# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1432056'
_audit_update_record             
;
2016-11-07 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;




_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H50 N2 O22 S2 V4, 1/2 (O C H4)'
_chemical_formula_sum            'C20.5 H52 N2 O22.5 S2 V4'
_chemical_formula_weight         954.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.7232(8)
_cell_length_b                   10.0127(9)
_cell_length_c                   11.9590(11)
_cell_angle_alpha                69.324(7)
_cell_angle_beta                 82.127(7)
_cell_angle_gamma                73.574(7)
_cell_volume                     936.57(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    210(2)
_cell_measurement_reflns_used    15420
_cell_measurement_theta_min      3.32
_cell_measurement_theta_max      29.62

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_F_000             500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_absorpt_coefficient_mu    1.166
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.5459
_exptl_absorpt_correction_T_max  0.7370
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      210(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            10419
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.594
_diffrn_reflns_theta_max         29.207
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             4989
_reflns_number_gt                4236
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'shelxs-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    diamond
_computing_publication_material  wingx
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0750P)²+0.4791P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4989
_refine_ls_number_parameters     240
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.1202
_refine_ls_wR_factor_gt          0.1165
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.87181(4) 0.26632(4) 0.05096(3) 0.01590(10) Uani 1 1 d . . . . .
V2 V 0.97321(4) 0.49179(4) 0.14697(3) 0.01500(10) Uani 1 1 d . . . . .
S5 S 0.64286(7) 0.39973(6) 0.24322(5) 0.01819(13) Uani 1 1 d . . . . .
O1 O 0.8923(2) 0.09158(19) 0.09626(16) 0.0252(4) Uani 1 1 d . . . . .
O2 O 1.0601(2) 0.4727(2) 0.26344(15) 0.0233(3) Uani 1 1 d . . . . .
O3 O 0.7327(2) 0.30533(19) -0.09171(16) 0.0228(3) Uani 1 1 d . . . . .
H3 H 0.6721 0.3832 -0.1333 0.034 Uiso 1 1 d R U . . .
O5 O 0.85072(19) 0.50857(16) -0.02203(14) 0.0154(3) Uani 1 1 d . . . . .
O6 O 0.99534(19) 0.28084(17) 0.17010(14) 0.0167(3) Uani 1 1 d . . . . .
O7 O 1.06294(19) 0.29039(17) -0.06227(14) 0.0169(3) Uani 1 1 d . . . . .
O9 O 0.7446(2) 0.50739(19) 0.21200(15) 0.0206(3) Uani 1 1 d . . . . .
O10 O 0.6685(2) 0.33189(18) 0.14538(15) 0.0208(3) Uani 1 1 d . . . . .
O15 O 0.4761(2) 0.4830(2) 0.24295(16) 0.0255(4) Uani 1 1 d . . . . .
O16 O 0.6835(2) 0.2865(2) 0.35747(16) 0.0304(4) Uani 1 1 d . . . . .
O31 O 1.4963(2) 0.1050(2) 0.22303(17) 0.0267(4) Uani 1 1 d . . . . .
H31 H 1.5503 0.1611 0.2078 0.040 Uiso 1 1 d R U . . .
C1 C 1.2174(3) 0.1994(2) -0.0235(2) 0.0186(4) Uani 1 1 d . . . . .
H1A H 1.2952 0.2210 -0.0892 0.022 Uiso 1 1 calc R U . . .
H1B H 1.2166 0.0969 -0.0035 0.022 Uiso 1 1 calc R U . . .
C2 C 0.7069(3) 0.6238(2) -0.0575(2) 0.0173(4) Uani 1 1 d . . . . .
H2A H 0.6253 0.6072 0.0061 0.021 Uiso 1 1 calc R U . . .
H2B H 0.6689 0.6184 -0.1279 0.021 Uiso 1 1 calc R U . . .
C3 C 1.2707(3) 0.2202(2) 0.0853(2) 0.0174(4) Uani 1 1 d . . . . .
C8 C 1.1525(3) 0.1841(2) 0.1919(2) 0.0185(4) Uani 1 1 d . . . . .
H8A H 1.1459 0.0833 0.2105 0.022 Uiso 1 1 calc R U . . .
H8B H 1.1926 0.1905 0.2611 0.022 Uiso 1 1 calc R U . . .
C10 C 1.4351(3) 0.1101(3) 0.1169(2) 0.0221(4) Uani 1 1 d . . . . .
H10A H 1.4261 0.0124 0.1262 0.026 Uiso 1 1 calc R U . . .
H10B H 1.5109 0.1366 0.0508 0.026 Uiso 1 1 calc R U . . .
C30 C 0.7950(3) 0.2318(3) -0.1782(2) 0.0287(5) Uani 1 1 d . . . . .
H30A H 0.7088 0.2129 -0.2073 0.043 Uiso 1 1 calc R U . . .
H30B H 0.8704 0.1402 -0.1413 0.043 Uiso 1 1 calc R U . . .
H30C H 0.8473 0.2933 -0.2437 0.043 Uiso 1 1 calc R U . . .
N1 N 0.3092(3) 0.2738(3) 0.5692(2) 0.0274(4) Uani 1 1 d . . . . .
C62 C 0.4626(4) 0.2549(4) 0.6210(3) 0.0376(6) Uani 1 1 d . . . . .
H62A H 0.5058 0.1525 0.6642 0.056 Uiso 1 1 calc R U . . .
H62B H 0.4439 0.3108 0.6745 0.056 Uiso 1 1 calc R U . . .
H62C H 0.5373 0.2894 0.5579 0.056 Uiso 1 1 calc R U . . .
C63 C 0.1931(4) 0.2203(4) 0.6684(3) 0.0396(7) Uani 1 1 d . . . . .
H63A H 0.0944 0.2308 0.6353 0.059 Uiso 1 1 calc R U . . .
H63B H 0.1734 0.2776 0.7209 0.059 Uiso 1 1 calc R U . . .
H63C H 0.2371 0.1184 0.7125 0.059 Uiso 1 1 calc R U . . .
C66 C 0.3385(5) 0.1860(5) 0.4864(3) 0.0481(9) Uani 1 1 d . . . . .
H66A H 0.2412 0.2038 0.4484 0.072 Uiso 1 1 calc R U . . .
H66B H 0.3739 0.0829 0.5311 0.072 Uiso 1 1 calc R U . . .
H66C H 0.4192 0.2149 0.4266 0.072 Uiso 1 1 calc R U . . .
C68 C 0.2456(5) 0.4341(4) 0.5007(3) 0.0449(8) Uani 1 1 d . . . . .
H68A H 0.1498 0.4472 0.4626 0.067 Uiso 1 1 calc R U . . .
H68B H 0.3243 0.4679 0.4410 0.067 Uiso 1 1 calc R U . . .
H68C H 0.2218 0.4899 0.5545 0.067 Uiso 1 1 calc R U . . .
C90 C -0.012(2) 0.0257(14) 0.5157(14) 0.046(3) Uiso 0.25 1 d D . P A -1
H90A H -0.1075 -0.0092 0.5311 0.068 Uiso 0.25 1 calc R U P A -1
H90B H 0.0567 -0.0280 0.5817 0.068 Uiso 0.25 1 calc R U P A -1
H90C H 0.0421 0.0109 0.4440 0.068 Uiso 0.25 1 calc R U P A -1
O90 O -0.0535(14) 0.1761(12) 0.5017(10) 0.055(3) Uiso 0.25 1 d D . P A -1
H90 H -0.1374 0.2090 0.4600 0.083 Uiso 0.25 1 d . U P B -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.6021(17) . ?
V1 O6 1.9667(16) . ?
V1 O7 2.0125(16) . ?
V1 O10 2.0415(17) . ?
V1 O3 2.0891(17) . ?
V1 O5 2.2307(15) . ?
V2 O2 1.6035(17) . ?
V2 O6 1.9866(16) . ?
V2 O5 1.9908(16) 2_765 ?
V2 O7 2.0051(16) 2_765 ?
V2 O9 2.0229(17) . ?
V2 O5 2.3462(16) . ?
S5 O16 1.4454(19) . ?
S5 O15 1.4581(18) . ?
S5 O9 1.5015(17) . ?
S5 O10 1.5113(17) . ?
O3 C30 1.436(3) . ?
O3 H3 0.8367 . ?
O5 C2 1.438(3) . ?
O5 V2 1.9908(16) 2_765 ?
O6 C8 1.433(3) . ?
O7 C1 1.428(3) . ?
O7 V2 2.0051(16) 2_765 ?
O31 C10 1.422(3) . ?
O31 H31 0.7903 . ?
C1 C3 1.538(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.541(3) 2_765 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C8 1.532(3) . ?
C3 C10 1.541(3) . ?
C3 C2 1.541(3) 2_765 ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
N1 C62 1.487(4) . ?
N1 C66 1.496(4) . ?
N1 C68 1.499(4) . ?
N1 C63 1.500(4) . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?
C90 O90 1.400(13) . ?
C90 H90A 0.9600 . ?
C90 H90B 0.9600 . ?
C90 H90C 0.9600 . ?
O90 H90 0.8604 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O6 100.10(8) . . ?
O1 V1 O7 102.48(8) . . ?
O6 V1 O7 86.79(7) . . ?
O1 V1 O10 100.92(8) . . ?
O6 V1 O10 88.16(7) . . ?
O7 V1 O10 156.58(7) . . ?
O1 V1 O3 93.56(8) . . ?
O6 V1 O3 166.33(7) . . ?
O7 V1 O3 90.18(7) . . ?
O10 V1 O3 89.36(7) . . ?
O1 V1 O5 176.67(8) . . ?
O6 V1 O5 81.44(6) . . ?
O7 V1 O5 74.60(6) . . ?
O10 V1 O5 82.04(6) . . ?
O3 V1 O5 84.90(6) . . ?
O2 V2 O6 99.39(8) . . ?
O2 V2 O5 103.83(8) . 2_765 ?
O6 V2 O5 88.47(6) . 2_765 ?
O2 V2 O7 100.88(8) . 2_765 ?
O6 V2 O7 158.67(7) . 2_765 ?
O5 V2 O7 80.33(6) 2_765 2_765 ?
O2 V2 O9 100.53(8) . . ?
O6 V2 O9 88.86(7) . . ?
O5 V2 O9 155.61(7) 2_765 . ?
O7 V2 O9 93.90(7) 2_765 . ?
O2 V2 O5 177.47(8) . . ?
O6 V2 O5 78.15(6) . . ?
O5 V2 O5 75.63(7) 2_765 . ?
O7 V2 O5 81.50(6) 2_765 . ?
O9 V2 O5 80.09(6) . . ?
O16 S5 O15 111.86(12) . . ?
O16 S5 O9 110.96(11) . . ?
O15 S5 O9 107.59(11) . . ?
O16 S5 O10 110.46(11) . . ?
O15 S5 O10 107.62(10) . . ?
O9 S5 O10 108.20(9) . . ?
C30 O3 V1 119.47(15) . . ?
C30 O3 H3 101.2 . . ?
V1 O3 H3 130.6 . . ?
C2 O5 V2 115.59(13) . 2_765 ?
C2 O5 V1 126.79(12) . . ?
V2 O5 V1 98.31(7) 2_765 . ?
C2 O5 V2 117.24(12) . . ?
V2 O5 V2 104.37(7) 2_765 . ?
V1 O5 V2 89.75(6) . . ?
C8 O6 V1 117.49(13) . . ?
C8 O6 V2 116.75(13) . . ?
V1 O6 V2 109.60(8) . . ?
C1 O7 V2 121.44(13) . 2_765 ?
C1 O7 V1 118.98(13) . . ?
V2 O7 V1 105.47(7) 2_765 . ?
S5 O9 V2 130.89(10) . . ?
S5 O10 V1 130.53(10) . . ?
C10 O31 H31 110.5 . . ?
O7 C1 C3 113.77(17) . . ?
O7 C1 H1A 108.8 . . ?
C3 C1 H1A 108.8 . . ?
O7 C1 H1B 108.8 . . ?
C3 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
O5 C2 C3 113.51(17) . 2_765 ?
O5 C2 H2A 108.9 . . ?
C3 C2 H2A 108.9 2_765 . ?
O5 C2 H2B 108.9 . . ?
C3 C2 H2B 108.9 2_765 . ?
H2A C2 H2B 107.7 . . ?
C8 C3 C1 110.37(18) . . ?
C8 C3 C10 109.04(18) . . ?
C1 C3 C10 106.43(18) . . ?
C8 C3 C2 110.84(18) . 2_765 ?
C1 C3 C2 112.51(18) . 2_765 ?
C10 C3 C2 107.46(18) . 2_765 ?
O6 C8 C3 112.93(18) . . ?
O6 C8 H8A 109.0 . . ?
C3 C8 H8A 109.0 . . ?
O6 C8 H8B 109.0 . . ?
C3 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
O31 C10 C3 114.04(19) . . ?
O31 C10 H10A 108.7 . . ?
C3 C10 H10A 108.7 . . ?
O31 C10 H10B 108.7 . . ?
C3 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
O3 C30 H30A 109.5 . . ?
O3 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O3 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C62 N1 C66 109.4(3) . . ?
C62 N1 C68 108.5(2) . . ?
C66 N1 C68 109.5(3) . . ?
C62 N1 C63 109.2(2) . . ?
C66 N1 C63 109.6(2) . . ?
C68 N1 C63 110.7(2) . . ?
N1 C62 H62A 109.5 . . ?
N1 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
N1 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
N1 C63 H63A 109.5 . . ?
N1 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
N1 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
N1 C66 H66A 109.5 . . ?
N1 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
N1 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
N1 C68 H68A 109.5 . . ?
N1 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
N1 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
O90 C90 H90A 109.5 . . ?
O90 C90 H90B 109.5 . . ?
H90A C90 H90B 109.5 . . ?
O90 C90 H90C 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
C90 O90 H90 102.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O16 S5 O9 V2 78.18(16) . . . . ?
O15 S5 O9 V2 -159.16(13) . . . . ?
O10 S5 O9 V2 -43.15(16) . . . . ?
O16 S5 O10 V1 -82.38(15) . . . . ?
O15 S5 O10 V1 155.24(13) . . . . ?
O9 S5 O10 V1 39.26(16) . . . . ?
V2 O7 C1 C3 72.8(2) 2_765 . . . ?
V1 O7 C1 C3 -61.4(2) . . . . ?
V2 O5 C2 C3 -65.2(2) 2_765 . . 2_765 ?
V1 O5 C2 C3 170.87(13) . . . 2_765 ?
V2 O5 C2 C3 58.6(2) . . . 2_765 ?
O7 C1 C3 C8 59.7(2) . . . . ?
O7 C1 C3 C10 177.86(17) . . . . ?
O7 C1 C3 C2 -64.7(2) . . . 2_765 ?
V1 O6 C8 C3 68.3(2) . . . . ?
V2 O6 C8 C3 -65.0(2) . . . . ?
C1 C3 C8 O6 -63.1(2) . . . . ?
C10 C3 C8 O6 -179.63(17) . . . . ?
C2 C3 C8 O6 62.3(2) 2_765 . . . ?
C8 C3 C10 O31 -55.6(2) . . . . ?
C1 C3 C10 O31 -174.62(18) . . . . ?
C2 C3 C10 O31 64.6(2) 2_765 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 O15 0.84 1.85 2.663(3) 163.0 2_665
O31 H31 O10 0.79 2.10 2.888(2) 170.8 1_655
O31 H31 S5 0.79 2.90 3.6226(19) 152.2 1_655
O90 H90 O16 0.86 1.93 2.786(12) 176.3 1_455

_refine_diff_density_max         1.348
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.104

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1432057'
_audit_update_record             
;
2016-11-07 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT602_shelx               
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info 
RESPONSE: Electron density of disordered solvent molecules (water and methanol) 
was 'squeezed' using Platon software.
;
_vrf_PLAT420_shelx               
;
PROBLEM: Without Acceptor       O14    --  H14X   ...     Please Check 
RESPONSE: The acceptor was a disordered solvent molecule treated with squeeze.
;
_vrf_PLAT420_shelx_2             
;
PROBLEM: Without Acceptor       O26    --  H26    ...     Please Check  
RESPONSE: The acceptor was a disordered solvent molecule treated with squeeze.
;
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          17 Note  
RESPONSE: Problem due to quality of data set.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H48 Br2 N2 O20 S2 V4'
_chemical_formula_sum            'C20 H48 Br2 N2 O20 S2 V4'
_chemical_formula_weight         1064.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   22.978(2)
_cell_length_b                   18.4636(13)
_cell_length_c                   10.5713(9)
_cell_angle_alpha                90
_cell_angle_beta                 91.738(7)
_cell_angle_gamma                90
_cell_volume                     4482.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    210(2)
_cell_measurement_reflns_used    17008
_cell_measurement_theta_min      3.31
_cell_measurement_theta_max      29.21

_exptl_crystal_description       platelet
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_F_000             2144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    2.749
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.5459
_exptl_absorpt_correction_T_max  0.7370
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      210(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            27903
_diffrn_reflns_av_unetI/netI     0.1188
_diffrn_reflns_av_R_equivalents  0.1030
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.395
_diffrn_reflns_theta_max         29.343
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             11602
_reflns_number_gt                5760
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'shelxs-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    diamond
_computing_publication_material  wingx
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1621P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11602
_refine_ls_number_parameters     452
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1467
_refine_ls_R_factor_gt           0.0923
_refine_ls_wR_factor_ref         0.2776
_refine_ls_wR_factor_gt          0.2437
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_restrained_S_all      0.925
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C6 C 0.0379(4) 1.0804(6) 0.9188(10) 0.063(3) Uani 1 1 d . . . . .
H6A H 0.0568 1.1234 0.9504 0.095 Uiso 1 1 calc R U . . .
H6B H 0.0000 1.0926 0.8845 0.095 Uiso 1 1 calc R U . . .
H6C H 0.0341 1.0463 0.9866 0.095 Uiso 1 1 calc R U . . .
O14 O 0.0724(3) 1.0486(3) 0.8205(6) 0.0500(14) Uani 1 1 d . . . . .
H14X H 0.1135 1.0617 0.8553 0.075 Uiso 1 1 d . U . . .
V1 V 0.03917(5) 0.93593(7) 0.42043(12) 0.0331(3) Uani 1 1 d . . . . .
V2 V 0.05072(5) 0.95628(7) 0.72340(13) 0.0376(3) Uani 1 1 d . . . . .
S1 S 0.16468(8) 0.92464(10) 0.5636(2) 0.0434(5) Uani 1 1 d . . . . .
O11 O 0.0332(3) 0.8668(3) 0.3315(6) 0.0497(14) Uani 1 1 d . . . . .
O12 O 0.0346(2) 0.8861(3) 0.5862(5) 0.0368(11) Uani 1 1 d . . . . .
O13 O 0.0472(2) 0.9043(4) 0.8426(6) 0.0503(14) Uani 1 1 d . . . . .
O15 O 0.04328(19) 1.0337(3) 0.5579(5) 0.0328(10) Uani 1 1 d . . . . .
O20 O 0.1355(2) 0.9538(3) 0.6774(6) 0.0459(13) Uani 1 1 d . . . . .
O21 O 0.1267(2) 0.9420(3) 0.4481(6) 0.0451(13) Uani 1 1 d . . . . .
O22 O 0.1738(2) 0.8477(3) 0.5732(8) 0.0606(19) Uani 1 1 d . . . . .
O23 O 0.2188(2) 0.9643(3) 0.5528(7) 0.0567(17) Uani 1 1 d . . . . .
O24 O 0.0344(2) 1.0164(3) 0.2921(5) 0.0361(11) Uani 1 1 d . . . . .
V3 V 0.44953(6) 0.95279(8) 0.21441(14) 0.0432(3) Uani 1 1 d . . . . .
V4 V 0.46305(5) 0.93503(7) -0.08715(13) 0.0379(3) Uani 1 1 d . . . . .
S2 S 0.33658(8) 0.92017(11) 0.0346(2) 0.0454(5) Uani 1 1 d . . . . .
O2 O 0.4682(2) 0.8844(3) 0.0797(6) 0.0444(13) Uani 1 1 d . . . . .
O3 O 0.4540(3) 0.8996(4) 0.3321(6) 0.0569(16) Uani 1 1 d . . . . .
O4 O 0.4709(2) 0.8671(3) -0.1776(6) 0.0470(13) Uani 1 1 d . . . . .
O5 O 0.3761(2) 0.9373(3) -0.0732(6) 0.0462(14) Uani 1 1 d . . . . .
O6 O 0.45540(19) 1.0311(3) 0.0529(5) 0.0359(11) Uani 1 1 d . . . . .
O7 O 0.3661(3) 0.9460(4) 0.1542(6) 0.0570(16) Uani 1 1 d . . . . .
O8 O 0.3249(2) 0.8440(3) 0.0398(8) 0.0596(18) Uani 1 1 d . . . . .
O9 O 0.2834(2) 0.9626(4) 0.0157(8) 0.0605(17) Uani 1 1 d . . . . .
O10 O 0.5337(2) 0.9836(3) 0.2123(5) 0.0387(11) Uani 1 1 d . . . . .
N1 N 0.1503(3) 0.6598(3) 0.5796(6) 0.0349(13) Uani 1 1 d . . . . .
N2 N 0.3540(3) 0.6601(3) 0.0670(6) 0.0359(13) Uani 1 1 d . . . . .
C18 C 0.4091(3) 0.7028(4) 0.0626(9) 0.0421(18) Uani 1 1 d . . . . .
H18A H 0.4318 0.6948 0.1390 0.063 Uiso 1 1 calc R U . . .
H18B H 0.4309 0.6877 -0.0088 0.063 Uiso 1 1 calc R U . . .
H18C H 0.4000 0.7534 0.0549 0.063 Uiso 1 1 calc R U . . .
C19 C 0.3676(3) 0.5803(4) 0.0766(9) 0.0447(18) Uani 1 1 d . . . . .
H19A H 0.3899 0.5711 0.1532 0.067 Uiso 1 1 calc R U . . .
H19B H 0.3320 0.5533 0.0777 0.067 Uiso 1 1 calc R U . . .
H19C H 0.3896 0.5657 0.0052 0.067 Uiso 1 1 calc R U . . .
C17 C 0.3194(3) 0.6732(5) -0.0521(8) 0.0431(18) Uani 1 1 d . . . . .
H17A H 0.3418 0.6590 -0.1232 0.065 Uiso 1 1 calc R U . . .
H17B H 0.2841 0.6454 -0.0511 0.065 Uiso 1 1 calc R U . . .
H17C H 0.3101 0.7238 -0.0587 0.065 Uiso 1 1 calc R U . . .
C20 C 0.3212(3) 0.6814(5) 0.1805(9) 0.0457(19) Uani 1 1 d . . . . .
H20A H 0.3446 0.6723 0.2555 0.068 Uiso 1 1 calc R U . . .
H20B H 0.3118 0.7321 0.1758 0.068 Uiso 1 1 calc R U . . .
H20C H 0.2859 0.6537 0.1835 0.068 Uiso 1 1 calc R U . . .
C14 C 0.0945(3) 0.7016(4) 0.5798(9) 0.047(2) Uani 1 1 d . . . . .
H14A H 0.0702 0.6871 0.5088 0.070 Uiso 1 1 calc R U . . .
H14B H 0.0748 0.6920 0.6568 0.070 Uiso 1 1 calc R U . . .
H14C H 0.1027 0.7524 0.5740 0.070 Uiso 1 1 calc R U . . .
C13 C 0.1385(4) 0.5791(4) 0.5868(10) 0.050(2) Uani 1 1 d . . . . .
H13A H 0.1145 0.5646 0.5152 0.075 Uiso 1 1 calc R U . . .
H13B H 0.1747 0.5532 0.5862 0.075 Uiso 1 1 calc R U . . .
H13C H 0.1188 0.5684 0.6634 0.075 Uiso 1 1 calc R U . . .
C15 C 0.1793(3) 0.6748(5) 0.4595(8) 0.0447(18) Uani 1 1 d . . . . .
H15A H 0.1545 0.6595 0.3897 0.067 Uiso 1 1 calc R U . . .
H15B H 0.1867 0.7258 0.4527 0.067 Uiso 1 1 calc R U . . .
H15C H 0.2154 0.6488 0.4579 0.067 Uiso 1 1 calc R U . . .
C16 C 0.1872(4) 0.6826(5) 0.6890(9) 0.056(2) Uani 1 1 d . . . . .
H16A H 0.1675 0.6723 0.7658 0.085 Uiso 1 1 calc R U . . .
H16B H 0.2234 0.6567 0.6888 0.085 Uiso 1 1 calc R U . . .
H16C H 0.1946 0.7336 0.6836 0.085 Uiso 1 1 calc R U . . .
O26 O 0.4230(3) 1.0432(4) 0.3114(6) 0.0545(15) Uani 1 1 d . . . . .
H26 H 0.3876 1.0638 0.2864 0.065 Uiso 1 1 calc R U . . .
C1 C 0.0830(3) 1.0909(4) 0.5300(7) 0.0356(15) Uani 1 1 d . . . . .
H1A H 0.1223 1.0716 0.5330 0.043 Uiso 1 1 calc R U . . .
H1B H 0.0807 1.1276 0.5953 0.043 Uiso 1 1 calc R U . . .
C3 C 0.0764(3) 1.0726(4) 0.2905(8) 0.0393(16) Uani 1 1 d . . . . .
H3A H 0.0718 1.0990 0.2115 0.047 Uiso 1 1 calc R U . . .
H3B H 0.1150 1.0512 0.2932 0.047 Uiso 1 1 calc R U . . .
C10 C 0.4144(3) 1.0875(4) 0.0207(8) 0.0428(17) Uani 1 1 d . . . . .
H10A H 0.4155 1.1237 0.0873 0.051 Uiso 1 1 calc R U . . .
H10B H 0.3755 1.0670 0.0166 0.051 Uiso 1 1 calc R U . . .
C8 C 0.5159(3) 0.8351(4) 0.0990(8) 0.0406(17) Uani 1 1 d . . . . .
H8A H 0.5160 0.8003 0.0304 0.049 Uiso 1 1 calc R U . . .
H8B H 0.5111 0.8088 0.1774 0.049 Uiso 1 1 calc R U . . .
C12 C 0.4545(5) 1.0764(6) 0.4132(10) 0.066(3) Uani 1 1 d . . . . .
H12A H 0.4331 1.1175 0.4424 0.099 Uiso 1 1 calc R U . . .
H12B H 0.4598 1.0423 0.4811 0.099 Uiso 1 1 calc R U . . .
H12C H 0.4918 1.0919 0.3850 0.099 Uiso 1 1 calc R U . . .
C5 C 0.1188(3) 1.1832(5) 0.3917(9) 0.0479(19) Uani 1 1 d . . . . .
H5A H 0.1562 1.1588 0.3924 0.057 Uiso 1 1 calc R U . . .
H5B H 0.1181 1.2135 0.4667 0.057 Uiso 1 1 calc R U . . .
C2 C 0.0716(3) 1.1263(4) 0.4018(7) 0.0333(15) Uani 1 1 d . . . . .
C4 C -0.0118(3) 0.8361(4) 0.6000(8) 0.0354(15) Uani 1 1 d . . . . .
H4A H -0.0062 0.8102 0.6793 0.042 Uiso 1 1 calc R U . . .
H4B H -0.0111 0.8010 0.5319 0.042 Uiso 1 1 calc R U . . .
C9 C 0.4263(3) 1.1242(4) -0.1047(8) 0.0432(17) Uani 1 1 d . . . . .
C7 C 0.5764(3) 0.9272(5) 0.2174(8) 0.0454(18) Uani 1 1 d . . . . .
H7A H 0.5715 0.8994 0.2941 0.055 Uiso 1 1 calc R U . . .
H7B H 0.6148 0.9491 0.2227 0.055 Uiso 1 1 calc R U . . .
C11 C 0.3764(4) 1.1798(5) -0.1226(10) 0.056(2) Uani 1 1 d . . . . .
H11A H 0.3735 1.2090 -0.0456 0.067 Uiso 1 1 d . U . . .
H11B H 0.3396 1.1543 -0.1330 0.067 Uiso 1 1 d . U . . .
Br1 Br 0.11396(6) 1.24498(6) 0.24603(13) 0.0779(4) Uani 1 1 d . . . . .
Br2 Br 0.38136(7) 1.24566(8) -0.26019(16) 0.1010(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C6 O14 1.450(11) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
O14 V2 2.043(6) . ?
O14 H14X 1.0325 . ?
V1 O11 1.589(6) . ?
V1 O12 1.985(5) . ?
V1 O15 1.996(5) 3_576 ?
V1 O24 2.012(5) . ?
V1 O21 2.028(5) . ?
V1 O15 2.318(5) . ?
V2 O13 1.588(6) . ?
V2 O12 1.971(5) . ?
V2 O24 2.022(5) 3_576 ?
V2 O20 2.022(5) . ?
V2 O15 2.262(5) . ?
S1 O22 1.440(6) . ?
S1 O23 1.451(6) . ?
S1 O20 1.495(6) . ?
S1 O21 1.513(6) . ?
O12 C4 1.422(8) . ?
O15 C1 1.431(9) . ?
O15 V1 1.995(5) 3_576 ?
O24 C3 1.417(9) . ?
O24 V2 2.022(5) 3_576 ?
V3 O3 1.586(6) . ?
V3 O2 1.960(6) . ?
V3 O7 2.006(6) . ?
V3 O10 2.016(5) . ?
V3 O26 2.060(6) . ?
V3 O6 2.245(5) . ?
V4 O4 1.590(6) . ?
V4 O2 1.996(6) . ?
V4 O6 1.998(5) 3_675 ?
V4 O10 2.005(5) 3_675 ?
V4 O5 2.009(5) . ?
V4 O6 2.321(6) . ?
S2 O8 1.432(6) . ?
S2 O9 1.460(6) . ?
S2 O7 1.495(7) . ?
S2 O5 1.512(6) . ?
O2 C8 1.435(9) . ?
O6 C10 1.437(9) . ?
O6 V4 1.998(5) 3_675 ?
O10 C7 1.431(10) . ?
O10 V4 2.005(5) 3_675 ?
N1 C16 1.473(11) . ?
N1 C15 1.477(9) . ?
N1 C14 1.497(9) . ?
N1 C13 1.517(10) . ?
N2 C17 1.488(10) . ?
N2 C20 1.490(10) . ?
N2 C18 1.493(9) . ?
N2 C19 1.509(10) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
O26 C12 1.417(12) . ?
O26 H26 0.9300 . ?
C1 C2 1.521(10) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C3 C2 1.545(11) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C10 C9 1.521(11) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C8 C9 1.526(10) 3_675 ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C5 C2 1.517(10) . ?
C5 Br1 1.917(9) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C2 C4 1.539(9) 3_576 ?
C4 C2 1.539(9) 3_576 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C9 C7 1.524(12) 3_675 ?
C9 C8 1.526(10) 3_675 ?
C9 C11 1.547(12) . ?
C7 C9 1.524(12) 3_675 ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C11 Br2 1.902(10) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9714 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O14 C6 H6A 109.5 . . ?
O14 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O14 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C6 O14 V2 124.6(6) . . ?
C6 O14 H14X 99.4 . . ?
V2 O14 H14X 125.6 . . ?
O11 V1 O12 98.3(3) . . ?
O11 V1 O15 103.2(3) . 3_576 ?
O12 V1 O15 87.3(2) . 3_576 ?
O11 V1 O24 101.1(3) . . ?
O12 V1 O24 159.1(2) . . ?
O15 V1 O24 80.7(2) 3_576 . ?
O11 V1 O21 101.4(3) . . ?
O12 V1 O21 88.7(2) . . ?
O15 V1 O21 155.4(2) 3_576 . ?
O24 V1 O21 95.1(2) . . ?
O11 V1 O15 176.4(3) . . ?
O12 V1 O15 79.0(2) . . ?
O15 V1 O15 74.3(2) 3_576 . ?
O24 V1 O15 81.26(19) . . ?
O21 V1 O15 81.1(2) . . ?
O13 V2 O12 100.0(3) . . ?
O13 V2 O24 98.2(3) . 3_576 ?
O12 V2 O24 86.8(2) . 3_576 ?
O13 V2 O20 104.5(3) . . ?
O12 V2 O20 88.2(2) . . ?
O24 V2 O20 157.3(2) 3_576 . ?
O13 V2 O14 97.0(3) . . ?
O12 V2 O14 162.8(2) . . ?
O24 V2 O14 93.0(2) 3_576 . ?
O20 V2 O14 85.3(2) . . ?
O13 V2 O15 172.4(2) . . ?
O12 V2 O15 80.7(2) . . ?
O24 V2 O15 74.29(19) 3_576 . ?
O20 V2 O15 83.1(2) . . ?
O14 V2 O15 82.7(2) . . ?
O22 S1 O23 112.3(4) . . ?
O22 S1 O20 111.5(4) . . ?
O23 S1 O20 106.8(4) . . ?
O22 S1 O21 110.2(4) . . ?
O23 S1 O21 107.7(4) . . ?
O20 S1 O21 108.2(3) . . ?
C4 O12 V2 118.4(4) . . ?
C4 O12 V1 116.8(4) . . ?
V2 O12 V1 109.4(3) . . ?
C1 O15 V1 115.5(4) . 3_576 ?
C1 O15 V2 126.3(4) . . ?
V1 O15 V2 98.0(2) 3_576 . ?
C1 O15 V1 117.3(4) . . ?
V1 O15 V1 105.7(2) 3_576 . ?
V2 O15 V1 89.61(17) . . ?
S1 O20 V2 131.3(4) . . ?
S1 O21 V1 130.5(3) . . ?
C3 O24 V1 121.7(5) . . ?
C3 O24 V2 118.2(4) . 3_576 ?
V1 O24 V2 105.8(2) . 3_576 ?
O3 V3 O2 99.3(3) . . ?
O3 V3 O7 104.4(3) . . ?
O2 V3 O7 87.6(3) . . ?
O3 V3 O10 98.3(3) . . ?
O2 V3 O10 86.7(2) . . ?
O7 V3 O10 157.2(3) . . ?
O3 V3 O26 97.1(3) . . ?
O2 V3 O26 163.3(3) . . ?
O7 V3 O26 85.1(3) . . ?
O10 V3 O26 94.3(2) . . ?
O3 V3 O6 172.6(3) . . ?
O2 V3 O6 81.0(2) . . ?
O7 V3 O6 83.0(2) . . ?
O10 V3 O6 74.34(19) . . ?
O26 V3 O6 83.2(2) . . ?
O4 V4 O2 99.1(3) . . ?
O4 V4 O6 103.5(3) . 3_675 ?
O2 V4 O6 87.5(2) . 3_675 ?
O4 V4 O10 100.8(3) . 3_675 ?
O2 V4 O10 158.7(2) . 3_675 ?
O6 V4 O10 80.3(2) 3_675 3_675 ?
O4 V4 O5 101.0(3) . . ?
O2 V4 O5 88.7(2) . . ?
O6 V4 O5 155.5(2) 3_675 . ?
O10 V4 O5 95.2(2) 3_675 . ?
O4 V4 O6 176.8(3) . . ?
O2 V4 O6 78.3(2) . . ?
O6 V4 O6 74.6(2) 3_675 . ?
O10 V4 O6 81.6(2) 3_675 . ?
O5 V4 O6 80.9(2) . . ?
O8 S2 O9 112.0(4) . . ?
O8 S2 O7 111.2(4) . . ?
O9 S2 O7 107.5(4) . . ?
O8 S2 O5 110.6(4) . . ?
O9 S2 O5 107.7(4) . . ?
O7 S2 O5 107.7(3) . . ?
C8 O2 V3 119.2(5) . . ?
C8 O2 V4 116.5(4) . . ?
V3 O2 V4 109.4(3) . . ?
S2 O5 V4 132.3(4) . . ?
C10 O6 V4 114.9(4) . 3_675 ?
C10 O6 V3 126.3(4) . . ?
V4 O6 V3 98.1(2) 3_675 . ?
C10 O6 V4 117.7(5) . . ?
V4 O6 V4 105.4(2) 3_675 . ?
V3 O6 V4 89.99(19) . . ?
S2 O7 V3 133.9(4) . . ?
C7 O10 V4 122.0(5) . 3_675 ?
C7 O10 V3 116.8(5) . . ?
V4 O10 V3 105.9(2) 3_675 . ?
C16 N1 C15 111.0(7) . . ?
C16 N1 C14 108.9(7) . . ?
C15 N1 C14 108.2(6) . . ?
C16 N1 C13 109.9(7) . . ?
C15 N1 C13 108.2(6) . . ?
C14 N1 C13 110.6(6) . . ?
C17 N2 C20 111.6(6) . . ?
C17 N2 C18 108.6(6) . . ?
C20 N2 C18 109.6(6) . . ?
C17 N2 C19 108.7(6) . . ?
C20 N2 C19 108.2(6) . . ?
C18 N2 C19 110.1(6) . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C19 H19A 109.5 . . ?
N2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C20 H20A 109.5 . . ?
N2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C12 O26 V3 125.3(6) . . ?
C12 O26 H26 117.4 . . ?
V3 O26 H26 117.4 . . ?
O15 C1 C2 114.0(6) . . ?
O15 C1 H1A 108.8 . . ?
C2 C1 H1A 108.8 . . ?
O15 C1 H1B 108.8 . . ?
C2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.6 . . ?
O24 C3 C2 113.3(6) . . ?
O24 C3 H3A 108.9 . . ?
C2 C3 H3A 108.9 . . ?
O24 C3 H3B 108.9 . . ?
C2 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
O6 C10 C9 113.3(6) . . ?
O6 C10 H10A 108.9 . . ?
C9 C10 H10A 108.9 . . ?
O6 C10 H10B 108.9 . . ?
C9 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
O2 C8 C9 110.7(6) . 3_675 ?
O2 C8 H8A 109.5 . . ?
C9 C8 H8A 109.5 3_675 . ?
O2 C8 H8B 109.5 . . ?
C9 C8 H8B 109.5 3_675 . ?
H8A C8 H8B 108.1 . . ?
O26 C12 H12A 109.5 . . ?
O26 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O26 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C2 C5 Br1 116.4(6) . . ?
C2 C5 H5A 108.2 . . ?
Br1 C5 H5A 108.2 . . ?
C2 C5 H5B 108.2 . . ?
Br1 C5 H5B 108.2 . . ?
H5A C5 H5B 107.3 . . ?
C5 C2 C1 104.8(6) . . ?
C5 C2 C4 109.0(6) . 3_576 ?
C1 C2 C4 109.6(6) . 3_576 ?
C5 C2 C3 108.9(6) . . ?
C1 C2 C3 112.9(6) . . ?
C4 C2 C3 111.4(6) 3_576 . ?
O12 C4 C2 112.2(6) . 3_576 ?
O12 C4 H4A 109.2 . . ?
C2 C4 H4A 109.2 3_576 . ?
O12 C4 H4B 109.2 . . ?
C2 C4 H4B 109.2 3_576 . ?
H4A C4 H4B 107.9 . . ?
C10 C9 C7 113.6(7) . 3_675 ?
C10 C9 C8 111.4(7) . 3_675 ?
C7 C9 C8 110.6(7) 3_675 3_675 ?
C10 C9 C11 104.5(7) . . ?
C7 C9 C11 107.8(7) 3_675 . ?
C8 C9 C11 108.7(7) 3_675 . ?
O10 C7 C9 114.4(6) . 3_675 ?
O10 C7 H7A 108.7 . . ?
C9 C7 H7A 108.7 3_675 . ?
O10 C7 H7B 108.7 . . ?
C9 C7 H7B 108.7 3_675 . ?
H7A C7 H7B 107.6 . . ?
C9 C11 Br2 117.1(7) . . ?
C9 C11 H11A 109.4 . . ?
Br2 C11 H11A 106.9 . . ?
C9 C11 H11B 109.4 . . ?
Br2 C11 H11B 107.2 . . ?
H11A C11 H11B 106.3 . . ?

_refine_diff_density_max         1.640
_refine_diff_density_min         -1.751
_refine_diff_density_rms         0.162

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1432058'
_audit_update_record             
;
2016-11-07 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;


# start Validation Reply Form
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 11 Note
RESPONSE: This is a problem of the data set quality
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H52 N4 O20 S2 V4, 4 (O C H4), 2 (H2 O)'
_chemical_formula_sum            'C32 H72 N4 O26 S2 V4'
_chemical_formula_weight         1196.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.670(2)
_cell_length_b                   11.411(2)
_cell_length_c                   11.905(2)
_cell_angle_alpha                92.030(10)
_cell_angle_beta                 110.130(10)
_cell_angle_gamma                107.540(10)
_cell_volume                     1281.9(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    210(2)
_cell_measurement_reflns_used    14849
_cell_measurement_theta_min      3.31
_cell_measurement_theta_max      29.11

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_F_000             624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.874
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.5892
_exptl_absorpt_correction_T_max  0.8682
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      210(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            14956
_diffrn_reflns_av_unetI/netI     0.1176
_diffrn_reflns_av_R_equivalents  0.1086
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.320
_diffrn_reflns_theta_max         29.291
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6854
_reflns_number_gt                3476
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    DIAMOND
_computing_publication_material  WINGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0570P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   constr
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6854
_refine_ls_number_parameters     315
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1316
_refine_ls_R_factor_gt           0.0605
_refine_ls_wR_factor_ref         0.1448
_refine_ls_wR_factor_gt          0.1190
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_restrained_S_all      0.909
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O6 O 0.2209(3) 0.0178(2) 0.4843(2) 0.0414(6) Uani 1 1 d . . . . .
O5 O 0.0904(3) 0.1305(3) 0.2974(2) 0.0488(7) Uani 1 1 d . . . . .
O3 O 0.0530(3) 0.1221(2) 0.5217(2) 0.0411(6) Uani 1 1 d . . . . .
O2 O 0.3347(3) 0.2802(3) 0.5518(3) 0.0500(7) Uani 1 1 d . . . . .
O1 O 0.4324(3) 0.1308(3) 0.7080(2) 0.0517(7) Uani 1 1 d . . . . .
O4 O 0.1697(3) -0.0077(2) 0.6941(2) 0.0406(6) Uani 1 1 d . . . . .
N11 N -0.2288(4) 0.1051(4) -0.0778(3) 0.0533(9) Uani 1 1 d . . . . .
C23 C -0.3372(5) 0.0906(5) -0.0208(4) 0.0695(14) Uani 1 1 d . . . . .
H23A H -0.3074 0.1617 0.0396 0.104 Uiso 1 1 calc R U . . .
H23B H -0.4267 0.0841 -0.0819 0.104 Uiso 1 1 calc R U . . .
H23C H -0.3468 0.0168 0.0163 0.104 Uiso 1 1 calc R U . . .
C20 C -0.2132(5) 0.2208(5) -0.1346(4) 0.0613(12) Uani 1 1 d . . . . .
H20A H -0.1831 0.2915 -0.0737 0.092 Uiso 1 1 calc R U . . .
H20B H -0.1439 0.2302 -0.1710 0.092 Uiso 1 1 calc R U . . .
H20C H -0.3025 0.2150 -0.1956 0.092 Uiso 1 1 calc R U . . .
C22 C -0.2753(6) -0.0048(5) -0.1709(5) 0.0761(15) Uani 1 1 d . . . . .
H22A H -0.3646 -0.0110 -0.2321 0.114 Uiso 1 1 calc R U . . .
H22B H -0.2060 0.0039 -0.2072 0.114 Uiso 1 1 calc R U . . .
H22C H -0.2854 -0.0787 -0.1337 0.114 Uiso 1 1 calc R U . . .
C21 C -0.0901(5) 0.1161(5) 0.0181(4) 0.0720(14) Uani 1 1 d . . . . .
H21A H -0.0610 0.1875 0.0778 0.108 Uiso 1 1 calc R U . . .
H21B H -0.0997 0.0426 0.0558 0.108 Uiso 1 1 calc R U . . .
H21C H -0.0203 0.1252 -0.0177 0.108 Uiso 1 1 calc R U . . .
O30 O 0.5020(4) 0.2615(5) 0.0512(4) 0.0931(13) Uani 1 1 d . . . . .
H30 H 0.4155 0.2421 0.0219 0.140 Uiso 1 1 calc R U . . .
C4 C 0.2024(4) -0.3021(4) 0.5639(4) 0.0468(9) Uani 1 1 d . . . . .
C2 C 0.2453(4) -0.0978(4) 0.4937(4) 0.0471(9) Uani 1 1 d . . . . .
H2A H 0.3459 -0.0819 0.5355 0.056 Uiso 1 1 calc R U . . .
H2B H 0.2179 -0.1411 0.4128 0.056 Uiso 1 1 calc R U . . .
C5 C 0.1648(5) -0.3795(4) 0.4560(4) 0.0528(10) Uani 1 1 d . . . . .
H5 H 0.1137 -0.3601 0.3828 0.063 Uiso 1 1 calc R U . . .
C3 C 0.1633(4) -0.1833(4) 0.5618(3) 0.0444(9) Uani 1 1 d . . . . .
C6 C 0.2027(5) -0.4839(4) 0.4573(4) 0.0564(11) Uani 1 1 d . . . . .
H6 H 0.1751 -0.5346 0.3842 0.068 Uiso 1 1 calc R U . . .
N1 N 0.2783(4) -0.5166(3) 0.5600(3) 0.0539(9) Uani 1 1 d . . . . .
C8 C 0.2803(5) -0.3366(4) 0.6689(4) 0.0563(11) Uani 1 1 d . . . . .
H8 H 0.3099 -0.2877 0.7434 0.068 Uiso 1 1 calc R U . . .
C7 C 0.3139(5) -0.4443(4) 0.6624(4) 0.0605(12) Uani 1 1 d . . . . .
H7 H 0.3643 -0.4666 0.7341 0.073 Uiso 1 1 calc R U . . .
O31 O 0.1676(5) 0.4364(5) 1.0841(4) 0.0989(13) Uani 1 1 d . . . . .
H31 H 0.1601 0.4111 1.0159 0.148 Uiso 1 1 calc R U . . .
C30 C 0.2788(7) 0.4086(8) 1.1709(5) 0.109(2) Uani 1 1 d . . . . .
H30A H 0.3326 0.3820 1.1315 0.163 Uiso 1 1 calc R U . . .
H30B H 0.2403 0.3433 1.2106 0.163 Uiso 1 1 calc R U . . .
H30C H 0.3392 0.4814 1.2296 0.163 Uiso 1 1 calc R U . . .
C31 C 0.5633(6) 0.3578(6) -0.0056(6) 0.102(2) Uani 1 1 d . . . . .
H31A H 0.5559 0.3228 -0.0831 0.153 Uiso 1 1 calc R U . . .
H31B H 0.6613 0.3986 0.0442 0.153 Uiso 1 1 calc R U . . .
H31C H 0.5142 0.4170 -0.0163 0.153 Uiso 1 1 calc R U . . .
C40 C 0.4254(5) 0.2885(5) 0.4864(5) 0.0683(13) Uani 1 1 d . . . . .
H40A H 0.4385 0.3650 0.4538 0.102 Uiso 1 1 calc R U . . .
H40B H 0.5154 0.2864 0.5398 0.102 Uiso 1 1 calc R U . . .
H40C H 0.3835 0.2196 0.4216 0.102 Uiso 1 1 calc R U . . .
C9 C 0.2047(4) -0.1181(4) 0.6915(3) 0.0445(9) Uani 1 1 d . . . . .
H9A H 0.1570 -0.1753 0.7339 0.053 Uiso 1 1 calc R U . . .
H9B H 0.3059 -0.0977 0.7343 0.053 Uiso 1 1 calc R U . . .
H2 H 0.323(4) 0.352(4) 0.559(4) 0.051(13) Uiso 1 1 d . . . . .
V1 V 0.27736(7) 0.13450(7) 0.63643(6) 0.04203(18) Uani 1 1 d . . . . .
V2 V 0.03475(7) 0.02527(7) 0.37065(6) 0.04130(18) Uani 1 1 d . . . . .
S1 S 0.15073(11) 0.22841(10) 0.81908(9) 0.0459(2) Uani 1 1 d . . . . .
O21 O 0.2472(3) 0.2511(3) 0.7494(2) 0.0447(6) Uani 1 1 d . . . . .
O22 O -0.0121(3) -0.1330(3) 0.2579(2) 0.0462(6) Uani 1 1 d . . . . .
O23 O 0.2132(3) 0.1833(3) 0.9306(2) 0.0602(8) Uani 1 1 d . . . . .
O24 O 0.1256(3) 0.3430(3) 0.8424(3) 0.0576(8) Uani 1 1 d . . . . .
C1 C 0.0006(4) -0.2240(4) 0.4969(3) 0.0434(9) Uani 1 1 d . . . . .
H1A H -0.0265 -0.2732 0.4189 0.052 Uiso 1 1 calc R U . . .
H1B H -0.0435 -0.2768 0.5444 0.052 Uiso 1 1 calc R U . . .
O90 O -0.0545(5) 0.4175(4) 0.1683(4) 0.0997(13) Uani 1 1 d . . . . .
H90A H 0.0103 0.4260 0.1382 0.150 Uiso 1 1 d . U . . .
H90B H -0.0593 0.4915 0.1778 0.150 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O6 C2 1.421(5) . ?
O6 V1 2.003(3) . ?
O6 V2 2.011(3) . ?
O5 V2 1.599(3) . ?
O3 C1 1.435(4) 2_556 ?
O3 V2 1.995(3) . ?
O3 V1 2.269(3) . ?
O3 V2 2.318(3) 2_556 ?
O2 C40 1.421(5) . ?
O2 V1 2.020(3) . ?
O1 V1 1.594(3) . ?
O4 C9 1.420(5) . ?
O4 V1 1.980(3) . ?
O4 V2 1.990(3) 2_556 ?
N11 C22 1.482(6) . ?
N11 C21 1.492(5) . ?
N11 C20 1.495(6) . ?
N11 C23 1.503(5) . ?
O30 C31 1.420(7) . ?
C4 C8 1.387(6) . ?
C4 C5 1.394(6) . ?
C4 C3 1.533(6) . ?
C2 C3 1.551(5) . ?
C5 C6 1.368(6) . ?
C3 C9 1.544(5) . ?
C3 C1 1.547(5) . ?
C6 N1 1.349(5) . ?
N1 C7 1.316(6) . ?
C8 C7 1.387(6) . ?
O31 C30 1.409(7) . ?
V1 O21 2.027(3) . ?
V2 O4 1.990(3) 2_556 ?
V2 O22 2.034(3) . ?
V2 O3 2.318(3) 2_556 ?
S1 O24 1.447(3) . ?
S1 O23 1.456(3) . ?
S1 O22 1.496(3) 2_556 ?
S1 O21 1.503(3) . ?
O22 S1 1.496(3) 2_556 ?
C1 O3 1.435(4) 2_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 O6 V1 118.8(2) . . ?
C2 O6 V2 120.3(2) . . ?
V1 O6 V2 106.98(11) . . ?
C1 O3 V2 114.8(2) 2_556 . ?
C1 O3 V1 126.2(2) 2_556 . ?
V2 O3 V1 98.08(10) . . ?
C1 O3 V2 117.8(2) 2_556 2_556 ?
V2 O3 V2 105.37(11) . 2_556 ?
V1 O3 V2 90.18(9) . 2_556 ?
C40 O2 V1 123.4(3) . . ?
C9 O4 V1 116.8(2) . . ?
C9 O4 V2 117.4(2) . 2_556 ?
V1 O4 V2 109.84(12) . 2_556 ?
C22 N11 C21 110.2(4) . . ?
C22 N11 C20 110.0(4) . . ?
C21 N11 C20 109.0(4) . . ?
C22 N11 C23 109.3(4) . . ?
C21 N11 C23 109.0(3) . . ?
C20 N11 C23 109.4(4) . . ?
C8 C4 C5 116.3(4) . . ?
C8 C4 C3 123.6(4) . . ?
C5 C4 C3 120.1(4) . . ?
O6 C2 C3 113.5(3) . . ?
C6 C5 C4 120.2(4) . . ?
C4 C3 C9 111.1(3) . . ?
C4 C3 C1 106.5(3) . . ?
C9 C3 C1 108.8(3) . . ?
C4 C3 C2 106.5(3) . . ?
C9 C3 C2 110.5(3) . . ?
C1 C3 C2 113.4(3) . . ?
N1 C6 C5 122.9(4) . . ?
C7 N1 C6 117.3(4) . . ?
C7 C8 C4 119.8(4) . . ?
N1 C7 C8 123.4(4) . . ?
O4 C9 C3 113.1(3) . . ?
O1 V1 O4 98.33(13) . . ?
O1 V1 O6 100.50(12) . . ?
O4 V1 O6 87.01(10) . . ?
O1 V1 O2 97.05(14) . . ?
O4 V1 O2 164.61(11) . . ?
O6 V1 O2 89.69(12) . . ?
O1 V1 O21 104.71(13) . . ?
O4 V1 O21 88.71(10) . . ?
O6 V1 O21 154.78(11) . . ?
O2 V1 O21 87.90(12) . . ?
O1 V1 O3 174.09(13) . . ?
O4 V1 O3 80.08(10) . . ?
O6 V1 O3 73.78(9) . . ?
O2 V1 O3 84.56(11) . . ?
O21 V1 O3 81.00(10) . . ?
O5 V2 O4 99.19(12) . 2_556 ?
O5 V2 O3 103.51(13) . . ?
O4 V2 O3 87.83(10) 2_556 . ?
O5 V2 O6 99.81(12) . . ?
O4 V2 O6 159.35(10) 2_556 . ?
O3 V2 O6 79.93(10) . . ?
O5 V2 O22 101.80(12) . . ?
O4 V2 O22 88.99(10) 2_556 . ?
O3 V2 O22 154.67(11) . . ?
O6 V2 O22 94.98(11) . . ?
O5 V2 O3 177.17(12) . 2_556 ?
O4 V2 O3 78.68(10) 2_556 2_556 ?
O3 V2 O3 74.64(11) . 2_556 ?
O6 V2 O3 82.05(10) . 2_556 ?
O22 V2 O3 80.10(10) . 2_556 ?
O24 S1 O23 111.86(19) . . ?
O24 S1 O22 108.20(17) . 2_556 ?
O23 S1 O22 109.62(18) . 2_556 ?
O24 S1 O21 108.57(17) . . ?
O23 S1 O21 110.03(16) . . ?
O22 S1 O21 108.48(15) 2_556 . ?
S1 O21 V1 131.84(17) . . ?
S1 O22 V2 131.46(16) 2_556 . ?
O3 C1 C3 113.8(3) 2_556 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O30 H30 O23 0.82 1.94 2.750(5) 170.9 1_554
O30 H30 S1 0.82 2.97 3.711(4) 150.7 1_554
O31 H31 O24 0.82 2.05 2.867(5) 175.8 .
O2 H2 N1 0.87(5) 1.71(5) 2.571(5) 172(4) 1_565
C23 H23A O30 0.96 2.65 3.223(7) 118.6 1_455
C23 H23B O1 0.96 2.61 3.464(6) 149.0 1_454
C20 H20C O1 0.96 2.51 3.393(5) 153.2 1_454
C22 H22B O5 0.96 2.64 3.438(6) 140.9 2
C22 H22B O22 0.96 2.63 3.513(6) 153.3 2
C21 H21B O23 0.96 2.53 3.429(7) 155.4 2_556
O30 H30 S1 0.82 2.97 3.711(4) 150.7 1_554
O30 H30 O23 0.82 1.94 2.750(5) 170.9 1_554
C2 H2B O22 0.97 2.54 3.088(5) 115.5 .
C8 H8 O30 0.93 2.51 3.241(6) 135.6 2_656
O31 H31 O24 0.82 2.05 2.867(5) 175.8 .
O2 H2 N1 0.87(5) 1.71(5) 2.571(5) 172(4) 1_565
C1 H1A S1 0.97 2.82 3.538(4) 131.1 2_556
C1 H1A O21 0.97 2.60 3.129(5) 114.3 2_556
C1 H1A O22 0.97 2.56 3.037(5) 110.7 .
O90 H90A O31 0.87 1.97 2.830(6) 173.8 1_554
O90 H90B O24 0.87 2.20 3.044(5) 164.2 2_566

_refine_diff_density_max         0.456
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.074

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1432059'
_audit_update_record             
;
2016-11-07 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT420_shelx               
;
PROBLEM: D-H Without Acceptor O21 -- H21 ... Please Check
RESPONSE: The acceptor was probably removed by the program squeeze
;

# end Validation Reply Form




_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H52 N8 O21 S2 V4, O C H4'
_chemical_formula_sum            'C22 H56 N8 O22 S2 V4'
_chemical_formula_weight         1052.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   17.8617(10)
_cell_length_b                   23.0313(14)
_cell_length_c                   10.4655(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4305.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    210(2)
_cell_measurement_reflns_used    17008
_cell_measurement_theta_min      3.31
_cell_measurement_theta_max      29.21

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_F_000             2176
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    1.024
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      210(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            82981
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_av_R_equivalents  0.1216
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.423
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4394
_reflns_number_gt                3346
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  WINGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0534P)²+8.6753P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4394
_refine_ls_number_parameters     264
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.1143
_refine_ls_wR_factor_gt          0.1044
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O3 O 0.95725(12) 0.63402(9) 0.6769(2) 0.0209(5) Uani 1 1 d . . . . .
O2 O 0.94320(12) 0.62803(9) 0.4451(2) 0.0196(5) Uani 1 1 d . . . . .
O4 O 0.84877(12) 0.67641(10) 0.5741(3) 0.0266(6) Uani 1 1 d . . . . .
O1 O 0.97132(12) 0.71883(10) 0.5469(3) 0.0261(6) Uani 1 1 d . . . . .
O7 O 0.88328(11) 0.53597(9) 0.5875(2) 0.0147(5) Uani 1 1 d . . . . .
O9 O 0.90186(13) 0.54612(10) 0.8435(2) 0.0236(5) Uani 1 1 d . . . . .
O8 O 1.13728(12) 0.46338(10) 0.6695(2) 0.0221(5) Uani 1 1 d . . . . .
N2 N 0.73411(16) 0.34580(14) 0.7737(3) 0.0293(7) Uani 1 1 d . . . . .
C1 C 0.92339(17) 0.42288(13) 0.7116(3) 0.0164(7) Uani 1 1 d . . . . .
H1A H 0.8963 0.4267 0.7916 0.020 Uiso 1 1 calc R U . . .
H1B H 0.9446 0.3841 0.7089 0.020 Uiso 1 1 calc R U . . .
N1 N 0.76503(17) 0.39024(13) 0.7341(3) 0.0304(7) Uani 1 1 d . . . . .
C5 C 1.09575(16) 0.58143(13) 0.5299(3) 0.0157(7) Uani 1 1 d . . . . .
H5A H 1.1336 0.5776 0.5958 0.019 Uiso 1 1 calc R U . . .
H5B H 1.0772 0.6210 0.5325 0.019 Uiso 1 1 calc R U . . .
C4 C 0.80766(17) 0.38236(14) 0.6147(3) 0.0208(7) Uani 1 1 d . . . . .
H4A H 0.7738 0.3842 0.5424 0.025 Uiso 1 1 calc R U . . .
H4B H 0.8312 0.3444 0.6149 0.025 Uiso 1 1 calc R U . . .
C3 C 0.83065(16) 0.48951(13) 0.6036(3) 0.0162(7) Uani 1 1 d . . . . .
H3A H 0.7935 0.4915 0.5361 0.019 Uiso 1 1 calc R U . . .
H3B H 0.8049 0.4944 0.6845 0.019 Uiso 1 1 calc R U . . .
N3 N 0.7032(2) 0.30838(15) 0.8223(4) 0.0438(9) Uani 1 1 d . . . . .
C2 C 0.86807(16) 0.42961(13) 0.6008(3) 0.0143(6) Uani 1 1 d . . . . .
V1 V 1.06518(3) 0.45922(2) 0.57966(5) 0.01376(14) Uani 1 1 d . . . . .
V2 V 0.95736(3) 0.54921(2) 0.72361(6) 0.01572(14) Uani 1 1 d . . . . .
S3 S 0.92817(4) 0.66517(3) 0.56139(9) 0.0190(2) Uani 1 1 d . . . . .
O5 O 1.03530(11) 0.54250(8) 0.5575(2) 0.0134(5) Uani 1 1 d . . . . .
O6 O 0.98336(11) 0.46450(9) 0.7097(2) 0.0153(5) Uani 1 1 d . . . . .
O10 O 1.05444(13) 0.56816(10) 0.8201(2) 0.0244(5) Uani 1 1 d . . . . .
H10 H 1.0571 0.6072 0.8450 0.037 Uiso 1 1 d . U . . .
C10 C 1.0834(2) 0.53445(17) 0.9216(4) 0.0340(9) Uani 1 1 d . . . . .
H10A H 1.1291 0.5516 0.9518 0.051 Uiso 1 1 calc R U . . .
H10B H 1.0476 0.5332 0.9899 0.051 Uiso 1 1 calc R U . . .
H10C H 1.0931 0.4957 0.8919 0.051 Uiso 1 1 calc R U . . .
N4 N 0.34188(13) 0.35004(10) 0.4260(3) 0.0132(5) Uani 1 1 d . . . . .
C8 C 0.32048(17) 0.31527(14) 0.3116(3) 0.0194(7) Uani 1 1 d . . . . .
H8A H 0.3309 0.3372 0.2356 0.029 Uiso 1 1 calc R U . . .
H8B H 0.3488 0.2798 0.3102 0.029 Uiso 1 1 calc R U . . .
H8C H 0.2680 0.3064 0.3152 0.029 Uiso 1 1 calc R U . . .
C7 C 0.42399(16) 0.36342(14) 0.4197(3) 0.0189(7) Uani 1 1 d . . . . .
H7A H 0.4382 0.3858 0.4931 0.028 Uiso 1 1 calc R U . . .
H7B H 0.4519 0.3278 0.4183 0.028 Uiso 1 1 calc R U . . .
H7C H 0.4344 0.3852 0.3435 0.028 Uiso 1 1 calc R U . . .
C9 C 0.32605(18) 0.31646(14) 0.5457(3) 0.0205(7) Uani 1 1 d . . . . .
H9A H 0.3400 0.3393 0.6187 0.031 Uiso 1 1 calc R U . . .
H9B H 0.2736 0.3076 0.5500 0.031 Uiso 1 1 calc R U . . .
H9C H 0.3544 0.2810 0.5451 0.031 Uiso 1 1 calc R U . . .
C6 C 0.29705(17) 0.40506(13) 0.4281(3) 0.0189(7) Uani 1 1 d . . . . .
H6A H 0.3107 0.4276 0.5017 0.028 Uiso 1 1 calc R U . . .
H6B H 0.3071 0.4270 0.3521 0.028 Uiso 1 1 calc R U . . .
H6C H 0.2447 0.3958 0.4320 0.028 Uiso 1 1 calc R U . . .
O21 O 1.0869(2) 0.67063(13) 0.8985(3) 0.0584(10) Uani 1 1 d . . . . .
H21 H 1.0664 0.6983 0.8636 0.088 Uiso 1 1 calc R U . . .
C21 C 1.1300(2) 0.6908(2) 1.0034(4) 0.0420(11) Uani 1 1 d . . . . .
H21A H 1.1752 0.7084 0.9725 0.063 Uiso 1 1 calc R U . . .
H21B H 1.1424 0.6586 1.0580 0.063 Uiso 1 1 calc R U . . .
H21C H 1.1016 0.7188 1.0509 0.063 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O3 S3 1.499(3) . ?
O3 V2 2.013(2) . ?
O2 S3 1.512(2) . ?
O2 V1 2.031(2) 5_766 ?
O4 S3 1.448(2) . ?
O1 S3 1.464(2) . ?
O7 C3 1.434(3) . ?
O7 V2 1.968(2) . ?
O7 V1 1.980(2) 5_766 ?
O9 V2 1.600(2) . ?
O8 V1 1.598(2) . ?
N2 N3 1.142(4) . ?
N2 N1 1.235(4) . ?
C1 O6 1.438(3) . ?
C1 C2 1.532(4) . ?
N1 C4 1.474(4) . ?
C5 O5 1.433(3) . ?
C5 C2 1.534(4) 5_766 ?
C4 C2 1.539(4) . ?
C3 C2 1.533(4) . ?
C2 C5 1.534(4) 5_766 ?
V1 O7 1.980(2) 5_766 ?
V1 O6 2.001(2) . ?
V1 O5 2.004(2) . ?
V1 O2 2.032(2) 5_766 ?
V1 O5 2.299(2) 5_766 ?
V2 O6 2.011(2) . ?
V2 O10 2.053(2) . ?
V2 O5 2.232(2) . ?
O5 V1 2.299(2) 5_766 ?
O10 C10 1.413(4) . ?
N4 C8 1.490(4) . ?
N4 C9 1.499(4) . ?
N4 C6 1.499(4) . ?
N4 C7 1.500(4) . ?
O21 C21 1.419(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S3 O3 V2 131.34(14) . . ?
S3 O2 V1 130.48(14) . 5_766 ?
C3 O7 V2 118.13(19) . . ?
C3 O7 V1 116.76(19) . 5_766 ?
V2 O7 V1 108.56(9) . 5_766 ?
N3 N2 N1 172.2(4) . . ?
O6 C1 C2 113.7(2) . . ?
N2 N1 C4 114.4(3) . . ?
O5 C5 C2 113.2(2) . 5_766 ?
N1 C4 C2 110.8(3) . . ?
O7 C3 C2 112.5(2) . . ?
C1 C2 C3 111.0(3) . . ?
C1 C2 C5 112.8(2) . 5_766 ?
C3 C2 C5 110.5(3) . 5_766 ?
C1 C2 C4 108.0(3) . . ?
C3 C2 C4 109.2(2) . . ?
C5 C2 C4 105.2(2) 5_766 . ?
O8 V1 O7 98.17(11) . 5_766 ?
O8 V1 O6 100.64(11) . . ?
O7 V1 O6 159.59(9) 5_766 . ?
O8 V1 O5 103.01(10) . . ?
O7 V1 O5 88.18(9) 5_766 . ?
O6 V1 O5 79.97(9) . . ?
O8 V1 O2 101.18(10) . 5_766 ?
O7 V1 O2 88.68(9) 5_766 5_766 ?
O6 V1 O2 95.33(9) . 5_766 ?
O5 V1 O2 155.81(9) . 5_766 ?
O8 V1 O5 176.49(10) . 5_766 ?
O7 V1 O5 79.16(8) 5_766 5_766 ?
O6 V1 O5 81.70(8) . 5_766 ?
O5 V1 O5 74.72(9) . 5_766 ?
O2 V1 O5 81.13(8) 5_766 5_766 ?
O9 V2 O7 98.27(11) . . ?
O9 V2 O6 99.01(11) . . ?
O7 V2 O6 87.28(9) . . ?
O9 V2 O3 103.46(11) . . ?
O7 V2 O3 88.51(9) . . ?
O6 V2 O3 157.52(10) . . ?
O9 V2 O10 98.47(11) . . ?
O7 V2 O10 163.06(10) . . ?
O6 V2 O10 92.68(9) . . ?
O3 V2 O10 85.07(10) . . ?
O9 V2 O5 173.47(10) . . ?
O7 V2 O5 81.09(8) . . ?
O6 V2 O5 74.49(8) . . ?
O3 V2 O5 83.04(9) . . ?
O10 V2 O5 82.58(9) . . ?
O4 S3 O1 111.98(14) . . ?
O4 S3 O3 110.56(15) . . ?
O1 S3 O3 107.77(14) . . ?
O4 S3 O2 110.42(14) . . ?
O1 S3 O2 107.49(14) . . ?
O3 S3 O2 108.49(13) . . ?
C5 O5 V1 114.93(17) . . ?
C5 O5 V2 125.71(18) . . ?
V1 O5 V2 98.18(9) . . ?
C5 O5 V1 118.24(18) . 5_766 ?
V1 O5 V1 105.28(9) . 5_766 ?
V2 O5 V1 90.03(7) . 5_766 ?
C1 O6 V1 120.87(18) . . ?
C1 O6 V2 118.29(18) . . ?
V1 O6 V2 106.07(10) . . ?
C10 O10 V2 124.2(2) . . ?
C8 N4 C9 110.2(2) . . ?
C8 N4 C6 109.2(2) . . ?
C9 N4 C6 108.8(2) . . ?
C8 N4 C7 109.0(2) . . ?
C9 N4 C7 109.1(2) . . ?
C6 N4 C7 110.4(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O10 H10 O21 0.94 1.65 2.565(4) 163.4 .

_refine_diff_density_max         0.876
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.096



####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1432060'
_audit_update_record             
;
2016-11-07 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H66 N6 O30 S3 V6'
_chemical_formula_sum            'C24 H66 N6 O30 S3 V6'
_chemical_formula_weight         1320.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.2883(5)
_cell_length_b                   13.4071(7)
_cell_length_c                   33.9678(17)
_cell_angle_alpha                90
_cell_angle_beta                 92.671(3)
_cell_angle_gamma                90
_cell_volume                     5135.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9990
_cell_measurement_theta_min      2.604
_cell_measurement_theta_max      72.229

_exptl_crystal_description       Plate
_exptl_crystal_colour            grey
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_F_000             2712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    10.770
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.4932
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54106
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         2.604
_diffrn_reflns_theta_max         72.266
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.976
_reflns_number_total             9810
_reflns_number_gt                7562
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    DIAMOND
_computing_publication_material  WINGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0317P)²+54.0405P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9810
_refine_ls_number_parameters     629
_refine_ls_number_restraints     86
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0850
_refine_ls_wR_factor_ref         0.1843
_refine_ls_wR_factor_gt          0.1735
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_restrained_S_all      1.157
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O30 O 0.6194(5) 0.3229(5) 0.18072(15) 0.0391(14) Uani 1 1 d . . . . .
C2 C 0.3378(6) 0.2272(5) 0.00936(19) 0.0218(15) Uani 1 1 d . . . . .
H2A H 0.4020 0.2267 -0.0087 0.026 Uiso 1 1 calc R U . . .
H2B H 0.2891 0.2854 0.0035 0.026 Uiso 1 1 calc R U . . .
C1 C 0.3328(6) 0.0376(5) 0.00986(18) 0.0212(15) Uani 1 1 d . . . . .
H1A H 0.2810 -0.0191 0.0046 0.025 Uiso 1 1 calc R U . . .
H1B H 0.3960 0.0348 -0.0085 0.025 Uiso 1 1 calc R U . . .
C3 C 0.2627(6) 0.1330(5) 0.00288(17) 0.0206(14) Uani 1 1 d . . . . .
N1 N 0.1649(5) 0.1370(4) 0.03105(16) 0.0225(12) Uani 1 1 d . . . . .
H1C H 0.1234 0.1929 0.0271 0.034 Uiso 1 1 calc R U . . .
H1D H 0.1175 0.0846 0.0272 0.034 Uiso 1 1 calc R U . . .
H1E H 0.1957 0.1360 0.0557 0.034 Uiso 1 1 calc R U . . .
N2 N 0.1631(6) -0.0751(5) 0.1843(2) 0.0372(16) Uani 1 1 d . . . . .
H2C H 0.1181 -0.1076 0.1663 0.056 Uiso 1 1 calc R U . . .
H2D H 0.1184 -0.0537 0.2035 0.056 Uiso 1 1 calc R U . . .
H2E H 0.1970 -0.0231 0.1730 0.056 Uiso 1 1 calc R U . . .
C7 C 0.3360(7) -0.0914(6) 0.2318(2) 0.0324(19) Uani 1 1 d . . . . .
H7A H 0.2890 -0.0714 0.2536 0.039 Uiso 1 1 calc R U . . .
H7B H 0.3964 -0.1375 0.2418 0.039 Uiso 1 1 calc R U . . .
C5 C 0.3242(7) -0.1867(5) 0.1669(2) 0.0312(18) Uani 1 1 d . . . . .
H5A H 0.3831 -0.2340 0.1770 0.037 Uiso 1 1 calc R U . . .
H5B H 0.2692 -0.2221 0.1491 0.037 Uiso 1 1 calc R U . . .
C6 C 0.2572(7) -0.1436(6) 0.2011(2) 0.0326(18) Uani 1 1 d . . . . .
N3 N 0.1693(6) 0.3441(4) 0.18461(18) 0.0279(14) Uani 1 1 d . . . . .
H3A H 0.1244 0.3765 0.1665 0.042 Uiso 1 1 calc R U . . .
H3B H 0.2026 0.2916 0.1736 0.042 Uiso 1 1 calc R U . . .
H3C H 0.1244 0.3236 0.2039 0.042 Uiso 1 1 calc R U . . .
C9 C 0.3408(6) 0.3581(5) 0.23190(19) 0.0251(15) Uani 1 1 d . . . . .
H9A H 0.4017 0.4029 0.2425 0.030 Uiso 1 1 calc R U . . .
H9B H 0.2925 0.3377 0.2534 0.030 Uiso 1 1 calc R U . . .
C10 C 0.2639(6) 0.4125(6) 0.2011(2) 0.0255(16) Uani 1 1 d . . . . .
C11 C 0.3330(8) 0.4525(6) 0.1670(2) 0.0307(18) Uani 1 1 d . . . . .
H11A H 0.2793 0.4889 0.1491 0.037 Uiso 1 1 calc R U . . .
H11B H 0.3929 0.4988 0.1771 0.037 Uiso 1 1 calc R U . . .
V1 V 0.48710(10) 0.13218(9) 0.07493(3) 0.0170(2) Uani 1 1 d . . . . .
V2 V 0.39919(11) -0.07864(8) 0.08875(3) 0.0196(3) Uani 1 1 d . . . . .
V3 V 0.40382(12) 0.34366(9) 0.08845(3) 0.0235(3) Uani 1 1 d . . . . .
V4 V 0.42161(11) 0.13327(10) 0.23405(3) 0.0230(3) Uani 1 1 d . . . . .
V5 V 0.49055(11) -0.00598(9) 0.16890(3) 0.0223(3) Uani 1 1 d . . . . .
V6 V 0.49425(11) 0.27063(9) 0.16896(3) 0.0220(3) Uani 1 1 d . . . . .
S1 S 0.14064(19) 0.35502(15) 0.08208(6) 0.0348(5) Uani 1 1 d . . . . .
S2 S 0.13121(17) -0.08674(14) 0.07956(6) 0.0304(4) Uani 1 1 d . . . . .
S3 S 0.15457(18) 0.13577(17) 0.24722(7) 0.0442(5) Uani 1 1 d . . . . .
O1 O 0.3858(4) 0.2341(3) 0.04853(13) 0.0237(11) Uani 1 1 d . . . . .
O2 O 0.3829(4) 0.0300(3) 0.04912(12) 0.0173(10) Uani 1 1 d . . . . .
O4 O 0.4877(4) 0.2363(4) 0.11385(12) 0.0212(10) Uani 1 1 d . . . . .
O20 O 0.3888(4) 0.3758(4) 0.14582(13) 0.0263(11) Uani 1 1 d . . . . .
O3 O 0.4851(4) 0.0291(3) 0.11403(12) 0.0205(10) Uani 1 1 d . . . . .
O15 O 0.3953(4) 0.2726(4) 0.21584(13) 0.0225(11) Uani 1 1 d . . . . .
O11 O 0.3923(4) -0.0049(4) 0.21590(13) 0.0253(11) Uani 1 1 d . . . . .
O7 O 0.2434(4) -0.1430(4) 0.07155(15) 0.0283(11) Uani 1 1 d . . . . .
O12 O 0.4973(4) 0.1326(4) 0.18472(12) 0.0235(10) Uani 1 1 d . . . . .
O16 O 0.5231(5) 0.1322(4) 0.26892(13) 0.0329(12) Uani 1 1 d . . . . .
O10 O 0.3815(4) -0.1093(3) 0.14577(13) 0.0223(10) Uani 1 1 d . . . . .
O21 O 0.4966(5) 0.4213(4) 0.07166(15) 0.0395(15) Uani 1 1 d . . . . .
O6 O 0.4904(5) -0.1578(4) 0.07254(14) 0.0299(12) Uani 1 1 d . . . . .
O23 O 0.1851(5) 0.2649(4) 0.10248(15) 0.0332(13) Uani 1 1 d . . . . .
O8 O 0.1695(5) -0.0008(4) 0.10404(16) 0.0364(13) Uani 1 1 d . . . . .
O26 O 0.0759(5) -0.0535(4) 0.04185(16) 0.0382(14) Uani 1 1 d . . . . .
O22 O 0.2491(5) 0.4111(4) 0.07137(15) 0.0365(13) Uani 1 1 d . . . . .
O13 O 0.6144(5) -0.0593(4) 0.18016(15) 0.0354(13) Uani 1 1 d . . . . .
O14 O 0.2738(5) 0.1348(5) 0.26695(15) 0.0390(13) Uani 1 1 d . . . . .
O24 O 0.0718(6) 0.3312(5) 0.04641(18) 0.0503(17) Uani 1 1 d . . . . .
O9 O 0.0512(6) -0.1536(5) 0.09910(19) 0.0517(17) Uani 1 1 d . . . . .
O5 O 0.6115(4) 0.1307(4) 0.05405(14) 0.0308(12) Uani 1 1 d . . . . .
O17 O 0.0939(6) 0.2280(6) 0.2548(3) 0.077(2) Uani 1 1 d . . . . .
O18 O 0.1784(7) 0.1361(5) 0.2045(2) 0.062(2) Uani 1 1 d . . . . .
O25 O 0.0737(6) 0.4160(5) 0.1087(2) 0.0598(19) Uani 1 1 d . . . . .
O19 O 0.0911(7) 0.0450(6) 0.2561(3) 0.095(3) Uani 1 1 d . . . . .
O27 O 0.1340(5) 0.2164(4) -0.04512(16) 0.0381(14) Uani 1 1 d . . . . .
H27 H 0.1037 0.2150 -0.0675 0.057 Uiso 1 1 calc R U . . .
C4 C 0.2061(7) 0.1305(6) -0.0388(2) 0.0269(15) Uani 1 1 d . . . . .
H4A H 0.2675 0.1290 -0.0579 0.032 Uiso 1 1 calc R U . . .
H4B H 0.1582 0.0708 -0.0423 0.032 Uiso 1 1 calc R U . . .
O28 O 0.1010(10) -0.2752(8) 0.1942(3) 0.054(2) Uani 0.597(10) 1 d D . P A 1
H28 H 0.0684 -0.3209 0.2055 0.081 Uiso 0.597(10) 1 calc R U P A 1
O29 O 0.1234(10) 0.4670(8) 0.2469(3) 0.048(2) Uani 0.564(9) 1 d D . P B 1
H29 H 0.0727 0.4329 0.2352 0.071 Uiso 0.564(9) 1 calc R U P B 1
C8 C 0.1925(10) -0.2305(6) 0.2209(3) 0.050(3) Uani 0.597(10) 1 d D . P A 1
H8A H 0.2499 -0.2812 0.2290 0.061 Uiso 0.597(10) 1 calc R U P A 1
H8B H 0.1560 -0.2061 0.2443 0.061 Uiso 0.597(10) 1 calc R U P A 1
C12 C 0.2025(8) 0.5005(6) 0.2208(2) 0.038(2) Uani 0.564(9) 1 d D . P B 1
H12A H 0.2616 0.5420 0.2345 0.046 Uiso 0.564(9) 1 calc R U P B 1
H12B H 0.1615 0.5409 0.2008 0.046 Uiso 0.564(9) 1 calc R U P B 1
O29B O 0.1059(12) 0.5396(10) 0.1980(4) 0.048(2) Uani 0.436(9) 1 d D . P B 2
H29B H 0.0766 0.5861 0.2099 0.071 Uiso 0.436(9) 1 calc R U P B 2
O28B O 0.1251(14) -0.1923(11) 0.2512(5) 0.054(2) Uani 0.403(10) 1 d D . P A 2
H28B H 0.0761 -0.1525 0.2419 0.081 Uiso 0.403(10) 1 calc R U P A 2
C8B C 0.1925(10) -0.2305(6) 0.2209(3) 0.050(3) Uani 0.403(10) 1 d D . P A 2
H8B1 H 0.1411 -0.2645 0.2015 0.061 Uiso 0.403(10) 1 calc R U P A 2
H8B2 H 0.2500 -0.2782 0.2316 0.061 Uiso 0.403(10) 1 calc R U P A 2
C12B C 0.2025(8) 0.5005(6) 0.2208(2) 0.038(2) Uani 0.436(9) 1 d D . P B 2
H12C H 0.1748 0.4787 0.2460 0.046 Uiso 0.436(9) 1 calc R U P B 2
H12D H 0.2602 0.5531 0.2259 0.046 Uiso 0.436(9) 1 calc R U P B 2
N4 N 0.3433(7) 0.1327(5) 0.37630(17) 0.050(2) Uani 1 1 d D . . . .
C42 C 0.2848(11) 0.2231(6) 0.3598(3) 0.072(4) Uani 1 1 d D . . . .
H42A H 0.3222 0.2813 0.3712 0.107 Uiso 1 1 calc R U . . .
H42B H 0.2916 0.2241 0.3317 0.107 Uiso 1 1 calc R U . . .
H42C H 0.2025 0.2226 0.3658 0.107 Uiso 1 1 calc R U . . .
C40 C 0.2885(12) 0.0409(6) 0.3596(3) 0.093(5) Uani 1 1 d D . . . .
H40A H 0.3283 -0.0163 0.3709 0.140 Uiso 1 1 calc R U . . .
H40B H 0.2062 0.0390 0.3656 0.140 Uiso 1 1 calc R U . . .
H40C H 0.2953 0.0405 0.3316 0.140 Uiso 1 1 calc R U . . .
C41 C 0.4724(9) 0.1341(8) 0.3668(3) 0.093(5) Uani 1 1 d D . . . .
H41A H 0.5108 0.0755 0.3775 0.139 Uiso 1 1 calc R U . . .
H41B H 0.4791 0.1352 0.3387 0.139 Uiso 1 1 calc R U . . .
H41C H 0.5097 0.1924 0.3782 0.139 Uiso 1 1 calc R U . . .
C43 C 0.3386(8) 0.1333(6) 0.41989(19) 0.0367(19) Uani 1 1 d D . . . .
H43A H 0.3768 0.0745 0.4305 0.055 Uiso 1 1 calc R U . . .
H43B H 0.3788 0.1914 0.4303 0.055 Uiso 1 1 calc R U . . .
H43C H 0.2574 0.1344 0.4271 0.055 Uiso 1 1 calc R U . . .
N5 N 0.8552(8) 0.1493(7) 0.1331(3) 0.030(3) Uani 0.650(7) 1 d D . P C 1
C50 C 0.9641(12) 0.1521(13) 0.1589(4) 0.072(2) Uani 0.650(7) 1 d D . P C 1
H50A H 1.0255 0.1864 0.1457 0.109 Uiso 0.650(7) 1 calc R U P C 1
H50B H 0.9483 0.1865 0.1829 0.109 Uiso 0.650(7) 1 calc R U P C 1
H50C H 0.9893 0.0852 0.1649 0.109 Uiso 0.650(7) 1 calc R U P C 1
C53 C 0.7591(12) 0.0969(12) 0.1526(4) 0.072(2) Uani 0.650(7) 1 d D . P C 1
H53A H 0.6892 0.0959 0.1354 0.109 Uiso 0.650(7) 1 calc R U P C 1
H53B H 0.7833 0.0298 0.1586 0.109 Uiso 0.650(7) 1 calc R U P C 1
H53C H 0.7422 0.1310 0.1766 0.109 Uiso 0.650(7) 1 calc R U P C 1
C52 C 0.8155(14) 0.2508(11) 0.1216(4) 0.072(2) Uani 0.650(7) 1 d D . P C 1
H52A H 0.8782 0.2847 0.1089 0.109 Uiso 0.650(7) 1 calc R U P C 1
H52B H 0.7472 0.2463 0.1038 0.109 Uiso 0.650(7) 1 calc R U P C 1
H52C H 0.7953 0.2872 0.1447 0.109 Uiso 0.650(7) 1 calc R U P C 1
C51 C 0.8824(13) 0.0930(12) 0.0963(4) 0.072(2) Uani 0.650(7) 1 d D . P C 1
H51A H 0.9449 0.1262 0.0833 0.109 Uiso 0.650(7) 1 calc R U P C 1
H51B H 0.9069 0.0264 0.1031 0.109 Uiso 0.650(7) 1 calc R U P C 1
H51C H 0.8127 0.0904 0.0790 0.109 Uiso 0.650(7) 1 calc R U P C 1
N5B N 0.8629(15) 0.1133(13) 0.1441(5) 0.030(3) Uani 0.350(7) 1 d D . P C 2
C57 C 0.837(2) 0.149(2) 0.1834(7) 0.072(2) Uani 0.350(7) 1 d D . P C 2
H57A H 0.9055 0.1389 0.2008 0.109 Uiso 0.350(7) 1 calc R U P C 2
H57B H 0.8174 0.2182 0.1822 0.109 Uiso 0.350(7) 1 calc R U P C 2
H57C H 0.7714 0.1117 0.1929 0.109 Uiso 0.350(7) 1 calc R U P C 2
C55 C 0.966(2) 0.165(2) 0.1298(8) 0.072(2) Uani 0.350(7) 1 d D . P C 2
H55A H 1.0329 0.1548 0.1479 0.109 Uiso 0.350(7) 1 calc R U P C 2
H55B H 0.9842 0.1392 0.1044 0.109 Uiso 0.350(7) 1 calc R U P C 2
H55C H 0.9497 0.2351 0.1276 0.109 Uiso 0.350(7) 1 calc R U P C 2
C54 C 0.760(2) 0.127(2) 0.1173(7) 0.072(2) Uani 0.350(7) 1 d D . P C 2
H54A H 0.7783 0.1040 0.0915 0.109 Uiso 0.350(7) 1 calc R U P C 2
H54B H 0.6944 0.0905 0.1266 0.109 Uiso 0.350(7) 1 calc R U P C 2
H54C H 0.7405 0.1969 0.1159 0.109 Uiso 0.350(7) 1 calc R U P C 2
C56 C 0.890(2) 0.0065(18) 0.1469(8) 0.072(2) Uani 0.350(7) 1 d D . P C 2
H56A H 0.9576 -0.0034 0.1646 0.109 Uiso 0.350(7) 1 calc R U P C 2
H56B H 0.8229 -0.0283 0.1567 0.109 Uiso 0.350(7) 1 calc R U P C 2
H56C H 0.9066 -0.0188 0.1213 0.109 Uiso 0.350(7) 1 calc R U P C 2
N6 N -0.2123(5) 0.3640(4) -0.00847(18) 0.0336(15) Uani 1 1 d D . . . .
C61 C -0.1945(8) 0.4491(6) 0.0193(3) 0.052(3) Uani 1 1 d D . . . .
H61A H -0.2542 0.4472 0.0386 0.077 Uiso 1 1 calc R U . . .
H61B H -0.1174 0.4442 0.0324 0.077 Uiso 1 1 calc R U . . .
H61C H -0.2004 0.5107 0.0050 0.077 Uiso 1 1 calc R U . . .
C60 C -0.1199(7) 0.3671(6) -0.0382(2) 0.0369(18) Uani 1 1 d D . . . .
H60A H -0.0428 0.3638 -0.0250 0.055 Uiso 1 1 calc R U . . .
H60B H -0.1300 0.3113 -0.0557 0.055 Uiso 1 1 calc R U . . .
H60C H -0.1270 0.4280 -0.0529 0.055 Uiso 1 1 calc R U . . .
C62 C -0.3320(7) 0.3689(7) -0.0285(3) 0.053(2) Uani 1 1 d D . . . .
H62A H -0.3913 0.3669 -0.0091 0.079 Uiso 1 1 calc R U . . .
H62B H -0.3396 0.4299 -0.0432 0.079 Uiso 1 1 calc R U . . .
H62C H -0.3426 0.3132 -0.0460 0.079 Uiso 1 1 calc R U . . .
C63 C -0.2013(8) 0.2681(6) 0.0138(2) 0.045(2) Uani 1 1 d D . . . .
H63A H -0.2607 0.2654 0.0330 0.068 Uiso 1 1 calc R U . . .
H63B H -0.2120 0.2133 -0.0042 0.068 Uiso 1 1 calc R U . . .
H63C H -0.1240 0.2641 0.0267 0.068 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O30 V6 1.611(5) . ?
C2 O1 1.416(7) . ?
C2 C3 1.531(9) . ?
C1 O2 1.428(7) . ?
C1 C3 1.517(10) . ?
C3 N1 1.495(8) . ?
C3 C4 1.527(8) . ?
N2 C6 1.497(10) . ?
C7 O11 1.440(9) . ?
C7 C6 1.509(12) . ?
C5 O10 1.433(8) . ?
C5 C6 1.530(10) . ?
C6 C8B 1.545(11) . ?
C6 C8 1.545(11) . ?
N3 C10 1.497(9) . ?
C9 O15 1.421(8) . ?
C9 C10 1.514(10) . ?
C10 C11 1.525(10) . ?
C10 C12B 1.538(10) . ?
C10 C12 1.538(10) . ?
C11 O20 1.417(9) . ?
V1 O5 1.603(5) . ?
V1 O3 1.918(5) . ?
V1 O4 1.922(5) . ?
V1 O1 1.971(5) . ?
V1 O2 1.983(4) . ?
V1 V3 3.0289(17) . ?
V1 V2 3.0393(17) . ?
V2 O6 1.595(5) . ?
V2 O3 1.920(5) . ?
V2 O2 1.986(4) . ?
V2 O10 1.999(4) . ?
V2 O7 2.020(5) . ?
V2 V5 3.0272(17) . ?
V3 O21 1.601(5) . ?
V3 O4 1.907(5) . ?
V3 O1 2.003(5) . ?
V3 O20 2.011(5) . ?
V3 O22 2.027(6) . ?
V3 V6 3.0366(16) . ?
V4 O16 1.609(5) . ?
V4 O12 1.916(4) . ?
V4 O11 1.975(5) . ?
V4 O15 1.986(5) . ?
V4 O14 2.051(5) . ?
V4 V6 3.0200(17) . ?
V4 V5 3.0245(17) . ?
V5 O13 1.600(5) . ?
V5 O3 1.920(4) . ?
V5 O12 1.935(5) . ?
V5 O11 1.986(5) . ?
V5 O10 1.991(5) . ?
V6 O12 1.926(5) . ?
V6 O4 1.926(4) . ?
V6 O20 1.984(5) . ?
V6 O15 1.987(5) . ?
S1 O24 1.445(6) . ?
S1 O25 1.456(7) . ?
S1 O23 1.470(5) . ?
S1 O22 1.496(6) . ?
S2 O9 1.455(6) . ?
S2 O26 1.468(5) . ?
S2 O8 1.474(6) . ?
S2 O7 1.510(5) . ?
S3 O17 1.443(7) . ?
S3 O19 1.450(7) . ?
S3 O14 1.476(6) . ?
S3 O18 1.488(8) . ?
O27 C4 1.421(9) . ?
O28 C8 1.470(13) . ?
O29 C12 1.362(12) . ?
O29B C12B 1.408(14) . ?
O28B C8B 1.405(15) . ?
N4 C42 1.477(9) . ?
N4 C40 1.478(9) . ?
N4 C43 1.484(8) . ?
N4 C41 1.508(10) . ?
N5 C53 1.476(13) . ?
N5 C50 1.477(13) . ?
N5 C52 1.479(13) . ?
N5 C51 1.504(13) . ?
N5B C54 1.45(2) . ?
N5B C57 1.46(2) . ?
N5B C55 1.46(2) . ?
N5B C56 1.47(2) . ?
N6 C60 1.485(8) . ?
N6 C62 1.486(8) . ?
N6 C61 1.489(8) . ?
N6 C63 1.493(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C2 C3 112.0(5) . . ?
O2 C1 C3 112.8(5) . . ?
N1 C3 C1 109.0(6) . . ?
N1 C3 C4 107.8(5) . . ?
C1 C3 C4 108.6(5) . . ?
N1 C3 C2 107.4(5) . . ?
C1 C3 C2 113.1(5) . . ?
C4 C3 C2 110.9(6) . . ?
O11 C7 C6 111.8(6) . . ?
O10 C5 C6 110.9(6) . . ?
N2 C6 C7 111.4(6) . . ?
N2 C6 C5 108.0(6) . . ?
C7 C6 C5 113.7(7) . . ?
N2 C6 C8B 106.7(7) . . ?
C7 C6 C8B 109.0(6) . . ?
C5 C6 C8B 107.8(6) . . ?
N2 C6 C8 106.7(7) . . ?
C7 C6 C8 109.0(6) . . ?
C5 C6 C8 107.8(6) . . ?
O15 C9 C10 111.5(5) . . ?
N3 C10 C9 109.9(6) . . ?
N3 C10 C11 108.2(6) . . ?
C9 C10 C11 113.4(6) . . ?
N3 C10 C12B 107.7(6) . . ?
C9 C10 C12B 109.0(6) . . ?
C11 C10 C12B 108.5(6) . . ?
N3 C10 C12 107.7(6) . . ?
C9 C10 C12 109.0(6) . . ?
C11 C10 C12 108.5(6) . . ?
O20 C11 C10 112.6(6) . . ?
O5 V1 O3 109.7(3) . . ?
O5 V1 O4 109.8(2) . . ?
O3 V1 O4 92.69(19) . . ?
O5 V1 O1 108.0(2) . . ?
O3 V1 O1 142.1(2) . . ?
O4 V1 O1 78.04(19) . . ?
O5 V1 O2 108.1(2) . . ?
O3 V1 O2 77.43(19) . . ?
O4 V1 O2 142.1(2) . . ?
O1 V1 O2 87.59(18) . . ?
O5 V1 V3 111.3(2) . . ?
O3 V1 V3 123.77(14) . . ?
O4 V1 V3 37.55(14) . . ?
O1 V1 V3 40.73(13) . . ?
O2 V1 V3 122.11(14) . . ?
O5 V1 V2 110.9(2) . . ?
O3 V1 V2 37.65(14) . . ?
O4 V1 V2 124.05(14) . . ?
O1 V1 V2 121.90(15) . . ?
O2 V1 V2 40.07(13) . . ?
V3 V1 V2 137.84(5) . . ?
O6 V2 O3 109.6(3) . . ?
O6 V2 O2 107.2(2) . . ?
O3 V2 O2 77.32(18) . . ?
O6 V2 O10 107.0(2) . . ?
O3 V2 O10 78.03(19) . . ?
O2 V2 O10 142.87(18) . . ?
O6 V2 O7 100.5(3) . . ?
O3 V2 O7 149.9(2) . . ?
O2 V2 O7 93.7(2) . . ?
O10 V2 O7 93.9(2) . . ?
O6 V2 V5 109.1(2) . . ?
O3 V2 V5 37.98(13) . . ?
O2 V2 V5 112.99(13) . . ?
O10 V2 V5 40.55(14) . . ?
O7 V2 V5 130.76(15) . . ?
O6 V2 V1 110.2(2) . . ?
O3 V2 V1 37.61(13) . . ?
O2 V2 V1 40.00(13) . . ?
O10 V2 V1 112.90(14) . . ?
O7 V2 V1 129.69(15) . . ?
V5 V2 V1 74.91(4) . . ?
O21 V3 O4 109.4(3) . . ?
O21 V3 O1 106.5(2) . . ?
O4 V3 O1 77.61(19) . . ?
O21 V3 O20 107.0(2) . . ?
O4 V3 O20 77.6(2) . . ?
O1 V3 O20 143.4(2) . . ?
O21 V3 O22 100.2(3) . . ?
O4 V3 O22 150.4(2) . . ?
O1 V3 O22 94.3(2) . . ?
O20 V3 O22 94.1(2) . . ?
O21 V3 V1 110.0(2) . . ?
O4 V3 V1 37.90(13) . . ?
O1 V3 V1 39.95(14) . . ?
O20 V3 V1 112.86(15) . . ?
O22 V3 V1 130.06(16) . . ?
O21 V3 V6 109.4(2) . . ?
O4 V3 V6 37.83(13) . . ?
O1 V3 V6 113.12(14) . . ?
O20 V3 V6 40.21(15) . . ?
O22 V3 V6 130.58(17) . . ?
V1 V3 V6 74.99(4) . . ?
O16 V4 O12 108.2(2) . . ?
O16 V4 O11 109.0(3) . . ?
O12 V4 O11 78.3(2) . . ?
O16 V4 O15 109.2(3) . . ?
O12 V4 O15 78.4(2) . . ?
O11 V4 O15 139.85(18) . . ?
O16 V4 O14 99.7(2) . . ?
O12 V4 O14 152.1(2) . . ?
O11 V4 O14 92.9(2) . . ?
O15 V4 O14 92.7(2) . . ?
O16 V4 V6 109.6(2) . . ?
O12 V4 V6 38.30(16) . . ?
O11 V4 V6 113.00(14) . . ?
O15 V4 V6 40.55(14) . . ?
O14 V4 V6 130.42(17) . . ?
O16 V4 V5 109.5(2) . . ?
O12 V4 V5 38.47(16) . . ?
O11 V4 V5 40.35(14) . . ?
O15 V4 V5 113.12(14) . . ?
O14 V4 V5 130.43(18) . . ?
V6 V4 V5 75.70(4) . . ?
O13 V5 O3 109.2(2) . . ?
O13 V5 O12 109.9(3) . . ?
O3 V5 O12 91.92(19) . . ?
O13 V5 O11 109.0(2) . . ?
O3 V5 O11 141.7(2) . . ?
O12 V5 O11 77.7(2) . . ?
O13 V5 O10 107.5(3) . . ?
O3 V5 O10 78.22(19) . . ?
O12 V5 O10 142.5(2) . . ?
O11 V5 O10 87.9(2) . . ?
O13 V5 V4 110.6(2) . . ?
O3 V5 V4 124.14(15) . . ?
O12 V5 V4 38.03(13) . . ?
O11 V5 V4 40.09(15) . . ?
O10 V5 V4 122.88(14) . . ?
O13 V5 V2 109.2(2) . . ?
O3 V5 V2 37.96(14) . . ?
O12 V5 V2 124.49(14) . . ?
O11 V5 V2 123.07(16) . . ?
O10 V5 V2 40.76(13) . . ?
V4 V5 V2 140.19(5) . . ?
O30 V6 O12 110.1(3) . . ?
O30 V6 O4 109.8(2) . . ?
O12 V6 O4 92.3(2) . . ?
O30 V6 O20 107.0(3) . . ?
O12 V6 O20 142.7(2) . . ?
O4 V6 O20 77.9(2) . . ?
O30 V6 O15 108.4(2) . . ?
O12 V6 O15 78.10(19) . . ?
O4 V6 O15 141.7(2) . . ?
O20 V6 O15 87.62(19) . . ?
O30 V6 V4 110.4(2) . . ?
O12 V6 V4 38.07(13) . . ?
O4 V6 V4 124.50(15) . . ?
O20 V6 V4 123.02(15) . . ?
O15 V6 V4 40.51(14) . . ?
O30 V6 V3 109.7(2) . . ?
O12 V6 V3 124.12(14) . . ?
O4 V6 V3 37.40(15) . . ?
O20 V6 V3 40.86(13) . . ?
O15 V6 V3 122.63(14) . . ?
V4 V6 V3 139.87(5) . . ?
O24 S1 O25 111.8(4) . . ?
O24 S1 O23 111.8(3) . . ?
O25 S1 O23 110.1(4) . . ?
O24 S1 O22 108.8(4) . . ?
O25 S1 O22 108.8(4) . . ?
O23 S1 O22 105.2(3) . . ?
O9 S2 O26 109.7(4) . . ?
O9 S2 O8 113.4(4) . . ?
O26 S2 O8 110.9(3) . . ?
O9 S2 O7 108.5(4) . . ?
O26 S2 O7 108.7(3) . . ?
O8 S2 O7 105.4(3) . . ?
O17 S3 O19 116.0(5) . . ?
O17 S3 O14 110.9(4) . . ?
O19 S3 O14 110.3(4) . . ?
O17 S3 O18 106.3(5) . . ?
O19 S3 O18 108.5(5) . . ?
O14 S3 O18 103.9(4) . . ?
C2 O1 V1 124.8(4) . . ?
C2 O1 V3 135.0(4) . . ?
V1 O1 V3 99.3(2) . . ?
C1 O2 V1 124.4(4) . . ?
C1 O2 V2 134.9(4) . . ?
V1 O2 V2 99.93(19) . . ?
V3 O4 V1 104.6(2) . . ?
V3 O4 V6 104.8(2) . . ?
V1 O4 V6 147.2(3) . . ?
C11 O20 V6 125.9(4) . . ?
C11 O20 V3 134.9(4) . . ?
V6 O20 V3 98.9(2) . . ?
V1 O3 V2 104.7(2) . . ?
V1 O3 V5 148.0(3) . . ?
V2 O3 V5 104.1(2) . . ?
C9 O15 V4 134.4(4) . . ?
C9 O15 V6 126.0(4) . . ?
V4 O15 V6 98.9(2) . . ?
C7 O11 V4 135.2(4) . . ?
C7 O11 V5 124.6(4) . . ?
V4 O11 V5 99.6(2) . . ?
S2 O7 V2 117.4(3) . . ?
V4 O12 V6 103.6(2) . . ?
V4 O12 V5 103.5(2) . . ?
V6 O12 V5 147.7(2) . . ?
C5 O10 V5 126.3(4) . . ?
C5 O10 V2 134.6(5) . . ?
V5 O10 V2 98.7(2) . . ?
S1 O22 V3 114.2(3) . . ?
S3 O14 V4 120.0(3) . . ?
O27 C4 C3 109.5(6) . . ?
O28 C8 C6 111.8(8) . . ?
O29 C12 C10 110.6(7) . . ?
O28B C8B C6 109.0(9) . . ?
O29B C12B C10 113.6(8) . . ?
C42 N4 C40 111.5(7) . . ?
C42 N4 C43 109.8(6) . . ?
C40 N4 C43 110.6(6) . . ?
C42 N4 C41 109.2(7) . . ?
C40 N4 C41 108.6(7) . . ?
C43 N4 C41 107.0(6) . . ?
C53 N5 C50 110.7(9) . . ?
C53 N5 C52 109.6(9) . . ?
C50 N5 C52 111.6(9) . . ?
C53 N5 C51 108.5(9) . . ?
C50 N5 C51 108.1(8) . . ?
C52 N5 C51 108.3(8) . . ?
C54 N5B C57 110.2(11) . . ?
C54 N5B C55 110.9(11) . . ?
C57 N5B C55 110.3(11) . . ?
C54 N5B C56 109.0(11) . . ?
C57 N5B C56 107.8(11) . . ?
C55 N5B C56 108.6(11) . . ?
C60 N6 C62 109.9(6) . . ?
C60 N6 C61 109.4(6) . . ?
C62 N6 C61 110.4(6) . . ?
C60 N6 C63 108.8(6) . . ?
C62 N6 C63 108.8(6) . . ?
C61 N6 C63 109.5(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1C S1 0.89 2.87 3.416(6) 121.4 .
N1 H1C O24 0.89 2.06 2.864(9) 149.8 .
N1 H1D S2 0.89 2.91 3.452(6) 121.3 .
N1 H1D O26 0.89 1.98 2.775(8) 148.2 .
N1 H1E O23 0.89 2.36 2.971(8) 126.4 .
N1 H1E O8 0.89 2.49 3.090(8) 125.3 .
N2 H2C S2 0.89 2.97 3.562(7) 125.4 .
N2 H2C O9 0.89 2.45 3.277(10) 154.6 .
N2 H2D S3 0.89 2.96 3.548(7) 125.0 .
N2 H2D O19 0.89 2.26 3.063(13) 150.6 .
N2 H2E O8 0.89 2.37 2.906(9) 119.0 .
N2 H2E O18 0.89 2.40 2.916(10) 117.1 .
N3 H3A S1 0.89 2.90 3.485(6) 125.0 .
N3 H3A O25 0.89 2.09 2.911(9) 153.4 .
N3 H3B O23 0.89 2.44 2.998(8) 121.1 .
N3 H3B O18 0.89 2.36 2.870(9) 116.8 .
N3 H3C S3 0.89 2.93 3.519(6) 125.3 .
N3 H3C O17 0.89 2.19 3.003(11) 151.3 .
O28 H28 O17 0.82 2.42 2.864(14) 115.3 2_545
O27 H27 O9 0.82 2.17 2.843(8) 139.3 3
O29B H29B O19 0.82 2.33 2.775(16) 114.8 2

_refine_diff_density_max         1.047
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.128



####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1432061'
_audit_update_record             
;
2016-11-07 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT220_shelx               
;
PROBLEM: Non-Solvent Resd 1   O   Ueq(max)/Ueq(min) Range        6.6 Ratio 
RESPONSE: Poor data quality.
;
# end Validation Reply Form 

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H71 N6 O30 S3 V7'
_chemical_formula_sum            'C28 H71 N6 O30 S3 V7'
_chemical_formula_weight         1424.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_H-M_alt        'I b a m'
_space_group_name_Hall           '-I 2 2c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'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'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'x, y, -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'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'

_cell_length_a                   22.0244(17)
_cell_length_b                   43.315(3)
_cell_length_c                   13.8066(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13171.3(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9887
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      26.41

_exptl_crystal_description       plate
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_F_000             5840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    1.121
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.5767
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46405
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.412
_diffrn_reflns_theta_max         27.884
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8120
_reflns_number_gt                6279
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    Diamond
_computing_publication_material  WINGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0260P)²+277.2604P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8120
_refine_ls_number_parameters     326
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0792
_refine_ls_wR_factor_ref         0.1767
_refine_ls_wR_factor_gt          0.1673
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_restrained_S_all      1.134
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N6 N 0.2022(9) 0.0210(4) 0.5000 0.156(9) Uani 0.74(2) 2 d DS TU P A 1
C61 C 0.1765(11) 0.0064(4) 0.4119(14) 0.165(10) Uani 0.74(2) 1 d D U P A 1
H61A H 0.1935 0.0160 0.3554 0.248 Uiso 0.74(2) 1 calc R U P A 1
H61B H 0.1863 -0.0152 0.4116 0.248 Uiso 0.74(2) 1 calc R U P A 1
H61C H 0.1332 0.0089 0.4116 0.248 Uiso 0.74(2) 1 calc R U P A 1
C62 C 0.1879(14) 0.0547(5) 0.5000 0.165(10) Uani 0.74(2) 2 d DS TU P A 1
H62A H 0.2045 0.0641 0.5571 0.248 Uiso 0.371(10) 1 calc R U P A 1
H62B H 0.2053 0.0642 0.4436 0.248 Uiso 0.371(10) 1 calc R U P A 1
H62C H 0.1446 0.0576 0.4993 0.248 Uiso 0.74(2) 2 calc R U P A 1
C63 C 0.2698(11) 0.0172(6) 0.5000 0.165(10) Uani 0.74(2) 2 d DS TU P A 1
H63A H 0.2865 0.0266 0.5570 0.248 Uiso 0.371(10) 1 calc R U P A 1
H63B H 0.2797 -0.0044 0.4995 0.248 Uiso 0.74(2) 2 calc R U P A 1
H63C H 0.2865 0.0269 0.4435 0.248 Uiso 0.371(10) 1 calc R U P A 1
N6A N 0.2022(9) 0.0210(4) 0.5000 0.156(9) Uani 0.26(2) 2 d DS TU P A 2
C61A C 0.227(3) 0.0533(8) 0.5000 0.165(10) Uani 0.26(2) 2 d DS TU P A 2
H61D H 0.2140 0.0639 0.4425 0.248 Uiso 0.129(10) 1 calc R U P A 2
H61E H 0.2124 0.0642 0.5560 0.248 Uiso 0.129(10) 1 calc R U P A 2
H61F H 0.2706 0.0526 0.5015 0.248 Uiso 0.26(2) 2 calc R U P A 2
C62A C 0.223(2) 0.0049(9) 0.589(3) 0.165(10) Uani 0.26(2) 1 d D U P A 2
H62D H 0.2085 0.0160 0.6449 0.248 Uiso 0.26(2) 1 calc R U P A 2
H62E H 0.2063 -0.0157 0.5899 0.248 Uiso 0.26(2) 1 calc R U P A 2
H62F H 0.2661 0.0039 0.5899 0.248 Uiso 0.26(2) 1 calc R U P A 2
C63A C 0.1342(12) 0.0232(16) 0.5000 0.165(10) Uani 0.26(2) 2 d DS TU P A 2
H63D H 0.1209 0.0336 0.4424 0.248 Uiso 0.129(10) 1 calc R U P A 2
H63E H 0.1171 0.0028 0.5017 0.248 Uiso 0.26(2) 2 calc R U P A 2
H63F H 0.1210 0.0345 0.5559 0.248 Uiso 0.129(10) 1 calc R U P A 2
N2 N 0.2920(3) 0.19415(16) 0.5000 0.0204(14) Uani 1 2 d S T P . .
C9 C 0.2681(4) 0.20972(16) 0.4130(5) 0.047(2) Uani 1 1 d . . . . .
H9A H 0.2835 0.1997 0.3561 0.071 Uiso 1 1 calc R U . . .
H9B H 0.2246 0.2087 0.4131 0.071 Uiso 1 1 calc R U . . .
H9C H 0.2807 0.2309 0.4131 0.071 Uiso 1 1 calc R U . . .
C10 C 0.2741(5) 0.1611(2) 0.5000 0.033(2) Uani 1 2 d S T P . .
H10A H 0.2899 0.1513 0.5569 0.050 Uiso 0.5 1 calc R U P . .
H10B H 0.2306 0.1596 0.4998 0.050 Uiso 1 2 calc R U P . .
H10C H 0.2901 0.1512 0.4433 0.050 Uiso 0.5 1 calc R U P . .
C11 C 0.3594(5) 0.1951(4) 0.5000 0.080(5) Uani 1 2 d S T P . .
H11A H 0.3745 0.1849 0.5569 0.120 Uiso 0.5 1 calc R U P . .
H11B H 0.3745 0.1848 0.4433 0.120 Uiso 0.5 1 calc R U P . .
H11C H 0.3728 0.2162 0.4998 0.120 Uiso 1 2 calc R U P . .
N3 N 0.0000 0.2971(2) 0.2500 0.0359(10) Uani 1 2 d S T P . .
C30 C 0.0544(3) 0.27760(16) 0.2485(5) 0.0359(10) Uani 1 1 d . . . . .
H30A H 0.0900 0.2904 0.2475 0.054 Uiso 1 1 calc R U . . .
H30B H 0.0550 0.2648 0.3053 0.054 Uiso 1 1 calc R U . . .
H30C H 0.0538 0.2648 0.1917 0.054 Uiso 1 1 calc R U . . .
C31 C 0.0023(3) 0.31683(16) 0.3380(5) 0.0359(10) Uani 1 1 d . . . . .
H31A H -0.0330 0.3298 0.3402 0.054 Uiso 1 1 calc R U . . .
H31B H 0.0034 0.3040 0.3946 0.054 Uiso 1 1 calc R U . . .
H31C H 0.0382 0.3295 0.3361 0.054 Uiso 1 1 calc R U . . .
N4 N 0.5000 0.0719(2) 0.2500 0.050(2) Uani 1 2 d S T P . .
C40 C 0.4483(9) 0.0554(4) 0.2342(16) 0.217(9) Uani 1 1 d . . . . .
H40A H 0.4150 0.0693 0.2240 0.325 Uiso 1 1 calc R U . . .
H40B H 0.4535 0.0426 0.1780 0.325 Uiso 1 1 calc R U . . .
H40C H 0.4401 0.0426 0.2895 0.325 Uiso 1 1 calc R U . . .
C41 C 0.5032(10) 0.0932(4) 0.1659(14) 0.217(9) Uani 1 1 d . . . . .
H41A H 0.5388 0.1058 0.1712 0.325 Uiso 1 1 calc R U . . .
H41B H 0.5051 0.0814 0.1071 0.325 Uiso 1 1 calc R U . . .
H41C H 0.4677 0.1060 0.1649 0.325 Uiso 1 1 calc R U . . .
O4 O 0.34502(15) -0.16803(8) 0.4015(2) 0.0127(7) Uani 1 1 d . . . . .
O2 O 0.34774(18) -0.11105(9) 0.4121(3) 0.0218(8) Uani 1 1 d . . . . .
O13 O 0.24880(16) -0.16447(8) 0.2968(2) 0.0138(7) Uani 1 1 d . . . . .
O8 O 0.19886(15) -0.21582(8) 0.3887(2) 0.0114(7) Uani 1 1 d . . . . .
O10 O 0.0980(2) -0.22469(12) 0.5000 0.0139(10) Uani 1 2 d S T P . .
O7 O 0.2254(2) -0.16826(12) 0.5000 0.0138(10) Uani 1 2 d S T P . .
O6 O 0.31043(15) -0.22220(8) 0.2986(3) 0.0155(7) Uani 1 1 d . . . . .
O5 O 0.3023(2) -0.21999(12) 0.5000 0.0123(10) Uani 1 2 d S T P . .
O1 O 0.3732(4) -0.05261(16) 0.5000 0.057(2) Uani 1 2 d S T P . .
O3 O 0.4439(2) -0.14312(13) 0.5000 0.0210(12) Uani 1 2 d S T P . .
O11 O 0.00851(17) -0.21087(9) 0.4123(3) 0.0228(9) Uani 1 1 d . . . . .
O15 O 0.36291(18) -0.13935(10) 0.2177(3) 0.0279(10) Uani 1 1 d . . . . .
O12 O 0.0130(2) -0.25934(12) 0.5000 0.0200(12) Uani 1 2 d S T P . .
N1 N 0.11613(19) -0.16972(9) 0.3901(3) 0.0119(8) Uani 1 1 d . . . . .
O14 O 0.2593(2) -0.10280(10) 0.2741(3) 0.0346(11) Uani 1 1 d . . . . .
C5 C 0.1086(3) -0.13598(13) 0.4060(4) 0.0220(12) Uani 1 1 d . . . . .
H5A H 0.0866 -0.1271 0.3520 0.026 Uiso 1 1 calc R U . . .
H5B H 0.1482 -0.1263 0.4089 0.026 Uiso 1 1 calc R U . . .
C3 C 0.1903(2) -0.15920(12) 0.2529(4) 0.0141(5) Uani 1 1 d . . . . .
H3A H 0.1939 -0.1625 0.1836 0.017 Uiso 1 1 calc R U . . .
H3B H 0.1791 -0.1378 0.2628 0.017 Uiso 1 1 calc R U . . .
C2 C 0.1593(2) -0.21302(12) 0.3054(4) 0.0141(5) Uani 1 1 d . . . . .
H2A H 0.1237 -0.2259 0.3145 0.017 Uiso 1 1 calc R U . . .
H2B H 0.1804 -0.2202 0.2480 0.017 Uiso 1 1 calc R U . . .
C4 C 0.0869(2) -0.17789(12) 0.2195(3) 0.0141(5) Uani 1 1 d . . . . .
H4A H 0.0525 -0.1893 0.2448 0.017 Uiso 1 1 calc R U . . .
H4B H 0.0745 -0.1566 0.2107 0.017 Uiso 1 1 calc R U . . .
C1 C 0.1398(2) -0.17949(12) 0.2913(4) 0.0141(5) Uani 1 1 d . . . . .
C6 C 0.0742(4) -0.12961(18) 0.5000 0.0239(18) Uani 1 2 d S T P . .
H6A H 0.0618 -0.1081 0.5000 0.029 Uiso 1 2 calc R U P . .
H6B H 0.0375 -0.1420 0.5000 0.029 Uiso 1 2 calc R U P . .
S1 S 0.25706(10) -0.06947(4) 0.29662(13) 0.0400(4) Uani 1 1 d . . . . .
O9 O 0.10496(17) -0.19061(10) 0.1289(3) 0.0237(9) Uani 1 1 d . . . . .
H9 H 0.0765 -0.1897 0.0907 0.036 Uiso 1 1 calc R U . . .
O16 O 0.2589(3) -0.06607(12) 0.4045(4) 0.0497(14) Uani 1 1 d . . . . .
O17 O 0.1987(3) -0.05805(15) 0.2644(5) 0.075(2) Uani 1 1 d . . . . .
O18 O 0.3072(3) -0.05388(12) 0.2533(5) 0.073(2) Uani 1 1 d . . . . .
C12 C 0.3621(3) -0.23458(19) 0.5000 0.0176(16) Uani 1 2 d S T P . .
H12A H 0.3690 -0.2442 0.4384 0.026 Uiso 0.5 1 calc R U P . .
H12B H 0.3927 -0.2192 0.5113 0.026 Uiso 0.5 1 calc R U P . .
H12C H 0.3637 -0.2499 0.5503 0.026 Uiso 0.5 1 calc R U P . .
V1 V 0.28159(4) -0.19884(2) 0.37546(6) 0.01024(18) Uani 1 1 d . . . . .
V2 V 0.16665(5) -0.19181(3) 0.5000 0.0097(2) Uani 1 2 d S T P . .
V3 V 0.37173(6) -0.14264(3) 0.5000 0.0144(3) Uani 1 2 d S T P . .
V4 V 0.31745(4) -0.13639(2) 0.30792(6) 0.0162(2) Uani 1 1 d . . . . .
V5 V 0.32266(8) -0.07822(3) 0.5000 0.0310(4) Uani 1 2 d S T P . .
S2 S 0.03004(8) -0.22692(4) 0.5000 0.0131(4) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N6 C61 1.483(15) . ?
N6 C61 1.483(15) 10_556 ?
N6 C62 1.496(17) . ?
N6 C63 1.499(17) . ?
N6A C62A 1.483(18) . ?
N6A C62A 1.483(18) 10_556 ?
N6A C63A 1.501(19) . ?
N6A C61A 1.506(19) . ?
N2 C9 1.475(7) . ?
N2 C9 1.475(7) 10_556 ?
N2 C10 1.483(10) . ?
N2 C11 1.485(12) . ?
N3 C30 1.467(8) . ?
N3 C30 1.467(8) 4 ?
N3 C31 1.485(8) . ?
N3 C31 1.486(8) 4 ?
N4 C40 1.361(14) . ?
N4 C40 1.361(14) 4_655 ?
N4 C41 1.485(17) . ?
N4 C41 1.485(17) 4_655 ?
O4 V3 1.845(3) . ?
O4 V1 1.965(3) . ?
O4 V4 1.979(4) . ?
O2 V3 1.904(4) . ?
O2 V4 1.929(4) . ?
O2 V5 1.949(4) . ?
O13 C3 1.442(6) . ?
O13 V4 1.946(4) . ?
O13 V1 1.979(4) . ?
O8 C2 1.448(6) . ?
O8 V1 1.973(3) . ?
O8 V2 1.987(3) . ?
O10 S2 1.500(5) . ?
O10 V2 2.077(5) . ?
O7 V2 1.648(5) . ?
O6 V1 1.597(3) . ?
O5 C12 1.460(8) . ?
O5 V1 2.001(3) 10_556 ?
O5 V1 2.001(3) . ?
O1 V5 1.571(8) . ?
O3 V3 1.590(6) . ?
O11 S2 1.474(4) . ?
O15 V4 1.603(4) . ?
O12 S2 1.453(6) . ?
N1 C5 1.487(7) . ?
N1 C1 1.521(6) . ?
N1 V2 2.111(4) . ?
O14 S1 1.478(5) . ?
O14 V4 1.993(5) . ?
C5 C6 1.528(7) . ?
C3 C1 1.513(7) . ?
C2 C1 1.527(7) . ?
C4 O9 1.423(6) . ?
C4 C1 1.532(7) . ?
C6 C5 1.528(7) 10_556 ?
S1 O18 1.426(6) . ?
S1 O17 1.447(6) . ?
S1 O16 1.498(5) . ?
O16 V5 1.997(5) . ?
V1 V4 2.9685(12) . ?
V1 V2 3.0754(13) . ?
V2 O8 1.986(3) 10_556 ?
V2 N1 2.111(4) 10_556 ?
V2 V1 3.0754(13) 10_556 ?
V3 O4 1.845(3) 10_556 ?
V3 O2 1.904(4) 10_556 ?
V3 V4 2.9216(10) . ?
V3 V4 2.9217(10) 10_556 ?
V3 V5 2.992(2) . ?
V5 O2 1.949(4) 10_556 ?
V5 O16 1.997(5) 10_556 ?
S2 O11 1.474(4) 10_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C61 N6 C61 110(2) . 10_556 ?
C61 N6 C62 109.7(9) . . ?
C61 N6 C62 109.7(9) 10_556 . ?
C61 N6 C63 109.4(10) . . ?
C61 N6 C63 109.4(10) 10_556 . ?
C62 N6 C63 108.5(12) . . ?
C62A N6A C62A 112(4) . 10_556 ?
C62A N6A C63A 109.4(13) . . ?
C62A N6A C63A 109.4(13) 10_556 . ?
C62A N6A C61A 109.1(12) . . ?
C62A N6A C61A 109.1(12) 10_556 . ?
C63A N6A C61A 107.7(13) . . ?
C9 N2 C9 109.1(8) . 10_556 ?
C9 N2 C10 110.2(5) . . ?
C9 N2 C10 110.2(5) 10_556 . ?
C9 N2 C11 110.2(6) . . ?
C9 N2 C11 110.2(6) 10_556 . ?
C10 N2 C11 107.0(9) . . ?
C30 N3 C30 109.5(8) . 4 ?
C30 N3 C31 108.3(4) . . ?
C30 N3 C31 110.4(4) 4 . ?
C30 N3 C31 110.4(4) . 4 ?
C30 N3 C31 108.3(4) 4 4 ?
C31 N3 C31 109.9(7) . 4 ?
C40 N4 C40 117(2) . 4_655 ?
C40 N4 C41 103.9(10) . . ?
C40 N4 C41 114.3(14) 4_655 . ?
C40 N4 C41 114.3(14) . 4_655 ?
C40 N4 C41 103.9(10) 4_655 4_655 ?
C41 N4 C41 103.2(17) . 4_655 ?
V3 O4 V1 140.02(19) . . ?
V3 O4 V4 99.57(16) . . ?
V1 O4 V4 97.62(15) . . ?
V3 O2 V4 99.34(18) . . ?
V3 O2 V5 101.89(18) . . ?
V4 O2 V5 141.4(2) . . ?
C3 O13 V4 128.9(3) . . ?
C3 O13 V1 132.5(3) . . ?
V4 O13 V1 98.26(15) . . ?
C2 O8 V1 116.8(3) . . ?
C2 O8 V2 110.9(3) . . ?
V1 O8 V2 101.91(15) . . ?
S2 O10 V2 140.4(3) . . ?
C12 O5 V1 113.79(19) . 10_556 ?
C12 O5 V1 113.79(19) . . ?
V1 O5 V1 118.5(2) 10_556 . ?
C5 N1 C1 116.4(4) . . ?
C5 N1 V2 113.5(3) . . ?
C1 N1 V2 109.7(3) . . ?
S1 O14 V4 133.3(3) . . ?
N1 C5 C6 111.0(5) . . ?
O13 C3 C1 114.7(4) . . ?
O8 C2 C1 110.5(4) . . ?
O9 C4 C1 109.8(4) . . ?
C3 C1 N1 113.9(4) . . ?
C3 C1 C2 113.0(4) . . ?
N1 C1 C2 104.3(4) . . ?
C3 C1 C4 107.8(4) . . ?
N1 C1 C4 107.9(4) . . ?
C2 C1 C4 109.9(4) . . ?
C5 C6 C5 116.3(7) 10_556 . ?
O18 S1 O17 113.4(4) . . ?
O18 S1 O14 110.4(4) . . ?
O17 S1 O14 107.4(3) . . ?
O18 S1 O16 110.5(4) . . ?
O17 S1 O16 107.2(4) . . ?
O14 S1 O16 107.7(3) . . ?
S1 O16 V5 130.5(3) . . ?
O6 V1 O4 105.60(17) . . ?
O6 V1 O8 101.11(16) . . ?
O4 V1 O8 153.18(15) . . ?
O6 V1 O13 104.92(17) . . ?
O4 V1 O13 81.30(14) . . ?
O8 V1 O13 89.67(14) . . ?
O6 V1 O5 100.96(18) . . ?
O4 V1 O5 89.53(18) . . ?
O8 V1 O5 87.71(17) . . ?
O13 V1 O5 154.01(16) . . ?
O6 V1 V4 105.23(14) . . ?
O4 V1 V4 41.36(10) . . ?
O8 V1 V4 127.90(10) . . ?
O13 V1 V4 40.46(10) . . ?
O5 V1 V4 128.80(14) . . ?
O6 V1 V2 139.58(14) . . ?
O4 V1 V2 114.55(11) . . ?
O8 V1 V2 39.20(10) . . ?
O13 V1 V2 86.09(11) . . ?
O5 V1 V2 75.66(13) . . ?
V4 V1 V2 107.72(4) . . ?
O7 V2 O8 92.49(15) . 10_556 ?
O7 V2 O8 92.49(15) . . ?
O8 V2 O8 101.3(2) 10_556 . ?
O7 V2 O10 174.9(2) . . ?
O8 V2 O10 84.31(14) 10_556 . ?
O8 V2 O10 84.31(14) . . ?
O7 V2 N1 97.67(17) . 10_556 ?
O8 V2 N1 82.51(15) 10_556 10_556 ?
O8 V2 N1 168.99(16) . 10_556 ?
O10 V2 N1 85.83(15) . 10_556 ?
O7 V2 N1 97.67(17) . . ?
O8 V2 N1 168.99(16) 10_556 . ?
O8 V2 N1 82.51(15) . . ?
O10 V2 N1 85.83(15) . . ?
N1 V2 N1 91.9(2) 10_556 . ?
O7 V2 V1 54.18(13) . . ?
O8 V2 V1 94.97(10) 10_556 . ?
O8 V2 V1 38.89(10) . . ?
O10 V2 V1 122.08(11) . . ?
N1 V2 V1 151.72(12) 10_556 . ?
N1 V2 V1 94.41(11) . . ?
O7 V2 V1 54.18(13) . 10_556 ?
O8 V2 V1 38.89(10) 10_556 10_556 ?
O8 V2 V1 94.97(10) . 10_556 ?
O10 V2 V1 122.08(11) . 10_556 ?
N1 V2 V1 94.41(11) 10_556 10_556 ?
N1 V2 V1 151.73(12) . 10_556 ?
V1 V2 V1 67.99(4) . 10_556 ?
O3 V3 O4 108.12(18) . . ?
O3 V3 O4 108.12(18) . 10_556 ?
O4 V3 O4 94.9(2) . 10_556 ?
O3 V3 O2 106.7(2) . 10_556 ?
O4 V3 O2 144.07(18) . 10_556 ?
O4 V3 O2 82.54(15) 10_556 10_556 ?
O3 V3 O2 106.7(2) . . ?
O4 V3 O2 82.54(15) . . ?
O4 V3 O2 144.07(18) 10_556 . ?
O2 V3 O2 79.2(2) 10_556 . ?
O3 V3 V4 114.23(4) . . ?
O4 V3 V4 41.91(11) . . ?
O4 V3 V4 126.42(11) 10_556 . ?
O2 V3 V4 113.48(13) 10_556 . ?
O2 V3 V4 40.64(11) . . ?
O3 V3 V4 114.23(4) . 10_556 ?
O4 V3 V4 126.42(11) . 10_556 ?
O4 V3 V4 41.91(11) 10_556 10_556 ?
O2 V3 V4 40.64(11) 10_556 10_556 ?
O2 V3 V4 113.48(13) . 10_556 ?
V4 V3 V4 130.38(6) . 10_556 ?
O3 V3 V5 111.9(2) . . ?
O4 V3 V5 116.15(12) . . ?
O4 V3 V5 116.15(12) 10_556 . ?
O2 V3 V5 39.60(12) 10_556 . ?
O2 V3 V5 39.60(12) . . ?
V4 V3 V5 76.46(3) . . ?
V4 V3 V5 76.46(3) 10_556 . ?
O15 V4 O2 114.14(19) . . ?
O15 V4 O13 111.96(18) . . ?
O2 V4 O13 133.08(16) . . ?
O15 V4 O4 105.08(19) . . ?
O2 V4 O4 78.52(15) . . ?
O13 V4 O4 81.78(14) . . ?
O15 V4 O14 106.1(2) . . ?
O2 V4 O14 88.94(18) . . ?
O13 V4 O14 86.49(16) . . ?
O4 V4 O14 148.81(18) . . ?
O15 V4 V3 116.24(15) . . ?
O2 V4 V3 40.01(12) . . ?
O13 V4 V3 109.35(11) . . ?
O4 V4 V3 38.52(10) . . ?
O14 V4 V3 122.89(14) . . ?
O15 V4 V1 109.71(17) . . ?
O2 V4 V1 112.11(12) . . ?
O13 V4 V1 41.29(10) . . ?
O4 V4 V1 41.01(10) . . ?
O14 V4 V1 124.60(13) . . ?
V3 V4 V1 74.89(4) . . ?
O1 V5 O2 108.3(3) . . ?
O1 V5 O2 108.3(3) . 10_556 ?
O2 V5 O2 77.0(2) . 10_556 ?
O1 V5 O16 108.2(3) . . ?
O2 V5 O16 88.89(19) . . ?
O2 V5 O16 143.4(2) 10_556 . ?
O1 V5 O16 108.2(3) . 10_556 ?
O2 V5 O16 143.4(2) . 10_556 ?
O2 V5 O16 88.89(19) 10_556 10_556 ?
O16 V5 O16 82.6(3) . 10_556 ?
O1 V5 V3 113.7(4) . . ?
O2 V5 V3 38.50(12) . . ?
O2 V5 V3 38.50(12) 10_556 . ?
O16 V5 V3 119.99(16) . . ?
O16 V5 V3 119.99(16) 10_556 . ?
O12 S2 O11 111.9(2) . 10_556 ?
O12 S2 O11 111.9(2) . . ?
O11 S2 O11 110.4(3) 10_556 . ?
O12 S2 O10 108.6(3) . . ?
O11 S2 O10 106.9(2) 10_556 . ?
O11 S2 O10 106.9(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9 O11 0.82 2.09 2.709(5) 132.7 4

_refine_diff_density_max         2.245
_refine_diff_density_min         -1.534
_refine_diff_density_rms         0.142



####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1432062'
_audit_update_record             
;
2016-11-07 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H26 N2 O20 S2 V4, 4 (C O H4)'
_chemical_formula_sum            'C14 H42 N2 O24 S2 V4'
_chemical_formula_weight         890.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.9167(5)
_cell_length_b                   8.5362(4)
_cell_length_c                   17.1702(8)
_cell_angle_alpha                90
_cell_angle_beta                 97.2180(10)
_cell_angle_gamma                90
_cell_volume                     1587.36(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9922
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.10

_exptl_crystal_description       hexagon
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_F_000             912
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    1.370
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.6916
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18803
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.391
_diffrn_reflns_theta_max         27.120
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3483
_reflns_number_gt                3033
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    WINGX
_computing_publication_material  DIAMOND
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0379P)²+5.1857P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3483
_refine_ls_number_parameters     218
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.0978
_refine_ls_wR_factor_gt          0.0931
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      2.989
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.09325(4) 0.84419(5) 0.02934(3) 0.00924(13) Uani 1 1 d . . . . .
V2 V 0.19139(4) 1.13422(5) -0.06521(3) 0.00978(13) Uani 1 1 d . . . . .
S1 S 0.02219(6) 0.74199(8) 0.19970(4) 0.01052(15) Uani 1 1 d . . . . .
O8 O 0.03467(17) 0.9595(2) -0.06941(10) 0.0107(4) Uani 1 1 d . . . . .
O6 O -0.06806(17) 0.7351(2) 0.01987(10) 0.0108(4) Uani 1 1 d . . . . .
O7 O 0.21453(17) 1.0208(2) 0.03780(10) 0.0102(4) Uani 1 1 d . . . . .
O5 O 0.17768(18) 0.7061(2) 0.00275(12) 0.0149(4) Uani 1 1 d . . . . .
O9 O 0.27489(18) 0.9588(2) -0.11995(11) 0.0142(4) Uani 1 1 d . . . . .
H9 H 0.2342 0.9133 -0.1652 0.017 Uiso 1 1 calc R U . . .
O10 O 0.30717(18) 1.2494(2) -0.05323(12) 0.0161(4) Uani 1 1 d . . . . .
O1 O 0.01870(19) 0.5714(2) 0.19623(12) 0.0173(4) Uani 1 1 d . . . . .
O2 O 0.06156(18) 0.8012(3) 0.27768(11) 0.0159(4) Uani 1 1 d . . . . .
O4 O 0.11046(17) 0.8038(2) 0.14616(11) 0.0123(4) Uani 1 1 d . . . . .
O3 O 0.10415(17) 1.1940(2) -0.17242(11) 0.0126(4) Uani 1 1 d . . . . .
N1 N 0.1738(2) 1.3135(3) 0.19361(13) 0.0135(5) Uani 1 1 d . . . . .
H1A H 0.1249 1.3963 0.1962 0.020 Uiso 1 1 calc R U . . .
H1B H 0.2512 1.3454 0.1930 0.020 Uiso 1 1 calc R U . . .
H1C H 0.1695 1.2524 0.2352 0.020 Uiso 1 1 calc R U . . .
C4 C 0.2396(2) 1.1120(3) 0.10765(15) 0.0117(5) Uani 1 1 d . . . . .
H4A H 0.3137 1.1734 0.1050 0.014 Uiso 1 1 calc R U . . .
H4B H 0.2549 1.0423 0.1524 0.014 Uiso 1 1 calc R U . . .
C3 C 0.1324(2) 1.2226(3) 0.11981(15) 0.0116(5) Uani 1 1 d . . . . .
C1 C -0.1077(3) 0.6583(3) -0.05284(16) 0.0124(5) Uani 1 1 d . . . . .
H1D H -0.1825 0.5995 -0.0483 0.015 Uiso 1 1 calc R U . . .
H1E H -0.0446 0.5851 -0.0646 0.015 Uiso 1 1 calc R U . . .
C2 C -0.0136(3) 0.8639(3) -0.13471(15) 0.0119(5) Uani 1 1 d . . . . .
H2A H 0.0483 0.7876 -0.1450 0.014 Uiso 1 1 calc R U . . .
H2B H -0.0311 0.9292 -0.1810 0.014 Uiso 1 1 calc R U . . .
C5 C 0.3964(3) 0.9049(4) -0.08887(18) 0.0216(7) Uani 1 1 d . . . . .
H5A H 0.4215 0.8227 -0.1216 0.032 Uiso 1 1 calc R U . . .
H5B H 0.4538 0.9903 -0.0878 0.032 Uiso 1 1 calc R U . . .
H5C H 0.3949 0.8660 -0.0366 0.032 Uiso 1 1 calc R U . . .
O21 O 0.3271(2) 0.6228(3) 0.17058(13) 0.0255(5) Uani 1 1 d . . . . .
H21 H 0.2657 0.6610 0.1451 0.038 Uiso 1 1 calc R U . . .
C21 C 0.4294(3) 0.6287(5) 0.1249(2) 0.0384(10) Uani 1 1 d . . . . .
H21A H 0.4504 0.5244 0.1105 0.058 Uiso 1 1 calc R U . . .
H21B H 0.4993 0.6761 0.1556 0.058 Uiso 1 1 calc R U . . .
H21C H 0.4066 0.6896 0.0784 0.058 Uiso 1 1 calc DR U . . .
O20A O 0.2295(3) 0.9199(4) -0.26972(19) 0.0176(6) Uani 0.6 1 d . . P A 1
H20A H 0.2680 0.8466 -0.2857 0.026 Uiso 0.6 1 calc R U P A 1
C20A C 0.2354(3) 1.0501(4) -0.3196(2) 0.0282(7) Uani 0.6 1 d . . P A 1
H20B H 0.1728 1.1244 -0.3104 0.042 Uiso 0.6 1 calc R U P A 1
H20C H 0.2222 1.0163 -0.3733 0.042 Uiso 0.6 1 calc R U P A 1
H20D H 0.3152 1.0984 -0.3090 0.042 Uiso 0.6 1 calc R U P A 1
O20B O 0.3189(5) 1.0647(6) -0.2558(3) 0.0176(6) Uani 0.4 1 d . . P B 2
H20E H 0.3845 1.0258 -0.2645 0.026 Uiso 0.4 1 calc R U P B 2
C20B C 0.2354(3) 1.0501(4) -0.3196(2) 0.0282(7) Uani 0.4 1 d . . P B 2
H20F H 0.2372 1.1419 -0.3518 0.042 Uiso 0.4 1 calc DR U P B 2
H20G H 0.1546 1.0386 -0.3038 0.042 Uiso 0.4 1 calc R U P B 2
H20H H 0.2545 0.9595 -0.3489 0.042 Uiso 0.4 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O5 1.598(2) . ?
V1 O6 1.9804(19) . ?
V1 O8 1.9951(19) . ?
V1 O7 1.9998(19) . ?
V1 O4 2.0205(19) . ?
V1 O8 2.3393(19) 3_575 ?
V2 O10 1.594(2) . ?
V2 O6 1.9814(19) 3_575 ?
V2 O7 2.0041(19) . ?
V2 O3 2.0285(19) . ?
V2 O9 2.043(2) . ?
V2 O8 2.264(2) . ?
S1 O2 1.445(2) . ?
S1 O1 1.458(2) . ?
S1 O3 1.5027(19) 3_575 ?
S1 O4 1.5084(19) . ?
O8 C2 1.433(3) . ?
O8 V1 2.3393(19) 3_575 ?
O6 C1 1.428(3) . ?
O6 V2 1.9814(19) 3_575 ?
O7 C4 1.427(3) . ?
O9 C5 1.441(3) . ?
O3 S1 1.5027(19) 3_575 ?
N1 C3 1.506(3) . ?
C4 C3 1.538(4) . ?
C3 C1 1.533(4) 3_575 ?
C3 C2 1.541(4) 3_575 ?
C1 C3 1.533(4) 3_575 ?
C2 C3 1.541(4) 3_575 ?
O21 C21 1.444(4) . ?
O20A C20A 1.410(5) . ?
O20B C20B 1.340(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 V1 O6 99.70(9) . . ?
O5 V1 O8 104.84(9) . . ?
O6 V1 O8 88.59(8) . . ?
O5 V1 O7 100.18(9) . . ?
O6 V1 O7 159.09(8) . . ?
O8 V1 O7 80.11(8) . . ?
O5 V1 O4 99.95(9) . . ?
O6 V1 O4 88.41(8) . . ?
O8 V1 O4 155.18(8) . . ?
O7 V1 O4 94.49(8) . . ?
O5 V1 O8 178.20(9) . 3_575 ?
O6 V1 O8 78.66(7) . 3_575 ?
O8 V1 O8 75.94(8) . 3_575 ?
O7 V1 O8 81.54(7) . 3_575 ?
O4 V1 O8 79.31(7) . 3_575 ?
O10 V2 O6 99.73(9) . 3_575 ?
O10 V2 O7 100.02(9) . . ?
O6 V2 O7 86.65(8) 3_575 . ?
O10 V2 O3 103.67(9) . . ?
O6 V2 O3 87.15(8) 3_575 . ?
O7 V2 O3 156.21(8) . . ?
O10 V2 O9 96.84(9) . . ?
O6 V2 O9 163.34(8) 3_575 . ?
O7 V2 O9 92.17(8) . . ?
O3 V2 O9 87.29(8) . . ?
O10 V2 O8 173.80(9) . . ?
O6 V2 O8 80.51(7) 3_575 . ?
O7 V2 O8 73.80(7) . . ?
O3 V2 O8 82.53(7) . . ?
O9 V2 O8 83.20(7) . . ?
O2 S1 O1 113.00(13) . . ?
O2 S1 O3 108.43(12) . 3_575 ?
O1 S1 O3 109.42(12) . 3_575 ?
O2 S1 O4 107.68(12) . . ?
O1 S1 O4 109.89(12) . . ?
O3 S1 O4 108.31(11) 3_575 . ?
C2 O8 V1 115.52(16) . . ?
C2 O8 V2 127.05(16) . . ?
V1 O8 V2 97.92(8) . . ?
C2 O8 V1 117.63(15) . 3_575 ?
V1 O8 V1 104.06(8) . 3_575 ?
V2 O8 V1 89.74(7) . 3_575 ?
C1 O6 V1 117.14(16) . . ?
C1 O6 V2 117.11(16) . 3_575 ?
V1 O6 V2 110.13(9) . 3_575 ?
C4 O7 V1 121.82(16) . . ?
C4 O7 V2 117.90(16) . . ?
V1 O7 V2 106.93(8) . . ?
C5 O9 V2 120.43(17) . . ?
S1 O4 V1 132.68(12) . . ?
S1 O3 V2 133.02(12) 3_575 . ?
O7 C4 C3 112.4(2) . . ?
N1 C3 C1 107.2(2) . 3_575 ?
N1 C3 C4 106.1(2) . . ?
C1 C3 C4 111.7(2) 3_575 . ?
N1 C3 C2 106.0(2) . 3_575 ?
C1 C3 C2 111.7(2) 3_575 3_575 ?
C4 C3 C2 113.5(2) . 3_575 ?
O6 C1 C3 110.9(2) . 3_575 ?
O8 C2 C3 112.2(2) . 3_575 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O1 0.89 1.89 2.780(3) 177.1 1_565
N1 H1B S1 0.89 3.02 3.636(2) 127.6 2
N1 H1B O2 0.89 2.08 2.871(3) 148.1 2
N1 H1B O21 0.89 2.55 3.178(4) 127.8 1_565
N1 H1C O21 0.89 1.96 2.845(3) 175.7 2
O21 H21 S1 0.82 3.01 3.575(2) 128.4 .
O21 H21 O5 0.82 2.54 3.207(3) 139.2 .
O21 H21 O4 0.82 2.09 2.812(3) 146.8 .
O20A H20A S1 0.82 2.92 3.580(3) 139.4 4_675
O20A H20A O3 0.82 2.10 2.908(4) 168.0 2_544
O20B H20E S1 0.82 2.85 3.576(5) 149.5 4_675
O20B H20E O1 0.82 1.88 2.690(5) 169.0 4_675
O9 H9 O20A 0.93 1.79 2.579(4) 140.9 .
O9 H9 O20B 0.93 2.30 2.602(5) 98.1 .

_refine_diff_density_max         1.384
_refine_diff_density_min         -1.733
_refine_diff_density_rms         0.102

