# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Carl Redshaw' 'Mark R.J. Elsegood' _publ_contact_author_name 'Carl Redshaw ' _publ_contact_author_address ; School of Chemical Sciences & Pharmacy The University of East Anglia Norwich NR4 7TJ UNITED KINGDOM ; _publ_contact_author_email 'CARL.REDSHAW@UEA.AC.UK ' _publ_section_title ; Synthesis of bis(bora)calix[4]arenes bearing perfluoroaryl substituents ; # # Manuscript submitted to Chemical Communications. # Authors: Carl Redshaw and Mark R.J. Elsegood. # Title: Synthesis of bis(bors)calix[4]arenes bearing # perfluoroaryl substituents. # Corresponding author for crystallography: # m.r.j.elsegood@lboro.ac.uk # This cif contains 4 structures. # data_1.3MeCN _database_code_depnum_ccdc_archive 'CCDC 278174' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H61 B2 F10 N3 O4' _chemical_formula_weight 1123.76 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 13.3771(4) _cell_length_b 28.5640(9) _cell_length_c 15.3254(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5855.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 22664 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 28.26 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.74 _exptl_crystal_size_mid 0.73 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.930 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_process_details 'SADABS, Sheldrick, G.M.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 49143 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.79 _reflns_number_total 13756 _reflns_number_gt 11982 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0604P)^2^+1.1829P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.2(3) _refine_ls_number_reflns 13756 _refine_ls_number_parameters 745 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1084 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 O1 O 0.44244(9) 0.64063(4) 0.17821(8) 0.0306(2) Uani 1 1 d . . . O2 O 0.34539(9) 0.69449(4) 0.26824(8) 0.0327(3) Uani 1 1 d . . . O3 O 0.12074(9) 0.64210(4) 0.25644(8) 0.0321(3) Uani 1 1 d . . . O4 O 0.22435(9) 0.58511(4) 0.18137(9) 0.0358(3) Uani 1 1 d . . . C1 C 0.49361(12) 0.61208(6) 0.23670(10) 0.0262(3) Uani 1 1 d . . . C2 C 0.48574(12) 0.56410(6) 0.22505(10) 0.0259(3) Uani 1 1 d . . . C3 C 0.54643(12) 0.53532(6) 0.27697(11) 0.0275(3) Uani 1 1 d . . . H3 H 0.5427 0.5024 0.2693 0.033 Uiso 1 1 calc R . . C4 C 0.61181(12) 0.55308(6) 0.33912(11) 0.0299(3) Uani 1 1 d . . . C5 C 0.61514(13) 0.60170(6) 0.34927(11) 0.0302(3) Uani 1 1 d . . . H5 H 0.6583 0.6147 0.3921 0.036 Uiso 1 1 calc R . . C6 C 0.55726(12) 0.63173(6) 0.29861(11) 0.0287(3) Uani 1 1 d . . . C7 C 0.68193(13) 0.52159(6) 0.39304(12) 0.0342(4) Uani 1 1 d . . . C8 C 0.6480(2) 0.47091(9) 0.3920(3) 0.0828(11) Uani 1 1 d . . . H8A H 0.6535 0.4585 0.3326 0.124 Uiso 1 1 calc R . . H8B H 0.5783 0.4690 0.4113 0.124 Uiso 1 1 calc R . . H8C H 0.6903 0.4525 0.4313 0.124 Uiso 1 1 calc R . . C9 C 0.78774(17) 0.52580(11) 0.3566(2) 0.0696(8) Uani 1 1 d . . . H9A H 0.8339 0.5078 0.3933 0.104 Uiso 1 1 calc R . . H9B H 0.8079 0.5588 0.3562 0.104 Uiso 1 1 calc R . . H9C H 0.7893 0.5135 0.2969 0.104 Uiso 1 1 calc R . . C10 C 0.6834(2) 0.53757(10) 0.48807(16) 0.0633(7) Uani 1 1 d . . . H10A H 0.6150 0.5378 0.5111 0.095 Uiso 1 1 calc R . . H10B H 0.7117 0.5692 0.4916 0.095 Uiso 1 1 calc R . . H10C H 0.7244 0.5160 0.5226 0.095 Uiso 1 1 calc R . . C11 C 0.55703(13) 0.68394(6) 0.31545(12) 0.0311(3) Uani 1 1 d . . . H11A H 0.5455 0.7010 0.2601 0.037 Uiso 1 1 calc R . . H11B H 0.6226 0.6937 0.3392 0.037 Uiso 1 1 calc R . . C12 C 0.37468(13) 0.69694(5) 0.35511(11) 0.0276(3) Uani 1 1 d . . . C13 C 0.47463(13) 0.69552(5) 0.38034(11) 0.0293(3) Uani 1 1 d . . . C14 C 0.49771(14) 0.70172(6) 0.46794(12) 0.0324(4) Uani 1 1 d . . . H14 H 0.5656 0.6996 0.4857 0.039 Uiso 1 1 calc R . . C15 C 0.42466(14) 0.71099(6) 0.53089(12) 0.0339(4) Uani 1 1 d . . . C16 C 0.32611(14) 0.71237(6) 0.50247(11) 0.0322(4) Uani 1 1 d . . . H16 H 0.2751 0.7187 0.5439 0.039 Uiso 1 1 calc R . . C17 C 0.29879(13) 0.70483(6) 0.41564(11) 0.0296(3) Uani 1 1 d . . . C18 C 0.45151(16) 0.71694(8) 0.62769(13) 0.0424(4) Uani 1 1 d . . . C19 C 0.5561(2) 0.73749(11) 0.63954(16) 0.0635(7) Uani 1 1 d . . . H19A H 0.6053 0.7170 0.6114 0.095 Uiso 1 1 calc R . . H19B H 0.5713 0.7400 0.7019 0.095 Uiso 1 1 calc R . . H19C H 0.5589 0.7687 0.6129 0.095 Uiso 1 1 calc R . . C20 C 0.3751(2) 0.74733(12) 0.67562(17) 0.0716(8) Uani 1 1 d . . . H20A H 0.3960 0.7514 0.7364 0.107 Uiso 1 1 calc R . . H20B H 0.3095 0.7321 0.6739 0.107 Uiso 1 1 calc R . . H20C H 0.3707 0.7780 0.6472 0.107 Uiso 1 1 calc R . . C21 C 0.4497(2) 0.66799(10) 0.67009(18) 0.0669(7) Uani 1 1 d . . . H21A H 0.4950 0.6471 0.6383 0.100 Uiso 1 1 calc R . . H21B H 0.3816 0.6554 0.6678 0.100 Uiso 1 1 calc R . . H21C H 0.4713 0.6704 0.7310 0.100 Uiso 1 1 calc R . . C22 C 0.18936(13) 0.70398(6) 0.39073(11) 0.0289(3) Uani 1 1 d . . . H22A H 0.1823 0.7116 0.3280 0.035 Uiso 1 1 calc R . . H22B H 0.1528 0.7280 0.4246 0.035 Uiso 1 1 calc R . . C23 C 0.11879(12) 0.62543(6) 0.34117(11) 0.0277(3) Uani 1 1 d . . . C24 C 0.14425(12) 0.65601(6) 0.40861(11) 0.0286(3) Uani 1 1 d . . . C25 C 0.12936(14) 0.64064(6) 0.49409(11) 0.0331(4) Uani 1 1 d . . . H25 H 0.1453 0.6613 0.5406 0.040 Uiso 1 1 calc R . . C26 C 0.09239(15) 0.59661(7) 0.51427(13) 0.0380(4) Uani 1 1 d . . . C27 C 0.06919(13) 0.56712(6) 0.44458(13) 0.0361(4) Uani 1 1 d . . . H27 H 0.0440 0.5367 0.4565 0.043 Uiso 1 1 calc R . . C28 C 0.08169(12) 0.58079(6) 0.35826(12) 0.0308(3) Uani 1 1 d . . . C29 C 0.07589(19) 0.58193(8) 0.60992(15) 0.0526(6) Uani 1 1 d . . . C30 C 0.0799(4) 0.52988(11) 0.6212(2) 0.1006(13) Uani 1 1 d . . . H30A H 0.0860 0.5223 0.6833 0.151 Uiso 1 1 calc R . . H30B H 0.1378 0.5174 0.5896 0.151 Uiso 1 1 calc R . . H30C H 0.0186 0.5159 0.5979 0.151 Uiso 1 1 calc R . . C31 C -0.0173(3) 0.60429(17) 0.6432(2) 0.1146(17) Uani 1 1 d . . . H31A H -0.0754 0.5903 0.6142 0.172 Uiso 1 1 calc R . . H31B H -0.0154 0.6380 0.6310 0.172 Uiso 1 1 calc R . . H31C H -0.0224 0.5993 0.7063 0.172 Uiso 1 1 calc R . . C32 C 0.1636(3) 0.60065(17) 0.6687(2) 0.1056(14) Uani 1 1 d . . . H32A H 0.1597 0.5860 0.7264 0.158 Uiso 1 1 calc R . . H32B H 0.1579 0.6347 0.6747 0.158 Uiso 1 1 calc R . . H32C H 0.2278 0.5929 0.6415 0.158 Uiso 1 1 calc R . . C33 C 0.06310(12) 0.54623(6) 0.28518(13) 0.0336(4) Uani 1 1 d . . . H33A H 0.0396 0.5630 0.2325 0.040 Uiso 1 1 calc R . . H33B H 0.0107 0.5237 0.3028 0.040 Uiso 1 1 calc R . . C34 C 0.23651(12) 0.54159(6) 0.21945(11) 0.0270(3) Uani 1 1 d . . . C35 C 0.15924(12) 0.52031(6) 0.26495(11) 0.0288(3) Uani 1 1 d . . . C36 C 0.17397(13) 0.47533(6) 0.29790(11) 0.0306(3) Uani 1 1 d . . . H36 H 0.1220 0.4610 0.3306 0.037 Uiso 1 1 calc R . . C37 C 0.26217(13) 0.45093(6) 0.28435(11) 0.0298(3) Uani 1 1 d . . . C38 C 0.33710(12) 0.47337(6) 0.23731(11) 0.0289(3) Uani 1 1 d . . . H38 H 0.3977 0.4570 0.2267 0.035 Uiso 1 1 calc R . . C39 C 0.32738(12) 0.51853(6) 0.20524(10) 0.0263(3) Uani 1 1 d . . . C40 C 0.27855(14) 0.40069(6) 0.31749(14) 0.0378(4) Uani 1 1 d . . . C41 C 0.37724(17) 0.39767(8) 0.36838(17) 0.0521(5) Uani 1 1 d . . . H41A H 0.4334 0.4023 0.3283 0.078 Uiso 1 1 calc R . . H41B H 0.3828 0.3668 0.3958 0.078 Uiso 1 1 calc R . . H41C H 0.3785 0.4220 0.4135 0.078 Uiso 1 1 calc R . . C42 C 0.19323(16) 0.38463(8) 0.37663(17) 0.0509(5) Uani 1 1 d . . . H42A H 0.2087 0.3536 0.4002 0.076 Uiso 1 1 calc R . . H42B H 0.1311 0.3831 0.3429 0.076 Uiso 1 1 calc R . . H42C H 0.1852 0.4069 0.4248 0.076 Uiso 1 1 calc R . . C43 C 0.28298(19) 0.36745(7) 0.23826(17) 0.0521(5) Uani 1 1 d . . . H43A H 0.3350 0.3781 0.1979 0.078 Uiso 1 1 calc R . . H43B H 0.2182 0.3675 0.2084 0.078 Uiso 1 1 calc R . . H43C H 0.2985 0.3357 0.2582 0.078 Uiso 1 1 calc R . . C44 C 0.41423(12) 0.54224(6) 0.15941(10) 0.0272(3) Uani 1 1 d . . . H44A H 0.3884 0.5668 0.1199 0.033 Uiso 1 1 calc R . . H44B H 0.4506 0.5189 0.1236 0.033 Uiso 1 1 calc R . . B1 B 0.38067(14) 0.67727(6) 0.19201(12) 0.0285(4) Uani 1 1 d . . . C45 C 0.33907(13) 0.70140(6) 0.10610(11) 0.0308(3) Uani 1 1 d . . . C46 C 0.34140(15) 0.67993(6) 0.02489(12) 0.0363(4) Uani 1 1 d . . . F1 F 0.37851(11) 0.63679(4) 0.01493(8) 0.0522(3) Uani 1 1 d . . . C47 C 0.30297(16) 0.70009(7) -0.05001(13) 0.0412(4) Uani 1 1 d . . . F2 F 0.30459(12) 0.67727(5) -0.12597(8) 0.0602(4) Uani 1 1 d . . . C48 C 0.26070(16) 0.74387(7) -0.04510(13) 0.0433(5) Uani 1 1 d . . . F3 F 0.22065(12) 0.76322(5) -0.11700(9) 0.0625(4) Uani 1 1 d . . . C49 C 0.25767(17) 0.76693(7) 0.03321(15) 0.0458(5) Uani 1 1 d . . . F4 F 0.21417(13) 0.80925(4) 0.03827(10) 0.0684(4) Uani 1 1 d . . . C50 C 0.29641(15) 0.74592(6) 0.10699(13) 0.0379(4) Uani 1 1 d . . . F5 F 0.28977(11) 0.77047(4) 0.18122(9) 0.0550(3) Uani 1 1 d . . . B2 B 0.15431(14) 0.61964(7) 0.18473(13) 0.0294(4) Uani 1 1 d . . . C51 C 0.11553(12) 0.63906(6) 0.09422(11) 0.0294(3) Uani 1 1 d . . . C52 C 0.10909(14) 0.60971(7) 0.02177(12) 0.0359(4) Uani 1 1 d . . . F6 F 0.13599(10) 0.56457(4) 0.02748(8) 0.0508(3) Uani 1 1 d . . . C53 C 0.07285(15) 0.62482(8) -0.05818(13) 0.0432(5) Uani 1 1 d . . . F7 F 0.06729(12) 0.59446(6) -0.12510(9) 0.0674(4) Uani 1 1 d . . . C54 C 0.04182(15) 0.66988(8) -0.06769(12) 0.0442(5) Uani 1 1 d . . . F8 F 0.00876(11) 0.68544(6) -0.14500(9) 0.0664(4) Uani 1 1 d . . . C55 C 0.04408(14) 0.69984(7) 0.00239(14) 0.0405(4) Uani 1 1 d . . . F9 F 0.01496(10) 0.74450(5) -0.00672(10) 0.0586(3) Uani 1 1 d . . . C56 C 0.08019(13) 0.68418(6) 0.08211(12) 0.0332(4) Uani 1 1 d . . . F10 F 0.08103(9) 0.71513(4) 0.14801(8) 0.0451(3) Uani 1 1 d . . . N1 N 0.6096(3) 0.47092(19) 0.0807(3) 0.163(2) Uani 1 1 d . . . C57 C 0.62392(19) 0.45196(10) 0.0181(2) 0.0705(8) Uani 1 1 d . . . C58 C 0.64210(18) 0.42656(10) -0.06037(16) 0.0585(6) Uani 1 1 d . . . H58A H 0.6620 0.3945 -0.0460 0.088 Uiso 1 1 calc R . . H58B H 0.6957 0.4418 -0.0933 0.088 Uiso 1 1 calc R . . H58C H 0.5810 0.4259 -0.0957 0.088 Uiso 1 1 calc R . . N2 N 0.2566(2) 0.82918(9) 0.5070(2) 0.0789(7) Uani 1 1 d . . . C59 C 0.31362(18) 0.82701(8) 0.4532(2) 0.0542(6) Uani 1 1 d . . . C60 C 0.3843(2) 0.82384(10) 0.3819(3) 0.0828(10) Uani 1 1 d . . . H60A H 0.4250 0.7955 0.3888 0.124 Uiso 1 1 calc R . . H60B H 0.4279 0.8514 0.3824 0.124 Uiso 1 1 calc R . . H60C H 0.3481 0.8224 0.3265 0.124 Uiso 1 1 calc R . . N3 N 0.3940(2) 0.88944(17) 0.1529(3) 0.151(2) Uani 1 1 d . . . C61 C 0.3167(2) 0.90126(11) 0.1374(2) 0.0718(8) Uani 1 1 d . . . C62 C 0.21841(19) 0.91626(11) 0.12016(19) 0.0626(6) Uani 1 1 d . . . H62A H 0.1842 0.8928 0.0842 0.094 Uiso 1 1 calc R . . H62B H 0.2203 0.9462 0.0890 0.094 Uiso 1 1 calc R . . H62C H 0.1823 0.9202 0.1753 0.094 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0363(6) 0.0288(6) 0.0266(6) 0.0027(5) 0.0020(5) 0.0046(5) O2 0.0347(6) 0.0356(6) 0.0278(6) 0.0019(5) 0.0020(5) 0.0055(5) O3 0.0364(6) 0.0314(6) 0.0284(6) 0.0016(5) -0.0034(5) 0.0063(5) O4 0.0315(6) 0.0334(6) 0.0426(7) 0.0090(6) 0.0023(5) 0.0086(5) C1 0.0266(8) 0.0272(8) 0.0250(7) 0.0024(6) 0.0059(6) 0.0033(6) C2 0.0253(7) 0.0271(8) 0.0255(8) -0.0008(6) 0.0039(6) 0.0012(6) C3 0.0264(7) 0.0245(7) 0.0316(8) 0.0001(6) 0.0040(6) -0.0002(6) C4 0.0255(8) 0.0329(8) 0.0314(8) 0.0033(7) 0.0028(6) 0.0015(6) C5 0.0270(8) 0.0335(8) 0.0300(8) -0.0005(7) 0.0009(6) -0.0021(6) C6 0.0278(8) 0.0272(8) 0.0311(8) 0.0000(6) 0.0061(6) -0.0020(6) C7 0.0289(8) 0.0354(9) 0.0384(10) 0.0070(7) -0.0043(7) 0.0005(7) C8 0.0835(19) 0.0403(13) 0.125(3) 0.0269(15) -0.062(2) -0.0055(12) C9 0.0399(12) 0.096(2) 0.0733(17) 0.0369(15) 0.0101(11) 0.0254(12) C10 0.0804(18) 0.0683(16) 0.0413(12) 0.0134(11) -0.0086(12) 0.0157(13) C11 0.0321(9) 0.0261(8) 0.0352(9) -0.0020(7) 0.0025(7) -0.0033(6) C12 0.0363(9) 0.0200(7) 0.0264(8) 0.0001(6) 0.0019(6) 0.0005(6) C13 0.0357(9) 0.0201(7) 0.0320(8) -0.0010(6) 0.0033(7) -0.0028(6) C14 0.0341(9) 0.0255(8) 0.0375(9) 0.0009(7) -0.0029(7) -0.0020(7) C15 0.0426(10) 0.0275(8) 0.0316(9) -0.0008(7) -0.0003(7) -0.0017(7) C16 0.0402(9) 0.0255(8) 0.0308(9) -0.0004(6) 0.0047(7) 0.0006(7) C17 0.0367(9) 0.0216(7) 0.0306(8) 0.0008(6) 0.0027(7) 0.0015(6) C18 0.0452(11) 0.0499(11) 0.0319(10) -0.0029(8) -0.0029(8) -0.0018(9) C19 0.0643(15) 0.0851(18) 0.0410(12) -0.0107(12) -0.0053(11) -0.0261(13) C20 0.0774(17) 0.102(2) 0.0355(11) -0.0219(13) -0.0097(12) 0.0272(15) C21 0.0823(18) 0.0723(16) 0.0463(13) 0.0153(12) -0.0189(13) -0.0097(14) C22 0.0343(9) 0.0242(7) 0.0282(8) 0.0002(6) 0.0038(7) 0.0055(6) C23 0.0245(8) 0.0293(8) 0.0292(8) 0.0016(6) 0.0023(6) 0.0072(6) C24 0.0269(8) 0.0277(8) 0.0312(8) 0.0014(6) 0.0044(6) 0.0056(6) C25 0.0374(9) 0.0330(9) 0.0288(8) 0.0010(7) 0.0067(7) 0.0052(7) C26 0.0408(10) 0.0377(9) 0.0356(9) 0.0053(8) 0.0143(8) 0.0067(8) C27 0.0327(9) 0.0299(9) 0.0455(10) 0.0038(7) 0.0131(8) 0.0029(7) C28 0.0246(7) 0.0306(8) 0.0372(9) -0.0021(7) 0.0029(7) 0.0052(6) C29 0.0668(14) 0.0488(12) 0.0422(11) 0.0138(10) 0.0217(10) 0.0055(11) C30 0.180(4) 0.0635(18) 0.0583(18) 0.0263(14) 0.014(2) 0.003(2) C31 0.099(3) 0.180(4) 0.0641(19) 0.050(2) 0.0488(19) 0.067(3) C32 0.104(3) 0.170(4) 0.0427(15) 0.036(2) -0.0079(16) -0.035(3) C33 0.0244(8) 0.0322(9) 0.0441(10) -0.0043(7) -0.0004(7) 0.0013(7) C34 0.0280(8) 0.0251(7) 0.0279(8) -0.0033(6) -0.0043(6) 0.0045(6) C35 0.0264(8) 0.0285(8) 0.0316(8) -0.0072(6) -0.0033(6) 0.0014(6) C36 0.0279(8) 0.0296(8) 0.0342(9) -0.0029(7) -0.0007(6) -0.0024(6) C37 0.0318(8) 0.0247(8) 0.0330(8) -0.0036(6) -0.0046(7) 0.0001(6) C38 0.0267(8) 0.0281(8) 0.0317(8) -0.0048(6) -0.0029(6) 0.0050(6) C39 0.0270(8) 0.0286(8) 0.0234(7) -0.0055(6) -0.0019(6) 0.0015(6) C40 0.0353(9) 0.0298(9) 0.0482(11) 0.0057(8) -0.0017(8) 0.0025(7) C41 0.0444(11) 0.0491(12) 0.0627(14) 0.0177(11) -0.0121(10) 0.0043(9) C42 0.0462(11) 0.0422(11) 0.0645(14) 0.0186(10) 0.0018(10) 0.0023(9) C43 0.0583(13) 0.0296(9) 0.0684(15) -0.0046(10) -0.0022(11) 0.0059(9) C44 0.0293(8) 0.0277(7) 0.0244(8) -0.0022(6) 0.0008(6) 0.0051(6) B1 0.0320(9) 0.0250(8) 0.0285(9) 0.0044(7) 0.0019(7) -0.0008(7) C45 0.0332(9) 0.0283(8) 0.0307(8) 0.0061(7) 0.0012(7) -0.0018(7) C46 0.0423(10) 0.0339(9) 0.0327(9) 0.0065(7) 0.0051(8) 0.0009(7) F1 0.0777(9) 0.0462(7) 0.0329(6) -0.0022(5) 0.0007(6) 0.0193(6) C47 0.0464(11) 0.0477(11) 0.0296(9) 0.0066(8) 0.0014(8) -0.0086(9) F2 0.0832(10) 0.0699(9) 0.0276(6) 0.0030(6) -0.0023(6) 0.0021(7) C48 0.0472(11) 0.0442(11) 0.0386(10) 0.0176(9) -0.0086(8) -0.0068(9) F3 0.0777(10) 0.0616(8) 0.0482(7) 0.0262(6) -0.0176(7) -0.0022(7) C49 0.0524(12) 0.0304(9) 0.0545(13) 0.0132(9) -0.0061(9) 0.0021(8) F4 0.0978(12) 0.0375(7) 0.0698(9) 0.0119(6) -0.0190(8) 0.0184(7) C50 0.0460(10) 0.0296(9) 0.0382(9) 0.0061(7) -0.0017(8) -0.0005(8) F5 0.0850(9) 0.0329(6) 0.0472(7) -0.0033(5) -0.0094(7) 0.0134(6) B2 0.0263(9) 0.0294(9) 0.0324(9) 0.0034(7) -0.0049(7) 0.0023(7) C51 0.0264(8) 0.0361(9) 0.0256(8) 0.0017(6) -0.0006(6) 0.0055(7) C52 0.0328(9) 0.0422(10) 0.0327(9) -0.0014(8) 0.0015(7) 0.0046(7) F6 0.0613(8) 0.0436(6) 0.0475(7) -0.0142(5) -0.0028(6) 0.0141(6) C53 0.0398(10) 0.0625(13) 0.0275(9) -0.0053(8) -0.0012(8) -0.0002(9) F7 0.0767(10) 0.0915(11) 0.0338(6) -0.0183(7) -0.0063(6) 0.0039(8) C54 0.0353(10) 0.0669(14) 0.0304(9) 0.0142(9) -0.0042(8) -0.0031(9) F8 0.0631(8) 0.0946(11) 0.0416(7) 0.0265(7) -0.0169(6) -0.0056(8) C55 0.0301(9) 0.0457(10) 0.0458(11) 0.0175(9) 0.0011(8) 0.0058(8) F9 0.0570(8) 0.0520(7) 0.0669(8) 0.0280(6) -0.0010(7) 0.0155(6) C56 0.0291(8) 0.0364(9) 0.0341(9) 0.0038(7) 0.0009(7) 0.0049(7) F10 0.0608(7) 0.0326(5) 0.0420(6) -0.0008(5) 0.0007(5) 0.0093(5) N1 0.101(2) 0.225(5) 0.162(4) -0.137(4) -0.032(2) 0.071(3) C57 0.0465(13) 0.0733(17) 0.092(2) -0.0418(16) -0.0162(13) 0.0205(12) C58 0.0472(12) 0.0763(17) 0.0521(14) -0.0159(12) -0.0105(10) 0.0159(11) N2 0.0788(17) 0.0741(16) 0.0838(19) 0.0043(14) -0.0091(15) 0.0212(13) C59 0.0391(11) 0.0372(11) 0.0865(18) 0.0057(11) -0.0215(12) 0.0020(9) C60 0.0510(15) 0.0487(14) 0.149(3) 0.0174(18) 0.0077(18) -0.0108(11) N3 0.0524(17) 0.195(4) 0.206(5) -0.095(4) -0.030(2) 0.028(2) C61 0.0456(14) 0.088(2) 0.0816(19) -0.0335(16) 0.0084(12) -0.0023(13) C62 0.0499(13) 0.0798(18) 0.0580(15) -0.0115(13) 0.0095(11) 0.0086(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 B1 1.350(2) . ? O1 C1 1.392(2) . ? O2 B1 1.353(2) . ? O2 C12 1.389(2) . ? O3 B2 1.350(2) . ? O3 C23 1.383(2) . ? O4 B2 1.361(2) . ? O4 C34 1.383(2) . ? C1 C2 1.386(2) . ? C1 C6 1.393(2) . ? C2 C3 1.403(2) . ? C2 C44 1.522(2) . ? C3 C4 1.389(2) . ? C4 C5 1.398(2) . ? C4 C7 1.540(2) . ? C5 C6 1.392(2) . ? C6 C11 1.513(2) . ? C7 C8 1.517(3) . ? C7 C9 1.526(3) . ? C7 C10 1.527(3) . ? C11 C13 1.521(2) . ? C12 C13 1.392(2) . ? C12 C17 1.394(2) . ? C13 C14 1.389(3) . ? C14 C15 1.398(3) . ? C15 C16 1.389(3) . ? C15 C18 1.536(3) . ? C16 C17 1.397(3) . ? C17 C22 1.513(3) . ? C18 C19 1.528(3) . ? C18 C20 1.529(3) . ? C18 C21 1.542(3) . ? C22 C24 1.522(2) . ? C23 C28 1.393(2) . ? C23 C24 1.395(2) . ? C24 C25 1.396(2) . ? C25 C26 1.386(3) . ? C26 C27 1.395(3) . ? C26 C29 1.541(3) . ? C27 C28 1.389(3) . ? C28 C33 1.514(3) . ? C29 C31 1.491(4) . ? C29 C30 1.498(4) . ? C29 C32 1.572(5) . ? C33 C35 1.516(2) . ? C34 C35 1.387(2) . ? C34 C39 1.400(2) . ? C35 C36 1.394(2) . ? C36 C37 1.386(2) . ? C37 C38 1.391(2) . ? C37 C40 1.538(2) . ? C38 C39 1.387(2) . ? C39 C44 1.517(2) . ? C40 C42 1.528(3) . ? C40 C41 1.536(3) . ? C40 C43 1.543(3) . ? B1 C45 1.587(2) . ? C45 C46 1.388(3) . ? C45 C50 1.394(3) . ? C46 F1 1.337(2) . ? C46 C47 1.383(3) . ? C47 F2 1.334(2) . ? C47 C48 1.374(3) . ? C48 F3 1.344(2) . ? C48 C49 1.370(3) . ? C49 F4 1.344(2) . ? C49 C50 1.381(3) . ? C50 F5 1.339(2) . ? B2 C51 1.581(2) . ? C51 C56 1.385(2) . ? C51 C52 1.394(3) . ? C52 F6 1.342(2) . ? C52 C53 1.387(3) . ? C53 F7 1.345(2) . ? C53 C54 1.360(3) . ? C54 F8 1.341(2) . ? C54 C55 1.373(3) . ? C55 F9 1.341(2) . ? C55 C56 1.388(3) . ? C56 F10 1.342(2) . ? N1 C57 1.118(4) . ? C57 C58 1.426(4) . ? N2 C59 1.125(4) . ? C59 C60 1.448(5) . ? N3 C61 1.114(4) . ? C61 C62 1.408(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B1 O1 C1 130.87(14) . . ? B1 O2 C12 138.37(14) . . ? B2 O3 C23 127.38(13) . . ? B2 O4 C34 135.74(15) . . ? C2 C1 O1 117.32(14) . . ? C2 C1 C6 122.18(15) . . ? O1 C1 C6 120.22(14) . . ? C1 C2 C3 117.54(15) . . ? C1 C2 C44 122.58(14) . . ? C3 C2 C44 119.87(14) . . ? C4 C3 C2 122.64(15) . . ? C3 C4 C5 117.33(15) . . ? C3 C4 C7 122.56(15) . . ? C5 C4 C7 120.07(15) . . ? C6 C5 C4 122.15(16) . . ? C5 C6 C1 118.14(15) . . ? C5 C6 C11 120.87(16) . . ? C1 C6 C11 120.79(15) . . ? C8 C7 C9 110.4(2) . . ? C8 C7 C10 107.4(2) . . ? C9 C7 C10 108.3(2) . . ? C8 C7 C4 111.66(16) . . ? C9 C7 C4 108.82(15) . . ? C10 C7 C4 110.18(16) . . ? C6 C11 C13 109.10(13) . . ? O2 C12 C13 122.37(15) . . ? O2 C12 C17 116.14(15) . . ? C13 C12 C17 121.29(15) . . ? C14 C13 C12 118.57(16) . . ? C14 C13 C11 119.90(16) . . ? C12 C13 C11 121.38(15) . . ? C13 C14 C15 122.38(17) . . ? C16 C15 C14 116.89(16) . . ? C16 C15 C18 121.45(17) . . ? C14 C15 C18 121.59(17) . . ? C15 C16 C17 122.87(17) . . ? C12 C17 C16 117.94(16) . . ? C12 C17 C22 122.29(15) . . ? C16 C17 C22 119.74(16) . . ? C19 C18 C20 109.7(2) . . ? C19 C18 C15 111.80(17) . . ? C20 C18 C15 111.73(18) . . ? C19 C18 C21 108.2(2) . . ? C20 C18 C21 107.6(2) . . ? C15 C18 C21 107.63(17) . . ? C17 C22 C24 110.65(13) . . ? O3 C23 C28 119.89(15) . . ? O3 C23 C24 118.38(14) . . ? C28 C23 C24 121.37(16) . . ? C23 C24 C25 117.61(16) . . ? C23 C24 C22 121.79(15) . . ? C25 C24 C22 120.57(15) . . ? C26 C25 C24 123.07(17) . . ? C25 C26 C27 117.15(17) . . ? C25 C26 C29 120.69(18) . . ? C27 C26 C29 122.15(18) . . ? C28 C27 C26 122.16(17) . . ? C27 C28 C23 118.64(16) . . ? C27 C28 C33 120.08(16) . . ? C23 C28 C33 121.10(16) . . ? C31 C29 C30 114.6(3) . . ? C31 C29 C26 109.2(2) . . ? C30 C29 C26 112.0(2) . . ? C31 C29 C32 106.4(3) . . ? C30 C29 C32 104.2(3) . . ? C26 C29 C32 110.2(2) . . ? C28 C33 C35 109.30(14) . . ? O4 C34 C35 121.22(14) . . ? O4 C34 C39 117.35(15) . . ? C35 C34 C39 121.28(15) . . ? C34 C35 C36 118.71(15) . . ? C34 C35 C33 121.40(15) . . ? C36 C35 C33 119.72(16) . . ? C37 C36 C35 121.96(16) . . ? C36 C37 C38 117.35(15) . . ? C36 C37 C40 122.75(16) . . ? C38 C37 C40 119.89(15) . . ? C39 C38 C37 123.00(15) . . ? C38 C39 C34 117.65(15) . . ? C38 C39 C44 120.50(14) . . ? C34 C39 C44 121.81(14) . . ? C42 C40 C41 108.90(18) . . ? C42 C40 C37 111.70(16) . . ? C41 C40 C37 110.04(16) . . ? C42 C40 C43 108.10(18) . . ? C41 C40 C43 109.39(18) . . ? C37 C40 C43 108.66(16) . . ? C39 C44 C2 111.01(13) . . ? O1 B1 O2 129.10(16) . . ? O1 B1 C45 114.92(15) . . ? O2 B1 C45 115.87(15) . . ? C46 C45 C50 114.90(16) . . ? C46 C45 B1 122.98(15) . . ? C50 C45 B1 122.12(16) . . ? F1 C46 C47 115.27(17) . . ? F1 C46 C45 121.18(16) . . ? C47 C46 C45 123.50(17) . . ? F2 C47 C48 119.93(18) . . ? F2 C47 C46 120.97(19) . . ? C48 C47 C46 119.09(19) . . ? F3 C48 C49 120.58(19) . . ? F3 C48 C47 119.5(2) . . ? C49 C48 C47 119.86(18) . . ? F4 C49 C48 119.75(18) . . ? F4 C49 C50 120.4(2) . . ? C48 C49 C50 119.82(18) . . ? F5 C50 C49 116.29(17) . . ? F5 C50 C45 120.87(17) . . ? C49 C50 C45 122.83(19) . . ? O3 B2 O4 127.18(17) . . ? O3 B2 C51 116.00(14) . . ? O4 B2 C51 116.53(16) . . ? C56 C51 C52 115.57(16) . . ? C56 C51 B2 123.77(16) . . ? C52 C51 B2 120.53(16) . . ? F6 C52 C53 116.78(17) . . ? F6 C52 C51 120.63(16) . . ? C53 C52 C51 122.57(18) . . ? F7 C53 C54 120.77(19) . . ? F7 C53 C52 119.5(2) . . ? C54 C53 C52 119.72(18) . . ? F8 C54 C53 120.6(2) . . ? F8 C54 C55 119.5(2) . . ? C53 C54 C55 119.94(17) . . ? F9 C55 C54 120.32(18) . . ? F9 C55 C56 120.0(2) . . ? C54 C55 C56 119.69(18) . . ? F10 C56 C51 120.60(16) . . ? F10 C56 C55 116.94(16) . . ? C51 C56 C55 122.45(18) . . ? N1 C57 C58 178.4(5) . . ? N2 C59 C60 178.1(3) . . ? N3 C61 C62 178.5(4) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.438 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.038 #===END data_2.2MeCN _database_code_depnum_ccdc_archive 'CCDC 278175' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H58 B2 Cl2 N2 O4' _chemical_formula_weight 819.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 16.4659(12) _cell_length_b 16.7508(12) _cell_length_c 18.1131(13) _cell_angle_alpha 90.00 _cell_angle_beta 115.137(2) _cell_angle_gamma 90.00 _cell_volume 4522.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7783 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 28.34 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.73 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 0.188 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.875 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_process_details 'SADABS v2.03, Sheldrick, G.M., (2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18907 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5145 _reflns_number_gt 3919 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0612P)^2^+4.7386P] 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 5145 _refine_ls_number_parameters 321 _refine_ls_number_restraints 155 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1435 _refine_ls_wR_factor_gt 0.1252 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.119 _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 Cl1 Cl 0.15772(5) -0.05654(4) 0.67784(3) 0.0644(2) Uani 1 1 d . . . B1 B 0.11462(16) 0.01541(14) 0.59807(12) 0.0374(5) Uani 1 1 d . . . O1 O 0.14057(9) 0.00185(8) 0.53833(7) 0.0370(3) Uani 1 1 d . . . O2 O 0.06175(9) 0.07074(8) 0.60966(8) 0.0383(3) Uani 1 1 d . . . C1 C 0.12750(12) 0.04019(12) 0.46581(11) 0.0324(4) Uani 1 1 d . . . C2 C 0.11280(13) -0.00776(12) 0.39914(11) 0.0340(4) Uani 1 1 d . . . C3 C 0.10196(13) 0.02956(13) 0.32672(12) 0.0389(4) Uani 1 1 d . . . H3 H 0.0906 -0.0025 0.2801 0.047 Uiso 1 1 calc R . . C4 C 0.10721(13) 0.11205(13) 0.32013(12) 0.0407(5) Uani 1 1 d . A . C5 C 0.12519(13) 0.15683(13) 0.38956(13) 0.0402(5) Uani 1 1 d . . . H5 H 0.1304 0.2131 0.3870 0.048 Uiso 1 1 calc R . . C6 C 0.13591(12) 0.12240(12) 0.46294(12) 0.0350(4) Uani 1 1 d . . . C7 C 0.09124(15) 0.15112(15) 0.23838(14) 0.0504(6) Uani 1 1 d DU . . C8 C 0.1582(4) 0.1233(3) 0.2116(3) 0.0589(14) Uani 0.550(5) 1 d PDU A 1 H8A H 0.2184 0.1339 0.2543 0.088 Uiso 0.550(5) 1 calc PR A 1 H8B H 0.1505 0.1514 0.1616 0.088 Uiso 0.550(5) 1 calc PR A 1 H8C H 0.1509 0.0658 0.2009 0.088 Uiso 0.550(5) 1 calc PR A 1 C9 C 0.1075(4) 0.2468(3) 0.2529(3) 0.0600(14) Uani 0.550(5) 1 d PDU A 1 H9A H 0.0637 0.2690 0.2706 0.090 Uiso 0.550(5) 1 calc PR A 1 H9B H 0.1004 0.2724 0.2018 0.090 Uiso 0.550(5) 1 calc PR A 1 H9C H 0.1683 0.2565 0.2949 0.090 Uiso 0.550(5) 1 calc PR A 1 C10 C -0.0044(4) 0.1411(5) 0.1826(4) 0.085(2) Uani 0.550(5) 1 d PDU A 1 H10A H -0.0415 0.1624 0.2083 0.128 Uiso 0.550(5) 1 calc PR A 1 H10B H -0.0175 0.0842 0.1708 0.128 Uiso 0.550(5) 1 calc PR A 1 H10C H -0.0175 0.1699 0.1317 0.128 Uiso 0.550(5) 1 calc PR A 1 C8X C 0.0845(5) 0.0829(4) 0.1690(3) 0.0644(19) Uani 0.450(5) 1 d PDU A 2 H8X1 H 0.0349 0.0463 0.1604 0.097 Uiso 0.450(5) 1 calc PR A 2 H8X2 H 0.1408 0.0529 0.1883 0.097 Uiso 0.450(5) 1 calc PR A 2 H8X3 H 0.0738 0.1096 0.1175 0.097 Uiso 0.450(5) 1 calc PR A 2 C9X C 0.1679(4) 0.2004(4) 0.2435(4) 0.070(2) Uani 0.450(5) 1 d PDU A 2 H9X1 H 0.2236 0.1697 0.2703 0.106 Uiso 0.450(5) 1 calc PR A 2 H9X2 H 0.1714 0.2487 0.2752 0.106 Uiso 0.450(5) 1 calc PR A 2 H9X3 H 0.1597 0.2153 0.1885 0.106 Uiso 0.450(5) 1 calc PR A 2 C10X C 0.0014(5) 0.1894(5) 0.2004(5) 0.070(2) Uani 0.450(5) 1 d PDU A 2 H10D H -0.0442 0.1514 0.1995 0.105 Uiso 0.450(5) 1 calc PR A 2 H10E H -0.0114 0.2055 0.1445 0.105 Uiso 0.450(5) 1 calc PR A 2 H10F H 0.0008 0.2365 0.2322 0.105 Uiso 0.450(5) 1 calc PR A 2 C11 C 0.14594(13) 0.17431(13) 0.53414(13) 0.0409(5) Uani 1 1 d . . . H11A H 0.1839 0.1475 0.5862 0.049 Uiso 1 1 calc R . . H11B H 0.1742 0.2258 0.5317 0.049 Uiso 1 1 calc R . . C12 C 0.01276(13) 0.13407(11) 0.56043(10) 0.0319(4) Uani 1 1 d . . . C13 C 0.05309(13) 0.18770(11) 0.52797(11) 0.0340(4) Uani 1 1 d . . . C14 C 0.00173(13) 0.25010(11) 0.48028(11) 0.0360(4) Uani 1 1 d . . . H14 H 0.0292 0.2878 0.4589 0.043 Uiso 1 1 calc R . . C15 C -0.08840(13) 0.25912(11) 0.46290(11) 0.0336(4) Uani 1 1 d . . . C16 C -0.12413(13) 0.20650(11) 0.50013(11) 0.0338(4) Uani 1 1 d . . . H16 H -0.1851 0.2128 0.4907 0.041 Uiso 1 1 calc R . . C17 C -0.07468(13) 0.14444(11) 0.55094(11) 0.0331(4) Uani 1 1 d . . . C18 C -0.14385(15) 0.32548(13) 0.40496(13) 0.0445(5) Uani 1 1 d . . . C19 C -0.1285(2) 0.3228(2) 0.32760(16) 0.0784(10) Uani 1 1 d . . . H19A H -0.1461 0.2703 0.3018 0.118 Uiso 1 1 calc R . . H19B H -0.0649 0.3321 0.3416 0.118 Uiso 1 1 calc R . . H19C H -0.1647 0.3642 0.2897 0.118 Uiso 1 1 calc R . . C20 C -0.1132(2) 0.40599(15) 0.4473(2) 0.0857(10) Uani 1 1 d . . . H20A H -0.1470 0.4489 0.4102 0.128 Uiso 1 1 calc R . . H20B H -0.0490 0.4130 0.4624 0.128 Uiso 1 1 calc R . . H20C H -0.1240 0.4077 0.4965 0.128 Uiso 1 1 calc R . . C21 C -0.24374(17) 0.31615(18) 0.38089(16) 0.0640(7) Uani 1 1 d . . . H21A H -0.2768 0.3573 0.3410 0.096 Uiso 1 1 calc R . . H21B H -0.2554 0.3219 0.4294 0.096 Uiso 1 1 calc R . . H21C H -0.2634 0.2632 0.3568 0.096 Uiso 1 1 calc R . . C22 C -0.11588(16) 0.09789(12) 0.59774(13) 0.0437(5) Uani 1 1 d . . . H22A H -0.1799 0.1135 0.5756 0.052 Uiso 1 1 calc R . . H22B H -0.0873 0.1171 0.6548 0.052 Uiso 1 1 calc R . . N1 N 0.6631(8) 0.5494(4) 0.3482(6) 0.130(4) Uani 0.585(16) 1 d PDU B 1 C23 C 0.6429(5) 0.5786(4) 0.4049(6) 0.083(3) Uani 0.585(16) 1 d PDU B 1 C24 C 0.6340(8) 0.6010(7) 0.4730(6) 0.122(4) Uani 0.585(16) 1 d PDU B 1 N1X N 0.6622(18) 0.6166(13) 0.4456(9) 0.227(11) Uani 0.415(16) 1 d PDU B 2 C23X C 0.648(2) 0.5966(12) 0.3713(12) 0.218(9) Uani 0.415(16) 1 d PDU B 2 C24X C 0.643(3) 0.540(2) 0.3124(18) 0.321(18) Uani 0.415(16) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0902(5) 0.0700(4) 0.0358(3) 0.0290(3) 0.0296(3) 0.0449(3) B1 0.0393(12) 0.0421(12) 0.0239(9) 0.0090(9) 0.0068(9) 0.0104(9) O1 0.0441(8) 0.0388(7) 0.0267(6) 0.0104(5) 0.0137(6) 0.0121(6) O2 0.0430(8) 0.0414(8) 0.0276(6) 0.0090(5) 0.0123(6) 0.0140(6) C1 0.0268(9) 0.0411(10) 0.0278(9) 0.0118(7) 0.0101(7) 0.0075(8) C2 0.0345(10) 0.0384(10) 0.0319(9) 0.0092(8) 0.0166(8) 0.0087(8) C3 0.0363(10) 0.0515(12) 0.0312(9) 0.0116(9) 0.0167(8) 0.0079(9) C4 0.0296(10) 0.0534(12) 0.0394(11) 0.0212(9) 0.0149(8) 0.0069(9) C5 0.0301(10) 0.0407(11) 0.0481(11) 0.0142(9) 0.0148(9) 0.0021(8) C6 0.0220(9) 0.0408(10) 0.0387(10) 0.0071(8) 0.0095(8) 0.0018(7) C7 0.0469(12) 0.0616(14) 0.0430(12) 0.0260(10) 0.0194(10) 0.0044(10) C8 0.087(4) 0.058(3) 0.045(2) 0.011(2) 0.041(3) 0.001(2) C9 0.088(4) 0.048(2) 0.051(2) 0.025(2) 0.037(2) 0.008(2) C10 0.072(4) 0.110(6) 0.049(3) 0.045(4) 0.001(3) -0.013(4) C8X 0.088(5) 0.078(4) 0.036(3) 0.020(3) 0.034(3) 0.012(3) C9X 0.072(4) 0.093(5) 0.048(3) 0.024(3) 0.027(3) -0.016(3) C10X 0.063(4) 0.089(5) 0.057(4) 0.044(4) 0.026(3) 0.029(4) C11 0.0312(10) 0.0392(11) 0.0432(11) -0.0003(9) 0.0070(9) -0.0039(8) C12 0.0378(10) 0.0294(9) 0.0227(8) 0.0013(7) 0.0073(7) 0.0064(7) C13 0.0327(10) 0.0327(9) 0.0292(9) -0.0039(7) 0.0061(7) -0.0017(7) C14 0.0420(11) 0.0288(9) 0.0340(9) 0.0000(7) 0.0131(8) -0.0043(8) C15 0.0405(11) 0.0295(9) 0.0261(8) 0.0008(7) 0.0096(8) 0.0042(8) C16 0.0362(10) 0.0348(10) 0.0291(9) 0.0016(7) 0.0126(8) 0.0060(8) C17 0.0418(11) 0.0316(9) 0.0259(8) 0.0006(7) 0.0143(8) 0.0059(8) C18 0.0503(12) 0.0420(11) 0.0383(10) 0.0147(9) 0.0160(9) 0.0126(10) C19 0.082(2) 0.107(2) 0.0521(15) 0.0440(16) 0.0348(15) 0.0402(18) C20 0.099(2) 0.0369(13) 0.092(2) 0.0142(14) 0.0128(19) 0.0180(14) C21 0.0549(15) 0.0758(18) 0.0550(14) 0.0332(13) 0.0173(12) 0.0253(13) C22 0.0605(14) 0.0398(11) 0.0429(11) 0.0098(9) 0.0337(11) 0.0153(10) N1 0.209(9) 0.083(5) 0.163(8) -0.052(4) 0.141(7) -0.018(4) C23 0.091(5) 0.053(3) 0.123(6) -0.004(3) 0.064(4) 0.031(3) C24 0.160(8) 0.124(7) 0.129(7) 0.033(6) 0.106(7) 0.070(6) N1X 0.34(2) 0.217(17) 0.112(9) 0.063(10) 0.087(12) 0.186(17) C23X 0.38(2) 0.160(16) 0.184(14) 0.010(11) 0.186(16) -0.040(17) C24X 0.40(4) 0.39(4) 0.21(2) -0.13(2) 0.17(2) -0.10(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 B1 1.781(2) . ? B1 O1 1.341(3) . ? B1 O2 1.348(3) . ? O1 C1 1.394(2) . ? O2 C12 1.400(2) . ? C1 C2 1.383(3) . ? C1 C6 1.387(3) . ? C2 C3 1.394(2) . ? C2 C22 1.511(3) 5_556 ? C3 C4 1.393(3) . ? C4 C5 1.384(3) . ? C4 C7 1.536(3) . ? C5 C6 1.390(3) . ? C6 C11 1.505(3) . ? C7 C8 1.457(5) . ? C7 C10 1.475(6) . ? C7 C9X 1.478(6) . ? C7 C10X 1.485(7) . ? C7 C9 1.627(5) . ? C7 C8X 1.666(6) . ? C11 C13 1.502(3) . ? C12 C17 1.387(3) . ? C12 C13 1.388(3) . ? C13 C14 1.390(3) . ? C14 C15 1.388(3) . ? C15 C16 1.384(3) . ? C15 C18 1.535(3) . ? C16 C17 1.398(3) . ? C17 C22 1.508(3) . ? C18 C21 1.520(3) . ? C18 C19 1.526(3) . ? C18 C20 1.527(4) . ? C22 C2 1.511(3) 5_556 ? N1 C23 1.302(8) . ? C23 C24 1.355(8) . ? N1X C23X 1.309(10) . ? C23X C24X 1.408(11) . ? 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 O1 B1 O2 133.68(18) . . ? O1 B1 Cl1 112.72(15) . . ? O2 B1 Cl1 113.58(15) . . ? B1 O1 C1 135.04(16) . . ? B1 O2 C12 131.10(15) . . ? C2 C1 C6 121.80(17) . . ? C2 C1 O1 117.05(17) . . ? C6 C1 O1 120.97(17) . . ? C1 C2 C3 117.77(18) . . ? C1 C2 C22 123.84(16) . 5_556 ? C3 C2 C22 118.17(18) . 5_556 ? C4 C3 C2 122.5(2) . . ? C5 C4 C3 117.19(18) . . ? C5 C4 C7 121.9(2) . . ? C3 C4 C7 120.9(2) . . ? C4 C5 C6 122.37(19) . . ? C1 C6 C5 118.27(19) . . ? C1 C6 C11 121.18(17) . . ? C5 C6 C11 120.19(18) . . ? C8 C7 C10 118.3(5) . . ? C8 C7 C9X 56.8(4) . . ? C10 C7 C9X 137.9(4) . . ? C8 C7 C10X 136.8(4) . . ? C10 C7 C10X 33.8(4) . . ? C9X C7 C10X 116.4(5) . . ? C8 C7 C4 109.9(2) . . ? C10 C7 C4 107.9(3) . . ? C9X C7 C4 112.6(3) . . ? C10X C7 C4 111.1(3) . . ? C8 C7 C9 105.8(3) . . ? C10 C7 C9 106.1(4) . . ? C9X C7 C9 50.4(3) . . ? C10X C7 C9 73.3(4) . . ? C4 C7 C9 108.4(2) . . ? C8 C7 C8X 49.3(3) . . ? C10 C7 C8X 72.3(5) . . ? C9X C7 C8X 102.2(4) . . ? C10X C7 C8X 102.3(5) . . ? C4 C7 C8X 111.4(2) . . ? C9 C7 C8X 138.6(3) . . ? C13 C11 C6 106.55(15) . . ? C17 C12 C13 121.67(17) . . ? C17 C12 O2 117.44(17) . . ? C13 C12 O2 120.70(17) . . ? C12 C13 C14 118.41(18) . . ? C12 C13 C11 121.81(17) . . ? C14 C13 C11 119.33(18) . . ? C15 C14 C13 122.15(18) . . ? C16 C15 C14 117.07(17) . . ? C16 C15 C18 122.81(18) . . ? C14 C15 C18 120.13(18) . . ? C15 C16 C17 123.04(18) . . ? C12 C17 C16 117.29(17) . . ? C12 C17 C22 123.83(17) . . ? C16 C17 C22 118.64(17) . . ? C21 C18 C19 108.3(2) . . ? C21 C18 C20 108.7(2) . . ? C19 C18 C20 109.8(3) . . ? C21 C18 C15 112.25(18) . . ? C19 C18 C15 108.90(19) . . ? C20 C18 C15 108.81(18) . . ? C17 C22 C2 121.45(16) . 5_556 ? N1 C23 C24 169.9(9) . . ? N1X C23X C24X 152(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 B1 O1 C1 3.3(4) . . . . ? Cl1 B1 O1 C1 -178.24(17) . . . . ? O1 B1 O2 C12 1.6(4) . . . . ? Cl1 B1 O2 C12 -176.85(16) . . . . ? B1 O1 C1 C2 -140.2(2) . . . . ? B1 O1 C1 C6 44.6(3) . . . . ? C6 C1 C2 C3 -3.2(3) . . . . ? O1 C1 C2 C3 -178.34(16) . . . . ? C6 C1 C2 C22 171.22(18) . . . 5_556 ? O1 C1 C2 C22 -3.9(3) . . . 5_556 ? C1 C2 C3 C4 1.3(3) . . . . ? C22 C2 C3 C4 -173.46(19) 5_556 . . . ? C2 C3 C4 C5 0.9(3) . . . . ? C2 C3 C4 C7 -177.59(18) . . . . ? C3 C4 C5 C6 -1.3(3) . . . . ? C7 C4 C5 C6 177.15(18) . . . . ? C2 C1 C6 C5 2.8(3) . . . . ? O1 C1 C6 C5 177.76(16) . . . . ? C2 C1 C6 C11 176.02(17) . . . . ? O1 C1 C6 C11 -9.1(3) . . . . ? C4 C5 C6 C1 -0.5(3) . . . . ? C4 C5 C6 C11 -173.72(17) . . . . ? C5 C4 C7 C8 119.7(3) . . . . ? C3 C4 C7 C8 -61.8(3) . . . . ? C5 C4 C7 C10 -110.0(5) . . . . ? C3 C4 C7 C10 68.5(5) . . . . ? C5 C4 C7 C9X 58.4(4) . . . . ? C3 C4 C7 C9X -123.2(4) . . . . ? C5 C4 C7 C10X -74.2(5) . . . . ? C3 C4 C7 C10X 104.3(5) . . . . ? C5 C4 C7 C9 4.5(3) . . . . ? C3 C4 C7 C9 -177.0(3) . . . . ? C5 C4 C7 C8X 172.6(3) . . . . ? C3 C4 C7 C8X -9.0(4) . . . . ? C1 C6 C11 C13 -82.2(2) . . . . ? C5 C6 C11 C13 90.8(2) . . . . ? B1 O2 C12 C17 134.6(2) . . . . ? B1 O2 C12 C13 -50.3(3) . . . . ? C17 C12 C13 C14 -4.4(3) . . . . ? O2 C12 C13 C14 -179.24(16) . . . . ? C17 C12 C13 C11 -176.57(17) . . . . ? O2 C12 C13 C11 8.6(3) . . . . ? C6 C11 C13 C12 85.8(2) . . . . ? C6 C11 C13 C14 -86.3(2) . . . . ? C12 C13 C14 C15 -1.5(3) . . . . ? C11 C13 C14 C15 170.93(17) . . . . ? C13 C14 C15 C16 4.7(3) . . . . ? C13 C14 C15 C18 -175.61(18) . . . . ? C14 C15 C16 C17 -2.3(3) . . . . ? C18 C15 C16 C17 177.96(18) . . . . ? C13 C12 C17 C16 6.5(3) . . . . ? O2 C12 C17 C16 -178.45(15) . . . . ? C13 C12 C17 C22 -167.76(18) . . . . ? O2 C12 C17 C22 7.3(3) . . . . ? C15 C16 C17 C12 -3.1(3) . . . . ? C15 C16 C17 C22 171.49(18) . . . . ? C16 C15 C18 C21 -11.2(3) . . . . ? C14 C15 C18 C21 169.1(2) . . . . ? C16 C15 C18 C19 -131.2(2) . . . . ? C14 C15 C18 C19 49.1(3) . . . . ? C16 C15 C18 C20 109.2(3) . . . . ? C14 C15 C18 C20 -70.5(3) . . . . ? C12 C17 C22 C2 -51.9(3) . . . 5_556 ? C16 C17 C22 C2 133.8(2) . . . 5_556 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.484 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.047 #===END data_3.C7H8 _database_code_depnum_ccdc_archive 'CCDC 278176' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H62 B2 F10 O4' _chemical_formula_weight 1058.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _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 13.5632(12) _cell_length_b 14.6088(13) _cell_length_c 16.3167(14) _cell_angle_alpha 112.636(2) _cell_angle_beta 90.622(2) _cell_angle_gamma 111.418(2) _cell_volume 2734.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2798 _cell_measurement_theta_min 3.62 _cell_measurement_theta_max 26.31 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.984 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_process_details 'SADABS v2.10, Sheldrick, G.M., (2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.8466 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 16.2SMX' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3 _diffrn_reflns_number 19437 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0705 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 31.50 _reflns_number_total 10452 _reflns_number_gt 7224 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0880P)^2^+0.4741P] 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 10452 _refine_ls_number_parameters 786 _refine_ls_number_restraints 351 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.1873 _refine_ls_wR_factor_gt 0.1657 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.437 _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 B1 B 0.5866(3) 0.5302(3) 0.1961(2) 0.0211(8) Uani 1 1 d . . . B2 B 0.5072(3) 0.7499(3) 0.4229(3) 0.0245(9) Uani 1 1 d . . . O1 O 0.51488(17) 0.4539(2) 0.21753(15) 0.0274(6) Uani 1 1 d . . . O2 O 0.57416(17) 0.59564(18) 0.16089(15) 0.0239(5) Uani 1 1 d . . . O3 O 0.57009(18) 0.8052(2) 0.37922(16) 0.0282(6) Uani 1 1 d . . . O4 O 0.51065(17) 0.66826(19) 0.44154(15) 0.0253(5) Uani 1 1 d . . . F1 F 0.69056(15) 0.54561(16) 0.21597(13) 0.0298(5) Uani 1 1 d . . . C1 C 0.4031(3) 0.4111(3) 0.2079(2) 0.0224(7) Uani 1 1 d . . . C2 C 0.3583(2) 0.3995(3) 0.2810(2) 0.0199(7) Uani 1 1 d . . . C3 C 0.2466(3) 0.3441(3) 0.2668(2) 0.0211(7) Uani 1 1 d . . . H3 H 0.2144 0.3351 0.3161 0.025 Uiso 1 1 calc R . . C4 C 0.1808(3) 0.3018(3) 0.1847(2) 0.0211(7) Uani 1 1 d . A . C5 C 0.2302(3) 0.3191(3) 0.1144(2) 0.0223(7) Uani 1 1 d . . . H5 H 0.1869 0.2928 0.0575 0.027 Uiso 1 1 calc R . . C6 C 0.3403(3) 0.3732(3) 0.1246(2) 0.0210(7) Uani 1 1 d . . . C7 C 0.0585(3) 0.2379(3) 0.1693(2) 0.0278(8) Uani 1 1 d DU . . C8 C 0.0016(4) 0.2950(5) 0.1370(4) 0.0429(15) Uani 0.792(6) 1 d PDU A 1 H8A H 0.0203 0.3683 0.1836 0.064 Uiso 0.792(6) 1 calc PR A 1 H8B H -0.0764 0.2541 0.1255 0.064 Uiso 0.792(6) 1 calc PR A 1 H8C H 0.0248 0.2989 0.0813 0.064 Uiso 0.792(6) 1 calc PR A 1 C9 C 0.0304(4) 0.1236(4) 0.0988(4) 0.0460(16) Uani 0.792(6) 1 d PDU A 1 H9A H -0.0474 0.0818 0.0882 0.069 Uiso 0.792(6) 1 calc PR A 1 H9B H 0.0683 0.0891 0.1203 0.069 Uiso 0.792(6) 1 calc PR A 1 H9C H 0.0523 0.1261 0.0424 0.069 Uiso 0.792(6) 1 calc PR A 1 C10 C 0.0195(4) 0.2343(5) 0.2564(3) 0.0429(16) Uani 0.792(6) 1 d PDU A 1 H10A H 0.0374 0.3082 0.3016 0.064 Uiso 0.792(6) 1 calc PR A 1 H10B H 0.0547 0.1990 0.2794 0.064 Uiso 0.792(6) 1 calc PR A 1 H10C H -0.0587 0.1934 0.2438 0.064 Uiso 0.792(6) 1 calc PR A 1 C8X C 0.0023(14) 0.1911(19) 0.0696(11) 0.052(7) Uani 0.208(6) 1 d PDU A 2 H8X1 H 0.0346 0.1444 0.0299 0.078 Uiso 0.208(6) 1 calc PR A 2 H8X2 H 0.0115 0.2507 0.0524 0.078 Uiso 0.208(6) 1 calc PR A 2 H8X3 H -0.0746 0.1487 0.0637 0.078 Uiso 0.208(6) 1 calc PR A 2 C9X C 0.0431(16) 0.1385(16) 0.1894(17) 0.059(7) Uani 0.208(6) 1 d PDU A 2 H9X1 H 0.0780 0.0955 0.1489 0.088 Uiso 0.208(6) 1 calc PR A 2 H9X2 H -0.0339 0.0940 0.1799 0.088 Uiso 0.208(6) 1 calc PR A 2 H9X3 H 0.0755 0.1632 0.2521 0.088 Uiso 0.208(6) 1 calc PR A 2 C10X C 0.0038(16) 0.3076(17) 0.2278(15) 0.061(7) Uani 0.208(6) 1 d PDU A 2 H10D H -0.0738 0.2646 0.2164 0.091 Uiso 0.208(6) 1 calc PR A 2 H10E H 0.0171 0.3697 0.2132 0.091 Uiso 0.208(6) 1 calc PR A 2 H10F H 0.0330 0.3335 0.2916 0.091 Uiso 0.208(6) 1 calc PR A 2 C11 C 0.3904(3) 0.3980(3) 0.0490(2) 0.0239(7) Uani 1 1 d . . . H11A H 0.4621 0.3948 0.0491 0.029 Uiso 1 1 calc R . . H11B H 0.3444 0.3440 -0.0100 0.029 Uiso 1 1 calc R . . C12 C 0.4860(3) 0.6028(3) 0.1237(2) 0.0213(7) Uani 1 1 d . . . C13 C 0.4012(3) 0.5101(3) 0.0632(2) 0.0222(7) Uani 1 1 d . . . C14 C 0.3203(3) 0.5227(3) 0.0208(2) 0.0260(8) Uani 1 1 d . . . H14 H 0.2626 0.4601 -0.0212 0.031 Uiso 1 1 calc R . . C15 C 0.3214(3) 0.6238(3) 0.0379(2) 0.0290(8) Uani 1 1 d . . . C16 C 0.4081(3) 0.7139(3) 0.0994(2) 0.0269(8) Uani 1 1 d . . . H16 H 0.4103 0.7838 0.1118 0.032 Uiso 1 1 calc R . . C17 C 0.4914(3) 0.7064(3) 0.1436(2) 0.0219(7) Uani 1 1 d . . . C18 C 0.2332(3) 0.6399(3) -0.0084(3) 0.0368(9) Uani 1 1 d . . . C19 C 0.1415(3) 0.5305(4) -0.0705(3) 0.0487(11) Uani 1 1 d . . . H19A H 0.1709 0.4880 -0.1179 0.073 Uiso 1 1 calc R . . H19B H 0.0868 0.5440 -0.0981 0.073 Uiso 1 1 calc R . . H19C H 0.1087 0.4904 -0.0347 0.073 Uiso 1 1 calc R . . C20 C 0.1846(4) 0.7045(4) 0.0629(3) 0.0560(13) Uani 1 1 d . . . H20A H 0.1561 0.6669 0.1013 0.084 Uiso 1 1 calc R . . H20B H 0.1263 0.7118 0.0335 0.084 Uiso 1 1 calc R . . H20C H 0.2402 0.7765 0.0998 0.084 Uiso 1 1 calc R . . C21 C 0.2825(4) 0.6983(4) -0.0676(3) 0.0459(11) Uani 1 1 d . . . H21A H 0.3374 0.7703 -0.0297 0.069 Uiso 1 1 calc R . . H21B H 0.2261 0.7056 -0.0995 0.069 Uiso 1 1 calc R . . H21C H 0.3156 0.6565 -0.1116 0.069 Uiso 1 1 calc R . . C22 C 0.5799(3) 0.8127(3) 0.2093(2) 0.0276(8) Uani 1 1 d . . . H22A H 0.6116 0.8553 0.1743 0.033 Uiso 1 1 calc R . . H22B H 0.5444 0.8528 0.2532 0.033 Uiso 1 1 calc R . . C23 C 0.6658(3) 0.8085(3) 0.3457(2) 0.0223(7) Uani 1 1 d . . . C24 C 0.6725(3) 0.8142(3) 0.2630(2) 0.0244(8) Uani 1 1 d . . . C25 C 0.7693(3) 0.8256(3) 0.2317(2) 0.0250(8) Uani 1 1 d . . . H25 H 0.7745 0.8285 0.1747 0.030 Uiso 1 1 calc R . . C26 C 0.8589(3) 0.8328(3) 0.2801(2) 0.0252(8) Uani 1 1 d . . . C27 C 0.8479(3) 0.8278(3) 0.3632(2) 0.0240(7) Uani 1 1 d . . . H27 H 0.9080 0.8330 0.3979 0.029 Uiso 1 1 calc R . . C28 C 0.7529(3) 0.8154(3) 0.3973(2) 0.0220(7) Uani 1 1 d . . . C29 C 0.9679(3) 0.8505(3) 0.2483(3) 0.0336(9) Uani 1 1 d . . . C30 C 0.9608(4) 0.8355(5) 0.1509(3) 0.0584(14) Uani 1 1 d . . . H30A H 0.9090 0.7622 0.1120 0.088 Uiso 1 1 calc R . . H30B H 1.0317 0.8462 0.1334 0.088 Uiso 1 1 calc R . . H30C H 0.9371 0.8885 0.1442 0.088 Uiso 1 1 calc R . . C31 C 1.0484(3) 0.9657(4) 0.3100(3) 0.0588(14) Uani 1 1 d . . . H31A H 1.1196 0.9770 0.2931 0.088 Uiso 1 1 calc R . . H31B H 1.0523 0.9751 0.3729 0.088 Uiso 1 1 calc R . . H31C H 1.0245 1.0185 0.3032 0.088 Uiso 1 1 calc R . . C32 C 1.0104(4) 0.7702(4) 0.2573(3) 0.0544(12) Uani 1 1 d . . . H32A H 0.9577 0.6961 0.2221 0.082 Uiso 1 1 calc R . . H32B H 1.0222 0.7832 0.3209 0.082 Uiso 1 1 calc R . . H32C H 1.0785 0.7800 0.2347 0.082 Uiso 1 1 calc R . . C33 C 0.7426(3) 0.7978(3) 0.4830(2) 0.0252(8) Uani 1 1 d . . . H33A H 0.8143 0.8307 0.5212 0.030 Uiso 1 1 calc R . . H33B H 0.6964 0.8319 0.5178 0.030 Uiso 1 1 calc R . . C34 C 0.5823(3) 0.6167(3) 0.4301(2) 0.0213(7) Uani 1 1 d . . . C35 C 0.6931(3) 0.6774(3) 0.4562(2) 0.0215(7) Uani 1 1 d . . . C36 C 0.7590(3) 0.6209(3) 0.4470(2) 0.0233(7) Uani 1 1 d . . . H36 H 0.8346 0.6610 0.4649 0.028 Uiso 1 1 calc R . . C37 C 0.7191(3) 0.5088(3) 0.4129(2) 0.0230(7) Uani 1 1 d . . . C38 C 0.6076(3) 0.4530(3) 0.3906(2) 0.0224(7) Uani 1 1 d . . . H38 H 0.5778 0.3764 0.3689 0.027 Uiso 1 1 calc R . . C39 C 0.5383(3) 0.5052(3) 0.3988(2) 0.0221(7) Uani 1 1 d . . . C40 C 0.7965(3) 0.4517(3) 0.4017(2) 0.0282(8) Uani 1 1 d . . . C41 C 0.8850(3) 0.4947(4) 0.3529(3) 0.0429(10) Uani 1 1 d . . . H41A H 0.8527 0.4813 0.2932 0.064 Uiso 1 1 calc R . . H41B H 0.9339 0.4577 0.3461 0.064 Uiso 1 1 calc R . . H41C H 0.9252 0.5726 0.3880 0.064 Uiso 1 1 calc R . . C42 C 0.7389(4) 0.3294(3) 0.3475(3) 0.0521(12) Uani 1 1 d . . . H42A H 0.6835 0.2995 0.3790 0.078 Uiso 1 1 calc R . . H42B H 0.7910 0.2962 0.3411 0.078 Uiso 1 1 calc R . . H42C H 0.7052 0.3140 0.2876 0.078 Uiso 1 1 calc R . . C43 C 0.8473(4) 0.4751(4) 0.4959(3) 0.0504(12) Uani 1 1 d . . . H43A H 0.8890 0.5531 0.5293 0.076 Uiso 1 1 calc R . . H43B H 0.8950 0.4369 0.4901 0.076 Uiso 1 1 calc R . . H43C H 0.7905 0.4502 0.5284 0.076 Uiso 1 1 calc R . . C44 C 0.4180(3) 0.4395(3) 0.3759(2) 0.0265(8) Uani 1 1 d . . . H44A H 0.3845 0.4836 0.4185 0.032 Uiso 1 1 calc R . . H44B H 0.4042 0.3753 0.3886 0.032 Uiso 1 1 calc R . . C45 C 0.4112(3) 0.7863(3) 0.4581(2) 0.0248(8) Uani 1 1 d . . . C46 C 0.4227(3) 0.8663(3) 0.5447(2) 0.0266(8) Uani 1 1 d . . . C47 C 0.3379(3) 0.8926(3) 0.5764(2) 0.0286(8) Uani 1 1 d . . . H47 H 0.3489 0.9472 0.6353 0.034 Uiso 1 1 calc R . . C48 C 0.2372(3) 0.8394(3) 0.5225(2) 0.0258(8) Uani 1 1 d . . . C49 C 0.2230(3) 0.7622(3) 0.4361(2) 0.0245(8) Uani 1 1 d . . . H49 H 0.1546 0.7263 0.3981 0.029 Uiso 1 1 calc R . . C50 C 0.3090(3) 0.7369(3) 0.4047(2) 0.0241(8) Uani 1 1 d . . . C51 C 0.5299(3) 0.9258(3) 0.6068(3) 0.0383(10) Uani 1 1 d . . . F2 F 0.60804(19) 0.9771(2) 0.57145(18) 0.0606(8) Uani 1 1 d . . . F3 F 0.5632(2) 0.8574(2) 0.62341(15) 0.0512(7) Uani 1 1 d . . . F4 F 0.5288(2) 0.9969(2) 0.68712(17) 0.0697(9) Uani 1 1 d . . . C52 C 0.1432(3) 0.8626(3) 0.5560(3) 0.0354(9) Uani 1 1 d . . . F5 F 0.05654(19) 0.7715(2) 0.5380(2) 0.0692(9) Uani 1 1 d . . . F6 F 0.1134(2) 0.9159(2) 0.5172(2) 0.0672(8) Uani 1 1 d . . . F7 F 0.16127(18) 0.9212(2) 0.64386(16) 0.0532(7) Uani 1 1 d . . . C53 C 0.2846(3) 0.6537(3) 0.3094(2) 0.0334(9) Uani 1 1 d . . . F8 F 0.2638(3) 0.6906(3) 0.25164(16) 0.0788(10) Uani 1 1 d . . . F9 F 0.1981(2) 0.5643(2) 0.29540(18) 0.0733(10) Uani 1 1 d . . . F10 F 0.36403(17) 0.62239(18) 0.28461(14) 0.0389(6) Uani 1 1 d . . . C54 C 0.7119(11) 1.0431(9) 0.1160(6) 0.096(4) Uani 0.568(5) 1 d PDU B 1 H54A H 0.6685 1.0006 0.1467 0.144 Uiso 0.568(5) 1 calc PR B 1 H54B H 0.6995 1.1095 0.1323 0.144 Uiso 0.568(5) 1 calc PR B 1 H54C H 0.7883 1.0619 0.1344 0.144 Uiso 0.568(5) 1 calc PR B 1 C55 C 0.6788(6) 0.9745(6) 0.0109(5) 0.0615(19) Uani 0.568(5) 1 d PDU B 1 C56 C 0.5996(7) 0.8758(6) -0.0202(6) 0.063(2) Uani 0.568(5) 1 d PDU B 1 H56 H 0.5636 0.8458 0.0189 0.075 Uiso 0.568(5) 1 calc PR B 1 C57 C 0.5737(8) 0.8206(7) -0.1123(7) 0.064(2) Uani 0.568(5) 1 d PDU B 1 H57 H 0.5162 0.7511 -0.1385 0.077 Uiso 0.568(5) 1 calc PR B 1 C58 C 0.6297(8) 0.8644(7) -0.1675(6) 0.063(2) Uani 0.568(5) 1 d PDU B 1 H58 H 0.6135 0.8254 -0.2313 0.075 Uiso 0.568(5) 1 calc PR B 1 C59 C 0.7089(7) 0.9651(7) -0.1274(6) 0.069(2) Uani 0.568(5) 1 d PDU B 1 H59 H 0.7495 0.9969 -0.1637 0.083 Uiso 0.568(5) 1 calc PR B 1 C60 C 0.7320(7) 1.0233(6) -0.0333(6) 0.063(2) Uani 0.568(5) 1 d PDU B 1 H60 H 0.7847 1.0954 -0.0047 0.075 Uiso 0.568(5) 1 calc PR B 1 C54X C 0.5503(15) 0.8580(14) -0.1401(8) 0.131(6) Uani 0.432(5) 1 d PDU B 2 H54D H 0.5999 0.8322 -0.1759 0.196 Uiso 0.432(5) 1 calc PR B 2 H54E H 0.5337 0.9067 -0.1603 0.196 Uiso 0.432(5) 1 calc PR B 2 H54F H 0.4838 0.7961 -0.1479 0.196 Uiso 0.432(5) 1 calc PR B 2 C55X C 0.6027(9) 0.9188(9) -0.0406(8) 0.078(3) Uani 0.432(5) 1 d PDU B 2 C56X C 0.6920(9) 0.9062(10) -0.0258(9) 0.080(3) Uani 0.432(5) 1 d PDU B 2 H56X H 0.7193 0.8644 -0.0724 0.096 Uiso 0.432(5) 1 calc PR B 2 C57X C 0.7411(10) 0.9582(11) 0.0615(10) 0.094(3) Uani 0.432(5) 1 d PDU B 2 H57X H 0.8059 0.9525 0.0765 0.113 Uiso 0.432(5) 1 calc PR B 2 C58X C 0.7021(13) 1.0194(12) 0.1306(9) 0.086(4) Uani 0.432(5) 1 d PDU B 2 H58X H 0.7370 1.0535 0.1918 0.104 Uiso 0.432(5) 1 calc PR B 2 C59X C 0.6107(11) 1.0275(9) 0.1051(9) 0.089(3) Uani 0.432(5) 1 d PDU B 2 H59X H 0.5817 1.0709 0.1485 0.107 Uiso 0.432(5) 1 calc PR B 2 C60X C 0.5586(9) 0.9705(9) 0.0129(8) 0.074(3) Uani 0.432(5) 1 d PDU B 2 H60X H 0.4933 0.9723 -0.0063 0.089 Uiso 0.432(5) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0177(19) 0.027(2) 0.0172(18) 0.0071(16) 0.0058(15) 0.0102(16) B2 0.0191(19) 0.030(2) 0.021(2) 0.0076(17) 0.0026(15) 0.0095(17) O1 0.0161(12) 0.0427(15) 0.0233(13) 0.0172(11) 0.0044(10) 0.0081(11) O2 0.0190(12) 0.0251(13) 0.0243(13) 0.0068(10) 0.0003(10) 0.0093(10) O3 0.0206(12) 0.0366(15) 0.0326(14) 0.0167(12) 0.0082(10) 0.0145(11) O4 0.0196(12) 0.0341(14) 0.0254(13) 0.0118(11) 0.0068(10) 0.0145(11) F1 0.0234(11) 0.0358(12) 0.0356(12) 0.0199(10) 0.0068(9) 0.0122(9) C1 0.0163(16) 0.0285(19) 0.0220(17) 0.0107(15) 0.0047(13) 0.0084(14) C2 0.0162(16) 0.0248(18) 0.0188(16) 0.0087(14) 0.0030(13) 0.0086(14) C3 0.0199(17) 0.0251(18) 0.0191(17) 0.0109(14) 0.0055(13) 0.0080(14) C4 0.0168(16) 0.0229(18) 0.0232(17) 0.0098(14) 0.0032(13) 0.0072(14) C5 0.0221(18) 0.0247(18) 0.0155(16) 0.0052(14) -0.0004(13) 0.0080(15) C6 0.0207(17) 0.0224(17) 0.0164(16) 0.0068(14) 0.0049(13) 0.0064(14) C7 0.0159(17) 0.036(2) 0.0265(19) 0.0140(16) 0.0007(14) 0.0047(15) C8 0.021(3) 0.059(4) 0.053(4) 0.028(3) 0.001(2) 0.016(2) C9 0.029(3) 0.034(3) 0.053(4) 0.009(3) 0.002(2) -0.002(2) C10 0.018(2) 0.066(4) 0.039(3) 0.028(3) 0.007(2) 0.004(2) C8X 0.013(9) 0.077(17) 0.039(9) 0.023(10) -0.011(8) -0.009(9) C9X 0.030(11) 0.054(12) 0.080(17) 0.044(12) -0.014(11) -0.013(9) C10X 0.029(11) 0.068(15) 0.062(14) 0.011(11) 0.014(10) 0.012(10) C11 0.0233(18) 0.0275(19) 0.0140(16) 0.0052(14) 0.0025(13) 0.0067(15) C12 0.0181(16) 0.034(2) 0.0145(16) 0.0110(14) 0.0050(13) 0.0117(15) C13 0.0202(17) 0.035(2) 0.0132(16) 0.0124(15) 0.0077(13) 0.0106(15) C14 0.0194(17) 0.038(2) 0.0170(17) 0.0120(16) 0.0035(13) 0.0071(15) C15 0.0236(19) 0.049(2) 0.0203(18) 0.0191(17) 0.0075(14) 0.0155(17) C16 0.0271(19) 0.038(2) 0.0231(18) 0.0159(16) 0.0079(15) 0.0176(17) C17 0.0221(17) 0.0312(19) 0.0157(16) 0.0114(14) 0.0077(13) 0.0124(15) C18 0.028(2) 0.058(3) 0.034(2) 0.024(2) 0.0033(16) 0.0213(19) C19 0.030(2) 0.067(3) 0.048(3) 0.025(2) -0.0021(19) 0.019(2) C20 0.054(3) 0.092(4) 0.041(3) 0.024(3) 0.006(2) 0.053(3) C21 0.048(3) 0.063(3) 0.041(2) 0.028(2) 0.004(2) 0.029(2) C22 0.029(2) 0.0261(19) 0.0297(19) 0.0125(16) 0.0013(15) 0.0119(16) C23 0.0187(17) 0.0200(17) 0.0257(18) 0.0076(14) 0.0056(14) 0.0072(14) C24 0.0261(18) 0.0183(17) 0.0245(18) 0.0065(14) 0.0022(14) 0.0071(14) C25 0.0262(19) 0.0204(18) 0.0238(18) 0.0075(15) 0.0053(14) 0.0061(15) C26 0.0222(18) 0.0189(17) 0.0270(19) 0.0039(15) 0.0061(14) 0.0064(14) C27 0.0202(17) 0.0214(18) 0.0261(18) 0.0066(15) 0.0002(14) 0.0074(14) C28 0.0227(17) 0.0182(17) 0.0203(17) 0.0037(14) 0.0015(13) 0.0078(14) C29 0.0253(19) 0.037(2) 0.032(2) 0.0103(17) 0.0106(16) 0.0107(17) C30 0.037(3) 0.099(4) 0.046(3) 0.035(3) 0.024(2) 0.029(3) C31 0.030(2) 0.050(3) 0.069(3) 0.011(2) 0.020(2) 0.001(2) C32 0.046(3) 0.072(3) 0.057(3) 0.024(3) 0.023(2) 0.039(3) C33 0.0207(17) 0.0274(19) 0.0209(17) 0.0049(15) 0.0004(14) 0.0081(15) C34 0.0180(17) 0.035(2) 0.0168(16) 0.0130(15) 0.0051(13) 0.0146(15) C35 0.0244(18) 0.0294(19) 0.0123(15) 0.0094(14) 0.0022(13) 0.0118(15) C36 0.0167(16) 0.034(2) 0.0199(17) 0.0131(15) 0.0014(13) 0.0095(15) C37 0.0246(18) 0.032(2) 0.0171(17) 0.0136(15) 0.0045(14) 0.0129(15) C38 0.0248(18) 0.0282(19) 0.0170(17) 0.0124(14) 0.0025(14) 0.0106(15) C39 0.0205(17) 0.032(2) 0.0134(16) 0.0112(14) 0.0017(13) 0.0078(15) C40 0.0274(19) 0.033(2) 0.031(2) 0.0157(17) 0.0057(15) 0.0157(16) C41 0.042(2) 0.050(3) 0.051(3) 0.024(2) 0.023(2) 0.029(2) C42 0.042(3) 0.037(2) 0.080(3) 0.020(2) 0.011(2) 0.024(2) C43 0.050(3) 0.081(3) 0.046(3) 0.036(3) 0.009(2) 0.044(3) C44 0.0210(18) 0.036(2) 0.0201(18) 0.0142(16) 0.0028(14) 0.0059(15) C45 0.0229(18) 0.0287(19) 0.0250(18) 0.0116(15) 0.0067(14) 0.0123(15) C46 0.0247(18) 0.0274(19) 0.0271(19) 0.0091(15) 0.0045(15) 0.0124(15) C47 0.0279(19) 0.0254(19) 0.029(2) 0.0062(16) 0.0060(15) 0.0120(16) C48 0.0237(18) 0.0245(19) 0.031(2) 0.0117(16) 0.0083(15) 0.0115(15) C49 0.0229(18) 0.0289(19) 0.0236(18) 0.0107(15) 0.0061(14) 0.0126(15) C50 0.0250(18) 0.0294(19) 0.0221(18) 0.0120(15) 0.0070(14) 0.0139(15) C51 0.033(2) 0.043(2) 0.030(2) 0.0019(18) 0.0031(17) 0.0216(19) F2 0.0306(14) 0.0635(18) 0.0649(18) 0.0223(14) -0.0026(12) -0.0002(12) F3 0.0502(15) 0.0668(17) 0.0369(14) 0.0111(12) -0.0064(11) 0.0353(14) F4 0.0489(16) 0.078(2) 0.0436(15) -0.0256(14) -0.0131(12) 0.0395(15) C52 0.027(2) 0.030(2) 0.039(2) 0.0032(18) 0.0064(17) 0.0121(17) F5 0.0320(14) 0.0422(15) 0.095(2) -0.0016(14) 0.0317(14) 0.0053(12) F6 0.0666(19) 0.090(2) 0.076(2) 0.0355(17) 0.0239(15) 0.0635(18) F7 0.0380(13) 0.0604(17) 0.0423(14) -0.0009(12) 0.0161(11) 0.0231(12) C53 0.0234(19) 0.051(3) 0.0233(19) 0.0101(18) 0.0052(15) 0.0175(18) F8 0.125(3) 0.128(3) 0.0254(13) 0.0265(16) 0.0136(15) 0.101(2) F9 0.0405(15) 0.0629(19) 0.0523(17) -0.0188(13) 0.0163(13) -0.0022(13) F10 0.0355(12) 0.0524(14) 0.0261(11) 0.0052(10) 0.0082(9) 0.0265(11) C54 0.090(7) 0.071(7) 0.088(4) 0.057(4) -0.003(6) -0.036(6) C55 0.057(4) 0.048(4) 0.089(3) 0.044(3) 0.016(3) 0.014(3) C56 0.060(4) 0.047(4) 0.085(3) 0.036(3) 0.022(4) 0.017(3) C57 0.064(5) 0.054(4) 0.084(4) 0.033(3) 0.012(4) 0.028(3) C58 0.069(5) 0.057(4) 0.074(4) 0.027(3) 0.018(4) 0.037(3) C59 0.067(5) 0.067(4) 0.084(4) 0.041(4) 0.026(4) 0.029(3) C60 0.056(5) 0.052(4) 0.083(4) 0.040(3) 0.013(4) 0.012(3) C54X 0.125(11) 0.099(11) 0.117(6) 0.021(8) -0.007(7) 0.017(9) C55X 0.073(5) 0.049(5) 0.110(5) 0.032(4) 0.013(4) 0.023(4) C56X 0.067(5) 0.050(5) 0.128(5) 0.040(4) 0.033(4) 0.025(4) C57X 0.068(6) 0.060(6) 0.149(6) 0.064(5) -0.001(5) 0.000(4) C58X 0.088(7) 0.056(7) 0.086(5) 0.058(5) -0.003(5) -0.032(6) C59X 0.093(7) 0.046(6) 0.110(5) 0.039(5) 0.033(5) 0.000(5) C60X 0.064(5) 0.049(5) 0.124(5) 0.043(4) 0.013(4) 0.030(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O2 1.346(4) . ? B1 O1 1.352(4) . ? B1 F1 1.359(4) . ? B2 O4 1.355(5) . ? B2 O3 1.357(5) . ? B2 C45 1.611(5) . ? O1 C1 1.393(4) . ? O2 C12 1.391(4) . ? O3 C23 1.406(4) . ? O4 C34 1.405(4) . ? C1 C2 1.384(4) . ? C1 C6 1.390(4) . ? C2 C3 1.399(4) . ? C2 C44 1.526(4) . ? C3 C4 1.381(4) . ? C4 C5 1.395(5) . ? C4 C7 1.538(4) . ? C5 C6 1.383(5) . ? C6 C11 1.517(4) . ? C7 C9 1.518(6) . ? C7 C10X 1.522(15) . ? C7 C10 1.534(6) . ? C7 C8 1.539(6) . ? C7 C9X 1.551(16) . ? C7 C8X 1.560(14) . ? C11 C13 1.513(5) . ? C12 C13 1.393(5) . ? C12 C17 1.393(5) . ? C13 C14 1.395(5) . ? C14 C15 1.387(5) . ? C15 C16 1.396(5) . ? C15 C18 1.543(5) . ? C16 C17 1.394(5) . ? C17 C22 1.527(5) . ? C18 C20 1.518(6) . ? C18 C21 1.531(6) . ? C18 C19 1.550(6) . ? C22 C24 1.511(5) . ? C23 C24 1.386(5) . ? C23 C28 1.393(4) . ? C24 C25 1.391(5) . ? C25 C26 1.390(5) . ? C26 C27 1.392(5) . ? C26 C29 1.536(5) . ? C27 C28 1.388(5) . ? C28 C33 1.516(5) . ? C29 C30 1.517(6) . ? C29 C32 1.535(6) . ? C29 C31 1.539(6) . ? C33 C35 1.509(5) . ? C34 C39 1.383(5) . ? C34 C35 1.396(5) . ? C35 C36 1.396(5) . ? C36 C37 1.388(5) . ? C37 C38 1.394(5) . ? C37 C40 1.536(5) . ? C38 C39 1.389(5) . ? C39 C44 1.514(5) . ? C40 C41 1.525(5) . ? C40 C42 1.528(5) . ? C40 C43 1.535(5) . ? C45 C50 1.401(5) . ? C45 C46 1.406(5) . ? C46 C47 1.385(5) . ? C46 C51 1.505(5) . ? C47 C48 1.384(5) . ? C48 C49 1.381(5) . ? C48 C52 1.493(5) . ? C49 C50 1.393(5) . ? C50 C53 1.498(5) . ? C51 F4 1.326(4) . ? C51 F2 1.336(5) . ? C51 F3 1.347(5) . ? C52 F7 1.320(4) . ? C52 F6 1.332(5) . ? C52 F5 1.337(4) . ? C53 F8 1.324(5) . ? C53 F10 1.328(4) . ? C53 F9 1.334(5) . ? C54 C55 1.574(6) . ? C55 C60 1.257(10) . ? C55 C56 1.336(9) . ? C56 C57 1.372(11) . ? C57 C58 1.379(13) . ? C58 C59 1.355(11) . ? C59 C60 1.403(11) . ? C54X C55X 1.527(6) . ? C55X C60X 1.234(12) . ? C55X C56X 1.323(11) . ? C56X C57X 1.352(14) . ? C57X C58X 1.390(15) . ? C58X C59X 1.363(15) . ? C59X C60X 1.428(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 O2 B1 O1 131.8(3) . . ? O2 B1 F1 114.1(3) . . ? O1 B1 F1 114.0(3) . . ? O4 B2 O3 131.0(3) . . ? O4 B2 C45 114.1(3) . . ? O3 B2 C45 114.9(3) . . ? B1 O1 C1 133.6(3) . . ? B1 O2 C12 134.5(3) . . ? B2 O3 C23 134.5(3) . . ? B2 O4 C34 134.0(3) . . ? C2 C1 C6 121.9(3) . . ? C2 C1 O1 117.9(3) . . ? C6 C1 O1 119.9(3) . . ? C1 C2 C3 117.1(3) . . ? C1 C2 C44 126.9(3) . . ? C3 C2 C44 115.9(3) . . ? C4 C3 C2 123.3(3) . . ? C3 C4 C5 116.9(3) . . ? C3 C4 C7 122.7(3) . . ? C5 C4 C7 120.4(3) . . ? C6 C5 C4 122.2(3) . . ? C5 C6 C1 118.5(3) . . ? C5 C6 C11 120.7(3) . . ? C1 C6 C11 120.6(3) . . ? C9 C7 C10X 140.0(9) . . ? C9 C7 C10 109.8(4) . . ? C10X C7 C10 54.5(10) . . ? C9 C7 C4 108.5(3) . . ? C10X C7 C4 111.5(9) . . ? C10 C7 C4 112.1(3) . . ? C9 C7 C8 110.8(4) . . ? C10X C7 C8 55.3(10) . . ? C10 C7 C8 107.2(4) . . ? C4 C7 C8 108.5(3) . . ? C9 C7 C9X 54.6(9) . . ? C10X C7 C9X 112.9(13) . . ? C10 C7 C9X 60.5(10) . . ? C4 C7 C9X 105.9(8) . . ? C8 C7 C9X 145.5(8) . . ? C9 C7 C8X 54.4(9) . . ? C10X C7 C8X 107.2(13) . . ? C10 C7 C8X 134.5(8) . . ? C4 C7 C8X 113.4(7) . . ? C8 C7 C8X 57.8(10) . . ? C9X C7 C8X 105.9(12) . . ? C13 C11 C6 108.5(3) . . ? O2 C12 C13 120.7(3) . . ? O2 C12 C17 116.9(3) . . ? C13 C12 C17 122.1(3) . . ? C12 C13 C14 118.3(3) . . ? C12 C13 C11 121.7(3) . . ? C14 C13 C11 119.8(3) . . ? C15 C14 C13 122.1(3) . . ? C14 C15 C16 117.2(3) . . ? C14 C15 C18 123.1(3) . . ? C16 C15 C18 119.7(3) . . ? C17 C16 C15 123.2(3) . . ? C12 C17 C16 117.0(3) . . ? C12 C17 C22 126.2(3) . . ? C16 C17 C22 116.7(3) . . ? C20 C18 C21 110.9(4) . . ? C20 C18 C15 109.5(3) . . ? C21 C18 C15 109.2(3) . . ? C20 C18 C19 108.1(3) . . ? C21 C18 C19 107.3(3) . . ? C15 C18 C19 111.9(3) . . ? C24 C22 C17 121.3(3) . . ? C24 C23 C28 121.9(3) . . ? C24 C23 O3 116.9(3) . . ? C28 C23 O3 121.0(3) . . ? C23 C24 C25 117.7(3) . . ? C23 C24 C22 121.9(3) . . ? C25 C24 C22 120.4(3) . . ? C26 C25 C24 123.0(3) . . ? C25 C26 C27 116.7(3) . . ? C25 C26 C29 123.5(3) . . ? C27 C26 C29 119.7(3) . . ? C28 C27 C26 122.7(3) . . ? C27 C28 C23 117.9(3) . . ? C27 C28 C33 119.9(3) . . ? C23 C28 C33 121.9(3) . . ? C30 C29 C32 108.1(3) . . ? C30 C29 C26 112.5(3) . . ? C32 C29 C26 110.0(3) . . ? C30 C29 C31 109.8(4) . . ? C32 C29 C31 108.1(4) . . ? C26 C29 C31 108.3(3) . . ? C35 C33 C28 107.6(3) . . ? C39 C34 C35 121.8(3) . . ? C39 C34 O4 117.4(3) . . ? C35 C34 O4 120.6(3) . . ? C36 C35 C34 117.4(3) . . ? C36 C35 C33 120.0(3) . . ? C34 C35 C33 122.2(3) . . ? C37 C36 C35 122.9(3) . . ? C36 C37 C38 116.9(3) . . ? C36 C37 C40 120.2(3) . . ? C38 C37 C40 122.9(3) . . ? C39 C38 C37 122.4(3) . . ? C34 C39 C38 118.4(3) . . ? C34 C39 C44 122.1(3) . . ? C38 C39 C44 119.4(3) . . ? C41 C40 C42 108.1(3) . . ? C41 C40 C43 109.2(3) . . ? C42 C40 C43 109.1(3) . . ? C41 C40 C37 110.2(3) . . ? C42 C40 C37 112.0(3) . . ? C43 C40 C37 108.2(3) . . ? C39 C44 C2 119.6(3) . . ? C50 C45 C46 115.6(3) . . ? C50 C45 B2 121.5(3) . . ? C46 C45 B2 122.8(3) . . ? C47 C46 C45 122.4(3) . . ? C47 C46 C51 117.7(3) . . ? C45 C46 C51 119.8(3) . . ? C48 C47 C46 120.2(3) . . ? C49 C48 C47 119.3(3) . . ? C49 C48 C52 119.2(3) . . ? C47 C48 C52 121.5(3) . . ? C48 C49 C50 120.0(3) . . ? C49 C50 C45 122.4(3) . . ? C49 C50 C53 115.2(3) . . ? C45 C50 C53 122.4(3) . . ? F4 C51 F2 108.2(4) . . ? F4 C51 F3 105.5(3) . . ? F2 C51 F3 104.9(3) . . ? F4 C51 C46 113.6(3) . . ? F2 C51 C46 112.6(3) . . ? F3 C51 C46 111.4(3) . . ? F7 C52 F6 106.4(3) . . ? F7 C52 F5 106.9(3) . . ? F6 C52 F5 105.8(3) . . ? F7 C52 C48 113.4(3) . . ? F6 C52 C48 112.4(3) . . ? F5 C52 C48 111.6(3) . . ? F8 C53 F10 106.5(3) . . ? F8 C53 F9 106.5(3) . . ? F10 C53 F9 106.5(3) . . ? F8 C53 C50 111.2(3) . . ? F10 C53 C50 113.9(3) . . ? F9 C53 C50 111.9(3) . . ? C60 C55 C56 128.4(8) . . ? C60 C55 C54 113.3(7) . . ? C56 C55 C54 118.4(7) . . ? C55 C56 C57 115.5(7) . . ? C56 C57 C58 121.1(8) . . ? C59 C58 C57 117.5(8) . . ? C58 C59 C60 121.3(7) . . ? C55 C60 C59 116.1(7) . . ? C60X C55X C56X 129.7(10) . . ? C60X C55X C54X 118.4(11) . . ? C56X C55X C54X 111.9(11) . . ? C55X C56X C57X 114.1(10) . . ? C56X C57X C58X 123.7(11) . . ? C59X C58X C57X 115.8(11) . . ? C58X C59X C60X 119.9(10) . . ? C55X C60X C59X 116.8(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 B1 O1 C1 3.4(6) . . . . ? F1 B1 O1 C1 -178.6(3) . . . . ? O1 B1 O2 C12 -8.9(6) . . . . ? F1 B1 O2 C12 173.0(3) . . . . ? O4 B2 O3 C23 -7.7(7) . . . . ? C45 B2 O3 C23 172.9(3) . . . . ? O3 B2 O4 C34 5.9(6) . . . . ? C45 B2 O4 C34 -174.7(3) . . . . ? B1 O1 C1 C2 -134.2(4) . . . . ? B1 O1 C1 C6 51.3(5) . . . . ? C6 C1 C2 C3 2.3(5) . . . . ? O1 C1 C2 C3 -172.1(3) . . . . ? C6 C1 C2 C44 -178.6(3) . . . . ? O1 C1 C2 C44 7.0(5) . . . . ? C1 C2 C3 C4 -0.2(5) . . . . ? C44 C2 C3 C4 -179.4(3) . . . . ? C2 C3 C4 C5 -1.8(5) . . . . ? C2 C3 C4 C7 177.9(3) . . . . ? C3 C4 C5 C6 1.8(5) . . . . ? C7 C4 C5 C6 -178.0(3) . . . . ? C4 C5 C6 C1 0.2(5) . . . . ? C4 C5 C6 C11 -175.3(3) . . . . ? C2 C1 C6 C5 -2.3(5) . . . . ? O1 C1 C6 C5 172.0(3) . . . . ? C2 C1 C6 C11 173.2(3) . . . . ? O1 C1 C6 C11 -12.5(5) . . . . ? C3 C4 C7 C9 -117.5(4) . . . . ? C5 C4 C7 C9 62.2(5) . . . . ? C3 C4 C7 C10X 63.0(12) . . . . ? C5 C4 C7 C10X -117.3(12) . . . . ? C3 C4 C7 C10 3.9(5) . . . . ? C5 C4 C7 C10 -176.4(4) . . . . ? C3 C4 C7 C8 122.1(4) . . . . ? C5 C4 C7 C8 -58.2(4) . . . . ? C3 C4 C7 C9X -60.1(11) . . . . ? C5 C4 C7 C9X 119.6(11) . . . . ? C3 C4 C7 C8X -175.8(11) . . . . ? C5 C4 C7 C8X 3.9(11) . . . . ? C5 C6 C11 C13 93.3(4) . . . . ? C1 C6 C11 C13 -82.1(4) . . . . ? B1 O2 C12 C13 -43.7(5) . . . . ? B1 O2 C12 C17 141.8(3) . . . . ? O2 C12 C13 C14 -173.4(3) . . . . ? C17 C12 C13 C14 0.8(5) . . . . ? O2 C12 C13 C11 11.9(4) . . . . ? C17 C12 C13 C11 -173.9(3) . . . . ? C6 C11 C13 C12 80.8(4) . . . . ? C6 C11 C13 C14 -93.8(3) . . . . ? C12 C13 C14 C15 -0.7(5) . . . . ? C11 C13 C14 C15 174.0(3) . . . . ? C13 C14 C15 C16 0.5(5) . . . . ? C13 C14 C15 C18 179.8(3) . . . . ? C14 C15 C16 C17 -0.2(5) . . . . ? C18 C15 C16 C17 -179.6(3) . . . . ? O2 C12 C17 C16 173.8(3) . . . . ? C13 C12 C17 C16 -0.6(5) . . . . ? O2 C12 C17 C22 -6.1(5) . . . . ? C13 C12 C17 C22 179.5(3) . . . . ? C15 C16 C17 C12 0.3(5) . . . . ? C15 C16 C17 C22 -179.7(3) . . . . ? C14 C15 C18 C20 123.4(4) . . . . ? C16 C15 C18 C20 -57.4(5) . . . . ? C14 C15 C18 C21 -115.1(4) . . . . ? C16 C15 C18 C21 64.2(4) . . . . ? C14 C15 C18 C19 3.6(5) . . . . ? C16 C15 C18 C19 -177.2(3) . . . . ? C12 C17 C22 C24 -1.8(5) . . . . ? C16 C17 C22 C24 178.2(3) . . . . ? B2 O3 C23 C24 139.8(4) . . . . ? B2 O3 C23 C28 -45.8(5) . . . . ? C28 C23 C24 C25 1.0(5) . . . . ? O3 C23 C24 C25 175.4(3) . . . . ? C28 C23 C24 C22 -176.7(3) . . . . ? O3 C23 C24 C22 -2.3(5) . . . . ? C17 C22 C24 C23 -87.2(4) . . . . ? C17 C22 C24 C25 95.2(4) . . . . ? C23 C24 C25 C26 -0.9(5) . . . . ? C22 C24 C25 C26 176.8(3) . . . . ? C24 C25 C26 C27 0.2(5) . . . . ? C24 C25 C26 C29 -177.2(3) . . . . ? C25 C26 C27 C28 0.4(5) . . . . ? C29 C26 C27 C28 177.9(3) . . . . ? C26 C27 C28 C23 -0.3(5) . . . . ? C26 C27 C28 C33 173.1(3) . . . . ? C24 C23 C28 C27 -0.4(5) . . . . ? O3 C23 C28 C27 -174.5(3) . . . . ? C24 C23 C28 C33 -173.7(3) . . . . ? O3 C23 C28 C33 12.2(5) . . . . ? C25 C26 C29 C30 -12.1(5) . . . . ? C27 C26 C29 C30 170.6(4) . . . . ? C25 C26 C29 C32 -132.7(4) . . . . ? C27 C26 C29 C32 50.0(4) . . . . ? C25 C26 C29 C31 109.5(4) . . . . ? C27 C26 C29 C31 -67.9(5) . . . . ? C27 C28 C33 C35 -93.1(3) . . . . ? C23 C28 C33 C35 80.1(4) . . . . ? B2 O4 C34 C39 -137.7(4) . . . . ? B2 O4 C34 C35 47.1(5) . . . . ? C39 C34 C35 C36 1.9(5) . . . . ? O4 C34 C35 C36 176.9(3) . . . . ? C39 C34 C35 C33 174.8(3) . . . . ? O4 C34 C35 C33 -10.2(5) . . . . ? C28 C33 C35 C36 90.5(3) . . . . ? C28 C33 C35 C34 -82.3(4) . . . . ? C34 C35 C36 C37 0.5(5) . . . . ? C33 C35 C36 C37 -172.6(3) . . . . ? C35 C36 C37 C38 -2.4(5) . . . . ? C35 C36 C37 C40 177.9(3) . . . . ? C36 C37 C38 C39 2.0(5) . . . . ? C40 C37 C38 C39 -178.3(3) . . . . ? C35 C34 C39 C38 -2.2(5) . . . . ? O4 C34 C39 C38 -177.4(3) . . . . ? C35 C34 C39 C44 176.1(3) . . . . ? O4 C34 C39 C44 0.9(4) . . . . ? C37 C38 C39 C34 0.2(5) . . . . ? C37 C38 C39 C44 -178.1(3) . . . . ? C36 C37 C40 C41 -49.0(4) . . . . ? C38 C37 C40 C41 131.3(3) . . . . ? C36 C37 C40 C42 -169.3(3) . . . . ? C38 C37 C40 C42 11.0(5) . . . . ? C36 C37 C40 C43 70.3(4) . . . . ? C38 C37 C40 C43 -109.4(4) . . . . ? C34 C39 C44 C2 88.6(4) . . . . ? C38 C39 C44 C2 -93.1(4) . . . . ? C1 C2 C44 C39 4.0(5) . . . . ? C3 C2 C44 C39 -176.9(3) . . . . ? O4 B2 C45 C50 -88.7(4) . . . . ? O3 B2 C45 C50 90.8(4) . . . . ? O4 B2 C45 C46 89.0(4) . . . . ? O3 B2 C45 C46 -91.5(4) . . . . ? C50 C45 C46 C47 1.8(5) . . . . ? B2 C45 C46 C47 -176.0(3) . . . . ? C50 C45 C46 C51 -178.8(3) . . . . ? B2 C45 C46 C51 3.4(5) . . . . ? C45 C46 C47 C48 0.1(6) . . . . ? C51 C46 C47 C48 -179.3(3) . . . . ? C46 C47 C48 C49 -1.7(5) . . . . ? C46 C47 C48 C52 177.4(3) . . . . ? C47 C48 C49 C50 1.2(5) . . . . ? C52 C48 C49 C50 -177.9(3) . . . . ? C48 C49 C50 C45 0.8(5) . . . . ? C48 C49 C50 C53 -178.8(3) . . . . ? C46 C45 C50 C49 -2.3(5) . . . . ? B2 C45 C50 C49 175.6(3) . . . . ? C46 C45 C50 C53 177.3(3) . . . . ? B2 C45 C50 C53 -4.9(5) . . . . ? C47 C46 C51 F4 1.1(5) . . . . ? C45 C46 C51 F4 -178.3(4) . . . . ? C47 C46 C51 F2 -122.4(4) . . . . ? C45 C46 C51 F2 58.2(5) . . . . ? C47 C46 C51 F3 120.1(4) . . . . ? C45 C46 C51 F3 -59.3(5) . . . . ? C49 C48 C52 F7 167.4(3) . . . . ? C47 C48 C52 F7 -11.7(5) . . . . ? C49 C48 C52 F6 -71.9(4) . . . . ? C47 C48 C52 F6 109.0(4) . . . . ? C49 C48 C52 F5 46.7(5) . . . . ? C47 C48 C52 F5 -132.4(4) . . . . ? C49 C50 C53 F8 66.8(4) . . . . ? C45 C50 C53 F8 -112.7(4) . . . . ? C49 C50 C53 F10 -172.8(3) . . . . ? C45 C50 C53 F10 7.6(5) . . . . ? C49 C50 C53 F9 -52.1(4) . . . . ? C45 C50 C53 F9 128.3(4) . . . . ? C60 C55 C56 C57 0.5(15) . . . . ? C54 C55 C56 C57 179.3(9) . . . . ? C55 C56 C57 C58 2.3(14) . . . . ? C56 C57 C58 C59 -2.0(14) . . . . ? C57 C58 C59 C60 -0.9(14) . . . . ? C56 C55 C60 C59 -3.3(15) . . . . ? C54 C55 C60 C59 177.9(9) . . . . ? C58 C59 C60 C55 3.4(14) . . . . ? C60X C55X C56X C57X 0(2) . . . . ? C54X C55X C56X C57X -179.7(11) . . . . ? C55X C56X C57X C58X 0(2) . . . . ? C56X C57X C58X C59X -2(2) . . . . ? C57X C58X C59X C60X 2.9(19) . . . . ? C56X C55X C60X C59X 1(2) . . . . ? C54X C55X C60X C59X -179.2(11) . . . . ? C58X C59X C60X C55X -2.6(19) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.481 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.059 #===END data_4.3MeCN _database_code_depnum_ccdc_archive 'CCDC 278177' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H65 B2 F18 N3 O4' _chemical_formula_weight 1351.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.8326(10) _cell_length_b 15.2792(6) _cell_length_c 19.0184(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.495(2) _cell_angle_gamma 90.00 _cell_volume 6605.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13315 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 28.67 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.73 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.41 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2792 _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.919 _exptl_absorpt_correction_T_max 0.953 _exptl_absorpt_process_details 'SADABS, v. 2.10, Sheldrick, G.M., 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 28545 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.97 _reflns_number_total 7939 _reflns_number_gt 6192 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0764P)^2^+8.0946P] 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 7939 _refine_ls_number_parameters 490 _refine_ls_number_restraints 190 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1379 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.036 _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 B1 B 0.08907(8) 1.03080(11) 0.27371(9) 0.0244(3) Uani 1 1 d . . . O1 O 0.08199(5) 0.99658(7) 0.20557(6) 0.0267(2) Uani 1 1 d . . . O2 O 0.08075(5) 0.98879(7) 0.33251(6) 0.0259(2) Uani 1 1 d . . . C1 C 0.08678(7) 0.91101(10) 0.18249(8) 0.0239(3) Uani 1 1 d . . . C2 C 0.04677(7) 0.88107(10) 0.11709(8) 0.0247(3) Uani 1 1 d . . . C3 C 0.06016(7) 0.80220(11) 0.08808(9) 0.0296(3) Uani 1 1 d . . . H3 H 0.0345 0.7825 0.0423 0.035 Uiso 1 1 calc R . . C4 C 0.10910(8) 0.75113(11) 0.12287(9) 0.0311(4) Uani 1 1 d . A . C5 C 0.14552(7) 0.78100(12) 0.19071(9) 0.0305(3) Uani 1 1 d . . . H5 H 0.1780 0.7462 0.2172 0.037 Uiso 1 1 calc R . . C6 C 0.13534(7) 0.86046(11) 0.22051(9) 0.0265(3) Uani 1 1 d . . . C7 C 0.12108(9) 0.66435(13) 0.08943(11) 0.0382(4) Uani 1 1 d DU . . C8 C 0.0851(2) 0.6570(3) 0.0082(2) 0.0527(13) Uani 0.517(4) 1 d PDU A 1 H8A H 0.0957 0.7049 -0.0196 0.079 Uiso 0.517(4) 1 calc PR A 1 H8B H 0.0431 0.6606 0.0037 0.079 Uiso 0.517(4) 1 calc PR A 1 H8C H 0.0934 0.6008 -0.0114 0.079 Uiso 0.517(4) 1 calc PR A 1 C9 C 0.1074(3) 0.5935(3) 0.1350(3) 0.0649(16) Uani 0.517(4) 1 d PDU A 1 H9A H 0.1315 0.6007 0.1864 0.097 Uiso 0.517(4) 1 calc PR A 1 H9B H 0.1159 0.5366 0.1167 0.097 Uiso 0.517(4) 1 calc PR A 1 H9C H 0.0657 0.5962 0.1321 0.097 Uiso 0.517(4) 1 calc PR A 1 C10 C 0.1864(2) 0.6633(3) 0.0927(3) 0.0574(13) Uani 0.517(4) 1 d PDU A 1 H10A H 0.1938 0.7100 0.0612 0.086 Uiso 0.517(4) 1 calc PR A 1 H10B H 0.1961 0.6066 0.0752 0.086 Uiso 0.517(4) 1 calc PR A 1 H10C H 0.2110 0.6726 0.1436 0.086 Uiso 0.517(4) 1 calc PR A 1 C8X C 0.0668(2) 0.6016(3) 0.0762(5) 0.071(2) Uani 0.483(4) 1 d PDU A 2 H8X1 H 0.0594 0.5898 0.1232 0.106 Uiso 0.483(4) 1 calc PR A 2 H8X2 H 0.0750 0.5465 0.0548 0.106 Uiso 0.483(4) 1 calc PR A 2 H8X3 H 0.0321 0.6294 0.0422 0.106 Uiso 0.483(4) 1 calc PR A 2 C9X C 0.1749(2) 0.6132(3) 0.1382(3) 0.0500(12) Uani 0.483(4) 1 d PDU A 2 H9X1 H 0.1692 0.6008 0.1862 0.075 Uiso 0.483(4) 1 calc PR A 2 H9X2 H 0.2106 0.6483 0.1454 0.075 Uiso 0.483(4) 1 calc PR A 2 H9X3 H 0.1790 0.5579 0.1140 0.075 Uiso 0.483(4) 1 calc PR A 2 C10X C 0.1322(3) 0.6818(3) 0.0161(3) 0.0533(13) Uani 0.483(4) 1 d PDU A 2 H10D H 0.1398 0.6263 -0.0053 0.080 Uiso 0.483(4) 1 calc PR A 2 H10E H 0.1664 0.7203 0.0238 0.080 Uiso 0.483(4) 1 calc PR A 2 H10F H 0.0976 0.7100 -0.0177 0.080 Uiso 0.483(4) 1 calc PR A 2 C11 C 0.17265(7) 0.88686(11) 0.29691(9) 0.0276(3) Uani 1 1 d . . . H11A H 0.1785 0.9511 0.2993 0.033 Uiso 1 1 calc R . . H11B H 0.2117 0.8584 0.3087 0.033 Uiso 1 1 calc R . . C12 C 0.09443(7) 0.90614(10) 0.36266(8) 0.0230(3) Uani 1 1 d . . . C13 C 0.14134(7) 0.85853(10) 0.35182(8) 0.0253(3) Uani 1 1 d . . . C14 C 0.15669(7) 0.77939(11) 0.38911(9) 0.0280(3) Uani 1 1 d . . . H14 H 0.1877 0.7458 0.3810 0.034 Uiso 1 1 calc R . . C15 C 0.12800(7) 0.74789(10) 0.43788(9) 0.0278(3) Uani 1 1 d . . . C16 C 0.08192(7) 0.79796(10) 0.44715(8) 0.0262(3) Uani 1 1 d . . . H16 H 0.0620 0.7777 0.4805 0.031 Uiso 1 1 calc R . . C17 C 0.06351(7) 0.87668(10) 0.40974(8) 0.0228(3) Uani 1 1 d . . . C18 C 0.14479(9) 0.66043(12) 0.47908(11) 0.0375(4) Uani 1 1 d . . . C19 C 0.1547(2) 0.6743(2) 0.56086(16) 0.1136(17) Uani 1 1 d . . . H19A H 0.1172 0.6882 0.5695 0.170 Uiso 1 1 calc R . . H19B H 0.1823 0.7228 0.5782 0.170 Uiso 1 1 calc R . . H19C H 0.1710 0.6208 0.5877 0.170 Uiso 1 1 calc R . . C20 C 0.09653(16) 0.59574(19) 0.4470(3) 0.1221(19) Uani 1 1 d . . . H20A H 0.1075 0.5387 0.4707 0.183 Uiso 1 1 calc R . . H20B H 0.0904 0.5902 0.3939 0.183 Uiso 1 1 calc R . . H20C H 0.0601 0.6160 0.4556 0.183 Uiso 1 1 calc R . . C21 C 0.20184(12) 0.62235(16) 0.47046(16) 0.0624(7) Uani 1 1 d . . . H21A H 0.2115 0.5679 0.4988 0.094 Uiso 1 1 calc R . . H21B H 0.2339 0.6646 0.4888 0.094 Uiso 1 1 calc R . . H21C H 0.1966 0.6102 0.4183 0.094 Uiso 1 1 calc R . . C22 C 0.01132(7) 0.92692(10) 0.42064(8) 0.0243(3) Uani 1 1 d . . . H22A H 0.0162 0.9323 0.4740 0.029 Uiso 1 1 calc R . . H22B H 0.0105 0.9867 0.4002 0.029 Uiso 1 1 calc R . . C23 C 0.10692(7) 1.13267(10) 0.28486(9) 0.0266(3) Uani 1 1 d . . . C24 C 0.14669(8) 1.16452(11) 0.35148(9) 0.0323(4) Uani 1 1 d . . . C25 C 0.16811(9) 1.25012(12) 0.35828(10) 0.0374(4) Uani 1 1 d . . . H25 H 0.1951 1.2690 0.4034 0.045 Uiso 1 1 calc R . . C26 C 0.15030(9) 1.30729(12) 0.29974(10) 0.0367(4) Uani 1 1 d . B . C27 C 0.10924(8) 1.28103(11) 0.23497(10) 0.0327(4) Uani 1 1 d . . . H27 H 0.0955 1.3212 0.1954 0.039 Uiso 1 1 calc R . . C28 C 0.08815(7) 1.19569(11) 0.22806(9) 0.0277(3) Uani 1 1 d . . . C29 C 0.16775(9) 1.11004(12) 0.42138(10) 0.0395(4) Uani 1 1 d . . . F1 F 0.19199(5) 1.03374(7) 0.41143(6) 0.0424(3) Uani 1 1 d . . . F2 F 0.12446(6) 1.09259(8) 0.45096(6) 0.0478(3) Uani 1 1 d . . . F3 F 0.20967(7) 1.15167(8) 0.47461(6) 0.0586(4) Uani 1 1 d . . . C30 C 0.17569(11) 1.39844(14) 0.30616(12) 0.0502(5) Uani 1 1 d DU . . F4 F 0.1831(4) 1.4328(4) 0.3694(3) 0.102(2) Uani 0.594(13) 1 d PDU B 1 F5 F 0.1446(4) 1.4517(4) 0.2589(5) 0.146(4) Uani 0.594(13) 1 d PDU B 1 F6 F 0.2290(3) 1.3961(5) 0.2996(7) 0.117(3) Uani 0.594(13) 1 d PDU B 1 F4X F 0.2060(6) 1.4175(6) 0.3723(4) 0.134(5) Uani 0.406(13) 1 d PDU B 2 F5X F 0.1339(4) 1.4576(6) 0.2893(8) 0.108(4) Uani 0.406(13) 1 d PDU B 2 F6X F 0.2041(7) 1.4149(6) 0.2611(7) 0.104(4) Uani 0.406(13) 1 d PDU B 2 C31 C 0.04211(8) 1.17511(11) 0.15604(9) 0.0319(4) Uani 1 1 d . . . F7 F 0.06372(5) 1.13485(8) 0.10702(6) 0.0422(3) Uani 1 1 d . . . F8 F -0.00124(4) 1.12500(7) 0.16505(6) 0.0347(2) Uani 1 1 d . . . F9 F 0.01618(6) 1.24828(8) 0.12205(7) 0.0531(3) Uani 1 1 d . . . N1 N 0.0000 0.5478(4) 0.2500 0.146(2) Uani 1 2 d S . . C32 C 0.0000 0.6247(4) 0.2500 0.0850(13) Uani 1 2 d S . . C33 C 0.0000 0.7196(3) 0.2500 0.0601(9) Uani 1 2 d S . . N2 N 0.22388(13) 0.8551(2) 0.69434(18) 0.1032(11) Uani 1 1 d . . . C34 C 0.20286(11) 0.9021(2) 0.64810(15) 0.0610(6) Uani 1 1 d . . . C35 C 0.17575(10) 0.96117(16) 0.58760(13) 0.0505(5) Uani 1 1 d . . . H35A H 0.2062 0.9972 0.5769 0.076 Uiso 1 1 calc R . . H35B H 0.1475 0.9990 0.6013 0.076 Uiso 1 1 calc R . . H35C H 0.1552 0.9271 0.5438 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0258(8) 0.0223(8) 0.0235(8) 0.0014(6) 0.0049(6) -0.0010(6) O1 0.0337(6) 0.0223(5) 0.0222(5) -0.0002(4) 0.0053(4) -0.0011(4) O2 0.0314(6) 0.0209(5) 0.0255(5) 0.0038(4) 0.0088(4) 0.0028(4) C1 0.0288(7) 0.0227(7) 0.0220(7) 0.0000(5) 0.0101(6) -0.0025(6) C2 0.0278(7) 0.0250(7) 0.0226(7) 0.0000(6) 0.0096(6) -0.0018(6) C3 0.0323(8) 0.0306(8) 0.0267(8) -0.0053(6) 0.0103(6) -0.0012(7) C4 0.0344(8) 0.0304(8) 0.0322(8) -0.0037(7) 0.0155(7) 0.0020(7) C5 0.0305(8) 0.0338(9) 0.0292(8) 0.0018(7) 0.0118(7) 0.0046(7) C6 0.0262(7) 0.0308(8) 0.0238(7) 0.0012(6) 0.0091(6) -0.0009(6) C7 0.0430(10) 0.0335(9) 0.0394(10) -0.0058(7) 0.0143(8) 0.0077(8) C8 0.066(3) 0.043(2) 0.043(2) -0.0157(17) 0.007(2) 0.020(2) C9 0.113(5) 0.029(2) 0.062(3) 0.0004(19) 0.041(3) 0.009(2) C10 0.056(2) 0.065(3) 0.053(3) -0.014(2) 0.019(2) 0.024(2) C8X 0.057(3) 0.036(2) 0.132(6) -0.037(3) 0.047(4) -0.013(2) C9X 0.061(3) 0.036(2) 0.052(3) -0.0042(19) 0.017(2) 0.017(2) C10X 0.068(3) 0.053(3) 0.044(2) -0.006(2) 0.025(2) 0.020(2) C11 0.0248(7) 0.0319(8) 0.0252(7) 0.0012(6) 0.0061(6) 0.0009(6) C12 0.0265(7) 0.0197(7) 0.0195(7) 0.0011(5) 0.0021(6) -0.0003(5) C13 0.0258(7) 0.0268(8) 0.0215(7) -0.0001(6) 0.0042(6) -0.0003(6) C14 0.0295(8) 0.0270(8) 0.0258(7) -0.0002(6) 0.0056(6) 0.0052(6) C15 0.0338(8) 0.0218(7) 0.0245(7) 0.0022(6) 0.0039(6) 0.0024(6) C16 0.0315(8) 0.0240(7) 0.0220(7) 0.0019(6) 0.0065(6) -0.0006(6) C17 0.0263(7) 0.0216(7) 0.0185(7) -0.0018(5) 0.0037(5) -0.0002(6) C18 0.0457(10) 0.0270(9) 0.0389(10) 0.0108(7) 0.0115(8) 0.0095(7) C19 0.206(4) 0.096(2) 0.0565(16) 0.0494(17) 0.066(2) 0.102(3) C20 0.083(2) 0.0393(15) 0.200(5) 0.052(2) -0.023(2) -0.0166(14) C21 0.0686(16) 0.0434(12) 0.0766(17) 0.0207(12) 0.0242(13) 0.0237(11) C22 0.0293(7) 0.0232(7) 0.0200(7) 0.0006(5) 0.0066(6) 0.0021(6) C23 0.0317(8) 0.0241(7) 0.0236(7) 0.0009(6) 0.0080(6) -0.0017(6) C24 0.0375(9) 0.0283(8) 0.0268(8) 0.0000(6) 0.0032(7) -0.0026(7) C25 0.0434(10) 0.0296(9) 0.0323(9) -0.0038(7) 0.0009(7) -0.0066(7) C26 0.0433(10) 0.0265(8) 0.0370(9) -0.0019(7) 0.0070(8) -0.0078(7) C27 0.0411(9) 0.0256(8) 0.0301(8) 0.0025(6) 0.0086(7) -0.0041(7) C28 0.0325(8) 0.0257(8) 0.0240(7) 0.0009(6) 0.0072(6) -0.0030(6) C29 0.0516(11) 0.0315(9) 0.0262(8) -0.0006(7) -0.0020(8) -0.0045(8) F1 0.0452(6) 0.0323(6) 0.0383(6) 0.0039(4) -0.0046(5) 0.0004(5) F2 0.0708(8) 0.0441(7) 0.0269(5) 0.0039(5) 0.0124(5) -0.0008(6) F3 0.0775(9) 0.0424(7) 0.0334(6) -0.0001(5) -0.0172(6) -0.0125(6) C30 0.0615(13) 0.0327(10) 0.0479(12) -0.0010(9) 0.0038(10) -0.0145(9) F4 0.183(6) 0.048(2) 0.099(4) -0.046(3) 0.081(4) -0.051(3) F5 0.171(6) 0.043(3) 0.141(5) 0.044(3) -0.079(5) -0.055(3) F6 0.103(4) 0.056(3) 0.229(9) -0.046(4) 0.105(5) -0.046(3) F4X 0.195(9) 0.063(5) 0.071(4) 0.027(3) -0.072(5) -0.082(5) F5X 0.086(4) 0.029(3) 0.199(11) -0.008(5) 0.025(5) 0.011(2) F6X 0.161(10) 0.046(4) 0.148(7) -0.010(4) 0.111(7) -0.041(5) C31 0.0395(9) 0.0257(8) 0.0272(8) 0.0046(6) 0.0049(7) -0.0039(7) F7 0.0536(7) 0.0493(7) 0.0239(5) -0.0035(4) 0.0119(5) -0.0128(5) F8 0.0312(5) 0.0333(5) 0.0364(5) -0.0003(4) 0.0054(4) -0.0046(4) F9 0.0626(8) 0.0312(6) 0.0461(7) 0.0112(5) -0.0133(6) -0.0028(5) N1 0.204(7) 0.092(4) 0.133(5) 0.000 0.036(5) 0.000 C32 0.105(4) 0.090(4) 0.058(2) 0.000 0.021(2) 0.000 C33 0.064(2) 0.067(2) 0.0456(17) 0.000 0.0115(16) 0.000 N2 0.0687(16) 0.136(3) 0.096(2) 0.057(2) 0.0099(15) 0.0008(17) C34 0.0431(12) 0.0792(18) 0.0569(14) 0.0131(13) 0.0093(10) -0.0063(12) C35 0.0437(11) 0.0575(13) 0.0474(12) 0.0017(10) 0.0096(9) -0.0029(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O2 1.355(2) . ? B1 O1 1.360(2) . ? B1 C23 1.611(2) . ? O1 C1 1.3949(19) . ? O2 C12 1.3848(18) . ? C1 C2 1.397(2) . ? C1 C6 1.398(2) . ? C2 C3 1.402(2) . ? C2 C22 1.525(2) 2 ? C3 C4 1.394(2) . ? C4 C5 1.398(2) . ? C4 C7 1.534(2) . ? C5 C6 1.392(2) . ? C6 C11 1.513(2) . ? C7 C9 1.484(5) . ? C7 C10X 1.520(5) . ? C7 C8 1.528(4) . ? C7 C10 1.541(5) . ? C7 C9X 1.550(5) . ? C7 C8X 1.568(5) . ? C11 C13 1.518(2) . ? C12 C17 1.394(2) . ? C12 C13 1.400(2) . ? C13 C14 1.394(2) . ? C14 C15 1.393(2) . ? C15 C16 1.392(2) . ? C15 C18 1.540(2) . ? C16 C17 1.399(2) . ? C17 C22 1.528(2) . ? C18 C20 1.500(4) . ? C18 C19 1.516(3) . ? C18 C21 1.532(3) . ? C22 C2 1.525(2) 2 ? C23 C28 1.416(2) . ? C23 C24 1.421(2) . ? C24 C25 1.396(2) . ? C24 C29 1.520(2) . ? C25 C26 1.378(3) . ? C26 C27 1.382(3) . ? C26 C30 1.509(3) . ? C27 C28 1.389(2) . ? C28 C31 1.508(2) . ? C29 F1 1.339(2) . ? C29 F2 1.342(3) . ? C29 F3 1.349(2) . ? C30 F6X 1.266(7) . ? C30 F5 1.272(6) . ? C30 F4 1.275(5) . ? C30 F4X 1.281(6) . ? C30 F5X 1.312(7) . ? C30 F6 1.313(6) . ? C31 F8 1.338(2) . ? C31 F7 1.342(2) . ? C31 F9 1.345(2) . ? N1 C32 1.175(7) . ? C32 C33 1.450(7) . ? N2 C34 1.129(4) . ? C34 C35 1.452(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 O2 B1 O1 126.68(15) . . ? O2 B1 C23 116.58(14) . . ? O1 B1 C23 116.69(14) . . ? B1 O1 C1 131.43(13) . . ? B1 O2 C12 134.37(13) . . ? O1 C1 C2 119.23(14) . . ? O1 C1 C6 119.24(14) . . ? C2 C1 C6 121.11(14) . . ? C1 C2 C3 117.17(15) . . ? C1 C2 C22 123.28(14) . 2 ? C3 C2 C22 119.45(14) . 2 ? C4 C3 C2 123.47(15) . . ? C3 C4 C5 117.02(15) . . ? C3 C4 C7 121.36(16) . . ? C5 C4 C7 121.58(16) . . ? C6 C5 C4 121.66(16) . . ? C5 C6 C1 119.33(15) . . ? C5 C6 C11 119.98(15) . . ? C1 C6 C11 120.37(14) . . ? C9 C7 C8 112.4(3) . . ? C9 C7 C4 106.7(2) . . ? C10X C7 C4 109.5(2) . . ? C8 C7 C4 111.4(2) . . ? C9 C7 C10 111.5(4) . . ? C8 C7 C10 107.1(3) . . ? C4 C7 C10 107.7(2) . . ? C10X C7 C9X 107.3(3) . . ? C4 C7 C9X 114.3(2) . . ? C10X C7 C8X 108.8(4) . . ? C4 C7 C8X 110.3(2) . . ? C9X C7 C8X 106.4(3) . . ? C6 C11 C13 108.44(13) . . ? O2 C12 C17 117.14(13) . . ? O2 C12 C13 120.79(14) . . ? C17 C12 C13 121.77(14) . . ? C14 C13 C12 118.35(14) . . ? C14 C13 C11 119.30(14) . . ? C12 C13 C11 122.19(14) . . ? C15 C14 C13 122.15(15) . . ? C16 C15 C14 117.27(14) . . ? C16 C15 C18 120.43(15) . . ? C14 C15 C18 122.28(15) . . ? C15 C16 C17 123.13(15) . . ? C12 C17 C16 117.29(14) . . ? C12 C17 C22 122.28(13) . . ? C16 C17 C22 120.43(14) . . ? C20 C18 C19 111.9(3) . . ? C20 C18 C21 107.6(3) . . ? C19 C18 C21 107.0(2) . . ? C20 C18 C15 108.36(18) . . ? C19 C18 C15 109.72(18) . . ? C21 C18 C15 112.22(17) . . ? C2 C22 C17 111.49(12) 2 . ? C28 C23 C24 114.87(14) . . ? C28 C23 B1 123.13(14) . . ? C24 C23 B1 121.83(14) . . ? C25 C24 C23 122.07(16) . . ? C25 C24 C29 114.62(15) . . ? C23 C24 C29 123.28(15) . . ? C26 C25 C24 120.26(16) . . ? C25 C26 C27 119.97(16) . . ? C25 C26 C30 120.08(17) . . ? C27 C26 C30 119.95(17) . . ? C26 C27 C28 119.71(16) . . ? C27 C28 C23 122.95(15) . . ? C27 C28 C31 115.16(14) . . ? C23 C28 C31 121.86(14) . . ? F1 C29 F2 107.74(15) . . ? F1 C29 F3 105.24(16) . . ? F2 C29 F3 105.56(16) . . ? F1 C29 C24 113.34(16) . . ? F2 C29 C24 112.46(16) . . ? F3 C29 C24 111.94(15) . . ? F5 C30 F4 106.8(5) . . ? F6X C30 F4X 111.1(7) . . ? F6X C30 F5X 102.6(7) . . ? F4X C30 F5X 104.3(7) . . ? F5 C30 F6 109.0(5) . . ? F4 C30 F6 103.7(5) . . ? F6X C30 C26 114.3(5) . . ? F5 C30 C26 113.5(3) . . ? F4 C30 C26 113.2(3) . . ? F4X C30 C26 112.5(4) . . ? F5X C30 C26 111.1(5) . . ? F6 C30 C26 110.1(3) . . ? F8 C31 F7 107.40(14) . . ? F8 C31 F9 106.04(15) . . ? F7 C31 F9 105.30(14) . . ? F8 C31 C28 112.45(14) . . ? F7 C31 C28 113.58(15) . . ? F9 C31 C28 111.52(14) . . ? N1 C32 C33 180.000(2) . . ? N2 C34 C35 178.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 B1 O1 C1 -27.5(3) . . . . ? C23 B1 O1 C1 154.92(15) . . . . ? O1 B1 O2 C12 41.8(3) . . . . ? C23 B1 O2 C12 -140.58(16) . . . . ? B1 O1 C1 C2 140.78(17) . . . . ? B1 O1 C1 C6 -46.5(2) . . . . ? O1 C1 C2 C3 167.12(14) . . . . ? C6 C1 C2 C3 -5.4(2) . . . . ? O1 C1 C2 C22 -16.6(2) . . . 2 ? C6 C1 C2 C22 170.89(14) . . . 2 ? C1 C2 C3 C4 3.3(2) . . . . ? C22 C2 C3 C4 -173.14(15) 2 . . . ? C2 C3 C4 C5 1.0(3) . . . . ? C2 C3 C4 C7 178.80(16) . . . . ? C3 C4 C5 C6 -3.4(2) . . . . ? C7 C4 C5 C6 178.82(16) . . . . ? C4 C5 C6 C1 1.4(2) . . . . ? C4 C5 C6 C11 174.85(15) . . . . ? O1 C1 C6 C5 -169.30(14) . . . . ? C2 C1 C6 C5 3.2(2) . . . . ? O1 C1 C6 C11 17.2(2) . . . . ? C2 C1 C6 C11 -170.23(14) . . . . ? C3 C4 C7 C9 -106.8(3) . . . . ? C5 C4 C7 C9 70.9(4) . . . . ? C3 C4 C7 C10X 63.7(3) . . . . ? C5 C4 C7 C10X -118.6(3) . . . . ? C3 C4 C7 C8 16.2(3) . . . . ? C5 C4 C7 C8 -166.1(3) . . . . ? C3 C4 C7 C10 133.3(3) . . . . ? C5 C4 C7 C10 -49.0(3) . . . . ? C3 C4 C7 C9X -175.9(3) . . . . ? C5 C4 C7 C9X 1.8(3) . . . . ? C3 C4 C7 C8X -56.0(4) . . . . ? C5 C4 C7 C8X 121.7(4) . . . . ? C5 C6 C11 C13 -93.86(17) . . . . ? C1 C6 C11 C13 79.56(18) . . . . ? B1 O2 C12 C17 -160.81(16) . . . . ? B1 O2 C12 C13 25.4(2) . . . . ? O2 C12 C13 C14 173.99(14) . . . . ? C17 C12 C13 C14 0.5(2) . . . . ? O2 C12 C13 C11 -10.7(2) . . . . ? C17 C12 C13 C11 175.82(14) . . . . ? C6 C11 C13 C14 96.33(17) . . . . ? C6 C11 C13 C12 -78.99(19) . . . . ? C12 C13 C14 C15 -1.8(2) . . . . ? C11 C13 C14 C15 -177.27(15) . . . . ? C13 C14 C15 C16 1.3(2) . . . . ? C13 C14 C15 C18 179.92(16) . . . . ? C14 C15 C16 C17 0.5(2) . . . . ? C18 C15 C16 C17 -178.15(15) . . . . ? O2 C12 C17 C16 -172.55(13) . . . . ? C13 C12 C17 C16 1.2(2) . . . . ? O2 C12 C17 C22 7.7(2) . . . . ? C13 C12 C17 C22 -178.52(14) . . . . ? C15 C16 C17 C12 -1.7(2) . . . . ? C15 C16 C17 C22 178.03(14) . . . . ? C16 C15 C18 C20 69.7(3) . . . . ? C14 C15 C18 C20 -108.8(3) . . . . ? C16 C15 C18 C19 -52.7(3) . . . . ? C14 C15 C18 C19 128.8(3) . . . . ? C16 C15 C18 C21 -171.56(19) . . . . ? C14 C15 C18 C21 9.9(3) . . . . ? C12 C17 C22 C2 107.07(16) . . . 2 ? C16 C17 C22 C2 -72.63(18) . . . 2 ? O2 B1 C23 C28 -145.42(16) . . . . ? O1 B1 C23 C28 32.5(2) . . . . ? O2 B1 C23 C24 39.5(2) . . . . ? O1 B1 C23 C24 -142.60(16) . . . . ? C28 C23 C24 C25 -3.7(3) . . . . ? B1 C23 C24 C25 171.70(17) . . . . ? C28 C23 C24 C29 174.20(17) . . . . ? B1 C23 C24 C29 -10.4(3) . . . . ? C23 C24 C25 C26 0.8(3) . . . . ? C29 C24 C25 C26 -177.25(19) . . . . ? C24 C25 C26 C27 2.7(3) . . . . ? C24 C25 C26 C30 -177.2(2) . . . . ? C25 C26 C27 C28 -3.0(3) . . . . ? C30 C26 C27 C28 176.86(19) . . . . ? C26 C27 C28 C23 -0.2(3) . . . . ? C26 C27 C28 C31 178.12(17) . . . . ? C24 C23 C28 C27 3.4(2) . . . . ? B1 C23 C28 C27 -171.94(16) . . . . ? C24 C23 C28 C31 -174.77(16) . . . . ? B1 C23 C28 C31 9.9(2) . . . . ? C25 C24 C29 F1 -127.00(18) . . . . ? C23 C24 C29 F1 54.9(3) . . . . ? C25 C24 C29 F2 110.49(19) . . . . ? C23 C24 C29 F2 -67.6(2) . . . . ? C25 C24 C29 F3 -8.2(3) . . . . ? C23 C24 C29 F3 173.77(17) . . . . ? C25 C26 C30 F6X 117.9(9) . . . . ? C27 C26 C30 F6X -62.0(9) . . . . ? C25 C26 C30 F5 -160.6(8) . . . . ? C27 C26 C30 F5 19.5(8) . . . . ? C25 C26 C30 F4 -38.7(5) . . . . ? C27 C26 C30 F4 141.5(5) . . . . ? C25 C26 C30 F4X -10.1(9) . . . . ? C27 C26 C30 F4X 170.1(9) . . . . ? C25 C26 C30 F5X -126.6(7) . . . . ? C27 C26 C30 F5X 53.6(8) . . . . ? C25 C26 C30 F6 76.9(7) . . . . ? C27 C26 C30 F6 -102.9(7) . . . . ? C27 C28 C31 F8 -139.29(16) . . . . ? C23 C28 C31 F8 39.0(2) . . . . ? C27 C28 C31 F7 98.47(18) . . . . ? C23 C28 C31 F7 -83.20(19) . . . . ? C27 C28 C31 F9 -20.3(2) . . . . ? C23 C28 C31 F9 158.00(16) . . . . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.748 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.054 #===END