# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry # and the Centre National de la Recherche Scientifique 1999 # CCDC Number: 440/128 #====================================================================== data_global #====================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Dr. Regine Herbst-Irmer Institut f\"ur Anorganische Chemie Universit\"at G\"ottingen Tammannstr. 4 37077 G\"ottingen Germany ; _publ_contact_author_phone '049 551 393007' _publ_contact_author_fax '049 551 392582' _publ_contact_author_email rherbst@shelx.uni-ac.gwdg.de _publ_requested_journal 'New Journal of Chemistry' _publ_requested_coeditor_name ? _publ_contact_letter ; Here you find the crystallographic data of the article PB20A/99 JES 9/03798E 'Structural Diversity in Nonafluoromesityl Chemistry' which is accepted for publication in the journal 'New Journal of Chemistry'. Sincerely Regine Herbst-Irmer ; #====================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #====================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Structural Diversity in Nonafluoromesityl Chemistry ; loop_ _publ_author_name _publ_author_address 'Voelker, Heike' ; Institut f\"ur Anorganische Chemie Universit\"at G\"ottingen Tammannstr. 4 37077 G\"ottingen Germany ; 'Labahn, Dieter' ; Institut f\"ur Anorganische Chemie Universit\"at G\"ottingen Tammannstr. 4 37077 G\"ottingen Germany ; 'Bohnen, Frank-Michael' ; Institut f\"ur Anorganische Chemie Universit\"at G\"ottingen Tammannstr. 4 37077 G\"ottingen Germany ; 'Herbst-Irmer, Regine' ; Institut f\"ur Anorganische Chemie Universit\"at G\"ottingen Tammannstr. 4 37077 G\"ottingen Germany ; 'Stalke, Dietmar' ; Anorganisch-Chemisches Institut Universit\"at W\"urzburg Am Hubland 97074 W\"urzburg ; 'Edelmann, Frank T.' ; Chemisches Institut Otto-von-Guericke-Universit\"at Magdeburg Universit\"atsplatz 2 39106 Magdeburg Germany ; 'Roesky, Herbert W.' ; Institut f\"ur Anorganische Chemie Universit\"at G\"ottingen Tammannstr. 4 37077 G\"ottingen Germany ; #====================================================================== data_h _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H17 Cl F9 P' _chemical_formula_weight 482.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 18.136(4) _cell_length_b 11.396(2) _cell_length_c 19.734(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.21(3) _cell_angle_gamma 90.00 _cell_volume 4067.6(14) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_crystal_description blocks _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 0.350 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8444 _exptl_absorpt_correction_T_max 0.8726 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Stoe-Siemens-AED four-circle-diffractometer' _diffrn_measurement_method 'Profile data from 2theta/omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% ? _diffrn_reflns_number 10388 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.03 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5290 _reflns_number_gt 4212 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHELXTL-Plus' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0393P)^2^+4.3096P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5290 _refine_ls_number_parameters 571 _refine_ls_number_restraints 828 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.340 _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 P1 P 0.22534(6) 0.16464(9) 0.12246(5) 0.0270(3) Uani 1 1 d . . . Cl1 Cl 0.24416(6) 0.00578(9) 0.17343(6) 0.0400(3) Uani 1 1 d . . . C1 C 0.1257(2) 0.1460(3) 0.0864(2) 0.0264(9) Uani 1 1 d . . . C3 C -0.0098(2) 0.1495(4) 0.0789(2) 0.0338(11) Uani 1 1 d . . . H3 H -0.0545 0.1427 0.1008 0.041 Uiso 1 1 calc R . . C5 C 0.0525(2) 0.1745(4) -0.0219(2) 0.0312(10) Uani 1 1 d . . . H5 H 0.0508 0.1852 -0.0698 0.037 Uiso 1 1 calc R . . C2 C 0.0579(2) 0.1345(4) 0.11650(19) 0.0283(10) Uani 1 1 d D . . C7 C 0.0479(2) 0.1028(4) 0.1889(2) 0.0394(12) Uani 1 1 d D . . F71 F 0.10883(13) 0.0727(2) 0.22585(12) 0.0462(7) Uani 1 1 d D . . F72 F 0.00064(15) 0.0129(3) 0.19217(14) 0.0640(9) Uani 1 1 d D . . F73 F 0.01774(16) 0.1916(3) 0.22214(13) 0.0610(8) Uani 1 1 d D . . C4 C -0.0122(2) 0.1739(4) 0.0107(2) 0.0318(10) Uani 1 1 d D A . C8 C -0.0842(2) 0.1985(4) -0.0285(2) 0.0443(12) Uani 1 1 d D . . F81 F -0.1400(2) 0.2086(12) 0.0092(3) 0.125(4) Uani 0.692(7) 1 d PD A 1 F82 F -0.0836(3) 0.3017(4) -0.0614(4) 0.0665(15) Uani 0.692(7) 1 d PD A 1 F83 F -0.0993(4) 0.1259(5) -0.0776(4) 0.110(3) Uani 0.692(7) 1 d PD A 1 F84 F -0.0827(7) 0.177(2) -0.0940(4) 0.125(4) Uani 0.308(7) 1 d PD A 2 F85 F -0.1356(5) 0.1210(10) -0.0117(8) 0.0665(15) Uani 0.308(7) 1 d PD A 2 F86 F -0.1108(10) 0.3005(11) -0.0173(11) 0.110(3) Uani 0.308(7) 1 d PD A 2 C6 C 0.1199(2) 0.1597(3) 0.0146(2) 0.0273(10) Uani 1 1 d D . . C9 C 0.1863(2) 0.1543(4) -0.0280(2) 0.0386(11) Uani 1 1 d D . . F91 F 0.16465(15) 0.1385(3) -0.09369(12) 0.0657(9) Uani 1 1 d D . . F92 F 0.22706(14) 0.2522(2) -0.02498(14) 0.0512(7) Uani 1 1 d D . . F93 F 0.23122(13) 0.0647(2) -0.01122(12) 0.0441(7) Uani 1 1 d D . . C21 C 0.2322(2) 0.2850(4) 0.1884(2) 0.0274(10) Uani 1 1 d . . . C22 C 0.3158(2) 0.2965(4) 0.1925(2) 0.0294(10) Uani 1 1 d . . . C23 C 0.3344(2) 0.3823(4) 0.1498(2) 0.0284(10) Uani 1 1 d . . . C24 C 0.2669(2) 0.4367(4) 0.11942(19) 0.0275(10) Uani 1 1 d . . . C25 C 0.2065(2) 0.3846(4) 0.1425(2) 0.0270(10) Uani 1 1 d . . . C26 C 0.1999(3) 0.2779(4) 0.2574(2) 0.0434(12) Uani 1 1 d . . . H26A H 0.2187 0.3431 0.2860 0.065 Uiso 1 1 calc R . . H26B H 0.2143 0.2033 0.2793 0.065 Uiso 1 1 calc R . . H26C H 0.1459 0.2825 0.2512 0.065 Uiso 1 1 calc R . . C27 C 0.3665(3) 0.2241(4) 0.2391(2) 0.0461(12) Uani 1 1 d . . . H27A H 0.3574 0.1406 0.2299 0.069 Uiso 1 1 calc R . . H27B H 0.3573 0.2414 0.2864 0.069 Uiso 1 1 calc R . . H27C H 0.4180 0.2429 0.2314 0.069 Uiso 1 1 calc R . . C28 C 0.4099(2) 0.4207(4) 0.1330(2) 0.0428(12) Uani 1 1 d . . . H28A H 0.4172 0.5034 0.1455 0.064 Uiso 1 1 calc R . . H28B H 0.4147 0.4112 0.0842 0.064 Uiso 1 1 calc R . . H28C H 0.4473 0.3727 0.1584 0.064 Uiso 1 1 calc R . . C29 C 0.2677(3) 0.5401(4) 0.0726(2) 0.0402(11) Uani 1 1 d . . . H29A H 0.3001 0.5234 0.0361 0.060 Uiso 1 1 calc R . . H29B H 0.2862 0.6092 0.0981 0.060 Uiso 1 1 calc R . . H29C H 0.2175 0.5554 0.0529 0.060 Uiso 1 1 calc R . . C30 C 0.1278(2) 0.4231(4) 0.1308(2) 0.0389(11) Uani 1 1 d . . . H30A H 0.1004 0.3997 0.1696 0.058 Uiso 1 1 calc R . . H30B H 0.1056 0.3863 0.0893 0.058 Uiso 1 1 calc R . . H30C H 0.1260 0.5086 0.1258 0.058 Uiso 1 1 calc R . . P2 P 0.38995(6) -0.24545(9) 0.32737(5) 0.0265(3) Uani 1 1 d . . . Cl2 Cl 0.39166(6) -0.27287(10) 0.22255(5) 0.0415(3) Uani 1 1 d . . . C11 C 0.2959(2) -0.1737(3) 0.33139(19) 0.0256(9) Uani 1 1 d . . . C13 C 0.1612(2) -0.1511(4) 0.3275(2) 0.0320(10) Uani 1 1 d . . . H13 H 0.1135 -0.1793 0.3126 0.038 Uiso 1 1 calc R . . C15 C 0.2368(2) -0.0067(4) 0.3844(2) 0.0281(10) Uani 1 1 d . . . H15 H 0.2415 0.0648 0.4091 0.034 Uiso 1 1 calc R . . C12 C 0.2239(2) -0.2122(3) 0.3095(2) 0.0287(10) Uani 1 1 d D . . C17 C 0.2022(2) -0.3160(4) 0.2658(2) 0.0422(12) Uani 1 1 d D . . F171 F 0.16097(16) -0.3916(3) 0.30003(18) 0.0701(10) Uani 1 1 d D . . F172 F 0.1594(2) -0.2833(3) 0.21195(16) 0.0855(12) Uani 1 1 d D . . F173 F 0.25588(14) -0.3799(2) 0.24385(13) 0.0476(7) Uani 1 1 d D . . C14 C 0.1677(2) -0.0516(4) 0.3663(2) 0.0299(10) Uani 1 1 d D B . C18 C 0.1005(2) 0.0089(4) 0.3886(2) 0.0403(12) Uani 1 1 d D . . F181 F 0.0947(4) 0.0046(8) 0.4536(2) 0.098(3) Uani 0.773(11) 1 d PD B 1 F182 F 0.03812(18) -0.0286(5) 0.3550(4) 0.0690(19) Uani 0.773(11) 1 d PD B 1 F183 F 0.1008(2) 0.1227(3) 0.3724(3) 0.0505(11) Uani 0.773(11) 1 d PD B 1 F184 F 0.0783(12) 0.1059(15) 0.3589(9) 0.098(3) Uani 0.227(11) 1 d PD B 2 F185 F 0.1129(10) 0.0393(18) 0.4549(5) 0.0690(19) Uani 0.227(11) 1 d PD B 2 F186 F 0.0436(6) -0.0639(11) 0.3946(11) 0.0505(11) Uani 0.227(11) 1 d PD B 2 C16 C 0.2997(2) -0.0654(3) 0.36681(19) 0.0240(9) Uani 1 1 d D . . C19 C 0.3722(2) -0.0035(3) 0.38831(19) 0.0295(10) Uani 1 1 d D . . F191 F 0.41585(12) 0.0093(2) 0.33715(12) 0.0351(6) Uani 1 1 d D . . F192 F 0.41165(12) -0.0582(2) 0.43896(12) 0.0368(6) Uani 1 1 d D . . F193 F 0.36001(13) 0.1050(2) 0.41110(14) 0.0444(7) Uani 1 1 d D . . C41 C 0.3881(2) -0.3924(3) 0.3719(2) 0.0247(9) Uani 1 1 d . . . C42 C 0.4693(2) -0.4227(4) 0.3696(2) 0.0298(10) Uani 1 1 d . . . C43 C 0.5065(2) -0.3833(4) 0.4267(2) 0.0313(10) Uani 1 1 d . . . C44 C 0.4543(2) -0.3321(3) 0.4717(2) 0.0294(10) Uani 1 1 d . . . C45 C 0.3847(2) -0.3406(3) 0.4423(2) 0.0261(9) Uani 1 1 d . . . C46 C 0.3359(2) -0.4936(4) 0.3530(2) 0.0345(10) Uani 1 1 d . . . H46A H 0.3405 -0.5155 0.3055 0.052 Uiso 1 1 calc R . . H46B H 0.2850 -0.4694 0.3590 0.052 Uiso 1 1 calc R . . H46C H 0.3487 -0.5610 0.3824 0.052 Uiso 1 1 calc R . . C47 C 0.4985(3) -0.4907(4) 0.3123(2) 0.0425(12) Uani 1 1 d . . . H47A H 0.4900 -0.4462 0.2699 0.064 Uiso 1 1 calc R . . H47B H 0.4729 -0.5664 0.3077 0.064 Uiso 1 1 calc R . . H47C H 0.5516 -0.5041 0.3217 0.064 Uiso 1 1 calc R . . C48 C 0.5882(2) -0.3908(5) 0.4457(3) 0.0482(13) Uani 1 1 d . . . H48A H 0.5965 -0.4295 0.4900 0.072 Uiso 1 1 calc R . . H48B H 0.6092 -0.3116 0.4483 0.072 Uiso 1 1 calc R . . H48C H 0.6120 -0.4363 0.4113 0.072 Uiso 1 1 calc R . . C49 C 0.4761(3) -0.2805(4) 0.5401(2) 0.0461(12) Uani 1 1 d . . . H49A H 0.5075 -0.2117 0.5347 0.069 Uiso 1 1 calc R . . H49B H 0.5034 -0.3391 0.5683 0.069 Uiso 1 1 calc R . . H49C H 0.4316 -0.2570 0.5620 0.069 Uiso 1 1 calc R . . C50 C 0.3139(2) -0.3115(4) 0.4738(2) 0.0336(10) Uani 1 1 d . . . H50A H 0.2718 -0.3377 0.4437 0.050 Uiso 1 1 calc R . . H50B H 0.3108 -0.2264 0.4805 0.050 Uiso 1 1 calc R . . H50C H 0.3131 -0.3512 0.5178 0.050 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 P1 0.0238(6) 0.0278(6) 0.0295(6) 0.0004(5) 0.0035(5) 0.0028(5) Cl1 0.0403(7) 0.0281(6) 0.0504(7) 0.0065(5) -0.0036(5) 0.0039(5) C1 0.028(2) 0.020(2) 0.031(2) 0.0005(18) 0.0042(18) 0.0035(18) C3 0.024(2) 0.033(3) 0.045(3) -0.004(2) 0.008(2) -0.002(2) C5 0.038(3) 0.027(2) 0.028(2) 0.0025(19) -0.002(2) -0.001(2) C2 0.029(2) 0.027(2) 0.030(2) 0.0003(19) 0.0042(19) -0.0012(19) C7 0.032(3) 0.051(3) 0.037(3) 0.006(2) 0.009(2) -0.001(2) F71 0.0398(16) 0.0647(19) 0.0345(14) 0.0149(13) 0.0057(12) 0.0003(14) F72 0.0563(18) 0.084(2) 0.0524(18) 0.0214(16) 0.0077(14) -0.0319(17) F73 0.0606(19) 0.086(2) 0.0381(16) -0.0026(16) 0.0171(14) 0.0243(17) C4 0.026(2) 0.027(2) 0.042(3) 0.000(2) 0.000(2) -0.0011(19) C8 0.038(3) 0.044(3) 0.050(3) 0.005(3) -0.002(2) -0.004(2) F81 0.027(3) 0.261(12) 0.088(4) 0.067(6) 0.010(2) 0.029(4) F82 0.053(3) 0.044(3) 0.098(4) 0.010(3) -0.029(3) 0.010(2) F83 0.109(5) 0.057(3) 0.149(6) -0.059(4) -0.096(5) 0.033(3) F84 0.027(3) 0.261(12) 0.088(4) 0.067(6) 0.010(2) 0.029(4) F85 0.053(3) 0.044(3) 0.098(4) 0.010(3) -0.029(3) 0.010(2) F86 0.109(5) 0.057(3) 0.149(6) -0.059(4) -0.096(5) 0.033(3) C6 0.030(2) 0.025(2) 0.027(2) 0.0015(18) 0.0048(19) 0.0013(19) C9 0.042(3) 0.045(3) 0.029(3) 0.007(2) 0.006(2) 0.005(3) F91 0.0536(18) 0.120(3) 0.0247(15) -0.0009(16) 0.0085(13) 0.0131(18) F92 0.0420(16) 0.0562(19) 0.0576(17) 0.0221(14) 0.0174(13) -0.0033(14) F93 0.0420(15) 0.0511(17) 0.0402(15) -0.0068(13) 0.0108(12) 0.0133(13) C21 0.030(2) 0.027(2) 0.026(2) 0.0016(19) 0.0046(18) 0.0017(19) C22 0.029(2) 0.029(2) 0.030(2) -0.005(2) -0.0059(19) 0.0036(19) C23 0.025(2) 0.029(2) 0.032(2) -0.008(2) 0.0032(18) 0.0022(19) C24 0.033(2) 0.025(2) 0.025(2) -0.0038(18) 0.0021(19) 0.0001(19) C25 0.025(2) 0.025(2) 0.031(2) -0.0033(19) 0.0017(18) 0.0027(19) C26 0.055(3) 0.044(3) 0.032(3) -0.004(2) 0.012(2) -0.006(2) C27 0.043(3) 0.037(3) 0.055(3) 0.000(2) -0.016(2) 0.006(2) C28 0.032(3) 0.042(3) 0.055(3) -0.008(2) 0.007(2) -0.003(2) C29 0.046(3) 0.037(3) 0.038(3) 0.008(2) 0.004(2) -0.002(2) C30 0.030(3) 0.033(3) 0.054(3) -0.001(2) 0.004(2) 0.006(2) P2 0.0248(6) 0.0251(6) 0.0303(6) 0.0018(5) 0.0059(5) 0.0008(5) Cl2 0.0511(7) 0.0443(7) 0.0305(6) 0.0029(5) 0.0125(5) 0.0050(6) C11 0.026(2) 0.028(2) 0.024(2) 0.0068(19) 0.0027(17) -0.0004(19) C13 0.021(2) 0.032(3) 0.042(3) 0.008(2) -0.0017(19) -0.0028(19) C15 0.031(2) 0.025(2) 0.028(2) 0.0014(19) 0.0040(18) 0.001(2) C12 0.029(2) 0.027(2) 0.029(2) 0.0045(19) -0.0010(19) -0.0013(19) C17 0.037(3) 0.038(3) 0.051(3) -0.005(2) -0.006(2) 0.002(2) F171 0.0549(19) 0.0439(18) 0.114(3) -0.0184(18) 0.0240(18) -0.0214(15) F172 0.109(3) 0.062(2) 0.075(2) -0.0245(18) -0.063(2) 0.023(2) F173 0.0489(16) 0.0442(16) 0.0492(16) -0.0166(13) 0.0008(13) -0.0007(14) C14 0.024(2) 0.032(3) 0.034(2) 0.008(2) 0.0034(19) 0.0008(19) C18 0.028(3) 0.045(3) 0.049(3) -0.001(2) 0.003(2) -0.001(2) F181 0.084(5) 0.172(7) 0.043(2) 0.052(3) 0.046(2) 0.079(4) F182 0.023(2) 0.067(3) 0.117(5) -0.017(4) 0.009(2) 0.0004(19) F183 0.039(2) 0.038(2) 0.076(3) -0.003(2) 0.012(2) 0.0160(17) F184 0.084(5) 0.172(7) 0.043(2) 0.052(3) 0.046(2) 0.079(4) F185 0.023(2) 0.067(3) 0.117(5) -0.017(4) 0.009(2) 0.0004(19) F186 0.039(2) 0.038(2) 0.076(3) -0.003(2) 0.012(2) 0.0160(17) C16 0.025(2) 0.022(2) 0.025(2) 0.0013(18) 0.0022(17) -0.0003(18) C19 0.029(2) 0.021(2) 0.039(3) 0.002(2) 0.004(2) 0.0040(19) F191 0.0282(13) 0.0307(14) 0.0476(15) 0.0077(12) 0.0099(11) -0.0028(11) F192 0.0323(14) 0.0385(14) 0.0383(14) 0.0018(12) -0.0060(11) -0.0027(11) F193 0.0344(14) 0.0281(14) 0.0709(19) -0.0141(13) 0.0041(13) -0.0020(11) C41 0.024(2) 0.022(2) 0.029(2) 0.0010(18) 0.0052(18) 0.0016(18) C42 0.027(2) 0.023(2) 0.040(3) 0.008(2) 0.011(2) 0.0035(19) C43 0.026(2) 0.026(2) 0.042(3) 0.015(2) 0.003(2) -0.0012(19) C44 0.036(3) 0.020(2) 0.032(2) 0.0070(19) 0.000(2) -0.0023(19) C45 0.031(2) 0.019(2) 0.029(2) 0.0028(18) 0.0072(19) 0.0005(18) C46 0.038(3) 0.029(2) 0.037(3) 0.000(2) 0.005(2) -0.004(2) C47 0.043(3) 0.037(3) 0.050(3) 0.003(2) 0.019(2) 0.012(2) C48 0.029(3) 0.049(3) 0.066(3) 0.023(3) 0.000(2) 0.001(2) C49 0.052(3) 0.043(3) 0.041(3) 0.002(2) -0.010(2) -0.008(2) C50 0.039(3) 0.032(2) 0.032(2) 0.002(2) 0.013(2) 0.002(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 P1 C21 1.889(4) . y P1 C1 1.906(4) . y P1 Cl1 2.0870(15) . y C1 C2 1.411(5) . ? C1 C6 1.420(5) . ? C3 C4 1.373(6) . ? C3 C2 1.396(6) . ? C5 C4 1.379(6) . ? C5 C6 1.383(6) . ? C2 C7 1.498(6) . ? C7 F71 1.324(4) . ? C7 F72 1.340(5) . ? C7 F73 1.345(5) . ? C4 C8 1.494(6) . ? C8 F86 1.284(7) . ? C8 F83 1.288(6) . ? C8 F81 1.303(6) . ? C8 F84 1.318(8) . ? C8 F85 1.343(7) . ? C8 F82 1.344(5) . ? C6 C9 1.520(6) . ? C9 F93 1.333(4) . ? C9 F92 1.336(5) . ? C9 F91 1.340(4) . ? C21 C25 1.504(6) . y C21 C22 1.519(6) . y C21 C26 1.523(5) . ? C22 C23 1.348(6) . y C22 C27 1.500(6) . ? C23 C24 1.461(6) . y C23 C28 1.498(6) . ? C24 C25 1.354(6) . y C24 C29 1.498(6) . ? C25 C30 1.495(6) . ? P2 C41 1.893(4) . y P2 C11 1.899(4) . y P2 Cl2 2.0944(15) . y C11 C12 1.415(5) . ? C11 C16 1.417(5) . ? C13 C14 1.369(6) . ? C13 C12 1.400(6) . ? C15 C14 1.376(6) . ? C15 C16 1.388(5) . ? C12 C17 1.499(6) . ? C17 F173 1.314(5) . ? C17 F172 1.323(5) . ? C17 F171 1.355(5) . ? C14 C18 1.494(6) . ? C18 F181 1.295(5) . ? C18 F184 1.301(8) . ? C18 F186 1.336(8) . ? C18 F183 1.336(5) . ? C18 F182 1.339(5) . ? C18 F185 1.357(8) . ? C16 C19 1.525(5) . ? C19 F191 1.335(4) . ? C19 F192 1.339(4) . ? C19 F193 1.340(4) . ? C41 C45 1.515(5) . y C41 C42 1.517(5) . y C41 C46 1.520(6) . ? C42 C43 1.347(6) . y C42 C47 1.499(6) . ? C43 C44 1.467(6) . y C43 C48 1.503(6) . ? C44 C45 1.353(6) . y C44 C49 1.498(6) . ? C45 C50 1.503(5) . ? 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 C21 P1 C1 110.57(18) . . y C21 P1 Cl1 107.32(13) . . y C1 P1 Cl1 101.57(13) . . y C2 C1 C6 115.3(4) . . ? C2 C1 P1 133.2(3) . . ? C6 C1 P1 111.0(3) . . ? C4 C3 C2 120.6(4) . . ? C4 C5 C6 120.4(4) . . ? C3 C2 C1 121.6(4) . . ? C3 C2 C7 111.9(3) . . ? C1 C2 C7 126.5(4) . . ? F71 C7 F72 106.6(3) . . ? F71 C7 F73 106.2(3) . . ? F72 C7 F73 105.5(3) . . ? F71 C7 C2 115.7(3) . . ? F72 C7 C2 110.7(4) . . ? F73 C7 C2 111.4(3) . . ? C3 C4 C5 119.5(4) . . ? C3 C4 C8 120.6(4) . . ? C5 C4 C8 119.9(4) . . ? F86 C8 F83 130.4(7) . . ? F86 C8 F81 60.3(9) . . ? F83 C8 F81 110.7(6) . . ? F86 C8 F84 111.6(9) . . ? F83 C8 F84 33.2(8) . . ? F81 C8 F84 130.4(7) . . ? F86 C8 F85 106.0(9) . . ? F83 C8 F85 69.5(6) . . ? F81 C8 F85 48.4(5) . . ? F84 C8 F85 100.8(8) . . ? F86 C8 F82 46.2(10) . . ? F83 C8 F82 101.9(5) . . ? F81 C8 F82 103.5(5) . . ? F84 C8 F82 71.5(9) . . ? F85 C8 F82 136.5(6) . . ? F86 C8 C4 114.0(6) . . ? F83 C8 C4 113.5(4) . . ? F81 C8 C4 114.1(4) . . ? F84 C8 C4 113.2(7) . . ? F85 C8 C4 110.2(6) . . ? F82 C8 C4 112.1(4) . . ? C5 C6 C1 122.1(4) . . ? C5 C6 C9 115.0(3) . . ? C1 C6 C9 122.9(3) . . ? F93 C9 F92 107.7(3) . . ? F93 C9 F91 105.5(3) . . ? F92 C9 F91 106.1(3) . . ? F93 C9 C6 112.9(3) . . ? F92 C9 C6 113.6(3) . . ? F91 C9 C6 110.6(3) . . ? C25 C21 C22 103.3(3) . . ? C25 C21 C26 117.2(4) . . ? C22 C21 C26 114.0(4) . . ? C25 C21 P1 97.5(3) . . ? C22 C21 P1 96.5(3) . . ? C26 C21 P1 124.5(3) . . ? C23 C22 C27 127.7(4) . . ? C23 C22 C21 108.9(3) . . ? C27 C22 C21 123.4(4) . . ? C22 C23 C24 108.9(3) . . ? C22 C23 C28 128.6(4) . . ? C24 C23 C28 122.5(4) . . ? C25 C24 C23 110.5(4) . . ? C25 C24 C29 126.6(4) . . ? C23 C24 C29 122.8(4) . . ? C24 C25 C30 127.3(4) . . ? C24 C25 C21 108.1(3) . . ? C30 C25 C21 124.4(4) . . ? C41 P2 C11 108.39(17) . . y C41 P2 Cl2 109.19(13) . . y C11 P2 Cl2 100.60(13) . . y C12 C11 C16 115.5(4) . . ? C12 C11 P2 131.7(3) . . ? C16 C11 P2 112.6(3) . . ? C14 C13 C12 121.1(4) . . ? C14 C15 C16 120.4(4) . . ? C13 C12 C11 121.1(4) . . ? C13 C12 C17 110.8(3) . . ? C11 C12 C17 128.1(4) . . ? F173 C17 F172 107.3(4) . . ? F173 C17 F171 105.1(3) . . ? F172 C17 F171 105.4(4) . . ? F173 C17 C12 117.3(4) . . ? F172 C17 C12 110.7(4) . . ? F171 C17 C12 110.2(4) . . ? C13 C14 C15 119.4(4) . . ? C13 C14 C18 120.6(4) . . ? C15 C14 C18 120.0(4) . . ? F181 C18 F184 115.8(10) . . ? F181 C18 F186 76.7(7) . . ? F184 C18 F186 110.7(10) . . ? F181 C18 F183 106.0(5) . . ? F184 C18 F183 22.2(12) . . ? F186 C18 F183 129.9(7) . . ? F181 C18 F182 110.6(4) . . ? F184 C18 F182 80.0(11) . . ? F186 C18 F182 38.4(7) . . ? F183 C18 F182 102.1(4) . . ? F181 C18 F185 22.2(9) . . ? F184 C18 F185 104.0(11) . . ? F186 C18 F185 98.5(9) . . ? F183 C18 F185 88.8(10) . . ? F182 C18 F185 129.3(8) . . ? F181 C18 C14 113.6(4) . . ? F184 C18 C14 119.4(8) . . ? F186 C18 C14 113.0(6) . . ? F183 C18 C14 111.1(4) . . ? F182 C18 C14 112.6(4) . . ? F185 C18 C14 108.7(9) . . ? C15 C16 C11 122.1(4) . . ? C15 C16 C19 114.6(3) . . ? C11 C16 C19 123.3(3) . . ? F191 C19 F192 107.6(3) . . ? F191 C19 F193 106.0(3) . . ? F192 C19 F193 105.8(3) . . ? F191 C19 C16 112.7(3) . . ? F192 C19 C16 113.2(3) . . ? F193 C19 C16 111.1(3) . . ? C45 C41 C42 102.8(3) . . ? C45 C41 C46 116.9(3) . . ? C42 C41 C46 114.1(3) . . ? C45 C41 P2 94.8(2) . . ? C42 C41 P2 97.9(2) . . ? C46 C41 P2 126.1(3) . . ? C43 C42 C47 128.4(4) . . ? C43 C42 C41 109.1(4) . . ? C47 C42 C41 122.5(4) . . ? C42 C43 C44 109.4(4) . . ? C42 C43 C48 127.9(4) . . ? C44 C43 C48 122.7(4) . . ? C45 C44 C43 109.6(4) . . ? C45 C44 C49 126.2(4) . . ? C43 C44 C49 124.2(4) . . ? C44 C45 C50 127.2(4) . . ? C44 C45 C41 108.7(3) . . ? C50 C45 C41 124.0(4) . . ? 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 Cl1 P1 C1 C2 64.8(4) . . . . ? Cl1 P1 C1 C6 -123.2(3) . . . . ? Cl2 P2 C11 C12 57.9(4) . . . . ? Cl2 P2 C11 C16 -126.7(3) . . . . ? C21 P1 C1 C2 -48.9(4) . . . . ? C21 P1 C1 C6 123.1(3) . . . . ? _diffrn_measured_fraction_theta_max .994 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full .994 _refine_diff_density_max .539 _refine_diff_density_min -.298 _refine_diff_density_rms .049 data_rtest _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46.50 H20 F36 Se4 Sn' _chemical_formula_weight 1697.16 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6537 1.4246 '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-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.136(4) _cell_length_b 13.253(3) _cell_length_c 17.247(4) _cell_angle_alpha 88.800(10) _cell_angle_beta 68.280(10) _cell_angle_gamma 75.470(10) _cell_volume 2691.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_crystal_description blocks _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1618 _exptl_absorpt_coefficient_mu 3.340 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.3484 _exptl_absorpt_correction_T_max 0.4340 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 188(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 'Stoe-Siemens-AED four-circle-diffractometer' _diffrn_measurement_method 'Profile data from 2theta/omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% ? _diffrn_reflns_number 9993 _diffrn_reflns_av_R_equivalents 0.0932 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.03 _diffrn_reflns_theta_max 24.11 _reflns_number_total 8494 _reflns_number_gt 6442 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHELXTL-Plus' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0506P)^2^+4.1628P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8494 _refine_ls_number_parameters 976 _refine_ls_number_restraints 4136 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 0.983 _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 Sn1 Sn 0.23362(3) 0.34784(3) 0.21541(2) 0.03326(11) Uani 1 1 d . . . Se1 Se 0.23671(4) 0.53463(4) 0.18352(4) 0.03841(14) Uani 1 1 d . . . Se2 Se 0.38175(5) 0.29239(4) 0.28033(4) 0.04328(15) Uani 1 1 d . . . Se3 Se 0.02707(5) 0.36023(4) 0.30305(4) 0.04510(16) Uani 1 1 d . . . Se4 Se 0.28825(5) 0.21148(5) 0.09563(4) 0.04696(16) Uani 1 1 d . . . C11 C 0.0823(4) 0.5900(4) 0.1903(3) 0.0325(11) Uani 1 1 d . . . C13 C -0.1130(5) 0.6753(4) 0.2685(4) 0.0434(14) Uani 1 1 d . . . H13 H -0.1722 0.7061 0.3199 0.052 Uiso 1 1 calc R . . C15 C -0.0529(5) 0.6279(4) 0.1235(4) 0.0486(15) Uani 1 1 d . . . H15 H -0.0700 0.6263 0.0747 0.058 Uiso 1 1 calc R . . C12 C -0.0037(4) 0.6370(4) 0.2653(3) 0.0355(12) Uani 1 1 d D . . C17 C 0.0177(4) 0.6516(4) 0.3434(3) 0.0420(13) Uani 1 1 d D . . F171 F 0.0526(3) 0.5610(3) 0.3730(2) 0.0545(9) Uani 1 1 d D . . F172 F -0.0752(3) 0.7060(3) 0.4045(2) 0.0564(9) Uani 1 1 d D . . F173 F 0.0973(3) 0.7029(2) 0.33138(19) 0.0491(8) Uani 1 1 d D . . C16 C 0.0573(5) 0.5880(4) 0.1187(3) 0.0394(13) Uani 1 1 d D . . C19 C 0.1475(5) 0.5484(4) 0.0337(3) 0.0510(15) Uani 1 1 d D . . F191 F 0.1034(3) 0.5561(3) -0.0254(2) 0.0679(11) Uani 1 1 d D . . F192 F 0.2241(3) 0.6031(3) 0.0109(2) 0.0668(10) Uani 1 1 d D . . F193 F 0.2011(3) 0.4484(3) 0.0294(2) 0.0560(9) Uani 1 1 d D . . C14 C -0.1369(5) 0.6695(4) 0.1982(4) 0.0480(15) Uani 1 1 d D A . C18 C -0.2553(6) 0.7114(6) 0.2024(5) 0.076(2) Uani 1 1 d D . . F181 F -0.3331(7) 0.7018(19) 0.2755(8) 0.151(5) Uani 0.646(7) 1 d PD A 1 F182 F -0.2813(11) 0.8117(7) 0.1962(16) 0.139(4) Uani 0.646(7) 1 d PD A 1 F183 F -0.2801(8) 0.6700(13) 0.1484(11) 0.131(4) Uani 0.646(7) 1 d PD A 1 F184 F -0.2522(13) 0.746(3) 0.1280(12) 0.151(5) Uani 0.354(7) 1 d PD A 2 F185 F -0.3069(16) 0.6361(13) 0.218(3) 0.139(4) Uani 0.354(7) 1 d PD A 2 F186 F -0.3197(15) 0.786(2) 0.2585(19) 0.131(4) Uani 0.354(7) 1 d PD A 2 C21 C 0.3780(4) 0.4321(4) 0.3140(3) 0.0355(12) Uani 1 1 d . . . C23 C 0.2872(5) 0.5859(5) 0.4094(4) 0.0447(14) Uani 1 1 d . . . H23 H 0.2329 0.6199 0.4616 0.054 Uiso 1 1 calc R . . C25 C 0.4360(5) 0.5904(5) 0.2795(4) 0.0450(14) Uani 1 1 d . . . H25 H 0.4839 0.6279 0.2421 0.054 Uiso 1 1 calc R . . C24 C 0.3520(5) 0.6406(4) 0.3525(4) 0.0466(14) Uani 1 1 d D B . C28 C 0.3311(6) 0.7560(6) 0.3689(5) 0.072(2) Uani 1 1 d D . . F281 F 0.2816(7) 0.8114(4) 0.3216(6) 0.123(3) Uani 0.883(7) 1 d PD B 1 F282 F 0.4231(4) 0.7864(4) 0.3556(5) 0.092(2) Uani 0.883(7) 1 d PD B 1 F283 F 0.2618(7) 0.7908(5) 0.4463(5) 0.125(3) Uani 0.883(7) 1 d PD B 1 F284 F 0.381(5) 0.769(2) 0.421(3) 0.123(3) Uani 0.117(7) 1 d PD B 2 F285 F 0.2244(13) 0.805(2) 0.401(3) 0.092(2) Uani 0.117(7) 1 d PD B 2 F286 F 0.383(4) 0.793(2) 0.2978(15) 0.125(3) Uani 0.117(7) 1 d PD B 2 C22 C 0.3006(4) 0.4816(4) 0.3910(3) 0.0384(12) Uani 1 1 d D . . C27 C 0.2300(5) 0.4247(4) 0.4564(3) 0.0458(14) Uani 1 1 d D . . F271 F 0.1524(3) 0.3969(3) 0.43544(19) 0.0486(8) Uani 1 1 d D . . F272 F 0.2919(3) 0.3384(3) 0.4740(2) 0.0624(10) Uani 1 1 d D . . F273 F 0.1739(3) 0.4837(3) 0.5286(2) 0.0683(11) Uani 1 1 d D . . C26 C 0.4513(4) 0.4869(5) 0.2601(3) 0.0414(13) Uani 1 1 d D . . C29 C 0.5473(5) 0.4365(5) 0.1810(4) 0.0587(17) Uani 1 1 d D . . F291 F 0.6130(4) 0.4993(4) 0.1473(2) 0.0913(15) Uani 1 1 d D . . F292 F 0.5120(3) 0.4111(3) 0.1230(2) 0.0717(11) Uani 1 1 d D . . F293 F 0.6137(3) 0.3488(4) 0.1932(2) 0.0777(12) Uani 1 1 d D . . C31 C 0.0210(4) 0.2220(4) 0.2770(4) 0.0409(13) Uani 1 1 d . . . C33 C 0.0384(6) 0.0419(5) 0.3073(5) 0.067(2) Uani 1 1 d . . . H33 H 0.0535 -0.0128 0.3411 0.081 Uiso 1 1 calc R . . C35 C -0.0108(5) 0.1012(4) 0.1914(5) 0.0588(18) Uani 1 1 d . . . H35 H -0.0302 0.0873 0.1456 0.071 Uiso 1 1 calc R . . C32 C 0.0401(5) 0.1420(5) 0.3275(4) 0.0513(15) Uani 1 1 d D . . C37 C 0.0595(6) 0.1586(5) 0.4069(5) 0.0653(19) Uani 1 1 d D . . F371 F 0.0682(5) 0.0727(4) 0.4468(3) 0.1084(18) Uani 1 1 d D . . F372 F -0.0260(4) 0.2318(4) 0.4600(3) 0.0944(15) Uani 1 1 d D . . F373 F 0.1532(3) 0.1884(3) 0.3929(2) 0.0609(9) Uani 1 1 d D . . C34 C 0.0154(6) 0.0214(4) 0.2395(5) 0.0613(19) Uani 1 1 d D . . C38 C 0.0144(7) -0.0879(6) 0.2196(6) 0.092(3) Uani 1 1 d D . . F381 F 0.1170(4) -0.1524(3) 0.1918(3) 0.0933(14) Uani 1 1 d D . . F382 F -0.0317(7) -0.0936(4) 0.1661(5) 0.174(4) Uani 1 1 d D . . F383 F -0.0457(4) -0.1269(3) 0.2883(4) 0.122(2) Uani 1 1 d D . . C36 C -0.0084(5) 0.2009(4) 0.2104(4) 0.0473(15) Uani 1 1 d D . . C39 C -0.0410(5) 0.2840(4) 0.1568(4) 0.0551(17) Uani 1 1 d D . . F391 F -0.0693(4) 0.2463(3) 0.0998(3) 0.0846(14) Uani 1 1 d D . . F392 F 0.0425(3) 0.3283(3) 0.1154(2) 0.0612(10) Uani 1 1 d D . . F393 F -0.1291(3) 0.3605(3) 0.2014(3) 0.0720(11) Uani 1 1 d D . . C41 C 0.4460(5) 0.1544(4) 0.0790(4) 0.0435(14) Uani 1 1 d . . . C43 C 0.6429(5) 0.1533(6) 0.0110(4) 0.0617(18) Uani 1 1 d . . . H43 H 0.7001 0.1817 -0.0271 0.074 Uiso 1 1 calc R . . C45 C 0.5902(6) 0.0300(5) 0.1099(5) 0.0651(19) Uani 1 1 d . . . H45 H 0.6119 -0.0278 0.1391 0.078 Uiso 1 1 calc R . . C42 C 0.5299(5) 0.1936(4) 0.0204(4) 0.0479(15) Uani 1 1 d D . . C47 C 0.5035(5) 0.2768(5) -0.0351(4) 0.0597(17) Uani 1 1 d D . . F471 F 0.5981(4) 0.2983(4) -0.0870(3) 0.0911(14) Uani 1 1 d D . . F472 F 0.4563(3) 0.2455(3) -0.0826(2) 0.0730(11) Uani 1 1 d D . . F473 F 0.4361(3) 0.3662(3) 0.0069(2) 0.0668(10) Uani 1 1 d D . . C44 C 0.6715(5) 0.0741(6) 0.0558(5) 0.068(2) Uani 1 1 d D C . C48 C 0.7934(8) 0.0297(8) 0.0451(6) 0.111(3) Uani 1 1 d D . . F481 F 0.8633(7) 0.0854(12) -0.0018(12) 0.174(5) Uani 0.749(10) 1 d PD C 1 F482 F 0.8078(8) 0.0328(15) 0.1150(7) 0.164(5) Uani 0.749(10) 1 d PD C 1 F483 F 0.8372(7) -0.0649(8) 0.0128(12) 0.156(5) Uani 0.749(10) 1 d PD C 1 F484 F 0.798(2) -0.046(3) 0.095(3) 0.174(5) Uani 0.251(10) 1 d PD C 2 F485 F 0.8539(18) -0.002(4) -0.0340(12) 0.164(5) Uani 0.251(10) 1 d PD C 2 F486 F 0.828(2) 0.102(2) 0.069(3) 0.156(5) Uani 0.251(10) 1 d PD C 2 C46 C 0.4781(5) 0.0695(4) 0.1216(4) 0.0485(15) Uani 1 1 d D . . C49 C 0.3940(6) 0.0177(5) 0.1818(4) 0.0633(18) Uani 1 1 d D . . F491 F 0.4466(4) -0.0625(3) 0.2129(3) 0.0960(14) Uani 1 1 d D . . F492 F 0.3198(3) 0.0824(3) 0.2469(2) 0.0707(11) Uani 1 1 d D . . F493 F 0.3363(4) -0.0198(3) 0.1467(3) 0.0804(12) Uani 1 1 d D . . C1 C 0.654(3) -0.028(2) 0.4145(17) 0.147(7) Uani 0.40 1 d PDU D 1 C2 C 0.591(3) 0.002(2) 0.366(2) 0.160(7) Uani 0.40 1 d PDU D 1 H2 H 0.5448 -0.0408 0.3608 0.192 Uiso 0.40 1 calc PR D 1 C3 C 0.592(3) 0.090(3) 0.3252(19) 0.163(8) Uani 0.40 1 d PDU D 1 H3 H 0.5462 0.1112 0.2933 0.196 Uiso 0.40 1 calc PR D 1 C4 C 0.663(3) 0.150(2) 0.3308(19) 0.164(8) Uani 0.40 1 d PDU D 1 H4 H 0.6728 0.2065 0.2967 0.196 Uiso 0.40 1 calc PR D 1 C5 C 0.718(3) 0.127(2) 0.385(2) 0.158(7) Uani 0.40 1 d PDU D 1 H5 H 0.7560 0.1743 0.3955 0.189 Uiso 0.40 1 calc PR D 1 C6 C 0.717(3) 0.035(3) 0.424(2) 0.152(7) Uani 0.40 1 d PDU D 1 H6 H 0.7605 0.0159 0.4580 0.183 Uiso 0.40 1 calc PR D 1 C7 C 0.647(3) -0.121(3) 0.457(3) 0.182(13) Uani 0.40 1 d PDU D 1 H7A H 0.5953 -0.1532 0.4431 0.273 Uiso 0.40 1 calc PR D 1 H7B H 0.6178 -0.1037 0.5172 0.273 Uiso 0.40 1 calc PR D 1 H7C H 0.7224 -0.1697 0.4385 0.273 Uiso 0.40 1 calc PR D 1 C1' C 0.680(3) -0.010(3) 0.4385(19) 0.150(8) Uani 0.30 1 d PDU E 2 C2' C 0.614(3) -0.040(3) 0.403(2) 0.152(8) Uani 0.30 1 d PDU E 2 H2' H 0.5814 -0.0964 0.4235 0.183 Uiso 0.30 1 calc PR E 2 C3' C 0.597(4) 0.011(4) 0.337(2) 0.163(8) Uani 0.30 1 d PDU E 2 H3' H 0.5496 -0.0090 0.3127 0.195 Uiso 0.30 1 calc PR E 2 C4' C 0.646(5) 0.090(4) 0.307(3) 0.170(9) Uani 0.30 1 d PDU E 2 H4' H 0.6362 0.1228 0.2597 0.204 Uiso 0.30 1 calc PR E 2 C5' C 0.711(4) 0.122(3) 0.343(3) 0.168(9) Uani 0.30 1 d PDU E 2 H5' H 0.7460 0.1765 0.3213 0.201 Uiso 0.30 1 calc PR E 2 C6' C 0.724(5) 0.073(4) 0.411(3) 0.160(8) Uani 0.30 1 d PDU E 2 H6' H 0.7646 0.0978 0.4390 0.192 Uiso 0.30 1 calc PR E 2 C7' C 0.694(4) -0.057(4) 0.510(2) 0.168(14) Uani 0.30 1 d PDU E 2 H7'1 H 0.6563 -0.1140 0.5227 0.252 Uiso 0.30 1 calc PR E 2 H7'2 H 0.6608 -0.0051 0.5578 0.252 Uiso 0.30 1 calc PR E 2 H7'3 H 0.7753 -0.0859 0.4981 0.252 Uiso 0.30 1 calc PR E 2 C1" C 0.655(3) 0.044(3) 0.3584(18) 0.158(7) Uani 0.30 1 d PDU F 3 C2" C 0.601(3) -0.034(3) 0.380(2) 0.160(8) Uani 0.30 1 d PDU F 3 H2" H 0.5496 -0.0411 0.3554 0.192 Uiso 0.30 1 calc PR F 3 C3" C 0.620(4) -0.102(3) 0.437(3) 0.153(8) Uani 0.30 1 d PDU F 3 H3" H 0.5819 -0.1558 0.4513 0.184 Uiso 0.30 1 calc PR F 3 C4" C 0.694(4) -0.092(3) 0.473(2) 0.146(9) Uani 0.30 1 d PDU F 3 H4" H 0.7083 -0.1392 0.5128 0.175 Uiso 0.30 1 calc PR F 3 C5" C 0.749(3) -0.014(3) 0.453(2) 0.148(8) Uani 0.30 1 d PDU F 3 H5" H 0.7993 -0.0059 0.4781 0.177 Uiso 0.30 1 calc PR F 3 C6" C 0.729(4) 0.054(3) 0.395(3) 0.156(7) Uani 0.30 1 d PDU F 3 H6" H 0.7675 0.1074 0.3801 0.187 Uiso 0.30 1 calc PR F 3 C7" C 0.636(5) 0.111(4) 0.297(3) 0.189(14) Uani 0.30 1 d PDU F 3 H7"1 H 0.6800 0.1634 0.2891 0.284 Uiso 0.30 1 calc PR F 3 H7"2 H 0.5554 0.1471 0.3149 0.284 Uiso 0.30 1 calc PR F 3 H7"3 H 0.6608 0.0701 0.2433 0.284 Uiso 0.30 1 calc PR F 3 C61 C 0.567(2) 0.483(3) 0.4427(18) 0.157(11) Uani 0.50 1 d PDU G -1 C62 C 0.507(2) 0.423(3) 0.4953(19) 0.151(10) Uani 0.50 1 d PDU G -1 H62 H 0.5262 0.3494 0.4816 0.181 Uiso 0.50 1 calc PR G -1 C63 C 0.419(3) 0.467(3) 0.568(2) 0.158(11) Uani 0.50 1 d PDU G -1 H63 H 0.3763 0.4251 0.6046 0.190 Uiso 0.50 1 calc PR G -1 C64 C 0.392(3) 0.573(4) 0.586(2) 0.165(12) Uani 0.50 1 d PDU G -1 H64 H 0.3313 0.6039 0.6367 0.197 Uiso 0.50 1 calc PR G -1 C65 C 0.451(3) 0.634(3) 0.534(2) 0.166(11) Uani 0.50 1 d PDU G -1 H65 H 0.4308 0.7075 0.5470 0.199 Uiso 0.50 1 calc PR G -1 C66 C 0.541(3) 0.588(3) 0.462(2) 0.152(10) Uani 0.50 1 d PDU G -1 H66 H 0.5849 0.6299 0.4263 0.183 Uiso 0.50 1 calc PR G -1 C67 C 0.662(3) 0.438(3) 0.3682(17) 0.234(15) Uani 0.50 1 d PDU G -1 H67A H 0.6705 0.3629 0.3624 0.351 Uiso 0.50 1 calc PR G -1 H67B H 0.7310 0.4506 0.3711 0.351 Uiso 0.50 1 calc PR G -1 H67C H 0.6493 0.4704 0.3197 0.351 Uiso 0.50 1 calc PR G -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0328(2) 0.0327(2) 0.0359(2) 0.00284(15) -0.01516(16) -0.00811(15) Se1 0.0338(3) 0.0379(3) 0.0478(3) 0.0109(2) -0.0176(3) -0.0140(2) Se2 0.0434(3) 0.0422(3) 0.0484(3) 0.0024(3) -0.0260(3) -0.0050(3) Se3 0.0365(3) 0.0390(3) 0.0563(4) 0.0020(3) -0.0108(3) -0.0141(2) Se4 0.0422(3) 0.0475(4) 0.0536(4) -0.0114(3) -0.0250(3) -0.0039(3) C11 0.041(3) 0.029(3) 0.039(3) 0.010(2) -0.023(3) -0.017(2) C13 0.035(3) 0.033(3) 0.059(4) 0.002(3) -0.013(3) -0.009(2) C15 0.061(4) 0.041(3) 0.057(4) 0.002(3) -0.036(3) -0.013(3) C12 0.042(3) 0.030(3) 0.042(3) 0.009(2) -0.018(3) -0.018(2) C17 0.046(3) 0.039(3) 0.039(3) 0.005(3) -0.012(3) -0.014(3) F171 0.066(2) 0.051(2) 0.050(2) 0.0196(16) -0.0270(18) -0.0159(17) F172 0.061(2) 0.058(2) 0.0394(19) 0.0038(16) -0.0122(17) -0.0090(18) F173 0.060(2) 0.053(2) 0.0483(19) 0.0051(15) -0.0290(17) -0.0260(17) C16 0.054(3) 0.025(3) 0.047(3) 0.007(2) -0.028(3) -0.009(2) C19 0.072(4) 0.052(4) 0.036(3) 0.005(3) -0.028(3) -0.018(3) F191 0.098(3) 0.065(2) 0.047(2) 0.0038(18) -0.044(2) -0.007(2) F192 0.077(3) 0.074(3) 0.046(2) 0.0123(18) -0.0093(19) -0.035(2) F193 0.069(2) 0.046(2) 0.0444(19) -0.0029(15) -0.0225(17) 0.0021(17) C14 0.040(3) 0.040(3) 0.073(4) -0.001(3) -0.032(3) -0.007(3) C18 0.060(5) 0.065(5) 0.108(7) -0.016(5) -0.041(5) -0.009(4) F181 0.039(4) 0.217(13) 0.169(10) 0.043(10) -0.028(5) -0.002(7) F182 0.073(6) 0.085(6) 0.256(14) 0.014(8) -0.079(8) 0.012(4) F183 0.065(5) 0.167(10) 0.174(10) -0.074(8) -0.085(7) 0.013(5) F184 0.039(4) 0.217(13) 0.169(10) 0.043(10) -0.028(5) -0.002(7) F185 0.073(6) 0.085(6) 0.256(14) 0.014(8) -0.079(8) 0.012(4) F186 0.065(5) 0.167(10) 0.174(10) -0.074(8) -0.085(7) 0.013(5) C21 0.032(3) 0.047(3) 0.036(3) 0.007(2) -0.023(2) -0.012(2) C23 0.042(3) 0.054(4) 0.038(3) -0.001(3) -0.013(3) -0.016(3) C25 0.043(3) 0.062(4) 0.045(3) 0.013(3) -0.022(3) -0.031(3) C24 0.044(3) 0.054(4) 0.050(4) -0.001(3) -0.021(3) -0.021(3) C28 0.074(5) 0.060(5) 0.089(6) 0.004(4) -0.029(5) -0.030(4) F281 0.138(6) 0.059(3) 0.216(8) 0.027(4) -0.115(6) -0.030(4) F282 0.070(3) 0.070(3) 0.147(6) -0.002(3) -0.037(3) -0.043(3) F283 0.122(5) 0.078(4) 0.130(5) -0.038(4) 0.019(4) -0.047(4) F284 0.138(6) 0.059(3) 0.216(8) 0.027(4) -0.115(6) -0.030(4) F285 0.070(3) 0.070(3) 0.147(6) -0.002(3) -0.037(3) -0.043(3) F286 0.122(5) 0.078(4) 0.130(5) -0.038(4) 0.019(4) -0.047(4) C22 0.036(3) 0.049(3) 0.033(3) 0.002(2) -0.014(2) -0.014(3) C27 0.047(3) 0.057(4) 0.035(3) 0.004(3) -0.017(3) -0.015(3) F271 0.0453(18) 0.061(2) 0.0485(19) 0.0157(16) -0.0209(16) -0.0261(16) F272 0.063(2) 0.081(3) 0.052(2) 0.0291(19) -0.0302(19) -0.023(2) F273 0.079(3) 0.088(3) 0.0332(19) -0.0021(18) -0.0027(18) -0.042(2) C26 0.033(3) 0.064(4) 0.036(3) 0.008(3) -0.017(2) -0.020(3) C29 0.053(4) 0.083(5) 0.041(4) -0.008(3) -0.011(3) -0.028(4) F291 0.080(3) 0.128(4) 0.055(2) -0.014(2) 0.012(2) -0.063(3) F292 0.071(3) 0.109(3) 0.037(2) -0.010(2) -0.0168(18) -0.033(2) F293 0.042(2) 0.107(3) 0.068(3) -0.009(2) -0.0155(19) 0.000(2) C31 0.039(3) 0.035(3) 0.055(4) 0.015(3) -0.021(3) -0.018(2) C33 0.078(5) 0.056(4) 0.101(6) 0.040(4) -0.059(5) -0.039(4) C35 0.071(4) 0.036(3) 0.096(5) 0.015(3) -0.058(4) -0.021(3) C32 0.048(4) 0.052(4) 0.069(4) 0.022(3) -0.030(3) -0.028(3) C37 0.076(5) 0.063(5) 0.072(5) 0.029(4) -0.037(4) -0.034(4) F371 0.173(5) 0.112(4) 0.104(4) 0.075(3) -0.092(4) -0.091(4) F372 0.077(3) 0.143(5) 0.057(3) 0.017(3) -0.012(2) -0.039(3) F373 0.067(2) 0.068(2) 0.061(2) 0.0133(18) -0.033(2) -0.026(2) C34 0.071(4) 0.033(3) 0.109(6) 0.019(3) -0.062(4) -0.022(3) C38 0.117(8) 0.050(5) 0.160(9) 0.038(5) -0.100(7) -0.037(5) F381 0.113(4) 0.050(3) 0.122(4) 0.006(2) -0.050(3) -0.021(3) F382 0.282(9) 0.055(3) 0.321(10) 0.037(4) -0.256(8) -0.062(4) F383 0.101(4) 0.048(3) 0.223(7) 0.033(3) -0.055(4) -0.039(3) C36 0.045(3) 0.032(3) 0.074(4) 0.014(3) -0.031(3) -0.013(3) C39 0.060(4) 0.035(3) 0.088(5) 0.020(3) -0.046(4) -0.016(3) F391 0.126(4) 0.062(3) 0.116(4) 0.029(2) -0.098(3) -0.033(2) F392 0.065(2) 0.051(2) 0.081(3) 0.0288(19) -0.039(2) -0.0211(18) F393 0.055(2) 0.058(2) 0.109(3) 0.027(2) -0.044(2) -0.0069(19) C41 0.043(3) 0.044(3) 0.047(3) -0.009(3) -0.025(3) -0.003(3) C43 0.048(4) 0.070(5) 0.064(4) -0.017(4) -0.023(3) -0.005(3) C45 0.073(5) 0.051(4) 0.074(5) -0.009(4) -0.048(4) 0.011(4) C42 0.046(4) 0.049(4) 0.050(4) -0.011(3) -0.024(3) -0.005(3) C47 0.060(4) 0.062(5) 0.053(4) 0.003(3) -0.016(4) -0.016(4) F471 0.073(3) 0.112(4) 0.081(3) 0.030(3) -0.015(2) -0.035(3) F472 0.090(3) 0.085(3) 0.055(2) 0.001(2) -0.043(2) -0.018(2) F473 0.085(3) 0.052(2) 0.066(2) 0.0039(19) -0.036(2) -0.011(2) C44 0.046(4) 0.071(5) 0.088(6) -0.012(4) -0.038(4) 0.002(4) C48 0.073(6) 0.117(9) 0.143(10) 0.002(8) -0.053(7) -0.007(6) F481 0.062(5) 0.197(11) 0.274(15) 0.028(10) -0.086(8) -0.018(6) F482 0.109(6) 0.220(13) 0.189(10) -0.044(9) -0.118(7) 0.011(7) F483 0.063(5) 0.125(7) 0.251(13) -0.078(8) -0.066(7) 0.046(5) F484 0.062(5) 0.197(11) 0.274(15) 0.028(10) -0.086(8) -0.018(6) F485 0.109(6) 0.220(13) 0.189(10) -0.044(9) -0.118(7) 0.011(7) F486 0.063(5) 0.125(7) 0.251(13) -0.078(8) -0.066(7) 0.046(5) C46 0.061(4) 0.037(3) 0.047(4) -0.010(3) -0.027(3) -0.001(3) C49 0.086(5) 0.034(4) 0.067(5) -0.005(3) -0.034(4) -0.001(3) F491 0.125(4) 0.059(3) 0.096(3) 0.024(2) -0.044(3) -0.008(3) F492 0.085(3) 0.062(2) 0.059(2) -0.001(2) -0.019(2) -0.020(2) F493 0.099(3) 0.062(3) 0.089(3) -0.008(2) -0.035(3) -0.035(2) C1 0.159(14) 0.156(14) 0.073(12) -0.008(10) -0.044(10) 0.052(10) C2 0.183(15) 0.173(15) 0.082(15) -0.022(12) -0.061(11) 0.045(12) C3 0.174(18) 0.182(17) 0.090(15) -0.012(12) -0.069(13) 0.060(15) C4 0.176(18) 0.189(17) 0.081(14) 0.004(13) -0.057(13) 0.042(13) C5 0.166(15) 0.184(16) 0.089(15) 0.014(13) -0.059(12) 0.028(13) C6 0.155(14) 0.173(16) 0.082(14) -0.001(11) -0.050(12) 0.045(12) C7 0.18(2) 0.132(18) 0.15(2) 0.003(16) -0.04(2) 0.079(15) C1' 0.160(15) 0.167(16) 0.086(14) -0.009(11) -0.058(11) 0.042(12) C2' 0.180(16) 0.168(16) 0.070(15) -0.029(11) -0.059(12) 0.042(13) C3' 0.188(17) 0.179(18) 0.079(16) -0.018(14) -0.061(13) 0.043(14) C4' 0.176(18) 0.186(18) 0.089(16) -0.011(13) -0.047(13) 0.053(16) C5' 0.166(17) 0.181(17) 0.101(16) 0.002(13) -0.044(14) 0.040(14) C6' 0.154(15) 0.178(18) 0.103(15) -0.008(13) -0.051(12) 0.038(13) C7' 0.19(3) 0.18(3) 0.11(2) -0.002(19) -0.09(2) 0.05(2) C1" 0.168(13) 0.179(14) 0.083(12) -0.012(10) -0.061(10) 0.054(11) C2" 0.179(16) 0.185(17) 0.080(16) -0.035(12) -0.064(12) 0.043(13) C3" 0.169(18) 0.167(18) 0.087(16) -0.031(12) -0.061(14) 0.043(15) C4" 0.163(19) 0.149(19) 0.083(17) -0.034(14) -0.057(13) 0.051(15) C5" 0.143(16) 0.165(19) 0.093(16) -0.010(14) -0.055(12) 0.050(13) C6" 0.157(14) 0.172(17) 0.096(15) -0.010(12) -0.055(11) 0.045(12) C7" 0.18(3) 0.22(3) 0.08(2) -0.002(18) -0.038(18) 0.10(2) C61 0.12(2) 0.25(3) 0.14(3) 0.02(2) -0.097(18) -0.05(2) C62 0.13(3) 0.20(3) 0.19(3) 0.038(19) -0.13(2) -0.042(19) C63 0.13(3) 0.26(3) 0.16(3) 0.06(2) -0.115(19) -0.08(2) C64 0.17(3) 0.27(4) 0.09(2) 0.02(2) -0.09(2) -0.06(2) C65 0.17(3) 0.24(3) 0.15(2) 0.020(19) -0.11(2) -0.08(2) C66 0.14(3) 0.24(3) 0.14(2) 0.048(19) -0.103(19) -0.10(2) C67 0.16(3) 0.42(4) 0.13(3) -0.04(2) -0.092(19) -0.05(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 Sn1 Se1 2.5317(8) . y Sn1 Se3 2.5347(10) . y Sn1 Se2 2.5377(8) . y Sn1 Se4 2.5411(8) . y Se1 C11 1.936(5) . y Se2 C21 1.936(5) . y Se3 C31 1.924(5) . y Se4 C41 1.932(5) . y C11 C16 1.391(7) . ? C11 C12 1.392(7) . ? C13 C14 1.368(8) . ? C13 C12 1.378(7) . ? C15 C14 1.361(8) . ? C15 C16 1.383(8) . ? C12 C17 1.499(7) . ? C17 F172 1.326(6) . ? C17 F171 1.335(6) . ? C17 F173 1.338(5) . ? C16 C19 1.504(8) . ? C19 F192 1.325(6) . ? C19 F193 1.325(6) . ? C19 F191 1.337(6) . ? C14 C18 1.489(9) . ? C18 F183 1.268(8) . ? C18 F186 1.286(11) . ? C18 F182 1.300(9) . ? C18 F185 1.311(11) . ? C18 F181 1.324(9) . ? C18 F184 1.344(11) . ? C21 C22 1.389(7) . ? C21 C26 1.407(7) . ? C23 C24 1.369(8) . ? C23 C22 1.377(8) . ? C25 C26 1.365(8) . ? C25 C24 1.373(8) . ? C24 C28 1.498(9) . ? C28 F285 1.294(13) . ? C28 F282 1.308(7) . ? C28 F286 1.318(13) . ? C28 F283 1.318(8) . ? C28 F281 1.325(8) . ? C28 F284 1.327(13) . ? C22 C27 1.497(7) . ? C27 F272 1.328(6) . ? C27 F271 1.332(6) . ? C27 F273 1.333(6) . ? C26 C29 1.497(8) . ? C29 F291 1.320(6) . ? C29 F292 1.329(6) . ? C29 F293 1.331(7) . ? C31 C32 1.391(8) . ? C31 C36 1.394(8) . ? C33 C34 1.359(9) . ? C33 C32 1.386(9) . ? C35 C36 1.379(8) . ? C35 C34 1.384(8) . ? C32 C37 1.513(9) . ? C37 F371 1.320(6) . ? C37 F373 1.323(7) . ? C37 F372 1.331(7) . ? C34 C38 1.500(9) . ? C38 F382 1.289(8) . ? C38 F381 1.318(8) . ? C38 F383 1.335(8) . ? C36 C39 1.505(8) . ? C39 F391 1.318(6) . ? C39 F393 1.321(6) . ? C39 F392 1.335(6) . ? C41 C46 1.393(8) . ? C41 C42 1.396(8) . ? C43 C44 1.350(10) . ? C43 C42 1.394(8) . ? C45 C46 1.372(9) . ? C45 C44 1.380(10) . ? C42 C47 1.504(8) . ? C47 F472 1.321(6) . ? C47 F473 1.323(6) . ? C47 F471 1.331(7) . ? C44 C48 1.503(10) . ? C48 F483 1.282(9) . ? C48 F482 1.291(10) . ? C48 F486 1.291(13) . ? C48 F485 1.314(12) . ? C48 F484 1.316(13) . ? C48 F481 1.343(10) . ? C46 C49 1.507(9) . ? C49 F493 1.315(7) . ? C49 F492 1.326(7) . ? C49 F491 1.333(6) . ? C1 C2 1.367(14) . ? C1 C6 1.371(14) . ? C1 C7 1.42(2) . ? C2 C3 1.358(14) . ? C3 C4 1.385(14) . ? C4 C5 1.363(14) . ? C5 C6 1.382(14) . ? C1' C2' 1.365(14) . ? C1' C6' 1.369(14) . ? C1' C7' 1.42(2) . ? C2' C3' 1.375(14) . ? C3' C4' 1.367(14) . ? C4' C5' 1.371(14) . ? C5' C6' 1.371(14) . ? C1" C2" 1.363(14) . ? C1" C6" 1.369(14) . ? C1" C7" 1.43(2) . ? C2" C3" 1.363(14) . ? C3" C4" 1.374(15) . ? C4" C5" 1.370(14) . ? C5" C6" 1.374(14) . ? C61 C62 1.363(13) . ? C61 C66 1.365(14) . ? C61 C67 1.43(2) . ? C62 C63 1.365(14) . ? C63 C64 1.373(14) . ? C64 C65 1.356(14) . ? C65 C66 1.370(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 Se1 Sn1 Se3 104.13(2) . . y Se1 Sn1 Se2 103.20(2) . . y Se3 Sn1 Se2 119.66(3) . . y Se1 Sn1 Se4 119.26(3) . . y Se3 Sn1 Se4 105.26(3) . . y Se2 Sn1 Se4 106.25(3) . . y C11 Se1 Sn1 99.75(14) . . y C21 Se2 Sn1 96.32(14) . . y C31 Se3 Sn1 99.76(16) . . y C41 Se4 Sn1 98.84(16) . . y C16 C11 C12 119.2(5) . . ? C16 C11 Se1 120.0(4) . . ? C12 C11 Se1 120.7(4) . . ? C14 C13 C12 120.5(5) . . ? C14 C15 C16 119.9(5) . . ? C13 C12 C11 119.5(5) . . ? C13 C12 C17 117.7(5) . . ? C11 C12 C17 122.7(5) . . ? F172 C17 F171 106.6(4) . . ? F172 C17 F173 106.7(4) . . ? F171 C17 F173 106.4(4) . . ? F172 C17 C12 111.7(4) . . ? F171 C17 C12 112.6(4) . . ? F173 C17 C12 112.4(4) . . ? C15 C16 C11 120.0(5) . . ? C15 C16 C19 117.5(5) . . ? C11 C16 C19 122.4(5) . . ? F192 C19 F193 108.2(5) . . ? F192 C19 F191 106.4(5) . . ? F193 C19 F191 105.7(4) . . ? F192 C19 C16 111.7(5) . . ? F193 C19 C16 113.0(4) . . ? F191 C19 C16 111.5(5) . . ? C15 C14 C13 120.7(5) . . ? C15 C14 C18 119.3(6) . . ? C13 C14 C18 120.0(6) . . ? F183 C18 F186 127.4(9) . . ? F183 C18 F182 106.7(9) . . ? F186 C18 F182 49.9(13) . . ? F183 C18 F185 57.3(12) . . ? F186 C18 F185 105.5(13) . . ? F182 C18 F185 137.8(10) . . ? F183 C18 F181 104.9(9) . . ? F186 C18 F181 54.3(13) . . ? F182 C18 F181 102.3(8) . . ? F185 C18 F181 54.9(12) . . ? F183 C18 F184 52.6(13) . . ? F186 C18 F184 107.1(13) . . ? F182 C18 F184 61.6(13) . . ? F185 C18 F184 109.0(13) . . ? F181 C18 F184 137.7(10) . . ? F183 C18 C14 115.7(7) . . ? F186 C18 C14 116.9(8) . . ? F182 C18 C14 112.7(7) . . ? F185 C18 C14 109.1(9) . . ? F181 C18 C14 113.3(7) . . ? F184 C18 C14 109.0(9) . . ? C22 C21 C26 118.5(5) . . ? C22 C21 Se2 120.7(4) . . ? C26 C21 Se2 120.7(4) . . ? C24 C23 C22 120.1(5) . . ? C26 C25 C24 120.6(5) . . ? C23 C24 C25 120.2(5) . . ? C23 C24 C28 120.3(5) . . ? C25 C24 C28 119.4(5) . . ? F285 C28 F282 132.2(15) . . ? F285 C28 F286 111.3(19) . . ? F282 C28 F286 58(2) . . ? F285 C28 F283 48(2) . . ? F282 C28 F283 106.5(6) . . ? F286 C28 F283 139.2(15) . . ? F285 C28 F281 60(2) . . ? F282 C28 F281 105.6(6) . . ? F286 C28 F281 54(2) . . ? F283 C28 F281 104.4(7) . . ? F285 C28 F284 109.8(19) . . ? F282 C28 F284 50(2) . . ? F286 C28 F284 107.5(18) . . ? F283 C28 F284 65(2) . . ? F281 C28 F284 139.9(15) . . ? F285 C28 C24 113.3(14) . . ? F282 C28 C24 114.1(6) . . ? F286 C28 C24 107.8(14) . . ? F283 C28 C24 112.8(6) . . ? F281 C28 C24 112.6(6) . . ? F284 C28 C24 106.9(14) . . ? C23 C22 C21 120.2(5) . . ? C23 C22 C27 117.9(5) . . ? C21 C22 C27 122.0(5) . . ? F272 C27 F271 107.0(4) . . ? F272 C27 F273 105.6(4) . . ? F271 C27 F273 106.5(4) . . ? F272 C27 C22 112.7(5) . . ? F271 C27 C22 113.4(4) . . ? F273 C27 C22 111.2(5) . . ? C25 C26 C21 119.8(5) . . ? C25 C26 C29 117.5(5) . . ? F291 C29 F292 106.7(5) . . ? F291 C29 F293 106.8(5) . . ? F292 C29 F293 106.3(5) . . ? F291 C29 C26 111.4(5) . . ? F292 C29 C26 112.7(5) . . ? F293 C29 C26 112.5(5) . . ? C32 C31 C36 118.5(5) . . ? C32 C31 Se3 120.2(4) . . ? C36 C31 Se3 121.2(4) . . ? C34 C33 C32 120.6(6) . . ? C36 C35 C34 119.6(6) . . ? C33 C32 C31 120.0(6) . . ? C33 C32 C37 116.7(5) . . ? C31 C32 C37 123.2(5) . . ? F371 C37 F373 106.7(5) . . ? F371 C37 F372 106.8(6) . . ? F373 C37 F372 106.9(5) . . ? F371 C37 C32 112.0(5) . . ? F373 C37 C32 112.8(5) . . ? F372 C37 C32 111.3(6) . . ? C33 C34 C35 120.3(6) . . ? C33 C34 C38 119.1(6) . . ? C35 C34 C38 120.5(6) . . ? F382 C38 F381 108.6(8) . . ? F382 C38 F383 105.9(7) . . ? F381 C38 F383 105.8(6) . . ? F382 C38 C34 113.3(6) . . ? F381 C38 C34 112.3(6) . . ? F383 C38 C34 110.5(7) . . ? C35 C36 C31 120.7(5) . . ? C35 C36 C39 116.5(5) . . ? C31 C36 C39 122.8(5) . . ? F391 C39 F393 106.6(5) . . ? F391 C39 F392 106.4(5) . . ? F393 C39 F392 106.6(4) . . ? F391 C39 C36 111.8(5) . . ? F393 C39 C36 112.0(5) . . ? F392 C39 C36 113.0(5) . . ? C46 C41 C42 119.1(5) . . ? C46 C41 Se4 120.4(5) . . ? C42 C41 Se4 120.4(4) . . ? C44 C43 C42 120.3(7) . . ? C46 C45 C44 120.1(6) . . ? C43 C42 C41 119.5(6) . . ? C43 C42 C47 118.2(6) . . ? C41 C42 C47 122.3(5) . . ? F472 C47 F473 108.5(5) . . ? F472 C47 F471 106.5(5) . . ? F473 C47 F471 106.4(5) . . ? F472 C47 C42 111.3(5) . . ? F473 C47 C42 113.2(5) . . ? F471 C47 C42 110.6(5) . . ? C43 C44 C45 120.8(6) . . ? C43 C44 C48 120.4(7) . . ? C45 C44 C48 118.8(7) . . ? F483 C48 F482 107.0(10) . . ? F483 C48 F486 136.5(13) . . ? F482 C48 F486 56(2) . . ? F483 C48 F485 52.5(19) . . ? F482 C48 F485 138.9(13) . . ? F486 C48 F485 111.0(18) . . ? F483 C48 F484 61(2) . . ? F482 C48 F484 53(2) . . ? F486 C48 F484 107.6(17) . . ? F485 C48 F484 112.7(18) . . ? F483 C48 F481 106.1(10) . . ? F482 C48 F481 101.9(10) . . ? F486 C48 F481 51.2(19) . . ? F485 C48 F481 61.1(19) . . ? F484 C48 F481 137.5(14) . . ? F483 C48 C44 115.0(8) . . ? F482 C48 C44 112.2(8) . . ? F486 C48 C44 108.5(12) . . ? F485 C48 C44 108.9(12) . . ? F484 C48 C44 107.9(12) . . ? F481 C48 C44 113.7(8) . . ? C45 C46 C41 120.0(6) . . ? C45 C46 C49 117.2(6) . . ? C41 C46 C49 122.8(5) . . ? F493 C49 F492 107.6(6) . . ? F493 C49 F491 106.6(5) . . ? F492 C49 F491 106.2(5) . . ? F493 C49 C46 113.0(5) . . ? F492 C49 C46 112.2(5) . . ? F491 C49 C46 110.9(6) . . ? C2 C1 C6 119.1(15) . . ? C2 C1 C7 118.8(18) . . ? C6 C1 C7 122.1(18) . . ? C3 C2 C1 121.6(16) . . ? C2 C3 C4 118.7(17) . . ? C5 C4 C3 120.5(17) . . ? C4 C5 C6 119.0(16) . . ? C1 C6 C5 120.4(16) . . ? C2' C1' C6' 120.4(16) . . ? C2' C1' C7' 120.2(19) . . ? C6' C1' C7' 119.2(19) . . ? C1' C2' C3' 119.3(17) . . ? C4' C3' C2' 119.9(17) . . ? C3' C4' C5' 120.9(18) . . ? C6' C5' C4' 118.6(17) . . ? C1' C6' C5' 120.6(17) . . ? C2" C1" C6" 118.9(16) . . ? C2" C1" C7" 119.9(19) . . ? C6" C1" C7" 121.2(19) . . ? C1" C2" C3" 121.4(17) . . ? C2" C3" C4" 119.6(17) . . ? C5" C4" C3" 119.7(17) . . ? C4" C5" C6" 120.0(17) . . ? C1" C6" C5" 120.5(17) . . ? C62 C61 C66 120.4(15) . . ? C62 C61 C67 120.9(19) . . ? C66 C61 C67 118.7(18) . . ? C61 C62 C63 119.9(16) . . ? C62 C63 C64 119.1(16) . . ? C65 C64 C63 121.4(17) . . ? C64 C65 C66 119.0(16) . . ? C61 C66 C65 120.1(16) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.11 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.685 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.089 data_t _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H4 F18 Te' _chemical_formula_weight 689.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 8.8740(10) _cell_length_b 17.781(2) _cell_length_c 13.3830(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.220(10) _cell_angle_gamma 90.00 _cell_volume 2094.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 55 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_crystal_description blocks _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 1.584 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.5047 _exptl_absorpt_correction_T_max 0.8577 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'Stoe-Siemens-AED four-circle-diffractometer' _diffrn_measurement_method 'Profile data from 2theta/omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% ? _diffrn_reflns_number 3247 _diffrn_reflns_av_R_equivalents 0.0145 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -2 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.07 _diffrn_reflns_theta_max 22.54 _reflns_number_total 2739 _reflns_number_gt 2216 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHELXTL-Plus' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0373P)^2^+5.1633P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2739 _refine_ls_number_parameters 344 _refine_ls_number_restraints 465 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.030 _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 Te1 Te 0.26884(4) 0.03020(2) 0.03051(2) 0.03619(15) Uani 1 1 d . . . C1 C 0.3925(6) 0.0012(3) 0.1739(4) 0.0291(12) Uani 1 1 d . . . C3 C 0.5865(6) 0.0226(4) 0.3158(4) 0.0428(15) Uani 1 1 d . . . H3 H 0.6573 0.0553 0.3530 0.051 Uiso 1 1 calc R . . C5 C 0.4700(6) -0.0983(3) 0.2936(4) 0.0395(14) Uani 1 1 d . . . H5 H 0.4613 -0.1488 0.3156 0.047 Uiso 1 1 calc R . . C2 C 0.4983(6) 0.0484(3) 0.2296(4) 0.0341(14) Uani 1 1 d D . . C7 C 0.5283(6) 0.1276(3) 0.1991(4) 0.0435(15) Uani 1 1 d D . . F71 F 0.4054(4) 0.16988(19) 0.1848(3) 0.0623(11) Uani 1 1 d D . . F72 F 0.6253(4) 0.1625(2) 0.2664(3) 0.0767(13) Uani 1 1 d D . . F73 F 0.5915(6) 0.1299(2) 0.1146(3) 0.0881(14) Uani 1 1 d D . . C4 C 0.5716(6) -0.0500(4) 0.3470(4) 0.0427(15) Uani 1 1 d D A . C8 C 0.6666(7) -0.0776(4) 0.4396(5) 0.063(2) Uani 1 1 d D . . F81 F 0.6280(14) -0.1401(7) 0.4763(10) 0.143(5) Uani 0.667(6) 1 d PD A 1 F82 F 0.8114(8) -0.0827(9) 0.4284(6) 0.112(4) Uani 0.667(6) 1 d PD A 1 F83 F 0.6729(13) -0.0282(6) 0.5159(5) 0.109(3) Uani 0.667(6) 1 d PD A 1 F84 F 0.774(3) -0.0351(13) 0.4758(19) 0.143(5) Uani 0.333(6) 1 d PD A 2 F85 F 0.5766(16) -0.0918(17) 0.5096(12) 0.112(4) Uani 0.333(6) 1 d PD A 2 F86 F 0.722(3) -0.1446(11) 0.4210(11) 0.109(3) Uani 0.333(6) 1 d PD A 2 C6 C 0.3805(6) -0.0729(3) 0.2074(4) 0.0337(13) Uani 1 1 d D . . C9 C 0.2724(6) -0.1287(3) 0.1547(4) 0.0421(15) Uani 1 1 d D . . F91 F 0.2851(4) -0.19641(19) 0.1975(3) 0.0633(11) Uani 1 1 d D . . F92 F 0.2940(4) -0.1394(2) 0.0589(2) 0.0536(9) Uani 1 1 d D . . F93 F 0.1273(3) -0.10951(19) 0.1545(3) 0.0497(9) Uani 1 1 d D . . C11 C 0.1459(5) 0.1322(3) 0.0510(4) 0.0282(12) Uani 1 1 d . . . C13 C 0.0528(6) 0.2495(3) -0.0256(4) 0.0347(13) Uani 1 1 d . . . H13 H 0.0525 0.2856 -0.0781 0.042 Uiso 1 1 calc R . . C15 C -0.0365(6) 0.2087(3) 0.1249(4) 0.0351(14) Uani 1 1 d . . . H15 H -0.0980 0.2166 0.1771 0.042 Uiso 1 1 calc R . . C12 C 0.1436(5) 0.1867(3) -0.0251(4) 0.0325(13) Uani 1 1 d D . . C17 C 0.2379(6) 0.1804(3) -0.1115(4) 0.0413(15) Uani 1 1 d D . . F171 F 0.3854(4) 0.1847(2) -0.0813(3) 0.0578(10) Uani 1 1 d D . . F172 F 0.2061(4) 0.2352(2) -0.1786(3) 0.0684(12) Uani 1 1 d D . . F173 F 0.2133(4) 0.1156(2) -0.1620(2) 0.0517(9) Uani 1 1 d D . . C14 C -0.0376(6) 0.2603(3) 0.0495(4) 0.0326(13) Uani 1 1 d D . . C18 C -0.1408(7) 0.3273(4) 0.0483(4) 0.0498(16) Uani 1 1 d D . . F181 F -0.2856(4) 0.3066(3) 0.0448(4) 0.0898(15) Uani 1 1 d D . . F182 F -0.1314(5) 0.3723(3) -0.0287(3) 0.0867(15) Uani 1 1 d D . . F183 F -0.1130(5) 0.3687(2) 0.1301(3) 0.0733(12) Uani 1 1 d D . . C16 C 0.0524(5) 0.1453(3) 0.1262(4) 0.0303(12) Uani 1 1 d D . . C19 C 0.0416(6) 0.0907(3) 0.2114(4) 0.0395(14) Uani 1 1 d D . . F191 F -0.0540(4) 0.1148(2) 0.2738(2) 0.0600(10) Uani 1 1 d D . . F192 F 0.1705(4) 0.0804(2) 0.2691(2) 0.0611(11) Uani 1 1 d D . . F193 F -0.0086(6) 0.0241(2) 0.1801(3) 0.0765(13) Uani 1 1 d 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 Te1 0.0455(2) 0.0355(2) 0.0268(2) -0.00210(18) 0.00126(15) 0.00803(19) C1 0.028(3) 0.029(3) 0.030(3) -0.001(2) 0.003(2) 0.005(2) C3 0.037(3) 0.052(4) 0.037(3) 0.000(3) -0.004(3) -0.003(3) C5 0.039(3) 0.037(3) 0.044(3) 0.006(3) 0.010(3) 0.005(3) C2 0.027(3) 0.037(4) 0.039(3) -0.005(3) 0.008(2) -0.003(2) C7 0.037(3) 0.042(4) 0.051(4) -0.009(3) 0.003(3) -0.012(3) F71 0.049(2) 0.036(2) 0.097(3) 0.003(2) -0.010(2) -0.0015(18) F72 0.068(3) 0.042(2) 0.109(3) -0.006(2) -0.032(2) -0.019(2) F73 0.125(4) 0.053(3) 0.098(3) 0.005(2) 0.062(3) -0.023(3) C4 0.032(3) 0.059(5) 0.036(3) 0.003(3) -0.001(3) 0.002(3) C8 0.055(5) 0.069(5) 0.059(5) 0.006(4) -0.011(4) 0.006(4) F81 0.112(8) 0.147(9) 0.148(9) 0.116(8) -0.073(7) -0.054(7) F82 0.049(4) 0.199(12) 0.081(5) 0.026(6) -0.017(3) 0.040(6) F83 0.103(6) 0.161(9) 0.052(4) -0.003(5) -0.032(4) 0.038(6) F84 0.112(8) 0.147(9) 0.148(9) 0.116(8) -0.073(7) -0.054(7) F85 0.049(4) 0.199(12) 0.081(5) 0.026(6) -0.017(3) 0.040(6) F86 0.103(6) 0.161(9) 0.052(4) -0.003(5) -0.032(4) 0.038(6) C6 0.032(3) 0.035(4) 0.034(3) 0.001(3) 0.002(2) 0.005(3) C9 0.048(4) 0.030(4) 0.047(4) 0.000(3) 0.000(3) -0.001(3) F91 0.080(3) 0.030(2) 0.076(3) 0.007(2) -0.007(2) -0.0076(19) F92 0.067(2) 0.044(2) 0.048(2) -0.0155(17) 0.0043(17) -0.0001(18) F93 0.040(2) 0.046(2) 0.061(2) -0.0026(18) -0.0020(16) -0.0102(16) C11 0.024(3) 0.031(3) 0.027(3) 0.001(2) -0.004(2) 0.002(2) C13 0.034(3) 0.037(3) 0.031(3) 0.000(3) -0.004(2) -0.002(3) C15 0.031(3) 0.044(4) 0.030(3) -0.008(3) 0.004(2) -0.002(3) C12 0.024(3) 0.039(3) 0.035(3) -0.006(3) 0.003(2) -0.001(3) C17 0.043(4) 0.043(4) 0.039(3) 0.015(3) 0.010(3) 0.003(3) F171 0.040(2) 0.069(3) 0.069(2) 0.011(2) 0.0240(17) -0.0001(18) F172 0.083(3) 0.071(3) 0.059(2) 0.034(2) 0.040(2) 0.029(2) F173 0.065(2) 0.059(2) 0.0331(18) -0.0046(18) 0.0144(16) 0.0106(19) C14 0.030(3) 0.036(3) 0.031(3) -0.006(3) 0.002(2) 0.005(3) C18 0.052(4) 0.055(4) 0.042(4) -0.003(4) 0.005(3) 0.015(3) F181 0.045(2) 0.077(3) 0.146(4) -0.020(3) 0.010(3) 0.023(2) F182 0.117(4) 0.087(3) 0.061(3) 0.026(2) 0.029(2) 0.068(3) F183 0.104(3) 0.055(3) 0.061(2) -0.015(2) 0.010(2) 0.028(2) C16 0.026(3) 0.039(3) 0.025(3) -0.004(3) 0.002(2) -0.004(3) C19 0.040(3) 0.043(4) 0.037(3) -0.006(3) 0.008(3) 0.000(3) F191 0.060(2) 0.078(3) 0.048(2) 0.015(2) 0.0305(18) 0.021(2) F192 0.048(2) 0.094(3) 0.0410(19) 0.025(2) 0.0040(17) 0.017(2) F193 0.139(4) 0.047(3) 0.046(2) 0.002(2) 0.020(2) -0.030(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 Te1 C1 2.151(5) . y Te1 C11 2.151(5) . y C1 C6 1.399(8) . ? C1 C2 1.402(7) . ? C3 C4 1.367(8) . ? C3 C2 1.389(8) . ? C5 C4 1.378(8) . ? C5 C6 1.392(7) . ? C2 C7 1.498(8) . ? C7 F71 1.318(6) . ? C7 F72 1.321(6) . ? C7 F73 1.325(6) . ? C4 C8 1.492(8) . ? C8 F84 1.266(11) . ? C8 F81 1.279(8) . ? C8 F82 1.315(9) . ? C8 F86 1.325(12) . ? C8 F85 1.329(12) . ? C8 F83 1.342(9) . ? C6 C9 1.494(8) . ? C9 F93 1.331(6) . ? C9 F91 1.332(6) . ? C9 F92 1.334(6) . ? C11 C16 1.401(7) . ? C11 C12 1.404(7) . ? C13 C14 1.376(7) . ? C13 C12 1.378(8) . ? C15 C14 1.363(8) . ? C15 C16 1.375(8) . ? C12 C17 1.514(7) . ? C17 F171 1.323(6) . ? C17 F172 1.332(6) . ? C17 F173 1.340(6) . ? C14 C18 1.501(8) . ? C18 F182 1.316(7) . ? C18 F183 1.317(6) . ? C18 F181 1.331(7) . ? C16 C19 1.509(8) . ? C19 F192 1.311(6) . ? C19 F193 1.314(6) . ? C19 F191 1.334(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 C1 Te1 C11 107.37(19) . . y C6 C1 C2 117.8(5) . . ? C6 C1 Te1 117.4(4) . . ? C2 C1 Te1 124.2(4) . . ? C4 C3 C2 120.0(6) . . ? C4 C5 C6 119.6(5) . . ? C3 C2 C1 120.8(5) . . ? C3 C2 C7 115.9(5) . . ? C1 C2 C7 123.3(5) . . ? F71 C7 F72 106.7(5) . . ? F71 C7 F73 106.8(5) . . ? F72 C7 F73 104.9(5) . . ? F71 C7 C2 113.8(4) . . ? F72 C7 C2 112.3(5) . . ? F73 C7 C2 111.8(5) . . ? C3 C4 C5 120.8(5) . . ? C3 C4 C8 119.9(6) . . ? C5 C4 C8 119.3(6) . . ? F84 C8 F81 126.7(10) . . ? F84 C8 F82 52.0(15) . . ? F81 C8 F82 107.2(8) . . ? F84 C8 F86 109.1(13) . . ? F81 C8 F86 54.2(9) . . ? F82 C8 F86 61.6(10) . . ? F84 C8 F85 109.6(14) . . ? F81 C8 F85 49.6(10) . . ? F82 C8 F85 138.5(9) . . ? F86 C8 F85 103.5(12) . . ? F84 C8 F83 50.3(15) . . ? F81 C8 F83 105.3(9) . . ? F82 C8 F83 100.6(7) . . ? F86 C8 F83 138.6(9) . . ? F85 C8 F83 63.8(11) . . ? F84 C8 C4 116.3(9) . . ? F81 C8 C4 117.0(6) . . ? F82 C8 C4 112.7(6) . . ? F86 C8 C4 109.0(8) . . ? F85 C8 C4 108.7(8) . . ? F83 C8 C4 112.5(6) . . ? C5 C6 C1 120.9(5) . . ? C5 C6 C9 116.2(5) . . ? C1 C6 C9 122.9(5) . . ? F93 C9 F91 105.2(5) . . ? F93 C9 F92 106.9(4) . . ? F91 C9 F92 105.6(5) . . ? F93 C9 C6 113.2(5) . . ? F91 C9 C6 112.5(4) . . ? F92 C9 C6 112.8(5) . . ? C16 C11 C12 116.7(5) . . ? C16 C11 Te1 126.0(4) . . ? C12 C11 Te1 116.8(4) . . ? C14 C13 C12 120.2(5) . . ? C14 C15 C16 120.8(5) . . ? C13 C12 C11 121.3(5) . . ? C13 C12 C17 115.8(5) . . ? C11 C12 C17 122.9(5) . . ? F171 C17 F172 106.3(4) . . ? F171 C17 F173 107.2(5) . . ? F172 C17 F173 106.4(4) . . ? F171 C17 C12 112.5(4) . . ? F172 C17 C12 111.8(5) . . ? F173 C17 C12 112.3(4) . . ? C15 C14 C13 119.8(5) . . ? C15 C14 C18 119.3(5) . . ? C13 C14 C18 120.9(5) . . ? F182 C18 F183 106.7(5) . . ? F182 C18 F181 107.3(5) . . ? F183 C18 F181 105.2(5) . . ? F182 C18 C14 113.1(5) . . ? F183 C18 C14 112.6(5) . . ? F181 C18 C14 111.5(5) . . ? C15 C16 C11 121.2(5) . . ? C15 C16 C19 116.5(4) . . ? C11 C16 C19 122.3(5) . . ? F192 C19 F193 107.3(5) . . ? F192 C19 F191 104.6(4) . . ? F193 C19 F191 105.7(5) . . ? F192 C19 C16 113.7(4) . . ? F193 C19 C16 113.0(4) . . ? F191 C19 C16 111.9(5) . . ? _diffrn_measured_fraction_theta_max .993 _diffrn_reflns_theta_full 22.54 _diffrn_measured_fraction_theta_full .993 _refine_diff_density_max .489 _refine_diff_density_min -.429 _refine_diff_density_rms .086 data_a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H8 Ag4 F36' _chemical_formula_weight 1555.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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' 'F' 'F' 0.0171 0.0103 '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 I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 16.5040(10) _cell_length_b 16.5040(10) _cell_length_c 30.677(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8355.9(9) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_crystal_description blocks _exptl_crystal_colour grey _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5888 _exptl_absorpt_coefficient_mu 2.041 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4958 _exptl_absorpt_correction_T_max 0.5796 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Stoe-Siemens-AED four-circle-diffractometer' _diffrn_measurement_method 'Profile data from 2theta/omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% ? _diffrn_reflns_number 4241 _diffrn_reflns_av_R_equivalents 0.0068 _diffrn_reflns_av_sigmaI/netI 0.0097 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 25.10 _reflns_number_total 2281 _reflns_number_gt 2129 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHELXTL-Plus' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0284P)^2^+40.9074P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000054(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2281 _refine_ls_number_parameters 364 _refine_ls_number_restraints 828 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0662 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.145 _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 Ag1 Ag 0.11274(2) 0.72090(2) 0.121954(10) 0.01956(13) Uani 1 1 d . . . Ag2 Ag 0.02824(2) 0.86425(2) 0.115400(10) 0.01931(13) Uani 1 1 d . . . C1 C 0.1585(3) 0.8464(3) 0.10558(13) 0.0184(9) Uani 1 1 d . . . C3 C 0.2711(3) 0.8655(3) 0.05439(14) 0.0262(11) Uani 1 1 d . . . H3 H 0.2906 0.8649 0.0253 0.031 Uiso 1 1 calc R . . C5 C 0.2932(3) 0.8885(3) 0.13033(14) 0.0246(11) Uani 1 1 d . . . H5 H 0.3279 0.9035 0.1537 0.029 Uiso 1 1 calc R . . C2 C 0.1908(3) 0.8464(3) 0.06319(13) 0.0206(10) Uani 1 1 d D . . C7 C 0.1372(3) 0.8291(3) 0.02474(13) 0.0265(12) Uani 1 1 d D . . F71 F 0.17682(18) 0.8206(2) -0.01235(8) 0.0487(9) Uani 1 1 d D . . F72 F 0.0916(2) 0.76370(19) 0.02971(9) 0.0504(10) Uani 1 1 d D . . F73 F 0.08452(18) 0.88878(19) 0.01796(9) 0.0413(8) Uani 1 1 d D . . C4 C 0.3223(3) 0.8853(3) 0.08826(15) 0.0277(11) Uani 1 1 d D A . C8 C 0.4098(3) 0.9007(3) 0.07973(15) 0.0353(13) Uani 1 1 d D . . F81 F 0.4553(4) 0.8412(6) 0.0909(6) 0.083(3) Uani 0.603(5) 1 d PD A 1 F82 F 0.4372(5) 0.9626(8) 0.1028(6) 0.100(3) Uani 0.603(5) 1 d PD A 1 F83 F 0.4286(4) 0.9191(12) 0.0401(2) 0.090(3) Uani 0.603(5) 1 d PD A 1 F84 F 0.4216(6) 0.9719(8) 0.0649(9) 0.083(3) Uani 0.397(5) 1 d PD A 2 F85 F 0.4406(8) 0.8495(13) 0.0514(8) 0.100(3) Uani 0.397(5) 1 d PD A 2 F86 F 0.4548(7) 0.8917(19) 0.1141(3) 0.090(3) Uani 0.397(5) 1 d PD A 2 C6 C 0.2127(3) 0.8697(3) 0.13815(13) 0.0214(10) Uani 1 1 d D . . C9 C 0.1834(3) 0.8767(3) 0.18450(14) 0.0270(11) Uani 1 1 d D . . F91 F 0.24104(19) 0.8986(2) 0.21207(8) 0.0460(9) Uani 1 1 d D . . F92 F 0.1522(2) 0.80758(17) 0.19925(8) 0.0361(8) Uani 1 1 d D . . F93 F 0.12471(18) 0.93257(18) 0.18822(8) 0.0362(7) Uani 1 1 d D . . C11 C 0.0976(3) 0.5901(3) 0.13297(13) 0.0190(10) Uani 1 1 d . . . C13 C 0.1112(3) 0.4773(3) 0.18414(14) 0.0243(11) Uani 1 1 d . . . H13 H 0.1069 0.4576 0.2131 0.029 Uiso 1 1 calc R . . C15 C 0.1445(3) 0.4564(3) 0.10955(14) 0.0235(11) Uani 1 1 d . . . H15 H 0.1628 0.4220 0.0867 0.028 Uiso 1 1 calc R . . C12 C 0.0927(3) 0.5574(3) 0.17508(12) 0.0191(10) Uani 1 1 d D . . C17 C 0.0728(3) 0.6100(3) 0.21374(13) 0.0247(11) Uani 1 1 d D . . F171 F 0.0404(2) 0.56877(19) 0.24614(9) 0.0565(10) Uani 1 1 d D . . F172 F 0.02301(18) 0.67044(19) 0.20516(8) 0.0385(8) Uani 1 1 d D . . F173 F 0.13926(19) 0.6444(2) 0.22955(9) 0.0489(9) Uani 1 1 d D . . C14 C 0.1358(3) 0.4265(3) 0.15129(14) 0.0246(11) Uani 1 1 d D B . C18 C 0.1512(3) 0.3402(3) 0.16030(15) 0.0343(13) Uani 1 1 d D . . F181 F 0.2061(13) 0.3095(10) 0.1334(7) 0.074(2) Uani 0.248(10) 1 d PD B 1 F182 F 0.0889(9) 0.2934(9) 0.1530(10) 0.0687(18) Uani 0.248(10) 1 d PD B 1 F183 F 0.180(2) 0.3219(12) 0.1981(5) 0.104(3) Uani 0.248(10) 1 d PD B 1 F184 F 0.0942(4) 0.3057(3) 0.1838(3) 0.074(2) Uani 0.752(10) 1 d PD B 2 F185 F 0.2171(4) 0.3287(3) 0.1835(3) 0.0687(18) Uani 0.752(10) 1 d PD B 2 F186 F 0.1583(9) 0.2955(4) 0.12561(15) 0.104(3) Uani 0.752(10) 1 d PD B 2 C16 C 0.1265(3) 0.5361(3) 0.10112(13) 0.0195(10) Uani 1 1 d D . . C19 C 0.1404(3) 0.5668(3) 0.05536(13) 0.0263(11) Uani 1 1 d D . . F191 F 0.16890(19) 0.50994(18) 0.02901(8) 0.0418(8) Uani 1 1 d D . . F192 F 0.07390(18) 0.59636(19) 0.03722(8) 0.0369(7) Uani 1 1 d D . . F193 F 0.19547(18) 0.62661(17) 0.05485(8) 0.0352(7) Uani 1 1 d 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 Ag1 0.0214(3) 0.0165(3) 0.02079(18) 0.00076(12) 0.00026(12) -0.0011(2) Ag2 0.0174(3) 0.0203(3) 0.02027(18) -0.00052(12) 0.00149(12) 0.0003(2) C1 0.025(3) 0.007(3) 0.023(2) 0.0015(17) 0.0015(18) 0.006(3) C3 0.029(3) 0.024(3) 0.026(2) 0.001(2) 0.004(2) 0.001(3) C5 0.026(3) 0.017(3) 0.031(2) -0.0029(19) -0.0069(19) 0.005(3) C2 0.025(3) 0.015(3) 0.0221(19) -0.0002(18) 0.0010(18) 0.003(3) C7 0.025(3) 0.033(4) 0.022(2) 0.001(2) 0.0055(19) -0.009(3) F71 0.036(2) 0.089(3) 0.0217(13) -0.0130(14) 0.0058(12) 0.004(2) F72 0.073(3) 0.046(2) 0.0320(14) 0.0106(13) -0.0216(16) -0.032(2) F73 0.040(2) 0.045(2) 0.0385(15) -0.0008(14) -0.0116(13) 0.0122(18) C4 0.024(3) 0.021(3) 0.038(2) 0.006(2) 0.005(2) -0.002(3) C8 0.029(4) 0.037(4) 0.040(3) 0.008(3) -0.001(2) -0.003(3) F81 0.027(4) 0.056(5) 0.166(8) 0.049(5) 0.021(4) 0.004(4) F82 0.038(4) 0.097(7) 0.165(9) -0.069(6) 0.034(5) -0.026(5) F83 0.024(4) 0.196(11) 0.051(3) 0.026(5) 0.008(3) -0.031(6) F84 0.027(4) 0.056(5) 0.166(8) 0.049(5) 0.021(4) 0.004(4) F85 0.038(4) 0.097(7) 0.165(9) -0.069(6) 0.034(5) -0.026(5) F86 0.024(4) 0.196(11) 0.051(3) 0.026(5) 0.008(3) -0.031(6) C6 0.020(3) 0.017(3) 0.026(2) 0.0015(19) 0.0028(19) -0.003(3) C9 0.031(4) 0.026(3) 0.025(2) -0.002(2) -0.005(2) -0.004(3) F91 0.039(2) 0.073(3) 0.0256(13) -0.0103(14) -0.0083(13) -0.0154(19) F92 0.052(2) 0.032(2) 0.0238(12) 0.0050(12) 0.0055(13) -0.0084(18) F93 0.043(2) 0.036(2) 0.0303(13) -0.0083(13) 0.0072(13) 0.0085(18) C11 0.011(3) 0.021(3) 0.026(2) 0.0016(18) -0.0035(17) -0.001(3) C13 0.022(3) 0.026(3) 0.025(2) 0.0005(19) -0.0038(19) 0.001(3) C15 0.018(3) 0.024(3) 0.028(2) -0.007(2) -0.0002(19) -0.002(3) C12 0.013(3) 0.022(3) 0.0219(19) -0.0006(18) 0.0001(18) -0.002(3) C17 0.037(3) 0.020(3) 0.0176(19) 0.0042(19) 0.001(2) 0.010(3) F171 0.100(3) 0.033(2) 0.0361(15) 0.0052(14) 0.0356(17) 0.006(2) F172 0.050(2) 0.040(2) 0.0257(13) -0.0080(13) -0.0056(13) 0.0192(19) F173 0.037(2) 0.065(3) 0.0446(16) -0.0246(16) -0.0153(15) -0.0013(19) C14 0.025(3) 0.020(3) 0.030(2) 0.001(2) -0.005(2) 0.006(3) C18 0.043(4) 0.023(4) 0.037(3) -0.003(2) -0.005(2) 0.010(3) F181 0.064(4) 0.025(3) 0.133(7) 0.032(3) 0.028(4) 0.006(3) F182 0.051(4) 0.038(3) 0.117(5) 0.024(3) -0.035(3) 0.009(3) F183 0.247(11) 0.024(4) 0.039(2) -0.007(2) -0.012(4) 0.040(5) F184 0.064(4) 0.025(3) 0.133(7) 0.032(3) 0.028(4) 0.006(3) F185 0.051(4) 0.038(3) 0.117(5) 0.024(3) -0.035(3) 0.009(3) F186 0.247(11) 0.024(4) 0.039(2) -0.007(2) -0.012(4) 0.040(5) C16 0.016(3) 0.021(3) 0.0218(19) -0.0005(18) -0.0021(18) 0.000(3) C19 0.027(4) 0.029(3) 0.024(2) -0.004(2) 0.002(2) 0.001(3) F191 0.067(2) 0.034(2) 0.0250(13) -0.0062(13) 0.0095(14) 0.0134(18) F192 0.037(2) 0.048(2) 0.0259(13) 0.0076(13) -0.0088(12) 0.0062(18) F193 0.036(2) 0.038(2) 0.0311(13) 0.0035(12) 0.0063(13) -0.0099(18) _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 C11 2.200(5) . y Ag1 C1 2.262(4) . y Ag1 Ag2 2.7255(5) 6_464 y Ag1 Ag2 2.7536(5) . y Ag2 C1 2.191(5) . y Ag2 C11 2.275(4) 6_464 y Ag2 Ag1 2.7255(5) 6_464 ? C1 C6 1.395(6) . ? C1 C2 1.405(6) . ? C3 C4 1.378(7) . ? C3 C2 1.389(6) . ? C5 C4 1.378(6) . ? C5 C6 1.385(6) . ? C2 C7 1.502(6) . ? C7 F71 1.320(5) . ? C7 F72 1.324(5) . ? C7 F73 1.330(6) . ? C4 C8 1.490(7) . ? C8 F84 1.276(9) . ? C8 F81 1.282(7) . ? C8 F83 1.292(7) . ? C8 F86 1.297(9) . ? C8 F85 1.313(10) . ? C8 F82 1.323(8) . ? C6 C9 1.507(6) . ? C9 F91 1.323(5) . ? C9 F92 1.332(5) . ? C9 F93 1.341(5) . ? C11 C12 1.402(6) . ? C11 C16 1.406(6) . ? C11 Ag2 2.275(4) 6_464 ? C13 C14 1.373(6) . ? C13 C12 1.384(6) . ? C15 C16 1.372(6) . ? C15 C14 1.380(6) . ? C12 C17 1.507(6) . ? C17 F171 1.318(5) . ? C17 F172 1.319(5) . ? C17 F173 1.327(5) . ? C14 C18 1.472(7) . ? C18 F183 1.286(11) . ? C18 F186 1.300(6) . ? C18 F182 1.305(11) . ? C18 F185 1.313(6) . ? C18 F184 1.315(7) . ? C18 F181 1.327(12) . ? C16 C19 1.510(6) . ? C19 F192 1.324(5) . ? C19 F191 1.325(5) . ? C19 F193 1.342(5) . ? 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 C11 Ag1 C1 166.19(16) . . y C11 Ag1 Ag2 53.74(12) . 6_464 ? C1 Ag1 Ag2 137.83(11) . 6_464 ? C11 Ag1 Ag2 142.87(12) . . ? C1 Ag1 Ag2 50.66(11) . . ? Ag2 Ag1 Ag2 90.301(13) 6_464 . ? C1 Ag2 C11 166.72(16) . 6_464 y C1 Ag2 Ag1 141.14(11) . 6_464 ? C11 Ag2 Ag1 51.24(12) 6_464 6_464 ? C1 Ag2 Ag1 52.97(11) . . ? C11 Ag2 Ag1 136.89(12) 6_464 . ? Ag1 Ag2 Ag1 89.082(13) 6_464 . ? C6 C1 C2 114.8(4) . . ? C6 C1 Ag2 119.6(3) . . ? C2 C1 Ag2 120.0(3) . . ? C6 C1 Ag1 107.9(3) . . ? C2 C1 Ag1 109.4(3) . . ? Ag2 C1 Ag1 76.38(14) . . y C4 C3 C2 119.5(4) . . ? C4 C5 C6 119.2(4) . . ? C3 C2 C1 122.8(4) . . ? C3 C2 C7 116.9(4) . . ? C1 C2 C7 120.2(4) . . ? F71 C7 F72 107.1(4) . . ? F71 C7 F73 105.5(4) . . ? F72 C7 F73 104.5(4) . . ? F71 C7 C2 113.9(4) . . ? F72 C7 C2 113.6(4) . . ? F73 C7 C2 111.5(4) . . ? C3 C4 C5 120.1(4) . . ? C3 C4 C8 120.1(4) . . ? C5 C4 C8 119.8(4) . . ? F84 C8 F81 135.4(7) . . ? F84 C8 F83 53.8(8) . . ? F81 C8 F83 107.0(7) . . ? F84 C8 F86 108.0(10) . . ? F81 C8 F86 50.2(8) . . ? F83 C8 F86 130.9(7) . . ? F84 C8 F85 107.3(10) . . ? F81 C8 F85 57.2(9) . . ? F83 C8 F85 55.7(8) . . ? F86 C8 F85 104.1(10) . . ? F84 C8 F82 55.1(8) . . ? F81 C8 F82 104.3(7) . . ? F83 C8 F82 103.9(7) . . ? F86 C8 F82 57.1(9) . . ? F85 C8 F82 136.0(7) . . ? F84 C8 C4 111.5(6) . . ? F81 C8 C4 112.9(5) . . ? F83 C8 C4 116.0(5) . . ? F86 C8 C4 113.1(6) . . ? F85 C8 C4 112.4(6) . . ? F82 C8 C4 111.6(5) . . ? C5 C6 C1 123.5(4) . . ? C5 C6 C9 117.0(4) . . ? C1 C6 C9 119.4(4) . . ? F91 C9 F92 107.1(4) . . ? F91 C9 F93 106.1(4) . . ? F92 C9 F93 106.3(4) . . ? F91 C9 C6 113.2(4) . . ? F92 C9 C6 112.2(4) . . ? F93 C9 C6 111.4(4) . . ? C12 C11 C16 114.6(4) . . ? C12 C11 Ag1 121.7(3) . . ? C16 C11 Ag1 118.5(3) . . ? C12 C11 Ag2 107.0(3) . 6_464 ? C16 C11 Ag2 110.8(3) . 6_464 ? Ag1 C11 Ag2 75.02(14) . 6_464 y C14 C13 C12 120.1(4) . . ? C16 C15 C14 119.7(4) . . ? C13 C12 C11 122.6(4) . . ? C13 C12 C17 116.1(4) . . ? C11 C12 C17 121.1(4) . . ? F171 C17 F172 106.8(4) . . ? F171 C17 F173 106.3(4) . . ? F172 C17 F173 105.4(4) . . ? F171 C17 C12 112.6(4) . . ? F172 C17 C12 114.5(3) . . ? F173 C17 C12 110.7(4) . . ? C13 C14 C15 119.5(4) . . ? C13 C14 C18 120.3(4) . . ? C15 C14 C18 120.2(4) . . ? F183 C18 F186 124.8(10) . . ? F183 C18 F182 107.5(13) . . ? F186 C18 F182 66.1(11) . . ? F183 C18 F185 34.5(14) . . ? F186 C18 F185 106.7(6) . . ? F182 C18 F185 131.2(9) . . ? F183 C18 F184 70.4(14) . . ? F186 C18 F184 105.5(6) . . ? F182 C18 F184 43.4(11) . . ? F185 C18 F184 103.4(5) . . ? F183 C18 F181 102.8(12) . . ? F186 C18 F181 38.0(9) . . ? F182 C18 F181 101.8(12) . . ? F185 C18 F181 73.6(11) . . ? F184 C18 F181 131.6(9) . . ? F183 C18 C14 117.4(9) . . ? F186 C18 C14 114.2(5) . . ? F182 C18 C14 113.9(7) . . ? F185 C18 C14 112.6(5) . . ? F184 C18 C14 113.5(4) . . ? F181 C18 C14 111.8(9) . . ? C15 C16 C11 123.3(4) . . ? C15 C16 C19 117.7(4) . . ? C11 C16 C19 119.0(4) . . ? F192 C19 F191 107.4(3) . . ? F192 C19 F193 106.6(4) . . ? F191 C19 F193 105.9(4) . . ? F192 C19 C16 112.9(4) . . ? F191 C19 C16 112.5(4) . . ? F193 C19 C16 111.1(3) . . ? 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 Ag1 Ag2 Ag1 Ag2 -8.351(17) . . 6_464 6_464 ? Ag2 Ag1 Ag2 Ag1 8.438(17) . 6_464 6_464 . ? _diffrn_measured_fraction_theta_max 0.614 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.614 _refine_diff_density_max 0.350 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.061