# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_twin_file_a
_database_code_depnum_ccdc_archive 'CCDC 1888651'
_audit_update_record             
;
2019-01-03 deposited with the CCDC.
2019-02-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H6 O6 P3 V'
_chemical_formula_weight         245.90

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'
H H 0.0000 0.0000 '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      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                   11.922(8)
_cell_length_b                   7.542(6)
_cell_length_c                   8.860(6)
_cell_angle_alpha                90
_cell_angle_beta                 106.29(2)
_cell_angle_gamma                90
_cell_volume                     764.7(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    491
_cell_measurement_theta_min      3.6
_cell_measurement_theta_max      16.4

_exptl_crystal_description       sheet
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.136
_exptl_crystal_F_000             488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    1.898
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.574231
_exptl_absorpt_correction_T_max  0.745019
_exptl_absorpt_process_details   twinabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1215
_diffrn_reflns_av_unetI/netI     0.1312
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         1.780
_diffrn_reflns_theta_max         24.151
_diffrn_reflns_theta_full        24.151
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             1215
_reflns_number_gt                691
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1327P)²+80.3330P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1215
_refine_ls_number_parameters     95
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.2330
_refine_ls_R_factor_gt           0.1509
_refine_ls_wR_factor_ref         0.4204
_refine_ls_wR_factor_gt          0.3856
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.004

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
V001 V 1.0000 0.5000 0.5000 0.0277(17) Uani 1 2 d S . P . .
V002 V 0.5000 0.5000 0.5000 0.0267(17) Uani 1 2 d S . P . .
P1 P 0.9318(6) 0.6447(9) 0.7955(8) 0.0307(18) Uani 1 1 d D . . . .
H2 H 0.8512(16) 0.714(4) 0.680(2) 0.08(5) Uiso 1 1 d D . . . .
H1 H 0.8938(19) 0.509(2) 0.857(3) 0.08(5) Uiso 1 1 d D . . . .
P3 P 0.4017(6) 0.3438(10) 0.1504(8) 0.0342(19) Uani 1 1 d D . . . .
H6 H 0.2973(12) 0.335(6) 0.053(2) 0.08(5) Uiso 1 1 d D . . . .
H5 H 0.4648(18) 0.467(3) 0.112(2) 0.08(5) Uiso 1 1 d D . . . .
P2 P 0.7333(7) 0.3548(12) 0.4147(10) 0.058(3) Uani 1 1 d D . . . .
H4 H 0.704(2) 0.354(7) 0.2618(12) 0.08(5) Uiso 1 1 d D . . . .
H3 H 0.8022(18) 0.224(3) 0.476(3) 0.08(5) Uiso 1 1 d D . . . .
O006 O 1.0257(13) 0.573(3) 0.723(2) 0.063(4) Uani 1 1 d D . . . .
O007 O 0.8309(18) 0.489(3) 0.465(3) 0.051(6) Uani 1 1 d . . . . .
O008 O 0.9882(17) 0.741(3) 0.946(2) 0.042(5) Uani 1 1 d . . . . .
O009 O 0.3895(15) 0.386(3) 0.3111(17) 0.063(4) Uani 1 1 d D . . . .
O00A O 0.4630(19) 0.180(3) 0.146(3) 0.063(4) Uani 1 1 d . . . . .
O00B O 0.6335(13) 0.365(3) 0.475(2) 0.063(4) Uani 1 1 d 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
V001 O007 1.95(2) 3_766 ?
V001 O007 1.95(2) . ?
V001 O006 1.990(19) . ?
V001 O006 1.990(19) 3_766 ?
V001 O008 2.006(19) 4_575 ?
V001 O008 2.006(19) 2_746 ?
V002 O00B 1.954(16) . ?
V002 O00B 1.954(16) 3_666 ?
V002 O00A 2.01(2) 4_566 ?
V002 O00A 2.01(2) 2_655 ?
V002 O009 2.008(16) . ?
V002 O009 2.008(16) 3_666 ?
P1 O008 1.50(2) . ?
P1 O006 1.537(17) . ?
P1 H2 1.301(8) . ?
P1 H1 1.301(8) . ?
P3 O00A 1.44(2) . ?
P3 O009 1.506(16) . ?
P3 H6 1.301(8) . ?
P3 H5 1.301(8) . ?
P2 O00B 1.435(16) . ?
P2 O007 1.51(2) . ?
P2 H4 1.301(8) . ?
P2 H3 1.301(8) . ?
O008 V001 2.006(19) 2_756 ?
O00A V002 2.01(2) 2_645 ?

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
O007 V001 O007 180.0 3_766 . ?
O007 V001 O006 88.1(8) 3_766 . ?
O007 V001 O006 91.9(8) . . ?
O007 V001 O006 91.9(8) 3_766 3_766 ?
O007 V001 O006 88.1(8) . 3_766 ?
O006 V001 O006 180.0 . 3_766 ?
O007 V001 O008 89.8(8) 3_766 4_575 ?
O007 V001 O008 90.2(8) . 4_575 ?
O006 V001 O008 87.1(8) . 4_575 ?
O006 V001 O008 92.9(8) 3_766 4_575 ?
O007 V001 O008 90.2(8) 3_766 2_746 ?
O007 V001 O008 89.8(8) . 2_746 ?
O006 V001 O008 92.9(8) . 2_746 ?
O006 V001 O008 87.1(8) 3_766 2_746 ?
O008 V001 O008 180.0 4_575 2_746 ?
O00B V002 O00B 180.0 . 3_666 ?
O00B V002 O00A 93.2(9) . 4_566 ?
O00B V002 O00A 86.8(9) 3_666 4_566 ?
O00B V002 O00A 86.8(9) . 2_655 ?
O00B V002 O00A 93.2(9) 3_666 2_655 ?
O00A V002 O00A 180.0 4_566 2_655 ?
O00B V002 O009 92.8(8) . . ?
O00B V002 O009 87.2(8) 3_666 . ?
O00A V002 O009 92.2(9) 4_566 . ?
O00A V002 O009 87.8(9) 2_655 . ?
O00B V002 O009 87.2(8) . 3_666 ?
O00B V002 O009 92.8(8) 3_666 3_666 ?
O00A V002 O009 87.8(9) 4_566 3_666 ?
O00A V002 O009 92.2(9) 2_655 3_666 ?
O009 V002 O009 180.0 . 3_666 ?
O008 P1 O006 110.1(11) . . ?
O008 P1 H2 123.3(16) . . ?
O006 P1 H2 106.2(10) . . ?
O008 P1 H1 97.5(14) . . ?
O006 P1 H1 106.2(10) . . ?
H2 P1 H1 112.4(14) . . ?
O00A P3 O009 113.0(13) . . ?
O00A P3 H6 110(2) . . ?
O009 P3 H6 108.0(10) . . ?
O00A P3 H5 105.9(16) . . ?
O009 P3 H5 108.0(10) . . ?
H6 P3 H5 112.4(14) . . ?
O00B P2 O007 120.1(13) . . ?
O00B P2 H4 112.3(11) . . ?
O007 P2 H4 106(2) . . ?
O00B P2 H3 112.3(11) . . ?
O007 P2 H3 92.3(15) . . ?
H4 P2 H3 112.4(14) . . ?
P1 O006 V001 125.8(10) . . ?
P2 O007 V001 138.6(14) . . ?
P1 O008 V001 131.9(13) . 2_756 ?
P3 O009 V002 131.6(10) . . ?
P3 O00A V002 143.1(16) . 2_645 ?
P2 O00B V002 149.1(15) . . ?

_refine_diff_density_max         1.423
_refine_diff_density_min         -1.600
_refine_diff_density_rms         0.315



