# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_1_sq
_database_code_depnum_ccdc_archive 'CCDC 1957849'
loop_
_audit_author_name
_audit_author_address
'zhiyuan Yao'
;Nanjing Tech university
China
;
_audit_update_record             
;
2019-10-27 deposited with the CCDC.	2019-11-04 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         
' H12 Mo4.55 O42 V7.45, O4 P, 12(H2 O), 0.3(O), 6(K) [+ solvent]'
_chemical_formula_sum            'H36 K6 Mo4.55 O58.28 P V7.45'
_chemical_formula_weight         2050.37

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'
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'

_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'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   10.6513(5)
_cell_length_b                   10.6513(5)
_cell_length_c                   10.6513(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1208.39(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6692
_cell_measurement_theta_min      3.3130
_cell_measurement_theta_max      27.1460

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.818
_exptl_crystal_F_000             994
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    3.200
_shelx_estimated_absorpt_T_min   0.856
_shelx_estimated_absorpt_T_max   0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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            16220
_diffrn_reflns_av_unetI/netI     0.0078
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.313
_diffrn_reflns_theta_max         27.536
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             328
_reflns_number_gt                302
_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       ?
_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          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1095P)²+45.8405P] 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_number_reflns         328
_refine_ls_number_parameters     31
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0754
_refine_ls_wR_factor_ref         0.2424
_refine_ls_wR_factor_gt          0.2399
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_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
Mo1 Mo 0.23359(14) 0.000000 0.23359(14) 0.0257(8) Uani 0.3792 4 d S T P . .
V1 V 0.23359(14) 0.000000 0.23359(14) 0.0257(8) Uani 0.6208 4 d S T P . .
K1 K 0.500000 0.1527(19) 0.500000 0.116(6) Uani 1 8 d S T P . .
P1 P 0.000000 0.000000 0.000000 0.014(3) Uani 1 48 d S T P . .
O1 O 0.0852(14) -0.0852(14) 0.0852(14) 0.014(5) Uani 0.5 6 d S T P . .
O2 O 0.2987(11) 0.1239(8) 0.1239(8) 0.055(3) Uani 1 2 d S T P . .
O3 O 0.3398(8) 0.000000 0.3398(8) 0.039(3) Uani 1 4 d S T P . .
O4 O 0.2613(14) 0.2613(14) 0.500000 0.067(6) Uani 1 4 d S T P . .
H4A H 0.261728 0.327920 0.546010 0.101 Uiso 0.25 1 d R U P . .
H4B H 0.241249 0.282910 0.425440 0.101 Uiso 0.25 1 d R U P . .
O5 O 0.500000 0.500000 0.500000 0.05(8) Uani 0.3(2) 48 d S T P . .
O6 O 0.352(3) 0.000000 0.000000 0.076(9) Uani 1 8 d S T P . .
H6A H 0.328789 0.054020 0.054020 0.113 Uiso 0.25 2 d R U P . .
H6B H 0.385969 0.037120 -0.061860 0.113 Uiso 0.125 1 d R U 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
Mo1 O3 1.599(13) . ?
Mo1 O2 1.894(5) 34 ?
Mo1 O2 1.894(5) 27 ?
Mo1 O2 1.894(5) 9 ?
Mo1 O2 1.894(5) . ?
Mo1 O1 2.412(14) 27 ?
Mo1 O1 2.412(14) . ?
K1 O4 2.793(12) 31_556 ?
K1 O4 2.793(12) 3_656 ?
K1 O4 2.793(12) 5 ?
K1 O4 2.793(12) . ?
K1 O3 2.911(15) 25_656 ?
K1 O3 2.911(15) 2_655 ?
K1 O3 2.911(15) 26_556 ?
K1 O3 2.911(15) . ?
K1 K1 3.25(4) 25_656 ?
P1 O1 1.57(3) . ?
P1 O1 1.57(3) 27 ?
P1 O1 1.57(3) 3 ?
P1 O1 1.57(3) 28 ?
P1 O1 1.57(3) 26 ?
P1 O1 1.57(3) 2 ?
P1 O1 1.57(3) 25 ?
P1 O1 1.57(3) 4 ?
O1 O1 1.82(3) 28 ?
O1 O1 1.82(3) 27 ?
O1 O1 1.82(3) 26 ?

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
O3 Mo1 O2 100.2(4) . 34 ?
O3 Mo1 O2 100.2(4) . 27 ?
O2 Mo1 O2 88.1(5) 34 27 ?
O3 Mo1 O2 100.2(4) . 9 ?
O2 Mo1 O2 88.3(6) 34 9 ?
O2 Mo1 O2 159.6(8) 27 9 ?
O3 Mo1 O2 100.2(4) . . ?
O2 Mo1 O2 159.6(8) 34 . ?
O2 Mo1 O2 88.3(6) 27 . ?
O2 Mo1 O2 88.1(5) 9 . ?
O3 Mo1 O1 157.9(5) . 27 ?
O2 Mo1 O1 95.6(6) 34 27 ?
O2 Mo1 O1 95.6(6) 27 27 ?
O2 Mo1 O1 64.8(5) 9 27 ?
O2 Mo1 O1 64.8(5) . 27 ?
O3 Mo1 O1 157.9(5) . . ?
O2 Mo1 O1 64.8(5) 34 . ?
O2 Mo1 O1 64.8(5) 27 . ?
O2 Mo1 O1 95.6(6) 9 . ?
O2 Mo1 O1 95.6(6) . . ?
O1 Mo1 O1 44.2(10) 27 . ?
O4 K1 O4 80.1(4) 31_556 3_656 ?
O4 K1 O4 131.1(11) 31_556 5 ?
O4 K1 O4 80.1(4) 3_656 5 ?
O4 K1 O4 80.1(4) 31_556 . ?
O4 K1 O4 131.1(11) 3_656 . ?
O4 K1 O4 80.1(4) 5 . ?
O4 K1 O3 72.4(3) 31_556 25_656 ?
O4 K1 O3 72.4(3) 3_656 25_656 ?
O4 K1 O3 139.9(2) 5 25_656 ?
O4 K1 O3 139.9(2) . 25_656 ?
O4 K1 O3 139.9(2) 31_556 2_655 ?
O4 K1 O3 72.4(3) 3_656 2_655 ?
O4 K1 O3 72.4(3) 5 2_655 ?
O4 K1 O3 139.9(2) . 2_655 ?
O3 K1 O3 71.8(4) 25_656 2_655 ?
O4 K1 O3 72.4(3) 31_556 26_556 ?
O4 K1 O3 139.9(2) 3_656 26_556 ?
O4 K1 O3 139.9(2) 5 26_556 ?
O4 K1 O3 72.4(3) . 26_556 ?
O3 K1 O3 71.8(4) 25_656 26_556 ?
O3 K1 O3 112.0(7) 2_655 26_556 ?
O4 K1 O3 139.9(2) 31_556 . ?
O4 K1 O3 139.9(2) 3_656 . ?
O4 K1 O3 72.4(3) 5 . ?
O4 K1 O3 72.4(3) . . ?
O3 K1 O3 112.0(7) 25_656 . ?
O3 K1 O3 71.8(4) 2_655 . ?
O3 K1 O3 71.8(4) 26_556 . ?
O4 K1 K1 114.5(5) 31_556 25_656 ?
O4 K1 K1 114.5(5) 3_656 25_656 ?
O4 K1 K1 114.5(5) 5 25_656 ?
O4 K1 K1 114.5(5) . 25_656 ?
O3 K1 K1 56.0(4) 25_656 25_656 ?
O3 K1 K1 56.0(4) 2_655 25_656 ?
O3 K1 K1 56.0(4) 26_556 25_656 ?
O3 K1 K1 56.0(4) . 25_656 ?
O1 P1 O1 70.529(1) . 27 ?
O1 P1 O1 109.471(1) . 3 ?
O1 P1 O1 180(3) 27 3 ?
O1 P1 O1 70.529(1) . 28 ?
O1 P1 O1 109.471(1) 27 28 ?
O1 P1 O1 70.529(1) 3 28 ?
O1 P1 O1 70.529(1) . 26 ?
O1 P1 O1 109.471(2) 27 26 ?
O1 P1 O1 70.529(2) 3 26 ?
O1 P1 O1 109.471(1) 28 26 ?
O1 P1 O1 109.471(1) . 2 ?
O1 P1 O1 70.529(2) 27 2 ?
O1 P1 O1 109.471(2) 3 2 ?
O1 P1 O1 70.529(1) 28 2 ?
O1 P1 O1 180(3) 26 2 ?
O1 P1 O1 180(3) . 25 ?
O1 P1 O1 109.471(1) 27 25 ?
O1 P1 O1 70.529(1) 3 25 ?
O1 P1 O1 109.471(1) 28 25 ?
O1 P1 O1 109.471(1) 26 25 ?
O1 P1 O1 70.529(1) 2 25 ?
O1 P1 O1 109.471(1) . 4 ?
O1 P1 O1 70.529(1) 27 4 ?
O1 P1 O1 109.471(1) 3 4 ?
O1 P1 O1 180(3) 28 4 ?
O1 P1 O1 70.5 26 4 ?
O1 P1 O1 109.471(1) 2 4 ?
O1 P1 O1 70.529(1) 25 4 ?
P1 O1 O1 54.736(1) . 28 ?
P1 O1 O1 54.736(1) . 27 ?
O1 O1 O1 90.001(1) 28 27 ?
P1 O1 O1 54.736(1) . 26 ?
O1 O1 O1 90.0 28 26 ?
O1 O1 O1 90.001(1) 27 26 ?
P1 O1 Mo1 122.6(5) . . ?
O1 O1 Mo1 130.93(18) 28 . ?
O1 O1 Mo1 67.9(5) 27 . ?
O1 O1 Mo1 130.93(18) 26 . ?
P1 O1 Mo1 122.6(5) . 34 ?
O1 O1 Mo1 67.9(5) 28 34 ?
O1 O1 Mo1 130.93(18) 27 34 ?
O1 O1 Mo1 130.93(18) 26 34 ?
Mo1 O1 Mo1 93.7(7) . 34 ?
P1 O1 Mo1 122.6(5) . 6 ?
O1 O1 Mo1 130.93(18) 28 6 ?
O1 O1 Mo1 130.93(18) 27 6 ?
O1 O1 Mo1 67.9(5) 26 6 ?
Mo1 O1 Mo1 93.7(7) . 6 ?
Mo1 O1 Mo1 93.7(7) 34 6 ?
Mo1 O2 Mo1 136.5(7) . 5 ?
Mo1 O3 K1 146.0(4) . . ?
Mo1 O3 K1 146.0(4) . 25_656 ?
K1 O3 K1 68.0(7) . 25_656 ?
K1 O4 K1 138.9(11) 9 . ?

_refine_diff_density_max         0.884
_refine_diff_density_min         -2.013
_refine_diff_density_rms         0.274



