# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2011

 
data_jpPass1

_publ_section_references
;
Bruker (2006). SAINT. Version 7.23A. Bruker AXS Inc., Madison, Wisconsin,
USA.

Bruker (1999). SMART. Version 5.054. Bruker AXS Inc., Madison, Wisconsin,
USA.

Sheldrick, G.M. (2000). SHELXTL. Version 6.14. Bruker AXS Inc., Madison,
Wisconsin, USA.

Sheldrick, G.M. (1997). SHELXL97 & SHELXS97. University of Gottingen,
Germany.

Sheldrick, G.M. (1997b). SADABS. Version 2.10. Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_publ_section_exptl_refinement
;
?
;
_publ_requested_journal          'Dalton Transactions'
_publ_contact_author_name        'Andreas Decken'
_publ_contact_author_address     
;Department of Chemistry
University of New Brunswick
Fredericton, NB
E3B 6E2
Canada
;
_publ_contact_author_email       adecken@unb.ca
_publ_contact_author_phone       '(506) 453-4875'
_publ_contact_author_fax         '(506) 453-4981'
loop_
_publ_author_name
_publ_author_address
'Andreas Decken'
;Department of Chemistry
University of New Brunswick
Fredericton, NB
E3B 6E2
Canada
;
'Jack Passmore'
;Department of Chemistry
University of New Brunswick
Fredericton, NB
E3B 6E2
Canada
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ag2 F60 O16 S2 Sb2 Se6 Te12'
_chemical_formula_weight         3924.32

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P a -3'
_symmetry_int_tables_number      205

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

_cell_length_a                   19.1532(2)
_cell_length_b                   19.1532(2)
_cell_length_c                   19.1532(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7026.26(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    213(1)

_exptl_crystal_description       Cube
_exptl_crystal_colour            Yellow-orange
_exptl_crystal_size_max          0.40 
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.35
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6894.4
_exptl_absorpt_coefficient_mu    9.565
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min  0.01671
_exptl_absorpt_correction_T_max  0.03564
_exptl_absorpt_process_details  'SADABS (Sheldrick, 1997b)'

_exptl_special_details           
; 
Crystal decay was monitored by repeating the initial 50 frames
at the end of the data collection and analyzing duplicate
reflections.
;

_diffrn_ambient_temperature      213(1)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode'
_diffrn_source_type              Siemens-RA
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_%       0
_diffrn_reflns_number            40218
_diffrn_reflns_av_R_equivalents  0.0998
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         24.98
_reflns_number_total             2072
_reflns_number_gt                1718
_reflns_threshold_expression    'I > 2σ(I)'

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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.
 Atoms F3 and F2A, F3A, F4A show high ADP ratios due to the rotational disorder. 
 Only two disorder sites are resolved. Therefore the Ueq comparison between Te1 
 and the neighbours failes.
;

_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)+(0.0213P)²+66.4006P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2072
_refine_ls_number_parameters     200
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.0852
_refine_ls_wR_factor_gt          0.0802
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_restrained_S_all      1.176
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Se Se 0.07997(6) 0.56959(7) 0.53791(6) 0.0541(3) Uani 1 1 d . . .
Ag Ag 0.07608(6) 0.42392(6) 0.57608(6) 0.0894(7) Uani 1 3 d S . .
Sb Sb 0.35783(3) 0.14217(3) 0.85783(3) 0.0299(3) Uani 1 3 d S . .
S S 0.1768(2) 0.3232(2) 0.6768(2) 0.102(3) Uani 1 3 d SD . .
O1 O 0.4511(3) 0.1675(4) 0.8905(4) 0.0461(18) Uani 1 1 d . . .
O2 O 0.3835(4) 0.1748(4) 0.7655(4) 0.053(2) Uani 1 1 d . . .
O3 O 0.1107(14) 0.349(3) 0.660(3) 0.14(2) Uani 0.33 1 d PD . .
O4 O 0.1961(17) 0.2929(14) 0.6137(12) 0.124(16) Uani 0.33 1 d PD . .
Te1 Te 0.41656(5) 0.25093(4) 0.71750(4) 0.0538(3) Uani 1 1 d . . .
Te2 Te 0.49561(4) 0.20335(4) 0.96653(4) 0.0472(2) Uani 1 1 d . . .
F1 F 0.4467(6) 0.3228(4) 0.6642(4) 0.109(4) Uani 1 1 d . . .
F2 F 0.5066(9) 0.2219(14) 0.7290(16) 0.18(2) Uani 0.60 1 d PD . .
F3 F 0.4081(12) 0.2000(8) 0.6394(8) 0.170(19) Uani 0.60 1 d PD . .
F4 F 0.3308(11) 0.2830(11) 0.7061(12) 0.122(11) Uani 0.60 1 d PD . .
F5 F 0.4261(10) 0.3050(8) 0.7939(9) 0.082(6) Uani 0.60 1 d PD . .
F2A F 0.4676(11) 0.2040(17) 0.6743(12) 0.23(4) Uani 0.40 1 d PD . .
F3A F 0.354(2) 0.240(2) 0.6565(17) 0.37(7) Uani 0.40 1 d PD . .
F4A F 0.3675(16) 0.3107(19) 0.7575(16) 0.38(6) Uani 0.40 1 d PD . .
F5A F 0.4790(18) 0.2679(19) 0.7715(19) 0.35(6) Uani 0.40 1 d PD . .
F6 F 0.5430(4) 0.2434(5) 1.0394(4) 0.095(3) Uani 1 1 d . . .
F7 F 0.5787(4) 0.1869(5) 0.9241(5) 0.098(3) Uani 1 1 d . . .
F8 F 0.5002(5) 0.1211(4) 1.0109(4) 0.098(3) Uani 1 1 d . . .
F9 F 0.4165(4) 0.2257(4) 1.0133(4) 0.076(2) Uani 1 1 d . . .
F10 F 0.4940(5) 0.2913(4) 0.9280(5) 0.096(3) 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
Se Se 2.3463(15) 24_556 ?
Se Se 2.3464(15) 18_665 ?
Se Ag 2.8853(19) . ?
Ag O3 2.26(3) 6_456 ?
Ag O3 2.26(3) 12_565 ?
Ag O3 2.26(3) . ?
Ag Se 2.8853(19) 6_456 ?
Ag Se 2.8853(19) 12_565 ?
Sb O2 1.939(7) 6_456 ?
Sb O2 1.939(7) . ?
Sb O2 1.939(7) 12_565 ?
Sb O1 1.954(6) 6_456 ?
Sb O1 1.954(6) . ?
Sb O1 1.954(6) 12_565 ?
S O4 1.390(19) . ?
S O4 1.390(19) 6_456 ?
S O4 1.390(19) 12_565 ?
S O3 1.395(19) . ?
S O3 1.395(19) 12_565 ?
S O3 1.395(19) 6_456 ?
O1 Te2 1.822(7) . ?
O2 Te1 1.836(7) . ?
O3 O3 1.23(6) 6_456 ?
O3 O3 1.23(6) 12_565 ?
O3 O4 1.25(4) 6_456 ?
O4 O3 1.25(4) 12_565 ?
Te1 F2A 1.57(2) . ?
Te1 F5A 1.61(4) . ?
Te1 F4A 1.67(4) . ?
Te1 F3A 1.69(4) . ?
Te1 F4 1.768(17) . ?
Te1 F3 1.794(13) . ?
Te1 F5 1.802(14) . ?
Te1 F1 1.808(7) . ?
Te1 F2 1.826(19) . ?
Te2 F8 1.793(8) . ?
Te2 F9 1.812(7) . ?
Te2 F7 1.815(7) . ?
Te2 F6 1.832(7) . ?
Te2 F10 1.839(8) . ?
F2 F5A 1.312(15) . ?
F2 F2A 1.331(15) . ?
F3 F2A 1.323(15) . ?
F3 F3A 1.336(15) . ?
F4 F4A 1.321(15) . ?
F4 F3A 1.329(15) . ?
F5 F5A 1.310(15) . ?
F5 F4A 1.325(15) . ?

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
Se Se Se 100.91(7) 24_556 18_665 ?
Se Se Ag 89.52(4) 24_556 . ?
Se Se Ag 89.52(4) 18_665 . ?
O3 Ag O3 31.7(13) 6_456 12_565 ?
O3 Ag O3 31.7(13) 6_456 . ?
O3 Ag O3 31.7(13) 12_565 . ?
O3 Ag Se 142.3(17) 6_456 6_456 ?
O3 Ag Se 115.3(8) 12_565 6_456 ?
O3 Ag Se 138.1(18) . 6_456 ?
O3 Ag Se 115.3(8) 6_456 . ?
O3 Ag Se 138.1(18) 12_565 . ?
O3 Ag Se 142.3(17) . . ?
Se Ag Se 77.67(6) 6_456 . ?
O3 Ag Se 138.1(18) 6_456 12_565 ?
O3 Ag Se 142.3(17) 12_565 12_565 ?
O3 Ag Se 115.3(8) . 12_565 ?
Se Ag Se 77.67(6) 6_456 12_565 ?
Se Ag Se 77.67(6) . 12_565 ?
O2 Sb O2 91.1(3) 6_456 . ?
O2 Sb O2 91.1(3) 6_456 12_565 ?
O2 Sb O2 91.1(3) . 12_565 ?
O2 Sb O1 88.8(3) 6_456 6_456 ?
O2 Sb O1 89.3(3) . 6_456 ?
O2 Sb O1 179.6(3) 12_565 6_456 ?
O2 Sb O1 179.6(3) 6_456 . ?
O2 Sb O1 88.8(3) . . ?
O2 Sb O1 89.3(3) 12_565 . ?
O1 Sb O1 90.8(3) 6_456 . ?
O2 Sb O1 89.3(3) 6_456 12_565 ?
O2 Sb O1 179.6(3) . 12_565 ?
O2 Sb O1 88.8(3) 12_565 12_565 ?
O1 Sb O1 90.8(3) 6_456 12_565 ?
O1 Sb O1 90.8(3) . 12_565 ?
O4 S O4 118.8(5) . 6_456 ?
O4 S O4 118.8(5) . 12_565 ?
O4 S O4 118.8(5) 6_456 12_565 ?
O4 S O3 100(3) . . ?
O4 S O3 53.2(18) 6_456 . ?
O4 S O3 98(3) 12_565 . ?
O4 S O3 53.2(18) . 12_565 ?
O4 S O3 98(3) 6_456 12_565 ?
O4 S O3 100(3) 12_565 12_565 ?
O3 S O3 52(3) . 12_565 ?
O4 S O3 98(3) . 6_456 ?
O4 S O3 100(3) 6_456 6_456 ?
O4 S O3 53.2(18) 12_565 6_456 ?
O3 S O3 52(3) . 6_456 ?
O3 S O3 52(3) 12_565 6_456 ?
Te2 O1 Sb 141.0(4) . . ?
Te1 O2 Sb 143.2(4) . . ?
O3 O3 O3 60.000(10) 6_456 12_565 ?
O3 O3 O4 120(4) 6_456 6_456 ?
O3 O3 O4 116(4) 12_565 6_456 ?
O3 O3 S 63.8(13) 6_456 . ?
O3 O3 S 63.8(13) 12_565 . ?
O4 O3 S 63.2(14) 6_456 . ?
O3 O3 Ag 74.2(7) 6_456 . ?
O3 O3 Ag 74.2(7) 12_565 . ?
O4 O3 Ag 166(3) 6_456 . ?
S O3 Ag 131(2) . . ?
O3 O4 S 63.6(15) 12_565 . ?
F2A Te1 F5A 89.5(9) . . ?
F2A Te1 F4A 171.7(17) . . ?
F5A Te1 F4A 89.1(8) . . ?
F2A Te1 F3A 90.5(8) . . ?
F5A Te1 F3A 174(2) . . ?
F4A Te1 F3A 90.0(8) . . ?
F2A Te1 F4 135.7(9) . . ?
F5A Te1 F4 134.2(9) . . ?
F4A Te1 F4 45.1(6) . . ?
F3A Te1 F4 45.2(6) . . ?
F2A Te1 F3 45.8(6) . . ?
F5A Te1 F3 135.3(8) . . ?
F4A Te1 F3 134.9(8) . . ?
F3A Te1 F3 45.0(6) . . ?
F4 Te1 F3 90.2(8) . . ?
F2A Te1 F5 134.2(9) . . ?
F5A Te1 F5 44.7(6) . . ?
F4A Te1 F5 44.7(5) . . ?
F3A Te1 F5 134.7(8) . . ?
F4 Te1 F5 89.7(7) . . ?
F3 Te1 F5 177.7(8) . . ?
F2A Te1 F1 86.6(11) . . ?
F5A Te1 F1 88.4(15) . . ?
F4A Te1 F1 85.2(12) . . ?
F3A Te1 F1 85.9(16) . . ?
F4 Te1 F1 87.9(9) . . ?
F3 Te1 F1 88.4(6) . . ?
F5 Te1 F1 89.3(6) . . ?
F2A Te1 F2 45.4(6) . . ?
F5A Te1 F2 44.3(6) . . ?
F4A Te1 F2 133.3(8) . . ?
F3A Te1 F2 135.9(8) . . ?
F4 Te1 F2 177.4(11) . . ?
F3 Te1 F2 91.1(7) . . ?
F5 Te1 F2 89.0(7) . . ?
F1 Te1 F2 89.9(10) . . ?
F2A Te1 O2 91.4(11) . . ?
F5A Te1 O2 95.4(15) . . ?
F4A Te1 O2 97.0(12) . . ?
F3A Te1 O2 90.3(16) . . ?
F4 Te1 O2 91.0(9) . . ?
F3 Te1 O2 87.4(6) . . ?
F5 Te1 O2 94.9(6) . . ?
F1 Te1 O2 175.7(4) . . ?
F2 Te1 O2 91.3(10) . . ?
F8 Te2 F9 90.8(4) . . ?
F8 Te2 F7 91.0(5) . . ?
F9 Te2 F7 175.0(4) . . ?
F8 Te2 O1 94.1(4) . . ?
F9 Te2 O1 95.3(3) . . ?
F7 Te2 O1 89.3(3) . . ?
F8 Te2 F6 89.0(4) . . ?
F9 Te2 F6 86.5(3) . . ?
F7 Te2 F6 88.8(4) . . ?
O1 Te2 F6 176.4(4) . . ?
F8 Te2 F10 175.0(4) . . ?
F9 Te2 F10 88.2(4) . . ?
F7 Te2 F10 89.7(5) . . ?
O1 Te2 F10 90.9(4) . . ?
F6 Te2 F10 86.0(4) . . ?
F5A F2 F2A 116(3) . . ?
F5A F2 Te1 59(2) . . ?
F2A F2 Te1 56.9(13) . . ?
F2A F3 F3A 121(3) . . ?
F2A F3 Te1 57.9(12) . . ?
F3A F3 Te1 63.2(19) . . ?
F4A F4 F3A 127(3) . . ?
F4A F4 Te1 63.4(19) . . ?
F3A F4 Te1 64(2) . . ?
F5A F5 F4A 122(3) . . ?
F5A F5 Te1 60(2) . . ?
F4A F5 Te1 62.3(19) . . ?
F3 F2A F2 154(2) . . ?
F3 F2A Te1 76.3(12) . . ?
F2 F2A Te1 77.7(15) . . ?
F4 F3A F3 142(3) . . ?
F4 F3A Te1 71(2) . . ?
F3 F3A Te1 71.8(17) . . ?
F4 F4A F5 144(3) . . ?
F4 F4A Te1 71.5(18) . . ?
F5 F4A Te1 73.1(18) . . ?
F5 F5A F2 152(4) . . ?
F5 F5A Te1 75(2) . . ?
F2 F5A Te1 76(2) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.215
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.135

