# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_b351
_database_code_depnum_ccdc_archive 'CCDC 1040912'
_audit_update_record             
;
2014-12-24 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H8 K2 O15 P2 V2'
_chemical_formula_weight         514.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   17.749(15)
_cell_length_b                   6.370(4)
_cell_length_c                   13.977(9)
_cell_angle_alpha                90
_cell_angle_beta                 115.421(13)
_cell_angle_gamma                90
_cell_volume                     1427.2(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    1789
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      27.41

_exptl_crystal_description       Block
_exptl_crystal_colour            Blue
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.393
_exptl_crystal_F_000             1016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    2.196
_shelx_estimated_absorpt_T_min   0.644
_shelx_estimated_absorpt_T_max   0.880
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6244
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2010)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4750
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.541
_diffrn_reflns_theta_max         27.493
_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             1638
_reflns_number_gt                1444
_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0617P)²+9.5285P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1638
_refine_ls_number_parameters     119
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.1212
_refine_ls_wR_factor_gt          0.1170
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.024
_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
K1 K 0.91454(5) 0.25619(15) 0.95035(7) 0.0257(2) Uani 1 1 d D . . . .
V1 V 0.67213(4) 0.08686(9) 0.79133(5) 0.01165(19) Uani 1 1 d . . . . .
P1 P 0.70650(6) 0.58255(13) 0.82388(7) 0.0125(2) Uani 1 1 d . . . . .
H1 H 0.720(3) 0.582(7) 0.921(4) 0.022(12) Uiso 1 1 d . . . . .
C1 C 0.4846(2) 0.0777(5) 0.6899(3) 0.0122(7) Uani 1 1 d . . . . .
O1 O 0.53948(16) 0.0772(4) 0.6562(2) 0.0162(5) Uani 1 1 d . . . . .
O2 O 0.40699(16) 0.0825(4) 0.6350(2) 0.0174(5) Uani 1 1 d . . . . .
O3 O 0.65704(17) 0.7781(4) 0.7734(2) 0.0233(6) Uani 1 1 d . . . . .
O4 O 0.65241(17) 0.3960(4) 0.7685(2) 0.0224(6) Uani 1 1 d . . . . .
O5 O 0.79302(16) 0.5797(4) 0.8262(2) 0.0185(6) Uani 1 1 d . . . . .
O6 O 0.75734(17) 0.0946(4) 0.8956(2) 0.0232(6) Uani 1 1 d . . . . .
O7 O 1.0772(2) 0.1648(7) 0.9908(4) 0.0465(9) Uani 1 1 d D . . . .
H7A H 1.110(3) 0.251(7) 1.036(4) 0.056 Uiso 1 1 d D U . . .
H7B H 1.078(3) 0.115(10) 0.934(6) 0.056 Uiso 1 1 d D U . . .
O1W O 0.5000 0.5940(13) 0.7500 0.106(4) Uani 1 2 d DS T P . .
H1W H 0.543(4) 0.538(14) 0.747(9) 0.127 Uiso 1 1 d 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
K1 O7 2.755(5) . ?
K1 O6 2.756(4) . ?
K1 O7 2.790(5) 5_757 ?
K1 O3 2.829(4) 4_646 ?
K1 O2 2.834(3) 8_556 ?
K1 O1 2.848(3) 4_656 ?
K1 O5 2.949(3) . ?
K1 O1 2.974(3) 8_556 ?
K1 C1 3.210(4) 8_556 ?
K1 P1 3.669(2) 4_646 ?
K1 V1 3.708(2) 4_656 ?
K1 V1 4.050(3) . ?
V1 O6 1.588(3) . ?
V1 O3 1.986(3) 1_545 ?
V1 O5 1.989(3) 4_646 ?
V1 O4 2.001(3) . ?
V1 O2 2.068(3) 2_656 ?
V1 O1 2.301(3) . ?
V1 K1 3.708(2) 4_646 ?
P1 O3 1.513(3) . ?
P1 O4 1.515(3) . ?
P1 O5 1.522(3) . ?
P1 K1 3.669(2) 4_656 ?
C1 O1 1.250(4) . ?
C1 O2 1.257(4) . ?
C1 C1 1.527(7) 2_656 ?
C1 K1 3.210(4) 8_455 ?
O1 K1 2.848(3) 4_646 ?
O1 K1 2.974(3) 8_455 ?
O2 V1 2.068(3) 2_656 ?
O2 K1 2.834(3) 8_455 ?
O3 V1 1.986(3) 1_565 ?
O3 K1 2.829(4) 4_656 ?
O5 V1 1.989(3) 4_656 ?
O7 K1 2.790(5) 5_757 ?

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
O7 K1 O6 145.55(12) . . ?
O7 K1 O7 79.54(14) . 5_757 ?
O6 K1 O7 69.02(10) . 5_757 ?
O7 K1 O3 99.83(11) . 4_646 ?
O6 K1 O3 77.92(9) . 4_646 ?
O7 K1 O3 108.38(11) 5_757 4_646 ?
O7 K1 O2 110.17(11) . 8_556 ?
O6 K1 O2 87.16(9) . 8_556 ?
O7 K1 O2 95.56(11) 5_757 8_556 ?
O3 K1 O2 144.54(9) 4_646 8_556 ?
O7 K1 O1 75.44(11) . 4_656 ?
O6 K1 O1 127.31(9) . 4_656 ?
O7 K1 O1 148.61(11) 5_757 4_656 ?
O3 K1 O1 58.65(8) 4_646 4_656 ?
O2 K1 O1 110.63(9) 8_556 4_656 ?
O7 K1 O5 134.88(11) . . ?
O6 K1 O5 72.54(9) . . ?
O7 K1 O5 141.06(10) 5_757 . ?
O3 K1 O5 56.44(8) 4_646 . ?
O2 K1 O5 88.51(9) 8_556 . ?
O1 K1 O5 59.47(9) 4_656 . ?
O7 K1 O1 66.21(11) . 8_556 ?
O6 K1 O1 130.35(9) . 8_556 ?
O7 K1 O1 97.73(11) 5_757 8_556 ?
O3 K1 O1 147.83(8) 4_646 8_556 ?
O2 K1 O1 45.29(8) 8_556 8_556 ?
O1 K1 O1 89.31(9) 4_656 8_556 ?
O5 K1 O1 111.91(9) . 8_556 ?
O7 K1 C1 87.31(12) . 8_556 ?
O6 K1 C1 107.80(9) . 8_556 ?
O7 K1 C1 93.50(11) 5_757 8_556 ?
O3 K1 C1 157.83(9) 4_646 8_556 ?
O2 K1 C1 22.94(8) 8_556 8_556 ?
O1 K1 C1 103.85(9) 4_656 8_556 ?
O5 K1 C1 103.98(9) . 8_556 ?
O1 K1 C1 22.92(8) 8_556 8_556 ?
O7 K1 P1 104.04(10) . 4_646 ?
O6 K1 P1 61.85(7) . 4_646 ?
O7 K1 P1 87.22(10) 5_757 4_646 ?
O3 K1 P1 22.52(6) 4_646 4_646 ?
O2 K1 P1 145.62(7) 8_556 4_646 ?
O1 K1 P1 80.83(7) 4_656 4_646 ?
O5 K1 P1 69.12(7) . 4_646 ?
O1 K1 P1 167.79(6) 8_556 4_646 ?
C1 K1 P1 168.56(7) 8_556 4_646 ?
O7 K1 V1 107.17(10) . 4_656 ?
O6 K1 V1 89.11(7) . 4_656 ?
O7 K1 V1 139.76(10) 5_757 4_656 ?
O3 K1 V1 31.91(6) 4_646 4_656 ?
O2 K1 V1 117.41(7) 8_556 4_656 ?
O1 K1 V1 38.34(6) 4_656 4_656 ?
O5 K1 V1 32.28(5) . 4_656 ?
O1 K1 V1 121.61(7) 8_556 4_656 ?
C1 K1 V1 125.91(8) 8_556 4_656 ?
P1 K1 V1 52.53(4) 4_646 4_656 ?
O7 K1 V1 145.98(10) . . ?
O6 K1 V1 15.82(6) . . ?
O7 K1 V1 79.34(9) 5_757 . ?
O3 K1 V1 62.57(6) 4_646 . ?
O2 K1 V1 98.17(7) 8_556 . ?
O1 K1 V1 112.31(7) 4_656 . ?
O5 K1 V1 61.76(7) . . ?
O1 K1 V1 143.24(6) 8_556 . ?
C1 K1 V1 120.32(7) 8_556 . ?
P1 K1 V1 48.60(2) 4_646 . ?
V1 K1 V1 73.97(3) 4_656 . ?
O6 V1 O3 99.80(13) . 1_545 ?
O6 V1 O5 104.32(15) . 4_646 ?
O3 V1 O5 86.90(12) 1_545 4_646 ?
O6 V1 O4 98.53(14) . . ?
O3 V1 O4 161.66(12) 1_545 . ?
O5 V1 O4 89.20(12) 4_646 . ?
O6 V1 O2 97.27(15) . 2_656 ?
O3 V1 O2 88.04(11) 1_545 2_656 ?
O5 V1 O2 158.36(11) 4_646 2_656 ?
O4 V1 O2 89.02(11) . 2_656 ?
O6 V1 O1 171.83(13) . . ?
O3 V1 O1 80.50(10) 1_545 . ?
O5 V1 O1 83.86(12) 4_646 . ?
O4 V1 O1 81.27(10) . . ?
O2 V1 O1 74.56(12) 2_656 . ?
O6 V1 K1 135.46(11) . 4_646 ?
O3 V1 K1 48.85(9) 1_545 4_646 ?
O5 V1 K1 52.34(9) 4_646 4_646 ?
O4 V1 K1 115.97(10) . 4_646 ?
O2 V1 K1 109.94(9) 2_656 4_646 ?
O1 V1 K1 50.15(7) . 4_646 ?
O6 V1 K1 28.25(11) . . ?
O3 V1 K1 112.76(8) 1_545 . ?
O5 V1 K1 79.96(9) 4_646 . ?
O4 V1 K1 84.11(8) . . ?
O2 V1 K1 121.26(9) 2_656 . ?
O1 V1 K1 158.29(7) . . ?
K1 V1 K1 125.36(2) 4_646 . ?
O3 P1 O4 107.10(17) . . ?
O3 P1 O5 113.46(16) . . ?
O4 P1 O5 114.46(16) . . ?
O3 P1 K1 45.75(12) . 4_656 ?
O4 P1 K1 75.19(12) . 4_656 ?
O5 P1 K1 99.15(12) . 4_656 ?
O1 C1 O2 126.6(3) . . ?
O1 C1 C1 116.5(4) . 2_656 ?
O2 C1 C1 116.9(4) . 2_656 ?
O1 C1 K1 67.9(2) . 8_455 ?
O2 C1 K1 61.49(18) . 8_455 ?
C1 C1 K1 160.55(8) 2_656 8_455 ?
C1 O1 V1 112.3(2) . . ?
C1 O1 K1 130.0(2) . 4_646 ?
V1 O1 K1 91.51(9) . 4_646 ?
C1 O1 K1 89.2(2) . 8_455 ?
V1 O1 K1 149.27(11) . 8_455 ?
K1 O1 K1 90.69(9) 4_646 8_455 ?
C1 O2 V1 119.8(2) . 2_656 ?
C1 O2 K1 95.6(2) . 8_455 ?
V1 O2 K1 139.14(12) 2_656 8_455 ?
P1 O3 V1 137.45(18) . 1_565 ?
P1 O3 K1 111.73(15) . 4_656 ?
V1 O3 K1 99.24(11) 1_565 4_656 ?
P1 O4 V1 131.39(18) . . ?
P1 O5 V1 130.58(17) . 4_656 ?
P1 O5 K1 119.83(14) . . ?
V1 O5 K1 95.38(10) 4_656 . ?
V1 O6 K1 135.93(16) . . ?
K1 O7 K1 100.45(14) . 5_757 ?

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
O1W H1W O4 0.858(10) 2.05(2) 2.894(5) 170(10) .
O1W H1W O3 0.858(10) 2.43(9) 2.910(5) 116(8) .
O7 H7A O5 0.850(7) 2.236(15) 3.073(5) 168(6) 5_767
O7 H7B O1W 0.86(6) 2.34(7) 3.073(5) 144(4) 3_545

_refine_diff_density_max         0.740
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.159

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_b322
_database_code_depnum_ccdc_archive 'CCDC 1040913'
_audit_update_record             
;
2014-12-24 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H6 Na2 O14 P2 V2'
_chemical_formula_weight         463.87

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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                   6.3255(4)
_cell_length_b                   6.7760(5)
_cell_length_c                   8.0759(6)
_cell_angle_alpha                104.9920(10)
_cell_angle_beta                 101.6790(10)
_cell_angle_gamma                99.1200(10)
_cell_volume                     319.20(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    2274
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      27.48

_exptl_crystal_description       Rectangular_Block
_exptl_crystal_colour            Blue
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.413
_exptl_crystal_F_000             228
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.859
_shelx_estimated_absorpt_T_min   0.781
_shelx_estimated_absorpt_T_max   0.866
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7862
_exptl_absorpt_correction_T_max  0.8456
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2010)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4133
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.700
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1454
_reflns_number_gt                1377
_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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+0.3564P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1454
_refine_ls_number_parameters     109
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0745
_refine_ls_wR_factor_gt          0.0734
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_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 0.16495(6) 0.27063(6) 0.34919(5) 0.01333(13) Uani 1 1 d . . . . .
Na1 Na 0.2102(2) 0.44332(19) 0.84588(15) 0.0374(3) Uani 1 1 d . . . . .
P1 P 0.31466(9) 0.74174(9) 0.58455(8) 0.01494(15) Uani 1 1 d . . . . .
H1 H 0.336(5) 0.933(4) 0.571(4) 0.018 Uiso 1 1 d . U . . .
O1 O 0.2630(3) 0.5790(3) 0.4026(2) 0.0206(4) Uani 1 1 d . . . . .
O2 O 0.1504(3) 0.6970(3) 0.6922(2) 0.0177(3) Uani 1 1 d . . . . .
O3 O 0.5460(3) 0.7707(3) 0.6972(2) 0.0330(5) Uani 1 1 d . . . . .
O4 O 0.1950(3) 0.2447(3) 0.5428(2) 0.0225(4) Uani 1 1 d . . . . .
O5 O 0.4330(4) 0.6894(4) 1.1230(3) 0.0398(5) Uani 1 1 d D . . . .
H5A H 0.388(6) 0.652(6) 1.205(4) 0.048 Uiso 1 1 d D U . . .
H5B H 0.450(7) 0.811(3) 1.117(5) 0.048 Uiso 1 1 d D U . . .
O6 O 0.0923(3) 0.2716(2) 0.0626(2) 0.0189(4) Uani 1 1 d . . . . .
O7 O -0.0420(3) 0.0417(3) -0.2072(2) 0.0187(3) Uani 1 1 d . . . . .
C1 C 0.0144(4) 0.0902(3) -0.0412(3) 0.0146(4) 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
V1 O4 1.5947(17) . ?
V1 O3 1.9865(18) 2_666 ?
V1 O1 1.9877(17) . ?
V1 O2 2.0112(16) 2_566 ?
V1 O7 2.0642(17) 2 ?
V1 O6 2.2689(17) . ?
V1 Na1 3.6599(13) 2_566 ?
Na1 O2 2.400(2) . ?
Na1 O5 2.413(3) . ?
Na1 O4 2.444(2) . ?
Na1 O6 2.506(2) 1_556 ?
Na1 O5 2.548(3) 2_667 ?
Na1 O7 2.806(2) 1_556 ?
Na1 C1 2.956(3) 1_556 ?
Na1 O6 2.991(2) 2_566 ?
Na1 V1 3.6600(13) 2_566 ?
Na1 Na1 3.827(3) 2_667 ?
Na1 Na1 4.025(3) 2_567 ?
P1 O3 1.5118(19) . ?
P1 O2 1.5260(16) . ?
P1 O1 1.5282(17) . ?
O2 V1 2.0112(16) 2_566 ?
O3 V1 1.9865(18) 2_666 ?
O5 Na1 2.548(3) 2_667 ?
O6 C1 1.251(3) . ?
O6 Na1 2.506(2) 1_554 ?
O6 Na1 2.991(2) 2_566 ?
O7 C1 1.255(3) . ?
O7 V1 2.0642(17) 2 ?
O7 Na1 2.806(2) 1_554 ?
C1 C1 1.539(4) 2 ?
C1 Na1 2.956(2) 1_554 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 V1 O3 100.87(9) . 2_666 ?
O4 V1 O1 101.99(8) . . ?
O3 V1 O1 91.02(8) 2_666 . ?
O4 V1 O2 98.27(8) . 2_566 ?
O3 V1 O2 160.48(8) 2_666 2_566 ?
O1 V1 O2 88.74(7) . 2_566 ?
O4 V1 O7 97.54(8) . 2 ?
O3 V1 O7 86.42(8) 2_666 2 ?
O1 V1 O7 160.43(7) . 2 ?
O2 V1 O7 87.31(7) 2_566 2 ?
O4 V1 O6 173.30(8) . . ?
O3 V1 O6 81.63(7) 2_666 . ?
O1 V1 O6 84.10(6) . . ?
O2 V1 O6 78.94(6) 2_566 . ?
O7 V1 O6 76.33(6) 2 . ?
O4 V1 Na1 125.90(7) . 2_566 ?
O3 V1 Na1 128.06(7) 2_666 2_566 ?
O1 V1 Na1 60.94(6) . 2_566 ?
O2 V1 Na1 37.50(5) 2_566 2_566 ?
O7 V1 Na1 106.09(5) 2 2_566 ?
O6 V1 Na1 54.69(5) . 2_566 ?
O2 Na1 O5 96.58(8) . . ?
O2 Na1 O4 78.67(7) . . ?
O5 Na1 O4 147.17(9) . . ?
O2 Na1 O6 145.59(8) . 1_556 ?
O5 Na1 O6 79.14(7) . 1_556 ?
O4 Na1 O6 122.46(7) . 1_556 ?
O2 Na1 O5 121.49(8) . 2_667 ?
O5 Na1 O5 79.08(10) . 2_667 ?
O4 Na1 O5 76.19(7) . 2_667 ?
O6 Na1 O5 91.50(8) 1_556 2_667 ?
O2 Na1 O7 130.64(7) . 1_556 ?
O5 Na1 O7 127.37(8) . 1_556 ?
O4 Na1 O7 74.68(6) . 1_556 ?
O6 Na1 O7 49.23(5) 1_556 1_556 ?
O5 Na1 O7 91.28(8) 2_667 1_556 ?
O2 Na1 C1 147.72(8) . 1_556 ?
O5 Na1 C1 102.47(8) . 1_556 ?
O4 Na1 C1 97.86(7) . 1_556 ?
O6 Na1 C1 24.76(6) 1_556 1_556 ?
O5 Na1 C1 87.88(8) 2_667 1_556 ?
O7 Na1 C1 24.98(6) 1_556 1_556 ?
O2 Na1 O6 59.61(6) . 2_566 ?
O5 Na1 O6 78.23(8) . 2_566 ?
O4 Na1 O6 123.72(7) . 2_566 ?
O6 Na1 O6 86.27(6) 1_556 2_566 ?
O5 Na1 O6 157.21(8) 2_667 2_566 ?
O7 Na1 O6 104.14(6) 1_556 2_566 ?
C1 Na1 O6 99.00(6) 1_556 2_566 ?
O2 Na1 V1 30.67(4) . 2_566 ?
O5 Na1 V1 105.51(7) . 2_566 ?
O4 Na1 V1 86.97(5) . 2_566 ?
O6 Na1 V1 117.24(6) 1_556 2_566 ?
O5 Na1 V1 151.26(7) 2_667 2_566 ?
O7 Na1 V1 106.72(5) 1_556 2_566 ?
C1 Na1 V1 117.78(6) 1_556 2_566 ?
O6 Na1 V1 38.25(4) 2_566 2_566 ?
O2 Na1 Na1 114.84(7) . 2_667 ?
O5 Na1 Na1 40.83(6) . 2_667 ?
O4 Na1 Na1 111.77(7) . 2_667 ?
O6 Na1 Na1 84.18(6) 1_556 2_667 ?
O5 Na1 Na1 38.25(6) 2_667 2_667 ?
O7 Na1 Na1 113.43(6) 1_556 2_667 ?
C1 Na1 Na1 96.40(6) 1_556 2_667 ?
O6 Na1 Na1 119.03(6) 2_566 2_667 ?
V1 Na1 Na1 138.80(5) 2_566 2_667 ?
O2 Na1 Na1 97.91(6) . 2_567 ?
O5 Na1 Na1 74.40(7) . 2_567 ?
O4 Na1 Na1 138.30(8) . 2_567 ?
O6 Na1 Na1 47.86(5) 1_556 2_567 ?
O5 Na1 Na1 134.54(7) 2_667 2_567 ?
O7 Na1 Na1 76.99(5) 1_556 2_567 ?
C1 Na1 Na1 63.31(5) 1_556 2_567 ?
O6 Na1 Na1 38.41(4) 2_566 2_567 ?
V1 Na1 Na1 72.63(4) 2_566 2_567 ?
Na1 Na1 Na1 107.31(5) 2_667 2_567 ?
O3 P1 O2 108.35(10) . . ?
O3 P1 O1 113.89(10) . . ?
O2 P1 O1 113.23(10) . . ?
P1 O1 V1 126.19(10) . . ?
P1 O2 V1 127.34(10) . 2_566 ?
P1 O2 Na1 116.25(9) . . ?
V1 O2 Na1 111.83(8) 2_566 . ?
P1 O3 V1 135.65(12) . 2_666 ?
V1 O4 Na1 140.65(10) . . ?
Na1 O5 Na1 100.92(10) . 2_667 ?
C1 O6 V1 111.19(14) . . ?
C1 O6 Na1 98.21(14) . 1_554 ?
V1 O6 Na1 145.50(8) . 1_554 ?
C1 O6 Na1 120.01(14) . 2_566 ?
V1 O6 Na1 87.06(6) . 2_566 ?
Na1 O6 Na1 93.73(6) 1_554 2_566 ?
C1 O7 V1 118.20(15) . 2 ?
C1 O7 Na1 84.19(13) . 1_554 ?
V1 O7 Na1 152.58(8) 2 1_554 ?
O6 C1 O7 125.7(2) . . ?
O6 C1 C1 117.4(2) . 2 ?
O7 C1 C1 116.9(2) . 2 ?
O6 C1 Na1 57.03(12) . 1_554 ?
O7 C1 Na1 70.83(12) . 1_554 ?
C1 C1 Na1 162.9(2) 2 1_554 ?

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
O5 H5A O1 0.854(19) 2.049(19) 2.901(3) 175(4) 1_556

_refine_diff_density_max         0.498
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.085

_shelxl_version_number           2014-3



