# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2020

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

data_x
_database_code_depnum_ccdc_archive 'CCDC 1976286'
loop_
_audit_author_name
_audit_author_address
'Meiling Feng'
;State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matte
China
;
_audit_update_record             
;
2020-01-09 deposited with the CCDC.	2020-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H3 O13 Se2 V3'
_chemical_formula_weight         521.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'

_cell_length_a                   7.1368(5)
_cell_length_b                   7.1368(5)
_cell_length_c                   11.4944(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     507.02(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1725
_cell_measurement_theta_min      4.7880
_cell_measurement_theta_max      28.8460

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.418
_exptl_crystal_F_000             488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    9.958
_shelx_estimated_absorpt_T_min   0.148
_shelx_estimated_absorpt_T_max   0.229
_exptl_absorpt_correction_T_min  0.48332
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3824
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.545
_diffrn_reflns_theta_max         29.487
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             870
_reflns_number_gt                818
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.855
_reflns_Friedel_fraction_max     0.887
_reflns_Friedel_fraction_full    0.990

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0500P)²+3.8000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 354 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.422(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         870
_refine_ls_number_parameters     56
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.0985
_refine_ls_wR_factor_gt          0.0954
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.009
_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
Se1 Se 0.333333 0.666667 0.47865(13) 0.0101(5) Uani 1 3 d S T P . .
Se2 Se 1.000000 1.000000 0.9257(2) 0.0088(5) Uani 1 3 d S T P . .
V1 V 0.6666(5) 0.7893(4) 0.7030(3) 0.0133(4) Uani 1 1 d . . . . .
O3 O 0.870(2) 0.7462(14) 0.6703(10) 0.0114(17) Uani 1 1 d . . . . .
O1 O 0.5827(15) 0.800(2) 0.5427(8) 0.0110(19) Uani 1 1 d . . . . .
O2 O 0.7509(15) 0.884(2) 0.8616(8) 0.014(2) Uani 1 1 d . . . . .
O4 O 0.461(2) 0.538(2) 0.7323(9) 0.018(2) Uani 1 1 d . . . . .
O5 O 0.666667 0.333333 0.509(3) 0.060(10) Uani 1 3 d S T P . .
H5A H 0.782552 0.335558 0.516465 0.090 Uiso 0.3333 1 d R U P A -1
H5B H 0.581840 0.278150 0.563567 0.090 Uiso 0.3333 1 d R U P A -1
H5C H 0.676095 0.445024 0.483073 0.090 Uiso 0.3333 1 d R U P A -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
Se1 O1 1.709(10) . ?
Se1 O1 1.709(9) 2_665 ?
Se1 O1 1.709(10) 3_565 ?
Se2 O2 1.708(9) . ?
Se2 O2 1.708(9) 3_675 ?
Se2 O2 1.708(9) 2_765 ?
V1 O3 1.672(13) . ?
V1 O4 1.690(14) . ?
V1 O2 1.933(10) . ?
V1 O1 1.949(9) . ?
V1 O4 2.131(14) 2_665 ?
V1 O3 2.155(14) 3_675 ?
O5 H5A 0.8234 . ?
O5 H5B 0.8200 . ?
O5 H5C 0.8228 . ?

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 Se1 O1 102.8(4) . 2_665 ?
O1 Se1 O1 102.8(4) . 3_565 ?
O1 Se1 O1 102.8(4) 2_665 3_565 ?
O2 Se2 O2 102.8(4) . 3_675 ?
O2 Se2 O2 102.8(4) . 2_765 ?
O2 Se2 O2 102.8(4) 3_675 2_765 ?
O3 V1 O4 102.9(4) . . ?
O3 V1 O2 97.4(6) . . ?
O4 V1 O2 97.8(5) . . ?
O3 V1 O1 96.1(5) . . ?
O4 V1 O1 96.2(6) . . ?
O2 V1 O1 157.8(4) . . ?
O3 V1 O4 166.0(6) . 2_665 ?
O4 V1 O4 91.0(7) . 2_665 ?
O2 V1 O4 81.8(5) . 2_665 ?
O1 V1 O4 80.8(5) . 2_665 ?
O3 V1 O3 89.6(5) . 3_675 ?
O4 V1 O3 167.5(5) . 3_675 ?
O2 V1 O3 81.5(5) . 3_675 ?
O1 V1 O3 81.1(5) . 3_675 ?
O4 V1 O3 76.5(4) 2_665 3_675 ?
V1 O3 V1 140.9(6) . 2_765 ?
Se1 O1 V1 129.8(6) . . ?
Se2 O2 V1 130.0(6) . . ?
V1 O4 V1 141.4(7) . 3_565 ?
H5A O5 H5B 115.2 . . ?
H5A O5 H5C 115.0 . . ?
H5B O5 H5C 115.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 V1 O3 V1 -136.5(7) . . . 2_765 ?
O2 V1 O3 V1 -36.7(10) . . . 2_765 ?
O1 V1 O3 V1 125.7(10) . . . 2_765 ?
O4 V1 O3 V1 49(3) 2_665 . . 2_765 ?
O3 V1 O3 V1 44.7(12) 3_675 . . 2_765 ?
O1 Se1 O1 V1 68.5(7) 2_665 . . . ?
O1 Se1 O1 V1 -38.0(8) 3_565 . . . ?
O2 Se2 O2 V1 68.7(8) 3_675 . . . ?
O2 Se2 O2 V1 -37.8(8) 2_765 . . . ?
O3 V1 O4 V1 -138.3(9) . . . 3_565 ?
O2 V1 O4 V1 122.2(11) . . . 3_565 ?
O1 V1 O4 V1 -40.5(12) . . . 3_565 ?
O4 V1 O4 V1 40.3(13) 2_665 . . 3_565 ?
O3 V1 O4 V1 36(4) 3_675 . . 3_565 ?

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
_geom_hbond_publ_flag
O5 H5A^a O3 0.82 2.59 3.15(2) 126.7 3_665 yes
O5 H5B^a O3 0.82 2.37 3.15(2) 159.6 2_655 yes
O5 H5C^a O2 0.82 2.37 3.09(2) 147.2 6_654 yes

_refine_diff_density_max         1.726
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.199



