . V1 . Se4 . 71.877(9) yes
Se3 . V1 . Se4 . 125.733(11) yes
Se2 1_565 V1 . O1 . 71.44(5) yes
Se1 . V1 . O1 . 108.51(5) yes
Se3 . V1 . O1 . 107.90(5) yes
Se4 . V1 . O1 . 71.58(5) yes
Se2 1_565 V1 . O2 . 92.43(4) yes
Se1 . V1 . O2 . 27.68(4) yes
Se3 . V1 . O2 . 139.44(4) yes
Se4 . V1 . O2 . 91.62(4) yes
O1 . V1 . O2 . 97.87(6) yes
Se2 1_565 V1 . O3 . 27.89(4) yes
Se1 . V1 . O3 . 109.99(4) yes
Se3 . V1 . O3 . 58.46(4) yes
Se4 . V1 . O3 . 170.59(4) yes
O1 . V1 . O3 . 99.29(6) yes
Se2 1_565 V1 . O4 . 89.68(4) yes
Se1 . V1 . O4 . 144.48(4) yes
Se3 . V1 . O4 . 28.89(4) yes
Se4 . V1 . O4 . 96.90(4) yes
O1 . V1 . O4 . 98.94(6) yes
Se2 1_565 V1 . O5 . 170.07(4) yes
Se1 . V1 . O5 . 63.03(4) yes
Se3 . V1 . O5 . 116.07(4) yes
Se4 . V1 . O5 . 27.11(4) yes
O1 . V1 . O5 . 98.65(6) yes
Se2 1_565 V1 . O6 . 107.61(4) yes
Se1 . V1 . O6 . 69.60(4) yes
Se3 . V1 . O6 . 73.82(4) yes
Se4 . V1 . O6 . 109.29(4) yes
O1 . V1 . O6 . 177.26(6) yes
O2 . V1 . O3 . 87.31(5) yes
O2 . V1 . O4 . 162.85(5) yes
O3 . V1 . O4 . 86.62(5) yes
O2 . V1 . O5 . 89.45(5) yes
O3 . V1 . O5 . 162.04(5) yes
O4 . V1 . O5 . 91.39(5) yes
O2 . V1 . O6 . 79.55(5) yes
O3 . V1 . O6 . 79.72(5) yes
O4 . V1 . O6 . 83.58(5) yes
O5 . V1 . O6 . 82.32(5) yes
Se3 1_545 V2 . Se1 . 140.353(11) yes
Se3 1_545 V2 . Se2 . 68.257(9) yes
Se1 . V2 . Se2 . 125.257(11) yes
Se3 1_545 V2 . Se4 . 120.075(10) yes
Se1 . V2 . Se4 . 71.824(9) yes
Se2 . V2 . Se4 . 145.669(11) yes
Se3 1_545 V2 . O7 . 68.77(5) yes
Se1 . V2 . O7 . 71.60(5) yes
Se2 . V2 . O7 . 108.48(5) yes
Se4 . V2 . O7 . 105.25(5) yes
Se3 1_545 V2 . O8 . 29.61(4) yes
Se1 . V2 . O8 . 168.91(4) yes
Se2 . V2 . O8 . 60.82(4) yes
Se4 . V2 . O8 . 108.50(4) yes
O7 . V2 . O8 . 97.95(6) yes
Se3 1_545 V2 . O9 . 87.81(4) yes
Se1 . V2 . O9 . 97.58(4) yes
Se2 . V2 . O9 . 27.77(4) yes
Se4 . V2 . O9 . 147.81(4) yes
O7 . V2 . O9 . 99.56(6) yes
Se3 1_545 V2 . O10 . 167.61(4) yes
Se1 . V2 . O10 . 28.16(4) yes
Se2 . V2 . O10 . 113.51(4) yes
Se4 . V2 . O10 . 66.00(4) yes
O7 . V2 . O10 . 99.59(6) yes
Se3 1_545 V2 . O11 . 93.82(4) yes
Se1 . V2 . O11 . 90.82(4) yes
Se2 . V2 . O11 . 141.25(4) yes
Se4 . V2 . O11 . 26.31(4) yes
O7 . V2 . O11 . 95.12(6) yes
Se3 1_545 V2 . O12 . 110.75(4) yes
Se1 . V2 . O12 . 108.87(4) yes
Se2 . V2 . O12 . 74.63(4) yes
Se4 . V2 . O12 . 71.40(4) yes
O7 . V2 . O12 . 175.99(6) yes
O8 . V2 . O9 . 87.67(5) yes
O8 . V2 . O10 . 162.44(5) yes
O9 . V2 . O10 . 90.11(5) yes
O8 . V2 . O11 . 86.34(5) yes
O9 . V2 . O11 . 164.77(5) yes
O10 . V2 . O11 . 91.40(5) yes
O8 . V2 . O12 . 81.28(5) yes
O9 . V2 . O12 . 84.36(5) yes
O10 . V2 . O12 . 81.17(5) yes
O11 . V2 . O12 . 80.91(5) yes
Se1 1_655 V3 . Se6 2_675 104.609(11) yes
Se1 1_655 V3 . Se5 2_666 81.747(10) yes
Se6 2_675 V3 . Se5 2_666 160.351(12) yes
Se1 1_655 V3 . O13 . 77.85(5) yes
Se6 2_675 V3 . O13 . 101.85(5) yes
Se5 2_666 V3 . O13 . 97.65(5) yes
Se1 1_655 V3 . O14 . 164.04(4) yes
Se6 2_675 V3 . O14 . 59.70(4) yes
Se5 2_666 V3 . O14 . 114.01(4) yes
O13 . V3 . O14 . 101.46(7) yes
Se1 1_655 V3 . O15 . 108.83(4) yes
Se6 2_675 V3 . O15 . 140.69(4) yes
Se5 2_666 V3 . O15 . 27.16(4) yes
O13 . V3 . O15 . 104.83(7) yes
O14 . V3 . O15 . 86.86(5) yes
Se1 1_655 V3 . O16 . 29.92(4) yes
Se6 2_675 V3 . O16 . 114.43(4) yes
Se5 2_666 V3 . O16 . 62.62(4) yes
O13 . V3 . O16 . 103.07(6) yes
O14 . V3 . O16 . 155.47(5) yes
Se1 1_655 V3 . O17 . 78.15(4) yes
Se6 2_675 V3 . O17 . 27.62(4) yes
Se5 2_666 V3 . O17 . 146.47(4) yes
O13 . V3 . O17 . 103.93(7) yes
O14 . V3 . O17 . 86.64(5) yes
O15 . V3 . O16 . 86.97(6) yes
O15 . V3 . O17 . 151.22(6) yes
O16 . V3 . O17 . 87.43(5) yes
V3 1_455 Se1 . O16 1_455 35.99(5) yes
V3 1_455 Se1 . V2 . 103.221(10) yes
O16 1_455 Se1 . V2 . 110.46(5) yes
V3 1_455 Se1 . V1 . 146.899(10) yes
O16 1_455 Se1 . V1 . 130.16(5) yes
V2 . Se1 . V1 . 109.304(10) yes
V3 1_455 Se1 . O2 . 123.55(4) yes
O16 1_455 Se1 . O2 . 97.49(6) yes
V2 . Se1 . O2 . 128.11(4) yes
V1 . Se1 . O2 . 33.03(4) yes
V3 1_455 Se1 . O10 . 115.02(4) yes
O16 1_455 Se1 . O10 . 100.71(6) yes
V2 . Se1 . O10 . 33.91(4) yes
V1 . Se1 . O10 . 95.82(4) yes
O2 . Se1 . O10 . 99.99(6) yes
O3 1_545 Se2 . V2 . 94.73(4) yes
O3 1_545 Se2 . V1 1_545 33.72(4) yes
V2 . Se2 . V1 1_545 110.530(10) yes
O3 1_545 Se2 . O9 . 101.65(6) yes
V2 . Se2 . O9 . 34.38(4) yes
V1 1_545 Se2 . O9 . 131.27(5) yes
O3 1_545 Se2 . O20 . 96.06(6) yes
V2 . Se2 . O20 . 132.46(5) yes
V1 1_545 Se2 . O20 . 103.73(5) yes
O9 . Se2 . O20 . 98.08(6) yes
O8 1_565 Se3 . V2 1_565 36.06(4) yes
O8 1_565 Se3 . V1 . 95.81(4) yes
V2 1_565 Se3 . V1 . 113.177(10) yes
O8 1_565 Se3 . O4 . 101.07(6) yes
V2 1_565 Se3 . O4 . 133.70(5) yes
V1 . Se3 . O4 . 35.80(4) yes
O8 1_565 Se3 . O18 . 95.56(6) yes
V2 1_565 Se3 . O18 . 101.98(4) yes
V1 . Se3 . O18 . 133.74(4) yes
O4 . Se3 . O18 . 97.96(6) yes
V1 . Se4 . V2 . 106.924(10) yes
V1 . Se4 . O5 . 32.54(4) yes
V2 . Se4 . O5 . 92.99(4) yes
V1 . Se4 . O11 . 127.76(4) yes
V2 . Se4 . O11 . 31.86(4) yes
O5 . Se4 . O11 . 101.12(6) yes
V1 . Se4 . O14 . 109.38(5) yes
V2 . Se4 . O14 . 128.67(5) yes
O5 . Se4 . O14 . 98.60(6) yes
O11 . Se4 . O14 . 96.85(6) yes
O15 2_666 Se5 . V3 2_666 32.06(5) yes
O15 2_666 Se5 . O12 . 101.74(7) yes
V3 2_666 Se5 . O12 . 114.66(5) yes
O15 2_666 Se5 . O21 . 91.89(6) yes
V3 2_666 Se5 . O21 . 115.33(5) yes
O12 . Se5 . O21 . 102.30(7) yes
O17 2_675 Se6 . V3 2_675 32.65(4) yes
O17 2_675 Se6 . O6 . 102.72(6) yes
V3 2_675 Se6 . O6 . 99.85(5) yes
O17 2_675 Se6 . O19 . 91.48(6) yes
V3 2_675 Se6 . O19 . 123.53(4) yes
O6 . Se6 . O19 . 101.25(6) yes
V1 . O2 . Se1 . 119.29(7) yes
V1 . O3 . Se2 1_565 118.39(7) yes
V1 . O4 . Se3 . 115.31(7) yes
V1 . O5 . Se4 . 120.35(7) yes
V1 . O6 . Se6 . 118.67(7) yes
V2 . O8 . Se3 1_545 114.33(7) yes
V2 . O9 . Se2 . 117.85(7) yes
V2 . O10 . Se1 . 117.94(7) yes
V2 . O11 . Se4 . 121.83(7) yes
V2 . O12 . Se5 . 115.92(7) yes
V3 . O14 . Se4 . 124.19(7) yes
V3 . O15 . Se5 2_666 120.78(7) yes
V3 . O16 . Se1 1_655 114.09(7) yes
V3 . O17 . Se6 2_675 119.73(7) yes
Se3 . O18 . H1 . 112.4(18) no
Se6 . O19 . H2 . 111.4(18) no
Se2 . O20 . H3 . 110.9(18) no
Se5 . O21 . H4 . 108.3(19) no
H5 . O22 . H6 . 104(3) no
C1 . N1 . C4 . 112.15(15) yes
C1 . N1 . H7 . 108.6(12) no
C4 . N1 . H7 . 109.8(12) no
C1 . N1 . H8 . 110.0(12) no
C4 . N1 . H8 . 108.7(12) no
H7 . N1 . H8 . 107.4(14) no
C2 . N2 . C3 . 111.69(16) yes
C2 . N2 . H13 . 108.6(13) no
C3 . N2 . H13 . 110.8(12) no
C2 . N2 . H14 . 107.2(12) no
C3 . N2 . H14 . 109.6(12) no
H13 . N2 . H14 . 108.9(15) no
N1 . C1 . C2 . 111.53(17) yes
N1 . C1 . H9 . 107.9 no
C2 . C1 . H9 . 108.4 no
N1 . C1 . H10 . 108.9 no
C2 . C1 . H10 . 110.1 no
H9 . C1 . H10 . 109.9 no
C1 . C2 . N2 . 110.17(16) yes
C1 . C2 . H11 . 110.0 no
N2 . C2 . H11 . 109.0 no
C1 . C2 . H12 . 108.9 no
N2 . C2 . H12 . 109.6 no
H11 . C2 . H12 . 109.1 no
N2 . C3 . C4 . 110.10(16) yes
N2 . C3 . H15 . 108.7 no
C4 . C3 . H15 . 109.9 no
N2 . C3 . H16 . 108.4 no
C4 . C3 . H16 . 108.5 no
H15 . C3 . H16 . 111.2 no
C3 . C4 . N1 . 110.91(16) yes
C3 . C4 . H17 . 110.3 no
N1 . C4 . H17 . 108.6 no
C3 . C4 . H18 . 109.7 no
N1 . C4 . H18 . 107.3 no
H17 . C4 . H18 . 109.9 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O18 . H1 . O11 2_675 169(3) 0.819 1.771 2.579(3) yes
O19 . H2 . O18 2_675 168(3) 0.814 1.920 2.722(3) yes
O20 . H3 . O2 2_566 169(3) 0.821 1.700 2.511(3) yes
O21 . H4 . O20 2_566 167(3) 0.825 1.960 2.769(3) yes
O22 . H6 . O1 . 159(3) 0.855 2.069 2.883(3) yes
N1 . H7 . O21 2_666 166.2(18) 0.892 1.990 2.865(3) yes
N1 . H8 . O8 . 139.0(17) 0.885 2.215 2.941(3) yes
N1 . H8 . O11 . 138.3(15) 0.885 2.473 3.189(3) yes
C2 . H11 . O20 1_655 169.07(13) 0.972 2.356 3.316(3) yes
N2 . H13 . O3 1_645 127.6(17) 0.884 2.419 3.040(3) yes
N2 . H13 . O6 1_645 156.0(18) 0.884 2.093 2.923(3) yes
N2 . H14 . O19 2_665 164.4(19) 0.892 1.937 2.806(3) yes
C3 . H16 . O13 2_765 159.30(13) 0.982 2.518 3.454(3) yes
C4 . H17 . O13 . 136.09(12) 0.974 2.489 3.261(3) yes
C4 . H18 . O18 1_545 152.97(12) 0.980 2.394 3.297(3) yes


####################################################################### 
# 
# 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_[C4H12N2][(VO)2O2(SeO3)2]-compound-5
_database_code_depnum_ccdc_archive 'CCDC 1588072'
_audit_update_record             
;
2017-11-28 deposited with the CCDC.
2018-02-01 downloaded from the CCDC.
;

_cell_length_a                   10.0879(4)
_cell_length_b                   6.2047(2)
_cell_length_c                   10.6765(4)
_cell_angle_alpha                90
_cell_angle_beta                 116.5657(17)
_cell_angle_gamma                90
_cell_volume                     597.71(2)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
V 0.3005 0.5294 10.2971 6.8657 7.3511 0.4385 2.0703 26.8938 2.0571 102.4780
1.2199 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Se -0.0929 2.2259 17.0006 2.4098 5.8196 0.2726 3.9731 15.2372 4.3543 43.8163
2.8409 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C4 H14 N2 O10 Se4 V2 
# Dc =      3.71 Fooo =    488.00 Mu =    138.06 M =    333.94
# Found Formula = C4 H12 N2 O10 Se2 V2 
# Dc =      2.82 FOOO =    488.00 Mu =     77.09 M =    253.97

_chemical_formula_sum            'C4 H12 N2 O10 Se2 V2'
_chemical_formula_moiety         'C4 H12 N2 O10 Se2 V2'
_chemical_compound_source        ?
_chemical_formula_weight         507.95


_cell_measurement_reflns_used    9888
_cell_measurement_theta_min      3.8330
_cell_measurement_theta_max      32.1076
_cell_measurement_temperature    100

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.075
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_max          0.205

_exptl_crystal_density_diffrn    2.822
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             488
_exptl_absorpt_coefficient_mu    7.709

# Sheldrick geometric approximatio 0.45 0.56 
# No experimental values of Tmin/max available 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_T_max  0.56
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      100
_diffrn_reflns_number            22548
_reflns_number_total             2066
_diffrn_reflns_av_R_equivalents  0.032
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 2066 
# Theoretical number of reflections is about 4287 


_diffrn_reflns_theta_min         2.257
_diffrn_reflns_theta_max         32.387
_diffrn_measured_fraction_theta_max 0.964

_diffrn_reflns_theta_full        30.444
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_reflns_limit_h_min              -15
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              9
_reflns_limit_l_min              0
_reflns_limit_l_max              16

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.69
_refine_diff_density_max         1.10


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         2066
_refine_ls_number_restraints     7
_refine_ls_number_parameters     98
_oxford_refine_ls_R_factor_ref   0.0210
_refine_ls_wR_factor_ref         0.0530
_refine_ls_goodness_of_fit_ref   1.0045
_refine_ls_shift/su_max          0.0004452
_refine_ls_shift/su_mean         0.0000294


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        2066
_refine_ls_R_factor_all          0.0210
_refine_ls_wR_factor_all         0.0530

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1926
_refine_ls_R_factor_gt           0.0190
_refine_ls_wR_factor_gt          0.0521

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.03P)² + 1.21P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
V1 V 0.15042(3) 0.52670(5) 0.01159(3) 0.0045 1.0000 Uani . . . . . .
Se1 Se 0.052782(17) 0.60078(3) -0.326805(17) 0.0044 1.0000 Uani . . . . . .
O1 O 0.32836(14) 0.4863(2) 0.08335(14) 0.0079 1.0000 Uani . . . . . .
O2 O 0.09203(14) 0.4115(2) 0.11939(14) 0.0066 1.0000 Uani . . . . . .
O3 O 0.09522(13) 0.2771(2) -0.11724(13) 0.0063 1.0000 Uani . . . . . .
O4 O 0.14419(14) 0.8221(2) 0.07789(13) 0.0071 1.0000 Uani . . . . . .
O5 O 0.16200(14) 0.6937(2) -0.16403(13) 0.0072 1.0000 Uani . . . . . .
N1 N 0.34733(16) 0.4607(3) 0.46314(16) 0.0073 1.0000 Uani D . . . . .
C1 C 0.45423(19) 0.5146(3) 0.61005(18) 0.0082 1.0000 Uani D . . . . .
C2 C 0.42236(19) 0.3465(3) 0.38935(19) 0.0079 1.0000 Uani D . . . . .
H1 H 0.300(2) 0.577(3) 0.4147(19) 0.0092 1.0000 Uiso D . . . . .
H2 H 0.275(2) 0.383(3) 0.462(2) 0.0092 1.0000 Uiso D . . . . .
H3 H 0.4028 0.5888 0.6530 0.0099 1.0000 Uiso R . . . . .
H4 H 0.4941 0.3825 0.6582 0.0101 1.0000 Uiso R . . . . .
H5 H 0.4620 0.2124 0.4364 0.0090 1.0000 Uiso R . . . . .
H6 H 0.3510 0.3179 0.2968 0.0088 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       2.4(6)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.17884(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 . O2 2_565 2.2418(13) yes
V1 . V1 2_565 2.9513(6) yes
V1 . Se1 4_565 3.2878(3) yes
V1 . O1 . 1.6254(13) yes
V1 . O2 . 1.6700(13) yes
V1 . O3 . 1.9789(13) yes
V1 . O4 . 1.9760(13) yes
V1 . O5 . 2.1906(13) yes
Se1 . O3 3_554 1.7276(12) yes
Se1 . O4 4_564 1.7186(12) yes
Se1 . O5 . 1.6894(13) yes
N1 . C1 . 1.491(2) yes
N1 . C2 . 1.493(2) yes
N1 . H1 . 0.891(16) no
N1 . H2 . 0.873(16) no
C1 . C2 2_666 1.512(2) yes
C1 . H3 . 0.951 no
C1 . H4 . 0.955 no
C2 . H5 . 0.962 no
C2 . H6 . 0.943 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 2_565 V1 . V1 2_565 34.18(3) yes
O2 2_565 V1 . Se1 4_565 73.00(3) yes
V1 2_565 V1 . Se1 4_565 65.463(10) yes
O2 2_565 V1 . O1 . 170.84(6) yes
V1 2_565 V1 . O1 . 154.11(5) yes
Se1 4_565 V1 . O1 . 112.83(5) yes
O2 2_565 V1 . O2 . 83.13(6) yes
V1 2_565 V1 . O2 . 48.95(4) yes
Se1 4_565 V1 . O2 . 70.03(4) yes
O1 . V1 . O2 . 105.34(7) yes
O2 2_565 V1 . O3 . 79.11(5) yes
V1 2_565 V1 . O3 . 83.96(4) yes
Se1 4_565 V1 . O3 . 149.07(4) yes
O1 . V1 . O3 . 96.60(6) yes
O2 . V1 . O3 . 93.88(6) yes
O2 2_565 V1 . O4 . 82.19(5) yes
V1 2_565 V1 . O4 . 86.44(4) yes
Se1 4_565 V1 . O4 . 25.16(4) yes
O1 . V1 . O4 . 100.35(6) yes
O2 . V1 . O4 . 94.17(6) yes
O2 2_565 V1 . O5 . 81.15(5) yes
V1 2_565 V1 . O5 . 115.33(4) yes
Se1 4_565 V1 . O5 . 105.06(4) yes
O1 . V1 . O5 . 90.35(6) yes
O2 . V1 . O5 . 164.28(6) yes
O3 . V1 . O4 . 158.58(5) yes
O3 . V1 . O5 . 83.19(5) yes
O4 . V1 . O5 . 83.70(5) yes
O3 3_554 Se1 . O4 4_564 103.21(6) yes
O3 3_554 Se1 . V1 4_564 77.81(4) yes
O4 4_564 Se1 . V1 4_564 29.26(4) yes
O3 3_554 Se1 . O5 . 101.82(6) yes
O4 4_564 Se1 . O5 . 103.78(6) yes
V1 4_564 Se1 . O5 . 95.12(4) yes
V1 2_565 O2 . V1 . 96.87(6) yes
V1 . O3 . Se1 3_544 131.83(7) yes
V1 . O4 . Se1 4_565 125.58(7) yes
V1 . O5 . Se1 . 117.33(7) yes
C1 . N1 . C2 . 111.27(13) yes
C1 . N1 . H1 . 112.2(12) no
C2 . N1 . H1 . 110.3(12) no
C1 . N1 . H2 . 110.1(13) no
C2 . N1 . H2 . 110.6(12) no
H1 . N1 . H2 . 101.9(15) no
C2 2_666 C1 . N1 . 109.82(14) yes
C2 2_666 C1 . H3 . 110.3 no
N1 . C1 . H3 . 108.8 no
C2 2_666 C1 . H4 . 109.8 no
N1 . C1 . H4 . 107.9 no
H3 . C1 . H4 . 110.2 no
C1 2_666 C2 . N1 . 109.76(14) yes
C1 2_666 C2 . H5 . 110.0 no
N1 . C2 . H5 . 109.0 no
C1 2_666 C2 . H6 . 110.7 no
N1 . C2 . H6 . 108.2 no
H5 . C2 . H6 . 109.2 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
N1 . H1 . O5 4_565 163.6(19) 0.891 1.902 2.769(3) yes
N1 . H2 . O1 4_555 120.1(16) 0.873 2.566 3.097(3) yes
N1 . H2 . O3 4_555 157.0(18) 0.873 1.901 2.726(3) yes
C1 . H3 . O4 4_565 133.58(5) 0.951 2.426 3.157(3) yes
C2 . H6 . O1 . 127.64(5) 0.943 2.423 3.091(3) yes
C2 . H6 . O2 . 142.62(5) 0.943 2.515 3.314(3) yes


####################################################################### 
# 
# 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_[C8H26N4][VO(SeO3)(HSeO3]6-6H2O-compound-2
_database_code_depnum_ccdc_archive 'CCDC 1588073'
_audit_update_record             
;
2017-11-28 deposited with the CCDC.
2018-02-01 downloaded from the CCDC.
;

_cell_length_a                   18.816(5)
_cell_length_b                   7.934(5)
_cell_length_c                   34.439(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.850(5)
_cell_angle_gamma                90
_cell_volume                     5114(4)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
V 0.3005 0.5294 10.2971 6.8657 7.3511 0.4385 2.0703 26.8938 2.0571 102.4780
1.2199 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Se -0.0929 2.2259 17.0006 2.4098 5.8196 0.2726 3.9731 15.2372 4.3543 43.8163
2.8409 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C14 H49 N7 O35 Se14 V7 
# Dc =      3.04 Fooo =   4200.00 Mu =    112.94 M =   1168.80
# Found Formula = C8 H44 N4 O48 Se12 V6 
# Dc =      2.88 FOOO =   4200.00 Mu =     97.20 M =   1108.80

_chemical_formula_sum            'C8 H44 N4 O48 Se12 V6'
_chemical_formula_moiety         'C8 H44 N4 O48 Se12 V6'
_chemical_compound_source        ?
_chemical_formula_weight         2217.60


_cell_measurement_reflns_used    9081
_cell_measurement_theta_min      3
_cell_measurement_theta_max      31
_cell_measurement_temperature    100

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.040
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_max          0.140

_exptl_crystal_density_diffrn    2.880
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             4200
_exptl_absorpt_coefficient_mu    9.720

# Sheldrick geometric approximatio 0.46 0.68 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_T_max  0.68
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      100
_diffrn_reflns_number            57284
_reflns_number_total             7751
_diffrn_reflns_av_R_equivalents  0.041
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 7751 
# Theoretical number of reflections is about 15654 


_diffrn_reflns_theta_min         1.189
_diffrn_reflns_theta_max         30.538
_diffrn_measured_fraction_theta_max 0.988

_diffrn_reflns_theta_full        29.316
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_reflns_limit_h_min              -26
_reflns_limit_h_max              26
_reflns_limit_k_min              0
_reflns_limit_k_max              11
_reflns_limit_l_min              0
_reflns_limit_l_max              48

_oxford_diffrn_Wilson_B_factor   0.44
_oxford_diffrn_Wilson_scale      177.60

_atom_sites_solution_primary     Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -3.18
_refine_diff_density_max         3.35


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         6665
_refine_ls_number_restraints     0
_refine_ls_number_parameters     361
_oxford_refine_ls_R_factor_ref   0.0478
_refine_ls_wR_factor_ref         0.1145
_refine_ls_goodness_of_fit_ref   1.1599
_refine_ls_shift/su_max          0.0008909
_refine_ls_shift/su_mean         0.0000359


# The values computed from all data 
_oxford_reflns_number_all        7732
_refine_ls_R_factor_all          0.0561
_refine_ls_wR_factor_all         0.1185

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6991
_refine_ls_R_factor_gt           0.0508
_refine_ls_wR_factor_gt          0.1167

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.01P)² +*****P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
V1 V 0.62640(5) 0.23991(14) 0.26149(3) 0.0060 1.0000 Uani . . . . . .
V2 V 0.54829(6) 0.30133(14) 0.40228(3) 0.0059 1.0000 Uani . . . . . .
V3 V 0.79328(6) 0.31751(15) 0.43112(3) 0.0078 1.0000 Uani . . . . . .
Se1 Se 0.49143(3) 0.25443(8) 0.312252(17) 0.0063 1.0000 Uani . . . . . .
Se2 Se 0.68334(3) 0.30554(8) 0.353190(18) 0.0067 1.0000 Uani . . . . . .
Se3 Se 0.65466(3) 0.27284(8) 0.479626(17) 0.0049 1.0000 Uani . . . . . .
Se4 Se 0.71920(3) 0.57436(9) 0.234972(19) 0.0101 1.0000 Uani . . . . . .
Se5 Se 0.95166(3) 0.47898(9) 0.428273(19) 0.0090 1.0000 Uani . . . . . .
Se6 Se 0.40468(7) 0.52385(16) 0.39912(5) 0.0052 0.8162 Uani . . . . . .
Se7 Se 0.3928(6) 0.4747(10) 0.4013(3) 0.0373 0.1838 Uani . . . . . .
O1 O 0.5839(3) 0.0628(7) 0.25842(14) 0.0114 1.0000 Uani . . . . . .
O2 O 0.5534(2) 0.3631(6) 0.28988(14) 0.0097 1.0000 Uani . . . . . .
O3 O 0.5877(2) 0.3309(6) 0.20863(14) 0.0100 1.0000 Uani . . . . . .
O4 O 0.7152(2) 0.1755(7) 0.23664(14) 0.0108 1.0000 Uani . . . . . .
O5 O 0.6864(2) 0.1949(6) 0.31213(13) 0.0099 1.0000 Uani . . . . . .
O6 O 0.6721(2) 0.4936(6) 0.26874(14) 0.0108 1.0000 Uani . . . . . .
O7 O 0.5922(3) 0.4727(6) 0.41068(14) 0.0105 1.0000 Uani . . . . . .
O8 O 0.4925(3) 0.3742(6) 0.35390(14) 0.0103 1.0000 Uani . . . . . .
O9 O 0.6110(2) 0.1969(6) 0.37072(13) 0.0085 1.0000 Uani . . . . . .
O10 O 0.5822(2) 0.1909(6) 0.44958(13) 0.0075 1.0000 Uani . . . . . .
O11 O 0.4599(2) 0.3789(6) 0.42524(14) 0.0104 1.0000 Uani . . . . . .
O12 O 0.4906(3) 0.0659(6) 0.39221(14) 0.0103 1.0000 Uani . . . . . .
O13 O 0.7488(3) 0.4918(7) 0.42880(14) 0.0120 1.0000 Uani . . . . . .
O14 O 0.7234(2) 0.1794(6) 0.45968(14) 0.0077 1.0000 Uani . . . . . .
O15 O 0.8761(2) 0.3996(7) 0.40378(14) 0.0113 1.0000 Uani . . . . . .
O16 O 0.7516(2) 0.2117(6) 0.38063(14) 0.0099 1.0000 Uani . . . . . .
O17 O 0.8537(2) 0.3570(6) 0.48210(13) 0.0080 1.0000 Uani . . . . . .
O18 O 0.8497(2) 0.0685(6) 0.43270(15) 0.0116 1.0000 Uani . . . . . .
O19 O 0.6625(3) 0.7468(8) 0.22315(18) 0.0213 1.0000 Uani . . . . . .
O20 O 0.9999(3) 0.2889(7) 0.43243(17) 0.0185 1.0000 Uani . . . . . .
O21 O 0.3468(3) 0.3793(8) 0.37097(17) 0.0227 1.0000 Uani . . . . . .
O22 O 0.8079(3) 0.4703(8) 0.32985(16) 0.0203 1.0000 Uani . . . . . .
O23 O 0.9515(8) -0.1434(17) 0.5032(2) 0.1051 1.0000 Uani . . . . . .
O24 O 0.8173(7) 0.6907(10) 0.5084(3) 0.0641 1.0000 Uani . . . . . .
N1 N 0.7760(4) 0.3656(10) 0.0857(2) 0.0238 1.0000 Uani . . . . . .
N2 N 0.9266(3) 0.2399(8) 0.20894(19) 0.0161 1.0000 Uani . . . . . .
C1 C 0.8488(4) 0.3304(10) 0.1044(2) 0.0166 1.0000 Uani . . . . . .
C2 C 0.8474(4) 0.2971(10) 0.1480(2) 0.0181 1.0000 Uani . . . . . .
C3 C 0.9235(4) 0.2635(11) 0.1656(2) 0.0196 1.0000 Uani . . . . . .
C4 C 1.0010(4) 0.2302(10) 0.2281(2) 0.0164 1.0000 Uani . . . . . .
H1 H 0.6812 0.8119 0.2032 0.0253 1.0000 Uiso . . . . . .
H2 H 1.0183 0.2722 0.4590 0.0217 1.0000 Uiso . . . . . .
H3 H 0.3745 0.3111 0.3553 0.0258 1.0000 Uiso . . . . . .
H4 H 0.8247 0.5643 0.3162 0.0246 1.0000 Uiso . . . . . .
H5 H 0.8357 0.4602 0.3545 0.0246 1.0000 Uiso . . . . . .
H6 H 0.9496 -0.0856 0.4781 0.1400 1.0000 Uiso . . . . . .
H7 H 0.9190 -0.0900 0.5182 0.1400 1.0000 Uiso . . . . . .
H8 H 0.8247 0.7511 0.5159 0.0766 1.0000 Uiso . . . . . .
H9 H 0.8301 0.5812 0.4998 0.0766 1.0000 Uiso . . . . . .
H10 H 0.7481 0.2768 0.0886 0.0361 1.0000 Uiso . . . . . .
H11 H 0.7584 0.4561 0.0969 0.0362 1.0000 Uiso . . . . . .
H12 H 0.7780 0.3859 0.0603 0.0360 1.0000 Uiso . . . . . .
H13 H 0.8677 0.2332 0.0921 0.0192 1.0000 Uiso . . . . . .
H14 H 0.8789 0.4276 0.1011 0.0191 1.0000 Uiso . . . . . .
H15 H 0.8175 0.1990 0.1517 0.0222 1.0000 Uiso . . . . . .
H16 H 0.8287 0.3952 0.1604 0.0220 1.0000 Uiso . . . . . .
H17 H 0.9412 0.1622 0.1542 0.0241 1.0000 Uiso . . . . . .
H18 H 0.9533 0.3585 0.1603 0.0240 1.0000 Uiso . . . . . .
H19 H 0.9036 0.3244 0.2193 0.0240 1.0000 Uiso . . . . . .
H20 H 0.9033 0.1461 0.2140 0.0241 1.0000 Uiso . . . . . .
H21 H 1.0277 0.3276 0.2206 0.0190 1.0000 Uiso . . . . . .
H22 H 1.0234 0.1278 0.2201 0.0190 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.072130(15)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 . Se4 7_645 3.1794(14) yes
V1 . Se1 5_655 3.1984(13) yes
V1 . Se1 . 3.2288(13) yes
V1 . O1 . 1.615(5) yes
V1 . O2 . 2.018(5) yes
V1 . O3 . 2.023(5) yes
V1 . O4 . 2.019(5) yes
V1 . O5 . 2.011(5) yes
V1 . O6 . 2.192(5) yes
V2 . Se2 . 3.1925(14) yes
V2 . Se3 . 3.1726(13) yes
V2 . Se6 . 3.220(2) yes
V2 . Se7 . 3.230(11) yes
V2 . O7 . 1.602(5) yes
V2 . O8 . 1.964(5) yes
V2 . O9 . 1.877(5) yes
V2 . O10 . 1.902(5) yes
V2 . O11 . 2.009(5) yes
V2 . O12 . 2.170(5) yes
V3 . Se2 . 3.2186(13) yes
V3 . Se3 . 3.2570(14) yes
V3 . Se5 . 3.2544(15) yes
V3 . O13 . 1.614(5) yes
V3 . O14 . 2.040(5) yes
V3 . O15 . 2.009(5) yes
V3 . O16 . 2.016(5) yes
V3 . O17 . 2.016(5) yes
V3 . O18 . 2.241(5) yes
Se1 . O3 5_655 1.699(5) yes
Se1 . O2 . 1.697(5) yes
Se1 . O8 . 1.719(5) yes
Se2 . O5 . 1.671(5) yes
Se2 . O9 . 1.768(5) yes
Se2 . O16 . 1.688(5) yes
Se3 . O17 4_656 1.693(4) yes
Se3 . O10 . 1.750(4) yes
Se3 . O14 . 1.696(4) yes
Se4 . O4 7_655 1.697(5) yes
Se4 . O6 . 1.662(5) yes
Se4 . O19 . 1.757(6) yes
Se5 . O12 3_555 1.656(5) yes
Se5 . O15 . 1.699(5) yes
Se5 . O20 . 1.758(5) yes
Se6 . O18 3_455 1.667(5) yes
Se6 . O11 . 1.738(5) yes
Se6 . O21 . 1.796(6) yes
Se7 . O18 3_455 1.601(12) yes
Se7 . O11 . 1.625(11) yes
Se7 . O21 . 1.492(11) yes
O19 . H1 . 0.955 no
O20 . H2 . 0.955 no
O21 . H3 . 0.956 no
O22 . H4 . 0.952 no
O22 . H5 . 0.954 no
O23 . H6 . 0.978 no
O23 . H7 . 0.939 no
O24 . H8 . 0.970 no
O24 . H9 . 0.956 no
N1 . C1 . 1.479(10) yes
N1 . H10 . 0.891 no
N1 . H11 . 0.896 no
N1 . H12 . 0.894 no
N2 . C3 . 1.499(10) yes
N2 . C4 . 1.488(9) yes
N2 . H19 . 0.891 no
N2 . H20 . 0.890 no
C1 . C2 . 1.526(11) yes
C1 . H13 . 0.966 no
C1 . H14 . 0.970 no
C2 . C3 . 1.520(11) yes
C2 . H15 . 0.977 no
C2 . H16 . 0.970 no
C3 . H17 . 0.968 no
C3 . H18 . 0.968 no
C4 . C4 5_755 1.512(15) yes
C4 . H21 . 0.972 no
C4 . H22 . 0.968 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Se4 7_645 V1 . Se1 5_655 127.02(4) yes
Se4 7_645 V1 . Se1 . 139.47(4) yes
Se1 5_655 V1 . Se1 . 84.77(4) yes
Se4 7_645 V1 . O1 . 95.03(18) yes
Se1 5_655 V1 . O1 . 71.38(17) yes
Se1 . V1 . O1 . 69.81(17) yes
Se4 7_645 V1 . O2 . 147.78(15) yes
Se1 5_655 V1 . O2 . 85.20(14) yes
Se1 . V1 . O2 . 26.94(14) yes
O1 . V1 . O2 . 95.5(2) yes
Se4 7_645 V1 . O3 . 115.16(14) yes
Se1 5_655 V1 . O3 . 27.90(13) yes
Se1 . V1 . O3 . 104.12(14) yes
O1 . V1 . O3 . 97.0(2) yes
O2 . V1 . O3 . 93.6(2) yes
Se4 7_645 V1 . O4 . 28.27(13) yes
Se1 5_655 V1 . O4 . 102.07(14) yes
Se1 . V1 . O4 . 165.73(15) yes
O1 . V1 . O4 . 100.2(2) yes
O2 . V1 . O4 . 164.1(2) yes
Se4 7_645 V1 . O5 . 57.51(13) yes
Se1 5_655 V1 . O5 . 167.87(15) yes
Se1 . V1 . O5 . 86.57(14) yes
O1 . V1 . O5 . 97.6(2) yes
O2 . V1 . O5 . 90.9(2) yes
Se4 7_645 V1 . O6 . 91.66(14) yes
Se1 5_655 V1 . O6 . 106.81(13) yes
Se1 . V1 . O6 . 103.07(13) yes
O1 . V1 . O6 . 172.7(2) yes
O2 . V1 . O6 . 77.19(19) yes
O3 . V1 . O4 . 86.90(19) yes
O3 . V1 . O5 . 164.2(2) yes
O4 . V1 . O5 . 84.64(19) yes
O3 . V1 . O6 . 82.87(19) yes
O4 . V1 . O6 . 87.1(2) yes
O5 . V1 . O6 . 83.4(2) yes
Se2 . V2 . Se3 . 88.70(3) yes
Se2 . V2 . Se6 . 133.38(4) yes
Se3 . V2 . Se6 . 121.52(5) yes
Se2 . V2 . Se7 . 139.4(2) yes
Se3 . V2 . Se7 . 122.18(19) yes
Se6 . V2 . Se7 . 8.16(16) yes
Se2 . V2 . O7 . 70.30(18) yes
Se3 . V2 . O7 . 68.85(18) yes
Se6 . V2 . O7 . 87.51(19) yes
Se7 . V2 . O7 . 95.2(2) yes
Se2 . V2 . O8 . 86.17(14) yes
Se3 . V2 . O8 . 166.01(16) yes
Se6 . V2 . O8 . 55.65(14) yes
Se7 . V2 . O8 . 57.3(2) yes
O7 . V2 . O8 . 97.2(2) yes
Se2 . V2 . O9 . 27.92(15) yes
Se3 . V2 . O9 . 94.27(15) yes
Se6 . V2 . O9 . 142.90(15) yes
Se7 . V2 . O9 . 143.5(2) yes
O7 . V2 . O9 . 97.8(2) yes
Se2 . V2 . O10 . 104.03(14) yes
Se3 . V2 . O10 . 28.37(14) yes
Se6 . V2 . O10 . 119.27(15) yes
Se7 . V2 . O10 . 115.5(2) yes
O7 . V2 . O10 . 96.6(2) yes
Se2 . V2 . O11 . 160.13(15) yes
Se3 . V2 . O11 . 99.67(15) yes
Se6 . V2 . O11 . 28.37(14) yes
Se7 . V2 . O11 . 24.3(2) yes
O7 . V2 . O11 . 95.8(2) yes
Se2 . V2 . O12 . 109.66(13) yes
Se3 . V2 . O12 . 109.58(13) yes
Se6 . V2 . O12 . 93.57(15) yes
Se7 . V2 . O12 . 85.8(2) yes
O7 . V2 . O12 . 178.4(2) yes
O8 . V2 . O9 . 87.3(2) yes
O8 . V2 . O10 . 165.1(2) yes
O9 . V2 . O10 . 96.7(2) yes
O8 . V2 . O11 . 81.5(2) yes
O9 . V2 . O11 . 163.3(2) yes
O10 . V2 . O11 . 91.3(2) yes
O8 . V2 . O12 . 84.4(2) yes
O9 . V2 . O12 . 82.0(2) yes
O10 . V2 . O12 . 81.9(2) yes
O11 . V2 . O12 . 84.6(2) yes
Se2 . V3 . Se3 . 86.80(4) yes
Se2 . V3 . Se5 . 119.95(4) yes
Se3 . V3 . Se5 . 147.34(4) yes
Se2 . V3 . O13 . 72.43(18) yes
Se3 . V3 . O13 . 71.36(18) yes
Se5 . V3 . O13 . 97.64(18) yes
Se2 . V3 . O14 . 89.73(14) yes
Se3 . V3 . O14 . 26.49(13) yes
Se5 . V3 . O14 . 149.67(14) yes
O13 . V3 . O14 . 97.4(2) yes
Se2 . V3 . O15 . 94.70(14) yes
Se3 . V3 . O15 . 167.27(16) yes
Se5 . V3 . O15 . 26.12(14) yes
O13 . V3 . O15 . 97.0(2) yes
O14 . V3 . O15 . 165.6(2) yes
Se2 . V3 . O16 . 26.89(14) yes
Se3 . V3 . O16 . 97.78(14) yes
Se5 . V3 . O16 . 114.53(14) yes
O13 . V3 . O16 . 99.2(2) yes
O14 . V3 . O16 . 88.79(19) yes
Se2 . V3 . O17 . 171.10(15) yes
Se3 . V3 . O17 . 88.86(13) yes
Se5 . V3 . O17 . 61.86(13) yes
O13 . V3 . O17 . 98.8(2) yes
O14 . V3 . O17 . 89.85(19) yes
Se2 . V3 . O18 . 104.88(13) yes
Se3 . V3 . O18 . 107.08(13) yes
Se5 . V3 . O18 . 85.12(13) yes
O13 . V3 . O18 . 176.8(2) yes
O14 . V3 . O18 . 80.87(19) yes
O15 . V3 . O16 . 89.03(19) yes
O15 . V3 . O17 . 87.85(19) yes
O16 . V3 . O17 . 162.0(2) yes
O15 . V3 . O18 . 84.8(2) yes
O16 . V3 . O18 . 78.2(2) yes
O17 . V3 . O18 . 83.82(19) yes
O3 5_655 Se1 . V1 5_655 33.87(16) yes
O3 5_655 Se1 . V1 . 119.19(17) yes
V1 5_655 Se1 . V1 . 95.08(4) yes
O3 5_655 Se1 . O2 . 103.9(2) yes
V1 5_655 Se1 . O2 . 96.35(17) yes
V1 . Se1 . O2 . 32.60(16) yes
O3 5_655 Se1 . O8 . 95.2(2) yes
V1 5_655 Se1 . O8 . 129.09(16) yes
V1 . Se1 . O8 . 121.91(17) yes
O2 . Se1 . O8 . 98.5(2) yes
V2 . Se2 . V3 . 92.14(3) yes
V2 . Se2 . O5 . 122.76(17) yes
V3 . Se2 . O5 . 130.27(16) yes
V2 . Se2 . O9 . 29.81(15) yes
V3 . Se2 . O9 . 100.44(15) yes
O5 . Se2 . O9 . 97.3(2) yes
V2 . Se2 . O16 . 107.45(16) yes
V3 . Se2 . O16 . 32.71(17) yes
O5 . Se2 . O16 . 98.7(2) yes
O9 . Se2 . O16 . 99.3(2) yes
O17 4_656 Se3 . V2 . 126.61(16) yes
O17 4_656 Se3 . V3 . 127.47(16) yes
V2 . Se3 . V3 . 91.79(4) yes
O17 4_656 Se3 . O10 . 96.1(2) yes
V2 . Se3 . O10 . 31.08(15) yes
V3 . Se3 . O10 . 110.68(15) yes
O17 4_656 Se3 . O14 . 100.6(2) yes
V2 . Se3 . O14 . 97.66(16) yes
V3 . Se3 . O14 . 32.43(16) yes
O10 . Se3 . O14 . 100.3(2) yes
O4 7_655 Se4 . V1 7_655 34.31(16) yes
O4 7_655 Se4 . O6 . 100.8(2) yes
V1 7_655 Se4 . O6 . 133.12(17) yes
O4 7_655 Se4 . O19 . 98.9(3) yes
V1 7_655 Se4 . O19 . 102.62(19) yes
O6 . Se4 . O19 . 96.2(3) yes
O12 3_555 Se5 . V3 . 131.56(17) yes
O12 3_555 Se5 . O15 . 101.2(2) yes
V3 . Se5 . O15 . 31.37(16) yes
O12 3_555 Se5 . O20 . 98.9(3) yes
V3 . Se5 . O20 . 97.27(18) yes
O15 . Se5 . O20 . 97.0(3) yes
O18 3_455 Se6 . V2 . 132.17(19) yes
O18 3_455 Se6 . O11 . 99.4(2) yes
V2 . Se6 . O11 . 33.31(16) yes
O18 3_455 Se6 . O21 . 97.2(3) yes
V2 . Se6 . O21 . 97.38(19) yes
O11 . Se6 . O21 . 98.9(3) yes
O18 3_455 Se7 . V2 . 135.4(6) yes
O18 3_455 Se7 . O11 . 107.2(7) yes
V2 . Se7 . O11 . 30.6(3) yes
O18 3_455 Se7 . O21 . 114.3(8) yes
V2 . Se7 . O21 . 104.6(5) yes
O11 . Se7 . O21 . 118.9(6) yes
V1 . O2 . Se1 . 120.5(3) yes
V1 . O3 . Se1 5_655 118.2(3) yes
V1 . O4 . Se4 7_645 117.4(3) yes
V1 . O5 . Se2 . 125.1(3) yes
V1 . O6 . Se4 . 120.3(3) yes
V2 . O8 . Se1 . 120.3(3) yes
Se2 . O9 . V2 . 122.3(3) yes
V2 . O10 . Se3 . 120.6(2) yes
V2 . O11 . Se6 . 118.3(3) yes
V2 . O11 . Se7 . 125.1(5) yes
Se6 . O11 . Se7 . 15.2(3) yes
V2 . O12 . Se5 3_445 119.4(3) yes
V3 . O14 . Se3 . 121.1(3) yes
V3 . O15 . Se5 . 122.5(3) yes
V3 . O16 . Se2 . 120.4(3) yes
V3 . O17 . Se3 4_656 119.6(2) yes
V3 . O18 . Se6 3_545 119.8(3) yes
V3 . O18 . Se7 3_545 131.7(4) yes
Se6 3_545 O18 . Se7 3_545 16.0(3) yes
Se4 . O19 . H1 . 109.2 no
Se5 . O20 . H2 . 109.3 no
Se6 . O21 . Se7 . 12.1(4) yes
Se6 . O21 . H3 . 109.3 no
Se7 . O21 . H3 . 111.8 no
H4 . O22 . H5 . 108.9 no
H6 . O23 . H7 . 108.0 no
H8 . O24 . H9 . 107.3 no
C1 . N1 . H10 . 109.4 no
C1 . N1 . H11 . 109.3 no
H10 . N1 . H11 . 109.6 no
C1 . N1 . H12 . 109.4 no
H10 . N1 . H12 . 109.7 no
H11 . N1 . H12 . 109.4 no
C3 . N2 . C4 . 112.8(6) yes
C3 . N2 . H19 . 109.4 no
C4 . N2 . H19 . 109.6 no
C3 . N2 . H20 . 109.3 no
C4 . N2 . H20 . 109.2 no
H19 . N2 . H20 . 106.4 no
N1 . C1 . C2 . 110.8(6) yes
N1 . C1 . H13 . 108.9 no
C2 . C1 . H13 . 109.8 no
N1 . C1 . H14 . 108.9 no
C2 . C1 . H14 . 108.9 no
H13 . C1 . H14 . 109.6 no
C1 . C2 . C3 . 108.2(6) yes
C1 . C2 . H15 . 109.5 no
C3 . C2 . H15 . 109.9 no
C1 . C2 . H16 . 109.6 no
C3 . C2 . H16 . 109.6 no
H15 . C2 . H16 . 110.0 no
C2 . C3 . N2 . 111.0(6) yes
C2 . C3 . H17 . 109.4 no
N2 . C3 . H17 . 108.7 no
C2 . C3 . H18 . 109.1 no
N2 . C3 . H18 . 108.8 no
H17 . C3 . H18 . 109.9 no
C4 5_755 C4 . N2 . 109.0(7) yes
C4 5_755 C4 . H21 . 109.4 no
N2 . C4 . H21 . 109.2 no
C4 5_755 C4 . H22 . 109.8 no
N2 . C4 . H22 . 109.6 no
H21 . C4 . H22 . 109.9 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O19 . H1 . O22 7_655 161.5(4) 0.955 1.722 2.645(11) yes
O20 . H2 . O23 2_756 151.0(6) 0.955 1.705 2.582(11) yes
O21 . H3 . O3 5_655 135.6(4) 0.956 2.386 3.141(11) yes
O22 . H4 . O4 7_655 130.6(4) 0.952 2.093 2.807(11) yes
O22 . H5 . O15 . 167.0(4) 0.954 1.851 2.789(11) yes
O23 . H6 . O11 3_545 142.6(7) 0.978 1.870 2.713(11) yes
O24 . H8 . O23 1_565 113.0(6) 0.970 1.979 2.869(11) yes
O24 . H9 . O17 . 178.6(8) 0.956 1.946 2.902(11) yes
N1 . H10 . O13 7_645 134.7(5) 0.891 2.342 3.036(11) yes
N1 . H11 . O16 7_655 161.0(5) 0.896 2.185 3.046(11) yes
N1 . H12 . O24 6_564 146.8(5) 0.894 2.093 2.883(11) yes
C1 . H13 . O7 7_645 155.5(5) 0.966 2.206 3.111(11) yes
C1 . H14 . O9 7_655 134.2(5) 0.970 2.347 3.102(11) yes
C2 . H16 . O5 7_655 163.1(5) 0.970 2.586 3.525(11) yes
N2 . H19 . O1 7_655 143.5(4) 0.891 2.046 2.812(11) yes
N2 . H20 . O2 7_645 126.5(4) 0.890 2.397 3.013(11) yes
N2 . H20 . O6 7_645 160.5(4) 0.890 1.999 2.854(11) yes
C4 . H21 . O1 3_555 132.1(5) 0.972 2.453 3.187(11) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 13/08/13 at 10:37:20
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 13/08/13 at 10:37:20
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.010000 = SE(13) TO SE(14) 
END                                                                             
;
####################################################################### 
# 
# 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_[C4H16N2]2[VO(SeO3)(HSeO3]8-9-333H2O-compound-3
_database_code_depnum_ccdc_archive 'CCDC 1588070'
_audit_update_record             
;
2017-11-28 deposited with the CCDC.
2018-02-01 downloaded from the CCDC.
;

_cell_length_a                   17.9990(7)
_cell_length_b                   15.6580(6)
_cell_length_c                   26.0344(10)
_cell_angle_alpha                90
_cell_angle_beta                 113.803(2)
_cell_angle_gamma                90
_cell_volume                     6713.1(5)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
V 0.3005 0.5294 10.2971 6.8657 7.3511 0.4385 2.0703 26.8938 2.0571 102.4780
1.2199 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Se -0.0929 2.2259 17.0006 2.4098 5.8196 0.2726 3.9731 15.2372 4.3543 43.8163
2.8409 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C16 H64 N12 O40 Se8 V8 
# Dc =      2.08 Fooo =   5597.29 Mu =     54.96 M =   2103.95
# Found Formula = C8 H58.67 N6 O65.33 Se16 V8 
# Dc =      2.92 FOOO =   5597.29 Mu =     98.75 M =   2955.43

_chemical_formula_sum            'C8 H58.67 N6 O65.33 Se16 V8'
_chemical_formula_moiety         'C8 H58.67 N6 O65.33 Se16 V8'
_chemical_compound_source        ?
_chemical_formula_weight         2955.43


_cell_measurement_reflns_used    9380
_cell_measurement_theta_min      2
_cell_measurement_theta_max      31
_cell_measurement_temperature    100

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_min          0.108
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_max          0.374

_exptl_crystal_density_diffrn    2.924
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             5597.288
_exptl_absorpt_coefficient_mu    9.875

# Sheldrick geometric approximatio 0.24 0.34 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.24
_exptl_absorpt_correction_T_max  0.34
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      100
_diffrn_reflns_number            239522
_reflns_number_total             21388
_diffrn_reflns_av_R_equivalents  0.064
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 21388 
# Theoretical number of reflections is about 44826 


_diffrn_reflns_theta_min         1.236
_diffrn_reflns_theta_max         31.536
_diffrn_measured_fraction_theta_max 0.955

_diffrn_reflns_theta_full        28.697
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       38
_reflns_limit_h_min              -26
_reflns_limit_h_max              23
_reflns_limit_k_min              0
_reflns_limit_k_max              22
_reflns_limit_l_min              0
_reflns_limit_l_max              38

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -2.24
_refine_diff_density_max         1.97


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         17182
_refine_ls_number_restraints     0
_refine_ls_number_parameters     947
_oxford_refine_ls_R_factor_ref   0.0383
_refine_ls_wR_factor_ref         0.1020
_refine_ls_goodness_of_fit_ref   1.0242
_refine_ls_shift/su_max          0.0032663
_refine_ls_shift/su_mean         0.0000712


# The values computed from all data 
_oxford_reflns_number_all        21338
_refine_ls_R_factor_all          0.0534
_refine_ls_wR_factor_all         0.1724

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                18464
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_gt          0.1134

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² +25.32P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
V1 V -0.27822(3) 0.64362(3) 0.07618(2) 0.0041 1.0000 Uani . . . . . .
V2 V -0.53136(3) 0.89287(3) 0.32808(2) 0.0042 1.0000 Uani . . . . . .
V3 V -0.21642(3) 0.85084(3) 0.42234(2) 0.0042 1.0000 Uani . . . . . .
V4 V -0.46298(3) 0.88998(3) 0.171774(19) 0.0039 1.0000 Uani . . . . . .
V5 V 0.22210(3) 0.64635(3) 0.57565(2) 0.0042 1.0000 Uani . . . . . .
V6 V -0.03334(3) 0.60776(3) 0.329369(19) 0.0039 1.0000 Uani . . . . . .
V7 V 0.28303(3) 0.64211(3) 0.42216(2) 0.0043 1.0000 Uani . . . . . .
V8 V 0.03588(3) 0.60523(3) 0.171962(19) 0.0039 1.0000 Uani . . . . . .
Se1 Se -0.116760(16) 0.868821(17) 0.554355(11) 0.0040 1.0000 Uani . . . . . .
Se2 Se -0.381677(16) 0.857391(17) 0.444594(11) 0.0041 1.0000 Uani . . . . . .
Se3 Se -0.367705(16) 0.874867(17) 0.304722(11) 0.0039 1.0000 Uani . . . . . .
Se4 Se 0.371309(16) 0.616212(17) 0.692859(11) 0.0042 1.0000 Uani . . . . . .
Se5 Se 0.383899(16) 0.630492(17) 0.553869(11) 0.0040 1.0000 Uani . . . . . .
Se6 Se 0.118471(16) 0.639137(17) 0.444528(11) 0.0040 1.0000 Uani . . . . . .
Se7 Se 0.129982(16) 0.616433(17) 0.304779(11) 0.0041 1.0000 Uani . . . . . .
Se8 Se -0.128659(16) 0.615965(17) 0.194466(11) 0.0040 1.0000 Uani . . . . . .
Se9 Se -0.124600(16) 1.024111(17) 0.403354(11) 0.0051 1.0000 Uani . . . . . .
Se10 Se -0.364800(17) 0.725879(17) 0.153604(12) 0.0065 1.0000 Uani . . . . . .
Se11 Se -0.129176(17) 0.779180(18) 0.346337(12) 0.0061 1.0000 Uani . . . . . .
Se12 Se -0.115047(16) 0.517337(17) 0.405339(11) 0.0054 1.0000 Uani . . . . . .
Se13 Se 0.139309(16) 0.729914(17) 0.654636(11) 0.0057 1.0000 Uani . . . . . .
Se14 Se -0.389360(16) 0.485215(17) 0.095552(11) 0.0054 1.0000 Uani . . . . . .
Se15 Se 0.359530(18) 0.73371(2) 0.347706(13) 0.0113 1.0000 Uani . . . . . .
Se16 Se 0.376051(16) 0.468891(18) 0.405739(12) 0.0054 1.0000 Uani . . . . . .
O1 O -0.26375(12) 0.73093(13) 0.04970(8) 0.0071 1.0000 Uani . . . . . .
O2 O -0.18904(12) 0.58282(13) 0.07457(9) 0.0063 1.0000 Uani . . . . . .
O3 O -0.35635(12) 0.59598(13) 0.01016(8) 0.0064 1.0000 Uani . . . . . .
O4 O -0.37192(12) 0.68203(13) 0.09202(8) 0.0076 1.0000 Uani . . . . . .
O5 O -0.21455(12) 0.67280(13) 0.15500(8) 0.0062 1.0000 Uani . . . . . .
O6 O -0.29567(12) 0.52060(13) 0.11038(9) 0.0070 1.0000 Uani . . . . . .
O7 O -0.51445(13) 0.98189(13) 0.30364(9) 0.0094 1.0000 Uani . . . . . .
O8 O -0.43812(12) 0.82685(13) 0.32358(9) 0.0064 1.0000 Uani . . . . . .
O9 O -0.61207(12) 0.84220(14) 0.25600(8) 0.0084 1.0000 Uani . . . . . .
O10 O -0.62684(12) 0.92722(13) 0.34555(8) 0.0079 1.0000 Uani . . . . . .
O11 O -0.46477(12) 0.91608(13) 0.41004(8) 0.0071 1.0000 Uani . . . . . .
O12 O -0.54818(12) 0.76572(13) 0.35735(9) 0.0078 1.0000 Uani . . . . . .
O13 O -0.22161(12) 0.76408(13) 0.45414(9) 0.0080 1.0000 Uani . . . . . .
O14 O -0.31306(12) 0.91056(13) 0.42683(8) 0.0062 1.0000 Uani . . . . . .
O15 O -0.14134(12) 0.91515(13) 0.49137(8) 0.0071 1.0000 Uani . . . . . .
O16 O -0.11549(12) 0.82309(13) 0.40941(8) 0.0071 1.0000 Uani . . . . . .
O17 O -0.21415(12) 0.97625(13) 0.38395(9) 0.0074 1.0000 Uani . . . . . .
O18 O -0.28435(12) 0.81514(13) 0.34324(8) 0.0063 1.0000 Uani . . . . . .
O19 O -0.46946(13) 0.97751(13) 0.20227(9) 0.0081 1.0000 Uani . . . . . .
O20 O -0.56048(12) 0.82976(13) 0.17447(9) 0.0069 1.0000 Uani . . . . . .
O21 O -0.38640(12) 0.82953(13) 0.24122(8) 0.0067 1.0000 Uani . . . . . .
O22 O -0.36486(12) 0.91818(14) 0.15483(9) 0.0086 1.0000 Uani . . . . . .
O23 O -0.53413(12) 0.92822(13) 0.09266(9) 0.0068 1.0000 Uani . . . . . .
O24 O -0.45824(12) 0.76588(13) 0.13345(9) 0.0083 1.0000 Uani . . . . . .
O25 O 0.23667(12) 0.73220(13) 0.54768(9) 0.0076 1.0000 Uani . . . . . .
O26 O 0.31131(12) 0.58419(13) 0.57403(9) 0.0066 1.0000 Uani . . . . . .
O27 O 0.14300(12) 0.59659(13) 0.51116(8) 0.0067 1.0000 Uani . . . . . .
O28 O 0.13040(12) 0.68875(13) 0.59175(8) 0.0072 1.0000 Uani . . . . . .
O29 O 0.28632(12) 0.67486(13) 0.65415(9) 0.0068 1.0000 Uani . . . . . .
O30 O -0.20744(12) 0.47729(13) 0.38777(9) 0.0063 1.0000 Uani . . . . . .
O31 O -0.02152(13) 0.51751(13) 0.30373(9) 0.0092 1.0000 Uani . . . . . .
O32 O -0.11297(12) 0.66040(14) 0.25703(8) 0.0079 1.0000 Uani . . . . . .
O33 O -0.13023(12) 0.57909(13) 0.34778(9) 0.0081 1.0000 Uani . . . . . .
O34 O 0.03459(12) 0.58109(13) 0.41106(8) 0.0070 1.0000 Uani . . . . . .
O35 O 0.06177(12) 0.66849(13) 0.32400(9) 0.0071 1.0000 Uani . . . . . .
O36 O -0.03911(12) 0.73483(13) 0.36217(9) 0.0075 1.0000 Uani . . . . . .
O37 O 0.27806(13) 0.72997(13) 0.45296(9) 0.0081 1.0000 Uani . . . . . .
O38 O 0.18691(12) 0.58311(13) 0.42825(9) 0.0066 1.0000 Uani . . . . . .
O39 O 0.36117(12) 0.58160(13) 0.49185(8) 0.0067 1.0000 Uani . . . . . .
O40 O 0.38087(12) 0.67235(14) 0.40587(9) 0.0091 1.0000 Uani . . . . . .
O41 O 0.21536(12) 0.67233(13) 0.34330(9) 0.0074 1.0000 Uani . . . . . .
O42 O 0.28618(12) 0.51503(13) 0.38709(9) 0.0079 1.0000 Uani . . . . . .
O43 O 0.02327(13) 0.51826(13) 0.20041(9) 0.0084 1.0000 Uani . . . . . .
O44 O -0.06113(12) 0.66835(13) 0.17477(9) 0.0069 1.0000 Uani . . . . . .
O45 O 0.11367(12) 0.66165(13) 0.24212(8) 0.0077 1.0000 Uani . . . . . .
O46 O -0.03489(12) 0.57148(13) 0.09145(8) 0.0068 1.0000 Uani . . . . . .
O47 O 0.13486(12) 0.57542(13) 0.15630(8) 0.0073 1.0000 Uani . . . . . .
O48 O 0.04611(12) 0.73062(13) 0.13595(9) 0.0069 1.0000 Uani . . . . . .
O49 O -0.14038(14) 1.11358(13) 0.43935(9) 0.0115 1.0000 Uani . . . . . .
O50 O -0.37733(14) 0.63037(14) 0.18461(10) 0.0141 1.0000 Uani . . . . . .
O51 O -0.11390(14) 0.87293(14) 0.31528(10) 0.0148 1.0000 Uani . . . . . .
O52 O -0.12287(14) 0.59511(14) 0.45127(9) 0.0135 1.0000 Uani . . . . . .
O53 O 0.12256(13) 0.63490(14) 0.68363(10) 0.0135 1.0000 Uani . . . . . .
O54 O -0.38672(13) 0.40402(15) 0.05007(9) 0.0139 1.0000 Uani . . . . . .
O55 O 0.3494(3) 0.6527(2) 0.29928(14) 0.0623 1.0000 Uani . . . . . .
O56 O 0.36304(14) 0.37844(14) 0.44185(9) 0.0130 1.0000 Uani . . . . . .
O57 O -0.2115(4) 0.8454(5) 0.2110(3) 0.0174 0.3330 Uani . . . . . .
O58 O 0.04780(13) 0.89914(14) 0.45223(9) 0.0150 1.0000 Uani . . . . . .
O59 O 0.20965(13) 0.88907(14) 0.41049(10) 0.0138 1.0000 Uani . . . . . .
O60 O 0.50054(15) 0.78763(15) 0.49082(10) 0.0197 1.0000 Uani . . . . . .
O61 O -0.30409(14) 0.60888(14) 0.40970(10) 0.0154 1.0000 Uani . . . . . .
O62 O -0.28596(14) 0.64521(15) 0.29231(10) 0.0190 1.0000 Uani . . . . . .
O63 O -0.23242(18) 0.46118(17) 0.24704(12) 0.0352 1.0000 Uani . . . . . .
O64 O 0.45596(14) 0.39807(15) 0.55022(10) 0.0178 1.0000 Uani . . . . . .
O65 O -0.01393(18) 0.71148(17) 0.49819(12) 0.0413 1.0000 Uani . . . . . .
O66 O 0.2266(3) 0.4685(3) 0.25017(17) 0.0333 0.6660 Uani . . . . . .
O67 O 0.2541(5) 0.5370(5) 0.2569(3) 0.0296 0.3330 Uani . . . . . .
N1 N -0.27849(16) 1.07774(16) 0.46932(11) 0.0130 1.0000 Uani . . . . . .
N2 N -0.44375(16) 1.14360(16) 0.33156(11) 0.0112 1.0000 Uani . . . . . .
N3 N -0.53779(16) 1.14115(16) 0.17330(11) 0.0121 1.0000 Uani . . . . . .
N4 N 0.21240(18) 0.41349(17) 0.46551(11) 0.0167 1.0000 Uani . . . . . .
N5 N 0.04165(16) 0.35415(16) 0.32840(11) 0.0110 1.0000 Uani . . . . . .
N6 N -0.05538(15) 0.35485(16) 0.17004(11) 0.0100 1.0000 Uani . . . . . .
C1 C -0.35902(19) 1.11465(18) 0.43248(13) 0.0123 1.0000 Uani . . . . . .
C2 C -0.36097(18) 1.12187(18) 0.37388(13) 0.0115 1.0000 Uani . . . . . .
C3 C -0.44526(19) 1.14472(18) 0.27359(13) 0.0111 1.0000 Uani . . . . . .
C4 C -0.53319(18) 1.14596(19) 0.23137(13) 0.0110 1.0000 Uani . . . . . .
C5 C 0.1299(2) 0.38190(19) 0.42830(13) 0.0145 1.0000 Uani . . . . . .
C6 C 0.12579(18) 0.37125(18) 0.36928(12) 0.0118 1.0000 Uani . . . . . .
C7 C 0.03506(19) 0.35131(19) 0.26929(13) 0.0118 1.0000 Uani . . . . . .
C8 C -0.05325(19) 0.35423(19) 0.22768(13) 0.0114 1.0000 Uani . . . . . .
H1 H -0.1169 1.1048 0.4737 0.0199 1.0000 Uiso . . . . . .
H2 H -0.3347 0.6304 0.2233 0.0500 1.0000 Uiso . . . . . .
H3 H -0.1497 0.9021 0.2866 0.0500 1.0000 Uiso . . . . . .
H4 H -0.0973 0.6413 0.4592 0.0222 1.0000 Uiso . . . . . .
H5 H 0.1623 0.6102 0.7087 0.0247 1.0000 Uiso . . . . . .
H6 H -0.4290 0.3789 0.0361 0.0500 1.0000 Uiso . . . . . .
H7 H 0.2924 0.6405 0.2794 0.0753 1.0000 Uiso . . . . . .
H8 H 0.3848 0.3826 0.4765 0.0198 1.0000 Uiso . . . . . .
H9 H -0.2633 0.8712 0.1921 0.0607 0.3330 Uiso . . . . . .
H10 H -0.2109 0.7917 0.1940 0.0607 0.3330 Uiso . . . . . .
H11 H -0.0068 0.8800 0.4383 0.0179 1.0000 Uiso . . . . . .
H12 H 0.0499 0.9540 0.4373 0.0179 1.0000 Uiso . . . . . .
H13 H 0.2330 0.9348 0.3979 0.0165 1.0000 Uiso . . . . . .
H14 H 0.2338 0.8368 0.4068 0.0165 1.0000 Uiso . . . . . .
H15 H 0.5048 0.7735 0.5273 0.0238 1.0000 Uiso . . . . . .
H16 H 0.4937 0.7370 0.4693 0.0238 1.0000 Uiso . . . . . .
H17 H -0.2763 0.6613 0.4122 0.0184 1.0000 Uiso . . . . . .
H18 H -0.2789 0.5652 0.3971 0.0184 1.0000 Uiso . . . . . .
H19 H -0.2862 0.7001 0.3085 0.0226 1.0000 Uiso . . . . . .
H20 H -0.2331 0.6219 0.3088 0.0226 1.0000 Uiso . . . . . .
H21 H -0.2825 0.4247 0.2245 0.0420 1.0000 Uiso . . . . . .
H22 H -0.2393 0.5212 0.2456 0.0420 1.0000 Uiso . . . . . .
H23 H 0.4452 0.4513 0.5633 0.0213 1.0000 Uiso . . . . . .
H24 H 0.5128 0.3874 0.5664 0.0213 1.0000 Uiso . . . . . .
H25 H 0.0396 0.6961 0.5236 0.0500 1.0000 Uiso . . . . . .
H26 H -0.0110 0.7574 0.4753 0.0500 1.0000 Uiso . . . . . .
H27 H 0.2560 0.4769 0.2754 0.0500 1.0000 Uiso . . . . . .
H28 H 0.2402 0.5071 0.2278 0.0500 1.0000 Uiso . . . . . .
H29 H -0.2721 1.0231 0.4554 0.0159 1.0000 Uiso . . . . . .
H30 H -0.2361 1.1144 0.4693 0.0159 1.0000 Uiso . . . . . .
H31 H -0.2741 1.0716 0.5067 0.0159 1.0000 Uiso . . . . . .
H32 H -0.3674 1.1698 0.4490 0.0175 1.0000 Uiso . . . . . .
H33 H -0.4011 1.0725 0.4315 0.0163 1.0000 Uiso . . . . . .
H34 H -0.3246 1.1693 0.3737 0.0153 1.0000 Uiso . . . . . .
H35 H -0.3437 1.0682 0.3630 0.0156 1.0000 Uiso . . . . . .
H36 H -0.4814 1.1019 0.3333 0.0137 1.0000 Uiso . . . . . .
H37 H -0.4593 1.1982 0.3399 0.0137 1.0000 Uiso . . . . . .
H38 H -0.4197 1.0916 0.2676 0.0149 1.0000 Uiso . . . . . .
H39 H -0.4171 1.1981 0.2692 0.0149 1.0000 Uiso . . . . . .
H40 H -0.5631 1.0954 0.2367 0.0148 1.0000 Uiso . . . . . .
H41 H -0.5622 1.1974 0.2357 0.0142 1.0000 Uiso . . . . . .
H42 H -0.5937 1.1418 0.1471 0.0153 1.0000 Uiso . . . . . .
H43 H -0.5111 1.1890 0.1663 0.0153 1.0000 Uiso . . . . . .
H44 H -0.5134 1.0900 0.1685 0.0153 1.0000 Uiso . . . . . .
H45 H 0.2165 0.4211 0.5029 0.0207 1.0000 Uiso . . . . . .
H46 H 0.2226 0.4669 0.4519 0.0207 1.0000 Uiso . . . . . .
H47 H 0.2524 0.3733 0.4659 0.0207 1.0000 Uiso . . . . . .
H48 H 0.0888 0.4247 0.4288 0.0186 1.0000 Uiso . . . . . .
H49 H 0.1218 0.3251 0.4410 0.0174 1.0000 Uiso . . . . . .
H50 H 0.1587 0.3231 0.3675 0.0153 1.0000 Uiso . . . . . .
H51 H 0.1444 0.4236 0.3562 0.0156 1.0000 Uiso . . . . . .
H52 H 0.0072 0.3988 0.3314 0.0138 1.0000 Uiso . . . . . .
H53 H 0.0238 0.3013 0.3372 0.0138 1.0000 Uiso . . . . . .
H54 H 0.0636 0.2986 0.2637 0.0155 1.0000 Uiso . . . . . .
H55 H 0.0678 0.4012 0.2651 0.0153 1.0000 Uiso . . . . . .
H56 H -0.0813 0.4068 0.2317 0.0146 1.0000 Uiso . . . . . .
H57 H -0.0817 0.3035 0.2325 0.0145 1.0000 Uiso . . . . . .
H58 H -0.0302 0.3048 0.1644 0.0124 1.0000 Uiso . . . . . .
H59 H -0.1104 0.3569 0.1432 0.0124 1.0000 Uiso . . . . . .
H60 H -0.0274 0.4039 0.1654 0.0124 1.0000 Uiso . . . . . .

_refine_ls_extinction_coef       15(4)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.0185738(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 . Se1 4_564 3.1842(5) yes
V1 . Se8 . 3.1977(5) yes
V1 . Se10 . 3.2689(5) yes
V1 . O1 . 1.599(2) yes
V1 . O2 . 1.881(2) yes
V1 . O3 . 1.881(2) yes
V1 . O4 . 1.984(2) yes
V1 . O5 . 1.958(2) yes
V1 . O6 . 2.197(2) yes
V2 . Se14 3_455 3.2203(5) yes
V2 . Se2 . 3.1893(5) yes
V2 . Se3 . 3.2514(5) yes
V2 . O7 . 1.611(2) yes
V2 . O8 . 2.014(2) yes
V2 . O9 . 2.015(2) yes
V2 . O10 . 2.020(2) yes
V2 . O11 . 2.014(2) yes
V2 . O12 . 2.196(2) yes
V3 . Se2 . 3.2535(5) yes
V3 . Se3 . 3.1941(5) yes
V3 . Se11 . 3.1855(5) yes
V3 . O13 . 1.613(2) yes
V3 . O14 . 2.019(2) yes
V3 . O15 . 2.027(2) yes
V3 . O16 . 2.024(2) yes
V3 . O17 . 2.211(2) yes
V3 . O18 . 2.004(2) yes
V4 . Se5 4_464 3.2081(5) yes
V4 . Se4 4_464 3.2447(5) yes
V4 . Se16 3_555 3.2551(5) yes
V4 . Se10 . 3.2595(5) yes
V4 . O19 . 1.612(2) yes
V4 . O20 . 2.018(2) yes
V4 . O21 . 2.013(2) yes
V4 . O22 . 2.034(2) yes
V4 . O23 . 2.028(2) yes
V4 . O24 . 2.202(2) yes
V5 . O30 2_566 2.220(2) yes
V5 . Se4 . 3.1831(5) yes
V5 . Se5 . 3.1934(5) yes
V5 . Se13 . 3.2611(5) yes
V5 . O25 . 1.600(2) yes
V5 . O26 . 1.893(2) yes
V5 . O27 . 1.877(2) yes
V5 . O28 . 1.975(2) yes
V5 . O29 . 1.951(2) yes
V6 . Se6 . 3.1754(5) yes
V6 . Se7 . 3.2540(5) yes
V6 . Se12 . 3.2291(5) yes
V6 . O31 . 1.613(2) yes
V6 . O32 . 2.025(2) yes
V6 . O33 . 2.037(2) yes
V6 . O34 . 2.023(2) yes
V6 . O35 . 2.012(2) yes
V6 . O36 . 2.184(2) yes
V7 . Se6 . 3.2414(5) yes
V7 . Se7 . 3.2083(5) yes
V7 . Se15 . 3.1407(6) yes
V7 . O37 . 1.613(2) yes
V7 . O38 . 2.023(2) yes
V7 . O39 . 2.027(2) yes
V7 . O40 . 2.027(2) yes
V7 . O41 . 1.976(2) yes
V7 . O42 . 2.200(2) yes
V8 . Se1 4_564 3.2090(5) yes
V8 . Se9 3_545 3.2458(5) yes
V8 . Se8 . 3.2470(5) yes
V8 . O43 . 1.610(2) yes
V8 . O44 . 2.033(2) yes
V8 . O45 . 2.003(2) yes
V8 . O46 . 2.035(2) yes
V8 . O47 . 2.036(2) yes
V8 . O48 . 2.215(2) yes
Se1 . O2 4_565 1.759(2) yes
Se1 . O46 4_565 1.682(2) yes
Se1 . O15 . 1.681(2) yes
Se2 . O3 4_565 1.740(2) yes
Se2 . O11 . 1.675(2) yes
Se2 . O14 . 1.701(2) yes
Se3 . O8 . 1.707(2) yes
Se3 . O18 . 1.708(2) yes
Se3 . O21 . 1.703(2) yes
Se4 . O20 4_665 1.711(2) yes
Se4 . O9 4_665 1.679(2) yes
Se4 . O29 . 1.719(2) yes
Se5 . O23 4_665 1.685(2) yes
Se5 . O26 . 1.750(2) yes
Se5 . O39 . 1.682(2) yes
Se6 . O27 . 1.741(2) yes
Se6 . O34 . 1.674(2) yes
Se6 . O38 . 1.699(2) yes
Se7 . O35 . 1.708(2) yes
Se7 . O41 . 1.700(2) yes
Se7 . O45 . 1.692(2) yes
Se8 . O5 . 1.719(2) yes
Se8 . O32 . 1.687(2) yes
Se8 . O44 . 1.708(2) yes
Se9 . O47 3_555 1.691(2) yes
Se9 . O17 . 1.661(2) yes
Se9 . O49 . 1.771(2) yes
Se10 . O4 . 1.701(2) yes
Se10 . O24 . 1.668(2) yes
Se10 . O50 . 1.757(2) yes
Se11 . O16 . 1.704(2) yes
Se11 . O36 . 1.655(2) yes
Se11 . O51 . 1.750(2) yes
Se12 . O30 . 1.659(2) yes
Se12 . O33 . 1.710(2) yes
Se12 . O52 . 1.752(2) yes
Se13 . O48 4_565 1.666(2) yes
Se13 . O28 . 1.706(2) yes
Se13 . O53 . 1.749(2) yes
Se14 . O10 3_445 1.703(2) yes
Se14 . O6 . 1.666(2) yes
Se14 . O54 . 1.751(2) yes
Se15 . O12 1_655 1.654(2) yes
Se15 . O40 . 1.701(2) yes
Se15 . O55 . 1.746(3) yes
Se16 . O22 3_545 1.703(2) yes
Se16 . O42 . 1.655(2) yes
Se16 . O56 . 1.767(2) yes
O49 . H1 . 0.831 no
O50 . H2 . 0.988 no
O51 . H3 . 0.890 no
O52 . H4 . 0.837 no
O53 . H5 . 0.843 no
O54 . H6 . 0.803 no
O55 . H7 . 0.962 no
O56 . H8 . 0.827 no
O57 . H9 . 0.951 no
O57 . H10 . 0.952 no
O58 . H11 . 0.948 no
O58 . H12 . 0.950 no
O59 . H13 . 0.954 no
O59 . H14 . 0.949 no
O60 . H15 . 0.948 no
O60 . H16 . 0.950 no
O61 . H17 . 0.949 no
O61 . H18 . 0.950 no
O62 . H19 . 0.957 no
O62 . H20 . 0.946 no
O63 . H21 . 0.947 no
O63 . H22 . 0.947 no
O64 . H23 . 0.949 no
O64 . H24 . 0.950 no
O65 . H25 . 0.953 no
O65 . H26 . 0.949 no
O66 . O67 . 1.164(9) yes
O66 . H27 . 0.669 no
O66 . H28 . 0.939 no
O67 . H27 . 1.050 no
O67 . H28 . 0.840 no
N1 . C1 . 1.494(4) yes
N1 . H29 . 0.955 no
N1 . H30 . 0.956 no
N1 . H31 . 0.950 no
N2 . C2 . 1.491(4) yes
N2 . C3 . 1.499(4) yes
N2 . H36 . 0.955 no
N2 . H37 . 0.952 no
N3 . C4 . 1.482(4) yes
N3 . H42 . 0.961 no
N3 . H43 . 0.946 no
N3 . H44 . 0.945 no
N4 . C5 . 1.493(4) yes
N4 . H45 . 0.954 no
N4 . H46 . 0.954 no
N4 . H47 . 0.953 no
N5 . C6 . 1.482(4) yes
N5 . C7 . 1.496(4) yes
N5 . H52 . 0.959 no
N5 . H53 . 0.949 no
N6 . C8 . 1.485(4) yes
N6 . H58 . 0.946 no
N6 . H59 . 0.954 no
N6 . H60 . 0.952 no
C1 . C2 . 1.516(4) yes
C1 . H32 . 1.002 no
C1 . H33 . 0.997 no
C2 . H34 . 0.991 no
C2 . H35 . 0.977 no
C3 . C4 . 1.520(4) yes
C3 . H38 . 0.993 no
C3 . H39 . 1.008 no
C4 . H40 . 0.998 no
C4 . H41 . 0.990 no
C5 . C6 . 1.517(4) yes
C5 . H48 . 1.001 no
C5 . H49 . 0.980 no
C6 . H50 . 0.971 no
C6 . H51 . 0.996 no
C7 . C8 . 1.521(4) yes
C7 . H54 . 1.014 no
C7 . H55 . 1.011 no
C8 . H56 . 0.993 no
C8 . H57 . 0.980 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Se1 4_564 V1 . Se8 . 71.903(12) yes
Se1 4_564 V1 . Se10 . 146.171(17) yes
Se8 . V1 . Se10 . 83.402(13) yes
Se1 4_564 V1 . O1 . 69.89(7) yes
Se8 . V1 . O1 . 108.10(8) yes
Se10 . V1 . O1 . 97.48(7) yes
Se1 4_564 V1 . O2 . 27.95(6) yes
Se8 . V1 . O2 . 63.82(6) yes
Se10 . V1 . O2 . 146.78(7) yes
O1 . V1 . O2 . 97.70(10) yes
Se1 4_564 V1 . O3 . 102.25(6) yes
Se8 . V1 . O3 . 148.73(7) yes
Se10 . V1 . O3 . 110.68(6) yes
O1 . V1 . O3 . 97.86(10) yes
O2 . V1 . O3 . 96.25(9) yes
Se1 4_564 V1 . O4 . 165.72(6) yes
Se8 . V1 . O4 . 107.26(6) yes
Se10 . V1 . O4 . 25.28(6) yes
O1 . V1 . O4 . 97.50(10) yes
O2 . V1 . O4 . 164.25(9) yes
Se1 4_564 V1 . O5 . 90.63(6) yes
Se8 . V1 . O5 . 27.54(6) yes
Se10 . V1 . O5 . 59.00(6) yes
O1 . V1 . O5 . 97.13(10) yes
O2 . V1 . O5 . 89.87(9) yes
Se1 4_564 V1 . O6 . 107.98(5) yes
Se8 . V1 . O6 . 72.15(5) yes
Se10 . V1 . O6 . 85.06(6) yes
O1 . V1 . O6 . 177.46(9) yes
O2 . V1 . O6 . 80.11(8) yes
O3 . V1 . O4 . 85.72(9) yes
O3 . V1 . O5 . 162.89(9) yes
O4 . V1 . O5 . 84.18(8) yes
O3 . V1 . O6 . 81.15(8) yes
O4 . V1 . O6 . 84.78(8) yes
O5 . V1 . O6 . 84.20(8) yes
Se14 3_455 V2 . Se2 . 84.590(14) yes
Se14 3_455 V2 . Se3 . 144.592(17) yes
Se2 . V2 . Se3 . 71.428(12) yes
Se14 3_455 V2 . O7 . 93.25(8) yes
Se2 . V2 . O7 . 107.73(8) yes
Se3 . V2 . O7 . 70.82(8) yes
Se14 3_455 V2 . O8 . 148.60(6) yes
Se2 . V2 . O8 . 64.03(6) yes
Se3 . V2 . O8 . 26.58(6) yes
O7 . V2 . O8 . 97.26(10) yes
Se14 3_455 V2 . O9 . 114.78(6) yes
Se2 . V2 . O9 . 146.29(6) yes
Se3 . V2 . O9 . 99.14(6) yes
O7 . V2 . O9 . 98.80(10) yes
O8 . V2 . O9 . 92.76(9) yes
Se14 3_455 V2 . O10 . 27.40(6) yes
Se2 . V2 . O10 . 107.53(6) yes
Se3 . V2 . O10 . 169.26(6) yes
O7 . V2 . O10 . 99.90(10) yes
O8 . V2 . O10 . 162.60(9) yes
Se14 3_455 V2 . O11 . 59.16(6) yes
Se2 . V2 . O11 . 27.23(6) yes
Se3 . V2 . O11 . 90.99(6) yes
O7 . V2 . O11 . 97.80(10) yes
O8 . V2 . O11 . 90.05(8) yes
Se14 3_455 V2 . O12 . 92.02(6) yes
Se2 . V2 . O12 . 72.18(6) yes
Se3 . V2 . O12 . 104.39(5) yes
O7 . V2 . O12 . 174.69(10) yes
O8 . V2 . O12 . 77.86(8) yes
O9 . V2 . O10 . 87.44(8) yes
O9 . V2 . O11 . 162.67(9) yes
O10 . V2 . O11 . 84.83(8) yes
O9 . V2 . O12 . 79.49(8) yes
O10 . V2 . O12 . 85.09(8) yes
O11 . V2 . O12 . 84.40(8) yes
Se2 . V3 . Se3 . 71.340(12) yes
Se2 . V3 . Se11 . 146.825(17) yes
Se3 . V3 . Se11 . 83.642(14) yes
Se2 . V3 . O13 . 71.86(7) yes
Se3 . V3 . O13 . 112.81(8) yes
Se11 . V3 . O13 . 99.64(8) yes
Se2 . V3 . O14 . 26.40(6) yes
Se3 . V3 . O14 . 65.16(6) yes
Se11 . V3 . O14 . 148.33(6) yes
O13 . V3 . O14 . 97.50(9) yes
Se2 . V3 . O15 . 99.02(6) yes
Se3 . V3 . O15 . 142.82(6) yes
Se11 . V3 . O15 . 113.97(6) yes
O13 . V3 . O15 . 96.85(9) yes
O14 . V3 . O15 . 90.02(8) yes
Se2 . V3 . O16 . 169.40(6) yes
Se3 . V3 . O16 . 109.94(6) yes
Se11 . V3 . O16 . 28.42(6) yes
O13 . V3 . O16 . 98.42(10) yes
O14 . V3 . O16 . 163.96(8) yes
Se2 . V3 . O17 . 103.74(5) yes
Se3 . V3 . O17 . 68.05(5) yes
Se11 . V3 . O17 . 85.90(6) yes
O13 . V3 . O17 . 174.45(10) yes
O14 . V3 . O17 . 77.78(8) yes
Se2 . V3 . O18 . 88.24(6) yes
Se3 . V3 . O18 . 28.02(6) yes
Se11 . V3 . O18 . 60.84(6) yes
O13 . V3 . O18 . 98.91(10) yes
O14 . V3 . O18 . 90.35(8) yes
O15 . V3 . O16 . 86.11(8) yes
O15 . V3 . O17 . 80.34(8) yes
O16 . V3 . O17 . 86.22(8) yes
O15 . V3 . O18 . 164.05(8) yes
O16 . V3 . O18 . 89.17(8) yes
O17 . V3 . O18 . 84.16(8) yes
Se5 4_464 V4 . Se4 4_464 70.460(12) yes
Se5 4_464 V4 . Se16 3_555 83.513(13) yes
Se4 4_464 V4 . Se16 3_555 145.175(17) yes
Se5 4_464 V4 . Se10 . 95.110(14) yes
Se4 4_464 V4 . Se10 . 126.171(16) yes
Se16 3_555 V4 . Se10 . 77.575(12) yes
Se5 4_464 V4 . O19 . 110.57(8) yes
Se4 4_464 V4 . O19 . 71.81(8) yes
Se16 3_555 V4 . O19 . 97.53(8) yes
Se10 . V4 . O19 . 153.28(8) yes
Se5 4_464 V4 . O20 . 64.11(6) yes
Se4 4_464 V4 . O20 . 26.95(6) yes
Se16 3_555 V4 . O20 . 147.26(6) yes
Se10 . V4 . O20 . 99.59(6) yes
O19 . V4 . O20 . 98.25(10) yes
Se5 4_464 V4 . O21 . 145.56(6) yes
Se4 4_464 V4 . O21 . 100.19(6) yes
Se16 3_555 V4 . O21 . 114.14(6) yes
Se10 . V4 . O21 . 62.93(6) yes
O19 . V4 . O21 . 96.71(9) yes
Se5 4_464 V4 . O22 . 107.45(6) yes
Se4 4_464 V4 . O22 . 168.82(6) yes
Se16 3_555 V4 . O22 . 26.68(6) yes
Se10 . V4 . O22 . 64.57(6) yes
O19 . V4 . O22 . 99.44(10) yes
Se5 4_464 V4 . O23 . 27.27(6) yes
Se4 4_464 V4 . O23 . 86.21(6) yes
Se16 3_555 V4 . O23 . 61.49(6) yes
Se10 . V4 . O23 . 104.03(6) yes
O19 . V4 . O23 . 96.19(10) yes
Se5 4_464 V4 . O24 . 69.74(5) yes
Se4 4_464 V4 . O24 . 104.87(6) yes
Se16 3_555 V4 . O24 . 86.43(6) yes
Se10 . V4 . O24 . 27.87(5) yes
O19 . V4 . O24 . 176.03(10) yes
O20 . V4 . O21 . 92.23(8) yes
O20 . V4 . O22 . 162.21(9) yes
O21 . V4 . O22 . 87.55(8) yes
O20 . V4 . O23 . 88.38(8) yes
O21 . V4 . O23 . 166.87(8) yes
O22 . V4 . O23 . 87.89(8) yes
O20 . V4 . O24 . 78.27(8) yes
O21 . V4 . O24 . 81.62(8) yes
O22 . V4 . O24 . 84.11(8) yes
O23 . V4 . O24 . 85.66(8) yes
O30 2_566 V5 . Se4 . 70.11(5) yes
O30 2_566 V5 . Se5 . 106.45(5) yes
Se4 . V5 . Se5 . 71.435(12) yes
O30 2_566 V5 . Se13 . 85.16(5) yes
Se4 . V5 . Se13 . 83.017(13) yes
Se5 . V5 . Se13 . 145.560(17) yes
O30 2_566 V5 . O25 . 176.08(9) yes
Se4 . V5 . O25 . 109.33(8) yes
Se5 . V5 . O25 . 69.86(7) yes
Se13 . V5 . O25 . 98.65(7) yes
O30 2_566 V5 . O26 . 79.04(8) yes
Se4 . V5 . O26 . 63.25(6) yes
Se5 . V5 . O26 . 27.54(6) yes
Se13 . V5 . O26 . 145.90(7) yes
O25 . V5 . O26 . 97.21(10) yes
O30 2_566 V5 . O27 . 80.98(8) yes
Se4 . V5 . O27 . 146.91(7) yes
Se5 . V5 . O27 . 103.05(6) yes
Se13 . V5 . O27 . 110.85(6) yes
O25 . V5 . O27 . 98.40(10) yes
O30 2_566 V5 . O28 . 87.01(8) yes
Se4 . V5 . O28 . 107.48(6) yes
Se5 . V5 . O28 . 164.61(6) yes
Se13 . V5 . O28 . 25.50(6) yes
O25 . V5 . O28 . 96.82(10) yes
O30 2_566 V5 . O29 . 82.70(8) yes
Se4 . V5 . O29 . 27.83(6) yes
Se5 . V5 . O29 . 90.38(6) yes
Se13 . V5 . O29 . 58.39(6) yes
O25 . V5 . O29 . 98.50(10) yes
O26 . V5 . O27 . 96.36(9) yes
O26 . V5 . O28 . 165.23(9) yes
O27 . V5 . O28 . 86.12(9) yes
O26 . V5 . O29 . 89.52(9) yes
O27 . V5 . O29 . 161.25(9) yes
O28 . V5 . O29 . 83.87(8) yes
Se6 . V6 . Se7 . 71.208(12) yes
Se6 . V6 . Se12 . 85.446(14) yes
Se7 . V6 . Se12 . 144.066(17) yes
Se6 . V6 . O31 . 108.62(8) yes
Se7 . V6 . O31 . 71.02(8) yes
Se12 . V6 . O31 . 92.18(8) yes
Se6 . V6 . O32 . 146.24(6) yes
Se7 . V6 . O32 . 99.01(6) yes
Se12 . V6 . O32 . 114.94(6) yes
O31 . V6 . O32 . 97.69(10) yes
Se6 . V6 . O33 . 107.71(6) yes
Se7 . V6 . O33 . 169.39(6) yes
Se12 . V6 . O33 . 27.65(6) yes
O31 . V6 . O33 . 99.94(10) yes
O32 . V6 . O33 . 87.52(8) yes
Se6 . V6 . O34 . 27.72(6) yes
Se7 . V6 . O34 . 90.27(6) yes
Se12 . V6 . O34 . 59.81(6) yes
O31 . V6 . O34 . 97.43(10) yes
O32 . V6 . O34 . 164.18(9) yes
Se6 . V6 . O35 . 63.92(6) yes
Se7 . V6 . O35 . 26.49(6) yes
Se12 . V6 . O35 . 149.37(6) yes
O31 . V6 . O35 . 97.32(10) yes
O32 . V6 . O35 . 92.62(9) yes
Se6 . V6 . O36 . 69.42(5) yes
Se7 . V6 . O36 . 103.19(5) yes
Se12 . V6 . O36 . 93.13(6) yes
O31 . V6 . O36 . 174.16(10) yes
O32 . V6 . O36 . 82.26(8) yes
O33 . V6 . O34 . 85.34(8) yes
O33 . V6 . O35 . 162.57(9) yes
O34 . V6 . O35 . 90.02(8) yes
O33 . V6 . O36 . 85.89(8) yes
O34 . V6 . O36 . 83.16(8) yes
O35 . V6 . O36 . 76.86(8) yes
Se6 . V7 . Se7 . 70.961(12) yes
Se6 . V7 . Se15 . 141.030(17) yes
Se7 . V7 . Se15 . 83.753(14) yes
Se6 . V7 . O37 . 71.63(8) yes
Se7 . V7 . O37 . 112.45(8) yes
Se15 . V7 . O37 . 92.49(8) yes
Se6 . V7 . O38 . 26.75(6) yes
Se7 . V7 . O38 . 65.47(6) yes
Se15 . V7 . O38 . 149.17(6) yes
O37 . V7 . O38 . 97.45(10) yes
Se6 . V7 . O39 . 100.76(6) yes
Se7 . V7 . O39 . 144.38(6) yes
Se15 . V7 . O39 . 116.57(6) yes
O37 . V7 . O39 . 96.39(9) yes
O38 . V7 . O39 . 91.30(8) yes
Se6 . V7 . O40 . 167.18(6) yes
Se7 . V7 . O40 . 108.33(6) yes
Se15 . V7 . O40 . 29.52(6) yes
O37 . V7 . O40 . 97.59(10) yes
O38 . V7 . O40 . 164.96(9) yes
Se6 . V7 . O41 . 88.02(6) yes
Se7 . V7 . O41 . 26.89(6) yes
Se15 . V7 . O41 . 59.29(6) yes
O37 . V7 . O41 . 100.24(10) yes
O38 . V7 . O41 . 90.16(8) yes
Se6 . V7 . O42 . 103.89(6) yes
Se7 . V7 . O42 . 69.35(5) yes
Se15 . V7 . O42 . 93.78(6) yes
O37 . V7 . O42 . 173.64(10) yes
O38 . V7 . O42 . 77.62(8) yes
O39 . V7 . O40 . 87.07(8) yes
O39 . V7 . O41 . 162.97(9) yes
O40 . V7 . O41 . 87.13(8) yes
O39 . V7 . O42 . 79.85(8) yes
O40 . V7 . O42 . 87.38(8) yes
O41 . V7 . O42 . 83.90(8) yes
Se1 4_564 V8 . Se9 3_545 85.046(13) yes
Se1 4_564 V8 . Se8 . 70.950(12) yes
Se9 3_545 V8 . Se8 . 146.739(17) yes
Se1 4_564 V8 . O43 . 108.71(8) yes
Se9 3_545 V8 . O43 . 98.16(8) yes
Se8 . V8 . O43 . 69.66(8) yes
Se1 4_564 V8 . O44 . 63.63(6) yes
Se9 3_545 V8 . O44 . 148.32(6) yes
Se8 . V8 . O44 . 27.03(6) yes
O43 . V8 . O44 . 96.43(10) yes
Se1 4_564 V8 . O45 . 145.93(6) yes
Se9 3_545 V8 . O45 . 112.97(6) yes
Se8 . V8 . O45 . 99.52(6) yes
O43 . V8 . O45 . 97.47(10) yes
O44 . V8 . O45 . 92.70(9) yes
Se1 4_564 V8 . O46 . 27.26(6) yes
Se9 3_545 V8 . O46 . 62.10(6) yes
Se8 . V8 . O46 . 87.82(6) yes
O43 . V8 . O46 . 96.22(10) yes
O44 . V8 . O46 . 88.49(8) yes
Se1 4_564 V8 . O47 . 108.62(6) yes
Se9 3_545 V8 . O47 . 26.57(6) yes
Se8 . V8 . O47 . 169.63(6) yes
O43 . V8 . O47 . 101.28(10) yes
O44 . V8 . O47 . 162.24(9) yes
Se1 4_564 V8 . O48 . 70.69(5) yes
Se9 3_545 V8 . O48 . 86.91(5) yes
Se8 . V8 . O48 . 105.55(5) yes
O43 . V8 . O48 . 174.85(10) yes
O44 . V8 . O48 . 78.68(8) yes
O45 . V8 . O46 . 166.04(9) yes
O45 . V8 . O47 . 86.43(8) yes
O46 . V8 . O47 . 88.21(8) yes
O45 . V8 . O48 . 81.27(8) yes
O46 . V8 . O48 . 85.34(8) yes
O47 . V8 . O48 . 83.66(8) yes
O2 4_565 Se1 . O46 4_565 99.86(10) yes
O2 4_565 Se1 . V1 4_565 30.08(7) yes
O46 4_565 Se1 . V1 4_565 125.64(7) yes
O2 4_565 Se1 . V8 4_565 96.42(7) yes
O46 4_565 Se1 . V8 4_565 33.64(7) yes
V1 4_565 Se1 . V8 4_565 109.211(14) yes
O2 4_565 Se1 . O15 . 99.84(10) yes
O46 4_565 Se1 . O15 . 98.33(10) yes
V1 4_565 Se1 . O15 . 107.50(7) yes
V8 4_565 Se1 . O15 . 131.53(7) yes
O3 4_565 Se2 . V2 . 130.27(7) yes
O3 4_565 Se2 . V3 . 106.95(7) yes
V2 . Se2 . V3 . 108.553(14) yes
O3 4_565 Se2 . O11 . 96.91(10) yes
V2 . Se2 . O11 . 33.39(7) yes
V3 . Se2 . O11 . 127.17(7) yes
O3 4_565 Se2 . O14 . 97.46(10) yes
V2 . Se2 . O14 . 94.79(7) yes
V3 . Se2 . O14 . 31.86(7) yes
O11 . Se2 . O14 . 100.05(10) yes
V3 . Se3 . V2 . 108.486(14) yes
V3 . Se3 . O8 . 96.72(7) yes
V2 . Se3 . O8 . 31.86(7) yes
V3 . Se3 . O18 . 33.45(7) yes
V2 . Se3 . O18 . 125.81(7) yes
O8 . Se3 . O18 . 99.68(10) yes
V3 . Se3 . O21 . 129.75(7) yes
V2 . Se3 . O21 . 112.25(7) yes
O8 . Se3 . O21 . 102.52(10) yes
O18 . Se3 . O21 . 97.14(9) yes
O20 4_665 Se4 . O9 4_665 102.58(10) yes
O20 4_665 Se4 . V5 . 94.68(7) yes
O9 4_665 Se4 . V5 . 128.99(7) yes
O20 4_665 Se4 . V4 4_665 32.32(7) yes
O9 4_665 Se4 . V4 4_665 111.38(7) yes
V5 . Se4 . V4 4_665 108.650(14) yes
O20 4_665 Se4 . O29 . 98.11(10) yes
O9 4_665 Se4 . O29 . 97.56(10) yes
V5 . Se4 . O29 . 31.99(7) yes
V4 4_665 Se4 . O29 . 125.32(7) yes
O23 4_665 Se5 . V5 . 125.22(7) yes
O23 4_665 Se5 . V4 4_665 33.46(7) yes
V5 . Se5 . V4 4_665 109.312(14) yes
O23 4_665 Se5 . O26 . 99.98(10) yes
V5 . Se5 . O26 . 30.01(7) yes
V4 4_665 Se5 . O26 . 97.39(7) yes
O23 4_665 Se5 . O39 . 98.16(10) yes
V5 . Se5 . O39 . 108.67(7) yes
V4 4_665 Se5 . O39 . 130.95(7) yes
O26 . Se5 . O39 . 100.24(10) yes
V6 . Se6 . V7 . 109.455(14) yes
V6 . Se6 . O27 . 131.09(7) yes
V7 . Se6 . O27 . 107.58(7) yes
V6 . Se6 . O34 . 34.21(7) yes
V7 . Se6 . O34 . 127.71(7) yes
O27 . Se6 . O34 . 97.10(10) yes
V6 . Se6 . O38 . 96.82(7) yes
V7 . Se6 . O38 . 32.41(7) yes
O27 . Se6 . O38 . 97.65(10) yes
O34 . Se6 . O38 . 100.49(10) yes
V7 . Se7 . V6 . 108.324(14) yes
V7 . Se7 . O35 . 95.94(7) yes
V6 . Se7 . O35 . 31.70(7) yes
V7 . Se7 . O41 . 31.71(7) yes
V6 . Se7 . O41 . 125.37(7) yes
O35 . Se7 . O41 . 99.61(10) yes
V7 . Se7 . O45 . 127.89(7) yes
V6 . Se7 . O45 . 112.84(7) yes
O35 . Se7 . O45 . 102.54(10) yes
O41 . Se7 . O45 . 96.73(10) yes
V1 . Se8 . V8 . 107.931(14) yes
V1 . Se8 . O5 . 31.78(7) yes
V8 . Se8 . O5 . 125.78(7) yes
V1 . Se8 . O32 . 128.45(7) yes
V8 . Se8 . O32 . 112.72(7) yes
O5 . Se8 . O32 . 97.08(10) yes
V1 . Se8 . O44 . 94.04(7) yes
V8 . Se8 . O44 . 32.77(7) yes
O5 . Se8 . O44 . 98.58(10) yes
O32 . Se8 . O44 . 103.28(10) yes
O47 3_555 Se9 . V8 3_555 32.58(7) yes
O47 3_555 Se9 . O17 . 101.67(10) yes
V8 3_555 Se9 . O17 . 130.29(7) yes
O47 3_555 Se9 . O49 . 97.40(10) yes
V8 3_555 Se9 . O49 . 103.49(7) yes
O17 . Se9 . O49 . 100.06(10) yes
V4 . Se10 . V1 . 145.228(15) yes
V4 . Se10 . O4 . 128.03(7) yes
V1 . Se10 . O4 . 29.88(7) yes
V4 . Se10 . O24 . 38.09(7) yes
V1 . Se10 . O24 . 128.67(7) yes
O4 . Se10 . O24 . 99.91(10) yes
V4 . Se10 . O50 . 115.26(7) yes
V1 . Se10 . O50 . 97.44(7) yes
O4 . Se10 . O50 . 96.59(10) yes
O24 . Se10 . O50 . 99.44(10) yes
V3 . Se11 . O16 . 34.42(7) yes
V3 . Se11 . O36 . 132.20(7) yes
O16 . Se11 . O36 . 100.55(10) yes
V3 . Se11 . O51 . 101.55(8) yes
O16 . Se11 . O51 . 96.79(11) yes
O36 . Se11 . O51 . 98.41(10) yes
V6 . Se12 . O30 . 130.56(7) yes
V6 . Se12 . O33 . 33.55(7) yes
O30 . Se12 . O33 . 100.61(10) yes
V6 . Se12 . O52 . 107.17(7) yes
O30 . Se12 . O52 . 95.92(10) yes
O33 . Se12 . O52 . 100.17(10) yes
O48 4_565 Se13 . V5 . 128.86(7) yes
O48 4_565 Se13 . O28 . 99.58(10) yes
V5 . Se13 . O28 . 29.89(7) yes
O48 4_565 Se13 . O53 . 96.48(10) yes
V5 . Se13 . O53 . 97.65(8) yes
O28 . Se13 . O53 . 97.29(10) yes
O10 3_445 Se14 . V2 3_445 33.08(7) yes
O10 3_445 Se14 . O6 . 100.33(10) yes
V2 3_445 Se14 . O6 . 131.74(7) yes
O10 3_445 Se14 . O54 . 100.38(11) yes
V2 3_445 Se14 . O54 . 103.37(8) yes
O6 . Se14 . O54 . 95.56(10) yes
V7 . Se15 . O12 1_655 135.08(7) yes
V7 . Se15 . O40 . 35.96(7) yes
O12 1_655 Se15 . O40 . 100.59(10) yes
V7 . Se15 . O55 . 99.76(10) yes
O12 1_655 Se15 . O55 . 97.81(14) yes
O40 . Se15 . O55 . 98.77(15) yes
O22 3_545 Se16 . V4 3_545 32.43(7) yes
O22 3_545 Se16 . O42 . 101.27(10) yes
V4 3_545 Se16 . O42 . 129.88(7) yes
O22 3_545 Se16 . O56 . 97.31(10) yes
V4 3_545 Se16 . O56 . 103.04(8) yes
O42 . Se16 . O56 . 100.50(11) yes
V1 . O2 . Se1 4_564 121.97(11) yes
V1 . O3 . Se2 4_564 122.24(11) yes
V1 . O4 . Se10 . 124.84(11) yes
V1 . O5 . Se8 . 120.68(11) yes
V1 . O6 . Se14 . 119.65(11) yes
V2 . O8 . Se3 . 121.55(11) yes
V2 . O9 . Se4 4_464 122.39(12) yes
V2 . O10 . Se14 3_455 119.52(11) yes
V2 . O11 . Se2 . 119.37(11) yes
V2 . O12 . Se15 1_455 119.52(11) yes
V3 . O14 . Se2 . 121.74(11) yes
V3 . O15 . Se1 . 117.99(11) yes
V3 . O16 . Se11 . 117.17(11) yes
V3 . O17 . Se9 . 117.13(11) yes
V3 . O18 . Se3 . 118.53(11) yes
V4 . O20 . Se4 4_464 120.73(11) yes
V4 . O21 . Se3 . 118.11(11) yes
V4 . O22 . Se16 3_555 120.89(11) yes
V4 . O23 . Se5 4_464 119.27(11) yes
V4 . O24 . Se10 . 114.03(11) yes
V5 . O26 . Se5 . 122.45(11) yes
V5 . O27 . Se6 . 121.89(11) yes
V5 . O28 . Se13 . 124.61(11) yes
V5 . O29 . Se4 . 120.18(11) yes
V5 2_566 O30 . Se12 . 119.38(11) yes
V6 . O32 . Se8 . 120.66(11) yes
V6 . O33 . Se12 . 118.80(11) yes
V6 . O34 . Se6 . 118.07(11) yes
V6 . O35 . Se7 . 121.81(11) yes
V6 . O36 . Se11 . 118.76(11) yes
V7 . O38 . Se6 . 120.84(11) yes
V7 . O39 . Se5 . 117.30(11) yes
V7 . O40 . Se15 . 114.52(11) yes
V7 . O41 . Se7 . 121.40(11) yes
V7 . O42 . Se16 . 117.32(11) yes
V8 . O44 . Se8 . 120.20(11) yes
V8 . O45 . Se7 . 118.70(11) yes
V8 . O46 . Se1 4_564 119.10(11) yes
V8 . O47 . Se9 3_545 120.85(11) yes
V8 . O48 . Se13 4_564 116.82(10) yes
Se9 . O49 . H1 . 108.5 no
Se10 . O50 . H2 . 106.1 no
Se11 . O51 . H3 . 128.5 no
Se12 . O52 . H4 . 125.5 no
Se13 . O53 . H5 . 119.0 no
Se14 . O54 . H6 . 112.5 no
Se15 . O55 . H7 . 108.1 no
Se16 . O56 . H8 . 114.3 no
H9 . O57 . H10 . 109.1 no
H11 . O58 . H12 . 109.6 no
H13 . O59 . H14 . 109.2 no
H15 . O60 . H16 . 109.7 no
H17 . O61 . H18 . 109.6 no
H19 . O62 . H20 . 109.2 no
H21 . O63 . H22 . 110.0 no
H23 . O64 . H24 . 109.5 no
H25 . O65 . H26 . 109.3 no
O67 . O66 . H27 . 63.3 no
O67 . O66 . H28 . 45.6 no
H27 . O66 . H28 . 100.4 no
O66 . O67 . H27 . 34.7 no
O66 . O67 . H28 . 52.9 no
H27 . O67 . H28 . 81.8 no
C1 . N1 . H29 . 109.7 no
C1 . N1 . H30 . 109.6 no
H29 . N1 . H30 . 108.6 no
C1 . N1 . H31 . 110.8 no
H29 . N1 . H31 . 109.1 no
H30 . N1 . H31 . 109.0 no
C2 . N2 . C3 . 110.7(2) yes
C2 . N2 . H36 . 109.0 no
C3 . N2 . H36 . 109.3 no
C2 . N2 . H37 . 109.5 no
C3 . N2 . H37 . 109.4 no
H36 . N2 . H37 . 108.9 no
C4 . N3 . H42 . 109.6 no
C4 . N3 . H43 . 109.4 no
H42 . N3 . H43 . 108.8 no
C4 . N3 . H44 . 109.9 no
H42 . N3 . H44 . 108.9 no
H43 . N3 . H44 . 110.2 no
C5 . N4 . H45 . 110.5 no
C5 . N4 . H46 . 109.9 no
H45 . N4 . H46 . 108.8 no
C5 . N4 . H47 . 109.8 no
H45 . N4 . H47 . 108.9 no
H46 . N4 . H47 . 108.9 no
C6 . N5 . C7 . 112.2(2) yes
C6 . N5 . H52 . 108.4 no
C7 . N5 . H52 . 108.7 no
C6 . N5 . H53 . 109.4 no
C7 . N5 . H53 . 109.2 no
H52 . N5 . H53 . 108.8 no
C8 . N6 . H58 . 109.5 no
C8 . N6 . H59 . 109.6 no
H58 . N6 . H59 . 109.5 no
C8 . N6 . H60 . 109.5 no
H58 . N6 . H60 . 109.7 no
H59 . N6 . H60 . 109.0 no
N1 . C1 . C2 . 107.3(2) yes
N1 . C1 . H32 . 109.4 no
C2 . C1 . H32 . 114.9 no
N1 . C1 . H33 . 106.8 no
C2 . C1 . H33 . 108.4 no
H32 . C1 . H33 . 109.7 no
C1 . C2 . N2 . 111.8(2) yes
C1 . C2 . H34 . 108.3 no
N2 . C2 . H34 . 106.8 no
C1 . C2 . H35 . 110.4 no
N2 . C2 . H35 . 108.8 no
H34 . C2 . H35 . 110.7 no
N2 . C3 . C4 . 108.6(2) yes
N2 . C3 . H38 . 109.1 no
C4 . C3 . H38 . 108.1 no
N2 . C3 . H39 . 108.5 no
C4 . C3 . H39 . 109.4 no
H38 . C3 . H39 . 113.1 no
C3 . C4 . N3 . 110.5(2) yes
C3 . C4 . H40 . 110.6 no
N3 . C4 . H40 . 106.8 no
C3 . C4 . H41 . 111.8 no
N3 . C4 . H41 . 110.0 no
H40 . C4 . H41 . 106.9 no
N4 . C5 . C6 . 108.8(3) yes
N4 . C5 . H48 . 108.5 no
C6 . C5 . H48 . 110.6 no
N4 . C5 . H49 . 109.0 no
C6 . C5 . H49 . 106.8 no
H48 . C5 . H49 . 113.1 no
C5 . C6 . N5 . 111.4(2) yes
C5 . C6 . H50 . 110.6 no
N5 . C6 . H50 . 107.0 no
C5 . C6 . H51 . 111.7 no
N5 . C6 . H51 . 106.9 no
H50 . C6 . H51 . 109.0 no
N5 . C7 . C8 . 111.0(2) yes
N5 . C7 . H54 . 109.7 no
C8 . C7 . H54 . 111.5 no
N5 . C7 . H55 . 106.3 no
C8 . C7 . H55 . 112.8 no
H54 . C7 . H55 . 105.2 no
C7 . C8 . N6 . 108.3(2) yes
C7 . C8 . H56 . 112.3 no
N6 . C8 . H56 . 107.0 no
C7 . C8 . H57 . 109.6 no
N6 . C8 . H57 . 109.4 no
H56 . C8 . H57 . 110.2 no
O67 . H27 . O66 . 82.0 no
O66 . H28 . O67 . 81.5 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O49 . H1 . O58 2_576 167.13(17) 0.831 1.827 2.643(5) yes
O50 . H2 . O62 . 162.08(15) 0.988 1.668 2.626(5) yes
O51 . H3 . O57 . 121.0(3) 0.890 2.033 2.606(5) yes
O51 . H3 . O66 3_555 160.5(2) 0.890 1.686 2.543(5) yes
O52 . H4 . O65 . 155.97(18) 0.837 1.806 2.593(5) yes
O53 . H5 . O63 2_566 167.07(18) 0.843 1.731 2.559(5) yes
O54 . H6 . O60 3_545 159.00(18) 0.803 1.860 2.625(5) yes
O55 . H7 . O67 . 123.3(4) 0.962 1.766 2.431(5) yes
O56 . H8 . O64 . 165.56(18) 0.827 1.845 2.654(5) yes
O57 . H9 . O22 . 178.4(4) 0.951 1.841 2.792(5) yes
O57 . H10 . O5 . 177.8(4) 0.952 2.109 3.061(5) yes
O58 . H11 . O16 . 171.90(15) 0.948 2.000 2.942(5) yes
O58 . H12 . O46 3_555 168.84(15) 0.950 1.963 2.901(5) yes
O59 . H13 . O6 3_555 167.10(15) 0.954 1.821 2.759(5) yes
O59 . H14 . O37 . 137.53(15) 0.949 2.026 2.801(5) yes
O60 . H16 . O40 . 131.72(16) 0.950 2.273 2.991(5) yes
O60 . H16 . O64 2_666 151.36(15) 0.950 2.434 3.299(5) yes
O61 . H17 . O13 . 151.06(15) 0.949 1.971 2.839(5) yes
O61 . H18 . O30 . 167.16(15) 0.950 1.965 2.898(5) yes
O62 . H19 . O18 . 178.91(15) 0.957 2.011 2.968(5) yes
O62 . H20 . O33 . 174.18(16) 0.946 1.841 2.783(5) yes
O63 . H21 . O9 3_445 135.74(17) 0.947 2.592 3.336(5) yes
O64 . H23 . O23 4_665 157.72(16) 0.949 2.013 2.914(5) yes
O64 . H24 . O40 2_666 161.86(15) 0.950 1.987 2.905(5) yes
O65 . H25 . O27 . 130.7(2) 0.953 2.547 3.249(5) yes
O65 . H25 . O28 . 157.8(2) 0.953 1.870 2.775(5) yes
O65 . H26 . O16 . 126.30(19) 0.949 2.221 2.886(5) yes
O67 . H27 . O22 3_545 126.2(4) 1.050 2.261 3.003(5) yes
O67 . H27 . O57 3_545 158.0(4) 1.050 2.289 3.286(5) yes
N1 . H29 . O14 . 151.03(17) 0.955 1.939 2.812(5) yes
N1 . H29 . O17 . 132.50(17) 0.955 2.578 3.299(5) yes
N1 . H30 . O25 2_576 130.22(16) 0.956 2.442 3.145(5) yes
N1 . H30 . O49 . 138.70(17) 0.956 2.158 2.944(5) yes
N1 . H31 . O59 2_576 144.23(17) 0.950 2.085 2.910(5) yes
C2 . H34 . O25 2_576 130.40(18) 0.991 2.542 3.273(5) yes
N2 . H36 . O7 . 136.11(16) 0.955 2.028 2.795(5) yes
N2 . H36 . O50 3_455 124.88(16) 0.955 2.435 3.082(5) yes
N2 . H37 . O20 3_455 137.43(16) 0.952 2.149 2.922(5) yes
N2 . H37 . O24 3_455 145.10(16) 0.952 2.153 2.984(5) yes
C3 . H38 . O19 . 132.56(18) 0.993 2.379 3.137(5) yes
C3 . H39 . O9 3_455 163.89(18) 1.008 2.465 3.444(5) yes
C4 . H40 . O7 . 129.06(18) 0.998 2.394 3.121(5) yes
C4 . H41 . O21 3_455 170.91(18) 0.990 2.439 3.420(5) yes
N3 . H42 . O61 3_455 162.34(16) 0.961 1.908 2.839(5) yes
N3 . H43 . O12 3_455 166.89(17) 0.946 1.869 2.799(5) yes
N3 . H44 . O19 . 144.64(17) 0.945 1.986 2.810(5) yes
N4 . H45 . O52 2_566 134.62(19) 0.954 2.439 3.182(5) yes
N4 . H45 . O61 2_566 138.20(19) 0.954 2.233 3.012(5) yes
N4 . H46 . O38 . 148.00(19) 0.954 1.946 2.801(5) yes
N4 . H46 . O42 . 136.25(18) 0.954 2.506 3.263(5) yes
N4 . H47 . O1 3_545 139.62(18) 0.953 2.290 3.079(5) yes
N4 . H47 . O56 . 134.59(18) 0.953 2.318 3.063(5) yes
N5 . H52 . O31 . 137.33(16) 0.959 1.985 2.767(5) yes
N5 . H53 . O44 3_545 128.66(16) 0.949 2.248 2.936(5) yes
N5 . H53 . O48 3_545 152.73(16) 0.949 2.001 2.878(5) yes
C7 . H54 . O32 3_545 171.54(18) 1.014 2.480 3.485(5) yes
C7 . H55 . O43 . 128.51(18) 1.011 2.397 3.128(5) yes
C8 . H56 . O31 . 125.44(18) 0.993 2.460 3.142(5) yes
C8 . H57 . O45 3_545 163.79(19) 0.980 2.451 3.404(5) yes
N6 . H58 . O35 3_545 126.78(16) 0.946 2.261 2.927(5) yes
N6 . H58 . O36 3_545 157.05(16) 0.946 1.983 2.877(5) yes
N6 . H59 . O59 3_545 165.42(16) 0.954 1.840 2.774(5) yes
N6 . H60 . O43 . 144.32(16) 0.952 2.049 2.876(5) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 02/01/12 at 13:38:55
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 02/01/12 at 13:38:55
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# 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_[C4H14N2]2[VO(SeO3)(HSeO3)]6-5H2O-compound-1
_database_code_depnum_ccdc_archive 'CCDC 1588071'
_audit_update_record             
;
2017-11-28 deposited with the CCDC.
2018-02-01 downloaded from the CCDC.
;

_cell_length_a                   24.713(2)
_cell_length_b                   7.9212(8)
_cell_length_c                   34.399(2)
_cell_angle_alpha                90
_cell_angle_beta                 130.376(4)
_cell_angle_gamma                90
_cell_volume                     5129.8(9)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
V 0.3005 0.5294 10.2971 6.8657 7.3511 0.4385 2.0703 26.8938 2.0571 102.4780
1.2199 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Se -0.0929 2.2259 17.0006 2.4098 5.8196 0.2726 3.9731 15.2372 4.3543 43.8163
2.8409 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C12 H26 N4 O56 Se16 V8 
# Dc =      3.62 Fooo =   4164.00 Mu =    128.98 M =   2793.22
# Found Formula = C8 H43 N4 O47 Se12 V6 
# Dc =      2.85 FOOO =   4164.00 Mu =     96.88 M =   2200.60

_chemical_formula_sum            'C8 H43 N4 O47 Se12 V6'
_chemical_formula_moiety         'C8 H43 N4 O47 Se12 V6'
_chemical_compound_source        ?
_chemical_formula_weight         2200.60


_cell_measurement_reflns_used    9970
_cell_measurement_theta_min      2
_cell_measurement_theta_max      32
_cell_measurement_temperature    298

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_min          0.330
_exptl_crystal_size_mid          0.440
_exptl_crystal_size_max          0.560

_exptl_crystal_density_diffrn    2.849
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             4164
_exptl_absorpt_coefficient_mu    9.688

# Sheldrick geometric approximatio 0.01 0.04 
# No experimental values of Tmin/max available 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.01
_exptl_absorpt_correction_T_max  0.04
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      298
_diffrn_reflns_number            81139
_reflns_number_total             16302
_diffrn_reflns_av_R_equivalents  0.042
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 16302 
# Theoretical number of reflections is about 35138 


_diffrn_reflns_theta_min         1.554
_diffrn_reflns_theta_max         31.909
_diffrn_measured_fraction_theta_max 0.922

_diffrn_reflns_theta_full        25.208
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_limit_l_max       50
_reflns_limit_h_min              -36
_reflns_limit_h_max              26
_reflns_limit_k_min              0
_reflns_limit_k_max              11
_reflns_limit_l_min              0
_reflns_limit_l_max              50

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.43
_refine_diff_density_max         1.48


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         11063
_refine_ls_number_restraints     0
_refine_ls_number_parameters     740
_oxford_refine_ls_R_factor_ref   0.0337
_refine_ls_wR_factor_ref         0.0867
_refine_ls_goodness_of_fit_ref   1.0613
_refine_ls_shift/su_max          0.0035865
_refine_ls_shift/su_mean         0.0001588


# The values computed from all data 
_oxford_reflns_number_all        16261
_refine_ls_R_factor_all          0.0563
_refine_ls_wR_factor_all         0.0970

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                12005
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_gt          0.0903

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.03P)² +23.32P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
V1 V 0.51529(4) -0.30534(8) 0.82689(2) 0.0073 1.0000 Uani . . . . . .
V2 V 0.65037(4) -0.28984(8) 1.00134(2) 0.0084 1.0000 Uani . . . . . .
V3 V 0.85206(4) -0.21284(8) 0.99303(2) 0.0075 1.0000 Uani . . . . . .
V4 V 0.98159(4) -0.20992(8) 1.17165(2) 0.0067 1.0000 Uani . . . . . .
V5 V 0.68169(4) -0.78734(8) 1.15814(2) 0.0076 1.0000 Uani . . . . . .
V6 V 0.81513(4) 0.27141(8) 0.83376(2) 0.0080 1.0000 Uani . . . . . .
Se1 Se 0.34951(2) -0.24071(5) 0.763622(14) 0.0078 1.0000 Uani . . . . . .
Se2 Se 0.48439(2) -0.28197(5) 0.905027(14) 0.0082 1.0000 Uani . . . . . .
Se3 Se 0.68298(2) -0.28070(5) 0.925350(14) 0.0084 1.0000 Uani . . . . . .
Se4 Se 0.81778(2) -0.23355(5) 1.069096(14) 0.0077 1.0000 Uani . . . . . .
Se5 Se 1.01577(2) -0.22381(4) 1.095700(14) 0.0077 1.0000 Uani . . . . . .
Se6 Se 0.84855(2) 0.26934(4) 0.758104(14) 0.0080 1.0000 Uani . . . . . .
Se7 Se 0.46679(2) -0.47412(5) 0.723792(15) 0.0113 1.0000 Uani . . . . . .
Se8 Se 0.80364(2) -0.07283(5) 0.886052(15) 0.0134 1.0000 Uani . . . . . .
Se9 Se 0.86595(2) -0.54447(5) 0.937214(16) 0.0150 1.0000 Uani . . . . . .
Se10 Se 1.02842(2) -0.05560(5) 1.275953(15) 0.0107 1.0000 Uani . . . . . .
Se11 Se 0.70293(2) -0.46017(5) 1.107424(15) 0.0114 1.0000 Uani . . . . . .
Se12 Se 0.6386(4) 0.0176(10) 1.0607(3) 0.0135 0.5000 Uani . . . . . .
Se13 Se 0.6314(5) 0.0394(11) 1.0543(3) 0.0166 0.5000 Uani . . . . . .
O1 O 0.53850(17) -0.4781(4) 0.85850(11) 0.0171 1.0000 Uani . . . . . .
O2 O 0.41181(15) -0.3580(4) 0.77026(11) 0.0124 1.0000 Uani . . . . . .
O3 O 0.48906(16) -0.1792(3) 0.86415(10) 0.0110 1.0000 Uani . . . . . .
O4 O 0.61213(16) -0.1946(4) 0.87040(11) 0.0133 1.0000 Uani . . . . . .
O5 O 0.53136(16) -0.3712(4) 0.77855(11) 0.0146 1.0000 Uani . . . . . .
O6 O 0.48660(16) -0.0530(3) 0.79155(11) 0.0133 1.0000 Uani . . . . . .
O7 O 0.62670(17) -0.4630(4) 0.97050(11) 0.0175 1.0000 Uani . . . . . .
O8 O 0.55766(15) -0.1965(4) 0.96237(10) 0.0128 1.0000 Uani . . . . . .
O9 O 0.67812(16) -0.1790(3) 0.96875(11) 0.0120 1.0000 Uani . . . . . .
O10 O 0.74979(16) -0.3466(4) 1.05771(11) 0.0125 1.0000 Uani . . . . . .
O11 O 0.63797(16) -0.3678(4) 1.05070(11) 0.0150 1.0000 Uani . . . . . .
O12 O 0.67858(18) -0.0436(4) 1.03977(12) 0.0178 1.0000 Uani . . . . . .
O13 O 0.87045(17) -0.0370(4) 1.02243(11) 0.0167 1.0000 Uani . . . . . .
O14 O 0.74731(16) -0.1618(4) 0.93504(11) 0.0133 1.0000 Uani . . . . . .
O15 O 0.82521(16) -0.3391(3) 1.02944(10) 0.0115 1.0000 Uani . . . . . .
O16 O 0.95077(16) -0.3122(4) 1.03842(10) 0.0136 1.0000 Uani . . . . . .
O17 O 0.86952(16) -0.1473(4) 0.94551(11) 0.0156 1.0000 Uani . . . . . .
O18 O 0.82273(17) -0.4671(4) 0.95517(11) 0.0161 1.0000 Uani . . . . . .
O19 O 0.96181(17) -0.0342(4) 1.14201(11) 0.0168 1.0000 Uani . . . . . .
O20 O 0.88404(16) -0.3159(4) 1.12672(11) 0.0136 1.0000 Uani . . . . . .
O21 O 1.01011(16) -0.3315(3) 1.13588(11) 0.0115 1.0000 Uani . . . . . .
O22 O 1.08567(15) -0.1531(4) 1.23060(11) 0.0117 1.0000 Uani . . . . . .
O23 O 0.96232(16) -0.1496(4) 1.21932(11) 0.0130 1.0000 Uani . . . . . .
O24 O 1.01635(16) -0.4621(3) 1.20926(11) 0.0134 1.0000 Uani . . . . . .
O25 O 0.70272(18) -0.9611(4) 1.18907(12) 0.0183 1.0000 Uani . . . . . .
O26 O 0.77961(16) -0.6794(4) 1.20322(10) 0.0130 1.0000 Uani . . . . . .
O27 O 0.34405(16) -0.3412(3) 0.80461(11) 0.0117 1.0000 Uani . . . . . .
O28 O 0.69765(17) 0.1426(4) 1.10988(11) 0.0159 1.0000 Uani . . . . . .
O29 O 0.42244(15) -0.1671(4) 0.89947(10) 0.0122 1.0000 Uani . . . . . .
O30 O 0.65470(16) -0.5369(4) 1.12158(11) 0.0139 1.0000 Uani . . . . . .
O31 O 0.79131(17) 0.4447(4) 0.80333(11) 0.0160 1.0000 Uani . . . . . .
O32 O 0.84327(16) 0.1652(3) 0.80105(10) 0.0112 1.0000 Uani . . . . . .
O33 O 1.08608(16) -0.3319(4) 1.10862(11) 0.0128 1.0000 Uani . . . . . .
O34 O 0.80075(17) -0.6541(4) 0.88335(11) 0.0156 1.0000 Uani . . . . . .
O35 O 0.27629(15) -0.3264(4) 0.70535(10) 0.0116 1.0000 Uani . . . . . .
O36 O 0.84892(17) 0.0278(4) 0.87331(11) 0.0160 1.0000 Uani . . . . . .
O37 O 0.4321(2) -0.2925(4) 0.68517(13) 0.0278 1.0000 Uani . . . . . .
O38 O 0.7857(2) -0.2604(5) 0.85259(14) 0.0358 1.0000 Uani . . . . . .
O39 O 0.9146(11) -0.703(3) 0.9806(10) 0.0509 0.5000 Uani . . . . . .
O40 O 0.8921(11) -0.729(3) 0.9774(10) 0.0342 0.5000 Uani . . . . . .
O41 O 1.0560(2) -0.2338(5) 1.31482(14) 0.0309 1.0000 Uani . . . . . .
O42 O 0.7348(2) -0.2730(4) 1.14398(13) 0.0254 1.0000 Uani . . . . . .
O43 O 0.5792(11) 0.172(2) 1.0142(8) 0.0470 0.5000 Uani . . . . . .
O44 O 0.5994(11) 0.216(2) 1.0134(8) 0.0496 0.5000 Uani . . . . . .
O45 O 1.1595(2) -0.4156(6) 1.3376(2) 0.0739 1.0000 Uani . . . . . .
O46 O 0.5064(6) 0.4397(13) 0.9968(7) 0.1013 0.5000 Uani . . . . . .
O47 O 0.3275(3) 0.4336(7) 0.1783(2) 0.0780 1.0000 Uani . . . . . .
O48 O 0.2932(2) 0.8148(5) 0.10247(16) 0.0369 1.0000 Uani . . . . . .
O49 O 0.86747(19) 0.6954(4) 0.23065(14) 0.0309 1.0000 Uani . . . . . .
O50 O 0.9946(10) 0.061(2) 1.0121(7) 0.0274 0.2500 Uani . . . . . .
O51 O 0.9855(9) 0.060(3) 0.9886(8) 0.0399 0.2500 Uani . . . . . .
N1 N 1.1775(2) -0.2953(5) 0.97933(14) 0.0223 1.0000 Uani . . . . . .
N2 N 0.9872(2) -0.3020(5) 0.85897(14) 0.0199 1.0000 Uani . . . . . .
N3 N 0.6730(2) -0.2000(5) 0.69292(16) 0.0235 1.0000 Uani . . . . . .
N4 N 0.4880(2) -0.3201(5) 0.63376(17) 0.0267 1.0000 Uani . . . . . .
C1 C 1.1162(3) -0.2954(5) 0.92366(16) 0.0201 1.0000 Uani . . . . . .
C2 C 1.0478(2) -0.2966(5) 0.91436(16) 0.0199 1.0000 Uani . . . . . .
C3 C 1.2461(3) -0.2753(7) 0.9908(2) 0.0371 1.0000 Uani . . . . . .
C4 C 0.9173(3) -0.2801(7) 0.8462(2) 0.0328 1.0000 Uani . . . . . .
C5 C 0.6119(3) -0.2430(6) 0.6898(2) 0.0300 1.0000 Uani . . . . . .
C6 C 0.5478(3) -0.2771(6) 0.6357(2) 0.0265 1.0000 Uani . . . . . .
C7 C 0.7405(3) -0.1765(6) 0.7458(2) 0.0320 1.0000 Uani . . . . . .
C8 C 0.4207(3) -0.3446(6) 0.5818(2) 0.0337 1.0000 Uani . . . . . .
H1 H 0.3895 -0.3071 0.6614 0.0412 1.0000 Uiso . . . . . .
H2 H 0.7355 -0.2809 0.8294 0.0437 1.0000 Uiso . . . . . .
H3 H 0.9309 -0.7828 0.9744 0.0820 1.0000 Uiso . . . . . .
H4 H 1.0913 -0.2767 1.3213 0.0440 1.0000 Uiso . . . . . .
H5 H 0.7772 -0.2781 1.1689 0.0361 1.0000 Uiso . . . . . .
H6 H 0.5608 0.2917 1.0023 0.0500 1.0000 Uiso . . . . . .
H7 H 1.2103 -0.4028 1.3604 0.0882 1.0000 Uiso . . . . . .
H8 H 1.1473 -0.5238 1.3228 0.0882 1.0000 Uiso . . . . . .
H9 H 0.5130 0.5512 1.0100 0.1092 0.5000 Uiso . . . . . .
H10 H 0.4565 0.4129 0.9759 0.1092 0.5000 Uiso . . . . . .
H11 H 0.3128 0.4343 0.1455 0.0949 1.0000 Uiso . . . . . .
H12 H 0.3764 0.4085 0.2032 0.0949 1.0000 Uiso . . . . . .
H13 H 0.2613 0.7594 0.1047 0.0446 1.0000 Uiso . . . . . .
H14 H 0.2813 0.9311 0.0953 0.0446 1.0000 Uiso . . . . . .
H15 H 0.8739 0.5768 0.2359 0.0372 1.0000 Uiso . . . . . .
H16 H 0.8934 0.7356 0.2208 0.0372 1.0000 Uiso . . . . . .
H17 H 1.1819 -0.3994 0.9927 0.0600 1.0000 Uiso . . . . . .
H18 H 1.1753 -0.2047 0.9929 0.0600 1.0000 Uiso . . . . . .
H19 H 1.1158 -0.4017 0.9077 0.0600 1.0000 Uiso . . . . . .
H20 H 1.1155 -0.2059 0.9059 0.0600 1.0000 Uiso . . . . . .
H21 H 1.0429 -0.3925 0.9306 0.0600 1.0000 Uiso . . . . . .
H22 H 1.0421 -0.1969 0.9281 0.0600 1.0000 Uiso . . . . . .
H23 H 0.9870 -0.4116 0.8451 0.0600 1.0000 Uiso . . . . . .
H24 H 0.9923 -0.2177 0.8419 0.0600 1.0000 Uiso . . . . . .
H25 H 1.2827 -0.2774 1.0261 0.0600 1.0000 Uiso . . . . . .
H26 H 1.2535 -0.3699 0.9762 0.0600 1.0000 Uiso . . . . . .
H27 H 1.2469 -0.1752 0.9764 0.0600 1.0000 Uiso . . . . . .
H28 H 0.9126 -0.3715 0.8621 0.0600 1.0000 Uiso . . . . . .
H29 H 0.9179 -0.1776 0.8589 0.0600 1.0000 Uiso . . . . . .
H30 H 0.8806 -0.2881 0.8104 0.0600 1.0000 Uiso . . . . . .
H31 H 0.6795 -0.2892 0.6778 0.0284 1.0000 Uiso . . . . . .
H32 H 0.6623 -0.0987 0.6743 0.0284 1.0000 Uiso . . . . . .
H33 H 0.6017 -0.1476 0.7028 0.0329 1.0000 Uiso . . . . . .
H34 H 0.6222 -0.3449 0.7099 0.0332 1.0000 Uiso . . . . . .
H35 H 0.5580 -0.3730 0.6227 0.0299 1.0000 Uiso . . . . . .
H36 H 0.5372 -0.1766 0.6155 0.0303 1.0000 Uiso . . . . . .
H37 H 0.4817 -0.2310 0.6491 0.0318 1.0000 Uiso . . . . . .
H38 H 0.4991 -0.4214 0.6524 0.0318 1.0000 Uiso . . . . . .
H39 H 0.7340 -0.0903 0.7623 0.0461 1.0000 Uiso . . . . . .
H40 H 0.7767 -0.1413 0.7448 0.0461 1.0000 Uiso . . . . . .
H41 H 0.7537 -0.2822 0.7640 0.0460 1.0000 Uiso . . . . . .
H42 H 0.4086 -0.2418 0.5626 0.0500 1.0000 Uiso . . . . . .
H43 H 0.3837 -0.3734 0.5826 0.0501 1.0000 Uiso . . . . . .
H44 H 0.4259 -0.4353 0.5657 0.0501 1.0000 Uiso . . . . . .

_refine_ls_extinction_coef       26(3)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.079690(15)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 . Se2 . 3.2404(7) yes
V1 . Se7 . 3.2086(7) yes
V1 . O1 . 1.605(3) yes
V1 . O2 . 2.013(3) yes
V1 . O3 . 2.034(3) yes
V1 . O4 . 2.024(3) yes
V1 . O5 . 2.013(3) yes
V1 . O6 . 2.205(3) yes
V2 . Se3 . 3.1963(7) yes
V2 . Se11 . 3.2686(8) yes
V2 . O7 . 1.595(3) yes
V2 . O8 . 1.901(3) yes
V2 . O9 . 1.869(3) yes
V2 . O10 . 1.956(3) yes
V2 . O11 . 2.008(3) yes
V2 . O12 . 2.201(3) yes
V3 . Se4 . 3.2346(7) yes
V3 . Se8 . 3.2401(7) yes
V3 . O13 . 1.605(3) yes
V3 . O14 . 2.038(3) yes
V3 . O15 . 2.021(3) yes
V3 . O16 . 2.018(3) yes
V3 . O17 . 2.010(3) yes
V3 . O18 . 2.248(3) yes
V4 . Se5 . 3.2264(7) yes
V4 . Se10 . 3.2135(7) yes
V4 . O19 . 1.603(3) yes
V4 . O20 . 2.019(3) yes
V4 . O21 . 2.015(3) yes
V4 . O22 . 2.043(3) yes
V4 . O23 . 2.039(3) yes
V4 . O24 . 2.227(3) yes
V5 . O27 2_647 2.034(3) yes
V5 . O29 2_647 2.018(3) yes
V5 . O28 1_545 2.017(3) yes
V5 . Se12 1_545 3.182(10) yes
V5 . Se13 1_545 3.232(10) yes
V5 . Se1 2_647 3.2520(7) yes
V5 . O25 . 1.607(3) yes
V5 . O26 . 2.032(3) yes
V5 . O30 . 2.208(3) yes
V6 . O34 1_565 2.042(3) yes
V6 . O33 2_757 1.962(3) yes
V6 . O35 3_656 1.891(3) yes
V6 . Se9 1_565 3.2525(8) yes
V6 . Se6 . 3.1997(7) yes
V6 . O31 . 1.590(3) yes
V6 . O32 . 1.863(3) yes
V6 . O36 . 2.191(3) yes
Se1 . O2 . 1.682(3) yes
Se1 . O27 . 1.699(3) yes
Se1 . O35 . 1.748(3) yes
Se2 . O3 . 1.692(3) yes
Se2 . O8 . 1.732(3) yes
Se2 . O29 . 1.682(3) yes
Se3 . O4 . 1.678(3) yes
Se3 . O9 . 1.767(3) yes
Se3 . O14 . 1.685(3) yes
Se4 . O10 . 1.711(3) yes
Se4 . O15 . 1.708(3) yes
Se4 . O20 . 1.682(3) yes
Se5 . O16 . 1.689(3) yes
Se5 . O21 . 1.705(3) yes
Se5 . O33 . 1.717(3) yes
Se6 . O22 2_757 1.680(3) yes
Se6 . O26 4_544 1.675(3) yes
Se6 . O32 . 1.769(3) yes
Se7 . O6 3_646 1.668(3) yes
Se7 . O5 . 1.692(3) yes
Se7 . O37 . 1.759(3) yes
Se8 . O17 . 1.693(3) yes
Se8 . O36 . 1.648(3) yes
Se8 . O38 . 1.752(4) yes
Se9 . O18 . 1.659(3) yes
Se9 . O34 . 1.707(3) yes
Se9 . O39 . 1.71(2) yes
Se9 . O40 . 1.82(2) yes
Se10 . O24 3_757 1.662(3) yes
Se10 . O23 . 1.701(3) yes
Se10 . O41 . 1.750(3) yes
Se11 . O11 . 1.692(3) yes
Se11 . O30 . 1.667(3) yes
Se11 . O42 . 1.766(3) yes
Se12 . O12 . 1.629(11) yes
Se12 . O28 . 1.665(9) yes
Se12 . O43 . 1.78(2) yes
Se12 . O44 . 2.002(18) yes
Se13 . O12 . 1.671(11) yes
Se13 . O28 . 1.718(10) yes
Se13 . O43 . 1.54(2) yes
Se13 . O44 . 1.763(19) yes
O37 . H1 . 0.822 no
O38 . H2 . 0.960 no
O39 . H3 . 0.849 no
O40 . H3 . 1.112 no
O41 . H4 . 0.822 no
O42 . H5 . 0.820 no
O43 . H6 . 1.015 no
O44 . H6 . 0.974 no
O45 . H7 . 0.964 no
O45 . H8 . 0.941 no
O46 . O46 2_667 1.07(2) yes
O46 . H9 . 0.957 no
O46 . H10 . 0.967 no
O47 . H11 . 0.935 no
O47 . H12 . 0.944 no
O48 . H13 . 0.947 no
O48 . H14 . 0.949 no
O49 . H15 . 0.950 no
O49 . H16 . 0.951 no
O50 . O50 2_757 1.41(3) yes
O50 . O51 2_757 1.08(2) yes
O51 . O51 2_757 1.14(4) yes
N1 . C1 . 1.484(6) yes
N1 . C3 . 1.480(7) yes
N1 . H17 . 0.915 no
N1 . H18 . 0.875 no
N2 . C2 . 1.476(6) yes
N2 . C4 . 1.492(6) yes
N2 . H23 . 0.989 no
N2 . H24 . 0.951 no
N3 . C5 . 1.484(6) yes
N3 . C7 . 1.482(7) yes
N3 . H31 . 0.950 no
N3 . H32 . 0.951 no
N4 . C6 . 1.475(6) yes
N4 . C8 . 1.465(7) yes
N4 . H37 . 0.952 no
N4 . H38 . 0.950 no
C1 . C2 . 1.505(6) yes
C1 . H19 . 1.001 no
C1 . H20 . 0.927 no
C2 . H21 . 0.995 no
C2 . H22 . 0.976 no
C3 . H25 . 0.934 no
C3 . H26 . 0.984 no
C3 . H27 . 0.942 no
C4 . H28 . 0.959 no
C4 . H29 . 0.917 no
C4 . H30 . 0.947 no
C5 . C6 . 1.492(8) yes
C5 . H33 . 0.989 no
C5 . H34 . 0.983 no
C6 . H35 . 0.994 no
C6 . H36 . 0.976 no
C7 . H39 . 0.964 no
C7 . H40 . 0.958 no
C7 . H41 . 0.966 no
C8 . H42 . 0.966 no
C8 . H43 . 0.960 no
C8 . H44 . 0.966 no
H9 . H10 2_667 0.641 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Se2 . V1 . Se7 . 145.15(2) yes
Se2 . V1 . O1 . 70.11(11) yes
Se7 . V1 . O1 . 96.15(11) yes
Se2 . V1 . O2 . 88.87(8) yes
Se7 . V1 . O2 . 60.88(8) yes
O1 . V1 . O2 . 98.71(14) yes
Se2 . V1 . O3 . 26.71(8) yes
Se7 . V1 . O3 . 149.08(9) yes
O1 . V1 . O3 . 96.42(13) yes
O2 . V1 . O3 . 89.31(11) yes
Se2 . V1 . O4 . 99.39(8) yes
Se7 . V1 . O4 . 114.45(8) yes
O1 . V1 . O4 . 97.82(14) yes
O2 . V1 . O4 . 163.23(12) yes
O3 . V1 . O4 . 91.61(12) yes
Se2 . V1 . O5 . 168.17(9) yes
Se7 . V1 . O5 . 27.26(9) yes
O1 . V1 . O5 . 99.40(14) yes
O2 . V1 . O5 . 87.34(12) yes
O3 . V1 . O5 . 164.15(12) yes
Se2 . V1 . O6 . 103.96(7) yes
Se7 . V1 . O6 . 90.68(7) yes
O1 . V1 . O6 . 173.16(13) yes
O2 . V1 . O6 . 84.32(12) yes
O3 . V1 . O6 . 77.42(10) yes
O4 . V1 . O5 . 87.22(12) yes
O4 . V1 . O6 . 79.55(12) yes
O5 . V1 . O6 . 86.82(11) yes
Se3 . V2 . Se11 . 142.56(3) yes
Se3 . V2 . O7 . 69.75(11) yes
Se11 . V2 . O7 . 95.54(11) yes
Se3 . V2 . O8 . 103.99(9) yes
Se11 . V2 . O8 . 111.94(9) yes
O7 . V2 . O8 . 96.33(15) yes
Se3 . V2 . O9 . 27.63(8) yes
Se11 . V2 . O9 . 145.96(10) yes
O7 . V2 . O9 . 97.13(14) yes
O8 . V2 . O9 . 97.89(13) yes
Se3 . V2 . O10 . 89.76(8) yes
Se11 . V2 . O10 . 57.50(8) yes
O7 . V2 . O10 . 98.36(15) yes
O8 . V2 . O10 . 162.66(12) yes
O9 . V2 . O10 . 89.39(12) yes
Se3 . V2 . O11 . 162.91(9) yes
Se11 . V2 . O11 . 25.44(9) yes
O7 . V2 . O11 . 96.11(14) yes
O8 . V2 . O11 . 86.65(12) yes
O9 . V2 . O11 . 165.43(13) yes
Se3 . V2 . O12 . 108.76(8) yes
Se11 . V2 . O12 . 87.30(8) yes
O7 . V2 . O12 . 176.79(14) yes
O8 . V2 . O12 . 81.20(12) yes
O9 . V2 . O12 . 81.23(11) yes
O10 . V2 . O11 . 82.69(12) yes
O10 . V2 . O12 . 84.41(12) yes
O11 . V2 . O12 . 85.83(11) yes
Se4 . V3 . Se8 . 146.98(3) yes
Se4 . V3 . O13 . 69.51(11) yes
Se8 . V3 . O13 . 99.44(11) yes
Se4 . V3 . O14 . 88.26(8) yes
Se8 . V3 . O14 . 61.32(8) yes
O13 . V3 . O14 . 96.10(15) yes
Se4 . V3 . O15 . 27.19(8) yes
Se8 . V3 . O15 . 147.69(9) yes
O13 . V3 . O15 . 96.41(13) yes
O14 . V3 . O15 . 89.19(11) yes
Se4 . V3 . O16 . 99.96(8) yes
Se8 . V3 . O16 . 112.59(8) yes
O13 . V3 . O16 . 98.27(14) yes
O14 . V3 . O16 . 165.22(12) yes
O15 . V3 . O16 . 92.59(12) yes
Se4 . V3 . O17 . 167.80(9) yes
Se8 . V3 . O17 . 26.37(9) yes
O13 . V3 . O17 . 99.54(14) yes
O14 . V3 . O17 . 87.63(12) yes
O15 . V3 . O17 . 163.98(12) yes
Se4 . V3 . O18 . 105.55(7) yes
Se8 . V3 . O18 . 84.58(8) yes
O13 . V3 . O18 . 175.04(13) yes
O14 . V3 . O18 . 83.24(12) yes
O15 . V3 . O18 . 78.68(10) yes
O16 . V3 . O17 . 86.64(12) yes
O16 . V3 . O18 . 82.73(12) yes
O17 . V3 . O18 . 85.35(11) yes
Se5 . V4 . Se10 . 145.41(3) yes
Se5 . V4 . O19 . 69.30(10) yes
Se10 . V4 . O19 . 96.93(11) yes
Se5 . V4 . O20 . 100.08(8) yes
Se10 . V4 . O20 . 113.61(8) yes
O19 . V4 . O20 . 98.81(15) yes
Se5 . V4 . O21 . 27.23(7) yes
Se10 . V4 . O21 . 147.99(9) yes
O19 . V4 . O21 . 96.30(13) yes
O20 . V4 . O21 . 92.89(12) yes
Se5 . V4 . O22 . 89.41(8) yes
Se10 . V4 . O22 . 59.78(7) yes
O19 . V4 . O22 . 96.27(14) yes
O20 . V4 . O22 . 164.27(12) yes
O21 . V4 . O22 . 89.88(12) yes
Se5 . V4 . O23 . 168.36(8) yes
Se10 . V4 . O23 . 27.82(8) yes
O19 . V4 . O23 . 100.03(13) yes
O20 . V4 . O23 . 85.86(12) yes
O21 . V4 . O23 . 163.62(11) yes
Se5 . V4 . O24 . 103.59(7) yes
Se10 . V4 . O24 . 88.18(7) yes
O19 . V4 . O24 . 172.72(13) yes
O20 . V4 . O24 . 83.79(12) yes
O21 . V4 . O24 . 76.72(10) yes
O22 . V4 . O23 . 87.12(11) yes
O22 . V4 . O24 . 81.79(12) yes
O23 . V4 . O24 . 86.91(11) yes
O27 2_647 V5 . O29 2_647 89.31(12) yes
O27 2_647 V5 . O28 1_545 164.51(12) yes
O29 2_647 V5 . O28 1_545 86.98(12) yes
O27 2_647 V5 . Se12 1_545 151.43(18) yes
O29 2_647 V5 . Se12 1_545 62.28(18) yes
O28 1_545 V5 . Se12 1_545 27.2(2) yes
O27 2_647 V5 . Se13 1_545 148.85(19) yes
O29 2_647 V5 . Se13 1_545 60.39(19) yes
O28 1_545 V5 . Se13 1_545 27.5(2) yes
Se12 1_545 V5 . Se13 1_545 4.3(3) yes
O27 2_647 V5 . Se1 2_647 26.64(8) yes
O29 2_647 V5 . Se1 2_647 89.42(8) yes
O28 1_545 V5 . Se1 2_647 167.86(9) yes
Se12 1_545 V5 . Se1 2_647 143.85(18) yes
Se13 1_545 V5 . Se1 2_647 144.75(19) yes
O27 2_647 V5 . O25 . 96.37(13) yes
O29 2_647 V5 . O25 . 99.02(15) yes
O28 1_545 V5 . O25 . 99.06(14) yes
Se12 1_545 V5 . O25 . 91.44(17) yes
Se13 1_545 V5 . O25 . 95.51(18) yes
O27 2_647 V5 . O26 . 90.71(12) yes
O29 2_647 V5 . O26 . 162.78(12) yes
O28 1_545 V5 . O26 . 88.44(12) yes
Se12 1_545 V5 . O26 . 115.39(19) yes
Se13 1_545 V5 . O26 . 115.9(2) yes
O27 2_647 V5 . O30 . 78.85(10) yes
O29 2_647 V5 . O30 . 83.04(12) yes
O28 1_545 V5 . O30 . 85.77(11) yes
Se12 1_545 V5 . O30 . 93.72(16) yes
Se13 1_545 V5 . O30 . 89.65(16) yes
Se1 2_647 V5 . O25 . 70.06(11) yes
Se1 2_647 V5 . O26 . 98.23(8) yes
O25 . V5 . O26 . 98.09(15) yes
Se1 2_647 V5 . O30 . 105.30(7) yes
O25 . V5 . O30 . 174.82(13) yes
O26 . V5 . O30 . 80.08(12) yes
O34 1_565 V6 . O33 2_757 82.04(12) yes
O34 1_565 V6 . O35 3_656 86.47(12) yes
O33 2_757 V6 . O35 3_656 161.79(12) yes
O34 1_565 V6 . Se9 1_565 27.02(9) yes
O33 2_757 V6 . Se9 1_565 55.90(8) yes
O35 3_656 V6 . Se9 1_565 113.49(8) yes
O34 1_565 V6 . Se6 . 163.17(9) yes
O33 2_757 V6 . Se6 . 90.87(8) yes
O35 3_656 V6 . Se6 . 103.78(8) yes
Se9 1_565 V6 . Se6 . 140.54(3) yes
O34 1_565 V6 . O31 . 96.30(14) yes
O33 2_757 V6 . O31 . 98.17(14) yes
O35 3_656 V6 . O31 . 97.08(15) yes
Se9 1_565 V6 . O31 . 92.81(11) yes
Se6 . V6 . O31 . 69.50(11) yes
O34 1_565 V6 . O32 . 165.93(13) yes
O33 2_757 V6 . O32 . 90.77(12) yes
O35 3_656 V6 . O32 . 97.27(12) yes
Se9 1_565 V6 . O32 . 146.38(10) yes
Se6 . V6 . O32 . 27.46(8) yes
O34 1_565 V6 . O36 . 86.47(11) yes
O33 2_757 V6 . O36 . 82.15(12) yes
O35 3_656 V6 . O36 . 83.10(12) yes
Se9 1_565 V6 . O36 . 89.65(8) yes
Se6 . V6 . O36 . 107.77(8) yes
O31 . V6 . O32 . 96.69(14) yes
O31 . V6 . O36 . 177.24(13) yes
O32 . V6 . O36 . 80.56(11) yes
V5 2_647 Se1 . O2 . 127.75(10) yes
V5 2_647 Se1 . O27 . 32.47(9) yes
O2 . Se1 . O27 . 100.74(14) yes
V5 2_647 Se1 . O35 . 110.57(9) yes
O2 . Se1 . O35 . 96.76(13) yes
O27 . Se1 . O35 . 100.95(13) yes
V1 . Se2 . O3 . 32.71(9) yes
V1 . Se2 . O8 . 109.43(9) yes
O3 . Se2 . O8 . 100.05(14) yes
V1 . Se2 . O29 . 128.52(10) yes
O3 . Se2 . O29 . 101.10(14) yes
O8 . Se2 . O29 . 96.95(13) yes
V2 . Se3 . O4 . 107.37(10) yes
V2 . Se3 . O9 . 29.37(9) yes
O4 . Se3 . O9 . 100.03(14) yes
V2 . Se3 . O14 . 123.80(10) yes
O4 . Se3 . O14 . 99.09(14) yes
O9 . Se3 . O14 . 98.62(14) yes
V3 . Se4 . O10 . 125.06(9) yes
V3 . Se4 . O15 . 32.73(9) yes
O10 . Se4 . O15 . 99.14(14) yes
V3 . Se4 . O20 . 114.07(10) yes
O10 . Se4 . O20 . 97.39(14) yes
O15 . Se4 . O20 . 103.02(14) yes
V4 . Se5 . O16 . 114.13(10) yes
V4 . Se5 . O21 . 32.74(9) yes
O16 . Se5 . O21 . 102.88(14) yes
V4 . Se5 . O33 . 124.00(9) yes
O16 . Se5 . O33 . 97.68(14) yes
O21 . Se5 . O33 . 98.13(14) yes
O22 2_757 Se6 . O26 4_544 98.79(14) yes
O22 2_757 Se6 . V6 . 122.38(10) yes
O26 4_544 Se6 . V6 . 107.98(10) yes
O22 2_757 Se6 . O32 . 97.77(13) yes
O26 4_544 Se6 . O32 . 99.87(13) yes
V6 . Se6 . O32 . 29.04(9) yes
O6 3_646 Se7 . V1 . 131.73(11) yes
O6 3_646 Se7 . O5 . 100.73(14) yes
V1 . Se7 . O5 . 33.00(9) yes
O6 3_646 Se7 . O37 . 99.54(15) yes
V1 . Se7 . O37 . 98.30(11) yes
O5 . Se7 . O37 . 95.37(16) yes
V3 . Se8 . O17 . 31.82(10) yes
V3 . Se8 . O36 . 130.76(11) yes
O17 . Se8 . O36 . 101.68(15) yes
V3 . Se8 . O38 . 101.90(13) yes
O17 . Se8 . O38 . 97.72(17) yes
O36 . Se8 . O38 . 99.29(17) yes
V6 1_545 Se9 . O18 . 133.45(11) yes
V6 1_545 Se9 . O34 . 32.92(10) yes
O18 . Se9 . O34 . 102.09(14) yes
V6 1_545 Se9 . O39 . 100.5(8) yes
O18 . Se9 . O39 . 101.8(7) yes
O34 . Se9 . O39 . 102.1(8) yes
V6 1_545 Se9 . O40 . 99.6(8) yes
O18 . Se9 . O40 . 90.7(7) yes
O34 . Se9 . O40 . 92.1(8) yes
O39 . Se9 . O40 . 17.0(10) yes
O24 3_757 Se10 . V4 . 132.98(11) yes
O24 3_757 Se10 . O23 . 102.11(14) yes
V4 . Se10 . O23 . 34.00(9) yes
O24 3_757 Se10 . O41 . 97.60(15) yes
V4 . Se10 . O41 . 103.10(12) yes
O23 . Se10 . O41 . 97.55(16) yes
V2 . Se11 . O11 . 30.66(10) yes
V2 . Se11 . O30 . 129.38(10) yes
O11 . Se11 . O30 . 99.83(14) yes
V2 . Se11 . O42 . 96.89(11) yes
O11 . Se11 . O42 . 96.35(15) yes
O30 . Se11 . O42 . 99.87(15) yes
V5 1_565 Se12 . O12 . 136.5(4) yes
V5 1_565 Se12 . O28 . 33.6(3) yes
O12 . Se12 . O28 . 104.0(5) yes
V5 1_565 Se12 . O43 . 97.6(8) yes
O12 . Se12 . O43 . 100.9(8) yes
O28 . Se12 . O43 . 100.0(8) yes
V5 1_565 Se12 . O44 . 97.6(7) yes
O12 . Se12 . O44 . 89.2(7) yes
O28 . Se12 . O44 . 90.2(8) yes
O43 . Se12 . O44 . 17.6(9) yes
V5 1_565 Se13 . O12 . 130.9(4) yes
V5 1_565 Se13 . O28 . 32.9(3) yes
O12 . Se13 . O28 . 100.0(5) yes
V5 1_565 Se13 . O43 . 101.5(9) yes
O12 . Se13 . O43 . 110.1(9) yes
O28 . Se13 . O43 . 108.3(10) yes
V5 1_565 Se13 . O44 . 101.5(8) yes
O12 . Se13 . O44 . 96.5(8) yes
O28 . Se13 . O44 . 97.1(9) yes
O43 . Se13 . O44 . 20.2(10) yes
V1 . O2 . Se1 . 119.61(15) yes
V1 . O3 . Se2 . 120.58(15) yes
V1 . O4 . Se3 . 121.87(16) yes
V1 . O5 . Se7 . 119.74(16) yes
V1 . O6 . Se7 3_656 118.21(15) yes
V2 . O8 . Se2 . 122.97(16) yes
Se3 . O9 . V2 . 123.00(16) yes
V2 . O10 . Se4 . 121.55(15) yes
V2 . O11 . Se11 . 123.90(17) yes
V2 . O12 . Se13 . 121.1(4) yes
V2 . O12 . Se12 . 118.9(3) yes
Se13 . O12 . Se12 . 8.4(5) yes
V3 . O14 . Se3 . 121.36(15) yes
V3 . O15 . Se4 . 120.08(15) yes
V3 . O16 . Se5 . 120.04(15) yes
V3 . O17 . Se8 . 121.82(17) yes
V3 . O18 . Se9 . 120.19(16) yes
V4 . O20 . Se4 . 120.58(15) yes
V4 . O21 . Se5 . 120.03(14) yes
V4 . O22 . Se6 2_757 121.08(15) yes
V4 . O23 . Se10 . 118.18(16) yes
V4 . O24 . Se10 3_747 119.66(15) yes
V5 . O26 . Se6 4_545 121.33(15) yes
V5 2_647 O27 . Se1 . 120.90(15) yes
V5 1_565 O28 . Se13 . 119.6(4) yes
V5 1_565 O28 . Se12 . 119.3(4) yes
Se13 . O28 . Se12 . 8.1(5) yes
V5 2_647 O29 . Se2 . 120.17(15) yes
V5 . O30 . Se11 . 118.99(15) yes
Se6 . O32 . V6 . 123.50(15) yes
V6 2_757 O33 . Se5 . 121.87(15) yes
V6 1_545 O34 . Se9 . 120.06(16) yes
V6 3_646 O35 . Se1 . 121.92(15) yes
V6 . O36 . Se8 . 122.67(17) yes
Se7 . O37 . H1 . 108.7 no
Se8 . O38 . H2 . 109.2 no
Se9 . O39 . H3 . 120.5 no
Se9 . O40 . H3 . 98.1 no
Se10 . O41 . H4 . 111.1 no
Se11 . O42 . H5 . 112.4 no
Se12 . O43 . Se13 . 1.0(8) yes
Se12 . O43 . H6 . 153.8 no
Se13 . O43 . H6 . 153.7 no
Se12 . O44 . Se13 . 1.6(6) yes
Se12 . O44 . H6 . 129.6 no
Se13 . O44 . H6 . 128.4 no
H7 . O45 . H8 . 109.0 no
O46 2_667 O46 . H9 . 20.6 no
O46 2_667 O46 . H10 . 86.9 no
H9 . O46 . H10 . 107.5 no
H11 . O47 . H12 . 111.4 no
H13 . O48 . H14 . 109.7 no
H15 . O49 . H16 . 109.4 no
O50 2_757 O50 . O51 2_757 28.2(13) yes
O51 2_757 O51 . O50 2_757 35.8(14) yes
C1 . N1 . C3 . 112.2(4) yes
C1 . N1 . H17 . 109.7 no
C3 . N1 . H17 . 102.5 no
C1 . N1 . H18 . 109.0 no
C3 . N1 . H18 . 103.0 no
H17 . N1 . H18 . 120.1 no
C2 . N2 . C4 . 112.9(4) yes
C2 . N2 . H23 . 109.4 no
C4 . N2 . H23 . 108.5 no
C2 . N2 . H24 . 110.4 no
C4 . N2 . H24 . 109.2 no
H23 . N2 . H24 . 106.2 no
C5 . N3 . C7 . 113.6(4) yes
C5 . N3 . H31 . 108.3 no
C7 . N3 . H31 . 108.1 no
C5 . N3 . H32 . 108.6 no
C7 . N3 . H32 . 108.7 no
H31 . N3 . H32 . 109.4 no
C6 . N4 . C8 . 113.4(4) yes
C6 . N4 . H37 . 108.7 no
C8 . N4 . H37 . 108.2 no
C6 . N4 . H38 . 108.8 no
C8 . N4 . H38 . 108.4 no
H37 . N4 . H38 . 109.2 no
N1 . C1 . C2 . 109.9(4) yes
N1 . C1 . H19 . 110.4 no
C2 . C1 . H19 . 105.4 no
N1 . C1 . H20 . 114.8 no
C2 . C1 . H20 . 108.9 no
H19 . C1 . H20 . 107.0 no
C1 . C2 . N2 . 109.6(3) yes
C1 . C2 . H21 . 114.4 no
N2 . C2 . H21 . 108.2 no
C1 . C2 . H22 . 112.8 no
N2 . C2 . H22 . 107.7 no
H21 . C2 . H22 . 103.8 no
N1 . C3 . H25 . 108.7 no
N1 . C3 . H26 . 110.1 no
H25 . C3 . H26 . 107.9 no
N1 . C3 . H27 . 111.2 no
H25 . C3 . H27 . 111.5 no
H26 . C3 . H27 . 107.3 no
N2 . C4 . H28 . 106.8 no
N2 . C4 . H29 . 107.7 no
H28 . C4 . H29 . 111.6 no
N2 . C4 . H30 . 109.0 no
H28 . C4 . H30 . 109.0 no
H29 . C4 . H30 . 112.6 no
N3 . C5 . C6 . 109.8(4) yes
N3 . C5 . H33 . 109.7 no
C6 . C5 . H33 . 109.0 no
N3 . C5 . H34 . 110.5 no
C6 . C5 . H34 . 108.1 no
H33 . C5 . H34 . 109.7 no
C5 . C6 . N4 . 108.8(4) yes
C5 . C6 . H35 . 109.1 no
N4 . C6 . H35 . 110.0 no
C5 . C6 . H36 . 108.7 no
N4 . C6 . H36 . 111.1 no
H35 . C6 . H36 . 109.3 no
N3 . C7 . H39 . 109.1 no
N3 . C7 . H40 . 109.2 no
H39 . C7 . H40 . 109.2 no
N3 . C7 . H41 . 109.0 no
H39 . C7 . H41 . 110.4 no
H40 . C7 . H41 . 110.0 no
N4 . C8 . H42 . 109.1 no
N4 . C8 . H43 . 110.2 no
H42 . C8 . H43 . 109.9 no
N4 . C8 . H44 . 109.4 no
H42 . C8 . H44 . 109.4 no
H43 . C8 . H44 . 108.7 no
O40 . H3 . O39 . 27.6 no
O43 . H6 . O44 . 36.3 no
H10 2_667 H9 . O46 . 121.7 no
H9 2_667 H10 . O46 . 14.4 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O37 . H1 . O48 4_555 171.8(3) 0.822 1.878 2.694(9) yes
O38 . H2 . O47 2_656 138.2(3) 0.960 1.850 2.644(9) yes
O39 . H3 . O50 1_545 133.5(18) 0.849 1.747 2.412(9) yes
O40 . H3 . O50 1_545 128.2(14) 1.112 1.747 2.587(9) yes
O39 . H3 . O51 1_545 155.9(19) 0.849 1.661 2.461(9) yes
O40 . H3 . O51 1_545 147.6(14) 1.112 1.661 2.667(9) yes
O41 . H4 . O45 . 165.5(3) 0.822 1.772 2.575(9) yes
O42 . H5 . O49 1_546 169.9(3) 0.820 1.842 2.653(9) yes
O43 . H6 . O46 . 143.7(10) 1.015 1.699 2.587(9) yes
O44 . H6 . O46 . 167.2(15) 0.974 1.699 2.657(9) yes
O45 . H7 . O28 3_747 166.4(4) 0.964 1.826 2.771(9) yes
O45 . H8 . O23 3_747 124.4(3) 0.941 2.313 2.949(9) yes
O46 . H10 . O11 2_657 166.4(12) 0.967 1.909 2.858(9) yes
O47 . H12 . O5 2_656 149.7(4) 0.944 1.956 2.811(9) yes
O48 . H13 . O34 2_656 173.9(3) 0.947 2.008 2.951(9) yes
O48 . H14 . O14 2_666 166.1(3) 0.949 1.993 2.924(9) yes
O49 . H15 . O22 3_756 162.1(2) 0.950 2.037 2.956(9) yes
O49 . H16 . O23 1_564 163.8(2) 0.951 1.962 2.887(9) yes
N1 . H17 . O15 2_747 136.7(2) 0.915 2.174 2.909(9) yes
N1 . H17 . O18 2_747 143.8(3) 0.915 2.149 2.938(9) yes
N1 . H18 . O13 2_757 144.9(3) 0.875 2.110 2.870(9) yes
C1 . H19 . O20 2_747 175.2(3) 1.001 2.533 3.531(9) yes
C1 . H20 . O19 2_757 135.8(3) 0.927 2.430 3.161(9) yes
C2 . H21 . O16 2_747 160.8(3) 0.995 2.533 3.488(9) yes
C2 . H22 . O13 2_757 126.7(3) 0.976 2.497 3.178(9) yes
N2 . H23 . O21 2_747 134.7(2) 0.989 2.125 2.907(9) yes
N2 . H23 . O24 2_747 147.4(2) 0.989 2.075 2.956(9) yes
N2 . H24 . O19 2_757 137.8(2) 0.951 2.182 2.956(9) yes
N2 . H24 . O41 4_544 121.9(2) 0.951 2.320 2.936(9) yes
C3 . H25 . O48 1_646 134.1(4) 0.934 2.572 3.292(9) yes
C3 . H26 . O10 2_747 163.6(4) 0.984 2.507 3.461(9) yes
C4 . H28 . O33 2_747 161.1(3) 0.959 2.548 3.469(9) yes
N3 . H31 . O25 4_534 138.5(2) 0.950 2.025 2.808(9) yes
N3 . H32 . O27 3_656 127.5(2) 0.951 2.203 2.883(9) yes
N3 . H32 . O30 4_544 151.7(3) 0.951 2.010 2.883(9) yes
C5 . H33 . O2 3_656 166.7(3) 0.989 2.576 3.545(9) yes
C6 . H35 . O29 3_646 165.9(3) 0.994 2.592 3.565(9) yes
N4 . H37 . O1 3_656 140.4(2) 0.952 2.040 2.840(9) yes
N4 . H38 . O3 3_646 129.7(3) 0.950 2.191 2.892(9) yes
N4 . H38 . O6 3_646 151.7(3) 0.950 2.010 2.882(9) yes
C7 . H39 . O35 3_656 166.7(3) 0.964 2.458 3.404(9) yes
C7 . H41 . O31 1_545 172.8(3) 0.966 2.398 3.358(9) yes
C8 . H42 . O7 3_656 165.1(3) 0.966 2.376 3.319(9) yes
C8 . H44 . O8 3_646 169.1(3) 0.966 2.425 3.378(9) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 20/01/12 at 16:54:10
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 20/01/12 at 16:54:10
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
