data_a _audit_creation_date 2017-05-17 _audit_creation_method ; Olex2 1.2-beta (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '2(C32 H37 S)' _chemical_formula_sum 'C64 H74 S2' _chemical_formula_weight 907.35 _chemical_melting_point ? 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.640(3) _cell_length_b 15.198(4) _cell_length_c 18.576(6) _cell_angle_alpha 106.712(5) _cell_angle_beta 93.358(5) _cell_angle_gamma 107.192(5) _cell_volume 2714.5(13) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2753 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 20.89 _cell_measurement_theta_min 2.32 _shelx_estimated_absorpt_T_max 0.992 _shelx_estimated_absorpt_T_min 0.945 _exptl_absorpt_coefficient_mu 0.136 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6440 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0899 before and 0.0465 after correction. The Ratio of minimum to maximum transmission is 0.8636. The \l/2 correction factor is 0.0015. ; _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.110 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 980 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.06 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_unetI/netI 0.0853 _diffrn_reflns_Laue_measured_fraction_full 0.986 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 13990 _diffrn_reflns_point_group_measured_fraction_full 0.986 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 25.099 _diffrn_reflns_theta_max 25.099 _diffrn_reflns_theta_min 2.029 _diffrn_ambient_temperature 296.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5195 _reflns_number_total 9546 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL-2014/7 (Sheldrick, 2008)' _computing_structure_solution 'ShelXS-1997 (Sheldrick, 2008)' _refine_diff_density_max 0.798 _refine_diff_density_min -1.112 _refine_diff_density_rms 0.108 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 521 _refine_ls_number_reflns 9546 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1687 _refine_ls_R_factor_gt 0.1133 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3058 _refine_ls_wR_factor_ref 0.3610 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C50-C51 = C62-C63 = C63-C64 = C29-C30 = C19-C20 1.53 with sigma of 0.01 C51-C52 = C49-C50 = C28-C29 1.53 with sigma of 0.01 3. Rigid bond restraints C29, C30 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C50, C51, C52 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C27, C28 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints : with sigma of 0.01 and sigma for terminal atoms of 0.02 5. Others Fixed Uiso: C20(0.1493) C30(0.1822) C31(0.18389) C32(0.19185) C50(0.1453) C51(0.1636) C52(0.16544) C62(0.17378) C63(0.21821) C64(0.18896) 6.a Secondary CH2 refined with riding coordinates: C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A, H19B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A, H62B), C63(H63A,H63B) 6.b Me refined with riding coordinates: C20(H20A,H20B,H20C), C52(H52A,H52B,H52C), C64(H64A,H64B,H64C) 6.c Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C6(H6), C10(H10), C11(H11), C13(H13), C14(H14), C22(H22), C23(H23), C25(H25), C26(H26), C33(H33), C34(H34), C39(H39), C42(H42), C43(H43), C45(H45), C46(H46), C54(H54), C55(H55), C57(H57), C58(H58) 6.d Idealised Me refined as rotating group: C32(H32A,H32B,H32C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? 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 S1 S 0.64436(12) 0.46150(10) 1.10095(7) 0.0547(4) Uani 1 1 d . . . . . S2 S 0.28121(12) -0.15236(9) 0.49317(8) 0.0567(4) Uani 1 1 d . . . . . C1 C 0.5013(4) 0.4003(4) 1.0370(3) 0.0537(13) Uani 1 1 d . . . . . H1 H 0.4170 0.3865 1.0511 0.064 Uiso 1 1 calc R . . . . C2 C 0.5222(4) 0.3736(4) 0.9634(3) 0.0501(12) Uani 1 1 d . . . . . H2 H 0.4550 0.3395 0.9217 0.060 Uiso 1 1 calc R . . . . C3 C 0.6615(4) 0.4050(3) 0.9588(3) 0.0428(11) Uani 1 1 d . . . . . C4 C 0.7371(4) 0.4526(3) 1.0290(2) 0.0397(11) Uani 1 1 d . . . . . C5 C 0.8780(4) 0.4834(3) 1.0225(2) 0.0394(10) Uani 1 1 d . . . . . C6 C 0.9906(4) 0.5307(3) 1.0777(2) 0.0414(11) Uani 1 1 d . . . . . H6 H 0.9829 0.5512 1.1290 0.050 Uiso 1 1 calc R . . . . C7 C 1.1125(4) 0.5463(3) 1.0553(3) 0.0398(10) Uani 1 1 d . . . . . C8 C 0.7473(4) 0.4030(3) 0.8956(2) 0.0406(11) Uani 1 1 d . . . . . C9 C 0.7359(4) 0.3013(3) 0.8447(3) 0.0451(12) Uani 1 1 d . . . . . C10 C 0.6742(6) 0.2181(4) 0.8623(3) 0.0612(14) Uani 1 1 d . . . . . H10 H 0.6348 0.2222 0.9060 0.073 Uiso 1 1 calc R . . . . C11 C 0.6712(6) 0.1277(4) 0.8142(4) 0.0755(18) Uani 1 1 d . . . . . H11 H 0.6262 0.0720 0.8255 0.091 Uiso 1 1 calc R . . . . C12 C 0.7336(5) 0.1183(4) 0.7497(3) 0.0612(15) Uani 1 1 d . . . . . C13 C 0.7907(6) 0.2005(4) 0.7330(3) 0.0614(15) Uani 1 1 d . . . . . H13 H 0.8305 0.1966 0.6894 0.074 Uiso 1 1 calc R . . . . C14 C 0.7915(5) 0.2907(4) 0.7792(3) 0.0547(13) Uani 1 1 d . . . . . H14 H 0.8308 0.3454 0.7653 0.066 Uiso 1 1 calc R . . . . C15 C 0.7361(6) 0.0199(4) 0.7025(4) 0.0721(17) Uani 1 1 d . . . . . H15A H 0.7423 0.0193 0.6505 0.087 Uiso 1 1 calc R . . . . H15B H 0.6533 -0.0292 0.7021 0.087 Uiso 1 1 calc R . . . . C16 C 0.8522(6) -0.0056(4) 0.7326(4) 0.0751(18) Uani 1 1 d . . . . . H16A H 0.9338 0.0480 0.7397 0.090 Uiso 1 1 calc R . . . . H16B H 0.8395 -0.0133 0.7820 0.090 Uiso 1 1 calc R . . . . C17 C 0.8682(8) -0.0980(5) 0.6805(4) 0.095(2) Uani 1 1 d . . . . . H17A H 0.7828 -0.1494 0.6674 0.114 Uiso 1 1 calc R . . . . H17B H 0.8940 -0.0868 0.6338 0.114 Uiso 1 1 calc R . . . . C18 C 0.9665(9) -0.1304(6) 0.7139(6) 0.134(4) Uani 1 1 d . . . . . H18A H 0.9344 -0.1550 0.7544 0.161 Uiso 1 1 calc R . . . . H18B H 1.0497 -0.0773 0.7344 0.161 Uiso 1 1 calc R . . . . C19 C 0.9897(13) -0.2259(11) 0.6368(9) 0.206(6) Uiso 1 1 d D . . . . H19A H 0.9187 -0.2870 0.6276 0.248 Uiso 1 1 calc R . . . . H19B H 0.9932 -0.2091 0.5902 0.248 Uiso 1 1 calc R . . . . C20 C 1.1218(10) -0.2318(8) 0.6654(7) 0.149 Uiso 1 1 d D . . . . H20A H 1.1433 -0.2813 0.6280 0.224 Uiso 1 1 calc R . . . . H20B H 1.1900 -0.1703 0.6747 0.224 Uiso 1 1 calc R . . . . H20C H 1.1161 -0.2476 0.7119 0.224 Uiso 1 1 calc R . . . . C21 C 0.7114(4) 0.4618(3) 0.8472(3) 0.0427(11) Uani 1 1 d . . . . . C22 C 0.5868(5) 0.4276(4) 0.8045(3) 0.0519(13) Uani 1 1 d . . . . . H22 H 0.5271 0.3691 0.8050 0.062 Uiso 1 1 calc R . . . . C23 C 0.5476(6) 0.4779(4) 0.7609(3) 0.0614(15) Uani 1 1 d . . . . . H23 H 0.4617 0.4536 0.7337 0.074 Uiso 1 1 calc R . . . . C24 C 0.6343(7) 0.5633(5) 0.7572(3) 0.0714(17) Uani 1 1 d . . . . . C25 C 0.7598(7) 0.5963(5) 0.7999(4) 0.085(2) Uani 1 1 d . . . . . H25 H 0.8216 0.6529 0.7976 0.102 Uiso 1 1 calc R . . . . C26 C 0.7966(5) 0.5481(4) 0.8459(4) 0.0659(16) Uani 1 1 d . . . . . H26 H 0.8800 0.5747 0.8761 0.079 Uiso 1 1 calc R . . . . C27 C 0.5966(9) 0.6185(6) 0.7093(4) 0.104(2) Uani 1 1 d . U . . . H27A H 0.6769 0.6573 0.6965 0.124 Uiso 1 1 calc R . . . . H27B H 0.5418 0.5726 0.6622 0.124 Uiso 1 1 calc R . . . . C28 C 0.5216(13) 0.6847(9) 0.7479(7) 0.166(4) Uiso 1 1 d D U . . . H28A H 0.4986 0.7156 0.7125 0.199 Uiso 1 1 calc R . . . . H28B H 0.4388 0.6445 0.7573 0.199 Uiso 1 1 calc R . . . . C29 C 0.5904(14) 0.7626(8) 0.8214(7) 0.188(5) Uani 1 1 d D U . . . H29A H 0.6802 0.7964 0.8156 0.225 Uiso 1 1 calc R . . . . H29B H 0.5967 0.7331 0.8608 0.225 Uiso 1 1 calc R . . . . C30 C 0.5156(13) 0.8360(9) 0.8458(8) 0.182 Uiso 1 1 d D U . . . H30A H 0.4957 0.8592 0.8044 0.219 Uiso 1 1 calc R . . . . H30B H 0.4331 0.8074 0.8626 0.219 Uiso 1 1 calc R . . . . C31 C 0.6086(14) 0.9142(10) 0.9083(8) 0.184 Uiso 1 1 d . U . . . H31A H 0.6000 0.9764 0.9095 0.221 Uiso 1 1 calc R . . . . H31B H 0.6995 0.9165 0.9029 0.221 Uiso 1 1 calc R . . . . C32 C 0.5688(13) 0.8891(10) 0.9865(8) 0.192 Uiso 1 1 d . U . . . H32A H 0.5336 0.9368 1.0160 0.288 Uiso 1 1 calc GR . . . . H32B H 0.6468 0.8902 1.0159 0.288 Uiso 1 1 calc GR . . . . H32C H 0.5030 0.8258 0.9730 0.288 Uiso 1 1 calc GR . . . . C33 C 0.4270(5) -0.0862(4) 0.5555(3) 0.0624(15) Uani 1 1 d . . . . . H33 H 0.4967 -0.1101 0.5609 0.075 Uiso 1 1 calc R . . . . C34 C 0.4300(4) 0.0038(4) 0.5956(3) 0.0508(12) Uani 1 1 d . . . . . H34 H 0.5020 0.0492 0.6312 0.061 Uiso 1 1 calc R . . . . C35 C 0.3122(4) 0.0208(3) 0.5775(2) 0.0421(11) Uani 1 1 d . . . . . C36 C 0.2226(4) -0.0571(3) 0.5226(3) 0.0428(11) Uani 1 1 d . . . . . C37 C 0.1011(4) -0.0375(3) 0.5044(2) 0.0394(10) Uani 1 1 d . . . . . C38 C 0.1184(4) 0.0589(3) 0.5493(2) 0.0408(11) Uani 1 1 d . . . . . C39 C 0.0167(4) 0.0965(3) 0.5452(3) 0.0439(11) Uani 1 1 d . . . . . H39 H 0.0260 0.1596 0.5746 0.053 Uiso 1 1 calc R . . . . C40 C 0.2579(4) 0.1068(3) 0.5991(3) 0.0423(11) Uani 1 1 d . . . . . C41 C 0.3503(4) 0.1901(3) 0.5772(3) 0.0447(11) Uani 1 1 d . . . . . C42 C 0.3144(5) 0.2191(4) 0.5176(3) 0.0598(14) Uani 1 1 d . . . . . H42 H 0.2299 0.1886 0.4888 0.072 Uiso 1 1 calc R . . . . C43 C 0.4056(6) 0.2946(5) 0.5009(4) 0.0796(18) Uani 1 1 d . . . . . H43 H 0.3810 0.3131 0.4601 0.095 Uiso 1 1 calc R . . . . C44 C 0.5300(6) 0.3424(4) 0.5423(4) 0.0723(17) Uani 1 1 d . . . . . C45 C 0.5655(5) 0.3124(4) 0.6008(4) 0.0650(16) Uani 1 1 d . . . . . H45 H 0.6507 0.3427 0.6288 0.078 Uiso 1 1 calc R . . . . C46 C 0.4777(5) 0.2384(4) 0.6189(3) 0.0570(14) Uani 1 1 d . . . . . H46 H 0.5036 0.2203 0.6597 0.068 Uiso 1 1 calc R . . . . C47 C 0.6241(8) 0.4265(6) 0.5222(7) 0.121(3) Uani 1 1 d . . . . . H47A H 0.5710 0.4607 0.5049 0.145 Uiso 1 1 calc R . . . . H47B H 0.6827 0.4715 0.5684 0.145 Uiso 1 1 calc R . . . . C48 C 0.7027(11) 0.4033(7) 0.4674(7) 0.145(4) Uani 1 1 d . . . . . H48A H 0.6481 0.3634 0.4187 0.174 Uiso 1 1 calc R . . . . H48B H 0.7577 0.3688 0.4823 0.174 Uiso 1 1 calc R . . . . C49 C 0.7929(13) 0.5065(9) 0.4633(7) 0.185(5) Uiso 1 1 d D . . . . H49A H 0.7427 0.5515 0.4709 0.221 Uiso 1 1 calc R . . . . H49B H 0.8710 0.5342 0.5024 0.221 Uiso 1 1 calc R . . . . C50 C 0.8327(11) 0.4885(7) 0.3868(6) 0.145 Uiso 1 1 d D U . . . H50A H 0.7561 0.4648 0.3471 0.174 Uiso 1 1 calc R . . . . H50B H 0.8816 0.4427 0.3778 0.174 Uiso 1 1 calc R . . . . C51 C 0.9224(12) 0.5913(8) 0.3922(7) 0.164 Uiso 1 1 d D U . . . H51A H 0.8768 0.6389 0.4058 0.196 Uiso 1 1 calc R . . . . H51B H 1.0047 0.6125 0.4272 0.196 Uiso 1 1 calc R . . . . C52 C 0.9440(12) 0.5688(9) 0.3118(6) 0.165 Uiso 1 1 d D U . . . H52A H 1.0001 0.6266 0.3039 0.248 Uiso 1 1 calc R . . . . H52B H 0.9861 0.5197 0.3002 0.248 Uiso 1 1 calc R . . . . H52C H 0.8598 0.5458 0.2791 0.248 Uiso 1 1 calc R . . . . C53 C 0.2415(4) 0.1409(4) 0.6831(3) 0.0466(12) Uani 1 1 d . . . . . C54 C 0.2611(6) 0.0947(5) 0.7328(3) 0.0645(15) Uani 1 1 d . . . . . H54 H 0.2874 0.0399 0.7169 0.077 Uiso 1 1 calc R . . . . C55 C 0.2416(6) 0.1297(5) 0.8086(3) 0.0748(17) Uani 1 1 d . . . . . H55 H 0.2566 0.0978 0.8425 0.090 Uiso 1 1 calc R . . . . C56 C 0.2013(5) 0.2090(5) 0.8340(3) 0.0656(17) Uani 1 1 d . . . . . C57 C 0.1859(5) 0.2567(4) 0.7849(3) 0.0630(15) Uani 1 1 d . . . . . H57 H 0.1585 0.3109 0.8009 0.076 Uiso 1 1 calc R . . . . C58 C 0.2105(5) 0.2256(4) 0.7104(3) 0.0582(14) Uani 1 1 d . . . . . H58 H 0.2061 0.2623 0.6786 0.070 Uiso 1 1 calc R . . . . C59 C 0.1735(6) 0.2429(5) 0.9149(3) 0.085(2) Uani 1 1 d . . . . . H59A H 0.2333 0.2295 0.9486 0.102 Uiso 1 1 calc R . . . . H59B H 0.1915 0.3127 0.9308 0.102 Uiso 1 1 calc R . . . . C60 C 0.0326(7) 0.1941(7) 0.9222(4) 0.112(3) Uani 1 1 d . . . . . H60A H 0.0140 0.1243 0.9046 0.135 Uiso 1 1 calc R . . . . H60B H -0.0268 0.2091 0.8895 0.135 Uiso 1 1 calc R . . . . C61 C 0.0032(10) 0.2243(8) 1.0030(5) 0.158(5) Uani 1 1 d . . . . . H61A H 0.0811 0.2324 1.0373 0.190 Uiso 1 1 calc R . . . . H61B H -0.0086 0.2874 1.0135 0.190 Uiso 1 1 calc R . . . . C62 C -0.1102(13) 0.1605(9) 1.0213(7) 0.174 Uiso 1 1 d D . . . . H62A H -0.1005 0.0966 1.0082 0.209 Uiso 1 1 calc R . . . . H62B H -0.1886 0.1549 0.9885 0.209 Uiso 1 1 calc R . . . . C63 C -0.1378(16) 0.1875(11) 1.1036(8) 0.218 Uiso 1 1 d D . . . . H63A H -0.2155 0.1376 1.1080 0.262 Uiso 1 1 calc R . . . . H63B H -0.0625 0.1902 1.1372 0.262 Uiso 1 1 calc R . . . . C64 C -0.1612(13) 0.2848(9) 1.1280(8) 0.189 Uiso 1 1 d D . . . . H64A H -0.1781 0.2994 1.1796 0.283 Uiso 1 1 calc R . . . . H64B H -0.0838 0.3346 1.1245 0.283 Uiso 1 1 calc R . . . . H64C H -0.2367 0.2820 1.0954 0.283 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0355(7) 0.0744(9) 0.0448(7) 0.0072(6) 0.0100(5) 0.0152(6) S2 0.0452(7) 0.0574(8) 0.0616(9) -0.0018(6) -0.0025(6) 0.0305(6) C1 0.027(2) 0.067(3) 0.062(3) 0.015(3) 0.011(2) 0.012(2) C2 0.031(2) 0.053(3) 0.053(3) 0.003(2) 0.003(2) 0.011(2) C3 0.026(2) 0.047(3) 0.048(3) 0.010(2) 0.0025(19) 0.007(2) C4 0.023(2) 0.047(3) 0.039(2) 0.002(2) 0.0023(18) 0.0084(19) C5 0.031(2) 0.047(3) 0.036(2) 0.003(2) 0.0038(18) 0.017(2) C6 0.030(2) 0.053(3) 0.032(2) 0.003(2) 0.0021(18) 0.011(2) C7 0.030(2) 0.045(3) 0.038(2) 0.003(2) 0.0027(18) 0.014(2) C8 0.031(2) 0.046(3) 0.037(2) 0.003(2) 0.0004(19) 0.012(2) C9 0.027(2) 0.052(3) 0.045(3) 0.001(2) -0.0067(19) 0.014(2) C10 0.068(4) 0.048(3) 0.064(4) 0.009(3) 0.019(3) 0.020(3) C11 0.067(4) 0.051(3) 0.093(5) 0.009(3) 0.007(4) 0.012(3) C12 0.050(3) 0.061(4) 0.056(3) -0.010(3) -0.013(3) 0.025(3) C13 0.067(4) 0.065(4) 0.044(3) -0.003(3) 0.002(3) 0.031(3) C14 0.056(3) 0.061(3) 0.042(3) 0.005(2) 0.009(2) 0.025(3) C15 0.070(4) 0.064(4) 0.064(4) -0.006(3) -0.013(3) 0.027(3) C16 0.071(4) 0.060(4) 0.077(4) -0.010(3) -0.005(3) 0.031(3) C17 0.105(6) 0.076(4) 0.095(5) -0.005(4) 0.017(4) 0.047(4) C18 0.113(7) 0.102(6) 0.175(10) -0.004(6) -0.007(6) 0.068(6) C21 0.034(2) 0.048(3) 0.040(3) 0.001(2) 0.0017(19) 0.016(2) C22 0.046(3) 0.060(3) 0.042(3) 0.003(2) -0.001(2) 0.021(2) C23 0.058(3) 0.080(4) 0.045(3) 0.005(3) 0.001(3) 0.036(3) C24 0.079(4) 0.086(5) 0.056(4) 0.015(3) 0.003(3) 0.045(4) C25 0.082(5) 0.072(4) 0.103(5) 0.040(4) -0.002(4) 0.019(4) C26 0.047(3) 0.066(4) 0.076(4) 0.025(3) -0.005(3) 0.006(3) C27 0.137(7) 0.124(6) 0.077(5) 0.041(4) 0.013(5) 0.073(5) C29 0.264(16) 0.138(9) 0.210(14) 0.067(9) 0.046(13) 0.124(11) C33 0.042(3) 0.078(4) 0.068(4) 0.012(3) -0.003(3) 0.034(3) C34 0.034(2) 0.059(3) 0.051(3) 0.003(2) -0.007(2) 0.019(2) C35 0.034(2) 0.054(3) 0.037(2) 0.006(2) 0.0012(19) 0.022(2) C36 0.033(2) 0.045(3) 0.045(3) 0.000(2) -0.003(2) 0.019(2) C37 0.030(2) 0.051(3) 0.035(2) 0.005(2) 0.0012(18) 0.020(2) C38 0.031(2) 0.048(3) 0.037(2) 0.001(2) 0.0000(19) 0.017(2) C39 0.033(2) 0.048(3) 0.043(3) -0.003(2) -0.001(2) 0.020(2) C40 0.032(2) 0.047(3) 0.039(3) 0.000(2) -0.0022(19) 0.016(2) C41 0.031(2) 0.052(3) 0.043(3) 0.000(2) 0.001(2) 0.018(2) C42 0.048(3) 0.067(4) 0.061(3) 0.016(3) 0.001(3) 0.019(3) C43 0.069(4) 0.080(4) 0.096(5) 0.040(4) 0.007(4) 0.023(4) C44 0.061(4) 0.058(4) 0.097(5) 0.019(3) 0.021(4) 0.022(3) C45 0.035(3) 0.063(4) 0.078(4) 0.002(3) 0.014(3) 0.008(3) C46 0.037(3) 0.060(3) 0.056(3) -0.005(3) -0.006(2) 0.014(2) C47 0.087(6) 0.089(6) 0.188(10) 0.063(6) 0.034(6) 0.011(5) C48 0.151(9) 0.113(7) 0.165(9) 0.059(7) 0.081(8) 0.007(6) C53 0.032(2) 0.058(3) 0.037(3) 0.001(2) -0.0020(19) 0.011(2) C54 0.063(3) 0.087(4) 0.050(3) 0.020(3) 0.008(3) 0.035(3) C55 0.078(4) 0.095(5) 0.050(3) 0.021(3) 0.005(3) 0.030(4) C56 0.033(3) 0.091(4) 0.047(3) -0.004(3) 0.002(2) 0.008(3) C57 0.056(3) 0.071(4) 0.046(3) -0.008(3) 0.006(3) 0.024(3) C58 0.054(3) 0.063(3) 0.049(3) 0.001(3) -0.001(2) 0.023(3) C59 0.063(4) 0.122(6) 0.042(3) 0.002(3) 0.012(3) 0.012(4) C60 0.070(5) 0.149(7) 0.072(5) -0.007(5) 0.014(4) 0.008(5) C61 0.108(7) 0.176(9) 0.105(7) -0.037(6) 0.053(6) -0.004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.705(5) . ? S1 C4 1.706(4) . ? S2 C33 1.719(5) . ? S2 C36 1.704(4) . ? C1 H1 0.9300 . ? C1 C2 1.361(7) . ? C2 H2 0.9300 . ? C2 C3 1.433(6) . ? C3 C4 1.363(6) . ? C3 C8 1.528(6) . ? C4 C5 1.455(6) . ? C5 C6 1.387(6) . ? C5 C7 1.404(6) 2_767 ? C6 H6 0.9300 . ? C6 C7 1.360(6) . ? C7 C5 1.404(6) 2_767 ? C7 C8 1.552(6) 2_767 ? C8 C7 1.552(6) 2_767 ? C8 C9 1.528(6) . ? C8 C21 1.542(7) . ? C9 C10 1.382(7) . ? C9 C14 1.374(7) . ? C10 H10 0.9300 . ? C10 C11 1.396(8) . ? C11 H11 0.9300 . ? C11 C12 1.396(9) . ? C12 C13 1.349(8) . ? C12 C15 1.510(7) . ? C13 H13 0.9300 . ? C13 C14 1.390(7) . ? C14 H14 0.9300 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 C16 1.522(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 C17 1.521(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 C18 1.458(10) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 C19 1.810(16) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 C20 1.510(9) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.374(6) . ? C21 C26 1.365(7) . ? C22 H22 0.9300 . ? C22 C23 1.386(8) . ? C23 H23 0.9300 . ? C23 C24 1.375(9) . ? C24 C25 1.384(8) . ? C24 C27 1.499(9) . ? C25 H25 0.9300 . ? C25 C26 1.380(8) . ? C26 H26 0.9300 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 C28 1.513(14) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 C29 1.497(9) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 C30 1.537(9) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 C31 1.454(15) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 C32 1.653(18) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33 0.9300 . ? C33 C34 1.347(7) . ? C34 H34 0.9300 . ? C34 C35 1.393(6) . ? C35 C36 1.370(6) . ? C35 C40 1.542(6) . ? C36 C37 1.452(6) . ? C37 C38 1.413(6) . ? C37 C39 1.395(6) 2_556 ? C38 C39 1.373(6) . ? C38 C40 1.550(6) . ? C39 C37 1.395(6) 2_556 ? C39 H39 0.9300 . ? C40 C41 1.531(7) . ? C40 C53 1.535(6) . ? C41 C42 1.376(7) . ? C41 C46 1.393(6) . ? C42 H42 0.9300 . ? C42 C43 1.392(8) . ? C43 H43 0.9300 . ? C43 C44 1.365(9) . ? C44 C45 1.366(9) . ? C44 C47 1.530(10) . ? C45 H45 0.9300 . ? C45 C46 1.373(8) . ? C46 H46 0.9300 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 C48 1.387(12) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 C49 1.605(14) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C49 C50 1.480(8) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C50 C51 1.542(8) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 C52 1.481(8) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.350(8) . ? C53 C58 1.384(7) . ? C54 H54 0.9300 . ? C54 C55 1.407(8) . ? C55 H55 0.9300 . ? C55 C56 1.363(9) . ? C56 C57 1.348(8) . ? C56 C59 1.520(8) . ? C57 H57 0.9300 . ? C57 C58 1.395(7) . ? C58 H58 0.9300 . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C59 C60 1.497(9) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C60 C61 1.518(11) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C61 C62 1.434(13) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C62 C63 1.534(9) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C63 C64 1.516(9) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C4 90.6(2) . . ? C36 S2 C33 90.1(2) . . ? S1 C1 H1 123.2 . . ? C2 C1 S1 113.7(3) . . ? C2 C1 H1 123.2 . . ? C1 C2 H2 124.6 . . ? C1 C2 C3 110.9(4) . . ? C3 C2 H2 124.6 . . ? C2 C3 C8 136.6(4) . . ? C4 C3 C2 111.9(4) . . ? C4 C3 C8 111.5(4) . . ? C3 C4 S1 113.0(3) . . ? C3 C4 C5 110.6(4) . . ? C5 C4 S1 136.4(3) . . ? C6 C5 C4 131.3(4) . . ? C6 C5 C7 121.5(4) . 2_767 ? C7 C5 C4 107.2(4) 2_767 . ? C5 C6 H6 120.6 . . ? C7 C6 C5 118.7(4) . . ? C7 C6 H6 120.6 . . ? C5 C7 C8 111.0(4) 2_767 2_767 ? C6 C7 C5 119.8(4) . 2_767 ? C6 C7 C8 129.2(4) . 2_767 ? C3 C8 C7 99.5(3) . 2_767 ? C3 C8 C9 114.7(4) . . ? C3 C8 C21 108.6(4) . . ? C9 C8 C7 110.3(3) . 2_767 ? C9 C8 C21 110.1(4) . . ? C21 C8 C7 113.3(4) . 2_767 ? C10 C9 C8 123.0(4) . . ? C10 C9 C14 117.5(5) . . ? C14 C9 C8 119.5(4) . . ? C9 C10 H10 120.1 . . ? C9 C10 C11 119.8(5) . . ? C11 C10 H10 120.1 . . ? C10 C11 H11 118.9 . . ? C10 C11 C12 122.1(6) . . ? C12 C11 H11 118.9 . . ? C11 C12 C15 120.3(6) . . ? C13 C12 C11 116.8(5) . . ? C13 C12 C15 122.9(6) . . ? C12 C13 H13 119.1 . . ? C12 C13 C14 121.7(5) . . ? C14 C13 H13 119.1 . . ? C9 C14 C13 121.9(5) . . ? C9 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C12 C15 H15A 109.1 . . ? C12 C15 H15B 109.1 . . ? C12 C15 C16 112.4(4) . . ? H15A C15 H15B 107.8 . . ? C16 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? C15 C16 H16A 108.8 . . ? C15 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C17 C16 C15 113.6(5) . . ? C17 C16 H16A 108.8 . . ? C17 C16 H16B 108.8 . . ? C16 C17 H17A 108.8 . . ? C16 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C18 C17 C16 113.8(6) . . ? C18 C17 H17A 108.8 . . ? C18 C17 H17B 108.8 . . ? C17 C18 H18A 110.6 . . ? C17 C18 H18B 110.6 . . ? C17 C18 C19 105.5(8) . . ? H18A C18 H18B 108.8 . . ? C19 C18 H18A 110.6 . . ? C19 C18 H18B 110.6 . . ? C18 C19 H19A 111.2 . . ? C18 C19 H19B 111.1 . . ? H19A C19 H19B 109.1 . . ? C20 C19 C18 103.1(9) . . ? C20 C19 H19A 111.1 . . ? C20 C19 H19B 111.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C8 119.0(4) . . ? C26 C21 C8 123.1(4) . . ? C26 C21 C22 117.8(5) . . ? C21 C22 H22 119.1 . . ? C21 C22 C23 121.8(5) . . ? C23 C22 H22 119.1 . . ? C22 C23 H23 119.7 . . ? C24 C23 C22 120.7(5) . . ? C24 C23 H23 119.7 . . ? C23 C24 C25 116.8(6) . . ? C23 C24 C27 122.2(6) . . ? C25 C24 C27 121.0(7) . . ? C24 C25 H25 118.8 . . ? C24 C25 C26 122.4(6) . . ? C26 C25 H25 118.8 . . ? C21 C26 C25 120.4(5) . . ? C21 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C24 C27 H27A 108.9 . . ? C24 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? C28 C27 C24 113.5(8) . . ? C28 C27 H27A 108.9 . . ? C28 C27 H27B 108.9 . . ? C27 C28 H28A 108.0 . . ? C27 C28 H28B 108.0 . . ? H28A C28 H28B 107.2 . . ? C29 C28 C27 117.4(10) . . ? C29 C28 H28A 108.0 . . ? C29 C28 H28B 108.0 . . ? C28 C29 H29A 109.3 . . ? C28 C29 H29B 109.3 . . ? C28 C29 C30 111.6(11) . . ? H29A C29 H29B 108.0 . . ? C30 C29 H29A 109.3 . . ? C30 C29 H29B 109.3 . . ? C29 C30 H30A 111.1 . . ? C29 C30 H30B 111.1 . . ? H30A C30 H30B 109.0 . . ? C31 C30 C29 103.4(11) . . ? C31 C30 H30A 111.1 . . ? C31 C30 H30B 111.1 . . ? C30 C31 H31A 110.6 . . ? C30 C31 H31B 110.6 . . ? C30 C31 C32 105.7(11) . . ? H31A C31 H31B 108.7 . . ? C32 C31 H31A 110.6 . . ? C32 C31 H31B 110.6 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? S2 C33 H33 123.4 . . ? C34 C33 S2 113.2(4) . . ? C34 C33 H33 123.4 . . ? C33 C34 H34 124.1 . . ? C33 C34 C35 111.8(4) . . ? C35 C34 H34 124.1 . . ? C34 C35 C40 137.0(4) . . ? C36 C35 C34 112.7(4) . . ? C36 C35 C40 110.2(4) . . ? C35 C36 S2 112.2(3) . . ? C35 C36 C37 111.7(4) . . ? C37 C36 S2 136.1(3) . . ? C38 C37 C36 106.9(4) . . ? C39 C37 C36 131.0(4) 2_556 . ? C39 C37 C38 122.1(4) 2_556 . ? C37 C38 C40 110.9(3) . . ? C39 C38 C37 119.7(4) . . ? C39 C38 C40 129.3(4) . . ? C37 C39 H39 120.9 2_556 . ? C38 C39 C37 118.2(4) . 2_556 ? C38 C39 H39 120.9 . . ? C35 C40 C38 100.1(3) . . ? C41 C40 C35 108.0(4) . . ? C41 C40 C38 114.1(4) . . ? C41 C40 C53 110.9(4) . . ? C53 C40 C35 114.2(4) . . ? C53 C40 C38 109.2(3) . . ? C42 C41 C40 123.3(4) . . ? C42 C41 C46 118.2(5) . . ? C46 C41 C40 118.5(5) . . ? C41 C42 H42 120.2 . . ? C41 C42 C43 119.5(5) . . ? C43 C42 H42 120.2 . . ? C42 C43 H43 118.9 . . ? C44 C43 C42 122.2(6) . . ? C44 C43 H43 118.9 . . ? C43 C44 C45 118.0(6) . . ? C43 C44 C47 119.5(7) . . ? C45 C44 C47 122.5(6) . . ? C44 C45 H45 119.4 . . ? C44 C45 C46 121.2(5) . . ? C46 C45 H45 119.4 . . ? C41 C46 H46 119.5 . . ? C45 C46 C41 120.9(6) . . ? C45 C46 H46 119.5 . . ? C44 C47 H47A 108.0 . . ? C44 C47 H47B 108.0 . . ? H47A C47 H47B 107.2 . . ? C48 C47 C44 117.2(7) . . ? C48 C47 H47A 108.0 . . ? C48 C47 H47B 108.0 . . ? C47 C48 H48A 110.9 . . ? C47 C48 H48B 110.9 . . ? C47 C48 C49 104.3(9) . . ? H48A C48 H48B 108.9 . . ? C49 C48 H48A 110.9 . . ? C49 C48 H48B 110.9 . . ? C48 C49 H49A 110.4 . . ? C48 C49 H49B 110.4 . . ? H49A C49 H49B 108.6 . . ? C50 C49 C48 106.7(9) . . ? C50 C49 H49A 110.4 . . ? C50 C49 H49B 110.4 . . ? C49 C50 H50A 111.6 . . ? C49 C50 H50B 111.6 . . ? C49 C50 C51 101.1(9) . . ? H50A C50 H50B 109.4 . . ? C51 C50 H50A 111.6 . . ? C51 C50 H50B 111.6 . . ? C50 C51 H51A 112.3 . . ? C50 C51 H51B 112.3 . . ? H51A C51 H51B 109.9 . . ? C52 C51 C50 97.3(9) . . ? C52 C51 H51A 112.3 . . ? C52 C51 H51B 112.3 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C40 123.3(5) . . ? C54 C53 C58 118.0(5) . . ? C58 C53 C40 118.6(5) . . ? C53 C54 H54 120.1 . . ? C53 C54 C55 119.8(6) . . ? C55 C54 H54 120.1 . . ? C54 C55 H55 119.0 . . ? C56 C55 C54 122.0(6) . . ? C56 C55 H55 119.0 . . ? C55 C56 C59 121.5(7) . . ? C57 C56 C55 118.0(5) . . ? C57 C56 C59 120.5(6) . . ? C56 C57 H57 119.6 . . ? C56 C57 C58 120.8(5) . . ? C58 C57 H57 119.6 . . ? C53 C58 C57 121.0(5) . . ? C53 C58 H58 119.5 . . ? C57 C58 H58 119.5 . . ? C56 C59 H59A 109.1 . . ? C56 C59 H59B 109.1 . . ? H59A C59 H59B 107.9 . . ? C60 C59 C56 112.3(5) . . ? C60 C59 H59A 109.1 . . ? C60 C59 H59B 109.1 . . ? C59 C60 H60A 108.9 . . ? C59 C60 H60B 108.9 . . ? C59 C60 C61 113.5(6) . . ? H60A C60 H60B 107.7 . . ? C61 C60 H60A 108.9 . . ? C61 C60 H60B 108.9 . . ? C60 C61 H61A 107.9 . . ? C60 C61 H61B 107.9 . . ? H61A C61 H61B 107.2 . . ? C62 C61 C60 117.4(8) . . ? C62 C61 H61A 107.9 . . ? C62 C61 H61B 107.9 . . ? C61 C62 H62A 107.8 . . ? C61 C62 H62B 107.8 . . ? C61 C62 C63 118.1(11) . . ? H62A C62 H62B 107.1 . . ? C63 C62 H62A 107.8 . . ? C63 C62 H62B 107.8 . . ? C62 C63 H63A 109.3 . . ? C62 C63 H63B 109.3 . . ? H63A C63 H63B 107.9 . . ? C64 C63 C62 111.7(12) . . ? C64 C63 H63A 109.3 . . ? C64 C63 H63B 109.3 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64B 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? _shelx_SHELXL_version_number '2014/7' _iucr_refine_instructions_details ; a.res created by SHELXL-2014/7 TITL A in P-1 CELL 0.71073 10.6399 15.1981 18.5765 106.712 93.358 107.192 ZERR 2 0.0029 0.0042 0.0055 0.005 0.005 0.005 LATT 1 SFAC C H S UNIT 128 148 4 DFIX 1.53 0.01 C50 C51 C62 C63 C63 C64 C29 C30 C19 C20 DFIX 1.53 0.01 C51 C52 C49 C50 C28 C29 DELU C29 C30 DELU C50 C51 C52 DELU C27 C28 ISOR 0.01 0.02 C32 C31 L.S. 20 PLAN 20 SIZE 0.42 0.28 0.06 TEMP 23 BOND $H HTAB fmap 2 acta OMIT -3 50.2 OMIT 4 -1 4 OMIT 1 -2 3 OMIT -4 1 2 OMIT -5 5 1 OMIT 3 -7 3 OMIT -1 3 3 OMIT 0 -5 2 OMIT 0 2 4 OMIT 2 -1 5 OMIT 2 -4 1 OMIT 1 6 2 OMIT 6 -1 4 OMIT -1 5 0 OMIT 0 -2 9 OMIT 4 -4 4 OMIT -2 -2 3 OMIT 2 2 0 OMIT 0 -4 7 OMIT 4 1 2 OMIT -1 5 2 OMIT 3 -4 4 OMIT 2 -2 1 OMIT -1 2 5 OMIT -2 -1 6 OMIT -2 1 0 OMIT 0 -8 1 OMIT 1 -1 1 OMIT 3 -5 2 OMIT -1 5 1 OMIT -3 0 4 OMIT 6 -2 6 OMIT 2 -4 10 OMIT -1 -1 10 OMIT -3 7 3 OMIT 0 -2 10 OMIT 0 -3 2 OMIT 4 3 2 OMIT 0 -1 2 OMIT -1 4 3 OMIT -4 1 9 OMIT 3 -4 2 OMIT 1 -8 7 OMIT 0 -3 3 OMIT 1 5 5 OMIT -4 1 7 OMIT 1 3 0 OMIT 4 -4 3 OMIT 5 -4 2 OMIT -5 1 0 OMIT 0 0 8 OMIT 5 -1 7 OMIT -1 3 2 OMIT -3 7 7 OMIT 5 -6 1 OMIT -3 3 1 OMIT -2 -4 5 OMIT 0 1 5 OMIT -4 -2 6 OMIT 5 -8 1 OMIT -2 7 5 OMIT 2 4 2 OMIT -1 7 2 REM REM REM WGHT 0.200000 FVAR 0.15859 S1 3 0.644363 0.461498 1.100946 11.00000 0.03550 0.07439 = 0.04485 0.00723 0.00997 0.01524 S2 3 0.281213 -0.152357 0.493166 11.00000 0.04525 0.05737 = 0.06160 -0.00176 -0.00248 0.03054 C1 1 0.501347 0.400314 1.036973 11.00000 0.02699 0.06691 = 0.06157 0.01467 0.01093 0.01224 AFIX 43 H1 2 0.417036 0.386519 1.051051 11.00000 -1.20000 AFIX 0 C2 1 0.522186 0.373568 0.963377 11.00000 0.03137 0.05332 = 0.05335 0.00284 0.00288 0.01083 AFIX 43 H2 2 0.455024 0.339462 0.921666 11.00000 -1.20000 AFIX 0 C3 1 0.661526 0.405036 0.958827 11.00000 0.02646 0.04696 = 0.04762 0.00991 0.00245 0.00703 C4 1 0.737126 0.452582 1.028950 11.00000 0.02251 0.04743 = 0.03868 0.00180 0.00234 0.00839 C5 1 0.878006 0.483430 1.022547 11.00000 0.03066 0.04715 = 0.03620 0.00280 0.00383 0.01696 C6 1 0.990640 0.530657 1.077672 11.00000 0.03030 0.05328 = 0.03159 0.00339 0.00207 0.01087 AFIX 43 H6 2 0.982944 0.551225 1.128953 11.00000 -1.20000 AFIX 0 C7 1 1.112528 0.546287 1.055252 11.00000 0.03015 0.04519 = 0.03809 0.00290 0.00271 0.01437 C8 1 0.747311 0.403040 0.895610 11.00000 0.03091 0.04597 = 0.03711 0.00326 0.00039 0.01212 C9 1 0.735927 0.301303 0.844728 11.00000 0.02735 0.05196 = 0.04488 0.00083 -0.00668 0.01362 C10 1 0.674230 0.218061 0.862268 11.00000 0.06772 0.04758 = 0.06419 0.00898 0.01918 0.01972 AFIX 43 H10 2 0.634824 0.222201 0.905970 11.00000 -1.20000 AFIX 0 C11 1 0.671207 0.127730 0.814214 11.00000 0.06719 0.05132 = 0.09283 0.00900 0.00742 0.01210 AFIX 43 H11 2 0.626165 0.072035 0.825542 11.00000 -1.20000 AFIX 0 C12 1 0.733623 0.118310 0.749696 11.00000 0.04981 0.06069 = 0.05574 -0.01045 -0.01308 0.02512 C13 1 0.790679 0.200457 0.732977 11.00000 0.06655 0.06514 = 0.04447 -0.00299 0.00197 0.03112 AFIX 43 H13 2 0.830478 0.196603 0.689423 11.00000 -1.20000 AFIX 0 C14 1 0.791510 0.290672 0.779154 11.00000 0.05610 0.06146 = 0.04239 0.00451 0.00878 0.02470 AFIX 43 H14 2 0.830839 0.345442 0.765262 11.00000 -1.20000 AFIX 0 C15 1 0.736145 0.019900 0.702485 11.00000 0.07046 0.06399 = 0.06408 -0.00641 -0.01288 0.02680 AFIX 23 H15A 2 0.742317 0.019278 0.650462 11.00000 -1.20000 H15B 2 0.653318 -0.029226 0.702053 11.00000 -1.20000 AFIX 0 C16 1 0.852248 -0.005617 0.732600 11.00000 0.07129 0.05966 = 0.07740 -0.01008 -0.00460 0.03118 AFIX 23 H16A 2 0.933783 0.047990 0.739671 11.00000 -1.20000 H16B 2 0.839466 -0.013303 0.781993 11.00000 -1.20000 AFIX 0 C17 1 0.868219 -0.097950 0.680518 11.00000 0.10466 0.07601 = 0.09501 -0.00474 0.01714 0.04723 AFIX 23 H17A 2 0.782767 -0.149351 0.667353 11.00000 -1.20000 H17B 2 0.893994 -0.086844 0.633822 11.00000 -1.20000 AFIX 0 C18 1 0.966537 -0.130424 0.713853 11.00000 0.11304 0.10207 = 0.17472 -0.00438 -0.00733 0.06838 AFIX 23 H18A 2 0.934372 -0.155037 0.754398 11.00000 -1.20000 H18B 2 1.049698 -0.077337 0.734409 11.00000 -1.20000 AFIX 0 C19 1 0.989699 -0.225939 0.636763 11.00000 0.20648 AFIX 23 H19A 2 0.918690 -0.287005 0.627632 11.00000 -1.20000 H19B 2 0.993169 -0.209094 0.590191 11.00000 -1.20000 AFIX 0 C20 1 1.121781 -0.231797 0.665442 11.00000 10.14930 AFIX 33 H20A 2 1.143283 -0.281256 0.627954 11.00000 -1.50000 H20B 2 1.189956 -0.170285 0.674730 11.00000 -1.50000 H20C 2 1.116073 -0.247574 0.711872 11.00000 -1.50000 AFIX 0 C21 1 0.711396 0.461786 0.847159 11.00000 0.03350 0.04752 = 0.03996 0.00096 0.00174 0.01626 C22 1 0.586763 0.427610 0.804533 11.00000 0.04636 0.06013 = 0.04163 0.00314 -0.00142 0.02064 AFIX 43 H22 2 0.527055 0.369130 0.805001 11.00000 -1.20000 AFIX 0 C23 1 0.547590 0.477906 0.760857 11.00000 0.05777 0.07972 = 0.04518 0.00530 0.00132 0.03563 AFIX 43 H23 2 0.461721 0.453626 0.733711 11.00000 -1.20000 AFIX 0 C24 1 0.634334 0.563287 0.757250 11.00000 0.07927 0.08561 = 0.05556 0.01460 0.00304 0.04505 C25 1 0.759805 0.596255 0.799948 11.00000 0.08218 0.07186 = 0.10311 0.04010 -0.00165 0.01861 AFIX 43 H25 2 0.821559 0.652894 0.797624 11.00000 -1.20000 AFIX 0 C26 1 0.796645 0.548150 0.845856 11.00000 0.04674 0.06587 = 0.07640 0.02536 -0.00459 0.00616 AFIX 43 H26 2 0.880030 0.574723 0.876080 11.00000 -1.20000 AFIX 0 C27 1 0.596625 0.618544 0.709335 11.00000 0.13672 0.12384 = 0.07691 0.04132 0.01339 0.07313 AFIX 23 H27A 2 0.676880 0.657323 0.696477 11.00000 -1.20000 H27B 2 0.541846 0.572631 0.662234 11.00000 -1.20000 AFIX 0 C28 1 0.521610 0.684669 0.747943 11.00000 0.16582 AFIX 23 H28A 2 0.498650 0.715639 0.712541 11.00000 -1.20000 H28B 2 0.438781 0.644461 0.757294 11.00000 -1.20000 AFIX 0 C29 1 0.590428 0.762601 0.821379 11.00000 0.26413 0.13770 = 0.21026 0.06701 0.04639 0.12420 AFIX 23 H29A 2 0.680190 0.796419 0.815642 11.00000 -1.20000 H29B 2 0.596748 0.733133 0.860765 11.00000 -1.20000 AFIX 0 C30 1 0.515561 0.836033 0.845817 11.00000 10.18220 AFIX 23 H30A 2 0.495664 0.859227 0.804436 11.00000 -1.20000 H30B 2 0.433124 0.807409 0.862634 11.00000 -1.20000 AFIX 0 C31 1 0.608582 0.914190 0.908261 11.00000 10.18389 AFIX 23 H31A 2 0.599989 0.976376 0.909503 11.00000 -1.20000 H31B 2 0.699534 0.916484 0.902911 11.00000 -1.20000 AFIX 0 C32 1 0.568819 0.889120 0.986491 11.00000 10.19185 AFIX 137 H32A 2 0.533584 0.936795 1.015950 11.00000 -1.50000 H32B 2 0.646808 0.890179 1.015921 11.00000 -1.50000 H32C 2 0.502967 0.825823 0.973044 11.00000 -1.50000 AFIX 0 C33 1 0.426972 -0.086173 0.555471 11.00000 0.04167 0.07829 = 0.06797 0.01183 -0.00345 0.03433 AFIX 43 H33 2 0.496701 -0.110115 0.560894 11.00000 -1.20000 AFIX 0 C34 1 0.430008 0.003843 0.595637 11.00000 0.03352 0.05851 = 0.05122 0.00260 -0.00745 0.01919 AFIX 43 H34 2 0.502026 0.049220 0.631162 11.00000 -1.20000 AFIX 0 C35 1 0.312230 0.020776 0.577541 11.00000 0.03431 0.05376 = 0.03668 0.00551 0.00123 0.02186 C36 1 0.222611 -0.057088 0.522576 11.00000 0.03266 0.04459 = 0.04454 -0.00001 -0.00262 0.01856 C37 1 0.101077 -0.037534 0.504359 11.00000 0.02974 0.05134 = 0.03536 0.00529 0.00124 0.01955 C38 1 0.118369 0.058870 0.549268 11.00000 0.03071 0.04823 = 0.03703 0.00126 -0.00005 0.01667 C39 1 0.016682 0.096497 0.545177 11.00000 0.03307 0.04750 = 0.04331 -0.00318 -0.00127 0.02047 AFIX 43 H39 2 0.026040 0.159616 0.574641 11.00000 -1.20000 AFIX 0 C40 1 0.257860 0.106775 0.599076 11.00000 0.03239 0.04714 = 0.03917 -0.00038 -0.00218 0.01616 C41 1 0.350265 0.190087 0.577162 11.00000 0.03094 0.05219 = 0.04329 0.00019 0.00059 0.01810 C42 1 0.314420 0.219141 0.517644 11.00000 0.04772 0.06705 = 0.06096 0.01645 0.00060 0.01881 AFIX 43 H42 2 0.229881 0.188567 0.488836 11.00000 -1.20000 AFIX 0 C43 1 0.405641 0.294640 0.500872 11.00000 0.06909 0.07953 = 0.09594 0.03959 0.00671 0.02273 AFIX 43 H43 2 0.381009 0.313144 0.460079 11.00000 -1.20000 AFIX 0 C44 1 0.530034 0.342388 0.542335 11.00000 0.06131 0.05809 = 0.09715 0.01926 0.02124 0.02250 C45 1 0.565517 0.312412 0.600763 11.00000 0.03485 0.06336 = 0.07781 0.00152 0.01362 0.00819 AFIX 43 H45 2 0.650735 0.342688 0.628766 11.00000 -1.20000 AFIX 0 C46 1 0.477678 0.238394 0.618919 11.00000 0.03664 0.06019 = 0.05584 -0.00453 -0.00604 0.01410 AFIX 43 H46 2 0.503640 0.220286 0.659655 11.00000 -1.20000 AFIX 0 C47 1 0.624145 0.426540 0.522168 11.00000 0.08666 0.08919 = 0.18766 0.06260 0.03409 0.01073 AFIX 23 H47A 2 0.571001 0.460738 0.504914 11.00000 -1.20000 H47B 2 0.682661 0.471501 0.568418 11.00000 -1.20000 AFIX 0 C48 1 0.702709 0.403346 0.467446 11.00000 0.15055 0.11266 = 0.16531 0.05930 0.08084 0.00750 AFIX 23 H48A 2 0.648109 0.363416 0.418652 11.00000 -1.20000 H48B 2 0.757685 0.368775 0.482328 11.00000 -1.20000 AFIX 0 C49 1 0.792934 0.506542 0.463332 11.00000 0.18455 AFIX 23 H49A 2 0.742688 0.551458 0.470917 11.00000 -1.20000 H49B 2 0.871038 0.534188 0.502376 11.00000 -1.20000 AFIX 0 C50 1 0.832704 0.488524 0.386778 11.00000 10.14530 AFIX 23 H50A 2 0.756148 0.464773 0.347055 11.00000 -1.20000 H50B 2 0.881626 0.442723 0.377778 11.00000 -1.20000 AFIX 0 C51 1 0.922386 0.591251 0.392171 11.00000 10.16360 AFIX 23 H51A 2 0.876824 0.638933 0.405839 11.00000 -1.20000 H51B 2 1.004719 0.612537 0.427242 11.00000 -1.20000 AFIX 0 C52 1 0.943990 0.568850 0.311764 11.00000 10.16544 AFIX 33 H52A 2 1.000051 0.626578 0.303890 11.00000 -1.50000 H52B 2 0.986087 0.519697 0.300207 11.00000 -1.50000 H52C 2 0.859832 0.545755 0.279078 11.00000 -1.50000 AFIX 0 C53 1 0.241471 0.140913 0.683103 11.00000 0.03156 0.05752 = 0.03733 0.00066 -0.00202 0.01065 C54 1 0.261054 0.094733 0.732770 11.00000 0.06265 0.08672 = 0.04994 0.01969 0.00761 0.03526 AFIX 43 H54 2 0.287354 0.039943 0.716884 11.00000 -1.20000 AFIX 0 C55 1 0.241556 0.129742 0.808629 11.00000 0.07812 0.09516 = 0.04962 0.02069 0.00523 0.02953 AFIX 43 H55 2 0.256559 0.097848 0.842470 11.00000 -1.20000 AFIX 0 C56 1 0.201350 0.208978 0.833987 11.00000 0.03302 0.09084 = 0.04671 -0.00369 0.00226 0.00799 C57 1 0.185931 0.256661 0.784909 11.00000 0.05621 0.07055 = 0.04620 -0.00838 0.00584 0.02411 AFIX 43 H57 2 0.158547 0.310939 0.800895 11.00000 -1.20000 AFIX 0 C58 1 0.210546 0.225596 0.710407 11.00000 0.05351 0.06251 = 0.04856 0.00101 -0.00140 0.02266 AFIX 43 H58 2 0.206111 0.262334 0.678610 11.00000 -1.20000 AFIX 0 C59 1 0.173502 0.242914 0.914887 11.00000 0.06328 0.12215 = 0.04169 0.00167 0.01224 0.01243 AFIX 23 H59A 2 0.233264 0.229537 0.948602 11.00000 -1.20000 H59B 2 0.191492 0.312660 0.930754 11.00000 -1.20000 AFIX 0 C60 1 0.032597 0.194087 0.922238 11.00000 0.06971 0.14868 = 0.07173 -0.00710 0.01421 0.00792 AFIX 23 H60A 2 0.014015 0.124266 0.904576 11.00000 -1.20000 H60B 2 -0.026756 0.209146 0.889527 11.00000 -1.20000 AFIX 0 C61 1 0.003187 0.224293 1.003007 11.00000 0.10830 0.17600 = 0.10512 -0.03747 0.05266 -0.00367 AFIX 23 H61A 2 0.081117 0.232446 1.037311 11.00000 -1.20000 H61B 2 -0.008583 0.287439 1.013537 11.00000 -1.20000 AFIX 0 C62 1 -0.110245 0.160540 1.021288 11.00000 10.17378 AFIX 23 H62A 2 -0.100462 0.096611 1.008234 11.00000 -1.20000 H62B 2 -0.188560 0.154934 0.988521 11.00000 -1.20000 AFIX 0 C63 1 -0.137756 0.187546 1.103579 11.00000 10.21821 AFIX 23 H63A 2 -0.215499 0.137569 1.108046 11.00000 -1.20000 H63B 2 -0.062490 0.190239 1.137224 11.00000 -1.20000 AFIX 0 C64 1 -0.161245 0.284772 1.128031 11.00000 10.18896 AFIX 33 H64A 2 -0.178094 0.299362 1.179633 11.00000 -1.50000 H64B 2 -0.083817 0.334577 1.124549 11.00000 -1.50000 H64C 2 -0.236700 0.281950 1.095395 11.00000 -1.50000 AFIX 0 HKLF 4 REM A in P-1 REM R1 = 0.1133 for 5195 Fo > 4sig(Fo) and 0.1687 for all 9546 data REM 521 parameters refined using 8 restraints END WGHT 0.2000 0.0000 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.798, deepest hole -1.112, 1-sigma level 0.108 Q1 1 0.9610 -0.2400 0.6799 11.00000 0.05 0.80 Q2 1 0.7826 0.1944 0.8341 11.00000 0.05 0.72 Q3 1 0.1406 -0.1994 0.4479 11.00000 0.05 0.69 Q4 1 0.6022 0.7168 0.7420 11.00000 0.05 0.67 Q5 1 0.1454 0.1113 0.7553 11.00000 0.05 0.59 Q6 1 0.7822 0.4821 0.4282 11.00000 0.05 0.59 Q7 1 0.9630 0.5232 0.3483 11.00000 0.05 0.57 Q8 1 1.0347 -0.1871 0.6652 11.00000 0.05 0.54 Q9 1 0.7816 0.4992 1.1466 11.00000 0.05 0.49 Q10 1 -0.1417 0.0640 1.0045 11.00000 0.05 0.45 Q11 1 0.0452 0.1352 1.0224 11.00000 0.05 0.42 Q12 1 0.2843 0.0644 0.5717 11.00000 0.05 0.42 Q13 1 0.0160 0.1172 1.0197 11.00000 0.05 0.42 Q14 1 0.7606 0.5100 0.8560 11.00000 0.05 0.42 Q15 1 0.0578 0.1597 1.0262 11.00000 0.05 0.41 Q16 1 -0.0824 0.0405 1.0004 11.00000 0.05 0.41 Q17 1 0.2019 -0.0784 0.5274 11.00000 0.05 0.38 Q18 1 0.7632 0.2444 0.7489 11.00000 0.05 0.38 Q19 1 0.3059 0.2229 0.5375 11.00000 0.05 0.38 Q20 1 0.8657 0.5011 0.3119 11.00000 0.05 0.37 REM The information below was added by Olex2. REM REM R1 = 0.1133 for 5195 Fo > 4sig(Fo) and 0.1687 for all 17243 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.80, deepest hole -1.11 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1687 REM R1_gt = 0.1133 REM wR_ref = 0.3610 REM GOOF = 1.166 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 17243 REM Reflections_gt = 5195 REM Parameters = n/a REM Hole = -1.11 REM Peak = 0.80 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma -1 0 0 27.95 1.3 -2 0 0 249.32 11.03 -2 0 0 239.46 10.95 -3 0 0 1.03 0.15 -3 0 0 0.91 0.15 -4 0 0 112.96 5.4 -4 0 0 122.87 5.43 -5 0 0 -0.02 0.15 -5 0 0 -0.02 0.16 -6 0 0 0.3 0.17 -6 0 0 0.16 0.19 -7 0 0 1.43 0.31 -7 0 0 1.18 0.26 -8 0 0 14.44 1 -8 0 0 15.93 0.98 -9 0 0 3.42 0.51 -9 0 0 3.86 0.54 -10 0 0 0.71 0.33 -11 0 0 1.55 0.44 -12 0 0 -0.43 0.28 -12 1 0 0.55 0.42 -11 1 0 0.17 0.29 -10 1 0 2.13 0.48 -10 1 0 2.57 0.45 -9 1 0 -0.73 0.23 -9 1 0 -0.15 0.2 -8 1 0 4.27 0.54 -8 1 0 3.73 0.45 -7 1 0 26.67 1.46 -7 1 0 25.31 1.38 -6 1 0 5.1 0.41 -6 1 0 4.66 0.45 -5 1 0 7.45 0.54 -5 1 0 7.43 0.49 -4 1 0 0.48 0.14 -4 1 0 0.33 0.16 -2 1 0 3.48 0.25 -1 1 0 67.98 3.08 -1 -1 0 113.83 5.09 -2 -1 0 86.69 3.97 -2 -1 0 85.93 3.91 -3 -1 0 10.87 0.59 -3 -1 0 10.3 0.6 -4 -1 0 63.55 2.92 -4 -1 0 60.74 2.95 -5 -1 0 2.93 0.33 -5 -1 0 2.6 0.33 -6 -1 0 63.43 3.18 -6 -1 0 68.13 3.17 -7 -1 0 5.2 0.51 -7 -1 0 6.1 0.52 -8 -1 0 1.37 0.37 -8 -1 0 1.19 0.35 -9 -1 0 0.15 0.27 -10 -1 0 0.12 0.32 -11 -1 0 1.58 0.44 -12 -1 0 0.37 0.36 -13 -1 0 0.21 0.48 -11 2 0 -0.03 0.28 -11 2 0 0.13 0.34 -10 2 0 -0.36 0.27 -10 2 0 0.02 0.24 -9 2 0 37.5 1.88 -9 2 0 32.66 1.97 -8 2 0 1.76 0.36 -8 2 0 2.01 0.33 -7 2 0 4.59 0.53 -6 2 0 2.43 0.27 -5 2 0 7.49 0.54 -5 2 0 7.52 0.47 -4 2 0 39.09 1.94 -4 2 0 40.14 1.87 -3 2 0 19.58 0.95 -3 2 0 20.38 1.03 2 -2 0 55.11 2.56 -2 2 0 57.23 2.6 -1 2 0 83.78 3.79 0 2 0 46.18 2.08 -1 -2 0 52.8 2.45 -2 -2 0 1.22 0.18 -2 -2 0 0.94 0.12 -3 -2 0 9.64 0.6 -3 -2 0 10.52 0.56 -4 -2 0 32.14 1.65 -4 -2 0 33.1 1.59 -5 -2 0 19.94 1.05 -5 -2 0 18.44 1.08 -6 -2 0 5.46 0.46 -6 -2 0 5.5 0.5 -7 -2 0 0.55 0.24 -7 -2 0 1.1 0.32 -8 -2 0 18.91 1.19 -9 -2 0 1.31 0.39 -10 -2 0 0.88 0.36 -11 -2 0 1.63 0.5 -12 -2 0 0.27 0.38 -12 3 0 0.01 0.38 -11 3 0 2.79 0.59 -10 3 0 4.56 0.53 -10 3 0 3.73 0.59 -9 3 0 -0.29 0.31 -9 3 0 0.33 0.26 -8 3 0 0.23 0.25 -8 3 0 0.21 0.17 -7 3 0 1.65 0.35 -7 3 0 1.62 0.25 -6 3 0 2.5 0.38 -6 3 0 2.67 0.28 -5 3 0 0.94 0.15 -5 3 0 0.9 0.23 4 -3 0 7.57 0.48 -4 3 0 8.4 0.44 -4 3 0 7.96 0.54 3 -3 0 138.36 6.22 -3 3 0 136.6 6.27 2 -3 0 461.59 19.85 -2 3 0 425.77 19.84 1 -3 0 304.58 13.65 0 -3 0 519.63 23.09 0 3 0 507.85 22.88 -1 -3 0 0.68 0.14 -2 -3 0 1.27 0.2 -2 -3 0 1.32 0.11 -3 -3 0 33.92 1.76 -3 -3 0 36.75 1.66 -4 -3 0 4.4 0.33 -4 -3 0 4.14 0.4 -5 -3 0 3.45 0.35 -5 -3 0 3.78 0.43 -6 -3 0 7.68 0.62 -6 -3 0 5.82 0.5 -7 -3 0 2.18 0.42 -8 -3 0 9.01 0.77 -9 -3 0 -0.53 0.22 -10 -3 0 -0.17 0.36 -11 -3 0 1.09 0.49 -12 -3 0 1.52 0.52 -13 4 0 -0.23 0.43 -12 4 0 -0.05 0.38 -11 4 0 0.18 0.36 -10 4 0 -0.25 0.31 -9 4 0 17.6 1.06 -9 4 0 19.83 1.28 -8 4 0 -0.01 0.17 -8 4 0 -0.06 0.25 -7 4 0 13.85 0.76 -7 4 0 12.44 0.9 -6 4 0 0.23 0.2 -6 4 0 0.32 0.12 -5 4 0 1.26 0.24 4 -4 0 9.67 0.56 -4 4 0 9.23 0.62 3 -4 0 13.57 0.74 -3 4 0 14.46 0.79 2 -4 0 34.35 1.63 -2 4 0 33.27 1.63 1 -4 0 212.57 9.4 -1 4 0 204.03 9.35 0 -4 0 9.05 0.5 0 4 0 8.78 0.45 -1 -4 0 0.02 0.1 -2 -4 0 17.06 0.93 -3 -4 0 18.07 0.85 -3 -4 0 17.27 0.99 -4 -4 0 93.56 4.2 -4 -4 0 90.61 4.37 -5 -4 0 38.75 1.9 -5 -4 0 40.28 2.05 -6 -4 0 27.24 1.54 -7 -4 0 0.39 0.34 -8 -4 0 6.46 0.74 -9 -4 0 0.37 0.33 -10 -4 0 0.99 0.43 -11 -4 0 0.11 0.37 -12 -4 0 2.34 0.64 -14 5 0 0.42 0.53 -13 5 0 0.05 0.37 -12 5 0 0.05 0.41 -11 5 0 0.88 0.45 -10 5 0 -0.13 0.33 -9 5 0 3.68 0.59 -8 5 0 -0.13 0.23 -7 5 0 0.93 0.29 -7 5 0 1.55 0.22 6 -5 0 -0.06 0.15 -6 5 0 0.01 0.16 -6 5 0 0.07 0.11 5 -5 0 1.38 0.24 -5 5 0 1.74 0.17 -5 5 0 1.7 0.31 4 -5 0 13.84 0.78 -4 5 0 13.91 0.83 -3 5 0 0.1 0.12 2 -5 0 0.74 0.16 -2 5 0 0.96 0.17 1 -5 0 8.42 0.52 1 -5 0 7.94 0.44 -1 5 0 7.36 0.45 0 -5 0 4.76 0.34 0 -5 0 4.06 0.36 0 5 0 5.07 0.29 -1 -5 0 2.35 0.27 -2 -5 0 4.77 0.4 -3 -5 0 7.73 0.56 -4 -5 0 1.15 0.3 -5 -5 0 3.57 0.47 -6 -5 0 15.3 1.04 -7 -5 0 18.57 1.22 -8 -5 0 3.85 0.58 -9 -5 0 0.4 0.37 -10 -5 0 0.89 0.44 -11 -5 0 4.3 0.75 -13 6 0 1.99 0.63 -12 6 0 -0.16 0.32 -11 6 0 0.98 0.42 -10 6 0 2.12 0.55 -9 6 0 1.01 0.39 -8 6 0 0.2 0.28 -7 6 0 8.74 0.75 6 -6 0 12.61 0.79 -6 6 0 12.42 0.87 -6 6 0 12.82 0.66 5 -6 0 48.33 2.38 -5 6 0 50.48 2.48 4 -6 0 20.43 1.08 -4 6 0 20.48 1.14 3 -6 0 0.67 0.17 -3 6 0 0.75 0.18 2 -6 0 33.39 1.65 2 -6 0 37.54 1.77 1 -6 0 25.27 1.28 1 -6 0 25.86 1.36 -1 6 0 26.95 1.28 0 -6 0 15.22 0.9 0 -6 0 14.92 0.83 0 6 0 15.62 0.76 -1 -6 0 31.8 1.61 -2 -6 0 15.12 0.89 -3 -6 0 -0.12 0.14 -4 -6 0 5.11 0.5 -5 -6 0 -0.01 0.21 -6 -6 0 1.17 0.38 -7 -6 0 1.96 0.49 -8 -6 0 0.94 0.44 -9 -6 0 -0.43 0.39 -10 -6 0 0.13 0.43 -11 -6 0 -0.51 0.39 -13 7 0 -0.15 0.37 -12 7 0 1.39 0.52 -11 7 0 0.16 0.38 -10 7 0 -0.11 0.35 -9 7 0 25.22 1.61 -8 7 0 0.46 0.31 7 -7 0 31.25 1.65 -7 7 0 30.82 1.76 6 -7 0 8.86 0.65 -6 7 0 9.44 0.72 5 -7 0 23.44 1.31 -5 7 0 26.34 1.41 4 -7 0 6.39 0.49 -4 7 0 6.63 0.52 3 -7 0 23.14 1.29 -3 7 0 25.98 1.31 2 -7 0 59.6 2.91 2 -7 0 59.86 2.8 -2 7 0 61.34 2.86 1 -7 0 138.51 6.62 1 -7 0 141.79 6.56 -1 7 0 149.66 6.52 0 -7 0 12.75 0.75 0 -7 0 12.01 0.82 0 7 0 13.44 0.67 -1 -7 0 19.61 1.08 -2 -7 0 9.73 0.68 -3 -7 0 5.41 0.5 -4 -7 0 -0.29 0.21 -5 -7 0 0.2 0.28 -6 -7 0 6.63 0.75 -7 -7 0 -0.18 0.28 -8 -7 0 -0.27 0.34 -9 -7 0 0.66 0.46 -10 -7 0 0.63 0.54 -13 8 0 -0.48 0.34 -12 8 0 -0.1 0.41 -11 8 0 2.39 0.56 -10 8 0 0.16 0.33 -9 8 0 0.75 0.36 8 -8 0 9.25 0.74 -8 8 0 8.77 0.82 7 -8 0 7.44 0.63 -7 8 0 7.21 0.68 6 -8 0 1.35 0.27 -6 8 0 1.09 0.32 5 -8 0 21.07 1.18 -5 8 0 21.65 1.25 4 -8 0 6.33 0.51 -4 8 0 5.17 0.5 3 -8 0 17.7 0.99 3 -8 0 18.13 0.83 -3 8 0 12.95 0.91 2 -8 0 7.24 0.56 2 -8 0 7.47 0.46 -2 8 0 7.34 0.52 1 -8 0 6.85 0.47 1 -8 0 6.73 0.56 -1 8 0 7.14 0.46 0 -8 0 -0.22 0.14 0 -8 0 -0.12 0.17 0 8 0 0.07 0.09 -1 -8 0 3.18 0.4 -2 -8 0 3.09 0.4 -3 -8 0 16.74 1.07 -4 -8 0 6.34 0.63 -5 -8 0 -0.15 0.27 -6 -8 0 0.13 0.38 -7 -8 0 0.14 0.33 -8 -8 0 -0.44 0.28 -9 -8 0 1.25 0.48 -10 -8 0 -0.13 0.39 -13 9 0 0.89 0.58 -12 9 0 1.84 0.61 -11 9 0 -0.08 0.33 -10 9 0 1.15 0.5 -9 9 0 1 0.41 8 -9 0 0.43 0.31 -8 9 0 0.08 0.3 7 -9 0 4.52 0.51 -7 9 0 3.51 0.54 6 -9 0 30.27 1.57 -6 9 0 26.33 1.6 5 -9 0 8.04 0.65 -5 9 0 8.61 0.7 4 -9 0 26.04 1.41 -4 9 0 24.71 1.4 3 -9 0 2.96 0.25 3 -9 0 3.18 0.42 -3 9 0 2.36 0.35 2 -9 0 0.62 0.24 2 -9 0 0.08 0.13 -2 9 0 -0.15 0.13 1 -9 0 6.18 0.47 1 -9 0 6.49 0.57 -1 9 0 6.23 0.45 0 -9 0 17.56 1.02 0 -9 0 17.99 1.13 -1 -9 0 0.56 0.27 -1 -9 0 0.1 0.18 -2 -9 0 0.61 0.26 -3 -9 0 3.83 0.51 -4 -9 0 3.98 0.56 -5 -9 0 -0.03 0.28 -6 -9 0 0.34 0.39 -7 -9 0 0.07 0.33 -8 -9 0 -0.12 0.43 -9 -9 0 0.12 0.42 -13 10 0 1.31 0.63 -12 10 0 1.35 0.59 -11 10 0 1.37 0.54 -10 10 0 1.64 0.52 9 -10 0 3.27 0.53 -9 10 0 3.33 0.6 8 -10 0 2.09 0.43 -8 10 0 2.43 0.52 7 -10 0 4.9 0.57 -7 10 0 5.38 0.66 6 -10 0 -0.03 0.23 -6 10 0 -0.13 0.23 5 -10 0 9.57 0.72 -5 10 0 9.21 0.76 4 -10 0 -0.01 0.18 -4 10 0 0.17 0.19 3 -10 0 1.67 0.33 -3 10 0 2.04 0.33 2 -10 0 1.32 0.3 2 -10 0 0.9 0.21 -2 10 0 1.17 0.25 1 -10 0 1.69 0.36 1 -10 0 1.97 0.29 0 -10 0 0.07 0.25 0 -10 0 -0.04 0.15 -1 -10 0 3.21 0.44 -1 -10 0 2.56 0.47 -2 -10 0 -0.26 0.25 -2 -10 0 0.28 0.26 -3 -10 0 -0.09 0.26 -4 -10 0 0.48 0.34 -5 -10 0 0.92 0.44 -6 -10 0 0.31 0.34 -7 -10 0 0.07 0.37 -8 -10 0 -0.12 0.47 -9 -10 0 -0.04 0.44 -12 11 0 0.56 0.53 -11 11 0 2.09 0.64 10 -11 0 0.71 0.39 -10 11 0 0.34 0.45 9 -11 0 0.54 0.37 -9 11 0 1.59 0.52 8 -11 0 9.19 0.83 -8 11 0 10.66 0.93 7 -11 0 0.12 0.28 -7 11 0 0 0.27 6 -11 0 0.05 0.26 -6 11 0 0.65 0.29 5 -11 0 8.22 0.69 -5 11 0 8.34 0.72 4 -11 0 2.35 0.43 3 -11 0 -0.06 0.21 -3 11 0 -0.1 0.18 2 -11 0 -0.24 0.19 -2 11 0 -0.08 0.15 1 -11 0 0.09 0.22 1 -11 0 -0.14 0.19 0 -11 0 0.35 0.24 0 -11 0 0.02 0.29 -1 -11 0 0.7 0.3 -1 -11 0 0.73 0.36 -2 -11 0 3.64 0.58 -2 -11 0 3.51 0.52 -3 -11 0 0.14 0.31 -3 -11 0 0.16 0.29 -4 -11 0 1.34 0.46 -5 -11 0 0.07 0.32 -6 -11 0 1 0.43 -7 -11 0 0.23 0.47 -8 -11 0 0.34 0.44 -12 12 0 2.3 0.71 -11 12 0 0.36 0.44 10 -12 0 0.3 0.39 -10 12 0 0.37 0.38 9 -12 0 -0.27 0.3 -9 12 0 0.51 0.37 8 -12 0 -0.28 0.28 -8 12 0 -0.01 0.28 7 -12 0 5.2 0.66 -7 12 0 7.36 0.79 6 -12 0 2.63 0.46 -6 12 0 3.64 0.55 5 -12 0 0.67 0.28 -5 12 0 0.73 0.32 4 -12 0 3.93 0.56 -4 12 0 4.02 0.53 3 -12 0 6.49 0.74 -3 12 0 6.55 0.6 2 -12 0 0.07 0.24 1 -12 0 2.57 0.47 0 -12 0 4.43 0.53 0 -12 0 3.25 0.55 -1 -12 0 4.05 0.65 -1 -12 0 4.72 0.57 -2 -12 0 5.74 0.7 -2 -12 0 4.67 0.67 -3 -12 0 0.34 0.31 -3 -12 0 0.48 0.37 -4 -12 0 0.44 0.42 -4 -12 0 0.9 0.35 -5 -12 0 0.29 0.38 -5 -12 0 0.71 0.38 -6 -12 0 -0.45 0.34 -7 -12 0 0.69 0.47 -12 13 0 0.87 0.61 -11 13 0 3.02 0.73 10 -13 0 -0.21 0.36 -10 13 0 -0.21 0.39 9 -13 0 0.47 0.38 -9 13 0 0.87 0.46 8 -13 0 -0.13 0.31 -8 13 0 -0.06 0.28 7 -13 0 8.21 0.81 -7 13 0 8.53 0.93 6 -13 0 0.36 0.33 -6 13 0 -0.18 0.26 5 -13 0 0.54 0.35 -5 13 0 0.12 0.21 4 -13 0 0.67 0.32 3 -13 0 -0.26 0.25 2 -13 0 0.25 0.32 1 -13 0 -0.16 0.29 0 -13 0 7.02 0.69 0 -13 0 5.51 0.73 -1 -13 0 1.32 0.43 -1 -13 0 1.9 0.44 -2 -13 0 0.09 0.33 -2 -13 0 0.42 0.4 -3 -13 0 1.17 0.42 -3 -13 0 0 0.33 -4 -13 0 0.65 0.39 -4 -13 0 -0.12 0.31 -5 -13 0 -0.29 0.38 -5 -13 0 0.11 0.39 -6 -13 0 -0.46 0.39 -6 -13 0 -0.04 0.41 -11 14 0 0.84 0.55 10 -14 0 2.44 0.55 -10 14 0 3.08 0.68 9 -14 0 -0.41 0.32 -9 14 0 0 0.32 8 -14 0 4.74 0.68 -8 14 0 7.76 0.9 7 -14 0 3.16 0.52 -7 14 0 2.71 0.54 6 -14 0 -0.28 0.27 -6 14 0 -0.36 0.26 5 -14 0 0.16 0.34 4 -14 0 0.92 0.37 3 -14 0 0.18 0.33 2 -14 0 0.19 0.34 1 -14 0 0.26 0.31 0 -14 0 0.25 0.3 -1 -14 0 0.1 0.3 -2 -14 0 0.03 0.34 -2 -14 0 0.17 0.38 -3 -14 0 0.19 0.42 -3 -14 0 0.07 0.4 -4 -14 0 -0.03 0.36 -4 -14 0 0 0.39 -5 -14 0 -0.36 0.41 -5 -14 0 -0.2 0.45 -11 15 0 -0.11 0.49 10 -15 0 0 0.4 -10 15 0 0.05 0.44 9 -15 0 0.72 0.46 -9 15 0 -0.23 0.38 8 -15 0 0.62 0.4 -8 15 0 0.71 0.42 7 -15 0 0.26 0.33 -7 15 0 0.81 0.41 6 -15 0 1.71 0.46 5 -15 0 -0.53 0.34 4 -15 0 0.22 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