# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_y33s _database_code_depnum_ccdc_archive 'CCDC 849576' #TrackingRef 'BF4-CH3OH.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H64 N16, 4(B F4), C H4 O2, O2' _chemical_formula_sum 'C55 H68 B4 F16 N16 O4' _chemical_formula_weight 1364.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.7015(5) _cell_length_b 12.8679(3) _cell_length_c 18.0196(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.0640(10) _cell_angle_gamma 90.00 _cell_volume 3515.66(18) _cell_formula_units_Z 2 _cell_measurement_temperature 113(1) _cell_measurement_reflns_used 11057 _cell_measurement_theta_min 1.3431 _cell_measurement_theta_max 31.1049 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.112 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7964 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(1) _diffrn_radiation_wavelength 0.710747 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Sealed tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30424 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6078 _reflns_number_gt 5154 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _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. ISOR was applied to disorder BF4 anion, water and MeOH molecules to allow their Uij components approximate to isotropic behavior. Hydrogen atoms of disorder water molecules were not added. ; _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^)+(0.1687P)^2^+6.6919P] 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 6078 _refine_ls_number_parameters 478 _refine_ls_number_restraints 103 _refine_ls_R_factor_all 0.1138 _refine_ls_R_factor_gt 0.1050 _refine_ls_wR_factor_ref 0.2881 _refine_ls_wR_factor_gt 0.2782 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.160 _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 B1 B 0.2905(3) 0.4703(4) -0.0032(3) 0.0330(10) Uani 1 1 d . . . F1 F 0.21597(16) 0.4725(2) 0.02396(16) 0.0462(7) Uani 1 1 d . . . F2 F 0.36081(17) 0.4337(2) 0.05529(16) 0.0523(8) Uani 1 1 d . . . F3 F 0.3102(2) 0.5694(3) -0.0218(2) 0.0667(9) Uani 1 1 d . . . F4 F 0.2764(2) 0.4028(3) -0.06498(18) 0.0702(10) Uani 1 1 d . . . B2 B 0.4646(5) 0.5986(6) 0.3986(4) 0.095(3) Uani 1 1 d D . . F5 F 0.4488(4) 0.4952(4) 0.3797(3) 0.1229(18) Uani 1 1 d DU . . F6 F 0.5518(5) 0.6180(9) 0.3924(7) 0.151(5) Uani 0.50 1 d PDU . . F6' F 0.4830(6) 0.6778(6) 0.3488(4) 0.086(2) Uani 0.50 1 d PDU . . F7 F 0.4063(3) 0.6444(3) 0.3376(2) 0.0648(11) Uani 0.80 1 d PDU . . F7' F 0.3769(5) 0.6164(10) 0.3968(7) 0.070(3) Uani 0.30 1 d PDU . . F8 F 0.4532(7) 0.6232(5) 0.4656(3) 0.100(2) Uani 0.60 1 d PDU . . F8' F 0.5172(8) 0.6113(10) 0.4677(4) 0.077(3) Uani 0.30 1 d PDU . . N1 N 0.5324(2) 0.2387(2) 0.36935(18) 0.0266(7) Uani 1 1 d . . . N2 N 0.4468(2) 0.2447(3) 0.3626(2) 0.0316(7) Uani 1 1 d . . . N3 N 0.4375(2) 0.2048(2) 0.42782(19) 0.0305(7) Uani 1 1 d . . . N4 N 0.6058(2) 0.1289(3) 0.60296(18) 0.0320(8) Uani 1 1 d . . . H4A H 0.6521 0.1583 0.5958 0.038 Uiso 1 1 calc R . . N5 N 0.51693(18) 0.4983(2) 0.17348(16) 0.0208(6) Uani 1 1 d . . . N6 N 0.53434(19) 0.5276(2) 0.10800(17) 0.0238(7) Uani 1 1 d . . . N7 N 0.49180(19) 0.6168(2) 0.09099(16) 0.0221(6) Uani 1 1 d . . . N8 N 0.38399(19) 0.7776(2) 0.20947(16) 0.0234(7) Uani 1 1 d . . . H8A H 0.3976 0.7453 0.2528 0.028 Uiso 1 1 calc R . . C1 C 0.7851(4) 0.1368(5) 0.2503(4) 0.0703(18) Uani 1 1 d . . . H1A H 0.8396 0.1157 0.2399 0.105 Uiso 1 1 calc R . . H1B H 0.7383 0.0926 0.2227 0.105 Uiso 1 1 calc R . . H1C H 0.7902 0.1312 0.3044 0.105 Uiso 1 1 calc R . . C2 C 0.8339(7) 0.3146(11) 0.2522(9) 0.153(4) Uani 1 1 d U . . H2B H 0.8866 0.2871 0.2420 0.229 Uiso 1 1 calc R . . H2C H 0.8431 0.3237 0.3066 0.229 Uiso 1 1 calc R . . H2D H 0.8201 0.3804 0.2269 0.229 Uiso 1 1 calc R . . C3 C 0.7440(6) 0.2273(9) 0.1318(5) 0.108(3) Uani 1 1 d U . . H3A H 0.7962 0.2026 0.1191 0.162 Uiso 1 1 calc R . . H3B H 0.7255 0.2914 0.1052 0.162 Uiso 1 1 calc R . . H3C H 0.6980 0.1766 0.1166 0.162 Uiso 1 1 calc R . . C4 C 0.7654(4) 0.2469(5) 0.2253(4) 0.0651(18) Uani 1 1 d . . . C5 C 0.6788(3) 0.2862(4) 0.2400(2) 0.0374(10) Uani 1 1 d . . . C6 C 0.6353(2) 0.3706(3) 0.1982(2) 0.0281(8) Uani 1 1 d . . . H6B H 0.6578 0.4019 0.1608 0.034 Uiso 1 1 calc R . . C7 C 0.5582(2) 0.4076(3) 0.2128(2) 0.0230(7) Uani 1 1 d . . . C8 C 0.5216(2) 0.3644(3) 0.2676(2) 0.0243(8) Uani 1 1 d . . . H8B H 0.4694 0.3894 0.2761 0.029 Uiso 1 1 calc R . . C9 C 0.5671(2) 0.2817(3) 0.3094(2) 0.0267(8) Uani 1 1 d . . . C10 C 0.6441(3) 0.2429(3) 0.2971(2) 0.0340(9) Uani 1 1 d . . . H10A H 0.6730 0.1879 0.3267 0.041 Uiso 1 1 calc R . . C11 C 0.5774(3) 0.1949(3) 0.4367(2) 0.0321(9) Uani 1 1 d . . . H11A H 0.6378 0.1827 0.4530 0.039 Uiso 1 1 calc R . . C12 C 0.5152(3) 0.1723(3) 0.4758(2) 0.0292(8) Uani 1 1 d . . . C13 C 0.5248(3) 0.1273(3) 0.5506(2) 0.0285(8) Uani 1 1 d . . . C14 C 0.4689(3) 0.0721(3) 0.5832(2) 0.0377(10) Uani 1 1 d . . . H14A H 0.4097 0.0577 0.5610 0.045 Uiso 1 1 calc R . . C15 C 0.5185(3) 0.0414(3) 0.6569(2) 0.0421(10) Uani 1 1 d . . . H15A H 0.4975 0.0030 0.6921 0.050 Uiso 1 1 calc R . . C16 C 0.6020(3) 0.0771(3) 0.6676(2) 0.0309(9) Uani 1 1 d . . . C17 C 0.6801(3) 0.0701(3) 0.7377(2) 0.0362(10) Uani 1 1 d . . . C18 C 0.7629(3) 0.1178(5) 0.7231(3) 0.0493(12) Uani 1 1 d . . . H18A H 0.7523 0.1896 0.7096 0.074 Uiso 1 1 calc R . . H18B H 0.7781 0.0815 0.6818 0.074 Uiso 1 1 calc R . . H18C H 0.8106 0.1123 0.7688 0.074 Uiso 1 1 calc R . . C19 C 0.6970(5) -0.0451(4) 0.7604(3) 0.0619(16) Uani 1 1 d . . . H19A H 0.6445 -0.0749 0.7693 0.093 Uiso 1 1 calc R . . H19B H 0.7443 -0.0500 0.8063 0.093 Uiso 1 1 calc R . . H19C H 0.7127 -0.0820 0.7195 0.093 Uiso 1 1 calc R . . C20 C 0.4639(2) 0.5674(3) 0.19746(19) 0.0222(7) Uani 1 1 d . . . H20A H 0.4434 0.5628 0.2414 0.027 Uiso 1 1 calc R . . C21 C 0.4469(2) 0.6447(3) 0.14370(19) 0.0216(7) Uani 1 1 d . . . C22 C 0.3994(2) 0.7414(3) 0.14234(19) 0.0230(7) Uani 1 1 d . . . C23 C 0.3660(3) 0.8131(4) 0.0859(2) 0.0428(11) Uani 1 1 d . . . H23A H 0.3666 0.8084 0.0345 0.051 Uiso 1 1 calc R . . C24 C 0.3306(4) 0.8955(4) 0.1206(3) 0.0486(13) Uani 1 1 d . . . H24A H 0.3031 0.9547 0.0959 0.058 Uiso 1 1 calc R . . C25 C 0.3439(3) 0.8722(3) 0.1972(2) 0.0294(8) Uani 1 1 d . . . C26 C 0.3496(3) 0.2034(5) 0.4415(3) 0.0575(14) Uani 1 1 d . . . H26A H 0.3074 0.2306 0.3972 0.086 Uiso 1 1 calc R . . H26B H 0.3496 0.2454 0.4855 0.086 Uiso 1 1 calc R . . H26C H 0.3340 0.1333 0.4506 0.086 Uiso 1 1 calc R . . C27 C 0.4984(3) 0.6724(3) 0.0221(2) 0.0301(8) Uani 1 1 d . . . H27A H 0.5350 0.6337 -0.0032 0.045 Uiso 1 1 calc R . . H27B H 0.5240 0.7396 0.0362 0.045 Uiso 1 1 calc R . . H27C H 0.4406 0.6804 -0.0120 0.045 Uiso 1 1 calc R . . C28 C 0.3131(16) 0.5829(17) 0.5337(12) 0.109(6) Uani 0.50 1 d PU . . H28A H 0.3572 0.6238 0.5684 0.163 Uiso 0.50 1 d PR . . H28B H 0.3274 0.5775 0.4852 0.163 Uiso 0.50 1 d PR . . O1 O 0.2432(12) 0.6229(12) 0.5244(9) 0.123(4) Uani 0.50 1 d PU . . H1D H 0.2045 0.6135 0.4822 0.147 Uiso 0.50 1 d PR . . H28C H 0.3119 0.5146 0.5550 0.184 Uiso 0.50 1 d PR . . O1WA O 0.3258(9) 0.6685(9) 0.4147(6) 0.082(3) Uani 0.50 1 d PU . . O1WB O 0.2669(12) 0.5418(13) 0.5705(9) 0.134(5) Uani 0.50 1 d PU . . O1WC O 0.2827(9) 0.7113(12) 0.4315(9) 0.114(4) Uani 0.50 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.026(2) 0.042(3) 0.034(2) -0.0044(19) 0.0134(17) -0.0008(19) F1 0.0324(13) 0.0551(16) 0.0567(16) 0.0084(13) 0.0220(11) 0.0044(11) F2 0.0348(13) 0.0712(19) 0.0466(15) -0.0130(13) 0.0031(11) 0.0072(13) F3 0.070(2) 0.061(2) 0.070(2) 0.0128(16) 0.0200(16) -0.0197(16) F4 0.0572(18) 0.103(3) 0.0495(17) -0.0414(18) 0.0117(14) -0.0184(17) B2 0.155(10) 0.064(5) 0.055(4) -0.005(4) 0.006(5) -0.013(5) F5 0.135(4) 0.120(4) 0.121(4) -0.056(3) 0.045(3) -0.033(3) F6 0.122(7) 0.165(8) 0.152(7) 0.022(6) 0.009(6) -0.048(6) F6' 0.116(6) 0.075(4) 0.059(4) 0.002(3) 0.009(4) 0.020(4) F7 0.071(3) 0.075(3) 0.052(2) 0.0079(19) 0.0219(19) 0.001(2) F7' 0.058(5) 0.077(6) 0.081(6) 0.014(5) 0.029(5) 0.008(5) F8 0.163(6) 0.074(4) 0.069(4) -0.001(3) 0.040(4) 0.011(4) F8' 0.094(7) 0.065(6) 0.064(6) -0.014(5) 0.007(5) 0.001(6) N1 0.0295(16) 0.0228(15) 0.0286(16) 0.0012(12) 0.0098(13) 0.0024(12) N2 0.0322(17) 0.0275(16) 0.0360(18) 0.0060(13) 0.0106(14) -0.0032(13) N3 0.0307(17) 0.0246(16) 0.0370(18) 0.0042(13) 0.0104(14) -0.0019(13) N4 0.0339(17) 0.0369(18) 0.0284(16) -0.0018(13) 0.0140(13) 0.0062(14) N5 0.0207(14) 0.0195(14) 0.0209(14) -0.0017(11) 0.0031(11) 0.0025(11) N6 0.0240(14) 0.0228(15) 0.0242(15) -0.0022(12) 0.0054(12) 0.0008(12) N7 0.0220(14) 0.0226(14) 0.0216(14) -0.0036(11) 0.0058(11) 0.0018(11) N8 0.0298(15) 0.0228(15) 0.0174(14) 0.0029(11) 0.0058(11) 0.0076(12) C1 0.066(4) 0.080(4) 0.075(4) 0.014(3) 0.036(3) 0.044(3) C2 0.075(5) 0.151(8) 0.240(10) -0.024(7) 0.055(6) 0.022(5) C3 0.112(5) 0.143(7) 0.085(5) 0.032(5) 0.052(4) 0.068(5) C4 0.048(3) 0.075(4) 0.085(4) 0.047(3) 0.042(3) 0.038(3) C5 0.036(2) 0.044(2) 0.033(2) 0.0127(18) 0.0112(17) 0.0192(19) C6 0.0255(18) 0.032(2) 0.0264(18) 0.0026(15) 0.0067(14) 0.0071(15) C7 0.0205(16) 0.0209(17) 0.0253(17) -0.0017(13) 0.0020(13) 0.0030(13) C8 0.0244(17) 0.0195(17) 0.0286(18) -0.0008(14) 0.0061(14) 0.0026(13) C9 0.0283(18) 0.0253(18) 0.0276(18) 0.0008(14) 0.0090(15) 0.0027(14) C10 0.032(2) 0.038(2) 0.033(2) 0.0118(17) 0.0100(16) 0.0135(17) C11 0.033(2) 0.036(2) 0.0278(19) 0.0022(16) 0.0094(15) 0.0081(17) C12 0.038(2) 0.0208(17) 0.0303(19) -0.0062(14) 0.0113(16) 0.0004(15) C13 0.037(2) 0.0235(18) 0.0274(18) -0.0065(14) 0.0130(16) -0.0006(15) C14 0.049(2) 0.034(2) 0.031(2) -0.0058(17) 0.0114(18) -0.0124(18) C15 0.064(3) 0.033(2) 0.030(2) -0.0001(17) 0.0143(19) -0.012(2) C16 0.048(2) 0.0231(18) 0.0254(18) -0.0054(14) 0.0159(16) 0.0055(16) C17 0.050(2) 0.035(2) 0.0260(19) -0.0034(16) 0.0139(17) 0.0186(18) C18 0.040(2) 0.077(3) 0.034(2) -0.010(2) 0.0138(19) 0.016(2) C19 0.097(4) 0.039(3) 0.050(3) -0.003(2) 0.020(3) 0.039(3) C20 0.0217(16) 0.0241(17) 0.0215(16) -0.0023(13) 0.0068(13) 0.0042(13) C21 0.0189(15) 0.0244(17) 0.0202(16) -0.0034(13) 0.0029(12) 0.0014(13) C22 0.0267(17) 0.0245(17) 0.0183(16) -0.0004(13) 0.0066(13) 0.0066(14) C23 0.061(3) 0.049(3) 0.0231(19) 0.0087(18) 0.0184(18) 0.027(2) C24 0.078(3) 0.040(2) 0.035(2) 0.0191(19) 0.029(2) 0.038(2) C25 0.037(2) 0.0265(19) 0.0255(18) 0.0010(15) 0.0099(15) 0.0132(16) C26 0.033(2) 0.072(4) 0.070(3) 0.031(3) 0.017(2) -0.001(2) C27 0.036(2) 0.0307(19) 0.0261(19) 0.0007(15) 0.0118(15) 0.0026(16) C28 0.124(10) 0.102(9) 0.102(9) 0.026(7) 0.032(8) -0.026(8) O1 0.141(9) 0.110(8) 0.120(8) 0.002(7) 0.040(7) 0.000(7) O1WA 0.100(7) 0.076(6) 0.070(5) -0.008(4) 0.019(5) -0.006(5) O1WB 0.157(9) 0.124(8) 0.114(8) 0.007(7) 0.023(7) -0.032(7) O1WC 0.080(6) 0.112(8) 0.131(8) 0.002(7) -0.007(6) 0.017(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 F3 1.374(6) . ? B1 F1 1.381(5) . ? B1 F4 1.384(6) . ? B1 F2 1.395(5) . ? B2 F8 1.304(8) . ? B2 F8' 1.314(8) . ? B2 F7 1.367(7) . ? B2 F5 1.380(9) . ? B2 F7' 1.388(8) . ? B2 F6 1.423(8) . ? B2 F6' 1.436(8) . ? F6 F8' 1.589(14) . ? N1 N2 1.320(5) . ? N1 C11 1.358(5) . ? N1 C9 1.441(5) . ? N2 N3 1.325(5) . ? N3 C12 1.364(5) . ? N3 C26 1.464(6) . ? N4 C16 1.356(5) . ? N4 C13 1.372(5) . ? N4 H4A 0.8600 . ? N5 N6 1.333(4) . ? N5 C20 1.363(4) . ? N5 C7 1.430(4) . ? N6 N7 1.323(4) . ? N7 C21 1.370(4) . ? N7 C27 1.459(5) . ? N8 C25 1.363(5) . ? N8 C22 1.375(4) . ? N8 H8A 0.8600 . ? C1 C4 1.495(8) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C4 1.371(14) . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C2 H2D 0.9600 . ? C3 C4 1.651(11) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.537(6) . ? C5 C6 1.395(6) . ? C5 C10 1.400(6) . ? C6 C7 1.388(5) . ? C6 H6B 0.9300 . ? C7 C8 1.382(5) . ? C8 C9 1.389(5) . ? C8 H8B 0.9300 . ? C9 C10 1.379(5) . ? C10 H10A 0.9300 . ? C11 C12 1.376(6) . ? C11 H11A 0.9300 . ? C12 C13 1.438(6) . ? C13 C14 1.375(6) . ? C14 C15 1.410(6) . ? C14 H14A 0.9300 . ? C15 C16 1.354(6) . ? C15 H15A 0.9300 . ? C16 C17 1.518(6) . ? C17 C25 1.517(5) 3_666 ? C17 C18 1.520(7) . ? C17 C19 1.541(6) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.366(5) . ? C20 H20A 0.9300 . ? C21 C22 1.447(5) . ? C22 C23 1.373(6) . ? C23 C24 1.416(6) . ? C23 H23A 0.9300 . ? C24 C25 1.374(6) . ? C24 H24A 0.9300 . ? C25 C17 1.517(5) 3_666 ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 O1 1.18(2) . ? C28 H28A 0.9601 . ? C28 H28B 0.9600 . ? C28 H28C 0.9606 . ? O1 H1D 0.8500 . ? O1WB H28C 0.8948 . ? 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 F3 B1 F1 109.5(4) . . ? F3 B1 F4 112.6(4) . . ? F1 B1 F4 109.0(4) . . ? F3 B1 F2 108.2(4) . . ? F1 B1 F2 108.5(3) . . ? F4 B1 F2 109.0(4) . . ? F8 B2 F8' 45.2(6) . . ? F8 B2 F7 114.5(7) . . ? F8' B2 F7 146.4(8) . . ? F8 B2 F5 113.7(6) . . ? F8' B2 F5 112.5(7) . . ? F7 B2 F5 100.2(5) . . ? F8 B2 F7' 66.9(7) . . ? F8' B2 F7' 112.1(8) . . ? F7 B2 F7' 57.1(5) . . ? F5 B2 F7' 92.3(8) . . ? F8 B2 F6 113.3(7) . . ? F8' B2 F6 70.9(8) . . ? F7 B2 F6 108.6(6) . . ? F5 B2 F6 105.4(7) . . ? F7' B2 F6 159.6(9) . . ? F8 B2 F6' 120.3(7) . . ? F8' B2 F6' 109.0(7) . . ? F7 B2 F6' 52.6(4) . . ? F5 B2 F6' 125.7(6) . . ? F7' B2 F6' 103.1(6) . . ? F6 B2 F6' 58.2(6) . . ? B2 F6 F8' 51.4(5) . . ? B2 F8' F6 57.8(6) . . ? N2 N1 C11 112.8(3) . . ? N2 N1 C9 118.8(3) . . ? C11 N1 C9 128.2(3) . . ? N1 N2 N3 103.8(3) . . ? N2 N3 C12 113.3(3) . . ? N2 N3 C26 118.6(3) . . ? C12 N3 C26 128.0(4) . . ? C16 N4 C13 110.1(3) . . ? C16 N4 H4A 124.9 . . ? C13 N4 H4A 124.9 . . ? N6 N5 C20 112.3(3) . . ? N6 N5 C7 119.9(3) . . ? C20 N5 C7 127.6(3) . . ? N7 N6 N5 104.1(3) . . ? N6 N7 C21 112.8(3) . . ? N6 N7 C27 118.6(3) . . ? C21 N7 C27 128.6(3) . . ? C25 N8 C22 109.8(3) . . ? C25 N8 H8A 125.1 . . ? C22 N8 H8A 125.1 . . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C2 H2D 109.5 . . ? H2B C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C1 114.5(7) . . ? C2 C4 C5 112.2(7) . . ? C1 C4 C5 112.6(4) . . ? C2 C4 C3 113.0(8) . . ? C1 C4 C3 97.7(6) . . ? C5 C4 C3 105.7(5) . . ? C6 C5 C10 118.5(4) . . ? C6 C5 C4 119.7(4) . . ? C10 C5 C4 121.7(4) . . ? C7 C6 C5 119.6(4) . . ? C7 C6 H6B 120.2 . . ? C5 C6 H6B 120.2 . . ? C8 C7 C6 122.9(3) . . ? C8 C7 N5 117.6(3) . . ? C6 C7 N5 119.4(3) . . ? C7 C8 C9 116.4(3) . . ? C7 C8 H8B 121.8 . . ? C9 C8 H8B 121.8 . . ? C10 C9 C8 122.6(3) . . ? C10 C9 N1 120.0(3) . . ? C8 C9 N1 117.4(3) . . ? C9 C10 C5 120.0(4) . . ? C9 C10 H10A 120.0 . . ? C5 C10 H10A 120.0 . . ? N1 C11 C12 105.8(3) . . ? N1 C11 H11A 127.1 . . ? C12 C11 H11A 127.1 . . ? N3 C12 C11 104.3(3) . . ? N3 C12 C13 125.2(4) . . ? C11 C12 C13 130.5(4) . . ? N4 C13 C14 107.1(3) . . ? N4 C13 C12 119.5(3) . . ? C14 C13 C12 133.2(4) . . ? C13 C14 C15 106.8(4) . . ? C13 C14 H14A 126.6 . . ? C15 C14 H14A 126.6 . . ? C16 C15 C14 108.5(4) . . ? C16 C15 H15A 125.7 . . ? C14 C15 H15A 125.7 . . ? C15 C16 N4 107.5(4) . . ? C15 C16 C17 129.9(4) . . ? N4 C16 C17 122.5(4) . . ? C25 C17 C16 107.7(3) 3_666 . ? C25 C17 C18 109.4(4) 3_666 . ? C16 C17 C18 112.0(4) . . ? C25 C17 C19 109.0(3) 3_666 . ? C16 C17 C19 108.9(4) . . ? C18 C17 C19 109.8(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N5 C20 C21 105.8(3) . . ? N5 C20 H20A 127.1 . . ? C21 C20 H20A 127.1 . . ? C20 C21 N7 105.1(3) . . ? C20 C21 C22 130.0(3) . . ? N7 C21 C22 124.7(3) . . ? C23 C22 N8 107.7(3) . . ? C23 C22 C21 133.3(3) . . ? N8 C22 C21 119.0(3) . . ? C22 C23 C24 107.1(3) . . ? C22 C23 H23A 126.4 . . ? C24 C23 H23A 126.4 . . ? C25 C24 C23 107.8(3) . . ? C25 C24 H24A 126.1 . . ? C23 C24 H24A 126.1 . . ? N8 C25 C24 107.5(3) . . ? N8 C25 C17 120.6(3) . 3_666 ? C24 C25 C17 131.8(3) . 3_666 ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N7 C27 H27A 109.5 . . ? N7 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N7 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O1 C28 H28A 109.8 . . ? O1 C28 H28B 109.3 . . ? H28A C28 H28B 109.5 . . ? O1 C28 H28C 109.9 . . ? H28A C28 H28C 109.1 . . ? H28B C28 H28C 109.3 . . ? C28 O1 H1D 119.0 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.495 _refine_diff_density_min -0.921 _refine_diff_density_rms 0.107 data_ys _database_code_depnum_ccdc_archive 'CCDC 849577' #TrackingRef 'BF4-TBA3HP2O7.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H64 N16, O7 P2, B F4' _chemical_formula_sum 'C54 H64 B F4 N16 O7 P2' _chemical_formula_weight 1197.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' 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 19.726(9) _cell_length_b 15.697(6) _cell_length_c 22.564(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.404(6) _cell_angle_gamma 90.00 _cell_volume 6849(5) _cell_formula_units_Z 4 _cell_measurement_temperature 113(1) _cell_measurement_reflns_used 8340 _cell_measurement_theta_min 1.4724 _cell_measurement_theta_max 31.1603 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2508 _exptl_absorpt_coefficient_mu 0.131 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5453 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(1) _diffrn_radiation_wavelength 0.710747 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Sealed tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48618 _diffrn_reflns_av_R_equivalents 0.0731 _diffrn_reflns_av_sigmaI/netI 0.1026 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11993 _reflns_number_gt 5836 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _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. Some MeOH and H2O molecules arround the macrocycle were found to be badly disordered. Attempts to model the disorder were unsatisfactory. The contributions to the scattering factors due to these solvent molecules were removed by use of the utility SQUEEZE (Sluis and Spek, 1990) in PLATON98 (Spek, 1998). PLATON98 was used as incorporated in WinGX (Farrugia, 1999). ISOR was applied to the PO3 group of P2O7 anion to allow their Uij components approximate to isotropic behavior. ; _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^)+(0.1571P)^2^+0.0000P] 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 11993 _refine_ls_number_parameters 785 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.1617 _refine_ls_R_factor_gt 0.0924 _refine_ls_wR_factor_ref 0.2684 _refine_ls_wR_factor_gt 0.2326 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.968 _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 0.24569(8) 0.87901(11) 0.04759(6) 0.0608(4) Uani 1 1 d . . . P2 P 0.27232(8) 0.92977(9) -0.07069(6) 0.0525(4) Uani 1 1 d . . . O1 O 0.2761(5) 0.8009(5) 0.0355(3) 0.082(3) Uani 0.588(6) 1 d PU A 1 O2 O 0.1769(4) 0.8832(5) 0.0607(3) 0.071(2) Uani 0.588(6) 1 d PU A 1 O3 O 0.2965(3) 0.9320(3) 0.1005(2) 0.0507(18) Uani 0.588(6) 1 d PU A 1 O1' O 0.3167(5) 0.8442(5) 0.0575(4) 0.048(2) Uani 0.412(6) 1 d PU A 2 O2' O 0.2202(4) 0.9212(5) 0.0898(4) 0.046(3) Uani 0.412(6) 1 d PU A 2 O3' O 0.1908(5) 0.7927(6) 0.0247(4) 0.074(3) Uani 0.412(6) 1 d PU A 2 O4 O 0.23939(19) 0.9377(2) -0.01237(14) 0.0596(10) Uani 1 1 d . A . O5 O 0.34447(18) 0.9618(2) -0.05745(15) 0.0631(10) Uani 1 1 d . A . O6 O 0.2701(2) 0.8298(2) -0.08476(17) 0.0737(12) Uani 1 1 d . A . O7 O 0.22250(18) 0.9712(2) -0.12062(14) 0.0541(9) Uani 1 1 d . A . B1 B 0.4555(6) 0.3223(9) 0.1059(5) 0.113(3) Uani 1 1 d . . . F1 F 0.4940(3) 0.3018(3) 0.0670(2) 0.1423(19) Uani 1 1 d . . . F4 F 0.4985(3) 0.3516(4) 0.1605(2) 0.149(2) Uani 1 1 d . . . F3 F 0.4096(3) 0.3865(4) 0.0850(3) 0.182(3) Uani 1 1 d . . . F2 F 0.4202(4) 0.2560(5) 0.1208(3) 0.186(3) Uani 1 1 d . . . N1 N 0.5338(2) 0.8361(2) 0.02082(17) 0.0443(10) Uani 1 1 d . . . N2 N 0.5981(2) 0.8415(3) 0.01084(19) 0.0564(11) Uani 1 1 d . . . N3 N 0.5918(2) 0.8909(3) -0.03718(19) 0.0538(11) Uani 1 1 d . . . N4 N 0.4383(2) 0.9974(2) -0.12935(17) 0.0459(10) Uani 1 1 d . . . H4A H 0.4068 0.9918 -0.1081 0.055 Uiso 1 1 calc R . . N5 N 0.2682(2) 0.9582(2) -0.22881(17) 0.0453(10) Uani 1 1 d . . . H5A H 0.2550 0.9697 -0.1956 0.054 Uiso 1 1 calc R . . N6 N 0.1452(2) 0.7885(2) -0.29658(18) 0.0510(11) Uani 1 1 d . . . N7 N 0.0968(2) 0.7503(3) -0.27353(18) 0.0549(11) Uani 1 1 d . . . N8 N 0.1042(2) 0.7812(2) -0.21796(18) 0.0479(10) Uani 1 1 d . . . N9 N -0.0078(2) 0.8284(2) -0.04739(18) 0.0509(10) Uani 1 1 d . . . N10 N -0.0713(2) 0.8503(3) -0.0458(2) 0.0582(11) Uani 1 1 d . . . N11 N -0.0659(2) 0.8938(3) 0.0047(2) 0.0580(11) Uani 1 1 d . . . N12 N 0.0890(2) 0.9573(2) 0.11871(17) 0.0446(10) Uani 1 1 d . . . H12A H 0.1234 0.9392 0.1040 0.054 Uiso 1 1 calc R . . N13 N 0.2550(2) 0.9151(2) 0.21273(17) 0.0440(10) Uani 1 1 d . . . H13A H 0.2651 0.9286 0.1786 0.053 Uiso 1 1 calc R . . N14 N 0.3869(2) 0.7489(2) 0.26989(18) 0.0495(10) Uani 1 1 d . . . N15 N 0.4365(2) 0.7201(2) 0.24446(17) 0.0500(10) Uani 1 1 d . . . N16 N 0.4270(2) 0.7596(2) 0.19154(16) 0.0426(9) Uani 1 1 d . . . C1 C 0.5576(5) 0.5019(7) 0.0878(5) 0.218(6) Uani 1 1 d DU . . H1B H 0.5705 0.4457 0.1027 0.327 Uiso 1 1 calc R . . H1C H 0.5656 0.5075 0.0474 0.327 Uiso 1 1 calc R . . H1D H 0.5095 0.5111 0.0877 0.327 Uiso 1 1 calc R . . C2 C 0.6158(5) 0.5404(5) 0.1934(3) 0.147(4) Uani 1 1 d DU . . H2C H 0.6433 0.4895 0.1972 0.221 Uiso 1 1 calc R . . H2D H 0.5729 0.5290 0.2058 0.221 Uiso 1 1 calc R . . H2E H 0.6404 0.5842 0.2185 0.221 Uiso 1 1 calc R . . C3 C 0.6684(4) 0.5803(6) 0.1071(4) 0.163(4) Uani 1 1 d DU . . H3B H 0.6945 0.5283 0.1130 0.245 Uiso 1 1 calc R . . H3C H 0.6949 0.6254 0.1293 0.245 Uiso 1 1 calc R . . H3D H 0.6583 0.5944 0.0649 0.245 Uiso 1 1 calc R . . C4 C 0.6017(4) 0.5691(4) 0.1293(3) 0.0785(18) Uani 1 1 d U . . C5 C 0.5575(3) 0.6487(3) 0.1211(2) 0.0554(14) Uani 1 1 d . . . C6 C 0.5616(3) 0.7048(3) 0.0751(2) 0.0533(13) Uani 1 1 d . . . H6A H 0.5905 0.6927 0.0482 0.064 Uiso 1 1 calc R . . C7 C 0.5232(3) 0.7789(3) 0.0684(2) 0.0464(12) Uani 1 1 d . . . C8 C 0.4888(3) 0.8827(3) -0.0194(2) 0.0455(12) Uani 1 1 d . . . H8A H 0.4418 0.8895 -0.0204 0.055 Uiso 1 1 calc R . . C9 C 0.5264(2) 0.9181(3) -0.0587(2) 0.0428(11) Uani 1 1 d . . . C10 C 0.6552(3) 0.9064(5) -0.0605(3) 0.092(2) Uani 1 1 d . . . H10B H 0.6933 0.8775 -0.0354 0.138 Uiso 1 1 calc R . . H10C H 0.6645 0.9665 -0.0601 0.138 Uiso 1 1 calc R . . H10D H 0.6493 0.8854 -0.1011 0.138 Uiso 1 1 calc R . . C11 C 0.5052(2) 0.9680(3) -0.1129(2) 0.0443(12) Uani 1 1 d . . . C12 C 0.5388(3) 0.9909(3) -0.1585(2) 0.0509(13) Uani 1 1 d . . . H12B H 0.5848 0.9795 -0.1596 0.061 Uiso 1 1 calc R . . C13 C 0.4918(3) 1.0342(3) -0.2028(2) 0.0507(13) Uani 1 1 d . . . H13B H 0.5011 1.0572 -0.2384 0.061 Uiso 1 1 calc R . . C14 C 0.4293(3) 1.0368(3) -0.1844(2) 0.0481(12) Uani 1 1 d . . . C15 C 0.3604(3) 1.0732(3) -0.2170(2) 0.0558(13) Uani 1 1 d . . . C16 C 0.3224(3) 1.1160(3) -0.1723(2) 0.0597(14) Uani 1 1 d . . . H16A H 0.3140 1.0749 -0.1431 0.090 Uiso 1 1 calc R . . H16B H 0.2792 1.1384 -0.1936 0.090 Uiso 1 1 calc R . . H16C H 0.3502 1.1615 -0.1520 0.090 Uiso 1 1 calc R . . C17 C 0.3737(3) 1.1388(4) -0.2641(3) 0.0823(19) Uani 1 1 d . . . H17A H 0.3972 1.1117 -0.2924 0.123 Uiso 1 1 calc R . . H17B H 0.4018 1.1843 -0.2441 0.123 Uiso 1 1 calc R . . H17C H 0.3304 1.1614 -0.2852 0.123 Uiso 1 1 calc R . . C18 C 0.3194(3) 0.9998(3) -0.2501(2) 0.0524(13) Uani 1 1 d . . . C19 C 0.3243(3) 0.9613(4) -0.3047(2) 0.0606(15) Uani 1 1 d . . . H19A H 0.3551 0.9765 -0.3293 0.073 Uiso 1 1 calc R . . C20 C 0.2755(3) 0.8964(4) -0.3164(2) 0.0549(13) Uani 1 1 d . . . H20A H 0.2678 0.8608 -0.3500 0.066 Uiso 1 1 calc R . . C21 C 0.2409(2) 0.8944(3) -0.2693(2) 0.0420(11) Uani 1 1 d . . . C22 C 0.1845(2) 0.8442(3) -0.2566(2) 0.0430(11) Uani 1 1 d . . . C23 C 0.1568(2) 0.8374(3) -0.2059(2) 0.0472(12) Uani 1 1 d . . . H23A H 0.1716 0.8663 -0.1697 0.057 Uiso 1 1 calc R . . C24 C 0.1497(3) 0.7691(4) -0.3585(3) 0.0804(19) Uani 1 1 d . . . H24A H 0.1151 0.7277 -0.3746 0.121 Uiso 1 1 calc R . . H24B H 0.1947 0.7465 -0.3595 0.121 Uiso 1 1 calc R . . H24C H 0.1422 0.8201 -0.3823 0.121 Uiso 1 1 calc R . . C25 C 0.0568(3) 0.7561(3) -0.1809(2) 0.0478(12) Uani 1 1 d . . . C26 C 0.0535(3) 0.8013(3) -0.1287(2) 0.0475(12) Uani 1 1 d . . . H26A H 0.0848 0.8446 -0.1150 0.057 Uiso 1 1 calc R . . C27 C 0.0030(3) 0.7799(3) -0.0984(2) 0.0515(13) Uani 1 1 d . . . C28 C -0.0430(3) 0.7126(3) -0.1165(2) 0.0588(14) Uani 1 1 d . . . H28A H -0.0763 0.6990 -0.0941 0.071 Uiso 1 1 calc R . . C29 C -0.0387(3) 0.6659(3) -0.1684(3) 0.0617(14) Uani 1 1 d . . . C30 C 0.0121(3) 0.6895(3) -0.1999(2) 0.0569(14) Uani 1 1 d . . . H30A H 0.0161 0.6597 -0.2347 0.068 Uiso 1 1 calc R . . C31 C -0.0893(3) 0.5935(4) -0.1903(3) 0.082(2) Uani 1 1 d . . . C32 C -0.1170(3) 0.6013(5) -0.2573(3) 0.099(2) Uani 1 1 d . . . H32A H -0.1437 0.6526 -0.2653 0.148 Uiso 1 1 calc R . . H32B H -0.1457 0.5531 -0.2710 0.148 Uiso 1 1 calc R . . H32C H -0.0791 0.6032 -0.2782 0.148 Uiso 1 1 calc R . . C33 C -0.1483(4) 0.5895(5) -0.1556(4) 0.131(4) Uani 1 1 d . . . H33A H -0.1753 0.6407 -0.1627 0.196 Uiso 1 1 calc R . . H33B H -0.1295 0.5840 -0.1131 0.196 Uiso 1 1 calc R . . H33C H -0.1771 0.5412 -0.1691 0.196 Uiso 1 1 calc R . . C34 C -0.0471(4) 0.5095(4) -0.1781(4) 0.108(3) Uani 1 1 d . . . H34A H -0.0094 0.5108 -0.1992 0.162 Uiso 1 1 calc R . . H34B H -0.0765 0.4619 -0.1919 0.162 Uiso 1 1 calc R . . H34C H -0.0292 0.5039 -0.1355 0.162 Uiso 1 1 calc R . . C35 C 0.0384(3) 0.8574(3) 0.0007(2) 0.0534(13) Uani 1 1 d . . . H35A H 0.0861 0.8497 0.0081 0.064 Uiso 1 1 calc R . . C36 C 0.0012(3) 0.9005(3) 0.0362(2) 0.0475(12) Uani 1 1 d . . . C37 C -0.1297(3) 0.9308(4) 0.0175(3) 0.088(2) Uani 1 1 d . . . H37A H -0.1682 0.9139 -0.0134 0.132 Uiso 1 1 calc R . . H37B H -0.1261 0.9918 0.0182 0.132 Uiso 1 1 calc R . . H37C H -0.1368 0.9108 0.0560 0.132 Uiso 1 1 calc R . . C38 C 0.0210(3) 0.9455(3) 0.0930(2) 0.0447(12) Uani 1 1 d . . . C39 C -0.0184(3) 0.9804(3) 0.1307(3) 0.0619(15) Uani 1 1 d . . . H39A H -0.0663 0.9801 0.1252 0.074 Uiso 1 1 calc R . . C40 C 0.0285(3) 1.0168(3) 0.1794(2) 0.0561(14) Uani 1 1 d . . . H40A H 0.0165 1.0460 0.2117 0.067 Uiso 1 1 calc R . . C41 C 0.0942(3) 1.0023(3) 0.1716(2) 0.0471(12) Uani 1 1 d . . . C42 C 0.1630(3) 1.0289(3) 0.2094(2) 0.0473(12) Uani 1 1 d . . . C43 C 0.1483(3) 1.0882(4) 0.2601(3) 0.0746(17) Uani 1 1 d . . . H43A H 0.1226 1.0576 0.2852 0.112 Uiso 1 1 calc R . . H43B H 0.1219 1.1364 0.2425 0.112 Uiso 1 1 calc R . . H43C H 0.1913 1.1074 0.2842 0.112 Uiso 1 1 calc R . . C44 C 0.2037(3) 1.0800(3) 0.1699(3) 0.0628(15) Uani 1 1 d . . . H44A H 0.2132 1.0443 0.1379 0.094 Uiso 1 1 calc R . . H44B H 0.2464 1.0993 0.1942 0.094 Uiso 1 1 calc R . . H44C H 0.1768 1.1282 0.1528 0.094 Uiso 1 1 calc R . . C45 C 0.2047(3) 0.9531(3) 0.2377(2) 0.0498(12) Uani 1 1 d . . . C46 C 0.2047(3) 0.9132(3) 0.2920(2) 0.0574(14) Uani 1 1 d . . . H46A H 0.1757 0.9262 0.3187 0.069 Uiso 1 1 calc R . . C47 C 0.2558(3) 0.8495(3) 0.3003(2) 0.0537(13) Uani 1 1 d . . . H47A H 0.2666 0.8127 0.3332 0.064 Uiso 1 1 calc R . . C48 C 0.2869(3) 0.8517(3) 0.2510(2) 0.0426(11) Uani 1 1 d . . . C49 C 0.3453(3) 0.8081(3) 0.2347(2) 0.0439(12) Uani 1 1 d . . . C50 C 0.3722(3) 0.8135(3) 0.1836(2) 0.0447(12) Uani 1 1 d . . . H50A H 0.3562 0.8474 0.1500 0.054 Uiso 1 1 calc R . . C51 C 0.3842(3) 0.7176(4) 0.3304(2) 0.0678(16) Uani 1 1 d . . . H51A H 0.4207 0.6770 0.3428 0.102 Uiso 1 1 calc R . . H51B H 0.3404 0.6907 0.3297 0.102 Uiso 1 1 calc R . . H51C H 0.3898 0.7645 0.3582 0.102 Uiso 1 1 calc R . . C52 C 0.4731(3) 0.7424(3) 0.1504(2) 0.0469(12) Uani 1 1 d . . . C53 C 0.4782(3) 0.8001(3) 0.1053(2) 0.0456(12) Uani 1 1 d . . . H53A H 0.4526 0.8503 0.1002 0.055 Uiso 1 1 calc R . . C54 C 0.5118(3) 0.6679(3) 0.1588(2) 0.0546(13) Uani 1 1 d . . . H54A H 0.5071 0.6307 0.1898 0.066 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 0.0459(9) 0.0924(12) 0.0449(8) 0.0108(8) 0.0111(7) 0.0104(8) P2 0.0519(9) 0.0672(9) 0.0393(7) 0.0035(6) 0.0110(7) 0.0186(7) O1 0.091(6) 0.062(4) 0.086(5) -0.023(4) -0.001(4) 0.015(4) O2 0.049(4) 0.104(5) 0.058(4) -0.027(4) 0.009(3) -0.012(4) O3 0.052(4) 0.058(3) 0.035(3) 0.002(2) -0.009(3) -0.007(3) O1' 0.042(5) 0.049(5) 0.052(5) -0.002(4) 0.003(4) 0.006(4) O2' 0.046(5) 0.054(5) 0.038(4) 0.000(4) 0.006(4) -0.006(4) O3' 0.052(6) 0.102(6) 0.072(6) 0.015(5) 0.020(5) 0.009(5) O4 0.061(2) 0.075(2) 0.042(2) 0.0081(17) 0.0092(18) 0.0238(19) O5 0.042(2) 0.095(3) 0.051(2) 0.0147(19) 0.0067(18) 0.0175(19) O6 0.083(3) 0.073(2) 0.067(3) 0.008(2) 0.020(2) 0.025(2) O7 0.057(2) 0.066(2) 0.0353(18) 0.0004(16) -0.0006(16) 0.0187(17) B1 0.098(8) 0.157(11) 0.081(7) -0.034(7) 0.011(6) 0.035(8) F1 0.162(5) 0.156(4) 0.096(3) -0.043(3) -0.007(3) 0.048(4) F4 0.138(4) 0.197(5) 0.102(4) -0.059(3) -0.002(3) 0.032(4) F3 0.146(5) 0.215(6) 0.174(6) -0.006(5) 0.001(4) 0.085(5) F2 0.210(7) 0.180(6) 0.174(6) -0.078(5) 0.054(5) -0.018(5) N1 0.040(3) 0.049(2) 0.039(2) -0.0078(19) -0.0052(19) 0.0095(19) N2 0.039(3) 0.079(3) 0.047(3) 0.003(2) -0.005(2) 0.008(2) N3 0.035(3) 0.076(3) 0.048(3) 0.002(2) 0.002(2) 0.009(2) N4 0.038(2) 0.062(2) 0.035(2) 0.0031(19) -0.0001(18) -0.004(2) N5 0.035(2) 0.062(2) 0.037(2) 0.0023(19) 0.0012(19) 0.004(2) N6 0.056(3) 0.046(2) 0.047(2) 0.007(2) 0.000(2) 0.001(2) N7 0.062(3) 0.058(3) 0.042(2) 0.000(2) 0.002(2) -0.002(2) N8 0.041(3) 0.052(2) 0.045(2) 0.000(2) -0.005(2) 0.002(2) N9 0.048(3) 0.049(2) 0.050(3) -0.004(2) -0.002(2) -0.009(2) N10 0.049(3) 0.057(3) 0.063(3) -0.014(2) -0.003(2) 0.006(2) N11 0.048(3) 0.056(3) 0.063(3) -0.008(2) -0.005(2) 0.014(2) N12 0.039(3) 0.053(2) 0.042(2) 0.0002(19) 0.007(2) 0.0047(19) N13 0.044(3) 0.050(2) 0.036(2) -0.0028(18) 0.0024(19) -0.0071(19) N14 0.047(3) 0.053(2) 0.042(2) 0.008(2) -0.006(2) -0.006(2) N15 0.047(3) 0.058(3) 0.038(2) 0.012(2) -0.007(2) -0.006(2) N16 0.048(3) 0.037(2) 0.037(2) 0.0038(17) -0.0064(19) 0.0006(18) C1 0.234(10) 0.132(7) 0.259(10) -0.048(7) -0.021(8) 0.068(7) C2 0.163(7) 0.154(6) 0.130(6) 0.062(5) 0.042(5) 0.109(6) C3 0.152(7) 0.170(7) 0.179(7) 0.058(6) 0.058(6) 0.109(6) C4 0.092(5) 0.060(3) 0.073(4) 0.005(3) -0.009(3) 0.026(3) C5 0.059(4) 0.043(3) 0.053(3) -0.004(2) -0.015(3) 0.019(3) C6 0.055(3) 0.055(3) 0.043(3) -0.005(2) -0.007(2) 0.020(3) C7 0.050(3) 0.048(3) 0.036(3) 0.002(2) -0.005(2) 0.007(2) C8 0.040(3) 0.049(3) 0.041(3) -0.006(2) -0.008(2) 0.011(2) C9 0.038(3) 0.048(3) 0.040(3) -0.009(2) 0.000(2) 0.004(2) C10 0.039(4) 0.170(7) 0.067(4) 0.017(4) 0.007(3) 0.024(4) C11 0.037(3) 0.051(3) 0.040(3) -0.005(2) -0.004(2) 0.005(2) C12 0.041(3) 0.062(3) 0.047(3) -0.009(2) 0.005(3) -0.005(3) C13 0.052(3) 0.054(3) 0.042(3) 0.005(2) -0.002(3) -0.011(2) C14 0.042(3) 0.060(3) 0.039(3) -0.001(2) -0.002(2) -0.014(2) C15 0.043(3) 0.067(3) 0.050(3) 0.009(3) -0.007(3) -0.002(3) C16 0.046(3) 0.057(3) 0.064(3) 0.010(3) -0.020(3) -0.003(3) C17 0.064(4) 0.102(5) 0.071(4) 0.032(4) -0.011(3) -0.018(3) C18 0.039(3) 0.072(3) 0.039(3) 0.014(3) -0.009(2) 0.005(3) C19 0.041(3) 0.098(4) 0.041(3) 0.003(3) 0.004(3) -0.008(3) C20 0.041(3) 0.080(4) 0.039(3) -0.006(3) -0.002(2) 0.006(3) C21 0.029(3) 0.048(3) 0.044(3) 0.000(2) -0.004(2) 0.006(2) C22 0.045(3) 0.038(3) 0.040(3) 0.002(2) -0.005(2) 0.007(2) C23 0.038(3) 0.048(3) 0.050(3) -0.003(2) -0.006(2) -0.004(2) C24 0.093(5) 0.096(5) 0.052(4) -0.022(3) 0.014(3) -0.028(4) C25 0.039(3) 0.051(3) 0.044(3) 0.001(2) -0.014(2) -0.001(2) C26 0.046(3) 0.046(3) 0.045(3) -0.001(2) -0.005(2) -0.011(2) C27 0.053(3) 0.054(3) 0.041(3) -0.012(2) -0.007(3) -0.008(3) C28 0.052(4) 0.063(3) 0.056(3) -0.003(3) -0.003(3) -0.010(3) C29 0.049(4) 0.064(3) 0.065(4) -0.012(3) -0.004(3) -0.015(3) C30 0.043(3) 0.064(3) 0.060(3) -0.006(3) 0.001(3) -0.007(3) C31 0.066(4) 0.088(5) 0.092(5) -0.041(4) 0.019(4) -0.037(4) C32 0.060(4) 0.135(6) 0.095(5) -0.058(5) 0.001(4) -0.033(4) C33 0.092(6) 0.152(7) 0.165(8) -0.098(6) 0.065(6) -0.078(5) C34 0.122(7) 0.083(5) 0.124(7) -0.031(4) 0.039(6) -0.045(5) C35 0.053(3) 0.058(3) 0.047(3) -0.001(3) 0.004(3) -0.013(3) C36 0.042(3) 0.054(3) 0.044(3) 0.009(2) 0.001(2) -0.003(2) C37 0.048(4) 0.108(5) 0.096(5) -0.030(4) -0.015(3) 0.019(4) C38 0.042(3) 0.050(3) 0.042(3) 0.004(2) 0.007(2) 0.006(2) C39 0.041(3) 0.073(4) 0.066(4) 0.009(3) -0.003(3) 0.006(3) C40 0.047(3) 0.074(4) 0.047(3) -0.006(3) 0.008(3) 0.013(3) C41 0.053(3) 0.045(3) 0.041(3) -0.001(2) 0.004(2) 0.003(2) C42 0.044(3) 0.054(3) 0.040(3) -0.009(2) -0.001(2) -0.004(2) C43 0.082(5) 0.074(4) 0.058(4) -0.015(3) -0.008(3) 0.004(3) C44 0.061(4) 0.053(3) 0.070(4) 0.010(3) 0.002(3) -0.005(3) C45 0.047(3) 0.052(3) 0.045(3) 0.005(2) -0.002(2) -0.012(2) C46 0.050(4) 0.075(4) 0.046(3) 0.012(3) 0.007(3) -0.011(3) C47 0.040(3) 0.060(3) 0.054(3) 0.009(3) -0.007(3) -0.011(3) C48 0.044(3) 0.038(2) 0.040(3) 0.001(2) -0.005(2) -0.017(2) C49 0.044(3) 0.038(2) 0.043(3) -0.001(2) -0.008(2) -0.011(2) C50 0.053(3) 0.039(3) 0.036(3) 0.003(2) -0.006(2) -0.002(2) C51 0.062(4) 0.078(4) 0.059(4) 0.028(3) 0.001(3) 0.010(3) C52 0.049(3) 0.043(3) 0.040(3) -0.007(2) -0.013(2) 0.000(2) C53 0.051(3) 0.039(3) 0.039(3) 0.001(2) -0.012(2) 0.007(2) C54 0.066(4) 0.041(3) 0.046(3) 0.004(2) -0.014(3) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O2' 1.337(8) . ? P1 O1 1.415(7) . ? P1 O2 1.446(6) . ? P1 O1' 1.479(8) . ? P1 O4 1.621(4) . ? P1 O3 1.628(6) . ? P1 O3' 1.747(10) . ? P2 O5 1.483(4) . ? P2 O7 1.490(3) . ? P2 O4 1.583(3) . ? P2 O6 1.599(4) . ? B1 F1 1.309(10) . ? B1 F2 1.330(13) . ? B1 F3 1.375(12) . ? B1 F4 1.427(12) . ? N1 N2 1.334(5) . ? N1 C8 1.352(6) . ? N1 C7 1.446(6) . ? N2 N3 1.318(6) . ? N3 C9 1.355(6) . ? N3 C10 1.470(6) . ? N4 C14 1.367(6) . ? N4 C11 1.378(6) . ? N4 H4A 0.8600 . ? N5 C18 1.366(6) . ? N5 C21 1.391(6) . ? N5 H5A 0.8600 . ? N6 N7 1.318(5) . ? N6 C22 1.379(6) . ? N6 C24 1.449(6) . ? N7 N8 1.326(5) . ? N8 C23 1.349(6) . ? N8 C25 1.427(6) . ? N9 N10 1.307(5) . ? N9 C35 1.350(6) . ? N9 C27 1.431(6) . ? N10 N11 1.313(6) . ? N11 C36 1.377(6) . ? N11 C37 1.467(7) . ? N12 C38 1.365(6) . ? N12 C41 1.372(6) . ? N12 H12A 0.8600 . ? N13 C45 1.370(6) . ? N13 C48 1.384(6) . ? N13 H13A 0.8600 . ? N14 N15 1.310(5) . ? N14 C49 1.381(6) . ? N14 C51 1.461(6) . ? N15 N16 1.326(5) . ? N16 C50 1.355(6) . ? N16 C52 1.448(6) . ? C1 C4 1.558(10) . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C4 1.486(9) . ? C2 H2C 0.9600 . ? C2 H2D 0.9600 . ? C2 H2E 0.9600 . ? C3 C4 1.509(9) . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C3 H3D 0.9600 . ? C4 C5 1.514(7) . ? C5 C6 1.376(7) . ? C5 C54 1.389(7) . ? C6 C7 1.380(6) . ? C6 H6A 0.9300 . ? C7 C53 1.373(6) . ? C8 C9 1.380(6) . ? C8 H8A 0.9300 . ? C9 C11 1.444(6) . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C10 H10D 0.9600 . ? C11 C12 1.375(6) . ? C12 C13 1.398(7) . ? C12 H12B 0.9300 . ? C13 C14 1.379(7) . ? C13 H13B 0.9300 . ? C14 C15 1.522(7) . ? C15 C18 1.517(7) . ? C15 C16 1.527(7) . ? C15 C17 1.539(7) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.394(7) . ? C19 C20 1.391(7) . ? C19 H19A 0.9300 . ? C20 C21 1.373(6) . ? C20 H20A 0.9300 . ? C21 C22 1.439(6) . ? C22 C23 1.365(6) . ? C23 H23A 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C30 1.379(7) . ? C25 C26 1.388(7) . ? C26 C27 1.359(6) . ? C26 H26A 0.9300 . ? C27 C28 1.399(7) . ? C28 C29 1.397(7) . ? C28 H28A 0.9300 . ? C29 C30 1.390(7) . ? C29 C31 1.529(7) . ? C30 H30A 0.9300 . ? C31 C32 1.506(9) . ? C31 C33 1.527(8) . ? C31 C34 1.556(10) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.368(7) . ? C35 H35A 0.9300 . ? C36 C38 1.447(7) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.375(7) . ? C39 C40 1.409(7) . ? C39 H39A 0.9300 . ? C40 C41 1.362(7) . ? C40 H40A 0.9300 . ? C41 C42 1.512(7) . ? C42 C45 1.514(7) . ? C42 C44 1.539(7) . ? C42 C43 1.547(7) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.377(7) . ? C46 C47 1.406(7) . ? C46 H46A 0.9300 . ? C47 C48 1.374(6) . ? C47 H47A 0.9300 . ? C48 C49 1.449(7) . ? C49 C50 1.363(6) . ? C50 H50A 0.9300 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 C53 1.381(6) . ? C52 C54 1.389(6) . ? C53 H53A 0.9300 . ? C54 H54A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2' P1 O1 143.2(5) . . ? O2' P1 O2 48.1(4) . . ? O1 P1 O2 122.0(5) . . ? O2' P1 O1' 123.6(5) . . ? O1 P1 O1' 44.3(4) . . ? O2 P1 O1' 152.2(4) . . ? O2' P1 O4 109.6(4) . . ? O1 P1 O4 107.3(3) . . ? O2 P1 O4 103.0(3) . . ? O1' P1 O4 104.5(3) . . ? O2' P1 O3 59.2(4) . . ? O1 P1 O3 111.2(4) . . ? O2 P1 O3 107.1(4) . . ? O1' P1 O3 69.5(4) . . ? O4 P1 O3 104.8(2) . . ? O2' P1 O3' 107.2(5) . . ? O1 P1 O3' 62.2(5) . . ? O2 P1 O3' 62.9(4) . . ? O1' P1 O3' 105.8(5) . . ? O4 P1 O3' 104.7(3) . . ? O3 P1 O3' 150.4(4) . . ? O5 P2 O7 117.9(2) . . ? O5 P2 O4 109.9(2) . . ? O7 P2 O4 106.05(18) . . ? O5 P2 O6 111.1(2) . . ? O7 P2 O6 106.9(2) . . ? O4 P2 O6 104.02(19) . . ? P2 O4 P1 132.3(2) . . ? F1 B1 F2 112.3(10) . . ? F1 B1 F3 112.4(10) . . ? F2 B1 F3 108.6(10) . . ? F1 B1 F4 109.4(9) . . ? F2 B1 F4 106.6(9) . . ? F3 B1 F4 107.4(9) . . ? N2 N1 C8 111.9(4) . . ? N2 N1 C7 116.6(4) . . ? C8 N1 C7 131.4(4) . . ? N3 N2 N1 103.8(4) . . ? N2 N3 C9 114.1(4) . . ? N2 N3 C10 116.3(4) . . ? C9 N3 C10 129.6(4) . . ? C14 N4 C11 109.9(4) . . ? C14 N4 H4A 125.0 . . ? C11 N4 H4A 125.0 . . ? C18 N5 C21 109.3(4) . . ? C18 N5 H5A 125.3 . . ? C21 N5 H5A 125.3 . . ? N7 N6 C22 112.7(4) . . ? N7 N6 C24 118.1(4) . . ? C22 N6 C24 129.1(4) . . ? N6 N7 N8 104.7(4) . . ? N7 N8 C23 111.5(4) . . ? N7 N8 C25 119.4(4) . . ? C23 N8 C25 129.1(4) . . ? N10 N9 C35 112.8(4) . . ? N10 N9 C27 117.3(4) . . ? C35 N9 C27 130.0(5) . . ? N9 N10 N11 104.3(4) . . ? N10 N11 C36 113.2(4) . . ? N10 N11 C37 116.8(5) . . ? C36 N11 C37 130.0(5) . . ? C38 N12 C41 109.7(4) . . ? C38 N12 H12A 125.1 . . ? C41 N12 H12A 125.1 . . ? C45 N13 C48 109.5(4) . . ? C45 N13 H13A 125.3 . . ? C48 N13 H13A 125.3 . . ? N15 N14 C49 113.0(4) . . ? N15 N14 C51 117.5(4) . . ? C49 N14 C51 129.5(4) . . ? N14 N15 N16 104.4(4) . . ? N15 N16 C50 112.2(4) . . ? N15 N16 C52 119.7(4) . . ? C50 N16 C52 128.1(4) . . ? C4 C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C4 C2 H2C 109.5 . . ? C4 C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? C4 C2 H2E 109.5 . . ? H2C C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? C4 C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C4 C3 H3D 109.5 . . ? H3B C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? C2 C4 C3 110.5(6) . . ? C2 C4 C5 111.3(5) . . ? C3 C4 C5 112.4(5) . . ? C2 C4 C1 110.8(6) . . ? C3 C4 C1 107.4(6) . . ? C5 C4 C1 104.3(6) . . ? C6 C5 C54 117.7(4) . . ? C6 C5 C4 120.2(5) . . ? C54 C5 C4 122.1(5) . . ? C7 C6 C5 120.6(5) . . ? C7 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? C53 C7 C6 123.0(4) . . ? C53 C7 N1 120.4(4) . . ? C6 C7 N1 116.6(4) . . ? N1 C8 C9 106.5(4) . . ? N1 C8 H8A 126.8 . . ? C9 C8 H8A 126.8 . . ? N3 C9 C8 103.8(4) . . ? N3 C9 C11 124.7(4) . . ? C8 C9 C11 131.4(4) . . ? N3 C10 H10B 109.5 . . ? N3 C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C10 H10D 109.5 . . ? H10B C10 H10D 109.5 . . ? H10C C10 H10D 109.5 . . ? C12 C11 N4 106.8(4) . . ? C12 C11 C9 132.3(5) . . ? N4 C11 C9 120.7(4) . . ? C11 C12 C13 108.3(4) . . ? C11 C12 H12B 125.9 . . ? C13 C12 H12B 125.9 . . ? C14 C13 C12 107.7(4) . . ? C14 C13 H13B 126.2 . . ? C12 C13 H13B 126.2 . . ? N4 C14 C13 107.3(5) . . ? N4 C14 C15 123.6(4) . . ? C13 C14 C15 129.1(4) . . ? C18 C15 C14 106.9(4) . . ? C18 C15 C16 112.0(4) . . ? C14 C15 C16 110.6(4) . . ? C18 C15 C17 108.4(4) . . ? C14 C15 C17 109.2(4) . . ? C16 C15 C17 109.6(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N5 C18 C19 106.8(5) . . ? N5 C18 C15 123.3(4) . . ? C19 C18 C15 129.8(5) . . ? C20 C19 C18 108.6(4) . . ? C20 C19 H19A 125.7 . . ? C18 C19 H19A 125.7 . . ? C21 C20 C19 107.5(4) . . ? C21 C20 H20A 126.2 . . ? C19 C20 H20A 126.2 . . ? C20 C21 N5 107.7(4) . . ? C20 C21 C22 133.7(5) . . ? N5 C21 C22 118.6(4) . . ? C23 C22 N6 103.5(4) . . ? C23 C22 C21 131.5(4) . . ? N6 C22 C21 125.0(4) . . ? N8 C23 C22 107.5(4) . . ? N8 C23 H23A 126.3 . . ? C22 C23 H23A 126.3 . . ? N6 C24 H24A 109.5 . . ? N6 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N6 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C30 C25 C26 121.1(5) . . ? C30 C25 N8 118.7(4) . . ? C26 C25 N8 120.1(4) . . ? C27 C26 C25 117.6(4) . . ? C27 C26 H26A 121.2 . . ? C25 C26 H26A 121.2 . . ? C26 C27 C28 122.5(5) . . ? C26 C27 N9 120.9(4) . . ? C28 C27 N9 116.5(5) . . ? C29 C28 C27 119.8(5) . . ? C29 C28 H28A 120.1 . . ? C27 C28 H28A 120.1 . . ? C30 C29 C28 117.3(5) . . ? C30 C29 C31 121.6(5) . . ? C28 C29 C31 121.2(5) . . ? C25 C30 C29 121.6(5) . . ? C25 C30 H30A 119.2 . . ? C29 C30 H30A 119.2 . . ? C32 C31 C33 110.9(6) . . ? C32 C31 C29 110.4(6) . . ? C33 C31 C29 112.3(5) . . ? C32 C31 C34 108.8(6) . . ? C33 C31 C34 108.0(6) . . ? C29 C31 C34 106.2(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N9 C35 C36 106.4(5) . . ? N9 C35 H35A 126.8 . . ? C36 C35 H35A 126.8 . . ? C35 C36 N11 103.4(5) . . ? C35 C36 C38 132.7(5) . . ? N11 C36 C38 124.0(4) . . ? N11 C37 H37A 109.5 . . ? N11 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N11 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N12 C38 C39 108.1(4) . . ? N12 C38 C36 120.9(4) . . ? C39 C38 C36 131.0(5) . . ? C38 C39 C40 106.3(5) . . ? C38 C39 H39A 126.8 . . ? C40 C39 H39A 126.8 . . ? C41 C40 C39 109.0(5) . . ? C41 C40 H40A 125.5 . . ? C39 C40 H40A 125.5 . . ? C40 C41 N12 106.9(5) . . ? C40 C41 C42 130.6(4) . . ? N12 C41 C42 122.5(4) . . ? C41 C42 C45 111.9(4) . . ? C41 C42 C44 109.2(4) . . ? C45 C42 C44 110.6(4) . . ? C41 C42 C43 107.8(4) . . ? C45 C42 C43 109.1(4) . . ? C44 C42 C43 108.1(4) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N13 C45 C46 107.2(5) . . ? N13 C45 C42 123.1(4) . . ? C46 C45 C42 129.6(5) . . ? C45 C46 C47 108.4(5) . . ? C45 C46 H46A 125.8 . . ? C47 C46 H46A 125.8 . . ? C48 C47 C46 107.3(4) . . ? C48 C47 H47A 126.4 . . ? C46 C47 H47A 126.4 . . ? C47 C48 N13 107.6(4) . . ? C47 C48 C49 134.3(5) . . ? N13 C48 C49 117.9(4) . . ? C50 C49 N14 104.0(4) . . ? C50 C49 C48 130.3(4) . . ? N14 C49 C48 125.7(4) . . ? N16 C50 C49 106.5(4) . . ? N16 C50 H50A 126.8 . . ? C49 C50 H50A 126.8 . . ? N14 C51 H51A 109.5 . . ? N14 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N14 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C54 122.4(5) . . ? C53 C52 N16 119.7(4) . . ? C54 C52 N16 117.9(4) . . ? C7 C53 C52 115.9(4) . . ? C7 C53 H53A 122.0 . . ? C52 C53 H53A 122.0 . . ? C52 C54 C5 120.3(5) . . ? C52 C54 H54A 119.8 . . ? C5 C54 H54A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.856 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.072 data_yys _database_code_depnum_ccdc_archive 'CCDC 849578' #TrackingRef 'BF4-TBAH2PO4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C54 H64 N16), 4(H2 O4 P), 8(B F4)' _chemical_formula_sum 'C162 H200 B8 F32 N48 O16 P4' _chemical_formula_weight 3894.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.554(6) _cell_length_b 16.552(5) _cell_length_c 31.568(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.445(7) _cell_angle_gamma 90.00 _cell_volume 10720(6) _cell_formula_units_Z 2 _cell_measurement_temperature 113(1) _cell_measurement_reflns_used 21884 _cell_measurement_theta_min 1.2164 _cell_measurement_theta_max 31.0898 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4048 _exptl_absorpt_coefficient_mu 0.127 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7863 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(1) _diffrn_radiation_wavelength 0.710747 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Sealed tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90740 _diffrn_reflns_av_R_equivalents 0.1256 _diffrn_reflns_av_sigmaI/netI 0.1599 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18622 _reflns_number_gt 8087 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _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. Some MeOH and H2O molecules arround the macrocycle were found to be badly disordered. Attempts to model the disorder were unsatisfactory. The contributions to the scattering factors due to these solvent molecules were removed by use of the utility SQUEEZE (Sluis and Spek, 1990) in PLATON98 (Spek, 1998). PLATON98 was used as incorporated in WinGX (Farrugia, 1999). ISOR was applied to one BF4 molecule and disorder methyl group of the macrocycle to allow their Uij components approximate to isotropic behavior. ; _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^)+(0.1370P)^2^+0.0000P] 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 18622 _refine_ls_number_parameters 1244 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.1924 _refine_ls_R_factor_gt 0.0981 _refine_ls_wR_factor_ref 0.2681 _refine_ls_wR_factor_gt 0.2262 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.964 _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 0.68621(9) 0.14585(12) 0.17655(5) 0.0495(5) Uani 1 1 d . . . P2 P 0.50746(12) 0.15606(16) 0.10997(6) 0.0724(7) Uani 1 1 d . . . O1 O 0.5357(2) 0.1994(3) 0.07177(11) 0.0534(13) Uani 1 1 d . . . H1A H 0.5114 0.2365 0.0639 0.064 Uiso 1 1 calc R . . O2 O 0.5431(2) 0.0796(3) 0.11725(12) 0.0441(11) Uani 1 1 d . . . O3 O 0.5217(2) 0.2110(3) 0.14734(11) 0.0450(11) Uani 1 1 d . . . H3A H 0.5071 0.2645 0.1400 0.067 Uiso 1 1 d R . . O4 O 0.43689(19) 0.1478(3) 0.10030(11) 0.0426(10) Uani 1 1 d . . . O5 O 0.7377(3) 0.1459(4) 0.14132(16) 0.102(2) Uani 1 1 d . . . O6 O 0.6480(3) 0.2239(3) 0.17181(13) 0.0754(16) Uani 1 1 d . . . H6A H 0.6100 0.2138 0.1643 0.113 Uiso 1 1 calc R . . O7 O 0.6434(2) 0.0701(3) 0.16758(13) 0.0572(13) Uani 1 1 d . . . H7A H 0.5984 0.0853 0.1677 0.086 Uiso 1 1 d R . . O8 O 0.72132(18) 0.1391(3) 0.21740(12) 0.0434(11) Uani 1 1 d . . . N1 N 0.4741(2) 0.3833(3) 0.13105(13) 0.0303(11) Uani 1 1 d . . . N2 N 0.5218(2) 0.4032(3) 0.10681(14) 0.0426(13) Uani 1 1 d . . . N3 N 0.4991(3) 0.3817(3) 0.06812(14) 0.0452(14) Uani 1 1 d . . . N4 N 0.3666(2) 0.2467(3) 0.03548(13) 0.0416(13) Uani 1 1 d . . . H4B H 0.3657 0.2195 0.0587 0.050 Uiso 1 1 calc R . . N5 N 0.3633(2) 0.0470(3) 0.03259(13) 0.0390(13) Uani 1 1 d . . . H5B H 0.3562 0.0654 0.0574 0.047 Uiso 1 1 calc R . . N6 N 0.4852(2) -0.1135(3) 0.05898(13) 0.0358(12) Uani 1 1 d . . . N7 N 0.5095(2) -0.1367(3) 0.09691(13) 0.0335(12) Uani 1 1 d . . . N8 N 0.4772(2) -0.0913(3) 0.12282(13) 0.0340(12) Uani 1 1 d . . . N9 N 0.6115(2) -0.0957(3) 0.25704(13) 0.0278(11) Uani 1 1 d . . . N10 N 0.6220(2) -0.1477(3) 0.28812(13) 0.0351(12) Uani 1 1 d . . . N11 N 0.6802(2) -0.1265(3) 0.30509(13) 0.0338(12) Uani 1 1 d . . . N12 N 0.7906(2) 0.0401(3) 0.27606(13) 0.0325(12) Uani 1 1 d . . . H12A H 0.7718 0.0603 0.2534 0.039 Uiso 1 1 calc R . . N13 N 0.7888(2) 0.2394(3) 0.27775(13) 0.0334(12) Uani 1 1 d . . . H13A H 0.7693 0.2191 0.2553 0.040 Uiso 1 1 calc R . . N14 N 0.6840(2) 0.4105(3) 0.30852(13) 0.0334(11) Uani 1 1 d . . . N15 N 0.6261(2) 0.4355(3) 0.29298(14) 0.0391(12) Uani 1 1 d . . . N16 N 0.6102(2) 0.3824(3) 0.26267(12) 0.0288(11) Uani 1 1 d . . . N17 N 1.1506(2) 0.4113(3) 0.08086(13) 0.0311(11) Uani 1 1 d . . . N18 N 1.2102(2) 0.4367(3) 0.07481(14) 0.0380(13) Uani 1 1 d . . . N19 N 1.2210(2) 0.4924(3) 0.10422(13) 0.0346(12) Uani 1 1 d . . . N20 N 1.1119(2) 0.5677(3) 0.18541(12) 0.0313(11) Uani 1 1 d . . . H20A H 1.0779 0.5377 0.1818 0.038 Uiso 1 1 calc R . . N21 N 0.9890(2) 0.6686(3) 0.18377(12) 0.0290(11) Uani 1 1 d . . . H21A H 1.0181 0.6818 0.1666 0.035 Uiso 1 1 calc R . . N22 N 0.8372(2) 0.6562(3) 0.11521(12) 0.0284(11) Uani 1 1 d . . . N23 N 0.8286(2) 0.6634(3) 0.07330(14) 0.0313(11) Uani 1 1 d . . . N24 N 0.8866(2) 0.6877(3) 0.06186(12) 0.0280(11) Uani 1 1 d . . . C1 C 0.4078(3) 0.5459(4) 0.29466(19) 0.0522(18) Uani 1 1 d . . . H1C H 0.4242 0.5887 0.2778 0.078 Uiso 1 1 calc R . . H1D H 0.4423 0.5253 0.3134 0.078 Uiso 1 1 calc R . . H1E H 0.3734 0.5663 0.3110 0.078 Uiso 1 1 calc R . . C2 C 0.3560(3) 0.4093(4) 0.2929(2) 0.0537(19) Uani 1 1 d . . . H2C H 0.3401 0.3665 0.2746 0.081 Uiso 1 1 calc R . . H2D H 0.3213 0.4289 0.3092 0.081 Uiso 1 1 calc R . . H2E H 0.3907 0.3895 0.3118 0.081 Uiso 1 1 calc R . . C3 C 0.3265(3) 0.5093(4) 0.23569(18) 0.0465(17) Uani 1 1 d . . . H3B H 0.3426 0.5516 0.2183 0.070 Uiso 1 1 calc R . . H3C H 0.2919 0.5299 0.2517 0.070 Uiso 1 1 calc R . . H3D H 0.3104 0.4657 0.2180 0.070 Uiso 1 1 calc R . . C4 C 0.3815(3) 0.4787(4) 0.26594(17) 0.0379(15) Uani 1 1 d . . . C5 C 0.4379(3) 0.4433(4) 0.24030(16) 0.0336(14) Uani 1 1 d . . . C6 C 0.4977(3) 0.4253(4) 0.26149(17) 0.0333(14) Uani 1 1 d . . . H6B H 0.5037 0.4348 0.2905 0.040 Uiso 1 1 calc R . . C7 C 0.5471(3) 0.3940(3) 0.23999(15) 0.0298(14) Uani 1 1 d . . . C8 C 0.5420(3) 0.3775(3) 0.19679(17) 0.0309(14) Uani 1 1 d . . . H8B H 0.5761 0.3551 0.1827 0.037 Uiso 1 1 calc R . . C9 C 0.4824(3) 0.3966(4) 0.17618(17) 0.0345(14) Uani 1 1 d . . . C10 C 0.4314(3) 0.4282(4) 0.19676(16) 0.0352(14) Uani 1 1 d . . . H10B H 0.3923 0.4396 0.1816 0.042 Uiso 1 1 calc R . . C11 C 0.4222(3) 0.3507(4) 0.10907(17) 0.0357(14) Uani 1 1 d . . . H11A H 0.3837 0.3332 0.1201 0.043 Uiso 1 1 calc R . . C12 C 0.4371(3) 0.3486(4) 0.06763(18) 0.0384(15) Uani 1 1 d . . . C13 C 0.4016(3) 0.3157(4) 0.03093(16) 0.0377(15) Uani 1 1 d . . . C14 C 0.3903(3) 0.3417(4) -0.01030(19) 0.0470(17) Uani 1 1 d . . . H14A H 0.4073 0.3877 -0.0224 0.056 Uiso 1 1 calc R . . C15 C 0.3478(3) 0.2849(4) -0.03048(18) 0.0485(18) Uani 1 1 d . . . H15B H 0.3322 0.2866 -0.0587 0.058 Uiso 1 1 calc R . . C16 C 0.3332(3) 0.2266(4) -0.00157(17) 0.0393(16) Uani 1 1 d . . . C17 C 0.2919(3) 0.1519(4) -0.00645(16) 0.0370(15) Uani 1 1 d . . . C18 C 0.2534(3) 0.1515(5) -0.04895(17) 0.0529(18) Uani 1 1 d . . . H18B H 0.2252 0.1978 -0.0509 0.079 Uiso 1 1 calc R . . H18C H 0.2277 0.1031 -0.0515 0.079 Uiso 1 1 calc R . . H18D H 0.2829 0.1533 -0.0714 0.079 Uiso 1 1 calc R . . C19 C 0.2429(3) 0.1487(4) 0.02907(18) 0.0492(18) Uani 1 1 d . . . H19A H 0.2664 0.1491 0.0563 0.074 Uiso 1 1 calc R . . H19B H 0.2174 0.1002 0.0262 0.074 Uiso 1 1 calc R . . H19C H 0.2146 0.1948 0.0267 0.074 Uiso 1 1 calc R . . C20 C 0.3353(3) 0.0774(4) -0.00469(16) 0.0369(15) Uani 1 1 d . . . C21 C 0.3588(3) 0.0305(4) -0.03598(17) 0.0443(17) Uani 1 1 d . . . H21B H 0.3478 0.0366 -0.0648 0.053 Uiso 1 1 calc R . . C22 C 0.4026(3) -0.0288(4) -0.01832(17) 0.0464(17) Uani 1 1 d . . . H22A H 0.4253 -0.0675 -0.0329 0.056 Uiso 1 1 calc R . . C23 C 0.4042(3) -0.0167(4) 0.02526(16) 0.0376(15) Uani 1 1 d . . . C24 C 0.4387(3) -0.0551(4) 0.06105(16) 0.0321(14) Uani 1 1 d . . . C25 C 0.4341(3) -0.0420(4) 0.10286(16) 0.0337(14) Uani 1 1 d . . . H25A H 0.4064 -0.0057 0.1153 0.040 Uiso 1 1 calc R . . C26 C 0.5070(3) -0.1566(4) 0.02192(18) 0.0503(18) Uani 1 1 d . . . H26A H 0.5400 -0.1951 0.0309 0.075 Uiso 1 1 calc R . . H26B H 0.5247 -0.1187 0.0027 0.075 Uiso 1 1 calc R . . H26C H 0.4708 -0.1843 0.0079 0.075 Uiso 1 1 calc R . . C27 C 0.4865(3) -0.1051(4) 0.16830(15) 0.0322(14) Uani 1 1 d . . . C28 C 0.4340(3) -0.1371(3) 0.18810(16) 0.0297(13) Uani 1 1 d . . . H28A H 0.3952 -0.1476 0.1724 0.036 Uiso 1 1 calc R . . C29 C 0.4388(3) -0.1536(3) 0.23140(16) 0.0293(13) Uani 1 1 d . . . C30 C 0.4990(3) -0.1372(3) 0.25306(16) 0.0294(13) Uani 1 1 d . . . H30A H 0.5045 -0.1476 0.2820 0.035 Uiso 1 1 calc R . . C31 C 0.5499(3) -0.1058(3) 0.23208(16) 0.0265(13) Uani 1 1 d . . . C32 C 0.5450(3) -0.0871(4) 0.18941(15) 0.0301(13) Uani 1 1 d . . . H32A H 0.5792 -0.0636 0.1758 0.036 Uiso 1 1 calc R . . C33 C 0.3819(3) -0.1891(4) 0.25372(16) 0.0333(14) Uani 1 1 d . . . C34 C 0.3542(3) -0.2612(4) 0.22847(19) 0.0491(17) Uani 1 1 d . . . H34A H 0.3868 -0.3027 0.2278 0.074 Uiso 1 1 calc R . . H34B H 0.3417 -0.2445 0.2000 0.074 Uiso 1 1 calc R . . H34C H 0.3168 -0.2818 0.2417 0.074 Uiso 1 1 calc R . . C35 C 0.3280(3) -0.1229(4) 0.25434(19) 0.0482(18) Uani 1 1 d . . . H35A H 0.2912 -0.1438 0.2682 0.072 Uiso 1 1 calc R . . H35B H 0.3146 -0.1079 0.2258 0.072 Uiso 1 1 calc R . . H35C H 0.3449 -0.0764 0.2695 0.072 Uiso 1 1 calc R . . C36 C 0.4008(3) -0.2153(4) 0.29872(17) 0.0450(17) Uani 1 1 d . . . H36A H 0.4337 -0.2565 0.2983 0.067 Uiso 1 1 calc R . . H36B H 0.3632 -0.2364 0.3116 0.067 Uiso 1 1 calc R . . H36C H 0.4176 -0.1698 0.3148 0.067 Uiso 1 1 calc R . . C37 C 0.6598(3) -0.0430(4) 0.25355(15) 0.0271(13) Uani 1 1 d . . . H37A H 0.6621 -0.0019 0.2336 0.033 Uiso 1 1 calc R . . C38 C 0.7056(3) -0.0619(4) 0.28559(16) 0.0323(14) Uani 1 1 d . . . C39 C 0.7054(3) -0.1714(4) 0.34276(19) 0.0567(19) Uani 1 1 d . . . H39A H 0.6762 -0.2149 0.3483 0.085 Uiso 1 1 calc R . . H39B H 0.7088 -0.1357 0.3668 0.085 Uiso 1 1 calc R . . H39C H 0.7477 -0.1929 0.3378 0.085 Uiso 1 1 calc R . . C40 C 0.7677(3) -0.0245(3) 0.29843(16) 0.0291(13) Uani 1 1 d . . . C41 C 0.8120(3) -0.0398(4) 0.33236(16) 0.0347(14) Uani 1 1 d . . . H41A H 0.8095 -0.0805 0.3525 0.042 Uiso 1 1 calc R . . C42 C 0.8619(3) 0.0190(4) 0.33011(16) 0.0358(15) Uani 1 1 d . . . H42A H 0.8981 0.0240 0.3490 0.043 Uiso 1 1 calc R . . C43 C 0.8478(3) 0.0672(3) 0.29542(16) 0.0304(14) Uani 1 1 d . . . C44 C 0.8834(3) 0.1411(4) 0.28079(17) 0.0373(14) Uani 1 1 d . . . C45 C 0.8863(3) 0.1422(4) 0.23126(17) 0.0391(15) Uani 1 1 d . . . H45A H 0.9091 0.1897 0.2229 0.059 Uiso 1 1 calc R . . H45B H 0.8428 0.1427 0.2183 0.059 Uiso 1 1 calc R . . H45C H 0.9088 0.0950 0.2223 0.059 Uiso 1 1 calc R . . C46 C 0.9531(3) 0.1413(4) 0.29988(18) 0.0407(15) Uani 1 1 d . . . H46A H 0.9528 0.1400 0.3303 0.061 Uiso 1 1 calc R . . H46B H 0.9749 0.1893 0.2912 0.061 Uiso 1 1 calc R . . H46C H 0.9757 0.0946 0.2902 0.061 Uiso 1 1 calc R . . C47 C 0.8472(3) 0.2136(4) 0.29611(16) 0.0350(15) Uani 1 1 d . . . C48 C 0.8616(3) 0.2613(4) 0.33178(17) 0.0376(15) Uani 1 1 d . . . H48A H 0.8982 0.2567 0.3504 0.045 Uiso 1 1 calc R . . C49 C 0.8109(3) 0.3175(4) 0.33459(16) 0.0351(14) Uani 1 1 d . . . H49A H 0.8082 0.3571 0.3553 0.042 Uiso 1 1 calc R . . C50 C 0.7660(3) 0.3040(4) 0.30127(16) 0.0319(14) Uani 1 1 d . . . C51 C 0.7044(3) 0.3437(4) 0.28891(15) 0.0292(14) Uani 1 1 d . . . C52 C 0.6562(3) 0.3249(4) 0.25864(16) 0.0325(14) Uani 1 1 d . . . H52A H 0.6554 0.2821 0.2395 0.039 Uiso 1 1 calc R . . C53 C 0.7146(4) 0.4610(4) 0.3422(2) 0.061(2) Uani 1 1 d . . . H53A H 0.6860 0.5049 0.3482 0.092 Uiso 1 1 calc R . . H53B H 0.7549 0.4822 0.3331 0.092 Uiso 1 1 calc R . . H53C H 0.7228 0.4291 0.3673 0.092 Uiso 1 1 calc R . . C54 C 1.0217(3) 0.1582(4) 0.05657(18) 0.0479(18) Uani 1 1 d . . . C55 C 1.0629(5) 0.0806(6) 0.0493(3) 0.072(4) Uani 0.802(13) 1 d PU A 1 H55A H 1.0407 0.0343 0.0596 0.108 Uiso 0.802(13) 1 calc PR A 1 H55B H 1.1048 0.0857 0.0643 0.108 Uiso 0.802(13) 1 calc PR A 1 H55C H 1.0686 0.0742 0.0195 0.108 Uiso 0.802(13) 1 calc PR A 1 C56 C 1.0103(6) 0.1637(7) 0.1034(3) 0.067(3) Uani 0.802(13) 1 d PU A 1 H56A H 0.9871 0.1167 0.1120 0.101 Uiso 0.802(13) 1 calc PR A 1 H56B H 0.9851 0.2111 0.1086 0.101 Uiso 0.802(13) 1 calc PR A 1 H56C H 1.0515 0.1669 0.1194 0.101 Uiso 0.802(13) 1 calc PR A 1 C57 C 0.9563(5) 0.1462(8) 0.0294(3) 0.072(3) Uani 0.802(13) 1 d PU A 1 H57A H 0.9332 0.1008 0.0401 0.107 Uiso 0.802(13) 1 calc PR A 1 H57B H 0.9654 0.1365 0.0004 0.107 Uiso 0.802(13) 1 calc PR A 1 H57C H 0.9300 0.1939 0.0311 0.107 Uiso 0.802(13) 1 calc PR A 1 C55' C 0.9815(18) 0.102(3) 0.0272(9) 0.068(14) Uani 0.198(13) 1 d PDU A 2 H55D H 1.0009 0.0490 0.0280 0.103 Uiso 0.198(13) 1 calc PR A 2 H55E H 0.9805 0.1223 -0.0012 0.103 Uiso 0.198(13) 1 calc PR A 2 H55F H 0.9379 0.0985 0.0364 0.103 Uiso 0.198(13) 1 calc PR A 2 C56' C 0.9683(17) 0.192(2) 0.0896(11) 0.066(13) Uani 0.198(13) 1 d PDU A 2 H56D H 0.9439 0.2360 0.0764 0.099 Uiso 0.198(13) 1 calc PR A 2 H56E H 0.9910 0.2114 0.1151 0.099 Uiso 0.198(13) 1 calc PR A 2 H56F H 0.9391 0.1496 0.0963 0.099 Uiso 0.198(13) 1 calc PR A 2 C57' C 1.0680(14) 0.107(2) 0.0863(10) 0.057(12) Uani 0.198(13) 1 d PDU A 2 H57D H 1.0448 0.0605 0.0961 0.085 Uiso 0.198(13) 1 calc PR A 2 H57E H 1.0834 0.1386 0.1102 0.085 Uiso 0.198(13) 1 calc PR A 2 H57F H 1.1044 0.0887 0.0711 0.085 Uiso 0.198(13) 1 calc PR A 2 C58 C 1.0575(3) 0.2309(4) 0.04008(17) 0.0371(15) Uani 1 1 d . . . C59 C 1.0855(3) 0.2888(4) 0.06806(17) 0.0323(14) Uani 1 1 d . . . H59A H 1.0801 0.2847 0.0970 0.039 Uiso 1 1 calc R A . C60 C 1.1213(3) 0.3522(4) 0.05235(16) 0.0329(14) Uani 1 1 d . A . C61 C 1.1318(3) 0.3613(4) 0.00986(16) 0.0306(13) Uani 1 1 d . . . H61A H 1.1560 0.4038 -0.0003 0.046 Uiso 1 1 calc R A . C62 C 1.1240(3) 0.4493(4) 0.11269(16) 0.0321(14) Uani 1 1 d . . . H62A H 1.0828 0.4405 0.1224 0.039 Uiso 1 1 calc R . . C63 C 1.1694(3) 0.5041(4) 0.12835(16) 0.0351(15) Uani 1 1 d . . . C64 C 1.2850(3) 0.5312(5) 0.10607(19) 0.0523(19) Uani 1 1 d . . . H64A H 1.3104 0.5095 0.0842 0.078 Uiso 1 1 calc R . . H64B H 1.3070 0.5212 0.1333 0.078 Uiso 1 1 calc R . . H64C H 1.2798 0.5884 0.1020 0.078 Uiso 1 1 calc R . . C65 C 1.1664(3) 0.5618(4) 0.16209(16) 0.0334(14) Uani 1 1 d . . . C66 C 1.2095(3) 0.6218(4) 0.17779(17) 0.0373(15) Uani 1 1 d . . . H66A H 1.2505 0.6331 0.1682 0.045 Uiso 1 1 calc R . . C67 C 1.1797(3) 0.6617(4) 0.21043(17) 0.0392(16) Uani 1 1 d . . . H67A H 1.1976 0.7041 0.2265 0.047 Uiso 1 1 calc R . . C68 C 1.1194(3) 0.6279(3) 0.21499(15) 0.0275(13) Uani 1 1 d . . . C69 C 1.0690(3) 0.6450(4) 0.24692(16) 0.0323(13) Uani 1 1 d . . . C70 C 1.0839(3) 0.7264(4) 0.26860(17) 0.0361(14) Uani 1 1 d . . . H70A H 1.0816 0.7686 0.2477 0.054 Uiso 1 1 calc R . . H70B H 1.1268 0.7250 0.2824 0.054 Uiso 1 1 calc R . . H70C H 1.0525 0.7366 0.2893 0.054 Uiso 1 1 calc R . . C71 C 1.0738(3) 0.5784(4) 0.28075(16) 0.0408(16) Uani 1 1 d . . . H71A H 1.0651 0.5269 0.2676 0.061 Uiso 1 1 calc R . . H71B H 1.0425 0.5884 0.3015 0.061 Uiso 1 1 calc R . . H71C H 1.1168 0.5782 0.2943 0.061 Uiso 1 1 calc R . . C72 C 1.0007(3) 0.6480(3) 0.22560(15) 0.0270(13) Uani 1 1 d . . . C73 C 0.9421(3) 0.6326(4) 0.24254(16) 0.0390(16) Uani 1 1 d . . . H73A H 0.9359 0.6175 0.2704 0.047 Uiso 1 1 calc R . . C74 C 0.8932(3) 0.6439(4) 0.20995(16) 0.0344(14) Uani 1 1 d . . . H74A H 0.8486 0.6382 0.2127 0.041 Uiso 1 1 calc R . . C75 C 0.9218(3) 0.6646(3) 0.17371(16) 0.0315(14) Uani 1 1 d . . . C76 C 0.8986(3) 0.6743(3) 0.13069(16) 0.0273(13) Uani 1 1 d . . . C77 C 0.9301(3) 0.6955(4) 0.09530(16) 0.0335(14) Uani 1 1 d . . . H77A H 0.9733 0.7120 0.0945 0.040 Uiso 1 1 calc R . . C78 C 0.7808(3) 0.6282(4) 0.13672(17) 0.0431(17) Uani 1 1 d . . . H78A H 0.7448 0.6203 0.1163 0.065 Uiso 1 1 calc R . . H78B H 0.7692 0.6679 0.1572 0.065 Uiso 1 1 calc R . . H78C H 0.7911 0.5781 0.1509 0.065 Uiso 1 1 calc R . . C79 C 0.8963(3) 0.6975(4) 0.01668(16) 0.0300(13) Uani 1 1 d . . . C80 C 0.9319(3) 0.7612(4) 0.00363(16) 0.0320(14) Uani 1 1 d . . . H80A H 0.9491 0.7989 0.0231 0.048 Uiso 1 1 calc R . . C81 C 0.5400(4) 0.3950(5) 0.03258(19) 0.064(2) Uani 1 1 d . . . H81A H 0.5807 0.4184 0.0428 0.095 Uiso 1 1 calc R . . H81B H 0.5182 0.4310 0.0125 0.095 Uiso 1 1 calc R . . H81C H 0.5480 0.3443 0.0190 0.095 Uiso 1 1 calc R . . B1 B 0.9498(4) 0.4623(5) 0.1280(3) 0.055(2) Uani 1 1 d . . . F1 F 0.9688(2) 0.5159(3) 0.09812(14) 0.0937(16) Uani 1 1 d . . . F2 F 0.99079(18) 0.4769(3) 0.16549(13) 0.0667(11) Uani 1 1 d . . . F3 F 0.9584(2) 0.3861(3) 0.11574(14) 0.0807(13) Uani 1 1 d . . . F4 F 0.88626(17) 0.4778(2) 0.13776(11) 0.0553(10) Uani 1 1 d . . . B2 B 0.4463(5) 0.5937(8) 0.0819(3) 0.072(3) Uani 1 1 d . . . F5 F 0.5107(3) 0.5901(5) 0.0829(2) 0.153(3) Uani 1 1 d . . . F6 F 0.4287(4) 0.6704(5) 0.0672(2) 0.162(3) Uani 1 1 d . . . F7 F 0.4245(3) 0.5791(5) 0.12017(14) 0.144(3) Uani 1 1 d . . . F8 F 0.4205(3) 0.5392(4) 0.05407(16) 0.1100(19) Uani 1 1 d . . . B3 B 0.2359(4) -0.2254(6) 0.3499(2) 0.049(2) Uani 1 1 d . . . F9 F 0.29312(17) -0.2297(3) 0.37408(10) 0.0609(11) Uani 1 1 d . . . F10 F 0.24238(17) -0.2640(3) 0.31119(10) 0.0685(13) Uani 1 1 d . . . F11 F 0.18644(17) -0.2651(2) 0.37094(11) 0.0545(10) Uani 1 1 d . . . F12 F 0.21673(18) -0.1452(3) 0.34290(11) 0.0629(11) Uani 1 1 d . . . B4 B 0.9392(5) 0.9114(7) 0.1078(3) 0.086(3) Uani 1 1 d DU . . F13 F 0.9834(3) 0.8851(6) 0.14074(19) 0.203(4) Uani 1 1 d DU . . F14 F 0.9241(4) 0.9889(3) 0.1156(2) 0.175(3) Uani 1 1 d DU . . F15 F 0.9657(3) 0.8969(4) 0.07149(16) 0.154(3) Uani 1 1 d DU . . F16 F 0.8849(2) 0.8630(3) 0.11179(19) 0.1156(18) Uani 1 1 d DU . . 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 0.0609(12) 0.0392(12) 0.0479(10) 0.0010(8) -0.0003(8) 0.0040(10) P2 0.0759(16) 0.0786(19) 0.0613(12) 0.0007(12) -0.0081(11) -0.0027(14) O1 0.076(3) 0.049(3) 0.035(2) 0.006(2) -0.002(2) 0.006(3) O2 0.041(3) 0.032(3) 0.058(2) -0.003(2) -0.0053(19) 0.006(2) O3 0.055(3) 0.039(3) 0.040(2) -0.011(2) -0.0006(19) 0.007(2) O4 0.032(2) 0.041(3) 0.053(2) 0.005(2) -0.0159(18) 0.003(2) O5 0.163(6) 0.065(4) 0.083(4) -0.010(3) 0.063(4) -0.031(4) O6 0.106(4) 0.055(4) 0.061(3) -0.007(2) -0.030(3) 0.018(3) O7 0.049(3) 0.053(3) 0.068(3) 0.001(2) -0.015(2) 0.002(3) O8 0.027(2) 0.047(3) 0.056(2) -0.005(2) -0.0005(18) -0.001(2) N1 0.034(3) 0.028(3) 0.029(2) 0.001(2) -0.001(2) 0.005(2) N2 0.045(3) 0.050(4) 0.033(3) 0.004(2) 0.000(2) -0.006(3) N3 0.046(3) 0.050(4) 0.040(3) 0.003(3) 0.001(3) -0.001(3) N4 0.052(3) 0.048(4) 0.024(2) 0.002(2) -0.006(2) -0.008(3) N5 0.041(3) 0.052(4) 0.024(2) -0.010(2) -0.006(2) 0.000(3) N6 0.029(3) 0.045(4) 0.033(3) -0.007(2) 0.000(2) 0.008(2) N7 0.025(2) 0.042(3) 0.033(2) -0.003(2) -0.004(2) 0.004(2) N8 0.027(3) 0.041(3) 0.033(3) 0.002(2) -0.002(2) 0.001(2) N9 0.024(3) 0.025(3) 0.034(2) 0.003(2) -0.0007(19) 0.001(2) N10 0.028(3) 0.036(3) 0.040(3) 0.005(2) -0.012(2) -0.005(2) N11 0.036(3) 0.021(3) 0.044(3) 0.010(2) -0.010(2) 0.001(2) N12 0.022(3) 0.037(3) 0.038(2) -0.001(2) -0.008(2) -0.004(2) N13 0.031(3) 0.036(3) 0.032(2) -0.003(2) -0.006(2) 0.000(2) N14 0.028(3) 0.028(3) 0.042(3) -0.006(2) -0.013(2) 0.007(2) N15 0.035(3) 0.034(3) 0.048(3) -0.006(2) -0.005(2) 0.003(3) N16 0.031(3) 0.025(3) 0.029(2) 0.003(2) -0.007(2) -0.001(2) N17 0.025(3) 0.035(3) 0.033(2) -0.006(2) 0.004(2) -0.005(2) N18 0.022(3) 0.052(4) 0.041(3) -0.010(3) 0.005(2) -0.002(2) N19 0.025(3) 0.043(3) 0.036(3) -0.008(2) 0.004(2) -0.004(2) N20 0.033(3) 0.030(3) 0.031(2) 0.000(2) 0.000(2) -0.008(2) N21 0.025(3) 0.031(3) 0.030(2) 0.006(2) -0.0045(19) 0.001(2) N22 0.022(2) 0.034(3) 0.029(2) 0.007(2) 0.0009(19) 0.007(2) N23 0.020(3) 0.029(3) 0.044(3) 0.003(2) -0.003(2) 0.000(2) N24 0.031(3) 0.024(3) 0.029(2) -0.002(2) -0.001(2) -0.004(2) C1 0.051(4) 0.049(5) 0.056(4) -0.020(3) -0.006(3) 0.015(4) C2 0.044(4) 0.047(5) 0.071(4) 0.006(4) 0.016(3) 0.016(4) C3 0.034(4) 0.047(5) 0.057(4) -0.013(3) 0.000(3) 0.007(3) C4 0.027(3) 0.041(4) 0.045(3) -0.005(3) -0.004(3) 0.002(3) C5 0.029(3) 0.030(4) 0.041(3) -0.002(3) -0.009(2) 0.000(3) C6 0.039(4) 0.029(4) 0.032(3) 0.002(3) -0.001(3) 0.005(3) C7 0.037(4) 0.024(4) 0.028(3) 0.002(2) -0.006(2) -0.002(3) C8 0.021(3) 0.024(4) 0.048(3) 0.004(3) 0.004(2) -0.002(3) C9 0.034(4) 0.032(4) 0.038(3) -0.001(3) 0.004(3) -0.007(3) C10 0.038(4) 0.025(4) 0.040(3) 0.000(3) -0.009(3) -0.004(3) C11 0.034(3) 0.031(4) 0.041(3) -0.006(3) -0.008(3) 0.004(3) C12 0.044(4) 0.026(4) 0.045(4) -0.004(3) 0.005(3) 0.006(3) C13 0.042(4) 0.039(4) 0.032(3) 0.005(3) 0.000(3) -0.001(3) C14 0.046(4) 0.041(5) 0.053(4) 0.014(3) -0.004(3) 0.009(3) C15 0.054(4) 0.052(5) 0.037(3) 0.006(3) -0.012(3) 0.004(4) C16 0.037(4) 0.041(4) 0.039(3) -0.005(3) -0.008(3) 0.021(3) C17 0.041(4) 0.034(4) 0.035(3) -0.003(3) -0.003(3) 0.007(3) C18 0.049(4) 0.059(5) 0.050(4) -0.003(3) -0.012(3) 0.014(4) C19 0.037(4) 0.059(5) 0.050(4) -0.001(3) -0.009(3) 0.018(4) C20 0.029(3) 0.050(4) 0.030(3) -0.007(3) -0.006(3) 0.001(3) C21 0.047(4) 0.055(5) 0.030(3) 0.004(3) -0.008(3) 0.005(4) C22 0.051(4) 0.050(5) 0.038(3) -0.006(3) 0.002(3) 0.014(4) C23 0.023(3) 0.054(5) 0.035(3) -0.006(3) 0.000(2) 0.007(3) C24 0.032(3) 0.028(4) 0.035(3) 0.001(3) -0.006(2) 0.005(3) C25 0.038(4) 0.029(4) 0.033(3) -0.007(3) -0.005(3) 0.009(3) C26 0.040(4) 0.064(5) 0.047(4) 0.001(3) 0.002(3) 0.017(4) C27 0.035(3) 0.031(4) 0.029(3) 0.001(3) -0.011(3) 0.009(3) C28 0.023(3) 0.028(4) 0.038(3) 0.000(3) -0.005(2) 0.002(3) C29 0.031(3) 0.020(4) 0.036(3) -0.001(3) -0.003(2) 0.007(3) C30 0.027(3) 0.021(3) 0.040(3) 0.002(3) -0.004(2) 0.006(3) C31 0.023(3) 0.016(3) 0.040(3) -0.006(2) -0.006(2) 0.001(2) C32 0.025(3) 0.034(4) 0.031(3) 0.000(3) 0.002(2) 0.001(3) C33 0.028(3) 0.031(4) 0.040(3) 0.001(3) -0.001(2) -0.004(3) C34 0.038(4) 0.046(5) 0.063(4) 0.011(3) -0.001(3) -0.009(3) C35 0.038(4) 0.051(5) 0.057(4) 0.005(3) 0.007(3) 0.000(3) C36 0.031(4) 0.053(5) 0.051(4) 0.012(3) -0.001(3) -0.002(3) C37 0.028(3) 0.029(4) 0.025(3) 0.000(2) 0.006(2) -0.002(3) C38 0.036(3) 0.024(4) 0.036(3) -0.003(3) -0.005(3) 0.005(3) C39 0.049(4) 0.052(5) 0.066(4) 0.020(4) -0.027(3) -0.014(4) C40 0.025(3) 0.022(4) 0.040(3) -0.004(3) 0.002(2) -0.001(3) C41 0.033(3) 0.032(4) 0.038(3) 0.003(3) -0.002(3) 0.004(3) C42 0.030(3) 0.037(4) 0.039(3) -0.002(3) -0.009(3) -0.003(3) C43 0.030(3) 0.024(4) 0.037(3) -0.005(3) 0.006(3) 0.001(3) C44 0.031(3) 0.030(4) 0.051(3) 0.003(3) 0.001(3) 0.006(3) C45 0.030(3) 0.032(4) 0.055(4) 0.008(3) 0.001(3) 0.002(3) C46 0.022(3) 0.033(4) 0.066(4) -0.002(3) -0.008(3) -0.002(3) C47 0.022(3) 0.047(4) 0.036(3) 0.005(3) 0.001(2) -0.005(3) C48 0.032(3) 0.041(4) 0.039(3) 0.007(3) -0.003(3) -0.005(3) C49 0.034(3) 0.034(4) 0.037(3) -0.002(3) 0.001(3) -0.006(3) C50 0.027(3) 0.029(4) 0.039(3) 0.012(3) -0.001(3) -0.004(3) C51 0.032(3) 0.026(4) 0.029(3) 0.010(3) -0.002(2) -0.003(3) C52 0.039(4) 0.024(4) 0.034(3) 0.004(3) -0.003(3) 0.004(3) C53 0.062(5) 0.041(5) 0.078(4) -0.023(4) -0.017(4) 0.005(4) C54 0.062(4) 0.036(4) 0.044(4) 0.016(3) -0.011(3) -0.022(4) C55 0.082(7) 0.052(6) 0.082(6) 0.011(5) 0.009(5) -0.015(5) C56 0.080(7) 0.064(7) 0.058(5) 0.009(4) 0.005(5) -0.020(5) C57 0.061(6) 0.086(7) 0.065(5) 0.021(5) -0.016(4) -0.040(6) C55' 0.074(16) 0.066(17) 0.066(15) -0.001(10) 0.005(10) 0.003(10) C56' 0.068(15) 0.065(15) 0.066(15) 0.000(9) 0.019(10) -0.002(10) C57' 0.061(15) 0.053(15) 0.054(14) 0.012(9) -0.008(9) -0.002(9) C58 0.027(3) 0.040(4) 0.042(3) 0.006(3) -0.011(3) 0.003(3) C59 0.020(3) 0.038(4) 0.038(3) 0.006(3) 0.000(2) 0.002(3) C60 0.033(3) 0.035(4) 0.031(3) -0.007(3) -0.001(2) 0.008(3) C61 0.026(3) 0.028(4) 0.037(3) 0.003(3) -0.005(2) 0.004(3) C62 0.029(3) 0.034(4) 0.033(3) 0.003(3) -0.003(2) 0.003(3) C63 0.034(3) 0.041(4) 0.029(3) -0.002(3) -0.006(3) -0.004(3) C64 0.039(4) 0.066(5) 0.053(4) -0.018(3) 0.012(3) -0.010(4) C65 0.028(3) 0.038(4) 0.034(3) 0.010(3) -0.007(2) 0.000(3) C66 0.025(3) 0.040(4) 0.046(3) -0.009(3) -0.008(3) 0.000(3) C67 0.038(4) 0.036(4) 0.042(3) -0.010(3) -0.012(3) -0.003(3) C68 0.029(3) 0.018(3) 0.034(3) 0.001(3) -0.006(2) 0.002(3) C69 0.030(3) 0.027(4) 0.038(3) -0.001(3) -0.008(2) 0.003(3) C70 0.033(3) 0.031(4) 0.043(3) -0.006(3) -0.003(3) 0.007(3) C71 0.043(4) 0.041(4) 0.038(3) 0.006(3) -0.006(3) 0.003(3) C72 0.027(3) 0.021(3) 0.032(3) -0.001(2) -0.008(2) 0.002(3) C73 0.037(4) 0.055(5) 0.025(3) 0.006(3) -0.005(2) -0.005(3) C74 0.025(3) 0.039(4) 0.039(3) 0.000(3) 0.004(2) -0.003(3) C75 0.034(3) 0.024(4) 0.036(3) 0.000(3) -0.004(3) 0.007(3) C76 0.024(3) 0.026(4) 0.032(3) 0.001(2) 0.001(2) 0.000(3) C77 0.029(3) 0.024(4) 0.047(3) -0.004(3) -0.009(3) -0.004(3) C78 0.023(3) 0.066(5) 0.040(3) 0.007(3) 0.000(3) 0.000(3) C79 0.027(3) 0.027(4) 0.035(3) 0.003(3) -0.007(2) 0.005(3) C80 0.029(3) 0.033(4) 0.032(3) -0.002(3) -0.010(2) -0.004(3) C81 0.062(5) 0.077(6) 0.053(4) 0.000(4) 0.018(4) -0.018(4) B1 0.050(5) 0.037(6) 0.081(6) 0.007(5) 0.025(5) 0.012(4) F1 0.097(4) 0.078(4) 0.111(3) 0.033(3) 0.048(3) 0.017(3) F2 0.040(2) 0.058(3) 0.100(3) 0.000(2) -0.008(2) -0.007(2) F3 0.085(3) 0.048(3) 0.110(3) -0.015(2) 0.013(3) 0.018(3) F4 0.036(2) 0.054(3) 0.076(2) -0.0018(19) 0.0077(18) 0.0035(19) B2 0.060(7) 0.089(9) 0.070(6) 0.006(6) 0.022(5) -0.002(6) F5 0.086(5) 0.211(8) 0.164(5) 0.065(5) 0.022(4) -0.034(5) F6 0.219(9) 0.114(6) 0.156(5) 0.012(5) 0.036(5) 0.019(6) F7 0.100(4) 0.258(9) 0.072(3) 0.009(4) -0.002(3) -0.093(5) F8 0.112(5) 0.124(5) 0.096(3) 0.005(3) 0.026(3) -0.019(4) B3 0.036(4) 0.076(7) 0.033(4) 0.000(4) -0.009(3) -0.018(4) F9 0.037(2) 0.084(3) 0.060(2) -0.012(2) -0.0120(17) -0.001(2) F10 0.039(2) 0.111(4) 0.055(2) -0.023(2) -0.0010(17) -0.017(2) F11 0.035(2) 0.059(3) 0.071(2) 0.0037(19) 0.0098(17) -0.0004(19) F12 0.051(2) 0.059(3) 0.078(2) 0.019(2) 0.0007(19) -0.006(2) B4 0.102(7) 0.076(7) 0.087(6) 0.026(5) 0.057(6) -0.008(6) F13 0.179(6) 0.294(8) 0.129(4) -0.080(5) -0.044(4) 0.056(6) F14 0.257(7) 0.094(5) 0.187(5) -0.032(4) 0.128(5) -0.061(5) F15 0.235(7) 0.126(5) 0.110(4) -0.045(3) 0.079(4) -0.057(5) F16 0.079(3) 0.070(4) 0.198(5) -0.027(3) 0.006(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O8 1.444(4) . ? P1 O6 1.514(5) . ? P1 O7 1.547(5) . ? P1 O5 1.580(5) . ? P2 O4 1.471(4) . ? P2 O2 1.473(5) . ? P2 O3 1.504(4) . ? P2 O1 1.546(4) . ? O1 H1A 0.8200 . ? O3 H3A 0.9600 . ? O6 H6A 0.8200 . ? O7 H7A 0.9600 . ? N1 N2 1.322(6) . ? N1 C11 1.349(7) . ? N1 C9 1.442(7) . ? N2 N3 1.330(6) . ? N3 C12 1.385(8) . ? N3 C81 1.459(7) . ? N4 C16 1.362(7) . ? N4 C13 1.362(8) . ? N4 H4B 0.8600 . ? N5 C20 1.374(7) . ? N5 C23 1.376(7) . ? N5 H5B 0.8600 . ? N6 N7 1.326(6) . ? N6 C24 1.362(7) . ? N6 C26 1.464(7) . ? N7 N8 1.318(6) . ? N8 C25 1.335(7) . ? N8 C27 1.455(7) . ? N9 N10 1.314(6) . ? N9 C37 1.331(7) . ? N9 C31 1.460(6) . ? N10 N11 1.329(6) . ? N11 C38 1.354(7) . ? N11 C39 1.470(7) . ? N12 C43 1.368(7) . ? N12 C40 1.380(7) . ? N12 H12A 0.8600 . ? N13 C47 1.370(7) . ? N13 C50 1.398(7) . ? N13 H13A 0.8600 . ? N14 N15 1.326(6) . ? N14 C51 1.346(7) . ? N14 C53 1.465(7) . ? N15 N16 1.325(6) . ? N16 C52 1.352(7) . ? N16 C7 1.457(7) . ? N17 N18 1.319(6) . ? N17 C62 1.330(7) . ? N17 C60 1.438(7) . ? N18 N19 1.318(6) . ? N19 C63 1.356(7) . ? N19 C64 1.463(7) . ? N20 C68 1.367(7) . ? N20 C65 1.380(7) . ? N20 H20A 0.8600 . ? N21 C72 1.371(6) . ? N21 C75 1.398(7) . ? N21 H21A 0.8600 . ? N22 N23 1.330(6) . ? N22 C76 1.360(6) . ? N22 C78 1.453(7) . ? N23 N24 1.330(6) . ? N24 C77 1.348(6) . ? N24 C79 1.461(7) . ? C1 C4 1.513(8) . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C2 C4 1.541(9) . ? C2 H2C 0.9600 . ? C2 H2D 0.9600 . ? C2 H2E 0.9600 . ? C3 C4 1.521(8) . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C3 H3D 0.9600 . ? C4 C5 1.567(8) . ? C5 C10 1.395(7) . ? C5 C6 1.396(7) . ? C6 C7 1.357(8) . ? C6 H6B 0.9300 . ? C7 C8 1.389(7) . ? C8 C9 1.388(8) . ? C8 H8B 0.9300 . ? C9 C10 1.369(8) . ? C10 H10B 0.9300 . ? C11 C12 1.362(8) . ? C11 H11A 0.9300 . ? C12 C13 1.439(8) . ? C13 C14 1.377(8) . ? C14 C15 1.409(9) . ? C14 H14A 0.9300 . ? C15 C16 1.374(9) . ? C15 H15B 0.9300 . ? C16 C17 1.502(9) . ? C17 C18 1.516(8) . ? C17 C20 1.522(8) . ? C17 C19 1.552(8) . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C18 H18D 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.367(8) . ? C21 C22 1.422(8) . ? C21 H21B 0.9300 . ? C22 C23 1.389(7) . ? C22 H22A 0.9300 . ? C23 C24 1.445(7) . ? C24 C25 1.347(7) . ? C25 H25A 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C32 1.371(7) . ? C27 C28 1.385(8) . ? C28 C29 1.392(7) . ? C28 H28A 0.9300 . ? C29 C30 1.404(7) . ? C29 C33 1.520(8) . ? C30 C31 1.373(7) . ? C30 H30A 0.9300 . ? C31 C32 1.380(7) . ? C32 H32A 0.9300 . ? C33 C36 1.514(7) . ? C33 C34 1.526(8) . ? C33 C35 1.558(8) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.376(7) . ? C37 H37A 0.9300 . ? C38 C40 1.454(7) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.386(7) . ? C41 C42 1.419(8) . ? C41 H41A 0.9300 . ? C42 C43 1.372(8) . ? C42 H42A 0.9300 . ? C43 C44 1.511(8) . ? C44 C47 1.505(8) . ? C44 C46 1.522(7) . ? C44 C45 1.568(8) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C48 1.393(8) . ? C48 C49 1.405(8) . ? C48 H48A 0.9300 . ? C49 C50 1.376(7) . ? C49 H49A 0.9300 . ? C50 C51 1.459(7) . ? C51 C52 1.370(7) . ? C52 H52A 0.9300 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 C56 1.515(10) . ? C54 C58 1.519(8) . ? C54 C55' 1.52(3) . ? C54 C57' 1.55(3) . ? C54 C55 1.562(12) . ? C54 C57 1.563(10) . ? C54 C56' 1.66(3) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C55' H55D 0.9600 . ? C55' H55E 0.9600 . ? C55' H55F 0.9600 . ? C56' H56D 0.9600 . ? C56' H56E 0.9600 . ? C56' H56F 0.9600 . ? C57' H57D 0.9600 . ? C57' H57E 0.9600 . ? C57' H57F 0.9600 . ? C58 C59 1.402(8) . ? C58 C80 1.416(7) 3_765 ? C59 C60 1.390(8) . ? C59 H59A 0.9300 . ? C60 C61 1.380(7) . ? C61 C79 1.388(8) 3_765 ? C61 H61A 0.9300 . ? C62 C63 1.372(8) . ? C62 H62A 0.9300 . ? C63 C65 1.434(8) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 C66 1.402(8) . ? C66 C67 1.396(8) . ? C66 H66A 0.9300 . ? C67 C68 1.374(8) . ? C67 H67A 0.9300 . ? C68 C69 1.516(7) . ? C69 C72 1.520(7) . ? C69 C71 1.534(8) . ? C69 C70 1.534(8) . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 C73 1.371(7) . ? C73 C74 1.408(7) . ? C73 H73A 0.9300 . ? C74 C75 1.362(7) . ? C74 H74A 0.9300 . ? C75 C76 1.422(7) . ? C76 C77 1.370(7) . ? C77 H77A 0.9300 . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 C80 1.361(8) . ? C79 C61 1.388(8) 3_765 ? C80 C58 1.416(7) 3_765 ? C80 H80A 0.9300 . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? B1 F3 1.335(9) . ? B1 F1 1.370(9) . ? B1 F4 1.383(8) . ? B1 F2 1.432(10) . ? B2 F5 1.323(11) . ? B2 F7 1.337(10) . ? B2 F8 1.346(12) . ? B2 F6 1.392(13) . ? B3 F9 1.365(8) . ? B3 F10 1.392(8) . ? B3 F12 1.397(10) . ? B3 F11 1.410(8) . ? B4 F15 1.322(9) . ? B4 F14 1.345(10) . ? B4 F16 1.386(10) . ? B4 F13 1.407(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 P1 O6 112.5(3) . . ? O8 P1 O7 110.4(3) . . ? O6 P1 O7 112.8(3) . . ? O8 P1 O5 108.0(3) . . ? O6 P1 O5 107.1(3) . . ? O7 P1 O5 105.6(3) . . ? O4 P2 O2 115.3(3) . . ? O4 P2 O3 111.2(3) . . ? O2 P2 O3 109.0(3) . . ? O4 P2 O1 107.0(3) . . ? O2 P2 O1 108.3(3) . . ? O3 P2 O1 105.5(3) . . ? P2 O1 H1A 109.5 . . ? P2 O3 H3A 109.1 . . ? P1 O6 H6A 109.5 . . ? P1 O7 H7A 109.0 . . ? N2 N1 C11 113.2(4) . . ? N2 N1 C9 119.1(5) . . ? C11 N1 C9 127.8(5) . . ? N1 N2 N3 103.5(5) . . ? N2 N3 C12 112.8(4) . . ? N2 N3 C81 118.6(5) . . ? C12 N3 C81 128.6(5) . . ? C16 N4 C13 110.9(5) . . ? C16 N4 H4B 124.5 . . ? C13 N4 H4B 124.5 . . ? C20 N5 C23 111.4(4) . . ? C20 N5 H5B 124.3 . . ? C23 N5 H5B 124.3 . . ? N7 N6 C24 112.9(4) . . ? N7 N6 C26 117.6(5) . . ? C24 N6 C26 129.3(5) . . ? N8 N7 N6 102.6(4) . . ? N7 N8 C25 113.6(4) . . ? N7 N8 C27 118.8(5) . . ? C25 N8 C27 127.3(5) . . ? N10 N9 C37 113.7(4) . . ? N10 N9 C31 115.2(4) . . ? C37 N9 C31 131.1(5) . . ? N9 N10 N11 103.3(4) . . ? N10 N11 C38 112.8(4) . . ? N10 N11 C39 117.2(5) . . ? C38 N11 C39 129.8(5) . . ? C43 N12 C40 109.7(4) . . ? C43 N12 H12A 125.2 . . ? C40 N12 H12A 125.2 . . ? C47 N13 C50 109.1(4) . . ? C47 N13 H13A 125.4 . . ? C50 N13 H13A 125.4 . . ? N15 N14 C51 112.5(4) . . ? N15 N14 C53 115.3(5) . . ? C51 N14 C53 132.1(5) . . ? N16 N15 N14 103.7(4) . . ? N15 N16 C52 113.1(4) . . ? N15 N16 C7 116.1(4) . . ? C52 N16 C7 130.9(5) . . ? N18 N17 C62 112.7(5) . . ? N18 N17 C60 119.0(4) . . ? C62 N17 C60 128.2(5) . . ? N19 N18 N17 103.8(4) . . ? N18 N19 C63 113.1(5) . . ? N18 N19 C64 116.6(4) . . ? C63 N19 C64 130.3(5) . . ? C68 N20 C65 110.8(5) . . ? C68 N20 H20A 124.6 . . ? C65 N20 H20A 124.6 . . ? C72 N21 C75 108.8(4) . . ? C72 N21 H21A 125.6 . . ? C75 N21 H21A 125.6 . . ? N23 N22 C76 113.8(4) . . ? N23 N22 C78 115.6(4) . . ? C76 N22 C78 130.7(4) . . ? N22 N23 N24 103.3(4) . . ? N23 N24 C77 112.3(4) . . ? N23 N24 C79 118.4(4) . . ? C77 N24 C79 129.2(5) . . ? C4 C1 H1C 109.5 . . ? C4 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C4 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? C4 C2 H2C 109.5 . . ? C4 C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? C4 C2 H2E 109.5 . . ? H2C C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? C4 C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C4 C3 H3D 109.5 . . ? H3B C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? C1 C4 C3 110.9(5) . . ? C1 C4 C2 109.7(5) . . ? C3 C4 C2 109.3(5) . . ? C1 C4 C5 109.7(5) . . ? C3 C4 C5 110.2(4) . . ? C2 C4 C5 107.0(5) . . ? C10 C5 C6 117.6(5) . . ? C10 C5 C4 123.1(5) . . ? C6 C5 C4 119.3(5) . . ? C7 C6 C5 120.3(5) . . ? C7 C6 H6B 119.8 . . ? C5 C6 H6B 119.8 . . ? C6 C7 C8 123.5(5) . . ? C6 C7 N16 118.4(4) . . ? C8 C7 N16 118.0(5) . . ? C9 C8 C7 115.3(5) . . ? C9 C8 H8B 122.3 . . ? C7 C8 H8B 122.3 . . ? C10 C9 C8 122.9(5) . . ? C10 C9 N1 118.6(5) . . ? C8 C9 N1 118.5(5) . . ? C9 C10 C5 120.4(5) . . ? C9 C10 H10B 119.8 . . ? C5 C10 H10B 119.8 . . ? N1 C11 C12 106.7(5) . . ? N1 C11 H11A 126.6 . . ? C12 C11 H11A 126.6 . . ? C11 C12 N3 103.8(5) . . ? C11 C12 C13 130.6(6) . . ? N3 C12 C13 125.4(5) . . ? N4 C13 C14 107.5(5) . . ? N4 C13 C12 118.6(5) . . ? C14 C13 C12 133.8(6) . . ? C13 C14 C15 106.5(6) . . ? C13 C14 H14A 126.8 . . ? C15 C14 H14A 126.8 . . ? C16 C15 C14 108.8(5) . . ? C16 C15 H15B 125.6 . . ? C14 C15 H15B 125.6 . . ? N4 C16 C15 106.2(6) . . ? N4 C16 C17 122.8(5) . . ? C15 C16 C17 130.9(5) . . ? C16 C17 C18 110.9(5) . . ? C16 C17 C20 109.6(5) . . ? C18 C17 C20 107.6(5) . . ? C16 C17 C19 109.9(5) . . ? C18 C17 C19 108.2(5) . . ? C20 C17 C19 110.5(5) . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C18 H18D 109.5 . . ? H18B C18 H18D 109.5 . . ? H18C C18 H18D 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 N5 105.3(5) . . ? C21 C20 C17 131.7(5) . . ? N5 C20 C17 122.9(5) . . ? C20 C21 C22 110.5(5) . . ? C20 C21 H21B 124.7 . . ? C22 C21 H21B 124.7 . . ? C23 C22 C21 105.4(5) . . ? C23 C22 H22A 127.3 . . ? C21 C22 H22A 127.3 . . ? N5 C23 C22 107.4(5) . . ? N5 C23 C24 118.8(5) . . ? C22 C23 C24 133.8(6) . . ? C25 C24 N6 104.6(5) . . ? C25 C24 C23 129.4(5) . . ? N6 C24 C23 126.0(5) . . ? N8 C25 C24 106.2(5) . . ? N8 C25 H25A 126.9 . . ? C24 C25 H25A 126.9 . . ? N6 C26 H26A 109.5 . . ? N6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 123.2(5) . . ? C32 C27 N8 120.3(5) . . ? C28 C27 N8 116.5(5) . . ? C27 C28 C29 120.4(5) . . ? C27 C28 H28A 119.8 . . ? C29 C28 H28A 119.8 . . ? C28 C29 C30 116.7(5) . . ? C28 C29 C33 121.3(5) . . ? C30 C29 C33 122.0(4) . . ? C31 C30 C29 120.8(5) . . ? C31 C30 H30A 119.6 . . ? C29 C30 H30A 119.6 . . ? C30 C31 C32 122.9(5) . . ? C30 C31 N9 116.4(4) . . ? C32 C31 N9 120.7(5) . . ? C27 C32 C31 115.9(5) . . ? C27 C32 H32A 122.1 . . ? C31 C32 H32A 122.1 . . ? C36 C33 C29 112.6(5) . . ? C36 C33 C34 109.4(5) . . ? C29 C33 C34 109.4(4) . . ? C36 C33 C35 109.5(5) . . ? C29 C33 C35 107.6(5) . . ? C34 C33 C35 108.3(5) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N9 C37 C38 105.7(5) . . ? N9 C37 H37A 127.2 . . ? C38 C37 H37A 127.2 . . ? N11 C38 C37 104.4(5) . . ? N11 C38 C40 124.4(5) . . ? C37 C38 C40 131.2(5) . . ? N11 C39 H39A 109.5 . . ? N11 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N11 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N12 C40 C41 107.9(5) . . ? N12 C40 C38 120.5(5) . . ? C41 C40 C38 131.5(5) . . ? C40 C41 C42 106.2(5) . . ? C40 C41 H41A 126.9 . . ? C42 C41 H41A 126.9 . . ? C43 C42 C41 108.7(5) . . ? C43 C42 H42A 125.6 . . ? C41 C42 H42A 125.6 . . ? N12 C43 C42 107.5(5) . . ? N12 C43 C44 123.2(5) . . ? C42 C43 C44 129.2(5) . . ? C47 C44 C43 106.8(4) . . ? C47 C44 C46 110.1(5) . . ? C43 C44 C46 109.9(5) . . ? C47 C44 C45 111.1(5) . . ? C43 C44 C45 111.2(5) . . ? C46 C44 C45 107.7(4) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N13 C47 C48 107.7(5) . . ? N13 C47 C44 123.3(5) . . ? C48 C47 C44 128.8(5) . . ? C47 C48 C49 107.7(5) . . ? C47 C48 H48A 126.1 . . ? C49 C48 H48A 126.1 . . ? C50 C49 C48 108.1(5) . . ? C50 C49 H49A 126.0 . . ? C48 C49 H49A 126.0 . . ? C49 C50 N13 107.4(5) . . ? C49 C50 C51 131.5(6) . . ? N13 C50 C51 121.1(5) . . ? N14 C51 C52 106.0(5) . . ? N14 C51 C50 122.4(5) . . ? C52 C51 C50 131.5(6) . . ? N16 C52 C51 104.7(5) . . ? N16 C52 H52A 127.6 . . ? C51 C52 H52A 127.6 . . ? N14 C53 H53A 109.5 . . ? N14 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N14 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C56 C54 C58 113.1(6) . . ? C56 C54 C55' 121.4(17) . . ? C58 C54 C55' 122.2(17) . . ? C56 C54 C57' 64.4(12) . . ? C58 C54 C57' 110.6(14) . . ? C55' C54 C57' 108.7(18) . . ? C56 C54 C55 108.1(7) . . ? C58 C54 C55 108.9(6) . . ? C55' C54 C55 71.7(15) . . ? C57' C54 C55 47.1(13) . . ? C56 C54 C57 111.4(7) . . ? C58 C54 C57 109.3(6) . . ? C55' C54 C57 34.1(14) . . ? C57' C54 C57 137.5(14) . . ? C55 C54 C57 105.7(8) . . ? C56 C54 C56' 38.6(12) . . ? C58 C54 C56' 107.3(15) . . ? C55' C54 C56' 103.7(16) . . ? C57' C54 C56' 102.3(13) . . ? C55 C54 C56' 139.3(14) . . ? C57 C54 C56' 78.9(14) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C54 C55' H55D 109.5 . . ? C54 C55' H55E 109.5 . . ? H55D C55' H55E 109.5 . . ? C54 C55' H55F 109.5 . . ? H55D C55' H55F 109.5 . . ? H55E C55' H55F 109.5 . . ? C54 C56' H56D 109.5 . . ? C54 C56' H56E 109.5 . . ? H56D C56' H56E 109.5 . . ? C54 C56' H56F 109.5 . . ? H56D C56' H56F 109.5 . . ? H56E C56' H56F 109.5 . . ? C54 C57' H57D 109.5 . . ? C54 C57' H57E 109.5 . . ? H57D C57' H57E 109.5 . . ? C54 C57' H57F 109.5 . . ? H57D C57' H57F 109.5 . . ? H57E C57' H57F 109.5 . . ? C59 C58 C80 118.0(5) . 3_765 ? C59 C58 C54 120.9(5) . . ? C80 C58 C54 120.9(5) 3_765 . ? C60 C59 C58 119.8(5) . . ? C60 C59 H59A 120.1 . . ? C58 C59 H59A 120.1 . . ? C61 C60 C59 123.2(5) . . ? C61 C60 N17 116.7(5) . . ? C59 C60 N17 120.1(5) . . ? C60 C61 C79 115.2(5) . 3_765 ? C60 C61 H61A 122.4 . . ? C79 C61 H61A 122.4 3_765 . ? N17 C62 C63 106.5(5) . . ? N17 C62 H62A 126.8 . . ? C63 C62 H62A 126.8 . . ? N19 C63 C62 103.9(5) . . ? N19 C63 C65 125.6(5) . . ? C62 C63 C65 130.5(5) . . ? N19 C64 H64A 109.5 . . ? N19 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N19 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N20 C65 C66 106.1(5) . . ? N20 C65 C63 121.0(5) . . ? C66 C65 C63 132.9(5) . . ? C67 C66 C65 107.4(5) . . ? C67 C66 H66A 126.3 . . ? C65 C66 H66A 126.3 . . ? C68 C67 C66 108.9(5) . . ? C68 C67 H67A 125.5 . . ? C66 C67 H67A 125.5 . . ? N20 C68 C67 106.8(5) . . ? N20 C68 C69 122.5(5) . . ? C67 C68 C69 130.6(5) . . ? C68 C69 C72 111.2(4) . . ? C68 C69 C71 108.1(5) . . ? C72 C69 C71 110.6(5) . . ? C68 C69 C70 109.6(5) . . ? C72 C69 C70 108.8(5) . . ? C71 C69 C70 108.5(4) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N21 C72 C73 108.3(4) . . ? N21 C72 C69 122.7(5) . . ? C73 C72 C69 129.1(4) . . ? C72 C73 C74 107.2(5) . . ? C72 C73 H73A 126.4 . . ? C74 C73 H73A 126.4 . . ? C75 C74 C73 108.7(5) . . ? C75 C74 H74A 125.6 . . ? C73 C74 H74A 125.6 . . ? C74 C75 N21 107.0(4) . . ? C74 C75 C76 133.9(5) . . ? N21 C75 C76 118.8(4) . . ? N22 C76 C77 103.8(4) . . ? N22 C76 C75 124.7(5) . . ? C77 C76 C75 131.3(5) . . ? N24 C77 C76 106.9(5) . . ? N24 C77 H77A 126.6 . . ? C76 C77 H77A 126.6 . . ? N22 C78 H78A 109.5 . . ? N22 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? N22 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C80 C79 C61 124.9(5) . 3_765 ? C80 C79 N24 119.3(5) . . ? C61 C79 N24 115.8(5) 3_765 . ? C79 C80 C58 118.9(5) . 3_765 ? C79 C80 H80A 120.5 . . ? C58 C80 H80A 120.5 3_765 . ? N3 C81 H81A 109.5 . . ? N3 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? N3 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? F3 B1 F1 111.3(6) . . ? F3 B1 F4 112.6(7) . . ? F1 B1 F4 110.2(7) . . ? F3 B1 F2 108.5(7) . . ? F1 B1 F2 106.3(7) . . ? F4 B1 F2 107.6(6) . . ? F5 B2 F7 111.1(9) . . ? F5 B2 F8 109.9(9) . . ? F7 B2 F8 109.1(9) . . ? F5 B2 F6 106.9(10) . . ? F7 B2 F6 111.7(9) . . ? F8 B2 F6 108.1(9) . . ? F9 B3 F10 110.0(6) . . ? F9 B3 F12 111.3(6) . . ? F10 B3 F12 109.8(6) . . ? F9 B3 F11 109.4(5) . . ? F10 B3 F11 108.0(6) . . ? F12 B3 F11 108.2(6) . . ? F15 B4 F14 116.4(7) . . ? F15 B4 F16 110.4(9) . . ? F14 B4 F16 109.8(8) . . ? F15 B4 F13 107.6(8) . . ? F14 B4 F13 107.8(9) . . ? F16 B4 F13 104.0(7) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.798 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.077