# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_HPO4 _database_code_depnum_ccdc_archive 'CCDC 895441' #TrackingRef 'cyclohexyl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C140 H234 N24 O28 P2' _chemical_formula_weight 2763.45 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' 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 16.201(8) _cell_length_b 14.693(7) _cell_length_c 31.511(15) _cell_angle_alpha 90.00 _cell_angle_beta 100.528(7) _cell_angle_gamma 90.00 _cell_volume 7375(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9958 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.12 _exptl_crystal_description flake _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 0.107 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9634 _exptl_absorpt_correction_T_max 0.9894 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48435 _diffrn_reflns_av_R_equivalents 0.0817 _diffrn_reflns_av_sigmaI/netI 0.1110 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 25.27 _reflns_number_total 22279 _reflns_number_gt 14568 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0745P)^2^+4.0577P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(14) _refine_ls_number_reflns 22279 _refine_ls_number_parameters 1769 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1207 _refine_ls_R_factor_gt 0.0711 _refine_ls_wR_factor_ref 0.1972 _refine_ls_wR_factor_gt 0.1651 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.63763(8) 0.07295(11) 0.75194(4) 0.0329(3) Uani 1 1 d . . . P2 P 0.85427(10) 0.22021(13) 0.74287(5) 0.0468(4) Uani 1 1 d . . . O1 O 0.9829(3) 0.1577(4) 1.02688(13) 0.0731(15) Uani 1 1 d . . . O2 O 0.9029(3) 0.2701(4) 1.00102(14) 0.0711(15) Uani 1 1 d . . . O3 O 1.0855(2) 0.0016(3) 0.84094(11) 0.0448(10) Uani 1 1 d . . . O4 O 0.9739(2) 0.0463(3) 0.61718(12) 0.0499(11) Uani 1 1 d . . . O5 O 1.0034(2) 0.3449(3) 0.61531(13) 0.0541(12) Uani 1 1 d . . . O6 O 0.9646(3) 0.5395(3) 0.80926(13) 0.0523(11) Uani 1 1 d . . . O7 O 0.6981(4) 0.4458(4) 0.96742(15) 0.0875(19) Uani 1 1 d . . . O8 O 0.8052(3) 0.5279(4) 0.99245(15) 0.0853(18) Uani 1 1 d . . . O9 O 0.5937(3) -0.0042(5) 0.49935(14) 0.0831(18) Uani 1 1 d . . . O10 O 0.5328(4) 0.1171(5) 0.47204(14) 0.097(2) Uani 1 1 d . . . O11 O 0.4137(3) 0.2899(3) 0.65118(12) 0.0477(11) Uani 1 1 d . . . O12 O 0.5032(2) 0.2652(3) 0.87660(10) 0.0376(9) Uani 1 1 d . . . O13 O 0.5346(2) -0.0318(3) 0.88925(10) 0.0379(9) Uani 1 1 d . . . O14 O 0.5304(3) -0.2584(3) 0.70013(12) 0.0517(11) Uani 1 1 d . . . O15 O 0.6835(3) -0.2425(4) 0.51331(14) 0.0801(17) Uani 1 1 d . . . O16 O 0.7908(3) -0.1592(4) 0.53605(15) 0.0798(18) Uani 1 1 d . . . O17 O 0.6724(2) -0.0126(3) 0.77460(10) 0.0337(9) Uani 1 1 d . . . O18 O 0.6595(2) 0.1584(3) 0.77803(10) 0.0393(9) Uani 1 1 d . . . O19 O 0.5453(2) 0.0630(3) 0.73513(10) 0.0345(9) Uani 1 1 d . . . O20 O 0.6777(2) 0.0819(3) 0.70982(10) 0.0374(9) Uani 1 1 d . . . H201 H 0.7289 0.0912 0.7077 0.021(13) Uiso 1 1 d R . . O21 O 0.8386(2) 0.1241(3) 0.72811(11) 0.0389(9) Uani 1 1 d . . . O22 O 0.9445(2) 0.2342(3) 0.76206(11) 0.0360(9) Uani 1 1 d . . . O23 O 0.8050(3) 0.2369(3) 0.78289(12) 0.0573(12) Uani 1 1 d . . . H231 H 0.7391 0.2566 0.7719 0.040(14) Uiso 1 1 d R . . O24 O 0.8247(2) 0.2871(3) 0.70914(11) 0.0385(9) Uani 1 1 d . . . O25 O 0.6748(3) 0.2494(4) 0.65823(16) 0.0783(15) Uani 1 1 d . . . H251 H 0.6626 0.1855 0.6731 0.07(2) Uiso 1 1 d R . . H252 H 0.7094 0.2519 0.6917 0.22(6) Uiso 1 1 d R . . O26 O 0.8425(3) -0.0014(4) 0.7995(2) 0.096(2) Uani 1 1 d . . . H261 H 0.7991 -0.0041 0.7999 0.14(5) Uiso 1 1 d R . . H262 H 0.8508 0.0288 0.7843 0.08(3) Uiso 1 1 d R . . O27 O 0.418(2) 0.463(2) 0.9445(9) 0.48(3) Uani 1 1 d . . . O28 O 0.0269(10) 0.8578(11) 0.5514(5) 0.232(6) Uani 1 1 d . . . N1 N 0.9510(4) 0.2070(5) 0.99644(17) 0.0585(16) Uani 1 1 d . . . N2 N 1.0092(3) 0.1339(3) 0.83179(13) 0.0352(11) Uani 1 1 d . . . H2 H 0.9902 0.1758 0.8125 0.042 Uiso 1 1 calc R . . N3 N 1.0381(3) 0.0572(3) 0.77360(12) 0.0361(11) Uani 1 1 d . . . H3 H 1.0079 0.1014 0.7596 0.043 Uiso 1 1 calc R . . N4 N 0.9634(3) 0.0364(4) 0.68850(14) 0.0418(13) Uani 1 1 d . . . H4 H 0.9343 0.0565 0.7076 0.050 Uiso 1 1 calc R . . N5 N 0.8549(3) 0.0917(4) 0.63890(13) 0.0400(12) Uani 1 1 d . . . H5A H 0.8239 0.0824 0.6587 0.048 Uiso 1 1 calc R . . N6 N 0.8875(3) 0.2805(4) 0.63120(13) 0.0446(13) Uani 1 1 d . . . H6A H 0.8525 0.2779 0.6495 0.054 Uiso 1 1 calc R . . N7 N 0.9592(3) 0.3811(3) 0.67842(13) 0.0372(12) Uani 1 1 d . . . H7 H 0.9209 0.3681 0.6940 0.045 Uiso 1 1 calc R . . N8 N 0.9796(3) 0.4200(4) 0.76507(14) 0.0442(12) Uani 1 1 d . . . H8 H 0.9677 0.3622 0.7599 0.053 Uiso 1 1 calc R . . N9 N 0.8910(3) 0.4115(4) 0.81405(14) 0.0513(14) Uani 1 1 d . . . H9A H 0.8735 0.3606 0.8006 0.062 Uiso 1 1 calc R . . N10 N 0.7654(4) 0.4813(4) 0.96443(17) 0.0608(16) Uani 1 1 d . . . N11 N 0.5546(4) 0.0653(7) 0.50239(18) 0.079(2) Uani 1 1 d . . . N12 N 0.4837(3) 0.1563(3) 0.66299(13) 0.0388(12) Uani 1 1 d . . . H12A H 0.5005 0.1153 0.6831 0.047 Uiso 1 1 calc R . . N13 N 0.4567(3) 0.2355(3) 0.71978(13) 0.0342(11) Uani 1 1 d . . . H13 H 0.4862 0.1920 0.7347 0.041 Uiso 1 1 calc R . . N14 N 0.5231(3) 0.2619(3) 0.80643(13) 0.0356(11) Uani 1 1 d . . . H14 H 0.5549 0.2393 0.7892 0.043 Uiso 1 1 calc R . . N15 N 0.6153(3) 0.1928(3) 0.85967(12) 0.0331(11) Uani 1 1 d . . . H15A H 0.6493 0.1881 0.8409 0.040 Uiso 1 1 calc R . . N16 N 0.6528(2) 0.0031(3) 0.86343(12) 0.0321(10) Uani 1 1 d . . . H16 H 0.6821 -0.0098 0.8433 0.039 Uiso 1 1 calc R . . N17 N 0.5533(3) -0.0819(3) 0.82276(13) 0.0348(11) Uani 1 1 d . . . H17 H 0.5845 -0.0725 0.8031 0.042 Uiso 1 1 calc R . . N18 N 0.5149(3) -0.1309(3) 0.73884(12) 0.0369(11) Uani 1 1 d . . . H18 H 0.5221 -0.0715 0.7394 0.044 Uiso 1 1 calc R . . N19 N 0.6097(3) -0.1312(4) 0.69444(15) 0.0502(14) Uani 1 1 d . . . H19 H 0.6318 -0.0834 0.7091 0.060 Uiso 1 1 calc R . . N20 N 0.7267(4) -0.1949(5) 0.54063(16) 0.0603(17) Uani 1 1 d . . . N21 N 0.9461(3) 0.7846(4) 0.84943(13) 0.0407(12) Uani 1 1 d . . . N22 N 0.1938(3) 0.1551(4) 0.59297(14) 0.0450(13) Uani 1 1 d . . . N23 N 0.3119(3) 0.1278(3) 0.89498(14) 0.0391(11) Uani 1 1 d . . . N24 N 0.5695(3) 0.4946(4) 0.6484(2) 0.0656(17) Uani 1 1 d . . . C1 C 0.9691(4) 0.1893(5) 0.95438(17) 0.0468(17) Uani 1 1 d . . . C2 C 1.0284(4) 0.1265(5) 0.95006(17) 0.0447(15) Uani 1 1 d . . . H2A H 1.0592 0.0971 0.9748 0.054 Uiso 1 1 calc R . . C3 C 1.0436(4) 0.1055(4) 0.90966(17) 0.0418(15) Uani 1 1 d . . . H3A H 1.0849 0.0614 0.9065 0.050 Uiso 1 1 calc R . . C4 C 0.9985(3) 0.1488(4) 0.87330(16) 0.0374(14) Uani 1 1 d . . . C5 C 0.9391(4) 0.2138(5) 0.87813(17) 0.0466(16) Uani 1 1 d . . . H5 H 0.9082 0.2439 0.8536 0.056 Uiso 1 1 calc R . . C6 C 0.9250(4) 0.2349(5) 0.91975(19) 0.0517(17) Uani 1 1 d . . . H6 H 0.8853 0.2802 0.9237 0.062 Uiso 1 1 calc R . . C7 C 1.0477(3) 0.0580(4) 0.81742(17) 0.0391(14) Uani 1 1 d . . . C8 C 1.0716(3) -0.0072(4) 0.74863(18) 0.0371(14) Uani 1 1 d . . . C9 C 1.1392(3) -0.0612(4) 0.7657(2) 0.0465(16) Uani 1 1 d . . . H9 H 1.1631 -0.0573 0.7955 0.056 Uiso 1 1 calc R . . C10 C 1.1714(4) -0.1199(5) 0.7397(2) 0.0585(19) Uani 1 1 d . . . H10 H 1.2170 -0.1583 0.7516 0.070 Uiso 1 1 calc R . . C11 C 1.1387(4) -0.1244(5) 0.6963(2) 0.0558(18) Uani 1 1 d . . . H11 H 1.1632 -0.1640 0.6782 0.067 Uiso 1 1 calc R . . C12 C 1.0719(4) -0.0729(4) 0.67920(19) 0.0446(15) Uani 1 1 d . . . H12 H 1.0495 -0.0773 0.6492 0.054 Uiso 1 1 calc R . . C13 C 1.0358(3) -0.0144(4) 0.70430(18) 0.0410(15) Uani 1 1 d . . . C14 C 0.9333(4) 0.0579(4) 0.64549(16) 0.0399(15) Uani 1 1 d . . . C15 C 0.8194(3) 0.1430(5) 0.60065(16) 0.0449(15) Uani 1 1 d . . . H15 H 0.7649 0.1683 0.6061 0.054 Uiso 1 1 calc R . . C16 C 0.7980(4) 0.0843(5) 0.56014(17) 0.0558(18) Uani 1 1 d . . . H16A H 0.8501 0.0571 0.5535 0.067 Uiso 1 1 calc R . . H16B H 0.7603 0.0342 0.5654 0.067 Uiso 1 1 calc R . . C17 C 0.7560(5) 0.1400(6) 0.52235(19) 0.073(2) Uani 1 1 d . . . H17A H 0.7017 0.1631 0.5281 0.088 Uiso 1 1 calc R . . H17B H 0.7445 0.1010 0.4963 0.088 Uiso 1 1 calc R . . C18 C 0.8100(5) 0.2190(6) 0.51419(19) 0.073(2) Uani 1 1 d . . . H18A H 0.7802 0.2554 0.4897 0.088 Uiso 1 1 calc R . . H18B H 0.8627 0.1960 0.5064 0.088 Uiso 1 1 calc R . . C19 C 0.8304(5) 0.2783(6) 0.55363(19) 0.068(2) Uani 1 1 d . . . H19A H 0.7781 0.3061 0.5597 0.081 Uiso 1 1 calc R . . H19B H 0.8683 0.3280 0.5481 0.081 Uiso 1 1 calc R . . C20 C 0.8724(4) 0.2240(5) 0.59282(16) 0.0470(15) Uani 1 1 d . . . H20 H 0.9276 0.2012 0.5873 0.056 Uiso 1 1 calc R . . C21 C 0.9527(3) 0.3356(4) 0.63933(17) 0.0406(14) Uani 1 1 d . . . C22 C 1.0180(3) 0.4433(4) 0.69527(18) 0.0393(14) Uani 1 1 d . . . C23 C 1.0672(4) 0.4896(5) 0.6704(2) 0.0492(16) Uani 1 1 d . . . H23 H 1.0607 0.4770 0.6404 0.059 Uiso 1 1 calc R . . C24 C 1.1248(4) 0.5529(5) 0.6887(2) 0.0573(18) Uani 1 1 d . . . H24 H 1.1581 0.5833 0.6712 0.069 Uiso 1 1 calc R . . C25 C 1.1355(4) 0.5735(5) 0.7319(2) 0.0579(18) Uani 1 1 d . . . H25 H 1.1748 0.6186 0.7441 0.070 Uiso 1 1 calc R . . C26 C 1.0885(4) 0.5277(5) 0.7574(2) 0.0480(16) Uani 1 1 d . . . H26 H 1.0966 0.5400 0.7874 0.058 Uiso 1 1 calc R . . C27 C 1.0307(3) 0.4653(4) 0.73967(17) 0.0380(14) Uani 1 1 d . . . C28 C 0.9480(4) 0.4622(5) 0.79716(18) 0.0463(16) Uani 1 1 d . . . C29 C 0.8584(4) 0.4334(4) 0.85067(18) 0.0465(16) Uani 1 1 d . . . C30 C 0.9038(4) 0.4855(5) 0.88433(18) 0.0478(16) Uani 1 1 d . . . H30 H 0.9565 0.5109 0.8816 0.057 Uiso 1 1 calc R . . C31 C 0.8722(4) 0.4993(5) 0.92074(18) 0.0508(16) Uani 1 1 d . . . H31 H 0.9041 0.5323 0.9441 0.061 Uiso 1 1 calc R . . C32 C 0.7956(4) 0.4665(4) 0.92422(18) 0.0447(15) Uani 1 1 d . . . C33 C 0.7507(4) 0.4162(5) 0.89209(18) 0.0534(18) Uani 1 1 d . . . H33 H 0.6970 0.3934 0.8948 0.064 Uiso 1 1 calc R . . C34 C 0.7831(4) 0.3979(5) 0.85527(19) 0.0542(18) Uani 1 1 d . . . H34 H 0.7526 0.3606 0.8332 0.065 Uiso 1 1 calc R . . C35 C 0.5352(4) 0.0894(5) 0.54394(17) 0.0541(19) Uani 1 1 d . . . C36 C 0.5656(4) 0.0379(6) 0.57912(18) 0.0578(19) Uani 1 1 d . . . H36 H 0.5992 -0.0141 0.5768 0.069 Uiso 1 1 calc R . . C37 C 0.5467(3) 0.0626(5) 0.61768(17) 0.0432(15) Uani 1 1 d . . . H37 H 0.5689 0.0278 0.6426 0.052 Uiso 1 1 calc R . . C38 C 0.4970(3) 0.1358(4) 0.62198(15) 0.0348(13) Uani 1 1 d . . . C39 C 0.4628(4) 0.1853(5) 0.58456(16) 0.0456(16) Uani 1 1 d . . . H39 H 0.4266 0.2355 0.5863 0.055 Uiso 1 1 calc R . . C40 C 0.4822(4) 0.1604(6) 0.54555(16) 0.0549(19) Uani 1 1 d . . . H40 H 0.4589 0.1924 0.5200 0.066 Uiso 1 1 calc R . . C41 C 0.4480(3) 0.2321(4) 0.67565(17) 0.0382(14) Uani 1 1 d . . . C42 C 0.4218(3) 0.3039(4) 0.74346(17) 0.0375(14) Uani 1 1 d . . . C43 C 0.3552(4) 0.3571(5) 0.7239(2) 0.0486(16) Uani 1 1 d . . . H43 H 0.3338 0.3501 0.6939 0.058 Uiso 1 1 calc R . . C44 C 0.3191(4) 0.4207(5) 0.7475(2) 0.0533(17) Uani 1 1 d . . . H44 H 0.2736 0.4573 0.7340 0.064 Uiso 1 1 calc R . . C45 C 0.3506(4) 0.4298(4) 0.7912(2) 0.0491(17) Uani 1 1 d . . . H45 H 0.3250 0.4711 0.8080 0.059 Uiso 1 1 calc R . . C46 C 0.4184(4) 0.3797(4) 0.8102(2) 0.0475(16) Uani 1 1 d . . . H46 H 0.4411 0.3896 0.8398 0.057 Uiso 1 1 calc R . . C47 C 0.4553(3) 0.3146(4) 0.78735(17) 0.0358(13) Uani 1 1 d . . . C48 C 0.5458(3) 0.2411(4) 0.84989(17) 0.0360(14) Uani 1 1 d . . . C49 C 0.6363(3) 0.1474(4) 0.90127(14) 0.0339(13) Uani 1 1 d . . . H49 H 0.5829 0.1276 0.9102 0.041 Uiso 1 1 calc R . . C50 C 0.6831(4) 0.2125(4) 0.93622(16) 0.0425(14) Uani 1 1 d . . . H50A H 0.7353 0.2344 0.9275 0.051 Uiso 1 1 calc R . . H50B H 0.6474 0.2659 0.9391 0.051 Uiso 1 1 calc R . . C51 C 0.7050(4) 0.1628(5) 0.98002(17) 0.0524(17) Uani 1 1 d . . . H51A H 0.7372 0.2041 1.0018 0.063 Uiso 1 1 calc R . . H51B H 0.6526 0.1456 0.9900 0.063 Uiso 1 1 calc R . . C52 C 0.7555(4) 0.0796(5) 0.97603(16) 0.0488(15) Uani 1 1 d . . . H52A H 0.7666 0.0473 1.0041 0.059 Uiso 1 1 calc R . . H52B H 0.8102 0.0974 0.9688 0.059 Uiso 1 1 calc R . . C53 C 0.7104(4) 0.0159(4) 0.94141(16) 0.0453(15) Uani 1 1 d . . . H53A H 0.6584 -0.0069 0.9500 0.054 Uiso 1 1 calc R . . H53B H 0.7468 -0.0370 0.9385 0.054 Uiso 1 1 calc R . . C54 C 0.6884(3) 0.0653(4) 0.89797(14) 0.0337(12) Uani 1 1 d . . . H54 H 0.7426 0.0876 0.8909 0.040 Uiso 1 1 calc R . . C55 C 0.5766(3) -0.0351(4) 0.86118(15) 0.0326(13) Uani 1 1 d . . . C56 C 0.4870(3) -0.1416(4) 0.81154(17) 0.0367(14) Uani 1 1 d . . . C57 C 0.4404(4) -0.1770(4) 0.83996(17) 0.0419(15) Uani 1 1 d . . . H57 H 0.4502 -0.1565 0.8690 0.050 Uiso 1 1 calc R . . C58 C 0.3799(4) -0.2414(4) 0.82684(19) 0.0471(16) Uani 1 1 d . . . H58 H 0.3494 -0.2662 0.8472 0.056 Uiso 1 1 calc R . . C59 C 0.3627(4) -0.2706(5) 0.78501(19) 0.0473(16) Uani 1 1 d . . . H59 H 0.3214 -0.3160 0.7762 0.057 Uiso 1 1 calc R . . C60 C 0.4067(4) -0.2325(4) 0.75597(19) 0.0463(15) Uani 1 1 d . . . H60 H 0.3936 -0.2508 0.7266 0.056 Uiso 1 1 calc R . . C61 C 0.4681(3) -0.1698(4) 0.76771(16) 0.0345(13) Uani 1 1 d . . . C62 C 0.5488(4) -0.1797(5) 0.71068(17) 0.0413(15) Uani 1 1 d . . . C63 C 0.6379(4) -0.1526(5) 0.65705(18) 0.0434(15) Uani 1 1 d . . . C64 C 0.7147(4) -0.1159(5) 0.65116(19) 0.0485(17) Uani 1 1 d . . . H64 H 0.7471 -0.0811 0.6736 0.058 Uiso 1 1 calc R . . C65 C 0.7440(4) -0.1294(5) 0.6135(2) 0.0533(18) Uani 1 1 d . . . H65 H 0.7953 -0.1026 0.6092 0.064 Uiso 1 1 calc R . . C66 C 0.6964(4) -0.1837(5) 0.58136(17) 0.0471(16) Uani 1 1 d . . . C67 C 0.6218(4) -0.2210(4) 0.58617(17) 0.0437(15) Uani 1 1 d . . . H67 H 0.5902 -0.2569 0.5639 0.052 Uiso 1 1 calc R . . C68 C 0.5932(4) -0.2057(5) 0.62412(17) 0.0464(16) Uani 1 1 d . . . H68 H 0.5415 -0.2321 0.6279 0.056 Uiso 1 1 calc R . . C69 C -0.0243(8) 0.7852(11) 0.5747(5) 0.154(5) Uani 1 1 d . . . H69A H -0.0477 0.8135 0.5984 0.185 Uiso 1 1 calc R . . H69B H -0.0704 0.7569 0.5539 0.185 Uiso 1 1 calc R . . C70 C 0.1034(6) 0.8476(9) 0.5726(3) 0.089(3) Uani 1 1 d . . . H70A H 0.1140 0.8925 0.5964 0.107 Uiso 1 1 calc R . . H70B H 0.1434 0.8600 0.5530 0.107 Uiso 1 1 calc R . . C71 C 0.1171(8) 0.7625(15) 0.5891(3) 0.152(7) Uani 1 1 d . . . H71A H 0.1514 0.7660 0.6185 0.183 Uiso 1 1 calc R . . H71B H 0.1485 0.7264 0.5708 0.183 Uiso 1 1 calc R . . C72 C 0.0406(9) 0.7196(9) 0.5909(6) 0.206(8) Uani 1 1 d . . . H72A H 0.0377 0.7023 0.6210 0.247 Uiso 1 1 calc R . . H72B H 0.0341 0.6640 0.5728 0.247 Uiso 1 1 calc R . . C73 C 0.3868(10) 0.516(3) 0.9253(9) 0.42(3) Uani 1 1 d . . . H73A H 0.3655 0.5602 0.9445 0.506 Uiso 1 1 calc R . . H73B H 0.3375 0.4899 0.9060 0.506 Uiso 1 1 calc R . . C74 C 0.4302(18) 0.5605(18) 0.9019(4) 0.31(2) Uani 1 1 d . . . H74A H 0.4280 0.6270 0.9065 0.367 Uiso 1 1 calc R . . H74B H 0.4128 0.5466 0.8708 0.367 Uiso 1 1 calc R . . C75 C 0.5086(11) 0.5244(12) 0.9188(4) 0.170(7) Uani 1 1 d . . . H75A H 0.5227 0.4716 0.9020 0.203 Uiso 1 1 calc R . . H75B H 0.5537 0.5706 0.9212 0.203 Uiso 1 1 calc R . . C76 C 0.4919(9) 0.499(3) 0.9585(8) 0.46(3) Uani 1 1 d . . . H76A H 0.5327 0.4542 0.9733 0.552 Uiso 1 1 calc R . . H76B H 0.4891 0.5522 0.9776 0.552 Uiso 1 1 calc R . . C77 C 1.1798(6) 0.6207(9) 0.8656(4) 0.132(5) Uani 1 1 d . . . H77A H 1.1834 0.6517 0.8385 0.198 Uiso 1 1 calc R . . H77B H 1.1329 0.5775 0.8608 0.198 Uiso 1 1 calc R . . H77C H 1.2323 0.5879 0.8760 0.198 Uiso 1 1 calc R . . C78 C 1.1665(5) 0.6856(7) 0.8967(3) 0.083(3) Uani 1 1 d . . . H78A H 1.2209 0.7153 0.9082 0.099 Uiso 1 1 calc R . . H78B H 1.1485 0.6531 0.9210 0.099 Uiso 1 1 calc R . . C79 C 1.1017(4) 0.7602(5) 0.8810(2) 0.0580(18) Uani 1 1 d . . . H79A H 1.1022 0.8060 0.9041 0.070 Uiso 1 1 calc R . . H79B H 1.1169 0.7913 0.8556 0.070 Uiso 1 1 calc R . . C80 C 1.0143(4) 0.7200(4) 0.86874(18) 0.0465(15) Uani 1 1 d . . . H80A H 1.0165 0.6700 0.8479 0.056 Uiso 1 1 calc R . . H80B H 0.9988 0.6928 0.8949 0.056 Uiso 1 1 calc R . . C81 C 0.8638(4) 0.7327(5) 0.84115(19) 0.0502(16) Uani 1 1 d . . . H81A H 0.8707 0.6790 0.8231 0.060 Uiso 1 1 calc R . . H81B H 0.8530 0.7097 0.8692 0.060 Uiso 1 1 calc R . . C82 C 0.7878(4) 0.7842(6) 0.8196(2) 0.064(2) Uani 1 1 d . . . H82A H 0.7830 0.8408 0.8361 0.077 Uiso 1 1 calc R . . H82B H 0.7954 0.8019 0.7903 0.077 Uiso 1 1 calc R . . C83 C 0.7102(4) 0.7328(5) 0.81637(19) 0.0542(17) Uani 1 1 d . . . H83A H 0.7180 0.6716 0.8045 0.065 Uiso 1 1 calc R . . H83B H 0.6652 0.7640 0.7961 0.065 Uiso 1 1 calc R . . C84 C 0.6839(6) 0.7229(8) 0.8593(3) 0.108(3) Uani 1 1 d . . . H84A H 0.6821 0.7830 0.8725 0.162 Uiso 1 1 calc R . . H84B H 0.7242 0.6842 0.8781 0.162 Uiso 1 1 calc R . . H84C H 0.6280 0.6951 0.8553 0.162 Uiso 1 1 calc R . . C85 C 0.9086(4) 0.9022(6) 0.99516(19) 0.065(2) Uani 1 1 d . . . H85A H 0.9380 0.8485 1.0089 0.098 Uiso 1 1 calc R . . H85B H 0.8479 0.8918 0.9904 0.098 Uiso 1 1 calc R . . H85C H 0.9227 0.9553 1.0139 0.098 Uiso 1 1 calc R . . C86 C 0.9354(4) 0.9194(5) 0.95227(18) 0.0545(18) Uani 1 1 d . . . H86A H 0.9079 0.9756 0.9395 0.065 Uiso 1 1 calc R . . H86B H 0.9968 0.9298 0.9575 0.065 Uiso 1 1 calc R . . C87 C 0.9148(4) 0.8433(5) 0.92040(18) 0.0490(16) Uani 1 1 d . . . H87A H 0.8535 0.8321 0.9151 0.059 Uiso 1 1 calc R . . H87B H 0.9433 0.7870 0.9327 0.059 Uiso 1 1 calc R . . C88 C 0.9418(4) 0.8649(4) 0.87809(17) 0.0388(14) Uani 1 1 d . . . H88A H 0.9020 0.9097 0.8623 0.047 Uiso 1 1 calc R . . H88B H 0.9978 0.8940 0.8843 0.047 Uiso 1 1 calc R . . C89 C 0.9633(4) 0.8227(5) 0.80676(16) 0.0459(15) Uani 1 1 d . . . H89A H 1.0164 0.8577 0.8122 0.055 Uiso 1 1 calc R . . H89B H 0.9175 0.8648 0.7944 0.055 Uiso 1 1 calc R . . C90 C 0.9699(5) 0.7450(7) 0.77352(19) 0.076(3) Uani 1 1 d . . . H90A H 0.9385 0.6903 0.7797 0.091 Uiso 1 1 calc R . . H90B H 1.0292 0.7282 0.7738 0.091 Uiso 1 1 calc R . . C91 C 0.9255(9) 0.7929(7) 0.7251(3) 0.168(7) Uani 1 1 d . . . H91A H 0.8636 0.7963 0.7217 0.202 Uiso 1 1 calc R . . H91B H 0.9482 0.8545 0.7216 0.202 Uiso 1 1 calc R . . C92 C 0.9491(9) 0.7339(10) 0.6980(6) 0.208(9) Uani 1 1 d . . . H92A H 0.9189 0.6765 0.6992 0.312 Uiso 1 1 calc R . . H92B H 1.0097 0.7231 0.7060 0.312 Uiso 1 1 calc R . . H92C H 0.9363 0.7585 0.6686 0.312 Uiso 1 1 calc R . . C93 C 0.1641(4) 0.2527(6) 0.7447(2) 0.063(2) Uani 1 1 d . . . H93A H 0.1578 0.3185 0.7402 0.095 Uiso 1 1 calc R . . H93B H 0.2237 0.2378 0.7537 0.095 Uiso 1 1 calc R . . H93C H 0.1333 0.2337 0.7673 0.095 Uiso 1 1 calc R . . C94 C 0.1298(4) 0.2039(5) 0.70363(19) 0.0543(18) Uani 1 1 d . . . H94A H 0.0723 0.2263 0.6925 0.065 Uiso 1 1 calc R . . H94B H 0.1258 0.1381 0.7098 0.065 Uiso 1 1 calc R . . C95 C 0.1830(3) 0.2162(5) 0.66877(18) 0.0454(15) Uani 1 1 d . . . H95A H 0.1869 0.2816 0.6619 0.054 Uiso 1 1 calc R . . H95B H 0.2404 0.1929 0.6792 0.054 Uiso 1 1 calc R . . C96 C 0.1422(4) 0.1641(5) 0.62856(18) 0.0499(17) Uani 1 1 d . . . H96A H 0.1284 0.1021 0.6375 0.060 Uiso 1 1 calc R . . H96B H 0.0886 0.1945 0.6163 0.060 Uiso 1 1 calc R . . C97 C 0.1368(4) 0.1133(5) 0.5565(2) 0.0561(18) Uani 1 1 d . . . H97A H 0.0877 0.1538 0.5481 0.067 Uiso 1 1 calc R . . H97B H 0.1160 0.0550 0.5663 0.067 Uiso 1 1 calc R . . C98 C 0.1748(4) 0.0949(6) 0.5170(2) 0.066(2) Uani 1 1 d . . . H98A H 0.2238 0.0540 0.5246 0.079 Uiso 1 1 calc R . . H98B H 0.1942 0.1527 0.5060 0.079 Uiso 1 1 calc R . . C99 C 0.1081(5) 0.0500(6) 0.4817(2) 0.084(3) Uani 1 1 d . . . H99A H 0.0946 -0.0114 0.4913 0.101 Uiso 1 1 calc R . . H99B H 0.0560 0.0868 0.4773 0.101 Uiso 1 1 calc R . . C100 C 0.1400(6) 0.0425(8) 0.4392(3) 0.115(4) Uani 1 1 d . . . H10V H 0.1985 0.0220 0.4449 0.173 Uiso 1 1 calc R . . H10W H 0.1364 0.1022 0.4251 0.173 Uiso 1 1 calc R . . H10$ H 0.1055 -0.0014 0.4204 0.173 Uiso 1 1 calc R . . C101 C 0.3387(8) -0.1361(12) 0.6318(5) 0.187(7) Uani 1 1 d . . . H10S H 0.3081 -0.1666 0.6060 0.281 Uiso 1 1 calc R . . H10T H 0.3090 -0.1453 0.6559 0.281 Uiso 1 1 calc R . . H10U H 0.3954 -0.1616 0.6392 0.281 Uiso 1 1 calc R . . C102 C 0.3436(6) -0.0481(6) 0.6240(4) 0.122(5) Uani 1 1 d . . . H10Q H 0.3645 -0.0399 0.5967 0.147 Uiso 1 1 calc R . . H10R H 0.3851 -0.0204 0.6474 0.147 Uiso 1 1 calc R . . C103 C 0.2564(4) 0.0047(6) 0.6206(3) 0.075(2) Uani 1 1 d . . . H10D H 0.2124 -0.0251 0.5992 0.090 Uiso 1 1 calc R . . H10E H 0.2380 0.0047 0.6489 0.090 Uiso 1 1 calc R . . C104 C 0.2706(4) 0.0988(5) 0.6072(2) 0.0484(16) Uani 1 1 d . . . H10O H 0.3024 0.0962 0.5831 0.058 Uiso 1 1 calc R . . H10P H 0.3066 0.1303 0.6316 0.058 Uiso 1 1 calc R . . C105 C 0.2244(3) 0.2463(4) 0.58133(18) 0.0405(14) Uani 1 1 d . . . H10H H 0.2598 0.2728 0.6073 0.049 Uiso 1 1 calc R . . H10I H 0.2605 0.2375 0.5595 0.049 Uiso 1 1 calc R . . C106 C 0.1573(3) 0.3130(4) 0.56407(19) 0.0441(15) Uani 1 1 d . . . H10J H 0.1117 0.3095 0.5811 0.053 Uiso 1 1 calc R . . H10K H 0.1334 0.2977 0.5337 0.053 Uiso 1 1 calc R . . C107 C 0.1928(4) 0.4090(5) 0.56641(16) 0.0457(16) Uani 1 1 d . . . H10F H 0.2406 0.4112 0.5508 0.055 Uiso 1 1 calc R . . H10G H 0.2142 0.4250 0.5970 0.055 Uiso 1 1 calc R . . C108 C 0.1268(4) 0.4788(5) 0.5468(2) 0.064(2) Uani 1 1 d . . . H10L H 0.0737 0.4657 0.5562 0.095 Uiso 1 1 calc R . . H10M H 0.1185 0.4754 0.5152 0.095 Uiso 1 1 calc R . . H10N H 0.1460 0.5400 0.5562 0.095 Uiso 1 1 calc R . . C109 C 0.3658(5) 0.2666(8) 1.0429(3) 0.102(3) Uani 1 1 d . . . H10A H 0.3455 0.2124 1.0560 0.153 Uiso 1 1 calc R . . H10B H 0.3195 0.3098 1.0351 0.153 Uiso 1 1 calc R . . H10C H 0.4108 0.2951 1.0637 0.153 Uiso 1 1 calc R . . C110 C 0.3986(5) 0.2399(7) 1.0036(2) 0.083(3) Uani 1 1 d . . . H11I H 0.4453 0.1962 1.0118 0.100 Uiso 1 1 calc R . . H11J H 0.4215 0.2945 0.9914 0.100 Uiso 1 1 calc R . . C111 C 0.3332(4) 0.1978(5) 0.96971(19) 0.0524(17) Uani 1 1 d . . . H11E H 0.3107 0.1422 0.9812 0.063 Uiso 1 1 calc R . . H11F H 0.2862 0.2410 0.9611 0.063 Uiso 1 1 calc R . . C112 C 0.3710(4) 0.1747(5) 0.93226(17) 0.0449(16) Uani 1 1 d . . . H11A H 0.4197 0.1343 0.9420 0.054 Uiso 1 1 calc R . . H11B H 0.3926 0.2313 0.9211 0.054 Uiso 1 1 calc R . . C113 C 0.3621(3) 0.1168(5) 0.85927(17) 0.0438(15) Uani 1 1 d . . . H11C H 0.4152 0.0853 0.8714 0.053 Uiso 1 1 calc R . . H11D H 0.3770 0.1783 0.8502 0.053 Uiso 1 1 calc R . . C114 C 0.3202(3) 0.0654(5) 0.81944(17) 0.0431(14) Uani 1 1 d . . . H11P H 0.2620 0.0875 0.8100 0.052 Uiso 1 1 calc R . . H11Q H 0.3182 -0.0004 0.8259 0.052 Uiso 1 1 calc R . . C115 C 0.3710(4) 0.0813(5) 0.78403(18) 0.0445(15) Uani 1 1 d . . . H11R H 0.3728 0.1475 0.7782 0.053 Uiso 1 1 calc R . . H11S H 0.4294 0.0606 0.7943 0.053 Uiso 1 1 calc R . . C116 C 0.3361(4) 0.0328(5) 0.74258(19) 0.0528(17) Uani 1 1 d . . . H11T H 0.2791 0.0546 0.7316 0.079 Uiso 1 1 calc R . . H11U H 0.3348 -0.0328 0.7479 0.079 Uiso 1 1 calc R . . H11V H 0.3718 0.0451 0.7213 0.079 Uiso 1 1 calc R . . C117 C 0.1403(5) 0.3649(6) 0.8989(2) 0.071(2) Uani 1 1 d . . . H11K H 0.1861 0.3982 0.9170 0.107 Uiso 1 1 calc R . . H11L H 0.1259 0.3113 0.9146 0.107 Uiso 1 1 calc R . . H11M H 0.0910 0.4046 0.8919 0.107 Uiso 1 1 calc R . . C118 C 0.1681(4) 0.3345(5) 0.8572(2) 0.0576(18) Uani 1 1 d . . . H11G H 0.1225 0.2978 0.8401 0.069 Uiso 1 1 calc R . . H11H H 0.1757 0.3892 0.8400 0.069 Uiso 1 1 calc R . . C119 C 0.2486(4) 0.2792(5) 0.86361(19) 0.0468(15) Uani 1 1 d . . . H11N H 0.2685 0.2740 0.8358 0.056 Uiso 1 1 calc R . . H11O H 0.2925 0.3108 0.8844 0.056 Uiso 1 1 calc R . . C120 C 0.2348(3) 0.1855(4) 0.88035(18) 0.0431(15) Uani 1 1 d . . . H12S H 0.1970 0.1519 0.8574 0.052 Uiso 1 1 calc R . . H12T H 0.2050 0.1920 0.9050 0.052 Uiso 1 1 calc R . . C121 C 0.2819(3) 0.0382(4) 0.90904(17) 0.0389(14) Uani 1 1 d . . . H12N H 0.2472 0.0085 0.8837 0.047 Uiso 1 1 calc R . . H12O H 0.2452 0.0498 0.9303 0.047 Uiso 1 1 calc R . . C122 C 0.3496(3) -0.0269(4) 0.92865(18) 0.0417(15) Uani 1 1 d . . . H12J H 0.3961 -0.0247 0.9122 0.050 Uiso 1 1 calc R . . H12K H 0.3721 -0.0083 0.9587 0.050 Uiso 1 1 calc R . . C123 C 0.3168(4) -0.1220(5) 0.92841(19) 0.0473(16) Uani 1 1 d . . . H12L H 0.2986 -0.1421 0.8982 0.057 Uiso 1 1 calc R . . H12M H 0.2671 -0.1228 0.9426 0.057 Uiso 1 1 calc R . . C124 C 0.3816(4) -0.1885(5) 0.95135(19) 0.0567(19) Uani 1 1 d . . . H12P H 0.3963 -0.1721 0.9819 0.085 Uiso 1 1 calc R . . H12Q H 0.4320 -0.1860 0.9383 0.085 Uiso 1 1 calc R . . H12R H 0.3584 -0.2502 0.9486 0.085 Uiso 1 1 calc R . . C125 C 0.5752(9) 0.5324(14) 0.8027(3) 0.248(12) Uani 1 1 d . . . H12U H 0.5189 0.5170 0.8077 0.373 Uiso 1 1 calc R . . H12V H 0.5789 0.5981 0.7981 0.373 Uiso 1 1 calc R . . H12W H 0.6170 0.5145 0.8278 0.373 Uiso 1 1 calc R . . C126 C 0.5905(7) 0.4870(9) 0.7669(3) 0.145(6) Uani 1 1 d . . . H12B H 0.5822 0.4212 0.7713 0.174 Uiso 1 1 calc R . . H12C H 0.6502 0.4960 0.7650 0.174 Uiso 1 1 calc R . . C127 C 0.5381(7) 0.5134(7) 0.7243(3) 0.111(4) Uani 1 1 d . . . H12H H 0.4780 0.5113 0.7265 0.133 Uiso 1 1 calc R . . H12I H 0.5518 0.5766 0.7171 0.133 Uiso 1 1 calc R . . C128 C 0.5536(6) 0.4512(7) 0.6893(3) 0.100(3) Uani 1 1 d . . . H12D H 0.5044 0.4105 0.6819 0.120 Uiso 1 1 calc R . . H12E H 0.6025 0.4125 0.7009 0.120 Uiso 1 1 calc R . . C129 C 0.5743(5) 0.4199(6) 0.6173(3) 0.086(3) Uani 1 1 d . . . H12F H 0.5188 0.3896 0.6107 0.103 Uiso 1 1 calc R . . H12G H 0.6153 0.3743 0.6314 0.103 Uiso 1 1 calc R . . C130 C 0.5988(5) 0.4474(7) 0.5755(3) 0.100(3) Uani 1 1 d . . . H13O H 0.6588 0.4648 0.5806 0.120 Uiso 1 1 calc R . . H13P H 0.5652 0.5007 0.5634 0.120 Uiso 1 1 calc R . . C131 C 0.5837(6) 0.3683(7) 0.5436(4) 0.107(3) Uani 1 1 d . . . H13J H 0.6136 0.3139 0.5571 0.128 Uiso 1 1 calc R . . H13K H 0.5229 0.3541 0.5375 0.128 Uiso 1 1 calc R . . C132 C 0.6125(7) 0.3875(9) 0.5014(4) 0.131(4) Uani 1 1 d . . . H13L H 0.6732 0.3982 0.5070 0.197 Uiso 1 1 calc R . . H13M H 0.5835 0.4416 0.4879 0.197 Uiso 1 1 calc R . . H13N H 0.5994 0.3352 0.4820 0.197 Uiso 1 1 calc R . . C133 C 0.3295(5) 0.6283(9) 0.6517(3) 0.120(4) Uani 1 1 d . . . H13E H 0.3817 0.6453 0.6710 0.180 Uiso 1 1 calc R . . H13F H 0.3011 0.5804 0.6652 0.180 Uiso 1 1 calc R . . H13G H 0.2929 0.6817 0.6461 0.180 Uiso 1 1 calc R . . C134 C 0.3489(5) 0.5948(5) 0.6109(2) 0.067(2) Uani 1 1 d . . . H13H H 0.3696 0.6459 0.5952 0.080 Uiso 1 1 calc R . . H13I H 0.2969 0.5713 0.5927 0.080 Uiso 1 1 calc R . . C135 C 0.4136(4) 0.5209(6) 0.6178(2) 0.067(2) Uani 1 1 d . . . H13A H 0.4014 0.4783 0.6402 0.081 Uiso 1 1 calc R . . H13B H 0.4117 0.4863 0.5906 0.081 Uiso 1 1 calc R . . C136 C 0.4986(4) 0.5612(5) 0.63157(19) 0.0500(16) Uani 1 1 d . . . H13C H 0.4955 0.6065 0.6545 0.060 Uiso 1 1 calc R . . H13D H 0.5136 0.5944 0.6067 0.060 Uiso 1 1 calc R . . C137 C 0.6482(4) 0.5476(6) 0.6557(3) 0.090(3) Uani 1 1 d . . . H13Q H 0.6451 0.5945 0.6779 0.109 Uiso 1 1 calc R . . H13R H 0.6535 0.5794 0.6286 0.109 Uiso 1 1 calc R . . C138 C 0.7248(5) 0.4909(7) 0.6698(4) 0.143(5) Uani 1 1 d . . . H13S H 0.7274 0.4405 0.6493 0.171 Uiso 1 1 calc R . . H13T H 0.7250 0.4650 0.6989 0.171 Uiso 1 1 calc R . . C139 C 0.8123(12) 0.5684(14) 0.6708(6) 0.290(17) Uani 1 1 d . . . H13U H 0.8661 0.5393 0.6680 0.348 Uiso 1 1 calc R . . H13V H 0.8001 0.6229 0.6523 0.348 Uiso 1 1 calc R . . C140 C 0.7991(8) 0.5782(11) 0.7120(6) 0.243(12) Uani 1 1 d . . . H14A H 0.7515 0.5403 0.7162 0.365 Uiso 1 1 calc R . . H14B H 0.7867 0.6421 0.7171 0.365 Uiso 1 1 calc R . . H14C H 0.8494 0.5594 0.7322 0.365 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 0.0341(8) 0.0366(9) 0.0297(7) 0.0020(6) 0.0100(6) -0.0036(7) P2 0.0494(10) 0.0492(12) 0.0435(8) -0.0059(8) 0.0130(7) -0.0123(8) O1 0.101(4) 0.089(4) 0.030(2) -0.020(3) 0.015(2) -0.017(3) O2 0.067(3) 0.098(5) 0.051(3) -0.027(3) 0.017(2) -0.005(3) O3 0.053(3) 0.046(3) 0.034(2) 0.0011(19) 0.0053(18) 0.004(2) O4 0.054(2) 0.060(3) 0.039(2) -0.016(2) 0.0187(19) -0.011(2) O5 0.057(3) 0.061(3) 0.055(2) 0.000(2) 0.039(2) -0.007(2) O6 0.077(3) 0.035(3) 0.049(2) -0.012(2) 0.022(2) -0.012(2) O7 0.098(4) 0.114(5) 0.063(3) -0.021(3) 0.048(3) -0.015(4) O8 0.099(4) 0.107(5) 0.056(3) -0.043(3) 0.031(3) -0.023(3) O9 0.084(4) 0.129(6) 0.037(2) -0.023(3) 0.014(2) 0.009(4) O10 0.127(5) 0.137(6) 0.028(2) 0.005(3) 0.015(3) 0.008(4) O11 0.060(3) 0.043(3) 0.037(2) 0.0099(19) 0.0014(19) 0.007(2) O12 0.043(2) 0.040(2) 0.0323(18) -0.0067(17) 0.0140(16) 0.0015(18) O13 0.044(2) 0.041(2) 0.0336(19) -0.0032(17) 0.0212(17) -0.0038(18) O14 0.068(3) 0.045(3) 0.047(2) -0.022(2) 0.022(2) -0.024(2) O15 0.110(4) 0.097(5) 0.039(2) -0.021(3) 0.028(3) -0.006(3) O16 0.064(3) 0.118(5) 0.068(3) -0.022(3) 0.041(3) -0.006(3) O17 0.034(2) 0.033(2) 0.0347(18) 0.0094(16) 0.0049(15) -0.0047(17) O18 0.058(2) 0.031(2) 0.0315(18) -0.0087(16) 0.0156(17) -0.0043(19) O19 0.031(2) 0.040(3) 0.0333(18) 0.0075(17) 0.0078(15) -0.0073(18) O20 0.038(2) 0.038(2) 0.0393(19) -0.0012(17) 0.0141(16) -0.0061(18) O21 0.052(2) 0.035(2) 0.0337(19) -0.0034(17) 0.0179(17) -0.0062(19) O22 0.0251(19) 0.037(2) 0.047(2) 0.0042(18) 0.0103(16) -0.0096(17) O23 0.066(3) 0.063(3) 0.048(2) -0.015(2) 0.021(2) -0.013(2) O24 0.039(2) 0.042(3) 0.0362(19) 0.0035(17) 0.0112(16) -0.0089(18) O25 0.076(3) 0.066(4) 0.081(3) 0.027(3) -0.015(3) -0.014(3) O26 0.040(3) 0.088(5) 0.154(5) 0.069(5) 0.004(3) 0.000(3) O27 0.75(6) 0.31(3) 0.32(3) 0.16(2) -0.03(3) -0.20(4) O28 0.258(15) 0.176(13) 0.262(14) 0.001(10) 0.050(12) -0.033(12) N1 0.065(4) 0.076(5) 0.034(3) -0.013(3) 0.009(3) -0.022(3) N2 0.038(3) 0.036(3) 0.032(2) 0.002(2) 0.0072(19) -0.001(2) N3 0.043(3) 0.038(3) 0.029(2) 0.002(2) 0.0107(19) 0.000(2) N4 0.044(3) 0.052(4) 0.032(2) -0.009(2) 0.016(2) 0.002(3) N5 0.036(3) 0.056(4) 0.032(2) 0.001(2) 0.014(2) -0.010(2) N6 0.046(3) 0.057(4) 0.038(2) -0.010(2) 0.026(2) -0.016(3) N7 0.045(3) 0.038(3) 0.034(2) 0.001(2) 0.020(2) -0.004(2) N8 0.055(3) 0.032(3) 0.050(3) -0.013(2) 0.020(2) -0.008(3) N9 0.078(4) 0.040(3) 0.043(3) -0.015(2) 0.030(3) -0.018(3) N10 0.076(4) 0.062(4) 0.051(3) -0.008(3) 0.029(3) 0.000(3) N11 0.076(5) 0.125(7) 0.036(3) -0.010(4) 0.008(3) 0.006(5) N12 0.042(3) 0.034(3) 0.038(2) 0.007(2) 0.002(2) 0.001(2) N13 0.036(3) 0.027(3) 0.042(2) 0.007(2) 0.013(2) 0.006(2) N14 0.039(3) 0.038(3) 0.032(2) -0.001(2) 0.013(2) 0.001(2) N15 0.034(3) 0.042(3) 0.026(2) 0.0006(19) 0.0126(19) 0.001(2) N16 0.032(2) 0.038(3) 0.027(2) -0.0101(19) 0.0062(18) -0.006(2) N17 0.036(3) 0.042(3) 0.029(2) -0.005(2) 0.0112(19) -0.015(2) N18 0.049(3) 0.035(3) 0.029(2) -0.008(2) 0.013(2) -0.011(2) N19 0.055(3) 0.053(4) 0.048(3) -0.026(3) 0.026(2) -0.025(3) N20 0.068(4) 0.078(5) 0.039(3) -0.013(3) 0.021(3) 0.018(3) N21 0.049(3) 0.036(3) 0.035(2) -0.005(2) 0.001(2) -0.002(2) N22 0.039(3) 0.049(4) 0.047(3) -0.001(2) 0.007(2) -0.006(2) N23 0.033(3) 0.037(3) 0.047(3) 0.005(2) 0.005(2) -0.002(2) N24 0.052(3) 0.038(4) 0.103(5) 0.021(3) 0.003(3) 0.004(3) C1 0.050(4) 0.066(5) 0.025(3) -0.012(3) 0.007(3) -0.014(3) C2 0.050(4) 0.048(4) 0.034(3) -0.006(3) 0.005(3) -0.013(3) C3 0.038(3) 0.044(4) 0.044(3) -0.003(3) 0.006(3) -0.005(3) C4 0.033(3) 0.044(4) 0.036(3) -0.004(3) 0.006(2) -0.005(3) C5 0.044(3) 0.064(5) 0.029(3) -0.007(3) 0.000(2) -0.002(3) C6 0.043(4) 0.061(5) 0.052(4) -0.013(3) 0.011(3) 0.000(3) C7 0.034(3) 0.041(4) 0.044(3) 0.009(3) 0.013(3) -0.011(3) C8 0.034(3) 0.030(4) 0.051(3) -0.003(3) 0.017(3) -0.004(3) C9 0.034(3) 0.042(4) 0.069(4) -0.001(3) 0.025(3) -0.003(3) C10 0.045(4) 0.050(5) 0.085(5) -0.008(4) 0.023(4) -0.001(3) C11 0.057(4) 0.047(5) 0.072(5) -0.017(4) 0.032(4) -0.003(4) C12 0.046(4) 0.041(4) 0.051(3) -0.008(3) 0.021(3) -0.002(3) C13 0.039(3) 0.040(4) 0.048(3) -0.011(3) 0.019(3) -0.013(3) C14 0.048(4) 0.041(4) 0.035(3) -0.012(3) 0.020(3) -0.019(3) C15 0.039(3) 0.063(5) 0.032(3) -0.013(3) 0.006(2) -0.004(3) C16 0.053(4) 0.072(5) 0.043(3) -0.014(3) 0.009(3) -0.010(4) C17 0.072(5) 0.110(7) 0.035(3) -0.017(4) 0.004(3) 0.006(5) C18 0.099(6) 0.087(6) 0.033(3) -0.005(4) 0.011(3) 0.012(5) C19 0.093(5) 0.073(6) 0.042(3) 0.013(3) 0.026(4) 0.010(4) C20 0.050(4) 0.060(4) 0.034(3) -0.011(3) 0.017(3) -0.006(3) C21 0.040(3) 0.043(4) 0.043(3) -0.003(3) 0.018(3) 0.006(3) C22 0.036(3) 0.035(4) 0.051(3) 0.007(3) 0.018(3) 0.000(3) C23 0.041(3) 0.045(4) 0.066(4) 0.013(3) 0.022(3) -0.002(3) C24 0.047(4) 0.050(5) 0.080(5) 0.016(4) 0.024(3) -0.006(3) C25 0.031(3) 0.053(5) 0.089(5) -0.006(4) 0.011(3) -0.014(3) C26 0.047(4) 0.044(4) 0.053(4) -0.004(3) 0.011(3) 0.004(3) C27 0.041(3) 0.029(3) 0.046(3) 0.002(3) 0.013(3) 0.000(3) C28 0.055(4) 0.049(5) 0.036(3) -0.004(3) 0.011(3) -0.006(3) C29 0.076(5) 0.026(4) 0.043(3) -0.013(3) 0.024(3) -0.003(3) C30 0.062(4) 0.042(4) 0.043(3) -0.013(3) 0.019(3) -0.009(3) C31 0.076(5) 0.037(4) 0.039(3) -0.013(3) 0.011(3) -0.002(3) C32 0.056(4) 0.039(4) 0.043(3) -0.006(3) 0.020(3) 0.005(3) C33 0.070(4) 0.053(5) 0.043(3) -0.010(3) 0.026(3) -0.006(4) C34 0.061(4) 0.059(5) 0.045(3) -0.013(3) 0.016(3) -0.008(4) C35 0.061(4) 0.076(6) 0.025(3) 0.000(3) 0.009(3) 0.009(4) C36 0.054(4) 0.082(6) 0.037(3) 0.002(3) 0.008(3) 0.006(4) C37 0.042(3) 0.052(4) 0.032(3) 0.004(3) 0.000(2) 0.009(3) C38 0.037(3) 0.043(4) 0.023(3) 0.001(2) 0.002(2) -0.008(3) C39 0.042(3) 0.056(5) 0.036(3) 0.007(3) -0.001(3) -0.003(3) C40 0.058(4) 0.087(6) 0.015(3) 0.005(3) -0.007(3) -0.007(4) C41 0.041(3) 0.036(4) 0.036(3) 0.000(3) 0.003(2) -0.008(3) C42 0.032(3) 0.040(4) 0.043(3) 0.008(3) 0.012(3) -0.003(3) C43 0.053(4) 0.045(4) 0.049(3) 0.003(3) 0.013(3) 0.001(3) C44 0.049(4) 0.047(4) 0.066(4) 0.014(3) 0.018(3) 0.012(3) C45 0.046(4) 0.030(4) 0.077(5) 0.008(3) 0.026(3) 0.014(3) C46 0.058(4) 0.035(4) 0.053(4) -0.006(3) 0.018(3) -0.001(3) C47 0.040(3) 0.030(3) 0.040(3) 0.002(2) 0.013(3) 0.003(3) C48 0.033(3) 0.034(4) 0.041(3) -0.012(3) 0.008(2) -0.012(3) C49 0.038(3) 0.040(4) 0.023(2) -0.005(2) 0.005(2) -0.005(3) C50 0.050(4) 0.035(4) 0.042(3) -0.007(3) 0.006(3) -0.001(3) C51 0.060(4) 0.061(5) 0.033(3) -0.010(3) 0.001(3) 0.008(3) C52 0.060(4) 0.052(4) 0.028(3) -0.009(3) -0.009(3) 0.011(3) C53 0.056(4) 0.041(4) 0.037(3) -0.006(3) 0.005(3) 0.005(3) C54 0.033(3) 0.041(4) 0.025(2) -0.001(2) 0.002(2) -0.004(3) C55 0.036(3) 0.035(3) 0.028(3) -0.004(2) 0.008(2) -0.005(3) C56 0.031(3) 0.037(4) 0.043(3) -0.002(3) 0.011(2) 0.000(3) C57 0.049(4) 0.043(4) 0.036(3) -0.004(3) 0.016(3) -0.009(3) C58 0.043(3) 0.046(4) 0.058(4) 0.004(3) 0.025(3) -0.007(3) C59 0.034(3) 0.046(4) 0.063(4) -0.013(3) 0.011(3) -0.016(3) C60 0.050(4) 0.042(4) 0.048(3) -0.006(3) 0.015(3) -0.016(3) C61 0.030(3) 0.037(4) 0.038(3) -0.006(3) 0.012(2) -0.014(3) C62 0.045(3) 0.045(4) 0.033(3) -0.006(3) 0.006(3) -0.007(3) C63 0.041(3) 0.044(4) 0.048(3) -0.004(3) 0.014(3) -0.008(3) C64 0.051(4) 0.053(5) 0.046(3) -0.014(3) 0.019(3) -0.017(3) C65 0.045(4) 0.059(5) 0.061(4) -0.014(3) 0.025(3) -0.003(3) C66 0.059(4) 0.050(4) 0.035(3) -0.007(3) 0.015(3) 0.007(3) C67 0.052(4) 0.045(4) 0.035(3) -0.008(3) 0.013(3) -0.011(3) C68 0.055(4) 0.048(4) 0.039(3) -0.006(3) 0.016(3) -0.019(3) C69 0.124(10) 0.118(12) 0.191(13) -0.037(10) -0.048(9) 0.032(9) C70 0.059(6) 0.114(9) 0.089(7) -0.048(6) -0.004(5) -0.033(6) C71 0.113(9) 0.30(2) 0.044(5) -0.048(9) 0.008(5) 0.076(12) C72 0.122(11) 0.077(10) 0.38(2) 0.049(12) -0.064(12) 0.031(9) C73 0.070(9) 0.99(10) 0.21(3) -0.12(4) 0.046(13) 0.00(2) C74 0.43(4) 0.38(4) 0.078(9) -0.017(13) -0.041(14) 0.33(3) C75 0.27(2) 0.166(16) 0.079(8) -0.002(8) 0.037(10) -0.054(14) C76 0.071(9) 0.97(10) 0.29(3) 0.34(4) -0.086(13) 0.01(2) C77 0.086(7) 0.131(11) 0.166(10) -0.056(9) -0.011(7) 0.016(7) C78 0.069(5) 0.086(7) 0.085(5) -0.018(5) -0.008(4) 0.011(5) C79 0.056(4) 0.049(5) 0.060(4) 0.001(3) -0.016(3) 0.004(4) C80 0.064(4) 0.032(4) 0.040(3) -0.006(3) 0.000(3) 0.003(3) C81 0.053(4) 0.050(4) 0.046(3) -0.011(3) 0.003(3) -0.002(3) C82 0.053(4) 0.077(6) 0.063(4) 0.004(4) 0.013(3) -0.004(4) C83 0.048(4) 0.061(5) 0.058(4) 0.001(3) 0.020(3) -0.003(3) C84 0.099(6) 0.139(10) 0.094(6) 0.034(6) 0.038(5) -0.013(6) C85 0.083(5) 0.074(6) 0.039(3) 0.001(3) 0.012(3) 0.026(4) C86 0.060(4) 0.056(5) 0.044(3) -0.009(3) 0.002(3) 0.013(4) C87 0.061(4) 0.034(4) 0.050(3) -0.004(3) 0.003(3) -0.003(3) C88 0.052(4) 0.024(3) 0.039(3) 0.004(2) 0.005(3) 0.003(3) C89 0.051(4) 0.054(4) 0.028(3) -0.006(3) -0.005(3) 0.000(3) C90 0.067(5) 0.116(8) 0.040(3) -0.020(4) -0.002(3) 0.030(5) C91 0.334(17) 0.097(8) 0.124(8) -0.107(7) 0.174(10) -0.156(10) C92 0.167(12) 0.102(12) 0.36(2) 0.130(15) 0.069(15) 0.003(10) C93 0.067(5) 0.074(6) 0.055(4) 0.001(4) 0.028(3) -0.005(4) C94 0.045(4) 0.063(5) 0.058(4) 0.021(3) 0.018(3) -0.003(3) C95 0.038(3) 0.038(4) 0.063(4) 0.017(3) 0.018(3) -0.001(3) C96 0.035(3) 0.064(5) 0.050(3) 0.011(3) 0.005(3) -0.005(3) C97 0.047(4) 0.052(5) 0.064(4) -0.006(3) -0.004(3) -0.015(3) C98 0.065(5) 0.058(5) 0.068(4) -0.017(4) -0.005(4) 0.002(4) C99 0.103(6) 0.057(6) 0.075(5) -0.006(4) -0.029(4) -0.011(5) C100 0.156(9) 0.100(8) 0.073(5) -0.044(5) -0.023(6) 0.035(7) C101 0.107(10) 0.161(17) 0.269(19) 0.005(13) -0.030(10) 0.015(10) C102 0.069(6) 0.036(6) 0.236(13) 0.055(7) -0.040(7) 0.010(5) C103 0.054(4) 0.055(5) 0.102(6) -0.001(4) -0.023(4) -0.001(4) C104 0.032(3) 0.043(4) 0.065(4) 0.000(3) -0.002(3) 0.008(3) C105 0.039(3) 0.038(4) 0.049(3) 0.001(3) 0.019(3) -0.011(3) C106 0.042(3) 0.050(4) 0.044(3) 0.006(3) 0.019(3) -0.001(3) C107 0.061(4) 0.053(4) 0.023(3) -0.002(3) 0.010(3) 0.000(3) C108 0.084(5) 0.056(5) 0.056(4) 0.011(4) 0.026(4) 0.002(4) C109 0.087(6) 0.130(10) 0.084(6) -0.030(6) 0.003(5) -0.001(6) C110 0.087(6) 0.104(8) 0.058(4) -0.024(5) 0.012(4) -0.017(5) C111 0.049(4) 0.051(5) 0.054(4) -0.006(3) 0.000(3) -0.003(3) C112 0.037(3) 0.056(4) 0.038(3) 0.006(3) -0.005(3) -0.012(3) C113 0.035(3) 0.047(4) 0.052(3) 0.014(3) 0.014(3) -0.002(3) C114 0.041(3) 0.040(4) 0.051(3) -0.008(3) 0.013(3) -0.007(3) C115 0.044(3) 0.043(4) 0.051(3) 0.011(3) 0.020(3) -0.009(3) C116 0.052(4) 0.058(5) 0.052(4) -0.006(3) 0.020(3) -0.005(3) C117 0.080(5) 0.063(6) 0.076(5) 0.006(4) 0.029(4) 0.017(4) C118 0.068(4) 0.037(4) 0.065(4) 0.004(3) 0.008(3) 0.001(3) C119 0.046(4) 0.043(4) 0.051(3) 0.005(3) 0.007(3) -0.005(3) C120 0.039(3) 0.044(4) 0.047(3) 0.003(3) 0.012(3) -0.005(3) C121 0.037(3) 0.041(4) 0.040(3) 0.003(3) 0.009(2) -0.006(3) C122 0.038(3) 0.050(4) 0.039(3) 0.020(3) 0.011(2) 0.007(3) C123 0.047(4) 0.053(5) 0.047(3) -0.002(3) 0.021(3) 0.003(3) C124 0.068(4) 0.057(5) 0.048(4) 0.020(3) 0.020(3) 0.010(4) C125 0.228(14) 0.43(3) 0.062(6) 0.075(11) -0.045(8) -0.267(18) C126 0.154(9) 0.198(14) 0.065(6) 0.064(7) -0.031(6) -0.105(10) C127 0.164(10) 0.071(7) 0.077(6) 0.016(5) -0.033(6) -0.012(7) C128 0.115(7) 0.073(7) 0.098(7) 0.050(6) -0.019(5) -0.002(6) C129 0.067(5) 0.036(5) 0.158(8) 0.009(5) 0.031(5) 0.011(4) C130 0.078(6) 0.066(7) 0.170(9) -0.004(6) 0.063(6) 0.008(5) C131 0.084(6) 0.050(6) 0.199(11) -0.015(6) 0.062(7) 0.011(5) C132 0.135(9) 0.096(9) 0.181(11) -0.008(8) 0.074(9) 0.016(7) C133 0.063(6) 0.179(13) 0.122(8) -0.041(8) 0.030(5) 0.015(6) C134 0.056(5) 0.050(5) 0.087(5) -0.017(4) -0.005(4) -0.008(4) C135 0.063(5) 0.064(6) 0.068(4) 0.002(4) -0.005(4) -0.007(4) C136 0.066(4) 0.035(4) 0.045(3) -0.004(3) -0.001(3) 0.003(3) C137 0.048(5) 0.052(6) 0.161(8) 0.027(5) -0.008(5) 0.004(4) C138 0.062(6) 0.057(7) 0.278(14) 0.032(8) -0.048(7) -0.009(5) C139 0.26(2) 0.19(2) 0.31(2) -0.160(19) -0.23(2) 0.135(18) C140 0.090(8) 0.145(15) 0.44(3) 0.180(18) -0.104(14) -0.083(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O19 1.500(4) . ? P1 O17 1.504(4) . ? P1 O18 1.507(4) . ? P1 O20 1.586(3) . ? P2 O24 1.463(4) . ? P2 O22 1.491(4) . ? P2 O21 1.495(4) . ? P2 O23 1.629(4) . ? O1 N1 1.238(8) . ? O2 N1 1.236(8) . ? O3 C7 1.202(7) . ? O4 C14 1.213(6) . ? O5 C21 1.222(6) . ? O6 C28 1.212(8) . ? O7 N10 1.226(7) . ? O8 N10 1.207(7) . ? O9 N11 1.215(9) . ? O10 N11 1.223(9) . ? O11 C41 1.211(7) . ? O12 C48 1.233(6) . ? O13 C55 1.212(5) . ? O14 C62 1.225(7) . ? O15 N20 1.225(7) . ? O16 N20 1.196(7) . ? O27 C73 1.06(5) . ? O27 C76 1.31(3) . ? O28 C70 1.304(15) . ? O28 C69 1.609(18) . ? N1 C1 1.432(7) . ? N2 C4 1.368(6) . ? N2 C7 1.393(8) . ? N3 C7 1.361(6) . ? N3 C8 1.403(7) . ? N4 C14 1.390(7) . ? N4 C13 1.403(8) . ? N5 C14 1.344(7) . ? N5 C15 1.449(7) . ? N6 C21 1.319(7) . ? N6 C20 1.450(7) . ? N7 C22 1.356(7) . ? N7 C21 1.389(7) . ? N8 C28 1.363(7) . ? N8 C27 1.418(7) . ? N9 C28 1.368(7) . ? N9 C29 1.392(6) . ? N10 C32 1.456(7) . ? N11 C35 1.445(8) . ? N12 C41 1.349(8) . ? N12 C38 1.382(6) . ? N13 C41 1.373(6) . ? N13 C42 1.428(7) . ? N14 C48 1.386(7) . ? N14 C47 1.388(7) . ? N15 C48 1.320(7) . ? N15 C49 1.455(6) . ? N16 C55 1.346(6) . ? N16 C54 1.457(6) . ? N17 C56 1.381(7) . ? N17 C55 1.383(7) . ? N18 C62 1.335(7) . ? N18 C61 1.408(6) . ? N19 C63 1.375(7) . ? N19 C62 1.389(7) . ? N20 C66 1.464(7) . ? N21 C88 1.495(7) . ? N21 C80 1.499(8) . ? N21 C81 1.517(8) . ? N21 C89 1.528(7) . ? N22 C97 1.472(7) . ? N22 C104 1.493(7) . ? N22 C105 1.497(8) . ? N22 C96 1.522(7) . ? N23 C121 1.498(7) . ? N23 C120 1.511(7) . ? N23 C113 1.512(6) . ? N23 C112 1.537(7) . ? N24 C137 1.476(10) . ? N24 C129 1.484(10) . ? N24 C128 1.502(10) . ? N24 C136 1.528(8) . ? C1 C2 1.357(9) . ? C1 C6 1.365(9) . ? C2 C3 1.375(7) . ? C3 C4 1.394(8) . ? C4 C5 1.383(9) . ? C5 C6 1.406(7) . ? C8 C9 1.378(8) . ? C8 C13 1.415(8) . ? C9 C10 1.358(9) . ? C10 C11 1.376(10) . ? C11 C12 1.350(9) . ? C12 C13 1.369(8) . ? C15 C20 1.514(9) . ? C15 C16 1.527(8) . ? C16 C17 1.502(10) . ? C17 C18 1.504(11) . ? C18 C19 1.504(10) . ? C19 C20 1.522(9) . ? C22 C23 1.394(7) . ? C22 C27 1.414(8) . ? C23 C24 1.370(9) . ? C24 C25 1.374(9) . ? C25 C26 1.379(9) . ? C26 C27 1.355(9) . ? C29 C34 1.359(9) . ? C29 C30 1.403(8) . ? C30 C31 1.354(7) . ? C31 C32 1.355(8) . ? C32 C33 1.353(9) . ? C33 C34 1.384(7) . ? C35 C40 1.357(10) . ? C35 C36 1.358(9) . ? C36 C37 1.355(8) . ? C37 C38 1.365(9) . ? C38 C39 1.410(8) . ? C39 C40 1.373(8) . ? C42 C43 1.384(8) . ? C42 C47 1.399(8) . ? C43 C44 1.388(9) . ? C44 C45 1.382(9) . ? C45 C46 1.365(8) . ? C46 C47 1.396(8) . ? C49 C54 1.487(8) . ? C49 C50 1.549(7) . ? C50 C51 1.544(8) . ? C51 C52 1.489(9) . ? C52 C53 1.519(8) . ? C53 C54 1.533(7) . ? C56 C57 1.375(7) . ? C56 C61 1.420(7) . ? C57 C58 1.371(8) . ? C58 C59 1.365(8) . ? C59 C60 1.377(8) . ? C60 C61 1.356(8) . ? C63 C68 1.391(8) . ? C63 C64 1.400(8) . ? C64 C65 1.372(7) . ? C65 C66 1.404(9) . ? C66 C67 1.361(8) . ? C67 C68 1.378(7) . ? C69 C72 1.449(16) . ? C70 C71 1.358(18) . ? C71 C72 1.400(18) . ? C73 C74 1.28(4) . ? C73 C75 2.02(2) . ? C74 C75 1.39(2) . ? C75 C76 1.38(2) . ? C77 C78 1.412(12) . ? C78 C79 1.536(11) . ? C79 C80 1.517(9) . ? C81 C82 1.499(9) . ? C82 C83 1.454(9) . ? C83 C84 1.497(9) . ? C85 C86 1.514(8) . ? C86 C87 1.499(9) . ? C87 C88 1.511(8) . ? C89 C90 1.565(9) . ? C90 C91 1.714(16) . ? C91 C92 1.323(18) . ? C93 C94 1.496(9) . ? C94 C95 1.526(7) . ? C95 C96 1.524(9) . ? C97 C98 1.510(9) . ? C98 C99 1.548(9) . ? C99 C100 1.523(11) . ? C101 C102 1.320(17) . ? C102 C103 1.598(11) . ? C103 C104 1.478(10) . ? C105 C106 1.490(8) . ? C106 C107 1.520(9) . ? C107 C108 1.528(9) . ? C109 C110 1.488(9) . ? C110 C111 1.494(9) . ? C111 C112 1.466(8) . ? C113 C114 1.515(8) . ? C114 C115 1.520(7) . ? C115 C116 1.504(8) . ? C117 C118 1.534(9) . ? C118 C119 1.518(9) . ? C119 C120 1.506(9) . ? C121 C122 1.500(8) . ? C122 C123 1.494(9) . ? C123 C124 1.516(9) . ? C125 C126 1.37(2) . ? C126 C127 1.501(11) . ? C127 C128 1.488(13) . ? C129 C130 1.496(12) . ? C130 C131 1.527(13) . ? C131 C132 1.514(13) . ? C133 C134 1.463(10) . ? C134 C135 1.498(10) . ? C135 C136 1.489(9) . ? C137 C138 1.493(11) . ? C138 C139 1.81(3) . ? C139 C140 1.36(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O19 P1 O17 110.4(2) . . ? O19 P1 O18 113.2(2) . . ? O17 P1 O18 114.0(2) . . ? O19 P1 O20 104.28(18) . . ? O17 P1 O20 106.9(2) . . ? O18 P1 O20 107.2(2) . . ? O24 P2 O22 111.6(2) . . ? O24 P2 O21 113.3(2) . . ? O22 P2 O21 110.8(2) . . ? O24 P2 O23 108.6(2) . . ? O22 P2 O23 104.3(2) . . ? O21 P2 O23 107.7(2) . . ? C73 O27 C76 102(3) . . ? C70 O28 C69 102.2(12) . . ? O2 N1 O1 122.1(6) . . ? O2 N1 C1 118.9(6) . . ? O1 N1 C1 118.9(7) . . ? C4 N2 C7 125.6(5) . . ? C7 N3 C8 126.2(5) . . ? C14 N4 C13 126.0(4) . . ? C14 N5 C15 122.8(4) . . ? C21 N6 C20 121.4(4) . . ? C22 N7 C21 127.3(4) . . ? C28 N8 C27 122.8(5) . . ? C28 N9 C29 125.6(5) . . ? O8 N10 O7 123.2(5) . . ? O8 N10 C32 120.1(6) . . ? O7 N10 C32 116.7(6) . . ? O9 N11 O10 122.8(6) . . ? O9 N11 C35 118.7(7) . . ? O10 N11 C35 118.5(8) . . ? C41 N12 C38 127.2(5) . . ? C41 N13 C42 125.2(5) . . ? C48 N14 C47 126.7(4) . . ? C48 N15 C49 120.4(4) . . ? C55 N16 C54 122.4(4) . . ? C56 N17 C55 127.9(4) . . ? C62 N18 C61 123.2(5) . . ? C63 N19 C62 124.6(5) . . ? O16 N20 O15 124.3(5) . . ? O16 N20 C66 119.6(6) . . ? O15 N20 C66 116.1(6) . . ? C88 N21 C80 111.5(4) . . ? C88 N21 C81 111.4(4) . . ? C80 N21 C81 108.1(5) . . ? C88 N21 C89 106.2(5) . . ? C80 N21 C89 110.5(4) . . ? C81 N21 C89 109.2(4) . . ? C97 N22 C104 111.9(5) . . ? C97 N22 C105 111.8(5) . . ? C104 N22 C105 105.9(4) . . ? C97 N22 C96 105.1(4) . . ? C104 N22 C96 111.6(4) . . ? C105 N22 C96 110.7(5) . . ? C121 N23 C120 106.8(4) . . ? C121 N23 C113 111.9(5) . . ? C120 N23 C113 111.1(4) . . ? C121 N23 C112 111.0(4) . . ? C120 N23 C112 110.3(5) . . ? C113 N23 C112 105.8(4) . . ? C137 N24 C129 110.2(6) . . ? C137 N24 C128 111.7(7) . . ? C129 N24 C128 106.9(7) . . ? C137 N24 C136 106.8(6) . . ? C129 N24 C136 111.8(6) . . ? C128 N24 C136 109.5(6) . . ? C2 C1 C6 122.0(5) . . ? C2 C1 N1 118.9(6) . . ? C6 C1 N1 119.1(6) . . ? C1 C2 C3 119.7(6) . . ? C2 C3 C4 120.2(6) . . ? N2 C4 C5 115.4(5) . . ? N2 C4 C3 125.0(5) . . ? C5 C4 C3 119.6(5) . . ? C4 C5 C6 119.3(6) . . ? C1 C6 C5 119.2(6) . . ? O3 C7 N3 124.8(6) . . ? O3 C7 N2 124.0(5) . . ? N3 C7 N2 111.1(5) . . ? C9 C8 N3 122.1(5) . . ? C9 C8 C13 119.7(5) . . ? N3 C8 C13 118.2(5) . . ? C10 C9 C8 119.7(6) . . ? C9 C10 C11 120.6(7) . . ? C12 C11 C10 120.3(6) . . ? C11 C12 C13 121.2(6) . . ? C12 C13 N4 123.1(5) . . ? C12 C13 C8 118.4(6) . . ? N4 C13 C8 118.4(5) . . ? O4 C14 N5 124.2(5) . . ? O4 C14 N4 123.0(6) . . ? N5 C14 N4 112.8(4) . . ? N5 C15 C20 113.1(5) . . ? N5 C15 C16 113.4(6) . . ? C20 C15 C16 110.9(5) . . ? C17 C16 C15 110.8(7) . . ? C16 C17 C18 111.2(6) . . ? C17 C18 C19 110.6(6) . . ? C18 C19 C20 111.4(7) . . ? N6 C20 C15 109.2(4) . . ? N6 C20 C19 111.1(6) . . ? C15 C20 C19 111.2(5) . . ? O5 C21 N6 123.6(5) . . ? O5 C21 N7 123.0(6) . . ? N6 C21 N7 113.3(4) . . ? N7 C22 C23 122.7(5) . . ? N7 C22 C27 120.4(5) . . ? C23 C22 C27 116.8(6) . . ? C24 C23 C22 120.7(6) . . ? C23 C24 C25 121.3(6) . . ? C24 C25 C26 119.1(6) . . ? C27 C26 C25 120.3(6) . . ? C26 C27 C22 121.8(5) . . ? C26 C27 N8 121.1(5) . . ? C22 C27 N8 117.2(5) . . ? O6 C28 N8 124.6(6) . . ? O6 C28 N9 121.0(5) . . ? N8 C28 N9 114.3(6) . . ? C34 C29 N9 119.0(5) . . ? C34 C29 C30 119.0(5) . . ? N9 C29 C30 121.8(5) . . ? C31 C30 C29 119.7(6) . . ? C30 C31 C32 120.6(6) . . ? C33 C32 C31 120.6(5) . . ? C33 C32 N10 120.8(6) . . ? C31 C32 N10 118.5(6) . . ? C32 C33 C34 119.9(6) . . ? C29 C34 C33 120.0(6) . . ? C40 C35 C36 122.3(6) . . ? C40 C35 N11 117.7(6) . . ? C36 C35 N11 119.8(7) . . ? C37 C36 C35 118.4(7) . . ? C36 C37 C38 122.3(6) . . ? C37 C38 N12 117.4(5) . . ? C37 C38 C39 118.2(5) . . ? N12 C38 C39 124.4(6) . . ? C40 C39 C38 119.5(6) . . ? C35 C40 C39 119.2(6) . . ? O11 C41 N12 124.2(5) . . ? O11 C41 N13 124.7(6) . . ? N12 C41 N13 111.0(5) . . ? C43 C42 C47 120.5(5) . . ? C43 C42 N13 121.1(5) . . ? C47 C42 N13 118.5(5) . . ? C42 C43 C44 120.7(6) . . ? C45 C44 C43 118.9(6) . . ? C46 C45 C44 120.4(6) . . ? C45 C46 C47 121.9(6) . . ? N14 C47 C46 122.6(5) . . ? N14 C47 C42 119.9(5) . . ? C46 C47 C42 117.5(5) . . ? O12 C48 N15 123.7(5) . . ? O12 C48 N14 122.1(5) . . ? N15 C48 N14 114.2(4) . . ? N15 C49 C54 110.5(4) . . ? N15 C49 C50 111.1(5) . . ? C54 C49 C50 109.8(4) . . ? C51 C50 C49 110.3(5) . . ? C52 C51 C50 110.7(5) . . ? C51 C52 C53 111.5(5) . . ? C52 C53 C54 110.7(5) . . ? N16 C54 C49 114.1(4) . . ? N16 C54 C53 111.5(5) . . ? C49 C54 C53 111.4(4) . . ? O13 C55 N16 125.2(5) . . ? O13 C55 N17 124.0(5) . . ? N16 C55 N17 110.8(4) . . ? C57 C56 N17 124.5(5) . . ? C57 C56 C61 118.4(5) . . ? N17 C56 C61 117.0(4) . . ? C58 C57 C56 120.8(5) . . ? C59 C58 C57 121.1(5) . . ? C58 C59 C60 118.4(6) . . ? C61 C60 C59 122.5(5) . . ? C60 C61 N18 123.6(5) . . ? C60 C61 C56 118.7(5) . . ? N18 C61 C56 117.6(5) . . ? O14 C62 N18 125.3(5) . . ? O14 C62 N19 122.6(5) . . ? N18 C62 N19 112.1(6) . . ? N19 C63 C68 123.9(5) . . ? N19 C63 C64 117.9(5) . . ? C68 C63 C64 118.1(5) . . ? C65 C64 C63 121.1(6) . . ? C64 C65 C66 118.3(5) . . ? C67 C66 C65 122.1(5) . . ? C67 C66 N20 119.9(6) . . ? C65 C66 N20 117.9(6) . . ? C66 C67 C68 118.5(5) . . ? C67 C68 C63 121.9(5) . . ? C72 C69 O28 101.5(11) . . ? O28 C70 C71 112.1(12) . . ? C70 C71 C72 110.3(10) . . ? C71 C72 C69 106.1(13) . . ? O27 C73 C74 117(3) . . ? O27 C73 C75 74(2) . . ? C74 C73 C75 42.8(9) . . ? C73 C74 C75 98.3(18) . . ? C76 C75 C74 97.6(16) . . ? C76 C75 C73 62.3(12) . . ? C74 C75 C73 38.9(15) . . ? O27 C76 C75 97(2) . . ? C77 C78 C79 116.1(7) . . ? C80 C79 C78 110.8(6) . . ? N21 C80 C79 116.2(5) . . ? C82 C81 N21 116.6(6) . . ? C83 C82 C81 113.4(7) . . ? C82 C83 C84 111.8(6) . . ? C87 C86 C85 114.1(6) . . ? C86 C87 C88 111.7(5) . . ? N21 C88 C87 114.8(5) . . ? N21 C89 C90 111.6(6) . . ? C89 C90 C91 103.1(6) . . ? C92 C91 C90 100.5(13) . . ? C93 C94 C95 113.4(5) . . ? C96 C95 C94 108.9(5) . . ? N22 C96 C95 116.3(5) . . ? N22 C97 C98 115.3(5) . . ? C97 C98 C99 109.4(6) . . ? C100 C99 C98 110.9(7) . . ? C101 C102 C103 114.0(10) . . ? C104 C103 C102 106.9(6) . . ? C103 C104 N22 116.0(5) . . ? C106 C105 N22 115.2(4) . . ? C105 C106 C107 110.4(5) . . ? C106 C107 C108 111.9(5) . . ? C109 C110 C111 112.9(6) . . ? C112 C111 C110 108.9(5) . . ? C111 C112 N23 115.2(5) . . ? N23 C113 C114 116.7(4) . . ? C113 C114 C115 108.1(5) . . ? C116 C115 C114 113.4(5) . . ? C119 C118 C117 114.9(6) . . ? C120 C119 C118 110.9(5) . . ? C119 C120 N23 116.9(5) . . ? N23 C121 C122 115.5(4) . . ? C123 C122 C121 111.2(5) . . ? C122 C123 C124 112.7(5) . . ? C125 C126 C127 116.9(13) . . ? C128 C127 C126 111.0(10) . . ? C127 C128 N24 116.9(8) . . ? N24 C129 C130 115.8(7) . . ? C129 C130 C131 109.7(8) . . ? C132 C131 C130 113.5(9) . . ? C133 C134 C135 111.9(7) . . ? C136 C135 C134 109.9(6) . . ? C135 C136 N24 116.3(6) . . ? N24 C137 C138 113.5(7) . . ? C137 C138 C139 105.0(9) . . ? C140 C139 C138 79.9(17) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 O22 0.88 1.84 2.694(6) 163.3 . N3 H3 O22 0.88 2.21 2.999(6) 148.3 . N4 H4 O21 0.88 2.04 2.868(6) 155.7 . N5 H5A O21 0.88 2.24 2.910(5) 132.5 . N6 H6A O24 0.88 2.02 2.827(5) 152.5 . N7 H7 O24 0.88 2.08 2.893(5) 152.2 . N8 H8 O22 0.88 1.92 2.787(7) 167.4 . N9 H9A O23 0.88 2.15 2.997(7) 161.6 . N12 H12A O19 0.88 1.84 2.685(6) 161.6 . N13 H13 O19 0.88 2.12 2.909(6) 148.4 . N14 H14 O18 0.88 2.15 2.954(6) 151.3 . N15 H15A O18 0.88 2.07 2.839(5) 146.1 . N16 H16 O17 0.88 2.14 2.884(5) 141.5 . N17 H17 O17 0.88 2.02 2.852(5) 157.6 . N18 H18 O19 0.88 2.02 2.898(7) 173.7 . N19 H19 O17 0.88 2.30 3.083(6) 148.7 . N19 H19 O20 0.88 2.54 3.324(7) 149.2 . O20 H201 O21 0.86 1.84 2.640(5) 154.6 . O23 H231 O18 1.10 1.97 2.604(6) 113.1 . O25 H251 O20 1.08 1.90 2.946(6) 160.7 . O25 H252 O24 1.10 1.92 2.712(6) 125.6 . O26 H261 O17 0.71 2.07 2.729(6) 156.7 . O26 H262 O21 0.68 2.24 2.900(7) 163.7 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.27 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.559 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.062 data_SO4 _database_code_depnum_ccdc_archive 'CCDC 895442' #TrackingRef 'cyclohexyl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C134 H217 N24 O25 S3' _chemical_formula_weight 2660.50 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 12.821(3) _cell_length_b 16.131(4) _cell_length_c 19.300(4) _cell_angle_alpha 77.453(2) _cell_angle_beta 77.365(3) _cell_angle_gamma 87.544(3) _cell_volume 3801.9(15) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7430 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 28.30 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1437 _exptl_absorpt_coefficient_mu 0.120 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9536 _exptl_absorpt_correction_T_max 0.9764 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.129 0.264 0.471 326 75 ' ' 2 0.833 0.025 0.479 7 0 ' ' _platon_squeeze_details ; ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25180 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0789 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total 20732 _reflns_number_gt 15493 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1573P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(9) _refine_ls_number_reflns 20732 _refine_ls_number_parameters 1693 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.2394 _refine_ls_wR_factor_gt 0.2172 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 S1 S 0.23125(10) 0.62170(8) 0.83184(6) 0.0250(3) Uani 1 1 d . . . S2 S 0.37014(10) 0.99498(8) 0.04623(7) 0.0267(3) Uani 1 1 d . . . S3 S 0.6014(2) 0.4836(2) 0.30222(14) 0.0874(8) Uani 1 1 d . . . O1 O 0.0058(5) 0.9094(4) 1.1999(3) 0.0710(17) Uani 1 1 d . . . O2 O 0.1345(4) 0.8198(3) 1.2124(2) 0.0532(13) Uani 1 1 d . . . O3 O -0.0173(3) 0.8904(3) 0.8572(2) 0.0400(11) Uani 1 1 d . . . O4 O 0.1984(4) 0.7169(4) 0.5628(2) 0.0630(16) Uani 1 1 d . . . O5 O 0.1814(5) 0.4441(4) 0.6280(3) 0.0758(18) Uani 1 1 d . . . O6 O -0.0222(3) 0.3666(2) 0.9961(2) 0.0353(10) Uani 1 1 d . . . O7 O -0.0314(5) 0.6333(4) 1.2740(3) 0.0656(15) Uani 1 1 d . . . O8 O -0.1419(4) 0.5259(4) 1.3096(3) 0.0686(16) Uani 1 1 d . . . O9 O 0.7143(6) 1.1323(5) -0.4321(3) 0.097(2) Uani 1 1 d . . . O10 O 0.6277(6) 1.0135(5) -0.3972(3) 0.094(3) Uani 1 1 d . . . O11 O 0.6062(3) 1.2608(3) -0.1042(2) 0.0362(10) Uani 1 1 d . . . O12 O 0.3702(4) 1.1679(3) 0.2548(2) 0.0516(12) Uani 1 1 d . . . O13 O 0.4562(4) 0.9138(4) 0.3137(3) 0.0670(16) Uani 1 1 d . . . O14 O 0.6270(4) 0.7316(3) 0.0188(2) 0.0423(11) Uani 1 1 d . . . O15 O 0.6530(6) 0.7258(4) -0.3315(3) 0.0791(19) Uani 1 1 d . . . O16 O 0.5044(5) 0.7940(4) -0.3435(3) 0.0625(15) Uani 1 1 d . . . O17 O 0.2228(3) 0.6179(2) 0.90991(19) 0.0277(9) Uani 1 1 d . . . O18 O 0.1214(3) 0.6137(2) 0.81984(19) 0.0284(9) Uani 1 1 d . . . O19 O 0.2961(3) 0.5504(3) 0.8086(2) 0.0336(9) Uani 1 1 d . . . O20 O 0.2755(3) 0.7039(2) 0.78956(19) 0.0313(9) Uani 1 1 d . . . O21 O 0.4828(3) 1.0030(2) 0.0528(2) 0.0339(10) Uani 1 1 d . . . O22 O 0.3723(3) 0.9753(3) -0.02541(19) 0.0382(11) Uani 1 1 d . . . O23 O 0.3168(3) 1.0761(3) 0.0515(2) 0.0324(9) Uani 1 1 d . . . O24 O 0.3178(3) 0.9263(3) 0.1059(2) 0.0374(10) Uani 1 1 d . . . O25 O 0.4590(11) 0.4893(14) 0.3152(8) 0.264(11) Uani 1 1 d . . . N1 N 0.0712(5) 0.8580(3) 1.1781(3) 0.0467(15) Uani 1 1 d . . . N2 N 0.0764(4) 0.7780(3) 0.9076(2) 0.0304(11) Uani 1 1 d . . . H2A H 0.1130 0.7323 0.8996 0.036 Uiso 1 1 calc R . . N3 N 0.0336(4) 0.7784(3) 0.7988(2) 0.0313(11) Uani 1 1 d . . . H3A H 0.0604 0.7269 0.8042 0.038 Uiso 1 1 calc R . . N4 N 0.1629(4) 0.7629(3) 0.6703(3) 0.0372(12) Uani 1 1 d . . . H4 H 0.1880 0.7628 0.7093 0.045 Uiso 1 1 calc R . . N5 N 0.3200(4) 0.6943(3) 0.6394(2) 0.0339(12) Uani 1 1 d . . . H5A H 0.3349 0.7076 0.6781 0.041 Uiso 1 1 calc R . . N6 N 0.2961(4) 0.5165(3) 0.6690(3) 0.0439(14) Uani 1 1 d . . . H6A H 0.3184 0.5246 0.7070 0.053 Uiso 1 1 calc R . . N7 N 0.1632(4) 0.4351(3) 0.7504(3) 0.0372(12) Uani 1 1 d . . . H7 H 0.1976 0.4430 0.7832 0.045 Uiso 1 1 calc R . . N8 N 0.0420(4) 0.4502(3) 0.8841(2) 0.0278(11) Uani 1 1 d . . . H8 H 0.0811 0.4953 0.8605 0.033 Uiso 1 1 calc R . . N9 N 0.0599(3) 0.4922(3) 0.9884(2) 0.0241(10) Uani 1 1 d . . . H9A H 0.1086 0.5276 0.9587 0.029 Uiso 1 1 calc R . . N10 N -0.0712(5) 0.5674(4) 1.2636(3) 0.0520(16) Uani 1 1 d . . . N11 N 0.6591(6) 1.0779(6) -0.3851(3) 0.074(2) Uani 1 1 d . . . N12 N 0.5434(4) 1.1279(3) -0.0991(3) 0.0316(11) Uani 1 1 d . . . H12A H 0.5021 1.0873 -0.0691 0.038 Uiso 1 1 calc R . . N13 N 0.5604(4) 1.1661(3) 0.0044(3) 0.0337(12) Uani 1 1 d . . . H13 H 0.5343 1.1150 0.0254 0.040 Uiso 1 1 calc R . . N14 N 0.4161(4) 1.1816(3) 0.1295(2) 0.0334(11) Uani 1 1 d . . . H14 H 0.3948 1.1708 0.0920 0.040 Uiso 1 1 calc R . . N15 N 0.2671(4) 1.1092(4) 0.1953(3) 0.0406(13) Uani 1 1 d . . . H22F H 0.2515 1.1118 0.1527 0.049 Uiso 1 1 calc R . . N16 N 0.3219(4) 0.9372(3) 0.2519(3) 0.0387(12) Uani 1 1 d . . . H16 H 0.2985 0.9294 0.2142 0.046 Uiso 1 1 calc R . . N17 N 0.4677(4) 0.8644(4) 0.2086(3) 0.0394(13) Uani 1 1 d . . . H17 H 0.4349 0.8649 0.1729 0.047 Uiso 1 1 calc R . . N18 N 0.5761(4) 0.8401(3) 0.0750(2) 0.0304(11) Uani 1 1 d . . . H25B H 0.5412 0.8885 0.0725 0.036 Uiso 1 1 calc R . . N19 N 0.5323(4) 0.8408(3) -0.0337(2) 0.0307(11) Uani 1 1 d . . . H19 H 0.4907 0.8841 -0.0258 0.037 Uiso 1 1 calc R . . N20 N 0.5730(5) 0.7662(4) -0.3088(3) 0.0508(16) Uani 1 1 d . . . N21 N 0.9544(6) 0.6274(5) 0.4918(3) 0.0636(18) Uani 1 1 d . . . N22 N 0.5088(4) 0.5076(3) 0.9543(2) 0.0285(11) Uani 1 1 d . . . N23 N 0.5966(6) 0.1223(4) 0.3778(3) 0.0632(18) Uani 1 1 d . . . N24 N 0.1020(4) 0.1139(3) 0.9155(3) 0.0366(12) Uani 1 1 d . . . C1 C 0.0722(5) 0.8424(4) 1.1063(3) 0.0338(14) Uani 1 1 d . . . C2 C 0.1652(5) 0.8061(4) 1.0702(3) 0.0310(13) Uani 1 1 d . . . H2 H 0.2265 0.7950 1.0909 0.037 Uiso 1 1 calc R . . C3 C 0.1640(5) 0.7876(4) 1.0044(3) 0.0301(13) Uani 1 1 d . . . H3 H 0.2264 0.7648 0.9788 0.036 Uiso 1 1 calc R . . C4 C 0.0747(5) 0.8012(4) 0.9742(3) 0.0320(14) Uani 1 1 d . . . C5 C -0.0184(5) 0.8381(4) 1.0109(3) 0.0363(15) Uani 1 1 d . . . H5 H -0.0801 0.8495 0.9906 0.044 Uiso 1 1 calc R . . C6 C -0.0153(5) 0.8563(4) 1.0766(3) 0.0371(15) Uani 1 1 d . . . H6 H -0.0770 0.8797 1.1024 0.045 Uiso 1 1 calc R . . C7 C 0.0262(5) 0.8199(4) 0.8540(3) 0.0339(14) Uani 1 1 d . . . C8 C 0.0002(5) 0.8139(4) 0.7328(3) 0.0344(14) Uani 1 1 d . . . C9 C -0.0961(5) 0.8573(4) 0.7318(3) 0.0410(16) Uani 1 1 d . . . H9 H -0.1392 0.8667 0.7761 0.049 Uiso 1 1 calc R . . C10 C -0.1302(6) 0.8871(6) 0.6677(4) 0.068(3) Uani 1 1 d . . . H10 H -0.1966 0.9158 0.6684 0.082 Uiso 1 1 calc R . . C11 C -0.0699(6) 0.8755(7) 0.6049(4) 0.073(3) Uani 1 1 d . . . H11 H -0.0931 0.8965 0.5608 0.088 Uiso 1 1 calc R . . C12 C 0.0276(6) 0.8323(6) 0.6036(4) 0.059(2) Uani 1 1 d . . . H12 H 0.0692 0.8230 0.5588 0.070 Uiso 1 1 calc R . . C13 C 0.0639(5) 0.8029(5) 0.6674(3) 0.0424(16) Uani 1 1 d . . . C14 C 0.2245(5) 0.7242(5) 0.6194(3) 0.0454(17) Uani 1 1 d . . . C15 C 0.3958(5) 0.6428(4) 0.6000(3) 0.0383(15) Uani 1 1 d . . . H15 H 0.4523 0.6264 0.6288 0.046 Uiso 1 1 calc R . . C16 C 0.4537(5) 0.6926(5) 0.5243(3) 0.0506(19) Uani 1 1 d . . . H23B H 0.4009 0.7121 0.4938 0.061 Uiso 1 1 calc R . . H16B H 0.4893 0.7434 0.5298 0.061 Uiso 1 1 calc R . . C17 C 0.5363(6) 0.6368(5) 0.4874(3) 0.058(2) Uani 1 1 d . . . H24B H 0.5680 0.6685 0.4377 0.070 Uiso 1 1 calc R . . H17B H 0.5944 0.6249 0.5145 0.070 Uiso 1 1 calc R . . C18 C 0.4928(7) 0.5544(5) 0.4824(4) 0.071(3) Uani 1 1 d . . . H18 H 0.4985 0.5348 0.4387 0.085 Uiso 1 1 calc R . . C19 C 0.4374(7) 0.5060(5) 0.5582(4) 0.058(2) Uani 1 1 d . . . H26B H 0.4909 0.4904 0.5888 0.069 Uiso 1 1 calc R . . H19B H 0.4053 0.4530 0.5542 0.069 Uiso 1 1 calc R . . C20 C 0.3496(5) 0.5609(4) 0.5943(3) 0.0430(15) Uani 1 1 d . . . H20 H 0.2947 0.5744 0.5639 0.052 Uiso 1 1 calc R . . C21 C 0.2143(5) 0.4644(5) 0.6776(4) 0.0466(17) Uani 1 1 d . . . C22 C 0.0644(5) 0.3948(4) 0.7766(3) 0.0331(14) Uani 1 1 d . . . C23 C 0.0259(5) 0.3449(4) 0.7353(3) 0.0394(15) Uani 1 1 d . . . H23 H 0.0697 0.3362 0.6910 0.047 Uiso 1 1 calc R . . C24 C -0.0744(5) 0.3090(4) 0.7590(3) 0.0395(15) Uani 1 1 d . . . H24 H -0.1008 0.2772 0.7305 0.047 Uiso 1 1 calc R . . C25 C -0.1386(5) 0.3199(4) 0.8264(4) 0.0410(15) Uani 1 1 d . . . H25 H -0.2082 0.2957 0.8432 0.049 Uiso 1 1 calc R . . C26 C -0.0987(5) 0.3655(3) 0.8667(3) 0.0320(13) Uani 1 1 d . . . H26 H -0.1419 0.3730 0.9117 0.038 Uiso 1 1 calc R . . C27 C 0.0026(4) 0.4011(4) 0.8442(3) 0.0294(13) Uani 1 1 d . . . C28 C 0.0222(4) 0.4308(4) 0.9597(3) 0.0279(13) Uani 1 1 d . . . C29 C 0.0290(4) 0.5035(4) 1.0588(3) 0.0275(13) Uani 1 1 d . . . C30 C -0.0488(5) 0.4548(4) 1.1125(3) 0.0331(13) Uani 1 1 d . . . H30 H -0.0809 0.4075 1.1032 0.040 Uiso 1 1 calc R . . C31 C -0.0793(5) 0.4773(4) 1.1817(3) 0.0402(16) Uani 1 1 d . . . H31 H -0.1301 0.4434 1.2193 0.048 Uiso 1 1 calc R . . C32 C -0.0363(5) 0.5469(4) 1.1942(3) 0.0351(14) Uani 1 1 d . . . C33 C 0.0430(5) 0.5955(4) 1.1403(3) 0.0389(15) Uani 1 1 d . . . H33 H 0.0753 0.6429 1.1494 0.047 Uiso 1 1 calc R . . C34 C 0.0722(5) 0.5731(4) 1.0747(3) 0.0307(13) Uani 1 1 d . . . H34 H 0.1247 0.6066 1.0380 0.037 Uiso 1 1 calc R . . C35 C 0.6260(6) 1.0960(5) -0.3117(3) 0.0465(18) Uani 1 1 d . . . C36 C 0.6643(6) 1.1656(5) -0.2948(4) 0.0501(18) Uani 1 1 d . . . H36 H 0.7117 1.2033 -0.3318 0.060 Uiso 1 1 calc R . . C37 C 0.6373(5) 1.1827(4) -0.2272(3) 0.0407(16) Uani 1 1 d . . . H37 H 0.6616 1.2328 -0.2172 0.049 Uiso 1 1 calc R . . C38 C 0.5696(4) 1.1212(4) -0.1709(3) 0.0301(13) Uani 1 1 d . . . C39 C 0.5307(5) 1.0514(4) -0.1893(3) 0.0389(16) Uani 1 1 d . . . H39 H 0.4844 1.0125 -0.1526 0.047 Uiso 1 1 calc R . . C40 C 0.5572(5) 1.0370(5) -0.2587(3) 0.0419(16) Uani 1 1 d . . . H40 H 0.5301 0.9891 -0.2704 0.050 Uiso 1 1 calc R . . C41 C 0.5738(4) 1.1902(3) -0.0682(3) 0.0263(12) Uani 1 1 d . . . C42 C 0.5859(4) 1.2180(3) 0.0488(3) 0.0258(12) Uani 1 1 d . . . C43 C 0.6849(5) 1.2599(4) 0.0310(4) 0.0407(16) Uani 1 1 d . . . H43 H 0.7344 1.2550 -0.0125 0.049 Uiso 1 1 calc R . . C44 C 0.7120(6) 1.3088(4) 0.0761(4) 0.0442(17) Uani 1 1 d . . . H44 H 0.7797 1.3360 0.0647 0.053 Uiso 1 1 calc R . . C45 C 0.6364(6) 1.3163(4) 0.1386(4) 0.0465(17) Uani 1 1 d . . . H45 H 0.6532 1.3507 0.1689 0.056 Uiso 1 1 calc R . . C46 C 0.5392(6) 1.2763(4) 0.1578(3) 0.0408(15) Uani 1 1 d . . . H46 H 0.4901 1.2823 0.2011 0.049 Uiso 1 1 calc R . . C47 C 0.5131(5) 1.2267(4) 0.1135(3) 0.0322(13) Uani 1 1 d . . . C48 C 0.3497(5) 1.1521(4) 0.1972(3) 0.0389(15) Uani 1 1 d . . . C49 C 0.1987(5) 1.0572(4) 0.2588(3) 0.0417(16) Uani 1 1 d . . . H49 H 0.1460 1.0289 0.2401 0.050 Uiso 1 1 calc R . . C50 C 0.1334(6) 1.1097(5) 0.3095(4) 0.055(2) Uani 1 1 d . . . H50A H 0.0948 1.1548 0.2816 0.066 Uiso 1 1 calc R . . H50B H 0.1817 1.1373 0.3314 0.066 Uiso 1 1 calc R . . C51 C 0.0524(8) 1.0521(6) 0.3701(5) 0.081(3) Uani 1 1 d . . . H51A H 0.0014 1.0273 0.3483 0.098 Uiso 1 1 calc R . . H51B H 0.0114 1.0862 0.4037 0.098 Uiso 1 1 calc R . . C52 C 0.1131(8) 0.9790(5) 0.4133(4) 0.073(3) Uani 1 1 d . . . H52A H 0.1612 1.0034 0.4375 0.088 Uiso 1 1 calc R . . H52B H 0.0610 0.9411 0.4512 0.088 Uiso 1 1 calc R . . C53 C 0.1773(6) 0.9290(4) 0.3611(4) 0.0496(18) Uani 1 1 d . . . H53A H 0.1284 0.9023 0.3390 0.060 Uiso 1 1 calc R . . H53B H 0.2164 0.8832 0.3879 0.060 Uiso 1 1 calc R . . C54 C 0.2560(6) 0.9859(4) 0.3018(3) 0.0466(17) Uani 1 1 d . . . H54 H 0.3046 1.0122 0.3252 0.056 Uiso 1 1 calc R . . C55 C 0.4176(5) 0.9043(5) 0.2626(3) 0.0441(16) Uani 1 1 d . . . C56 C 0.5658(5) 0.8230(5) 0.2049(3) 0.0441(17) Uani 1 1 d . . . C57 C 0.6084(6) 0.7900(6) 0.2667(4) 0.057(2) Uani 1 1 d . . . H57 H 0.5702 0.7949 0.3137 0.069 Uiso 1 1 calc R . . C58 C 0.7072(6) 0.7502(6) 0.2576(5) 0.069(3) Uani 1 1 d . . . H58 H 0.7367 0.7289 0.2990 0.083 Uiso 1 1 calc R . . C59 C 0.7626(5) 0.7407(5) 0.1921(4) 0.0490(18) Uani 1 1 d . . . H59 H 0.8313 0.7153 0.1876 0.059 Uiso 1 1 calc R . . C60 C 0.7191(5) 0.7685(4) 0.1300(4) 0.0412(16) Uani 1 1 d . . . H60 H 0.7561 0.7592 0.0840 0.049 Uiso 1 1 calc R . . C61 C 0.6225(5) 0.8091(4) 0.1372(3) 0.0345(14) Uani 1 1 d . . . C62 C 0.5830(4) 0.7998(3) 0.0212(3) 0.0261(12) Uani 1 1 d . . . C63 C 0.5435(5) 0.8174(3) -0.1004(3) 0.0266(12) Uani 1 1 d . . . C64 C 0.4563(5) 0.8281(3) -0.1331(3) 0.0294(13) Uani 1 1 d . . . H64 H 0.3896 0.8459 -0.1083 0.035 Uiso 1 1 calc R . . C65 C 0.4668(5) 0.8127(4) -0.2021(3) 0.0371(15) Uani 1 1 d . . . H65 H 0.4085 0.8231 -0.2258 0.045 Uiso 1 1 calc R . . C66 C 0.5629(5) 0.7820(4) -0.2368(3) 0.0363(15) Uani 1 1 d . . . C67 C 0.6503(5) 0.7677(4) -0.2017(3) 0.0380(15) Uani 1 1 d . . . H67 H 0.7155 0.7452 -0.2243 0.046 Uiso 1 1 calc R . . C68 C 0.6394(5) 0.7866(4) -0.1360(3) 0.0373(15) Uani 1 1 d . . . H68 H 0.6986 0.7788 -0.1130 0.045 Uiso 1 1 calc R . . C69 C 1.0524(6) 0.6087(5) 0.4323(4) 0.059(2) Uani 1 1 d . . . H69A H 1.0809 0.5521 0.4505 0.070 Uiso 1 1 calc R . . H69B H 1.0263 0.6058 0.3883 0.070 Uiso 1 1 calc R . . C70 C 1.1428(9) 0.6721(6) 0.4108(4) 0.079(3) Uani 1 1 d . . . H70A H 1.1172 0.7278 0.3877 0.095 Uiso 1 1 calc R . . H70B H 1.1660 0.6790 0.4549 0.095 Uiso 1 1 calc R . . C71 C 1.2326(10) 0.6460(13) 0.3611(8) 0.170(8) Uani 1 1 d . . . H71A H 1.2098 0.6424 0.3161 0.204 Uiso 1 1 calc R . . H71B H 1.2544 0.5884 0.3832 0.204 Uiso 1 1 calc R . . C72 C 1.3301(8) 0.7058(5) 0.3411(5) 0.079(3) Uani 1 1 d . . . H72A H 1.3255 0.7493 0.2977 0.119 Uiso 1 1 calc R . . H72B H 1.3958 0.6730 0.3313 0.119 Uiso 1 1 calc R . . H72C H 1.3311 0.7332 0.3816 0.119 Uiso 1 1 calc R . . C73 C 0.9218(9) 0.7212(7) 0.4779(5) 0.088(3) Uani 1 1 d . . . H73A H 0.8589 0.7275 0.5166 0.105 Uiso 1 1 calc R . . H73B H 0.9807 0.7544 0.4846 0.105 Uiso 1 1 calc R . . C74 C 0.8949(10) 0.7629(7) 0.4062(6) 0.094(3) Uani 1 1 d . . . H74A H 0.9608 0.7667 0.3677 0.113 Uiso 1 1 calc R . . H74B H 0.8437 0.7260 0.3951 0.113 Uiso 1 1 calc R . . C75 C 0.8506(11) 0.8449(7) 0.4035(6) 0.103(4) Uani 1 1 d . . . H75A H 0.8384 0.8677 0.3540 0.124 Uiso 1 1 calc R . . H75B H 0.9030 0.8826 0.4123 0.124 Uiso 1 1 calc R . . C76 C 0.7495(9) 0.8473(16) 0.4563(8) 0.182(10) Uani 1 1 d . . . H76A H 0.6903 0.8333 0.4362 0.274 Uiso 1 1 calc R . . H76B H 0.7391 0.9044 0.4665 0.274 Uiso 1 1 calc R . . H76C H 0.7518 0.8060 0.5014 0.274 Uiso 1 1 calc R . . C77 C 0.9926(7) 0.6064(6) 0.5627(4) 0.071(2) Uani 1 1 d . . . H77A H 1.0182 0.5470 0.5703 0.085 Uiso 1 1 calc R . . H77B H 1.0544 0.6436 0.5581 0.085 Uiso 1 1 calc R . . C78 C 0.9130(8) 0.6161(8) 0.6265(4) 0.085(3) Uani 1 1 d . . . H78A H 0.8449 0.5895 0.6264 0.102 Uiso 1 1 calc R . . H78B H 0.9000 0.6771 0.6259 0.102 Uiso 1 1 calc R . . C79 C 0.9505(6) 0.5758(6) 0.6914(4) 0.065(3) Uani 1 1 d . . . H79A H 1.0249 0.5942 0.6867 0.078 Uiso 1 1 calc R . . H79B H 0.9504 0.5134 0.6965 0.078 Uiso 1 1 calc R . . C80 C 0.8782(7) 0.5992(6) 0.7609(6) 0.075(3) Uani 1 1 d . . . H80A H 0.9233 0.6174 0.7899 0.113 Uiso 1 1 calc R . . H80B H 0.8359 0.5495 0.7899 0.113 Uiso 1 1 calc R . . H80C H 0.8301 0.6455 0.7465 0.113 Uiso 1 1 calc R . . C81 C 0.8639(7) 0.5726(7) 0.4911(5) 0.075(3) Uani 1 1 d . . . H81A H 0.7997 0.5870 0.5253 0.090 Uiso 1 1 calc R . . H81B H 0.8483 0.5863 0.4419 0.090 Uiso 1 1 calc R . . C82 C 0.8814(10) 0.4865(10) 0.5096(8) 0.120(5) Uani 1 1 d . . . H82A H 0.8930 0.4715 0.5599 0.144 Uiso 1 1 calc R . . H82B H 0.9468 0.4715 0.4767 0.144 Uiso 1 1 calc R . . C83 C 0.7824(14) 0.4333(6) 0.5041(4) 0.140(7) Uani 1 1 d . . . H83A H 0.7163 0.4574 0.5292 0.168 Uiso 1 1 calc R . . H83B H 0.7794 0.4423 0.4522 0.168 Uiso 1 1 calc R . . C84 C 0.781(2) 0.3362(10) 0.5354(10) 0.218(12) Uani 1 1 d . . . H84A H 0.8438 0.3103 0.5092 0.327 Uiso 1 1 calc R . . H84B H 0.7160 0.3113 0.5297 0.327 Uiso 1 1 calc R . . H84C H 0.7829 0.3256 0.5871 0.327 Uiso 1 1 calc R . . C85 C 0.6150(5) 0.4949(4) 0.9750(3) 0.0347(14) Uani 1 1 d . . . H85A H 0.6494 0.4447 0.9581 0.042 Uiso 1 1 calc R . . H85B H 0.6030 0.4821 1.0287 0.042 Uiso 1 1 calc R . . C86 C 0.6918(5) 0.5699(4) 0.9450(3) 0.0354(14) Uani 1 1 d . . . H86A H 0.6525 0.6232 0.9498 0.043 Uiso 1 1 calc R . . H86B H 0.7216 0.5726 0.8927 0.043 Uiso 1 1 calc R . . C87 C 0.7842(6) 0.5620(5) 0.9857(5) 0.053(2) Uani 1 1 d . . . H87A H 0.7541 0.5579 1.0382 0.064 Uiso 1 1 calc R . . H87B H 0.8241 0.5091 0.9802 0.064 Uiso 1 1 calc R . . C88 C 0.8600(5) 0.6362(4) 0.9580(4) 0.0392(15) Uani 1 1 d . . . H88A H 0.8979 0.6356 0.9081 0.059 Uiso 1 1 calc R . . H88B H 0.9118 0.6322 0.9891 0.059 Uiso 1 1 calc R . . H88C H 0.8197 0.6892 0.9586 0.059 Uiso 1 1 calc R . . C89 C 0.5186(5) 0.5308(4) 0.8723(3) 0.0287(13) Uani 1 1 d . . . H89A H 0.4458 0.5371 0.8623 0.034 Uiso 1 1 calc R . . H89B H 0.5548 0.5867 0.8533 0.034 Uiso 1 1 calc R . . C90 C 0.5795(5) 0.4672(4) 0.8309(3) 0.0418(16) Uani 1 1 d . . . H90A H 0.5438 0.4110 0.8486 0.050 Uiso 1 1 calc R . . H90B H 0.6531 0.4610 0.8393 0.050 Uiso 1 1 calc R . . C91 C 0.5829(6) 0.4980(5) 0.7495(3) 0.0470(17) Uani 1 1 d . . . H91A H 0.5089 0.5027 0.7419 0.056 Uiso 1 1 calc R . . H91B H 0.6155 0.5554 0.7331 0.056 Uiso 1 1 calc R . . C92 C 0.6449(7) 0.4406(6) 0.7039(4) 0.064(2) Uani 1 1 d . . . H92A H 0.7175 0.4337 0.7126 0.096 Uiso 1 1 calc R . . H92B H 0.6480 0.4655 0.6524 0.096 Uiso 1 1 calc R . . H92C H 0.6094 0.3850 0.7168 0.096 Uiso 1 1 calc R . . C93 C 0.4509(5) 0.5819(4) 0.9832(3) 0.0305(13) Uani 1 1 d . . . H93A H 0.4908 0.6346 0.9568 0.037 Uiso 1 1 calc R . . H93B H 0.3794 0.5868 0.9712 0.037 Uiso 1 1 calc R . . C94 C 0.4365(5) 0.5782(4) 1.0616(3) 0.0399(16) Uani 1 1 d . . . H94A H 0.5070 0.5835 1.0734 0.048 Uiso 1 1 calc R . . H94B H 0.4052 0.5225 1.0892 0.048 Uiso 1 1 calc R . . C95 C 0.3641(5) 0.6485(4) 1.0839(3) 0.0407(16) Uani 1 1 d . . . H95A H 0.2910 0.6376 1.0789 0.049 Uiso 1 1 calc R . . H95B H 0.3892 0.7029 1.0503 0.049 Uiso 1 1 calc R . . C96 C 0.3596(8) 0.6574(6) 1.1617(4) 0.069(3) Uani 1 1 d . . . H96A H 0.3416 0.6024 1.1950 0.104 Uiso 1 1 calc R . . H96B H 0.3049 0.6991 1.1746 0.104 Uiso 1 1 calc R . . H96C H 0.4293 0.6766 1.1653 0.104 Uiso 1 1 calc R . . C97 C 0.4467(5) 0.4248(4) 0.9876(3) 0.0302(13) Uani 1 1 d . . . H97A H 0.4873 0.3786 0.9676 0.036 Uiso 1 1 calc R . . H97B H 0.4431 0.4118 1.0406 0.036 Uiso 1 1 calc R . . C98 C 0.3344(5) 0.4242(4) 0.9755(3) 0.0388(15) Uani 1 1 d . . . H98A H 0.3369 0.4300 0.9230 0.047 Uiso 1 1 calc R . . H98B H 0.2945 0.4731 0.9912 0.047 Uiso 1 1 calc R . . C99 C 0.2755(5) 0.3406(4) 1.0185(4) 0.0436(16) Uani 1 1 d . . . H99A H 0.2115 0.3341 0.9992 0.052 Uiso 1 1 calc R . . H99B H 0.3232 0.2919 1.0113 0.052 Uiso 1 1 calc R . . C100 C 0.2410(6) 0.3389(5) 1.1002(4) 0.058(2) Uani 1 1 d . . . H10V H 0.3045 0.3377 1.1208 0.087 Uiso 1 1 calc R . . H10W H 0.1973 0.2882 1.1244 0.087 Uiso 1 1 calc R . . H10U H 0.1991 0.3898 1.1074 0.087 Uiso 1 1 calc R . . C101 C 0.7082(10) 0.1405(8) 0.3848(7) 0.106(5) Uani 1 1 d . . . H10H H 0.7054 0.1415 0.4363 0.128 Uiso 1 1 calc R . . H10I H 0.7544 0.0923 0.3734 0.128 Uiso 1 1 calc R . . C102 C 0.7609(11) 0.2199(9) 0.3393(10) 0.144(6) Uani 1 1 d . . . H10Q H 0.7732 0.2174 0.2873 0.172 Uiso 1 1 calc R . . H10R H 0.7140 0.2689 0.3470 0.172 Uiso 1 1 calc R . . C103 C 0.8625(15) 0.2306(13) 0.3584(16) 0.233(13) Uani 1 1 d . . . H10S H 0.8593 0.1890 0.4049 0.279 Uiso 1 1 calc R . . H10T H 0.9161 0.2081 0.3219 0.279 Uiso 1 1 calc R . . C104 C 0.903(2) 0.2894(14) 0.3659(17) 0.244(14) Uani 1 1 d . . . H10J H 0.9731 0.2983 0.3322 0.365 Uiso 1 1 calc R . . H10K H 0.9130 0.2803 0.4159 0.365 Uiso 1 1 calc R . . H10L H 0.8586 0.3394 0.3558 0.365 Uiso 1 1 calc R . . C105 C 0.5221(10) 0.1944(6) 0.3921(5) 0.085(3) Uani 1 1 d . . . H10A H 0.4518 0.1833 0.3825 0.102 Uiso 1 1 calc R . . H10B H 0.5513 0.2476 0.3583 0.102 Uiso 1 1 calc R . . C106 C 0.5064(10) 0.2061(8) 0.4721(7) 0.105(4) Uani 1 1 d . . . H10F H 0.4882 0.1503 0.5053 0.126 Uiso 1 1 calc R . . H10G H 0.5752 0.2248 0.4791 0.126 Uiso 1 1 calc R . . C107 C 0.4202(14) 0.2697(8) 0.4941(6) 0.167(9) Uani 1 1 d . . . H10M H 0.3561 0.2602 0.4759 0.200 Uiso 1 1 calc R . . H10N H 0.4468 0.3279 0.4704 0.200 Uiso 1 1 calc R . . C108 C 0.3875(13) 0.2626(8) 0.5781(7) 0.133(5) Uani 1 1 d . . . H10C H 0.4163 0.2100 0.6030 0.200 Uiso 1 1 calc R . . H10D H 0.3094 0.2619 0.5934 0.200 Uiso 1 1 calc R . . H10E H 0.4163 0.3114 0.5906 0.200 Uiso 1 1 calc R . . C109 C 0.6000(7) 0.1183(5) 0.2995(4) 0.0548(19) Uani 1 1 d . . . H10O H 0.6191 0.1756 0.2690 0.066 Uiso 1 1 calc R . . H10P H 0.5268 0.1055 0.2958 0.066 Uiso 1 1 calc R . . C110 C 0.6756(6) 0.0549(5) 0.2668(4) 0.0526(18) Uani 1 1 d . . . H11L H 0.6579 -0.0031 0.2964 0.063 Uiso 1 1 calc R . . H11M H 0.7499 0.0680 0.2679 0.063 Uiso 1 1 calc R . . C111 C 0.6674(7) 0.0577(6) 0.1846(4) 0.066(2) Uani 1 1 d . . . H11J H 0.5961 0.0367 0.1843 0.079 Uiso 1 1 calc R . . H11K H 0.6748 0.1172 0.1568 0.079 Uiso 1 1 calc R . . C112 C 0.7479(7) 0.0073(6) 0.1506(5) 0.077(3) Uani 1 1 d . . . H11N H 0.8175 0.0352 0.1411 0.116 Uiso 1 1 calc R . . H11O H 0.7322 0.0007 0.1046 0.116 Uiso 1 1 calc R . . H11P H 0.7494 -0.0487 0.1827 0.116 Uiso 1 1 calc R . . C113 C 0.5591(9) 0.0384(5) 0.4294(5) 0.081(3) Uani 1 1 d . . . H11A H 0.6014 -0.0078 0.4105 0.097 Uiso 1 1 calc R . . H11B H 0.5758 0.0390 0.4770 0.097 Uiso 1 1 calc R . . C114 C 0.4469(13) 0.0178(6) 0.4414(5) 0.114(5) Uani 1 1 d . . . H11C H 0.4284 0.0221 0.3936 0.137 Uiso 1 1 calc R . . H11D H 0.4045 0.0610 0.4648 0.137 Uiso 1 1 calc R . . C115 C 0.414(2) -0.0688(9) 0.4875(9) 0.211(13) Uani 1 1 d . . . H11E H 0.4175 -0.1088 0.4547 0.253 Uiso 1 1 calc R . . H11F H 0.4678 -0.0877 0.5176 0.253 Uiso 1 1 calc R . . C116 C 0.3340(18) -0.075(2) 0.5242(9) 0.33(3) Uani 1 1 d . . . H11G H 0.2793 -0.0590 0.4953 0.501 Uiso 1 1 calc R . . H11H H 0.3295 -0.0364 0.5579 0.501 Uiso 1 1 calc R . . H11I H 0.3221 -0.1332 0.5517 0.501 Uiso 1 1 calc R . . C117 C 0.1598(5) 0.0380(4) 0.8909(4) 0.0422(17) Uani 1 1 d . . . H22A H 0.1173 -0.0137 0.9170 0.051 Uiso 1 1 calc R . . H23F H 0.2293 0.0324 0.9058 0.051 Uiso 1 1 calc R . . C118 C 0.1808(6) 0.0404(5) 0.8081(4) 0.0529(19) Uani 1 1 d . . . H22C H 0.1118 0.0375 0.7937 0.063 Uiso 1 1 calc R . . H22D H 0.2161 0.0948 0.7809 0.063 Uiso 1 1 calc R . . C119 C 0.2505(5) -0.0321(5) 0.7886(4) 0.0508(19) Uani 1 1 d . . . H22E H 0.3204 -0.0274 0.8012 0.061 Uiso 1 1 calc R . . H14A H 0.2168 -0.0862 0.8180 0.061 Uiso 1 1 calc R . . C120 C 0.2678(8) -0.0346(6) 0.7129(5) 0.080(3) Uani 1 1 d . . . H12U H 0.1995 -0.0273 0.6975 0.119 Uiso 1 1 calc R . . H12V H 0.2987 -0.0895 0.7056 0.119 Uiso 1 1 calc R . . H12W H 0.3170 0.0112 0.6842 0.119 Uiso 1 1 calc R . . C121 C 0.1649(5) 0.1957(4) 0.8779(4) 0.0380(15) Uani 1 1 d . . . H12H H 0.1638 0.2071 0.8255 0.046 Uiso 1 1 calc R . . H12I H 0.1277 0.2431 0.8979 0.046 Uiso 1 1 calc R . . C122 C 0.2809(5) 0.1954(4) 0.8852(4) 0.0443(17) Uani 1 1 d . . . H12S H 0.2837 0.1908 0.9367 0.053 Uiso 1 1 calc R . . H12T H 0.3184 0.1459 0.8688 0.053 Uiso 1 1 calc R . . C123 C 0.3354(6) 0.2767(4) 0.8396(4) 0.056(2) Uani 1 1 d . . . H12O H 0.4029 0.2830 0.8549 0.067 Uiso 1 1 calc R . . H12P H 0.2890 0.3250 0.8500 0.067 Uiso 1 1 calc R . . C124 C 0.3612(7) 0.2826(6) 0.7574(4) 0.065(2) Uani 1 1 d . . . H18A H 0.4150 0.2401 0.7454 0.098 Uiso 1 1 calc R . . H12B H 0.3890 0.3394 0.7325 0.098 Uiso 1 1 calc R . . H12C H 0.2961 0.2721 0.7418 0.098 Uiso 1 1 calc R . . C125 C -0.0074(5) 0.1268(4) 0.8934(4) 0.0368(15) Uani 1 1 d . . . H12M H -0.0403 0.1792 0.9073 0.044 Uiso 1 1 calc R . . H12N H 0.0046 0.1356 0.8399 0.044 Uiso 1 1 calc R . . C126 C -0.0854(5) 0.0539(4) 0.9275(3) 0.0360(14) Uani 1 1 d . . . H12F H -0.0479 -0.0005 0.9239 0.043 Uiso 1 1 calc R . . H12G H -0.1122 0.0538 0.9797 0.043 Uiso 1 1 calc R . . C127 C -0.1782(5) 0.0606(5) 0.8907(4) 0.0509(19) Uani 1 1 d . . . H12Q H -0.1511 0.0633 0.8382 0.061 Uiso 1 1 calc R . . H12R H -0.2174 0.1137 0.8963 0.061 Uiso 1 1 calc R . . C128 C -0.2541(5) -0.0142(5) 0.9222(4) 0.0501(18) Uani 1 1 d . . . H12J H -0.2189 -0.0658 0.9099 0.075 Uiso 1 1 calc R . . H12K H -0.3183 -0.0038 0.9019 0.075 Uiso 1 1 calc R . . H12L H -0.2743 -0.0214 0.9752 0.075 Uiso 1 1 calc R . . C129 C 0.0887(5) 0.0951(4) 0.9961(4) 0.0406(16) Uani 1 1 d . . . H12D H 0.1606 0.0890 1.0075 0.049 Uiso 1 1 calc R . . H12E H 0.0519 0.0396 1.0161 0.049 Uiso 1 1 calc R . . C130 C 0.0274(6) 0.1598(4) 1.0351(4) 0.0435(16) Uani 1 1 d . . . H13A H 0.0618 0.2163 1.0151 0.052 Uiso 1 1 calc R . . H13B H -0.0466 0.1639 1.0274 0.052 Uiso 1 1 calc R . . C131 C 0.0255(6) 0.1345(6) 1.1141(4) 0.063(2) Uani 1 1 d . . . H13F H 0.0995 0.1342 1.1216 0.075 Uiso 1 1 calc R . . H13G H -0.0035 0.0761 1.1329 0.075 Uiso 1 1 calc R . . C132 C -0.0438(7) 0.1958(6) 1.1580(5) 0.069(2) Uani 1 1 d . . . H13C H -0.0088 0.2515 1.1453 0.103 Uiso 1 1 calc R . . H13D H -0.0514 0.1724 1.2102 0.103 Uiso 1 1 calc R . . H13E H -0.1146 0.2018 1.1461 0.103 Uiso 1 1 calc R . . C133 C 0.6104(15) 0.5176(15) 0.2213(7) 0.263(16) Uani 1 1 d . . . H13K H 0.6859 0.5247 0.1968 0.395 Uiso 1 1 calc R . . H13L H 0.5743 0.5726 0.2135 0.395 Uiso 1 1 calc R . . H13M H 0.5767 0.4775 0.2013 0.395 Uiso 1 1 calc R . . C134 C 0.6368(8) 0.3963(5) 0.2965(4) 0.066(2) Uani 1 1 d . . . H13H H 0.5742 0.3605 0.3025 0.100 Uiso 1 1 calc R . . H13I H 0.6762 0.3730 0.3345 0.100 Uiso 1 1 calc R . . H13J H 0.6833 0.3976 0.2487 0.100 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 S1 0.0180(7) 0.0318(7) 0.0258(6) -0.0072(5) -0.0048(5) -0.0013(5) S2 0.0185(7) 0.0313(7) 0.0278(7) -0.0027(5) -0.0027(5) -0.0042(5) S3 0.0817(18) 0.109(2) 0.0788(15) -0.0332(14) -0.0210(12) 0.0104(15) O1 0.100(5) 0.061(3) 0.065(3) -0.039(3) -0.022(3) 0.015(3) O2 0.051(3) 0.070(3) 0.038(2) -0.012(2) -0.004(2) -0.028(3) O3 0.035(2) 0.031(2) 0.052(3) -0.0071(19) -0.0073(19) 0.0048(19) O4 0.034(3) 0.128(5) 0.036(2) -0.036(3) -0.0094(19) 0.003(3) O5 0.077(4) 0.116(5) 0.040(3) -0.033(3) 0.001(2) -0.051(4) O6 0.034(2) 0.028(2) 0.043(2) -0.0037(18) -0.0093(18) -0.0066(17) O7 0.067(4) 0.096(4) 0.042(3) -0.029(3) -0.013(2) -0.011(3) O8 0.065(4) 0.094(4) 0.037(3) -0.014(3) 0.014(2) -0.023(3) O9 0.128(6) 0.120(6) 0.029(3) -0.004(3) 0.015(3) -0.063(5) O10 0.142(7) 0.105(5) 0.041(3) -0.026(3) -0.007(3) -0.071(5) O11 0.028(2) 0.035(2) 0.043(2) 0.0011(18) -0.0102(17) -0.0044(17) O12 0.055(3) 0.057(3) 0.038(2) -0.013(2) 0.004(2) -0.019(2) O13 0.050(3) 0.120(5) 0.043(3) -0.035(3) -0.017(2) 0.004(3) O14 0.044(3) 0.042(3) 0.039(2) -0.0013(19) -0.0142(19) 0.007(2) O15 0.104(5) 0.081(4) 0.055(3) -0.036(3) -0.004(3) 0.022(4) O16 0.062(4) 0.091(4) 0.043(3) -0.024(3) -0.015(2) -0.012(3) O17 0.022(2) 0.033(2) 0.0283(18) -0.0040(15) -0.0075(15) 0.0024(15) O18 0.019(2) 0.034(2) 0.0319(19) -0.0070(16) -0.0066(15) 0.0009(16) O19 0.029(2) 0.043(2) 0.0312(19) -0.0150(17) -0.0058(16) 0.0068(18) O20 0.029(2) 0.037(2) 0.0241(18) -0.0011(16) -0.0009(15) -0.0152(17) O21 0.017(2) 0.029(2) 0.056(2) -0.0060(18) -0.0084(17) -0.0025(16) O22 0.048(3) 0.042(2) 0.0235(19) -0.0049(17) -0.0075(17) 0.007(2) O23 0.026(2) 0.038(2) 0.036(2) -0.0140(17) -0.0068(16) 0.0054(17) O24 0.032(2) 0.041(2) 0.036(2) -0.0002(18) -0.0060(17) -0.0151(18) O25 0.135(10) 0.39(3) 0.224(14) 0.070(16) -0.072(10) -0.003(13) N1 0.062(4) 0.037(3) 0.041(3) -0.016(2) -0.002(3) -0.008(3) N2 0.035(3) 0.027(2) 0.029(2) -0.009(2) -0.006(2) 0.000(2) N3 0.026(3) 0.036(3) 0.031(2) -0.004(2) -0.0066(19) 0.005(2) N4 0.026(3) 0.055(3) 0.030(2) -0.003(2) -0.009(2) -0.001(2) N5 0.022(3) 0.055(3) 0.024(2) -0.008(2) -0.0041(18) -0.004(2) N6 0.046(3) 0.050(3) 0.033(3) -0.011(2) 0.003(2) -0.015(3) N7 0.031(3) 0.047(3) 0.036(3) -0.019(2) -0.003(2) -0.004(2) N8 0.027(3) 0.027(2) 0.029(2) -0.0043(19) -0.0041(19) -0.0055(19) N9 0.020(2) 0.027(2) 0.024(2) -0.0066(18) 0.0013(17) -0.0080(18) N10 0.040(3) 0.077(4) 0.043(3) -0.019(3) -0.010(3) -0.009(3) N11 0.078(5) 0.113(6) 0.030(3) -0.006(4) -0.010(3) -0.029(5) N12 0.019(2) 0.035(3) 0.036(3) 0.000(2) 0.0002(19) -0.006(2) N13 0.021(3) 0.033(3) 0.043(3) -0.005(2) -0.002(2) -0.012(2) N14 0.028(3) 0.043(3) 0.028(2) -0.007(2) -0.0049(19) -0.008(2) N15 0.031(3) 0.056(3) 0.029(2) -0.002(2) 0.000(2) -0.008(3) N16 0.034(3) 0.053(3) 0.030(2) -0.014(2) -0.007(2) 0.005(2) N17 0.025(3) 0.058(3) 0.033(3) -0.009(2) -0.004(2) 0.006(2) N18 0.029(3) 0.036(3) 0.026(2) 0.001(2) -0.0107(19) 0.000(2) N19 0.028(3) 0.028(3) 0.037(3) -0.009(2) -0.009(2) 0.005(2) N20 0.061(4) 0.051(3) 0.041(3) -0.015(3) -0.002(3) -0.025(3) N21 0.073(5) 0.076(4) 0.063(4) -0.039(3) -0.037(3) 0.015(4) N22 0.019(2) 0.028(2) 0.040(3) -0.008(2) -0.0059(19) -0.0023(19) N23 0.087(5) 0.059(4) 0.061(4) -0.028(3) -0.042(3) 0.027(4) N24 0.021(3) 0.024(2) 0.067(3) -0.005(2) -0.020(2) 0.002(2) C1 0.037(4) 0.032(3) 0.032(3) -0.005(2) -0.007(2) -0.003(3) C2 0.021(3) 0.034(3) 0.038(3) -0.005(2) -0.007(2) -0.007(2) C3 0.021(3) 0.033(3) 0.037(3) -0.008(2) -0.007(2) 0.001(2) C4 0.030(3) 0.029(3) 0.038(3) -0.012(2) -0.004(2) -0.003(2) C5 0.025(3) 0.038(3) 0.043(3) -0.009(3) -0.002(3) 0.003(3) C6 0.033(4) 0.033(3) 0.042(3) -0.016(3) 0.006(3) 0.007(3) C7 0.019(3) 0.044(4) 0.035(3) -0.004(3) 0.001(2) -0.008(3) C8 0.020(3) 0.046(3) 0.034(3) 0.003(3) -0.009(2) -0.002(3) C9 0.031(3) 0.045(4) 0.040(3) -0.001(3) -0.003(3) 0.002(3) C10 0.038(4) 0.098(6) 0.051(4) 0.013(4) -0.005(3) 0.022(4) C11 0.047(5) 0.127(8) 0.028(3) 0.022(4) -0.011(3) 0.003(5) C12 0.037(4) 0.100(6) 0.035(3) -0.009(4) -0.009(3) 0.010(4) C13 0.028(3) 0.067(4) 0.028(3) 0.000(3) -0.006(2) -0.004(3) C14 0.019(3) 0.081(5) 0.034(3) -0.014(3) 0.001(3) -0.002(3) C15 0.021(3) 0.052(4) 0.037(3) -0.010(3) 0.005(2) -0.004(3) C16 0.031(4) 0.081(5) 0.030(3) -0.006(3) 0.009(3) -0.012(3) C17 0.054(5) 0.084(5) 0.026(3) -0.011(3) 0.010(3) 0.011(4) C18 0.074(6) 0.071(5) 0.053(4) -0.033(4) 0.038(4) -0.013(4) C19 0.068(5) 0.061(4) 0.037(3) -0.020(3) 0.018(3) -0.018(4) C20 0.036(4) 0.060(4) 0.032(3) -0.018(3) 0.003(3) -0.006(3) C21 0.037(4) 0.059(4) 0.047(4) -0.025(3) 0.001(3) -0.017(3) C22 0.027(3) 0.029(3) 0.039(3) -0.002(2) -0.004(2) -0.005(2) C23 0.043(4) 0.040(3) 0.039(3) -0.013(3) -0.013(3) -0.001(3) C24 0.044(4) 0.034(3) 0.043(3) 0.001(3) -0.021(3) -0.010(3) C25 0.036(4) 0.031(3) 0.058(4) -0.006(3) -0.016(3) -0.002(3) C26 0.027(3) 0.024(3) 0.045(3) -0.008(2) -0.008(2) 0.003(2) C27 0.020(3) 0.028(3) 0.042(3) -0.009(2) -0.008(2) -0.006(2) C28 0.018(3) 0.031(3) 0.032(3) -0.001(2) -0.003(2) -0.001(2) C29 0.016(3) 0.039(3) 0.025(3) -0.003(2) -0.002(2) 0.002(2) C30 0.030(3) 0.042(3) 0.029(3) -0.009(2) -0.008(2) -0.006(3) C31 0.029(3) 0.059(4) 0.029(3) -0.007(3) 0.001(2) -0.015(3) C32 0.029(3) 0.053(4) 0.023(3) -0.007(3) -0.005(2) 0.003(3) C33 0.036(4) 0.043(4) 0.044(3) -0.016(3) -0.016(3) 0.000(3) C34 0.028(3) 0.033(3) 0.031(3) -0.005(2) -0.006(2) -0.007(2) C35 0.051(4) 0.060(4) 0.024(3) 0.003(3) -0.010(3) -0.006(3) C36 0.050(4) 0.058(4) 0.038(4) -0.003(3) -0.003(3) -0.025(3) C37 0.041(4) 0.047(4) 0.030(3) 0.007(3) -0.011(3) -0.019(3) C38 0.017(3) 0.035(3) 0.035(3) 0.002(2) -0.008(2) -0.001(2) C39 0.028(3) 0.047(4) 0.036(3) 0.000(3) -0.003(3) -0.001(3) C40 0.034(4) 0.059(4) 0.031(3) 0.002(3) -0.011(3) -0.021(3) C41 0.017(3) 0.026(3) 0.034(3) -0.004(2) -0.004(2) -0.006(2) C42 0.025(3) 0.024(3) 0.026(3) 0.004(2) -0.008(2) -0.011(2) C43 0.031(3) 0.041(3) 0.048(4) -0.003(3) -0.010(3) 0.001(3) C44 0.039(4) 0.030(3) 0.064(4) 0.005(3) -0.026(3) -0.012(3) C45 0.064(5) 0.034(3) 0.046(4) -0.001(3) -0.027(3) -0.011(3) C46 0.051(4) 0.028(3) 0.047(4) -0.011(3) -0.016(3) 0.000(3) C47 0.032(3) 0.036(3) 0.030(3) -0.005(2) -0.011(2) -0.002(3) C48 0.033(4) 0.041(3) 0.045(4) -0.020(3) -0.002(3) -0.004(3) C49 0.034(4) 0.047(4) 0.035(3) -0.005(3) 0.008(3) -0.005(3) C50 0.054(4) 0.048(4) 0.055(4) -0.015(3) 0.013(3) -0.002(3) C51 0.082(6) 0.072(6) 0.064(5) -0.016(4) 0.040(5) 0.003(5) C52 0.093(7) 0.053(5) 0.056(5) -0.001(4) 0.011(4) 0.007(4) C53 0.060(5) 0.041(4) 0.041(3) -0.009(3) 0.004(3) 0.000(3) C54 0.051(4) 0.049(4) 0.034(3) -0.007(3) 0.001(3) -0.003(3) C55 0.037(4) 0.056(4) 0.042(4) -0.020(3) -0.004(3) 0.000(3) C56 0.030(4) 0.058(4) 0.044(3) -0.003(3) -0.014(3) 0.005(3) C57 0.040(4) 0.092(6) 0.039(4) 0.001(4) -0.023(3) 0.001(4) C58 0.046(5) 0.091(6) 0.064(5) 0.019(4) -0.029(4) -0.009(4) C59 0.019(3) 0.075(5) 0.050(4) -0.002(3) -0.011(3) -0.003(3) C60 0.029(3) 0.043(4) 0.048(4) -0.005(3) -0.006(3) 0.003(3) C61 0.031(3) 0.045(3) 0.026(3) 0.003(2) -0.010(2) -0.013(3) C62 0.028(3) 0.020(3) 0.030(3) -0.005(2) -0.007(2) 0.007(2) C63 0.030(3) 0.018(3) 0.031(3) 0.001(2) -0.008(2) -0.011(2) C64 0.023(3) 0.023(3) 0.038(3) -0.005(2) 0.002(2) -0.004(2) C65 0.031(3) 0.033(3) 0.046(3) 0.001(3) -0.009(3) -0.013(3) C66 0.046(4) 0.024(3) 0.037(3) -0.009(2) 0.001(3) -0.013(3) C67 0.035(4) 0.041(3) 0.036(3) -0.005(3) -0.006(3) 0.002(3) C68 0.034(3) 0.038(3) 0.038(3) -0.003(3) -0.010(3) 0.005(3) C69 0.053(5) 0.068(5) 0.059(4) -0.033(4) -0.001(3) -0.001(4) C70 0.121(8) 0.066(5) 0.044(4) -0.006(4) -0.014(4) 0.015(5) C71 0.089(9) 0.28(2) 0.151(11) -0.131(13) 0.061(9) -0.108(12) C72 0.100(7) 0.055(5) 0.059(5) 0.023(4) -0.002(5) -0.014(5) C73 0.096(7) 0.100(7) 0.075(5) -0.033(5) -0.032(5) 0.060(6) C74 0.105(9) 0.096(8) 0.096(7) -0.015(6) -0.061(6) 0.015(7) C75 0.126(10) 0.089(7) 0.109(8) -0.012(6) -0.067(8) 0.027(7) C76 0.045(7) 0.36(3) 0.140(12) -0.046(15) -0.032(7) 0.032(12) C77 0.073(6) 0.089(6) 0.055(5) -0.007(4) -0.027(4) -0.013(5) C78 0.065(6) 0.123(8) 0.059(5) 0.006(5) -0.017(4) -0.026(6) C79 0.049(5) 0.081(6) 0.041(4) 0.022(4) 0.002(3) 0.026(4) C80 0.042(5) 0.074(6) 0.123(8) -0.057(5) -0.011(5) -0.003(4) C81 0.053(5) 0.107(8) 0.080(6) -0.039(5) -0.028(4) 0.008(5) C82 0.101(9) 0.160(13) 0.155(11) -0.104(10) -0.089(8) 0.091(9) C83 0.298(19) 0.059(6) 0.025(4) -0.007(4) 0.052(7) -0.041(8) C84 0.42(4) 0.115(12) 0.127(12) -0.034(10) -0.056(17) -0.081(18) C85 0.017(3) 0.038(3) 0.052(4) -0.005(3) -0.019(2) 0.008(2) C86 0.028(3) 0.030(3) 0.046(3) -0.001(3) -0.010(3) -0.001(3) C87 0.034(4) 0.041(4) 0.081(5) 0.002(4) -0.023(3) 0.002(3) C88 0.023(3) 0.036(3) 0.063(4) -0.007(3) -0.019(3) -0.003(3) C89 0.025(3) 0.036(3) 0.025(3) -0.008(2) -0.006(2) 0.001(2) C90 0.032(4) 0.038(3) 0.055(4) -0.019(3) 0.003(3) -0.004(3) C91 0.043(4) 0.063(4) 0.032(3) -0.010(3) -0.002(3) 0.002(3) C92 0.053(5) 0.077(5) 0.052(4) -0.014(4) 0.009(3) 0.019(4) C93 0.020(3) 0.037(3) 0.037(3) -0.013(3) -0.008(2) 0.007(2) C94 0.037(4) 0.048(4) 0.035(3) -0.009(3) -0.009(3) 0.010(3) C95 0.027(3) 0.050(4) 0.050(4) -0.019(3) -0.012(3) 0.010(3) C96 0.075(6) 0.080(6) 0.057(5) -0.024(4) -0.020(4) 0.031(5) C97 0.026(3) 0.026(3) 0.038(3) -0.007(2) -0.004(2) -0.002(2) C98 0.030(3) 0.038(3) 0.047(3) 0.002(3) -0.016(3) -0.011(3) C99 0.029(4) 0.044(4) 0.058(4) -0.005(3) -0.016(3) 0.003(3) C100 0.039(4) 0.052(4) 0.061(5) 0.021(4) 0.003(3) 0.005(3) C101 0.113(10) 0.107(9) 0.152(10) -0.100(9) -0.085(8) 0.067(8) C102 0.086(9) 0.106(10) 0.242(17) -0.053(11) -0.038(10) 0.065(8) C103 0.125(15) 0.189(18) 0.48(4) -0.25(2) -0.12(2) 0.100(14) C104 0.24(3) 0.169(18) 0.44(4) -0.19(2) -0.21(3) 0.033(17) C105 0.119(9) 0.062(5) 0.080(6) -0.030(5) -0.022(5) 0.008(5) C106 0.108(9) 0.110(8) 0.130(9) -0.085(7) -0.048(7) 0.044(7) C107 0.247(18) 0.085(8) 0.101(8) 0.014(7) 0.055(10) 0.093(10) C108 0.170(14) 0.096(8) 0.129(10) -0.059(8) 0.015(9) -0.013(9) C109 0.067(5) 0.052(4) 0.047(4) -0.011(3) -0.016(3) 0.004(4) C110 0.061(5) 0.047(4) 0.066(4) -0.026(3) -0.035(4) 0.006(3) C111 0.062(5) 0.080(6) 0.050(4) -0.013(4) -0.001(4) 0.000(4) C112 0.058(5) 0.072(5) 0.091(6) -0.032(5) 0.021(5) -0.011(4) C113 0.118(9) 0.053(5) 0.061(5) -0.018(4) 0.003(5) 0.033(5) C114 0.192(15) 0.063(6) 0.061(6) -0.018(5) 0.035(7) 0.000(7) C115 0.36(3) 0.096(10) 0.114(11) -0.026(9) 0.082(15) 0.050(14) C116 0.22(2) 0.67(7) 0.081(10) -0.049(19) -0.040(11) 0.28(3) C117 0.030(3) 0.021(3) 0.076(5) 0.003(3) -0.025(3) -0.003(3) C118 0.047(4) 0.044(4) 0.070(5) -0.007(3) -0.024(4) 0.009(3) C119 0.024(4) 0.047(4) 0.086(5) -0.017(4) -0.017(3) -0.004(3) C120 0.076(7) 0.077(6) 0.096(7) -0.039(5) -0.029(5) 0.035(5) C121 0.025(3) 0.028(3) 0.060(4) -0.002(3) -0.013(3) -0.005(2) C122 0.025(3) 0.043(4) 0.065(4) 0.001(3) -0.021(3) -0.007(3) C123 0.051(5) 0.037(4) 0.076(5) 0.004(3) -0.019(4) -0.014(3) C124 0.050(5) 0.075(5) 0.064(5) -0.009(4) -0.002(4) -0.009(4) C125 0.024(3) 0.025(3) 0.064(4) -0.008(3) -0.018(3) 0.005(2) C126 0.022(3) 0.037(3) 0.051(4) -0.004(3) -0.017(3) -0.003(3) C127 0.023(4) 0.045(4) 0.083(5) 0.000(4) -0.019(3) -0.006(3) C128 0.022(3) 0.048(4) 0.081(5) -0.008(4) -0.020(3) -0.001(3) C129 0.024(3) 0.031(3) 0.064(4) 0.009(3) -0.022(3) -0.005(3) C130 0.037(4) 0.034(3) 0.062(4) -0.002(3) -0.023(3) -0.002(3) C131 0.035(4) 0.070(5) 0.078(5) -0.007(4) -0.011(4) 0.009(4) C132 0.052(5) 0.088(6) 0.067(5) -0.020(4) -0.014(4) 0.002(4) C133 0.29(2) 0.47(3) 0.123(10) -0.220(16) -0.156(13) 0.33(2) C134 0.089(6) 0.047(4) 0.067(5) -0.019(4) -0.020(4) 0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O20 1.463(4) . ? S1 O17 1.475(4) . ? S1 O19 1.481(4) . ? S1 O18 1.491(4) . ? S2 O23 1.463(4) . ? S2 O24 1.475(4) . ? S2 O22 1.478(4) . ? S2 O21 1.490(4) . ? S3 C134 1.480(8) . ? S3 C133 1.520(13) . ? S3 O25 1.789(14) . ? O1 N1 1.227(8) . ? O2 N1 1.222(8) . ? O3 C7 1.252(7) . ? O4 C14 1.238(8) . ? O5 C21 1.235(9) . ? O6 C28 1.205(7) . ? O7 N10 1.271(9) . ? O8 N10 1.225(7) . ? O9 N11 1.233(9) . ? O10 N11 1.216(10) . ? O11 C41 1.234(6) . ? O12 C48 1.275(8) . ? O13 C55 1.235(9) . ? O14 C62 1.219(7) . ? O15 N20 1.241(8) . ? O16 N20 1.231(8) . ? N1 C1 1.459(8) . ? N2 C7 1.376(8) . ? N2 C4 1.410(8) . ? N3 C7 1.361(8) . ? N3 C8 1.427(8) . ? N4 C14 1.366(8) . ? N4 C13 1.406(8) . ? N5 C14 1.400(8) . ? N5 C15 1.448(7) . ? N6 C21 1.332(9) . ? N6 C20 1.491(7) . ? N7 C22 1.389(8) . ? N7 C21 1.400(8) . ? N8 C28 1.391(7) . ? N8 C27 1.395(8) . ? N9 C29 1.379(7) . ? N9 C28 1.385(8) . ? N10 C32 1.422(8) . ? N11 C35 1.476(9) . ? N12 C38 1.380(8) . ? N12 C41 1.385(8) . ? N13 C41 1.343(7) . ? N13 C42 1.415(8) . ? N14 C48 1.392(7) . ? N14 C47 1.408(8) . ? N15 C48 1.301(9) . ? N15 C49 1.457(7) . ? N16 C55 1.356(9) . ? N16 C54 1.474(8) . ? N17 C55 1.370(8) . ? N17 C56 1.394(8) . ? N18 C62 1.326(8) . ? N18 C61 1.439(7) . ? N19 C63 1.393(8) . ? N19 C62 1.394(7) . ? N20 C66 1.443(8) . ? N21 C81 1.491(12) . ? N21 C77 1.520(10) . ? N21 C73 1.535(11) . ? N21 C69 1.572(9) . ? N22 C85 1.495(8) . ? N22 C89 1.522(7) . ? N22 C97 1.524(7) . ? N22 C93 1.529(7) . ? N23 C105 1.507(11) . ? N23 C101 1.513(14) . ? N23 C109 1.517(9) . ? N23 C113 1.521(11) . ? N24 C129 1.492(9) . ? N24 C117 1.516(8) . ? N24 C121 1.528(7) . ? N24 C125 1.546(8) . ? C1 C6 1.357(9) . ? C1 C2 1.415(8) . ? C2 C3 1.369(9) . ? C3 C4 1.384(9) . ? C4 C5 1.425(8) . ? C5 C6 1.372(9) . ? C8 C13 1.387(8) . ? C8 C9 1.395(9) . ? C9 C10 1.384(10) . ? C10 C11 1.334(11) . ? C11 C12 1.403(11) . ? C12 C13 1.391(9) . ? C15 C20 1.505(10) . ? C15 C16 1.548(8) . ? C16 C17 1.519(10) . ? C17 C18 1.494(12) . ? C18 C19 1.533(9) . ? C19 C20 1.541(9) . ? C22 C27 1.392(8) . ? C22 C23 1.419(9) . ? C23 C24 1.375(9) . ? C24 C25 1.420(9) . ? C25 C26 1.365(9) . ? C26 C27 1.384(8) . ? C29 C34 1.393(9) . ? C29 C30 1.396(8) . ? C30 C31 1.426(9) . ? C31 C32 1.361(10) . ? C32 C33 1.409(9) . ? C33 C34 1.361(9) . ? C35 C36 1.372(11) . ? C35 C40 1.409(9) . ? C36 C37 1.359(9) . ? C37 C38 1.453(8) . ? C38 C39 1.392(9) . ? C39 C40 1.377(9) . ? C42 C43 1.403(8) . ? C42 C47 1.415(8) . ? C43 C44 1.399(10) . ? C44 C45 1.396(10) . ? C45 C46 1.368(10) . ? C46 C47 1.389(9) . ? C49 C50 1.522(9) . ? C49 C54 1.527(9) . ? C50 C51 1.546(10) . ? C51 C52 1.571(12) . ? C52 C53 1.509(10) . ? C53 C54 1.514(9) . ? C56 C57 1.410(9) . ? C56 C61 1.410(9) . ? C57 C58 1.390(11) . ? C58 C59 1.344(11) . ? C59 C60 1.408(10) . ? C60 C61 1.371(9) . ? C63 C64 1.388(9) . ? C63 C68 1.399(8) . ? C64 C65 1.383(9) . ? C65 C66 1.394(9) . ? C66 C67 1.418(10) . ? C67 C68 1.346(9) . ? C69 C70 1.506(13) . ? C70 C71 1.440(15) . ? C71 C72 1.541(15) . ? C73 C74 1.507(12) . ? C74 C75 1.412(15) . ? C75 C76 1.468(16) . ? C77 C78 1.449(12) . ? C78 C79 1.451(11) . ? C79 C80 1.564(11) . ? C81 C82 1.379(16) . ? C82 C83 1.60(2) . ? C83 C84 1.551(18) . ? C85 C86 1.522(9) . ? C86 C87 1.546(10) . ? C87 C88 1.502(9) . ? C89 C90 1.522(8) . ? C90 C91 1.532(9) . ? C91 C92 1.501(10) . ? C93 C94 1.471(8) . ? C94 C95 1.511(8) . ? C95 C96 1.527(10) . ? C97 C98 1.510(9) . ? C98 C99 1.550(9) . ? C99 C100 1.535(10) . ? C101 C102 1.480(19) . ? C102 C103 1.46(2) . ? C103 C104 1.15(2) . ? C105 C106 1.564(14) . ? C106 C107 1.529(13) . ? C107 C108 1.564(17) . ? C109 C110 1.522(10) . ? C110 C111 1.603(11) . ? C111 C112 1.421(11) . ? C113 C114 1.448(18) . ? C114 C115 1.507(17) . ? C115 C116 1.11(2) . ? C117 C118 1.553(11) . ? C118 C119 1.504(10) . ? C119 C120 1.437(12) . ? C121 C122 1.524(9) . ? C122 C123 1.514(9) . ? C123 C124 1.529(12) . ? C125 C126 1.515(8) . ? C126 C127 1.502(10) . ? C127 C128 1.515(9) . ? C129 C130 1.512(10) . ? C130 C131 1.485(11) . ? C131 C132 1.563(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 O20 S1 O17 109.8(2) . . ? O20 S1 O19 111.6(2) . . ? O17 S1 O19 110.9(2) . . ? O20 S1 O18 108.3(2) . . ? O17 S1 O18 108.1(2) . . ? O19 S1 O18 108.1(2) . . ? O23 S2 O24 110.7(2) . . ? O23 S2 O22 110.4(2) . . ? O24 S2 O22 111.2(3) . . ? O23 S2 O21 108.1(2) . . ? O24 S2 O21 108.4(2) . . ? O22 S2 O21 107.9(2) . . ? C134 S3 C133 96.0(7) . . ? C134 S3 O25 109.5(9) . . ? C133 S3 O25 89.2(9) . . ? O2 N1 O1 124.4(6) . . ? O2 N1 C1 118.7(5) . . ? O1 N1 C1 116.9(6) . . ? C7 N2 C4 126.1(5) . . ? C7 N3 C8 123.6(5) . . ? C14 N4 C13 127.2(6) . . ? C14 N5 C15 123.6(6) . . ? C21 N6 C20 119.4(6) . . ? C22 N7 C21 127.3(6) . . ? C28 N8 C27 122.7(5) . . ? C29 N9 C28 126.6(4) . . ? O8 N10 O7 121.7(6) . . ? O8 N10 C32 120.6(7) . . ? O7 N10 C32 117.5(5) . . ? O10 N11 O9 123.5(7) . . ? O10 N11 C35 119.7(6) . . ? O9 N11 C35 116.7(8) . . ? C38 N12 C41 128.3(5) . . ? C41 N13 C42 123.8(5) . . ? C48 N14 C47 128.1(5) . . ? C48 N15 C49 124.6(6) . . ? C55 N16 C54 121.7(6) . . ? C55 N17 C56 125.9(6) . . ? C62 N18 C61 123.6(5) . . ? C63 N19 C62 124.0(5) . . ? O16 N20 O15 124.7(6) . . ? O16 N20 C66 119.1(6) . . ? O15 N20 C66 116.1(7) . . ? C81 N21 C77 113.4(7) . . ? C81 N21 C73 110.2(7) . . ? C77 N21 C73 108.2(7) . . ? C81 N21 C69 107.4(6) . . ? C77 N21 C69 105.3(6) . . ? C73 N21 C69 112.3(7) . . ? C85 N22 C89 112.6(4) . . ? C85 N22 C97 106.5(4) . . ? C89 N22 C97 111.1(5) . . ? C85 N22 C93 109.8(5) . . ? C89 N22 C93 105.7(4) . . ? C97 N22 C93 111.2(4) . . ? C105 N23 C101 111.0(7) . . ? C105 N23 C109 105.1(6) . . ? C101 N23 C109 108.7(7) . . ? C105 N23 C113 112.4(7) . . ? C101 N23 C113 108.2(8) . . ? C109 N23 C113 111.4(7) . . ? C129 N24 C117 105.5(5) . . ? C129 N24 C121 113.1(5) . . ? C117 N24 C121 110.7(5) . . ? C129 N24 C125 111.2(5) . . ? C117 N24 C125 111.1(5) . . ? C121 N24 C125 105.4(4) . . ? C6 C1 C2 120.3(6) . . ? C6 C1 N1 121.6(5) . . ? C2 C1 N1 117.9(6) . . ? C3 C2 C1 117.8(6) . . ? C2 C3 C4 122.1(5) . . ? C3 C4 N2 119.7(5) . . ? C3 C4 C5 119.7(6) . . ? N2 C4 C5 120.6(6) . . ? C6 C5 C4 117.2(6) . . ? C1 C6 C5 122.9(5) . . ? O3 C7 N3 126.0(6) . . ? O3 C7 N2 121.0(6) . . ? N3 C7 N2 113.0(5) . . ? C13 C8 C9 118.7(5) . . ? C13 C8 N3 119.2(5) . . ? C9 C8 N3 122.2(5) . . ? C10 C9 C8 121.5(6) . . ? C11 C10 C9 119.9(7) . . ? C10 C11 C12 120.2(6) . . ? C13 C12 C11 120.6(6) . . ? C8 C13 C12 119.0(6) . . ? C8 C13 N4 116.9(5) . . ? C12 C13 N4 124.1(6) . . ? O4 C14 N4 123.9(6) . . ? O4 C14 N5 124.8(6) . . ? N4 C14 N5 111.2(6) . . ? N5 C15 C20 114.0(5) . . ? N5 C15 C16 112.8(5) . . ? C20 C15 C16 111.0(6) . . ? C17 C16 C15 110.3(6) . . ? C18 C17 C16 114.0(6) . . ? C17 C18 C19 110.0(6) . . ? C18 C19 C20 110.7(6) . . ? N6 C20 C15 107.8(5) . . ? N6 C20 C19 112.0(5) . . ? C15 C20 C19 110.7(5) . . ? O5 C21 N6 125.5(6) . . ? O5 C21 N7 121.0(6) . . ? N6 C21 N7 113.5(6) . . ? N7 C22 C27 120.9(6) . . ? N7 C22 C23 120.2(5) . . ? C27 C22 C23 118.9(5) . . ? C24 C23 C22 120.4(6) . . ? C23 C24 C25 119.7(6) . . ? C26 C25 C24 119.0(6) . . ? C25 C26 C27 122.0(6) . . ? C26 C27 C22 119.6(6) . . ? C26 C27 N8 122.1(5) . . ? C22 C27 N8 118.0(5) . . ? O6 C28 N9 123.7(5) . . ? O6 C28 N8 123.1(6) . . ? N9 C28 N8 113.2(4) . . ? N9 C29 C34 116.9(5) . . ? N9 C29 C30 124.5(6) . . ? C34 C29 C30 118.3(5) . . ? C29 C30 C31 118.9(6) . . ? C32 C31 C30 120.7(5) . . ? C31 C32 C33 120.5(5) . . ? C31 C32 N10 118.4(5) . . ? C33 C32 N10 121.1(6) . . ? C34 C33 C32 118.4(6) . . ? C33 C34 C29 123.2(5) . . ? C36 C35 C40 121.2(6) . . ? C36 C35 N11 121.4(6) . . ? C40 C35 N11 117.3(7) . . ? C37 C36 C35 122.7(6) . . ? C36 C37 C38 117.2(6) . . ? N12 C38 C39 118.0(5) . . ? N12 C38 C37 122.7(6) . . ? C39 C38 C37 119.2(6) . . ? C40 C39 C38 122.2(6) . . ? C39 C40 C35 117.4(7) . . ? O11 C41 N13 124.8(6) . . ? O11 C41 N12 122.5(5) . . ? N13 C41 N12 112.6(5) . . ? C43 C42 C47 118.6(6) . . ? C43 C42 N13 120.8(5) . . ? C47 C42 N13 120.6(5) . . ? C44 C43 C42 121.0(6) . . ? C45 C44 C43 118.0(6) . . ? C46 C45 C44 122.7(7) . . ? C45 C46 C47 119.3(6) . . ? C46 C47 N14 123.4(5) . . ? C46 C47 C42 120.5(6) . . ? N14 C47 C42 116.1(5) . . ? O12 C48 N15 124.6(5) . . ? O12 C48 N14 121.2(6) . . ? N15 C48 N14 114.2(6) . . ? N15 C49 C50 112.7(5) . . ? N15 C49 C54 114.8(5) . . ? C50 C49 C54 110.1(5) . . ? C49 C50 C51 109.9(6) . . ? C50 C51 C52 109.9(7) . . ? C53 C52 C51 109.0(7) . . ? C52 C53 C54 110.8(6) . . ? N16 C54 C53 111.3(5) . . ? N16 C54 C49 109.6(5) . . ? C53 C54 C49 111.1(6) . . ? O13 C55 N16 122.7(6) . . ? O13 C55 N17 124.8(6) . . ? N16 C55 N17 112.3(6) . . ? N17 C56 C57 123.0(6) . . ? N17 C56 C61 118.7(6) . . ? C57 C56 C61 118.2(6) . . ? C58 C57 C56 118.8(7) . . ? C59 C58 C57 122.2(7) . . ? C58 C59 C60 120.2(6) . . ? C61 C60 C59 118.8(6) . . ? C60 C61 C56 121.6(6) . . ? C60 C61 N18 120.7(5) . . ? C56 C61 N18 117.7(5) . . ? O14 C62 N18 124.6(5) . . ? O14 C62 N19 121.1(5) . . ? N18 C62 N19 114.3(4) . . ? C64 C63 N19 117.9(5) . . ? C64 C63 C68 119.4(5) . . ? N19 C63 C68 122.7(6) . . ? C65 C64 C63 119.8(5) . . ? C64 C65 C66 120.1(6) . . ? C65 C66 C67 119.9(6) . . ? C65 C66 N20 119.6(7) . . ? C67 C66 N20 120.6(6) . . ? C68 C67 C66 118.8(6) . . ? C67 C68 C63 122.0(6) . . ? C70 C69 N21 115.9(7) . . ? C71 C70 C69 112.0(9) . . ? C70 C71 C72 114.0(12) . . ? C74 C73 N21 119.8(9) . . ? C75 C74 C73 114.8(10) . . ? C74 C75 C76 113.9(14) . . ? C78 C77 N21 115.1(8) . . ? C77 C78 C79 109.5(8) . . ? C78 C79 C80 111.3(7) . . ? C82 C81 N21 114.9(9) . . ? C81 C82 C83 111.3(9) . . ? C84 C83 C82 117.5(17) . . ? N22 C85 C86 115.2(5) . . ? C85 C86 C87 111.3(5) . . ? C88 C87 C86 112.3(5) . . ? C90 C89 N22 115.0(5) . . ? C89 C90 C91 109.6(5) . . ? C92 C91 C90 113.4(6) . . ? C94 C93 N22 117.0(5) . . ? C93 C94 C95 110.8(5) . . ? C94 C95 C96 113.7(6) . . ? C98 C97 N22 115.7(5) . . ? C97 C98 C99 110.9(5) . . ? C100 C99 C98 112.2(6) . . ? C102 C101 N23 117.6(10) . . ? C103 C102 C101 109.7(16) . . ? C104 C103 C102 131.9(19) . . ? N23 C105 C106 112.2(8) . . ? C107 C106 C105 115.4(10) . . ? C106 C107 C108 113.2(11) . . ? N23 C109 C110 117.7(6) . . ? C109 C110 C111 111.2(6) . . ? C112 C111 C110 111.4(8) . . ? C114 C113 N23 116.5(8) . . ? C113 C114 C115 115.2(15) . . ? C116 C115 C114 117(2) . . ? N24 C117 C118 116.0(5) . . ? C119 C118 C117 111.5(6) . . ? C120 C119 C118 113.3(7) . . ? C122 C121 N24 115.6(5) . . ? C123 C122 C121 109.5(5) . . ? C122 C123 C124 115.6(7) . . ? C126 C125 N24 114.4(5) . . ? C127 C126 C125 111.4(5) . . ? C126 C127 C128 111.9(6) . . ? N24 C129 C130 116.3(5) . . ? C131 C130 C129 110.0(5) . . ? C130 C131 C132 112.2(6) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.770 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.075 ######END