# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_x1
_audit_block_doi                 10.5517/ccdc.csd.cc1m25ql
_database_code_depnum_ccdc_archive 'CCDC 1491649'
_audit_update_record             
;
2016-07-08 deposited with the CCDC.
2016-10-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Li Mo O6 V'
_chemical_formula_weight         249.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li -0.0003 0.0001 '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'
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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/m  '

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

_cell_length_a                   9.3531(9)
_cell_length_b                   3.6477(4)
_cell_length_c                   6.6470(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.6430(10)
_cell_angle_gamma                90.00
_cell_volume                     210.79(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1116
_cell_measurement_theta_min      3.30
_cell_measurement_theta_max      27.43

_exptl_crystal_description       brown
_exptl_crystal_colour            block
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.936
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             232
_exptl_absorpt_coefficient_mu    5.121
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.7157
_exptl_absorpt_correction_T_max  0.7838
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1251
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.30
_diffrn_reflns_theta_max         27.52
_reflns_number_total             285
_reflns_number_gt                281
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0061P)²+0.7069P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0108(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         285
_refine_ls_number_parameters     30
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0116
_refine_ls_R_factor_gt           0.0113
_refine_ls_wR_factor_ref         0.0306
_refine_ls_wR_factor_gt          0.0304
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_restrained_S_all      1.232
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.18599(3) 0.0000 0.65105(5) 0.00769(14) Uani 0.50 2 d SP . .
Mo1 Mo 0.18599(3) 0.0000 0.65105(5) 0.00769(14) Uani 0.50 2 d SP . .
Li Li 0.0000 0.0000 0.0000 0.039(2) Uani 1 4 d S . .
O1 O 0.3321(2) 0.0000 0.8877(3) 0.0159(4) Uani 1 2 d S . .
O3 O 0.0256(2) 0.0000 0.7122(4) 0.0146(4) Uani 1 2 d S . .
O2 O 0.1916(2) 0.5000 0.5642(3) 0.0097(4) Uani 1 2 d S . .

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
V1 0.00893(19) 0.00613(18) 0.0088(2) 0.000 0.00416(12) 0.000
Mo1 0.00893(19) 0.00613(18) 0.0088(2) 0.000 0.00416(12) 0.000
Li 0.033(5) 0.067(7) 0.018(4) 0.000 0.011(4) 0.000
O1 0.0141(10) 0.0187(11) 0.0136(10) 0.000 0.0037(8) 0.000
O3 0.0106(9) 0.0105(9) 0.0238(11) 0.000 0.0076(9) 0.000
O2 0.0124(9) 0.0052(8) 0.0141(9) 0.000 0.0078(8) 0.000

_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 O1 1.660(2) . ?
V1 O3 1.693(2) . ?
V1 O2 1.9194(6) 1_545 ?
V1 O2 1.9194(6) . ?
V1 O2 2.1375(19) 7_556 ?
Li O3 2.013(2) 5_556 ?
Li O3 2.013(2) 1_554 ?
Li O1 2.3422(13) 3_444 ?
Li O1 2.3422(13) 7_556 ?
Li O1 2.3422(13) 3_454 ?
Li O1 2.3422(13) 7_546 ?
Li Mo1 3.3737(4) 1_554 ?
Li Mo1 3.3737(4) 5_556 ?
O1 Li 2.3422(13) 3_556 ?
O1 Li 2.3422(13) 3_546 ?
O3 Li 2.013(2) 1_556 ?
O3 Mo1 2.494(2) 5_556 ?
O2 Mo1 1.9194(6) 1_565 ?
O2 V1 1.9194(6) 1_565 ?
O2 Mo1 2.1375(19) 7_556 ?
O2 V1 2.1375(19) 7_556 ?

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 V1 O3 105.36(10) . . ?
O1 V1 O2 100.41(6) . 1_545 ?
O3 V1 O2 101.36(6) . 1_545 ?
O1 V1 O2 100.41(6) . . ?
O3 V1 O2 101.36(6) . . ?
O2 V1 O2 143.68(11) 1_545 . ?
O1 V1 O2 100.23(9) . 7_556 ?
O3 V1 O2 154.41(9) . 7_556 ?
O2 V1 O2 73.62(5) 1_545 7_556 ?
O2 V1 O2 73.62(5) . 7_556 ?
O3 Li O3 180.00(11) 5_556 1_554 ?
O3 Li O1 90.11(6) 5_556 3_444 ?
O3 Li O1 89.89(6) 1_554 3_444 ?
O3 Li O1 89.89(6) 5_556 7_556 ?
O3 Li O1 90.11(6) 1_554 7_556 ?
O1 Li O1 180.00(16) 3_444 7_556 ?
O3 Li O1 90.11(6) 5_556 3_454 ?
O3 Li O1 89.89(6) 1_554 3_454 ?
O1 Li O1 102.28(8) 3_444 3_454 ?
O1 Li O1 77.72(8) 7_556 3_454 ?
O3 Li O1 89.89(6) 5_556 7_546 ?
O3 Li O1 90.11(6) 1_554 7_546 ?
O1 Li O1 77.72(8) 3_444 7_546 ?
O1 Li O1 102.28(8) 7_556 7_546 ?
O1 Li O1 180.00(9) 3_454 7_546 ?
O3 Li Mo1 157.70(6) 5_556 1_554 ?
O3 Li Mo1 22.30(6) 1_554 1_554 ?
O1 Li Mo1 103.66(5) 3_444 1_554 ?
O1 Li Mo1 76.34(5) 7_556 1_554 ?
O1 Li Mo1 103.66(5) 3_454 1_554 ?
O1 Li Mo1 76.34(5) 7_546 1_554 ?
O3 Li Mo1 22.30(6) 5_556 5_556 ?
O3 Li Mo1 157.70(6) 1_554 5_556 ?
O1 Li Mo1 76.34(5) 3_444 5_556 ?
O1 Li Mo1 103.66(5) 7_556 5_556 ?
O1 Li Mo1 76.34(5) 3_454 5_556 ?
O1 Li Mo1 103.66(5) 7_546 5_556 ?
Mo1 Li Mo1 180.000(7) 1_554 5_556 ?
V1 O1 Li 121.51(6) . 3_556 ?
V1 O1 Li 121.51(6) . 3_546 ?
Li O1 Li 102.28(8) 3_556 3_546 ?
V1 O3 Li 130.88(12) . 1_556 ?
V1 O3 Mo1 102.96(10) . 5_556 ?
Li O3 Mo1 126.15(9) 1_556 5_556 ?
Mo1 O2 V1 0.00(2) 1_565 1_565 ?
Mo1 O2 V1 143.68(11) 1_565 . ?
V1 O2 V1 143.68(11) 1_565 . ?
Mo1 O2 Mo1 106.38(5) 1_565 7_556 ?
V1 O2 Mo1 106.38(5) 1_565 7_556 ?
V1 O2 Mo1 106.38(5) . 7_556 ?
Mo1 O2 V1 106.38(5) 1_565 7_556 ?
V1 O2 V1 106.38(5) 1_565 7_556 ?
V1 O2 V1 106.38(5) . 7_556 ?
Mo1 O2 V1 0.000(8) 7_556 7_556 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.086
