# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global #TrackingRef '- CC-Supracryptand-ESI-02.cif' _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- CC-Supracryptand-ESI-02.cif' _journal_year 2011 _journal_page_first ? _publ_contact_author_name 'Feihe Huang' _publ_contact_author_address ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; _publ_contact_author_email fhuang@zju.edu.cn _publ_contact_author_fax 86-571-87953189 _publ_contact_author_phone 86-571-87953189 _publ_section_title ; pH-responsive Assembly and Disassembly of a Supramolecular Cryptand-based Pseudorotaxane Driven by p-p Stacking Interactions ; loop_ _publ_author_name _publ_author_address 'Xuzhou Yan' ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; 'Mingming Zhang' ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; 'Peifa Wei' ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; 'Bo Zheng' ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; 'Xiaodong Chi' ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; 'Xiaofan Ji' ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; 'Feihe Huang' ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; #===END data_110331_xz_229a #TrackingRef '- CC-Supracryptand-ESI-02.cif' _database_code_depnum_ccdc_archive 'CCDC 829263' #TrackingRef '- CC-Supracryptand-ESI-02.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H50 N2 O14, C12 H12 N2, 2(F6 P)' _chemical_formula_sum 'C54 H62 F12 N4 O14 P2' _chemical_formula_weight 1281.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 10.8701(3) _cell_length_b 22.6954(6) _cell_length_c 22.8977(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.794(3) _cell_angle_gamma 90.00 _cell_volume 5549.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13753 _cell_measurement_theta_min 3.8922 _cell_measurement_theta_max 66.5546 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 1.700 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6476 _exptl_absorpt_correction_T_max 0.7495 _exptl_absorpt_process_details ; CrysAlis PRO (Oxford Diffraction, 2010) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3592 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31682 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.90 _diffrn_reflns_theta_max 66.66 _reflns_number_total 9701 _reflns_number_gt 8046 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'CrysAlis PRO (Oxford Diffraction, 2010)' _computing_data_collection 'CrysAlis PRO' _computing_data_reduction 'CrysAlis PRO' _computing_molecular_graphics 'OLEX2 (Dolomanov et al., 2009)' _computing_publication_material OLEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0724P)^2^+2.6672P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9701 _refine_ls_number_parameters 775 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1325 _refine_ls_wR_factor_gt 0.1224 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 0.78636(5) 0.20700(3) 0.51788(3) 0.02552(15) Uani 1 1 d . . . P2 P 0.25403(5) 0.21090(2) 0.44340(3) 0.02287(15) Uani 1 1 d . . . F1 F 0.81256(17) 0.18253(9) 0.58381(7) 0.0511(5) Uani 1 1 d . . . F2 F 0.65470(16) 0.23167(9) 0.52639(12) 0.0722(7) Uani 1 1 d . . . F3 F 0.7595(2) 0.23113(9) 0.45107(8) 0.0670(6) Uani 1 1 d . . . F4 F 0.91673(14) 0.18224(8) 0.50871(8) 0.0490(4) Uani 1 1 d . . . F5 F 0.85060(15) 0.26805(7) 0.54081(8) 0.0456(4) Uani 1 1 d . . . F6 F 0.72030(13) 0.14576(6) 0.49486(6) 0.0313(3) Uani 1 1 d . . . F7 F 0.39647(13) 0.21718(7) 0.47804(7) 0.0377(4) Uani 1 1 d . . . F8 F 0.30085(15) 0.22062(8) 0.38139(7) 0.0423(4) Uani 1 1 d . . . F9 F 0.27618(16) 0.14173(6) 0.43807(7) 0.0392(4) Uani 1 1 d . . . F10 F 0.21053(15) 0.20114(7) 0.50535(7) 0.0393(4) Uani 1 1 d . . . F11 F 0.23598(14) 0.28003(6) 0.44885(8) 0.0406(4) Uani 1 1 d . . . F12 F 0.11475(14) 0.20400(7) 0.40812(8) 0.0405(4) Uani 1 1 d . . . O1 O 0.9725(2) 0.03787(10) 0.05869(10) 0.0517(5) Uani 1 1 d . . . O2 O 0.8685(2) 0.03290(8) 0.13332(9) 0.0442(5) Uani 1 1 d . . . O3 O 0.89697(15) 0.07105(7) 0.34200(7) 0.0260(4) Uani 1 1 d . . . O4 O 0.78519(14) 0.00657(7) 0.41922(7) 0.0246(3) Uani 1 1 d . . . O5 O 0.55402(14) -0.04478(7) 0.42858(7) 0.0235(3) Uani 1 1 d . . . O6 O 0.31662(14) -0.00164(7) 0.36379(7) 0.0229(3) Uani 1 1 d . . . O7 O 0.21246(14) 0.05956(7) 0.25763(7) 0.0222(3) Uani 1 1 d . . . O8 O 0.14613(14) 0.25641(6) 0.18758(7) 0.0222(3) Uani 1 1 d . . . O9 O 0.21652(14) 0.37346(7) 0.20100(7) 0.0222(3) Uani 1 1 d . . . O10 O 0.43529(15) 0.43238(7) 0.24893(8) 0.0284(4) Uani 1 1 d . . . O11 O 0.66339(15) 0.36944(7) 0.25177(8) 0.0318(4) Uani 1 1 d . . . O12 O 0.79322(16) 0.26104(7) 0.26012(7) 0.0274(4) Uani 1 1 d . . . O13 O 0.46992(16) 0.07085(7) 0.08416(8) 0.0303(4) Uani 1 1 d . . . O14 O 0.27283(15) 0.04148(7) 0.04717(7) 0.0244(3) Uani 1 1 d . . . N1 N 0.9059(2) -0.08225(10) 0.14632(11) 0.0388(5) Uani 1 1 d . . . N2 N 0.3427(2) -0.06910(9) 0.03221(10) 0.0310(5) Uani 1 1 d . . . N3 N 0.45808(16) 0.25238(8) 0.22416(8) 0.0196(4) Uani 1 1 d . . . N4 N 0.52941(16) 0.18519(8) 0.32842(8) 0.0214(4) Uani 1 1 d . . . C1 C 0.9307(3) -0.13965(13) 0.15380(16) 0.0495(8) Uani 1 1 d . . . H1 H 0.8916 -0.1605 0.1801 0.059 Uiso 1 1 calc R . . C2 C 1.0122(3) -0.16994(14) 0.12412(17) 0.0543(9) Uani 1 1 d . . . H2 H 1.0259 -0.2101 0.1303 0.065 Uiso 1 1 calc R . . C3 C 1.0716(3) -0.13967(16) 0.08588(15) 0.0549(9) Uani 1 1 d . . . H3 H 1.1282 -0.1586 0.0664 0.066 Uiso 1 1 calc R . . C4 C 1.0458(3) -0.08052(15) 0.07676(13) 0.0459(7) Uani 1 1 d . . . H4 H 1.0834 -0.0589 0.0504 0.055 Uiso 1 1 calc R . . C5 C 0.9630(2) -0.05419(12) 0.10763(11) 0.0314(6) Uani 1 1 d . . . C6 C 0.9358(2) 0.00976(12) 0.09658(11) 0.0295(5) Uani 1 1 d . . . C7 C 0.8478(3) 0.09553(12) 0.12909(13) 0.0428(7) Uani 1 1 d . . . H7A H 0.7685 0.1037 0.1030 0.051 Uiso 1 1 calc R . . H7B H 0.9139 0.1142 0.1126 0.051 Uiso 1 1 calc R . . C8 C 0.8463(2) 0.11972(11) 0.18984(11) 0.0278(5) Uani 1 1 d . . . C9 C 0.8698(2) 0.08470(10) 0.23973(11) 0.0270(5) Uani 1 1 d . . . H9 H 0.8858 0.0447 0.2363 0.032 Uiso 1 1 calc R . . C10 C 0.86948(19) 0.10935(10) 0.29543(10) 0.0224(5) Uani 1 1 d . . . C11 C 0.8443(2) 0.16852(10) 0.30138(10) 0.0222(5) Uani 1 1 d . . . H11 H 0.8436 0.1848 0.3386 0.027 Uiso 1 1 calc R . . C12 C 0.8200(2) 0.20322(10) 0.25016(11) 0.0231(5) Uani 1 1 d . . . C13 C 0.8212(2) 0.17984(11) 0.19436(11) 0.0258(5) Uani 1 1 d . . . H13 H 0.8055 0.2036 0.1607 0.031 Uiso 1 1 calc R . . C14 C 0.8919(2) 0.09278(10) 0.40042(10) 0.0245(5) Uani 1 1 d . . . H14A H 0.8156 0.1152 0.3998 0.029 Uiso 1 1 calc R . . H14B H 0.9630 0.1182 0.4146 0.029 Uiso 1 1 calc R . . C15 C 0.8946(2) 0.04003(10) 0.43984(11) 0.0249(5) Uani 1 1 d . . . H15A H 0.9686 0.0165 0.4385 0.030 Uiso 1 1 calc R . . H15B H 0.8969 0.0523 0.4806 0.030 Uiso 1 1 calc R . . C16 C 0.7772(2) -0.04435(10) 0.45395(10) 0.0227(5) Uani 1 1 d . . . H16A H 0.7718 -0.0331 0.4943 0.027 Uiso 1 1 calc R . . H16B H 0.8515 -0.0684 0.4554 0.027 Uiso 1 1 calc R . . C17 C 0.6632(2) -0.07850(10) 0.42663(10) 0.0224(5) Uani 1 1 d . . . H17A H 0.6670 -0.0880 0.3857 0.027 Uiso 1 1 calc R . . H17B H 0.6600 -0.1151 0.4481 0.027 Uiso 1 1 calc R . . C18 C 0.4448(2) -0.07974(10) 0.41097(11) 0.0245(5) Uani 1 1 d . . . H18A H 0.4460 -0.1127 0.4380 0.029 Uiso 1 1 calc R . . H18B H 0.4429 -0.0953 0.3713 0.029 Uiso 1 1 calc R . . C19 C 0.3307(2) -0.04278(11) 0.41157(11) 0.0262(5) Uani 1 1 d . . . H19A H 0.2572 -0.0678 0.4074 0.031 Uiso 1 1 calc R . . H19B H 0.3392 -0.0219 0.4491 0.031 Uiso 1 1 calc R . . C20 C 0.19804(19) 0.02692(10) 0.35508(10) 0.0212(4) Uani 1 1 d . . . H20A H 0.1798 0.0393 0.3931 0.025 Uiso 1 1 calc R . . H20B H 0.1331 -0.0003 0.3370 0.025 Uiso 1 1 calc R . . C21 C 0.1992(2) 0.07953(10) 0.31559(9) 0.0196(4) Uani 1 1 d . . . H21A H 0.1218 0.1015 0.3130 0.023 Uiso 1 1 calc R . . H21B H 0.2684 0.1053 0.3319 0.023 Uiso 1 1 calc R . . C22 C 0.20472(19) 0.10149(10) 0.21426(10) 0.0193(4) Uani 1 1 d . . . C23 C 0.18020(19) 0.16049(10) 0.22275(10) 0.0199(4) Uani 1 1 d . . . H23 H 0.1711 0.1742 0.2600 0.024 Uiso 1 1 calc R . . C24 C 0.16936(19) 0.19897(9) 0.17444(10) 0.0194(4) Uani 1 1 d . . . C25 C 0.18439(19) 0.17954(9) 0.11873(10) 0.0195(4) Uani 1 1 d . . . H25 H 0.1756 0.2055 0.0868 0.023 Uiso 1 1 calc R . . C26 C 0.21304(19) 0.12002(10) 0.11164(10) 0.0203(4) Uani 1 1 d . . . C27 C 0.2228(2) 0.08116(10) 0.15853(10) 0.0211(4) Uani 1 1 d . . . H27 H 0.2412 0.0417 0.1533 0.025 Uiso 1 1 calc R . . C28 C 0.1187(2) 0.29681(9) 0.13873(10) 0.0213(4) Uani 1 1 d . . . H28A H 0.0430 0.2849 0.1118 0.026 Uiso 1 1 calc R . . H28B H 0.1870 0.2976 0.1169 0.026 Uiso 1 1 calc R . . C29 C 0.1015(2) 0.35643(10) 0.16429(10) 0.0228(5) Uani 1 1 d . . . H29A H 0.0778 0.3848 0.1325 0.027 Uiso 1 1 calc R . . H29B H 0.0356 0.3550 0.1876 0.027 Uiso 1 1 calc R . . C30 C 0.2125(2) 0.43240(10) 0.22245(11) 0.0240(5) Uani 1 1 d . . . H30A H 0.1355 0.4389 0.2371 0.029 Uiso 1 1 calc R . . H30B H 0.2158 0.4603 0.1907 0.029 Uiso 1 1 calc R . . C31 C 0.3233(2) 0.44071(11) 0.27170(11) 0.0275(5) Uani 1 1 d . . . H31A H 0.3220 0.4801 0.2881 0.033 Uiso 1 1 calc R . . H31B H 0.3199 0.4125 0.3032 0.033 Uiso 1 1 calc R . . C32 C 0.5421(2) 0.43736(11) 0.29562(12) 0.0324(6) Uani 1 1 d . . . H32A H 0.5377 0.4078 0.3258 0.039 Uiso 1 1 calc R . . H32B H 0.5430 0.4759 0.3140 0.039 Uiso 1 1 calc R . . C33 C 0.6582(2) 0.42903(11) 0.27146(12) 0.0325(6) Uani 1 1 d . . . H33A H 0.6587 0.4558 0.2385 0.039 Uiso 1 1 calc R . . H33B H 0.7308 0.4375 0.3020 0.039 Uiso 1 1 calc R . . C34 C 0.7769(2) 0.36124(11) 0.23127(12) 0.0307(5) Uani 1 1 d . . . H34A H 0.8471 0.3692 0.2632 0.037 Uiso 1 1 calc R . . H34B H 0.7811 0.3885 0.1991 0.037 Uiso 1 1 calc R . . C35 C 0.7848(2) 0.29992(10) 0.21015(11) 0.0267(5) Uani 1 1 d . . . H35A H 0.7110 0.2906 0.1807 0.032 Uiso 1 1 calc R . . H35B H 0.8579 0.2954 0.1920 0.032 Uiso 1 1 calc R . . C36 C 0.2279(2) 0.10114(10) 0.05026(10) 0.0258(5) Uani 1 1 d . . . H36A H 0.1476 0.1047 0.0237 0.031 Uiso 1 1 calc R . . H36B H 0.2858 0.1278 0.0362 0.031 Uiso 1 1 calc R . . C37 C 0.3964(2) 0.03295(10) 0.06401(10) 0.0223(5) Uani 1 1 d . . . C38 C 0.4331(2) -0.02978(10) 0.05534(9) 0.0221(5) Uani 1 1 d . . . C39 C 0.5566(2) -0.04379(10) 0.07204(9) 0.0228(5) Uani 1 1 d . . . H39 H 0.6154 -0.0153 0.0874 0.027 Uiso 1 1 calc R . . C40 C 0.5915(2) -0.10110(12) 0.06557(11) 0.0314(5) Uani 1 1 d . . . H40 H 0.6751 -0.1120 0.0766 0.038 Uiso 1 1 calc R . . C41 C 0.5027(2) -0.14287(11) 0.04259(11) 0.0293(5) Uani 1 1 d . . . H41 H 0.5257 -0.1819 0.0384 0.035 Uiso 1 1 calc R . . C42 C 0.3794(2) -0.12552(11) 0.02611(11) 0.0301(5) Uani 1 1 d . . . H42 H 0.3197 -0.1534 0.0103 0.036 Uiso 1 1 calc R . . C43 C 0.5440(2) 0.15362(11) 0.37932(11) 0.0253(5) Uani 1 1 d . . . H43 H 0.5512 0.1730 0.4156 0.030 Uiso 1 1 calc R . . C44 C 0.5483(2) 0.09311(11) 0.37784(11) 0.0279(5) Uani 1 1 d . . . H44 H 0.5594 0.0715 0.4130 0.033 Uiso 1 1 calc R . . C45 C 0.5362(2) 0.06475(10) 0.32383(12) 0.0282(5) Uani 1 1 d . . . H45 H 0.5402 0.0239 0.3222 0.034 Uiso 1 1 calc R . . C46 C 0.5179(2) 0.09766(10) 0.27195(11) 0.0248(5) Uani 1 1 d . . . H46 H 0.5075 0.0787 0.2353 0.030 Uiso 1 1 calc R . . C47 C 0.51490(19) 0.15843(10) 0.27429(10) 0.0201(4) Uani 1 1 d . . . C48 C 0.49687(18) 0.19570(10) 0.22063(10) 0.0197(4) Uani 1 1 d . . . C49 C 0.5165(2) 0.17470(10) 0.16648(10) 0.0241(5) Uani 1 1 d . . . H49 H 0.5442 0.1363 0.1633 0.029 Uiso 1 1 calc R . . C50 C 0.4949(2) 0.21093(11) 0.11699(11) 0.0262(5) Uani 1 1 d . . . H50 H 0.5064 0.1966 0.0803 0.031 Uiso 1 1 calc R . . C51 C 0.4562(2) 0.26827(11) 0.12208(11) 0.0261(5) Uani 1 1 d . . . H51 H 0.4423 0.2930 0.0891 0.031 Uiso 1 1 calc R . . C52 C 0.4385(2) 0.28841(10) 0.17664(11) 0.0230(5) Uani 1 1 d . . . H52 H 0.4129 0.3271 0.1807 0.028 Uiso 1 1 calc R . . C53 C 0.4336(2) 0.27431(10) 0.28193(10) 0.0227(5) Uani 1 1 d . . . H53A H 0.3517 0.2613 0.2877 0.027 Uiso 1 1 calc R . . H53B H 0.4351 0.3170 0.2825 0.027 Uiso 1 1 calc R . . C54 C 0.5336(2) 0.25043(10) 0.33083(10) 0.0240(5) Uani 1 1 d . . . H54A H 0.6153 0.2643 0.3256 0.029 Uiso 1 1 calc R . . H54B H 0.5192 0.2640 0.3692 0.029 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 0.0219(3) 0.0275(3) 0.0255(3) 0.0004(2) 0.0000(2) -0.0031(2) P2 0.0249(3) 0.0206(3) 0.0227(3) 0.0017(2) 0.0034(2) -0.0021(2) F1 0.0638(11) 0.0659(12) 0.0210(8) 0.0003(8) 0.0010(7) -0.0270(9) F2 0.0269(9) 0.0585(12) 0.130(2) -0.0278(13) 0.0120(10) 0.0033(8) F3 0.0882(14) 0.0592(12) 0.0395(10) 0.0250(9) -0.0248(9) -0.0426(11) F4 0.0323(8) 0.0594(11) 0.0581(11) -0.0209(9) 0.0155(7) -0.0064(7) F5 0.0405(9) 0.0338(8) 0.0577(11) -0.0101(8) -0.0032(8) -0.0082(7) F6 0.0341(7) 0.0300(7) 0.0270(7) 0.0035(6) -0.0014(6) -0.0090(6) F7 0.0289(8) 0.0402(8) 0.0402(9) 0.0012(7) -0.0038(6) 0.0007(6) F8 0.0432(9) 0.0557(10) 0.0302(8) 0.0146(7) 0.0125(7) 0.0017(7) F9 0.0628(10) 0.0232(7) 0.0300(8) -0.0010(6) 0.0043(7) 0.0042(7) F10 0.0447(9) 0.0462(9) 0.0306(8) 0.0045(7) 0.0160(7) 0.0079(7) F11 0.0403(8) 0.0225(7) 0.0538(10) 0.0007(7) -0.0046(7) 0.0010(6) F12 0.0303(8) 0.0386(9) 0.0483(10) 0.0047(7) -0.0039(7) -0.0104(6) O1 0.0722(15) 0.0488(12) 0.0416(12) -0.0021(10) 0.0303(11) 0.0014(11) O2 0.0650(13) 0.0306(10) 0.0457(12) -0.0040(9) 0.0330(10) 0.0037(9) O3 0.0306(8) 0.0188(8) 0.0297(9) 0.0057(7) 0.0087(7) 0.0021(6) O4 0.0266(8) 0.0204(8) 0.0245(8) 0.0070(6) -0.0011(6) -0.0044(6) O5 0.0232(8) 0.0205(8) 0.0273(8) 0.0012(6) 0.0058(6) 0.0030(6) O6 0.0222(7) 0.0230(8) 0.0247(8) 0.0087(6) 0.0074(6) 0.0059(6) O7 0.0297(8) 0.0189(7) 0.0183(8) 0.0017(6) 0.0053(6) 0.0029(6) O8 0.0300(8) 0.0156(7) 0.0211(8) 0.0006(6) 0.0051(6) 0.0022(6) O9 0.0218(7) 0.0171(7) 0.0269(8) -0.0029(6) 0.0028(6) 0.0013(6) O10 0.0238(8) 0.0304(9) 0.0299(9) -0.0099(7) 0.0023(7) 0.0011(7) O11 0.0303(9) 0.0225(8) 0.0395(10) -0.0060(7) -0.0010(7) 0.0013(7) O12 0.0356(9) 0.0197(8) 0.0274(9) 0.0063(7) 0.0070(7) 0.0048(7) O13 0.0352(9) 0.0261(9) 0.0299(9) -0.0072(7) 0.0067(7) -0.0032(7) O14 0.0295(8) 0.0206(8) 0.0236(8) -0.0023(6) 0.0064(6) 0.0034(6) N1 0.0334(11) 0.0358(12) 0.0452(14) -0.0074(10) 0.0020(10) -0.0053(10) N2 0.0343(11) 0.0268(11) 0.0322(11) -0.0017(9) 0.0069(9) -0.0001(9) N3 0.0180(8) 0.0203(9) 0.0202(9) -0.0008(7) 0.0027(7) -0.0008(7) N4 0.0179(8) 0.0217(9) 0.0233(10) 0.0008(8) 0.0003(7) -0.0001(7) C1 0.0432(16) 0.0359(16) 0.062(2) -0.0004(14) -0.0093(14) -0.0094(13) C2 0.0471(17) 0.0322(15) 0.068(2) -0.0177(15) -0.0279(16) 0.0070(13) C3 0.060(2) 0.056(2) 0.0434(18) -0.0141(16) -0.0045(15) 0.0225(17) C4 0.0477(16) 0.0570(19) 0.0311(15) -0.0107(13) 0.0029(12) 0.0154(14) C5 0.0257(12) 0.0362(14) 0.0291(13) -0.0117(11) -0.0035(10) -0.0002(10) C6 0.0249(11) 0.0382(14) 0.0251(12) -0.0106(11) 0.0043(10) -0.0032(10) C7 0.0668(19) 0.0317(14) 0.0331(15) -0.0015(12) 0.0176(14) 0.0084(13) C8 0.0247(11) 0.0290(13) 0.0312(13) -0.0002(10) 0.0093(10) 0.0010(9) C9 0.0263(11) 0.0202(11) 0.0362(14) 0.0013(10) 0.0098(10) 0.0013(9) C10 0.0162(10) 0.0223(11) 0.0286(12) 0.0038(9) 0.0035(9) -0.0019(8) C11 0.0203(10) 0.0212(11) 0.0250(11) 0.0021(9) 0.0040(9) -0.0014(9) C12 0.0186(10) 0.0190(11) 0.0313(13) 0.0027(9) 0.0036(9) -0.0002(8) C13 0.0216(11) 0.0284(12) 0.0274(12) 0.0056(10) 0.0045(9) 0.0027(9) C14 0.0246(11) 0.0209(11) 0.0272(12) 0.0008(9) 0.0027(9) -0.0018(9) C15 0.0217(11) 0.0237(12) 0.0273(12) 0.0035(9) -0.0008(9) -0.0013(9) C16 0.0272(11) 0.0184(11) 0.0220(11) 0.0046(9) 0.0036(9) 0.0033(9) C17 0.0248(11) 0.0178(10) 0.0251(12) 0.0031(9) 0.0062(9) 0.0024(9) C18 0.0228(11) 0.0222(11) 0.0295(12) 0.0062(9) 0.0077(9) 0.0003(9) C19 0.0276(12) 0.0274(12) 0.0253(12) 0.0112(10) 0.0093(9) 0.0033(9) C20 0.0181(10) 0.0247(11) 0.0214(11) 0.0028(9) 0.0053(8) 0.0022(8) C21 0.0203(10) 0.0218(11) 0.0173(11) -0.0010(9) 0.0052(8) 0.0026(8) C22 0.0177(10) 0.0204(11) 0.0191(11) 0.0038(8) 0.0017(8) 0.0004(8) C23 0.0177(10) 0.0219(11) 0.0199(11) -0.0014(9) 0.0031(8) -0.0008(8) C24 0.0167(10) 0.0166(10) 0.0241(11) -0.0003(8) 0.0020(8) 0.0002(8) C25 0.0189(10) 0.0186(10) 0.0205(11) 0.0031(8) 0.0029(8) 0.0012(8) C26 0.0189(10) 0.0218(11) 0.0196(11) -0.0016(9) 0.0025(8) 0.0006(8) C27 0.0227(10) 0.0187(10) 0.0215(11) 0.0004(9) 0.0032(9) 0.0036(8) C28 0.0210(10) 0.0201(11) 0.0218(11) 0.0032(9) 0.0014(9) 0.0016(8) C29 0.0190(10) 0.0207(11) 0.0280(12) 0.0019(9) 0.0023(9) 0.0030(8) C30 0.0272(11) 0.0175(11) 0.0287(12) -0.0029(9) 0.0087(9) 0.0026(9) C31 0.0296(12) 0.0249(12) 0.0279(12) -0.0071(10) 0.0054(10) 0.0038(9) C32 0.0347(13) 0.0283(13) 0.0313(13) -0.0091(10) -0.0014(10) 0.0015(10) C33 0.0340(13) 0.0241(12) 0.0378(14) 0.0003(11) 0.0030(11) -0.0028(10) C34 0.0256(12) 0.0245(12) 0.0386(14) 0.0091(10) -0.0032(10) -0.0023(10) C35 0.0226(11) 0.0270(12) 0.0299(13) 0.0116(10) 0.0038(9) 0.0011(9) C36 0.0346(12) 0.0213(11) 0.0220(12) 0.0011(9) 0.0064(9) 0.0061(9) C37 0.0275(11) 0.0248(12) 0.0155(10) -0.0001(9) 0.0068(9) -0.0005(9) C38 0.0282(11) 0.0230(11) 0.0159(11) 0.0007(9) 0.0063(9) -0.0004(9) C39 0.0241(11) 0.0307(12) 0.0141(10) 0.0006(9) 0.0047(8) -0.0022(9) C40 0.0316(13) 0.0430(15) 0.0198(12) 0.0053(10) 0.0056(10) 0.0077(11) C41 0.0410(14) 0.0252(12) 0.0237(12) 0.0041(9) 0.0116(10) 0.0100(10) C42 0.0389(13) 0.0220(11) 0.0297(13) -0.0013(10) 0.0069(10) -0.0022(10) C43 0.0195(10) 0.0316(13) 0.0222(12) 0.0036(10) -0.0024(9) -0.0005(9) C44 0.0206(11) 0.0294(13) 0.0310(13) 0.0082(10) -0.0015(9) -0.0008(9) C45 0.0187(11) 0.0203(11) 0.0441(15) 0.0067(10) 0.0020(10) 0.0003(9) C46 0.0191(10) 0.0226(11) 0.0317(13) -0.0019(10) 0.0022(9) -0.0010(9) C47 0.0150(9) 0.0217(11) 0.0226(11) -0.0017(9) 0.0012(8) 0.0003(8) C48 0.0142(10) 0.0200(11) 0.0240(11) -0.0024(9) 0.0010(8) -0.0012(8) C49 0.0191(10) 0.0253(12) 0.0277(12) -0.0058(9) 0.0039(9) -0.0017(9) C50 0.0239(11) 0.0336(13) 0.0213(12) -0.0039(10) 0.0045(9) -0.0067(9) C51 0.0225(11) 0.0333(13) 0.0215(11) 0.0041(10) 0.0013(9) -0.0050(9) C52 0.0192(10) 0.0213(11) 0.0280(12) 0.0034(9) 0.0028(9) 0.0000(8) C53 0.0244(11) 0.0214(11) 0.0230(11) -0.0014(9) 0.0065(9) 0.0023(9) C54 0.0280(12) 0.0198(11) 0.0231(12) -0.0032(9) 0.0021(9) -0.0020(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 1.5747(17) . ? P1 F2 1.5825(18) . ? P1 F1 1.5835(17) . ? P1 F5 1.5955(16) . ? P1 F3 1.5994(18) . ? P1 F6 1.6074(15) . ? P2 F12 1.5847(15) . ? P2 F11 1.5890(15) . ? P2 F10 1.5923(15) . ? P2 F9 1.5961(15) . ? P2 F7 1.6084(15) . ? P2 F8 1.6108(16) . ? O1 C6 1.204(3) . ? O2 C6 1.323(3) . ? O2 C7 1.439(3) . ? O3 C10 1.365(3) . ? O3 C14 1.436(3) . ? O4 C16 1.414(3) . ? O4 C15 1.416(3) . ? O5 C17 1.420(3) . ? O5 C18 1.422(3) . ? O6 C20 1.423(3) . ? O6 C19 1.425(3) . ? O7 C22 1.367(3) . ? O7 C21 1.435(3) . ? O8 C24 1.372(3) . ? O8 C28 1.434(3) . ? O9 C29 1.423(3) . ? O9 C30 1.428(3) . ? O10 C31 1.424(3) . ? O10 C32 1.428(3) . ? O11 C34 1.412(3) . ? O11 C33 1.430(3) . ? O12 C12 1.373(3) . ? O12 C35 1.434(3) . ? O13 C37 1.205(3) . ? O14 C37 1.341(3) . ? O14 C36 1.446(3) . ? N1 C5 1.334(4) . ? N1 C1 1.335(4) . ? N2 C42 1.356(3) . ? N2 C38 1.359(3) . ? N3 C52 1.346(3) . ? N3 C48 1.361(3) . ? N3 C53 1.483(3) . ? N4 C43 1.352(3) . ? N4 C47 1.363(3) . ? N4 C54 1.482(3) . ? C1 C2 1.395(5) . ? C1 H1 0.9300 . ? C2 C3 1.366(5) . ? C2 H2 0.9300 . ? C3 C4 1.379(5) . ? C3 H3 0.9300 . ? C4 C5 1.381(4) . ? C4 H4 0.9300 . ? C5 C6 1.493(4) . ? C7 C8 1.498(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.376(4) . ? C8 C13 1.399(3) . ? C9 C10 1.393(4) . ? C9 H9 0.9300 . ? C10 C11 1.382(3) . ? C11 C12 1.396(3) . ? C11 H11 0.9300 . ? C12 C13 1.386(3) . ? C13 H13 0.9300 . ? C14 C15 1.496(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.496(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.499(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.499(3) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.386(3) . ? C22 C27 1.405(3) . ? C23 C24 1.397(3) . ? C23 H23 0.9300 . ? C24 C25 1.388(3) . ? C25 C26 1.402(3) . ? C25 H25 0.9300 . ? C26 C27 1.378(3) . ? C26 C36 1.507(3) . ? C27 H27 0.9300 . ? C28 C29 1.500(3) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.500(3) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.482(4) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.481(3) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.502(3) . ? C38 C39 1.363(3) . ? C39 C40 1.371(4) . ? C39 H39 0.9300 . ? C40 C41 1.385(4) . ? C40 H40 0.9300 . ? C41 C42 1.379(4) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.375(3) . ? C43 H43 0.9300 . ? C44 C45 1.378(4) . ? C44 H44 0.9300 . ? C45 C46 1.386(4) . ? C45 H45 0.9300 . ? C46 C47 1.381(3) . ? C46 H46 0.9300 . ? C47 C48 1.474(3) . ? C48 C49 1.382(3) . ? C49 C50 1.384(3) . ? C49 H49 0.9300 . ? C50 C51 1.379(4) . ? C50 H50 0.9300 . ? C51 C52 1.377(3) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 C54 1.508(3) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? 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 179.38(12) . . ? F4 P1 F1 89.79(11) . . ? F2 P1 F1 90.68(13) . . ? F4 P1 F5 90.26(9) . . ? F2 P1 F5 90.14(10) . . ? F1 P1 F5 90.07(10) . . ? F4 P1 F3 90.14(12) . . ? F2 P1 F3 89.38(14) . . ? F1 P1 F3 179.49(10) . . ? F5 P1 F3 90.44(10) . . ? F4 P1 F6 90.32(9) . . ? F2 P1 F6 89.29(9) . . ? F1 P1 F6 89.94(8) . . ? F5 P1 F6 179.42(10) . . ? F3 P1 F6 89.55(9) . . ? F12 P2 F11 90.99(8) . . ? F12 P2 F10 91.47(9) . . ? F11 P2 F10 90.33(9) . . ? F12 P2 F9 90.42(9) . . ? F11 P2 F9 178.43(9) . . ? F10 P2 F9 90.32(8) . . ? F12 P2 F7 178.75(10) . . ? F11 P2 F7 89.73(8) . . ? F10 P2 F7 89.55(9) . . ? F9 P2 F7 88.85(9) . . ? F12 P2 F8 89.63(9) . . ? F11 P2 F8 89.88(9) . . ? F10 P2 F8 178.87(9) . . ? F9 P2 F8 89.44(9) . . ? F7 P2 F8 89.35(9) . . ? C6 O2 C7 116.6(2) . . ? C10 O3 C14 117.90(17) . . ? C16 O4 C15 112.76(17) . . ? C17 O5 C18 110.40(17) . . ? C20 O6 C19 111.75(16) . . ? C22 O7 C21 116.68(16) . . ? C24 O8 C28 117.15(17) . . ? C29 O9 C30 112.17(16) . . ? C31 O10 C32 110.28(18) . . ? C34 O11 C33 108.52(18) . . ? C12 O12 C35 116.08(19) . . ? C37 O14 C36 116.80(18) . . ? C5 N1 C1 116.3(3) . . ? C42 N2 C38 117.1(2) . . ? C52 N3 C48 122.03(19) . . ? C52 N3 C53 119.31(18) . . ? C48 N3 C53 118.65(18) . . ? C43 N4 C47 121.5(2) . . ? C43 N4 C54 119.98(19) . . ? C47 N4 C54 118.47(18) . . ? N1 C1 C2 123.4(3) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 118.9(3) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 118.6(3) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C3 C4 C5 118.5(3) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 124.2(3) . . ? N1 C5 C6 118.4(2) . . ? C4 C5 C6 117.5(3) . . ? O1 C6 O2 123.1(3) . . ? O1 C6 C5 123.8(2) . . ? O2 C6 C5 113.2(2) . . ? O2 C7 C8 109.1(2) . . ? O2 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O2 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C9 C8 C13 120.7(2) . . ? C9 C8 C7 121.8(2) . . ? C13 C8 C7 117.5(2) . . ? C8 C9 C10 119.8(2) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? O3 C10 C11 124.1(2) . . ? O3 C10 C9 115.0(2) . . ? C11 C10 C9 121.0(2) . . ? C10 C11 C12 118.3(2) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? O12 C12 C13 123.9(2) . . ? O12 C12 C11 114.3(2) . . ? C13 C12 C11 121.7(2) . . ? C12 C13 C8 118.5(2) . . ? C12 C13 H13 120.8 . . ? C8 C13 H13 120.8 . . ? O3 C14 C15 106.69(18) . . ? O3 C14 H14A 110.4 . . ? C15 C14 H14A 110.4 . . ? O3 C14 H14B 110.4 . . ? C15 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? O4 C15 C14 107.91(18) . . ? O4 C15 H15A 110.1 . . ? C14 C15 H15A 110.1 . . ? O4 C15 H15B 110.1 . . ? C14 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? O4 C16 C17 108.74(18) . . ? O4 C16 H16A 109.9 . . ? C17 C16 H16A 109.9 . . ? O4 C16 H16B 109.9 . . ? C17 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? O5 C17 C16 109.85(18) . . ? O5 C17 H17A 109.7 . . ? C16 C17 H17A 109.7 . . ? O5 C17 H17B 109.7 . . ? C16 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? O5 C18 C19 109.47(19) . . ? O5 C18 H18A 109.8 . . ? C19 C18 H18A 109.8 . . ? O5 C18 H18B 109.8 . . ? C19 C18 H18B 109.8 . . ? H18A C18 H18B 108.2 . . ? O6 C19 C18 109.27(18) . . ? O6 C19 H19A 109.8 . . ? C18 C19 H19A 109.8 . . ? O6 C19 H19B 109.8 . . ? C18 C19 H19B 109.8 . . ? H19A C19 H19B 108.3 . . ? O6 C20 C21 109.73(17) . . ? O6 C20 H20A 109.7 . . ? C21 C20 H20A 109.7 . . ? O6 C20 H20B 109.7 . . ? C21 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? O7 C21 C20 108.66(17) . . ? O7 C21 H21A 110.0 . . ? C20 C21 H21A 110.0 . . ? O7 C21 H21B 110.0 . . ? C20 C21 H21B 110.0 . . ? H21A C21 H21B 108.3 . . ? O7 C22 C23 123.9(2) . . ? O7 C22 C27 115.55(19) . . ? C23 C22 C27 120.5(2) . . ? C22 C23 C24 118.9(2) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? O8 C24 C25 124.2(2) . . ? O8 C24 C23 114.33(19) . . ? C25 C24 C23 121.5(2) . . ? C24 C25 C26 118.6(2) . . ? C24 C25 H25 120.7 . . ? C26 C25 H25 120.7 . . ? C27 C26 C25 120.8(2) . . ? C27 C26 C36 122.6(2) . . ? C25 C26 C36 116.54(19) . . ? C26 C27 C22 119.6(2) . . ? C26 C27 H27 120.2 . . ? C22 C27 H27 120.2 . . ? O8 C28 C29 107.18(18) . . ? O8 C28 H28A 110.3 . . ? C29 C28 H28A 110.3 . . ? O8 C28 H28B 110.3 . . ? C29 C28 H28B 110.3 . . ? H28A C28 H28B 108.5 . . ? O9 C29 C28 108.40(17) . . ? O9 C29 H29A 110.0 . . ? C28 C29 H29A 110.0 . . ? O9 C29 H29B 110.0 . . ? C28 C29 H29B 110.0 . . ? H29A C29 H29B 108.4 . . ? O9 C30 C31 107.73(18) . . ? O9 C30 H30A 110.2 . . ? C31 C30 H30A 110.2 . . ? O9 C30 H30B 110.2 . . ? C31 C30 H30B 110.2 . . ? H30A C30 H30B 108.5 . . ? O10 C31 C30 109.22(19) . . ? O10 C31 H31A 109.8 . . ? C30 C31 H31A 109.8 . . ? O10 C31 H31B 109.8 . . ? C30 C31 H31B 109.8 . . ? H31A C31 H31B 108.3 . . ? O10 C32 C33 109.9(2) . . ? O10 C32 H32A 109.7 . . ? C33 C32 H32A 109.7 . . ? O10 C32 H32B 109.7 . . ? C33 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? O11 C33 C32 108.9(2) . . ? O11 C33 H33A 109.9 . . ? C32 C33 H33A 109.9 . . ? O11 C33 H33B 109.9 . . ? C32 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? O11 C34 C35 109.85(19) . . ? O11 C34 H34A 109.7 . . ? C35 C34 H34A 109.7 . . ? O11 C34 H34B 109.7 . . ? C35 C34 H34B 109.7 . . ? H34A C34 H34B 108.2 . . ? O12 C35 C34 108.5(2) . . ? O12 C35 H35A 110.0 . . ? C34 C35 H35A 110.0 . . ? O12 C35 H35B 110.0 . . ? C34 C35 H35B 110.0 . . ? H35A C35 H35B 108.4 . . ? O14 C36 C26 114.10(18) . . ? O14 C36 H36A 108.7 . . ? C26 C36 H36A 108.7 . . ? O14 C36 H36B 108.7 . . ? C26 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? O13 C37 O14 124.3(2) . . ? O13 C37 C38 123.6(2) . . ? O14 C37 C38 112.04(19) . . ? N2 C38 C39 123.9(2) . . ? N2 C38 C37 118.9(2) . . ? C39 C38 C37 117.1(2) . . ? C38 C39 C40 118.0(2) . . ? C38 C39 H39 121.0 . . ? C40 C39 H39 121.0 . . ? C39 C40 C41 120.2(2) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C42 C41 C40 118.8(2) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? N2 C42 C41 122.1(2) . . ? N2 C42 H42 119.0 . . ? C41 C42 H42 119.0 . . ? N4 C43 C44 120.5(2) . . ? N4 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C45 119.4(2) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C44 C45 C46 119.5(2) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C47 C46 C45 120.4(2) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? N4 C47 C46 118.7(2) . . ? N4 C47 C48 118.49(19) . . ? C46 C47 C48 122.8(2) . . ? N3 C48 C49 118.7(2) . . ? N3 C48 C47 119.16(19) . . ? C49 C48 C47 122.1(2) . . ? C48 C49 C50 119.9(2) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C51 C50 C49 119.9(2) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C52 C51 C50 119.1(2) . . ? C52 C51 H51 120.5 . . ? C50 C51 H51 120.5 . . ? N3 C52 C51 120.3(2) . . ? N3 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? N3 C53 C54 108.49(17) . . ? N3 C53 H53A 110.0 . . ? C54 C53 H53A 110.0 . . ? N3 C53 H53B 110.0 . . ? C54 C53 H53B 110.0 . . ? H53A C53 H53B 108.4 . . ? N4 C54 C53 108.57(18) . . ? N4 C54 H54A 110.0 . . ? C53 C54 H54A 110.0 . . ? N4 C54 H54B 110.0 . . ? C53 C54 H54B 110.0 . . ? H54A C54 H54B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 66.66 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.969 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.084 #===END data_110404_xz_229b #TrackingRef '- CC-Supracryptand-ESI-02.cif' _database_code_depnum_ccdc_archive 'CCDC 829264' #TrackingRef '- CC-Supracryptand-ESI-02.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H50 N2 O14, C26 H24 N2, 2(F6 P)' _chemical_formula_sum 'C68 H74 F12 N4 O14 P2' _chemical_formula_weight 1461.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7621(4) _cell_length_b 12.8281(5) _cell_length_c 29.8195(11) _cell_angle_alpha 85.387(3) _cell_angle_beta 84.518(3) _cell_angle_gamma 70.803(4) _cell_volume 3864.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16788 _cell_measurement_theta_min 2.9791 _cell_measurement_theta_max 66.4533 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 1.286 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6618 _exptl_absorpt_correction_T_max 0.7564 _exptl_absorpt_process_details ; CrysAlis PRO (Oxford Diffraction, 2010) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3592 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29018 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 66.56 _reflns_number_total 13386 _reflns_number_gt 11455 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'CrysAlis PRO (Oxford Diffraction, 2010)' _computing_data_collection 'CrysAlis PRO' _computing_data_reduction 'CrysAlis PRO' _computing_molecular_graphics 'OLEX2 (Dolomanov et al., 2009)' _computing_publication_material OLEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+4.9002P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13386 _refine_ls_number_parameters 901 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1625 _refine_ls_wR_factor_gt 0.1573 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.05823(7) 0.21822(7) 0.03437(2) 0.03688(18) Uani 1 1 d . . . P2 P 0.36308(13) 0.24012(7) 0.41844(3) 0.0621(3) Uani 1 1 d . . . F1 F 0.0976(2) 0.1920(2) -0.01723(6) 0.0652(6) Uani 1 1 d . . . F2 F -0.0851(2) 0.2894(3) 0.02271(8) 0.0953(10) Uani 1 1 d . . . F3 F 0.1080(3) 0.32220(18) 0.02707(8) 0.0777(7) Uani 1 1 d . . . F4 F 0.02001(19) 0.2471(2) 0.08556(6) 0.0735(7) Uani 1 1 d . . . F5 F 0.20313(18) 0.14560(15) 0.04668(7) 0.0527(5) Uani 1 1 d . . . F6 F 0.0149(3) 0.1108(3) 0.04233(9) 0.0929(9) Uani 1 1 d . . . F7 F 0.2595(9) 0.1914(4) 0.4076(2) 0.304(5) Uani 1 1 d . . . F8 F 0.4506(9) 0.1819(2) 0.38005(12) 0.325(6) Uani 1 1 d . . . F9 F 0.4630(3) 0.2921(3) 0.43289(14) 0.1239(12) Uani 1 1 d . . . F10 F 0.2721(3) 0.3002(2) 0.45985(11) 0.1075(11) Uani 1 1 d . . . F11 F 0.4180(3) 0.13344(17) 0.45080(7) 0.0758(7) Uani 1 1 d . . . F12 F 0.3077(4) 0.34539(19) 0.38594(9) 0.1260(15) Uani 1 1 d . . . O1 O -0.1281(2) 0.36705(15) 0.18658(7) 0.0421(5) Uani 1 1 d . . . O2 O -0.00286(17) 0.20315(13) 0.21517(6) 0.0293(4) Uani 1 1 d . . . O3 O 0.00564(19) -0.18979(14) 0.28444(6) 0.0326(4) Uani 1 1 d . . . O4 O 0.0438(2) -0.27274(16) 0.37350(6) 0.0437(5) Uani 1 1 d . . . O5 O 0.2270(2) -0.34806(16) 0.44080(7) 0.0490(6) Uani 1 1 d . . . O6 O 0.4316(2) -0.25639(19) 0.43425(7) 0.0518(6) Uani 1 1 d . . . O7 O 0.5839(2) -0.19772(16) 0.36125(6) 0.0391(5) Uani 1 1 d . . . O8 O 0.74510(18) -0.23464(14) 0.21043(6) 0.0308(4) Uani 1 1 d . . . O9 O 0.75997(17) -0.34065(15) 0.12844(6) 0.0302(4) Uani 1 1 d . . . O10 O 0.62589(18) -0.43771(14) 0.07441(6) 0.0288(4) Uani 1 1 d . . . O11 O 0.34553(18) -0.34183(14) 0.07660(5) 0.0289(4) Uani 1 1 d . . . O12 O 0.13848(18) -0.22368(14) 0.13280(5) 0.0281(4) Uani 1 1 d . . . O13 O 0.47116(18) 0.18474(14) 0.23263(6) 0.0302(4) Uani 1 1 d . . . O14 O 0.4770(2) 0.35229(15) 0.24653(7) 0.0415(5) Uani 1 1 d . . . N1 N 0.1076(2) 0.30224(18) 0.26831(7) 0.0345(5) Uani 1 1 d . . . N2 N 0.3147(2) 0.26656(18) 0.16607(7) 0.0314(5) Uani 1 1 d . . . N3 N 0.51587(19) 0.86775(16) 0.08414(6) 0.0219(4) Uani 1 1 d . . . N4 N 0.1774(2) 0.9700(2) 0.38007(7) 0.0376(5) Uani 1 1 d . . . C1 C 0.1589(3) 0.3526(3) 0.29552(10) 0.0429(7) Uani 1 1 d . . . H1 H 0.2243 0.3081 0.3145 0.051 Uiso 1 1 calc R . . C2 C 0.1214(4) 0.4666(3) 0.29740(10) 0.0486(8) Uani 1 1 d . . . H2 H 0.1603 0.4988 0.3174 0.058 Uiso 1 1 calc R . . C3 C 0.0277(4) 0.5323(3) 0.27009(10) 0.0469(8) Uani 1 1 d . . . H3 H 0.0004 0.6105 0.2709 0.056 Uiso 1 1 calc R . . C4 C -0.0263(3) 0.4820(2) 0.24132(9) 0.0376(6) Uani 1 1 d . . . H4 H -0.0909 0.5250 0.2217 0.045 Uiso 1 1 calc R . . C5 C 0.0164(3) 0.3670(2) 0.24178(8) 0.0302(6) Uani 1 1 d . . . C6 C -0.0458(3) 0.3142(2) 0.21146(8) 0.0295(5) Uani 1 1 d . . . C7 C -0.0681(3) 0.1531(2) 0.18684(9) 0.0321(6) Uani 1 1 d . . . H7A H -0.0507 0.1735 0.1547 0.039 Uiso 1 1 calc R . . H7B H -0.1646 0.1803 0.1943 0.039 Uiso 1 1 calc R . . C8 C -0.0163(2) 0.0293(2) 0.19482(9) 0.0276(5) Uani 1 1 d . . . C9 C -0.0313(3) -0.0181(2) 0.23788(9) 0.0287(5) Uani 1 1 d . . . H9 H -0.0720 0.0269 0.2624 0.034 Uiso 1 1 calc R . . C10 C 0.0147(2) -0.1329(2) 0.24416(8) 0.0270(5) Uani 1 1 d . . . C11 C 0.0751(2) -0.1988(2) 0.20850(8) 0.0253(5) Uani 1 1 d . . . H11 H 0.1096 -0.2768 0.2134 0.030 Uiso 1 1 calc R . . C12 C 0.0849(2) -0.1501(2) 0.16565(8) 0.0242(5) Uani 1 1 d . . . C13 C 0.0413(2) -0.0354(2) 0.15844(8) 0.0263(5) Uani 1 1 d . . . H13 H 0.0509 -0.0022 0.1292 0.032 Uiso 1 1 calc R . . C14 C -0.0701(3) -0.1297(2) 0.32168(9) 0.0344(6) Uani 1 1 d . . . H14A H -0.1583 -0.0833 0.3126 0.041 Uiso 1 1 calc R . . H14B H -0.0251 -0.0810 0.3321 0.041 Uiso 1 1 calc R . . C15 C -0.0831(3) -0.2132(2) 0.35871(9) 0.0402(7) Uani 1 1 d . . . H15A H -0.1416 -0.1751 0.3842 0.048 Uiso 1 1 calc R . . H15B H -0.1225 -0.2648 0.3474 0.048 Uiso 1 1 calc R . . C16 C 0.0391(4) -0.3575(3) 0.40690(10) 0.0500(8) Uani 1 1 d . . . H16A H 0.0003 -0.4086 0.3948 0.060 Uiso 1 1 calc R . . H16B H -0.0173 -0.3243 0.4337 0.060 Uiso 1 1 calc R . . C17 C 0.1745(4) -0.4194(3) 0.42005(11) 0.0570(10) Uani 1 1 d . . . H17A H 0.1721 -0.4822 0.4414 0.068 Uiso 1 1 calc R . . H17B H 0.2319 -0.4496 0.3930 0.068 Uiso 1 1 calc R . . C18 C 0.3536(4) -0.4071(3) 0.45516(11) 0.0587(10) Uani 1 1 d . . . H18A H 0.4108 -0.4470 0.4298 0.070 Uiso 1 1 calc R . . H18B H 0.3469 -0.4621 0.4797 0.070 Uiso 1 1 calc R . . C19 C 0.4120(4) -0.3274(3) 0.47157(10) 0.0574(10) Uani 1 1 d . . . H19A H 0.3517 -0.2834 0.4954 0.069 Uiso 1 1 calc R . . H19B H 0.4972 -0.3681 0.4844 0.069 Uiso 1 1 calc R . . C20 C 0.5279(4) -0.2068(3) 0.44014(10) 0.0503(8) Uani 1 1 d . . . H20A H 0.6147 -0.2644 0.4435 0.060 Uiso 1 1 calc R . . H20B H 0.5036 -0.1642 0.4677 0.060 Uiso 1 1 calc R . . C21 C 0.5358(3) -0.1309(2) 0.39937(9) 0.0428(7) Uani 1 1 d . . . H21A H 0.4474 -0.0772 0.3944 0.051 Uiso 1 1 calc R . . H21B H 0.5962 -0.0894 0.4039 0.051 Uiso 1 1 calc R . . C22 C 0.6009(3) -0.1433(2) 0.32078(8) 0.0319(6) Uani 1 1 d . . . C23 C 0.5651(3) -0.0284(2) 0.31485(9) 0.0335(6) Uani 1 1 d . . . H23 H 0.5239 0.0172 0.3392 0.040 Uiso 1 1 calc R . . C24 C 0.5906(3) 0.0182(2) 0.27300(9) 0.0308(6) Uani 1 1 d . . . C25 C 0.6503(3) -0.0475(2) 0.23672(9) 0.0295(5) Uani 1 1 d . . . H25 H 0.6676 -0.0146 0.2081 0.035 Uiso 1 1 calc R . . C26 C 0.6842(3) -0.1618(2) 0.24301(8) 0.0276(5) Uani 1 1 d . . . C27 C 0.6600(3) -0.2102(2) 0.28500(8) 0.0306(6) Uani 1 1 d . . . H27 H 0.6836 -0.2883 0.2892 0.037 Uiso 1 1 calc R . . C28 C 0.7723(3) -0.1887(2) 0.16657(8) 0.0284(5) Uani 1 1 d . . . H28A H 0.8262 -0.1402 0.1689 0.034 Uiso 1 1 calc R . . H28B H 0.6887 -0.1439 0.1536 0.034 Uiso 1 1 calc R . . C29 C 0.8455(3) -0.2819(2) 0.13692(9) 0.0311(6) Uani 1 1 d . . . H29A H 0.8776 -0.2523 0.1081 0.037 Uiso 1 1 calc R . . H29B H 0.9228 -0.3322 0.1519 0.037 Uiso 1 1 calc R . . C30 C 0.8259(3) -0.4335(2) 0.10161(9) 0.0359(6) Uani 1 1 d . . . H30A H 0.9077 -0.4796 0.1153 0.043 Uiso 1 1 calc R . . H30B H 0.8504 -0.4074 0.0710 0.043 Uiso 1 1 calc R . . C31 C 0.7375(3) -0.5006(2) 0.09868(9) 0.0357(6) Uani 1 1 d . . . H31A H 0.7864 -0.5690 0.0831 0.043 Uiso 1 1 calc R . . H31B H 0.7073 -0.5218 0.1294 0.043 Uiso 1 1 calc R . . C32 C 0.5384(3) -0.4993(2) 0.07244(8) 0.0320(6) Uani 1 1 d . . . H32A H 0.5115 -0.5219 0.1034 0.038 Uiso 1 1 calc R . . H32B H 0.5837 -0.5668 0.0558 0.038 Uiso 1 1 calc R . . C33 C 0.4193(3) -0.4303(2) 0.04922(8) 0.0315(6) Uani 1 1 d . . . H33A H 0.4465 -0.4007 0.0196 0.038 Uiso 1 1 calc R . . H33B H 0.3643 -0.4761 0.0440 0.038 Uiso 1 1 calc R . . C34 C 0.2217(3) -0.2810(2) 0.05962(8) 0.0298(5) Uani 1 1 d . . . H34A H 0.1646 -0.3282 0.0613 0.036 Uiso 1 1 calc R . . H34B H 0.2347 -0.2567 0.0277 0.036 Uiso 1 1 calc R . . C35 C 0.1573(3) -0.1824(2) 0.08737(8) 0.0283(5) Uani 1 1 d . . . H35A H 0.2143 -0.1352 0.0861 0.034 Uiso 1 1 calc R . . H35B H 0.0715 -0.1379 0.0758 0.034 Uiso 1 1 calc R . . C36 C 0.5610(3) 0.1412(2) 0.26810(9) 0.0352(6) Uani 1 1 d . . . H36A H 0.5202 0.1750 0.2969 0.042 Uiso 1 1 calc R . . H36B H 0.6436 0.1588 0.2603 0.042 Uiso 1 1 calc R . . C37 C 0.4375(3) 0.2948(2) 0.22563(8) 0.0284(5) Uani 1 1 d . . . C38 C 0.3462(2) 0.3391(2) 0.18860(8) 0.0258(5) Uani 1 1 d . . . C39 C 0.3011(3) 0.4525(2) 0.17936(8) 0.0285(5) Uani 1 1 d . . . H39 H 0.3247 0.5009 0.1968 0.034 Uiso 1 1 calc R . . C40 C 0.2209(3) 0.4932(2) 0.14413(9) 0.0318(6) Uani 1 1 d . . . H40 H 0.1886 0.5703 0.1367 0.038 Uiso 1 1 calc R . . C41 C 0.1887(3) 0.4196(2) 0.12005(9) 0.0325(6) Uani 1 1 d . . . H41 H 0.1346 0.4450 0.0954 0.039 Uiso 1 1 calc R . . C42 C 0.2365(3) 0.3078(2) 0.13241(9) 0.0334(6) Uani 1 1 d . . . H42 H 0.2123 0.2578 0.1160 0.040 Uiso 1 1 calc R . . C43 C 0.5362(3) 0.7683(2) -0.03188(8) 0.0300(6) Uani 1 1 d . . . H43 H 0.6235 0.7176 -0.0331 0.036 Uiso 1 1 calc R . . C44 C 0.4553(3) 0.7742(2) -0.06574(9) 0.0372(7) Uani 1 1 d . . . H44 H 0.4876 0.7284 -0.0906 0.045 Uiso 1 1 calc R . . C45 C 0.3268(3) 0.8467(3) -0.06385(9) 0.0392(7) Uani 1 1 d . . . H45 H 0.2711 0.8490 -0.0870 0.047 Uiso 1 1 calc R . . C46 C 0.2800(3) 0.9152(2) -0.02842(9) 0.0351(6) Uani 1 1 d . . . H46 H 0.1922 0.9650 -0.0271 0.042 Uiso 1 1 calc R . . C47 C 0.3628(3) 0.9110(2) 0.00567(8) 0.0277(5) Uani 1 1 d . . . H47 H 0.3314 0.9592 0.0298 0.033 Uiso 1 1 calc R . . C48 C 0.4898(2) 0.83722(19) 0.00444(8) 0.0246(5) Uani 1 1 d . . . C49 C 0.5840(2) 0.8298(2) 0.04007(8) 0.0261(5) Uani 1 1 d . . . H49A H 0.6417 0.7522 0.0440 0.031 Uiso 1 1 calc R . . H49B H 0.6408 0.8752 0.0295 0.031 Uiso 1 1 calc R . . C50 C 0.4837(2) 0.79429(19) 0.11406(7) 0.0218(5) Uani 1 1 d . . . H50 H 0.5055 0.7194 0.1066 0.026 Uiso 1 1 calc R . . C51 C 0.4197(2) 0.82702(19) 0.15501(8) 0.0236(5) Uani 1 1 d . . . H51 H 0.3961 0.7749 0.1756 0.028 Uiso 1 1 calc R . . C52 C 0.3888(2) 0.93651(19) 0.16694(8) 0.0229(5) Uani 1 1 d . . . C53 C 0.4225(3) 1.0105(2) 0.13496(8) 0.0260(5) Uani 1 1 d . . . H53 H 0.4023 1.0858 0.1416 0.031 Uiso 1 1 calc R . . C54 C 0.4847(3) 0.9747(2) 0.09403(8) 0.0267(5) Uani 1 1 d . . . H54 H 0.5061 1.0257 0.0723 0.032 Uiso 1 1 calc R . . C55 C 0.3270(2) 0.9746(2) 0.21117(8) 0.0255(5) Uani 1 1 d . . . H55 H 0.2985 1.0514 0.2161 0.031 Uiso 1 1 calc R . . C56 C 0.3096(2) 0.9045(2) 0.24471(8) 0.0261(5) Uani 1 1 d . . . H56 H 0.3335 0.8290 0.2380 0.031 Uiso 1 1 calc R . . C57 C 0.2575(2) 0.9323(2) 0.29066(8) 0.0276(5) Uani 1 1 d . . . C58 C 0.2641(3) 0.8452(2) 0.32276(8) 0.0346(6) Uani 1 1 d . . . H58 H 0.2968 0.7712 0.3137 0.041 Uiso 1 1 calc R . . C59 C 0.2241(3) 0.8656(2) 0.36706(9) 0.0391(7) Uani 1 1 d . . . H59 H 0.2293 0.8058 0.3886 0.047 Uiso 1 1 calc R . . C60 C 0.1640(3) 1.0565(2) 0.34961(9) 0.0364(6) Uani 1 1 d . . . H60 H 0.1273 1.1297 0.3594 0.044 Uiso 1 1 calc R . . C61 C 0.2025(3) 1.0404(2) 0.30497(9) 0.0314(6) Uani 1 1 d . . . H61 H 0.1921 1.1017 0.2839 0.038 Uiso 1 1 calc R . . C62 C 0.1363(4) 0.9894(3) 0.42874(9) 0.0521(8) Uani 1 1 d . . . H62A H 0.1386 1.0630 0.4354 0.062 Uiso 1 1 calc R . . H62B H 0.1996 0.9331 0.4474 0.062 Uiso 1 1 calc R . . C63 C 0.0004(3) 0.9836(3) 0.44102(9) 0.0453(8) Uani 1 1 d . . . C64 C -0.1093(4) 1.0726(3) 0.43095(11) 0.0567(9) Uani 1 1 d . . . H64 H -0.0979 1.1367 0.4153 0.068 Uiso 1 1 calc R . . C65 C -0.2343(4) 1.0698(3) 0.44312(12) 0.0639(10) Uani 1 1 d . . . H65 H -0.3083 1.1315 0.4356 0.077 Uiso 1 1 calc R . . C66 C -0.2536(4) 0.9778(3) 0.46629(11) 0.0573(9) Uani 1 1 d . . . H66 H -0.3402 0.9764 0.4751 0.069 Uiso 1 1 calc R . . C67 C -0.1453(4) 0.8881(3) 0.47648(10) 0.0562(10) Uani 1 1 d . . . H67 H -0.1573 0.8244 0.4923 0.067 Uiso 1 1 calc R . . C68 C -0.0192(4) 0.8907(3) 0.46377(9) 0.0517(9) Uani 1 1 d . . . H68 H 0.0547 0.8282 0.4707 0.062 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 0.0319(4) 0.0549(5) 0.0261(3) -0.0095(3) -0.0021(3) -0.0153(3) P2 0.1199(9) 0.0296(4) 0.0374(4) 0.0045(3) -0.0219(5) -0.0218(5) F1 0.0640(13) 0.1037(17) 0.0316(9) -0.0214(10) 0.0006(9) -0.0291(12) F2 0.0483(12) 0.147(2) 0.0704(15) -0.0521(16) -0.0312(11) 0.0138(14) F3 0.112(2) 0.0554(13) 0.0779(15) 0.0092(11) -0.0350(14) -0.0381(13) F4 0.0428(11) 0.144(2) 0.0334(10) -0.0298(12) 0.0036(8) -0.0256(12) F5 0.0450(10) 0.0504(11) 0.0573(11) -0.0137(9) -0.0127(8) -0.0030(8) F6 0.109(2) 0.123(2) 0.0875(18) -0.0049(16) -0.0065(15) -0.0925(19) F7 0.535(12) 0.168(4) 0.345(8) 0.162(5) -0.386(9) -0.241(6) F8 0.719(14) 0.0380(15) 0.078(2) -0.0055(14) 0.175(5) 0.012(4) F9 0.105(2) 0.104(2) 0.175(3) 0.038(2) -0.026(2) -0.057(2) F10 0.106(2) 0.0613(15) 0.119(2) 0.0196(15) 0.0291(18) 0.0068(14) F11 0.1029(18) 0.0425(11) 0.0578(13) 0.0171(10) 0.0053(12) 0.0014(11) F12 0.276(5) 0.0427(13) 0.0693(16) 0.0210(11) -0.092(2) -0.0490(19) O1 0.0530(12) 0.0257(10) 0.0397(11) 0.0041(8) -0.0112(9) -0.0014(9) O2 0.0362(10) 0.0186(8) 0.0304(9) 0.0009(7) -0.0045(7) -0.0053(7) O3 0.0493(11) 0.0262(9) 0.0195(8) -0.0004(7) 0.0031(8) -0.0103(8) O4 0.0666(14) 0.0363(11) 0.0256(10) 0.0049(8) 0.0020(9) -0.0163(10) O5 0.0656(14) 0.0324(11) 0.0304(10) 0.0090(8) 0.0048(10) 0.0046(10) O6 0.0583(14) 0.0578(14) 0.0297(11) 0.0181(10) -0.0040(10) -0.0101(11) O7 0.0564(12) 0.0323(10) 0.0220(9) 0.0016(7) 0.0006(8) -0.0074(9) O8 0.0422(10) 0.0272(9) 0.0237(9) -0.0010(7) -0.0015(7) -0.0124(8) O9 0.0275(9) 0.0330(9) 0.0287(9) -0.0096(7) 0.0009(7) -0.0070(7) O10 0.0377(10) 0.0227(8) 0.0259(9) -0.0028(7) -0.0019(7) -0.0092(7) O11 0.0368(10) 0.0335(9) 0.0197(8) -0.0074(7) -0.0018(7) -0.0145(8) O12 0.0399(10) 0.0263(9) 0.0192(8) 0.0008(7) -0.0006(7) -0.0130(8) O13 0.0428(10) 0.0216(9) 0.0274(9) 0.0004(7) -0.0118(8) -0.0100(8) O14 0.0628(13) 0.0264(10) 0.0426(11) 0.0013(8) -0.0236(10) -0.0194(9) N1 0.0470(14) 0.0304(12) 0.0264(11) -0.0021(9) 0.0010(10) -0.0136(10) N2 0.0386(12) 0.0276(11) 0.0282(11) -0.0037(9) -0.0061(9) -0.0095(9) N3 0.0277(10) 0.0227(10) 0.0167(9) -0.0010(7) -0.0021(8) -0.0099(8) N4 0.0484(14) 0.0441(14) 0.0166(10) -0.0042(9) -0.0018(9) -0.0095(11) C1 0.0574(19) 0.0453(17) 0.0304(14) -0.0045(12) -0.0013(13) -0.0225(15) C2 0.072(2) 0.0484(18) 0.0352(16) -0.0139(14) 0.0082(15) -0.0326(17) C3 0.070(2) 0.0321(15) 0.0417(17) -0.0100(13) 0.0194(15) -0.0253(15) C4 0.0523(17) 0.0258(13) 0.0319(14) -0.0013(11) 0.0119(12) -0.0131(12) C5 0.0406(15) 0.0228(12) 0.0239(12) 0.0008(10) 0.0081(11) -0.0093(11) C6 0.0357(14) 0.0220(12) 0.0254(12) 0.0023(10) 0.0044(11) -0.0047(11) C7 0.0361(14) 0.0254(13) 0.0328(14) 0.0011(10) -0.0075(11) -0.0064(11) C8 0.0288(13) 0.0241(12) 0.0308(13) 0.0010(10) -0.0061(10) -0.0090(10) C9 0.0333(13) 0.0260(13) 0.0274(13) -0.0025(10) -0.0047(10) -0.0095(10) C10 0.0321(13) 0.0273(13) 0.0234(12) 0.0018(10) -0.0035(10) -0.0124(10) C11 0.0301(13) 0.0218(12) 0.0250(12) 0.0006(9) -0.0035(10) -0.0096(10) C12 0.0238(12) 0.0272(12) 0.0229(12) -0.0001(9) -0.0037(9) -0.0098(10) C13 0.0280(12) 0.0286(13) 0.0236(12) 0.0038(10) -0.0049(10) -0.0114(10) C14 0.0446(16) 0.0324(14) 0.0241(13) -0.0038(11) 0.0031(11) -0.0107(12) C15 0.0533(18) 0.0421(16) 0.0234(13) -0.0030(11) 0.0046(12) -0.0146(14) C16 0.087(3) 0.0329(15) 0.0267(14) 0.0040(12) 0.0041(15) -0.0183(16) C17 0.097(3) 0.0277(15) 0.0320(16) 0.0023(12) 0.0091(16) -0.0064(17) C18 0.069(2) 0.0403(18) 0.0414(18) 0.0176(14) 0.0115(16) 0.0083(16) C19 0.057(2) 0.061(2) 0.0272(15) 0.0210(15) 0.0050(14) 0.0095(17) C20 0.060(2) 0.0536(19) 0.0244(14) 0.0033(13) -0.0031(13) -0.0019(16) C21 0.0561(19) 0.0409(16) 0.0221(13) -0.0041(12) -0.0011(12) -0.0030(14) C22 0.0414(15) 0.0291(13) 0.0233(12) 0.0009(10) -0.0046(11) -0.0089(11) C23 0.0419(15) 0.0294(13) 0.0274(13) -0.0030(10) -0.0084(11) -0.0071(11) C24 0.0379(14) 0.0269(13) 0.0294(13) -0.0007(10) -0.0110(11) -0.0107(11) C25 0.0368(14) 0.0279(13) 0.0265(13) 0.0038(10) -0.0101(11) -0.0131(11) C26 0.0336(13) 0.0284(13) 0.0233(12) -0.0022(10) -0.0055(10) -0.0124(11) C27 0.0419(15) 0.0242(12) 0.0267(13) 0.0002(10) -0.0070(11) -0.0110(11) C28 0.0315(13) 0.0319(13) 0.0242(12) 0.0023(10) -0.0050(10) -0.0136(11) C29 0.0272(13) 0.0407(15) 0.0262(13) -0.0007(11) -0.0021(10) -0.0122(11) C30 0.0308(14) 0.0366(15) 0.0327(14) -0.0109(11) -0.0012(11) 0.0011(11) C31 0.0409(15) 0.0243(13) 0.0344(14) -0.0051(11) -0.0063(12) 0.0014(11) C32 0.0502(16) 0.0250(13) 0.0239(12) -0.0067(10) 0.0052(11) -0.0175(12) C33 0.0460(15) 0.0341(14) 0.0214(12) -0.0087(10) 0.0030(11) -0.0221(12) C34 0.0406(14) 0.0356(14) 0.0189(11) 0.0006(10) -0.0046(10) -0.0199(12) C35 0.0363(14) 0.0328(13) 0.0195(11) 0.0045(10) -0.0065(10) -0.0164(11) C36 0.0498(16) 0.0276(13) 0.0305(14) 0.0017(11) -0.0175(12) -0.0125(12) C37 0.0361(14) 0.0240(12) 0.0250(12) -0.0011(10) -0.0026(10) -0.0095(11) C38 0.0305(13) 0.0253(12) 0.0218(11) -0.0024(9) 0.0012(10) -0.0098(10) C39 0.0350(14) 0.0247(12) 0.0265(12) -0.0006(10) -0.0011(10) -0.0113(10) C40 0.0348(14) 0.0291(13) 0.0282(13) 0.0037(10) -0.0001(11) -0.0076(11) C41 0.0309(13) 0.0380(15) 0.0240(12) -0.0016(11) -0.0018(10) -0.0049(11) C42 0.0359(14) 0.0350(14) 0.0295(13) -0.0083(11) -0.0063(11) -0.0093(11) C43 0.0470(15) 0.0251(12) 0.0219(12) -0.0024(10) 0.0051(11) -0.0191(11) C44 0.066(2) 0.0368(15) 0.0210(12) -0.0031(11) 0.0010(12) -0.0343(15) C45 0.0551(18) 0.0505(17) 0.0261(13) 0.0048(12) -0.0084(12) -0.0364(15) C46 0.0388(15) 0.0447(16) 0.0279(13) 0.0088(11) -0.0059(11) -0.0232(13) C47 0.0360(14) 0.0315(13) 0.0194(11) 0.0017(10) 0.0006(10) -0.0176(11) C48 0.0366(13) 0.0241(12) 0.0167(11) 0.0005(9) 0.0020(10) -0.0163(10) C49 0.0324(13) 0.0279(12) 0.0184(11) -0.0028(9) 0.0021(10) -0.0109(10) C50 0.0274(12) 0.0207(11) 0.0198(11) -0.0004(9) -0.0058(9) -0.0103(9) C51 0.0290(12) 0.0236(12) 0.0195(11) 0.0007(9) -0.0011(9) -0.0107(10) C52 0.0250(12) 0.0237(12) 0.0205(11) -0.0006(9) -0.0055(9) -0.0078(9) C53 0.0379(14) 0.0204(11) 0.0211(11) -0.0016(9) -0.0034(10) -0.0107(10) C54 0.0387(14) 0.0232(12) 0.0210(11) 0.0024(9) -0.0029(10) -0.0146(10) C55 0.0338(13) 0.0215(11) 0.0216(12) -0.0037(9) -0.0017(10) -0.0090(10) C56 0.0331(13) 0.0224(12) 0.0216(12) -0.0020(9) -0.0041(10) -0.0064(10) C57 0.0297(13) 0.0274(13) 0.0228(12) -0.0006(10) -0.0037(10) -0.0049(10) C58 0.0446(16) 0.0288(13) 0.0217(12) 0.0018(10) 0.0019(11) -0.0022(12) C59 0.0475(17) 0.0378(15) 0.0235(13) 0.0026(11) -0.0015(12) -0.0036(13) C60 0.0467(16) 0.0320(14) 0.0296(14) -0.0100(11) 0.0024(12) -0.0112(12) C61 0.0397(15) 0.0291(13) 0.0239(12) -0.0008(10) -0.0007(11) -0.0095(11) C62 0.066(2) 0.066(2) 0.0188(14) -0.0113(13) 0.0019(13) -0.0141(17) C63 0.068(2) 0.0419(16) 0.0160(12) -0.0061(11) 0.0053(13) -0.0060(15) C64 0.074(2) 0.0429(18) 0.0378(17) 0.0062(14) 0.0149(16) -0.0053(17) C65 0.067(2) 0.059(2) 0.0467(19) 0.0019(17) 0.0120(17) -0.0011(18) C66 0.076(2) 0.062(2) 0.0312(16) -0.0150(15) 0.0156(16) -0.0213(19) C67 0.100(3) 0.0471(19) 0.0224(14) -0.0099(13) 0.0106(16) -0.027(2) C68 0.088(3) 0.0375(16) 0.0197(13) -0.0069(12) 0.0034(15) -0.0084(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 F2 1.568(2) . ? P1 F4 1.5836(19) . ? P1 F3 1.586(2) . ? P1 F6 1.588(2) . ? P1 F1 1.5891(19) . ? P1 F5 1.5917(19) . ? P2 F8 1.491(3) . ? P2 F7 1.515(5) . ? P2 F9 1.547(4) . ? P2 F12 1.578(2) . ? P2 F10 1.582(3) . ? P2 F11 1.587(2) . ? O1 C6 1.202(3) . ? O2 C6 1.344(3) . ? O2 C7 1.455(3) . ? O3 C10 1.367(3) . ? O3 C14 1.429(3) . ? O4 C15 1.420(4) . ? O4 C16 1.424(3) . ? O5 C18 1.412(4) . ? O5 C17 1.428(4) . ? O6 C20 1.413(4) . ? O6 C19 1.425(4) . ? O7 C22 1.372(3) . ? O7 C21 1.430(3) . ? O8 C26 1.367(3) . ? O8 C28 1.435(3) . ? O9 C29 1.418(3) . ? O9 C30 1.432(3) . ? O10 C32 1.421(3) . ? O10 C31 1.432(3) . ? O11 C33 1.421(3) . ? O11 C34 1.423(3) . ? O12 C12 1.366(3) . ? O12 C35 1.435(3) . ? O13 C37 1.341(3) . ? O13 C36 1.453(3) . ? O14 C37 1.202(3) . ? N1 C5 1.336(4) . ? N1 C1 1.336(4) . ? N2 C42 1.333(3) . ? N2 C38 1.336(3) . ? N3 C54 1.350(3) . ? N3 C50 1.351(3) . ? N3 C49 1.478(3) . ? N4 C59 1.342(4) . ? N4 C60 1.355(4) . ? N4 C62 1.492(3) . ? C1 C2 1.387(4) . ? C1 H1 0.9500 . ? C2 C3 1.370(5) . ? C2 H2 0.9500 . ? C3 C4 1.386(5) . ? C3 H3 0.9500 . ? C4 C5 1.392(4) . ? C4 H4 0.9500 . ? C5 C6 1.495(4) . ? C7 C8 1.507(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.389(4) . ? C8 C9 1.394(4) . ? C9 C10 1.394(4) . ? C9 H9 0.9500 . ? C10 C11 1.385(4) . ? C11 C12 1.387(3) . ? C11 H11 0.9500 . ? C12 C13 1.395(3) . ? C13 H13 0.9500 . ? C14 C15 1.505(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.485(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.497(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.509(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.392(4) . ? C22 C23 1.397(4) . ? C23 C24 1.383(4) . ? C23 H23 0.9500 . ? C24 C25 1.397(4) . ? C24 C36 1.501(4) . ? C25 C26 1.390(4) . ? C25 H25 0.9500 . ? C26 C27 1.393(4) . ? C27 H27 0.9500 . ? C28 C29 1.500(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.490(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.494(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.499(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.499(3) . ? C38 C39 1.387(3) . ? C39 C40 1.382(4) . ? C39 H39 0.9500 . ? C40 C41 1.378(4) . ? C40 H40 0.9500 . ? C41 C42 1.387(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.378(4) . ? C43 C48 1.401(3) . ? C43 H43 0.9500 . ? C44 C45 1.388(5) . ? C44 H44 0.9500 . ? C45 C46 1.378(4) . ? C45 H45 0.9500 . ? C46 C47 1.401(4) . ? C46 H46 0.9500 . ? C47 C48 1.382(4) . ? C47 H47 0.9500 . ? C48 C49 1.514(3) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.369(3) . ? C50 H50 0.9500 . ? C51 C52 1.400(3) . ? C51 H51 0.9500 . ? C52 C53 1.399(3) . ? C52 C55 1.464(3) . ? C53 C54 1.372(3) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.332(3) . ? C55 H55 0.9500 . ? C56 C57 1.456(3) . ? C56 H56 0.9500 . ? C57 C58 1.399(4) . ? C57 C61 1.401(4) . ? C58 C59 1.368(4) . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C60 C61 1.367(4) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 C63 1.497(5) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.383(5) . ? C63 C68 1.391(5) . ? C64 C65 1.371(6) . ? C64 H64 0.9500 . ? C65 C66 1.384(5) . ? C65 H65 0.9500 . ? C66 C67 1.380(5) . ? C66 H66 0.9500 . ? C67 C68 1.383(6) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? 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 F2 P1 F4 89.51(12) . . ? F2 P1 F3 92.04(16) . . ? F4 P1 F3 88.40(14) . . ? F2 P1 F6 90.59(18) . . ? F4 P1 F6 91.51(15) . . ? F3 P1 F6 177.37(16) . . ? F2 P1 F1 90.44(12) . . ? F4 P1 F1 178.55(15) . . ? F3 P1 F1 90.16(13) . . ? F6 P1 F1 89.93(14) . . ? F2 P1 F5 179.41(16) . . ? F4 P1 F5 90.01(11) . . ? F3 P1 F5 88.30(12) . . ? F6 P1 F5 89.07(14) . . ? F1 P1 F5 90.04(11) . . ? F8 P2 F7 89.0(5) . . ? F8 P2 F9 95.1(4) . . ? F7 P2 F9 175.8(4) . . ? F8 P2 F12 89.6(2) . . ? F7 P2 F12 92.5(2) . . ? F9 P2 F12 88.59(18) . . ? F8 P2 F10 178.9(3) . . ? F7 P2 F10 91.3(4) . . ? F9 P2 F10 84.6(2) . . ? F12 P2 F10 91.47(17) . . ? F8 P2 F11 90.11(17) . . ? F7 P2 F11 86.92(18) . . ? F9 P2 F11 92.04(17) . . ? F12 P2 F11 179.32(16) . . ? F10 P2 F11 88.81(13) . . ? C6 O2 C7 113.35(19) . . ? C10 O3 C14 118.33(19) . . ? C15 O4 C16 111.9(2) . . ? C18 O5 C17 110.6(3) . . ? C20 O6 C19 113.6(3) . . ? C22 O7 C21 116.5(2) . . ? C26 O8 C28 117.04(19) . . ? C29 O9 C30 111.9(2) . . ? C32 O10 C31 110.48(19) . . ? C33 O11 C34 112.36(18) . . ? C12 O12 C35 118.94(19) . . ? C37 O13 C36 113.33(19) . . ? C5 N1 C1 116.9(2) . . ? C42 N2 C38 116.6(2) . . ? C54 N3 C50 120.6(2) . . ? C54 N3 C49 120.39(19) . . ? C50 N3 C49 119.04(19) . . ? C59 N4 C60 121.0(2) . . ? C59 N4 C62 118.6(2) . . ? C60 N4 C62 120.4(2) . . ? N1 C1 C2 123.3(3) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 119.3(3) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 118.5(3) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C3 C4 C5 118.5(3) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 123.5(3) . . ? N1 C5 C6 118.8(2) . . ? C4 C5 C6 117.7(2) . . ? O1 C6 O2 123.4(2) . . ? O1 C6 C5 122.6(2) . . ? O2 C6 C5 114.0(2) . . ? O2 C7 C8 108.9(2) . . ? O2 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O2 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C13 C8 C9 121.3(2) . . ? C13 C8 C7 118.8(2) . . ? C9 C8 C7 119.8(2) . . ? C10 C9 C8 118.7(2) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? O3 C10 C11 114.6(2) . . ? O3 C10 C9 124.6(2) . . ? C11 C10 C9 120.8(2) . . ? C10 C11 C12 119.5(2) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? O12 C12 C11 114.2(2) . . ? O12 C12 C13 125.0(2) . . ? C11 C12 C13 120.9(2) . . ? C8 C13 C12 118.7(2) . . ? C8 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? O3 C14 C15 107.3(2) . . ? O3 C14 H14A 110.3 . . ? C15 C14 H14A 110.3 . . ? O3 C14 H14B 110.3 . . ? C15 C14 H14B 110.3 . . ? H14A C14 H14B 108.5 . . ? O4 C15 C14 109.2(2) . . ? O4 C15 H15A 109.8 . . ? C14 C15 H15A 109.8 . . ? O4 C15 H15B 109.8 . . ? C14 C15 H15B 109.8 . . ? H15A C15 H15B 108.3 . . ? O4 C16 C17 109.7(3) . . ? O4 C16 H16A 109.7 . . ? C17 C16 H16A 109.7 . . ? O4 C16 H16B 109.7 . . ? C17 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? O5 C17 C16 110.0(2) . . ? O5 C17 H17A 109.7 . . ? C16 C17 H17A 109.7 . . ? O5 C17 H17B 109.7 . . ? C16 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? O5 C18 C19 109.0(3) . . ? O5 C18 H18A 109.9 . . ? C19 C18 H18A 109.9 . . ? O5 C18 H18B 109.9 . . ? C19 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? O6 C19 C18 108.2(3) . . ? O6 C19 H19A 110.1 . . ? C18 C19 H19A 110.1 . . ? O6 C19 H19B 110.1 . . ? C18 C19 H19B 110.1 . . ? H19A C19 H19B 108.4 . . ? O6 C20 C21 108.5(3) . . ? O6 C20 H20A 110.0 . . ? C21 C20 H20A 110.0 . . ? O6 C20 H20B 110.0 . . ? C21 C20 H20B 110.0 . . ? H20A C20 H20B 108.4 . . ? O7 C21 C20 107.8(2) . . ? O7 C21 H21A 110.1 . . ? C20 C21 H21A 110.1 . . ? O7 C21 H21B 110.1 . . ? C20 C21 H21B 110.1 . . ? H21A C21 H21B 108.5 . . ? O7 C22 C27 115.8(2) . . ? O7 C22 C23 123.6(2) . . ? C27 C22 C23 120.6(2) . . ? C24 C23 C22 119.0(2) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C23 C24 C25 121.2(2) . . ? C23 C24 C36 118.4(2) . . ? C25 C24 C36 120.3(2) . . ? C26 C25 C24 119.1(2) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? O8 C26 C25 124.5(2) . . ? O8 C26 C27 114.9(2) . . ? C25 C26 C27 120.5(2) . . ? C22 C27 C26 119.5(2) . . ? C22 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? O8 C28 C29 108.4(2) . . ? O8 C28 H28A 110.0 . . ? C29 C28 H28A 110.0 . . ? O8 C28 H28B 110.0 . . ? C29 C28 H28B 110.0 . . ? H28A C28 H28B 108.4 . . ? O9 C29 C28 109.3(2) . . ? O9 C29 H29A 109.8 . . ? C28 C29 H29A 109.8 . . ? O9 C29 H29B 109.8 . . ? C28 C29 H29B 109.8 . . ? H29A C29 H29B 108.3 . . ? O9 C30 C31 109.8(2) . . ? O9 C30 H30A 109.7 . . ? C31 C30 H30A 109.7 . . ? O9 C30 H30B 109.7 . . ? C31 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? O10 C31 C30 109.7(2) . . ? O10 C31 H31A 109.7 . . ? C30 C31 H31A 109.7 . . ? O10 C31 H31B 109.7 . . ? C30 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? O10 C32 C33 109.8(2) . . ? O10 C32 H32A 109.7 . . ? C33 C32 H32A 109.7 . . ? O10 C32 H32B 109.7 . . ? C33 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? O11 C33 C32 109.08(19) . . ? O11 C33 H33A 109.9 . . ? C32 C33 H33A 109.9 . . ? O11 C33 H33B 109.9 . . ? C32 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? O11 C34 C35 108.82(19) . . ? O11 C34 H34A 109.9 . . ? C35 C34 H34A 109.9 . . ? O11 C34 H34B 109.9 . . ? C35 C34 H34B 109.9 . . ? H34A C34 H34B 108.3 . . ? O12 C35 C34 106.9(2) . . ? O12 C35 H35A 110.3 . . ? C34 C35 H35A 110.3 . . ? O12 C35 H35B 110.3 . . ? C34 C35 H35B 110.3 . . ? H35A C35 H35B 108.6 . . ? O13 C36 C24 108.4(2) . . ? O13 C36 H36A 110.0 . . ? C24 C36 H36A 110.0 . . ? O13 C36 H36B 110.0 . . ? C24 C36 H36B 110.0 . . ? H36A C36 H36B 108.4 . . ? O14 C37 O13 123.7(2) . . ? O14 C37 C38 123.1(2) . . ? O13 C37 C38 113.1(2) . . ? N2 C38 C39 124.0(2) . . ? N2 C38 C37 117.8(2) . . ? C39 C38 C37 118.2(2) . . ? C40 C39 C38 118.3(2) . . ? C40 C39 H39 120.9 . . ? C38 C39 H39 120.9 . . ? C41 C40 C39 118.6(2) . . ? C41 C40 H40 120.7 . . ? C39 C40 H40 120.7 . . ? C40 C41 C42 118.8(2) . . ? C40 C41 H41 120.6 . . ? C42 C41 H41 120.6 . . ? N2 C42 C41 123.6(2) . . ? N2 C42 H42 118.2 . . ? C41 C42 H42 118.2 . . ? C44 C43 C48 120.0(3) . . ? C44 C43 H43 120.0 . . ? C48 C43 H43 120.0 . . ? C43 C44 C45 120.5(3) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C46 C45 C44 120.1(3) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 119.5(3) . . ? C45 C46 H46 120.2 . . ? C47 C46 H46 120.2 . . ? C48 C47 C46 120.5(2) . . ? C48 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C47 C48 C43 119.3(2) . . ? C47 C48 C49 122.8(2) . . ? C43 C48 C49 117.9(2) . . ? N3 C49 C48 113.1(2) . . ? N3 C49 H49A 109.0 . . ? C48 C49 H49A 109.0 . . ? N3 C49 H49B 109.0 . . ? C48 C49 H49B 109.0 . . ? H49A C49 H49B 107.8 . . ? N3 C50 C51 120.4(2) . . ? N3 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C50 C51 C52 120.7(2) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? C53 C52 C51 117.3(2) . . ? C53 C52 C55 119.7(2) . . ? C51 C52 C55 123.0(2) . . ? C54 C53 C52 120.1(2) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? N3 C54 C53 120.9(2) . . ? N3 C54 H54 119.6 . . ? C53 C54 H54 119.6 . . ? C56 C55 C52 121.8(2) . . ? C56 C55 H55 119.1 . . ? C52 C55 H55 119.1 . . ? C55 C56 C57 126.4(2) . . ? C55 C56 H56 116.8 . . ? C57 C56 H56 116.8 . . ? C58 C57 C61 117.8(2) . . ? C58 C57 C56 117.8(2) . . ? C61 C57 C56 124.3(2) . . ? C59 C58 C57 120.7(3) . . ? C59 C58 H58 119.6 . . ? C57 C58 H58 119.6 . . ? N4 C59 C58 119.9(3) . . ? N4 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? N4 C60 C61 121.2(2) . . ? N4 C60 H60 119.4 . . ? C61 C60 H60 119.4 . . ? C60 C61 C57 119.2(2) . . ? C60 C61 H61 120.4 . . ? C57 C61 H61 120.4 . . ? N4 C62 C63 111.9(3) . . ? N4 C62 H62A 109.2 . . ? C63 C62 H62A 109.2 . . ? N4 C62 H62B 109.2 . . ? C63 C62 H62B 109.2 . . ? H62A C62 H62B 107.9 . . ? C64 C63 C68 118.3(3) . . ? C64 C63 C62 120.4(3) . . ? C68 C63 C62 121.3(3) . . ? C65 C64 C63 121.1(3) . . ? C65 C64 H64 119.5 . . ? C63 C64 H64 119.5 . . ? C64 C65 C66 120.6(4) . . ? C64 C65 H65 119.7 . . ? C66 C65 H65 119.7 . . ? C67 C66 C65 119.1(4) . . ? C67 C66 H66 120.4 . . ? C65 C66 H66 120.4 . . ? C66 C67 C68 120.2(3) . . ? C66 C67 H67 119.9 . . ? C68 C67 H67 119.9 . . ? C67 C68 C63 120.7(3) . . ? C67 C68 H68 119.6 . . ? C63 C68 H68 119.6 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 66.56 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.455 _refine_diff_density_min -1.118 _refine_diff_density_rms 0.058 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.500 606 141 ' ' 2 0.347 0.705 0.850 12 0 ' ' 3 0.652 0.295 0.150 12 0 ' ' _platon_squeeze_details ; ;