# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 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_200721a
_database_code_depnum_ccdc_archive 'CCDC 2027158'
_audit_update_record             
;
2020-09-03 deposited with the CCDC.	2020-11-19 downloaded from the CCDC.
;
_audit_creation_date             2020-07-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(Mo8 O30 Y4)'
_chemical_formula_sum            'Mo4 O15 Y2'
_chemical_formula_weight         801.58
_chemical_melting_point          ?
_chemical_oxdiff_formula         MoYO
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mo Mo -1.6832 0.6857 '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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   6.8110(4)
_cell_length_b                   9.5833(6)
_cell_length_c                   10.5124(7)
_cell_angle_alpha                90
_cell_angle_beta                 105.512(7)
_cell_angle_gamma                90
_cell_volume                     661.17(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2980
_cell_measurement_temperature    292.99(10)
_cell_measurement_theta_max      30.3230
_cell_measurement_theta_min      2.9030
_shelx_estimated_absorpt_T_max   0.789
_shelx_estimated_absorpt_T_min   0.575
_exptl_absorpt_coefficient_mu    12.429
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.026
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1013
_diffrn_reflns_av_unetI/netI     0.0859
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5250
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.926
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -27.00   4.00   1.00    0.58    --    5.65 -17.00 -51.00   31
  2  ω    -66.00 -32.00   1.00    0.58    --    5.65 -17.00 -51.00   34
  3  ω    -64.00  28.00   1.00    0.58    --    5.65 -77.00 120.00   92
  4  ω    -21.00  29.00   1.00    0.58    --   -4.56 -99.00  30.00   50
  5  ω    -43.00 -18.00   1.00    0.58    --   -4.56 -17.00 -51.00   25
  6  ω     27.00  60.00   1.00    0.58    --   -4.56  17.00 118.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0480271000
_diffrn_orient_matrix_UB_12      -0.0128244000
_diffrn_orient_matrix_UB_13      -0.0509695000
_diffrn_orient_matrix_UB_21      -0.0967948000
_diffrn_orient_matrix_UB_22      -0.0085149000
_diffrn_orient_matrix_UB_23      -0.0458012000
_diffrn_orient_matrix_UB_31      -0.0029900000
_diffrn_orient_matrix_UB_32      0.0723977000
_diffrn_orient_matrix_UB_33      -0.0143943000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1217
_reflns_number_total             1342
_reflns_odcompleteness_completeness 99.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.188
_refine_diff_density_min         -2.120
_refine_diff_density_rms         0.444
_refine_ls_extinction_coef       0.257(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1342
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0531
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0771P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1306
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.41840(12) 0.74323(7) 0.48880(7) 0.0121(4) Uani 1 1 d . . . . .
Mo2 Mo 0.87906(11) 0.59534(8) 0.84388(7) 0.0127(4) Uani 1 1 d . . . . .
Y1 Y 0.71252(13) 0.97708(8) 0.77670(8) 0.0117(4) Uani 1 1 d . . . . .
O1 O 1.000000 0.500000 1.000000 0.025(2) Uani 1 2 d S T P . .
O2 O 0.2542(11) 0.8641(7) 0.3822(6) 0.0193(14) Uani 1 1 d . . . . .
O3 O 0.5227(11) 0.6261(7) 0.3976(6) 0.0214(15) Uani 1 1 d . . . . .
O4 O 0.9458(10) 0.5283(7) 0.7079(7) 0.0191(14) Uani 1 1 d . . . . .
O5 O 0.8891(11) 0.7762(7) 0.8544(7) 0.0206(15) Uani 1 1 d . . . . .
O6 O 0.6220(10) 0.5574(7) 0.8163(7) 0.0200(14) Uani 1 1 d . . . . .
O7 O 0.6175(11) 0.8321(7) 0.6015(6) 0.0223(15) Uani 1 1 d . . . . .
O8 O 0.2791(10) 0.6525(7) 0.5801(6) 0.0205(15) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0125(5) 0.0143(5) 0.0097(5) 0.0002(2) 0.0032(4) 0.0013(2)
Mo2 0.0104(5) 0.0150(5) 0.0117(5) 0.0004(2) 0.0012(4) 0.0008(3)
Y1 0.0112(6) 0.0135(5) 0.0106(5) 0.0005(3) 0.0031(4) 0.0002(3)
O1 0.019(6) 0.029(5) 0.022(5) 0.014(4) -0.003(4) -0.001(4)
O2 0.019(4) 0.019(3) 0.021(3) 0.006(2) 0.008(3) -0.002(3)
O3 0.023(4) 0.023(3) 0.020(3) -0.006(2) 0.010(3) 0.001(3)
O4 0.010(3) 0.031(4) 0.017(3) -0.010(3) 0.005(3) -0.001(3)
O5 0.015(4) 0.021(3) 0.024(3) 0.004(2) 0.003(3) 0.005(2)
O6 0.008(3) 0.032(4) 0.022(3) -0.006(3) 0.008(3) 0.000(3)
O7 0.023(4) 0.026(4) 0.016(3) -0.008(3) 0.002(3) -0.002(3)
O8 0.018(4) 0.028(3) 0.019(3) 0.011(3) 0.010(3) 0.011(3)

_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 O2 1.783(7) . ?
Mo1 O3 1.746(6) . ?
Mo1 O7 1.763(7) . ?
Mo1 O8 1.750(6) . ?
Mo2 Y1 3.5377(11) 2_746 ?
Mo2 O1 1.8665(7) . ?
Mo2 O2 2.508(7) 4_676 ?
Mo2 O4 1.735(6) . ?
Mo2 O5 1.737(7) . ?
Mo2 O6 1.735(6) . ?
Y1 O2 2.316(6) 3_676 ?
Y1 O3 2.268(6) 4_576 ?
Y1 O4 2.342(7) 2_756 ?
Y1 O5 2.301(7) . ?
Y1 O6 2.355(7) 2_656 ?
Y1 O7 2.260(6) . ?
Y1 O8 2.247(6) 2_656 ?

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 110.6(3) . . ?
O3 Mo1 O7 109.1(3) . . ?
O3 Mo1 O8 110.0(3) . . ?
O7 Mo1 O2 110.4(3) . . ?
O8 Mo1 O2 109.0(3) . . ?
O8 Mo1 O7 107.7(3) . . ?
O1 Mo2 Y1 87.35(3) . 2_746 ?
O1 Mo2 O2 75.14(16) . 4_676 ?
O2 Mo2 Y1 40.75(14) 4_676 2_746 ?
O4 Mo2 Y1 35.1(2) . 2_746 ?
O4 Mo2 O1 113.1(2) . . ?
O4 Mo2 O2 73.1(3) . 4_676 ?
O4 Mo2 O5 114.1(3) . . ?
O4 Mo2 O6 105.1(3) . . ?
O5 Mo2 Y1 108.7(2) . 2_746 ?
O5 Mo2 O1 115.6(2) . . ?
O5 Mo2 O2 79.3(3) . 4_676 ?
O6 Mo2 Y1 136.7(2) . 2_746 ?
O6 Mo2 O1 103.5(2) . . ?
O6 Mo2 O2 176.8(3) . 4_676 ?
O6 Mo2 O5 103.9(3) . . ?
O2 Y1 Mo2 44.99(18) 3_676 2_756 ?
O2 Y1 O4 68.0(2) 3_676 2_756 ?
O2 Y1 O6 75.9(2) 3_676 2_656 ?
O3 Y1 Mo2 163.98(18) 4_576 2_756 ?
O3 Y1 O2 150.6(3) 4_576 3_676 ?
O3 Y1 O4 139.3(2) 4_576 2_756 ?
O3 Y1 O5 76.0(2) 4_576 . ?
O3 Y1 O6 75.1(2) 4_576 2_656 ?
O4 Y1 Mo2 25.21(16) 2_756 2_756 ?
O4 Y1 O6 142.5(2) 2_756 2_656 ?
O5 Y1 Mo2 90.51(17) . 2_756 ?
O5 Y1 O2 131.6(2) . 3_676 ?
O5 Y1 O4 74.6(2) . 2_756 ?
O5 Y1 O6 141.0(2) . 2_656 ?
O6 Y1 Mo2 120.83(15) 2_656 2_756 ?
O7 Y1 Mo2 89.21(18) . 2_756 ?
O7 Y1 O2 83.0(2) . 3_676 ?
O7 Y1 O3 96.1(3) . 4_576 ?
O7 Y1 O4 104.4(2) . 2_756 ?
O7 Y1 O5 77.5(3) . . ?
O7 Y1 O6 80.1(3) . 2_656 ?
O8 Y1 Mo2 96.83(16) 2_656 2_756 ?
O8 Y1 O2 90.1(2) 2_656 3_676 ?
O8 Y1 O3 82.3(2) 2_656 4_576 ?
O8 Y1 O4 87.2(2) 2_656 2_756 ?
O8 Y1 O5 118.1(2) 2_656 . ?
O8 Y1 O6 83.2(2) 2_656 2_656 ?
O8 Y1 O7 163.1(3) 2_656 . ?
Mo2 O1 Mo2 180.0 3_767 . ?
Mo1 O2 Mo2 130.0(3) . 4_475 ?
Mo1 O2 Y1 135.6(4) . 3_676 ?
Y1 O2 Mo2 94.3(2) 3_676 4_475 ?
Mo1 O3 Y1 164.7(4) . 4_575 ?
Mo2 O4 Y1 119.7(3) . 2_746 ?
Mo2 O5 Y1 143.6(4) . . ?
Mo2 O6 Y1 163.5(4) . 2_646 ?
Mo1 O7 Y1 147.8(4) . . ?
Mo1 O8 Y1 144.9(4) . 2_646 ?

_shelx_res_file                  
;
TITL 200721a_a.res in P2(1)/c
    200721a.res
    created by SHELXL-2018/3 at 21:38:44 on 21-Jul-2020
REM Old TITL 200721A in P21/c #14
REM SHELXT solution in P2(1)/c: R1 0.133, Rweak 0.016, Alpha 0.040
REM <I/s> 0.338 for 87 systematic absences, Orientation as input
REM Formula found by SHELXT: O5 Y2
CELL 0.71073 6.811 9.5833 10.5124 90 105.512 90
ZERR 2 0.0004 0.0006 0.0007 0 0.007 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC Mo O Y
UNIT 8 30 4

L.S. 10 0 0
PLAN  20
SIZE 0.02 0.04 0.05
list 4
fmap 2 53
acta
SHEL 999 0.8
REM <olex2.extras>
REM <HklSrc "%.\\200721A.hkl">
REM </olex2.extras>

WGHT    0.077100
EXTI    0.256615
FVAR       0.65702
MO1   1    0.418403    0.743230    0.488798    11.00000    0.01250    0.01428 =
         0.00966    0.00024    0.00321    0.00133
MO2   1    0.879059    0.595340    0.843876    11.00000    0.01037    0.01504 =
         0.01171    0.00037    0.00119    0.00081
Y1    3    0.712520    0.977081    0.776700    11.00000    0.01123    0.01349 =
         0.01063    0.00048    0.00315    0.00015
O1    2    1.000000    0.500000    1.000000    10.50000    0.01921    0.02914 =
         0.02208    0.01361   -0.00255   -0.00052
O2    2    0.254167    0.864091    0.382233    11.00000    0.01926    0.01946 =
         0.02066    0.00587    0.00769   -0.00164
O3    2    0.522723    0.626080    0.397641    11.00000    0.02313    0.02304 =
         0.02008   -0.00605    0.00960    0.00122
O4    2    0.945755    0.528257    0.707934    11.00000    0.00969    0.03121 =
         0.01749   -0.00976    0.00536   -0.00143
O5    2    0.889068    0.776224    0.854399    11.00000    0.01546    0.02059 =
         0.02437    0.00410    0.00297    0.00470
O6    2    0.621963    0.557440    0.816313    11.00000    0.00827    0.03189 =
         0.02223   -0.00553    0.00826   -0.00036
O7    2    0.617456    0.832058    0.601467    11.00000    0.02260    0.02611 =
         0.01619   -0.00817    0.00179   -0.00196
O8    2    0.279125    0.652492    0.580095    11.00000    0.01764    0.02826 =
         0.01853    0.01108    0.00973    0.01073
HKLF 4




REM  200721a_a.res in P2(1)/c
REM wR2 = 0.1306, GooF = S = 1.076, Restrained GooF = 1.076 for all data
REM R1 = 0.0531 for 1217 Fo > 4sig(Fo) and 0.0563 for all 1342 data
REM 98 parameters refined using 0 restraints

END

WGHT      0.0771      0.0000

REM Highest difference peak  2.188,  deepest hole -2.120,  1-sigma level  0.444
Q1    1   0.5549  0.7408  0.5573  11.00000  0.05    2.19
Q2    1   1.0176  0.5822  0.9221  11.00000  0.05    2.14
Q3    1   0.7417  1.0333  0.7267  11.00000  0.05    1.79
Q4    1   0.7474  0.5960  0.7733  11.00000  0.05    1.75
Q5    1   0.2865  0.7491  0.4184  11.00000  0.05    1.63
Q6    1   0.6945  1.0136  0.8541  11.00000  0.05    1.60
Q7    1   0.8987  0.5840  0.7550  11.00000  0.05    1.58
Q8    1   0.8579  0.9854  0.8583  11.00000  0.05    1.56
Q9    1   0.8455  0.5376  0.9035  11.00000  0.05    1.51
Q10   1   0.5913  0.9786  0.7220  11.00000  0.05    1.46
Q11   1   0.8527  0.6659  0.9011  11.00000  0.05    1.41
Q12   1   0.8832  0.9792  0.8908  11.00000  0.05    1.37
Q13   1   0.1399  0.7531  0.4124  11.00000  0.05    1.31
Q14   1   0.7034  0.7438  0.5750  11.00000  0.05    1.31
Q15   1   0.6728  0.7409  0.7344  11.00000  0.05    1.26
Q16   1   0.8668  0.5975  0.9394  11.00000  0.05    1.25
Q17   1   0.4033  0.5846  0.6133  11.00000  0.05    1.25
Q18   1   0.6831  0.9490  0.8536  11.00000  0.05    1.24
Q19   1   0.6433  0.6735  0.8216  11.00000  0.05    1.24
Q20   1   0.1674  0.8969  0.4174  11.00000  0.05    1.21
;
_shelx_res_checksum              29413
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.224
_oxdiff_exptl_absorpt_empirical_full_min 0.540
