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




_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
;
?
;
data_jp010753
_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            'Ag3 F18 Sb3 Se6'

_chemical_formula_weight         1504.62



loop_

_atom_type_symbol

_atom_type_description

_atom_type_scat_dispersion_real

_atom_type_scat_dispersion_imag

_atom_type_scat_source








F F 0.0171 0.0103 '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'



_symmetry_cell_setting           monoclinic

_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_int_tables_number      15



loop_

_symmetry_equiv_pos_as_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'
'-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                   21.821(5)

_cell_length_b                   10.748(3)

_cell_length_c                   10.718(3)

_cell_angle_alpha                90.00

_cell_angle_beta                 119.113(3)

_cell_angle_gamma                90.00

_cell_volume                     2196.2(10)

_cell_formula_units_Z            4

_cell_measurement_temperature    173(1)

_cell_measurement_reflns_used    2288

_cell_measurement_theta_min      3.72

_cell_measurement_theta_max      25.72



_exptl_crystal_description       Irregular

_exptl_crystal_colour            Orange

_exptl_crystal_size_max          0.45

_exptl_crystal_size_mid          0.08

_exptl_crystal_size_min          0.08

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    4.550

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             2640

_exptl_absorpt_coefficient_mu    16.342

_exptl_absorpt_correction_type    multi-scan

_exptl_absorpt_correction_T_min  0.037

_exptl_absorpt_correction_T_max  0.269

_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      173(1)
_diffrn_radiation_probe          x-ray

_diffrn_radiation_type           MoK\a

_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              K760

_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        0

_diffrn_standards_interval_count 0

_diffrn_standards_interval_time 0

_diffrn_standards_decay_%       0

_diffrn_reflns_number            5315

_diffrn_reflns_av_R_equivalents  0.0349

_diffrn_reflns_av_sigmaI/netI    0.0392

_diffrn_reflns_limit_h_min       -26

_diffrn_reflns_limit_h_max       26

_diffrn_reflns_limit_k_min       -13

_diffrn_reflns_limit_k_max       13

_diffrn_reflns_limit_l_min       -12

_diffrn_reflns_limit_l_max       12

_diffrn_reflns_theta_min         2.14

_diffrn_reflns_theta_max         25.80

_reflns_number_total             1890

_reflns_number_gt                1401

_reflns_threshold_expression     'I > 2\s(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 F^2^ against ALL reflections.  The weighted R-factor wR and

 goodness of fit S are based on F^2^, conventional R-factors R are based

 on F, with F set to zero for negative F^2^. The threshold expression of

 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is

 not relevant to the choice of reflections for refinement.  R-factors based

 on F^2^ 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/[\s^2^(Fo^2^)+(0.0457P)^2^+16.1286P] where P=(Fo^2^+2Fc^2^)/3'

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_number_reflns         1890

_refine_ls_number_parameters     141

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0605

_refine_ls_R_factor_gt           0.0381

_refine_ls_wR_factor_ref         0.0957

_refine_ls_wR_factor_gt          0.0885

_refine_ls_goodness_of_fit_ref   1.095

_refine_ls_restrained_S_all      1.095

_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


















Se1 Se 0.45364(6) 0.17114(11) 0.39484(12) 0.0344(3) Uani 1 1 d . . .
Se2 Se 0.39411(6) 0.02456(11) 0.45872(13) 0.0341(3) Uani 1 1 d . . .
Se3 Se 0.43425(7) -0.15918(12) 0.40465(13) 0.0365(3) Uani 1 1 d . . .
Ag1 Ag 0.5000 0.01913(16) 0.7500 0.0600(5) Uani 1 2 d S . .
Ag2 Ag 0.16817(5) -0.02209(9) 0.15561(9) 0.0366(3) Uani 1 1 d . . .
Sb1 Sb 0.2500 0.2500 0.5000 0.0233(3) Uani 1 2 d S . .
Sb2 Sb 0.0000 0.01913(10) 0.2500 0.0241(3) Uani 1 2 d S . .
Sb3 Sb 0.2500 0.2500 0.0000 0.0272(3) Uani 1 2 d S . .
F1 F 0.2253(3) 0.1367(6) 0.3488(6) 0.0359(16) Uani 1 1 d . . .
F2 F 0.1661(4) 0.2140(7) 0.5011(7) 0.0461(19) Uani 1 1 d . . .
F3 F 0.2936(4) 0.1216(6) 0.6298(7) 0.052(2) Uani 1 1 d . . .
F4 F 0.0836(3) 0.0190(7) 0.2416(7) 0.048(2) Uani 1 1 d . . .
F5 F 0.0000 -0.1543(10) 0.2500 0.066(3) Uani 1 2 d S . .
F6 F 0.0000 0.1929(9) 0.2500 0.059(3) Uani 1 2 d S . .
F7 F 0.0515(4) 0.0194(8) 0.4490(7) 0.055(2) Uani 1 1 d . . .
F8 F 0.1953(4) 0.1244(6) 0.0202(7) 0.0488(19) Uani 1 1 d . . .
F9 F 0.3306(4) 0.1534(8) 0.0986(9) 0.069(3) Uani 1 1 d . . .
F10 F 0.2335(5) 0.1790(8) -0.1730(8) 0.068(3) 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


















Se1 0.0361(7) 0.0341(7) 0.0330(7) 0.0027(5) 0.0167(6) 0.0051(6)
Se2 0.0296(7) 0.0391(7) 0.0360(6) -0.0001(6) 0.0179(5) 0.0035(5)
Se3 0.0336(7) 0.0357(7) 0.0365(7) -0.0067(5) 0.0141(6) -0.0011(6)
Ag1 0.0814(12) 0.0719(11) 0.0306(8) 0.000 0.0304(8) 0.000
Ag2 0.0377(6) 0.0433(6) 0.0294(5) -0.0003(4) 0.0168(4) 0.0022(4)
Sb1 0.0217(5) 0.0282(5) 0.0214(5) -0.0014(5) 0.0115(4) -0.0013(5)
Sb2 0.0227(6) 0.0326(6) 0.0190(5) 0.000 0.0116(4) 0.000
Sb3 0.0299(6) 0.0308(6) 0.0216(5) -0.0005(5) 0.0131(5) -0.0022(5)
F1 0.037(4) 0.039(4) 0.035(4) -0.014(3) 0.020(3) -0.011(3)
F2 0.038(4) 0.064(5) 0.050(4) -0.020(4) 0.032(4) -0.015(4)
F3 0.071(6) 0.043(4) 0.030(4) 0.008(3) 0.016(4) 0.010(4)
F4 0.026(4) 0.090(6) 0.033(4) -0.009(4) 0.019(3) -0.010(4)
F5 0.083(9) 0.036(6) 0.105(10) 0.000 0.068(8) 0.000
F6 0.082(9) 0.029(6) 0.074(8) 0.000 0.045(7) 0.000
F7 0.040(4) 0.102(7) 0.022(3) -0.001(4) 0.013(3) 0.005(4)
F8 0.058(5) 0.045(4) 0.046(4) -0.003(3) 0.027(4) -0.020(4)
F9 0.041(5) 0.066(6) 0.081(6) 0.023(5) 0.014(5) 0.019(4)
F10 0.110(7) 0.069(6) 0.048(5) -0.032(4) 0.056(5) -0.036(5)



_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





































Se1 Se2 2.3460(18) . ?
Se1 Se3 2.3460(18) 5_656 ?
Se1 Ag1 3.0239(17) 5_656 ?
Se2 Se3 2.3446(18) . ?
Se2 Ag1 2.8408(13) . ?
Se3 Se1 2.3460(18) 5_656 ?
Se3 Ag1 3.0636(16) 5_656 ?
Ag1 Se2 2.8408(13) 2_656 ?
Ag1 Se1 3.0239(17) 5_656 ?
Ag1 Se1 3.0239(17) 6_556 ?
Ag1 Se3 3.0636(16) 6_556 ?
Ag1 Se3 3.0636(16) 5_656 ?
Ag2 F10 2.388(7) 6_556 ?
Ag2 F8 2.403(7) . ?
Ag2 F7 2.429(7) 6 ?
Ag2 F4 2.471(7) . ?
Ag2 F1 2.498(6) . ?
Sb1 F3 1.859(6) 7_556 ?
Sb1 F3 1.859(6) . ?
Sb1 F2 1.876(7) 7_556 ?
Sb1 F2 1.876(7) . ?
Sb1 F1 1.884(6) 7_556 ?
Sb1 F1 1.884(6) . ?
Sb2 F5 1.864(10) . ?
Sb2 F7 1.866(7) 2 ?
Sb2 F7 1.866(7) . ?
Sb2 F6 1.868(10) . ?
Sb2 F4 1.869(6) . ?
Sb2 F4 1.869(6) 2 ?
Sb3 F9 1.866(7) 7 ?
Sb3 F9 1.866(7) . ?
Sb3 F10 1.871(7) . ?
Sb3 F10 1.871(7) 7 ?
Sb3 F8 1.883(7) 7 ?
Sb3 F8 1.883(7) . ?
F7 Ag2 2.429(7) 6_556 ?
F10 Ag2 2.388(7) 6 ?



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




















































































Se2 Se1 Se3 100.05(6) . 5_656 ?
Se2 Se1 Ag1 93.83(6) . 5_656 ?
Se3 Se1 Ag1 88.46(5) 5_656 5_656 ?
Se3 Se2 Se1 99.61(7) . . ?
Se3 Se2 Ag1 93.00(6) . . ?
Se1 Se2 Ag1 93.71(6) . . ?
Se2 Se3 Se1 99.68(6) . 5_656 ?
Se2 Se3 Ag1 92.84(6) . 5_656 ?
Se1 Se3 Ag1 88.19(5) 5_656 5_656 ?
Se2 Ag1 Se2 177.65(8) 2_656 . ?
Se2 Ag1 Se1 106.36(5) 2_656 5_656 ?
Se2 Ag1 Se1 75.29(4) . 5_656 ?
Se2 Ag1 Se1 75.29(4) 2_656 6_556 ?
Se2 Ag1 Se1 106.36(5) . 6_556 ?
Se1 Ag1 Se1 94.89(7) 5_656 6_556 ?
Se2 Ag1 Se3 74.92(4) 2_656 6_556 ?
Se2 Ag1 Se3 103.88(4) . 6_556 ?
Se1 Ag1 Se3 166.35(6) 5_656 6_556 ?
Se1 Ag1 Se3 72.11(4) 6_556 6_556 ?
Se2 Ag1 Se3 103.88(4) 2_656 5_656 ?
Se2 Ag1 Se3 74.92(4) . 5_656 ?
Se1 Ag1 Se3 72.11(4) 5_656 5_656 ?
Se1 Ag1 Se3 166.35(6) 6_556 5_656 ?
Se3 Ag1 Se3 121.14(7) 6_556 5_656 ?
F10 Ag2 F8 134.2(3) 6_556 . ?
F10 Ag2 F7 132.7(3) 6_556 6 ?
F8 Ag2 F7 84.2(2) . 6 ?
F10 Ag2 F4 96.5(3) 6_556 . ?
F8 Ag2 F4 123.8(3) . . ?
F7 Ag2 F4 72.3(2) 6 . ?
F10 Ag2 F1 88.5(3) 6_556 . ?
F8 Ag2 F1 83.3(2) . . ?
F7 Ag2 F1 128.8(2) 6 . ?
F4 Ag2 F1 74.4(2) . . ?
F3 Sb1 F3 180.0(4) 7_556 . ?
F3 Sb1 F2 89.3(3) 7_556 7_556 ?
F3 Sb1 F2 90.7(3) . 7_556 ?
F3 Sb1 F2 90.7(3) 7_556 . ?
F3 Sb1 F2 89.3(3) . . ?
F2 Sb1 F2 180.000(1) 7_556 . ?
F3 Sb1 F1 89.5(3) 7_556 7_556 ?
F3 Sb1 F1 90.5(3) . 7_556 ?
F2 Sb1 F1 90.0(3) 7_556 7_556 ?
F2 Sb1 F1 90.0(3) . 7_556 ?
F3 Sb1 F1 90.5(3) 7_556 . ?
F3 Sb1 F1 89.5(3) . . ?
F2 Sb1 F1 90.0(3) 7_556 . ?
F2 Sb1 F1 90.0(3) . . ?
F1 Sb1 F1 180.0 7_556 . ?
F5 Sb2 F7 90.1(3) . 2 ?
F5 Sb2 F7 90.1(3) . . ?
F7 Sb2 F7 179.8(5) 2 . ?
F5 Sb2 F6 180.000(1) . . ?
F7 Sb2 F6 89.9(3) 2 . ?
F7 Sb2 F6 89.9(3) . . ?
F5 Sb2 F4 90.0(2) . . ?
F7 Sb2 F4 90.3(3) 2 . ?
F7 Sb2 F4 89.7(3) . . ?
F6 Sb2 F4 90.0(2) . . ?
F5 Sb2 F4 90.0(2) . 2 ?
F7 Sb2 F4 89.7(3) 2 2 ?
F7 Sb2 F4 90.3(3) . 2 ?
F6 Sb2 F4 90.0(2) . 2 ?
F4 Sb2 F4 179.9(5) . 2 ?
F9 Sb3 F9 180.0(5) 7 . ?
F9 Sb3 F10 89.5(4) 7 . ?
F9 Sb3 F10 90.5(4) . . ?
F9 Sb3 F10 90.5(4) 7 7 ?
F9 Sb3 F10 89.5(4) . 7 ?
F10 Sb3 F10 180.0(5) . 7 ?
F9 Sb3 F8 90.6(4) 7 7 ?
F9 Sb3 F8 89.4(4) . 7 ?
F10 Sb3 F8 90.3(3) . 7 ?
F10 Sb3 F8 89.7(3) 7 7 ?
F9 Sb3 F8 89.4(4) 7 . ?
F9 Sb3 F8 90.6(4) . . ?
F10 Sb3 F8 89.7(3) . . ?
F10 Sb3 F8 90.3(3) 7 . ?
F8 Sb3 F8 180.0(4) 7 . ?
Sb1 F1 Ag2 166.6(3) . . ?
Sb2 F4 Ag2 160.3(4) . . ?
Sb2 F7 Ag2 145.5(4) . 6_556 ?
Sb3 F8 Ag2 153.6(4) . . ?
Sb3 F10 Ag2 143.7(4) . 6 ?



_diffrn_measured_fraction_theta_max 0.894

_diffrn_reflns_theta_full        25.00

_diffrn_measured_fraction_theta_full 0.957

_refine_diff_density_max         1.644

_refine_diff_density_min         -0.870

_refine_diff_density_rms         0.238

