Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Alan H. Cowley' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of Texas-Austin 1 University Station, A5300 Austin, TX 78701 USA ; _publ_contact_author_phone 512-471-7710 _publ_contact_author_fax 512-471-6822 _publ_contact_author_email cowley@mail.utexas.edu _publ_contact_letter ; Please consider this CIF submission for publication in ; # 2. TITLE AND AUTHOR LIST _publ_section_title ; Group 14 Triple-Decker cations ; _publ_section_synopsis ; ; _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_references ; Allen, F.H. (2002). Acta Cryst. B58, 380-388. Cremer D. & Pople J.A. (1975). J. Am. Chem. Soc. 97, 1358-1367. Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. ; _publ_section_figure_captions ; ; _publ_section_exptl_prep ; ; loop_ _publ_author_name 'A. Cowley' 'Jamie N. Jones' 'Charles L. B. Macdonald' 'Jennifer Moore' data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 276993' _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 B F20, C10 H15 Sn' _chemical_formula_sum 'C34 H15 B F20 Sn' _chemical_formula_weight 932.96 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' B B 0.0013 0.0007 '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' Si Si 0.0817 0.0704 '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 P21/c _symmetry_space_group_name_hall -P2ybc 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 13.442(5) _cell_length_b 14.160(5) _cell_length_c 17.551(5) _cell_angle_alpha 90 _cell_angle_beta 91.929(5) _cell_angle_gamma 90 _cell_volume 3339(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.856 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.904 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8615 _exptl_absorpt_correction_T_max 0.9071 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13883 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7559 _reflns_number_gt 6237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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^)+(0.0149P)^2^+2.5780P] 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 SHELXL _refine_ls_extinction_coef 0.00084(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7559 _refine_ls_number_parameters 511 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0562 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 C1 C 0.26095(16) 0.73962(16) 0.59730(12) 0.0270(5) Uani 1 1 d . . . C2 C 0.31487(15) 0.76398(16) 0.66595(13) 0.0264(5) Uani 1 1 d . . . C3 C 0.28830(17) 0.69851(16) 0.72390(13) 0.0293(5) Uani 1 1 d . . . C4 C 0.21716(18) 0.63425(16) 0.69123(13) 0.0330(6) Uani 1 1 d . . . C5 C 0.20012(18) 0.65951(17) 0.61317(13) 0.0338(6) Uani 1 1 d . . . C6 C 0.27365(18) 0.78503(18) 0.52133(13) 0.0360(6) Uani 1 1 d . . . H6A H 0.2835 0.8531 0.5281 0.054 Uiso 1 1 calc R . . H6B H 0.2140 0.7739 0.4889 0.054 Uiso 1 1 calc R . . H6C H 0.3318 0.7578 0.4972 0.054 Uiso 1 1 calc R . . C7 C 0.39215(16) 0.84037(17) 0.67294(14) 0.0334(6) Uani 1 1 d . . . H7A H 0.4566 0.8153 0.6580 0.050 Uiso 1 1 calc R . . H7B H 0.3973 0.8624 0.7259 0.050 Uiso 1 1 calc R . . H7C H 0.3730 0.8932 0.6395 0.050 Uiso 1 1 calc R . . C8 C 0.33486(19) 0.6912(2) 0.80256(14) 0.0421(6) Uani 1 1 d . . . H8A H 0.2830 0.6790 0.8393 0.063 Uiso 1 1 calc R . . H8B H 0.3688 0.7505 0.8157 0.063 Uiso 1 1 calc R . . H8C H 0.3831 0.6393 0.8041 0.063 Uiso 1 1 calc R . . C9 C 0.1758(2) 0.54847(18) 0.72915(17) 0.0514(7) Uani 1 1 d . . . H9A H 0.1050 0.5420 0.7149 0.077 Uiso 1 1 calc R . . H9B H 0.1836 0.5552 0.7846 0.077 Uiso 1 1 calc R . . H9C H 0.2118 0.4922 0.7127 0.077 Uiso 1 1 calc R . . C10 C 0.1368(2) 0.6044(2) 0.55658(16) 0.0558(8) Uani 1 1 d . . . H10A H 0.1756 0.5520 0.5365 0.084 Uiso 1 1 calc R . . H10B H 0.1150 0.6459 0.5146 0.084 Uiso 1 1 calc R . . H10C H 0.0784 0.5794 0.5818 0.084 Uiso 1 1 calc R . . C20 C 0.24941(15) 0.26267(14) 0.79152(12) 0.0213(5) Uani 1 1 d . . . C21 C 0.18348(16) 0.25359(16) 0.85072(13) 0.0286(5) Uani 1 1 d . . . C22 C 0.18136(18) 0.31229(18) 0.91320(13) 0.0361(6) Uani 1 1 d . . . C23 C 0.2484(2) 0.38468(18) 0.92016(14) 0.0391(6) Uani 1 1 d . . . C24 C 0.31523(19) 0.39794(16) 0.86374(14) 0.0361(6) Uani 1 1 d . . . C25 C 0.31418(16) 0.33787(15) 0.80126(13) 0.0268(5) Uani 1 1 d . . . C30 C 0.30552(14) 0.09186(14) 0.77989(11) 0.0184(4) Uani 1 1 d . . . C31 C 0.25587(14) 0.01606(15) 0.81117(12) 0.0212(4) Uani 1 1 d . . . C32 C 0.29953(16) -0.04776(15) 0.86115(12) 0.0261(5) Uani 1 1 d . . . C33 C 0.39815(17) -0.03887(15) 0.88285(13) 0.0285(5) Uani 1 1 d . . . C34 C 0.45166(15) 0.03488(16) 0.85435(13) 0.0263(5) Uani 1 1 d . . . C35 C 0.40455(15) 0.09759(14) 0.80551(12) 0.0210(4) Uani 1 1 d . . . C40 C 0.32186(14) 0.20536(14) 0.65177(12) 0.0189(4) Uani 1 1 d . . . C41 C 0.29812(15) 0.28586(15) 0.60963(12) 0.0221(5) Uani 1 1 d . . . C42 C 0.34171(16) 0.31119(15) 0.54297(12) 0.0250(5) Uani 1 1 d . . . C43 C 0.41328(15) 0.25345(16) 0.51365(12) 0.0255(5) Uani 1 1 d . . . C44 C 0.43917(15) 0.17218(15) 0.55152(12) 0.0244(5) Uani 1 1 d . . . C45 C 0.39339(14) 0.14954(14) 0.61840(12) 0.0211(4) Uani 1 1 d . . . C50 C 0.14793(14) 0.15021(14) 0.68600(11) 0.0191(4) Uani 1 1 d . . . C51 C 0.13531(14) 0.06621(15) 0.64608(12) 0.0211(5) Uani 1 1 d . . . C52 C 0.04865(16) 0.03857(15) 0.60836(12) 0.0248(5) Uani 1 1 d . . . C53 C -0.03154(15) 0.09873(17) 0.60610(12) 0.0283(5) Uani 1 1 d . . . C54 C -0.02213(15) 0.18496(17) 0.64098(13) 0.0271(5) Uani 1 1 d . . . C55 C 0.06511(15) 0.20857(15) 0.68020(12) 0.0222(5) Uani 1 1 d . . . B B 0.25651(17) 0.17758(16) 0.72677(14) 0.0195(5) Uani 1 1 d . . . F21 F 0.11584(10) 0.18267(10) 0.84864(8) 0.0376(3) Uani 1 1 d . . . F22 F 0.11494(12) 0.29754(12) 0.96812(8) 0.0546(4) Uani 1 1 d . . . F23 F 0.25037(13) 0.44111(11) 0.98179(8) 0.0581(5) Uani 1 1 d . . . F24 F 0.38196(12) 0.46868(10) 0.86932(9) 0.0538(4) Uani 1 1 d . . . F25 F 0.38282(9) 0.35733(9) 0.74886(8) 0.0336(3) Uani 1 1 d . . . F31 F 0.15767(8) -0.00022(9) 0.79415(7) 0.0286(3) Uani 1 1 d . . . F32 F 0.24541(10) -0.11958(9) 0.88880(8) 0.0390(3) Uani 1 1 d . . . F33 F 0.44054(11) -0.10062(10) 0.93215(8) 0.0467(4) Uani 1 1 d . . . F34 F 0.54819(9) 0.04612(10) 0.87502(8) 0.0405(3) Uani 1 1 d . . . F35 F 0.46067(8) 0.17083(8) 0.78190(7) 0.0275(3) Uani 1 1 d . . . F41 F 0.22708(9) 0.34503(9) 0.63448(7) 0.0303(3) Uani 1 1 d . . . F42 F 0.31450(10) 0.39066(10) 0.50579(8) 0.0399(3) Uani 1 1 d . . . F43 F 0.45721(10) 0.27658(10) 0.44834(7) 0.0378(3) Uani 1 1 d . . . F44 F 0.50774(9) 0.11403(9) 0.52277(7) 0.0367(3) Uani 1 1 d . . . F45 F 0.42225(9) 0.06651(8) 0.65035(7) 0.0276(3) Uani 1 1 d . . . F51 F 0.21212(8) 0.00393(8) 0.64380(7) 0.0255(3) Uani 1 1 d . . . F52 F 0.04108(10) -0.04709(9) 0.57512(8) 0.0360(3) Uani 1 1 d . . . F53 F -0.11793(9) 0.07330(11) 0.57132(8) 0.0420(4) Uani 1 1 d . . . F54 F -0.09967(9) 0.24576(11) 0.63780(8) 0.0393(3) Uani 1 1 d . . . F55 F 0.06443(9) 0.29456(9) 0.71438(7) 0.0299(3) Uani 1 1 d . . . Sn Sn 0.140003(11) 0.790682(11) 0.688857(9) 0.02999(7) 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 0.0311(12) 0.0256(12) 0.0244(12) -0.0015(10) 0.0030(9) 0.0039(10) C2 0.0259(11) 0.0268(12) 0.0266(12) -0.0023(10) 0.0029(9) 0.0120(10) C3 0.0360(13) 0.0277(12) 0.0244(12) 0.0000(10) 0.0035(10) 0.0168(10) C4 0.0475(14) 0.0213(12) 0.0305(13) 0.0016(10) 0.0090(11) 0.0097(11) C5 0.0444(14) 0.0282(13) 0.0289(13) -0.0040(10) 0.0046(11) 0.0000(11) C6 0.0419(14) 0.0388(14) 0.0272(13) 0.0049(11) 0.0004(10) -0.0029(12) C7 0.0265(12) 0.0356(14) 0.0381(14) -0.0057(11) -0.0012(10) 0.0052(10) C8 0.0469(15) 0.0510(16) 0.0283(14) 0.0040(12) 0.0000(11) 0.0194(13) C9 0.083(2) 0.0265(13) 0.0455(17) 0.0063(12) 0.0191(15) 0.0043(14) C10 0.074(2) 0.0529(18) 0.0401(16) -0.0089(14) 0.0015(14) -0.0262(16) C20 0.0221(10) 0.0191(11) 0.0221(11) -0.0003(9) -0.0063(8) 0.0053(9) C21 0.0314(12) 0.0288(12) 0.0255(12) -0.0010(10) -0.0017(9) 0.0083(11) C22 0.0437(14) 0.0420(15) 0.0224(13) -0.0016(11) -0.0024(10) 0.0216(12) C23 0.0586(16) 0.0331(14) 0.0243(13) -0.0119(11) -0.0168(12) 0.0261(13) C24 0.0480(15) 0.0195(12) 0.0391(15) -0.0045(11) -0.0247(12) 0.0081(11) C25 0.0307(12) 0.0234(12) 0.0256(12) 0.0020(10) -0.0090(9) 0.0071(10) C30 0.0209(10) 0.0180(10) 0.0162(10) -0.0012(8) 0.0017(8) 0.0012(8) C31 0.0205(10) 0.0237(11) 0.0194(11) -0.0023(9) 0.0006(8) -0.0003(9) C32 0.0363(13) 0.0200(11) 0.0224(12) 0.0027(9) 0.0046(9) -0.0028(10) C33 0.0384(13) 0.0223(12) 0.0244(12) 0.0042(10) -0.0041(10) 0.0091(10) C34 0.0218(11) 0.0286(12) 0.0280(12) -0.0040(10) -0.0050(9) 0.0039(10) C35 0.0213(11) 0.0186(11) 0.0231(11) -0.0015(9) 0.0012(8) -0.0017(9) C40 0.0165(10) 0.0184(10) 0.0217(11) -0.0003(9) -0.0024(8) -0.0043(8) C41 0.0199(10) 0.0213(11) 0.0250(12) -0.0009(9) -0.0007(8) 0.0022(9) C42 0.0281(11) 0.0225(11) 0.0241(12) 0.0058(9) -0.0055(9) -0.0015(9) C43 0.0265(11) 0.0320(12) 0.0182(11) 0.0023(10) 0.0014(9) -0.0093(10) C44 0.0201(11) 0.0278(12) 0.0255(12) -0.0047(10) 0.0029(9) -0.0005(9) C45 0.0196(10) 0.0188(11) 0.0247(12) 0.0010(9) -0.0006(8) -0.0018(9) C50 0.0175(10) 0.0220(11) 0.0178(11) 0.0028(9) 0.0020(8) -0.0016(9) C51 0.0206(11) 0.0219(11) 0.0210(11) 0.0041(9) 0.0023(8) 0.0024(9) C52 0.0295(12) 0.0248(12) 0.0200(11) -0.0017(9) -0.0018(9) -0.0058(10) C53 0.0184(11) 0.0424(14) 0.0238(12) 0.0012(11) -0.0049(9) -0.0052(10) C54 0.0183(11) 0.0390(14) 0.0239(12) 0.0013(10) 0.0007(9) 0.0069(10) C55 0.0196(10) 0.0261(12) 0.0208(11) -0.0018(9) 0.0015(8) 0.0008(9) B 0.0187(11) 0.0189(12) 0.0210(13) 0.0005(10) 0.0013(9) 0.0002(10) F21 0.0369(7) 0.0442(8) 0.0325(8) -0.0018(6) 0.0120(6) -0.0006(7) F22 0.0664(10) 0.0698(11) 0.0283(8) -0.0058(8) 0.0137(7) 0.0270(9) F23 0.0893(12) 0.0478(9) 0.0351(9) -0.0224(7) -0.0267(8) 0.0346(9) F24 0.0716(10) 0.0268(8) 0.0608(11) -0.0110(7) -0.0306(8) -0.0041(7) F25 0.0334(7) 0.0269(7) 0.0399(8) 0.0017(6) -0.0075(6) -0.0079(6) F31 0.0230(6) 0.0327(7) 0.0300(7) 0.0057(6) 0.0006(5) -0.0081(5) F32 0.0491(8) 0.0286(7) 0.0396(8) 0.0141(6) 0.0034(6) -0.0077(6) F33 0.0516(9) 0.0395(8) 0.0482(9) 0.0198(7) -0.0115(7) 0.0100(7) F34 0.0256(7) 0.0460(8) 0.0487(9) 0.0058(7) -0.0132(6) 0.0043(6) F35 0.0205(6) 0.0266(7) 0.0352(7) 0.0041(6) -0.0030(5) -0.0061(5) F41 0.0315(7) 0.0276(7) 0.0320(7) 0.0051(6) 0.0031(5) 0.0110(6) F42 0.0508(8) 0.0352(8) 0.0339(8) 0.0178(6) 0.0034(6) 0.0075(7) F43 0.0435(8) 0.0462(9) 0.0245(7) 0.0066(6) 0.0112(6) -0.0041(7) F44 0.0359(7) 0.0390(8) 0.0363(8) -0.0014(6) 0.0164(6) 0.0069(6) F45 0.0298(6) 0.0216(6) 0.0317(7) 0.0040(5) 0.0079(5) 0.0062(5) F51 0.0268(6) 0.0227(6) 0.0267(7) -0.0028(5) -0.0019(5) 0.0047(5) F52 0.0429(8) 0.0290(7) 0.0352(8) -0.0061(6) -0.0126(6) -0.0049(6) F53 0.0252(7) 0.0591(9) 0.0408(8) -0.0068(7) -0.0135(6) -0.0057(7) F54 0.0218(7) 0.0552(9) 0.0405(8) -0.0083(7) -0.0064(6) 0.0157(6) F55 0.0250(6) 0.0289(7) 0.0357(8) -0.0077(6) -0.0011(5) 0.0082(5) Sn 0.02823(10) 0.02815(10) 0.03386(11) 0.00574(7) 0.00498(6) 0.00677(7) _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 1.427(3) . ? C1 C5 1.431(3) . ? C1 C6 1.495(3) . ? C1 Sn 2.434(2) . ? C2 C3 1.430(3) . ? C2 C7 1.502(3) . ? C2 Sn 2.428(2) . ? C3 C4 1.426(3) . ? C3 C8 1.500(3) . ? C3 Sn 2.444(2) . ? C4 C5 1.427(3) . ? C4 C9 1.501(3) . ? C4 Sn 2.446(2) . ? C5 C10 1.505(4) . ? C5 Sn 2.437(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C20 C25 1.382(3) . ? C20 C21 1.394(3) . ? C20 B 1.661(3) . ? C21 F21 1.354(3) . ? C21 C22 1.377(3) . ? C22 F22 1.352(3) . ? C22 C23 1.367(4) . ? C23 F23 1.344(3) . ? C23 C24 1.372(4) . ? C24 F24 1.346(3) . ? C24 C25 1.388(3) . ? C25 F25 1.353(3) . ? C30 C31 1.387(3) . ? C30 C35 1.393(3) . ? C30 B 1.654(3) . ? C31 F31 1.363(2) . ? C31 C32 1.377(3) . ? C32 F32 1.350(2) . ? C32 C33 1.373(3) . ? C33 F33 1.343(2) . ? C33 C34 1.372(3) . ? C34 F34 1.345(2) . ? C34 C35 1.374(3) . ? C35 F35 1.356(2) . ? C40 C45 1.389(3) . ? C40 C41 1.390(3) . ? C40 B 1.654(3) . ? C41 F41 1.354(2) . ? C41 C42 1.374(3) . ? C42 F42 1.345(2) . ? C42 C43 1.376(3) . ? C43 F43 1.347(2) . ? C43 C44 1.368(3) . ? C44 F44 1.347(2) . ? C44 C45 1.381(3) . ? C45 F45 1.354(2) . ? C50 C55 1.388(3) . ? C50 C51 1.388(3) . ? C50 B 1.650(3) . ? C51 F51 1.359(2) . ? C51 C52 1.377(3) . ? C52 F52 1.348(2) . ? C52 C53 1.373(3) . ? C53 F53 1.343(2) . ? C53 C54 1.370(3) . ? C54 F54 1.352(2) . ? C54 C55 1.381(3) . ? C55 F55 1.357(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 107.7(2) . . ? C2 C1 C6 125.4(2) . . ? C5 C1 C6 126.7(2) . . ? C2 C1 Sn 72.69(12) . . ? C5 C1 Sn 73.04(13) . . ? C6 C1 Sn 124.04(16) . . ? C1 C2 C3 108.2(2) . . ? C1 C2 C7 125.0(2) . . ? C3 C2 C7 126.7(2) . . ? C1 C2 Sn 73.17(12) . . ? C3 C2 Sn 73.55(12) . . ? C7 C2 Sn 123.04(15) . . ? C4 C3 C2 107.9(2) . . ? C4 C3 C8 125.4(2) . . ? C2 C3 C8 126.4(2) . . ? C4 C3 Sn 73.11(13) . . ? C2 C3 Sn 72.30(12) . . ? C8 C3 Sn 125.45(15) . . ? C3 C4 C5 108.0(2) . . ? C3 C4 C9 126.3(2) . . ? C5 C4 C9 125.4(2) . . ? C3 C4 Sn 72.98(12) . . ? C5 C4 Sn 72.68(13) . . ? C9 C4 Sn 125.27(17) . . ? C4 C5 C1 108.1(2) . . ? C4 C5 C10 124.9(2) . . ? C1 C5 C10 126.7(2) . . ? C4 C5 Sn 73.33(13) . . ? C1 C5 Sn 72.79(13) . . ? C10 C5 Sn 124.36(19) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C25 C20 C21 113.1(2) . . ? C25 C20 B 126.36(19) . . ? C21 C20 B 119.70(19) . . ? F21 C21 C22 115.9(2) . . ? F21 C21 C20 119.43(19) . . ? C22 C21 C20 124.6(2) . . ? F22 C22 C23 120.1(2) . . ? F22 C22 C21 120.4(2) . . ? C23 C22 C21 119.5(2) . . ? F23 C23 C22 120.8(2) . . ? F23 C23 C24 120.2(3) . . ? C22 C23 C24 118.9(2) . . ? F24 C24 C23 120.0(2) . . ? F24 C24 C25 120.2(2) . . ? C23 C24 C25 119.8(2) . . ? F25 C25 C20 120.93(19) . . ? F25 C25 C24 115.0(2) . . ? C20 C25 C24 124.0(2) . . ? C31 C30 C35 112.62(18) . . ? C31 C30 B 127.11(17) . . ? C35 C30 B 119.83(17) . . ? F31 C31 C32 114.67(18) . . ? F31 C31 C30 121.30(18) . . ? C32 C31 C30 124.03(19) . . ? F32 C32 C33 119.76(19) . . ? F32 C32 C31 120.00(19) . . ? C33 C32 C31 120.24(19) . . ? F33 C33 C32 120.3(2) . . ? F33 C33 C34 120.9(2) . . ? C32 C33 C34 118.81(19) . . ? F34 C34 C33 120.31(19) . . ? F34 C34 C35 120.79(19) . . ? C33 C34 C35 118.89(19) . . ? F35 C35 C34 115.83(17) . . ? F35 C35 C30 118.78(18) . . ? C34 C35 C30 125.39(19) . . ? C45 C40 C41 113.07(18) . . ? C45 C40 B 126.43(18) . . ? C41 C40 B 119.98(17) . . ? F41 C41 C42 116.01(18) . . ? F41 C41 C40 119.21(18) . . ? C42 C41 C40 124.78(19) . . ? F42 C42 C41 120.98(19) . . ? F42 C42 C43 119.86(19) . . ? C41 C42 C43 119.15(19) . . ? F43 C43 C44 120.40(19) . . ? F43 C43 C42 120.4(2) . . ? C44 C43 C42 119.21(19) . . ? F44 C44 C43 119.90(19) . . ? F44 C44 C45 120.44(19) . . ? C43 C44 C45 119.65(19) . . ? F45 C45 C44 115.08(18) . . ? F45 C45 C40 120.80(18) . . ? C44 C45 C40 124.11(19) . . ? C55 C50 C51 112.91(18) . . ? C55 C50 B 126.00(18) . . ? C51 C50 B 120.77(17) . . ? F51 C51 C52 115.62(18) . . ? F51 C51 C50 119.39(18) . . ? C52 C51 C50 124.98(19) . . ? F52 C52 C53 119.85(19) . . ? F52 C52 C51 120.93(19) . . ? C53 C52 C51 119.2(2) . . ? F53 C53 C54 120.5(2) . . ? F53 C53 C52 120.8(2) . . ? C54 C53 C52 118.64(19) . . ? F54 C54 C53 119.33(19) . . ? F54 C54 C55 120.5(2) . . ? C53 C54 C55 120.2(2) . . ? F55 C55 C54 114.79(18) . . ? F55 C55 C50 121.28(18) . . ? C54 C55 C50 123.9(2) . . ? C50 B C40 101.33(16) . . ? C50 B C30 113.70(17) . . ? C40 B C30 114.26(16) . . ? C50 B C20 113.38(16) . . ? C40 B C20 114.59(17) . . ? C30 B C20 100.23(16) . . ? C2 Sn C1 34.15(7) . . ? C2 Sn C5 56.66(8) . . ? C1 Sn C5 34.17(8) . . ? C2 Sn C3 34.15(8) . . ? C1 Sn C3 56.65(8) . . ? C5 Sn C3 56.47(8) . . ? C2 Sn C4 56.59(8) . . ? C1 Sn C4 56.62(8) . . ? C5 Sn C4 33.99(8) . . ? C3 Sn C4 33.92(8) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.313 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.060 data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 276994' _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _publ_section_figure_captions ; ; _publ_section_exptl_prep ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H30 B2 F40 Pb2' _chemical_formula_sum 'C68 H30 B2 F40 Pb2' _chemical_formula_weight 2042.92 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' B B 0.0013 0.0007 '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' Pb Pb -3.3944 10.1111 '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 -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.642(5) _cell_length_b 11.749(5) _cell_length_c 13.392(5) _cell_angle_alpha 64.003(5) _cell_angle_beta 77.837(5) _cell_angle_gamma 85.223(5) _cell_volume 1609.4(11) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 5.386 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7274 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12396 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.39 _reflns_number_total 7270 _reflns_number_gt 6702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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^)+(0.0163P)^2^+6.4795P] 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 7270 _refine_ls_number_parameters 510 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 C1 C 0.2588(4) 0.1467(4) 0.9565(3) 0.0308(8) Uani 1 1 d . . . C2 C 0.3755(4) 0.1938(4) 0.9324(3) 0.0324(8) Uani 1 1 d . . . C3 C 0.4502(4) 0.1358(4) 0.8682(4) 0.0359(9) Uani 1 1 d . . . C4 C 0.3790(4) 0.0529(4) 0.8537(3) 0.0310(8) Uani 1 1 d . . . C5 C 0.2613(3) 0.0593(4) 0.9085(3) 0.0300(8) Uani 1 1 d . . . C6 C 0.1559(4) 0.1741(5) 1.0316(5) 0.0487(12) Uani 1 1 d . . . H6A H 0.0841 0.1601 1.0139 0.073 Uiso 1 1 calc R . . H6B H 0.1600 0.2606 1.0194 0.073 Uiso 1 1 calc R . . H6C H 0.1578 0.1190 1.1094 0.073 Uiso 1 1 calc R . . C7 C 0.4119(5) 0.2773(5) 0.9794(5) 0.0517(12) Uani 1 1 d . . . H7A H 0.3648 0.3522 0.9595 0.078 Uiso 1 1 calc R . . H7B H 0.4932 0.3007 0.9484 0.078 Uiso 1 1 calc R . . H7C H 0.4009 0.2323 1.0604 0.078 Uiso 1 1 calc R . . C8 C 0.5813(4) 0.1494(6) 0.8330(5) 0.0568(14) Uani 1 1 d . . . H8A H 0.6172 0.0847 0.8910 0.085 Uiso 1 1 calc R . . H8B H 0.6046 0.2312 0.8221 0.085 Uiso 1 1 calc R . . H8C H 0.6060 0.1409 0.7636 0.085 Uiso 1 1 calc R . . C9 C 0.4207(5) -0.0369(5) 0.8007(4) 0.0495(12) Uani 1 1 d . . . H9A H 0.4229 -0.1213 0.8593 0.074 Uiso 1 1 calc R . . H9B H 0.4979 -0.0119 0.7554 0.074 Uiso 1 1 calc R . . H9C H 0.3677 -0.0346 0.7538 0.074 Uiso 1 1 calc R . . C10 C 0.1606(4) -0.0239(4) 0.9254(4) 0.0416(10) Uani 1 1 d . . . H10A H 0.1778 -0.0583 0.8707 0.062 Uiso 1 1 calc R . . H10B H 0.0903 0.0252 0.9158 0.062 Uiso 1 1 calc R . . H10C H 0.1496 -0.0918 1.0003 0.062 Uiso 1 1 calc R . . C20 C 0.7876(4) 0.1166(4) 0.4176(3) 0.0317(8) Uani 1 1 d . . . C21 C 0.6901(4) 0.0533(4) 0.4990(4) 0.0351(9) Uani 1 1 d . . . C22 C 0.6535(4) -0.0659(4) 0.5250(4) 0.0364(9) Uani 1 1 d . . . C23 C 0.7163(4) -0.1312(4) 0.4673(4) 0.0355(9) Uani 1 1 d . . . C24 C 0.8128(4) -0.0744(4) 0.3864(3) 0.0337(9) Uani 1 1 d . . . C25 C 0.8456(4) 0.0468(4) 0.3615(3) 0.0326(9) Uani 1 1 d . . . C30 C 0.9317(4) 0.3288(4) 0.2948(4) 0.0341(9) Uani 1 1 d . . . C31 C 1.0393(4) 0.2712(4) 0.3149(3) 0.0337(9) Uani 1 1 d . . . C32 C 1.1454(4) 0.3152(4) 0.2425(4) 0.0366(9) Uani 1 1 d . . . C33 C 1.1491(4) 0.4257(4) 0.1457(4) 0.0390(10) Uani 1 1 d . . . C34 C 1.0467(4) 0.4907(4) 0.1234(4) 0.0389(10) Uani 1 1 d . . . C35 C 0.9420(4) 0.4419(4) 0.1977(4) 0.0367(10) Uani 1 1 d . . . C40 C 0.8291(3) 0.2852(4) 0.4997(4) 0.0349(9) Uani 1 1 d . . . C41 C 0.8472(4) 0.1921(5) 0.6026(4) 0.0361(9) Uani 1 1 d . . . C42 C 0.8692(4) 0.2162(5) 0.6897(4) 0.0410(11) Uani 1 1 d . . . C43 C 0.8758(4) 0.3388(6) 0.6750(4) 0.0459(12) Uani 1 1 d . . . C44 C 0.8604(4) 0.4355(5) 0.5746(5) 0.0439(12) Uani 1 1 d . . . C45 C 0.8389(3) 0.4073(5) 0.4900(4) 0.0389(10) Uani 1 1 d . . . C50 C 0.6895(4) 0.3344(5) 0.3407(5) 0.0460(12) Uani 1 1 d . . . C51 C 0.6682(5) 0.3358(4) 0.2433(5) 0.0485(13) Uani 1 1 d . . . C52 C 0.5676(6) 0.3853(5) 0.1970(6) 0.069(2) Uani 1 1 d . . . C53 C 0.4822(6) 0.4359(5) 0.2538(8) 0.084(3) Uani 1 1 d . . . C54 C 0.4976(5) 0.4345(6) 0.3505(8) 0.085(3) Uani 1 1 d . . . C55 C 0.5978(5) 0.3823(6) 0.3947(7) 0.070(2) Uani 1 1 d . . . B1 B 0.8102(4) 0.2662(5) 0.3885(4) 0.0356(10) Uani 1 1 d . . . F21 F 0.6237(2) 0.1125(3) 0.5585(2) 0.0472(7) Uani 1 1 d . . . F22 F 0.5570(2) -0.1198(3) 0.6050(2) 0.0461(6) Uani 1 1 d . . . F23 F 0.6813(3) -0.2476(2) 0.4893(2) 0.0510(7) Uani 1 1 d . . . F24 F 0.8734(2) -0.1382(2) 0.3291(2) 0.0445(6) Uani 1 1 d . . . F25 F 0.9389(2) 0.0955(2) 0.2756(2) 0.0388(6) Uani 1 1 d . . . F31 F 1.0416(2) 0.1630(2) 0.4104(2) 0.0385(6) Uani 1 1 d . . . F32 F 1.2454(2) 0.2511(3) 0.2665(2) 0.0483(7) Uani 1 1 d . . . F33 F 1.2511(3) 0.4716(3) 0.0728(2) 0.0543(7) Uani 1 1 d . . . F34 F 1.0495(3) 0.6016(3) 0.0308(2) 0.0500(7) Uani 1 1 d . . . F35 F 0.8466(2) 0.5156(2) 0.1684(2) 0.0469(7) Uani 1 1 d . . . F41 F 0.8449(3) 0.0682(3) 0.6264(2) 0.0448(6) Uani 1 1 d . . . F42 F 0.8835(3) 0.1206(3) 0.7887(2) 0.0549(8) Uani 1 1 d . . . F43 F 0.8975(3) 0.3623(4) 0.7589(3) 0.0710(10) Uani 1 1 d . . . F44 F 0.8673(3) 0.5569(3) 0.5572(3) 0.0599(8) Uani 1 1 d . . . F45 F 0.8261(2) 0.5082(3) 0.3917(3) 0.0488(7) Uani 1 1 d . . . F51 F 0.7500(3) 0.2882(3) 0.1840(2) 0.0538(8) Uani 1 1 d . . . F52 F 0.5570(4) 0.3813(3) 0.1006(3) 0.0954(16) Uani 1 1 d . . . F53 F 0.3868(3) 0.4853(3) 0.2098(5) 0.124(2) Uani 1 1 d . . . F54 F 0.4124(3) 0.4815(5) 0.4064(6) 0.134(3) Uani 1 1 d . . . F55 F 0.5984(3) 0.3805(5) 0.4946(5) 0.111(2) Uani 1 1 d . . . Pb1 Pb 0.310198(16) 0.278105(15) 0.743546(15) 0.04026(6) 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 0.033(2) 0.0266(19) 0.029(2) -0.0104(16) -0.0013(16) -0.0004(15) C2 0.036(2) 0.0280(19) 0.030(2) -0.0093(16) -0.0079(17) -0.0023(16) C3 0.027(2) 0.037(2) 0.036(2) -0.0099(18) -0.0034(17) 0.0011(16) C4 0.034(2) 0.0285(19) 0.0261(19) -0.0093(16) -0.0052(16) 0.0064(16) C5 0.030(2) 0.0270(19) 0.030(2) -0.0112(16) -0.0020(16) -0.0010(15) C6 0.042(3) 0.053(3) 0.059(3) -0.038(3) 0.005(2) 0.002(2) C7 0.059(3) 0.045(3) 0.056(3) -0.023(2) -0.015(3) -0.013(2) C8 0.030(2) 0.071(4) 0.061(3) -0.022(3) -0.006(2) -0.001(2) C9 0.054(3) 0.050(3) 0.047(3) -0.028(2) -0.005(2) 0.015(2) C10 0.046(3) 0.041(2) 0.038(2) -0.018(2) 0.000(2) -0.016(2) C20 0.033(2) 0.043(2) 0.0269(19) -0.0198(18) -0.0159(16) 0.0111(17) C21 0.035(2) 0.051(3) 0.032(2) -0.028(2) -0.0130(17) 0.0121(18) C22 0.032(2) 0.050(3) 0.027(2) -0.0170(19) -0.0083(17) 0.0089(18) C23 0.043(2) 0.031(2) 0.028(2) -0.0101(17) -0.0101(18) 0.0101(18) C24 0.042(2) 0.035(2) 0.0239(19) -0.0139(17) -0.0083(17) 0.0144(18) C25 0.035(2) 0.040(2) 0.0224(18) -0.0128(17) -0.0106(16) 0.0096(17) C30 0.042(2) 0.040(2) 0.033(2) -0.0225(19) -0.0213(18) 0.0103(18) C31 0.044(2) 0.037(2) 0.0253(19) -0.0158(17) -0.0152(17) 0.0093(18) C32 0.042(2) 0.042(2) 0.030(2) -0.0179(19) -0.0164(18) 0.0134(19) C33 0.053(3) 0.042(2) 0.026(2) -0.0177(19) -0.0098(19) 0.005(2) C34 0.062(3) 0.035(2) 0.030(2) -0.0180(18) -0.024(2) 0.009(2) C35 0.048(3) 0.036(2) 0.039(2) -0.0216(19) -0.028(2) 0.0133(19) C40 0.0225(18) 0.054(3) 0.045(2) -0.035(2) -0.0142(17) 0.0119(17) C41 0.0255(19) 0.058(3) 0.040(2) -0.035(2) -0.0094(17) 0.0048(18) C42 0.025(2) 0.075(3) 0.035(2) -0.035(2) -0.0032(17) -0.003(2) C43 0.031(2) 0.082(4) 0.049(3) -0.050(3) -0.0037(19) -0.009(2) C44 0.024(2) 0.066(3) 0.066(3) -0.053(3) -0.002(2) -0.002(2) C45 0.0208(19) 0.057(3) 0.055(3) -0.038(2) -0.0133(18) 0.0102(18) C50 0.042(3) 0.045(3) 0.073(3) -0.035(3) -0.038(2) 0.013(2) C51 0.061(3) 0.029(2) 0.065(3) -0.016(2) -0.040(3) 0.003(2) C52 0.087(4) 0.027(2) 0.085(4) 0.010(3) -0.067(4) -0.025(3) C53 0.057(4) 0.025(2) 0.167(8) -0.014(3) -0.078(5) 0.000(2) C54 0.040(3) 0.055(3) 0.196(9) -0.074(5) -0.058(4) 0.015(3) C55 0.041(3) 0.072(4) 0.139(6) -0.076(4) -0.046(3) 0.021(3) B1 0.037(2) 0.045(3) 0.040(3) -0.028(2) -0.022(2) 0.014(2) F21 0.0381(14) 0.0688(18) 0.0538(17) -0.0462(15) -0.0067(12) 0.0085(13) F22 0.0374(14) 0.0589(17) 0.0411(15) -0.0251(13) 0.0009(11) 0.0023(12) F23 0.0638(18) 0.0328(13) 0.0449(16) -0.0132(12) 0.0029(13) 0.0064(12) F24 0.0536(16) 0.0357(13) 0.0388(14) -0.0186(11) 0.0040(12) 0.0095(12) F25 0.0457(14) 0.0431(14) 0.0268(12) -0.0172(11) -0.0010(10) 0.0006(11) F31 0.0413(14) 0.0430(14) 0.0281(12) -0.0101(11) -0.0163(10) 0.0112(11) F32 0.0396(15) 0.0536(16) 0.0413(15) -0.0128(13) -0.0096(12) 0.0145(12) F33 0.0603(18) 0.0586(18) 0.0331(14) -0.0132(13) -0.0041(13) 0.0066(14) F34 0.074(2) 0.0393(14) 0.0355(14) -0.0091(12) -0.0262(14) 0.0061(13) F35 0.0532(16) 0.0365(14) 0.0572(17) -0.0173(13) -0.0346(14) 0.0129(12) F41 0.0568(17) 0.0521(16) 0.0360(14) -0.0255(12) -0.0199(12) 0.0101(13) F42 0.0544(17) 0.088(2) 0.0313(14) -0.0313(15) -0.0102(12) -0.0091(16) F43 0.073(2) 0.114(3) 0.060(2) -0.066(2) -0.0062(17) -0.025(2) F44 0.0489(17) 0.071(2) 0.088(2) -0.062(2) -0.0071(16) -0.0045(15) F45 0.0473(16) 0.0487(16) 0.0672(19) -0.0352(15) -0.0294(14) 0.0191(13) F51 0.087(2) 0.0410(15) 0.0371(15) -0.0069(12) -0.0356(15) -0.0143(15) F52 0.114(3) 0.070(2) 0.079(2) 0.0242(19) -0.078(2) -0.050(2) F53 0.070(2) 0.0434(18) 0.225(6) 0.008(3) -0.108(3) -0.0092(17) F54 0.0419(19) 0.116(3) 0.335(8) -0.167(5) -0.078(3) 0.040(2) F55 0.0379(18) 0.202(5) 0.201(5) -0.181(5) -0.049(2) 0.044(2) Pb1 0.04589(11) 0.02789(9) 0.04115(10) -0.00583(7) -0.01667(7) -0.00059(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.427(6) . ? C1 C2 1.428(6) . ? C1 C6 1.504(6) . ? C1 Pb1 2.539(4) . ? C2 C3 1.435(6) . ? C2 C7 1.504(6) . ? C2 Pb1 2.539(4) . ? C3 C4 1.428(6) . ? C3 C8 1.499(6) . ? C3 Pb1 2.546(4) . ? C4 C5 1.424(6) . ? C4 C9 1.509(6) . ? C4 Pb1 2.557(4) . ? C5 C10 1.505(6) . ? C5 Pb1 2.559(4) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C20 C25 1.388(6) . ? C20 C21 1.392(6) . ? C20 B1 1.657(7) . ? C21 F21 1.361(5) . ? C21 C22 1.369(7) . ? C22 F22 1.352(5) . ? C22 C23 1.381(6) . ? C23 F23 1.346(5) . ? C23 C24 1.363(6) . ? C24 F24 1.356(4) . ? C24 C25 1.380(6) . ? C25 F25 1.353(5) . ? C30 C35 1.385(6) . ? C30 C31 1.394(6) . ? C30 B1 1.653(7) . ? C31 F31 1.354(5) . ? C31 C32 1.377(6) . ? C32 F32 1.351(5) . ? C32 C33 1.370(6) . ? C33 F33 1.346(6) . ? C33 C34 1.376(7) . ? C34 F34 1.345(5) . ? C34 C35 1.381(7) . ? C35 F35 1.365(5) . ? C40 C41 1.380(6) . ? C40 C45 1.395(6) . ? C40 B1 1.660(6) . ? C41 F41 1.348(5) . ? C41 C42 1.391(6) . ? C42 F42 1.343(6) . ? C42 C43 1.372(7) . ? C43 F43 1.344(5) . ? C43 C44 1.364(8) . ? C44 F44 1.348(6) . ? C44 C45 1.385(6) . ? C45 F45 1.358(6) . ? C50 C51 1.371(7) . ? C50 C55 1.382(8) . ? C50 B1 1.664(6) . ? C51 F51 1.354(7) . ? C51 C52 1.404(7) . ? C52 F52 1.344(8) . ? C52 C53 1.378(11) . ? C53 F53 1.337(6) . ? C53 C54 1.337(12) . ? C54 F54 1.344(8) . ? C54 C55 1.393(8) . ? C55 F55 1.330(8) . ? 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 C5 C1 C2 108.1(3) . . ? C5 C1 C6 126.7(4) . . ? C2 C1 C6 124.8(4) . . ? C5 C1 Pb1 74.5(2) . . ? C2 C1 Pb1 73.6(2) . . ? C6 C1 Pb1 123.4(3) . . ? C1 C2 C3 107.8(4) . . ? C1 C2 C7 124.3(4) . . ? C3 C2 C7 127.5(4) . . ? C1 C2 Pb1 73.7(2) . . ? C3 C2 Pb1 73.9(2) . . ? C7 C2 Pb1 123.6(3) . . ? C4 C3 C2 107.8(4) . . ? C4 C3 C8 125.9(4) . . ? C2 C3 C8 126.0(4) . . ? C4 C3 Pb1 74.2(2) . . ? C2 C3 Pb1 73.3(2) . . ? C8 C3 Pb1 123.0(3) . . ? C5 C4 C3 108.2(4) . . ? C5 C4 C9 124.7(4) . . ? C3 C4 C9 126.8(4) . . ? C5 C4 Pb1 73.9(2) . . ? C3 C4 Pb1 73.3(2) . . ? C9 C4 Pb1 123.5(3) . . ? C4 C5 C1 108.1(4) . . ? C4 C5 C10 125.7(4) . . ? C1 C5 C10 125.8(4) . . ? C4 C5 Pb1 73.8(2) . . ? C1 C5 Pb1 73.0(2) . . ? C10 C5 Pb1 124.9(3) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C25 C20 C21 112.9(4) . . ? C25 C20 B1 128.3(4) . . ? C21 C20 B1 118.3(4) . . ? F21 C21 C22 115.9(4) . . ? F21 C21 C20 118.9(4) . . ? C22 C21 C20 125.3(4) . . ? F22 C22 C21 121.2(4) . . ? F22 C22 C23 119.8(4) . . ? C21 C22 C23 119.0(4) . . ? F23 C23 C24 120.9(4) . . ? F23 C23 C22 120.4(4) . . ? C24 C23 C22 118.7(4) . . ? F24 C24 C23 118.4(4) . . ? F24 C24 C25 121.0(4) . . ? C23 C24 C25 120.5(4) . . ? F25 C25 C24 115.0(3) . . ? F25 C25 C20 121.3(4) . . ? C24 C25 C20 123.6(4) . . ? C35 C30 C31 113.2(4) . . ? C35 C30 B1 126.9(4) . . ? C31 C30 B1 119.7(4) . . ? F31 C31 C32 116.7(4) . . ? F31 C31 C30 118.9(4) . . ? C32 C31 C30 124.4(4) . . ? F32 C32 C33 120.0(4) . . ? F32 C32 C31 120.7(4) . . ? C33 C32 C31 119.3(4) . . ? F33 C33 C32 121.1(4) . . ? F33 C33 C34 119.7(4) . . ? C32 C33 C34 119.2(4) . . ? F34 C34 C33 119.9(4) . . ? F34 C34 C35 120.7(4) . . ? C33 C34 C35 119.4(4) . . ? F35 C35 C34 114.3(4) . . ? F35 C35 C30 121.4(4) . . ? C34 C35 C30 124.3(4) . . ? C41 C40 C45 113.1(4) . . ? C41 C40 B1 127.4(4) . . ? C45 C40 B1 119.3(4) . . ? F41 C41 C40 121.7(4) . . ? F41 C41 C42 114.4(4) . . ? C40 C41 C42 123.9(4) . . ? F42 C42 C43 119.5(4) . . ? F42 C42 C41 120.7(5) . . ? C43 C42 C41 119.9(5) . . ? F43 C43 C44 120.8(5) . . ? F43 C43 C42 120.0(5) . . ? C44 C43 C42 119.2(4) . . ? F44 C44 C43 120.6(4) . . ? F44 C44 C45 120.3(5) . . ? C43 C44 C45 119.1(4) . . ? F45 C45 C44 115.9(4) . . ? F45 C45 C40 119.2(4) . . ? C44 C45 C40 124.8(5) . . ? C51 C50 C55 113.1(5) . . ? C51 C50 B1 119.8(4) . . ? C55 C50 B1 126.8(5) . . ? F51 C51 C50 118.9(4) . . ? F51 C51 C52 115.8(5) . . ? C50 C51 C52 125.3(6) . . ? F52 C52 C53 122.4(6) . . ? F52 C52 C51 119.7(7) . . ? C53 C52 C51 117.9(6) . . ? F53 C53 C54 122.2(8) . . ? F53 C53 C52 118.7(8) . . ? C54 C53 C52 119.2(5) . . ? C53 C54 F54 118.5(6) . . ? C53 C54 C55 121.0(7) . . ? F54 C54 C55 120.4(8) . . ? F55 C55 C50 122.0(5) . . ? F55 C55 C54 114.7(6) . . ? C50 C55 C54 123.3(7) . . ? C30 B1 C20 113.7(3) . . ? C30 B1 C40 102.8(3) . . ? C20 B1 C40 113.1(4) . . ? C30 B1 C50 112.5(4) . . ? C20 B1 C50 101.5(3) . . ? C40 B1 C50 113.6(4) . . ? C2 Pb1 C1 32.67(13) . . ? C2 Pb1 C3 32.79(14) . . ? C1 Pb1 C3 54.13(13) . . ? C2 Pb1 C4 53.99(13) . . ? C1 Pb1 C4 53.85(13) . . ? C3 Pb1 C4 32.50(14) . . ? C2 Pb1 C5 53.92(13) . . ? C1 Pb1 C5 32.50(12) . . ? C3 Pb1 C5 53.82(13) . . ? C4 Pb1 C5 32.32(13) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.39 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.710 _refine_diff_density_min -2.175 _refine_diff_density_rms 0.105 data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 276995' _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 B F20, C10 H15, 2 (C10 H15 Sn)' _chemical_formula_sum 'C54 H45 B F20 Sn2' _chemical_formula_weight 1322.09 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' B B 0.0013 0.0007 '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' 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 C2/c _symmetry_space_group_name_Hall -C2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.138(5) _cell_length_b 14.955(5) _cell_length_c 17.097(5) _cell_angle_alpha 90 _cell_angle_beta 114.259(5) _cell_angle_gamma 90 _cell_volume 5161(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max .14 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2616 _exptl_absorpt_coefficient_mu 1.078 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26112 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.44 _reflns_number_total 5869 _reflns_number_gt 4894 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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^)+(0.0270P)^2^+23.6892P] 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 5869 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_restrained_S_all 1.163 _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 C1 C 0.26395(19) 0.9291(3) 0.7346(3) 0.0329(9) Uani 1 1 d . . . C2 C 0.24727(19) 0.9087(3) 0.6475(3) 0.0337(8) Uani 1 1 d . . . C3 C 0.27246(19) 0.9795(3) 0.6125(2) 0.0311(8) Uani 1 1 d . . . C4 C 0.30272(17) 1.0442(2) 0.6782(2) 0.0292(8) Uani 1 1 d . . . C5 C 0.29877(18) 1.0120(3) 0.7545(2) 0.0305(8) Uani 1 1 d . . . C6 C 0.49077(19) 0.8350(3) 0.7051(2) 0.0293(8) Uani 1 1 d . . . C7 C 0.48451(18) 0.9260(2) 0.6769(2) 0.0264(8) Uani 1 1 d . . . C8 C 0.5000 0.9828(3) 0.7500 0.0242(10) Uani 1 2 d S . . C9 C 0.44516(17) 0.4885(2) 0.7594(2) 0.0264(8) Uani 1 1 d . . . C10 C 0.40865(18) 0.5453(2) 0.6916(2) 0.0293(8) Uani 1 1 d . . . C11 C 0.36589(19) 0.6113(3) 0.6956(3) 0.0365(9) Uani 1 1 d . . . C12 C 0.3573(2) 0.6223(3) 0.7698(3) 0.0411(10) Uani 1 1 d . . . C13 C 0.3911(2) 0.5685(3) 0.8391(3) 0.0394(10) Uani 1 1 d . . . C14 C 0.43423(18) 0.5045(3) 0.8331(3) 0.0314(8) Uani 1 1 d . . . C15 C 0.47001(16) 0.3493(2) 0.6671(2) 0.0209(7) Uani 1 1 d . . . C16 C 0.51355(17) 0.2959(2) 0.6487(2) 0.0251(7) Uani 1 1 d . . . C17 C 0.49546(19) 0.2366(2) 0.5812(2) 0.0284(8) Uani 1 1 d . . . C18 C 0.42963(19) 0.2264(2) 0.5278(2) 0.0292(8) Uani 1 1 d . . . C19 C 0.38399(17) 0.2759(3) 0.5437(2) 0.0269(8) Uani 1 1 d . . . C20 C 0.40402(17) 0.3343(2) 0.6118(2) 0.0234(7) Uani 1 1 d . . . C101 C 0.2438(2) 0.8759(4) 0.7943(3) 0.0514(12) Uani 1 1 d . . . H10A H 0.2015 0.8987 0.7920 0.077 Uiso 1 1 calc R . . H10B H 0.2778 0.8813 0.8530 0.077 Uiso 1 1 calc R . . H10C H 0.2387 0.8129 0.7770 0.077 Uiso 1 1 calc R . . C201 C 0.2058(2) 0.8314(3) 0.5977(3) 0.0546(13) Uani 1 1 d . . . H20A H 0.1608 0.8523 0.5623 0.082 Uiso 1 1 calc R . . H20B H 0.2041 0.7855 0.6377 0.082 Uiso 1 1 calc R . . H20C H 0.2255 0.8059 0.5608 0.082 Uiso 1 1 calc R . . C301 C 0.2605(3) 0.9900(4) 0.5199(3) 0.0562(13) Uani 1 1 d . . . H30A H 0.2153 1.0116 0.4871 0.084 Uiso 1 1 calc R . . H30B H 0.2663 0.9320 0.4970 0.084 Uiso 1 1 calc R . . H30C H 0.2922 1.0331 0.5152 0.084 Uiso 1 1 calc R . . C401 C 0.3252(2) 1.1356(3) 0.6654(3) 0.0491(12) Uani 1 1 d . . . H40A H 0.2867 1.1749 0.6392 0.074 Uiso 1 1 calc R . . H40B H 0.3485 1.1314 0.6276 0.074 Uiso 1 1 calc R . . H40C H 0.3552 1.1602 0.7210 0.074 Uiso 1 1 calc R . . C501 C 0.3217(2) 1.0606(4) 0.8389(3) 0.0533(12) Uani 1 1 d . . . H50A H 0.3508 1.1102 0.8393 0.080 Uiso 1 1 calc R . . H50B H 0.3461 1.0192 0.8857 0.080 Uiso 1 1 calc R . . H50C H 0.2832 1.0842 0.8467 0.080 Uiso 1 1 calc R . . C601 C 0.4811(2) 0.7544(3) 0.6483(3) 0.0404(10) Uani 1 1 d . . . H60A H 0.5114 0.7579 0.6197 0.061 Uiso 1 1 calc R . . H60B H 0.4352 0.7529 0.6050 0.061 Uiso 1 1 calc R . . H60C H 0.4903 0.6999 0.6831 0.061 Uiso 1 1 calc R . . C701 C 0.4662(2) 0.9579(3) 0.5866(3) 0.0403(10) Uani 1 1 d . . . H70A H 0.4435 1.0157 0.5783 0.061 Uiso 1 1 calc R . . H70B H 0.4367 0.9142 0.5461 0.061 Uiso 1 1 calc R . . H70C H 0.5064 0.9646 0.5764 0.061 Uiso 1 1 calc R . . C801 C 0.5000 1.0832(4) 0.7500 0.0375(13) Uani 1 2 d S . . H80A H 0.4560 1.1050 0.7116 0.056 Uiso 0.50 1 calc PR . . H80B H 0.5330 1.1050 0.7300 0.056 Uiso 0.50 1 calc PR . . H80C H 0.5110 1.1050 0.8083 0.056 Uiso 0.50 1 calc PR . . B B 0.5000 0.4185(4) 0.7500 0.0213(11) Uani 1 2 d S . . F10 F 0.41601(11) 0.53909(14) 0.61742(14) 0.0340(5) Uani 1 1 d . . . F11 F 0.33350(12) 0.66483(16) 0.62811(17) 0.0499(7) Uani 1 1 d . . . F12 F 0.31642(13) 0.68645(18) 0.77555(19) 0.0579(8) Uani 1 1 d . . . F13 F 0.38344(14) 0.57897(19) 0.91256(17) 0.0553(7) Uani 1 1 d . . . F14 F 0.46693(12) 0.45773(16) 0.90600(14) 0.0399(6) Uani 1 1 d . . . F16 F 0.57962(10) 0.30232(14) 0.69829(13) 0.0303(5) Uani 1 1 d . . . F17 F 0.54201(12) 0.18806(17) 0.56835(15) 0.0434(6) Uani 1 1 d . . . F18 F 0.41088(12) 0.16833(16) 0.46182(14) 0.0431(6) Uani 1 1 d . . . F19 F 0.31889(10) 0.26578(16) 0.49274(14) 0.0375(5) Uani 1 1 d . . . F20 F 0.35492(10) 0.37838(15) 0.62274(14) 0.0314(5) Uani 1 1 d . . . Sn1 Sn 0.374803(12) 0.907810(18) 0.721961(17) 0.02989(9) 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 0.0295(19) 0.040(2) 0.031(2) 0.0067(17) 0.0145(16) 0.0058(17) C2 0.0311(19) 0.031(2) 0.033(2) 0.0003(17) 0.0076(16) 0.0003(17) C3 0.031(2) 0.035(2) 0.0246(19) 0.0055(16) 0.0087(16) 0.0019(16) C4 0.0187(17) 0.0273(19) 0.037(2) 0.0044(16) 0.0062(15) 0.0018(14) C5 0.0251(18) 0.036(2) 0.030(2) -0.0043(16) 0.0113(16) 0.0044(16) C6 0.034(2) 0.0289(19) 0.0280(19) -0.0040(16) 0.0159(16) -0.0010(16) C7 0.0274(18) 0.032(2) 0.0218(18) 0.0011(15) 0.0121(15) 0.0019(15) C8 0.019(2) 0.028(3) 0.028(3) 0.000 0.013(2) 0.000 C9 0.0244(18) 0.0246(18) 0.0276(19) -0.0061(15) 0.0080(15) -0.0037(14) C10 0.0267(19) 0.0279(19) 0.030(2) -0.0050(16) 0.0086(16) -0.0013(15) C11 0.030(2) 0.027(2) 0.043(2) -0.0046(17) 0.0054(18) 0.0018(16) C12 0.029(2) 0.035(2) 0.053(3) -0.015(2) 0.0102(19) 0.0076(17) C13 0.037(2) 0.041(2) 0.042(2) -0.0193(19) 0.0175(19) -0.0017(18) C14 0.0271(19) 0.032(2) 0.032(2) -0.0077(17) 0.0090(16) -0.0010(16) C15 0.0225(16) 0.0233(17) 0.0173(16) 0.0046(13) 0.0087(13) 0.0004(13) C16 0.0234(17) 0.0296(19) 0.0217(18) 0.0041(15) 0.0086(14) 0.0026(14) C17 0.035(2) 0.0308(19) 0.0222(18) 0.0013(15) 0.0145(16) 0.0090(16) C18 0.041(2) 0.0283(19) 0.0173(18) -0.0032(15) 0.0109(16) -0.0024(16) C19 0.0252(18) 0.0312(19) 0.0209(18) 0.0028(15) 0.0059(14) -0.0030(15) C20 0.0239(17) 0.0249(17) 0.0237(18) 0.0056(14) 0.0122(14) 0.0019(14) C101 0.047(3) 0.064(3) 0.056(3) 0.018(2) 0.034(2) 0.003(2) C201 0.048(3) 0.046(3) 0.057(3) -0.009(2) 0.009(2) -0.013(2) C301 0.060(3) 0.074(4) 0.027(2) 0.013(2) 0.010(2) -0.001(3) C401 0.034(2) 0.032(2) 0.071(3) 0.013(2) 0.011(2) 0.0014(19) C501 0.048(3) 0.065(3) 0.044(3) -0.019(2) 0.016(2) 0.004(2) C601 0.054(3) 0.033(2) 0.036(2) -0.0085(18) 0.021(2) -0.0008(19) C701 0.048(2) 0.048(3) 0.026(2) 0.0054(19) 0.0174(19) 0.006(2) C801 0.032(3) 0.032(3) 0.048(4) 0.000 0.016(3) 0.000 B 0.023(3) 0.020(3) 0.021(3) 0.000 0.009(2) 0.000 F10 0.0350(12) 0.0316(12) 0.0308(12) 0.0025(9) 0.0089(10) 0.0038(9) F11 0.0446(14) 0.0371(13) 0.0514(16) 0.0012(12) 0.0028(12) 0.0167(11) F12 0.0471(15) 0.0494(16) 0.0729(19) -0.0192(14) 0.0203(14) 0.0187(13) F13 0.0587(17) 0.0663(18) 0.0483(16) -0.0212(14) 0.0296(13) 0.0105(14) F14 0.0484(14) 0.0469(14) 0.0271(12) -0.0056(10) 0.0183(11) 0.0085(11) F16 0.0217(10) 0.0393(12) 0.0275(11) -0.0023(9) 0.0078(9) 0.0057(9) F17 0.0425(13) 0.0534(15) 0.0344(13) -0.0094(11) 0.0158(11) 0.0174(12) F18 0.0486(14) 0.0450(14) 0.0284(12) -0.0159(11) 0.0084(11) 0.0002(11) F19 0.0273(11) 0.0469(14) 0.0299(12) -0.0055(10) 0.0033(9) -0.0059(10) F20 0.0203(10) 0.0390(12) 0.0344(12) -0.0072(10) 0.0108(9) 0.0013(9) Sn1 0.02422(13) 0.03109(14) 0.03609(16) 0.00285(12) 0.01414(11) 0.00314(11) _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 1.412(6) . ? C1 C5 1.425(6) . ? C1 C101 1.501(6) . ? C1 Sn1 2.570(4) . ? C2 C3 1.436(6) . ? C2 C201 1.504(6) . ? C2 Sn1 2.576(4) . ? C3 C4 1.424(5) . ? C3 C301 1.503(6) . ? C3 Sn1 2.510(4) . ? C4 C5 1.427(6) . ? C4 C401 1.501(6) . ? C4 Sn1 2.507(4) . ? C5 C501 1.507(6) . ? C5 Sn1 2.517(4) . ? C6 C6 1.419(7) 2_656 ? C6 C7 1.432(5) . ? C6 C601 1.507(5) . ? C7 C8 1.431(5) . ? C7 C701 1.505(5) . ? C8 C7 1.431(5) 2_656 ? C8 C801 1.501(7) . ? C9 C10 1.394(5) . ? C9 C14 1.398(5) . ? C9 B 1.660(5) . ? C10 F10 1.347(4) . ? C10 C11 1.388(5) . ? C11 F11 1.344(5) . ? C11 C12 1.368(6) . ? C12 F12 1.349(4) . ? C12 C13 1.373(6) . ? C13 F13 1.345(5) . ? C13 C14 1.385(5) . ? C14 F14 1.351(5) . ? C15 C16 1.384(5) . ? C15 C20 1.394(5) . ? C15 B 1.657(5) . ? C16 F16 1.360(4) . ? C16 C17 1.378(5) . ? C17 F17 1.350(4) . ? C17 C18 1.374(5) . ? C18 F18 1.347(4) . ? C18 C19 1.367(5) . ? C19 F19 1.352(4) . ? C19 C20 1.374(5) . ? C20 F20 1.349(4) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? C301 H30A 0.9800 . ? C301 H30B 0.9800 . ? C301 H30C 0.9800 . ? C401 H40A 0.9800 . ? C401 H40B 0.9800 . ? C401 H40C 0.9800 . ? C501 H50A 0.9800 . ? C501 H50B 0.9800 . ? C501 H50C 0.9800 . ? C601 H60A 0.9800 . ? C601 H60B 0.9800 . ? C601 H60C 0.9800 . ? C701 H70A 0.9800 . ? C701 H70B 0.9800 . ? C701 H70C 0.9800 . ? C801 H80A 0.9800 . ? C801 H80B 0.9800 . ? C801 H80C 0.9800 . ? B C15 1.657(5) 2_656 ? B C9 1.660(5) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 108.7(3) . . ? C2 C1 C101 125.6(4) . . ? C5 C1 C101 125.6(4) . . ? C2 C1 Sn1 74.3(2) . . ? C5 C1 Sn1 71.7(2) . . ? C101 C1 Sn1 123.6(3) . . ? C1 C2 C3 107.6(3) . . ? C1 C2 C201 126.6(4) . . ? C3 C2 C201 125.6(4) . . ? C1 C2 Sn1 73.8(2) . . ? C3 C2 Sn1 71.1(2) . . ? C201 C2 Sn1 124.4(3) . . ? C4 C3 C2 108.1(3) . . ? C4 C3 C301 125.6(4) . . ? C2 C3 C301 125.8(4) . . ? C4 C3 Sn1 73.4(2) . . ? C2 C3 Sn1 76.2(2) . . ? C301 C3 Sn1 122.9(3) . . ? C3 C4 C5 107.8(3) . . ? C3 C4 C401 125.5(4) . . ? C5 C4 C401 126.1(4) . . ? C3 C4 Sn1 73.6(2) . . ? C5 C4 Sn1 73.9(2) . . ? C401 C4 Sn1 125.1(3) . . ? C1 C5 C4 107.8(3) . . ? C1 C5 C501 125.8(4) . . ? C4 C5 C501 126.2(4) . . ? C1 C5 Sn1 75.8(2) . . ? C4 C5 Sn1 73.1(2) . . ? C501 C5 Sn1 121.2(3) . . ? C6 C6 C7 108.0(2) 2_656 . ? C6 C6 C601 126.8(2) 2_656 . ? C7 C6 C601 125.2(3) . . ? C8 C7 C6 108.4(3) . . ? C8 C7 C701 125.1(3) . . ? C6 C7 C701 126.4(3) . . ? C7 C8 C7 107.2(4) 2_656 . ? C7 C8 C801 126.4(2) 2_656 . ? C7 C8 C801 126.4(2) . . ? C10 C9 C14 112.9(3) . . ? C10 C9 B 120.1(3) . . ? C14 C9 B 126.8(3) . . ? F10 C10 C11 116.3(3) . . ? F10 C10 C9 119.2(3) . . ? C11 C10 C9 124.5(4) . . ? F11 C11 C12 119.7(4) . . ? F11 C11 C10 121.1(4) . . ? C12 C11 C10 119.2(4) . . ? F12 C12 C11 120.4(4) . . ? F12 C12 C13 119.9(4) . . ? C11 C12 C13 119.6(4) . . ? F13 C13 C12 120.2(4) . . ? F13 C13 C14 120.4(4) . . ? C12 C13 C14 119.4(4) . . ? F14 C14 C13 114.4(4) . . ? F14 C14 C9 121.2(3) . . ? C13 C14 C9 124.4(4) . . ? C16 C15 C20 112.7(3) . . ? C16 C15 B 118.9(3) . . ? C20 C15 B 128.4(3) . . ? F16 C16 C17 115.8(3) . . ? F16 C16 C15 119.3(3) . . ? C17 C16 C15 124.9(3) . . ? F17 C17 C18 120.3(3) . . ? F17 C17 C16 120.2(3) . . ? C18 C17 C16 119.4(3) . . ? F18 C18 C19 121.1(3) . . ? F18 C18 C17 120.4(3) . . ? C19 C18 C17 118.5(3) . . ? F19 C19 C18 119.4(3) . . ? F19 C19 C20 120.3(3) . . ? C18 C19 C20 120.3(3) . . ? F20 C20 C19 115.5(3) . . ? F20 C20 C15 120.4(3) . . ? C19 C20 C15 124.1(3) . . ? C1 C101 H10A 109.5 . . ? C1 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C1 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C2 C201 H20A 109.5 . . ? C2 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C2 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? C3 C301 H30A 109.5 . . ? C3 C301 H30B 109.5 . . ? H30A C301 H30B 109.5 . . ? C3 C301 H30C 109.5 . . ? H30A C301 H30C 109.5 . . ? H30B C301 H30C 109.5 . . ? C4 C401 H40A 109.5 . . ? C4 C401 H40B 109.5 . . ? H40A C401 H40B 109.5 . . ? C4 C401 H40C 109.5 . . ? H40A C401 H40C 109.5 . . ? H40B C401 H40C 109.5 . . ? C5 C501 H50A 109.5 . . ? C5 C501 H50B 109.5 . . ? H50A C501 H50B 109.5 . . ? C5 C501 H50C 109.5 . . ? H50A C501 H50C 109.5 . . ? H50B C501 H50C 109.5 . . ? C6 C601 H60A 109.5 . . ? C6 C601 H60B 109.5 . . ? H60A C601 H60B 109.5 . . ? C6 C601 H60C 109.5 . . ? H60A C601 H60C 109.5 . . ? H60B C601 H60C 109.5 . . ? C7 C701 H70A 109.5 . . ? C7 C701 H70B 109.5 . . ? H70A C701 H70B 109.5 . . ? C7 C701 H70C 109.5 . . ? H70A C701 H70C 109.5 . . ? H70B C701 H70C 109.5 . . ? C8 C801 H80A 109.5 . . ? C8 C801 H80B 109.5 . . ? H80A C801 H80B 109.5 . . ? C8 C801 H80C 109.5 . . ? H80A C801 H80C 109.5 . . ? H80B C801 H80C 109.5 . . ? C15 B C15 102.7(4) . 2_656 ? C15 B C9 115.11(17) . . ? C15 B C9 111.32(17) 2_656 . ? C15 B C9 111.32(17) . 2_656 ? C15 B C9 115.11(17) 2_656 2_656 ? C9 B C9 101.8(4) . 2_656 ? C4 Sn1 C3 32.97(12) . . ? C4 Sn1 C5 32.99(13) . . ? C3 Sn1 C5 54.52(13) . . ? C4 Sn1 C1 53.97(12) . . ? C3 Sn1 C1 53.78(12) . . ? C5 Sn1 C1 32.51(13) . . ? C4 Sn1 C2 54.14(12) . . ? C3 Sn1 C2 32.76(12) . . ? C5 Sn1 C2 53.80(13) . . ? C1 Sn1 C2 31.86(13) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.460 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.087 data_Compound4 _database_code_depnum_ccdc_archive 'CCDC 276996' _database_code_CSD XXXXXXX _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _publ_section_synopsis ; ; _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_references ; Allen, F.H. (2002). Acta Cryst. B58, 380-388. Cremer D. & Pople J.A. (1975). J. Am. Chem. Soc. 97, 1358-1367. Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. ; _publ_section_figure_captions ; ; _publ_section_exptl_prep ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H45 Pb2, C24 B F20' _chemical_formula_sum 'C54 H45 B F20 Pb2' _chemical_formula_weight 1499.09 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' B B 0.0013 0.0007 '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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M c2/c _symmetry_space_group_name_Hall -c2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.545(5) _cell_length_b 14.773(5) _cell_length_c 17.087(5) _cell_angle_alpha 90 _cell_angle_beta 114.911(5) _cell_angle_gamma 90 _cell_volume 5162(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.929 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2872 _exptl_absorpt_coefficient_mu 6.625 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.737 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8546 _diffrn_reflns_av_R_equivalents 0.0138 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4518 _reflns_number_gt 4284 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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^)+(0.0167P)^2^+10.6413P] 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 4518 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0187 _refine_ls_R_factor_gt 0.0173 _refine_ls_wR_factor_ref 0.0444 _refine_ls_wR_factor_gt 0.0437 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 C1 C 0.24462(14) 0.91021(18) 0.14712(19) 0.0270(6) Uani 1 1 d . . . C2 C 0.26988(13) 0.98026(19) 0.11274(17) 0.0276(6) Uani 1 1 d . . . C3 C 0.30046(13) 1.04517(18) 0.17913(19) 0.0268(6) Uani 1 1 d . . . C4 C 0.29560(13) 1.01379(19) 0.25480(18) 0.0280(6) Uani 1 1 d . . . C5 C 0.26066(13) 0.9304(2) 0.23430(18) 0.0275(6) Uani 1 1 d . . . C6 C 0.48980(12) 0.83244(17) 0.20464(17) 0.0208(5) Uani 1 1 d . . . C7 C 0.48281(13) 0.92452(17) 0.17610(17) 0.0209(5) Uani 1 1 d . . . C8 C 0.5000 0.9809(2) 0.2500 0.0211(7) Uani 1 2 d S . . C9 C 0.46958(12) 0.34747(16) 0.16649(16) 0.0195(5) Uani 1 1 d . . . C10 C 0.40469(12) 0.33211(16) 0.11160(16) 0.0202(5) Uani 1 1 d . . . C11 C 0.38397(13) 0.27286(18) 0.04244(16) 0.0238(6) Uani 1 1 d . . . C12 C 0.42900(14) 0.22354(17) 0.02604(17) 0.0261(6) Uani 1 1 d . . . C13 C 0.49423(13) 0.23401(17) 0.07984(17) 0.0247(6) Uani 1 1 d . . . C14 C 0.51243(12) 0.29374(17) 0.14779(16) 0.0215(5) Uani 1 1 d . . . C15 C 0.44602(12) 0.48789(17) 0.25990(17) 0.0212(5) Uani 1 1 d . . . C16 C 0.40953(13) 0.54565(17) 0.19223(17) 0.0238(6) Uani 1 1 d . . . C17 C 0.36756(14) 0.61174(18) 0.1965(2) 0.0295(6) Uani 1 1 d . . . C18 C 0.36017(14) 0.62322(19) 0.2718(2) 0.0331(7) Uani 1 1 d . . . C19 C 0.39465(14) 0.5689(2) 0.3408(2) 0.0319(7) Uani 1 1 d . . . C20 C 0.43676(13) 0.50433(18) 0.33455(17) 0.0259(6) Uani 1 1 d . . . C101 C 0.20252(16) 0.8327(2) 0.0963(2) 0.0459(8) Uani 1 1 d . . . H1A H 0.2042 0.7836 0.1357 0.069 Uiso 1 1 calc R . . H1B H 0.2187 0.8107 0.0548 0.069 Uiso 1 1 calc R . . H1C H 0.1573 0.8535 0.0653 0.069 Uiso 1 1 calc R . . C102 C 0.25850(18) 0.9905(3) 0.0201(2) 0.0505(9) Uani 1 1 d . . . H2A H 0.2624 0.9312 -0.0032 0.076 Uiso 1 1 calc R . . H2B H 0.2911 1.0319 0.0162 0.076 Uiso 1 1 calc R . . H2C H 0.2146 1.0149 -0.0134 0.076 Uiso 1 1 calc R . . C103 C 0.32420(16) 1.1370(2) 0.1662(2) 0.0450(8) Uani 1 1 d . . . H3A H 0.2869 1.1782 0.1406 0.068 Uiso 1 1 calc R . . H3B H 0.3462 1.1314 0.1277 0.068 Uiso 1 1 calc R . . H3C H 0.3550 1.1610 0.2220 0.068 Uiso 1 1 calc R . . C104 C 0.31762(18) 1.0637(3) 0.3393(2) 0.0479(9) Uani 1 1 d . . . H4A H 0.3508 1.1086 0.3433 0.072 Uiso 1 1 calc R . . H4B H 0.3363 1.0206 0.3871 0.072 Uiso 1 1 calc R . . H4C H 0.2801 1.0943 0.3423 0.072 Uiso 1 1 calc R . . C105 C 0.23940(17) 0.8785(3) 0.2936(2) 0.0460(8) Uani 1 1 d . . . H5A H 0.1993 0.9054 0.2925 0.069 Uiso 1 1 calc R . . H5B H 0.2740 0.8808 0.3525 0.069 Uiso 1 1 calc R . . H5C H 0.2310 0.8153 0.2745 0.069 Uiso 1 1 calc R . . C108 C 0.5000 1.0826(2) 0.2500 0.0318(9) Uani 1 2 d S . . H6A H 0.5188 1.1047 0.2113 0.048 Uiso 0.50 1 calc PR . . H6B H 0.5262 1.1047 0.3086 0.048 Uiso 0.50 1 calc PR . . H6C H 0.4550 1.1047 0.2301 0.048 Uiso 0.50 1 calc PR . . C107 C 0.53835(15) 0.9559(2) 0.41486(18) 0.0334(7) Uani 1 1 d . . . H7A H 0.5653 1.0104 0.4245 0.050 Uiso 1 1 calc R . . H7B H 0.5639 0.9081 0.4545 0.050 Uiso 1 1 calc R . . H7C H 0.4997 0.9697 0.4252 0.050 Uiso 1 1 calc R . . C106 C 0.52076(14) 0.75111(18) 0.35321(19) 0.0306(6) Uani 1 1 d . . . H8A H 0.5112 0.6958 0.3184 0.046 Uiso 1 1 calc R . . H8B H 0.4917 0.7550 0.3825 0.046 Uiso 1 1 calc R . . H8C H 0.5663 0.7498 0.3963 0.046 Uiso 1 1 calc R . . B1 B 0.5000 0.4177(3) 0.2500 0.0188(8) Uani 1 2 d S . . F10 F 0.35608(7) 0.37570(11) 0.12274(10) 0.0278(3) Uani 1 1 d . . . F11 F 0.31982(8) 0.26297(11) -0.00902(10) 0.0344(4) Uani 1 1 d . . . F12 F 0.40987(9) 0.16554(12) -0.04126(11) 0.0390(4) Uani 1 1 d . . . F13 F 0.53975(8) 0.18521(12) 0.06651(11) 0.0392(4) Uani 1 1 d . . . F14 F 0.57764(7) 0.30037(10) 0.19753(10) 0.0270(3) Uani 1 1 d . . . F15 F 0.47019(8) 0.45725(11) 0.40799(10) 0.0339(4) Uani 1 1 d . . . F17 F 0.38816(10) 0.57964(13) 0.41538(13) 0.0465(5) Uani 1 1 d . . . F18 F 0.32045(9) 0.68867(12) 0.27763(13) 0.0473(5) Uani 1 1 d . . . F19 F 0.33462(8) 0.66640(11) 0.12856(12) 0.0400(4) Uani 1 1 d . . . F20 F 0.41512(8) 0.53895(10) 0.11667(10) 0.0280(3) Uani 1 1 d . . . Pb1 Pb 0.374978(4) 0.903383(6) 0.225827(7) 0.02421(5) 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 0.0189(14) 0.0249(14) 0.0332(15) 0.0008(11) 0.0070(12) -0.0004(11) C2 0.0231(13) 0.0317(15) 0.0254(14) 0.0042(12) 0.0076(11) 0.0014(12) C3 0.0186(13) 0.0214(13) 0.0370(16) 0.0041(11) 0.0084(12) 0.0029(11) C4 0.0189(13) 0.0338(15) 0.0308(15) -0.0037(12) 0.0100(11) 0.0080(12) C5 0.0182(13) 0.0344(15) 0.0328(15) 0.0078(13) 0.0136(12) 0.0058(12) C6 0.0168(12) 0.0196(12) 0.0280(13) -0.0024(11) 0.0115(11) -0.0011(10) C7 0.0191(13) 0.0222(13) 0.0234(14) 0.0011(11) 0.0109(11) 0.0008(10) C8 0.0206(18) 0.0194(17) 0.0242(19) 0.000 0.0104(15) 0.000 C9 0.0223(13) 0.0187(12) 0.0196(12) 0.0036(10) 0.0109(10) 0.0002(10) C10 0.0206(12) 0.0192(12) 0.0235(13) 0.0028(10) 0.0120(11) 0.0018(10) C11 0.0245(13) 0.0234(13) 0.0202(13) 0.0020(10) 0.0062(11) -0.0035(11) C12 0.0377(16) 0.0213(13) 0.0191(13) -0.0013(11) 0.0117(12) -0.0007(12) C13 0.0310(15) 0.0217(13) 0.0256(14) 0.0012(11) 0.0160(12) 0.0073(11) C14 0.0220(13) 0.0224(13) 0.0214(12) 0.0034(11) 0.0104(11) 0.0004(11) C15 0.0183(12) 0.0184(12) 0.0270(14) -0.0041(10) 0.0096(11) -0.0030(10) C16 0.0222(13) 0.0214(13) 0.0270(14) -0.0056(11) 0.0094(11) -0.0041(11) C17 0.0228(14) 0.0201(13) 0.0398(17) -0.0004(12) 0.0074(12) 0.0025(11) C18 0.0254(15) 0.0239(14) 0.0507(19) -0.0109(13) 0.0167(14) 0.0036(12) C19 0.0313(16) 0.0325(15) 0.0365(17) -0.0134(13) 0.0187(14) -0.0034(13) C20 0.0259(14) 0.0230(13) 0.0262(14) -0.0036(11) 0.0085(12) -0.0011(11) C101 0.0354(17) 0.0366(17) 0.055(2) -0.0077(16) 0.0087(16) -0.0109(14) C102 0.053(2) 0.064(2) 0.0287(17) 0.0081(16) 0.0117(16) -0.0031(18) C103 0.0338(17) 0.0256(16) 0.064(2) 0.0091(15) 0.0097(16) -0.0011(13) C104 0.0428(19) 0.059(2) 0.0394(19) -0.0175(17) 0.0149(16) 0.0048(17) C105 0.0367(18) 0.062(2) 0.051(2) 0.0177(18) 0.0306(17) 0.0064(17) C108 0.034(2) 0.0204(19) 0.041(2) 0.000 0.015(2) 0.000 C107 0.0409(17) 0.0358(16) 0.0262(15) -0.0030(12) 0.0167(13) -0.0041(13) C106 0.0333(16) 0.0254(14) 0.0341(16) 0.0080(12) 0.0151(13) 0.0027(12) B1 0.018(2) 0.0199(19) 0.019(2) 0.000 0.0083(17) 0.000 F10 0.0191(8) 0.0325(8) 0.0332(8) -0.0054(7) 0.0124(7) 0.0006(7) F11 0.0237(8) 0.0407(9) 0.0307(9) -0.0061(7) 0.0036(7) -0.0060(7) F12 0.0465(10) 0.0379(9) 0.0284(9) -0.0144(7) 0.0118(8) -0.0007(8) F13 0.0400(10) 0.0418(10) 0.0388(10) -0.0094(8) 0.0195(8) 0.0137(8) F14 0.0180(7) 0.0327(8) 0.0288(8) -0.0016(7) 0.0085(6) 0.0064(6) F15 0.0440(10) 0.0351(9) 0.0243(8) -0.0028(7) 0.0160(7) 0.0090(8) F17 0.0554(12) 0.0498(11) 0.0435(11) -0.0137(9) 0.0297(10) 0.0108(9) F18 0.0402(10) 0.0354(10) 0.0671(13) -0.0128(9) 0.0233(10) 0.0136(8) F19 0.0354(9) 0.0289(9) 0.0462(10) 0.0040(8) 0.0078(8) 0.0124(8) F20 0.0319(8) 0.0257(8) 0.0261(8) 0.0033(6) 0.0118(7) 0.0041(7) Pb1 0.01827(7) 0.02340(7) 0.03372(7) 0.00314(4) 0.01364(5) 0.00258(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 C1 C5 1.409(4) . ? C1 C2 1.422(4) . ? C1 C101 1.507(4) . ? C1 Pb1 2.670(3) . ? C2 C3 1.422(4) . ? C2 C102 1.501(4) . ? C2 Pb1 2.604(3) . ? C3 C4 1.420(4) . ? C3 C103 1.508(4) . ? C3 Pb1 2.592(3) . ? C4 C5 1.424(4) . ? C4 C104 1.506(4) . ? C4 Pb1 2.618(3) . ? C5 C105 1.502(4) . ? C5 Pb1 2.672(3) . ? C6 C6 1.419(5) 2_655 ? C6 C7 1.431(4) . ? C6 C106 1.510(4) 2_655 ? C7 C8 1.423(3) . ? C7 C107 1.494(4) 2_655 ? C8 C7 1.423(3) 2_655 ? C8 C108 1.503(5) . ? C9 C10 1.384(4) . ? C9 C14 1.388(4) . ? C9 B1 1.661(3) . ? C10 F10 1.352(3) . ? C10 C11 1.384(4) . ? C11 F11 1.347(3) . ? C11 C12 1.371(4) . ? C12 F12 1.351(3) . ? C12 C13 1.376(4) . ? C13 F13 1.350(3) . ? C13 C14 1.376(4) . ? C14 F14 1.357(3) . ? C15 C16 1.393(4) . ? C15 C20 1.398(4) . ? C15 B1 1.661(3) . ? C16 F20 1.353(3) . ? C16 C17 1.383(4) . ? C17 F19 1.350(3) . ? C17 C18 1.376(5) . ? C18 F18 1.350(3) . ? C18 C19 1.366(5) . ? C19 F17 1.352(3) . ? C19 C20 1.381(4) . ? C20 F15 1.353(3) . ? C101 H1A 0.9800 . ? C101 H1B 0.9800 . ? C101 H1C 0.9800 . ? C102 H2A 0.9800 . ? C102 H2B 0.9800 . ? C102 H2C 0.9800 . ? C103 H3A 0.9800 . ? C103 H3B 0.9800 . ? C103 H3C 0.9800 . ? C104 H4A 0.9800 . ? C104 H4B 0.9800 . ? C104 H4C 0.9800 . ? C105 H5A 0.9800 . ? C105 H5B 0.9800 . ? C105 H5C 0.9800 . ? C108 H6A 0.9800 . ? C108 H6B 0.9800 . ? C108 H6C 0.9800 . ? C107 C7 1.494(4) 2_655 ? C107 H7A 0.9800 . ? C107 H7B 0.9800 . ? C107 H7C 0.9800 . ? C106 C6 1.510(4) 2_655 ? C106 H8A 0.9800 . ? C106 H8B 0.9800 . ? C106 H8C 0.9800 . ? B1 C15 1.661(3) 2_655 ? B1 C9 1.661(3) 2_655 ? 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 C5 C1 C2 108.3(2) . . ? C5 C1 C101 126.1(3) . . ? C2 C1 C101 125.4(3) . . ? C5 C1 Pb1 74.78(16) . . ? C2 C1 Pb1 71.83(15) . . ? C101 C1 Pb1 123.6(2) . . ? C1 C2 C3 107.8(2) . . ? C1 C2 C102 126.1(3) . . ? C3 C2 C102 125.7(3) . . ? C1 C2 Pb1 76.92(16) . . ? C3 C2 Pb1 73.64(15) . . ? C102 C2 Pb1 121.6(2) . . ? C4 C3 C2 108.0(2) . . ? C4 C3 C103 126.5(3) . . ? C2 C3 C103 124.9(3) . . ? C4 C3 Pb1 75.20(15) . . ? C2 C3 Pb1 74.59(15) . . ? C103 C3 Pb1 123.22(19) . . ? C3 C4 C5 107.8(2) . . ? C3 C4 C104 126.3(3) . . ? C5 C4 C104 125.7(3) . . ? C3 C4 Pb1 73.16(15) . . ? C5 C4 Pb1 76.47(15) . . ? C104 C4 Pb1 120.68(19) . . ? C1 C5 C4 108.2(2) . . ? C1 C5 C105 126.3(3) . . ? C4 C5 C105 125.2(3) . . ? C1 C5 Pb1 74.63(16) . . ? C4 C5 Pb1 72.32(15) . . ? C105 C5 Pb1 123.3(2) . . ? C6 C6 C7 108.10(15) 2_655 . ? C6 C6 C106 127.19(15) 2_655 2_655 ? C7 C6 C106 124.7(2) . 2_655 ? C8 C7 C6 107.7(2) . . ? C8 C7 C107 126.1(2) . 2_655 ? C6 C7 C107 126.2(2) . 2_655 ? C7 C8 C7 108.4(3) . 2_655 ? C7 C8 C108 125.79(16) . . ? C7 C8 C108 125.79(16) 2_655 . ? C10 C9 C14 112.9(2) . . ? C10 C9 B1 128.4(2) . . ? C14 C9 B1 118.7(2) . . ? F10 C10 C9 121.0(2) . . ? F10 C10 C11 114.8(2) . . ? C9 C10 C11 124.2(2) . . ? F11 C11 C12 119.5(2) . . ? F11 C11 C10 120.6(2) . . ? C12 C11 C10 119.9(2) . . ? F12 C12 C11 120.8(2) . . ? F12 C12 C13 120.6(2) . . ? C11 C12 C13 118.6(2) . . ? F13 C13 C12 120.1(2) . . ? F13 C13 C14 120.5(2) . . ? C12 C13 C14 119.4(2) . . ? F14 C14 C13 115.7(2) . . ? F14 C14 C9 119.4(2) . . ? C13 C14 C9 124.9(2) . . ? C16 C15 C20 112.8(2) . . ? C16 C15 B1 120.0(2) . . ? C20 C15 B1 126.8(2) . . ? F20 C16 C17 116.3(2) . . ? F20 C16 C15 119.2(2) . . ? C17 C16 C15 124.6(3) . . ? F19 C17 C18 119.4(2) . . ? F19 C17 C16 121.2(3) . . ? C18 C17 C16 119.4(3) . . ? F18 C18 C19 120.7(3) . . ? F18 C18 C17 120.2(3) . . ? C19 C18 C17 119.1(3) . . ? F17 C19 C18 119.8(3) . . ? F17 C19 C20 120.3(3) . . ? C18 C19 C20 119.9(3) . . ? F15 C20 C19 114.6(2) . . ? F15 C20 C15 121.2(2) . . ? C19 C20 C15 124.2(3) . . ? C1 C101 H1A 109.5 . . ? C1 C101 H1B 109.5 . . ? H1A C101 H1B 109.5 . . ? C1 C101 H1C 109.5 . . ? H1A C101 H1C 109.5 . . ? H1B C101 H1C 109.5 . . ? C2 C102 H2A 109.5 . . ? C2 C102 H2B 109.5 . . ? H2A C102 H2B 109.5 . . ? C2 C102 H2C 109.5 . . ? H2A C102 H2C 109.5 . . ? H2B C102 H2C 109.5 . . ? C3 C103 H3A 109.5 . . ? C3 C103 H3B 109.5 . . ? H3A C103 H3B 109.5 . . ? C3 C103 H3C 109.5 . . ? H3A C103 H3C 109.5 . . ? H3B C103 H3C 109.5 . . ? C4 C104 H4A 109.5 . . ? C4 C104 H4B 109.5 . . ? H4A C104 H4B 109.5 . . ? C4 C104 H4C 109.5 . . ? H4A C104 H4C 109.5 . . ? H4B C104 H4C 109.5 . . ? C5 C105 H5A 109.5 . . ? C5 C105 H5B 109.5 . . ? H5A C105 H5B 109.5 . . ? C5 C105 H5C 109.5 . . ? H5A C105 H5C 109.5 . . ? H5B C105 H5C 109.5 . . ? C8 C108 H6A 109.5 . . ? C8 C108 H6B 109.5 . . ? H6A C108 H6B 109.5 . . ? C8 C108 H6C 109.5 . . ? H6A C108 H6C 109.5 . . ? H6B C108 H6C 109.5 . . ? C7 C107 H7A 109.5 2_655 . ? C7 C107 H7B 109.5 2_655 . ? H7A C107 H7B 109.5 . . ? C7 C107 H7C 109.5 2_655 . ? H7A C107 H7C 109.5 . . ? H7B C107 H7C 109.5 . . ? C6 C106 H8A 109.5 2_655 . ? C6 C106 H8B 109.5 2_655 . ? H8A C106 H8B 109.5 . . ? C6 C106 H8C 109.5 2_655 . ? H8A C106 H8C 109.5 . . ? H8B C106 H8C 109.5 . . ? C15 B1 C15 102.7(3) 2_655 . ? C15 B1 C9 110.96(12) 2_655 . ? C15 B1 C9 114.99(12) . . ? C15 B1 C9 114.99(12) 2_655 2_655 ? C15 B1 C9 110.96(12) . 2_655 ? C9 B1 C9 102.7(3) . 2_655 ? C3 Pb1 C2 31.78(9) . . ? C3 Pb1 C4 31.64(9) . . ? C2 Pb1 C4 52.25(9) . . ? C3 Pb1 C1 51.76(8) . . ? C2 Pb1 C1 31.26(9) . . ? C4 Pb1 C1 51.43(9) . . ? C3 Pb1 C5 51.74(9) . . ? C2 Pb1 C5 51.53(9) . . ? C4 Pb1 C5 31.21(9) . . ? C1 Pb1 C5 30.59(9) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.414 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.071