# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _publ_contact_author_name 'Stephen Hanessian' _publ_contact_author_email 'stephen.hanessian@umontreal.ca ' loop_ _publ_author_name S.Hanessian J.Maianti V.Ly B.Deschenes-Simard data_bent52 _database_code_depnum_ccdc_archive 'CCDC 838347' #TrackingRef '- BENT52.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H21 N9 O6' _chemical_formula_sum 'C14 H21 N9 O6' _chemical_formula_weight 411.40 _chemical_compound_source 'Synthesized by the authors. See text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 _symmetry_space_group_name_hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 15.8942(5) _cell_length_b 16.2322(5) _cell_length_c 17.6688(6) _cell_angle_alpha 89.7480(10) _cell_angle_beta 72.741(2) _cell_angle_gamma 63.5370(10) _cell_volume 3853.3(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150 _cell_measurement_reflns_used 32142 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 63.73 _exptl_crystal_description plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.966 _exptl_absorpt_correction_Type multi-scan _exptl_absorpt_correction_T_min 0.8116 _exptl_absorpt_correction_T_max 0.9437 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 2004)' _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Platform diffractometer, equipped with a Bruker SMART 4K Charged-Coupled Device (CCD) Area Detector using the program APEX2 and a Nonius FR591 rotating anode equiped with a Montel 200 optics The crystal-to-detector distance was 5.0 cm, and the data collection was carried out in 512 x 512 pixel mode. The initial unit cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 10.0 degree scan in 33 frames over four different parts of the reciprocal space (132 frames total). One complete sphere of data was collected, to better than 0.80\%A resolution. ; _vrf_PLAT029_bent52 ; RESPONSE: Due to geometrical constraints of the instrument and the use of copper radiation, we obtain consistently a data completeness lower than 100% in dependence of the crystal system and the orientation of the mounted crystal, even with appropriate data collection routines. Typical values for data completeness range from 83-92% for triclinic, 85-97% for monoclinic and 85-98% for all other crystal systems. (Note: This comment is routinely included into the CIF-file and can be ignored if the data completeness is satisfactory.) ; _vrf_THETM01_bent52 ; RESPONSE: Low diffraction was observed for this crystal and was especially low for high angles. Many solvent systems were tested for recrystallization. The best crystal was chosen and its size was in the limits of the diffractometer. X-ray measurements were acquired at 150K with optimized radiation exposure time and intensity. Low diffraction is also a consequence of disorder present in some molecules and the large asymmetric unit that contains 8 molecules. The final structure was satisfactory for confirming the desired chemical information with R1 = 0.0440 and wR2=0.1118. ; _vrf_PLAT340_bent52 ; RESPONSE: See response for THETM01 Alert 3 C. ; _vrf_PLAT911_bent52 ; RESPONSE: See response for PLAT029 Alert 3 B and THETM01 Alert 3 C. ; _vrf_PLAT915_bent52 ; RESPONSE: Absolute stereochemistry is known and confirmed with flack parameter. ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Montel 200 optics' _diffrn_measurement_device_type 'Bruker Smart 6000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 5.5 _diffrn_reflns_number 53806 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 64.12 _reflns_number_total 20234 _reflns_number_gt 16661 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT V7.60A(Bruker AXS, 2008)' _computing_data_reduction 'SAINT V7.60A(Bruker AXS, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_publication_material 'UdMX (Maris, 2004)' _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^)+(0.0688P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00085(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Friedel Pairs merged' _chemical_absolute_configuration rmad _refine_ls_abs_structure_Flack 0.10(11) _refine_ls_number_reflns 20234 _refine_ls_number_parameters 2194 _refine_ls_number_restraints 447 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1117 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 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 O11 O 0.83496(18) 0.12084(18) 1.04059(14) 0.0348(6) Uani 1 1 d . . . O12 O 0.94268(18) 0.17918(19) 0.97347(15) 0.0365(6) Uani 1 1 d . . . O13 O 0.77342(17) 0.14093(17) 0.90357(13) 0.0278(5) Uani 1 1 d . . . O14 O 0.78180(17) 0.02535(16) 0.81814(14) 0.0267(5) Uani 1 1 d . . . O15 O 0.57412(19) 0.12536(17) 0.82241(15) 0.0317(6) Uani 1 1 d . . . H15 H 0.5370 0.1383 0.7942 0.048 Uiso 1 1 calc R . . O16 O 0.48758(18) 0.01023(18) 0.80924(14) 0.0306(6) Uani 1 1 d . . . H16 H 0.4287 0.0453 0.8383 0.046 Uiso 1 1 calc R . . N11 N 0.8095(2) 0.1120(2) 0.68419(17) 0.0366(7) Uani 1 1 d DU . . N12 N 0.8641(3) 0.0303(3) 0.6519(2) 0.0461(9) Uani 1 1 d DU . . N13 N 0.9077(3) -0.0434(3) 0.6191(3) 0.0692(12) Uani 1 1 d U . . N14 N 0.5362(2) -0.1502(2) 0.89746(17) 0.0349(7) Uani 1 1 d D . . N15 N 0.4821(2) -0.1541(2) 0.86389(16) 0.0319(7) Uani 1 1 d D . . N16 N 0.4260(2) -0.1627(2) 0.84127(18) 0.0400(8) Uani 1 1 d D . . N17 N 0.8212(2) -0.1207(2) 0.91253(19) 0.0367(8) Uani 1 1 d . . . N18 N 0.9073(3) -0.1373(2) 0.8757(2) 0.0433(8) Uani 1 1 d . . . N19 N 0.9880(3) -0.1529(3) 0.8490(3) 0.0763(13) Uani 1 1 d . . . C11 C 0.8548(3) 0.1747(3) 0.9810(2) 0.0297(8) Uani 1 1 d . . . H11 H 0.7987 0.2395 0.9976 0.036 Uiso 1 1 calc R . . C12 C 0.8619(2) 0.1397(3) 0.89887(19) 0.0299(8) Uani 1 1 d D . . C13 C 0.9393(2) 0.1146(3) 0.8333(2) 0.0324(9) Uani 1 1 d D . . H13 H 0.9980 0.1148 0.8359 0.039 Uiso 1 1 calc R . . C14 C 0.9350(3) 0.0856(3) 0.7540(2) 0.0343(9) Uani 1 1 d D . . H14A H 0.9769 0.1024 0.7097 0.041 Uiso 1 1 calc R . . H14B H 0.9600 0.0174 0.7448 0.041 Uiso 1 1 calc R . . C15 C 0.8285(3) 0.1354(3) 0.7571(2) 0.0300(8) Uani 1 1 d D . . H15A H 0.8080 0.2036 0.7630 0.036 Uiso 1 1 calc R . . C16 C 0.7598(3) 0.1192(2) 0.8300(2) 0.0251(8) Uani 1 1 d D . . H16A H 0.6890 0.1595 0.8334 0.030 Uiso 1 1 calc R . . C17 C 0.7029(2) 0.0039(2) 0.8607(2) 0.0236(8) Uani 1 1 d . . . H17 H 0.6695 0.0389 0.9164 0.028 Uiso 1 1 calc R . . C18 C 0.6265(3) 0.0274(2) 0.8181(2) 0.0257(8) Uani 1 1 d . . . H18 H 0.6620 -0.0013 0.7605 0.031 Uiso 1 1 calc R . . C19 C 0.5524(3) -0.0100(3) 0.8557(2) 0.0285(8) Uani 1 1 d . . . H19 H 0.5124 0.0226 0.9119 0.034 Uiso 1 1 calc R . . C110 C 0.6066(3) -0.1138(3) 0.8566(2) 0.0295(8) Uani 1 1 d . . . H110 H 0.6438 -0.1467 0.8003 0.035 Uiso 1 1 calc R . . C111 C 0.6794(3) -0.1346(2) 0.9022(2) 0.0284(8) Uani 1 1 d . . . H11A H 0.7147 -0.2026 0.9024 0.034 Uiso 1 1 calc R . . H11B H 0.6425 -0.1038 0.9585 0.034 Uiso 1 1 calc R . . C112 C 0.7547(3) -0.1000(2) 0.8636(2) 0.0286(8) Uani 1 1 d . . . H112 H 0.7948 -0.1343 0.8079 0.034 Uiso 1 1 calc R . . C113 C 0.9062(3) 0.0240(3) 1.0227(3) 0.0498(11) Uani 1 1 d . . . H11C H 0.9057 -0.0039 0.9739 0.075 Uiso 1 1 calc R . . H11D H 0.8889 -0.0078 1.0675 0.075 Uiso 1 1 calc R . . H11E H 0.9728 0.0175 1.0146 0.075 Uiso 1 1 calc R . . C114 C 0.9363(3) 0.2335(3) 1.0401(2) 0.0502(11) Uani 1 1 d . . . H11F H 0.8753 0.2930 1.0536 0.075 Uiso 1 1 calc R . . H11G H 0.9942 0.2450 1.0263 0.075 Uiso 1 1 calc R . . H11H H 0.9351 0.1997 1.0863 0.075 Uiso 1 1 calc R . . O21 O 0.94709(19) 0.50016(18) 1.00215(15) 0.0378(6) Uani 1 1 d . . . O22 O 0.80668(19) 0.64470(18) 1.04903(15) 0.0371(6) Uani 1 1 d . . . O23 O 0.77348(18) 0.62460(17) 0.90275(14) 0.0312(6) Uani 1 1 d . A . O24 O 0.77997(17) 0.51941(16) 0.80880(14) 0.0276(5) Uani 1 1 d . A . O25 O 0.5777(2) 0.62394(17) 0.81149(16) 0.0371(6) Uani 1 1 d . . . H25 H 0.5544 0.6369 0.7736 0.056 Uiso 1 1 calc R . . O26 O 0.48926(18) 0.50758(19) 0.79431(14) 0.0345(6) Uani 1 1 d . A . H26 H 0.4284 0.5373 0.8208 0.052 Uiso 1 1 calc R . . N22A N 0.8867(5) 0.5360(4) 0.6417(4) 0.053(2) Uani 0.49 1 d PDU A 1 N23A N 0.9242(6) 0.4684(4) 0.5985(4) 0.0737(18) Uani 0.49 1 d PDU A 1 N32A N 0.8915(4) 0.2910(6) 0.6518(4) 0.043(2) Uani 0.49 1 d PD B 1 N33A N 0.9523(4) 0.2837(6) 0.6767(4) 0.0679(17) Uani 0.49 1 d PD B 1 C63A C 0.1626(6) 0.853(2) 0.5700(7) 0.045(5) Uani 0.49 1 d PD C 1 H63A H 0.1006 0.8796 0.6122 0.054 Uiso 0.49 1 calc PR C 1 C64A C 0.1654(7) 0.845(2) 0.4832(6) 0.062(3) Uani 0.49 1 d PD C 1 H64A H 0.1515 0.9057 0.4640 0.074 Uiso 0.49 1 calc PR C 1 H64B H 0.1129 0.8293 0.4801 0.074 Uiso 0.49 1 calc PR C 1 C65A C 0.2667(8) 0.7703(14) 0.4294(6) 0.071(2) Uani 0.49 1 d PD C 1 H65A H 0.2721 0.7084 0.4420 0.085 Uiso 0.49 1 calc PR C 1 C66A C 0.3488(7) 0.7809(5) 0.4500(4) 0.0507(12) Uani 0.49 1 d PD C 1 H66A H 0.4156 0.7331 0.4142 0.061 Uiso 0.49 1 calc PR C 1 N61A N 0.2905(7) 0.7676(8) 0.3418(5) 0.0830(19) Uani 0.49 1 d PDU C 1 N62A N 0.2244(6) 0.8038(5) 0.3139(4) 0.0714(18) Uani 0.49 1 d PDU C 1 N63A N 0.1708(6) 0.8278(6) 0.2782(5) 0.0882(19) Uani 0.49 1 d PDU C 1 N82A N 0.2439(4) 1.0488(4) 0.3110(4) 0.0477(18) Uani 0.49 1 d PD D 1 N83A N 0.2003(5) 1.0123(6) 0.3439(4) 0.0750(18) Uani 0.49 1 d PD D 1 N88A N 0.2207(2) 0.8877(6) 0.0563(4) 0.0471(15) Uani 0.49 1 d PDU E 1 N89A N 0.1375(3) 0.9134(7) 0.0711(5) 0.0764(19) Uani 0.49 1 d PDU E 1 N22B N 0.9023(4) 0.5652(5) 0.6229(3) 0.053(2) Uani 0.51 1 d PDU A 2 N23B N 0.9561(4) 0.5274(6) 0.5607(3) 0.0737(18) Uani 0.51 1 d PDU A 2 N32B N 0.8733(4) 0.3324(4) 0.6391(4) 0.043(2) Uani 0.51 1 d PD B 2 N33B N 0.9145(5) 0.3711(5) 0.6493(4) 0.0679(17) Uani 0.51 1 d PD B 2 C63B C 0.1621(5) 0.872(2) 0.5750(6) 0.045(5) Uani 0.51 1 d PD C 2 H63B H 0.1057 0.9137 0.6183 0.054 Uiso 0.51 1 calc PR C 2 C64B C 0.1524(7) 0.863(2) 0.4924(6) 0.062(3) Uani 0.51 1 d PD C 2 H64C H 0.1396 0.9219 0.4701 0.074 Uiso 0.51 1 calc PR C 2 H64D H 0.0959 0.8503 0.4968 0.074 Uiso 0.51 1 calc PR C 2 C65B C 0.2494(8) 0.7830(13) 0.4368(6) 0.071(2) Uani 0.51 1 d PD C 2 H65B H 0.2497 0.7228 0.4494 0.085 Uiso 0.51 1 calc PR C 2 C66B C 0.3388(6) 0.7832(5) 0.4490(4) 0.0507(12) Uani 0.51 1 d PD C 2 H66B H 0.4007 0.7325 0.4101 0.061 Uiso 0.51 1 calc PR C 2 N61B N 0.2596(8) 0.7882(7) 0.3476(5) 0.0830(19) Uani 0.51 1 d PDU C 2 N62B N 0.2254(6) 0.8625(6) 0.3252(4) 0.0714(18) Uani 0.51 1 d PDU C 2 N63B N 0.2018(7) 0.9285(7) 0.2967(5) 0.0882(19) Uani 0.51 1 d PDU C 2 N82B N 0.2279(4) 1.0992(5) 0.3350(3) 0.0477(18) Uani 0.51 1 d PD D 2 N83B N 0.1672(4) 1.1110(6) 0.3940(3) 0.0750(18) Uani 0.51 1 d PD D 2 N88B N 0.2236(3) 0.9143(5) 0.0659(4) 0.0471(15) Uani 0.51 1 d PDU E 2 N89B N 0.1421(3) 0.9685(5) 0.0904(5) 0.0764(19) Uani 0.51 1 d PDU E 2 N21 N 0.8360(3) 0.6107(2) 0.6834(2) 0.0539(10) Uani 1 1 d DU . . N24 N 0.5244(2) 0.3575(2) 0.89768(17) 0.0338(7) Uani 1 1 d . . . N25 N 0.4692(2) 0.3516(2) 0.86376(18) 0.0320(7) Uani 1 1 d . . . N26 N 0.4131(3) 0.3408(2) 0.84277(19) 0.0420(8) Uani 1 1 d . . . N27 N 0.8087(2) 0.3847(2) 0.91576(17) 0.0309(7) Uani 1 1 d . . . N28 N 0.8988(3) 0.3513(2) 0.87751(19) 0.0356(7) Uani 1 1 d . . . N29 N 0.9828(3) 0.3209(2) 0.8493(2) 0.0507(9) Uani 1 1 d . . . C21 C 0.8545(3) 0.5590(3) 0.9968(2) 0.0305(9) Uani 1 1 d . . . H21 H 0.8119 0.5273 1.0134 0.037 Uiso 1 1 calc R . . C22 C 0.8663(3) 0.5714(2) 0.9102(2) 0.0288(8) Uani 1 1 d . . . C23 C 0.9500(3) 0.5331(3) 0.8491(2) 0.0353(9) Uani 1 1 d . A . H23 H 1.0109 0.4994 0.8594 0.042 Uiso 1 1 calc R . . C24 C 0.9526(3) 0.5409(3) 0.7634(2) 0.0391(10) Uani 1 1 d . . . H24A H 0.9684 0.4802 0.7362 0.047 Uiso 1 1 calc R A . H24B H 1.0056 0.5573 0.7349 0.047 Uiso 1 1 calc R . . C25 C 0.8535(3) 0.6145(3) 0.7601(2) 0.0390(10) Uani 1 1 d D A . H25A H 0.8491 0.6768 0.7720 0.047 Uiso 1 1 calc R . . C26 C 0.7684(3) 0.6090(3) 0.8246(2) 0.0315(9) Uani 1 1 d . . . H26A H 0.7031 0.6564 0.8210 0.038 Uiso 1 1 calc R A . C27 C 0.6986(3) 0.5038(2) 0.8544(2) 0.0264(8) Uani 1 1 d . . . H27 H 0.6650 0.5437 0.9081 0.032 Uiso 1 1 calc R A . C28 C 0.6240(3) 0.5261(2) 0.8099(2) 0.0288(8) Uani 1 1 d . A . H28 H 0.6609 0.4952 0.7530 0.035 Uiso 1 1 calc R . . C29 C 0.5466(3) 0.4931(3) 0.8470(2) 0.0279(8) Uani 1 1 d . . . H29 H 0.5021 0.5306 0.9010 0.033 Uiso 1 1 calc R A . C210 C 0.5967(3) 0.3904(3) 0.8549(2) 0.0301(8) Uani 1 1 d . A . H210 H 0.6371 0.3524 0.8006 0.036 Uiso 1 1 calc R . . C211 C 0.6637(3) 0.3744(3) 0.9055(2) 0.0310(9) Uani 1 1 d . . . H21A H 0.6944 0.3081 0.9126 0.037 Uiso 1 1 calc R A . H21B H 0.6236 0.4122 0.9592 0.037 Uiso 1 1 calc R . . C212 C 0.7449(3) 0.4014(2) 0.8649(2) 0.0266(8) Uani 1 1 d . A . H212 H 0.7862 0.3621 0.8112 0.032 Uiso 1 1 calc R . . C213 C 0.9403(3) 0.4693(3) 1.0793(2) 0.0498(11) Uani 1 1 d . . . H21C H 0.9226 0.5208 1.1196 0.075 Uiso 1 1 calc R . . H21D H 1.0046 0.4175 1.0767 0.075 Uiso 1 1 calc R . . H21E H 0.8891 0.4486 1.0941 0.075 Uiso 1 1 calc R . . C214 C 0.8569(4) 0.7004(3) 1.0336(3) 0.0525(11) Uani 1 1 d . . . H21F H 0.9235 0.6653 1.0379 0.079 Uiso 1 1 calc R . . H21G H 0.8190 0.7573 1.0729 0.079 Uiso 1 1 calc R . . H21H H 0.8626 0.7168 0.9795 0.079 Uiso 1 1 calc R . . O31 O 0.9290(2) 0.1361(2) 0.27444(16) 0.0468(7) Uani 1 1 d . . . O32 O 0.81299(19) 0.2871(2) 0.27485(15) 0.0394(6) Uani 1 1 d . . . O33 O 0.76571(18) 0.30819(18) 0.44434(14) 0.0318(6) Uani 1 1 d . B . O34 O 0.78495(18) 0.41313(17) 0.51810(14) 0.0302(6) Uani 1 1 d . B . O35 O 0.57811(19) 0.49738(18) 0.62520(15) 0.0355(6) Uani 1 1 d . . . H35 H 0.5413 0.5173 0.6732 0.053 Uiso 1 1 calc R . . O36 O 0.49934(19) 0.68812(18) 0.68521(14) 0.0358(6) Uani 1 1 d . B . H36 H 0.4407 0.6999 0.6904 0.054 Uiso 1 1 calc R . . N31 N 0.8201(2) 0.2992(2) 0.63550(18) 0.0442(8) Uani 1 1 d D . . N34 N 0.5486(3) 0.8020(2) 0.56615(19) 0.0397(8) Uani 1 1 d U . . N35 N 0.4920(3) 0.8545(2) 0.6313(2) 0.0350(8) Uani 1 1 d U . . N36 N 0.4361(3) 0.9114(3) 0.6843(2) 0.0424(8) Uani 1 1 d U . . N37 N 0.8239(3) 0.5228(2) 0.39951(18) 0.0383(8) Uani 1 1 d . . . N38 N 0.9092(3) 0.4594(3) 0.3897(2) 0.0434(9) Uani 1 1 d . . . N39 N 0.9883(3) 0.4027(3) 0.3719(2) 0.0640(11) Uani 1 1 d . . . C31 C 0.8427(3) 0.2122(3) 0.3190(2) 0.0360(9) Uani 1 1 d . . . H31 H 0.7889 0.1930 0.3347 0.043 Uiso 1 1 calc R . . C32 C 0.8555(3) 0.2387(3) 0.3948(2) 0.0335(9) Uani 1 1 d . . . C33 C 0.9376(3) 0.1983(3) 0.4140(2) 0.0384(9) Uani 1 1 d . B . H33 H 0.9968 0.1519 0.3759 0.046 Uiso 1 1 calc R . . C34 C 0.9395(3) 0.2240(3) 0.4951(2) 0.0413(10) Uani 1 1 d . . . H34A H 0.9634 0.2711 0.4925 0.050 Uiso 1 1 calc R B . H34B H 0.9848 0.1684 0.5126 0.050 Uiso 1 1 calc R . . C35 C 0.8346(3) 0.2630(3) 0.5534(2) 0.0338(9) Uani 1 1 d D B . H35A H 0.8161 0.2113 0.5580 0.041 Uiso 1 1 calc R . . C36 C 0.7618(3) 0.3391(3) 0.5215(2) 0.0306(9) Uani 1 1 d . . . H36A H 0.6929 0.3608 0.5599 0.037 Uiso 1 1 calc R B . C37 C 0.7067(3) 0.5033(2) 0.5175(2) 0.0275(8) Uani 1 1 d . . . H37 H 0.6717 0.4973 0.4809 0.033 Uiso 1 1 calc R B . C38 C 0.6319(3) 0.5482(3) 0.6010(2) 0.0283(8) Uani 1 1 d . B . H38 H 0.6691 0.5441 0.6388 0.034 Uiso 1 1 calc R . . C39 C 0.5611(3) 0.6503(3) 0.6035(2) 0.0313(9) Uani 1 1 d . . . H39 H 0.5180 0.6542 0.5709 0.038 Uiso 1 1 calc R B . C310 C 0.6155(3) 0.7048(3) 0.5709(2) 0.0317(9) Uani 1 1 d . B . H310 H 0.6553 0.7046 0.6055 0.038 Uiso 1 1 calc R . . C311 C 0.6854(3) 0.6610(3) 0.4857(2) 0.0352(9) Uani 1 1 d . . . H31A H 0.6463 0.6629 0.4507 0.042 Uiso 1 1 calc R B . H31B H 0.7217 0.6970 0.4648 0.042 Uiso 1 1 calc R . . C312 C 0.7591(3) 0.5611(3) 0.4843(2) 0.0308(9) Uani 1 1 d . B . H312 H 0.8009 0.5601 0.5172 0.037 Uiso 1 1 calc R . . C313 C 0.8814(3) 0.3243(3) 0.2494(2) 0.0488(11) Uani 1 1 d . . . H31C H 0.8934 0.3434 0.2961 0.073 Uiso 1 1 calc R . . H31D H 0.8534 0.3783 0.2228 0.073 Uiso 1 1 calc R . . H31E H 0.9444 0.2767 0.2118 0.073 Uiso 1 1 calc R . . C314 C 0.9134(4) 0.0843(3) 0.2190(3) 0.0639(14) Uani 1 1 d . . . H31F H 0.8618 0.0673 0.2481 0.096 Uiso 1 1 calc R . . H31G H 0.9756 0.0277 0.1925 0.096 Uiso 1 1 calc R . . H31H H 0.8920 0.1225 0.1787 0.096 Uiso 1 1 calc R . . O41 O 0.8144(2) 0.7683(2) 0.27913(17) 0.0481(7) Uani 1 1 d . . . O42 O 0.9466(2) 0.80340(19) 0.25059(15) 0.0401(6) Uani 1 1 d . . . O43 O 0.77482(18) 0.82606(18) 0.44324(15) 0.0362(6) Uani 1 1 d . . . O44 O 0.77738(18) 0.92887(17) 0.53274(14) 0.0308(6) Uani 1 1 d . . . O45 O 0.5761(2) 0.99536(18) 0.63905(14) 0.0361(6) Uani 1 1 d . . . H45 H 0.5406 1.0122 0.6876 0.054 Uiso 1 1 calc R . . O46 O 0.47908(19) 1.18794(19) 0.70065(14) 0.0374(6) Uani 1 1 d . . . H46 H 0.4191 1.2056 0.7056 0.056 Uiso 1 1 calc R . . N41 N 0.8369(3) 0.7930(3) 0.6291(2) 0.0529(9) Uani 1 1 d U . . N42 N 0.9100(3) 0.7690(3) 0.6492(2) 0.0585(10) Uani 1 1 d U . . N43 N 0.9726(4) 0.7481(3) 0.6770(2) 0.0772(13) Uani 1 1 d U . . N44 N 0.5088(3) 1.3100(2) 0.57986(19) 0.0410(8) Uani 1 1 d U . . N45 N 0.4579(3) 1.3663(3) 0.6432(2) 0.0388(8) Uani 1 1 d U . . N46 N 0.4059(3) 1.4270(3) 0.6930(2) 0.0553(10) Uani 1 1 d U . . N47 N 0.8026(2) 1.0412(2) 0.41319(18) 0.0390(8) Uani 1 1 d . . . N48 N 0.8918(3) 0.9979(3) 0.4063(2) 0.0438(9) Uani 1 1 d . . . N49 N 0.9754(3) 0.9585(3) 0.3932(3) 0.0668(12) Uani 1 1 d . . . C41 C 0.8548(3) 0.8203(3) 0.3056(2) 0.0351(9) Uani 1 1 d . . . H41 H 0.8076 0.8879 0.3111 0.042 Uiso 1 1 calc R . . C42 C 0.8675(3) 0.8004(3) 0.3854(2) 0.0373(9) Uani 1 1 d . . . C43 C 0.9509(3) 0.7684(3) 0.4027(2) 0.0389(10) Uani 1 1 d . . . H43 H 1.0118 0.7502 0.3603 0.047 Uiso 1 1 calc R . . C44 C 0.9531(3) 0.7594(3) 0.4875(2) 0.0417(10) Uani 1 1 d . . . H44A H 0.9676 0.8075 0.5063 0.050 Uiso 1 1 calc R . . H44B H 1.0068 0.6976 0.4884 0.050 Uiso 1 1 calc R . . C45 C 0.8534(3) 0.7710(3) 0.5437(2) 0.0408(10) Uani 1 1 d . . . H45A H 0.8505 0.7115 0.5355 0.049 Uiso 1 1 calc R . . C46 C 0.7696(3) 0.8473(3) 0.5230(2) 0.0356(9) Uani 1 1 d . . . H46A H 0.7048 0.8555 0.5610 0.043 Uiso 1 1 calc R . . C47 C 0.6926(3) 1.0148(3) 0.5313(2) 0.0275(8) Uani 1 1 d . . . H47 H 0.6597 1.0029 0.4954 0.033 Uiso 1 1 calc R . . C48 C 0.6187(3) 1.0561(3) 0.6147(2) 0.0288(8) Uani 1 1 d . . . H48 H 0.6552 1.0576 0.6516 0.035 Uiso 1 1 calc R . . C49 C 0.5386(3) 1.1541(3) 0.6186(2) 0.0289(8) Uani 1 1 d . . . H49 H 0.4962 1.1519 0.5875 0.035 Uiso 1 1 calc R . . C410 C 0.5833(3) 1.2173(3) 0.5844(2) 0.0336(9) Uani 1 1 d . . . H410 H 0.6217 1.2233 0.6178 0.040 Uiso 1 1 calc R . . C411 C 0.6528(3) 1.1754(3) 0.4989(2) 0.0344(9) Uani 1 1 d . . . H41A H 0.6818 1.2166 0.4764 0.041 Uiso 1 1 calc R . . H41B H 0.6149 1.1703 0.4653 0.041 Uiso 1 1 calc R . . C412 C 0.7360(3) 1.0794(3) 0.4974(2) 0.0301(8) Uani 1 1 d . . . H412 H 0.7749 1.0851 0.5304 0.036 Uiso 1 1 calc R . . C413 C 0.8730(4) 0.6692(3) 0.2665(3) 0.0603(13) Uani 1 1 d . . . H41C H 0.9328 0.6505 0.2195 0.090 Uiso 1 1 calc R . . H41D H 0.8340 0.6400 0.2574 0.090 Uiso 1 1 calc R . . H41E H 0.8925 0.6495 0.3138 0.090 Uiso 1 1 calc R . . C414 C 0.9388(3) 0.8384(3) 0.1775(2) 0.0495(11) Uani 1 1 d . . . H41F H 0.9203 0.8018 0.1480 0.074 Uiso 1 1 calc R . . H41G H 1.0030 0.8337 0.1450 0.074 Uiso 1 1 calc R . . H41H H 0.8877 0.9037 0.1894 0.074 Uiso 1 1 calc R . . O51 O 0.2935(3) 0.2663(2) 0.6851(2) 0.0327(9) Uani 0.75 1 d PD F 3 O52 O 0.1894(2) 0.2037(2) 0.67892(17) 0.0354(8) Uani 0.75 1 d PD F 3 O53 O 0.3476(3) 0.2435(6) 0.5110(2) 0.0328(9) Uani 0.75 1 d PD F 3 C51 C 0.2734(3) 0.2138(2) 0.6368(2) 0.0283(11) Uani 0.75 1 d PD F 3 H51C H 0.3317 0.1502 0.6206 0.034 Uiso 0.75 1 calc PR F 3 C52 C 0.2583(3) 0.2516(3) 0.5615(2) 0.0295(13) Uani 0.75 1 d PD F 3 C53 C 0.1743(3) 0.2839(4) 0.5456(3) 0.044(2) Uani 0.75 1 d PD F 3 H53A H 0.1165 0.2867 0.5842 0.053 Uiso 0.75 1 calc PR F 3 C54 C 0.1696(3) 0.3169(5) 0.4656(3) 0.0502(13) Uani 0.75 1 d PD F 3 H54A H 0.1212 0.3050 0.4490 0.060 Uiso 0.75 1 calc PR F 3 H54B H 0.1483 0.3845 0.4699 0.060 Uiso 0.75 1 calc PR F 3 C513 C 0.2168(5) 0.3611(3) 0.7113(4) 0.0476(15) Uani 0.75 1 d PD F 3 H51D H 0.2351 0.3933 0.7452 0.071 Uiso 0.75 1 calc PR F 3 H51E H 0.1538 0.3620 0.7419 0.071 Uiso 0.75 1 calc PR F 3 H51F H 0.2091 0.3926 0.6645 0.071 Uiso 0.75 1 calc PR F 3 C514 C 0.2054(4) 0.1421(3) 0.7378(3) 0.0400(13) Uani 0.75 1 d PD F 3 H51G H 0.1437 0.1391 0.7654 0.060 Uiso 0.75 1 calc PR F 3 H51H H 0.2254 0.1655 0.7768 0.060 Uiso 0.75 1 calc PR F 3 H51I H 0.2580 0.0798 0.7113 0.060 Uiso 0.75 1 calc PR F 3 O91 O 0.2883(10) 0.3015(7) 0.6876(8) 0.0327(9) Uani 0.25 1 d PD F 4 O92 O 0.3005(6) 0.1632(5) 0.6436(4) 0.0354(8) Uani 0.25 1 d PD F 4 O93 O 0.3400(8) 0.2540(19) 0.5147(6) 0.0328(9) Uani 0.25 1 d PD F 4 C91 C 0.2483(7) 0.2602(4) 0.6487(3) 0.0283(11) Uani 0.25 1 d PD F 4 H91A H 0.1783 0.2802 0.6839 0.034 Uiso 0.25 1 calc PR F 4 C92 C 0.2448(7) 0.2840(10) 0.5676(4) 0.0295(13) Uani 0.25 1 d PD F 4 C93 C 0.1642(7) 0.3176(17) 0.5466(5) 0.044(2) Uani 0.25 1 d PD F 4 H93A H 0.1014 0.3360 0.5866 0.053 Uiso 0.25 1 calc PR F 4 C94 C 0.1688(5) 0.3279(12) 0.4602(4) 0.0502(13) Uani 0.25 1 d PD F 4 H94A H 0.1202 0.3124 0.4480 0.060 Uiso 0.25 1 calc PR F 4 H94B H 0.1517 0.3930 0.4518 0.060 Uiso 0.25 1 calc PR F 4 C913 C 0.2182(16) 0.3938(10) 0.7295(14) 0.0476(15) Uani 0.25 1 d PD F 4 H91B H 0.2519 0.4198 0.7523 0.071 Uiso 0.25 1 calc PR F 4 H91C H 0.1643 0.3913 0.7726 0.071 Uiso 0.25 1 calc PR F 4 H91D H 0.1905 0.4333 0.6920 0.071 Uiso 0.25 1 calc PR F 4 C914 C 0.2822(11) 0.1303(7) 0.7195(6) 0.0400(13) Uani 0.25 1 d PD F 4 H91E H 0.3220 0.0624 0.7117 0.060 Uiso 0.25 1 calc PR F 4 H91F H 0.2114 0.1472 0.7423 0.060 Uiso 0.25 1 calc PR F 4 H91G H 0.3008 0.1587 0.7563 0.060 Uiso 0.25 1 calc PR F 4 O54 O 0.33136(18) 0.36565(17) 0.43371(14) 0.0310(6) Uani 1 1 d . . . O55 O 0.53728(19) 0.26637(17) 0.32618(14) 0.0323(6) Uani 1 1 d . . . H55 H 0.5771 0.2540 0.2792 0.049 Uiso 1 1 calc R . . O56 O 0.62317(19) 0.38352(19) 0.26816(14) 0.0353(6) Uani 1 1 d . . . H56 H 0.6814 0.3428 0.2628 0.053 Uiso 1 1 calc R . . N51 N 0.2848(3) 0.2837(3) 0.32200(19) 0.0497(9) Uani 1 1 d . F . N52 N 0.2364(3) 0.3681(3) 0.3179(2) 0.0509(10) Uani 1 1 d . . . N53 N 0.1978(4) 0.4411(3) 0.3045(2) 0.0753(13) Uani 1 1 d . . . N54 N 0.5793(3) 0.5373(2) 0.3883(2) 0.0450(9) Uani 1 1 d D . . N55 N 0.6354(2) 0.54282(15) 0.3239(2) 0.0383(8) Uani 1 1 d D . . N56 N 0.6910(3) 0.5524(2) 0.2729(2) 0.0457(9) Uani 1 1 d D . . N57 N 0.2953(3) 0.5052(2) 0.55227(19) 0.0459(9) Uani 1 1 d . . . N58 N 0.2114(3) 0.5234(3) 0.5588(2) 0.0555(11) Uani 1 1 d . . . N59 N 0.1303(3) 0.5418(3) 0.5738(3) 0.0858(16) Uani 1 1 d . . . C55 C 0.2721(3) 0.2636(3) 0.4055(2) 0.0418(10) Uani 1 1 d D . . H55A H 0.2882 0.1965 0.4032 0.050 Uiso 1 1 calc R F 3 C56 C 0.3501(3) 0.2727(3) 0.4339(2) 0.0336(9) Uani 1 1 d D F . H56A H 0.4175 0.2321 0.3944 0.040 Uiso 1 1 calc R G 3 C57 C 0.4121(3) 0.3839(2) 0.4349(2) 0.0276(8) Uani 1 1 d . . . H57 H 0.4462 0.3456 0.4714 0.033 Uiso 1 1 calc R . . C58 C 0.4873(3) 0.3634(3) 0.3509(2) 0.0273(8) Uani 1 1 d . . . H58 H 0.4508 0.3945 0.3133 0.033 Uiso 1 1 calc R . . C59 C 0.5612(3) 0.3996(3) 0.3501(2) 0.0303(8) Uani 1 1 d . . . H59 H 0.6033 0.3638 0.3828 0.036 Uiso 1 1 calc R . . C510 C 0.5097(3) 0.5027(3) 0.3825(2) 0.0314(9) Uani 1 1 d D . . H510 H 0.4711 0.5391 0.3478 0.038 Uiso 1 1 calc R . . C511 C 0.4393(3) 0.5194(3) 0.4675(2) 0.0365(9) Uani 1 1 d . . . H51A H 0.4049 0.5865 0.4889 0.044 Uiso 1 1 calc R . . H51B H 0.4778 0.4850 0.5023 0.044 Uiso 1 1 calc R . . C512 C 0.3627(3) 0.4868(3) 0.4681(2) 0.0324(9) Uani 1 1 d . . . H512 H 0.3225 0.5237 0.4345 0.039 Uiso 1 1 calc R . . O61 O 0.3100(2) 0.74195(19) 0.69047(18) 0.0512(8) Uani 1 1 d . C . O62 O 0.1684(2) 0.8861(2) 0.72476(18) 0.0508(7) Uani 1 1 d . C . O63 O 0.3399(2) 0.76999(19) 0.53034(18) 0.0492(7) Uani 1 1 d D . . O64 O 0.33457(19) 0.86917(19) 0.43441(15) 0.0369(6) Uani 1 1 d D . . O65 O 0.5342(2) 0.76295(18) 0.32702(15) 0.0420(7) Uani 1 1 d . C . H65 H 0.5749 0.7477 0.2802 0.063 Uiso 1 1 calc R . . O66 O 0.63034(19) 0.8732(2) 0.26319(14) 0.0383(6) Uani 1 1 d . . . H66 H 0.6867 0.8279 0.2561 0.058 Uiso 1 1 calc R . . N64 N 0.5981(3) 1.0222(3) 0.38166(19) 0.0443(9) Uani 1 1 d . C . N65 N 0.6438(2) 1.0393(2) 0.31904(19) 0.0332(7) Uani 1 1 d . . . N66 N 0.6918(3) 1.0569(2) 0.2675(2) 0.0422(8) Uani 1 1 d . . . N67 N 0.3092(2) 1.0036(2) 0.55322(18) 0.0393(8) Uani 1 1 d . C . N68 N 0.2204(3) 1.0409(2) 0.5625(2) 0.0462(9) Uani 1 1 d . . . N69 N 0.1350(3) 1.0767(3) 0.5788(3) 0.0755(13) Uani 1 1 d . . . C61 C 0.2603(3) 0.8310(3) 0.6671(3) 0.0461(11) Uani 1 1 d . . . H61 H 0.3023 0.8631 0.6626 0.055 Uiso 1 1 calc R C . C62 C 0.2472(3) 0.8228(3) 0.5870(3) 0.0426(10) Uani 1 1 d D C . C67 C 0.4175(3) 0.8836(3) 0.4348(2) 0.0326(9) Uani 1 1 d . C . H67 H 0.4513 0.8437 0.4707 0.039 Uiso 1 1 calc R . . C68 C 0.4918(3) 0.8599(3) 0.3498(2) 0.0313(9) Uani 1 1 d . . . H68 H 0.4549 0.8926 0.3129 0.038 Uiso 1 1 calc R C . C69 C 0.5703(3) 0.8905(3) 0.3458(2) 0.0325(9) Uani 1 1 d . C . H69 H 0.6130 0.8527 0.3774 0.039 Uiso 1 1 calc R . . C610 C 0.5240(3) 0.9926(3) 0.3781(2) 0.0332(9) Uani 1 1 d . . . H610 H 0.4852 1.0309 0.3442 0.040 Uiso 1 1 calc R C . C611 C 0.4547(3) 1.0115(3) 0.4645(2) 0.0328(9) Uani 1 1 d . C . H61A H 0.4936 0.9747 0.4982 0.039 Uiso 1 1 calc R . . H61B H 0.4246 1.0782 0.4859 0.039 Uiso 1 1 calc R . . C612 C 0.3735(3) 0.9857(3) 0.4682(2) 0.0321(9) Uani 1 1 d . . . H612 H 0.3324 1.0251 0.4362 0.038 Uiso 1 1 calc R C . C613 C 0.1778(4) 0.9117(3) 0.7972(3) 0.0641(13) Uani 1 1 d . . . H61C H 0.2138 0.8555 0.8184 0.096 Uiso 1 1 calc R C . H61D H 0.1115 0.9494 0.8363 0.096 Uiso 1 1 calc R . . H61E H 0.2146 0.9478 0.7869 0.096 Uiso 1 1 calc R . . C614 C 0.2617(4) 0.6854(3) 0.6961(3) 0.0596(13) Uani 1 1 d . . . H61F H 0.1931 0.7198 0.7325 0.089 Uiso 1 1 calc R C . H61G H 0.2974 0.6285 0.7168 0.089 Uiso 1 1 calc R . . H61H H 0.2615 0.6689 0.6429 0.089 Uiso 1 1 calc R . . O71 O 0.3011(2) 0.6078(2) -0.10132(16) 0.0448(7) Uani 1 1 d . . . O72 O 0.1452(2) 0.6155(2) -0.04258(17) 0.0495(7) Uani 1 1 d . . . O73 O 0.34430(18) 0.55151(18) 0.03650(16) 0.0415(7) Uani 1 1 d . . . O74 O 0.34786(18) 0.45810(18) 0.13680(14) 0.0325(6) Uani 1 1 d . . . O75 O 0.54782(19) 0.39104(18) 0.13699(15) 0.0338(6) Uani 1 1 d . . . H75 H 0.5820 0.3769 0.1677 0.051 Uiso 1 1 calc R . . O76 O 0.64454(18) 0.20059(19) 0.15380(14) 0.0371(6) Uani 1 1 d . . . H76 H 0.7042 0.1679 0.1253 0.056 Uiso 1 1 calc R . . N71 N 0.3094(3) 0.5968(3) 0.2524(3) 0.0638(12) Uani 1 1 d . . . N72 N 0.2463(3) 0.6101(3) 0.3139(3) 0.0581(10) Uani 1 1 d . . . N73 N 0.1885(4) 0.6266(4) 0.3778(3) 0.0784(14) Uani 1 1 d . . . N74 N 0.6114(3) 0.0747(2) 0.05655(19) 0.0439(9) Uani 1 1 d U . . N75 N 0.6644(3) 0.0182(2) 0.09148(19) 0.0376(8) Uani 1 1 d U . . N76 N 0.7168(3) -0.0417(3) 0.1142(2) 0.0493(9) Uani 1 1 d U . . N77 N 0.3120(3) 0.3397(3) 0.0484(2) 0.0432(8) Uani 1 1 d . . . N78 N 0.2250(3) 0.3882(3) 0.0920(2) 0.0480(9) Uani 1 1 d . . . N79 N 0.1427(3) 0.4318(3) 0.1265(3) 0.0688(12) Uani 1 1 d . . . C71 C 0.2439(3) 0.5732(3) -0.0454(2) 0.0399(10) Uani 1 1 d . . . H71 H 0.2729 0.5049 -0.0631 0.048 Uiso 1 1 calc R . . C72 C 0.2466(3) 0.5869(3) 0.0385(2) 0.0366(9) Uani 1 1 d . . . C73 C 0.1691(3) 0.6228(3) 0.1040(3) 0.0445(10) Uani 1 1 d . . . H73 H 0.1046 0.6450 0.0997 0.053 Uiso 1 1 calc R . . C74 C 0.1783(3) 0.6303(3) 0.1860(3) 0.0497(11) Uani 1 1 d . . . H74A H 0.1658 0.5828 0.2157 0.060 Uiso 1 1 calc R . . H74B H 0.1284 0.6925 0.2168 0.060 Uiso 1 1 calc R . . C75 C 0.2821(3) 0.6156(3) 0.1768(3) 0.0523(12) Uani 1 1 d . . . H75A H 0.2867 0.6729 0.1604 0.063 Uiso 1 1 calc R . . C76 C 0.3590(3) 0.5349(3) 0.1130(2) 0.0377(9) Uani 1 1 d . . . H76A H 0.4270 0.5249 0.1092 0.045 Uiso 1 1 calc R . . C77 C 0.4283(2) 0.3696(3) 0.0963(2) 0.0263(8) Uani 1 1 d . . . H77 H 0.4616 0.3756 0.0404 0.032 Uiso 1 1 calc R . . C78 C 0.5039(3) 0.3313(3) 0.1400(2) 0.0269(8) Uani 1 1 d . . . H78 H 0.4682 0.3322 0.1974 0.032 Uiso 1 1 calc R . . C79 C 0.5838(3) 0.2311(3) 0.1039(2) 0.0298(8) Uani 1 1 d . . . H79 H 0.6254 0.2305 0.0486 0.036 Uiso 1 1 calc R . . C710 C 0.5369(3) 0.1679(3) 0.1000(2) 0.0307(9) Uani 1 1 d . . . H710 H 0.5006 0.1631 0.1554 0.037 Uiso 1 1 calc R . . C711 C 0.4653(3) 0.2073(3) 0.0530(2) 0.0337(9) Uani 1 1 d . . . H71A H 0.4350 0.1663 0.0500 0.040 Uiso 1 1 calc R . . H71B H 0.5018 0.2100 -0.0023 0.040 Uiso 1 1 calc R . . C712 C 0.3836(3) 0.3049(3) 0.0938(2) 0.0317(9) Uani 1 1 d . . . H712 H 0.3478 0.3016 0.1498 0.038 Uiso 1 1 calc R . . C713 C 0.2700(4) 0.7045(3) -0.0834(3) 0.0634(13) Uani 1 1 d . . . H71C H 0.2014 0.7406 -0.0832 0.095 Uiso 1 1 calc R . . H71D H 0.3138 0.7220 -0.1241 0.095 Uiso 1 1 calc R . . H71E H 0.2734 0.7175 -0.0306 0.095 Uiso 1 1 calc R . . C714 C 0.1340(4) 0.5902(4) -0.1151(3) 0.0637(13) Uani 1 1 d . . . H71F H 0.1723 0.6083 -0.1602 0.096 Uiso 1 1 calc R . . H71G H 0.0635 0.6222 -0.1107 0.096 Uiso 1 1 calc R . . H71H H 0.1585 0.5228 -0.1241 0.096 Uiso 1 1 calc R . . O81 O 0.29507(19) 1.10662(18) -0.08376(15) 0.0361(6) Uani 1 1 d . . . O82 O 0.17567(18) 1.25668(18) -0.01844(15) 0.0348(6) Uani 1 1 d . . . O83 O 0.34660(18) 1.08028(17) 0.05816(14) 0.0306(6) Uani 1 1 d . D . O84 O 0.33467(18) 0.96909(17) 0.13930(14) 0.0294(6) Uani 1 1 d . D . O85 O 0.53895(19) 0.88990(17) 0.14247(15) 0.0312(6) Uani 1 1 d . . . H85 H 0.5712 0.8728 0.1745 0.047 Uiso 1 1 calc R . . O86 O 0.62211(18) 0.69800(18) 0.15801(14) 0.0318(6) Uani 1 1 d . D . H86 H 0.6826 0.6783 0.1317 0.048 Uiso 1 1 calc R . . N81 N 0.2998(2) 1.0784(2) 0.27670(18) 0.0440(9) Uani 1 1 d D . . N84 N 0.5825(3) 0.5821(2) 0.05842(18) 0.0385(8) Uani 1 1 d . . . N85 N 0.6360(3) 0.5285(2) 0.09479(18) 0.0320(7) Uani 1 1 d . . . N86 N 0.6905(3) 0.4706(2) 0.11790(19) 0.0374(8) Uani 1 1 d . . . N87 N 0.3092(2) 0.8600(2) 0.03126(19) 0.0438(8) Uani 1 1 d DU . . C81 C 0.2656(3) 1.1796(3) -0.0224(2) 0.0309(8) Uani 1 1 d . . . H81 H 0.3183 1.2002 -0.0351 0.037 Uiso 1 1 calc R . . C82 C 0.2557(3) 1.1489(3) 0.0592(2) 0.0301(8) Uani 1 1 d . . . C83 C 0.1745(3) 1.1858(3) 0.1230(2) 0.0366(9) Uani 1 1 d . D . H83 H 0.1142 1.2321 0.1177 0.044 Uiso 1 1 calc R . . C84 C 0.1751(3) 1.1563(3) 0.2037(2) 0.0390(10) Uani 1 1 d . . . H84A H 0.1540 1.1072 0.2124 0.047 Uiso 1 1 calc R D . H84B H 0.1289 1.2100 0.2468 0.047 Uiso 1 1 calc R . . C85 C 0.2803(3) 1.1199(3) 0.2044(2) 0.0325(9) Uani 1 1 d D D . H85A H 0.2963 1.1731 0.2005 0.039 Uiso 1 1 calc R . . C86 C 0.3545(3) 1.0453(2) 0.1320(2) 0.0290(8) Uani 1 1 d . . . H86A H 0.4236 1.0251 0.1327 0.035 Uiso 1 1 calc R D . C87 C 0.4159(2) 0.8809(2) 0.0965(2) 0.0250(8) Uani 1 1 d . . . H87 H 0.4520 0.8897 0.0428 0.030 Uiso 1 1 calc R D . C88 C 0.4885(3) 0.8358(2) 0.1429(2) 0.0265(8) Uani 1 1 d . D . H88 H 0.4499 0.8375 0.1996 0.032 Uiso 1 1 calc R . . C89 C 0.5642(3) 0.7348(3) 0.1065(2) 0.0284(8) Uani 1 1 d . . . H89 H 0.6086 0.7332 0.0523 0.034 Uiso 1 1 calc R D . C810 C 0.5126(3) 0.6780(3) 0.0993(2) 0.0312(9) Uani 1 1 d . D . H810 H 0.4712 0.6765 0.1538 0.037 Uiso 1 1 calc R . . C811 C 0.4464(3) 0.7209(3) 0.0485(2) 0.0329(9) Uani 1 1 d . . . H81A H 0.4129 0.6833 0.0437 0.039 Uiso 1 1 calc R D . H81B H 0.4876 0.7207 -0.0060 0.039 Uiso 1 1 calc R . . C812 C 0.3680(3) 0.8211(2) 0.0861(2) 0.0298(8) Uani 1 1 d D D . H812 H 0.3231 0.8209 0.1394 0.036 Uiso 1 1 calc R . . C813 C 0.2267(3) 1.0693(3) -0.0734(3) 0.0459(11) Uani 1 1 d . . . H81C H 0.2131 1.0511 -0.0199 0.069 Uiso 1 1 calc R . . H81D H 0.2557 1.0147 -0.1141 0.069 Uiso 1 1 calc R . . H81E H 0.1644 1.1166 -0.0792 0.069 Uiso 1 1 calc R . . C814 C 0.1851(3) 1.3087(3) -0.0831(2) 0.0401(10) Uani 1 1 d . . . H81F H 0.2359 1.3279 -0.0848 0.060 Uiso 1 1 calc R . . H81G H 0.1211 1.3640 -0.0750 0.060 Uiso 1 1 calc R . . H81H H 0.2046 1.2699 -0.1337 0.060 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 O11 0.0385(15) 0.0394(16) 0.0284(15) 0.0112(12) -0.0143(12) -0.0178(13) O12 0.0356(14) 0.0493(17) 0.0339(15) 0.0028(12) -0.0145(11) -0.0254(13) O13 0.0293(13) 0.0352(14) 0.0227(13) 0.0037(11) -0.0100(10) -0.0173(11) O14 0.0287(13) 0.0254(13) 0.0288(14) 0.0061(11) -0.0080(10) -0.0158(11) O15 0.0391(15) 0.0242(14) 0.0389(16) 0.0092(11) -0.0246(12) -0.0135(12) O16 0.0314(14) 0.0408(16) 0.0241(13) 0.0062(11) -0.0127(11) -0.0184(12) N11 0.052(2) 0.0345(18) 0.0260(18) 0.0094(14) -0.0202(15) -0.0172(16) N12 0.049(2) 0.052(2) 0.038(2) 0.0020(18) -0.0246(17) -0.0180(18) N13 0.063(3) 0.061(3) 0.070(3) -0.017(2) -0.031(2) -0.011(2) N14 0.048(2) 0.044(2) 0.0301(18) 0.0130(15) -0.0181(15) -0.0335(17) N15 0.0348(19) 0.0320(18) 0.0299(18) 0.0062(14) -0.0095(15) -0.0172(15) N16 0.047(2) 0.043(2) 0.038(2) 0.0111(16) -0.0156(16) -0.0278(18) N17 0.0360(19) 0.040(2) 0.042(2) 0.0160(15) -0.0210(16) -0.0201(16) N18 0.039(2) 0.040(2) 0.050(2) 0.0045(16) -0.0189(18) -0.0151(17) N19 0.043(3) 0.100(4) 0.080(3) 0.004(3) -0.020(2) -0.029(2) C11 0.030(2) 0.035(2) 0.029(2) 0.0111(17) -0.0162(16) -0.0159(17) C12 0.034(2) 0.034(2) 0.030(2) 0.0098(17) -0.0160(17) -0.0189(18) C13 0.027(2) 0.038(2) 0.031(2) 0.0032(17) -0.0071(16) -0.0166(17) C14 0.038(2) 0.044(2) 0.021(2) 0.0044(17) -0.0054(16) -0.0213(19) C15 0.042(2) 0.027(2) 0.025(2) 0.0077(16) -0.0129(17) -0.0185(18) C16 0.0293(19) 0.026(2) 0.0244(19) 0.0087(15) -0.0150(15) -0.0127(16) C17 0.0258(18) 0.0254(19) 0.0219(19) 0.0091(15) -0.0084(14) -0.0137(15) C18 0.034(2) 0.024(2) 0.0219(19) 0.0021(15) -0.0105(15) -0.0153(16) C19 0.032(2) 0.034(2) 0.0191(19) 0.0043(16) -0.0075(15) -0.0157(17) C110 0.039(2) 0.035(2) 0.0198(19) 0.0056(16) -0.0095(16) -0.0221(18) C111 0.039(2) 0.024(2) 0.024(2) 0.0067(16) -0.0107(16) -0.0164(17) C112 0.032(2) 0.029(2) 0.026(2) 0.0081(16) -0.0133(16) -0.0127(17) C113 0.074(3) 0.033(3) 0.049(3) 0.014(2) -0.032(2) -0.023(2) C114 0.065(3) 0.063(3) 0.043(3) 0.006(2) -0.028(2) -0.040(3) O21 0.0346(15) 0.0372(16) 0.0362(16) 0.0053(12) -0.0150(12) -0.0100(13) O22 0.0350(15) 0.0349(16) 0.0358(15) -0.0007(12) -0.0095(11) -0.0128(12) O23 0.0296(14) 0.0324(14) 0.0321(15) 0.0054(11) -0.0137(11) -0.0126(12) O24 0.0290(13) 0.0271(14) 0.0303(14) 0.0067(11) -0.0110(10) -0.0153(11) O25 0.0478(16) 0.0259(14) 0.0478(18) 0.0116(12) -0.0321(13) -0.0157(12) O26 0.0322(14) 0.0497(17) 0.0291(14) 0.0119(12) -0.0167(11) -0.0212(13) N22A 0.052(3) 0.085(5) 0.037(3) 0.015(3) -0.025(3) -0.038(3) N23A 0.079(4) 0.096(5) 0.042(4) 0.012(3) -0.031(3) -0.031(4) N32A 0.049(3) 0.053(6) 0.027(3) 0.005(3) -0.008(2) -0.027(4) N33A 0.067(4) 0.101(5) 0.037(3) -0.004(3) -0.009(3) -0.045(4) C63A 0.038(3) 0.046(12) 0.068(4) 0.016(3) -0.020(2) -0.033(3) C64A 0.061(4) 0.085(10) 0.069(4) 0.018(4) -0.029(3) -0.054(5) C65A 0.084(5) 0.070(5) 0.073(4) -0.002(3) -0.018(4) -0.054(5) C66A 0.057(3) 0.038(3) 0.058(3) 0.000(2) -0.009(2) -0.029(2) N61A 0.110(6) 0.085(4) 0.058(3) -0.029(3) -0.030(3) -0.047(4) N62A 0.091(4) 0.082(5) 0.060(4) -0.009(3) -0.022(3) -0.058(4) N63A 0.112(5) 0.110(5) 0.052(4) 0.000(3) -0.020(3) -0.063(4) N82A 0.041(3) 0.062(6) 0.028(4) 0.004(3) -0.014(3) -0.012(4) N83A 0.061(4) 0.117(5) 0.045(4) 0.032(3) -0.029(3) -0.034(4) N88A 0.0371(17) 0.060(3) 0.055(2) 0.019(2) -0.0249(18) -0.026(2) N89A 0.041(3) 0.099(5) 0.086(4) 0.020(4) -0.026(3) -0.026(3) N22B 0.052(3) 0.085(5) 0.037(3) 0.015(3) -0.025(3) -0.038(3) N23B 0.079(4) 0.096(5) 0.042(4) 0.012(3) -0.031(3) -0.031(4) N32B 0.049(3) 0.053(6) 0.027(3) 0.005(3) -0.008(2) -0.027(4) N33B 0.067(4) 0.101(5) 0.037(3) -0.004(3) -0.009(3) -0.045(4) C63B 0.038(3) 0.046(12) 0.068(4) 0.016(3) -0.020(2) -0.033(3) C64B 0.061(4) 0.085(10) 0.069(4) 0.018(4) -0.029(3) -0.054(5) C65B 0.084(5) 0.070(5) 0.073(4) -0.002(3) -0.018(4) -0.054(5) C66B 0.057(3) 0.038(3) 0.058(3) 0.000(2) -0.009(2) -0.029(2) N61B 0.110(6) 0.085(4) 0.058(3) -0.029(3) -0.030(3) -0.047(4) N62B 0.091(4) 0.082(5) 0.060(4) -0.009(3) -0.022(3) -0.058(4) N63B 0.112(5) 0.110(5) 0.052(4) 0.000(3) -0.020(3) -0.063(4) N82B 0.041(3) 0.062(6) 0.028(4) 0.004(3) -0.014(3) -0.012(4) N83B 0.061(4) 0.117(5) 0.045(4) 0.032(3) -0.029(3) -0.034(4) N88B 0.0371(17) 0.060(3) 0.055(2) 0.019(2) -0.0249(18) -0.026(2) N89B 0.041(3) 0.099(5) 0.086(4) 0.020(4) -0.026(3) -0.026(3) N21 0.078(3) 0.049(2) 0.038(2) 0.0197(17) -0.0291(19) -0.027(2) N24 0.047(2) 0.045(2) 0.0230(17) 0.0097(14) -0.0141(15) -0.0309(17) N25 0.040(2) 0.0300(18) 0.0236(17) 0.0044(13) -0.0074(15) -0.0158(16) N26 0.050(2) 0.053(2) 0.035(2) 0.0086(16) -0.0160(16) -0.0331(19) N27 0.0291(18) 0.0325(18) 0.0261(17) 0.0054(14) -0.0108(14) -0.0089(14) N28 0.036(2) 0.0317(19) 0.040(2) 0.0076(15) -0.0160(17) -0.0147(16) N29 0.031(2) 0.046(2) 0.067(3) 0.0066(19) -0.0114(18) -0.0140(17) C21 0.025(2) 0.031(2) 0.037(2) 0.0024(17) -0.0113(16) -0.0133(17) C22 0.026(2) 0.026(2) 0.036(2) 0.0049(17) -0.0098(16) -0.0135(17) C23 0.036(2) 0.040(2) 0.035(2) 0.0055(18) -0.0125(18) -0.0221(19) C24 0.043(2) 0.045(2) 0.034(2) 0.0093(19) -0.0084(18) -0.028(2) C25 0.053(3) 0.038(2) 0.036(2) 0.0139(19) -0.0170(19) -0.029(2) C26 0.043(2) 0.028(2) 0.032(2) 0.0107(17) -0.0205(17) -0.0184(18) C27 0.0290(19) 0.029(2) 0.0228(19) 0.0065(15) -0.0078(15) -0.0147(16) C28 0.035(2) 0.026(2) 0.026(2) 0.0049(16) -0.0142(16) -0.0131(17) C29 0.029(2) 0.032(2) 0.0205(19) 0.0014(16) -0.0074(15) -0.0132(17) C210 0.036(2) 0.037(2) 0.020(2) 0.0079(16) -0.0078(16) -0.0198(18) C211 0.038(2) 0.037(2) 0.023(2) 0.0086(17) -0.0134(16) -0.0201(18) C212 0.036(2) 0.024(2) 0.0190(19) 0.0036(15) -0.0118(16) -0.0114(16) C213 0.056(3) 0.054(3) 0.042(3) 0.016(2) -0.025(2) -0.023(2) C214 0.076(3) 0.043(3) 0.047(3) 0.003(2) -0.021(2) -0.035(2) O31 0.0562(18) 0.0466(18) 0.0306(16) -0.0041(13) -0.0118(13) -0.0196(15) O32 0.0401(15) 0.0516(17) 0.0321(15) 0.0151(13) -0.0161(12) -0.0234(14) O33 0.0300(14) 0.0355(15) 0.0286(14) 0.0024(11) -0.0095(11) -0.0140(12) O34 0.0303(14) 0.0289(14) 0.0337(15) 0.0085(11) -0.0094(11) -0.0165(12) O35 0.0405(15) 0.0352(15) 0.0295(15) 0.0013(12) 0.0002(11) -0.0238(13) O36 0.0388(15) 0.0369(15) 0.0240(14) 0.0054(11) -0.0068(11) -0.0132(13) N31 0.060(2) 0.055(2) 0.0240(19) 0.0098(16) -0.0124(16) -0.0337(19) N34 0.060(2) 0.033(2) 0.0272(19) 0.0079(15) -0.0193(16) -0.0201(17) N35 0.047(2) 0.033(2) 0.040(2) 0.0172(17) -0.0243(17) -0.0246(17) N36 0.052(2) 0.042(2) 0.039(2) 0.0119(17) -0.0184(17) -0.0254(18) N37 0.040(2) 0.043(2) 0.0291(19) 0.0119(15) -0.0043(15) -0.0213(17) N38 0.044(2) 0.057(3) 0.034(2) 0.0067(18) -0.0084(17) -0.029(2) N39 0.038(2) 0.085(3) 0.052(3) 0.004(2) -0.0077(19) -0.018(2) C31 0.037(2) 0.044(3) 0.030(2) 0.0084(19) -0.0103(18) -0.022(2) C32 0.038(2) 0.034(2) 0.030(2) 0.0061(18) -0.0101(18) -0.0184(19) C33 0.036(2) 0.042(2) 0.030(2) 0.0036(18) -0.0129(18) -0.0099(19) C34 0.039(2) 0.045(3) 0.035(2) 0.0118(19) -0.0199(19) -0.012(2) C35 0.050(2) 0.035(2) 0.025(2) 0.0133(17) -0.0156(18) -0.0257(19) C36 0.033(2) 0.032(2) 0.027(2) 0.0033(17) -0.0052(16) -0.0187(18) C37 0.029(2) 0.030(2) 0.027(2) 0.0086(16) -0.0123(16) -0.0150(17) C38 0.032(2) 0.034(2) 0.027(2) 0.0113(17) -0.0143(16) -0.0199(18) C39 0.039(2) 0.036(2) 0.025(2) 0.0085(17) -0.0149(17) -0.0204(18) C310 0.044(2) 0.037(2) 0.024(2) 0.0113(17) -0.0204(17) -0.0207(19) C311 0.048(2) 0.039(2) 0.029(2) 0.0116(18) -0.0175(18) -0.026(2) C312 0.040(2) 0.037(2) 0.023(2) 0.0080(17) -0.0101(17) -0.0245(19) C313 0.064(3) 0.063(3) 0.033(2) 0.014(2) -0.015(2) -0.041(3) C314 0.099(4) 0.065(3) 0.037(3) -0.002(2) -0.022(3) -0.046(3) O41 0.0404(16) 0.059(2) 0.0432(17) -0.0043(14) -0.0141(13) -0.0216(15) O42 0.0400(15) 0.0477(17) 0.0335(16) 0.0124(13) -0.0146(12) -0.0196(13) O43 0.0340(14) 0.0383(15) 0.0332(15) -0.0028(12) -0.0068(11) -0.0169(12) O44 0.0361(14) 0.0298(15) 0.0301(14) 0.0059(11) -0.0108(11) -0.0184(12) O45 0.0472(16) 0.0378(15) 0.0259(14) 0.0029(12) 0.0001(12) -0.0294(13) O46 0.0369(15) 0.0444(16) 0.0241(14) 0.0034(12) -0.0097(11) -0.0135(14) N41 0.066(3) 0.058(2) 0.035(2) 0.0178(17) -0.0150(18) -0.030(2) N42 0.075(3) 0.061(3) 0.037(2) 0.0085(19) -0.014(2) -0.032(2) N43 0.090(3) 0.089(3) 0.047(3) 0.006(2) -0.031(2) -0.032(3) N44 0.060(2) 0.0320(19) 0.0284(19) 0.0102(15) -0.0221(17) -0.0148(17) N45 0.056(2) 0.033(2) 0.040(2) 0.0173(18) -0.0261(18) -0.0248(18) N46 0.080(3) 0.037(2) 0.043(2) 0.0026(18) -0.026(2) -0.019(2) N47 0.0310(19) 0.053(2) 0.0306(19) 0.0123(16) -0.0065(14) -0.0202(17) N48 0.045(3) 0.048(2) 0.043(2) 0.0200(17) -0.0133(18) -0.026(2) N49 0.039(2) 0.073(3) 0.078(3) 0.025(2) -0.012(2) -0.022(2) C41 0.024(2) 0.037(2) 0.039(2) -0.0006(18) -0.0114(17) -0.0088(17) C42 0.033(2) 0.039(2) 0.031(2) -0.0020(18) -0.0031(18) -0.0141(19) C43 0.033(2) 0.040(2) 0.038(2) 0.0045(19) -0.0133(18) -0.0118(19) C44 0.044(2) 0.038(2) 0.035(2) 0.0045(18) -0.0149(19) -0.0110(19) C45 0.052(3) 0.032(2) 0.036(2) 0.0014(18) -0.0137(19) -0.018(2) C46 0.042(2) 0.037(2) 0.029(2) 0.0025(18) -0.0062(17) -0.023(2) C47 0.029(2) 0.035(2) 0.0209(19) 0.0067(16) -0.0113(15) -0.0151(17) C48 0.035(2) 0.037(2) 0.024(2) 0.0085(17) -0.0117(16) -0.0234(18) C49 0.035(2) 0.038(2) 0.019(2) 0.0055(16) -0.0110(16) -0.0205(18) C410 0.043(2) 0.033(2) 0.030(2) 0.0098(17) -0.0198(18) -0.0172(19) C411 0.048(2) 0.041(2) 0.027(2) 0.0119(18) -0.0191(18) -0.027(2) C412 0.043(2) 0.041(2) 0.0177(19) 0.0095(16) -0.0115(16) -0.0278(19) C413 0.086(4) 0.053(3) 0.049(3) 0.004(2) -0.015(3) -0.043(3) C414 0.058(3) 0.052(3) 0.034(2) 0.013(2) -0.016(2) -0.022(2) O51 0.0442(18) 0.025(3) 0.0328(16) 0.005(2) -0.0165(13) -0.017(2) O52 0.0385(19) 0.039(2) 0.0259(18) 0.0127(15) -0.0083(14) -0.0172(16) O53 0.0302(15) 0.038(3) 0.0275(15) 0.0119(14) -0.0064(12) -0.0158(16) C51 0.028(3) 0.019(3) 0.035(3) 0.009(3) -0.012(2) -0.007(3) C52 0.032(3) 0.022(4) 0.031(2) 0.006(2) -0.0075(19) -0.012(3) C53 0.036(3) 0.066(6) 0.042(3) 0.029(3) -0.016(2) -0.030(3) C54 0.048(3) 0.083(4) 0.036(3) 0.027(2) -0.024(2) -0.038(3) C513 0.055(3) 0.040(5) 0.032(4) -0.005(3) -0.011(3) -0.010(4) C514 0.057(3) 0.036(3) 0.021(3) 0.007(2) -0.001(2) -0.024(3) O91 0.0442(18) 0.025(3) 0.0328(16) 0.005(2) -0.0165(13) -0.017(2) O92 0.0385(19) 0.039(2) 0.0259(18) 0.0127(15) -0.0083(14) -0.0172(16) O93 0.0302(15) 0.038(3) 0.0275(15) 0.0119(14) -0.0064(12) -0.0158(16) C91 0.028(3) 0.019(3) 0.035(3) 0.009(3) -0.012(2) -0.007(3) C92 0.032(3) 0.022(4) 0.031(2) 0.006(2) -0.0075(19) -0.012(3) C93 0.036(3) 0.066(6) 0.042(3) 0.029(3) -0.016(2) -0.030(3) C94 0.048(3) 0.083(4) 0.036(3) 0.027(2) -0.024(2) -0.038(3) C913 0.055(3) 0.040(5) 0.032(4) -0.005(3) -0.011(3) -0.010(4) C914 0.057(3) 0.036(3) 0.021(3) 0.007(2) -0.001(2) -0.024(3) O54 0.0389(14) 0.0281(14) 0.0250(14) 0.0034(11) -0.0090(11) -0.0157(12) O55 0.0396(15) 0.0267(14) 0.0259(14) 0.0038(11) -0.0046(11) -0.0151(12) O56 0.0335(14) 0.0485(18) 0.0293(14) 0.0104(12) -0.0131(11) -0.0220(13) N51 0.075(3) 0.054(3) 0.028(2) 0.0029(18) -0.0155(17) -0.037(2) N52 0.081(3) 0.058(3) 0.026(2) 0.0101(19) -0.0143(18) -0.046(2) N53 0.113(4) 0.061(3) 0.052(3) 0.031(2) -0.027(2) -0.040(3) N54 0.069(2) 0.057(2) 0.031(2) 0.0140(17) -0.0233(18) -0.044(2) N55 0.050(2) 0.042(2) 0.038(2) 0.0109(17) -0.0250(18) -0.0282(18) N56 0.061(2) 0.050(2) 0.041(2) 0.0138(17) -0.0236(19) -0.035(2) N57 0.051(2) 0.044(2) 0.0276(19) -0.0030(16) 0.0001(17) -0.0170(19) N58 0.050(3) 0.042(2) 0.040(2) 0.0004(17) 0.009(2) -0.008(2) N59 0.055(3) 0.088(3) 0.064(3) 0.019(2) 0.011(2) -0.009(3) C55 0.067(3) 0.049(3) 0.031(2) 0.018(2) -0.025(2) -0.039(2) C56 0.046(2) 0.030(2) 0.024(2) 0.0039(17) -0.0078(17) -0.0193(18) C57 0.036(2) 0.029(2) 0.0199(19) 0.0078(16) -0.0125(16) -0.0154(17) C58 0.0287(19) 0.026(2) 0.026(2) 0.0042(16) -0.0101(15) -0.0116(16) C59 0.043(2) 0.033(2) 0.022(2) 0.0085(16) -0.0152(16) -0.0210(18) C510 0.050(2) 0.031(2) 0.025(2) 0.0127(16) -0.0225(17) -0.0223(19) C511 0.057(3) 0.032(2) 0.024(2) 0.0060(17) -0.0156(18) -0.022(2) C512 0.042(2) 0.030(2) 0.020(2) 0.0050(16) -0.0081(16) -0.0136(18) O61 0.0408(16) 0.0377(17) 0.064(2) 0.0189(14) -0.0121(14) -0.0125(14) O62 0.0374(16) 0.0524(19) 0.054(2) 0.0054(15) -0.0159(14) -0.0135(14) O63 0.0464(17) 0.0354(16) 0.062(2) 0.0132(14) -0.0082(15) -0.0217(14) O64 0.0441(16) 0.0395(16) 0.0306(15) 0.0004(12) -0.0095(12) -0.0241(13) O65 0.0579(18) 0.0334(16) 0.0269(15) 0.0014(12) -0.0042(13) -0.0209(14) O66 0.0387(15) 0.0543(19) 0.0231(14) 0.0065(12) -0.0086(11) -0.0235(14) N64 0.066(2) 0.066(2) 0.0238(19) 0.0179(17) -0.0233(17) -0.045(2) N65 0.046(2) 0.0290(18) 0.0263(19) 0.0045(15) -0.0165(16) -0.0162(16) N66 0.049(2) 0.042(2) 0.035(2) 0.0099(16) -0.0148(17) -0.0203(18) N67 0.0319(19) 0.045(2) 0.0293(19) -0.0124(15) -0.0016(14) -0.0129(16) N68 0.039(2) 0.037(2) 0.054(2) 0.0082(17) -0.0055(18) -0.0161(18) N69 0.044(3) 0.080(3) 0.084(3) 0.036(2) -0.009(2) -0.022(2) C61 0.033(2) 0.033(2) 0.070(3) 0.020(2) -0.015(2) -0.0154(19) C62 0.032(2) 0.043(3) 0.051(3) 0.013(2) -0.008(2) -0.020(2) C67 0.038(2) 0.037(2) 0.025(2) 0.0059(17) -0.0115(17) -0.0182(18) C68 0.035(2) 0.029(2) 0.028(2) 0.0007(17) -0.0133(16) -0.0118(17) C69 0.041(2) 0.036(2) 0.021(2) 0.0093(17) -0.0161(17) -0.0145(18) C610 0.045(2) 0.035(2) 0.030(2) 0.0082(17) -0.0222(18) -0.0215(19) C611 0.043(2) 0.033(2) 0.029(2) 0.0032(17) -0.0186(17) -0.0185(18) C612 0.038(2) 0.031(2) 0.025(2) 0.0044(16) -0.0128(17) -0.0125(17) C613 0.072(3) 0.056(3) 0.060(3) 0.006(3) -0.031(3) -0.020(3) C614 0.077(3) 0.038(3) 0.061(3) 0.014(2) -0.009(3) -0.033(2) O71 0.0398(16) 0.0472(18) 0.0471(17) 0.0148(13) -0.0087(13) -0.0236(14) O72 0.0366(17) 0.063(2) 0.0479(18) 0.0031(15) -0.0120(13) -0.0239(15) O73 0.0253(15) 0.0368(16) 0.0514(18) 0.0119(13) -0.0062(12) -0.0092(12) O74 0.0271(13) 0.0369(15) 0.0294(14) 0.0007(12) -0.0074(11) -0.0126(12) O75 0.0378(15) 0.0418(16) 0.0391(16) 0.0160(12) -0.0213(12) -0.0275(13) O76 0.0328(15) 0.0452(17) 0.0273(14) 0.0075(12) -0.0134(12) -0.0109(13) N71 0.037(2) 0.078(3) 0.054(3) -0.031(2) -0.016(2) -0.007(2) N72 0.057(3) 0.059(3) 0.061(3) -0.004(2) -0.030(2) -0.023(2) N73 0.084(3) 0.105(4) 0.069(3) 0.031(3) -0.046(3) -0.050(3) N74 0.066(2) 0.033(2) 0.0265(19) 0.0042(15) -0.0203(16) -0.0147(17) N75 0.055(2) 0.036(2) 0.0246(18) 0.0031(15) -0.0104(15) -0.0245(17) N76 0.066(2) 0.038(2) 0.037(2) 0.0077(16) -0.0211(18) -0.0159(18) N77 0.035(2) 0.057(2) 0.044(2) 0.0012(17) -0.0175(17) -0.0233(18) N78 0.043(2) 0.058(2) 0.054(2) -0.0006(19) -0.023(2) -0.028(2) N79 0.041(2) 0.076(3) 0.089(3) 0.000(2) -0.023(2) -0.024(2) C71 0.023(2) 0.035(2) 0.052(3) 0.0064(19) -0.0022(18) -0.0116(18) C72 0.026(2) 0.030(2) 0.045(3) 0.0069(18) -0.0058(18) -0.0090(17) C73 0.030(2) 0.044(3) 0.050(3) 0.005(2) -0.012(2) -0.0103(19) C74 0.030(2) 0.048(3) 0.053(3) -0.006(2) -0.008(2) -0.006(2) C75 0.035(2) 0.039(3) 0.068(3) -0.007(2) -0.009(2) -0.009(2) C76 0.029(2) 0.033(2) 0.047(3) 0.0011(19) -0.0117(18) -0.0103(18) C77 0.0261(19) 0.035(2) 0.0174(19) -0.0010(16) -0.0078(15) -0.0132(17) C78 0.031(2) 0.038(2) 0.0197(19) 0.0081(16) -0.0124(15) -0.0201(18) C79 0.033(2) 0.041(2) 0.0181(19) 0.0078(16) -0.0099(16) -0.0185(18) C710 0.039(2) 0.038(2) 0.0175(19) 0.0094(16) -0.0081(16) -0.0205(19) C711 0.040(2) 0.044(2) 0.026(2) 0.0074(18) -0.0134(17) -0.026(2) C712 0.031(2) 0.043(2) 0.024(2) 0.0082(17) -0.0104(16) -0.0191(18) C713 0.081(4) 0.056(3) 0.078(4) 0.030(3) -0.038(3) -0.045(3) C714 0.063(3) 0.088(4) 0.061(3) 0.012(3) -0.023(2) -0.050(3) O81 0.0404(15) 0.0397(16) 0.0316(15) 0.0014(12) -0.0162(12) -0.0188(13) O82 0.0327(14) 0.0355(15) 0.0328(15) 0.0108(12) -0.0135(11) -0.0113(12) O83 0.0277(14) 0.0294(14) 0.0318(15) 0.0082(11) -0.0144(11) -0.0080(11) O84 0.0288(13) 0.0274(14) 0.0346(15) 0.0057(11) -0.0129(11) -0.0138(11) O85 0.0381(15) 0.0299(14) 0.0375(16) 0.0117(11) -0.0234(12) -0.0189(12) O86 0.0317(14) 0.0346(15) 0.0257(14) 0.0034(11) -0.0125(11) -0.0107(12) N81 0.062(2) 0.053(2) 0.036(2) 0.0168(17) -0.0318(18) -0.0328(19) N84 0.051(2) 0.036(2) 0.0254(18) 0.0073(15) -0.0140(16) -0.0171(17) N85 0.045(2) 0.0300(19) 0.0264(18) 0.0029(15) -0.0095(16) -0.0230(17) N86 0.047(2) 0.031(2) 0.0347(19) 0.0059(16) -0.0117(16) -0.0194(17) N87 0.0399(17) 0.053(2) 0.048(2) 0.0118(16) -0.0264(16) -0.0228(16) C81 0.033(2) 0.033(2) 0.025(2) 0.0019(17) -0.0100(16) -0.0139(18) C82 0.028(2) 0.027(2) 0.032(2) -0.0014(17) -0.0102(16) -0.0099(17) C83 0.026(2) 0.041(2) 0.035(2) 0.0073(18) -0.0122(17) -0.0070(18) C84 0.035(2) 0.045(3) 0.027(2) 0.0056(18) -0.0082(17) -0.0115(19) C85 0.047(2) 0.028(2) 0.030(2) 0.0105(17) -0.0199(18) -0.0197(18) C86 0.032(2) 0.027(2) 0.033(2) 0.0092(17) -0.0161(17) -0.0137(17) C87 0.0272(19) 0.024(2) 0.0231(19) 0.0027(15) -0.0102(15) -0.0102(16) C88 0.030(2) 0.032(2) 0.0225(19) 0.0053(16) -0.0122(15) -0.0166(17) C89 0.036(2) 0.033(2) 0.0164(19) 0.0036(16) -0.0090(15) -0.0160(17) C810 0.041(2) 0.032(2) 0.023(2) 0.0057(16) -0.0093(16) -0.0207(18) C811 0.044(2) 0.035(2) 0.031(2) 0.0091(17) -0.0181(18) -0.0236(19) C812 0.035(2) 0.036(2) 0.026(2) 0.0080(17) -0.0146(16) -0.0195(18) C813 0.061(3) 0.042(3) 0.044(3) 0.004(2) -0.022(2) -0.028(2) C814 0.047(2) 0.041(2) 0.028(2) 0.0129(18) -0.0174(18) -0.014(2) _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_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O11 C11 . . 1.419(4) y O11 C113 . . 1.435(5) y O12 C11 . . 1.399(4) y O12 C114 . . 1.426(4) y O13 C12 . . 1.374(4) y O13 C16 . . 1.448(4) y O14 C16 . . 1.404(4) y O14 C17 . . 1.444(4) y O15 C18 . . 1.418(4) y O15 H15 . . 0.8400 ? O16 C19 . . 1.429(4) y O16 H16 . . 0.8400 ? N11 N12 . . 1.234(4) y N11 C15 . . 1.494(4) y N12 N13 . . 1.130(5) y N14 N15 . . 1.204(2) y N14 C110 . . 1.493(4) y N15 N16 . . 1.138(2) y N17 N18 . . 1.230(4) y N17 C112 . . 1.485(4) y N18 N19 . . 1.133(5) y C11 C12 . . 1.514(5) y C11 H11 . . 1.0000 ? C12 C13 . . 1.317(4) y C13 C14 . . 1.510(5) y C13 H13 . . 0.9500 ? C14 C15 . . 1.499(5) y C14 H14a . . 0.9900 ? C14 H14b . . 0.9900 ? C15 C16 . . 1.531(5) y C15 H15a . . 1.0000 ? C16 H16a . . 1.0000 ? C17 C112 . . 1.520(5) y C17 C18 . . 1.521(5) y C17 H17 . . 1.0000 ? C18 C19 . . 1.539(5) y C18 H18 . . 1.0000 ? C19 C110 . . 1.515(5) y C19 H19 . . 1.0000 ? C110 C111 . . 1.518(5) y C110 H110 . . 1.0000 ? C111 C112 . . 1.525(5) y C111 H11a . . 0.9900 ? C111 H11b . . 0.9900 ? C112 H112 . . 1.0000 ? C113 H11c . . 0.9800 ? C113 H11d . . 0.9800 ? C113 H11e . . 0.9800 ? C114 H11f . . 0.9800 ? C114 H11g . . 0.9800 ? C114 H11h . . 0.9800 ? O21 C21 . . 1.385(4) y O21 C213 . . 1.441(4) y O22 C21 . . 1.420(4) y O22 C214 . . 1.428(5) y O23 C22 . . 1.386(4) y O23 C26 . . 1.436(4) y O24 C26 . . 1.401(4) y O24 C27 . . 1.436(4) y O25 C28 . . 1.419(4) y O25 H25 . . 0.8400 ? O26 C29 . . 1.436(4) y O26 H26 . . 0.8400 ? N22a N23a . . 1.138(2) y N22a N21 . . 1.203(2) y N32a N33a . . 1.138(2) y N32a N31 . . 1.202(2) y C63a C62 . . 1.337(9) y C63a C64a . . 1.526(9) y C63a H63a . . 0.9500 ? C64a C65a . . 1.527(9) y C64a H64a . . 0.9900 ? C64a H64b . . 0.9900 ? C65a N61a . . 1.476(11) y C65a C66a . . 1.532(8) y C65a H65a . . 1.0000 ? C66a O64 . . 1.387(7) y C66a O63 . . 1.403(6) y C66a H66a . . 1.0000 ? N61a N62a . . 1.203(2) y N62a N63a . . 1.139(2) y N82a N83a . . 1.138(2) y N82a N81 . . 1.202(2) y N88a N89a . . 1.138(2) y N88a N87 . . 1.202(2) y N22b N23b . . 1.138(2) y N22b N21 . . 1.202(2) y N32b N33b . . 1.138(2) y N32b N31 . . 1.202(2) y C63b C62 . . 1.311(8) y C63b C64b . . 1.527(8) y C63b H63b . . 0.9500 ? C64b C65b . . 1.536(9) y C64b H64c . . 0.9900 ? C64b H64d . . 0.9900 ? C65b C66b . . 1.500(8) y C65b N61b . . 1.541(10) y C65b H65b . . 1.0000 ? C66b O64 . . 1.394(7) y C66b O63 . . 1.456(6) y C66b H66b . . 1.0000 ? N61b N62b . . 1.202(2) y N62b N63b . . 1.138(2) y N82b N83b . . 1.138(2) y N82b N81 . . 1.201(2) y N88b N89b . . 1.138(2) y N88b N87 . . 1.202(2) y N21 C25 . . 1.468(5) y N24 N25 . . 1.235(4) y N24 C210 . . 1.483(4) y N25 N26 . . 1.141(4) y N27 N28 . . 1.241(4) y N27 C212 . . 1.484(4) y N28 N29 . . 1.137(4) y C21 C22 . . 1.509(5) y C21 H21 . . 1.0000 ? C22 C23 . . 1.319(5) y C23 C24 . . 1.508(5) y C23 H23 . . 0.9500 ? C24 C25 . . 1.514(6) y C24 H24a . . 0.9900 ? C24 H24b . . 0.9900 ? C25 C26 . . 1.526(5) y C25 H25a . . 1.0000 ? C26 H26a . . 1.0000 ? C27 C28 . . 1.523(5) y C27 C212 . . 1.525(5) y C27 H27 . . 1.0000 ? C28 C29 . . 1.529(5) y C28 H28 . . 1.0000 ? C29 C210 . . 1.521(5) y C29 H29 . . 1.0000 ? C210 C211 . . 1.523(5) y C210 H210 . . 1.0000 ? C211 C212 . . 1.524(5) y C211 H21a . . 0.9900 ? C211 H21b . . 0.9900 ? C212 H212 . . 1.0000 ? C213 H21c . . 0.9800 ? C213 H21d . . 0.9800 ? C213 H21e . . 0.9800 ? C214 H21f . . 0.9800 ? C214 H21g . . 0.9800 ? C214 H21h . . 0.9800 ? O31 C31 . . 1.373(4) y O31 C314 . . 1.438(5) y O32 C31 . . 1.417(4) y O32 C313 . . 1.430(4) y O33 C32 . . 1.382(4) y O33 C36 . . 1.430(4) y O34 C36 . . 1.401(4) y O34 C37 . . 1.441(4) y O35 C38 . . 1.415(4) y O35 H35 . . 0.8400 ? O36 C39 . . 1.434(4) y O36 H36 . . 0.8400 ? N31 C35 . . 1.480(4) y N34 N35 . . 1.254(4) y N34 C310 . . 1.478(5) y N35 N36 . . 1.141(4) y N37 N38 . . 1.244(5) y N37 C312 . . 1.488(4) y N38 N39 . . 1.124(5) y C31 C32 . . 1.505(5) y C31 H31 . . 1.0000 ? C32 C33 . . 1.322(5) y C33 C34 . . 1.505(5) y C33 H33 . . 0.9500 ? C34 C35 . . 1.513(5) y C34 H34a . . 0.9900 ? C34 H34b . . 0.9900 ? C35 C36 . . 1.513(5) y C35 H35a . . 1.0000 ? C36 H36a . . 1.0000 ? C37 C312 . . 1.522(4) y C37 C38 . . 1.523(5) y C37 H37 . . 1.0000 ? C38 C39 . . 1.524(5) y C38 H38 . . 1.0000 ? C39 C310 . . 1.498(5) y C39 H39 . . 1.0000 ? C310 C311 . . 1.523(5) y C310 H310 . . 1.0000 ? C311 C312 . . 1.515(5) y C311 H31a . . 0.9900 ? C311 H31b . . 0.9900 ? C312 H312 . . 1.0000 ? C313 H31c . . 0.9800 ? C313 H31d . . 0.9800 ? C313 H31e . . 0.9800 ? C314 H31f . . 0.9800 ? C314 H31g . . 0.9800 ? C314 H31h . . 0.9800 ? O41 C41 . . 1.418(4) y O41 C413 . . 1.431(5) y O42 C41 . . 1.397(4) y O42 C414 . . 1.424(4) y O43 C42 . . 1.397(4) y O43 C46 . . 1.422(4) y O44 C46 . . 1.399(4) y O44 C47 . . 1.451(4) y O45 C48 . . 1.427(4) y O45 H45 . . 0.8400 ? O46 C49 . . 1.424(4) y O46 H46 . . 0.8400 ? N41 N42 . . 1.213(5) y N41 C45 . . 1.469(5) y N42 N43 . . 1.154(5) y N44 N45 . . 1.247(5) y N44 C410 . . 1.463(5) y N45 N46 . . 1.130(4) y N47 N48 . . 1.237(5) y N47 C412 . . 1.485(4) y N48 N49 . . 1.135(5) y C41 C42 . . 1.497(5) y C41 H41 . . 1.0000 ? C42 C43 . . 1.321(5) y C43 C44 . . 1.515(5) y C43 H43 . . 0.9500 ? C44 C45 . . 1.528(5) y C44 H44a . . 0.9900 ? C44 H44b . . 0.9900 ? C45 C46 . . 1.502(5) y C45 H45a . . 1.0000 ? C46 H46a . . 1.0000 ? C47 C48 . . 1.509(5) y C47 C412 . . 1.527(5) y C47 H47 . . 1.0000 ? C48 C49 . . 1.516(5) y C48 H48 . . 1.0000 ? C49 C410 . . 1.521(5) y C49 H49 . . 1.0000 ? C410 C411 . . 1.521(5) y C410 H410 . . 1.0000 ? C411 C412 . . 1.523(5) y C411 H41a . . 0.9900 ? C411 H41b . . 0.9900 ? C412 H412 . . 1.0000 ? C413 H41c . . 0.9800 ? C413 H41d . . 0.9800 ? C413 H41e . . 0.9800 ? C414 H41f . . 0.9800 ? C414 H41g . . 0.9800 ? C414 H41h . . 0.9800 ? O51 C51 . . 1.403(3) y O51 C513 . . 1.438(4) y O52 C51 . . 1.403(3) y O52 C514 . . 1.438(4) y O53 C52 . . 1.383(4) y O53 C56 . . 1.435(4) y C51 C52 . . 1.503(5) y C51 H51c . . 1.0000 ? C52 C53 . . 1.316(4) y C53 C54 . . 1.519(5) y C53 H53a . . 0.9500 ? C54 C55 . . 1.502(6) y C54 H54a . . 0.9900 ? C54 H54b . . 0.9900 ? C513 H51d . . 0.9800 ? C513 H51e . . 0.9800 ? C513 H51f . . 0.9800 ? C514 H51g . . 0.9800 ? C514 H51h . . 0.9800 ? C514 H51i . . 0.9800 ? O91 C91 . . 1.403(3) y O91 C913 . . 1.438(4) y O92 C91 . . 1.403(3) y O92 C914 . . 1.438(4) y O93 C92 . . 1.383(4) y O93 C56 . . 1.435(4) y C91 C92 . . 1.493(8) y C91 H91a . . 1.0000 ? C92 C93 . . 1.317(4) y C93 C94 . . 1.519(6) y C93 H93a . . 0.9500 ? C94 C55 . . 1.502(6) y C94 H94a . . 0.9900 ? C94 H94b . . 0.9900 ? C913 H91b . . 0.9800 ? C913 H91c . . 0.9800 ? C913 H91d . . 0.9800 ? C914 H91e . . 0.9800 ? C914 H91f . . 0.9800 ? C914 H91g . . 0.9800 ? O54 C56 . . 1.402(4) y O54 C57 . . 1.445(4) y O55 C58 . . 1.409(4) y O55 H55 . . 0.8400 ? O56 C59 . . 1.436(4) y O56 H56 . . 0.8400 ? N51 N52 . . 1.252(5) y N51 C55 . . 1.483(5) y N52 N53 . . 1.127(5) y N54 N55 . . 1.251(5) y N54 C510 . . 1.474(5) y N55 N56 . . 1.125(4) y N57 N58 . . 1.200(5) y N57 C512 . . 1.490(5) y N58 N59 . . 1.129(5) y C55 C56 . . 1.531(5) y C55 H55a . . 1.0000 ? C56 H56a . . 1.0000 ? C57 C512 . . 1.522(5) y C57 C58 . . 1.530(5) y C57 H57 . . 1.0000 ? C58 C59 . . 1.527(5) y C58 H58 . . 1.0000 ? C59 C510 . . 1.519(5) y C59 H59 . . 1.0000 ? C510 C511 . . 1.522(5) y C510 H510 . . 1.0000 ? C511 C512 . . 1.526(5) y C511 H51a . . 0.9900 ? C511 H51b . . 0.9900 ? C512 H512 . . 1.0000 ? O61 C614 . . 1.422(5) y O61 C61 . . 1.434(5) y O62 C61 . . 1.390(5) y O62 C613 . . 1.416(5) y O63 C62 . . 1.384(5) y O64 C67 . . 1.440(4) y O65 C68 . . 1.411(4) y O65 H65 . . 0.8400 ? O66 C69 . . 1.434(4) y O66 H66 . . 0.8400 ? N64 N65 . . 1.237(4) y N64 C610 . . 1.472(5) y N65 N66 . . 1.128(4) y N67 N68 . . 1.220(5) y N67 C612 . . 1.488(4) y N68 N69 . . 1.153(5) y C61 C62 . . 1.506(6) y C61 H61 . . 1.0000 ? C67 C612 . . 1.521(5) y C67 C68 . . 1.531(5) y C67 H67 . . 1.0000 ? C68 C69 . . 1.519(5) y C68 H68 . . 1.0000 ? C69 C610 . . 1.512(5) y C69 H69 . . 1.0000 ? C610 C611 . . 1.531(5) y C610 H610 . . 1.0000 ? C611 C612 . . 1.510(5) y C611 H61a . . 0.9900 ? C611 H61b . . 0.9900 ? C612 H612 . . 1.0000 ? C613 H61c . . 0.9800 ? C613 H61d . . 0.9800 ? C613 H61e . . 0.9800 ? C614 H61f . . 0.9800 ? C614 H61g . . 0.9800 ? C614 H61h . . 0.9800 ? O71 C713 . . 1.425(5) y O71 C71 . . 1.426(4) y O72 C71 . . 1.390(4) y O72 C714 . . 1.430(5) y O73 C72 . . 1.383(4) y O73 C76 . . 1.443(5) y O74 C76 . . 1.382(4) y O74 C77 . . 1.428(4) y O75 C78 . . 1.419(4) y O75 H75 . . 0.8400 ? O76 C79 . . 1.425(4) y O76 H76 . . 0.8400 ? N71 N72 . . 1.182(6) y N71 C75 . . 1.512(6) y N72 N73 . . 1.165(5) y N74 N75 . . 1.243(5) y N74 C710 . . 1.468(5) y N75 N76 . . 1.130(4) y N77 N78 . . 1.236(5) y N77 C712 . . 1.491(5) y N78 N79 . . 1.134(5) y C71 C72 . . 1.517(5) y C71 H71 . . 1.0000 ? C72 C73 . . 1.310(5) y C73 C74 . . 1.510(6) y C73 H73 . . 0.9500 ? C74 C75 . . 1.515(6) y C74 H74a . . 0.9900 ? C74 H74b . . 0.9900 ? C75 C76 . . 1.500(5) y C75 H75a . . 1.0000 ? C76 H76a . . 1.0000 ? C77 C712 . . 1.513(5) y C77 C78 . . 1.519(5) y C77 H77 . . 1.0000 ? C78 C79 . . 1.534(5) y C78 H78 . . 1.0000 ? C79 C710 . . 1.526(5) y C79 H79 . . 1.0000 ? C710 C711 . . 1.516(5) y C710 H710 . . 1.0000 ? C711 C712 . . 1.528(5) y C711 H71a . . 0.9900 ? C711 H71b . . 0.9900 ? C712 H712 . . 1.0000 ? C713 H71c . . 0.9800 ? C713 H71d . . 0.9800 ? C713 H71e . . 0.9800 ? C714 H71f . . 0.9800 ? C714 H71g . . 0.9800 ? C714 H71h . . 0.9800 ? O81 C81 . . 1.419(4) y O81 C813 . . 1.432(4) y O82 C81 . . 1.401(4) y O82 C814 . . 1.429(4) y O83 C82 . . 1.371(4) y O83 C86 . . 1.438(4) y O84 C86 . . 1.403(4) y O84 C87 . . 1.439(4) y O85 C88 . . 1.427(4) y O85 H85 . . 0.8400 ? O86 C89 . . 1.426(4) y O86 H86 . . 0.8400 ? N81 C85 . . 1.491(4) y N84 N85 . . 1.246(4) y N84 C810 . . 1.473(5) y N85 N86 . . 1.132(4) y N87 C812 . . 1.490(4) y C81 C82 . . 1.511(5) y C81 H81 . . 1.0000 ? C82 C83 . . 1.322(5) y C83 C84 . . 1.504(5) y C83 H83 . . 0.9500 ? C84 C85 . . 1.508(5) y C84 H84a . . 0.9900 ? C84 H84b . . 0.9900 ? C85 C86 . . 1.531(5) y C85 H85a . . 1.0000 ? C86 H86a . . 1.0000 ? C87 C812 . . 1.516(4) y C87 C88 . . 1.531(5) y C87 H87 . . 1.0000 ? C88 C89 . . 1.531(5) y C88 H88 . . 1.0000 ? C89 C810 . . 1.509(5) y C89 H89 . . 1.0000 ? C810 C811 . . 1.515(5) y C810 H810 . . 1.0000 ? C811 C812 . . 1.533(5) y C811 H81a . . 0.9900 ? C811 H81b . . 0.9900 ? C812 H812 . . 1.0000 ? C813 H81c . . 0.9800 ? C813 H81d . . 0.9800 ? C813 H81e . . 0.9800 ? C814 H81f . . 0.9800 ? C814 H81g . . 0.9800 ? C814 H81h . . 0.9800 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11 O11 C113 . . . 114.4(3) y C11 O12 C114 . . . 113.8(3) y C12 O13 C16 . . . 118.3(2) y C16 O14 C17 . . . 115.8(2) y C18 O15 H15 . . . 109.5 ? C19 O16 H16 . . . 109.5 ? N12 N11 C15 . . . 113.5(3) y N13 N12 N11 . . . 173.5(4) y N15 N14 C110 . . . 118.0(3) y N16 N15 N14 . . . 170.4(3) y N18 N17 C112 . . . 115.6(3) y N19 N18 N17 . . . 173.1(4) y O12 C11 O11 . . . 112.1(3) y O12 C11 C12 . . . 107.8(3) y O11 C11 C12 . . . 113.5(3) y O12 C11 H11 . . . 107.7 ? O11 C11 H11 . . . 107.7 ? C12 C11 H11 . . . 107.7 ? C13 C12 O13 . . . 125.7(3) y C13 C12 C11 . . . 125.4(3) y O13 C12 C11 . . . 108.9(3) y C12 C13 C14 . . . 120.3(3) y C12 C13 H13 . . . 119.9 ? C14 C13 H13 . . . 119.9 ? C15 C14 C13 . . . 107.6(3) y C15 C14 H14A . . . 110.2 ? C13 C14 H14A . . . 110.2 ? C15 C14 H14B . . . 110.2 ? C13 C14 H14B . . . 110.2 ? H14A C14 H14B . . . 108.5 ? N11 C15 C14 . . . 115.1(3) y N11 C15 C16 . . . 108.1(3) y C14 C15 C16 . . . 111.8(3) y N11 C15 H15A . . . 107.2 ? C14 C15 H15A . . . 107.2 ? C16 C15 H15A . . . 107.2 ? O14 C16 O13 . . . 110.6(3) y O14 C16 C15 . . . 107.4(3) y O13 C16 C15 . . . 111.5(3) y O14 C16 H16A . . . 109.1 ? O13 C16 H16A . . . 109.1 ? C15 C16 H16A . . . 109.1 ? O14 C17 C112 . . . 105.0(3) y O14 C17 C18 . . . 111.6(3) y C112 C17 C18 . . . 110.9(3) y O14 C17 H17 . . . 109.7 ? C112 C17 H17 . . . 109.7 ? C18 C17 H17 . . . 109.7 ? O15 C18 C17 . . . 109.2(3) y O15 C18 C19 . . . 109.5(3) y C17 C18 C19 . . . 111.4(3) y O15 C18 H18 . . . 108.9 ? C17 C18 H18 . . . 108.9 ? C19 C18 H18 . . . 108.9 ? O16 C19 C110 . . . 110.6(3) y O16 C19 C18 . . . 107.5(3) y C110 C19 C18 . . . 110.8(3) y O16 C19 H19 . . . 109.3 ? C110 C19 H19 . . . 109.3 ? C18 C19 H19 . . . 109.3 ? N14 C110 C19 . . . 111.5(3) y N14 C110 C111 . . . 107.2(3) y C19 C110 C111 . . . 110.0(3) y N14 C110 H110 . . . 109.4 ? C19 C110 H110 . . . 109.4 ? C111 C110 H110 . . . 109.4 ? C110 C111 C112 . . . 110.4(3) y C110 C111 H11A . . . 109.6 ? C112 C111 H11A . . . 109.6 ? C110 C111 H11B . . . 109.6 ? C112 C111 H11B . . . 109.6 ? H11A C111 H11B . . . 108.1 ? N17 C112 C17 . . . 110.3(3) y N17 C112 C111 . . . 107.1(3) y C17 C112 C111 . . . 111.1(3) y N17 C112 H112 . . . 109.4 ? C17 C112 H112 . . . 109.4 ? C111 C112 H112 . . . 109.4 ? O11 C113 H11C . . . 109.5 ? O11 C113 H11D . . . 109.5 ? H11C C113 H11D . . . 109.5 ? O11 C113 H11E . . . 109.5 ? H11C C113 H11E . . . 109.5 ? H11D C113 H11E . . . 109.5 ? O12 C114 H11F . . . 109.5 ? O12 C114 H11G . . . 109.5 ? H11F C114 H11G . . . 109.5 ? O12 C114 H11H . . . 109.5 ? H11F C114 H11H . . . 109.5 ? H11G C114 H11H . . . 109.5 ? C21 O21 C213 . . . 112.1(3) y C21 O22 C214 . . . 115.4(3) y C22 O23 C26 . . . 114.3(3) y C26 O24 C27 . . . 115.6(3) y C28 O25 H25 . . . 109.5 ? C29 O26 H26 . . . 109.5 ? N23A N22A N21 . . . 170.8(7) y N33A N32A N31 . . . 171.5(7) y C62 C63A C64A . . . 120.3(8) y C62 C63A H63A . . . 119.8 ? C64A C63A H63A . . . 119.8 ? C63A C64A C65A . . . 110.9(6) y C63A C64A H64A . . . 109.5 ? C65A C64A H64A . . . 109.5 ? C63A C64A H64B . . . 109.5 ? C65A C64A H64B . . . 109.5 ? H64A C64A H64B . . . 108.0 ? N61A C65A C64A . . . 118.0(8) y N61A C65A C66A . . . 106.3(8) y C64A C65A C66A . . . 109.2(7) y N61A C65A H65A . . . 107.6 ? C64A C65A H65A . . . 107.6 ? C66A C65A H65A . . . 107.6 ? O64 C66A O63 . . . 113.0(5) y O64 C66A C65A . . . 104.6(10) y O63 C66A C65A . . . 109.7(5) y O64 C66A H66A . . . 109.8 ? O63 C66A H66A . . . 109.8 ? C65A C66A H66A . . . 109.8 ? N62A N61A C65A . . . 119.8(7) y N63A N62A N61A . . . 169.9(7) y N83A N82A N81 . . . 172.3(7) y N89A N88A N87 . . . 172.2(7) y N23B N22B N21 . . . 171.1(7) y N33B N32B N31 . . . 172.2(7) y C62 C63B C64B . . . 120.7(6) y C62 C63B H63B . . . 119.6 ? C64B C63B H63B . . . 119.6 ? C63B C64B C65B . . . 109.0(6) y C63B C64B H64C . . . 109.9 ? C65B C64B H64C . . . 109.9 ? C63B C64B H64D . . . 109.9 ? C65B C64B H64D . . . 109.9 ? H64C C64B H64D . . . 108.3 ? C66B C65B C64B . . . 111.3(7) y C66B C65B N61B . . . 107.9(7) y C64B C65B N61B . . . 112.2(7) y C66B C65B H65B . . . 108.5 ? C64B C65B H65B . . . 108.5 ? N61B C65B H65B . . . 108.5 ? O64 C66B O63 . . . 109.4(5) y O64 C66B C65B . . . 107.4(10) y O63 C66B C65B . . . 111.7(5) y O64 C66B H66B . . . 109.4 ? O63 C66B H66B . . . 109.4 ? C65B C66B H66B . . . 109.4 ? N62B N61B C65B . . . 120.1(7) y N63B N62B N61B . . . 172.5(8) y N83B N82B N81 . . . 172.0(7) y N89B N88B N87 . . . 172.2(7) y N22B N21 C25 . . . 122.0(4) y N22A N21 C25 . . . 114.2(5) y N25 N24 C210 . . . 118.4(3) y N26 N25 N24 . . . 169.3(3) y N28 N27 C212 . . . 114.1(3) y N29 N28 N27 . . . 173.5(4) y O21 C21 O22 . . . 112.3(3) y O21 C21 C22 . . . 108.5(3) y O22 C21 C22 . . . 113.0(3) y O21 C21 H21 . . . 107.6 ? O22 C21 H21 . . . 107.6 ? C22 C21 H21 . . . 107.6 ? C23 C22 O23 . . . 123.9(3) y C23 C22 C21 . . . 126.5(3) y O23 C22 C21 . . . 109.4(3) y C22 C23 C24 . . . 122.5(4) y C22 C23 H23 . . . 118.7 ? C24 C23 H23 . . . 118.7 ? C23 C24 C25 . . . 110.7(3) y C23 C24 H24A . . . 109.5 ? C25 C24 H24A . . . 109.5 ? C23 C24 H24B . . . 109.5 ? C25 C24 H24B . . . 109.5 ? H24A C24 H24B . . . 108.1 ? N21 C25 C24 . . . 115.9(3) y N21 C25 C26 . . . 107.3(3) y C24 C25 C26 . . . 110.2(3) y N21 C25 H25A . . . 107.8 ? C24 C25 H25A . . . 107.8 ? C26 C25 H25A . . . 107.8 ? O24 C26 O23 . . . 110.7(3) y O24 C26 C25 . . . 106.3(3) y O23 C26 C25 . . . 110.3(3) y O24 C26 H26A . . . 109.8 ? O23 C26 H26A . . . 109.8 ? C25 C26 H26A . . . 109.8 ? O24 C27 C28 . . . 110.1(3) y O24 C27 C212 . . . 105.7(3) y C28 C27 C212 . . . 111.6(3) y O24 C27 H27 . . . 109.8 ? C28 C27 H27 . . . 109.8 ? C212 C27 H27 . . . 109.8 ? O25 C28 C27 . . . 106.8(3) y O25 C28 C29 . . . 110.8(3) y C27 C28 C29 . . . 112.5(3) y O25 C28 H28 . . . 108.9 ? C27 C28 H28 . . . 108.9 ? C29 C28 H28 . . . 108.9 ? O26 C29 C210 . . . 109.8(3) y O26 C29 C28 . . . 106.9(3) y C210 C29 C28 . . . 110.9(3) y O26 C29 H29 . . . 109.8 ? C210 C29 H29 . . . 109.8 ? C28 C29 H29 . . . 109.8 ? N24 C210 C29 . . . 112.7(3) y N24 C210 C211 . . . 105.4(3) y C29 C210 C211 . . . 109.4(3) y N24 C210 H210 . . . 109.8 ? C29 C210 H210 . . . 109.8 ? C211 C210 H210 . . . 109.8 ? C210 C211 C212 . . . 110.1(3) y C210 C211 H21A . . . 109.6 ? C212 C211 H21A . . . 109.6 ? C210 C211 H21B . . . 109.6 ? C212 C211 H21B . . . 109.6 ? H21A C211 H21B . . . 108.2 ? N27 C212 C211 . . . 108.6(3) y N27 C212 C27 . . . 109.8(3) y C211 C212 C27 . . . 110.2(3) y N27 C212 H212 . . . 109.4 ? C211 C212 H212 . . . 109.4 ? C27 C212 H212 . . . 109.4 ? O21 C213 H21C . . . 109.5 ? O21 C213 H21D . . . 109.5 ? H21C C213 H21D . . . 109.5 ? O21 C213 H21E . . . 109.5 ? H21C C213 H21E . . . 109.5 ? H21D C213 H21E . . . 109.5 ? O22 C214 H21F . . . 109.5 ? O22 C214 H21G . . . 109.5 ? H21F C214 H21G . . . 109.5 ? O22 C214 H21H . . . 109.5 ? H21F C214 H21H . . . 109.5 ? H21G C214 H21H . . . 109.5 ? C31 O31 C314 . . . 112.6(3) y C31 O32 C313 . . . 114.5(3) y C32 O33 C36 . . . 117.6(3) y C36 O34 C37 . . . 116.4(2) y C38 O35 H35 . . . 109.5 ? C39 O36 H36 . . . 109.5 ? N32B N31 C35 . . . 114.7(4) y N32A N31 C35 . . . 118.8(4) y N35 N34 C310 . . . 116.8(3) y N36 N35 N34 . . . 170.7(4) y N38 N37 C312 . . . 115.6(3) y N39 N38 N37 . . . 172.3(4) y O31 C31 O32 . . . 112.3(3) y O31 C31 C32 . . . 108.8(3) y O32 C31 C32 . . . 112.8(3) y O31 C31 H31 . . . 107.6 ? O32 C31 H31 . . . 107.6 ? C32 C31 H31 . . . 107.6 ? C33 C32 O33 . . . 124.6(3) y C33 C32 C31 . . . 125.9(3) y O33 C32 C31 . . . 109.4(3) y C32 C33 C34 . . . 121.5(3) y C32 C33 H33 . . . 119.3 ? C34 C33 H33 . . . 119.3 ? C33 C34 C35 . . . 107.8(3) y C33 C34 H34A . . . 110.1 ? C35 C34 H34A . . . 110.1 ? C33 C34 H34B . . . 110.1 ? C35 C34 H34B . . . 110.1 ? H34A C34 H34B . . . 108.5 ? N31 C35 C34 . . . 115.6(3) y N31 C35 C36 . . . 108.4(3) y C34 C35 C36 . . . 110.8(3) y N31 C35 H35A . . . 107.2 ? C34 C35 H35A . . . 107.2 ? C36 C35 H35A . . . 107.2 ? O34 C36 O33 . . . 110.6(3) y O34 C36 C35 . . . 107.3(3) y O33 C36 C35 . . . 112.3(3) y O34 C36 H36A . . . 108.9 ? O33 C36 H36A . . . 108.9 ? C35 C36 H36A . . . 108.9 ? O34 C37 C312 . . . 105.3(3) y O34 C37 C38 . . . 111.9(3) y C312 C37 C38 . . . 110.8(3) y O34 C37 H37 . . . 109.6 ? C312 C37 H37 . . . 109.6 ? C38 C37 H37 . . . 109.6 ? O35 C38 C37 . . . 108.3(3) y O35 C38 C39 . . . 110.5(3) y C37 C38 C39 . . . 112.0(3) y O35 C38 H38 . . . 108.6 ? C37 C38 H38 . . . 108.6 ? C39 C38 H38 . . . 108.6 ? O36 C39 C310 . . . 110.3(3) y O36 C39 C38 . . . 107.8(3) y C310 C39 C38 . . . 112.2(3) y O36 C39 H39 . . . 108.8 ? C310 C39 H39 . . . 108.8 ? C38 C39 H39 . . . 108.8 ? N34 C310 C39 . . . 113.2(3) y N34 C310 C311 . . . 106.0(3) y C39 C310 C311 . . . 110.1(3) y N34 C310 H310 . . . 109.2 ? C39 C310 H310 . . . 109.2 ? C311 C310 H310 . . . 109.2 ? C312 C311 C310 . . . 110.2(3) y C312 C311 H31A . . . 109.6 ? C310 C311 H31A . . . 109.6 ? C312 C311 H31B . . . 109.6 ? C310 C311 H31B . . . 109.6 ? H31A C311 H31B . . . 108.1 ? N37 C312 C311 . . . 107.2(3) y N37 C312 C37 . . . 110.6(3) y C311 C312 C37 . . . 111.6(3) y N37 C312 H312 . . . 109.1 ? C311 C312 H312 . . . 109.1 ? C37 C312 H312 . . . 109.1 ? O32 C313 H31C . . . 109.5 ? O32 C313 H31D . . . 109.5 ? H31C C313 H31D . . . 109.5 ? O32 C313 H31E . . . 109.5 ? H31C C313 H31E . . . 109.5 ? H31D C313 H31E . . . 109.5 ? O31 C314 H31F . . . 109.5 ? O31 C314 H31G . . . 109.5 ? H31F C314 H31G . . . 109.5 ? O31 C314 H31H . . . 109.5 ? H31F C314 H31H . . . 109.5 ? H31G C314 H31H . . . 109.5 ? C41 O41 C413 . . . 116.0(3) y C41 O42 C414 . . . 113.1(3) y C42 O43 C46 . . . 114.6(3) y C46 O44 C47 . . . 115.9(3) y C48 O45 H45 . . . 109.5 ? C49 O46 H46 . . . 109.5 ? N42 N41 C45 . . . 117.2(4) y N43 N42 N41 . . . 172.4(5) y N45 N44 C410 . . . 117.9(3) y N46 N45 N44 . . . 169.2(4) y N48 N47 C412 . . . 113.6(3) y N49 N48 N47 . . . 174.2(4) y O42 C41 O41 . . . 111.7(3) y O42 C41 C42 . . . 108.7(3) y O41 C41 C42 . . . 112.2(3) y O42 C41 H41 . . . 108.0 ? O41 C41 H41 . . . 108.0 ? C42 C41 H41 . . . 108.0 ? C43 C42 O43 . . . 123.0(3) y C43 C42 C41 . . . 127.2(3) y O43 C42 C41 . . . 109.7(3) y C42 C43 C44 . . . 122.5(3) y C42 C43 H43 . . . 118.8 ? C44 C43 H43 . . . 118.8 ? C43 C44 C45 . . . 110.6(3) y C43 C44 H44A . . . 109.5 ? C45 C44 H44A . . . 109.5 ? C43 C44 H44B . . . 109.5 ? C45 C44 H44B . . . 109.5 ? H44A C44 H44B . . . 108.1 ? N41 C45 C46 . . . 107.8(3) y N41 C45 C44 . . . 114.3(3) y C46 C45 C44 . . . 109.9(3) y N41 C45 H45A . . . 108.2 ? C46 C45 H45A . . . 108.2 ? C44 C45 H45A . . . 108.2 ? O44 C46 O43 . . . 111.0(3) y O44 C46 C45 . . . 107.0(3) y O43 C46 C45 . . . 111.1(3) y O44 C46 H46A . . . 109.2 ? O43 C46 H46A . . . 109.2 ? C45 C46 H46A . . . 109.2 ? O44 C47 C48 . . . 110.8(3) y O44 C47 C412 . . . 105.1(3) y C48 C47 C412 . . . 110.8(3) y O44 C47 H47 . . . 110.0 ? C48 C47 H47 . . . 110.0 ? C412 C47 H47 . . . 110.0 ? O45 C48 C47 . . . 107.0(3) y O45 C48 C49 . . . 110.8(3) y C47 C48 C49 . . . 112.7(3) y O45 C48 H48 . . . 108.7 ? C47 C48 H48 . . . 108.7 ? C49 C48 H48 . . . 108.7 ? O46 C49 C48 . . . 107.3(3) y O46 C49 C410 . . . 110.6(3) y C48 C49 C410 . . . 111.5(3) y O46 C49 H49 . . . 109.1 ? C48 C49 H49 . . . 109.1 ? C410 C49 H49 . . . 109.1 ? N44 C410 C411 . . . 106.1(3) y N44 C410 C49 . . . 113.2(3) y C411 C410 C49 . . . 109.4(3) y N44 C410 H410 . . . 109.3 ? C411 C410 H410 . . . 109.3 ? C49 C410 H410 . . . 109.3 ? C410 C411 C412 . . . 110.3(3) y C410 C411 H41A . . . 109.6 ? C412 C411 H41A . . . 109.6 ? C410 C411 H41B . . . 109.6 ? C412 C411 H41B . . . 109.6 ? H41A C411 H41B . . . 108.1 ? N47 C412 C411 . . . 108.7(3) y N47 C412 C47 . . . 110.1(3) y C411 C412 C47 . . . 110.3(3) y N47 C412 H412 . . . 109.3 ? C411 C412 H412 . . . 109.3 ? C47 C412 H412 . . . 109.3 ? O41 C413 H41C . . . 109.5 ? O41 C413 H41D . . . 109.5 ? H41C C413 H41D . . . 109.5 ? O41 C413 H41E . . . 109.5 ? H41C C413 H41E . . . 109.5 ? H41D C413 H41E . . . 109.5 ? O42 C414 H41F . . . 109.5 ? O42 C414 H41G . . . 109.5 ? H41F C414 H41G . . . 109.5 ? O42 C414 H41H . . . 109.5 ? H41F C414 H41H . . . 109.5 ? H41G C414 H41H . . . 109.5 ? C51 O51 C513 . . . 113.8(2) y C51 O52 C514 . . . 113.8(2) y C52 O53 C56 . . . 117.7(3) y O52 C51 O51 . . . 111.7(4) y O52 C51 C52 . . . 107.7(2) y O51 C51 C52 . . . 114.8(3) y O52 C51 H51C . . . 107.5 ? O51 C51 H51C . . . 107.5 ? C52 C51 H51C . . . 107.5 ? C53 C52 O53 . . . 126.0(4) y C53 C52 C51 . . . 125.2(4) y O53 C52 C51 . . . 108.8(3) y C52 C53 C54 . . . 120.1(4) y C52 C53 H53A . . . 119.9 ? C54 C53 H53A . . . 119.9 ? C55 C54 C53 . . . 107.3(4) y C55 C54 H54A . . . 110.3 ? C53 C54 H54A . . . 110.3 ? C55 C54 H54B . . . 110.3 ? C53 C54 H54B . . . 110.3 ? H54A C54 H54B . . . 108.5 ? O51 C513 H51D . . . 109.5 ? O51 C513 H51E . . . 109.5 ? H51D C513 H51E . . . 109.5 ? O51 C513 H51F . . . 109.5 ? H51D C513 H51F . . . 109.5 ? H51E C513 H51F . . . 109.5 ? O52 C514 H51G . . . 109.5 ? O52 C514 H51H . . . 109.5 ? H51G C514 H51H . . . 109.5 ? O52 C514 H51I . . . 109.5 ? H51G C514 H51I . . . 109.5 ? H51H C514 H51I . . . 109.5 ? C91 O91 C913 . . . 113.8(2) y C91 O92 C914 . . . 113.8(2) y C92 O93 C56 . . . 117.5(6) y O92 C91 O91 . . . 109.0(7) y O92 C91 C92 . . . 109.1(6) y O91 C91 C92 . . . 117.1(7) y O92 C91 H91A . . . 107.1 ? O91 C91 H91A . . . 107.1 ? C92 C91 H91A . . . 107.1 ? C93 C92 O93 . . . 124.2(6) y C93 C92 C91 . . . 125.0(6) y O93 C92 C91 . . . 110.2(5) y C92 C93 C94 . . . 121.9(6) y C92 C93 H93A . . . 119.1 ? C94 C93 H93A . . . 119.1 ? C55 C94 C93 . . . 109.2(6) y C55 C94 H94A . . . 109.8 ? C93 C94 H94A . . . 109.8 ? C55 C94 H94B . . . 109.8 ? C93 C94 H94B . . . 109.8 ? H94A C94 H94B . . . 108.3 ? O91 C913 H91B . . . 109.5 ? O91 C913 H91C . . . 109.5 ? H91B C913 H91C . . . 109.5 ? O91 C913 H91D . . . 109.5 ? H91B C913 H91D . . . 109.5 ? H91C C913 H91D . . . 109.5 ? O92 C914 H91E . . . 109.5 ? O92 C914 H91F . . . 109.5 ? H91E C914 H91F . . . 109.5 ? O92 C914 H91G . . . 109.5 ? H91E C914 H91G . . . 109.5 ? H91F C914 H91G . . . 109.5 ? C56 O54 C57 . . . 115.9(3) y C58 O55 H55 . . . 109.5 ? C59 O56 H56 . . . 109.5 ? N52 N51 C55 . . . 113.2(3) y N53 N52 N51 . . . 171.7(4) y N55 N54 C510 . . . 117.0(3) y N56 N55 N54 . . . 170.0(4) y N58 N57 C512 . . . 114.7(3) y N59 N58 N57 . . . 172.4(5) y N51 C55 C94 . . . 110.8(5) y N51 C55 C54 . . . 116.7(4) y N51 C55 C56 . . . 109.6(3) y C94 C55 C56 . . . 110.7(6) y C54 C55 C56 . . . 111.4(4) y N51 C55 H55A . . . 106.2 ? C94 C55 H55A . . . 113.2 ? C54 C55 H55A . . . 106.2 ? C56 C55 H55A . . . 106.2 ? O54 C56 O53 . . . 112.9(4) y O54 C56 O93 . . . 107.3(12) y O54 C56 C55 . . . 106.8(3) y O53 C56 C55 . . . 111.2(3) y O93 C56 C55 . . . 111.3(6) y O54 C56 H56A . . . 108.6 ? O53 C56 H56A . . . 108.6 ? O93 C56 H56A . . . 113.9 ? C55 C56 H56A . . . 108.6 ? O54 C57 C512 . . . 105.0(3) y O54 C57 C58 . . . 111.6(3) y C512 C57 C58 . . . 110.6(3) y O54 C57 H57 . . . 109.8 ? C512 C57 H57 . . . 109.8 ? C58 C57 H57 . . . 109.8 ? O55 C58 C59 . . . 110.7(3) y O55 C58 C57 . . . 108.2(3) y C59 C58 C57 . . . 111.2(3) y O55 C58 H58 . . . 108.9 ? C59 C58 H58 . . . 108.9 ? C57 C58 H58 . . . 108.9 ? O56 C59 C510 . . . 109.7(3) y O56 C59 C58 . . . 106.8(3) y C510 C59 C58 . . . 112.3(3) y O56 C59 H59 . . . 109.3 ? C510 C59 H59 . . . 109.3 ? C58 C59 H59 . . . 109.3 ? N54 C510 C59 . . . 113.1(3) y N54 C510 C511 . . . 106.0(3) y C59 C510 C511 . . . 109.0(3) y N54 C510 H510 . . . 109.6 ? C59 C510 H510 . . . 109.6 ? C511 C510 H510 . . . 109.6 ? C510 C511 C512 . . . 110.3(3) y C510 C511 H51A . . . 109.6 ? C512 C511 H51A . . . 109.6 ? C510 C511 H51B . . . 109.6 ? C512 C511 H51B . . . 109.6 ? H51A C511 H51B . . . 108.1 ? N57 C512 C57 . . . 110.4(3) y N57 C512 C511 . . . 108.1(3) y C57 C512 C511 . . . 111.7(3) y N57 C512 H512 . . . 108.9 ? C57 C512 H512 . . . 108.9 ? C511 C512 H512 . . . 108.9 ? C614 O61 C61 . . . 114.9(3) y C61 O62 C613 . . . 112.2(3) y C62 O63 C66A . . . 117.0(5) y C62 O63 C66B . . . 112.0(4) y C66A O64 C67 . . . 111.9(4) y C66B O64 C67 . . . 118.2(4) y C68 O65 H65 . . . 109.5 ? C69 O66 H66 . . . 109.5 ? N65 N64 C610 . . . 117.7(3) y N66 N65 N64 . . . 171.4(4) y N68 N67 C612 . . . 113.8(3) y N69 N68 N67 . . . 173.6(4) y O62 C61 O61 . . . 111.0(3) y O62 C61 C62 . . . 109.8(3) y O61 C61 C62 . . . 112.3(3) y O62 C61 H61 . . . 107.9 ? O61 C61 H61 . . . 107.9 ? C62 C61 H61 . . . 107.9 ? C63B C62 O63 . . . 128.2(6) y C63A C62 O63 . . . 122.7(5) y C63B C62 C61 . . . 122.3(6) y C63A C62 C61 . . . 128.5(5) y O63 C62 C61 . . . 108.6(3) y O64 C67 C612 . . . 105.9(3) y O64 C67 C68 . . . 110.4(3) y C612 C67 C68 . . . 111.5(3) y O64 C67 H67 . . . 109.6 ? C612 C67 H67 . . . 109.6 ? C68 C67 H67 . . . 109.6 ? O65 C68 C69 . . . 112.0(3) y O65 C68 C67 . . . 107.1(3) y C69 C68 C67 . . . 111.5(3) y O65 C68 H68 . . . 108.7 ? C69 C68 H68 . . . 108.7 ? C67 C68 H68 . . . 108.7 ? O66 C69 C610 . . . 109.8(3) y O66 C69 C68 . . . 107.2(3) y C610 C69 C68 . . . 111.8(3) y O66 C69 H69 . . . 109.3 ? C610 C69 H69 . . . 109.3 ? C68 C69 H69 . . . 109.3 ? N64 C610 C69 . . . 112.9(3) y N64 C610 C611 . . . 105.8(3) y C69 C610 C611 . . . 109.3(3) y N64 C610 H610 . . . 109.6 ? C69 C610 H610 . . . 109.6 ? C611 C610 H610 . . . 109.6 ? C612 C611 C610 . . . 110.7(3) y C612 C611 H61A . . . 109.5 ? C610 C611 H61A . . . 109.5 ? C612 C611 H61B . . . 109.5 ? C610 C611 H61B . . . 109.5 ? H61A C611 H61B . . . 108.1 ? N67 C612 C611 . . . 108.8(3) y N67 C612 C67 . . . 109.6(3) y C611 C612 C67 . . . 110.8(3) y N67 C612 H612 . . . 109.2 ? C611 C612 H612 . . . 109.2 ? C67 C612 H612 . . . 109.2 ? O62 C613 H61C . . . 109.5 ? O62 C613 H61D . . . 109.5 ? H61C C613 H61D . . . 109.5 ? O62 C613 H61E . . . 109.5 ? H61C C613 H61E . . . 109.5 ? H61D C613 H61E . . . 109.5 ? O61 C614 H61F . . . 109.5 ? O61 C614 H61G . . . 109.5 ? H61F C614 H61G . . . 109.5 ? O61 C614 H61H . . . 109.5 ? H61F C614 H61H . . . 109.5 ? H61G C614 H61H . . . 109.5 ? C713 O71 C71 . . . 114.9(3) y C71 O72 C714 . . . 112.3(3) y C72 O73 C76 . . . 114.9(3) y C76 O74 C77 . . . 116.0(3) y C78 O75 H75 . . . 109.5 ? C79 O76 H76 . . . 109.5 ? N72 N71 C75 . . . 119.2(4) y N73 N72 N71 . . . 173.7(5) y N75 N74 C710 . . . 118.9(3) y N76 N75 N74 . . . 170.6(4) y N78 N77 C712 . . . 113.1(3) y N79 N78 N77 . . . 174.1(4) y O72 C71 O71 . . . 111.8(3) y O72 C71 C72 . . . 108.5(3) y O71 C71 C72 . . . 112.0(3) y O72 C71 H71 . . . 108.2 ? O71 C71 H71 . . . 108.2 ? C72 C71 H71 . . . 108.2 ? C73 C72 O73 . . . 124.5(4) y C73 C72 C71 . . . 125.7(4) y O73 C72 C71 . . . 109.7(3) y C72 C73 C74 . . . 122.5(4) y C72 C73 H73 . . . 118.7 ? C74 C73 H73 . . . 118.7 ? C73 C74 C75 . . . 109.2(3) y C73 C74 H74A . . . 109.8 ? C75 C74 H74A . . . 109.8 ? C73 C74 H74B . . . 109.8 ? C75 C74 H74B . . . 109.8 ? H74A C74 H74B . . . 108.3 ? C76 C75 N71 . . . 106.9(3) y C76 C75 C74 . . . 110.9(3) y N71 C75 C74 . . . 114.0(4) y C76 C75 H75A . . . 108.3 ? N71 C75 H75A . . . 108.3 ? C74 C75 H75A . . . 108.3 ? O74 C76 O73 . . . 110.7(3) y O74 C76 C75 . . . 106.3(3) y O73 C76 C75 . . . 110.7(3) y O74 C76 H76A . . . 109.7 ? O73 C76 H76A . . . 109.7 ? C75 C76 H76A . . . 109.7 ? O74 C77 C712 . . . 106.8(3) y O74 C77 C78 . . . 111.3(3) y C712 C77 C78 . . . 109.9(3) y O74 C77 H77 . . . 109.6 ? C712 C77 H77 . . . 109.6 ? C78 C77 H77 . . . 109.6 ? O75 C78 C77 . . . 107.9(3) y O75 C78 C79 . . . 110.6(3) y C77 C78 C79 . . . 112.2(3) y O75 C78 H78 . . . 108.7 ? C77 C78 H78 . . . 108.7 ? C79 C78 H78 . . . 108.7 ? O76 C79 C710 . . . 110.7(3) y O76 C79 C78 . . . 106.8(3) y C710 C79 C78 . . . 111.1(3) y O76 C79 H79 . . . 109.4 ? C710 C79 H79 . . . 109.4 ? C78 C79 H79 . . . 109.4 ? N74 C710 C711 . . . 105.8(3) y N74 C710 C79 . . . 111.8(3) y C711 C710 C79 . . . 109.4(3) y N74 C710 H710 . . . 109.9 ? C711 C710 H710 . . . 109.9 ? C79 C710 H710 . . . 109.9 ? C710 C711 C712 . . . 110.0(3) y C710 C711 H71A . . . 109.7 ? C712 C711 H71A . . . 109.7 ? C710 C711 H71B . . . 109.7 ? C712 C711 H71B . . . 109.7 ? H71A C711 H71B . . . 108.2 ? N77 C712 C77 . . . 110.6(3) y N77 C712 C711 . . . 108.6(3) y C77 C712 C711 . . . 110.4(3) y N77 C712 H712 . . . 109.1 ? C77 C712 H712 . . . 109.1 ? C711 C712 H712 . . . 109.1 ? O71 C713 H71C . . . 109.5 ? O71 C713 H71D . . . 109.5 ? H71C C713 H71D . . . 109.5 ? O71 C713 H71E . . . 109.5 ? H71C C713 H71E . . . 109.5 ? H71D C713 H71E . . . 109.5 ? O72 C714 H71F . . . 109.5 ? O72 C714 H71G . . . 109.5 ? H71F C714 H71G . . . 109.5 ? O72 C714 H71H . . . 109.5 ? H71F C714 H71H . . . 109.5 ? H71G C714 H71H . . . 109.5 ? C81 O81 C813 . . . 114.3(3) y C81 O82 C814 . . . 113.2(3) y C82 O83 C86 . . . 117.6(3) y C86 O84 C87 . . . 115.8(2) y C88 O85 H85 . . . 109.5 ? C89 O86 H86 . . . 109.5 ? N82B N81 C85 . . . 116.0(4) y N82A N81 C85 . . . 114.3(4) y N85 N84 C810 . . . 117.4(3) y N86 N85 N84 . . . 169.9(4) y N88A N87 C812 . . . 119.0(5) y N88B N87 C812 . . . 113.2(4) y O82 C81 O81 . . . 112.1(3) y O82 C81 C82 . . . 108.6(3) y O81 C81 C82 . . . 112.5(3) y O82 C81 H81 . . . 107.8 ? O81 C81 H81 . . . 107.8 ? C82 C81 H81 . . . 107.8 ? C83 C82 O83 . . . 125.1(3) y C83 C82 C81 . . . 125.9(3) y O83 C82 C81 . . . 108.9(3) y C82 C83 C84 . . . 121.7(3) y C82 C83 H83 . . . 119.2 ? C84 C83 H83 . . . 119.2 ? C83 C84 C85 . . . 107.0(3) y C83 C84 H84A . . . 110.3 ? C85 C84 H84A . . . 110.3 ? C83 C84 H84B . . . 110.3 ? C85 C84 H84B . . . 110.3 ? H84A C84 H84B . . . 108.6 ? N81 C85 C84 . . . 115.9(3) y N81 C85 C86 . . . 106.5(3) y C84 C85 C86 . . . 111.1(3) y N81 C85 H85A . . . 107.7 ? C84 C85 H85A . . . 107.7 ? C86 C85 H85A . . . 107.7 ? O84 C86 O83 . . . 110.8(3) y O84 C86 C85 . . . 107.7(3) y O83 C86 C85 . . . 111.2(3) y O84 C86 H86A . . . 109.0 ? O83 C86 H86A . . . 109.0 ? C85 C86 H86A . . . 109.0 ? O84 C87 C812 . . . 105.4(3) y O84 C87 C88 . . . 111.7(3) y C812 C87 C88 . . . 110.7(3) y O84 C87 H87 . . . 109.7 ? C812 C87 H87 . . . 109.7 ? C88 C87 H87 . . . 109.7 ? O85 C88 C89 . . . 109.9(3) y O85 C88 C87 . . . 107.6(3) y C89 C88 C87 . . . 112.4(3) y O85 C88 H88 . . . 108.9 ? C89 C88 H88 . . . 108.9 ? C87 C88 H88 . . . 108.9 ? O86 C89 C810 . . . 110.2(3) y O86 C89 C88 . . . 107.4(3) y C810 C89 C88 . . . 111.0(3) y O86 C89 H89 . . . 109.4 ? C810 C89 H89 . . . 109.4 ? C88 C89 H89 . . . 109.4 ? N84 C810 C89 . . . 112.9(3) y N84 C810 C811 . . . 105.5(3) y C89 C810 C811 . . . 109.8(3) y N84 C810 H810 . . . 109.5 ? C89 C810 H810 . . . 109.5 ? C811 C810 H810 . . . 109.5 ? C810 C811 C812 . . . 110.6(3) y C810 C811 H81A . . . 109.5 ? C812 C811 H81A . . . 109.5 ? C810 C811 H81B . . . 109.5 ? C812 C811 H81B . . . 109.5 ? H81A C811 H81B . . . 108.1 ? N87 C812 C87 . . . 109.1(3) y N87 C812 C811 . . . 107.5(3) y C87 C812 C811 . . . 111.5(3) y N87 C812 H812 . . . 109.5 ? C87 C812 H812 . . . 109.5 ? C811 C812 H812 . . . 109.5 ? O81 C813 H81C . . . 109.5 ? O81 C813 H81D . . . 109.5 ? H81C C813 H81D . . . 109.5 ? O81 C813 H81E . . . 109.5 ? H81C C813 H81E . . . 109.5 ? H81D C813 H81E . . . 109.5 ? O82 C814 H81F . . . 109.5 ? O82 C814 H81G . . . 109.5 ? H81F C814 H81G . . . 109.5 ? O82 C814 H81H . . . 109.5 ? H81F C814 H81H . . . 109.5 ? H81G C814 H81H . . . 109.5 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C114 O12 C11 O11 . . . . -70.1(4) y C114 O12 C11 C12 . . . . 164.2(3) y C113 O11 C11 O12 . . . . -65.3(4) y C113 O11 C11 C12 . . . . 57.1(4) y C16 O13 C12 C13 . . . . -4.5(5) y C16 O13 C12 C11 . . . . 173.7(3) y O12 C11 C12 C13 . . . . 2.5(5) y O11 C11 C12 C13 . . . . -122.4(4) y O12 C11 C12 O13 . . . . -175.8(3) y O11 C11 C12 O13 . . . . 59.4(4) y O13 C12 C13 C14 . . . . 1.2(6) y C11 C12 C13 C14 . . . . -176.8(3) y C12 C13 C14 C15 . . . . 28.5(5) y N12 N11 C15 C14 . . . . 34.0(4) y N12 N11 C15 C16 . . . . -91.7(4) y C13 C14 C15 N11 . . . . -177.7(3) y C13 C14 C15 C16 . . . . -53.9(4) y C17 O14 C16 O13 . . . . 82.3(3) y C17 O14 C16 C15 . . . . -155.9(3) y C12 O13 C16 O14 . . . . 96.9(3) y C12 O13 C16 C15 . . . . -22.4(4) y N11 C15 C16 O14 . . . . 59.1(3) y C14 C15 C16 O14 . . . . -68.5(3) y N11 C15 C16 O13 . . . . -179.7(3) y C14 C15 C16 O13 . . . . 52.7(4) y C16 O14 C17 C112 . . . . -159.6(3) y C16 O14 C17 C18 . . . . 80.2(3) y O14 C17 C18 O15 . . . . -68.1(3) y C112 C17 C18 O15 . . . . 175.2(3) y O14 C17 C18 C19 . . . . 170.8(3) y C112 C17 C18 C19 . . . . 54.1(4) y O15 C18 C19 O16 . . . . 62.4(3) y C17 C18 C19 O16 . . . . -176.6(3) y O15 C18 C19 C110 . . . . -176.5(3) y C17 C18 C19 C110 . . . . -55.6(4) y N15 N14 C110 C19 . . . . 71.0(4) y N15 N14 C110 C111 . . . . -168.6(3) y O16 C19 C110 N14 . . . . -64.4(3) y C18 C19 C110 N14 . . . . 176.5(3) y O16 C19 C110 C111 . . . . 176.8(3) y C18 C19 C110 C111 . . . . 57.7(4) y N14 C110 C111 C112 . . . . 179.6(3) y C19 C110 C111 C112 . . . . -59.0(4) y N18 N17 C112 C17 . . . . -90.2(4) y N18 N17 C112 C111 . . . . 148.7(3) y O14 C17 C112 N17 . . . . 65.2(3) y C18 C17 C112 N17 . . . . -174.1(3) y O14 C17 C112 C111 . . . . -176.2(3) y C18 C17 C112 C111 . . . . -55.4(4) y C110 C111 C112 N17 . . . . 178.6(3) y C110 C111 C112 C17 . . . . 58.1(4) y C62 C63A C64A C65A . . . . 22(4) y C63A C64A C65A N61A . . . . -166(2) y C63A C64A C65A C66A . . . . -45(2) y N61A C65A C66A O64 . . . . 67.4(12) y C64A C65A C66A O64 . . . . -61.0(13) y N61A C65A C66A O63 . . . . -171.2(8) y C64A C65A C66A O63 . . . . 60.5(11) y C64A C65A N61A N62A . . . . -20.6(18) y C66A C65A N61A N62A . . . . -143.6(13) y C65A N61A N62A N63A . . . . -147(7) y C62 C63B C64B C65B . . . . 7(3) y C63B C64B C65B C66B . . . . -41(2) y C63B C64B C65B N61B . . . . -162(2) y C64B C65B C66B O64 . . . . -58.3(12) y N61B C65B C66B O64 . . . . 65.2(10) y C64B C65B C66B O63 . . . . 61.7(11) y N61B C65B C66B O63 . . . . -174.9(7) y C66B C65B N61B N62B . . . . -90.5(14) y C64B C65B N61B N62B . . . . 32.4(16) y C213 O21 C21 O22 . . . . 66.2(4) y C213 O21 C21 C22 . . . . -168.1(3) y C214 O22 C21 O21 . . . . 62.4(4) y C214 O22 C21 C22 . . . . -60.8(4) y C26 O23 C22 C23 . . . . 21.3(4) y C26 O23 C22 C21 . . . . -154.5(3) y O21 C21 C22 C23 . . . . 0.1(5) y O22 C21 C22 C23 . . . . 125.3(4) y O21 C21 C22 O23 . . . . 175.7(3) y O22 C21 C22 O23 . . . . -59.1(3) y O23 C22 C23 C24 . . . . -2.2(5) y C21 C22 C23 C24 . . . . 172.8(3) y C22 C23 C24 C25 . . . . 13.3(5) y N22B N21 C25 C24 . . . . -14.5(7) y N22A N21 C25 C24 . . . . 21.3(6) y N22B N21 C25 C26 . . . . -138.0(6) y N22A N21 C25 C26 . . . . -102.2(6) y C23 C24 C25 N21 . . . . -162.8(3) y C23 C24 C25 C26 . . . . -40.8(4) y C27 O24 C26 O23 . . . . 70.0(3) y C27 O24 C26 C25 . . . . -170.2(3) y C22 O23 C26 O24 . . . . 67.6(3) y C22 O23 C26 C25 . . . . -49.8(4) y N21 C25 C26 O24 . . . . 67.4(4) y C24 C25 C26 O24 . . . . -59.5(4) y N21 C25 C26 O23 . . . . -172.5(3) y C24 C25 C26 O23 . . . . 60.6(4) y C26 O24 C27 C28 . . . . 90.5(3) y C26 O24 C27 C212 . . . . -148.9(3) y O24 C27 C28 O25 . . . . -69.4(3) y C212 C27 C28 O25 . . . . 173.6(3) y O24 C27 C28 C29 . . . . 168.8(3) y C212 C27 C28 C29 . . . . 51.7(4) y O25 C28 C29 O26 . . . . 67.5(3) y C27 C28 C29 O26 . . . . -173.0(3) y O25 C28 C29 C210 . . . . -172.9(3) y C27 C28 C29 C210 . . . . -53.4(4) y N25 N24 C210 C29 . . . . 69.9(4) y N25 N24 C210 C211 . . . . -170.8(3) y O26 C29 C210 N24 . . . . -67.6(3) y C28 C29 C210 N24 . . . . 174.5(3) y O26 C29 C210 C211 . . . . 175.6(3) y C28 C29 C210 C211 . . . . 57.7(4) y N24 C210 C211 C212 . . . . 177.2(3) y C29 C210 C211 C212 . . . . -61.5(4) y N28 N27 C212 C211 . . . . 140.1(3) y N28 N27 C212 C27 . . . . -99.4(3) y C210 C211 C212 N27 . . . . -179.9(3) y C210 C211 C212 C27 . . . . 59.8(4) y O24 C27 C212 N27 . . . . 66.2(3) y C28 C27 C212 N27 . . . . -174.1(3) y O24 C27 C212 C211 . . . . -174.3(3) y C28 C27 C212 C211 . . . . -54.5(4) y C314 O31 C31 O32 . . . . -77.0(4) y C314 O31 C31 C32 . . . . 157.3(3) y C313 O32 C31 O31 . . . . -63.2(4) y C313 O32 C31 C32 . . . . 60.2(4) y C36 O33 C32 C33 . . . . 0.7(5) y C36 O33 C32 C31 . . . . 176.6(3) y O31 C31 C32 C33 . . . . 2.7(5) y O32 C31 C32 C33 . . . . -122.6(4) y O31 C31 C32 O33 . . . . -173.1(3) y O32 C31 C32 O33 . . . . 61.5(4) y O33 C32 C33 C34 . . . . 1.4(6) y C31 C32 C33 C34 . . . . -173.8(3) y C32 C33 C34 C35 . . . . 24.7(5) y N32B N31 C35 C34 . . . . 32.1(6) y N32A N31 C35 C34 . . . . -4.1(6) y N32B N31 C35 C36 . . . . -93.0(5) y N32A N31 C35 C36 . . . . -129.2(5) y C33 C34 C35 N31 . . . . -175.4(3) y C33 C34 C35 C36 . . . . -51.5(4) y C37 O34 C36 O33 . . . . 78.8(3) y C37 O34 C36 C35 . . . . -158.5(3) y C32 O33 C36 O34 . . . . 90.3(3) y C32 O33 C36 C35 . . . . -29.6(4) y N31 C35 C36 O34 . . . . 62.3(3) y C34 C35 C36 O34 . . . . -65.6(4) y N31 C35 C36 O33 . . . . -176.0(3) y C34 C35 C36 O33 . . . . 56.1(4) y C36 O34 C37 C312 . . . . -160.4(3) y C36 O34 C37 C38 . . . . 79.2(3) y O34 C37 C38 O35 . . . . -69.0(3) y C312 C37 C38 O35 . . . . 173.8(3) y O34 C37 C38 C39 . . . . 168.8(3) y C312 C37 C38 C39 . . . . 51.6(4) y O35 C38 C39 O36 . . . . 63.8(3) y C37 C38 C39 O36 . . . . -175.3(3) y O35 C38 C39 C310 . . . . -174.6(3) y C37 C38 C39 C310 . . . . -53.7(4) y N35 N34 C310 C39 . . . . 67.2(4) y N35 N34 C310 C311 . . . . -172.0(3) y O36 C39 C310 N34 . . . . -64.8(4) y C38 C39 C310 N34 . . . . 175.0(3) y O36 C39 C310 C311 . . . . 176.8(3) y C38 C39 C310 C311 . . . . 56.6(4) y N34 C310 C311 C312 . . . . 178.7(3) y C39 C310 C311 C312 . . . . -58.6(4) y N38 N37 C312 C311 . . . . 152.2(3) y N38 N37 C312 C37 . . . . -85.9(4) y C310 C311 C312 N37 . . . . 179.4(3) y C310 C311 C312 C37 . . . . 58.2(4) y O34 C37 C312 N37 . . . . 65.0(3) y C38 C37 C312 N37 . . . . -173.8(3) y O34 C37 C312 C311 . . . . -175.7(3) y C38 C37 C312 C311 . . . . -54.5(4) y C414 O42 C41 O41 . . . . 68.0(4) y C414 O42 C41 C42 . . . . -167.7(3) y C413 O41 C41 O42 . . . . 60.3(4) y C413 O41 C41 C42 . . . . -62.1(4) y C46 O43 C42 C43 . . . . 21.5(5) y C46 O43 C42 C41 . . . . -155.2(3) y O42 C41 C42 C43 . . . . -2.7(5) y O41 C41 C42 C43 . . . . 121.4(4) y O42 C41 C42 O43 . . . . 173.9(3) y O41 C41 C42 O43 . . . . -62.0(4) y O43 C42 C43 C44 . . . . -2.1(6) y C41 C42 C43 C44 . . . . 174.1(4) y C42 C43 C44 C45 . . . . 12.6(5) y N42 N41 C45 C46 . . . . -147.2(4) y N42 N41 C45 C44 . . . . -24.8(5) y C43 C44 C45 N41 . . . . -161.6(3) y C43 C44 C45 C46 . . . . -40.3(4) y C47 O44 C46 O43 . . . . 70.4(3) y C47 O44 C46 C45 . . . . -168.2(3) y C42 O43 C46 O44 . . . . 67.9(4) y C42 O43 C46 C45 . . . . -51.0(4) y N41 C45 C46 O44 . . . . 64.8(4) y C44 C45 C46 O44 . . . . -60.3(4) y N41 C45 C46 O43 . . . . -173.9(3) y C44 C45 C46 O43 . . . . 61.0(4) y C46 O44 C47 C48 . . . . 90.5(3) y C46 O44 C47 C412 . . . . -149.8(3) y O44 C47 C48 O45 . . . . -68.4(3) y C412 C47 C48 O45 . . . . 175.3(3) y O44 C47 C48 C49 . . . . 169.5(3) y C412 C47 C48 C49 . . . . 53.3(4) y O45 C48 C49 O46 . . . . 64.9(3) y C47 C48 C49 O46 . . . . -175.2(3) y O45 C48 C49 C410 . . . . -173.8(3) y C47 C48 C49 C410 . . . . -54.0(4) y N45 N44 C410 C411 . . . . -163.4(3) y N45 N44 C410 C49 . . . . 76.5(4) y O46 C49 C410 N44 . . . . -66.3(4) y C48 C49 C410 N44 . . . . 174.4(3) y O46 C49 C410 C411 . . . . 175.6(3) y C48 C49 C410 C411 . . . . 56.2(4) y N44 C410 C411 C412 . . . . 178.0(3) y C49 C410 C411 C412 . . . . -59.5(4) y N48 N47 C412 C411 . . . . 141.2(3) y N48 N47 C412 C47 . . . . -97.9(4) y C410 C411 C412 N47 . . . . -179.5(3) y C410 C411 C412 C47 . . . . 59.7(4) y O44 C47 C412 N47 . . . . 64.6(3) y C48 C47 C412 N47 . . . . -175.7(3) y O44 C47 C412 C411 . . . . -175.5(3) y C48 C47 C412 C411 . . . . -55.8(4) y C514 O52 C51 O51 . . . . -71.8(4) y C514 O52 C51 C52 . . . . 161.3(4) y C513 O51 C51 O52 . . . . -64.1(5) y C513 O51 C51 C52 . . . . 58.8(5) y C56 O53 C52 C53 . . . . -0.2(11) y C56 O53 C52 C51 . . . . 177.7(5) y O52 C51 C52 C53 . . . . 10.6(6) y O51 C51 C52 C53 . . . . -114.5(5) y O52 C51 C52 O53 . . . . -167.3(5) y O51 C51 C52 O53 . . . . 67.6(6) y O53 C52 C53 C54 . . . . -0.1(10) y C51 C52 C53 C54 . . . . -177.7(5) y C52 C53 C54 C55 . . . . 27.7(8) y C914 O92 C91 O91 . . . . 69.8(13) y C914 O92 C91 C92 . . . . -161.2(10) y C913 O91 C91 O92 . . . . -152.2(15) y C913 O91 C91 C92 . . . . 83.4(18) y C56 O93 C92 C93 . . . . 9(3) y C56 O93 C92 C91 . . . . -179.1(15) y O92 C91 C92 C93 . . . . 110(2) y O91 C91 C92 C93 . . . . -125.3(18) y O92 C91 C92 O93 . . . . -61.6(16) y O91 C91 C92 O93 . . . . 62.8(18) y O93 C92 C93 C94 . . . . -1(3) y C91 C92 C93 C94 . . . . -171.6(15) y C92 C93 C94 C55 . . . . 22(3) y N52 N51 C55 C94 . . . . 33.6(9) y N52 N51 C55 C54 . . . . 38.9(6) y N52 N51 C55 C56 . . . . -88.9(4) y C93 C94 C55 N51 . . . . -169.7(12) y C93 C94 C55 C54 . . . . 48(4) y C93 C94 C55 C56 . . . . -47.9(16) y C53 C54 C55 N51 . . . . 179.1(4) y C53 C54 C55 C94 . . . . -141(5) y C53 C54 C55 C56 . . . . -54.0(6) y C57 O54 C56 O53 . . . . 75.4(4) y C57 O54 C56 O93 . . . . 78.5(5) y C57 O54 C56 C55 . . . . -162.0(3) y C52 O53 C56 O54 . . . . 92.8(7) y C52 O53 C56 O93 . . . . 64(6) y C52 O53 C56 C55 . . . . -27.3(8) y C92 O93 C56 O54 . . . . 80(2) y C92 O93 C56 O53 . . . . -128(9) y C92 O93 C56 C55 . . . . -37(2) y N51 C55 C56 O54 . . . . 63.0(4) y C94 C55 C56 O54 . . . . -59.5(8) y C54 C55 C56 O54 . . . . -67.7(4) y N51 C55 C56 O53 . . . . -173.4(5) y C94 C55 C56 O53 . . . . 64.1(9) y C54 C55 C56 O53 . . . . 55.9(6) y N51 C55 C56 O93 . . . . 179.8(12) y C94 C55 C56 O93 . . . . 57.3(13) y C54 C55 C56 O93 . . . . 49.2(12) y C56 O54 C57 C512 . . . . -157.5(3) y C56 O54 C57 C58 . . . . 82.6(3) y O54 C57 C58 O55 . . . . -68.9(3) y C512 C57 C58 O55 . . . . 174.6(3) y O54 C57 C58 C59 . . . . 169.4(3) y C512 C57 C58 C59 . . . . 52.9(4) y O55 C58 C59 O56 . . . . 64.2(3) y C57 C58 C59 O56 . . . . -175.6(3) y O55 C58 C59 C510 . . . . -175.6(3) y C57 C58 C59 C510 . . . . -55.3(4) y N55 N54 C510 C59 . . . . 70.5(4) y N55 N54 C510 C511 . . . . -170.1(3) y O56 C59 C510 N54 . . . . -66.1(4) y C58 C59 C510 N54 . . . . 175.4(3) y O56 C59 C510 C511 . . . . 176.3(3) y C58 C59 C510 C511 . . . . 57.8(4) y N54 C510 C511 C512 . . . . 179.3(3) y C59 C510 C511 C512 . . . . -58.7(4) y N58 N57 C512 C57 . . . . -89.6(4) y N58 N57 C512 C511 . . . . 148.0(4) y O54 C57 C512 N57 . . . . 63.9(4) y C58 C57 C512 N57 . . . . -175.6(3) y O54 C57 C512 C511 . . . . -175.8(3) y C58 C57 C512 C511 . . . . -55.2(4) y C510 C511 C512 N57 . . . . -179.6(3) y C510 C511 C512 C57 . . . . 58.8(4) y O64 C66A O63 C62 . . . . 65.3(7) y C65A C66A O63 C62 . . . . -51.0(10) y O64 C66A O63 C66B . . . . 97(5) y C65A C66A O63 C66B . . . . -19(4) y O64 C66B O63 C62 . . . . 75.1(6) y C65B C66B O63 C62 . . . . -43.7(9) y O64 C66B O63 C66A . . . . -75(4) y C65B C66B O63 C66A . . . . 167(5) y O63 C66A O64 C66B . . . . -109(4) y C65A C66A O64 C66B . . . . 11(3) y O63 C66A O64 C67 . . . . 72.7(6) y C65A C66A O64 C67 . . . . -168.0(5) y O63 C66B O64 C66A . . . . 63(3) y C65B C66B O64 C66A . . . . -176(4) y O63 C66B O64 C67 . . . . 64.4(6) y C65B C66B O64 C67 . . . . -174.2(5) y C613 O62 C61 O61 . . . . 67.1(4) y C613 O62 C61 C62 . . . . -168.1(3) y C614 O61 C61 O62 . . . . 64.7(5) y C614 O61 C61 C62 . . . . -58.6(4) y C64B C63B C62 C63A . . . . -60(5) y C64B C63B C62 O63 . . . . 11(4) y C64B C63B C62 C61 . . . . 178.8(19) y C64A C63A C62 C63B . . . . 107(9) y C64A C63A C62 O63 . . . . -11(4) y C64A C63A C62 C61 . . . . 174.7(18) y C66A O63 C62 C63B . . . . 11(2) y C66B O63 C62 C63B . . . . 8(2) y C66A O63 C62 C63A . . . . 27(2) y C66B O63 C62 C63A . . . . 23(2) y C66A O63 C62 C61 . . . . -158.1(4) y C66B O63 C62 C61 . . . . -161.3(4) y O62 C61 C62 C63B . . . . 8(2) y O61 C61 C62 C63B . . . . 132(2) y O62 C61 C62 C63A . . . . -7(2) y O61 C61 C62 C63A . . . . 117(2) y O62 C61 C62 O63 . . . . 178.3(3) y O61 C61 C62 O63 . . . . -57.7(4) y C66A O64 C67 C612 . . . . -145.9(4) y C66B O64 C67 C612 . . . . -146.1(4) y C66A O64 C67 C68 . . . . 93.3(4) y C66B O64 C67 C68 . . . . 93.1(4) y O64 C67 C68 O65 . . . . -67.3(4) y C612 C67 C68 O65 . . . . 175.2(3) y O64 C67 C68 C69 . . . . 169.9(3) y C612 C67 C68 C69 . . . . 52.4(4) y O65 C68 C69 O66 . . . . 65.3(4) y C67 C68 C69 O66 . . . . -174.8(3) y O65 C68 C69 C610 . . . . -174.3(3) y C67 C68 C69 C610 . . . . -54.4(4) y N65 N64 C610 C69 . . . . 81.0(4) y N65 N64 C610 C611 . . . . -159.6(3) y O66 C69 C610 N64 . . . . -66.4(4) y C68 C69 C610 N64 . . . . 174.8(3) y O66 C69 C610 C611 . . . . 176.3(3) y C68 C69 C610 C611 . . . . 57.4(4) y N64 C610 C611 C612 . . . . 178.7(3) y C69 C610 C611 C612 . . . . -59.5(4) y N68 N67 C612 C611 . . . . 137.0(3) y N68 N67 C612 C67 . . . . -101.8(4) y C610 C611 C612 N67 . . . . 179.0(3) y C610 C611 C612 C67 . . . . 58.5(4) y O64 C67 C612 N67 . . . . 65.2(3) y C68 C67 C612 N67 . . . . -174.7(3) y O64 C67 C612 C611 . . . . -174.8(3) y C68 C67 C612 C611 . . . . -54.7(4) y C714 O72 C71 O71 . . . . 68.0(4) y C714 O72 C71 C72 . . . . -168.0(3) y C713 O71 C71 O72 . . . . 62.2(5) y C713 O71 C71 C72 . . . . -59.7(4) y C76 O73 C72 C73 . . . . 14.8(5) y C76 O73 C72 C71 . . . . -162.4(3) y O72 C71 C72 C73 . . . . 7.3(5) y O71 C71 C72 C73 . . . . 131.1(4) y O72 C71 C72 O73 . . . . -175.5(3) y O71 C71 C72 O73 . . . . -51.7(4) y O73 C72 C73 C74 . . . . 0.5(6) y C71 C72 C73 C74 . . . . 177.3(4) y C72 C73 C74 C75 . . . . 15.0(6) y N72 N71 C75 C76 . . . . -135.6(4) y N72 N71 C75 C74 . . . . -12.6(6) y C73 C74 C75 C76 . . . . -44.2(5) y C73 C74 C75 N71 . . . . -165.0(4) y C77 O74 C76 O73 . . . . 75.0(3) y C77 O74 C76 C75 . . . . -164.8(3) y C72 O73 C76 O74 . . . . 72.8(4) y C72 O73 C76 C75 . . . . -44.9(4) y N71 C75 C76 O74 . . . . 65.4(4) y C74 C75 C76 O74 . . . . -59.4(4) y N71 C75 C76 O73 . . . . -174.3(3) y C74 C75 C76 O73 . . . . 60.9(5) y C76 O74 C77 C712 . . . . -148.8(3) y C76 O74 C77 C78 . . . . 91.3(3) y O74 C77 C78 O75 . . . . -65.2(3) y C712 C77 C78 O75 . . . . 176.7(3) y O74 C77 C78 C79 . . . . 172.7(3) y C712 C77 C78 C79 . . . . 54.6(4) y O75 C78 C79 O76 . . . . 64.3(3) y C77 C78 C79 O76 . . . . -175.1(3) y O75 C78 C79 C710 . . . . -174.9(3) y C77 C78 C79 C710 . . . . -54.3(4) y N75 N74 C710 C711 . . . . -162.6(3) y N75 N74 C710 C79 . . . . 78.5(4) y O76 C79 C710 N74 . . . . -68.6(4) y C78 C79 C710 N74 . . . . 172.9(3) y O76 C79 C710 C711 . . . . 174.7(3) y C78 C79 C710 C711 . . . . 56.1(4) y N74 C710 C711 C712 . . . . 179.7(3) y C79 C710 C711 C712 . . . . -59.7(4) y N78 N77 C712 C77 . . . . -94.0(4) y N78 N77 C712 C711 . . . . 144.7(3) y O74 C77 C712 N77 . . . . 61.2(3) y C78 C77 C712 N77 . . . . -177.9(3) y O74 C77 C712 C711 . . . . -178.6(3) y C78 C77 C712 C711 . . . . -57.7(4) y C710 C711 C712 N77 . . . . -177.3(3) y C710 C711 C712 C77 . . . . 61.3(4) y C814 O82 C81 O81 . . . . -73.1(4) y C814 O82 C81 C82 . . . . 162.0(3) y C813 O81 C81 O82 . . . . -61.8(4) y C813 O81 C81 C82 . . . . 60.9(4) y C86 O83 C82 C83 . . . . 0.2(5) y C86 O83 C82 C81 . . . . 176.3(3) y O82 C81 C82 C83 . . . . 2.6(5) y O81 C81 C82 C83 . . . . -122.0(4) y O82 C81 C82 O83 . . . . -173.3(3) y O81 C81 C82 O83 . . . . 62.0(4) y O83 C82 C83 C84 . . . . 1.5(6) y C81 C82 C83 C84 . . . . -173.8(3) y C82 C83 C84 C85 . . . . 25.5(5) y N82B N81 C85 C84 . . . . -18.9(6) y N82A N81 C85 C84 . . . . 25.1(6) y N82B N81 C85 C86 . . . . -143.1(5) y N82A N81 C85 C86 . . . . -99.0(5) y C83 C84 C85 N81 . . . . -174.4(3) y C83 C84 C85 C86 . . . . -52.7(4) y C87 O84 C86 O83 . . . . 81.0(3) y C87 O84 C86 C85 . . . . -157.2(3) y C82 O83 C86 O84 . . . . 90.7(3) y C82 O83 C86 C85 . . . . -29.1(4) y N81 C85 C86 O84 . . . . 62.2(3) y C84 C85 C86 O84 . . . . -64.8(4) y N81 C85 C86 O83 . . . . -176.2(3) y C84 C85 C86 O83 . . . . 56.8(4) y C86 O84 C87 C812 . . . . -158.4(3) y C86 O84 C87 C88 . . . . 81.4(3) y O84 C87 C88 O85 . . . . -69.5(3) y C812 C87 C88 O85 . . . . 173.4(3) y O84 C87 C88 C89 . . . . 169.3(3) y C812 C87 C88 C89 . . . . 52.3(4) y O85 C88 C89 O86 . . . . 64.8(3) y C87 C88 C89 O86 . . . . -175.4(3) y O85 C88 C89 C810 . . . . -174.8(3) y C87 C88 C89 C810 . . . . -54.9(4) y N85 N84 C810 C89 . . . . 69.6(4) y N85 N84 C810 C811 . . . . -170.4(3) y O86 C89 C810 N84 . . . . -65.9(4) y C88 C89 C810 N84 . . . . 175.3(3) y O86 C89 C810 C811 . . . . 176.7(3) y C88 C89 C810 C811 . . . . 57.8(4) y N84 C810 C811 C812 . . . . 178.7(3) y C89 C810 C811 C812 . . . . -59.4(4) y N88A N87 C812 C87 . . . . -117.3(6) y N88B N87 C812 C87 . . . . -91.9(6) y N88A N87 C812 C811 . . . . 121.6(6) y N88B N87 C812 C811 . . . . 147.0(5) y O84 C87 C812 N87 . . . . 67.0(3) y C88 C87 C812 N87 . . . . -172.1(3) y O84 C87 C812 C811 . . . . -174.4(3) y C88 C87 C812 C811 . . . . -53.5(4) y C810 C811 C812 N87 . . . . 177.4(3) y C810 C811 C812 C87 . . . . 57.8(4) y 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 _geom_hbond_publ_flag O15 H15 O46 0.84 2.11 2.913(3) 159.6 1_545 y O16 H16 O81 0.84 1.95 2.777(3) 169.2 1_546 y O25 H25 O36 0.84 2.01 2.843(3) 170.5 . y O26 H26 O71 0.84 1.9 2.722(3) 167.4 1_556 y O35 H35 O26 0.84 2.09 2.871(3) 155.4 . y O36 H36 O61 0.84 1.87 2.705(4) 170 . y O45 H45 O16 0.84 2.07 2.876(3) 161 1_565 y O46 H46 O51 0.84 1.94 2.743(4) 160 1_565 y O46 H46 O91 0.84 2.09 2.841(12) 149.5 1_565 y O55 H55 O76 0.84 2.14 2.941(3) 158.6 . y O56 H56 O32 0.84 1.95 2.751(3) 158.2 . y O65 H65 O86 0.84 2.09 2.867(3) 152.7 . y O66 H66 O41 0.84 1.99 2.753(4) 150.8 . y O75 H75 O56 0.84 2.08 2.887(3) 159.8 . y O76 H76 O11 0.84 1.97 2.789(3) 163.6 1_554 y O85 H85 O66 0.84 2.05 2.866(3) 162.8 . y O86 H86 O22 0.84 1.91 2.732(3) 164.7 1_554 y _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 64.12 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.357 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.047 #=== END OF THE CIF FILE # Attachment '- BENT66.cif' data_bent66 _database_code_depnum_ccdc_archive 'CCDC 838348' #TrackingRef '- BENT66.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H42 N6 O8, 2(O4 S), 14(H2 O)' _chemical_formula_sum 'C24 H70 N6 O30 S2' _chemical_formula_weight 986.98 _chemical_compound_source 'Synthesized by the authors. See text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.8516(4) _cell_length_b 26.1435(15) _cell_length_c 12.6653(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.975(3) _cell_angle_gamma 90.00 _cell_volume 2210.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200 _cell_measurement_reflns_used 18335 _cell_measurement_theta_min 3.38 _cell_measurement_theta_max 53.23 _exptl_crystal_description needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 2.018 _exptl_absorpt_correction_Type multi-scan _exptl_absorpt_correction_T_min 0.6632 _exptl_absorpt_correction_T_max 0.9413 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Platform diffractometer, equipped with a Bruker SMART 4K Charged-Coupled Device (CCD) Area Detector using the program APEX2 and a Nonius FR591 rotating anode equiped with a Helios optics. The crystal-to-detector distance was 5.0 cm, and the data collection was carried out in 512 x 512 pixel mode. The initial unit cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 10.0 degree scan in 33 frames over four different parts of the reciprocal space (132 frames total). One complete sphere of data was collected, to better than 0.80\%A resolution. ; _vrf_THETM01_bent66 ; RESPONSE: Low diffraction was observed for this crystal and was especially low for high angles. Many solvent systems were tested for recrystallization. The best crystal was chosen and its size was in the limits of the diffractometer. X-ray measurements were acquired at 200K with optimized radiation exposure time and intensity. The final structure was satisfactory for confirming the desired chemical information with R1 = 0.0437 and wR2=0.1060. ; _vrf_REFNR01_bent66 ; RESPONSE: See response for THETM01 Alert 3 A. ; _vrf_PLAT089_bent66 ; RESPONSE: See response for THETM01 Alert 3 A. ; _vrf_PLAT340_bent66 ; RESPONSE: See response for THETM01 Alert 3 A. ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Helios optics' _diffrn_measurement_device_type 'Bruker Smart 6000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 5.5 _diffrn_reflns_number 28784 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 53.69 _reflns_number_total 5428 _reflns_number_gt 4867 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT V7.60A(Bruker AXS, 2008)' _computing_data_reduction 'SAINT V7.60A(Bruker AXS, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_publication_material 'UdMX (Maris, 2004)' _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^)+(0.0487P)^2^+1.2198P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), 2714 Friedel Pairs' _chemical_absolute_configuration rmad _refine_ls_abs_structure_Flack 0.07(2) _refine_ls_number_reflns 5428 _refine_ls_number_parameters 689 _refine_ls_number_restraints 572 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1060 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.024 _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 O11 O 0.3510(4) 0.92807(11) 0.2195(2) 0.0299(5) Uani 1 1 d U . . O12 O 0.0863(4) 0.87196(11) 0.2207(2) 0.0313(6) Uani 1 1 d U . . O13 O 0.1519(5) 0.98183(13) 0.0277(3) 0.0428(9) Uani 1 1 d . . . H13D H 0.1315 1.0103 -0.0034 0.064 Uiso 1 1 calc R . . O14 O 0.4196(5) 1.01662(11) -0.1041(3) 0.0371(8) Uani 1 1 d . . . H14C H 0.3458 1.0145 -0.1666 0.056 Uiso 1 1 calc R . . N11 N 0.7249(6) 0.94730(16) -0.1322(3) 0.0391(11) Uani 1 1 d . . . H11A H 0.8566 0.9383 -0.1169 0.059 Uiso 1 1 calc R . . H11B H 0.7099 0.9784 -0.1653 0.059 Uiso 1 1 calc R . . H11C H 0.6523 0.9235 -0.1769 0.059 Uiso 1 1 calc R . . N12 N 0.2033(6) 1.00255(14) 0.3374(3) 0.0363(10) Uani 1 1 d . . . H12A H 0.3343 1.0045 0.3340 0.054 Uiso 1 1 calc R . . H12B H 0.1865 1.0177 0.3994 0.054 Uiso 1 1 calc R . . H12C H 0.1264 1.0189 0.2792 0.054 Uiso 1 1 calc R . . N13 N 0.6070(5) 0.84721(14) 0.1757(3) 0.0288(9) Uani 1 1 d . . . C11 C 0.6534(7) 0.95005(19) -0.0304(4) 0.0324(12) Uani 1 1 d . . . H11D H 0.7375 0.9751 0.0197 0.039 Uiso 1 1 calc R . . C12 C 0.6705(7) 0.89717(18) 0.0245(4) 0.0318(12) Uani 1 1 d . . . H12D H 0.5871 0.8722 -0.0246 0.038 Uiso 1 1 calc R . . H12E H 0.8113 0.8854 0.0387 0.038 Uiso 1 1 calc R . . C13 C 0.6022(7) 0.89951(18) 0.1305(4) 0.0296(7) Uani 1 1 d U . . H13A H 0.6951 0.9220 0.1827 0.036 Uiso 1 1 calc R . . C14 C 0.3881(7) 0.92043(18) 0.1129(4) 0.0297(5) Uani 1 1 d U . . H14A H 0.2922 0.8943 0.0734 0.036 Uiso 1 1 calc R . . C15 C 0.3607(7) 0.97015(18) 0.0491(4) 0.0303(7) Uani 1 1 d U . . H15A H 0.4356 0.9978 0.0959 0.036 Uiso 1 1 calc R . . C16 C 0.4366(7) 0.96729(18) -0.0537(4) 0.0320(12) Uani 1 1 d . . . H16A H 0.3529 0.9423 -0.1042 0.038 Uiso 1 1 calc R . . C11' C 0.1517(7) 0.92469(18) 0.2272(4) 0.0305(5) Uani 1 1 d U . . H11E H 0.0651 0.9449 0.1676 0.037 Uiso 1 1 calc R . . C12' C 0.1414(7) 0.94744(17) 0.3366(4) 0.0314(7) Uani 1 1 d U . . H12F H -0.0012 0.9462 0.3434 0.038 Uiso 1 1 calc R . . C13' C 0.2659(8) 0.91818(17) 0.4295(4) 0.0357(12) Uani 1 1 d . . . H13B H 0.4099 0.9247 0.4339 0.043 Uiso 1 1 calc R . . H13C H 0.2338 0.9293 0.4983 0.043 Uiso 1 1 calc R . . C14' C 0.2224(7) 0.8626(2) 0.4119(4) 0.0371(13) Uani 1 1 d . . . H14B H 0.2531 0.8402 0.4725 0.045 Uiso 1 1 calc R . . C15' C 0.1426(7) 0.84309(19) 0.3155(4) 0.0315(12) Uani 1 1 d . . . C16' C 0.1045(7) 0.78834(18) 0.2981(4) 0.0319(12) Uani 1 1 d . . . H16B H 0.1129 0.7675 0.3604 0.038 Uiso 1 1 calc R . . O21 O 0.3750(4) 0.70092(11) 0.3151(2) 0.0300(6) Uani 1 1 d U . . O22 O 0.6208(4) 0.75180(12) 0.2681(2) 0.0304(6) Uani 1 1 d U . . O23 O 0.4153(5) 0.60624(12) 0.2108(3) 0.0413(9) Uani 1 1 d . . . H23D H 0.4194 0.5751 0.2275 0.062 Uiso 1 1 calc R . . O24 O 0.0430(5) 0.55278(11) 0.1223(2) 0.0351(8) Uani 1 1 d . . . H24C H 0.0290 0.5442 0.1841 0.053 Uiso 1 1 calc R . . N21 N -0.2942(6) 0.61497(15) 0.0238(3) 0.0368(10) Uani 1 1 d . . . H21A H -0.2440 0.6143 -0.0369 0.055 Uiso 1 1 calc R . . H21B H -0.4017 0.6363 0.0131 0.055 Uiso 1 1 calc R . . H21C H -0.3327 0.5829 0.0383 0.055 Uiso 1 1 calc R . . N22 N 0.6368(5) 0.64884(14) 0.4733(3) 0.0333(9) Uani 1 1 d . . . H22A H 0.5042 0.6487 0.4739 0.050 Uiso 1 1 calc R . . H22B H 0.7106 0.6438 0.5418 0.050 Uiso 1 1 calc R . . H22C H 0.6626 0.6233 0.4295 0.050 Uiso 1 1 calc R . . N23 N 0.0611(5) 0.76655(14) 0.2065(3) 0.0298(9) Uani 1 1 d . . . C21 C -0.1361(7) 0.63380(17) 0.1176(4) 0.0345(12) Uani 1 1 d . . . H21D H -0.1770 0.6253 0.1865 0.041 Uiso 1 1 calc R . . C22 C -0.1119(7) 0.69173(18) 0.1108(4) 0.0353(12) Uani 1 1 d . . . H22D H -0.0656 0.7005 0.0445 0.042 Uiso 1 1 calc R . . H22E H -0.2426 0.7087 0.1069 0.042 Uiso 1 1 calc R . . C23 C 0.0392(6) 0.71047(18) 0.2100(4) 0.0292(11) Uani 1 1 d . . . H23C H -0.0083 0.7010 0.2765 0.035 Uiso 1 1 calc R . . C24 C 0.2412(7) 0.68494(18) 0.2141(4) 0.0297(11) Uani 1 1 d . . . H24B H 0.2958 0.6965 0.1512 0.036 Uiso 1 1 calc R . . C25 C 0.2255(7) 0.62636(17) 0.2137(4) 0.0315(12) Uani 1 1 d . . . H25A H 0.1898 0.6151 0.2825 0.038 Uiso 1 1 calc R . . C26 C 0.0629(7) 0.60763(18) 0.1178(4) 0.0326(12) Uani 1 1 d . . . H26 H 0.1038 0.6167 0.0491 0.039 Uiso 1 1 calc R . . C21' C 0.5772(7) 0.70434(18) 0.3136(4) 0.0300(5) Uani 1 1 d U . . H21E H 0.6143 0.6754 0.2704 0.036 Uiso 1 1 calc R . . C22' C 0.6912(7) 0.69945(17) 0.4315(4) 0.0306(7) Uani 1 1 d U . . H22F H 0.8381 0.6997 0.4342 0.037 Uiso 1 1 calc R . . C23' C 0.6434(7) 0.74294(19) 0.5006(4) 0.0377(12) Uani 1 1 d . . . H23A H 0.5069 0.7387 0.5132 0.045 Uiso 1 1 calc R . . H23B H 0.7398 0.7432 0.5717 0.045 Uiso 1 1 calc R . . C24' C 0.6574(6) 0.79228(19) 0.4416(4) 0.0307(12) Uani 1 1 d . . . H24A H 0.6762 0.8232 0.4819 0.037 Uiso 1 1 calc R . . C25' C 0.6448(6) 0.79443(18) 0.3365(4) 0.0310(11) Uani 1 1 d . . . C26' C 0.6456(7) 0.84296(19) 0.2782(4) 0.0343(12) Uani 1 1 d . . . H26A H 0.6771 0.8732 0.3200 0.041 Uiso 1 1 calc R . . O31 O 0.1364(7) 0.74547(17) 0.6246(4) 0.0817(13) Uani 1 1 d D . . O32 O 0.0748(5) 0.80097(15) -0.0055(3) 0.0537(10) Uani 1 1 d D . . O33 O 0.1506(6) 0.84972(15) 0.6663(3) 0.0605(11) Uani 1 1 d D . . O34 O 0.4734(6) 0.77722(14) 0.0015(3) 0.0557(10) Uani 1 1 d D . . O35 O 0.5648(6) 0.86849(16) 0.7153(4) 0.0621(11) Uani 1 1 d D . . O36 O 0.3848(6) 0.52850(16) 0.6571(3) 0.0622(11) Uani 1 1 d D . . O37 O 0.0588(6) 0.88446(15) 0.8616(3) 0.0565(11) Uani 1 1 d D . . O38 O 0.2450(6) 0.65281(16) 0.5148(3) 0.0584(10) Uani 1 1 d D . . O39 O 0.1465(6) 0.52762(15) 0.8239(3) 0.0641(11) Uani 1 1 d D . . O40 O 0.3720(6) 0.67758(15) 0.9764(3) 0.0547(10) Uani 1 1 d D . . O41 O 0.7131(6) 0.78055(15) 0.8468(3) 0.0592(11) Uani 1 1 d D . . O42 O 0.8159(7) 0.90746(15) 0.5659(4) 0.0634(11) Uani 1 1 d D . . O43 O 0.3834(5) 0.51036(15) 0.3211(3) 0.0478(9) Uani 1 1 d D . . O44 O 0.3741(6) 0.62662(17) 0.7270(4) 0.0701(12) Uani 1 1 d D . . H31A H 0.180(9) 0.7201(15) 0.591(4) 0.105 Uiso 1 1 d D . . H31B H 0.126(10) 0.733(2) 0.687(3) 0.105 Uiso 1 1 d D . . H32A H 0.036(5) 0.791(3) 0.052(3) 0.105 Uiso 1 1 d D . . H32B H 0.203(2) 0.7937(19) 0.007(4) 0.105 Uiso 1 1 d D . . H33A H 0.114(8) 0.8176(6) 0.663(6) 0.105 Uiso 1 1 d D . . H33B H 0.051(5) 0.8662(15) 0.6247(19) 0.105 Uiso 1 1 d D . . H34A H 0.546(6) 0.7838(11) -0.045(3) 0.105 Uiso 1 1 d D . . H34B H 0.533(7) 0.793(2) 0.061(2) 0.105 Uiso 1 1 d D . . H35A H 0.4347(14) 0.867(2) 0.706(6) 0.105 Uiso 1 1 d D . . H35B H 0.610(7) 0.8392(13) 0.744(6) 0.105 Uiso 1 1 d D . . H36A H 0.314(8) 0.524(2) 0.591(2) 0.105 Uiso 1 1 d D . . H36B H 0.399(7) 0.5616(5) 0.666(3) 0.105 Uiso 1 1 d D . . H37A H 0.083(9) 0.875(2) 0.800(2) 0.105 Uiso 1 1 d D . . H37B H 0.073(10) 0.8571(12) 0.902(3) 0.105 Uiso 1 1 d D . . H38A H 0.158(7) 0.6321(17) 0.476(4) 0.105 Uiso 1 1 d D . . H38B H 0.288(8) 0.6369(18) 0.576(2) 0.105 Uiso 1 1 d D . . H39A H 0.211(7) 0.537(2) 0.775(3) 0.105 Uiso 1 1 d D . . H39B H 0.102(9) 0.5557(12) 0.847(5) 0.105 Uiso 1 1 d D . . H40A H 0.259(5) 0.675(2) 0.929(4) 0.105 Uiso 1 1 d D . . H40B H 0.421(8) 0.7073(12) 0.965(5) 0.105 Uiso 1 1 d D . . H41A H 0.832(2) 0.770(2) 0.843(5) 0.105 Uiso 1 1 d D . . H41B H 0.629(3) 0.7603(9) 0.8043(16) 0.105 Uiso 1 1 d D . . H42A H 0.734(7) 0.905(2) 0.610(4) 0.105 Uiso 1 1 d D . . H42B H 0.815(10) 0.9397(7) 0.548(5) 0.105 Uiso 1 1 d D . . H43A H 0.506(2) 0.514(3) 0.359(3) 0.105 Uiso 1 1 d D . . H43B H 0.306(5) 0.516(3) 0.366(3) 0.105 Uiso 1 1 d D . . H44A H 0.472(4) 0.634(3) 0.782(3) 0.105 Uiso 1 1 d D . . H44B H 0.265(4) 0.636(3) 0.746(3) 0.105 Uiso 1 1 d D . . S1 S 0.91818(18) 0.53992(5) 0.39472(10) 0.0370(3) Uani 1 1 d . . . O51 O 0.9407(5) 0.59668(12) 0.3871(3) 0.0477(9) Uani 1 1 d . . . O52 O 0.8752(5) 0.51860(14) 0.2857(3) 0.0468(9) Uani 1 1 d . . . O53 O 1.1058(5) 0.51770(14) 0.4579(3) 0.0517(10) Uani 1 1 d . . . O54 O 0.7520(5) 0.53031(14) 0.4471(3) 0.0459(9) Uani 1 1 d . . . S2 S 0.8865(2) 0.64675(5) 0.77137(11) 0.0448(4) Uani 1 1 d DU . . O61 O 0.8636(8) 0.6209(2) 0.6677(3) 0.0547(11) Uani 0.920(4) 1 d PDU A 1 O62 O 0.9075(6) 0.60919(18) 0.8573(3) 0.0613(13) Uani 0.920(4) 1 d PDU A 1 O63 O 0.7126(5) 0.67977(16) 0.7718(4) 0.0607(13) Uani 0.920(4) 1 d PDU A 1 O64 O 1.0688(5) 0.67885(17) 0.7900(3) 0.0555(12) Uani 0.920(4) 1 d PDU A 1 O71 O 0.855(7) 0.6194(15) 0.6695(19) 0.054(6) Uani 0.080(4) 1 d PDU A 2 O72 O 0.729(4) 0.6356(14) 0.827(3) 0.056(6) Uani 0.080(4) 1 d PDU A 2 O73 O 0.897(5) 0.7024(5) 0.754(3) 0.065(5) Uani 0.080(4) 1 d PDU A 2 O74 O 1.083(3) 0.6312(14) 0.841(3) 0.055(6) Uani 0.080(4) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O11 0.0287(9) 0.0270(10) 0.0339(10) -0.0007(9) 0.0070(9) -0.0015(9) O12 0.0320(11) 0.0255(11) 0.0354(12) -0.0021(11) 0.0051(11) -0.0010(10) O13 0.041(2) 0.041(2) 0.051(2) 0.0165(18) 0.0193(18) 0.0140(16) O14 0.043(2) 0.0242(19) 0.042(2) 0.0111(16) 0.0056(16) 0.0030(15) N11 0.037(2) 0.037(3) 0.046(3) 0.007(2) 0.016(2) 0.0087(19) N12 0.045(2) 0.026(2) 0.038(2) -0.0040(19) 0.009(2) -0.0021(19) N13 0.031(2) 0.021(2) 0.036(3) 0.0055(18) 0.0086(19) 0.0063(17) C11 0.040(3) 0.029(3) 0.030(3) 0.006(2) 0.013(2) 0.000(2) C12 0.034(3) 0.024(3) 0.037(3) 0.006(2) 0.007(2) 0.000(2) C13 0.0279(13) 0.0272(13) 0.0337(13) 0.0000(12) 0.0066(12) -0.0018(12) C14 0.0282(10) 0.0270(11) 0.0339(11) -0.0004(10) 0.0070(10) -0.0013(10) C15 0.0288(13) 0.0273(13) 0.0348(13) -0.0003(12) 0.0070(12) 0.0000(12) C16 0.032(3) 0.029(3) 0.036(3) 0.002(2) 0.009(2) -0.002(2) C11' 0.0300(10) 0.0261(10) 0.0348(10) -0.0017(9) 0.0061(9) -0.0010(9) C12' 0.0310(13) 0.0271(13) 0.0355(13) -0.0018(12) 0.0060(12) -0.0016(12) C13' 0.053(3) 0.026(3) 0.030(3) -0.003(2) 0.014(3) -0.006(2) C14' 0.037(3) 0.043(3) 0.034(3) 0.001(3) 0.013(2) -0.001(3) C15' 0.030(3) 0.037(3) 0.029(3) 0.003(2) 0.010(2) 0.003(2) C16' 0.027(3) 0.031(3) 0.036(3) 0.003(2) 0.005(2) 0.000(2) O21 0.0284(11) 0.0269(12) 0.0335(12) 0.0014(11) 0.0046(11) -0.0003(10) O22 0.0306(12) 0.0266(12) 0.0329(12) 0.0029(11) 0.0048(11) -0.0017(10) O23 0.033(2) 0.0277(19) 0.061(2) 0.0001(18) 0.0053(17) 0.0022(16) O24 0.044(2) 0.0228(19) 0.039(2) -0.0034(14) 0.0095(17) -0.0032(14) N21 0.038(2) 0.033(3) 0.038(2) 0.001(2) 0.003(2) -0.0059(19) N22 0.038(2) 0.027(2) 0.032(2) 0.0021(19) 0.0025(18) 0.0023(19) N23 0.028(2) 0.025(2) 0.036(3) -0.0009(19) 0.0062(19) 0.0040(17) C21 0.040(3) 0.032(3) 0.030(3) 0.001(2) 0.003(2) -0.003(2) C22 0.032(3) 0.035(3) 0.039(3) -0.005(2) 0.011(2) -0.003(2) C23 0.026(3) 0.030(3) 0.033(3) 0.002(2) 0.008(2) -0.002(2) C24 0.030(3) 0.032(3) 0.026(3) -0.002(2) 0.004(2) -0.004(2) C25 0.031(3) 0.028(3) 0.038(3) 0.004(2) 0.011(2) 0.000(2) C26 0.036(3) 0.025(3) 0.037(3) 0.000(2) 0.008(2) -0.005(2) C21' 0.0294(11) 0.0260(11) 0.0337(12) 0.0027(10) 0.0049(10) -0.0012(10) C22' 0.0303(13) 0.0257(14) 0.0345(14) 0.0034(12) 0.0047(12) -0.0019(12) C23' 0.043(3) 0.037(3) 0.033(3) 0.003(2) 0.007(2) -0.001(3) C24' 0.027(3) 0.033(3) 0.030(3) -0.002(2) 0.000(2) -0.005(2) C25' 0.025(3) 0.025(3) 0.039(3) -0.002(2) 0.000(2) 0.000(2) C26' 0.031(3) 0.034(3) 0.039(3) -0.001(2) 0.010(2) 0.002(2) O31 0.091(3) 0.061(3) 0.094(4) 0.005(3) 0.023(3) 0.006(3) O32 0.057(2) 0.051(2) 0.051(2) 0.005(2) 0.008(2) -0.001(2) O33 0.059(3) 0.060(3) 0.062(3) 0.003(2) 0.011(2) 0.003(2) O34 0.073(3) 0.034(2) 0.057(2) -0.0037(19) 0.009(2) -0.0030(19) O35 0.051(2) 0.063(3) 0.069(3) 0.001(2) 0.008(2) 0.001(2) O36 0.059(3) 0.066(3) 0.058(3) 0.003(2) 0.005(2) 0.005(2) O37 0.051(3) 0.062(3) 0.058(3) -0.003(2) 0.014(2) 0.001(2) O38 0.053(2) 0.068(3) 0.053(2) -0.003(2) 0.011(2) -0.019(2) O39 0.068(3) 0.059(3) 0.063(3) 0.015(2) 0.008(2) 0.000(2) O40 0.051(2) 0.054(2) 0.056(3) -0.001(2) 0.005(2) 0.0036(19) O41 0.060(3) 0.053(3) 0.064(3) -0.005(2) 0.013(2) 0.001(2) O42 0.072(3) 0.042(2) 0.077(3) -0.008(2) 0.019(2) 0.004(2) O43 0.042(2) 0.051(2) 0.049(2) -0.007(2) 0.0070(17) 0.001(2) O44 0.065(3) 0.070(3) 0.075(3) -0.023(2) 0.014(2) 0.006(2) S1 0.0373(8) 0.0375(8) 0.0355(7) 0.0007(6) 0.0068(6) -0.0010(6) O51 0.064(2) 0.026(2) 0.054(2) 0.0037(17) 0.0141(19) -0.0014(17) O52 0.052(2) 0.053(2) 0.034(2) -0.0025(17) 0.0075(16) -0.0067(17) O53 0.044(2) 0.054(2) 0.051(2) -0.0039(19) -0.0008(18) 0.0086(18) O54 0.040(2) 0.058(2) 0.041(2) 0.0022(18) 0.0117(16) -0.0071(18) S2 0.0434(9) 0.0491(8) 0.0399(8) -0.0006(7) 0.0053(6) 0.0032(7) O61 0.072(3) 0.054(3) 0.032(2) -0.003(2) -0.001(2) 0.007(2) O62 0.069(3) 0.077(3) 0.041(3) 0.017(2) 0.018(2) 0.017(2) O63 0.035(2) 0.060(3) 0.088(3) -0.017(2) 0.016(2) 0.011(2) O64 0.033(2) 0.069(3) 0.063(3) -0.004(2) 0.007(2) -0.010(2) O71 0.071(10) 0.052(10) 0.033(10) -0.003(9) -0.002(9) 0.006(10) O72 0.055(10) 0.080(10) 0.042(10) 0.018(10) 0.032(9) 0.020(10) O73 0.048(10) 0.056(7) 0.092(10) -0.009(10) 0.016(10) 0.011(10) O74 0.025(9) 0.069(10) 0.064(10) -0.004(10) -0.006(9) -0.008(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O11 C11' . . 1.394(5) y O11 C14 . . 1.443(5) y O12 C15' . . 1.397(5) y O12 C11' . . 1.446(6) y O13 C15 . . 1.428(5) y O13 H13d . . 0.8400 ? O14 C16 . . 1.432(6) y O14 H14c . . 0.8400 ? N11 C11 . . 1.480(6) y N11 H11a . . 0.9100 ? N11 H11b . . 0.9100 ? N11 H11c . . 0.9100 ? N12 C12' . . 1.501(6) y N12 H12a . . 0.9100 ? N12 H12b . . 0.9100 ? N12 H12c . . 0.9100 ? N13 C26' . . 1.271(6) y N13 C13 . . 1.480(6) y C11 C16 . . 1.517(7) y C11 C12 . . 1.540(7) y C11 H11d . . 1.0000 ? C12 C13 . . 1.518(6) y C12 H12d . . 0.9900 ? C12 H12e . . 0.9900 ? C13 C14 . . 1.534(6) y C13 H13a . . 1.0000 ? C14 C15 . . 1.520(6) y C14 H14a . . 1.0000 ? C15 C16 . . 1.508(7) y C15 H15a . . 1.0000 ? C16 H16a . . 1.0000 ? C11' C12' . . 1.525(6) y C11' H11e . . 1.0000 ? C12' C13' . . 1.499(7) y C12' H12f . . 1.0000 ? C13' C14' . . 1.490(7) y C13' H13b . . 0.9900 ? C13' H13c . . 0.9900 ? C14' C15' . . 1.323(7) y C14' H14b . . 0.9500 ? C15' C16' . . 1.463(7) y C16' N23 . . 1.267(6) y C16' H16b . . 0.9500 ? O21 C21' . . 1.393(5) y O21 C24 . . 1.457(5) y O22 C25' . . 1.398(6) y O22 C21' . . 1.427(5) y O23 C25 . . 1.411(5) y O23 H23d . . 0.8400 ? O24 C26 . . 1.443(6) y O24 H24c . . 0.8400 ? N21 C21 . . 1.499(6) y N21 H21a . . 0.9100 ? N21 H21b . . 0.9100 ? N21 H21c . . 0.9100 ? N22 C22' . . 1.503(6) y N22 H22a . . 0.9100 ? N22 H22b . . 0.9100 ? N22 H22c . . 0.9100 ? N23 C23 . . 1.476(6) y C21 C26 . . 1.525(7) y C21 C22 . . 1.528(7) y C21 H21d . . 1.0000 ? C22 C23 . . 1.519(7) y C22 H22d . . 0.9900 ? C22 H22e . . 0.9900 ? C23 C24 . . 1.527(6) y C23 H23c . . 1.0000 ? C24 C25 . . 1.535(7) y C24 H24b . . 1.0000 ? C25 C26 . . 1.533(7) y C25 H25a . . 1.0000 ? C26 H26 . . 1.0000 ? C21' C22' . . 1.528(6) y C21' H21e . . 1.0000 ? C22' C23' . . 1.515(7) y C22' H22f . . 1.0000 ? C23' C24' . . 1.505(7) y C23' H23a . . 0.9900 ? C23' H23b . . 0.9900 ? C24' C25' . . 1.316(6) y C24' H24a . . 0.9500 ? C25' C26' . . 1.468(7) y C26' H26a . . 0.9500 ? O31 H31a . . 0.874(7) ? O31 H31b . . 0.873(7) ? O32 H32a . . 0.874(7) ? O32 H32b . . 0.875(7) ? O33 H33a . . 0.874(7) ? O33 H33b . . 0.873(7) ? O34 H34a . . 0.873(7) ? O34 H34b . . 0.874(7) ? O35 H35a . . 0.873(7) ? O35 H35b . . 0.873(7) ? O36 H36a . . 0.873(7) ? O36 H36b . . 0.874(7) ? O37 H37a . . 0.873(7) ? O37 H37b . . 0.874(7) ? O38 H38a . . 0.874(7) ? O38 H38b . . 0.874(7) ? O39 H39a . . 0.873(7) ? O39 H39b . . 0.874(7) ? O40 H40a . . 0.873(7) ? O40 H40b . . 0.873(7) ? O41 H41a . . 0.873(7) ? O41 H41b . . 0.873(7) ? O42 H42a . . 0.873(7) ? O42 H42b . . 0.873(7) ? O43 H43a . . 0.873(7) ? O43 H43b . . 0.873(7) ? O44 H44a . . 0.871(6) ? O44 H44b . . 0.871(6) ? S1 O52 . . 1.457(3) y S1 O54 . . 1.462(3) y S1 O53 . . 1.473(4) y S1 O51 . . 1.497(4) y S2 O72 . . 1.444(10) y S2 O62 . . 1.449(4) y S2 O71 . . 1.449(9) y S2 O61 . . 1.453(4) y S2 O63 . . 1.472(4) y S2 O73 . . 1.475(10) y S2 O64 . . 1.479(4) y S2 O74 . . 1.488(10) y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11' O11 C14 . . . 116.0(3) y C15' O12 C11' . . . 116.4(4) y C15 O13 H13D . . . 109.5 ? C16 O14 H14C . . . 109.5 ? C11 N11 H11A . . . 109.5 ? C11 N11 H11B . . . 109.5 ? H11A N11 H11B . . . 109.5 ? C11 N11 H11C . . . 109.5 ? H11A N11 H11C . . . 109.5 ? H11B N11 H11C . . . 109.5 ? C12' N12 H12A . . . 109.5 ? C12' N12 H12B . . . 109.5 ? H12A N12 H12B . . . 109.5 ? C12' N12 H12C . . . 109.5 ? H12A N12 H12C . . . 109.5 ? H12B N12 H12C . . . 109.5 ? C26' N13 C13 . . . 117.2(4) y N11 C11 C16 . . . 110.3(4) y N11 C11 C12 . . . 110.1(4) y C16 C11 C12 . . . 109.0(4) y N11 C11 H11D . . . 109.1 ? C16 C11 H11D . . . 109.1 ? C12 C11 H11D . . . 109.1 ? C13 C12 C11 . . . 110.9(4) y C13 C12 H12D . . . 109.5 ? C11 C12 H12D . . . 109.5 ? C13 C12 H12E . . . 109.5 ? C11 C12 H12E . . . 109.5 ? H12D C12 H12E . . . 108.1 ? N13 C13 C12 . . . 108.7(4) y N13 C13 C14 . . . 108.8(4) y C12 C13 C14 . . . 111.1(4) y N13 C13 H13A . . . 109.4 ? C12 C13 H13A . . . 109.4 ? C14 C13 H13A . . . 109.4 ? O11 C14 C15 . . . 110.6(4) y O11 C14 C13 . . . 106.1(3) y C15 C14 C13 . . . 112.5(4) y O11 C14 H14A . . . 109.2 ? C15 C14 H14A . . . 109.2 ? C13 C14 H14A . . . 109.2 ? O13 C15 C16 . . . 111.8(4) y O13 C15 C14 . . . 106.4(4) y C16 C15 C14 . . . 113.0(4) y O13 C15 H15A . . . 108.5 ? C16 C15 H15A . . . 108.5 ? C14 C15 H15A . . . 108.5 ? O14 C16 C15 . . . 109.3(4) y O14 C16 C11 . . . 109.4(4) y C15 C16 C11 . . . 111.0(4) y O14 C16 H16A . . . 109.0 ? C15 C16 H16A . . . 109.0 ? C11 C16 H16A . . . 109.0 ? O11 C11' O12 . . . 110.6(3) y O11 C11' C12' . . . 106.6(4) y O12 C11' C12' . . . 110.3(4) y O11 C11' H11E . . . 109.8 ? O12 C11' H11E . . . 109.8 ? C12' C11' H11E . . . 109.8 ? C13' C12' N12 . . . 112.0(4) y C13' C12' C11' . . . 112.3(4) y N12 C12' C11' . . . 108.0(4) y C13' C12' H12F . . . 108.1 ? N12 C12' H12F . . . 108.1 ? C11' C12' H12F . . . 108.1 ? C14' C13' C12' . . . 108.7(4) y C14' C13' H13B . . . 109.9 ? C12' C13' H13B . . . 109.9 ? C14' C13' H13C . . . 109.9 ? C12' C13' H13C . . . 109.9 ? H13B C13' H13C . . . 108.3 ? C15' C14' C13' . . . 122.7(5) y C15' C14' H14B . . . 118.6 ? C13' C14' H14B . . . 118.6 ? C14' C15' O12 . . . 124.2(4) y C14' C15' C16' . . . 122.6(5) y O12 C15' C16' . . . 113.2(4) y N23 C16' C15' . . . 125.1(5) y N23 C16' H16B . . . 117.4 ? C15' C16' H16B . . . 117.4 ? C21' O21 C24 . . . 116.0(3) y C25' O22 C21' . . . 116.7(3) y C25 O23 H23D . . . 109.5 ? C26 O24 H24C . . . 109.5 ? C21 N21 H21A . . . 109.5 ? C21 N21 H21B . . . 109.5 ? H21A N21 H21B . . . 109.5 ? C21 N21 H21C . . . 109.5 ? H21A N21 H21C . . . 109.5 ? H21B N21 H21C . . . 109.5 ? C22' N22 H22A . . . 109.5 ? C22' N22 H22B . . . 109.5 ? H22A N22 H22B . . . 109.5 ? C22' N22 H22C . . . 109.5 ? H22A N22 H22C . . . 109.5 ? H22B N22 H22C . . . 109.5 ? C16' N23 C23 . . . 115.1(4) y N21 C21 C26 . . . 109.9(4) y N21 C21 C22 . . . 110.4(4) y C26 C21 C22 . . . 109.7(4) y N21 C21 H21D . . . 108.9 ? C26 C21 H21D . . . 108.9 ? C22 C21 H21D . . . 108.9 ? C23 C22 C21 . . . 109.6(4) y C23 C22 H22D . . . 109.7 ? C21 C22 H22D . . . 109.7 ? C23 C22 H22E . . . 109.7 ? C21 C22 H22E . . . 109.7 ? H22D C22 H22E . . . 108.2 ? N23 C23 C22 . . . 110.5(4) y N23 C23 C24 . . . 109.7(4) y C22 C23 C24 . . . 109.4(4) y N23 C23 H23C . . . 109.0 ? C22 C23 H23C . . . 109.0 ? C24 C23 H23C . . . 109.0 ? O21 C24 C23 . . . 107.0(4) y O21 C24 C25 . . . 108.6(4) y C23 C24 C25 . . . 111.9(4) y O21 C24 H24B . . . 109.8 ? C23 C24 H24B . . . 109.8 ? C25 C24 H24B . . . 109.8 ? O23 C25 C26 . . . 111.7(4) y O23 C25 C24 . . . 107.9(4) y C26 C25 C24 . . . 111.1(4) y O23 C25 H25A . . . 108.7 ? C26 C25 H25A . . . 108.7 ? C24 C25 H25A . . . 108.7 ? O24 C26 C21 . . . 110.7(4) y O24 C26 C25 . . . 110.1(4) y C21 C26 C25 . . . 110.4(4) y O24 C26 H26 . . . 108.5 ? C21 C26 H26 . . . 108.5 ? C25 C26 H26 . . . 108.5 ? O21 C21' O22 . . . 111.1(3) y O21 C21' C22' . . . 105.9(4) y O22 C21' C22' . . . 111.1(4) y O21 C21' H21E . . . 109.6 ? O22 C21' H21E . . . 109.6 ? C22' C21' H21E . . . 109.6 ? N22 C22' C23' . . . 110.8(4) y N22 C22' C21' . . . 107.8(4) y C23' C22' C21' . . . 111.9(4) y N22 C22' H22F . . . 108.8 ? C23' C22' H22F . . . 108.8 ? C21' C22' H22F . . . 108.8 ? C24' C23' C22' . . . 108.1(4) y C24' C23' H23A . . . 110.1 ? C22' C23' H23A . . . 110.1 ? C24' C23' H23B . . . 110.1 ? C22' C23' H23B . . . 110.1 ? H23A C23' H23B . . . 108.4 ? C25' C24' C23' . . . 122.9(4) y C25' C24' H24A . . . 118.6 ? C23' C24' H24A . . . 118.6 ? C24' C25' O22 . . . 124.4(4) y C24' C25' C26' . . . 122.6(5) y O22 C25' C26' . . . 113.0(4) y N13 C26' C25' . . . 124.5(4) y N13 C26' H26A . . . 117.8 ? C25' C26' H26A . . . 117.8 ? H31A O31 H31B . . . 107(5) ? H32A O32 H32B . . . 106(4) ? H33A O33 H33B . . . 106(5) ? H34A O34 H34B . . . 106(4) ? H35A O35 H35B . . . 106(5) ? H36A O36 H36B . . . 106(4) ? H37A O37 H37B . . . 106(4) ? H38A O38 H38B . . . 106(5) ? H39A O39 H39B . . . 106(5) ? H40A O40 H40B . . . 106(5) ? H41A O41 H41B . . . 106(4) ? H42A O42 H42B . . . 106(6) ? H43A O43 H43B . . . 106(4) ? H44A O44 H44B . . . 106(4) ? O52 S1 O54 . . . 110.6(2) y O52 S1 O53 . . . 109.3(2) y O54 S1 O53 . . . 111.1(2) y O52 S1 O51 . . . 108.7(2) y O54 S1 O51 . . . 107.6(2) y O53 S1 O51 . . . 109.6(2) y O72 S2 O62 . . . 57.1(13) y O72 S2 O71 . . . 110.8(13) y O62 S2 O71 . . . 107.7(18) y O72 S2 O61 . . . 113.9(17) y O62 S2 O61 . . . 109.6(3) y O72 S2 O63 . . . 54.7(14) y O62 S2 O63 . . . 109.8(3) y O71 S2 O63 . . . 109.5(18) y O61 S2 O63 . . . 110.7(3) y O72 S2 O73 . . . 109.9(12) y O62 S2 O73 . . . 141.4(17) y O71 S2 O73 . . . 110.8(12) y O61 S2 O73 . . . 108.7(18) y O63 S2 O73 . . . 59.3(14) y O72 S2 O64 . . . 137.2(16) y O62 S2 O64 . . . 109.1(3) y O71 S2 O64 . . . 112.0(18) y O61 S2 O64 . . . 108.9(3) y O63 S2 O64 . . . 108.8(3) y O73 S2 O64 . . . 52.9(14) y O72 S2 O74 . . . 109.4(12) y O62 S2 O74 . . . 56.4(14) y O71 S2 O74 . . . 109.0(13) y O61 S2 O74 . . . 107.9(17) y O63 S2 O74 . . . 141.4(16) y O73 S2 O74 . . . 106.8(12) y O64 S2 O74 . . . 56.1(14) y loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N11 C11 C12 C13 . . . . 178.7(4) y C16 C11 C12 C13 . . . . -60.2(5) y C26' N13 C13 C12 . . . . 148.6(4) y C26' N13 C13 C14 . . . . -90.3(5) y C11 C12 C13 N13 . . . . 175.8(4) y C11 C12 C13 C14 . . . . 56.1(5) y C11' O11 C14 C15 . . . . 85.3(4) y C11' O11 C14 C13 . . . . -152.5(4) y N13 C13 C14 O11 . . . . 68.7(4) y C12 C13 C14 O11 . . . . -171.7(4) y N13 C13 C14 C15 . . . . -170.2(4) y C12 C13 C14 C15 . . . . -50.6(5) y O11 C14 C15 O13 . . . . -68.4(4) y C13 C14 C15 O13 . . . . 173.2(4) y O11 C14 C15 C16 . . . . 168.5(4) y C13 C14 C15 C16 . . . . 50.1(5) y O13 C15 C16 O14 . . . . 64.5(5) y C14 C15 C16 O14 . . . . -175.5(4) y O13 C15 C16 C11 . . . . -174.7(4) y C14 C15 C16 C11 . . . . -54.7(5) y N11 C11 C16 O14 . . . . -59.4(5) y C12 C11 C16 O14 . . . . 179.6(4) y N11 C11 C16 C15 . . . . 179.8(4) y C12 C11 C16 C15 . . . . 58.8(5) y C14 O11 C11' O12 . . . . 74.7(5) y C14 O11 C11' C12' . . . . -165.4(4) y C15' O12 C11' O11 . . . . 79.8(5) y C15' O12 C11' C12' . . . . -37.8(5) y O11 C11' C12' C13' . . . . -62.1(5) y O12 C11' C12' C13' . . . . 58.1(5) y O11 C11' C12' N12 . . . . 62.0(5) y O12 C11' C12' N12 . . . . -177.9(3) y N12 C12' C13' C14' . . . . -169.5(4) y C11' C12' C13' C14' . . . . -47.7(5) y C12' C13' C14' C15' . . . . 20.6(7) y C13' C14' C15' O12 . . . . -1.6(8) y C13' C14' C15' C16' . . . . 178.5(4) y C11' O12 C15' C14' . . . . 10.9(6) y C11' O12 C15' C16' . . . . -169.2(4) y C14' C15' C16' N23 . . . . -167.3(5) y O12 C15' C16' N23 . . . . 12.8(7) y C15' C16' N23 C23 . . . . 177.1(4) y N21 C21 C22 C23 . . . . 176.5(4) y C26 C21 C22 C23 . . . . -62.3(5) y C16' N23 C23 C22 . . . . 149.4(4) y C16' N23 C23 C24 . . . . -89.8(5) y C21 C22 C23 N23 . . . . -178.6(4) y C21 C22 C23 C24 . . . . 60.5(5) y C21' O21 C24 C23 . . . . -149.5(4) y C21' O21 C24 C25 . . . . 89.6(4) y N23 C23 C24 O21 . . . . 63.2(5) y C22 C23 C24 O21 . . . . -175.3(4) y N23 C23 C24 C25 . . . . -177.9(4) y C22 C23 C24 C25 . . . . -56.5(5) y O21 C24 C25 O23 . . . . -65.8(5) y C23 C24 C25 O23 . . . . 176.4(4) y O21 C24 C25 C26 . . . . 171.4(4) y C23 C24 C25 C26 . . . . 53.6(5) y N21 C21 C26 O24 . . . . -57.4(5) y C22 C21 C26 O24 . . . . -179.0(4) y N21 C21 C26 C25 . . . . -179.7(4) y C22 C21 C26 C25 . . . . 58.7(5) y O23 C25 C26 O24 . . . . 62.6(5) y C24 C25 C26 O24 . . . . -176.8(4) y O23 C25 C26 C21 . . . . -174.8(4) y C24 C25 C26 C21 . . . . -54.3(5) y C24 O21 C21' O22 . . . . 82.1(4) y C24 O21 C21' C22' . . . . -157.2(3) y C25' O22 C21' O21 . . . . 80.4(4) y C25' O22 C21' C22' . . . . -37.2(5) y O21 C21' C22' N22 . . . . 59.1(4) y O22 C21' C22' N22 . . . . 179.8(3) y O21 C21' C22' C23' . . . . -63.0(5) y O22 C21' C22' C23' . . . . 57.8(5) y N22 C22' C23' C24' . . . . -167.6(4) y C21' C22' C23' C24' . . . . -47.3(5) y C22' C23' C24' C25' . . . . 20.7(6) y C23' C24' C25' O22 . . . . -1.2(7) y C23' C24' C25' C26' . . . . 176.0(4) y C21' O22 C25' C24' . . . . 9.8(6) y C21' O22 C25' C26' . . . . -167.5(4) y C13 N13 C26' C25' . . . . 176.2(4) y C24' C25' C26' N13 . . . . -170.1(4) y O22 C25' C26' N13 . . . . 7.3(6) y 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 _geom_hbond_publ_flag O13 H13D O24 0.84 2.03 2.774(4) 147.3 2 y O14 H14C O52 0.84 1.88 2.699(4) 162.9 2_655 y N11 H11A O37 0.91 2.04 2.832(5) 145.3 1_654 y N11 H11B O43 0.91 2.11 2.863(5) 140 2_655 y N11 H11B O24 0.91 2.56 3.171(5) 125.5 2_655 y N11 H11C O35 0.91 1.98 2.869(6) 164.4 1_554 y N12 H12A O36 0.91 2 2.889(6) 163.8 2_656 y N12 H12B O54 0.91 1.92 2.774(5) 155 2_656 y N12 H12C O39 0.91 2.04 2.854(6) 148.4 2_556 y O23 H23D O43 0.84 2.11 2.902(5) 156.4 . y O23 H23D O14 0.84 2.6 3.047(4) 114.4 2_645 y O24 H24C O52 0.84 1.96 2.734(5) 153.6 1_455 y N21 H21A O72 0.91 1.78 2.59(3) 146.5 1_454 y N21 H21A O62 0.91 1.88 2.773(5) 168.5 1_454 y N21 H21B O40 0.91 1.86 2.766(5) 174.1 1_454 y N21 H21C O14 0.91 2.07 2.962(5) 167.5 2_545 y N22 H22A O38 0.91 1.96 2.850(5) 165.2 . y N22 H22B O61 0.91 1.8 2.700(6) 168.3 . y N22 H22B O71 0.91 1.81 2.71(4) 167.5 . y N22 H22C O51 0.91 2.21 2.900(5) 132.6 . y N22 H22C O54 0.91 2.51 3.233(5) 137.3 . y O31 H31A O38 0.874(7) 2.104(14) 2.970(6) 171(6) . y O31 H31B O64 0.873(7) 2.03(3) 2.841(6) 155(6) 1_455 y O31 H31B O73 0.873(7) 2.10(6) 2.80(3) 136(6) 1_455 y O32 H32A N23 0.874(7) 2.024(17) 2.853(5) 158(4) . y O32 H32B O34 0.875(7) 1.921(13) 2.782(5) 168(5) . y O33 H33A O31 0.874(7) 1.96(3) 2.774(6) 154(6) . y O33 H33B O42 0.873(7) 1.946(11) 2.801(6) 166(3) 1_455 y O34 H34A O41 0.873(7) 1.971(11) 2.826(6) 166(3) 1_554 y O34 H34B N13 0.874(7) 2.02(3) 2.854(5) 160(7) . y O35 H35A O33 0.873(7) 1.949(18) 2.808(6) 168(7) . y O35 H35B O41 0.873(7) 2.04(2) 2.887(6) 165(7) . y O36 H36A O53 0.873(7) 1.958(17) 2.816(5) 167(6) 1_455 y O36 H36B O44 0.874(7) 1.894(11) 2.720(6) 157(2) . y O37 H37A O33 0.873(7) 1.963(10) 2.835(6) 177(5) . y O37 H37B O32 0.874(7) 1.875(11) 2.744(5) 173(6) 1_556 y O38 H38A O51 0.874(7) 1.891(12) 2.757(5) 171(6) 1_455 y O38 H38B O44 0.874(7) 1.886(19) 2.722(6) 159(5) . y O39 H39A O36 0.873(7) 2.12(2) 2.946(6) 157(5) . y O39 H39B O62 0.874(7) 1.95(3) 2.778(6) 157(7) 1_455 y O39 H39B O74 0.874(7) 1.98(5) 2.76(4) 148(5) 1_455 y O40 H40A O74 0.873(7) 1.84(5) 2.61(3) 146(5) 1_455 y O40 H40A O64 0.873(7) 1.94(2) 2.773(5) 159(5) 1_455 y O40 H40B O34 0.873(7) 1.90(4) 2.696(5) 151(7) 1_556 y O41 H41A O73 0.873(7) 2.20(4) 2.80(3) 125(3) . y O41 H41A O32 0.873(7) 2.38(4) 2.801(5) 110(3) 1_656 y O41 H41B O63 0.873(7) 2.24(2) 2.801(6) 121(2) . y O42 H42A O35 0.873(7) 2.18(2) 3.006(6) 158(5) . y O42 H42B O53 0.873(7) 2.12(2) 2.959(6) 162(7) 2_756 y O43 H43A O54 0.873(7) 1.850(13) 2.718(4) 172(6) . y O43 H43B O53 0.873(7) 1.988(13) 2.853(5) 171(6) 1_455 y O44 H44A O72 0.871(6) 1.72(4) 2.49(3) 145(4) . y O44 H44A O63 0.871(6) 2.07(6) 2.653(6) 124(6) . y O44 H44B O74 0.871(6) 1.92(5) 2.72(4) 151(5) 1_455 y O44 H44B O64 0.871(6) 1.93(3) 2.762(6) 160(7) 1_455 y _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 53.69 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.225 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.049 #=== END OF THE CIF FILE # Attachment '- BENT68.cif' data_bent68 _database_code_depnum_ccdc_archive 'CCDC 838349' #TrackingRef '- BENT68.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H42 N6 O8, 2(O4 S), 14(H2 O) ' _chemical_formula_sum 'C24 H70 N6 O30 S2' _chemical_formula_weight 986.98 _chemical_compound_source 'Synthesized by the authors. See text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M C2221 _symmetry_space_group_name_hall 'C 2c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.74530(10) _cell_length_b 25.6806(5) _cell_length_c 25.6822(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4448.76(14) _cell_formula_units_Z 4 _cell_measurement_temperature 170 _cell_measurement_reflns_used 20614 _cell_measurement_theta_min 3.44 _cell_measurement_theta_max 72.30 _exptl_crystal_description needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 2.005 _exptl_absorpt_correction_Type multi-scan _exptl_absorpt_correction_T_min 0.7782 _exptl_absorpt_correction_T_max 0.9607 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 2004)' _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Platform diffractometer, equipped with a Bruker SMART 4K Charged-Coupled Device (CCD) Area Detector using the program APEX2 and a Nonius FR591 rotating anode equiped with a Helios optics. The crystal-to-detector distance was 5.0 cm, and the data collection was carried out in 512 x 512 pixel mode. The initial unit cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 10.0 degree scan in 33 frames over four different parts of the reciprocal space (132 frames total). One complete sphere of data was collected, to better than 0.80\%A resolution. ; _vrf_PLAT420_bent68 ; RESPONSE: This is attributed to a disordered hydrogen bond network resulting from a disordered water molecule (O15) which may appear on either side of the corresponding symmetry element. ; _diffrn_ambient_temperature 170 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Helios optics' _diffrn_measurement_device_type 'Bruker Smart 6000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 5.5 _diffrn_reflns_number 29758 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 72.54 _reflns_number_total 4389 _reflns_number_gt 4200 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT V7.60A(Bruker AXS, 2008)' _computing_data_reduction 'SAINT V7.60A(Bruker AXS, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_publication_material 'UdMX (Maris, 2004)' _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^)+(0.0717P)^2^+1.6615P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), 1878 Friedel Pairs' _chemical_absolute_configuration rmad _refine_ls_abs_structure_Flack 0.017(16) _refine_ls_number_reflns 4389 _refine_ls_number_parameters 364 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 0.52956(7) 0.099724(18) 0.53210(2) 0.02949(13) Uani 1 1 d . . . O1 O -0.2483(2) 0.10784(5) 0.31285(5) 0.0226(3) Uani 1 1 d . . . O2 O 0.01619(19) 0.09709(5) 0.37059(5) 0.0220(3) Uani 1 1 d . . . O3 O -0.0660(2) 0.17230(7) 0.45098(5) 0.0319(3) Uani 1 1 d . . . H3 H -0.0635 0.1703 0.4836 0.048 Uiso 1 1 calc R . . O4 O 0.2921(2) 0.22265(6) 0.49185(5) 0.0273(3) Uani 1 1 d . . . H4 H 0.3568 0.1981 0.5052 0.041 Uiso 1 1 calc R . . O5 O 0.5023(3) 0.08811(6) 0.47635(6) 0.0393(4) Uani 1 1 d . . . O6 O 0.5501(3) 0.15605(6) 0.53965(7) 0.0384(4) Uani 1 1 d . . . O7 O 0.3579(3) 0.08050(7) 0.56167(7) 0.0440(4) Uani 1 1 d . . . O8 O 0.7119(3) 0.07337(7) 0.55017(8) 0.0474(5) Uani 1 1 d . . . N1 N 0.5823(3) 0.25214(7) 0.41669(6) 0.0288(4) Uani 1 1 d . . . H1A H 0.6340 0.2520 0.4494 0.043 Uiso 1 1 calc R . . H1B H 0.5078 0.2813 0.4121 0.043 Uiso 1 1 calc R . . H1C H 0.6825 0.2517 0.3930 0.043 Uiso 1 1 calc R . . N2 N 0.2703(2) 0.13359(6) 0.29059(6) 0.0218(3) Uani 1 1 d . . . N3 N -0.1836(3) 0.02838(7) 0.43291(6) 0.0310(4) Uani 1 1 d . . . H3A H -0.2194 -0.0046 0.4419 0.046 Uiso 1 1 calc R . . H3B H -0.2394 0.0514 0.4555 0.046 Uiso 1 1 calc R . . H3C H -0.0493 0.0314 0.4342 0.046 Uiso 1 1 calc R . . C1 C 0.4548(3) 0.20493(7) 0.40938(7) 0.0228(4) Uani 1 1 d . . . H1 H 0.5251 0.1743 0.4247 0.027 Uiso 1 1 calc R . . C2 C 0.4202(3) 0.19449(7) 0.35168(7) 0.0236(4) Uani 1 1 d . . . H2A H 0.3455 0.2237 0.3360 0.028 Uiso 1 1 calc R . . H2B H 0.5490 0.1914 0.3334 0.028 Uiso 1 1 calc R . . C3 C 0.3032(3) 0.14409(7) 0.34582(7) 0.0207(4) Uani 1 1 d . . . H3D H 0.3811 0.1148 0.3613 0.025 Uiso 1 1 calc R . . C4 C 0.1025(3) 0.14806(7) 0.37377(7) 0.0213(4) Uani 1 1 d . . . H4A H 0.0158 0.1739 0.3556 0.026 Uiso 1 1 calc R . . C5 C 0.1274(3) 0.16341(8) 0.43092(7) 0.0236(4) Uani 1 1 d . . . H5 H 0.1887 0.1337 0.4502 0.028 Uiso 1 1 calc R . . C6 C 0.2584(3) 0.21192(7) 0.43795(7) 0.0237(4) Uani 1 1 d . . . H6 H 0.1877 0.2424 0.4223 0.028 Uiso 1 1 calc R . . C1' C -0.1896(3) 0.09483(7) 0.36478(7) 0.0213(3) Uani 1 1 d . . . H1' H -0.2522 0.1200 0.3895 0.026 Uiso 1 1 calc R . . C2' C -0.2535(3) 0.03969(7) 0.37926(7) 0.0249(4) Uani 1 1 d . . . H2' H -0.4017 0.0380 0.3788 0.030 Uiso 1 1 calc R . . C3' C -0.1732(3) -0.00053(8) 0.34159(7) 0.0270(4) Uani 1 1 d . . . H3'1 H -0.0289 -0.0050 0.3469 0.032 Uiso 1 1 calc R . . H3'2 H -0.2387 -0.0345 0.3476 0.032 Uiso 1 1 calc R . . C4' C -0.2133(3) 0.01786(7) 0.28738(7) 0.0254(4) Uani 1 1 d . . . H4' H -0.2178 -0.0069 0.2599 0.031 Uiso 1 1 calc R . . C5' C -0.2430(3) 0.06827(7) 0.27656(7) 0.0220(4) Uani 1 1 d . . . C6' C -0.2756(3) 0.08584(7) 0.22302(7) 0.0231(4) Uani 1 1 d . . . H6' H -0.3020 0.0604 0.1971 0.028 Uiso 1 1 calc R . . O9 O 0.6929(4) 0.17760(9) 0.64269(9) 0.0627(6) Uani 1 1 d D . . H9A H 0.665(7) 0.1654(15) 0.6119(8) 0.094 Uiso 1 1 d D . . H9B H 0.651(13) 0.1524(19) 0.6627(16) 0.094 Uiso 0.50 1 d PD A 1 H9C H 0.596(7) 0.199(3) 0.650(2) 0.094 Uiso 0.50 1 d PD B 2 O10 O 0.8460(3) 0.27052(7) 0.32875(7) 0.0423(4) Uani 1 1 d D . . H10A H 0.889(5) 0.2485(10) 0.3055(10) 0.063 Uiso 1 1 d D . . H10B H 0.749(4) 0.2859(12) 0.3136(11) 0.063 Uiso 1 1 d D . . O11 O 0.0162(3) 0.14328(7) 0.55899(7) 0.0403(4) Uani 1 1 d D . . H11A H -0.078(3) 0.1200(10) 0.5605(14) 0.060 Uiso 1 1 d D . . H11B H 0.121(3) 0.1248(11) 0.5656(14) 0.060 Uiso 1 1 d D . . O12A O 0.2385(9) 0.0197(2) 0.4308(2) 0.0520(13) Uani 0.60 1 d PD C 3 H12A H 0.315(9) 0.039(2) 0.449(3) 0.078 Uiso 0.60 1 d PD D 3 H12B H 0.258(11) -0.0121(8) 0.439(3) 0.078 Uiso 0.60 1 d PD E 3 O12B O 0.1876(15) 0.0179(4) 0.4551(5) 0.079(3) Uani 0.40 1 d PD F 4 H12C H 0.289(10) 0.038(3) 0.460(7) 0.118 Uiso 0.40 1 d PD G 4 H12D H 0.228(16) -0.0138(14) 0.455(6) 0.118 Uiso 0.40 1 d PD H 4 O13 O 1.0441(4) 0.15819(10) 0.69691(9) 0.0650(6) Uani 1 1 d D . . H13A H 1.112(8) 0.132(2) 0.685(4) 0.097 Uiso 0.50 1 d PD I 7 H13B H 0.924(4) 0.152(3) 0.686(3) 0.097 Uiso 0.50 1 d PD J 7 H13C H 1.048(10) 0.164(2) 0.7305(5) 0.097 Uiso 0.50 1 d PD K 8 H13D H 0.995(15) 0.1265(16) 0.6948(19) 0.097 Uiso 0.50 1 d PD L 8 O14 O 0.2670(4) 0.07010(11) 0.67229(9) 0.0724(7) Uani 1 1 d D . . H14A H 0.313(7) 0.0804(16) 0.6421(9) 0.109 Uiso 1 1 d D . . H14B H 0.353(8) 0.082(3) 0.6939(16) 0.109 Uiso 0.50 1 d PD M 5 H14C H 0.276(17) 0.0365(5) 0.669(3) 0.109 Uiso 0.50 1 d PD N 6 O15 O 0.5554(12) 0.1004(3) 0.7338(3) 0.099(2) Uani 0.50 1 d PD . . H15A H 0.53(2) 0.109(4) 0.7657(17) 0.148 Uiso 0.50 1 d PD . . H15B H 0.615(11) 0.126(3) 0.719(2) 0.148 Uiso 0.50 1 d PD . . O16 O 0.0000 0.20726(8) 0.2500 0.0338(5) Uani 1 2 d SD . . H16A H 0.103(3) 0.1878(10) 0.2572(13) 0.051 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0248(2) 0.0286(2) 0.0350(2) 0.00233(18) -0.00336(19) 0.00112(19) O1 0.0242(6) 0.0244(6) 0.0193(6) 0.0018(5) -0.0026(5) 0.0011(5) O2 0.0192(6) 0.0227(6) 0.0243(6) -0.0003(5) -0.0009(5) 0.0001(5) O3 0.0232(7) 0.0481(8) 0.0246(6) -0.0074(6) 0.0046(5) -0.0010(6) O4 0.0300(7) 0.0321(7) 0.0197(6) -0.0064(5) -0.0021(5) 0.0037(6) O5 0.0400(8) 0.0415(8) 0.0363(8) -0.0039(6) 0.0004(7) 0.0017(7) O6 0.0397(9) 0.0301(8) 0.0453(9) -0.0008(6) -0.0109(7) 0.0031(6) O7 0.0409(9) 0.0440(9) 0.0471(9) 0.0025(7) 0.0094(8) -0.0049(7) O8 0.0350(9) 0.0339(8) 0.0733(12) 0.0107(8) -0.0170(8) 0.0019(7) N1 0.0321(9) 0.0307(8) 0.0236(8) -0.0042(7) 0.0002(6) -0.0050(7) N2 0.0191(7) 0.0287(8) 0.0177(7) -0.0030(6) -0.0009(6) -0.0008(6) N3 0.0438(10) 0.0300(9) 0.0192(7) 0.0051(6) 0.0011(7) -0.0005(8) C1 0.0224(9) 0.0236(8) 0.0224(8) -0.0022(6) -0.0024(7) -0.0008(7) C2 0.0224(9) 0.0288(9) 0.0196(8) -0.0014(7) 0.0002(7) -0.0005(7) C3 0.0186(8) 0.0256(9) 0.0178(8) -0.0022(6) 0.0001(7) 0.0002(7) C4 0.0194(8) 0.0233(8) 0.0213(8) -0.0007(7) 0.0000(7) -0.0002(7) C5 0.0222(9) 0.0295(9) 0.0190(8) -0.0020(7) 0.0019(7) 0.0036(7) C6 0.0256(9) 0.0280(9) 0.0175(8) -0.0027(7) -0.0021(7) 0.0049(7) C1' 0.0197(8) 0.0269(9) 0.0172(8) -0.0002(7) -0.0007(6) 0.0016(7) C2' 0.0247(9) 0.0298(10) 0.0201(8) 0.0047(7) 0.0001(7) -0.0017(8) C3' 0.0329(10) 0.0235(9) 0.0247(9) 0.0023(7) -0.0013(8) 0.0002(8) C4' 0.0267(9) 0.0272(9) 0.0224(8) 0.0002(7) -0.0001(7) -0.0011(7) C5' 0.0186(8) 0.0270(9) 0.0204(9) -0.0009(7) -0.0005(7) -0.0028(7) C6' 0.0199(8) 0.0280(9) 0.0212(9) -0.0002(7) -0.0017(7) -0.0024(7) O9 0.0549(12) 0.0701(14) 0.0632(12) -0.0222(10) -0.0158(10) 0.0135(11) O10 0.0430(10) 0.0428(9) 0.0409(9) -0.0022(7) 0.0066(8) -0.0026(8) O11 0.0316(8) 0.0421(9) 0.0471(9) -0.0005(7) 0.0020(7) -0.0037(7) O12A 0.041(3) 0.0356(19) 0.080(3) 0.004(2) -0.028(2) 0.0032(16) O12B 0.056(6) 0.053(4) 0.128(9) -0.020(6) -0.049(6) 0.013(4) O13 0.0585(14) 0.0861(16) 0.0503(11) 0.0026(11) -0.0009(10) -0.0050(12) O14 0.0742(16) 0.0855(17) 0.0573(13) 0.0088(11) 0.0006(12) -0.0107(14) O15 0.108(6) 0.093(4) 0.095(5) 0.017(3) -0.028(4) -0.011(4) O16 0.0379(12) 0.0313(10) 0.0322(10) 0.000 -0.0059(9) 0.000 _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_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 O6 . . 1.4661(15) y S1 O7 . . 1.4700(18) y S1 O5 . . 1.4738(16) y S1 O8 . . 1.4785(17) y O1 C5' . . 1.379(2) y O1 C1' . . 1.431(2) y O2 C1' . . 1.397(2) y O2 C4 . . 1.435(2) y O3 C5 . . 1.421(2) y O3 H3 . . 0.8400 ? O4 C6 . . 1.430(2) y O4 H4 . . 0.8400 ? N1 C1 . . 1.498(2) y N1 H1a . . 0.9100 ? N1 H1b . . 0.9100 ? N1 H1c . . 0.9100 ? N2 C6' . 3 1.275(2) y N2 C3 . . 1.461(2) y N3 C2' . . 1.485(2) y N3 H3a . . 0.9100 ? N3 H3b . . 0.9100 ? N3 H3c . . 0.9100 ? C1 C2 . . 1.524(2) y C1 C6 . . 1.525(3) y C1 H1 . . 1.0000 ? C2 C3 . . 1.524(2) y C2 H2a . . 0.9900 ? C2 H2b . . 0.9900 ? C3 C4 . . 1.536(2) y C3 H3d . . 1.0000 ? C4 C5 . . 1.529(2) y C4 H4a . . 1.0000 ? C5 C6 . . 1.538(3) y C5 H5 . . 1.0000 ? C6 H6 . . 1.0000 ? C1' C2' . . 1.526(3) y C1' H1' . . 1.0000 ? C2' C3' . . 1.515(3) y C2' H2' . . 1.0000 ? C3' C4' . . 1.495(3) y C3' H3'1 . . 0.9900 ? C3' H3'2 . . 0.9900 ? C4' C5' . . 1.339(3) y C4' H4' . . 0.9500 ? C5' C6' . . 1.464(2) y C6' N2 . 3 1.275(2) y C6' H6' . . 0.9500 ? O9 H9a . . 0.871(10) ? O9 H9b . . 0.873(10) ? O9 H9c . . 0.866(10) ? O10 H10a . . 0.872(10) ? O10 H10b . . 0.859(10) ? O11 H11a . . 0.875(10) ? O11 H11b . . 0.867(10) ? O12a H12a . . 0.862(10) ? O12a H12b . . 0.856(10) ? O12a H12c . . 0.94(12) ? O12a H12d . . 1.06(9) ? O12b H12a . . 1.03(6) ? O12b H12b . . 0.99(6) ? O12b H12c . . 0.861(11) ? O12b H12d . . 0.858(10) ? O13 H13a . . 0.873(10) ? O13 H13b . . 0.873(10) ? O13 H13c . . 0.873(10) ? O13 H13d . . 0.879(10) ? O14 H14a . . 0.876(10) ? O14 H14b . . 0.867(10) ? O14 H14c . . 0.868(10) ? O15 O15 . 3_656 1.118(15) y O15 H15a . . 0.861(10) ? O15 H15b . . 0.861(10) ? O16 H16a . . 0.874(10) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O6 S1 O7 . . . 109.72(11) y O6 S1 O5 . . . 109.87(10) y O7 S1 O5 . . . 109.62(10) y O6 S1 O8 . . . 109.37(10) y O7 S1 O8 . . . 109.82(11) y O5 S1 O8 . . . 108.41(11) y C5' O1 C1' . . . 116.77(14) y C1' O2 C4 . . . 116.56(14) y C5 O3 H3 . . . 109.5 ? C6 O4 H4 . . . 109.5 ? C1 N1 H1A . . . 109.5 ? C1 N1 H1B . . . 109.5 ? H1A N1 H1B . . . 109.5 ? C1 N1 H1C . . . 109.5 ? H1A N1 H1C . . . 109.5 ? H1B N1 H1C . . . 109.5 ? C6' N2 C3 3 . . 116.06(16) y C2' N3 H3A . . . 109.5 ? C2' N3 H3B . . . 109.5 ? H3A N3 H3B . . . 109.5 ? C2' N3 H3C . . . 109.5 ? H3A N3 H3C . . . 109.5 ? H3B N3 H3C . . . 109.5 ? N1 C1 C2 . . . 110.61(15) y N1 C1 C6 . . . 110.07(15) y C2 C1 C6 . . . 110.84(15) y N1 C1 H1 . . . 108.4 ? C2 C1 H1 . . . 108.4 ? C6 C1 H1 . . . 108.4 ? C3 C2 C1 . . . 108.95(15) y C3 C2 H2A . . . 109.9 ? C1 C2 H2A . . . 109.9 ? C3 C2 H2B . . . 109.9 ? C1 C2 H2B . . . 109.9 ? H2A C2 H2B . . . 108.3 ? N2 C3 C2 . . . 109.35(14) y N2 C3 C4 . . . 109.42(15) y C2 C3 C4 . . . 110.74(15) y N2 C3 H3D . . . 109.1 ? C2 C3 H3D . . . 109.1 ? C4 C3 H3D . . . 109.1 ? O2 C4 C5 . . . 109.54(15) y O2 C4 C3 . . . 105.69(14) y C5 C4 C3 . . . 111.65(15) y O2 C4 H4A . . . 110.0 ? C5 C4 H4A . . . 110.0 ? C3 C4 H4A . . . 110.0 ? O3 C5 C4 . . . 106.77(15) y O3 C5 C6 . . . 110.78(15) y C4 C5 C6 . . . 112.63(15) y O3 C5 H5 . . . 108.9 ? C4 C5 H5 . . . 108.9 ? C6 C5 H5 . . . 108.9 ? O4 C6 C1 . . . 110.51(16) y O4 C6 C5 . . . 111.17(15) y C1 C6 C5 . . . 110.32(15) y O4 C6 H6 . . . 108.2 ? C1 C6 H6 . . . 108.2 ? C5 C6 H6 . . . 108.2 ? O2 C1' O1 . . . 111.41(14) y O2 C1' C2' . . . 107.07(15) y O1 C1' C2' . . . 111.44(14) y O2 C1' H1' . . . 109.0 ? O1 C1' H1' . . . 109.0 ? C2' C1' H1' . . . 109.0 ? N3 C2' C3' . . . 110.21(16) y N3 C2' C1' . . . 108.53(15) y C3' C2' C1' . . . 112.07(16) y N3 C2' H2' . . . 108.7 ? C3' C2' H2' . . . 108.7 ? C1' C2' H2' . . . 108.7 ? C4' C3' C2' . . . 108.34(16) y C4' C3' H3'1 . . . 110.0 ? C2' C3' H3'1 . . . 110.0 ? C4' C3' H3'2 . . . 110.0 ? C2' C3' H3'2 . . . 110.0 ? H3'1 C3' H3'2 . . . 108.4 ? C5' C4' C3' . . . 121.71(17) y C5' C4' H4' . . . 119.1 ? C3' C4' H4' . . . 119.1 ? C4' C5' O1 . . . 125.17(17) y C4' C5' C6' . . . 121.03(16) y O1 C5' C6' . . . 113.80(15) y N2 C6' C5' 3 . . 123.35(16) y N2 C6' H6' 3 . . 118.3 ? C5' C6' H6' . . . 118.3 ? H9A O9 H9B . . . 101(2) ? H9A O9 H9C . . . 105(2) ? H10A O10 H10B . . . 104(2) ? H11A O11 H11B . . . 102.3(19) ? H12A O12A H12B . . . 108(3) ? H12C O12B H12D . . . 108(3) ? H13A O13 H13B . . . 104(2) ? H13C O13 H13D . . . 102(2) ? H14A O14 H14B . . . 103(2) ? H14A O14 H14C . . . 101(2) ? H15A O15 H15B . . . 107(3) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N1 C1 C2 C3 . . . . 175.86(16) y C6 C1 C2 C3 . . . . -61.77(19) y C6' N2 C3 C2 3 . . . 143.78(17) y C6' N2 C3 C4 3 . . . -94.76(19) y C1 C2 C3 N2 . . . . -179.67(15) y C1 C2 C3 C4 . . . . 59.68(19) y C1' O2 C4 C5 . . . . 94.96(17) y C1' O2 C4 C3 . . . . -144.61(15) y N2 C3 C4 O2 . . . . 65.59(17) y C2 C3 C4 O2 . . . . -173.80(14) y N2 C3 C4 C5 . . . . -175.37(15) y C2 C3 C4 C5 . . . . -54.8(2) y O2 C4 C5 O3 . . . . -70.46(19) y C3 C4 C5 O3 . . . . 172.82(15) y O2 C4 C5 C6 . . . . 167.74(14) y C3 C4 C5 C6 . . . . 51.0(2) y N1 C1 C6 O4 . . . . -56.2(2) y C2 C1 C6 O4 . . . . -178.93(15) y N1 C1 C6 C5 . . . . -179.59(15) y C2 C1 C6 C5 . . . . 57.72(19) y O3 C5 C6 O4 . . . . 65.32(19) y C4 C5 C6 O4 . . . . -175.17(15) y O3 C5 C6 C1 . . . . -171.72(15) y C4 C5 C6 C1 . . . . -52.2(2) y C4 O2 C1' O1 . . . . 75.33(18) y C4 O2 C1' C2' . . . . -162.59(14) y C5' O1 C1' O2 . . . . 83.98(19) y C5' O1 C1' C2' . . . . -35.5(2) y O2 C1' C2' N3 . . . . 56.54(19) y O1 C1' C2' N3 . . . . 178.60(15) y O2 C1' C2' C3' . . . . -65.40(19) y O1 C1' C2' C3' . . . . 56.7(2) y N3 C2' C3' C4' . . . . -169.10(16) y C1' C2' C3' C4' . . . . -48.1(2) y C2' C3' C4' C5' . . . . 22.6(3) y C3' C4' C5' O1 . . . . -2.7(3) y C3' C4' C5' C6' . . . . 177.97(18) y C1' O1 C5' C4' . . . . 9.4(3) y C1' O1 C5' C6' . . . . -171.24(15) y C4' C5' C6' N2 . . . 3 -167.4(2) y O1 C5' C6' N2 . . . 3 13.2(3) y 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 _geom_hbond_publ_flag O3 H3 O11 0.84 2.13 2.925(2) 159.1 . y O4 H4 O6 0.84 1.91 2.731(2) 165.5 . y N1 H1C O10 0.91 2.04 2.914(2) 159.9 . y N3 H3C O12A 0.91 1.97 2.857(6) 165.6 . y N3 H3C O12B 0.91 1.72 2.582(10) 156.7 . y O9 H9A O6 0.871(10) 2.026(17) 2.870(3) 163(4) . y O9 H9B O15 0.873(10) 2.354(17) 3.205(7) 165(5) . y O11 H11B O7 0.867(10) 1.965(14) 2.814(3) 166(4) . y O12A H12A O5 0.862(10) 1.913(19) 2.761(6) 167(8) . y O12B H12C O5 0.861(11) 1.98(2) 2.839(11) 173(13) . y O13 H13B O9 0.873(10) 2.02(5) 2.793(3) 147(9) . y O14 H14A O7 0.876(10) 2.087(19) 2.919(3) 158(4) . y O14 H14B O15 0.867(10) 1.765(18) 2.624(8) 171(9) . y O15 H15B O9 0.861(10) 2.42(3) 3.205(7) 151(5) . y O16 H16A N2 0.874(10) 1.988(14) 2.827(2) 160(3) . y N1 H1A O4 0.91 1.96 2.818(2) 156.8 8_556 y N1 H1B O11 0.91 2.07 2.793(2) 135.1 8_556 y N3 H3A O8 0.91 1.84 2.741(2) 171.6 4_456 y N3 H3B O5 0.91 2.05 2.843(3) 144.7 1_455 y N3 H3B O8 0.91 2.52 3.302(3) 144.6 1_455 y O9 H9C O10 0.866(10) 1.94(2) 2.791(3) 165(8) 8_456 y O10 H10A O16 0.872(10) 1.928(11) 2.794(2) 173(3) 1_655 y O10 H10B O13 0.859(10) 2.009(15) 2.817(3) 156(3) 8_456 y O11 H11A O8 0.875(10) 1.872(12) 2.737(2) 169(3) 1_455 y O12A H12B O7 0.856(10) 1.88(3) 2.704(6) 161(8) 4_556 y O12B H12D O7 0.858(10) 1.97(4) 2.809(10) 165(13) 4_556 y O13 H13A O14 0.873(10) 1.92(2) 2.789(4) 170(9) 1_655 y O13 H13C O13 0.873(10) 1.969(16) 2.791(5) 156(3) 3_756 y O14 H14B O15 0.867(10) 2.01(3) 2.802(7) 152(5) 3_656 y O15 H15A O14 0.861(10) 2.31(13) 2.802(7) 117(12) 3_656 y _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 72.54 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.258 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.053 #=== END OF THE CIF FILE # Attachment '- BENT70.cif' data_bent70 _database_code_depnum_ccdc_archive 'CCDC 838350' #TrackingRef '- BENT70.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C28 H46 N6 O8), 5(O4 S), H4 N, 11(H2 O)' _chemical_formula_sum 'C56 H118 N13 O47 S5' _chemical_formula_weight 1885.98 _chemical_compound_source 'Synthesized by the authors. See text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 _symmetry_space_group_name_hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 6.6138(4) _cell_length_b 16.3922(10) _cell_length_c 23.9598(14) _cell_angle_alpha 101.113(3) _cell_angle_beta 92.328(3) _cell_angle_gamma 95.176(3) _cell_volume 2534.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150 _cell_measurement_reflns_used 24946 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 68.56 _exptl_crystal_description needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1001 _exptl_absorpt_coefficient_mu 1.835 _exptl_absorpt_correction_Type multi-scan _exptl_absorpt_correction_T_min 0.5025 _exptl_absorpt_correction_T_max 0.9640 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker microstar diffractometer equiped with a Platinum 135 CCD Detector, a Helios optics and a Kappa goniometer. The crystal-to-detector distance was 4.0 cm, and the data collection was carried out in 512 x 512 pixel mode. The initial unit cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 10.0 degree scan in 33 frames over three different parts of the reciprocal space (99 frames total). Due to geometrical constraints of the instrument and the use of copper radiation, we obtain consistently a data completeness lower than 100% in dependence of the crystal system and the orientation of the mounted crystal, even with appropriate data collection routines. Typical values for data completeness range from 83-92% for triclinic, 85-97% for monoclinic and 85-98% for all other crystal systems. ; _vrf_PLAT029_bent70 ; RESPONSE: Due to geometrical constraints of the instrument and the use of copper radiation, we obtain consistently a data completeness lower than 100% in dependence of the crystal system and the orientation of the mounted crystal, even with appropriate data collection routines. Typical values for data completeness range from 83-92% for triclinic, 85-97% for monoclinic and 85-98% for all other crystal systems. (Note: This comment is routinely included into the CIF-file and can be ignored if the data completeness is satisfactory.) ; 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 -0.014 0.546 0.530 457 125 ' ' 2 0.107 0.567 0.145 16 4 ' ' _platon_squeeze_details ; The crystal structure has been squeezed with PLATON to remove highly disordered H2O, EtOH and ammonium ion contributions from its solvate structure. Overall, PLATON found a solvent accessible void volume of 473.8 A^3 corresponding to a contribution of 129 electrons per cell. More precisely, this void is estimated to contain 9 molecules of H2O, 2 molecules of EtOH and 1 ammonium ion, which were used as crystallization solvents and crystallization agents ((NH4)2SO4). This speculation is based on an attempt to solve this disordered area of the structure. Considering the solvents and the ammonium ion the physical data should be: Formula moiety: '2(C28 H46 N6 O8), 5(O4 S), 2(H4 N), 20(H2 O), 2(C2H5O)' or 'C60 H150 N14 O58 S5' Density: 1.413 g cm-3 Absorption coefficient: 1.988 mm-1 F000: 1152.0 ; _vrf_PLAT244_bent70 ; RESPONSE: Due to minor rotation disorder of the sulfate anion around the sulfur. ; _vrf_PLAT340_bent70 ; RESPONSE: Low diffraction was observed for this crystal and was especially low for high angles. Many solvent systems were tested for recrystallization. The best crystal was chosen and its size was in the limits of the diffractometer. X-ray measurements were acquired at 150K with optimized radiation exposure time and intensity. The final structure was satisfactory for confirming the desired chemical information. ; _vrf_PLAT420_bent70 ; RESPONSE: The O111-H11D bond (H2O molecule) is making a weak electrostatic interaction with the main molecule. For N21-H21A (protonated amine) this is due to hydrogen-bonding, with highly disordered solvent as the acceptor (H2O), which is not included in the final model. See PLATON squeeze details in CIF ; _vrf_PLAT480_bent70 ; RESPONSE: These H-Bonds are listed and reported by SHELXTL and they should be considered as weak H-bond interactions (2.2A-3.2A). ; _vrf_PLAT606_bent70 ; RESPONSE: The crystal structure has been squeezed with PLATON to remove highly disordered H2O, EtOH and ammonium ion contributions from its solvate structure. Overall, PLATON found a solvent accessible void volume of 473.8 A^3 corresponding to a contribution of 129 electrons per cell. More precisely, this void is estimated to contain 9 molecules of H2O, 2 molecules of EtOH and 1 ammonium ion, which were used as crystallization solvents and crystallization agents ((NH4)2SO4). This speculation is based on an attempt to solve this disordered area of the structure. Considering the solvents and the ammonium ion the physical data should be: Formula moiety: '2(C28 H46 N6 O8), 5(O4 S), 2(H4 N), 20(H2 O), 2(C2 H5 O)' or 'C60 H150 N14 O58 S5' Density: 1.413 g cm-3 Absorption coefficient: 1.988 mm-1 F000: 1152.0 ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Helios optics' _diffrn_measurement_device_type 'Bruker Microstar' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 42684 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 69.17 _reflns_number_total 12907 _reflns_number_gt 9594 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT V7.60A(Bruker AXS, 2008)' _computing_data_reduction 'SAINT V7.60A(Bruker AXS, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_publication_material 'UdMX (Maris, 2004)' _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^)+(0.1474P)^2^] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Friedel Pairs merged' _chemical_absolute_configuration rmad _refine_ls_abs_structure_Flack 0.10(2) _refine_ls_number_reflns 12907 _refine_ls_number_parameters 1168 _refine_ls_number_restraints 343 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.1971 _refine_ls_wR_factor_gt 0.1888 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.003 _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 0.07816(18) 0.02788(9) 1.29442(6) 0.0304(4) Uani 1 1 d . . . O51 O 0.0044(6) -0.0545(3) 1.3059(2) 0.0427(11) Uani 1 1 d . . . O52 O 0.0779(8) 0.0939(3) 1.3450(2) 0.0561(14) Uani 1 1 d . . . O53 O 0.2856(5) 0.0229(3) 1.27425(19) 0.0371(10) Uani 1 1 d . . . O54 O -0.0583(6) 0.0472(3) 1.24941(17) 0.0353(10) Uani 1 1 d . . . S2 S 0.75581(18) 0.05612(9) 0.82742(6) 0.0292(3) Uani 1 1 d . . . O61 O 0.6749(6) -0.0265(2) 0.83601(19) 0.0347(10) Uani 1 1 d . . . O62 O 0.6282(5) 0.0786(3) 0.78154(16) 0.0325(10) Uani 1 1 d . . . O63 O 0.7432(7) 0.1191(3) 0.8783(2) 0.0491(12) Uani 1 1 d . . . O64 O 0.9678(5) 0.0523(3) 0.81084(19) 0.0358(10) Uani 1 1 d . . . S3 S 0.2521(3) 0.91182(13) 0.52632(9) 0.0571(5) Uani 1 1 d . . . O71 O 0.4491(9) 0.9303(4) 0.5564(3) 0.0754(18) Uani 1 1 d . . . O72 O 0.1638(9) 0.8269(4) 0.5226(3) 0.0797(19) Uani 1 1 d . . . O73 O 0.1172(13) 0.9721(5) 0.5508(3) 0.110(3) Uani 1 1 d . . . O74 O 0.2812(11) 0.9222(4) 0.4690(3) 0.089(2) Uani 1 1 d . . . S4 S 0.5898(2) 0.87172(10) 1.00154(7) 0.0374(4) Uani 1 1 d . . . O81 O 0.6050(7) 0.7976(3) 1.0275(2) 0.0513(13) Uani 1 1 d . . . O82 O 0.8012(6) 0.9130(3) 1.00311(19) 0.0418(11) Uani 1 1 d . . . O83 O 0.4671(8) 0.9315(4) 1.0347(3) 0.0730(18) Uani 1 1 d . . . O84 O 0.5094(6) 0.8461(3) 0.9435(2) 0.0454(12) Uani 1 1 d . . . S5 S 0.6979(3) 0.14564(16) 1.47688(11) 0.0697(6) Uani 1 1 d . . . O91 O 0.6168(8) 0.1042(3) 1.4195(2) 0.0550(13) Uani 1 1 d . . . O92 O 0.8397(11) 0.2219(5) 1.4762(5) 0.129(3) Uani 1 1 d . . . O93 O 0.5392(11) 0.1768(5) 1.5113(3) 0.090(2) Uani 1 1 d . . . O94 O 0.7923(10) 0.0836(5) 1.5022(3) 0.091(2) Uani 1 1 d . . . O11 O 0.0993(5) 0.2521(2) 0.77881(16) 0.0284(9) Uani 1 1 d . . . O12 O 0.3631(6) 0.3606(3) 0.79184(19) 0.0358(10) Uani 1 1 d . . . O13 O 0.2118(5) 0.1177(3) 0.6894(2) 0.0364(10) Uani 1 1 d . . . H13 H 0.2712 0.1150 0.7205 0.055 Uiso 1 1 calc R . . O14 O -0.1418(6) 0.0192(3) 0.63050(19) 0.0374(10) Uani 1 1 d . . . H14 H -0.1502 0.0029 0.5949 0.056 Uiso 1 1 calc R . . N11 N -0.4801(8) 0.1015(4) 0.6056(2) 0.0436(14) Uani 1 1 d . . . H11A H -0.4765 0.0451 0.5974 0.065 Uiso 1 1 calc R . . H11B H -0.4462 0.1233 0.5747 0.065 Uiso 1 1 calc R . . H11C H -0.6076 0.1135 0.6149 0.065 Uiso 1 1 calc R . . N12 N -0.1623(7) 0.3587(3) 0.7272(3) 0.0416(14) Uani 1 1 d . . . N13 N 0.3244(7) 0.1595(3) 0.8430(2) 0.0297(11) Uani 1 1 d . . . H13A H 0.3508 0.1473 0.8779 0.044 Uiso 1 1 calc R . . H13B H 0.4033 0.1311 0.8173 0.044 Uiso 1 1 calc R . . H13C H 0.1909 0.1443 0.8319 0.044 Uiso 1 1 calc R . . C11 C 0.5568(8) 0.8500(4) 0.6994(3) 0.0301(13) Uani 1 1 d . . . H11 H 0.6446 0.8775 0.7341 0.036 Uiso 1 1 calc R . . C12 C 0.5230(9) 0.7583(4) 0.6989(3) 0.0361(15) Uani 1 1 d . . . H12A H 0.6553 0.7343 0.6966 0.043 Uiso 1 1 calc R . . H12B H 0.4361 0.7305 0.6647 0.043 Uiso 1 1 calc R . . C13 C 0.4205(8) 0.7411(4) 0.7529(3) 0.0298(13) Uani 1 1 d . . . H13D H 0.5136 0.7657 0.7870 0.036 Uiso 1 1 calc R . . C14 C 0.2194(8) 0.7801(4) 0.7592(3) 0.0287(13) Uani 1 1 d . . . H14A H 0.1155 0.7471 0.7301 0.034 Uiso 1 1 calc R . . C15 C 0.2379(8) 0.8725(4) 0.7530(3) 0.0341(15) Uani 1 1 d . . . H15 H 0.3124 0.9069 0.7881 0.041 Uiso 1 1 calc R . . C16 C 0.3504(8) 0.8893(4) 0.7014(3) 0.0314(14) Uani 1 1 d . . . H16 H 0.2647 0.8618 0.6663 0.038 Uiso 1 1 calc R . . C11' C -0.0514(8) 0.7559(4) 0.8211(3) 0.0306(14) Uani 1 1 d . . . H11' H -0.1318 0.7808 0.7935 0.037 Uiso 1 1 calc R . . C12' C -0.0972(8) 0.7961(4) 0.8813(2) 0.0295(13) Uani 1 1 d . . . H12' H -0.2445 0.7814 0.8863 0.035 Uiso 1 1 calc R . . C13' C 0.0268(9) 0.7597(4) 0.9235(3) 0.0322(14) Uani 1 1 d . . . H13E H 0.1723 0.7801 0.9234 0.039 Uiso 1 1 calc R . . H13F H -0.0191 0.7777 0.9624 0.039 Uiso 1 1 calc R . . C14' C 0.0005(9) 0.6690(5) 0.9073(3) 0.0417(16) Uani 1 1 d . . . H14' H 0.0322 0.6373 0.9353 0.050 Uiso 1 1 calc R . . C15' C -0.0663(8) 0.6279(4) 0.8550(3) 0.0374(15) Uani 1 1 d . . . C16' C -0.1011(8) 0.5409(4) 0.8394(3) 0.0417(17) Uani 1 1 d . . . H16' H -0.1028 0.5117 0.8699 0.050 Uiso 1 1 calc R . . C17' C -0.1326(8) 0.4928(4) 0.7867(3) 0.0405(16) Uani 1 1 d . . . H17' H -0.1375 0.5196 0.7549 0.049 Uiso 1 1 calc R . . C18' C -0.1589(8) 0.4036(4) 0.7764(3) 0.0391(16) Uani 1 1 d . . . H18' H -0.1746 0.3768 0.8080 0.047 Uiso 1 1 calc R . . O21 O 0.1569(5) 0.7751(3) 0.81468(17) 0.0319(10) Uani 1 1 d . . . O22 O -0.1073(6) 0.6685(3) 0.81069(18) 0.0357(10) Uani 1 1 d . . . O23 O 0.0358(5) 0.8950(3) 0.7512(2) 0.0379(11) Uani 1 1 d . . . H23 H 0.0380 0.9472 0.7570 0.057 Uiso 1 1 calc R . . O24 O 0.3799(6) 0.9748(3) 0.70150(19) 0.0365(10) Uani 1 1 d . . . H24 H 0.3908 1.0017 0.7353 0.055 Uiso 1 1 calc RD . . N21 N 0.6608(8) 0.8644(4) 0.6486(3) 0.0438(14) Uani 1 1 d . . . H21A H 0.7811 0.8413 0.6476 0.066 Uiso 1 1 calc R . . H21B H 0.6847 0.9203 0.6500 0.066 Uiso 1 1 calc R . . H21C H 0.5811 0.8404 0.6168 0.066 Uiso 1 1 calc R . . N22 N 0.3886(7) 0.6502(3) 0.7484(3) 0.0374(13) Uani 1 1 d . . . N23 N -0.0585(7) 0.8879(3) 0.8919(2) 0.0295(11) Uani 1 1 d . . . H23A H -0.0489 0.9084 0.9301 0.044 Uiso 1 1 calc R . . H23B H -0.1625 0.9094 0.8755 0.044 Uiso 1 1 calc R . . H23C H 0.0600 0.9025 0.8767 0.044 Uiso 1 1 calc R . . C21 C -0.3345(8) 0.1382(4) 0.6539(3) 0.0321(14) Uani 1 1 d . . . H21 H -0.3849 0.1188 0.6884 0.039 Uiso 1 1 calc R . . C22 C -0.3200(8) 0.2303(4) 0.6659(3) 0.0300(13) Uani 1 1 d . . . H22A H -0.4582 0.2487 0.6699 0.036 Uiso 1 1 calc R . . H22B H -0.2608 0.2513 0.6335 0.036 Uiso 1 1 calc R . . C23 C -0.1869(8) 0.2685(4) 0.7212(3) 0.0342(15) Uani 1 1 d . . . H23D H -0.2577 0.2539 0.7546 0.041 Uiso 1 1 calc R . . C24 C 0.0210(8) 0.2347(4) 0.7197(3) 0.0315(14) Uani 1 1 d . . . H24A H 0.1129 0.2640 0.6961 0.038 Uiso 1 1 calc R . . C25 C 0.0092(8) 0.1402(4) 0.6990(3) 0.0306(14) Uani 1 1 d . . . H25 H -0.0463 0.1123 0.7295 0.037 Uiso 1 1 calc R . . C26 C -0.1237(8) 0.1081(3) 0.6439(3) 0.0313(14) Uani 1 1 d . . . H26 H -0.0629 0.1311 0.6120 0.038 Uiso 1 1 calc R . . C21' C 0.3090(7) 0.2748(4) 0.7904(3) 0.0285(13) Uani 1 1 d . . . H21' H 0.3824 0.2419 0.7594 0.034 Uiso 1 1 calc R . . C22' C 0.3699(9) 0.2495(4) 0.8462(3) 0.0316(14) Uani 1 1 d . . . H22' H 0.5195 0.2645 0.8546 0.038 Uiso 1 1 calc R . . C23' C 0.2564(11) 0.2995(4) 0.8938(3) 0.0431(16) Uani 1 1 d U . . H23E H 0.1099 0.2793 0.8897 0.052 Uiso 1 1 calc R . . H23F H 0.3111 0.2924 0.9315 0.052 Uiso 1 1 calc R . . C24' C 0.2843(10) 0.3887(5) 0.8896(3) 0.0440(16) Uani 1 1 d U . . H24' H 0.2641 0.4291 0.9226 0.053 Uiso 1 1 calc R . . C25' C 0.3349(8) 0.4159(4) 0.8437(3) 0.0344(15) Uani 1 1 d . . . C26' C 0.3719(8) 0.5011(4) 0.8391(3) 0.0443(18) Uani 1 1 d . . . H26' H 0.3944 0.5407 0.8739 0.053 Uiso 1 1 calc R . . C27' C 0.3787(8) 0.5321(4) 0.7909(3) 0.0356(15) Uani 1 1 d . . . H27' H 0.3656 0.4947 0.7550 0.043 Uiso 1 1 calc R . . C28' C 0.4051(8) 0.6200(5) 0.7927(3) 0.0425(17) Uani 1 1 d . . . H28' H 0.4361 0.6568 0.8284 0.051 Uiso 1 1 calc R . . O31 O 0.4080(5) 0.2182(3) 1.24080(17) 0.0306(9) Uani 1 1 d . . . O32 O 0.6701(6) 0.3259(3) 1.25062(18) 0.0352(10) Uani 1 1 d . . . O33 O 0.5190(5) 0.0864(2) 1.15051(18) 0.0304(9) Uani 1 1 d . . . H33 H 0.5317 0.0394 1.1586 0.046 Uiso 1 1 calc R . . O34 O 0.1591(5) -0.0118(2) 1.09183(18) 0.0321(10) Uani 1 1 d . . . H34 H 0.2429 -0.0284 1.0678 0.048 Uiso 1 1 calc R . . N31 N -0.1729(6) 0.0749(3) 1.0652(2) 0.0302(11) Uani 1 1 d . . . H31A H -0.1325 0.0985 1.0356 0.045 Uiso 1 1 calc R . . H31B H -0.2999 0.0884 1.0740 0.045 Uiso 1 1 calc R . . H31C H -0.1746 0.0184 1.0553 0.045 Uiso 1 1 calc R . . N32 N 0.1519(7) 0.3263(3) 1.1912(2) 0.0347(12) Uani 1 1 d . . . N33 N 0.6356(7) 0.1298(3) 1.3074(2) 0.0306(11) Uani 1 1 d . . . H33A H 0.5059 0.1127 1.2930 0.046 Uiso 1 1 calc R . . H33B H 0.6499 0.1201 1.3434 0.046 Uiso 1 1 calc R . . H33C H 0.7238 0.1010 1.2850 0.046 Uiso 1 1 calc R . . C31 C -0.0272(7) 0.1071(4) 1.1161(2) 0.0284(13) Uani 1 1 d . . . H31 H -0.0814 0.0862 1.1497 0.034 Uiso 1 1 calc R . . C32 C -0.0095(8) 0.2020(4) 1.1290(3) 0.0284(13) Uani 1 1 d . . . H32A H 0.0531 0.2236 1.0972 0.034 Uiso 1 1 calc R . . H32B H -0.1464 0.2216 1.1330 0.034 Uiso 1 1 calc R . . C33 C 0.1204(7) 0.2347(4) 1.1837(3) 0.0271(13) Uani 1 1 d . . . H33D H 0.0467 0.2195 1.2164 0.033 Uiso 1 1 calc R . . C34 C 0.3308(7) 0.2005(4) 1.1828(2) 0.0248(12) Uani 1 1 d . . . H34A H 0.4228 0.2302 1.1594 0.030 Uiso 1 1 calc R . . C35 C 0.3130(7) 0.1077(3) 1.1598(2) 0.0233(12) Uani 1 1 d . . . H35 H 0.2578 0.0785 1.1898 0.028 Uiso 1 1 calc R . . C36 C 0.1820(7) 0.0776(3) 1.1058(2) 0.0257(12) Uani 1 1 d . . . H36 H 0.2427 0.1008 1.0739 0.031 Uiso 1 1 calc R . . C31' C 0.6194(8) 0.2409(4) 1.2515(3) 0.0296(13) Uani 1 1 d . . . H31' H 0.6928 0.2064 1.2213 0.035 Uiso 1 1 calc R . . C32' C 0.6799(9) 0.2209(4) 1.3085(3) 0.0328(14) Uani 1 1 d . . . H32' H 0.8291 0.2370 1.3170 0.039 Uiso 1 1 calc R . . C33' C 0.5623(10) 0.2728(4) 1.3546(3) 0.0426(16) Uani 1 1 d . . . H33E H 0.4158 0.2526 1.3497 0.051 Uiso 1 1 calc R . . H33F H 0.6133 0.2671 1.3929 0.051 Uiso 1 1 calc R . . C34' C 0.5917(10) 0.3612(4) 1.3491(3) 0.0452(17) Uani 1 1 d . . . H34' H 0.5745 0.4039 1.3810 0.054 Uiso 1 1 calc R . . C35' C 0.6428(9) 0.3825(4) 1.2994(3) 0.0386(16) Uani 1 1 d . . . C36' C 0.6745(8) 0.4684(4) 1.2949(3) 0.0425(17) Uani 1 1 d . . . H36' H 0.6923 0.5087 1.3294 0.051 Uiso 1 1 calc R . . C37' C 0.6814(8) 0.4973(5) 1.2456(3) 0.0448(18) Uani 1 1 d . . . H37' H 0.6675 0.4589 1.2102 0.054 Uiso 1 1 calc R . . C38' C 0.7099(8) 0.5862(4) 1.2463(3) 0.0384(16) Uani 1 1 d . . . H38' H 0.7470 0.6228 1.2818 0.046 Uiso 1 1 calc R . . O41 O 0.4722(5) 0.7387(3) 1.27677(16) 0.0295(9) Uani 1 1 d . . . O42 O 0.2007(5) 0.6363(3) 1.27440(18) 0.0358(10) Uani 1 1 d . . . O43 O 0.3493(5) 0.8666(3) 1.2217(2) 0.0386(11) Uani 1 1 d . . . H43G H 0.3536 0.9163 1.2393 0.058 Uiso 1 1 calc R . . O44 O 0.6844(6) 0.9499(3) 1.17067(18) 0.0357(10) Uani 1 1 d . . . H44B H 0.7615 0.9716 1.1994 0.053 Uiso 1 1 calc R . . N41 N 0.9441(7) 0.8390(3) 1.1075(2) 0.0377(13) Uani 1 1 d . . . H41A H 1.0507 0.8079 1.1001 0.057 Uiso 1 1 calc R . . H41B H 0.9885 0.8942 1.1122 0.057 Uiso 1 1 calc R . . H41C H 0.8489 0.8249 1.0778 0.057 Uiso 1 1 calc R . . N42 N 0.6888(7) 0.6177(3) 1.2033(2) 0.0365(13) Uani 1 1 d . . . N43 N 0.2793(8) 0.8566(3) 1.3534(2) 0.0345(12) Uani 1 1 d . . . H43A H 0.4080 0.8664 1.3426 0.052 Uiso 1 1 calc R . . H43B H 0.2734 0.8796 1.3910 0.052 Uiso 1 1 calc R . . H43C H 0.1915 0.8799 1.3324 0.052 Uiso 1 1 calc R . . C41 C 0.8523(8) 0.8224(4) 1.1606(3) 0.0312(14) Uani 1 1 d . . . H41 H 0.9479 0.8479 1.1940 0.037 Uiso 1 1 calc R . . C42 C 0.8167(8) 0.7297(4) 1.1578(3) 0.0328(14) Uani 1 1 d . . . H42A H 0.7252 0.7042 1.1241 0.039 Uiso 1 1 calc R . . H42B H 0.9479 0.7052 1.1531 0.039 Uiso 1 1 calc R . . C43 C 0.7249(8) 0.7089(4) 1.2101(3) 0.0308(14) Uani 1 1 d . . . H43D H 0.8237 0.7306 1.2435 0.037 Uiso 1 1 calc R . . C44 C 0.5290(8) 0.7477(4) 1.2214(3) 0.0313(14) Uani 1 1 d . . . H44A H 0.4204 0.7182 1.1924 0.038 Uiso 1 1 calc R . . C45 C 0.5519(7) 0.8411(4) 1.2196(3) 0.0325(14) Uani 1 1 d . . . H45 H 0.6342 0.8719 1.2545 0.039 Uiso 1 1 calc R . . C46 C 0.6519(8) 0.8616(4) 1.1674(3) 0.0291(13) Uani 1 1 d . . . H46 H 0.5592 0.8370 1.1331 0.035 Uiso 1 1 calc R . . C41' C 0.2599(8) 0.7246(4) 1.2840(3) 0.0329(14) Uani 1 1 d . . . H41' H 0.1817 0.7501 1.2563 0.039 Uiso 1 1 calc R . . C42' C 0.2231(8) 0.7665(4) 1.3444(3) 0.0329(14) Uani 1 1 d . . . H42' H 0.0749 0.7567 1.3505 0.039 Uiso 1 1 calc R . . C43' C 0.3422(11) 0.7284(4) 1.3871(3) 0.0429(16) Uani 1 1 d . . . H43E H 0.4894 0.7455 1.3864 0.051 Uiso 1 1 calc R . . H43F H 0.2993 0.7486 1.4261 0.051 Uiso 1 1 calc R . . C44' C 0.3041(11) 0.6354(5) 1.3721(3) 0.0449(17) Uani 1 1 d . . . H44' H 0.3284 0.6035 1.4004 0.054 Uiso 1 1 calc R . . C45' C 0.2368(9) 0.5962(4) 1.3198(3) 0.0367(15) Uani 1 1 d . . . C46' C 0.2007(8) 0.5068(4) 1.3042(3) 0.0401(16) Uani 1 1 d . . . H46' H 0.1935 0.4771 1.3345 0.048 Uiso 1 1 calc R . . C47' C 0.1762(8) 0.4609(4) 1.2510(3) 0.0375(15) Uani 1 1 d . . . H47' H 0.1766 0.4882 1.2194 0.045 Uiso 1 1 calc R . . C48' C 0.1494(8) 0.3717(4) 1.2414(3) 0.0383(16) Uani 1 1 d . . . H48' H 0.1291 0.3452 1.2730 0.046 Uiso 1 1 calc R . . O101 O 0.3401(7) 0.1315(3) 0.9576(2) 0.0466(12) Uani 1 1 d D . . H1E H 0.394(8) 0.0851(19) 0.955(2) 0.070 Uiso 1 1 d D . . H1F H 0.354(8) 0.154(3) 0.9936(7) 0.070 Uiso 1 1 d D . . O102 O 0.3488(6) 0.9692(3) 0.9052(2) 0.0419(11) Uani 1 1 d D . . H2A H 0.375(7) 0.936(2) 0.9280(17) 0.063 Uiso 1 1 d D . . H2B H 0.462(4) 0.980(2) 0.8900(17) 0.063 Uiso 1 1 d D . . O103 O 0.2516(7) 0.7397(3) 1.0766(2) 0.0568(14) Uani 1 1 d D . . H3A H 0.246(10) 0.6860(10) 1.074(4) 0.085 Uiso 1 1 d D . . H3B H 0.363(5) 0.751(4) 1.061(3) 0.085 Uiso 1 1 d D . . O104 O 0.2864(7) 0.3717(3) 1.0897(2) 0.0715(16) Uani 1 1 d D . . H4A H 0.1755 0.3584 1.0689 0.107 Uiso 1 1 d D . . H4B H 0.3643 0.3336 1.0780 0.107 Uiso 1 1 d D . . O105 O 0.9444(7) 0.1599(3) 0.9788(2) 0.0529(13) Uani 1 1 d D . . H5A H 0.824(3) 0.152(4) 0.9600(17) 0.079 Uiso 1 1 d D . . H5B H 1.009(8) 0.124(4) 0.954(3) 0.079 Uiso 1 1 d D . . O106 O 0.9191(9) 0.3299(4) 1.0184(3) 0.0754(17) Uani 1 1 d D . . H6A H 0.887(4) 0.3015(14) 0.9837(9) 0.113 Uiso 1 1 d D . . H6B H 0.8901 0.3796 1.0155 0.113 Uiso 1 1 d D . . O107 O 0.2223(9) 0.5715(4) 1.0280(3) 0.0803(18) Uani 1 1 d D . . H7A H 0.3152 0.5560 1.0500 0.120 Uiso 1 1 d D . . H7B H 0.168(5) 0.5228(16) 1.0086(17) 0.120 Uiso 1 1 d D . . O108 O 0.5259(9) 0.5192(4) 1.0962(3) 0.0764(18) Uani 1 1 d D . . H8A H 0.652(3) 0.514(4) 1.107(2) 0.115 Uiso 1 1 d D . . H8B H 0.470(10) 0.4674(19) 1.090(5) 0.115 Uiso 1 1 d D . . O109 O 0.5392(11) 0.6276(5) 0.9655(4) 0.107(3) Uani 1 1 d D . . H9A H 0.545(14) 0.6821(14) 0.970(6) 0.160 Uiso 1 1 d D . . H9B H 0.426(4) 0.615(5) 0.980(3) 0.160 Uiso 1 1 d D . . O110 O 0.8172(11) 0.5048(5) 1.0042(4) 0.120(3) Uani 1 1 d D . . H10A H 0.7383 0.5413 0.9953 0.180 Uiso 1 1 d D . . H10B H 0.860(6) 0.527(3) 1.0391(9) 0.180 Uiso 1 1 d D . . O111 O 0.5475(8) 0.2479(4) 1.0492(3) 0.0690(16) Uani 1 1 d D . . H11D H 0.619(4) 0.2066(15) 1.051(2) 0.104 Uiso 1 1 d D . . H11E H 0.625(7) 0.2825(17) 1.035(3) 0.104 Uiso 1 1 d D . . N101 N 0.1814(10) 0.0856(5) 1.4550(3) 0.072(2) Uani 1 1 d D . . H1A H 0.252(6) 0.124(2) 1.4385(17) 0.109 Uiso 1 1 d D . . H1B H 0.265(5) 0.053(2) 1.467(2) 0.109 Uiso 1 1 d D . . H1C H 0.117(7) 0.113(3) 1.4841(16) 0.109 Uiso 1 1 d D . . H1D H 0.089(6) 0.055(3) 1.4290(17) 0.109 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0262(6) 0.0304(9) 0.0350(8) 0.0053(7) 0.0041(6) 0.0061(6) O51 0.039(2) 0.039(3) 0.059(3) 0.023(2) 0.016(2) 0.0143(19) O52 0.061(3) 0.062(4) 0.041(3) -0.012(2) 0.002(2) 0.026(2) O53 0.0188(17) 0.038(3) 0.056(3) 0.009(2) 0.0132(18) 0.0077(16) O54 0.0284(19) 0.041(3) 0.035(2) 0.008(2) -0.0069(17) 0.0027(17) S2 0.0230(6) 0.0293(9) 0.0340(8) 0.0034(7) -0.0003(6) 0.0036(5) O61 0.0270(19) 0.025(2) 0.055(3) 0.013(2) 0.0045(18) 0.0044(16) O62 0.0244(18) 0.048(3) 0.027(2) 0.0107(19) -0.0027(15) 0.0072(16) O63 0.052(3) 0.052(3) 0.041(3) -0.001(2) -0.006(2) 0.016(2) O64 0.0171(17) 0.032(3) 0.059(3) 0.009(2) 0.0091(17) 0.0052(15) S3 0.0608(11) 0.0566(14) 0.0475(12) -0.0071(10) 0.0092(9) 0.0064(9) O71 0.078(4) 0.066(4) 0.070(4) -0.009(3) -0.032(3) 0.001(3) O72 0.059(3) 0.067(4) 0.103(5) -0.002(4) -0.009(3) -0.005(3) O73 0.135(6) 0.099(6) 0.108(5) 0.009(4) 0.065(5) 0.072(5) O74 0.120(5) 0.096(5) 0.049(4) -0.009(3) -0.001(3) 0.055(4) S4 0.0298(7) 0.0372(10) 0.0422(9) 0.0006(8) 0.0063(6) 0.0018(6) O81 0.045(2) 0.050(3) 0.057(3) 0.013(3) -0.003(2) -0.010(2) O82 0.028(2) 0.042(3) 0.048(3) -0.005(2) 0.0025(18) -0.0087(18) O83 0.041(3) 0.070(4) 0.094(4) -0.023(3) 0.018(3) 0.010(2) O84 0.032(2) 0.050(3) 0.048(3) 0.000(2) -0.008(2) -0.0024(19) S5 0.0655(13) 0.0735(16) 0.0711(14) 0.0181(12) -0.0036(11) 0.0077(11) O91 0.059(3) 0.075(4) 0.034(3) 0.014(3) 0.004(2) 0.015(3) O92 0.073(5) 0.102(6) 0.220(11) 0.062(7) -0.002(5) -0.016(4) O93 0.104(5) 0.107(6) 0.062(4) 0.006(4) 0.010(4) 0.044(4) O94 0.077(4) 0.115(6) 0.093(5) 0.045(4) -0.005(4) 0.024(4) O11 0.0172(16) 0.030(2) 0.035(2) 0.0012(18) -0.0059(15) -0.0014(15) O12 0.0285(19) 0.032(3) 0.046(3) 0.008(2) -0.0009(18) -0.0014(17) O13 0.0144(17) 0.035(3) 0.059(3) 0.008(2) -0.0036(17) 0.0048(15) O14 0.0299(19) 0.032(3) 0.043(3) -0.007(2) 0.0028(18) -0.0033(17) N11 0.033(3) 0.045(4) 0.045(3) -0.006(3) -0.004(2) -0.002(2) N12 0.028(2) 0.034(3) 0.059(4) -0.003(3) 0.002(2) 0.006(2) N13 0.025(2) 0.031(3) 0.032(3) 0.004(2) -0.0016(19) 0.0058(19) C11 0.028(3) 0.029(3) 0.032(3) 0.004(3) 0.001(2) 0.001(2) C12 0.030(3) 0.030(4) 0.050(4) 0.006(3) 0.006(3) 0.011(2) C13 0.025(3) 0.028(4) 0.034(3) 0.002(3) 0.003(2) 0.002(2) C14 0.023(2) 0.023(3) 0.039(3) 0.000(3) 0.002(2) 0.005(2) C15 0.020(2) 0.038(4) 0.046(4) 0.007(3) 0.003(2) 0.013(2) C16 0.030(3) 0.026(3) 0.036(3) 0.004(3) -0.005(2) 0.000(2) C11' 0.023(3) 0.030(4) 0.037(3) 0.004(3) 0.004(2) 0.000(2) C12' 0.020(2) 0.037(4) 0.031(3) 0.005(3) 0.001(2) 0.005(2) C13' 0.034(3) 0.035(4) 0.025(3) 0.001(3) 0.001(2) 0.006(2) C14' 0.035(3) 0.048(5) 0.044(4) 0.013(3) 0.005(3) 0.004(3) C15' 0.027(3) 0.032(4) 0.054(4) 0.011(3) 0.003(3) -0.001(2) C16' 0.025(3) 0.034(4) 0.063(5) 0.007(4) 0.003(3) -0.006(2) C17' 0.023(3) 0.036(4) 0.059(4) -0.002(3) 0.007(3) 0.008(2) C18' 0.025(3) 0.037(4) 0.052(4) 0.002(3) 0.002(3) 0.005(2) O21 0.0160(17) 0.043(3) 0.036(2) 0.006(2) 0.0008(16) -0.0014(16) O22 0.033(2) 0.029(3) 0.042(3) 0.002(2) 0.0008(18) -0.0023(17) O23 0.0197(18) 0.026(2) 0.066(3) 0.002(2) 0.0014(18) 0.0070(15) O24 0.039(2) 0.024(2) 0.043(3) 0.003(2) -0.0079(19) 0.0000(17) N21 0.042(3) 0.036(3) 0.053(4) 0.009(3) 0.005(3) -0.004(2) N22 0.031(2) 0.026(3) 0.057(4) 0.009(3) 0.015(2) 0.007(2) N23 0.031(2) 0.023(3) 0.032(3) 0.000(2) 0.000(2) 0.0006(19) C21 0.023(3) 0.029(4) 0.040(3) -0.002(3) -0.001(2) -0.001(2) C22 0.030(3) 0.029(4) 0.029(3) 0.001(3) -0.002(2) 0.003(2) C23 0.019(2) 0.039(4) 0.044(4) 0.008(3) -0.002(2) 0.005(2) C24 0.028(3) 0.034(4) 0.032(3) 0.005(3) 0.004(2) 0.004(2) C25 0.022(3) 0.031(4) 0.039(3) 0.005(3) 0.002(2) 0.009(2) C26 0.027(3) 0.022(3) 0.042(4) -0.001(3) -0.002(2) 0.002(2) C21' 0.020(2) 0.024(3) 0.040(3) 0.002(3) 0.000(2) 0.001(2) C22' 0.032(3) 0.024(3) 0.036(3) 0.001(3) -0.003(2) 0.000(2) C23' 0.058(4) 0.033(4) 0.037(4) 0.006(3) -0.001(3) 0.005(3) C24' 0.043(3) 0.044(4) 0.041(4) -0.003(3) 0.002(3) 0.008(3) C25' 0.029(3) 0.024(4) 0.048(4) 0.004(3) -0.005(3) -0.003(2) C26' 0.029(3) 0.037(4) 0.062(5) -0.004(4) -0.001(3) 0.003(3) C27' 0.025(3) 0.027(4) 0.058(4) 0.011(3) 0.003(3) 0.007(2) C28' 0.021(3) 0.049(5) 0.057(5) 0.009(4) 0.008(3) 0.000(3) O31 0.0197(17) 0.036(3) 0.034(2) 0.0041(19) -0.0029(15) -0.0016(15) O32 0.0273(19) 0.035(3) 0.042(3) 0.010(2) -0.0066(17) -0.0046(17) O33 0.0154(16) 0.021(2) 0.056(3) 0.006(2) 0.0071(16) 0.0049(14) O34 0.0236(18) 0.021(2) 0.046(3) -0.0055(19) 0.0068(17) -0.0015(15) N31 0.019(2) 0.027(3) 0.039(3) -0.007(2) -0.0052(19) -0.0030(17) N32 0.025(2) 0.030(3) 0.049(3) 0.003(3) -0.003(2) 0.010(2) N33 0.028(2) 0.023(3) 0.041(3) 0.010(2) -0.005(2) 0.0017(19) C31 0.015(2) 0.037(4) 0.031(3) 0.002(3) -0.004(2) -0.001(2) C32 0.026(3) 0.025(3) 0.031(3) -0.002(3) 0.000(2) 0.004(2) C33 0.017(2) 0.028(3) 0.034(3) -0.001(3) -0.001(2) 0.008(2) C34 0.018(2) 0.027(3) 0.031(3) 0.006(3) 0.005(2) 0.008(2) C35 0.017(2) 0.022(3) 0.031(3) 0.002(2) 0.003(2) 0.0067(19) C36 0.021(2) 0.024(3) 0.030(3) 0.000(3) 0.000(2) 0.002(2) C31' 0.028(3) 0.027(4) 0.033(3) 0.005(3) 0.001(2) -0.001(2) C32' 0.032(3) 0.033(4) 0.032(3) 0.001(3) 0.000(2) 0.006(2) C33' 0.047(3) 0.045(4) 0.037(4) 0.008(3) 0.006(3) 0.006(3) C34' 0.054(4) 0.034(4) 0.046(4) 0.002(3) -0.002(3) 0.009(3) C35' 0.036(3) 0.030(4) 0.048(4) 0.006(3) -0.007(3) 0.000(3) C36' 0.034(3) 0.038(4) 0.054(4) 0.010(4) -0.010(3) -0.002(3) C37' 0.017(3) 0.052(5) 0.065(5) 0.009(4) 0.001(3) 0.005(2) C38' 0.021(3) 0.030(4) 0.065(5) 0.013(3) -0.003(3) 0.003(2) O41 0.0208(17) 0.037(3) 0.028(2) 0.0027(19) -0.0018(15) -0.0012(16) O42 0.0255(19) 0.034(3) 0.041(3) -0.001(2) -0.0018(17) -0.0113(17) O43 0.0250(19) 0.027(2) 0.060(3) -0.002(2) 0.0027(19) 0.0076(16) O44 0.034(2) 0.030(3) 0.042(2) 0.004(2) -0.0042(18) 0.0067(17) N41 0.037(3) 0.027(3) 0.046(3) -0.001(3) 0.013(2) 0.001(2) N42 0.030(2) 0.030(3) 0.051(3) 0.009(3) 0.008(2) 0.010(2) N43 0.040(3) 0.032(3) 0.028(3) -0.003(2) 0.003(2) 0.005(2) C41 0.024(3) 0.025(3) 0.044(4) 0.002(3) 0.000(2) 0.009(2) C42 0.019(2) 0.032(4) 0.047(4) 0.005(3) 0.004(2) 0.005(2) C43 0.023(3) 0.021(3) 0.044(4) -0.002(3) 0.001(2) 0.001(2) C44 0.020(2) 0.037(4) 0.037(3) 0.005(3) 0.003(2) 0.007(2) C45 0.022(2) 0.028(4) 0.045(4) 0.002(3) 0.002(2) 0.001(2) C46 0.024(2) 0.022(3) 0.041(3) 0.003(3) -0.001(2) 0.006(2) C41' 0.019(2) 0.032(4) 0.044(4) 0.001(3) -0.002(2) -0.003(2) C42' 0.028(3) 0.035(4) 0.032(3) 0.003(3) -0.002(2) -0.005(2) C43' 0.056(4) 0.043(4) 0.032(4) 0.011(3) 0.003(3) 0.008(3) C44' 0.058(4) 0.043(4) 0.037(4) 0.012(3) 0.006(3) 0.011(3) C45' 0.038(3) 0.028(4) 0.043(4) 0.007(3) 0.005(3) -0.001(2) C46' 0.039(3) 0.033(4) 0.045(4) 0.002(3) 0.012(3) 0.000(3) C47' 0.020(3) 0.038(4) 0.048(4) -0.006(3) -0.002(2) 0.003(2) C48' 0.024(3) 0.034(4) 0.053(4) 0.000(3) -0.001(3) 0.005(2) O101 0.050(3) 0.048(3) 0.042(3) 0.009(2) 0.010(2) 0.006(2) O102 0.030(2) 0.047(3) 0.051(3) 0.016(2) 0.0009(19) 0.0043(18) O103 0.049(3) 0.050(3) 0.072(4) 0.012(3) 0.024(3) -0.001(2) O104 0.065(3) 0.066(4) 0.077(4) 0.003(3) 0.007(3) -0.008(3) O105 0.049(3) 0.064(4) 0.043(3) 0.008(3) -0.006(2) 0.002(2) O106 0.069(4) 0.067(4) 0.087(4) 0.011(3) -0.001(3) 0.003(3) O107 0.068(4) 0.053(4) 0.113(5) 0.005(4) -0.004(3) -0.004(3) O108 0.062(3) 0.062(4) 0.103(5) 0.015(4) 0.007(3) -0.007(3) O109 0.074(4) 0.121(6) 0.103(6) -0.018(5) 0.023(4) -0.027(4) O110 0.074(5) 0.133(7) 0.151(8) 0.040(6) 0.004(5) -0.018(4) O111 0.057(3) 0.083(5) 0.066(4) 0.013(3) -0.002(3) 0.006(3) N101 0.046(4) 0.100(6) 0.063(4) -0.010(4) -0.002(3) 0.018(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_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 O52 . . 1.460(5) y S1 O51 . . 1.474(5) y S1 O53 . . 1.477(4) y S1 O54 . . 1.477(4) y S2 O63 . . 1.448(5) y S2 O61 . . 1.465(4) y S2 O64 . . 1.476(4) y S2 O62 . . 1.481(4) y S3 O74 . . 1.434(7) y S3 O71 . . 1.441(6) y S3 O72 . . 1.444(6) y S3 O73 . . 1.447(6) y S4 O84 . . 1.439(5) y S4 O83 . . 1.465(5) y S4 O81 . . 1.477(5) y S4 O82 . . 1.493(4) y S5 O93 . . 1.431(7) y S5 O94 . . 1.454(7) y S5 O91 . . 1.468(6) y S5 O92 . . 1.497(8) y O11 C21' . . 1.405(6) y O11 C24 . . 1.455(7) y O12 C21' . . 1.413(7) y O12 C25' . . 1.419(8) y O13 C25 . . 1.437(6) y O13 H13 . . 0.8400 ? O14 C26 . . 1.424(6) y O14 H14 . . 0.8400 ? N11 C21 . . 1.471(8) y N11 H11a . . 0.9100 ? N11 H11b . . 0.9100 ? N11 H11c . . 0.9100 ? N12 C18' . . 1.262(9) y N12 C23 . . 1.453(8) y N13 C22' . . 1.465(8) y N13 H13a . . 0.9100 ? N13 H13b . . 0.9100 ? N13 H13c . . 0.9100 ? C11 N21 . . 1.469(8) y C11 C12 . . 1.496(8) y C11 C16 . . 1.560(8) y C11 H11 . . 1.0000 ? C12 C13 . . 1.546(9) y C12 H12a . . 0.9900 ? C12 H12b . . 0.9900 ? C13 N22 . . 1.468(8) y C13 C14 . . 1.528(7) y C13 H13d . . 1.0000 ? C14 O21 . . 1.424(7) y C14 C15 . . 1.545(8) y C14 H14a . . 1.0000 ? C15 O23 . . 1.419(6) y C15 C16 . . 1.525(9) y C15 H15 . . 1.0000 ? C16 O24 . . 1.397(7) y C16 H16 . . 1.0000 ? C11' O21 . . 1.407(6) y C11' O22 . . 1.419(7) y C11' C12' . . 1.520(8) y C11' H11' . . 1.0000 ? C12' N23 . . 1.474(8) y C12' C13' . . 1.518(8) y C12' H12' . . 1.0000 ? C13' C14' . . 1.456(9) y C13' H13e . . 0.9900 ? C13' H13f . . 0.9900 ? C14' C15' . . 1.340(10) y C14' H14' . . 0.9500 ? C15' O22 . . 1.387(8) y C15' C16' . . 1.398(9) y C16' C17' . . 1.351(10) y C16' H16' . . 0.9500 ? C17' C18' . . 1.429(9) y C17' H17' . . 0.9500 ? C18' H18' . . 0.9500 ? O23 H23 . . 0.8400 ? O24 H24 . . 0.8400 ? N21 H21a . . 0.9100 ? N21 H21b . . 0.9100 ? N21 H21c . . 0.9100 ? N22 C28' . . 1.261(9) y N23 H23a . . 0.9100 ? N23 H23b . . 0.9100 ? N23 H23c . . 0.9100 ? C21 C22 . . 1.475(8) y C21 C26 . . 1.533(7) y C21 H21 . . 1.0000 ? C22 C23 . . 1.550(8) y C22 H22a . . 0.9900 ? C22 H22b . . 0.9900 ? C23 C24 . . 1.527(7) y C23 H23d . . 1.0000 ? C24 C25 . . 1.527(8) y C24 H24a . . 1.0000 ? C25 C26 . . 1.531(8) y C25 H25 . . 1.0000 ? C26 H26 . . 1.0000 ? C21' C22' . . 1.523(9) y C21' H21' . . 1.0000 ? C22' C23' . . 1.537(9) y C22' H22' . . 1.0000 ? C23' C24' . . 1.481(10) y C23' H23e . . 0.9900 ? C23' H23f . . 0.9900 ? C24' C25' . . 1.309(10) y C24' H24' . . 0.9500 ? C25' C26' . . 1.422(9) y C26' C27' . . 1.349(10) y C26' H26' . . 0.9500 ? C27' C28' . . 1.427(9) y C27' H27' . . 0.9500 ? C28' H28' . . 0.9500 ? O31 C31' . . 1.414(6) y O31 C34 . . 1.426(7) y O32 C35' . . 1.374(8) y O32 C31' . . 1.409(7) y O33 C35 . . 1.452(5) y O33 H33 . . 0.8400 ? O34 C36 . . 1.432(6) y O34 H34 . . 0.8400 ? N31 C31 . . 1.503(7) y N31 H31a . . 0.9100 ? N31 H31b . . 0.9100 ? N31 H31c . . 0.9100 ? N32 C48' . . 1.289(8) y N32 C33 . . 1.471(8) y N33 C32' . . 1.490(8) y N33 H33a . . 0.9100 ? N33 H33b . . 0.9100 ? N33 H33c . . 0.9100 ? C31 C32 . . 1.520(8) y C31 C36 . . 1.521(7) y C31 H31 . . 1.0000 ? C32 C33 . . 1.516(8) y C32 H32a . . 0.9900 ? C32 H32b . . 0.9900 ? C33 C34 . . 1.546(6) y C33 H33d . . 1.0000 ? C34 C35 . . 1.508(8) y C34 H34a . . 1.0000 ? C35 C36 . . 1.502(8) y C35 H35 . . 1.0000 ? C36 H36 . . 1.0000 ? C31' C32' . . 1.510(9) y C31' H31' . . 1.0000 ? C32' C33' . . 1.542(9) y C32' H32' . . 1.0000 ? C33' C34' . . 1.477(10) y C33' H33e . . 0.9900 ? C33' H33f . . 0.9900 ? C34' C35' . . 1.351(10) y C34' H34' . . 0.9500 ? C35' C36' . . 1.430(9) y C36' C37' . . 1.356(10) y C36' H36' . . 0.9500 ? C37' C38' . . 1.449(9) y C37' H37' . . 0.9500 ? C38' N42 . . 1.247(9) y C38' H38' . . 0.9500 ? O41 C44 . . 1.425(7) y O41 C41' . . 1.425(6) y O42 C45' . . 1.398(8) y O42 C41' . . 1.437(7) y O43 C45 . . 1.439(5) y O43 H43g . . 0.8400 ? O44 C46 . . 1.430(7) y O44 H44b . . 0.8400 ? N41 C41 . . 1.492(8) y N41 H41a . . 0.9100 ? N41 H41b . . 0.9100 ? N41 H41c . . 0.9100 ? N42 C43 . . 1.469(8) y N43 C42' . . 1.462(8) y N43 H43a . . 0.9100 ? N43 H43b . . 0.9100 ? N43 H43c . . 0.9100 ? C41 C42 . . 1.505(8) y C41 C46 . . 1.526(7) y C41 H41 . . 1.0000 ? C42 C43 . . 1.496(9) y C42 H42a . . 0.9900 ? C42 H42b . . 0.9900 ? C43 C44 . . 1.506(7) y C43 H43d . . 1.0000 ? C44 C45 . . 1.533(9) y C44 H44a . . 1.0000 ? C45 C46 . . 1.519(9) y C45 H45 . . 1.0000 ? C46 H46 . . 1.0000 ? C41' C42' . . 1.518(9) y C41' H41' . . 1.0000 ? C42' C43' . . 1.526(9) y C42' H42' . . 1.0000 ? C43' C44' . . 1.492(10) y C43' H43e . . 0.9900 ? C43' H43f . . 0.9900 ? C44' C45' . . 1.333(10) y C44' H44' . . 0.9500 ? C45' C46' . . 1.435(9) y C46' C47' . . 1.346(9) y C46' H46' . . 0.9500 ? C47' C48' . . 1.429(9) y C47' H47' . . 0.9500 ? C48' H48' . . 0.9500 ? O101 H1e . . 0.863(9) ? O101 H1f . . 0.868(8) ? O102 H2a . . 0.861(9) ? O102 H2b . . 0.863(9) ? O103 H3a . . 0.867(9) ? O103 H3b . . 0.864(9) ? O104 H4a . . 0.8558 ? O104 H4b . . 0.8576 ? O105 H5a . . 0.884(15) ? O105 H5b . . 0.898(15) ? O106 H6a . . 0.878(15) ? O106 H6b . . 0.8693 ? O107 H7a . . 0.8789 ? O107 H7b . . 0.880(15) ? O108 H8a . . 0.874(15) ? O108 H8b . . 0.876(15) ? O109 H9a . . 0.877(15) ? O109 H9b . . 0.870(15) ? O110 H10a . . 0.8790 ? O110 H10b . . 0.868(15) ? O111 H11d . . 0.865(8) ? O111 H11e . . 0.864(9) ? N101 H1a . . 0.906(17) ? N101 H1b . . 0.889(17) ? N101 H1c . . 0.899(17) ? N101 H1d . . 0.900(17) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O52 S1 O51 . . . 111.8(3) y O52 S1 O53 . . . 110.6(3) y O51 S1 O53 . . . 108.0(2) y O52 S1 O54 . . . 108.3(3) y O51 S1 O54 . . . 108.5(3) y O53 S1 O54 . . . 109.7(3) y O63 S2 O61 . . . 110.9(3) y O63 S2 O64 . . . 111.2(3) y O61 S2 O64 . . . 108.9(2) y O63 S2 O62 . . . 107.3(3) y O61 S2 O62 . . . 108.2(2) y O64 S2 O62 . . . 110.3(2) y O74 S3 O71 . . . 106.5(4) y O74 S3 O72 . . . 106.6(4) y O71 S3 O72 . . . 114.0(4) y O74 S3 O73 . . . 107.5(4) y O71 S3 O73 . . . 109.9(5) y O72 S3 O73 . . . 111.9(5) y O84 S4 O83 . . . 111.5(3) y O84 S4 O81 . . . 109.8(3) y O83 S4 O81 . . . 111.4(4) y O84 S4 O82 . . . 109.9(3) y O83 S4 O82 . . . 107.9(3) y O81 S4 O82 . . . 106.3(3) y O93 S5 O94 . . . 109.4(4) y O93 S5 O91 . . . 111.0(4) y O94 S5 O91 . . . 107.3(4) y O93 S5 O92 . . . 103.9(5) y O94 S5 O92 . . . 113.1(5) y O91 S5 O92 . . . 112.2(5) y C21' O11 C24 . . . 118.1(4) y C21' O12 C25' . . . 116.2(5) y C25 O13 H13 . . . 109.5 ? C26 O14 H14 . . . 109.5 ? C21 N11 H11A . . . 109.5 ? C21 N11 H11B . . . 109.5 ? H11A N11 H11B . . . 109.5 ? C21 N11 H11C . . . 109.5 ? H11A N11 H11C . . . 109.5 ? H11B N11 H11C . . . 109.5 ? C18' N12 C23 . . . 118.7(6) y C22' N13 H13A . . . 109.5 ? C22' N13 H13B . . . 109.5 ? H13A N13 H13B . . . 109.5 ? C22' N13 H13C . . . 109.5 ? H13A N13 H13C . . . 109.5 ? H13B N13 H13C . . . 109.5 ? N21 C11 C12 . . . 110.2(5) y N21 C11 C16 . . . 109.8(5) y C12 C11 C16 . . . 110.6(5) y N21 C11 H11 . . . 108.7 ? C12 C11 H11 . . . 108.7 ? C16 C11 H11 . . . 108.7 ? C11 C12 C13 . . . 111.5(5) y C11 C12 H12A . . . 109.3 ? C13 C12 H12A . . . 109.3 ? C11 C12 H12B . . . 109.3 ? C13 C12 H12B . . . 109.3 ? H12A C12 H12B . . . 108.0 ? N22 C13 C14 . . . 111.0(4) y N22 C13 C12 . . . 108.0(5) y C14 C13 C12 . . . 111.0(5) y N22 C13 H13D . . . 108.9 ? C14 C13 H13D . . . 108.9 ? C12 C13 H13D . . . 108.9 ? O21 C14 C13 . . . 106.7(5) y O21 C14 C15 . . . 108.9(5) y C13 C14 C15 . . . 113.1(5) y O21 C14 H14A . . . 109.3 ? C13 C14 H14A . . . 109.3 ? C15 C14 H14A . . . 109.3 ? O23 C15 C16 . . . 111.9(5) y O23 C15 C14 . . . 105.7(5) y C16 C15 C14 . . . 114.2(5) y O23 C15 H15 . . . 108.3 ? C16 C15 H15 . . . 108.3 ? C14 C15 H15 . . . 108.3 ? O24 C16 C15 . . . 111.3(5) y O24 C16 C11 . . . 111.1(4) y C15 C16 C11 . . . 110.3(5) y O24 C16 H16 . . . 108.0 ? C15 C16 H16 . . . 108.0 ? C11 C16 H16 . . . 108.0 ? O21 C11' O22 . . . 112.0(4) y O21 C11' C12' . . . 107.9(5) y O22 C11' C12' . . . 110.7(5) y O21 C11' H11' . . . 108.7 ? O22 C11' H11' . . . 108.7 ? C12' C11' H11' . . . 108.7 ? N23 C12' C13' . . . 111.2(5) y N23 C12' C11' . . . 112.1(5) y C13' C12' C11' . . . 109.1(5) y N23 C12' H12' . . . 108.1 ? C13' C12' H12' . . . 108.1 ? C11' C12' H12' . . . 108.1 ? C14' C13' C12' . . . 109.0(5) y C14' C13' H13E . . . 109.9 ? C12' C13' H13E . . . 109.9 ? C14' C13' H13F . . . 109.9 ? C12' C13' H13F . . . 109.9 ? H13E C13' H13F . . . 108.3 ? C15' C14' C13' . . . 123.2(6) y C15' C14' H14' . . . 118.4 ? C13' C14' H14' . . . 118.4 ? C14' C15' O22 . . . 122.7(6) y C14' C15' C16' . . . 124.0(7) y O22 C15' C16' . . . 113.3(6) y C17' C16' C15' . . . 128.9(7) y C17' C16' H16' . . . 115.6 ? C15' C16' H16' . . . 115.6 ? C16' C17' C18' . . . 123.2(7) y C16' C17' H17' . . . 118.4 ? C18' C17' H17' . . . 118.4 ? N12 C18' C17' . . . 122.8(7) y N12 C18' H18' . . . 118.6 ? C17' C18' H18' . . . 118.6 ? C11' O21 C14 . . . 118.0(4) y C15' O22 C11' . . . 116.6(5) y C15 O23 H23 . . . 109.5 ? C16 O24 H24 . . . 109.5 ? C11 N21 H21A . . . 109.5 ? C11 N21 H21B . . . 109.5 ? H21A N21 H21B . . . 109.5 ? C11 N21 H21C . . . 109.5 ? H21A N21 H21C . . . 109.5 ? H21B N21 H21C . . . 109.5 ? C28' N22 C13 . . . 119.4(6) y C12' N23 H23A . . . 109.5 ? C12' N23 H23B . . . 109.5 ? H23A N23 H23B . . . 109.5 ? C12' N23 H23C . . . 109.5 ? H23A N23 H23C . . . 109.5 ? H23B N23 H23C . . . 109.5 ? N11 C21 C22 . . . 111.9(5) y N11 C21 C26 . . . 111.3(5) y C22 C21 C26 . . . 110.3(4) y N11 C21 H21 . . . 107.7 ? C22 C21 H21 . . . 107.7 ? C26 C21 H21 . . . 107.7 ? C21 C22 C23 . . . 111.8(5) y C21 C22 H22A . . . 109.3 ? C23 C22 H22A . . . 109.3 ? C21 C22 H22B . . . 109.3 ? C23 C22 H22B . . . 109.3 ? H22A C22 H22B . . . 107.9 ? N12 C23 C24 . . . 110.0(5) y N12 C23 C22 . . . 108.7(5) y C24 C23 C22 . . . 111.2(5) y N12 C23 H23D . . . 109.0 ? C24 C23 H23D . . . 109.0 ? C22 C23 H23D . . . 109.0 ? O11 C24 C25 . . . 106.9(5) y O11 C24 C23 . . . 104.8(4) y C25 C24 C23 . . . 113.3(5) y O11 C24 H24A . . . 110.6 ? C25 C24 H24A . . . 110.6 ? C23 C24 H24A . . . 110.6 ? O13 C25 C24 . . . 108.3(4) y O13 C25 C26 . . . 108.5(5) y C24 C25 C26 . . . 113.8(5) y O13 C25 H25 . . . 108.7 ? C24 C25 H25 . . . 108.7 ? C26 C25 H25 . . . 108.7 ? O14 C26 C25 . . . 110.2(5) y O14 C26 C21 . . . 109.5(4) y C25 C26 C21 . . . 107.6(5) y O14 C26 H26 . . . 109.9 ? C25 C26 H26 . . . 109.9 ? C21 C26 H26 . . . 109.9 ? O11 C21' O12 . . . 112.4(4) y O11 C21' C22' . . . 108.0(5) y O12 C21' C22' . . . 112.1(5) y O11 C21' H21' . . . 108.1 ? O12 C21' H21' . . . 108.1 ? C22' C21' H21' . . . 108.1 ? N13 C22' C21' . . . 111.7(5) y N13 C22' C23' . . . 110.8(5) y C21' C22' C23' . . . 108.1(5) y N13 C22' H22' . . . 108.7 ? C21' C22' H22' . . . 108.7 ? C23' C22' H22' . . . 108.7 ? C24' C23' C22' . . . 108.3(6) y C24' C23' H23E . . . 110.0 ? C22' C23' H23E . . . 110.0 ? C24' C23' H23F . . . 110.0 ? C22' C23' H23F . . . 110.0 ? H23E C23' H23F . . . 108.4 ? C25' C24' C23' . . . 124.6(6) y C25' C24' H24' . . . 117.7 ? C23' C24' H24' . . . 117.7 ? C24' C25' O12 . . . 122.0(6) y C24' C25' C26' . . . 125.9(6) y O12 C25' C26' . . . 112.1(6) y C27' C26' C25' . . . 127.3(7) y C27' C26' H26' . . . 116.3 ? C25' C26' H26' . . . 116.3 ? C26' C27' C28' . . . 121.2(7) y C26' C27' H27' . . . 119.4 ? C28' C27' H27' . . . 119.4 ? N22 C28' C27' . . . 121.9(7) y N22 C28' H28' . . . 119.0 ? C27' C28' H28' . . . 119.0 ? C31' O31 C34 . . . 117.4(4) y C35' O32 C31' . . . 116.9(5) y C35 O33 H33 . . . 109.5 ? C36 O34 H34 . . . 109.5 ? C31 N31 H31A . . . 109.5 ? C31 N31 H31B . . . 109.5 ? H31A N31 H31B . . . 109.5 ? C31 N31 H31C . . . 109.5 ? H31A N31 H31C . . . 109.5 ? H31B N31 H31C . . . 109.5 ? C48' N32 C33 . . . 119.5(6) y C32' N33 H33A . . . 109.5 ? C32' N33 H33B . . . 109.5 ? H33A N33 H33B . . . 109.5 ? C32' N33 H33C . . . 109.5 ? H33A N33 H33C . . . 109.5 ? H33B N33 H33C . . . 109.5 ? N31 C31 C32 . . . 109.3(4) y N31 C31 C36 . . . 111.4(5) y C32 C31 C36 . . . 109.4(4) y N31 C31 H31 . . . 108.9 ? C32 C31 H31 . . . 108.9 ? C36 C31 H31 . . . 108.9 ? C33 C32 C31 . . . 109.5(5) y C33 C32 H32A . . . 109.8 ? C31 C32 H32A . . . 109.8 ? C33 C32 H32B . . . 109.8 ? C31 C32 H32B . . . 109.8 ? H32A C32 H32B . . . 108.2 ? N32 C33 C32 . . . 107.7(5) y N32 C33 C34 . . . 108.4(4) y C32 C33 C34 . . . 113.0(4) y N32 C33 H33D . . . 109.2 ? C32 C33 H33D . . . 109.2 ? C34 C33 H33D . . . 109.2 ? O31 C34 C35 . . . 110.0(4) y O31 C34 C33 . . . 105.3(4) y C35 C34 C33 . . . 111.4(4) y O31 C34 H34A . . . 110.0 ? C35 C34 H34A . . . 110.0 ? C33 C34 H34A . . . 110.0 ? O33 C35 C36 . . . 109.6(4) y O33 C35 C34 . . . 106.0(4) y C36 C35 C34 . . . 115.7(4) y O33 C35 H35 . . . 108.4 ? C36 C35 H35 . . . 108.4 ? C34 C35 H35 . . . 108.4 ? O34 C36 C35 . . . 110.4(4) y O34 C36 C31 . . . 108.0(4) y C35 C36 C31 . . . 107.8(4) y O34 C36 H36 . . . 110.2 ? C35 C36 H36 . . . 110.2 ? C31 C36 H36 . . . 110.2 ? O32 C31' O31 . . . 111.4(4) y O32 C31' C32' . . . 111.5(5) y O31 C31' C32' . . . 107.8(5) y O32 C31' H31' . . . 108.7 ? O31 C31' H31' . . . 108.7 ? C32' C31' H31' . . . 108.7 ? N33 C32' C31' . . . 110.5(5) y N33 C32' C33' . . . 110.9(5) y C31' C32' C33' . . . 108.4(5) y N33 C32' H32' . . . 109.0 ? C31' C32' H32' . . . 109.0 ? C33' C32' H32' . . . 109.0 ? C34' C33' C32' . . . 108.5(6) y C34' C33' H33E . . . 110.0 ? C32' C33' H33E . . . 110.0 ? C34' C33' H33F . . . 110.0 ? C32' C33' H33F . . . 110.0 ? H33E C33' H33F . . . 108.4 ? C35' C34' C33' . . . 121.1(6) y C35' C34' H34' . . . 119.4 ? C33' C34' H34' . . . 119.4 ? C34' C35' O32 . . . 124.1(6) y C34' C35' C36' . . . 120.6(6) y O32 C35' C36' . . . 115.3(6) y C37' C36' C35' . . . 125.7(7) y C37' C36' H36' . . . 117.2 ? C35' C36' H36' . . . 117.2 ? C36' C37' C38' . . . 120.7(7) y C36' C37' H37' . . . 119.6 ? C38' C37' H37' . . . 119.6 ? N42 C38' C37' . . . 124.1(7) y N42 C38' H38' . . . 118.0 ? C37' C38' H38' . . . 118.0 ? C44 O41 C41' . . . 116.5(4) y C45' O42 C41' . . . 117.0(5) y C45 O43 H43G . . . 109.5 ? C46 O44 H44B . . . 109.5 ? C41 N41 H41A . . . 109.5 ? C41 N41 H41B . . . 109.5 ? H41A N41 H41B . . . 109.5 ? C41 N41 H41C . . . 109.5 ? H41A N41 H41C . . . 109.5 ? H41B N41 H41C . . . 109.5 ? C38' N42 C43 . . . 118.4(6) y C42' N43 H43A . . . 109.5 ? C42' N43 H43B . . . 109.5 ? H43A N43 H43B . . . 109.5 ? C42' N43 H43C . . . 109.5 ? H43A N43 H43C . . . 109.5 ? H43B N43 H43C . . . 109.5 ? N41 C41 C42 . . . 109.9(5) y N41 C41 C46 . . . 109.6(5) y C42 C41 C46 . . . 110.1(5) y N41 C41 H41 . . . 109.1 ? C42 C41 H41 . . . 109.1 ? C46 C41 H41 . . . 109.1 ? C43 C42 C41 . . . 112.5(5) y C43 C42 H42A . . . 109.1 ? C41 C42 H42A . . . 109.1 ? C43 C42 H42B . . . 109.1 ? C41 C42 H42B . . . 109.1 ? H42A C42 H42B . . . 107.8 ? N42 C43 C42 . . . 109.2(5) y N42 C43 C44 . . . 109.9(5) y C42 C43 C44 . . . 111.9(5) y N42 C43 H43D . . . 108.6 ? C42 C43 H43D . . . 108.6 ? C44 C43 H43D . . . 108.6 ? O41 C44 C43 . . . 108.3(5) y O41 C44 C45 . . . 108.3(5) y C43 C44 C45 . . . 111.8(5) y O41 C44 H44A . . . 109.4 ? C43 C44 H44A . . . 109.4 ? C45 C44 H44A . . . 109.4 ? O43 C45 C46 . . . 110.5(5) y O43 C45 C44 . . . 105.8(4) y C46 C45 C44 . . . 114.1(5) y O43 C45 H45 . . . 108.8 ? C46 C45 H45 . . . 108.8 ? C44 C45 H45 . . . 108.8 ? O44 C46 C45 . . . 111.4(5) y O44 C46 C41 . . . 110.5(4) y C45 C46 C41 . . . 109.9(5) y O44 C46 H46 . . . 108.3 ? C45 C46 H46 . . . 108.3 ? C41 C46 H46 . . . 108.3 ? O41 C41' O42 . . . 109.4(4) y O41 C41' C42' . . . 107.2(4) y O42 C41' C42' . . . 111.0(5) y O41 C41' H41' . . . 109.7 ? O42 C41' H41' . . . 109.7 ? C42' C41' H41' . . . 109.7 ? N43 C42' C41' . . . 110.7(5) y N43 C42' C43' . . . 110.5(5) y C41' C42' C43' . . . 110.2(5) y N43 C42' H42' . . . 108.4 ? C41' C42' H42' . . . 108.4 ? C43' C42' H42' . . . 108.4 ? C44' C43' C42' . . . 109.5(6) y C44' C43' H43E . . . 109.8 ? C42' C43' H43E . . . 109.8 ? C44' C43' H43F . . . 109.8 ? C42' C43' H43F . . . 109.8 ? H43E C43' H43F . . . 108.2 ? C45' C44' C43' . . . 121.4(6) y C45' C44' H44' . . . 119.3 ? C43' C44' H44' . . . 119.3 ? C44' C45' O42 . . . 124.3(6) y C44' C45' C46' . . . 122.4(7) y O42 C45' C46' . . . 113.3(6) y C47' C46' C45' . . . 126.5(7) y C47' C46' H46' . . . 116.7 ? C45' C46' H46' . . . 116.7 ? C46' C47' C48' . . . 120.8(7) y C46' C47' H47' . . . 119.6 ? C48' C47' H47' . . . 119.6 ? N32 C48' C47' . . . 121.8(7) y N32 C48' H48' . . . 119.1 ? C47' C48' H48' . . . 119.1 ? H1E O101 H1F . . . 105(5) ? H2A O102 H2B . . . 106(4) ? H3A O103 H3B . . . 103(6) ? H4A O104 H4B . . . 106.1 ? H5A O105 H5B . . . 98(5) ? H6A O106 H6B . . . 101.8 ? H7A O107 H7B . . . 101.0 ? H8A O108 H8B . . . 102(6) ? H9A O109 H9B . . . 103(9) ? H10A O110 H10B . . . 103.2 ? H11D O111 H11E . . . 104.4(17) ? H1A N101 H1B . . . 110(2) ? H1A N101 H1C . . . 108(2) ? H1B N101 H1C . . . 110(2) ? H1A N101 H1D . . . 109(2) ? H1B N101 H1D . . . 110(2) ? H1C N101 H1D . . . 109(2) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N21 C11 C12 C13 . . . . 178.0(5) y C16 C11 C12 C13 . . . . -60.4(6) y C11 C12 C13 N22 . . . . 178.7(4) y C11 C12 C13 C14 . . . . 56.8(6) y N22 C13 C14 O21 . . . . 70.8(6) y C12 C13 C14 O21 . . . . -169.1(5) y N22 C13 C14 C15 . . . . -169.4(5) y C12 C13 C14 C15 . . . . -49.3(7) y O21 C14 C15 O23 . . . . -70.2(6) y C13 C14 C15 O23 . . . . 171.3(5) y O21 C14 C15 C16 . . . . 166.4(4) y C13 C14 C15 C16 . . . . 47.9(7) y O23 C15 C16 O24 . . . . 66.0(6) y C14 C15 C16 O24 . . . . -173.9(4) y O23 C15 C16 C11 . . . . -170.2(5) y C14 C15 C16 C11 . . . . -50.1(6) y N21 C11 C16 O24 . . . . -57.8(6) y C12 C11 C16 O24 . . . . -179.6(5) y N21 C11 C16 C15 . . . . 178.3(5) y C12 C11 C16 C15 . . . . 56.5(6) y O21 C11' C12' N23 . . . . 62.3(6) y O22 C11' C12' N23 . . . . -174.8(4) y O21 C11' C12' C13' . . . . -61.3(6) y O22 C11' C12' C13' . . . . 61.6(6) y N23 C12' C13' C14' . . . . -173.7(5) y C11' C12' C13' C14' . . . . -49.6(6) y C12' C13' C14' C15' . . . . 19.4(8) y C13' C14' C15' O22 . . . . 3.1(9) y C13' C14' C15' C16' . . . . -177.0(5) y C14' C15' C16' C17' . . . . -167.0(6) y O22 C15' C16' C17' . . . . 12.8(8) y C15' C16' C17' C18' . . . . 177.5(5) y C23 N12 C18' C17' . . . . 179.1(5) y C16' C17' C18' N12 . . . . -170.7(5) y O22 C11' O21 C14 . . . . 86.7(6) y C12' C11' O21 C14 . . . . -151.2(5) y C13 C14 O21 C11' . . . . -141.0(5) y C15 C14 O21 C11' . . . . 96.6(5) y C14' C15' O22 C11' . . . . 7.6(8) y C16' C15' O22 C11' . . . . -172.3(4) y O21 C11' O22 C15' . . . . 80.7(6) y C12' C11' O22 C15' . . . . -39.7(6) y C14 C13 N22 C28' . . . . -93.2(6) y C12 C13 N22 C28' . . . . 144.9(5) y N11 C21 C22 C23 . . . . 173.1(5) y C26 C21 C22 C23 . . . . -62.4(7) y C18' N12 C23 C24 . . . . -94.6(6) y C18' N12 C23 C22 . . . . 143.5(5) y C21 C22 C23 N12 . . . . 174.2(5) y C21 C22 C23 C24 . . . . 53.0(7) y C21' O11 C24 C25 . . . . 95.8(5) y C21' O11 C24 C23 . . . . -143.7(5) y N12 C23 C24 O11 . . . . 78.1(6) y C22 C23 C24 O11 . . . . -161.5(5) y N12 C23 C24 C25 . . . . -165.8(5) y C22 C23 C24 C25 . . . . -45.3(7) y O11 C24 C25 O13 . . . . -75.5(5) y C23 C24 C25 O13 . . . . 169.6(5) y O11 C24 C25 C26 . . . . 163.7(4) y C23 C24 C25 C26 . . . . 48.8(7) y O13 C25 C26 O14 . . . . 64.7(6) y C24 C25 C26 O14 . . . . -174.7(4) y O13 C25 C26 C21 . . . . -176.0(5) y C24 C25 C26 C21 . . . . -55.4(6) y N11 C21 C26 O14 . . . . -53.2(7) y C22 C21 C26 O14 . . . . -178.0(5) y N11 C21 C26 C25 . . . . -172.9(5) y C22 C21 C26 C25 . . . . 62.2(7) y C24 O11 C21' O12 . . . . 82.6(6) y C24 O11 C21' C22' . . . . -153.2(5) y C25' O12 C21' O11 . . . . 82.2(6) y C25' O12 C21' C22' . . . . -39.6(6) y O11 C21' C22' N13 . . . . 59.1(6) y O12 C21' C22' N13 . . . . -176.6(4) y O11 C21' C22' C23' . . . . -63.0(6) y O12 C21' C22' C23' . . . . 61.3(6) y N13 C22' C23' C24' . . . . -172.0(5) y C21' C22' C23' C24' . . . . -49.4(6) y C22' C23' C24' C25' . . . . 20.9(9) y C23' C24' C25' O12 . . . . 1.8(9) y C23' C24' C25' C26' . . . . -176.9(6) y C21' O12 C25' C24' . . . . 7.6(7) y C21' O12 C25' C26' . . . . -173.5(4) y C24' C25' C26' C27' . . . . -163.7(6) y O12 C25' C26' C27' . . . . 17.5(8) y C25' C26' C27' C28' . . . . 176.1(5) y C13 N22 C28' C27' . . . . -179.1(5) y C26' C27' C28' N22 . . . . -171.7(5) y N31 C31 C32 C33 . . . . 174.3(4) y C36 C31 C32 C33 . . . . -63.5(6) y C48' N32 C33 C32 . . . . 141.0(5) y C48' N32 C33 C34 . . . . -96.5(6) y C31 C32 C33 N32 . . . . 174.0(4) y C31 C32 C33 C34 . . . . 54.3(6) y C31' O31 C34 C35 . . . . 96.3(5) y C31' O31 C34 C33 . . . . -143.6(5) y N32 C33 C34 O31 . . . . 76.1(5) y C32 C33 C34 O31 . . . . -164.7(5) y N32 C33 C34 C35 . . . . -164.7(5) y C32 C33 C34 C35 . . . . -45.4(7) y O31 C34 C35 O33 . . . . -74.7(5) y C33 C34 C35 O33 . . . . 168.9(4) y O31 C34 C35 C36 . . . . 163.6(4) y C33 C34 C35 C36 . . . . 47.2(6) y O33 C35 C36 O34 . . . . 66.6(6) y C34 C35 C36 O34 . . . . -173.6(4) y O33 C35 C36 C31 . . . . -175.7(4) y C34 C35 C36 C31 . . . . -55.9(6) y N31 C31 C36 O34 . . . . -57.1(6) y C32 C31 C36 O34 . . . . -178.0(4) y N31 C31 C36 C35 . . . . -176.3(5) y C32 C31 C36 C35 . . . . 62.8(6) y C35' O32 C31' O31 . . . . 81.7(6) y C35' O32 C31' C32' . . . . -38.7(6) y C34 O31 C31' O32 . . . . 81.1(6) y C34 O31 C31' C32' . . . . -156.3(5) y O32 C31' C32' N33 . . . . -176.8(4) y O31 C31' C32' N33 . . . . 60.7(6) y O32 C31' C32' C33' . . . . 61.5(6) y O31 C31' C32' C33' . . . . -61.0(6) y N33 C32' C33' C34' . . . . -173.1(5) y C31' C32' C33' C34' . . . . -51.6(7) y C32' C33' C34' C35' . . . . 23.0(8) y C33' C34' C35' O32 . . . . 0.4(10) y C33' C34' C35' C36' . . . . -178.8(6) y C31' O32 C35' C34' . . . . 7.2(8) y C31' O32 C35' C36' . . . . -173.5(5) y C34' C35' C36' C37' . . . . -164.5(6) y O32 C35' C36' C37' . . . . 16.1(8) y C35' C36' C37' C38' . . . . 178.5(5) y C36' C37' C38' N42 . . . . -169.2(6) y C37' C38' N42 C43 . . . . -179.2(5) y N41 C41 C42 C43 . . . . 179.9(5) y C46 C41 C42 C43 . . . . -59.3(6) y C38' N42 C43 C42 . . . . 145.4(5) y C38' N42 C43 C44 . . . . -91.5(6) y C41 C42 C43 N42 . . . . 178.1(4) y C41 C42 C43 C44 . . . . 56.2(6) y C41' O41 C44 C43 . . . . -144.7(5) y C41' O41 C44 C45 . . . . 93.9(5) y N42 C43 C44 O41 . . . . 69.5(6) y C42 C43 C44 O41 . . . . -169.1(5) y N42 C43 C44 C45 . . . . -171.3(5) y C42 C43 C44 C45 . . . . -49.8(7) y O41 C44 C45 O43 . . . . -69.8(5) y C43 C44 C45 O43 . . . . 170.9(5) y O41 C44 C45 C46 . . . . 168.6(4) y C43 C44 C45 C46 . . . . 49.3(7) y O43 C45 C46 O44 . . . . 65.9(6) y C44 C45 C46 O44 . . . . -175.0(4) y O43 C45 C46 C41 . . . . -171.2(5) y C44 C45 C46 C41 . . . . -52.2(6) y N41 C41 C46 O44 . . . . -59.7(6) y C42 C41 C46 O44 . . . . 179.3(5) y N41 C41 C46 C45 . . . . 177.0(5) y C42 C41 C46 C45 . . . . 56.0(6) y C44 O41 C41' O42 . . . . 92.7(6) y C44 O41 C41' C42' . . . . -146.8(5) y C45' O42 C41' O41 . . . . 81.6(6) y C45' O42 C41' C42' . . . . -36.6(6) y O41 C41' C42' N43 . . . . 61.8(6) y O42 C41' C42' N43 . . . . -178.7(4) y O41 C41' C42' C43' . . . . -60.8(6) y O42 C41' C42' C43' . . . . 58.7(6) y N43 C42' C43' C44' . . . . -172.2(5) y C41' C42' C43' C44' . . . . -49.5(7) y C42' C43' C44' C45' . . . . 20.9(9) y C43' C44' C45' O42 . . . . 1.7(10) y C43' C44' C45' C46' . . . . 179.4(6) y C41' O42 C45' C44' . . . . 6.5(9) y C41' O42 C45' C46' . . . . -171.5(4) y C44' C45' C46' C47' . . . . -164.6(6) y O42 C45' C46' C47' . . . . 13.4(8) y C45' C46' C47' C48' . . . . 177.4(5) y C33 N32 C48' C47' . . . . -179.1(5) y C46' C47' C48' N32 . . . . -170.9(5) y 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 _geom_hbond_publ_flag O14 H14 O73 0.84 2.15 2.668(7) 119.9 1_545 y N11 H11A O71 0.91 1.96 2.816(8) 156.7 1_445 y N11 H11B O93 0.91 1.9 2.778(9) 162.1 1_454 y N11 H11B O94 0.91 2.43 3.105(9) 131.4 1_454 y N11 H11C O13 0.91 2.18 2.911(7) 136.8 1_455 y N13 H13A O101 0.91 1.98 2.868(7) 165.4 . y N13 H13B O62 0.91 1.93 2.817(6) 163.2 . y N13 H13C O64 0.91 1.99 2.798(6) 147.5 1_455 y O23 H23 O64 0.84 2.05 2.782(6) 146 1_465 y O24 H24 O62 0.84 2.06 2.693(6) 131.6 1_565 y N21 H21B O14 0.91 2.04 2.865(7) 150 1_665 y N21 H21C O71 0.91 2.45 2.993(8) 118.9 . y N23 H23A O82 0.91 2.04 2.824(7) 144 1_455 y N23 H23B O61 0.91 1.91 2.803(6) 165.1 1_465 y N23 H23C O102 0.91 2.13 2.873(6) 138.1 . y O33 H33 O44 0.84 1.91 2.693(5) 153.6 1_545 y O34 H34 O83 0.84 1.82 2.639(6) 162.8 1_545 y N31 H31A O105 0.91 1.9 2.807(7) 173.2 1_455 y N31 H31B O33 0.91 2.23 2.936(6) 133.5 1_455 y N31 H31C O82 0.91 1.92 2.769(6) 154.9 1_445 y N31 H31C O83 0.91 2.63 3.150(7) 117 1_445 y N33 H33A O53 0.91 1.95 2.764(6) 148.3 . y N33 H33B O91 0.91 1.91 2.804(7) 167 . y N33 H33C O54 0.91 1.9 2.803(6) 169.9 1_655 y O43 H43G O53 0.84 1.89 2.705(6) 164.3 1_565 y O44 H44B O54 0.84 1.85 2.663(6) 161.1 1_665 y N41 H41A O103 0.91 1.85 2.755(7) 173.2 1_655 y N41 H41B O34 0.91 1.98 2.814(7) 152.2 1_665 y N41 H41C O81 0.91 1.94 2.835(7) 167.6 . y N41 H41C O82 0.91 2.53 3.131(7) 123.6 . y N43 H43B O74 0.91 1.86 2.770(8) 175.1 1_556 y N43 H43C O51 0.91 1.88 2.771(7) 166 1_565 y O101 H1E O102 0.863(9) 2.03(3) 2.722(7) 137(4) 1_545 y O101 H1F O111 0.868(8) 2.12(4) 2.830(8) 138(5) . y O102 H2A O84 0.861(9) 1.88(3) 2.657(6) 149(5) . y O102 H2A O83 0.861(9) 2.62(3) 3.355(8) 144(4) . y O102 H2B O61 0.863(9) 1.947(15) 2.777(6) 161(4) 1_565 y O103 H3A O107 0.867(9) 1.97(5) 2.765(8) 151(8) . y O103 H3B O81 0.864(9) 1.974(15) 2.829(7) 170(6) . y O104 H4A O106 0.86 2.01 2.863(8) 178 1_455 y O104 H4B O111 0.86 1.98 2.837(8) 178.1 . y O105 H5A O63 0.884(15) 1.97(4) 2.641(6) 132(4) . y O105 H5B O101 0.898(15) 2.18(5) 2.749(7) 121(5) 1_655 y O106 H6B O110 0.87 2.21 3.082(10) 177.6 . y O107 H7A O108 0.88 1.95 2.832(9) 177.8 . y O107 H7B O110 0.880(15) 2.31(4) 2.794(10) 115(3) 1_455 y O108 H8B O104 0.876(15) 1.90(3) 2.743(8) 162(9) . y O109 H9A O81 0.877(15) 2.11(9) 2.880(9) 146(14) . y O109 H9B O107 0.870(15) 1.969(15) 2.814(10) 163(4) . y O110 H10A O109 0.88 2.21 3.089(12) 175.3 . y O111 H11E O106 0.864(9) 2.11(3) 2.886(9) 150(5) . y N101 H1A O91 0.906(17) 2.51(4) 3.042(8) 118(3) . y N101 H1B O74 0.889(17) 2.16(3) 2.894(10) 139(4) 1_546 y N101 H1C O94 0.899(17) 2.24(4) 2.853(10) 125(4) 1_455 y N101 H1D O52 0.900(17) 2.23(4) 2.730(9) 115(4) . y _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 69.17 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 1.126 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.114 #=== END OF THE CIF FILE