# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 # Attachment 'boltalina--1-.cif' #============================================================================== # Chemical tailoring of fullerene acceptor materials: # synthesis, structures and electrochemical properties # of perfluoroisopropylfullerenes data_New_Global_Publ_Block #TrackingRef 'boltalina--1-.cif' _publ_section_related_literature ? # Added by publCIF - use a unique identifier for each data block #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Steven Strauss' # Name of author for correspondence _publ_contact_author_address # Address of author for correspondence ; Chemistry Department Colorado State University Fort Collins CO 80523 USA ; _publ_contact_author_email steven.strauss@colostate.edu _publ_contact_author_fax +1-970-491-1801 _publ_contact_author_phone +1-970-491-5104 _publ_requested_journal 'Chemical Communications' _publ_requested_category ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Chemical tailoring of fullerene acceptor materials: synthesis, structures and electrochemical properties of perfluoroisopropylfullerenes ; _publ_section_title_footnote # remove if not required . # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. # NB if using publCIF, the Author database tool might prove useful # (see the Tools menu in publCIF) loop_ _publ_author_name _publ_author_address N.Shustova ; Chemistry Department Colorado State University Fort Collins CO 80523 USA ; I.Kuvychko . D.Peryshkov ; Chemistry Department Colorado State University Fort Collins CO 80523 USA ; J.Whitaker . Yu.S.Chen ; Chemistry Department Colorado State University Fort Collins CO 80523 USA ; L.Dunsch . A.Popov ; Chemistry Department Colorado State University Fort Collins CO 80523 USA ; S.Strauss . O.Boltalina ; Center for Advanced Radiation Sources The University of Chicago c/o Advanced Photon Source/ANL 9700 S. Cass Avenue. Bldg. 434 D Argonne, IL 60439 ; #============================================================================== # TEXT _publ_section_synopsis . _publ_section_abstract ; (type here to add abstract) ; _publ_section_comment ; (type here to add) ; _publ_section_acknowledgements # remove if not required ; (type here to add acknowledgements) ; _publ_section_references ; ? ; _publ_section_figure_captions ; ; _publ_section_exptl_prep ; (type here to add preparation details) ; _publ_section_exptl_refinement ; (type here to add refinement details) ; #============================================================================== data_a _database_code_depnum_ccdc_archive 'CCDC 796276' #TrackingRef 'boltalina--1-.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 F42' _chemical_formula_sum 'C78 F42' _chemical_formula_weight 1734.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F -0.0051 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2212(6) _cell_length_b 13.6183(8) _cell_length_c 21.3423(13) _cell_angle_alpha 80.248(2) _cell_angle_beta 87.129(2) _cell_angle_gamma 71.128(2) _cell_volume 2770.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9972 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 18.99 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.042 _exptl_crystal_size_mid 0.033 _exptl_crystal_size_min 0.021 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1692 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9966 _exptl_absorpt_correction_T_max 0.9983 _exptl_absorpt_process_details 'SADABS, v. 2.10, Bruker AXS, Madison, WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.44280 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator 'diamond 1 1 1' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker D8 goniometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 77132 _diffrn_reflns_av_R_equivalents 0.0984 _diffrn_reflns_av_sigmaI/netI 0.0813 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 18.72 _reflns_number_total 16740 _reflns_number_gt 11492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II v.2.2 (Bruker, 2007)' _computing_cell_refinement 'APEX II v.2.2 (Bruker, 2007)' _computing_data_reduction 'APEX II v.2.2 (Bruker, 2007)' _computing_structure_solution 'SHELXTL, v. 6.14, Bruker AXS' _computing_structure_refinement 'SHELXTL, v. 6.14, Bruker AXS' _computing_molecular_graphics 'SHELXTL (Bruker, 2008)' _computing_publication_material 'SHELXTL (Bruker, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+1.2140P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.150(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 16740 _refine_ls_number_parameters 1155 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1625 _refine_ls_wR_factor_gt 0.1433 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0116(2) 0.21031(16) 0.35044(10) 0.0102(4) Uani 1 1 d . A . C2 C -0.0446(2) 0.22615(16) 0.28183(10) 0.0111(4) Uani 1 1 d . . . C3 C 0.0605(2) 0.17208(16) 0.24209(10) 0.0106(4) Uani 1 1 d . A . C4 C 0.1927(2) 0.13702(16) 0.27678(10) 0.0105(4) Uani 1 1 d . . . C5 C 0.1696(2) 0.16795(16) 0.33852(10) 0.0109(4) Uani 1 1 d . . . C6 C 0.2654(2) 0.20113(16) 0.36425(10) 0.0110(4) Uani 1 1 d . A . C7 C 0.2285(2) 0.28694(16) 0.40794(10) 0.0113(4) Uani 1 1 d . . . C8 C 0.0779(2) 0.35183(16) 0.39479(10) 0.0109(4) Uani 1 1 d . A . C9 C -0.0176(2) 0.31826(16) 0.37008(10) 0.0109(4) Uani 1 1 d . . . C10 C -0.1300(2) 0.41052(16) 0.34074(10) 0.0112(4) Uani 1 1 d . A . C11 C -0.1954(2) 0.41043(16) 0.28582(10) 0.0107(4) Uani 1 1 d . . . C011 C -0.0410(2) 0.13160(17) 0.39999(10) 0.0130(4) Uani 1 1 d . . . C12 C -0.1491(2) 0.31538(16) 0.25517(10) 0.0101(4) Uani 1 1 d . A . C012 C -0.0520(3) 0.03610(19) 0.37256(12) 0.0234(5) Uani 1 1 d . A . C13 C -0.1535(2) 0.34961(16) 0.18806(10) 0.0105(4) Uani 1 1 d . . . C013 C -0.1796(3) 0.18582(19) 0.43191(12) 0.0194(5) Uani 1 1 d . A . C14 C -0.0498(2) 0.29328(16) 0.14957(10) 0.0104(4) Uani 1 1 d . A . C15 C 0.0552(2) 0.20117(16) 0.17644(10) 0.0104(4) Uani 1 1 d . . . C16 C 0.1859(2) 0.18179(16) 0.13355(10) 0.0098(4) Uani 1 1 d . A . C17 C 0.3108(2) 0.16940(16) 0.17396(10) 0.0101(4) Uani 1 1 d . . . C18 C 0.3131(2) 0.13563(15) 0.24333(10) 0.0106(4) Uani 1 1 d . A . C19 C 0.4137(2) 0.16925(16) 0.26971(10) 0.0108(4) Uani 1 1 d . . . C20 C 0.3875(2) 0.20440(16) 0.32863(10) 0.0112(4) Uani 1 1 d . A . C21 C 0.4207(2) 0.29656(16) 0.33716(10) 0.0115(4) Uani 1 1 d . . . C22 C 0.3214(2) 0.35354(16) 0.37778(10) 0.0111(4) Uani 1 1 d . A . C23 C 0.2729(2) 0.46223(16) 0.36345(10) 0.0107(4) Uani 1 1 d . . . C24 C 0.1251(2) 0.52181(16) 0.36661(10) 0.0108(4) Uani 1 1 d . A . C25 C 0.0324(2) 0.46714(16) 0.38217(10) 0.0106(4) Uani 1 1 d . . . C26 C -0.0977(2) 0.50332(16) 0.34941(10) 0.0100(4) Uani 1 1 d . A . C27 C -0.1268(2) 0.59128(16) 0.30160(10) 0.0101(4) Uani 1 1 d . . . C28 C -0.1935(2) 0.59056(16) 0.24369(10) 0.0109(4) Uani 1 1 d . A . C29 C -0.2275(2) 0.50103(16) 0.23623(10) 0.0106(4) Uani 1 1 d . A . C30 C -0.2018(2) 0.46369(17) 0.17588(10) 0.0114(4) Uani 1 1 d . A . C31 C -0.1448(2) 0.51709(17) 0.12657(10) 0.0114(4) Uani 1 1 d . . . C32 C -0.0389(2) 0.45872(16) 0.08632(10) 0.0104(4) Uani 1 1 d . A . C33 C 0.0080(2) 0.34923(17) 0.09737(10) 0.0105(4) Uani 1 1 d . . . C34 C 0.1523(2) 0.29084(16) 0.09050(10) 0.0101(4) Uani 1 1 d . A . C35 C 0.2458(2) 0.34390(16) 0.07523(9) 0.0097(4) Uani 1 1 d . . . C36 C 0.3992(2) 0.30194(16) 0.09860(10) 0.0097(4) Uani 1 1 d . A . C37 C 0.4053(2) 0.22190(16) 0.15870(10) 0.0100(4) Uani 1 1 d . A . C38 C 0.4712(2) 0.22496(16) 0.21771(10) 0.0102(4) Uani 1 1 d . A . C39 C 0.5034(2) 0.31241(16) 0.22597(10) 0.0107(4) Uani 1 1 d . . . C40 C 0.4778(2) 0.35029(17) 0.28624(10) 0.0111(4) Uani 1 1 d . A . C41 C 0.4310(2) 0.46301(17) 0.27468(10) 0.0109(4) Uani 1 1 d . . . C42 C 0.3327(2) 0.51815(16) 0.31369(10) 0.0109(4) Uani 1 1 d . A . C43 C 0.2293(2) 0.62935(16) 0.29064(10) 0.0106(4) Uani 1 1 d . . . C44 C 0.0932(2) 0.61471(16) 0.31915(10) 0.0105(4) Uani 1 1 d . A . C45 C -0.0313(2) 0.64989(16) 0.28739(10) 0.0105(4) Uani 1 1 d . A . C46 C -0.0533(2) 0.70732(16) 0.21756(10) 0.0110(4) Uani 1 1 d . . . C47 C -0.1406(2) 0.64769(16) 0.19225(10) 0.0110(4) Uani 1 1 d . A . C48 C -0.1127(2) 0.60989(16) 0.13507(10) 0.0112(4) Uani 1 1 d . A . C49 C 0.0154(2) 0.60817(16) 0.09969(10) 0.0117(4) Uani 1 1 d . . . C50 C 0.0586(2) 0.51450(16) 0.07013(10) 0.0106(4) Uani 1 1 d . A . C51 C 0.1994(2) 0.45727(16) 0.06636(10) 0.0103(4) Uani 1 1 d . A . C52 C 0.3007(2) 0.49297(17) 0.09196(10) 0.0110(4) Uani 1 1 d . . . C53 C 0.4132(2) 0.40353(16) 0.11768(10) 0.0108(4) Uani 1 1 d . A . C54 C 0.4712(2) 0.40459(16) 0.17486(10) 0.0106(4) Uani 1 1 d . A . C55 C 0.4264(2) 0.49691(17) 0.20481(10) 0.0107(4) Uani 1 1 d . A . C56 C 0.3208(2) 0.58517(16) 0.17834(10) 0.0107(4) Uani 1 1 d . . . C57 C 0.2133(2) 0.64592(16) 0.21838(10) 0.0111(4) Uani 1 1 d . A . C58 C 0.0894(2) 0.67974(15) 0.18630(10) 0.0106(4) Uani 1 1 d . A . C59 C 0.1126(2) 0.64107(16) 0.12487(10) 0.0104(4) Uani 1 1 d . A . C60 C 0.2575(2) 0.58364(16) 0.12069(10) 0.0109(4) Uani 1 1 d . A . C071 C 0.2549(2) 0.24432(18) 0.48146(10) 0.0156(4) Uani 0.855(3) 1 d PD A 1 C072 C 0.2709(4) 0.3273(3) 0.51924(15) 0.0213(7) Uani 0.855(3) 1 d PD A 1 C073 C 0.3745(3) 0.1408(2) 0.49602(12) 0.0172(6) Uani 0.855(3) 1 d PD A 1 C074 C 0.2042(15) 0.3288(12) 0.5234(6) 0.037(6) Uani 0.145(3) 1 d PD A 2 C075 C 0.4206(15) 0.1910(12) 0.4937(7) 0.036(5) Uani 0.145(3) 1 d PD A 2 C076 C 0.2549(2) 0.24432(18) 0.48146(10) 0.0156(4) Uani 0.145(3) 1 d PD A 2 C161 C 0.2097(2) 0.08744(17) 0.09596(10) 0.0125(4) Uani 1 1 d . . . C162 C 0.2724(3) -0.02090(18) 0.13876(12) 0.0181(5) Uani 1 1 d . A . C163 C 0.0794(2) 0.08928(18) 0.06106(11) 0.0158(4) Uani 1 1 d . A . C361 C 0.5071(2) 0.25475(16) 0.04706(10) 0.0108(4) Uani 1 1 d . . . C362 C 0.4616(2) 0.30740(18) -0.02233(11) 0.0156(4) Uani 1 1 d . A . C363 C 0.6551(2) 0.25372(18) 0.05964(11) 0.0145(4) Uani 1 1 d . A . C431 C 0.2646(2) 0.72040(17) 0.31438(11) 0.0143(4) Uani 1 1 d . A . C432 C 0.2445(3) 0.72178(19) 0.38723(12) 0.0185(5) Uani 1 1 d . . . C433 C 0.4101(3) 0.7271(2) 0.29501(13) 0.0210(5) Uani 1 1 d . . . C461 C -0.1279(2) 0.83092(16) 0.20866(11) 0.0138(4) Uani 1 1 d . A . C462 C -0.2258(3) 0.86630(18) 0.26399(13) 0.0205(5) Uani 1 1 d . . . C463 C -0.2052(3) 0.87579(18) 0.14385(13) 0.0214(5) Uani 1 1 d . . . F011 F 0.05408(15) 0.08950(12) 0.44831(7) 0.0224(3) Uani 1 1 d . A . F015 F -0.22754(16) 0.11617(12) 0.46841(8) 0.0238(3) Uani 1 1 d . . . F071 F 0.13769(18) 0.22215(15) 0.50697(8) 0.0184(4) Uani 0.855(3) 1 d PD A 1 F072 F 0.2122(16) 0.1615(10) 0.4986(5) 0.034(3) Uani 0.145(3) 1 d PD A 2 F073 F 0.1767(3) 0.4207(2) 0.50231(16) 0.0271(7) Uani 0.855(3) 1 d PD A 1 F074 F 0.2559(2) 0.29787(13) 0.58149(7) 0.0320(4) Uani 0.855(3) 1 d PD A 1 F075 F 0.3961(2) 0.33856(16) 0.50998(9) 0.0302(5) Uani 0.855(3) 1 d PD A 1 F076 F 0.3425(2) 0.06301(13) 0.47681(8) 0.0233(4) Uani 0.855(3) 1 d PD A 1 F077 F 0.4031(3) 0.1129(2) 0.55794(14) 0.0256(6) Uani 0.855(3) 1 d PD A 1 F078 F 0.4888(5) 0.1499(4) 0.4657(2) 0.0244(7) Uani 0.855(3) 1 d PD A 1 F079 F 0.0687(13) 0.3475(12) 0.5230(6) 0.046(4) Uani 0.145(3) 1 d PD A 2 F080 F 0.2319(19) 0.4153(16) 0.4990(11) 0.034(5) Uani 0.145(3) 1 d PD A 2 F081 F 0.2559(2) 0.29787(13) 0.58149(7) 0.0320(4) Uani 0.145(3) 1 d PD A 2 F082 F 0.447(2) 0.1349(17) 0.5530(8) 0.042(5) Uani 0.145(3) 1 d PD A 2 F083 F 0.4917(14) 0.2604(11) 0.4919(6) 0.045(4) Uani 0.145(3) 1 d PD A 2 F084 F 0.488(4) 0.125(2) 0.4541(13) 0.038(7) Uani 0.145(3) 1 d PD A 2 F112 F -0.0658(2) -0.03873(12) 0.41846(8) 0.0316(4) Uani 1 1 d . . . F113 F -0.1624(2) 0.06632(14) 0.33331(8) 0.0358(4) Uani 1 1 d . . . F114 F 0.0591(2) -0.00563(12) 0.33947(9) 0.0349(4) Uani 1 1 d . . . F116 F -0.16164(18) 0.25099(12) 0.46832(8) 0.0268(4) Uani 1 1 d . . . F117 F -0.27479(16) 0.24278(13) 0.38849(8) 0.0274(4) Uani 1 1 d . . . F161 F 0.30428(15) 0.09472(11) 0.04901(7) 0.0185(3) Uani 1 1 d . A . F162 F 0.20254(17) -0.02632(11) 0.19269(7) 0.0230(3) Uani 1 1 d . . . F163 F 0.27045(18) -0.10011(11) 0.11016(8) 0.0275(4) Uani 1 1 d . . . F164 F 0.40385(16) -0.03599(12) 0.15293(8) 0.0274(4) Uani 1 1 d . . . F165 F 0.01720(15) 0.18525(11) 0.02863(7) 0.0191(3) Uani 1 1 d . . . F166 F 0.11393(16) 0.02289(12) 0.01919(7) 0.0222(3) Uani 1 1 d . . . F167 F -0.01056(15) 0.06250(12) 0.10194(7) 0.0221(3) Uani 1 1 d . . . F361 F 0.51883(14) 0.15080(10) 0.04954(6) 0.0143(3) Uani 1 1 d . A . F362 F 0.35100(15) 0.28533(12) -0.03798(7) 0.0211(3) Uani 1 1 d . . . F363 F 0.56087(15) 0.27342(12) -0.06380(7) 0.0205(3) Uani 1 1 d . . . F364 F 0.42925(16) 0.41193(11) -0.02896(7) 0.0213(3) Uani 1 1 d . . . F365 F 0.74703(14) 0.19075(13) 0.02535(7) 0.0229(3) Uani 1 1 d . . . F366 F 0.66744(15) 0.34978(12) 0.04535(7) 0.0218(3) Uani 1 1 d . . . F367 F 0.68935(14) 0.21789(11) 0.12095(7) 0.0177(3) Uani 1 1 d . . . F431 F 0.17303(15) 0.81378(10) 0.28632(7) 0.0207(3) Uani 1 1 d . . . F432 F 0.28752(17) 0.79435(12) 0.40559(8) 0.0254(3) Uani 1 1 d . A . F433 F 0.31235(19) 0.62912(12) 0.42132(7) 0.0288(4) Uani 1 1 d . A . F434 F 0.10960(17) 0.74400(14) 0.40111(8) 0.0280(4) Uani 1 1 d . A . F435 F 0.43824(19) 0.71339(15) 0.23514(8) 0.0339(4) Uani 1 1 d . A . F436 F 0.41884(18) 0.82068(13) 0.30025(9) 0.0314(4) Uani 1 1 d . A . F437 F 0.50823(16) 0.65323(14) 0.33167(10) 0.0339(4) Uani 1 1 d . A . F461 F -0.03062(15) 0.88091(11) 0.20788(8) 0.0230(3) Uani 1 1 d . . . F462 F -0.15252(18) 0.84996(12) 0.31712(8) 0.0288(4) Uani 1 1 d . A . F463 F -0.31481(16) 0.81269(12) 0.27538(9) 0.0282(4) Uani 1 1 d . A . F464 F -0.29857(17) 0.96830(11) 0.25183(8) 0.0292(4) Uani 1 1 d . A . F465 F -0.12448(19) 0.83689(12) 0.09722(7) 0.0308(4) Uani 1 1 d . A . F466 F -0.23861(18) 0.97997(11) 0.13148(8) 0.0292(4) Uani 1 1 d . A . F467 F -0.32062(17) 0.85024(13) 0.14371(9) 0.0303(4) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0120(9) 0.0083(8) 0.0111(9) -0.0014(7) 0.0026(7) -0.0045(7) C2 0.0121(9) 0.0108(9) 0.0128(9) -0.0020(7) 0.0013(7) -0.0072(8) C3 0.0122(9) 0.0066(8) 0.0138(9) -0.0012(7) 0.0017(8) -0.0044(7) C4 0.0141(9) 0.0068(8) 0.0106(9) -0.0006(7) 0.0004(7) -0.0040(7) C5 0.0124(9) 0.0071(8) 0.0122(9) -0.0005(7) 0.0012(7) -0.0024(7) C6 0.0132(9) 0.0082(9) 0.0089(9) -0.0001(7) -0.0011(7) -0.0005(7) C7 0.0134(9) 0.0090(9) 0.0104(9) -0.0017(7) -0.0001(7) -0.0021(7) C8 0.0132(9) 0.0095(9) 0.0088(9) -0.0014(7) 0.0011(7) -0.0021(7) C9 0.0141(9) 0.0093(9) 0.0097(9) -0.0015(7) 0.0040(7) -0.0048(7) C10 0.0111(9) 0.0103(9) 0.0123(9) -0.0024(7) 0.0039(7) -0.0039(7) C11 0.0076(9) 0.0108(9) 0.0145(9) -0.0023(7) 0.0031(7) -0.0041(7) C011 0.0168(10) 0.0105(9) 0.0118(9) -0.0001(7) 0.0019(8) -0.0055(8) C12 0.0091(9) 0.0116(9) 0.0120(9) -0.0022(7) 0.0012(7) -0.0068(7) C012 0.0387(15) 0.0152(11) 0.0196(11) -0.0032(9) 0.0096(11) -0.0144(10) C13 0.0082(9) 0.0123(9) 0.0120(9) -0.0013(7) -0.0006(7) -0.0047(7) C013 0.0197(11) 0.0170(11) 0.0210(11) 0.0014(9) 0.0039(9) -0.0078(9) C14 0.0107(9) 0.0131(9) 0.0111(9) -0.0037(7) -0.0003(7) -0.0077(8) C15 0.0107(9) 0.0112(9) 0.0122(9) -0.0038(7) 0.0011(7) -0.0063(7) C16 0.0113(9) 0.0093(9) 0.0098(9) -0.0031(7) 0.0002(7) -0.0038(7) C17 0.0088(9) 0.0099(9) 0.0113(9) -0.0042(7) 0.0005(7) -0.0015(7) C18 0.0131(9) 0.0048(8) 0.0127(9) -0.0024(7) 0.0008(8) -0.0007(7) C19 0.0102(9) 0.0067(8) 0.0126(9) -0.0008(7) -0.0015(7) 0.0010(7) C20 0.0110(9) 0.0082(9) 0.0115(9) 0.0000(7) -0.0023(7) 0.0003(7) C21 0.0090(9) 0.0106(9) 0.0126(9) -0.0010(7) -0.0041(7) 0.0001(7) C22 0.0123(9) 0.0116(9) 0.0100(9) -0.0027(7) -0.0024(7) -0.0037(8) C23 0.0116(9) 0.0116(9) 0.0097(9) -0.0045(7) -0.0009(7) -0.0034(7) C24 0.0128(9) 0.0094(9) 0.0104(9) -0.0035(7) 0.0001(7) -0.0029(7) C25 0.0121(9) 0.0101(9) 0.0095(9) -0.0033(7) 0.0013(7) -0.0026(7) C26 0.0092(9) 0.0100(9) 0.0110(9) -0.0036(7) 0.0036(7) -0.0032(7) C27 0.0075(8) 0.0081(8) 0.0149(9) -0.0034(7) 0.0033(7) -0.0023(7) C28 0.0066(8) 0.0089(9) 0.0146(9) -0.0007(7) 0.0009(7) 0.0003(7) C29 0.0066(8) 0.0115(9) 0.0131(9) -0.0026(7) 0.0016(7) -0.0020(7) C30 0.0055(8) 0.0131(9) 0.0156(10) -0.0022(8) -0.0006(7) -0.0029(7) C31 0.0078(9) 0.0134(9) 0.0118(9) -0.0004(7) -0.0021(7) -0.0024(7) C32 0.0081(8) 0.0125(9) 0.0102(9) -0.0008(7) -0.0023(7) -0.0029(7) C33 0.0098(9) 0.0143(9) 0.0095(9) -0.0029(7) -0.0022(7) -0.0057(8) C34 0.0115(9) 0.0113(9) 0.0081(9) -0.0023(7) -0.0009(7) -0.0039(7) C35 0.0095(9) 0.0117(9) 0.0081(8) -0.0028(7) -0.0005(7) -0.0029(7) C36 0.0081(8) 0.0108(9) 0.0107(9) -0.0022(7) 0.0010(7) -0.0035(7) C37 0.0091(9) 0.0103(9) 0.0102(9) -0.0031(7) 0.0009(7) -0.0019(7) C38 0.0073(8) 0.0112(9) 0.0104(9) -0.0029(7) -0.0002(7) -0.0001(7) C39 0.0048(8) 0.0130(9) 0.0137(9) -0.0031(8) 0.0003(7) -0.0014(7) C40 0.0074(8) 0.0128(9) 0.0133(9) -0.0024(8) -0.0025(7) -0.0030(7) C41 0.0078(9) 0.0132(9) 0.0136(9) -0.0043(8) -0.0012(7) -0.0048(7) C42 0.0092(9) 0.0101(9) 0.0138(9) -0.0026(7) -0.0019(7) -0.0031(7) C43 0.0097(9) 0.0089(9) 0.0144(9) -0.0032(7) 0.0020(7) -0.0042(7) C44 0.0112(9) 0.0079(8) 0.0133(9) -0.0036(7) 0.0026(7) -0.0038(7) C45 0.0108(9) 0.0068(8) 0.0130(9) -0.0032(7) 0.0037(7) -0.0015(7) C46 0.0102(9) 0.0080(8) 0.0137(9) 0.0001(7) 0.0004(7) -0.0025(7) C47 0.0065(8) 0.0079(8) 0.0165(10) -0.0003(7) -0.0002(7) -0.0003(7) C48 0.0072(8) 0.0103(9) 0.0125(9) 0.0024(7) -0.0023(7) 0.0003(7) C49 0.0118(9) 0.0094(9) 0.0114(9) 0.0026(7) -0.0007(7) -0.0017(7) C50 0.0093(9) 0.0125(9) 0.0093(9) 0.0015(7) -0.0011(7) -0.0038(7) C51 0.0105(9) 0.0118(9) 0.0077(8) 0.0001(7) 0.0012(7) -0.0035(7) C52 0.0090(9) 0.0133(9) 0.0103(9) -0.0004(7) 0.0034(7) -0.0044(7) C53 0.0077(8) 0.0117(9) 0.0132(9) -0.0020(7) 0.0034(7) -0.0039(7) C54 0.0057(8) 0.0120(9) 0.0149(10) -0.0026(8) 0.0011(7) -0.0038(7) C55 0.0060(8) 0.0134(9) 0.0152(10) -0.0042(8) 0.0007(7) -0.0056(7) C56 0.0081(9) 0.0108(9) 0.0158(10) -0.0027(8) 0.0019(7) -0.0063(7) C57 0.0121(9) 0.0064(8) 0.0160(10) -0.0025(7) 0.0019(8) -0.0043(7) C58 0.0103(9) 0.0062(8) 0.0145(9) -0.0006(7) 0.0023(7) -0.0025(7) C59 0.0104(9) 0.0078(8) 0.0113(9) 0.0019(7) 0.0012(7) -0.0025(7) C60 0.0095(9) 0.0097(9) 0.0132(9) 0.0011(7) 0.0025(7) -0.0045(7) C071 0.0201(11) 0.0147(10) 0.0099(9) 0.0000(8) -0.0012(8) -0.0033(9) C072 0.0305(18) 0.0166(14) 0.0128(13) -0.0037(11) -0.0081(13) -0.0002(14) C073 0.0203(13) 0.0165(13) 0.0112(12) -0.0006(10) -0.0032(10) -0.0012(11) C074 0.031(13) 0.037(12) 0.022(10) -0.005(9) -0.003(10) 0.017(11) C075 0.057(15) 0.032(11) 0.016(9) -0.013(8) 0.022(10) -0.010(11) C076 0.0201(11) 0.0147(10) 0.0099(9) 0.0000(8) -0.0012(8) -0.0033(9) C161 0.0123(9) 0.0141(9) 0.0142(10) -0.0068(8) 0.0037(8) -0.0068(8) C162 0.0194(11) 0.0146(10) 0.0225(11) -0.0090(9) 0.0001(9) -0.0051(9) C163 0.0173(10) 0.0166(10) 0.0170(10) -0.0045(8) 0.0002(8) -0.0095(9) C361 0.0098(9) 0.0108(9) 0.0129(9) -0.0039(7) 0.0012(7) -0.0039(7) C362 0.0132(10) 0.0184(10) 0.0138(10) -0.0047(8) 0.0040(8) -0.0028(8) C363 0.0106(9) 0.0183(10) 0.0165(10) -0.0058(8) 0.0033(8) -0.0061(8) C431 0.0143(10) 0.0128(10) 0.0194(10) -0.0067(8) 0.0025(8) -0.0075(8) C432 0.0237(12) 0.0173(11) 0.0192(11) -0.0070(9) 0.0024(9) -0.0115(9) C433 0.0198(11) 0.0213(11) 0.0292(13) -0.0122(10) 0.0055(10) -0.0133(10) C461 0.0126(9) 0.0084(9) 0.0202(11) -0.0009(8) 0.0011(8) -0.0037(8) C462 0.0184(11) 0.0095(10) 0.0304(13) -0.0040(9) 0.0046(10) -0.0005(8) C463 0.0215(12) 0.0118(10) 0.0256(12) 0.0011(9) -0.0006(10) -0.0001(9) F011 0.0220(7) 0.0251(7) 0.0176(7) 0.0076(6) -0.0033(6) -0.0090(6) F015 0.0242(8) 0.0212(7) 0.0278(8) 0.0006(6) 0.0101(6) -0.0135(6) F071 0.0164(8) 0.0229(9) 0.0119(8) 0.0020(6) 0.0035(6) -0.0039(7) F072 0.057(9) 0.036(7) 0.013(5) 0.002(5) -0.001(5) -0.025(7) F073 0.0455(19) 0.0143(10) 0.0153(11) -0.0062(8) -0.0034(13) 0.0013(12) F074 0.0523(11) 0.0272(8) 0.0100(7) -0.0045(6) -0.0030(7) -0.0026(8) F075 0.0366(11) 0.0338(11) 0.0261(10) -0.0061(8) -0.0102(8) -0.0173(9) F076 0.0332(10) 0.0115(8) 0.0209(9) -0.0004(6) -0.0051(7) -0.0016(7) F077 0.0325(16) 0.0226(12) 0.0117(9) 0.0023(8) -0.0071(10) 0.0034(10) F078 0.0159(11) 0.0285(17) 0.0219(17) 0.0020(12) -0.0025(13) -0.0003(12) F079 0.049(8) 0.053(9) 0.033(7) -0.017(6) 0.015(6) -0.009(7) F080 0.053(13) 0.021(8) 0.029(8) -0.003(6) 0.017(10) -0.016(9) F081 0.0523(11) 0.0272(8) 0.0100(7) -0.0045(6) -0.0030(7) -0.0026(8) F082 0.047(13) 0.048(12) 0.023(8) -0.002(7) -0.013(8) -0.004(8) F083 0.030(7) 0.070(10) 0.032(7) -0.010(7) -0.006(5) -0.011(7) F084 0.034(9) 0.046(16) 0.022(9) -0.009(8) -0.004(7) 0.005(10) F112 0.0574(11) 0.0143(7) 0.0264(8) -0.0011(6) 0.0161(8) -0.0191(7) F113 0.0594(12) 0.0354(9) 0.0264(8) -0.0041(7) -0.0044(8) -0.0338(9) F114 0.0562(11) 0.0146(7) 0.0373(9) -0.0116(7) 0.0288(9) -0.0163(7) F116 0.0363(9) 0.0248(8) 0.0246(8) -0.0118(6) 0.0139(7) -0.0149(7) F117 0.0174(7) 0.0277(8) 0.0303(8) 0.0061(7) 0.0018(6) -0.0035(6) F161 0.0179(7) 0.0256(7) 0.0190(7) -0.0130(6) 0.0092(5) -0.0130(6) F162 0.0335(8) 0.0134(6) 0.0211(7) -0.0018(5) 0.0029(6) -0.0073(6) F163 0.0388(9) 0.0130(7) 0.0312(8) -0.0112(6) -0.0028(7) -0.0050(6) F164 0.0182(7) 0.0207(7) 0.0395(9) -0.0092(7) -0.0072(7) 0.0023(6) F165 0.0217(7) 0.0188(7) 0.0189(7) -0.0019(5) -0.0073(6) -0.0088(6) F166 0.0285(8) 0.0234(7) 0.0224(7) -0.0127(6) -0.0002(6) -0.0142(6) F167 0.0181(7) 0.0290(8) 0.0250(7) -0.0051(6) 0.0042(6) -0.0156(6) F361 0.0143(6) 0.0104(6) 0.0192(6) -0.0051(5) 0.0039(5) -0.0047(5) F362 0.0162(7) 0.0335(8) 0.0145(7) -0.0054(6) -0.0019(5) -0.0081(6) F363 0.0193(7) 0.0258(7) 0.0140(6) -0.0059(6) 0.0086(5) -0.0036(6) F364 0.0263(7) 0.0157(6) 0.0166(7) 0.0010(5) 0.0038(6) -0.0018(6) F365 0.0107(6) 0.0327(8) 0.0246(7) -0.0138(6) 0.0050(5) -0.0021(6) F366 0.0192(7) 0.0237(7) 0.0273(8) -0.0047(6) 0.0049(6) -0.0137(6) F367 0.0106(6) 0.0246(7) 0.0176(7) -0.0055(6) -0.0017(5) -0.0038(5) F431 0.0240(7) 0.0097(6) 0.0282(8) -0.0034(5) -0.0026(6) -0.0046(5) F432 0.0344(9) 0.0269(8) 0.0254(8) -0.0152(6) 0.0036(7) -0.0190(7) F433 0.0461(10) 0.0216(8) 0.0201(7) -0.0037(6) -0.0067(7) -0.0116(7) F434 0.0263(8) 0.0383(9) 0.0294(8) -0.0206(7) 0.0134(7) -0.0182(7) F435 0.0354(9) 0.0519(11) 0.0336(9) -0.0249(8) 0.0193(7) -0.0341(9) F436 0.0325(9) 0.0329(9) 0.0446(10) -0.0203(8) 0.0132(8) -0.0269(8) F437 0.0155(7) 0.0365(9) 0.0531(11) -0.0143(8) -0.0030(7) -0.0089(7) F461 0.0161(7) 0.0114(6) 0.0425(9) -0.0021(6) 0.0007(6) -0.0071(5) F462 0.0381(9) 0.0182(7) 0.0262(8) -0.0082(6) -0.0002(7) -0.0014(7) F463 0.0193(7) 0.0202(7) 0.0443(10) -0.0071(7) 0.0154(7) -0.0065(6) F464 0.0307(8) 0.0106(7) 0.0368(9) -0.0040(6) 0.0081(7) 0.0054(6) F465 0.0401(9) 0.0196(7) 0.0201(8) 0.0033(6) 0.0026(7) 0.0040(7) F466 0.0343(9) 0.0101(6) 0.0336(9) 0.0055(6) -0.0020(7) 0.0015(6) F467 0.0223(8) 0.0229(8) 0.0414(10) -0.0023(7) -0.0120(7) -0.0009(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C9 1.529(3) . ? C1 C5 1.553(3) . ? C1 C2 1.555(3) . ? C1 C011 1.577(3) . ? C2 C12 1.388(3) . ? C2 C3 1.423(3) . ? C3 C15 1.389(3) . ? C3 C4 1.471(3) . ? C4 C18 1.388(3) . ? C4 C5 1.436(3) . ? C5 C6 1.374(3) . ? C6 C20 1.438(3) . ? C6 C7 1.558(3) . ? C7 C8 1.520(3) . ? C7 C22 1.561(3) . ? C7 C071 1.582(3) . ? C8 C9 1.364(3) . ? C8 C25 1.467(3) . ? C9 C10 1.471(3) . ? C10 C11 1.378(3) . ? C10 C26 1.448(3) . ? C11 C29 1.442(3) . ? C11 C12 1.479(3) . ? C011 F011 1.370(3) . ? C011 C012 1.551(3) . ? C011 C013 1.553(3) . ? C12 C13 1.427(3) . ? C012 F114 1.322(3) . ? C012 F112 1.326(3) . ? C012 F113 1.350(4) . ? C13 C14 1.410(3) . ? C13 C30 1.451(3) . ? C013 F015 1.326(3) . ? C013 F117 1.329(3) . ? C013 F116 1.334(3) . ? C14 C15 1.414(3) . ? C14 C33 1.452(3) . ? C15 C16 1.557(3) . ? C16 C17 1.524(3) . ? C16 C34 1.551(3) . ? C16 C161 1.575(3) . ? C17 C37 1.374(3) . ? C17 C18 1.473(3) . ? C18 C19 1.426(3) . ? C19 C20 1.403(3) . ? C19 C38 1.446(3) . ? C20 C21 1.443(3) . ? C21 C40 1.414(3) . ? C21 C22 1.420(3) . ? C22 C23 1.385(3) . ? C23 C42 1.430(3) . ? C23 C24 1.470(3) . ? C24 C25 1.380(3) . ? C24 C44 1.437(3) . ? C25 C26 1.433(3) . ? C26 C27 1.396(3) . ? C27 C45 1.440(3) . ? C27 C28 1.444(3) . ? C28 C29 1.406(3) . ? C28 C47 1.423(3) . ? C29 C30 1.445(3) . ? C30 C31 1.388(3) . ? C31 C48 1.446(3) . ? C31 C32 1.457(3) . ? C32 C33 1.392(3) . ? C32 C50 1.434(3) . ? C33 C34 1.445(3) . ? C34 C35 1.370(3) . ? C35 C51 1.442(3) . ? C35 C36 1.560(3) . ? C36 C37 1.526(3) . ? C36 C53 1.558(3) . ? C36 C361 1.581(3) . ? C37 C38 1.470(3) . ? C38 C39 1.374(3) . ? C39 C40 1.447(3) . ? C39 C54 1.476(3) . ? C40 C41 1.433(3) . ? C41 C42 1.380(3) . ? C41 C55 1.483(3) . ? C42 C43 1.555(3) . ? C43 C57 1.530(3) . ? C43 C44 1.549(3) . ? C43 C431 1.563(3) . ? C44 C45 1.375(3) . ? C45 C46 1.552(3) . ? C46 C58 1.532(3) . ? C46 C47 1.554(3) . ? C46 C461 1.590(3) . ? C47 C48 1.385(3) . ? C48 C49 1.474(3) . ? C49 C59 1.378(3) . ? C49 C50 1.449(3) . ? C50 C51 1.404(3) . ? C51 C52 1.442(3) . ? C52 C60 1.404(3) . ? C52 C53 1.428(3) . ? C53 C54 1.388(3) . ? C54 C55 1.438(3) . ? C55 C56 1.386(3) . ? C56 C60 1.424(3) . ? C56 C57 1.476(3) . ? C57 C58 1.374(3) . ? C58 C59 1.475(3) . ? C59 C60 1.441(3) . ? C071 F071 1.391(3) . ? C071 C073 1.534(3) . ? C071 C072 1.548(4) . ? C072 F073 1.327(4) . ? C072 F074 1.338(3) . ? C072 F075 1.338(4) . ? C073 F077 1.331(4) . ? C073 F076 1.335(4) . ? C073 F078 1.338(5) . ? C074 F080 1.317(14) . ? C074 F079 1.325(13) . ? C075 F084 1.336(14) . ? C075 F082 1.353(14) . ? C075 F083 1.361(14) . ? C161 F161 1.371(2) . ? C161 C163 1.549(3) . ? C161 C162 1.553(3) . ? C162 F162 1.328(3) . ? C162 F163 1.332(3) . ? C162 F164 1.334(3) . ? C163 F167 1.330(3) . ? C163 F166 1.333(3) . ? C163 F165 1.339(3) . ? C361 F361 1.374(2) . ? C361 C363 1.544(3) . ? C361 C362 1.555(3) . ? C362 F363 1.331(2) . ? C362 F362 1.331(3) . ? C362 F364 1.337(3) . ? C363 F365 1.333(3) . ? C363 F366 1.337(3) . ? C363 F367 1.339(3) . ? C431 F431 1.371(3) . ? C431 C433 1.551(3) . ? C431 C432 1.560(3) . ? C432 F432 1.324(3) . ? C432 F433 1.333(3) . ? C432 F434 1.342(3) . ? C433 F435 1.327(3) . ? C433 F436 1.329(3) . ? C433 F437 1.338(3) . ? C461 F461 1.373(3) . ? C461 C462 1.546(3) . ? C461 C463 1.556(3) . ? C462 F463 1.330(3) . ? C462 F464 1.334(3) . ? C462 F462 1.337(3) . ? C463 F465 1.329(3) . ? C463 F466 1.330(3) . ? C463 F467 1.334(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 C1 C5 106.60(17) . . ? C9 C1 C2 108.62(17) . . ? C5 C1 C2 100.43(16) . . ? C9 C1 C011 113.57(17) . . ? C5 C1 C011 112.63(16) . . ? C2 C1 C011 113.98(18) . . ? C12 C2 C3 119.48(19) . . ? C12 C2 C1 123.15(19) . . ? C3 C2 C1 110.49(18) . . ? C15 C3 C2 121.51(19) . . ? C15 C3 C4 121.02(19) . . ? C2 C3 C4 107.99(18) . . ? C18 C4 C5 121.3(2) . . ? C18 C4 C3 119.24(19) . . ? C5 C4 C3 109.44(18) . . ? C6 C5 C4 119.78(19) . . ? C6 C5 C1 123.99(19) . . ? C4 C5 C1 109.17(19) . . ? C5 C6 C20 119.21(19) . . ? C5 C6 C7 124.14(19) . . ? C20 C6 C7 109.08(19) . . ? C8 C7 C6 106.68(18) . . ? C8 C7 C22 108.76(17) . . ? C6 C7 C22 100.00(16) . . ? C8 C7 C071 111.08(17) . . ? C6 C7 C071 115.42(17) . . ? C22 C7 C071 114.11(18) . . ? C9 C8 C25 108.75(19) . . ? C9 C8 C7 125.10(19) . . ? C25 C8 C7 121.85(19) . . ? C8 C9 C10 108.84(18) . . ? C8 C9 C1 125.09(19) . . ? C10 C9 C1 121.57(19) . . ? C11 C10 C26 119.70(19) . . ? C11 C10 C9 121.80(19) . . ? C26 C10 C9 107.51(19) . . ? C10 C11 C29 120.26(19) . . ? C10 C11 C12 118.85(18) . . ? C29 C11 C12 107.82(18) . . ? F011 C011 C012 105.28(18) . . ? F011 C011 C013 105.81(18) . . ? C012 C011 C013 109.8(2) . . ? F011 C011 C1 108.35(18) . . ? C012 C011 C1 113.70(18) . . ? C013 C011 C1 113.27(17) . . ? C2 C12 C13 119.92(19) . . ? C2 C12 C11 121.12(19) . . ? C13 C12 C11 107.43(18) . . ? F114 C012 F112 107.7(2) . . ? F114 C012 F113 107.6(2) . . ? F112 C012 F113 108.4(2) . . ? F114 C012 C011 111.5(2) . . ? F112 C012 C011 111.3(2) . . ? F113 C012 C011 110.2(2) . . ? C14 C13 C12 119.46(19) . . ? C14 C13 C30 119.99(18) . . ? C12 C13 C30 108.59(19) . . ? F015 C013 F117 108.8(2) . . ? F015 C013 F116 107.9(2) . . ? F117 C013 F116 107.3(2) . . ? F015 C013 C011 111.60(19) . . ? F117 C013 C011 111.0(2) . . ? F116 C013 C011 110.1(2) . . ? C13 C14 C15 120.72(19) . . ? C13 C14 C33 120.10(19) . . ? C15 C14 C33 108.98(18) . . ? C3 C15 C14 118.60(19) . . ? C3 C15 C16 123.40(19) . . ? C14 C15 C16 110.30(17) . . ? C17 C16 C34 106.71(17) . . ? C17 C16 C15 108.83(17) . . ? C34 C16 C15 100.17(16) . . ? C17 C16 C161 112.38(17) . . ? C34 C16 C161 114.00(17) . . ? C15 C16 C161 113.86(17) . . ? C37 C17 C18 108.77(19) . . ? C37 C17 C16 125.26(19) . . ? C18 C17 C16 121.68(18) . . ? C4 C18 C19 119.4(2) . . ? C4 C18 C17 121.3(2) . . ? C19 C18 C17 107.89(18) . . ? C20 C19 C18 119.05(19) . . ? C20 C19 C38 120.86(19) . . ? C18 C19 C38 107.26(18) . . ? C19 C20 C6 121.1(2) . . ? C19 C20 C21 119.05(19) . . ? C6 C20 C21 109.46(18) . . ? C40 C21 C22 120.39(19) . . ? C40 C21 C20 119.81(19) . . ? C22 C21 C20 109.17(19) . . ? C23 C22 C21 118.79(19) . . ? C23 C22 C7 122.84(19) . . ? C21 C22 C7 109.94(18) . . ? C22 C23 C42 121.41(19) . . ? C22 C23 C24 121.8(2) . . ? C42 C23 C24 107.85(18) . . ? C25 C24 C44 121.49(19) . . ? C25 C24 C23 118.71(19) . . ? C44 C24 C23 109.32(18) . . ? C24 C25 C26 118.98(19) . . ? C24 C25 C8 121.57(19) . . ? C26 C25 C8 108.20(19) . . ? C27 C26 C25 119.58(19) . . ? C27 C26 C10 120.7(2) . . ? C25 C26 C10 106.67(18) . . ? C26 C27 C45 120.87(19) . . ? C26 C27 C28 119.49(19) . . ? C45 C27 C28 109.51(18) . . ? C29 C28 C47 121.4(2) . . ? C29 C28 C27 119.43(19) . . ? C47 C28 C27 108.43(19) . . ? C28 C29 C11 120.35(19) . . ? C28 C29 C30 119.08(19) . . ? C11 C29 C30 107.81(18) . . ? C31 C30 C29 119.4(2) . . ? C31 C30 C13 119.83(19) . . ? C29 C30 C13 108.35(18) . . ? C30 C31 C48 120.5(2) . . ? C30 C31 C32 120.10(19) . . ? C48 C31 C32 108.24(18) . . ? C33 C32 C50 119.30(19) . . ? C33 C32 C31 120.64(19) . . ? C50 C32 C31 108.30(19) . . ? C32 C33 C34 121.25(19) . . ? C32 C33 C14 119.32(19) . . ? C34 C33 C14 109.06(18) . . ? C35 C34 C33 119.54(19) . . ? C35 C34 C16 124.06(18) . . ? C33 C34 C16 109.12(17) . . ? C34 C35 C51 119.77(18) . . ? C34 C35 C36 124.24(18) . . ? C51 C35 C36 108.84(18) . . ? C37 C36 C53 108.73(17) . . ? C37 C36 C35 106.68(16) . . ? C53 C36 C35 100.10(16) . . ? C37 C36 C361 112.21(16) . . ? C53 C36 C361 114.01(16) . . ? C35 C36 C361 114.21(17) . . ? C17 C37 C38 108.44(18) . . ? C17 C37 C36 124.45(19) . . ? C38 C37 C36 122.33(18) . . ? C39 C38 C19 120.02(19) . . ? C39 C38 C37 120.95(19) . . ? C19 C38 C37 107.63(18) . . ? C38 C39 C40 120.30(19) . . ? C38 C39 C54 119.48(19) . . ? C40 C39 C54 107.98(18) . . ? C21 C40 C41 119.38(19) . . ? C21 C40 C39 119.9(2) . . ? C41 C40 C39 109.00(18) . . ? C42 C41 C40 120.04(19) . . ? C42 C41 C55 121.21(19) . . ? C40 C41 C55 107.34(18) . . ? C41 C42 C23 119.56(19) . . ? C41 C42 C43 123.10(19) . . ? C23 C42 C43 110.38(17) . . ? C57 C43 C44 106.39(17) . . ? C57 C43 C42 109.34(17) . . ? C44 C43 C42 100.31(16) . . ? C57 C43 C431 113.06(17) . . ? C44 C43 C431 112.71(17) . . ? C42 C43 C431 114.07(18) . . ? C45 C44 C24 119.93(19) . . ? C45 C44 C43 124.61(19) . . ? C24 C44 C43 109.33(17) . . ? C44 C45 C27 119.04(19) . . ? C44 C45 C46 124.42(18) . . ? C27 C45 C46 109.20(19) . . ? C58 C46 C45 106.48(17) . . ? C58 C46 C47 109.53(17) . . ? C45 C46 C47 99.77(16) . . ? C58 C46 C461 111.66(17) . . ? C45 C46 C461 115.56(17) . . ? C47 C46 C461 113.04(17) . . ? C48 C47 C28 119.2(2) . . ? C48 C47 C46 122.53(19) . . ? C28 C47 C46 110.49(19) . . ? C47 C48 C31 120.31(19) . . ? C47 C48 C49 121.5(2) . . ? C31 C48 C49 107.29(18) . . ? C59 C49 C50 120.11(19) . . ? C59 C49 C48 119.6(2) . . ? C50 C49 C48 107.67(18) . . ? C51 C50 C32 119.12(19) . . ? C51 C50 C49 120.4(2) . . ? C32 C50 C49 108.50(18) . . ? C50 C51 C52 119.26(19) . . ? C50 C51 C35 120.89(19) . . ? C52 C51 C35 109.79(18) . . ? C60 C52 C53 120.9(2) . . ? C60 C52 C51 119.84(19) . . ? C53 C52 C51 108.81(18) . . ? C54 C53 C52 118.40(19) . . ? C54 C53 C36 122.97(18) . . ? C52 C53 C36 110.15(18) . . ? C53 C54 C55 120.66(19) . . ? C53 C54 C39 121.31(19) . . ? C55 C54 C39 107.26(18) . . ? C56 C55 C54 120.6(2) . . ? C56 C55 C41 119.19(18) . . ? C54 C55 C41 108.41(18) . . ? C55 C56 C60 119.10(19) . . ? C55 C56 C57 121.25(19) . . ? C60 C56 C57 108.29(18) . . ? C58 C57 C56 108.35(19) . . ? C58 C57 C43 125.06(19) . . ? C56 C57 C43 121.54(18) . . ? C57 C58 C59 108.43(18) . . ? C57 C58 C46 125.05(19) . . ? C59 C58 C46 121.47(19) . . ? C49 C59 C60 120.0(2) . . ? C49 C59 C58 121.01(19) . . ? C60 C59 C58 107.82(19) . . ? C52 C60 C56 120.07(19) . . ? C52 C60 C59 120.4(2) . . ? C56 C60 C59 107.09(18) . . ? F071 C071 C073 105.6(2) . . ? F071 C071 C072 104.3(2) . . ? C073 C071 C072 111.0(2) . . ? F071 C071 C7 108.10(19) . . ? C073 C071 C7 113.76(19) . . ? C072 C071 C7 113.2(2) . . ? F073 C072 F074 107.4(3) . . ? F073 C072 F075 108.2(3) . . ? F074 C072 F075 108.2(3) . . ? F073 C072 C071 111.9(3) . . ? F074 C072 C071 110.3(3) . . ? F075 C072 C071 110.7(3) . . ? F077 C073 F076 107.5(3) . . ? F077 C073 F078 108.1(3) . . ? F076 C073 F078 108.5(3) . . ? F077 C073 C071 112.1(2) . . ? F076 C073 C071 110.2(2) . . ? F078 C073 C071 110.2(3) . . ? F080 C074 F079 109.4(13) . . ? F084 C075 F082 106.0(17) . . ? F084 C075 F083 105.2(16) . . ? F082 C075 F083 103.1(14) . . ? F161 C161 C163 105.26(17) . . ? F161 C161 C162 106.50(17) . . ? C163 C161 C162 110.06(18) . . ? F161 C161 C16 108.09(17) . . ? C163 C161 C16 114.20(18) . . ? C162 C161 C16 112.18(18) . . ? F162 C162 F163 107.8(2) . . ? F162 C162 F164 108.4(2) . . ? F163 C162 F164 107.44(19) . . ? F162 C162 C161 110.83(18) . . ? F163 C162 C161 111.9(2) . . ? F164 C162 C161 110.35(19) . . ? F167 C163 F166 108.71(19) . . ? F167 C163 F165 108.64(19) . . ? F166 C163 F165 107.21(19) . . ? F167 C163 C161 111.08(19) . . ? F166 C163 C161 110.49(19) . . ? F165 C163 C161 110.60(18) . . ? F361 C361 C363 104.66(17) . . ? F361 C361 C362 105.12(17) . . ? C363 C361 C362 110.49(17) . . ? F361 C361 C36 109.02(16) . . ? C363 C361 C36 113.36(17) . . ? C362 C361 C36 113.47(17) . . ? F363 C362 F362 107.64(19) . . ? F363 C362 F364 107.92(18) . . ? F362 C362 F364 108.16(18) . . ? F363 C362 C361 111.72(18) . . ? F362 C362 C361 110.19(18) . . ? F364 C362 C361 111.06(19) . . ? F365 C363 F366 108.11(18) . . ? F365 C363 F367 107.48(18) . . ? F366 C363 F367 107.78(19) . . ? F365 C363 C361 110.87(19) . . ? F366 C363 C361 111.87(18) . . ? F367 C363 C361 110.57(17) . . ? F431 C431 C433 105.46(18) . . ? F431 C431 C432 104.60(17) . . ? C433 C431 C432 109.3(2) . . ? F431 C431 C43 107.89(18) . . ? C433 C431 C43 114.32(18) . . ? C432 C431 C43 114.42(18) . . ? F432 C432 F433 108.1(2) . . ? F432 C432 F434 107.68(19) . . ? F433 C432 F434 108.2(2) . . ? F432 C432 C431 111.79(19) . . ? F433 C432 C431 111.73(19) . . ? F434 C432 C431 109.3(2) . . ? F435 C433 F436 107.4(2) . . ? F435 C433 F437 107.6(2) . . ? F436 C433 F437 108.4(2) . . ? F435 C433 C431 111.4(2) . . ? F436 C433 C431 111.0(2) . . ? F437 C433 C431 111.0(2) . . ? F461 C461 C462 105.21(19) . . ? F461 C461 C463 105.01(18) . . ? C462 C461 C463 110.38(19) . . ? F461 C461 C46 109.48(17) . . ? C462 C461 C46 113.31(17) . . ? C463 C461 C46 112.83(19) . . ? F463 C462 F464 107.8(2) . . ? F463 C462 F462 107.9(2) . . ? F464 C462 F462 107.8(2) . . ? F463 C462 C461 111.3(2) . . ? F464 C462 C461 111.8(2) . . ? F462 C462 C461 110.0(2) . . ? F465 C463 F466 107.9(2) . . ? F465 C463 F467 108.4(2) . . ? F466 C463 F467 108.5(2) . . ? F465 C463 C461 109.87(19) . . ? F466 C463 C461 111.1(2) . . ? F467 C463 C461 111.0(2) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 18.72 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.864 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.165 #===END data_csu005 _database_code_depnum_ccdc_archive 'CCDC 796277' #TrackingRef 'boltalina--1-.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 F14' _chemical_formula_sum 'C66 F14' _chemical_formula_weight 1058.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F -0.0053 0.0125 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 19.622(4) _cell_length_b 17.836(3) _cell_length_c 10.009(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3502.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6518 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 28.63 _exptl_crystal_description 'small plate' _exptl_crystal_colour 'dark red-brown' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 0.205 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9738 _exptl_absorpt_correction_T_max 0.9959 _exptl_absorpt_process_details 'SADABS, v. 2.10, Bruker AXS, Madison, WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator 'Si-<111> channel cut crystal' _diffrn_measurement_device_type 'Bruker APEXII' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 37896 _diffrn_reflns_av_R_equivalents 0.0808 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 29.09 _reflns_number_total 3737 _reflns_number_gt 2799 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2.1-4' _computing_cell_refinement 'Bruker SAINT v7.34A' _computing_data_reduction 'Bruker SAINT v7.34A' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 3737 _refine_ls_number_parameters 462 _refine_ls_number_restraints 276 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.41853(11) 0.16314(14) 1.1073(2) 0.0220(4) Uani 0.825(2) 1 d PU . 1 C2 C 0.45254(11) 0.21194(15) 0.9987(2) 0.0217(4) Uani 0.825(2) 1 d PU . 1 C3 C 0.45292(11) 0.17238(15) 0.8733(2) 0.0264(5) Uani 0.825(2) 1 d PU . 1 C4 C 0.41062(13) 0.10599(15) 0.8851(2) 0.0278(6) Uani 0.825(2) 1 d PU . 1 C5 C 0.38269(12) 0.10355(13) 1.0178(2) 0.0271(5) Uani 0.825(2) 1 d PU . 1 C6 C 0.31672(13) 0.08165(13) 1.0355(2) 0.0285(5) Uani 0.825(2) 1 d PU . 1 C7 C 0.27085(13) 0.12246(15) 1.1261(2) 0.0293(6) Uani 0.825(2) 1 d PU . 1 C8 C 0.29373(14) 0.1853(2) 1.1908(3) 0.0269(8) Uani 0.825(2) 1 d PU . 1 C9 C 0.36416(12) 0.21189(15) 1.1741(2) 0.0217(4) Uani 0.825(2) 1 d PU . 1 C15 C 0.45662(11) 0.21012(15) 0.7527(2) 0.0299(6) Uani 0.825(2) 1 d PU . 1 C16 C 0.41702(12) 0.18409(17) 0.6380(2) 0.0351(6) Uani 0.825(2) 1 d PU . 1 C17 C 0.37617(16) 0.12150(18) 0.6499(3) 0.0349(7) Uani 0.825(2) 1 d PU . 1 C18 C 0.37279(12) 0.08136(13) 0.7755(2) 0.0326(6) Uani 0.825(2) 1 d PU . 1 C19 C 0.30424(14) 0.05598(13) 0.7952(3) 0.0351(5) Uani 0.825(2) 1 d PU . 1 C20 C 0.27641(14) 0.05660(13) 0.9222(3) 0.0350(6) Uani 0.825(2) 1 d PU . 1 C21 C 0.20684(13) 0.08135(14) 0.9425(3) 0.0362(6) Uani 0.825(2) 1 d PU . 1 C22 C 0.20329(16) 0.12198(17) 1.0677(3) 0.0357(7) Uani 0.825(2) 1 d PU . 1 C23 C 0.16147(12) 0.18425(17) 1.0794(3) 0.0375(6) Uani 0.825(2) 1 d PU . 1 C24 C 0.18570(16) 0.2500 1.1486(3) 0.0341(8) Uani 0.825(2) 2 d SPU . 1 C25 C 0.25125(19) 0.2500 1.2037(4) 0.0283(9) Uani 0.825(2) 2 d SPU . 1 C34 C 0.39285(16) 0.2500 0.5680(3) 0.0341(8) Uani 0.825(2) 2 d SPU . 1 C35 C 0.32730(18) 0.2500 0.5121(3) 0.0343(9) Uani 0.825(2) 2 d SPU . 1 C36 C 0.28481(13) 0.18395(16) 0.5249(2) 0.0341(5) Uani 0.825(2) 1 d PU . 1 C37 C 0.30846(13) 0.12110(15) 0.5915(3) 0.0340(6) Uani 0.825(2) 1 d PU . 1 C38 C 0.26393(14) 0.08068(15) 0.6811(3) 0.0344(6) Uani 0.825(2) 1 d PU . 1 C39 C 0.19770(13) 0.10483(15) 0.7006(3) 0.0359(5) Uani 0.825(2) 1 d PU . 1 C40 C 0.16795(15) 0.10520(18) 0.8341(3) 0.0372(7) Uani 0.825(2) 1 d PU . 1 C41 C 0.12452(12) 0.17078(17) 0.8464(3) 0.0378(6) Uani 0.825(2) 1 d PU . 1 C42 C 0.12102(12) 0.20932(16) 0.9651(3) 0.0389(7) Uani 0.825(2) 1 d PU . 1 C53 C 0.21570(13) 0.20947(17) 0.5445(2) 0.0319(4) Uani 0.825(2) 1 d PU . 1 C54 C 0.17294(12) 0.17022(17) 0.6309(2) 0.0334(4) Uani 0.825(2) 1 d PU . 1 C55 C 0.12784(12) 0.21115(17) 0.7197(3) 0.0342(5) Uani 0.825(2) 1 d PU . 1 C101 C 0.4176(2) 0.1630(4) 1.1075(4) 0.0220(4) Uani 0.175(2) 1 d PGU . 2 C102 C 0.3730(2) 0.1036(3) 1.0357(4) 0.0271(5) Uani 0.175(2) 1 d PGU . 2 C103 C 0.3033(2) 0.1060(3) 1.0940(4) 0.024(2) Uani 0.175(2) 1 d PGU . 2 C104 C 0.2979(3) 0.1741(4) 1.1801(3) 0.023(4) Uani 0.175(2) 1 d PGU . 2 C105 C 0.3627(3) 0.2120(4) 1.1755(4) 0.0217(4) Uani 0.175(2) 1 d PGU . 2 C109 C 0.4510(2) 0.2116(4) 1.0003(5) 0.0217(4) Uani 0.175(2) 1 d PGU . 2 C110 C 0.45810(18) 0.1834(4) 0.8638(5) 0.0264(5) Uani 0.175(2) 1 d PGU . 2 C111 C 0.42471(18) 0.1220(3) 0.8206(5) 0.027(2) Uani 0.175(2) 1 d PGU . 2 C112 C 0.3806(2) 0.0826(3) 0.9083(4) 0.027(2) Uani 0.175(2) 1 d PGU . 2 C113 C 0.3198(2) 0.0569(2) 0.8281(4) 0.0351(5) Uani 0.175(2) 1 d PGU . 2 C114 C 0.2588(2) 0.0564(2) 0.8909(4) 0.0350(6) Uani 0.175(2) 1 d PGU . 2 C115 C 0.2479(2) 0.0818(3) 1.0222(4) 0.032(2) Uani 0.175(2) 1 d PGU . 2 C116 C 0.1857(2) 0.1218(3) 1.0343(4) 0.040(3) Uani 0.175(2) 1 d PGU . 2 C117 C 0.1763(2) 0.1844(4) 1.1076(5) 0.0375(6) Uani 0.175(2) 1 d PGU . 2 C118 C 0.2376(3) 0.2118(4) 1.1874(4) 0.030(3) Uani 0.175(2) 1 d PGU . 2 C126 C 0.4641(2) 0.2500(4) 0.7762(6) 0.021(3) Uani 0.175(2) 2 d SPGU . 2 C127 C 0.4363(3) 0.2500(4) 0.6511(6) 0.027(3) Uani 0.175(2) 2 d SPGU . 2 C128 C 0.4020(2) 0.1844(3) 0.6072(4) 0.0278(6) Uani 0.175(2) 1 d PGU . 2 C129 C 0.3931(2) 0.1220(3) 0.6831(4) 0.031(3) Uani 0.175(2) 1 d PGU . 2 C130 C 0.3312(2) 0.0818(3) 0.6949(4) 0.033(2) Uani 0.175(2) 1 d PGU . 2 C131 C 0.2760(2) 0.1050(3) 0.6217(4) 0.030(2) Uani 0.175(2) 1 d PGU . 2 C132 C 0.2062(2) 0.1050(4) 0.6821(4) 0.0359(5) Uani 0.175(2) 1 d PGU . 2 C133 C 0.1974(2) 0.0818(3) 0.8109(5) 0.036(2) Uani 0.175(2) 1 d PGU . 2 C134 C 0.15388(18) 0.1203(4) 0.8959(5) 0.036(2) Uani 0.175(2) 1 d PGU . 2 C135 C 0.11955(18) 0.1823(4) 0.8516(6) 0.0378(6) Uani 0.175(2) 1 d PGU . 2 C136 C 0.1133(2) 0.2500(4) 0.9389(7) 0.035(4) Uani 0.175(2) 2 d SPGU . 2 C137 C 0.1420(3) 0.2500(4) 1.0640(6) 0.038(3) Uani 0.175(2) 2 d SPGU . 2 C147 C 0.3411(3) 0.2113(4) 0.5254(4) 0.0343(9) Uani 0.175(2) 1 d PGU . 2 C148 C 0.2814(3) 0.1728(4) 0.5332(3) 0.0341(5) Uani 0.175(2) 1 d PGU . 2 C149 C 0.2163(3) 0.2110(4) 0.5431(4) 0.0319(4) Uani 0.175(2) 1 d PGU . 2 C150 C 0.1718(2) 0.1705(4) 0.6318(5) 0.0334(4) Uani 0.175(2) 1 d PGU . 2 C151 C 0.1279(2) 0.2099(5) 0.7174(6) 0.0342(5) Uani 0.175(2) 1 d PGU . 2 C201 C 0.46982(9) 0.12835(10) 1.21181(18) 0.0282(4) Uani 1 1 d U . . C202 C 0.54002(10) 0.11085(11) 1.1526(2) 0.0326(4) Uani 1 1 d U . . C203 C 0.44154(11) 0.05885(11) 1.2848(2) 0.0349(5) Uani 1 1 d U . . F1 F 0.48169(6) 0.17997(6) 1.31065(11) 0.0371(3) Uani 1 1 d U . . F2 F 0.57895(6) 0.07376(6) 1.24028(13) 0.0450(3) Uani 1 1 d U . . F3 F 0.57277(5) 0.17405(6) 1.12280(13) 0.0419(3) Uani 1 1 d U . . F4 F 0.53570(6) 0.06980(6) 1.04276(12) 0.0382(3) Uani 1 1 d U . . F5 F 0.47644(7) 0.04445(7) 1.39581(12) 0.0534(4) Uani 1 1 d U . . F6 F 0.44428(6) -0.00178(6) 1.20700(12) 0.0398(3) Uani 1 1 d U . . F7 F 0.37680(6) 0.06933(7) 1.32083(12) 0.0428(3) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0255(9) 0.0196(9) 0.0209(9) 0.0003(7) -0.0045(7) 0.0011(7) C2 0.0164(8) 0.0282(9) 0.0206(9) -0.0010(7) -0.0030(6) 0.0014(7) C3 0.0180(9) 0.0372(12) 0.0240(9) -0.0056(8) -0.0012(7) 0.0090(8) C4 0.0281(14) 0.0285(14) 0.0267(13) -0.0076(11) -0.0050(11) 0.0105(10) C5 0.0361(12) 0.0157(9) 0.0297(11) -0.0001(8) -0.0114(9) 0.0018(8) C6 0.0385(14) 0.0180(12) 0.0292(14) 0.0046(10) -0.0071(10) -0.0039(10) C7 0.0337(14) 0.0306(14) 0.0236(12) 0.0104(10) 0.0006(11) -0.0100(11) C8 0.0287(16) 0.0372(17) 0.0149(19) 0.0055(14) 0.0016(13) -0.0057(13) C9 0.0253(9) 0.0264(9) 0.0135(8) 0.0005(7) -0.0033(7) -0.0008(7) C15 0.0170(11) 0.0490(16) 0.0237(12) -0.0058(11) 0.0040(8) 0.0050(10) C16 0.0243(12) 0.0619(18) 0.0192(11) -0.0089(11) 0.0059(9) 0.0096(12) C17 0.0351(15) 0.0443(17) 0.0252(13) -0.0161(11) -0.0016(12) 0.0125(12) C18 0.0398(14) 0.0278(12) 0.0301(12) -0.0138(10) -0.0067(10) 0.0117(10) C19 0.0465(14) 0.0216(10) 0.0372(14) -0.0087(9) -0.0107(11) 0.0015(10) C20 0.0459(15) 0.0206(10) 0.0385(14) 0.0026(9) -0.0105(11) -0.0079(10) C21 0.0370(14) 0.0334(13) 0.0382(14) 0.0070(11) -0.0081(11) -0.0195(10) C22 0.0313(14) 0.0446(17) 0.0313(14) 0.0098(12) 0.0026(12) -0.0178(12) C23 0.0240(12) 0.0597(14) 0.0289(12) 0.0075(11) 0.0086(10) -0.0123(11) C24 0.0225(16) 0.057(2) 0.0225(16) 0.000 0.0095(13) 0.000 C25 0.0283(19) 0.043(3) 0.0136(16) 0.000 0.0029(14) 0.000 C34 0.0248(16) 0.062(2) 0.0155(15) 0.000 0.0056(13) 0.000 C35 0.0350(17) 0.057(3) 0.0108(13) 0.000 -0.0001(12) 0.000 C36 0.0323(10) 0.0530(14) 0.0168(9) -0.0115(9) -0.0053(8) 0.0016(10) C37 0.0370(15) 0.0427(15) 0.0224(12) -0.0160(11) -0.0054(11) 0.0026(12) C38 0.0424(15) 0.0304(14) 0.0305(15) -0.0136(11) -0.0100(11) -0.0040(11) C39 0.0371(12) 0.0353(11) 0.0354(12) -0.0065(9) -0.0142(10) -0.0129(9) C40 0.0318(15) 0.0418(16) 0.0382(16) 0.0001(13) -0.0065(13) -0.0189(12) C41 0.0183(10) 0.0585(16) 0.0368(11) 0.0045(10) -0.0035(8) -0.0147(9) C42 0.0159(12) 0.0652(19) 0.0356(13) 0.0029(13) 0.0050(10) -0.0088(12) C53 0.0285(10) 0.0490(11) 0.0183(9) -0.0050(8) -0.0096(7) -0.0018(8) C54 0.0252(10) 0.0455(12) 0.0294(10) -0.0055(9) -0.0129(8) -0.0061(8) C55 0.0174(9) 0.0546(12) 0.0305(10) -0.0002(9) -0.0079(7) -0.0057(8) C101 0.0255(9) 0.0196(9) 0.0209(9) 0.0003(7) -0.0045(7) 0.0011(7) C102 0.0361(12) 0.0157(9) 0.0297(11) -0.0001(8) -0.0114(9) 0.0018(8) C103 0.036(5) 0.016(6) 0.022(6) 0.005(4) 0.002(4) -0.004(5) C104 0.030(6) 0.026(8) 0.014(9) 0.012(5) 0.003(6) 0.005(5) C105 0.0253(9) 0.0264(9) 0.0135(8) 0.0005(7) -0.0033(7) -0.0008(7) C109 0.0164(8) 0.0282(9) 0.0206(9) -0.0010(7) -0.0030(6) 0.0014(7) C110 0.0180(9) 0.0372(12) 0.0240(9) -0.0056(8) -0.0012(7) 0.0090(8) C111 0.029(5) 0.023(5) 0.030(5) -0.005(4) -0.002(4) 0.017(4) C112 0.026(5) 0.016(5) 0.038(5) -0.001(4) -0.005(4) 0.010(4) C113 0.0465(14) 0.0216(10) 0.0372(14) -0.0087(9) -0.0107(11) 0.0015(10) C114 0.0459(15) 0.0206(10) 0.0385(14) 0.0026(9) -0.0105(11) -0.0079(10) C115 0.040(5) 0.021(5) 0.035(5) 0.018(4) -0.004(4) -0.017(4) C116 0.025(6) 0.058(7) 0.037(6) 0.010(5) 0.001(5) -0.023(5) C117 0.0240(12) 0.0597(14) 0.0289(12) 0.0075(11) 0.0086(10) -0.0123(11) C118 0.026(5) 0.055(9) 0.007(5) -0.007(5) 0.008(4) -0.004(5) C126 0.010(7) 0.028(8) 0.024(6) 0.000 0.000(5) 0.000 C127 0.019(7) 0.043(7) 0.020(6) 0.000 0.010(5) 0.000 C128 0.0281(14) 0.0285(14) 0.0267(13) -0.0076(11) -0.0050(11) 0.0105(10) C129 0.029(6) 0.034(6) 0.029(6) -0.017(4) 0.002(5) 0.005(5) C130 0.037(5) 0.027(5) 0.034(5) -0.016(4) -0.006(4) 0.007(4) C131 0.031(6) 0.031(6) 0.027(7) -0.014(4) -0.005(5) -0.001(5) C132 0.0371(12) 0.0353(11) 0.0354(12) -0.0065(9) -0.0142(10) -0.0129(9) C133 0.033(6) 0.033(6) 0.042(5) 0.000(5) -0.011(5) -0.021(4) C134 0.022(5) 0.045(6) 0.040(6) 0.006(5) -0.001(4) -0.027(4) C135 0.0183(10) 0.0585(16) 0.0368(11) 0.0045(10) -0.0035(8) -0.0147(9) C136 0.016(8) 0.059(9) 0.030(7) 0.000 0.005(6) 0.000 C137 0.017(7) 0.079(9) 0.018(6) 0.000 0.014(5) 0.000 C147 0.0350(17) 0.057(3) 0.0108(13) 0.000 -0.0001(12) 0.000 C148 0.0323(10) 0.0530(14) 0.0168(9) -0.0115(9) -0.0053(8) 0.0016(10) C149 0.0285(10) 0.0490(11) 0.0183(9) -0.0050(8) -0.0096(7) -0.0018(8) C150 0.0252(10) 0.0455(12) 0.0294(10) -0.0055(9) -0.0129(8) -0.0061(8) C151 0.0174(9) 0.0546(12) 0.0305(10) -0.0002(9) -0.0079(7) -0.0057(8) C201 0.0353(10) 0.0240(9) 0.0253(9) -0.0039(7) -0.0089(8) 0.0045(7) C202 0.0331(10) 0.0267(10) 0.0381(11) -0.0024(8) -0.0115(8) 0.0045(8) C203 0.0467(12) 0.0298(10) 0.0280(10) 0.0050(8) -0.0043(9) 0.0099(9) F1 0.0508(7) 0.0305(6) 0.0299(6) -0.0103(5) -0.0185(5) 0.0109(5) F2 0.0430(7) 0.0390(7) 0.0530(8) -0.0019(6) -0.0222(6) 0.0136(5) F3 0.0295(6) 0.0361(7) 0.0601(8) 0.0017(6) -0.0080(5) 0.0000(5) F4 0.0358(6) 0.0395(6) 0.0391(7) -0.0099(5) -0.0048(5) 0.0084(5) F5 0.0759(9) 0.0499(8) 0.0343(7) 0.0140(6) -0.0169(6) 0.0133(7) F6 0.0539(7) 0.0230(6) 0.0425(7) 0.0010(5) 0.0013(6) 0.0028(5) F7 0.0515(8) 0.0385(7) 0.0385(7) 0.0129(5) 0.0108(6) 0.0082(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C9 1.530(3) . ? C1 C2 1.545(3) . ? C1 C5 1.558(3) . ? C1 C201 1.579(3) . ? C2 C2 1.358(5) 7_565 ? C2 C3 1.440(3) . ? C3 C15 1.384(3) . ? C3 C4 1.451(4) . ? C4 C18 1.395(3) . ? C4 C5 1.438(4) . ? C5 C6 1.364(3) . ? C6 C20 1.453(3) . ? C6 C7 1.470(4) . ? C7 C8 1.370(4) . ? C7 C22 1.449(4) . ? C8 C25 1.429(4) . ? C8 C9 1.470(3) . ? C9 C9 1.359(5) 7_565 ? C15 C15 1.422(5) 7_565 ? C15 C16 1.462(3) . ? C16 C17 1.380(4) . ? C16 C34 1.448(3) . ? C17 C18 1.448(4) . ? C17 C37 1.452(4) . ? C18 C19 1.433(4) . ? C19 C20 1.384(4) . ? C19 C38 1.457(4) . ? C20 C21 1.449(4) . ? C21 C40 1.393(4) . ? C21 C22 1.449(4) . ? C22 C23 1.386(4) . ? C23 C24 1.442(3) . ? C23 C42 1.463(4) . ? C24 C25 1.400(5) . ? C24 C23 1.442(3) 7_565 ? C25 C8 1.429(4) 7_565 ? C34 C35 1.403(5) . ? C34 C16 1.448(3) 7_565 ? C35 C36 1.449(3) . ? C35 C36 1.449(3) 7_565 ? C36 C37 1.385(4) . ? C36 C53 1.444(3) . ? C37 C38 1.444(4) . ? C38 C39 1.383(4) . ? C39 C54 1.443(4) . ? C39 C40 1.458(4) . ? C40 C41 1.452(4) . ? C41 C42 1.374(4) . ? C41 C55 1.460(3) . ? C42 C42 1.451(6) 7_565 ? C53 C54 1.394(3) . ? C53 C53 1.446(6) 7_565 ? C54 C55 1.451(3) . ? C55 C55 1.386(6) 7_565 ? C101 C109 1.5275 . ? C101 C105 1.5461 . ? C101 C102 1.5511 . ? C101 C201 1.587(5) . ? C102 C112 1.3370 . ? C102 C103 1.4873 . ? C103 C115 1.3729 . ? C103 C104 1.4923 . ? C104 C118 1.3635 . ? C104 C105 1.4410 . ? C105 C105 1.357(15) 7_565 ? C109 C109 1.369(15) 7_565 ? C109 C110 1.4621 . ? C110 C111 1.3486 . ? C110 C126 1.4805 . ? C111 C112 1.4194 . ? C111 C129 1.5093 . ? C112 C113 1.5097 . ? C113 C114 1.3526 . ? C113 C130 1.4222 . ? C114 C115 1.4061 . ? C114 C133 1.5154 . ? C115 C116 1.4190 . ? C116 C117 1.3488 . ? C116 C134 1.5203 . ? C117 C137 1.4187 . ? C117 C118 1.5238 . ? C118 C118 1.362(14) 7_565 ? C126 C127 1.3660 . ? C126 C110 1.481(11) 7_565 ? C127 C128 1.4188 . ? C127 C128 1.419(10) 7_565 ? C128 C129 1.3588 . ? C128 C147 1.5267 . ? C129 C130 1.4158 . ? C130 C131 1.3718 . ? C131 C132 1.4970 . ? C131 C148 1.5025 . ? C132 C133 1.3658 . ? C132 C150 1.4393 . ? C133 C134 1.3873 . ? C134 C135 1.3689 . ? C135 C151 1.4394 . ? C135 C136 1.4950 . ? C136 C137 1.3731 . ? C136 C135 1.495(13) 7_565 ? C137 C117 1.419(11) 7_565 ? C147 C148 1.3588 . ? C147 C147 1.382(13) 7_565 ? C148 C149 1.4523 . ? C149 C149 1.392(16) 7_565 ? C149 C150 1.4377 . ? C150 C151 1.4038 . ? C151 C151 1.430(17) 7_565 ? C201 F1 1.371(2) . ? C201 C202 1.532(3) . ? C201 C203 1.542(3) . ? C202 F4 1.323(2) . ? C202 F3 1.331(2) . ? C202 F2 1.339(2) . ? C203 F5 1.331(2) . ? C203 F6 1.333(2) . ? C203 F7 1.334(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 C1 C2 106.77(16) . . ? C9 C1 C5 108.91(17) . . ? C2 C1 C5 100.04(16) . . ? C9 C1 C201 112.26(17) . . ? C2 C1 C201 114.37(17) . . ? C5 C1 C201 113.62(17) . . ? C2 C2 C3 119.34(13) 7_565 . ? C2 C2 C1 124.30(11) 7_565 . ? C3 C2 C1 109.87(18) . . ? C15 C3 C2 121.5(2) . . ? C15 C3 C4 119.9(2) . . ? C2 C3 C4 109.0(2) . . ? C18 C4 C5 120.9(2) . . ? C18 C4 C3 119.8(2) . . ? C5 C4 C3 108.5(2) . . ? C6 C5 C4 119.4(2) . . ? C6 C5 C1 123.3(2) . . ? C4 C5 C1 109.8(2) . . ? C5 C6 C20 120.2(2) . . ? C5 C6 C7 121.3(2) . . ? C20 C6 C7 107.5(2) . . ? C8 C7 C22 119.7(3) . . ? C8 C7 C6 119.7(2) . . ? C22 C7 C6 108.0(2) . . ? C7 C8 C25 120.8(3) . . ? C7 C8 C9 121.2(3) . . ? C25 C8 C9 107.4(3) . . ? C9 C9 C8 108.80(16) 7_565 . ? C9 C9 C1 124.64(11) 7_565 . ? C8 C9 C1 121.5(2) . . ? C3 C15 C15 119.11(15) . 7_565 ? C3 C15 C16 120.2(2) . . ? C15 C15 C16 108.52(15) 7_565 . ? C17 C16 C34 120.6(2) . . ? C17 C16 C15 119.9(2) . . ? C34 C16 C15 107.2(2) . . ? C16 C17 C18 120.1(3) . . ? C16 C17 C37 120.1(3) . . ? C18 C17 C37 107.8(2) . . ? C4 C18 C19 119.4(2) . . ? C4 C18 C17 120.1(2) . . ? C19 C18 C17 108.6(2) . . ? C20 C19 C18 119.6(2) . . ? C20 C19 C38 120.2(2) . . ? C18 C19 C38 107.9(2) . . ? C19 C20 C21 120.2(2) . . ? C19 C20 C6 120.3(2) . . ? C21 C20 C6 108.1(2) . . ? C40 C21 C20 120.0(2) . . ? C40 C21 C22 119.6(3) . . ? C20 C21 C22 108.6(2) . . ? C23 C22 C7 120.2(3) . . ? C23 C22 C21 120.2(3) . . ? C7 C22 C21 107.9(2) . . ? C22 C23 C24 119.8(3) . . ? C22 C23 C42 120.0(3) . . ? C24 C23 C42 107.8(3) . . ? C25 C24 C23 119.48(18) . . ? C25 C24 C23 119.48(18) . 7_565 ? C23 C24 C23 108.8(3) . 7_565 ? C24 C25 C8 120.0(2) . 7_565 ? C24 C25 C8 120.0(2) . . ? C8 C25 C8 107.6(3) 7_565 . ? C35 C34 C16 119.56(17) . 7_565 ? C35 C34 C16 119.56(17) . . ? C16 C34 C16 108.5(3) 7_565 . ? C34 C35 C36 119.49(17) . . ? C34 C35 C36 119.49(17) . 7_565 ? C36 C35 C36 108.8(3) . 7_565 ? C37 C36 C53 120.3(2) . . ? C37 C36 C35 120.5(2) . . ? C53 C36 C35 107.2(2) . . ? C36 C37 C38 120.0(2) . . ? C36 C37 C17 119.8(3) . . ? C38 C37 C17 107.8(2) . . ? C39 C38 C37 120.0(3) . . ? C39 C38 C19 119.6(2) . . ? C37 C38 C19 108.0(2) . . ? C38 C39 C54 120.0(2) . . ? C38 C39 C40 120.5(2) . . ? C54 C39 C40 107.7(2) . . ? C21 C40 C41 120.1(3) . . ? C21 C40 C39 119.5(3) . . ? C41 C40 C39 108.4(2) . . ? C42 C41 C40 120.4(2) . . ? C42 C41 C55 120.4(3) . . ? C40 C41 C55 107.3(2) . . ? C41 C42 C42 120.01(17) . 7_565 ? C41 C42 C23 119.8(3) . . ? C42 C42 C23 107.80(16) 7_565 . ? C54 C53 C36 119.4(2) . . ? C54 C53 C53 120.15(14) . 7_565 ? C36 C53 C53 108.38(15) . 7_565 ? C53 C54 C39 120.2(2) . . ? C53 C54 C55 119.6(2) . . ? C39 C54 C55 108.4(2) . . ? C55 C55 C54 120.20(14) 7_565 . ? C55 C55 C41 119.54(15) 7_565 . ? C54 C55 C41 108.1(2) . . ? C109 C101 C105 106.7 . . ? C109 C101 C102 107.7 . . ? C105 C101 C102 101.3 . . ? C109 C101 C201 114.0(3) . . ? C105 C101 C201 112.3(3) . . ? C102 C101 C201 113.8(4) . . ? C112 C102 C103 119.0 . . ? C112 C102 C101 124.8 . . ? C103 C102 C101 108.5 . . ? C115 C103 C102 120.9 . . ? C115 C103 C104 120.1 . . ? C102 C103 C104 108.4 . . ? C118 C104 C105 122.4 . . ? C118 C104 C103 119.7 . . ? C105 C104 C103 107.4 . . ? C105 C105 C104 118.0 7_565 . ? C105 C105 C101 124.4 7_565 . ? C104 C105 C101 111.4 . . ? C109 C109 C110 110.1 7_565 . ? C109 C109 C101 124.6 7_565 . ? C110 C109 C101 120.1 . . ? C111 C110 C109 122.2 . . ? C111 C110 C126 120.0 . . ? C109 C110 C126 106.6 . . ? C110 C111 C112 120.0 . . ? C110 C111 C129 119.5 . . ? C112 C111 C129 108.3 . . ? C102 C112 C111 121.3 . . ? C102 C112 C113 120.3 . . ? C111 C112 C113 107.6 . . ? C114 C113 C130 125.2 . . ? C114 C113 C112 117.0 . . ? C130 C113 C112 106.3 . . ? C113 C114 C115 124.5 . . ? C113 C114 C133 117.1 . . ? C115 C114 C133 106.1 . . ? C103 C115 C114 118.1 . . ? C103 C115 C116 118.5 . . ? C114 C115 C116 111.8 . . ? C117 C116 C115 125.5 . . ? C117 C116 C134 116.9 . . ? C115 C116 C134 105.5 . . ? C116 C117 C137 125.5 . . ? C116 C117 C118 116.3 . . ? C137 C117 C118 105.7 . . ? C118 C118 C104 119.6 7_565 . ? C118 C118 C117 108.7 7_565 . ? C104 C118 C117 119.9 . . ? C127 C126 C110 120.8 . . ? C127 C126 C110 120.8(3) . 7_565 ? C110 C126 C110 106.6(3) . 7_565 ? C126 C127 C128 118.2 . . ? C126 C127 C128 118.2(2) . 7_565 ? C128 C127 C128 111.1(3) . 7_565 ? C129 C128 C127 124.3 . . ? C129 C128 C147 117.1 . . ? C127 C128 C147 106.2 . . ? C128 C129 C130 124.9 . . ? C128 C129 C111 117.2 . . ? C130 C129 C111 106.1 . . ? C131 C130 C129 118.7 . . ? C131 C130 C113 118.1 . . ? C129 C130 C113 111.8 . . ? C130 C131 C132 120.4 . . ? C130 C131 C148 120.1 . . ? C132 C131 C148 107.7 . . ? C133 C132 C150 121.2 . . ? C133 C132 C131 119.8 . . ? C150 C132 C131 106.7 . . ? C132 C133 C134 120.4 . . ? C132 C133 C114 119.3 . . ? C134 C133 C114 108.3 . . ? C135 C134 C133 120.3 . . ? C135 C134 C116 119.0 . . ? C133 C134 C116 108.3 . . ? C134 C135 C151 121.5 . . ? C134 C135 C136 120.2 . . ? C151 C135 C136 106.2 . . ? C137 C136 C135 120.0 . . ? C137 C136 C135 120.0(3) . 7_565 ? C135 C136 C135 107.6(4) . 7_565 ? C136 C137 C117 118.4(2) . 7_565 ? C136 C137 C117 118.4 . . ? C117 C137 C117 111.1(3) 7_565 . ? C148 C147 C147 120.3 . 7_565 ? C148 C147 C128 119.0 . . ? C147 C147 C128 108.3 7_565 . ? C147 C148 C149 121.7 . . ? C147 C148 C131 120.1 . . ? C149 C148 C131 105.9 . . ? C149 C149 C150 120.1 7_565 . ? C149 C149 C148 118.0 7_565 . ? C150 C149 C148 109.9 . . ? C151 C150 C149 119.8 . . ? C151 C150 C132 118.7 . . ? C149 C150 C132 109.9 . . ? C150 C151 C151 120.0 . 7_565 ? C150 C151 C135 118.0 . . ? C151 C151 C135 110.0 7_565 . ? F1 C201 C202 105.28(15) . . ? F1 C201 C203 105.03(15) . . ? C202 C201 C203 110.08(15) . . ? F1 C201 C1 108.79(15) . . ? C202 C201 C1 113.38(16) . . ? C203 C201 C1 113.59(16) . . ? F1 C201 C101 108.8(3) . . ? C202 C201 C101 113.9(2) . . ? C203 C201 C101 113.1(3) . . ? C1 C201 C101 0.6(3) . . ? F4 C202 F3 108.27(17) . . ? F4 C202 F2 107.92(15) . . ? F3 C202 F2 106.84(15) . . ? F4 C202 C201 112.14(15) . . ? F3 C202 C201 110.38(15) . . ? F2 C202 C201 111.09(17) . . ? F5 C203 F6 108.08(15) . . ? F5 C203 F7 106.92(16) . . ? F6 C203 F7 108.07(17) . . ? F5 C203 C201 111.44(17) . . ? F6 C203 C201 111.16(16) . . ? F7 C203 C201 111.00(15) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 29.09 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.310 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.051 #===END data_ss234m _database_code_depnum_ccdc_archive 'CCDC 796278' #TrackingRef 'boltalina--1-.cif' _audit_update_record ; 2010-07-13 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 F28, 0.5(C7 H2)' _chemical_formula_sum 'C75.50 H F28' _chemical_formula_weight 1439.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 22.645(4) _cell_length_b 10.1528(17) _cell_length_c 23.011(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.435(8) _cell_angle_gamma 90.00 _cell_volume 4777.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9636 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 29.25 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2824 _exptl_absorpt_coefficient_mu 0.193 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8765 _exptl_absorpt_correction_T_max 0.9931 _exptl_absorpt_process_details 'SADABS, v. 2.10, Bruker AXS, Madison, WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEX II diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 118763 _diffrn_reflns_av_R_equivalents 0.1710 _diffrn_reflns_av_sigmaI/netI 0.1383 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.41 _reflns_number_total 9688 _reflns_number_gt 4614 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2, v. 2.0-2, Bruker AXS, 2006' _computing_cell_refinement 'APEX2, v. 2.0-2, Bruker AXS, 2006' _computing_data_reduction 'APEX2, v. 2.0-2, Bruker AXS, 2006' _computing_structure_solution 'SHELXTL, v. 6.14, Bruker AXS' _computing_structure_refinement 'SHELXTL, v. 6.14, Bruker AXS' _computing_molecular_graphics 'SHELXTL, v. 6.14, Bruker AXS' _computing_publication_material 'SHELXTL, v. 6.14, Bruker AXS' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+9.2334P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9688 _refine_ls_number_parameters 1065 _refine_ls_number_restraints 588 _refine_ls_R_factor_all 0.1763 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1759 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5369(2) 0.2332(5) 0.1276(2) 0.0229(10) Uani 1 1 d U . . C2 C 0.4881(2) 0.1179(5) 0.1120(2) 0.0236(10) Uani 1 1 d U . . C3 C 0.5032(2) 0.0396(5) 0.1669(2) 0.0258(11) Uani 1 1 d U . . C4 C 0.5517(2) 0.1075(5) 0.2224(2) 0.0249(11) Uani 1 1 d U . . C5 C 0.5686(2) 0.2299(5) 0.2018(2) 0.0234(10) Uani 1 1 d U . . C6 C 0.5802(2) 0.3395(5) 0.2393(2) 0.0232(10) Uani 1 1 d U . . C7 C 0.5635(2) 0.4811(5) 0.2140(2) 0.0234(10) Uani 1 1 d U . . C8 C 0.5098(2) 0.4696(5) 0.1456(2) 0.0230(10) Uani 1 1 d U . . C9 C 0.4989(2) 0.3614(5) 0.1077(2) 0.0224(10) Uani 1 1 d U . . C10 C 0.4311(2) 0.3656(5) 0.0588(2) 0.0236(10) Uani 1 1 d U . . C11 C 0.3952(2) 0.2545(5) 0.0402(2) 0.0241(10) Uani 1 1 d U . . C12 C 0.4238(2) 0.1281(5) 0.0676(2) 0.0222(10) Uani 1 1 d U . . C13 C 0.3740(2) 0.0536(5) 0.0752(2) 0.0251(11) Uani 1 1 d U A . C14 C 0.3890(2) -0.0295(5) 0.1262(2) 0.0264(11) Uani 1 1 d U . . C15 C 0.4551(2) -0.0362(5) 0.1744(2) 0.0259(11) Uani 1 1 d U . . C16 C 0.4539(2) -0.0456(5) 0.2361(2) 0.0305(11) Uani 1 1 d U A . C17 C 0.5009(2) 0.0170(5) 0.2888(2) 0.0294(11) Uani 1 1 d U . . C18 C 0.5511(2) 0.0956(5) 0.2814(2) 0.0281(11) Uani 1 1 d U . . C19 C 0.5635(2) 0.2097(5) 0.3213(2) 0.0291(11) Uani 1 1 d U A . C20 C 0.5759(2) 0.3291(5) 0.2999(2) 0.0274(11) Uani 1 1 d U . . C21 C 0.5476(2) 0.4485(5) 0.3108(2) 0.0281(11) Uani 1 1 d U A . C22 C 0.5324(2) 0.5352(5) 0.2573(2) 0.0267(11) Uani 1 1 d U . . C23 C 0.4761(2) 0.6064(5) 0.2349(2) 0.0267(11) Uani 1 1 d U A . C24 C 0.4342(2) 0.6189(5) 0.1658(2) 0.0244(11) Uani 1 1 d U A . C25 C 0.4502(2) 0.5501(5) 0.1237(2) 0.0228(10) Uani 1 1 d U . . C26 C 0.4010(2) 0.4855(5) 0.0693(2) 0.0233(10) Uani 1 1 d U . . C27 C 0.3369(2) 0.4895(5) 0.0585(2) 0.0218(10) Uani 1 1 d U A . C28 C 0.2883(2) 0.3769(5) 0.0243(2) 0.0261(11) Uani 1 1 d U . . C29 C 0.3266(2) 0.2511(5) 0.03024(19) 0.0213(10) Uani 1 1 d U A . C30 C 0.3145(2) 0.1346(5) 0.0507(2) 0.0234(10) Uani 1 1 d U . . C31 C 0.2598(2) 0.1106(5) 0.0715(2) 0.0264(11) Uani 1 1 d U A . C32 C 0.2889(2) 0.0375(5) 0.1367(2) 0.0257(11) Uani 1 1 d U . . C33 C 0.3457(2) -0.0349(5) 0.1586(2) 0.0271(11) Uani 1 1 d U A . C34 C 0.3867(2) -0.0459(5) 0.2269(2) 0.0293(11) Uani 1 1 d U . . C35 C 0.3698(2) 0.0184(5) 0.2704(2) 0.0310(12) Uani 1 1 d U A . C36 C 0.4193(2) 0.0856(6) 0.3258(2) 0.0353(12) Uani 1 1 d U . . C37 C 0.4834(2) 0.0843(6) 0.3339(2) 0.0332(12) Uani 1 1 d U A . C38 C 0.5224(2) 0.2037(6) 0.3541(2) 0.0345(12) Uani 1 1 d U . . C39 C 0.4952(2) 0.3187(6) 0.3651(2) 0.0343(12) Uani 1 1 d U A . C40 C 0.5083(2) 0.4436(5) 0.3429(2) 0.0320(12) Uani 1 1 d U . . C41 C 0.4502(2) 0.5211(6) 0.3207(2) 0.0339(12) Uani 1 1 d U A . C42 C 0.4342(2) 0.6025(5) 0.2669(2) 0.0313(12) Uani 1 1 d U . . C43 C 0.3670(2) 0.6102(5) 0.2185(2) 0.0297(11) Uani 1 1 d U A . C44 C 0.3673(2) 0.6195(5) 0.1563(2) 0.0272(11) Uani 1 1 d U . . C45 C 0.3205(2) 0.5521(5) 0.1041(2) 0.0240(10) Uani 1 1 d U A . C46 C 0.2707(2) 0.4762(5) 0.1113(2) 0.0281(11) Uani 1 1 d U . . C47 C 0.2545(2) 0.3632(5) 0.0698(2) 0.0252(11) Uani 1 1 d U A . C48 C 0.2428(2) 0.2444(5) 0.0902(2) 0.0263(11) Uani 1 1 d U . . C49 C 0.2458(2) 0.2345(5) 0.1540(2) 0.0275(11) Uani 1 1 d U A . C50 C 0.2733(2) 0.1085(5) 0.1816(2) 0.0288(11) Uani 1 1 d U A . C51 C 0.3119(2) 0.0975(5) 0.2472(2) 0.0298(11) Uani 1 1 d U . . C52 C 0.3241(2) 0.2121(6) 0.2879(2) 0.0326(12) Uani 1 1 d U A . C53 C 0.3911(2) 0.2042(6) 0.3364(2) 0.0334(12) Uani 1 1 d U A . C54 C 0.4283(2) 0.3191(6) 0.3561(2) 0.0343(12) Uani 1 1 d U . . C55 C 0.4004(3) 0.4458(6) 0.3281(2) 0.0373(13) Uani 1 1 d U A . C56 C 0.3362(2) 0.4522(5) 0.2814(2) 0.0318(12) Uani 1 1 d U . . C58 C 0.2698(2) 0.4680(5) 0.1715(2) 0.0276(11) Uani 1 1 d U A . C59 C 0.2567(2) 0.3442(5) 0.1926(2) 0.0310(11) Uani 1 1 d U . . C60 C 0.2975(2) 0.3343(6) 0.2614(2) 0.0324(12) Uani 1 1 d U A . C61 C 0.5879(2) 0.2152(5) 0.0981(2) 0.0275(11) Uani 1 1 d U . . C62 C 0.5616(2) 0.2648(5) 0.0289(2) 0.0297(12) Uani 1 1 d U . . C63 C 0.6141(2) 0.0756(5) 0.1034(2) 0.0320(12) Uani 1 1 d U . . C67 C 0.3188(2) 0.5363(5) 0.2258(2) 0.0313(11) Uani 1 1 d U A . C71 C 0.6235(2) 0.5636(5) 0.2171(2) 0.0267(11) Uani 1 1 d U . . C72 C 0.6866(3) 0.5385(7) 0.2773(3) 0.0457(14) Uani 1 1 d U . . C73 C 0.6106(2) 0.7112(6) 0.2073(3) 0.0398(13) Uani 1 1 d U . . C81 C 0.2392(2) 0.4103(5) -0.0471(2) 0.0300(11) Uani 0.894(4) 1 d PDU A 1 F811 F 0.18482(17) 0.3318(4) -0.06317(16) 0.0367(9) Uani 0.894(4) 1 d PDU A 1 C82 C 0.2667(3) 0.3755(6) -0.0955(2) 0.0349(13) Uani 0.894(4) 1 d PDU A 1 F821 F 0.22972(17) 0.4207(4) -0.15410(15) 0.0468(11) Uani 0.894(4) 1 d PDU A 1 F822 F 0.27107(18) 0.2455(4) -0.10073(15) 0.0512(11) Uani 0.894(4) 1 d PDU A 1 F823 F 0.3257(2) 0.4263(6) -0.0766(3) 0.0411(13) Uani 0.894(4) 1 d PDU A 1 C83 C 0.2142(3) 0.5502(6) -0.0570(2) 0.0331(13) Uani 0.894(4) 1 d PDU A 1 F831 F 0.1612(2) 0.5665(6) -0.1131(2) 0.0469(12) Uani 0.894(4) 1 d PDU A 1 F832 F 0.25871(18) 0.6347(4) -0.05604(19) 0.0396(11) Uani 0.894(4) 1 d PDU A 1 F833 F 0.1944(6) 0.5860(10) -0.0117(4) 0.0427(10) Uani 0.894(4) 1 d PDU A 1 C81A C 0.2392(2) 0.4103(5) -0.0471(2) 0.0300(11) Uani 0.106(4) 1 d PDU A 2 F814 F 0.2130(16) 0.298(2) -0.0793(14) 0.046(7) Uani 0.106(4) 1 d PDU A 2 C82A C 0.2687(13) 0.504(3) -0.0804(12) 0.0349(13) Uani 0.106(4) 1 d PDU A 2 F824 F 0.2303(15) 0.501(4) -0.1427(12) 0.0468(11) Uani 0.106(4) 1 d PDU A 2 F825 F 0.3269(17) 0.458(6) -0.071(3) 0.0411(13) Uani 0.106(4) 1 d PDU A 2 F826 F 0.2790(18) 0.631(3) -0.0642(18) 0.0396(11) Uani 0.106(4) 1 d PDU A 2 C83A C 0.1791(11) 0.487(3) -0.0500(16) 0.0331(13) Uani 0.106(4) 1 d PDU A 2 F834 F 0.146(2) 0.540(6) -0.109(2) 0.0469(12) Uani 0.106(4) 1 d PDU A 2 F835 F 0.200(5) 0.590(8) -0.010(3) 0.0427(10) Uani 0.106(4) 1 d PDU A 2 F836 F 0.1331(12) 0.430(4) -0.0366(14) 0.068(9) Uani 0.106(4) 1 d PDU A 2 C91 C 0.2000(2) 0.0345(5) 0.0177(2) 0.0292(10) Uani 1 1 d DU . . C92 C 0.1363(4) 0.0591(10) 0.0184(4) 0.038(2) Uani 0.582(5) 1 d PDU A 3 C93 C 0.2125(5) -0.1134(10) 0.0140(5) 0.042(2) Uani 0.582(5) 1 d PDU A 3 C501 C 0.4813(5) 0.8168(9) 0.4453(4) 0.097(3) Uani 1 1 d U B -5 C502 C 0.5432(7) 0.8774(15) 0.4777(8) 0.063(4) Uani 0.50 1 d PDU B -5 H502 H 0.581(4) 0.832(11) 0.482(6) 0.075 Uiso 0.50 1 d PD C -5 C503 C 0.4278(7) 0.9008(19) 0.4488(7) 0.076(4) Uani 0.50 1 d PU B -5 H503 H 0.3831 0.8772 0.4255 0.091 Uiso 0.50 1 calc PR B -5 C504 C 0.5026(10) 1.0637(16) 0.5157(7) 0.075(5) Uani 0.50 1 d PU B -5 C505 C 0.4448(4) 1.0101(10) 0.4858(4) 0.076(2) Uani 1 1 d U B -5 C92A C 0.1492(6) -0.0064(11) 0.0414(6) 0.030(3) Uani 0.418(5) 1 d PDU A 4 C93A C 0.2180(6) -0.0732(13) -0.0135(5) 0.034(3) Uani 0.418(5) 1 d PDU A 4 F611 F 0.64190(12) 0.2912(3) 0.13277(12) 0.0317(7) Uani 1 1 d U . . F621 F 0.55598(14) 0.3959(3) 0.02632(13) 0.0352(7) Uani 1 1 d U . . F622 F 0.50344(14) 0.2144(3) -0.00706(13) 0.0420(8) Uani 1 1 d U . . F623 F 0.60110(14) 0.2333(3) 0.00177(13) 0.0415(8) Uani 1 1 d U . . F631 F 0.66597(13) 0.0693(3) 0.09084(14) 0.0396(8) Uani 1 1 d U . . F632 F 0.56904(14) -0.0065(3) 0.06301(15) 0.0438(8) Uani 1 1 d U . . F633 F 0.63317(14) 0.0285(3) 0.16279(14) 0.0398(7) Uani 1 1 d U . . F711 F 0.63592(14) 0.5265(3) 0.16705(13) 0.0384(7) Uani 1 1 d U . . F721 F 0.73408(14) 0.6184(3) 0.28075(14) 0.0499(9) Uani 1 1 d U . . F722 F 0.70745(14) 0.4141(4) 0.27518(18) 0.0652(11) Uani 1 1 d U . . F723 F 0.67861(15) 0.5495(5) 0.32983(15) 0.0748(13) Uani 1 1 d U . . F731 F 0.65521(14) 0.7712(3) 0.19399(16) 0.0493(9) Uani 1 1 d U . . F732 F 0.61187(18) 0.7681(4) 0.26035(19) 0.0704(11) Uani 1 1 d U . . F733 F 0.55301(14) 0.7380(3) 0.16033(17) 0.0575(10) Uani 1 1 d U . . F911 F 0.1949(3) 0.0779(6) -0.0423(2) 0.0355(15) Uani 0.582(5) 1 d PDU A 3 F912 F 0.1635(3) 0.1289(7) -0.0296(3) 0.0321(19) Uani 0.418(5) 1 d PDU A 4 F921 F 0.0891(10) -0.0216(18) -0.0201(8) 0.042(4) Uani 0.582(5) 1 d PDU A 3 F922 F 0.1172(2) 0.1810(5) 0.0000(2) 0.0428(16) Uani 0.582(5) 1 d PDU A 3 F923 F 0.1393(8) 0.0419(12) 0.0773(5) 0.045(3) Uani 0.582(5) 1 d PDU A 3 F924 F 0.1708(3) -0.1119(7) 0.0806(3) 0.037(2) Uani 0.418(5) 1 d PDU A 4 F925 F 0.1365(13) 0.0885(15) 0.0753(9) 0.042(4) Uani 0.418(5) 1 d PDU A 4 F926 F 0.0921(13) -0.042(2) -0.0058(11) 0.042(5) Uani 0.418(5) 1 d PDU A 4 F931 F 0.2724(7) -0.1452(18) 0.0198(8) 0.046(3) Uani 0.582(5) 1 d PDU A 3 F932 F 0.1697(14) -0.161(4) -0.0432(7) 0.050(2) Uani 0.582(5) 1 d PDU A 3 F933 F 0.2030(3) -0.1807(6) 0.0595(3) 0.0478(17) Uani 0.582(5) 1 d PDU A 3 F934 F 0.2478(3) -0.0223(8) -0.0466(3) 0.049(2) Uani 0.418(5) 1 d PDU A 4 F935 F 0.1682(19) -0.148(5) -0.0526(11) 0.050(2) Uani 0.418(5) 1 d PDU A 4 F936 F 0.2594(8) -0.151(2) 0.0326(9) 0.040(3) Uani 0.418(5) 1 d PDU A 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.019(2) 0.030(3) 0.017(2) -0.001(2) 0.0049(19) -0.003(2) C2 0.024(2) 0.031(3) 0.016(2) -0.004(2) 0.010(2) 0.001(2) C3 0.020(2) 0.028(3) 0.029(3) 0.004(2) 0.011(2) 0.002(2) C4 0.018(2) 0.031(3) 0.023(2) 0.003(2) 0.006(2) 0.009(2) C5 0.016(2) 0.032(3) 0.020(2) 0.004(2) 0.006(2) 0.003(2) C6 0.015(2) 0.033(3) 0.019(2) 0.000(2) 0.005(2) 0.000(2) C7 0.019(2) 0.034(3) 0.014(2) 0.000(2) 0.0040(19) 0.001(2) C8 0.021(2) 0.035(3) 0.013(2) 0.000(2) 0.0077(19) -0.004(2) C9 0.023(2) 0.034(3) 0.014(2) 0.001(2) 0.0116(19) -0.003(2) C10 0.023(2) 0.035(3) 0.013(2) 0.000(2) 0.0079(19) -0.004(2) C11 0.024(2) 0.036(3) 0.012(2) 0.000(2) 0.007(2) -0.001(2) C12 0.024(2) 0.029(3) 0.015(2) -0.006(2) 0.010(2) -0.005(2) C13 0.028(3) 0.031(3) 0.015(2) -0.004(2) 0.007(2) -0.006(2) C14 0.027(3) 0.030(3) 0.025(2) -0.005(2) 0.013(2) -0.006(2) C15 0.025(3) 0.023(3) 0.028(3) 0.003(2) 0.010(2) 0.005(2) C16 0.030(3) 0.030(3) 0.029(3) 0.011(2) 0.010(2) 0.006(2) C17 0.023(3) 0.037(3) 0.023(3) 0.014(2) 0.005(2) 0.010(2) C18 0.021(3) 0.036(3) 0.021(2) 0.009(2) 0.003(2) 0.009(2) C19 0.016(2) 0.046(3) 0.018(2) 0.003(2) 0.000(2) 0.003(2) C20 0.022(3) 0.042(3) 0.008(2) -0.002(2) -0.0037(19) 0.001(2) C21 0.016(2) 0.049(3) 0.012(2) -0.004(2) -0.0008(19) -0.002(2) C22 0.022(3) 0.034(3) 0.018(2) -0.008(2) 0.004(2) -0.002(2) C23 0.024(2) 0.032(3) 0.022(2) -0.009(2) 0.007(2) -0.002(2) C24 0.022(2) 0.024(3) 0.025(2) -0.001(2) 0.008(2) 0.000(2) C25 0.025(2) 0.028(3) 0.016(2) 0.003(2) 0.010(2) -0.005(2) C26 0.025(2) 0.028(3) 0.014(2) 0.0055(19) 0.005(2) -0.001(2) C27 0.020(2) 0.028(3) 0.014(2) 0.0043(19) 0.0045(19) -0.004(2) C28 0.022(2) 0.035(3) 0.018(2) 0.003(2) 0.0059(19) -0.003(2) C29 0.019(2) 0.034(3) 0.007(2) -0.0031(19) 0.0015(18) -0.005(2) C30 0.024(2) 0.033(3) 0.011(2) -0.007(2) 0.006(2) -0.008(2) C31 0.024(2) 0.036(3) 0.014(2) 0.004(2) 0.0031(19) -0.006(2) C32 0.021(3) 0.033(3) 0.021(2) 0.004(2) 0.007(2) -0.009(2) C33 0.027(3) 0.030(3) 0.023(2) 0.003(2) 0.010(2) -0.006(2) C34 0.027(3) 0.035(3) 0.026(3) 0.011(2) 0.011(2) -0.001(2) C35 0.025(3) 0.043(3) 0.022(3) 0.014(2) 0.008(2) -0.002(2) C36 0.034(3) 0.054(3) 0.017(2) 0.012(2) 0.009(2) 0.003(2) C37 0.026(3) 0.052(3) 0.013(2) 0.013(2) 0.000(2) 0.000(2) C38 0.026(3) 0.060(3) 0.009(2) 0.005(2) -0.001(2) 0.002(2) C39 0.030(3) 0.064(3) 0.007(2) -0.003(2) 0.006(2) -0.001(2) C40 0.031(3) 0.048(3) 0.010(2) -0.011(2) 0.002(2) -0.002(2) C41 0.029(3) 0.056(3) 0.016(2) -0.015(2) 0.008(2) -0.002(2) C42 0.033(3) 0.037(3) 0.025(3) -0.016(2) 0.014(2) 0.001(2) C43 0.031(3) 0.030(3) 0.031(3) -0.008(2) 0.016(2) 0.006(2) C44 0.026(3) 0.028(3) 0.027(3) -0.001(2) 0.011(2) 0.005(2) C45 0.020(2) 0.026(3) 0.021(2) 0.006(2) 0.004(2) 0.008(2) C46 0.015(2) 0.044(3) 0.021(2) 0.007(2) 0.003(2) 0.006(2) C47 0.013(2) 0.040(3) 0.019(2) 0.005(2) 0.003(2) 0.001(2) C48 0.012(2) 0.046(3) 0.015(2) 0.000(2) 0.0004(19) -0.002(2) C49 0.018(2) 0.044(3) 0.023(2) 0.001(2) 0.011(2) -0.004(2) C50 0.020(3) 0.043(3) 0.023(2) 0.007(2) 0.010(2) -0.002(2) C51 0.025(3) 0.046(3) 0.021(2) 0.007(2) 0.012(2) -0.003(2) C52 0.027(3) 0.057(3) 0.019(2) 0.003(2) 0.015(2) -0.002(2) C53 0.031(3) 0.060(3) 0.013(2) 0.007(2) 0.012(2) 0.004(2) C54 0.034(3) 0.065(4) 0.004(2) -0.005(2) 0.009(2) 0.004(2) C55 0.039(3) 0.061(4) 0.016(2) -0.009(2) 0.016(2) 0.001(3) C56 0.029(3) 0.047(3) 0.027(3) -0.004(2) 0.020(2) 0.007(2) C58 0.019(3) 0.041(3) 0.025(2) 0.003(2) 0.012(2) 0.009(2) C59 0.024(3) 0.051(3) 0.027(3) 0.003(2) 0.020(2) 0.008(2) C60 0.029(3) 0.053(3) 0.024(3) 0.000(2) 0.019(2) 0.007(2) C61 0.023(3) 0.032(3) 0.027(2) -0.007(2) 0.010(2) -0.005(2) C62 0.024(3) 0.042(3) 0.025(3) -0.009(2) 0.012(2) -0.006(2) C63 0.026(3) 0.041(3) 0.031(3) -0.004(2) 0.014(2) -0.002(2) C67 0.028(3) 0.041(3) 0.029(3) -0.004(2) 0.016(2) 0.009(2) C71 0.029(3) 0.035(3) 0.018(2) -0.006(2) 0.012(2) -0.005(2) C72 0.030(3) 0.063(4) 0.038(3) 0.002(3) 0.009(2) -0.012(3) C73 0.023(3) 0.037(3) 0.054(4) -0.011(3) 0.011(3) -0.012(2) C81 0.020(2) 0.042(3) 0.019(2) 0.003(2) 0.0003(19) -0.011(2) F811 0.025(2) 0.049(2) 0.024(2) 0.0047(16) -0.0009(15) -0.0136(17) C82 0.028(3) 0.054(4) 0.014(3) 0.006(3) 0.000(2) -0.006(3) F821 0.0438(19) 0.073(3) 0.0140(16) 0.0064(18) 0.0028(14) -0.002(2) F822 0.069(3) 0.058(3) 0.0190(17) -0.0055(17) 0.0117(17) 0.001(2) F823 0.0317(17) 0.070(4) 0.021(2) 0.007(2) 0.0100(14) -0.0043(19) C83 0.028(3) 0.048(3) 0.018(3) 0.011(3) 0.005(2) -0.004(3) F831 0.038(3) 0.056(4) 0.0279(18) 0.0147(17) -0.0046(18) -0.006(2) F832 0.036(3) 0.045(2) 0.032(2) 0.0068(15) 0.0094(17) -0.0126(18) F833 0.034(3) 0.059(2) 0.0334(18) 0.0093(16) 0.0130(18) 0.0071(17) C81A 0.020(2) 0.042(3) 0.019(2) 0.003(2) 0.0003(19) -0.011(2) F814 0.03(2) 0.062(13) 0.038(14) -0.017(13) 0.011(13) -0.018(11) C82A 0.028(3) 0.054(4) 0.014(3) 0.006(3) 0.000(2) -0.006(3) F824 0.0438(19) 0.073(3) 0.0140(16) 0.0064(18) 0.0028(14) -0.002(2) F825 0.0317(17) 0.070(4) 0.021(2) 0.007(2) 0.0100(14) -0.0043(19) F826 0.036(3) 0.045(2) 0.032(2) 0.0068(15) 0.0094(17) -0.0126(18) C83A 0.028(3) 0.048(3) 0.018(3) 0.011(3) 0.005(2) -0.004(3) F834 0.038(3) 0.056(4) 0.0279(18) 0.0147(17) -0.0046(18) -0.006(2) F835 0.034(3) 0.059(2) 0.0334(18) 0.0093(16) 0.0130(18) 0.0071(17) F836 0.009(12) 0.12(2) 0.061(19) 0.032(16) 0.001(12) -0.009(12) C91 0.027(2) 0.038(3) 0.016(2) 0.007(2) 0.003(2) -0.006(2) C92 0.031(5) 0.057(7) 0.015(5) 0.012(5) 0.000(4) -0.013(5) C93 0.040(6) 0.044(5) 0.029(6) -0.001(4) 0.002(5) -0.018(5) C501 0.114(7) 0.088(7) 0.096(7) 0.016(5) 0.053(6) -0.013(5) C502 0.055(7) 0.056(9) 0.088(11) 0.030(8) 0.042(8) 0.039(6) C503 0.041(7) 0.123(12) 0.058(9) 0.021(7) 0.017(7) -0.028(7) C504 0.109(12) 0.075(11) 0.054(9) 0.014(7) 0.047(9) -0.022(10) C505 0.066(5) 0.089(6) 0.081(6) 0.035(5) 0.039(5) 0.006(5) C92A 0.023(7) 0.040(8) 0.027(8) 0.002(5) 0.010(6) 0.000(6) C93A 0.016(7) 0.064(9) 0.017(7) -0.014(5) 0.002(5) -0.009(5) F611 0.0248(15) 0.0401(17) 0.0307(15) -0.0091(13) 0.0124(12) -0.0092(13) F621 0.0476(18) 0.0360(18) 0.0333(16) 0.0023(13) 0.0281(14) 0.0021(14) F622 0.0386(17) 0.062(2) 0.0233(15) -0.0065(14) 0.0112(13) -0.0084(16) F623 0.0465(18) 0.052(2) 0.0378(17) -0.0033(15) 0.0293(15) 0.0077(15) F631 0.0300(16) 0.049(2) 0.0447(18) -0.0078(15) 0.0211(14) 0.0049(14) F632 0.0408(18) 0.0383(19) 0.056(2) -0.0191(16) 0.0240(16) -0.0044(15) F633 0.0386(17) 0.0403(18) 0.0453(18) 0.0072(15) 0.0224(15) 0.0098(14) F711 0.0452(18) 0.0427(18) 0.0371(16) -0.0130(14) 0.0268(15) -0.0136(15) F721 0.0267(17) 0.067(2) 0.0411(18) 0.0092(17) 0.0008(14) -0.0141(16) F722 0.0260(18) 0.069(3) 0.084(3) 0.030(2) 0.0082(17) 0.0036(17) F723 0.037(2) 0.151(4) 0.0220(17) -0.003(2) -0.0003(15) -0.029(2) F731 0.0325(17) 0.0376(19) 0.070(2) 0.0050(17) 0.0147(16) -0.0089(15) F732 0.068(2) 0.061(2) 0.092(3) -0.049(2) 0.044(2) -0.022(2) F733 0.0298(18) 0.040(2) 0.085(3) 0.0147(18) 0.0077(17) -0.0011(15) F911 0.037(3) 0.049(4) 0.015(2) 0.004(2) 0.006(2) -0.013(3) F912 0.020(4) 0.049(5) 0.026(4) 0.007(3) 0.008(3) -0.005(3) F921 0.028(4) 0.056(5) 0.028(7) 0.009(5) -0.001(5) -0.017(4) F922 0.027(3) 0.055(4) 0.034(3) 0.010(3) 0.001(2) 0.001(2) F923 0.027(4) 0.076(9) 0.022(4) 0.016(5) 0.002(3) -0.022(6) F924 0.043(4) 0.043(5) 0.027(4) 0.006(3) 0.016(3) -0.007(4) F925 0.045(7) 0.051(8) 0.047(8) -0.011(6) 0.035(6) -0.022(7) F926 0.028(6) 0.067(11) 0.028(9) 0.001(7) 0.008(5) -0.015(7) F931 0.048(5) 0.038(4) 0.050(7) -0.008(4) 0.019(4) -0.004(4) F932 0.043(2) 0.066(6) 0.031(4) -0.017(5) 0.006(4) -0.020(3) F933 0.049(4) 0.044(4) 0.041(3) 0.013(3) 0.010(3) -0.010(3) F934 0.042(5) 0.078(6) 0.035(4) -0.026(4) 0.024(4) -0.023(4) F935 0.043(2) 0.066(6) 0.031(4) -0.017(5) 0.006(4) -0.020(3) F936 0.032(8) 0.046(7) 0.032(7) -0.017(5) 0.005(5) -0.001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C9 1.519(7) . ? C1 C5 1.543(6) . ? C1 C2 1.544(7) . ? C1 C61 1.579(6) . ? C2 C12 1.376(6) . ? C2 C3 1.404(6) . ? C3 C15 1.405(7) . ? C3 C4 1.451(7) . ? C4 C18 1.370(6) . ? C4 C5 1.440(7) . ? C5 C6 1.363(7) . ? C6 C20 1.442(6) . ? C6 C7 1.536(7) . ? C7 C8 1.526(6) . ? C7 C22 1.547(6) . ? C7 C71 1.570(7) . ? C8 C9 1.357(7) . ? C8 C25 1.469(6) . ? C9 C10 1.463(6) . ? C10 C11 1.349(7) . ? C10 C26 1.464(7) . ? C11 C12 1.454(7) . ? C11 C29 1.470(6) . ? C12 C13 1.432(6) . ? C13 C14 1.365(7) . ? C13 C30 1.469(7) . ? C14 C15 1.430(6) . ? C14 C33 1.464(6) . ? C15 C16 1.436(7) . ? C16 C17 1.379(7) . ? C16 C34 1.441(7) . ? C17 C37 1.432(7) . ? C17 C18 1.458(7) . ? C18 C19 1.429(7) . ? C19 C20 1.382(7) . ? C19 C38 1.430(7) . ? C20 C21 1.443(7) . ? C21 C40 1.379(7) . ? C21 C22 1.429(7) . ? C22 C23 1.361(6) . ? C23 C42 1.428(7) . ? C23 C24 1.466(6) . ? C24 C25 1.365(6) . ? C24 C44 1.433(6) . ? C25 C26 1.429(6) . ? C26 C27 1.364(6) . ? C27 C45 1.407(6) . ? C27 C28 1.547(6) . ? C28 C29 1.517(7) . ? C28 C47 1.546(6) . ? C28 C81 1.574(6) . ? C29 C30 1.344(7) . ? C30 C31 1.526(7) . ? C31 C48 1.524(7) . ? C31 C32 1.546(6) . ? C31 C91 1.589(6) . ? C32 C33 1.376(7) . ? C32 C50 1.423(7) . ? C33 C34 1.446(6) . ? C34 C35 1.382(7) . ? C35 C51 1.430(7) . ? C35 C36 1.456(7) . ? C36 C37 1.383(7) . ? C36 C53 1.431(8) . ? C37 C38 1.454(7) . ? C38 C39 1.394(8) . ? C39 C54 1.439(7) . ? C39 C40 1.446(8) . ? C40 C41 1.427(7) . ? C41 C42 1.402(7) . ? C41 C55 1.432(7) . ? C42 C43 1.450(7) . ? C43 C67 1.393(7) . ? C43 C44 1.438(7) . ? C44 C45 1.394(7) . ? C45 C46 1.433(7) . ? C46 C58 1.396(6) . ? C46 C47 1.436(7) . ? C47 C48 1.361(7) . ? C48 C49 1.443(6) . ? C49 C59 1.379(7) . ? C49 C50 1.446(7) . ? C50 C51 1.386(6) . ? C51 C52 1.444(7) . ? C52 C60 1.400(7) . ? C52 C53 1.450(7) . ? C53 C54 1.395(8) . ? C54 C55 1.456(8) . ? C55 C56 1.390(7) . ? C56 C60 1.437(7) . ? C56 C67 1.446(7) . ? C58 C59 1.425(7) . ? C58 C67 1.443(7) . ? C59 C60 1.453(7) . ? C61 F611 1.375(5) . ? C61 C63 1.521(7) . ? C61 C62 1.527(7) . ? C62 F622 1.321(5) . ? C62 F623 1.330(5) . ? C62 F621 1.336(6) . ? C63 F631 1.326(5) . ? C63 F633 1.334(6) . ? C63 F632 1.335(6) . ? C71 F711 1.352(5) . ? C71 C73 1.525(8) . ? C71 C72 1.526(7) . ? C72 F723 1.300(6) . ? C72 F721 1.322(6) . ? C72 F722 1.356(7) . ? C73 F733 1.316(6) . ? C73 F731 1.324(6) . ? C73 F732 1.340(6) . ? C81 F811 1.379(5) . ? C81 C83 1.509(8) . ? C81 C82 1.532(8) . ? C82 F823 1.319(7) . ? C82 F821 1.327(6) . ? C82 F822 1.333(6) . ? C83 F832 1.317(6) . ? C83 F831 1.343(6) . ? C83 F833 1.349(9) . ? C82A F824 1.321(15) . ? C82A F825 1.324(15) . ? C82A F826 1.327(15) . ? C83A F836 1.339(15) . ? C83A F835 1.343(16) . ? C83A F834 1.345(16) . ? C91 F911 1.406(6) . ? C91 F912 1.419(8) . ? C91 C93A 1.460(12) . ? C91 C92 1.472(10) . ? C91 C92A 1.527(12) . ? C91 C93 1.537(11) . ? C92 F922 1.319(9) . ? C92 F921 1.336(11) . ? C92 F923 1.338(11) . ? C93 F933 1.342(9) . ? C93 F932 1.343(11) . ? C93 F931 1.345(11) . ? C501 C502 1.414(18) . ? C501 C503 1.512(19) . ? C502 H502 0.94(2) . ? C503 C505 1.350(19) . ? C503 H503 0.9500 . ? C504 C505 1.306(18) . ? C92A F926 1.332(13) . ? C92A F925 1.346(13) . ? C92A F924 1.348(11) . ? C93A F934 1.320(11) . ? C93A F936 1.334(13) . ? C93A F935 1.338(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 C1 C5 106.5(4) . . ? C9 C1 C2 108.8(4) . . ? C5 C1 C2 100.7(4) . . ? C9 C1 C61 113.2(4) . . ? C5 C1 C61 113.3(4) . . ? C2 C1 C61 113.3(4) . . ? C12 C2 C3 119.0(4) . . ? C12 C2 C1 122.6(4) . . ? C3 C2 C1 110.3(4) . . ? C2 C3 C15 121.1(4) . . ? C2 C3 C4 108.9(4) . . ? C15 C3 C4 119.1(4) . . ? C18 C4 C5 121.3(4) . . ? C18 C4 C3 120.3(4) . . ? C5 C4 C3 109.1(4) . . ? C6 C5 C4 120.1(4) . . ? C6 C5 C1 123.8(4) . . ? C4 C5 C1 108.7(4) . . ? C5 C6 C20 118.6(4) . . ? C5 C6 C7 125.1(4) . . ? C20 C6 C7 109.1(4) . . ? C8 C7 C6 106.1(4) . . ? C8 C7 C22 108.1(4) . . ? C6 C7 C22 101.2(4) . . ? C8 C7 C71 112.2(4) . . ? C6 C7 C71 114.5(4) . . ? C22 C7 C71 113.9(4) . . ? C9 C8 C25 110.0(4) . . ? C9 C8 C7 124.7(4) . . ? C25 C8 C7 121.2(4) . . ? C8 C9 C10 108.2(4) . . ? C8 C9 C1 125.3(4) . . ? C10 C9 C1 121.9(4) . . ? C11 C10 C9 120.7(4) . . ? C11 C10 C26 119.2(4) . . ? C9 C10 C26 107.9(4) . . ? C10 C11 C12 120.3(4) . . ? C10 C11 C29 121.5(4) . . ? C12 C11 C29 107.0(4) . . ? C2 C12 C13 120.4(4) . . ? C2 C12 C11 121.4(4) . . ? C13 C12 C11 106.9(4) . . ? C14 C13 C12 120.9(4) . . ? C14 C13 C30 121.7(4) . . ? C12 C13 C30 107.4(4) . . ? C13 C14 C15 119.2(4) . . ? C13 C14 C33 119.1(4) . . ? C15 C14 C33 108.1(4) . . ? C3 C15 C14 119.2(4) . . ? C3 C15 C16 120.2(4) . . ? C14 C15 C16 108.1(4) . . ? C17 C16 C15 120.3(4) . . ? C17 C16 C34 119.9(5) . . ? C15 C16 C34 108.7(4) . . ? C16 C17 C37 120.5(4) . . ? C16 C17 C18 119.8(4) . . ? C37 C17 C18 107.2(4) . . ? C4 C18 C19 118.9(5) . . ? C4 C18 C17 120.3(4) . . ? C19 C18 C17 108.5(4) . . ? C20 C19 C18 119.8(4) . . ? C20 C19 C38 120.3(5) . . ? C18 C19 C38 108.2(4) . . ? C19 C20 C6 121.1(4) . . ? C19 C20 C21 120.1(4) . . ? C6 C20 C21 109.1(4) . . ? C40 C21 C22 120.8(4) . . ? C40 C21 C20 120.0(5) . . ? C22 C21 C20 109.1(4) . . ? C23 C22 C21 119.5(4) . . ? C23 C22 C7 123.8(4) . . ? C21 C22 C7 109.2(4) . . ? C22 C23 C42 120.8(5) . . ? C22 C23 C24 121.4(4) . . ? C42 C23 C24 107.3(4) . . ? C25 C24 C44 118.7(4) . . ? C25 C24 C23 118.7(4) . . ? C44 C24 C23 108.4(4) . . ? C24 C25 C26 120.8(4) . . ? C24 C25 C8 121.8(4) . . ? C26 C25 C8 107.6(4) . . ? C27 C26 C25 121.0(4) . . ? C27 C26 C10 121.9(4) . . ? C25 C26 C10 106.3(4) . . ? C26 C27 C45 118.6(4) . . ? C26 C27 C28 122.7(4) . . ? C45 C27 C28 110.8(4) . . ? C29 C28 C47 107.0(4) . . ? C29 C28 C27 108.8(4) . . ? C47 C28 C27 100.0(4) . . ? C29 C28 C81 113.3(4) . . ? C47 C28 C81 113.2(4) . . ? C27 C28 C81 113.6(4) . . ? C30 C29 C11 109.1(4) . . ? C30 C29 C28 125.3(4) . . ? C11 C29 C28 121.3(4) . . ? C29 C30 C13 109.6(4) . . ? C29 C30 C31 124.4(4) . . ? C13 C30 C31 121.6(4) . . ? C48 C31 C30 106.6(4) . . ? C48 C31 C32 102.0(4) . . ? C30 C31 C32 108.5(4) . . ? C48 C31 C91 114.8(4) . . ? C30 C31 C91 111.6(4) . . ? C32 C31 C91 112.8(4) . . ? C33 C32 C50 119.3(4) . . ? C33 C32 C31 123.5(4) . . ? C50 C32 C31 109.1(4) . . ? C32 C33 C34 120.1(4) . . ? C32 C33 C14 121.3(4) . . ? C34 C33 C14 107.3(4) . . ? C35 C34 C16 119.7(5) . . ? C35 C34 C33 120.2(4) . . ? C16 C34 C33 107.7(4) . . ? C34 C35 C51 119.4(4) . . ? C34 C35 C36 120.5(4) . . ? C51 C35 C36 107.5(5) . . ? C37 C36 C53 120.3(5) . . ? C37 C36 C35 118.8(5) . . ? C53 C36 C35 108.1(4) . . ? C36 C37 C17 120.6(5) . . ? C36 C37 C38 119.6(5) . . ? C17 C37 C38 108.1(4) . . ? C39 C38 C19 120.0(5) . . ? C39 C38 C37 120.1(5) . . ? C19 C38 C37 108.1(5) . . ? C38 C39 C54 119.8(5) . . ? C38 C39 C40 119.7(4) . . ? C54 C39 C40 108.1(5) . . ? C21 C40 C41 119.8(5) . . ? C21 C40 C39 119.9(5) . . ? C41 C40 C39 108.1(4) . . ? C42 C41 C40 119.4(4) . . ? C42 C41 C55 120.1(4) . . ? C40 C41 C55 108.4(5) . . ? C41 C42 C23 119.6(4) . . ? C41 C42 C43 119.9(5) . . ? C23 C42 C43 108.3(4) . . ? C67 C43 C44 119.6(4) . . ? C67 C43 C42 119.8(5) . . ? C44 C43 C42 108.4(4) . . ? C45 C44 C24 119.5(4) . . ? C45 C44 C43 119.9(4) . . ? C24 C44 C43 107.7(4) . . ? C44 C45 C27 121.2(4) . . ? C44 C45 C46 120.6(4) . . ? C27 C45 C46 108.4(4) . . ? C58 C46 C45 119.7(4) . . ? C58 C46 C47 120.3(5) . . ? C45 C46 C47 110.0(4) . . ? C48 C47 C46 120.7(4) . . ? C48 C47 C28 122.7(4) . . ? C46 C47 C28 108.6(4) . . ? C47 C48 C49 118.8(4) . . ? C47 C48 C31 125.6(4) . . ? C49 C48 C31 108.6(4) . . ? C59 C49 C48 121.1(5) . . ? C59 C49 C50 120.5(4) . . ? C48 C49 C50 109.4(4) . . ? C51 C50 C32 120.8(5) . . ? C51 C50 C49 120.1(5) . . ? C32 C50 C49 108.9(4) . . ? C50 C51 C35 120.0(5) . . ? C50 C51 C52 119.7(5) . . ? C35 C51 C52 108.8(4) . . ? C60 C52 C51 120.4(4) . . ? C60 C52 C53 119.8(5) . . ? C51 C52 C53 107.4(5) . . ? C54 C53 C36 120.6(5) . . ? C54 C53 C52 119.3(5) . . ? C36 C53 C52 108.2(5) . . ? C53 C54 C39 119.7(5) . . ? C53 C54 C55 120.6(4) . . ? C39 C54 C55 107.2(5) . . ? C56 C55 C41 119.9(5) . . ? C56 C55 C54 119.6(5) . . ? C41 C55 C54 108.1(5) . . ? C55 C56 C60 120.1(5) . . ? C55 C56 C67 120.6(5) . . ? C60 C56 C67 108.2(4) . . ? C46 C58 C59 119.0(5) . . ? C46 C58 C67 119.8(4) . . ? C59 C58 C67 108.9(4) . . ? C49 C59 C58 119.9(4) . . ? C49 C59 C60 120.0(5) . . ? C58 C59 C60 107.7(5) . . ? C52 C60 C56 120.6(4) . . ? C52 C60 C59 119.3(5) . . ? C56 C60 C59 107.9(5) . . ? F611 C61 C63 104.9(4) . . ? F611 C61 C62 105.7(4) . . ? C63 C61 C62 110.7(4) . . ? F611 C61 C1 108.5(4) . . ? C63 C61 C1 113.9(4) . . ? C62 C61 C1 112.4(4) . . ? F622 C62 F623 107.7(4) . . ? F622 C62 F621 107.9(4) . . ? F623 C62 F621 106.8(4) . . ? F622 C62 C61 111.2(4) . . ? F623 C62 C61 111.8(4) . . ? F621 C62 C61 111.2(4) . . ? F631 C63 F633 106.2(4) . . ? F631 C63 F632 107.6(4) . . ? F633 C63 F632 107.7(4) . . ? F631 C63 C61 112.3(4) . . ? F633 C63 C61 111.1(4) . . ? F632 C63 C61 111.8(4) . . ? C43 C67 C58 120.4(4) . . ? C43 C67 C56 119.7(4) . . ? C58 C67 C56 107.3(5) . . ? F711 C71 C73 104.1(4) . . ? F711 C71 C72 105.7(4) . . ? C73 C71 C72 110.1(4) . . ? F711 C71 C7 107.8(4) . . ? C73 C71 C7 114.2(4) . . ? C72 C71 C7 114.0(4) . . ? F723 C72 F721 109.0(5) . . ? F723 C72 F722 107.7(5) . . ? F721 C72 F722 106.6(5) . . ? F723 C72 C71 112.3(5) . . ? F721 C72 C71 111.9(5) . . ? F722 C72 C71 109.1(5) . . ? F733 C73 F731 107.5(5) . . ? F733 C73 F732 106.6(5) . . ? F731 C73 F732 107.0(4) . . ? F733 C73 C71 112.6(4) . . ? F731 C73 C71 111.7(4) . . ? F732 C73 C71 111.2(5) . . ? F811 C81 C83 105.6(4) . . ? F811 C81 C82 105.4(4) . . ? C83 C81 C82 110.5(4) . . ? F811 C81 C28 107.7(4) . . ? C83 C81 C28 114.3(4) . . ? C82 C81 C28 112.6(4) . . ? F823 C82 F821 107.9(5) . . ? F823 C82 F822 108.2(5) . . ? F821 C82 F822 106.9(4) . . ? F823 C82 C81 109.8(5) . . ? F821 C82 C81 112.5(5) . . ? F822 C82 C81 111.3(4) . . ? F832 C83 F831 107.3(4) . . ? F832 C83 F833 108.5(5) . . ? F831 C83 F833 104.6(6) . . ? F832 C83 C81 112.1(5) . . ? F831 C83 C81 112.6(5) . . ? F833 C83 C81 111.4(7) . . ? F824 C82A F825 109(2) . . ? F824 C82A F826 107(2) . . ? F825 C82A F826 105(2) . . ? F836 C83A F835 105(3) . . ? F836 C83A F834 105(2) . . ? F835 C83A F834 105(3) . . ? F911 C91 F912 42.3(3) . . ? F911 C91 C93A 70.9(6) . . ? F912 C91 C93A 108.8(6) . . ? F911 C91 C92 106.9(5) . . ? F912 C91 C92 69.1(5) . . ? C93A C91 C92 128.0(7) . . ? F911 C91 C92A 132.8(6) . . ? F912 C91 C92A 100.2(6) . . ? C93A C91 C92A 112.7(7) . . ? C92 C91 C92A 31.7(4) . . ? F911 C91 C93 101.0(5) . . ? F912 C91 C93 132.6(6) . . ? C93A C91 C93 31.1(5) . . ? C92 C91 C93 111.8(6) . . ? C92A C91 C93 86.5(6) . . ? F911 C91 C31 107.2(4) . . ? F912 C91 C31 106.9(5) . . ? C93A C91 C31 115.0(6) . . ? C92 C91 C31 114.9(5) . . ? C92A C91 C31 112.0(6) . . ? C93 C91 C31 113.8(5) . . ? F922 C92 F921 107.7(10) . . ? F922 C92 F923 108.4(8) . . ? F921 C92 F923 105.8(11) . . ? F922 C92 C91 110.0(7) . . ? F921 C92 C91 113.4(14) . . ? F923 C92 C91 111.4(9) . . ? F933 C93 F932 107.0(11) . . ? F933 C93 F931 107.0(9) . . ? F932 C93 F931 106.5(16) . . ? F933 C93 C91 111.0(8) . . ? F932 C93 C91 109(2) . . ? F931 C93 C91 115.6(11) . . ? C502 C501 C503 111.2(11) . . ? C501 C502 H502 120(8) . . ? C505 C503 C501 118.6(11) . . ? C505 C503 H503 120.7 . . ? C501 C503 H503 120.7 . . ? C504 C505 C503 128.6(14) . . ? F926 C92A F925 107.0(16) . . ? F926 C92A F924 106.0(12) . . ? F925 C92A F924 106.7(11) . . ? F926 C92A C91 113.4(18) . . ? F925 C92A C91 113.2(12) . . ? F924 C92A C91 110.0(8) . . ? F934 C93A F936 109.5(10) . . ? F934 C93A F935 109.2(16) . . ? F936 C93A F935 107.2(19) . . ? F934 C93A C91 108.1(9) . . ? F936 C93A C91 107.7(13) . . ? F935 C93A C91 115(3) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.586 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.081 #===END data_ss246 _database_code_depnum_ccdc_archive 'CCDC 796279' #TrackingRef 'boltalina--1-.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 F28, C6 H6' _chemical_formula_sum 'C78 H6 F28' _chemical_formula_weight 1474.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0294(4) _cell_length_b 12.1981(5) _cell_length_c 21.9933(9) _cell_angle_alpha 75.600(2) _cell_angle_beta 81.858(2) _cell_angle_gamma 75.199(2) _cell_volume 2510.87(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9558 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 30.58 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.69 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452 _exptl_absorpt_coefficient_mu 0.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8827 _exptl_absorpt_correction_T_max 0.9869 _exptl_absorpt_process_details 'SADABS, v. 2.10, Bruker AXS, Madison, WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEX II diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 95722 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 30.58 _reflns_number_total 15331 _reflns_number_gt 12254 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2, v. 2.0-2, Bruker AXS, 2006' _computing_cell_refinement 'APEX2, v. 2.0-2, Bruker AXS, 2006' _computing_data_reduction 'APEX2, v. 2.0-2, Bruker AXS, 2006' _computing_structure_solution 'SHELXTL, v. 6.14, Bruker AXS' _computing_structure_refinement 'SHELXTL, v. 6.14, Bruker AXS' _computing_molecular_graphics 'SHELXTL, v. 6.14, Bruker AXS' _computing_publication_material 'SHELXTL, v. 6.14, Bruker AXS' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1044P)^2^+4.5979P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15331 _refine_ls_number_parameters 1272 _refine_ls_number_restraints 251 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.2005 _refine_ls_wR_factor_gt 0.1845 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.067 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3958(3) 0.8543(2) 0.35943(12) 0.0156(4) Uani 0.8641(15) 1 d P A 1 C2 C 0.3006(2) 0.8821(2) 0.30535(12) 0.0164(4) Uani 0.8641(15) 1 d P A 1 C3 C 0.2573(3) 0.7816(2) 0.30291(13) 0.0142(5) Uani 0.8641(15) 1 d P A 1 C4 C 0.3354(3) 0.6815(2) 0.34438(13) 0.0138(5) Uani 0.8641(15) 1 d P A 1 C5 C 0.4285(2) 0.7197(2) 0.37416(12) 0.0135(4) Uani 0.8641(15) 1 d P A 1 C6 C 0.5593(3) 0.6498(2) 0.38389(12) 0.0134(5) Uani 0.8641(15) 1 d P A 1 C7 C 0.6902(3) 0.6966(2) 0.38216(13) 0.0131(5) Uani 0.8641(15) 1 d P A 1 C8 C 0.6615(4) 0.8219(2) 0.34297(19) 0.0164(7) Uani 0.8641(15) 1 d P A 1 C9 C 0.5306(3) 0.8897(2) 0.33369(13) 0.0163(5) Uani 0.8641(15) 1 d P A 1 C10 C 0.5404(3) 0.9792(2) 0.27550(13) 0.0161(5) Uani 0.8641(15) 1 d P A 1 C11 C 0.4370(4) 1.0152(3) 0.23757(13) 0.0169(7) Uani 0.8641(15) 1 d P A 1 C011 C 0.3242(3) 0.9065(3) 0.41785(13) 0.0213(5) Uani 0.881(2) 1 d PD A 1 C12 C 0.3147(3) 0.9634(2) 0.25042(12) 0.0175(4) Uani 0.8641(15) 1 d P A 1 C012 C 0.3219(4) 1.0366(3) 0.40791(18) 0.0388(8) Uani 0.881(2) 1 d PD A 1 C13 C 0.2777(3) 0.9504(2) 0.19189(15) 0.0155(6) Uani 0.8641(15) 1 d P A 1 C013 C 0.1760(3) 0.8858(3) 0.43925(14) 0.0252(6) Uani 0.881(2) 1 d PD A 1 C014 C 0.3499(19) 0.9543(17) 0.4061(10) 0.0213(5) Uani 0.119(2) 1 d PD A 2 C14 C 0.2296(3) 0.8536(2) 0.18996(13) 0.0148(5) Uani 0.8641(15) 1 d P A 1 C015 C 0.3277(19) 1.0850(18) 0.3880(8) 0.0388(8) Uani 0.119(2) 1 d PD A 2 C15 C 0.2187(2) 0.7669(2) 0.24694(13) 0.0132(5) Uani 0.8641(15) 1 d P A 1 C016 C 0.2224(19) 0.9070(14) 0.4369(8) 0.0252(6) Uani 0.119(2) 1 d PD A 2 C16 C 0.2591(3) 0.6549(2) 0.23091(17) 0.0145(6) Uani 0.8641(15) 1 d P A 1 C17 C 0.3358(2) 0.5596(2) 0.27051(13) 0.0113(4) Uani 0.8641(15) 1 d P A 1 C18 C 0.3721(2) 0.5740(2) 0.32828(11) 0.0107(4) Uani 0.8641(15) 1 d P A 1 C19 C 0.5069(2) 0.5024(2) 0.33838(11) 0.0132(4) Uani 0.8641(15) 1 d P A 1 C20 C 0.5984(2) 0.5408(2) 0.36442(11) 0.0142(4) Uani 0.8641(15) 1 d P A 1 C21 C 0.7442(3) 0.5218(2) 0.33949(12) 0.0124(3) Uani 0.8641(15) 1 d P A 1 C22 C 0.7938(3) 0.6186(2) 0.34309(13) 0.0125(5) Uani 0.8641(15) 1 d P A 1 C23 C 0.8819(5) 0.6597(2) 0.2952(3) 0.0162(7) Uani 0.8641(15) 1 d P A 1 C24 C 0.8678(2) 0.7877(2) 0.26837(12) 0.0170(3) Uani 0.8641(15) 1 d P A 1 C25 C 0.7584(2) 0.8636(2) 0.29237(12) 0.0170(3) Uani 0.8641(15) 1 d P A 1 C26 C 0.6829(3) 0.9632(2) 0.25022(15) 0.0164(5) Uani 0.8641(15) 1 d P A 1 C27 C 0.7172(3) 0.9824(2) 0.18527(15) 0.0180(5) Uani 0.8641(15) 1 d P A 1 C28 C 0.6079(3) 1.0194(2) 0.14310(15) 0.0182(6) Uani 0.8641(15) 1 d P A 1 C29 C 0.4675(10) 1.0355(8) 0.1701(4) 0.0216(12) Uani 0.8641(15) 1 d P A 1 C30 C 0.3732(3) 0.9948(3) 0.14096(14) 0.0174(6) Uani 0.8641(15) 1 d P A 1 C31 C 0.4169(4) 0.9415(2) 0.09023(15) 0.0168(6) Uani 0.8641(15) 1 d P A 1 C32 C 0.3680(3) 0.8396(2) 0.08869(13) 0.0164(5) Uani 0.8641(15) 1 d P A 1 C33 C 0.2770(3) 0.7963(3) 0.13778(13) 0.0146(6) Uani 0.8641(15) 1 d P A 1 C34 C 0.2949(2) 0.6731(2) 0.16213(12) 0.0152(4) Uani 0.8641(15) 1 d P A 1 C35 C 0.4006(2) 0.5958(2) 0.13717(11) 0.0145(4) Uani 0.8641(15) 1 d P A 1 C36 C 0.4713(3) 0.47553(19) 0.17587(12) 0.0113(4) Uani 0.8641(15) 1 d P A 1 C37 C 0.4502(3) 0.4777(2) 0.24528(12) 0.0121(5) Uani 0.8641(15) 1 d P A 1 C38 C 0.5519(2) 0.4436(2) 0.28620(14) 0.0129(5) Uani 0.8641(15) 1 d P A 1 C39 C 0.7045(3) 0.3959(2) 0.26797(12) 0.0116(4) Uani 0.8641(15) 1 d P A 1 C40 C 0.7918(2) 0.4624(2) 0.29132(13) 0.0124(3) Uani 0.8641(15) 1 d P A 1 C41 C 0.8813(3) 0.5085(2) 0.24068(13) 0.0144(5) Uani 0.8641(15) 1 d P A 1 C42 C 0.9290(3) 0.6057(2) 0.24246(14) 0.0148(6) Uani 0.8641(15) 1 d P A 1 C43 C 0.9418(3) 0.6940(2) 0.18506(13) 0.0156(5) Uani 0.8641(15) 1 d P A 1 C44 C 0.9037(3) 0.8066(3) 0.20079(14) 0.0168(5) Uani 0.8641(15) 1 d P A 1 C45 C 0.8303(3) 0.9020(2) 0.15991(15) 0.0185(5) Uani 0.8641(15) 1 d P A 1 C46 C 0.7928(3) 0.8884(3) 0.10162(15) 0.0195(5) Uani 0.8641(15) 1 d P A 1 C47 C 0.6549(3) 0.9618(2) 0.09087(12) 0.0198(5) Uani 0.8641(15) 1 d P A 1 C48 C 0.5608(3) 0.9233(2) 0.06516(12) 0.0194(4) Uani 0.8641(15) 1 d P A 1 C49 C 0.6005(3) 0.8103(3) 0.04888(16) 0.0171(6) Uani 0.8641(15) 1 d P A 1 C50 C 0.4806(3) 0.7601(2) 0.06377(12) 0.0153(5) Uani 0.8641(15) 1 d P A 1 C51 C 0.4969(3) 0.6397(2) 0.08918(13) 0.0145(5) Uani 0.8641(15) 1 d P A 1 C52 C 0.6344(3) 0.5671(2) 0.10005(12) 0.0148(5) Uani 0.8641(15) 1 d P A 1 C53 C 0.6259(3) 0.4753(2) 0.15476(12) 0.0136(4) Uani 0.8641(15) 1 d P A 1 C54 C 0.7279(3) 0.4400(2) 0.19581(13) 0.0136(4) Uani 0.8641(15) 1 d P A 1 C55 C 0.8435(2) 0.4951(2) 0.18225(12) 0.0157(4) Uani 0.8641(15) 1 d P A 1 C56 C 0.8564(2) 0.5795(2) 0.12761(12) 0.0167(4) Uani 0.8641(15) 1 d P A 1 C57 C 0.9066(4) 0.6795(4) 0.12886(14) 0.0158(7) Uani 0.8641(15) 1 d P A 1 C58 C 0.8298(3) 0.7800(3) 0.08597(15) 0.0185(6) Uani 0.8641(15) 1 d P A 1 C59 C 0.7327(3) 0.7399(3) 0.05937(12) 0.0169(5) Uani 0.8641(15) 1 d P A 1 C60 C 0.7494(3) 0.6163(2) 0.08487(12) 0.0150(5) Uani 0.8641(15) 1 d P A 1 C071 C 0.7381(3) 0.6897(3) 0.44865(18) 0.0182(6) Uani 0.8119(19) 1 d PD A 1 C072 C 0.8910(4) 0.6962(4) 0.44586(17) 0.0306(7) Uani 0.8119(19) 1 d PD A 1 C073 C 0.7095(4) 0.5827(3) 0.49859(16) 0.0360(8) Uani 0.8119(19) 1 d PD A 1 C074 C 0.7226(16) 0.6634(13) 0.4520(9) 0.0182(6) Uani 0.1881(19) 1 d PD A 2 C075 C 0.8414(14) 0.7280(11) 0.4514(6) 0.0306(7) Uani 0.1881(19) 1 d PD A 2 C076 C 0.7665(14) 0.5429(14) 0.4875(6) 0.0360(8) Uani 0.1881(19) 1 d PD A 2 C100 C 0.3505(15) 0.6743(13) 0.1245(8) 0.0152(4) Uani 0.1359(15) 1 d P A 2 C101 C 0.483(2) 0.6727(19) 0.0793(10) 0.0153(5) Uani 0.1359(15) 1 d P A 2 C102 C 0.3371(15) 0.5919(13) 0.1791(7) 0.0152(4) Uani 0.1359(15) 1 d P A 2 C103 C 0.5788(19) 0.4860(14) 0.1581(8) 0.0113(4) Uani 0.1359(15) 1 d P A 2 C104 C 0.664(2) 0.677(2) 0.3838(11) 0.0134(5) Uani 0.1359(15) 1 d P A 2 C105 C 0.8088(16) 0.7913(14) 0.3013(8) 0.0170(3) Uani 0.1359(15) 1 d P A 2 C106 C 0.3665(19) 0.6077(19) 0.3375(9) 0.0138(5) Uani 0.1359(15) 1 d P A 2 C107 C 0.446(3) 1.018(3) 0.2230(14) 0.0161(5) Uani 0.1359(15) 1 d P A 2 C108 C 0.575(2) 0.8926(19) 0.3309(10) 0.0164(7) Uani 0.1359(15) 1 d P A 2 C110 C 0.924(3) 0.6334(19) 0.2492(13) 0.0162(7) Uani 0.1359(15) 1 d P A 2 C111 C 0.877(4) 0.682(3) 0.2922(18) 0.0125(5) Uani 0.1359(15) 1 d P A 2 C112 C 0.743(2) 0.6966(18) 0.0640(9) 0.0169(5) Uani 0.1359(15) 1 d P A 2 C113 C 0.705(2) 0.4531(16) 0.1790(9) 0.0136(4) Uani 0.1359(15) 1 d P A 2 C114 C 0.794(2) 0.864(2) 0.0866(10) 0.0185(6) Uani 0.1359(15) 1 d P A 2 C115 C 0.591(2) 0.433(2) 0.2834(11) 0.0116(4) Uani 0.1359(15) 1 d P A 2 C116 C 0.508(2) 0.7844(18) 0.0535(10) 0.0171(6) Uani 0.1359(15) 1 d P A 2 C117 C 0.716(2) 0.5918(18) 0.0900(9) 0.0150(5) Uani 0.1359(15) 1 d P A 2 C118 C 0.6075(15) 0.4888(13) 0.3367(7) 0.0142(4) Uani 0.1359(15) 1 d P A 2 C119 C 0.936(2) 0.7288(19) 0.1900(11) 0.0168(5) Uani 0.1359(15) 1 d P A 2 C120 C 0.638(3) 0.798(3) 0.0469(13) 0.0169(5) Uani 0.1359(15) 1 d P A 2 C121 C 0.586(2) 0.5798(17) 0.0971(9) 0.0145(5) Uani 0.1359(15) 1 d P A 2 C122 C 0.8206(16) 0.8737(14) 0.2464(8) 0.0170(3) Uani 0.1359(15) 1 d P A 2 C123 C 0.5043(15) 0.5644(13) 0.3606(7) 0.0142(4) Uani 0.1359(15) 1 d P A 2 C124 C 0.6573(19) 0.9036(14) 0.0610(7) 0.0194(4) Uani 0.1359(15) 1 d P A 2 C125 C 0.4304(18) 0.8891(16) 0.3493(8) 0.0156(4) Uani 0.1359(15) 1 d P A 2 C126 C 0.851(3) 0.744(2) 0.0925(12) 0.0185(6) Uani 0.1359(15) 1 d P A 2 C127 C 0.7538(19) 0.5018(15) 0.3250(9) 0.0124(3) Uani 0.1359(15) 1 d P A 2 C128 C 0.4193(18) 0.7661(16) 0.3641(8) 0.0135(4) Uani 0.1359(15) 1 d P A 2 C129 C 0.298(3) 0.805(2) 0.1218(12) 0.0164(5) Uani 0.1359(15) 1 d P A 2 C130 C 0.467(6) 1.031(6) 0.162(3) 0.0169(7) Uani 0.1359(15) 1 d P A 2 C131 C 0.384(2) 0.8705(18) 0.0829(11) 0.0168(6) Uani 0.1359(15) 1 d P A 2 C132 C 0.4461(18) 0.4756(15) 0.1979(9) 0.0121(5) Uani 0.1359(15) 1 d P A 2 C133 C 0.593(2) 0.9777(15) 0.2678(9) 0.0164(5) Uani 0.1359(15) 1 d P A 2 C134 C 0.2644(16) 0.9120(14) 0.2627(8) 0.0175(4) Uani 0.1359(15) 1 d P A 2 C135 C 0.901(2) 0.5406(18) 0.2334(11) 0.0144(5) Uani 0.1359(15) 1 d P A 2 C136 C 0.405(3) 0.966(2) 0.0986(14) 0.0174(6) Uani 0.1359(15) 1 d P A 2 C137 C 0.3497(17) 0.5620(14) 0.2928(9) 0.0113(4) Uani 0.1359(15) 1 d P A 2 C138 C 0.777(2) 0.594(2) 0.3416(11) 0.0156(4) Uani 0.1359(15) 1 d P A 2 C139 C 0.5493(18) 0.9819(14) 0.0848(8) 0.0194(4) Uani 0.1359(15) 1 d P A 2 C140 C 0.341(2) 0.993(2) 0.1552(12) 0.0155(6) Uani 0.1359(15) 1 d P A 2 C141 C 0.8030(15) 0.5192(12) 0.1397(7) 0.014(3) Uani 0.1359(15) 1 d P A 2 C142 C 0.521(2) 0.6717(18) 0.3787(10) 0.0135(4) Uani 0.1359(15) 1 d P A 2 C143 C 0.2239(19) 0.7386(17) 0.2352(10) 0.0145(6) Uani 0.1359(15) 1 d P A 2 C144 C 0.671(3) 0.797(2) 0.3498(15) 0.0131(5) Uani 0.1359(15) 1 d P A 2 C145 C 0.240(2) 0.7842(17) 0.2851(10) 0.0132(5) Uani 0.1359(15) 1 d P A 2 C146 C 0.254(2) 0.929(2) 0.1930(12) 0.0148(5) Uani 0.1359(15) 1 d P A 2 C147 C 0.8178(17) 0.4729(14) 0.2702(9) 0.0124(3) Uani 0.1359(15) 1 d P A 2 C148 C 0.3554(16) 0.9501(13) 0.2862(8) 0.0175(4) Uani 0.1359(15) 1 d P A 2 C149 C 0.7276(19) 0.4018(16) 0.2469(9) 0.0136(4) Uani 0.1359(15) 1 d P A 2 C150 C 0.466(2) 0.4658(18) 0.2633(10) 0.0129(5) Uani 0.1359(15) 1 d P A 2 C151 C 0.278(2) 0.6252(19) 0.2343(12) 0.0113(4) Uani 0.1359(15) 1 d P A 2 C152 C 0.8946(16) 0.5570(14) 0.1638(8) 0.0167(4) Uani 0.1359(15) 1 d P A 2 C153 C 0.811(2) 0.9117(16) 0.1345(11) 0.0195(5) Uani 0.1359(15) 1 d P A 2 C154 C 0.920(3) 0.680(3) 0.1416(14) 0.0156(5) Uani 0.1359(15) 1 d P A 2 C155 C 0.704(2) 0.9714(16) 0.2252(12) 0.0164(5) Uani 0.1359(15) 1 d P A 2 C156 C 0.882(2) 0.8441(19) 0.1857(11) 0.0168(5) Uani 0.1359(15) 1 d P A 2 C157 C 0.693(2) 0.9968(15) 0.1607(10) 0.0180(5) Uani 0.1359(15) 1 d P A 2 C158 C 0.236(2) 0.8296(18) 0.1752(10) 0.0148(5) Uani 0.1359(15) 1 d P A 2 C159 C 0.565(3) 1.0276(19) 0.1374(13) 0.0216(12) Uani 0.1359(15) 1 d P A 2 C160 C 0.314(2) 0.7217(17) 0.3350(10) 0.0138(5) Uani 0.1359(15) 1 d P A 2 C361 C 0.4283(3) 0.3705(2) 0.16086(13) 0.0140(5) Uani 0.854(2) 1 d PD A 1 C362 C 0.4244(3) 0.3786(2) 0.08932(13) 0.0194(5) Uani 0.854(2) 1 d PD A 1 C363 C 0.2900(3) 0.3501(3) 0.19700(15) 0.0241(6) Uani 0.854(2) 1 d PD A 1 C364 C 0.2491(17) 0.3673(13) 0.1984(7) 0.0241(6) Uani 0.146(2) 1 d PD A 2 C365 C 0.3947(16) 0.3687(14) 0.1776(7) 0.0140(5) Uani 0.146(2) 1 d PD A 2 C366 C 0.4284(15) 0.3621(13) 0.1079(7) 0.0194(5) Uani 0.146(2) 1 d PD A 2 C391 C 0.7483(3) 0.2614(2) 0.29233(14) 0.0194(6) Uani 0.8944(16) 1 d PD A 1 C392 C 0.8717(3) 0.1994(2) 0.25277(16) 0.0287(6) Uani 0.8944(16) 1 d PD A 1 C393 C 0.7742(3) 0.2212(2) 0.36311(14) 0.0270(6) Uani 0.8944(16) 1 d PD A 1 C394 C 0.751(2) 0.238(3) 0.2861(10) 0.0194(6) Uani 0.1056(16) 1 d PD A 2 C395 C 0.8853(15) 0.2256(15) 0.2291(11) 0.0287(6) Uani 0.1056(16) 1 d PD A 2 C396 C 0.8529(19) 0.2055(14) 0.3383(9) 0.0270(6) Uani 0.1056(16) 1 d PD A 2 C400 C 0.9042(3) 0.1537(2) 0.02713(13) 0.0288(5) Uani 1 1 d . . . H400 H 0.8664 0.0995 0.0165 0.035 Uiso 1 1 calc R . . C401 C 1.0158(3) 0.1167(2) 0.06368(13) 0.0299(5) Uani 1 1 d . . . H401 H 1.0532 0.0376 0.0775 0.036 Uiso 1 1 calc R . . C402 C 1.0717(3) 0.1977(2) 0.07970(12) 0.0280(5) Uani 1 1 d . . . H402 H 1.1465 0.1728 0.1043 0.034 Uiso 1 1 calc R . . C403 C 1.0162(3) 0.3153(2) 0.05915(12) 0.0263(5) Uani 1 1 d . . . H403 H 1.0536 0.3695 0.0700 0.032 Uiso 1 1 calc R . . C404 C 0.9050(3) 0.3523(2) 0.02246(13) 0.0290(5) Uani 1 1 d . . . H404 H 0.8678 0.4314 0.0086 0.035 Uiso 1 1 calc R . . C405 C 0.8490(3) 0.2716(3) 0.00641(13) 0.0300(5) Uani 1 1 d . . . H405 H 0.7743 0.2965 -0.0183 0.036 Uiso 1 1 calc R . . F011 F 0.39825(19) 0.8502(2) 0.46872(9) 0.0322(4) Uani 0.881(2) 1 d PD A 1 F012 F 0.4496(3) 1.0499(2) 0.40726(15) 0.0618(8) Uani 0.881(2) 1 d PD A 1 F013 F 0.2464(3) 1.0831(2) 0.45402(12) 0.0510(6) Uani 0.881(2) 1 d PD A 1 F014 F 0.2694(4) 1.0967(2) 0.35425(13) 0.0576(7) Uani 0.881(2) 1 d PD A 1 F015 F 0.1313(2) 0.9107(2) 0.49511(9) 0.0353(5) Uani 0.881(2) 1 d PD A 1 F016 F 0.0864(3) 0.9506(3) 0.39824(12) 0.0394(6) Uani 0.881(2) 1 d PD A 1 F017 F 0.1751(2) 0.77513(18) 0.44466(11) 0.0358(5) Uani 0.881(2) 1 d PD A 1 F018 F 0.4378(13) 0.9067(15) 0.4512(7) 0.0322(4) Uani 0.119(2) 1 d PD A 2 F019 F 0.2448(19) 0.7955(15) 0.4676(7) 0.057(6) Uani 0.119(2) 1 d PD A 2 F020 F 0.1548(15) 0.9755(15) 0.4767(7) 0.0353(5) Uani 0.119(2) 1 d PD A 2 F021 F 0.1351(18) 0.917(2) 0.3946(8) 0.049(6) Uani 0.119(2) 1 d PD A 2 F022 F 0.219(2) 1.1329(17) 0.3547(10) 0.0576(7) Uani 0.119(2) 1 d PD A 2 F023 F 0.312(2) 1.1190(17) 0.4421(8) 0.0510(6) Uani 0.119(2) 1 d PD A 2 F024 F 0.4351(19) 1.1199(18) 0.3534(10) 0.0618(8) Uani 0.119(2) 1 d PD A 2 F071 F 0.6618(2) 0.7826(2) 0.47161(10) 0.0370(5) Uani 0.8119(19) 1 d PD A 1 F072 F 0.9193(3) 0.7790(3) 0.39922(11) 0.0492(7) Uani 0.8119(19) 1 d PD A 1 F073 F 0.9176(2) 0.7178(2) 0.49935(11) 0.0319(5) Uani 0.8119(19) 1 d PD A 1 F074 F 0.9749(2) 0.5965(3) 0.43731(12) 0.0460(6) Uani 0.8119(19) 1 d PD A 1 F075 F 0.7663(3) 0.5697(2) 0.55191(9) 0.0404(5) Uani 0.8119(19) 1 d PD A 1 F076 F 0.7592(3) 0.4853(2) 0.47970(11) 0.0469(6) Uani 0.8119(19) 1 d PD A 1 F077 F 0.5729(3) 0.5928(3) 0.51146(11) 0.0557(7) Uani 0.8119(19) 1 d PD A 1 F078 F 0.6211(10) 0.7224(10) 0.4874(5) 0.0370(5) Uani 0.1881(19) 1 d PD A 2 F079 F 0.8163(11) 0.8457(10) 0.4302(5) 0.0492(7) Uani 0.1881(19) 1 d PD A 2 F080 F 0.9584(12) 0.6870(9) 0.4164(5) 0.038(2) Uani 0.1881(19) 1 d PD A 2 F081 F 0.8805(12) 0.6980(12) 0.5110(5) 0.0319(5) Uani 0.1881(19) 1 d PD A 2 F082 F 0.6623(12) 0.4939(13) 0.4844(5) 0.0557(7) Uani 0.1881(19) 1 d PD A 2 F083 F 0.7531(11) 0.5047(10) 0.5479(4) 0.0404(5) Uani 0.1881(19) 1 d PD A 2 F084 F 0.8785(12) 0.4826(8) 0.4628(4) 0.0469(6) Uani 0.1881(19) 1 d PD A 2 F361 F 0.5249(2) 0.27086(16) 0.18143(11) 0.0212(4) Uani 0.854(2) 1 d PD A 1 F362 F 0.4142(2) 0.27827(16) 0.07880(9) 0.0271(4) Uani 0.854(2) 1 d PD A 1 F363 F 0.3166(3) 0.46052(17) 0.06642(10) 0.0360(5) Uani 0.854(2) 1 d PD A 1 F364 F 0.5388(2) 0.40385(19) 0.05692(9) 0.0340(5) Uani 0.854(2) 1 d PD A 1 F365 F 0.3034(3) 0.3118(2) 0.25831(9) 0.0402(5) Uani 0.854(2) 1 d PD A 1 F366 F 0.2441(2) 0.27150(18) 0.17786(11) 0.0278(4) Uani 0.854(2) 1 d PD A 1 F367 F 0.1916(2) 0.44818(18) 0.18839(14) 0.0414(6) Uani 0.854(2) 1 d PD A 1 F368 F 0.4829(11) 0.2727(9) 0.2056(6) 0.018(2) Uani 0.146(2) 1 d PD A 2 F369 F 0.5603(11) 0.3327(11) 0.0857(5) 0.0340(5) Uani 0.146(2) 1 d PD A 2 F370 F 0.3641(14) 0.2879(11) 0.0943(6) 0.0271(4) Uani 0.146(2) 1 d PD A 2 F371 F 0.3751(16) 0.4635(10) 0.0711(7) 0.0360(5) Uani 0.146(2) 1 d PD A 2 F372 F 0.1709(13) 0.4476(11) 0.1558(7) 0.0414(6) Uani 0.146(2) 1 d PD A 2 F373 F 0.2210(15) 0.3859(12) 0.2571(5) 0.0402(5) Uani 0.146(2) 1 d PD A 2 F374 F 0.2367(15) 0.2579(11) 0.2040(6) 0.0278(4) Uani 0.146(2) 1 d PD A 2 F391 F 0.64068(17) 0.21269(13) 0.28694(8) 0.0233(3) Uani 0.8944(16) 1 d PD A 1 F392 F 0.8338(2) 0.20684(16) 0.19507(9) 0.0370(4) Uani 0.8944(16) 1 d PD A 1 F393 F 0.97646(18) 0.25054(16) 0.24470(12) 0.0388(5) Uani 0.8944(16) 1 d PD A 1 F394 F 0.9177(2) 0.08787(15) 0.27883(10) 0.0367(4) Uani 0.8944(16) 1 d PD A 1 F395 F 0.7701(2) 0.10852(14) 0.38494(9) 0.0356(4) Uani 0.8944(16) 1 d PD A 1 F396 F 0.8974(2) 0.23339(18) 0.37192(11) 0.0456(5) Uani 0.8944(16) 1 d PD A 1 F397 F 0.6787(2) 0.28166(16) 0.39723(8) 0.0377(5) Uani 0.8944(16) 1 d PD A 1 F398 F 0.6299(13) 0.2000(11) 0.3318(7) 0.0233(3) Uani 0.1056(16) 1 d PD A 2 F399 F 0.9760(17) 0.2374(14) 0.3200(9) 0.0456(5) Uani 0.1056(16) 1 d PD A 2 F400 F 0.8372(18) 0.0954(11) 0.3438(8) 0.0356(4) Uani 0.1056(16) 1 d PD A 2 F401 F 0.768(2) 0.2600(15) 0.3786(8) 0.0377(5) Uani 0.1056(16) 1 d PD A 2 F402 F 0.9856(16) 0.1214(11) 0.2387(9) 0.0367(4) Uani 0.1056(16) 1 d PD A 2 F403 F 0.7569(15) 0.2206(13) 0.2207(8) 0.0370(4) Uani 0.1056(16) 1 d PD A 2 F404 F 0.9772(14) 0.2949(12) 0.1976(10) 0.0388(5) Uani 0.1056(16) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0124(10) 0.0184(12) 0.0190(11) -0.0101(9) -0.0025(8) -0.0023(8) C2 0.0129(9) 0.0162(10) 0.0204(11) -0.0084(9) -0.0024(8) 0.0008(8) C3 0.0094(10) 0.0191(11) 0.0165(13) -0.0089(10) -0.0012(8) -0.0026(8) C4 0.0110(10) 0.0163(12) 0.0144(11) -0.0050(10) 0.0017(8) -0.0036(10) C5 0.0146(9) 0.0133(11) 0.0142(10) -0.0059(9) 0.0009(8) -0.0043(10) C6 0.0122(11) 0.0169(12) 0.0114(10) -0.0035(9) -0.0013(9) -0.0032(9) C7 0.0100(12) 0.0172(12) 0.0143(10) -0.0050(9) -0.0033(9) -0.0046(8) C8 0.0240(14) 0.0133(15) 0.0142(14) -0.0032(12) -0.0043(10) -0.0066(13) C9 0.0185(12) 0.0162(11) 0.0179(11) -0.0078(9) -0.0034(10) -0.0053(11) C10 0.0196(11) 0.0105(9) 0.0208(12) -0.0060(8) -0.0025(10) -0.0053(9) C11 0.0221(13) 0.0102(10) 0.0177(17) -0.0055(13) 0.0021(13) -0.0022(8) C011 0.0209(11) 0.0229(13) 0.0223(12) -0.0134(10) -0.0031(9) -0.0003(10) C12 0.0165(10) 0.0131(10) 0.0232(11) -0.0075(9) -0.0050(8) 0.0016(8) C012 0.0471(18) 0.0321(17) 0.045(2) -0.0277(16) 0.0109(15) -0.0132(15) C13 0.0140(13) 0.0104(13) 0.0216(11) -0.0036(10) -0.0070(10) 0.0012(8) C013 0.0187(13) 0.0328(14) 0.0251(13) -0.0140(11) 0.0003(11) -0.0019(11) C014 0.0209(11) 0.0229(13) 0.0223(12) -0.0134(10) -0.0031(9) -0.0003(10) C14 0.0117(9) 0.0141(12) 0.0177(13) -0.0036(8) -0.0055(9) 0.0011(8) C015 0.0471(18) 0.0321(17) 0.045(2) -0.0277(16) 0.0109(15) -0.0132(15) C15 0.0092(9) 0.0117(11) 0.0195(12) -0.0055(8) -0.0031(8) -0.0007(8) C016 0.0187(13) 0.0328(14) 0.0251(13) -0.0140(11) 0.0003(11) -0.0019(11) C16 0.0099(11) 0.0126(13) 0.0221(12) -0.0046(12) -0.0026(9) -0.0033(10) C17 0.0128(9) 0.0134(9) 0.0114(11) -0.0064(8) 0.0016(8) -0.0073(7) C18 0.0112(9) 0.0099(10) 0.0112(10) -0.0036(7) 0.0014(7) -0.0031(8) C19 0.0137(9) 0.0140(9) 0.0117(9) -0.0011(7) -0.0008(7) -0.0048(8) C20 0.0138(9) 0.0146(9) 0.0126(9) 0.0012(7) -0.0028(7) -0.0035(8) C21 0.0110(7) 0.0111(7) 0.0144(9) -0.0020(6) -0.0037(6) -0.0010(5) C22 0.0125(11) 0.0120(12) 0.0150(10) -0.0047(9) -0.0058(8) -0.0024(8) C23 0.0151(11) 0.0103(18) 0.0247(13) -0.0023(16) -0.0089(9) -0.0032(15) C24 0.0154(7) 0.0176(7) 0.0214(8) -0.0054(6) -0.0034(6) -0.0080(6) C25 0.0154(7) 0.0176(7) 0.0214(8) -0.0054(6) -0.0034(6) -0.0080(6) C26 0.0202(12) 0.0116(9) 0.0204(13) -0.0039(10) -0.0041(11) -0.0072(8) C27 0.0225(12) 0.0112(10) 0.0225(16) -0.0015(10) -0.0015(10) -0.0102(9) C28 0.0261(15) 0.0096(10) 0.0197(13) 0.0006(9) -0.0024(11) -0.0091(11) C29 0.0332(14) 0.0076(13) 0.026(3) -0.0012(17) -0.014(2) -0.0044(10) C30 0.0213(15) 0.0084(9) 0.0211(15) 0.0009(10) -0.0074(10) -0.0018(10) C31 0.0235(13) 0.0107(14) 0.0148(13) 0.0008(9) -0.0057(10) -0.0024(11) C32 0.0225(12) 0.0114(12) 0.0157(12) -0.0013(10) -0.0100(9) -0.0016(9) C33 0.0148(13) 0.0134(11) 0.0157(15) -0.0004(11) -0.0082(10) -0.0021(9) C34 0.0144(9) 0.0141(9) 0.0195(11) -0.0031(8) -0.0082(8) -0.0043(8) C35 0.0175(10) 0.0128(9) 0.0148(10) -0.0022(8) -0.0059(8) -0.0045(8) C36 0.0160(10) 0.0100(9) 0.0094(10) -0.0035(8) -0.0023(8) -0.0035(8) C37 0.0131(10) 0.0106(10) 0.0128(11) -0.0011(9) -0.0014(9) -0.0043(8) C38 0.0121(11) 0.0097(10) 0.0154(10) -0.0015(8) 0.0012(11) -0.0022(10) C39 0.0132(10) 0.0093(9) 0.0114(10) -0.0008(8) -0.0019(8) -0.0016(7) C40 0.0110(7) 0.0111(7) 0.0144(9) -0.0020(6) -0.0037(6) -0.0010(5) C41 0.0111(11) 0.0126(13) 0.0191(11) -0.0047(10) -0.0024(9) -0.0004(8) C42 0.0081(9) 0.0179(15) 0.0183(12) -0.0047(10) 0.0003(8) -0.0028(10) C43 0.0099(9) 0.0166(12) 0.0207(12) -0.0048(10) 0.0025(8) -0.0053(9) C44 0.0133(11) 0.0190(13) 0.0209(14) -0.0051(10) 0.0009(9) -0.0096(10) C45 0.0192(11) 0.0163(11) 0.0221(12) -0.0025(10) 0.0022(10) -0.0115(9) C46 0.0222(12) 0.0172(13) 0.0193(14) 0.0002(9) 0.0026(10) -0.0113(10) C47 0.0280(12) 0.0139(10) 0.0171(11) 0.0025(8) -0.0016(9) -0.0101(9) C48 0.0276(12) 0.0150(10) 0.0149(10) 0.0022(8) -0.0040(9) -0.0079(9) C49 0.0241(15) 0.0157(12) 0.0112(10) -0.0003(8) -0.0026(13) -0.0061(13) C50 0.0194(12) 0.0168(12) 0.0103(11) -0.0009(9) -0.0037(8) -0.0060(8) C51 0.0222(12) 0.0117(12) 0.0112(12) -0.0016(9) -0.0041(9) -0.0062(10) C52 0.0188(11) 0.0140(11) 0.0130(10) -0.0059(8) 0.0004(10) -0.0039(10) C53 0.0149(8) 0.0118(7) 0.0151(8) -0.0054(6) 0.0003(7) -0.0035(6) C54 0.0149(8) 0.0118(7) 0.0151(8) -0.0054(6) 0.0003(7) -0.0035(6) C55 0.0130(9) 0.0144(10) 0.0195(11) -0.0066(8) 0.0004(8) -0.0013(8) C56 0.0150(10) 0.0186(11) 0.0168(11) -0.0066(9) 0.0036(8) -0.0043(8) C57 0.0138(13) 0.0201(11) 0.0159(17) -0.0078(12) 0.0052(10) -0.0081(9) C58 0.0194(13) 0.0212(15) 0.0134(12) 0.0017(13) 0.0031(9) -0.0101(12) C59 0.0245(11) 0.0164(12) 0.0105(9) -0.0010(10) 0.0037(8) -0.0107(12) C60 0.0158(12) 0.0169(12) 0.0130(10) -0.0039(9) 0.0037(9) -0.0070(8) C071 0.0195(12) 0.0187(16) 0.0200(11) -0.0068(13) -0.0057(9) -0.0063(10) C072 0.0180(17) 0.051(2) 0.0269(15) -0.0079(15) -0.0107(15) -0.0104(15) C073 0.050(2) 0.040(2) 0.0217(15) -0.0001(13) -0.0134(15) -0.0184(17) C074 0.0195(12) 0.0187(16) 0.0200(11) -0.0068(13) -0.0057(9) -0.0063(10) C075 0.0180(17) 0.051(2) 0.0269(15) -0.0079(15) -0.0107(15) -0.0104(15) C076 0.050(2) 0.040(2) 0.0217(15) -0.0001(13) -0.0134(15) -0.0184(17) C100 0.0144(9) 0.0141(9) 0.0195(11) -0.0031(8) -0.0082(8) -0.0043(8) C101 0.0194(12) 0.0168(12) 0.0103(11) -0.0009(9) -0.0037(8) -0.0060(8) C102 0.0144(9) 0.0141(9) 0.0195(11) -0.0031(8) -0.0082(8) -0.0043(8) C103 0.0160(10) 0.0100(9) 0.0094(10) -0.0035(8) -0.0023(8) -0.0035(8) C104 0.0122(11) 0.0169(12) 0.0114(10) -0.0035(9) -0.0013(9) -0.0032(9) C105 0.0154(7) 0.0176(7) 0.0214(8) -0.0054(6) -0.0034(6) -0.0080(6) C106 0.0110(10) 0.0163(12) 0.0144(11) -0.0050(10) 0.0017(8) -0.0036(10) C107 0.0196(11) 0.0105(9) 0.0208(12) -0.0060(8) -0.0025(10) -0.0053(9) C108 0.0240(14) 0.0133(15) 0.0142(14) -0.0032(12) -0.0043(10) -0.0066(13) C110 0.0151(11) 0.0103(18) 0.0247(13) -0.0023(16) -0.0089(9) -0.0032(15) C111 0.0125(11) 0.0120(12) 0.0150(10) -0.0047(9) -0.0058(8) -0.0024(8) C112 0.0245(11) 0.0164(12) 0.0105(9) -0.0010(10) 0.0037(8) -0.0107(12) C113 0.0149(8) 0.0118(7) 0.0151(8) -0.0054(6) 0.0003(7) -0.0035(6) C114 0.0194(13) 0.0212(15) 0.0134(12) 0.0017(13) 0.0031(9) -0.0101(12) C115 0.0132(10) 0.0093(9) 0.0114(10) -0.0008(8) -0.0019(8) -0.0016(7) C116 0.0241(15) 0.0157(12) 0.0112(10) -0.0003(8) -0.0026(13) -0.0061(13) C117 0.0158(12) 0.0169(12) 0.0130(10) -0.0039(9) 0.0037(9) -0.0070(8) C118 0.0138(9) 0.0146(9) 0.0126(9) 0.0012(7) -0.0028(7) -0.0035(8) C119 0.0133(11) 0.0190(13) 0.0209(14) -0.0051(10) 0.0009(9) -0.0096(10) C120 0.0245(11) 0.0164(12) 0.0105(9) -0.0010(10) 0.0037(8) -0.0107(12) C121 0.0222(12) 0.0117(12) 0.0112(12) -0.0016(9) -0.0041(9) -0.0062(10) C122 0.0154(7) 0.0176(7) 0.0214(8) -0.0054(6) -0.0034(6) -0.0080(6) C123 0.0138(9) 0.0146(9) 0.0126(9) 0.0012(7) -0.0028(7) -0.0035(8) C124 0.0276(12) 0.0150(10) 0.0149(10) 0.0022(8) -0.0040(9) -0.0079(9) C125 0.0124(10) 0.0184(12) 0.0190(11) -0.0101(9) -0.0025(8) -0.0023(8) C126 0.0194(13) 0.0212(15) 0.0134(12) 0.0017(13) 0.0031(9) -0.0101(12) C127 0.0110(7) 0.0111(7) 0.0144(9) -0.0020(6) -0.0037(6) -0.0010(5) C128 0.0146(9) 0.0133(11) 0.0142(10) -0.0059(9) 0.0009(8) -0.0043(10) C129 0.0225(12) 0.0114(12) 0.0157(12) -0.0013(10) -0.0100(9) -0.0016(9) C130 0.0221(13) 0.0102(10) 0.0177(17) -0.0055(13) 0.0021(13) -0.0022(8) C131 0.0235(13) 0.0107(14) 0.0148(13) 0.0008(9) -0.0057(10) -0.0024(11) C132 0.0131(10) 0.0106(10) 0.0128(11) -0.0011(9) -0.0014(9) -0.0043(8) C133 0.0202(12) 0.0116(9) 0.0204(13) -0.0039(10) -0.0041(11) -0.0072(8) C134 0.0165(10) 0.0131(10) 0.0232(11) -0.0075(9) -0.0050(8) 0.0016(8) C135 0.0111(11) 0.0126(13) 0.0191(11) -0.0047(10) -0.0024(9) -0.0004(8) C136 0.0213(15) 0.0084(9) 0.0211(15) 0.0009(10) -0.0074(10) -0.0018(10) C137 0.0128(9) 0.0134(9) 0.0114(11) -0.0064(8) 0.0016(8) -0.0073(7) C138 0.0124(10) 0.0184(12) 0.0190(11) -0.0101(9) -0.0025(8) -0.0023(8) C139 0.0276(12) 0.0150(10) 0.0149(10) 0.0022(8) -0.0040(9) -0.0079(9) C140 0.0140(13) 0.0104(13) 0.0216(11) -0.0036(10) -0.0070(10) 0.0012(8) C141 0.017(6) 0.011(6) 0.014(6) -0.005(5) -0.002(5) -0.003(5) C142 0.0146(9) 0.0133(11) 0.0142(10) -0.0059(9) 0.0009(8) -0.0043(10) C143 0.0099(11) 0.0126(13) 0.0221(12) -0.0046(12) -0.0026(9) -0.0033(10) C144 0.0100(12) 0.0172(12) 0.0143(10) -0.0050(9) -0.0033(9) -0.0046(8) C145 0.0092(9) 0.0117(11) 0.0195(12) -0.0055(8) -0.0031(8) -0.0007(8) C146 0.0117(9) 0.0141(12) 0.0177(13) -0.0036(8) -0.0055(9) 0.0011(8) C147 0.0110(7) 0.0111(7) 0.0144(9) -0.0020(6) -0.0037(6) -0.0010(5) C148 0.0165(10) 0.0131(10) 0.0232(11) -0.0075(9) -0.0050(8) 0.0016(8) C149 0.0149(8) 0.0118(7) 0.0151(8) -0.0054(6) 0.0003(7) -0.0035(6) C150 0.0121(11) 0.0097(10) 0.0154(10) -0.0015(8) 0.0012(11) -0.0022(10) C151 0.0128(9) 0.0134(9) 0.0114(11) -0.0064(8) 0.0016(8) -0.0073(7) C152 0.0150(10) 0.0186(11) 0.0168(11) -0.0066(9) 0.0036(8) -0.0043(8) C153 0.0222(12) 0.0172(13) 0.0193(14) 0.0002(9) 0.0026(10) -0.0113(10) C154 0.0099(9) 0.0166(12) 0.0207(12) -0.0048(10) 0.0025(8) -0.0053(9) C155 0.0202(12) 0.0116(9) 0.0204(13) -0.0039(10) -0.0041(11) -0.0072(8) C156 0.0133(11) 0.0190(13) 0.0209(14) -0.0051(10) 0.0009(9) -0.0096(10) C157 0.0225(12) 0.0112(10) 0.0225(16) -0.0015(10) -0.0015(10) -0.0102(9) C158 0.0117(9) 0.0141(12) 0.0177(13) -0.0036(8) -0.0055(9) 0.0011(8) C159 0.0332(14) 0.0076(13) 0.026(3) -0.0012(17) -0.014(2) -0.0044(10) C160 0.0110(10) 0.0163(12) 0.0144(11) -0.0050(10) 0.0017(8) -0.0036(10) C361 0.0149(12) 0.0124(9) 0.0151(13) -0.0030(9) -0.0009(8) -0.0039(9) C362 0.0298(12) 0.0184(12) 0.0123(13) -0.0025(10) -0.0069(11) -0.0078(9) C363 0.0216(15) 0.0235(13) 0.0335(13) -0.0145(11) 0.0017(12) -0.0102(12) C364 0.0216(15) 0.0235(13) 0.0335(13) -0.0145(11) 0.0017(12) -0.0102(12) C365 0.0149(12) 0.0124(9) 0.0151(13) -0.0030(9) -0.0009(8) -0.0039(9) C366 0.0298(12) 0.0184(12) 0.0123(13) -0.0025(10) -0.0069(11) -0.0078(9) C391 0.0220(10) 0.0096(14) 0.0289(13) -0.0063(9) -0.0089(9) -0.0019(9) C392 0.0264(12) 0.0161(12) 0.0391(17) -0.0043(11) 0.0032(12) -0.0017(10) C393 0.0376(15) 0.0157(11) 0.0245(13) -0.0006(10) -0.0111(11) 0.0005(11) C394 0.0220(10) 0.0096(14) 0.0289(13) -0.0063(9) -0.0089(9) -0.0019(9) C395 0.0264(12) 0.0161(12) 0.0391(17) -0.0043(11) 0.0032(12) -0.0017(10) C396 0.0376(15) 0.0157(11) 0.0245(13) -0.0006(10) -0.0111(11) 0.0005(11) C400 0.0326(13) 0.0310(12) 0.0272(12) -0.0079(10) 0.0020(10) -0.0161(10) C401 0.0361(13) 0.0217(11) 0.0277(12) 0.0002(9) -0.0018(10) -0.0053(10) C402 0.0262(11) 0.0284(12) 0.0271(12) -0.0047(9) -0.0077(9) -0.0006(9) C403 0.0270(11) 0.0250(11) 0.0289(12) -0.0092(9) -0.0050(9) -0.0048(9) C404 0.0309(12) 0.0233(11) 0.0285(12) -0.0060(9) -0.0073(10) 0.0043(9) C405 0.0231(11) 0.0374(14) 0.0290(12) -0.0089(10) -0.0065(9) -0.0026(10) F011 0.0248(8) 0.0500(12) 0.0234(9) -0.0192(8) -0.0060(7) 0.0014(8) F012 0.0598(15) 0.0613(16) 0.088(2) -0.0572(15) 0.0244(14) -0.0341(13) F013 0.0617(16) 0.0441(13) 0.0557(14) -0.0401(11) 0.0152(12) -0.0103(11) F014 0.099(2) 0.0208(11) 0.0481(13) -0.0131(10) 0.0034(14) -0.0041(12) F015 0.0300(9) 0.0485(12) 0.0278(9) -0.0228(9) 0.0061(7) -0.0003(8) F016 0.0221(12) 0.0565(16) 0.0335(12) -0.0121(10) -0.0059(10) 0.0058(11) F017 0.0307(10) 0.0388(10) 0.0407(11) -0.0196(9) 0.0141(8) -0.0121(8) F018 0.0248(8) 0.0500(12) 0.0234(9) -0.0192(8) -0.0060(7) 0.0014(8) F019 0.043(9) 0.083(14) 0.017(7) 0.004(7) 0.013(6) 0.014(9) F020 0.0300(9) 0.0485(12) 0.0278(9) -0.0228(9) 0.0061(7) -0.0003(8) F021 0.018(9) 0.075(15) 0.040(10) -0.020(9) 0.008(8) 0.014(8) F022 0.099(2) 0.0208(11) 0.0481(13) -0.0131(10) 0.0034(14) -0.0041(12) F023 0.0617(16) 0.0441(13) 0.0557(14) -0.0401(11) 0.0152(12) -0.0103(11) F024 0.0598(15) 0.0613(16) 0.088(2) -0.0572(15) 0.0244(14) -0.0341(13) F071 0.0374(11) 0.0432(13) 0.0320(10) -0.0241(10) -0.0145(9) 0.0094(9) F072 0.0479(13) 0.0719(19) 0.0385(12) 0.0030(11) -0.0172(10) -0.0404(14) F073 0.0283(12) 0.0466(13) 0.0311(11) -0.0108(9) -0.0116(9) -0.0197(9) F074 0.0289(11) 0.0653(18) 0.0460(13) -0.0255(12) -0.0144(9) 0.0041(11) F075 0.0563(13) 0.0545(14) 0.0179(8) 0.0047(9) -0.0186(8) -0.0301(11) F076 0.084(2) 0.0303(11) 0.0313(11) 0.0058(8) -0.0249(12) -0.0228(12) F077 0.0473(14) 0.098(2) 0.0270(11) 0.0024(12) -0.0054(9) -0.0412(14) F078 0.0374(11) 0.0432(13) 0.0320(10) -0.0241(10) -0.0145(9) 0.0094(9) F079 0.0479(13) 0.0719(19) 0.0385(12) 0.0030(11) -0.0172(10) -0.0404(14) F080 0.045(6) 0.030(5) 0.046(6) -0.017(5) -0.027(5) -0.002(4) F081 0.0283(12) 0.0466(13) 0.0311(11) -0.0108(9) -0.0116(9) -0.0197(9) F082 0.0473(14) 0.098(2) 0.0270(11) 0.0024(12) -0.0054(9) -0.0412(14) F083 0.0563(13) 0.0545(14) 0.0179(8) 0.0047(9) -0.0186(8) -0.0301(11) F084 0.084(2) 0.0303(11) 0.0313(11) 0.0058(8) -0.0249(12) -0.0228(12) F361 0.0266(11) 0.0119(7) 0.0265(11) -0.0037(8) -0.0126(8) -0.0017(7) F362 0.0445(13) 0.0213(8) 0.0216(10) -0.0111(7) -0.0041(8) -0.0113(9) F363 0.0489(14) 0.0248(8) 0.0364(10) -0.0070(7) -0.0286(10) 0.0017(9) F364 0.0448(11) 0.0442(11) 0.0230(9) -0.0167(8) 0.0073(8) -0.0249(9) F365 0.0568(14) 0.0521(13) 0.0254(9) -0.0110(9) 0.0085(9) -0.0412(11) F366 0.0292(8) 0.0290(9) 0.0348(11) -0.0154(9) -0.0003(10) -0.0171(7) F367 0.0225(9) 0.0299(9) 0.0767(19) -0.0280(11) 0.0098(10) -0.0065(7) F368 0.013(5) 0.011(4) 0.031(7) -0.010(5) -0.003(4) 0.000(3) F369 0.0448(11) 0.0442(11) 0.0230(9) -0.0167(8) 0.0073(8) -0.0249(9) F370 0.0445(13) 0.0213(8) 0.0216(10) -0.0111(7) -0.0041(8) -0.0113(9) F371 0.0489(14) 0.0248(8) 0.0364(10) -0.0070(7) -0.0286(10) 0.0017(9) F372 0.0225(9) 0.0299(9) 0.0767(19) -0.0280(11) 0.0098(10) -0.0065(7) F373 0.0568(14) 0.0521(13) 0.0254(9) -0.0110(9) 0.0085(9) -0.0412(11) F374 0.0292(8) 0.0290(9) 0.0348(11) -0.0154(9) -0.0003(10) -0.0171(7) F391 0.0253(7) 0.0150(6) 0.0309(8) -0.0020(6) -0.0092(6) -0.0061(6) F392 0.0477(11) 0.0259(9) 0.0346(10) -0.0133(7) 0.0088(8) -0.0038(8) F393 0.0202(8) 0.0227(8) 0.0693(14) -0.0131(9) 0.0093(8) -0.0018(6) F394 0.0332(9) 0.0151(7) 0.0543(12) -0.0055(7) -0.0040(8) 0.0057(6) F395 0.0558(12) 0.0150(7) 0.0311(9) 0.0053(6) -0.0139(8) -0.0042(7) F396 0.0518(13) 0.0328(10) 0.0556(13) -0.0020(9) -0.0365(11) -0.0061(9) F397 0.0633(14) 0.0234(8) 0.0199(8) -0.0019(6) -0.0039(8) -0.0008(9) F398 0.0253(7) 0.0150(6) 0.0309(8) -0.0020(6) -0.0092(6) -0.0061(6) F399 0.0518(13) 0.0328(10) 0.0556(13) -0.0020(9) -0.0365(11) -0.0061(9) F400 0.0558(12) 0.0150(7) 0.0311(9) 0.0053(6) -0.0139(8) -0.0042(7) F401 0.0633(14) 0.0234(8) 0.0199(8) -0.0019(6) -0.0039(8) -0.0008(9) F402 0.0332(9) 0.0151(7) 0.0543(12) -0.0055(7) -0.0040(8) 0.0057(6) F403 0.0477(11) 0.0259(9) 0.0346(10) -0.0133(7) 0.0088(8) -0.0038(8) F404 0.0202(8) 0.0227(8) 0.0693(14) -0.0131(9) 0.0093(8) -0.0018(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C9 1.515(4) . ? C1 C2 1.548(3) . ? C1 C5 1.548(4) . ? C1 C011 1.576(3) . ? C2 C12 1.375(4) . ? C2 C3 1.417(3) . ? C3 C15 1.406(4) . ? C3 C4 1.447(4) . ? C4 C18 1.389(4) . ? C4 C5 1.436(3) . ? C5 C6 1.383(4) . ? C6 C20 1.440(4) . ? C6 C7 1.552(4) . ? C7 C8 1.533(4) . ? C7 C22 1.541(4) . ? C7 C071 1.579(4) . ? C8 C9 1.373(4) . ? C8 C25 1.451(5) . ? C9 C10 1.471(4) . ? C10 C11 1.340(5) . ? C10 C26 1.441(4) . ? C11 C29 1.444(8) . ? C11 C12 1.480(5) . ? C011 F011 1.366(3) . ? C011 C012 1.541(4) . ? C011 C013 1.558(4) . ? C12 C13 1.445(4) . ? C012 F014 1.325(5) . ? C012 F012 1.329(4) . ? C012 F013 1.332(4) . ? C13 C14 1.396(4) . ? C13 C30 1.458(4) . ? C013 F016 1.326(4) . ? C013 F015 1.327(3) . ? C013 F017 1.328(4) . ? C014 F018 1.34(2) . ? C014 C015 1.509(19) . ? C014 C016 1.538(19) . ? C014 C125 1.65(3) . ? C14 C15 1.436(4) . ? C14 C33 1.452(4) . ? C015 F022 1.325(15) . ? C015 F024 1.327(15) . ? C015 F023 1.330(14) . ? C15 C16 1.440(4) . ? C016 F021 1.329(15) . ? C016 F019 1.337(15) . ? C016 F020 1.352(14) . ? C16 C17 1.389(4) . ? C16 C34 1.479(4) . ? C17 C18 1.433(4) . ? C17 C37 1.460(4) . ? C18 C19 1.423(3) . ? C19 C20 1.375(3) . ? C19 C38 1.461(4) . ? C20 C21 1.468(3) . ? C21 C40 1.392(3) . ? C21 C22 1.415(3) . ? C22 C23 1.357(6) . ? C23 C42 1.439(6) . ? C23 C24 1.503(4) . ? C24 C25 1.378(3) . ? C24 C44 1.453(4) . ? C25 C26 1.441(4) . ? C26 C27 1.396(4) . ? C27 C45 1.443(4) . ? C27 C28 1.447(4) . ? C28 C29 1.434(11) . ? C28 C47 1.453(4) . ? C29 C30 1.456(8) . ? C30 C31 1.392(4) . ? C31 C48 1.452(4) . ? C31 C32 1.458(4) . ? C32 C33 1.400(4) . ? C32 C50 1.431(4) . ? C33 C34 1.437(4) . ? C34 C35 1.377(3) . ? C35 C51 1.424(4) . ? C35 C36 1.548(3) . ? C36 C37 1.517(4) . ? C36 C53 1.554(4) . ? C36 C361 1.571(3) . ? C37 C38 1.371(4) . ? C38 C39 1.526(3) . ? C39 C40 1.545(3) . ? C39 C54 1.548(4) . ? C39 C391 1.560(3) . ? C40 C41 1.423(4) . ? C41 C42 1.397(4) . ? C41 C55 1.448(4) . ? C42 C43 1.456(4) . ? C43 C57 1.395(4) . ? C43 C44 1.443(4) . ? C44 C45 1.391(4) . ? C45 C46 1.445(4) . ? C46 C58 1.394(4) . ? C46 C47 1.459(4) . ? C47 C48 1.393(4) . ? C48 C49 1.453(4) . ? C49 C59 1.398(4) . ? C49 C50 1.447(4) . ? C50 C51 1.411(4) . ? C51 C52 1.451(4) . ? C52 C60 1.396(4) . ? C52 C53 1.435(4) . ? C53 C54 1.375(4) . ? C54 C55 1.444(3) . ? C55 C56 1.389(3) . ? C56 C60 1.438(4) . ? C56 C57 1.441(4) . ? C57 C58 1.461(5) . ? C58 C59 1.442(4) . ? C59 C60 1.447(4) . ? C071 F071 1.363(4) . ? C071 C073 1.543(5) . ? C071 C072 1.546(5) . ? C072 F072 1.305(4) . ? C072 F074 1.329(5) . ? C072 F073 1.343(4) . ? C073 F076 1.310(5) . ? C073 F075 1.333(4) . ? C073 F077 1.339(5) . ? C074 F078 1.356(16) . ? C074 C076 1.470(17) . ? C074 C075 1.585(16) . ? C074 C104 1.64(3) . ? C075 F081 1.356(13) . ? C075 F079 1.363(13) . ? C075 F080 1.363(12) . ? C076 F083 1.292(12) . ? C076 F084 1.305(13) . ? C076 F082 1.347(13) . ? C100 C102 1.38(2) . ? C100 C129 1.53(3) . ? C100 C101 1.54(3) . ? C101 C121 1.34(3) . ? C101 C116 1.41(3) . ? C102 C151 1.38(3) . ? C102 C132 1.56(2) . ? C103 C113 1.34(2) . ? C103 C132 1.50(2) . ? C103 C121 1.54(3) . ? C104 C142 1.48(3) . ? C104 C144 1.48(3) . ? C104 C138 1.66(3) . ? C105 C122 1.38(2) . ? C105 C111 1.39(4) . ? C105 C144 1.62(4) . ? C106 C137 1.29(2) . ? C106 C160 1.34(3) . ? C106 C123 1.46(2) . ? C107 C130 1.30(6) . ? C107 C148 1.70(3) . ? C107 C133 1.78(4) . ? C108 C144 1.33(3) . ? C108 C125 1.46(3) . ? C108 C133 1.53(3) . ? C110 C111 1.21(4) . ? C110 C135 1.35(3) . ? C110 C119 1.53(3) . ? C111 C138 1.74(4) . ? C112 C117 1.34(3) . ? C112 C120 1.41(3) . ? C112 C126 1.61(3) . ? C113 C141 1.47(2) . ? C113 C149 1.49(3) . ? C114 C153 1.37(3) . ? C114 C126 1.40(3) . ? C114 C124 1.48(3) . ? C115 C150 1.32(3) . ? C115 C149 1.50(3) . ? C115 C118 1.54(3) . ? C116 C120 1.34(3) . ? C116 C131 1.58(3) . ? C117 C121 1.33(3) . ? C117 C141 1.46(3) . ? C118 C123 1.34(2) . ? C118 C127 1.50(2) . ? C119 C156 1.36(3) . ? C119 C154 1.38(3) . ? C120 C124 1.46(3) . ? C122 C155 1.47(2) . ? C122 C156 1.48(3) . ? C123 C142 1.51(3) . ? C124 C139 1.39(2) . ? C125 C128 1.48(3) . ? C125 C148 1.59(2) . ? C126 C154 1.33(3) . ? C127 C138 1.34(3) . ? C127 C147 1.37(2) . ? C128 C142 1.33(3) . ? C128 C160 1.57(3) . ? C129 C158 1.32(3) . ? C129 C131 1.39(3) . ? C130 C159 1.05(8) . ? C130 C140 1.50(7) . ? C131 C136 1.37(3) . ? C132 C150 1.45(3) . ? C132 C365 1.69(2) . ? C133 C155 1.35(3) . ? C134 C148 1.34(2) . ? C134 C146 1.51(3) . ? C134 C145 1.59(3) . ? C135 C147 1.36(2) . ? C135 C152 1.50(3) . ? C136 C140 1.39(3) . ? C136 C139 1.49(3) . ? C137 C151 1.50(3) . ? C137 C150 1.62(3) . ? C139 C159 1.45(3) . ? C140 C146 1.37(3) . ? C141 C152 1.35(2) . ? C143 C151 1.35(3) . ? C143 C145 1.39(3) . ? C143 C158 1.51(3) . ? C145 C160 1.37(3) . ? C146 C158 1.43(3) . ? C147 C149 1.61(2) . ? C149 C394 1.93(4) . ? C152 C154 1.54(4) . ? C153 C156 1.39(3) . ? C153 C157 1.51(3) . ? C155 C157 1.39(3) . ? C157 C159 1.38(3) . ? C361 F361 1.367(3) . ? C361 C363 1.544(4) . ? C361 C362 1.557(4) . ? C362 F364 1.327(3) . ? C362 F362 1.331(3) . ? C362 F363 1.331(3) . ? C363 F365 1.327(4) . ? C363 F367 1.333(4) . ? C363 F366 1.337(3) . ? C364 F373 1.345(13) . ? C364 F372 1.346(14) . ? C364 F374 1.346(14) . ? C364 C365 1.471(17) . ? C365 F368 1.341(15) . ? C365 C366 1.541(17) . ? C366 F371 1.326(13) . ? C366 F369 1.335(13) . ? C366 F370 1.346(14) . ? C391 F391 1.389(3) . ? C391 C393 1.550(4) . ? C391 C392 1.551(4) . ? C392 F393 1.323(3) . ? C392 F394 1.326(3) . ? C392 F392 1.351(4) . ? C393 F397 1.318(4) . ? C393 F396 1.328(4) . ? C393 F395 1.348(3) . ? C394 F403 1.50(3) . ? C394 C396 1.553(19) . ? C394 F398 1.555(18) . ? C394 C395 1.709(18) . ? C395 F403 1.345(14) . ? C395 F402 1.395(14) . ? C395 F404 1.404(14) . ? C396 F401 1.319(14) . ? C396 F399 1.365(14) . ? C396 F400 1.366(13) . ? C400 C401 1.385(4) . ? C400 C405 1.386(4) . ? C400 H400 0.9300 . ? C401 C402 1.388(4) . ? C401 H401 0.9300 . ? C402 C403 1.383(4) . ? C402 H402 0.9300 . ? C403 C404 1.384(4) . ? C403 H403 0.9300 . ? C404 C405 1.386(4) . ? C404 H404 0.9300 . ? C405 H405 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 C1 C2 109.6(2) . . ? C9 C1 C5 106.8(2) . . ? C2 C1 C5 99.91(19) . . ? C9 C1 C011 112.9(2) . . ? C2 C1 C011 113.59(19) . . ? C5 C1 C011 113.1(2) . . ? C12 C2 C3 118.8(2) . . ? C12 C2 C1 122.8(2) . . ? C3 C2 C1 110.3(2) . . ? C15 C3 C2 121.8(3) . . ? C15 C3 C4 118.7(2) . . ? C2 C3 C4 109.1(2) . . ? C18 C4 C5 121.3(2) . . ? C18 C4 C3 120.0(2) . . ? C5 C4 C3 108.6(2) . . ? C6 C5 C4 118.8(2) . . ? C6 C5 C1 123.8(2) . . ? C4 C5 C1 109.9(2) . . ? C5 C6 C20 119.4(2) . . ? C5 C6 C7 124.1(3) . . ? C20 C6 C7 109.5(2) . . ? C8 C7 C22 108.6(3) . . ? C8 C7 C6 107.2(3) . . ? C22 C7 C6 99.8(2) . . ? C8 C7 C071 111.2(2) . . ? C22 C7 C071 113.9(2) . . ? C6 C7 C071 115.3(2) . . ? C9 C8 C25 109.6(2) . . ? C9 C8 C7 123.4(3) . . ? C25 C8 C7 122.4(3) . . ? C8 C9 C10 107.5(3) . . ? C8 C9 C1 126.4(3) . . ? C10 C9 C1 121.8(2) . . ? C11 C10 C26 121.2(3) . . ? C11 C10 C9 119.7(3) . . ? C26 C10 C9 108.6(2) . . ? C10 C11 C29 120.0(5) . . ? C10 C11 C12 122.1(3) . . ? C29 C11 C12 105.1(4) . . ? F011 C011 C012 106.4(2) . . ? F011 C011 C013 104.3(2) . . ? C012 C011 C013 110.1(2) . . ? F011 C011 C1 108.8(2) . . ? C012 C011 C1 112.8(3) . . ? C013 C011 C1 113.8(2) . . ? C2 C12 C13 120.7(2) . . ? C2 C12 C11 119.4(2) . . ? C13 C12 C11 109.1(2) . . ? F014 C012 F012 109.3(4) . . ? F014 C012 F013 107.5(3) . . ? F012 C012 F013 106.8(3) . . ? F014 C012 C011 111.0(3) . . ? F012 C012 C011 109.8(3) . . ? F013 C012 C011 112.2(3) . . ? C14 C13 C12 120.4(3) . . ? C14 C13 C30 119.9(3) . . ? C12 C13 C30 108.4(2) . . ? F016 C013 F015 108.2(2) . . ? F016 C013 F017 108.0(3) . . ? F015 C013 F017 107.1(3) . . ? F016 C013 C011 111.3(3) . . ? F015 C013 C011 111.4(2) . . ? F017 C013 C011 110.7(2) . . ? F018 C014 C015 111.9(17) . . ? F018 C014 C016 101.0(16) . . ? C015 C014 C016 115.9(14) . . ? F018 C014 C125 101.0(14) . . ? C015 C014 C125 113.7(15) . . ? C016 C014 C125 111.5(15) . . ? C13 C14 C15 118.9(3) . . ? C13 C14 C33 119.8(3) . . ? C15 C14 C33 108.8(2) . . ? F022 C015 F024 106.8(18) . . ? F022 C015 F023 112.2(17) . . ? F024 C015 F023 108.3(16) . . ? F022 C015 C014 111.2(16) . . ? F024 C015 C014 112.7(17) . . ? F023 C015 C014 105.6(16) . . ? C3 C15 C14 119.2(2) . . ? C3 C15 C16 120.3(2) . . ? C14 C15 C16 107.8(2) . . ? F021 C016 F019 105.0(16) . . ? F021 C016 F020 106.5(15) . . ? F019 C016 F020 109.7(15) . . ? F021 C016 C014 111.3(16) . . ? F019 C016 C014 117.2(16) . . ? F020 C016 C014 106.7(14) . . ? C17 C16 C15 120.7(3) . . ? C17 C16 C34 119.1(2) . . ? C15 C16 C34 108.1(2) . . ? C16 C17 C18 118.9(2) . . ? C16 C17 C37 121.1(2) . . ? C18 C17 C37 108.6(2) . . ? C4 C18 C19 119.6(2) . . ? C4 C18 C17 121.3(2) . . ? C19 C18 C17 106.8(2) . . ? C20 C19 C18 119.3(2) . . ? C20 C19 C38 121.2(2) . . ? C18 C19 C38 107.8(2) . . ? C19 C20 C6 121.5(2) . . ? C19 C20 C21 119.4(2) . . ? C6 C20 C21 108.8(2) . . ? C40 C21 C22 122.0(2) . . ? C40 C21 C20 120.9(2) . . ? C22 C21 C20 107.8(2) . . ? C23 C22 C21 118.5(3) . . ? C23 C22 C7 123.1(3) . . ? C21 C22 C7 111.6(2) . . ? C22 C23 C42 121.9(3) . . ? C22 C23 C24 122.0(4) . . ? C42 C23 C24 105.2(4) . . ? C25 C24 C44 120.0(2) . . ? C25 C24 C23 117.9(3) . . ? C44 C24 C23 109.0(3) . . ? C24 C25 C26 119.6(2) . . ? C24 C25 C8 121.3(2) . . ? C26 C25 C8 108.3(2) . . ? C27 C26 C10 120.8(2) . . ? C27 C26 C25 120.9(3) . . ? C10 C26 C25 106.0(2) . . ? C26 C27 C45 119.7(3) . . ? C26 C27 C28 119.3(3) . . ? C45 C27 C28 108.4(3) . . ? C29 C28 C27 118.2(4) . . ? C29 C28 C47 121.8(3) . . ? C27 C28 C47 107.5(3) . . ? C28 C29 C11 120.5(5) . . ? C28 C29 C30 116.4(5) . . ? C11 C29 C30 111.0(7) . . ? C31 C30 C29 122.1(4) . . ? C31 C30 C13 120.5(3) . . ? C29 C30 C13 106.3(5) . . ? C30 C31 C48 120.2(3) . . ? C30 C31 C32 119.5(3) . . ? C48 C31 C32 107.6(2) . . ? C33 C32 C50 119.3(3) . . ? C33 C32 C31 120.1(3) . . ? C50 C32 C31 108.0(3) . . ? C32 C33 C34 120.4(3) . . ? C32 C33 C14 120.1(3) . . ? C34 C33 C14 108.1(2) . . ? C35 C34 C33 120.7(2) . . ? C35 C34 C16 120.9(2) . . ? C33 C34 C16 107.1(2) . . ? C34 C35 C51 119.0(2) . . ? C34 C35 C36 123.4(2) . . ? C51 C35 C36 110.0(2) . . ? C37 C36 C35 109.2(2) . . ? C37 C36 C53 106.81(19) . . ? C35 C36 C53 100.45(19) . . ? C37 C36 C361 113.5(2) . . ? C35 C36 C361 113.91(18) . . ? C53 C36 C361 112.0(2) . . ? C38 C37 C17 107.6(2) . . ? C38 C37 C36 125.8(3) . . ? C17 C37 C36 122.0(2) . . ? C37 C38 C19 109.2(2) . . ? C37 C38 C39 124.2(3) . . ? C19 C38 C39 122.1(2) . . ? C38 C39 C40 108.7(2) . . ? C38 C39 C54 106.7(2) . . ? C40 C39 C54 100.5(2) . . ? C38 C39 C391 111.7(2) . . ? C40 C39 C391 113.24(19) . . ? C54 C39 C391 115.2(2) . . ? C21 C40 C41 118.5(2) . . ? C21 C40 C39 123.3(2) . . ? C41 C40 C39 110.1(2) . . ? C42 C41 C40 120.2(3) . . ? C42 C41 C55 120.6(3) . . ? C40 C41 C55 108.9(2) . . ? C41 C42 C23 118.6(3) . . ? C41 C42 C43 119.9(3) . . ? C23 C42 C43 109.9(2) . . ? C57 C43 C44 120.8(3) . . ? C57 C43 C42 119.1(3) . . ? C44 C43 C42 108.6(2) . . ? C45 C44 C43 120.0(3) . . ? C45 C44 C24 120.6(3) . . ? C43 C44 C24 107.3(2) . . ? C44 C45 C27 119.3(3) . . ? C44 C45 C46 119.9(2) . . ? C27 C45 C46 108.4(3) . . ? C58 C46 C45 120.4(3) . . ? C58 C46 C47 119.7(3) . . ? C45 C46 C47 107.5(3) . . ? C48 C47 C28 119.5(3) . . ? C48 C47 C46 119.9(2) . . ? C28 C47 C46 108.1(2) . . ? C47 C48 C31 120.0(2) . . ? C47 C48 C49 120.0(2) . . ? C31 C48 C49 108.0(2) . . ? C59 C49 C50 120.2(3) . . ? C59 C49 C48 120.1(3) . . ? C50 C49 C48 107.5(2) . . ? C51 C50 C32 119.1(3) . . ? C51 C50 C49 120.0(3) . . ? C32 C50 C49 108.9(2) . . ? C50 C51 C35 121.4(3) . . ? C50 C51 C52 119.5(3) . . ? C35 C51 C52 108.8(2) . . ? C60 C52 C53 121.3(3) . . ? C60 C52 C51 120.0(2) . . ? C53 C52 C51 109.3(2) . . ? C54 C53 C52 119.8(2) . . ? C54 C53 C36 123.4(2) . . ? C52 C53 C36 109.2(2) . . ? C53 C54 C55 119.0(2) . . ? C53 C54 C39 124.9(2) . . ? C55 C54 C39 109.1(2) . . ? C56 C55 C54 121.5(2) . . ? C56 C55 C41 119.2(2) . . ? C54 C55 C41 108.9(2) . . ? C55 C56 C60 119.2(2) . . ? C55 C56 C57 120.6(2) . . ? C60 C56 C57 108.3(2) . . ? C43 C57 C56 120.7(3) . . ? C43 C57 C58 119.1(3) . . ? C56 C57 C58 108.0(2) . . ? C46 C58 C59 120.5(3) . . ? C46 C58 C57 119.8(3) . . ? C59 C58 C57 107.2(3) . . ? C49 C59 C58 119.8(3) . . ? C49 C59 C60 119.8(3) . . ? C58 C59 C60 108.5(2) . . ? C52 C60 C56 118.9(2) . . ? C52 C60 C59 120.5(2) . . ? C56 C60 C59 108.0(2) . . ? F071 C071 C073 104.5(3) . . ? F071 C071 C072 105.9(3) . . ? C073 C071 C072 110.7(3) . . ? F071 C071 C7 109.2(3) . . ? C073 C071 C7 112.7(2) . . ? C072 C071 C7 113.2(3) . . ? F072 C072 F074 107.9(4) . . ? F072 C072 F073 107.9(3) . . ? F074 C072 F073 108.9(3) . . ? F072 C072 C071 110.9(3) . . ? F074 C072 C071 110.3(3) . . ? F073 C072 C071 110.8(3) . . ? F076 C073 F075 106.2(3) . . ? F076 C073 F077 106.9(3) . . ? F075 C073 F077 108.8(3) . . ? F076 C073 C071 112.6(3) . . ? F075 C073 C071 112.0(3) . . ? F077 C073 C071 110.1(3) . . ? F078 C074 C076 108.8(14) . . ? F078 C074 C075 99.6(12) . . ? C076 C074 C075 107.8(13) . . ? F078 C074 C104 107.8(14) . . ? C076 C074 C104 114.9(13) . . ? C075 C074 C104 116.7(14) . . ? F081 C075 F079 110.0(11) . . ? F081 C075 F080 103.9(11) . . ? F079 C075 F080 104.3(11) . . ? F081 C075 C074 106.5(12) . . ? F079 C075 C074 119.1(11) . . ? F080 C075 C074 112.2(12) . . ? F083 C076 F084 110.7(12) . . ? F083 C076 F082 87.1(10) . . ? F084 C076 F082 106.8(13) . . ? F083 C076 C074 127.4(15) . . ? F084 C076 C074 114.4(11) . . ? F082 C076 C074 104.0(12) . . ? C102 C100 C129 122.1(16) . . ? C102 C100 C101 124.6(15) . . ? C129 C100 C101 101.1(16) . . ? C121 C101 C116 122(2) . . ? C121 C101 C100 113.3(18) . . ? C116 C101 C100 113.2(18) . . ? C100 C102 C151 120.3(16) . . ? C100 C102 C132 123.9(15) . . ? C151 C102 C132 107.0(15) . . ? C113 C103 C132 125.6(17) . . ? C113 C103 C121 106.8(16) . . ? C132 C103 C121 122.8(15) . . ? C142 C104 C144 104(2) . . ? C142 C104 C074 122.2(17) . . ? C144 C104 C074 103.7(18) . . ? C142 C104 C138 111.2(17) . . ? C144 C104 C138 103.6(19) . . ? C074 C104 C138 110.0(16) . . ? C122 C105 C111 110(2) . . ? C122 C105 C144 123.7(16) . . ? C111 C105 C144 116(2) . . ? C137 C106 C160 120.2(19) . . ? C137 C106 C123 113.6(17) . . ? C160 C106 C123 113.6(17) . . ? C130 C107 C148 141(4) . . ? C130 C107 C133 118(3) . . ? C148 C107 C133 89.5(17) . . ? C144 C108 C125 118(2) . . ? C144 C108 C133 122(2) . . ? C125 C108 C133 112.2(18) . . ? C111 C110 C135 133(3) . . ? C111 C110 C119 107(2) . . ? C135 C110 C119 110(2) . . ? C110 C111 C105 139(3) . . ? C110 C111 C138 105(2) . . ? C105 C111 C138 102(3) . . ? C117 C112 C120 123(2) . . ? C117 C112 C126 121.4(18) . . ? C120 C112 C126 102.3(18) . . ? C103 C113 C141 112.9(16) . . ? C103 C113 C149 122.0(18) . . ? C141 C113 C149 119.1(16) . . ? C153 C114 C126 117(2) . . ? C153 C114 C124 116.5(19) . . ? C126 C114 C124 113.7(19) . . ? C150 C115 C149 129(2) . . ? C150 C115 C118 114.4(18) . . ? C149 C115 C118 109.9(16) . . ? C120 C116 C101 119(2) . . ? C120 C116 C131 122(2) . . ? C101 C116 C131 105.0(18) . . ? C121 C117 C112 120(2) . . ? C121 C117 C141 115.4(17) . . ? C112 C117 C141 115.6(18) . . ? C123 C118 C127 123.1(14) . . ? C123 C118 C115 123.1(14) . . ? C127 C118 C115 104.0(14) . . ? C156 C119 C154 118(2) . . ? C156 C119 C110 125(2) . . ? C154 C119 C110 104(2) . . ? C116 C120 C112 117(2) . . ? C116 C120 C124 117(2) . . ? C112 C120 C124 116(2) . . ? C117 C121 C101 120(2) . . ? C117 C121 C103 104.3(17) . . ? C101 C121 C103 124.7(18) . . ? C105 C122 C155 122.1(16) . . ? C105 C122 C156 123.2(16) . . ? C155 C122 C156 100.8(17) . . ? C118 C123 C106 124.4(15) . . ? C118 C123 C142 124.8(15) . . ? C106 C123 C142 99.9(15) . . ? C139 C124 C120 122.3(17) . . ? C139 C124 C114 122.4(16) . . ? C120 C124 C114 102.3(18) . . ? C108 C125 C128 108.5(15) . . ? C108 C125 C148 104.0(15) . . ? C128 C125 C148 106.0(13) . . ? C108 C125 C014 117.8(15) . . ? C128 C125 C014 110.7(15) . . ? C148 C125 C014 109.0(13) . . ? C154 C126 C114 122(3) . . ? C154 C126 C112 122(2) . . ? C114 C126 C112 105.5(19) . . ? C138 C127 C147 119(2) . . ? C138 C127 C118 115.5(17) . . ? C147 C127 C118 112.7(15) . . ? C142 C128 C125 127.1(17) . . ? C142 C128 C160 103.3(16) . . ? C125 C128 C160 123.8(15) . . ? C158 C129 C131 122(2) . . ? C158 C129 C100 114(2) . . ? C131 C129 C100 113(2) . . ? C159 C130 C107 124(5) . . ? C159 C130 C140 134(5) . . ? C107 C130 C140 95(4) . . ? C136 C131 C129 120(2) . . ? C136 C131 C116 121(2) . . ? C129 C131 C116 107.8(19) . . ? C150 C132 C103 109.6(15) . . ? C150 C132 C102 105.2(15) . . ? C103 C132 C102 108.3(14) . . ? C150 C132 C365 119.4(14) . . ? C103 C132 C365 105.3(13) . . ? C102 C132 C365 108.8(12) . . ? C155 C133 C108 127.5(19) . . ? C155 C133 C107 105.6(18) . . ? C108 C133 C107 113.3(18) . . ? C148 C134 C146 123.4(17) . . ? C148 C134 C145 124.0(15) . . ? C146 C134 C145 98.7(15) . . ? C110 C135 C147 123(2) . . ? C110 C135 C152 113.1(19) . . ? C147 C135 C152 114.5(17) . . ? C131 C136 C140 118(3) . . ? C131 C136 C139 115(2) . . ? C140 C136 C139 114(2) . . ? C106 C137 C151 126.2(18) . . ? C106 C137 C150 125.3(17) . . ? C151 C137 C150 98.5(15) . . ? C127 C138 C104 124.8(19) . . ? C127 C138 C111 121(2) . . ? C104 C138 C111 106.7(19) . . ? C124 C139 C159 121.1(17) . . ? C124 C139 C136 123.4(16) . . ? C159 C139 C136 101.9(18) . . ? C146 C140 C136 121(2) . . ? C146 C140 C130 137(3) . . ? C136 C140 C130 88(3) . . ? C152 C141 C117 123.5(15) . . ? C152 C141 C113 123.1(14) . . ? C117 C141 C113 100.4(14) . . ? C128 C142 C104 123(2) . . ? C128 C142 C123 115.6(17) . . ? C104 C142 C123 115.9(17) . . ? C151 C143 C145 121(2) . . ? C151 C143 C158 118.8(18) . . ? C145 C143 C158 107.8(17) . . ? C108 C144 C104 133(3) . . ? C108 C144 C105 111(2) . . ? C104 C144 C105 109(2) . . ? C160 C145 C143 123.8(19) . . ? C160 C145 C134 111.3(17) . . ? C143 C145 C134 112.5(16) . . ? C140 C146 C158 119(2) . . ? C140 C146 C134 114.4(19) . . ? C158 C146 C134 114.1(18) . . ? C135 C147 C127 118.5(18) . . ? C135 C147 C149 127.0(17) . . ? C127 C147 C149 108.5(16) . . ? C134 C148 C125 126.7(15) . . ? C134 C148 C107 106.1(16) . . ? C125 C148 C107 118.6(16) . . ? C113 C149 C115 106.8(17) . . ? C113 C149 C147 109.0(15) . . ? C115 C149 C147 101.7(15) . . ? C113 C149 C394 124.6(15) . . ? C115 C149 C394 92.5(14) . . ? C147 C149 C394 117.2(14) . . ? C115 C150 C132 121(2) . . ? C115 C150 C137 119.0(18) . . ? C132 C150 C137 110.9(16) . . ? C143 C151 C102 121(2) . . ? C143 C151 C137 111(2) . . ? C102 C151 C137 116.3(17) . . ? C141 C152 C135 122.7(15) . . ? C141 C152 C154 123.7(17) . . ? C135 C152 C154 99.3(16) . . ? C114 C153 C156 121(2) . . ? C114 C153 C157 121.0(19) . . ? C156 C153 C157 105.7(19) . . ? C126 C154 C119 121(3) . . ? C126 C154 C152 114(2) . . ? C119 C154 C152 114(2) . . ? C133 C155 C157 123.0(19) . . ? C133 C155 C122 113(2) . . ? C157 C155 C122 113.5(18) . . ? C119 C156 C153 121(2) . . ? C119 C156 C122 113.7(19) . . ? C153 C156 C122 113.8(18) . . ? C159 C157 C155 120(2) . . ? C159 C157 C153 121(2) . . ? C155 C157 C153 106.1(18) . . ? C129 C158 C146 119(2) . . ? C129 C158 C143 123.4(19) . . ? C146 C158 C143 106.8(18) . . ? C130 C159 C157 129(4) . . ? C130 C159 C139 102(3) . . ? C157 C159 C139 118(2) . . ? C106 C160 C145 117.2(19) . . ? C106 C160 C128 107.4(16) . . ? C145 C160 C128 125.1(17) . . ? F361 C361 C363 105.4(2) . . ? F361 C361 C362 105.4(2) . . ? C363 C361 C362 110.2(2) . . ? F361 C361 C36 108.7(2) . . ? C363 C361 C36 112.3(2) . . ? C362 C361 C36 114.2(2) . . ? F364 C362 F362 107.3(2) . . ? F364 C362 F363 108.3(2) . . ? F362 C362 F363 107.9(2) . . ? F364 C362 C361 111.1(2) . . ? F362 C362 C361 111.3(2) . . ? F363 C362 C361 110.8(2) . . ? F365 C363 F367 108.4(3) . . ? F365 C363 F366 107.3(3) . . ? F367 C363 F366 107.0(2) . . ? F365 C363 C361 110.9(2) . . ? F367 C363 C361 110.8(2) . . ? F366 C363 C361 112.2(2) . . ? F373 C364 F372 113.7(14) . . ? F373 C364 F374 105.1(12) . . ? F372 C364 F374 114.3(14) . . ? F373 C364 C365 109.1(13) . . ? F372 C364 C365 107.6(13) . . ? F374 C364 C365 106.8(13) . . ? F368 C365 C364 112.8(13) . . ? F368 C365 C366 101.1(12) . . ? C364 C365 C366 111.4(13) . . ? F368 C365 C132 102.4(12) . . ? C364 C365 C132 113.0(13) . . ? C366 C365 C132 115.2(13) . . ? F371 C366 F369 105.8(13) . . ? F371 C366 F370 103.9(12) . . ? F369 C366 F370 106.3(12) . . ? F371 C366 C365 110.0(13) . . ? F369 C366 C365 119.2(12) . . ? F370 C366 C365 110.5(13) . . ? F391 C391 C393 104.4(2) . . ? F391 C391 C392 103.5(2) . . ? C393 C391 C392 109.8(2) . . ? F391 C391 C39 108.9(2) . . ? C393 C391 C39 114.6(2) . . ? C392 C391 C39 114.6(2) . . ? F393 C392 F394 107.8(2) . . ? F393 C392 F392 107.4(3) . . ? F394 C392 F392 108.0(2) . . ? F393 C392 C391 110.4(2) . . ? F394 C392 C391 113.2(3) . . ? F392 C392 C391 109.8(2) . . ? F397 C393 F396 108.8(3) . . ? F397 C393 F395 107.1(3) . . ? F396 C393 F395 108.4(2) . . ? F397 C393 C391 111.1(2) . . ? F396 C393 C391 110.5(3) . . ? F395 C393 C391 110.8(2) . . ? F403 C394 C396 136.3(18) . . ? F403 C394 F398 115.0(17) . . ? C396 C394 F398 94.4(14) . . ? F403 C394 C395 49.0(8) . . ? C396 C394 C395 91.4(14) . . ? F398 C394 C395 156(2) . . ? F403 C394 C149 85.8(14) . . ? C396 C394 C149 109.4(17) . . ? F398 C394 C149 117.6(17) . . ? C395 C394 C149 82.4(13) . . ? F403 C395 F402 117.5(15) . . ? F403 C395 F404 134.7(17) . . ? F402 C395 F404 95.3(12) . . ? F403 C395 C394 57.3(13) . . ? F402 C395 C394 116.4(17) . . ? F404 C395 C394 135.1(18) . . ? F401 C396 F399 116.3(15) . . ? F401 C396 F400 112.7(14) . . ? F399 C396 F400 123.5(15) . . ? F401 C396 C394 96.6(16) . . ? F399 C396 C394 115.5(15) . . ? F400 C396 C394 84.1(16) . . ? C401 C400 C405 119.9(2) . . ? C401 C400 H400 120.0 . . ? C405 C400 H400 120.0 . . ? C400 C401 C402 120.0(2) . . ? C400 C401 H401 120.0 . . ? C402 C401 H401 120.0 . . ? C403 C402 C401 120.1(2) . . ? C403 C402 H402 120.0 . . ? C401 C402 H402 120.0 . . ? C402 C403 C404 119.9(2) . . ? C402 C403 H403 120.0 . . ? C404 C403 H403 120.0 . . ? C403 C404 C405 120.1(2) . . ? C403 C404 H404 120.0 . . ? C405 C404 H404 120.0 . . ? C400 C405 C404 120.0(2) . . ? C400 C405 H405 120.0 . . ? C404 C405 H405 120.0 . . ? C395 F403 C394 73.6(12) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.58 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.450 _refine_diff_density_min -1.337 _refine_diff_density_rms 0.095