# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1565724'
_audit_update_record             
;
2017-07-31 deposited with the CCDC.
2017-08-28 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            'Ag3 I3 Mo2 O12'
_chemical_formula_weight         1088.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

_cell_length_a                   8.0072(2)
_cell_length_b                   21.2678(6)
_cell_length_c                   7.3241(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1247.26(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4094
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      27.56

_exptl_crystal_description       needle-shaped
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    5.795
_exptl_crystal_F_000             1920
_exptl_transmission_factor_min   0.1653
_exptl_transmission_factor_max   0.3336
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    14.066
_shelx_estimated_absorpt_T_min   0.165
_shelx_estimated_absorpt_T_max   0.334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_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       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6030
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.915
_diffrn_reflns_theta_max         27.564
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2696
_reflns_number_gt                2647
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_max     0.984
_reflns_Friedel_fraction_full    1.000

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion 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)+(0.0130P)²+2.4780P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00117(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.59(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2696
_refine_ls_number_parameters     183
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0180
_refine_ls_wR_factor_ref         0.0387
_refine_ls_wR_factor_gt          0.0384
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.001
_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
I1 I 0.64127(6) 0.26227(2) 0.36806(8) 0.01021(11) Uani 1 1 d . . . . .
I2 I 0.68255(6) 0.28190(2) -0.13384(8) 0.01071(11) Uani 1 1 d . . . . .
I3 I 0.87473(7) 0.00015(3) 0.29560(11) 0.02128(12) Uani 1 1 d . . . . .
Mo1 Mo 0.48797(10) 0.12265(3) 0.54221(10) 0.00927(14) Uani 1 1 d . . . . .
Mo2 Mo 0.49379(10) 0.12381(3) 0.04171(11) 0.00951(14) Uani 1 1 d . . . . .
Ag1 Ag 1.00048(12) 0.09797(4) 0.54037(12) 0.02809(18) Uani 1 1 d . . . . .
Ag2 Ag 1.21679(9) -0.00617(4) 0.28895(14) 0.02909(17) Uani 1 1 d . . . . .
Ag3 Ag 0.98826(11) 0.10171(5) 0.09267(12) 0.0329(2) Uani 1 1 d . . . . .
O1 O 0.5265(6) 0.1526(2) 0.2878(8) 0.0131(11) Uani 1 1 d . . . . .
O2 O 0.4102(6) 0.1345(2) 0.7879(8) 0.0115(11) Uani 1 1 d . . . . .
O3 O 0.5114(7) 0.3342(3) -0.1799(9) 0.0206(13) Uani 1 1 d . . . . .
O4 O 0.7402(7) 0.3263(3) 0.4969(7) 0.0139(13) Uani 1 1 d . . . . .
O5 O 0.5771(8) 0.2210(3) 0.5797(7) 0.0153(13) Uani 1 1 d . . . . .
O6 O 0.3843(8) 0.0561(3) 0.4810(8) 0.0184(14) Uani 1 1 d . . . . .
O7 O 0.6835(9) 0.0961(3) 0.5921(8) 0.0198(15) Uani 1 1 d . . . . .
O8 O 0.4481(7) 0.3037(3) 0.3303(8) 0.0194(14) Uani 1 1 d . . . . .
O9 O 0.5660(9) 0.2243(3) -0.0030(8) 0.0233(16) Uani 1 1 d . . . . .
O10 O 0.3959(9) 0.0555(3) 0.0929(8) 0.0188(14) Uani 1 1 d . . . . .
O11 O 0.6911(8) 0.1001(4) -0.0193(8) 0.0223(15) Uani 1 1 d . . . . .
O12 O 0.7502(8) 0.3246(3) 0.0753(7) 0.0160(14) Uani 1 1 d . . . . .


_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
I1 O8 1.802(5) . ?
I1 O4 1.836(6) . ?
I1 O5 1.854(6) . ?
I2 O3 1.797(5) . ?
I2 O9 1.813(6) . ?
I2 O12 1.862(5) . ?
I3 Ag2 2.7427(9) . ?
I3 Ag3 2.7750(11) . ?
I3 Ag1 2.9251(11) . ?
I3 Ag1 2.9746(11) 2_754 ?
I3 Ag3 3.2605(12) 2_755 ?
Mo1 O6 1.700(6) . ?
Mo1 O7 1.704(7) . ?
Mo1 O2 1.921(6) . ?
Mo1 O1 1.993(6) . ?
Mo1 O5 2.227(6) . ?
Mo1 O4 2.286(6) 3_455 ?
Mo2 O10 1.693(7) . ?
Mo2 O11 1.718(6) . ?
Mo2 O1 1.922(6) . ?
Mo2 O2 1.989(6) 1_554 ?
Mo2 O9 2.239(6) . ?
Mo2 O12 2.251(7) 3_455 ?
Ag1 O3 2.507(6) 3_556 ?
Ag1 O4 2.526(6) 3 ?
Ag1 O7 2.566(7) . ?
Ag1 I3 2.9746(11) 2_755 ?
Ag1 Ag2 3.1864(12) 2_755 ?
Ag1 Ag3 3.2814(11) . ?
Ag1 Ag2 3.3610(12) . ?
Ag2 O6 2.352(6) 1_655 ?
Ag2 O10 2.417(6) 1_655 ?
Ag2 O7 2.525(7) 2_754 ?
Ag2 O11 2.550(7) 2_755 ?
Ag2 Ag1 3.1865(12) 2_754 ?
Ag2 Ag3 3.2680(12) . ?
Ag3 O3 2.424(6) 3 ?
Ag3 O11 2.517(7) . ?
Ag3 I3 3.2606(12) 2_754 ?
O2 Mo2 1.989(6) 1_556 ?
O3 Ag3 2.425(6) 3_455 ?
O3 Ag1 2.507(6) 3_454 ?
O4 Mo1 2.286(6) 3 ?
O4 Ag1 2.526(6) 3_455 ?
O6 Ag2 2.352(6) 1_455 ?
O7 Ag2 2.524(7) 2_755 ?
O10 Ag2 2.417(6) 1_455 ?
O11 Ag2 2.550(7) 2_754 ?
O12 Mo2 2.251(7) 3 ?

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
O8 I1 O4 94.9(3) . . ?
O8 I1 O5 97.0(3) . . ?
O4 I1 O5 92.3(3) . . ?
O3 I2 O9 97.2(3) . . ?
O3 I2 O12 94.3(3) . . ?
O9 I2 O12 92.6(3) . . ?
Ag2 I3 Ag3 72.63(3) . . ?
Ag2 I3 Ag1 72.66(3) . . ?
Ag3 I3 Ag1 70.24(3) . . ?
Ag2 I3 Ag1 67.60(3) . 2_754 ?
Ag3 I3 Ag1 95.71(3) . 2_754 ?
Ag1 I3 Ag1 140.22(2) . 2_754 ?
Ag2 I3 Ag3 69.10(3) . 2_755 ?
Ag3 I3 Ag3 139.85(2) . 2_755 ?
Ag1 I3 Ag3 87.00(3) . 2_755 ?
Ag1 I3 Ag3 80.80(3) 2_754 2_755 ?
O6 Mo1 O7 103.3(3) . . ?
O6 Mo1 O2 101.4(2) . . ?
O7 Mo1 O2 98.1(3) . . ?
O6 Mo1 O1 95.5(3) . . ?
O7 Mo1 O1 99.4(3) . . ?
O2 Mo1 O1 152.2(2) . . ?
O6 Mo1 O5 166.0(3) . . ?
O7 Mo1 O5 89.5(3) . . ?
O2 Mo1 O5 82.3(2) . . ?
O1 Mo1 O5 76.4(2) . . ?
O6 Mo1 O4 86.2(3) . 3_455 ?
O7 Mo1 O4 170.4(3) . 3_455 ?
O2 Mo1 O4 78.0(2) . 3_455 ?
O1 Mo1 O4 81.2(2) . 3_455 ?
O5 Mo1 O4 81.3(2) . 3_455 ?
O10 Mo2 O11 103.4(4) . . ?
O10 Mo2 O1 97.4(3) . . ?
O11 Mo2 O1 102.3(3) . . ?
O10 Mo2 O2 98.6(3) . 1_554 ?
O11 Mo2 O2 95.7(2) . 1_554 ?
O1 Mo2 O2 152.4(2) . 1_554 ?
O10 Mo2 O9 166.3(3) . . ?
O11 Mo2 O9 90.3(3) . . ?
O1 Mo2 O9 78.3(2) . . ?
O2 Mo2 O9 80.9(2) 1_554 . ?
O10 Mo2 O12 89.6(3) . 3_455 ?
O11 Mo2 O12 165.6(3) . 3_455 ?
O1 Mo2 O12 82.0(2) . 3_455 ?
O2 Mo2 O12 75.8(2) 1_554 3_455 ?
O9 Mo2 O12 77.0(3) . 3_455 ?
O3 Ag1 O4 73.11(18) 3_556 3 ?
O3 Ag1 O7 85.6(2) 3_556 . ?
O4 Ag1 O7 141.3(2) 3 . ?
O3 Ag1 I3 157.23(13) 3_556 . ?
O4 Ag1 I3 129.65(13) 3 . ?
O7 Ag1 I3 74.87(15) . . ?
O3 Ag1 I3 83.01(14) 3_556 2_755 ?
O4 Ag1 I3 105.75(13) 3 2_755 ?
O7 Ag1 I3 103.21(15) . 2_755 ?
I3 Ag1 I3 90.10(2) . 2_755 ?
O3 Ag1 Ag2 84.53(13) 3_556 2_755 ?
O4 Ag1 Ag2 151.36(13) 3 2_755 ?
O7 Ag1 Ag2 50.67(15) . 2_755 ?
I3 Ag1 Ag2 74.12(3) . 2_755 ?
I3 Ag1 Ag2 52.73(2) 2_755 2_755 ?
O3 Ag1 Ag3 143.48(14) 3_556 . ?
O4 Ag1 Ag3 83.19(13) 3 . ?
O7 Ag1 Ag3 96.80(14) . . ?
I3 Ag1 Ag3 52.74(3) . . ?
I3 Ag1 Ag3 130.92(4) 2_755 . ?
Ag2 Ag1 Ag3 124.72(4) 2_755 . ?
O3 Ag1 Ag2 143.98(14) 3_556 . ?
O4 Ag1 Ag2 87.70(13) 3 . ?
O7 Ag1 Ag2 125.47(16) . . ?
I3 Ag1 Ag2 51.16(2) . . ?
I3 Ag1 Ag2 73.07(3) 2_755 . ?
Ag2 Ag1 Ag2 100.99(2) 2_755 . ?
Ag3 Ag1 Ag2 58.93(3) . . ?
O6 Ag2 O10 73.21(19) 1_655 1_655 ?
O6 Ag2 O7 126.0(2) 1_655 2_754 ?
O10 Ag2 O7 83.4(2) 1_655 2_754 ?
O6 Ag2 O11 87.0(2) 1_655 2_755 ?
O10 Ag2 O11 125.5(2) 1_655 2_755 ?
O7 Ag2 O11 68.27(19) 2_754 2_755 ?
O6 Ag2 I3 122.09(16) 1_655 . ?
O10 Ag2 I3 125.21(16) 1_655 . ?
O7 Ag2 I3 111.28(16) 2_754 . ?
O11 Ag2 I3 108.51(15) 2_755 . ?
O6 Ag2 Ag1 176.50(17) 1_655 2_754 ?
O10 Ag2 Ag1 108.49(15) 1_655 2_754 ?
O7 Ag2 Ag1 51.84(16) 2_754 2_754 ?
O11 Ag2 Ag1 89.58(16) 2_755 2_754 ?
I3 Ag2 Ag1 59.67(3) . 2_754 ?
O6 Ag2 Ag3 100.77(17) 1_655 . ?
O10 Ag2 Ag3 71.93(16) 1_655 . ?
O7 Ag2 Ag3 117.24(15) 2_754 . ?
O11 Ag2 Ag3 162.54(15) 2_755 . ?
I3 Ag2 Ag3 54.14(2) . . ?
Ag1 Ag2 Ag3 82.71(3) 2_754 . ?
O6 Ag2 Ag1 66.11(16) 1_655 . ?
O10 Ag2 Ag1 105.88(16) 1_655 . ?
O7 Ag2 Ag1 167.17(16) 2_754 . ?
O11 Ag2 Ag1 111.31(14) 2_755 . ?
I3 Ag2 Ag1 56.17(2) . . ?
Ag1 Ag2 Ag1 115.82(2) 2_754 . ?
Ag3 Ag2 Ag1 59.32(2) . . ?
O3 Ag3 O11 79.1(2) 3 . ?
O3 Ag3 I3 154.64(14) 3 . ?
O11 Ag3 I3 81.61(16) . . ?
O3 Ag3 I3 78.36(14) 3 2_754 ?
O11 Ag3 I3 95.24(15) . 2_754 ?
I3 Ag3 I3 87.16(3) . 2_754 ?
O3 Ag3 Ag2 135.57(14) 3 . ?
O11 Ag3 Ag2 131.53(17) . . ?
I3 Ag3 Ag2 53.23(2) . . ?
I3 Ag3 Ag2 68.82(3) 2_754 . ?
O3 Ag3 Ag1 146.54(14) 3 . ?
O11 Ag3 Ag1 110.71(14) . . ?
I3 Ag3 Ag1 57.02(3) . . ?
I3 Ag3 Ag1 129.84(4) 2_754 . ?
Ag2 Ag3 Ag1 61.75(3) . . ?
Mo2 O1 Mo1 138.9(3) . . ?
Mo1 O2 Mo2 138.8(3) . 1_556 ?
I2 O3 Ag3 104.6(3) . 3_455 ?
I2 O3 Ag1 122.4(3) . 3_454 ?
Ag3 O3 Ag1 110.3(2) 3_455 3_454 ?
I1 O4 Mo1 143.2(3) . 3 ?
I1 O4 Ag1 102.1(3) . 3_455 ?
Mo1 O4 Ag1 109.8(2) 3 3_455 ?
I1 O5 Mo1 115.5(3) . . ?
Mo1 O6 Ag2 154.8(4) . 1_455 ?
Mo1 O7 Ag2 131.6(4) . 2_755 ?
Mo1 O7 Ag1 150.7(4) . . ?
Ag2 O7 Ag1 77.5(2) 2_755 . ?
I2 O9 Mo2 148.7(4) . . ?
Mo2 O10 Ag2 150.7(4) . 1_455 ?
Mo2 O11 Ag3 141.3(3) . . ?
Mo2 O11 Ag2 129.7(4) . 2_754 ?
Ag3 O11 Ag2 85.2(2) . 2_754 ?
I2 O12 Mo2 113.6(3) . 3 ?

_refine_diff_density_max         0.799
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.155

