# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_12 _database_code_depnum_ccdc_archive 'CCDC 848952' #TrackingRef '12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C63 H84 O9 Se6, 2(C H Cl3)' _chemical_formula_sum 'C65 H86 Cl6 O9 Se6' _chemical_formula_weight 1697.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.9433(4) _cell_length_b 16.7585(4) _cell_length_c 17.4804(4) _cell_angle_alpha 109.7050(10) _cell_angle_beta 98.3310(10) _cell_angle_gamma 112.9910(10) _cell_volume 3595.47(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1708 _exptl_absorpt_coefficient_mu 6.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.344 _exptl_absorpt_correction_T_max 0.545 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'crossed G\"obel mirrors' _diffrn_measurement_device_type 'SMART 6000' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70888 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 70.78 _reflns_number_total 13363 _reflns_number_gt 10164 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0590P)^2^+1.5783P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13363 _refine_ls_number_parameters 824 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1188 _refine_ls_wR_factor_gt 0.1095 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se1 Se 0.95103(4) 1.30945(4) 0.36357(3) 0.02146(12) Uani 1 1 d . . . C2 C 1.0463(4) 1.3061(3) 0.2973(3) 0.0201(10) Uani 1 1 d . . . H2A H 1.0353 1.3310 0.2548 0.024 Uiso 1 1 calc R . . H2B H 1.1177 1.3486 0.3364 0.024 Uiso 1 1 calc R . . C3 C 1.0318(3) 1.2066(3) 0.2517(3) 0.0188(9) Uani 1 1 d . . . C4 C 0.9772(3) 1.1509(3) 0.1643(3) 0.0195(9) Uani 1 1 d . . . C5 C 0.9569(3) 1.0556(3) 0.1213(3) 0.0203(10) Uani 1 1 d . . . C6 C 0.9931(4) 1.0155(3) 0.1692(3) 0.0207(10) Uani 1 1 d . . . C7 C 1.0474(4) 1.0688(3) 0.2577(3) 0.0226(10) Uani 1 1 d . . . C8 C 1.0674(4) 1.1639(3) 0.2960(3) 0.0201(10) Uani 1 1 d . . . O9 O 0.9373(2) 1.1889(2) 0.1176(2) 0.0216(7) Uani 1 1 d . . . C10 C 1.0083(4) 1.2402(4) 0.0829(3) 0.0312(12) Uani 1 1 d . . . H10A H 1.0710 1.2919 0.1295 0.047 Uiso 1 1 calc R . . H10B H 0.9773 1.2679 0.0532 0.047 Uiso 1 1 calc R . . H10C H 1.0253 1.1960 0.0423 0.047 Uiso 1 1 calc R . . O11 O 0.9789(3) 0.9240(2) 0.1288(2) 0.0274(8) Uani 1 1 d . . . C12 C 0.8875(5) 0.8502(4) 0.1293(4) 0.0421(15) Uani 1 1 d . . . H12A H 0.8618 0.8796 0.1733 0.063 Uiso 1 1 calc R . . H12B H 0.9039 0.8039 0.1421 0.063 Uiso 1 1 calc R . . H12C H 0.8350 0.8170 0.0730 0.063 Uiso 1 1 calc R . . O13 O 1.1209(3) 1.2189(2) 0.3832(2) 0.0256(7) Uani 1 1 d . . . C14 C 1.2301(4) 1.2607(4) 0.4011(3) 0.0276(11) Uani 1 1 d . . . H14A H 1.2492 1.2094 0.3806 0.041 Uiso 1 1 calc R . . H14B H 1.2642 1.2988 0.4631 0.041 Uiso 1 1 calc R . . H14C H 1.2514 1.3022 0.3719 0.041 Uiso 1 1 calc R . . C15 C 0.8940(4) 0.9962(4) 0.0280(3) 0.0231(10) Uani 1 1 d . . . H15A H 0.9084 0.9418 0.0030 0.028 Uiso 1 1 calc R . . H15B H 0.9117 1.0361 -0.0038 0.028 Uiso 1 1 calc R . . Se16 Se 0.74798(4) 0.94758(3) 0.01875(3) 0.02028(12) Uani 1 1 d . . . C17 C 0.6946(4) 0.8677(3) -0.1073(3) 0.0227(10) Uani 1 1 d . . . H17A H 0.6504 0.8881 -0.1347 0.027 Uiso 1 1 calc R . . H17B H 0.7526 0.8771 -0.1306 0.027 Uiso 1 1 calc R . . C18 C 0.6344(4) 0.7642(3) -0.1273(3) 0.0182(9) Uani 1 1 d . . . C19 C 0.6705(3) 0.6987(3) -0.1595(3) 0.0187(9) Uani 1 1 d . . . H19 H 0.7345 0.7205 -0.1698 0.022 Uiso 1 1 calc R . . C20 C 0.6152(3) 0.6020(3) -0.1772(3) 0.0169(9) Uani 1 1 d . . . C21 C 0.5241(4) 0.5731(3) -0.1576(3) 0.0183(9) Uani 1 1 d . . . H21 H 0.4862 0.5080 -0.1674 0.022 Uiso 1 1 calc R . . C22 C 0.4867(4) 0.6377(3) -0.1235(3) 0.0176(9) Uani 1 1 d . . . C23 C 0.5423(3) 0.7321(3) -0.1101(3) 0.0175(9) Uani 1 1 d . . . C24 C 0.6564(4) 0.5312(3) -0.2131(3) 0.0198(10) Uani 1 1 d . . . C25 C 0.7070(4) 0.5540(4) -0.2788(3) 0.0275(11) Uani 1 1 d . . . H25A H 0.6564 0.5486 -0.3253 0.041 Uiso 1 1 calc R . . H25B H 0.7326 0.5084 -0.3022 0.041 Uiso 1 1 calc R . . H25C H 0.7643 0.6196 -0.2507 0.041 Uiso 1 1 calc R . . C26 C 0.5701(4) 0.4271(3) -0.2581(4) 0.0308(12) Uani 1 1 d . . . H26A H 0.5374 0.4107 -0.2170 0.046 Uiso 1 1 calc R . . H26B H 0.5986 0.3838 -0.2808 0.046 Uiso 1 1 calc R . . H26C H 0.5190 0.4201 -0.3054 0.046 Uiso 1 1 calc R . . C27 C 0.7341(4) 0.5413(4) -0.1390(3) 0.0302(12) Uani 1 1 d . . . H27A H 0.7852 0.6091 -0.1056 0.045 Uiso 1 1 calc R . . H27B H 0.7684 0.5035 -0.1616 0.045 Uiso 1 1 calc R . . H27C H 0.6988 0.5177 -0.1020 0.045 Uiso 1 1 calc R . . O28 O 0.5086(3) 0.7984(2) -0.07463(19) 0.0209(7) Uani 1 1 d . . . C29 C 0.4414(4) 0.8030(4) -0.1386(3) 0.0266(11) Uani 1 1 d . . . H29A H 0.4735 0.8119 -0.1822 0.040 Uiso 1 1 calc R . . H29B H 0.4282 0.8571 -0.1117 0.040 Uiso 1 1 calc R . . H29C H 0.3764 0.7430 -0.1657 0.040 Uiso 1 1 calc R . . C30 C 0.3887(4) 0.6037(3) -0.1020(3) 0.0211(10) Uani 1 1 d . . . H30A H 0.3401 0.5373 -0.1452 0.025 Uiso 1 1 calc R . . H30B H 0.3571 0.6452 -0.1046 0.025 Uiso 1 1 calc R . . Se31 Se 0.41266(4) 0.60677(4) 0.01286(3) 0.02640(13) Uani 1 1 d . . . C32 C 0.5167(4) 0.7435(3) 0.0779(3) 0.0216(10) Uani 1 1 d . . . H32A H 0.5780 0.7547 0.0589 0.026 Uiso 1 1 calc R . . H32B H 0.4886 0.7842 0.0661 0.026 Uiso 1 1 calc R . . C33 C 0.5472(4) 0.7712(3) 0.1724(3) 0.0190(10) Uani 1 1 d . . . C34 C 0.4903(3) 0.8023(3) 0.2210(3) 0.0154(9) Uani 1 1 d . . . C35 C 0.5214(3) 0.8386(3) 0.3102(3) 0.0158(9) Uani 1 1 d . . . C36 C 0.6082(4) 0.8383(3) 0.3503(3) 0.0178(9) Uani 1 1 d . . . C37 C 0.6679(3) 0.8071(3) 0.3053(3) 0.0174(9) Uani 1 1 d . . . C38 C 0.6350(4) 0.7746(3) 0.2155(3) 0.0185(9) Uani 1 1 d . . . O39 O 0.4066(3) 0.8048(2) 0.1800(2) 0.0210(7) Uani 1 1 d . . . C40 C 0.3096(4) 0.7271(4) 0.1659(3) 0.0241(10) Uani 1 1 d . . . H40A H 0.2980 0.6681 0.1189 0.036 Uiso 1 1 calc R . . H40B H 0.2545 0.7426 0.1511 0.036 Uiso 1 1 calc R . . H40C H 0.3099 0.7176 0.2183 0.036 Uiso 1 1 calc R . . O41 O 0.6426(3) 0.8764(2) 0.43894(19) 0.0214(7) Uani 1 1 d . . . C42 C 0.5944(4) 0.8092(3) 0.4721(3) 0.0216(10) Uani 1 1 d . . . H42A H 0.5198 0.7815 0.4495 0.032 Uiso 1 1 calc R . . H42B H 0.6169 0.8422 0.5348 0.032 Uiso 1 1 calc R . . H42C H 0.6137 0.7578 0.4546 0.032 Uiso 1 1 calc R . . O43 O 0.6992(3) 0.7543(2) 0.1722(2) 0.0272(8) Uani 1 1 d . . . C44 C 0.6692(4) 0.6550(4) 0.1214(3) 0.0319(12) Uani 1 1 d . . . H44A H 0.6921 0.6287 0.1578 0.048 Uiso 1 1 calc R . . H44B H 0.7006 0.6498 0.0757 0.048 Uiso 1 1 calc R . . H44C H 0.5944 0.6188 0.0960 0.048 Uiso 1 1 calc R . . C45 C 0.4682(4) 0.8847(3) 0.3620(3) 0.0184(9) Uani 1 1 d . . . H45A H 0.4625 0.8657 0.4097 0.022 Uiso 1 1 calc R . . H45B H 0.3979 0.8609 0.3252 0.022 Uiso 1 1 calc R . . Se46 Se 0.54268(4) 1.02584(3) 0.40911(3) 0.02261(12) Uani 1 1 d . . . C47 C 0.5075(4) 1.0386(3) 0.3024(3) 0.0221(10) Uani 1 1 d . . . H47A H 0.5101 0.9883 0.2542 0.027 Uiso 1 1 calc R . . H47B H 0.4372 1.0312 0.2887 0.027 Uiso 1 1 calc R . . C48 C 0.5833(4) 1.1361(3) 0.3150(3) 0.0195(9) Uani 1 1 d . . . C49 C 0.5720(4) 1.2168(3) 0.3595(3) 0.0195(10) Uani 1 1 d . . . H49 H 0.5154 1.2082 0.3805 0.023 Uiso 1 1 calc R . . C50 C 0.6410(4) 1.3088(3) 0.3738(3) 0.0179(9) Uani 1 1 d . . . C51 C 0.7241(4) 1.3196(3) 0.3439(3) 0.0198(10) Uani 1 1 d . . . H51 H 0.7734 1.3823 0.3550 0.024 Uiso 1 1 calc R . . C52 C 0.7377(4) 1.2411(3) 0.2981(3) 0.0192(9) Uani 1 1 d . . . C53 C 0.6662(4) 1.1495(3) 0.2836(3) 0.0199(10) Uani 1 1 d . . . C54 C 0.6268(4) 1.3971(3) 0.4193(3) 0.0235(10) Uani 1 1 d . . . C55 C 0.5398(6) 1.3750(5) 0.4570(5) 0.0517(18) Uani 1 1 d . . . H55A H 0.5363 1.4342 0.4872 0.078 Uiso 1 1 calc R . . H55B H 0.5519 1.3485 0.4972 0.078 Uiso 1 1 calc R . . H55C H 0.4749 1.3280 0.4108 0.078 Uiso 1 1 calc R . . C56 C 0.6061(5) 1.4359(4) 0.3550(4) 0.0408(15) Uani 1 1 d . . . H56A H 0.5410 1.3878 0.3094 0.061 Uiso 1 1 calc R . . H56B H 0.6618 1.4498 0.3301 0.061 Uiso 1 1 calc R . . H56C H 0.6020 1.4949 0.3843 0.061 Uiso 1 1 calc R . . C57 C 0.7260(5) 1.4772(4) 0.4930(4) 0.0434(15) Uani 1 1 d . . . H57A H 0.7825 1.4968 0.4696 0.065 Uiso 1 1 calc R . . H57B H 0.7428 1.4531 0.5339 0.065 Uiso 1 1 calc R . . H57C H 0.7157 1.5326 0.5223 0.065 Uiso 1 1 calc R . . O58 O 0.6716(3) 1.0697(2) 0.2305(2) 0.0249(7) Uani 1 1 d . . . C59 C 0.7329(4) 1.0392(4) 0.2709(3) 0.0265(11) Uani 1 1 d . . . H59A H 0.8032 1.0920 0.3000 0.040 Uiso 1 1 calc R . . H59B H 0.7333 0.9840 0.2276 0.040 Uiso 1 1 calc R . . H59C H 0.7045 1.0205 0.3129 0.040 Uiso 1 1 calc R . . C60 C 0.8278(4) 1.2565(4) 0.2659(3) 0.0257(11) Uani 1 1 d . . . H60A H 0.8368 1.3018 0.2395 0.031 Uiso 1 1 calc R . . H60B H 0.8165 1.1948 0.2219 0.031 Uiso 1 1 calc R . . C61 C 1.0773(4) 1.0226(4) 0.3103(3) 0.0267(11) Uani 1 1 d . . . H61A H 1.0185 0.9591 0.2944 0.032 Uiso 1 1 calc R . . H61B H 1.0927 1.0630 0.3717 0.032 Uiso 1 1 calc R . . Se62 Se 1.19727(4) 1.00547(4) 0.29414(3) 0.02190(12) Uani 1 1 d . . . C63 C 1.1966(4) 0.9406(3) 0.3697(3) 0.0230(10) Uani 1 1 d . . . H63A H 1.2569 0.9291 0.3746 0.028 Uiso 1 1 calc R . . H63B H 1.2030 0.9834 0.4278 0.028 Uiso 1 1 calc R . . C64 C 1.1001(4) 0.8456(3) 0.3373(3) 0.0196(10) Uani 1 1 d . . . C65 C 1.0793(4) 0.7705(3) 0.2598(3) 0.0193(9) Uani 1 1 d . . . H65 H 1.1259 0.7804 0.2281 0.023 Uiso 1 1 calc R . . C66 C 0.9929(4) 0.6817(3) 0.2274(3) 0.0186(9) Uani 1 1 d . A . C67 C 0.9284(4) 0.6683(3) 0.2771(3) 0.0203(10) Uani 1 1 d . . . H67 H 0.8701 0.6072 0.2571 0.024 Uiso 1 1 calc R . . C68 C 0.9462(4) 0.7414(4) 0.3554(3) 0.0204(10) Uani 1 1 d . . . C69 C 1.0318(4) 0.8312(3) 0.3839(3) 0.0202(10) Uani 1 1 d . . . C70 C 0.9697(4) 0.6001(3) 0.1405(3) 0.0241(10) Uani 1 1 d . . . C71 C 0.9893(9) 0.6448(7) 0.0736(6) 0.038(3) Uani 0.570(9) 1 d P A 1 H71A H 0.9705 0.5933 0.0168 0.057 Uiso 0.570(9) 1 calc PR A 1 H71B H 1.0620 0.6913 0.0919 0.057 Uiso 0.570(9) 1 calc PR A 1 H71C H 0.9475 0.6771 0.0709 0.057 Uiso 0.570(9) 1 calc PR A 1 C72 C 0.8633(8) 0.5222(7) 0.1049(7) 0.040(3) Uani 0.570(9) 1 d P A 1 H72A H 0.8520 0.4768 0.0471 0.059 Uiso 0.570(9) 1 calc PR A 1 H72B H 0.8161 0.5493 0.1023 0.059 Uiso 0.570(9) 1 calc PR A 1 H72C H 0.8510 0.4886 0.1417 0.059 Uiso 0.570(9) 1 calc PR A 1 C73 C 1.0483(8) 0.5628(7) 0.1516(6) 0.032(2) Uani 0.570(9) 1 d P A 1 H73A H 1.0375 0.5333 0.1915 0.048 Uiso 0.570(9) 1 calc PR A 1 H73B H 1.1180 0.6167 0.1745 0.048 Uiso 0.570(9) 1 calc PR A 1 H73C H 1.0393 0.5150 0.0959 0.048 Uiso 0.570(9) 1 calc PR A 1 C91 C 0.8765(10) 0.5836(11) 0.0765(8) 0.040(4) Uani 0.430(9) 1 d P A 2 H91A H 0.8934 0.6400 0.0647 0.060 Uiso 0.430(9) 1 calc PR A 2 H91B H 0.8197 0.5732 0.1003 0.060 Uiso 0.430(9) 1 calc PR A 2 H91C H 0.8563 0.5269 0.0231 0.060 Uiso 0.430(9) 1 calc PR A 2 C92 C 0.9339(12) 0.5009(9) 0.1493(9) 0.043(4) Uani 0.430(9) 1 d P A 2 H92A H 0.9197 0.4491 0.0942 0.065 Uiso 0.430(9) 1 calc PR A 2 H92B H 0.8717 0.4860 0.1661 0.065 Uiso 0.430(9) 1 calc PR A 2 H92C H 0.9885 0.5071 0.1930 0.065 Uiso 0.430(9) 1 calc PR A 2 C93 C 1.0574(8) 0.6148(8) 0.1073(7) 0.024(3) Uani 0.430(9) 1 d P A 2 H93A H 1.0366 0.5600 0.0522 0.036 Uiso 0.430(9) 1 calc PR A 2 H93B H 1.1142 0.6202 0.1483 0.036 Uiso 0.430(9) 1 calc PR A 2 H93C H 1.0797 0.6739 0.0993 0.036 Uiso 0.430(9) 1 calc PR A 2 O74 O 1.0451(3) 0.9077(2) 0.4565(2) 0.0265(8) Uani 1 1 d . . . C75 C 1.1031(4) 0.9185(4) 0.5354(3) 0.0305(12) Uani 1 1 d . . . H75A H 1.0741 0.8572 0.5396 0.046 Uiso 1 1 calc R . . H75B H 1.1005 0.9678 0.5836 0.046 Uiso 1 1 calc R . . H75C H 1.1746 0.9379 0.5370 0.046 Uiso 1 1 calc R . . C76 C 0.8757(4) 0.7215(4) 0.4079(3) 0.0259(11) Uani 1 1 d . . . H76A H 0.9026 0.7795 0.4627 0.031 Uiso 1 1 calc R . . H76B H 0.8760 0.6689 0.4216 0.031 Uiso 1 1 calc R . . Se77 Se 0.73355(4) 0.68550(3) 0.34953(3) 0.02080(12) Uani 1 1 d . . . C78 C 0.7632(4) 0.8106(3) 0.3498(3) 0.0216(10) Uani 1 1 d . . . H78A H 0.7922 0.8608 0.4096 0.026 Uiso 1 1 calc R . . H78B H 0.8148 0.8276 0.3204 0.026 Uiso 1 1 calc R . . C79 C 0.7202(4) 0.1335(3) 0.9808(3) 0.0257(11) Uani 1 1 d . . . H79 H 0.7452 0.1148 1.0247 0.031 Uiso 1 1 calc R . . Cl80 Cl 0.75889(11) 0.25811(9) 1.03083(8) 0.0328(3) Uani 1 1 d . . . Cl81 Cl 0.58597(11) 0.06554(10) 0.93867(9) 0.0345(3) Uani 1 1 d . . . Cl82 Cl 0.77559(10) 0.10872(9) 0.89866(8) 0.0303(3) Uani 1 1 d . . . C83 C 0.1454(4) 0.6666(3) 0.3931(3) 0.0255(11) Uani 1 1 d . . . H83 H 0.1032 0.6856 0.3605 0.031 Uiso 1 1 calc R . . Cl84 Cl 0.2400(2) 0.65963(16) 0.34663(16) 0.0828(8) Uani 1 1 d . . . Cl85 Cl 0.06476(12) 0.55392(11) 0.38806(11) 0.0507(4) Uani 1 1 d . . . Cl86 Cl 0.20344(15) 0.75331(12) 0.49784(9) 0.0531(4) 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 0.0202(3) 0.0229(3) 0.0196(2) 0.0072(2) 0.0062(2) 0.0104(2) C2 0.016(2) 0.021(2) 0.025(2) 0.012(2) 0.0104(19) 0.0067(19) C3 0.014(2) 0.017(2) 0.022(2) 0.0060(19) 0.0085(19) 0.0056(18) C4 0.012(2) 0.024(2) 0.025(2) 0.013(2) 0.0070(19) 0.0079(19) C5 0.012(2) 0.023(2) 0.024(2) 0.010(2) 0.0074(19) 0.0057(18) C6 0.015(2) 0.020(2) 0.027(3) 0.010(2) 0.009(2) 0.0079(19) C7 0.020(3) 0.026(3) 0.029(3) 0.016(2) 0.014(2) 0.013(2) C8 0.016(2) 0.023(2) 0.021(2) 0.010(2) 0.0072(19) 0.0074(19) O9 0.0202(18) 0.0214(17) 0.0211(17) 0.0104(14) 0.0037(14) 0.0079(14) C10 0.027(3) 0.032(3) 0.033(3) 0.020(2) 0.007(2) 0.007(2) O11 0.0234(19) 0.0204(17) 0.035(2) 0.0103(15) 0.0066(15) 0.0097(14) C12 0.035(3) 0.023(3) 0.064(4) 0.026(3) 0.011(3) 0.006(2) O13 0.030(2) 0.0308(19) 0.0182(17) 0.0121(15) 0.0076(15) 0.0153(16) C14 0.025(3) 0.025(3) 0.024(3) 0.007(2) -0.002(2) 0.010(2) C15 0.022(3) 0.027(3) 0.024(2) 0.012(2) 0.010(2) 0.013(2) Se16 0.0186(3) 0.0167(2) 0.0199(2) 0.0058(2) 0.0048(2) 0.00536(19) C17 0.028(3) 0.019(2) 0.015(2) 0.0066(19) 0.004(2) 0.007(2) C18 0.024(3) 0.016(2) 0.008(2) 0.0029(17) -0.0004(18) 0.0063(19) C19 0.015(2) 0.021(2) 0.018(2) 0.0107(19) 0.0043(18) 0.0044(18) C20 0.019(2) 0.023(2) 0.012(2) 0.0086(18) 0.0061(18) 0.0114(19) C21 0.024(3) 0.014(2) 0.015(2) 0.0072(18) 0.0047(19) 0.0073(18) C22 0.018(2) 0.022(2) 0.011(2) 0.0072(18) 0.0053(18) 0.0080(19) C23 0.018(2) 0.022(2) 0.008(2) 0.0035(18) 0.0000(17) 0.0090(19) C24 0.018(3) 0.021(2) 0.022(2) 0.010(2) 0.0088(19) 0.0099(19) C25 0.033(3) 0.028(3) 0.028(3) 0.014(2) 0.016(2) 0.017(2) C26 0.030(3) 0.019(3) 0.040(3) 0.004(2) 0.017(2) 0.013(2) C27 0.031(3) 0.032(3) 0.037(3) 0.022(2) 0.013(2) 0.017(2) O28 0.0284(19) 0.0200(16) 0.0132(15) 0.0047(13) 0.0032(13) 0.0135(14) C29 0.033(3) 0.031(3) 0.022(2) 0.014(2) 0.007(2) 0.018(2) C30 0.018(2) 0.017(2) 0.023(2) 0.0051(19) 0.0065(19) 0.0062(18) Se31 0.0356(3) 0.0181(3) 0.0182(3) 0.0062(2) 0.0135(2) 0.0055(2) C32 0.027(3) 0.017(2) 0.014(2) 0.0036(18) 0.0076(19) 0.0060(19) C33 0.028(3) 0.011(2) 0.016(2) 0.0063(18) 0.010(2) 0.0060(18) C34 0.018(2) 0.010(2) 0.015(2) 0.0047(17) 0.0046(18) 0.0054(17) C35 0.021(2) 0.010(2) 0.016(2) 0.0072(17) 0.0081(18) 0.0055(17) C36 0.024(3) 0.010(2) 0.015(2) 0.0063(17) 0.0069(19) 0.0039(18) C37 0.014(2) 0.014(2) 0.022(2) 0.0102(18) 0.0053(18) 0.0030(17) C38 0.023(3) 0.011(2) 0.024(2) 0.0105(18) 0.013(2) 0.0058(18) O39 0.0249(19) 0.0245(17) 0.0195(16) 0.0138(14) 0.0082(14) 0.0130(14) C40 0.016(3) 0.034(3) 0.023(2) 0.013(2) 0.007(2) 0.012(2) O41 0.0257(18) 0.0175(16) 0.0150(15) 0.0069(13) 0.0046(13) 0.0054(14) C42 0.028(3) 0.018(2) 0.017(2) 0.0078(19) 0.007(2) 0.010(2) O43 0.031(2) 0.0242(18) 0.0338(19) 0.0136(15) 0.0230(16) 0.0147(15) C44 0.041(3) 0.027(3) 0.035(3) 0.012(2) 0.022(3) 0.020(2) C45 0.025(3) 0.014(2) 0.014(2) 0.0068(18) 0.0089(19) 0.0065(18) Se46 0.0400(3) 0.0160(2) 0.0149(2) 0.00707(19) 0.0115(2) 0.0148(2) C47 0.031(3) 0.019(2) 0.019(2) 0.0109(19) 0.006(2) 0.013(2) C48 0.027(3) 0.017(2) 0.014(2) 0.0080(18) 0.0032(19) 0.011(2) C49 0.024(3) 0.022(2) 0.018(2) 0.0093(19) 0.0091(19) 0.014(2) C50 0.023(3) 0.021(2) 0.018(2) 0.0113(19) 0.0076(19) 0.0155(19) C51 0.022(3) 0.016(2) 0.017(2) 0.0069(18) 0.0000(19) 0.0064(19) C52 0.016(2) 0.028(3) 0.016(2) 0.011(2) 0.0019(18) 0.012(2) C53 0.024(3) 0.024(2) 0.015(2) 0.0081(19) 0.0034(19) 0.015(2) C54 0.036(3) 0.024(2) 0.019(2) 0.011(2) 0.009(2) 0.020(2) C55 0.073(5) 0.046(4) 0.077(5) 0.038(4) 0.053(4) 0.046(4) C56 0.067(4) 0.037(3) 0.029(3) 0.016(3) 0.009(3) 0.034(3) C57 0.058(4) 0.037(3) 0.034(3) 0.006(3) 0.008(3) 0.031(3) O58 0.032(2) 0.0265(18) 0.0166(16) 0.0045(14) 0.0035(14) 0.0200(16) C59 0.029(3) 0.026(3) 0.030(3) 0.012(2) 0.010(2) 0.018(2) C60 0.019(3) 0.037(3) 0.017(2) 0.010(2) 0.001(2) 0.014(2) C61 0.028(3) 0.029(3) 0.035(3) 0.019(2) 0.016(2) 0.017(2) Se62 0.0244(3) 0.0217(3) 0.0227(3) 0.0106(2) 0.0088(2) 0.0125(2) C63 0.023(3) 0.021(2) 0.020(2) 0.007(2) 0.000(2) 0.008(2) C64 0.022(3) 0.021(2) 0.023(2) 0.013(2) 0.004(2) 0.016(2) C65 0.020(3) 0.021(2) 0.019(2) 0.0099(19) 0.0061(19) 0.0108(19) C66 0.017(2) 0.021(2) 0.016(2) 0.0046(19) 0.0023(18) 0.0121(19) C67 0.014(2) 0.025(2) 0.019(2) 0.009(2) 0.0026(18) 0.0081(19) C68 0.020(3) 0.031(3) 0.017(2) 0.012(2) 0.0054(19) 0.017(2) C69 0.030(3) 0.019(2) 0.012(2) 0.0029(18) 0.0017(19) 0.017(2) C70 0.019(3) 0.023(2) 0.022(2) 0.002(2) 0.005(2) 0.011(2) C71 0.048(7) 0.026(5) 0.023(5) -0.001(4) 0.008(4) 0.013(5) C72 0.028(6) 0.019(5) 0.049(7) 0.001(5) 0.015(5) 0.002(4) C73 0.037(6) 0.031(5) 0.030(5) 0.005(4) 0.007(4) 0.026(4) C91 0.032(8) 0.045(9) 0.020(6) -0.012(6) -0.002(5) 0.022(7) C92 0.054(10) 0.022(7) 0.036(8) 0.001(6) 0.025(7) 0.009(6) C93 0.016(6) 0.017(5) 0.017(6) -0.003(4) 0.002(4) -0.003(4) O74 0.042(2) 0.0284(19) 0.0144(16) 0.0063(14) 0.0063(15) 0.0251(17) C75 0.044(3) 0.030(3) 0.014(2) 0.008(2) 0.003(2) 0.018(2) C76 0.013(3) 0.050(3) 0.022(2) 0.018(2) 0.005(2) 0.020(2) Se77 0.0194(3) 0.0216(3) 0.0255(3) 0.0123(2) 0.0095(2) 0.0109(2) C78 0.016(2) 0.017(2) 0.031(3) 0.014(2) 0.006(2) 0.0054(18) C79 0.039(3) 0.022(2) 0.022(2) 0.010(2) 0.012(2) 0.018(2) Cl80 0.0479(8) 0.0252(6) 0.0324(7) 0.0122(5) 0.0189(6) 0.0220(6) Cl81 0.0405(8) 0.0340(7) 0.0356(7) 0.0174(6) 0.0180(6) 0.0197(6) Cl82 0.0444(8) 0.0282(6) 0.0300(6) 0.0151(5) 0.0218(6) 0.0224(6) C83 0.034(3) 0.021(2) 0.024(3) 0.012(2) 0.007(2) 0.014(2) Cl84 0.130(2) 0.0867(14) 0.1242(18) 0.0786(14) 0.1104(17) 0.0844(15) Cl85 0.0412(9) 0.0347(8) 0.0699(11) 0.0308(8) 0.0079(8) 0.0087(6) Cl86 0.0762(12) 0.0441(9) 0.0290(7) 0.0085(7) -0.0034(7) 0.0323(8) _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 C2 1.967(4) . ? Se1 C60 1.971(5) . ? C2 C3 1.495(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.396(7) . ? C3 C4 1.397(7) . ? C4 O9 1.391(6) . ? C4 C5 1.398(7) . ? C5 C6 1.406(7) . ? C5 C15 1.505(7) . ? C6 O11 1.368(6) . ? C6 C7 1.410(7) . ? C7 C8 1.389(7) . ? C7 C61 1.509(7) . ? C8 O13 1.391(6) . ? O9 C10 1.435(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? O11 C12 1.444(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? O13 C14 1.436(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Se16 1.967(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? Se16 C17 1.987(4) . ? C17 C18 1.491(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.388(7) . ? C18 C19 1.395(6) . ? C19 C20 1.395(6) . ? C19 H19 0.9500 . ? C20 C21 1.393(6) . ? C20 C24 1.537(6) . ? C21 C22 1.405(6) . ? C21 H21 0.9500 . ? C22 C23 1.384(6) . ? C22 C30 1.504(6) . ? C23 O28 1.391(5) . ? C24 C27 1.523(7) . ? C24 C26 1.533(7) . ? C24 C25 1.535(6) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? O28 C29 1.435(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 Se31 1.968(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? Se31 C32 1.977(4) . ? C32 C33 1.501(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C38 1.385(7) . ? C33 C34 1.405(6) . ? C34 O39 1.372(6) . ? C34 C35 1.395(6) . ? C35 C36 1.385(7) . ? C35 C45 1.505(6) . ? C36 O41 1.385(5) . ? C36 C37 1.405(6) . ? C37 C38 1.412(6) . ? C37 C78 1.490(7) . ? C38 O43 1.380(5) . ? O39 C40 1.437(6) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? O41 C42 1.432(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? O43 C44 1.436(6) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 Se46 1.969(4) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? Se46 C47 1.969(5) . ? C47 C48 1.496(6) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C53 1.397(7) . ? C48 C49 1.403(6) . ? C49 C50 1.389(7) . ? C49 H49 0.9500 . ? C50 C51 1.386(7) . ? C50 C54 1.539(6) . ? C51 C52 1.400(6) . ? C51 H51 0.9500 . ? C52 C53 1.393(7) . ? C52 C60 1.497(7) . ? C53 O58 1.387(5) . ? C54 C55 1.517(8) . ? C54 C56 1.526(7) . ? C54 C57 1.545(8) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? O58 C59 1.422(6) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 Se62 1.967(5) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? Se62 C63 1.974(5) . ? C63 C64 1.514(7) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.393(6) . ? C64 C69 1.394(7) . ? C65 C66 1.386(7) . ? C65 H65 0.9500 . ? C66 C67 1.394(6) . ? C66 C70 1.540(6) . ? C67 C68 1.398(6) . ? C67 H67 0.9500 . ? C68 C69 1.399(7) . ? C68 C76 1.509(6) . ? C69 O74 1.387(5) . ? C70 C72 1.470(10) . ? C70 C93 1.477(12) . ? C70 C91 1.519(14) . ? C70 C73 1.548(10) . ? C70 C71 1.592(11) . ? C70 C92 1.604(15) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? O74 C75 1.431(6) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 Se77 1.968(5) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? Se77 C78 1.964(4) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 Cl81 1.756(5) . ? C79 Cl82 1.769(5) . ? C79 Cl80 1.772(5) . ? C79 H79 1.0000 . ? C83 Cl86 1.726(5) . ? C83 Cl84 1.751(5) . ? C83 Cl85 1.762(5) . ? C83 H83 1.0000 . ? 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 C2 Se1 C60 97.0(2) . . ? C3 C2 Se1 111.8(3) . . ? C3 C2 H2A 109.3 . . ? Se1 C2 H2A 109.3 . . ? C3 C2 H2B 109.3 . . ? Se1 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? C8 C3 C4 117.5(4) . . ? C8 C3 C2 121.0(4) . . ? C4 C3 C2 121.4(4) . . ? O9 C4 C5 117.6(4) . . ? O9 C4 C3 119.8(4) . . ? C5 C4 C3 122.5(4) . . ? C4 C5 C6 117.7(4) . . ? C4 C5 C15 121.2(4) . . ? C6 C5 C15 121.0(4) . . ? O11 C6 C5 119.5(4) . . ? O11 C6 C7 118.9(4) . . ? C5 C6 C7 121.6(4) . . ? C8 C7 C6 117.8(4) . . ? C8 C7 C61 120.9(4) . . ? C6 C7 C61 121.3(4) . . ? C7 C8 O13 119.6(4) . . ? C7 C8 C3 122.8(4) . . ? O13 C8 C3 117.5(4) . . ? C4 O9 C10 113.2(4) . . ? O9 C10 H10A 109.5 . . ? O9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 O11 C12 114.8(4) . . ? O11 C12 H12A 109.5 . . ? O11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 O13 C14 112.6(4) . . ? O13 C14 H14A 109.5 . . ? O13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C5 C15 Se16 108.5(3) . . ? C5 C15 H15A 110.0 . . ? Se16 C15 H15A 110.0 . . ? C5 C15 H15B 110.0 . . ? Se16 C15 H15B 110.0 . . ? H15A C15 H15B 108.4 . . ? C15 Se16 C17 95.9(2) . . ? C18 C17 Se16 110.3(3) . . ? C18 C17 H17A 109.6 . . ? Se16 C17 H17A 109.6 . . ? C18 C17 H17B 109.6 . . ? Se16 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C23 C18 C19 118.5(4) . . ? C23 C18 C17 119.7(4) . . ? C19 C18 C17 121.7(4) . . ? C18 C19 C20 122.0(4) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C21 C20 C19 117.7(4) . . ? C21 C20 C24 121.3(4) . . ? C19 C20 C24 120.9(4) . . ? C20 C21 C22 121.7(4) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C23 C22 C21 118.5(4) . . ? C23 C22 C30 121.6(4) . . ? C21 C22 C30 119.9(4) . . ? C22 C23 C18 121.6(4) . . ? C22 C23 O28 119.8(4) . . ? C18 C23 O28 118.5(4) . . ? C27 C24 C26 108.9(4) . . ? C27 C24 C20 108.5(4) . . ? C26 C24 C20 111.4(4) . . ? C27 C24 C25 110.5(4) . . ? C26 C24 C25 108.2(4) . . ? C20 C24 C25 109.4(4) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 O28 C29 112.4(3) . . ? O28 C29 H29A 109.5 . . ? O28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C22 C30 Se31 111.7(3) . . ? C22 C30 H30A 109.3 . . ? Se31 C30 H30A 109.3 . . ? C22 C30 H30B 109.3 . . ? Se31 C30 H30B 109.3 . . ? H30A C30 H30B 107.9 . . ? C30 Se31 C32 97.72(19) . . ? C33 C32 Se31 110.9(3) . . ? C33 C32 H32A 109.5 . . ? Se31 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? Se31 C32 H32B 109.5 . . ? H32A C32 H32B 108.0 . . ? C38 C33 C34 118.0(4) . . ? C38 C33 C32 122.2(4) . . ? C34 C33 C32 119.7(4) . . ? O39 C34 C35 119.1(4) . . ? O39 C34 C33 118.7(4) . . ? C35 C34 C33 122.0(4) . . ? C36 C35 C34 117.9(4) . . ? C36 C35 C45 120.7(4) . . ? C34 C35 C45 121.2(4) . . ? O41 C36 C35 119.1(4) . . ? O41 C36 C37 117.9(4) . . ? C35 C36 C37 122.8(4) . . ? C36 C37 C38 116.8(4) . . ? C36 C37 C78 122.1(4) . . ? C38 C37 C78 121.0(4) . . ? O43 C38 C33 120.3(4) . . ? O43 C38 C37 117.1(4) . . ? C33 C38 C37 122.4(4) . . ? C34 O39 C40 114.4(3) . . ? O39 C40 H40A 109.5 . . ? O39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C36 O41 C42 113.7(3) . . ? O41 C42 H42A 109.5 . . ? O41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C38 O43 C44 117.7(4) . . ? O43 C44 H44A 109.5 . . ? O43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C35 C45 Se46 111.7(3) . . ? C35 C45 H45A 109.3 . . ? Se46 C45 H45A 109.3 . . ? C35 C45 H45B 109.3 . . ? Se46 C45 H45B 109.3 . . ? H45A C45 H45B 107.9 . . ? C47 Se46 C45 98.47(19) . . ? C48 C47 Se46 108.2(3) . . ? C48 C47 H47A 110.1 . . ? Se46 C47 H47A 110.1 . . ? C48 C47 H47B 110.1 . . ? Se46 C47 H47B 110.1 . . ? H47A C47 H47B 108.4 . . ? C53 C48 C49 118.4(4) . . ? C53 C48 C47 121.6(4) . . ? C49 C48 C47 119.9(4) . . ? C50 C49 C48 122.1(4) . . ? C50 C49 H49 119.0 . . ? C48 C49 H49 119.0 . . ? C51 C50 C49 117.8(4) . . ? C51 C50 C54 119.8(4) . . ? C49 C50 C54 122.4(4) . . ? C50 C51 C52 122.2(4) . . ? C50 C51 H51 118.9 . . ? C52 C51 H51 118.9 . . ? C53 C52 C51 118.6(4) . . ? C53 C52 C60 121.3(4) . . ? C51 C52 C60 120.1(4) . . ? O58 C53 C52 119.7(4) . . ? O58 C53 C48 119.2(4) . . ? C52 C53 C48 120.9(4) . . ? C55 C54 C56 109.1(5) . . ? C55 C54 C50 113.1(4) . . ? C56 C54 C50 108.7(4) . . ? C55 C54 C57 107.8(5) . . ? C56 C54 C57 107.9(5) . . ? C50 C54 C57 110.1(4) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C53 O58 C59 116.2(3) . . ? O58 C59 H59A 109.5 . . ? O58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? O58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C52 C60 Se1 108.4(3) . . ? C52 C60 H60A 110.0 . . ? Se1 C60 H60A 110.0 . . ? C52 C60 H60B 110.0 . . ? Se1 C60 H60B 110.0 . . ? H60A C60 H60B 108.4 . . ? C7 C61 Se62 112.8(3) . . ? C7 C61 H61A 109.0 . . ? Se62 C61 H61A 109.0 . . ? C7 C61 H61B 109.0 . . ? Se62 C61 H61B 109.0 . . ? H61A C61 H61B 107.8 . . ? C61 Se62 C63 95.3(2) . . ? C64 C63 Se62 112.7(3) . . ? C64 C63 H63A 109.1 . . ? Se62 C63 H63A 109.1 . . ? C64 C63 H63B 109.1 . . ? Se62 C63 H63B 109.1 . . ? H63A C63 H63B 107.8 . . ? C65 C64 C69 119.0(4) . . ? C65 C64 C63 119.6(4) . . ? C69 C64 C63 121.4(4) . . ? C66 C65 C64 122.2(4) . . ? C66 C65 H65 118.9 . . ? C64 C65 H65 118.9 . . ? C65 C66 C67 117.4(4) . . ? C65 C66 C70 121.6(4) . . ? C67 C66 C70 121.0(4) . . ? C66 C67 C68 122.5(4) . . ? C66 C67 H67 118.8 . . ? C68 C67 H67 118.8 . . ? C67 C68 C69 118.2(4) . . ? C67 C68 C76 120.0(4) . . ? C69 C68 C76 121.8(4) . . ? O74 C69 C64 120.0(4) . . ? O74 C69 C68 119.2(4) . . ? C64 C69 C68 120.7(4) . . ? C72 C70 C93 131.6(6) . . ? C72 C70 C91 49.4(8) . . ? C93 C70 C91 111.8(8) . . ? C72 C70 C66 114.0(5) . . ? C93 C70 C66 114.4(5) . . ? C91 C70 C66 109.0(5) . . ? C72 C70 C73 112.1(7) . . ? C93 C70 C73 52.1(6) . . ? C91 C70 C73 143.1(6) . . ? C66 C70 C73 107.9(5) . . ? C72 C70 C71 107.5(7) . . ? C93 C70 C71 55.6(6) . . ? C91 C70 C71 62.5(8) . . ? C66 C70 C71 108.0(5) . . ? C73 C70 C71 107.1(6) . . ? C72 C70 C92 55.8(8) . . ? C93 C70 C92 107.4(7) . . ? C91 C70 C92 104.2(9) . . ? C66 C70 C92 109.5(6) . . ? C73 C70 C92 61.1(7) . . ? C71 C70 C92 142.5(6) . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? C70 C73 H73A 109.5 . . ? C70 C73 H73B 109.5 . . ? C70 C73 H73C 109.5 . . ? C70 C91 H91A 109.5 . . ? C70 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C70 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C70 C92 H92A 109.5 . . ? C70 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C70 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C70 C93 H93A 109.5 . . ? C70 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C70 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C69 O74 C75 114.9(4) . . ? O74 C75 H75A 109.5 . . ? O74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? O74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C68 C76 Se77 113.3(3) . . ? C68 C76 H76A 108.9 . . ? Se77 C76 H76A 108.9 . . ? C68 C76 H76B 108.9 . . ? Se77 C76 H76B 108.9 . . ? H76A C76 H76B 107.7 . . ? C78 Se77 C76 96.3(2) . . ? C37 C78 Se77 110.4(3) . . ? C37 C78 H78A 109.6 . . ? Se77 C78 H78A 109.6 . . ? C37 C78 H78B 109.6 . . ? Se77 C78 H78B 109.6 . . ? H78A C78 H78B 108.1 . . ? Cl81 C79 Cl82 110.2(3) . . ? Cl81 C79 Cl80 111.1(3) . . ? Cl82 C79 Cl80 110.1(3) . . ? Cl81 C79 H79 108.5 . . ? Cl82 C79 H79 108.5 . . ? Cl80 C79 H79 108.5 . . ? Cl86 C83 Cl84 109.3(3) . . ? Cl86 C83 Cl85 110.9(3) . . ? Cl84 C83 Cl85 110.3(3) . . ? Cl86 C83 H83 108.8 . . ? Cl84 C83 H83 108.8 . . ? Cl85 C83 H83 108.8 . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 70.78 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.278 _refine_diff_density_min -0.909 _refine_diff_density_rms 0.124 data_14THF _database_code_depnum_ccdc_archive 'CCDC 848953' #TrackingRef '14.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H72 O4 Se4, 2(C4 H8 O)' _chemical_formula_sum 'C60 H88 O6 Se4' _chemical_formula_weight 1221.14 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x, -y+1/2, z' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1/2, -y+1, z+1/2' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x, y-1/2, -z' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x+1/2, y, -z+1/2' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 28.310(4) _cell_length_b 28.310(4) _cell_length_c 14.618(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11716(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9805 _cell_measurement_theta_min 2.566 _cell_measurement_theta_max 26.679 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5056 _exptl_absorpt_coefficient_mu 2.552 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4956 _exptl_absorpt_correction_T_max 0.8028 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_type KM4CCD _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 94873 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 26.41 _reflns_number_total 5998 _reflns_number_gt 4733 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrysAlisCCD _computing_cell_refinement CrysAlisRED _computing_data_reduction CrysAlisRED _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0409P)^2^+35.2950P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5998 _refine_ls_number_parameters 324 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.002 _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 0.472857(11) 0.648065(11) 0.46108(2) 0.02283(9) Uani 1 1 d . . . C1 C 0.40363(11) 0.64475(11) 0.4566(2) 0.0244(7) Uani 1 1 d . . . H1A H 0.3919 0.6666 0.4087 0.029 Uiso 1 1 calc R . . H1B H 0.3940 0.6123 0.4394 0.029 Uiso 1 1 calc R . . Se2 Se 0.434363(11) 0.666562(11) -0.04077(2) 0.02278(9) Uani 1 1 d . . . C2 C 0.38136(10) 0.65742(11) 0.5463(2) 0.0230(6) Uani 1 1 d . . . C3 C 0.36505(11) 0.62255(11) 0.6042(2) 0.0238(6) Uani 1 1 d . . . H3 H 0.3673 0.5906 0.5849 0.029 Uiso 1 1 calc R . . C4 C 0.34546(11) 0.63208(11) 0.6896(2) 0.0238(7) Uani 1 1 d . . . C5 C 0.34240(10) 0.67899(11) 0.7151(2) 0.0237(6) Uani 1 1 d . . . H5 H 0.3293 0.6865 0.7731 0.028 Uiso 1 1 calc R . . C6 C 0.35787(10) 0.71576(11) 0.6588(2) 0.0217(6) Uani 1 1 d . . . C7 C 0.37775(10) 0.70451(11) 0.5746(2) 0.0221(6) Uani 1 1 d . . . C8 C 0.32841(12) 0.59159(12) 0.7499(2) 0.0301(7) Uani 1 1 d . . . C9 C 0.36959(16) 0.55818(14) 0.7686(3) 0.0483(10) Uani 1 1 d . . . H9A H 0.3587 0.5319 0.8070 0.072 Uiso 1 1 calc R . . H9B H 0.3948 0.5753 0.8004 0.072 Uiso 1 1 calc R . . H9C H 0.3817 0.5458 0.7106 0.072 Uiso 1 1 calc R . . C10 C 0.28922(15) 0.56545(14) 0.7010(3) 0.0451(10) Uani 1 1 d . . . H10A H 0.2639 0.5876 0.6855 0.068 Uiso 1 1 calc R . . H10B H 0.2767 0.5406 0.7411 0.068 Uiso 1 1 calc R . . H10C H 0.3017 0.5512 0.6449 0.068 Uiso 1 1 calc R . . C11 C 0.30933(15) 0.60897(13) 0.8411(2) 0.0411(9) Uani 1 1 d . . . H11A H 0.2995 0.5819 0.8782 0.062 Uiso 1 1 calc R . . H11B H 0.2821 0.6297 0.8304 0.062 Uiso 1 1 calc R . . H11C H 0.3340 0.6266 0.8734 0.062 Uiso 1 1 calc R . . O12 O 0.38962(8) 0.73923(8) 0.51220(14) 0.0256(5) Uani 1 1 d . . . C13 C 0.43076(11) 0.76721(11) 0.5322(2) 0.0262(7) Uani 1 1 d . . . H13A H 0.4588 0.7520 0.5062 0.039 Uiso 1 1 calc R . . H13B H 0.4345 0.7700 0.5986 0.039 Uiso 1 1 calc R . . H13C H 0.4270 0.7987 0.5055 0.039 Uiso 1 1 calc R . . C14 C 0.35235(10) 0.76573(11) 0.6902(2) 0.0218(6) Uani 1 1 d . . . H14A H 0.3198 0.7710 0.7128 0.026 Uiso 1 1 calc R . . H14B H 0.3583 0.7877 0.6388 0.026 Uiso 1 1 calc R . . C15 C 0.39137(11) 0.64727(11) 0.0582(2) 0.0241(7) Uani 1 1 d . . . H15A H 0.3683 0.6239 0.0352 0.029 Uiso 1 1 calc R . . H15B H 0.4095 0.6327 0.1088 0.029 Uiso 1 1 calc R . . C16 C 0.36633(10) 0.69055(11) 0.0912(2) 0.0219(6) Uani 1 1 d . . . C17 C 0.33352(10) 0.71242(11) 0.0339(2) 0.0226(6) Uani 1 1 d . . . H17 H 0.3276 0.6992 -0.0248 0.027 Uiso 1 1 calc R . . C18 C 0.30928(10) 0.75287(11) 0.0600(2) 0.0220(6) Uani 1 1 d . . . C19 C 0.31873(10) 0.77095(11) 0.1464(2) 0.0215(6) Uani 1 1 d . . . H19 H 0.3021 0.7983 0.1661 0.026 Uiso 1 1 calc R . . C20 C 0.35118(10) 0.75090(11) 0.2048(2) 0.0213(6) Uani 1 1 d . . . C21 C 0.37523(10) 0.71009(11) 0.1765(2) 0.0214(6) Uani 1 1 d . . . C22 C 0.27304(11) 0.77746(12) -0.0013(2) 0.0268(7) Uani 1 1 d . . . C23 C 0.22569(12) 0.77580(17) 0.0462(2) 0.0445(10) Uani 1 1 d . . . H23A H 0.2141 0.7432 0.0471 0.067 Uiso 1 1 calc R . . H23B H 0.2032 0.7958 0.0133 0.067 Uiso 1 1 calc R . . H23C H 0.2291 0.7873 0.1091 0.067 Uiso 1 1 calc R . . C24 C 0.28892(14) 0.82899(13) -0.0153(3) 0.0414(9) Uani 1 1 d . . . H24A H 0.2660 0.8454 -0.0541 0.062 Uiso 1 1 calc R . . H24B H 0.3200 0.8295 -0.0448 0.062 Uiso 1 1 calc R . . H24C H 0.2909 0.8449 0.0442 0.062 Uiso 1 1 calc R . . C25 C 0.26881(12) 0.75441(13) -0.0946(2) 0.0327(8) Uani 1 1 d . . . H25A H 0.2584 0.7216 -0.0874 0.049 Uiso 1 1 calc R . . H25B H 0.2996 0.7550 -0.1253 0.049 Uiso 1 1 calc R . . H25C H 0.2457 0.7717 -0.1316 0.049 Uiso 1 1 calc R . . O26 O 0.40512(7) 0.68797(8) 0.23786(14) 0.0262(5) Uani 1 1 d . . . C27 C 0.45487(11) 0.69343(12) 0.2202(2) 0.0266(7) Uani 1 1 d . . . H27A H 0.4607 0.6909 0.1543 0.040 Uiso 1 1 calc R . . H27B H 0.4724 0.6686 0.2523 0.040 Uiso 1 1 calc R . . H27C H 0.4653 0.7245 0.2419 0.040 Uiso 1 1 calc R . . C28 C 0.36087(11) 0.77416(11) 0.2948(2) 0.0238(6) Uani 1 1 d . . . H28A H 0.3659 0.7495 0.3419 0.029 Uiso 1 1 calc R . . H28B H 0.3329 0.7930 0.3131 0.029 Uiso 1 1 calc R . . O29 O 0.37568(9) 1.02108(9) -0.0074(2) 0.0476(7) Uani 1 1 d . . . C30 C 0.39234(15) 0.97737(13) 0.0285(3) 0.0459(10) Uani 1 1 d . . . H30A H 0.3831 0.9741 0.0935 0.055 Uiso 1 1 calc R . . H30B H 0.4272 0.9758 0.0243 0.055 Uiso 1 1 calc R . . C31 C 0.37066(18) 0.93955(16) -0.0267(4) 0.0684(15) Uani 1 1 d . . . H31A H 0.3590 0.9137 0.0130 0.082 Uiso 1 1 calc R . . H31B H 0.3938 0.9264 -0.0707 0.082 Uiso 1 1 calc R . . C32 C 0.3306(2) 0.9628(2) -0.0761(5) 0.095(2) Uani 1 1 d . . . H32A H 0.3356 0.9615 -0.1431 0.114 Uiso 1 1 calc R . . H32B H 0.3003 0.9470 -0.0614 0.114 Uiso 1 1 calc R . . C33 C 0.33012(17) 1.01159(17) -0.0442(4) 0.0708(15) Uani 1 1 d . . . H33A H 0.3233 1.0333 -0.0956 0.085 Uiso 1 1 calc R . . H33B H 0.3056 1.0159 0.0033 0.085 Uiso 1 1 calc R . . 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 0.02371(16) 0.02471(17) 0.02006(16) 0.00290(12) 0.00059(12) 0.00172(12) C1 0.0260(16) 0.0288(16) 0.0185(15) -0.0023(13) -0.0039(13) 0.0012(13) Se2 0.02626(17) 0.02294(16) 0.01915(16) 0.00142(12) 0.00064(12) 0.00179(12) C2 0.0193(15) 0.0287(16) 0.0209(15) -0.0011(13) -0.0044(12) 0.0003(12) C3 0.0240(16) 0.0228(15) 0.0245(16) -0.0023(12) -0.0052(13) -0.0005(12) C4 0.0222(15) 0.0293(17) 0.0198(15) 0.0008(13) -0.0042(12) -0.0029(13) C5 0.0211(15) 0.0296(17) 0.0202(15) -0.0015(13) -0.0030(12) -0.0023(12) C6 0.0194(15) 0.0252(16) 0.0204(15) -0.0002(12) -0.0056(12) -0.0018(12) C7 0.0188(15) 0.0257(16) 0.0218(15) 0.0037(13) -0.0060(12) -0.0016(12) C8 0.0386(19) 0.0283(17) 0.0234(16) 0.0036(14) 0.0010(14) -0.0072(15) C9 0.072(3) 0.037(2) 0.036(2) 0.0129(17) 0.003(2) 0.009(2) C10 0.057(3) 0.045(2) 0.033(2) 0.0024(17) 0.0042(18) -0.0187(19) C11 0.055(2) 0.033(2) 0.035(2) 0.0030(16) 0.0107(18) -0.0132(17) O12 0.0299(12) 0.0283(12) 0.0187(11) 0.0062(9) -0.0045(9) -0.0059(9) C13 0.0255(16) 0.0278(17) 0.0255(17) 0.0024(13) -0.0011(13) -0.0055(13) C14 0.0207(15) 0.0258(16) 0.0189(15) -0.0011(12) -0.0031(12) 0.0002(12) C15 0.0297(17) 0.0230(16) 0.0197(15) 0.0012(12) 0.0026(13) -0.0005(13) C16 0.0200(15) 0.0235(15) 0.0223(15) 0.0020(12) 0.0030(12) -0.0015(12) C17 0.0227(15) 0.0243(15) 0.0209(15) -0.0004(12) -0.0009(12) -0.0050(12) C18 0.0169(14) 0.0253(16) 0.0237(16) 0.0044(12) 0.0013(12) -0.0042(12) C19 0.0198(15) 0.0236(15) 0.0212(15) 0.0010(12) 0.0025(12) -0.0007(12) C20 0.0187(14) 0.0263(16) 0.0188(14) 0.0002(12) 0.0037(12) -0.0027(12) C21 0.0192(15) 0.0251(16) 0.0198(15) 0.0047(12) 0.0018(12) -0.0017(12) C22 0.0203(15) 0.0353(18) 0.0249(16) 0.0045(14) -0.0012(13) 0.0043(13) C23 0.0212(17) 0.084(3) 0.0278(19) 0.0045(19) -0.0060(15) 0.0033(18) C24 0.052(2) 0.034(2) 0.038(2) 0.0063(16) -0.0151(18) 0.0034(17) C25 0.0288(18) 0.044(2) 0.0251(17) 0.0013(15) -0.0067(14) 0.0027(15) O26 0.0235(11) 0.0348(12) 0.0204(11) 0.0063(9) 0.0003(9) 0.0031(9) C27 0.0218(16) 0.0315(17) 0.0266(17) 0.0015(14) -0.0016(13) 0.0035(13) C28 0.0214(15) 0.0290(17) 0.0209(15) 0.0005(13) 0.0040(12) -0.0008(12) O29 0.0396(15) 0.0333(14) 0.0698(19) 0.0048(13) -0.0015(14) -0.0005(12) C30 0.046(2) 0.036(2) 0.055(3) 0.0006(19) -0.0007(19) 0.0048(17) C31 0.064(3) 0.036(2) 0.105(4) -0.004(3) -0.032(3) -0.009(2) C32 0.088(4) 0.067(4) 0.131(6) -0.009(4) -0.055(4) -0.005(3) C33 0.044(3) 0.053(3) 0.115(5) -0.005(3) -0.011(3) 0.010(2) _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 C1 1.963(3) . ? Se1 C14 1.965(3) 16_656 ? C1 C2 1.499(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? Se2 C28 1.967(3) 16_655 ? Se2 C15 1.968(3) . ? C2 C3 1.380(4) . ? C2 C7 1.400(4) . ? C3 C4 1.393(4) . ? C3 H3 0.9500 . ? C4 C5 1.382(4) . ? C4 C8 1.524(4) . ? C5 C6 1.398(4) . ? C5 H5 0.9500 . ? C6 C7 1.390(4) . ? C6 C14 1.496(4) . ? C7 O12 1.383(4) . ? C8 C10 1.513(5) . ? C8 C11 1.520(5) . ? C8 C9 1.526(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? O12 C13 1.439(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Se1 1.965(3) 14_566 ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.495(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.386(4) . ? C16 C17 1.396(4) . ? C17 C18 1.388(4) . ? C17 H17 0.9500 . ? C18 C19 1.389(4) . ? C18 C22 1.530(4) . ? C19 C20 1.376(4) . ? C19 H19 0.9500 . ? C20 C21 1.403(4) . ? C20 C28 1.498(4) . ? C21 O26 1.383(4) . ? C22 C23 1.511(5) . ? C22 C25 1.518(5) . ? C22 C24 1.540(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? O26 C27 1.440(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 Se2 1.967(3) 14_565 ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? O29 C30 1.424(5) . ? O29 C33 1.423(5) . ? C30 C31 1.475(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.497(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.457(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? 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 C1 Se1 C14 99.06(13) . 16_656 ? C2 C1 Se1 112.3(2) . . ? C2 C1 H1A 109.1 . . ? Se1 C1 H1A 109.1 . . ? C2 C1 H1B 109.1 . . ? Se1 C1 H1B 109.1 . . ? H1A C1 H1B 107.9 . . ? C28 Se2 C15 99.73(13) 16_655 . ? C3 C2 C7 118.4(3) . . ? C3 C2 C1 120.4(3) . . ? C7 C2 C1 121.2(3) . . ? C2 C3 C4 123.0(3) . . ? C2 C3 H3 118.5 . . ? C4 C3 H3 118.5 . . ? C5 C4 C3 116.9(3) . . ? C5 C4 C8 123.2(3) . . ? C3 C4 C8 119.9(3) . . ? C4 C5 C6 122.5(3) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C7 C6 C5 118.5(3) . . ? C7 C6 C14 122.1(3) . . ? C5 C6 C14 119.4(3) . . ? O12 C7 C6 121.3(3) . . ? O12 C7 C2 117.6(3) . . ? C6 C7 C2 120.6(3) . . ? C10 C8 C11 108.2(3) . . ? C10 C8 C4 109.1(3) . . ? C11 C8 C4 112.1(3) . . ? C10 C8 C9 110.0(3) . . ? C11 C8 C9 108.4(3) . . ? C4 C8 C9 109.1(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 O12 C13 117.0(2) . . ? O12 C13 H13A 109.5 . . ? O12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C6 C14 Se1 108.2(2) . 14_566 ? C6 C14 H14A 110.1 . . ? Se1 C14 H14A 110.1 14_566 . ? C6 C14 H14B 110.1 . . ? Se1 C14 H14B 110.1 14_566 . ? H14A C14 H14B 108.4 . . ? C16 C15 Se2 107.6(2) . . ? C16 C15 H15A 110.2 . . ? Se2 C15 H15A 110.2 . . ? C16 C15 H15B 110.2 . . ? Se2 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? C21 C16 C17 118.9(3) . . ? C21 C16 C15 122.1(3) . . ? C17 C16 C15 119.0(3) . . ? C18 C17 C16 122.0(3) . . ? C18 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? C19 C18 C17 117.3(3) . . ? C19 C18 C22 119.6(3) . . ? C17 C18 C22 123.1(3) . . ? C20 C19 C18 122.7(3) . . ? C20 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? C19 C20 C21 118.8(3) . . ? C19 C20 C28 119.1(3) . . ? C21 C20 C28 122.2(3) . . ? O26 C21 C16 120.9(3) . . ? O26 C21 C20 118.6(3) . . ? C16 C21 C20 120.3(3) . . ? C23 C22 C25 109.3(3) . . ? C23 C22 C18 108.2(3) . . ? C25 C22 C18 112.6(3) . . ? C23 C22 C24 110.5(3) . . ? C25 C22 C24 108.1(3) . . ? C18 C22 C24 108.2(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 O26 C27 115.7(2) . . ? O26 C27 H27A 109.5 . . ? O26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C20 C28 Se2 112.5(2) . 14_565 ? C20 C28 H28A 109.1 . . ? Se2 C28 H28A 109.1 14_565 . ? C20 C28 H28B 109.1 . . ? Se2 C28 H28B 109.1 14_565 . ? H28A C28 H28B 107.8 . . ? C30 O29 C33 106.0(3) . . ? O29 C30 C31 107.0(4) . . ? O29 C30 H30A 110.3 . . ? C31 C30 H30A 110.3 . . ? O29 C30 H30B 110.3 . . ? C31 C30 H30B 110.3 . . ? H30A C30 H30B 108.6 . . ? C30 C31 C32 105.0(4) . . ? C30 C31 H31A 110.7 . . ? C32 C31 H31A 110.7 . . ? C30 C31 H31B 110.7 . . ? C32 C31 H31B 110.7 . . ? H31A C31 H31B 108.8 . . ? C33 C32 C31 105.6(4) . . ? C33 C32 H32A 110.6 . . ? C31 C32 H32A 110.6 . . ? C33 C32 H32B 110.6 . . ? C31 C32 H32B 110.6 . . ? H32A C32 H32B 108.7 . . ? O29 C33 C32 107.0(4) . . ? O29 C33 H33A 110.3 . . ? C32 C33 H33A 110.3 . . ? O29 C33 H33B 110.3 . . ? C32 C33 H33B 110.3 . . ? H33A C33 H33B 108.6 . . ? 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 C14 Se1 C1 C2 58.7(2) 16_656 . . . ? Se1 C1 C2 C3 -101.3(3) . . . . ? Se1 C1 C2 C7 76.9(3) . . . . ? C7 C2 C3 C4 -0.4(5) . . . . ? C1 C2 C3 C4 177.8(3) . . . . ? C2 C3 C4 C5 0.6(4) . . . . ? C2 C3 C4 C8 -179.7(3) . . . . ? C3 C4 C5 C6 0.2(4) . . . . ? C8 C4 C5 C6 -179.5(3) . . . . ? C4 C5 C6 C7 -1.0(4) . . . . ? C4 C5 C6 C14 178.6(3) . . . . ? C5 C6 C7 O12 173.8(3) . . . . ? C14 C6 C7 O12 -5.8(4) . . . . ? C5 C6 C7 C2 1.2(4) . . . . ? C14 C6 C7 C2 -178.4(3) . . . . ? C3 C2 C7 O12 -173.4(3) . . . . ? C1 C2 C7 O12 8.4(4) . . . . ? C3 C2 C7 C6 -0.5(4) . . . . ? C1 C2 C7 C6 -178.7(3) . . . . ? C5 C4 C8 C10 118.1(4) . . . . ? C3 C4 C8 C10 -61.6(4) . . . . ? C5 C4 C8 C11 -1.7(5) . . . . ? C3 C4 C8 C11 178.6(3) . . . . ? C5 C4 C8 C9 -121.7(3) . . . . ? C3 C4 C8 C9 58.6(4) . . . . ? C6 C7 O12 C13 73.7(4) . . . . ? C2 C7 O12 C13 -113.5(3) . . . . ? C7 C6 C14 Se1 -108.4(3) . . . 14_566 ? C5 C6 C14 Se1 71.9(3) . . . 14_566 ? C28 Se2 C15 C16 163.0(2) 16_655 . . . ? Se2 C15 C16 C21 -110.1(3) . . . . ? Se2 C15 C16 C17 68.9(3) . . . . ? C21 C16 C17 C18 -0.6(4) . . . . ? C15 C16 C17 C18 -179.6(3) . . . . ? C16 C17 C18 C19 -0.3(4) . . . . ? C16 C17 C18 C22 -179.8(3) . . . . ? C17 C18 C19 C20 1.1(4) . . . . ? C22 C18 C19 C20 -179.4(3) . . . . ? C18 C19 C20 C21 -1.0(4) . . . . ? C18 C19 C20 C28 177.0(3) . . . . ? C17 C16 C21 O26 175.8(3) . . . . ? C15 C16 C21 O26 -5.3(4) . . . . ? C17 C16 C21 C20 0.7(4) . . . . ? C15 C16 C21 C20 179.7(3) . . . . ? C19 C20 C21 O26 -175.1(3) . . . . ? C28 C20 C21 O26 7.0(4) . . . . ? C19 C20 C21 C16 0.1(4) . . . . ? C28 C20 C21 C16 -177.8(3) . . . . ? C19 C18 C22 C23 -61.8(4) . . . . ? C17 C18 C22 C23 117.6(3) . . . . ? C19 C18 C22 C25 177.3(3) . . . . ? C17 C18 C22 C25 -3.2(4) . . . . ? C19 C18 C22 C24 57.9(4) . . . . ? C17 C18 C22 C24 -122.7(3) . . . . ? C16 C21 O26 C27 77.8(4) . . . . ? C20 C21 O26 C27 -107.0(3) . . . . ? C19 C20 C28 Se2 -96.0(3) . . . 14_565 ? C21 C20 C28 Se2 81.9(3) . . . 14_565 ? C33 O29 C30 C31 29.3(5) . . . . ? O29 C30 C31 C32 -16.4(6) . . . . ? C30 C31 C32 C33 -2.3(7) . . . . ? C30 O29 C33 C32 -30.9(6) . . . . ? C31 C32 C33 O29 20.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.121 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.080 data_15 _database_code_depnum_ccdc_archive 'CCDC 848954' #TrackingRef '15.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H72 Ag O4 Se4, C F3 O3 S' _chemical_formula_sum 'C53 H72 Ag F3 O7 S Se4' _chemical_formula_weight 1333.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.801(7) _cell_length_b 27.671(12) _cell_length_c 31.568(16) _cell_angle_alpha 90.00 _cell_angle_beta 93.689(14) _cell_angle_gamma 90.00 _cell_volume 12030(10) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5376 _exptl_absorpt_coefficient_mu 6.225 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.159 _exptl_absorpt_correction_T_max 0.536 _exptl_absorpt_process_details 'WinGX v1.70.01' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'crossed G\"obel mirrors' _diffrn_measurement_device_type 'SMART 6000' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21230 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 66.59 _reflns_number_total 21230 _reflns_number_gt 18418 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material Platon _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^)+(0.0112P)^2^+189.0525P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21230 _refine_ls_number_parameters 1452 _refine_ls_number_restraints 1723 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0837 _refine_ls_wR_factor_ref 0.1779 _refine_ls_wR_factor_gt 0.1718 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.097 _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 C1 C 0.3453(6) 0.4195(3) 0.4132(3) 0.0339(9) Uani 1 1 d U . . C2 C 0.2787(6) 0.3958(3) 0.4373(3) 0.0384(10) Uani 1 1 d U . . C3 C 0.1796(6) 0.4027(3) 0.4258(3) 0.0408(11) Uani 1 1 d U . . H3 H 0.1326 0.3882 0.4425 0.049 Uiso 1 1 calc R . . C4 C 0.1485(6) 0.4303(3) 0.3904(3) 0.0423(11) Uani 1 1 d U . . C5 C 0.2181(6) 0.4496(3) 0.3657(3) 0.0377(11) Uani 1 1 d U . . H5 H 0.1979 0.4668 0.3407 0.045 Uiso 1 1 calc R . . C6 C 0.3175(6) 0.4445(3) 0.3766(3) 0.0345(9) Uani 1 1 d U . . C7 C 0.4820(6) 0.4486(3) 0.4537(3) 0.0423(18) Uani 1 1 d U . . H7A H 0.4762 0.4808 0.4407 0.064 Uiso 1 1 calc R . . H7B H 0.5504 0.4417 0.4615 0.064 Uiso 1 1 calc R . . H7C H 0.4450 0.4477 0.4792 0.064 Uiso 1 1 calc R . . C8 C 0.0393(6) 0.4390(4) 0.3811(4) 0.0491(13) Uani 1 1 d U . . C9 C 0.0026(7) 0.4685(4) 0.4164(4) 0.060(2) Uani 1 1 d U . . H9A H 0.0116 0.4505 0.4431 0.091 Uiso 1 1 calc R . . H9B H -0.0666 0.4753 0.4104 0.091 Uiso 1 1 calc R . . H9C H 0.0387 0.4990 0.4188 0.091 Uiso 1 1 calc R . . C10 C -0.0137(7) 0.3904(4) 0.3775(4) 0.055(2) Uani 1 1 d U . . H10A H 0.0010 0.3715 0.4033 0.083 Uiso 1 1 calc R . . H10B H 0.0077 0.3726 0.3529 0.083 Uiso 1 1 calc R . . H10C H -0.0839 0.3961 0.3738 0.083 Uiso 1 1 calc R . . C11 C 0.0182(7) 0.4668(4) 0.3397(4) 0.060(2) Uani 1 1 d U . . H11A H -0.0521 0.4705 0.3343 0.090 Uiso 1 1 calc R . . H11B H 0.0445 0.4489 0.3162 0.090 Uiso 1 1 calc R . . H11C H 0.0487 0.4988 0.3420 0.090 Uiso 1 1 calc R . . C12 C 0.3925(6) 0.4612(3) 0.3479(3) 0.0349(11) Uani 1 1 d U . . H12A H 0.4476 0.4763 0.3647 0.042 Uiso 1 1 calc R . . H12B H 0.3643 0.4855 0.3276 0.042 Uiso 1 1 calc R . . C13 C 0.3140(7) 0.3597(3) 0.4692(3) 0.0415(11) Uani 1 1 d U . . H13A H 0.2611 0.3511 0.4876 0.050 Uiso 1 1 calc R . . H13B H 0.3683 0.3734 0.4874 0.050 Uiso 1 1 calc R . . C14 C 0.2724(6) 0.2597(3) 0.3443(3) 0.0438(10) Uani 1 1 d U . . C15 C 0.2428(7) 0.2445(4) 0.3832(4) 0.0481(11) Uani 1 1 d U . . C16 C 0.2358(7) 0.1950(4) 0.3916(4) 0.0571(12) Uani 1 1 d U . . H16 H 0.2141 0.1842 0.4179 0.069 Uiso 1 1 calc R . . C17 C 0.2613(8) 0.1610(4) 0.3605(5) 0.0668(13) Uani 1 1 d U . . C18 C 0.2969(8) 0.1773(4) 0.3238(4) 0.0598(13) Uani 1 1 d U . . H18 H 0.3165 0.1543 0.3037 0.072 Uiso 1 1 calc R . . C19 C 0.3058(7) 0.2263(4) 0.3146(4) 0.0516(11) Uani 1 1 d U . . C20 C 0.1953(6) 0.3272(3) 0.3129(3) 0.0441(18) Uani 1 1 d U . . H20A H 0.1851 0.3100 0.2859 0.066 Uiso 1 1 calc R . . H20B H 0.2048 0.3617 0.3074 0.066 Uiso 1 1 calc R . . H20C H 0.1385 0.3229 0.3296 0.066 Uiso 1 1 calc R . . C21 C 0.2480(10) 0.1064(5) 0.3730(5) 0.0799(15) Uani 1 1 d U . . C22 C 0.1935(12) 0.0967(5) 0.4105(6) 0.098(2) Uani 1 1 d U . . H22A H 0.1313 0.1139 0.4079 0.147 Uiso 1 1 calc R . . H22B H 0.2311 0.1078 0.4361 0.147 Uiso 1 1 calc R . . H22C H 0.1815 0.0619 0.4127 0.147 Uiso 1 1 calc R . . C23 C 0.3481(10) 0.0849(5) 0.3813(6) 0.093(3) Uani 1 1 d U . . H23A H 0.3823 0.1019 0.4051 0.139 Uiso 1 1 calc R . . H23B H 0.3847 0.0883 0.3559 0.139 Uiso 1 1 calc R . . H23C H 0.3423 0.0506 0.3884 0.139 Uiso 1 1 calc R . . C24 C 0.1952(11) 0.0820(5) 0.3379(6) 0.092(3) Uani 1 1 d U . . H24A H 0.1870 0.0478 0.3451 0.138 Uiso 1 1 calc R . . H24B H 0.2317 0.0846 0.3124 0.138 Uiso 1 1 calc R . . H24C H 0.1313 0.0970 0.3327 0.138 Uiso 1 1 calc R . . C25 C 0.2285(6) 0.2811(3) 0.4173(3) 0.0454(13) Uani 1 1 d U . . H25A H 0.1919 0.2667 0.4401 0.055 Uiso 1 1 calc R . . H25B H 0.1916 0.3092 0.4054 0.055 Uiso 1 1 calc R . . C26 C 0.3580(7) 0.2449(4) 0.2787(4) 0.0525(12) Uani 1 1 d U . . H26A H 0.3211 0.2719 0.2650 0.063 Uiso 1 1 calc R . . H26B H 0.3642 0.2190 0.2574 0.063 Uiso 1 1 calc R . . C27 C 0.6268(6) 0.2264(3) 0.3850(3) 0.0376(10) Uani 1 1 d U . . C28 C 0.7120(6) 0.2401(3) 0.4086(3) 0.0362(10) Uani 1 1 d U . . C29 C 0.8003(6) 0.2349(3) 0.3892(3) 0.0372(11) Uani 1 1 d U . . H29 H 0.8587 0.2440 0.4046 0.045 Uiso 1 1 calc R . . C30 C 0.8055(6) 0.2168(3) 0.3478(3) 0.0416(10) Uani 1 1 d U A . C31 C 0.7177(6) 0.2057(3) 0.3253(3) 0.0415(11) Uani 1 1 d U . . H31 H 0.7188 0.1948 0.2968 0.050 Uiso 1 1 calc R . . C32 C 0.6289(6) 0.2104(3) 0.3434(3) 0.0416(10) Uani 1 1 d U . . C33 C 0.5075(7) 0.1899(3) 0.4254(4) 0.0468(19) Uani 1 1 d U . . H33A H 0.4957 0.1640 0.4046 0.070 Uiso 1 1 calc R . . H33B H 0.4475 0.1969 0.4392 0.070 Uiso 1 1 calc R . . H33C H 0.5581 0.1799 0.4468 0.070 Uiso 1 1 calc R . . C34 C 0.9027(6) 0.2109(3) 0.3272(3) 0.0470(12) Uani 1 1 d DU . . C35A C 0.9645(12) 0.1793(6) 0.3589(6) 0.049(2) Uani 0.525(9) 1 d PDU A 1 H35A H 1.0296 0.1751 0.3487 0.074 Uiso 0.525(9) 1 calc PR A 1 H35B H 0.9336 0.1476 0.3614 0.074 Uiso 0.525(9) 1 calc PR A 1 H35C H 0.9696 0.1951 0.3867 0.074 Uiso 0.525(9) 1 calc PR A 1 C36A C 0.9491(12) 0.2603(5) 0.3251(7) 0.051(2) Uani 0.525(9) 1 d PDU A 1 H36A H 1.0189 0.2567 0.3218 0.076 Uiso 0.525(9) 1 calc PR A 1 H36B H 0.9392 0.2780 0.3514 0.076 Uiso 0.525(9) 1 calc PR A 1 H36C H 0.9194 0.2783 0.3009 0.076 Uiso 0.525(9) 1 calc PR A 1 C37A C 0.8911(13) 0.1814(7) 0.2863(5) 0.051(2) Uani 0.525(9) 1 d PDU A 1 H37A H 0.8573 0.2008 0.2639 0.076 Uiso 0.525(9) 1 calc PR A 1 H37B H 0.8533 0.1522 0.2912 0.076 Uiso 0.525(9) 1 calc PR A 1 H37C H 0.9553 0.1722 0.2774 0.076 Uiso 0.525(9) 1 calc PR A 1 C35B C 0.9898(11) 0.2334(8) 0.3526(7) 0.050(2) Uani 0.475(9) 1 d PDU A 2 H35D H 1.0483 0.2294 0.3369 0.076 Uiso 0.475(9) 1 calc PR A 2 H35E H 0.9989 0.2174 0.3802 0.076 Uiso 0.475(9) 1 calc PR A 2 H35F H 0.9777 0.2679 0.3568 0.076 Uiso 0.475(9) 1 calc PR A 2 C36B C 0.9033(14) 0.2418(7) 0.2863(5) 0.050(2) Uani 0.475(9) 1 d PDU A 2 H36D H 0.8906 0.2756 0.2932 0.075 Uiso 0.475(9) 1 calc PR A 2 H36E H 0.8528 0.2301 0.2656 0.075 Uiso 0.475(9) 1 calc PR A 2 H36F H 0.9668 0.2392 0.2743 0.075 Uiso 0.475(9) 1 calc PR A 2 C37B C 0.9241(14) 0.1590(5) 0.3153(8) 0.050(2) Uani 0.475(9) 1 d PDU A 2 H37D H 0.9906 0.1567 0.3063 0.075 Uiso 0.475(9) 1 calc PR A 2 H37E H 0.8783 0.1487 0.2920 0.075 Uiso 0.475(9) 1 calc PR A 2 H37F H 0.9172 0.1380 0.3400 0.075 Uiso 0.475(9) 1 calc PR A 2 C38 C 0.5350(6) 0.2037(3) 0.3178(3) 0.0455(13) Uani 1 1 d U . . H38A H 0.4869 0.1878 0.3352 0.055 Uiso 1 1 calc R . . H38B H 0.5448 0.1832 0.2928 0.055 Uiso 1 1 calc R . . C39 C 0.7047(6) 0.2621(3) 0.4509(3) 0.0376(12) Uani 1 1 d U . . H39A H 0.7706 0.2651 0.4651 0.045 Uiso 1 1 calc R . . H39B H 0.6664 0.2406 0.4685 0.045 Uiso 1 1 calc R . . C40 C 0.6703(5) 0.3989(3) 0.3618(2) 0.0234(9) Uani 1 1 d U . . C41 C 0.7204(5) 0.4036(3) 0.4008(2) 0.0228(9) Uani 1 1 d U . . C42 C 0.7342(5) 0.4501(3) 0.4178(3) 0.0249(10) Uani 1 1 d U . . H42 H 0.7688 0.4538 0.4446 0.030 Uiso 1 1 calc R . . C43 C 0.6988(5) 0.4906(3) 0.3967(3) 0.0282(9) Uani 1 1 d U . . C44 C 0.6452(5) 0.4842(3) 0.3584(3) 0.0268(10) Uani 1 1 d U . . H44 H 0.6192 0.5117 0.3438 0.032 Uiso 1 1 calc R . . C45 C 0.6283(5) 0.4384(3) 0.3405(2) 0.0252(9) Uani 1 1 d U . . C46 C 0.7261(6) 0.3404(3) 0.3150(3) 0.0354(16) Uani 1 1 d U . . H46A H 0.7241 0.3635 0.2915 0.053 Uiso 1 1 calc R . . H46B H 0.7120 0.3079 0.3039 0.053 Uiso 1 1 calc R . . H46C H 0.7908 0.3407 0.3297 0.053 Uiso 1 1 calc R . . C47 C 0.7184(6) 0.5426(3) 0.4139(3) 0.0359(11) Uani 1 1 d U . . C48 C 0.7728(7) 0.5421(3) 0.4578(3) 0.0469(18) Uani 1 1 d U . . H48A H 0.8356 0.5260 0.4559 0.070 Uiso 1 1 calc R . . H48B H 0.7343 0.5245 0.4778 0.070 Uiso 1 1 calc R . . H48C H 0.7832 0.5753 0.4677 0.070 Uiso 1 1 calc R . . C49 C 0.6232(6) 0.5699(3) 0.4170(3) 0.0424(17) Uani 1 1 d U . . H49A H 0.6369 0.6033 0.4258 0.064 Uiso 1 1 calc R . . H49B H 0.5845 0.5541 0.4380 0.064 Uiso 1 1 calc R . . H49C H 0.5870 0.5697 0.3893 0.064 Uiso 1 1 calc R . . C50 C 0.7805(7) 0.5684(3) 0.3827(4) 0.0463(17) Uani 1 1 d U . . H50A H 0.7472 0.5679 0.3543 0.070 Uiso 1 1 calc R . . H50B H 0.8433 0.5520 0.3819 0.070 Uiso 1 1 calc R . . H50C H 0.7910 0.6020 0.3917 0.070 Uiso 1 1 calc R . . C51 C 0.7549(5) 0.3596(3) 0.4244(2) 0.0254(11) Uani 1 1 d U . . H51A H 0.8030 0.3687 0.4477 0.030 Uiso 1 1 calc R . . H51B H 0.7869 0.3374 0.4050 0.030 Uiso 1 1 calc R . . C52 C 0.5622(6) 0.4320(3) 0.3021(3) 0.0279(10) Uani 1 1 d U . . H52A H 0.5931 0.4104 0.2818 0.033 Uiso 1 1 calc R . . H52B H 0.5505 0.4637 0.2881 0.033 Uiso 1 1 calc R . . C53 C 0.7168(6) 0.2452(3) 0.6385(3) 0.0371(10) Uani 1 1 d U . . C54 C 0.6851(6) 0.2829(3) 0.6639(3) 0.0408(10) Uani 1 1 d U . . C55 C 0.6957(6) 0.3306(3) 0.6488(3) 0.0401(11) Uani 1 1 d U . . H55 H 0.6763 0.3568 0.6658 0.048 Uiso 1 1 calc R . . C56 C 0.7336(6) 0.3403(3) 0.6099(3) 0.0388(10) Uani 1 1 d U . . C57 C 0.7580(6) 0.3015(3) 0.5843(3) 0.0354(11) Uani 1 1 d U . . H57 H 0.7810 0.3074 0.5570 0.042 Uiso 1 1 calc R . . C58 C 0.7488(6) 0.2540(3) 0.5986(3) 0.0353(10) Uani 1 1 d U . . C59 C 0.7914(7) 0.1816(4) 0.6782(4) 0.054(2) Uani 1 1 d U . . H59A H 0.8482 0.1822 0.6611 0.081 Uiso 1 1 calc R . . H59B H 0.7803 0.1485 0.6879 0.081 Uiso 1 1 calc R . . H59C H 0.8028 0.2029 0.7029 0.081 Uiso 1 1 calc R . . C60 C 0.7468(7) 0.3932(3) 0.5951(4) 0.0439(12) Uani 1 1 d U . . C61 C 0.8080(7) 0.4194(3) 0.6300(4) 0.0529(19) Uani 1 1 d U . . H61A H 0.8720 0.4041 0.6337 0.079 Uiso 1 1 calc R . . H61B H 0.7755 0.4175 0.6566 0.079 Uiso 1 1 calc R . . H61C H 0.8157 0.4533 0.6220 0.079 Uiso 1 1 calc R . . C62 C 0.6474(7) 0.4176(3) 0.5903(4) 0.0507(19) Uani 1 1 d U . . H62A H 0.6140 0.4134 0.6166 0.076 Uiso 1 1 calc R . . H62B H 0.6087 0.4029 0.5666 0.076 Uiso 1 1 calc R . . H62C H 0.6557 0.4522 0.5848 0.076 Uiso 1 1 calc R . . C63 C 0.7963(8) 0.3968(3) 0.5533(4) 0.0530(18) Uani 1 1 d U . . H63A H 0.8026 0.4309 0.5454 0.080 Uiso 1 1 calc R . . H63B H 0.7572 0.3798 0.5310 0.080 Uiso 1 1 calc R . . H63C H 0.8609 0.3821 0.5567 0.080 Uiso 1 1 calc R . . C64 C 0.6305(7) 0.2708(4) 0.7020(3) 0.0469(12) Uani 1 1 d U . . H64A H 0.6235 0.3001 0.7196 0.056 Uiso 1 1 calc R . . H64B H 0.6667 0.2462 0.7195 0.056 Uiso 1 1 calc R . . C65 C 0.7628(6) 0.2126(3) 0.5692(3) 0.0375(12) Uani 1 1 d U . . H65A H 0.7992 0.1863 0.5843 0.045 Uiso 1 1 calc R . . H65B H 0.8001 0.2232 0.5450 0.045 Uiso 1 1 calc R . . C66 C 0.6465(7) 0.0767(3) 0.5890(4) 0.0506(11) Uani 1 1 d U . . C67 C 0.6747(7) 0.0571(4) 0.6284(4) 0.0567(11) Uani 1 1 d U . . C68 C 0.7754(8) 0.0529(4) 0.6385(4) 0.0602(13) Uani 1 1 d U . . H68 H 0.7974 0.0384 0.6647 0.072 Uiso 1 1 calc R . . C69 C 0.8433(8) 0.0693(4) 0.6112(5) 0.0634(12) Uani 1 1 d U . . C70 C 0.8117(8) 0.0911(4) 0.5733(4) 0.0580(13) Uani 1 1 d U . . H70 H 0.8584 0.1025 0.5548 0.070 Uiso 1 1 calc R . . C71 C 0.7121(7) 0.0969(4) 0.5614(4) 0.0524(11) Uani 1 1 d U . . C72 C 0.5132(7) 0.0413(4) 0.5518(4) 0.053(2) Uani 1 1 d U . . H72A H 0.5362 0.0445 0.5233 0.080 Uiso 1 1 calc R . . H72B H 0.4421 0.0414 0.5502 0.080 Uiso 1 1 calc R . . H72C H 0.5370 0.0108 0.5645 0.080 Uiso 1 1 calc R . . C73 C 0.9527(8) 0.0610(4) 0.6216(5) 0.0699(15) Uani 1 1 d U . . C74 C 0.9753(10) 0.0380(5) 0.6642(5) 0.083(2) Uani 1 1 d U . . H74A H 0.9532 0.0592 0.6865 0.124 Uiso 1 1 calc R . . H74B H 1.0456 0.0330 0.6686 0.124 Uiso 1 1 calc R . . H74C H 0.9420 0.0068 0.6653 0.124 Uiso 1 1 calc R . . C75 C 1.0056(8) 0.1098(4) 0.6215(5) 0.072(2) Uani 1 1 d U . . H75A H 0.9864 0.1274 0.5954 0.108 Uiso 1 1 calc R . . H75B H 1.0759 0.1044 0.6231 0.108 Uiso 1 1 calc R . . H75C H 0.9883 0.1289 0.6461 0.108 Uiso 1 1 calc R . . C76 C 0.9914(9) 0.0284(5) 0.5894(5) 0.080(2) Uani 1 1 d U . . H76A H 1.0605 0.0223 0.5966 0.121 Uiso 1 1 calc R . . H76B H 0.9835 0.0436 0.5613 0.121 Uiso 1 1 calc R . . H76C H 0.9558 -0.0023 0.5890 0.121 Uiso 1 1 calc R . . C77 C 0.6774(7) 0.1278(3) 0.5263(4) 0.0501(12) Uani 1 1 d U . . H77A H 0.6232 0.1117 0.5098 0.060 Uiso 1 1 calc R . . H77B H 0.7304 0.1336 0.5072 0.060 Uiso 1 1 calc R . . C78 C 0.6010(7) 0.0444(4) 0.6597(4) 0.0567(13) Uani 1 1 d U . . H78A H 0.6314 0.0242 0.6827 0.068 Uiso 1 1 calc R . . H78B H 0.5469 0.0259 0.6453 0.068 Uiso 1 1 calc R . . C79 C 0.3225(6) 0.1026(3) 0.6356(3) 0.0312(9) Uani 1 1 d U . . C80 C 0.3631(6) 0.0656(3) 0.6607(3) 0.0388(10) Uani 1 1 d U . . C81 C 0.3470(7) 0.0180(3) 0.6458(3) 0.0441(12) Uani 1 1 d U . . H81 H 0.3743 -0.0079 0.6623 0.053 Uiso 1 1 calc R . . C82 C 0.2934(7) 0.0071(3) 0.6084(4) 0.0469(11) Uani 1 1 d U . . C83 C 0.2592(6) 0.0448(3) 0.5845(3) 0.0388(11) Uani 1 1 d U . . H83 H 0.2241 0.0385 0.5583 0.047 Uiso 1 1 calc R . . C84 C 0.2740(6) 0.0927(3) 0.5973(3) 0.0327(10) Uani 1 1 d U . . C85 C 0.2646(7) 0.1678(3) 0.6745(3) 0.0434(18) Uani 1 1 d U . . H85A H 0.2011 0.1660 0.6588 0.065 Uiso 1 1 calc R . . H85B H 0.2788 0.2015 0.6823 0.065 Uiso 1 1 calc R . . H85C H 0.2636 0.1481 0.7003 0.065 Uiso 1 1 calc R . . C86 C 0.2708(8) -0.0458(4) 0.5946(4) 0.0589(14) Uani 1 1 d U . . C87 C 0.3666(8) -0.0732(4) 0.5916(5) 0.070(2) Uani 1 1 d U . . H87A H 0.4034 -0.0723 0.6192 0.105 Uiso 1 1 calc R . . H87B H 0.4047 -0.0580 0.5701 0.105 Uiso 1 1 calc R . . H87C H 0.3529 -0.1069 0.5836 0.105 Uiso 1 1 calc R . . C88 C 0.2105(9) -0.0687(4) 0.6270(5) 0.072(2) Uani 1 1 d U . . H88A H 0.1963 -0.1023 0.6189 0.109 Uiso 1 1 calc R . . H88B H 0.1495 -0.0508 0.6284 0.109 Uiso 1 1 calc R . . H88C H 0.2463 -0.0680 0.6548 0.109 Uiso 1 1 calc R . . C89 C 0.2135(9) -0.0491(4) 0.5513(4) 0.071(2) Uani 1 1 d U . . H89A H 0.2479 -0.0312 0.5301 0.107 Uiso 1 1 calc R . . H89B H 0.1487 -0.0351 0.5535 0.107 Uiso 1 1 calc R . . H89C H 0.2072 -0.0830 0.5427 0.107 Uiso 1 1 calc R . . C90 C 0.4270(7) 0.0764(3) 0.6984(3) 0.0443(12) Uani 1 1 d U . . H90A H 0.4401 0.0463 0.7147 0.053 Uiso 1 1 calc R . . H90B H 0.3938 0.0992 0.7168 0.053 Uiso 1 1 calc R . . C91 C 0.2404(6) 0.1341(3) 0.5691(3) 0.0350(12) Uani 1 1 d U . . H91A H 0.2081 0.1588 0.5860 0.042 Uiso 1 1 calc R . . H91B H 0.1928 0.1223 0.5466 0.042 Uiso 1 1 calc R . . C92 C 0.3651(7) 0.2727(3) 0.5933(4) 0.0481(11) Uani 1 1 d U . . C93 C 0.3614(7) 0.2943(4) 0.6327(4) 0.0534(11) Uani 1 1 d U . . C94 C 0.2710(7) 0.3015(4) 0.6491(4) 0.0559(13) Uani 1 1 d U . . H94 H 0.2684 0.3180 0.6754 0.067 Uiso 1 1 calc R . . C95 C 0.1862(7) 0.2858(4) 0.6291(4) 0.0579(12) Uani 1 1 d U . . C96 C 0.1935(7) 0.2620(3) 0.5904(4) 0.0524(12) Uani 1 1 d U . . H96 H 0.1359 0.2502 0.5757 0.063 Uiso 1 1 calc R . . C97 C 0.2823(7) 0.2548(3) 0.5725(4) 0.0490(11) Uani 1 1 d U . . C98 C 0.4930(7) 0.3035(3) 0.5539(4) 0.049(2) Uani 1 1 d U . . H98A H 0.4511 0.3097 0.5282 0.073 Uiso 1 1 calc R . . H98B H 0.5588 0.2958 0.5459 0.073 Uiso 1 1 calc R . . H98C H 0.4951 0.3322 0.5720 0.073 Uiso 1 1 calc R . . C99 C 0.0855(8) 0.2944(4) 0.6471(5) 0.0666(15) Uani 1 1 d U . . C100 C 0.0895(9) 0.3253(5) 0.6846(5) 0.078(2) Uani 1 1 d U . . H10D H 0.0233 0.3323 0.6925 0.118 Uiso 1 1 calc R . . H10E H 0.1224 0.3556 0.6784 0.118 Uiso 1 1 calc R . . H10F H 0.1253 0.3088 0.7082 0.118 Uiso 1 1 calc R . . C101 C 0.0213(8) 0.3216(5) 0.6120(5) 0.079(2) Uani 1 1 d U . . H10G H -0.0447 0.3253 0.6213 0.119 Uiso 1 1 calc R . . H10H H 0.0192 0.3029 0.5856 0.119 Uiso 1 1 calc R . . H10I H 0.0492 0.3535 0.6071 0.119 Uiso 1 1 calc R . . C102 C 0.0382(8) 0.2465(4) 0.6542(5) 0.078(2) Uani 1 1 d U . . H10J H 0.0681 0.2315 0.6800 0.116 Uiso 1 1 calc R . . H10K H 0.0469 0.2254 0.6298 0.116 Uiso 1 1 calc R . . H10L H -0.0313 0.2513 0.6575 0.116 Uiso 1 1 calc R . . C103 C 0.2915(7) 0.2272(4) 0.5330(4) 0.0503(13) Uani 1 1 d U . . H10M H 0.3311 0.2461 0.5138 0.060 Uiso 1 1 calc R . . H10N H 0.2263 0.2228 0.5187 0.060 Uiso 1 1 calc R . . C104 C 0.4533(7) 0.3066(4) 0.6574(4) 0.0556(14) Uani 1 1 d U . . H10O H 0.4414 0.3307 0.6797 0.067 Uiso 1 1 calc R . . H10P H 0.5011 0.3201 0.6385 0.067 Uiso 1 1 calc R . . O1 O 0.4444(4) 0.4132(2) 0.42405(19) 0.0336(10) Uani 1 1 d U . . O2 O 0.2788(4) 0.3084(2) 0.3359(2) 0.0386(11) Uani 1 1 d U . . O3 O 0.5385(4) 0.2325(2) 0.4043(2) 0.0382(10) Uani 1 1 d U . . O4 O 0.6555(4) 0.35338(18) 0.34397(17) 0.0265(9) Uani 1 1 d U . . O5 O 0.7081(4) 0.1980(2) 0.6531(2) 0.0405(11) Uani 1 1 d U . . O6 O 0.5488(4) 0.0808(2) 0.5776(2) 0.0471(12) Uani 1 1 d U . . O7 O 0.3380(4) 0.1500(2) 0.64841(18) 0.0316(10) Uani 1 1 d U . . O8 O 0.4554(4) 0.2637(2) 0.5764(2) 0.0462(12) Uani 1 1 d U . . S1A S 0.9967(3) 0.27910(18) 0.48422(15) 0.0654(11) Uani 0.643(4) 1 d PDU B 1 C10A C 0.9976(7) 0.2151(3) 0.4976(3) 0.0559(13) Uani 0.643(4) 1 d PDU B 1 O9A O 0.9915(7) 0.2830(4) 0.4397(3) 0.061(2) Uani 0.643(4) 1 d PDU B 1 O10A O 0.9148(6) 0.2972(4) 0.5052(3) 0.061(2) Uani 0.643(4) 1 d PDU B 1 O11A O 1.0841(6) 0.2984(4) 0.5046(3) 0.058(2) Uani 0.643(4) 1 d PDU B 1 F1A F 1.0725(6) 0.1938(4) 0.4802(3) 0.0656(15) Uani 0.643(4) 1 d PDU B 1 F2A F 0.9152(6) 0.1945(4) 0.4798(3) 0.0618(15) Uani 0.643(4) 1 d PDU B 1 F3A F 0.9962(7) 0.2069(4) 0.5382(3) 0.0649(17) Uani 0.643(4) 1 d PDU B 1 S1B S 0.9759(5) 0.1919(3) 0.4951(2) 0.0579(12) Uani 0.357(4) 1 d PDU B 2 C10B C 1.0268(9) 0.1372(4) 0.4726(4) 0.068(2) Uani 0.357(4) 1 d PDU B 2 F1B F 0.9938(11) 0.1298(7) 0.4326(4) 0.074(3) Uani 0.357(4) 1 d PDU B 2 F2B F 1.1226(8) 0.1412(6) 0.4727(5) 0.068(2) Uani 0.357(4) 1 d PDU B 2 F3B F 1.0071(12) 0.0979(5) 0.4943(5) 0.073(3) Uani 0.357(4) 1 d PDU B 2 O9B O 0.8726(7) 0.1813(7) 0.4876(6) 0.060(2) Uani 0.357(4) 1 d PDU B 2 O10B O 1.0144(14) 0.1902(8) 0.5379(4) 0.060(2) Uani 0.357(4) 1 d PDU B 2 O11B O 1.0101(12) 0.2286(6) 0.4682(5) 0.0629(16) Uani 0.357(4) 1 d PDU B 2 S2A S 0.4909(4) 0.42198(17) 0.73444(17) 0.0586(11) Uani 0.591(4) 1 d PDU C 1 O12A O 0.5066(13) 0.4300(6) 0.6898(3) 0.0597(17) Uani 0.591(4) 1 d PDU C 1 O13A O 0.4504(10) 0.3759(3) 0.7443(4) 0.0617(18) Uani 0.591(4) 1 d PDU C 1 O14A O 0.4496(10) 0.4630(3) 0.7550(4) 0.0648(17) Uani 0.591(4) 1 d PDU C 1 C11A C 0.6126(7) 0.4199(4) 0.7589(3) 0.0603(14) Uani 0.591(4) 1 d PDU C 1 F4A F 0.6580(8) 0.4617(3) 0.7549(3) 0.0622(18) Uani 0.591(4) 1 d PDU C 1 F5A F 0.6642(8) 0.3853(3) 0.7425(3) 0.0625(18) Uani 0.591(4) 1 d PDU C 1 F6A F 0.6093(9) 0.4101(4) 0.8000(3) 0.070(2) Uani 0.591(4) 1 d PDU C 1 S2B S 0.5368(6) 0.4282(2) 0.7295(2) 0.0575(12) Uani 0.409(4) 1 d PDU C 2 O14B O 0.5751(13) 0.4734(4) 0.7457(5) 0.0598(19) Uani 0.409(4) 1 d PDU C 2 O13B O 0.5842(12) 0.3854(4) 0.7470(5) 0.0608(18) Uani 0.409(4) 1 d PDU C 2 O12B O 0.5150(18) 0.4264(9) 0.6845(3) 0.0590(18) Uani 0.409(4) 1 d PDU C 2 C11B C 0.4208(8) 0.4251(4) 0.7534(4) 0.0635(15) Uani 0.409(4) 1 d PDU C 2 F4B F 0.3627(11) 0.4612(4) 0.7407(5) 0.068(2) Uani 0.409(4) 1 d PDU C 2 F5B F 0.3738(11) 0.3848(4) 0.7425(5) 0.068(2) Uani 0.409(4) 1 d PDU C 2 F6B F 0.4360(12) 0.4256(5) 0.7949(3) 0.069(2) Uani 0.409(4) 1 d PDU C 2 Se1 Se 0.43771(6) 0.40397(3) 0.31687(3) 0.02842(19) Uani 1 1 d U . . Se2 Se 0.35810(6) 0.30154(3) 0.43991(3) 0.0335(2) Uani 1 1 d U . . Se3 Se 0.48823(7) 0.26745(4) 0.29963(3) 0.0404(2) Uani 1 1 d U . . Se4 Se 0.64315(6) 0.32677(3) 0.44808(3) 0.0321(2) Uani 1 1 d U . . Se5 Se 0.50103(7) 0.24562(4) 0.68299(3) 0.0447(2) Uani 1 1 d U . . Se6 Se 0.63293(7) 0.18961(3) 0.54842(3) 0.0357(2) Uani 1 1 d U . . Se7 Se 0.55134(7) 0.10487(4) 0.68325(3) 0.0436(3) Uani 1 1 d U . . Se8 Se 0.35248(7) 0.16301(4) 0.54313(3) 0.0390(2) Uani 1 1 d U . . Ag1 Ag 0.47053(5) 0.32557(2) 0.37331(2) 0.03324(15) Uani 1 1 d U . . Ag2 Ag 0.51959(5) 0.17578(2) 0.61750(2) 0.03595(16) Uani 1 1 d U . . 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 C1 0.0222(18) 0.029(2) 0.050(2) -0.0040(17) -0.0008(16) 0.0022(17) C2 0.0264(19) 0.035(2) 0.054(2) -0.0031(18) 0.0060(18) 0.0019(17) C3 0.0252(19) 0.034(2) 0.063(3) -0.005(2) 0.005(2) -0.001(2) C4 0.0244(18) 0.033(2) 0.069(3) -0.004(2) -0.0020(18) -0.0007(18) C5 0.0230(19) 0.027(2) 0.061(3) -0.003(2) -0.0071(19) -0.001(2) C6 0.0224(18) 0.026(2) 0.054(2) -0.0021(17) -0.0058(16) -0.0007(17) C7 0.028(3) 0.047(4) 0.051(4) -0.013(3) -0.001(3) -0.001(3) C8 0.025(2) 0.039(3) 0.083(3) -0.006(2) -0.004(2) 0.000(2) C9 0.031(4) 0.050(4) 0.099(4) -0.015(4) 0.001(4) 0.007(3) C10 0.026(3) 0.043(3) 0.096(5) -0.008(3) -0.001(4) -0.004(3) C11 0.030(4) 0.053(4) 0.095(4) 0.005(4) -0.014(4) 0.001(3) C12 0.023(2) 0.027(2) 0.053(3) 0.001(2) -0.007(2) -0.001(2) C13 0.032(3) 0.042(3) 0.052(3) 0.0009(18) 0.012(2) 0.003(2) C14 0.026(2) 0.0353(18) 0.068(2) -0.0051(17) -0.0101(18) -0.0018(18) C15 0.029(2) 0.039(2) 0.075(2) 0.0051(17) -0.0062(19) -0.0029(19) C16 0.038(2) 0.042(2) 0.089(3) 0.006(2) -0.011(2) -0.004(2) C17 0.049(2) 0.047(2) 0.102(3) -0.005(2) -0.017(2) -0.002(2) C18 0.041(2) 0.043(2) 0.092(3) -0.017(2) -0.018(2) 0.000(2) C19 0.0332(19) 0.042(2) 0.077(2) -0.0178(19) -0.0160(19) -0.0001(18) C20 0.030(3) 0.041(3) 0.060(4) -0.002(3) -0.010(3) 0.002(3) C21 0.066(3) 0.050(2) 0.120(3) -0.001(2) -0.019(3) -0.003(3) C22 0.092(5) 0.068(5) 0.132(4) 0.015(4) -0.008(4) -0.009(4) C23 0.078(4) 0.059(4) 0.137(6) 0.003(5) -0.028(4) 0.007(4) C24 0.078(5) 0.056(4) 0.138(5) -0.009(4) -0.025(4) -0.011(4) C25 0.027(2) 0.040(3) 0.068(3) 0.010(2) 0.001(2) -0.004(2) C26 0.034(2) 0.049(3) 0.072(3) -0.023(2) -0.015(2) 0.002(2) C27 0.0231(18) 0.028(2) 0.061(2) 0.0000(19) -0.0012(17) 0.0028(18) C28 0.0241(18) 0.028(2) 0.056(2) 0.0076(18) -0.0037(18) 0.0029(18) C29 0.0233(19) 0.030(2) 0.058(3) 0.006(2) -0.0042(19) 0.003(2) C30 0.0263(18) 0.034(2) 0.063(3) -0.001(2) -0.0012(19) 0.0040(19) C31 0.0274(19) 0.033(2) 0.063(3) -0.008(2) -0.0016(19) 0.004(2) C32 0.0263(18) 0.033(2) 0.065(2) -0.0094(19) -0.0018(17) 0.0023(18) C33 0.030(4) 0.033(4) 0.077(5) 0.010(3) 0.001(3) -0.001(3) C34 0.028(2) 0.043(3) 0.070(3) -0.003(2) 0.003(2) 0.004(2) C35A 0.026(3) 0.046(4) 0.076(4) -0.002(4) 0.003(4) 0.005(3) C36A 0.030(4) 0.047(4) 0.075(5) -0.002(3) 0.007(4) 0.000(3) C37A 0.031(4) 0.049(4) 0.073(4) -0.006(3) 0.006(3) 0.004(4) C35B 0.028(3) 0.049(4) 0.074(4) -0.002(4) 0.004(3) 0.000(3) C36B 0.031(4) 0.048(4) 0.072(4) -0.001(3) 0.006(3) 0.005(4) C37B 0.029(4) 0.046(3) 0.075(5) -0.004(3) 0.006(4) 0.006(3) C38 0.028(2) 0.040(2) 0.068(3) -0.018(2) -0.003(2) 0.001(2) C39 0.029(3) 0.032(2) 0.052(3) 0.011(2) -0.003(2) 0.000(2) C40 0.0209(19) 0.0228(17) 0.0259(19) -0.0020(15) -0.0039(16) -0.0027(16) C41 0.0170(19) 0.0247(17) 0.0262(19) -0.0019(15) -0.0033(16) -0.0018(16) C42 0.017(2) 0.0267(18) 0.031(2) -0.0061(17) -0.0036(19) 0.0003(18) C43 0.020(2) 0.0251(17) 0.039(2) -0.0071(17) -0.0035(18) 0.0006(17) C44 0.021(2) 0.0239(19) 0.034(2) -0.0014(18) -0.0033(19) -0.0003(19) C45 0.0222(18) 0.0241(18) 0.029(2) 0.0007(16) -0.0043(17) -0.0025(16) C46 0.035(4) 0.033(4) 0.038(4) -0.012(3) -0.002(3) 0.003(3) C47 0.026(2) 0.028(2) 0.053(3) -0.013(2) -0.004(2) 0.003(2) C48 0.039(4) 0.038(4) 0.062(3) -0.024(3) -0.016(3) 0.006(3) C49 0.029(3) 0.033(3) 0.064(5) -0.019(3) -0.005(3) 0.005(3) C50 0.035(4) 0.029(3) 0.075(4) -0.011(3) 0.004(3) -0.007(3) C51 0.019(2) 0.028(2) 0.028(3) 0.001(2) -0.004(2) -0.001(2) C52 0.028(2) 0.025(3) 0.029(3) 0.0036(18) -0.0067(18) -0.0041(19) C53 0.028(2) 0.0292(19) 0.053(2) 0.0003(17) -0.0012(18) -0.0071(18) C54 0.033(2) 0.034(2) 0.055(2) -0.0061(18) 0.0005(19) -0.0101(18) C55 0.030(2) 0.031(2) 0.059(3) -0.008(2) 0.001(2) -0.008(2) C56 0.026(2) 0.0277(18) 0.062(3) -0.0030(18) 0.002(2) -0.0044(18) C57 0.023(2) 0.0262(19) 0.057(3) 0.0007(18) 0.001(2) -0.002(2) C58 0.024(2) 0.0264(18) 0.056(2) 0.0013(17) 0.0029(18) -0.0023(17) C59 0.046(4) 0.045(4) 0.069(5) 0.016(4) -0.015(4) -0.008(3) C60 0.032(2) 0.027(2) 0.072(3) -0.002(2) 0.003(2) -0.003(2) C61 0.041(4) 0.029(3) 0.087(4) -0.004(4) -0.005(4) -0.007(3) C62 0.036(3) 0.033(3) 0.083(5) 0.003(4) 0.001(3) 0.001(3) C63 0.046(4) 0.032(4) 0.082(4) 0.005(3) 0.013(3) -0.009(3) C64 0.041(2) 0.043(3) 0.057(3) -0.008(2) 0.004(2) -0.013(2) C65 0.028(2) 0.027(2) 0.058(3) 0.002(2) 0.007(2) 0.001(2) C66 0.0371(19) 0.033(2) 0.081(2) -0.0044(19) 0.0028(18) -0.0032(18) C67 0.041(2) 0.037(2) 0.091(3) 0.0064(19) -0.0052(18) -0.0064(19) C68 0.042(2) 0.041(3) 0.096(3) 0.004(2) -0.004(2) -0.004(2) C69 0.044(2) 0.046(2) 0.100(3) -0.001(2) 0.003(2) -0.002(2) C70 0.041(2) 0.041(2) 0.092(3) -0.007(2) 0.009(2) -0.002(2) C71 0.039(2) 0.036(2) 0.083(3) -0.010(2) 0.0106(19) -0.0010(18) C72 0.044(4) 0.039(4) 0.076(5) -0.015(3) 0.005(3) -0.005(3) C73 0.046(2) 0.055(3) 0.108(3) 0.001(3) 0.002(2) -0.001(2) C74 0.057(4) 0.072(5) 0.117(4) 0.014(4) -0.007(4) -0.003(4) C75 0.045(4) 0.059(4) 0.111(5) 0.001(4) 0.002(4) -0.004(3) C76 0.051(4) 0.064(4) 0.126(5) -0.008(4) 0.006(4) 0.005(4) C77 0.039(3) 0.038(2) 0.075(3) -0.013(2) 0.018(2) -0.002(2) C78 0.040(3) 0.039(2) 0.089(3) 0.017(2) -0.009(2) -0.006(2) C79 0.028(2) 0.0282(18) 0.037(2) 0.0015(16) -0.0004(17) -0.0069(17) C80 0.035(2) 0.033(2) 0.048(2) 0.0113(18) -0.0014(18) -0.0090(18) C81 0.037(2) 0.031(2) 0.064(3) 0.008(2) 0.004(2) -0.006(2) C82 0.038(2) 0.0324(19) 0.071(3) -0.0046(19) 0.006(2) -0.0058(19) C83 0.031(2) 0.033(2) 0.053(3) -0.0088(19) 0.003(2) -0.007(2) C84 0.027(2) 0.0312(19) 0.040(2) -0.0031(16) -0.0009(18) -0.0067(18) C85 0.044(4) 0.040(4) 0.046(4) -0.013(3) 0.007(3) -0.007(3) C86 0.049(3) 0.035(2) 0.093(3) -0.010(2) 0.009(3) -0.005(2) C87 0.057(4) 0.039(4) 0.114(6) -0.014(4) 0.013(4) 0.001(3) C88 0.060(5) 0.040(4) 0.119(5) -0.006(4) 0.019(4) -0.017(4) C89 0.061(5) 0.047(5) 0.105(4) -0.030(4) 0.000(4) -0.006(4) C90 0.044(2) 0.040(3) 0.048(3) 0.020(2) -0.007(2) -0.012(2) C91 0.029(3) 0.037(2) 0.038(3) 0.000(2) -0.004(2) -0.006(2) C92 0.0297(19) 0.033(2) 0.082(3) 0.010(2) 0.0090(19) 0.0011(18) C93 0.0343(19) 0.035(2) 0.092(3) -0.003(2) 0.0138(19) -0.0016(19) C94 0.036(2) 0.036(3) 0.097(3) -0.003(2) 0.015(2) 0.000(2) C95 0.034(2) 0.039(2) 0.102(3) 0.001(2) 0.016(2) 0.000(2) C96 0.030(2) 0.037(3) 0.092(3) 0.009(2) 0.008(2) 0.001(2) C97 0.030(2) 0.036(2) 0.081(3) 0.014(2) 0.006(2) 0.0008(19) C98 0.028(4) 0.041(4) 0.077(5) 0.020(4) 0.001(3) -0.003(3) C99 0.038(2) 0.048(3) 0.115(4) -0.003(3) 0.022(3) 0.000(2) C100 0.049(5) 0.066(5) 0.123(5) -0.015(4) 0.031(4) -0.003(4) C101 0.045(4) 0.062(5) 0.133(5) -0.003(4) 0.015(4) 0.015(4) C102 0.047(4) 0.056(4) 0.133(6) -0.003(4) 0.034(5) -0.007(3) C103 0.033(3) 0.043(2) 0.075(3) 0.016(2) 0.004(3) -0.002(2) C104 0.035(2) 0.038(2) 0.094(4) -0.013(2) 0.015(2) -0.002(2) O1 0.0218(18) 0.033(2) 0.045(2) -0.0050(19) -0.0026(18) 0.0034(18) O2 0.024(2) 0.0337(19) 0.057(3) -0.0039(19) -0.007(2) -0.0017(19) O3 0.0236(19) 0.026(2) 0.064(3) 0.003(2) 0.0017(19) 0.0016(18) O4 0.026(2) 0.0236(18) 0.029(2) -0.0050(17) -0.0062(17) -0.0029(17) O5 0.034(2) 0.031(2) 0.055(3) 0.0062(19) -0.006(2) -0.008(2) O6 0.035(2) 0.032(2) 0.075(3) -0.008(2) 0.003(2) -0.003(2) O7 0.031(2) 0.0296(19) 0.034(2) -0.0028(18) -0.0021(19) -0.0060(18) O8 0.030(2) 0.033(2) 0.076(3) 0.015(2) 0.008(2) 0.002(2) S1A 0.0396(18) 0.084(2) 0.072(2) 0.012(2) 0.0002(18) 0.0045(17) C10A 0.027(3) 0.085(3) 0.055(3) 0.020(3) -0.001(2) 0.012(2) O9A 0.035(4) 0.079(5) 0.068(3) 0.023(3) -0.001(3) -0.004(4) O10A 0.031(3) 0.076(4) 0.074(5) 0.016(4) 0.001(3) 0.003(3) O11A 0.031(3) 0.083(4) 0.062(4) 0.008(4) 0.005(3) 0.008(3) F1A 0.039(3) 0.090(3) 0.067(3) 0.012(3) 0.003(3) 0.013(3) F2A 0.038(3) 0.088(3) 0.060(3) 0.015(3) 0.004(3) 0.002(3) F3A 0.037(3) 0.096(4) 0.061(3) 0.019(3) -0.002(2) 0.012(3) S1B 0.032(2) 0.092(3) 0.050(2) 0.022(2) 0.000(2) 0.020(2) C10B 0.042(4) 0.092(4) 0.069(4) 0.005(4) -0.003(4) 0.013(4) F1B 0.048(6) 0.101(6) 0.071(5) 0.000(4) -0.006(5) 0.007(6) F2B 0.040(4) 0.095(5) 0.069(5) 0.001(5) -0.001(4) 0.017(4) F3B 0.053(6) 0.089(4) 0.077(6) 0.005(5) -0.005(6) 0.009(5) O9B 0.035(3) 0.091(5) 0.052(5) 0.017(4) 0.000(3) 0.010(3) O10B 0.032(4) 0.091(4) 0.057(3) 0.016(3) -0.003(3) 0.018(4) O11B 0.038(3) 0.089(3) 0.061(3) 0.016(3) 0.002(3) 0.008(3) S2A 0.098(3) 0.0321(16) 0.0441(18) 0.0059(14) -0.007(2) 0.0028(19) O12A 0.102(4) 0.036(3) 0.039(2) 0.005(3) -0.010(3) 0.002(3) O13A 0.099(4) 0.036(3) 0.049(4) 0.009(3) -0.006(4) 0.000(3) O14A 0.104(4) 0.039(3) 0.051(3) 0.002(3) 0.002(3) 0.002(3) C11A 0.102(3) 0.036(2) 0.041(2) 0.000(2) -0.011(3) 0.000(2) F4A 0.100(4) 0.038(3) 0.047(4) -0.004(3) -0.006(4) -0.002(3) F5A 0.097(4) 0.038(3) 0.050(4) -0.003(3) -0.017(4) 0.002(3) F6A 0.116(6) 0.051(4) 0.040(3) -0.001(3) -0.015(3) -0.010(4) S2B 0.100(3) 0.0328(19) 0.0384(19) 0.0014(17) -0.009(2) 0.003(2) O14B 0.101(4) 0.035(3) 0.042(4) 0.000(3) -0.009(4) 0.001(3) O13B 0.101(4) 0.035(3) 0.044(3) 0.003(3) -0.011(3) 0.004(3) O12B 0.101(4) 0.036(4) 0.038(2) 0.002(3) -0.008(3) 0.002(4) C11B 0.103(3) 0.037(3) 0.050(3) 0.005(3) 0.000(3) 0.001(2) F4B 0.104(4) 0.043(3) 0.057(4) 0.006(4) 0.005(4) 0.004(4) F5B 0.107(5) 0.041(3) 0.056(4) 0.005(4) 0.000(4) -0.003(4) F6B 0.112(5) 0.045(4) 0.051(3) 0.003(3) 0.003(3) -0.001(4) Se1 0.0252(4) 0.0301(4) 0.0278(4) 0.0030(3) -0.0146(3) -0.0040(3) Se2 0.0286(4) 0.0375(5) 0.0348(5) 0.0125(4) 0.0060(4) 0.0036(4) Se3 0.0317(5) 0.0530(6) 0.0349(5) -0.0248(4) -0.0106(4) 0.0045(4) Se4 0.0285(4) 0.0347(5) 0.0334(5) 0.0066(4) 0.0041(4) -0.0022(3) Se5 0.0420(5) 0.0517(6) 0.0413(6) -0.0140(4) 0.0102(4) -0.0181(4) Se6 0.0376(5) 0.0319(5) 0.0386(5) -0.0030(4) 0.0109(4) -0.0072(4) Se7 0.0408(5) 0.0431(5) 0.0437(6) 0.0240(4) -0.0223(4) -0.0129(4) Se8 0.0390(5) 0.0487(6) 0.0292(5) 0.0060(4) 0.0022(4) -0.0016(4) Ag1 0.0402(3) 0.0271(3) 0.0334(3) 0.0015(2) 0.0104(3) -0.0014(2) Ag2 0.0437(4) 0.0285(3) 0.0370(3) 0.0042(2) 0.0129(3) -0.0016(3) _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 C1 C6 1.377(13) . ? C1 C2 1.393(12) . ? C1 O1 1.400(9) . ? C2 C3 1.405(12) . ? C2 C13 1.480(13) . ? C3 C4 1.397(14) . ? C3 H3 0.9500 . ? C4 C5 1.383(13) . ? C4 C8 1.536(12) . ? C5 C6 1.400(11) . ? C5 H5 0.9500 . ? C6 C12 1.493(12) . ? C7 O1 1.430(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.495(15) . ? C8 C11 1.528(16) . ? C8 C10 1.532(13) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Se1 1.985(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 Se2 1.972(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O2 1.378(11) . ? C14 C15 1.386(15) . ? C14 C19 1.414(14) . ? C15 C16 1.399(14) . ? C15 C25 1.499(15) . ? C16 C17 1.419(17) . ? C16 H16 0.9500 . ? C17 C18 1.364(18) . ? C17 C21 1.576(17) . ? C18 C19 1.393(15) . ? C18 H18 0.9500 . ? C19 C26 1.473(16) . ? C20 O2 1.420(10) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C24 1.453(19) . ? C21 C22 1.47(2) . ? C21 C23 1.512(18) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 Se2 1.965(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 Se3 1.976(9) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C32 1.389(14) . ? C27 C28 1.403(12) . ? C27 O3 1.406(10) . ? C28 C29 1.405(12) . ? C28 C39 1.479(13) . ? C29 C30 1.404(14) . ? C29 H29 0.9500 . ? C30 C31 1.398(12) . ? C30 C34 1.538(12) . ? C31 C32 1.392(13) . ? C31 H31 0.9500 . ? C32 C38 1.493(12) . ? C33 O3 1.433(11) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36A 1.513(9) . ? C34 C37B 1.519(10) . ? C34 C37A 1.528(10) . ? C34 C35B 1.533(10) . ? C34 C35A 1.545(9) . ? C34 C36B 1.547(10) . ? C35A H35A 0.9800 . ? C35A H35B 0.9800 . ? C35A H35C 0.9800 . ? C36A H36A 0.9800 . ? C36A H36B 0.9800 . ? C36A H36C 0.9800 . ? C37A H37A 0.9800 . ? C37A H37B 0.9800 . ? C37A H37C 0.9800 . ? C35B H35D 0.9800 . ? C35B H35E 0.9800 . ? C35B H35F 0.9800 . ? C36B H36D 0.9800 . ? C36B H36E 0.9800 . ? C36B H36F 0.9800 . ? C37B H37D 0.9800 . ? C37B H37E 0.9800 . ? C37B H37F 0.9800 . ? C38 Se3 1.951(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 Se4 1.980(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.380(10) . ? C40 O4 1.388(9) . ? C40 C45 1.391(10) . ? C41 C42 1.403(10) . ? C41 C51 1.490(10) . ? C42 C43 1.377(11) . ? C42 H42 0.9500 . ? C43 C44 1.387(11) . ? C43 C47 1.557(11) . ? C44 C45 1.401(11) . ? C44 H44 0.9500 . ? C45 C52 1.481(10) . ? C46 O4 1.425(10) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C49 1.523(11) . ? C47 C50 1.525(13) . ? C47 C48 1.531(13) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 Se4 1.977(7) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 Se1 1.969(8) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C58 1.384(13) . ? C53 O5 1.393(10) . ? C53 C54 1.402(13) . ? C54 C55 1.413(13) . ? C54 C64 1.499(14) . ? C55 C56 1.394(14) . ? C55 H55 0.9500 . ? C56 C57 1.400(12) . ? C56 C60 1.550(12) . ? C57 C58 1.396(12) . ? C57 H57 0.9500 . ? C58 C65 1.496(12) . ? C59 O5 1.427(11) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C61 1.527(14) . ? C60 C63 1.526(15) . ? C60 C62 1.528(12) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 Se5 1.976(9) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 Se6 1.974(9) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 O6 1.377(12) . ? C66 C67 1.387(16) . ? C66 C71 1.412(15) . ? C67 C68 1.411(14) . ? C67 C78 1.506(16) . ? C68 C69 1.389(17) . ? C68 H68 0.9500 . ? C69 C70 1.386(17) . ? C69 C73 1.541(16) . ? C70 C71 1.411(14) . ? C70 H70 0.9500 . ? C71 C77 1.456(16) . ? C72 O6 1.432(11) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C76 1.484(18) . ? C73 C74 1.503(19) . ? C73 C75 1.537(16) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 Se6 1.959(9) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 Se7 1.972(11) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C84 1.370(12) . ? C79 O7 1.385(10) . ? C79 C80 1.390(12) . ? C80 C81 1.411(13) . ? C80 C90 1.467(13) . ? C81 C82 1.385(14) . ? C81 H81 0.9500 . ? C82 C83 1.355(14) . ? C82 C86 1.553(13) . ? C83 C84 1.398(12) . ? C83 H83 0.9500 . ? C84 C91 1.505(12) . ? C85 O7 1.433(10) . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 C88 1.500(17) . ? C86 C87 1.532(15) . ? C86 C89 1.538(17) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 Se7 1.975(9) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 Se8 1.967(8) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 C97 1.374(14) . ? C92 C93 1.384(16) . ? C92 O8 1.410(11) . ? C93 C94 1.395(14) . ? C93 C104 1.484(15) . ? C94 C95 1.365(15) . ? C94 H94 0.9500 . ? C95 C96 1.398(17) . ? C95 C99 1.553(14) . ? C96 C97 1.398(14) . ? C96 H96 0.9500 . ? C97 C103 1.473(16) . ? C98 O8 1.425(11) . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? C99 C100 1.459(18) . ? C99 C102 1.500(15) . ? C99 C101 1.567(19) . ? C100 H10D 0.9800 . ? C100 H10E 0.9800 . ? C100 H10F 0.9800 . ? C101 H10G 0.9800 . ? C101 H10H 0.9800 . ? C101 H10I 0.9800 . ? C102 H10J 0.9800 . ? C102 H10K 0.9800 . ? C102 H10L 0.9800 . ? C103 Se8 1.983(10) . ? C103 H10M 0.9900 . ? C103 H10N 0.9900 . ? C104 Se5 1.967(11) . ? C104 H10O 0.9900 . ? C104 H10P 0.9900 . ? S1A O9A 1.407(8) . ? S1A O11A 1.433(7) . ? S1A O10A 1.438(7) . ? S1A C10A 1.821(8) . ? C10A F3A 1.303(9) . ? C10A F1A 1.338(9) . ? C10A F2A 1.362(9) . ? S1B O10B 1.422(9) . ? S1B O11B 1.422(9) . ? S1B O9B 1.460(9) . ? S1B C10B 1.831(9) . ? C10B F3B 1.324(9) . ? C10B F2B 1.326(9) . ? C10B F1B 1.329(9) . ? S2A O13A 1.435(8) . ? S2A O14A 1.444(8) . ? S2A O12A 1.455(8) . ? S2A C11A 1.803(8) . ? C11A F5A 1.318(9) . ? C11A F4A 1.324(9) . ? C11A F6A 1.330(9) . ? S2B O12B 1.433(9) . ? S2B O14B 1.439(9) . ? S2B O13B 1.447(8) . ? S2B C11B 1.815(9) . ? C11B F6B 1.315(9) . ? C11B F5B 1.325(9) . ? C11B F4B 1.327(9) . ? Se1 Ag1 2.8253(14) . ? Se2 Ag1 2.7730(14) . ? Se3 Ag1 2.8511(15) . ? Se5 Ag2 2.8534(15) . ? Se6 Ag2 2.7906(15) . ? Se7 Ag2 2.8692(14) . ? 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 C6 C1 C2 122.4(8) . . ? C6 C1 O1 118.9(8) . . ? C2 C1 O1 118.4(8) . . ? C1 C2 C3 117.4(9) . . ? C1 C2 C13 119.3(8) . . ? C3 C2 C13 122.6(8) . . ? C4 C3 C2 121.6(9) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 118.2(8) . . ? C5 C4 C8 122.7(9) . . ? C3 C4 C8 119.1(9) . . ? C4 C5 C6 121.9(9) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C1 C6 C5 118.2(8) . . ? C1 C6 C12 119.9(7) . . ? C5 C6 C12 121.7(8) . . ? O1 C7 H7A 109.5 . . ? O1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C11 107.9(9) . . ? C9 C8 C10 110.6(9) . . ? C11 C8 C10 108.3(9) . . ? C9 C8 C4 108.5(9) . . ? C11 C8 C4 112.0(9) . . ? C10 C8 C4 109.6(8) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C12 Se1 107.7(6) . . ? C6 C12 H12A 110.2 . . ? Se1 C12 H12A 110.2 . . ? C6 C12 H12B 110.2 . . ? Se1 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? C2 C13 Se2 109.3(7) . . ? C2 C13 H13A 109.8 . . ? Se2 C13 H13A 109.8 . . ? C2 C13 H13B 109.8 . . ? Se2 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? O2 C14 C15 119.6(9) . . ? O2 C14 C19 119.0(10) . . ? C15 C14 C19 121.0(9) . . ? C14 C15 C16 119.5(11) . . ? C14 C15 C25 119.4(9) . . ? C16 C15 C25 120.9(11) . . ? C15 C16 C17 119.6(12) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 119.2(11) . . ? C18 C17 C21 125.8(12) . . ? C16 C17 C21 115.0(13) . . ? C17 C18 C19 122.7(12) . . ? C17 C18 H18 118.7 . . ? C19 C18 H18 118.7 . . ? C18 C19 C14 117.5(11) . . ? C18 C19 C26 123.6(10) . . ? C14 C19 C26 118.4(9) . . ? O2 C20 H20A 109.5 . . ? O2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 C21 C22 105.8(13) . . ? C24 C21 C23 110.9(13) . . ? C22 C21 C23 107.4(14) . . ? C24 C21 C17 108.4(12) . . ? C22 C21 C17 116.9(13) . . ? C23 C21 C17 107.5(11) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C15 C25 Se2 107.2(6) . . ? C15 C25 H25A 110.3 . . ? Se2 C25 H25A 110.3 . . ? C15 C25 H25B 110.3 . . ? Se2 C25 H25B 110.3 . . ? H25A C25 H25B 108.5 . . ? C19 C26 Se3 109.5(7) . . ? C19 C26 H26A 109.8 . . ? Se3 C26 H26A 109.8 . . ? C19 C26 H26B 109.8 . . ? Se3 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? C32 C27 C28 121.3(8) . . ? C32 C27 O3 121.2(8) . . ? C28 C27 O3 117.3(8) . . ? C27 C28 C29 117.5(9) . . ? C27 C28 C39 119.2(8) . . ? C29 C28 C39 123.2(8) . . ? C30 C29 C28 122.7(8) . . ? C30 C29 H29 118.7 . . ? C28 C29 H29 118.7 . . ? C31 C30 C29 117.1(8) . . ? C31 C30 C34 120.8(9) . . ? C29 C30 C34 122.0(8) . . ? C32 C31 C30 121.9(10) . . ? C32 C31 H31 119.0 . . ? C30 C31 H31 119.0 . . ? C27 C32 C31 119.3(8) . . ? C27 C32 C38 118.8(8) . . ? C31 C32 C38 121.6(9) . . ? O3 C33 H33A 109.5 . . ? O3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C36A C34 C37B 139.1(13) . . ? C36A C34 C37A 118.0(13) . . ? C37B C34 C37A 45.3(11) . . ? C36A C34 C35B 48.3(11) . . ? C37B C34 C35B 110.8(13) . . ? C37A C34 C35B 134.1(13) . . ? C36A C34 C30 107.8(9) . . ? C37B C34 C30 113.1(10) . . ? C37A C34 C30 111.6(9) . . ? C35B C34 C30 114.3(11) . . ? C36A C34 C35A 108.8(12) . . ? C37B C34 C35A 61.0(12) . . ? C37A C34 C35A 105.6(12) . . ? C35B C34 C35A 60.6(11) . . ? C30 C34 C35A 104.2(10) . . ? C36A C34 C36B 56.0(12) . . ? C37B C34 C36B 107.8(14) . . ? C37A C34 C36B 66.2(12) . . ? C35B C34 C36B 99.6(13) . . ? C30 C34 C36B 110.3(10) . . ? C35A C34 C36B 145.2(12) . . ? C34 C35A H35A 109.5 . . ? C34 C35A H35B 109.5 . . ? C34 C35A H35C 109.5 . . ? C34 C36A H36A 109.5 . . ? C34 C36A H36B 109.5 . . ? C34 C36A H36C 109.5 . . ? C34 C37A H37A 109.5 . . ? C34 C37A H37B 109.5 . . ? C34 C37A H37C 109.5 . . ? C34 C35B H35D 109.5 . . ? C34 C35B H35E 109.5 . . ? H35D C35B H35E 109.5 . . ? C34 C35B H35F 109.5 . . ? H35D C35B H35F 109.5 . . ? H35E C35B H35F 109.5 . . ? C34 C36B H36D 109.5 . . ? C34 C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C34 C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? C34 C37B H37D 109.5 . . ? C34 C37B H37E 109.5 . . ? H37D C37B H37E 109.5 . . ? C34 C37B H37F 109.5 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? C32 C38 Se3 107.9(6) . . ? C32 C38 H38A 110.1 . . ? Se3 C38 H38A 110.1 . . ? C32 C38 H38B 110.1 . . ? Se3 C38 H38B 110.1 . . ? H38A C38 H38B 108.4 . . ? C28 C39 Se4 112.7(6) . . ? C28 C39 H39A 109.1 . . ? Se4 C39 H39A 109.1 . . ? C28 C39 H39B 109.1 . . ? Se4 C39 H39B 109.1 . . ? H39A C39 H39B 107.8 . . ? C41 C40 O4 120.0(7) . . ? C41 C40 C45 121.7(7) . . ? O4 C40 C45 118.1(6) . . ? C40 C41 C42 118.5(7) . . ? C40 C41 C51 119.6(7) . . ? C42 C41 C51 121.9(7) . . ? C43 C42 C41 121.7(7) . . ? C43 C42 H42 119.2 . . ? C41 C42 H42 119.2 . . ? C42 C43 C44 118.1(7) . . ? C42 C43 C47 122.3(7) . . ? C44 C43 C47 119.6(7) . . ? C43 C44 C45 122.2(7) . . ? C43 C44 H44 118.9 . . ? C45 C44 H44 118.9 . . ? C40 C45 C44 117.6(7) . . ? C40 C45 C52 121.2(7) . . ? C44 C45 C52 121.1(7) . . ? O4 C46 H46A 109.5 . . ? O4 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O4 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C49 C47 C50 109.5(8) . . ? C49 C47 C48 108.7(8) . . ? C50 C47 C48 109.0(8) . . ? C49 C47 C43 110.4(7) . . ? C50 C47 C43 107.4(7) . . ? C48 C47 C43 111.7(7) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C41 C51 Se4 109.4(5) . . ? C41 C51 H51A 109.8 . . ? Se4 C51 H51A 109.8 . . ? C41 C51 H51B 109.8 . . ? Se4 C51 H51B 109.8 . . ? H51A C51 H51B 108.2 . . ? C45 C52 Se1 110.7(5) . . ? C45 C52 H52A 109.5 . . ? Se1 C52 H52A 109.5 . . ? C45 C52 H52B 109.5 . . ? Se1 C52 H52B 109.5 . . ? H52A C52 H52B 108.1 . . ? C58 C53 O5 120.5(8) . . ? C58 C53 C54 121.2(8) . . ? O5 C53 C54 118.1(8) . . ? C53 C54 C55 117.4(9) . . ? C53 C54 C64 119.0(8) . . ? C55 C54 C64 123.1(9) . . ? C56 C55 C54 122.1(9) . . ? C56 C55 H55 119.0 . . ? C54 C55 H55 119.0 . . ? C55 C56 C57 118.6(8) . . ? C55 C56 C60 120.5(8) . . ? C57 C56 C60 120.9(9) . . ? C58 C57 C56 120.3(9) . . ? C58 C57 H57 119.8 . . ? C56 C57 H57 119.8 . . ? C53 C58 C57 120.1(8) . . ? C53 C58 C65 119.4(8) . . ? C57 C58 C65 120.1(9) . . ? O5 C59 H59A 109.5 . . ? O5 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? O5 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C61 C60 C63 109.6(8) . . ? C61 C60 C62 108.2(8) . . ? C63 C60 C62 109.6(9) . . ? C61 C60 C56 107.5(8) . . ? C63 C60 C56 113.0(8) . . ? C62 C60 C56 108.9(7) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C60 C63 H63A 109.5 . . ? C60 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C60 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C54 C64 Se5 109.0(7) . . ? C54 C64 H64A 109.9 . . ? Se5 C64 H64A 109.9 . . ? C54 C64 H64B 109.9 . . ? Se5 C64 H64B 109.9 . . ? H64A C64 H64B 108.3 . . ? C58 C65 Se6 107.6(6) . . ? C58 C65 H65A 110.2 . . ? Se6 C65 H65A 110.2 . . ? C58 C65 H65B 110.2 . . ? Se6 C65 H65B 110.2 . . ? H65A C65 H65B 108.5 . . ? O6 C66 C67 118.7(10) . . ? O6 C66 C71 117.4(10) . . ? C67 C66 C71 123.5(10) . . ? C66 C67 C68 116.9(11) . . ? C66 C67 C78 121.0(9) . . ? C68 C67 C78 122.0(11) . . ? C69 C68 C67 121.7(12) . . ? C69 C68 H68 119.2 . . ? C67 C68 H68 119.2 . . ? C70 C69 C68 119.4(11) . . ? C70 C69 C73 119.8(11) . . ? C68 C69 C73 120.7(12) . . ? C69 C70 C71 121.8(11) . . ? C69 C70 H70 119.1 . . ? C71 C70 H70 119.1 . . ? C70 C71 C66 116.3(11) . . ? C70 C71 C77 122.5(10) . . ? C66 C71 C77 120.7(9) . . ? O6 C72 H72A 109.5 . . ? O6 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? O6 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C76 C73 C74 107.1(11) . . ? C76 C73 C75 110.0(11) . . ? C74 C73 C75 107.5(12) . . ? C76 C73 C69 109.7(11) . . ? C74 C73 C69 113.4(11) . . ? C75 C73 C69 109.1(10) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C73 C76 H76A 109.5 . . ? C73 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C73 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C71 C77 Se6 109.7(7) . . ? C71 C77 H77A 109.7 . . ? Se6 C77 H77A 109.7 . . ? C71 C77 H77B 109.7 . . ? Se6 C77 H77B 109.7 . . ? H77A C77 H77B 108.2 . . ? C67 C78 Se7 108.4(7) . . ? C67 C78 H78A 110.0 . . ? Se7 C78 H78A 110.0 . . ? C67 C78 H78B 110.0 . . ? Se7 C78 H78B 110.0 . . ? H78A C78 H78B 108.4 . . ? C84 C79 O7 120.3(7) . . ? C84 C79 C80 120.8(8) . . ? O7 C79 C80 118.8(8) . . ? C79 C80 C81 116.6(9) . . ? C79 C80 C90 120.8(8) . . ? C81 C80 C90 122.3(8) . . ? C82 C81 C80 123.5(9) . . ? C82 C81 H81 118.2 . . ? C80 C81 H81 118.2 . . ? C83 C82 C81 116.9(9) . . ? C83 C82 C86 120.9(10) . . ? C81 C82 C86 122.1(10) . . ? C82 C83 C84 122.1(9) . . ? C82 C83 H83 118.9 . . ? C84 C83 H83 118.9 . . ? C79 C84 C83 119.8(8) . . ? C79 C84 C91 119.0(7) . . ? C83 C84 C91 121.2(8) . . ? O7 C85 H85A 109.5 . . ? O7 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? O7 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C88 C86 C87 110.6(10) . . ? C88 C86 C89 107.8(10) . . ? C87 C86 C89 108.3(10) . . ? C88 C86 C82 108.4(10) . . ? C87 C86 C82 109.0(9) . . ? C89 C86 C82 112.8(10) . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C86 C88 H88A 109.5 . . ? C86 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C86 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C86 C89 H89A 109.5 . . ? C86 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C86 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C80 C90 Se7 111.7(7) . . ? C80 C90 H90A 109.3 . . ? Se7 C90 H90A 109.3 . . ? C80 C90 H90B 109.3 . . ? Se7 C90 H90B 109.3 . . ? H90A C90 H90B 107.9 . . ? C84 C91 Se8 109.6(6) . . ? C84 C91 H91A 109.8 . . ? Se8 C91 H91A 109.8 . . ? C84 C91 H91B 109.8 . . ? Se8 C91 H91B 109.8 . . ? H91A C91 H91B 108.2 . . ? C97 C92 C93 120.7(9) . . ? C97 C92 O8 118.9(10) . . ? C93 C92 O8 120.1(9) . . ? C92 C93 C94 118.7(10) . . ? C92 C93 C104 119.4(9) . . ? C94 C93 C104 121.8(11) . . ? C95 C94 C93 123.0(12) . . ? C95 C94 H94 118.5 . . ? C93 C94 H94 118.5 . . ? C94 C95 C96 116.5(10) . . ? C94 C95 C99 122.9(12) . . ? C96 C95 C99 120.6(10) . . ? C97 C96 C95 122.4(10) . . ? C97 C96 H96 118.8 . . ? C95 C96 H96 118.8 . . ? C92 C97 C96 118.6(11) . . ? C92 C97 C103 118.6(9) . . ? C96 C97 C103 122.8(10) . . ? O8 C98 H98A 109.5 . . ? O8 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? O8 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C100 C99 C102 113.0(12) . . ? C100 C99 C95 113.5(10) . . ? C102 C99 C95 109.1(9) . . ? C100 C99 C101 106.4(11) . . ? C102 C99 C101 107.3(11) . . ? C95 C99 C101 107.0(11) . . ? C99 C100 H10D 109.5 . . ? C99 C100 H10E 109.5 . . ? H10D C100 H10E 109.5 . . ? C99 C100 H10F 109.5 . . ? H10D C100 H10F 109.5 . . ? H10E C100 H10F 109.5 . . ? C99 C101 H10G 109.5 . . ? C99 C101 H10H 109.5 . . ? H10G C101 H10H 109.5 . . ? C99 C101 H10I 109.5 . . ? H10G C101 H10I 109.5 . . ? H10H C101 H10I 109.5 . . ? C99 C102 H10J 109.5 . . ? C99 C102 H10K 109.5 . . ? H10J C102 H10K 109.5 . . ? C99 C102 H10L 109.5 . . ? H10J C102 H10L 109.5 . . ? H10K C102 H10L 109.5 . . ? C97 C103 Se8 112.7(7) . . ? C97 C103 H10M 109.0 . . ? Se8 C103 H10M 109.0 . . ? C97 C103 H10N 109.0 . . ? Se8 C103 H10N 109.0 . . ? H10M C103 H10N 107.8 . . ? C93 C104 Se5 105.7(7) . . ? C93 C104 H10O 110.6 . . ? Se5 C104 H10O 110.6 . . ? C93 C104 H10P 110.6 . . ? Se5 C104 H10P 110.6 . . ? H10O C104 H10P 108.7 . . ? C1 O1 C7 112.5(6) . . ? C14 O2 C20 113.3(7) . . ? C27 O3 C33 113.2(6) . . ? C40 O4 C46 113.7(6) . . ? C53 O5 C59 113.5(7) . . ? C66 O6 C72 112.3(7) . . ? C79 O7 C85 113.1(6) . . ? C92 O8 C98 114.4(7) . . ? O9A S1A O11A 114.1(7) . . ? O9A S1A O10A 116.3(7) . . ? O11A S1A O10A 109.1(7) . . ? O9A S1A C10A 107.8(6) . . ? O11A S1A C10A 105.4(6) . . ? O10A S1A C10A 103.1(6) . . ? F3A C10A F1A 112.8(9) . . ? F3A C10A F2A 105.6(9) . . ? F1A C10A F2A 107.0(9) . . ? F3A C10A S1A 113.5(8) . . ? F1A C10A S1A 109.1(7) . . ? F2A C10A S1A 108.6(7) . . ? O10B S1B O11B 118.3(11) . . ? O10B S1B O9B 116.6(10) . . ? O11B S1B O9B 113.9(10) . . ? O10B S1B C10B 102.2(9) . . ? O11B S1B C10B 102.0(9) . . ? O9B S1B C10B 99.6(9) . . ? F3B C10B F2B 107.7(12) . . ? F3B C10B F1B 107.2(12) . . ? F2B C10B F1B 107.2(11) . . ? F3B C10B S1B 112.4(10) . . ? F2B C10B S1B 109.7(10) . . ? F1B C10B S1B 112.3(10) . . ? O13A S2A O14A 115.5(8) . . ? O13A S2A O12A 115.5(8) . . ? O14A S2A O12A 113.8(8) . . ? O13A S2A C11A 104.1(6) . . ? O14A S2A C11A 102.5(7) . . ? O12A S2A C11A 103.1(8) . . ? F5A C11A F4A 109.0(9) . . ? F5A C11A F6A 106.7(9) . . ? F4A C11A F6A 108.5(9) . . ? F5A C11A S2A 111.6(8) . . ? F4A C11A S2A 111.3(7) . . ? F6A C11A S2A 109.6(8) . . ? O12B S2B O14B 115.6(11) . . ? O12B S2B O13B 114.3(11) . . ? O14B S2B O13B 115.3(9) . . ? O12B S2B C11B 106.0(10) . . ? O14B S2B C11B 101.9(8) . . ? O13B S2B C11B 101.0(8) . . ? F6B C11B F5B 108.1(11) . . ? F6B C11B F4B 110.4(11) . . ? F5B C11B F4B 106.2(11) . . ? F6B C11B S2B 109.1(9) . . ? F5B C11B S2B 111.2(10) . . ? F4B C11B S2B 111.7(10) . . ? C52 Se1 C12 96.3(3) . . ? C52 Se1 Ag1 110.2(2) . . ? C12 Se1 Ag1 110.1(3) . . ? C25 Se2 C13 96.0(4) . . ? C25 Se2 Ag1 109.5(3) . . ? C13 Se2 Ag1 111.4(3) . . ? C38 Se3 C26 95.1(4) . . ? C38 Se3 Ag1 108.3(3) . . ? C26 Se3 Ag1 109.1(3) . . ? C51 Se4 C39 95.1(3) . . ? C104 Se5 C64 95.4(4) . . ? C104 Se5 Ag2 109.1(4) . . ? C64 Se5 Ag2 109.7(3) . . ? C77 Se6 C65 95.8(4) . . ? C77 Se6 Ag2 111.3(3) . . ? C65 Se6 Ag2 109.1(3) . . ? C78 Se7 C90 94.7(4) . . ? C78 Se7 Ag2 110.4(3) . . ? C90 Se7 Ag2 110.7(3) . . ? C91 Se8 C103 95.4(4) . . ? Se2 Ag1 Se1 125.98(4) . . ? Se2 Ag1 Se3 124.38(4) . . ? Se1 Ag1 Se3 86.41(5) . . ? Se6 Ag2 Se5 123.66(4) . . ? Se6 Ag2 Se7 126.29(4) . . ? Se5 Ag2 Se7 87.46(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 66.59 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.020 _refine_diff_density_min -1.627 _refine_diff_density_rms 0.161 data_16 _database_code_depnum_ccdc_archive 'CCDC 848955' #TrackingRef '16.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H72 Ag O4 Se4, F6 P' _chemical_formula_sum 'C52 H72 Ag F6 O4 P Se4' _chemical_formula_weight 1329.78 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 n 2' _symmetry_space_group_name_Hall 'P -4 -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.994(2) _cell_length_b 13.994(2) _cell_length_c 14.223(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2785.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2948 _cell_measurement_theta_min 2.8596 _cell_measurement_theta_max 28.0841 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 3.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3888 _exptl_absorpt_correction_T_max 0.7291 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_type KM4CCD _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11491 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_sigmaI/netI 0.1234 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2855 _reflns_number_gt 1461 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrysAlisCCD _computing_cell_refinement CrysAlisRED _computing_data_reduction CrysAlisRED _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0329P)^2^] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(19) _refine_ls_number_reflns 2855 _refine_ls_number_parameters 168 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.0937 _refine_ls_wR_factor_gt 0.0887 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.003 _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 Ag1 Ag 0.0000 1.0000 0.0000 0.0654(4) Uani 1 4 d S . . Se1 Se -0.02512(5) 0.86350(6) 0.15611(7) 0.0599(3) Uani 1 1 d . . . C1 C 0.1027(5) 0.8094(5) 0.1890(5) 0.057(2) Uani 1 1 d . . . H1A H 0.1393 0.8567 0.2261 0.069 Uiso 1 1 calc R . . H1B H 0.0943 0.7515 0.2280 0.069 Uiso 1 1 calc R . . C2 C 0.1561(5) 0.7849(6) 0.1032(6) 0.049(2) Uani 1 1 d . . . C3 C 0.1697(4) 0.6901(5) 0.0730(6) 0.048(2) Uani 1 1 d . . . H3 H 0.1472 0.6393 0.1114 0.058 Uiso 1 1 calc R . . C4 C 0.2155(5) 0.6683(5) -0.0121(6) 0.052(2) Uani 1 1 d . . . C5 C 0.2447(5) 0.7435(5) -0.0668(6) 0.056(2) Uani 1 1 d . . . H5 H 0.2756 0.7304 -0.1249 0.068 Uiso 1 1 calc R . . C6 C 0.2307(5) 0.8397(5) -0.0402(7) 0.047(2) Uani 1 1 d . . . C7 C 0.1920(5) 0.8584(6) 0.0475(7) 0.047(2) Uani 1 1 d . . . C8 C 0.2546(5) 0.9211(5) -0.1053(6) 0.073(3) Uani 1 1 d . . . H8A H 0.2955 0.8979 -0.1572 0.088 Uiso 1 1 calc R . . H8B H 0.2902 0.9710 -0.0705 0.088 Uiso 1 1 calc R . . C9 C 0.2333(6) 0.5654(5) -0.0403(6) 0.060(3) Uani 1 1 d . . . C10 C 0.1388(6) 0.5219(6) -0.0692(7) 0.095(3) Uani 1 1 d U . . H10A H 0.1167 0.5521 -0.1274 0.143 Uiso 1 1 calc R . . H10B H 0.0916 0.5324 -0.0194 0.143 Uiso 1 1 calc R . . H10C H 0.1470 0.4532 -0.0795 0.143 Uiso 1 1 calc R . . C11 C 0.2816(9) 0.5123(6) 0.0409(8) 0.122(5) Uani 1 1 d . . . H11A H 0.3008 0.4485 0.0199 0.183 Uiso 1 1 calc R . . H11B H 0.2367 0.5065 0.0935 0.183 Uiso 1 1 calc R . . H11C H 0.3381 0.5480 0.0614 0.183 Uiso 1 1 calc R . . C12 C 0.2990(7) 0.5560(6) -0.1228(7) 0.110(4) Uani 1 1 d . . . H12A H 0.2767 0.5975 -0.1738 0.165 Uiso 1 1 calc R . . H12B H 0.2995 0.4895 -0.1444 0.165 Uiso 1 1 calc R . . H12C H 0.3637 0.5749 -0.1043 0.165 Uiso 1 1 calc R . . O13 O 0.1809(3) 0.9514(3) 0.0763(4) 0.0601(16) Uani 1 1 d . . . C14 C 0.2640(7) 0.9834(6) 0.1264(7) 0.092(4) Uani 1 1 d . . . H14A H 0.2736 0.9433 0.1821 0.138 Uiso 1 1 calc R . . H14B H 0.2551 1.0500 0.1459 0.138 Uiso 1 1 calc R . . H14C H 0.3201 0.9788 0.0855 0.138 Uiso 1 1 calc R . . P15 P 0.0000 0.5000 0.2500 0.0636(14) Uani 1 4 d SD . . F16 F 0.0357(7) 0.4009(7) 0.2583(7) 0.134(6) Uani 0.50 1 d PD A -1 F16A F 0.1057(4) 0.5390(7) 0.2521(6) 0.082(4) Uani 0.50 1 d PD A -1 F17 F 0.0000 0.5000 0.1427(6) 0.107(3) Uani 1 2 d SD A . 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 Ag1 0.0545(5) 0.0545(5) 0.0872(11) 0.000 0.000 0.000 Se1 0.0435(4) 0.0532(5) 0.0830(6) -0.0032(5) 0.0051(5) 0.0181(4) C1 0.041(4) 0.059(5) 0.071(7) -0.006(5) -0.011(5) 0.026(4) C2 0.026(4) 0.051(5) 0.070(6) -0.011(5) -0.007(4) 0.018(4) C3 0.026(4) 0.048(5) 0.072(6) 0.009(5) 0.000(4) 0.006(4) C4 0.043(4) 0.028(4) 0.084(7) -0.009(5) 0.019(5) -0.008(3) C5 0.032(4) 0.046(5) 0.092(6) -0.024(5) 0.010(4) -0.003(4) C6 0.020(4) 0.030(4) 0.091(7) 0.011(5) 0.003(4) 0.000(3) C7 0.029(4) 0.033(5) 0.080(7) -0.004(5) 0.006(4) 0.010(4) C8 0.052(5) 0.058(5) 0.110(8) -0.022(5) 0.031(5) -0.025(5) C9 0.045(5) 0.036(4) 0.100(8) -0.006(5) 0.016(5) 0.002(4) C10 0.076(6) 0.065(5) 0.144(8) -0.051(5) 0.001(6) -0.017(5) C11 0.164(10) 0.043(6) 0.160(12) -0.002(7) -0.029(9) 0.042(7) C12 0.095(7) 0.070(6) 0.165(11) -0.037(7) 0.073(7) -0.006(6) O13 0.042(3) 0.026(3) 0.112(5) -0.008(3) -0.004(3) 0.007(2) C14 0.089(8) 0.048(6) 0.139(11) -0.029(6) -0.018(7) 0.012(5) P15 0.053(2) 0.053(2) 0.084(5) 0.000 0.000 -0.014(3) F16 0.072(8) 0.066(8) 0.263(18) -0.049(10) 0.043(11) -0.017(7) F16A 0.049(6) 0.090(8) 0.106(9) 0.039(9) 0.011(7) -0.030(6) F17 0.088(5) 0.106(6) 0.126(8) 0.000 0.000 -0.038(4) _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 Ag1 Se1 2.9500(10) 3_575 ? Ag1 Se1 2.9500(10) 2_465 ? Ag1 Se1 2.9500(10) 4_665 ? Ag1 Se1 2.9500(10) . ? Se1 C8 1.954(8) 2_465 ? Se1 C1 1.998(6) . ? C1 C2 1.471(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.393(10) . ? C2 C3 1.407(10) . ? C3 C4 1.404(10) . ? C3 H3 0.9500 . ? C4 C5 1.372(9) . ? C4 C9 1.515(10) . ? C5 C6 1.412(9) . ? C5 H5 0.9500 . ? C6 C7 1.385(10) . ? C6 C8 1.505(10) . ? C7 O13 1.373(8) . ? C8 Se1 1.954(8) 4_665 ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C12 1.497(11) . ? C9 C10 1.513(11) . ? C9 C11 1.530(11) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? O13 C14 1.436(9) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? P15 F16 1.479(9) 3_565 ? P15 F16 1.479(9) 6 ? P15 F16 1.479(9) . ? P15 F16 1.479(9) 5_455 ? P15 F17 1.527(8) . ? P15 F17 1.527(8) 5_455 ? P15 F16A 1.577(4) 5_455 ? P15 F16A 1.577(4) 3_565 ? P15 F16A 1.577(4) . ? P15 F16A 1.577(4) 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 Se1 Ag1 Se1 124.51(2) 3_575 2_465 ? Se1 Ag1 Se1 124.51(2) 3_575 4_665 ? Se1 Ag1 Se1 82.35(4) 2_465 4_665 ? Se1 Ag1 Se1 82.35(4) 3_575 . ? Se1 Ag1 Se1 124.51(2) 2_465 . ? Se1 Ag1 Se1 124.51(2) 4_665 . ? C8 Se1 C1 96.4(3) 2_465 . ? C8 Se1 Ag1 108.3(2) 2_465 . ? C1 Se1 Ag1 108.3(2) . . ? C2 C1 Se1 110.4(5) . . ? C2 C1 H1A 109.6 . . ? Se1 C1 H1A 109.6 . . ? C2 C1 H1B 109.6 . . ? Se1 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? C7 C2 C3 118.3(7) . . ? C7 C2 C1 118.9(7) . . ? C3 C2 C1 122.8(8) . . ? C4 C3 C2 122.0(7) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C5 C4 C3 117.3(6) . . ? C5 C4 C9 122.1(7) . . ? C3 C4 C9 120.7(7) . . ? C4 C5 C6 122.6(8) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C7 C6 C5 118.4(7) . . ? C7 C6 C8 119.9(7) . . ? C5 C6 C8 121.7(8) . . ? O13 C7 C6 119.5(7) . . ? O13 C7 C2 119.3(7) . . ? C6 C7 C2 121.0(7) . . ? C6 C8 Se1 109.3(5) . 4_665 ? C6 C8 H8A 109.8 . . ? Se1 C8 H8A 109.8 4_665 . ? C6 C8 H8B 109.8 . . ? Se1 C8 H8B 109.8 4_665 . ? H8A C8 H8B 108.3 . . ? C12 C9 C10 106.7(8) . . ? C12 C9 C4 113.0(7) . . ? C10 C9 C4 108.1(7) . . ? C12 C9 C11 106.2(8) . . ? C10 C9 C11 113.3(8) . . ? C4 C9 C11 109.6(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C7 O13 C14 110.6(5) . . ? O13 C14 H14A 109.5 . . ? O13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? F16 P15 F16 129.8(8) 3_565 6 ? F16 P15 F16 170.8(8) 3_565 . ? F16 P15 F16 51.2(8) 6 . ? F16 P15 F16 51.2(8) 3_565 5_455 ? F16 P15 F16 170.8(8) 6 5_455 ? F16 P15 F16 129.8(8) . 5_455 ? F16 P15 F17 94.6(4) 3_565 . ? F16 P15 F17 85.4(4) 6 . ? F16 P15 F17 94.6(4) . . ? F16 P15 F17 85.4(4) 5_455 . ? F16 P15 F17 85.4(4) 3_565 5_455 ? F16 P15 F17 94.6(4) 6 5_455 ? F16 P15 F17 85.4(4) . 5_455 ? F16 P15 F17 94.6(4) 5_455 5_455 ? F17 P15 F17 180.000(1) . 5_455 ? F16 P15 F16A 89.5(7) 6 5_455 ? F16 P15 F16A 139.8(4) . 5_455 ? F16 P15 F16A 90.4(7) 5_455 5_455 ? F17 P15 F16A 88.9(3) . 5_455 ? F17 P15 F16A 91.1(3) 5_455 5_455 ? F16 P15 F16A 90.4(7) 3_565 3_565 ? F16 P15 F16A 139.8(4) 6 3_565 ? F16 P15 F16A 89.5(7) . 3_565 ? F17 P15 F16A 91.1(3) . 3_565 ? F17 P15 F16A 88.9(3) 5_455 3_565 ? F16A P15 F16A 130.5(8) 5_455 3_565 ? F16 P15 F16A 89.5(7) 3_565 . ? F16 P15 F16A 90.4(7) . . ? F16 P15 F16A 139.8(4) 5_455 . ? F17 P15 F16A 91.1(3) . . ? F17 P15 F16A 88.9(3) 5_455 . ? F16A P15 F16A 49.5(8) 5_455 . ? F16A P15 F16A 177.8(6) 3_565 . ? F16 P15 F16A 139.8(4) 3_565 6 ? F16 P15 F16A 90.4(7) 6 6 ? F16 P15 F16A 89.5(7) 5_455 6 ? F17 P15 F16A 88.9(3) . 6 ? F17 P15 F16A 91.1(3) 5_455 6 ? F16A P15 F16A 177.8(6) 5_455 6 ? F16A P15 F16A 49.5(8) 3_565 6 ? F16A P15 F16A 130.5(8) . 6 ? 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 Se1 Ag1 Se1 C8 166.3(2) 3_575 . . 2_465 ? Se1 Ag1 Se1 C8 39.3(2) 2_465 . . 2_465 ? Se1 Ag1 Se1 C8 -66.8(2) 4_665 . . 2_465 ? Se1 Ag1 Se1 C1 -90.3(2) 3_575 . . . ? Se1 Ag1 Se1 C1 142.8(2) 2_465 . . . ? Se1 Ag1 Se1 C1 36.7(2) 4_665 . . . ? C8 Se1 C1 C2 68.1(6) 2_465 . . . ? Ag1 Se1 C1 C2 -43.7(6) . . . . ? Se1 C1 C2 C7 71.6(7) . . . . ? Se1 C1 C2 C3 -106.0(7) . . . . ? C7 C2 C3 C4 -1.8(10) . . . . ? C1 C2 C3 C4 175.8(6) . . . . ? C2 C3 C4 C5 -1.7(10) . . . . ? C2 C3 C4 C9 177.0(7) . . . . ? C3 C4 C5 C6 0.3(11) . . . . ? C9 C4 C5 C6 -178.4(7) . . . . ? C4 C5 C6 C7 4.6(11) . . . . ? C4 C5 C6 C8 -174.0(7) . . . . ? C5 C6 C7 O13 177.7(6) . . . . ? C8 C6 C7 O13 -3.7(10) . . . . ? C5 C6 C7 C2 -8.3(10) . . . . ? C8 C6 C7 C2 170.3(6) . . . . ? C3 C2 C7 O13 -179.0(6) . . . . ? C1 C2 C7 O13 3.2(9) . . . . ? C3 C2 C7 C6 7.0(10) . . . . ? C1 C2 C7 C6 -170.8(6) . . . . ? C7 C6 C8 Se1 -73.3(8) . . . 4_665 ? C5 C6 C8 Se1 105.3(7) . . . 4_665 ? C5 C4 C9 C12 9.8(11) . . . . ? C3 C4 C9 C12 -168.8(7) . . . . ? C5 C4 C9 C10 -108.1(8) . . . . ? C3 C4 C9 C10 73.3(10) . . . . ? C5 C4 C9 C11 128.0(9) . . . . ? C3 C4 C9 C11 -50.6(10) . . . . ? C6 C7 O13 C14 -91.1(9) . . . . ? C2 C7 O13 C14 94.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.603 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.090 data_3 _database_code_depnum_ccdc_archive 'CCDC 848956' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H88 O8 Se4, 2(C H Cl3)' _chemical_formula_sum 'C64 H90 Cl6 O8 Se4' _chemical_formula_weight 1515.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8677(13) _cell_length_b 12.6155(10) _cell_length_c 26.392(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.784(8) _cell_angle_gamma 90.00 _cell_volume 3600.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 4.871 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.159 _exptl_absorpt_correction_T_max 0.482 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'crossed G\"obel mirrors' _diffrn_measurement_device_type 'SMART 6000' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30601 _diffrn_reflns_av_R_equivalents 0.0777 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 71.72 _reflns_number_total 6885 _reflns_number_gt 5837 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material Platon _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^)+(0.0426P)^2^+3.3176P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6885 _refine_ls_number_parameters 411 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1137 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.056 _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 C1 C 0.8971(3) 0.7685(2) 0.00709(11) 0.0196(6) Uani 1 1 d . . . C2 C 0.9272(3) 0.7807(2) -0.04249(12) 0.0209(6) Uani 1 1 d . . . H2 H 0.9531 0.8484 -0.0530 0.025 Uiso 1 1 calc R . . C3 C 0.9208(3) 0.6971(3) -0.07750(12) 0.0221(6) Uani 1 1 d . . . C4 C 0.8855(3) 0.5987(3) -0.06066(12) 0.0218(6) Uani 1 1 d . . . H4 H 0.8804 0.5406 -0.0837 0.026 Uiso 1 1 calc R . . C5 C 0.8570(3) 0.5824(2) -0.01079(12) 0.0199(6) Uani 1 1 d . . . C6 C 0.8611(3) 0.6683(2) 0.02258(11) 0.0181(6) Uani 1 1 d . . . C7 C 0.7140(3) 0.6378(3) 0.08187(12) 0.0230(6) Uani 1 1 d . . . H7A H 0.6731 0.5892 0.0559 0.028 Uiso 1 1 calc R . . H7B H 0.6690 0.7061 0.0799 0.028 Uiso 1 1 calc R . . C8 C 0.7132(3) 0.5902(3) 0.13452(12) 0.0248(7) Uani 1 1 d . . . C9 C 0.5708(3) 0.5088(3) 0.18958(12) 0.0300(7) Uani 1 1 d . . . C10 C 0.6087(4) 0.5755(4) 0.23608(14) 0.0446(10) Uani 1 1 d . . . H10A H 0.6988 0.5838 0.2400 0.067 Uiso 1 1 calc R . . H10B H 0.5823 0.5406 0.2663 0.067 Uiso 1 1 calc R . . H10C H 0.5696 0.6454 0.2321 0.067 Uiso 1 1 calc R . . C11 C 0.6334(4) 0.4017(3) 0.19144(14) 0.0370(8) Uani 1 1 d . . . H11A H 0.6116 0.3643 0.1592 0.056 Uiso 1 1 calc R . . H11B H 0.6059 0.3600 0.2196 0.056 Uiso 1 1 calc R . . H11C H 0.7232 0.4113 0.1967 0.056 Uiso 1 1 calc R . . C12 C 0.4310(4) 0.4967(4) 0.18159(16) 0.0419(10) Uani 1 1 d . . . H12A H 0.3923 0.5669 0.1811 0.063 Uiso 1 1 calc R . . H12B H 0.4029 0.4545 0.2094 0.063 Uiso 1 1 calc R . . H12C H 0.4078 0.4609 0.1491 0.063 Uiso 1 1 calc R . . C13 C 0.9534(3) 0.7174(3) -0.13178(12) 0.0309(7) Uani 1 1 d . . . C14 C 0.8678(5) 0.8010(5) -0.15664(16) 0.0604(14) Uani 1 1 d . . . H14A H 0.7820 0.7762 -0.1579 0.091 Uiso 1 1 calc R . . H14B H 0.8889 0.8144 -0.1913 0.091 Uiso 1 1 calc R . . H14C H 0.8769 0.8667 -0.1368 0.091 Uiso 1 1 calc R . . C15 C 1.0880(4) 0.7554(4) -0.12992(15) 0.0461(10) Uani 1 1 d . . . H15A H 1.0983 0.8200 -0.1093 0.069 Uiso 1 1 calc R . . H15B H 1.1083 0.7703 -0.1646 0.069 Uiso 1 1 calc R . . H15C H 1.1432 0.7001 -0.1147 0.069 Uiso 1 1 calc R . . C16 C 0.9427(5) 0.6160(4) -0.16387(17) 0.0588(13) Uani 1 1 d . . . H16A H 1.0018 0.5633 -0.1489 0.088 Uiso 1 1 calc R . . H16B H 0.9610 0.6321 -0.1987 0.088 Uiso 1 1 calc R . . H16C H 0.8586 0.5877 -0.1646 0.088 Uiso 1 1 calc R . . C17 C 0.8298(3) 0.4718(2) 0.00562(12) 0.0227(6) Uani 1 1 d . . . H17A H 0.8306 0.4695 0.0432 0.027 Uiso 1 1 calc R . . H17B H 0.8948 0.4232 -0.0042 0.027 Uiso 1 1 calc R . . C18 C 0.3060(3) 0.7247(2) 0.00670(13) 0.0269(7) Uani 1 1 d . . . H18A H 0.2973 0.7312 -0.0309 0.032 Uiso 1 1 calc R . . H18B H 0.2287 0.7506 0.0193 0.032 Uiso 1 1 calc R . . C19 C 0.4128(3) 0.7906(2) 0.02886(12) 0.0213(6) Uani 1 1 d . . . C20 C 0.4229(3) 0.8205(3) 0.08009(13) 0.0251(7) Uani 1 1 d . . . H20 H 0.3650 0.7932 0.1014 0.030 Uiso 1 1 calc R . . C21 C 0.5145(3) 0.8886(3) 0.10090(12) 0.0235(6) Uani 1 1 d . A . C22 C 0.6011(3) 0.9248(2) 0.06915(12) 0.0213(6) Uani 1 1 d . . . H22 H 0.6655 0.9707 0.0828 0.026 Uiso 1 1 calc R . . C23 C 0.5957(3) 0.8955(2) 0.01815(11) 0.0186(6) Uani 1 1 d . . . C24 C 0.5006(3) 0.8275(2) -0.00138(11) 0.0200(6) Uani 1 1 d . . . C25 C 0.5550(4) 0.7093(3) -0.06478(14) 0.0316(7) Uani 1 1 d . . . H25A H 0.6401 0.7124 -0.0486 0.047 Uiso 1 1 calc R . . H25B H 0.5560 0.7034 -0.1018 0.047 Uiso 1 1 calc R . . H25C H 0.5131 0.6474 -0.0521 0.047 Uiso 1 1 calc R . . C26 C 0.5241(4) 0.9244(3) 0.15672(13) 0.0324(8) Uani 1 1 d D . . C27A C 0.6433(5) 0.8786(5) 0.18412(19) 0.0473(15) Uani 0.798(8) 1 d PU A 1 H27A H 0.6499 0.8991 0.2201 0.071 Uiso 0.798(8) 1 calc PR A 1 H27B H 0.7147 0.9062 0.1684 0.071 Uiso 0.798(8) 1 calc PR A 1 H27C H 0.6416 0.8011 0.1814 0.071 Uiso 0.798(8) 1 calc PR A 1 C28A C 0.4143(6) 0.8849(7) 0.18344(19) 0.0585(18) Uani 0.798(8) 1 d PU A 1 H28A H 0.4137 0.8072 0.1836 0.088 Uiso 0.798(8) 1 calc PR A 1 H28B H 0.3371 0.9110 0.1653 0.088 Uiso 0.798(8) 1 calc PR A 1 H28C H 0.4215 0.9111 0.2186 0.088 Uiso 0.798(8) 1 calc PR A 1 C29A C 0.5294(8) 1.0444(5) 0.1592(2) 0.0541(17) Uani 0.798(8) 1 d PU A 1 H29A H 0.5411 1.0670 0.1949 0.081 Uiso 0.798(8) 1 calc PR A 1 H29B H 0.4519 1.0739 0.1429 0.081 Uiso 0.798(8) 1 calc PR A 1 H29C H 0.5986 1.0698 0.1414 0.081 Uiso 0.798(8) 1 calc PR A 1 C27B C 0.559(2) 0.8301(14) 0.1910(8) 0.055(6) Uani 0.202(8) 1 d PDU A 2 H27D H 0.6432 0.8077 0.1867 0.082 Uiso 0.202(8) 1 calc PR A 2 H27E H 0.5014 0.7715 0.1819 0.082 Uiso 0.202(8) 1 calc PR A 2 H27F H 0.5533 0.8502 0.2266 0.082 Uiso 0.202(8) 1 calc PR A 2 C28B C 0.3987(14) 0.972(2) 0.1668(10) 0.059(6) Uani 0.202(8) 1 d PDU A 2 H28D H 0.3351 0.9165 0.1626 0.089 Uiso 0.202(8) 1 calc PR A 2 H28E H 0.3771 1.0293 0.1427 0.089 Uiso 0.202(8) 1 calc PR A 2 H28F H 0.4039 0.9994 0.2017 0.089 Uiso 0.202(8) 1 calc PR A 2 C29B C 0.613(2) 1.0170(16) 0.1690(9) 0.048(5) Uani 0.202(8) 1 d PDU A 2 H29D H 0.6047 1.0430 0.2035 0.073 Uiso 0.202(8) 1 calc PR A 2 H29E H 0.5942 1.0743 0.1444 0.073 Uiso 0.202(8) 1 calc PR A 2 H29F H 0.6985 0.9929 0.1671 0.073 Uiso 0.202(8) 1 calc PR A 2 C30 C 0.6821(3) 0.9394(2) -0.01769(12) 0.0215(6) Uani 1 1 d . . . H30A H 0.6388 0.9973 -0.0376 0.026 Uiso 1 1 calc R . . H30B H 0.6991 0.8828 -0.0420 0.026 Uiso 1 1 calc R . . C31 C 0.9041(3) 0.8605(2) 0.04349(12) 0.0224(6) Uani 1 1 d . . . H31A H 0.9915 0.8711 0.0571 0.027 Uiso 1 1 calc R . . H31B H 0.8570 0.8426 0.0725 0.027 Uiso 1 1 calc R . . C32 C 0.0497(4) 0.7144(4) 0.17085(14) 0.0391(9) Uani 1 1 d . . . H32 H -0.0334 0.6811 0.1624 0.047 Uiso 1 1 calc R . . O30 O 0.4903(2) 0.80364(18) -0.05302(8) 0.0248(5) Uani 1 1 d . . . O32 O 0.8039(2) 0.5774(2) 0.16380(9) 0.0385(6) Uani 1 1 d . . . O33 O 0.5974(2) 0.5651(2) 0.14230(8) 0.0279(5) Uani 1 1 d . . . O34 O 0.8399(2) 0.65373(18) 0.07306(8) 0.0228(5) Uani 1 1 d . . . Cl1 Cl 0.03211(13) 0.85273(11) 0.17395(4) 0.0633(3) Uani 1 1 d . . . Cl2 Cl 0.11551(17) 0.66495(14) 0.22972(4) 0.0796(4) Uani 1 1 d . . . Cl3 Cl 0.14581(8) 0.68026(8) 0.12358(3) 0.0379(2) Uani 1 1 d . . . Se1 Se 0.33263(3) 0.57556(3) 0.026069(14) 0.02524(11) Uani 1 1 d . . . Se2 Se 0.83982(3) 0.99407(3) 0.013159(13) 0.02488(11) 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 C1 0.0165(14) 0.0170(14) 0.0249(14) 0.0007(12) 0.0009(11) -0.0028(11) C2 0.0200(15) 0.0176(14) 0.0252(15) 0.0019(12) 0.0022(12) -0.0046(12) C3 0.0201(15) 0.0234(15) 0.0228(14) 0.0001(12) 0.0017(12) -0.0033(12) C4 0.0198(15) 0.0210(14) 0.0243(14) -0.0042(12) 0.0008(12) -0.0014(12) C5 0.0133(13) 0.0188(14) 0.0271(15) 0.0018(12) -0.0006(11) -0.0023(11) C6 0.0132(13) 0.0208(14) 0.0201(13) 0.0015(12) 0.0010(11) -0.0028(11) C7 0.0204(15) 0.0245(15) 0.0248(15) 0.0058(13) 0.0052(12) -0.0002(12) C8 0.0253(16) 0.0265(16) 0.0229(15) 0.0004(13) 0.0042(13) -0.0036(13) C9 0.0309(18) 0.039(2) 0.0207(15) 0.0070(14) 0.0075(13) -0.0051(15) C10 0.059(3) 0.050(2) 0.0268(18) 0.0019(17) 0.0127(17) -0.010(2) C11 0.037(2) 0.040(2) 0.0339(18) 0.0095(16) 0.0051(15) -0.0028(17) C12 0.0294(19) 0.058(3) 0.040(2) 0.0144(19) 0.0108(16) -0.0062(18) C13 0.0366(19) 0.0371(19) 0.0195(15) 0.0010(14) 0.0057(13) -0.0047(16) C14 0.062(3) 0.087(4) 0.032(2) 0.025(2) 0.008(2) 0.018(3) C15 0.046(2) 0.061(3) 0.0338(19) 0.0064(19) 0.0174(17) -0.009(2) C16 0.082(4) 0.062(3) 0.035(2) -0.014(2) 0.021(2) -0.020(3) C17 0.0209(15) 0.0149(14) 0.0313(16) 0.0014(12) -0.0013(12) -0.0028(12) C18 0.0252(16) 0.0159(14) 0.0389(18) 0.0064(14) -0.0007(13) -0.0026(12) C19 0.0227(15) 0.0132(13) 0.0275(15) 0.0038(12) -0.0004(12) -0.0014(12) C20 0.0259(16) 0.0209(15) 0.0291(16) 0.0061(13) 0.0055(13) -0.0005(13) C21 0.0238(16) 0.0227(15) 0.0239(15) 0.0007(13) 0.0011(12) 0.0016(13) C22 0.0208(15) 0.0171(14) 0.0254(15) -0.0009(12) -0.0015(12) -0.0013(12) C23 0.0186(14) 0.0125(13) 0.0247(14) 0.0002(11) 0.0020(11) -0.0009(11) C24 0.0229(15) 0.0138(13) 0.0223(14) 0.0001(11) -0.0037(11) 0.0026(11) C25 0.039(2) 0.0222(16) 0.0332(17) -0.0091(14) 0.0027(15) -0.0007(14) C26 0.040(2) 0.037(2) 0.0205(15) -0.0030(14) 0.0032(14) -0.0036(16) C27A 0.054(3) 0.056(3) 0.029(2) -0.002(2) -0.010(2) -0.001(3) C28A 0.059(3) 0.094(5) 0.024(2) -0.004(3) 0.011(2) -0.017(3) C29A 0.089(5) 0.041(3) 0.034(3) -0.011(2) 0.015(3) 0.005(3) C27B 0.060(9) 0.058(9) 0.045(8) -0.001(7) 0.004(7) -0.001(7) C28B 0.058(9) 0.072(9) 0.047(8) -0.017(7) 0.004(7) 0.002(8) C29B 0.056(9) 0.050(8) 0.040(8) -0.012(7) 0.003(7) -0.005(7) C30 0.0194(15) 0.0170(14) 0.0279(15) 0.0004(12) 0.0016(12) -0.0018(11) C31 0.0209(15) 0.0207(15) 0.0256(15) -0.0016(13) 0.0024(12) -0.0044(12) C32 0.0306(19) 0.059(3) 0.0289(17) -0.0071(18) 0.0076(14) -0.0090(18) O30 0.0276(12) 0.0229(11) 0.0230(10) -0.0014(9) -0.0011(9) -0.0015(9) O32 0.0276(13) 0.0586(18) 0.0286(12) 0.0157(12) -0.0012(10) -0.0088(12) O33 0.0238(11) 0.0376(13) 0.0227(11) 0.0096(10) 0.0041(9) -0.0037(10) O34 0.0227(11) 0.0261(11) 0.0196(10) 0.0048(9) 0.0018(8) -0.0072(9) Cl1 0.0781(8) 0.0675(8) 0.0421(5) -0.0210(5) -0.0051(5) 0.0240(6) Cl2 0.1143(12) 0.0887(10) 0.0348(5) 0.0183(6) 0.0023(6) -0.0106(9) Cl3 0.0344(4) 0.0410(5) 0.0404(5) -0.0062(4) 0.0137(4) -0.0078(4) Se1 0.01962(18) 0.01541(17) 0.0395(2) 0.00418(14) -0.00309(13) -0.00312(12) Se2 0.02485(19) 0.01441(17) 0.03583(19) -0.00148(13) 0.00532(14) -0.00775(12) _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 C1 C2 1.389(4) . ? C1 C6 1.396(4) . ? C1 C31 1.504(4) . ? C2 C3 1.399(4) . ? C2 H2 0.9500 . ? C3 C4 1.386(5) . ? C3 C13 1.531(4) . ? C4 C5 1.397(4) . ? C4 H4 0.9500 . ? C5 C6 1.394(4) . ? C5 C17 1.499(4) . ? C6 O34 1.387(4) . ? C7 O34 1.426(4) . ? C7 C8 1.514(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O32 1.200(4) . ? C8 O33 1.333(4) . ? C9 O33 1.490(4) . ? C9 C10 1.511(5) . ? C9 C11 1.511(5) . ? C9 C12 1.520(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.512(6) . ? C13 C16 1.532(6) . ? C13 C15 1.535(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Se1 1.969(3) 3_665 ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.498(4) . ? C18 Se1 1.964(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C24 1.385(5) . ? C19 C20 1.397(5) . ? C20 C21 1.385(5) . ? C20 H20 0.9500 . ? C21 C22 1.399(5) . ? C21 C26 1.535(4) . ? C22 C23 1.391(4) . ? C22 H22 0.9500 . ? C23 C24 1.401(4) . ? C23 C30 1.504(4) . ? C24 O30 1.389(4) . ? C25 O30 1.432(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C29A 1.516(7) . ? C26 C27B 1.519(10) . ? C26 C28A 1.530(7) . ? C26 C27A 1.532(7) . ? C26 C29B 1.532(9) . ? C26 C28B 1.535(10) . ? C27A H27A 0.9800 . ? C27A H27B 0.9800 . ? C27A H27C 0.9800 . ? C28A H28A 0.9800 . ? C28A H28B 0.9800 . ? C28A H28C 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C27B H27D 0.9800 . ? C27B H27E 0.9800 . ? C27B H27F 0.9800 . ? C28B H28D 0.9800 . ? C28B H28E 0.9800 . ? C28B H28F 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30 Se2 1.949(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 Se2 1.963(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 Cl2 1.758(4) . ? C32 Cl1 1.759(5) . ? C32 Cl3 1.760(4) . ? C32 H32 1.0000 . ? Se1 C17 1.969(3) 3_665 ? 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 C2 C1 C6 118.4(3) . . ? C2 C1 C31 121.0(3) . . ? C6 C1 C31 120.6(3) . . ? C1 C2 C3 122.6(3) . . ? C1 C2 H2 118.7 . . ? C3 C2 H2 118.7 . . ? C4 C3 C2 117.4(3) . . ? C4 C3 C13 123.2(3) . . ? C2 C3 C13 119.4(3) . . ? C3 C4 C5 121.9(3) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 119.0(3) . . ? C6 C5 C17 122.4(3) . . ? C4 C5 C17 118.6(3) . . ? O34 C6 C5 120.4(3) . . ? O34 C6 C1 118.6(3) . . ? C5 C6 C1 120.7(3) . . ? O34 C7 C8 107.4(2) . . ? O34 C7 H7A 110.2 . . ? C8 C7 H7A 110.2 . . ? O34 C7 H7B 110.2 . . ? C8 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? O32 C8 O33 126.5(3) . . ? O32 C8 C7 124.3(3) . . ? O33 C8 C7 109.1(3) . . ? O33 C9 C10 110.8(3) . . ? O33 C9 C11 109.2(3) . . ? C10 C9 C11 112.7(3) . . ? O33 C9 C12 102.0(3) . . ? C10 C9 C12 110.8(3) . . ? C11 C9 C12 110.8(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C3 109.4(3) . . ? C14 C13 C16 109.5(4) . . ? C3 C13 C16 111.5(3) . . ? C14 C13 C15 109.8(4) . . ? C3 C13 C15 109.4(3) . . ? C16 C13 C15 107.3(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C5 C17 Se1 110.7(2) . 3_665 ? C5 C17 H17A 109.5 . . ? Se1 C17 H17A 109.5 3_665 . ? C5 C17 H17B 109.5 . . ? Se1 C17 H17B 109.5 3_665 . ? H17A C17 H17B 108.1 . . ? C19 C18 Se1 110.0(2) . . ? C19 C18 H18A 109.7 . . ? Se1 C18 H18A 109.7 . . ? C19 C18 H18B 109.7 . . ? Se1 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? C24 C19 C20 118.4(3) . . ? C24 C19 C18 120.9(3) . . ? C20 C19 C18 120.6(3) . . ? C21 C20 C19 122.3(3) . . ? C21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C20 C21 C22 117.7(3) . . ? C20 C21 C26 122.7(3) . . ? C22 C21 C26 119.6(3) . . ? C23 C22 C21 121.8(3) . . ? C23 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? C22 C23 C24 118.5(3) . . ? C22 C23 C30 122.8(3) . . ? C24 C23 C30 118.6(3) . . ? C19 C24 O30 120.0(3) . . ? C19 C24 C23 121.3(3) . . ? O30 C24 C23 118.5(3) . . ? O30 C25 H25A 109.5 . . ? O30 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O30 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C29A C26 C27B 138.6(10) . . ? C29A C26 C28A 109.5(5) . . ? C27B C26 C28A 68.1(11) . . ? C29A C26 C27A 109.3(4) . . ? C28A C26 C27A 108.7(4) . . ? C27B C26 C29B 111.0(14) . . ? C28A C26 C29B 131.1(9) . . ? C27A C26 C29B 72.6(11) . . ? C29A C26 C21 109.6(3) . . ? C27B C26 C21 109.3(10) . . ? C28A C26 C21 111.4(3) . . ? C27A C26 C21 108.3(3) . . ? C29B C26 C21 114.1(9) . . ? C29A C26 C28B 68.6(12) . . ? C27B C26 C28B 111.7(16) . . ? C28A C26 C28B 45.5(12) . . ? C27A C26 C28B 142.0(10) . . ? C29B C26 C28B 102.8(15) . . ? C21 C26 C28B 107.8(9) . . ? C26 C27A H27A 109.5 . . ? C26 C27A H27B 109.5 . . ? C26 C27A H27C 109.5 . . ? C26 C28A H28A 109.5 . . ? C26 C28A H28B 109.5 . . ? C26 C28A H28C 109.5 . . ? C26 C29A H29A 109.5 . . ? C26 C29A H29B 109.5 . . ? C26 C29A H29C 109.5 . . ? C26 C27B H27D 109.5 . . ? C26 C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C26 C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C26 C28B H28D 109.5 . . ? C26 C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C26 C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C26 C29B H29D 109.5 . . ? C26 C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C26 C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C23 C30 Se2 116.5(2) . . ? C23 C30 H30A 108.2 . . ? Se2 C30 H30A 108.2 . . ? C23 C30 H30B 108.2 . . ? Se2 C30 H30B 108.2 . . ? H30A C30 H30B 107.3 . . ? C1 C31 Se2 114.1(2) . . ? C1 C31 H31A 108.7 . . ? Se2 C31 H31A 108.7 . . ? C1 C31 H31B 108.7 . . ? Se2 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? Cl2 C32 Cl1 110.3(2) . . ? Cl2 C32 Cl3 108.8(2) . . ? Cl1 C32 Cl3 110.5(2) . . ? Cl2 C32 H32 109.1 . . ? Cl1 C32 H32 109.1 . . ? Cl3 C32 H32 109.1 . . ? C24 O30 C25 113.6(2) . . ? C8 O33 C9 120.6(2) . . ? C6 O34 C7 115.5(2) . . ? C18 Se1 C17 94.46(13) . 3_665 ? C30 Se2 C31 97.39(13) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 71.72 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.909 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.106