Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. #============================================================================== # 0. AUDIT DETAILS _audit_creation_date '2001-03-06 15:24:09' _audit_creation_method ; PLATON option SHELXL97-2 & Manual Editing ; _audit_update_record ; 2003_06-30 Impact of setting C44 to isotropic displacement parameter ; _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Jan C. Hummelen' _publ_contact_author_address ; Molecular Electronics, MSC Groningen University Nijenborgh 4 Groningen 9747 AG NETHERLANDS ; _publ_contact_author_email J.C.HUMMELEN@CHEM.RUG.NL _publ_contact_letter # Include date of submission ; Date of submission : 2003-05-25 Consider this CIF submission for deposition of the second X-ray structure of the manuscript entitled: Influence of the solvent on the crystal structure of PCBM and the efficiency of MDMO-PPV:PCBM 'plastic' solar cells (Our Compound_Identification_Code: CP578B) ; _publ_section_title ; Influence of the solvent on the crystal structure of PCBM and the efficiency of MDMO-PPV:PCBM 'plastic' solar cells ; loop_ _publ_author_name _publ_author_address M.T.Rispens ; Molecular Electronics, MSC+, University of Groningen, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; A.Meetsma ; Molecular Electronics, MSC+, Groningen University, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; R.Rittberger ; Linz Institute for Organic Solar Cells (LIOS), Physical Chemistry, Johannes Keppler University of Linz, Altenbergerstr. 69 A-4040 Linz, Austria. ; C.J.Brabec ; Siemens AG, CT MM1, Innovative Electronics, Paul-Gossen-Str 100, D-91052 Erlangen, Germany. ; N.S.Sariciftci ; Linz Institute for Organic Solar Cells (LIOS), Physical Chemistry, Johannes Keppler University of Linz, Altenbergerstr. 69 A-4040 Linz, Austria. ; ; J.C.Hummelen ; ; Molecular Electronics, MSC+, University of Groningen, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; #=============================================================================== _publ_section_exptl_refinement ; Refinement was complicated (frustrated) by a disorder problem: from the solution it was clear that the chlorobenzene solvent molecules were (highly) disordered over an inversion centre (residue 3 on (0.0,.0.5,0.0) and residue 4 on (0.0,0.5,0.5)). The electron density of the chloride and the carbon atoms appeared to be spread out, indicating translation disorder. A disorder model (50:50) with bond restraints ("variable metric rigid hexagon") was used in the refinement. The C44 position converged to non-positive definite displacement parameters when allowed to vary anisotropically, so ultimately this was returned to an isotropic displacement parameter. A subsequent difference Fourier synthesis resulted in the location of all the hydrogen atoms which co-ordinates and isotropic displacement parameters were refined, except those belonging to disordered C atoms of the chlorobenzene solvent molecules, which were constrained to idealised geometries and allowed to ride on their carrier atoms with an isotropic displacement parameter related to the equivalent displacement parameter of their carrier atoms. ; # Insert blank lines between references _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C. Guagliardi, A., Moliterni, A.G.G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. Bondi, A. (1964). J. Phys. Chem. 68, 441-451. Bruker, (2000). SMART, SAINT, SADABS, XPREP and SHELXTL/NT. Software Reference Manual Bruker AXS Inc. Madison, Wisconsin, USA. International Tables for Crystallography (1983). Vol. A. Space-group symmetry, edited by T. Hahn. Dordrecht: Reidel. (Present distributor Kluwer Academic Publishers, Dordrecht). International Tables for Crystallography (1992). Vol. C. Edited by A.J.C Wilson, Kluwer Academic Publishers, Dordrecht, The Netherlands. Le Page, Y. (1987). J. Appl. Cryst. 20, 264-269. Le Page, Y. (1988). J. Appl. Cryst. 21, 983-984. Meetsma, A. (2000). Extended version of the program PLUTO. Groningen University, The Netherlands. (unpublished). Sheldrick, G.M. SHELXL97. Program for Crystal Structure Refinement. University of Gottingen, Germany, 1997. Sheldrick, G.M. SADABS. Version 2. Multi-Scan Absorption Correction Program. University of Gottingen, Germany, 2001 Spek, A.L. (1988). J. Appl. Cryst. 21, 578-579. Spek, A.L. (1990). Acta Cryst. A46, C-34. Spek, A.L. (1994). Am. Crystallogr. Assoc.-Abstracts, 22, 66. ; _publ_section_figure_captions ; Fig. 1. Chemical structural diagram (scheme 1) of the title compound Fig. 2. Perspective PLUTO drawing of the molecule illustrating the configuration and the adopted numbering scheme. Fig. 3. Molecular packing viewed down unit cell axes. Fig. 4. Perspective ORTEP drawing of the title compound. Displacement ellipsoids for non-H are represented at the 50% probability level. The H-atoms are drawn with an arbitrary radius. ; #=============================================================================== data_c78h18cl _database_code_CSD 211976 _audit_creation_date '2001-01-03 16:10:48' _audit_creation_method 'PLATON
option' _audit_update_record ; ? ; #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; Methyl 5-(3'H-cyclopropa[1,9](C60-Ih)[5,6]fullerenyl)-5-phenylpentanoate. ; _chemical_name_common 'Phenyl-C61-Butyric acid Methyl ester (PCBM)' _chemical_melting_point ? _chemical_formula_moiety 'C72 H14 O2, C6 H4 Cl2' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C78 H18 Cl2 O2' _chemical_formula_weight 1057.91 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 13.7565(9) _cell_length_b 16.634(1) _cell_length_c 19.077(1) _cell_angle_alpha 90 _cell_angle_beta 105.289(1) _cell_angle_gamma 90 _cell_volume 4210.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 90 _cell_measurement_reflns_used 3065 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 25.20 _cell_special_details ; The final unit cell was obtained from the xyz centroids of 3065 reflections after integration using the SAINT software package (Bruker, 2000). The intensity data were corrected for decay and absorption using SADABS (Sheldrick, 2000). ; _exptl_crystal_description ' platelet' _exptl_crystal_colour ' red-brown' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.020 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 0.221 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_process_details '(SADABS (Sheldrick, Bruker, 2000))' _exptl_absorpt_correction_T_min 0.9280 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(r12) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine focus sealed Siemens Mo tube ' _diffrn_radiation_monochromator 'parallel mounted graphite' _diffrn_radiation_detector ; CCD area-detector ; _diffrn_measurement_device_type ; Bruker Smart Apex ; _diffrn_measurement_method 'phi and omega scans' _diffrn_special_details ; Crystal into the cold nitrogen stream of the low-temparature unit (KROFLEX, (Bruker, 2000)). ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 25918 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.1710 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 27.53 _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.962 _diffrn_reflns_reduction_process ; Intensity data were corrected for Lorentz and polarization effects, decay and absorption and reduced to F~o~^2^ using SAINT (Bruker, 2000) and SABABS (Sheldrick, 2000) ; # number of unique reflections _reflns_number_total 9661 _reflns_number_gt 4425 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker Version 5.168, 2000' _computing_cell_refinement 'SAINT, Bruker Version 6.02A, 2000' _computing_data_reduction 'XPREP, Bruker Version 5.1/NT, 2000' _computing_structure_solution ; SIR-97 (Altomare et al., 1997) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLUTO (Meetsma, 2000) PLATON (Spek, 1994, 1996) ; _computing_publication_material ; PLATON (Spek, 1990) SHELXL (Sheldrick, 1997) ; #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_details calc _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0147P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 9661 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.1084 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 0.687 _refine_ls_restrained_S_all 0.687 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.375 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.054 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv O1 O Uani 0.30167(12) 0.25012(11) 0.16769(9) 1.000 0.0307(7) O2 O Uani 0.46681(12) 0.27914(10) 0.19456(8) 1.000 0.0218(6) C1 C Uani 0.21552(17) 0.18439(15) 0.39206(12) 1.000 0.0156(8) C2 C Uani 0.16516(17) 0.12651(15) 0.32347(12) 1.000 0.0147(8) C3 C Uani 0.08339(17) 0.07276(14) 0.33397(13) 1.000 0.0152(8) C4 C Uani 0.05938(17) 0.06441(14) 0.39948(13) 1.000 0.0167(8) C5 C Uani 0.10516(18) 0.11667(16) 0.46158(13) 1.000 0.0193(9) C6 C Uani 0.17293(17) 0.17526(16) 0.45591(12) 1.000 0.0167(9) C7 C Uani 0.16444(17) 0.25449(16) 0.48457(12) 1.000 0.0177(8) C8 C Uani 0.18729(17) 0.31365(16) 0.43548(13) 1.000 0.0183(9) C9 C Uani 0.20972(16) 0.27147(15) 0.37531(13) 1.000 0.0160(8) C10 C Uani 0.17644(17) 0.30312(15) 0.30666(13) 1.000 0.0166(9) C11 C Uani 0.12966(17) 0.25066(15) 0.24431(12) 1.000 0.0162(8) C12 C Uani 0.12026(17) 0.16925(15) 0.25396(12) 1.000 0.0149(8) C13 C Uani 0.02684(17) 0.12996(16) 0.21822(12) 1.000 0.0177(9) C14 C Uani 0.00401(17) 0.07132(15) 0.26755(13) 1.000 0.0169(8) C15 C Uani -0.09529(18) 0.05664(15) 0.26691(13) 1.000 0.0189(9) C16 C Uani -0.12048(17) 0.04569(15) 0.33530(13) 1.000 0.0180(9) C17 C Uani -0.04491(18) 0.05061(15) 0.39978(13) 1.000 0.0191(9) C18 C Uani -0.06378(18) 0.09280(16) 0.46164(13) 1.000 0.0208(9) C19 C Uani 0.02800(18) 0.13403(16) 0.49922(12) 1.000 0.0194(9) C20 C Uani 0.02316(18) 0.20932(17) 0.52948(12) 1.000 0.0203(9) C21 C Uani 0.09253(18) 0.27151(17) 0.52204(12) 1.000 0.0197(9) C22 C Uani 0.04032(18) 0.34793(16) 0.51164(13) 1.000 0.0219(9) C23 C Uani 0.06231(18) 0.40426(16) 0.46451(13) 1.000 0.0218(9) C24 C Uani 0.13779(17) 0.38746(16) 0.42581(13) 1.000 0.0204(9) C25 C Uani 0.10469(17) 0.42065(15) 0.35414(13) 1.000 0.0194(9) C26 C Uani 0.12236(17) 0.37890(15) 0.29525(13) 1.000 0.0191(9) C27 C Uani 0.04436(18) 0.37426(16) 0.22755(13) 1.000 0.0207(9) C28 C Uani 0.04926(18) 0.29563(16) 0.19668(13) 1.000 0.0190(9) C29 C Uani -0.03941(18) 0.25652(16) 0.15980(12) 1.000 0.0200(9) C30 C Uani -0.05055(18) 0.17218(16) 0.17106(12) 1.000 0.0191(9) C31 C Uani -0.15473(18) 0.15757(16) 0.17117(12) 1.000 0.0188(9) C32 C Uani -0.17652(17) 0.10075(15) 0.21822(13) 1.000 0.0192(9) C33 C Uani -0.25188(17) 0.11764(16) 0.25686(13) 1.000 0.0195(9) C34 C Uani -0.21750(18) 0.08424(15) 0.32918(14) 1.000 0.0218(9) C35 C Uani -0.23565(18) 0.12445(16) 0.38782(14) 1.000 0.0207(9) C36 C Uani -0.15693(18) 0.12941(16) 0.45572(13) 1.000 0.0205(9) C37 C Uani -0.16217(18) 0.20785(16) 0.48687(13) 1.000 0.0210(9) C38 C Uani -0.07377(18) 0.24756(17) 0.52329(12) 1.000 0.0211(9) C39 C Uani -0.06328(19) 0.33307(17) 0.51227(12) 1.000 0.0211(10) C40 C Uani -0.14123(18) 0.37545(16) 0.46556(13) 1.000 0.0214(9) C41 C Uani -0.11811(18) 0.43470(15) 0.41612(13) 1.000 0.0222(9) C42 C Uani -0.01842(18) 0.44887(15) 0.41573(13) 1.000 0.0205(9) C43 C Uani 0.00784(18) 0.45890(15) 0.34729(14) 1.000 0.0221(9) C44 C Uani -0.06671(19) 0.45434(15) 0.28233(14) 1.000 0.0229(9) C45 C Uani -0.04817(19) 0.41175(15) 0.22108(13) 1.000 0.0215(9) C46 C Uani -0.14084(18) 0.37089(16) 0.18289(13) 1.000 0.0208(9) C47 C Uani -0.13623(18) 0.29583(17) 0.15301(12) 1.000 0.0210(9) C48 C Uani -0.20703(18) 0.23371(17) 0.16039(12) 1.000 0.0207(9) C49 C Uani -0.27978(17) 0.25014(17) 0.19717(13) 1.000 0.0202(9) C50 C Uani -0.30278(17) 0.19098(16) 0.24639(13) 1.000 0.0203(9) C51 C Uani -0.32178(17) 0.23346(16) 0.30797(13) 1.000 0.0182(9) C52 C Uani -0.28847(17) 0.20073(16) 0.37709(14) 1.000 0.0201(9) C53 C Uani -0.24323(18) 0.25247(16) 0.43855(13) 1.000 0.0193(9) C54 C Uani -0.23251(18) 0.33379(16) 0.42761(13) 1.000 0.0195(9) C55 C Uani -0.26694(17) 0.36802(16) 0.35510(13) 1.000 0.0193(9) C56 C Uani -0.31056(17) 0.31869(16) 0.29690(13) 1.000 0.0193(9) C57 C Uani -0.28481(17) 0.32900(16) 0.22827(13) 1.000 0.0207(9) C58 C Uani -0.21662(17) 0.38804(16) 0.22102(13) 1.000 0.0205(9) C59 C Uani -0.17055(18) 0.43967(15) 0.28304(14) 1.000 0.0203(9) C60 C Uani -0.19594(18) 0.42983(15) 0.34839(13) 1.000 0.0202(9) C61 C Uani 0.27592(17) 0.12167(15) 0.36385(12) 1.000 0.0178(8) C62 C Uani 0.31030(17) 0.04927(15) 0.41092(13) 1.000 0.0168(8) C63 C Uani 0.35860(18) 0.05901(17) 0.48445(14) 1.000 0.0199(9) C64 C Uani 0.39384(18) -0.00750(17) 0.52827(15) 1.000 0.0226(10) C65 C Uani 0.38183(18) -0.08382(17) 0.49845(15) 1.000 0.0213(10) C66 C Uani 0.33468(18) -0.09416(17) 0.42532(15) 1.000 0.0218(9) C67 C Uani 0.29842(18) -0.02808(16) 0.38184(14) 1.000 0.0196(9) C68 C Uani 0.35108(19) 0.15337(16) 0.32371(14) 1.000 0.0176(9) C69 C Uani 0.35346(19) 0.10560(16) 0.25585(14) 1.000 0.0187(9) C70 C Uani 0.4233(2) 0.14578(16) 0.21527(15) 1.000 0.0209(9) C71 C Uani 0.38872(19) 0.22948(17) 0.19016(13) 1.000 0.0203(9) C72 C Uani 0.4415(2) 0.36232(18) 0.17376(17) 1.000 0.0260(10) Cl1 Cl Uani 0.41388(5) 0.39302(4) 0.35693(3) 1.000 0.0314(3) Cl2 Cl Uani 0.46934(5) 0.26987(4) 0.48695(3) 1.000 0.0316(3) C73 C Uani 0.51598(17) 0.41028(16) 0.43143(12) 1.000 0.0190(9) C74 C Uani 0.54048(18) 0.35682(15) 0.48876(13) 1.000 0.0207(9) C75 C Uani 0.62126(19) 0.37129(18) 0.54799(14) 1.000 0.0243(10) C76 C Uani 0.67732(19) 0.44094(19) 0.55001(15) 1.000 0.0273(10) C77 C Uani 0.6522(2) 0.49505(18) 0.49267(15) 1.000 0.0263(10) C78 C Uani 0.57226(19) 0.47956(17) 0.43304(14) 1.000 0.0221(10) H63 H Uiso 0.3669(16) 0.1161(15) 0.5047(12) 1.000 0.036(8) H64 H Uiso 0.4317(15) 0.0015(13) 0.5816(11) 1.000 0.018(7) H65 H Uiso 0.4108(15) -0.1315(14) 0.5297(11) 1.000 0.026(7) H66 H Uiso 0.3224(15) -0.1483(14) 0.4023(11) 1.000 0.018(7) H67 H Uiso 0.2609(15) -0.0417(14) 0.3289(12) 1.000 0.025(7) H68 H Uiso 0.3322(15) 0.2107(14) 0.3092(11) 1.000 0.025(7) H68' H Uiso 0.4253(15) 0.1541(13) 0.3617(10) 1.000 0.019(6) H69 H Uiso 0.2809(16) 0.1024(13) 0.2189(11) 1.000 0.025(7) H69' H Uiso 0.3771(14) 0.0485(13) 0.2708(10) 1.000 0.015(6) H70 H Uiso 0.4929(16) 0.1491(14) 0.2466(12) 1.000 0.029(7) H70' H Uiso 0.4252(16) 0.1156(15) 0.1691(12) 1.000 0.038(8) H72 H Uiso 0.3920(16) 0.3649(14) 0.1277(12) 1.000 0.026(7) H72' H Uiso 0.4102(19) 0.3879(18) 0.2143(14) 1.000 0.075(11) H72" H Uiso 0.510(2) 0.3863(17) 0.1708(13) 1.000 0.065(10) H75 H Uiso 0.6375(17) 0.3363(15) 0.5906(12) 1.000 0.039(8) H76 H Uiso 0.7309(15) 0.4524(13) 0.5937(11) 1.000 0.021(7) H77 H Uiso 0.6942(15) 0.5499(14) 0.4958(11) 1.000 0.026(7) H78 H Uiso 0.5514(16) 0.5203(14) 0.3901(12) 1.000 0.033(8) 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 O1 0.0221(11) 0.0352(13) 0.0358(11) 0.0142(10) 0.0092(9) 0.0051(9) O2 0.0226(10) 0.0169(11) 0.0252(10) 0.0018(9) 0.0049(8) -0.0012(9) C1 0.0152(14) 0.0179(16) 0.0123(13) -0.0015(12) 0.0010(11) 0.0007(12) C2 0.0170(14) 0.0122(15) 0.0150(13) -0.0017(12) 0.0046(11) 0.0006(11) C3 0.0163(14) 0.0113(15) 0.0176(14) -0.0005(12) 0.0039(12) 0.0033(11) C4 0.0173(14) 0.0101(15) 0.0240(15) 0.0044(12) 0.0076(12) 0.0046(11) C5 0.0202(15) 0.0206(17) 0.0166(14) 0.0076(13) 0.0042(12) 0.0076(12) C6 0.0149(14) 0.0234(17) 0.0107(13) 0.0005(12) 0.0012(11) 0.0033(12) C7 0.0114(13) 0.0241(17) 0.0135(13) -0.0038(13) -0.0041(11) 0.0021(12) C8 0.0114(14) 0.0205(17) 0.0203(15) -0.0043(13) -0.0006(12) -0.0024(12) C9 0.0088(13) 0.0175(16) 0.0222(14) -0.0037(13) 0.0051(11) -0.0047(11) C10 0.0118(14) 0.0144(16) 0.0244(15) 0.0005(12) 0.0064(12) -0.0044(11) C11 0.0165(14) 0.0177(16) 0.0168(14) -0.0002(12) 0.0086(11) -0.0009(12) C12 0.0176(14) 0.0196(16) 0.0111(13) -0.0002(12) 0.0099(12) 0.0029(12) C13 0.0195(15) 0.0226(17) 0.0119(13) -0.0049(12) 0.0058(12) 0.0008(12) C14 0.0174(14) 0.0111(15) 0.0236(15) -0.0064(12) 0.0081(12) 0.0007(11) C15 0.0214(15) 0.0123(16) 0.0233(15) -0.0091(13) 0.0066(13) -0.0044(12) C16 0.0169(14) 0.0095(15) 0.0278(16) -0.0018(12) 0.0062(13) -0.0036(11) C17 0.0210(15) 0.0114(15) 0.0269(16) 0.0069(13) 0.0099(13) 0.0008(12) C18 0.0257(16) 0.0196(17) 0.0202(15) 0.0081(13) 0.0117(13) 0.0009(13) C19 0.0209(15) 0.0256(18) 0.0115(14) 0.0088(12) 0.0040(12) 0.0065(13) C20 0.0218(15) 0.0291(19) 0.0107(14) 0.0032(13) 0.0055(12) 0.0043(13) C21 0.0184(15) 0.0280(18) 0.0099(13) -0.0044(13) -0.0011(11) 0.0039(13) C22 0.0231(16) 0.0274(18) 0.0128(14) -0.0114(13) 0.0003(12) -0.0003(13) C23 0.0205(15) 0.0176(17) 0.0251(15) -0.0140(14) 0.0019(13) -0.0002(13) C24 0.0156(14) 0.0161(16) 0.0273(16) -0.0080(13) 0.0017(12) -0.0040(12) C25 0.0169(15) 0.0118(16) 0.0287(16) 0.0005(13) 0.0046(13) -0.0040(12) C26 0.0177(14) 0.0120(16) 0.0292(16) 0.0052(13) 0.0088(13) -0.0056(12) C27 0.0236(15) 0.0179(17) 0.0221(15) 0.0104(13) 0.0086(13) -0.0007(13) C28 0.0200(15) 0.0243(18) 0.0159(14) 0.0038(13) 0.0105(12) -0.0004(13) C29 0.0252(16) 0.0271(18) 0.0091(13) 0.0036(13) 0.0070(12) 0.0025(13) C30 0.0218(15) 0.0233(17) 0.0121(14) -0.0037(13) 0.0045(12) 0.0004(13) C31 0.0180(15) 0.0252(18) 0.0108(13) -0.0091(13) -0.0003(12) -0.0040(13) C32 0.0162(14) 0.0154(16) 0.0221(15) -0.0130(13) -0.0018(12) -0.0043(12) C33 0.0132(14) 0.0178(17) 0.0245(15) -0.0050(13) -0.0003(12) -0.0050(12) C34 0.0172(15) 0.0137(16) 0.0360(17) 0.0010(14) 0.0099(13) -0.0066(12) C35 0.0176(15) 0.0184(17) 0.0301(16) 0.0046(14) 0.0134(13) -0.0040(12) C36 0.0189(15) 0.0245(18) 0.0230(15) 0.0090(13) 0.0140(12) 0.0010(13) C37 0.0220(15) 0.0298(19) 0.0159(14) 0.0017(13) 0.0135(12) 0.0038(13) C38 0.0220(15) 0.033(2) 0.0094(13) 0.0012(13) 0.0061(12) 0.0052(14) C39 0.0226(16) 0.0278(19) 0.0138(14) -0.0058(13) 0.0066(12) 0.0020(13) C40 0.0232(16) 0.0235(18) 0.0184(14) -0.0063(13) 0.0069(13) 0.0056(13) C41 0.0223(16) 0.0161(17) 0.0296(16) -0.0098(13) 0.0093(13) 0.0041(12) C42 0.0226(16) 0.0087(15) 0.0294(16) -0.0074(13) 0.0053(13) -0.0022(12) C43 0.0240(16) 0.0078(15) 0.0344(17) -0.0034(13) 0.0077(14) -0.0022(12) C44 0.0245(16) 0.0121(16) 0.0337(17) 0.0060(14) 0.0104(14) 0.0021(12) C45 0.0266(16) 0.0155(16) 0.0231(15) 0.0105(13) 0.0079(13) 0.0025(13) C46 0.0228(16) 0.0219(18) 0.0169(14) 0.0093(13) 0.0036(12) 0.0032(13) C47 0.0227(16) 0.0305(19) 0.0077(13) 0.0060(13) 0.0002(12) 0.0032(13) C48 0.0201(15) 0.0273(18) 0.0103(13) -0.0012(13) -0.0039(11) 0.0036(13) C49 0.0129(14) 0.0292(19) 0.0156(14) -0.0004(13) -0.0014(11) 0.0000(12) C50 0.0089(14) 0.0241(18) 0.0244(15) -0.0035(14) -0.0016(12) -0.0027(12) C51 0.0120(14) 0.0225(17) 0.0204(15) -0.0033(13) 0.0047(12) -0.0004(12) C52 0.0120(14) 0.0219(17) 0.0293(16) 0.0002(13) 0.0103(12) -0.0032(12) C53 0.0186(14) 0.0239(18) 0.0196(14) 0.0007(13) 0.0123(12) 0.0037(13) C54 0.0169(15) 0.0232(18) 0.0220(15) -0.0032(13) 0.0114(12) 0.0069(13) C55 0.0147(14) 0.0173(16) 0.0251(15) -0.0015(13) 0.0041(12) 0.0053(12) C56 0.0102(14) 0.0241(17) 0.0224(15) 0.0018(14) 0.0022(12) 0.0043(12) C57 0.0113(14) 0.0246(18) 0.0221(15) 0.0049(13) -0.0026(12) 0.0067(12) C58 0.0159(14) 0.0226(17) 0.0211(15) 0.0086(13) 0.0014(12) 0.0074(13) C59 0.0201(15) 0.0109(16) 0.0289(16) 0.0042(13) 0.0049(13) 0.0079(12) C60 0.0203(15) 0.0148(16) 0.0248(15) -0.0010(13) 0.0047(13) 0.0059(12) C61 0.0198(15) 0.0182(16) 0.0157(13) -0.0028(12) 0.0051(12) -0.0006(12) C62 0.0107(12) 0.0215(16) 0.0203(14) 0.0017(14) 0.0076(11) 0.0021(12) C63 0.0156(15) 0.0224(18) 0.0233(16) -0.0036(14) 0.0080(12) -0.0005(13) C64 0.0162(15) 0.0279(19) 0.0235(16) 0.0028(14) 0.0051(13) 0.0014(13) C65 0.0189(15) 0.0194(18) 0.0291(17) 0.0089(14) 0.0126(13) 0.0038(13) C66 0.0184(15) 0.0181(17) 0.0323(17) -0.0003(15) 0.0129(13) 0.0005(13) C67 0.0159(15) 0.0200(17) 0.0244(16) -0.0014(14) 0.0077(13) -0.0009(12) C68 0.0161(15) 0.0178(17) 0.0193(15) 0.0021(13) 0.0055(12) 0.0008(12) C69 0.0207(15) 0.0138(16) 0.0236(15) 0.0009(14) 0.0093(13) 0.0020(13) C70 0.0227(16) 0.0171(17) 0.0251(16) -0.0013(14) 0.0101(14) 0.0014(13) C71 0.0226(16) 0.0241(18) 0.0166(14) -0.0039(13) 0.0096(13) 0.0016(13) C72 0.0312(19) 0.0150(17) 0.0298(18) 0.0032(15) 0.0047(16) 0.0011(14) Cl1 0.0312(4) 0.0376(5) 0.0217(4) 0.0003(3) 0.0002(3) -0.0092(4) Cl2 0.0448(5) 0.0234(4) 0.0282(4) 0.0002(3) 0.0127(3) -0.0088(4) C73 0.0161(14) 0.0241(17) 0.0163(14) -0.0069(13) 0.0033(11) 0.0003(12) C74 0.0222(15) 0.0186(16) 0.0245(15) -0.0041(13) 0.0119(13) -0.0011(13) C75 0.0241(16) 0.032(2) 0.0181(15) -0.0024(15) 0.0078(13) 0.0047(14) C76 0.0158(16) 0.041(2) 0.0228(17) -0.0111(16) 0.0008(14) 0.0027(14) C77 0.0177(16) 0.0274(19) 0.0354(18) -0.0082(15) 0.0100(14) -0.0051(14) C78 0.0236(16) 0.0216(18) 0.0220(16) 0.0004(14) 0.0077(13) -0.0005(13) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C73 1.738(2) . . yes Cl2 C74 1.742(3) . . yes O1 C71 1.210(3) . . yes O2 C71 1.340(3) . . yes O2 C72 1.456(3) . . yes C1 C2 1.625(3) . . no C1 C61 1.518(3) . . no C1 C6 1.492(3) . . no C1 C9 1.481(4) . . no C2 C3 1.491(3) . . no C2 C12 1.488(3) . . no C2 C61 1.517(3) . . no C3 C4 1.381(3) . . no C3 C14 1.438(3) . . no C4 C5 1.470(3) . . no C4 C17 1.454(4) . . no C5 C19 1.459(4) . . no C5 C6 1.373(4) . . no C6 C7 1.443(4) . . no C7 C21 1.394(3) . . no C7 C8 1.449(4) . . no C8 C24 1.392(4) . . no C8 C9 1.446(3) . . no C9 C10 1.373(3) . . no C10 C11 1.479(3) . . no C10 C26 1.451(4) . . no C11 C28 1.442(3) . . no C11 C12 1.377(4) . . no C12 C13 1.443(3) . . no C13 C14 1.446(3) . . no C13 C30 1.390(3) . . no C14 C15 1.385(4) . . no C15 C32 1.450(3) . . no C15 C16 1.447(3) . . no C16 C17 1.388(3) . . no C16 C34 1.457(4) . . no C17 C18 1.454(3) . . no C18 C36 1.396(4) . . no C18 C19 1.449(4) . . no C19 C20 1.388(4) . . no C20 C21 1.440(4) . . no C20 C38 1.454(4) . . no C21 C22 1.448(4) . . no C22 C23 1.386(4) . . no C22 C39 1.450(4) . . no C23 C24 1.451(4) . . no C23 C42 1.451(4) . . no C24 C25 1.433(3) . . no C25 C26 1.396(3) . . no C25 C43 1.451(4) . . no C26 C27 1.447(3) . . no C27 C28 1.443(4) . . no C27 C45 1.393(4) . . no C28 C29 1.398(4) . . no C29 C47 1.459(4) . . no C29 C30 1.434(4) . . no C30 C31 1.454(4) . . no C31 C48 1.444(4) . . no C31 C32 1.389(3) . . no C32 C33 1.449(3) . . no C33 C34 1.446(4) . . no C33 C50 1.395(4) . . no C34 C35 1.381(4) . . no C35 C52 1.450(4) . . no C35 C36 1.455(4) . . no C36 C37 1.443(4) . . no C37 C38 1.397(4) . . no C37 C53 1.450(4) . . no C38 C39 1.451(4) . . no C39 C40 1.392(4) . . no C40 C54 1.450(4) . . no C40 C41 1.456(4) . . no C41 C42 1.393(4) . . no C41 C60 1.447(3) . . no C42 C43 1.453(4) . . no C43 C44 1.387(4) . . no C44 C59 1.453(4) . . no C44 C45 1.445(4) . . no C45 C46 1.459(4) . . no C46 C58 1.448(4) . . no C46 C47 1.381(4) . . no C47 C48 1.452(4) . . no C48 C49 1.392(3) . . no C49 C50 1.451(4) . . no C49 C57 1.449(4) . . no C50 C51 1.452(3) . . no C51 C56 1.448(4) . . no C51 C52 1.388(4) . . no C52 C53 1.455(4) . . no C53 C54 1.382(4) . . no C54 C55 1.455(3) . . no C55 C60 1.447(4) . . no C55 C56 1.384(4) . . no C56 C57 1.454(3) . . no C57 C58 1.390(4) . . no C58 C59 1.464(4) . . no C59 C60 1.390(4) . . no C61 C62 1.502(3) . . no C61 C68 1.533(4) . . no C62 C63 1.394(4) . . no C62 C67 1.394(4) . . no C63 C64 1.394(4) . . no C64 C65 1.383(4) . . no C65 C66 1.385(4) . . no C66 C67 1.388(4) . . no C68 C69 1.527(4) . . no C69 C70 1.537(4) . . no C70 C71 1.508(4) . . no C63 H63 1.02(2) . . no C64 H64 1.02(2) . . no C65 H65 1.01(2) . . no C66 H66 1.00(2) . . no C67 H67 1.03(2) . . no C68 H68' 1.09(2) . . no C68 H68 1.01(2) . . no C69 H69' 1.02(2) . . no C69 H69 1.06(2) . . no C70 H70' 1.02(2) . . no C70 H70 0.99(2) . . no C72 H72" 1.04(3) . . no C72 H72 0.96(2) . . no C72 H72' 1.07(3) . . no C73 C74 1.381(3) . . no C73 C78 1.384(4) . . no C74 C75 1.381(4) . . no C75 C76 1.387(4) . . no C76 C77 1.388(4) . . no C77 C78 1.382(4) . . no C75 H75 0.98(2) . . no C76 H76 0.97(2) . . no C77 H77 1.07(2) . . no C78 H78 1.04(2) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C71 O2 C72 116.0(2) . . . yes C2 C1 C6 114.9(2) . . . no C2 C1 C9 114.74(19) . . . no C2 C1 C61 57.61(15) . . . no C6 C1 C9 105.4(2) . . . no C6 C1 C61 126.1(2) . . . no C9 C1 C61 126.8(2) . . . no C1 C2 C3 115.06(19) . . . no C1 C2 C12 115.0(2) . . . no C1 C2 C61 57.65(15) . . . no C3 C2 C12 104.81(19) . . . no C3 C2 C61 126.3(2) . . . no C12 C2 C61 127.1(2) . . . no C2 C3 C4 123.4(2) . . . no C2 C3 C14 108.4(2) . . . no C4 C3 C14 119.2(2) . . . no C3 C4 C5 121.0(2) . . . no C3 C4 C17 119.4(2) . . . no C5 C4 C17 107.7(2) . . . no C4 C5 C6 120.8(2) . . . no C4 C5 C19 107.5(2) . . . no C6 C5 C19 119.7(2) . . . no C1 C6 C5 123.9(2) . . . no C1 C6 C7 107.7(2) . . . no C5 C6 C7 119.6(2) . . . no C6 C7 C8 108.8(2) . . . no C6 C7 C21 121.3(2) . . . no C8 C7 C21 119.9(2) . . . no C7 C8 C9 108.2(2) . . . no C7 C8 C24 120.2(2) . . . no C9 C8 C24 121.5(2) . . . no C1 C9 C8 108.3(2) . . . no C1 C9 C10 124.5(2) . . . no C8 C9 C10 118.9(2) . . . no C9 C10 C11 120.4(2) . . . no C9 C10 C26 120.3(2) . . . no C11 C10 C26 107.2(2) . . . no C10 C11 C12 120.6(2) . . . no C10 C11 C28 107.4(2) . . . no C12 C11 C28 120.7(2) . . . no C2 C12 C11 123.9(2) . . . no C2 C12 C13 108.3(2) . . . no C11 C12 C13 119.0(2) . . . no C12 C13 C14 108.5(2) . . . no C12 C13 C30 120.8(2) . . . no C14 C13 C30 120.1(2) . . . no C3 C14 C13 108.5(2) . . . no C3 C14 C15 121.9(2) . . . no C13 C14 C15 119.8(2) . . . no C14 C15 C16 119.0(2) . . . no C14 C15 C32 120.6(2) . . . no C16 C15 C32 108.3(2) . . . no C15 C16 C17 119.4(2) . . . no C15 C16 C34 107.7(2) . . . no C17 C16 C34 120.1(2) . . . no C4 C17 C16 121.0(2) . . . no C4 C17 C18 108.3(2) . . . no C16 C17 C18 119.7(2) . . . no C17 C18 C19 108.1(2) . . . no C17 C18 C36 120.1(2) . . . no C19 C18 C36 119.7(2) . . . no C5 C19 C18 108.4(2) . . . no C5 C19 C20 120.3(2) . . . no C18 C19 C20 120.1(2) . . . no C19 C20 C21 120.1(2) . . . no C19 C20 C38 120.3(2) . . . no C21 C20 C38 107.2(2) . . . no C7 C21 C20 118.9(2) . . . no C7 C21 C22 120.1(2) . . . no C20 C21 C22 109.1(2) . . . no C21 C22 C23 119.8(2) . . . no C21 C22 C39 107.6(2) . . . no C23 C22 C39 120.3(2) . . . no C22 C23 C24 120.5(2) . . . no C22 C23 C42 120.0(2) . . . no C24 C23 C42 107.6(2) . . . no C8 C24 C23 119.5(2) . . . no C8 C24 C25 119.2(2) . . . no C23 C24 C25 108.7(2) . . . no C24 C25 C26 119.8(2) . . . no C24 C25 C43 107.9(2) . . . no C26 C25 C43 119.8(2) . . . no C10 C26 C25 120.2(2) . . . no C10 C26 C27 108.5(2) . . . no C25 C26 C27 120.0(2) . . . no C26 C27 C28 108.0(2) . . . no C26 C27 C45 120.0(2) . . . no C28 C27 C45 120.6(2) . . . no C11 C28 C27 108.9(2) . . . no C11 C28 C29 119.9(2) . . . no C27 C28 C29 119.9(2) . . . no C28 C29 C30 119.6(2) . . . no C28 C29 C47 119.4(2) . . . no C30 C29 C47 108.7(2) . . . no C13 C30 C29 119.8(2) . . . no C13 C30 C31 120.1(2) . . . no C29 C30 C31 107.9(2) . . . no C30 C31 C32 119.7(2) . . . no C30 C31 C48 107.9(2) . . . no C32 C31 C48 120.3(2) . . . no C15 C32 C31 119.8(2) . . . no C15 C32 C33 107.8(2) . . . no C31 C32 C33 120.1(2) . . . no C32 C33 C34 108.2(2) . . . no C32 C33 C50 119.8(2) . . . no C34 C33 C50 119.9(2) . . . no C16 C34 C33 107.9(2) . . . no C16 C34 C35 120.4(2) . . . no C33 C34 C35 120.2(2) . . . no C34 C35 C36 119.8(2) . . . no C34 C35 C52 120.0(2) . . . no C36 C35 C52 107.7(2) . . . no C18 C36 C35 119.9(2) . . . no C18 C36 C37 120.4(2) . . . no C35 C36 C37 108.1(2) . . . no C36 C37 C38 120.0(2) . . . no C36 C37 C53 108.3(2) . . . no C38 C37 C53 119.8(2) . . . no C20 C38 C37 119.5(2) . . . no C20 C38 C39 108.5(2) . . . no C37 C38 C39 119.9(2) . . . no C22 C39 C38 107.7(2) . . . no C22 C39 C40 120.1(2) . . . no C38 C39 C40 120.0(2) . . . no C39 C40 C41 119.6(2) . . . no C39 C40 C54 119.8(2) . . . no C41 C40 C54 108.0(2) . . . no C40 C41 C42 120.1(2) . . . no C40 C41 C60 107.7(2) . . . no C42 C41 C60 120.2(2) . . . no C23 C42 C41 119.9(2) . . . no C23 C42 C43 107.8(2) . . . no C41 C42 C43 120.2(2) . . . no C25 C43 C42 108.0(2) . . . no C25 C43 C44 120.1(2) . . . no C42 C43 C44 119.7(2) . . . no C43 C44 C45 120.2(2) . . . no C43 C44 C59 119.9(2) . . . no C45 C44 C59 108.0(2) . . . no C27 C45 C44 120.0(2) . . . no C27 C45 C46 119.6(2) . . . no C44 C45 C46 108.4(2) . . . no C45 C46 C47 119.9(2) . . . no C45 C46 C58 107.9(2) . . . no C47 C46 C58 120.2(2) . . . no C29 C47 C46 120.6(2) . . . no C29 C47 C48 107.0(2) . . . no C46 C47 C48 119.9(2) . . . no C31 C48 C47 108.4(2) . . . no C31 C48 C49 119.8(2) . . . no C47 C48 C49 119.9(2) . . . no C48 C49 C50 120.1(2) . . . no C48 C49 C57 120.2(2) . . . no C50 C49 C57 107.9(2) . . . no C33 C50 C49 119.9(2) . . . no C33 C50 C51 120.0(2) . . . no C49 C50 C51 108.0(2) . . . no C50 C51 C52 119.5(2) . . . no C50 C51 C56 108.0(2) . . . no C52 C51 C56 120.1(2) . . . no C35 C52 C51 120.3(2) . . . no C35 C52 C53 108.2(2) . . . no C51 C52 C53 119.8(2) . . . no C37 C53 C52 107.7(2) . . . no C37 C53 C54 120.1(2) . . . no C52 C53 C54 119.8(2) . . . no C40 C54 C53 120.3(2) . . . no C40 C54 C55 108.0(2) . . . no C53 C54 C55 120.4(2) . . . no C54 C55 C56 119.6(2) . . . no C54 C55 C60 107.7(2) . . . no C56 C55 C60 120.7(2) . . . no C51 C56 C55 120.3(2) . . . no C51 C56 C57 107.9(2) . . . no C55 C56 C57 119.7(2) . . . no C49 C57 C56 108.1(2) . . . no C49 C57 C58 119.5(2) . . . no C56 C57 C58 120.3(2) . . . no C46 C58 C57 120.3(2) . . . no C46 C58 C59 107.8(2) . . . no C57 C58 C59 119.6(2) . . . no C44 C59 C58 107.9(2) . . . no C44 C59 C60 120.6(2) . . . no C58 C59 C60 119.9(2) . . . no C41 C60 C55 108.6(2) . . . no C41 C60 C59 119.5(2) . . . no C55 C60 C59 119.9(2) . . . no C1 C61 C2 64.74(16) . . . no C1 C61 C62 117.04(19) . . . no C1 C61 C68 116.4(2) . . . no C2 C61 C62 117.5(2) . . . no C2 C61 C68 116.57(19) . . . no C62 C61 C68 115.3(2) . . . no C61 C62 C63 120.0(2) . . . no C61 C62 C67 121.1(2) . . . no C63 C62 C67 118.9(2) . . . no C62 C63 C64 120.6(3) . . . no C63 C64 C65 119.8(3) . . . no C64 C65 C66 120.1(3) . . . no C65 C66 C67 120.2(3) . . . no C62 C67 C66 120.5(2) . . . no C61 C68 C69 114.4(2) . . . no C68 C69 C70 110.9(2) . . . no C69 C70 C71 112.0(2) . . . no O1 C71 O2 123.3(2) . . . yes O1 C71 C70 125.0(3) . . . yes O2 C71 C70 111.6(2) . . . yes C62 C63 H63 117.7(13) . . . no C64 C63 H63 121.7(13) . . . no C63 C64 H64 119.0(12) . . . no C65 C64 H64 121.1(12) . . . no C64 C65 H65 119.5(12) . . . no C66 C65 H65 120.3(12) . . . no C65 C66 H66 122.4(12) . . . no C67 C66 H66 117.4(12) . . . no C62 C67 H67 124.7(13) . . . no C66 C67 H67 114.8(13) . . . no C61 C68 H68 107.7(12) . . . no C61 C68 H68' 108.1(11) . . . no C69 C68 H68 108.7(12) . . . no C69 C68 H68' 110.2(11) . . . no H68 C68 H68' 107.6(17) . . . no C68 C69 H69 111.3(12) . . . no C68 C69 H69' 108.9(11) . . . no C70 C69 H69 106.9(12) . . . no C70 C69 H69' 110.5(11) . . . no H69 C69 H69' 108.3(16) . . . no C69 C70 H70 110.8(13) . . . no C69 C70 H70' 112.5(14) . . . no C71 C70 H70 108.4(14) . . . no C71 C70 H70' 104.9(14) . . . no H70 C70 H70' 108.0(19) . . . no O2 C72 H72 110.7(14) . . . no O2 C72 H72' 107.1(16) . . . no O2 C72 H72" 103.0(16) . . . no H72 C72 H72' 109(2) . . . no H72 C72 H72" 111.6(19) . . . no H72' C72 H72" 116(2) . . . no Cl1 C73 C74 121.1(2) . . . yes Cl1 C73 C78 118.83(19) . . . yes C74 C73 C78 120.0(2) . . . no Cl2 C74 C73 120.05(19) . . . yes Cl2 C74 C75 119.2(2) . . . yes C73 C74 C75 120.8(2) . . . no C74 C75 C76 119.3(3) . . . no C75 C76 C77 119.9(3) . . . no C76 C77 C78 120.4(3) . . . no C73 C78 C77 119.5(2) . . . no C74 C75 H75 122.4(14) . . . no C76 C75 H75 118.1(14) . . . no C75 C76 H76 118.5(13) . . . no C77 C76 H76 121.5(13) . . . no C76 C77 H77 119.3(11) . . . no C78 C77 H77 120.3(11) . . . no C73 C78 H78 119.1(13) . . . no C77 C78 H78 121.3(13) . . . no 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 C72 O2 C71 O1 2.9(3) . . . . no C72 O2 C71 C70 -178.1(2) . . . . no C6 C1 C2 C12 122.2(2) . . . . no C9 C1 C2 C12 -0.2(3) . . . . no C6 C1 C2 C61 -118.3(2) . . . . no C9 C1 C2 C3 -122.2(2) . . . . no C6 C1 C2 C3 0.2(3) . . . . no C2 C1 C6 C5 7.5(3) . . . . no C2 C1 C6 C7 -139.6(2) . . . . no C9 C1 C6 C5 134.9(3) . . . . no C9 C1 C6 C7 -12.3(3) . . . . no C9 C1 C2 C61 119.3(2) . . . . no C61 C1 C2 C3 118.5(2) . . . . no C61 C1 C2 C12 -119.5(2) . . . . no C2 C1 C9 C10 -7.7(3) . . . . no C6 C1 C9 C8 12.5(3) . . . . no C6 C1 C9 C10 -135.2(2) . . . . no C61 C1 C9 C8 -153.1(2) . . . . no C61 C1 C9 C10 59.2(3) . . . . no C2 C1 C61 C62 -109.4(2) . . . . no C2 C1 C61 C68 108.5(2) . . . . no C6 C1 C61 C2 98.9(3) . . . . no C6 C1 C61 C62 -10.5(3) . . . . no C6 C1 C61 C68 -152.6(2) . . . . no C9 C1 C61 C2 -98.3(3) . . . . no C9 C1 C61 C62 152.3(2) . . . . no C61 C1 C6 C5 -59.4(4) . . . . no C61 C1 C6 C7 153.5(2) . . . . no C2 C1 C9 C8 140.0(2) . . . . no C9 C1 C61 C68 10.2(3) . . . . no C12 C2 C3 C14 11.6(3) . . . . no C61 C2 C3 C4 59.3(3) . . . . no C61 C2 C3 C14 -153.9(2) . . . . no C1 C2 C12 C11 7.4(3) . . . . no C1 C2 C12 C13 -139.4(2) . . . . no C3 C2 C12 C11 134.8(2) . . . . no C3 C2 C12 C13 -12.1(3) . . . . no C61 C2 C12 C11 -59.8(4) . . . . no C61 C2 C12 C13 153.3(2) . . . . no C1 C2 C61 C62 108.7(2) . . . . no C1 C2 C61 C68 -108.3(2) . . . . no C3 C2 C61 C1 -99.0(3) . . . . no C3 C2 C61 C62 9.7(3) . . . . no C3 C2 C61 C68 152.7(2) . . . . no C12 C2 C3 C4 -135.1(2) . . . . no C12 C2 C61 C62 -152.7(2) . . . . no C12 C2 C61 C68 -9.7(4) . . . . no C1 C2 C3 C14 139.0(2) . . . . no C12 C2 C61 C1 98.6(3) . . . . no C1 C2 C3 C4 -7.7(3) . . . . no C2 C3 C4 C17 146.2(2) . . . . no C2 C3 C14 C13 -7.0(3) . . . . no C14 C3 C4 C5 -135.4(2) . . . . no C14 C3 C4 C17 2.8(3) . . . . no C2 C3 C4 C5 8.0(4) . . . . no C4 C3 C14 C15 -4.2(4) . . . . no C2 C3 C14 C15 -152.6(2) . . . . no C4 C3 C14 C13 141.4(2) . . . . no C3 C4 C5 C6 0.1(4) . . . . no C3 C4 C5 C19 142.6(2) . . . . no C17 C4 C5 C6 -142.4(2) . . . . no C17 C4 C5 C19 0.1(4) . . . . no C5 C4 C17 C18 -0.7(3) . . . . no C5 C4 C17 C16 143.2(2) . . . . no C3 C4 C17 C16 0.0(4) . . . . no C3 C4 C17 C18 -143.9(2) . . . . no C4 C5 C6 C7 135.4(2) . . . . no C4 C5 C19 C18 0.5(3) . . . . no C19 C5 C6 C1 -146.1(2) . . . . no C19 C5 C6 C7 -2.6(3) . . . . no C4 C5 C6 C1 -8.1(4) . . . . no C6 C5 C19 C20 -0.2(4) . . . . no C4 C5 C19 C20 -143.2(2) . . . . no C6 C5 C19 C18 143.4(2) . . . . no C1 C6 C7 C8 7.6(3) . . . . no C1 C6 C7 C21 152.9(2) . . . . no C5 C6 C7 C8 -141.2(2) . . . . no C5 C6 C7 C21 4.1(3) . . . . no C21 C7 C8 C24 0.2(4) . . . . no C6 C7 C21 C20 -2.5(3) . . . . no C6 C7 C21 C22 -141.2(2) . . . . no C8 C7 C21 C20 139.1(2) . . . . no C8 C7 C21 C22 0.4(4) . . . . no C6 C7 C8 C9 0.3(3) . . . . no C6 C7 C8 C24 146.0(2) . . . . no C21 C7 C8 C9 -145.5(2) . . . . no C24 C8 C9 C10 -3.6(4) . . . . no C7 C8 C24 C23 -0.8(4) . . . . no C7 C8 C24 C25 -138.4(2) . . . . no C9 C8 C24 C23 140.3(2) . . . . no C7 C8 C9 C1 -8.2(3) . . . . no C7 C8 C9 C10 141.6(2) . . . . no C24 C8 C9 C1 -153.3(2) . . . . no C9 C8 C24 C25 2.6(4) . . . . no C8 C9 C10 C26 1.9(4) . . . . no C1 C9 C10 C26 146.4(2) . . . . no C8 C9 C10 C11 -135.8(2) . . . . no C1 C9 C10 C11 8.8(4) . . . . no C9 C10 C11 C28 142.8(2) . . . . no C9 C10 C26 C25 0.7(4) . . . . no C26 C10 C11 C12 -143.6(2) . . . . no C26 C10 C11 C28 0.3(3) . . . . no C9 C10 C11 C12 -1.0(4) . . . . no C11 C10 C26 C27 -0.3(3) . . . . no C9 C10 C26 C27 -142.9(2) . . . . no C11 C10 C26 C25 143.2(2) . . . . no C10 C11 C12 C2 -7.2(4) . . . . no C10 C11 C12 C13 136.4(2) . . . . no C28 C11 C12 C2 -146.4(2) . . . . no C28 C11 C12 C13 -2.8(3) . . . . no C12 C11 C28 C29 0.1(4) . . . . no C12 C11 C28 C27 143.6(2) . . . . no C10 C11 C28 C27 -0.2(3) . . . . no C10 C11 C28 C29 -143.8(2) . . . . no C2 C12 C13 C14 8.2(3) . . . . no C2 C12 C13 C30 152.8(2) . . . . no C11 C12 C13 C14 -140.6(2) . . . . no C11 C12 C13 C30 4.0(3) . . . . no C30 C13 C14 C15 0.9(4) . . . . no C12 C13 C30 C29 -2.5(3) . . . . no C12 C13 C30 C31 -140.5(2) . . . . no C14 C13 C30 C29 138.0(2) . . . . no C12 C13 C14 C3 -0.7(3) . . . . no C12 C13 C14 C15 145.7(2) . . . . no C30 C13 C14 C3 -145.6(2) . . . . no C14 C13 C30 C31 0.0(4) . . . . no C13 C14 C15 C32 -1.3(4) . . . . no C3 C14 C15 C32 140.6(2) . . . . no C13 C14 C15 C16 -139.3(2) . . . . no C3 C14 C15 C16 2.6(4) . . . . no C14 C15 C16 C17 0.4(4) . . . . no C14 C15 C16 C34 142.0(2) . . . . no C32 C15 C16 C17 -142.3(2) . . . . no C32 C15 C16 C34 -0.7(3) . . . . no C16 C15 C32 C33 0.4(3) . . . . no C14 C15 C32 C31 0.8(4) . . . . no C14 C15 C32 C33 -141.6(2) . . . . no C16 C15 C32 C31 142.7(2) . . . . no C15 C16 C17 C4 -1.7(4) . . . . no C15 C16 C17 C18 138.2(3) . . . . no C34 C16 C17 C4 -138.5(2) . . . . no C17 C16 C34 C33 142.0(2) . . . . no C17 C16 C34 C35 -1.3(4) . . . . no C34 C16 C17 C18 1.4(4) . . . . no C15 C16 C34 C33 0.8(3) . . . . no C15 C16 C34 C35 -142.6(2) . . . . no C4 C17 C18 C19 1.0(3) . . . . no C4 C17 C18 C36 143.3(2) . . . . no C16 C17 C18 C19 -143.5(2) . . . . no C16 C17 C18 C36 -1.1(4) . . . . no C36 C18 C19 C5 -143.4(2) . . . . no C17 C18 C36 C35 0.8(4) . . . . no C17 C18 C36 C37 -138.1(3) . . . . no C36 C18 C19 C20 0.4(4) . . . . no C17 C18 C19 C5 -0.9(3) . . . . no C17 C18 C19 C20 142.9(2) . . . . no C19 C18 C36 C37 -0.1(4) . . . . no C19 C18 C36 C35 138.8(2) . . . . no C18 C19 C20 C38 -0.4(3) . . . . no C5 C19 C20 C21 1.8(3) . . . . no C5 C19 C20 C38 139.0(2) . . . . no C18 C19 C20 C21 -137.7(2) . . . . no C38 C20 C21 C7 -142.6(2) . . . . no C19 C20 C21 C22 142.4(2) . . . . no C19 C20 C38 C39 -142.2(2) . . . . no C38 C20 C21 C22 0.3(3) . . . . no C19 C20 C38 C37 0.2(3) . . . . no C19 C20 C21 C7 -0.4(3) . . . . no C21 C20 C38 C37 142.3(2) . . . . no C21 C20 C38 C39 -0.1(2) . . . . no C7 C21 C22 C39 142.0(2) . . . . no C7 C21 C22 C23 -0.2(4) . . . . no C20 C21 C22 C23 -142.6(2) . . . . no C20 C21 C22 C39 -0.3(3) . . . . no C21 C22 C23 C24 -0.4(4) . . . . no C21 C22 C39 C38 0.2(3) . . . . no C21 C22 C39 C40 -142.2(2) . . . . no C23 C22 C39 C38 142.3(2) . . . . no C23 C22 C39 C40 -0.1(4) . . . . no C39 C22 C23 C42 0.2(4) . . . . no C21 C22 C23 C42 137.8(2) . . . . no C39 C22 C23 C24 -137.9(3) . . . . no C22 C23 C24 C8 0.9(4) . . . . no C22 C23 C42 C41 -0.3(4) . . . . no C22 C23 C42 C43 -142.7(2) . . . . no C24 C23 C42 C41 142.6(2) . . . . no C24 C23 C42 C43 0.2(3) . . . . no C22 C23 C24 C25 142.5(2) . . . . no C42 C23 C24 C8 -141.8(2) . . . . no C42 C23 C24 C25 -0.2(3) . . . . no C23 C24 C25 C43 0.1(3) . . . . no C23 C24 C25 C26 -141.8(2) . . . . no C8 C24 C25 C26 0.0(4) . . . . no C8 C24 C25 C43 141.9(2) . . . . no C24 C25 C26 C27 137.8(3) . . . . no C24 C25 C43 C42 0.0(3) . . . . no C43 C25 C26 C10 -139.1(2) . . . . no C43 C25 C26 C27 0.3(4) . . . . no C24 C25 C26 C10 -1.6(4) . . . . no C26 C25 C43 C44 -0.3(4) . . . . no C24 C25 C43 C44 -142.3(2) . . . . no C26 C25 C43 C42 142.0(2) . . . . no C10 C26 C27 C28 0.2(3) . . . . no C10 C26 C27 C45 143.9(2) . . . . no C25 C26 C27 C28 -143.4(2) . . . . no C25 C26 C27 C45 0.3(4) . . . . no C45 C27 C28 C29 0.1(4) . . . . no C26 C27 C45 C44 -0.9(4) . . . . no C26 C27 C45 C46 -139.0(2) . . . . no C28 C27 C45 C44 138.3(3) . . . . no C28 C27 C45 C46 0.2(4) . . . . no C26 C27 C28 C11 0.0(3) . . . . no C26 C27 C28 C29 143.6(2) . . . . no C45 C27 C28 C11 -143.5(2) . . . . no C27 C28 C29 C47 -0.1(3) . . . . no C11 C28 C29 C30 1.5(4) . . . . no C11 C28 C29 C47 139.5(2) . . . . no C27 C28 C29 C30 -138.1(2) . . . . no C28 C29 C30 C13 -0.2(4) . . . . no C28 C29 C30 C31 142.3(2) . . . . no C47 C29 C30 C13 -142.3(2) . . . . no C30 C29 C47 C46 141.9(2) . . . . no C30 C29 C47 C48 0.0(2) . . . . no C28 C29 C47 C48 -142.1(2) . . . . no C47 C29 C30 C31 0.2(3) . . . . no C28 C29 C47 C46 -0.3(4) . . . . no C13 C30 C31 C48 142.0(2) . . . . no C13 C30 C31 C32 -0.5(4) . . . . no C29 C30 C31 C32 -143.0(2) . . . . no C29 C30 C31 C48 -0.4(2) . . . . no C30 C31 C32 C15 0.1(4) . . . . no C30 C31 C48 C47 0.4(2) . . . . no C30 C31 C48 C49 -142.5(2) . . . . no C32 C31 C48 C47 142.7(2) . . . . no C32 C31 C48 C49 -0.2(4) . . . . no C30 C31 C32 C33 137.9(2) . . . . no C48 C31 C32 C15 -137.8(2) . . . . no C48 C31 C32 C33 -0.1(4) . . . . no C31 C32 C33 C50 0.3(4) . . . . no C31 C32 C33 C34 -142.1(2) . . . . no C15 C32 C33 C34 0.1(3) . . . . no C15 C32 C33 C50 142.5(2) . . . . no C32 C33 C34 C16 -0.5(3) . . . . no C32 C33 C34 C35 142.9(2) . . . . no C50 C33 C34 C16 -142.9(2) . . . . no C50 C33 C34 C35 0.5(4) . . . . no C34 C33 C50 C51 -0.4(4) . . . . no C32 C33 C50 C49 -0.3(4) . . . . no C32 C33 C50 C51 -138.5(2) . . . . no C34 C33 C50 C49 137.8(2) . . . . no C16 C34 C35 C36 1.0(4) . . . . no C16 C34 C35 C52 138.3(3) . . . . no C33 C34 C35 C36 -137.9(3) . . . . no C33 C34 C35 C52 -0.6(4) . . . . no C52 C35 C36 C37 0.7(3) . . . . no C34 C35 C52 C51 0.5(4) . . . . no C52 C35 C36 C18 -142.7(2) . . . . no C36 C35 C52 C51 142.4(2) . . . . no C36 C35 C52 C53 -0.6(3) . . . . no C34 C35 C52 C53 -142.5(2) . . . . no C34 C35 C36 C18 -0.7(4) . . . . no C34 C35 C36 C37 142.7(2) . . . . no C35 C36 C37 C53 -0.5(3) . . . . no C18 C36 C37 C38 -0.1(4) . . . . no C18 C36 C37 C53 142.7(2) . . . . no C35 C36 C37 C38 -143.3(2) . . . . no C36 C37 C38 C20 0.0(4) . . . . no C36 C37 C38 C39 138.2(2) . . . . no C53 C37 C38 C20 -138.5(2) . . . . no C38 C37 C53 C52 143.0(2) . . . . no C38 C37 C53 C54 1.0(4) . . . . no C53 C37 C38 C39 -0.4(4) . . . . no C36 C37 C53 C52 0.1(3) . . . . no C36 C37 C53 C54 -141.8(2) . . . . no C20 C38 C39 C22 0.0(3) . . . . no C20 C38 C39 C40 142.4(2) . . . . no C37 C38 C39 C22 -142.3(2) . . . . no C37 C38 C39 C40 0.1(4) . . . . no C38 C39 C40 C41 -137.8(2) . . . . no C22 C39 C40 C41 0.0(4) . . . . no C22 C39 C40 C54 137.3(3) . . . . no C38 C39 C40 C54 -0.4(4) . . . . no C39 C40 C41 C42 -0.1(4) . . . . no C39 C40 C41 C60 142.5(2) . . . . no C39 C40 C54 C55 -142.6(2) . . . . no C41 C40 C54 C53 142.9(2) . . . . no C41 C40 C54 C55 -0.9(3) . . . . no C39 C40 C54 C53 1.1(4) . . . . no C54 C40 C41 C42 -141.9(2) . . . . no C54 C40 C41 C60 0.7(3) . . . . no C40 C41 C42 C43 138.0(2) . . . . no C40 C41 C60 C55 -0.2(3) . . . . no C60 C41 C42 C23 -137.8(2) . . . . no C60 C41 C42 C43 0.1(4) . . . . no C40 C41 C42 C23 0.2(4) . . . . no C42 C41 C60 C59 -0.2(4) . . . . no C40 C41 C60 C59 -142.8(2) . . . . no C42 C41 C60 C55 142.3(2) . . . . no C23 C42 C43 C25 -0.1(3) . . . . no C23 C42 C43 C44 142.3(2) . . . . no C41 C42 C43 C25 -142.4(2) . . . . no C41 C42 C43 C44 0.0(4) . . . . no C42 C43 C44 C59 0.1(4) . . . . no C42 C43 C44 C45 -138.2(3) . . . . no C25 C43 C44 C45 -0.2(4) . . . . no C25 C43 C44 C59 138.0(3) . . . . no C43 C44 C45 C27 0.8(4) . . . . no C43 C44 C45 C46 143.1(2) . . . . no C59 C44 C45 C27 -141.8(2) . . . . no C59 C44 C45 C46 0.5(3) . . . . no C45 C44 C59 C60 142.5(2) . . . . no C43 C44 C59 C58 -143.3(2) . . . . no C43 C44 C59 C60 -0.2(4) . . . . no C45 C44 C59 C58 -0.5(3) . . . . no C27 C45 C46 C47 -0.5(4) . . . . no C27 C45 C46 C58 142.2(2) . . . . no C44 C45 C46 C47 -143.0(2) . . . . no C44 C45 C46 C58 -0.3(3) . . . . no C58 C46 C47 C48 -0.5(4) . . . . no C45 C46 C58 C57 -142.1(2) . . . . no C58 C46 C47 C29 -137.6(2) . . . . no C47 C46 C58 C57 0.4(4) . . . . no C47 C46 C58 C59 142.5(2) . . . . no C45 C46 C58 C59 0.0(3) . . . . no C45 C46 C47 C29 0.5(4) . . . . no C45 C46 C47 C48 137.6(2) . . . . no C46 C47 C48 C49 0.4(3) . . . . no C29 C47 C48 C31 -0.3(2) . . . . no C29 C47 C48 C49 142.6(2) . . . . no C46 C47 C48 C31 -142.4(2) . . . . no C31 C48 C49 C50 0.2(4) . . . . no C31 C48 C49 C57 138.5(2) . . . . no C47 C48 C49 C50 -138.5(2) . . . . no C47 C48 C49 C57 -0.2(4) . . . . no C57 C49 C50 C33 -142.8(2) . . . . no C57 C49 C50 C51 -0.1(3) . . . . no C48 C49 C57 C58 0.1(4) . . . . no C50 C49 C57 C56 0.2(3) . . . . no C48 C49 C57 C56 -142.6(2) . . . . no C48 C49 C50 C33 0.0(4) . . . . no C48 C49 C50 C51 142.7(2) . . . . no C50 C49 C57 C58 142.9(2) . . . . no C49 C50 C51 C52 -142.2(2) . . . . no C33 C50 C51 C52 0.3(4) . . . . no C33 C50 C51 C56 142.6(2) . . . . no C49 C50 C51 C56 0.0(3) . . . . no C50 C51 C52 C35 -0.4(4) . . . . no C50 C51 C52 C53 138.4(3) . . . . no C50 C51 C56 C57 0.1(3) . . . . no C52 C51 C56 C55 -0.2(4) . . . . no C52 C51 C56 C57 142.1(2) . . . . no C50 C51 C56 C55 -142.2(2) . . . . no C56 C51 C52 C35 -138.1(3) . . . . no C56 C51 C52 C53 0.7(4) . . . . no C35 C52 C53 C37 0.3(3) . . . . no C35 C52 C53 C54 142.4(2) . . . . no C51 C52 C53 C37 -143.0(2) . . . . no C51 C52 C53 C54 -0.8(4) . . . . no C52 C53 C54 C55 0.5(4) . . . . no C37 C53 C54 C40 -1.4(4) . . . . no C37 C53 C54 C55 137.9(2) . . . . no C52 C53 C54 C40 -138.9(2) . . . . no C40 C54 C55 C56 143.7(2) . . . . no C40 C54 C55 C60 0.8(3) . . . . no C53 C54 C55 C56 0.0(4) . . . . no C53 C54 C55 C60 -143.0(2) . . . . no C60 C55 C56 C51 138.0(3) . . . . no C60 C55 C56 C57 0.0(4) . . . . no C54 C55 C60 C59 142.1(2) . . . . no C56 C55 C60 C41 -142.8(2) . . . . no C54 C55 C60 C41 -0.4(3) . . . . no C54 C55 C56 C51 -0.1(4) . . . . no C54 C55 C56 C57 -138.1(3) . . . . no C56 C55 C60 C59 -0.4(4) . . . . no C55 C56 C57 C49 142.4(2) . . . . no C51 C56 C57 C49 -0.2(3) . . . . no C51 C56 C57 C58 -142.5(2) . . . . no C55 C56 C57 C58 0.1(4) . . . . no C49 C57 C58 C46 -0.2(4) . . . . no C49 C57 C58 C59 -137.9(2) . . . . no C56 C57 C58 C59 0.2(4) . . . . no C56 C57 C58 C46 137.9(2) . . . . no C57 C58 C59 C44 142.7(2) . . . . no C57 C58 C59 C60 -0.6(4) . . . . no C46 C58 C59 C60 -143.0(2) . . . . no C46 C58 C59 C44 0.4(3) . . . . no C44 C59 C60 C41 0.3(4) . . . . no C44 C59 C60 C55 -138.1(3) . . . . no C58 C59 C60 C41 139.1(3) . . . . no C58 C59 C60 C55 0.7(4) . . . . no C2 C61 C62 C63 -123.3(2) . . . . no C68 C61 C62 C63 93.2(3) . . . . no C68 C61 C62 C67 -84.2(3) . . . . no C2 C61 C62 C67 59.2(3) . . . . no C1 C61 C62 C63 -49.3(3) . . . . no C1 C61 C62 C67 133.3(2) . . . . no C62 C61 C68 C69 78.8(3) . . . . no C1 C61 C68 C69 -138.5(2) . . . . no C2 C61 C68 C69 -65.0(3) . . . . no C67 C62 C63 C64 -0.4(4) . . . . no C61 C62 C63 C64 -177.9(2) . . . . no C61 C62 C67 C66 177.0(2) . . . . no C63 C62 C67 C66 -0.4(4) . . . . no C62 C63 C64 C65 0.7(4) . . . . no C63 C64 C65 C66 -0.2(4) . . . . no C64 C65 C66 C67 -0.6(4) . . . . no C65 C66 C67 C62 0.9(4) . . . . no C61 C68 C69 C70 174.8(2) . . . . no C68 C69 C70 C71 -61.0(3) . . . . no C69 C70 C71 O1 -37.1(4) . . . . no C69 C70 C71 O2 143.8(2) . . . . no Cl1 C73 C74 Cl2 0.6(3) . . . . no Cl1 C73 C74 C75 -179.5(2) . . . . no C78 C73 C74 Cl2 179.7(2) . . . . no C78 C73 C74 C75 -0.4(4) . . . . no Cl1 C73 C78 C77 178.5(2) . . . . no C74 C73 C78 C77 -0.7(4) . . . . no Cl2 C74 C75 C76 -179.2(2) . . . . no C73 C74 C75 C76 0.8(4) . . . . no C74 C75 C76 C77 -0.3(4) . . . . no C75 C76 C77 C78 -0.8(4) . . . . no C76 C77 C78 C73 1.2(4) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl1 C72 3.649(3) . . no Cl1 C10 3.489(3) . . no Cl1 Cl2 3.1516(9) . . no Cl1 C9 3.552(2) . . no Cl2 Cl1 3.1516(9) . . no Cl2 C9 3.644(2) . . no Cl2 C29 3.360(2) . 4_555 no Cl1 H72' 2.71(3) . . no Cl2 H63 2.98(2) . . no Cl2 H68' 3.00(2) . . no Cl2 H65 2.90(2) . 3_656 no O1 C11 3.092(3) . . no O1 C68 3.293(3) . . no O1 C66 3.409(3) . 2_555 no O2 C51 3.225(3) . 1_655 no O2 C56 3.236(3) . 1_655 no O2 C50 3.394(3) . 1_655 no O2 C38 3.197(3) . 4_554 no O2 C57 3.408(3) . 1_655 no O1 H68 2.70(2) . . no O1 H72' 2.75(3) . . no O1 H69 2.69(2) . . no O1 H72 2.50(2) . . no O1 H66 2.52(2) . 2_555 no O1 H75 2.75(2) . 4_454 no C3 C72 3.516(4) . 2_545 no C3 C67 3.313(4) . . no C4 C62 3.410(3) . . no C5 C62 3.405(4) . . no C5 C63 3.530(4) . . no C6 C63 3.135(4) . . no C7 C48 3.360(3) . 4_555 no C9 Cl2 3.644(2) . . no C9 Cl1 3.552(2) . . no C10 C68 3.416(4) . . no C10 Cl1 3.489(3) . . no C11 O1 3.092(3) . . no C11 C68 3.429(4) . . no C12 C69 3.369(4) . . no C16 C58 3.433(4) . 2_445 no C17 C18 3.582(4) . 3_556 no C18 C17 3.582(4) . 3_556 no C20 C72 3.448(4) . 4_455 no C21 C48 3.277(3) . 4_555 no C21 C49 3.359(3) . 4_555 no C23 C42 3.504(4) . 3_566 no C23 C41 3.468(4) . 3_566 no C24 C77 3.495(4) . 3_666 no C29 Cl2 3.360(2) . 4_454 no C32 C60 3.406(4) . 2_445 no C32 C59 3.403(4) . 2_445 no C33 C59 3.171(4) . 2_445 no C34 C58 3.454(4) . 2_445 no C34 C59 3.316(4) . 2_445 no C35 C65 3.392(4) . 3_556 no C35 C64 3.594(4) . 3_556 no C36 C65 3.513(4) . 3_556 no C38 C72 3.363(4) . 4_455 no C38 C71 3.378(3) . 4_455 no C38 O2 3.197(3) . 4_455 no C40 C76 3.483(4) . 1_455 no C41 C23 3.468(4) . 3_566 no C42 C23 3.504(4) . 3_566 no C42 C42 3.554(3) . 3_566 no C43 C70 3.547(4) . 2_555 no C48 C7 3.360(3) . 4_454 no C48 C21 3.277(3) . 4_454 no C49 C21 3.359(3) . 4_454 no C50 O2 3.394(3) . 1_455 no C51 O2 3.225(3) . 1_455 no C52 C65 3.560(4) . 3_556 no C54 C76 3.420(4) . 1_455 no C54 C75 3.485(4) . 1_455 no C54 C77 3.506(4) . 1_455 no C55 C78 3.504(4) . 1_455 no C56 O2 3.236(3) . 1_455 no C57 O2 3.408(3) . 1_455 no C58 C34 3.454(4) . 2_455 no C58 C16 3.433(4) . 2_455 no C59 C34 3.316(4) . 2_455 no C59 C32 3.403(4) . 2_455 no C59 C33 3.171(4) . 2_455 no C60 C32 3.406(4) . 2_455 no C62 C5 3.405(4) . . no C62 C4 3.410(3) . . no C63 C64 3.581(4) . 3_656 no C63 C6 3.135(4) . . no C63 C65 3.523(4) . 3_656 no C63 C5 3.530(4) . . no C64 C35 3.594(4) . 3_556 no C64 C63 3.581(4) . 3_656 no C64 C65 3.594(4) . 3_656 no C64 C64 3.379(4) . 3_656 no C65 C35 3.392(4) . 3_556 no C65 C63 3.523(4) . 3_656 no C65 C36 3.513(4) . 3_556 no C65 C64 3.594(4) . 3_656 no C65 C52 3.560(4) . 3_556 no C66 O1 3.409(3) . 2_545 no C67 C69 3.501(4) . . no C67 C3 3.313(4) . . no C68 C11 3.429(4) . . no C68 O1 3.293(3) . . no C68 C10 3.416(4) . . no C69 C67 3.501(4) . . no C69 C12 3.369(4) . . no C70 C43 3.547(4) . 2_545 no C71 C38 3.378(3) . 4_554 no C72 Cl1 3.649(3) . . no C72 C3 3.516(4) . 2_555 no C72 C38 3.363(4) . 4_554 no C72 C20 3.448(4) . 4_554 no C73 C77 3.420(4) . 3_666 no C75 C54 3.485(4) . 1_655 no C76 C54 3.420(4) . 1_655 no C76 C40 3.483(4) . 1_655 no C77 C24 3.495(4) . 3_666 no C77 C73 3.420(4) . 3_666 no C77 C54 3.506(4) . 1_655 no C78 C55 3.504(4) . 1_655 no C1 H63 2.81(2) . . no C2 H67 3.08(2) . . no C2 H69 2.89(2) . . no C6 H63 2.76(2) . . no C8 H77 2.90(2) . 3_666 no C9 H68 2.56(2) . . no C10 H68 2.63(2) . . no C11 H68 2.81(2) . . no C12 H69 2.71(2) . . no C12 H68 2.91(2) . . no C13 H78 2.75(2) . 2_545 no C14 H78 3.02(2) . 2_545 no C16 H72" 3.07(3) . 2_545 no C24 H77 2.62(2) . 3_666 no C25 H76 3.06(2) . 3_666 no C26 H69' 3.09(2) . 2_555 no C27 H69' 3.09(2) . 2_555 no C28 H66 3.05(2) . 2_555 no C30 H78 2.78(2) . 2_545 no C31 H78 3.08(2) . 2_545 no C37 H72 2.86(2) . 4_455 no C38 H72 2.86(2) . 4_455 no C43 H70' 2.81(2) . 2_555 no C45 H64 2.97(2) . 4_454 no C50 H70 2.90(2) . 1_455 no C51 H70 2.87(2) . 1_455 no C52 H65 2.98(2) . 3_556 no C57 H72" 2.91(3) . 1_455 no C62 H69' 3.047(19) . . no C66 H72 3.09(2) . 2_545 no C67 H69' 2.91(2) . . no C71 H68 2.61(2) . . no H63 Cl2 2.98(2) . . no H63 C1 2.81(2) . . no H63 C6 2.76(2) . . no H64 C45 2.97(2) . 4_555 no H65 Cl2 2.90(2) . 3_656 no H65 C52 2.98(2) . 3_556 no H66 C28 3.05(2) . 2_545 no H66 O1 2.52(2) . 2_545 no H67 C2 3.08(2) . . no H67 H72' 2.56(4) . 2_545 no H68 O1 2.70(2) . . no H68 C9 2.56(2) . . no H68 C10 2.63(2) . . no H68 C11 2.81(2) . . no H68 C12 2.91(2) . . no H68 C71 2.61(2) . . no H68' Cl2 3.00(2) . . no H69 O1 2.69(2) . . no H69 C2 2.89(2) . . no H69 C12 2.71(2) . . no H69 H76 2.48(3) . 4_454 no H69' C27 3.09(2) . 2_545 no H69' C26 3.09(2) . 2_545 no H69' C62 3.047(19) . . no H69' C67 2.91(2) . . no H70 C51 2.87(2) . 1_655 no H70 C50 2.90(2) . 1_655 no H70' C43 2.81(2) . 2_545 no H72 O1 2.50(2) . . no H72 C66 3.09(2) . 2_555 no H72 C37 2.86(2) . 4_554 no H72 C38 2.86(2) . 4_554 no H72' Cl1 2.71(3) . . no H72' H67 2.56(4) . 2_555 no H72' O1 2.75(3) . . no H72" C57 2.91(3) . 1_655 no H72" C16 3.07(3) . 2_555 no H75 O1 2.75(2) . 4_555 no H76 C25 3.06(2) . 3_666 no H76 H69 2.48(3) . 4_555 no H77 C8 2.90(2) . 3_666 no H77 C24 2.62(2) . 3_666 no H78 C13 2.75(2) . 2_555 no H78 C14 3.02(2) . 2_555 no H78 C30 2.78(2) . 2_555 no H78 C31 3.08(2) . 2_555 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C66 H66 O1 1.00(2) 2.52(2) 3.409(3) 148.4(17) 2_545 yes C72 H72' Cl1 1.07(3) 2.71(3) 3.649(3) 147(2) . yes #=============================================================================== data_c150h33c _database_code_CSD 211977 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; Methyl 5-(3'H-cyclopropa[1,9](C60-Ih)[5,6]fullerenyl)-5-phenylpentanoate. ; _chemical_name_common ;Methyl 5-(3'H-cyclopropa(1,9)(C60-Ih)(5,6)fullerenyl)-5- phenylpentanoate. ; _chemical_melting_point ? _chemical_formula_moiety '2(C72 H14 O2), C6 H5 Cl' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C150 H33 Cl O4' _chemical_formula_weight 1934.21 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 13.8333(9) _cell_length_b 15.288(1) _cell_length_c 19.249(1) _cell_angle_alpha 80.259(1) _cell_angle_beta 78.557(1) _cell_angle_gamma 80.406(1) _cell_volume 3894.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 90 _cell_measurement_reflns_used 4343 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 26.52 _cell_special_details ; The final unit cell was obtained from the xyz centroids of 4343 reflections after integration using the SAINT software package (Bruker, 2000). The intensity data were corrected for decay and absorption using SADABS (Sheldrick, 2000). ; _exptl_crystal_description 'triangle platelet' _exptl_crystal_colour reddish _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1964 _exptl_absorpt_coefficient_mu 0.131 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_process_detais 'SADABS (Sheldrick, Bruker, 2000))' _exptl_absorpt_correction_T_min 0.9768 _exptl_absorpt_correction_T_max 0.9870 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine focus sealed Siemens Mo tube ' _diffrn_radiation_monochromator 'parallel mounted graphite' _diffrn_radiation_detector ; CCD area-detector ; _diffrn_measurement_device_type ; Bruker Smart Apex ; _diffrn_measurement_method 'phi and omega scans' _diffrn_special_details ; Crystal into the cold nitrogen stream of the low-temparature unit (KRYOFLEX, (Bruker, 2000)). ; _diffrn_detector_area_resol_mean '4096x4096 / 62x62 (binned 512)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 34221 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0991 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.37 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_reduction_process ; Intensity data were corrected for Lorentz and polarization effects, decay and absorption and reduced to F~o~^2^ using SAINT (Bruker, 2000) and SADABS (Sheldrick, 2001) ; # number of unique reflections _reflns_number_total 15737 _reflns_number_gt 9339 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART, Bruker Version 5.168, 2000' _computing_cell_refinement 'SAINT, Bruker Version 6.02A, 2000' _computing_data_reduction 'XPREP, Bruker Version 5.1/NT, 2000' _computing_structure_solution ; SIR-97 (Altomare et al., 1997) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLUTO (Meetsma, 2000) PLATON (Spek, 1994) ; _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 15737 _refine_ls_number_parameters 1544 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1184 _refine_ls_wR_factor_gt 0.1009 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.340 _refine_ls_shift/su_mean 0.005 _refine_diff_density_max 0.279 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.056 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Cl31 Cl Uani 0.03025(14) 0.30906(12) 0.06906(10) 0.500 0.0660(7) . . C31 C Uani 0.0126(3) 0.4230(2) 0.0280(3) 0.500 0.029(2) . . C32 C Uani 0.0916(3) 0.4723(3) 0.0144(3) 0.500 0.032(3) . . C33 C Uani 0.0803(4) 0.5602(3) -0.0191(3) 0.500 0.042(3) . . C34 C Uani -0.0101(4) 0.5989(3) -0.0389(3) 0.500 0.057(4) . . C35 C Uani -0.0891(4) 0.5497(3) -0.0253(3) 0.500 0.051(3) . . C36 C Uani -0.0777(4) 0.4617(3) 0.0082(3) 0.500 0.036(3) . . H32 H Uiso 0.15346 0.44580 0.02803 0.500 0.0388 . . H33 H Uiso 0.13439 0.59394 -0.02840 0.500 0.0502 . . H34 H Uiso -0.01784 0.65913 -0.06183 0.500 0.0677 . . H35 H Uiso -0.15096 0.57615 -0.03885 0.500 0.0615 . . H36 H Uiso -0.13183 0.42797 0.01753 0.500 0.0428 . . Cl41 Cl Uani 0.18808(10) 0.53356(9) 0.44696(8) 0.500 0.0339(5) . . C41 C Uani 0.0662(2) 0.5176(2) 0.4808(2) 0.500 0.0237(17) . . C42 C Uani -0.0006(3) 0.5200(2) 0.43535(18) 0.500 0.029(2) . . C43 C Uani -0.0983(2) 0.5074(2) 0.4634(2) 0.500 0.039(2) . . C44 C Uiso -0.12932 0.49251 0.53679 0.500(6) 0.0378(2) . . C45 C Uani -0.0626(3) 0.4901(2) 0.58225(19) 0.500 0.034(2) . . C46 C Uani 0.0352(3) 0.5027(2) 0.5543(2) 0.500 0.032(2) . . H42 H Uiso 0.02061 0.53023 0.38497 0.500 0.0346 . . H43 H Uiso -0.14414 0.50910 0.43220 0.500 0.0471 . . H44 H Uiso -0.19637 0.48389 0.55600 0.500 0.0454 . . H45 H Uiso -0.08384 0.47989 0.63264 0.500 0.0411 . . H46 H Uiso 0.08097 0.50102 0.58542 0.500 0.0388 . . O11 O Uani -0.06945(13) 0.54030(12) 0.28514(9) 1.000 0.0314(6) . . O12 O Uani -0.03770(13) 0.52452(11) 0.16877(9) 1.000 0.0293(6) . . C11 C Uani 0.38899(17) 0.37397(15) 0.23324(13) 1.000 0.0186(8) . . C12 C Uani 0.40245(18) 0.26859(15) 0.22321(13) 1.000 0.0182(8) . . C13 C Uani 0.50198(18) 0.23277(15) 0.18481(13) 1.000 0.0201(8) . . C14 C Uani 0.57502(18) 0.28550(15) 0.15284(12) 1.000 0.0184(8) . . C15 C Uani 0.56300(18) 0.38054(15) 0.16272(12) 1.000 0.0188(8) . . C16 C Uani 0.47889(17) 0.41913(15) 0.20382(12) 1.000 0.0176(8) . . C17 C Uani 0.48867(18) 0.47627(15) 0.25336(13) 1.000 0.0199(8) . . C18 C Uani 0.41565(18) 0.45972(15) 0.31769(13) 1.000 0.0194(8) . . C19 C Uani 0.36048(17) 0.39176(15) 0.30885(13) 1.000 0.0195(8) . . C110 C Uani 0.33577(17) 0.32678(16) 0.36604(13) 1.000 0.0198(8) . . C111 C Uani 0.34801(17) 0.23158(16) 0.35662(13) 1.000 0.0203(8) . . C112 C Uani 0.38467(18) 0.20495(15) 0.29060(13) 1.000 0.0201(8) . . C113 C Uani 0.45878(18) 0.12706(15) 0.28462(13) 1.000 0.0198(8) . . C114 C Uani 0.53039(18) 0.14378(15) 0.22010(13) 1.000 0.0201(8) . . C115 C Uani 0.62977(18) 0.10786(16) 0.21822(13) 1.000 0.0221(8) . . C116 C Uani 0.70615(18) 0.16250(16) 0.18365(13) 1.000 0.0219(8) . . C117 C Uani 0.67899(18) 0.25004(16) 0.15251(12) 1.000 0.0211(8) . . C118 C Uani 0.73123(18) 0.32080(16) 0.16072(12) 1.000 0.0218(8) . . C119 C Uani 0.65993(18) 0.40089(16) 0.16764(13) 1.000 0.0210(8) . . C120 C Uani 0.66805(18) 0.45964(16) 0.21371(14) 1.000 0.0231(8) . . C121 C Uani 0.58062(19) 0.49760(15) 0.25769(13) 1.000 0.0212(8) . . C122 C Uani 0.60490(19) 0.50285(15) 0.32665(14) 1.000 0.0242(9) . . C123 C Uani 0.5356(2) 0.48617(15) 0.38813(14) 1.000 0.0243(9) . . C124 C Uani 0.43868(19) 0.46451(15) 0.38419(14) 1.000 0.0233(8) . . C125 C Uani 0.41084(19) 0.39777(16) 0.44420(13) 1.000 0.0244(8) . . C126 C Uani 0.36080(18) 0.33000(16) 0.43523(13) 1.000 0.0226(8) . . C127 C Uani 0.38837(18) 0.23899(17) 0.46785(13) 1.000 0.0239(8) . . C128 C Uani 0.38000(18) 0.17877(16) 0.42011(13) 1.000 0.0219(8) . . C129 C Uani 0.44797(18) 0.10140(15) 0.41402(13) 1.000 0.0223(8) . . C130 C Uani 0.48881(18) 0.07512(15) 0.34499(13) 1.000 0.0211(8) . . C131 C Uani 0.59252(19) 0.03788(15) 0.34349(14) 1.000 0.0225(9) . . C132 C Uani 0.66158(19) 0.05409(15) 0.28162(13) 1.000 0.0226(8) . . C133 C Uani 0.75822(18) 0.07601(16) 0.28558(14) 1.000 0.0233(8) . . C134 C Uani 0.78542(18) 0.14299(16) 0.22495(13) 1.000 0.0240(8) . . C135 C Uani 0.83555(17) 0.21088(17) 0.23313(13) 1.000 0.0243(8) . . C136 C Uani 0.80794(18) 0.30162(17) 0.20043(13) 1.000 0.0240(8) . . C137 C Uani 0.81594(18) 0.36220(17) 0.24886(14) 1.000 0.0251(9) . . C138 C Uani 0.74749(19) 0.43941(16) 0.25544(14) 1.000 0.0253(9) . . C139 C Uani 0.70844(19) 0.46614(16) 0.32519(14) 1.000 0.0254(9) . . C140 C Uani 0.73939(19) 0.41484(16) 0.38561(14) 1.000 0.0253(9) . . C141 C Uani 0.6671(2) 0.39753(16) 0.45013(14) 1.000 0.0257(9) . . C142 C Uani 0.5674(2) 0.43229(16) 0.45160(13) 1.000 0.0248(9) . . C143 C Uani 0.4898(2) 0.37786(16) 0.48614(13) 1.000 0.0255(8) . . C144 C Uani 0.51661(19) 0.29067(17) 0.51760(12) 1.000 0.0244(8) . . C145 C Uani 0.46377(19) 0.22019(16) 0.50882(13) 1.000 0.0236(8) . . C146 C Uani 0.53535(19) 0.13953(16) 0.50255(13) 1.000 0.0229(8) . . C147 C Uani 0.52774(18) 0.08195(15) 0.45604(13) 1.000 0.0221(8) . . C148 C Uani 0.61678(19) 0.04224(15) 0.41259(13) 1.000 0.0220(8) . . C149 C Uani 0.70922(19) 0.06318(15) 0.41685(13) 1.000 0.0228(8) . . C150 C Uani 0.78148(18) 0.08013(15) 0.35203(13) 1.000 0.0223(8) . . C151 C Uani 0.83413(18) 0.15094(16) 0.36049(13) 1.000 0.0223(8) . . C152 C Uani 0.86032(17) 0.21521(17) 0.30238(14) 1.000 0.0240(8) . . C153 C Uani 0.84810(18) 0.30861(17) 0.31220(14) 1.000 0.0254(9) . . C154 C Uani 0.81070(18) 0.33476(17) 0.37872(14) 1.000 0.0256(9) . . C155 C Uani 0.78259(19) 0.26751(17) 0.43975(13) 1.000 0.0238(9) . . C156 C Uani 0.79472(18) 0.17752(16) 0.43072(13) 1.000 0.0215(8) . . C157 C Uani 0.71755(18) 0.12350(15) 0.46531(13) 1.000 0.0210(8) . . C158 C Uani 0.63202(19) 0.16088(16) 0.50681(12) 1.000 0.0216(8) . . C159 C Uani 0.61981(19) 0.25444(17) 0.51636(13) 1.000 0.0244(9) . . C160 C Uani 0.6937(2) 0.30656(16) 0.48361(13) 1.000 0.0241(8) . . C161 C Uani 0.32667(18) 0.33907(15) 0.19135(13) 1.000 0.0195(8) . . C162 C Uani 0.34298(17) 0.36102(15) 0.11100(13) 1.000 0.0198(8) . . C163 C Uani 0.33142(19) 0.29660(17) 0.07118(14) 1.000 0.0230(8) . . C164 C Uani 0.33906(19) 0.31543(17) -0.00226(14) 1.000 0.0266(9) . . C165 C Uani 0.36056(19) 0.39861(17) -0.03763(14) 1.000 0.0262(9) . . C166 C Uani 0.37235(19) 0.46310(17) 0.00123(14) 1.000 0.0256(9) . . C167 C Uani 0.36291(18) 0.44475(16) 0.07529(14) 1.000 0.0221(8) . . C168 C Uani 0.21763(19) 0.33415(17) 0.22466(15) 1.000 0.0223(8) . . C169 C Uani 0.15245(19) 0.42508(17) 0.21640(15) 1.000 0.0229(8) . . C170 C Uani 0.0438(2) 0.41329(18) 0.24489(17) 1.000 0.0295(9) . . C171 C Uani -0.02695(18) 0.49910(17) 0.23678(14) 1.000 0.0233(9) . . C172 C Uani -0.1092(2) 0.60340(19) 0.15503(17) 1.000 0.0310(10) . . H163 H Uiso 0.31701 0.23793 0.09397 1.00(3) 0.0232(16) . . H164 H Uiso 0.33184 0.26880 -0.02999 1.00(4) 0.0280(17) . . H165 H Uiso 0.36295 0.41323 -0.09044 1.00(3) 0.0169(16) . . H166 H Uiso 0.38837 0.52291 -0.02426 1.00(3) 0.0300(17) . . H167 H Uiso 0.37090 0.49306 0.10292 1.00(3) 0.0247(16) . . H168 H Uiso 0.21331 0.31267 0.27515 1.00(3) 0.0289(17) . . H168' H Uiso 0.18943 0.29509 0.19976 1.00(4) 0.0246(17) . . H169 H Uiso 0.17473 0.46564 0.24416 1.00(4) 0.0226(16) . . H169' H Uiso 0.15710 0.45225 0.16444 1.00(3) 0.0284(17) . . H170 H Uiso 0.02619 0.36738 0.21612 1.00(4) 0.048(2) . . H170' H Uiso 0.03803 0.39044 0.29659 1.00(4) 0.0463(19) . . H172 H Uiso -0.10189 0.65552 0.18418 1.00(5) 0.062(2) . . H172' H Uiso -0.09360 0.62155 0.09795 1.00(5) 0.090(2) . . H172" H Uiso -0.17858 0.59100 0.17574 1.00(5) 0.072(2) . . O21 O Uani -0.31589(15) 0.70087(13) 0.21471(11) 1.000 0.0442(8) . . O22 O Uani -0.28656(16) 0.83984(14) 0.21476(11) 1.000 0.0481(8) . . C21 C Uani 0.00301(18) 0.79062(15) 0.31163(13) 1.000 0.0193(8) . . C22 C Uani -0.01259(18) 0.89795(15) 0.31377(13) 1.000 0.0189(8) . . C23 C Uani 0.07022(18) 0.93114(15) 0.33542(12) 1.000 0.0187(8) . . C24 C Uani 0.14935(18) 0.87591(16) 0.36022(12) 1.000 0.0202(8) . . C25 C Uani 0.16353(18) 0.77881(16) 0.35806(12) 1.000 0.0201(8) . . C26 C Uani 0.09770(18) 0.74087(15) 0.33123(12) 1.000 0.0193(8) . . C27 C Uani 0.13564(18) 0.67550(15) 0.28285(13) 1.000 0.0197(8) . . C28 C Uani 0.07511(18) 0.69044(15) 0.22775(13) 1.000 0.0197(8) . . C29 C Uani -0.00125(17) 0.76535(15) 0.24103(13) 1.000 0.0189(8) . . C210 C Uani -0.02706(17) 0.82539(15) 0.18359(13) 1.000 0.0187(8) . . C211 C Uani -0.04109(17) 0.92282(15) 0.18561(13) 1.000 0.0189(8) . . C212 C Uani -0.02822(17) 0.95546(15) 0.24532(13) 1.000 0.0189(8) . . C213 C Uani 0.02698(17) 1.03007(15) 0.23592(13) 1.000 0.0200(8) . . C214 C Uani 0.08710(18) 1.01517(15) 0.29085(13) 1.000 0.0204(8) . . C215 C Uani 0.17994(19) 1.04434(16) 0.27655(13) 1.000 0.0226(8) . . C216 C Uani 0.26234(19) 0.98676(16) 0.30363(13) 1.000 0.0222(8) . . C217 C Uani 0.24711(18) 0.90434(17) 0.34365(13) 1.000 0.0219(8) . . C218 C Uani 0.32089(19) 0.82697(16) 0.33168(13) 1.000 0.0228(8) . . C219 C Uani 0.26966(18) 0.74981(16) 0.33971(13) 1.000 0.0213(8) . . C220 C Uani 0.30583(18) 0.68378(15) 0.29666(13) 1.000 0.0216(8) . . C221 C Uani 0.23717(18) 0.64556(15) 0.26673(13) 1.000 0.0211(8) . . C222 C Uani 0.28138(18) 0.63017(15) 0.19474(14) 1.000 0.0219(8) . . C223 C Uani 0.22402(18) 0.64432(15) 0.14141(14) 1.000 0.0223(8) . . C224 C Uani 0.11813(18) 0.67497(15) 0.15841(13) 1.000 0.0213(8) . . C225 C Uani 0.08879(18) 0.73663(16) 0.09857(13) 1.000 0.0209(8) . . C226 C Uani 0.01834(17) 0.81095(16) 0.11122(13) 1.000 0.0187(8) . . C227 C Uani 0.03276(18) 0.89738(16) 0.06899(13) 1.000 0.0202(8) . . C228 C Uani -0.00363(17) 0.96536(16) 0.11521(13) 1.000 0.0213(8) . . C229 C Uani 0.04573(17) 1.04031(15) 0.10616(13) 1.000 0.0203(8) . . C230 C Uani 0.06127(18) 1.07361(15) 0.16809(13) 1.000 0.0198(8) . . C231 C Uani 0.15849(18) 1.10313(15) 0.15230(13) 1.000 0.0207(8) . . C232 C Uani 0.21682(18) 1.08860(15) 0.20565(13) 1.000 0.0213(8) . . C233 C Uani 0.32246(18) 1.05812(15) 0.18845(13) 1.000 0.0208(8) . . C234 C Uani 0.35038(18) 0.99516(16) 0.24912(13) 1.000 0.0212(8) . . C235 C Uani 0.42113(18) 0.92132(16) 0.23785(13) 1.000 0.0222(8) . . C236 C Uani 0.40666(18) 0.83477(16) 0.28001(13) 1.000 0.0222(8) . . C237 C Uani 0.44322(18) 0.76649(16) 0.23411(14) 1.000 0.0237(8) . . C238 C Uani 0.39391(17) 0.69226(15) 0.24198(13) 1.000 0.0213(8) . . C239 C Uani 0.37864(18) 0.65923(15) 0.17925(14) 1.000 0.0242(8) . . C240 C Uani 0.41415(18) 0.70126(16) 0.11093(14) 1.000 0.0233(8) . . C241 C Uani 0.35385(18) 0.71579(16) 0.05568(14) 1.000 0.0242(8) . . C242 C Uani 0.26036(19) 0.68794(16) 0.07023(13) 1.000 0.0221(8) . . C243 C Uani 0.17707(19) 0.74532(16) 0.04393(13) 1.000 0.0229(8) . . C244 C Uani 0.19045(18) 0.82792(17) 0.00400(12) 1.000 0.0220(8) . . C245 C Uani 0.11691(18) 0.90534(16) 0.01644(13) 1.000 0.0220(8) . . C246 C Uani 0.16854(18) 0.98263(16) 0.00774(13) 1.000 0.0226(8) . . C247 C Uani 0.13402(18) 1.04865(15) 0.05133(13) 1.000 0.0211(8) . . C248 C Uani 0.20335(18) 1.08777(15) 0.08032(13) 1.000 0.0218(8) . . C249 C Uani 0.30518(18) 1.05865(15) 0.06360(13) 1.000 0.0206(8) . . C250 C Uani 0.36604(18) 1.04371(15) 0.11914(13) 1.000 0.0214(8) . . C251 C Uani 0.43937(17) 0.96611(15) 0.10734(13) 1.000 0.0207(8) . . C252 C Uani 0.46640(17) 0.90625(16) 0.16576(14) 1.000 0.0223(8) . . C253 C Uani 0.47972(17) 0.81028(16) 0.16328(14) 1.000 0.0238(8) . . C254 C Uani 0.46565(17) 0.77843(16) 0.10321(14) 1.000 0.0233(8) . . C255 C Uani 0.43727(18) 0.84105(16) 0.04267(13) 1.000 0.0225(8) . . C256 C Uani 0.42428(18) 0.93248(16) 0.04463(13) 1.000 0.0222(8) . . C257 C Uani 0.34148(18) 0.98984(16) 0.01792(13) 1.000 0.0222(8) . . C258 C Uani 0.27405(19) 0.95297(16) -0.00927(12) 1.000 0.0223(8) . . C259 C Uani 0.28817(19) 0.85736(17) -0.01205(13) 1.000 0.0244(9) . . C260 C Uani 0.36760(18) 0.80271(16) 0.01333(13) 1.000 0.0230(8) . . C261 C Uani -0.08286(18) 0.83616(15) 0.36084(13) 1.000 0.0201(8) . . C262 C Uani -0.07994(18) 0.82421(16) 0.43985(13) 1.000 0.0220(8) . . C263 C Uani -0.0696(2) 0.74017(18) 0.48030(14) 1.000 0.0285(9) . . C264 C Uani -0.0722(2) 0.73236(19) 0.55345(15) 1.000 0.0355(10) . . C265 C Uani -0.0833(2) 0.80724(19) 0.58634(15) 1.000 0.0326(10) . . C266 C Uani -0.0932(2) 0.89159(19) 0.54651(15) 1.000 0.0313(10) . . C267 C Uani -0.09206(19) 0.89978(17) 0.47363(14) 1.000 0.0258(9) . . C268 C Uani -0.18618(19) 0.84078(16) 0.34212(15) 1.000 0.0233(8) . . C269 C Uani -0.2218(2) 0.74896(17) 0.35360(15) 1.000 0.0249(8) . . C270 C Uani -0.3207(2) 0.75252(19) 0.32677(14) 1.000 0.0258(9) . . C271 C Uani -0.30842(19) 0.75956(19) 0.24708(15) 1.000 0.0295(9) . . C272 C Uani -0.2638(3) 0.8501(3) 0.13676(18) 1.000 0.0646(14) . . H263 H Uiso -0.06359 0.68799 0.45711 1.00(3) 0.0254(16) . . H264 H Uiso -0.06455 0.67561 0.58111 1.00(4) 0.0327(18) . . H265 H Uiso -0.08292 0.80469 0.63621 1.00(3) 0.0279(17) . . H266 H Uiso -0.09944 0.94586 0.56869 1.00(4) 0.0400(18) . . H267 H Uiso -0.09439 0.96116 0.44495 1.00(3) 0.0294(17) . . H268 H Uiso -0.23547 0.88214 0.37512 1.00(3) 0.0240(17) . . H268' H Uiso -0.18655 0.87075 0.29074 1.00(3) 0.0225(16) . . H269 H Uiso -0.22863 0.72578 0.40698 1.00(3) 0.0309(17) . . H269' H Uiso -0.16746 0.70222 0.32774 1.00(4) 0.055(2) . . H270 H Uiso -0.36996 0.80660 0.34140 1.00(3) 0.0299(18) . . H270' H Uiso -0.34413 0.69461 0.34572 1.00(4) 0.0351(18) . . H272 H Uiso -0.32454 0.84719 0.11987 1.00(5) 0.060(2) . . H272' H Uiso -0.24401 0.91235 0.12077 1.00(6) 0.101(3) . . H272" H Uiso -0.20599 0.80219 0.11951 1.00(6) 0.139(3) . . 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 O11 0.0325(11) 0.0352(11) 0.0262(11) -0.0065(9) -0.0028(9) -0.0048(9) O12 0.0304(11) 0.0294(10) 0.0263(11) -0.0028(8) -0.0050(9) 0.0000(8) C11 0.0178(14) 0.0162(12) 0.0208(14) -0.0008(10) -0.0032(11) -0.0014(10) C12 0.0215(14) 0.0171(12) 0.0181(14) -0.0018(10) -0.0067(11) -0.0057(10) C13 0.0259(15) 0.0220(13) 0.0152(14) -0.0051(11) -0.0099(12) -0.0009(11) C14 0.0230(14) 0.0226(13) 0.0107(13) -0.0029(10) -0.0059(11) -0.0022(11) C15 0.0216(14) 0.0206(13) 0.0132(13) 0.0035(10) -0.0055(11) -0.0035(11) C16 0.0197(14) 0.0157(12) 0.0178(14) 0.0041(10) -0.0090(11) -0.0034(10) C17 0.0243(14) 0.0122(12) 0.0215(14) 0.0019(10) -0.0068(12) 0.0012(10) C18 0.0203(14) 0.0145(12) 0.0219(14) -0.0049(10) -0.0046(11) 0.0054(10) C19 0.0172(13) 0.0178(13) 0.0216(14) -0.0024(11) -0.0031(11) 0.0022(10) C110 0.0132(13) 0.0240(14) 0.0203(14) -0.0008(11) -0.0004(11) -0.0025(10) C111 0.0146(13) 0.0236(14) 0.0222(15) 0.0029(11) -0.0027(11) -0.0079(11) C112 0.0217(14) 0.0181(13) 0.0237(15) -0.0005(11) -0.0081(12) -0.0091(11) C113 0.0232(14) 0.0154(12) 0.0249(15) -0.0044(11) -0.0089(12) -0.0075(11) C114 0.0257(15) 0.0175(13) 0.0209(14) -0.0076(11) -0.0096(12) -0.0024(11) C115 0.0269(15) 0.0207(13) 0.0218(15) -0.0143(11) -0.0066(12) 0.0022(11) C116 0.0252(15) 0.0240(14) 0.0159(14) -0.0099(11) -0.0012(11) 0.0026(11) C117 0.0212(14) 0.0293(14) 0.0106(13) -0.0029(11) -0.0003(11) 0.0002(11) C118 0.0219(14) 0.0277(14) 0.0121(13) 0.0012(11) 0.0027(11) -0.0034(11) C119 0.0183(14) 0.0236(14) 0.0187(14) 0.0074(11) -0.0025(11) -0.0074(11) C120 0.0232(15) 0.0194(13) 0.0261(15) 0.0075(11) -0.0058(12) -0.0107(11) C121 0.0288(15) 0.0108(12) 0.0249(15) 0.0053(11) -0.0098(12) -0.0070(11) C122 0.0333(16) 0.0117(12) 0.0313(16) -0.0035(11) -0.0116(13) -0.0057(11) C123 0.0380(17) 0.0123(12) 0.0258(16) -0.0084(11) -0.0091(13) -0.0024(12) C124 0.0270(15) 0.0144(13) 0.0264(15) -0.0069(11) -0.0026(12) 0.0043(11) C125 0.0297(16) 0.0240(14) 0.0177(14) -0.0088(11) -0.0006(12) 0.0027(12) C126 0.0200(14) 0.0272(14) 0.0163(14) -0.0054(11) 0.0033(11) 0.0034(11) C127 0.0199(14) 0.0299(15) 0.0176(14) 0.0005(11) 0.0051(11) -0.0055(11) C128 0.0172(14) 0.0262(14) 0.0206(14) 0.0040(11) 0.0009(11) -0.0105(11) C129 0.0252(15) 0.0153(13) 0.0257(15) 0.0074(11) -0.0061(12) -0.0097(11) C130 0.0271(15) 0.0127(12) 0.0262(15) 0.0011(11) -0.0084(12) -0.0096(11) C131 0.0306(16) 0.0086(12) 0.0291(16) -0.0004(11) -0.0097(13) -0.0015(11) C132 0.0306(16) 0.0138(12) 0.0253(15) -0.0068(11) -0.0094(12) 0.0014(11) C133 0.0248(15) 0.0184(13) 0.0249(15) -0.0049(11) -0.0054(12) 0.0051(11) C134 0.0186(14) 0.0276(14) 0.0228(15) -0.0063(12) -0.0006(12) 0.0041(11) C135 0.0118(13) 0.0358(16) 0.0218(15) -0.0027(12) 0.0003(11) 0.0013(11) C136 0.0158(14) 0.0331(15) 0.0193(14) 0.0015(12) 0.0015(11) -0.0036(12) C137 0.0160(14) 0.0341(15) 0.0254(16) 0.0045(12) -0.0051(12) -0.0113(12) C138 0.0237(15) 0.0254(14) 0.0282(16) 0.0077(12) -0.0055(12) -0.0175(12) C139 0.0310(16) 0.0171(13) 0.0331(17) -0.0009(12) -0.0124(13) -0.0118(12) C140 0.0294(16) 0.0227(14) 0.0307(16) -0.0064(12) -0.0127(13) -0.0116(12) C141 0.0355(17) 0.0252(14) 0.0227(15) -0.0083(12) -0.0124(13) -0.0084(12) C142 0.0353(16) 0.0225(14) 0.0218(15) -0.0127(12) -0.0101(13) -0.0032(12) C143 0.0342(16) 0.0250(14) 0.0180(14) -0.0106(11) -0.0041(12) 0.0011(12) C144 0.0331(16) 0.0302(15) 0.0097(13) -0.0063(11) -0.0014(12) -0.0030(12) C145 0.0284(15) 0.0284(14) 0.0107(13) 0.0021(11) 0.0008(12) -0.0041(12) C146 0.0259(15) 0.0237(14) 0.0160(14) 0.0060(11) -0.0014(12) -0.0065(12) C147 0.0269(15) 0.0176(13) 0.0205(14) 0.0086(11) -0.0043(12) -0.0107(11) C148 0.0297(15) 0.0133(12) 0.0228(15) 0.0040(11) -0.0089(12) -0.0039(11) C149 0.0286(15) 0.0153(13) 0.0229(15) 0.0019(11) -0.0093(12) 0.0026(11) C150 0.0203(14) 0.0187(13) 0.0269(16) -0.0023(11) -0.0089(12) 0.0047(11) C151 0.0180(14) 0.0245(14) 0.0236(15) -0.0011(12) -0.0081(12) 0.0027(11) C152 0.0109(13) 0.0323(15) 0.0277(16) -0.0003(12) -0.0052(12) -0.0018(11) C153 0.0147(14) 0.0309(15) 0.0323(17) 0.0027(12) -0.0086(12) -0.0100(11) C154 0.0228(15) 0.0301(15) 0.0286(16) -0.0005(12) -0.0117(12) -0.0118(12) C155 0.0248(15) 0.0295(15) 0.0222(15) 0.0003(12) -0.0155(12) -0.0083(12) C156 0.0206(14) 0.0253(14) 0.0206(14) 0.0005(11) -0.0121(12) -0.0021(11) C157 0.0253(15) 0.0203(13) 0.0177(14) 0.0024(11) -0.0098(12) -0.0022(11) C158 0.0310(16) 0.0229(14) 0.0108(13) 0.0046(11) -0.0083(12) -0.0052(12) C159 0.0335(16) 0.0291(15) 0.0119(14) -0.0019(11) -0.0092(12) -0.0031(12) C160 0.0359(16) 0.0258(14) 0.0163(14) -0.0055(11) -0.0136(12) -0.0070(12) C161 0.0185(14) 0.0182(13) 0.0229(14) 0.0004(11) -0.0067(11) -0.0051(10) C162 0.0152(13) 0.0205(13) 0.0236(15) -0.0044(11) -0.0055(11) 0.0020(10) C163 0.0226(15) 0.0202(14) 0.0256(15) 0.0005(12) -0.0065(12) -0.0020(11) C164 0.0260(15) 0.0266(15) 0.0273(16) -0.0071(12) -0.0077(12) 0.0033(12) C165 0.0278(16) 0.0309(15) 0.0156(14) 0.0017(12) -0.0046(12) 0.0038(12) C166 0.0272(15) 0.0232(14) 0.0236(16) 0.0038(12) -0.0052(12) -0.0020(12) C167 0.0206(14) 0.0222(14) 0.0236(15) -0.0045(12) -0.0064(12) 0.0011(11) C168 0.0203(14) 0.0222(13) 0.0254(16) 0.0009(12) -0.0081(12) -0.0054(11) C169 0.0199(14) 0.0256(14) 0.0231(15) 0.0004(12) -0.0029(12) -0.0077(11) C170 0.0194(15) 0.0300(15) 0.0347(18) 0.0029(13) -0.0016(13) -0.0018(12) C171 0.0189(14) 0.0283(15) 0.0245(16) 0.0008(12) -0.0030(12) -0.0135(12) C172 0.0291(17) 0.0300(16) 0.0330(18) -0.0024(13) -0.0102(14) 0.0025(13) O21 0.0448(13) 0.0497(13) 0.0397(13) -0.0169(11) -0.0121(10) 0.0057(10) O22 0.0570(15) 0.0604(14) 0.0327(12) 0.0147(11) -0.0178(11) -0.0343(12) C21 0.0208(14) 0.0192(13) 0.0176(14) -0.0018(11) -0.0008(11) -0.0055(11) C22 0.0214(14) 0.0176(13) 0.0166(14) -0.0048(10) -0.0025(11) 0.0019(10) C23 0.0236(14) 0.0193(13) 0.0125(13) -0.0082(10) 0.0022(11) -0.0016(11) C24 0.0254(15) 0.0267(14) 0.0090(13) -0.0051(10) 0.0003(11) -0.0061(11) C25 0.0261(15) 0.0222(13) 0.0115(13) 0.0022(10) -0.0046(11) -0.0047(11) C26 0.0240(14) 0.0168(12) 0.0154(14) 0.0025(10) -0.0017(11) -0.0050(11) C27 0.0217(14) 0.0154(12) 0.0213(14) 0.0030(10) -0.0033(11) -0.0072(11) C28 0.0231(14) 0.0136(12) 0.0235(15) 0.0001(11) -0.0040(12) -0.0087(11) C29 0.0140(13) 0.0199(13) 0.0230(15) -0.0006(11) -0.0017(11) -0.0076(10) C210 0.0143(13) 0.0235(14) 0.0196(14) -0.0015(11) -0.0040(11) -0.0063(11) C211 0.0140(13) 0.0228(13) 0.0192(14) -0.0010(11) -0.0053(11) 0.0002(10) C212 0.0126(13) 0.0170(13) 0.0246(15) -0.0021(11) -0.0015(11) 0.0024(10) C213 0.0182(14) 0.0166(13) 0.0225(14) -0.0056(11) -0.0006(11) 0.0048(10) C214 0.0252(14) 0.0170(13) 0.0197(14) -0.0080(11) -0.0025(12) -0.0011(11) C215 0.0312(16) 0.0184(13) 0.0221(15) -0.0111(11) -0.0044(12) -0.0061(12) C216 0.0279(15) 0.0223(14) 0.0216(15) -0.0090(11) -0.0081(12) -0.0079(12) C217 0.0256(15) 0.0311(15) 0.0127(14) -0.0039(11) -0.0084(11) -0.0072(12) C218 0.0256(15) 0.0302(15) 0.0163(14) -0.0013(11) -0.0129(12) -0.0055(12) C219 0.0245(14) 0.0213(13) 0.0169(14) 0.0064(11) -0.0098(12) -0.0014(11) C220 0.0204(14) 0.0198(13) 0.0224(15) 0.0065(11) -0.0082(12) -0.0012(11) C221 0.0238(15) 0.0117(12) 0.0248(15) 0.0040(11) -0.0041(12) -0.0009(11) C222 0.0245(15) 0.0126(12) 0.0272(15) -0.0024(11) -0.0027(12) -0.0012(11) C223 0.0246(15) 0.0147(12) 0.0288(16) -0.0109(11) 0.0007(12) -0.0047(11) C224 0.0264(15) 0.0165(13) 0.0240(15) -0.0062(11) -0.0035(12) -0.0092(11) C225 0.0225(14) 0.0261(14) 0.0206(14) -0.0101(11) -0.0058(12) -0.0123(11) C226 0.0180(14) 0.0256(14) 0.0164(14) -0.0054(11) -0.0054(11) -0.0084(11) C227 0.0194(14) 0.0251(14) 0.0191(14) 0.0004(11) -0.0113(11) -0.0053(11) C228 0.0150(13) 0.0260(14) 0.0228(15) 0.0009(11) -0.0087(11) -0.0003(11) C229 0.0186(14) 0.0199(13) 0.0202(14) 0.0030(11) -0.0075(11) 0.0023(11) C230 0.0214(14) 0.0123(12) 0.0227(15) 0.0005(10) -0.0031(11) 0.0019(10) C231 0.0271(15) 0.0102(12) 0.0234(15) 0.0020(10) -0.0044(12) -0.0033(10) C232 0.0272(15) 0.0132(12) 0.0261(15) -0.0072(11) -0.0055(12) -0.0049(11) C233 0.0237(14) 0.0161(13) 0.0257(15) -0.0036(11) -0.0065(12) -0.0083(11) C234 0.0201(14) 0.0242(14) 0.0248(15) -0.0080(11) -0.0074(12) -0.0099(11) C235 0.0179(14) 0.0256(14) 0.0272(16) -0.0047(12) -0.0103(12) -0.0064(11) C236 0.0193(14) 0.0265(14) 0.0235(15) 0.0002(12) -0.0137(12) -0.0023(11) C237 0.0167(14) 0.0262(14) 0.0269(16) 0.0036(12) -0.0110(12) 0.0020(11) C238 0.0167(14) 0.0179(13) 0.0255(15) 0.0015(11) -0.0047(12) 0.0050(11) C239 0.0213(14) 0.0154(13) 0.0320(16) -0.0052(12) -0.0018(12) 0.0066(11) C240 0.0190(14) 0.0189(13) 0.0300(16) -0.0096(12) 0.0010(12) 0.0031(11) C241 0.0236(15) 0.0235(14) 0.0250(15) -0.0115(12) 0.0032(12) -0.0025(12) C242 0.0263(15) 0.0209(13) 0.0210(15) -0.0117(11) -0.0002(12) -0.0041(11) C243 0.0276(15) 0.0275(14) 0.0190(14) -0.0121(12) -0.0050(12) -0.0087(12) C244 0.0265(15) 0.0343(15) 0.0085(13) -0.0061(11) -0.0034(11) -0.0104(12) C245 0.0269(15) 0.0308(15) 0.0122(14) 0.0004(11) -0.0098(12) -0.0109(12) C246 0.0245(15) 0.0275(14) 0.0159(14) 0.0051(11) -0.0083(12) -0.0065(12) C247 0.0238(14) 0.0193(13) 0.0183(14) 0.0069(11) -0.0087(12) -0.0011(11) C248 0.0249(15) 0.0151(12) 0.0240(15) 0.0039(11) -0.0056(12) -0.0038(11) C249 0.0260(15) 0.0163(13) 0.0190(14) 0.0051(11) -0.0025(12) -0.0107(11) C250 0.0237(15) 0.0165(13) 0.0262(15) 0.0015(11) -0.0046(12) -0.0129(11) C251 0.0160(14) 0.0209(13) 0.0251(15) -0.0004(11) -0.0009(11) -0.0088(11) C252 0.0128(13) 0.0279(14) 0.0279(16) -0.0029(12) -0.0042(12) -0.0075(11) C253 0.0120(13) 0.0249(14) 0.0330(16) 0.0001(12) -0.0051(12) -0.0013(11) C254 0.0128(13) 0.0256(14) 0.0280(16) -0.0040(12) 0.0019(12) 0.0012(11) C255 0.0162(14) 0.0274(14) 0.0199(14) -0.0022(11) 0.0056(11) -0.0034(11) C256 0.0180(14) 0.0271(14) 0.0190(14) 0.0002(11) 0.0039(11) -0.0079(11) C257 0.0236(15) 0.0242(14) 0.0163(14) 0.0033(11) 0.0022(11) -0.0093(11) C258 0.0277(15) 0.0303(14) 0.0067(13) 0.0019(11) 0.0010(11) -0.0067(12) C259 0.0284(16) 0.0344(15) 0.0107(14) -0.0072(11) 0.0016(12) -0.0074(12) C260 0.0235(15) 0.0240(14) 0.0209(15) -0.0099(11) 0.0043(12) -0.0047(11) C261 0.0213(14) 0.0186(13) 0.0184(14) -0.0023(11) 0.0011(11) -0.0029(11) C262 0.0181(14) 0.0284(14) 0.0174(14) -0.0038(11) 0.0025(11) -0.0037(11) C263 0.0370(17) 0.0251(15) 0.0233(16) -0.0036(12) -0.0005(13) -0.0094(12) C264 0.050(2) 0.0283(16) 0.0246(17) 0.0068(13) -0.0047(14) -0.0080(14) C265 0.0385(18) 0.0435(18) 0.0162(15) -0.0044(13) -0.0028(13) -0.0089(14) C266 0.0334(17) 0.0356(17) 0.0243(16) -0.0087(13) -0.0004(13) -0.0043(13) C267 0.0307(16) 0.0232(14) 0.0202(15) -0.0012(12) -0.0020(12) 0.0008(12) C268 0.0208(14) 0.0220(14) 0.0245(15) -0.0022(12) -0.0014(12) -0.0001(11) C269 0.0237(15) 0.0267(14) 0.0232(15) 0.0000(12) -0.0029(12) -0.0052(12) C270 0.0221(15) 0.0292(15) 0.0257(16) -0.0013(12) -0.0024(12) -0.0073(12) C271 0.0174(15) 0.0402(17) 0.0313(17) -0.0067(14) -0.0025(12) -0.0058(12) C272 0.047(2) 0.119(3) 0.028(2) 0.034(2) -0.0193(17) -0.042(2) Cl31 0.0674(13) 0.0598(12) 0.0579(12) -0.0035(10) 0.0061(10) 0.0028(10) C31 0.036(5) 0.028(3) 0.023(4) -0.013(3) 0.004(4) -0.002(3) C32 0.017(5) 0.046(4) 0.035(5) -0.014(4) -0.003(4) -0.001(3) C33 0.053(7) 0.048(4) 0.029(5) -0.013(4) -0.003(4) -0.019(4) C34 0.085(9) 0.037(4) 0.040(5) 0.006(4) -0.006(5) -0.003(4) C35 0.068(8) 0.050(4) 0.033(5) -0.005(4) -0.008(5) -0.003(4) C36 0.024(5) 0.049(4) 0.038(5) -0.017(4) 0.001(4) -0.013(4) Cl41 0.0262(8) 0.0371(8) 0.0365(9) -0.0021(7) -0.0029(7) -0.0054(6) C41 0.028(3) 0.014(3) 0.028(3) -0.006(2) -0.004(3) 0.002(2) C42 0.043(4) 0.021(3) 0.022(4) -0.012(3) -0.007(3) 0.008(4) C43 0.039(4) 0.021(3) 0.068(5) -0.012(3) -0.032(4) -0.001(3) C45 0.054(4) 0.015(3) 0.030(4) -0.010(3) 0.007(3) -0.004(3) C46 0.052(5) 0.016(3) 0.032(4) -0.001(3) -0.018(4) -0.003(4) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl31 C31 1.785(4) . . yes Cl41 C41 1.725(3) . . yes O11 C171 1.211(3) . . yes O12 C172 1.449(3) . . yes O12 C171 1.331(3) . . yes O21 C271 1.204(3) . . yes O22 C272 1.458(4) . . yes O22 C271 1.332(4) . . yes C11 C161 1.501(3) . . no C11 C12 1.630(3) . . no C11 C16 1.489(3) . . no C11 C19 1.489(3) . . no C12 C161 1.514(3) . . no C12 C13 1.491(4) . . no C12 C112 1.489(3) . . no C13 C114 1.443(3) . . no C13 C14 1.381(3) . . no C14 C117 1.449(4) . . no C14 C15 1.475(3) . . no C15 C119 1.450(4) . . no C15 C16 1.375(3) . . no C16 C17 1.436(3) . . no C17 C18 1.449(3) . . no C17 C121 1.386(4) . . no C18 C19 1.438(3) . . no C18 C124 1.395(4) . . no C19 C110 1.382(3) . . no C110 C126 1.452(3) . . no C110 C111 1.475(3) . . no C111 C112 1.374(3) . . no C111 C128 1.450(3) . . no C112 C113 1.440(3) . . no C113 C114 1.441(3) . . no C113 C130 1.387(3) . . no C114 C115 1.389(4) . . no C115 C132 1.453(3) . . no C115 C116 1.444(4) . . no C116 C134 1.442(4) . . no C116 C117 1.393(3) . . no C117 C118 1.443(4) . . no C118 C119 1.446(3) . . no C118 C136 1.392(4) . . no C119 C120 1.396(4) . . no C120 C138 1.450(4) . . no C120 C121 1.429(4) . . no C121 C122 1.450(4) . . no C122 C139 1.445(4) . . no C122 C123 1.383(4) . . no C123 C142 1.455(4) . . no C123 C124 1.453(4) . . no C124 C125 1.442(4) . . no C125 C126 1.389(4) . . no C125 C143 1.447(4) . . no C126 C127 1.448(4) . . no C127 C128 1.439(4) . . no C127 C145 1.394(4) . . no C128 C129 1.389(3) . . no C129 C147 1.457(4) . . no C129 C130 1.433(3) . . no C130 C131 1.449(4) . . no C131 C148 1.449(4) . . no C131 C132 1.386(4) . . no C132 C133 1.450(4) . . no C133 C134 1.450(4) . . no C133 C150 1.393(4) . . no C134 C135 1.386(4) . . no C135 C152 1.455(4) . . no C135 C136 1.446(4) . . no C136 C137 1.451(4) . . no C137 C138 1.392(4) . . no C137 C153 1.453(4) . . no C138 C139 1.444(4) . . no C139 C140 1.389(4) . . no C140 C154 1.446(4) . . no C140 C141 1.448(4) . . no C141 C160 1.451(3) . . no C141 C142 1.389(4) . . no C142 C143 1.454(4) . . no C143 C144 1.390(4) . . no C144 C159 1.440(4) . . no C144 C145 1.448(4) . . no C145 C146 1.453(4) . . no C146 C158 1.449(4) . . no C146 C147 1.387(3) . . no C147 C148 1.449(4) . . no C148 C149 1.390(4) . . no C149 C150 1.451(4) . . no C149 C157 1.450(3) . . no C150 C151 1.449(3) . . no C151 C156 1.452(3) . . no C151 C152 1.391(4) . . no C152 C153 1.450(4) . . no C153 C154 1.381(4) . . no C154 C155 1.460(4) . . no C155 C156 1.394(4) . . no C155 C160 1.447(4) . . no C156 C157 1.446(4) . . no C157 C158 1.385(4) . . no C158 C159 1.451(4) . . no C159 C160 1.387(4) . . no C161 C162 1.506(3) . . no C161 C168 1.526(4) . . no C162 C163 1.393(4) . . no C162 C167 1.390(3) . . no C163 C164 1.380(4) . . no C164 C165 1.386(4) . . no C165 C166 1.382(4) . . no C166 C167 1.390(4) . . no C168 C169 1.528(4) . . no C169 C170 1.524(4) . . no C170 C171 1.506(4) . . no C21 C26 1.484(4) . . no C21 C22 1.625(3) . . no C21 C29 1.489(3) . . no C21 C261 1.515(3) . . no C22 C23 1.483(4) . . no C22 C261 1.525(3) . . no C22 C212 1.488(3) . . no C23 C214 1.445(3) . . no C23 C24 1.379(3) . . no C24 C217 1.448(4) . . no C24 C25 1.471(3) . . no C25 C219 1.452(4) . . no C25 C26 1.377(4) . . no C26 C27 1.445(3) . . no C27 C28 1.444(4) . . no C27 C221 1.393(4) . . no C28 C29 1.443(3) . . no C28 C224 1.392(3) . . no C29 C210 1.377(3) . . no C163 H163 0.9636 . . no C164 H164 0.9883 . . no C165 H165 0.9983 . . no C166 H166 0.9993 . . no C167 H167 1.0119 . . no C168 H168 0.9651 . . no C168 H168' 0.9936 . . no C169 H169 1.0031 . . no C169 H169' 1.0099 . . no C170 H170 1.0491 . . no C170 H170' 0.9894 . . no C172 H172" 0.9996 . . no C172 H172 1.0773 . . no C172 H172' 1.0740 . . no C210 C226 1.447(3) . . no C210 C211 1.476(3) . . no C211 C212 1.381(3) . . no C211 C228 1.436(3) . . no C212 C213 1.443(3) . . no C213 C230 1.392(3) . . no C213 C214 1.437(3) . . no C214 C215 1.390(4) . . no C215 C216 1.446(4) . . no C215 C232 1.452(3) . . no C216 C217 1.386(4) . . no C216 C234 1.449(4) . . no C217 C218 1.446(4) . . no C218 C236 1.396(4) . . no C218 C219 1.446(4) . . no C219 C220 1.381(3) . . no C220 C238 1.451(3) . . no C220 C221 1.446(4) . . no C221 C222 1.441(4) . . no C222 C239 1.446(4) . . no C222 C223 1.386(4) . . no C223 C242 1.451(4) . . no C223 C224 1.451(4) . . no C224 C225 1.439(3) . . no C225 C226 1.389(3) . . no C225 C243 1.453(4) . . no C226 C227 1.451(3) . . no C227 C228 1.444(3) . . no C227 C245 1.390(4) . . no C228 C229 1.398(3) . . no C229 C230 1.439(3) . . no C229 C247 1.455(3) . . no C230 C231 1.449(4) . . no C231 C248 1.442(3) . . no C31 C32 1.387(6) . . no C31 C36 1.386(7) . . no C231 C232 1.395(4) . . no C32 C33 1.387(7) . . no C232 C233 1.448(4) . . no C233 C250 1.389(3) . . no C33 C34 1.388(8) . . no C233 C234 1.454(3) . . no C234 C235 1.382(4) . . no C34 C35 1.387(8) . . no C235 C236 1.453(3) . . no C235 C252 1.444(4) . . no C35 C36 1.388(7) . . no C236 C237 1.444(3) . . no C237 C238 1.391(3) . . no C237 C253 1.447(4) . . no C238 C239 1.449(3) . . no C239 C240 1.395(4) . . no C240 C241 1.444(4) . . no C240 C254 1.449(3) . . no C241 C260 1.457(3) . . no C241 C242 1.390(4) . . no C242 C243 1.448(4) . . no C243 C244 1.383(3) . . no C244 C245 1.446(4) . . no C244 C259 1.454(4) . . no C245 C246 1.450(4) . . no C246 C258 1.443(4) . . no C246 C247 1.385(3) . . no C247 C248 1.451(4) . . no C248 C249 1.395(4) . . no C249 C250 1.454(4) . . no C249 C257 1.447(3) . . no C250 C251 1.445(3) . . no C251 C252 1.395(3) . . no C251 C256 1.453(3) . . no C252 C253 1.456(3) . . no C253 C254 1.387(4) . . no C254 C255 1.452(4) . . no C255 C260 1.452(4) . . no C255 C256 1.385(3) . . no C256 C257 1.446(4) . . no C257 C258 1.389(4) . . no C258 C259 1.451(4) . . no C259 C260 1.383(4) . . no C261 C262 1.509(3) . . no C261 C268 1.530(4) . . no C262 C263 1.386(4) . . no C262 C267 1.390(4) . . no C263 C264 1.387(4) . . no C264 C265 1.372(4) . . no C265 C266 1.385(4) . . no C266 C267 1.384(4) . . no C268 C269 1.531(4) . . no C269 C270 1.545(4) . . no C270 C271 1.497(4) . . no C32 H32 0.9502 . . no C33 H33 0.9499 . . no C34 H34 0.9500 . . no C35 H35 0.9494 . . no C36 H36 0.9502 . . no C263 H263 0.9624 . . no C264 H264 0.9396 . . no C265 H265 0.9552 . . no C266 H266 0.9795 . . no C267 H267 1.0040 . . no C268 H268' 1.0178 . . no C268 H268 1.0433 . . no C269 H269' 1.0565 . . no C269 H269 1.0197 . . no C270 H270 1.0208 . . no C270 H270' 0.9805 . . no C272 H272 0.9692 . . no C272 H272" 1.0334 . . no C272 H272' 1.0147 . . no C41 C42 1.385(5) . . no C41 C46 1.386(5) . . no C42 C43 1.385(5) . . no C43 C44 1.3838 . . no C44 C45 1.3846 . . no C45 C46 1.386(6) . . no C42 H42 0.9498 . . no C43 H43 0.9507 . . no C44 H44 0.9500 . . no C45 H45 0.9500 . . no C46 H46 0.9488 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C171 O12 C172 116.1(2) . . . yes C271 O22 C272 115.5(3) . . . yes C12 C11 C16 114.85(19) . . . no C12 C11 C161 57.63(15) . . . no C16 C11 C19 104.85(19) . . . no C16 C11 C161 126.8(2) . . . no C19 C11 C161 126.7(2) . . . no C12 C11 C19 114.71(19) . . . no C11 C12 C112 115.44(19) . . . no C11 C12 C161 56.88(15) . . . no C11 C12 C13 115.2(2) . . . no C13 C12 C161 126.1(2) . . . no C112 C12 C161 127.2(2) . . . no C13 C12 C112 105.0(2) . . . no C12 C13 C14 123.5(2) . . . no C14 C13 C114 119.2(2) . . . no C12 C13 C114 108.2(2) . . . no C13 C14 C15 120.8(2) . . . no C15 C14 C117 107.1(2) . . . no C13 C14 C117 120.0(2) . . . no C14 C15 C119 107.5(2) . . . no C16 C15 C119 119.8(2) . . . no C14 C15 C16 121.1(2) . . . no C11 C16 C15 123.7(2) . . . no C15 C16 C17 119.4(2) . . . no C11 C16 C17 108.4(2) . . . no C16 C17 C18 108.3(2) . . . no C18 C17 C121 120.3(2) . . . no C16 C17 C121 121.4(2) . . . no C17 C18 C19 108.7(2) . . . no C17 C18 C124 119.7(2) . . . no C19 C18 C124 121.0(2) . . . no C11 C19 C18 108.1(2) . . . no C11 C19 C110 123.6(2) . . . no C18 C19 C110 119.3(2) . . . no C19 C110 C126 120.2(2) . . . no C111 C110 C126 107.2(2) . . . no C19 C110 C111 121.1(2) . . . no C110 C111 C112 120.8(2) . . . no C112 C111 C128 120.0(2) . . . no C110 C111 C128 107.6(2) . . . no C12 C112 C111 123.5(2) . . . no C111 C112 C113 119.5(2) . . . no C12 C112 C113 108.1(2) . . . no C112 C113 C114 108.9(2) . . . no C112 C113 C130 121.0(2) . . . no C114 C113 C130 120.2(2) . . . no C13 C114 C113 108.4(2) . . . no C13 C114 C115 121.4(2) . . . no C113 C114 C115 120.0(2) . . . no C114 C115 C132 119.9(2) . . . no C116 C115 C132 108.2(2) . . . no C114 C115 C116 119.3(2) . . . no C115 C116 C134 108.1(2) . . . no C117 C116 C134 120.0(2) . . . no C115 C116 C117 119.5(2) . . . no C14 C117 C118 108.8(2) . . . no C116 C117 C118 119.9(2) . . . no C14 C117 C116 120.5(2) . . . no C117 C118 C136 119.9(2) . . . no C119 C118 C136 120.1(2) . . . no C117 C118 C119 108.1(2) . . . no C15 C119 C118 108.4(2) . . . no C118 C119 C120 120.2(2) . . . no C15 C119 C120 120.2(2) . . . no C119 C120 C121 119.7(2) . . . no C121 C120 C138 107.8(2) . . . no C119 C120 C138 119.7(2) . . . no C17 C121 C122 120.3(2) . . . no C120 C121 C122 108.6(2) . . . no C17 C121 C120 119.4(2) . . . no C121 C122 C139 107.6(2) . . . no C123 C122 C139 120.1(2) . . . no C121 C122 C123 119.5(2) . . . no C122 C123 C142 119.8(2) . . . no C124 C123 C142 107.6(2) . . . no C122 C123 C124 120.7(2) . . . no C18 C124 C123 119.6(2) . . . no C123 C124 C125 108.4(2) . . . no C18 C124 C125 119.5(2) . . . no C124 C125 C126 119.6(2) . . . no C126 C125 C143 120.3(2) . . . no C124 C125 C143 108.0(2) . . . no C110 C126 C127 108.2(2) . . . no C125 C126 C127 119.6(2) . . . no C110 C126 C125 120.3(2) . . . no C126 C127 C128 108.5(2) . . . no C128 C127 C145 120.6(2) . . . no C126 C127 C145 119.9(2) . . . no C111 C128 C127 108.4(2) . . . no C127 C128 C129 120.0(2) . . . no C111 C128 C129 119.9(2) . . . no C128 C129 C130 120.2(2) . . . no C128 C129 C147 119.6(2) . . . no C130 C129 C147 107.3(2) . . . no C113 C130 C129 119.3(2) . . . no C113 C130 C131 120.0(2) . . . no C129 C130 C131 109.0(2) . . . no C130 C131 C148 107.7(2) . . . no C132 C131 C148 120.1(2) . . . no C130 C131 C132 119.9(2) . . . no C115 C132 C131 120.0(2) . . . no C131 C132 C133 120.2(2) . . . no C115 C132 C133 107.6(2) . . . no C132 C133 C134 108.0(2) . . . no C134 C133 C150 120.3(2) . . . no C132 C133 C150 119.6(2) . . . no C116 C134 C133 108.1(2) . . . no C116 C134 C135 120.2(2) . . . no C133 C134 C135 119.7(2) . . . no C134 C135 C136 119.9(2) . . . no C134 C135 C152 120.1(2) . . . no C136 C135 C152 107.7(2) . . . no C118 C136 C137 119.8(2) . . . no C135 C136 C137 108.3(2) . . . no C118 C136 C135 120.1(2) . . . no C136 C137 C153 108.0(2) . . . no C138 C137 C153 119.9(2) . . . no C136 C137 C138 120.2(2) . . . no C120 C138 C137 120.0(2) . . . no C137 C138 C139 120.0(2) . . . no C120 C138 C139 108.2(2) . . . no C122 C139 C138 107.8(2) . . . no C138 C139 C140 120.0(2) . . . no C122 C139 C140 120.4(2) . . . no C139 C140 C141 119.6(2) . . . no C139 C140 C154 120.0(2) . . . no C141 C140 C154 108.0(2) . . . no C140 C141 C142 120.2(2) . . . no C140 C141 C160 108.2(2) . . . no C142 C141 C160 119.7(2) . . . no C123 C142 C143 107.8(2) . . . no C141 C142 C143 120.4(2) . . . no C123 C142 C141 119.9(2) . . . no C125 C143 C142 108.1(2) . . . no C142 C143 C144 119.2(2) . . . no C125 C143 C144 120.3(2) . . . no C143 C144 C145 119.3(2) . . . no C145 C144 C159 108.3(2) . . . no C143 C144 C159 120.7(2) . . . no C127 C145 C144 120.5(2) . . . no C127 C145 C146 119.6(2) . . . no C144 C145 C146 107.7(2) . . . no C145 C146 C147 119.7(2) . . . no C145 C146 C158 108.0(2) . . . no C147 C146 C158 120.0(2) . . . no C129 C147 C148 108.3(2) . . . no C146 C147 C148 119.8(2) . . . no C129 C147 C146 120.4(2) . . . no C131 C148 C147 107.6(2) . . . no C131 C148 C149 120.0(2) . . . no C147 C148 C149 119.9(2) . . . no C148 C149 C150 119.8(2) . . . no C148 C149 C157 120.5(2) . . . no C150 C149 C157 107.9(2) . . . no C133 C150 C151 120.0(2) . . . no C149 C150 C151 108.0(2) . . . no C133 C150 C149 120.2(2) . . . no C150 C151 C156 108.0(2) . . . no C152 C151 C156 120.0(2) . . . no C150 C151 C152 119.8(2) . . . no C135 C152 C153 108.2(2) . . . no C151 C152 C153 119.8(2) . . . no C135 C152 C151 120.0(2) . . . no C137 C153 C152 107.7(2) . . . no C137 C153 C154 119.8(2) . . . no C152 C153 C154 120.8(2) . . . no C140 C154 C153 120.3(2) . . . no C140 C154 C155 107.9(2) . . . no C153 C154 C155 119.5(2) . . . no C154 C155 C160 107.9(2) . . . no C156 C155 C160 120.3(2) . . . no C154 C155 C156 119.9(2) . . . no C151 C156 C157 108.0(2) . . . no C155 C156 C157 119.5(2) . . . no C151 C156 C155 120.0(2) . . . no C149 C157 C158 119.2(2) . . . no C156 C157 C158 120.3(2) . . . no C149 C157 C156 108.1(2) . . . no C146 C158 C159 107.8(2) . . . no C157 C158 C159 120.1(2) . . . no C146 C158 C157 120.6(2) . . . no C144 C159 C158 108.2(2) . . . no C158 C159 C160 119.9(2) . . . no C144 C159 C160 120.1(2) . . . no C141 C160 C155 107.9(2) . . . no C155 C160 C159 119.9(2) . . . no C141 C160 C159 120.0(2) . . . no C11 C161 C12 65.48(16) . . . no C11 C161 C162 119.9(2) . . . no C12 C161 C162 117.0(2) . . . no C12 C161 C168 116.3(2) . . . no C11 C161 C168 117.3(2) . . . no C162 C161 C168 113.0(2) . . . no C161 C162 C167 122.7(2) . . . no C163 C162 C167 118.7(2) . . . no C161 C162 C163 118.5(2) . . . no C162 C163 C164 120.8(2) . . . no C163 C164 C165 120.2(2) . . . no C164 C165 C166 119.6(2) . . . no C165 C166 C167 120.3(2) . . . no C162 C167 C166 120.4(2) . . . no C161 C168 C169 112.7(2) . . . no C168 C169 C170 109.6(2) . . . no C169 C170 C171 113.5(2) . . . no O11 C171 C170 125.3(2) . . . yes O12 C171 C170 111.1(2) . . . yes O11 C171 O12 123.6(2) . . . yes C22 C21 C26 115.4(2) . . . no C22 C21 C29 114.45(19) . . . no C22 C21 C261 57.98(15) . . . no C26 C21 C29 105.22(19) . . . no C26 C21 C261 126.8(2) . . . no C29 C21 C261 126.1(2) . . . no C21 C22 C23 114.7(2) . . . no C21 C22 C212 115.45(19) . . . no C21 C22 C261 57.37(15) . . . no C23 C22 C212 104.96(19) . . . no C23 C22 C261 126.4(2) . . . no C212 C22 C261 126.9(2) . . . no C22 C23 C24 123.8(2) . . . no C22 C23 C214 108.2(2) . . . no C24 C23 C214 119.3(2) . . . no C23 C24 C25 121.0(2) . . . no C23 C24 C217 119.7(2) . . . no C25 C24 C217 107.3(2) . . . no C24 C25 C26 120.6(2) . . . no C24 C25 C219 107.7(2) . . . no C26 C25 C219 119.5(2) . . . no C21 C26 C25 123.6(2) . . . no C21 C26 C27 108.1(2) . . . no C25 C26 C27 119.4(2) . . . no C26 C27 C28 108.6(2) . . . no C26 C27 C221 121.2(2) . . . no C28 C27 C221 120.1(2) . . . no C27 C28 C29 108.4(2) . . . no C27 C28 C224 120.1(2) . . . no C29 C28 C224 121.3(2) . . . no C21 C29 C210 124.2(2) . . . no C28 C29 C210 118.7(2) . . . no C21 C29 C28 108.1(2) . . . no C162 C163 H163 121.20 . . . no C164 C163 H163 117.97 . . . no C163 C164 H164 120.03 . . . no C165 C164 H164 119.76 . . . no C166 C165 H165 120.12 . . . no C164 C165 H165 120.16 . . . no C165 C166 H166 119.63 . . . no C167 C166 H166 120.08 . . . no C162 C167 H167 120.37 . . . no C166 C167 H167 119.18 . . . no C169 C168 H168' 105.33 . . . no H168' C168 H168 112.06 . . . no C161 C168 H168 108.81 . . . no C169 C168 H168 108.02 . . . no C161 C168 H168' 109.90 . . . no C168 C169 H169' 111.33 . . . no H169' C169 H169 110.26 . . . no C170 C169 H169 110.33 . . . no C168 C169 H169 108.29 . . . no C170 C169 H169' 107.07 . . . no C169 C170 H170' 107.38 . . . no C169 C170 H170 106.81 . . . no C171 C170 H170' 107.85 . . . no C171 C170 H170 109.37 . . . no H170' C170 H170 111.93 . . . no O12 C172 H172 111.21 . . . no H172' C172 H172 113.43 . . . no H172" C172 H172 101.69 . . . no H172' C172 H172" 115.88 . . . no O12 C172 H172' 104.02 . . . no O12 C172 H172" 110.84 . . . no C29 C210 C211 120.9(2) . . . no C29 C210 C226 120.4(2) . . . no C211 C210 C226 107.3(2) . . . no C210 C211 C212 120.4(2) . . . no C210 C211 C228 107.6(2) . . . no C212 C211 C228 120.1(2) . . . no C22 C212 C211 123.8(2) . . . no C22 C212 C213 108.3(2) . . . no C211 C212 C213 119.1(2) . . . no C212 C213 C214 108.4(2) . . . no C212 C213 C230 121.4(2) . . . no C214 C213 C230 120.3(2) . . . no C23 C214 C213 108.7(2) . . . no C23 C214 C215 121.3(2) . . . no C213 C214 C215 120.1(2) . . . no C214 C215 C216 119.0(2) . . . no C214 C215 C232 119.9(2) . . . no C216 C215 C232 108.5(2) . . . no C215 C216 C217 119.5(2) . . . no C215 C216 C234 107.5(2) . . . no C217 C216 C234 120.4(2) . . . no C24 C217 C216 121.0(2) . . . no C24 C217 C218 108.6(2) . . . no C216 C217 C218 119.5(2) . . . no C217 C218 C219 108.2(2) . . . no C217 C218 C236 120.5(2) . . . no C219 C218 C236 119.8(2) . . . no C25 C219 C218 108.2(2) . . . no C25 C219 C220 121.2(2) . . . no C218 C219 C220 120.1(2) . . . no C219 C220 C221 119.5(2) . . . no C219 C220 C238 120.4(2) . . . no C221 C220 C238 107.0(2) . . . no C27 C221 C220 119.1(2) . . . no C27 C221 C222 119.6(2) . . . no C220 C221 C222 109.2(2) . . . no C221 C222 C223 120.8(2) . . . no C221 C222 C239 107.5(2) . . . no C223 C222 C239 119.6(2) . . . no C222 C223 C224 119.5(2) . . . no C222 C223 C242 120.8(2) . . . no C224 C223 C242 107.6(2) . . . no C28 C224 C223 119.9(2) . . . no C28 C224 C225 119.5(2) . . . no C223 C224 C225 108.6(2) . . . no C224 C225 C226 119.2(2) . . . no C224 C225 C243 107.7(2) . . . no C226 C225 C243 120.3(2) . . . no C210 C226 C225 120.6(2) . . . no C210 C226 C227 108.3(2) . . . no C225 C226 C227 119.6(2) . . . no C226 C227 C228 107.9(2) . . . no C226 C227 C245 119.9(2) . . . no C228 C227 C245 120.6(2) . . . no C211 C228 C227 108.8(2) . . . no C211 C228 C229 120.7(2) . . . no C227 C228 C229 119.5(2) . . . no C228 C229 C230 119.5(2) . . . no C228 C229 C247 120.0(2) . . . no C230 C229 C247 107.9(2) . . . no C213 C230 C229 119.1(2) . . . no C213 C230 C231 120.0(2) . . . no C229 C230 C231 108.4(2) . . . no C230 C231 C232 119.6(2) . . . no C230 C231 C248 107.9(2) . . . no C232 C231 C248 120.1(2) . . . no C32 C31 C36 120.0(4) . . . no Cl31 C31 C32 119.1(3) . . . yes Cl31 C31 C36 121.0(3) . . . yes C215 C232 C231 120.0(2) . . . no C215 C232 C233 108.0(2) . . . no C231 C232 C233 119.7(2) . . . no C31 C32 C33 120.0(4) . . . no C232 C233 C234 107.6(2) . . . no C32 C33 C34 120.0(5) . . . no C234 C233 C250 120.1(2) . . . no C232 C233 C250 120.4(2) . . . no C216 C234 C233 108.5(2) . . . no C33 C34 C35 120.0(5) . . . no C216 C234 C235 120.2(2) . . . no C233 C234 C235 120.0(2) . . . no C234 C235 C252 119.9(2) . . . no C234 C235 C236 120.0(2) . . . no C34 C35 C36 119.9(5) . . . no C236 C235 C252 107.8(2) . . . no C31 C36 C35 120.0(5) . . . no C218 C236 C235 119.5(2) . . . no C218 C236 C237 120.0(2) . . . no C235 C236 C237 108.3(2) . . . no C236 C237 C253 108.0(2) . . . no C238 C237 C253 119.9(2) . . . no C236 C237 C238 120.1(2) . . . no C220 C238 C237 119.6(2) . . . no C237 C238 C239 120.0(2) . . . no C220 C238 C239 108.2(2) . . . no C222 C239 C240 120.0(2) . . . no C238 C239 C240 120.1(2) . . . no C222 C239 C238 108.1(2) . . . no C239 C240 C241 120.1(2) . . . no C239 C240 C254 119.6(2) . . . no C241 C240 C254 108.2(2) . . . no C240 C241 C242 120.2(2) . . . no C240 C241 C260 108.0(2) . . . no C242 C241 C260 119.5(2) . . . no C223 C242 C241 119.3(2) . . . no C223 C242 C243 107.9(2) . . . no C241 C242 C243 120.2(2) . . . no C225 C243 C242 108.1(2) . . . no C225 C243 C244 119.7(2) . . . no C242 C243 C244 120.1(2) . . . no C243 C244 C259 120.2(2) . . . no C245 C244 C259 107.8(2) . . . no C243 C244 C245 120.2(2) . . . no C227 C245 C244 120.2(2) . . . no C227 C245 C246 119.8(2) . . . no C244 C245 C246 108.2(2) . . . no C245 C246 C247 120.2(2) . . . no C245 C246 C258 108.0(2) . . . no C247 C246 C258 119.8(2) . . . no C229 C247 C248 107.7(2) . . . no C229 C247 C246 119.9(2) . . . no C246 C247 C248 120.3(2) . . . no C247 C248 C249 119.4(2) . . . no C231 C248 C247 108.1(2) . . . no C231 C248 C249 120.3(2) . . . no C248 C249 C257 120.4(2) . . . no C250 C249 C257 107.7(2) . . . no C248 C249 C250 119.7(2) . . . no C233 C250 C251 119.9(2) . . . no C249 C250 C251 108.0(2) . . . no C233 C250 C249 119.9(2) . . . no C250 C251 C256 108.2(2) . . . no C252 C251 C256 120.0(2) . . . no C250 C251 C252 119.7(2) . . . no C235 C252 C251 120.3(2) . . . no C235 C252 C253 108.0(2) . . . no C251 C252 C253 119.6(2) . . . no C237 C253 C252 107.9(2) . . . no C237 C253 C254 120.2(2) . . . no C252 C253 C254 120.2(2) . . . no C240 C254 C253 120.3(2) . . . no C253 C254 C255 119.9(2) . . . no C240 C254 C255 108.0(2) . . . no C254 C255 C260 108.0(2) . . . no C256 C255 C260 119.8(2) . . . no C254 C255 C256 120.3(2) . . . no C251 C256 C257 107.7(2) . . . no C255 C256 C257 120.4(2) . . . no C251 C256 C255 120.0(2) . . . no C249 C257 C258 119.5(2) . . . no C256 C257 C258 119.8(2) . . . no C249 C257 C256 108.4(2) . . . no C257 C258 C259 119.8(2) . . . no C246 C258 C257 120.6(2) . . . no C246 C258 C259 108.1(2) . . . no C244 C259 C260 119.7(2) . . . no C258 C259 C260 120.2(2) . . . no C244 C259 C258 107.8(2) . . . no C241 C260 C259 120.3(2) . . . no C255 C260 C259 120.0(2) . . . no C241 C260 C255 107.8(2) . . . no C21 C261 C22 64.66(16) . . . no C21 C261 C262 118.9(2) . . . no C22 C261 C262 115.1(2) . . . no C22 C261 C268 117.9(2) . . . no C21 C261 C268 115.9(2) . . . no C262 C261 C268 115.1(2) . . . no C261 C262 C263 121.9(2) . . . no C261 C262 C267 119.0(2) . . . no C263 C262 C267 119.0(2) . . . no C262 C263 C264 120.0(2) . . . no C263 C264 C265 120.6(3) . . . no C264 C265 C266 119.9(3) . . . no C265 C266 C267 119.7(3) . . . no C262 C267 C266 120.7(2) . . . no C261 C268 C269 113.0(2) . . . no C268 C269 C270 112.7(2) . . . no C269 C270 C271 113.4(2) . . . no O21 C271 C270 125.5(3) . . . yes O22 C271 C270 111.6(2) . . . yes O21 C271 O22 122.9(3) . . . yes C31 C32 H32 119.98 . . . no C33 C32 H32 120.01 . . . no C32 C33 H33 120.00 . . . no C34 C33 H33 120.02 . . . no C33 C34 H34 119.97 . . . no C35 C34 H34 119.99 . . . no C34 C35 H35 120.07 . . . no C36 C35 H35 119.99 . . . no C31 C36 H36 120.00 . . . no C35 C36 H36 119.95 . . . no C264 C263 H263 121.02 . . . no C262 C263 H263 118.89 . . . no C265 C264 H264 118.88 . . . no C263 C264 H264 120.48 . . . no C264 C265 H265 123.19 . . . no C266 C265 H265 116.85 . . . no C267 C266 H266 119.06 . . . no C265 C266 H266 121.26 . . . no C266 C267 H267 118.63 . . . no C262 C267 H267 120.47 . . . no C261 C268 H268 107.10 . . . no C261 C268 H268' 109.82 . . . no H268' C268 H268 107.03 . . . no C269 C268 H268' 110.55 . . . no C269 C268 H268 109.11 . . . no C270 C269 H269 111.19 . . . no H269' C269 H269 105.85 . . . no C270 C269 H269' 108.74 . . . no C268 C269 H269' 110.96 . . . no C268 C269 H269 107.15 . . . no C269 C270 H270' 106.12 . . . no C269 C270 H270 110.83 . . . no C271 C270 H270' 105.55 . . . no C271 C270 H270 106.74 . . . no H270' C270 H270 114.25 . . . no O22 C272 H272 107.49 . . . no H272' C272 H272 109.23 . . . no H272" C272 H272 112.80 . . . no H272' C272 H272" 110.35 . . . no O22 C272 H272' 105.84 . . . no O22 C272 H272" 110.84 . . . no Cl41 C41 C42 120.7(3) . . . yes Cl41 C41 C46 119.3(3) . . . yes C42 C41 C46 120.0(3) . . . no C41 C42 C43 120.0(3) . . . no C42 C43 C44 120.07 . . . no C43 C44 C45 119.99 . . . no C44 C45 C46 120.04 . . . no C41 C46 C45 119.9(3) . . . no C41 C42 H42 120.03 . . . no C43 C42 H42 120.00 . . . no C42 C43 H43 119.96 . . . no C44 C43 H43 119.98 . . . no C43 C44 H44 120.03 . . . no C45 C44 H44 119.98 . . . no C44 C45 H45 120.04 . . . no C46 C45 H45 119.92 . . . no C41 C46 H46 119.99 . . . no C45 C46 H46 120.08 . . . no 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 C172 O12 C171 O11 -3.6(4) . . . . no C172 O12 C171 C170 176.2(2) . . . . no C272 O22 C271 O21 -4.9(4) . . . . no C272 O22 C271 C270 174.3(3) . . . . no C16 C11 C12 C112 121.5(2) . . . . no C12 C11 C16 C15 8.5(3) . . . . no C19 C11 C12 C112 -0.1(3) . . . . no C19 C11 C16 C17 -12.2(3) . . . . no C16 C11 C12 C161 -119.2(2) . . . . no C19 C11 C12 C13 -122.8(2) . . . . no C16 C11 C12 C13 -1.2(3) . . . . no C12 C11 C19 C110 -7.2(3) . . . . no C16 C11 C19 C18 12.5(3) . . . . no C16 C11 C19 C110 -134.1(2) . . . . no C161 C11 C19 C18 -153.7(2) . . . . no C161 C11 C19 C110 59.7(4) . . . . no C12 C11 C161 C162 -108.2(2) . . . . no C12 C11 C161 C168 108.2(2) . . . . no C16 C11 C161 C12 98.5(3) . . . . no C16 C11 C161 C162 -9.7(4) . . . . no C16 C11 C161 C168 -153.3(2) . . . . no C19 C11 C161 C12 -98.3(3) . . . . no C19 C11 C161 C162 153.5(2) . . . . no C161 C11 C16 C15 -58.5(3) . . . . no C161 C11 C16 C17 153.9(2) . . . . no C12 C11 C19 C18 139.4(2) . . . . no C19 C11 C161 C168 9.9(3) . . . . no C161 C11 C12 C112 -119.3(2) . . . . no C19 C11 C16 C15 135.4(2) . . . . no C19 C11 C12 C161 119.2(2) . . . . no C12 C11 C16 C17 -139.1(2) . . . . no C161 C11 C12 C13 118.0(2) . . . . no C161 C12 C13 C14 59.4(4) . . . . no C161 C12 C13 C114 -154.1(2) . . . . no C112 C12 C13 C114 11.6(3) . . . . no C112 C12 C161 C11 98.5(3) . . . . no C112 C12 C161 C162 -148.9(2) . . . . no C11 C12 C161 C162 112.5(2) . . . . no C11 C12 C161 C168 -109.7(2) . . . . no C11 C12 C112 C113 -139.5(2) . . . . no C13 C12 C112 C113 -11.6(3) . . . . no C112 C12 C13 C14 -134.8(2) . . . . no C11 C12 C13 C14 -6.7(3) . . . . no C11 C12 C13 C114 139.7(2) . . . . no C11 C12 C112 C111 7.5(4) . . . . no C13 C12 C112 C111 135.4(3) . . . . no C161 C12 C112 C111 -59.0(4) . . . . no C112 C12 C161 C168 -11.2(3) . . . . no C161 C12 C112 C113 154.0(2) . . . . no C13 C12 C161 C11 -98.8(3) . . . . no C13 C12 C161 C162 13.7(3) . . . . no C13 C12 C161 C168 151.5(2) . . . . no C114 C13 C14 C15 -135.2(2) . . . . no C114 C13 C14 C117 2.4(3) . . . . no C12 C13 C14 C117 145.5(2) . . . . no C12 C13 C14 C15 7.8(4) . . . . no C12 C13 C114 C113 -7.5(3) . . . . no C14 C13 C114 C115 -4.6(4) . . . . no C12 C13 C114 C115 -152.7(2) . . . . no C14 C13 C114 C113 140.6(2) . . . . no C13 C14 C117 C116 0.7(3) . . . . no C117 C14 C15 C16 -142.5(2) . . . . no C117 C14 C15 C119 0.4(2) . . . . no C13 C14 C15 C119 142.8(2) . . . . no C15 C14 C117 C116 143.4(2) . . . . no C13 C14 C117 C118 -143.7(2) . . . . no C13 C14 C15 C16 -0.1(4) . . . . no C15 C14 C117 C118 -0.9(2) . . . . no C119 C15 C16 C11 -146.9(2) . . . . no C14 C15 C16 C17 135.9(2) . . . . no C16 C15 C119 C120 -0.2(3) . . . . no C14 C15 C16 C11 -8.3(4) . . . . no C119 C15 C16 C17 -2.6(3) . . . . no C14 C15 C119 C120 -143.7(2) . . . . no C14 C15 C119 C118 0.2(3) . . . . no C16 C15 C119 C118 143.7(2) . . . . no C11 C16 C17 C121 153.0(2) . . . . no C15 C16 C17 C121 3.8(3) . . . . no C11 C16 C17 C18 7.6(3) . . . . no C15 C16 C17 C18 -141.7(2) . . . . no C16 C17 C121 C122 -141.0(2) . . . . no C121 C17 C18 C124 -0.6(3) . . . . no C18 C17 C121 C122 0.5(3) . . . . no C16 C17 C18 C124 145.3(2) . . . . no C121 C17 C18 C19 -145.5(2) . . . . no C18 C17 C121 C120 139.4(2) . . . . no C16 C17 C121 C120 -2.1(4) . . . . no C16 C17 C18 C19 0.4(3) . . . . no C17 C18 C124 C125 -137.6(2) . . . . no C17 C18 C19 C11 -8.2(3) . . . . no C124 C18 C19 C11 -152.6(2) . . . . no C19 C18 C124 C125 3.0(4) . . . . no C19 C18 C124 C123 140.6(2) . . . . no C17 C18 C124 C123 0.1(3) . . . . no C17 C18 C19 C110 140.0(2) . . . . no C124 C18 C19 C110 -4.3(4) . . . . no C18 C19 C110 C126 3.2(4) . . . . no C18 C19 C110 C111 -135.5(2) . . . . no C11 C19 C110 C126 146.3(2) . . . . no C11 C19 C110 C111 7.6(4) . . . . no C261 C21 C29 C210 60.1(4) . . . . no C29 C21 C261 C22 -98.5(3) . . . . no C29 C21 C261 C262 155.5(2) . . . . no C22 C21 C261 C262 -106.0(2) . . . . no C22 C21 C261 C268 110.2(2) . . . . no C26 C21 C261 C22 99.5(3) . . . . no C26 C21 C261 C262 -6.5(4) . . . . no C26 C21 C261 C268 -150.3(2) . . . . no C26 C21 C22 C23 -0.3(3) . . . . no C26 C21 C22 C212 122.0(2) . . . . no C26 C21 C22 C261 -119.0(2) . . . . no C29 C21 C22 C23 -122.6(2) . . . . no C29 C21 C22 C212 -0.3(3) . . . . no C29 C21 C22 C261 118.7(2) . . . . no C261 C21 C22 C23 118.7(2) . . . . no C261 C21 C22 C212 -119.0(2) . . . . no C22 C21 C26 C25 7.8(3) . . . . no C22 C21 C26 C27 -138.9(2) . . . . no C29 C21 C26 C25 135.0(2) . . . . no C29 C21 C26 C27 -11.8(3) . . . . no C261 C21 C26 C25 -60.0(3) . . . . no C261 C21 C26 C27 153.2(2) . . . . no C22 C21 C29 C28 139.6(2) . . . . no C22 C21 C29 C210 -7.0(3) . . . . no C26 C21 C29 C28 11.8(3) . . . . no C26 C21 C29 C210 -134.8(2) . . . . no C261 C21 C29 C28 -153.3(2) . . . . no C29 C21 C261 C268 11.7(3) . . . . no C21 C22 C261 C268 -107.2(2) . . . . no C23 C22 C261 C21 -98.4(3) . . . . no C21 C22 C212 C211 7.6(3) . . . . no C23 C22 C212 C211 135.0(2) . . . . no C261 C22 C212 C211 -59.4(4) . . . . no C21 C22 C212 C213 -139.2(2) . . . . no C23 C22 C212 C213 -11.8(3) . . . . no C261 C22 C212 C213 153.7(2) . . . . no C23 C22 C261 C262 13.3(3) . . . . no C212 C22 C23 C24 -135.2(2) . . . . no C212 C22 C23 C214 11.8(3) . . . . no C261 C22 C23 C24 59.1(3) . . . . no C261 C22 C23 C214 -153.9(2) . . . . no C21 C22 C261 C262 111.7(2) . . . . no C23 C22 C261 C268 154.4(2) . . . . no C212 C22 C261 C21 99.1(3) . . . . no C212 C22 C261 C262 -149.3(2) . . . . no C212 C22 C261 C268 -8.1(3) . . . . no C21 C22 C23 C24 -7.4(3) . . . . no C21 C22 C23 C214 139.6(2) . . . . no C24 C23 C214 C215 -4.5(3) . . . . no C214 C23 C24 C217 2.4(3) . . . . no C214 C23 C24 C25 -135.5(2) . . . . no C22 C23 C214 C215 -153.2(2) . . . . no C22 C23 C214 C213 -7.5(3) . . . . no C24 C23 C214 C213 141.2(2) . . . . no C22 C23 C24 C25 8.1(4) . . . . no C22 C23 C24 C217 146.0(2) . . . . no C217 C24 C25 C219 -0.4(3) . . . . no C217 C24 C25 C26 -142.6(2) . . . . no C25 C24 C217 C216 143.6(2) . . . . no C23 C24 C25 C219 142.0(2) . . . . no C23 C24 C217 C216 0.5(4) . . . . no C25 C24 C217 C218 -0.2(3) . . . . no C23 C24 C25 C26 -0.1(3) . . . . no C23 C24 C217 C218 -143.3(2) . . . . no C219 C25 C26 C27 -2.6(3) . . . . no C24 C25 C26 C27 135.2(2) . . . . no C26 C25 C219 C220 -1.0(4) . . . . no C24 C25 C26 C21 -8.0(4) . . . . no C219 C25 C26 C21 -145.8(2) . . . . no C26 C25 C219 C218 143.5(2) . . . . no C24 C25 C219 C220 -143.6(2) . . . . no C24 C25 C219 C218 0.9(3) . . . . no C25 C26 C27 C28 -140.9(2) . . . . no C21 C26 C27 C221 152.9(2) . . . . no C25 C26 C27 C221 4.5(3) . . . . no C21 C26 C27 C28 7.5(3) . . . . no C28 C27 C221 C222 0.4(3) . . . . no C26 C27 C28 C29 0.1(3) . . . . no C26 C27 C28 C224 145.8(2) . . . . no C221 C27 C28 C224 0.0(4) . . . . no C28 C27 C221 C220 138.8(2) . . . . no C26 C27 C221 C222 -141.1(2) . . . . no C221 C27 C28 C29 -145.8(2) . . . . no C26 C27 C221 C220 -2.8(3) . . . . no C224 C28 C29 C21 -152.8(2) . . . . no C224 C28 C29 C210 -4.1(4) . . . . no C27 C28 C29 C210 141.2(2) . . . . no C27 C28 C29 C21 -7.6(3) . . . . no C27 C28 C224 C225 -138.9(2) . . . . no C29 C28 C224 C225 2.4(4) . . . . no C29 C28 C224 C223 140.9(2) . . . . no C27 C28 C224 C223 -0.4(3) . . . . no C28 C29 C210 C211 -135.9(2) . . . . no C28 C29 C210 C226 2.9(4) . . . . no C21 C29 C210 C211 7.5(4) . . . . no C21 C29 C210 C226 146.3(2) . . . . no C12 C161 C168 H168 33.56 . . . . no C162 C161 C168 H168' 49.87 . . . . no C11 C161 C168 H168' -164.09 . . . . no C162 C161 C168 H168 172.92 . . . . no C12 C161 C168 H168' -89.48 . . . . no C11 C161 C168 H168 -41.05 . . . . no C161 C162 C163 H163 -3.47 . . . . no C167 C162 C163 H163 -179.49 . . . . no C161 C162 C167 H167 3.47 . . . . no C163 C162 C167 H167 179.32 . . . . no H163 C163 C164 C165 -179.43 . . . . no C162 C163 C164 H164 178.96 . . . . no H163 C163 C164 H164 -1.85 . . . . no H164 C164 C165 C166 -178.85 . . . . no H164 C164 C165 H165 5.27 . . . . no C163 C164 C165 H165 -177.14 . . . . no C164 C165 C166 H166 179.53 . . . . no H165 C165 C166 H166 -4.60 . . . . no H165 C165 C166 C167 175.99 . . . . no H166 C166 C167 H167 1.38 . . . . no H166 C166 C167 C162 -178.47 . . . . no C165 C166 C167 H167 -179.21 . . . . no H168' C168 C169 H169' -63.08 . . . . no H168 C168 C169 C170 -64.76 . . . . no H168 C168 C169 H169 55.62 . . . . no H168' C168 C169 H169 175.54 . . . . no C161 C168 C169 H169' 56.75 . . . . no C161 C168 C169 H169 -64.63 . . . . no H168 C168 C169 H169' 177.00 . . . . no H168' C168 C169 C170 55.16 . . . . no C168 C169 C170 H170 -57.41 . . . . no H169 C169 C170 H170 -176.55 . . . . no C168 C169 C170 H170' 62.82 . . . . no H169 C169 C170 H170' -56.31 . . . . no H169' C169 C170 C171 -57.19 . . . . no H169 C169 C170 C171 62.81 . . . . no H169' C169 C170 H170' -176.32 . . . . no H169' C169 C170 H170 63.45 . . . . no H170 C170 C171 O12 -45.90 . . . . no H170' C170 C171 O11 11.88 . . . . no H170' C170 C171 O12 -167.85 . . . . no H170 C170 C171 O11 133.83 . . . . no C226 C210 C211 C212 -143.3(2) . . . . no C29 C210 C226 C225 -0.2(4) . . . . no C211 C210 C226 C225 143.5(2) . . . . no C211 C210 C226 C227 0.2(3) . . . . no C29 C210 C211 C228 143.1(2) . . . . no C226 C210 C211 C228 -0.4(3) . . . . no C29 C210 C226 C227 -143.5(2) . . . . no C29 C210 C211 C212 0.2(4) . . . . no C212 C211 C228 C227 143.5(2) . . . . no C228 C211 C212 C22 -146.2(2) . . . . no C210 C211 C228 C229 -143.3(2) . . . . no C210 C211 C212 C213 135.6(2) . . . . no C210 C211 C228 C227 0.4(3) . . . . no C210 C211 C212 C22 -7.9(4) . . . . no C212 C211 C228 C229 -0.3(4) . . . . no C228 C211 C212 C213 -2.7(3) . . . . no C22 C212 C213 C230 153.2(2) . . . . no C211 C212 C213 C214 -141.0(2) . . . . no C22 C212 C213 C214 7.6(3) . . . . no C211 C212 C213 C230 4.6(4) . . . . no C230 C213 C214 C215 0.1(3) . . . . no C214 C213 C230 C231 0.8(3) . . . . no C212 C213 C230 C229 -3.3(4) . . . . no C212 C213 C214 C23 -0.1(3) . . . . no C214 C213 C230 C229 138.3(2) . . . . no C230 C213 C214 C23 -146.1(2) . . . . no C212 C213 C214 C215 146.2(2) . . . . no C212 C213 C230 C231 -140.9(2) . . . . no C213 C214 C215 C216 -138.4(2) . . . . no C23 C214 C215 C216 3.6(4) . . . . no C213 C214 C215 C232 -1.0(3) . . . . no C23 C214 C215 C232 140.9(2) . . . . no C214 C215 C216 C217 -0.6(4) . . . . no C214 C215 C232 C231 1.0(3) . . . . no C214 C215 C232 C233 -141.1(2) . . . . no C214 C215 C216 C234 141.5(2) . . . . no C216 C215 C232 C233 0.3(3) . . . . no C232 C215 C216 C234 -0.3(3) . . . . no C232 C215 C216 C217 -142.3(2) . . . . no C216 C215 C232 C231 142.4(2) . . . . no C215 C216 C217 C24 -1.5(4) . . . . no C234 C216 C217 C218 1.3(4) . . . . no C215 C216 C234 C233 0.2(3) . . . . no C215 C216 C217 C218 138.5(2) . . . . no C217 C216 C234 C235 -1.6(4) . . . . no C215 C216 C234 C235 -143.3(2) . . . . no C234 C216 C217 C24 -138.7(3) . . . . no C217 C216 C234 C233 141.8(2) . . . . no C216 C217 C218 C236 -0.3(4) . . . . no C24 C217 C218 C236 144.1(2) . . . . no C216 C217 C218 C219 -143.7(2) . . . . no C24 C217 C218 C219 0.8(3) . . . . no C217 C218 C219 C25 -1.0(3) . . . . no C219 C218 C236 C237 0.8(4) . . . . no C217 C218 C219 C220 144.0(2) . . . . no C217 C218 C236 C237 -138.3(3) . . . . no C236 C218 C219 C220 0.4(4) . . . . no C219 C218 C236 C235 138.8(2) . . . . no C236 C218 C219 C25 -144.6(2) . . . . no C217 C218 C236 C235 -0.4(4) . . . . no C218 C219 C220 C221 -137.7(2) . . . . no C218 C219 C220 C238 -1.5(4) . . . . no C25 C219 C220 C221 2.7(4) . . . . no C25 C219 C220 C238 138.9(2) . . . . no C221 C220 C238 C239 -0.1(3) . . . . no C219 C220 C221 C27 -0.8(3) . . . . no C219 C220 C238 C239 -141.0(2) . . . . no C238 C220 C221 C27 -142.2(2) . . . . no C221 C220 C238 C237 142.3(2) . . . . no C219 C220 C238 C237 1.4(4) . . . . no C219 C220 C221 C222 141.5(2) . . . . no C238 C220 C221 C222 0.1(3) . . . . no C27 C221 C222 C223 -0.4(3) . . . . no C27 C221 C222 C239 141.9(2) . . . . no C220 C221 C222 C223 -142.5(2) . . . . no C220 C221 C222 C239 -0.1(3) . . . . no C221 C222 C223 C224 0.0(3) . . . . no C223 C222 C239 C240 0.0(3) . . . . no C221 C222 C223 C242 137.9(2) . . . . no C239 C222 C223 C224 -137.9(2) . . . . no C239 C222 C223 C242 0.0(4) . . . . no C221 C222 C239 C238 0.1(3) . . . . no C221 C222 C239 C240 -142.8(2) . . . . no C223 C222 C239 C238 143.0(2) . . . . no C222 C223 C224 C28 0.4(3) . . . . no C222 C223 C224 C225 143.0(2) . . . . no C242 C223 C224 C28 -142.4(2) . . . . no C242 C223 C224 C225 0.2(3) . . . . no C222 C223 C242 C241 -0.1(4) . . . . no C222 C223 C242 C243 -142.0(2) . . . . no C224 C223 C242 C241 142.2(2) . . . . no C224 C223 C242 C243 0.2(3) . . . . no C223 C224 C225 C243 -0.5(3) . . . . no C223 C224 C225 C226 -142.4(2) . . . . no C28 C224 C225 C226 0.4(4) . . . . no C28 C224 C225 C243 142.3(2) . . . . no C224 C225 C226 C227 137.7(2) . . . . no C224 C225 C243 C242 0.6(3) . . . . no C243 C225 C226 C210 -138.5(2) . . . . no C243 C225 C226 C227 0.7(4) . . . . no C224 C225 C226 C210 -1.5(4) . . . . no C226 C225 C243 C244 -0.5(4) . . . . no C224 C225 C243 C244 -141.9(2) . . . . no C226 C225 C243 C242 142.0(2) . . . . no C210 C226 C227 C228 0.0(3) . . . . no C210 C226 C227 C245 143.4(2) . . . . no C225 C226 C227 C228 -143.6(2) . . . . no C225 C226 C227 C245 -0.2(4) . . . . no C245 C227 C228 C229 0.9(4) . . . . no C226 C227 C245 C244 -0.4(4) . . . . no C226 C227 C245 C246 -139.0(2) . . . . no C228 C227 C245 C244 138.4(2) . . . . no C228 C227 C245 C246 -0.2(4) . . . . no C226 C227 C228 C211 -0.3(3) . . . . no C226 C227 C228 C229 144.0(2) . . . . no C245 C227 C228 C211 -143.4(2) . . . . no C227 C228 C229 C247 -1.0(4) . . . . no C211 C228 C229 C230 1.6(4) . . . . no C211 C228 C229 C247 139.0(2) . . . . no C227 C228 C229 C230 -138.4(2) . . . . no C228 C229 C230 C213 0.2(4) . . . . no C228 C229 C230 C231 142.2(2) . . . . no C247 C229 C230 C213 -141.7(2) . . . . no C230 C229 C247 C246 142.3(2) . . . . no C230 C229 C247 C248 -0.3(3) . . . . no C228 C229 C247 C248 -142.0(2) . . . . no C247 C229 C230 C231 0.3(3) . . . . no C228 C229 C247 C246 0.6(4) . . . . no C213 C230 C231 C248 141.4(2) . . . . no C213 C230 C231 C232 -0.8(3) . . . . no C229 C230 C231 C232 -142.3(2) . . . . no C229 C230 C231 C248 -0.2(3) . . . . no C230 C231 C232 C215 -0.2(3) . . . . no C230 C231 C248 C247 0.0(3) . . . . no C230 C231 C248 C249 -142.2(2) . . . . no C232 C231 C248 C247 141.9(2) . . . . no C232 C231 C248 C249 -0.2(3) . . . . no C230 C231 C232 C233 137.6(2) . . . . no C248 C231 C232 C215 -137.7(2) . . . . no C248 C231 C232 C233 0.0(3) . . . . no Cl31 C31 C32 C33 178.4(4) . . . . no C36 C31 C32 C33 -0.1(8) . . . . no C32 C31 C36 C35 0.1(8) . . . . no Cl31 C31 C36 C35 -178.4(4) . . . . no C31 C32 C33 C34 0.1(8) . . . . no C215 C232 C233 C234 -0.2(3) . . . . no C231 C232 C233 C250 0.3(3) . . . . no C231 C232 C233 C234 -142.4(2) . . . . no C215 C232 C233 C250 142.6(2) . . . . no C232 C233 C234 C235 143.5(2) . . . . no C232 C233 C250 C249 -0.5(3) . . . . no C232 C233 C234 C216 0.0(3) . . . . no C234 C233 C250 C251 -0.1(4) . . . . no C250 C233 C234 C216 -142.9(2) . . . . no C250 C233 C234 C235 0.6(4) . . . . no C234 C233 C250 C249 137.7(2) . . . . no C32 C33 C34 C35 -0.1(8) . . . . no C232 C233 C250 C251 -138.3(2) . . . . no C216 C234 C235 C236 0.9(4) . . . . no C33 C34 C35 C36 0.1(8) . . . . no C233 C234 C235 C252 -0.7(4) . . . . no C216 C234 C235 C252 138.6(3) . . . . no C233 C234 C235 C236 -138.4(2) . . . . no C234 C235 C252 C251 0.3(4) . . . . no C252 C235 C236 C237 0.2(3) . . . . no C234 C235 C252 C253 -142.1(2) . . . . no C252 C235 C236 C218 -142.1(2) . . . . no C236 C235 C252 C253 0.1(3) . . . . no C234 C235 C236 C237 142.4(2) . . . . no C236 C235 C252 C251 142.5(2) . . . . no C234 C235 C236 C218 0.1(4) . . . . no C34 C35 C36 C31 0.0(8) . . . . no C218 C236 C237 C238 -0.9(4) . . . . no C218 C236 C237 C253 141.6(2) . . . . no C235 C236 C237 C238 -143.0(2) . . . . no C235 C236 C237 C253 -0.5(3) . . . . no C238 C237 C253 C254 0.0(4) . . . . no C238 C237 C253 C252 143.2(2) . . . . no C236 C237 C238 C220 -0.2(4) . . . . no C236 C237 C253 C252 0.5(3) . . . . no C236 C237 C253 C254 -142.6(2) . . . . no C236 C237 C238 C239 137.8(2) . . . . no C253 C237 C238 C220 -138.3(2) . . . . no C253 C237 C238 C239 -0.4(4) . . . . no C220 C238 C239 C240 142.8(2) . . . . no C237 C238 C239 C222 -142.3(2) . . . . no C237 C238 C239 C240 0.6(4) . . . . no C220 C238 C239 C222 0.0(3) . . . . no C238 C239 C240 C254 -0.5(4) . . . . no C222 C239 C240 C241 0.0(4) . . . . no C238 C239 C240 C241 -138.5(2) . . . . no C222 C239 C240 C254 138.1(2) . . . . no C239 C240 C241 C242 -0.1(4) . . . . no C239 C240 C241 C260 142.1(2) . . . . no C239 C240 C254 C255 -142.6(2) . . . . no C241 C240 C254 C253 142.6(2) . . . . no C241 C240 C254 C255 -0.2(3) . . . . no C239 C240 C254 C253 0.1(4) . . . . no C254 C240 C241 C242 -142.3(2) . . . . no C254 C240 C241 C260 -0.2(3) . . . . no C260 C241 C242 C223 -137.8(2) . . . . no C240 C241 C260 C259 -142.3(2) . . . . no C260 C241 C242 C243 -0.5(4) . . . . no C240 C241 C260 C255 0.4(3) . . . . no C240 C241 C242 C243 137.4(2) . . . . no C240 C241 C242 C223 0.1(4) . . . . no C242 C241 C260 C255 142.9(2) . . . . no C242 C241 C260 C259 0.2(4) . . . . no C241 C242 C243 C225 -142.1(2) . . . . no C223 C242 C243 C225 -0.5(3) . . . . no C223 C242 C243 C244 141.8(2) . . . . no C241 C242 C243 C244 0.2(4) . . . . no C242 C243 C244 C245 -138.2(2) . . . . no C225 C243 C244 C259 138.4(2) . . . . no C242 C243 C244 C259 0.3(4) . . . . no C225 C243 C244 C245 -0.1(4) . . . . no C243 C244 C245 C246 143.3(2) . . . . no C259 C244 C245 C227 -142.5(2) . . . . no C259 C244 C245 C246 0.3(3) . . . . no C243 C244 C259 C258 -142.9(2) . . . . no C243 C244 C245 C227 0.5(4) . . . . no C243 C244 C259 C260 -0.6(4) . . . . no C245 C244 C259 C258 0.1(3) . . . . no C245 C244 C259 C260 142.4(2) . . . . no C227 C245 C246 C247 -0.3(4) . . . . no C227 C245 C246 C258 142.3(2) . . . . no C244 C245 C246 C247 -143.3(2) . . . . no C244 C245 C246 C258 -0.6(3) . . . . no C245 C246 C258 C257 -142.6(2) . . . . no C245 C246 C258 C259 0.7(3) . . . . no C258 C246 C247 C229 -138.2(2) . . . . no C247 C246 C258 C259 143.5(2) . . . . no C258 C246 C247 C248 -0.4(4) . . . . no C247 C246 C258 C257 0.2(4) . . . . no C245 C246 C247 C229 0.1(4) . . . . no C245 C246 C247 C248 138.0(2) . . . . no C229 C247 C248 C231 0.2(3) . . . . no C229 C247 C248 C249 142.7(2) . . . . no C246 C247 C248 C231 -142.2(2) . . . . no C246 C247 C248 C249 0.3(4) . . . . no C247 C248 C249 C250 -137.9(2) . . . . no C247 C248 C249 C257 -0.2(3) . . . . no C231 C248 C249 C257 137.8(2) . . . . no C231 C248 C249 C250 0.1(3) . . . . no C248 C249 C257 C258 0.1(4) . . . . no C248 C249 C250 C233 0.3(3) . . . . no C248 C249 C257 C256 -142.2(2) . . . . no C250 C249 C257 C258 142.2(2) . . . . no C248 C249 C250 C251 142.5(2) . . . . no C250 C249 C257 C256 0.0(3) . . . . no C257 C249 C250 C251 0.1(3) . . . . no C257 C249 C250 C233 -142.2(2) . . . . no C249 C250 C251 C256 -0.1(3) . . . . no C233 C250 C251 C252 -0.3(4) . . . . no C249 C250 C251 C252 -142.6(2) . . . . no C233 C250 C251 C256 142.2(2) . . . . no C250 C251 C252 C235 0.3(4) . . . . no C250 C251 C252 C253 138.4(2) . . . . no C250 C251 C256 C257 0.1(3) . . . . no C252 C251 C256 C255 -0.4(4) . . . . no C252 C251 C256 C257 142.5(2) . . . . no C250 C251 C256 C255 -142.8(2) . . . . no C256 C251 C252 C235 -137.8(2) . . . . no C256 C251 C252 C253 0.3(4) . . . . no C235 C252 C253 C254 142.7(2) . . . . no C251 C252 C253 C237 -143.1(2) . . . . no C251 C252 C253 C254 0.0(4) . . . . no C235 C252 C253 C237 -0.4(3) . . . . no C237 C253 C254 C240 0.1(4) . . . . no C237 C253 C254 C255 138.5(2) . . . . no C252 C253 C254 C240 -138.5(2) . . . . no C252 C253 C254 C255 -0.2(4) . . . . no C253 C254 C255 C260 -142.5(2) . . . . no C240 C254 C255 C256 143.0(2) . . . . no C240 C254 C255 C260 0.4(3) . . . . no C253 C254 C255 C256 0.1(4) . . . . no C254 C255 C260 C241 -0.5(3) . . . . no C260 C255 C256 C251 138.4(2) . . . . no C254 C255 C256 C257 -138.0(3) . . . . no C256 C255 C260 C259 -0.5(4) . . . . no C254 C255 C260 C259 142.3(2) . . . . no C256 C255 C260 C241 -143.3(2) . . . . no C254 C255 C256 C251 0.2(4) . . . . no C260 C255 C256 C257 0.3(4) . . . . no C255 C256 C257 C258 0.6(4) . . . . no C251 C256 C257 C258 -142.1(2) . . . . no C255 C256 C257 C249 142.7(2) . . . . no C251 C256 C257 C249 0.0(3) . . . . no C249 C257 C258 C246 -0.1(3) . . . . no C249 C257 C258 C259 -139.2(2) . . . . no C256 C257 C258 C259 -1.2(4) . . . . no C256 C257 C258 C246 137.9(2) . . . . no C257 C258 C259 C244 143.2(2) . . . . no C257 C258 C259 C260 1.0(4) . . . . no C246 C258 C259 C260 -142.6(2) . . . . no C246 C258 C259 C244 -0.5(3) . . . . no C244 C259 C260 C255 -137.9(2) . . . . no C258 C259 C260 C241 138.0(2) . . . . no C258 C259 C260 C255 -0.2(4) . . . . no C244 C259 C260 C241 0.3(4) . . . . no C262 C261 C268 C269 -76.6(3) . . . . no C21 C261 C262 C267 126.3(3) . . . . no C22 C261 C262 C267 52.6(3) . . . . no C21 C261 C262 C263 -56.4(3) . . . . no C21 C261 C268 C269 68.6(3) . . . . no C22 C261 C262 C263 -130.0(3) . . . . no C22 C261 C268 C269 142.2(2) . . . . no C268 C261 C262 C263 87.7(3) . . . . no C268 C261 C262 C267 -89.6(3) . . . . no C263 C262 C267 C266 0.4(4) . . . . no C261 C262 C267 C266 177.8(2) . . . . no C261 C262 C263 C264 -176.8(3) . . . . no C267 C262 C263 C264 0.5(4) . . . . no C262 C263 C264 C265 -1.1(4) . . . . no C263 C264 C265 C266 0.8(4) . . . . no C264 C265 C266 C267 0.2(4) . . . . no C265 C266 C267 C262 -0.7(4) . . . . no C261 C268 C269 C270 -173.6(2) . . . . no C268 C269 C270 C271 76.6(3) . . . . no C269 C270 C271 O21 108.5(3) . . . . no C269 C270 C271 O22 -70.8(3) . . . . no Cl41 C41 C42 C43 -179.7(2) . . . . no C46 C41 C42 C43 -0.1(5) . . . . no Cl41 C41 C46 C45 179.8(2) . . . . no C42 C41 C46 C45 0.1(5) . . . . no C41 C42 C43 C44 0.07 . . . . no C42 C43 C44 C45 -0.07 . . . . no C43 C44 C45 C46 0.08 . . . . no C44 C45 C46 C41 -0.08 . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl31 C136 3.577(3) . 1_455 no Cl31 C231 3.631(3) . 1_545 no Cl41 C125 3.413(3) . . no Cl41 C141 3.469(3) . 2_666 no Cl41 C126 3.604(3) . . no Cl41 C221 3.588(3) . . no Cl41 C124 3.484(3) . . no Cl41 C27 3.644(3) . . no Cl31 H170 3.0961 . . no O11 C42 3.171(4) . . no O11 C28 3.207(3) . . no O11 C139 3.353(3) . 1_455 no O11 C43 3.336(4) . . no O11 C138 3.361(3) . 1_455 no O11 C46 3.162(4) . 2_566 no O11 C45 3.352(4) . 2_566 no O12 C32 3.299(6) . . no O12 C35 3.235(6) . 2_565 no O12 C34 3.282(5) . 2_565 no O12 C224 3.362(3) . . no O12 C31 3.248(5) . . no O21 C172 3.094(4) . . no O21 C237 3.282(3) . 1_455 no O21 C253 3.278(3) . 1_455 no O22 C268 3.051(4) . . no O11 H172 2.4505 . . no O11 H42 2.4606 . . no O11 H45 2.8363 . 2_566 no O11 H172" 2.7629 . . no O11 H269' 2.7866 . . no O11 H46 2.4446 . 2_566 no O11 H43 2.8027 . . no O12 H169' 2.7274 . . no O21 H272" 2.6053 . . no O21 H172 2.8902 . . no O21 H272 2.6394 . . no O21 H172" 2.4061 . . no O22 H268' 2.3518 . . no C13 C163 3.444(4) . . no C14 C162 3.429(4) . . no C14 C260 3.574(3) . 2_665 no C15 C162 3.457(4) . . no C15 C167 3.441(4) . . no C16 C167 3.144(3) . . no C17 C238 3.331(3) . . no C17 C239 3.204(3) . . no C18 C220 3.499(3) . . no C18 C238 3.594(3) . . no C18 C221 3.579(3) . . no C19 C169 3.598(4) . . no C23 C267 3.147(4) . . no C24 C262 3.396(4) . . no C25 C262 3.434(4) . . no C26 C263 3.309(4) . . no C27 Cl41 3.644(3) . . no C27 C45 3.429(4) . 2_566 no C28 C171 3.419(4) . . no C28 O11 3.207(3) . . no C29 C269 3.393(4) . . no C31 O12 3.248(5) . . no C31 C172 3.577(6) . 2_565 no C32 O12 3.299(6) . . no C32 C172 3.592(6) . 2_565 no C34 O12 3.282(5) . 2_565 no C35 O12 3.235(6) . 2_565 no C42 C263 3.546(4) . . no C42 O11 3.171(4) . . no C43 C140 3.521(4) . 1_455 no C43 O11 3.336(4) . . no C45 O11 3.352(4) . 2_566 no C45 C27 3.429(4) . 2_566 no C46 C264 3.576(4) . . no C46 O11 3.162(4) . 2_566 no C110 C168 3.419(4) . . no C111 C168 3.419(4) . . no C11 H167 2.8674 . . no C11 H169 3.0432 . . no C12 H163 3.0905 . . no C112 C234 3.560(3) . 1_545 no C112 C233 3.529(3) . 1_545 no C113 C234 2.943(3) . 1_545 no C113 C233 3.287(4) . 1_545 no C113 C235 3.559(3) . 1_545 no C114 C233 3.547(4) . 1_545 no C114 C234 3.547(4) . 1_545 no C15 H166 2.8325 . 2_665 no C16 H167 2.6696 . . no C116 C244 3.599(3) . 2_665 no C116 C259 3.352(3) . 2_665 no C117 C244 3.478(3) . 2_665 no C117 C259 3.313(3) . 2_665 no C19 H168 2.7636 . . no C19 H169 3.0422 . . no C21 H269' 2.8485 . . no C21 H263 3.0206 . . no C22 H267 2.8139 . . no C23 H266 2.9716 . 2_576 no C123 C143 3.380(3) . 2_666 no C123 C142 3.474(4) . 2_666 no C23 H267 2.8134 . . no C124 Cl41 3.484(3) . . no C125 Cl41 3.413(3) . . no C126 Cl41 3.604(3) . . no C26 H263 3.0490 . . no C27 H45 2.7569 . 2_566 no C28 H172 2.8958 . . no C129 C147 3.446(3) . 2_656 no C29 H269' 2.7705 . . no C29 H172 2.8214 . . no C29 H268' 2.8730 . . no C130 C234 3.393(4) . 1_545 no C31 H172' 2.6122 . 2_565 no C32 H172' 2.7838 . 2_565 no C133 C268 3.577(4) . 1_645 no C133 C212 3.238(3) . 1_645 no C33 H172' 3.0912 . . no C34 H172' 2.7132 . . no C134 C212 3.546(3) . 1_645 no C134 C213 3.525(4) . 1_645 no C135 C230 3.588(4) . 1_645 no C135 C213 3.496(3) . 1_645 no C35 H169' 3.0158 . 2_565 no C35 H172' 2.7639 . . no C36 H172' 3.0600 . 2_565 no C136 Cl31 3.577(3) . 1_655 no C137 C170 3.355(4) . 1_655 no C137 C171 3.211(4) . 1_655 no C138 O11 3.361(3) . 1_655 no C138 C171 3.330(4) . 1_655 no C138 C172 3.528(4) . 1_655 no C139 O11 3.353(3) . 1_655 no C140 C43 3.521(4) . 1_655 no C141 Cl41 3.469(3) . 2_666 no C41 H263 2.9293 . . no C142 C142 3.142(4) . 2_666 no C142 C123 3.474(4) . 2_666 no C42 H264 3.0273 . 2_566 no C142 C143 3.244(3) . 2_666 no C42 H263 2.6465 . . no C143 C142 3.244(3) . 2_666 no C43 H263 2.8589 . . no C143 C123 3.380(3) . 2_666 no C145 C270 3.434(4) . 2_566 no C45 H264 2.8281 . . no C46 H264 2.8498 . . no C46 H263 2.9158 . 2_566 no C146 C147 3.558(3) . 2_656 no C147 C129 3.446(3) . 2_656 no C147 C147 2.902(3) . 2_656 no C147 C146 3.558(3) . 2_656 no C147 C148 3.410(3) . 2_656 no C148 C147 3.410(3) . 2_656 no C150 C212 3.506(3) . 1_645 no C152 C213 3.584(3) . 1_645 no C153 C171 3.582(4) . 1_655 no C153 C170 3.304(4) . 1_655 no C158 C218 3.341(3) . 2_666 no C158 C217 3.530(3) . 2_666 no C159 C219 3.407(4) . 2_666 no C159 C218 3.187(4) . 2_666 no C160 C219 3.480(3) . 2_666 no C162 C15 3.457(4) . . no C162 C14 3.429(4) . . no C163 C13 3.444(4) . . no C164 C254 3.271(4) . 2_665 no C165 C254 3.533(4) . 2_665 no C165 C240 3.381(4) . 2_665 no C167 C15 3.441(4) . . no C167 C169 3.581(4) . . no C167 C16 3.144(3) . . no C168 C110 3.419(4) . . no C168 C111 3.419(4) . . no C169 C167 3.581(4) . . no C169 C19 3.598(4) . . no C170 C137 3.355(4) . 1_455 no C170 C153 3.304(4) . 1_455 no C171 C224 3.572(4) . . no C171 C153 3.582(4) . 1_455 no C171 C138 3.330(4) . 1_455 no C171 C137 3.211(4) . 1_455 no C171 C28 3.419(4) . . no C172 C225 3.572(4) . . no C172 O21 3.094(4) . . no C172 C138 3.528(4) . 1_455 no C172 C224 3.513(4) . . no C172 C31 3.577(6) . 2_565 no C172 C32 3.592(6) . 2_565 no C210 C272 3.511(5) . . no C210 C268 3.408(4) . . no C110 H168 2.7208 . . no C211 C268 3.441(4) . . no C111 H168 2.6832 . . no C212 C134 3.546(3) . 1_465 no C212 C133 3.238(3) . 1_465 no C112 H168 2.6893 . . no C212 C150 3.506(3) . 1_465 no C213 C134 3.525(4) . 1_465 no C213 C135 3.496(3) . 1_465 no C213 C152 3.584(3) . 1_465 no C217 C158 3.530(3) . 2_666 no C118 H33 3.0737 . 2_665 no C218 C159 3.187(4) . 2_666 no C218 C158 3.341(3) . 2_666 no C119 H165 2.9735 . 2_665 no C219 C160 3.480(3) . 2_666 no C219 C159 3.407(4) . 2_666 no C119 H166 2.9673 . 2_665 no C120 H172" 3.0621 . 1_655 no C120 H165 2.8560 . 2_665 no C220 C18 3.499(3) . . no C221 C18 3.579(3) . . no C221 Cl41 3.588(3) . . no C224 O12 3.362(3) . . no C224 C171 3.572(4) . . no C224 C172 3.513(4) . . no C225 C172 3.572(4) . . no C227 C247 3.494(4) . 2_575 no C227 C246 3.509(4) . 2_575 no C127 H269 2.9846 . 2_566 no C228 C245 3.411(3) . 2_575 no C228 C246 3.513(4) . 2_575 no C229 C245 3.484(3) . 2_575 no C230 C135 3.588(4) . 1_465 no C231 Cl31 3.631(3) . 1_565 no C133 H268' 3.0929 . 1_645 no C233 C114 3.547(4) . 1_565 no C233 C112 3.529(3) . 1_565 no C233 C113 3.287(4) . 1_565 no C234 C112 3.560(3) . 1_565 no C234 C114 3.547(4) . 1_565 no C234 C113 2.943(3) . 1_565 no C234 C130 3.393(4) . 1_565 no C235 C113 3.559(3) . 1_565 no C237 C271 3.477(4) . 1_655 no C237 O21 3.282(3) . 1_655 no C137 H170 2.8627 . 1_655 no C238 C17 3.331(3) . . no C138 H172" 2.7811 . 1_655 no C238 C18 3.594(3) . . no C239 C17 3.204(3) . . no C140 H43 2.6947 . 1_655 no C240 C165 3.381(4) . 2_665 no C244 C116 3.599(3) . 2_665 no C244 C117 3.478(3) . 2_665 no C245 C229 3.484(3) . 2_575 no C145 H270 2.9081 . 2_566 no C245 C228 3.411(3) . 2_575 no C246 C228 3.513(4) . 2_575 no C246 C227 3.509(4) . 2_575 no C247 C227 3.494(4) . 2_575 no C148 H268 3.0056 . 1_645 no C149 H268 2.9485 . 1_645 no C149 H267 2.9985 . 1_645 no C150 H268 3.0256 . 1_645 no C150 H267 2.9210 . 1_645 no C251 C257 3.562(4) . 2_675 no C251 C256 3.431(3) . 2_675 no C153 H170 2.9436 . 1_655 no C153 H170' 3.0354 . 1_655 no C253 C271 3.534(4) . 1_655 no C253 O21 3.278(3) . 1_655 no C254 C164 3.271(4) . 2_665 no C254 C165 3.533(4) . 2_665 no C256 C257 3.551(4) . 2_675 no C256 C251 3.431(3) . 2_675 no C256 C256 3.227(4) . 2_675 no C257 C256 3.551(4) . 2_675 no C257 C251 3.562(4) . 2_675 no C258 C272 3.550(5) . 2_575 no C259 C117 3.313(3) . 2_665 no C259 C116 3.352(3) . 2_665 no C260 C14 3.574(3) . 2_665 no C162 H169' 2.8028 . . no C262 C25 3.434(4) . . no C262 C24 3.396(4) . . no C263 C269 3.497(4) . . no C263 C26 3.309(4) . . no C163 H168' 2.8375 . . no C263 C42 3.546(4) . . no C163 H35 2.9986 . 2_565 no C164 H35 2.8868 . 2_565 no C264 C46 3.576(4) . . no C164 H32 2.9996 . . no C165 H35 2.9747 . 2_565 no C165 H32 2.9169 . . no C166 H32 3.0176 . . no C167 H169' 3.0138 . . no C267 C23 3.147(4) . . no C268 C210 3.408(4) . . no C168 H163 3.0965 . . no C268 O22 3.051(4) . . no C268 C133 3.577(3) . 1_465 no C268 C211 3.441(4) . . no C269 C29 3.393(4) . . no C269 C263 3.497(4) . . no C270 C145 3.434(4) . 2_566 no C271 C253 3.534(4) . 1_455 no C271 C237 3.477(4) . 1_455 no C272 C258 3.550(5) . 2_575 no C272 C210 3.511(5) . . no C210 H268' 2.7877 . . no C210 H172 2.9491 . . no C210 H272" 3.0702 . . no C211 H268' 2.6741 . . no C212 H268' 2.6535 . . no C214 H266 2.9080 . 2_576 no C215 H266 2.9860 . 2_576 no C215 H265 3.0550 . 2_576 no C222 H169 3.0461 . . no C222 H167 2.9277 . . no C223 H167 2.9053 . . no C224 H172 3.0415 . . no C226 H272" 3.0997 . . no C233 H163 3.0271 . 1_565 no C243 H33 3.0846 . . no C246 H272' 2.8243 . 2_575 no C248 H163 3.0631 . 1_565 no C249 H163 2.9343 . 1_565 no C250 H163 2.9126 . 1_565 no C252 H272 2.8888 . 1_655 no C253 H272 2.7929 . 1_655 no C254 H164 2.9084 . 2_665 no C258 H272' 2.7553 . 2_575 no C262 H269 2.9607 . . no C263 H269 2.8945 . . no C267 H268 3.0738 . . no C271 H268' 2.9050 . . no H168' H170 2.3288 . . no H168' H163 2.5860 . . no H168' C163 2.8375 . . no H169' C35 3.0158 . 2_565 no H169' H35 2.5473 . 2_565 no H169' C167 3.0138 . . no H169' C162 2.8028 . . no H169' O12 2.7274 . . no H170' H168 2.5042 . . no H170' H264 2.4721 . 2_566 no H170' C153 3.0354 . 1_455 no H172' C34 2.7132 . . no H172' C35 2.7639 . . no H172' C33 3.0912 . . no H172' C36 3.0600 . 2_565 no H172' C32 2.7838 . 2_565 no H172' C31 2.6122 . 2_565 no H172" O21 2.4061 . . no H172" C138 2.7811 . 1_455 no H172" O11 2.7629 . . no H172" C120 3.0621 . 1_455 no H268' C133 3.0929 . 1_465 no H268' C29 2.8730 . . no H268' C271 2.9050 . . no H268' C210 2.7877 . . no H268' C211 2.6741 . . no H268' C212 2.6535 . . no H268' O22 2.3518 . . no H269' O11 2.7866 . . no H269' C29 2.7705 . . no H269' C21 2.8485 . . no H272' C246 2.8243 . 2_575 no H272' C258 2.7553 . 2_575 no H272" C210 3.0702 . . no H272" C226 3.0997 . . no H272" O21 2.6053 . . no H32 C165 2.9169 . . no H32 C166 3.0176 . . no H32 C164 2.9996 . . no H33 C118 3.0737 . 2_665 no H33 C243 3.0846 . . no H35 C163 2.9986 . 2_565 no H35 C165 2.9747 . 2_565 no H35 H169' 2.5473 . 2_565 no H35 C164 2.8868 . 2_565 no H42 O11 2.4606 . . no H43 C140 2.6947 . 1_455 no H43 O11 2.8027 . . no H45 O11 2.8363 . 2_566 no H45 C27 2.7569 . 2_566 no H46 O11 2.4446 . 2_566 no H163 C12 3.0905 . . no H163 C250 2.9126 . 1_545 no H163 H168' 2.5860 . . no H163 C248 3.0631 . 1_545 no H163 C168 3.0965 . . no H163 C233 3.0271 . 1_545 no H163 C249 2.9343 . 1_545 no H164 C254 2.9084 . 2_665 no H165 C119 2.9735 . 2_665 no H165 C120 2.8560 . 2_665 no H166 C15 2.8325 . 2_665 no H166 C119 2.9673 . 2_665 no H167 C222 2.9277 . . no H167 C16 2.6696 . . no H167 C223 2.9053 . . no H167 C11 2.8674 . . no H168 C112 2.6893 . . no H168 C111 2.6832 . . no H168 C110 2.7208 . . no H168 H170' 2.5042 . . no H168 C19 2.7636 . . no H169 C19 3.0422 . . no H169 C222 3.0461 . . no H169 C11 3.0432 . . no H170 Cl31 3.0961 . . no H170 C153 2.9436 . 1_455 no H170 H168' 2.3288 . . no H170 C137 2.8627 . 1_455 no H172 O21 2.8902 . . no H172 C210 2.9491 . . no H172 C28 2.8958 . . no H172 C29 2.8214 . . no H172 C224 3.0415 . . no H172 O11 2.4505 . . no H263 C21 3.0206 . . no H263 H269 2.5929 . . no H263 C46 2.9158 . 2_566 no H263 C41 2.9293 . . no H263 C42 2.6465 . . no H263 C26 3.0490 . . no H263 C43 2.8589 . . no H264 C45 2.8281 . . no H264 C46 2.8498 . . no H264 C42 3.0273 . 2_566 no H264 H170' 2.4721 . 2_566 no H265 C215 3.0550 . 2_576 no H266 C214 2.9080 . 2_576 no H266 C215 2.9860 . 2_576 no H266 C23 2.9716 . 2_576 no H267 C22 2.8139 . . no H267 C150 2.9210 . 1_465 no H267 C23 2.8134 . . no H267 C149 2.9985 . 1_465 no H268 C267 3.0738 . . no H268 H270 2.5817 . . no H268 C150 3.0256 . 1_465 no H268 C148 3.0056 . 1_465 no H268 C149 2.9485 . 1_465 no H269 C263 2.8945 . . no H269 C262 2.9607 . . no H269 H263 2.5929 . . no H269 C127 2.9846 . 2_566 no H270 H268 2.5817 . . no H270 C145 2.9081 . 2_566 no H272 C253 2.7929 . 1_455 no H272 O21 2.6394 . . no H272 C252 2.8888 . 1_455 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C172 H172" O21 1.0000 2.4100 3.094(4) 125.00 . yes C268 H268' O22 1.0200 2.3500 3.051(4) 125.00 . yes C42 H42 O11 0.9500 2.4600 3.171(4) 132.00 . yes C46 H46 O11 0.9500 2.4400 3.162(4) 132.00 2_566 yes #===END of Crystallographic Information File