# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_Compound_I _database_code_depnum_ccdc_archive 'CCDC 863188' #TrackingRef '1CO.cif' #----------------------------------------------------------------------------- _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'APEX2 (Bruker, 2006)' _computing_data_reduction 'APEX2 (Bruker, 2006)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' #----------------------------------------------------------------------------- _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35.50 D B Cl F25 O' _chemical_formula_weight 972.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.3510(12) _cell_length_b 13.1576(6) _cell_length_c 19.6080(7) _cell_angle_alpha 90.00 _cell_angle_beta 112.633(2) _cell_angle_gamma 90.00 _cell_volume 6751.1(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 21967 _cell_measurement_theta_min 3.38 _cell_measurement_theta_max 68.03 _exptl_crystal_description prism' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.914 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3752 _exptl_absorpt_coefficient_mu 2.634 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5475 _exptl_absorpt_correction_T_max 0.7258 _exptl_absorpt_process_details 'APEX2 (Bruker, 2006)' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 CCD' _diffrn_measurement_method ' \w and \f ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21967 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 68.03 _reflns_number_total 6101 _reflns_number_gt 4715 _reflns_threshold_expression >2sigma(I) _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^)+(0.0758P)^2^+1.55P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6101 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1236 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.10513(10) 0.20207(19) 0.48468(15) 0.0398(5) Uani 1 1 d . . . O1 O 0.00146(7) 0.21206(16) 0.42337(13) 0.0661(6) Uani 1 1 d . . . C1 C 0.04367(10) 0.20448(19) 0.45266(16) 0.0493(6) Uani 1 1 d . . . C2 C 0.11633(8) 0.13668(17) 0.42232(13) 0.0378(5) Uani 1 1 d . . . C3 C 0.12504(8) 0.20224(16) 0.37562(13) 0.0372(5) Uani 1 1 d . . . C4 C 0.12369(8) 0.30973(17) 0.39890(13) 0.0380(5) Uani 1 1 d . . . C5 C 0.11495(8) 0.31578(17) 0.46150(12) 0.0373(5) Uani 1 1 d . . . C6 C 0.12240(9) 0.02541(18) 0.42452(13) 0.0406(5) Uani 1 1 d . . . C7 C 0.08813(10) -0.03810(19) 0.43836(15) 0.0491(6) Uani 1 1 d . . . C8 C 0.09588(13) -0.1408(2) 0.44953(18) 0.0609(7) Uani 1 1 d . . . C9 C 0.13960(13) -0.1844(2) 0.44743(18) 0.0622(7) Uani 1 1 d . . . C10 C 0.17519(11) -0.1244(2) 0.43455(15) 0.0537(6) Uani 1 1 d . . . C11 C 0.16624(9) -0.02166(18) 0.42280(13) 0.0431(5) Uani 1 1 d . . . C12 C 0.13538(8) 0.17732(17) 0.30882(13) 0.0388(5) Uani 1 1 d . . . C13 C 0.10017(9) 0.12772(18) 0.24823(14) 0.0446(5) Uani 1 1 d . . . C14 C 0.10964(10) 0.10912(19) 0.18527(14) 0.0512(6) Uani 1 1 d . . . C15 C 0.15509(12) 0.1397(2) 0.18190(15) 0.0535(6) Uani 1 1 d . . . C16 C 0.19156(10) 0.1877(2) 0.24182(16) 0.0507(6) Uani 1 1 d . . . C17 C 0.18118(9) 0.20548(18) 0.30351(13) 0.0421(5) Uani 1 1 d . . . C18 C 0.13197(8) 0.39797(17) 0.35796(13) 0.0385(5) Uani 1 1 d . . . C19 C 0.09924(9) 0.41895(19) 0.28576(14) 0.0448(5) Uani 1 1 d . . . C20 C 0.10637(11) 0.5007(2) 0.24792(16) 0.0549(6) Uani 1 1 d . . . C21 C 0.14714(12) 0.5646(2) 0.28066(18) 0.0596(7) Uani 1 1 d . . . C22 C 0.18038(10) 0.54754(19) 0.35301(17) 0.0534(6) Uani 1 1 d . . . C23 C 0.17224(9) 0.46506(18) 0.39050(14) 0.0424(5) Uani 1 1 d . . . C24 C 0.10973(8) 0.41150(17) 0.49682(13) 0.0376(5) Uani 1 1 d . . . C25 C 0.06627(8) 0.47163(17) 0.46763(13) 0.0391(5) Uani 1 1 d . . . C26 C 0.05975(9) 0.55947(17) 0.50060(15) 0.0431(5) Uani 1 1 d . . . C27 C 0.09813(10) 0.59143(18) 0.56466(15) 0.0471(6) Uani 1 1 d . . . C28 C 0.14205(10) 0.5352(2) 0.59532(14) 0.0482(6) Uani 1 1 d . . . C29 C 0.14707(8) 0.44537(18) 0.56259(13) 0.0423(5) Uani 1 1 d . . . C30 C 0.12925(9) 0.16790(16) 0.56896(13) 0.0387(5) Uani 1 1 d . . . C31 C 0.17829(9) 0.12851(18) 0.59925(13) 0.0413(5) Uani 1 1 d . . . C32 C 0.20140(10) 0.0996(2) 0.67240(15) 0.0504(6) Uani 1 1 d . . . C33 C 0.17565(11) 0.1095(2) 0.71768(15) 0.0540(6) Uani 1 1 d . . . C34 C 0.12701(12) 0.1476(2) 0.69119(16) 0.0558(7) Uani 1 1 d . . . C35 C 0.10477(10) 0.1767(2) 0.61778(17) 0.0530(6) Uani 1 1 d . . . F1 F 0.04533(6) 0.00140(12) 0.44202(11) 0.0645(5) Uani 1 1 d . . . F2 F 0.06185(9) -0.19808(14) 0.46330(14) 0.0862(6) Uani 1 1 d . . . F3 F 0.14784(10) -0.28422(13) 0.45920(14) 0.0899(7) Uani 1 1 d . . . F4 F 0.21802(7) -0.16544(13) 0.43388(11) 0.0693(5) Uani 1 1 d . . . F5 F 0.20244(5) 0.03424(11) 0.41354(8) 0.0466(3) Uani 1 1 d . . . F6 F 0.05522(6) 0.09945(13) 0.24934(10) 0.0610(4) Uani 1 1 d . . . F7 F 0.07469(7) 0.06176(13) 0.12748(9) 0.0701(5) Uani 1 1 d . . . F8 F 0.16426(8) 0.12269(14) 0.12104(9) 0.0736(5) Uani 1 1 d . . . F9 F 0.23601(7) 0.21484(15) 0.23898(11) 0.0719(5) Uani 1 1 d . . . F10 F 0.21704(5) 0.25080(12) 0.36117(8) 0.0526(4) Uani 1 1 d . . . F11 F 0.05895(6) 0.35814(12) 0.25197(8) 0.0560(4) Uani 1 1 d . . . F12 F 0.07344(7) 0.52068(15) 0.17852(10) 0.0733(5) Uani 1 1 d . . . F13 F 0.15494(9) 0.64337(15) 0.24355(13) 0.0875(6) Uani 1 1 d . . . F14 F 0.22027(7) 0.60861(13) 0.38530(12) 0.0748(5) Uani 1 1 d . . . F16 F 0.02829(5) 0.44176(11) 0.40517(9) 0.0528(4) Uani 1 1 d . . . F15 F 0.20493(5) 0.44909(12) 0.45961(8) 0.0536(4) Uani 1 1 d . . . F17 F 0.01621(5) 0.61297(11) 0.47170(10) 0.0567(4) Uani 1 1 d . . . F18 F 0.09253(7) 0.67594(12) 0.59869(10) 0.0642(4) Uani 1 1 d . . . F19 F 0.17885(7) 0.56583(15) 0.65852(10) 0.0721(5) Uani 1 1 d . . . F20 F 0.18965(5) 0.39035(12) 0.59447(9) 0.0566(4) Uani 1 1 d . . . F21 F 0.20556(5) 0.11777(14) 0.55743(8) 0.0573(4) Uani 1 1 d . . . F22 F 0.24866(6) 0.06092(15) 0.69841(9) 0.0715(5) Uani 1 1 d . . . F23 F 0.19753(8) 0.08019(15) 0.78873(9) 0.0756(5) Uani 1 1 d . . . F24 F 0.10157(9) 0.15550(19) 0.73586(12) 0.0884(6) Uani 1 1 d . . . F25 F 0.05730(7) 0.21428(17) 0.59378(11) 0.0770(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0480(13) 0.0312(12) 0.0429(14) -0.0020(10) 0.0207(11) 0.0012(10) O1 0.0442(10) 0.0576(12) 0.0924(16) -0.0109(11) 0.0216(10) -0.0007(8) C1 0.0542(15) 0.0366(12) 0.0618(16) -0.0072(11) 0.0275(13) -0.0025(10) C2 0.0405(10) 0.0326(11) 0.0399(12) -0.0022(9) 0.0148(9) 0.0002(8) C3 0.0370(10) 0.0320(11) 0.0391(12) -0.0010(9) 0.0110(9) 0.0012(8) C4 0.0380(10) 0.0329(11) 0.0413(12) -0.0008(9) 0.0134(9) 0.0017(8) C5 0.0392(10) 0.0332(11) 0.0386(12) 0.0005(9) 0.0140(9) 0.0015(8) C6 0.0522(12) 0.0336(11) 0.0363(11) -0.0024(9) 0.0176(10) 0.0015(9) C7 0.0621(14) 0.0364(12) 0.0551(15) -0.0022(11) 0.0297(12) -0.0004(11) C8 0.0865(19) 0.0362(13) 0.0724(19) 0.0019(13) 0.0443(16) -0.0048(13) C9 0.100(2) 0.0291(12) 0.0676(18) 0.0059(12) 0.0432(17) 0.0080(13) C10 0.0751(16) 0.0433(14) 0.0484(14) 0.0031(11) 0.0300(13) 0.0147(12) C11 0.0575(13) 0.0367(12) 0.0364(12) -0.0003(9) 0.0196(10) 0.0033(10) C12 0.0450(11) 0.0290(10) 0.0399(12) 0.0027(9) 0.0137(9) 0.0053(9) C13 0.0464(12) 0.0348(12) 0.0471(13) -0.0028(10) 0.0120(10) 0.0050(9) C14 0.0665(15) 0.0361(12) 0.0376(13) -0.0020(10) 0.0053(11) 0.0113(11) C15 0.0799(17) 0.0429(14) 0.0425(14) 0.0065(11) 0.0288(13) 0.0175(12) C16 0.0613(14) 0.0419(13) 0.0569(16) 0.0053(12) 0.0318(13) 0.0053(11) C17 0.0478(11) 0.0378(12) 0.0413(12) 0.0013(10) 0.0177(10) 0.0027(9) C18 0.0444(11) 0.0308(11) 0.0448(12) -0.0001(9) 0.0220(10) 0.0036(9) C19 0.0508(12) 0.0389(12) 0.0467(14) 0.0009(10) 0.0209(11) 0.0066(10) C20 0.0646(15) 0.0514(15) 0.0537(15) 0.0145(12) 0.0284(13) 0.0166(12) C21 0.0796(18) 0.0408(14) 0.075(2) 0.0186(13) 0.0478(16) 0.0104(13) C22 0.0597(14) 0.0371(13) 0.0760(19) -0.0073(12) 0.0400(14) -0.0063(11) C23 0.0436(11) 0.0370(12) 0.0491(13) -0.0009(10) 0.0206(10) 0.0020(9) C24 0.0434(11) 0.0328(11) 0.0401(12) 0.0003(9) 0.0200(9) -0.0012(9) C25 0.0389(10) 0.0345(11) 0.0431(12) -0.0005(10) 0.0149(9) -0.0038(9) C26 0.0454(11) 0.0322(11) 0.0579(15) 0.0021(10) 0.0266(11) 0.0009(9) C27 0.0604(13) 0.0337(12) 0.0544(15) -0.0079(11) 0.0301(12) -0.0023(10) C28 0.0570(13) 0.0461(13) 0.0392(13) -0.0088(11) 0.0161(11) -0.0065(11) C29 0.0431(11) 0.0410(12) 0.0413(12) 0.0013(10) 0.0147(10) 0.0033(9) C30 0.0504(12) 0.0280(10) 0.0429(13) -0.0013(9) 0.0238(10) -0.0017(9) C31 0.0493(12) 0.0371(12) 0.0390(12) -0.0035(10) 0.0188(10) -0.0007(9) C32 0.0581(14) 0.0455(14) 0.0439(14) -0.0023(11) 0.0157(11) 0.0016(11) C33 0.0798(17) 0.0416(14) 0.0422(14) -0.0004(11) 0.0251(13) -0.0060(12) C34 0.0803(18) 0.0504(15) 0.0512(16) -0.0049(12) 0.0415(14) -0.0051(13) C35 0.0607(14) 0.0456(14) 0.0622(17) -0.0022(12) 0.0340(13) 0.0040(11) F1 0.0660(9) 0.0428(8) 0.1001(13) 0.0031(8) 0.0490(9) -0.0013(7) F2 0.1134(15) 0.0436(9) 0.1306(19) 0.0109(10) 0.0791(15) -0.0086(9) F3 0.1344(17) 0.0351(9) 0.1254(18) 0.0192(10) 0.0777(15) 0.0188(10) F4 0.0866(11) 0.0540(10) 0.0775(12) 0.0126(9) 0.0430(10) 0.0302(9) F5 0.0515(7) 0.0427(7) 0.0484(8) 0.0013(6) 0.0224(6) 0.0045(6) F6 0.0503(8) 0.0587(9) 0.0672(10) -0.0151(8) 0.0152(7) -0.0082(7) F7 0.0819(11) 0.0600(10) 0.0469(9) -0.0153(8) 0.0010(8) 0.0145(8) F8 0.1166(14) 0.0670(11) 0.0483(9) 0.0035(8) 0.0440(10) 0.0186(10) F9 0.0827(11) 0.0726(11) 0.0835(12) -0.0052(10) 0.0577(10) -0.0049(9) F10 0.0467(7) 0.0561(9) 0.0554(9) -0.0109(7) 0.0202(6) -0.0060(6) F11 0.0537(8) 0.0570(9) 0.0478(8) 0.0001(7) 0.0091(6) -0.0027(7) F12 0.0867(11) 0.0794(12) 0.0537(10) 0.0250(9) 0.0268(9) 0.0212(10) F13 0.1149(15) 0.0574(11) 0.1113(17) 0.0353(11) 0.0670(14) 0.0034(10) F14 0.0808(11) 0.0508(9) 0.1067(15) -0.0132(10) 0.0513(11) -0.0261(8) F16 0.0444(7) 0.0447(8) 0.0572(9) -0.0061(7) 0.0064(6) 0.0017(6) F15 0.0469(7) 0.0581(9) 0.0530(9) -0.0066(7) 0.0163(6) -0.0078(6) F17 0.0502(7) 0.0394(8) 0.0810(11) -0.0002(7) 0.0258(7) 0.0096(6) F18 0.0834(10) 0.0426(8) 0.0703(11) -0.0184(8) 0.0338(9) 0.0017(7) F19 0.0766(10) 0.0695(11) 0.0526(10) -0.0216(8) 0.0054(8) -0.0021(9) F20 0.0517(7) 0.0565(9) 0.0497(8) -0.0024(7) 0.0063(6) 0.0112(7) F21 0.0437(7) 0.0844(11) 0.0470(8) -0.0091(8) 0.0211(6) 0.0036(7) F22 0.0646(9) 0.0883(13) 0.0487(9) -0.0008(9) 0.0076(7) 0.0193(9) F23 0.1075(14) 0.0740(12) 0.0423(9) 0.0081(8) 0.0255(9) -0.0015(10) F24 0.1082(15) 0.1153(18) 0.0707(13) 0.0009(11) 0.0664(12) 0.0032(12) F25 0.0710(10) 0.0994(15) 0.0757(12) 0.0062(10) 0.0449(9) 0.0292(10) _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 B1 C30 1.591(4) . ? B1 C1 1.609(3) . ? B1 C5 1.619(3) . ? B1 C2 1.623(3) . ? O1 C1 1.115(3) . ? C2 C3 1.348(3) . ? C2 C6 1.473(3) . ? C3 C12 1.485(3) . ? C3 C4 1.491(3) . ? C4 C5 1.345(3) . ? C4 C18 1.481(3) . ? C5 C24 1.472(3) . ? C6 C7 1.385(4) . ? C6 C11 1.401(3) . ? C7 F1 1.347(3) . ? C7 C8 1.373(4) . ? C8 F2 1.331(3) . ? C8 C9 1.381(5) . ? C9 F3 1.338(3) . ? C9 C10 1.379(4) . ? C10 F4 1.334(3) . ? C10 C11 1.378(4) . ? C11 F5 1.331(3) . ? C12 C13 1.386(3) . ? C12 C17 1.392(3) . ? C13 F6 1.336(3) . ? C13 C14 1.382(4) . ? C14 F7 1.338(3) . ? C14 C15 1.376(4) . ? C15 F8 1.334(3) . ? C15 C16 1.383(4) . ? C16 F9 1.331(3) . ? C16 C17 1.371(4) . ? C17 F10 1.335(3) . ? C18 C23 1.389(3) . ? C18 C19 1.389(3) . ? C19 F11 1.342(3) . ? C19 C20 1.365(4) . ? C20 F12 1.347(3) . ? C20 C21 1.373(4) . ? C21 F13 1.333(3) . ? C21 C22 1.386(4) . ? C22 F14 1.332(3) . ? C22 C23 1.379(4) . ? C23 F15 1.331(3) . ? C24 C25 1.389(3) . ? C24 C29 1.390(3) . ? C25 F16 1.341(3) . ? C25 C26 1.371(3) . ? C26 F17 1.343(3) . ? C26 C27 1.373(4) . ? C27 F18 1.337(3) . ? C27 C28 1.372(4) . ? C28 F19 1.338(3) . ? C28 C29 1.379(4) . ? C29 F20 1.339(3) . ? C30 C31 1.385(3) . ? C30 C35 1.387(4) . ? C31 F21 1.333(3) . ? C31 C32 1.381(4) . ? C32 F22 1.337(3) . ? C32 C33 1.355(4) . ? C33 F23 1.345(3) . ? C33 C34 1.368(4) . ? C34 F24 1.336(3) . ? C34 C35 1.385(4) . ? C35 F25 1.338(3) . ? 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 C30 B1 C1 112.3(2) . . ? C30 B1 C5 120.1(2) . . ? C1 B1 C5 98.61(18) . . ? C30 B1 C2 120.1(2) . . ? C1 B1 C2 102.29(19) . . ? C5 B1 C2 100.00(19) . . ? O1 C1 B1 171.6(3) . . ? C3 C2 C6 127.3(2) . . ? C3 C2 B1 108.2(2) . . ? C6 C2 B1 124.0(2) . . ? C2 C3 C12 127.4(2) . . ? C2 C3 C4 111.5(2) . . ? C12 C3 C4 121.1(2) . . ? C5 C4 C18 124.9(2) . . ? C5 C4 C3 111.8(2) . . ? C18 C4 C3 123.3(2) . . ? C4 C5 C24 124.6(2) . . ? C4 C5 B1 108.3(2) . . ? C24 C5 B1 126.8(2) . . ? C7 C6 C11 115.7(2) . . ? C7 C6 C2 121.5(2) . . ? C11 C6 C2 122.2(2) . . ? F1 C7 C8 117.6(2) . . ? F1 C7 C6 119.5(2) . . ? C8 C7 C6 122.9(3) . . ? F2 C8 C7 120.4(3) . . ? F2 C8 C9 120.0(3) . . ? C7 C8 C9 119.6(3) . . ? F3 C9 C10 120.2(3) . . ? F3 C9 C8 120.1(3) . . ? C10 C9 C8 119.7(3) . . ? F4 C10 C11 120.4(3) . . ? F4 C10 C9 120.2(2) . . ? C11 C10 C9 119.5(3) . . ? F5 C11 C10 117.6(2) . . ? F5 C11 C6 119.8(2) . . ? C10 C11 C6 122.5(2) . . ? C13 C12 C17 116.5(2) . . ? C13 C12 C3 122.6(2) . . ? C17 C12 C3 120.9(2) . . ? F6 C13 C14 118.7(2) . . ? F6 C13 C12 119.6(2) . . ? C14 C13 C12 121.7(2) . . ? F7 C14 C15 119.9(3) . . ? F7 C14 C13 120.2(3) . . ? C15 C14 C13 119.9(2) . . ? F8 C15 C14 120.2(3) . . ? F8 C15 C16 119.8(3) . . ? C14 C15 C16 120.0(2) . . ? F9 C16 C17 121.3(3) . . ? F9 C16 C15 119.8(3) . . ? C17 C16 C15 118.9(2) . . ? F10 C17 C16 118.1(2) . . ? F10 C17 C12 118.9(2) . . ? C16 C17 C12 123.0(2) . . ? C23 C18 C19 116.8(2) . . ? C23 C18 C4 121.5(2) . . ? C19 C18 C4 121.7(2) . . ? F11 C19 C20 118.5(2) . . ? F11 C19 C18 119.5(2) . . ? C20 C19 C18 122.0(2) . . ? F12 C20 C19 120.9(3) . . ? F12 C20 C21 119.0(3) . . ? C19 C20 C21 120.2(3) . . ? F13 C21 C20 120.5(3) . . ? F13 C21 C22 119.6(3) . . ? C20 C21 C22 119.9(2) . . ? F14 C22 C23 120.5(3) . . ? F14 C22 C21 120.5(3) . . ? C23 C22 C21 119.0(2) . . ? F15 C23 C22 118.2(2) . . ? F15 C23 C18 119.6(2) . . ? C22 C23 C18 122.1(2) . . ? C25 C24 C29 116.0(2) . . ? C25 C24 C5 121.8(2) . . ? C29 C24 C5 122.2(2) . . ? F16 C25 C26 118.1(2) . . ? F16 C25 C24 118.9(2) . . ? C26 C25 C24 123.0(2) . . ? F17 C26 C25 120.8(2) . . ? F17 C26 C27 120.1(2) . . ? C25 C26 C27 119.1(2) . . ? F18 C27 C28 119.4(2) . . ? F18 C27 C26 120.4(2) . . ? C28 C27 C26 120.1(2) . . ? F19 C28 C27 119.8(2) . . ? F19 C28 C29 120.4(2) . . ? C27 C28 C29 119.8(2) . . ? F20 C29 C28 118.9(2) . . ? F20 C29 C24 119.2(2) . . ? C28 C29 C24 121.9(2) . . ? C31 C30 C35 114.9(2) . . ? C31 C30 B1 120.7(2) . . ? C35 C30 B1 124.3(2) . . ? F21 C31 C32 117.0(2) . . ? F21 C31 C30 120.0(2) . . ? C32 C31 C30 123.0(2) . . ? F22 C32 C33 120.0(2) . . ? F22 C32 C31 120.4(2) . . ? C33 C32 C31 119.6(2) . . ? F23 C33 C32 120.1(3) . . ? F23 C33 C34 119.6(3) . . ? C32 C33 C34 120.3(3) . . ? F24 C34 C33 120.0(3) . . ? F24 C34 C35 121.0(3) . . ? C33 C34 C35 119.0(2) . . ? F25 C35 C34 117.5(2) . . ? F25 C35 C30 119.4(3) . . ? C34 C35 C30 123.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C30 B1 C2 C3 -138.1(2) . . . . ? C1 B1 C2 C3 96.8(2) . . . . ? C5 B1 C2 C3 -4.4(2) . . . . ? C30 B1 C2 C6 34.5(3) . . . . ? C1 B1 C2 C6 -90.6(3) . . . . ? C5 B1 C2 C6 168.2(2) . . . . ? C6 C2 C3 C12 9.7(4) . . . . ? B1 C2 C3 C12 -178.0(2) . . . . ? C6 C2 C3 C4 -169.8(2) . . . . ? B1 C2 C3 C4 2.5(2) . . . . ? C2 C3 C4 C5 1.0(3) . . . . ? C12 C3 C4 C5 -178.55(19) . . . . ? C2 C3 C4 C18 -180.0(2) . . . . ? C12 C3 C4 C18 0.4(3) . . . . ? C18 C4 C5 C24 3.2(3) . . . . ? C3 C4 C5 C24 -177.79(19) . . . . ? C18 C4 C5 B1 177.0(2) . . . . ? C3 C4 C5 B1 -4.0(2) . . . . ? C30 B1 C5 C4 138.7(2) . . . . ? C1 B1 C5 C4 -99.2(2) . . . . ? C2 B1 C5 C4 5.0(2) . . . . ? C30 B1 C5 C24 -47.7(3) . . . . ? C1 B1 C5 C24 74.4(3) . . . . ? C2 B1 C5 C24 178.6(2) . . . . ? C3 C2 C6 C7 -141.1(3) . . . . ? B1 C2 C6 C7 47.7(3) . . . . ? C3 C2 C6 C11 47.7(4) . . . . ? B1 C2 C6 C11 -123.5(3) . . . . ? C11 C6 C7 F1 179.0(2) . . . . ? C2 C6 C7 F1 7.3(4) . . . . ? C11 C6 C7 C8 -0.2(4) . . . . ? C2 C6 C7 C8 -172.0(3) . . . . ? F1 C7 C8 F2 0.1(4) . . . . ? C6 C7 C8 F2 179.4(3) . . . . ? F1 C7 C8 C9 -179.0(3) . . . . ? C6 C7 C8 C9 0.3(5) . . . . ? F2 C8 C9 F3 0.0(5) . . . . ? C7 C8 C9 F3 179.1(3) . . . . ? F2 C8 C9 C10 -178.8(3) . . . . ? C7 C8 C9 C10 0.4(5) . . . . ? F3 C9 C10 F4 -0.1(5) . . . . ? C8 C9 C10 F4 178.7(3) . . . . ? F3 C9 C10 C11 -179.8(3) . . . . ? C8 C9 C10 C11 -1.0(5) . . . . ? F4 C10 C11 F5 -2.3(4) . . . . ? C9 C10 C11 F5 177.4(3) . . . . ? F4 C10 C11 C6 -178.6(2) . . . . ? C9 C10 C11 C6 1.0(4) . . . . ? C7 C6 C11 F5 -176.7(2) . . . . ? C2 C6 C11 F5 -5.0(3) . . . . ? C7 C6 C11 C10 -0.4(4) . . . . ? C2 C6 C11 C10 171.3(2) . . . . ? C2 C3 C12 C13 62.8(3) . . . . ? C4 C3 C12 C13 -117.7(2) . . . . ? C2 C3 C12 C17 -118.9(3) . . . . ? C4 C3 C12 C17 60.6(3) . . . . ? C17 C12 C13 F6 -179.3(2) . . . . ? C3 C12 C13 F6 -0.9(3) . . . . ? C17 C12 C13 C14 -1.3(3) . . . . ? C3 C12 C13 C14 177.1(2) . . . . ? F6 C13 C14 F7 -1.4(3) . . . . ? C12 C13 C14 F7 -179.5(2) . . . . ? F6 C13 C14 C15 178.4(2) . . . . ? C12 C13 C14 C15 0.3(4) . . . . ? F7 C14 C15 F8 0.3(4) . . . . ? C13 C14 C15 F8 -179.5(2) . . . . ? F7 C14 C15 C16 -179.3(2) . . . . ? C13 C14 C15 C16 0.9(4) . . . . ? F8 C15 C16 F9 -1.4(4) . . . . ? C14 C15 C16 F9 178.3(2) . . . . ? F8 C15 C16 C17 179.3(2) . . . . ? C14 C15 C16 C17 -1.0(4) . . . . ? F9 C16 C17 F10 -0.1(4) . . . . ? C15 C16 C17 F10 179.2(2) . . . . ? F9 C16 C17 C12 -179.3(2) . . . . ? C15 C16 C17 C12 0.0(4) . . . . ? C13 C12 C17 F10 -178.0(2) . . . . ? C3 C12 C17 F10 3.5(3) . . . . ? C13 C12 C17 C16 1.2(3) . . . . ? C3 C12 C17 C16 -177.3(2) . . . . ? C5 C4 C18 C23 60.1(3) . . . . ? C3 C4 C18 C23 -118.7(2) . . . . ? C5 C4 C18 C19 -118.5(3) . . . . ? C3 C4 C18 C19 62.7(3) . . . . ? C23 C18 C19 F11 -178.5(2) . . . . ? C4 C18 C19 F11 0.2(3) . . . . ? C23 C18 C19 C20 0.7(3) . . . . ? C4 C18 C19 C20 179.4(2) . . . . ? F11 C19 C20 F12 0.7(4) . . . . ? C18 C19 C20 F12 -178.5(2) . . . . ? F11 C19 C20 C21 180.0(2) . . . . ? C18 C19 C20 C21 0.8(4) . . . . ? F12 C20 C21 F13 -2.1(4) . . . . ? C19 C20 C21 F13 178.6(2) . . . . ? F12 C20 C21 C22 177.6(2) . . . . ? C19 C20 C21 C22 -1.7(4) . . . . ? F13 C21 C22 F14 -0.7(4) . . . . ? C20 C21 C22 F14 179.6(2) . . . . ? F13 C21 C22 C23 -179.2(2) . . . . ? C20 C21 C22 C23 1.1(4) . . . . ? F14 C22 C23 F15 0.7(4) . . . . ? C21 C22 C23 F15 179.1(2) . . . . ? F14 C22 C23 C18 -178.0(2) . . . . ? C21 C22 C23 C18 0.4(4) . . . . ? C19 C18 C23 F15 180.0(2) . . . . ? C4 C18 C23 F15 1.3(3) . . . . ? C19 C18 C23 C22 -1.3(3) . . . . ? C4 C18 C23 C22 -180.0(2) . . . . ? C4 C5 C24 C25 73.7(3) . . . . ? B1 C5 C24 C25 -98.9(3) . . . . ? C4 C5 C24 C29 -108.6(3) . . . . ? B1 C5 C24 C29 78.8(3) . . . . ? C29 C24 C25 F16 -178.4(2) . . . . ? C5 C24 C25 F16 -0.6(3) . . . . ? C29 C24 C25 C26 0.1(3) . . . . ? C5 C24 C25 C26 177.9(2) . . . . ? F16 C25 C26 F17 1.1(3) . . . . ? C24 C25 C26 F17 -177.5(2) . . . . ? F16 C25 C26 C27 179.9(2) . . . . ? C24 C25 C26 C27 1.4(4) . . . . ? F17 C26 C27 F18 -0.1(4) . . . . ? C25 C26 C27 F18 -179.0(2) . . . . ? F17 C26 C27 C28 178.2(2) . . . . ? C25 C26 C27 C28 -0.7(4) . . . . ? F18 C27 C28 F19 -0.4(4) . . . . ? C26 C27 C28 F19 -178.7(2) . . . . ? F18 C27 C28 C29 176.8(2) . . . . ? C26 C27 C28 C29 -1.5(4) . . . . ? F19 C28 C29 F20 -1.1(4) . . . . ? C27 C28 C29 F20 -178.2(2) . . . . ? F19 C28 C29 C24 -179.7(2) . . . . ? C27 C28 C29 C24 3.1(4) . . . . ? C25 C24 C29 F20 179.0(2) . . . . ? C5 C24 C29 F20 1.2(3) . . . . ? C25 C24 C29 C28 -2.4(3) . . . . ? C5 C24 C29 C28 179.8(2) . . . . ? C1 B1 C30 C31 158.2(2) . . . . ? C5 B1 C30 C31 -86.7(3) . . . . ? C2 B1 C30 C31 37.9(3) . . . . ? C1 B1 C30 C35 -23.5(3) . . . . ? C5 B1 C30 C35 91.6(3) . . . . ? C2 B1 C30 C35 -143.8(2) . . . . ? C35 C30 C31 F21 -179.3(2) . . . . ? B1 C30 C31 F21 -0.8(3) . . . . ? C35 C30 C31 C32 0.2(4) . . . . ? B1 C30 C31 C32 178.7(2) . . . . ? F21 C31 C32 F22 -1.2(4) . . . . ? C30 C31 C32 F22 179.2(2) . . . . ? F21 C31 C32 C33 179.5(2) . . . . ? C30 C31 C32 C33 0.0(4) . . . . ? F22 C32 C33 F23 -0.2(4) . . . . ? C31 C32 C33 F23 179.0(2) . . . . ? F22 C32 C33 C34 -179.0(3) . . . . ? C31 C32 C33 C34 0.2(4) . . . . ? F23 C33 C34 F24 0.1(4) . . . . ? C32 C33 C34 F24 178.9(3) . . . . ? F23 C33 C34 C35 -179.5(2) . . . . ? C32 C33 C34 C35 -0.7(4) . . . . ? F24 C34 C35 F25 0.9(4) . . . . ? C33 C34 C35 F25 -179.5(3) . . . . ? F24 C34 C35 C30 -178.6(3) . . . . ? C33 C34 C35 C30 1.0(4) . . . . ? C31 C30 C35 F25 179.8(2) . . . . ? B1 C30 C35 F25 1.4(4) . . . . ? C31 C30 C35 C34 -0.7(4) . . . . ? B1 C30 C35 C34 -179.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 68.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.398 _refine_diff_density_min -0.209 _refine_diff_density_rms 0.048 # start Validation Reply Form _vrf_PUBL012_GLOBAL ; PROBLEM: _publ_section_abstract is missing. RESPONSE: Will appear in the article ; _vrf_PLAT051_Compound_I ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 28.28 Perc. RESPONSE: The asymmetric unit contains a half molecule of CD2Cl2 that showed gross disorder and was therefore, removed by the routine SQUEEZE. However, its contribution was used in the calculation of Mu, density of the crystal and molecular mass of the compound. ; ####################################################################### # # 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_jd1_47f _database_code_depnum_ccdc_archive 'CCDC 863189' #TrackingRef '863189.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2 1DMAP 1 CH2Cl2' _chemical_formula_sum 'C41.25 H10.50 B Cl0.25 F25 N2' _chemical_formula_weight 1028.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.003(2) _cell_length_b 19.158(4) _cell_length_c 20.004(4) _cell_angle_alpha 76.77(3) _cell_angle_beta 85.03(3) _cell_angle_gamma 73.96(3) _cell_volume 3944.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12589 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2025 _exptl_absorpt_coefficient_mu 0.201 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9329 _exptl_absorpt_correction_T_max 0.9647 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius APEX2 CCD' _diffrn_measurement_method ' \w and \f ' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25050 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.02 _reflns_number_total 13686 _reflns_number_gt 10651 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS (Schneider & Sheldrick, 2002)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. One molecule of CH2Cl2 has been modelled as disordered across the inversion centre' ; _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^)+(0.0908P)^2^+5.6789P] 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 13686 _refine_ls_number_parameters 1261 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1963 _refine_ls_wR_factor_gt 0.1758 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F24 F 0.2245(2) 0.16654(13) 0.13107(11) 0.0465(6) Uani 1 1 d . . . F23 F 0.0140(2) 0.40840(12) 0.29241(12) 0.0470(6) Uani 1 1 d . . . F22 F -0.0393(2) 0.36371(13) 0.10470(12) 0.0468(5) Uani 1 1 d . . . F21 F -0.1629(2) 0.50265(15) 0.04106(12) 0.0568(6) Uani 1 1 d . . . F20 F 0.2531(2) 0.46233(12) 0.18669(12) 0.0466(6) Uani 1 1 d . . . F19 F 0.1243(2) 0.24377(13) 0.39088(12) 0.0521(6) Uani 1 1 d . . . F18 F -0.0638(2) 0.20234(12) 0.22997(13) 0.0495(6) Uani 1 1 d . . . F17 F 0.6225(2) 0.15342(13) 0.21330(12) 0.0489(6) Uani 1 1 d . . . F16 F 0.1345(3) 0.59876(12) 0.11967(13) 0.0587(7) Uani 1 1 d . . . F15 F 0.2169(3) 0.06634(13) 0.25224(13) 0.0562(6) Uani 1 1 d . . . F14 F 0.7346(2) 0.06174(13) 0.13156(12) 0.0507(6) Uani 1 1 d . . . F13 F -0.2927(2) 0.23059(15) 0.29201(15) 0.0621(7) Uani 1 1 d . . . F12 F -0.0736(3) 0.62011(14) 0.04742(14) 0.0663(8) Uani 1 1 d . . . F11 F -0.2200(2) 0.43961(14) 0.34943(14) 0.0554(6) Uani 1 1 d . . . F10 F 0.3404(2) 0.07351(16) 0.05059(13) 0.0637(7) Uani 1 1 d . . . F9 F 0.2732(2) 0.32227(17) 0.03706(12) 0.0608(7) Uani 1 1 d . . . F8 F 0.5952(2) 0.01819(14) 0.05119(13) 0.0591(7) Uani 1 1 d . . . F7 F 0.0921(3) 0.13925(18) 0.49958(13) 0.0772(9) Uani 1 1 d . . . F6 F -0.3732(2) 0.35084(16) 0.35081(15) 0.0672(8) Uani 1 1 d . . . N3 N 0.4104(3) 0.21276(16) 0.29587(15) 0.0348(7) Uani 1 1 d . . . F5 F 0.5203(3) 0.34554(16) 0.20702(13) 0.0622(7) Uani 1 1 d . . . F4 F 0.1813(3) -0.03731(14) 0.36140(17) 0.0752(8) Uani 1 1 d . . . N4 N 0.4866(3) 0.19089(19) 0.50116(16) 0.0428(8) Uani 1 1 d . . . F3 F 0.4262(3) 0.37545(19) -0.06103(13) 0.0804(9) Uani 1 1 d . . . C7 C 0.1797(3) 0.33262(19) 0.18419(18) 0.0333(8) Uani 1 1 d . . . C39 C 0.1119(3) 0.40767(19) 0.14719(18) 0.0331(8) Uani 1 1 d . . . C38 C 0.5463(4) 0.1332(2) 0.17604(19) 0.0353(8) Uani 1 1 d . . . C37 C -0.0165(3) 0.30442(19) 0.25925(18) 0.0322(8) Uani 1 1 d . . . C36 C -0.0621(4) 0.3647(2) 0.28994(19) 0.0362(8) Uani 1 1 d . . . C35 C -0.2177(4) 0.2748(2) 0.2907(2) 0.0415(9) Uani 1 1 d . . . C50 C 0.4651(3) 0.1982(2) 0.43455(19) 0.0368(8) Uani 1 1 d . . . C34 C -0.0991(4) 0.26072(19) 0.25979(19) 0.0358(8) Uani 1 1 d . . . C33 C 0.1532(4) 0.4698(2) 0.14949(19) 0.0371(8) Uani 1 1 d . . . C32 C 0.0930(4) 0.5402(2) 0.1158(2) 0.0421(9) Uani 1 1 d . . . C31 C 0.0046(4) 0.4214(2) 0.10964(19) 0.0382(8) Uani 1 1 d . . . C150 C -0.2586(4) 0.3354(2) 0.3209(2) 0.0442(9) Uani 1 1 d . . . C29 C 0.3823(3) 0.2727(2) 0.3256(2) 0.0375(8) Uani 1 1 d . . . H29A H 0.3438 0.3203 0.2987 0.045 Uiso 1 1 calc R . . C28 C 0.6071(4) 0.0861(2) 0.13374(19) 0.0382(8) Uani 1 1 d . . . C27 C 0.4973(4) 0.1372(2) 0.40203(19) 0.0394(9) Uani 1 1 d . . . H27A H 0.5402 0.0894 0.4269 0.047 Uiso 1 1 calc R . . C26 C 0.4158(3) 0.16014(19) 0.18100(18) 0.0332(8) Uani 1 1 d . . . F91 F 0.1251(3) -0.00308(17) 0.48621(16) 0.0855(10) Uani 1 1 d . . . C25 C 0.4080(4) 0.0918(2) 0.0932(2) 0.0424(9) Uani 1 1 d . . . C24 C 0.5379(4) 0.0644(2) 0.0927(2) 0.0426(9) Uani 1 1 d . . . C23 C 0.1706(3) 0.1594(2) 0.31617(18) 0.0350(8) Uani 1 1 d . . . C22 C 0.3505(4) 0.1395(2) 0.13562(19) 0.0366(8) Uani 1 1 d . . . C21 C -0.0589(4) 0.4918(2) 0.0764(2) 0.0440(9) Uani 1 1 d . . . F2 F 0.6306(4) 0.4119(2) -0.02556(18) 0.1050(13) Uani 1 1 d . . . C20 C 0.4675(4) 0.1462(2) 0.33574(19) 0.0363(8) Uani 1 1 d . . . H20A H 0.4877 0.1035 0.3161 0.044 Uiso 1 1 calc R . . C19 C 0.4947(4) 0.3519(2) 0.1410(2) 0.0460(10) Uani 1 1 d . . . C18 C 0.4070(3) 0.2673(2) 0.39245(19) 0.0363(8) Uani 1 1 d . . . H18A H 0.3847 0.3108 0.4109 0.044 Uiso 1 1 calc R . . C17 C -0.1803(4) 0.3808(2) 0.3200(2) 0.0409(9) Uani 1 1 d . . . C16 C 0.4376(4) 0.2544(2) 0.5343(2) 0.0488(10) Uani 1 1 d . . . H16A H 0.3920 0.2975 0.5007 0.073 Uiso 1 1 calc R . . H16B H 0.5081 0.2663 0.5519 0.073 Uiso 1 1 calc R . . H16C H 0.3798 0.2417 0.5724 0.073 Uiso 1 1 calc R . . C15 C 0.3887(3) 0.33361(19) 0.12569(19) 0.0350(8) Uani 1 1 d . . . F1 F 0.6777(3) 0.3942(2) 0.1096(2) 0.1043(13) Uani 1 1 d . . . C8 C 0.3053(3) 0.30205(19) 0.17903(18) 0.0327(8) Uani 1 1 d . . . C13 C 0.3699(4) 0.3421(2) 0.0563(2) 0.0426(9) Uani 1 1 d . . . C6 C 0.1165(3) 0.28222(19) 0.23442(18) 0.0318(8) Uani 1 1 d . . . C11 C -0.0137(4) 0.5516(2) 0.0793(2) 0.0487(10) Uani 1 1 d . . . C9 C 0.1985(3) 0.21615(19) 0.25711(18) 0.0322(8) Uani 1 1 d . . . C301 C 0.5582(4) 0.1203(2) 0.5411(2) 0.0494(10) Uani 1 1 d . . . H30A H 0.5841 0.0839 0.5118 0.074 Uiso 1 1 calc R . . H30B H 0.5053 0.1024 0.5795 0.074 Uiso 1 1 calc R . . H30C H 0.6334 0.1271 0.5589 0.074 Uiso 1 1 calc R . . C208 C 0.1221(4) 0.1218(3) 0.4379(2) 0.0528(11) Uani 1 1 d . . . C207 C 0.1858(4) 0.0863(2) 0.3125(2) 0.0427(9) Uani 1 1 d . . . C206 C 0.1685(4) 0.0319(2) 0.3688(2) 0.0512(11) Uani 1 1 d . . . C205 C 0.1377(4) 0.1749(2) 0.3815(2) 0.0442(9) Uani 1 1 d . . . C204 C 0.1378(4) 0.0500(3) 0.4310(2) 0.0578(12) Uani 1 1 d . . . C203 C 0.5765(5) 0.3777(3) 0.0917(3) 0.0628(13) Uani 1 1 d . . . B2 B 0.3402(4) 0.2189(2) 0.2276(2) 0.0331(9) Uani 1 1 d . . . C201 C 0.4488(5) 0.3687(3) 0.0053(2) 0.0560(11) Uani 1 1 d . . . C202 C 0.5524(5) 0.3862(3) 0.0230(3) 0.0648(13) Uani 1 1 d . . . F83 F 0.1280(2) 0.60700(12) 0.27290(12) 0.0470(5) Uani 1 1 d . . . F82 F -0.3005(2) 0.84501(13) 0.36271(12) 0.0491(6) Uani 1 1 d . . . F81 F -0.0268(2) 0.94434(12) 0.19568(11) 0.0452(5) Uani 1 1 d . . . F80 F -0.2434(2) 0.60354(13) 0.40890(12) 0.0490(6) Uani 1 1 d . . . F79 F 0.1460(2) 0.80213(13) 0.24792(12) 0.0519(6) Uani 1 1 d . . . F78 F -0.0768(2) 0.69694(13) 0.43907(11) 0.0483(6) Uani 1 1 d . . . F77 F -0.0485(3) 1.05307(13) 0.25978(12) 0.0554(6) Uani 1 1 d . . . F76 F -0.3201(2) 0.95625(14) 0.42665(13) 0.0564(6) Uani 1 1 d . . . F75 F -0.1375(2) 0.58495(13) 0.20545(12) 0.0508(6) Uani 1 1 d . . . F74 F 0.2395(3) 0.46974(14) 0.34236(14) 0.0622(7) Uani 1 1 d . . . F73 F 0.3012(2) 0.82278(14) 0.33317(15) 0.0592(7) Uani 1 1 d . . . F72 F -0.4843(2) 0.89850(14) 0.26174(13) 0.0596(7) Uani 1 1 d . . . F71 F -0.2939(2) 0.74268(14) 0.10887(12) 0.0568(7) Uani 1 1 d . . . F70 F -0.1309(3) 0.46492(14) 0.47669(12) 0.0602(7) Uani 1 1 d . . . F69 F 0.0906(3) 0.70817(15) 0.52256(12) 0.0607(7) Uani 1 1 d . . . F68 F -0.1949(3) 1.06234(13) 0.37514(13) 0.0583(7) Uani 1 1 d . . . F67 F -0.4958(2) 0.72136(16) 0.30914(16) 0.0682(8) Uani 1 1 d . . . F66 F -0.2705(3) 0.49362(14) 0.18516(15) 0.0647(7) Uani 1 1 d . . . F65 F -0.5026(3) 0.79640(17) 0.03275(14) 0.0731(8) Uani 1 1 d . . . F64 F 0.2759(3) 0.77373(17) 0.47151(16) 0.0703(8) Uani 1 1 d . . . F63 F -0.6911(3) 0.95090(16) 0.18505(16) 0.0713(8) Uani 1 1 d . . . F62 F 0.1122(3) 0.39827(13) 0.44409(14) 0.0702(8) Uani 1 1 d . . . F61 F -0.7035(3) 0.89946(17) 0.07093(16) 0.0764(9) Uani 1 1 d . . . C90 C -0.0618(4) 0.61048(19) 0.33885(18) 0.0337(8) Uani 1 1 d . . . N1 N -0.0930(3) 0.82632(16) 0.16556(15) 0.0372(7) Uani 1 1 d . . . C100 C -0.1048(4) 0.9450(2) 0.25163(18) 0.0352(8) Uani 1 1 d . . . C89 C 0.0615(4) 0.5741(2) 0.32388(19) 0.0378(8) Uani 1 1 d . . . C88 C -0.1132(4) 1.0021(2) 0.2842(2) 0.0409(9) Uani 1 1 d . . . C87 C -0.2407(4) 0.8978(2) 0.3335(2) 0.0384(8) Uani 1 1 d . . . C86 C -0.2510(4) 0.9537(2) 0.3679(2) 0.0434(9) Uani 1 1 d . . . C4 C -0.2398(4) 0.7102(2) 0.26352(18) 0.0351(8) Uani 1 1 d . . . C2 C -0.0677(3) 0.74497(19) 0.29394(17) 0.0323(8) Uani 1 1 d . . . C83 C -0.3118(3) 0.6569(2) 0.25700(18) 0.0340(8) Uani 1 1 d . . . C82 C -0.1076(4) 0.8953(2) 0.04930(19) 0.0426(9) Uani 1 1 d . . . H82A H -0.1473 0.9389 0.0173 0.051 Uiso 1 1 calc R . . C81 C -0.3820(4) 0.8174(2) 0.18955(19) 0.0384(8) Uani 1 1 d . . . F60 F -0.6295(3) 0.6325(2) 0.2866(2) 0.1057(13) Uani 1 1 d . . . C80 C 0.0299(4) 0.74634(19) 0.33909(19) 0.0343(8) Uani 1 1 d . . . C79 C -0.2597(4) 0.5974(2) 0.22643(19) 0.0378(8) Uani 1 1 d . . . C30 C -0.1706(4) 0.89096(19) 0.27314(18) 0.0355(8) Uani 1 1 d . . . C3 C -0.1199(3) 0.68749(19) 0.30085(17) 0.0328(8) Uani 1 1 d . . . C76 C 0.1292(4) 0.7786(2) 0.3156(2) 0.0387(8) Uani 1 1 d . . . C75 C 0.0207(4) 0.7235(2) 0.4106(2) 0.0392(8) Uani 1 1 d . . . C74 C -0.5923(4) 0.9002(2) 0.1664(2) 0.0515(11) Uani 1 1 d . . . C73 C -0.1466(4) 0.8861(2) 0.11649(19) 0.0400(9) Uani 1 1 d . . . H73A H -0.2149 0.9236 0.1296 0.048 Uiso 1 1 calc R . . C72 C -0.1867(4) 1.0069(2) 0.3428(2) 0.0425(9) Uani 1 1 d . . . C71 C -0.4852(4) 0.8722(2) 0.2050(2) 0.0443(9) Uani 1 1 d . . . C70 C 0.1032(4) 0.7312(2) 0.4543(2) 0.0447(9) Uani 1 1 d . . . C69 C -0.0089(4) 0.8403(2) 0.02701(19) 0.0448(10) Uani 1 1 d . . . C68 C 0.1980(4) 0.7645(2) 0.4288(2) 0.0482(10) Uani 1 1 d . . . N2 N 0.0332(4) 0.8471(2) -0.03848(17) 0.0568(10) Uani 1 1 d . . . F51 F -0.5177(3) 0.51673(19) 0.2245(2) 0.0922(11) Uani 1 1 d . . . C67 C 0.1208(4) 0.5035(2) 0.3590(2) 0.0440(9) Uani 1 1 d . . . C66 C -0.3907(4) 0.7943(2) 0.1291(2) 0.0455(9) Uani 1 1 d . . . C65 C -0.0672(4) 0.5007(2) 0.42626(19) 0.0430(10) Uani 1 1 d . . . C64 C -0.3262(4) 0.5507(2) 0.2151(2) 0.0463(10) Uani 1 1 d . . . C63 C -0.0003(4) 0.7722(2) 0.1449(2) 0.0458(10) Uani 1 1 d . . . H63A H 0.0360 0.7288 0.1781 0.055 Uiso 1 1 calc R . . C62 C -0.5989(4) 0.8738(2) 0.1086(2) 0.0539(11) Uani 1 1 d . . . C61 C -0.4370(4) 0.6663(2) 0.2771(2) 0.0480(10) Uani 1 1 d . . . C60 C 0.2112(4) 0.7888(2) 0.3588(2) 0.0445(10) Uani 1 1 d . . . C5 C -0.2718(4) 0.7834(2) 0.23479(18) 0.0359(8) Uani 1 1 d . . . B1 B -0.1523(4) 0.8167(2) 0.2421(2) 0.0353(9) Uani 1 1 d . . . C58 C -0.1241(4) 0.5716(2) 0.39074(19) 0.0381(8) Uani 1 1 d . . . C57 C 0.1361(7) 0.7891(3) -0.0595(3) 0.086(2) Uani 1 1 d . . . H57A H 0.1607 0.7474 -0.0202 0.129 Uiso 1 1 calc R . . H57B H 0.2088 0.8091 -0.0759 0.129 Uiso 1 1 calc R . . H57C H 0.1079 0.7719 -0.0964 0.129 Uiso 1 1 calc R . . C56 C 0.0551(5) 0.4670(2) 0.4105(2) 0.0478(10) Uani 1 1 d . . . C55 C -0.5079(4) 0.6199(3) 0.2667(3) 0.0630(13) Uani 1 1 d . . . C54 C -0.4969(5) 0.8207(3) 0.0898(2) 0.0536(11) Uani 1 1 d . . . C53 C -0.4515(5) 0.5622(3) 0.2350(3) 0.0579(12) Uani 1 1 d . . . C52 C -0.0185(5) 0.9148(3) -0.0896(2) 0.0594(12) Uani 1 1 d . . . H52A H -0.0865 0.9484 -0.0684 0.089 Uiso 1 1 calc R . . H52B H -0.0521 0.9019 -0.1276 0.089 Uiso 1 1 calc R . . H52C H 0.0486 0.9393 -0.1072 0.089 Uiso 1 1 calc R . . C51 C 0.0437(5) 0.7772(2) 0.0784(2) 0.0532(11) Uani 1 1 d . . . H51A H 0.1100 0.7379 0.0665 0.064 Uiso 1 1 calc R . . Cl1 Cl 0.5775(6) 0.4266(3) 0.5415(4) 0.181(3) Uani 0.50 1 d PD . . C101 C 0.521(2) 0.5221(6) 0.5456(9) 0.152(8) Uani 0.50 1 d PD . . H10A H 0.5926 0.5435 0.5476 0.183 Uiso 0.50 1 calc PR . . H10B H 0.4656 0.5278 0.5868 0.183 Uiso 0.50 1 calc PR . . 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 F24 0.0350(12) 0.0586(14) 0.0479(13) -0.0241(11) -0.0058(10) -0.0037(10) F23 0.0443(13) 0.0480(13) 0.0617(14) -0.0292(11) 0.0112(11) -0.0229(10) F22 0.0435(13) 0.0543(14) 0.0464(13) -0.0098(11) -0.0057(10) -0.0185(11) F21 0.0422(14) 0.0695(17) 0.0470(14) -0.0048(12) -0.0091(11) 0.0006(12) F20 0.0486(14) 0.0378(12) 0.0572(14) -0.0131(10) -0.0107(11) -0.0125(10) F19 0.0635(16) 0.0522(14) 0.0428(13) -0.0205(11) 0.0034(11) -0.0118(12) F18 0.0518(14) 0.0409(12) 0.0659(15) -0.0257(11) 0.0017(11) -0.0180(11) F17 0.0374(12) 0.0575(14) 0.0588(14) -0.0287(12) -0.0041(10) -0.0099(11) F16 0.0783(18) 0.0302(12) 0.0651(16) -0.0090(11) 0.0004(13) -0.0120(12) F15 0.0801(18) 0.0383(13) 0.0551(15) -0.0179(11) 0.0099(13) -0.0208(12) F14 0.0358(13) 0.0536(14) 0.0590(15) -0.0205(12) 0.0009(10) 0.0003(10) F13 0.0484(15) 0.0621(16) 0.090(2) -0.0252(14) 0.0053(13) -0.0325(13) F12 0.0761(19) 0.0413(14) 0.0585(16) 0.0027(12) -0.0091(13) 0.0133(13) F11 0.0470(14) 0.0541(14) 0.0721(16) -0.0355(13) 0.0127(12) -0.0111(11) F10 0.0580(16) 0.0834(19) 0.0618(16) -0.0459(15) -0.0097(13) -0.0115(14) F9 0.0506(15) 0.096(2) 0.0399(13) -0.0168(13) -0.0051(11) -0.0224(14) F8 0.0586(16) 0.0640(16) 0.0567(15) -0.0389(13) 0.0036(12) 0.0004(12) F7 0.092(2) 0.084(2) 0.0370(14) -0.0053(13) 0.0089(14) -0.0033(17) F6 0.0401(14) 0.0830(19) 0.088(2) -0.0367(16) 0.0224(13) -0.0238(13) N3 0.0376(17) 0.0316(16) 0.0351(16) -0.0120(13) -0.0035(13) -0.0046(13) F5 0.0576(16) 0.091(2) 0.0535(15) -0.0227(14) -0.0023(12) -0.0388(15) F4 0.091(2) 0.0351(14) 0.093(2) 0.0003(13) 0.0034(17) -0.0190(14) N4 0.047(2) 0.0500(19) 0.0348(17) -0.0111(15) -0.0052(14) -0.0153(16) F3 0.091(2) 0.104(2) 0.0391(15) -0.0067(15) 0.0113(14) -0.0257(19) C7 0.037(2) 0.0308(18) 0.0346(19) -0.0108(15) -0.0040(15) -0.0085(15) C39 0.0317(19) 0.0317(18) 0.0338(18) -0.0086(15) -0.0003(15) -0.0037(15) C38 0.037(2) 0.0333(18) 0.0376(19) -0.0119(15) -0.0041(16) -0.0090(15) C37 0.0322(19) 0.0292(18) 0.0332(18) -0.0058(14) -0.0020(15) -0.0055(15) C36 0.038(2) 0.0340(19) 0.040(2) -0.0127(16) 0.0003(16) -0.0127(16) C35 0.036(2) 0.043(2) 0.052(2) -0.0108(18) -0.0016(17) -0.0199(17) C50 0.0289(19) 0.046(2) 0.038(2) -0.0132(17) 0.0008(15) -0.0118(16) C34 0.041(2) 0.0281(18) 0.040(2) -0.0091(15) -0.0050(16) -0.0094(15) C33 0.036(2) 0.036(2) 0.0355(19) -0.0097(16) -0.0004(16) -0.0024(16) C32 0.049(2) 0.033(2) 0.040(2) -0.0111(16) 0.0037(18) -0.0038(17) C31 0.037(2) 0.039(2) 0.037(2) -0.0078(16) 0.0036(16) -0.0081(16) C150 0.031(2) 0.051(2) 0.051(2) -0.0114(19) 0.0029(17) -0.0131(18) C29 0.035(2) 0.0325(19) 0.045(2) -0.0160(16) -0.0034(16) -0.0032(15) C28 0.035(2) 0.037(2) 0.038(2) -0.0078(16) 0.0011(16) -0.0021(16) C27 0.040(2) 0.038(2) 0.038(2) -0.0060(16) -0.0068(16) -0.0060(16) C26 0.038(2) 0.0304(18) 0.0309(18) -0.0076(15) -0.0014(15) -0.0074(15) F91 0.087(2) 0.0694(19) 0.0707(19) 0.0272(15) 0.0103(16) -0.0111(17) C25 0.050(2) 0.045(2) 0.037(2) -0.0195(17) -0.0052(17) -0.0114(18) C24 0.048(2) 0.042(2) 0.039(2) -0.0202(17) 0.0030(17) -0.0057(18) C23 0.0316(19) 0.038(2) 0.0339(19) -0.0069(15) -0.0012(15) -0.0071(15) C22 0.035(2) 0.039(2) 0.0365(19) -0.0123(16) -0.0027(15) -0.0060(16) C21 0.032(2) 0.053(2) 0.037(2) -0.0068(18) 0.0002(16) 0.0022(18) F2 0.110(3) 0.138(3) 0.084(2) -0.026(2) 0.051(2) -0.077(3) C20 0.040(2) 0.0295(18) 0.038(2) -0.0101(15) -0.0029(16) -0.0042(15) C19 0.044(2) 0.051(2) 0.048(2) -0.0192(19) 0.0025(19) -0.0154(19) C18 0.036(2) 0.039(2) 0.038(2) -0.0172(16) 0.0003(16) -0.0090(16) C17 0.041(2) 0.041(2) 0.043(2) -0.0176(17) 0.0011(17) -0.0084(17) C16 0.053(3) 0.061(3) 0.040(2) -0.025(2) 0.0033(19) -0.019(2) C15 0.0320(19) 0.0308(18) 0.040(2) -0.0098(15) 0.0039(15) -0.0043(15) F1 0.087(2) 0.159(4) 0.110(3) -0.057(3) 0.031(2) -0.090(3) C8 0.034(2) 0.0301(18) 0.0369(19) -0.0126(15) -0.0020(15) -0.0085(15) C13 0.037(2) 0.047(2) 0.043(2) -0.0116(18) 0.0019(17) -0.0090(17) C6 0.035(2) 0.0316(18) 0.0315(18) -0.0125(15) -0.0006(15) -0.0090(15) C11 0.051(3) 0.041(2) 0.040(2) -0.0055(18) 0.0044(19) 0.0075(19) C9 0.037(2) 0.0302(18) 0.0332(18) -0.0101(15) -0.0021(15) -0.0111(15) C301 0.053(3) 0.061(3) 0.037(2) -0.0074(19) -0.0067(19) -0.020(2) C208 0.054(3) 0.056(3) 0.037(2) -0.0025(19) 0.0036(19) -0.004(2) C207 0.043(2) 0.038(2) 0.044(2) -0.0105(18) 0.0015(18) -0.0064(17) C206 0.051(3) 0.032(2) 0.063(3) 0.0031(19) -0.002(2) -0.0096(18) C205 0.041(2) 0.046(2) 0.043(2) -0.0073(18) -0.0034(17) -0.0071(18) C204 0.051(3) 0.056(3) 0.050(3) 0.014(2) 0.003(2) -0.009(2) C203 0.050(3) 0.072(3) 0.081(4) -0.030(3) 0.018(2) -0.036(2) B2 0.035(2) 0.033(2) 0.033(2) -0.0098(17) -0.0028(17) -0.0076(17) C201 0.064(3) 0.059(3) 0.039(2) -0.008(2) 0.007(2) -0.011(2) C202 0.068(3) 0.072(3) 0.062(3) -0.023(3) 0.027(3) -0.031(3) F83 0.0451(13) 0.0415(12) 0.0482(13) -0.0010(10) 0.0077(10) -0.0111(10) F82 0.0607(15) 0.0478(13) 0.0458(13) -0.0135(11) 0.0161(11) -0.0283(12) F81 0.0586(15) 0.0421(12) 0.0381(12) -0.0073(10) 0.0099(10) -0.0228(11) F80 0.0532(15) 0.0500(13) 0.0455(13) -0.0081(11) 0.0102(11) -0.0218(11) F79 0.0496(14) 0.0523(14) 0.0518(14) 0.0003(11) 0.0084(11) -0.0227(11) F78 0.0581(15) 0.0598(14) 0.0359(12) -0.0090(10) 0.0051(10) -0.0328(12) F77 0.0809(18) 0.0442(13) 0.0528(14) -0.0095(11) 0.0040(13) -0.0379(13) F76 0.0639(16) 0.0604(15) 0.0528(14) -0.0277(12) 0.0196(12) -0.0229(13) F75 0.0461(14) 0.0542(14) 0.0563(14) -0.0263(12) 0.0116(11) -0.0122(11) F74 0.0584(17) 0.0468(14) 0.0680(17) -0.0062(12) -0.0021(13) 0.0032(12) F73 0.0381(13) 0.0567(15) 0.0896(19) -0.0174(14) 0.0067(13) -0.0245(12) F72 0.0597(16) 0.0577(15) 0.0618(16) -0.0293(13) -0.0056(12) -0.0018(12) F71 0.0652(17) 0.0554(15) 0.0442(13) -0.0184(12) -0.0043(12) 0.0001(12) F70 0.094(2) 0.0481(14) 0.0428(13) 0.0023(11) 0.0050(13) -0.0383(14) F69 0.0703(18) 0.0737(18) 0.0422(14) -0.0133(12) -0.0084(12) -0.0231(14) F68 0.0818(19) 0.0438(13) 0.0591(15) -0.0257(12) 0.0025(13) -0.0219(13) F67 0.0496(15) 0.0699(18) 0.098(2) -0.0519(17) 0.0216(14) -0.0169(13) F66 0.0794(19) 0.0506(15) 0.0749(18) -0.0353(14) 0.0024(15) -0.0182(13) F65 0.092(2) 0.0759(19) 0.0488(15) -0.0174(14) -0.0265(14) -0.0075(16) F64 0.0549(16) 0.086(2) 0.084(2) -0.0294(16) -0.0193(14) -0.0262(15) F63 0.0525(16) 0.0639(17) 0.088(2) -0.0232(15) -0.0109(14) 0.0084(13) F62 0.103(2) 0.0336(13) 0.0579(16) 0.0082(12) -0.0101(15) -0.0043(14) F61 0.0655(19) 0.0762(19) 0.081(2) -0.0056(16) -0.0331(16) -0.0081(15) C90 0.043(2) 0.0292(18) 0.0313(18) -0.0050(14) -0.0030(15) -0.0146(16) N1 0.0489(19) 0.0300(16) 0.0314(16) -0.0053(13) 0.0041(14) -0.0110(14) C100 0.041(2) 0.0320(18) 0.0308(18) -0.0025(15) 0.0001(15) -0.0098(16) C89 0.047(2) 0.0321(19) 0.0354(19) -0.0046(16) -0.0017(17) -0.0136(17) C88 0.054(2) 0.0306(19) 0.039(2) -0.0013(16) -0.0065(18) -0.0173(17) C87 0.043(2) 0.0319(19) 0.043(2) -0.0086(16) 0.0052(17) -0.0151(16) C86 0.049(2) 0.041(2) 0.038(2) -0.0118(17) 0.0065(18) -0.0079(18) C4 0.041(2) 0.0338(19) 0.0318(18) -0.0092(15) 0.0039(15) -0.0124(16) C2 0.038(2) 0.0289(17) 0.0308(18) -0.0074(14) 0.0054(15) -0.0109(15) C83 0.036(2) 0.0349(19) 0.0335(18) -0.0077(15) 0.0000(15) -0.0129(15) C82 0.056(3) 0.041(2) 0.0319(19) -0.0005(16) -0.0066(17) -0.0190(19) C81 0.043(2) 0.0346(19) 0.037(2) -0.0057(16) -0.0004(16) -0.0117(17) F60 0.0486(18) 0.123(3) 0.178(4) -0.082(3) 0.029(2) -0.0449(19) C80 0.039(2) 0.0258(17) 0.039(2) -0.0072(15) 0.0031(16) -0.0114(15) C79 0.041(2) 0.041(2) 0.0331(19) -0.0092(16) 0.0015(16) -0.0132(17) C30 0.043(2) 0.0294(18) 0.0332(19) -0.0021(15) -0.0018(16) -0.0110(16) C3 0.039(2) 0.0322(18) 0.0283(17) -0.0073(14) 0.0047(15) -0.0116(15) C76 0.037(2) 0.0294(18) 0.046(2) -0.0050(16) 0.0049(17) -0.0063(16) C75 0.042(2) 0.036(2) 0.042(2) -0.0102(16) 0.0032(17) -0.0156(17) C74 0.048(3) 0.038(2) 0.062(3) -0.008(2) -0.006(2) -0.0025(19) C73 0.051(2) 0.0313(19) 0.037(2) -0.0047(16) -0.0032(17) -0.0117(17) C72 0.055(3) 0.0321(19) 0.041(2) -0.0093(16) -0.0043(18) -0.0112(18) C71 0.051(2) 0.039(2) 0.044(2) -0.0106(18) -0.0031(18) -0.0111(18) C70 0.049(2) 0.044(2) 0.043(2) -0.0109(18) -0.0076(18) -0.0102(19) C69 0.068(3) 0.040(2) 0.033(2) -0.0088(17) 0.0083(19) -0.028(2) C68 0.037(2) 0.048(2) 0.064(3) -0.019(2) -0.0124(19) -0.0088(18) N2 0.091(3) 0.051(2) 0.0340(18) -0.0088(16) 0.0083(18) -0.030(2) F51 0.082(2) 0.090(2) 0.137(3) -0.053(2) 0.001(2) -0.0548(19) C67 0.052(3) 0.033(2) 0.045(2) -0.0073(17) -0.0071(18) -0.0055(18) C66 0.052(3) 0.039(2) 0.044(2) -0.0075(18) -0.0032(19) -0.0087(18) C65 0.069(3) 0.036(2) 0.0302(19) -0.0028(16) -0.0024(18) -0.027(2) C64 0.058(3) 0.036(2) 0.048(2) -0.0186(18) -0.004(2) -0.0105(19) C63 0.068(3) 0.0244(18) 0.039(2) -0.0011(16) 0.0078(19) -0.0090(18) C62 0.053(3) 0.048(2) 0.056(3) -0.002(2) -0.015(2) -0.009(2) C61 0.042(2) 0.047(2) 0.063(3) -0.027(2) 0.005(2) -0.0144(19) C60 0.032(2) 0.035(2) 0.069(3) -0.0153(19) 0.0020(19) -0.0104(16) C5 0.042(2) 0.0337(19) 0.0312(18) -0.0076(15) 0.0011(15) -0.0092(16) B1 0.042(2) 0.031(2) 0.033(2) -0.0054(17) 0.0037(18) -0.0129(18) C58 0.048(2) 0.036(2) 0.0353(19) -0.0104(16) 0.0016(17) -0.0186(17) C57 0.138(6) 0.069(3) 0.049(3) -0.023(3) 0.036(3) -0.027(4) C56 0.074(3) 0.028(2) 0.039(2) -0.0010(17) -0.012(2) -0.011(2) C55 0.039(3) 0.069(3) 0.090(4) -0.029(3) 0.009(2) -0.023(2) C54 0.069(3) 0.052(3) 0.040(2) -0.0052(19) -0.013(2) -0.015(2) C53 0.058(3) 0.055(3) 0.075(3) -0.029(2) -0.004(2) -0.027(2) C52 0.076(3) 0.071(3) 0.032(2) 0.001(2) 0.004(2) -0.033(3) C51 0.079(3) 0.033(2) 0.041(2) -0.0082(18) 0.014(2) -0.010(2) Cl1 0.158(5) 0.110(4) 0.263(8) -0.014(4) 0.050(5) -0.052(3) C101 0.19(2) 0.164(18) 0.116(13) -0.057(13) 0.087(14) -0.078(16) _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 F24 C22 1.342(4) . ? F23 C36 1.349(4) . ? F22 C31 1.348(4) . ? F21 C21 1.339(5) . ? F20 C33 1.337(4) . ? F19 C205 1.341(5) . ? F18 C34 1.335(4) . ? F17 C38 1.352(4) . ? F16 C32 1.341(5) . ? F15 C207 1.335(5) . ? F14 C28 1.351(4) . ? F13 C35 1.331(4) . ? F12 C11 1.333(5) . ? F11 C17 1.339(4) . ? F10 C25 1.339(4) . ? F9 C13 1.336(5) . ? F8 C24 1.344(4) . ? F7 C208 1.342(5) . ? F6 C150 1.334(5) . ? N3 C20 1.355(5) . ? N3 C29 1.362(4) . ? N3 B2 1.593(5) . ? F5 C19 1.345(5) . ? F4 C206 1.335(5) . ? N4 C50 1.342(5) . ? N4 C301 1.453(5) . ? N4 C16 1.467(5) . ? F3 C201 1.342(5) . ? C7 C8 1.349(5) . ? C7 C39 1.479(5) . ? C7 C6 1.494(5) . ? C39 C31 1.385(5) . ? C39 C33 1.398(5) . ? C38 C28 1.378(5) . ? C38 C26 1.388(5) . ? C37 C36 1.383(5) . ? C37 C34 1.394(5) . ? C37 C6 1.481(5) . ? C36 C17 1.370(5) . ? C35 C34 1.378(6) . ? C35 C150 1.379(6) . ? C50 C18 1.409(5) . ? C50 C27 1.413(5) . ? C33 C32 1.370(5) . ? C32 C11 1.376(6) . ? C31 C21 1.378(6) . ? C150 C17 1.380(6) . ? C29 C18 1.362(5) . ? C29 H29A 0.9500 . ? C28 C24 1.366(5) . ? C27 C20 1.355(5) . ? C27 H27A 0.9500 . ? C26 C22 1.390(5) . ? C26 B2 1.630(5) . ? F91 C204 1.346(5) . ? C25 C22 1.377(5) . ? C25 C24 1.380(6) . ? C23 C207 1.383(5) . ? C23 C205 1.400(5) . ? C23 C9 1.485(5) . ? C21 C11 1.384(6) . ? F2 C202 1.340(5) . ? C20 H20A 0.9500 . ? C19 C203 1.377(6) . ? C19 C15 1.383(5) . ? C18 H18A 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C15 C13 1.388(5) . ? C15 C8 1.479(5) . ? F1 C203 1.335(6) . ? C8 B2 1.626(5) . ? C13 C201 1.381(6) . ? C6 C9 1.341(5) . ? C9 B2 1.629(6) . ? C301 H30A 0.9800 . ? C301 H30B 0.9800 . ? C301 H30C 0.9800 . ? C208 C205 1.370(6) . ? C208 C204 1.375(7) . ? C207 C206 1.388(6) . ? C206 C204 1.359(7) . ? C203 C202 1.388(7) . ? C201 C202 1.368(7) . ? F83 C89 1.343(4) . ? F82 C87 1.352(4) . ? F81 C100 1.351(4) . ? F80 C58 1.343(5) . ? F79 C76 1.340(5) . ? F78 C75 1.340(4) . ? F77 C88 1.344(4) . ? F76 C86 1.346(5) . ? F75 C79 1.347(4) . ? F74 C67 1.339(5) . ? F73 C60 1.336(5) . ? F72 C71 1.345(5) . ? F71 C66 1.343(5) . ? F70 C65 1.344(5) . ? F69 C70 1.343(5) . ? F68 C72 1.345(4) . ? F67 C61 1.343(5) . ? F66 C64 1.340(4) . ? F65 C54 1.340(5) . ? F64 C68 1.332(5) . ? F63 C74 1.333(5) . ? F62 C56 1.338(5) . ? F61 C62 1.343(5) . ? C90 C58 1.381(5) . ? C90 C89 1.385(5) . ? C90 C3 1.488(5) . ? N1 C63 1.350(5) . ? N1 C73 1.355(5) . ? N1 B1 1.604(5) . ? C100 C88 1.375(5) . ? C100 C30 1.391(5) . ? C89 C67 1.381(5) . ? C88 C72 1.370(6) . ? C87 C86 1.376(5) . ? C87 C30 1.387(5) . ? C86 C72 1.375(6) . ? C4 C5 1.347(5) . ? C4 C3 1.480(5) . ? C4 C83 1.488(5) . ? C2 C3 1.352(5) . ? C2 C80 1.471(5) . ? C2 B1 1.624(6) . ? C83 C61 1.376(6) . ? C83 C79 1.378(5) . ? C82 C73 1.362(5) . ? C82 C69 1.409(6) . ? C82 H82A 0.9500 . ? C81 C71 1.384(6) . ? C81 C66 1.398(5) . ? C81 C5 1.482(5) . ? F60 C55 1.334(5) . ? C80 C76 1.396(5) . ? C80 C75 1.401(5) . ? C79 C64 1.367(5) . ? C30 B1 1.634(5) . ? C76 C60 1.380(6) . ? C75 C70 1.372(5) . ? C74 C71 1.376(6) . ? C74 C62 1.378(6) . ? C73 H73A 0.9500 . ? C70 C68 1.372(6) . ? C69 N2 1.341(5) . ? C69 C51 1.415(6) . ? C68 C60 1.379(6) . ? N2 C57 1.459(7) . ? N2 C52 1.462(6) . ? F51 C53 1.339(5) . ? C67 C56 1.376(6) . ? C66 C54 1.376(6) . ? C65 C56 1.367(6) . ? C65 C58 1.381(6) . ? C64 C53 1.373(7) . ? C63 C51 1.369(6) . ? C63 H63A 0.9500 . ? C62 C54 1.381(7) . ? C61 C55 1.392(6) . ? C5 B1 1.643(6) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C55 C53 1.372(7) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C51 H51A 0.9500 . ? Cl1 C101 1.780(9) . ? Cl1 C101 2.03(2) 2_666 ? C101 Cl1 2.03(2) 2_666 ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 N3 C29 116.7(3) . . ? C20 N3 B2 121.9(3) . . ? C29 N3 B2 118.7(3) . . ? C50 N4 C301 120.5(3) . . ? C50 N4 C16 120.0(3) . . ? C301 N4 C16 119.5(3) . . ? C8 C7 C39 124.9(3) . . ? C8 C7 C6 111.6(3) . . ? C39 C7 C6 123.4(3) . . ? C31 C39 C33 116.0(3) . . ? C31 C39 C7 123.2(3) . . ? C33 C39 C7 120.7(3) . . ? F17 C38 C28 115.6(3) . . ? F17 C38 C26 120.5(3) . . ? C28 C38 C26 123.9(3) . . ? C36 C37 C34 115.9(3) . . ? C36 C37 C6 122.3(3) . . ? C34 C37 C6 121.4(3) . . ? F23 C36 C17 118.3(3) . . ? F23 C36 C37 118.9(3) . . ? C17 C36 C37 122.8(3) . . ? F13 C35 C34 121.0(3) . . ? F13 C35 C150 119.7(4) . . ? C34 C35 C150 119.4(3) . . ? N4 C50 C18 122.2(3) . . ? N4 C50 C27 122.4(4) . . ? C18 C50 C27 115.3(3) . . ? F18 C34 C35 117.5(3) . . ? F18 C34 C37 119.9(3) . . ? C35 C34 C37 122.6(3) . . ? F20 C33 C32 117.3(3) . . ? F20 C33 C39 120.2(3) . . ? C32 C33 C39 122.4(4) . . ? F16 C32 C33 120.9(4) . . ? F16 C32 C11 119.3(4) . . ? C33 C32 C11 119.8(4) . . ? F22 C31 C21 118.4(3) . . ? F22 C31 C39 119.0(3) . . ? C21 C31 C39 122.6(4) . . ? F6 C150 C35 120.9(4) . . ? F6 C150 C17 119.5(4) . . ? C35 C150 C17 119.6(4) . . ? C18 C29 N3 122.8(3) . . ? C18 C29 H29A 118.6 . . ? N3 C29 H29A 118.6 . . ? F14 C28 C24 119.4(3) . . ? F14 C28 C38 120.9(3) . . ? C24 C28 C38 119.7(4) . . ? C20 C27 C50 120.6(4) . . ? C20 C27 H27A 119.7 . . ? C50 C27 H27A 119.7 . . ? C38 C26 C22 113.9(3) . . ? C38 C26 B2 125.6(3) . . ? C22 C26 B2 120.1(3) . . ? F10 C25 C22 121.1(4) . . ? F10 C25 C24 119.2(3) . . ? C22 C25 C24 119.6(3) . . ? F8 C24 C28 120.7(4) . . ? F8 C24 C25 120.2(3) . . ? C28 C24 C25 119.1(3) . . ? C207 C23 C205 115.1(4) . . ? C207 C23 C9 122.8(3) . . ? C205 C23 C9 121.9(3) . . ? F24 C22 C25 116.3(3) . . ? F24 C22 C26 120.2(3) . . ? C25 C22 C26 123.6(4) . . ? F21 C21 C31 120.7(4) . . ? F21 C21 C11 119.9(4) . . ? C31 C21 C11 119.4(4) . . ? C27 C20 N3 123.6(3) . . ? C27 C20 H20A 118.2 . . ? N3 C20 H20A 118.2 . . ? F5 C19 C203 117.1(4) . . ? F5 C19 C15 119.5(4) . . ? C203 C19 C15 123.4(4) . . ? C29 C18 C50 121.0(3) . . ? C29 C18 H18A 119.5 . . ? C50 C18 H18A 119.5 . . ? F11 C17 C36 120.6(3) . . ? F11 C17 C150 119.7(4) . . ? C36 C17 C150 119.7(3) . . ? N4 C16 H16A 109.5 . . ? N4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C15 C13 115.4(4) . . ? C19 C15 C8 122.9(3) . . ? C13 C15 C8 121.6(3) . . ? C7 C8 C15 123.4(3) . . ? C7 C8 B2 109.0(3) . . ? C15 C8 B2 126.2(3) . . ? F9 C13 C201 117.7(4) . . ? F9 C13 C15 119.3(4) . . ? C201 C13 C15 123.0(4) . . ? C9 C6 C37 124.8(3) . . ? C9 C6 C7 110.8(3) . . ? C37 C6 C7 124.2(3) . . ? F12 C11 C32 119.9(4) . . ? F12 C11 C21 120.3(4) . . ? C32 C11 C21 119.8(4) . . ? C6 C9 C23 123.4(3) . . ? C6 C9 B2 109.5(3) . . ? C23 C9 B2 124.5(3) . . ? N4 C301 H30A 109.5 . . ? N4 C301 H30B 109.5 . . ? H30A C301 H30B 109.5 . . ? N4 C301 H30C 109.5 . . ? H30A C301 H30C 109.5 . . ? H30B C301 H30C 109.5 . . ? F7 C208 C205 120.6(4) . . ? F7 C208 C204 120.0(4) . . ? C205 C208 C204 119.4(4) . . ? F15 C207 C23 119.3(3) . . ? F15 C207 C206 117.6(4) . . ? C23 C207 C206 123.0(4) . . ? F4 C206 C204 120.7(4) . . ? F4 C206 C207 120.1(4) . . ? C204 C206 C207 119.2(4) . . ? F19 C205 C208 117.4(4) . . ? F19 C205 C23 119.7(4) . . ? C208 C205 C23 122.8(4) . . ? F91 C204 C206 119.5(4) . . ? F91 C204 C208 120.2(4) . . ? C206 C204 C208 120.4(4) . . ? F1 C203 C19 120.7(5) . . ? F1 C203 C202 120.3(4) . . ? C19 C203 C202 118.9(4) . . ? N3 B2 C8 113.8(3) . . ? N3 B2 C9 101.8(3) . . ? C8 B2 C9 98.7(3) . . ? N3 B2 C26 114.0(3) . . ? C8 B2 C26 108.7(3) . . ? C9 B2 C26 119.0(3) . . ? F3 C201 C202 120.2(4) . . ? F3 C201 C13 120.3(4) . . ? C202 C201 C13 119.5(4) . . ? F2 C202 C201 120.6(5) . . ? F2 C202 C203 119.6(5) . . ? C201 C202 C203 119.8(4) . . ? C58 C90 C89 116.2(3) . . ? C58 C90 C3 123.3(3) . . ? C89 C90 C3 120.4(3) . . ? C63 N1 C73 117.1(3) . . ? C63 N1 B1 122.4(3) . . ? C73 N1 B1 120.0(3) . . ? F81 C100 C88 115.1(3) . . ? F81 C100 C30 121.0(3) . . ? C88 C100 C30 123.9(4) . . ? F83 C89 C67 117.2(4) . . ? F83 C89 C90 120.2(3) . . ? C67 C89 C90 122.6(4) . . ? F77 C88 C72 119.3(3) . . ? F77 C88 C100 120.6(4) . . ? C72 C88 C100 120.1(4) . . ? F82 C87 C86 116.5(3) . . ? F82 C87 C30 118.8(3) . . ? C86 C87 C30 124.6(4) . . ? F76 C86 C72 119.5(3) . . ? F76 C86 C87 121.2(4) . . ? C72 C86 C87 119.3(4) . . ? C5 C4 C3 111.8(3) . . ? C5 C4 C83 125.1(3) . . ? C3 C4 C83 123.0(3) . . ? C3 C2 C80 124.0(3) . . ? C3 C2 B1 108.9(3) . . ? C80 C2 B1 125.5(3) . . ? C61 C83 C79 115.5(3) . . ? C61 C83 C4 122.3(3) . . ? C79 C83 C4 122.2(3) . . ? C73 C82 C69 120.4(4) . . ? C73 C82 H82A 119.8 . . ? C69 C82 H82A 119.8 . . ? C71 C81 C66 115.2(4) . . ? C71 C81 C5 122.7(3) . . ? C66 C81 C5 122.1(3) . . ? C76 C80 C75 114.6(3) . . ? C76 C80 C2 123.2(3) . . ? C75 C80 C2 121.7(3) . . ? F75 C79 C64 117.9(3) . . ? F75 C79 C83 118.6(3) . . ? C64 C79 C83 123.5(4) . . ? C87 C30 C100 113.2(3) . . ? C87 C30 B1 119.9(3) . . ? C100 C30 B1 126.1(3) . . ? C2 C3 C4 111.4(3) . . ? C2 C3 C90 124.3(3) . . ? C4 C3 C90 124.3(3) . . ? F79 C76 C60 117.6(3) . . ? F79 C76 C80 119.0(3) . . ? C60 C76 C80 123.4(4) . . ? F78 C75 C70 117.2(3) . . ? F78 C75 C80 119.7(3) . . ? C70 C75 C80 123.0(4) . . ? F63 C74 C71 121.1(4) . . ? F63 C74 C62 119.5(4) . . ? C71 C74 C62 119.4(4) . . ? N1 C73 C82 123.4(4) . . ? N1 C73 H73A 118.3 . . ? C82 C73 H73A 118.3 . . ? F68 C72 C88 120.4(4) . . ? F68 C72 C86 120.8(4) . . ? C88 C72 C86 118.8(3) . . ? F72 C71 C74 117.2(4) . . ? F72 C71 C81 119.3(4) . . ? C74 C71 C81 123.5(4) . . ? F69 C70 C75 120.7(4) . . ? F69 C70 C68 119.0(4) . . ? C75 C70 C68 120.2(4) . . ? N2 C69 C82 122.6(4) . . ? N2 C69 C51 121.8(4) . . ? C82 C69 C51 115.6(3) . . ? F64 C68 C70 120.1(4) . . ? F64 C68 C60 120.5(4) . . ? C70 C68 C60 119.5(4) . . ? C69 N2 C57 120.9(4) . . ? C69 N2 C52 120.5(4) . . ? C57 N2 C52 118.5(4) . . ? F74 C67 C56 120.0(4) . . ? F74 C67 C89 120.9(4) . . ? C56 C67 C89 119.2(4) . . ? F71 C66 C54 117.7(4) . . ? F71 C66 C81 119.6(4) . . ? C54 C66 C81 122.7(4) . . ? F70 C65 C56 119.8(4) . . ? F70 C65 C58 120.4(4) . . ? C56 C65 C58 119.8(4) . . ? F66 C64 C79 120.9(4) . . ? F66 C64 C53 119.5(4) . . ? C79 C64 C53 119.6(4) . . ? N1 C63 C51 122.9(4) . . ? N1 C63 H63A 118.5 . . ? C51 C63 H63A 118.5 . . ? F61 C62 C74 120.3(4) . . ? F61 C62 C54 120.2(4) . . ? C74 C62 C54 119.5(4) . . ? F67 C61 C83 120.2(3) . . ? F67 C61 C55 116.9(4) . . ? C83 C61 C55 122.9(4) . . ? F73 C60 C68 120.3(4) . . ? F73 C60 C76 120.4(4) . . ? C68 C60 C76 119.3(4) . . ? C4 C5 C81 121.3(3) . . ? C4 C5 B1 108.2(3) . . ? C81 C5 B1 128.6(3) . . ? N1 B1 C2 111.9(3) . . ? N1 B1 C30 112.1(3) . . ? C2 B1 C30 109.5(3) . . ? N1 B1 C5 102.0(3) . . ? C2 B1 C5 98.6(3) . . ? C30 B1 C5 122.0(3) . . ? F80 C58 C65 118.0(3) . . ? F80 C58 C90 119.7(3) . . ? C65 C58 C90 122.3(4) . . ? N2 C57 H57A 109.5 . . ? N2 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N2 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? F62 C56 C65 120.9(4) . . ? F62 C56 C67 119.2(4) . . ? C65 C56 C67 120.0(4) . . ? F60 C55 C53 120.9(4) . . ? F60 C55 C61 120.0(4) . . ? C53 C55 C61 119.1(4) . . ? F65 C54 C66 121.0(4) . . ? F65 C54 C62 119.3(4) . . ? C66 C54 C62 119.7(4) . . ? F51 C53 C55 120.3(4) . . ? F51 C53 C64 120.3(4) . . ? C55 C53 C64 119.5(4) . . ? N2 C52 H52A 109.5 . . ? N2 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N2 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C63 C51 C69 120.5(4) . . ? C63 C51 H51A 119.8 . . ? C69 C51 H51A 119.8 . . ? C101 Cl1 C101 74.2(10) . 2_666 ? Cl1 C101 Cl1 105.8(10) . 2_666 ? Cl1 C101 H10A 110.6 . . ? Cl1 C101 H10A 110.6 2_666 . ? Cl1 C101 H10B 110.6 . . ? Cl1 C101 H10B 110.6 2_666 . ? H10A C101 H10B 108.7 . . ? 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 C8 C7 C39 C31 129.5(4) . . . . ? C6 C7 C39 C31 -52.9(5) . . . . ? C8 C7 C39 C33 -51.5(5) . . . . ? C6 C7 C39 C33 126.0(4) . . . . ? C34 C37 C36 F23 178.7(3) . . . . ? C6 C37 C36 F23 5.5(5) . . . . ? C34 C37 C36 C17 0.8(6) . . . . ? C6 C37 C36 C17 -172.4(4) . . . . ? C301 N4 C50 C18 -173.7(4) . . . . ? C16 N4 C50 C18 6.4(6) . . . . ? C301 N4 C50 C27 7.2(6) . . . . ? C16 N4 C50 C27 -172.6(4) . . . . ? F13 C35 C34 F18 1.6(6) . . . . ? C150 C35 C34 F18 -178.8(4) . . . . ? F13 C35 C34 C37 -177.9(4) . . . . ? C150 C35 C34 C37 1.7(6) . . . . ? C36 C37 C34 F18 178.5(3) . . . . ? C6 C37 C34 F18 -8.2(5) . . . . ? C36 C37 C34 C35 -2.0(5) . . . . ? C6 C37 C34 C35 171.3(4) . . . . ? C31 C39 C33 F20 177.4(3) . . . . ? C7 C39 C33 F20 -1.6(5) . . . . ? C31 C39 C33 C32 -1.1(5) . . . . ? C7 C39 C33 C32 179.9(3) . . . . ? F20 C33 C32 F16 0.8(5) . . . . ? C39 C33 C32 F16 179.3(3) . . . . ? F20 C33 C32 C11 -177.1(3) . . . . ? C39 C33 C32 C11 1.4(6) . . . . ? C33 C39 C31 F22 179.2(3) . . . . ? C7 C39 C31 F22 -1.8(5) . . . . ? C33 C39 C31 C21 -0.2(5) . . . . ? C7 C39 C31 C21 178.8(3) . . . . ? F13 C35 C150 F6 -0.8(6) . . . . ? C34 C35 C150 F6 179.6(4) . . . . ? F13 C35 C150 C17 179.4(4) . . . . ? C34 C35 C150 C17 -0.3(6) . . . . ? C20 N3 C29 C18 -1.3(5) . . . . ? B2 N3 C29 C18 160.4(4) . . . . ? F17 C38 C28 F14 0.9(5) . . . . ? C26 C38 C28 F14 -179.8(3) . . . . ? F17 C38 C28 C24 -178.1(3) . . . . ? C26 C38 C28 C24 1.2(6) . . . . ? N4 C50 C27 C20 176.2(4) . . . . ? C18 C50 C27 C20 -2.9(6) . . . . ? F17 C38 C26 C22 175.0(3) . . . . ? C28 C38 C26 C22 -4.3(5) . . . . ? F17 C38 C26 B2 2.3(6) . . . . ? C28 C38 C26 B2 -177.0(4) . . . . ? F14 C28 C24 F8 1.2(6) . . . . ? C38 C28 C24 F8 -179.8(4) . . . . ? F14 C28 C24 C25 -177.4(4) . . . . ? C38 C28 C24 C25 1.6(6) . . . . ? F10 C25 C24 F8 -1.8(6) . . . . ? C22 C25 C24 F8 -179.6(4) . . . . ? F10 C25 C24 C28 176.8(4) . . . . ? C22 C25 C24 C28 -1.0(6) . . . . ? F10 C25 C22 F24 -0.7(6) . . . . ? C24 C25 C22 F24 177.1(4) . . . . ? F10 C25 C22 C26 179.7(4) . . . . ? C24 C25 C22 C26 -2.5(6) . . . . ? C38 C26 C22 F24 -174.7(3) . . . . ? B2 C26 C22 F24 -1.5(5) . . . . ? C38 C26 C22 C25 4.9(6) . . . . ? B2 C26 C22 C25 178.1(4) . . . . ? F22 C31 C21 F21 1.1(5) . . . . ? C39 C31 C21 F21 -179.5(3) . . . . ? F22 C31 C21 C11 -178.4(3) . . . . ? C39 C31 C21 C11 1.0(6) . . . . ? C50 C27 C20 N3 2.4(6) . . . . ? C29 N3 C20 C27 -0.3(6) . . . . ? B2 N3 C20 C27 -161.3(4) . . . . ? N3 C29 C18 C50 0.7(6) . . . . ? N4 C50 C18 C29 -177.7(4) . . . . ? C27 C50 C18 C29 1.4(5) . . . . ? F23 C36 C17 F11 1.8(6) . . . . ? C37 C36 C17 F11 179.7(3) . . . . ? F23 C36 C17 C150 -177.4(4) . . . . ? C37 C36 C17 C150 0.5(6) . . . . ? F6 C150 C17 F11 0.2(6) . . . . ? C35 C150 C17 F11 -179.9(4) . . . . ? F6 C150 C17 C36 179.4(4) . . . . ? C35 C150 C17 C36 -0.8(6) . . . . ? F5 C19 C15 C13 179.9(4) . . . . ? C203 C19 C15 C13 0.8(6) . . . . ? F5 C19 C15 C8 -4.4(6) . . . . ? C203 C19 C15 C8 176.6(4) . . . . ? C39 C7 C8 C15 -12.2(5) . . . . ? C6 C7 C8 C15 170.0(3) . . . . ? C39 C7 C8 B2 -179.5(3) . . . . ? C6 C7 C8 B2 2.7(4) . . . . ? C19 C15 C8 C7 124.4(4) . . . . ? C13 C15 C8 C7 -60.1(5) . . . . ? C19 C15 C8 B2 -70.5(5) . . . . ? C13 C15 C8 B2 105.0(4) . . . . ? C19 C15 C13 F9 176.8(3) . . . . ? C8 C15 C13 F9 0.9(6) . . . . ? C19 C15 C13 C201 -1.6(6) . . . . ? C8 C15 C13 C201 -177.5(4) . . . . ? C36 C37 C6 C9 119.6(4) . . . . ? C34 C37 C6 C9 -53.2(5) . . . . ? C36 C37 C6 C7 -55.9(5) . . . . ? C34 C37 C6 C7 131.3(4) . . . . ? C8 C7 C6 C9 -5.9(4) . . . . ? C39 C7 C6 C9 176.3(3) . . . . ? C8 C7 C6 C37 170.2(3) . . . . ? C39 C7 C6 C37 -7.7(5) . . . . ? F16 C32 C11 F12 1.0(6) . . . . ? C33 C32 C11 F12 179.0(3) . . . . ? F16 C32 C11 C21 -178.5(3) . . . . ? C33 C32 C11 C21 -0.6(6) . . . . ? F21 C21 C11 F12 0.3(6) . . . . ? C31 C21 C11 F12 179.9(3) . . . . ? F21 C21 C11 C32 179.8(3) . . . . ? C31 C21 C11 C32 -0.6(6) . . . . ? C37 C6 C9 C23 -7.3(5) . . . . ? C7 C6 C9 C23 168.7(3) . . . . ? C37 C6 C9 B2 -169.8(3) . . . . ? C7 C6 C9 B2 6.2(4) . . . . ? C207 C23 C9 C6 128.3(4) . . . . ? C205 C23 C9 C6 -57.5(5) . . . . ? C207 C23 C9 B2 -71.7(5) . . . . ? C205 C23 C9 B2 102.4(4) . . . . ? C205 C23 C207 F15 179.9(3) . . . . ? C9 C23 C207 F15 -5.6(6) . . . . ? C205 C23 C207 C206 0.7(6) . . . . ? C9 C23 C207 C206 175.3(4) . . . . ? F15 C207 C206 F4 -1.0(6) . . . . ? C23 C207 C206 F4 178.2(4) . . . . ? F15 C207 C206 C204 179.5(4) . . . . ? C23 C207 C206 C204 -1.4(7) . . . . ? F7 C208 C205 F19 1.3(6) . . . . ? C204 C208 C205 F19 -178.6(4) . . . . ? F7 C208 C205 C23 179.2(4) . . . . ? C204 C208 C205 C23 -0.7(7) . . . . ? C207 C23 C205 F19 178.1(3) . . . . ? C9 C23 C205 F19 3.5(6) . . . . ? C207 C23 C205 C208 0.3(6) . . . . ? C9 C23 C205 C208 -174.3(4) . . . . ? F4 C206 C204 F91 2.7(7) . . . . ? C207 C206 C204 F91 -177.8(4) . . . . ? F4 C206 C204 C208 -178.6(4) . . . . ? C207 C206 C204 C208 1.0(7) . . . . ? F7 C208 C204 F91 -1.1(7) . . . . ? C205 C208 C204 F91 178.7(4) . . . . ? F7 C208 C204 C206 -179.8(4) . . . . ? C205 C208 C204 C206 0.0(7) . . . . ? F5 C19 C203 F1 1.2(7) . . . . ? C15 C19 C203 F1 -179.7(4) . . . . ? F5 C19 C203 C202 -179.0(4) . . . . ? C15 C19 C203 C202 0.1(7) . . . . ? C20 N3 B2 C8 -167.4(3) . . . . ? C29 N3 B2 C8 32.0(5) . . . . ? C20 N3 B2 C9 87.5(4) . . . . ? C29 N3 B2 C9 -73.2(4) . . . . ? C20 N3 B2 C26 -41.9(5) . . . . ? C29 N3 B2 C26 157.4(3) . . . . ? C7 C8 B2 N3 -106.3(3) . . . . ? C15 C8 B2 N3 86.9(4) . . . . ? C7 C8 B2 C9 0.8(3) . . . . ? C15 C8 B2 C9 -166.1(3) . . . . ? C7 C8 B2 C26 125.5(3) . . . . ? C15 C8 B2 C26 -41.4(5) . . . . ? C6 C9 B2 N3 112.4(3) . . . . ? C23 C9 B2 N3 -49.9(4) . . . . ? C6 C9 B2 C8 -4.3(3) . . . . ? C23 C9 B2 C8 -166.6(3) . . . . ? C6 C9 B2 C26 -121.5(3) . . . . ? C23 C9 B2 C26 76.2(4) . . . . ? C38 C26 B2 N3 -31.3(5) . . . . ? C22 C26 B2 N3 156.4(3) . . . . ? C38 C26 B2 C8 96.8(4) . . . . ? C22 C26 B2 C8 -75.5(4) . . . . ? C38 C26 B2 C9 -151.4(4) . . . . ? C22 C26 B2 C9 36.3(5) . . . . ? F9 C13 C201 F3 1.3(6) . . . . ? C15 C13 C201 F3 179.7(4) . . . . ? F9 C13 C201 C202 -176.9(4) . . . . ? C15 C13 C201 C202 1.6(7) . . . . ? F3 C201 C202 F2 1.6(8) . . . . ? C13 C201 C202 F2 179.8(5) . . . . ? F3 C201 C202 C203 -178.8(5) . . . . ? C13 C201 C202 C203 -0.6(8) . . . . ? F1 C203 C202 F2 -0.7(8) . . . . ? C19 C203 C202 F2 179.5(5) . . . . ? F1 C203 C202 C201 179.6(5) . . . . ? C19 C203 C202 C201 -0.2(8) . . . . ? C58 C90 C89 F83 178.2(3) . . . . ? C3 C90 C89 F83 -2.7(5) . . . . ? C58 C90 C89 C67 -0.9(5) . . . . ? C3 C90 C89 C67 178.1(3) . . . . ? F81 C100 C88 F77 1.1(5) . . . . ? C30 C100 C88 F77 -178.8(3) . . . . ? F81 C100 C88 C72 -178.0(3) . . . . ? C30 C100 C88 C72 2.1(6) . . . . ? F82 C87 C86 F76 -1.8(6) . . . . ? C30 C87 C86 F76 -179.4(4) . . . . ? F82 C87 C86 C72 176.5(4) . . . . ? C30 C87 C86 C72 -1.1(6) . . . . ? C5 C4 C83 C61 -57.8(5) . . . . ? C3 C4 C83 C61 124.8(4) . . . . ? C5 C4 C83 C79 118.0(4) . . . . ? C3 C4 C83 C79 -59.4(5) . . . . ? C3 C2 C80 C76 143.5(4) . . . . ? B1 C2 C80 C76 -52.4(5) . . . . ? C3 C2 C80 C75 -44.8(5) . . . . ? B1 C2 C80 C75 119.4(4) . . . . ? C61 C83 C79 F75 179.9(4) . . . . ? C4 C83 C79 F75 3.9(5) . . . . ? C61 C83 C79 C64 1.1(6) . . . . ? C4 C83 C79 C64 -174.9(4) . . . . ? F82 C87 C30 C100 -174.6(3) . . . . ? C86 C87 C30 C100 3.0(6) . . . . ? F82 C87 C30 B1 -4.9(6) . . . . ? C86 C87 C30 B1 172.7(4) . . . . ? F81 C100 C30 C87 176.7(3) . . . . ? C88 C100 C30 C87 -3.5(6) . . . . ? F81 C100 C30 B1 7.7(6) . . . . ? C88 C100 C30 B1 -172.4(4) . . . . ? C80 C2 C3 C4 162.4(3) . . . . ? B1 C2 C3 C4 -4.0(4) . . . . ? C80 C2 C3 C90 -19.8(5) . . . . ? B1 C2 C3 C90 173.8(3) . . . . ? C5 C4 C3 C2 -3.4(4) . . . . ? C83 C4 C3 C2 174.4(3) . . . . ? C5 C4 C3 C90 178.9(3) . . . . ? C83 C4 C3 C90 -3.4(5) . . . . ? C58 C90 C3 C2 126.2(4) . . . . ? C89 C90 C3 C2 -52.8(5) . . . . ? C58 C90 C3 C4 -56.3(5) . . . . ? C89 C90 C3 C4 124.7(4) . . . . ? C75 C80 C76 F79 179.8(3) . . . . ? C2 C80 C76 F79 -7.9(5) . . . . ? C75 C80 C76 C60 -1.1(5) . . . . ? C2 C80 C76 C60 171.2(3) . . . . ? C76 C80 C75 F78 175.0(3) . . . . ? C2 C80 C75 F78 2.5(5) . . . . ? C76 C80 C75 C70 -0.7(5) . . . . ? C2 C80 C75 C70 -173.2(4) . . . . ? C63 N1 C73 C82 -3.2(6) . . . . ? B1 N1 C73 C82 -174.9(4) . . . . ? C69 C82 C73 N1 1.7(6) . . . . ? F77 C88 C72 F68 0.6(6) . . . . ? C100 C88 C72 F68 179.7(4) . . . . ? F77 C88 C72 C86 -179.0(4) . . . . ? C100 C88 C72 C86 0.1(6) . . . . ? F76 C86 C72 F68 -1.8(6) . . . . ? C87 C86 C72 F68 179.9(4) . . . . ? F76 C86 C72 C88 177.8(4) . . . . ? C87 C86 C72 C88 -0.5(6) . . . . ? F63 C74 C71 F72 -0.6(6) . . . . ? C62 C74 C71 F72 -178.5(4) . . . . ? F63 C74 C71 C81 177.3(4) . . . . ? C62 C74 C71 C81 -0.6(7) . . . . ? C66 C81 C71 F72 -179.1(4) . . . . ? C5 C81 C71 F72 3.0(6) . . . . ? C66 C81 C71 C74 3.1(6) . . . . ? C5 C81 C71 C74 -174.9(4) . . . . ? F78 C75 C70 F69 4.4(6) . . . . ? C80 C75 C70 F69 -179.8(4) . . . . ? F78 C75 C70 C68 -173.9(4) . . . . ? C80 C75 C70 C68 1.9(6) . . . . ? C73 C82 C69 N2 -179.5(4) . . . . ? C73 C82 C69 C51 0.3(6) . . . . ? F69 C70 C68 F64 -0.2(6) . . . . ? C75 C70 C68 F64 178.1(4) . . . . ? F69 C70 C68 C60 -179.5(4) . . . . ? C75 C70 C68 C60 -1.2(6) . . . . ? C82 C69 N2 C57 179.7(5) . . . . ? C51 C69 N2 C57 -0.1(7) . . . . ? C82 C69 N2 C52 3.0(6) . . . . ? C51 C69 N2 C52 -176.7(4) . . . . ? F83 C89 C67 F74 -0.1(5) . . . . ? C90 C89 C67 F74 179.0(3) . . . . ? F83 C89 C67 C56 -178.4(3) . . . . ? C90 C89 C67 C56 0.8(6) . . . . ? C71 C81 C66 F71 178.4(4) . . . . ? C5 C81 C66 F71 -3.7(6) . . . . ? C71 C81 C66 C54 -3.7(6) . . . . ? C5 C81 C66 C54 174.3(4) . . . . ? F75 C79 C64 F66 1.2(6) . . . . ? C83 C79 C64 F66 -179.9(4) . . . . ? F75 C79 C64 C53 -179.2(4) . . . . ? C83 C79 C64 C53 -0.3(7) . . . . ? C73 N1 C63 C51 2.8(6) . . . . ? B1 N1 C63 C51 174.3(4) . . . . ? F63 C74 C62 F61 0.8(7) . . . . ? C71 C74 C62 F61 178.8(4) . . . . ? F63 C74 C62 C54 -179.3(4) . . . . ? C71 C74 C62 C54 -1.4(7) . . . . ? C79 C83 C61 F67 178.1(4) . . . . ? C4 C83 C61 F67 -5.8(6) . . . . ? C79 C83 C61 C55 -0.9(7) . . . . ? C4 C83 C61 C55 175.1(4) . . . . ? F64 C68 C60 F73 -0.8(6) . . . . ? C70 C68 C60 F73 178.5(4) . . . . ? F64 C68 C60 C76 -179.9(4) . . . . ? C70 C68 C60 C76 -0.6(6) . . . . ? F79 C76 C60 F73 1.7(5) . . . . ? C80 C76 C60 F73 -177.3(3) . . . . ? F79 C76 C60 C68 -179.2(3) . . . . ? C80 C76 C60 C68 1.8(6) . . . . ? C3 C4 C5 C81 174.3(3) . . . . ? C83 C4 C5 C81 -3.3(6) . . . . ? C3 C4 C5 B1 9.0(4) . . . . ? C83 C4 C5 B1 -168.7(3) . . . . ? C71 C81 C5 C4 118.3(4) . . . . ? C66 C81 C5 C4 -59.5(5) . . . . ? C71 C81 C5 B1 -79.5(5) . . . . ? C66 C81 C5 B1 102.7(5) . . . . ? C63 N1 B1 C2 13.0(5) . . . . ? C73 N1 B1 C2 -175.7(3) . . . . ? C63 N1 B1 C30 136.5(4) . . . . ? C73 N1 B1 C30 -52.3(5) . . . . ? C63 N1 B1 C5 -91.4(4) . . . . ? C73 N1 B1 C5 79.8(4) . . . . ? C3 C2 B1 N1 -98.4(4) . . . . ? C80 C2 B1 N1 95.5(4) . . . . ? C3 C2 B1 C30 136.7(3) . . . . ? C80 C2 B1 C30 -29.4(5) . . . . ? C3 C2 B1 C5 8.3(4) . . . . ? C80 C2 B1 C5 -157.8(3) . . . . ? C87 C30 B1 N1 168.6(3) . . . . ? C100 C30 B1 N1 -23.1(5) . . . . ? C87 C30 B1 C2 -66.6(5) . . . . ? C100 C30 B1 C2 101.7(4) . . . . ? C87 C30 B1 C5 47.4(5) . . . . ? C100 C30 B1 C5 -144.3(4) . . . . ? C4 C5 B1 N1 104.5(3) . . . . ? C81 C5 B1 N1 -59.5(4) . . . . ? C4 C5 B1 C2 -10.2(4) . . . . ? C81 C5 B1 C2 -174.2(3) . . . . ? C4 C5 B1 C30 -129.7(4) . . . . ? C81 C5 B1 C30 66.4(5) . . . . ? F70 C65 C58 F80 1.0(5) . . . . ? C56 C65 C58 F80 -178.4(3) . . . . ? F70 C65 C58 C90 179.6(3) . . . . ? C56 C65 C58 C90 0.2(6) . . . . ? C89 C90 C58 F80 179.1(3) . . . . ? C3 C90 C58 F80 0.0(5) . . . . ? C89 C90 C58 C65 0.4(5) . . . . ? C3 C90 C58 C65 -178.6(3) . . . . ? F70 C65 C56 F62 0.7(6) . . . . ? C58 C65 C56 F62 -179.9(3) . . . . ? F70 C65 C56 C67 -179.8(3) . . . . ? C58 C65 C56 C67 -0.4(6) . . . . ? F74 C67 C56 F62 1.2(6) . . . . ? C89 C67 C56 F62 179.4(4) . . . . ? F74 C67 C56 C65 -178.3(4) . . . . ? C89 C67 C56 C65 -0.1(6) . . . . ? F67 C61 C55 F60 1.7(8) . . . . ? C83 C61 C55 F60 -179.2(5) . . . . ? F67 C61 C55 C53 -179.1(5) . . . . ? C83 C61 C55 C53 -0.1(8) . . . . ? F71 C66 C54 F65 -0.9(6) . . . . ? C81 C66 C54 F65 -178.8(4) . . . . ? F71 C66 C54 C62 179.9(4) . . . . ? C81 C66 C54 C62 1.9(7) . . . . ? F61 C62 C54 F65 1.4(7) . . . . ? C74 C62 C54 F65 -178.5(4) . . . . ? F61 C62 C54 C66 -179.4(4) . . . . ? C74 C62 C54 C66 0.7(7) . . . . ? F60 C55 C53 F51 -1.1(8) . . . . ? C61 C55 C53 F51 179.8(5) . . . . ? F60 C55 C53 C64 -180.0(5) . . . . ? C61 C55 C53 C64 0.9(8) . . . . ? F66 C64 C53 F51 0.0(7) . . . . ? C79 C64 C53 F51 -179.6(4) . . . . ? F66 C64 C53 C55 178.9(5) . . . . ? C79 C64 C53 C55 -0.7(7) . . . . ? N1 C63 C51 C69 -1.0(7) . . . . ? N2 C69 C51 C63 179.2(4) . . . . ? C82 C69 C51 C63 -0.6(6) . . . . ? C101 Cl1 C101 Cl1 0.000(2) 2_666 . . 2_666 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.786 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.077