# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name V.L.Pecoraro J.W.Kampf G.Mezei _publ_contact_author_name 'Vincent L. Pecoraro' _publ_contact_author_address ; Chemistry The University of Michigan 930 N. University Ann Arbor Michigan 48109 UNITED STATES OF AMERICA ; _publ_contact_author_email VLPEC@UMICH.EDU _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Temperature-, molar ratio- and counterion-effect on the crystal growth of bipyridinium-bis-alkylcarboxylic acid/crown ether pseudorotaxanes ; data_Pseudorotaxane_IIa(gm07) _database_code_depnum_ccdc_archive 'CCDC 633578' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C36 H44 O10, 2(C20 H26 N2 O4), 2(P F6), 2(H2 O4 P), C2 H3 N, H2 O ; _chemical_formula_sum 'C78 H105 F12 N5 O27 P4' _chemical_formula_weight 1896.55 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' 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' P P 0.1023 0.0942 '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 13.6418(16) _cell_length_b 16.700(2) _cell_length_c 20.050(2) _cell_angle_alpha 85.446(8) _cell_angle_beta 83.877(7) _cell_angle_gamma 70.685(7) _cell_volume 4281.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5912 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 21.04 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 0.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9693 _exptl_absorpt_correction_T_max 0.9807 _exptl_absorpt_process_details ? _exptl_special_details ; 4095 frames x 45 sec. @ 4.969 cm; 0.5 deg. steps in omega & phi ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86695 _diffrn_reflns_av_R_equivalents 0.0872 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 22.70 _reflns_number_total 11395 _reflns_number_gt 7850 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART-1K' _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' _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^)+(0.0817P)^2^+10.6380P] 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 11395 _refine_ls_number_parameters 1152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1011 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1777 _refine_ls_wR_factor_gt 0.1530 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.011 _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 P1 P 0.28656(8) 0.53519(7) 0.00111(6) 0.0402(3) Uani 1 1 d . . . P2 P 0.24764(10) 0.95823(7) 0.43746(6) 0.0493(3) Uani 1 1 d . . . P3 P 0.12868(9) 0.92050(7) 0.06328(6) 0.0434(3) Uani 1 1 d . . . P4 P 0.85205(8) 0.54516(7) 0.42312(5) 0.0374(3) Uani 1 1 d . . . O1 O 0.71108(18) 0.37699(15) 0.27362(12) 0.0323(7) Uani 1 1 d . . . O2 O 0.5773(2) 0.56283(19) 0.26672(15) 0.0552(9) Uani 1 1 d . . . O3 O 0.3897(2) 0.5698(2) 0.21472(19) 0.0798(12) Uani 1 1 d . . . O4 O 0.2154(3) 0.6084(2) 0.31766(15) 0.0615(9) Uani 1 1 d . . . O5 O 0.1726(2) 0.45048(16) 0.31096(13) 0.0370(7) Uani 1 1 d . . . O6 O 0.27053(19) 0.10604(15) 0.20801(13) 0.0358(7) Uani 1 1 d . . . O7 O 0.38855(19) -0.06884(16) 0.21036(13) 0.0376(7) Uani 1 1 d . . . O8 O 0.5727(2) -0.20435(16) 0.22122(13) 0.0413(7) Uani 1 1 d . . . O9 O 0.7169(2) -0.12090(16) 0.24986(15) 0.0475(8) Uani 1 1 d . . . O10 O 0.7966(2) 0.01174(16) 0.22279(13) 0.0391(7) Uani 1 1 d . . . O11 O 1.0588(3) 0.8394(2) -0.76292(18) 0.0866(13) Uani 1 1 d . . . O12 O 1.0338(2) 0.97373(17) -0.75052(15) 0.0527(9) Uani 1 1 d . . . H12B H 1.0526 0.9721 -0.7918 0.079 Uiso 1 1 calc R . . O13 O 0.9309(2) 0.64689(18) 0.23320(14) 0.0515(8) Uani 1 1 d . . . O14 O 0.9339(2) 0.51279(17) 0.23452(14) 0.0459(8) Uani 1 1 d . . . H14 H 0.931(4) 0.522(4) 0.286(3) 0.11(2) Uiso 1 1 d . . . O15 O 0.2288(3) 0.1388(2) -0.01256(18) 0.0710(11) Uani 1 1 d . . . O16 O 0.3530(3) 0.01095(18) -0.02343(15) 0.0597(9) Uani 1 1 d . . . H16B H 0.3034 -0.0071 -0.0097 0.090 Uiso 1 1 calc R . . O17 O 0.5869(2) 0.48357(16) 0.56088(14) 0.0449(8) Uani 1 1 d . . . O18 O 0.7259(2) 0.37979(18) 0.52150(14) 0.0428(8) Uani 1 1 d . . . H18 H 0.743(3) 0.419(2) 0.5071(17) 0.023(10) Uiso 1 1 d . . . O19 O 0.91872(18) 0.58300(15) 0.45945(12) 0.0318(6) Uani 1 1 d . . . H19C H 0.9672 0.5436 0.4760 0.048 Uiso 1 1 calc R . . O20 O 0.9134(2) 0.49990(16) 0.36567(13) 0.0396(7) Uani 1 1 d . . . O21 O 0.7748(2) 0.62942(17) 0.39971(15) 0.0517(9) Uani 1 1 d . . . H21C H 0.7308 0.6200 0.3779 0.078 Uiso 1 1 calc R . . O22 O 0.7971(2) 0.5041(2) 0.47321(15) 0.0669(9) Uani 1 1 d . . . O23 O 0.0485(2) 0.90207(18) 0.02387(15) 0.0537(8) Uani 1 1 d . . . H23C H 0.0115 0.9475 0.0057 0.081 Uiso 1 1 calc R . . O24 O 0.2094(2) 0.93649(18) 0.01529(14) 0.0532(8) Uani 1 1 d . . . O25 O 0.0735(2) 0.98333(18) 0.11307(15) 0.0554(9) Uani 1 1 d . . . O26 O 0.1749(3) 0.83482(18) 0.09775(19) 0.0728(11) Uani 1 1 d . . . H26C H 0.1446 0.8339 0.1364 0.109 Uiso 1 1 calc R . . C1 C 0.6869(3) 0.4373(2) 0.3251(2) 0.0355(10) Uani 1 1 d . . . H1A H 0.7441 0.4219 0.3551 0.043 Uiso 1 1 calc R . . H1B H 0.6220 0.4372 0.3523 0.043 Uiso 1 1 calc R . . C2 C 0.6734(3) 0.5232(2) 0.2926(2) 0.0447(12) Uani 1 1 d . . . H2A H 0.6828 0.5601 0.3260 0.054 Uiso 1 1 calc R . . H2B H 0.7291 0.5182 0.2557 0.054 Uiso 1 1 calc R . . C3 C 0.5712(3) 0.5440(3) 0.2012(2) 0.0510(12) Uani 1 1 d . . . H3A H 0.5807 0.4828 0.1992 0.061 Uiso 1 1 calc R . . H3B H 0.6270 0.5569 0.1711 0.061 Uiso 1 1 calc R . . C4 C 0.4679(4) 0.5955(3) 0.1791(2) 0.0552(14) Uani 1 1 d . . . H4A H 0.4553 0.6562 0.1863 0.066 Uiso 1 1 calc R . . H4B H 0.4669 0.5892 0.1306 0.066 Uiso 1 1 calc R . . C5 C 0.2876(4) 0.6361(4) 0.2105(3) 0.099(2) Uani 1 1 d . . . H5A H 0.2907 0.6890 0.2279 0.118 Uiso 1 1 calc R . . H5B H 0.2731 0.6479 0.1627 0.118 Uiso 1 1 calc R . . C6 C 0.2050(4) 0.6141(4) 0.2466(3) 0.0775(18) Uani 1 1 d . . . H6A H 0.2049 0.5588 0.2321 0.093 Uiso 1 1 calc R . . H6B H 0.1378 0.6574 0.2367 0.093 Uiso 1 1 calc R . . C7 C 0.1306(3) 0.5883(3) 0.3528(2) 0.0484(12) Uani 1 1 d . . . H7A H 0.0711 0.6058 0.3246 0.058 Uiso 1 1 calc R . . H7B H 0.1087 0.6204 0.3942 0.058 Uiso 1 1 calc R . . C8 C 0.1579(3) 0.4959(2) 0.3708(2) 0.0376(11) Uani 1 1 d . . . H8A H 0.2227 0.4763 0.3942 0.045 Uiso 1 1 calc R . . H8B H 0.1013 0.4851 0.4015 0.045 Uiso 1 1 calc R . . C9 C 0.1937(3) 0.3650(2) 0.31838(19) 0.0305(10) Uani 1 1 d . . . C10 C 0.1981(3) 0.3203(2) 0.37932(19) 0.0341(10) Uani 1 1 d . . . H10A H 0.1848 0.3492 0.4199 0.041 Uiso 1 1 calc R . . C11 C 0.2226(3) 0.2313(2) 0.3812(2) 0.0349(10) Uani 1 1 d . . . H11A H 0.2263 0.2007 0.4234 0.042 Uiso 1 1 calc R . . C12 C 0.2409(3) 0.1883(2) 0.32409(18) 0.0304(10) Uani 1 1 d . . . H12A H 0.2570 0.1284 0.3265 0.036 Uiso 1 1 calc R . . C13 C 0.2359(3) 0.2331(2) 0.26073(18) 0.0278(9) Uani 1 1 d . . . C14 C 0.2538(3) 0.1912(2) 0.19956(19) 0.0291(10) Uani 1 1 d . . . C15 C 0.2504(3) 0.2352(2) 0.13851(19) 0.0306(10) Uani 1 1 d . . . H15A H 0.2620 0.2060 0.0981 0.037 Uiso 1 1 calc R . . C16 C 0.2297(3) 0.3234(2) 0.13612(19) 0.0317(10) Uani 1 1 d . . . H16A H 0.2289 0.3534 0.0938 0.038 Uiso 1 1 calc R . . C17 C 0.2107(3) 0.3668(2) 0.19311(19) 0.0335(10) Uani 1 1 d . . . H17A H 0.1962 0.4266 0.1904 0.040 Uiso 1 1 calc R . . C18 C 0.2126(3) 0.3222(2) 0.25737(18) 0.0279(9) Uani 1 1 d . . . C19 C 0.2952(3) 0.0563(2) 0.1498(2) 0.0378(11) Uani 1 1 d . . . H19A H 0.3630 0.0566 0.1267 0.045 Uiso 1 1 calc R . . H19B H 0.2408 0.0796 0.1180 0.045 Uiso 1 1 calc R . . C20 C 0.3005(3) -0.0315(2) 0.1733(2) 0.0412(11) Uani 1 1 d . . . H20A H 0.2362 -0.0302 0.2019 0.049 Uiso 1 1 calc R . . H20B H 0.3056 -0.0658 0.1342 0.049 Uiso 1 1 calc R . . C21 C 0.3905(3) -0.1491(2) 0.2414(2) 0.0417(11) Uani 1 1 d . . . H21A H 0.3836 -0.1864 0.2076 0.050 Uiso 1 1 calc R . . H21B H 0.3314 -0.1413 0.2763 0.050 Uiso 1 1 calc R . . C22 C 0.4905(3) -0.1887(3) 0.2724(2) 0.0463(12) Uani 1 1 d . . . H22A H 0.4991 -0.1502 0.3048 0.056 Uiso 1 1 calc R . . H22B H 0.4909 -0.2426 0.2969 0.056 Uiso 1 1 calc R . . C23 C 0.6739(3) -0.2492(3) 0.2434(2) 0.0490(12) Uani 1 1 d . . . H23A H 0.7238 -0.2677 0.2036 0.059 Uiso 1 1 calc R . . H23B H 0.6708 -0.3009 0.2701 0.059 Uiso 1 1 calc R . . C24 C 0.7135(4) -0.1989(3) 0.2842(2) 0.0525(13) Uani 1 1 d . . . H24A H 0.6682 -0.1858 0.3266 0.063 Uiso 1 1 calc R . . H24B H 0.7845 -0.2331 0.2959 0.063 Uiso 1 1 calc R . . C25 C 0.8075(4) -0.1297(3) 0.2053(2) 0.0528(13) Uani 1 1 d . . . H25A H 0.8122 -0.1705 0.1709 0.063 Uiso 1 1 calc R . . H25B H 0.8703 -0.1522 0.2305 0.063 Uiso 1 1 calc R . . C26 C 0.8030(3) -0.0452(2) 0.1719(2) 0.0468(12) Uani 1 1 d . . . H26A H 0.8663 -0.0511 0.1409 0.056 Uiso 1 1 calc R . . H26B H 0.7413 -0.0231 0.1456 0.056 Uiso 1 1 calc R . . C27 C 0.7838(3) 0.0949(2) 0.2022(2) 0.0310(10) Uani 1 1 d . . . C28 C 0.7908(3) 0.1238(2) 0.1374(2) 0.0346(10) Uani 1 1 d . . . H28A H 0.8081 0.0853 0.1022 0.041 Uiso 1 1 calc R . . C29 C 0.7724(3) 0.2111(2) 0.12235(19) 0.0329(10) Uani 1 1 d . . . H29A H 0.7759 0.2309 0.0767 0.039 Uiso 1 1 calc R . . C30 C 0.7497(3) 0.2680(2) 0.17137(18) 0.0284(9) Uani 1 1 d . . . H30A H 0.7372 0.3267 0.1601 0.034 Uiso 1 1 calc R . . C31 C 0.7452(2) 0.2383(2) 0.23944(18) 0.0251(9) Uani 1 1 d . . . C32 C 0.7238(3) 0.2938(2) 0.29312(19) 0.0285(10) Uani 1 1 d . . . C33 C 0.7197(3) 0.2642(2) 0.35887(19) 0.0305(10) Uani 1 1 d . . . H33A H 0.7066 0.3021 0.3941 0.037 Uiso 1 1 calc R . . C34 C 0.7349(3) 0.1774(2) 0.37379(19) 0.0315(10) Uani 1 1 d . . . H34A H 0.7310 0.1573 0.4193 0.038 Uiso 1 1 calc R . . C35 C 0.7549(3) 0.1220(2) 0.32433(19) 0.0300(10) Uani 1 1 d . . . H35A H 0.7645 0.0637 0.3355 0.036 Uiso 1 1 calc R . . C36 C 0.7615(3) 0.1505(2) 0.25592(18) 0.0264(9) Uani 1 1 d . . . C37 C 1.0346(3) 0.8993(3) -0.7273(2) 0.0411(11) Uani 1 1 d . . . C38 C 1.0020(4) 0.8967(3) -0.6539(2) 0.0578(14) Uani 1 1 d . . . H38A H 1.0564 0.9053 -0.6290 0.069 Uiso 1 1 calc R . . H38B H 0.9369 0.9445 -0.6446 0.069 Uiso 1 1 calc R . . C39 C 0.9844(5) 0.8167(4) -0.6280(3) 0.0860(17) Uani 1 1 d . . . H39A H 1.0472 0.7685 -0.6410 0.103 Uiso 1 1 calc R . . H39B H 0.9255 0.8108 -0.6498 0.103 Uiso 1 1 calc R . . C40 C 0.9603(4) 0.8104(3) -0.5511(2) 0.0547(12) Uani 1 1 d . . . H40A H 0.9051 0.8628 -0.5363 0.066 Uiso 1 1 calc R . . H40B H 0.9346 0.7618 -0.5388 0.066 Uiso 1 1 calc R . . C41 C 1.0574(3) 0.7983(3) -0.51631(19) 0.0393(11) Uani 1 1 d . . . H41A H 1.1132 0.7472 -0.5330 0.047 Uiso 1 1 calc R . . H41B H 1.0815 0.8479 -0.5279 0.047 Uiso 1 1 calc R . . C42 C 1.0182(3) 0.8565(2) -0.40510(19) 0.0331(10) Uani 1 1 d . . . H42A H 1.0119 0.9105 -0.4267 0.040 Uiso 1 1 calc R . . C43 C 1.0050(3) 0.8496(2) -0.33640(19) 0.0310(10) Uani 1 1 d . . . H43A H 0.9894 0.8987 -0.3111 0.037 Uiso 1 1 calc R . . C44 C 1.0144(3) 0.7713(2) -0.30351(18) 0.0252(9) Uani 1 1 d . . . C45 C 1.0337(3) 0.7022(2) -0.34409(18) 0.0289(9) Uani 1 1 d . . . H45A H 1.0383 0.6477 -0.3240 0.035 Uiso 1 1 calc R . . C46 C 1.0458(3) 0.7127(2) -0.4119(2) 0.0330(10) Uani 1 1 d . . . H46A H 1.0589 0.6652 -0.4386 0.040 Uiso 1 1 calc R . . C47 C 1.0067(2) 0.7610(2) -0.22906(18) 0.0256(9) Uani 1 1 d . . . C48 C 0.9817(3) 0.8301(2) -0.18877(19) 0.0295(10) Uani 1 1 d . . . H48A H 0.9663 0.8859 -0.2088 0.035 Uiso 1 1 calc R . . C49 C 0.9793(3) 0.8180(2) -0.12009(19) 0.0311(10) Uani 1 1 d . . . H49A H 0.9630 0.8658 -0.0932 0.037 Uiso 1 1 calc R . . C50 C 1.0242(3) 0.6723(2) -0.12831(19) 0.0315(10) Uani 1 1 d . . . H50A H 1.0391 0.6171 -0.1072 0.038 Uiso 1 1 calc R . . C51 C 1.0282(3) 0.6812(2) -0.19674(19) 0.0299(10) Uani 1 1 d . . . H51A H 1.0460 0.6323 -0.2225 0.036 Uiso 1 1 calc R . . C52 C 1.0012(3) 0.7297(2) -0.01554(18) 0.0325(10) Uani 1 1 d . . . H52A H 0.9588 0.7842 0.0042 0.039 Uiso 1 1 calc R . . H52B H 1.0737 0.7172 -0.0041 0.039 Uiso 1 1 calc R . . C53 C 0.9606(3) 0.6605(2) 0.01632(19) 0.0364(10) Uani 1 1 d . . . H53A H 1.0068 0.6045 0.0010 0.044 Uiso 1 1 calc R . . H53B H 0.8899 0.6696 0.0027 0.044 Uiso 1 1 calc R . . C54 C 0.9569(3) 0.6619(2) 0.09218(19) 0.0372(11) Uani 1 1 d . . . H54A H 1.0225 0.6679 0.1043 0.045 Uiso 1 1 calc R . . H54B H 0.8988 0.7122 0.1078 0.045 Uiso 1 1 calc R . . C55 C 0.9425(3) 0.5831(3) 0.12821(19) 0.0391(11) Uani 1 1 d . . . H55A H 0.8782 0.5759 0.1148 0.047 Uiso 1 1 calc R . . H55B H 1.0019 0.5330 0.1138 0.047 Uiso 1 1 calc R . . C56 C 0.9350(3) 0.5855(3) 0.2035(2) 0.0344(10) Uani 1 1 d . . . C57 C 0.3190(3) 0.0920(3) -0.0297(2) 0.0395(11) Uani 1 1 d . . . C58 C 0.4011(4) 0.1319(3) -0.0538(2) 0.0642(16) Uani 1 1 d . . . H58A H 0.4650 0.1002 -0.0314 0.077 Uiso 1 1 calc R . . H58B H 0.4178 0.1234 -0.1025 0.077 Uiso 1 1 calc R . . C59 C 0.3776(4) 0.2234(3) -0.0432(2) 0.0598(14) Uani 1 1 d . . . H59A H 0.3595 0.2330 0.0053 0.072 Uiso 1 1 calc R . . H59B H 0.3157 0.2562 -0.0670 0.072 Uiso 1 1 calc R . . C60 C 0.4649(3) 0.2564(3) -0.0669(2) 0.0474(12) Uani 1 1 d . . . H60A H 0.4358 0.3192 -0.0676 0.057 Uiso 1 1 calc R . . H60B H 0.4862 0.2405 -0.1141 0.057 Uiso 1 1 calc R . . C61 C 0.5626(3) 0.2314(3) -0.03119(19) 0.0402(11) Uani 1 1 d . . . H61A H 0.6014 0.1706 -0.0376 0.048 Uiso 1 1 calc R . . H61B H 0.6074 0.2646 -0.0516 0.048 Uiso 1 1 calc R . . C62 C 0.5134(3) 0.3251(2) 0.06313(19) 0.0329(10) Uani 1 1 d . . . H62A H 0.5092 0.3711 0.0312 0.039 Uiso 1 1 calc R . . C63 C 0.4905(3) 0.3409(2) 0.12965(19) 0.0316(10) Uani 1 1 d . . . H63A H 0.4707 0.3975 0.1436 0.038 Uiso 1 1 calc R . . C64 C 0.4960(2) 0.2742(2) 0.17752(18) 0.0261(9) Uani 1 1 d . . . C65 C 0.5238(3) 0.1929(2) 0.15344(19) 0.0323(10) Uani 1 1 d . . . H65A H 0.5272 0.1456 0.1839 0.039 Uiso 1 1 calc R . . C66 C 0.5461(3) 0.1809(2) 0.0864(2) 0.0374(11) Uani 1 1 d . . . H66A H 0.5653 0.1251 0.0708 0.045 Uiso 1 1 calc R . . C67 C 0.4759(3) 0.2881(2) 0.25036(19) 0.0272(9) Uani 1 1 d . . . C68 C 0.4491(3) 0.3695(2) 0.2752(2) 0.0335(10) Uani 1 1 d . . . H68A H 0.4430 0.4172 0.2448 0.040 Uiso 1 1 calc R . . C69 C 0.4319(3) 0.3805(2) 0.3424(2) 0.0347(10) Uani 1 1 d . . . H69A H 0.4155 0.4358 0.3584 0.042 Uiso 1 1 calc R . . C70 C 0.4628(3) 0.2354(2) 0.36456(19) 0.0311(10) Uani 1 1 d . . . H70A H 0.4671 0.1890 0.3961 0.037 Uiso 1 1 calc R . . C71 C 0.4827(3) 0.2210(2) 0.29733(19) 0.0297(10) Uani 1 1 d . . . H71A H 0.5011 0.1647 0.2827 0.036 Uiso 1 1 calc R . . C72 C 0.4172(3) 0.3282(2) 0.45994(19) 0.0348(10) Uani 1 1 d . . . H72A H 0.3877 0.2852 0.4823 0.042 Uiso 1 1 calc R . . H72B H 0.3656 0.3851 0.4677 0.042 Uiso 1 1 calc R . . C73 C 0.5169(3) 0.3210(2) 0.48949(19) 0.0341(10) Uani 1 1 d . . . H73A H 0.5496 0.3603 0.4641 0.041 Uiso 1 1 calc R . . H73B H 0.5660 0.2624 0.4852 0.041 Uiso 1 1 calc R . . C74 C 0.4971(3) 0.3423(2) 0.56342(19) 0.0369(10) Uani 1 1 d . . . H74A H 0.4684 0.3009 0.5893 0.044 Uiso 1 1 calc R . . H74B H 0.4446 0.3995 0.5680 0.044 Uiso 1 1 calc R . . C75 C 0.5977(3) 0.3405(2) 0.5926(2) 0.0362(10) Uani 1 1 d . . . H75A H 0.5840 0.3494 0.6414 0.043 Uiso 1 1 calc R . . H75B H 0.6518 0.2844 0.5860 0.043 Uiso 1 1 calc R . . C76 C 0.6351(3) 0.4085(3) 0.55829(18) 0.0336(10) Uani 1 1 d . . . C98 C 0.5692(5) 0.9918(3) 0.4020(2) 0.0706(16) Uani 1 1 d . . . H98A H 0.4966 1.0115 0.3907 0.106 Uiso 1 1 calc R . . H98B H 0.6159 0.9786 0.3608 0.106 Uiso 1 1 calc R . . H98C H 0.5830 1.0364 0.4247 0.106 Uiso 1 1 calc R . . C99 C 0.5872(4) 0.9167(3) 0.4459(2) 0.0557(13) Uani 1 1 d . . . N1 N 1.0399(2) 0.78869(19) -0.44238(15) 0.0309(8) Uani 1 1 d . . . N2 N 0.9995(2) 0.74007(18) -0.09004(15) 0.0267(8) Uani 1 1 d . . . N3 N 0.5417(2) 0.2458(2) 0.04195(15) 0.0323(8) Uani 1 1 d . . . N4 N 0.4374(2) 0.31475(19) 0.38652(15) 0.0305(8) Uani 1 1 d . . . N5 N 0.6008(5) 0.8584(3) 0.4804(3) 0.1000(18) Uani 1 1 d . . . F1 F 0.1914(2) 0.5427(2) 0.05487(16) 0.0891(11) Uani 1 1 d . . . F2 F 0.2706(2) 0.63274(16) 0.00863(15) 0.0743(9) Uani 1 1 d . . . F3 F 0.2109(2) 0.56042(19) -0.05715(15) 0.0771(9) Uani 1 1 d . . . F4 F 0.3028(2) 0.43765(16) -0.00659(16) 0.0728(9) Uani 1 1 d . . . F5 F 0.3823(2) 0.5276(2) -0.05217(15) 0.0773(9) Uani 1 1 d . . . F6 F 0.3624(2) 0.51168(18) 0.05945(14) 0.0784(10) Uani 1 1 d . . . F7 F 0.3152(3) 0.9342(3) 0.4974(2) 0.1942(16) Uani 1 1 d . . . F8 F 0.2297(3) 1.0540(2) 0.44549(18) 0.1331(14) Uani 1 1 d . . . F9 F 0.1808(2) 0.9846(3) 0.37671(16) 0.0982(12) Uani 1 1 d . . . F10 F 0.3475(2) 0.9533(2) 0.38708(18) 0.0920(11) Uani 1 1 d . . . F11 F 0.2616(3) 0.86389(18) 0.4303(3) 0.144(2) Uani 1 1 d . . . F12 F 0.1447(2) 0.96425(18) 0.48566(16) 0.0844(10) Uani 1 1 d . . . O99 O 0.5308(2) 0.01967(16) 0.23494(15) 0.0468(8) Uani 1 1 d . . . H98 H 0.5950(14) -0.0308(14) 0.233(3) 0.102(19) Uiso 1 1 d . . . H99 H 0.4778(11) -0.0066(15) 0.227(3) 0.13(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0322(6) 0.0384(6) 0.0407(6) 0.0077(5) -0.0009(5) -0.0017(5) P2 0.0619(7) 0.0417(6) 0.0512(7) 0.0119(5) -0.0174(6) -0.0253(5) P3 0.0486(6) 0.0430(6) 0.0435(7) -0.0024(5) -0.0016(5) -0.0220(5) P4 0.0379(6) 0.0447(6) 0.0301(6) -0.0051(5) 0.0021(5) -0.0147(5) O1 0.0362(14) 0.0263(13) 0.0333(15) -0.0020(11) 0.0029(12) -0.0103(11) O2 0.0517(18) 0.0540(19) 0.0408(18) 0.0025(15) 0.0047(15) 0.0048(15) O3 0.0483(19) 0.096(3) 0.087(3) 0.043(2) -0.0161(18) -0.0211(18) O4 0.095(2) 0.0590(19) 0.0411(18) 0.0037(15) -0.0113(17) -0.0394(17) O5 0.0449(15) 0.0328(14) 0.0335(15) -0.0070(12) -0.0084(12) -0.0100(12) O6 0.0401(14) 0.0314(14) 0.0361(15) -0.0075(12) -0.0025(12) -0.0111(12) O7 0.0389(14) 0.0326(14) 0.0445(16) -0.0008(12) -0.0080(13) -0.0150(12) O8 0.0488(15) 0.0395(15) 0.0375(16) 0.0097(12) -0.0136(13) -0.0167(13) O9 0.0468(16) 0.0247(14) 0.070(2) 0.0031(14) -0.0092(15) -0.0109(12) O10 0.0433(15) 0.0312(14) 0.0474(17) -0.0070(12) -0.0077(13) -0.0158(12) O11 0.145(3) 0.048(2) 0.059(2) -0.0228(18) 0.002(2) -0.019(2) O12 0.0631(18) 0.0378(17) 0.0566(19) 0.0041(14) -0.0118(16) -0.0150(14) O13 0.078(2) 0.0392(16) 0.0397(17) -0.0035(14) -0.0119(15) -0.0189(15) O14 0.0681(18) 0.0363(15) 0.0359(17) -0.0053(13) 0.0076(14) -0.0234(13) O15 0.055(2) 0.072(2) 0.084(3) 0.002(2) -0.0099(19) -0.0173(17) O16 0.091(2) 0.0334(16) 0.055(2) -0.0063(14) 0.0010(17) -0.0224(16) O17 0.0547(17) 0.0286(15) 0.0482(17) -0.0079(13) 0.0014(14) -0.0097(13) O18 0.0443(16) 0.0413(16) 0.0435(17) -0.0047(14) 0.0023(14) -0.0162(13) O19 0.0351(13) 0.0344(13) 0.0322(14) -0.0143(11) 0.0068(11) -0.0196(11) O20 0.0471(15) 0.0381(15) 0.0317(15) -0.0059(12) 0.0069(13) -0.0135(12) O21 0.0468(17) 0.0356(16) 0.0584(19) -0.0091(14) -0.0159(15) 0.0109(14) O22 0.0797(19) 0.102(2) 0.0406(18) -0.0073(16) 0.0162(16) -0.0636(18) O23 0.0490(15) 0.0577(17) 0.071(2) -0.0172(15) -0.0148(15) -0.0339(14) O24 0.0693(18) 0.0601(18) 0.0415(17) -0.0144(14) 0.0139(15) -0.0389(15) O25 0.0581(18) 0.0449(17) 0.060(2) -0.0139(15) 0.0184(16) -0.0176(14) O26 0.073(2) 0.0314(17) 0.100(3) 0.0250(17) 0.012(2) -0.0099(15) C1 0.035(2) 0.029(2) 0.041(2) -0.0073(18) 0.0019(18) -0.0074(17) C2 0.049(2) 0.033(2) 0.048(3) -0.008(2) 0.006(2) -0.009(2) C3 0.058(3) 0.055(3) 0.046(3) -0.007(2) -0.001(2) -0.027(2) C4 0.077(3) 0.041(3) 0.045(3) 0.016(2) -0.002(2) -0.020(2) C5 0.047(3) 0.126(5) 0.113(5) 0.061(4) -0.034(3) -0.022(3) C6 0.061(3) 0.086(4) 0.077(4) 0.022(3) -0.008(3) -0.018(3) C7 0.052(3) 0.042(2) 0.050(3) -0.006(2) -0.015(2) -0.010(2) C8 0.036(2) 0.039(2) 0.037(2) -0.0114(19) -0.0067(18) -0.0083(18) C9 0.0272(19) 0.034(2) 0.034(2) -0.0062(17) -0.0051(17) -0.0133(16) C10 0.0314(19) 0.046(2) 0.029(2) -0.0082(18) -0.0006(17) -0.0185(17) C11 0.0316(19) 0.045(2) 0.032(2) 0.0026(18) -0.0052(17) -0.0180(17) C12 0.0266(18) 0.036(2) 0.031(2) -0.0019(18) -0.0027(17) -0.0131(16) C13 0.0218(18) 0.032(2) 0.032(2) -0.0012(17) -0.0029(16) -0.0112(15) C14 0.0244(18) 0.031(2) 0.033(2) -0.0040(17) -0.0023(16) -0.0095(16) C15 0.0254(19) 0.035(2) 0.031(2) -0.0082(17) -0.0031(17) -0.0078(16) C16 0.0304(19) 0.040(2) 0.026(2) 0.0008(17) -0.0057(16) -0.0126(17) C17 0.0299(19) 0.036(2) 0.039(2) -0.0016(18) -0.0065(17) -0.0159(17) C18 0.0188(17) 0.039(2) 0.027(2) -0.0003(17) -0.0040(15) -0.0107(16) C19 0.037(2) 0.037(2) 0.038(2) -0.0150(19) -0.0074(18) -0.0059(18) C20 0.034(2) 0.040(2) 0.052(3) -0.014(2) -0.008(2) -0.0112(18) C21 0.053(2) 0.037(2) 0.040(2) -0.0026(19) 0.007(2) -0.0250(19) C22 0.073(3) 0.038(2) 0.033(2) 0.0019(19) -0.006(2) -0.025(2) C23 0.058(3) 0.030(2) 0.060(3) 0.010(2) -0.022(2) -0.013(2) C24 0.068(3) 0.032(2) 0.060(3) 0.009(2) -0.019(2) -0.018(2) C25 0.057(3) 0.033(2) 0.064(3) -0.014(2) 0.000(2) -0.008(2) C26 0.052(2) 0.038(2) 0.054(3) -0.017(2) 0.003(2) -0.017(2) C27 0.0246(18) 0.029(2) 0.042(2) 0.0021(18) -0.0085(17) -0.0109(16) C28 0.033(2) 0.040(2) 0.035(2) -0.0098(18) -0.0018(18) -0.0163(17) C29 0.0245(18) 0.047(2) 0.030(2) 0.0019(18) -0.0030(16) -0.0164(17) C30 0.0206(17) 0.031(2) 0.034(2) 0.0020(17) -0.0029(16) -0.0094(15) C31 0.0165(17) 0.031(2) 0.028(2) -0.0017(16) -0.0019(15) -0.0078(15) C32 0.0216(18) 0.027(2) 0.036(2) 0.0054(17) -0.0027(16) -0.0070(15) C33 0.0259(19) 0.030(2) 0.034(2) -0.0010(17) -0.0045(17) -0.0068(16) C34 0.0283(19) 0.038(2) 0.028(2) 0.0044(18) -0.0028(17) -0.0110(17) C35 0.0227(18) 0.026(2) 0.038(2) 0.0055(18) -0.0066(17) -0.0033(15) C36 0.0192(17) 0.027(2) 0.034(2) 0.0037(17) -0.0046(16) -0.0091(15) C37 0.050(2) 0.038(2) 0.031(2) 0.007(2) -0.002(2) -0.011(2) C38 0.061(3) 0.058(3) 0.055(3) 0.012(2) -0.014(2) -0.021(2) C39 0.135(4) 0.105(4) 0.054(3) 0.015(3) -0.029(3) -0.084(3) C40 0.076(3) 0.073(3) 0.035(3) 0.011(2) -0.011(2) -0.051(2) C41 0.047(2) 0.037(2) 0.028(2) 0.0034(18) 0.0004(19) -0.0085(19) C42 0.033(2) 0.028(2) 0.038(2) 0.0055(18) -0.0028(18) -0.0117(16) C43 0.0312(19) 0.027(2) 0.036(2) -0.0026(17) -0.0025(17) -0.0100(16) C44 0.0181(17) 0.0241(19) 0.034(2) -0.0002(16) -0.0047(16) -0.0067(14) C45 0.0272(18) 0.027(2) 0.033(2) 0.0012(17) -0.0035(17) -0.0101(16) C46 0.033(2) 0.030(2) 0.038(2) -0.0036(18) -0.0037(18) -0.0111(16) C47 0.0186(17) 0.0258(19) 0.035(2) 0.0012(17) -0.0066(16) -0.0097(14) C48 0.0226(18) 0.029(2) 0.037(2) 0.0007(17) -0.0033(17) -0.0081(15) C49 0.0284(19) 0.026(2) 0.038(2) -0.0065(17) -0.0049(17) -0.0054(16) C50 0.033(2) 0.0227(19) 0.039(2) 0.0003(17) -0.0004(18) -0.0100(16) C51 0.0281(19) 0.028(2) 0.033(2) -0.0055(17) 0.0002(17) -0.0077(16) C52 0.031(2) 0.034(2) 0.032(2) -0.0018(17) -0.0055(17) -0.0086(17) C53 0.036(2) 0.041(2) 0.033(2) -0.0007(18) 0.0009(18) -0.0161(18) C54 0.039(2) 0.037(2) 0.033(2) -0.0029(18) 0.0049(18) -0.0111(18) C55 0.047(2) 0.041(2) 0.029(2) -0.0035(18) -0.0016(19) -0.0154(19) C56 0.031(2) 0.034(2) 0.035(2) -0.0005(19) -0.0002(18) -0.0072(17) C57 0.034(2) 0.049(3) 0.036(2) 0.005(2) -0.0048(19) -0.0146(19) C58 0.113(4) 0.039(3) 0.034(3) -0.004(2) 0.027(3) -0.024(3) C59 0.071(3) 0.071(3) 0.041(3) -0.008(2) 0.001(2) -0.029(3) C60 0.052(2) 0.060(3) 0.039(3) -0.017(2) 0.007(2) -0.030(2) C61 0.042(2) 0.042(2) 0.034(2) 0.0012(19) 0.0064(19) -0.0128(19) C62 0.034(2) 0.034(2) 0.033(2) 0.0102(18) -0.0078(17) -0.0140(17) C63 0.0325(19) 0.0229(19) 0.042(2) 0.0025(17) -0.0117(18) -0.0104(16) C64 0.0182(17) 0.0274(19) 0.034(2) -0.0001(17) -0.0055(16) -0.0089(15) C65 0.038(2) 0.024(2) 0.034(2) -0.0010(17) 0.0018(18) -0.0100(16) C66 0.041(2) 0.024(2) 0.043(3) 0.0005(19) 0.0034(19) -0.0094(17) C67 0.0180(17) 0.028(2) 0.037(2) -0.0027(17) -0.0013(16) -0.0100(15) C68 0.036(2) 0.027(2) 0.042(2) 0.0005(18) -0.0045(18) -0.0158(16) C69 0.038(2) 0.028(2) 0.042(2) -0.0055(18) 0.0046(18) -0.0171(17) C70 0.0291(19) 0.026(2) 0.038(2) -0.0009(17) -0.0036(17) -0.0084(16) C71 0.0259(18) 0.026(2) 0.038(2) -0.0033(17) -0.0037(17) -0.0083(15) C72 0.033(2) 0.035(2) 0.036(2) -0.0067(18) 0.0068(18) -0.0128(17) C73 0.038(2) 0.030(2) 0.034(2) -0.0017(17) 0.0018(18) -0.0105(17) C74 0.044(2) 0.035(2) 0.031(2) -0.0011(18) 0.0062(18) -0.0152(18) C75 0.050(2) 0.026(2) 0.034(2) 0.0002(17) -0.0065(19) -0.0131(18) C76 0.033(2) 0.042(2) 0.026(2) -0.0089(18) -0.0046(17) -0.0097(18) C98 0.118(4) 0.053(3) 0.052(3) 0.011(2) -0.014(3) -0.043(3) C99 0.081(3) 0.053(3) 0.040(3) -0.004(2) -0.009(2) -0.029(2) N1 0.0272(16) 0.0319(18) 0.0315(18) 0.0002(15) -0.0014(14) -0.0076(13) N2 0.0212(14) 0.0296(17) 0.0308(18) -0.0024(14) -0.0033(13) -0.0096(13) N3 0.0280(16) 0.0351(18) 0.0308(18) 0.0011(15) 0.0016(14) -0.0079(14) N4 0.0241(15) 0.0349(18) 0.0337(18) -0.0059(15) 0.0022(14) -0.0118(13) N5 0.160(5) 0.071(3) 0.083(3) 0.031(3) -0.043(3) -0.055(3) F1 0.0631(18) 0.107(2) 0.079(2) 0.0100(18) 0.0268(16) -0.0166(17) F2 0.093(2) 0.0358(15) 0.083(2) 0.0020(14) -0.0107(17) -0.0066(14) F3 0.0641(17) 0.090(2) 0.0703(19) 0.0138(16) -0.0321(15) -0.0116(15) F4 0.0753(18) 0.0405(15) 0.099(2) 0.0016(15) -0.0100(17) -0.0142(13) F5 0.0581(15) 0.110(2) 0.0725(19) -0.0295(16) 0.0250(14) -0.0419(15) F6 0.0777(19) 0.0679(19) 0.0676(18) -0.0120(15) -0.0342(15) 0.0162(15) F7 0.220(3) 0.329(4) 0.127(3) 0.158(3) -0.126(2) -0.219(3) F8 0.250(4) 0.087(2) 0.096(2) -0.0310(17) 0.068(3) -0.118(2) F9 0.0679(19) 0.153(3) 0.067(2) 0.011(2) -0.0273(16) -0.024(2) F10 0.0552(17) 0.099(2) 0.116(3) 0.015(2) 0.0009(18) -0.0254(16) F11 0.071(2) 0.0314(16) 0.318(6) -0.023(3) 0.032(3) -0.0110(15) F12 0.115(2) 0.0649(17) 0.081(2) -0.0017(15) 0.0293(18) -0.0513(16) O99 0.0474(16) 0.0312(15) 0.065(2) 0.0094(14) -0.0139(15) -0.0166(13) _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 P1 F5 1.574(3) . ? P1 F1 1.575(3) . ? P1 F3 1.580(3) . ? P1 F6 1.584(3) . ? P1 F4 1.588(3) . ? P1 F2 1.588(3) . ? P2 F11 1.539(3) . ? P2 F7 1.539(4) . ? P2 F9 1.548(3) . ? P2 F8 1.554(3) . ? P2 F10 1.590(3) . ? P2 F12 1.596(3) . ? P3 O24 1.462(3) . ? P3 O25 1.465(3) . ? P3 O26 1.504(3) . ? P3 O23 1.536(3) . ? P4 O22 1.453(3) . ? P4 O20 1.454(3) . ? P4 O21 1.527(3) . ? P4 O19 1.534(3) . ? O1 C32 1.372(4) . ? O1 C1 1.435(4) . ? O2 C3 1.392(5) . ? O2 C2 1.393(5) . ? O3 C4 1.387(6) . ? O3 C5 1.470(6) . ? O4 C7 1.412(5) . ? O4 C6 1.440(6) . ? O5 C9 1.359(4) . ? O5 C8 1.432(5) . ? O6 C14 1.363(4) . ? O6 C19 1.432(4) . ? O7 C20 1.417(5) . ? O7 C21 1.425(5) . ? O8 C22 1.408(5) . ? O8 C23 1.435(5) . ? O9 C25 1.418(5) . ? O9 C24 1.436(5) . ? O10 C27 1.376(4) . ? O10 C26 1.426(5) . ? O11 C37 1.210(5) . ? O12 C37 1.289(5) . ? O13 C56 1.208(5) . ? O14 C56 1.323(5) . ? O15 C57 1.248(5) . ? O16 C57 1.278(5) . ? O17 C76 1.210(4) . ? O18 C76 1.333(4) . ? C1 C2 1.490(5) . ? C3 C4 1.480(6) . ? C5 C6 1.410(8) . ? C7 C8 1.486(6) . ? C9 C10 1.377(5) . ? C9 C18 1.422(5) . ? C10 C11 1.409(5) . ? C11 C12 1.355(5) . ? C12 C13 1.418(5) . ? C13 C18 1.413(5) . ? C13 C14 1.419(5) . ? C14 C15 1.374(5) . ? C15 C16 1.403(5) . ? C16 C17 1.357(5) . ? C17 C18 1.434(5) . ? C19 C20 1.484(6) . ? C21 C22 1.484(6) . ? C23 C24 1.474(6) . ? C25 C26 1.499(6) . ? C27 C28 1.355(5) . ? C27 C36 1.419(5) . ? C28 C29 1.409(5) . ? C29 C30 1.361(5) . ? C30 C31 1.417(5) . ? C31 C32 1.419(5) . ? C31 C36 1.426(5) . ? C32 C33 1.373(5) . ? C33 C34 1.407(5) . ? C34 C35 1.354(5) . ? C35 C36 1.419(5) . ? C37 C38 1.494(6) . ? C38 C39 1.479(7) . ? C39 C40 1.544(7) . ? C40 C41 1.510(6) . ? C41 N1 1.481(5) . ? C42 N1 1.340(5) . ? C42 C43 1.371(5) . ? C43 C44 1.390(5) . ? C44 C45 1.402(5) . ? C44 C47 1.485(5) . ? C45 C46 1.357(5) . ? C46 N1 1.344(5) . ? C47 C51 1.388(5) . ? C47 C48 1.390(5) . ? C48 C49 1.374(5) . ? C49 N2 1.344(5) . ? C50 N2 1.346(5) . ? C50 C51 1.366(5) . ? C52 N2 1.492(5) . ? C52 C53 1.510(5) . ? C53 C54 1.518(5) . ? C54 C55 1.511(6) . ? C55 C56 1.506(5) . ? C57 C58 1.503(7) . ? C58 C59 1.481(6) . ? C59 C60 1.490(6) . ? C60 C61 1.500(6) . ? C61 N3 1.487(5) . ? C62 N3 1.342(5) . ? C62 C63 1.363(5) . ? C63 C64 1.400(5) . ? C64 C65 1.395(5) . ? C64 C67 1.479(5) . ? C65 C66 1.362(5) . ? C66 N3 1.336(5) . ? C67 C71 1.391(5) . ? C67 C68 1.404(5) . ? C68 C69 1.359(5) . ? C69 N4 1.341(5) . ? C70 N4 1.352(5) . ? C70 C71 1.371(5) . ? C72 N4 1.489(5) . ? C72 C73 1.507(5) . ? C73 C74 1.527(5) . ? C74 C75 1.539(6) . ? C75 C76 1.486(6) . ? C98 C99 1.440(7) . ? C99 N5 1.124(6) . ? 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 F5 P1 F1 179.53(19) . . ? F5 P1 F3 89.95(16) . . ? F1 P1 F3 90.52(17) . . ? F5 P1 F6 89.88(17) . . ? F1 P1 F6 89.65(18) . . ? F3 P1 F6 178.93(18) . . ? F5 P1 F4 89.05(17) . . ? F1 P1 F4 90.99(18) . . ? F3 P1 F4 90.29(17) . . ? F6 P1 F4 90.77(16) . . ? F5 P1 F2 90.79(17) . . ? F1 P1 F2 89.17(18) . . ? F3 P1 F2 89.70(17) . . ? F6 P1 F2 89.25(17) . . ? F4 P1 F2 179.8(2) . . ? F11 P2 F7 90.1(3) . . ? F11 P2 F9 91.3(3) . . ? F7 P2 F9 178.3(2) . . ? F11 P2 F8 178.1(2) . . ? F7 P2 F8 90.5(3) . . ? F9 P2 F8 88.1(2) . . ? F11 P2 F10 92.2(2) . . ? F7 P2 F10 90.8(2) . . ? F9 P2 F10 88.37(18) . . ? F8 P2 F10 89.5(2) . . ? F11 P2 F12 87.84(19) . . ? F7 P2 F12 91.4(2) . . ? F9 P2 F12 89.44(18) . . ? F8 P2 F12 90.39(18) . . ? F10 P2 F12 177.8(2) . . ? O24 P3 O25 119.58(18) . . ? O24 P3 O26 107.95(18) . . ? O25 P3 O26 110.0(2) . . ? O24 P3 O23 108.38(18) . . ? O25 P3 O23 109.07(18) . . ? O26 P3 O23 100.0(2) . . ? O22 P4 O20 120.87(19) . . ? O22 P4 O21 108.24(19) . . ? O20 P4 O21 110.17(16) . . ? O22 P4 O19 108.24(17) . . ? O20 P4 O19 109.81(15) . . ? O21 P4 O19 96.82(16) . . ? C32 O1 C1 117.9(3) . . ? C3 O2 C2 115.5(3) . . ? C4 O3 C5 110.9(4) . . ? C7 O4 C6 109.7(4) . . ? C9 O5 C8 117.2(3) . . ? C14 O6 C19 118.7(3) . . ? C20 O7 C21 112.3(3) . . ? C22 O8 C23 114.7(3) . . ? C25 O9 C24 114.1(3) . . ? C27 O10 C26 116.9(3) . . ? O1 C1 C2 108.7(3) . . ? O2 C2 C1 114.9(4) . . ? O2 C3 C4 109.1(4) . . ? O3 C4 C3 110.6(4) . . ? C6 C5 O3 113.5(5) . . ? C5 C6 O4 110.7(5) . . ? O4 C7 C8 111.8(3) . . ? O5 C8 C7 109.2(3) . . ? O5 C9 C10 124.4(3) . . ? O5 C9 C18 115.1(3) . . ? C10 C9 C18 120.6(3) . . ? C9 C10 C11 119.7(4) . . ? C12 C11 C10 121.5(4) . . ? C11 C12 C13 119.9(4) . . ? C18 C13 C14 118.1(3) . . ? C18 C13 C12 119.9(3) . . ? C14 C13 C12 122.0(3) . . ? O6 C14 C15 124.8(3) . . ? O6 C14 C13 113.8(3) . . ? C15 C14 C13 121.4(3) . . ? C14 C15 C16 119.7(3) . . ? C17 C16 C15 121.3(4) . . ? C16 C17 C18 119.9(4) . . ? C13 C18 C9 118.6(3) . . ? C13 C18 C17 119.6(3) . . ? C9 C18 C17 121.9(3) . . ? O6 C19 C20 107.1(3) . . ? O7 C20 C19 109.7(3) . . ? O7 C21 C22 109.1(3) . . ? O8 C22 C21 108.7(3) . . ? O8 C23 C24 113.9(3) . . ? O9 C24 C23 112.4(4) . . ? O9 C25 C26 109.8(3) . . ? O10 C26 C25 108.2(4) . . ? C28 C27 O10 124.9(3) . . ? C28 C27 C36 121.4(3) . . ? O10 C27 C36 113.8(3) . . ? C27 C28 C29 119.8(4) . . ? C30 C29 C28 121.9(4) . . ? C29 C30 C31 118.9(3) . . ? C30 C31 C32 122.0(3) . . ? C30 C31 C36 120.2(3) . . ? C32 C31 C36 117.8(3) . . ? C33 C32 O1 123.9(3) . . ? C33 C32 C31 121.4(3) . . ? O1 C32 C31 114.7(3) . . ? C32 C33 C34 119.7(4) . . ? C35 C34 C33 121.1(4) . . ? C34 C35 C36 120.4(3) . . ? C27 C36 C35 122.7(3) . . ? C27 C36 C31 117.8(3) . . ? C35 C36 C31 119.5(3) . . ? O11 C37 O12 121.9(4) . . ? O11 C37 C38 125.2(4) . . ? O12 C37 C38 112.9(4) . . ? C39 C38 C37 114.3(4) . . ? C38 C39 C40 114.5(4) . . ? C41 C40 C39 110.1(4) . . ? N1 C41 C40 112.5(3) . . ? N1 C42 C43 121.4(3) . . ? C42 C43 C44 120.5(4) . . ? C43 C44 C45 116.7(3) . . ? C43 C44 C47 121.7(3) . . ? C45 C44 C47 121.7(3) . . ? C46 C45 C44 120.3(3) . . ? N1 C46 C45 121.7(4) . . ? C51 C47 C48 117.0(3) . . ? C51 C47 C44 121.2(3) . . ? C48 C47 C44 121.7(3) . . ? C49 C48 C47 120.2(3) . . ? N2 C49 C48 121.5(3) . . ? N2 C50 C51 121.5(3) . . ? C50 C51 C47 120.7(3) . . ? N2 C52 C53 114.5(3) . . ? C52 C53 C54 109.3(3) . . ? C55 C54 C53 113.3(3) . . ? C56 C55 C54 113.4(3) . . ? O13 C56 O14 122.9(4) . . ? O13 C56 C55 124.1(4) . . ? O14 C56 C55 113.0(3) . . ? O15 C57 O16 126.2(4) . . ? O15 C57 C58 119.1(4) . . ? O16 C57 C58 114.4(4) . . ? C59 C58 C57 118.0(4) . . ? C58 C59 C60 114.0(4) . . ? C59 C60 C61 121.5(4) . . ? N3 C61 C60 112.8(3) . . ? N3 C62 C63 121.1(3) . . ? C62 C63 C64 120.4(3) . . ? C65 C64 C63 116.8(3) . . ? C65 C64 C67 121.1(3) . . ? C63 C64 C67 122.1(3) . . ? C66 C65 C64 120.2(4) . . ? N3 C66 C65 121.7(4) . . ? C71 C67 C68 117.0(3) . . ? C71 C67 C64 121.4(3) . . ? C68 C67 C64 121.6(3) . . ? C69 C68 C67 120.5(4) . . ? N4 C69 C68 121.3(4) . . ? N4 C70 C71 120.8(3) . . ? C70 C71 C67 120.5(3) . . ? N4 C72 C73 110.2(3) . . ? C72 C73 C74 111.4(3) . . ? C73 C74 C75 111.5(3) . . ? C76 C75 C74 109.4(3) . . ? O17 C76 O18 122.0(4) . . ? O17 C76 C75 123.9(3) . . ? O18 C76 C75 114.1(3) . . ? N5 C99 C98 179.5(7) . . ? C42 N1 C46 119.4(3) . . ? C42 N1 C41 119.6(3) . . ? C46 N1 C41 121.0(3) . . ? C49 N2 C50 119.1(3) . . ? C49 N2 C52 119.6(3) . . ? C50 N2 C52 121.3(3) . . ? C66 N3 C62 119.8(3) . . ? C66 N3 C61 120.6(3) . . ? C62 N3 C61 119.5(3) . . ? C69 N4 C70 120.0(3) . . ? C69 N4 C72 120.5(3) . . ? C70 N4 C72 119.4(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O12 H12B O25 0.84 1.90 2.734(4) 170.3 1_654 O16 H16B O24 0.84 1.84 2.668(4) 170.6 1_545 O26 H26C O11 0.84 2.22 3.055(5) 176.7 1_456 O23 H23C O23 0.84 2.42 3.206(6) 156.8 2_575 O19 H19C O19 0.84 2.53 3.352(5) 167.7 2_766 O18 H18 O22 0.78(3) 1.86(4) 2.646(4) 174(3) . O14 H14 O20 1.06(6) 1.62(6) 2.614(4) 155(5) . O99 H98 O9 0.995(10) 1.878(16) 2.856(4) 167(5) . O99 H99 O7 0.994(10) 1.910(11) 2.900(4) 173.6(18) . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 22.70 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.970 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.065 # Attachment 'Pecoraro-CIF_IIb.cif' data_Pseudorotaxane_IIb(gm08) _database_code_depnum_ccdc_archive 'CCDC 633579' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C36 H44 O10, 2(C20 H26 N2 O4), 4(F6 P), 2(C2 H3 N) ; _chemical_formula_sum 'C80 H102 F24 N6 O18 P4' _chemical_formula_weight 2015.56 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.3358(19) _cell_length_b 16.055(2) _cell_length_c 20.135(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.999(9) _cell_angle_gamma 90.00 _cell_volume 4533.1(10) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8424 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 23.93 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 0.201 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9384 _exptl_absorpt_correction_T_max 0.9685 _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38. Sheldrick, G. SADABS (Version 2.10) Bruker/Siemens area detector absorption and other corrections, University of Gottingen, Germany 2003. ; _exptl_special_details ; 2590 frames x 30 sec. @ 4.969 cm; 0.5 deg. steps in omega & phi ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8424 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0285 _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 -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 24.50 _reflns_number_total 7516 _reflns_number_gt 5633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0484P)^2^+4.1160P] 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 7516 _refine_ls_number_parameters 602 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 P1 P 1.07147(5) 0.22508(5) 0.95949(5) 0.0441(2) Uani 1 1 d . . . P2 P 0.65971(5) 0.43987(4) 0.15388(3) 0.03411(19) Uani 1 1 d . . . N1 N 0.42496(13) 0.37278(12) 0.62873(9) 0.0208(4) Uani 1 1 d . . . N2 N 0.75880(14) 0.35686(12) 0.93591(10) 0.0247(5) Uani 1 1 d . . . N5 N 0.8722(3) 0.3012(3) 0.72254(18) 0.0864(11) Uani 1 1 d . . . O1 O 0.17507(15) 0.49581(19) 0.33548(11) 0.0674(8) Uani 1 1 d . . . O2 O 0.28205(14) 0.49977(14) 0.27135(9) 0.0421(5) Uani 1 1 d . . . H2 H 0.234(3) 0.505(2) 0.2378(19) 0.063 Uiso 1 1 d . . . O3 O 1.02800(14) 0.51974(16) 1.23387(10) 0.0520(6) Uani 1 1 d . . . H3 H 1.085(3) 0.515(2) 1.266(2) 0.078 Uiso 1 1 d . . . O4 O 1.13429(12) 0.51745(12) 1.16770(9) 0.0357(4) Uani 1 1 d . . . O5 O 0.67191(13) 0.82297(11) 0.42678(9) 0.0348(4) Uani 1 1 d . . . O6 O 0.70056(13) 0.73856(11) 0.30702(9) 0.0355(4) Uani 1 1 d . . . O7 O 0.79763(12) 0.57787(11) 0.33827(9) 0.0311(4) Uani 1 1 d . . . O8 O 0.75288(12) 0.42485(11) 0.39310(9) 0.0319(4) Uani 1 1 d . . . O9 O 0.46201(12) 0.21424(11) 0.48812(9) 0.0325(4) Uani 1 1 d . . . C1 C 0.25833(18) 0.49267(16) 0.32918(12) 0.0275(6) Uani 1 1 d . . . C2 C 0.33908(17) 0.48168(16) 0.38951(12) 0.0265(6) Uani 1 1 d . . . H2A H 0.3617 0.5372 0.4074 0.032 Uiso 1 1 calc R . . H2B H 0.3927 0.4533 0.3749 0.032 Uiso 1 1 calc R . . C3 C 0.30976(17) 0.43113(16) 0.44588(12) 0.0245(5) Uani 1 1 d . . . H3A H 0.2953 0.3734 0.4297 0.029 Uiso 1 1 calc R . . H3B H 0.2507 0.4553 0.4560 0.029 Uiso 1 1 calc R . . C4 C 0.38641(16) 0.42897(15) 0.51100(11) 0.0225(5) Uani 1 1 d . . . H4A H 0.4458 0.4049 0.5015 0.027 Uiso 1 1 calc R . . H4B H 0.4004 0.4863 0.5282 0.027 Uiso 1 1 calc R . . C5 C 0.35233(16) 0.37670(15) 0.56434(11) 0.0227(5) Uani 1 1 d . . . H5A H 0.2927 0.4009 0.5734 0.027 Uiso 1 1 calc R . . H5B H 0.3380 0.3196 0.5466 0.027 Uiso 1 1 calc R . . C6 C 0.48532(16) 0.30789(15) 0.64109(12) 0.0231(5) Uani 1 1 d . . . H6A H 0.4812 0.2644 0.6086 0.028 Uiso 1 1 calc R . . C7 C 0.55289(17) 0.30395(15) 0.70038(12) 0.0232(5) Uani 1 1 d . . . H7A H 0.5956 0.2581 0.7086 0.028 Uiso 1 1 calc R . . C8 C 0.55874(16) 0.36707(14) 0.74833(11) 0.0211(5) Uani 1 1 d . . . C9 C 0.49581(17) 0.43414(15) 0.73367(12) 0.0251(5) Uani 1 1 d . . . H9A H 0.4991 0.4789 0.7649 0.030 Uiso 1 1 calc R . . C10 C 0.42914(17) 0.43508(15) 0.67396(12) 0.0246(5) Uani 1 1 d . . . H10A H 0.3855 0.4802 0.6644 0.030 Uiso 1 1 calc R . . C11 C 0.62854(16) 0.36271(14) 0.81419(12) 0.0226(5) Uani 1 1 d . . . C12 C 0.71651(17) 0.32350(15) 0.81941(12) 0.0260(6) Uani 1 1 d . . . H12A H 0.7323 0.2979 0.7806 0.031 Uiso 1 1 calc R . . C13 C 0.78035(17) 0.32178(15) 0.88046(13) 0.0275(6) Uani 1 1 d . . . H13A H 0.8405 0.2955 0.8835 0.033 Uiso 1 1 calc R . . C14 C 0.67322(17) 0.39348(15) 0.93283(12) 0.0258(5) Uani 1 1 d . . . H14A H 0.6582 0.4165 0.9728 0.031 Uiso 1 1 calc R . . C15 C 0.60792(17) 0.39780(15) 0.87280(12) 0.0241(5) Uani 1 1 d . . . H15A H 0.5485 0.4247 0.8711 0.029 Uiso 1 1 calc R . . C16 C 0.83008(18) 0.35757(16) 1.00175(13) 0.0304(6) Uani 1 1 d . . . H16A H 0.8844 0.3211 0.9979 0.037 Uiso 1 1 calc R . . H16B H 0.8002 0.3349 1.0380 0.037 Uiso 1 1 calc R . . C17 C 0.86655(17) 0.44477(15) 1.02102(12) 0.0255(5) Uani 1 1 d . . . H17A H 0.8133 0.4806 1.0282 0.031 Uiso 1 1 calc R . . H17B H 0.8933 0.4691 0.9838 0.031 Uiso 1 1 calc R . . C18 C 0.94343(18) 0.44120(16) 1.08600(13) 0.0284(6) Uani 1 1 d . . . H18A H 1.0012 0.4143 1.0762 0.034 Uiso 1 1 calc R . . H18B H 0.9204 0.4067 1.1201 0.034 Uiso 1 1 calc R . . C19 C 0.96929(18) 0.52846(16) 1.11555(13) 0.0289(6) Uani 1 1 d . . . H19A H 0.9870 0.5648 1.0804 0.035 Uiso 1 1 calc R . . H19B H 0.9134 0.5534 1.1298 0.035 Uiso 1 1 calc R . . C20 C 1.05067(18) 0.52273(16) 1.17500(13) 0.0282(6) Uani 1 1 d . . . C21 C 0.6445(2) 0.87900(17) 0.47362(16) 0.0405(7) Uani 1 1 d . . . H21A H 0.5861 0.9094 0.4516 0.049 Uiso 1 1 calc R . . H21B H 0.6958 0.9202 0.4889 0.049 Uiso 1 1 calc R . . C22 C 0.7019(2) 0.86362(18) 0.37187(16) 0.0430(7) Uani 1 1 d . . . H22A H 0.7408 0.9131 0.3889 0.052 Uiso 1 1 calc R . . H22B H 0.6454 0.8826 0.3382 0.052 Uiso 1 1 calc R . . C23 C 0.7594(2) 0.80454(18) 0.33892(15) 0.0406(7) Uani 1 1 d . . . H23A H 0.7872 0.8347 0.3047 0.049 Uiso 1 1 calc R . . H23B H 0.8124 0.7815 0.3736 0.049 Uiso 1 1 calc R . . C24 C 0.7434(2) 0.69009(18) 0.26213(14) 0.0369(7) Uani 1 1 d . . . H24A H 0.7644 0.7284 0.2295 0.044 Uiso 1 1 calc R . . H24B H 0.6939 0.6532 0.2357 0.044 Uiso 1 1 calc R . . C25 C 0.8272(2) 0.63712(17) 0.29433(14) 0.0361(6) Uani 1 1 d . . . H25A H 0.8529 0.6080 0.2587 0.043 Uiso 1 1 calc R . . H25B H 0.8783 0.6727 0.3205 0.043 Uiso 1 1 calc R . . C26 C 0.86589(19) 0.51285(18) 0.35606(15) 0.0386(7) Uani 1 1 d . . . H26A H 0.9308 0.5369 0.3685 0.046 Uiso 1 1 calc R . . H26B H 0.8636 0.4753 0.3168 0.046 Uiso 1 1 calc R . . C27 C 0.84428(18) 0.46479(18) 0.41473(15) 0.0355(6) Uani 1 1 d . . . H27A H 0.8943 0.4224 0.4299 0.043 Uiso 1 1 calc R . . H27B H 0.8426 0.5028 0.4532 0.043 Uiso 1 1 calc R . . C28 C 0.72048(17) 0.37785(15) 0.44018(12) 0.0260(6) Uani 1 1 d . . . C29 C 0.76866(18) 0.36644(15) 0.50595(13) 0.0279(6) Uani 1 1 d . . . H29A H 0.8296 0.3911 0.5212 0.033 Uiso 1 1 calc R . . C30 C 0.72776(18) 0.31818(15) 0.55078(13) 0.0274(6) Uani 1 1 d . . . H30A H 0.7618 0.3104 0.5961 0.033 Uiso 1 1 calc R . . C31 C 0.63985(18) 0.28214(15) 0.53036(13) 0.0270(6) Uani 1 1 d . . . H31A H 0.6136 0.2495 0.5613 0.032 Uiso 1 1 calc R . . C32 C 0.58793(17) 0.29378(15) 0.46267(12) 0.0250(5) Uani 1 1 d . . . C33 C 0.49562(18) 0.25796(15) 0.43970(13) 0.0287(6) Uani 1 1 d . . . C34 C 0.44744(19) 0.26845(16) 0.37386(13) 0.0325(6) Uani 1 1 d . . . H34A H 0.3856 0.2453 0.3591 0.039 Uiso 1 1 calc R . . C35 C 0.49021(19) 0.31385(17) 0.32823(14) 0.0342(6) Uani 1 1 d . . . H35A H 0.4567 0.3201 0.2825 0.041 Uiso 1 1 calc R . . C36 C 0.57805(19) 0.34911(16) 0.34763(13) 0.0311(6) Uani 1 1 d . . . H36A H 0.6054 0.3791 0.3157 0.037 Uiso 1 1 calc R . . C37 C 0.62873(17) 0.34069(15) 0.41617(12) 0.0264(6) Uani 1 1 d . . . C38 C 0.37406(19) 0.16923(18) 0.46685(15) 0.0388(7) Uani 1 1 d . . . H38A H 0.3790 0.1308 0.4292 0.047 Uiso 1 1 calc R . . H38B H 0.3210 0.2086 0.4506 0.047 Uiso 1 1 calc R . . C40 C 1.0035(4) 0.1890(3) 0.7552(2) 0.1020(16) Uani 1 1 d . . . H40A H 1.0366 0.1823 0.7175 0.153 Uiso 1 1 calc R . . H40B H 0.9758 0.1356 0.7645 0.153 Uiso 1 1 calc R . . H40C H 1.0489 0.2077 0.7957 0.153 Uiso 1 1 calc R . . C49 C 0.9282(3) 0.2504(3) 0.73693(19) 0.0604(10) Uani 1 1 d . . . F1 F 1.05550(13) 0.13834(12) 0.92064(12) 0.0689(6) Uani 1 1 d . . . F2 F 1.15131(13) 0.24805(13) 0.91854(11) 0.0655(6) Uani 1 1 d . . . F3 F 0.99397(13) 0.26818(13) 0.89971(10) 0.0671(6) Uani 1 1 d . . . F4 F 1.14865(14) 0.18419(12) 1.01771(11) 0.0695(6) Uani 1 1 d . . . F5 F 0.98897(15) 0.20302(13) 0.99859(13) 0.0777(7) Uani 1 1 d . . . F6 F 1.08501(15) 0.31307(11) 0.99739(10) 0.0631(5) Uani 1 1 d . . . F7 F 0.7046(2) 0.35021(14) 0.15451(14) 0.1010(9) Uani 1 1 d . . . F8 F 0.6289(2) 0.43736(17) 0.07391(10) 0.1031(9) Uani 1 1 d . . . F9 F 0.75498(15) 0.48247(16) 0.14702(13) 0.0864(7) Uani 1 1 d . . . F10 F 0.68803(14) 0.44384(13) 0.23315(9) 0.0629(5) Uani 1 1 d . . . F11 F 0.56068(16) 0.39860(14) 0.16094(11) 0.0805(7) Uani 1 1 d . . . F12 F 0.61139(14) 0.52880(11) 0.15379(10) 0.0597(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0245(4) 0.0385(4) 0.0650(6) -0.0035(4) -0.0009(4) 0.0050(3) P2 0.0473(4) 0.0308(4) 0.0261(4) -0.0032(3) 0.0119(3) -0.0023(3) N1 0.0202(10) 0.0233(11) 0.0185(10) 0.0006(8) 0.0029(8) -0.0021(8) N2 0.0227(11) 0.0225(11) 0.0247(11) 0.0003(9) -0.0047(9) -0.0016(9) N5 0.068(2) 0.129(4) 0.065(2) -0.002(2) 0.0212(19) 0.012(2) O1 0.0311(12) 0.133(2) 0.0374(12) 0.0291(14) 0.0049(10) 0.0094(13) O2 0.0325(11) 0.0707(15) 0.0214(10) 0.0034(10) 0.0019(8) -0.0002(10) O3 0.0293(11) 0.0974(19) 0.0275(11) 0.0061(11) 0.0018(9) -0.0007(11) O4 0.0281(10) 0.0505(12) 0.0269(10) -0.0030(9) 0.0021(8) 0.0001(9) O5 0.0350(10) 0.0254(10) 0.0453(11) -0.0036(8) 0.0112(9) -0.0044(8) O6 0.0312(10) 0.0328(11) 0.0411(11) 0.0047(8) 0.0045(9) -0.0034(8) O7 0.0323(10) 0.0308(10) 0.0318(10) 0.0061(8) 0.0103(8) 0.0041(8) O8 0.0334(10) 0.0323(10) 0.0299(10) 0.0054(8) 0.0066(8) 0.0019(8) O9 0.0271(9) 0.0331(10) 0.0371(11) -0.0081(8) 0.0063(8) -0.0069(8) C1 0.0292(14) 0.0308(14) 0.0217(13) 0.0006(11) 0.0036(11) -0.0033(11) C2 0.0261(13) 0.0298(14) 0.0223(13) -0.0001(11) 0.0019(10) 0.0017(11) C3 0.0239(13) 0.0275(13) 0.0210(12) -0.0020(10) 0.0021(10) 0.0006(10) C4 0.0216(12) 0.0237(13) 0.0212(12) -0.0015(10) 0.0022(10) 0.0005(10) C5 0.0204(12) 0.0264(13) 0.0185(12) -0.0011(10) -0.0024(10) -0.0004(10) C6 0.0251(13) 0.0234(13) 0.0211(12) -0.0016(10) 0.0054(10) -0.0001(10) C7 0.0225(12) 0.0239(13) 0.0224(13) 0.0013(10) 0.0031(10) 0.0022(10) C8 0.0191(12) 0.0230(12) 0.0207(12) 0.0027(10) 0.0029(10) -0.0026(10) C9 0.0259(13) 0.0246(13) 0.0237(13) -0.0042(10) 0.0025(11) 0.0000(11) C10 0.0247(13) 0.0218(13) 0.0256(13) -0.0007(10) 0.0011(10) 0.0026(10) C11 0.0216(12) 0.0204(12) 0.0242(13) 0.0000(10) 0.0011(10) -0.0040(10) C12 0.0242(13) 0.0272(14) 0.0259(13) -0.0019(11) 0.0033(11) -0.0005(11) C13 0.0216(13) 0.0254(13) 0.0336(15) -0.0006(11) 0.0011(11) 0.0009(10) C14 0.0260(13) 0.0242(13) 0.0251(13) -0.0028(10) 0.0006(11) -0.0003(11) C15 0.0214(12) 0.0233(13) 0.0258(13) -0.0002(10) 0.0006(10) 0.0034(10) C16 0.0285(14) 0.0288(14) 0.0282(14) 0.0009(11) -0.0073(11) 0.0006(11) C17 0.0228(13) 0.0293(14) 0.0227(13) 0.0007(10) 0.0007(10) -0.0014(11) C18 0.0248(13) 0.0303(14) 0.0268(14) -0.0005(11) -0.0022(11) -0.0009(11) C19 0.0272(13) 0.0285(14) 0.0287(14) -0.0034(11) 0.0007(11) -0.0017(11) C20 0.0301(14) 0.0263(14) 0.0272(14) -0.0020(11) 0.0039(11) -0.0063(11) C21 0.0339(15) 0.0277(15) 0.060(2) -0.0123(14) 0.0110(14) -0.0081(12) C22 0.0454(17) 0.0319(16) 0.0539(19) 0.0020(14) 0.0152(15) -0.0094(13) C23 0.0375(16) 0.0372(16) 0.0476(18) 0.0015(13) 0.0101(14) -0.0105(13) C24 0.0417(16) 0.0375(16) 0.0304(15) 0.0054(12) 0.0050(13) -0.0052(13) C25 0.0398(16) 0.0361(16) 0.0354(15) 0.0061(12) 0.0144(13) -0.0021(13) C26 0.0315(15) 0.0406(17) 0.0458(17) 0.0095(13) 0.0131(13) 0.0081(13) C27 0.0237(14) 0.0371(16) 0.0456(17) 0.0113(13) 0.0073(12) 0.0039(12) C28 0.0298(13) 0.0215(13) 0.0282(14) -0.0001(10) 0.0092(11) 0.0050(11) C29 0.0238(13) 0.0266(14) 0.0322(15) -0.0023(11) 0.0032(11) 0.0027(11) C30 0.0300(14) 0.0266(14) 0.0246(13) -0.0013(11) 0.0034(11) 0.0039(11) C31 0.0287(14) 0.0263(13) 0.0272(14) -0.0047(11) 0.0086(11) 0.0017(11) C32 0.0266(13) 0.0205(12) 0.0272(14) -0.0075(10) 0.0043(11) 0.0036(10) C33 0.0280(14) 0.0253(14) 0.0321(15) -0.0102(11) 0.0049(12) 0.0042(11) C34 0.0272(14) 0.0315(15) 0.0362(16) -0.0123(12) 0.0009(12) 0.0037(11) C35 0.0385(16) 0.0325(15) 0.0268(14) -0.0109(12) -0.0038(12) 0.0119(12) C36 0.0395(16) 0.0257(14) 0.0271(14) -0.0025(11) 0.0051(12) 0.0096(12) C37 0.0279(13) 0.0219(13) 0.0285(14) -0.0055(10) 0.0040(11) 0.0093(11) C38 0.0309(15) 0.0358(16) 0.0494(18) -0.0213(14) 0.0075(13) -0.0093(12) C40 0.151(5) 0.083(3) 0.074(3) -0.010(3) 0.029(3) 0.014(3) C49 0.057(2) 0.072(3) 0.053(2) -0.0143(19) 0.0147(19) -0.009(2) F1 0.0522(11) 0.0487(12) 0.1061(17) -0.0241(11) 0.0168(11) -0.0069(9) F2 0.0383(10) 0.0637(13) 0.0954(16) 0.0063(11) 0.0159(10) 0.0000(9) F3 0.0386(10) 0.0781(14) 0.0725(14) -0.0133(11) -0.0160(9) 0.0194(10) F4 0.0553(12) 0.0560(12) 0.0869(15) 0.0125(11) -0.0088(11) 0.0203(10) F5 0.0588(13) 0.0643(14) 0.1208(19) -0.0011(13) 0.0434(13) 0.0036(11) F6 0.0754(13) 0.0402(10) 0.0627(12) -0.0044(9) -0.0108(10) 0.0101(10) F7 0.146(2) 0.0503(14) 0.114(2) -0.0151(13) 0.0440(18) 0.0289(14) F8 0.164(3) 0.120(2) 0.0231(11) -0.0112(12) 0.0162(13) -0.0237(19) F9 0.0575(13) 0.1022(18) 0.1149(19) -0.0079(15) 0.0533(13) -0.0175(12) F10 0.0731(13) 0.0806(14) 0.0299(10) -0.0001(9) -0.0012(9) 0.0052(11) F11 0.0745(14) 0.0817(16) 0.0786(15) 0.0147(12) 0.0006(12) -0.0455(12) F12 0.0659(12) 0.0486(11) 0.0727(13) 0.0223(9) 0.0331(10) 0.0196(9) _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 P1 F4 1.578(2) . ? P1 F2 1.587(2) . ? P1 F1 1.590(2) . ? P1 F5 1.591(2) . ? P1 F6 1.598(2) . ? P1 F3 1.614(2) . ? P2 F9 1.559(2) . ? P2 F10 1.5643(18) . ? P2 F7 1.576(2) . ? P2 F8 1.579(2) . ? P2 F12 1.5867(19) . ? P2 F11 1.600(2) . ? N1 C6 1.344(3) . ? N1 C10 1.346(3) . ? N1 C5 1.486(3) . ? N2 C13 1.343(3) . ? N2 C14 1.350(3) . ? N2 C16 1.496(3) . ? N5 C49 1.138(5) . ? O1 C1 1.227(3) . ? O2 C1 1.284(3) . ? O3 C20 1.293(3) . ? O4 C20 1.241(3) . ? O5 C21 1.417(3) . ? O5 C22 1.425(3) . ? O6 C23 1.422(3) . ? O6 C24 1.425(3) . ? O7 C25 1.422(3) . ? O7 C26 1.425(3) . ? O8 C28 1.366(3) . ? O8 C27 1.442(3) . ? O9 C33 1.368(3) . ? O9 C38 1.439(3) . ? C1 C2 1.504(3) . ? C2 C3 1.524(3) . ? C3 C4 1.526(3) . ? C4 C5 1.521(3) . ? C6 C7 1.374(3) . ? C7 C8 1.390(3) . ? C8 C9 1.396(3) . ? C8 C11 1.487(3) . ? C9 C10 1.372(3) . ? C11 C12 1.394(3) . ? C11 C15 1.394(3) . ? C12 C13 1.372(3) . ? C14 C15 1.368(3) . ? C16 C17 1.516(3) . ? C17 C18 1.527(3) . ? C18 C19 1.537(3) . ? C19 C20 1.491(4) . ? C21 C38 1.496(4) 3_666 ? C22 C23 1.500(4) . ? C24 C25 1.504(4) . ? C26 C27 1.496(4) . ? C28 C29 1.373(3) . ? C28 C37 1.434(4) . ? C29 C30 1.407(4) . ? C30 C31 1.370(4) . ? C31 C32 1.423(3) . ? C32 C37 1.419(4) . ? C32 C33 1.429(4) . ? C33 C34 1.372(4) . ? C34 C35 1.409(4) . ? C35 C36 1.362(4) . ? C36 C37 1.426(4) . ? C38 C21 1.496(4) 3_666 ? C40 C49 1.451(6) . ? 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 F4 P1 F2 90.72(12) . . ? F4 P1 F1 90.47(12) . . ? F2 P1 F1 89.63(12) . . ? F4 P1 F5 91.05(13) . . ? F2 P1 F5 178.21(13) . . ? F1 P1 F5 90.16(12) . . ? F4 P1 F6 90.93(11) . . ? F2 P1 F6 90.77(12) . . ? F1 P1 F6 178.54(12) . . ? F5 P1 F6 89.40(12) . . ? F4 P1 F3 178.93(13) . . ? F2 P1 F3 88.39(12) . . ? F1 P1 F3 90.13(12) . . ? F5 P1 F3 89.84(12) . . ? F6 P1 F3 88.48(11) . . ? F9 P2 F10 91.50(13) . . ? F9 P2 F7 92.14(15) . . ? F10 P2 F7 90.58(13) . . ? F9 P2 F8 89.17(15) . . ? F10 P2 F8 178.54(15) . . ? F7 P2 F8 90.70(15) . . ? F9 P2 F12 89.74(12) . . ? F10 P2 F12 89.15(11) . . ? F7 P2 F12 178.11(14) . . ? F8 P2 F12 89.55(14) . . ? F9 P2 F11 178.46(14) . . ? F10 P2 F11 88.46(12) . . ? F7 P2 F11 89.40(15) . . ? F8 P2 F11 90.84(14) . . ? F12 P2 F11 88.72(12) . . ? C6 N1 C10 121.0(2) . . ? C6 N1 C5 120.12(19) . . ? C10 N1 C5 118.92(19) . . ? C13 N2 C14 120.6(2) . . ? C13 N2 C16 120.5(2) . . ? C14 N2 C16 119.0(2) . . ? C21 O5 C22 113.3(2) . . ? C23 O6 C24 113.5(2) . . ? C25 O7 C26 111.63(19) . . ? C28 O8 C27 117.0(2) . . ? C33 O9 C38 117.5(2) . . ? O1 C1 O2 122.5(2) . . ? O1 C1 C2 121.5(2) . . ? O2 C1 C2 116.0(2) . . ? C1 C2 C3 112.3(2) . . ? C2 C3 C4 113.0(2) . . ? C5 C4 C3 109.85(19) . . ? N1 C5 C4 111.70(19) . . ? N1 C6 C7 120.5(2) . . ? C6 C7 C8 120.0(2) . . ? C7 C8 C9 118.2(2) . . ? C7 C8 C11 121.1(2) . . ? C9 C8 C11 120.7(2) . . ? C10 C9 C8 119.7(2) . . ? N1 C10 C9 120.7(2) . . ? C12 C11 C15 117.8(2) . . ? C12 C11 C8 121.3(2) . . ? C15 C11 C8 120.9(2) . . ? C13 C12 C11 120.1(2) . . ? N2 C13 C12 120.7(2) . . ? N2 C14 C15 120.7(2) . . ? C14 C15 C11 120.1(2) . . ? N2 C16 C17 111.7(2) . . ? C16 C17 C18 109.5(2) . . ? C17 C18 C19 111.8(2) . . ? C20 C19 C18 109.9(2) . . ? O4 C20 O3 122.6(2) . . ? O4 C20 C19 121.6(2) . . ? O3 C20 C19 115.7(2) . . ? O5 C21 C38 108.9(2) . 3_666 ? O5 C22 C23 109.6(2) . . ? O6 C23 C22 110.0(2) . . ? O6 C24 C25 116.5(2) . . ? O7 C25 C24 109.4(2) . . ? O7 C26 C27 109.4(2) . . ? O8 C27 C26 108.4(2) . . ? O8 C28 C29 124.6(2) . . ? O8 C28 C37 114.6(2) . . ? C29 C28 C37 120.8(2) . . ? C28 C29 C30 120.0(2) . . ? C31 C30 C29 121.3(2) . . ? C30 C31 C32 119.8(2) . . ? C37 C32 C31 119.8(2) . . ? C37 C32 C33 118.8(2) . . ? C31 C32 C33 121.5(2) . . ? O9 C33 C34 124.8(2) . . ? O9 C33 C32 114.6(2) . . ? C34 C33 C32 120.6(2) . . ? C33 C34 C35 119.6(2) . . ? C36 C35 C34 122.0(2) . . ? C35 C36 C37 119.5(3) . . ? C32 C37 C36 119.5(2) . . ? C32 C37 C28 118.3(2) . . ? C36 C37 C28 122.3(2) . . ? O9 C38 C21 108.2(2) . 3_666 ? N5 C49 C40 176.9(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O4 0.86(4) 1.80(4) 2.662(3) 179(4) 1_454 O3 H3 O1 0.94(4) 1.72(4) 2.643(3) 168(4) 1_656 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.572 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.053 # Attachment 'Pecoraro-CIF_Ia.cif' data_Pseudorotaxane_Ia(m05) _database_code_depnum_ccdc_archive 'CCDC 633580' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H44 O10, C18 H22 N2 O4, 2(F6 P)' _chemical_formula_sum 'C54 H66 F12 N2 O14 P2' _chemical_formula_weight 1257.03 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7969(13) _cell_length_b 11.6598(14) _cell_length_c 13.4326(16) _cell_angle_alpha 69.073(2) _cell_angle_beta 66.558(2) _cell_angle_gamma 76.000(2) _cell_volume 1439.2(3) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7649 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 23.30 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 654 _exptl_absorpt_coefficient_mu 0.180 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9281 _exptl_absorpt_correction_T_max 0.9446 _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38. Sheldrick, G. SADABS (Version 2.10) Bruker/Siemens area detector absorption and other corrections, University of Gottingen, Germany 2003. ; _exptl_special_details ; 2740 frames x 20 sec. @ 4.969 cm; 0.5 deg. steps in omega & phi ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30512 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.35 _reflns_number_total 7147 _reflns_number_gt 6056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0515P)^2^+0.5344P] 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 7147 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.1020 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 P1 P 0.72763(4) 0.10773(3) 0.20663(3) 0.02765(9) Uani 1 1 d . . . F1 F 0.79306(12) -0.03047(9) 0.20946(11) 0.0565(3) Uani 1 1 d . . . F2 F 0.80199(12) 0.15444(10) 0.07237(8) 0.0514(3) Uani 1 1 d . . . F3 F 0.65230(9) 0.06410(9) 0.34147(7) 0.0405(2) Uani 1 1 d . . . F4 F 0.59844(11) 0.08518(9) 0.18920(9) 0.0485(3) Uani 1 1 d . . . F5 F 0.85691(9) 0.13212(8) 0.22474(7) 0.03612(19) Uani 1 1 d . . . F6 F 0.66334(9) 0.24758(7) 0.20502(8) 0.03524(19) Uani 1 1 d . . . O1 O 0.51917(9) 0.57817(9) 0.35285(8) 0.0273(2) Uani 1 1 d . . . H1 H 0.548(2) 0.571(2) 0.413(2) 0.066(7) Uiso 1 1 d . . . O2 O 0.38905(9) 0.43328(8) 0.48718(8) 0.02661(19) Uani 1 1 d . . . O3 O -0.26952(10) 0.05227(9) 0.83691(8) 0.0289(2) Uani 1 1 d . . . O4 O -0.12854(9) 0.39044(9) 0.36446(8) 0.02705(19) Uani 1 1 d . . . O5 O 0.07045(9) 0.46683(9) 0.13851(8) 0.0303(2) Uani 1 1 d . . . O6 O 0.35268(9) 0.39752(8) 0.07011(7) 0.02409(18) Uani 1 1 d . . . O7 O 0.34020(10) 0.17887(9) 0.03100(8) 0.0303(2) Uani 1 1 d . . . N1 N 0.25226(10) 0.19839(9) 0.37782(9) 0.0213(2) Uani 1 1 d . . . C1 C 0.42676(12) 0.50216(11) 0.39032(10) 0.0226(2) Uani 1 1 d . . . C2 C 0.37234(13) 0.50980(11) 0.30073(10) 0.0239(2) Uani 1 1 d . . . H2A H 0.4495 0.4963 0.2332 0.029 Uiso 1 1 calc R . . H2B H 0.3260 0.5941 0.2778 0.029 Uiso 1 1 calc R . . C3 C 0.27355(12) 0.41673(11) 0.33913(11) 0.0233(2) Uani 1 1 d . . . H3A H 0.2160 0.4454 0.2910 0.028 Uiso 1 1 calc R . . H3B H 0.2134 0.4102 0.4185 0.028 Uiso 1 1 calc R . . C4 C 0.34977(12) 0.29032(11) 0.33105(11) 0.0230(2) Uani 1 1 d . . . H4A H 0.4039 0.2950 0.2507 0.028 Uiso 1 1 calc R . . H4B H 0.4130 0.2645 0.3740 0.028 Uiso 1 1 calc R . . C5 C 0.22678(13) 0.12643(11) 0.48564(11) 0.0239(2) Uani 1 1 d . . . H5A H 0.2770 0.1304 0.5283 0.029 Uiso 1 1 calc R . . C6 C 0.12892(13) 0.04719(11) 0.53493(10) 0.0231(2) Uani 1 1 d . . . H6A H 0.1126 -0.0040 0.6110 0.028 Uiso 1 1 calc R . . C7 C 0.05384(11) 0.04189(10) 0.47356(10) 0.0187(2) Uani 1 1 d . . . C8 C 0.08407(13) 0.11704(11) 0.36083(10) 0.0227(2) Uani 1 1 d . . . H8A H 0.0356 0.1145 0.3162 0.027 Uiso 1 1 calc R . . C9 C 0.18342(13) 0.19442(12) 0.31449(10) 0.0243(2) Uani 1 1 d . . . H9A H 0.2037 0.2451 0.2380 0.029 Uiso 1 1 calc R . . C10 C -0.32077(17) -0.09652(13) 1.01672(12) 0.0351(3) Uani 1 1 d . . . H10A H -0.2893 -0.1440 1.0815 0.042 Uiso 1 1 calc R . . H10B H -0.4077 -0.0459 1.0448 0.042 Uiso 1 1 calc R . . C11 C -0.21669(16) -0.01426(13) 0.92709(12) 0.0326(3) Uani 1 1 d . . . H11A H -0.2011 0.0439 0.9584 0.039 Uiso 1 1 calc R . . H11B H -0.1294 -0.0643 0.8989 0.039 Uiso 1 1 calc R . . C12 C -0.19901(13) 0.14190(11) 0.74897(11) 0.0247(2) Uani 1 1 d . . . C13 C -0.09541(14) 0.19167(13) 0.74859(12) 0.0290(3) Uani 1 1 d . . . H13A H -0.0671 0.1632 0.8128 0.035 Uiso 1 1 calc R . . C14 C -0.03155(13) 0.28547(13) 0.65201(12) 0.0289(3) Uani 1 1 d . . . H14A H 0.0381 0.3213 0.6529 0.035 Uiso 1 1 calc R . . C15 C -0.06758(12) 0.32602(12) 0.55729(11) 0.0252(2) Uani 1 1 d . . . H15A H -0.0233 0.3893 0.4933 0.030 Uiso 1 1 calc R . . C16 C -0.17138(12) 0.27311(11) 0.55488(10) 0.0221(2) Uani 1 1 d . . . C17 C -0.20577(12) 0.30660(11) 0.45491(11) 0.0233(2) Uani 1 1 d . . . C18 C -0.30636(13) 0.25458(12) 0.45379(11) 0.0260(2) Uani 1 1 d . . . H18A H -0.3277 0.2767 0.3867 0.031 Uiso 1 1 calc R . . C19 C -0.37808(13) 0.16766(12) 0.55359(12) 0.0269(3) Uani 1 1 d . . . H19A H -0.4494 0.1338 0.5531 0.032 Uiso 1 1 calc R . . C20 C -0.34736(12) 0.13120(11) 0.65053(11) 0.0251(2) Uani 1 1 d . . . H20A H -0.3965 0.0724 0.7163 0.030 Uiso 1 1 calc R . . C21 C -0.24122(12) 0.18196(11) 0.65216(10) 0.0223(2) Uani 1 1 d . . . C22 C -0.15561(13) 0.42931(13) 0.26025(11) 0.0290(3) Uani 1 1 d . . . H22A H -0.2518 0.4646 0.2728 0.035 Uiso 1 1 calc R . . H22B H -0.1379 0.3581 0.2308 0.035 Uiso 1 1 calc R . . C23 C -0.06297(13) 0.52542(12) 0.17719(11) 0.0291(3) Uani 1 1 d . . . H23A H -0.0946 0.5709 0.1122 0.035 Uiso 1 1 calc R . . H23B H -0.0643 0.5855 0.2144 0.035 Uiso 1 1 calc R . . C24 C 0.16436(14) 0.55357(12) 0.06291(12) 0.0300(3) Uani 1 1 d . . . H24A H 0.1893 0.5917 0.1063 0.036 Uiso 1 1 calc R . . H24B H 0.1227 0.6199 0.0111 0.036 Uiso 1 1 calc R . . C25 C 0.28850(13) 0.48686(12) -0.00416(11) 0.0275(3) Uani 1 1 d . . . H25A H 0.2625 0.4455 -0.0446 0.033 Uiso 1 1 calc R . . H25B H 0.3523 0.5467 -0.0613 0.033 Uiso 1 1 calc R . . C26 C 0.47031(13) 0.32799(13) 0.01218(11) 0.0277(3) Uani 1 1 d . . . H26A H 0.5124 0.2705 0.0679 0.033 Uiso 1 1 calc R . . H26B H 0.5369 0.3857 -0.0442 0.033 Uiso 1 1 calc R . . C27 C 0.44343(14) 0.25442(13) -0.04797(11) 0.0303(3) Uani 1 1 d . . . H27A H 0.4140 0.3110 -0.1117 0.036 Uiso 1 1 calc R . . H27B H 0.5275 0.2023 -0.0791 0.036 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 P1 0.03693(19) 0.02272(16) 0.02805(17) -0.00262(13) -0.01952(14) -0.00467(13) F1 0.0668(7) 0.0278(5) 0.0803(8) -0.0176(5) -0.0345(6) 0.0034(4) F2 0.0778(7) 0.0541(6) 0.0281(4) -0.0128(4) -0.0157(5) -0.0212(5) F3 0.0453(5) 0.0442(5) 0.0292(4) 0.0043(4) -0.0169(4) -0.0162(4) F4 0.0635(6) 0.0402(5) 0.0596(6) 0.0012(4) -0.0456(5) -0.0187(4) F5 0.0330(4) 0.0397(5) 0.0386(5) -0.0064(4) -0.0188(4) -0.0060(3) F6 0.0373(4) 0.0248(4) 0.0441(5) -0.0050(3) -0.0202(4) -0.0014(3) O1 0.0283(4) 0.0285(5) 0.0259(4) -0.0062(4) -0.0076(4) -0.0105(4) O2 0.0291(4) 0.0264(4) 0.0250(4) -0.0040(4) -0.0101(4) -0.0085(4) O3 0.0318(5) 0.0265(5) 0.0263(4) -0.0044(4) -0.0092(4) -0.0058(4) O4 0.0257(4) 0.0306(5) 0.0243(4) -0.0055(4) -0.0080(4) -0.0073(4) O5 0.0260(4) 0.0229(4) 0.0333(5) -0.0018(4) -0.0063(4) -0.0044(4) O6 0.0276(4) 0.0241(4) 0.0202(4) -0.0027(3) -0.0108(3) -0.0037(3) O7 0.0391(5) 0.0268(5) 0.0224(4) -0.0070(4) -0.0048(4) -0.0100(4) N1 0.0225(5) 0.0184(5) 0.0239(5) -0.0053(4) -0.0094(4) -0.0029(4) C1 0.0213(5) 0.0192(5) 0.0259(6) -0.0079(5) -0.0060(5) -0.0014(4) C2 0.0264(6) 0.0215(6) 0.0225(5) -0.0053(5) -0.0071(5) -0.0042(4) C3 0.0225(5) 0.0226(6) 0.0258(6) -0.0066(5) -0.0093(5) -0.0029(4) C4 0.0222(5) 0.0218(6) 0.0250(6) -0.0052(5) -0.0079(5) -0.0052(4) C5 0.0283(6) 0.0212(6) 0.0257(6) -0.0034(5) -0.0155(5) -0.0035(5) C6 0.0285(6) 0.0194(5) 0.0233(5) -0.0021(4) -0.0142(5) -0.0031(4) C7 0.0212(5) 0.0148(5) 0.0217(5) -0.0068(4) -0.0093(4) 0.0008(4) C8 0.0277(6) 0.0231(6) 0.0204(5) -0.0049(5) -0.0116(5) -0.0047(5) C9 0.0289(6) 0.0245(6) 0.0206(5) -0.0042(5) -0.0108(5) -0.0049(5) C10 0.0520(9) 0.0304(7) 0.0243(6) -0.0077(5) -0.0119(6) -0.0100(6) C11 0.0456(8) 0.0295(7) 0.0270(6) -0.0069(5) -0.0157(6) -0.0083(6) C12 0.0258(6) 0.0211(6) 0.0260(6) -0.0096(5) -0.0064(5) -0.0008(4) C13 0.0318(6) 0.0296(7) 0.0293(6) -0.0103(5) -0.0128(5) -0.0031(5) C14 0.0278(6) 0.0304(7) 0.0336(7) -0.0125(5) -0.0112(5) -0.0062(5) C15 0.0225(6) 0.0239(6) 0.0290(6) -0.0102(5) -0.0061(5) -0.0038(4) C16 0.0193(5) 0.0204(5) 0.0263(6) -0.0110(5) -0.0053(4) 0.0001(4) C17 0.0197(5) 0.0226(6) 0.0262(6) -0.0096(5) -0.0056(5) -0.0003(4) C18 0.0235(6) 0.0274(6) 0.0290(6) -0.0109(5) -0.0099(5) -0.0007(5) C19 0.0215(6) 0.0268(6) 0.0350(7) -0.0128(5) -0.0087(5) -0.0035(5) C20 0.0220(5) 0.0217(6) 0.0301(6) -0.0102(5) -0.0051(5) -0.0028(4) C21 0.0209(5) 0.0196(5) 0.0262(6) -0.0107(5) -0.0061(5) 0.0004(4) C22 0.0242(6) 0.0339(7) 0.0281(6) -0.0061(5) -0.0110(5) -0.0032(5) C23 0.0274(6) 0.0279(6) 0.0297(6) -0.0041(5) -0.0123(5) -0.0013(5) C24 0.0310(6) 0.0221(6) 0.0303(6) 0.0009(5) -0.0098(5) -0.0061(5) C25 0.0308(6) 0.0266(6) 0.0218(6) 0.0008(5) -0.0118(5) -0.0052(5) C26 0.0251(6) 0.0311(6) 0.0229(6) -0.0029(5) -0.0083(5) -0.0042(5) C27 0.0335(7) 0.0284(6) 0.0219(6) -0.0048(5) -0.0039(5) -0.0048(5) _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 P1 F1 1.5887(10) . ? P1 F4 1.5972(9) . ? P1 F2 1.5974(10) . ? P1 F3 1.6033(9) . ? P1 F6 1.6063(9) . ? P1 F5 1.6124(9) . ? O1 C1 1.3206(15) . ? O2 C1 1.2222(15) . ? O3 C12 1.3618(15) . ? O3 C11 1.4349(16) . ? O4 C17 1.3664(15) . ? O4 C22 1.4349(16) . ? O5 C23 1.4120(16) . ? O5 C24 1.4232(15) . ? O6 C25 1.4208(15) . ? O6 C26 1.4289(16) . ? O7 C27 1.4179(16) . ? O7 C10 1.4216(17) 2_556 ? N1 C5 1.3431(16) . ? N1 C9 1.3513(16) . ? N1 C4 1.4801(15) . ? C1 C2 1.5040(17) . ? C2 C3 1.5179(17) . ? C3 C4 1.5224(17) . ? C5 C6 1.3737(17) . ? C6 C7 1.3902(16) . ? C7 C8 1.4016(16) . ? C7 C7 1.486(2) 2_556 ? C8 C9 1.3741(17) . ? C10 O7 1.4216(17) 2_556 ? C10 C11 1.501(2) . ? C12 C13 1.3768(18) . ? C12 C21 1.4323(18) . ? C13 C14 1.4121(19) . ? C14 C15 1.3670(19) . ? C15 C16 1.4195(17) . ? C16 C21 1.4203(17) . ? C16 C17 1.4303(18) . ? C17 C18 1.3734(18) . ? C18 C19 1.4167(18) . ? C19 C20 1.3662(19) . ? C20 C21 1.4218(17) . ? C22 C23 1.5040(18) . ? C24 C25 1.4995(19) . ? C26 C27 1.508(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 P1 F4 90.62(6) . . ? F1 P1 F2 91.08(6) . . ? F4 P1 F2 90.58(6) . . ? F1 P1 F3 90.19(6) . . ? F4 P1 F3 89.76(5) . . ? F2 P1 F3 178.68(6) . . ? F1 P1 F6 178.88(6) . . ? F4 P1 F6 90.43(5) . . ? F2 P1 F6 89.29(5) . . ? F3 P1 F6 89.42(5) . . ? F1 P1 F5 90.11(6) . . ? F4 P1 F5 179.24(6) . . ? F2 P1 F5 89.63(5) . . ? F3 P1 F5 90.01(5) . . ? F6 P1 F5 88.84(5) . . ? C12 O3 C11 118.35(11) . . ? C17 O4 C22 117.78(10) . . ? C23 O5 C24 111.94(10) . . ? C25 O6 C26 112.67(10) . . ? C27 O7 C10 111.44(10) . 2_556 ? C5 N1 C9 121.16(11) . . ? C5 N1 C4 119.07(10) . . ? C9 N1 C4 119.60(10) . . ? O2 C1 O1 123.88(12) . . ? O2 C1 C2 123.52(11) . . ? O1 C1 C2 112.59(10) . . ? C1 C2 C3 113.59(10) . . ? C2 C3 C4 110.66(10) . . ? N1 C4 C3 109.96(10) . . ? N1 C5 C6 120.74(11) . . ? C5 C6 C7 120.01(11) . . ? C6 C7 C8 117.83(11) . . ? C6 C7 C7 120.57(13) . 2_556 ? C8 C7 C7 121.60(13) . 2_556 ? C9 C8 C7 120.31(11) . . ? N1 C9 C8 119.94(11) . . ? O7 C10 C11 108.79(11) 2_556 . ? O3 C11 C10 106.82(12) . . ? O3 C12 C13 125.16(12) . . ? O3 C12 C21 113.77(11) . . ? C13 C12 C21 121.07(12) . . ? C12 C13 C14 119.44(12) . . ? C15 C14 C13 121.59(12) . . ? C14 C15 C16 119.74(12) . . ? C15 C16 C21 120.08(12) . . ? C15 C16 C17 121.57(11) . . ? C21 C16 C17 118.32(11) . . ? O4 C17 C18 125.20(12) . . ? O4 C17 C16 113.86(11) . . ? C18 C17 C16 120.94(12) . . ? C17 C18 C19 119.43(12) . . ? C20 C19 C18 121.76(12) . . ? C19 C20 C21 119.46(12) . . ? C16 C21 C20 120.01(12) . . ? C16 C21 C12 118.00(11) . . ? C20 C21 C12 121.97(12) . . ? O4 C22 C23 107.24(11) . . ? O5 C23 C22 109.20(11) . . ? O5 C24 C25 108.47(11) . . ? O6 C25 C24 109.57(10) . . ? O6 C26 C27 114.76(11) . . ? O7 C27 C26 108.55(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O2 0.95(2) 1.71(2) 2.6537(13) 174(2) 2_666 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.497 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.047 # Attachment 'Pecoraro-CIF_Ib.cif' data_Pseudorotaxane_Ib(gm11) _database_code_depnum_ccdc_archive 'CCDC 633581' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H44 O10, C18 H22 N2 O4, 2(P F6)' _chemical_formula_sum 'C54 H66 F12 N2 O14 P2' _chemical_formula_weight 1257.03 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.405(2) _cell_length_b 11.148(2) _cell_length_c 14.021(3) _cell_angle_alpha 69.539(3) _cell_angle_beta 81.494(3) _cell_angle_gamma 74.025(3) _cell_volume 1462.4(5) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6425 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 23.32 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 654 _exptl_absorpt_coefficient_mu 0.177 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9244 _exptl_absorpt_correction_T_max 0.9454 _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38. Sheldrick, G. SADABS (Version 2.10) Bruker/Siemens area detector absorption and other corrections, University of Gottingen, Germany 2003. ; _exptl_special_details ; 2735 frames x 25 sec. @ 4.969 cm; 0.5 deg. steps in omega & phi ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30954 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.32 _reflns_number_total 7233 _reflns_number_gt 5701 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0854P)^2^+1.6976P] 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 7233 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1782 _refine_ls_wR_factor_gt 0.1653 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.005 _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 P1 P -0.00683(6) 1.00942(5) 0.28107(5) 0.03050(16) Uani 1 1 d . . . F1 F 0.0941(2) 0.93186(17) 0.36992(15) 0.0600(5) Uani 1 1 d . . . F2 F 0.10432(17) 0.96448(15) 0.20070(14) 0.0509(4) Uani 1 1 d . . . F3 F -0.06053(16) 0.87950(13) 0.30460(11) 0.0406(3) Uani 1 1 d . . . F4 F -0.10886(16) 1.08663(14) 0.19264(12) 0.0427(4) Uani 1 1 d . . . F5 F -0.11973(19) 1.05624(16) 0.36028(13) 0.0511(4) Uani 1 1 d . . . F6 F 0.04509(16) 1.14025(14) 0.25772(13) 0.0450(4) Uani 1 1 d . . . O1 O 0.5228(3) 0.3255(3) 0.0788(2) 0.0772(8) Uani 1 1 d . . . H1 H 0.488(7) 0.416(6) 0.014(5) 0.08(2) Uiso 1 1 d . . . O2 O 0.5441(3) 0.5031(2) 0.10524(19) 0.0701(7) Uani 1 1 d . . . O3 O 0.6958(2) 0.7319(3) 0.05677(18) 0.0579(6) Uani 1 1 d . . . O4 O 0.5580(2) 0.8130(3) 0.2234(2) 0.0695(8) Uani 1 1 d . . . O5 O 0.57506(19) 0.79341(18) 0.42033(14) 0.0414(4) Uani 1 1 d . . . O6 O 0.81916(18) 0.43819(17) 0.80998(13) 0.0385(4) Uani 1 1 d . . . O7 O 1.0269(2) 0.3652(2) 0.93587(14) 0.0534(5) Uani 1 1 d . . . N1 N 0.84713(17) 0.42898(18) 0.32457(13) 0.0240(3) Uani 1 1 d . . . C1 C 0.5535(2) 0.3855(3) 0.1344(2) 0.0364(5) Uani 1 1 d . . . C2 C 0.5985(2) 0.2946(2) 0.23766(19) 0.0336(5) Uani 1 1 d . . . H2A H 0.6705 0.2193 0.2288 0.040 Uiso 1 1 calc R . . H2B H 0.5225 0.2591 0.2772 0.040 Uiso 1 1 calc R . . C3 C 0.6502(2) 0.3593(2) 0.29926(18) 0.0316(5) Uani 1 1 d . . . H3A H 0.5818 0.4394 0.3033 0.038 Uiso 1 1 calc R . . H3B H 0.6642 0.2975 0.3696 0.038 Uiso 1 1 calc R . . C4 C 0.7813(2) 0.3971(2) 0.25195(16) 0.0287(4) Uani 1 1 d . . . H4A H 0.8425 0.3231 0.2323 0.034 Uiso 1 1 calc R . . H4B H 0.7630 0.4746 0.1894 0.034 Uiso 1 1 calc R . . C5 C 0.8454(2) 0.5552(2) 0.31096(16) 0.0284(4) Uani 1 1 d . . . H5A H 0.8029 0.6241 0.2546 0.034 Uiso 1 1 calc R . . C6 C 0.9053(2) 0.5846(2) 0.37882(16) 0.0271(4) Uani 1 1 d . . . H6A H 0.9041 0.6738 0.3684 0.033 Uiso 1 1 calc R . . C7 C 0.96780(19) 0.48486(19) 0.46273(14) 0.0210(4) Uani 1 1 d . . . C8 C 0.9664(2) 0.3554(2) 0.47435(16) 0.0245(4) Uani 1 1 d . . . H8A H 1.0070 0.2847 0.5306 0.029 Uiso 1 1 calc R . . C9 C 0.9064(2) 0.3301(2) 0.40485(16) 0.0254(4) Uani 1 1 d . . . H9A H 0.9066 0.2417 0.4134 0.030 Uiso 1 1 calc R . . C10 C 0.8998(3) 0.6538(4) -0.0207(2) 0.0624(9) Uani 1 1 d . . . H10A H 0.8713 0.5723 -0.0107 0.075 Uiso 1 1 calc R . . H10B H 0.9590 0.6702 -0.0837 0.075 Uiso 1 1 calc R . . C11 C 0.7832(4) 0.7630(4) -0.0332(3) 0.0635(9) Uani 1 1 d . . . H11A H 0.8098 0.8450 -0.0418 0.076 Uiso 1 1 calc R . . H11B H 0.7370 0.7762 -0.0942 0.076 Uiso 1 1 calc R . . C12 C 0.5833(4) 0.8354(3) 0.0476(2) 0.0562(8) Uani 1 1 d . . . H12A H 0.5338 0.8465 -0.0113 0.067 Uiso 1 1 calc R . . H12B H 0.6103 0.9182 0.0354 0.067 Uiso 1 1 calc R . . C13 C 0.4973(3) 0.8081(3) 0.1408(2) 0.0498(7) Uani 1 1 d . . . H13A H 0.4101 0.8740 0.1300 0.060 Uiso 1 1 calc R . . H13B H 0.4803 0.7197 0.1576 0.060 Uiso 1 1 calc R . . C14 C 0.4936(3) 0.9179(3) 0.2581(2) 0.0434(6) Uani 1 1 d . . . H14A H 0.4018 0.9101 0.2854 0.052 Uiso 1 1 calc R . . H14B H 0.4869 1.0021 0.2012 0.052 Uiso 1 1 calc R . . C15 C 0.5723(3) 0.9165(2) 0.34066(19) 0.0387(5) Uani 1 1 d . . . H15A H 0.6644 0.9239 0.3141 0.046 Uiso 1 1 calc R . . H15B H 0.5286 0.9911 0.3663 0.046 Uiso 1 1 calc R . . C16 C 0.6401(2) 0.7686(2) 0.50535(17) 0.0310(5) Uani 1 1 d . . . C17 C 0.6791(2) 0.8615(2) 0.5306(2) 0.0359(5) Uani 1 1 d . . . H17A H 0.6642 0.9501 0.4862 0.043 Uiso 1 1 calc R . . C18 C 0.7415(2) 0.8242(2) 0.6229(2) 0.0349(5) Uani 1 1 d . . . H18A H 0.7678 0.8886 0.6405 0.042 Uiso 1 1 calc R . . C19 C 0.7648(2) 0.6970(2) 0.68737(18) 0.0306(5) Uani 1 1 d . . . H19A H 0.8048 0.6741 0.7500 0.037 Uiso 1 1 calc R . . C20 C 0.7292(2) 0.5990(2) 0.66078(17) 0.0268(4) Uani 1 1 d . . . C21 C 0.7601(2) 0.4632(2) 0.72211(17) 0.0295(4) Uani 1 1 d . . . C22 C 0.7321(2) 0.3687(2) 0.69171(18) 0.0323(5) Uani 1 1 d . . . H22A H 0.7563 0.2783 0.7320 0.039 Uiso 1 1 calc R . . C23 C 0.6673(2) 0.4067(2) 0.60068(18) 0.0304(5) Uani 1 1 d . . . H23A H 0.6461 0.3412 0.5810 0.037 Uiso 1 1 calc R . . C24 C 0.6342(2) 0.5354(2) 0.54007(17) 0.0284(4) Uani 1 1 d . . . H24A H 0.5901 0.5592 0.4791 0.034 Uiso 1 1 calc R . . C25 C 0.6662(2) 0.6340(2) 0.56875(17) 0.0266(4) Uani 1 1 d . . . C26 C 0.8662(3) 0.3025(3) 0.8699(2) 0.0457(6) Uani 1 1 d . . . H26A H 0.9368 0.2564 0.8304 0.055 Uiso 1 1 calc R . . H26B H 0.7917 0.2577 0.8888 0.055 Uiso 1 1 calc R . . C27 C 0.9214(3) 0.2994(3) 0.9638(2) 0.0511(7) Uani 1 1 d . . . H27A H 0.8497 0.3431 1.0040 0.061 Uiso 1 1 calc R . . H27B H 0.9553 0.2067 1.0067 0.061 Uiso 1 1 calc R . . Q1 C 0.7883(12) 0.6368(12) -0.0036(9) 0.048(3) Uiso 0.25 1 d P . . Q2 C 0.6956(14) 0.6548(15) 0.0800(11) 0.052(3) Uiso 0.25 1 d P . . 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 P1 0.0385(3) 0.0203(3) 0.0334(3) -0.0062(2) -0.0051(2) -0.0099(2) F1 0.0741(12) 0.0424(9) 0.0636(11) 0.0020(8) -0.0386(10) -0.0209(8) F2 0.0501(9) 0.0337(8) 0.0640(11) -0.0180(8) 0.0129(8) -0.0079(7) F3 0.0568(9) 0.0246(6) 0.0432(8) -0.0054(6) -0.0083(7) -0.0189(6) F4 0.0487(9) 0.0329(7) 0.0409(8) -0.0031(6) -0.0124(7) -0.0072(6) F5 0.0702(11) 0.0441(9) 0.0454(9) -0.0217(7) 0.0148(8) -0.0240(8) F6 0.0524(9) 0.0271(7) 0.0593(10) -0.0114(7) -0.0045(7) -0.0185(6) O1 0.119(2) 0.0529(14) 0.0726(17) -0.0262(13) -0.0495(16) -0.0116(14) O2 0.109(2) 0.0465(12) 0.0658(15) -0.0192(11) -0.0459(14) -0.0129(13) O3 0.0533(13) 0.0743(17) 0.0499(13) -0.0265(12) 0.0039(10) -0.0165(12) O4 0.0600(13) 0.0811(17) 0.0712(15) -0.0507(14) -0.0305(12) 0.0248(12) O5 0.0504(10) 0.0368(9) 0.0356(9) -0.0009(7) -0.0147(8) -0.0163(8) O6 0.0461(10) 0.0362(9) 0.0329(9) -0.0099(7) -0.0108(7) -0.0066(7) O7 0.0467(11) 0.0832(16) 0.0287(9) -0.0142(10) -0.0063(8) -0.0162(10) N1 0.0239(8) 0.0298(9) 0.0222(8) -0.0118(7) 0.0017(6) -0.0096(7) C1 0.0313(11) 0.0388(13) 0.0467(14) -0.0228(11) -0.0092(10) -0.0051(9) C2 0.0265(10) 0.0398(12) 0.0406(13) -0.0195(11) -0.0043(9) -0.0082(9) C3 0.0258(10) 0.0424(12) 0.0327(11) -0.0193(10) -0.0006(8) -0.0092(9) C4 0.0303(10) 0.0372(11) 0.0255(10) -0.0164(9) -0.0016(8) -0.0111(9) C5 0.0344(11) 0.0272(10) 0.0241(10) -0.0047(8) -0.0034(8) -0.0119(9) C6 0.0353(11) 0.0229(9) 0.0241(10) -0.0041(8) -0.0029(8) -0.0127(8) C7 0.0213(8) 0.0230(9) 0.0206(9) -0.0082(7) 0.0020(7) -0.0086(7) C8 0.0254(9) 0.0214(9) 0.0272(10) -0.0088(8) -0.0025(8) -0.0046(7) C9 0.0266(10) 0.0227(9) 0.0297(10) -0.0119(8) -0.0018(8) -0.0059(8) C10 0.0476(17) 0.102(3) 0.0365(15) -0.0291(17) -0.0083(12) -0.0041(17) C11 0.069(2) 0.074(2) 0.0450(17) -0.0142(16) -0.0060(15) -0.0188(18) C12 0.0650(19) 0.0575(18) 0.0448(16) -0.0042(14) -0.0175(14) -0.0214(15) C13 0.0459(15) 0.0548(17) 0.0502(16) -0.0225(14) -0.0138(13) -0.0017(13) C14 0.0482(15) 0.0366(13) 0.0356(13) -0.0071(11) -0.0085(11) 0.0023(11) C15 0.0447(13) 0.0292(11) 0.0357(12) -0.0059(10) -0.0031(10) -0.0041(10) C16 0.0286(10) 0.0336(11) 0.0313(11) -0.0093(9) -0.0012(9) -0.0098(9) C17 0.0350(12) 0.0296(11) 0.0434(13) -0.0108(10) -0.0013(10) -0.0101(9) C18 0.0312(11) 0.0345(12) 0.0459(13) -0.0205(11) -0.0005(10) -0.0101(9) C19 0.0258(10) 0.0381(12) 0.0345(11) -0.0194(10) 0.0004(8) -0.0092(9) C20 0.0210(9) 0.0320(11) 0.0294(10) -0.0134(9) 0.0028(8) -0.0070(8) C21 0.0251(10) 0.0345(11) 0.0286(10) -0.0107(9) 0.0007(8) -0.0073(8) C22 0.0310(11) 0.0290(11) 0.0360(12) -0.0091(9) 0.0014(9) -0.0094(9) C23 0.0259(10) 0.0336(11) 0.0377(12) -0.0172(10) 0.0041(9) -0.0122(9) C24 0.0226(9) 0.0345(11) 0.0312(11) -0.0136(9) 0.0005(8) -0.0094(8) C25 0.0205(9) 0.0306(10) 0.0300(10) -0.0120(9) 0.0018(8) -0.0072(8) C26 0.0559(16) 0.0394(14) 0.0367(13) -0.0034(11) -0.0096(12) -0.0115(12) C27 0.0605(18) 0.0558(17) 0.0285(12) -0.0023(12) -0.0065(12) -0.0136(14) _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 P1 F1 1.5925(17) . ? P1 F4 1.5954(16) . ? P1 F2 1.5964(17) . ? P1 F5 1.6023(17) . ? P1 F6 1.6043(15) . ? P1 F3 1.6048(14) . ? O1 C1 1.308(3) . ? O2 C1 1.210(3) . ? O3 C12 1.384(4) . ? O3 C11 1.437(4) . ? O4 C14 1.388(3) . ? O4 C13 1.422(3) . ? O5 C16 1.364(3) . ? O5 C15 1.431(3) . ? O6 C21 1.365(3) . ? O6 C26 1.435(3) . ? O7 C27 1.418(4) . ? O7 C10 1.431(3) 2_766 ? N1 C5 1.348(3) . ? N1 C9 1.351(3) . ? N1 C4 1.492(3) . ? C1 C2 1.502(4) . ? C2 C3 1.530(3) . ? C3 C4 1.527(3) . ? C5 C6 1.381(3) . ? C6 C7 1.399(3) . ? C7 C8 1.398(3) . ? C7 C7 1.494(4) 2_766 ? C8 C9 1.374(3) . ? C10 O7 1.431(3) 2_766 ? C10 C11 1.444(5) . ? C12 C13 1.459(5) . ? C14 C15 1.506(4) . ? C16 C17 1.375(3) . ? C16 C25 1.425(3) . ? C17 C18 1.412(4) . ? C18 C19 1.366(4) . ? C19 C20 1.421(3) . ? C20 C25 1.416(3) . ? C20 C21 1.428(3) . ? C21 C22 1.377(3) . ? C22 C23 1.408(3) . ? C23 C24 1.365(3) . ? C24 C25 1.424(3) . ? C26 C27 1.499(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 F1 P1 F4 179.54(11) . . ? F1 P1 F2 90.35(11) . . ? F4 P1 F2 89.97(10) . . ? F1 P1 F5 90.52(11) . . ? F4 P1 F5 89.16(10) . . ? F2 P1 F5 179.10(11) . . ? F1 P1 F6 90.58(9) . . ? F4 P1 F6 89.75(9) . . ? F2 P1 F6 90.23(9) . . ? F5 P1 F6 89.53(9) . . ? F1 P1 F3 89.80(9) . . ? F4 P1 F3 89.87(8) . . ? F2 P1 F3 90.32(9) . . ? F5 P1 F3 89.92(9) . . ? F6 P1 F3 179.33(9) . . ? C12 O3 C11 109.0(3) . . ? C14 O4 C13 114.2(2) . . ? C16 O5 C15 117.79(19) . . ? C21 O6 C26 117.2(2) . . ? C27 O7 C10 112.9(2) . 2_766 ? C5 N1 C9 120.54(18) . . ? C5 N1 C4 120.23(18) . . ? C9 N1 C4 119.22(18) . . ? O2 C1 O1 122.7(3) . . ? O2 C1 C2 123.8(2) . . ? O1 C1 C2 113.5(2) . . ? C1 C2 C3 114.4(2) . . ? C4 C3 C2 112.08(18) . . ? N1 C4 C3 111.30(17) . . ? N1 C5 C6 120.1(2) . . ? C5 C6 C7 120.95(19) . . ? C8 C7 C6 117.02(18) . . ? C8 C7 C7 121.4(2) . 2_766 ? C6 C7 C7 121.6(2) . 2_766 ? C9 C8 C7 120.30(19) . . ? N1 C9 C8 121.06(19) . . ? O7 C10 C11 112.1(3) 2_766 . ? O3 C11 C10 107.6(3) . . ? O3 C12 C13 109.5(3) . . ? O4 C13 C12 110.8(3) . . ? O4 C14 C15 108.9(2) . . ? O5 C15 C14 106.4(2) . . ? O5 C16 C17 125.0(2) . . ? O5 C16 C25 113.7(2) . . ? C17 C16 C25 121.2(2) . . ? C16 C17 C18 119.6(2) . . ? C19 C18 C17 121.1(2) . . ? C18 C19 C20 120.0(2) . . ? C25 C20 C19 119.9(2) . . ? C25 C20 C21 117.93(19) . . ? C19 C20 C21 122.1(2) . . ? O6 C21 C22 124.7(2) . . ? O6 C21 C20 114.18(19) . . ? C22 C21 C20 121.1(2) . . ? C21 C22 C23 119.7(2) . . ? C24 C23 C22 121.4(2) . . ? C23 C24 C25 119.6(2) . . ? C20 C25 C24 120.2(2) . . ? C20 C25 C16 118.1(2) . . ? C24 C25 C16 121.7(2) . . ? O6 C26 C27 107.7(2) . . ? O7 C27 C26 109.7(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O2 1.11(7) 1.63(7) 2.674(4) 154(5) 2_665 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.685 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.070 # Attachment 'Pecoraro-CIF_Ic.cif' data_Pseudorotaxane_Ic(gm13) _database_code_depnum_ccdc_archive 'CCDC 633582' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C36 H44 O10, C18 H22 N2 O4, 2(F6 P), 4(C2 H3 N) ; _chemical_formula_sum 'C62 H78 F12 N6 O14 P2' _chemical_formula_weight 1421.24 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7067(11) _cell_length_b 12.1212(11) _cell_length_c 13.9127(13) _cell_angle_alpha 94.769(6) _cell_angle_beta 110.295(6) _cell_angle_gamma 109.052(6) _cell_volume 1706.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5755 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.07 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 742 _exptl_absorpt_coefficient_mu 0.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9651 _exptl_absorpt_correction_T_max 0.9871 _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38. Sheldrick, G. SADABS (Version 2.10) Bruker/Siemens area detector absorption and other corrections, University of Gottingen, Germany 2003. ; _exptl_special_details ; 2875 frames x 45 sec. @ 4.969 cm; 0.5 deg. steps in omega & phi ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32530 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.41 _reflns_number_total 6965 _reflns_number_gt 4452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART-1K' _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' _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^)+(0.0478P)^2^+0.9117P] 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 6965 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0953 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1261 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 P1 P 0.66958(7) 0.36237(7) 0.50495(5) 0.0376(2) Uani 1 1 d . . . F1 F 0.63352(18) 0.23907(15) 0.42939(12) 0.0566(5) Uani 1 1 d . . . F2 F 0.58623(19) 0.29328(16) 0.56627(14) 0.0620(5) Uani 1 1 d . . . F3 F 0.75417(19) 0.43093(17) 0.44418(14) 0.0691(6) Uani 1 1 d . . . F4 F 0.54413(19) 0.3777(2) 0.42525(14) 0.0726(6) Uani 1 1 d . . . F5 F 0.79390(19) 0.3428(2) 0.58429(14) 0.0841(7) Uani 1 1 d . . . F6 F 0.7080(2) 0.48639(16) 0.58092(14) 0.0733(6) Uani 1 1 d . . . N1 N 0.91499(18) 0.39799(17) 0.20391(15) 0.0258(5) Uani 1 1 d . . . N2 N 0.1964(3) 0.8647(2) 0.19287(19) 0.0482(6) Uani 1 1 d . . . N3 N 0.6969(3) 0.8936(3) 0.3914(2) 0.0753(9) Uani 1 1 d . . . O1 O 0.9677(2) 0.12287(19) 0.55509(14) 0.0456(5) Uani 1 1 d . . . H1 H 0.990(3) 0.053(3) 0.573(3) 0.085(12) Uiso 1 1 d . . . O2 O 0.99805(19) 0.07772(17) 0.40746(14) 0.0419(5) Uani 1 1 d . . . O3 O 0.74001(15) 0.03117(13) 0.08103(12) 0.0260(4) Uani 1 1 d . . . O4 O 0.61198(15) 0.11707(13) 0.18989(12) 0.0265(4) Uani 1 1 d . . . O5 O 0.55644(16) 0.29899(14) 0.09535(12) 0.0281(4) Uani 1 1 d . . . O6 O 0.76819(15) 0.67616(13) -0.11783(12) 0.0250(4) Uani 1 1 d . . . O7 O 0.97554(15) 0.86374(14) -0.13689(13) 0.0281(4) Uani 1 1 d . . . C1 C 0.9673(3) 0.1390(2) 0.4613(2) 0.0365(6) Uani 1 1 d . . . C2 C 0.9229(3) 0.2361(3) 0.4276(2) 0.0399(7) Uani 1 1 d . . . H2A H 0.9581 0.3022 0.4896 0.048 Uiso 1 1 calc R . . H2B H 0.8256 0.2053 0.4007 0.048 Uiso 1 1 calc R . . C3 C 0.9654(3) 0.2853(2) 0.3433(2) 0.0341(6) Uani 1 1 d . . . H3A H 1.0594 0.3395 0.3752 0.041 Uiso 1 1 calc R . . H3B H 0.9549 0.2187 0.2904 0.041 Uiso 1 1 calc R . . C4 C 0.8821(2) 0.3529(2) 0.2909(2) 0.0314(6) Uani 1 1 d . . . H4A H 0.7880 0.2994 0.2628 0.038 Uiso 1 1 calc R . . H4B H 0.8961 0.4212 0.3437 0.038 Uiso 1 1 calc R . . C5 C 0.8816(2) 0.3187(2) 0.11521(19) 0.0284(6) Uani 1 1 d . . . H5A H 0.8350 0.2360 0.1085 0.034 Uiso 1 1 calc R . . C6 C 0.9146(2) 0.3565(2) 0.03464(19) 0.0288(6) Uani 1 1 d . . . H6A H 0.8917 0.2998 -0.0270 0.035 Uiso 1 1 calc R . . C7 C 0.9818(2) 0.4785(2) 0.04291(17) 0.0241(5) Uani 1 1 d . . . C8 C 1.0118(2) 0.5576(2) 0.13515(19) 0.0313(6) Uani 1 1 d . . . H8A H 1.0560 0.6410 0.1433 0.038 Uiso 1 1 calc R . . C9 C 0.9781(2) 0.5159(2) 0.2137(2) 0.0314(6) Uani 1 1 d . . . H9A H 0.9994 0.5708 0.2760 0.038 Uiso 1 1 calc R . . C10 C 0.8157(2) -0.0174(2) 0.04201(19) 0.0292(6) Uani 1 1 d . . . H10A H 0.8199 0.0135 -0.0208 0.035 Uiso 1 1 calc R . . H10B H 0.7692 -0.1055 0.0194 0.035 Uiso 1 1 calc R . . C11 C 0.7021(2) -0.0260(2) 0.15742(19) 0.0295(6) Uani 1 1 d . . . H11A H 0.7746 0.0087 0.2279 0.035 Uiso 1 1 calc R . . H11B H 0.6832 -0.1127 0.1397 0.035 Uiso 1 1 calc R . . C12 C 0.5809(2) -0.0075(2) 0.15765(19) 0.0270(5) Uani 1 1 d . . . H12A H 0.5098 -0.0392 0.0863 0.032 Uiso 1 1 calc R . . H12B H 0.5496 -0.0511 0.2064 0.032 Uiso 1 1 calc R . . C13 C 0.4971(2) 0.1414(2) 0.17895(19) 0.0272(5) Uani 1 1 d . . . H13A H 0.4677 0.1167 0.2353 0.033 Uiso 1 1 calc R . . H13B H 0.4249 0.0955 0.1103 0.033 Uiso 1 1 calc R . . C14 C 0.5293(2) 0.2733(2) 0.18596(18) 0.0264(5) Uani 1 1 d . . . H14A H 0.4539 0.2937 0.1858 0.032 Uiso 1 1 calc R . . H14B H 0.6070 0.3202 0.2513 0.032 Uiso 1 1 calc R . . C15 C 0.6151(2) 0.4161(2) 0.09226(17) 0.0228(5) Uani 1 1 d . . . C16 C 0.6539(2) 0.5134(2) 0.17104(18) 0.0273(6) Uani 1 1 d . . . H16A H 0.6380 0.5030 0.2328 0.033 Uiso 1 1 calc R . . C17 C 0.7176(2) 0.6289(2) 0.15899(19) 0.0289(6) Uani 1 1 d . . . H17A H 0.7463 0.6961 0.2140 0.035 Uiso 1 1 calc R . . C18 C 0.7391(2) 0.6464(2) 0.06982(18) 0.0254(5) Uani 1 1 d . . . H18A H 0.7826 0.7251 0.0638 0.031 Uiso 1 1 calc R . . C19 C 0.6967(2) 0.5474(2) -0.01369(17) 0.0218(5) Uani 1 1 d . . . C20 C 0.7119(2) 0.5598(2) -0.11066(17) 0.0221(5) Uani 1 1 d . . . C21 C 0.6721(2) 0.4611(2) -0.18860(18) 0.0264(5) Uani 1 1 d . . . H21A H 0.6831 0.4709 -0.2523 0.032 Uiso 1 1 calc R . . C22 C 0.6150(2) 0.3457(2) -0.17373(18) 0.0267(5) Uani 1 1 d . . . H22A H 0.5890 0.2779 -0.2274 0.032 Uiso 1 1 calc R . . C23 C 0.5962(2) 0.3292(2) -0.08349(17) 0.0248(5) Uani 1 1 d . . . H23A H 0.5571 0.2506 -0.0751 0.030 Uiso 1 1 calc R . . C24 C 0.6351(2) 0.4294(2) -0.00227(17) 0.0209(5) Uani 1 1 d . . . C25 C 0.7774(2) 0.6929(2) -0.21654(17) 0.0258(5) Uani 1 1 d . . . H25A H 0.6884 0.6601 -0.2740 0.031 Uiso 1 1 calc R . . H25B H 0.8304 0.6505 -0.2323 0.031 Uiso 1 1 calc R . . C26 C 0.8414(2) 0.8241(2) -0.20813(18) 0.0268(5) Uani 1 1 d . . . H26A H 0.8361 0.8397 -0.2780 0.032 Uiso 1 1 calc R . . H26B H 0.7959 0.8678 -0.1821 0.032 Uiso 1 1 calc R . . C27 C 1.0458(2) 0.9892(2) -0.11976(19) 0.0272(5) Uani 1 1 d . . . H27A H 1.0036 1.0346 -0.0913 0.033 Uiso 1 1 calc R . . H27B H 1.0466 1.0111 -0.1866 0.033 Uiso 1 1 calc R . . C28 C 0.2597(3) 0.9052(2) 0.2792(2) 0.0399(7) Uani 1 1 d . . . C29 C 0.3407(4) 0.9577(3) 0.3899(2) 0.0756(12) Uani 1 1 d . . . H29A H 0.3784 1.0450 0.4007 0.113 Uiso 1 1 calc R . . H29B H 0.4118 0.9277 0.4131 0.113 Uiso 1 1 calc R . . H29C H 0.2865 0.9357 0.4307 0.113 Uiso 1 1 calc R . . C30 C 0.6869(3) 0.8018(3) 0.4110(2) 0.0484(8) Uani 1 1 d . . . C31 C 0.6728(3) 0.6845(3) 0.4344(2) 0.0539(8) Uani 1 1 d . . . H31A H 0.5896 0.6243 0.3828 0.081 Uiso 1 1 calc R . . H31B H 0.6731 0.6855 0.5050 0.081 Uiso 1 1 calc R . . H31C H 0.7463 0.6645 0.4312 0.081 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 P1 0.0369(4) 0.0520(5) 0.0239(3) 0.0020(3) 0.0128(3) 0.0176(4) F1 0.0723(12) 0.0599(11) 0.0362(9) -0.0011(8) 0.0186(9) 0.0295(10) F2 0.0771(13) 0.0666(12) 0.0592(11) 0.0190(9) 0.0459(11) 0.0265(10) F3 0.0781(14) 0.0735(13) 0.0541(11) -0.0008(10) 0.0474(11) 0.0078(11) F4 0.0647(13) 0.1127(17) 0.0597(12) 0.0287(11) 0.0208(10) 0.0593(13) F5 0.0569(13) 0.137(2) 0.0422(11) 0.0045(12) -0.0033(10) 0.0459(13) F6 0.1222(18) 0.0551(12) 0.0483(11) -0.0001(9) 0.0554(12) 0.0204(11) N1 0.0194(11) 0.0258(11) 0.0309(11) 0.0056(9) 0.0075(9) 0.0099(9) N2 0.0593(17) 0.0314(13) 0.0413(15) 0.0037(11) 0.0089(13) 0.0148(12) N3 0.070(2) 0.068(2) 0.0615(19) 0.0237(17) 0.0115(16) 0.0074(17) O1 0.0637(14) 0.0489(13) 0.0361(11) 0.0208(10) 0.0247(10) 0.0281(11) O2 0.0510(12) 0.0502(12) 0.0380(10) 0.0182(9) 0.0239(10) 0.0271(10) O3 0.0281(9) 0.0222(9) 0.0311(9) 0.0088(7) 0.0144(8) 0.0103(7) O4 0.0227(9) 0.0226(9) 0.0324(9) 0.0055(7) 0.0098(7) 0.0078(7) O5 0.0374(10) 0.0238(9) 0.0231(8) 0.0068(7) 0.0133(8) 0.0099(8) O6 0.0286(9) 0.0235(9) 0.0224(8) 0.0051(7) 0.0127(7) 0.0068(7) O7 0.0221(9) 0.0224(9) 0.0362(9) 0.0091(7) 0.0087(8) 0.0065(7) C1 0.0328(15) 0.0435(17) 0.0326(15) 0.0136(13) 0.0133(12) 0.0120(13) C2 0.0428(17) 0.0479(17) 0.0404(16) 0.0172(13) 0.0220(14) 0.0236(14) C3 0.0298(14) 0.0413(16) 0.0378(15) 0.0162(12) 0.0169(12) 0.0161(12) C4 0.0282(14) 0.0309(14) 0.0379(14) 0.0088(12) 0.0169(12) 0.0105(11) C5 0.0266(14) 0.0227(13) 0.0320(13) 0.0033(11) 0.0069(11) 0.0101(11) C6 0.0303(14) 0.0227(13) 0.0295(13) 0.0012(11) 0.0069(11) 0.0117(11) C7 0.0173(12) 0.0208(12) 0.0283(13) 0.0037(10) 0.0027(10) 0.0072(10) C8 0.0318(15) 0.0187(13) 0.0356(14) 0.0010(11) 0.0126(12) 0.0020(11) C9 0.0293(14) 0.0227(13) 0.0335(14) -0.0025(11) 0.0102(12) 0.0037(11) C10 0.0303(14) 0.0230(13) 0.0330(13) 0.0032(11) 0.0127(12) 0.0089(11) C11 0.0328(15) 0.0234(13) 0.0330(14) 0.0104(11) 0.0140(12) 0.0094(11) C12 0.0267(13) 0.0188(12) 0.0339(13) 0.0080(10) 0.0131(11) 0.0050(10) C13 0.0254(13) 0.0307(14) 0.0266(13) 0.0083(11) 0.0120(11) 0.0098(11) C14 0.0259(13) 0.0314(14) 0.0265(12) 0.0082(11) 0.0132(11) 0.0132(11) C15 0.0222(13) 0.0223(13) 0.0256(12) 0.0076(10) 0.0078(10) 0.0116(10) C16 0.0344(14) 0.0295(14) 0.0231(12) 0.0061(10) 0.0131(11) 0.0166(12) C17 0.0370(15) 0.0234(13) 0.0269(13) 0.0016(10) 0.0120(11) 0.0139(11) C18 0.0313(14) 0.0197(12) 0.0283(13) 0.0053(10) 0.0133(11) 0.0118(11) C19 0.0186(12) 0.0237(13) 0.0229(12) 0.0033(10) 0.0060(10) 0.0107(10) C20 0.0186(12) 0.0227(12) 0.0263(12) 0.0062(10) 0.0099(10) 0.0079(10) C21 0.0266(13) 0.0292(14) 0.0218(12) 0.0030(10) 0.0103(11) 0.0084(11) C22 0.0254(13) 0.0241(13) 0.0246(12) -0.0030(10) 0.0078(11) 0.0066(11) C23 0.0240(13) 0.0210(12) 0.0239(12) 0.0019(10) 0.0063(10) 0.0061(10) C24 0.0173(12) 0.0244(13) 0.0198(11) 0.0037(10) 0.0044(10) 0.0099(10) C25 0.0251(13) 0.0305(14) 0.0229(12) 0.0057(10) 0.0122(11) 0.0090(11) C26 0.0228(13) 0.0308(14) 0.0286(13) 0.0092(11) 0.0113(11) 0.0105(11) C27 0.0295(14) 0.0231(13) 0.0326(13) 0.0104(11) 0.0147(11) 0.0109(11) C28 0.0460(18) 0.0257(14) 0.0421(17) 0.0106(13) 0.0112(14) 0.0123(13) C29 0.089(3) 0.058(2) 0.0367(18) 0.0063(16) -0.0016(18) 0.004(2) C30 0.0387(18) 0.058(2) 0.0394(17) 0.0075(16) 0.0132(14) 0.0100(16) C31 0.050(2) 0.061(2) 0.0539(19) 0.0095(16) 0.0193(16) 0.0267(17) _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 P1 F4 1.5825(19) . ? P1 F1 1.5926(17) . ? P1 F6 1.5949(18) . ? P1 F2 1.5950(18) . ? P1 F3 1.5958(18) . ? P1 F5 1.596(2) . ? N1 C9 1.348(3) . ? N1 C5 1.350(3) . ? N1 C4 1.485(3) . ? N2 C28 1.131(3) . ? N3 C30 1.146(4) . ? O1 C1 1.335(3) . ? O2 C1 1.229(3) . ? O3 C10 1.431(3) . ? O3 C11 1.434(3) . ? O4 C12 1.424(3) . ? O4 C13 1.430(3) . ? O5 C15 1.372(3) . ? O5 C14 1.437(3) . ? O6 C20 1.377(3) . ? O6 C25 1.440(3) . ? O7 C26 1.424(3) . ? O7 C27 1.426(3) . ? C1 C2 1.481(4) . ? C2 C3 1.520(3) . ? C3 C4 1.510(3) . ? C5 C6 1.373(3) . ? C6 C7 1.403(3) . ? C7 C8 1.397(3) . ? C7 C7 1.480(5) 2_765 ? C8 C9 1.366(3) . ? C10 C27 1.509(3) 2_765 ? C11 C12 1.508(3) . ? C13 C14 1.505(3) . ? C15 C16 1.374(3) . ? C15 C24 1.426(3) . ? C16 C17 1.410(3) . ? C17 C18 1.369(3) . ? C18 C19 1.420(3) . ? C19 C24 1.426(3) . ? C19 C20 1.434(3) . ? C20 C21 1.376(3) . ? C21 C22 1.407(3) . ? C22 C23 1.367(3) . ? C23 C24 1.419(3) . ? C25 C26 1.496(3) . ? C27 C10 1.509(3) 2_765 ? C28 C29 1.451(4) . ? C30 C31 1.455(5) . ? 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 F4 P1 F1 90.07(11) . . ? F4 P1 F6 90.58(12) . . ? F1 P1 F6 179.13(11) . . ? F4 P1 F2 90.96(11) . . ? F1 P1 F2 90.51(10) . . ? F6 P1 F2 90.06(10) . . ? F4 P1 F3 89.64(11) . . ? F1 P1 F3 89.29(10) . . ? F6 P1 F3 90.13(10) . . ? F2 P1 F3 179.37(12) . . ? F4 P1 F5 178.36(13) . . ? F1 P1 F5 88.52(11) . . ? F6 P1 F5 90.83(12) . . ? F2 P1 F5 88.22(11) . . ? F3 P1 F5 91.18(12) . . ? C9 N1 C5 120.5(2) . . ? C9 N1 C4 120.6(2) . . ? C5 N1 C4 118.9(2) . . ? C10 O3 C11 114.05(17) . . ? C12 O4 C13 111.67(17) . . ? C15 O5 C14 118.87(17) . . ? C20 O6 C25 116.38(17) . . ? C26 O7 C27 113.25(17) . . ? O2 C1 O1 123.2(2) . . ? O2 C1 C2 123.6(2) . . ? O1 C1 C2 113.2(2) . . ? C1 C2 C3 113.8(2) . . ? C4 C3 C2 109.3(2) . . ? N1 C4 C3 111.69(19) . . ? N1 C5 C6 120.5(2) . . ? C5 C6 C7 120.3(2) . . ? C8 C7 C6 117.1(2) . . ? C8 C7 C7 121.5(3) . 2_765 ? C6 C7 C7 121.4(3) . 2_765 ? C9 C8 C7 120.6(2) . . ? N1 C9 C8 120.8(2) . . ? O3 C10 C27 114.71(19) . 2_765 ? O3 C11 C12 108.68(19) . . ? O4 C12 C11 109.27(18) . . ? O4 C13 C14 108.96(19) . . ? O5 C14 C13 106.35(18) . . ? O5 C15 C16 125.1(2) . . ? O5 C15 C24 113.32(19) . . ? C16 C15 C24 121.6(2) . . ? C15 C16 C17 119.1(2) . . ? C18 C17 C16 121.6(2) . . ? C17 C18 C19 120.3(2) . . ? C18 C19 C24 119.3(2) . . ? C18 C19 C20 123.1(2) . . ? C24 C19 C20 117.60(19) . . ? C21 C20 O6 124.2(2) . . ? C21 C20 C19 121.2(2) . . ? O6 C20 C19 114.62(18) . . ? C20 C21 C22 119.8(2) . . ? C23 C22 C21 121.3(2) . . ? C22 C23 C24 120.1(2) . . ? C23 C24 C15 121.8(2) . . ? C23 C24 C19 120.0(2) . . ? C15 C24 C19 118.21(19) . . ? O6 C25 C26 108.10(18) . . ? O7 C26 C25 108.23(18) . . ? O7 C27 C10 106.98(18) . 2_765 ? N2 C28 C29 179.8(4) . . ? N3 C30 C31 179.3(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O2 0.99(4) 1.67(4) 2.654(3) 171(3) 2_756 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.370 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.052