# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address I.Krossing ;Institut f\"ur Anorganische und Analytische Chemie Albertstr. 21 79104 Freiburg Germany ; T.Kochner ;Institut f\"ur Anorganische und Analytische Chemie Albertstr. 21 79104 Freiburg Germany ; J.Passmore ;Department of Chemistry, University of New Brunswick, Fredericton N.B., E3B 6E2, Canada ; D.Aris ;Department of Chemistry, University of New Brunswick, Fredericton N.B., E3B 6E2, Canada ; A.Decken ;Department of Chemistry, University of New Brunswick, Fredericton N.B., E3B 6E2, Canada ; I.Dionne ;Department of Chemistry, University of New Brunswick, Fredericton N.B., E3B 6E2, Canada ; ; X.Wang ; ;Department of Chemistry, University of New Brunswick, Fredericton N.B., E3B 6E2, Canada ; E.Rivard ;Department of Chemistry, University of New Brunswick, Fredericton N.B., E3B 6E2, Canada ; J.Beck ;Institut f\"ur Anorganische Chemie, Friedrich Wilhelms Universit\"at Bonn, 53121 Bonn, Germany ; F.Steden ;Institut f\"ur Anorganische Chemie, Friedrich Wilhelms Universit\"at Bonn, 53121 Bonn, Germany ; W.Hoffbauer ;Institut f\"ur Anorganische Chemie, Friedrich Wilhelms Universit\"at Bonn, 53121 Bonn, Germany ; 'J.Schmedt auf der Gunne' ;Department of Chemistry and Biochemistry, Ludwig Maximilians Universit\"at, 81377 M\"unchen, Germany ; _publ_contact_author_address ;Institut f\"ur Anorganische und Analytische Chemie Albertstr. 21 79104 Freiburg ; _publ_contact_author_email krossing@uni-freiburg.de _publ_contact_author_fax +49-761-203-6001 _publ_contact_author_phone +49-761-203-6121 _publ_contact_author_name 'Krossing Ingo' # Attachment '- ag2se6so2_4_r.cif' data_p-1a _database_code_depnum_ccdc_archive 'CCDC 814799' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C16 Al F36 O4, 0.5(Ag2 O8 S4 Se6)' _chemical_formula_sum 'C16 Ag Al F36 O8 S2 Se3' _chemical_properties_physical 'air-sensitive, moisture-sensitive, photo-sensitive, oxygen-sensitive' _exptl_crystal_recrystallization_method SO2 _exptl_crystal_description cubes _exptl_crystal_colour orange _chemical_formula_weight 1440.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.639(2) _cell_length_b 13.638(3) _cell_length_c 13.834(3) _cell_angle_alpha 71.06(3) _cell_angle_beta 78.05(3) _cell_angle_gamma 86.37(3) _cell_volume 1857.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8487 _cell_measurement_theta_min 7.78 _cell_measurement_theta_max 54.96 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 3.842 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.648510 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'FSPROCESS (T. Higashi, Rigaku Inc., 2001)' _exptl_special_details ; Crystal mounted on CRYOLOOP (Hampton) at 253 K in N2 stream in perfluoroetheroil ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS Spider' _diffrn_measurement_method 'Curved Image Plate' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18617 _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_av_sigmaI/netI 0.0718 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 23.96 _reflns_number_total 5792 _reflns_number_gt 3535 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSTALCLEAR (Rigaku Inc.,2008)' _computing_cell_refinement 'FSPROCESS (T. Higashi, Rigaku Inc., 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics DIAMOND _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^)+(0.1638P)^2^+41.2973P] 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 5792 _refine_ls_number_parameters 731 _refine_ls_number_restraints 273 _refine_ls_R_factor_all 0.1651 _refine_ls_R_factor_gt 0.1104 _refine_ls_wR_factor_ref 0.3321 _refine_ls_wR_factor_gt 0.2816 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.053 _refine_ls_shift/su_mean 0.001 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 Al1 Al 0.7338(3) 0.3077(2) 0.8549(2) 0.0298(8) Uani 1 1 d . . . O1 O 0.7703(10) 0.3188(6) 0.9638(6) 0.058(3) Uani 1 1 d . A . O2 O 0.8208(8) 0.2106(5) 0.8219(6) 0.046(2) Uani 1 1 d . . . O3 O 0.5772(8) 0.2787(12) 0.8747(9) 0.115(6) Uani 1 1 d . . . O4 O 0.7774(11) 0.4208(6) 0.7550(6) 0.070(3) Uani 1 1 d . B . C1 C 0.7822(11) 0.2817(8) 1.0645(8) 0.039(3) Uani 1 1 d . . . C5 C 0.8869(5) 0.1502(5) 0.7763(5) 0.049(3) Uani 1 1 d D C . C6 C 0.8635(4) 0.1873(3) 0.6616(4) 0.085(6) Uani 1 1 d D . . C7 C 0.8393(4) 0.0340(5) 0.8299(3) 0.076(5) Uani 1 1 d D . . C8 C 1.0340(6) 0.1543(4) 0.7751(4) 0.266(12) Uani 1 1 d D . . C9 C 0.4613(11) 0.2705(4) 0.8653(4) 0.044(3) Uani 1 1 d D . . C10 C 0.4410(5) 0.1617(4) 0.8610(3) 0.185(8) Uani 1 1 d D . . C11 C 0.4288(5) 0.3515(3) 0.7673(4) 0.064(4) Uani 1 1 d D . . C12 C 0.3705(5) 0.2843(3) 0.9618(4) 0.093(7) Uani 1 1 d D . . C13 C 0.8122(5) 0.5209(8) 0.7278(4) 0.049(4) Uani 1 1 d D . . F13 F 0.8333(8) 0.0081(7) 0.9290(4) 0.137(6) Uani 1 1 d D C . F14 F 0.7270(7) 0.0281(8) 0.8095(7) 0.214(8) Uani 1 1 d D C . F15 F 0.9214(9) -0.0229(7) 0.7885(6) 0.275(9) Uani 1 1 d D C . F16 F 1.0584(10) 0.2491(5) 0.7709(7) 0.353(14) Uani 1 1 d D C . F17 F 1.0448(11) 0.0866(6) 0.8664(6) 0.215(5) Uani 1 1 d D C . F18 F 1.1074(13) 0.1278(8) 0.6990(7) 0.516(17) Uani 1 1 d D C . F19 F 0.3231(6) 0.1386(9) 0.8834(6) 0.326(7) Uani 1 1 d D . . F20 F 0.4870(9) 0.1589(8) 0.7704(5) 0.407(16) Uani 1 1 d D . . F21 F 0.4977(9) 0.0957(8) 0.9251(6) 0.228(9) Uani 1 1 d D . . F22 F 0.4119(7) 0.4438(4) 0.7770(6) 0.100(4) Uani 1 1 d D . . F23 F 0.5223(8) 0.3604(6) 0.6869(6) 0.154(6) Uani 1 1 d D . . F24 F 0.3255(7) 0.3302(7) 0.7409(7) 0.237(5) Uani 1 1 d D . . F25 F 0.2529(6) 0.2964(7) 0.9449(9) 0.288(13) Uani 1 1 d D . . F26 F 0.4051(10) 0.3661(5) 0.9793(7) 0.238(11) Uani 1 1 d D . . F27 F 0.3732(8) 0.2028(7) 1.0446(6) 0.137(5) Uani 1 1 d D . . F4 F 0.6179(8) 0.4033(5) 1.0802(6) 0.071(4) Uani 0.648(5) 1 d PD A 2 F5 F 0.5596(8) 0.2459(6) 1.1485(7) 0.152(8) Uani 0.648(5) 1 d PD A 2 F6 F 0.6655(12) 0.3134(7) 1.2247(5) 0.118(7) Uani 0.648(5) 1 d PD A 2 F7 F 0.8489(10) 0.4277(5) 1.0842(7) 0.223(7) Uani 0.648(5) 1 d PD A 2 F8 F 0.9095(9) 0.2903(9) 1.1891(5) 0.150(7) Uani 0.648(5) 1 d PD A 2 F9 F 1.0001(8) 0.3392(9) 1.0297(8) 0.098(5) Uani 0.648(5) 1 d PD A 2 C2 C 0.7824(4) 0.1633(5) 1.1104(4) 0.060(6) Uani 0.648(5) 1 d PD A 2 F1 F 0.7580(6) 0.1237(7) 1.2116(4) 0.045(3) Uani 0.648(5) 1 d PD A 2 F2 F 0.7021(6) 0.1189(7) 1.0780(5) 0.106(5) Uani 0.648(5) 1 d PD A 2 F3 F 0.8951(6) 0.1291(9) 1.0798(7) 0.196(9) Uani 0.648(5) 1 d PD A 2 C3 C 0.6466(7) 0.3124(4) 1.1362(5) 0.095(9) Uani 0.648(5) 1 d PD A 2 C4 C 0.8853(7) 0.3297(5) 1.0929(5) 0.153(13) Uani 0.648(5) 1 d PD A 2 F34 F 0.8757(11) 0.5428(6) 0.8786(5) 0.095(5) Uani 0.552(6) 1 d PD B 2 F32 F 0.9826(6) 0.5406(6) 0.5811(9) 0.108(6) Uani 0.552(6) 1 d PD B 2 F29 F 0.5965(6) 0.5945(7) 0.7117(6) 0.065(4) Uani 0.552(6) 1 d PD B 2 F33 F 0.8449(8) 0.6733(5) 0.5739(8) 0.065(4) Uani 0.552(6) 1 d PD B 2 F35 F 0.9940(9) 0.6269(6) 0.7173(8) 0.150(8) Uani 0.552(6) 1 d PD B 2 F36 F 0.9940(12) 0.4494(7) 0.7807(10) 0.179(14) Uani 0.552(6) 1 d PD B 2 C16 C 0.9233(6) 0.5386(5) 0.7791(4) 0.070(9) Uani 0.552(6) 1 d PD B 2 C14 C 0.6934(5) 0.5831(4) 0.7632(4) 0.049(6) Uani 0.552(6) 1 d PD B 2 C15 C 0.8561(5) 0.5674(4) 0.6075(5) 0.079(9) Uani 0.552(6) 1 d PDU B 2 F28 F 0.6427(8) 0.5337(6) 0.8639(5) 0.040(4) Uani 0.552(6) 1 d PD B 2 F30 F 0.7228(10) 0.6792(6) 0.7586(7) 0.069(4) Uani 0.552(6) 1 d PD B 2 F31 F 0.7825(8) 0.5249(6) 0.5605(7) 0.073(5) Uani 0.552(6) 1 d PDU B 2 F10 F 0.9327(7) 0.2661(5) 0.6001(8) 0.056(4) Uani 0.551(9) 1 d PDU C 2 F11 F 0.8713(8) 0.1207(5) 0.6118(7) 0.071(4) Uani 0.551(9) 1 d PDU C 2 F12 F 0.7443(6) 0.2217(6) 0.6611(8) 0.058(4) Uani 0.551(9) 1 d PDU C 2 C2A C 0.9283(15) 0.2537(9) 1.0435(8) 0.059(10) Uiso 0.352(5) 1 d PD A 1 F2A1 F 0.957(2) 0.1642(9) 1.0287(14) 0.079(7) Uiso 0.352(5) 1 d PD A 1 F2A2 F 0.9786(13) 0.2519(10) 1.1220(8) 0.028(4) Uiso 0.352(5) 1 d PD A 1 F2A3 F 0.9960(16) 0.3138(11) 0.9602(10) 0.048(5) Uiso 0.352(5) 1 d PD A 1 C3A C 0.7180(12) 0.1885(11) 1.1156(9) 0.053(10) Uiso 0.352(5) 1 d PD A 1 F3A1 F 0.5963(13) 0.2090(18) 1.1426(18) 0.095(9) Uiso 0.352(5) 1 d PD A 1 F3A2 F 0.7548(18) 0.137(2) 1.2021(11) 0.096(12) Uiso 0.352(5) 1 d PD A 1 F3A3 F 0.716(2) 0.1250(13) 1.0648(13) 0.089(10) Uiso 0.352(5) 1 d PD A 1 C4A C 0.7707(11) 0.3713(11) 1.1108(10) 0.065(11) Uiso 0.352(5) 1 d PD A 1 F4A1 F 0.8573(12) 0.4447(11) 1.0817(13) 0.044(5) Uiso 0.352(5) 1 d PD A 1 F4A2 F 0.7623(15) 0.3291(13) 1.2115(9) 0.044(5) Uiso 0.352(5) 1 d PD A 1 F4A3 F 0.6668(12) 0.4221(14) 1.1002(14) 0.052(5) Uiso 0.352(5) 1 d PD A 1 C14A C 0.7670(10) 0.5761(9) 0.7974(10) 0.028(5) Uiso 0.448(6) 1 d PD B 1 F14A F 0.6495(11) 0.5469(14) 0.8426(15) 0.071(6) Uiso 0.448(6) 1 d PD B 1 F14B F 0.7680(15) 0.6771(8) 0.7624(12) 0.048(4) Uiso 0.448(6) 1 d PD B 1 F14C F 0.8284(12) 0.5538(11) 0.8724(9) 0.047(4) Uiso 0.448(6) 1 d PD B 1 C16A C 0.9540(14) 0.5195(9) 0.6994(9) 0.061(8) Uiso 0.448(6) 1 d PD B 1 F16A F 1.0270(13) 0.4880(11) 0.7688(9) 0.052(4) Uiso 0.448(6) 1 d PD B 1 F16B F 0.989(2) 0.6162(9) 0.6558(15) 0.097(7) Uiso 0.448(6) 1 d PD B 1 F16C F 1.006(3) 0.4760(14) 0.6308(13) 0.190(16) Uiso 0.448(6) 1 d PD B 1 C80 C 0.7542(13) 0.5696(9) 0.6215(12) 0.067(9) Uiso 0.448(6) 1 d PD B 1 F80A F 0.753(3) 0.5072(12) 0.5674(17) 0.190(18) Uiso 0.448(6) 1 d PD B 1 F80B F 0.7978(15) 0.6574(10) 0.5526(13) 0.068(5) Uiso 0.448(6) 1 d PD B 1 F80C F 0.6345(13) 0.5909(15) 0.6459(16) 0.091(7) Uiso 0.448(6) 1 d PD B 1 F10A F 0.9783(7) 0.1579(6) 0.6066(10) 0.114(7) Uani 0.449(9) 1 d PDU C 1 F11A F 0.8650(8) 0.2921(5) 0.6055(10) 0.060(5) Uani 0.449(9) 1 d PDU C 1 F12A F 0.7760(9) 0.1508(8) 0.6196(12) 0.185(12) Uani 0.449(9) 1 d PDU C 1 Ag1 Ag 0.70716(11) 0.10023(9) 0.45945(9) 0.0680(4) Uani 1 1 d . . . S1 S 1.0539(4) 0.1395(3) 0.3552(4) 0.0748(12) Uani 1 1 d . . . S2 S 0.6909(5) 0.3712(4) 0.4308(3) 0.0970(15) Uani 1 1 d . . . O5 O 0.9299(10) 0.1108(10) 0.3898(8) 0.089(3) Uani 1 1 d . . . O6 O 1.1499(10) 0.0881(8) 0.4091(8) 0.079(3) Uani 1 1 d . . . O7 O 0.7606(12) 0.2802(9) 0.4297(8) 0.091(4) Uani 1 1 d . . . O8 O 0.5614(17) 0.3604(12) 0.4621(10) 0.142(6) Uani 1 1 d . . . Se1 Se 0.54227(14) -0.00201(10) 0.64625(9) 0.0535(4) Uani 1 1 d . . 1 Se2 Se 0.45903(15) 0.15132(10) 0.40162(11) 0.0595(4) Uani 1 1 d . . 1 Se3 Se 0.36448(14) 0.08692(11) 0.57971(11) 0.0614(4) Uani 1 1 d . . 1 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 Al1 0.0265(15) 0.0281(14) 0.0276(14) -0.0050(12) 0.0010(12) 0.0091(12) O1 0.108(7) 0.039(4) 0.029(4) -0.014(3) -0.012(4) 0.001(4) O2 0.051(4) 0.030(4) 0.053(4) -0.017(3) 0.001(4) 0.016(3) O3 0.014(4) 0.197(14) 0.084(8) 0.020(8) -0.003(5) -0.006(6) O4 0.141(9) 0.015(4) 0.034(4) 0.005(3) 0.006(5) 0.002(5) C1 0.053(6) 0.035(5) 0.031(5) -0.010(4) -0.017(4) 0.014(5) C5 0.046(6) 0.062(7) 0.043(6) -0.023(5) -0.011(5) 0.024(6) C6 0.152(16) 0.045(7) 0.039(7) -0.010(6) 0.010(9) 0.012(9) C7 0.149(13) 0.043(6) 0.057(7) -0.036(5) -0.043(7) 0.029(8) C8 0.180(13) 0.57(3) 0.143(11) -0.229(15) -0.129(10) 0.267(17) C9 0.051(7) 0.045(6) 0.044(6) -0.018(5) -0.015(5) -0.007(5) C10 0.43(3) 0.036(7) 0.150(11) -0.033(7) -0.188(13) -0.018(13) C11 0.080(9) 0.063(8) 0.056(7) -0.013(6) -0.038(6) -0.003(7) C12 0.052(8) 0.127(14) 0.063(10) -0.007(10) 0.023(7) 0.028(9) C13 0.053(7) 0.043(7) 0.031(6) 0.003(5) 0.011(5) 0.000(6) F13 0.271(16) 0.066(6) 0.061(6) -0.009(5) -0.024(8) -0.001(8) F14 0.39(2) 0.108(7) 0.130(11) -0.031(7) 0.020(13) -0.146(10) F15 0.63(3) 0.124(6) 0.089(6) -0.073(5) -0.118(11) 0.227(10) F16 0.084(6) 0.169(14) 0.81(4) -0.070(19) -0.220(12) -0.021(8) F17 0.262(8) 0.181(11) 0.296(10) -0.112(8) -0.249(7) 0.147(8) F18 0.188(10) 0.77(4) 0.219(19) 0.18(2) 0.123(12) 0.318(15) F19 0.472(12) 0.126(8) 0.383(16) 0.106(9) -0.328(11) -0.209(8) F20 1.02(5) 0.104(6) 0.237(9) -0.148(6) -0.314(17) 0.135(15) F21 0.53(3) 0.056(6) 0.132(9) -0.039(6) -0.144(12) 0.087(11) F22 0.133(8) 0.056(5) 0.100(7) -0.004(5) -0.035(6) 0.001(5) F23 0.265(16) 0.130(10) 0.038(5) -0.011(6) -0.003(7) 0.033(10) F24 0.294(8) 0.155(10) 0.250(9) 0.092(7) -0.246(7) -0.122(8) F25 0.043(6) 0.35(3) 0.29(2) 0.075(19) 0.065(9) 0.062(10) F26 0.52(3) 0.095(7) 0.066(6) -0.043(5) 0.010(11) 0.109(12) F27 0.124(9) 0.165(11) 0.053(6) 0.027(7) 0.024(6) 0.017(8) F4 0.048(6) 0.057(6) 0.077(7) -0.014(6) 0.036(6) 0.025(5) F5 0.071(8) 0.071(10) 0.218(18) 0.007(11) 0.103(10) -0.028(8) F6 0.237(19) 0.073(7) 0.026(5) -0.034(5) 0.054(8) -0.030(10) F7 0.433(16) 0.066(8) 0.212(12) 0.033(8) -0.244(11) -0.119(10) F8 0.180(12) 0.164(16) 0.097(9) 0.035(9) -0.109(8) -0.072(12) F9 0.067(8) 0.124(11) 0.112(11) -0.051(9) -0.017(8) 0.010(8) C2 0.114(16) 0.033(9) 0.016(8) 0.012(7) -0.018(9) 0.030(11) F1 0.077(7) 0.029(5) 0.021(4) 0.003(4) -0.009(4) 0.003(5) F2 0.243(14) 0.022(5) 0.072(7) 0.000(5) -0.088(8) -0.031(7) F3 0.160(12) 0.109(10) 0.162(16) 0.077(10) 0.084(12) 0.119(9) C3 0.16(2) 0.046(10) 0.075(15) -0.024(10) -0.023(15) 0.071(13) C4 0.094(14) 0.17(3) 0.135(19) 0.093(18) -0.095(13) -0.080(17) F34 0.077(8) 0.099(11) 0.131(10) -0.031(9) -0.079(8) -0.007(9) F32 0.112(12) 0.165(14) 0.044(7) -0.063(8) 0.050(7) -0.036(11) F29 0.058(8) 0.072(9) 0.056(7) -0.001(7) -0.023(6) -0.007(7) F33 0.108(10) 0.038(7) 0.027(6) 0.025(5) -0.018(6) -0.027(7) F35 0.075(8) 0.188(17) 0.119(12) 0.091(11) -0.072(8) -0.093(10) F36 0.060(10) 0.102(15) 0.24(3) 0.068(16) 0.054(14) 0.020(11) C16 0.045(14) 0.079(17) 0.075(17) -0.026(14) 0.015(13) 0.008(13) C14 0.085(15) 0.040(11) 0.017(9) 0.004(8) -0.021(9) -0.002(11) C15 0.102(17) 0.071(14) 0.038(12) -0.001(11) 0.011(12) 0.016(13) F28 0.055(7) 0.026(5) 0.022(5) -0.002(4) 0.019(5) 0.011(5) F30 0.106(9) 0.021(6) 0.091(8) 0.000(5) -0.072(7) -0.013(6) F31 0.152(12) 0.047(7) 0.009(5) 0.016(5) -0.028(6) -0.017(8) F10 0.055(7) 0.037(6) 0.055(7) -0.003(6) 0.011(6) 0.008(6) F11 0.124(9) 0.032(6) 0.078(7) -0.010(5) -0.082(6) 0.010(6) F12 0.073(8) 0.063(7) 0.045(6) -0.022(5) -0.028(5) 0.021(6) F10A 0.171(17) 0.135(13) 0.069(9) -0.069(9) -0.042(10) 0.017(13) F11A 0.092(12) 0.037(7) 0.035(7) -0.014(6) 0.028(8) 0.003(8) F12A 0.19(2) 0.180(18) 0.20(2) -0.083(15) 0.005(17) -0.086(16) Ag1 0.0625(6) 0.0712(7) 0.0541(6) -0.0013(5) -0.0025(5) -0.0123(6) S1 0.067(2) 0.0476(19) 0.097(3) 0.0089(19) -0.037(2) -0.0121(17) S2 0.145(4) 0.082(3) 0.072(2) -0.010(2) -0.064(2) 0.003(3) O5 0.063(6) 0.152(9) 0.067(5) -0.060(6) 0.001(5) -0.026(6) O6 0.084(6) 0.073(6) 0.084(6) -0.015(5) -0.048(5) 0.024(5) O7 0.126(9) 0.066(7) 0.063(6) 0.012(5) -0.030(6) -0.010(7) O8 0.212(13) 0.147(11) 0.083(7) -0.044(7) -0.080(8) 0.095(10) Se1 0.0688(8) 0.0560(7) 0.0337(6) -0.0133(5) -0.0047(5) -0.0091(6) Se2 0.0854(9) 0.0348(6) 0.0548(7) -0.0032(6) -0.0251(7) 0.0046(6) Se3 0.0607(8) 0.0632(7) 0.0637(8) -0.0332(6) -0.0036(6) 0.0161(6) _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 Al1 O3 1.683(10) . ? Al1 O1 1.685(9) . ? Al1 O2 1.697(8) . ? Al1 O4 1.717(8) . ? O1 C1 1.349(13) . ? O2 C5 1.285(11) . ? O3 C9 1.281(15) . ? O4 C13 1.347(13) . ? C1 C3A 1.382(17) . ? C1 C4 1.491(15) . ? C1 C2 1.532(12) . ? C1 C4A 1.54(2) . ? C1 C2A 1.568(19) . ? C1 C3 1.685(13) . ? C5 C8 1.567(7) . ? C5 C6 1.569(7) . ? C5 C7 1.581(7) . ? C6 F10 1.291(7) . ? C6 F11 1.297(8) . ? C6 F12 1.325(7) . ? C6 F11A 1.387(7) . ? C6 F12A 1.388(10) . ? C6 F10A 1.408(8) . ? C7 F13 1.289(6) . ? C7 F14 1.296(7) . ? C7 F15 1.300(8) . ? C8 F18 1.311(8) . ? C8 F16 1.314(7) . ? C8 F17 1.323(7) . ? C9 C11 1.534(7) . ? C9 C10 1.535(7) . ? C9 C12 1.535(7) . ? C10 F20 1.260(7) . ? C10 F21 1.262(7) . ? C10 F19 1.262(7) . ? C11 F24 1.304(7) . ? C11 F22 1.306(7) . ? C11 F23 1.308(7) . ? C12 F26 1.306(8) . ? C12 F25 1.310(7) . ? C12 F27 1.316(7) . ? C13 C14A 1.399(16) . ? C13 C16A 1.479(16) . ? C13 C15 1.555(7) . ? C13 C14 1.560(8) . ? C13 C16 1.567(8) . ? C13 C80 1.635(16) . ? F4 C3 1.287(7) . ? F5 C3 1.284(7) . ? F6 C3 1.286(8) . ? F7 C4 1.341(8) . ? F8 C4 1.337(8) . ? F9 C4 1.333(8) . ? C2 F3 1.296(7) . ? C2 F2 1.303(7) . ? C2 F1 1.303(6) . ? F34 C16 1.384(7) . ? F32 C15 1.378(7) . ? F29 C14 1.343(7) . ? F33 C15 1.371(7) . ? F35 C16 1.388(8) . ? F36 C16 1.386(8) . ? C14 F30 1.346(8) . ? C14 F28 1.346(7) . ? C15 F31 1.373(8) . ? C2A F2A3 1.280(13) . ? C2A F2A2 1.299(14) . ? C2A F2A1 1.310(14) . ? C3A F3A3 1.283(15) . ? C3A F3A2 1.302(14) . ? C3A F3A1 1.310(13) . ? C4A F4A3 1.275(14) . ? C4A F4A2 1.308(13) . ? C4A F4A1 1.310(14) . ? C14A F14C 1.284(13) . ? C14A F14A 1.300(13) . ? C14A F14B 1.303(12) . ? C16A F16C 1.288(15) . ? C16A F16B 1.303(13) . ? C16A F16A 1.307(14) . ? C80 F80C 1.288(14) . ? C80 F80A 1.305(15) . ? C80 F80B 1.305(13) . ? Ag1 O5 2.361(10) . ? Ag1 O7 2.438(12) . ? Ag1 Se1 2.792(2) . ? Ag1 Se2 2.894(2) . ? Ag1 Se3 2.950(2) 2_656 ? S1 O5 1.343(11) . ? S1 O6 1.405(11) . ? S2 O8 1.359(18) . ? S2 O7 1.408(13) . ? Se1 Se2 2.338(2) 2_656 ? Se1 Se3 2.367(2) . ? Se2 Se1 2.338(2) 2_656 ? Se2 Se3 2.353(2) . ? Se3 Ag1 2.950(2) 2_656 ? 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 O3 Al1 O1 110.6(6) . . ? O3 Al1 O2 107.8(7) . . ? O1 Al1 O2 109.9(5) . . ? O3 Al1 O4 112.8(6) . . ? O1 Al1 O4 108.2(5) . . ? O2 Al1 O4 107.4(4) . . ? C1 O1 Al1 153.3(8) . . ? C5 O2 Al1 167.4(6) . . ? C9 O3 Al1 165.4(9) . . ? C13 O4 Al1 146.6(7) . . ? O1 C1 C3A 111.5(11) . . ? O1 C1 C4 116.1(9) . . ? C3A C1 C4 130.1(9) . . ? O1 C1 C2 114.9(9) . . ? C3A C1 C2 29.1(6) . . ? C4 C1 C2 111.7(7) . . ? O1 C1 C4A 109.7(9) . . ? C3A C1 C4A 122.8(10) . . ? C4 C1 C4A 51.7(6) . . ? C2 C1 C4A 134.5(8) . . ? O1 C1 C2A 96.7(9) . . ? C3A C1 C2A 105.7(9) . . ? C4 C1 C2A 55.4(7) . . ? C2 C1 C2A 76.6(7) . . ? C4A C1 C2A 106.9(10) . . ? O1 C1 C3 107.3(8) . . ? C3A C1 C3 75.4(8) . . ? C4 C1 C3 103.3(7) . . ? C2 C1 C3 101.7(6) . . ? C4A C1 C3 55.5(6) . . ? C2A C1 C3 153.8(9) . . ? O2 C5 C8 112.5(7) . . ? O2 C5 C6 106.3(5) . . ? C8 C5 C6 109.7(4) . . ? O2 C5 C7 111.3(5) . . ? C8 C5 C7 108.6(4) . . ? C6 C5 C7 108.3(5) . . ? F10 C6 F11 106.5(6) . . ? F10 C6 F12 103.5(5) . . ? F11 C6 F12 102.6(6) . . ? F10 C6 F11A 33.8(5) . . ? F11 C6 F11A 118.7(8) . . ? F12 C6 F11A 70.1(5) . . ? F10 C6 F12A 116.6(8) . . ? F11 C6 F12A 46.7(6) . . ? F12 C6 F12A 55.9(6) . . ? F11A C6 F12A 100.7(6) . . ? F10 C6 F10A 67.6(5) . . ? F11 C6 F10A 55.1(6) . . ? F12 C6 F10A 147.9(9) . . ? F11A C6 F10A 99.0(5) . . ? F12A C6 F10A 99.1(7) . . ? F10 C6 C5 114.1(6) . . ? F11 C6 C5 119.2(5) . . ? F12 C6 C5 109.4(6) . . ? F11A C6 C5 120.4(7) . . ? F12A C6 C5 129.2(7) . . ? F10A C6 C5 102.2(6) . . ? F13 C7 F14 110.9(5) . . ? F13 C7 F15 111.3(5) . . ? F14 C7 F15 110.4(6) . . ? F13 C7 C5 109.6(6) . . ? F14 C7 C5 107.5(6) . . ? F15 C7 C5 107.0(6) . . ? F18 C8 F16 112.0(6) . . ? F18 C8 F17 110.5(6) . . ? F16 C8 F17 111.2(6) . . ? F18 C8 C5 113.7(8) . . ? F16 C8 C5 106.4(7) . . ? F17 C8 C5 102.6(6) . . ? O3 C9 C11 112.6(7) . . ? O3 C9 C10 109.1(10) . . ? C11 C9 C10 109.1(5) . . ? O3 C9 C12 108.3(8) . . ? C11 C9 C12 109.1(6) . . ? C10 C9 C12 108.7(5) . . ? F20 C10 F21 109.2(6) . . ? F20 C10 F19 108.9(6) . . ? F21 C10 F19 108.7(6) . . ? F20 C10 C9 109.1(6) . . ? F21 C10 C9 109.6(7) . . ? F19 C10 C9 111.2(8) . . ? F24 C11 F22 106.4(5) . . ? F24 C11 F23 106.4(6) . . ? F22 C11 F23 106.2(5) . . ? F24 C11 C9 114.1(6) . . ? F22 C11 C9 112.4(5) . . ? F23 C11 C9 110.8(6) . . ? F26 C12 F25 109.5(6) . . ? F26 C12 F27 109.0(6) . . ? F25 C12 F27 108.7(5) . . ? F26 C12 C9 109.3(6) . . ? F25 C12 C9 109.2(8) . . ? F27 C12 C9 111.1(6) . . ? O4 C13 C14A 118.8(7) . . ? O4 C13 C16A 104.2(9) . . ? C14A C13 C16A 113.0(9) . . ? O4 C13 C15 110.7(7) . . ? C14A C13 C15 126.6(8) . . ? C16A C13 C15 70.3(5) . . ? O4 C13 C14 108.4(6) . . ? C14A C13 C14 38.2(5) . . ? C16A C13 C14 145.0(9) . . ? C15 C13 C14 108.5(5) . . ? O4 C13 C16 113.9(7) . . ? C14A C13 C16 69.7(6) . . ? C16A C13 C16 45.9(6) . . ? C15 C13 C16 107.8(4) . . ? C14 C13 C16 107.4(6) . . ? O4 C13 C80 100.4(8) . . ? C14A C13 C80 110.4(8) . . ? C16A C13 C80 109.0(7) . . ? C15 C13 C80 38.8(5) . . ? C14 C13 C80 77.3(6) . . ? C16 C13 C80 140.8(7) . . ? F3 C2 F2 105.7(6) . . ? F3 C2 F1 105.6(5) . . ? F2 C2 F1 105.7(5) . . ? F3 C2 C1 109.0(7) . . ? F2 C2 C1 112.9(7) . . ? F1 C2 C1 117.1(7) . . ? F5 C3 F6 110.9(6) . . ? F5 C3 F4 111.0(6) . . ? F6 C3 F4 111.2(6) . . ? F5 C3 C1 108.1(7) . . ? F6 C3 C1 111.1(8) . . ? F4 C3 C1 104.2(6) . . ? F9 C4 F8 104.9(7) . . ? F9 C4 F7 104.2(7) . . ? F8 C4 F7 104.8(7) . . ? F9 C4 C1 116.0(9) . . ? F8 C4 C1 118.9(8) . . ? F7 C4 C1 106.4(8) . . ? F34 C16 F36 111.7(6) . . ? F34 C16 F35 111.4(6) . . ? F36 C16 F35 111.4(6) . . ? F34 C16 C13 110.9(6) . . ? F36 C16 C13 99.8(9) . . ? F35 C16 C13 111.2(7) . . ? F29 C14 F30 105.9(6) . . ? F29 C14 F28 105.9(5) . . ? F30 C14 F28 105.8(6) . . ? F29 C14 C13 116.3(6) . . ? F30 C14 C13 113.4(7) . . ? F28 C14 C13 108.8(6) . . ? F33 C15 F31 109.7(6) . . ? F33 C15 F32 109.4(5) . . ? F31 C15 F32 108.9(6) . . ? F33 C15 C13 111.8(7) . . ? F31 C15 C13 108.8(6) . . ? F32 C15 C13 108.3(6) . . ? F2A3 C2A F2A2 108.5(14) . . ? F2A3 C2A F2A1 99.7(13) . . ? F2A2 C2A F2A1 105.4(14) . . ? F2A3 C2A C1 115.2(12) . . ? F2A2 C2A C1 110.0(11) . . ? F2A1 C2A C1 117.1(15) . . ? F3A3 C3A F3A2 107.3(16) . . ? F3A3 C3A F3A1 103.3(16) . . ? F3A2 C3A F3A1 105.6(14) . . ? F3A3 C3A C1 118.5(13) . . ? F3A2 C3A C1 113.2(16) . . ? F3A1 C3A C1 107.8(14) . . ? F4A3 C4A F4A2 105.4(13) . . ? F4A3 C4A F4A1 102.8(13) . . ? F4A2 C4A F4A1 105.5(14) . . ? F4A3 C4A C1 112.1(14) . . ? F4A2 C4A C1 106.8(12) . . ? F4A1 C4A C1 122.9(13) . . ? F14C C14A F14A 104.5(12) . . ? F14C C14A F14B 104.2(13) . . ? F14A C14A F14B 107.3(13) . . ? F14C C14A C13 112.4(11) . . ? F14A C14A C13 108.4(13) . . ? F14B C14A C13 119.1(11) . . ? F16C C16A F16B 103.9(14) . . ? F16C C16A F16A 102.7(16) . . ? F16B C16A F16A 101.1(14) . . ? F16C C16A C13 118.1(19) . . ? F16B C16A C13 105.6(13) . . ? F16A C16A C13 122.8(11) . . ? F80C C80 F80A 103.2(17) . . ? F80C C80 F80B 101.2(13) . . ? F80A C80 F80B 104.7(14) . . ? F80C C80 C13 109.4(13) . . ? F80A C80 C13 115.5(14) . . ? F80B C80 C13 120.6(14) . . ? O5 Ag1 O7 76.2(4) . . ? O5 Ag1 Se1 138.0(3) . . ? O7 Ag1 Se1 117.2(3) . . ? O5 Ag1 Se2 142.6(3) . . ? O7 Ag1 Se2 93.6(3) . . ? Se1 Ag1 Se2 78.77(6) . . ? O5 Ag1 Se3 101.5(3) . 2_656 ? O7 Ag1 Se3 160.4(3) . 2_656 ? Se1 Ag1 Se3 77.81(6) . 2_656 ? Se2 Ag1 Se3 76.30(6) . 2_656 ? O5 S1 O6 121.6(7) . . ? O8 S2 O7 116.3(9) . . ? S1 O5 Ag1 165.6(9) . . ? S2 O7 Ag1 135.8(8) . . ? Se2 Se1 Se3 100.21(8) 2_656 . ? Se2 Se1 Ag1 91.79(7) 2_656 . ? Se3 Se1 Ag1 90.33(6) . . ? Se1 Se2 Se3 100.55(7) 2_656 . ? Se1 Se2 Ag1 91.95(7) 2_656 . ? Se3 Se2 Ag1 88.15(7) . . ? Se2 Se3 Se1 99.75(8) . . ? Se2 Se3 Ag1 87.65(7) . 2_656 ? Se1 Se3 Ag1 89.99(6) . 2_656 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.96 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.299 _refine_diff_density_min -1.370 _refine_diff_density_rms 0.238