data_51022d _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H65 F12 N5 O10 P2' _chemical_formula_weight 1234.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.62(3) _cell_length_b 15.32(3) _cell_length_c 16.28(3) _cell_angle_alpha 84.07(4) _cell_angle_beta 88.28(4) _cell_angle_gamma 64.43(3) _cell_volume 3272(12) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 3251 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 21.81 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1284 _exptl_absorpt_coefficient_mu 0.154 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.814128 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16108 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0844 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11333 _reflns_number_gt 4726 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 SHELXL _refine_ls_extinction_coef 0.0008(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11333 _refine_ls_number_parameters 882 _refine_ls_number_restraints 470 _refine_ls_R_factor_all 0.2039 _refine_ls_R_factor_gt 0.1047 _refine_ls_wR_factor_ref 0.3844 _refine_ls_wR_factor_gt 0.3039 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.181 _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 O1 O 0.5335(3) 0.4620(3) 0.8177(3) 0.0749(13) Uani 1 1 d . . . O2 O 0.7293(4) 0.3039(5) 0.8851(3) 0.126(2) Uani 1 1 d . . . O3 O 0.9086(4) 0.1861(4) 0.7883(3) 0.1042(19) Uani 1 1 d . . . O4 O 0.8996(4) 0.1898(4) 0.6114(3) 0.109(2) Uani 1 1 d . . . O5 O 0.4453(3) 0.3487(3) 0.7640(3) 0.0805(14) Uani 1 1 d . . . O6 O 0.5626(3) 0.1425(3) 0.7515(2) 0.0639(11) Uani 1 1 d . . . O7 O 0.7133(3) -0.0275(3) 0.6705(3) 0.0733(13) Uani 1 1 d . . . O8 O 0.8271(4) 0.0652(4) 0.5595(3) 0.1000(17) Uani 1 1 d . . . C1 C 0.2009(4) 0.7700(4) 0.7459(3) 0.0520(14) Uani 1 1 d . . . C2 C 0.2713(4) 0.6570(4) 0.7545(3) 0.0476(14) Uani 1 1 d . . . C3 C 0.3739(4) 0.6094(4) 0.7856(3) 0.0554(15) Uani 1 1 d . . . H3 H 0.4039 0.6464 0.8043 0.067 Uiso 1 1 calc R . . C4 C 0.4300(4) 0.5077(4) 0.7883(4) 0.0575(16) Uani 1 1 d . . . C5 C 0.3821(5) 0.4501(4) 0.7592(4) 0.0586(16) Uani 1 1 d . . . C6 C 0.2783(4) 0.4965(4) 0.7277(4) 0.0573(15) Uani 1 1 d . . . H6 H 0.2484 0.4594 0.7089 0.069 Uiso 1 1 calc R . . C7 C 0.2228(4) 0.5992(4) 0.7259(3) 0.0502(14) Uani 1 1 d . . . C8 C 0.1078(4) 0.6624(4) 0.6915(4) 0.0552(15) Uani 1 1 d . . . C9 C 0.1192(4) 0.7376(4) 0.6208(3) 0.0547(15) Uani 1 1 d . . . C10 C 0.0916(5) 0.7487(5) 0.5351(4) 0.0684(18) Uani 1 1 d . . . H10 H 0.0595 0.7129 0.5176 0.082 Uiso 1 1 calc R . . C11 C 0.1119(5) 0.8125(5) 0.4769(4) 0.0728(19) Uani 1 1 d . . . C12 C 0.1564(5) 0.8728(5) 0.5038(4) 0.074(2) Uani 1 1 d . . . C13 C 0.1838(5) 0.8655(4) 0.5916(4) 0.0647(17) Uani 1 1 d . . . H13 H 0.2112 0.9050 0.6095 0.078 Uiso 1 1 calc R . . C14 C 0.1671(4) 0.7955(4) 0.6491(3) 0.0556(15) Uani 1 1 d . . . C15 C 0.0963(3) 0.7800(3) 0.7949(2) 0.0574(16) Uani 1 1 d G . . C16 C 0.0550(4) 0.8366(3) 0.8599(3) 0.0710(19) Uani 1 1 d G . . H16 H 0.0857 0.8732 0.8781 0.085 Uiso 1 1 calc R . . C17 C -0.0322(4) 0.8383(3) 0.8976(2) 0.094(3) Uani 1 1 d G . . H17 H -0.0599 0.8762 0.9410 0.113 Uiso 1 1 calc R . . C18 C -0.0782(3) 0.7836(4) 0.8704(3) 0.092(2) Uani 1 1 d G . . H18 H -0.1365 0.7848 0.8956 0.111 Uiso 1 1 calc R . . C19 C -0.0369(3) 0.7271(3) 0.8054(3) 0.080(2) Uani 1 1 d G . . H19 H -0.0676 0.6904 0.7872 0.096 Uiso 1 1 calc R . . C20 C 0.0504(3) 0.7253(3) 0.7677(2) 0.0625(17) Uani 1 1 d G . . C21 C 0.2536(5) 0.8318(5) 0.7760(4) 0.0709(18) Uani 1 1 d . . . H21A H 0.2769 0.8092 0.8321 0.106 Uiso 1 1 calc R . . H21B H 0.2059 0.8990 0.7727 0.106 Uiso 1 1 calc R . . H21C H 0.3103 0.8247 0.7414 0.106 Uiso 1 1 calc R . . C22 C 0.0556(5) 0.5992(5) 0.6618(5) 0.078(2) Uani 1 1 d . . . H22A H -0.0130 0.6410 0.6446 0.117 Uiso 1 1 calc R . . H22B H 0.0558 0.5531 0.7066 0.117 Uiso 1 1 calc R . . H22C H 0.0924 0.5652 0.6164 0.117 Uiso 1 1 calc R . . C23 C 0.5513(6) 0.4159(7) 0.9019(5) 0.114(3) Uani 1 1 d . . . H23A H 0.5093 0.4637 0.9380 0.137 Uiso 1 1 calc R . . H23B H 0.5287 0.3647 0.9058 0.137 Uiso 1 1 calc R . . C24 C 0.6549(6) 0.3742(7) 0.9327(5) 0.121(4) Uani 1 1 d . . . H24A H 0.6743 0.4268 0.9365 0.145 Uiso 1 1 calc R . . H24B H 0.6568 0.3437 0.9883 0.145 Uiso 1 1 calc R . . C25 C 0.8225(8) 0.2419(8) 0.9177(5) 0.146(5) Uani 1 1 d . . . H25A H 0.8116 0.2132 0.9709 0.175 Uiso 1 1 calc R . . H25B H 0.8573 0.2811 0.9284 0.175 Uiso 1 1 calc R . . C26 C 0.8904(7) 0.1644(7) 0.8738(5) 0.123(4) Uani 1 1 d . . . H26A H 0.8650 0.1152 0.8766 0.147 Uiso 1 1 calc R . . H26B H 0.9552 0.1355 0.9030 0.147 Uiso 1 1 calc R . . C27 C 0.9768(6) 0.1161(8) 0.7455(5) 0.137(4) Uani 1 1 d . . . H27A H 0.9659 0.0583 0.7593 0.164 Uiso 1 1 calc R . . H27B H 1.0432 0.1018 0.7677 0.164 Uiso 1 1 calc R . . C28 C 0.9839(6) 0.1273(7) 0.6562(4) 0.100(3) Uani 1 1 d . . . H28A H 1.0371 0.1481 0.6432 0.120 Uiso 1 1 calc R . . H28B H 1.0059 0.0636 0.6370 0.120 Uiso 1 1 calc R . . C29 C 0.3970(5) 0.2810(4) 0.7649(5) 0.0727(19) Uani 1 1 d . . . H29A H 0.3794 0.2762 0.7091 0.087 Uiso 1 1 calc R . . H29B H 0.3357 0.3042 0.7971 0.087 Uiso 1 1 calc R . . C30 C 0.4735(5) 0.1819(4) 0.8035(4) 0.075(2) Uani 1 1 d . . . H30A H 0.4941 0.1884 0.8578 0.090 Uiso 1 1 calc R . . H30B H 0.4420 0.1374 0.8102 0.090 Uiso 1 1 calc R . . C31 C 0.6474(5) 0.0569(5) 0.7934(4) 0.0692(18) Uani 1 1 d . . . H31A H 0.6258 0.0061 0.8095 0.083 Uiso 1 1 calc R . . H31B H 0.6676 0.0747 0.8429 0.083 Uiso 1 1 calc R . . C32 C 0.7370(5) 0.0197(5) 0.7354(4) 0.0741(19) Uani 1 1 d . . . H32A H 0.7502 0.0734 0.7107 0.089 Uiso 1 1 calc R . . H32B H 0.7972 -0.0265 0.7660 0.089 Uiso 1 1 calc R . . C33 C 0.8019(5) -0.0808(5) 0.6181(4) 0.081(2) Uani 1 1 d . . . H33A H 0.7982 -0.1388 0.6030 0.097 Uiso 1 1 calc R . . H33B H 0.8641 -0.1010 0.6498 0.097 Uiso 1 1 calc R . . C34 C 0.8050(6) -0.0146(6) 0.5354(5) 0.098(3) Uani 1 1 d . . . H34A H 0.8572 -0.0536 0.4991 0.118 Uiso 1 1 calc R . . H34B H 0.7403 0.0121 0.5063 0.118 Uiso 1 1 calc R . . C35 C 0.5120(6) 0.7243(6) 0.6219(4) 0.084(2) Uani 1 1 d . . . H35A H 0.5338 0.7039 0.6766 0.101 Uiso 1 1 calc R . . C36 C 0.4666(5) 0.6744(5) 0.5810(4) 0.076(2) Uani 1 1 d . A . H36A H 0.4591 0.6226 0.6105 0.092 Uiso 1 1 calc R . . C37 C 0.4310(4) 0.7011(4) 0.4938(3) 0.0657(18) Uani 1 1 d D . . C38 C 0.4472(5) 0.7851(5) 0.4548(4) 0.0734(19) Uani 1 1 d . A . H38A H 0.4270 0.8076 0.4000 0.088 Uiso 1 1 calc R . . C39 C 0.4925(5) 0.8319(5) 0.4985(5) 0.084(2) Uani 1 1 d . . . H39A H 0.5017 0.8839 0.4713 0.101 Uiso 1 1 calc R A . C45 C 0.5687(6) 0.8582(6) 0.6287(5) 0.094(2) Uani 1 1 d . . . H45A H 0.6044 0.8855 0.5909 0.113 Uiso 1 1 calc R A . H45B H 0.6165 0.8139 0.6707 0.113 Uiso 1 1 calc R . . C46 C 0.4807(6) 0.9413(6) 0.6698(5) 0.098(2) Uani 1 1 d . A . H46A H 0.4455 0.9143 0.7084 0.118 Uiso 1 1 calc R . . H46B H 0.5074 0.9771 0.6997 0.118 Uiso 1 1 calc R . . C40 C 0.2700(10) 0.5664(9) 0.4597(6) 0.080(4) Uani 0.50 1 d PGDU A 1 H40A H 0.2404 0.5317 0.4913 0.096 Uiso 0.50 1 calc PR A 1 C41 C 0.3377(12) 0.5930(11) 0.4962(6) 0.077(2) Uani 0.50 1 d PGDU A 1 H41A H 0.3534 0.5761 0.5523 0.092 Uiso 0.50 1 calc PR A 1 C42 C 0.3820(12) 0.6450(12) 0.4490(7) 0.057(2) Uani 0.50 1 d PGDU A 1 C43 C 0.3586(13) 0.6703(13) 0.3652(6) 0.072(2) Uani 0.50 1 d PGDU A 1 H43A H 0.3882 0.7050 0.3336 0.086 Uiso 0.50 1 calc PR A 1 C44 C 0.2909(11) 0.6437(10) 0.3287(5) 0.076(3) Uani 0.50 1 d PGDU A 1 H44A H 0.2753 0.6607 0.2726 0.091 Uiso 0.50 1 calc PR A 1 N2 N 0.2466(6) 0.5918(6) 0.3759(6) 0.078(3) Uani 0.50 1 d PGDU A 1 C47 C 0.1734(8) 0.5640(10) 0.3346(10) 0.130(5) Uani 0.50 1 d PDU A 1 H47A H 0.1160 0.5750 0.3704 0.157 Uiso 0.50 1 calc PR A 1 H47B H 0.1481 0.6063 0.2838 0.157 Uiso 0.50 1 calc PR A 1 C48 C 0.2187(16) 0.4608(13) 0.3151(15) 0.212(10) Uani 0.50 1 d PDU A 1 H48A H 0.2473 0.4184 0.3653 0.255 Uiso 0.50 1 calc PR A 1 H48B H 0.1656 0.4461 0.2950 0.255 Uiso 0.50 1 calc PR A 1 O10 O 0.2955(14) 0.4415(13) 0.2549(12) 0.214(6) Uani 0.50 1 d PDU A 1 H10A H 0.3498 0.4289 0.2774 0.321 Uiso 0.50 1 d PR A 1 C40' C 0.3003(10) 0.5462(9) 0.4445(6) 0.080(4) Uani 0.50 1 d PGDU A 2 H40B H 0.2800 0.5013 0.4719 0.096 Uiso 0.50 1 calc PR A 2 C41' C 0.3426(12) 0.5929(11) 0.4889(5) 0.077(2) Uani 0.50 1 d PGDU A 2 H41B H 0.3506 0.5792 0.5459 0.092 Uiso 0.50 1 calc PR A 2 C42' C 0.3730(13) 0.6599(11) 0.4480(6) 0.057(2) Uani 0.50 1 d PGDU A 2 C43' C 0.3611(14) 0.6803(12) 0.3627(6) 0.072(2) Uani 0.50 1 d PGDU A 2 H43B H 0.3814 0.7252 0.3354 0.086 Uiso 0.50 1 calc PR A 2 C44' C 0.3188(11) 0.6337(10) 0.3184(5) 0.076(3) Uani 0.50 1 d PGDU A 2 H44B H 0.3108 0.6473 0.2613 0.091 Uiso 0.50 1 calc PR A 2 N2' N 0.2884(6) 0.5666(7) 0.3593(6) 0.078(3) Uani 0.50 1 d PGDU A 2 C47' C 0.2431(9) 0.5183(10) 0.3077(9) 0.130(5) Uani 0.50 1 d PDU A 2 H47C H 0.2746 0.5101 0.2540 0.157 Uiso 0.50 1 calc PR A 2 H47D H 0.2558 0.4544 0.3345 0.157 Uiso 0.50 1 calc PR A 2 C48' C 0.1305(11) 0.5797(18) 0.2972(12) 0.212(10) Uani 0.50 1 d PDU A 2 H48C H 0.1175 0.6453 0.2752 0.255 Uiso 0.50 1 calc PR A 2 H48D H 0.1029 0.5528 0.2585 0.255 Uiso 0.50 1 calc PR A 2 O10' O 0.0828(11) 0.5814(15) 0.3755(12) 0.214(6) Uani 0.50 1 d PDU A 2 H10' H 0.0962 0.6153 0.4045 0.321 Uiso 0.50 1 d PR A 2 N1 N 0.5238(4) 0.8026(4) 0.5811(4) 0.0800(17) Uani 1 1 d U A . O9 O 0.4122(5) 1.0049(4) 0.6047(4) 0.117(2) Uani 1 1 d U . . H9 H 0.3561 1.0353 0.6239 0.175 Uiso 1 1 d R A . P1 P 0.8056(3) 0.6825(3) 0.4589(4) 0.0763(12) Uani 0.735(12) 1 d PDU B 1 F1 F 0.7774(6) 0.7043(5) 0.5520(5) 0.150(4) Uani 0.735(12) 1 d PDU B 1 F2 F 0.8850(6) 0.7253(8) 0.4623(6) 0.171(4) Uani 0.735(12) 1 d PDU B 1 F3 F 0.8850(5) 0.5782(5) 0.4902(4) 0.127(3) Uani 0.735(12) 1 d PDU B 1 F4 F 0.7204(6) 0.6434(6) 0.4561(5) 0.138(3) Uani 0.735(12) 1 d PDU B 1 F5 F 0.7198(6) 0.7877(4) 0.4309(6) 0.156(4) Uani 0.735(12) 1 d PDU B 1 F6 F 0.8285(6) 0.6613(5) 0.3647(4) 0.123(3) Uani 0.735(12) 1 d PDU B 1 P2 P 0.3998(5) 0.2591(5) 0.0884(4) 0.1170(11) Uani 0.679(15) 1 d PDU C 1 F7 F 0.3041(8) 0.2892(10) 0.1460(8) 0.215(6) Uani 0.679(15) 1 d PDU C 1 F8 F 0.3752(9) 0.3696(5) 0.0673(8) 0.191(6) Uani 0.679(15) 1 d PDU C 1 F9 F 0.4678(8) 0.2531(8) 0.1639(5) 0.157(5) Uani 0.679(15) 1 d PDU C 1 F10 F 0.4207(9) 0.1496(6) 0.1118(7) 0.196(6) Uani 0.679(15) 1 d PDU C 1 F11 F 0.3296(10) 0.2658(9) 0.0140(7) 0.252(8) Uani 0.679(15) 1 d PDU C 1 F12 F 0.4934(7) 0.2277(7) 0.0314(6) 0.200(6) Uani 0.679(15) 1 d PDU C 1 P1' P 0.8163(9) 0.7016(9) 0.4314(8) 0.0763(12) Uani 0.265(12) 1 d PDU B 2 F1' F 0.7746(18) 0.7199(18) 0.5202(11) 0.34(4) Uani 0.265(12) 1 d PDU B 2 F2' F 0.8464(18) 0.7875(15) 0.4296(14) 0.151(10) Uani 0.265(12) 1 d PDU B 2 F3' F 0.9237(13) 0.6297(17) 0.4678(13) 0.155(10) Uani 0.265(12) 1 d PDU B 2 F4' F 0.787(2) 0.6142(13) 0.4324(15) 0.160(11) Uani 0.265(12) 1 d PDU B 2 F5' F 0.7096(11) 0.7727(14) 0.3935(15) 0.183(15) Uani 0.265(12) 1 d PDU B 2 F6' F 0.8576(17) 0.6813(17) 0.3421(9) 0.162(12) Uani 0.265(12) 1 d PDU B 2 P2' P 0.3891(10) 0.2646(10) 0.0944(9) 0.1170(11) Uani 0.321(15) 1 d PDU C 2 F7' F 0.391(2) 0.3102(19) 0.1760(12) 0.251(16) Uani 0.321(15) 1 d PDU C 2 F8' F 0.4038(19) 0.3491(17) 0.0426(16) 0.33(3) Uani 0.321(15) 1 d PDU C 2 F9' F 0.5064(11) 0.2036(19) 0.102(2) 0.36(3) Uani 0.321(15) 1 d PDU C 2 F10' F 0.3732(18) 0.1803(13) 0.1462(13) 0.169(10) Uani 0.321(15) 1 d PDU C 2 F11' F 0.2713(10) 0.3252(12) 0.0878(14) 0.145(9) Uani 0.321(15) 1 d PDU C 2 F12' F 0.387(2) 0.2192(18) 0.0127(11) 0.210(13) Uani 0.321(15) 1 d PDU C 2 N3 N 0.1945(8) -0.0192(7) 0.9565(6) 0.138(3) Uani 1 1 d U . . C49 C 0.2644(11) -0.0049(9) 0.9589(7) 0.133(4) Uani 1 1 d U . . C50 C 0.3545(11) 0.0190(11) 0.9617(9) 0.197(6) Uani 1 1 d U . . H50A H 0.3334 0.0817 0.9814 0.296 Uiso 1 1 calc R . . H50B H 0.3815 0.0198 0.9073 0.296 Uiso 1 1 calc R . . H50C H 0.4058 -0.0293 0.9983 0.296 Uiso 1 1 calc R . . N4 N 0.2566(10) 0.0908(10) 0.7471(8) 0.194(5) Uani 1 1 d U . . C51 C 0.2062(11) 0.1563(12) 0.7844(9) 0.167(5) Uani 1 1 d U . . C52 C 0.1377(12) 0.2401(12) 0.8350(10) 0.217(6) Uani 1 1 d U . . H52A H 0.0678 0.2560 0.8241 0.325 Uiso 1 1 calc R . . H52B H 0.1501 0.2961 0.8196 0.325 Uiso 1 1 calc R . . H52C H 0.1525 0.2202 0.8928 0.325 Uiso 1 1 calc R . . C54 C 0.073(4) 0.535(5) 0.094(2) 0.288(14) Uani 0.50 1 d PDU D 1 H54A H 0.0673 0.5895 0.1220 0.432 Uiso 0.50 1 calc PR D 1 H54B H 0.1151 0.4757 0.1265 0.432 Uiso 0.50 1 calc PR D 1 H54C H 0.0072 0.5379 0.0865 0.432 Uiso 0.50 1 calc PR D 1 C53 C 0.1203(18) 0.5388(18) 0.0118(14) 0.150(8) Uani 0.50 1 d PDU D 1 N5 N 0.1588(13) 0.5296(13) -0.0483(12) 0.120(5) Uani 0.50 1 d PDU D 1 N5' N -0.122(3) 0.513(3) 0.083(2) 0.272(17) Uani 0.50 1 d PDU E 2 C53' C -0.067(3) 0.540(3) 0.1043(19) 0.201(13) Uani 0.50 1 d PDU E 2 C54' C 0.029(4) 0.555(5) 0.100(3) 0.288(14) Uani 0.50 1 d PDU E 2 H54D H 0.0350 0.5832 0.1488 0.432 Uiso 0.50 1 calc PR E 2 H54E H 0.0264 0.5982 0.0522 0.432 Uiso 0.50 1 calc PR E 2 H54F H 0.0869 0.4938 0.0973 0.432 Uiso 0.50 1 calc PR E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.050(3) 0.077(3) 0.083(3) 0.001(2) -0.006(2) -0.015(2) O2 0.071(3) 0.166(6) 0.057(3) 0.004(3) -0.012(3) 0.024(4) O3 0.121(4) 0.091(4) 0.051(3) -0.006(3) 0.001(3) 0.001(3) O4 0.091(4) 0.125(5) 0.054(3) -0.010(3) -0.011(3) 0.008(3) O5 0.055(3) 0.045(3) 0.128(4) 0.000(2) 0.002(3) -0.011(2) O6 0.070(3) 0.052(2) 0.051(2) 0.0050(19) 0.002(2) -0.010(2) O7 0.074(3) 0.069(3) 0.076(3) -0.013(2) 0.014(2) -0.030(2) O8 0.124(4) 0.085(4) 0.083(3) 0.008(3) 0.017(3) -0.042(3) C1 0.054(4) 0.046(3) 0.054(3) -0.007(3) -0.004(3) -0.019(3) C2 0.048(3) 0.043(3) 0.045(3) -0.003(2) -0.003(3) -0.013(3) C3 0.056(4) 0.052(4) 0.056(4) -0.001(3) -0.007(3) -0.022(3) C4 0.039(3) 0.058(4) 0.063(4) 0.000(3) 0.000(3) -0.011(3) C5 0.058(4) 0.040(3) 0.067(4) 0.001(3) 0.008(3) -0.013(3) C6 0.045(3) 0.048(4) 0.073(4) -0.005(3) -0.003(3) -0.014(3) C7 0.043(3) 0.044(3) 0.055(3) 0.002(3) -0.007(3) -0.012(3) C8 0.044(3) 0.052(3) 0.063(4) 0.001(3) -0.014(3) -0.015(3) C9 0.048(3) 0.048(3) 0.054(4) -0.002(3) -0.012(3) -0.008(3) C10 0.060(4) 0.063(4) 0.068(4) -0.012(4) -0.007(3) -0.012(3) C11 0.065(4) 0.072(5) 0.060(4) -0.011(4) -0.003(3) -0.008(4) C12 0.071(5) 0.058(4) 0.062(4) 0.009(3) 0.017(3) -0.003(4) C13 0.068(4) 0.051(4) 0.063(4) 0.000(3) 0.001(3) -0.016(3) C14 0.054(4) 0.045(3) 0.051(3) -0.002(3) 0.001(3) -0.006(3) C15 0.062(4) 0.053(4) 0.045(3) 0.004(3) -0.011(3) -0.015(3) C16 0.065(4) 0.066(4) 0.059(4) -0.005(3) 0.007(3) -0.008(4) C17 0.103(6) 0.078(5) 0.063(5) -0.007(4) 0.008(4) -0.004(5) C18 0.061(5) 0.092(6) 0.094(6) 0.007(5) 0.015(4) -0.010(4) C19 0.053(4) 0.087(5) 0.085(5) 0.008(4) 0.000(4) -0.019(4) C20 0.053(4) 0.055(4) 0.064(4) 0.007(3) -0.009(3) -0.011(3) C21 0.076(5) 0.059(4) 0.080(4) -0.011(3) -0.006(4) -0.031(4) C22 0.064(4) 0.069(4) 0.103(5) -0.003(4) -0.021(4) -0.031(4) C23 0.074(5) 0.150(8) 0.069(5) -0.022(5) -0.007(4) 0.000(5) C24 0.081(6) 0.147(8) 0.071(5) -0.009(5) -0.010(4) 0.010(6) C25 0.141(9) 0.140(8) 0.052(5) 0.009(5) -0.012(5) 0.033(7) C26 0.102(6) 0.128(8) 0.061(5) 0.005(5) -0.011(4) 0.020(6) C27 0.086(6) 0.180(10) 0.058(5) 0.019(6) -0.001(4) 0.017(6) C28 0.078(5) 0.135(7) 0.072(5) -0.022(5) -0.007(4) -0.029(5) C29 0.062(4) 0.052(4) 0.102(5) -0.009(4) 0.011(4) -0.022(3) C30 0.082(5) 0.047(4) 0.085(5) -0.006(3) 0.024(4) -0.019(4) C31 0.077(5) 0.057(4) 0.054(4) 0.006(3) -0.013(3) -0.013(4) C32 0.066(4) 0.066(4) 0.071(4) 0.005(4) -0.017(4) -0.012(4) C33 0.084(5) 0.056(4) 0.085(5) -0.008(4) 0.021(4) -0.016(4) C34 0.096(6) 0.102(6) 0.105(6) -0.033(5) 0.043(5) -0.047(5) C35 0.089(5) 0.088(5) 0.064(4) 0.000(4) -0.002(4) -0.029(5) C36 0.084(5) 0.074(5) 0.063(4) 0.006(4) 0.002(4) -0.029(4) C37 0.053(4) 0.066(4) 0.049(4) 0.011(3) 0.011(3) -0.003(3) C38 0.070(5) 0.084(5) 0.057(4) 0.006(4) 0.004(3) -0.027(4) C39 0.078(5) 0.075(5) 0.091(6) 0.013(4) 0.008(4) -0.031(4) C45 0.090(6) 0.105(6) 0.095(6) -0.012(5) -0.007(5) -0.048(5) C46 0.094(6) 0.091(6) 0.105(6) -0.009(5) -0.004(5) -0.036(5) C40 0.091(7) 0.064(6) 0.076(5) -0.009(4) 0.021(5) -0.026(6) C41 0.088(4) 0.069(4) 0.060(4) -0.001(3) 0.005(3) -0.024(4) C42 0.050(4) 0.046(5) 0.052(3) 0.003(3) 0.008(3) -0.003(4) C43 0.075(4) 0.075(4) 0.059(4) 0.002(3) -0.002(3) -0.028(3) C44 0.074(7) 0.071(5) 0.058(4) 0.000(4) 0.014(4) -0.011(5) N2 0.080(6) 0.068(5) 0.078(5) -0.023(4) 0.007(4) -0.022(5) C47 0.131(8) 0.116(8) 0.130(8) 0.000(6) 0.028(6) -0.044(6) C48 0.213(12) 0.218(12) 0.230(12) -0.023(7) -0.005(7) -0.115(8) O10 0.228(8) 0.212(8) 0.206(8) -0.048(6) -0.007(6) -0.091(6) C40' 0.091(7) 0.064(6) 0.076(5) -0.009(4) 0.021(5) -0.026(6) C41' 0.088(4) 0.069(4) 0.060(4) -0.001(3) 0.005(3) -0.024(4) C42' 0.050(4) 0.046(5) 0.052(3) 0.003(3) 0.008(3) -0.003(4) C43' 0.075(4) 0.075(4) 0.059(4) 0.002(3) -0.002(3) -0.028(3) C44' 0.074(7) 0.071(5) 0.058(4) 0.000(4) 0.014(4) -0.011(5) N2' 0.080(6) 0.068(5) 0.078(5) -0.023(4) 0.007(4) -0.022(5) C47' 0.131(8) 0.116(8) 0.130(8) 0.000(6) 0.028(6) -0.044(6) C48' 0.213(12) 0.218(12) 0.230(12) -0.023(7) -0.005(7) -0.115(8) O10' 0.228(8) 0.212(8) 0.206(8) -0.048(6) -0.007(6) -0.091(6) N1 0.074(4) 0.077(4) 0.079(4) 0.002(3) 0.008(3) -0.025(3) O9 0.114(4) 0.101(4) 0.117(4) -0.011(3) 0.011(4) -0.029(3) P1 0.0807(16) 0.062(2) 0.088(3) -0.0087(19) -0.0109(18) -0.0315(14) F1 0.186(7) 0.133(6) 0.125(5) -0.060(5) 0.017(5) -0.055(5) F2 0.155(7) 0.195(8) 0.222(8) -0.019(7) -0.035(6) -0.128(6) F3 0.119(5) 0.094(5) 0.124(5) -0.002(4) -0.010(4) -0.006(4) F4 0.125(6) 0.145(6) 0.174(6) 0.006(5) -0.020(5) -0.090(5) F5 0.153(7) 0.087(5) 0.190(8) 0.019(5) 0.007(5) -0.022(5) F6 0.137(6) 0.143(6) 0.099(5) -0.018(4) -0.001(4) -0.070(5) P2 0.134(3) 0.116(2) 0.111(2) 0.0025(17) -0.0120(19) -0.065(2) F7 0.185(9) 0.236(10) 0.227(10) -0.060(8) 0.026(8) -0.088(8) F8 0.232(10) 0.126(7) 0.223(10) 0.004(6) -0.012(7) -0.088(6) F9 0.147(8) 0.192(8) 0.140(7) -0.012(6) -0.052(5) -0.079(6) F10 0.240(10) 0.143(7) 0.218(10) 0.011(6) 0.025(8) -0.103(7) F11 0.268(11) 0.252(11) 0.220(10) -0.045(8) -0.064(8) -0.088(8) F12 0.212(9) 0.208(9) 0.162(8) -0.006(6) 0.086(7) -0.083(7) P1' 0.0807(16) 0.062(2) 0.088(3) -0.0087(19) -0.0109(18) -0.0315(14) F1' 0.34(4) 0.34(4) 0.33(4) -0.047(11) 0.007(11) -0.141(19) F2' 0.169(14) 0.134(13) 0.169(13) -0.007(9) 0.008(9) -0.087(10) F3' 0.148(13) 0.147(13) 0.157(13) -0.024(10) -0.012(9) -0.048(9) F4' 0.174(15) 0.153(13) 0.176(14) -0.032(9) 0.014(10) -0.088(10) F5' 0.182(17) 0.180(17) 0.192(17) -0.038(10) -0.032(10) -0.076(11) F6' 0.165(15) 0.170(15) 0.134(14) 0.002(9) 0.050(9) -0.065(10) P2' 0.134(3) 0.116(2) 0.111(2) 0.0025(17) -0.0120(19) -0.065(2) F7' 0.262(19) 0.250(18) 0.237(18) -0.044(10) -0.008(10) -0.101(11) F8' 0.33(3) 0.33(3) 0.34(3) -0.008(11) 0.031(11) -0.155(16) F9' 0.34(3) 0.36(3) 0.36(3) -0.038(11) -0.001(11) -0.142(15) F10' 0.182(14) 0.156(13) 0.175(13) 0.023(9) 0.019(9) -0.087(10) F11' 0.115(11) 0.146(12) 0.150(12) 0.014(8) 0.009(8) -0.039(8) F12' 0.226(16) 0.217(15) 0.174(15) -0.067(10) -0.003(10) -0.074(10) N3 0.146(7) 0.142(6) 0.142(6) -0.054(5) 0.035(5) -0.070(6) C49 0.140(8) 0.138(7) 0.127(7) -0.032(6) 0.015(6) -0.063(6) C50 0.195(9) 0.225(10) 0.184(9) 0.008(7) 0.008(7) -0.109(8) N4 0.186(8) 0.175(8) 0.207(9) -0.011(7) 0.023(7) -0.068(7) C51 0.156(8) 0.174(9) 0.171(9) -0.016(7) 0.022(7) -0.073(7) C52 0.213(10) 0.216(10) 0.221(10) -0.034(8) 0.031(8) -0.091(8) C54 0.296(16) 0.281(15) 0.292(15) -0.038(7) -0.013(7) -0.125(10) C53 0.144(12) 0.147(12) 0.160(12) -0.023(9) -0.018(9) -0.062(9) N5 0.120(9) 0.133(9) 0.099(8) -0.007(7) -0.007(7) -0.048(7) N5' 0.268(19) 0.269(19) 0.270(19) -0.010(10) 0.017(10) -0.111(12) C53' 0.200(16) 0.203(16) 0.197(15) -0.008(10) 0.015(10) -0.087(10) C54' 0.296(16) 0.281(15) 0.292(15) -0.038(7) -0.013(7) -0.125(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C4 1.438(7) . ? O1 C23 1.451(9) . ? O2 C25 1.365(9) . ? O2 C24 1.434(9) . ? O3 C27 1.349(9) . ? O3 C26 1.442(9) . ? O4 C28 1.363(9) . ? O4 C11 1.457(8) 2_666 ? O5 C5 1.419(7) . ? O5 C29 1.485(8) . ? O6 C30 1.464(7) . ? O6 C31 1.478(7) . ? O7 C32 1.468(8) . ? O7 C33 1.495(8) . ? O8 C12 1.416(8) 2_666 ? O8 C34 1.482(9) . ? C1 C21 1.574(8) . ? C1 C2 1.580(8) . ? C1 C14 1.623(8) . ? C1 C15 1.657(7) . ? C2 C3 1.437(8) . ? C2 C7 1.466(8) . ? C3 C4 1.410(8) . ? C3 H3 0.9300 . ? C4 C5 1.460(8) . ? C5 C6 1.454(8) . ? C6 C7 1.424(8) . ? C6 H6 0.9300 . ? C7 C8 1.618(8) . ? C8 C22 1.584(8) . ? C8 C9 1.600(9) . ? C8 C20 1.631(7) . ? C9 C10 1.436(9) . ? C9 C14 1.459(8) . ? C10 C11 1.408(10) . ? C10 H10 0.9300 . ? C11 C12 1.446(10) . ? C11 O4 1.457(8) 2_666 ? C12 O8 1.416(8) 2_666 ? C12 C13 1.476(9) . ? C13 C14 1.446(8) . ? C13 H13 0.9300 . ? C15 C16 1.3900 . ? C15 C20 1.3900 . ? C16 C17 1.3900 . ? C16 H16 0.9300 . ? C17 C18 1.3900 . ? C17 H17 0.9300 . ? C18 C19 1.3900 . ? C18 H18 0.9300 . ? C19 C20 1.3900 . ? C19 H19 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.449(11) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.421(11) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.451(10) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.527(9) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.526(9) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.612(11) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 N1 1.384(9) . ? C35 C36 1.427(10) . ? C35 H35A 0.9300 . ? C36 C37 1.482(9) . ? C36 H36A 0.9300 . ? C37 C38 1.483(9) . ? C37 C42' 1.507(8) . ? C37 C42 1.575(8) . ? C38 C39 1.415(10) . ? C38 H38A 0.9300 . ? C39 N1 1.400(9) . ? C39 H39A 0.9300 . ? C45 N1 1.551(9) . ? C45 C46 1.560(11) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 O9 1.444(9) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C40 C41 1.3900 . ? C40 N2 1.3900 . ? C40 H40A 0.9300 . ? C41 C42 1.3900 . ? C41 H41A 0.9300 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C43 H43A 0.9300 . ? C44 N2 1.3900 . ? C44 H44A 0.9300 . ? N2 C47 1.509(9) . ? C47 C48 1.493(10) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H10' 1.5898 . ? C48 O10 1.420(11) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? O10 H10A 0.8200 . ? C40' C41' 1.3900 . ? C40' N2' 1.3900 . ? C40' H40B 0.9300 . ? C41' C42' 1.3900 . ? C41' H41B 0.9300 . ? C42' C43' 1.3900 . ? C43' C44' 1.3900 . ? C43' H43B 0.9300 . ? C44' N2' 1.3900 . ? C44' H44B 0.9300 . ? N2' C47' 1.508(9) . ? C47' C48' 1.507(10) . ? C47' H47C 0.9700 . ? C47' H47D 0.9700 . ? C48' O10' 1.432(11) . ? C48' H48C 0.9700 . ? C48' H48D 0.9700 . ? O10' H10' 0.8200 . ? O9 H9 0.8200 . ? P1 F3 1.557(6) . ? P1 F2 1.566(6) . ? P1 F5 1.587(6) . ? P1 F1 1.591(7) . ? P1 F6 1.596(7) . ? P1 F4 1.601(6) . ? P2 F12 1.554(8) . ? P2 F8 1.575(8) . ? P2 F10 1.576(8) . ? P2 F9 1.576(7) . ? P2 F11 1.578(8) . ? P2 F7 1.582(8) . ? P1' F2' 1.556(9) . ? P1' F1' 1.557(9) . ? P1' F5' 1.566(9) . ? P1' F6' 1.567(9) . ? P1' F3' 1.569(9) . ? P1' F4' 1.575(9) . ? P2' F9' 1.561(9) . ? P2' F8' 1.561(9) . ? P2' F11' 1.565(9) . ? P2' F10' 1.567(9) . ? P2' F12' 1.568(9) . ? P2' F7' 1.570(9) . ? N3 C49 1.137(13) . ? C49 C50 1.516(17) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? N4 C51 1.174(15) . ? C51 C52 1.545(18) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C54 C53 1.494(9) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C53 N5 1.106(9) . ? N5' C53' 1.123(10) . ? C53' C54' 1.515(10) . ? C54' H54D 0.9600 . ? C54' H54E 0.9600 . ? C54' H54F 0.9600 . ? 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 C4 O1 C23 116.6(5) . . ? C25 O2 C24 121.3(6) . . ? C27 O3 C26 120.3(6) . . ? C28 O4 C11 123.3(5) . 2_666 ? C5 O5 C29 118.6(5) . . ? C30 O6 C31 112.7(5) . . ? C32 O7 C33 113.7(5) . . ? C12 O8 C34 118.3(6) 2_666 . ? C21 C1 C2 113.4(5) . . ? C21 C1 C14 113.9(5) . . ? C2 C1 C14 104.1(4) . . ? C21 C1 C15 115.8(4) . . ? C2 C1 C15 104.1(4) . . ? C14 C1 C15 104.3(4) . . ? C3 C2 C7 119.8(5) . . ? C3 C2 C1 126.6(5) . . ? C7 C2 C1 113.6(5) . . ? C4 C3 C2 121.4(5) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 O1 120.3(5) . . ? C3 C4 C5 118.9(5) . . ? O1 C4 C5 120.8(5) . . ? O5 C5 C6 124.7(5) . . ? O5 C5 C4 114.5(5) . . ? C6 C5 C4 120.8(5) . . ? C7 C6 C5 119.3(5) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C2 119.8(5) . . ? C6 C7 C8 125.6(5) . . ? C2 C7 C8 114.5(5) . . ? C22 C8 C9 114.6(5) . . ? C22 C8 C7 114.1(5) . . ? C9 C8 C7 103.1(4) . . ? C22 C8 C20 113.9(5) . . ? C9 C8 C20 106.4(4) . . ? C7 C8 C20 103.5(4) . . ? C10 C9 C14 119.5(6) . . ? C10 C9 C8 126.5(6) . . ? C14 C9 C8 113.9(5) . . ? C11 C10 C9 121.7(6) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 119.8(6) . . ? C10 C11 O4 120.8(7) . 2_666 ? C12 C11 O4 119.0(7) . 2_666 ? O8 C12 C11 115.2(6) 2_666 . ? O8 C12 C13 124.4(7) 2_666 . ? C11 C12 C13 120.3(6) . . ? C14 C13 C12 118.5(6) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C9 120.1(5) . . ? C13 C14 C1 125.9(5) . . ? C9 C14 C1 114.0(5) . . ? C16 C15 C20 120.0 . . ? C16 C15 C1 124.8(3) . . ? C20 C15 C1 115.2(3) . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C19 C18 C17 120.0 . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.0 . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C15 120.0 . . ? C19 C20 C8 125.6(3) . . ? C15 C20 C8 114.4(4) . . ? C1 C21 H21A 109.5 . . ? C1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C8 C22 H22A 109.5 . . ? C8 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C8 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 O1 116.6(7) . . ? C24 C23 H23A 108.2 . . ? O1 C23 H23A 108.2 . . ? C24 C23 H23B 108.2 . . ? O1 C23 H23B 108.2 . . ? H23A C23 H23B 107.3 . . ? O2 C24 C23 116.2(7) . . ? O2 C24 H24A 108.2 . . ? C23 C24 H24A 108.2 . . ? O2 C24 H24B 108.2 . . ? C23 C24 H24B 108.2 . . ? H24A C24 H24B 107.4 . . ? O2 C25 C26 120.6(8) . . ? O2 C25 H25A 107.2 . . ? C26 C25 H25A 107.2 . . ? O2 C25 H25B 107.2 . . ? C26 C25 H25B 107.2 . . ? H25A C25 H25B 106.8 . . ? C25 C26 O3 118.2(8) . . ? C25 C26 H26A 107.8 . . ? O3 C26 H26A 107.8 . . ? C25 C26 H26B 107.8 . . ? O3 C26 H26B 107.8 . . ? H26A C26 H26B 107.1 . . ? O3 C27 C28 122.8(7) . . ? O3 C27 H27A 106.6 . . ? C28 C27 H27A 106.6 . . ? O3 C27 H27B 106.6 . . ? C28 C27 H27B 106.6 . . ? H27A C27 H27B 106.6 . . ? O4 C28 C27 118.5(7) . . ? O4 C28 H28A 107.7 . . ? C27 C28 H28A 107.7 . . ? O4 C28 H28B 107.7 . . ? C27 C28 H28B 107.7 . . ? H28A C28 H28B 107.1 . . ? O5 C29 C30 107.3(5) . . ? O5 C29 H29A 110.3 . . ? C30 C29 H29A 110.3 . . ? O5 C29 H29B 110.3 . . ? C30 C29 H29B 110.3 . . ? H29A C29 H29B 108.5 . . ? O6 C30 C29 110.6(5) . . ? O6 C30 H30A 109.5 . . ? C29 C30 H30A 109.5 . . ? O6 C30 H30B 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? O6 C31 C32 109.7(5) . . ? O6 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? O6 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? O7 C32 C31 109.2(6) . . ? O7 C32 H32A 109.8 . . ? C31 C32 H32A 109.8 . . ? O7 C32 H32B 109.8 . . ? C31 C32 H32B 109.8 . . ? H32A C32 H32B 108.3 . . ? O7 C33 C34 111.9(5) . . ? O7 C33 H33A 109.2 . . ? C34 C33 H33A 109.2 . . ? O7 C33 H33B 109.2 . . ? C34 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? O8 C34 C33 108.3(6) . . ? O8 C34 H34A 110.0 . . ? C33 C34 H34A 110.0 . . ? O8 C34 H34B 110.0 . . ? C33 C34 H34B 110.0 . . ? H34A C34 H34B 108.4 . . ? N1 C35 C36 120.8(7) . . ? N1 C35 H35A 119.6 . . ? C36 C35 H35A 119.6 . . ? C35 C36 C37 123.1(6) . . ? C35 C36 H36A 118.5 . . ? C37 C36 H36A 118.5 . . ? C36 C37 C38 112.6(6) . . ? C36 C37 C42' 127.0(7) . . ? C38 C37 C42' 120.1(6) . . ? C36 C37 C42 122.7(6) . . ? C38 C37 C42 124.7(6) . . ? C42' C37 C42 7.3(13) . . ? C39 C38 C37 121.9(6) . . ? C39 C38 H38A 119.1 . . ? C37 C38 H38A 119.1 . . ? N1 C39 C38 122.2(7) . . ? N1 C39 H39A 118.9 . . ? C38 C39 H39A 118.9 . . ? N1 C45 C46 109.1(6) . . ? N1 C45 H45A 109.9 . . ? C46 C45 H45A 109.9 . . ? N1 C45 H45B 109.9 . . ? C46 C45 H45B 109.9 . . ? H45A C45 H45B 108.3 . . ? O9 C46 C45 107.5(7) . . ? O9 C46 H46A 110.2 . . ? C45 C46 H46A 110.2 . . ? O9 C46 H46B 110.2 . . ? C45 C46 H46B 110.2 . . ? H46A C46 H46B 108.5 . . ? C41 C40 N2 120.0 . . ? C41 C40 H40A 120.0 . . ? N2 C40 H40A 120.0 . . ? C42 C41 C40 120.0 . . ? C42 C41 H41A 120.0 . . ? C40 C41 H41A 120.0 . . ? C43 C42 C41 120.0 . . ? C43 C42 C37 118.4(6) . . ? C41 C42 C37 119.0(7) . . ? C42 C43 C44 120.0 . . ? C42 C43 H43A 120.0 . . ? C44 C43 H43A 120.0 . . ? C43 C44 N2 120.0 . . ? C43 C44 H44A 120.0 . . ? N2 C44 H44A 120.0 . . ? C44 N2 C40 120.0 . . ? C44 N2 C47 118.8(7) . . ? C40 N2 C47 121.2(7) . . ? C48 C47 N2 113.8(9) . . ? C48 C47 H47A 108.8 . . ? N2 C47 H47A 108.8 . . ? C48 C47 H47B 108.8 . . ? N2 C47 H47B 108.8 . . ? H47A C47 H47B 107.7 . . ? C48 C47 H10' 130.3 . . ? N2 C47 H10' 86.1 . . ? H47A C47 H10' 25.3 . . ? H47B C47 H10' 106.3 . . ? O10 C48 C47 112.5(10) . . ? O10 C48 H48A 109.1 . . ? C47 C48 H48A 109.1 . . ? O10 C48 H48B 109.1 . . ? C47 C48 H48B 109.1 . . ? H48A C48 H48B 107.8 . . ? C48 O10 H10A 109.6 . . ? C41' C40' N2' 120.0 . . ? C41' C40' H40B 120.0 . . ? N2' C40' H40B 120.0 . . ? C40' C41' C42' 120.0 . . ? C40' C41' H41B 120.0 . . ? C42' C41' H41B 120.0 . . ? C43' C42' C41' 120.0 . . ? C43' C42' C37 119.3(7) . . ? C41' C42' C37 120.2(7) . . ? C44' C43' C42' 120.0 . . ? C44' C43' H43B 120.0 . . ? C42' C43' H43B 120.0 . . ? C43' C44' N2' 120.0 . . ? C43' C44' H44B 120.0 . . ? N2' C44' H44B 120.0 . . ? C44' N2' C40' 120.0 . . ? C44' N2' C47' 117.5(7) . . ? C40' N2' C47' 122.5(7) . . ? C48' C47' N2' 109.8(9) . . ? C48' C47' H47C 109.7 . . ? N2' C47' H47C 109.7 . . ? C48' C47' H47D 109.7 . . ? N2' C47' H47D 109.7 . . ? H47C C47' H47D 108.2 . . ? O10' C48' C47' 109.4(10) . . ? O10' C48' H48C 109.8 . . ? C47' C48' H48C 109.8 . . ? O10' C48' H48D 109.8 . . ? C47' C48' H48D 109.8 . . ? H48C C48' H48D 108.2 . . ? C48' O10' H10' 109.5 . . ? C35 N1 C39 119.5(7) . . ? C35 N1 C45 119.4(6) . . ? C39 N1 C45 121.1(7) . . ? C46 O9 H9 109.5 . . ? F3 P1 F2 92.3(4) . . ? F3 P1 F5 176.4(5) . . ? F2 P1 F5 90.2(5) . . ? F3 P1 F1 89.4(4) . . ? F2 P1 F1 89.3(4) . . ? F5 P1 F1 88.1(4) . . ? F3 P1 F6 91.9(4) . . ? F2 P1 F6 93.1(4) . . ? F5 P1 F6 90.5(4) . . ? F1 P1 F6 177.3(4) . . ? F3 P1 F4 90.0(4) . . ? F2 P1 F4 177.4(5) . . ? F5 P1 F4 87.4(4) . . ? F1 P1 F4 89.6(4) . . ? F6 P1 F4 88.0(4) . . ? F12 P2 F8 91.4(5) . . ? F12 P2 F10 90.8(5) . . ? F8 P2 F10 177.7(7) . . ? F12 P2 F9 90.6(5) . . ? F8 P2 F9 89.9(5) . . ? F10 P2 F9 90.0(5) . . ? F12 P2 F11 90.6(6) . . ? F8 P2 F11 90.0(5) . . ? F10 P2 F11 90.1(5) . . ? F9 P2 F11 178.8(7) . . ? F12 P2 F7 178.9(6) . . ? F8 P2 F7 89.5(5) . . ? F10 P2 F7 88.2(5) . . ? F9 P2 F7 90.0(5) . . ? F11 P2 F7 88.8(5) . . ? F2' P1' F1' 90.4(6) . . ? F2' P1' F5' 90.2(6) . . ? F1' P1' F5' 90.6(6) . . ? F2' P1' F6' 90.8(6) . . ? F1' P1' F6' 178.8(8) . . ? F5' P1' F6' 89.4(6) . . ? F2' P1' F3' 90.0(6) . . ? F1' P1' F3' 90.4(6) . . ? F5' P1' F3' 179.0(8) . . ? F6' P1' F3' 89.5(6) . . ? F2' P1' F4' 179.4(8) . . ? F1' P1' F4' 90.1(6) . . ? F5' P1' F4' 90.0(6) . . ? F6' P1' F4' 88.7(6) . . ? F3' P1' F4' 89.8(6) . . ? F9' P2' F8' 90.4(6) . . ? F9' P2' F11' 179.4(8) . . ? F8' P2' F11' 90.2(6) . . ? F9' P2' F10' 90.1(6) . . ? F8' P2' F10' 179.5(8) . . ? F11' P2' F10' 89.3(6) . . ? F9' P2' F12' 90.2(6) . . ? F8' P2' F12' 89.7(6) . . ? F11' P2' F12' 90.1(6) . . ? F10' P2' F12' 90.2(6) . . ? F9' P2' F7' 89.9(6) . . ? F8' P2' F7' 90.1(6) . . ? F11' P2' F7' 89.8(6) . . ? F10' P2' F7' 89.9(6) . . ? F12' P2' F7' 179.9(8) . . ? N3 C49 C50 177.4(14) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N4 C51 C52 177.8(16) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N5 C53 C54 171(4) . . ? N5' C53' C54' 155(3) . . ? C53' C54' H54D 109.5 . . ? C53' C54' H54E 109.5 . . ? H54D C54' H54E 109.5 . . ? C53' C54' H54F 109.5 . . ? H54D C54' H54F 109.5 . . ? H54E C54' H54F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 C1 C2 C3 -0.2(8) . . . . ? C14 C1 C2 C3 124.1(6) . . . . ? C15 C1 C2 C3 -126.9(5) . . . . ? C21 C1 C2 C7 -179.5(5) . . . . ? C14 C1 C2 C7 -55.3(6) . . . . ? C15 C1 C2 C7 53.7(5) . . . . ? C7 C2 C3 C4 0.9(8) . . . . ? C1 C2 C3 C4 -178.4(5) . . . . ? C2 C3 C4 O1 178.4(5) . . . . ? C2 C3 C4 C5 -0.3(8) . . . . ? C23 O1 C4 C3 100.8(7) . . . . ? C23 O1 C4 C5 -80.5(8) . . . . ? C29 O5 C5 C6 -21.8(9) . . . . ? C29 O5 C5 C4 158.7(5) . . . . ? C3 C4 C5 O5 179.6(5) . . . . ? O1 C4 C5 O5 0.9(8) . . . . ? C3 C4 C5 C6 0.1(8) . . . . ? O1 C4 C5 C6 -178.6(5) . . . . ? O5 C5 C6 C7 -179.8(5) . . . . ? C4 C5 C6 C7 -0.4(8) . . . . ? C5 C6 C7 C2 1.0(8) . . . . ? C5 C6 C7 C8 178.8(5) . . . . ? C3 C2 C7 C6 -1.2(8) . . . . ? C1 C2 C7 C6 178.2(5) . . . . ? C3 C2 C7 C8 -179.3(5) . . . . ? C1 C2 C7 C8 0.1(6) . . . . ? C6 C7 C8 C22 2.9(8) . . . . ? C2 C7 C8 C22 -179.3(5) . . . . ? C6 C7 C8 C9 -122.1(6) . . . . ? C2 C7 C8 C9 55.8(6) . . . . ? C6 C7 C8 C20 127.2(6) . . . . ? C2 C7 C8 C20 -55.0(6) . . . . ? C22 C8 C9 C10 -3.2(8) . . . . ? C7 C8 C9 C10 121.4(6) . . . . ? C20 C8 C9 C10 -130.0(6) . . . . ? C22 C8 C9 C14 179.7(5) . . . . ? C7 C8 C9 C14 -55.6(6) . . . . ? C20 C8 C9 C14 53.0(6) . . . . ? C14 C9 C10 C11 1.7(9) . . . . ? C8 C9 C10 C11 -175.2(5) . . . . ? C9 C10 C11 C12 -3.6(9) . . . . ? C9 C10 C11 O4 168.8(5) . . . 2_666 ? C10 C11 C12 O8 -179.5(5) . . . 2_666 ? O4 C11 C12 O8 7.9(8) 2_666 . . 2_666 ? C10 C11 C12 C13 2.1(9) . . . . ? O4 C11 C12 C13 -170.5(5) 2_666 . . . ? O8 C12 C13 C14 -177.0(5) 2_666 . . . ? C11 C12 C13 C14 1.3(9) . . . . ? C12 C13 C14 C9 -3.1(8) . . . . ? C12 C13 C14 C1 174.4(5) . . . . ? C10 C9 C14 C13 1.7(8) . . . . ? C8 C9 C14 C13 179.0(5) . . . . ? C10 C9 C14 C1 -176.1(5) . . . . ? C8 C9 C14 C1 1.2(6) . . . . ? C21 C1 C14 C13 1.6(8) . . . . ? C2 C1 C14 C13 -122.3(6) . . . . ? C15 C1 C14 C13 128.8(5) . . . . ? C21 C1 C14 C9 179.3(5) . . . . ? C2 C1 C14 C9 55.3(6) . . . . ? C15 C1 C14 C9 -53.6(5) . . . . ? C21 C1 C15 C16 -1.2(6) . . . . ? C2 C1 C15 C16 124.0(4) . . . . ? C14 C1 C15 C16 -127.1(4) . . . . ? C21 C1 C15 C20 179.9(4) . . . . ? C2 C1 C15 C20 -54.9(4) . . . . ? C14 C1 C15 C20 54.0(4) . . . . ? C20 C15 C16 C17 0.0 . . . . ? C1 C15 C16 C17 -178.9(4) . . . . ? C15 C16 C17 C18 0.0 . . . . ? C16 C17 C18 C19 0.0 . . . . ? C17 C18 C19 C20 0.0 . . . . ? C18 C19 C20 C15 0.0 . . . . ? C18 C19 C20 C8 179.7(4) . . . . ? C16 C15 C20 C19 0.0 . . . . ? C1 C15 C20 C19 179.0(4) . . . . ? C16 C15 C20 C8 -179.7(4) . . . . ? C1 C15 C20 C8 -0.7(4) . . . . ? C22 C8 C20 C19 -0.5(6) . . . . ? C9 C8 C20 C19 126.7(4) . . . . ? C7 C8 C20 C19 -124.9(4) . . . . ? C22 C8 C20 C15 179.2(4) . . . . ? C9 C8 C20 C15 -53.6(4) . . . . ? C7 C8 C20 C15 54.7(5) . . . . ? C4 O1 C23 C24 -177.0(7) . . . . ? C25 O2 C24 C23 -162.7(10) . . . . ? O1 C23 C24 O2 -55.8(13) . . . . ? C24 O2 C25 C26 171.6(10) . . . . ? O2 C25 C26 O3 49.1(16) . . . . ? C27 O3 C26 C25 176.1(10) . . . . ? C26 O3 C27 C28 167.0(9) . . . . ? C11 O4 C28 C27 -162.1(9) 2_666 . . . ? O3 C27 C28 O4 -25.7(15) . . . . ? C5 O5 C29 C30 -158.0(5) . . . . ? C31 O6 C30 C29 168.4(5) . . . . ? O5 C29 C30 O6 -64.8(7) . . . . ? C30 O6 C31 C32 179.6(5) . . . . ? C33 O7 C32 C31 -170.6(5) . . . . ? O6 C31 C32 O7 -72.3(7) . . . . ? C32 O7 C33 C34 -94.4(7) . . . . ? C12 O8 C34 C33 173.7(6) 2_666 . . . ? O7 C33 C34 O8 67.8(8) . . . . ? N1 C35 C36 C37 0.8(10) . . . . ? C35 C36 C37 C38 -0.4(9) . . . . ? C35 C36 C37 C42' -173.3(10) . . . . ? C35 C36 C37 C42 179.4(10) . . . . ? C36 C37 C38 C39 0.3(9) . . . . ? C42' C37 C38 C39 173.7(10) . . . . ? C42 C37 C38 C39 -179.5(9) . . . . ? C37 C38 C39 N1 -0.6(10) . . . . ? N1 C45 C46 O9 -59.6(8) . . . . ? N2 C40 C41 C42 0.0 . . . . ? C40 C41 C42 C43 0.0 . . . . ? C40 C41 C42 C37 161.7(12) . . . . ? C36 C37 C42 C43 -174.8(7) . . . . ? C38 C37 C42 C43 5.0(12) . . . . ? C42' C37 C42 C43 58(7) . . . . ? C36 C37 C42 C41 23.2(13) . . . . ? C38 C37 C42 C41 -157.0(7) . . . . ? C42' C37 C42 C41 -104(7) . . . . ? C41 C42 C43 C44 0.0 . . . . ? C37 C42 C43 C44 -161.9(12) . . . . ? C42 C43 C44 N2 0.0 . . . . ? C43 C44 N2 C40 0.0 . . . . ? C43 C44 N2 C47 179.95(9) . . . . ? C41 C40 N2 C44 0.0 . . . . ? C41 C40 N2 C47 -179.95(9) . . . . ? C44 N2 C47 C48 101.0(13) . . . . ? C40 N2 C47 C48 -79.0(13) . . . . ? N2 C47 C48 O10 -66(2) . . . . ? N2' C40' C41' C42' 0.0 . . . . ? C40' C41' C42' C43' 0.0 . . . . ? C40' C41' C42' C37 -172.1(12) . . . . ? C36 C37 C42' C43' -168.7(7) . . . . ? C38 C37 C42' C43' 18.9(12) . . . . ? C42 C37 C42' C43' -112(7) . . . . ? C36 C37 C42' C41' 3.5(15) . . . . ? C38 C37 C42' C41' -168.9(7) . . . . ? C42 C37 C42' C41' 60(7) . . . . ? C41' C42' C43' C44' 0.0 . . . . ? C37 C42' C43' C44' 172.2(12) . . . . ? C42' C43' C44' N2' 0.0 . . . . ? C43' C44' N2' C40' 0.0 . . . . ? C43' C44' N2' C47' -179.93(9) . . . . ? C41' C40' N2' C44' 0.0 . . . . ? C41' C40' N2' C47' 179.92(9) . . . . ? C44' N2' C47' C48' -87.6(12) . . . . ? C40' N2' C47' C48' 92.5(12) . . . . ? N2' C47' C48' O10' -66.5(19) . . . . ? C36 C35 N1 C39 -1.1(10) . . . . ? C36 C35 N1 C45 177.1(6) . . . . ? C38 C39 N1 C35 1.0(10) . . . . ? C38 C39 N1 C45 -177.1(6) . . . . ? C46 C45 N1 C35 -89.0(8) . . . . ? C46 C45 N1 C39 89.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.584 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.066