Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 X-Sun-Data-Type: default X-Sun-Data-Description: default X-Sun-Data-Name: 182_1851 X-Sun-Charset: us-ascii X-Sun-Content-Lines: 1464 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first 51 _journal_year 2001 loop_ _publ_author_name 'R.Malleier' 'H.Kopacka' 'W.Schuh' 'K.Wurst' 'P.Peringer' data_3c _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C50 H98 F12 Hg4 O37 S5' _chemical_formula_weight 2481.94 _chemical_melting_point ? _chemical_compound_source ? 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' 'H' 'H' 0.0000 0.0000 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hg' 'Hg' -2.3894 9.2266 '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 12.289(2) _cell_length_b 15.902(4) _cell_length_c 21.254(4) _cell_angle_alpha 92.25(2) _cell_angle_beta 93.06(2) _cell_angle_gamma 93.35(2) _cell_volume 4136.7(15) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 5.4 _cell_measurement_theta_max 12.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.993 _exptl_crystal_density_method ? _exptl_crystal_F_000 2404 _exptl_absorpt_coefficient_mu 7.635 _exptl_absorpt_correction_type PSI-scan _exptl_absorpt_correction_T_min 0.348 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker P4' _diffrn_measurement_method omega-scans _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8498 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 20.50 _reflns_number_total 8004 _reflns_number_observed 5405 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; 2:1 disordering of water molecule O37; 1:1 disordering of crown-ether at Hg2 (atoms of the ether were refined isotropically), H-Atoms at water molecules were omitted ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+23.9249P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7213 _refine_ls_number_parameters 954 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1036 _refine_ls_R_factor_obs 0.0566 _refine_ls_wR_factor_all 0.1483 _refine_ls_wR_factor_obs 0.1227 _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_obs 1.112 _refine_ls_restrained_S_all 1.072 _refine_ls_restrained_S_obs 1.112 _refine_ls_shift/esd_max -0.016 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Hg1 Hg 0.20490(6) 0.30793(4) 0.56778(4) 0.0444(3) Uani 1 d . . Hg2 Hg 0.31337(7) 0.18768(5) 0.60320(5) 0.0600(3) Uani 1 d . . Hg3 Hg 1.31163(7) -0.25348(6) 0.97936(5) 0.0695(3) Uani 1 d . . Hg4 Hg 1.16290(7) -0.26230(5) 0.89260(4) 0.0585(3) Uani 1 d . . S1 S 0.1773(4) 0.5058(3) 0.5650(3) 0.0480(14) Uani 1 d . . S2 S 0.2894(6) 0.7565(4) 0.6269(3) 0.068(2) Uani 1 d . . S3 S -0.2368(7) 0.4632(4) 0.7198(3) 0.086(2) Uani 1 d . . S4 S 1.7307(6) -0.2754(5) 1.0876(3) 0.084(2) Uani 1 d . . S5 S 0.1692(6) -0.0047(5) 0.2911(4) 0.088(2) Uani 1 d . . O1 O 0.3880(12) 0.4024(8) 0.5109(8) 0.060(4) Uani 1 d . . O2 O 0.3773(11) 0.4065(8) 0.6446(7) 0.057(4) Uani 1 d . . O3 O 0.1635(16) 0.3786(9) 0.6936(7) 0.074(5) Uani 1 d . . O4 O 0.0125(14) 0.2618(9) 0.6211(8) 0.072(5) Uani 1 d . . O5 O 0.0244(12) 0.2517(8) 0.4890(8) 0.071(5) Uani 1 d . . O6 O 0.2332(14) 0.2819(9) 0.4424(6) 0.059(4) Uani 1 d . . O12 O 0.1255(10) 0.4213(7) 0.5403(6) 0.053(4) Uani 1 d . . O13 O 1.2572(15) -0.4083(12) 1.0336(9) 0.092(6) Uani 1 d . . O14 O 1.4269(11) -0.4019(9) 0.9499(7) 0.058(4) Uani 1 d . . O15 O 1.4709(11) -0.2504(9) 0.8883(6) 0.060(4) Uani 1 d . . O16 O 1.4264(13) -0.0966(11) 0.9466(10) 0.094(6) Uani 1 d . . O17 O 1.2512(16) -0.0968(15) 1.0315(14) 0.139(10) Uani 1 d . . O18 O 1.2158(15) -0.2522(18) 1.0941(9) 0.117(8) Uani 1 d . . O19 O 1.1006(11) -0.2661(8) 0.7883(6) 0.056(4) Uani 1 d . . O20 O 1.1573(12) -0.4258(9) 0.8359(7) 0.062(4) Uani 1 d . . O21 O 0.9855(12) -0.3704(10) 0.8975(7) 0.072(5) Uani 1 d . . O22 O 0.9662(13) -0.2006(10) 0.9211(8) 0.086(5) Uani 1 d . . O23 O 1.1173(13) -0.1096(10) 0.8555(10) 0.079(5) Uani 1 d . . O24 O -0.3529(23) 0.4327(32) 0.7605(18) 0.434(39) Uani 1 d . . O25 O -0.1549(16) 0.4386(17) 0.7560(10) 0.171(12) Uani 1 d . . O26 O -0.2628(18) 0.4575(14) 0.6592(8) 0.138(9) Uani 1 d . . O27 O 0.1922(15) 0.7705(18) 0.6497(9) 0.155(10) Uani 1 d . . O28 O 0.3152(20) 0.7979(28) 0.5775(17) 0.305(26) Uani 1 d . . O29 O 0.3047(23) 0.6729(17) 0.6158(20) 0.284(23) Uani 1 d . . O30 O 1.6662(12) -0.2542(12) 1.0334(7) 0.091(6) Uani 1 d . . O31 O 1.6735(14) -0.2850(13) 1.1425(8) 0.119(7) Uani 1 d . . O32 O 1.8089(18) -0.3339(12) 1.0777(10) 0.135(8) Uani 1 d . . O33 O 0.1117(15) -0.0275(12) 0.2333(10) 0.114(7) Uani 1 d . . O34 O 0.2137(17) -0.0682(14) 0.3229(11) 0.148(9) Uani 1 d . . O35 O 0.1110(16) 0.0526(12) 0.3315(9) 0.124(7) Uani 1 d . . O36 O 1.4493(13) -0.2388(12) 1.0517(8) 0.106(6) Uani 1 d . . O37A O 1.4702(21) -0.3337(25) 1.1630(14) 0.152(15) Uani 0.67 d P . O37B O 1.4521(46) -0.1908(40) 1.1606(21) 0.121(23) Uani 0.33 d P . C1 C 0.4806(21) 0.4118(15) 0.5535(16) 0.084(9) Uani 1 d . . H1A H 0.5406 0.4422 0.5338 0.100 Uiso 1 calc . . H1B H 0.5044 0.3562 0.5644 0.100 Uiso 1 calc . . C2 C 0.4523(19) 0.4598(14) 0.6119(14) 0.074(8) Uani 1 d . . H2A H 0.5183 0.4747 0.6389 0.089 Uiso 1 calc . . H2B H 0.4185 0.5119 0.6007 0.089 Uiso 1 calc . . C3 C 0.3439(24) 0.4463(15) 0.7010(17) 0.096(10) Uani 1 d . . H3A H 0.3107 0.4991 0.6912 0.115 Uiso 1 calc . . H3B H 0.4075 0.4596 0.7302 0.115 Uiso 1 calc . . C4 C 0.2641(33) 0.3893(17) 0.7307(12) 0.098(10) Uani 1 d . . H4A H 0.2946 0.3342 0.7358 0.118 Uiso 1 calc . . H4B H 0.2504 0.4126 0.7727 0.118 Uiso 1 calc . . C5 C 0.0856(33) 0.3230(16) 0.7188(13) 0.116(13) Uani 1 d . . H5A H 0.0654 0.3456 0.7598 0.140 Uiso 1 calc . . H5B H 0.1166 0.2683 0.7250 0.140 Uiso 1 calc . . C6 C -0.0100(27) 0.3122(21) 0.6760(18) 0.114(11) Uiso 1 d . . H6A H -0.0703 0.2848 0.6974 0.137 Uiso 1 calc . . H6B H -0.0322 0.3675 0.6632 0.137 Uiso 1 calc . . C7 C -0.0823(22) 0.2423(16) 0.5798(20) 0.103(11) Uani 1 d . . H7A H -0.1173 0.2941 0.5691 0.123 Uiso 1 calc . . H7B H -0.1351 0.2053 0.6001 0.123 Uiso 1 calc . . C8 C -0.0461(22) 0.2002(17) 0.5230(17) 0.092(9) Uani 1 d . . H8A H -0.0086 0.1500 0.5349 0.110 Uiso 1 calc . . H8B H -0.1102 0.1815 0.4955 0.110 Uiso 1 calc . . C9 C 0.0620(22) 0.2110(18) 0.4331(15) 0.087(9) Uani 1 d . . H9A H -0.0003 0.1947 0.4035 0.105 Uiso 1 calc . . H9B H 0.0982 0.1600 0.4442 0.105 Uiso 1 calc . . C10 C 0.1406(30) 0.2706(20) 0.4025(12) 0.096(10) Uani 1 d . . H10A H 0.1588 0.2468 0.3614 0.115 Uiso 1 calc . . H10B H 0.1081 0.3247 0.3961 0.115 Uiso 1 calc . . C11 C 0.3085(27) 0.3361(16) 0.4153(10) 0.075(8) Uani 1 d . . H11A H 0.2764 0.3901 0.4081 0.091 Uiso 1 calc . . H11B H 0.3270 0.3117 0.3744 0.091 Uiso 1 calc . . C12 C 0.4084(22) 0.3503(14) 0.4567(14) 0.077(8) Uani 1 d . . H12A H 0.4332 0.2961 0.4703 0.092 Uiso 1 calc . . H12B H 0.4664 0.3777 0.4334 0.092 Uiso 1 calc . . C23 C 1.3301(24) -0.4724(18) 1.0241(18) 0.106(10) Uani 1 d . . H23A H 1.2946 -0.5271 1.0332 0.128 Uiso 1 calc . . H23B H 1.3946 -0.4621 1.0532 0.128 Uiso 1 calc . . C24 C 1.3636(22) -0.4747(17) 0.9596(14) 0.085(8) Uani 1 d . . H24A H 1.4057 -0.5242 0.9519 0.102 Uiso 1 calc . . H24B H 1.2991 -0.4787 0.9302 0.102 Uiso 1 calc . . C25 C 1.4548(17) -0.3999(13) 0.8861(12) 0.062(7) Uani 1 d . . H25A H 1.3881 -0.4000 0.8587 0.074 Uiso 1 calc . . H25B H 1.4928 -0.4505 0.8750 0.074 Uiso 1 calc . . C26 C 1.5255(19) -0.3244(18) 0.8754(12) 0.082(8) Uani 1 d . . H26A H 1.5923 -0.3242 0.9027 0.099 Uiso 1 calc . . H26B H 1.5462 -0.3256 0.8315 0.099 Uiso 1 calc . . C27 C 1.5286(20) -0.1751(16) 0.8759(11) 0.078(8) Uani 1 d . . H27A H 1.5541 -0.1779 0.8330 0.093 Uiso 1 calc . . H27B H 1.5923 -0.1654 0.9056 0.093 Uiso 1 calc . . C28 C 1.4562(22) -0.1079(16) 0.8827(16) 0.092(9) Uani 1 d . . H28A H 1.4920 -0.0554 0.8693 0.110 Uiso 1 calc . . H28B H 1.3902 -0.1205 0.8553 0.110 Uiso 1 calc . . C29 C 1.3572(23) -0.0296(17) 0.9560(22) 0.124(14) Uani 1 d . . H29A H 1.2915 -0.0384 0.9277 0.149 Uiso 1 calc . . H29B H 1.3951 0.0238 0.9460 0.149 Uiso 1 calc . . C30 C 1.3272(27) -0.0257(28) 1.0198(24) 0.173(23) Uani 1 d . . H30A H 1.2928 0.0273 1.0285 0.207 Uiso 1 calc . . H30B H 1.3926 -0.0269 1.0481 0.207 Uiso 1 calc . . C31 C 1.2295(33) -0.0966(28) 1.0955(21) 0.157(18) Uani 1 d . . H31A H 1.1943 -0.0453 1.1080 0.189 Uiso 1 calc . . H31B H 1.2973 -0.0995 1.1216 0.189 Uiso 1 calc . . C32 C 1.1535(27) -0.1745(34) 1.1031(17) 0.151(16) Uani 1 d . . H32A H 1.1248 -0.1727 1.1453 0.181 Uiso 1 calc . . H32B H 1.0918 -0.1756 1.0719 0.181 Uiso 1 calc . . C33 C 1.1537(24) -0.3271(34) 1.1024(13) 0.129(15) Uani 1 d . . H33A H 1.0923 -0.3337 1.0709 0.155 Uiso 1 calc . . H33B H 1.1247 -0.3264 1.1445 0.155 Uiso 1 calc . . C34 C 1.2268(27) -0.3974(27) 1.0950(20) 0.136(14) Uani 1 d . . H34A H 1.2924 -0.3860 1.1230 0.163 Uiso 1 calc . . H34B H 1.1894 -0.4496 1.1078 0.163 Uiso 1 calc . . C35 C 1.0602(21) -0.3448(17) 0.7569(10) 0.082(8) Uani 1 d . . H35A H 1.0503 -0.3383 0.7113 0.098 Uiso 1 calc . . H35B H 0.9900 -0.3638 0.7729 0.098 Uiso 1 calc . . C36 C 1.1464(20) -0.4083(13) 0.7712(13) 0.075(7) Uani 1 d . . H36A H 1.1266 -0.4609 0.7467 0.091 Uiso 1 calc . . H36B H 1.2170 -0.3859 0.7577 0.091 Uiso 1 calc . . C37 C 1.0779(23) -0.4843(15) 0.8550(14) 0.088(8) Uani 1 d . . H37A H 1.1104 -0.5377 0.8639 0.106 Uiso 1 calc . . H37B H 1.0201 -0.4950 0.8216 0.106 Uiso 1 calc . . C38 C 1.0305(21) -0.4468(16) 0.9150(14) 0.087(9) Uani 1 d . . H38A H 0.9739 -0.4857 0.9302 0.104 Uiso 1 calc . . H38B H 1.0880 -0.4359 0.9486 0.104 Uiso 1 calc . . C39 C 0.9149(22) -0.3404(19) 0.9430(13) 0.088(8) Uani 1 d . . H39A H 0.9542 -0.3329 0.9844 0.106 Uiso 1 calc . . H39B H 0.8527 -0.3811 0.9464 0.106 Uiso 1 calc . . C40 C 0.8761(19) -0.2586(18) 0.9226(13) 0.086(9) Uani 1 d . . H40A H 0.8389 -0.2659 0.8806 0.104 Uiso 1 calc . . H40B H 0.8241 -0.2378 0.9520 0.104 Uiso 1 calc . . C41 C 0.9463(24) -0.1201(20) 0.9020(13) 0.096(9) Uani 1 d . . H41A H 0.9049 -0.0920 0.9339 0.115 Uiso 1 calc . . H41B H 0.9007 -0.1250 0.8626 0.115 Uiso 1 calc . . C42 C 1.0472(25) -0.0663(14) 0.8918(15) 0.099(10) Uani 1 d . . H42A H 1.0272 -0.0153 0.8707 0.119 Uiso 1 calc . . H42B H 1.0842 -0.0491 0.9327 0.119 Uiso 1 calc . . C43 C 1.0936(21) -0.1173(16) 0.7913(15) 0.078(8) Uani 1 d . . H43A H 1.1621 -0.1118 0.7699 0.093 Uiso 1 calc . . H43B H 1.0498 -0.0705 0.7790 0.093 Uiso 1 calc . . C44 C 1.0333(17) -0.1985(16) 0.7685(10) 0.062(6) Uani 1 d . . H44A H 0.9620 -0.2039 0.7870 0.074 Uiso 1 calc . . H44B H 1.0219 -0.2003 0.7225 0.074 Uiso 1 calc . . C45 C 0.0638(17) 0.5602(12) 0.5873(10) 0.056(6) Uani 1 d . . H45A H 0.0380 0.5384 0.6261 0.084 Uiso 1 calc . . H45B H 0.0061 0.5525 0.5543 0.084 Uiso 1 calc . . H45C H 0.0849 0.6198 0.5937 0.084 Uiso 1 calc . . C46 C 0.2028(19) 0.5589(12) 0.4956(10) 0.066(7) Uani 1 d . . H46A H 0.2652 0.5361 0.4763 0.099 Uiso 1 calc . . H46B H 0.2181 0.6185 0.5059 0.099 Uiso 1 calc . . H46C H 0.1392 0.5512 0.4664 0.099 Uiso 1 calc . . C47 C 0.3892(32) 0.7861(23) 0.6968(34) 0.188(28) Uani 1 d . . C48 C -0.2925(25) 0.5487(22) 0.7556(15) 0.106(12) Uani 1 d . . C49 C 1.8185(25) -0.1781(20) 1.1056(18) 0.095(9) Uani 1 d . . C50 C 0.2769(26) 0.0600(18) 0.2713(16) 0.088(9) Uani 1 d . . F1 F 0.3923(28) 0.8556(25) 0.7025(25) 0.367(31) Uani 1 d . . F2 F 0.3778(28) 0.7240(39) 0.7320(18) 0.364(31) Uani 1 d . . F3 F 0.4879(16) 0.7677(14) 0.6731(10) 0.155(8) Uani 1 d . . F4 F -0.2145(21) 0.6249(14) 0.7386(12) 0.185(10) Uani 1 d . . F5 F -0.3660(14) 0.5867(9) 0.7289(7) 0.106(5) Uani 1 d . . F6 F -0.2662(15) 0.5719(10) 0.8137(7) 0.121(6) Uani 1 d . . F7 F 1.8812(18) -0.1877(16) 1.1564(9) 0.174(9) Uani 1 d . . F8 F 1.8747(16) -0.1553(12) 1.0583(9) 0.149(8) Uani 1 d . . F9 F 1.7531(21) -0.1179(13) 1.1188(10) 0.172(9) Uani 1 d . . F10 F 0.2516(16) 0.1292(13) 0.2429(11) 0.163(8) Uani 1 d . . F11 F 0.3465(16) 0.0858(15) 0.3192(11) 0.173(10) Uani 1 d . . F12 F 0.3434(14) 0.0236(13) 0.2327(10) 0.150(8) Uani 1 d . . O7 O 0.5200(19) 0.2000(14) 0.5799(12) 0.124(9) Uiso 1 d . . O10 O 0.1746(13) 0.0540(10) 0.5538(8) 0.084(5) Uiso 1 d . . O8 O 0.4277(27) 0.1220(20) 0.6710(16) 0.080(9) Uiso 0.50 d P 1 O9 O 0.2503(28) 0.0682(20) 0.6705(15) 0.060(9) Uiso 0.50 d P 1 O11 O 0.3692(33) 0.0685(21) 0.5092(22) 0.063(11) Uiso 0.50 d P 1 C13 C 0.5502(40) 0.2094(28) 0.6141(28) 0.051(13) Uiso 0.50 d P 1 H13A H 0.5177 0.2564 0.6360 0.061 Uiso 0.50 calc P 1 H13B H 0.6278 0.2247 0.6100 0.061 Uiso 0.50 calc P 1 C14 C 0.5342(58) 0.1134(42) 0.6592(33) 0.133(23) Uiso 0.50 d P 1 H14A H 0.5449 0.0621 0.6338 0.159 Uiso 0.50 calc P 1 H14B H 0.5818 0.1158 0.6977 0.159 Uiso 0.50 calc P 1 C15 C 0.3831(51) 0.0692(39) 0.7275(29) 0.085(17) Uiso 0.50 d P 1 H15A H 0.3899 0.0090 0.7184 0.102 Uiso 0.50 calc P 1 H15B H 0.4267 0.0854 0.7665 0.102 Uiso 0.50 calc P 1 C16 C 0.2868(38) 0.0827(26) 0.7344(21) 0.049(11) Uiso 0.50 d P 1 H16A H 0.2775 0.1407 0.7497 0.059 Uiso 0.50 calc P 1 H16B H 0.2518 0.0428 0.7621 0.059 Uiso 0.50 calc P 1 C17 C 0.1426(55) 0.0302(43) 0.6486(37) 0.097(20) Uiso 0.50 d P 1 H17A H 0.1188 -0.0113 0.6788 0.117 Uiso 0.50 calc P 1 H17B H 0.0899 0.0741 0.6478 0.117 Uiso 0.50 calc P 1 C18 C 0.1421(104) -0.0063(77) 0.5935(64) 0.207(65) Uiso 0.50 d P 1 H18A H 0.0686 -0.0300 0.5804 0.248 Uiso 0.50 calc P 1 H18B H 0.1923 -0.0519 0.5936 0.248 Uiso 0.50 calc P 1 C19 C 0.2201(40) 0.0010(29) 0.5169(27) 0.051(17) Uiso 0.50 d P 1 H19A H 0.1643 -0.0350 0.4923 0.061 Uiso 0.50 calc P 1 H19B H 0.2666 -0.0351 0.5416 0.061 Uiso 0.50 calc P 1 C20 C 0.2818(69) 0.0487(45) 0.4774(35) 0.089(27) Uiso 0.50 d P 1 H20A H 0.2958 0.0158 0.4390 0.106 Uiso 0.50 calc P 1 H20B H 0.2446 0.0990 0.4655 0.106 Uiso 0.50 calc P 1 C21 C 0.4461(65) 0.1123(41) 0.4754(36) 0.121(25) Uiso 0.50 d P 1 H21A H 0.4152 0.1615 0.4565 0.145 Uiso 0.50 calc P 1 H21B H 0.4724 0.0759 0.4419 0.145 Uiso 0.50 calc P 1 C22 C 0.5431(56) 0.1408(40) 0.5273(36) 0.087(21) Uiso 0.50 d P 1 H22A H 0.5691 0.0896 0.5457 0.104 Uiso 0.50 calc P 1 H22B H 0.6036 0.1665 0.5050 0.104 Uiso 0.50 calc P 1 O8A O 0.4391(22) 0.1744(17) 0.7076(14) 0.057(8) Uiso 0.50 d P 2 O9A O 0.2226(37) 0.1103(26) 0.7020(22) 0.113(13) Uiso 0.50 d P 2 O11A O 0.4040(22) 0.0845(15) 0.5316(13) 0.028(8) Uiso 0.50 d P 2 C13A C 0.5842(32) 0.2267(23) 0.6565(21) 0.041(10) Uiso 0.50 d P 2 H13C H 0.6634 0.2256 0.6533 0.049 Uiso 0.50 calc P 2 H13D H 0.5684 0.2847 0.6682 0.049 Uiso 0.50 calc P 2 C14A C 0.5541(32) 0.1750(24) 0.7059(19) 0.048(11) Uiso 0.50 d P 2 H14C H 0.5888 0.1976 0.7461 0.057 Uiso 0.50 calc P 2 H14D H 0.5770 0.1177 0.6982 0.057 Uiso 0.50 calc P 2 C15A C 0.3997(46) 0.1180(38) 0.7490(27) 0.087(18) Uiso 0.50 d P 2 H15C H 0.3618 0.1461 0.7826 0.105 Uiso 0.50 calc P 2 H15D H 0.4581 0.0862 0.7679 0.105 Uiso 0.50 calc P 2 C16A C 0.3012(86) 0.0474(55) 0.6955(50) 0.158(33) Uiso 0.50 d P 2 H16C H 0.3248 0.0392 0.6525 0.190 Uiso 0.50 calc P 2 H16D H 0.2799 -0.0066 0.7134 0.190 Uiso 0.50 calc P 2 C17A C 0.1261(49) 0.0730(39) 0.6666(28) 0.088(19) Uiso 0.50 d P 2 H17C H 0.0803 0.1200 0.6576 0.105 Uiso 0.50 calc P 2 H17D H 0.0870 0.0385 0.6964 0.105 Uiso 0.50 calc P 2 C18A C 0.1222(45) 0.0150(35) 0.6004(29) 0.050(15) Uiso 0.50 d P 2 H18C H 0.1559 -0.0381 0.6086 0.060 Uiso 0.50 calc P 2 H18D H 0.0459 0.0015 0.5861 0.060 Uiso 0.50 calc P 2 C19A C 0.2131(40) 0.0136(29) 0.4908(25) 0.040(14) Uiso 0.50 d P 2 H19C H 0.1570 0.0174 0.4567 0.048 Uiso 0.50 calc P 2 H19D H 0.2263 -0.0460 0.4960 0.048 Uiso 0.50 calc P 2 C20A C 0.3235(53) 0.0647(31) 0.4746(27) 0.042(16) Uiso 0.50 d P 2 H20C H 0.3597 0.0319 0.4428 0.051 Uiso 0.50 calc P 2 H20D H 0.3049 0.1178 0.4561 0.051 Uiso 0.50 calc P 2 C21A C 0.5005(39) 0.1167(24) 0.5040(22) 0.025(10) Uiso 0.50 d P 2 H21C H 0.4858 0.1660 0.4794 0.030 Uiso 0.50 calc P 2 H21D H 0.5302 0.0737 0.4767 0.030 Uiso 0.50 calc P 2 C22A C 0.5824(31) 0.1420(22) 0.5635(20) 0.034(10) Uiso 0.50 d P 2 H22C H 0.5882 0.0975 0.5939 0.041 Uiso 0.50 calc P 2 H22D H 0.6549 0.1635 0.5522 0.041 Uiso 0.50 calc P 2 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 Hg1 0.0479(6) 0.0324(4) 0.0542(6) 0.0047(4) 0.0059(4) 0.0083(4) Hg2 0.0682(7) 0.0436(5) 0.0734(7) 0.0193(5) 0.0216(5) 0.0186(5) Hg3 0.0462(6) 0.0987(8) 0.0600(7) -0.0215(5) -0.0127(5) 0.0043(5) Hg4 0.0473(6) 0.0666(6) 0.0585(6) -0.0082(5) -0.0112(5) -0.0015(5) S1 0.055(4) 0.030(3) 0.057(4) 0.002(3) -0.015(3) 0.003(3) S2 0.072(5) 0.066(4) 0.066(5) 0.004(4) 0.000(4) 0.001(4) S3 0.127(7) 0.080(5) 0.050(5) -0.011(4) -0.031(4) 0.033(5) S4 0.079(5) 0.119(6) 0.056(5) 0.024(4) 0.005(4) 0.016(5) S5 0.072(5) 0.104(6) 0.088(6) 0.009(5) 0.013(5) 0.008(5) O1 0.049(10) 0.044(9) 0.090(13) 0.017(8) 0.028(10) 0.001(8) O2 0.054(10) 0.053(9) 0.059(11) -0.003(8) -0.012(8) -0.009(8) O3 0.111(14) 0.063(10) 0.052(11) 0.019(9) 0.020(11) 0.019(10) O4 0.063(12) 0.050(9) 0.106(14) 0.013(9) 0.034(10) -0.004(9) O5 0.057(11) 0.045(9) 0.107(14) -0.004(10) -0.020(10) 0.002(9) O6 0.074(11) 0.069(10) 0.034(10) -0.001(8) -0.002(9) 0.006(9) O12 0.056(9) 0.045(8) 0.058(10) 0.015(7) -0.009(7) 0.006(7) O13 0.075(13) 0.139(17) 0.060(13) 0.033(12) -0.011(10) -0.005(12) O14 0.040(9) 0.065(10) 0.065(12) 0.012(8) -0.005(8) -0.023(8) O15 0.054(10) 0.062(10) 0.063(10) 0.000(8) 0.017(8) 0.002(9) O16 0.053(11) 0.093(14) 0.132(18) -0.045(12) 0.007(11) 0.000(10) O17 0.040(13) 0.151(20) 0.215(28) -0.112(19) -0.001(14) 0.004(13) O18 0.037(12) 0.204(24) 0.099(16) -0.077(16) -0.007(10) -0.018(15) O19 0.065(10) 0.054(9) 0.050(10) -0.002(8) 0.004(8) 0.015(8) O20 0.069(11) 0.058(10) 0.056(11) 0.010(8) -0.002(9) -0.009(9) O21 0.056(11) 0.089(12) 0.069(12) 0.000(10) 0.010(9) -0.020(9) O22 0.065(12) 0.062(11) 0.133(16) 0.001(10) 0.007(10) 0.022(10) O23 0.056(11) 0.067(11) 0.112(16) 0.001(11) -0.006(11) -0.014(9) O24 0.187(27) 0.737(80) 0.360(47) 0.478(57) -0.142(29) -0.289(41) O25 0.113(17) 0.313(31) 0.097(16) -0.051(18) -0.021(13) 0.154(20) O26 0.177(21) 0.209(22) 0.040(13) -0.008(13) 0.019(13) 0.108(18) O27 0.063(14) 0.321(32) 0.081(15) -0.031(17) -0.001(11) 0.038(17) O28 0.110(20) 0.540(62) 0.290(39) 0.339(45) 0.022(22) 0.008(28) O29 0.190(29) 0.145(23) 0.486(58) -0.126(30) -0.220(33) 0.069(21) O30 0.053(10) 0.178(17) 0.042(10) 0.029(11) 0.001(8) 0.000(11) O31 0.091(14) 0.191(20) 0.079(14) 0.055(13) 0.033(12) -0.003(13) O32 0.153(20) 0.114(15) 0.149(20) 0.024(13) 0.064(16) 0.051(15) O33 0.098(15) 0.125(16) 0.115(18) -0.020(13) -0.014(13) 0.006(13) O34 0.111(17) 0.149(18) 0.197(24) 0.112(18) 0.042(16) 0.016(15) O35 0.125(17) 0.133(16) 0.120(17) -0.020(13) 0.052(14) 0.033(14) O36 0.062(12) 0.169(18) 0.079(13) -0.038(12) -0.032(10) 0.011(12) O37A 0.069(20) 0.282(43) 0.103(25) 0.092(27) -0.021(17) -0.043(23) O37B 0.123(47) 0.195(61) 0.038(32) -0.078(36) -0.009(30) 0.008(43) C1 0.058(19) 0.057(16) 0.139(28) 0.042(17) 0.014(19) -0.006(14) C2 0.037(15) 0.053(15) 0.129(25) -0.006(16) -0.016(15) -0.008(13) C3 0.102(23) 0.048(16) 0.127(28) -0.014(18) -0.074(21) -0.004(16) C4 0.176(34) 0.068(19) 0.053(20) -0.011(15) 0.011(22) 0.026(22) C5 0.231(39) 0.064(17) 0.067(21) 0.019(15) 0.102(26) 0.021(21) C7 0.039(18) 0.057(17) 0.216(38) 0.015(20) 0.046(23) -0.001(14) C8 0.042(17) 0.080(19) 0.150(30) 0.038(21) -0.036(18) -0.006(16) C9 0.064(19) 0.099(21) 0.094(23) -0.047(19) -0.045(16) 0.041(17) C10 0.134(29) 0.114(24) 0.043(18) -0.025(17) -0.007(20) 0.055(23) C11 0.121(25) 0.080(18) 0.032(16) 0.001(13) 0.029(17) 0.034(19) C12 0.078(20) 0.063(16) 0.100(23) 0.025(16) 0.066(19) 0.019(15) C23 0.068(21) 0.096(22) 0.157(35) 0.039(22) 0.006(21) 0.001(18) C24 0.069(19) 0.091(21) 0.093(23) 0.013(17) 0.007(17) -0.010(16) C25 0.041(14) 0.052(14) 0.092(22) 0.025(14) -0.004(14) -0.002(12) C26 0.060(17) 0.114(22) 0.075(19) -0.006(16) 0.011(14) 0.017(18) C27 0.070(18) 0.076(18) 0.081(20) -0.004(15) 0.019(15) -0.054(16) C28 0.070(20) 0.059(17) 0.143(30) -0.008(18) -0.010(19) -0.003(15) C29 0.053(20) 0.063(18) 0.249(46) -0.046(24) -0.031(24) 0.018(16) C30 0.040(22) 0.188(41) 0.274(54) -0.178(40) -0.023(26) 0.027(24) C31 0.109(33) 0.197(42) 0.158(39) -0.119(34) 0.011(28) 0.029(30) C32 0.073(25) 0.255(50) 0.117(30) -0.090(31) 0.008(21) 0.004(31) C33 0.048(21) 0.282(51) 0.048(19) -0.037(24) -0.008(15) -0.029(29) C34 0.057(23) 0.224(42) 0.127(35) 0.075(30) -0.013(22) -0.017(24) C35 0.102(21) 0.110(21) 0.035(15) -0.006(14) -0.012(14) 0.027(18) C36 0.090(20) 0.048(14) 0.092(22) 0.006(14) 0.018(16) 0.022(14) C37 0.095(22) 0.067(17) 0.099(24) -0.009(17) 0.007(18) -0.020(17) C38 0.079(19) 0.070(17) 0.109(24) 0.062(17) -0.036(17) -0.019(15) C39 0.070(20) 0.107(23) 0.082(21) 0.003(18) 0.007(16) -0.038(18) C40 0.045(17) 0.102(21) 0.106(23) -0.013(18) 0.023(15) -0.051(17) C41 0.096(24) 0.113(24) 0.078(21) -0.031(18) 0.001(17) 0.012(21) C42 0.081(22) 0.043(15) 0.170(30) -0.047(17) -0.007(20) 0.018(16) C43 0.076(19) 0.070(18) 0.095(23) 0.027(17) 0.044(17) 0.017(15) C44 0.043(14) 0.089(18) 0.054(16) 0.012(13) -0.012(12) 0.009(14) C45 0.057(15) 0.056(13) 0.057(15) -0.004(11) 0.023(12) 0.005(12) C46 0.086(18) 0.041(13) 0.068(17) -0.002(12) -0.009(14) -0.011(12) C47 0.052(26) 0.073(24) 0.420(87) -0.055(37) -0.104(38) 0.000(22) C48 0.079(22) 0.158(31) 0.077(23) -0.055(22) -0.045(18) 0.066(24) C49 0.060(21) 0.101(24) 0.118(31) 0.004(21) -0.011(20) -0.033(18) C50 0.097(25) 0.075(20) 0.096(25) 0.025(18) 0.024(21) 0.005(19) F1 0.211(33) 0.263(37) 0.593(75) -0.271(49) -0.127(39) 0.047(32) F2 0.172(29) 0.661(87) 0.249(35) 0.235(50) -0.090(24) -0.102(43) F3 0.094(15) 0.199(21) 0.168(19) -0.027(15) -0.008(13) 0.018(14) F4 0.206(25) 0.148(18) 0.192(25) -0.010(16) -0.021(19) -0.030(18) F5 0.111(13) 0.098(11) 0.106(13) -0.008(9) -0.030(10) 0.035(10) F6 0.189(18) 0.117(12) 0.052(11) -0.012(9) -0.026(11) 0.004(12) F7 0.145(18) 0.282(28) 0.083(14) -0.015(15) -0.030(13) -0.049(18) F8 0.133(16) 0.178(18) 0.132(17) -0.011(14) 0.039(14) -0.058(14) F9 0.234(26) 0.127(16) 0.160(20) -0.006(14) 0.030(18) 0.055(17) F10 0.140(17) 0.139(16) 0.211(23) 0.060(16) 0.002(16) -0.007(14) F11 0.108(15) 0.242(25) 0.153(20) 0.005(17) -0.018(14) -0.094(16) F12 0.101(14) 0.198(19) 0.161(19) 0.030(15) 0.067(14) 0.019(13) _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 Hg1 O12 2.185(11) . ? Hg1 Hg2 2.5108(12) . ? Hg1 O6 2.726(14) . ? Hg1 O4 2.750(14) . ? Hg1 O5 2.789(15) . ? Hg1 O2 2.942(14) . ? Hg1 O3 2.942(15) . ? Hg1 O1 2.970(12) . ? Hg2 O8 2.28(3) . ? Hg2 O9 2.53(3) . ? Hg2 O11A 2.54(2) . ? Hg2 O7 2.61(2) . ? Hg2 O8A 2.66(3) . ? Hg2 O10 2.78(2) . ? Hg2 O11 2.84(4) . ? Hg3 O36 2.219(15) . ? Hg3 Hg4 2.5201(14) . ? Hg3 O18 2.77(2) . ? Hg3 O13 2.82(2) . ? Hg3 O15 2.825(13) . ? Hg3 O17 2.84(2) . ? Hg3 O14 2.888(14) . ? Hg3 O16 2.92(2) . ? Hg4 O19 2.305(13) . ? Hg4 O23 2.66(2) . ? Hg4 O21 2.705(14) . ? Hg4 O22 2.750(15) . ? Hg4 O20 2.819(14) . ? S1 O12 1.515(13) . ? S1 C45 1.76(2) . ? S1 C46 1.76(2) . ? S2 O28 1.30(2) . ? S2 O27 1.34(2) . ? S2 O29 1.37(2) . ? S2 C47 1.90(5) . ? S3 O26 1.31(2) . ? S3 O25 1.32(2) . ? S3 C48 1.73(3) . ? S3 O24 1.76(3) . ? S4 O32 1.39(2) . ? S4 O31 1.40(2) . ? S4 O30 1.43(2) . ? S4 C49 1.85(3) . ? S5 O34 1.36(2) . ? S5 O33 1.41(2) . ? S5 O35 1.47(2) . ? S5 C50 1.71(3) . ? O1 C1 1.41(3) . ? O1 C12 1.43(3) . ? O2 C3 1.42(3) . ? O2 C2 1.44(3) . ? O3 C5 1.41(3) . ? O3 C4 1.43(3) . ? O4 C7 1.43(3) . ? O4 C6 1.44(4) . ? O5 C8 1.40(3) . ? O5 C9 1.44(3) . ? O6 C10 1.38(3) . ? O6 C11 1.39(3) . ? O13 C34 1.39(4) . ? O13 C23 1.41(3) . ? O14 C24 1.39(3) . ? O14 C25 1.42(3) . ? O15 C27 1.40(2) . ? O15 C26 1.41(3) . ? O16 C29 1.42(3) . ? O16 C28 1.43(3) . ? O17 C31 1.40(4) . ? O17 C30 1.46(5) . ? O18 C33 1.40(4) . ? O18 C32 1.50(4) . ? O19 C35 1.44(3) . ? O19 C44 1.45(2) . ? O20 C37 1.40(3) . ? O20 C36 1.41(3) . ? O21 C38 1.42(2) . ? O21 C39 1.42(3) . ? O22 C41 1.39(3) . ? O22 C40 1.40(2) . ? O23 C43 1.38(3) . ? O23 C42 1.38(3) . ? C1 C2 1.50(3) . ? C3 C4 1.48(4) . ? C5 C6 1.44(4) . ? C7 C8 1.46(4) . ? C9 C10 1.50(4) . ? C11 C12 1.47(3) . ? C23 C24 1.45(4) . ? C25 C26 1.47(3) . ? C27 C28 1.44(3) . ? C29 C30 1.42(5) . ? C31 C32 1.53(5) . ? C33 C34 1.48(5) . ? C35 C36 1.53(3) . ? C37 C38 1.54(4) . ? C39 C40 1.48(3) . ? C41 C42 1.50(4) . ? C43 C44 1.50(3) . ? C47 F1 1.11(4) . ? C47 F2 1.27(5) . ? C47 F3 1.38(5) . ? C48 F5 1.24(3) . ? C48 F6 1.29(3) . ? C48 F4 1.57(4) . ? C49 F8 1.30(3) . ? C49 F7 1.31(3) . ? C49 F9 1.32(3) . ? C50 F10 1.32(3) . ? C50 F12 1.33(3) . ? C50 F11 1.33(3) . ? O7 C13 0.80(6) . ? O7 C22A 1.28(4) . ? O7 C22 1.48(7) . ? O7 C13A 1.79(5) . ? O10 C19 1.30(5) . ? O10 C18 1.36(13) . ? O10 C18A 1.36(6) . ? O10 C19A 1.57(5) . ? O8 C14 1.36(7) . ? O8 C15 1.59(6) . ? O9 C16 1.41(6) . ? O9 C17 1.47(7) . ? O11 C20 1.26(8) . ? O11 C21 1.39(7) . ? C13 C14 1.84(8) . ? C15 C16 1.23(7) . ? C17 C18 1.29(14) . ? C18 C19 1.94(13) . ? C19 C20 1.38(9) . ? C21 C22 1.61(9) . ? O8A C15A 1.37(6) . ? O8A C14A 1.41(4) . ? O9A C16A 1.44(10) . ? O9A C17A 1.45(6) . ? O11A C21A 1.43(5) . ? O11A C20A 1.53(7) . ? C13A C14A 1.41(5) . ? C15A C16A 1.90(12) . ? C17A C18A 1.65(9) . ? C19A C20A 1.60(8) . ? C21A C22A 1.60(7) . ? 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 O12 Hg1 Hg2 174.0(3) . . ? O12 Hg1 O6 85.6(4) . . ? Hg2 Hg1 O6 95.8(3) . . ? O12 Hg1 O4 86.0(4) . . ? Hg2 Hg1 O4 98.2(3) . . ? O6 Hg1 O4 122.2(5) . . ? O12 Hg1 O5 74.2(4) . . ? Hg2 Hg1 O5 111.6(3) . . ? O6 Hg1 O5 61.5(5) . . ? O4 Hg1 O5 61.2(5) . . ? O12 Hg1 O2 92.3(4) . . ? Hg2 Hg1 O2 81.9(3) . . ? O6 Hg1 O2 118.2(5) . . ? O4 Hg1 O2 119.2(5) . . ? O5 Hg1 O2 166.5(4) . . ? O12 Hg1 O3 80.7(4) . . ? Hg2 Hg1 O3 97.5(3) . . ? O6 Hg1 O3 165.7(4) . . ? O4 Hg1 O3 60.9(5) . . ? O5 Hg1 O3 117.6(5) . . ? O2 Hg1 O3 58.9(5) . . ? O12 Hg1 O1 79.4(4) . . ? Hg2 Hg1 O1 96.1(3) . . ? O6 Hg1 O1 61.3(5) . . ? O4 Hg1 O1 164.8(4) . . ? O5 Hg1 O1 118.0(5) . . ? O2 Hg1 O1 57.7(4) . . ? O3 Hg1 O1 111.8(5) . . ? O8 Hg2 Hg1 154.5(9) . . ? O8 Hg2 O9 56.6(11) . . ? Hg1 Hg2 O9 127.0(8) . . ? Hg1 Hg2 O11A 125.8(6) . . ? O8 Hg2 O7 64.2(10) . . ? Hg1 Hg2 O7 115.2(5) . . ? O9 Hg2 O7 117.2(9) . . ? O11A Hg2 O7 56.0(9) . . ? Hg1 Hg2 O8A 129.8(6) . . ? O11A Hg2 O8A 98.7(9) . . ? O7 Hg2 O8A 68.7(8) . . ? O8 Hg2 O10 102.1(9) . . ? Hg1 Hg2 O10 99.1(3) . . ? O9 Hg2 O10 58.3(8) . . ? O11A Hg2 O10 65.9(7) . . ? O7 Hg2 O10 121.8(7) . . ? O8A Hg2 O10 121.6(7) . . ? O8 Hg2 O11 86.6(12) . . ? Hg1 Hg2 O11 117.4(9) . . ? O9 Hg2 O11 89.8(11) . . ? O7 Hg2 O11 67.0(10) . . ? O10 Hg2 O11 55.6(9) . . ? O36 Hg3 Hg4 175.8(5) . . ? O36 Hg3 O18 74.6(6) . . ? Hg4 Hg3 O18 108.6(4) . . ? O36 Hg3 O13 86.3(6) . . ? Hg4 Hg3 O13 97.7(3) . . ? O18 Hg3 O13 61.1(7) . . ? O36 Hg3 O15 86.8(5) . . ? Hg4 Hg3 O15 90.0(3) . . ? O18 Hg3 O15 161.4(5) . . ? O13 Hg3 O15 118.1(5) . . ? O36 Hg3 O17 84.6(6) . . ? Hg4 Hg3 O17 94.4(5) . . ? O18 Hg3 O17 61.7(8) . . ? O13 Hg3 O17 122.4(8) . . ? O15 Hg3 O17 118.0(7) . . ? O36 Hg3 O14 79.3(5) . . ? Hg4 Hg3 O14 101.4(3) . . ? O18 Hg3 O14 115.3(7) . . ? O13 Hg3 O14 59.0(5) . . ? O15 Hg3 O14 59.2(4) . . ? O17 Hg3 O14 163.8(5) . . ? O36 Hg3 O16 77.2(6) . . ? Hg4 Hg3 O16 98.8(4) . . ? O18 Hg3 O16 116.5(7) . . ? O13 Hg3 O16 163.1(5) . . ? O15 Hg3 O16 58.2(4) . . ? O17 Hg3 O16 60.0(7) . . ? O14 Hg3 O16 113.5(4) . . ? O19 Hg4 Hg3 153.0(3) . . ? O19 Hg4 O23 68.5(5) . . ? Hg3 Hg4 O23 111.2(4) . . ? O19 Hg4 O21 80.3(5) . . ? Hg3 Hg4 O21 121.0(3) . . ? O23 Hg4 O21 114.0(5) . . ? O19 Hg4 O22 87.2(5) . . ? Hg3 Hg4 O22 117.0(4) . . ? O23 Hg4 O22 61.2(5) . . ? O21 Hg4 O22 60.6(5) . . ? O19 Hg4 O20 67.6(4) . . ? Hg3 Hg4 O20 107.3(3) . . ? O23 Hg4 O20 136.1(5) . . ? O21 Hg4 O20 58.8(5) . . ? O22 Hg4 O20 117.0(5) . . ? O12 S1 C45 102.6(9) . . ? O12 S1 C46 103.1(9) . . ? C45 S1 C46 98.1(10) . . ? O28 S2 O27 116.4(17) . . ? O28 S2 O29 109.1(28) . . ? O27 S2 O29 113.3(21) . . ? O28 S2 C47 111.0(25) . . ? O27 S2 C47 103.2(21) . . ? O29 S2 C47 102.7(16) . . ? O26 S3 O25 134.7(13) . . ? O26 S3 C48 111.5(14) . . ? O25 S3 C48 109.7(14) . . ? O26 S3 O24 108.6(16) . . ? O25 S3 O24 103.4(15) . . ? C48 S3 O24 68.2(23) . . ? O32 S4 O31 115.2(12) . . ? O32 S4 O30 116.4(13) . . ? O31 S4 O30 115.1(11) . . ? O32 S4 C49 101.0(15) . . ? O31 S4 C49 103.3(16) . . ? O30 S4 C49 102.7(14) . . ? O34 S5 O33 116.6(15) . . ? O34 S5 O35 113.4(15) . . ? O33 S5 O35 113.2(13) . . ? O34 S5 C50 105.8(14) . . ? O33 S5 C50 104.6(15) . . ? O35 S5 C50 101.3(14) . . ? C1 O1 C12 111.3(20) . . ? C1 O1 Hg1 110.8(12) . . ? C12 O1 Hg1 103.3(12) . . ? C3 O2 C2 112.5(20) . . ? C3 O2 Hg1 115.8(13) . . ? C2 O2 Hg1 117.3(13) . . ? C5 O3 C4 113.8(23) . . ? C5 O3 Hg1 106.5(14) . . ? C4 O3 Hg1 109.3(13) . . ? C7 O4 C6 112.8(23) . . ? C7 O4 Hg1 117.9(15) . . ? C6 O4 Hg1 114.6(16) . . ? C8 O5 C9 114.3(22) . . ? C8 O5 Hg1 108.9(14) . . ? C9 O5 Hg1 108.9(12) . . ? C10 O6 C11 108.9(22) . . ? C10 O6 Hg1 117.4(14) . . ? C11 O6 Hg1 117.1(13) . . ? S1 O12 Hg1 117.8(7) . . ? C34 O13 C23 114.7(25) . . ? C34 O13 Hg3 112.1(20) . . ? C23 O13 Hg3 115.8(15) . . ? C24 O14 C25 110.3(18) . . ? C24 O14 Hg3 111.0(13) . . ? C25 O14 Hg3 108.4(11) . . ? C27 O15 C26 115.2(18) . . ? C27 O15 Hg3 120.6(12) . . ? C26 O15 Hg3 118.9(13) . . ? C29 O16 C28 113.5(27) . . ? C29 O16 Hg3 108.6(16) . . ? C28 O16 Hg3 106.9(13) . . ? C31 O17 C30 110.0(30) . . ? C31 O17 Hg3 115.1(24) . . ? C30 O17 Hg3 113.8(16) . . ? C33 O18 C32 113.5(28) . . ? C33 O18 Hg3 112.0(16) . . ? C32 O18 Hg3 110.7(20) . . ? C35 O19 C44 110.0(16) . . ? C35 O19 Hg4 120.3(11) . . ? C44 O19 Hg4 117.0(11) . . ? C37 O20 C36 114.0(19) . . ? C37 O20 Hg4 116.9(13) . . ? C36 O20 Hg4 101.3(11) . . ? C38 O21 C39 111.7(21) . . ? C38 O21 Hg4 103.4(12) . . ? C39 O21 Hg4 110.2(13) . . ? C41 O22 C40 117.3(22) . . ? C41 O22 Hg4 117.0(16) . . ? C40 O22 Hg4 117.6(14) . . ? C43 O23 C42 117.8(20) . . ? C43 O23 Hg4 106.6(13) . . ? C42 O23 Hg4 116.2(16) . . ? O1 C1 C2 109.3(20) . . ? O2 C2 C1 107.6(18) . . ? O2 C3 C4 109.5(19) . . ? O3 C4 C3 111.4(23) . . ? O3 C5 C6 109.5(24) . . ? O4 C6 C5 110.4(26) . . ? O4 C7 C8 107.2(20) . . ? O5 C8 C7 113.4(22) . . ? O5 C9 C10 109.5(21) . . ? O6 C10 C9 107.2(22) . . ? O6 C11 C12 110.6(19) . . ? O1 C12 C11 110.4(18) . . ? O13 C23 C24 110.6(24) . . ? O14 C24 C23 109.2(23) . . ? O14 C25 C26 111.0(20) . . ? O15 C26 C25 110.6(18) . . ? O15 C27 C28 107.9(19) . . ? O16 C28 C27 111.4(24) . . ? O16 C29 C30 109.8(32) . . ? C29 C30 O17 110.3(28) . . ? O17 C31 C32 105.8(29) . . ? O18 C32 C31 109.2(28) . . ? O18 C33 C34 107.3(26) . . ? O13 C34 C33 112.2(28) . . ? O19 C35 C36 106.2(19) . . ? O20 C36 C35 112.9(18) . . ? O20 C37 C38 107.6(19) . . ? O21 C38 C37 106.0(20) . . ? O21 C39 C40 108.1(22) . . ? O22 C40 C39 108.8(21) . . ? O22 C41 C42 114.1(23) . . ? O23 C42 C41 110.8(18) . . ? O23 C43 C44 115.0(19) . . ? O19 C44 C43 106.7(17) . . ? F1 C47 F2 136.9(85) . . ? F1 C47 F3 105.2(47) . . ? F2 C47 F3 98.3(35) . . ? F1 C47 S2 106.2(39) . . ? F2 C47 S2 103.3(29) . . ? F3 C47 S2 102.2(41) . . ? F5 C48 F6 116.4(22) . . ? F5 C48 F4 85.6(26) . . ? F6 C48 F4 85.6(22) . . ? F5 C48 S3 121.9(21) . . ? F6 C48 S3 121.4(21) . . ? F4 C48 S3 103.2(21) . . ? F8 C49 F7 111.9(26) . . ? F8 C49 F9 108.0(29) . . ? F7 C49 F9 107.4(32) . . ? F8 C49 S4 112.9(25) . . ? F7 C49 S4 109.5(24) . . ? F9 C49 S4 106.8(21) . . ? F10 C50 F12 104.0(25) . . ? F10 C50 F11 105.4(26) . . ? F12 C50 F11 101.0(26) . . ? F10 C50 S5 115.9(24) . . ? F12 C50 S5 114.1(21) . . ? F11 C50 S5 114.8(22) . . ? C13 O7 C22 131.3(56) . . ? C22A O7 C13A 97.9(27) . . ? C13 O7 Hg2 103.6(43) . . ? C22A O7 Hg2 129.2(22) . . ? C22 O7 Hg2 110.8(31) . . ? C13A O7 Hg2 102.4(15) . . ? C19 O10 C18 93.5(55) . . ? C18A O10 C19A 128.1(35) . . ? C19 O10 Hg2 114.7(24) . . ? C18 O10 Hg2 118.0(58) . . ? C18A O10 Hg2 110.9(27) . . ? C19A O10 Hg2 113.3(21) . . ? C14 O8 C15 115.6(42) . . ? C14 O8 Hg2 121.6(36) . . ? C15 O8 Hg2 121.9(28) . . ? C16 O9 C17 125.0(41) . . ? C16 O9 Hg2 111.8(23) . . ? C17 O9 Hg2 112.4(32) . . ? C20 O11 C21 113.1(69) . . ? C20 O11 Hg2 105.3(34) . . ? C21 O11 Hg2 104.3(35) . . ? O7 C13 C14 108.0(54) . . ? O8 C14 C13 95.8(43) . . ? C16 C15 O8 109.9(44) . . ? C15 C16 O9 96.7(45) . . ? C18 C17 O9 113.0(78) . . ? C17 C18 O10 106.4(91) . . ? C17 C18 C19 139.5(98) . . ? O10 C18 C19 42.1(40) . . ? O10 C19 C20 106.4(41) . . ? O10 C19 C18 44.4(39) . . ? C20 C19 C18 149.1(57) . . ? O11 C20 C19 104.5(62) . . ? O11 C21 C22 104.2(56) . . ? O7 C22 C21 118.7(45) . . ? C15A O8A C14A 111.9(34) . . ? C15A O8A Hg2 115.0(30) . . ? C14A O8A Hg2 121.2(23) . . ? C16A O9A C17A 103.5(60) . . ? C21A O11A C20A 103.5(31) . . ? C21A O11A Hg2 115.7(22) . . ? C20A O11A Hg2 106.1(20) . . ? C14A C13A O7 116.8(31) . . ? C13A C14A O8A 107.1(32) . . ? O8A C15A C16A 101.6(44) . . ? O9A C16A C15A 87.9(55) . . ? O9A C17A C18A 127.1(46) . . ? O10 C18A C17A 112.9(40) . . ? O10 C19A C20A 107.3(31) . . ? O11A C20A C19A 114.2(37) . . ? O11A C21A C22A 103.7(30) . . ? O7 C22A C21A 89.6(29) . . ? _refine_diff_density_max 1.548 _refine_diff_density_min -1.811 _refine_diff_density_rms 0.158 data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H72 F12 Hg4 O28 S8' _chemical_formula_weight 2239.78 _chemical_melting_point ? _chemical_compound_source ? 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' 'H' 'H' 0.0000 0.0000 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hg' 'Hg' -2.3894 9.2266 '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 9.547(5) _cell_length_b 11.836(2) _cell_length_c 15.548(2) _cell_angle_alpha 78.39(2) _cell_angle_beta 77.21(4) _cell_angle_gamma 83.79(2) _cell_volume 1674.5(9) _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 5.4 _cell_measurement_theta_max 12.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.221 _exptl_crystal_density_method ? _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 9.498 _exptl_absorpt_correction_type PSI-scan _exptl_absorpt_correction_T_min 0.515 _exptl_absorpt_correction_T_max 0.989 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker P4' _diffrn_measurement_method omega-scans _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5809 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 23.50 _reflns_number_total 4795 _reflns_number_observed 3457 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 402 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+1.2323P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4393 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_obs 0.0373 _refine_ls_wR_factor_all 0.0726 _refine_ls_wR_factor_obs 0.0607 _refine_ls_goodness_of_fit_all 1.021 _refine_ls_goodness_of_fit_obs 1.088 _refine_ls_restrained_S_all 1.086 _refine_ls_restrained_S_obs 1.088 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Hg1 Hg 0.04955(4) 0.73984(3) 0.73542(2) 0.02834(13) Uani 1 d . . Hg2 Hg 0.06327(5) 0.87878(3) 0.58820(2) 0.03175(14) Uani 1 d . . S1 S 0.1785(3) 0.5014(2) 0.8391(2) 0.0369(7) Uani 1 d . . S2 S 0.2458(3) 0.9212(2) 0.37010(15) 0.0274(6) Uani 1 d . . S3 S 0.2115(3) 1.1797(2) 0.5702(2) 0.0327(6) Uani 1 d . . S4 S 0.5091(3) 0.7875(3) 0.1593(2) 0.0533(9) Uani 1 d . . O1 O -0.2278(7) 0.6674(5) 0.7653(4) 0.039(2) Uani 1 d . . O2 O 0.0112(7) 0.5347(5) 0.6720(4) 0.034(2) Uani 1 d . . O3 O 0.2903(7) 0.6217(5) 0.6191(4) 0.032(2) Uani 1 d . . O4 O 0.3656(7) 0.7435(5) 0.7407(4) 0.032(2) Uani 1 d . . O5 O 0.1306(8) 0.8754(5) 0.8363(4) 0.035(2) Uani 1 d . . O6 O -0.1458(7) 0.8028(5) 0.8766(4) 0.037(2) Uani 1 d . . O7 O 0.0653(7) 0.6022(5) 0.8500(4) 0.037(2) Uani 1 d . . O8 O 0.1210(6) 0.9563(5) 0.4430(4) 0.0251(15) Uani 1 d . . O9 O 0.2518(7) 1.0576(5) 0.5710(4) 0.041(2) Uani 1 d . . O10 O 0.0977(8) 1.2260(6) 0.5236(4) 0.048(2) Uani 1 d . . O11 O 0.3300(7) 1.2517(6) 0.5531(5) 0.050(2) Uani 1 d . . O12 O 0.6304(8) 0.8057(7) 0.0870(5) 0.071(3) Uani 1 d . . O13 O 0.4604(8) 0.8866(6) 0.2012(5) 0.057(2) Uani 1 d . . O14 O 0.5093(10) 0.6757(6) 0.2172(5) 0.072(3) Uani 1 d . . F1 F 0.2237(8) 1.1424(5) 0.7413(4) 0.062(2) Uani 1 d . . F2 F 0.0767(7) 1.2837(5) 0.7029(4) 0.064(2) Uani 1 d . . F3 F 0.0218(7) 1.1096(5) 0.7157(4) 0.054(2) Uani 1 d . . F4 F 0.3925(10) 0.6904(6) 0.0576(5) 0.096(3) Uani 1 d . . F5 F 0.3504(10) 0.8750(7) 0.0421(5) 0.100(3) Uani 1 d . . F6 F 0.2401(9) 0.7640(8) 0.1584(6) 0.109(3) Uani 1 d . . C1 C -0.2907(11) 0.8066(9) 0.8621(7) 0.043(3) Uani 1 d . . H1A H -0.3027 0.8651 0.8094 0.052 Uiso 1 calc . . H1B H -0.3602 0.8266 0.9143 0.052 Uiso 1 calc . . C2 C -0.3149(11) 0.6899(9) 0.8479(7) 0.045(3) Uani 1 d . . H2A H -0.2909 0.6310 0.8975 0.054 Uiso 1 calc . . H2B H -0.4166 0.6860 0.8472 0.054 Uiso 1 calc . . C3 C -0.2318(11) 0.5515(8) 0.7543(7) 0.043(3) Uani 1 d . . H3A H -0.3308 0.5355 0.7552 0.052 Uiso 1 calc . . H3B H -0.1987 0.4980 0.8038 0.052 Uiso 1 calc . . C4 C -0.1361(14) 0.5343(9) 0.6663(8) 0.053(3) Uani 1 d . . H4A H -0.1533 0.4605 0.6523 0.064 Uiso 1 calc . . H4B H -0.1583 0.5963 0.6181 0.064 Uiso 1 calc . . C5 C 0.1034(13) 0.5260(8) 0.5876(7) 0.041(3) Uani 1 d . . H5A H 0.0866 0.5947 0.5430 0.049 Uiso 1 calc . . H5B H 0.0826 0.4580 0.5667 0.049 Uiso 1 calc . . C6 C 0.2562(12) 0.5157(7) 0.5976(6) 0.036(3) Uani 1 d . . H6A H 0.2710 0.4506 0.6456 0.043 Uiso 1 calc . . H6B H 0.3201 0.5012 0.5417 0.043 Uiso 1 calc . . C7 C 0.4320(11) 0.6158(8) 0.6341(6) 0.036(3) Uani 1 d . . H7A H 0.5018 0.6016 0.5802 0.044 Uiso 1 calc . . H7B H 0.4446 0.5522 0.6836 0.044 Uiso 1 calc . . C8 C 0.4559(10) 0.7281(8) 0.6569(6) 0.033(2) Uani 1 d . . H8A H 0.5570 0.7294 0.6602 0.039 Uiso 1 calc . . H8B H 0.4346 0.7918 0.6096 0.039 Uiso 1 calc . . C9 C 0.3729(12) 0.8559(8) 0.7573(7) 0.039(3) Uani 1 d . . H9A H 0.3424 0.9137 0.7091 0.046 Uiso 1 calc . . H9B H 0.4723 0.8682 0.7582 0.046 Uiso 1 calc . . C10 C 0.2775(14) 0.8697(8) 0.8452(7) 0.047(3) Uani 1 d . . H10A H 0.2960 0.8040 0.8918 0.057 Uiso 1 calc . . H10B H 0.2972 0.9406 0.8626 0.057 Uiso 1 calc . . C11 C 0.0321(15) 0.8970(9) 0.9145(7) 0.054(3) Uani 1 d . . H11A H 0.0528 0.9686 0.9303 0.065 Uiso 1 calc . . H11B H 0.0412 0.8335 0.9646 0.065 Uiso 1 calc . . C12 C -0.1149(14) 0.9073(9) 0.8980(7) 0.054(3) Uani 1 d . . H12A H -0.1839 0.9238 0.9516 0.065 Uiso 1 calc . . H12B H -0.1242 0.9714 0.8483 0.065 Uiso 1 calc . . C13 C 0.2896(14) 0.5096(9) 0.9147(8) 0.065(4) Uani 1 d . . H13A H 0.3643(50) 0.4472(40) 0.9126(37) 0.098 Uiso 1 calc R . H13B H 0.2319(20) 0.5029(63) 0.9751(10) 0.098 Uiso 1 calc R . H13C H 0.3334(63) 0.5832(29) 0.8978(30) 0.098 Uiso 1 calc R . C14 C 0.0879(13) 0.3773(8) 0.8988(8) 0.056(3) Uani 1 d . . H14A H 0.1528(26) 0.3089(10) 0.8938(41) 0.084 Uiso 1 calc R . H14B H 0.0050(45) 0.3713(34) 0.8738(31) 0.084 Uiso 1 calc R . H14C H 0.0562(68) 0.3836(29) 0.9615(11) 0.084 Uiso 1 calc R . C15 C 0.4024(10) 0.9450(9) 0.4023(7) 0.047(3) Uani 1 d . . H15A H 0.4071(36) 1.0271(10) 0.3995(42) 0.071 Uiso 1 calc R . H15B H 0.4856(11) 0.9168(50) 0.3621(26) 0.071 Uiso 1 calc R . H15C H 0.4015(33) 0.9043(45) 0.4631(16) 0.071 Uiso 1 calc R . C16 C 0.2590(12) 0.7688(7) 0.3921(7) 0.046(3) Uani 1 d . . H16A H 0.3352(49) 0.7408(7) 0.3472(27) 0.069 Uiso 1 calc R . H16B H 0.1684(26) 0.7405(7) 0.3900(44) 0.069 Uiso 1 calc R . H16C H 0.2807(70) 0.7412(7) 0.4511(20) 0.069 Uiso 1 calc R . C17 C 0.3682(17) 0.7744(13) 0.1050(9) 0.075(4) Uani 1 d . . C18 C 0.1312(12) 1.1793(8) 0.6879(7) 0.036(3) Uani 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 Hg1 0.0361(3) 0.0265(2) 0.0194(2) 0.0028(2) -0.0065(2) -0.0002(2) Hg2 0.0414(3) 0.0284(2) 0.0204(2) 0.0043(2) -0.0055(2) 0.0016(2) S1 0.046(2) 0.0330(14) 0.0238(14) 0.0003(11) -0.0023(13) 0.0115(13) S2 0.0301(15) 0.0263(12) 0.0213(13) -0.0002(10) -0.0010(12) 0.0011(11) S3 0.033(2) 0.0306(14) 0.035(2) -0.0070(11) -0.0046(13) -0.0065(12) S4 0.059(2) 0.063(2) 0.033(2) -0.0125(14) -0.006(2) 0.021(2) O1 0.035(4) 0.041(4) 0.033(4) 0.005(3) 0.002(4) -0.008(3) O2 0.039(5) 0.034(4) 0.031(4) -0.003(3) -0.014(4) -0.002(3) O3 0.028(4) 0.028(4) 0.037(4) -0.007(3) -0.001(3) 0.001(3) O4 0.026(4) 0.038(4) 0.028(4) -0.001(3) -0.001(3) -0.004(3) O5 0.049(5) 0.041(4) 0.019(4) -0.012(3) -0.006(4) -0.005(3) O6 0.041(5) 0.042(4) 0.023(4) -0.005(3) 0.001(3) -0.001(3) O7 0.046(5) 0.030(4) 0.026(4) 0.003(3) -0.004(4) 0.010(3) O8 0.025(4) 0.031(3) 0.016(3) -0.002(3) -0.002(3) 0.002(3) O9 0.050(5) 0.032(4) 0.046(4) -0.020(3) -0.010(4) 0.003(3) O10 0.053(5) 0.048(4) 0.039(4) 0.015(3) -0.018(4) -0.004(4) O11 0.038(5) 0.052(5) 0.058(5) -0.015(4) 0.000(4) -0.010(4) O12 0.047(5) 0.116(7) 0.037(5) -0.022(5) 0.016(4) 0.020(5) O13 0.063(6) 0.054(5) 0.052(5) -0.028(4) 0.007(4) 0.003(4) O14 0.101(7) 0.057(5) 0.043(5) 0.010(4) -0.017(5) 0.028(5) F1 0.079(5) 0.068(4) 0.049(4) -0.012(3) -0.032(4) -0.006(4) F2 0.094(5) 0.035(3) 0.050(4) -0.011(3) 0.010(4) 0.003(3) F3 0.059(4) 0.055(4) 0.038(4) 0.009(3) 0.001(3) -0.017(3) F4 0.130(8) 0.077(5) 0.098(6) -0.037(5) -0.052(6) 0.013(5) F5 0.137(8) 0.097(6) 0.073(5) -0.020(5) -0.063(5) 0.056(5) F6 0.058(6) 0.153(8) 0.124(8) -0.061(7) -0.006(6) -0.002(6) C1 0.030(7) 0.051(7) 0.036(7) 0.004(5) 0.006(5) 0.007(5) C2 0.027(7) 0.054(7) 0.042(7) 0.008(5) -0.002(6) -0.001(5) C3 0.037(7) 0.041(6) 0.052(7) 0.011(5) -0.019(6) -0.010(5) C4 0.079(10) 0.037(6) 0.050(8) -0.008(5) -0.027(7) -0.003(6) C5 0.071(9) 0.028(5) 0.024(6) -0.001(4) -0.013(6) -0.008(6) C6 0.052(8) 0.025(5) 0.032(6) -0.014(4) -0.009(6) 0.004(5) C7 0.033(7) 0.036(6) 0.028(6) 0.003(4) 0.007(5) 0.005(5) C8 0.018(6) 0.033(6) 0.042(6) -0.002(5) 0.002(5) -0.003(4) C9 0.053(8) 0.031(6) 0.038(6) -0.001(5) -0.024(6) -0.011(5) C10 0.073(9) 0.039(6) 0.043(7) -0.012(5) -0.032(7) -0.011(6) C11 0.088(11) 0.046(7) 0.027(6) -0.013(5) 0.006(7) -0.027(7) C12 0.059(9) 0.046(7) 0.047(8) -0.019(6) 0.026(7) -0.008(6) C13 0.075(10) 0.059(8) 0.062(9) -0.004(6) -0.030(8) 0.011(7) C14 0.065(9) 0.029(6) 0.065(8) 0.004(5) -0.009(7) 0.002(6) C15 0.027(7) 0.053(7) 0.057(8) -0.012(6) 0.003(6) -0.001(5) C16 0.049(7) 0.033(6) 0.048(7) -0.013(5) 0.009(6) 0.002(5) C17 0.081(12) 0.107(12) 0.050(9) -0.046(9) -0.017(9) 0.001(9) C18 0.042(7) 0.025(5) 0.045(7) -0.005(5) -0.011(6) -0.011(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 Hg1 O7 2.179(6) . ? Hg1 Hg2 2.5218(7) . ? Hg1 O6 2.719(6) . ? Hg1 O5 2.730(6) . ? Hg1 O1 2.784(7) . ? Hg1 O2 2.884(6) . ? Hg1 O3 2.998(6) . ? Hg1 O4 3.042(6) . ? Hg2 O8 2.229(5) . ? Hg2 O8 2.529(6) 2_576 ? Hg2 O9 2.859(7) . ? Hg2 O10 3.063(7) 2_576 ? Hg2 Hg2 3.8426(13) 2_576 ? S1 O7 1.530(6) . ? S1 C13 1.771(11) . ? S1 C14 1.772(10) . ? S2 O8 1.536(6) . ? S2 C15 1.745(10) . ? S2 C16 1.763(9) . ? S3 O11 1.435(7) . ? S3 O10 1.438(7) . ? S3 O9 1.453(6) . ? S3 C18 1.820(10) . ? S4 O12 1.425(8) . ? S4 O13 1.440(7) . ? S4 O14 1.444(7) . ? S4 C17 1.774(14) . ? O1 C3 1.421(11) . ? O1 C2 1.425(11) . ? O2 C5 1.426(11) . ? O2 C4 1.430(13) . ? O3 C7 1.416(12) . ? O3 C6 1.447(10) . ? O4 C9 1.416(10) . ? O4 C8 1.427(10) . ? O5 C11 1.412(12) . ? O5 C10 1.433(13) . ? O6 C12 1.420(12) . ? O6 C1 1.445(12) . ? O8 Hg2 2.529(6) 2_576 ? F1 C18 1.325(11) . ? F2 C18 1.333(10) . ? F3 C18 1.342(11) . ? F4 C17 1.324(13) . ? F5 C17 1.40(2) . ? F6 C17 1.321(15) . ? C1 C2 1.491(14) . ? C3 C4 1.506(15) . ? C5 C6 1.492(15) . ? C7 C8 1.495(13) . ? C9 C10 1.493(14) . ? C11 C12 1.47(2) . ? 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 O7 Hg1 Hg2 170.4(2) . . ? O7 Hg1 O6 73.9(2) . . ? Hg2 Hg1 O6 115.67(13) . . ? O7 Hg1 O5 84.2(2) . . ? Hg2 Hg1 O5 100.51(13) . . ? O6 Hg1 O5 60.9(2) . . ? O7 Hg1 O1 82.5(2) . . ? Hg2 Hg1 O1 101.50(13) . . ? O6 Hg1 O1 62.6(2) . . ? O5 Hg1 O1 123.5(2) . . ? O7 Hg1 O2 76.7(2) . . ? Hg2 Hg1 O2 97.39(12) . . ? O6 Hg1 O2 119.2(2) . . ? O5 Hg1 O2 159.5(2) . . ? O1 Hg1 O2 61.7(2) . . ? O7 Hg1 O3 90.8(2) . . ? Hg2 Hg1 O3 79.64(12) . . ? O6 Hg1 O3 164.5(2) . . ? O5 Hg1 O3 115.8(2) . . ? O1 Hg1 O3 119.1(2) . . ? O2 Hg1 O3 57.9(2) . . ? O7 Hg1 O4 79.8(2) . . ? Hg2 Hg1 O4 95.26(12) . . ? O6 Hg1 O4 116.7(2) . . ? O5 Hg1 O4 59.9(2) . . ? O1 Hg1 O4 161.5(2) . . ? O2 Hg1 O4 108.6(2) . . ? O3 Hg1 O4 56.2(2) . . ? O8 Hg2 Hg1 161.97(14) . . ? O8 Hg2 O8 72.4(2) . 2_576 ? Hg1 Hg2 O8 124.60(13) . 2_576 ? O8 Hg2 O9 72.7(2) . . ? Hg1 Hg2 O9 111.97(14) . . ? O8 Hg2 O9 84.7(2) 2_576 . ? O8 Hg2 O10 68.4(2) . 2_576 ? Hg1 Hg2 O10 106.31(12) . 2_576 ? O8 Hg2 O10 80.2(2) 2_576 2_576 ? O9 Hg2 O10 140.9(2) . 2_576 ? O8 Hg2 Hg2 38.87(14) . 2_576 ? Hg1 Hg2 Hg2 157.73(3) . 2_576 ? O8 Hg2 Hg2 33.58(12) 2_576 2_576 ? O9 Hg2 Hg2 76.46(13) . 2_576 ? O10 Hg2 Hg2 71.03(12) 2_576 2_576 ? O7 S1 C13 104.1(5) . . ? O7 S1 C14 104.6(5) . . ? C13 S1 C14 98.9(6) . . ? O8 S2 C15 105.5(4) . . ? O8 S2 C16 105.3(4) . . ? C15 S2 C16 98.8(5) . . ? O11 S3 O10 115.0(4) . . ? O11 S3 O9 115.0(4) . . ? O10 S3 O9 114.9(4) . . ? O11 S3 C18 103.5(4) . . ? O10 S3 C18 104.5(5) . . ? O9 S3 C18 101.4(4) . . ? O12 S4 O13 114.1(5) . . ? O12 S4 O14 115.7(5) . . ? O13 S4 O14 117.3(5) . . ? O12 S4 C17 103.2(6) . . ? O13 S4 C17 103.5(6) . . ? O14 S4 C17 99.8(7) . . ? C3 O1 C2 112.5(8) . . ? C3 O1 Hg1 113.7(6) . . ? C2 O1 Hg1 112.7(6) . . ? C5 O2 C4 110.4(8) . . ? C5 O2 Hg1 112.5(5) . . ? C4 O2 Hg1 109.0(5) . . ? C7 O3 C6 112.4(7) . . ? C7 O3 Hg1 119.6(5) . . ? C6 O3 Hg1 115.4(5) . . ? C9 O4 C8 111.0(7) . . ? C9 O4 Hg1 102.3(5) . . ? C8 O4 Hg1 111.0(5) . . ? C11 O5 C10 112.8(8) . . ? C11 O5 Hg1 117.8(6) . . ? C10 O5 Hg1 120.2(5) . . ? C12 O6 C1 112.4(8) . . ? C12 O6 Hg1 112.5(5) . . ? C1 O6 Hg1 111.0(5) . . ? S1 O7 Hg1 119.5(4) . . ? S2 O8 Hg2 129.4(3) . . ? S2 O8 Hg2 123.0(3) . 2_576 ? Hg2 O8 Hg2 107.6(2) . 2_576 ? S3 O9 Hg2 127.0(4) . . ? O6 C1 C2 107.6(8) . . ? O1 C2 C1 110.3(8) . . ? O1 C3 C4 109.2(8) . . ? O2 C4 C3 109.5(9) . . ? O2 C5 C6 109.1(8) . . ? O3 C6 C5 109.4(7) . . ? O3 C7 C8 108.3(7) . . ? O4 C8 C7 110.5(7) . . ? O4 C9 C10 109.9(8) . . ? O5 C10 C9 108.7(8) . . ? O5 C11 C12 109.2(9) . . ? O6 C12 C11 109.8(9) . . ? F6 C17 F4 108.3(13) . . ? F6 C17 F5 104.0(12) . . ? F4 C17 F5 104.3(10) . . ? F6 C17 S4 114.7(9) . . ? F4 C17 S4 114.5(11) . . ? F5 C17 S4 110.0(10) . . ? F1 C18 F2 107.3(8) . . ? F1 C18 F3 106.9(8) . . ? F2 C18 F3 106.3(8) . . ? F1 C18 S3 112.9(7) . . ? F2 C18 S3 112.3(7) . . ? F3 C18 S3 110.7(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 C1 C2 O1 -67.9(10) . . . . ? O1 C3 C4 O2 71.1(10) . . . . ? O2 C5 C6 O3 -65.6(9) . . . . ? O3 C7 C8 O4 66.2(9) . . . . ? O4 C9 C10 O5 -71.3(10) . . . . ? O5 C11 C12 C6 28.9(6) . . . . ? _refine_diff_density_max 0.767 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.149