# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_dr017 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H55 Br4 N3 Sn2' _chemical_formula_weight 1218.96 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 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 14.8198(2) _cell_length_b 19.1524(3) _cell_length_c 16.9799(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.2240(10) _cell_angle_gamma 90.00 _cell_volume 4818.39(13) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9843 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 28.10 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 4.388 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5786 _exptl_absorpt_correction_T_max 0.6681 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg (650 frames). Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41698 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.29 _reflns_number_total 11834 _reflns_number_gt 9121 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _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^)+(0.0432P)^2^+3.8124P] 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 11834 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Sn1 Sn 0.120158(13) 0.430365(11) 0.159814(11) 0.02855(6) Uani 1 1 d . . . Br1 Br 0.07566(2) 0.31083(2) 0.09252(3) 0.06292(13) Uani 1 1 d . . . N1 N 0.26024(15) 0.38282(12) 0.22214(13) 0.0254(5) Uani 1 1 d . . . N2 N 0.09211(14) 0.37506(11) 0.27528(12) 0.0222(4) Uani 1 1 d . . . N3 N -0.04560(15) 0.43363(12) 0.19033(13) 0.0253(5) Uani 1 1 d . . . C1 C 0.25359(18) 0.37199(14) 0.29649(16) 0.0264(6) Uani 1 1 d . . . C2 C 0.16046(18) 0.35727(14) 0.32455(15) 0.0240(5) Uani 1 1 d . . . C3 C 0.14449(19) 0.32476(15) 0.39595(16) 0.0298(6) Uani 1 1 d . . . H3A H 0.1933 0.3129 0.4306 0.036 Uiso 1 1 calc R . . C4 C 0.0567(2) 0.30979(16) 0.41608(17) 0.0333(7) Uani 1 1 d . . . H4A H 0.0444 0.2874 0.4646 0.040 Uiso 1 1 calc R . . C5 C -0.01265(19) 0.32774(15) 0.36488(16) 0.0290(6) Uani 1 1 d . . . H5A H -0.0733 0.3171 0.3775 0.035 Uiso 1 1 calc R . . C6 C 0.00627(17) 0.36146(14) 0.29473(15) 0.0238(5) Uani 1 1 d . . . C7 C -0.06587(17) 0.38598(14) 0.23975(15) 0.0241(5) Uani 1 1 d . . . C8 C 0.32889(19) 0.37451(16) 0.35561(17) 0.0308(6) Uani 1 1 d . . . C9 C 0.3221(2) 0.42029(18) 0.4183(2) 0.0423(8) Uani 1 1 d . . . H9A H 0.2679 0.4457 0.4254 0.051 Uiso 1 1 calc R . . C10 C 0.3945(3) 0.4291(2) 0.4708(2) 0.0570(10) Uani 1 1 d . . . H10A H 0.3898 0.4612 0.5132 0.068 Uiso 1 1 calc R . . C11 C 0.4718(3) 0.3923(2) 0.4618(2) 0.0603(12) Uani 1 1 d . . . H11A H 0.5214 0.3991 0.4974 0.072 Uiso 1 1 calc R . . C12 C 0.4786(2) 0.3450(2) 0.4008(2) 0.0562(11) Uani 1 1 d . . . H12A H 0.5321 0.3183 0.3958 0.067 Uiso 1 1 calc R . . C13 C 0.4077(2) 0.33604(19) 0.3466(2) 0.0436(8) Uani 1 1 d . . . H13A H 0.4130 0.3042 0.3041 0.052 Uiso 1 1 calc R . . C14 C -0.15617(18) 0.35131(15) 0.24515(16) 0.0286(6) Uani 1 1 d . . . C15 C -0.1635(2) 0.28198(18) 0.2222(2) 0.0422(8) Uani 1 1 d . . . H15A H -0.1113 0.2569 0.2071 0.051 Uiso 1 1 calc R . . C16 C -0.2468(3) 0.2496(2) 0.2212(2) 0.0515(9) Uani 1 1 d . . . H16A H -0.2523 0.2025 0.2041 0.062 Uiso 1 1 calc R . . C17 C -0.3206(2) 0.2850(2) 0.2449(3) 0.0592(11) Uani 1 1 d . . . H17A H -0.3776 0.2625 0.2444 0.071 Uiso 1 1 calc R . . C18 C -0.3139(2) 0.3528(2) 0.2693(3) 0.0716(14) Uani 1 1 d . . . H18A H -0.3661 0.3768 0.2862 0.086 Uiso 1 1 calc R . . C19 C -0.2305(2) 0.38681(19) 0.2697(3) 0.0498(9) Uani 1 1 d . . . H19A H -0.2255 0.4339 0.2868 0.060 Uiso 1 1 calc R . . C20 C 0.34587(18) 0.40457(15) 0.19085(16) 0.0264(6) Uani 1 1 d . . . C21 C 0.3919(2) 0.36581(16) 0.13472(18) 0.0336(6) Uani 1 1 d . . . C22 C 0.4695(3) 0.3981(2) 0.1075(3) 0.0559(10) Uani 1 1 d . . . H22A H 0.5017 0.3754 0.0671 0.067 Uiso 1 1 calc R . . C23 C 0.5026(3) 0.4612(2) 0.1354(3) 0.0597(11) Uani 1 1 d . . . H23A H 0.5560 0.4801 0.1141 0.072 Uiso 1 1 calc R . . C24 C 0.4586(2) 0.49711(17) 0.1944(2) 0.0384(7) Uani 1 1 d . . . C25 C 0.37843(19) 0.46875(15) 0.21901(17) 0.0288(6) Uani 1 1 d . . . H25A H 0.3441 0.4936 0.2564 0.035 Uiso 1 1 calc R . . C26 C 0.3693(2) 0.29251(16) 0.10308(17) 0.0326(6) Uani 1 1 d . . . C27 C 0.3257(3) 0.2991(2) 0.0213(2) 0.0574(10) Uani 1 1 d . . . H27A H 0.2695 0.3258 0.0248 0.086 Uiso 1 1 calc R . . H27B H 0.3124 0.2525 0.0004 0.086 Uiso 1 1 calc R . . H27C H 0.3671 0.3233 -0.0137 0.086 Uiso 1 1 calc R . . C28 C 0.4565(3) 0.2506(2) 0.0969(3) 0.0606(11) Uani 1 1 d . . . H28A H 0.4846 0.2455 0.1493 0.091 Uiso 1 1 calc R . . H28B H 0.4980 0.2750 0.0621 0.091 Uiso 1 1 calc R . . H28C H 0.4428 0.2043 0.0751 0.091 Uiso 1 1 calc R . . C29 C 0.3071(3) 0.24917(17) 0.1547(2) 0.0448(8) Uani 1 1 d . . . H29A H 0.3337 0.2453 0.2079 0.067 Uiso 1 1 calc R . . H29B H 0.2996 0.2025 0.1319 0.067 Uiso 1 1 calc R . . H29C H 0.2481 0.2720 0.1574 0.067 Uiso 1 1 calc R . . C30 C 0.4998(2) 0.56265(17) 0.2321(2) 0.0444(8) Uani 1 1 d . . . C31 C 0.5220(3) 0.6164(2) 0.1695(3) 0.0748(14) Uani 1 1 d . . . H31A H 0.5632 0.5958 0.1316 0.112 Uiso 1 1 calc R . . H31B H 0.5507 0.6571 0.1945 0.112 Uiso 1 1 calc R . . H31C H 0.4663 0.6310 0.1420 0.112 Uiso 1 1 calc R . . C32 C 0.5866(3) 0.5416(2) 0.2759(3) 0.0733(14) Uani 1 1 d . . . H32A H 0.5727 0.5070 0.3164 0.110 Uiso 1 1 calc R . . H32B H 0.6140 0.5828 0.3008 0.110 Uiso 1 1 calc R . . H32C H 0.6289 0.5213 0.2386 0.110 Uiso 1 1 calc R . . C33 C 0.4358(3) 0.5952(2) 0.2914(3) 0.0690(13) Uani 1 1 d . . . H33A H 0.4210 0.5606 0.3316 0.103 Uiso 1 1 calc R . . H33B H 0.3804 0.6104 0.2640 0.103 Uiso 1 1 calc R . . H33C H 0.4651 0.6355 0.3166 0.103 Uiso 1 1 calc R . . C34 C -0.11269(17) 0.45568(15) 0.13193(16) 0.0259(6) Uani 1 1 d . . . C35 C -0.14836(19) 0.52371(15) 0.12818(17) 0.0287(6) Uani 1 1 d . . . C36 C -0.2150(2) 0.53325(17) 0.07010(18) 0.0361(7) Uani 1 1 d . . . H36A H -0.2427 0.5779 0.0658 0.043 Uiso 1 1 calc R . . C37 C -0.2433(2) 0.48149(17) 0.01832(18) 0.0369(7) Uani 1 1 d . . . H37A H -0.2901 0.4913 -0.0192 0.044 Uiso 1 1 calc R . . C38 C -0.20452(18) 0.41547(15) 0.02036(16) 0.0283(6) Uani 1 1 d . . . C39 C -0.13949(18) 0.40421(16) 0.07856(16) 0.0275(6) Uani 1 1 d . . . H39A H -0.1120 0.3595 0.0823 0.033 Uiso 1 1 calc R . . C40 C -0.1156(2) 0.58556(16) 0.18004(18) 0.0336(7) Uani 1 1 d . . . C41 C -0.1146(3) 0.56809(18) 0.26760(19) 0.0459(8) Uani 1 1 d . . . H41A H -0.0751 0.5278 0.2775 0.069 Uiso 1 1 calc R . . H41B H -0.1759 0.5569 0.2839 0.069 Uiso 1 1 calc R . . H41C H -0.0920 0.6083 0.2978 0.069 Uiso 1 1 calc R . . C42 C -0.0215(2) 0.6061(2) 0.1543(2) 0.0492(9) Uani 1 1 d . . . H42A H 0.0190 0.5658 0.1596 0.074 Uiso 1 1 calc R . . H42B H 0.0012 0.6444 0.1875 0.074 Uiso 1 1 calc R . . H42C H -0.0241 0.6213 0.0992 0.074 Uiso 1 1 calc R . . C43 C -0.1778(3) 0.64917(18) 0.1695(2) 0.0515(9) Uani 1 1 d . . . H43A H -0.1813 0.6622 0.1137 0.077 Uiso 1 1 calc R . . H43B H -0.1535 0.6884 0.2003 0.077 Uiso 1 1 calc R . . H43C H -0.2383 0.6376 0.1877 0.077 Uiso 1 1 calc R . . C44 C -0.23745(19) 0.35676(16) -0.03465(17) 0.0309(6) Uani 1 1 d . . . C45 C -0.3292(2) 0.3320(2) -0.0064(2) 0.0518(9) Uani 1 1 d . . . H45A H -0.3229 0.3146 0.0478 0.078 Uiso 1 1 calc R . . H45B H -0.3515 0.2944 -0.0407 0.078 Uiso 1 1 calc R . . H45C H -0.3719 0.3710 -0.0080 0.078 Uiso 1 1 calc R . . C46 C -0.2462(3) 0.3834(2) -0.1191(2) 0.0506(9) Uani 1 1 d . . . H46A H -0.2667 0.3453 -0.1537 0.076 Uiso 1 1 calc R . . H46B H -0.1874 0.4003 -0.1364 0.076 Uiso 1 1 calc R . . H46C H -0.2901 0.4216 -0.1216 0.076 Uiso 1 1 calc R . . C47 C -0.1729(2) 0.29500(18) -0.0348(2) 0.0455(8) Uani 1 1 d . . . H47A H -0.1661 0.2764 0.0187 0.068 Uiso 1 1 calc R . . H47B H -0.1140 0.3103 -0.0535 0.068 Uiso 1 1 calc R . . H47C H -0.1971 0.2586 -0.0699 0.068 Uiso 1 1 calc R . . Sn2 Sn 0.115323(19) 0.592029(16) 0.452780(16) 0.05561(8) Uani 1 1 d . . . Br2 Br 0.15394(2) 0.541583(19) 0.311436(19) 0.04344(9) Uani 1 1 d . . . Br3 Br 0.28465(4) 0.62042(3) 0.48447(4) 0.0929(2) Uani 1 1 d . . . Br4 Br 0.12144(4) 0.47425(3) 0.53090(3) 0.08976(18) 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 Sn1 0.02640(10) 0.03759(12) 0.02169(9) 0.00426(8) 0.00082(7) -0.00260(8) Br1 0.03610(18) 0.0802(3) 0.0720(3) -0.0507(2) -0.01022(17) 0.00740(18) N1 0.0243(11) 0.0250(12) 0.0270(12) -0.0021(9) 0.0031(9) 0.0004(9) N2 0.0220(10) 0.0222(12) 0.0225(11) 0.0004(8) -0.0006(8) -0.0006(9) N3 0.0245(11) 0.0273(12) 0.0240(11) 0.0037(9) -0.0015(9) -0.0001(9) C1 0.0250(13) 0.0227(14) 0.0316(14) -0.0010(11) -0.0007(11) 0.0020(11) C2 0.0255(13) 0.0216(14) 0.0247(13) -0.0012(10) -0.0023(10) 0.0002(10) C3 0.0306(14) 0.0329(16) 0.0257(13) 0.0034(11) -0.0027(11) 0.0018(12) C4 0.0383(16) 0.0351(17) 0.0267(14) 0.0098(12) 0.0023(12) 0.0016(13) C5 0.0280(14) 0.0305(16) 0.0285(14) 0.0061(11) 0.0035(11) -0.0031(12) C6 0.0248(13) 0.0211(14) 0.0254(13) 0.0012(10) 0.0010(10) -0.0019(10) C7 0.0246(13) 0.0227(14) 0.0251(13) -0.0003(10) 0.0010(10) 0.0003(11) C8 0.0262(14) 0.0359(17) 0.0302(14) 0.0065(12) -0.0024(11) -0.0009(12) C9 0.0426(18) 0.043(2) 0.0405(18) 0.0001(14) -0.0132(14) 0.0022(15) C10 0.064(3) 0.057(2) 0.049(2) 0.0022(18) -0.0264(19) -0.011(2) C11 0.044(2) 0.081(3) 0.055(2) 0.023(2) -0.0250(18) -0.018(2) C12 0.0273(16) 0.083(3) 0.059(2) 0.030(2) -0.0052(15) 0.0077(18) C13 0.0340(16) 0.053(2) 0.0436(18) 0.0109(16) -0.0008(14) 0.0093(15) C14 0.0246(13) 0.0318(16) 0.0293(14) 0.0094(12) -0.0023(11) -0.0043(12) C15 0.0434(18) 0.0374(19) 0.0458(19) -0.0010(15) 0.0065(14) -0.0076(15) C16 0.059(2) 0.048(2) 0.047(2) 0.0016(16) -0.0036(17) -0.0243(19) C17 0.0326(18) 0.064(3) 0.080(3) 0.027(2) -0.0113(18) -0.0232(18) C18 0.0267(17) 0.058(3) 0.131(4) 0.029(3) 0.021(2) 0.0022(18) C19 0.0297(16) 0.0336(19) 0.086(3) 0.0106(18) 0.0131(17) -0.0013(14) C20 0.0226(13) 0.0271(15) 0.0295(14) 0.0013(11) 0.0020(10) 0.0025(11) C21 0.0325(15) 0.0288(16) 0.0397(16) -0.0028(12) 0.0062(12) 0.0025(12) C22 0.046(2) 0.051(2) 0.073(3) -0.0179(19) 0.0317(19) -0.0053(17) C23 0.044(2) 0.048(2) 0.089(3) -0.009(2) 0.032(2) -0.0138(17) C24 0.0274(15) 0.0302(17) 0.058(2) 0.0008(14) 0.0019(14) -0.0003(13) C25 0.0271(14) 0.0239(15) 0.0355(15) -0.0006(11) 0.0012(11) 0.0036(11) C26 0.0332(15) 0.0317(16) 0.0328(15) -0.0075(12) -0.0010(12) 0.0054(13) C27 0.064(2) 0.063(3) 0.045(2) 0.0078(18) -0.0163(18) -0.015(2) C28 0.048(2) 0.041(2) 0.093(3) -0.019(2) -0.004(2) 0.0151(18) C29 0.062(2) 0.0264(17) 0.0462(19) -0.0038(14) 0.0026(16) -0.0013(15) C30 0.0338(16) 0.0298(18) 0.069(2) -0.0003(16) -0.0078(16) -0.0060(14) C31 0.078(3) 0.047(3) 0.098(4) 0.015(2) -0.019(3) -0.027(2) C32 0.053(2) 0.054(3) 0.111(4) -0.001(3) -0.028(2) -0.002(2) C33 0.062(3) 0.045(2) 0.099(4) -0.032(2) -0.009(2) -0.009(2) C34 0.0211(12) 0.0294(15) 0.0273(13) 0.0060(11) 0.0006(10) -0.0015(11) C35 0.0299(14) 0.0270(15) 0.0293(14) 0.0051(11) 0.0003(11) 0.0004(12) C36 0.0392(17) 0.0313(17) 0.0374(16) 0.0066(13) -0.0031(13) 0.0078(13) C37 0.0363(16) 0.0395(18) 0.0344(16) 0.0063(13) -0.0092(12) 0.0069(14) C38 0.0247(13) 0.0317(16) 0.0285(14) 0.0025(11) 0.0030(11) -0.0007(11) C39 0.0251(13) 0.0279(15) 0.0295(14) 0.0046(11) 0.0026(11) -0.0008(11) C40 0.0373(16) 0.0278(16) 0.0356(16) 0.0027(12) -0.0010(12) 0.0001(13) C41 0.069(2) 0.0348(19) 0.0334(17) -0.0019(14) -0.0010(16) -0.0019(17) C42 0.050(2) 0.042(2) 0.056(2) -0.0004(16) 0.0007(17) -0.0120(17) C43 0.058(2) 0.0323(19) 0.063(2) -0.0037(16) -0.0110(18) 0.0090(17) C44 0.0289(14) 0.0348(17) 0.0289(14) 0.0005(12) -0.0013(11) -0.0010(12) C45 0.0367(18) 0.061(2) 0.058(2) -0.0080(19) 0.0076(16) -0.0093(17) C46 0.067(2) 0.052(2) 0.0323(17) 0.0001(15) -0.0059(16) -0.0015(19) C47 0.0403(18) 0.038(2) 0.058(2) -0.0118(16) -0.0048(15) 0.0016(15) Sn2 0.05743(16) 0.06060(18) 0.04914(16) -0.01865(12) 0.00941(12) 0.01189(13) Br2 0.0558(2) 0.03917(19) 0.03530(17) -0.00416(13) -0.00134(14) 0.00233(15) Br3 0.0752(3) 0.0804(4) 0.1214(5) -0.0453(3) -0.0380(3) 0.0105(3) Br4 0.1118(4) 0.1045(4) 0.0540(3) 0.0185(3) 0.0281(3) 0.0110(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 Sn1 N2 2.275(2) . ? Sn1 N1 2.483(2) . ? Sn1 N3 2.522(2) . ? Sn1 Br1 2.6362(4) . ? Sn1 Br2 3.3706(4) . ? N1 C1 1.285(4) . ? N1 C20 1.447(3) . ? N2 C6 1.347(3) . ? N2 C2 1.344(3) . ? N3 C7 1.280(3) . ? N3 C34 1.452(3) . ? C1 C2 1.496(4) . ? C1 C8 1.486(4) . ? C2 C3 1.388(4) . ? C3 C4 1.382(4) . ? C4 C5 1.376(4) . ? C5 C6 1.389(4) . ? C6 C7 1.481(4) . ? C7 C14 1.498(4) . ? C8 C9 1.384(5) . ? C8 C13 1.392(4) . ? C9 C10 1.391(5) . ? C10 C11 1.357(6) . ? C11 C12 1.381(6) . ? C12 C13 1.393(5) . ? C14 C19 1.367(4) . ? C14 C15 1.388(4) . ? C15 C16 1.382(5) . ? C16 C17 1.355(6) . ? C17 C18 1.365(6) . ? C18 C19 1.398(5) . ? C20 C21 1.397(4) . ? C20 C25 1.401(4) . ? C21 C22 1.393(5) . ? C21 C26 1.538(4) . ? C22 C23 1.383(5) . ? C23 C24 1.389(5) . ? C24 C25 1.379(4) . ? C24 C30 1.530(5) . ? C26 C27 1.524(4) . ? C26 C28 1.527(5) . ? C26 C29 1.531(5) . ? C30 C32 1.526(5) . ? C30 C31 1.521(6) . ? C30 C33 1.531(6) . ? C34 C39 1.391(4) . ? C34 C35 1.407(4) . ? C35 C36 1.393(4) . ? C35 C40 1.548(4) . ? C36 C37 1.384(5) . ? C37 C38 1.389(4) . ? C38 C39 1.383(4) . ? C38 C44 1.535(4) . ? C40 C41 1.524(4) . ? C40 C42 1.523(5) . ? C40 C43 1.535(5) . ? C44 C46 1.525(4) . ? C44 C45 1.527(4) . ? C44 C47 1.521(4) . ? Sn2 Br3 2.6123(6) . ? Sn2 Br4 2.6175(6) . ? Sn2 Br2 2.6608(4) . ? 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 N2 Sn1 N1 68.18(7) . . ? N2 Sn1 N3 68.76(7) . . ? N1 Sn1 N3 136.94(7) . . ? N2 Sn1 Br1 85.45(6) . . ? N1 Sn1 Br1 93.75(5) . . ? N3 Sn1 Br1 82.81(5) . . ? N2 Sn1 Br2 70.29(6) . . ? N1 Sn1 Br2 78.29(5) . . ? N3 Sn1 Br2 87.53(5) . . ? Br1 Sn1 Br2 155.727(15) . . ? C1 N1 C20 119.6(2) . . ? C1 N1 Sn1 113.38(17) . . ? C20 N1 Sn1 118.02(16) . . ? C6 N2 C2 120.1(2) . . ? C6 N2 Sn1 119.50(17) . . ? C2 N2 Sn1 120.36(17) . . ? C7 N3 C34 119.2(2) . . ? C7 N3 Sn1 111.12(17) . . ? C34 N3 Sn1 121.51(16) . . ? N1 C1 C2 115.7(2) . . ? N1 C1 C8 125.9(3) . . ? C2 C1 C8 118.4(2) . . ? N2 C2 C3 121.2(2) . . ? N2 C2 C1 116.2(2) . . ? C3 C2 C1 122.6(2) . . ? C4 C3 C2 119.2(3) . . ? C3 C4 C5 119.1(3) . . ? C4 C5 C6 119.8(3) . . ? N2 C6 C5 120.6(2) . . ? N2 C6 C7 117.2(2) . . ? C5 C6 C7 122.1(2) . . ? N3 C7 C6 117.6(2) . . ? N3 C7 C14 125.3(2) . . ? C6 C7 C14 117.0(2) . . ? C9 C8 C13 119.7(3) . . ? C9 C8 C1 118.3(3) . . ? C13 C8 C1 121.9(3) . . ? C10 C9 C8 120.2(3) . . ? C11 C10 C9 120.4(4) . . ? C10 C11 C12 120.0(3) . . ? C11 C12 C13 120.8(4) . . ? C12 C13 C8 119.0(4) . . ? C19 C14 C15 120.2(3) . . ? C19 C14 C7 121.6(3) . . ? C15 C14 C7 118.1(3) . . ? C14 C15 C16 119.8(3) . . ? C17 C16 C15 119.9(4) . . ? C16 C17 C18 120.9(3) . . ? C17 C18 C19 120.2(4) . . ? C14 C19 C18 119.0(4) . . ? C21 C20 C25 122.0(3) . . ? C21 C20 N1 122.8(3) . . ? C25 C20 N1 115.2(2) . . ? C20 C21 C22 114.1(3) . . ? C20 C21 C26 128.1(3) . . ? C22 C21 C26 117.7(3) . . ? C23 C22 C21 124.3(3) . . ? C24 C23 C22 120.7(3) . . ? C25 C24 C23 116.3(3) . . ? C25 C24 C30 122.4(3) . . ? C23 C24 C30 121.2(3) . . ? C24 C25 C20 122.4(3) . . ? C27 C26 C28 108.9(3) . . ? C27 C26 C21 109.1(3) . . ? C28 C26 C21 109.0(3) . . ? C27 C26 C29 108.5(3) . . ? C28 C26 C29 106.0(3) . . ? C21 C26 C29 115.1(3) . . ? C32 C30 C31 109.1(3) . . ? C32 C30 C33 108.3(4) . . ? C31 C30 C33 109.3(4) . . ? C32 C30 C24 108.1(3) . . ? C31 C30 C24 110.7(3) . . ? C33 C30 C24 111.2(3) . . ? C39 C34 C35 121.7(3) . . ? C39 C34 N3 114.9(2) . . ? C35 C34 N3 123.5(3) . . ? C36 C35 C34 114.4(3) . . ? C36 C35 C40 120.7(3) . . ? C34 C35 C40 124.8(2) . . ? C37 C36 C35 123.8(3) . . ? C38 C37 C36 121.1(3) . . ? C37 C38 C39 116.2(3) . . ? C37 C38 C44 121.7(3) . . ? C39 C38 C44 121.9(3) . . ? C34 C39 C38 122.7(3) . . ? C41 C40 C42 110.3(3) . . ? C41 C40 C35 112.6(3) . . ? C42 C40 C35 108.2(3) . . ? C41 C40 C43 106.4(3) . . ? C42 C40 C43 108.2(3) . . ? C35 C40 C43 111.2(3) . . ? C46 C44 C45 110.0(3) . . ? C46 C44 C47 107.4(3) . . ? C45 C44 C47 108.8(3) . . ? C46 C44 C38 110.3(3) . . ? C45 C44 C38 108.1(3) . . ? C47 C44 C38 112.3(2) . . ? Br3 Sn2 Br4 93.00(2) . . ? Br3 Sn2 Br2 92.131(18) . . ? Br4 Sn2 Br2 97.956(17) . . ? Sn2 Br2 Sn1 152.513(16) . . ? 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 N2 Sn1 N1 C1 -21.35(19) . . . . ? N3 Sn1 N1 C1 -21.4(2) . . . . ? Br1 Sn1 N1 C1 -104.93(19) . . . . ? Br2 Sn1 N1 C1 51.91(19) . . . . ? N2 Sn1 N1 C20 -168.4(2) . . . . ? N3 Sn1 N1 C20 -168.45(17) . . . . ? Br1 Sn1 N1 C20 108.07(18) . . . . ? Br2 Sn1 N1 C20 -95.09(18) . . . . ? N1 Sn1 N2 C6 -169.0(2) . . . . ? N3 Sn1 N2 C6 10.90(19) . . . . ? Br1 Sn1 N2 C6 -73.15(19) . . . . ? Br2 Sn1 N2 C6 106.1(2) . . . . ? N1 Sn1 N2 C2 12.27(19) . . . . ? N3 Sn1 N2 C2 -167.8(2) . . . . ? Br1 Sn1 N2 C2 108.16(19) . . . . ? Br2 Sn1 N2 C2 -72.63(19) . . . . ? N2 Sn1 N3 C7 -20.11(18) . . . . ? N1 Sn1 N3 C7 -20.0(2) . . . . ? Br1 Sn1 N3 C7 67.78(18) . . . . ? Br2 Sn1 N3 C7 -89.91(18) . . . . ? N2 Sn1 N3 C34 -168.4(2) . . . . ? N1 Sn1 N3 C34 -168.32(18) . . . . ? Br1 Sn1 N3 C34 -80.5(2) . . . . ? Br2 Sn1 N3 C34 121.8(2) . . . . ? C20 N1 C1 C2 173.6(2) . . . . ? Sn1 N1 C1 C2 27.2(3) . . . . ? C20 N1 C1 C8 -4.9(4) . . . . ? Sn1 N1 C1 C8 -151.3(2) . . . . ? C6 N2 C2 C3 0.0(4) . . . . ? Sn1 N2 C2 C3 178.7(2) . . . . ? C6 N2 C2 C1 177.7(2) . . . . ? Sn1 N2 C2 C1 -3.6(3) . . . . ? N1 C1 C2 N2 -17.3(4) . . . . ? C8 C1 C2 N2 161.3(2) . . . . ? N1 C1 C2 C3 160.4(3) . . . . ? C8 C1 C2 C3 -21.0(4) . . . . ? N2 C2 C3 C4 0.8(4) . . . . ? C1 C2 C3 C4 -176.8(3) . . . . ? C2 C3 C4 C5 -0.2(5) . . . . ? C3 C4 C5 C6 -1.0(5) . . . . ? C2 N2 C6 C5 -1.3(4) . . . . ? Sn1 N2 C6 C5 180.0(2) . . . . ? C2 N2 C6 C7 176.7(2) . . . . ? Sn1 N2 C6 C7 -2.0(3) . . . . ? C4 C5 C6 N2 1.8(4) . . . . ? C4 C5 C6 C7 -176.1(3) . . . . ? C34 N3 C7 C6 175.8(2) . . . . ? Sn1 N3 C7 C6 26.7(3) . . . . ? C34 N3 C7 C14 -2.3(4) . . . . ? Sn1 N3 C7 C14 -151.4(2) . . . . ? N2 C6 C7 N3 -18.7(4) . . . . ? C5 C6 C7 N3 159.3(3) . . . . ? N2 C6 C7 C14 159.6(2) . . . . ? C5 C6 C7 C14 -22.4(4) . . . . ? N1 C1 C8 C9 122.5(3) . . . . ? C2 C1 C8 C9 -56.0(4) . . . . ? N1 C1 C8 C13 -53.0(4) . . . . ? C2 C1 C8 C13 128.6(3) . . . . ? C13 C8 C9 C10 1.6(5) . . . . ? C1 C8 C9 C10 -173.9(3) . . . . ? C8 C9 C10 C11 -1.0(6) . . . . ? C9 C10 C11 C12 -0.9(6) . . . . ? C10 C11 C12 C13 2.0(6) . . . . ? C11 C12 C13 C8 -1.3(5) . . . . ? C9 C8 C13 C12 -0.5(5) . . . . ? C1 C8 C13 C12 174.9(3) . . . . ? N3 C7 C14 C19 -68.3(4) . . . . ? C6 C7 C14 C19 113.5(3) . . . . ? N3 C7 C14 C15 109.8(3) . . . . ? C6 C7 C14 C15 -68.4(4) . . . . ? C19 C14 C15 C16 2.5(5) . . . . ? C7 C14 C15 C16 -175.7(3) . . . . ? C14 C15 C16 C17 -1.8(5) . . . . ? C15 C16 C17 C18 0.3(6) . . . . ? C16 C17 C18 C19 0.5(7) . . . . ? C15 C14 C19 C18 -1.6(6) . . . . ? C7 C14 C19 C18 176.5(4) . . . . ? C17 C18 C19 C14 0.1(7) . . . . ? C1 N1 C20 C21 120.0(3) . . . . ? Sn1 N1 C20 C21 -95.1(3) . . . . ? C1 N1 C20 C25 -61.9(3) . . . . ? Sn1 N1 C20 C25 83.0(3) . . . . ? C25 C20 C21 C22 -2.7(4) . . . . ? N1 C20 C21 C22 175.2(3) . . . . ? C25 C20 C21 C26 174.7(3) . . . . ? N1 C20 C21 C26 -7.4(5) . . . . ? C20 C21 C22 C23 3.4(6) . . . . ? C26 C21 C22 C23 -174.3(4) . . . . ? C21 C22 C23 C24 0.0(7) . . . . ? C22 C23 C24 C25 -4.1(6) . . . . ? C22 C23 C24 C30 173.3(4) . . . . ? C23 C24 C25 C20 4.7(5) . . . . ? C30 C24 C25 C20 -172.6(3) . . . . ? C21 C20 C25 C24 -1.3(4) . . . . ? N1 C20 C25 C24 -179.4(3) . . . . ? C20 C21 C26 C27 103.3(4) . . . . ? C22 C21 C26 C27 -79.3(4) . . . . ? C20 C21 C26 C28 -137.9(4) . . . . ? C22 C21 C26 C28 39.5(4) . . . . ? C20 C21 C26 C29 -19.0(5) . . . . ? C22 C21 C26 C29 158.4(3) . . . . ? C25 C24 C30 C32 112.3(4) . . . . ? C23 C24 C30 C32 -64.9(5) . . . . ? C25 C24 C30 C31 -128.2(4) . . . . ? C23 C24 C30 C31 54.6(5) . . . . ? C25 C24 C30 C33 -6.6(5) . . . . ? C23 C24 C30 C33 176.3(4) . . . . ? C7 N3 C34 C39 -63.7(3) . . . . ? Sn1 N3 C34 C39 82.2(3) . . . . ? C7 N3 C34 C35 116.7(3) . . . . ? Sn1 N3 C34 C35 -97.4(3) . . . . ? C39 C34 C35 C36 3.3(4) . . . . ? N3 C34 C35 C36 -177.1(3) . . . . ? C39 C34 C35 C40 -173.9(3) . . . . ? N3 C34 C35 C40 5.7(4) . . . . ? C34 C35 C36 C37 -1.6(5) . . . . ? C40 C35 C36 C37 175.7(3) . . . . ? C35 C36 C37 C38 -1.3(5) . . . . ? C36 C37 C38 C39 2.5(4) . . . . ? C36 C37 C38 C44 177.8(3) . . . . ? C35 C34 C39 C38 -2.2(4) . . . . ? N3 C34 C39 C38 178.2(2) . . . . ? C37 C38 C39 C34 -0.8(4) . . . . ? C44 C38 C39 C34 -176.1(3) . . . . ? C36 C35 C40 C41 130.5(3) . . . . ? C34 C35 C40 C41 -52.5(4) . . . . ? C36 C35 C40 C42 -107.4(3) . . . . ? C34 C35 C40 C42 69.6(4) . . . . ? C36 C35 C40 C43 11.3(4) . . . . ? C34 C35 C40 C43 -171.7(3) . . . . ? C37 C38 C44 C46 47.7(4) . . . . ? C39 C38 C44 C46 -137.3(3) . . . . ? C37 C38 C44 C45 -72.5(4) . . . . ? C39 C38 C44 C45 102.5(3) . . . . ? C37 C38 C44 C47 167.4(3) . . . . ? C39 C38 C44 C47 -17.6(4) . . . . ? Br3 Sn2 Br2 Sn1 145.97(3) . . . . ? Br4 Sn2 Br2 Sn1 52.65(4) . . . . ? N2 Sn1 Br2 Sn2 -34.97(6) . . . . ? N1 Sn1 Br2 Sn2 -105.77(6) . . . . ? N3 Sn1 Br2 Sn2 33.33(6) . . . . ? Br1 Sn1 Br2 Sn2 -33.06(5) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.024 _refine_diff_density_min -1.241 _refine_diff_density_rms 0.082 _database_code_depnum_ccdc_archive 'CCDC 909098' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_dr018 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48.40 H57.45 Cl4 N3 O0.35 Sn2' _chemical_formula_weight 1066.00 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6251(5) _cell_length_b 14.0413(7) _cell_length_c 19.5349(10) _cell_angle_alpha 74.108(2) _cell_angle_beta 77.877(3) _cell_angle_gamma 75.277(2) _cell_volume 2679.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9938 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 28.30 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_density_meas n/a _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_F_000 1079 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 1.164 _shelx_estimated_absorpt_T_min 0.776 _shelx_estimated_absorpt_T_max 0.944 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.481 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with four batch runs at phi = 0.00 deg (600 frames), at phi = 90.00 deg (600 frames), at phi = 180.00 deg (600 frames), and at phi = 270.00 deg (600 frames). A fifth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33517 _diffrn_reflns_av_unetI/netI 0.0554 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.005 _diffrn_reflns_theta_max 24.712 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.965 _diffrn_measured_fraction_theta_full 0.910 _diffrn_reflns_Laue_measured_fraction_max 0.965 _diffrn_reflns_Laue_measured_fraction_full 0.910 _diffrn_reflns_point_group_measured_fraction_max 0.965 _diffrn_reflns_point_group_measured_fraction_full 0.910 _reflns_number_total 8822 _reflns_number_gt 6520 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-03 (Sheldrick, 2003)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+39.6697P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8822 _refine_ls_number_parameters 575 _refine_ls_number_restraints 196 _refine_ls_R_factor_all 0.1094 _refine_ls_R_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.1973 _refine_ls_wR_factor_gt 0.1747 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.081 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.31663(6) 0.02576(5) 0.19485(3) 0.02927(19) Uani 1 1 d . . . . . Cl1 Cl 0.1199(3) 0.07379(19) 0.13497(14) 0.0432(6) Uani 1 1 d . . . . . N1 N 0.2852(7) 0.1975(5) 0.2147(4) 0.0279(16) Uani 1 1 d . . . . . N2 N 0.1647(7) 0.0470(5) 0.2939(4) 0.0228(15) Uani 1 1 d . . . . . N3 N 0.2288(7) -0.1303(5) 0.2502(4) 0.0278(17) Uani 1 1 d . . . . . C1 C 0.2248(9) 0.2067(7) 0.2781(5) 0.030(2) Uani 1 1 d . . . . . C2 C 0.1424(8) 0.1314(6) 0.3171(4) 0.0217(18) Uani 1 1 d . . . . . C3 C 0.0477(9) 0.1478(7) 0.3755(5) 0.031(2) Uani 1 1 d . . . . . H3A H 0.0307 0.2091 0.3907 0.037 Uiso 1 1 calc R U . . . C4 C -0.0225(9) 0.0725(7) 0.4115(5) 0.035(2) Uani 1 1 d . . . . . H4A H -0.0877 0.0819 0.4520 0.041 Uiso 1 1 calc R U . . . C5 C 0.0036(9) -0.0159(7) 0.3880(5) 0.031(2) Uani 1 1 d . . . . . H5A H -0.0415 -0.0687 0.4128 0.037 Uiso 1 1 calc R U . . . C6 C 0.0973(8) -0.0261(6) 0.3272(5) 0.0240(18) Uani 1 1 d . . . . . C7 C 0.2295(9) 0.2866(7) 0.3136(5) 0.030(2) Uani 1 1 d . . . . . C8 C 0.2046(11) 0.3877(7) 0.2788(6) 0.042(3) Uani 1 1 d . . . . . H8A H 0.1817 0.4070 0.2318 0.051 Uiso 1 1 calc R U . . . C9 C 0.2123(13) 0.4611(8) 0.3112(6) 0.054(3) Uani 1 1 d . . . . . H9A H 0.1945 0.5305 0.2869 0.065 Uiso 1 1 calc R U . . . C10 C 0.2462(12) 0.4328(9) 0.3791(7) 0.054(3) Uani 1 1 d . . . . . H10A H 0.2517 0.4833 0.4016 0.065 Uiso 1 1 calc R U . . . C11 C 0.2722(11) 0.3330(9) 0.4149(6) 0.050(3) Uani 1 1 d . . . . . H11A H 0.2954 0.3147 0.4618 0.060 Uiso 1 1 calc R U . . . C12 C 0.2645(10) 0.2588(8) 0.3826(6) 0.042(2) Uani 1 1 d . . . . . H12A H 0.2829 0.1895 0.4071 0.051 Uiso 1 1 calc R U . . . C13 C 0.1251(8) -0.1171(6) 0.2976(5) 0.0258(19) Uani 1 1 d . . . . . C14 C 0.0279(9) -0.1836(6) 0.3240(5) 0.028(2) Uani 1 1 d . . . . . C15 C -0.1016(9) -0.1432(8) 0.3108(6) 0.041(2) Uani 1 1 d . . . . . H15A H -0.1255 -0.0747 0.2855 0.049 Uiso 1 1 calc R U . . . C16 C -0.1955(11) -0.2030(9) 0.3347(7) 0.052(3) Uani 1 1 d . . . . . H16A H -0.2833 -0.1757 0.3253 0.062 Uiso 1 1 calc R U . . . C17 C -0.1608(12) -0.3011(9) 0.3718(8) 0.061(4) Uani 1 1 d . . . . . H17A H -0.2250 -0.3419 0.3879 0.074 Uiso 1 1 calc R U . . . C18 C -0.0336(13) -0.3419(9) 0.3863(8) 0.067(4) Uani 1 1 d . . . . . H18A H -0.0108 -0.4098 0.4130 0.081 Uiso 1 1 calc R U . . . C19 C 0.0605(10) -0.2822(7) 0.3613(7) 0.048(3) Uani 1 1 d . . . . . H19A H 0.1485 -0.3102 0.3701 0.057 Uiso 1 1 calc R U . . . C20 C 0.3864(9) 0.2558(7) 0.1808(5) 0.028(2) Uani 1 1 d . . . . . C21 C 0.3878(9) 0.3212(7) 0.1123(5) 0.032(2) Uani 1 1 d . . . . . C22 C 0.4966(11) 0.3674(8) 0.0898(6) 0.048(3) Uani 1 1 d . . . . . H22A H 0.5020 0.4136 0.0441 0.057 Uiso 1 1 calc R U . . . C23 C 0.5974(11) 0.3503(8) 0.1299(6) 0.048(3) Uani 1 1 d . . . . . H23A H 0.6663 0.3867 0.1119 0.058 Uiso 1 1 calc R U . . . C24 C 0.5982(9) 0.2806(7) 0.1959(5) 0.036(2) Uani 1 1 d . . . . . C25 C 0.4898(8) 0.2359(6) 0.2199(5) 0.028(2) Uani 1 1 d . . . . . H25A H 0.4856 0.1892 0.2655 0.033 Uiso 1 1 calc R U . . . C26 C 0.2868(9) 0.3410(7) 0.0621(5) 0.034(2) Uani 1 1 d . . . . . C27 C 0.2936(12) 0.4376(9) 0.0018(6) 0.054(3) Uani 1 1 d . . . . . H27A H 0.3840 0.4339 -0.0238 0.081 Uiso 1 1 calc R U . . . H27B H 0.2670 0.4969 0.0228 0.081 Uiso 1 1 calc R U . . . H27C H 0.2343 0.4435 -0.0321 0.081 Uiso 1 1 calc R U . . . C28 C 0.3222(12) 0.2536(8) 0.0241(6) 0.050(3) Uani 1 1 d . . . . . H28A H 0.4128 0.2485 -0.0011 0.075 Uiso 1 1 calc R U . . . H28B H 0.2620 0.2663 -0.0107 0.075 Uiso 1 1 calc R U . . . H28C H 0.3143 0.1902 0.0598 0.075 Uiso 1 1 calc R U . . . C29 C 0.1441(10) 0.3499(9) 0.1010(6) 0.048(3) Uani 1 1 d . . . . . H29A H 0.1213 0.4063 0.1249 0.072 Uiso 1 1 calc R U . . . H29B H 0.1355 0.2868 0.1370 0.072 Uiso 1 1 calc R U . . . H29C H 0.0846 0.3623 0.0659 0.072 Uiso 1 1 calc R U . . . C30 C 0.7081(10) 0.2538(8) 0.2419(6) 0.047(3) Uani 1 1 d . . . . . C31 C 0.8126(12) 0.3178(11) 0.2078(8) 0.070(4) Uani 1 1 d . . . . . H31A H 0.8512 0.3060 0.1599 0.105 Uiso 1 1 calc R U . . . H31B H 0.8818 0.2985 0.2382 0.105 Uiso 1 1 calc R U . . . H31C H 0.7717 0.3896 0.2035 0.105 Uiso 1 1 calc R U . . . C32 C 0.7741(13) 0.1424(9) 0.2477(8) 0.071(4) Uani 1 1 d . . . . . H32A H 0.7086 0.1004 0.2697 0.106 Uiso 1 1 calc R U . . . H32B H 0.8440 0.1239 0.2775 0.106 Uiso 1 1 calc R U . . . H32C H 0.8120 0.1314 0.1995 0.106 Uiso 1 1 calc R U . . . C33 C 0.6493(13) 0.2706(10) 0.3178(6) 0.061(3) Uani 1 1 d . . . . . H33A H 0.5842 0.2283 0.3400 0.092 Uiso 1 1 calc R U . . . H33B H 0.6065 0.3420 0.3143 0.092 Uiso 1 1 calc R U . . . H33C H 0.7196 0.2522 0.3473 0.092 Uiso 1 1 calc R U . . . C34 C 0.2503(9) -0.2064(7) 0.2093(5) 0.031(2) Uani 1 1 d . . . . . C35 C 0.3649(9) -0.2802(7) 0.2034(5) 0.032(2) Uani 1 1 d . . . . . C36 C 0.3672(11) -0.3428(9) 0.1587(6) 0.049(3) Uani 1 1 d . . . . . H36A H 0.4420 -0.3960 0.1542 0.059 Uiso 1 1 calc R U . . . C37 C 0.2674(11) -0.3318(8) 0.1209(7) 0.053(3) Uani 1 1 d . . . . . H37A H 0.2757 -0.3768 0.0909 0.064 Uiso 1 1 calc R U . . . C38 C 0.1541(11) -0.2564(8) 0.1255(6) 0.046(3) Uani 1 1 d . . . . . C39 C 0.1496(9) -0.1941(7) 0.1700(5) 0.033(2) Uani 1 1 d . . . . . H39A H 0.0748 -0.1408 0.1741 0.039 Uiso 1 1 calc R U . . . C40 C 0.4860(10) -0.2989(8) 0.2415(5) 0.038(2) Uani 1 1 d . U . . . C41 C 0.561(3) -0.2136(16) 0.2062(14) 0.039(5) Uani 0.5 1 d D U P A 1 H41A H 0.5147 -0.1524 0.2229 0.058 Uiso 0.5 1 calc R U P A 1 H41B H 0.5678 -0.1996 0.1538 0.058 Uiso 0.5 1 calc R U P A 1 H41C H 0.6501 -0.2344 0.2194 0.058 Uiso 0.5 1 calc R U P A 1 C42 C 0.442(4) -0.306(2) 0.3222(14) 0.048(7) Uani 0.5 1 d D U P A 1 H42A H 0.3750 -0.2460 0.3295 0.072 Uiso 0.5 1 calc R U P A 1 H42B H 0.5181 -0.3101 0.3448 0.072 Uiso 0.5 1 calc R U P A 1 H42C H 0.4056 -0.3668 0.3441 0.072 Uiso 0.5 1 calc R U P A 1 C43 C 0.588(3) -0.3978(17) 0.2320(15) 0.046(6) Uani 0.5 1 d D U P A 1 H43A H 0.6464 -0.4176 0.2686 0.069 Uiso 0.5 1 calc R U P A 1 H43B H 0.6408 -0.3859 0.1840 0.069 Uiso 0.5 1 calc R U P A 1 H43C H 0.5420 -0.4521 0.2374 0.069 Uiso 0.5 1 calc R U P A 1 C41' C 0.586(4) -0.243(2) 0.1913(17) 0.066(8) Uani 0.5 1 d D U P A 2 H41D H 0.6132 -0.2676 0.1471 0.098 Uiso 0.5 1 calc R U P A 2 H41E H 0.6634 -0.2541 0.2149 0.098 Uiso 0.5 1 calc R U P A 2 H41F H 0.5474 -0.1702 0.1794 0.098 Uiso 0.5 1 calc R U P A 2 C42' C 0.448(3) -0.267(2) 0.3135(14) 0.041(6) Uani 0.5 1 d D U P A 2 H42D H 0.4990 -0.3168 0.3491 0.061 Uiso 0.5 1 calc R U P A 2 H42E H 0.3539 -0.2646 0.3305 0.061 Uiso 0.5 1 calc R U P A 2 H42F H 0.4670 -0.2004 0.3071 0.061 Uiso 0.5 1 calc R U P A 2 C43' C 0.550(3) -0.4135(18) 0.2580(17) 0.061(7) Uani 0.5 1 d D U P A 2 H43D H 0.5637 -0.4387 0.2144 0.091 Uiso 0.5 1 calc R U P A 2 H43E H 0.4911 -0.4503 0.2959 0.091 Uiso 0.5 1 calc R U P A 2 H43F H 0.6343 -0.4239 0.2743 0.091 Uiso 0.5 1 calc R U P A 2 C44 C 0.0407(13) -0.2443(11) 0.0841(8) 0.068(3) Uani 1 1 d . U . . . C45 C 0.093(4) -0.246(3) 0.007(2) 0.080(8) Uani 0.6 1 d . U P B 1 H45A H 0.0243 -0.2538 -0.0162 0.120 Uiso 0.6 1 calc R U P B 1 H45B H 0.1690 -0.3020 0.0043 0.120 Uiso 0.6 1 calc R U P B 1 H45C H 0.1204 -0.1816 -0.0181 0.120 Uiso 0.6 1 calc R U P B 1 C46 C -0.074(2) -0.1616(19) 0.0964(14) 0.061(5) Uani 0.6 1 d . U P B 1 H46A H -0.0959 -0.1629 0.1479 0.092 Uiso 0.6 1 calc R U P B 1 H46B H -0.1502 -0.1711 0.0797 0.092 Uiso 0.6 1 calc R U P B 1 H46C H -0.0533 -0.0962 0.0696 0.092 Uiso 0.6 1 calc R U P B 1 C47 C -0.018(3) -0.349(2) 0.1194(17) 0.084(6) Uani 0.6 1 d . U P B 1 H47A H -0.0252 -0.3647 0.1720 0.126 Uiso 0.6 1 calc R U P B 1 H47B H 0.0421 -0.4054 0.1011 0.126 Uiso 0.6 1 calc R U P B 1 H47C H -0.1048 -0.3391 0.1059 0.126 Uiso 0.6 1 calc R U P B 1 C45' C 0.081(6) -0.282(4) 0.017(3) 0.073(9) Uani 0.4 1 d . U P B 2 H45D H 0.1523 -0.2502 -0.0133 0.109 Uiso 0.4 1 calc R U P B 2 H45E H 0.0058 -0.2645 -0.0087 0.109 Uiso 0.4 1 calc R U P B 2 H45F H 0.1120 -0.3555 0.0295 0.109 Uiso 0.4 1 calc R U P B 2 C46' C -0.012(4) -0.124(3) 0.056(3) 0.090(9) Uani 0.4 1 d . U P B 2 H46D H 0.0572 -0.0945 0.0220 0.135 Uiso 0.4 1 calc R U P B 2 H46E H -0.0363 -0.0922 0.0975 0.135 Uiso 0.4 1 calc R U P B 2 H46F H -0.0895 -0.1119 0.0329 0.135 Uiso 0.4 1 calc R U P B 2 C47' C -0.062(4) -0.300(4) 0.135(3) 0.089(9) Uani 0.4 1 d . U P B 2 H47D H -0.1093 -0.3226 0.1064 0.134 Uiso 0.4 1 calc R U P B 2 H47E H -0.1238 -0.2539 0.1620 0.134 Uiso 0.4 1 calc R U P B 2 H47F H -0.0176 -0.3585 0.1680 0.134 Uiso 0.4 1 calc R U P B 2 Sn2 Sn 0.45305(7) 0.87432(5) 0.46568(4) 0.0366(2) Uani 1 1 d . . . . . Cl2 Cl 0.3164(3) 1.0121(2) 0.52166(16) 0.0498(7) Uani 1 1 d . . . . . Cl3 Cl 0.4585(3) 0.9838(2) 0.34097(14) 0.0477(7) Uani 1 1 d . . . . . Cl4 Cl 0.2540(3) 0.8120(2) 0.46181(14) 0.0441(6) Uani 1 1 d . . . . . O1 O 0.494(3) -0.004(2) 0.0264(13) 0.080(5) Uiso 0.35 1 d D . P C -1 C48 C 0.454(4) -0.013(4) -0.0403(17) 0.080(5) Uiso 0.35 1 d D . P C -1 H48A H 0.4343 0.0560 -0.0720 0.096 Uiso 0.35 1 calc R U P C -1 H48B H 0.5298 -0.0530 -0.0662 0.096 Uiso 0.35 1 calc R U P C -1 C49 C 0.339(4) -0.059(3) -0.028(2) 0.080(5) Uiso 0.35 1 d D . P C -1 H49A H 0.3524 -0.1240 0.0074 0.120 Uiso 0.35 1 calc R U P C -1 H49B H 0.3284 -0.0715 -0.0738 0.120 Uiso 0.35 1 calc R U P C -1 H49C H 0.2594 -0.0139 -0.0110 0.120 Uiso 0.35 1 calc R U P C -1 C50 C 0.613(3) 0.038(4) 0.0109(18) 0.080(5) Uiso 0.35 1 d D . P C -1 H50A H 0.5970 0.1040 -0.0244 0.096 Uiso 0.35 1 calc R U P C -1 H50B H 0.6855 -0.0079 -0.0122 0.096 Uiso 0.35 1 calc R U P C -1 C51 C 0.657(4) 0.054(3) 0.076(2) 0.080(5) Uiso 0.35 1 d D . P C -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 0.0321(4) 0.0291(4) 0.0271(3) -0.0127(3) 0.0000(3) -0.0043(3) Cl1 0.0514(16) 0.0425(14) 0.0380(14) -0.0061(11) -0.0186(12) -0.0080(12) N1 0.028(4) 0.028(4) 0.024(4) -0.004(3) -0.002(3) -0.004(3) N2 0.023(4) 0.021(4) 0.025(4) -0.007(3) -0.004(3) -0.003(3) N3 0.026(4) 0.026(4) 0.032(4) -0.013(3) -0.006(3) 0.003(3) C1 0.031(5) 0.027(5) 0.030(5) -0.003(4) -0.010(4) 0.000(4) C2 0.025(4) 0.024(4) 0.018(4) -0.013(3) 0.002(3) -0.003(3) C3 0.035(5) 0.034(5) 0.031(5) -0.019(4) -0.005(4) -0.008(4) C4 0.033(5) 0.038(6) 0.034(5) -0.019(4) 0.002(4) -0.004(4) C5 0.031(5) 0.032(5) 0.029(5) -0.012(4) 0.001(4) -0.006(4) C6 0.020(4) 0.025(5) 0.028(5) -0.012(4) -0.005(4) 0.002(4) C7 0.026(5) 0.028(5) 0.040(5) -0.019(4) -0.003(4) -0.003(4) C8 0.061(7) 0.029(5) 0.038(6) -0.013(4) -0.008(5) -0.003(5) C9 0.082(9) 0.026(6) 0.055(7) -0.009(5) -0.017(6) -0.008(6) C10 0.065(8) 0.038(7) 0.074(9) -0.032(6) -0.017(7) -0.010(6) C11 0.057(7) 0.057(8) 0.047(7) -0.028(6) -0.014(5) -0.009(6) C12 0.047(6) 0.035(6) 0.047(6) -0.014(5) -0.015(5) -0.001(5) C13 0.028(5) 0.022(5) 0.027(5) -0.005(4) -0.011(4) 0.001(4) C14 0.029(5) 0.023(5) 0.035(5) -0.018(4) 0.000(4) -0.001(4) C15 0.030(5) 0.042(6) 0.050(6) -0.013(5) -0.004(5) -0.004(4) C16 0.030(6) 0.055(8) 0.077(8) -0.032(7) -0.002(6) -0.010(5) C17 0.044(7) 0.051(8) 0.097(10) -0.030(7) 0.008(7) -0.027(6) C18 0.064(9) 0.040(7) 0.089(10) 0.000(7) -0.001(7) -0.020(6) C19 0.034(6) 0.028(6) 0.073(8) -0.010(5) 0.000(5) 0.000(4) C20 0.030(5) 0.025(5) 0.029(5) -0.007(4) -0.001(4) -0.007(4) C21 0.036(5) 0.029(5) 0.029(5) -0.008(4) -0.001(4) -0.004(4) C22 0.050(7) 0.048(7) 0.038(6) 0.005(5) -0.003(5) -0.018(5) C23 0.041(6) 0.043(6) 0.051(7) 0.015(5) -0.011(5) -0.016(5) C24 0.029(5) 0.030(5) 0.042(6) -0.004(4) -0.002(4) -0.004(4) C25 0.030(5) 0.022(5) 0.026(5) -0.003(4) 0.004(4) -0.005(4) C26 0.037(5) 0.031(5) 0.030(5) -0.002(4) -0.004(4) -0.009(4) C27 0.064(8) 0.049(7) 0.047(7) 0.004(5) -0.020(6) -0.016(6) C28 0.060(7) 0.048(7) 0.048(7) -0.017(5) -0.005(6) -0.017(6) C29 0.039(6) 0.060(7) 0.042(6) -0.010(5) -0.015(5) -0.001(5) C30 0.036(6) 0.046(6) 0.052(7) 0.005(5) -0.011(5) -0.013(5) C31 0.049(7) 0.087(10) 0.077(9) 0.000(8) -0.022(7) -0.030(7) C32 0.056(8) 0.048(7) 0.102(11) -0.003(7) -0.033(8) 0.004(6) C33 0.060(8) 0.076(9) 0.049(7) -0.008(6) -0.015(6) -0.016(7) C34 0.035(5) 0.029(5) 0.029(5) -0.011(4) -0.006(4) -0.002(4) C35 0.030(5) 0.030(5) 0.033(5) -0.010(4) -0.007(4) 0.001(4) C36 0.049(7) 0.051(7) 0.047(6) -0.025(5) -0.016(5) 0.014(5) C37 0.056(7) 0.044(7) 0.072(8) -0.049(6) -0.023(6) 0.017(5) C38 0.050(7) 0.048(7) 0.043(6) -0.020(5) -0.018(5) 0.003(5) C39 0.036(5) 0.035(5) 0.031(5) -0.021(4) -0.008(4) 0.002(4) C40 0.035(5) 0.042(5) 0.038(5) -0.014(4) -0.012(4) 0.002(4) C41 0.032(11) 0.034(8) 0.048(11) -0.012(7) -0.016(8) 0.009(7) C42 0.049(14) 0.046(14) 0.040(7) -0.013(7) -0.014(6) 0.013(12) C43 0.039(11) 0.042(8) 0.055(14) -0.016(8) -0.012(9) 0.004(7) C41' 0.054(14) 0.073(14) 0.062(12) -0.010(10) 0.000(10) -0.012(13) C42' 0.022(10) 0.056(14) 0.049(8) -0.022(9) -0.017(7) 0.004(11) C43' 0.061(18) 0.053(8) 0.061(16) -0.015(7) -0.014(11) 0.008(7) C44 0.054(6) 0.087(8) 0.081(8) -0.049(7) -0.040(5) 0.011(5) C45 0.085(15) 0.091(18) 0.079(9) -0.046(10) -0.035(8) 0.002(14) C46 0.040(9) 0.085(10) 0.080(13) -0.044(10) -0.040(8) 0.004(7) C47 0.076(15) 0.089(11) 0.105(14) -0.045(10) -0.040(11) -0.005(10) C45' 0.062(18) 0.094(19) 0.085(12) -0.050(13) -0.036(11) -0.005(16) C46' 0.08(2) 0.094(11) 0.109(19) -0.049(10) -0.053(15) 0.014(9) C47' 0.061(15) 0.117(17) 0.103(15) -0.044(13) -0.034(11) -0.002(14) Sn2 0.0347(4) 0.0384(4) 0.0330(4) -0.0047(3) -0.0076(3) -0.0031(3) Cl2 0.0435(15) 0.0565(17) 0.0556(17) -0.0272(14) 0.0076(12) -0.0182(13) Cl3 0.0453(15) 0.0533(16) 0.0361(14) 0.0022(12) -0.0063(11) -0.0089(12) Cl4 0.0428(15) 0.0530(16) 0.0431(14) -0.0240(12) -0.0036(11) -0.0101(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 N2 2.280(7) . ? Sn1 Cl1 2.464(3) . ? Sn1 N1 2.475(7) . ? Sn1 N3 2.482(7) . ? N1 C1 1.294(11) . ? N1 C20 1.454(11) . ? N2 C2 1.331(10) . ? N2 C6 1.342(11) . ? N3 C13 1.292(11) . ? N3 C34 1.449(11) . ? C1 C7 1.486(12) . ? C1 C2 1.489(12) . ? C2 C3 1.382(12) . ? C3 C4 1.392(13) . ? C4 C5 1.383(13) . ? C5 C6 1.395(12) . ? C6 C13 1.482(12) . ? C7 C8 1.380(13) . ? C7 C12 1.399(14) . ? C8 C9 1.374(14) . ? C9 C10 1.373(16) . ? C10 C11 1.369(16) . ? C11 C12 1.383(14) . ? C13 C14 1.485(12) . ? C14 C19 1.370(14) . ? C14 C15 1.397(13) . ? C15 C16 1.390(15) . ? C16 C17 1.366(17) . ? C17 C18 1.383(18) . ? C18 C19 1.393(16) . ? C20 C21 1.400(13) . ? C20 C25 1.396(13) . ? C21 C22 1.401(14) . ? C21 C26 1.528(13) . ? C22 C23 1.391(15) . ? C23 C24 1.390(14) . ? C24 C25 1.385(13) . ? C24 C30 1.530(14) . ? C26 C28 1.531(14) . ? C26 C29 1.538(14) . ? C26 C27 1.540(14) . ? C30 C32 1.526(16) . ? C30 C31 1.535(15) . ? C30 C33 1.540(16) . ? C34 C35 1.390(13) . ? C34 C39 1.394(13) . ? C35 C36 1.391(14) . ? C35 C40 1.550(13) . ? C36 C37 1.371(15) . ? C37 C38 1.392(14) . ? C38 C39 1.379(13) . ? C38 C44 1.537(15) . ? C40 C41' 1.51(3) . ? C40 C42 1.53(3) . ? C40 C42' 1.53(2) . ? C40 C41 1.53(2) . ? C40 C43' 1.55(3) . ? C40 C43 1.56(2) . ? C44 C45' 1.48(5) . ? C44 C46 1.49(2) . ? C44 C45 1.50(4) . ? C44 C47' 1.52(5) . ? C44 C46' 1.62(4) . ? C44 C47 1.66(3) . ? Sn2 Cl2 2.472(3) . ? Sn2 Cl3 2.497(3) . ? Sn2 Cl4 2.508(3) . ? O1 C50 1.464(19) . ? O1 C48 1.497(18) . ? C48 C49 1.481(19) . ? C50 C51 1.524(19) . ? 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 N2 Sn1 Cl1 82.98(18) . . ? N2 Sn1 N1 68.8(2) . . ? Cl1 Sn1 N1 92.41(18) . . ? N2 Sn1 N3 69.8(2) . . ? Cl1 Sn1 N3 81.84(18) . . ? N1 Sn1 N3 138.6(2) . . ? C1 N1 C20 117.8(8) . . ? C1 N1 Sn1 113.8(6) . . ? C20 N1 Sn1 118.8(5) . . ? C2 N2 C6 121.0(7) . . ? C2 N2 Sn1 120.2(5) . . ? C6 N2 Sn1 118.8(5) . . ? C13 N3 C34 120.9(8) . . ? C13 N3 Sn1 113.2(6) . . ? C34 N3 Sn1 119.3(6) . . ? N1 C1 C7 125.4(8) . . ? N1 C1 C2 116.2(8) . . ? C7 C1 C2 118.3(8) . . ? N2 C2 C3 121.4(8) . . ? N2 C2 C1 117.2(7) . . ? C3 C2 C1 121.5(8) . . ? C2 C3 C4 118.7(8) . . ? C5 C4 C3 119.5(9) . . ? C4 C5 C6 118.9(9) . . ? N2 C6 C5 120.5(8) . . ? N2 C6 C13 118.3(7) . . ? C5 C6 C13 121.3(8) . . ? C8 C7 C12 119.1(9) . . ? C8 C7 C1 121.4(9) . . ? C12 C7 C1 119.5(8) . . ? C9 C8 C7 121.1(10) . . ? C8 C9 C10 119.2(10) . . ? C11 C10 C9 121.1(10) . . ? C10 C11 C12 120.0(11) . . ? C11 C12 C7 119.5(10) . . ? N3 C13 C6 117.6(8) . . ? N3 C13 C14 125.9(8) . . ? C6 C13 C14 116.5(7) . . ? C19 C14 C15 119.2(9) . . ? C19 C14 C13 122.4(8) . . ? C15 C14 C13 118.5(8) . . ? C16 C15 C14 120.2(10) . . ? C17 C16 C15 119.6(11) . . ? C16 C17 C18 121.0(10) . . ? C17 C18 C19 119.1(11) . . ? C14 C19 C18 120.9(11) . . ? C21 C20 C25 121.4(8) . . ? C21 C20 N1 123.9(8) . . ? C25 C20 N1 114.5(8) . . ? C20 C21 C22 114.0(9) . . ? C20 C21 C26 125.9(8) . . ? C22 C21 C26 120.0(8) . . ? C23 C22 C21 124.5(10) . . ? C24 C23 C22 120.6(10) . . ? C25 C24 C23 115.7(9) . . ? C25 C24 C30 120.2(9) . . ? C23 C24 C30 124.0(9) . . ? C24 C25 C20 123.5(8) . . ? C21 C26 C28 107.6(8) . . ? C21 C26 C29 113.6(8) . . ? C28 C26 C29 109.5(9) . . ? C21 C26 C27 112.2(8) . . ? C28 C26 C27 105.8(9) . . ? C29 C26 C27 107.9(9) . . ? C24 C30 C32 108.5(10) . . ? C24 C30 C31 111.4(9) . . ? C32 C30 C31 108.5(10) . . ? C24 C30 C33 109.7(9) . . ? C32 C30 C33 109.2(10) . . ? C31 C30 C33 109.5(10) . . ? C35 C34 C39 121.6(8) . . ? C35 C34 N3 124.3(8) . . ? C39 C34 N3 113.8(8) . . ? C36 C35 C34 114.9(9) . . ? C36 C35 C40 118.3(8) . . ? C34 C35 C40 126.8(8) . . ? C37 C36 C35 123.5(9) . . ? C36 C37 C38 121.5(9) . . ? C39 C38 C37 115.7(9) . . ? C39 C38 C44 122.3(10) . . ? C37 C38 C44 122.0(10) . . ? C38 C39 C34 122.6(9) . . ? C41' C40 C42' 111.2(19) . . ? C42 C40 C41 111.9(17) . . ? C41' C40 C43' 108.2(18) . . ? C42' C40 C43' 107.1(17) . . ? C41' C40 C35 108.8(18) . . ? C42 C40 C35 110.2(17) . . ? C42' C40 C35 112.0(14) . . ? C41 C40 C35 109.0(13) . . ? C43' C40 C35 109.5(16) . . ? C42 C40 C43 108.0(17) . . ? C41 C40 C43 104.6(15) . . ? C35 C40 C43 113.1(13) . . ? C46 C44 C45 116(2) . . ? C45' C44 C47' 110(3) . . ? C45' C44 C38 114(3) . . ? C46 C44 C38 115.2(11) . . ? C45 C44 C38 110(2) . . ? C47' C44 C38 108.0(19) . . ? C45' C44 C46' 104(3) . . ? C47' C44 C46' 114(3) . . ? C38 C44 C46' 106.2(17) . . ? C46 C44 C47 103.9(17) . . ? C45 C44 C47 105.9(18) . . ? C38 C44 C47 104.8(13) . . ? Cl2 Sn2 Cl3 93.60(10) . . ? Cl2 Sn2 Cl4 91.74(9) . . ? Cl3 Sn2 Cl4 94.48(9) . . ? C50 O1 C48 112.4(19) . . ? C49 C48 O1 115(3) . . ? O1 C50 C51 116(2) . . ? 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 C20 N1 C1 C7 13.3(13) . . . . ? Sn1 N1 C1 C7 159.1(7) . . . . ? C20 N1 C1 C2 -168.0(7) . . . . ? Sn1 N1 C1 C2 -22.1(9) . . . . ? C6 N2 C2 C3 -1.2(12) . . . . ? Sn1 N2 C2 C3 177.7(6) . . . . ? C6 N2 C2 C1 178.1(7) . . . . ? Sn1 N2 C2 C1 -2.9(10) . . . . ? N1 C1 C2 N2 17.8(12) . . . . ? C7 C1 C2 N2 -163.4(8) . . . . ? N1 C1 C2 C3 -162.9(8) . . . . ? C7 C1 C2 C3 16.0(12) . . . . ? N2 C2 C3 C4 1.9(13) . . . . ? C1 C2 C3 C4 -177.4(8) . . . . ? C2 C3 C4 C5 -0.4(14) . . . . ? C3 C4 C5 C6 -1.8(14) . . . . ? C2 N2 C6 C5 -1.1(12) . . . . ? Sn1 N2 C6 C5 180.0(6) . . . . ? C2 N2 C6 C13 178.8(7) . . . . ? Sn1 N2 C6 C13 -0.2(10) . . . . ? C4 C5 C6 N2 2.6(13) . . . . ? C4 C5 C6 C13 -177.2(8) . . . . ? N1 C1 C7 C8 50.8(13) . . . . ? C2 C1 C7 C8 -128.0(10) . . . . ? N1 C1 C7 C12 -126.9(10) . . . . ? C2 C1 C7 C12 54.4(12) . . . . ? C12 C7 C8 C9 -0.7(16) . . . . ? C1 C7 C8 C9 -178.3(10) . . . . ? C7 C8 C9 C10 0.4(18) . . . . ? C8 C9 C10 C11 -0.1(19) . . . . ? C9 C10 C11 C12 0.0(19) . . . . ? C10 C11 C12 C7 -0.3(17) . . . . ? C8 C7 C12 C11 0.6(15) . . . . ? C1 C7 C12 C11 178.3(9) . . . . ? C34 N3 C13 C6 -168.7(7) . . . . ? Sn1 N3 C13 C6 -17.4(9) . . . . ? C34 N3 C13 C14 9.3(13) . . . . ? Sn1 N3 C13 C14 160.7(7) . . . . ? N2 C6 C13 N3 12.9(12) . . . . ? C5 C6 C13 N3 -167.3(8) . . . . ? N2 C6 C13 C14 -165.4(8) . . . . ? C5 C6 C13 C14 14.4(12) . . . . ? N3 C13 C14 C19 64.1(13) . . . . ? C6 C13 C14 C19 -117.8(10) . . . . ? N3 C13 C14 C15 -116.8(10) . . . . ? C6 C13 C14 C15 61.3(11) . . . . ? C19 C14 C15 C16 -0.7(15) . . . . ? C13 C14 C15 C16 -179.9(9) . . . . ? C14 C15 C16 C17 0.7(17) . . . . ? C15 C16 C17 C18 0.3(19) . . . . ? C16 C17 C18 C19 -1(2) . . . . ? C15 C14 C19 C18 -0.3(17) . . . . ? C13 C14 C19 C18 178.8(11) . . . . ? C17 C18 C19 C14 1(2) . . . . ? C1 N1 C20 C21 -125.8(9) . . . . ? Sn1 N1 C20 C21 90.0(9) . . . . ? C1 N1 C20 C25 58.9(11) . . . . ? Sn1 N1 C20 C25 -85.3(8) . . . . ? C25 C20 C21 C22 -3.4(13) . . . . ? N1 C20 C21 C22 -178.4(9) . . . . ? C25 C20 C21 C26 174.1(8) . . . . ? N1 C20 C21 C26 -0.9(14) . . . . ? C20 C21 C22 C23 1.2(16) . . . . ? C26 C21 C22 C23 -176.5(10) . . . . ? C21 C22 C23 C24 2.6(18) . . . . ? C22 C23 C24 C25 -4.0(16) . . . . ? C22 C23 C24 C30 177.3(10) . . . . ? C23 C24 C25 C20 1.7(14) . . . . ? C30 C24 C25 C20 -179.4(9) . . . . ? C21 C20 C25 C24 2.1(14) . . . . ? N1 C20 C25 C24 177.5(8) . . . . ? C20 C21 C26 C28 -80.6(11) . . . . ? C22 C21 C26 C28 96.8(11) . . . . ? C20 C21 C26 C29 40.8(13) . . . . ? C22 C21 C26 C29 -141.8(10) . . . . ? C20 C21 C26 C27 163.5(9) . . . . ? C22 C21 C26 C27 -19.1(13) . . . . ? C25 C24 C30 C32 65.0(13) . . . . ? C23 C24 C30 C32 -116.2(12) . . . . ? C25 C24 C30 C31 -175.6(10) . . . . ? C23 C24 C30 C31 3.1(16) . . . . ? C25 C24 C30 C33 -54.2(13) . . . . ? C23 C24 C30 C33 124.6(11) . . . . ? C13 N3 C34 C35 -127.6(10) . . . . ? Sn1 N3 C34 C35 82.8(10) . . . . ? C13 N3 C34 C39 57.9(11) . . . . ? Sn1 N3 C34 C39 -91.7(9) . . . . ? C39 C34 C35 C36 -3.1(14) . . . . ? N3 C34 C35 C36 -177.1(9) . . . . ? C39 C34 C35 C40 177.4(9) . . . . ? N3 C34 C35 C40 3.3(16) . . . . ? C34 C35 C36 C37 2.1(17) . . . . ? C40 C35 C36 C37 -178.3(11) . . . . ? C35 C36 C37 C38 -1(2) . . . . ? C36 C37 C38 C39 0.1(19) . . . . ? C36 C37 C38 C44 -179.2(13) . . . . ? C37 C38 C39 C34 -1.2(17) . . . . ? C44 C38 C39 C34 178.1(11) . . . . ? C35 C34 C39 C38 2.8(16) . . . . ? N3 C34 C39 C38 177.4(9) . . . . ? C36 C35 C40 C41' 85.9(17) . . . . ? C34 C35 C40 C41' -94.6(17) . . . . ? C36 C35 C40 C42 -129.1(14) . . . . ? C34 C35 C40 C42 50.4(17) . . . . ? C36 C35 C40 C42' -150.8(14) . . . . ? C34 C35 C40 C42' 28.7(18) . . . . ? C36 C35 C40 C41 107.8(14) . . . . ? C34 C35 C40 C41 -72.7(15) . . . . ? C36 C35 C40 C43' -32.2(17) . . . . ? C34 C35 C40 C43' 147.4(15) . . . . ? C36 C35 C40 C43 -8.1(17) . . . . ? C34 C35 C40 C43 171.4(14) . . . . ? C39 C38 C44 C45' 154(3) . . . . ? C37 C38 C44 C45' -27(3) . . . . ? C39 C38 C44 C46 -1(2) . . . . ? C37 C38 C44 C46 178.5(16) . . . . ? C39 C38 C44 C45 132.1(17) . . . . ? C37 C38 C44 C45 -49(2) . . . . ? C39 C38 C44 C47' -84(2) . . . . ? C37 C38 C44 C47' 96(2) . . . . ? C39 C38 C44 C46' 39(2) . . . . ? C37 C38 C44 C46' -141(2) . . . . ? C39 C38 C44 C47 -114.3(15) . . . . ? C37 C38 C44 C47 64.9(18) . . . . ? C50 O1 C48 C49 177(4) . . . . ? C48 O1 C50 C51 177(3) . . . . ? _refine_diff_density_max 1.876 _refine_diff_density_min -1.747 _refine_diff_density_rms 0.173 _shelxl_version_number 2013-3 _shelx_res_file ; TITL dr018 in P-1 CELL 0.71073 10.6251 14.0413 19.5349 74.108 77.877 75.277 ZERR 2.00 0.0005 0.0007 0.0010 0.002 0.003 0.002 LATT 1 SFAC C H N O Cl Sn UNIT 96.8 114.9 6 0.7 8 4 LIST 0 L.S. 80 ACTA CONF BOND FMAP 2 PLAN 5 SIZE 0.05 0.21 0.23 DFIX 1.48 0.02 O1 C48 O1 C50 DFIX 1.51 0.02 C48 C49 C50 C51 DFIX 2.50 0.04 C51 O1 C49 O1 C48 C50 TEMP -73.15C SIMU C40 C41 C42 C43 C41' C42' C43' C44 C45 C46 C47 C45' C46' C47' RIGU C40 C41 C42 C43 C41' C42' C43' C44 C45 C46 C47 C45' C46' C47' OMIT 0 -1 1 OMIT 0 2 0 OMIT 1 1 1 OMIT 1 1 2 OMIT 10 -3 7 OMIT 0 0 2 OMIT 1 1 3 OMIT 1 2 2 OMIT 5 14 15 OMIT 1 0 2 OMIT 5 14 14 OMIT 1 0 4 OMIT 0 -2 1 OMIT 0 -2 2 OMIT 1 2 3 OMIT 10 -2 6 OMIT 9 11 16 OMIT 5 15 14 OMIT 0 -1 2 OMIT 11 1 13 OMIT -1 -4 1 OMIT 6 14 15 OMIT 1 1 5 OMIT 5 13 15 OMIT 9 10 16 OMIT 0 0 4 OMIT 7 13 16 OMIT 1 2 1 OMIT 4 14 16 OMIT 7 14 15 OMIT -1 15 4 OMIT 7 12 16 OMIT 0 1 2 OMIT 1 0 3 OMIT -1 -3 1 OMIT 7 13 14 OMIT 0 2 2 OMIT 0 15 12 OMIT 1 0 6 OMIT 2 15 14 OMIT 4 14 15 OMIT 5 13 14 OMIT 3 15 13 OMIT 1 -1 1 OMIT 5 13 17 OMIT 1 1 0 OMIT 1 15 13 OMIT -1 15 10 OMIT 1 15 11 OMIT 2 -3 4 WGHT 0.058000 39.669701 FVAR 0.11214 SN1 6 0.316630 0.025762 0.194853 11.00000 0.03215 0.02908 = 0.02714 -0.01274 -0.00003 -0.00432 CL1 5 0.119862 0.073786 0.134974 11.00000 0.05140 0.04250 = 0.03803 -0.00610 -0.01865 -0.00805 N1 3 0.285200 0.197502 0.214683 11.00000 0.02797 0.02841 = 0.02374 -0.00380 -0.00178 -0.00378 N2 3 0.164681 0.047040 0.293892 11.00000 0.02300 0.02070 = 0.02494 -0.00710 -0.00387 -0.00309 N3 3 0.228817 -0.130300 0.250237 11.00000 0.02572 0.02598 = 0.03201 -0.01292 -0.00649 0.00256 C1 1 0.224846 0.206709 0.278106 11.00000 0.03108 0.02690 = 0.03021 -0.00289 -0.01033 0.00019 C2 1 0.142402 0.131361 0.317148 11.00000 0.02509 0.02429 = 0.01750 -0.01340 0.00161 -0.00308 C3 1 0.047650 0.147773 0.375518 11.00000 0.03530 0.03406 = 0.03115 -0.01944 -0.00453 -0.00794 AFIX 43 H3A 2 0.030711 0.209142 0.390747 11.00000 -1.20000 AFIX 0 C4 1 -0.022468 0.072545 0.411545 11.00000 0.03313 0.03796 = 0.03362 -0.01871 0.00175 -0.00384 AFIX 43 H4A 2 -0.087732 0.081867 0.451986 11.00000 -1.20000 AFIX 0 C5 1 0.003616 -0.015859 0.388010 11.00000 0.03139 0.03174 = 0.02854 -0.01157 0.00081 -0.00593 AFIX 43 H5A 2 -0.041533 -0.068731 0.412822 11.00000 -1.20000 AFIX 0 C6 1 0.097310 -0.026077 0.327241 11.00000 0.01984 0.02481 = 0.02801 -0.01179 -0.00498 0.00153 C7 1 0.229527 0.286594 0.313584 11.00000 0.02585 0.02803 = 0.03952 -0.01916 -0.00319 -0.00319 C8 1 0.204605 0.387733 0.278839 11.00000 0.06070 0.02859 = 0.03763 -0.01333 -0.00770 -0.00252 AFIX 43 H8A 2 0.181718 0.406980 0.231757 11.00000 -1.20000 AFIX 0 C9 1 0.212338 0.461096 0.311203 11.00000 0.08150 0.02640 = 0.05508 -0.00864 -0.01698 -0.00783 AFIX 43 H9A 2 0.194463 0.530540 0.286897 11.00000 -1.20000 AFIX 0 C10 1 0.246220 0.432797 0.379110 11.00000 0.06519 0.03813 = 0.07381 -0.03238 -0.01691 -0.01034 AFIX 43 H10A 2 0.251749 0.483271 0.401648 11.00000 -1.20000 AFIX 0 C11 1 0.272165 0.333013 0.414862 11.00000 0.05668 0.05744 = 0.04682 -0.02808 -0.01421 -0.00903 AFIX 43 H11A 2 0.295426 0.314749 0.461820 11.00000 -1.20000 AFIX 0 C12 1 0.264501 0.258834 0.382604 11.00000 0.04684 0.03538 = 0.04675 -0.01413 -0.01519 -0.00107 AFIX 43 H12A 2 0.282859 0.189515 0.407146 11.00000 -1.20000 AFIX 0 C13 1 0.125065 -0.117108 0.297635 11.00000 0.02792 0.02243 = 0.02675 -0.00525 -0.01100 0.00050 C14 1 0.027927 -0.183586 0.323961 11.00000 0.02883 0.02262 = 0.03474 -0.01780 0.00031 -0.00142 C15 1 -0.101560 -0.143219 0.310847 11.00000 0.02998 0.04181 = 0.04964 -0.01334 -0.00387 -0.00429 AFIX 43 H15A 2 -0.125497 -0.074721 0.285515 11.00000 -1.20000 AFIX 0 C16 1 -0.195519 -0.202952 0.334742 11.00000 0.03032 0.05529 = 0.07731 -0.03226 -0.00216 -0.00957 AFIX 43 H16A 2 -0.283320 -0.175698 0.325339 11.00000 -1.20000 AFIX 0 C17 1 -0.160791 -0.301075 0.371825 11.00000 0.04440 0.05125 = 0.09726 -0.02983 0.00756 -0.02719 AFIX 43 H17A 2 -0.224997 -0.341884 0.387893 11.00000 -1.20000 AFIX 0 C18 1 -0.033648 -0.341926 0.386340 11.00000 0.06351 0.03994 = 0.08922 0.00020 -0.00087 -0.01956 AFIX 43 H18A 2 -0.010840 -0.409795 0.413046 11.00000 -1.20000 AFIX 0 C19 1 0.060507 -0.282192 0.361264 11.00000 0.03397 0.02769 = 0.07303 -0.00981 -0.00033 0.00025 AFIX 43 H19A 2 0.148491 -0.310187 0.370142 11.00000 -1.20000 AFIX 0 C20 1 0.386370 0.255812 0.180813 11.00000 0.03032 0.02542 = 0.02870 -0.00667 -0.00125 -0.00660 C21 1 0.387783 0.321168 0.112310 11.00000 0.03648 0.02850 = 0.02903 -0.00787 -0.00081 -0.00399 C22 1 0.496649 0.367390 0.089821 11.00000 0.04991 0.04784 = 0.03838 0.00502 -0.00323 -0.01780 AFIX 43 H22A 2 0.501978 0.413570 0.044069 11.00000 -1.20000 AFIX 0 C23 1 0.597401 0.350321 0.129854 11.00000 0.04115 0.04265 = 0.05104 0.01541 -0.01063 -0.01616 AFIX 43 H23A 2 0.666263 0.386652 0.111918 11.00000 -1.20000 AFIX 0 C24 1 0.598226 0.280550 0.195898 11.00000 0.02886 0.03028 = 0.04164 -0.00378 -0.00150 -0.00359 C25 1 0.489799 0.235893 0.219933 11.00000 0.03005 0.02250 = 0.02559 -0.00303 0.00352 -0.00510 AFIX 43 H25A 2 0.485603 0.189200 0.265489 11.00000 -1.20000 AFIX 0 C26 1 0.286780 0.341011 0.062055 11.00000 0.03744 0.03143 = 0.03031 -0.00241 -0.00359 -0.00896 C27 1 0.293648 0.437582 0.001765 11.00000 0.06355 0.04897 = 0.04690 0.00399 -0.02016 -0.01572 AFIX 33 H27A 2 0.383984 0.433864 -0.023761 11.00000 -1.50000 H27B 2 0.267010 0.496878 0.022778 11.00000 -1.50000 H27C 2 0.234322 0.443471 -0.032096 11.00000 -1.50000 AFIX 0 C28 1 0.322170 0.253630 0.024096 11.00000 0.05974 0.04803 = 0.04786 -0.01717 -0.00536 -0.01714 AFIX 33 H28A 2 0.412824 0.248481 -0.001114 11.00000 -1.50000 H28B 2 0.262041 0.266291 -0.010704 11.00000 -1.50000 H28C 2 0.314300 0.190177 0.059804 11.00000 -1.50000 AFIX 0 C29 1 0.144083 0.349921 0.100978 11.00000 0.03949 0.05990 = 0.04171 -0.00953 -0.01510 -0.00123 AFIX 33 H29A 2 0.121271 0.406281 0.124881 11.00000 -1.50000 H29B 2 0.135454 0.286835 0.136961 11.00000 -1.50000 H29C 2 0.084571 0.362327 0.065899 11.00000 -1.50000 AFIX 0 C30 1 0.708052 0.253788 0.241853 11.00000 0.03585 0.04571 = 0.05231 0.00527 -0.01134 -0.01266 C31 1 0.812643 0.317786 0.207800 11.00000 0.04890 0.08670 = 0.07723 0.00017 -0.02181 -0.03041 AFIX 33 H31A 2 0.851236 0.306045 0.159884 11.00000 -1.50000 H31B 2 0.881789 0.298540 0.238218 11.00000 -1.50000 H31C 2 0.771698 0.389645 0.203549 11.00000 -1.50000 AFIX 0 C32 1 0.774086 0.142408 0.247655 11.00000 0.05634 0.04764 = 0.10172 -0.00321 -0.03305 0.00354 AFIX 33 H32A 2 0.708628 0.100411 0.269682 11.00000 -1.50000 H32B 2 0.843983 0.123859 0.277527 11.00000 -1.50000 H32C 2 0.812045 0.131439 0.199480 11.00000 -1.50000 AFIX 0 C33 1 0.649252 0.270590 0.317752 11.00000 0.06020 0.07551 = 0.04907 -0.00796 -0.01528 -0.01641 AFIX 33 H33A 2 0.584198 0.228293 0.339979 11.00000 -1.50000 H33B 2 0.606525 0.342002 0.314267 11.00000 -1.50000 H33C 2 0.719618 0.252166 0.347306 11.00000 -1.50000 AFIX 0 C34 1 0.250319 -0.206410 0.209305 11.00000 0.03453 0.02916 = 0.02925 -0.01103 -0.00642 -0.00211 C35 1 0.364872 -0.280197 0.203445 11.00000 0.02989 0.03021 = 0.03273 -0.00953 -0.00684 0.00087 C36 1 0.367229 -0.342787 0.158730 11.00000 0.04870 0.05069 = 0.04716 -0.02531 -0.01624 0.01409 AFIX 43 H36A 2 0.442047 -0.395974 0.154181 11.00000 -1.20000 AFIX 0 C37 1 0.267409 -0.331841 0.120887 11.00000 0.05551 0.04403 = 0.07215 -0.04868 -0.02336 0.01700 AFIX 43 H37A 2 0.275737 -0.376774 0.090858 11.00000 -1.20000 AFIX 0 C38 1 0.154099 -0.256373 0.125458 11.00000 0.05000 0.04816 = 0.04346 -0.01959 -0.01830 0.00290 C39 1 0.149593 -0.194140 0.170016 11.00000 0.03634 0.03463 = 0.03130 -0.02066 -0.00836 0.00182 AFIX 43 H39A 2 0.074843 -0.140760 0.174102 11.00000 -1.20000 AFIX 0 C40 1 0.486048 -0.298907 0.241517 11.00000 0.03477 0.04195 = 0.03817 -0.01387 -0.01230 0.00176 PART 1 10.5 SAME C41' > C43' C41 1 0.561455 -0.213644 0.206206 10.50000 0.03186 0.03413 = 0.04752 -0.01156 -0.01608 0.00922 AFIX 133 H41A 2 0.514657 -0.152415 0.222874 10.50000 -1.50000 H41B 2 0.567763 -0.199637 0.153759 10.50000 -1.50000 H41C 2 0.650108 -0.234421 0.219433 10.50000 -1.50000 AFIX 0 C42 1 0.442242 -0.306118 0.322239 10.50000 0.04950 0.04583 = 0.04046 -0.01274 -0.01389 0.01317 AFIX 133 H42A 2 0.374976 -0.245978 0.329515 10.50000 -1.50000 H42B 2 0.518099 -0.310148 0.344842 10.50000 -1.50000 H42C 2 0.405597 -0.366847 0.344055 10.50000 -1.50000 AFIX 0 C43 1 0.588334 -0.397848 0.231984 10.50000 0.03888 0.04244 = 0.05464 -0.01575 -0.01211 0.00363 AFIX 133 H43A 2 0.646441 -0.417620 0.268630 10.50000 -1.50000 H43B 2 0.640833 -0.385914 0.183978 10.50000 -1.50000 H43C 2 0.541966 -0.452146 0.237357 10.50000 -1.50000 AFIX 0 PART 2 10.5 SAME C41 > C43 C41' 1 0.586314 -0.242765 0.191328 10.50000 0.05395 0.07257 = 0.06241 -0.00965 -0.00047 -0.01242 AFIX 133 H41D 2 0.613179 -0.267639 0.147115 10.50000 -1.50000 H41E 2 0.663403 -0.254069 0.214899 10.50000 -1.50000 H41F 2 0.547399 -0.170171 0.179414 10.50000 -1.50000 AFIX 0 C42' 1 0.448068 -0.267336 0.313544 10.50000 0.02217 0.05572 = 0.04870 -0.02195 -0.01680 0.00353 AFIX 133 H42D 2 0.498980 -0.316820 0.349104 10.50000 -1.50000 H42E 2 0.353901 -0.264603 0.330481 10.50000 -1.50000 H42F 2 0.467050 -0.200409 0.307080 10.50000 -1.50000 AFIX 0 C43' 1 0.549639 -0.413475 0.258039 10.50000 0.06120 0.05269 = 0.06076 -0.01466 -0.01357 0.00786 AFIX 133 H43D 2 0.563662 -0.438674 0.214365 10.50000 -1.50000 H43E 2 0.491125 -0.450263 0.295853 10.50000 -1.50000 H43F 2 0.634329 -0.423912 0.274342 10.50000 -1.50000 AFIX 0 PART 0 C44 1 0.040724 -0.244251 0.084092 11.00000 0.05410 0.08738 = 0.08110 -0.04918 -0.03962 0.01077 PART 1 10.6 SAME C45 > C46 C45 1 0.093154 -0.245519 0.006841 10.60000 0.08513 0.09061 = 0.07851 -0.04628 -0.03536 0.00239 AFIX 133 H45A 2 0.024330 -0.253810 -0.016171 10.60000 -1.50000 H45B 2 0.168995 -0.301976 0.004273 10.60000 -1.50000 H45C 2 0.120431 -0.181600 -0.018110 10.60000 -1.50000 AFIX 0 C46 1 -0.074487 -0.161569 0.096373 10.60000 0.03966 0.08482 = 0.07976 -0.04380 -0.03997 0.00392 AFIX 133 H46A 2 -0.095944 -0.162911 0.147886 10.60000 -1.50000 H46B 2 -0.150193 -0.171145 0.079691 10.60000 -1.50000 H46C 2 -0.053261 -0.096154 0.069638 10.60000 -1.50000 AFIX 0 C47 1 -0.017772 -0.349135 0.119387 10.60000 0.07642 0.08927 = 0.10485 -0.04491 -0.04004 -0.00500 AFIX 133 H47A 2 -0.025170 -0.364738 0.171956 10.60000 -1.50000 H47B 2 0.042144 -0.405438 0.101148 10.60000 -1.50000 H47C 2 -0.104797 -0.339102 0.105878 10.60000 -1.50000 AFIX 0 PART 2 10.4 SAME C45' > C46' C45' 1 0.081123 -0.281783 0.017243 10.40000 0.06191 0.09404 = 0.08497 -0.05027 -0.03580 -0.00511 AFIX 133 H45D 2 0.152294 -0.250216 -0.013307 10.40000 -1.50000 H45E 2 0.005791 -0.264491 -0.008689 10.40000 -1.50000 H45F 2 0.112013 -0.355474 0.029493 10.40000 -1.50000 AFIX 0 C46' 1 -0.012160 -0.123870 0.056394 10.40000 0.08294 0.09374 = 0.10870 -0.04855 -0.05325 0.01351 AFIX 133 H46D 2 0.057224 -0.094503 0.021956 10.40000 -1.50000 H46E 2 -0.036270 -0.092194 0.097526 10.40000 -1.50000 H46F 2 -0.089517 -0.111885 0.032899 10.40000 -1.50000 AFIX 0 C47' 1 -0.061647 -0.299783 0.134621 10.40000 0.06067 0.11725 = 0.10255 -0.04449 -0.03352 -0.00228 AFIX 133 H47D 2 -0.109340 -0.322620 0.106396 10.40000 -1.50000 H47E 2 -0.123806 -0.253945 0.161992 10.40000 -1.50000 H47F 2 -0.017603 -0.358481 0.167957 10.40000 -1.50000 AFIX 0 PART 0 SN2 6 0.453047 0.874322 0.465683 11.00000 0.03466 0.03837 = 0.03298 -0.00471 -0.00759 -0.00306 CL2 5 0.316427 1.012106 0.521658 11.00000 0.04350 0.05646 = 0.05560 -0.02719 0.00761 -0.01822 CL3 5 0.458500 0.983764 0.340967 11.00000 0.04529 0.05332 = 0.03606 0.00217 -0.00631 -0.00889 CL4 5 0.253962 0.811961 0.461807 11.00000 0.04283 0.05296 = 0.04308 -0.02404 -0.00358 -0.01012 PART -1 10.35 EADP O1 C48 C49 C50 C51 O1 4 0.493954 -0.003696 0.026408 10.35000 0.07997 C48 1 0.454065 -0.012578 -0.040275 10.35000 0.07997 AFIX 23 H48A 2 0.434332 0.056004 -0.071974 10.35000 -1.20000 H48B 2 0.529848 -0.052989 -0.066170 10.35000 -1.20000 AFIX 0 C49 1 0.338817 -0.059453 -0.028395 10.35000 0.07997 AFIX 33 H49A 2 0.352362 -0.123984 0.007438 10.35000 -1.50000 H49B 2 0.328382 -0.071459 -0.073807 10.35000 -1.50000 H49C 2 0.259443 -0.013935 -0.010956 10.35000 -1.50000 AFIX 0 C50 1 0.612549 0.038089 0.010926 10.35000 0.07997 AFIX 23 H50A 2 0.596989 0.103968 -0.024414 10.35000 -1.20000 H50B 2 0.685481 -0.007900 -0.012208 10.35000 -1.20000 AFIX 0 C51 1 0.656895 0.054161 0.075502 10.35000 0.07997 PART HKLF 4 REM dr018 in P-1 REM R1 = 0.0783 for 6520 Fo > 4sig(Fo) and 0.1094 for all 8822 data REM 575 parameters refined using 196 restraints END WGHT 0.0488 35.4353 REM Highest difference peak 1.876, deepest hole -1.747, 1-sigma level 0.173 Q1 1 0.4474 -0.4743 0.5167 11.00000 0.05 1.88 Q2 1 0.2781 -0.0228 0.1864 11.00000 0.05 1.78 Q3 1 0.3440 0.0851 0.2032 11.00000 0.05 1.68 Q4 1 0.3536 -0.0387 0.1983 11.00000 0.05 1.57 Q5 1 -0.3440 -0.5082 0.4739 11.00000 0.05 1.56 ; _shelx_res_checksum 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0 17.35 2.53 -5 -2 0 15.29 1.33 -5 -2 0 19.07 1.59 -5 -2 0 15.61 2.00 -5 -2 0 12.47 1.25 5 2 0 15.66 0.90 -6 -2 0 27.61 2.39 -6 -2 0 27.43 1.81 -6 -2 0 28.60 2.49 -6 -2 0 27.66 2.86 -6 -2 0 29.52 2.04 6 2 0 28.11 1.34 -7 -2 0 23.60 3.39 -7 -2 0 21.58 2.69 -7 -2 0 22.52 1.87 -7 -2 0 25.06 2.07 -7 -2 0 26.16 2.67 7 2 0 17.36 2.53 -8 -2 0 84.95 4.79 -8 -2 0 83.99 4.10 -8 -2 0 85.17 4.33 -8 -2 0 80.27 4.64 -8 -2 0 87.69 5.26 8 2 0 69.53 4.75 -9 -2 0 118.67 6.15 -9 -2 0 120.19 5.68 -9 -2 0 123.87 6.02 -9 -2 0 125.14 6.43 9 2 0 119.49 6.39 -10 -2 0 0.24 0.77 -10 -2 0 1.64 2.44 -10 -2 0 1.31 0.84 -11 -2 0 7.58 1.82 -11 -2 0 4.50 0.90 -12 -2 0 6.25 2.68 -11 3 0 7.52 1.89 -10 3 0 23.70 2.47 -10 3 0 27.37 2.30 -9 3 0 0.62 0.92 -9 3 0 3.02 0.97 8 -3 0 -0.60 1.17 -8 3 0 0.06 0.94 -8 3 0 0.14 0.96 7 -3 0 -0.69 1.14 7 -3 0 0.27 0.43 -7 3 0 0.78 0.83 -7 3 0 0.44 0.99 -7 3 0 0.22 0.90 -7 3 0 1.13 0.64 6 -3 0 79.98 3.63 6 -3 0 83.85 4.54 -6 3 0 79.33 3.95 -6 3 0 80.18 4.09 -6 3 0 78.19 4.04 -6 3 0 83.78 4.37 5 -3 0 153.63 6.62 5 -3 0 159.95 7.46 -5 3 0 157.62 7.39 -5 3 0 152.90 6.93 -5 3 0 152.68 6.81 -5 3 0 155.49 7.27 4 -3 0 12.14 1.07 4 -3 0 11.21 1.68 -4 3 0 12.80 1.52 -4 3 0 11.86 1.30 -4 3 0 10.88 1.13 -4 3 0 12.01 1.67 -4 3 0 12.02 1.36 3 -3 0 89.14 4.44 3 -3 0 86.43 4.11 3 -3 0 94.41 4.00 -3 3 0 90.11 4.18 -3 3 0 93.49 4.44 -3 3 0 91.16 4.08 -3 3 0 97.22 4.39 -3 3 0 93.77 4.08 2 -3 0 7.69 0.95 2 -3 0 7.34 0.97 2 -3 0 7.32 0.71 -2 3 0 6.62 1.06 -2 3 0 5.33 0.83 -2 3 0 5.22 1.10 -2 3 0 7.35 0.91 1 -3 0 -0.41 0.46 1 -3 0 0.73 0.41 1 -3 0 1.11 0.32 -1 3 0 0.37 0.43 -1 3 0 0.09 0.43 -1 3 0 0.99 0.52 -1 3 0 1.01 0.37 0 -3 0 138.61 5.72 0 -3 0 133.58 6.25 0 -3 0 131.72 5.83 0 3 0 136.47 5.71 0 3 0 135.77 5.90 0 3 0 117.67 6.24 0 3 0 138.26 5.86 0 3 0 141.49 6.27 -1 -3 0 145.57 6.51 -1 -3 0 136.83 6.08 -1 -3 0 124.82 6.48 -1 -3 0 129.28 6.12 -1 -3 0 142.14 5.93 1 3 0 153.31 6.53 1 3 0 129.16 6.49 1 3 0 144.42 6.10 1 3 0 144.40 5.94 1 3 0 150.30 6.14 -2 -3 0 100.66 4.77 -2 -3 0 102.89 4.66 -2 -3 0 104.47 5.02 -2 -3 0 106.46 4.52 2 3 0 111.97 5.01 2 3 0 105.54 4.78 2 3 0 104.40 4.51 -3 -3 0 242.33 12.11 -3 -3 0 260.64 11.33 -3 -3 0 259.82 10.99 -3 -3 0 256.19 10.94 -3 -3 0 266.28 12.07 3 3 0 290.51 12.07 3 3 0 263.25 12.07 3 3 0 268.11 11.06 3 3 0 264.74 11.41 -4 -3 0 282.21 12.19 -4 -3 0 306.22 13.50 -4 -3 0 305.82 13.41 -4 -3 0 284.21 12.66 -4 -3 0 312.57 12.19 4 3 0 283.36 12.64 4 3 0 300.98 12.19 4 3 0 259.33 13.42 4 3 0 299.95 13.41 -5 -3 0 6.01 1.35 -5 -3 0 3.17 0.79 -5 -3 0 7.20 1.83 -5 -3 0 4.63 1.13 -5 -3 0 2.75 1.52 5 3 0 5.05 0.72 -6 -3 0 81.21 4.26 -6 -3 0 83.40 4.19 -6 -3 0 82.87 3.92 -6 -3 0 84.28 3.79 -6 -3 0 83.77 4.50 -6 -3 0 83.67 4.54 6 3 0 83.20 3.59 -7 -3 0 0.79 1.11 -7 -3 0 2.00 0.66 -7 -3 0 1.52 0.72 -7 -3 0 1.61 2.11 -7 -3 0 2.64 1.14 7 3 0 1.16 0.32 7 3 0 2.51 1.02 -8 -3 0 45.57 2.76 -8 -3 0 42.88 4.07 -8 -3 0 45.35 3.48 -8 -3 0 45.02 2.86 -8 -3 0 43.87 3.67 8 3 0 40.39 3.46 -9 -3 0 2.29 0.87 -9 -3 0 2.58 2.55 -9 -3 0 1.46 0.84 -10 -3 0 8.06 1.80 -10 -3 0 8.76 1.69 -10 -3 0 10.79 2.57 -11 -3 0 11.27 2.77 -11 -3 0 9.07 1.83 -11 -3 0 7.58 1.85 -12 -3 0 10.39 2.80 -12 -3 0 5.49 0.96 -12 -3 0 5.06 1.14 -10 4 0 32.45 2.45 -10 4 0 26.07 2.62 -9 4 0 1.37 0.95 -8 4 0 -0.06 0.95 -8 4 0 0.44 0.91 7 -4 0 -0.29 0.49 7 -4 0 0.30 1.18 -7 4 0 0.01 1.06 -7 4 0 -0.49 0.97 -7 4 0 0.70 0.84 6 -4 0 7.00 1.31 6 -4 0 4.16 1.11 -6 4 0 4.20 1.03 -6 4 0 4.29 0.94 -6 4 0 5.67 0.76 5 -4 0 64.69 3.04 5 -4 0 62.54 3.66 -5 4 0 66.57 3.28 -5 4 0 60.87 3.38 -5 4 0 63.62 3.61 -5 4 0 66.73 3.36 -5 4 0 68.52 3.22 4 -4 0 7.49 1.67 4 -4 0 10.36 1.23 -4 4 0 8.15 1.63 -4 4 0 10.73 1.35 -4 4 0 8.45 1.56 -4 4 0 11.36 1.35 -4 4 0 10.10 1.22 3 -4 0 64.82 3.16 3 -4 0 67.37 3.10 3 -4 0 63.04 3.43 -3 4 0 67.71 3.12 -3 4 0 64.11 3.22 -3 4 0 72.64 3.39 -3 4 0 64.87 3.12 -3 4 0 72.58 3.45 2 -4 0 56.79 3.11 2 -4 0 57.22 2.76 2 -4 0 57.72 3.05 2 -4 0 61.65 2.79 2 -4 0 58.19 2.69 -2 4 0 66.05 2.99 -2 4 0 64.55 3.03 -2 4 0 55.85 2.76 -2 4 0 57.20 2.72 -2 4 0 56.95 2.81 1 -4 0 2.85 0.78 1 -4 0 1.42 0.39 1 -4 0 1.01 0.45 -1 4 0 2.28 0.50 -1 4 0 3.14 0.89 -1 4 0 1.51 0.43 -1 4 0 1.43 0.42 0 -4 0 39.12 1.99 0 -4 0 38.52 2.26 0 -4 0 40.25 2.05 0 4 0 41.47 2.26 0 4 0 37.75 2.08 0 4 0 38.96 1.99 0 4 0 40.77 1.96 -1 -4 0 89.51 4.18 -1 -4 0 96.25 4.63 -1 -4 0 92.84 4.27 1 4 0 98.80 4.33 1 4 0 96.07 4.28 1 4 0 95.09 4.17 1 4 0 99.77 4.60 -2 -4 0 191.81 8.83 -2 -4 0 182.18 8.28 -2 -4 0 185.95 8.04 -2 -4 0 168.49 8.30 -2 -4 0 193.49 8.86 2 4 0 183.34 8.30 2 4 0 207.02 8.84 2 4 0 214.03 8.88 2 4 0 193.10 8.05 -3 -4 0 376.34 15.81 -3 -4 0 342.42 16.82 -3 -4 0 377.68 16.82 -3 -4 0 346.01 15.84 -3 -4 0 392.85 15.36 3 4 0 366.39 15.83 3 4 0 390.53 16.82 3 4 0 343.62 16.80 3 4 0 383.86 15.51 -4 -4 0 58.04 2.88 -4 -4 0 54.77 2.60 -4 -4 0 55.10 2.52 -4 -4 0 45.87 3.18 -4 -4 0 55.99 3.13 4 4 0 53.49 3.00 4 4 0 55.91 2.45 4 4 0 48.13 2.86 -5 -4 0 4.05 1.14 -5 -4 0 2.71 1.57 -5 -4 0 6.64 1.81 -5 -4 0 4.51 1.39 5 4 0 4.73 0.84 -6 -4 0 120.75 5.95 -6 -4 0 127.45 6.28 -6 -4 0 123.58 5.71 -6 -4 0 125.87 6.07 -6 -4 0 120.92 5.49 -6 -4 0 123.16 6.08 6 4 0 144.00 6.27 6 4 0 121.65 5.37 -7 -4 0 3.47 2.19 -7 -4 0 2.69 0.79 -7 -4 0 3.27 0.75 -7 -4 0 2.48 0.65 -7 -4 0 3.51 1.15 -7 -4 0 2.12 1.14 7 4 0 3.85 0.94 -8 -4 0 22.80 3.74 -8 -4 0 22.06 1.97 -8 -4 0 22.48 2.15 -8 -4 0 17.78 3.36 -8 -4 0 22.42 2.19 -8 -4 0 20.99 3.05 8 4 0 20.13 1.29 8 4 0 16.92 3.01 -9 -4 0 0.50 2.48 -9 -4 0 0.96 0.83 -9 -4 0 0.44 0.81 -10 -4 0 0.54 0.82 -10 -4 0 0.26 0.79 -10 -4 0 2.62 2.46 -11 -4 0 3.55 0.93 -11 -4 0 6.58 2.70 -11 -4 0 4.23 0.98 -12 -4 0 17.06 2.13 -12 -4 0 21.06 2.20 -12 -4 0 26.34 4.05 -9 5 0 0.85 1.02 -8 5 0 23.59 2.45 -8 5 0 23.54 2.25 7 -5 0 13.43 2.71 7 -5 0 9.14 1.55 -7 5 0 10.37 2.14 -7 5 0 10.83 2.41 6 -5 0 2.30 1.07 6 -5 0 1.63 0.56 -6 5 0 1.59 1.02 -6 5 0 2.14 0.69 -6 5 0 2.32 0.64 -6 5 0 0.83 0.95 5 -5 0 7.71 1.40 -5 5 0 8.33 1.56 -5 5 0 8.93 1.64 -5 5 0 9.11 1.58 -5 5 0 7.85 1.89 4 -5 0 1.20 0.47 4 -5 0 1.33 0.70 -4 5 0 0.13 0.69 -4 5 0 2.24 0.82 -4 5 0 1.71 0.45 -4 5 0 1.65 0.54 -4 5 0 1.28 0.70 3 -5 0 19.43 1.81 3 -5 0 21.06 1.54 3 -5 0 21.44 1.61 -3 5 0 20.21 1.51 -3 5 0 21.88 1.45 -3 5 0 21.04 1.74 -3 5 0 23.05 1.73 2 -5 0 264.74 11.80 2 -5 0 279.56 11.57 2 -5 0 270.79 12.63 -2 5 0 301.29 12.65 -2 5 0 270.35 11.83 -2 5 0 260.58 12.60 -2 5 0 266.22 11.87 -2 5 0 284.31 11.65 1 -5 0 74.01 3.40 1 -5 0 67.34 3.70 1 -5 0 75.10 3.41 -1 5 0 68.47 3.49 -1 5 0 81.14 3.77 -1 5 0 74.14 3.37 -1 5 0 74.57 3.39 -1 5 0 84.65 3.80 -1 5 0 75.46 3.44 0 -5 0 13.28 1.17 0 -5 0 11.99 1.37 0 -5 0 13.25 1.07 0 -5 0 10.40 1.53 0 5 0 13.86 1.38 0 5 0 13.16 1.08 0 5 0 12.11 1.23 0 5 0 13.01 1.09 0 5 0 9.66 1.49 -1 -5 0 141.78 5.91 -1 -5 0 142.08 6.51 -1 -5 0 117.03 6.49 -1 -5 0 141.22 6.05 1 5 0 142.85 5.89 1 5 0 131.00 6.50 1 5 0 143.53 6.49 1 5 0 140.25 6.09 -2 -5 0 0.13 0.37 -2 -5 0 0.19 0.34 -2 -5 0 0.17 0.46 -2 -5 0 -0.28 0.71 2 5 0 0.23 0.51 2 5 0 0.17 0.33 2 5 0 -0.39 0.63 2 5 0 0.10 0.44 -3 -5 0 152.95 7.10 -3 -5 0 156.78 7.64 -3 -5 0 170.37 6.85 -3 -5 0 156.32 7.05 -3 -5 0 164.80 7.53 3 5 0 152.18 7.07 3 5 0 166.45 6.84 3 5 0 163.90 7.60 -4 -5 0 60.63 3.26 -4 -5 0 62.68 2.92 -4 -5 0 62.01 3.25 -4 -5 0 61.92 3.03 4 5 0 63.40 2.87 4 5 0 62.06 3.30 -5 -5 0 34.17 2.90 -5 -5 0 32.17 1.91 -5 -5 0 34.46 2.20 5 5 0 33.55 1.77 5 5 0 33.79 2.67 5 5 0 27.88 2.42 -6 -5 0 101.49 4.70 -6 -5 0 103.85 5.30 -6 -5 0 107.98 5.22 -6 -5 0 115.60 5.68 6 5 0 105.17 4.58 6 5 0 94.61 5.33 -7 -5 0 13.42 2.04 -7 -5 0 16.34 2.00 -7 -5 0 14.38 2.72 -7 -5 0 13.72 1.96 -7 -5 0 15.30 3.50 -7 -5 0 16.76 2.68 7 5 0 14.29 1.29 7 5 0 16.90 2.64 -8 -5 0 0.42 0.83 -8 -5 0 0.24 0.75 -8 -5 0 0.59 0.84 -8 -5 0 -0.13 2.47 8 5 0 0.39 0.43 -9 -5 0 1.92 0.87 -9 -5 0 2.42 0.88 -9 -5 0 2.09 2.48 -10 -5 0 -0.63 0.79 -10 -5 0 -0.99 2.44 -10 -5 0 -0.81 0.79 -11 -5 0 4.13 1.01 -11 -5 0 6.71 2.73 -11 -5 0 4.03 0.94 -12 -5 0 14.28 2.07 -12 -5 0 16.06 3.77 -12 -5 0 11.24 2.23 -10 6 0 2.72 1.12 -9 6 0 -0.98 1.03 -9 6 0 1.21 1.05 -8 6 0 29.90 2.48 -8 6 0 31.14 2.75 7 -6 0 65.99 4.06 -7 6 0 67.30 3.93 -7 6 0 62.27 3.67 6 -6 0 18.45 2.79 -6 6 0 15.88 2.66 -6 6 0 20.58 2.09 -6 6 0 15.20 2.46 5 -6 0 1.76 0.99 -5 6 0 2.48 0.68 -5 6 0 0.86 1.00 -5 6 0 1.59 0.92 -5 6 0 3.96 1.09 -5 6 0 2.76 0.67 4 -6 0 1.75 0.82 4 -6 0 1.71 0.55 -4 6 0 2.09 0.54 -4 6 0 1.41 0.80 -4 6 0 2.97 0.89 -4 6 0 1.57 0.84 -4 6 0 2.18 0.64 3 -6 0 60.36 2.96 3 -6 0 56.07 3.27 -3 6 0 53.92 3.24 -3 6 0 60.11 2.90 -3 6 0 64.36 3.28 -3 6 0 61.90 3.00 -3 6 0 58.88 3.08 2 -6 0 101.66 4.69 2 -6 0 99.93 5.16 2 -6 0 104.75 4.72 -2 6 0 103.62 4.84 -2 6 0 102.14 4.65 -2 6 0 118.29 5.20 1 -6 0 28.02 1.62 1 -6 0 27.55 1.79 1 -6 0 25.59 1.98 -1 6 0 28.30 1.95 -1 6 0 28.69 1.72 -1 6 0 28.38 1.72 -1 6 0 30.87 2.01 -1 6 0 25.39 1.66 0 -6 0 70.20 3.40 0 -6 0 73.12 3.73 0 -6 0 73.83 3.42 0 6 0 80.60 3.78 0 6 0 71.71 3.45 0 6 0 73.45 3.37 0 6 0 73.32 3.54 -1 -6 0 155.65 7.58 -1 -6 0 164.91 7.07 -1 -6 0 158.82 6.91 1 6 0 164.88 6.90 1 6 0 161.38 7.12 1 6 0 156.48 7.65 1 6 0 164.17 7.58 -2 -6 0 24.76 1.81 -2 -6 0 23.65 1.58 -2 -6 0 24.97 1.61 2 6 0 24.95 1.78 2 6 0 28.10 2.17 2 6 0 26.53 1.56 -3 -6 0 0.83 0.55 -3 -6 0 0.70 0.42 -3 -6 0 1.55 0.49 3 6 0 1.50 0.68 3 6 0 1.31 0.40 -4 -6 0 26.02 1.92 -4 -6 0 25.93 1.71 -4 -6 0 24.62 1.71 -4 -6 0 21.06 1.98 4 6 0 26.55 1.56 4 6 0 25.61 2.06 -5 -6 0 11.90 2.66 -5 -6 0 13.23 1.66 -5 -6 0 11.92 2.02 -5 -6 0 11.31 1.51 5 6 0 12.26 2.14 5 6 0 13.43 1.19 -6 -6 0 104.38 5.29 -6 -6 0 96.99 4.99 -6 -6 0 99.33 4.55 6 6 0 101.24 4.40 6 6 0 91.94 5.14 -7 -6 0 68.56 3.90 -7 -6 0 72.54 3.80 -7 -6 0 72.35 4.62 -7 -6 0 68.51 3.61 7 6 0 67.90 4.21 7 6 0 73.82 3.31 -8 -6 0 0.59 2.46 -8 -6 0 -0.12 0.86 -8 -6 0 -0.22 0.90 -8 -6 0 -1.04 0.79 8 6 0 0.63 1.23 8 6 0 0.07 0.48 -9 -6 0 14.74 2.05 -9 -6 0 16.49 3.43 -9 -6 0 17.00 2.19 9 6 0 20.42 2.89 -10 -6 0 2.25 0.93 -10 -6 0 2.94 2.53 -10 -6 0 1.56 0.85 -11 -6 0 1.65 2.66 -11 -6 0 1.28 0.89 -11 -6 0 1.15 0.94 -12 -6 0 1.75 0.94 -12 -6 0 1.10 1.03 -12 -6 0 2.04 2.83 -9 7 0 1.15 1.08 -9 7 0 -1.18 1.07 -8 7 0 27.33 2.58 -8 7 0 29.00 2.76 -7 7 0 41.76 3.00 -7 7 0 45.49 3.20 6 -7 0 14.59 2.62 -6 7 0 10.85 1.89 -6 7 0 11.30 2.24 -6 7 0 13.52 2.43 5 -7 0 8.85 2.49 -5 7 0 5.85 1.12 -5 7 0 10.07 1.76 -5 7 0 6.05 1.20 4 -7 0 20.10 2.52 -4 7 0 26.24 2.08 -4 7 0 23.59 2.54 -4 7 0 25.05 2.28 -4 7 0 23.87 1.95 -4 7 0 21.38 2.24 3 -7 0 -0.17 0.76 -3 7 0 0.01 0.83 -3 7 0 -0.50 0.77 -3 7 0 0.27 0.65 -3 7 0 0.00 0.78 2 -7 0 1.60 0.46 2 -7 0 1.19 0.70 -2 7 0 2.09 0.77 -2 7 0 1.93 0.62 -2 7 0 1.70 0.72 -2 7 0 2.25 0.76 1 -7 0 0.18 0.43 1 -7 0 0.12 0.60 -1 7 0 -0.07 0.64 -1 7 0 0.61 0.41 -1 7 0 0.42 0.56 -1 7 0 0.35 0.68 0 -7 0 99.18 4.99 0 -7 0 101.68 4.60 0 7 0 102.59 4.53 0 7 0 99.14 4.69 0 7 0 101.86 4.62 -1 -7 0 242.03 10.13 -1 -7 0 240.49 10.37 -1 -7 0 233.59 11.09 1 7 0 253.41 11.21 1 7 0 239.82 10.09 1 7 0 219.14 10.40 -2 -7 0 68.05 3.28 -2 -7 0 65.38 3.62 2 7 0 66.75 3.37 2 7 0 67.84 3.16 -3 -7 0 0.06 0.50 -3 -7 0 0.42 0.59 -3 -7 0 -0.03 0.45 3 7 0 0.12 0.69 3 7 0 -0.18 0.40 -4 -7 0 12.75 1.65 -4 -7 0 9.23 1.50 -4 -7 0 11.56 1.44 4 7 0 11.11 1.23 4 7 0 11.14 1.86 -5 -7 0 1.20 0.83 -5 -7 0 1.53 0.70 -5 -7 0 0.55 0.54 5 7 0 0.84 0.95 5 7 0 1.71 0.49 5 7 0 1.45 0.94 -6 -7 0 50.56 3.13 -6 -7 0 47.64 3.37 -6 -7 0 47.52 2.86 -6 -7 0 51.41 3.95 6 7 0 53.60 3.58 6 7 0 53.58 2.59 6 7 0 45.23 3.40 -7 -7 0 50.96 3.21 -7 -7 0 56.23 3.42 -7 -7 0 58.90 4.45 -7 -7 0 54.53 3.46 7 7 0 61.05 2.88 7 7 0 63.46 3.93 -8 -7 0 22.56 3.84 -8 -7 0 21.45 2.45 -8 -7 0 19.24 2.34 8 7 0 22.59 1.67 -9 -7 0 51.04 3.29 -9 -7 0 54.56 4.21 -9 -7 0 56.06 3.27 9 7 0 49.26 3.82 -10 -7 0 15.03 2.32 -10 -7 0 17.33 2.18 -10 -7 0 17.28 3.68 -11 -7 0 -1.38 0.93 -11 -7 0 -1.31 0.87 -11 -7 0 -1.59 2.62 -9 8 0 2.30 1.20 -9 8 0 -1.37 1.12 -8 8 0 11.31 2.33 -8 8 0 12.05 2.45 -7 8 0 20.07 2.63 -7 8 0 15.64 2.40 -6 8 0 0.23 1.13 -6 8 0 2.02 1.07 -6 8 0 0.72 0.99 5 -8 0 31.40 3.01 -5 8 0 27.33 2.17 -5 8 0 29.36 2.85 -5 8 0 26.51 2.62 4 -8 0 36.03 3.12 -4 8 0 37.65 2.40 -4 8 0 36.67 2.83 -4 8 0 33.79 3.05 3 -8 0 15.42 2.50 -3 8 0 23.01 2.46 -3 8 0 18.71 1.79 -3 8 0 17.61 2.29 2 -8 0 3.29 0.88 -2 8 0 3.58 0.91 -2 8 0 5.44 1.39 -2 8 0 1.84 0.90 1 -8 0 15.80 1.90 1 -8 0 15.53 1.49 -1 8 0 16.51 1.85 -1 8 0 13.19 2.10 -1 8 0 15.90 1.47 -1 8 0 19.68 1.66 0 -8 0 48.38 2.92 0 -8 0 47.98 2.58 0 8 0 48.09 2.77 0 8 0 52.16 3.26 0 8 0 49.50 2.57 -1 -8 0 182.04 8.01 -1 -8 0 176.77 8.58 1 8 0 180.69 7.79 1 8 0 194.53 8.71 1 8 0 169.66 8.05 -2 -8 0 126.00 5.64 -2 -8 0 119.80 6.10 2 8 0 116.78 5.69 2 8 0 125.47 5.47 2 8 0 130.12 6.31 -3 -8 0 8.23 1.75 -3 -8 0 9.12 1.51 3 8 0 9.11 1.82 3 8 0 8.18 1.21 -4 -8 0 29.96 2.38 -4 -8 0 29.93 2.10 4 8 0 30.08 1.88 4 8 0 32.23 2.48 4 8 0 31.97 2.70 -5 -8 0 1.13 0.80 5 8 0 0.87 1.00 5 8 0 0.94 0.53 5 8 0 0.67 1.09 -6 -8 0 12.78 2.41 -6 -8 0 13.19 2.06 6 8 0 13.92 1.48 6 8 0 13.03 2.66 -7 -8 0 5.58 1.15 -7 -8 0 5.68 2.46 -7 -8 0 4.05 1.01 7 8 0 2.85 1.37 7 8 0 6.82 1.41 -8 -8 0 38.82 3.96 -8 -8 0 34.95 2.85 -8 -8 0 32.01 2.72 8 8 0 31.68 3.42 8 8 0 34.37 2.09 -9 -8 0 64.99 3.81 -9 -8 0 61.48 3.81 -9 -8 0 67.18 4.61 9 8 0 65.67 4.43 -10 -8 0 15.62 2.20 -10 -8 0 16.56 3.70 -10 -8 0 15.25 2.40 -11 -8 0 0.12 1.06 -11 -8 0 0.22 0.95 -11 -8 0 0.84 2.64 -8 9 0 1.05 1.19 -8 9 0 1.90 1.18 -7 9 0 17.98 2.74 -7 9 0 11.04 2.49 -6 9 0 1.14 1.17 -6 9 0 2.43 1.12 5 -9 0 41.75 3.15 -5 9 0 31.73 2.36 -5 9 0 39.04 3.03 -5 9 0 32.74 2.79 4 -9 0 109.16 5.96 -4 9 0 107.66 5.16 -4 9 0 118.76 5.60 -4 9 0 111.20 5.87 3 -9 0 29.93 2.99 -3 9 0 34.69 2.29 -3 9 0 34.92 2.91 -3 9 0 34.11 2.92 2 -9 0 -0.37 0.96 -2 9 0 -0.06 0.98 -2 9 0 0.27 0.97 -2 9 0 0.82 1.01 1 -9 0 0.31 0.87 1 -9 0 0.74 0.69 -1 9 0 1.19 0.95 -1 9 0 1.43 1.04 -1 9 0 1.47 0.90 0 -9 0 29.70 2.56 0 -9 0 29.46 2.06 0 9 0 25.52 2.68 0 9 0 33.51 2.42 -1 -9 0 86.21 4.70 -1 -9 0 88.66 4.31 1 9 0 90.65 4.49 1 9 0 89.82 4.18 1 9 0 90.32 4.85 -2 -9 0 11.55 2.06 -2 -9 0 12.68 1.63 2 9 0 8.14 2.50 2 9 0 14.13 1.50 2 9 0 13.12 1.92 -3 -9 0 24.68 2.48 -3 -9 0 26.42 2.01 3 9 0 25.74 1.82 3 9 0 18.55 2.75 3 9 0 26.56 2.31 -4 -9 0 50.68 2.90 -4 -9 0 47.62 3.22 4 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23.11 2.50 6 9 20 19.53 2.68 -7 -9 -20 6.54 2.28 0 -10 -20 0.80 1.55 0 10 20 1.57 1.38 -1 -10 -20 30.59 3.73 1 10 20 25.52 2.85 1 10 20 33.71 3.36 2 10 20 11.64 2.84 -6 -10 -20 16.65 3.42 -1 -11 -20 16.12 3.44 1 11 20 17.49 3.10 4 11 20 8.38 2.68 0 2 -21 19.34 2.88 0 2 -21 20.76 3.69 0 -2 21 15.16 3.71 -1 2 -21 19.10 2.74 -1 2 -21 18.85 3.49 -1 2 -21 27.15 2.39 1 -2 21 27.94 3.36 -2 2 -21 1.30 1.34 -2 2 -21 -1.71 1.40 -2 2 -21 -0.18 1.23 2 -2 21 1.10 1.33 1 1 -21 0.99 1.82 1 1 -21 -1.82 1.53 -1 -1 21 3.94 1.31 -1 -1 21 -0.94 1.58 0 1 -21 16.18 2.82 0 -1 21 22.32 3.07 -1 1 -21 3.51 1.32 -1 1 -21 6.49 1.84 1 -1 21 3.43 1.30 -2 1 -21 1.51 1.20 -2 1 -21 1.45 1.31 2 -1 21 0.19 1.26 -3 1 -21 4.36 1.46 -3 1 -21 7.87 1.89 -3 1 -21 8.02 2.20 3 -1 21 4.79 1.39 -4 1 -21 1.27 1.38 -4 1 -21 0.46 1.15 -4 1 -21 -0.44 1.30 4 -1 21 0.68 1.30 1 0 -21 2.75 1.21 1 0 -21 0.27 1.61 -1 0 21 0.05 1.19 0 0 -21 16.06 2.11 0 0 -21 15.86 2.84 0 0 21 14.59 2.92 -1 0 -21 3.34 1.31 -1 0 -21 2.56 1.69 -1 0 -21 3.08 1.27 1 0 21 1.01 1.25 -2 0 -21 1.50 1.21 -2 0 -21 0.52 1.23 2 0 21 0.18 1.24 -3 0 -21 15.02 2.06 -3 0 -21 13.54 2.37 3 0 21 12.97 2.92 -4 0 -21 12.67 2.04 -4 0 -21 13.79 2.29 4 0 21 10.36 2.88 -5 0 -21 -1.03 1.23 -5 0 -21 1.07 1.44 -5 0 -21 1.16 1.15 5 0 21 0.16 1.29 2 -1 -21 4.50 1.51 2 -1 -21 1.31 1.84 -2 1 21 -1.25 1.56 -2 1 21 -0.81 1.17 1 -1 -21 1.69 1.51 1 -1 -21 4.29 1.25 1 -1 -21 1.36 1.73 1 -1 -21 3.93 1.45 -1 1 21 0.93 1.19 0 -1 -21 6.38 1.84 0 -1 -21 3.95 1.76 0 1 21 3.80 1.29 -1 -1 -21 1.09 1.63 -1 -1 -21 1.97 1.19 -1 -1 -21 3.46 1.33 1 1 21 1.56 1.23 -2 -1 -21 2.62 1.59 -2 -1 -21 4.81 1.34 -2 -1 -21 3.61 1.32 2 1 21 1.84 1.26 -3 -1 -21 27.17 2.72 -3 -1 -21 25.93 2.29 -3 -1 -21 21.73 3.77 3 1 21 26.90 3.25 -4 -1 -21 18.24 2.44 -4 -1 -21 17.30 2.17 4 1 21 17.99 3.03 -5 -1 -21 1.54 1.16 -5 -1 -21 -0.19 1.34 5 1 21 -1.12 1.28 -6 -1 -21 0.11 1.42 -6 -1 -21 1.45 1.14 -6 -1 -21 -1.37 1.14 6 1 21 -0.53 1.30 -2 2 21 13.82 3.53 -2 2 21 14.89 2.78 1 -2 -21 21.39 3.40 1 -2 -21 22.23 4.50 1 -2 -21 27.65 3.41 1 -2 -21 22.89 2.18 -1 2 21 17.64 2.88 0 -2 -21 4.09 1.47 0 -2 -21 6.78 1.78 0 -2 -21 4.79 2.03 0 2 21 2.72 1.24 -1 -2 -21 0.01 1.79 -1 -2 -21 0.91 1.13 -1 -2 -21 3.36 1.36 -1 -2 -21 1.03 1.31 1 2 21 0.19 1.18 -2 -2 -21 3.68 1.33 -2 -2 -21 10.28 2.65 -2 -2 -21 4.61 1.30 -2 -2 -21 0.82 1.80 2 2 21 1.55 1.26 -3 -2 -21 14.69 3.77 -3 -2 -21 17.03 2.09 -3 -2 -21 19.78 2.65 3 2 21 14.38 2.89 -4 -2 -21 11.77 3.36 -4 -2 -21 16.11 2.53 -4 -2 -21 12.70 2.05 4 2 21 12.24 2.90 -5 -2 -21 8.86 2.02 -5 -2 -21 5.57 1.70 5 2 21 4.25 1.39 -6 -2 -21 6.09 1.63 -6 -2 -21 10.06 2.26 2 -3 -21 29.14 3.78 -2 3 21 23.32 3.02 -2 3 21 22.97 3.79 1 -3 -21 34.97 2.39 1 -3 -21 29.61 3.70 -1 3 21 25.72 3.86 -1 3 21 28.36 3.11 0 -3 -21 6.03 1.71 0 -3 -21 3.21 1.51 -1 -3 -21 5.66 1.27 -2 -3 -21 0.43 1.14 -2 -3 -21 -0.40 1.31 2 3 21 -1.03 1.16 -3 -3 -21 2.52 1.34 -3 -3 -21 0.40 1.28 -3 -3 -21 1.08 1.23 3 3 21 -1.03 1.20 -4 -3 -21 6.13 1.46 -4 -3 -21 3.72 1.83 -4 -3 -21 9.20 2.71 -4 -3 -21 11.91 2.60 4 3 21 2.32 1.32 -5 -3 -21 8.81 2.07 -5 -3 -21 12.51 2.54 -6 -3 -21 19.85 2.36 6 3 21 18.13 3.01 2 -4 -21 7.07 1.77 -2 4 21 5.73 1.27 -2 4 21 6.32 1.75 1 -4 -21 8.73 1.76 0 -4 -21 6.87 1.70 -1 -4 -21 9.94 1.79 -2 -4 -21 1.61 1.37 -2 -4 -21 4.37 1.23 -3 -4 -21 0.12 1.18 -3 -4 -21 2.25 1.40 -3 -4 -21 -0.22 1.28 3 4 21 -0.87 1.18 -4 -4 -21 1.43 1.27 -4 -4 -21 0.01 1.25 4 4 21 -1.14 1.18 -5 -4 -21 4.62 1.47 -5 -4 -21 2.56 1.24 5 4 21 0.69 1.24 -6 -4 -21 21.02 3.87 -6 -4 -21 23.62 2.42 6 4 21 19.60 3.03 -7 -4 -21 16.75 2.29 2 -5 -21 1.22 1.63 -2 5 21 -0.75 1.56 -2 5 21 -1.52 1.09 1 -5 -21 -0.19 1.52 -1 5 21 -2.12 1.42 -1 5 21 -1.93 1.05 0 -5 -21 10.39 1.72 -1 -5 -21 19.62 3.32 -1 -5 -21 22.87 2.03 1 5 21 19.01 3.29 1 5 21 18.52 2.92 -2 -5 -21 19.75 1.99 -2 -5 -21 16.03 3.10 2 5 21 12.46 3.16 2 5 21 14.52 2.71 -3 -5 -21 -0.36 1.29 -3 -5 -21 2.52 1.23 -4 -5 -21 -1.02 1.22 -4 -5 -21 0.41 1.29 4 5 21 -1.37 1.17 -5 -5 -21 -1.70 1.18 -5 -5 -21 0.11 1.32 -5 -5 -21 3.35 1.52 -6 -5 -21 18.93 2.93 -6 -5 -21 25.31 2.40 6 5 21 19.29 3.09 -7 -5 -21 17.92 2.64 -7 -5 -21 14.05 2.31 1 -6 -21 -1.16 1.56 -1 6 21 -1.71 1.42 -1 -6 -21 44.53 4.05 1 6 21 45.30 3.50 1 6 21 46.80 3.91 -2 -6 -21 37.24 2.55 -2 -6 -21 31.68 3.58 2 6 21 33.33 3.52 2 6 21 31.68 3.12 -3 -6 -21 2.26 1.21 -3 -6 -21 0.07 1.35 -4 -6 -21 1.12 1.24 -5 -6 -21 4.69 1.47 -6 -6 -21 10.94 2.17 -7 -6 -21 3.90 1.61 1 -7 -21 -1.84 1.55 -1 7 21 -2.04 1.44 -1 -7 -21 28.11 3.61 1 7 21 29.64 3.44 1 7 21 28.89 3.00 -2 -7 -21 5.81 1.55 2 7 21 6.62 1.48 2 7 21 5.75 1.26 -3 -7 -21 8.15 1.88 -4 -7 -21 4.56 1.37 -4 -7 -21 1.68 1.34 -5 -7 -21 7.34 1.99 0 -8 -21 -0.82 1.54 0 8 21 -1.37 1.38 -3 -8 -21 9.83 2.98 3 8 21 6.08 1.28 3 8 21 12.23 2.86 -4 -8 -21 9.83 2.87 4 8 21 6.03 1.30 -5 -8 -21 11.45 2.04 -6 -8 -21 -1.31 1.19 -6 -8 -21 0.31 1.47 6 8 21 -1.69 1.12 0 -9 -21 1.44 1.62 0 9 21 -1.55 1.04 0 9 21 0.39 1.41 -5 -9 -21 13.84 2.88 5 9 21 9.56 2.46 -1 0 -22 1.98 1.34 1 0 22 1.34 1.30 -2 0 -22 14.32 2.04 -2 0 -22 15.11 2.55 2 0 22 13.22 3.05 0 -1 -22 -0.32 1.65 0 -1 -22 0.60 1.20 0 -1 -22 -0.35 1.44 0 1 22 -1.33 1.21 -1 -1 -22 20.28 2.91 -1 -1 -22 16.46 2.06 -1 -1 -22 14.52 3.63 1 1 22 14.07 2.97 -2 -1 -22 24.93 2.77 -2 -1 -22 14.89 3.55 -2 -1 -22 20.41 2.17 2 1 22 18.52 3.01 -3 -1 -22 6.92 1.88 -3 -1 -22 -0.38 1.74 3 1 22 3.42 1.35 -4 -1 -22 1.71 1.21 -4 -1 -22 0.96 1.31 4 1 22 -1.68 1.25 0 -2 -22 1.35 1.46 0 -2 -22 0.10 1.09 0 -2 -22 -1.39 1.78 0 -2 -22 1.63 1.39 0 2 22 -1.16 1.17 -1 -2 -22 21.46 3.00 -1 -2 -22 19.98 3.10 -1 -2 -22 15.46 2.05 1 2 22 12.48 2.93 -2 -2 -22 6.68 1.82 -3 -2 -22 10.97 2.63 -3 -2 -22 8.12 1.92 -4 -2 -22 -0.12 1.57 -4 -2 -22 3.07 1.26 -4 -2 -22 2.12 1.39 4 2 22 0.21 1.30 -5 -2 -22 6.14 1.55 -5 -2 -22 9.52 2.39 1 -3 -22 7.87 1.82 1 -3 -22 4.24 1.61 0 -3 -22 2.79 1.52 0 -3 -22 5.62 1.29 -1 -3 -22 7.30 1.79 -2 -3 -22 4.63 1.28 -2 -3 -22 3.21 1.37 2 3 22 1.46 1.25 -3 -3 -22 2.87 1.92 -3 -3 -22 3.86 1.34 -3 -3 -22 5.21 1.37 3 3 22 1.92 1.29 -4 -3 -22 8.48 2.00 -4 -3 -22 14.53 2.14 4 3 22 10.38 2.81 -5 -3 -22 23.30 2.47 -5 -3 -22 26.97 3.65 -5 -3 -22 29.96 2.89 5 3 22 20.75 3.17 0 -4 -22 11.83 3.30 0 -4 -22 15.35 1.92 -2 -4 -22 1.74 1.17 -3 -4 -22 0.96 1.26 -3 -4 -22 -0.94 1.28 3 4 22 -1.45 1.20 -4 -4 -22 23.83 2.30 -4 -4 -22 20.60 3.05 4 4 22 17.89 2.98 -5 -4 -22 27.33 4.41 -5 -4 -22 31.61 3.18 -5 -4 -22 29.28 2.58 5 4 22 24.83 3.16 0 -5 -22 15.42 3.34 0 5 22 11.05 2.78 0 5 22 11.66 3.26 -1 -5 -22 3.82 1.18 -2 -5 -22 0.73 1.11 -2 -5 -22 -1.68 1.33 -3 -5 -22 -1.53 1.27 -3 -5 -22 0.79 1.23 3 5 22 -1.98 1.15 -4 -5 -22 9.32 1.99 -5 -5 -22 11.35 2.15 -6 -5 -22 9.26 2.11 0 -6 -22 30.13 3.74 0 6 22 30.05 3.64 0 6 22 25.25 3.02 -2 -6 -22 0.27 1.14 -2 -6 -22 -1.43 1.37 2 6 22 -1.92 1.12 -4 -6 -22 0.96 1.30 -4 -6 -22 -1.49 1.26 4 6 22 -1.88 1.17 -5 -6 -22 3.11 1.42 -6 -6 -22 4.34 1.53 -4 -7 -22 -1.28 1.29 -4 -7 -22 1.67 1.31 -5 -7 -22 0.60 1.35 -3 -8 -22 25.52 3.34 3 8 22 22.30 2.89 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 21994 _database_code_depnum_ccdc_archive 'CCDC 909099' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_dr021 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H63 Cl4 N3 Sn2' _chemical_formula_weight 1133.25 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.2152(5) _cell_length_b 14.1924(4) _cell_length_c 22.1938(6) _cell_angle_alpha 90 _cell_angle_beta 111.5820(10) _cell_angle_gamma 90 _cell_volume 5335.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9983 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 24.67 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_density_meas n/a _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_F_000 2304 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 1.173 _shelx_estimated_absorpt_T_min 0.872 _shelx_estimated_absorpt_T_max 0.977 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6660 _exptl_absorpt_correction_T_max 0.7451 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg (650 frames). Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 93952 _diffrn_reflns_av_unetI/netI 0.0509 _diffrn_reflns_av_R_equivalents 0.0761 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.741 _diffrn_reflns_theta_max 24.733 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.937 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_Laue_measured_fraction_full 0.937 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_point_group_measured_fraction_full 0.937 _reflns_number_total 9053 _reflns_number_gt 6399 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-03 (Sheldrick, 2003)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+5.5794P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 9053 _refine_ls_number_parameters 521 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1060 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.67681(2) 0.14630(2) 0.35007(2) 0.03228(4) Uani 1 1 d . . . . . Cl1 Cl 0.69926(4) 0.17930(4) 0.24873(3) 0.04632(19) Uani 1 1 d . . . . . N1 N 0.69805(9) -0.02784(12) 0.34784(8) 0.0293(5) Uani 1 1 d . . . . . N2 N 0.80766(9) 0.11253(12) 0.38796(8) 0.0256(5) Uani 1 1 d . . . . . N3 N 0.75980(9) 0.29205(12) 0.38839(8) 0.0275(5) Uani 1 1 d . . . . . Sn2 Sn 0.82467(2) 0.12703(2) 0.60626(2) 0.04787(5) Uani 1 1 d . . . . . Cl2 Cl 0.72500(4) 0.06705(5) 0.50306(3) 0.0560(2) Uani 1 1 d . . . . . Cl3 Cl 0.92103(4) 0.16596(5) 0.55601(3) 0.0599(2) Uani 1 1 d . . . . . Cl4 Cl 0.87932(5) -0.03053(5) 0.63961(3) 0.0656(2) Uani 1 1 d . . . . . C1 C 0.76929(12) -0.05102(15) 0.38429(10) 0.0300(6) Uani 1 1 d . . . . . C2 C 0.83131(11) 0.02226(15) 0.39735(9) 0.0285(6) Uani 1 1 d . . . . . C3 C 0.91110(12) -0.00065(17) 0.41623(10) 0.0347(7) Uani 1 1 d . . . . . H3A H 0.9278 -0.0644 0.4238 0.042 Uiso 1 1 calc R U . . . C4 C 0.96481(12) 0.06971(16) 0.42361(11) 0.0373(7) Uani 1 1 d . . . . . H4A H 1.0193 0.0552 0.4357 0.045 Uiso 1 1 calc R U . . . C5 C 0.93958(12) 0.16167(17) 0.41349(10) 0.0368(7) Uani 1 1 d . . . . . H5A H 0.9764 0.2112 0.4183 0.044 Uiso 1 1 calc R U . . . C6 C 0.86008(11) 0.18158(15) 0.39624(9) 0.0284(6) Uani 1 1 d . . . . . C7 C 0.82873(12) 0.27934(15) 0.38728(9) 0.0290(6) Uani 1 1 d . . . . . C8 C 0.79571(12) -0.14588(15) 0.41348(10) 0.0325(6) Uani 1 1 d . . . . . C9 C 0.79508(14) -0.22281(18) 0.37491(12) 0.0487(9) Uani 1 1 d . . . . . H9A H 0.7760 -0.2167 0.3291 0.058 Uiso 1 1 calc R U . . . C10 C 0.82263(16) -0.30887(18) 0.40394(14) 0.0619(10) Uani 1 1 d . . . . . H10A H 0.8211 -0.3623 0.3777 0.074 Uiso 1 1 calc R U . . . C11 C 0.85196(15) -0.31791(19) 0.46983(14) 0.0599(10) Uani 1 1 d . . . . . H11A H 0.8718 -0.3769 0.4892 0.072 Uiso 1 1 calc R U . . . C12 C 0.85269(13) -0.24072(19) 0.50826(12) 0.0498(8) Uani 1 1 d . . . . . H12A H 0.8717 -0.2471 0.5541 0.060 Uiso 1 1 calc R U . . . C13 C 0.82605(12) -0.15538(17) 0.48022(11) 0.0389(7) Uani 1 1 d . . . . . H13A H 0.8284 -0.1021 0.5068 0.047 Uiso 1 1 calc R U . . . C14 C 0.88077(12) 0.35435(16) 0.37683(10) 0.0339(6) Uani 1 1 d . . . . . C15 C 0.90240(16) 0.3463(2) 0.32380(12) 0.0722(10) Uani 1 1 d . . . . . H15A H 0.8861 0.2933 0.2959 0.087 Uiso 1 1 calc R U . . . C16 C 0.94839(18) 0.4167(3) 0.31136(15) 0.0934(12) Uani 1 1 d . . . . . H16A H 0.9614 0.4133 0.2737 0.112 Uiso 1 1 calc R U . . . C17 C 0.97485(17) 0.4907(2) 0.35331(16) 0.0826(11) Uani 1 1 d . . . . . H17A H 1.0067 0.5380 0.3449 0.099 Uiso 1 1 calc R U . . . C18 C 0.95613(15) 0.4970(2) 0.40640(16) 0.0783(11) Uani 1 1 d . . . . . H18A H 0.9753 0.5482 0.4356 0.094 Uiso 1 1 calc R U . . . C19 C 0.90837(14) 0.42820(19) 0.41860(13) 0.0618(8) Uani 1 1 d . . . . . H19A H 0.8951 0.4328 0.4561 0.074 Uiso 1 1 calc R U . . . C20 C 0.63474(11) -0.09492(14) 0.33913(9) 0.0260(6) Uani 1 1 d . . . . . C21 C 0.58530(11) -0.12815(15) 0.27796(10) 0.0296(6) Uani 1 1 d . . . . . C22 C 0.52802(12) -0.19208(16) 0.27991(10) 0.0359(7) Uani 1 1 d . . . . . H22A H 0.4936 -0.2182 0.2402 0.043 Uiso 1 1 calc R U . . . C23 C 0.51853(12) -0.21939(16) 0.33595(11) 0.0375(7) Uani 1 1 d . . . . . H23A H 0.4783 -0.2635 0.3335 0.045 Uiso 1 1 calc R U . . . C24 C 0.56595(12) -0.18435(16) 0.39597(10) 0.0331(7) Uani 1 1 d . . . . . C25 C 0.62368(12) -0.12144(15) 0.39551(10) 0.0300(6) Uani 1 1 d . . . . . H25A H 0.6573 -0.0951 0.4355 0.036 Uiso 1 1 calc R U . . . C26 C 0.58764(12) -0.09512(17) 0.21256(10) 0.0350(7) Uani 1 1 d . . . . . C27 C 0.53867(16) -0.1587(2) 0.15633(11) 0.0578(9) Uani 1 1 d . . . . . H27A H 0.5604 -0.2227 0.1635 0.087 Uiso 1 1 calc R U . . . H27B H 0.5404 -0.1340 0.1156 0.087 Uiso 1 1 calc R U . . . H27C H 0.4838 -0.1600 0.1539 0.087 Uiso 1 1 calc R U . . . C28 C 0.55054(14) 0.00374(19) 0.19873(12) 0.0521(9) Uani 1 1 d . . . . . H28A H 0.4969 0.0014 0.1991 0.078 Uiso 1 1 calc R U . . . H28B H 0.5484 0.0251 0.1561 0.078 Uiso 1 1 calc R U . . . H28C H 0.5826 0.0477 0.2321 0.078 Uiso 1 1 calc R U . . . C29 C 0.67141(13) -0.09118(19) 0.21159(11) 0.0448(8) Uani 1 1 d . . . . . H29A H 0.6952 -0.1541 0.2203 0.067 Uiso 1 1 calc R U . . . H29B H 0.7035 -0.0473 0.2449 0.067 Uiso 1 1 calc R U . . . H29C H 0.6690 -0.0697 0.1689 0.067 Uiso 1 1 calc R U . . . C30 C 0.55612(13) -0.21002(18) 0.45982(11) 0.0416(7) Uani 1 1 d . . . . . C31 C 0.52047(18) -0.1268(2) 0.48134(13) 0.0797(11) Uani 1 1 d . . . . . H31A H 0.5548 -0.0718 0.4868 0.120 Uiso 1 1 calc R U . . . H31B H 0.5151 -0.1414 0.5227 0.120 Uiso 1 1 calc R U . . . H31C H 0.4683 -0.1130 0.4486 0.120 Uiso 1 1 calc R U . . . C32 C 0.50377(16) -0.2959(2) 0.45153(13) 0.0719(10) Uani 1 1 d . . . . . H32A H 0.4987 -0.3109 0.4929 0.108 Uiso 1 1 calc R U . . . H32B H 0.5273 -0.3496 0.4375 0.108 Uiso 1 1 calc R U . . . H32C H 0.4515 -0.2827 0.4189 0.108 Uiso 1 1 calc R U . . . C33 C 0.63664(16) -0.2332(2) 0.51135(12) 0.0641(10) Uani 1 1 d . . . . . H33A H 0.6718 -0.1788 0.5175 0.096 Uiso 1 1 calc R U . . . H33B H 0.6594 -0.2875 0.4973 0.096 Uiso 1 1 calc R U . . . H33C H 0.6304 -0.2481 0.5523 0.096 Uiso 1 1 calc R U . . . C34 C 0.72216(11) 0.38351(15) 0.37284(10) 0.0297(6) Uani 1 1 d . . . . . C35 C 0.70097(12) 0.43703(15) 0.41731(10) 0.0317(6) Uani 1 1 d . . . . . C36 C 0.66800(13) 0.52528(16) 0.39316(11) 0.0387(7) Uani 1 1 d . . . . . H36A H 0.6549 0.5663 0.4215 0.046 Uiso 1 1 calc R U . . . C37 C 0.65363(12) 0.55581(17) 0.33132(10) 0.0361(7) Uani 1 1 d . . . . . H37A H 0.6317 0.6166 0.3185 0.043 Uiso 1 1 calc R U . . . C38 C 0.67061(11) 0.49942(16) 0.28700(10) 0.0336(7) Uani 1 1 d . . . . . C39 C 0.70553(11) 0.41420(15) 0.30977(10) 0.0301(6) Uani 1 1 d . . . . . H39A H 0.7190 0.3743 0.2810 0.036 Uiso 1 1 calc R U . . . C40 C 0.71190(13) 0.40601(17) 0.48637(10) 0.0374(7) Uani 1 1 d . . . . . C41 C 0.67301(15) 0.3105(2) 0.48494(12) 0.0570(9) Uani 1 1 d . . . . . H41A H 0.6966 0.2638 0.4650 0.085 Uiso 1 1 calc R U . . . H41B H 0.6163 0.3154 0.4596 0.085 Uiso 1 1 calc R U . . . H41C H 0.6811 0.2911 0.5293 0.085 Uiso 1 1 calc R U . . . C42 C 0.79973(14) 0.3977(2) 0.52899(12) 0.0524(9) Uani 1 1 d . . . . . H42A H 0.8256 0.4587 0.5305 0.079 Uiso 1 1 calc R U . . . H42B H 0.8246 0.3501 0.5108 0.079 Uiso 1 1 calc R U . . . H42C H 0.8051 0.3791 0.5729 0.079 Uiso 1 1 calc R U . . . C43 C 0.67375(16) 0.4751(2) 0.51935(12) 0.0667(9) Uani 1 1 d . . . . . H43A H 0.6975 0.5376 0.5216 0.100 Uiso 1 1 calc R U . . . H43B H 0.6825 0.4529 0.5633 0.100 Uiso 1 1 calc R U . . . H43C H 0.6169 0.4789 0.4943 0.100 Uiso 1 1 calc R U . . . C44 C 0.65231(13) 0.53242(16) 0.21669(11) 0.0402(7) Uani 1 1 d . . . . . C45 C 0.56328(14) 0.55020(19) 0.18462(11) 0.0511(9) Uani 1 1 d . . . . . H45A H 0.5507 0.5713 0.1399 0.077 Uiso 1 1 calc R U . . . H45B H 0.5476 0.5989 0.2088 0.077 Uiso 1 1 calc R U . . . H45C H 0.5346 0.4918 0.1846 0.077 Uiso 1 1 calc R U . . . C46 C 0.67559(17) 0.4608(2) 0.17765(12) 0.0631(10) Uani 1 1 d . . . . . H46A H 0.6628 0.4844 0.1335 0.095 Uiso 1 1 calc R U . . . H46B H 0.6467 0.4020 0.1763 0.095 Uiso 1 1 calc R U . . . H46C H 0.7325 0.4489 0.1976 0.095 Uiso 1 1 calc R U . . . C47 C 0.69680(16) 0.62462(19) 0.21815(13) 0.0638(9) Uani 1 1 d . . . . . H47A H 0.6854 0.6464 0.1737 0.096 Uiso 1 1 calc R U . . . H47B H 0.7537 0.6139 0.2397 0.096 Uiso 1 1 calc R U . . . H47C H 0.6797 0.6725 0.2420 0.096 Uiso 1 1 calc R U . . . C48 C 0.88120(9) 0.93892(13) 0.23061(8) 0.0888(11) Uiso 1 1 d G . . . . C49 C 0.83674(12) 0.89080(16) 0.17448(8) 0.1097(13) Uiso 1 1 d G . . . . H49A H 0.8044 0.9248 0.1373 0.132 Uiso 1 1 calc R U . . . C50 C 0.83957(16) 0.79300(16) 0.17276(13) 0.0982(12) Uiso 1 1 d G . . . . H50A H 0.8092 0.7601 0.1344 0.118 Uiso 1 1 calc R U . . . C51 C 0.88686(17) 0.74332(13) 0.22717(16) 0.1291(16) Uiso 1 1 d G . . . . H51A H 0.8888 0.6765 0.2260 0.155 Uiso 1 1 calc R U . . . C52 C 0.93132(15) 0.79144(16) 0.28330(13) 0.1196(15) Uiso 1 1 d G . . . . H52A H 0.9636 0.7575 0.3205 0.144 Uiso 1 1 calc R U . . . C53 C 0.92849(12) 0.88923(16) 0.28503(9) 0.0711(9) Uiso 1 1 d G . . . . H53A H 0.9589 0.9221 0.3234 0.085 Uiso 1 1 calc R U . . . C54 C 0.8797(3) 1.0402(3) 0.2330(2) 0.1304(16) Uiso 1 1 d . . . . . H54A H 0.8443 1.0647 0.1911 0.196 Uiso 1 1 calc R U . . . H54B H 0.9331 1.0648 0.2425 0.196 Uiso 1 1 calc R U . . . H54C H 0.8609 1.0602 0.2671 0.196 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02251(6) 0.03229(8) 0.03900(7) 0.00074(7) 0.00774(5) 0.00295(7) Cl1 0.0561(3) 0.0425(3) 0.0351(3) 0.0019(3) 0.0106(2) 0.0020(3) N1 0.0251(8) 0.0311(10) 0.0302(9) -0.0006(8) 0.0086(6) 0.0005(7) N2 0.0202(8) 0.0259(9) 0.0299(8) 0.0031(7) 0.0082(6) 0.0048(7) N3 0.0287(8) 0.0262(9) 0.0303(8) 0.0018(8) 0.0141(6) 0.0020(7) Sn2 0.06184(10) 0.04689(10) 0.03633(8) -0.00374(8) 0.01975(7) 0.00162(8) Cl2 0.0605(4) 0.0529(4) 0.0490(3) -0.0078(3) 0.0136(3) -0.0009(3) Cl3 0.0591(4) 0.0714(5) 0.0485(3) 0.0128(3) 0.0192(3) 0.0087(3) Cl4 0.0880(5) 0.0560(4) 0.0523(4) 0.0127(3) 0.0253(3) 0.0102(4) C1 0.0331(10) 0.0287(12) 0.0273(10) -0.0018(9) 0.0103(8) 0.0033(9) C2 0.0252(10) 0.0322(12) 0.0267(10) -0.0026(9) 0.0079(7) -0.0010(9) C3 0.0299(10) 0.0323(12) 0.0376(12) 0.0031(10) 0.0071(8) 0.0084(10) C4 0.0208(10) 0.0381(13) 0.0518(13) 0.0003(11) 0.0120(8) 0.0040(10) C5 0.0259(10) 0.0405(14) 0.0449(12) 0.0023(11) 0.0143(8) -0.0055(10) C6 0.0288(10) 0.0279(12) 0.0306(10) -0.0013(9) 0.0133(7) -0.0017(9) C7 0.0317(10) 0.0312(12) 0.0242(10) -0.0030(9) 0.0103(7) -0.0028(9) C8 0.0257(10) 0.0261(11) 0.0411(11) -0.0018(10) 0.0070(8) -0.0036(9) C9 0.0449(14) 0.0403(14) 0.0465(14) -0.0059(12) -0.0002(11) 0.0042(12) C10 0.0643(17) 0.0279(14) 0.0756(18) -0.0048(14) 0.0047(14) 0.0049(13) C11 0.0466(15) 0.0369(14) 0.0855(19) 0.0241(14) 0.0118(13) 0.0061(12) C12 0.0391(12) 0.0573(16) 0.0504(14) 0.0175(13) 0.0137(10) 0.0030(12) C13 0.0347(11) 0.0384(13) 0.0418(12) 0.0041(11) 0.0120(9) 0.0036(10) C14 0.0295(10) 0.0319(12) 0.0402(11) 0.0084(10) 0.0127(8) -0.0008(10) C15 0.0722(15) 0.106(2) 0.0458(13) -0.0056(15) 0.0308(10) -0.0388(15) C16 0.0874(18) 0.134(3) 0.0695(17) 0.0127(18) 0.0413(12) -0.0433(18) C17 0.0674(15) 0.0615(18) 0.129(2) 0.0286(17) 0.0484(13) -0.0160(14) C18 0.0648(14) 0.0507(17) 0.137(2) -0.0264(17) 0.0577(13) -0.0213(13) C19 0.0638(12) 0.0507(16) 0.0931(15) -0.0189(14) 0.0549(9) -0.0246(12) C20 0.0199(9) 0.0222(11) 0.0329(10) -0.0003(9) 0.0061(7) -0.0004(8) C21 0.0244(9) 0.0266(12) 0.0367(11) -0.0027(9) 0.0100(8) 0.0021(9) C22 0.0328(11) 0.0397(13) 0.0321(11) -0.0087(10) 0.0085(8) -0.0053(10) C23 0.0325(11) 0.0336(13) 0.0460(12) -0.0046(11) 0.0139(8) -0.0095(10) C24 0.0345(11) 0.0329(12) 0.0328(11) -0.0010(10) 0.0134(8) 0.0002(10) C25 0.0265(10) 0.0286(12) 0.0302(10) -0.0049(9) 0.0047(8) 0.0012(9) C26 0.0330(11) 0.0403(13) 0.0289(11) -0.0007(10) 0.0081(8) 0.0003(10) C27 0.0711(16) 0.0737(19) 0.0252(11) -0.0098(13) 0.0137(10) -0.0159(15) C28 0.0463(13) 0.0594(17) 0.0451(14) 0.0068(13) 0.0104(11) 0.0094(13) C29 0.0455(12) 0.0514(15) 0.0404(12) 0.0073(12) 0.0192(9) 0.0101(12) C30 0.0431(12) 0.0454(15) 0.0375(12) -0.0021(11) 0.0161(9) -0.0051(11) C31 0.1058(18) 0.091(2) 0.0600(14) 0.0043(15) 0.0515(11) 0.0338(16) C32 0.0845(16) 0.085(2) 0.0586(14) 0.0006(15) 0.0403(11) -0.0341(15) C33 0.0674(17) 0.076(2) 0.0449(14) 0.0165(14) 0.0157(12) -0.0020(15) C34 0.0259(10) 0.0286(12) 0.0354(10) 0.0017(9) 0.0124(7) -0.0018(9) C35 0.0278(10) 0.0301(12) 0.0363(11) -0.0021(10) 0.0108(8) 0.0024(9) C36 0.0385(11) 0.0343(13) 0.0435(12) -0.0047(11) 0.0151(9) 0.0050(10) C37 0.0358(11) 0.0324(13) 0.0382(11) 0.0019(10) 0.0112(9) 0.0031(10) C38 0.0282(10) 0.0355(13) 0.0408(11) 0.0023(10) 0.0168(8) -0.0072(9) C39 0.0327(10) 0.0252(12) 0.0358(10) -0.0020(9) 0.0164(7) -0.0006(9) C40 0.0424(12) 0.0375(13) 0.0339(11) 0.0012(10) 0.0158(8) 0.0081(10) C41 0.0704(15) 0.0630(18) 0.0460(13) 0.0047(13) 0.0314(10) -0.0050(14) C42 0.0504(14) 0.0662(18) 0.0390(12) 0.0003(13) 0.0146(10) 0.0039(13) C43 0.0897(16) 0.0724(19) 0.0492(13) 0.0056(14) 0.0388(11) 0.0297(15) C44 0.0505(13) 0.0320(13) 0.0394(12) 0.0040(10) 0.0179(9) -0.0024(11) C45 0.0546(14) 0.0561(17) 0.0369(13) 0.0110(12) 0.0101(10) 0.0031(13) C46 0.0894(17) 0.0667(19) 0.0400(13) 0.0136(13) 0.0320(11) 0.0158(15) C47 0.0687(16) 0.0664(18) 0.0530(14) 0.0165(13) 0.0184(11) -0.0267(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 N2 2.2680(15) . ? Sn1 Cl1 2.4742(7) . ? Sn1 N1 2.5049(18) . ? Sn1 N3 2.5182(16) . ? N1 C1 1.294(2) . ? N1 C20 1.452(3) . ? N2 C6 1.333(3) . ? N2 C2 1.343(3) . ? N3 C7 1.278(3) . ? N3 C34 1.449(3) . ? Sn2 Cl4 2.4489(7) . ? Sn2 Cl3 2.4637(8) . ? Sn2 Cl2 2.4915(6) . ? C1 C2 1.484(3) . ? C1 C8 1.495(3) . ? C2 C3 1.395(3) . ? C3 C4 1.365(3) . ? C4 C5 1.374(3) . ? C5 C6 1.384(3) . ? C6 C7 1.486(3) . ? C7 C14 1.499(3) . ? C8 C13 1.384(3) . ? C8 C9 1.385(3) . ? C9 C10 1.386(4) . ? C10 C11 1.366(4) . ? C11 C12 1.385(4) . ? C12 C13 1.367(3) . ? C14 C19 1.367(3) . ? C14 C15 1.376(4) . ? C15 C16 1.395(5) . ? C16 C17 1.368(5) . ? C17 C18 1.345(5) . ? C18 C19 1.399(4) . ? C20 C25 1.390(3) . ? C20 C21 1.406(3) . ? C21 C22 1.395(3) . ? C21 C26 1.541(3) . ? C22 C23 1.373(3) . ? C23 C24 1.386(3) . ? C24 C25 1.382(3) . ? C24 C30 1.536(3) . ? C26 C27 1.532(3) . ? C26 C29 1.535(3) . ? C26 C28 1.538(3) . ? C30 C31 1.508(4) . ? C30 C32 1.517(4) . ? C30 C33 1.527(3) . ? C34 C39 1.389(3) . ? C34 C35 1.407(3) . ? C35 C36 1.407(3) . ? C35 C40 1.536(3) . ? C36 C37 1.370(3) . ? C37 C38 1.388(3) . ? C38 C39 1.373(3) . ? C38 C44 1.544(3) . ? C40 C41 1.524(4) . ? C40 C42 1.535(3) . ? C40 C43 1.534(4) . ? C44 C46 1.495(4) . ? C44 C47 1.533(4) . ? C44 C45 1.533(3) . ? C48 C49 1.3900 . ? C48 C53 1.3900 . ? C48 C54 1.440(5) . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? 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 N2 Sn1 Cl1 82.79(5) . . ? N2 Sn1 N1 69.50(6) . . ? Cl1 Sn1 N1 95.19(5) . . ? N2 Sn1 N3 68.28(6) . . ? Cl1 Sn1 N3 82.65(4) . . ? N1 Sn1 N3 137.67(5) . . ? C1 N1 C20 118.76(17) . . ? C1 N1 Sn1 111.42(13) . . ? C20 N1 Sn1 121.90(12) . . ? C6 N2 C2 120.49(17) . . ? C6 N2 Sn1 119.84(13) . . ? C2 N2 Sn1 119.50(13) . . ? C7 N3 C34 120.27(18) . . ? C7 N3 Sn1 110.47(14) . . ? C34 N3 Sn1 118.87(11) . . ? Cl4 Sn2 Cl3 93.64(3) . . ? Cl4 Sn2 Cl2 92.50(2) . . ? Cl3 Sn2 Cl2 93.44(2) . . ? N1 C1 C2 117.42(19) . . ? N1 C1 C8 126.08(19) . . ? C2 C1 C8 116.49(16) . . ? N2 C2 C3 120.54(19) . . ? N2 C2 C1 117.43(17) . . ? C3 C2 C1 122.0(2) . . ? C4 C3 C2 119.2(2) . . ? C3 C4 C5 119.5(2) . . ? C4 C5 C6 119.5(2) . . ? N2 C6 C5 120.8(2) . . ? N2 C6 C7 116.59(18) . . ? C5 C6 C7 122.64(19) . . ? N3 C7 C6 117.5(2) . . ? N3 C7 C14 125.8(2) . . ? C6 C7 C14 116.75(19) . . ? C13 C8 C9 119.6(2) . . ? C13 C8 C1 119.3(2) . . ? C9 C8 C1 120.9(2) . . ? C10 C9 C8 119.2(2) . . ? C11 C10 C9 120.8(3) . . ? C10 C11 C12 119.8(2) . . ? C13 C12 C11 119.9(2) . . ? C12 C13 C8 120.6(2) . . ? C19 C14 C15 119.6(2) . . ? C19 C14 C7 122.4(2) . . ? C15 C14 C7 118.0(2) . . ? C14 C15 C16 119.5(3) . . ? C17 C16 C15 120.1(3) . . ? C18 C17 C16 120.5(3) . . ? C17 C18 C19 120.0(3) . . ? C14 C19 C18 120.2(3) . . ? C25 C20 C21 121.64(19) . . ? C25 C20 N1 115.36(16) . . ? C21 C20 N1 122.93(19) . . ? C22 C21 C20 114.1(2) . . ? C22 C21 C26 120.48(17) . . ? C20 C21 C26 125.28(19) . . ? C23 C22 C21 123.80(19) . . ? C22 C23 C24 121.9(2) . . ? C25 C24 C23 115.5(2) . . ? C25 C24 C30 120.48(18) . . ? C23 C24 C30 124.0(2) . . ? C24 C25 C20 122.96(18) . . ? C27 C26 C29 107.1(2) . . ? C27 C26 C28 107.04(18) . . ? C29 C26 C28 109.3(2) . . ? C27 C26 C21 112.2(2) . . ? C29 C26 C21 113.36(16) . . ? C28 C26 C21 107.6(2) . . ? C31 C30 C32 110.1(2) . . ? C31 C30 C33 109.8(2) . . ? C32 C30 C33 107.8(2) . . ? C31 C30 C24 108.4(2) . . ? C32 C30 C24 111.12(19) . . ? C33 C30 C24 109.6(2) . . ? C39 C34 C35 121.54(19) . . ? C39 C34 N3 115.44(19) . . ? C35 C34 N3 122.98(19) . . ? C34 C35 C36 113.7(2) . . ? C34 C35 C40 125.24(19) . . ? C36 C35 C40 121.1(2) . . ? C37 C36 C35 124.1(2) . . ? C36 C37 C38 121.2(2) . . ? C39 C38 C37 116.1(2) . . ? C39 C38 C44 122.5(2) . . ? C37 C38 C44 121.3(2) . . ? C38 C39 C34 123.1(2) . . ? C41 C40 C42 108.4(2) . . ? C41 C40 C35 110.22(18) . . ? C42 C40 C35 111.1(2) . . ? C41 C40 C43 106.8(2) . . ? C42 C40 C43 107.90(19) . . ? C35 C40 C43 112.20(19) . . ? C46 C44 C47 109.4(2) . . ? C46 C44 C45 108.66(19) . . ? C47 C44 C45 109.3(2) . . ? C46 C44 C38 112.19(19) . . ? C47 C44 C38 108.77(18) . . ? C45 C44 C38 108.5(2) . . ? C49 C48 C53 120.0 . . ? C49 C48 C54 120.75(18) . . ? C53 C48 C54 119.25(18) . . ? C50 C49 C48 120.0 . . ? C49 C50 C51 120.0 . . ? C52 C51 C50 120.0 . . ? C51 C52 C53 120.0 . . ? C52 C53 C48 120.0 . . ? 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 C20 N1 C1 C2 -174.21(19) . . . . ? Sn1 N1 C1 C2 -24.6(2) . . . . ? C20 N1 C1 C8 7.3(3) . . . . ? Sn1 N1 C1 C8 156.97(19) . . . . ? C6 N2 C2 C3 0.3(3) . . . . ? Sn1 N2 C2 C3 175.45(16) . . . . ? C6 N2 C2 C1 -177.24(19) . . . . ? Sn1 N2 C2 C1 -2.1(3) . . . . ? N1 C1 C2 N2 19.6(3) . . . . ? C8 C1 C2 N2 -161.8(2) . . . . ? N1 C1 C2 C3 -157.9(2) . . . . ? C8 C1 C2 C3 20.7(3) . . . . ? N2 C2 C3 C4 -1.5(3) . . . . ? C1 C2 C3 C4 176.0(2) . . . . ? C2 C3 C4 C5 1.2(3) . . . . ? C3 C4 C5 C6 0.3(3) . . . . ? C2 N2 C6 C5 1.2(3) . . . . ? Sn1 N2 C6 C5 -173.94(16) . . . . ? C2 N2 C6 C7 -177.65(18) . . . . ? Sn1 N2 C6 C7 7.2(2) . . . . ? C4 C5 C6 N2 -1.5(3) . . . . ? C4 C5 C6 C7 177.3(2) . . . . ? C34 N3 C7 C6 -173.13(17) . . . . ? Sn1 N3 C7 C6 -28.6(2) . . . . ? C34 N3 C7 C14 6.0(3) . . . . ? Sn1 N3 C7 C14 150.54(16) . . . . ? N2 C6 C7 N3 16.9(3) . . . . ? C5 C6 C7 N3 -161.9(2) . . . . ? N2 C6 C7 C14 -162.35(18) . . . . ? C5 C6 C7 C14 18.8(3) . . . . ? N1 C1 C8 C13 -117.0(3) . . . . ? C2 C1 C8 C13 64.6(3) . . . . ? N1 C1 C8 C9 67.3(3) . . . . ? C2 C1 C8 C9 -111.1(2) . . . . ? C13 C8 C9 C10 2.1(4) . . . . ? C1 C8 C9 C10 177.8(2) . . . . ? C8 C9 C10 C11 -1.6(4) . . . . ? C9 C10 C11 C12 1.4(4) . . . . ? C10 C11 C12 C13 -1.7(4) . . . . ? C11 C12 C13 C8 2.2(4) . . . . ? C9 C8 C13 C12 -2.4(4) . . . . ? C1 C8 C13 C12 -178.2(2) . . . . ? N3 C7 C14 C19 62.6(3) . . . . ? C6 C7 C14 C19 -118.3(2) . . . . ? N3 C7 C14 C15 -118.9(3) . . . . ? C6 C7 C14 C15 60.3(3) . . . . ? C19 C14 C15 C16 -3.8(4) . . . . ? C7 C14 C15 C16 177.7(2) . . . . ? C14 C15 C16 C17 3.1(4) . . . . ? C15 C16 C17 C18 -0.8(5) . . . . ? C16 C17 C18 C19 -0.8(4) . . . . ? C15 C14 C19 C18 2.2(4) . . . . ? C7 C14 C19 C18 -179.3(2) . . . . ? C17 C18 C19 C14 0.2(4) . . . . ? C1 N1 C20 C25 60.2(3) . . . . ? Sn1 N1 C20 C25 -86.14(19) . . . . ? C1 N1 C20 C21 -122.5(2) . . . . ? Sn1 N1 C20 C21 91.1(2) . . . . ? C25 C20 C21 C22 -2.8(3) . . . . ? N1 C20 C21 C22 -179.89(19) . . . . ? C25 C20 C21 C26 173.5(2) . . . . ? N1 C20 C21 C26 -3.6(3) . . . . ? C20 C21 C22 C23 1.5(3) . . . . ? C26 C21 C22 C23 -175.0(2) . . . . ? C21 C22 C23 C24 0.3(4) . . . . ? C22 C23 C24 C25 -0.8(3) . . . . ? C22 C23 C24 C30 177.9(2) . . . . ? C23 C24 C25 C20 -0.6(3) . . . . ? C30 C24 C25 C20 -179.3(2) . . . . ? C21 C20 C25 C24 2.5(3) . . . . ? N1 C20 C25 C24 179.79(19) . . . . ? C22 C21 C26 C27 -15.8(3) . . . . ? C20 C21 C26 C27 168.1(2) . . . . ? C22 C21 C26 C29 -137.3(2) . . . . ? C20 C21 C26 C29 46.6(3) . . . . ? C22 C21 C26 C28 101.7(2) . . . . ? C20 C21 C26 C28 -74.3(3) . . . . ? C25 C24 C30 C31 72.4(3) . . . . ? C23 C24 C30 C31 -106.2(3) . . . . ? C25 C24 C30 C32 -166.5(2) . . . . ? C23 C24 C30 C32 14.9(3) . . . . ? C25 C24 C30 C33 -47.4(3) . . . . ? C23 C24 C30 C33 133.9(2) . . . . ? C7 N3 C34 C39 64.1(2) . . . . ? Sn1 N3 C34 C39 -77.5(2) . . . . ? C7 N3 C34 C35 -118.0(2) . . . . ? Sn1 N3 C34 C35 100.35(19) . . . . ? C39 C34 C35 C36 -4.7(3) . . . . ? N3 C34 C35 C36 177.63(18) . . . . ? C39 C34 C35 C40 175.73(19) . . . . ? N3 C34 C35 C40 -2.0(3) . . . . ? C34 C35 C36 C37 3.1(3) . . . . ? C40 C35 C36 C37 -177.2(2) . . . . ? C35 C36 C37 C38 0.6(3) . . . . ? C36 C37 C38 C39 -2.8(3) . . . . ? C36 C37 C38 C44 178.2(2) . . . . ? C37 C38 C39 C34 1.3(3) . . . . ? C44 C38 C39 C34 -179.84(19) . . . . ? C35 C34 C39 C38 2.7(3) . . . . ? N3 C34 C39 C38 -179.45(18) . . . . ? C34 C35 C40 C41 -54.2(3) . . . . ? C36 C35 C40 C41 126.2(2) . . . . ? C34 C35 C40 C42 66.0(3) . . . . ? C36 C35 C40 C42 -113.6(2) . . . . ? C34 C35 C40 C43 -173.1(2) . . . . ? C36 C35 C40 C43 7.3(3) . . . . ? C39 C38 C44 C46 1.0(3) . . . . ? C37 C38 C44 C46 179.9(2) . . . . ? C39 C38 C44 C47 -120.2(2) . . . . ? C37 C38 C44 C47 58.7(3) . . . . ? C39 C38 C44 C45 121.1(2) . . . . ? C37 C38 C44 C45 -60.1(3) . . . . ? C53 C48 C49 C50 0.0 . . . . ? C54 C48 C49 C50 179.2(3) . . . . ? C48 C49 C50 C51 0.0 . . . . ? C49 C50 C51 C52 0.0 . . . . ? C50 C51 C52 C53 0.0 . . . . ? C51 C52 C53 C48 0.0 . . . . ? C49 C48 C53 C52 0.0 . . . . ? C54 C48 C53 C52 -179.2(3) . . . . ? _refine_diff_density_max 1.174 _refine_diff_density_min -0.898 _refine_diff_density_rms 0.083 _shelxl_version_number 2013-3 _shelx_res_file ; TITL dr021 in P2(1)/c CELL 0.71073 18.2152 14.1924 22.1938 90.000 111.582 90.000 ZERR 4.00 0.0005 0.0004 0.0006 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N Cl Sn UNIT 216 252 12 16 8 LIST 0 L.S. 80 DAMP 3000 BOND FMAP 2 PLAN 5 SIZE 0.02 0.08 0.12 TEMP -73.0C ACTA CONF OMIT 2 2 0 OMIT 2 1 4 OMIT -6 2 3 OMIT 3 0 0 OMIT 16 0 2 OMIT 4 2 3 OMIT -4 3 10 OMIT 7 7 8 OMIT -7 3 3 OMIT 0 0 2 OMIT 0 3 2 OMIT -2 2 4 OMIT 4 9 1 OMIT -19 5 2 OMIT 4 2 1 OMIT -10 11 2 OMIT -10 1 25 OMIT 4 6 3 OMIT 5 7 0 OMIT -2 1 3 OMIT 1 13 10 OMIT -8 1 3 OMIT 1 14 7 OMIT -1 2 4 OMIT -2 3 7 OMIT 1 4 1 OMIT -3 2 15 OMIT 1 0 8 OMIT 0 2 4 OMIT -7 2 10 OMIT -3 2 2 OMIT 1 3 5 OMIT -2 2 12 OMIT -8 10 11 OMIT -1 8 18 OMIT -9 10 13 OMIT 10 2 12 OMIT 2 10 10 OMIT -7 9 19 OMIT -9 15 1 OMIT 6 1 10 OMIT -5 8 5 OMIT -17 3 5 OMIT 18 1 3 OMIT 5 11 6 OMIT 1 10 16 OMIT -8 14 13 OMIT -18 6 12 OMIT -18 1 13 OMIT -3 14 12 WGHT 0.051500 5.579400 FVAR 0.06644 SN1 5 0.676809 0.146305 0.350073 11.00000 0.02251 0.03229 = 0.03900 0.00074 0.00774 0.00295 CL1 4 0.699259 0.179303 0.248733 11.00000 0.05614 0.04252 = 0.03506 0.00193 0.01062 0.00198 N1 3 0.698052 -0.027840 0.347842 11.00000 0.02510 0.03112 = 0.03023 -0.00057 0.00856 0.00048 N2 3 0.807665 0.112526 0.387959 11.00000 0.02020 0.02594 = 0.02990 0.00311 0.00820 0.00482 N3 3 0.759799 0.292050 0.388386 11.00000 0.02875 0.02620 = 0.03034 0.00181 0.01414 0.00199 SN2 5 0.824667 0.127029 0.606258 11.00000 0.06184 0.04689 = 0.03633 -0.00374 0.01975 0.00162 CL2 4 0.724996 0.067048 0.503056 11.00000 0.06046 0.05285 = 0.04901 -0.00775 0.01363 -0.00089 CL3 4 0.921028 0.165962 0.556010 11.00000 0.05915 0.07144 = 0.04851 0.01284 0.01918 0.00869 CL4 4 0.879316 -0.030526 0.639613 11.00000 0.08795 0.05603 = 0.05231 0.01265 0.02529 0.01021 C1 1 0.769287 -0.051017 0.384291 11.00000 0.03314 0.02874 = 0.02733 -0.00175 0.01027 0.00328 C2 1 0.831308 0.022256 0.397355 11.00000 0.02520 0.03221 = 0.02666 -0.00265 0.00793 -0.00101 C3 1 0.911098 -0.000648 0.416229 11.00000 0.02987 0.03231 = 0.03758 0.00308 0.00712 0.00841 AFIX 43 H3A 2 0.927847 -0.064405 0.423849 11.00000 -1.20000 AFIX 0 C4 1 0.964810 0.069712 0.423610 11.00000 0.02077 0.03812 = 0.05183 0.00027 0.01202 0.00404 AFIX 43 H4A 2 1.019262 0.055218 0.435661 11.00000 -1.20000 AFIX 0 C5 1 0.939576 0.161668 0.413491 11.00000 0.02594 0.04053 = 0.04494 0.00230 0.01428 -0.00545 AFIX 43 H5A 2 0.976412 0.211171 0.418303 11.00000 -1.20000 AFIX 0 C6 1 0.860082 0.181579 0.396235 11.00000 0.02876 0.02789 = 0.03060 -0.00132 0.01330 -0.00175 C7 1 0.828729 0.279338 0.387278 11.00000 0.03173 0.03124 = 0.02418 -0.00303 0.01032 -0.00276 C8 1 0.795706 -0.145878 0.413484 11.00000 0.02570 0.02614 = 0.04108 -0.00179 0.00704 -0.00362 C9 1 0.795083 -0.222813 0.374908 11.00000 0.04493 0.04029 = 0.04647 -0.00590 -0.00018 0.00425 AFIX 43 H9A 2 0.776002 -0.216666 0.329089 11.00000 -1.20000 AFIX 0 C10 1 0.822625 -0.308872 0.403937 11.00000 0.06429 0.02791 = 0.07561 -0.00485 0.00467 0.00489 AFIX 43 H10A 2 0.821086 -0.362255 0.377674 11.00000 -1.20000 AFIX 0 C11 1 0.851956 -0.317907 0.469832 11.00000 0.04660 0.03685 = 0.08552 0.02409 0.01181 0.00607 AFIX 43 H11A 2 0.871778 -0.376902 0.489237 11.00000 -1.20000 AFIX 0 C12 1 0.852688 -0.240717 0.508259 11.00000 0.03910 0.05735 = 0.05044 0.01746 0.01366 0.00298 AFIX 43 H12A 2 0.871692 -0.247104 0.554061 11.00000 -1.20000 AFIX 0 C13 1 0.826050 -0.155383 0.480219 11.00000 0.03468 0.03845 = 0.04182 0.00410 0.01202 0.00358 AFIX 43 H13A 2 0.828383 -0.102105 0.506775 11.00000 -1.20000 AFIX 0 C14 1 0.880768 0.354354 0.376827 11.00000 0.02953 0.03194 = 0.04021 0.00838 0.01266 -0.00078 C15 1 0.902396 0.346343 0.323799 11.00000 0.07222 0.10636 = 0.04583 -0.00555 0.03078 -0.03881 AFIX 43 H15A 2 0.886135 0.293323 0.295898 11.00000 -1.20000 AFIX 0 C16 1 0.948393 0.416721 0.311359 11.00000 0.08737 0.13378 = 0.06952 0.01269 0.04132 -0.04329 AFIX 43 H16A 2 0.961370 0.413266 0.273692 11.00000 -1.20000 AFIX 0 C17 1 0.974848 0.490714 0.353314 11.00000 0.06742 0.06154 = 0.12914 0.02857 0.04836 -0.01599 AFIX 43 H17A 2 1.006701 0.538021 0.344872 11.00000 -1.20000 AFIX 0 C18 1 0.956125 0.497014 0.406399 11.00000 0.06475 0.05075 = 0.13690 -0.02638 0.05765 -0.02127 AFIX 43 H18A 2 0.975313 0.548163 0.435599 11.00000 -1.20000 AFIX 0 C19 1 0.908370 0.428196 0.418605 11.00000 0.06377 0.05073 = 0.09314 -0.01894 0.05487 -0.02460 AFIX 43 H19A 2 0.895079 0.432812 0.456073 11.00000 -1.20000 AFIX 0 C20 1 0.634741 -0.094921 0.339127 11.00000 0.01991 0.02221 = 0.03293 -0.00032 0.00613 -0.00044 C21 1 0.585296 -0.128154 0.277958 11.00000 0.02443 0.02660 = 0.03666 -0.00268 0.01004 0.00212 C22 1 0.528024 -0.192081 0.279908 11.00000 0.03285 0.03972 = 0.03212 -0.00870 0.00846 -0.00527 AFIX 43 H22A 2 0.493595 -0.218236 0.240153 11.00000 -1.20000 AFIX 0 C23 1 0.518532 -0.219387 0.335951 11.00000 0.03248 0.03358 = 0.04601 -0.00461 0.01393 -0.00948 AFIX 43 H23A 2 0.478336 -0.263533 0.333520 11.00000 -1.20000 AFIX 0 C24 1 0.565950 -0.184353 0.395975 11.00000 0.03446 0.03289 = 0.03279 -0.00097 0.01342 0.00015 C25 1 0.623678 -0.121441 0.395506 11.00000 0.02654 0.02858 = 0.03018 -0.00492 0.00473 0.00122 AFIX 43 H25A 2 0.657305 -0.095143 0.435504 11.00000 -1.20000 AFIX 0 C26 1 0.587641 -0.095124 0.212560 11.00000 0.03298 0.04034 = 0.02887 -0.00073 0.00805 0.00025 C27 1 0.538666 -0.158680 0.156331 11.00000 0.07109 0.07374 = 0.02524 -0.00978 0.01366 -0.01585 AFIX 33 H27A 2 0.560417 -0.222658 0.163528 11.00000 -1.50000 H27B 2 0.540418 -0.133982 0.115646 11.00000 -1.50000 H27C 2 0.483839 -0.160048 0.153856 11.00000 -1.50000 AFIX 0 C28 1 0.550539 0.003738 0.198735 11.00000 0.04628 0.05941 = 0.04507 0.00685 0.01039 0.00940 AFIX 33 H28A 2 0.496944 0.001403 0.199122 11.00000 -1.50000 H28B 2 0.548440 0.025130 0.156147 11.00000 -1.50000 H28C 2 0.582601 0.047654 0.232128 11.00000 -1.50000 AFIX 0 C29 1 0.671408 -0.091178 0.211586 11.00000 0.04552 0.05136 = 0.04040 0.00731 0.01916 0.01013 AFIX 33 H29A 2 0.695160 -0.154098 0.220257 11.00000 -1.50000 H29B 2 0.703548 -0.047257 0.244938 11.00000 -1.50000 H29C 2 0.668997 -0.069658 0.168942 11.00000 -1.50000 AFIX 0 C30 1 0.556124 -0.210024 0.459817 11.00000 0.04306 0.04537 = 0.03750 -0.00211 0.01615 -0.00508 C31 1 0.520472 -0.126775 0.481340 11.00000 0.10582 0.09130 = 0.05998 0.00432 0.05151 0.03383 AFIX 33 H31A 2 0.554829 -0.071756 0.486773 11.00000 -1.50000 H31B 2 0.515070 -0.141429 0.522662 11.00000 -1.50000 H31C 2 0.468348 -0.113040 0.448571 11.00000 -1.50000 AFIX 0 C32 1 0.503768 -0.295913 0.451533 11.00000 0.08450 0.08455 = 0.05859 0.00062 0.04028 -0.03412 AFIX 33 H32A 2 0.498679 -0.310940 0.492920 11.00000 -1.50000 H32B 2 0.527344 -0.349559 0.437457 11.00000 -1.50000 H32C 2 0.451451 -0.282738 0.418870 11.00000 -1.50000 AFIX 0 C33 1 0.636643 -0.233173 0.511351 11.00000 0.06739 0.07591 = 0.04485 0.01655 0.01569 -0.00204 AFIX 33 H33A 2 0.671788 -0.178757 0.517548 11.00000 -1.50000 H33B 2 0.659443 -0.287514 0.497272 11.00000 -1.50000 H33C 2 0.630357 -0.248100 0.552298 11.00000 -1.50000 AFIX 0 C34 1 0.722164 0.383509 0.372844 11.00000 0.02592 0.02859 = 0.03544 0.00168 0.01245 -0.00178 C35 1 0.700972 0.437027 0.417311 11.00000 0.02782 0.03007 = 0.03634 -0.00207 0.01078 0.00238 C36 1 0.668001 0.525276 0.393157 11.00000 0.03847 0.03426 = 0.04349 -0.00472 0.01515 0.00504 AFIX 43 H36A 2 0.654882 0.566255 0.421528 11.00000 -1.20000 AFIX 0 C37 1 0.653633 0.555805 0.331318 11.00000 0.03579 0.03236 = 0.03819 0.00190 0.01123 0.00305 AFIX 43 H37A 2 0.631662 0.616635 0.318525 11.00000 -1.20000 AFIX 0 C38 1 0.670609 0.499425 0.287003 11.00000 0.02820 0.03545 = 0.04077 0.00227 0.01681 -0.00719 C39 1 0.705534 0.414204 0.309770 11.00000 0.03266 0.02521 = 0.03582 -0.00204 0.01642 -0.00061 AFIX 43 H39A 2 0.718961 0.374343 0.280998 11.00000 -1.20000 AFIX 0 C40 1 0.711897 0.406010 0.486366 11.00000 0.04241 0.03755 = 0.03386 0.00124 0.01577 0.00809 C41 1 0.673012 0.310539 0.484942 11.00000 0.07041 0.06299 = 0.04603 0.00468 0.03137 -0.00495 AFIX 33 H41A 2 0.696648 0.263797 0.465040 11.00000 -1.50000 H41B 2 0.616316 0.315367 0.459582 11.00000 -1.50000 H41C 2 0.681065 0.291055 0.529287 11.00000 -1.50000 AFIX 0 C42 1 0.799730 0.397721 0.528986 11.00000 0.05040 0.06615 = 0.03902 0.00033 0.01459 0.00385 AFIX 33 H42A 2 0.825648 0.458661 0.530496 11.00000 -1.50000 H42B 2 0.824566 0.350075 0.510751 11.00000 -1.50000 H42C 2 0.805067 0.379133 0.572928 11.00000 -1.50000 AFIX 0 C43 1 0.673755 0.475087 0.519348 11.00000 0.08973 0.07237 = 0.04919 0.00560 0.03878 0.02970 AFIX 33 H43A 2 0.697500 0.537578 0.521569 11.00000 -1.50000 H43B 2 0.682476 0.452928 0.563269 11.00000 -1.50000 H43C 2 0.616923 0.478881 0.494275 11.00000 -1.50000 AFIX 0 C44 1 0.652312 0.532423 0.216692 11.00000 0.05046 0.03202 = 0.03940 0.00400 0.01785 -0.00242 C45 1 0.563283 0.550199 0.184622 11.00000 0.05460 0.05608 = 0.03692 0.01103 0.01014 0.00313 AFIX 33 H45A 2 0.550732 0.571314 0.139898 11.00000 -1.50000 H45B 2 0.547598 0.598871 0.208831 11.00000 -1.50000 H45C 2 0.534615 0.491774 0.184641 11.00000 -1.50000 AFIX 0 C46 1 0.675588 0.460768 0.177651 11.00000 0.08944 0.06668 = 0.04003 0.01362 0.03202 0.01580 AFIX 33 H46A 2 0.662804 0.484413 0.133469 11.00000 -1.50000 H46B 2 0.646749 0.402022 0.176302 11.00000 -1.50000 H46C 2 0.732468 0.448898 0.197591 11.00000 -1.50000 AFIX 0 C47 1 0.696800 0.624619 0.218146 11.00000 0.06875 0.06638 = 0.05302 0.01651 0.01841 -0.02667 AFIX 33 H47A 2 0.685445 0.646367 0.173715 11.00000 -1.50000 H47B 2 0.753669 0.613883 0.239664 11.00000 -1.50000 H47C 2 0.679723 0.672538 0.241990 11.00000 -1.50000 AFIX 66 C48 1 0.881202 0.938916 0.230615 11.00000 0.08885 C49 1 0.836740 0.890797 0.174481 11.00000 0.10972 AFIX 43 H49A 2 0.804420 0.924751 0.137294 11.00000 -1.20000 AFIX 65 C50 1 0.839569 0.792999 0.172757 11.00000 0.09824 AFIX 43 H50A 2 0.809181 0.760112 0.134392 11.00000 -1.20000 AFIX 65 C51 1 0.886857 0.743319 0.227166 11.00000 0.12915 AFIX 43 H51A 2 0.888790 0.676478 0.225987 11.00000 -1.20000 AFIX 65 C52 1 0.931319 0.791437 0.283300 11.00000 0.11959 AFIX 43 H52A 2 0.963638 0.757482 0.320487 11.00000 -1.20000 AFIX 65 C53 1 0.928492 0.889234 0.285025 11.00000 0.07106 AFIX 43 H53A 2 0.958880 0.922121 0.323390 11.00000 -1.20000 AFIX 0 C54 1 0.879743 1.040239 0.233010 11.00000 0.13043 AFIX 33 H54A 2 0.844271 1.064689 0.191117 11.00000 -1.50000 H54B 2 0.933105 1.064830 0.242490 11.00000 -1.50000 H54C 2 0.860861 1.060175 0.267054 11.00000 -1.50000 AFIX 0 HKLF 4 REM dr021 in P2(1)/c REM R1 = 0.0463 for 6399 Fo > 4sig(Fo) and 0.0811 for all 9053 data REM 521 parameters refined using 0 restraints END WGHT 0.0518 5.4652 REM Highest difference peak 1.174, deepest hole -0.898, 1-sigma level 0.083 Q1 1 0.8385 0.9529 0.1789 11.00000 0.05 1.17 Q2 1 0.8271 0.8500 0.1601 11.00000 0.05 1.08 Q3 1 0.9023 0.8042 0.2470 11.00000 0.05 0.72 Q4 1 0.9373 0.7023 0.2796 11.00000 0.05 0.68 Q5 1 0.8692 0.1775 0.6399 11.00000 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4.11 0.99 2 5 0 5.02 1.03 -2 5 0 5.28 1.18 -2 5 0 4.35 1.86 2 5 0 5.00 1.01 2 5 0 5.69 0.96 2 5 0 4.80 0.99 -2 5 0 5.95 0.99 -2 5 0 6.40 1.12 -3 -5 0 11.86 1.76 3 -5 0 11.62 1.06 3 -5 0 10.38 1.16 3 -5 0 9.46 1.07 -3 -5 0 11.92 1.46 3 -5 0 11.21 1.44 -3 -5 0 11.57 1.06 3 -5 0 12.61 1.47 -3 -5 0 9.77 1.05 3 -5 0 10.99 1.12 3 5 0 11.87 1.15 3 5 0 11.68 1.93 -3 5 0 9.45 1.02 -3 5 0 12.75 2.01 -3 5 0 9.78 1.15 3 5 0 13.04 1.77 -3 5 0 12.24 1.11 -3 5 0 9.09 1.07 3 5 0 9.45 1.00 -3 5 0 11.51 1.13 3 5 0 10.81 1.07 3 5 0 12.18 1.29 3 5 0 11.38 1.28 -4 -5 0 58.94 1.85 4 -5 0 61.81 2.22 4 -5 0 60.05 2.00 4 -5 0 62.62 2.02 -4 -5 0 60.79 2.03 4 -5 0 62.18 2.05 -4 -5 0 59.53 3.07 4 -5 0 59.73 1.97 -4 -5 0 62.06 2.07 4 -5 0 59.95 1.98 -4 5 0 61.45 2.08 -4 5 0 60.98 2.13 4 5 0 56.46 2.58 -4 5 0 56.13 3.56 4 5 0 60.21 1.99 4 5 0 63.75 1.87 -4 5 0 61.48 2.14 4 5 0 57.81 1.91 4 5 0 64.25 1.97 -4 5 0 57.40 2.16 4 5 0 61.09 3.06 -5 -5 0 187.72 4.19 -5 -5 0 191.11 4.63 5 -5 0 191.41 4.18 5 -5 0 189.94 4.31 5 -5 0 189.23 4.27 5 -5 0 191.35 4.55 -5 -5 0 193.59 6.56 5 -5 0 189.42 4.54 5 -5 0 196.33 4.22 5 5 0 188.81 4.05 5 5 0 190.57 6.59 -5 5 0 189.97 4.28 -5 5 0 195.34 4.25 5 5 0 187.15 4.22 5 5 0 191.78 4.05 5 5 0 186.73 5.92 -5 5 0 195.44 4.76 5 5 0 194.14 4.20 -5 5 0 219.60 6.80 -5 5 0 188.42 4.72 6 -5 0 6.43 1.21 6 -5 0 6.59 1.11 6 -5 0 6.14 1.23 -6 -5 0 9.35 1.79 -6 -5 0 6.26 0.91 6 -5 0 5.67 1.05 -6 -5 0 6.07 1.04 -6 5 0 4.60 1.15 -6 5 0 5.84 1.14 -6 5 0 5.40 1.03 6 5 0 8.68 1.43 6 5 0 6.78 0.86 -6 5 0 5.65 1.15 6 5 0 4.58 0.88 6 5 0 5.85 1.17 6 5 0 5.43 1.04 -7 -5 0 87.31 2.52 7 -5 0 93.33 2.65 7 -5 0 92.74 2.59 -7 -5 0 93.20 3.92 7 -5 0 94.57 2.47 7 -5 0 95.81 2.61 -7 5 0 93.60 2.74 7 5 0 93.49 2.50 7 5 0 92.19 2.23 7 5 0 95.08 2.53 7 5 0 94.80 2.26 -7 5 0 95.33 2.79 -7 5 0 93.09 2.69 8 -5 0 38.13 2.07 8 -5 0 31.71 1.49 8 -5 0 40.20 1.78 8 -5 0 37.06 2.12 -8 -5 0 39.30 2.79 -8 -5 0 38.49 1.75 8 5 0 39.23 1.84 -8 5 0 42.10 1.93 8 5 0 38.58 1.71 -8 5 0 40.30 1.79 8 5 0 40.34 1.20 -8 5 0 37.80 2.05 8 5 0 39.19 1.19 9 -5 0 34.36 1.77 9 -5 0 28.95 2.16 -9 -5 0 32.60 2.77 9 -5 0 31.11 1.64 -9 -5 0 28.96 1.71 9 -5 0 29.91 2.05 9 5 0 33.67 1.78 -9 5 0 29.80 1.76 -9 5 0 31.32 1.89 9 5 0 29.45 1.76 -9 5 0 31.75 2.05 10 -5 0 32.26 1.62 10 -5 0 36.82 2.30 10 -5 0 33.58 1.67 -10 -5 0 34.74 1.86 -10 -5 0 34.46 3.17 10 -5 0 37.25 2.21 -10 5 0 36.62 1.93 10 5 0 32.27 1.79 -10 5 0 35.30 2.20 -10 5 0 33.36 2.02 10 5 0 38.63 1.94 -11 -5 0 14.41 1.31 11 -5 0 13.80 1.26 11 -5 0 14.24 1.30 11 -5 0 14.23 1.66 -11 -5 0 17.71 2.36 11 -5 0 13.61 2.46 11 -5 0 14.42 1.62 11 5 0 13.05 1.34 11 5 0 13.41 1.31 -11 5 0 15.20 1.88 -11 5 0 19.34 1.78 -11 5 0 14.78 1.52 12 -5 0 9.78 2.60 -12 -5 0 13.99 2.43 12 -5 0 13.21 1.66 -12 -5 0 12.17 1.34 12 -5 0 10.76 1.61 12 5 0 14.51 1.35 12 5 0 16.33 1.72 -12 5 0 12.16 1.31 -12 5 0 12.56 1.36 -12 5 0 10.69 1.62 13 -5 0 28.48 2.26 13 -5 0 28.73 3.91 13 -5 0 35.56 2.49 -13 5 0 31.53 2.04 13 5 0 30.19 1.85 -13 5 0 32.84 2.12 13 5 0 31.15 1.74 14 -5 0 1.65 1.50 14 -5 0 -0.53 1.45 14 -5 0 0.15 2.21 14 5 0 0.31 0.99 14 5 0 1.89 1.09 -14 5 0 2.90 1.22 -14 5 0 0.88 1.16 15 -5 0 23.53 1.88 15 -5 0 25.06 2.17 15 -5 0 20.62 2.84 15 5 0 21.48 1.37 -15 5 0 27.40 1.87 15 5 0 20.34 1.39 16 -5 0 5.79 1.51 16 -5 0 5.80 1.52 16 -5 0 8.15 2.79 16 5 0 4.88 0.87 16 5 0 5.21 0.88 -16 5 0 -4.51 3.90 17 -5 0 0.21 1.41 17 -5 0 0.21 2.65 17 -5 0 2.53 1.45 -17 5 0 4.51 3.78 18 -5 0 3.48 1.37 18 -5 0 3.79 2.72 18 -5 0 0.89 1.37 19 -5 0 10.48 1.39 19 -5 0 6.64 1.35 19 -5 0 6.33 2.88 0 -6 0 146.23 3.50 0 -6 0 144.09 3.75 0 -6 0 140.62 3.79 0 -6 0 142.54 3.60 0 -6 0 141.65 3.44 0 6 0 143.23 3.52 0 6 0 144.59 3.40 0 6 0 137.07 3.33 0 6 0 143.90 5.22 0 6 0 136.57 3.75 1 -6 0 0.42 1.21 1 -6 0 -1.95 1.14 -1 -6 0 -1.60 1.09 1 -6 0 -0.05 1.06 1 -6 0 0.26 1.08 -1 -6 0 -0.08 1.08 -1 -6 0 0.19 1.04 1 -6 0 1.61 1.13 -1 -6 0 0.56 1.10 -1 6 0 1.34 1.02 -1 6 0 0.36 1.15 -1 6 0 1.60 1.13 1 6 0 -0.45 1.09 1 6 0 -2.46 1.18 1 6 0 -0.20 0.50 1 6 0 1.45 1.07 -1 6 0 -0.14 1.21 1 6 0 -0.03 1.10 1 6 0 1.21 1.96 -1 6 0 -0.75 1.87 2 -6 0 2.02 1.10 2 -6 0 -0.62 1.09 -2 -6 0 0.08 1.06 2 -6 0 0.90 1.15 -2 -6 0 -0.58 1.02 -2 -6 0 -0.52 1.73 2 -6 0 3.59 1.13 -2 -6 0 0.98 1.10 -2 -6 0 -1.51 1.09 2 -6 0 1.15 1.20 -2 6 0 0.15 1.05 2 6 0 1.03 1.01 2 6 0 0.97 1.05 2 6 0 0.28 1.87 2 6 0 -0.53 1.07 -2 6 0 -1.21 1.12 2 6 0 0.62 1.03 -2 6 0 0.60 2.20 -2 6 0 1.37 1.12 2 6 0 -1.97 1.11 -2 6 0 1.98 1.20 3 -6 0 9.19 1.29 3 -6 0 8.43 1.18 -3 -6 0 6.46 1.14 3 -6 0 7.67 0.97 3 -6 0 8.01 1.12 3 -6 0 7.57 1.20 -3 -6 0 10.89 1.19 3 -6 0 9.56 1.26 -3 -6 0 13.10 2.36 -3 -6 0 7.30 1.15 3 6 0 10.25 1.19 3 6 0 8.49 2.08 -3 6 0 9.39 1.21 -3 6 0 7.91 1.30 3 6 0 9.90 1.14 3 6 0 8.55 1.28 -3 6 0 8.78 1.28 -3 6 0 8.20 2.12 -3 6 0 9.12 1.24 3 6 0 7.38 1.21 3 6 0 8.45 1.02 4 -6 0 20.76 1.71 -4 -6 0 20.56 1.75 -4 -6 0 20.46 2.43 4 -6 0 30.64 1.67 4 -6 0 20.36 1.84 4 -6 0 21.38 1.68 -4 -6 0 21.96 1.66 -4 -6 0 20.04 1.61 4 -6 0 21.65 1.76 4 -6 0 20.15 2.07 -4 6 0 19.94 1.97 -4 6 0 18.50 1.89 4 6 0 17.66 1.76 4 6 0 17.88 1.37 -4 6 0 20.33 1.78 -4 6 0 21.51 1.84 4 6 0 20.03 1.70 4 6 0 19.62 2.76 4 6 0 19.04 1.57 5 -6 0 73.05 2.41 -5 -6 0 70.56 2.30 5 -6 0 76.64 2.34 5 -6 0 70.96 2.26 -5 -6 0 73.70 3.57 5 -6 0 73.60 2.31 5 -6 0 74.41 2.48 -5 -6 0 70.58 2.39 5 -6 0 72.09 2.60 5 6 0 72.21 2.15 5 6 0 72.55 2.29 -5 6 0 73.54 2.57 5 6 0 67.23 2.98 5 6 0 78.09 2.42 -5 6 0 65.50 3.86 5 6 0 70.60 3.60 5 6 0 72.13 2.23 -5 6 0 70.13 2.23 -5 6 0 73.00 2.52 -5 6 0 75.09 2.52 -6 -6 0 55.11 3.13 -6 -6 0 51.04 1.99 6 -6 0 52.57 2.19 6 -6 0 56.87 2.26 6 -6 0 52.71 1.76 6 -6 0 52.77 1.76 -6 -6 0 52.82 2.04 6 -6 0 56.76 2.05 6 -6 0 54.22 2.37 6 6 0 55.31 2.26 -6 6 0 46.09 3.54 6 6 0 54.13 3.18 6 6 0 54.46 2.02 -6 6 0 54.82 2.23 -6 6 0 53.16 2.22 6 6 0 56.12 1.89 -6 6 0 52.86 2.29 -6 6 0 49.73 2.20 6 6 0 52.26 2.40 7 -6 0 2.23 1.29 7 -6 0 2.97 1.17 -7 -6 0 2.73 1.90 -7 -6 0 1.91 1.02 7 -6 0 1.53 1.35 -7 -6 0 2.89 1.17 7 -6 0 1.77 1.39 -7 6 0 1.30 1.15 7 6 0 0.83 0.94 7 6 0 0.59 1.24 7 6 0 1.22 1.22 -7 6 0 2.94 1.34 7 6 0 1.60 0.97 -7 6 0 2.08 2.70 7 6 0 3.24 1.15 -7 6 0 0.96 1.28 8 -6 0 75.57 2.37 8 -6 0 77.37 2.67 -8 -6 0 71.89 3.72 -8 -6 0 73.95 2.38 8 -6 0 74.17 2.57 8 -6 0 75.50 2.58 -8 -6 0 75.71 2.36 8 6 0 78.66 2.44 8 6 0 76.69 2.07 -8 6 0 62.21 4.10 8 6 0 71.28 2.44 -8 6 0 72.87 2.54 -8 6 0 75.15 2.71 -8 6 0 73.71 2.58 8 6 0 74.56 2.05 9 -6 0 33.68 2.14 -9 -6 0 35.23 3.16 9 -6 0 34.70 2.60 9 -6 0 35.91 2.04 -9 -6 0 34.07 1.81 -9 -6 0 40.08 2.10 9 6 0 35.56 2.02 9 6 0 34.75 1.31 -9 6 0 39.89 2.30 -9 6 0 35.82 3.68 -9 6 0 35.45 2.11 9 6 0 37.92 2.20 -9 6 0 37.89 2.46 9 6 0 33.88 1.31 -10 -6 0 1.15 1.30 -10 -6 0 2.64 2.13 10 -6 0 -1.64 1.66 10 -6 0 3.44 1.73 10 -6 0 1.60 1.18 10 -6 0 2.02 1.29 -10 6 0 -1.33 3.32 -10 6 0 1.92 1.33 -10 6 0 3.22 1.57 10 6 0 0.37 1.43 10 6 0 2.97 1.44 -10 6 0 -0.99 1.46 11 -6 0 23.74 1.80 11 -6 0 25.22 2.59 11 -6 0 22.63 1.76 11 -6 0 23.40 2.43 -11 -6 0 28.49 2.21 -11 6 0 19.74 2.29 -11 6 0 26.27 2.15 11 6 0 21.49 2.10 11 6 0 24.01 1.99 -11 6 0 22.61 2.52 -11 6 0 23.16 3.85 12 -6 0 21.42 1.57 12 -6 0 21.26 1.54 12 -6 0 33.26 3.95 12 -6 0 26.59 2.33 12 -6 0 23.43 2.61 -12 6 0 24.75 2.23 -12 6 0 24.61 4.00 -12 6 0 20.71 1.85 -12 6 0 23.91 2.36 12 6 0 20.51 1.97 12 6 0 24.35 2.07 13 -6 0 12.68 1.70 13 -6 0 8.78 2.64 13 -6 0 13.94 1.77 -13 6 0 14.94 1.64 -13 6 0 14.51 1.52 -13 6 0 11.43 3.86 13 6 0 14.43 1.45 13 6 0 17.97 1.77 14 -6 0 21.84 2.19 14 -6 0 22.72 2.42 14 -6 0 13.68 2.69 -14 6 0 22.70 2.21 14 6 0 21.28 1.60 14 6 0 20.61 1.79 -14 6 0 16.49 3.93 15 -6 0 4.67 1.56 15 -6 0 3.58 2.58 15 -6 0 2.39 1.62 -15 6 0 4.99 1.48 15 6 0 2.00 1.09 -15 6 0 9.18 3.73 15 6 0 2.79 1.17 16 -6 0 8.61 1.64 16 -6 0 8.20 1.63 16 -6 0 6.62 2.82 16 6 0 5.19 1.09 16 6 0 7.13 1.12 -16 6 0 17.44 4.21 17 -6 0 11.31 2.90 17 -6 0 6.47 1.59 17 -6 0 5.96 1.62 17 6 0 5.86 0.99 17 6 0 4.76 1.03 18 -6 0 -1.06 1.48 18 -6 0 2.15 1.49 18 -6 0 1.54 2.81 0 -7 0 -2.87 1.23 0 -7 0 0.68 1.28 0 -7 0 0.54 1.40 0 -7 0 -2.31 1.27 0 -7 0 1.81 1.45 0 7 0 -0.16 1.29 0 7 0 -0.19 1.18 0 7 0 0.75 1.27 0 7 0 -3.99 1.39 0 7 0 -0.58 2.13 -1 -7 0 2.89 1.35 1 -7 0 2.85 1.32 1 -7 0 3.76 1.35 -1 -7 0 5.29 1.42 1 -7 0 3.49 1.29 -1 -7 0 3.89 1.41 -1 -7 0 2.65 1.20 1 -7 0 1.72 1.34 1 -7 0 2.00 1.25 -1 7 0 3.99 1.37 -1 7 0 3.53 1.34 1 7 0 0.85 1.09 1 7 0 2.43 2.10 1 7 0 2.72 1.27 -1 7 0 1.88 2.40 1 7 0 3.70 1.32 1 7 0 2.31 1.27 -1 7 0 4.03 1.35 -1 7 0 2.90 1.23 -2 -7 0 45.62 2.19 -2 -7 0 45.80 2.22 2 -7 0 47.63 2.25 2 -7 0 49.59 2.07 2 -7 0 45.52 2.52 2 -7 0 46.74 2.24 -2 -7 0 48.90 2.03 2 -7 0 49.84 2.06 -2 7 0 47.10 2.29 2 7 0 43.75 1.97 2 7 0 49.99 3.46 -2 7 0 49.18 2.28 -2 7 0 41.24 3.79 2 7 0 48.20 2.10 2 7 0 38.75 2.33 -2 7 0 47.51 2.15 2 7 0 44.26 2.15 -2 7 0 44.40 2.29 3 -7 0 11.64 1.44 -3 -7 0 11.22 1.36 3 -7 0 13.53 1.52 3 -7 0 13.15 1.39 3 -7 0 9.58 1.32 -3 -7 0 11.20 1.39 -3 -7 0 14.40 1.90 3 7 0 10.67 1.39 3 7 0 12.79 1.29 3 7 0 12.21 1.22 -3 7 0 12.11 1.48 -3 7 0 14.12 1.44 -3 7 0 14.20 1.52 3 7 0 12.11 1.49 3 7 0 11.96 2.26 -3 7 0 14.94 2.55 3 7 0 10.27 1.31 -3 7 0 8.81 1.42 4 -7 0 118.79 3.27 -4 -7 0 120.51 3.12 4 -7 0 121.57 3.45 4 -7 0 122.34 3.41 -4 -7 0 116.91 3.18 -4 -7 0 119.77 3.44 4 -7 0 119.19 3.42 4 -7 0 115.03 3.12 4 7 0 125.97 3.23 4 7 0 119.68 3.05 -4 7 0 118.87 3.56 -4 7 0 115.94 5.07 4 7 0 117.26 4.85 -4 7 0 122.01 3.29 4 7 0 115.47 3.03 4 7 0 119.29 3.19 4 7 0 125.51 3.29 -4 7 0 119.32 3.37 5 -7 0 3.51 1.15 5 -7 0 3.86 1.15 -5 -7 0 4.90 1.25 5 -7 0 2.13 1.41 5 -7 0 3.80 1.43 5 -7 0 2.46 1.51 -5 -7 0 2.99 1.27 5 -7 0 3.31 1.26 -5 7 0 2.84 1.30 5 7 0 3.56 1.21 -5 7 0 1.60 1.41 5 7 0 1.45 2.03 -5 7 0 3.18 2.75 5 7 0 0.28 1.37 -5 7 0 2.74 1.40 5 7 0 2.28 1.19 5 7 0 4.09 1.30 -5 7 0 0.96 1.37 -6 -7 0 0.13 1.23 6 -7 0 -0.43 1.04 6 -7 0 -0.50 1.02 6 -7 0 -2.18 1.47 -6 -7 0 0.26 1.20 6 -7 0 1.19 1.49 6 -7 0 -0.74 1.44 6 -7 0 0.12 1.26 -6 7 0 1.69 1.36 -6 7 0 -0.12 1.43 6 7 0 0.09 1.18 6 7 0 1.19 1.37 -6 7 0 0.74 1.31 -6 7 0 -0.59 2.91 6 7 0 0.69 1.40 6 7 0 -0.27 1.11 6 7 0 0.90 1.67 6 7 0 1.86 2.18 -6 7 0 -1.45 1.42 7 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-8 -4 4 82.41 3.51 8 -4 -4 84.25 2.30 8 -4 -4 85.18 2.39 -8 -4 4 81.06 2.21 8 -4 -4 84.21 2.38 8 4 -4 83.36 2.22 -8 4 4 85.76 2.48 -8 4 4 81.90 4.37 8 4 -4 88.09 1.99 -8 4 4 84.72 2.48 -8 4 4 87.23 2.45 8 4 -4 83.80 2.06 8 4 -4 84.91 2.33 7 -4 -4 9.74 1.16 -7 -4 4 10.59 0.93 7 -4 -4 9.98 1.02 7 -4 -4 9.46 1.02 -7 -4 4 8.67 1.34 -7 -4 4 10.14 1.67 7 4 -4 8.43 1.08 7 4 -4 8.08 1.36 -7 4 4 10.24 1.01 -7 4 4 9.34 1.13 7 4 -4 8.20 0.87 -7 4 4 11.99 2.20 -7 4 4 10.17 1.12 7 4 -4 9.84 0.80 -6 -4 4 149.18 3.88 6 -4 -4 157.27 3.48 6 -4 -4 156.15 3.55 -6 -4 4 150.03 4.57 -6 -4 4 152.75 3.43 6 -4 -4 162.50 3.53 -6 -4 4 155.97 3.43 6 -4 -4 154.22 3.63 6 -4 -4 158.59 3.49 -6 -4 4 151.25 5.13 -6 4 4 155.61 5.72 -6 4 4 154.92 3.86 6 4 -4 153.93 3.38 6 4 -4 152.43 3.45 6 4 -4 146.87 5.01 -6 4 4 148.44 3.47 -6 4 4 155.85 3.46 6 4 -4 158.29 3.48 5 -4 -4 4.03 0.83 5 -4 -4 3.56 1.03 -5 -4 4 2.95 0.87 5 -4 -4 4.00 1.83 5 -4 -4 3.37 0.80 -5 -4 4 2.57 1.67 -5 -4 4 3.03 0.95 5 -4 -4 4.40 0.95 -5 -4 4 2.34 0.86 5 -4 -4 2.26 0.93 5 -4 -4 2.53 1.03 -5 4 4 4.22 1.01 -5 4 4 3.50 0.95 5 4 -4 1.91 0.88 -5 4 4 1.46 0.98 5 4 -4 4.30 0.96 -5 4 4 4.09 2.00 5 4 -4 1.96 0.92 5 4 -4 3.31 0.80 5 4 -4 2.05 1.19 4 -4 -4 49.02 1.78 4 -4 -4 48.70 1.79 4 -4 -4 48.86 1.83 -4 -4 4 49.78 1.78 4 -4 -4 48.60 2.83 4 -4 -4 50.42 1.93 4 -4 -4 49.08 1.82 -4 -4 4 51.26 1.77 -4 -4 4 51.14 1.93 -4 -4 4 51.92 2.86 -4 -4 4 51.27 1.83 -4 4 4 44.42 1.89 4 4 -4 48.66 1.66 4 4 -4 49.60 1.76 -4 4 4 48.39 3.17 4 4 -4 49.38 1.89 4 4 -4 45.65 2.46 4 4 -4 50.48 1.69 -4 4 4 49.70 1.80 -4 4 4 50.41 1.71 -4 4 4 48.20 1.90 -3 -4 4 7.57 1.07 3 -4 -4 7.01 1.01 -3 -4 4 7.83 0.94 3 -4 -4 8.62 1.04 3 -4 -4 7.29 1.09 -3 -4 4 8.98 1.06 -3 -4 4 7.39 1.02 -3 -4 4 6.91 1.01 -3 -4 4 8.70 1.86 3 -4 -4 10.50 1.91 3 -4 -4 7.56 0.95 3 4 -4 6.84 0.98 3 4 -4 8.52 1.02 -3 4 4 8.52 1.89 -3 4 4 8.72 1.03 3 4 -4 9.43 1.04 -3 4 4 8.15 1.12 -3 4 4 6.66 1.03 3 4 -4 7.82 1.02 -3 4 4 6.54 1.05 3 4 -4 7.54 0.95 -2 -4 4 29.58 1.61 2 -4 -4 25.52 1.59 -2 -4 4 30.10 1.72 2 -4 -4 28.55 1.66 -2 -4 4 25.11 2.67 2 -4 -4 27.89 1.73 -2 -4 4 29.78 1.80 2 -4 -4 28.53 2.54 2 -4 -4 29.14 1.46 -2 -4 4 32.22 1.69 2 -4 -4 30.70 1.51 -2 -4 4 29.56 1.74 -2 4 4 28.25 1.42 -2 4 4 30.13 1.58 2 4 -4 29.16 1.72 2 4 -4 31.24 1.67 -2 4 4 27.56 1.68 2 4 -4 29.45 1.43 -2 4 4 31.77 1.56 -2 4 4 27.19 2.58 2 4 -4 28.88 1.63 2 4 -4 29.89 1.64 -1 -4 4 62.08 2.17 1 -4 -4 58.66 3.52 1 -4 -4 60.25 2.08 -1 -4 4 59.27 2.12 -1 -4 4 61.19 1.93 1 -4 -4 60.89 2.16 1 -4 -4 61.11 2.00 -1 -4 4 62.42 2.24 -1 -4 4 63.97 3.31 1 -4 -4 65.44 1.90 -1 -4 4 64.53 2.04 -1 4 4 61.89 1.85 -1 4 4 59.13 2.17 -1 4 4 61.93 3.52 -1 4 4 63.35 1.95 1 4 -4 62.65 2.24 1 4 -4 61.52 1.91 1 4 -4 61.72 2.07 -1 4 4 63.03 1.94 -1 4 4 63.58 1.97 1 4 -4 59.78 2.02 1 4 -4 61.74 1.90 1 4 -4 64.95 2.17 0 -4 -4 129.29 3.05 0 -4 4 128.19 3.10 0 -4 -4 127.23 3.03 0 -4 -4 124.88 3.38 0 -4 -4 125.64 3.09 0 -4 -4 125.43 4.77 0 -4 4 131.54 3.42 0 -4 4 127.95 3.43 0 -4 4 127.27 3.06 0 -4 4 128.37 3.02 0 -4 4 128.57 3.13 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169.12 3.90 6 -4 4 169.66 5.31 6 -4 4 168.32 3.73 6 -4 4 166.61 3.84 -6 -4 -4 171.60 4.03 6 4 4 166.53 3.53 -6 4 -4 164.22 3.81 -6 4 -4 166.96 4.22 6 4 4 168.97 3.60 6 4 4 168.69 3.73 6 4 4 163.57 3.74 -6 4 -4 161.20 4.17 -7 -4 -4 36.44 1.72 7 -4 4 34.38 1.91 7 -4 4 34.33 2.03 7 -4 4 32.19 1.79 7 -4 4 34.25 2.83 7 -4 4 33.05 1.65 -7 -4 -4 30.37 1.70 -7 4 -4 34.45 1.81 -7 4 -4 31.18 1.67 7 4 4 32.91 1.66 -7 4 -4 32.00 1.97 7 4 4 32.27 1.72 7 4 4 32.35 1.20 7 4 4 30.98 1.26 8 -4 4 26.67 1.71 8 -4 4 28.31 2.96 8 -4 4 27.97 1.92 8 -4 4 26.97 2.02 -8 -4 -4 26.96 1.63 8 -4 4 24.32 1.44 8 4 4 24.95 1.70 8 4 4 26.49 1.72 -8 4 -4 25.87 2.13 -8 4 -4 23.93 1.76 -8 4 -4 26.27 1.68 9 -4 4 16.31 1.29 9 -4 4 15.05 1.49 -9 -4 -4 13.03 1.19 9 -4 4 16.03 1.54 9 -4 4 14.50 1.46 9 -4 4 15.31 2.24 -9 4 -4 12.56 1.30 9 4 4 15.12 1.69 -9 4 -4 15.62 1.47 -9 4 -4 14.46 1.64 9 4 4 15.18 1.64 10 -4 4 2.70 1.46 10 -4 4 4.45 1.40 10 -4 4 1.93 2.30 -10 -4 -4 2.19 1.17 -10 4 -4 4.57 1.19 -10 4 -4 3.98 1.27 -10 4 -4 3.66 1.44 10 4 4 3.16 1.22 10 4 4 4.01 1.28 11 -4 4 12.29 1.49 11 -4 4 11.93 2.58 11 -4 4 13.81 1.66 -11 4 -4 12.85 1.37 -11 4 -4 12.27 1.30 11 4 4 14.50 1.43 -11 4 -4 11.88 1.55 11 4 4 11.87 1.28 12 -4 4 9.58 2.58 12 -4 4 8.03 1.49 12 -4 4 9.77 1.61 -12 4 -4 11.87 1.37 -12 4 -4 11.39 1.31 12 4 4 9.75 1.28 12 4 4 12.73 1.35 13 -4 4 12.72 2.52 13 -4 4 11.74 1.47 13 -4 4 12.60 1.42 13 4 4 11.66 1.24 -13 4 -4 13.77 1.75 13 4 4 10.09 1.15 14 -4 4 32.01 2.00 14 -4 4 31.88 2.03 14 -4 4 31.06 3.61 14 4 4 29.65 1.58 14 4 4 28.62 1.70 15 -4 4 12.03 1.49 15 -4 4 10.65 1.33 15 -4 4 9.88 2.65 15 4 4 10.48 1.12 15 4 4 11.71 1.30 16 -4 4 1.80 1.43 16 -4 4 2.27 1.27 16 -4 4 0.44 2.68 16 4 4 2.01 0.89 16 4 4 1.10 0.98 17 -4 4 3.32 1.21 17 -4 4 3.28 1.36 17 -4 4 1.69 2.73 19 -5 -4 15.54 1.75 19 -5 -4 9.67 1.56 19 -5 -4 9.50 2.88 18 -5 -4 2.49 1.53 18 -5 -4 0.97 1.41 18 -5 -4 0.79 2.83 -18 5 4 11.50 3.73 -18 5 4 10.31 3.67 17 -5 -4 4.24 2.72 17 -5 -4 4.44 1.56 17 -5 -4 2.10 1.40 17 5 -4 1.46 0.92 17 5 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1.13 11 -5 -4 5.22 1.04 11 -5 -4 5.03 1.07 -11 5 4 6.59 1.44 -11 5 4 3.67 1.25 11 5 -4 6.45 1.35 11 5 -4 4.52 1.22 -11 5 4 5.13 1.29 -11 5 4 6.92 3.07 -10 -5 4 0.89 1.93 10 -5 -4 0.82 1.14 10 -5 -4 0.55 1.09 -10 -5 4 1.50 1.10 10 -5 -4 -1.47 1.34 10 -5 -4 1.16 1.47 -10 5 4 -0.76 1.16 10 5 -4 -0.07 1.26 -10 5 4 -1.70 1.30 10 5 -4 -1.31 1.17 -10 5 4 0.40 1.17 -10 5 4 -1.97 2.72 -9 -5 4 22.34 2.45 -9 -5 4 21.68 1.78 9 -5 -4 29.46 1.92 9 -5 -4 23.23 2.01 9 -5 -4 22.14 1.70 -9 -5 4 29.50 2.03 -9 5 4 26.16 1.98 9 5 -4 26.23 1.66 9 5 -4 23.55 1.25 -9 5 4 25.67 3.47 9 5 -4 24.27 1.27 9 5 -4 22.36 1.81 -9 5 4 26.60 1.82 -9 5 4 25.20 1.81 8 -5 -4 47.24 2.01 -8 -5 4 39.15 2.09 8 -5 -4 45.71 2.06 -8 -5 4 43.09 1.89 -8 -5 4 42.50 2.65 8 -5 -4 47.62 1.89 8 -5 -4 45.73 2.04 -8 5 4 43.22 1.94 -8 5 4 46.58 2.05 8 5 -4 48.14 1.99 -8 5 4 44.21 3.59 8 5 -4 45.95 1.89 8 5 -4 47.27 1.65 8 5 -4 46.61 1.72 -7 -5 4 107.03 3.94 7 -5 -4 115.49 2.93 7 -5 -4 110.55 2.93 7 -5 -4 115.85 2.81 -7 -5 4 111.60 3.17 -7 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2.02 -7 -6 9 26.23 2.14 7 -6 -9 30.19 2.06 -7 -6 9 26.62 2.50 -7 -6 9 28.79 2.14 7 -6 -9 29.54 2.51 7 -6 -9 26.57 2.24 -7 6 9 30.19 2.08 7 6 -9 31.18 2.25 7 6 -9 33.27 2.13 -7 6 9 29.78 2.37 -7 6 9 30.13 2.31 -7 6 9 26.52 3.92 7 6 -9 30.13 2.06 -7 6 9 28.63 3.12 7 6 -9 32.74 2.48 -6 -6 9 3.09 1.12 -6 -6 9 2.82 1.38 6 -6 -9 3.23 1.50 -6 -6 9 3.37 1.39 6 -6 -9 3.13 1.02 6 -6 -9 4.08 1.34 6 -6 -9 4.88 1.51 -6 -6 9 2.06 1.45 -6 -6 9 3.14 1.50 -6 -6 9 5.89 2.85 6 6 -9 2.95 1.52 -6 6 9 2.93 2.93 -6 6 9 3.97 1.42 -6 6 9 2.25 2.41 -6 6 9 5.54 1.54 -6 6 9 4.54 1.49 6 6 -9 9.70 1.85 6 6 -9 4.34 1.54 6 6 -9 1.58 1.23 -5 -6 9 49.99 2.48 -5 -6 9 51.50 2.42 -5 -6 9 51.91 2.56 -5 -6 9 49.03 2.54 -5 -6 9 54.06 3.97 5 -6 -9 51.41 2.18 5 -6 -9 50.05 2.42 5 -6 -9 53.06 2.65 5 -6 -9 52.17 2.48 -5 6 9 50.48 2.43 5 6 -9 53.66 2.37 -5 6 9 49.20 2.58 5 6 -9 50.53 2.37 5 6 -9 51.40 2.32 -5 6 9 50.13 2.44 5 6 -9 63.90 3.32 -5 6 9 52.73 3.75 5 6 -9 51.98 2.13 -5 6 9 50.60 3.71 4 -6 -9 108.35 3.13 -4 -6 9 111.04 4.75 -4 -6 9 105.61 3.39 4 -6 -9 112.12 3.26 4 -6 -9 108.74 3.34 4 -6 -9 103.63 3.12 -4 -6 9 103.19 3.42 -4 -6 9 109.26 3.21 -4 -6 9 110.45 3.30 -4 6 9 107.64 3.08 -4 6 9 100.86 3.04 -4 6 9 106.85 3.15 -4 6 9 105.89 4.67 4 6 -9 108.47 3.31 4 6 -9 108.03 3.20 4 6 -9 108.24 3.16 -4 6 9 107.64 4.94 4 6 -9 109.74 3.67 -4 6 9 104.40 3.35 3 -6 -9 13.98 1.62 -3 -6 9 12.59 3.12 -3 -6 9 13.58 1.46 -3 -6 9 12.33 1.49 3 -6 -9 10.98 1.48 -3 -6 9 11.90 1.55 -3 -6 9 11.21 1.38 3 -6 -9 13.83 1.43 -3 -6 9 12.78 1.50 3 -6 -9 11.05 1.50 3 6 -9 16.73 1.79 3 6 -9 10.49 1.56 -3 6 9 11.75 1.45 3 6 -9 13.20 1.46 -3 6 9 13.18 2.46 -3 6 9 13.92 1.52 -3 6 9 12.56 1.45 3 6 -9 12.75 1.56 3 6 -9 13.59 1.61 -3 6 9 11.90 1.44 -3 6 9 14.09 2.96 2 -6 -9 130.17 3.61 2 -6 -9 139.23 3.96 -2 -6 9 140.30 5.86 -2 -6 9 138.21 3.76 2 -6 -9 141.67 3.69 -2 -6 9 140.24 3.59 -2 -6 9 134.78 3.90 -2 -6 9 137.95 4.02 2 -6 -9 139.15 3.46 -2 -6 9 139.06 3.52 2 6 -9 135.91 3.87 -2 6 9 135.61 5.20 2 6 -9 133.70 3.93 -2 6 9 134.90 3.55 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62.52 2.89 4 6 9 62.36 3.56 4 6 9 61.66 2.77 -4 6 -9 70.17 3.12 4 6 9 60.98 2.72 -4 6 -9 63.98 3.06 4 6 9 66.63 2.77 4 6 9 66.53 2.65 -4 6 -9 66.08 3.09 5 -6 9 -0.68 1.67 5 -6 9 -0.32 1.75 5 -6 9 2.41 1.37 5 -6 9 -2.17 1.09 5 -6 9 0.71 1.87 5 -6 9 1.33 1.73 -5 -6 -9 1.95 1.57 -5 -6 -9 0.03 1.70 5 6 9 1.95 2.11 -5 6 -9 -1.55 1.62 5 6 9 0.46 1.49 5 6 9 -1.10 1.47 -5 6 -9 -1.64 1.75 5 6 9 0.09 1.73 -5 6 -9 -0.90 1.81 5 6 9 -0.42 1.67 6 -6 9 66.64 3.05 6 -6 9 74.25 3.15 6 -6 9 75.77 4.03 6 -6 9 77.68 3.13 -6 -6 -9 71.03 3.09 -6 -6 -9 71.61 2.82 6 6 9 74.03 2.73 6 6 9 69.87 3.05 6 6 9 71.16 3.34 -6 6 -9 69.78 3.36 -6 6 -9 72.26 3.09 6 6 9 71.35 3.09 -6 6 -9 70.51 3.27 7 -6 9 0.01 1.79 7 -6 9 -1.16 1.87 -7 -6 -9 1.36 1.76 7 -6 9 -2.48 2.26 7 -6 9 -1.36 1.89 -7 -6 -9 0.04 1.72 -7 6 -9 0.40 1.88 7 6 9 0.13 1.70 7 6 9 2.85 1.44 7 6 9 0.69 1.72 -7 6 -9 0.47 1.95 -7 6 -9 0.10 1.80 8 -6 9 10.57 1.89 8 -6 9 8.72 2.38 8 -6 9 14.44 1.96 8 -6 9 12.40 1.84 -8 -6 -9 13.54 1.80 -8 6 -9 12.59 2.03 8 6 9 11.39 1.80 -8 6 -9 12.04 1.89 -8 6 -9 11.54 2.06 8 6 9 12.41 1.45 8 6 9 14.50 1.76 9 -6 9 4.56 1.64 9 -6 9 1.56 2.20 -9 -6 -9 4.57 1.59 9 -6 9 1.95 1.68 9 -6 9 2.94 1.62 9 6 9 4.34 1.08 9 6 9 3.55 1.55 -9 6 -9 0.05 1.77 9 6 9 3.70 1.66 -9 6 -9 2.57 1.69 10 -6 9 11.39 1.56 10 -6 9 12.72 2.32 10 -6 9 9.80 1.71 10 -6 9 10.11 1.75 -10 -6 -9 13.19 1.64 10 6 9 11.96 1.76 -10 6 -9 11.68 1.81 10 6 9 13.08 1.61 -10 6 -9 10.92 1.75 11 -6 9 5.53 1.61 11 -6 9 3.94 2.48 11 -6 9 3.48 1.70 11 -6 9 4.88 1.40 -11 6 -9 5.21 1.74 11 6 9 2.61 1.68 11 6 9 4.98 1.62 12 -6 9 17.26 2.84 12 -6 9 20.64 1.57 12 -6 9 20.53 2.31 12 -6 9 23.89 2.47 12 6 9 22.41 2.33 12 6 9 19.85 2.17 13 -6 9 1.12 2.60 13 -6 9 0.23 1.78 13 -6 9 1.07 1.63 13 6 9 0.96 1.51 13 6 9 2.16 1.60 14 -6 9 0.66 1.61 14 -6 9 0.65 2.66 14 -6 9 2.50 1.87 14 6 9 -0.57 1.53 14 6 9 2.99 1.64 19 -7 -9 -1.72 1.90 19 -7 -9 1.08 1.75 19 -7 -9 2.20 2.97 -19 7 9 6.66 3.93 19 7 -9 0.93 1.44 -19 7 9 7.41 4.13 19 7 -9 1.86 1.55 18 -7 -9 9.26 2.10 18 -7 -9 6.02 2.99 18 -7 -9 10.70 1.78 18 7 -9 5.53 1.58 -18 7 9 19.07 4.26 -18 7 9 15.59 4.07 18 7 -9 10.77 1.55 17 -7 -9 16.15 2.05 17 -7 -9 16.20 1.87 17 7 -9 10.83 1.66 17 7 -9 13.44 1.60 -17 7 9 17.75 4.12 -17 7 9 29.82 4.36 -16 -7 9 0.98 1.50 16 -7 -9 6.29 1.98 16 -7 -9 4.28 1.14 16 -7 -9 5.53 1.80 16 7 -9 5.20 1.43 -16 7 9 8.68 3.92 -16 7 9 17.67 3.95 16 7 -9 4.41 1.53 15 -7 -9 53.49 3.03 15 -7 -9 51.04 2.67 15 -7 -9 49.46 1.92 -15 -7 9 47.82 3.84 -15 -7 9 50.52 2.56 -15 7 9 57.72 4.68 -15 7 9 48.84 2.88 -15 7 9 56.51 4.77 15 7 -9 50.28 2.60 15 7 -9 52.05 2.43 14 -7 -9 5.10 1.67 -14 -7 9 4.08 2.89 -14 -7 9 5.53 1.87 14 -7 -9 5.81 1.83 -14 -7 9 5.06 1.51 14 -7 -9 3.45 1.33 -14 7 9 8.99 1.73 -14 7 9 8.35 3.74 14 7 -9 4.96 1.50 -14 7 9 9.02 3.55 14 7 -9 4.77 1.59 -13 -7 9 25.65 3.09 13 -7 -9 24.88 2.05 13 -7 -9 28.32 2.68 -13 -7 9 26.13 2.43 13 -7 -9 23.51 2.36 -13 -7 9 23.68 3.97 13 7 -9 27.80 1.80 -13 7 9 26.40 4.16 -13 7 9 22.83 2.01 13 7 -9 24.64 2.43 13 7 -9 26.53 2.47 -13 7 9 30.84 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1.47 1.61 -6 -4 -10 1.49 1.53 6 -4 10 2.20 1.69 6 -4 10 2.55 2.03 -6 -4 -10 1.70 1.59 6 -4 10 1.56 1.58 6 -4 10 1.84 1.25 -6 4 -10 3.79 1.64 -6 4 -10 1.29 1.75 6 4 10 2.81 1.52 6 4 10 -0.41 1.48 6 4 10 0.50 2.44 6 4 10 -1.44 1.55 -6 4 -10 2.04 1.66 6 4 10 1.42 1.22 7 -4 10 22.47 2.53 -7 -4 -10 29.05 2.44 -7 -4 -10 22.32 2.41 7 -4 10 25.00 3.55 7 -4 10 22.27 2.42 7 -4 10 23.97 2.51 -7 -4 -10 33.95 2.63 -7 -4 -10 16.16 1.80 7 4 10 29.07 2.30 7 4 10 27.45 2.07 7 4 10 24.55 2.11 7 4 10 29.03 2.18 -7 4 -10 23.15 1.91 7 4 10 21.16 2.96 -7 4 -10 27.95 2.57 -7 4 -10 26.40 2.71 8 -4 10 0.25 1.79 -8 -4 -10 5.56 1.71 8 -4 10 3.35 2.40 8 -4 10 1.95 1.68 -8 -4 -10 0.09 2.68 -8 -4 -10 2.32 1.63 8 -4 10 3.78 1.72 -8 -4 -10 5.31 1.57 8 4 10 3.02 1.60 -8 4 -10 2.30 1.86 8 4 10 4.24 1.35 8 4 10 4.65 1.65 -8 4 -10 5.33 1.76 -8 4 -10 4.29 1.84 8 4 10 4.39 1.26 9 -4 10 57.49 2.81 9 -4 10 56.38 2.36 -9 -4 -10 40.76 3.88 -9 -4 -10 57.40 2.70 9 -4 10 53.88 2.71 9 -4 10 60.78 3.98 9 4 10 55.36 2.46 9 4 10 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18 -5 -10 16.02 2.99 -18 -5 10 24.30 4.08 -18 5 10 25.75 4.26 -18 5 10 19.96 2.43 -18 5 10 21.76 3.51 18 5 -10 19.99 2.00 18 5 -10 21.29 2.07 17 -5 -10 0.86 1.77 17 -5 -10 1.47 2.66 17 -5 -10 1.61 1.59 -17 -5 10 0.82 3.06 -17 5 10 2.85 3.20 -17 5 10 0.48 1.54 17 5 -10 -0.31 1.33 17 5 -10 0.21 1.45 -17 5 10 7.42 3.83 16 -5 -10 18.72 1.27 16 -5 -10 17.47 1.84 -16 -5 10 18.69 3.27 16 -5 -10 17.34 1.68 -16 -5 10 18.16 2.01 16 5 -10 19.97 2.04 -16 5 10 19.91 3.42 16 5 -10 21.01 2.00 -16 5 10 21.99 2.34 -16 5 10 18.99 3.80 15 -5 -10 1.72 1.58 -15 -5 10 3.55 1.38 -15 -5 10 13.61 2.47 15 -5 -10 1.04 1.11 -15 -5 10 1.76 2.89 15 -5 -10 2.20 1.55 15 5 -10 2.02 1.39 -15 5 10 3.32 3.24 -15 5 10 6.80 3.66 -15 5 10 0.80 1.54 15 5 -10 2.78 1.43 -14 -5 10 1.09 1.48 14 -5 -10 -0.92 1.68 -14 -5 10 2.68 3.15 14 -5 -10 -0.16 1.65 14 -5 -10 0.51 1.26 14 5 -10 0.37 1.47 -14 5 10 2.12 1.64 -14 5 10 0.91 1.78 14 5 -10 -0.25 1.61 -14 5 10 3.61 3.86 -14 5 10 -4.16 3.36 -13 -5 10 3.85 1.60 13 -5 -10 3.97 1.79 -13 -5 10 7.80 3.32 13 -5 -10 5.20 1.81 -13 -5 10 4.35 1.62 -13 -5 10 6.80 3.06 13 -5 -10 4.67 1.48 13 5 -10 5.77 1.69 -13 5 10 4.44 3.31 13 5 -10 4.82 1.10 -13 5 10 4.68 3.54 -13 5 10 4.09 1.85 -13 5 10 4.31 1.73 13 5 -10 1.40 1.27 13 5 -10 4.82 1.61 -12 -5 10 52.48 2.62 -12 -5 10 44.99 2.72 12 -5 -10 43.50 2.48 12 -5 -10 46.06 2.21 -12 -5 10 47.57 3.88 12 -5 -10 46.22 2.70 -12 -5 10 47.68 4.37 -12 5 10 50.03 2.80 -12 5 10 43.35 4.76 12 5 -10 49.55 2.61 -12 5 10 49.63 2.93 12 5 -10 48.65 2.22 12 5 -10 47.46 2.47 12 5 -10 45.44 2.05 -12 5 10 47.99 4.54 11 -5 -10 -0.31 1.66 11 -5 -10 -0.43 1.64 -11 -5 10 0.33 2.67 -11 -5 10 -0.51 1.49 11 -5 -10 -0.77 1.50 11 -5 -10 2.12 1.49 -11 -5 10 -1.41 1.54 -11 -5 10 -0.31 3.12 -11 5 10 2.87 3.28 -11 5 10 -0.95 1.62 11 5 -10 4.24 1.48 -11 5 10 1.08 1.59 11 5 -10 0.56 1.45 11 5 -10 -0.27 1.62 -11 5 10 -3.46 3.13 11 5 -10 1.00 1.16 -10 -5 10 68.25 2.83 10 -5 -10 69.46 2.63 10 -5 -10 65.17 2.47 -10 -5 10 63.88 3.26 -10 -5 10 60.62 2.92 10 -5 -10 69.58 2.77 -10 -5 10 64.87 4.64 10 -5 -10 70.96 2.87 -10 -5 10 62.30 3.61 -10 5 10 67.30 2.78 10 5 -10 69.60 2.65 10 5 -10 70.41 2.58 -10 5 10 65.32 4.44 -10 5 10 67.69 2.90 -10 5 10 64.52 4.82 10 5 -10 66.99 2.74 10 5 -10 65.60 2.51 9 -5 -10 10.56 1.46 9 -5 -10 10.37 1.50 -9 -5 10 8.00 1.49 9 -5 -10 8.12 1.47 -9 -5 10 9.96 3.00 9 -5 -10 10.66 1.48 -9 -5 10 9.69 1.93 9 -5 -10 9.50 1.16 9 -5 -10 8.60 1.47 9 -5 -10 10.43 1.16 -9 -5 10 9.51 1.36 -9 -5 10 10.36 1.54 9 5 -10 8.97 1.54 -9 5 10 9.68 1.58 -9 5 10 11.03 3.24 -9 5 10 11.36 3.03 9 5 -10 12.10 1.57 -9 5 10 11.15 1.60 9 5 -10 9.64 1.55 9 5 -10 10.03 1.20 -9 5 10 11.05 1.55 -8 -5 10 23.00 2.12 8 -5 -10 24.97 2.19 -8 -5 10 24.37 2.16 8 -5 -10 26.68 2.26 8 -5 -10 21.63 1.86 8 -5 -10 23.15 2.08 8 -5 -10 21.62 2.00 -8 -5 10 23.33 3.27 -8 -5 10 20.00 2.20 8 -5 -10 24.41 2.28 -8 5 10 20.30 3.09 -8 5 10 20.28 1.99 8 5 -10 23.21 2.18 -8 5 10 23.32 2.22 8 5 -10 32.17 2.37 -8 5 10 20.17 1.67 8 5 -10 23.80 2.13 -8 5 10 18.74 3.23 8 5 -10 22.24 2.20 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1.64 6 4 -14 4.59 1.77 -6 4 14 1.03 3.30 6 4 -14 0.43 1.08 -6 4 14 3.28 1.58 -6 4 14 3.46 1.65 6 4 -14 7.44 1.84 -5 -4 14 73.21 5.23 -5 -4 14 72.44 2.85 5 -4 -14 64.31 2.93 -5 -4 14 69.14 2.90 5 -4 -14 71.41 2.82 5 -4 -14 73.69 2.86 5 -4 -14 70.96 3.03 -5 -4 14 72.63 3.11 -5 -4 14 75.05 3.37 -5 4 14 76.05 2.96 5 4 -14 75.77 3.13 5 4 -14 72.77 3.02 5 4 -14 75.65 2.95 -5 4 14 70.28 3.01 -5 4 14 76.89 3.14 -5 4 14 81.69 4.99 5 4 -14 72.33 3.18 -5 4 14 68.76 2.82 -4 -4 14 32.09 2.88 -4 -4 14 34.62 2.71 -4 -4 14 35.34 2.90 4 -4 -14 34.94 2.94 -4 -4 14 37.33 2.52 4 -4 -14 33.05 2.57 -4 -4 14 32.59 4.76 4 -4 -14 37.56 2.43 -4 -4 14 33.79 2.43 4 -4 -14 37.27 2.82 4 4 -14 35.54 2.58 -4 4 14 33.12 2.53 4 4 -14 37.93 2.51 -4 4 14 36.31 2.47 4 4 -14 35.49 2.46 4 4 -14 33.83 3.02 4 4 -14 32.82 2.43 -4 4 14 33.48 2.55 -4 4 14 35.68 2.74 -4 4 14 34.11 4.26 -3 -4 14 99.79 3.55 -3 -4 14 103.40 3.64 -3 -4 14 99.89 3.56 -3 -4 14 100.12 3.67 3 -4 -14 92.78 3.28 -3 -4 14 102.69 5.73 3 -4 -14 103.84 3.48 3 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1.65 0 -4 -14 3.75 1.83 0 -4 14 8.16 1.87 0 -4 14 1.53 1.07 0 -4 14 3.76 1.68 0 -4 14 5.34 3.73 0 -4 -14 3.79 1.68 0 -4 14 4.81 1.61 0 -4 14 7.83 1.96 0 4 -14 7.05 2.18 0 4 -14 5.34 1.84 0 4 14 5.36 3.19 0 4 14 4.16 1.74 0 4 14 6.18 1.77 0 4 14 5.66 1.62 0 4 14 6.34 1.90 0 4 14 7.16 1.63 0 4 -14 3.76 1.79 0 4 -14 6.64 1.97 1 -4 14 65.30 3.13 1 -4 14 66.10 2.81 -1 -4 -14 56.15 3.12 1 -4 14 62.84 3.06 1 -4 14 65.86 3.16 -1 -4 -14 56.05 2.74 -1 -4 -14 57.80 3.16 1 -4 14 62.11 5.43 1 -4 14 65.89 3.26 1 4 14 63.52 2.86 -1 4 -14 56.48 3.64 1 4 14 64.14 2.80 -1 4 -14 62.82 3.15 -1 4 -14 57.39 3.29 1 4 14 59.90 2.97 -1 4 -14 61.35 2.88 1 4 14 61.83 3.16 1 4 14 60.33 2.71 1 4 14 63.09 4.46 2 -4 14 9.17 1.81 2 -4 14 7.10 2.00 -2 -4 -14 10.11 2.01 2 -4 14 9.64 1.60 2 -4 14 9.81 1.88 2 -4 14 12.26 1.89 2 -4 14 14.20 4.46 -2 -4 -14 8.89 1.95 2 4 14 12.64 1.58 -2 4 -14 10.36 2.04 -2 4 -14 9.23 2.01 -2 4 -14 10.30 1.80 2 4 14 13.41 3.44 -2 4 -14 9.84 2.10 2 4 14 10.42 2.03 2 4 14 9.81 1.50 2 4 14 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4.00 -12 -5 14 50.34 3.17 -12 -5 14 56.91 3.15 12 -5 -14 57.34 3.16 12 5 -14 56.88 3.18 -12 5 14 56.82 4.75 12 5 -14 52.67 2.98 -12 5 14 60.58 4.59 12 5 -14 63.44 2.78 -12 5 14 55.53 3.18 -12 5 14 49.87 3.23 11 -5 -14 4.88 1.88 -11 -5 14 0.63 1.83 11 -5 -14 3.60 1.27 11 -5 -14 1.69 1.64 11 -5 -14 -0.85 1.85 11 -5 -14 3.05 1.92 -11 -5 14 3.21 2.12 -11 -5 14 -0.06 2.47 -11 -5 14 3.47 3.82 -11 5 14 -0.06 2.03 -11 5 14 4.34 3.56 11 5 -14 1.14 1.82 -11 5 14 1.30 1.83 -11 5 14 -0.32 3.58 11 5 -14 -0.59 1.89 11 5 -14 1.74 1.92 10 -5 -14 63.55 2.93 10 -5 -14 64.72 2.89 -10 -5 14 66.19 3.92 10 -5 -14 67.95 2.74 -10 -5 14 70.55 3.36 -10 -5 14 61.99 3.17 10 -5 -14 68.68 3.31 10 -5 -14 62.00 2.73 -10 -5 14 67.72 5.32 -10 5 14 66.36 3.16 -10 5 14 68.66 5.48 10 5 -14 67.53 3.10 10 5 -14 67.40 3.18 -10 5 14 65.91 2.90 10 5 -14 60.05 2.93 -9 -5 14 4.35 2.18 -9 -5 14 3.66 1.78 9 -5 -14 2.36 1.76 9 -5 -14 2.30 1.86 9 -5 -14 5.65 1.89 -9 -5 14 3.41 1.92 9 -5 -14 3.93 1.89 9 -5 -14 1.78 1.57 -9 -5 14 0.88 3.83 9 5 -14 3.45 1.61 -9 5 14 3.79 1.75 -9 5 14 2.94 1.94 -9 5 14 3.34 3.41 9 5 -14 0.55 1.90 9 5 -14 3.16 1.95 -9 5 14 3.24 1.92 -8 -5 14 3.89 1.70 8 -5 -14 2.38 1.77 8 -5 -14 2.57 1.65 -8 -5 14 3.56 1.61 8 -5 -14 1.83 1.63 -8 -5 14 0.55 2.02 8 -5 -14 1.26 1.80 -8 -5 14 4.22 1.97 8 -5 -14 -0.30 1.77 -8 -5 14 3.24 3.86 -8 5 14 2.58 1.72 -8 5 14 3.70 3.63 8 5 -14 2.20 1.87 -8 5 14 1.28 1.74 8 5 -14 3.36 1.61 8 5 -14 2.09 1.61 -8 5 14 5.26 1.72 8 5 -14 4.24 1.84 7 -5 -14 0.30 1.67 -7 -5 14 2.85 3.90 -7 -5 14 2.86 1.61 7 -5 -14 0.31 1.78 7 -5 -14 0.70 1.82 -7 -5 14 0.26 2.01 7 -5 -14 3.04 1.79 -7 -5 14 1.29 1.66 -7 -5 14 1.85 1.91 7 -5 -14 1.16 1.78 -7 5 14 0.79 1.73 7 5 -14 1.83 1.72 -7 5 14 -0.37 1.72 -7 5 14 2.16 3.54 7 5 -14 -1.02 1.86 -7 5 14 1.50 1.88 7 5 -14 1.93 1.82 7 5 -14 2.60 1.67 -6 -5 14 10.04 2.00 6 -5 -14 9.29 1.79 6 -5 -14 11.44 1.81 -6 -5 14 9.54 1.84 -6 -5 14 11.22 1.82 6 -5 -14 13.82 1.82 6 -5 -14 9.71 1.89 6 -5 -14 10.53 1.76 -6 -5 14 11.38 1.83 -6 -5 14 6.67 3.95 6 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2.12 8 2 -25 1.62 2.34 7 -2 -25 2.65 2.33 -7 -2 25 3.10 2.22 -7 -2 25 7.32 4.48 7 2 -25 5.89 2.45 -7 2 25 5.61 2.44 -7 2 25 10.04 4.73 -6 -2 25 0.97 2.41 6 -2 -25 1.98 2.38 -6 -2 25 5.46 4.90 6 2 -25 0.54 2.40 -6 2 25 -0.98 2.36 -6 2 25 3.70 4.63 -5 -2 25 3.50 2.44 5 -2 -25 2.09 2.41 -5 -2 25 -1.78 4.31 5 2 -25 3.72 2.46 -5 2 25 8.50 4.64 -5 2 25 1.27 2.36 4 -2 -25 3.43 2.45 -4 -2 25 5.77 4.98 -4 -2 25 3.40 2.44 -4 2 25 -2.19 2.26 4 2 -25 -0.99 2.44 -4 2 25 -2.97 4.55 3 -2 -25 18.59 2.62 -3 -2 25 12.98 4.99 -3 -2 25 15.11 2.58 3 2 -25 15.38 2.66 -3 2 25 18.10 5.15 -3 2 25 16.31 2.46 12 -3 -25 1.39 2.21 -12 -3 25 -4.21 2.48 -12 -3 25 -1.18 4.76 -12 3 25 0.89 4.90 12 3 -25 0.47 2.35 -12 3 25 -2.64 2.44 -11 -3 25 -2.16 2.46 -11 -3 25 -1.25 4.84 11 -3 -25 1.75 2.20 11 3 -25 -1.99 2.23 -11 3 25 5.87 4.78 -11 3 25 3.09 2.42 10 -3 -25 9.30 2.36 -10 -3 25 6.51 4.85 -10 -3 25 10.60 2.59 -10 3 25 6.42 2.48 10 3 -25 11.10 2.39 -10 3 25 18.35 4.89 -9 -3 25 -1.16 2.21 -9 -3 25 2.58 4.83 9 -3 -25 3.16 2.36 -9 3 25 6.87 4.81 -9 3 25 4.00 2.47 9 3 -25 2.22 2.35 8 -3 -25 17.86 2.59 -8 -3 25 13.87 5.19 -8 -3 25 14.58 2.38 8 3 -25 15.81 2.55 -8 3 25 14.59 2.57 -8 3 25 16.33 4.45 7 -3 -25 2.80 2.47 -7 -3 25 -7.72 4.35 -7 -3 25 0.72 2.53 7 3 -25 0.49 2.21 -7 3 25 0.33 2.38 -7 3 25 -4.05 4.54 -6 -3 25 -4.51 4.74 6 -3 -25 0.09 2.18 -6 -3 25 -2.57 2.46 -6 3 25 -1.09 4.54 6 3 -25 -1.40 2.47 -6 3 25 -0.34 2.29 -5 -3 25 0.48 2.46 -5 -3 25 0.90 4.88 5 -3 -25 5.74 2.42 5 3 -25 -1.00 2.53 -5 3 25 3.83 2.37 -5 3 25 3.76 4.59 4 -3 -25 12.21 2.54 -4 -3 25 7.44 4.98 -4 -3 25 4.29 2.47 -4 3 25 6.30 2.39 -4 3 25 10.20 4.69 4 3 -25 9.74 2.62 3 -3 -25 -0.70 2.42 -3 -3 25 3.00 5.01 -3 3 25 -3.32 2.27 -10 -4 25 -0.58 2.60 10 -4 -25 2.08 2.29 -10 -4 25 -1.23 4.92 -10 4 25 -1.93 2.41 -10 4 25 2.84 4.74 10 4 -25 -0.43 2.49 -9 -4 25 1.76 2.59 9 -4 -25 3.61 2.30 -9 -4 25 1.37 5.03 -9 4 25 7.49 4.79 -9 4 25 -0.40 2.41 9 4 -25 1.60 2.40 8 -4 -25 1.38 2.34 -8 -4 25 3.75 4.92 -8 -4 25 -1.75 2.56 8 4 -25 -1.30 2.44 -8 4 25 6.55 4.64 -8 4 25 0.15 2.16 -7 -4 25 4.93 2.57 -7 -4 25 -0.99 4.89 7 -4 -25 1.91 2.39 7 4 -25 -1.58 2.45 -7 4 25 0.80 2.41 -7 4 25 3.21 4.56 6 -4 -25 1.37 2.43 -6 -4 25 1.63 2.51 -6 -4 25 1.94 4.94 -6 4 25 2.96 2.45 -6 4 25 6.60 4.68 6 4 -25 2.37 2.52 -5 -4 25 2.20 2.52 -5 -4 25 0.93 5.00 5 -4 -25 4.72 2.44 5 4 -25 1.38 2.53 -5 4 25 4.58 4.59 -5 4 25 1.22 2.40 -9 0 26 -0.21 2.25 9 0 -26 -1.31 2.34 -9 0 26 4.92 4.86 -8 0 26 7.25 4.97 -8 0 26 0.24 2.44 8 0 -26 -0.18 2.44 -7 0 26 3.70 4.93 7 0 -26 3.87 2.48 -7 0 26 2.47 2.46 -6 0 26 7.01 4.97 6 0 -26 2.12 2.48 -6 0 26 -1.04 2.49 -9 -1 26 5.56 2.56 -9 -1 26 4.51 4.92 9 -1 -26 8.76 2.49 9 1 -26 8.53 2.48 -9 1 26 6.04 2.56 -9 1 26 8.13 4.93 -8 -1 26 0.69 2.25 8 -1 -26 1.22 2.44 -8 -1 26 2.16 4.95 -8 1 26 0.57 4.79 -8 1 26 1.08 2.43 8 1 -26 0.57 2.46 -7 -1 26 -1.96 2.47 -7 -1 26 -3.97 4.82 7 -1 -26 4.11 2.45 7 1 -26 -0.64 2.36 -7 1 26 5.26 2.51 -7 1 26 4.21 4.77 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 89832 _database_code_depnum_ccdc_archive 'CCDC 909100' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_dr042 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H33 Cl6 N3 Sn2' _chemical_formula_weight 957.73 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 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 13.7902(3) _cell_length_b 18.1623(4) _cell_length_c 16.7627(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.4330(10) _cell_angle_gamma 90.00 _cell_volume 3880.71(14) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9550 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 28.27 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 1.730 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6918 _exptl_absorpt_correction_T_max 0.7938 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg (650 frames). Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 56379 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 28.28 _reflns_number_total 9552 _reflns_number_gt 8264 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _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^)+(0.0385P)^2^+3.0920P] 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 9552 _refine_ls_number_parameters 451 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0728 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 0.152437(12) 0.711064(9) 0.861391(9) 0.03128(5) Uani 1 1 d . . . Sn2 Sn 0.629159(14) 0.507648(9) -0.051735(11) 0.03639(5) Uani 1 1 d . . . Cl1 Cl 0.05294(6) 0.82317(4) 0.80149(4) 0.05099(17) Uani 1 1 d . . . Cl2 Cl 0.67108(5) 0.63967(4) -0.02311(5) 0.04709(15) Uani 1 1 d . . . Cl3 Cl 0.62641(6) 0.48695(5) 0.09290(5) 0.05815(19) Uani 1 1 d . . . Cl4 Cl 0.81510(7) 0.46215(4) 0.00106(7) 0.0674(2) Uani 1 1 d . . . N1 N -0.00781(14) 0.64735(11) 0.78637(11) 0.0289(4) Uani 1 1 d . . . N2 N 0.06276(13) 0.69165(9) 0.94930(10) 0.0227(3) Uani 1 1 d . . . N3 N 0.23199(14) 0.77519(10) 0.99738(10) 0.0254(3) Uani 1 1 d . . . C1 C -0.06393(16) 0.62740(11) 0.82851(12) 0.0248(4) Uani 1 1 d . . . C2 C -0.02490(16) 0.65041(11) 0.92093(12) 0.0245(4) Uani 1 1 d . . . C3 C -0.07236(17) 0.62761(13) 0.97625(14) 0.0309(4) Uani 1 1 d . . . H3A H -0.1333 0.5975 0.9557 0.037 Uiso 1 1 calc R . . C4 C -0.02963(18) 0.64942(14) 1.06197(14) 0.0346(5) Uani 1 1 d . . . H4A H -0.0621 0.6355 1.1005 0.042 Uiso 1 1 calc R . . C5 C 0.06036(18) 0.69147(13) 1.09074(13) 0.0311(4) Uani 1 1 d . . . H5A H 0.0905 0.7071 1.1492 0.037 Uiso 1 1 calc R . . C6 C 0.10629(16) 0.71069(11) 1.03293(12) 0.0238(4) Uani 1 1 d . . . C7 C 0.20668(16) 0.75238(11) 1.05908(12) 0.0245(4) Uani 1 1 d . . . C8 C -0.16132(17) 0.58309(12) 0.79184(12) 0.0281(4) Uani 1 1 d . . . C9 C -0.1583(2) 0.51388(13) 0.75723(15) 0.0349(5) Uani 1 1 d . . . H9A H -0.0937 0.4943 0.7587 0.042 Uiso 1 1 calc R . . C10 C -0.2503(2) 0.47363(15) 0.72056(16) 0.0444(6) Uani 1 1 d . . . H10A H -0.2484 0.4261 0.6976 0.053 Uiso 1 1 calc R . . C11 C -0.3439(2) 0.50214(17) 0.71725(16) 0.0470(7) Uani 1 1 d . . . H11A H -0.4066 0.4746 0.6910 0.056 Uiso 1 1 calc R . . C12 C -0.34749(19) 0.57040(16) 0.75167(15) 0.0420(6) Uani 1 1 d . . . H12A H -0.4126 0.5898 0.7490 0.050 Uiso 1 1 calc R . . C13 C -0.25571(18) 0.61098(14) 0.79044(14) 0.0345(5) Uani 1 1 d . . . H13A H -0.2577 0.6575 0.8158 0.041 Uiso 1 1 calc R . . C14 C 0.27349(17) 0.76191(12) 1.15237(12) 0.0272(4) Uani 1 1 d . . . C15 C 0.3096(2) 0.83158(13) 1.18541(14) 0.0343(5) Uani 1 1 d . . . H15A H 0.2852 0.8740 1.1502 0.041 Uiso 1 1 calc R . . C16 C 0.3812(2) 0.83895(15) 1.26963(15) 0.0423(6) Uani 1 1 d . . . H16A H 0.4060 0.8864 1.2921 0.051 Uiso 1 1 calc R . . C17 C 0.4164(2) 0.77731(16) 1.32101(14) 0.0434(6) Uani 1 1 d . . . H17A H 0.4670 0.7823 1.3782 0.052 Uiso 1 1 calc R . . C18 C 0.3784(2) 0.70873(16) 1.28964(15) 0.0426(6) Uani 1 1 d . . . H18A H 0.4015 0.6667 1.3258 0.051 Uiso 1 1 calc R . . C19 C 0.30630(19) 0.70049(13) 1.20501(14) 0.0344(5) Uani 1 1 d . . . H19A H 0.2798 0.6531 1.1836 0.041 Uiso 1 1 calc R . . C20 C -0.03455(19) 0.63265(15) 0.69592(13) 0.0363(5) Uani 1 1 d . . . C21 C -0.1146(2) 0.67386(17) 0.63484(15) 0.0479(7) Uani 1 1 d . . . C22 C -0.1307(3) 0.6632(2) 0.54808(18) 0.0729(12) Uani 1 1 d . . . H22A H -0.1847 0.6897 0.5048 0.087 Uiso 1 1 calc R . . C23 C -0.0699(4) 0.6150(3) 0.5242(2) 0.0854(14) Uani 1 1 d . . . H23A H -0.0814 0.6095 0.4649 0.102 Uiso 1 1 calc R . . C24 C 0.0074(3) 0.5749(2) 0.5852(2) 0.0715(11) Uani 1 1 d . . . H24A H 0.0481 0.5414 0.5674 0.086 Uiso 1 1 calc R . . C25 C 0.0275(2) 0.58232(18) 0.67356(17) 0.0481(7) Uani 1 1 d . . . C26 C -0.1815(2) 0.7279(2) 0.6591(2) 0.0601(9) Uani 1 1 d . . . H26A H -0.1608 0.7279 0.7219 0.090 Uiso 1 1 calc R . . H26B H -0.2554 0.7136 0.6313 0.090 Uiso 1 1 calc R . . H26C H -0.1718 0.7773 0.6398 0.090 Uiso 1 1 calc R . . C27 C 0.1095(3) 0.5365(2) 0.7380(2) 0.0614(9) Uani 1 1 d . . . H27A H 0.1434 0.5054 0.7084 0.092 Uiso 1 1 calc R . . H27B H 0.0772 0.5053 0.7687 0.092 Uiso 1 1 calc R . . H27C H 0.1620 0.5685 0.7793 0.092 Uiso 1 1 calc R . . C28 C 0.33010(16) 0.81149(12) 1.01163(12) 0.0253(4) Uani 1 1 d . . . C29 C 0.32914(18) 0.88735(12) 0.99895(14) 0.0312(4) Uani 1 1 d . . . C30 C 0.4235(2) 0.92062(14) 1.00722(18) 0.0439(6) Uani 1 1 d . . . H30A H 0.4256 0.9724 1.0000 0.053 Uiso 1 1 calc R . . C31 C 0.5142(2) 0.87986(16) 1.02570(19) 0.0472(6) Uani 1 1 d . . . H31A H 0.5776 0.9036 1.0305 0.057 Uiso 1 1 calc R . . C32 C 0.51265(19) 0.80470(14) 1.03716(16) 0.0375(5) Uani 1 1 d . . . H32A H 0.5752 0.7771 1.0497 0.045 Uiso 1 1 calc R . . C33 C 0.42089(17) 0.76877(12) 1.03065(13) 0.0292(4) Uani 1 1 d . . . C34 C 0.2311(2) 0.93282(13) 0.97932(16) 0.0386(5) Uani 1 1 d . . . H34A H 0.1726 0.9005 0.9755 0.058 Uiso 1 1 calc R . . H34B H 0.2146 0.9585 0.9243 0.058 Uiso 1 1 calc R . . H34C H 0.2426 0.9689 1.0255 0.058 Uiso 1 1 calc R . . C35 C 0.4215(2) 0.68700(13) 1.04290(17) 0.0388(5) Uani 1 1 d . . . H35A H 0.4923 0.6679 1.0554 0.058 Uiso 1 1 calc R . . H35B H 0.3722 0.6640 0.9901 0.058 Uiso 1 1 calc R . . H35C H 0.4004 0.6757 1.0911 0.058 Uiso 1 1 calc R . . Cl5 Cl 0.6472(3) 0.80340(13) 0.7926(3) 0.1259(13) Uani 0.55 1 d PDU A 1 C36 C 0.6611(13) 0.8920(5) 0.7590(10) 0.105(5) Uani 0.55 1 d PDU A 1 H36A H 0.7312 0.8966 0.7561 0.125 Uiso 0.55 1 calc PR A 1 H36B H 0.6079 0.8998 0.7001 0.125 Uiso 0.55 1 calc PR A 1 Cl6 Cl 0.6472(5) 0.9595(2) 0.8263(3) 0.0922(14) Uani 0.55 1 d PDU A 1 Cl5' Cl 0.7370(8) 0.8291(4) 0.7999(3) 0.246(4) Uani 0.45 1 d PDU B 2 C36' C 0.6234(13) 0.8811(7) 0.7569(9) 0.101(5) Uani 0.45 1 d PDU B 2 H36C H 0.5612 0.8494 0.7460 0.121 Uiso 0.45 1 calc PR B 2 H36D H 0.6181 0.9031 0.7013 0.121 Uiso 0.45 1 calc PR B 2 Cl6' Cl 0.6272(6) 0.9494(4) 0.8289(6) 0.123(3) Uani 0.45 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02484(8) 0.04643(10) 0.02442(7) -0.00748(6) 0.01148(6) -0.01064(6) Sn2 0.03651(10) 0.03535(9) 0.04144(9) -0.00101(6) 0.01951(7) -0.00374(7) Cl1 0.0615(4) 0.0476(4) 0.0318(3) 0.0097(2) 0.0042(3) -0.0093(3) Cl2 0.0414(3) 0.0351(3) 0.0645(4) -0.0051(3) 0.0200(3) 0.0039(3) Cl3 0.0474(4) 0.0869(6) 0.0417(3) 0.0160(3) 0.0187(3) 0.0022(4) Cl4 0.0522(4) 0.0413(4) 0.1236(7) 0.0212(4) 0.0501(5) 0.0173(3) N1 0.0227(9) 0.0390(10) 0.0234(8) -0.0036(7) 0.0070(7) -0.0045(7) N2 0.0201(8) 0.0245(8) 0.0230(7) 0.0003(6) 0.0077(6) -0.0012(6) N3 0.0237(9) 0.0269(8) 0.0243(7) -0.0012(6) 0.0077(7) -0.0053(7) C1 0.0202(9) 0.0273(10) 0.0252(9) -0.0003(7) 0.0067(7) -0.0007(8) C2 0.0195(9) 0.0267(10) 0.0257(9) -0.0003(7) 0.0069(7) -0.0010(8) C3 0.0242(10) 0.0379(12) 0.0305(10) -0.0005(8) 0.0105(8) -0.0058(9) C4 0.0294(11) 0.0479(14) 0.0305(10) -0.0001(9) 0.0158(9) -0.0076(10) C5 0.0303(11) 0.0389(12) 0.0250(9) -0.0025(8) 0.0116(8) -0.0042(9) C6 0.0231(10) 0.0249(9) 0.0233(8) -0.0012(7) 0.0087(7) -0.0023(8) C7 0.0250(10) 0.0243(9) 0.0233(8) -0.0028(7) 0.0081(7) -0.0026(8) C8 0.0247(10) 0.0328(11) 0.0238(8) -0.0008(8) 0.0059(8) -0.0058(8) C9 0.0366(13) 0.0339(12) 0.0365(11) -0.0057(9) 0.0166(10) -0.0078(10) C10 0.0545(17) 0.0422(14) 0.0389(12) -0.0114(10) 0.0205(12) -0.0212(12) C11 0.0382(14) 0.0639(18) 0.0351(12) -0.0072(11) 0.0096(11) -0.0273(13) C12 0.0257(12) 0.0589(16) 0.0371(11) 0.0045(11) 0.0072(9) -0.0072(11) C13 0.0274(11) 0.0395(12) 0.0343(10) 0.0002(9) 0.0093(9) -0.0023(9) C14 0.0257(10) 0.0336(11) 0.0219(8) -0.0037(8) 0.0085(8) -0.0063(8) C15 0.0424(13) 0.0325(11) 0.0295(10) -0.0072(8) 0.0157(9) -0.0088(10) C16 0.0491(15) 0.0479(15) 0.0323(11) -0.0155(10) 0.0182(11) -0.0207(12) C17 0.0371(13) 0.0677(18) 0.0221(9) -0.0076(10) 0.0074(9) -0.0179(12) C18 0.0400(14) 0.0536(16) 0.0278(10) 0.0056(10) 0.0057(10) -0.0051(11) C19 0.0364(13) 0.0360(12) 0.0271(10) -0.0009(8) 0.0079(9) -0.0075(10) C20 0.0322(12) 0.0517(14) 0.0242(9) -0.0074(9) 0.0101(9) -0.0179(10) C21 0.0408(14) 0.0632(18) 0.0300(11) 0.0046(11) 0.0027(10) -0.0236(13) C22 0.081(3) 0.094(3) 0.0268(12) 0.0048(14) 0.0018(14) -0.041(2) C23 0.106(3) 0.121(3) 0.0298(14) -0.0239(18) 0.0270(18) -0.055(3) C24 0.081(2) 0.098(3) 0.0500(17) -0.0395(18) 0.0408(18) -0.042(2) C25 0.0425(14) 0.0670(18) 0.0406(12) -0.0238(12) 0.0224(11) -0.0218(13) C26 0.0391(16) 0.072(2) 0.0529(16) 0.0242(15) -0.0012(13) -0.0030(14) C27 0.0442(17) 0.073(2) 0.072(2) -0.0308(17) 0.0280(15) -0.0028(15) C28 0.0250(10) 0.0282(10) 0.0214(8) -0.0019(7) 0.0074(7) -0.0067(8) C29 0.0327(12) 0.0302(11) 0.0301(10) -0.0006(8) 0.0112(9) -0.0047(9) C30 0.0418(14) 0.0307(12) 0.0591(15) 0.0009(11) 0.0191(12) -0.0117(11) C31 0.0339(14) 0.0451(15) 0.0617(16) -0.0015(12) 0.0174(12) -0.0157(11) C32 0.0252(11) 0.0439(13) 0.0397(12) -0.0027(10) 0.0082(9) -0.0053(10) C33 0.0281(11) 0.0318(11) 0.0258(9) -0.0033(8) 0.0082(8) -0.0050(9) C34 0.0403(13) 0.0316(12) 0.0423(12) 0.0028(9) 0.0140(10) 0.0008(10) C35 0.0347(13) 0.0331(12) 0.0462(13) 0.0027(10) 0.0128(10) 0.0003(10) Cl5 0.113(2) 0.0479(10) 0.239(4) 0.0236(15) 0.091(2) 0.0121(12) C36 0.161(14) 0.052(4) 0.102(8) -0.011(4) 0.052(9) -0.030(7) Cl6 0.130(4) 0.0572(13) 0.0846(17) -0.0174(11) 0.0356(19) -0.0299(18) Cl5' 0.385(10) 0.165(5) 0.130(3) -0.026(3) 0.033(5) 0.161(6) C36' 0.136(10) 0.086(8) 0.055(5) -0.013(5) 0.008(6) -0.054(6) Cl6' 0.073(2) 0.134(5) 0.168(5) -0.059(4) 0.051(2) -0.002(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 Sn1 N2 2.2839(16) . ? Sn1 N1 2.3839(18) . ? Sn1 N3 2.4183(17) . ? Sn1 Cl1 2.4464(7) . ? Sn2 Cl3 2.4680(7) . ? Sn2 Cl2 2.4703(7) . ? Sn2 Cl4 2.5118(8) . ? N1 C1 1.283(3) . ? N1 C20 1.442(3) . ? N2 C2 1.345(3) . ? N2 C6 1.343(2) . ? N3 C7 1.280(3) . ? N3 C28 1.441(3) . ? C1 C8 1.483(3) . ? C1 C2 1.493(3) . ? C2 C3 1.387(3) . ? C3 C4 1.387(3) . ? C4 C5 1.378(3) . ? C5 C6 1.389(3) . ? C6 C7 1.490(3) . ? C7 C14 1.492(3) . ? C8 C13 1.389(3) . ? C8 C9 1.392(3) . ? C9 C10 1.388(3) . ? C10 C11 1.372(4) . ? C11 C12 1.376(4) . ? C12 C13 1.393(3) . ? C14 C19 1.387(3) . ? C14 C15 1.395(3) . ? C15 C16 1.386(3) . ? C16 C17 1.383(4) . ? C17 C18 1.375(4) . ? C18 C19 1.396(3) . ? C20 C25 1.397(4) . ? C20 C21 1.402(4) . ? C21 C22 1.399(4) . ? C21 C26 1.504(5) . ? C22 C23 1.373(6) . ? C23 C24 1.371(6) . ? C24 C25 1.405(4) . ? C25 C27 1.485(5) . ? C28 C29 1.393(3) . ? C28 C33 1.402(3) . ? C29 C30 1.393(3) . ? C29 C34 1.509(3) . ? C30 C31 1.383(4) . ? C31 C32 1.380(4) . ? C32 C33 1.390(3) . ? C33 C35 1.499(3) . ? Cl5 C36 1.739(11) . ? C36 Cl6 1.726(10) . ? Cl5' C36' 1.734(15) . ? C36' Cl6' 1.718(12) . ? 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 N2 Sn1 N1 69.16(6) . . ? N2 Sn1 N3 68.20(6) . . ? N1 Sn1 N3 136.62(6) . . ? N2 Sn1 Cl1 92.08(5) . . ? N1 Sn1 Cl1 85.74(5) . . ? N3 Sn1 Cl1 88.15(5) . . ? Cl3 Sn2 Cl2 92.70(3) . . ? Cl3 Sn2 Cl4 90.00(3) . . ? Cl2 Sn2 Cl4 96.84(3) . . ? C1 N1 C20 124.10(18) . . ? C1 N1 Sn1 118.63(13) . . ? C20 N1 Sn1 117.27(13) . . ? C2 N2 C6 119.73(17) . . ? C2 N2 Sn1 119.51(13) . . ? C6 N2 Sn1 119.83(13) . . ? C7 N3 C28 122.86(17) . . ? C7 N3 Sn1 116.12(13) . . ? C28 N3 Sn1 115.86(12) . . ? N1 C1 C8 124.47(18) . . ? N1 C1 C2 115.97(18) . . ? C8 C1 C2 119.54(17) . . ? N2 C2 C3 121.30(18) . . ? N2 C2 C1 116.25(17) . . ? C3 C2 C1 122.36(19) . . ? C4 C3 C2 119.0(2) . . ? C5 C4 C3 119.4(2) . . ? C4 C5 C6 118.98(19) . . ? N2 C6 C5 121.48(19) . . ? N2 C6 C7 115.67(17) . . ? C5 C6 C7 122.85(18) . . ? N3 C7 C6 115.86(17) . . ? N3 C7 C14 124.03(19) . . ? C6 C7 C14 120.03(17) . . ? C13 C8 C9 120.0(2) . . ? C13 C8 C1 120.3(2) . . ? C9 C8 C1 119.8(2) . . ? C10 C9 C8 119.5(2) . . ? C11 C10 C9 120.4(3) . . ? C10 C11 C12 120.4(2) . . ? C11 C12 C13 120.0(3) . . ? C8 C13 C12 119.6(2) . . ? C19 C14 C15 119.78(19) . . ? C19 C14 C7 119.65(19) . . ? C15 C14 C7 120.39(19) . . ? C16 C15 C14 120.0(2) . . ? C15 C16 C17 120.0(2) . . ? C18 C17 C16 120.2(2) . . ? C17 C18 C19 120.4(2) . . ? C14 C19 C18 119.6(2) . . ? C25 C20 C21 123.1(2) . . ? C25 C20 N1 117.8(2) . . ? C21 C20 N1 118.9(2) . . ? C22 C21 C20 117.0(3) . . ? C22 C21 C26 120.1(3) . . ? C20 C21 C26 123.0(2) . . ? C23 C22 C21 121.3(4) . . ? C24 C23 C22 120.5(3) . . ? C23 C24 C25 121.3(4) . . ? C20 C25 C24 116.8(3) . . ? C20 C25 C27 123.1(2) . . ? C24 C25 C27 120.1(3) . . ? C29 C28 C33 122.5(2) . . ? C29 C28 N3 118.26(19) . . ? C33 C28 N3 119.01(19) . . ? C30 C29 C28 117.4(2) . . ? C30 C29 C34 120.6(2) . . ? C28 C29 C34 122.0(2) . . ? C31 C30 C29 121.4(2) . . ? C30 C31 C32 120.0(2) . . ? C31 C32 C33 121.0(2) . . ? C28 C33 C32 117.7(2) . . ? C28 C33 C35 122.5(2) . . ? C32 C33 C35 119.8(2) . . ? Cl6 C36 Cl5 113.1(8) . . ? Cl5' C36' Cl6' 108.7(8) . . ? 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 N2 Sn1 N1 C1 -5.00(16) . . . . ? N3 Sn1 N1 C1 -16.1(2) . . . . ? Cl1 Sn1 N1 C1 -98.86(16) . . . . ? N2 Sn1 N1 C20 175.96(19) . . . . ? N3 Sn1 N1 C20 164.86(15) . . . . ? Cl1 Sn1 N1 C20 82.10(17) . . . . ? N1 Sn1 N2 C2 6.20(14) . . . . ? N3 Sn1 N2 C2 178.01(17) . . . . ? Cl1 Sn1 N2 C2 90.84(15) . . . . ? N1 Sn1 N2 C6 175.17(17) . . . . ? N3 Sn1 N2 C6 -13.02(14) . . . . ? Cl1 Sn1 N2 C6 -100.19(15) . . . . ? N2 Sn1 N3 C7 18.73(15) . . . . ? N1 Sn1 N3 C7 29.9(2) . . . . ? Cl1 Sn1 N3 C7 111.72(15) . . . . ? N2 Sn1 N3 C28 174.12(16) . . . . ? N1 Sn1 N3 C28 -174.71(13) . . . . ? Cl1 Sn1 N3 C28 -92.90(14) . . . . ? C20 N1 C1 C8 3.3(4) . . . . ? Sn1 N1 C1 C8 -175.62(16) . . . . ? C20 N1 C1 C2 -177.7(2) . . . . ? Sn1 N1 C1 C2 3.3(2) . . . . ? C6 N2 C2 C3 0.7(3) . . . . ? Sn1 N2 C2 C3 169.70(16) . . . . ? C6 N2 C2 C1 -175.93(18) . . . . ? Sn1 N2 C2 C1 -7.0(2) . . . . ? N1 C1 C2 N2 2.2(3) . . . . ? C8 C1 C2 N2 -178.79(19) . . . . ? N1 C1 C2 C3 -174.4(2) . . . . ? C8 C1 C2 C3 4.6(3) . . . . ? N2 C2 C3 C4 1.6(3) . . . . ? C1 C2 C3 C4 178.0(2) . . . . ? C2 C3 C4 C5 -1.7(4) . . . . ? C3 C4 C5 C6 -0.3(4) . . . . ? C2 N2 C6 C5 -2.8(3) . . . . ? Sn1 N2 C6 C5 -171.78(16) . . . . ? C2 N2 C6 C7 176.35(18) . . . . ? Sn1 N2 C6 C7 7.4(2) . . . . ? C4 C5 C6 N2 2.6(3) . . . . ? C4 C5 C6 C7 -176.5(2) . . . . ? C28 N3 C7 C6 -175.23(18) . . . . ? Sn1 N3 C7 C6 -21.7(2) . . . . ? C28 N3 C7 C14 1.5(3) . . . . ? Sn1 N3 C7 C14 155.00(16) . . . . ? N2 C6 C7 N3 10.3(3) . . . . ? C5 C6 C7 N3 -170.5(2) . . . . ? N2 C6 C7 C14 -166.55(19) . . . . ? C5 C6 C7 C14 12.6(3) . . . . ? N1 C1 C8 C13 -120.5(2) . . . . ? C2 C1 C8 C13 60.6(3) . . . . ? N1 C1 C8 C9 58.3(3) . . . . ? C2 C1 C8 C9 -120.6(2) . . . . ? C13 C8 C9 C10 0.8(3) . . . . ? C1 C8 C9 C10 -178.0(2) . . . . ? C8 C9 C10 C11 0.9(4) . . . . ? C9 C10 C11 C12 -1.2(4) . . . . ? C10 C11 C12 C13 -0.2(4) . . . . ? C9 C8 C13 C12 -2.2(3) . . . . ? C1 C8 C13 C12 176.6(2) . . . . ? C11 C12 C13 C8 1.9(4) . . . . ? N3 C7 C14 C19 -121.3(2) . . . . ? C6 C7 C14 C19 55.3(3) . . . . ? N3 C7 C14 C15 53.8(3) . . . . ? C6 C7 C14 C15 -129.6(2) . . . . ? C19 C14 C15 C16 2.4(4) . . . . ? C7 C14 C15 C16 -172.7(2) . . . . ? C14 C15 C16 C17 -0.3(4) . . . . ? C15 C16 C17 C18 -1.8(4) . . . . ? C16 C17 C18 C19 1.8(4) . . . . ? C15 C14 C19 C18 -2.5(4) . . . . ? C7 C14 C19 C18 172.6(2) . . . . ? C17 C18 C19 C14 0.4(4) . . . . ? C1 N1 C20 C25 -110.9(3) . . . . ? Sn1 N1 C20 C25 68.1(3) . . . . ? C1 N1 C20 C21 74.8(3) . . . . ? Sn1 N1 C20 C21 -106.3(2) . . . . ? C25 C20 C21 C22 -0.4(4) . . . . ? N1 C20 C21 C22 173.6(2) . . . . ? C25 C20 C21 C26 179.9(3) . . . . ? N1 C20 C21 C26 -6.1(4) . . . . ? C20 C21 C22 C23 -0.7(5) . . . . ? C26 C21 C22 C23 179.0(3) . . . . ? C21 C22 C23 C24 1.3(6) . . . . ? C22 C23 C24 C25 -0.8(6) . . . . ? C21 C20 C25 C24 0.9(4) . . . . ? N1 C20 C25 C24 -173.2(2) . . . . ? C21 C20 C25 C27 -177.5(3) . . . . ? N1 C20 C25 C27 8.4(4) . . . . ? C23 C24 C25 C20 -0.3(5) . . . . ? C23 C24 C25 C27 178.2(3) . . . . ? C7 N3 C28 C29 -105.4(2) . . . . ? Sn1 N3 C28 C29 101.02(18) . . . . ? C7 N3 C28 C33 79.7(3) . . . . ? Sn1 N3 C28 C33 -73.8(2) . . . . ? C33 C28 C29 C30 -1.0(3) . . . . ? N3 C28 C29 C30 -175.7(2) . . . . ? C33 C28 C29 C34 -179.4(2) . . . . ? N3 C28 C29 C34 5.9(3) . . . . ? C28 C29 C30 C31 1.2(4) . . . . ? C34 C29 C30 C31 179.6(2) . . . . ? C29 C30 C31 C32 -0.6(4) . . . . ? C30 C31 C32 C33 -0.2(4) . . . . ? C29 C28 C33 C32 0.3(3) . . . . ? N3 C28 C33 C32 174.90(19) . . . . ? C29 C28 C33 C35 -179.0(2) . . . . ? N3 C28 C33 C35 -4.4(3) . . . . ? C31 C32 C33 C28 0.3(3) . . . . ? C31 C32 C33 C35 179.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.139 _refine_diff_density_min -1.217 _refine_diff_density_rms 0.073 _database_code_depnum_ccdc_archive 'CCDC 909101'