# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1851303'
_audit_update_record             
;
2018-06-24 deposited with the CCDC.
2018-09-06 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            'Gd2.28 Li1.16 Mo4 O16'
_chemical_formula_weight         1006.34

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_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+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   5.1932(8)
_cell_length_b                   5.1932(8)
_cell_length_c                   11.426(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     308.16(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    358
_cell_measurement_theta_min      4.2490
_cell_measurement_theta_max      32.4050

_exptl_crystal_description       block
_exptl_crystal_colour            color
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    5.423
_exptl_crystal_F_000             445
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.1600
_exptl_crystal_size_min          0.1600
_exptl_absorpt_coefficient_mu    16.124
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.25072
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            743
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.311
_diffrn_reflns_theta_max         24.948
_diffrn_reflns_theta_full        24.948
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             135
_reflns_number_gt                123
_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       
'CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015)'
_computing_cell_refinement       
'CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        
'CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015)'
_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)+(0.0911P)²+1.6373P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.037(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         135
_refine_ls_number_parameters     15
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0438
_refine_ls_wR_factor_ref         0.1475
_refine_ls_wR_factor_gt          0.1433
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_restrained_S_all      1.172
_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 0.5000 0.7500 0.1250 0.0111(11) Uani 1 4 d S T P . .
Gd1 Gd 1.0000 0.2500 0.1250 0.0070(10) Uani 0.572 4 d S T P . .
Li1 Li 1.0000 0.2500 0.1250 0.0070(10) Uani 0.286 4 d S T P . .
O1 O 0.7442(8) 0.5981(8) 0.0407(4) 0.0283(18) 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 0.0108(12) 0.0108(12) 0.0117(16) 0.000 0.000 0.000
Gd1 0.0080(12) 0.0080(12) 0.0051(15) 0.000 0.000 0.000
Li1 0.0080(12) 0.0080(12) 0.0051(15) 0.000 0.000 0.000
O1 0.034(3) 0.022(3) 0.030(3) 0.001(2) 0.0068(17) 0.0030(17)

_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 O1 1.777(4) . ?
Mo1 O1 1.777(4) 12_766 ?
Mo1 O1 1.777(4) 6_564 ?
Mo1 O1 1.777(4) 15_565 ?
Gd1 O1 2.441(4) . ?
Gd1 O1 2.441(4) 15_665 ?
Gd1 O1 2.441(4) 12_756 ?
Gd1 O1 2.441(4) 6_654 ?
Gd1 O1 2.444(4) 14_545 ?
Gd1 O1 2.444(4) 8_454 ?
Gd1 O1 2.444(4) 3_645 ?
Gd1 O1 2.444(4) 9_765 ?
Gd1 Gd1 3.8604(8) 13_755 ?
Gd1 Gd1 3.8604(8) 9_755 ?
Gd1 Gd1 3.8604(8) 9_765 ?
Gd1 Gd1 3.8604(8) 13_655 ?
O1 Li1 2.444(4) 9_765 ?
O1 Gd1 2.444(4) 9_765 ?

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 Mo1 O1 107.09(14) . 12_766 ?
O1 Mo1 O1 114.3(3) . 6_564 ?
O1 Mo1 O1 107.09(14) 12_766 6_564 ?
O1 Mo1 O1 107.09(14) . 15_565 ?
O1 Mo1 O1 114.3(3) 12_766 15_565 ?
O1 Mo1 O1 107.09(14) 6_564 15_565 ?
O1 Gd1 O1 98.96(8) . 15_665 ?
O1 Gd1 O1 98.96(8) . 12_756 ?
O1 Gd1 O1 133.5(2) 15_665 12_756 ?
O1 Gd1 O1 133.5(2) . 6_654 ?
O1 Gd1 O1 98.96(8) 15_665 6_654 ?
O1 Gd1 O1 98.96(8) 12_756 6_654 ?
O1 Gd1 O1 68.75(10) . 14_545 ?
O1 Gd1 O1 152.12(19) 15_665 14_545 ?
O1 Gd1 O1 74.18(9) 12_756 14_545 ?
O1 Gd1 O1 75.59(15) 6_654 14_545 ?
O1 Gd1 O1 74.18(9) . 8_454 ?
O1 Gd1 O1 68.74(10) 15_665 8_454 ?
O1 Gd1 O1 75.59(15) 12_756 8_454 ?
O1 Gd1 O1 152.12(19) 6_654 8_454 ?
O1 Gd1 O1 126.88(13) 14_545 8_454 ?
O1 Gd1 O1 152.12(19) . 3_645 ?
O1 Gd1 O1 75.59(15) 15_665 3_645 ?
O1 Gd1 O1 68.74(10) 12_756 3_645 ?
O1 Gd1 O1 74.18(9) 6_654 3_645 ?
O1 Gd1 O1 126.88(13) 14_545 3_645 ?
O1 Gd1 O1 78.4(2) 8_454 3_645 ?
O1 Gd1 O1 75.59(15) . 9_765 ?
O1 Gd1 O1 74.18(9) 15_665 9_765 ?
O1 Gd1 O1 152.12(19) 12_756 9_765 ?
O1 Gd1 O1 68.74(10) 6_654 9_765 ?
O1 Gd1 O1 78.4(2) 14_545 9_765 ?
O1 Gd1 O1 126.88(13) 8_454 9_765 ?
O1 Gd1 O1 126.88(13) 3_645 9_765 ?
O1 Gd1 Gd1 131.15(10) . 13_755 ?
O1 Gd1 Gd1 37.82(10) 15_665 13_755 ?
O1 Gd1 Gd1 101.89(11) 12_756 13_755 ?
O1 Gd1 Gd1 85.75(10) 6_654 13_755 ?
O1 Gd1 Gd1 159.88(9) 14_545 13_755 ?
O1 Gd1 Gd1 69.14(10) 8_454 13_755 ?
O1 Gd1 Gd1 37.77(10) 3_645 13_755 ?
O1 Gd1 Gd1 101.98(11) 9_765 13_755 ?
O1 Gd1 Gd1 101.89(11) . 9_755 ?
O1 Gd1 Gd1 131.15(10) 15_665 9_755 ?
O1 Gd1 Gd1 85.75(10) 12_756 9_755 ?
O1 Gd1 Gd1 37.82(10) 6_654 9_755 ?
O1 Gd1 Gd1 37.77(9) 14_545 9_755 ?
O1 Gd1 Gd1 159.88(9) 8_454 9_755 ?
O1 Gd1 Gd1 101.98(11) 3_645 9_755 ?
O1 Gd1 Gd1 69.14(10) 9_765 9_755 ?
Gd1 Gd1 Gd1 123.200(12) 13_755 9_755 ?
O1 Gd1 Gd1 37.82(10) . 9_765 ?
O1 Gd1 Gd1 85.75(10) 15_665 9_765 ?
O1 Gd1 Gd1 131.15(10) 12_756 9_765 ?
O1 Gd1 Gd1 101.89(11) 6_654 9_765 ?
O1 Gd1 Gd1 69.14(10) 14_545 9_765 ?
O1 Gd1 Gd1 101.98(11) 8_454 9_765 ?
O1 Gd1 Gd1 159.88(9) 3_645 9_765 ?
O1 Gd1 Gd1 37.77(9) 9_765 9_765 ?
Gd1 Gd1 Gd1 123.200(12) 13_755 9_765 ?
Gd1 Gd1 Gd1 84.54(2) 9_755 9_765 ?
O1 Gd1 Gd1 85.75(10) . 13_655 ?
O1 Gd1 Gd1 101.89(11) 15_665 13_655 ?
O1 Gd1 Gd1 37.82(10) 12_756 13_655 ?
O1 Gd1 Gd1 131.15(10) 6_654 13_655 ?
O1 Gd1 Gd1 101.98(11) 14_545 13_655 ?
O1 Gd1 Gd1 37.77(10) 8_454 13_655 ?
O1 Gd1 Gd1 69.14(10) 3_645 13_655 ?
O1 Gd1 Gd1 159.88(9) 9_765 13_655 ?
Gd1 Gd1 Gd1 84.54(2) 13_755 13_655 ?
Gd1 Gd1 Gd1 123.200(12) 9_755 13_655 ?
Gd1 Gd1 Gd1 123.200(12) 9_765 13_655 ?
Mo1 O1 Gd1 120.2(2) . . ?
Mo1 O1 Li1 131.6(2) . 9_765 ?
Gd1 O1 Li1 104.4 . 9_765 ?
Mo1 O1 Gd1 131.6(2) . 9_765 ?
Gd1 O1 Gd1 104.41(15) . 9_765 ?
Li1 O1 Gd1 0.0 9_765 9_765 ?

_refine_diff_density_max         1.257
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.358

_shelx_res_file                  
;

    1.res created by SHELXL-2014/7


TITL 1 in I4(1)/a
CELL 0.71073   5.1932   5.1932  11.4263  90.000  90.000  90.000
ZERR   1.00   0.0008   0.0008   0.0038   0.000   0.000   0.000
LATT  2
SYMM 0.5-X, -Y, 0.5+Z
SYMM 0.75-Y, 0.25+X, 0.25+Z
SYMM 0.75+Y, 0.75-X, 0.75+Z
SFAC LI O MO GD
UNIT 1.16 16 4 2.28
L.S. 100
BOND
ACTA
FMAP 2
OMIT -1 50
eadp  GD1 LI1
exyz  GD1 LI1
PLAN 20
WGHT    0.091100    1.637300
EXTI    0.037218
FVAR       0.17817
MO1   3    0.500000    0.750000    0.125000    10.25000    0.01081    0.01081 =
         0.01166    0.00000    0.00000    0.00000
GD1   4    1.000000    0.250000    0.125000    10.14300    0.00804    0.00804 =
         0.00507    0.00000    0.00000    0.00000
LI1   1    1.000000    0.250000    0.125000    10.07150    0.00804    0.00804 =
         0.00507    0.00000    0.00000    0.00000
O1    2    0.744159    0.598073    0.040686    11.00000    0.03371    0.02155 =
         0.02952    0.00118    0.00675    0.00299

HKLF 4

REM  1 in I4(1)/a
REM R1 =  0.0438 for     123 Fo > 4sig(Fo)  and  0.0452 for all     135 data
REM     15 parameters refined using      0 restraints

END

WGHT      0.0926      1.5461

REM Highest difference peak  1.257,  deepest hole -1.617,  1-sigma level  0.358
Q1    1   1.0699  0.4344  0.1246  11.00000  0.05    1.26
Q2    1   0.4568  0.5527  0.1248  11.00000  0.05    1.10
Q3    1   0.7596  0.3994  0.0438  11.00000  0.05    0.81
Q4    1   0.8722  0.7999  0.1205  11.00000  0.05    0.55
Q5    1   0.8899  0.5064 -0.0423  11.00000  0.05    0.45
Q6    1   0.7845  0.7618  0.0426  11.00000  0.05    0.41
Q7    1   0.9725  0.6288  0.1322  11.00000  0.05    0.39
Q8    1   0.6892  0.7503  0.0194  11.00000  0.05    0.37
Q9    1   0.5973  0.4866 -0.0404  11.00000  0.05    0.34
Q10   1   0.9816  0.5613 -0.0246  11.00000  0.05    0.33
Q11   1   0.5274  0.3862  0.0426  11.00000  0.05    0.27
Q12   1   0.7366  0.7265 -0.0395  11.00000  0.05    0.26
Q13   1   0.7897  0.5516  0.1261  11.00000  0.05    0.25
;
_shelx_res_checksum              6464
