# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Turowska-Tyrk, Ilona' _publ_contact_author_email ilona.turowska-tyrk@pwr.wroc.pl loop_ _publ_author_name J.Bakowicz J.Skarzewski I.Turowska-Tyrk data_0.0%P _database_code_depnum_ccdc_archive 'CCDC 799253' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 N O4' _chemical_formula_weight 513.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.375(2) _cell_length_b 10.734(3) _cell_length_c 29.950(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3013.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 3.8 _cell_measurement_theta_max 19.9 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14678 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3010 _reflns_number_gt 2263 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSALIS (Oxford Diffraction, 2003)' _computing_cell_refinement 'CRYSALIS (Oxford Diffraction, 2003)' _computing_data_reduction 'CRYSALIS (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Owing to a reactant-product disorder, the following weak restraints from SHELXL97 were applied: DFIX, DANG and SIMU. DFIX and DANG restrained bond lengths and valence angles to target values. The target values were taken from the structures of the pure reactant and the pure product of crystal 1a. SIMU restrained displacement parameters of atoms of the products. ; _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^)+(0.0983P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.009(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _chemical_absolute_configuration syn _refine_ls_number_reflns 3010 _refine_ls_number_parameters 368 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1563 _refine_ls_wR_factor_gt 0.1433 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.7386(3) 0.2962(3) -0.00653(10) 0.0631(8) Uani 1 1 d . . . HN1 H 0.646(4) 0.270(4) -0.0062(12) 0.069(11) Uiso 1 1 d . . . O1 O 0.5360(4) -0.2531(3) 0.10533(10) 0.0890(9) Uani 1 1 d . A . O2 O 0.9477(2) 0.2809(2) 0.02943(8) 0.0645(7) Uani 1 1 d . . . O3 O 0.7736(5) 0.6169(3) -0.00961(18) 0.1397(16) Uani 1 1 d . . . O4 O 0.5775(3) 0.5079(3) -0.00735(12) 0.0958(10) Uani 1 1 d . . . C1 C 0.6537(5) -0.1886(4) 0.20111(12) 0.0696(10) Uani 1 1 d . . . C2 C 0.7260(6) -0.2205(4) 0.23956(14) 0.0861(13) Uani 1 1 d . A . H2 H 0.6869 -0.1969 0.2668 0.103 Uiso 1 1 calc R . . C3 C 0.8520(6) -0.2849(5) 0.23986(13) 0.0911(14) Uani 1 1 d D . . C4 C 0.9082(5) -0.3182(5) 0.19931(18) 0.0937(14) Uani 1 1 d . A . H4 H 0.9940 -0.3617 0.1987 0.112 Uiso 1 1 calc R . . C5 C 0.8411(5) -0.2892(4) 0.15844(13) 0.0766(11) Uani 1 1 d . . . C6 C 0.7141(4) -0.2247(3) 0.16041(11) 0.0604(9) Uani 1 1 d . A . C7 C 0.6383(4) -0.1915(3) 0.11791(12) 0.0613(9) Uani 1 1 d . . . C8 C 0.6857(4) -0.0805(3) 0.09309(11) 0.0537(8) Uani 1 1 d . A . C9 C 0.6308(4) -0.0561(3) 0.05095(11) 0.0543(8) Uani 1 1 d . . . H9 H 0.5642 -0.1099 0.0384 0.065 Uiso 1 1 calc R A . C10 C 0.6750(4) 0.0476(3) 0.02778(11) 0.0547(8) Uani 1 1 d . A . H10 H 0.6381 0.0628 -0.0005 0.066 Uiso 1 1 calc R . . C11 C 0.7729(3) 0.1297(3) 0.04575(10) 0.0511(8) Uani 1 1 d . . . C12 C 0.8276(4) 0.1045(4) 0.08798(11) 0.0565(9) Uani 1 1 d . A . H12 H 0.8941 0.1582 0.1006 0.068 Uiso 1 1 calc R . . C13 C 0.7842(4) 0.0017(3) 0.11086(11) 0.0590(9) Uani 1 1 d . . . H13 H 0.8216 -0.0137 0.1391 0.071 Uiso 1 1 calc R A . C14 C 0.5175(6) -0.1168(4) 0.20300(17) 0.0888(14) Uani 1 1 d . . . H14 H 0.4974 -0.0885 0.1725 0.107 Uiso 1 1 calc R . . C15 C 0.3954(8) -0.1992(7) 0.2167(3) 0.174(4) Uani 1 1 d . . . H15A H 0.3093 -0.1510 0.2180 0.261 Uiso 1 1 calc R . . H15B H 0.4146 -0.2342 0.2456 0.261 Uiso 1 1 calc R . . H15C H 0.3844 -0.2651 0.1953 0.261 Uiso 1 1 calc R . . C16 C 0.5280(10) -0.0010(7) 0.2319(2) 0.157(3) Uani 1 1 d . . . H16A H 0.4378 0.0413 0.2321 0.235 Uiso 1 1 calc R . . H16B H 0.6000 0.0535 0.2201 0.235 Uiso 1 1 calc R . . H16C H 0.5529 -0.0244 0.2618 0.235 Uiso 1 1 calc R . . C17A C 0.9234(8) -0.3141(6) 0.28304(18) 0.140(3) Uani 0.44(3) 1 d PD A 1 H17A H 0.8418 -0.3159 0.3035 0.167 Uiso 0.44(3) 1 calc PR A 1 C18A C 1.006(3) -0.2084(16) 0.3011(7) 0.132(8) Uani 0.44(3) 1 d PDU A 1 H18A H 0.9568 -0.1320 0.2945 0.198 Uiso 0.44(3) 1 calc PR A 1 H18B H 1.0986 -0.2071 0.2876 0.198 Uiso 0.44(3) 1 calc PR A 1 H18C H 1.0150 -0.2174 0.3328 0.198 Uiso 0.44(3) 1 calc PR A 1 C19A C 0.971(3) -0.4455(12) 0.2846(8) 0.148(8) Uani 0.44(3) 1 d PDU A 1 H19A H 0.8969 -0.4981 0.2728 0.221 Uiso 0.44(3) 1 calc PR A 1 H19B H 0.9906 -0.4686 0.3149 0.221 Uiso 0.44(3) 1 calc PR A 1 H19C H 1.0556 -0.4550 0.2669 0.221 Uiso 0.44(3) 1 calc PR A 1 C17B C 0.9234(8) -0.3141(6) 0.28304(18) 0.140(3) Uani 0.56(3) 1 d PD A 2 H17B H 0.8679 -0.2622 0.3036 0.167 Uiso 0.56(3) 1 calc PR A 2 C18B C 1.0684(17) -0.259(2) 0.2888(6) 0.142(7) Uani 0.56(3) 1 d PDU A 2 H18D H 1.0711 -0.1781 0.2752 0.213 Uiso 0.56(3) 1 calc PR A 2 H18E H 1.1378 -0.3120 0.2747 0.213 Uiso 0.56(3) 1 calc PR A 2 H18F H 1.0897 -0.2519 0.3200 0.213 Uiso 0.56(3) 1 calc PR A 2 C19B C 0.8987(19) -0.4358(11) 0.3017(5) 0.105(5) Uani 0.56(3) 1 d PDU A 2 H19D H 0.9482 -0.4431 0.3296 0.157 Uiso 0.56(3) 1 calc PR A 2 H19E H 0.9330 -0.4982 0.2813 0.157 Uiso 0.56(3) 1 calc PR A 2 H19F H 0.7983 -0.4474 0.3065 0.157 Uiso 0.56(3) 1 calc PR A 2 C20 C 0.9075(6) -0.3269(5) 0.11417(16) 0.0990(17) Uani 1 1 d . A . H20 H 0.8493 -0.2899 0.0904 0.119 Uiso 1 1 calc R . . C21 C 0.9037(9) -0.4655(6) 0.1078(2) 0.148(3) Uani 1 1 d . . . H21A H 0.9466 -0.4864 0.0797 0.222 Uiso 1 1 calc R A . H21B H 0.8066 -0.4937 0.1082 0.222 Uiso 1 1 calc R . . H21C H 0.9557 -0.5051 0.1315 0.222 Uiso 1 1 calc R . . C22 C 1.0575(8) -0.2759(8) 0.1092(3) 0.156(3) Uani 1 1 d . . . H22A H 1.0963 -0.3020 0.0810 0.234 Uiso 1 1 calc R A . H22B H 1.1163 -0.3070 0.1329 0.234 Uiso 1 1 calc R . . H22C H 1.0549 -0.1866 0.1103 0.234 Uiso 1 1 calc R . . C23 C 0.8271(4) 0.2417(3) 0.02236(10) 0.0525(8) Uani 1 1 d . A . C24 C 0.7801(4) 0.4032(4) -0.03272(12) 0.0649(10) Uani 1 1 d . . . H24 H 0.8837 0.4127 -0.0299 0.078 Uiso 1 1 calc R . . C25 C 0.7119(5) 0.5213(4) -0.01541(15) 0.0758(11) Uani 1 1 d . . . C26 C 0.4986(6) 0.6138(5) 0.0082(2) 0.1131(18) Uani 1 1 d . . . H26A H 0.5335 0.6383 0.0371 0.170 Uiso 1 1 calc R . . H26B H 0.3994 0.5926 0.0104 0.170 Uiso 1 1 calc R . . H26C H 0.5101 0.6816 -0.0124 0.170 Uiso 1 1 calc R . . C27 C 0.7462(5) 0.3839(4) -0.08200(13) 0.0750(11) Uani 1 1 d . . . H27A H 0.6446 0.3694 -0.0854 0.090 Uiso 1 1 calc R . . H27B H 0.7701 0.4591 -0.0984 0.090 Uiso 1 1 calc R . . C28 C 0.8261(4) 0.2769(4) -0.10133(12) 0.0700(11) Uani 1 1 d D . . C29 C 0.7683(6) 0.1591(4) -0.10167(17) 0.0995(15) Uani 1 1 d D . . H29 H 0.6763 0.1471 -0.0909 0.119 Uiso 1 1 calc R . . C30 C 0.8437(7) 0.0591(5) -0.1175(2) 0.1168(19) Uani 1 1 d D . . H30 H 0.8023 -0.0196 -0.1172 0.140 Uiso 1 1 calc R . . C31 C 0.9798(7) 0.0735(5) -0.13407(19) 0.1131(18) Uani 1 1 d D . . H31 H 1.0316 0.0054 -0.1443 0.136 Uiso 1 1 calc R . . C32 C 1.0363(6) 0.1903(5) -0.13494(19) 0.1087(17) Uani 1 1 d D . . H32 H 1.1271 0.2023 -0.1467 0.130 Uiso 1 1 calc R . . C33 C 0.9618(4) 0.2907(4) -0.11880(15) 0.0853(13) Uani 1 1 d D . . H33 H 1.0032 0.3694 -0.1196 0.102 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 N1 0.0491(17) 0.0677(19) 0.0724(18) 0.0209(16) -0.0061(15) -0.0067(15) O1 0.106(2) 0.0750(18) 0.0859(18) 0.0176(15) -0.0286(17) -0.0270(18) O2 0.0477(13) 0.0707(16) 0.0750(15) 0.0104(13) -0.0060(11) -0.0045(12) O3 0.119(3) 0.085(2) 0.215(5) -0.010(3) 0.030(3) -0.033(2) O4 0.075(2) 0.085(2) 0.128(3) -0.0300(19) 0.0010(18) -0.0073(17) C1 0.092(3) 0.055(2) 0.062(2) 0.0095(18) 0.000(2) 0.002(2) C2 0.120(4) 0.075(3) 0.063(2) 0.011(2) -0.005(2) 0.006(3) C3 0.123(4) 0.088(3) 0.063(2) 0.022(2) -0.020(3) -0.009(3) C4 0.091(3) 0.083(3) 0.107(3) 0.025(3) -0.024(3) 0.018(3) C5 0.089(3) 0.071(2) 0.070(2) 0.012(2) -0.007(2) 0.020(2) C6 0.074(2) 0.0512(19) 0.0558(18) 0.0117(16) -0.0065(17) 0.0068(18) C7 0.071(2) 0.052(2) 0.060(2) 0.0038(17) -0.0052(18) 0.002(2) C8 0.0550(19) 0.0513(18) 0.0547(18) 0.0040(15) -0.0076(15) 0.0066(16) C9 0.056(2) 0.0503(19) 0.0561(19) -0.0015(16) -0.0128(15) 0.0010(16) C10 0.0586(19) 0.0568(19) 0.0488(17) 0.0019(16) -0.0097(16) 0.0041(18) C11 0.0460(17) 0.0558(19) 0.0516(17) 0.0034(15) 0.0001(14) 0.0058(16) C12 0.0483(18) 0.067(2) 0.0543(17) 0.0000(17) -0.0080(15) -0.0020(17) C13 0.059(2) 0.067(2) 0.0509(18) 0.0091(17) -0.0101(15) 0.0006(19) C14 0.106(4) 0.067(3) 0.093(3) 0.009(2) 0.014(3) 0.021(3) C15 0.115(5) 0.129(6) 0.279(10) 0.066(6) 0.059(6) 0.017(5) C16 0.192(7) 0.120(5) 0.159(6) -0.036(4) -0.005(6) 0.063(6) C17A 0.183(7) 0.131(5) 0.105(4) 0.048(4) -0.068(4) -0.018(6) C18A 0.163(16) 0.128(14) 0.105(10) -0.031(9) -0.061(12) -0.016(12) C19A 0.155(17) 0.166(13) 0.122(14) 0.075(11) -0.075(11) -0.031(12) C17B 0.183(7) 0.131(5) 0.105(4) 0.048(4) -0.068(4) -0.018(6) C18B 0.158(13) 0.144(14) 0.125(12) 0.040(10) -0.062(10) -0.045(11) C19B 0.118(10) 0.119(8) 0.077(7) 0.048(6) -0.022(6) -0.032(7) C20 0.106(4) 0.104(4) 0.087(3) 0.009(3) 0.000(3) 0.047(3) C21 0.184(7) 0.122(5) 0.139(5) -0.016(4) 0.013(5) 0.058(5) C22 0.125(5) 0.179(7) 0.164(6) 0.018(6) 0.048(5) 0.039(5) C23 0.0470(18) 0.058(2) 0.0522(16) 0.0012(15) -0.0009(15) 0.0042(16) C24 0.0520(18) 0.072(2) 0.071(2) 0.022(2) -0.0073(17) -0.0074(19) C25 0.075(3) 0.069(3) 0.083(3) 0.012(2) -0.005(2) -0.015(2) C26 0.105(4) 0.092(3) 0.142(5) -0.047(3) 0.007(3) 0.003(3) C27 0.066(2) 0.083(3) 0.075(2) 0.024(2) -0.008(2) -0.007(2) C28 0.069(2) 0.078(3) 0.063(2) 0.015(2) -0.0123(19) -0.014(2) C29 0.094(3) 0.094(3) 0.110(4) 0.005(3) -0.003(3) -0.034(3) C30 0.136(5) 0.091(4) 0.123(4) -0.002(3) -0.001(4) -0.035(4) C31 0.134(5) 0.091(4) 0.114(4) -0.020(3) -0.022(4) 0.007(4) C32 0.083(3) 0.108(4) 0.135(4) -0.028(4) 0.010(3) -0.006(3) C33 0.077(3) 0.081(3) 0.098(3) -0.004(3) 0.006(2) -0.024(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C23 1.334(4) . ? N1 C24 1.445(5) . ? N1 HN1 0.91(4) . ? O1 C7 1.224(5) . ? O2 C23 1.224(4) . ? O3 C25 1.191(5) . ? O4 C25 1.291(6) . ? O4 C26 1.435(6) . ? C1 C2 1.379(6) . ? C1 C6 1.399(5) . ? C1 C14 1.492(6) . ? C2 C3 1.369(7) . ? C2 H2 0.9300 . ? C3 C4 1.371(7) . ? C3 C17A 1.490(5) . ? C4 C5 1.411(6) . ? C4 H4 0.9300 . ? C5 C6 1.379(5) . ? C5 C20 1.519(6) . ? C6 C7 1.501(5) . ? C7 C8 1.473(5) . ? C8 C13 1.383(5) . ? C8 C9 1.388(4) . ? C9 C10 1.376(5) . ? C9 H9 0.9300 . ? C10 C11 1.382(5) . ? C10 H10 0.9300 . ? C11 C12 1.391(4) . ? C11 C23 1.481(5) . ? C12 C13 1.362(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.504(8) . ? C14 C16 1.519(8) . ? C14 H14 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17A C18A 1.473(9) . ? C17A C19A 1.479(9) . ? C17A H17A 0.9800 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C19A H19A 0.9600 . ? C19A H19B 0.9600 . ? C19A H19C 0.9600 . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? C19B H19D 0.9600 . ? C19B H19E 0.9600 . ? C19B H19F 0.9600 . ? C17B C18B 1.492(9) . ? C17B C19B 1.440(8) . ? C17B H17B 0.9800 . ? C20 C21 1.501(8) . ? C20 C22 1.517(9) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C24 C25 1.511(6) . ? C24 C27 1.524(5) . ? C24 H24 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.489(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.375(5) . ? C28 C33 1.383(5) . ? C29 C30 1.370(6) . ? C29 H29 0.9300 . ? C30 C31 1.377(6) . ? C30 H30 0.9300 . ? C31 C32 1.362(5) . ? C31 H31 0.9300 . ? C32 C33 1.373(5) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 N1 C24 122.2(3) . . ? C23 N1 HN1 117(2) . . ? C24 N1 HN1 121(2) . . ? C25 O4 C26 118.4(4) . . ? C2 C1 C6 117.4(4) . . ? C2 C1 C14 121.1(4) . . ? C6 C1 C14 121.5(4) . . ? C3 C2 C1 123.7(4) . . ? C3 C2 H2 118.2 . . ? C1 C2 H2 118.2 . . ? C2 C3 C4 117.2(4) . . ? C2 C3 C17A 120.0(5) . . ? C4 C3 C17A 122.8(5) . . ? C3 C4 C5 122.6(4) . . ? C3 C4 H4 118.7 . . ? C5 C4 H4 118.7 . . ? C6 C5 C4 117.3(4) . . ? C6 C5 C20 121.6(3) . . ? C4 C5 C20 121.1(4) . . ? C5 C6 C1 121.7(3) . . ? C5 C6 C7 119.5(3) . . ? C1 C6 C7 118.8(3) . . ? O1 C7 C8 121.2(3) . . ? O1 C7 C6 120.3(3) . . ? C8 C7 C6 118.5(3) . . ? C13 C8 C9 118.5(3) . . ? C13 C8 C7 121.5(3) . . ? C9 C8 C7 120.0(3) . . ? C10 C9 C8 120.0(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 121.3(3) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C12 118.3(3) . . ? C10 C11 C23 124.2(3) . . ? C12 C11 C23 117.5(3) . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C8 121.5(3) . . ? C12 C13 H13 119.2 . . ? C8 C13 H13 119.2 . . ? C1 C14 C15 111.0(4) . . ? C1 C14 C16 112.9(5) . . ? C15 C14 C16 112.1(6) . . ? C1 C14 H14 106.8 . . ? C15 C14 H14 106.8 . . ? C16 C14 H14 106.8 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18A C17A C19A 124.5(10) . . ? C18A C17A C3 113.0(9) . . ? C19A C17A C3 111.2(8) . . ? C18A C17A H17A 101.3 . . ? C19A C17A H17A 101.3 . . ? C3 C17A H17A 101.3 . . ? C17A C18A H18A 109.5 . . ? C17A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C17A C19A H19A 109.5 . . ? C17A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C17A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? H18D C18B H18E 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? H19D C19B H19E 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C18B C17B C19B 117.5(9) . . ? C18B C17B C3 115.2(7) . . ? C19B C17B C3 117.0(7) . . ? C21 C20 C22 111.5(6) . . ? C21 C20 C5 111.4(5) . . ? C22 C20 C5 111.7(5) . . ? C21 C20 H20 107.3 . . ? C22 C20 H20 107.3 . . ? C5 C20 H20 107.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O2 C23 N1 122.4(3) . . ? O2 C23 C11 120.9(3) . . ? N1 C23 C11 116.7(3) . . ? N1 C24 C25 111.5(3) . . ? N1 C24 C27 111.2(3) . . ? C25 C24 C27 110.9(3) . . ? N1 C24 H24 107.7 . . ? C25 C24 H24 107.7 . . ? C27 C24 H24 107.7 . . ? O3 C25 O4 122.9(5) . . ? O3 C25 C24 124.6(4) . . ? O4 C25 C24 112.6(4) . . ? O4 C26 H26A 109.5 . . ? O4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C24 112.1(3) . . ? C28 C27 H27A 109.2 . . ? C24 C27 H27A 109.2 . . ? C28 C27 H27B 109.2 . . ? C24 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C29 C28 C33 117.2(4) . . ? C29 C28 C27 120.9(4) . . ? C33 C28 C27 121.8(4) . . ? C30 C29 C28 121.3(5) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 C31 121.0(5) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C32 C31 C30 118.1(5) . . ? C32 C31 H31 120.9 . . ? C30 C31 H31 120.9 . . ? C31 C32 C33 121.2(5) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C32 C33 C28 121.2(4) . . ? C32 C33 H33 119.4 . . ? C28 C33 H33 119.4 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.192 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.031 #===END data_15.0%P _database_code_depnum_ccdc_archive 'CCDC 799254' #TrackingRef '- 1.cif' #==================================================================== # start Validation Reply Form _vrf_PLAT201_15.0%P ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 18 RESPONSE: In the crystal there are reactant and photoproduct molecules. Part of atoms were refined isotropically in order to decrease a large number of the parameters in the refinement. ; # end Validation Reply Form #==================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 N O4' _chemical_formula_weight 513.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.3750(15) _cell_length_b 10.7698(19) _cell_length_c 29.857(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3014.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 3.8 _cell_measurement_theta_max 13.3 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14671 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3006 _reflns_number_gt 2156 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSALIS (Oxford Diffraction, 2003)' _computing_cell_refinement 'CRYSALIS (Oxford Diffraction, 2003)' _computing_data_reduction 'CRYSALIS (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Owing to a reactant-product disorder, the following weak restraints from SHELXL97 were applied: DFIX, DANG and SIMU. DFIX and DANG restrained bond lengths and valence angles to target values. The target values were taken from the structures of the pure reactant and the pure product of crystal 1a. SIMU restrained displacement parameters of atoms of the products. ; _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^)+(0.1284P)^2^+0.2660P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration syn _refine_ls_number_reflns 3006 _refine_ls_number_parameters 384 _refine_ls_number_restraints 300 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0725 _refine_ls_wR_factor_ref 0.2170 _refine_ls_wR_factor_gt 0.1971 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.110 _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 N1R N 0.7371(6) 0.2990(5) -0.0053(2) 0.0634(16) Uani 0.850(6) 1 d PDU A 1 H1R H 0.6517 0.2708 -0.0078 0.076 Uiso 0.850(6) 1 calc PR A 1 O1R O 0.5351(9) -0.2522(6) 0.1041(2) 0.092(2) Uani 0.850(6) 1 d PDU A 1 O2R O 0.9451(5) 0.2832(5) 0.03117(19) 0.0630(14) Uani 0.850(6) 1 d PDU A 1 O3R O 0.7730(6) 0.6167(5) -0.0087(3) 0.127(2) Uani 0.850(6) 1 d PDU A 1 O4R O 0.5741(5) 0.5088(5) -0.0079(2) 0.0904(17) Uani 0.850(6) 1 d PDU A 1 C1R C 0.6488(6) -0.1892(6) 0.20133(16) 0.0661(15) Uiso 0.850(6) 1 d PDU A 1 C2R C 0.7186(7) -0.2202(6) 0.24055(19) 0.0777(17) Uiso 0.850(6) 1 d PDU A 1 H2R H 0.6791 -0.1962 0.2678 0.093 Uiso 0.850(6) 1 calc PR A 1 C3R C 0.8453(7) -0.2856(6) 0.24052(18) 0.0804(18) Uiso 0.850(6) 1 d PDU A 1 C4R C 0.9014(8) -0.3203(7) 0.2003(2) 0.088(2) Uiso 0.850(6) 1 d PDU A 1 H4R H 0.9872 -0.3635 0.2001 0.106 Uiso 0.850(6) 1 calc PR A 1 C5R C 0.8340(7) -0.2929(6) 0.15871(18) 0.0743(18) Uiso 0.850(6) 1 d PDU A 1 C6R C 0.7080(6) -0.2262(6) 0.16058(16) 0.0610(16) Uiso 0.850(6) 1 d PDU A 1 C7R C 0.6365(5) -0.1912(4) 0.11752(16) 0.0572(13) Uani 0.850(6) 1 d PDU A 1 C8R C 0.6860(6) -0.0812(5) 0.09258(18) 0.0515(15) Uiso 0.850(6) 1 d PD A 1 C9R C 0.6328(6) -0.0560(5) 0.04994(18) 0.0571(14) Uiso 0.850(6) 1 d PDU A 1 H9R H 0.5684 -0.1104 0.0366 0.069 Uiso 0.850(6) 1 calc PR A 1 C10R C 0.6757(7) 0.0499(6) 0.0274(2) 0.0581(17) Uiso 0.850(6) 1 d PDU A 1 H10R H 0.6394 0.0664 -0.0010 0.070 Uiso 0.850(6) 1 calc PR A 1 C11R C 0.7725(7) 0.1317(6) 0.04665(19) 0.053(2) Uiso 0.850(6) 1 d PDU A 1 C12R C 0.8243(6) 0.1070(6) 0.08917(18) 0.0546(19) Uiso 0.850(6) 1 d PDU A 1 H12R H 0.8850 0.1631 0.1032 0.066 Uiso 0.850(6) 1 calc PR A 1 C13R C 0.7854(7) -0.0009(6) 0.1106(2) 0.063(2) Uiso 0.850(6) 1 d PDU A 1 H13R H 0.8273 -0.0203 0.1379 0.076 Uiso 0.850(6) 1 calc PR A 1 C14R C 0.5154(6) -0.1160(5) 0.2040(2) 0.0834(19) Uani 0.850(6) 1 d PDU A 1 H14R H 0.4931 -0.0880 0.1736 0.100 Uiso 0.850(6) 1 calc PR A 1 C15R C 0.3930(9) -0.1949(10) 0.2193(4) 0.158(4) Uani 0.850(6) 1 d PDU A 1 H15A H 0.3080 -0.1453 0.2207 0.237 Uiso 0.850(6) 1 calc PR A 1 H15B H 0.4134 -0.2279 0.2485 0.237 Uiso 0.850(6) 1 calc PR A 1 H15C H 0.3792 -0.2619 0.1986 0.237 Uiso 0.850(6) 1 calc PR A 1 C16R C 0.5308(12) -0.0001(8) 0.2329(3) 0.145(4) Uani 0.850(6) 1 d PDU A 1 H16A H 0.4425 0.0450 0.2329 0.218 Uiso 0.850(6) 1 calc PR A 1 H16B H 0.6052 0.0515 0.2210 0.218 Uiso 0.850(6) 1 calc PR A 1 H16C H 0.5544 -0.0238 0.2630 0.218 Uiso 0.850(6) 1 calc PR A 1 C17R C 0.9181(10) -0.3131(8) 0.2845(2) 0.112(3) Uani 0.850(6) 1 d PDU A 1 H17R H 0.8441 -0.2817 0.3048 0.135 Uiso 0.850(6) 1 calc PR A 1 C18R C 1.0326(13) -0.2283(10) 0.2969(4) 0.167(5) Uani 0.850(6) 1 d PDU A 1 H18A H 1.0134 -0.1476 0.2846 0.251 Uiso 0.850(6) 1 calc PR A 1 H18B H 1.1214 -0.2588 0.2853 0.251 Uiso 0.850(6) 1 calc PR A 1 H18C H 1.0383 -0.2226 0.3289 0.251 Uiso 0.850(6) 1 calc PR A 1 C19R C 0.9169(12) -0.4373(8) 0.2979(3) 0.139(4) Uani 0.850(6) 1 d PDU A 1 H19A H 0.8368 -0.4788 0.2846 0.209 Uiso 0.850(6) 1 calc PR A 1 H19B H 0.9096 -0.4417 0.3300 0.209 Uiso 0.850(6) 1 calc PR A 1 H19C H 1.0035 -0.4768 0.2884 0.209 Uiso 0.850(6) 1 calc PR A 1 C20R C 0.9051(9) -0.3272(9) 0.1150(2) 0.105(3) Uani 0.850(6) 1 d PDU A 1 H20R H 0.8466 -0.2917 0.0909 0.126 Uiso 0.850(6) 1 calc PR A 1 C21R C 0.9060(14) -0.4656(9) 0.1081(4) 0.140(4) Uani 0.850(6) 1 d PDU A 1 H21A H 0.9427 -0.4842 0.0788 0.211 Uiso 0.850(6) 1 calc PR A 1 H21B H 0.8105 -0.4971 0.1107 0.211 Uiso 0.850(6) 1 calc PR A 1 H21C H 0.9653 -0.5038 0.1304 0.211 Uiso 0.850(6) 1 calc PR A 1 C22R C 1.0534(11) -0.2728(12) 0.1100(4) 0.150(4) Uani 0.850(6) 1 d PDU A 1 H22A H 1.0493 -0.1845 0.1142 0.226 Uiso 0.850(6) 1 calc PR A 1 H22B H 1.0892 -0.2906 0.0805 0.226 Uiso 0.850(6) 1 calc PR A 1 H22C H 1.1156 -0.3087 0.1320 0.226 Uiso 0.850(6) 1 calc PR A 1 C23R C 0.8263(6) 0.2435(8) 0.0229(3) 0.0511(19) Uani 0.850(6) 1 d PD A 1 C24R C 0.7782(6) 0.4044(6) -0.0318(2) 0.0648(16) Uani 0.850(6) 1 d PD A 1 H24R H 0.8819 0.4136 -0.0291 0.078 Uiso 0.850(6) 1 calc PR A 1 C25R C 0.7108(6) 0.5218(5) -0.0139(2) 0.0743(17) Uani 0.850(6) 1 d PDU A 1 C26R C 0.4933(10) 0.6137(8) 0.0071(4) 0.106(3) Uani 0.850(6) 1 d PDU A 1 H26A H 0.5452 0.6563 0.0302 0.159 Uiso 0.850(6) 1 calc PR A 1 H26B H 0.4034 0.5860 0.0188 0.159 Uiso 0.850(6) 1 calc PR A 1 H26C H 0.4771 0.6692 -0.0175 0.159 Uiso 0.850(6) 1 calc PR A 1 C27R C 0.7438(7) 0.3862(6) -0.08097(19) 0.0736(16) Uani 0.850(6) 1 d PDU A 1 H27A H 0.6422 0.3722 -0.0844 0.088 Uiso 0.850(6) 1 calc PR A 1 H27B H 0.7683 0.4611 -0.0973 0.088 Uiso 0.850(6) 1 calc PR A 1 C28R C 0.8232(5) 0.2793(4) -0.10026(16) 0.0690(15) Uiso 0.850(6) 1 d PGDU A 1 C29R C 0.7650(4) 0.1621(5) -0.10012(18) 0.091(2) Uiso 0.850(6) 1 d PGD A 1 H29R H 0.6741 0.1503 -0.0884 0.109 Uiso 0.850(6) 1 d PG A 1 C30R C 0.8383(6) 0.0623(4) -0.1169(2) 0.115(3) Uiso 0.850(6) 1 d PGU A 1 H30R H 0.7966 -0.0161 -0.1162 0.138 Uiso 0.850(6) 1 d PG A 1 C31R C 0.9726(6) 0.0763(4) -0.1348(2) 0.108(2) Uiso 0.850(6) 1 d PG A 1 H31R H 1.0230 0.0084 -0.1457 0.129 Uiso 0.850(6) 1 d PG A 1 C32R C 1.0295(5) 0.1926(5) -0.13618(17) 0.104(2) Uiso 0.850(6) 1 d PG A 1 H32R H 1.1191 0.2044 -0.1489 0.125 Uiso 0.850(6) 1 d PG A 1 C33R C 0.9571(5) 0.2928(4) -0.11914(17) 0.086(2) Uiso 0.850(6) 1 d PGDU A 1 H33R H 0.9987 0.3711 -0.1203 0.104 Uiso 0.850(6) 1 d PG A 1 N1P N 0.731(3) 0.273(3) -0.0133(10) 0.063(9) Uiso 0.150(6) 1 d PDU A 2 H1P H 0.6450 0.2469 -0.0152 0.075 Uiso 0.150(6) 1 calc PR A 2 O1P O 0.527(4) -0.253(3) 0.1123(10) 0.076(9) Uiso 0.150(6) 1 d PDU A 2 O2P O 0.943(3) 0.258(3) 0.0203(10) 0.050(7) Uiso 0.150(6) 1 d PDU A 2 O3P O 0.742(4) 0.594(2) -0.0463(12) 0.126(9) Uiso 0.150(6) 1 d PDU A 2 O4P O 0.610(4) 0.485(3) 0.0019(12) 0.104(10) Uiso 0.150(6) 1 d PDU A 2 C1P C 0.697(2) -0.188(2) 0.2013(5) 0.057(7) Uiso 0.150(6) 1 d PDU A 2 C2P C 0.773(2) -0.223(2) 0.2388(5) 0.061(6) Uiso 0.150(6) 1 d PDU A 2 H2P H 0.7412 -0.2029 0.2674 0.073 Uiso 0.150(6) 1 calc PR A 2 C3P C 0.899(2) -0.288(2) 0.2321(6) 0.050(6) Uiso 0.150(6) 1 d PDU A 2 C4P C 0.942(3) -0.319(3) 0.1899(6) 0.074(7) Uiso 0.150(6) 1 d PDU A 2 H4P H 1.0200 -0.3709 0.1865 0.089 Uiso 0.150(6) 1 calc PR A 2 C5P C 0.873(2) -0.275(3) 0.1515(6) 0.061(9) Uiso 0.150(6) 1 d PDU A 2 C6P C 0.740(2) -0.224(2) 0.1598(5) 0.048(7) Uiso 0.150(6) 1 d PDU A 2 C7P C 0.6147(18) -0.1671(18) 0.1347(5) 0.065(5) Uiso 0.150(6) 1 d PDU A 2 C8P C 0.663(3) -0.065(2) 0.1024(7) 0.065(12) Uiso 0.150(6) 1 d PD A 2 C9P C 0.604(2) -0.0502(18) 0.0613(6) 0.036(6) Uiso 0.150(6) 1 d PDU A 2 H9P H 0.5264 -0.0993 0.0532 0.043 Uiso 0.150(6) 1 calc PR A 2 C10P C 0.655(3) 0.036(2) 0.0310(7) 0.047(7) Uiso 0.150(6) 1 d PDU A 2 H10P H 0.6128 0.0440 0.0030 0.056 Uiso 0.150(6) 1 calc PR A 2 C11P C 0.769(3) 0.110(2) 0.0420(8) 0.043(10) Uiso 0.150(6) 1 d PDU A 2 C12P C 0.836(2) 0.084(3) 0.0822(7) 0.045(9) Uiso 0.150(6) 1 d PDU A 2 H12P H 0.9288 0.1116 0.0870 0.055 Uiso 0.150(6) 1 calc PR A 2 C13P C 0.767(3) 0.019(3) 0.1148(7) 0.050(8) Uiso 0.150(6) 1 d PDU A 2 H13P H 0.7898 0.0314 0.1449 0.061 Uiso 0.150(6) 1 calc PR A 2 C14P C 0.555(2) -0.136(3) 0.1858(7) 0.110(10) Uiso 0.150(6) 1 d PDU A 2 C15P C 0.426(3) -0.216(5) 0.1968(13) 0.155(12) Uiso 0.150(6) 1 d PDU A 2 H15D H 0.4422 -0.2993 0.1865 0.232 Uiso 0.150(6) 1 calc PR A 2 H15E H 0.3427 -0.1830 0.1821 0.232 Uiso 0.150(6) 1 calc PR A 2 H15F H 0.4104 -0.2168 0.2286 0.232 Uiso 0.150(6) 1 calc PR A 2 C16P C 0.528(5) -0.004(3) 0.1991(14) 0.150(11) Uiso 0.150(6) 1 d PDU A 2 H16D H 0.4440 0.0263 0.1844 0.225 Uiso 0.150(6) 1 calc PR A 2 H16E H 0.6085 0.0463 0.1904 0.225 Uiso 0.150(6) 1 calc PR A 2 H16F H 0.5156 0.0011 0.2309 0.225 Uiso 0.150(6) 1 calc PR A 2 C17P C 0.975(3) -0.348(3) 0.2723(7) 0.092(10) Uiso 0.150(6) 1 d PDU A 2 H17P H 0.9133 -0.3331 0.2982 0.111 Uiso 0.150(6) 1 calc PR A 2 C18P C 1.109(5) -0.283(5) 0.2825(19) 0.158(13) Uiso 0.150(6) 1 d PDU A 2 H18D H 1.0952 -0.1950 0.2799 0.237 Uiso 0.150(6) 1 calc PR A 2 H18E H 1.1816 -0.3089 0.2617 0.237 Uiso 0.150(6) 1 calc PR A 2 H18F H 1.1389 -0.3029 0.3124 0.237 Uiso 0.150(6) 1 calc PR A 2 C19P C 0.989(6) -0.481(3) 0.2685(17) 0.143(11) Uiso 0.150(6) 1 d PDU A 2 H19D H 0.8959 -0.5176 0.2660 0.215 Uiso 0.150(6) 1 calc PR A 2 H19E H 1.0359 -0.5131 0.2947 0.215 Uiso 0.150(6) 1 calc PR A 2 H19F H 1.0441 -0.5011 0.2424 0.215 Uiso 0.150(6) 1 calc PR A 2 C20P C 0.909(4) -0.325(4) 0.1054(7) 0.114(11) Uiso 0.150(6) 1 d PDU A 2 H20P H 0.8595 -0.2746 0.0830 0.136 Uiso 0.150(6) 1 calc PR A 2 C21P C 0.861(8) -0.458(5) 0.100(3) 0.14(2) Uiso 0.150(6) 1 d PDU A 2 H21D H 0.8895 -0.4882 0.0709 0.213 Uiso 0.150(6) 1 calc PR A 2 H21E H 0.7592 -0.4626 0.1025 0.213 Uiso 0.150(6) 1 calc PR A 2 H21F H 0.9043 -0.5087 0.1226 0.213 Uiso 0.150(6) 1 calc PR A 2 C22P C 1.067(5) -0.316(7) 0.0965(19) 0.138(18) Uiso 0.150(6) 1 d PDU A 2 H22D H 1.0855 -0.3363 0.0658 0.206 Uiso 0.150(6) 1 calc PR A 2 H22E H 1.1165 -0.3737 0.1156 0.206 Uiso 0.150(6) 1 calc PR A 2 H22F H 1.0987 -0.2334 0.1027 0.206 Uiso 0.150(6) 1 calc PR A 2 C23P C 0.819(4) 0.219(4) 0.0162(15) 0.06(2) Uiso 0.150(6) 1 d PD A 2 C24P C 0.775(3) 0.3736(19) -0.0418(7) 0.072(15) Uiso 0.150(6) 1 d PD A 2 H24P H 0.8784 0.3837 -0.0380 0.086 Uiso 0.150(6) 1 calc PR A 2 C25P C 0.707(4) 0.4947(19) -0.0298(10) 0.074(9) Uiso 0.150(6) 1 d PDU A 2 C26P C 0.542(6) 0.596(5) 0.0179(18) 0.115(18) Uiso 0.150(6) 1 d PDU A 2 H26D H 0.5210 0.5873 0.0491 0.172 Uiso 0.150(6) 1 calc PR A 2 H26E H 0.4555 0.6096 0.0015 0.172 Uiso 0.150(6) 1 calc PR A 2 H26F H 0.6049 0.6657 0.0136 0.172 Uiso 0.150(6) 1 calc PR A 2 C27P C 0.748(3) 0.344(2) -0.0908(7) 0.065(9) Uiso 0.150(6) 1 d PDU A 2 H27C H 0.6491 0.3191 -0.0942 0.078 Uiso 0.150(6) 1 calc PR A 2 H27D H 0.7619 0.4190 -0.1082 0.078 Uiso 0.150(6) 1 calc PR A 2 C28P C 0.8394(18) 0.2456(16) -0.1094(6) 0.039(5) Uiso 0.150(6) 1 d PGDU A 2 C29P C 0.788(2) 0.1286(18) -0.1169(9) 0.088(11) Uiso 0.150(6) 1 d PGD A 2 H29P H 0.6904 0.1138 -0.1151 0.106 Uiso 0.150(6) 1 d PG A 2 C30P C 0.879(3) 0.0325(15) -0.1272(11) 0.086(10) Uiso 0.150(6) 1 d PGU A 2 H30P H 0.8424 -0.0470 -0.1312 0.104 Uiso 0.150(6) 1 d PG A 2 C31P C 1.023(3) 0.052(2) -0.1316(10) 0.130(19) Uiso 0.150(6) 1 d PG A 2 H31P H 1.0837 -0.0132 -0.1392 0.156 Uiso 0.150(6) 1 d PG A 2 C32P C 1.0741(19) 0.169(2) -0.1247(10) 0.084(11) Uiso 0.150(6) 1 d PG A 2 H32P H 1.1713 0.1842 -0.1277 0.101 Uiso 0.150(6) 1 d PG A 2 C33P C 0.9840(19) 0.2646(18) -0.1134(8) 0.062(8) Uiso 0.150(6) 1 d PGDU A 2 H33P H 1.0213 0.3434 -0.1083 0.074 Uiso 0.150(6) 1 d PG 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 N1R 0.049(3) 0.067(3) 0.075(3) 0.015(3) -0.008(2) -0.012(2) O1R 0.118(4) 0.077(3) 0.082(3) 0.020(3) -0.028(3) -0.032(3) O2R 0.050(2) 0.071(3) 0.068(3) -0.004(3) -0.0073(19) -0.002(2) O3R 0.114(4) 0.084(3) 0.182(6) -0.005(4) 0.017(4) -0.033(3) O4R 0.067(3) 0.082(3) 0.123(4) -0.024(3) -0.005(3) 0.000(3) C7R 0.065(3) 0.053(3) 0.054(3) -0.004(2) 0.002(2) 0.004(3) C14R 0.095(4) 0.065(3) 0.090(4) 0.002(3) 0.025(4) 0.022(4) C15R 0.099(6) 0.130(7) 0.244(12) 0.047(8) 0.053(7) 0.017(6) C16R 0.170(9) 0.127(7) 0.138(7) -0.035(6) -0.008(7) 0.059(7) C17R 0.130(7) 0.121(6) 0.086(5) 0.036(5) -0.033(5) 0.008(6) C18R 0.198(11) 0.163(9) 0.141(8) 0.036(7) -0.084(8) -0.062(9) C19R 0.173(8) 0.130(7) 0.114(6) 0.050(6) -0.067(6) -0.021(7) C20R 0.107(6) 0.123(6) 0.086(5) 0.004(5) 0.006(4) 0.050(5) C21R 0.165(11) 0.126(7) 0.130(8) -0.015(6) 0.009(8) 0.057(8) C22R 0.126(7) 0.192(12) 0.133(8) -0.007(8) 0.053(6) 0.035(8) C23R 0.044(4) 0.058(4) 0.051(3) -0.002(4) -0.001(2) 0.002(2) C24R 0.054(3) 0.068(4) 0.073(3) 0.018(3) -0.012(3) -0.012(3) C25R 0.079(4) 0.075(4) 0.069(4) 0.007(3) -0.004(3) -0.016(3) C26R 0.102(6) 0.086(5) 0.130(7) -0.037(5) -0.005(5) 0.005(5) C27R 0.068(4) 0.076(4) 0.078(4) 0.013(4) -0.009(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1R C23R 1.329(5) . ? N1R C24R 1.436(5) . ? N1R H1R 0.8600 . ? O1R C7R 1.222(6) . ? O2R C23R 1.218(6) . ? O3R C25R 1.188(6) . ? O4R C25R 1.301(6) . ? O4R C26R 1.433(7) . ? C1R C2R 1.382(6) . ? C1R C6R 1.395(6) . ? C1R C14R 1.481(6) . ? C2R C3R 1.381(7) . ? C2R H2R 0.9300 . ? C3R C4R 1.362(7) . ? C3R C17R 1.510(6) . ? C4R C5R 1.425(6) . ? C4R H4R 0.9300 . ? C5R C6R 1.384(6) . ? C5R C20R 1.512(7) . ? C6R C7R 1.498(6) . ? C7R C8R 1.474(5) . ? C8R C13R 1.380(6) . ? C8R C9R 1.394(6) . ? C9R C10R 1.384(6) . ? C9R H9R 0.9300 . ? C10R C11R 1.390(6) . ? C10R H10R 0.9300 . ? C11R C12R 1.385(6) . ? C11R C23R 1.486(6) . ? C12R C13R 1.375(6) . ? C12R H12R 0.9300 . ? C13R H13R 0.9300 . ? C14R C15R 1.499(7) . ? C14R C16R 1.523(8) . ? C14R H14R 0.9800 . ? C15R H15A 0.9600 . ? C15R H15B 0.9600 . ? C15R H15C 0.9600 . ? C16R H16A 0.9600 . ? C16R H16B 0.9600 . ? C16R H16C 0.9600 . ? C17R C19R 1.396(8) . ? C17R C18R 1.457(8) . ? C17R H17R 0.9800 . ? C18R H18A 0.9600 . ? C18R H18B 0.9600 . ? C18R H18C 0.9600 . ? C19R H19A 0.9600 . ? C19R H19B 0.9600 . ? C19R H19C 0.9600 . ? C20R C21R 1.504(8) . ? C20R C22R 1.517(8) . ? C20R H20R 0.9800 . ? C21R H21A 0.9600 . ? C21R H21B 0.9600 . ? C21R H21C 0.9600 . ? C22R H22A 0.9600 . ? C22R H22B 0.9600 . ? C22R H22C 0.9600 . ? C24R C25R 1.511(7) . ? C24R C27R 1.516(7) . ? C24R H24R 0.9800 . ? C26R H26A 0.9600 . ? C26R H26B 0.9600 . ? C26R H26C 0.9600 . ? C27R C28R 1.488(6) . ? C27R H27A 0.9700 . ? C27R H27B 0.9700 . ? C28R C29R 1.3753 . ? C28R C33R 1.3832 . ? C29R C30R 1.3702 . ? C29R H29R 0.9300 . ? C30R C31R 1.3771 . ? C30R H30R 0.9300 . ? C31R C32R 1.3616 . ? C31R H31R 0.9300 . ? C32R C33R 1.3726 . ? C32R H32R 0.9300 . ? C33R H33R 0.9300 . ? N1P C23P 1.342(10) . ? N1P C24P 1.435(10) . ? N1P H1P 0.8600 . ? O1P C7P 1.409(10) . ? O2P C23P 1.235(10) . ? O3P C25P 1.220(10) . ? O4P C25P 1.314(10) . ? O4P C26P 1.435(11) . ? C1P C6P 1.355(9) . ? C1P C2P 1.376(9) . ? C1P C14P 1.526(9) . ? C2P C3P 1.388(9) . ? C2P H2P 0.9300 . ? C3P C4P 1.364(9) . ? C3P C17P 1.540(9) . ? C4P C5P 1.397(9) . ? C4P H4P 0.9300 . ? C5P C6P 1.386(9) . ? C5P C20P 1.520(10) . ? C6P C7P 1.520(9) . ? C7P C8P 1.526(9) . ? C7P C14P 1.664(10) . ? C8P C9P 1.358(9) . ? C8P C13P 1.388(9) . ? C9P C10P 1.384(10) . ? C9P H9P 0.9300 . ? C10P C11P 1.368(9) . ? C10P H10P 0.9300 . ? C11P C12P 1.383(9) . ? C11P C23P 1.480(9) . ? C12P C13P 1.362(10) . ? C12P H12P 0.9300 . ? C13P H13P 0.9300 . ? C14P C16P 1.496(10) . ? C14P C15P 1.523(10) . ? C15P H15D 0.9600 . ? C15P H15E 0.9600 . ? C15P H15F 0.9600 . ? C16P H16D 0.9600 . ? C16P H16E 0.9600 . ? C16P H16F 0.9600 . ? C17P C19P 1.448(10) . ? C17P C18P 1.466(10) . ? C17P H17P 0.9800 . ? C18P H18D 0.9600 . ? C18P H18E 0.9600 . ? C18P H18F 0.9600 . ? C19P H19D 0.9600 . ? C19P H19E 0.9600 . ? C19P H19F 0.9600 . ? C20P C22P 1.503(10) . ? C20P C21P 1.510(11) . ? C20P H20P 0.9800 . ? C21P H21D 0.9600 . ? C21P H21E 0.9600 . ? C21P H21F 0.9600 . ? C22P H22D 0.9600 . ? C22P H22E 0.9600 . ? C22P H22F 0.9600 . ? C24P C25P 1.496(10) . ? C24P C27P 1.521(10) . ? C24P H24P 0.9800 . ? C26P H26D 0.9600 . ? C26P H26E 0.9600 . ? C26P H26F 0.9600 . ? C27P C28P 1.471(9) . ? C27P H27C 0.9700 . ? C27P H27D 0.9700 . ? C28P C29P 1.3688 . ? C28P C33P 1.3759 . ? C29P C30P 1.3762 . ? C29P H29P 0.9300 . ? C30P C31P 1.3693 . ? C30P H30P 0.9300 . ? C31P C32P 1.3674 . ? C31P H31P 0.9300 . ? C32P C33P 1.3744 . ? C32P H32P 0.9300 . ? C33P H33P 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23R N1R C24R 122.4(5) . . ? C23R N1R H1R 118.8 . . ? C24R N1R H1R 118.8 . . ? C25R O4R C26R 118.6(6) . . ? C2R C1R C6R 118.8(5) . . ? C2R C1R C14R 118.8(5) . . ? C6R C1R C14R 122.4(5) . . ? C3R C2R C1R 122.0(5) . . ? C3R C2R H2R 119.0 . . ? C1R C2R H2R 119.0 . . ? C4R C3R C2R 118.2(5) . . ? C4R C3R C17R 122.6(6) . . ? C2R C3R C17R 119.2(6) . . ? C3R C4R C5R 122.7(6) . . ? C3R C4R H4R 118.6 . . ? C5R C4R H4R 118.6 . . ? C6R C5R C4R 116.8(5) . . ? C6R C5R C20R 122.5(5) . . ? C4R C5R C20R 120.5(5) . . ? C5R C6R C1R 121.5(4) . . ? C5R C6R C7R 118.5(4) . . ? C1R C6R C7R 119.9(5) . . ? O1R C7R C8R 120.8(5) . . ? O1R C7R C6R 119.6(5) . . ? C8R C7R C6R 119.6(4) . . ? C13R C8R C9R 118.4(4) . . ? C13R C8R C7R 121.3(4) . . ? C9R C8R C7R 120.3(4) . . ? C10R C9R C8R 120.0(4) . . ? C10R C9R H9R 120.0 . . ? C8R C9R H9R 120.0 . . ? C9R C10R C11R 120.7(5) . . ? C9R C10R H10R 119.6 . . ? C11R C10R H10R 119.6 . . ? C12R C11R C10R 119.1(5) . . ? C12R C11R C23R 118.3(5) . . ? C10R C11R C23R 122.6(5) . . ? C13R C12R C11R 119.7(5) . . ? C13R C12R H12R 120.1 . . ? C11R C12R H12R 120.1 . . ? C12R C13R C8R 121.8(5) . . ? C12R C13R H13R 119.1 . . ? C8R C13R H13R 119.1 . . ? C1R C14R C15R 111.2(5) . . ? C1R C14R C16R 112.8(6) . . ? C15R C14R C16R 111.4(7) . . ? C1R C14R H14R 107.0 . . ? C15R C14R H14R 107.0 . . ? C16R C14R H14R 107.0 . . ? C14R C15R H15A 109.5 . . ? C14R C15R H15B 109.5 . . ? H15A C15R H15B 109.5 . . ? C14R C15R H15C 109.5 . . ? H15A C15R H15C 109.5 . . ? H15B C15R H15C 109.5 . . ? C14R C16R H16A 109.5 . . ? C14R C16R H16B 109.5 . . ? H16A C16R H16B 109.5 . . ? C14R C16R H16C 109.5 . . ? H16A C16R H16C 109.5 . . ? H16B C16R H16C 109.5 . . ? C19R C17R C18R 122.3(7) . . ? C19R C17R C3R 115.7(6) . . ? C18R C17R C3R 115.5(6) . . ? C19R C17R H17R 98.6 . . ? C18R C17R H17R 98.6 . . ? C3R C17R H17R 98.6 . . ? C17R C18R H18A 109.5 . . ? C17R C18R H18B 109.5 . . ? H18A C18R H18B 109.5 . . ? C17R C18R H18C 109.5 . . ? H18A C18R H18C 109.5 . . ? H18B C18R H18C 109.5 . . ? C17R C19R H19A 109.5 . . ? C17R C19R H19B 109.5 . . ? H19A C19R H19B 109.5 . . ? C17R C19R H19C 109.5 . . ? H19A C19R H19C 109.5 . . ? H19B C19R H19C 109.5 . . ? C21R C20R C5R 111.2(7) . . ? C21R C20R C22R 111.4(7) . . ? C5R C20R C22R 113.2(7) . . ? C21R C20R H20R 106.9 . . ? C5R C20R H20R 106.9 . . ? C22R C20R H20R 106.9 . . ? C20R C21R H21A 109.5 . . ? C20R C21R H21B 109.5 . . ? H21A C21R H21B 109.5 . . ? C20R C21R H21C 109.5 . . ? H21A C21R H21C 109.5 . . ? H21B C21R H21C 109.5 . . ? C20R C22R H22A 109.5 . . ? C20R C22R H22B 109.5 . . ? H22A C22R H22B 109.5 . . ? C20R C22R H22C 109.5 . . ? H22A C22R H22C 109.5 . . ? H22B C22R H22C 109.5 . . ? O2R C23R N1R 123.1(5) . . ? O2R C23R C11R 119.8(4) . . ? N1R C23R C11R 117.0(5) . . ? N1R C24R C25R 110.8(5) . . ? N1R C24R C27R 112.0(5) . . ? C25R C24R C27R 111.1(4) . . ? N1R C24R H24R 107.6 . . ? C25R C24R H24R 107.6 . . ? C27R C24R H24R 107.6 . . ? O3R C25R O4R 123.9(6) . . ? O3R C25R C24R 124.2(6) . . ? O4R C25R C24R 111.8(5) . . ? C28R C27R C24R 111.6(5) . . ? C28R C27R H27A 109.3 . . ? C24R C27R H27A 109.3 . . ? C28R C27R H27B 109.3 . . ? C24R C27R H27B 109.3 . . ? H27A C27R H27B 108.0 . . ? C29R C28R C33R 117.2 . . ? C29R C28R C27R 120.7(4) . . ? C33R C28R C27R 122.0(4) . . ? C30R C29R C28R 121.3 . . ? C29R C30R C31R 121.0 . . ? C32R C31R C30R 118.1 . . ? C31R C32R C33R 121.2 . . ? C32R C33R C28R 121.2 . . ? C23P N1P C24P 122.8(17) . . ? C23P N1P H1P 118.6 . . ? C24P N1P H1P 118.6 . . ? C25P O4P C26P 118.8(18) . . ? C6P C1P C2P 121.1(11) . . ? C6P C1P C14P 94.9(8) . . ? C2P C1P C14P 143.0(12) . . ? C1P C2P C3P 117.2(11) . . ? C1P C2P H2P 121.4 . . ? C3P C2P H2P 121.4 . . ? C4P C3P C2P 120.5(11) . . ? C4P C3P C17P 118.9(12) . . ? C2P C3P C17P 119.7(12) . . ? C3P C4P C5P 122.6(12) . . ? C3P C4P H4P 118.7 . . ? C5P C4P H4P 118.7 . . ? C6P C5P C4P 113.9(11) . . ? C6P C5P C20P 120.5(14) . . ? C4P C5P C20P 121.3(14) . . ? C1P C6P C5P 122.7(10) . . ? C1P C6P C7P 96.5(8) . . ? C5P C6P C7P 139.9(11) . . ? O1P C7P C6P 115.0(15) . . ? O1P C7P C8P 110.3(12) . . ? C6P C7P C8P 111.8(12) . . ? O1P C7P C14P 111.7(13) . . ? C6P C7P C14P 83.6(7) . . ? C8P C7P C14P 122.2(17) . . ? C9P C8P C13P 116.8(10) . . ? C9P C8P C7P 122.4(11) . . ? C13P C8P C7P 120.8(11) . . ? C8P C9P C10P 121.9(12) . . ? C8P C9P H9P 119.1 . . ? C10P C9P H9P 119.1 . . ? C11P C10P C9P 120.4(12) . . ? C11P C10P H10P 119.8 . . ? C9P C10P H10P 119.8 . . ? C10P C11P C12P 116.4(10) . . ? C10P C11P C23P 125.8(12) . . ? C12P C11P C23P 117.7(12) . . ? C13P C12P C11P 120.6(13) . . ? C13P C12P H12P 119.7 . . ? C11P C12P H12P 119.7 . . ? C12P C13P C8P 118.7(13) . . ? C12P C13P H13P 120.7 . . ? C8P C13P H13P 120.7 . . ? C16P C14P C15P 110.7(13) . . ? C16P C14P C1P 114.7(14) . . ? C15P C14P C1P 114.9(14) . . ? C16P C14P C7P 119.5(14) . . ? C15P C14P C7P 110.5(13) . . ? C1P C14P C7P 84.5(7) . . ? C14P C15P H15D 109.5 . . ? C14P C15P H15E 109.5 . . ? H15D C15P H15E 109.5 . . ? C14P C15P H15F 109.5 . . ? H15D C15P H15F 109.5 . . ? H15E C15P H15F 109.5 . . ? C14P C16P H16D 109.5 . . ? C14P C16P H16E 109.5 . . ? H16D C16P H16E 109.5 . . ? C14P C16P H16F 109.5 . . ? H16D C16P H16F 109.5 . . ? H16E C16P H16F 109.5 . . ? C19P C17P C18P 114.3(16) . . ? C19P C17P C3P 113.1(15) . . ? C18P C17P C3P 111.4(15) . . ? C19P C17P H17P 105.7 . . ? C18P C17P H17P 105.7 . . ? C3P C17P H17P 105.7 . . ? C17P C18P H18D 109.5 . . ? C17P C18P H18E 109.5 . . ? H18D C18P H18E 109.5 . . ? C17P C18P H18F 109.5 . . ? H18D C18P H18F 109.5 . . ? H18E C18P H18F 109.5 . . ? C17P C19P H19D 109.5 . . ? C17P C19P H19E 109.5 . . ? H19D C19P H19E 109.5 . . ? C17P C19P H19F 109.5 . . ? H19D C19P H19F 109.5 . . ? H19E C19P H19F 109.5 . . ? C22P C20P C21P 109.5(15) . . ? C22P C20P C5P 110.9(15) . . ? C21P C20P C5P 111.7(16) . . ? C22P C20P H20P 108.2 . . ? C21P C20P H20P 108.2 . . ? C5P C20P H20P 108.2 . . ? C20P C21P H21D 109.5 . . ? C20P C21P H21E 109.5 . . ? H21D C21P H21E 109.5 . . ? C20P C21P H21F 109.5 . . ? H21D C21P H21F 109.5 . . ? H21E C21P H21F 109.5 . . ? C20P C22P H22D 109.5 . . ? C20P C22P H22E 109.5 . . ? H22D C22P H22E 109.5 . . ? C20P C22P H22F 109.5 . . ? H22D C22P H22F 109.5 . . ? H22E C22P H22F 109.5 . . ? O2P C23P N1P 119.2(14) . . ? O2P C23P C11P 121.4(14) . . ? N1P C23P C11P 119.4(12) . . ? N1P C24P C25P 113.1(15) . . ? N1P C24P C27P 111.4(15) . . ? C25P C24P C27P 110.0(14) . . ? N1P C24P H24P 107.4 . . ? C25P C24P H24P 107.4 . . ? C27P C24P H24P 107.4 . . ? O3P C25P O4P 122.9(15) . . ? O3P C25P C24P 123.4(15) . . ? O4P C25P C24P 113.6(13) . . ? O4P C26P H26D 109.5 . . ? O4P C26P H26E 109.5 . . ? H26D C26P H26E 109.5 . . ? O4P C26P H26F 109.5 . . ? H26D C26P H26F 109.5 . . ? H26E C26P H26F 109.5 . . ? C28P C27P C24P 114.7(14) . . ? C28P C27P H27C 108.6 . . ? C24P C27P H27C 108.6 . . ? C28P C27P H27D 108.6 . . ? C24P C27P H27D 108.6 . . ? H27C C27P H27D 107.6 . . ? C29P C28P C33P 118.1 . . ? C29P C28P C27P 121.3(11) . . ? C33P C28P C27P 120.0(11) . . ? C28P C29P C30P 120.7 . . ? C28P C29P H29P 119.7 . . ? C30P C29P H29P 119.7 . . ? C31P C30P C29P 121.2 . . ? C31P C30P H30P 119.4 . . ? C29P C30P H30P 119.4 . . ? C32P C31P C30P 118.1 . . ? C32P C31P H31P 120.9 . . ? C30P C31P H31P 120.9 . . ? C31P C32P C33P 120.9 . . ? C31P C32P H32P 119.6 . . ? C33P C32P H32P 119.6 . . ? C32P C33P C28P 121.0 . . ? C32P C33P H33P 119.5 . . ? C28P C33P H33P 119.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.212 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.041 #===END data_21.6%P _database_code_depnum_ccdc_archive 'CCDC 799255' #TrackingRef '- 1.cif' #==================================================================== # start Validation Reply Form _vrf_PLAT201_21.6%P ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 18 RESPONSE: In the crystal there are reactant and photoproduct molecules. Part of atoms were refined isotropically in order to decrease a large number of the parameters in the refinement. ; # end Validation Reply Form #==================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 N O4' _chemical_formula_weight 513.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.3769(13) _cell_length_b 10.8131(18) _cell_length_c 29.707(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3012.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 3.8 _cell_measurement_theta_max 13.3 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14655 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3005 _reflns_number_gt 2025 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSALIS (Oxford Diffraction, 2003)' _computing_cell_refinement 'CRYSALIS (Oxford Diffraction, 2003)' _computing_data_reduction 'CRYSALIS (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Owing to a reactant-product disorder, the following weak restraints from SHELXL97 were applied: DFIX, DANG and SIMU. DFIX and DANG restrained bond lengths and valence angles to target values. The target values were taken from the structures of the pure reactant and the pure product of crystal 1a. SIMU restrained displacement parameters of atoms of the products. ; _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^)+(0.1442P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration syn _refine_ls_number_reflns 3005 _refine_ls_number_parameters 384 _refine_ls_number_restraints 296 _refine_ls_R_factor_all 0.1057 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2411 _refine_ls_wR_factor_gt 0.2152 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1R N 0.7346(7) 0.2993(7) -0.0047(3) 0.072(2) Uani 0.784(7) 1 d PD A 1 H1R H 0.6486 0.2722 -0.0067 0.086 Uiso 0.784(7) 1 calc PR A 1 O1R O 0.5312(12) -0.2526(9) 0.1044(3) 0.099(3) Uani 0.784(7) 1 d PDU A 1 O2R O 0.9414(5) 0.2835(6) 0.0322(2) 0.0679(16) Uani 0.784(7) 1 d PDU A 1 O3R O 0.7681(7) 0.6158(6) -0.0097(3) 0.142(3) Uani 0.784(7) 1 d PDU A 1 O4R O 0.5716(6) 0.5067(6) -0.0071(3) 0.098(2) Uani 0.784(7) 1 d PDU A 1 C1R C 0.6474(8) -0.1904(7) 0.20147(19) 0.071(2) Uiso 0.784(7) 1 d PD A 1 C2R C 0.7144(8) -0.2252(7) 0.2412(2) 0.085(2) Uiso 0.784(7) 1 d PDU A 1 H2R H 0.6719 -0.2057 0.2685 0.102 Uiso 0.784(7) 1 calc PR A 1 C3R C 0.8427(8) -0.2880(7) 0.2410(2) 0.086(2) Uiso 0.784(7) 1 d PDU A 1 C4R C 0.8994(9) -0.3211(10) 0.2004(2) 0.093(2) Uiso 0.784(7) 1 d PDU A 1 H4R H 0.9821 -0.3686 0.2001 0.112 Uiso 0.784(7) 1 calc PR A 1 C5R C 0.8376(8) -0.2863(9) 0.1586(2) 0.080(3) Uiso 0.784(7) 1 d PD A 1 C6R C 0.7061(9) -0.2274(9) 0.16037(19) 0.072(3) Uiso 0.784(7) 1 d PDU A 1 C7R C 0.6335(7) -0.1911(5) 0.1175(2) 0.0637(17) Uani 0.784(7) 1 d PD A 1 C8R C 0.6824(7) -0.0812(5) 0.0926(2) 0.0610(19) Uiso 0.784(7) 1 d PD A 1 C9R C 0.6302(7) -0.0566(6) 0.0495(2) 0.0664(19) Uiso 0.784(7) 1 d PDU A 1 H9R H 0.5672 -0.1112 0.0358 0.080 Uiso 0.784(7) 1 calc PR A 1 C10R C 0.6732(9) 0.0503(7) 0.0273(3) 0.068(3) Uiso 0.784(7) 1 d PDU A 1 H10R H 0.6373 0.0674 -0.0012 0.082 Uiso 0.784(7) 1 calc PR A 1 C11R C 0.7690(9) 0.1321(7) 0.0471(2) 0.062(3) Uiso 0.784(7) 1 d PDU A 1 C12R C 0.8213(8) 0.1067(7) 0.0897(2) 0.059(3) Uiso 0.784(7) 1 d PD A 1 H12R H 0.8815 0.1625 0.1040 0.071 Uiso 0.784(7) 1 calc PR A 1 C13R C 0.7830(8) -0.0027(7) 0.1106(2) 0.072(2) Uiso 0.784(7) 1 d PDU A 1 H13R H 0.8264 -0.0238 0.1377 0.086 Uiso 0.784(7) 1 calc PR A 1 C14R C 0.5159(8) -0.1156(6) 0.2042(3) 0.096(2) Uani 0.784(7) 1 d PDU A 1 H14R H 0.4936 -0.0890 0.1735 0.115 Uiso 0.784(7) 1 calc PR A 1 C15R C 0.3927(10) -0.1931(11) 0.2198(6) 0.176(6) Uani 0.784(7) 1 d PDU A 1 H15A H 0.3082 -0.1431 0.2210 0.264 Uiso 0.784(7) 1 calc PR A 1 H15B H 0.4129 -0.2256 0.2491 0.264 Uiso 0.784(7) 1 calc PR A 1 H15C H 0.3782 -0.2601 0.1991 0.264 Uiso 0.784(7) 1 calc PR A 1 C16R C 0.5330(14) 0.0013(9) 0.2323(4) 0.160(5) Uani 0.784(7) 1 d PDU A 1 H16A H 0.4449 0.0466 0.2323 0.240 Uiso 0.784(7) 1 calc PR A 1 H16B H 0.6070 0.0518 0.2196 0.240 Uiso 0.784(7) 1 calc PR A 1 H16C H 0.5578 -0.0207 0.2626 0.240 Uiso 0.784(7) 1 calc PR A 1 C17R C 0.9161(11) -0.3133(8) 0.2851(3) 0.111(3) Uani 0.784(7) 1 d PDU A 1 H17R H 0.8422 -0.2833 0.3057 0.133 Uiso 0.784(7) 1 calc PR A 1 C18R C 1.0303(16) -0.2275(11) 0.2968(4) 0.165(6) Uani 0.784(7) 1 d PDU A 1 H18A H 1.0097 -0.1475 0.2843 0.247 Uiso 0.784(7) 1 calc PR A 1 H18B H 1.1189 -0.2573 0.2848 0.247 Uiso 0.784(7) 1 calc PR A 1 H18C H 1.0374 -0.2211 0.3289 0.247 Uiso 0.784(7) 1 calc PR A 1 C19R C 0.9179(13) -0.4393(9) 0.2978(4) 0.136(4) Uani 0.784(7) 1 d PDU A 1 H19A H 0.8379 -0.4810 0.2845 0.204 Uiso 0.784(7) 1 calc PR A 1 H19B H 0.9124 -0.4456 0.3300 0.204 Uiso 0.784(7) 1 calc PR A 1 H19C H 1.0047 -0.4769 0.2875 0.204 Uiso 0.784(7) 1 calc PR A 1 C20R C 0.9050(10) -0.3237(9) 0.1143(3) 0.113(3) Uani 0.784(7) 1 d PDU A 1 H20R H 0.8452 -0.2892 0.0904 0.135 Uiso 0.784(7) 1 calc PR A 1 C21R C 0.9037(15) -0.4620(9) 0.1085(5) 0.136(4) Uani 0.784(7) 1 d PDU A 1 H21A H 0.9402 -0.4827 0.0792 0.204 Uiso 0.784(7) 1 calc PR A 1 H21B H 0.8077 -0.4920 0.1112 0.204 Uiso 0.784(7) 1 calc PR A 1 H21C H 0.9622 -0.4996 0.1312 0.204 Uiso 0.784(7) 1 calc PR A 1 C22R C 1.0521(13) -0.2692(13) 0.1084(5) 0.149(5) Uani 0.784(7) 1 d PDU A 1 H22A H 1.0478 -0.1813 0.1126 0.224 Uiso 0.784(7) 1 calc PR A 1 H22B H 1.0861 -0.2870 0.0786 0.224 Uiso 0.784(7) 1 calc PR A 1 H22C H 1.1158 -0.3047 0.1301 0.224 Uiso 0.784(7) 1 calc PR A 1 C23R C 0.8239(8) 0.2426(9) 0.0232(3) 0.060(2) Uani 0.784(7) 1 d PDU A 1 C24R C 0.7754(7) 0.4036(6) -0.0314(2) 0.0717(18) Uani 0.784(7) 1 d PDU A 1 H24R H 0.8789 0.4132 -0.0285 0.086 Uiso 0.784(7) 1 calc PR A 1 C25R C 0.7073(7) 0.5209(6) -0.0139(3) 0.083(2) Uani 0.784(7) 1 d PDU A 1 C26R C 0.4911(12) 0.6112(10) 0.0082(5) 0.116(3) Uani 0.784(7) 1 d PDU A 1 H26A H 0.5290 0.6396 0.0364 0.174 Uiso 0.784(7) 1 calc PR A 1 H26B H 0.3932 0.5876 0.0121 0.174 Uiso 0.784(7) 1 calc PR A 1 H26C H 0.4972 0.6763 -0.0137 0.174 Uiso 0.784(7) 1 calc PR A 1 C27R C 0.7427(7) 0.3855(7) -0.0811(2) 0.0787(19) Uani 0.784(7) 1 d PDU A 1 H27A H 0.6410 0.3728 -0.0849 0.094 Uiso 0.784(7) 1 calc PR A 1 H27B H 0.7688 0.4598 -0.0975 0.094 Uiso 0.784(7) 1 calc PR A 1 C28R C 0.8206(5) 0.2783(5) -0.10047(19) 0.0750(18) Uiso 0.784(7) 1 d PGDU A 1 C29R C 0.7621(5) 0.1617(5) -0.1005(2) 0.097(2) Uiso 0.784(7) 1 d PGD A 1 H29R H 0.6707 0.1501 -0.0891 0.116 Uiso 0.784(7) 1 d PG A 1 C30R C 0.8358(7) 0.0621(4) -0.1170(2) 0.124(3) Uiso 0.784(7) 1 d PG A 1 H30R H 0.7939 -0.0159 -0.1165 0.149 Uiso 0.784(7) 1 d PG A 1 C31R C 0.9709(7) 0.0758(5) -0.1345(2) 0.113(3) Uiso 0.784(7) 1 d PG A 1 H31R H 1.0216 0.0080 -0.1452 0.136 Uiso 0.784(7) 1 d PG A 1 C32R C 1.0281(6) 0.1915(6) -0.1357(2) 0.114(3) Uiso 0.784(7) 1 d PG A 1 H32R H 1.1182 0.2030 -0.1481 0.137 Uiso 0.784(7) 1 d PG A 1 C33R C 0.9552(6) 0.2914(5) -0.1189(2) 0.094(2) Uiso 0.784(7) 1 d PGDU A 1 H33R H 0.9971 0.3693 -0.1199 0.112 Uiso 0.784(7) 1 d PG A 1 N1P N 0.733(3) 0.2709(19) -0.0141(7) 0.058(9) Uiso 0.216(7) 1 d PD A 2 H1P H 0.6489 0.2410 -0.0173 0.070 Uiso 0.216(7) 1 calc PR A 2 O1P O 0.518(4) -0.248(3) 0.1097(9) 0.092(8) Uiso 0.216(7) 1 d PDU A 2 O2P O 0.943(2) 0.259(2) 0.0201(7) 0.058(7) Uiso 0.216(7) 1 d PDU A 2 O3P O 0.739(3) 0.5889(18) -0.0497(10) 0.141(9) Uiso 0.216(7) 1 d PDU A 2 O4P O 0.610(3) 0.482(3) 0.0004(10) 0.113(9) Uiso 0.216(7) 1 d PDU A 2 C1P C 0.685(2) -0.189(2) 0.2012(5) 0.087(12) Uiso 0.216(7) 1 d PD A 2 C2P C 0.765(2) -0.2141(19) 0.2390(5) 0.067(6) Uiso 0.216(7) 1 d PDU A 2 H2P H 0.7401 -0.1833 0.2671 0.080 Uiso 0.216(7) 1 calc PR A 2 C3P C 0.885(2) -0.288(2) 0.2327(5) 0.073(6) Uiso 0.216(7) 1 d PDU A 2 C4P C 0.921(2) -0.327(3) 0.1904(6) 0.084(7) Uiso 0.216(7) 1 d PDU A 2 H4P H 1.0098 -0.3640 0.1864 0.101 Uiso 0.216(7) 1 calc PR A 2 C5P C 0.832(2) -0.313(2) 0.1529(5) 0.077(11) Uiso 0.216(7) 1 d PD A 2 C6P C 0.725(2) -0.228(2) 0.1598(5) 0.060(10) Uiso 0.216(7) 1 d PDU A 2 C7P C 0.6059(16) -0.1658(15) 0.1337(5) 0.072(9) Uiso 0.216(7) 1 d PD A 2 C8P C 0.659(2) -0.0625(17) 0.1032(6) 0.067(8) Uiso 0.216(7) 1 d PD A 2 C9P C 0.6044(18) -0.0484(15) 0.0610(5) 0.044(5) Uiso 0.216(7) 1 d PDU A 2 H9P H 0.5285 -0.0980 0.0520 0.053 Uiso 0.216(7) 1 calc PR A 2 C10P C 0.658(2) 0.038(2) 0.0310(6) 0.062(10) Uiso 0.216(7) 1 d PDU A 2 H10P H 0.6197 0.0438 0.0023 0.075 Uiso 0.216(7) 1 calc PR A 2 C11P C 0.769(2) 0.113(2) 0.0433(7) 0.046(8) Uiso 0.216(7) 1 d PDU A 2 C12P C 0.832(2) 0.088(2) 0.0842(7) 0.068(13) Uiso 0.216(7) 1 d PD A 2 H12P H 0.9221 0.1192 0.0900 0.082 Uiso 0.216(7) 1 calc PR A 2 C13P C 0.765(2) 0.0189(19) 0.1163(6) 0.054(6) Uiso 0.216(7) 1 d PDU A 2 H13P H 0.7903 0.0263 0.1465 0.065 Uiso 0.216(7) 1 calc PR A 2 C14P C 0.5437(18) -0.135(2) 0.1848(6) 0.105(9) Uiso 0.216(7) 1 d PDU A 2 C15P C 0.411(3) -0.212(4) 0.1941(12) 0.172(18) Uiso 0.216(7) 1 d PDU A 2 H15D H 0.4270 -0.2955 0.1840 0.258 Uiso 0.216(7) 1 calc PR A 2 H15E H 0.3314 -0.1775 0.1784 0.258 Uiso 0.216(7) 1 calc PR A 2 H15F H 0.3921 -0.2125 0.2259 0.258 Uiso 0.216(7) 1 calc PR A 2 C16P C 0.520(4) -0.002(2) 0.1972(11) 0.140(12) Uiso 0.216(7) 1 d PDU A 2 H16D H 0.4359 0.0278 0.1825 0.210 Uiso 0.216(7) 1 calc PR A 2 H16E H 0.6009 0.0460 0.1878 0.210 Uiso 0.216(7) 1 calc PR A 2 H16F H 0.5090 0.0046 0.2292 0.210 Uiso 0.216(7) 1 calc PR A 2 C17P C 0.961(2) -0.345(2) 0.2735(7) 0.100(9) Uiso 0.216(7) 1 d PDU A 2 H17P H 0.9007 -0.3273 0.2995 0.120 Uiso 0.216(7) 1 calc PR A 2 C18P C 1.097(3) -0.283(3) 0.2824(12) 0.123(13) Uiso 0.216(7) 1 d PDU A 2 H18D H 1.0846 -0.1954 0.2801 0.184 Uiso 0.216(7) 1 calc PR A 2 H18E H 1.1669 -0.3099 0.2608 0.184 Uiso 0.216(7) 1 calc PR A 2 H18F H 1.1293 -0.3038 0.3122 0.184 Uiso 0.216(7) 1 calc PR A 2 C19P C 0.971(5) -0.479(2) 0.2712(14) 0.162(16) Uiso 0.216(7) 1 d PDU A 2 H19D H 0.8770 -0.5134 0.2688 0.244 Uiso 0.216(7) 1 calc PR A 2 H19E H 1.0162 -0.5095 0.2980 0.244 Uiso 0.216(7) 1 calc PR A 2 H19F H 1.0263 -0.5022 0.2454 0.244 Uiso 0.216(7) 1 calc PR A 2 C20P C 0.883(3) -0.350(3) 0.1063(7) 0.114(10) Uiso 0.216(7) 1 d PDU A 2 H20P H 0.8298 -0.3022 0.0838 0.137 Uiso 0.216(7) 1 calc PR A 2 C21P C 0.855(5) -0.486(4) 0.0982(17) 0.143(17) Uiso 0.216(7) 1 d PDU A 2 H21D H 0.8877 -0.5081 0.0685 0.215 Uiso 0.216(7) 1 calc PR A 2 H21E H 0.7551 -0.5027 0.1006 0.215 Uiso 0.216(7) 1 calc PR A 2 H21F H 0.9062 -0.5341 0.1201 0.215 Uiso 0.216(7) 1 calc PR A 2 C22P C 1.040(4) -0.324(4) 0.1011(15) 0.120(13) Uiso 0.216(7) 1 d PDU A 2 H22D H 1.0685 -0.3419 0.0708 0.180 Uiso 0.216(7) 1 calc PR A 2 H22E H 1.0927 -0.3746 0.1216 0.180 Uiso 0.216(7) 1 calc PR A 2 H22F H 1.0575 -0.2383 0.1075 0.180 Uiso 0.216(7) 1 calc PR A 2 C23P C 0.819(3) 0.222(4) 0.0176(14) 0.069(9) Uiso 0.216(7) 1 d PDU A 2 C24P C 0.777(3) 0.3706(15) -0.0428(6) 0.076(8) Uiso 0.216(7) 1 d PDU A 2 H24P H 0.8803 0.3803 -0.0393 0.091 Uiso 0.216(7) 1 calc PR A 2 C25P C 0.709(3) 0.4916(16) -0.0307(8) 0.082(8) Uiso 0.216(7) 1 d PDU A 2 C26P C 0.535(6) 0.591(4) 0.014(2) 0.140(17) Uiso 0.216(7) 1 d PDU A 2 H26D H 0.5089 0.5839 0.0452 0.210 Uiso 0.216(7) 1 calc PR A 2 H26E H 0.4499 0.5994 -0.0038 0.210 Uiso 0.216(7) 1 calc PR A 2 H26F H 0.5943 0.6620 0.0099 0.210 Uiso 0.216(7) 1 calc PR A 2 C27P C 0.748(2) 0.3393(19) -0.0919(6) 0.072(7) Uiso 0.216(7) 1 d PDU A 2 H27C H 0.6489 0.3157 -0.0950 0.086 Uiso 0.216(7) 1 calc PR A 2 H27D H 0.7635 0.4128 -0.1100 0.086 Uiso 0.216(7) 1 calc PR A 2 C28P C 0.8383(16) 0.2388(14) -0.1095(5) 0.052(4) Uiso 0.216(7) 1 d PGDU A 2 C29P C 0.7844(17) 0.1239(15) -0.1186(8) 0.109(10) Uiso 0.216(7) 1 d PGD A 2 H29P H 0.6870 0.1097 -0.1158 0.131 Uiso 0.216(7) 1 d PG A 2 C30P C 0.873(2) 0.0291(13) -0.1318(9) 0.110(10) Uiso 0.216(7) 1 d PG A 2 H30P H 0.8347 -0.0491 -0.1368 0.132 Uiso 0.216(7) 1 d PG A 2 C31P C 1.016(2) 0.0477(18) -0.1377(9) 0.151(16) Uiso 0.216(7) 1 d PG A 2 H31P H 1.0752 -0.0162 -0.1473 0.181 Uiso 0.216(7) 1 d PG A 2 C32P C 1.0698(16) 0.163(2) -0.1292(9) 0.122(12) Uiso 0.216(7) 1 d PG A 2 H32P H 1.1667 0.1777 -0.1332 0.147 Uiso 0.216(7) 1 d PG A 2 C33P C 0.9824(17) 0.2571(16) -0.1150(7) 0.087(8) Uiso 0.216(7) 1 d PGDU A 2 H33P H 1.0214 0.3345 -0.1089 0.104 Uiso 0.216(7) 1 d PG 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 N1R 0.056(3) 0.081(4) 0.078(4) 0.012(4) -0.012(3) -0.013(3) O1R 0.119(5) 0.081(4) 0.098(4) 0.019(3) -0.028(4) -0.034(4) O2R 0.048(3) 0.083(4) 0.073(4) -0.007(3) -0.003(2) 0.001(2) O3R 0.123(5) 0.092(4) 0.210(8) 0.005(5) 0.020(5) -0.043(4) O4R 0.077(4) 0.092(4) 0.126(5) -0.021(3) 0.000(4) -0.003(3) C7R 0.073(4) 0.054(3) 0.064(4) 0.000(3) 0.004(3) 0.011(3) C14R 0.111(5) 0.073(4) 0.102(5) 0.003(4) 0.023(4) 0.024(5) C15R 0.096(6) 0.122(8) 0.310(19) 0.049(11) 0.058(9) 0.012(7) C16R 0.188(11) 0.126(8) 0.167(11) -0.048(7) -0.020(9) 0.059(9) C17R 0.135(7) 0.118(7) 0.079(5) 0.025(5) -0.024(5) 0.025(7) C18R 0.207(13) 0.147(10) 0.141(9) 0.020(8) -0.083(10) -0.051(11) C19R 0.155(9) 0.151(8) 0.102(6) 0.055(7) -0.057(7) -0.026(8) C20R 0.104(6) 0.126(8) 0.107(6) -0.009(5) -0.010(5) 0.053(6) C21R 0.161(11) 0.114(8) 0.134(9) -0.026(6) 0.013(8) 0.038(8) C22R 0.126(8) 0.163(13) 0.160(10) -0.016(10) 0.050(7) 0.013(9) C23R 0.051(4) 0.069(5) 0.061(4) -0.001(4) 0.001(3) 0.004(3) C24R 0.057(3) 0.073(4) 0.085(4) 0.019(4) -0.012(3) -0.012(4) C25R 0.090(5) 0.086(5) 0.073(5) 0.011(4) -0.006(4) -0.015(4) C26R 0.105(7) 0.097(6) 0.146(9) -0.037(6) -0.003(7) 0.003(6) C27R 0.069(4) 0.090(5) 0.077(4) 0.017(4) -0.010(3) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1R C23R 1.327(6) . ? N1R C24R 1.432(6) . ? N1R H1R 0.8600 . ? O1R C7R 1.230(6) . ? O2R C23R 1.218(6) . ? O3R C25R 1.180(7) . ? O4R C25R 1.297(7) . ? O4R C26R 1.432(8) . ? C1R C2R 1.388(7) . ? C1R C6R 1.398(6) . ? C1R C14R 1.477(7) . ? C2R C3R 1.382(7) . ? C2R H2R 0.9300 . ? C3R C4R 1.365(7) . ? C3R C17R 1.506(7) . ? C4R C5R 1.420(7) . ? C4R H4R 0.9300 . ? C5R C6R 1.389(7) . ? C5R C20R 1.515(7) . ? C6R C7R 1.497(6) . ? C7R C8R 1.474(6) . ? C8R C13R 1.378(6) . ? C8R C9R 1.395(6) . ? C9R C10R 1.390(7) . ? C9R H9R 0.9300 . ? C10R C11R 1.390(7) . ? C10R H10R 0.9300 . ? C11R C12R 1.385(6) . ? C11R C23R 1.482(6) . ? C12R C13R 1.384(7) . ? C12R H12R 0.9300 . ? C13R H13R 0.9300 . ? C14R C15R 1.500(8) . ? C14R C16R 1.523(8) . ? C14R H14R 0.9800 . ? C15R H15A 0.9600 . ? C15R H15B 0.9600 . ? C15R H15C 0.9600 . ? C16R H16A 0.9600 . ? C16R H16B 0.9600 . ? C16R H16C 0.9600 . ? C17R C19R 1.414(8) . ? C17R C18R 1.458(8) . ? C17R H17R 0.9800 . ? C18R H18A 0.9600 . ? C18R H18B 0.9600 . ? C18R H18C 0.9600 . ? C19R H19A 0.9600 . ? C19R H19B 0.9600 . ? C19R H19C 0.9600 . ? C20R C21R 1.506(8) . ? C20R C22R 1.510(8) . ? C20R H20R 0.9800 . ? C21R H21A 0.9600 . ? C21R H21B 0.9600 . ? C21R H21C 0.9600 . ? C22R H22A 0.9600 . ? C22R H22B 0.9600 . ? C22R H22C 0.9600 . ? C24R C25R 1.513(7) . ? C24R C27R 1.521(7) . ? C24R H24R 0.9800 . ? C26R H26A 0.9600 . ? C26R H26B 0.9600 . ? C26R H26C 0.9600 . ? C27R C28R 1.486(6) . ? C27R H27A 0.9700 . ? C27R H27B 0.9700 . ? C28R C29R 1.3754 . ? C28R C33R 1.3831 . ? C29R C30R 1.3701 . ? C29R H29R 0.9300 . ? C30R C31R 1.3771 . ? C30R H30R 0.9300 . ? C31R C32R 1.3617 . ? C31R H31R 0.9300 . ? C32R C33R 1.3725 . ? C32R H32R 0.9300 . ? C33R H33R 0.9300 . ? N1P C23P 1.342(9) . ? N1P C24P 1.435(10) . ? N1P H1P 0.8600 . ? O1P C7P 1.409(9) . ? O2P C23P 1.235(10) . ? O3P C25P 1.226(9) . ? O4P C25P 1.313(10) . ? O4P C26P 1.433(10) . ? C1P C6P 1.353(9) . ? C1P C2P 1.376(9) . ? C1P C14P 1.526(9) . ? C2P C3P 1.393(9) . ? C2P H2P 0.9300 . ? C3P C4P 1.368(9) . ? C3P C17P 1.538(9) . ? C4P C5P 1.404(9) . ? C4P H4P 0.9300 . ? C5P C6P 1.379(9) . ? C5P C20P 1.519(9) . ? C6P C7P 1.516(9) . ? C7P C8P 1.519(9) . ? C7P C14P 1.661(9) . ? C8P C9P 1.363(9) . ? C8P C13P 1.385(9) . ? C9P C10P 1.383(9) . ? C9P H9P 0.9300 . ? C10P C11P 1.368(9) . ? C10P H10P 0.9300 . ? C11P C12P 1.377(9) . ? C11P C23P 1.481(9) . ? C12P C13P 1.365(9) . ? C12P H12P 0.9300 . ? C13P H13P 0.9300 . ? C14P C16P 1.498(9) . ? C14P C15P 1.521(10) . ? C15P H15D 0.9600 . ? C15P H15E 0.9600 . ? C15P H15F 0.9600 . ? C16P H16D 0.9600 . ? C16P H16E 0.9600 . ? C16P H16F 0.9600 . ? C17P C19P 1.449(10) . ? C17P C18P 1.464(10) . ? C17P H17P 0.9800 . ? C18P H18D 0.9600 . ? C18P H18E 0.9600 . ? C18P H18F 0.9600 . ? C19P H19D 0.9600 . ? C19P H19E 0.9600 . ? C19P H19F 0.9600 . ? C20P C22P 1.508(10) . ? C20P C21P 1.511(10) . ? C20P H20P 0.9800 . ? C21P H21D 0.9600 . ? C21P H21E 0.9600 . ? C21P H21F 0.9600 . ? C22P H22D 0.9600 . ? C22P H22E 0.9600 . ? C22P H22F 0.9600 . ? C24P C25P 1.497(9) . ? C24P C27P 1.522(10) . ? C24P H24P 0.9800 . ? C26P H26D 0.9600 . ? C26P H26E 0.9600 . ? C26P H26F 0.9600 . ? C27P C28P 1.473(9) . ? C27P H27C 0.9700 . ? C27P H27D 0.9700 . ? C28P C29P 1.3688 . ? C28P C33P 1.3759 . ? C29P C30P 1.3762 . ? C29P H29P 0.9300 . ? C30P C31P 1.3694 . ? C30P H30P 0.9300 . ? C31P C32P 1.3674 . ? C31P H31P 0.9300 . ? C32P C33P 1.3743 . ? C32P H32P 0.9300 . ? C33P H33P 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23R N1R C24R 122.8(6) . . ? C23R N1R H1R 118.6 . . ? C24R N1R H1R 118.6 . . ? C25R O4R C26R 118.2(7) . . ? C2R C1R C6R 119.1(6) . . ? C2R C1R C14R 118.7(6) . . ? C6R C1R C14R 122.3(6) . . ? C3R C2R C1R 121.6(6) . . ? C3R C2R H2R 119.2 . . ? C1R C2R H2R 119.2 . . ? C4R C3R C2R 118.2(5) . . ? C4R C3R C17R 122.9(7) . . ? C2R C3R C17R 118.9(6) . . ? C3R C4R C5R 122.8(6) . . ? C3R C4R H4R 118.6 . . ? C5R C4R H4R 118.6 . . ? C6R C5R C4R 116.8(6) . . ? C6R C5R C20R 121.7(5) . . ? C4R C5R C20R 121.1(6) . . ? C5R C6R C1R 120.9(5) . . ? C5R C6R C7R 119.5(5) . . ? C1R C6R C7R 119.3(6) . . ? O1R C7R C8R 121.3(6) . . ? O1R C7R C6R 118.9(6) . . ? C8R C7R C6R 119.8(6) . . ? C13R C8R C9R 118.7(5) . . ? C13R C8R C7R 121.0(5) . . ? C9R C8R C7R 120.3(5) . . ? C10R C9R C8R 119.4(5) . . ? C10R C9R H9R 120.3 . . ? C8R C9R H9R 120.3 . . ? C11R C10R C9R 121.0(6) . . ? C11R C10R H10R 119.5 . . ? C9R C10R H10R 119.5 . . ? C12R C11R C10R 119.3(5) . . ? C12R C11R C23R 118.3(6) . . ? C10R C11R C23R 122.3(6) . . ? C13R C12R C11R 119.2(6) . . ? C13R C12R H12R 120.4 . . ? C11R C12R H12R 120.4 . . ? C8R C13R C12R 121.9(6) . . ? C8R C13R H13R 119.0 . . ? C12R C13R H13R 119.0 . . ? C1R C14R C15R 110.7(6) . . ? C1R C14R C16R 113.4(7) . . ? C15R C14R C16R 112.1(9) . . ? C1R C14R H14R 106.7 . . ? C15R C14R H14R 106.7 . . ? C16R C14R H14R 106.7 . . ? C14R C15R H15A 109.5 . . ? C14R C15R H15B 109.5 . . ? H15A C15R H15B 109.5 . . ? C14R C15R H15C 109.5 . . ? H15A C15R H15C 109.5 . . ? H15B C15R H15C 109.5 . . ? C14R C16R H16A 109.5 . . ? C14R C16R H16B 109.5 . . ? H16A C16R H16B 109.5 . . ? C14R C16R H16C 109.5 . . ? H16A C16R H16C 109.5 . . ? H16B C16R H16C 109.5 . . ? C19R C17R C18R 122.8(8) . . ? C19R C17R C3R 114.4(7) . . ? C18R C17R C3R 115.3(7) . . ? C19R C17R H17R 99.2 . . ? C18R C17R H17R 99.2 . . ? C3R C17R H17R 99.2 . . ? C17R C18R H18A 109.5 . . ? C17R C18R H18B 109.5 . . ? H18A C18R H18B 109.5 . . ? C17R C18R H18C 109.5 . . ? H18A C18R H18C 109.5 . . ? H18B C18R H18C 109.5 . . ? C17R C19R H19A 109.5 . . ? C17R C19R H19B 109.5 . . ? H19A C19R H19B 109.5 . . ? C17R C19R H19C 109.5 . . ? H19A C19R H19C 109.5 . . ? H19B C19R H19C 109.5 . . ? C21R C20R C22R 112.5(8) . . ? C21R C20R C5R 111.3(7) . . ? C22R C20R C5R 112.3(7) . . ? C21R C20R H20R 106.8 . . ? C22R C20R H20R 106.8 . . ? C5R C20R H20R 106.8 . . ? C20R C21R H21A 109.5 . . ? C20R C21R H21B 109.5 . . ? H21A C21R H21B 109.5 . . ? C20R C21R H21C 109.5 . . ? H21A C21R H21C 109.5 . . ? H21B C21R H21C 109.5 . . ? C20R C22R H22A 109.5 . . ? C20R C22R H22B 109.5 . . ? H22A C22R H22B 109.5 . . ? C20R C22R H22C 109.5 . . ? H22A C22R H22C 109.5 . . ? H22B C22R H22C 109.5 . . ? O2R C23R N1R 122.7(6) . . ? O2R C23R C11R 120.1(5) . . ? N1R C23R C11R 116.9(5) . . ? N1R C24R C25R 110.9(6) . . ? N1R C24R C27R 112.5(6) . . ? C25R C24R C27R 111.0(5) . . ? N1R C24R H24R 107.4 . . ? C25R C24R H24R 107.4 . . ? C27R C24R H24R 107.4 . . ? O3R C25R O4R 124.1(7) . . ? O3R C25R C24R 124.1(7) . . ? O4R C25R C24R 111.6(6) . . ? C28R C27R C24R 112.2(5) . . ? C28R C27R H27A 109.2 . . ? C24R C27R H27A 109.2 . . ? C28R C27R H27B 109.2 . . ? C24R C27R H27B 109.2 . . ? H27A C27R H27B 107.9 . . ? C29R C28R C33R 117.2 . . ? C29R C28R C27R 121.3(4) . . ? C33R C28R C27R 121.4(4) . . ? C30R C29R C28R 121.3 . . ? C29R C30R C31R 121.0 . . ? C32R C31R C30R 118.1 . . ? C31R C32R C33R 121.2 . . ? C32R C33R C28R 121.2 . . ? C23P N1P C24P 122.7(15) . . ? C23P N1P H1P 118.7 . . ? C24P N1P H1P 118.7 . . ? C25P O4P C26P 118.9(18) . . ? C6P C1P C2P 121.9(10) . . ? C6P C1P C14P 94.0(8) . . ? C2P C1P C14P 144.0(11) . . ? C1P C2P C3P 116.5(10) . . ? C1P C2P H2P 121.8 . . ? C3P C2P H2P 121.8 . . ? C4P C3P C2P 120.0(10) . . ? C4P C3P C17P 118.9(11) . . ? C2P C3P C17P 120.2(11) . . ? C3P C4P C5P 123.3(12) . . ? C3P C4P H4P 118.4 . . ? C5P C4P H4P 118.4 . . ? C6P C5P C4P 112.7(11) . . ? C6P C5P C20P 122.8(13) . . ? C4P C5P C20P 120.6(12) . . ? C1P C6P C5P 123.0(10) . . ? C1P C6P C7P 97.1(8) . . ? C5P C6P C7P 139.0(11) . . ? O1P C7P C6P 114.3(14) . . ? O1P C7P C8P 110.8(12) . . ? C6P C7P C8P 112.8(12) . . ? O1P C7P C14P 112.5(13) . . ? C6P C7P C14P 83.0(7) . . ? C8P C7P C14P 120.8(14) . . ? C9P C8P C13P 117.1(10) . . ? C9P C8P C7P 120.6(10) . . ? C13P C8P C7P 122.3(10) . . ? C8P C9P C10P 122.1(11) . . ? C8P C9P H9P 118.9 . . ? C10P C9P H9P 118.9 . . ? C11P C10P C9P 120.5(11) . . ? C11P C10P H10P 119.8 . . ? C9P C10P H10P 119.8 . . ? C10P C11P C12P 116.1(10) . . ? C10P C11P C23P 125.4(12) . . ? C12P C11P C23P 118.4(12) . . ? C13P C12P C11P 122.0(13) . . ? C13P C12P H12P 119.0 . . ? C11P C12P H12P 119.0 . . ? C12P C13P C8P 118.8(12) . . ? C12P C13P H13P 120.6 . . ? C8P C13P H13P 120.6 . . ? C16P C14P C15P 111.2(12) . . ? C16P C14P C1P 114.6(13) . . ? C15P C14P C1P 116.0(14) . . ? C16P C14P C7P 117.9(13) . . ? C15P C14P C7P 110.0(12) . . ? C1P C14P C7P 84.9(7) . . ? C14P C15P H15D 109.5 . . ? C14P C15P H15E 109.5 . . ? H15D C15P H15E 109.5 . . ? C14P C15P H15F 109.5 . . ? H15D C15P H15F 109.5 . . ? H15E C15P H15F 109.5 . . ? C14P C16P H16D 109.5 . . ? C14P C16P H16E 109.5 . . ? H16D C16P H16E 109.5 . . ? C14P C16P H16F 109.5 . . ? H16D C16P H16F 109.5 . . ? H16E C16P H16F 109.5 . . ? C19P C17P C18P 114.3(15) . . ? C19P C17P C3P 113.2(14) . . ? C18P C17P C3P 111.3(14) . . ? C19P C17P H17P 105.7 . . ? C18P C17P H17P 105.7 . . ? C3P C17P H17P 105.7 . . ? C17P C18P H18D 109.5 . . ? C17P C18P H18E 109.5 . . ? H18D C18P H18E 109.5 . . ? C17P C18P H18F 109.5 . . ? H18D C18P H18F 109.5 . . ? H18E C18P H18F 109.5 . . ? C17P C19P H19D 109.5 . . ? C17P C19P H19E 109.5 . . ? H19D C19P H19E 109.5 . . ? C17P C19P H19F 109.5 . . ? H19D C19P H19F 109.5 . . ? H19E C19P H19F 109.5 . . ? C22P C20P C21P 109.4(15) . . ? C22P C20P C5P 110.5(14) . . ? C21P C20P C5P 110.5(15) . . ? C22P C20P H20P 108.8 . . ? C21P C20P H20P 108.8 . . ? C5P C20P H20P 108.8 . . ? C20P C21P H21D 109.5 . . ? C20P C21P H21E 109.5 . . ? H21D C21P H21E 109.5 . . ? C20P C21P H21F 109.5 . . ? H21D C21P H21F 109.5 . . ? H21E C21P H21F 109.5 . . ? C20P C22P H22D 109.5 . . ? C20P C22P H22E 109.5 . . ? H22D C22P H22E 109.5 . . ? C20P C22P H22F 109.5 . . ? H22D C22P H22F 109.5 . . ? H22E C22P H22F 109.5 . . ? O2P C23P N1P 118.6(13) . . ? O2P C23P C11P 121.7(14) . . ? N1P C23P C11P 118.9(11) . . ? N1P C24P C25P 113.1(13) . . ? N1P C24P C27P 110.6(13) . . ? C25P C24P C27P 110.4(12) . . ? N1P C24P H24P 107.5 . . ? C25P C24P H24P 107.5 . . ? C27P C24P H24P 107.5 . . ? O3P C25P O4P 123.6(14) . . ? O3P C25P C24P 122.9(14) . . ? O4P C25P C24P 113.5(12) . . ? O4P C26P H26D 109.5 . . ? O4P C26P H26E 109.5 . . ? H26D C26P H26E 109.5 . . ? O4P C26P H26F 109.5 . . ? H26D C26P H26F 109.5 . . ? H26E C26P H26F 109.5 . . ? C28P C27P C24P 113.8(12) . . ? C28P C27P H27C 108.8 . . ? C24P C27P H27C 108.8 . . ? C28P C27P H27D 108.8 . . ? C24P C27P H27D 108.8 . . ? H27C C27P H27D 107.7 . . ? C29P C28P C33P 118.0 . . ? C29P C28P C27P 121.9(10) . . ? C33P C28P C27P 120.0(10) . . ? C28P C29P C30P 120.7 . . ? C28P C29P H29P 119.7 . . ? C30P C29P H29P 119.7 . . ? C31P C30P C29P 121.2 . . ? C31P C30P H30P 119.4 . . ? C29P C30P H30P 119.4 . . ? C32P C31P C30P 118.1 . . ? C32P C31P H31P 120.9 . . ? C30P C31P H31P 120.9 . . ? C31P C32P C33P 120.9 . . ? C31P C32P H32P 119.6 . . ? C33P C32P H32P 119.6 . . ? C32P C33P C28P 121.0 . . ? C32P C33P H33P 119.5 . . ? C28P C33P H33P 119.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.192 _refine_diff_density_min -0.255 _refine_diff_density_rms 0.040 #===END data_28.6%P _database_code_depnum_ccdc_archive 'CCDC 799256' #TrackingRef '- 1.cif' #==================================================================== # start Validation Reply Form _vrf_PLAT201_28.6%P ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 18 RESPONSE: In the crystal there are reactant and photoproduct molecules. Part of atoms were refined isotropically in order to decrease a large number of the parameters in the refinement. ; # end Validation Reply Form #==================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 N O4' _chemical_formula_weight 513.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.382(2) _cell_length_b 10.864(3) _cell_length_c 29.571(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3014.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 13.3 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14682 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2994 _reflns_number_gt 1900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSALIS (Oxford Diffraction, 2003)' _computing_cell_refinement 'CRYSALIS (Oxford Diffraction, 2003)' _computing_data_reduction 'CRYSALIS (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Owing to a reactant-product disorder, the following weak restraints from SHELXL97 were applied: DFIX, DANG and SIMU. DFIX and DANG restrained bond lengths and valence angles to target values. The target values were taken from the structures of the pure reactant and the pure product of crystal 1a. SIMU restrained displacement parameters of atoms of the products. ; _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^)+(0.1413P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration syn _refine_ls_number_reflns 2994 _refine_ls_number_parameters 384 _refine_ls_number_restraints 301 _refine_ls_R_factor_all 0.1344 _refine_ls_R_factor_gt 0.0873 _refine_ls_wR_factor_ref 0.2658 _refine_ls_wR_factor_gt 0.2281 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.127 _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 N1R N 0.7330(8) 0.2986(8) -0.0046(3) 0.072(2) Uani 0.713(8) 1 d PDU A 1 H1R H 0.6477 0.2706 -0.0071 0.087 Uiso 0.713(8) 1 calc PR A 1 O1R O 0.5320(16) -0.2521(11) 0.1047(4) 0.105(5) Uani 0.713(8) 1 d PDU A 1 O2R O 0.9392(9) 0.2849(11) 0.0325(4) 0.077(3) Uani 0.713(8) 1 d PDU A 1 O3R O 0.7669(9) 0.6140(7) -0.0096(4) 0.143(4) Uani 0.713(8) 1 d PDU A 1 O4R O 0.5702(7) 0.5052(7) -0.0075(3) 0.097(2) Uani 0.713(8) 1 d PDU A 1 C1R C 0.6473(10) -0.1915(10) 0.2018(2) 0.079(4) Uiso 0.713(8) 1 d PDU A 1 C2R C 0.7130(11) -0.2263(10) 0.2418(3) 0.087(3) Uiso 0.713(8) 1 d PD A 1 H2R H 0.6703 -0.2069 0.2693 0.105 Uiso 0.713(8) 1 calc PR A 1 C3R C 0.8399(11) -0.2891(10) 0.2414(3) 0.090(3) Uiso 0.713(8) 1 d PD A 1 C4R C 0.8999(12) -0.3207(14) 0.2006(3) 0.099(5) Uiso 0.713(8) 1 d PD A 1 H4R H 0.9825 -0.3680 0.2004 0.119 Uiso 0.713(8) 1 calc PR A 1 C5R C 0.8398(9) -0.2836(10) 0.1585(3) 0.079(3) Uiso 0.713(8) 1 d PD A 1 C6R C 0.7087(10) -0.2259(12) 0.1604(2) 0.074(5) Uiso 0.713(8) 1 d PDU A 1 C7R C 0.6331(8) -0.1906(7) 0.1175(3) 0.069(2) Uani 0.713(8) 1 d PDU A 1 C8R C 0.6813(9) -0.0806(7) 0.0923(3) 0.065(3) Uiso 0.713(8) 1 d PDU A 1 C9R C 0.6299(9) -0.0551(8) 0.0491(3) 0.069(2) Uiso 0.713(8) 1 d PDU A 1 H9R H 0.5660 -0.1088 0.0353 0.083 Uiso 0.713(8) 1 calc PR A 1 C10R C 0.6738(12) 0.0502(9) 0.0266(3) 0.074(4) Uiso 0.713(8) 1 d PDU A 1 H10R H 0.6396 0.0661 -0.0024 0.089 Uiso 0.713(8) 1 calc PR A 1 C11R C 0.7679(13) 0.1320(9) 0.0467(3) 0.065(4) Uiso 0.713(8) 1 d PDU A 1 C12R C 0.8186(11) 0.1064(9) 0.0900(3) 0.066(3) Uiso 0.713(8) 1 d PDU A 1 H12R H 0.8767 0.1628 0.1049 0.079 Uiso 0.713(8) 1 calc PR A 1 C13R C 0.7825(12) -0.0022(9) 0.1106(3) 0.074(5) Uiso 0.713(8) 1 d PD A 1 H13R H 0.8269 -0.0238 0.1376 0.089 Uiso 0.713(8) 1 calc PR A 1 C14R C 0.5157(9) -0.1152(8) 0.2040(4) 0.096(3) Uani 0.713(8) 1 d PDU A 1 H14R H 0.4930 -0.0901 0.1730 0.115 Uiso 0.713(8) 1 calc PR A 1 C15R C 0.3938(12) -0.1920(13) 0.2205(7) 0.164(6) Uani 0.713(8) 1 d PDU A 1 H15A H 0.3091 -0.1425 0.2218 0.246 Uiso 0.713(8) 1 calc PR A 1 H15B H 0.4153 -0.2230 0.2501 0.246 Uiso 0.713(8) 1 calc PR A 1 H15C H 0.3788 -0.2596 0.2002 0.246 Uiso 0.713(8) 1 calc PR A 1 C16R C 0.5349(17) 0.0021(11) 0.2316(5) 0.165(6) Uani 0.713(8) 1 d PDU A 1 H16A H 0.4472 0.0477 0.2317 0.248 Uiso 0.713(8) 1 calc PR A 1 H16B H 0.6088 0.0514 0.2183 0.248 Uiso 0.713(8) 1 calc PR A 1 H16C H 0.5607 -0.0189 0.2620 0.248 Uiso 0.713(8) 1 calc PR A 1 C17R C 0.9143(13) -0.3139(10) 0.2856(3) 0.113(4) Uani 0.713(8) 1 d PDU A 1 H17R H 0.8402 -0.2854 0.3065 0.135 Uiso 0.713(8) 1 calc PR A 1 C18R C 1.0274(18) -0.2274(14) 0.2975(5) 0.153(6) Uani 0.713(8) 1 d PDU A 1 H18A H 1.0061 -0.1480 0.2850 0.229 Uiso 0.713(8) 1 calc PR A 1 H18B H 1.1165 -0.2563 0.2856 0.229 Uiso 0.713(8) 1 calc PR A 1 H18C H 1.0340 -0.2210 0.3298 0.229 Uiso 0.713(8) 1 calc PR A 1 C19R C 0.9181(16) -0.4402(10) 0.2980(4) 0.130(5) Uani 0.713(8) 1 d PDU A 1 H19A H 0.8381 -0.4821 0.2848 0.194 Uiso 0.713(8) 1 calc PR A 1 H19B H 0.9136 -0.4473 0.3303 0.194 Uiso 0.713(8) 1 calc PR A 1 H19C H 1.0049 -0.4766 0.2873 0.194 Uiso 0.713(8) 1 calc PR A 1 C20R C 0.9045(11) -0.3221(10) 0.1140(3) 0.110(4) Uani 0.713(8) 1 d PDU A 1 H20R H 0.8444 -0.2868 0.0902 0.132 Uiso 0.713(8) 1 calc PR A 1 C21R C 0.9034(19) -0.4594(11) 0.1071(6) 0.144(6) Uani 0.713(8) 1 d PDU A 1 H21A H 0.9404 -0.4783 0.0776 0.216 Uiso 0.713(8) 1 calc PR A 1 H21B H 0.8075 -0.4894 0.1095 0.216 Uiso 0.713(8) 1 calc PR A 1 H21C H 0.9617 -0.4979 0.1297 0.216 Uiso 0.713(8) 1 calc PR A 1 C22R C 1.0529(14) -0.2690(16) 0.1074(7) 0.154(6) Uani 0.713(8) 1 d PDU A 1 H22A H 1.0499 -0.1814 0.1116 0.231 Uiso 0.713(8) 1 calc PR A 1 H22B H 1.0857 -0.2873 0.0774 0.231 Uiso 0.713(8) 1 calc PR A 1 H22C H 1.1168 -0.3047 0.1291 0.231 Uiso 0.713(8) 1 calc PR A 1 C23R C 0.8215(9) 0.2433(9) 0.0236(3) 0.060(3) Uani 0.713(8) 1 d PDU A 1 C24R C 0.7734(9) 0.4038(7) -0.0312(3) 0.076(2) Uani 0.713(8) 1 d PDU A 1 H24R H 0.8769 0.4132 -0.0283 0.091 Uiso 0.713(8) 1 calc PR A 1 C25R C 0.7062(9) 0.5203(8) -0.0131(3) 0.084(3) Uani 0.713(8) 1 d PDU A 1 C26R C 0.4884(13) 0.6086(12) 0.0077(5) 0.114(4) Uani 0.713(8) 1 d PDU A 1 H26A H 0.5148 0.6285 0.0382 0.171 Uiso 0.713(8) 1 calc PR A 1 H26B H 0.3888 0.5885 0.0066 0.171 Uiso 0.713(8) 1 calc PR A 1 H26C H 0.5067 0.6780 -0.0115 0.171 Uiso 0.713(8) 1 calc PR A 1 C27R C 0.7415(9) 0.3845(8) -0.0809(3) 0.081(3) Uani 0.713(8) 1 d PD A 1 H27A H 0.6398 0.3716 -0.0846 0.098 Uiso 0.713(8) 1 calc PR A 1 H27B H 0.7669 0.4585 -0.0974 0.098 Uiso 0.713(8) 1 calc PR A 1 C28R C 0.8192(7) 0.2781(6) -0.1007(2) 0.077(2) Uiso 0.713(8) 1 d PGDU A 1 C29R C 0.7608(6) 0.1620(7) -0.1008(3) 0.094(3) Uiso 0.713(8) 1 d PGD A 1 H29R H 0.6694 0.1505 -0.0894 0.113 Uiso 0.713(8) 1 d PG A 1 C30R C 0.8345(9) 0.0628(6) -0.1173(3) 0.121(4) Uiso 0.713(8) 1 d PG A 1 H30R H 0.7927 -0.0148 -0.1167 0.145 Uiso 0.713(8) 1 d PG A 1 C31R C 0.9696(9) 0.0764(7) -0.1348(3) 0.121(4) Uiso 0.713(8) 1 d PG A 1 H31R H 1.0203 0.0089 -0.1455 0.145 Uiso 0.713(8) 1 d PG A 1 C32R C 1.0268(7) 0.1916(8) -0.1360(3) 0.116(4) Uiso 0.713(8) 1 d PG A 1 H32R H 1.1169 0.2030 -0.1484 0.140 Uiso 0.713(8) 1 d PG A 1 C33R C 0.9538(8) 0.2911(7) -0.1192(3) 0.103(4) Uiso 0.713(8) 1 d PGDU A 1 H33R H 0.9956 0.3687 -0.1203 0.123 Uiso 0.713(8) 1 d PG A 1 N1P N 0.734(3) 0.2670(19) -0.0140(7) 0.082(8) Uiso 0.287(8) 1 d PDU A 2 H1P H 0.6492 0.2372 -0.0167 0.099 Uiso 0.287(8) 1 calc PR A 2 O1P O 0.510(3) -0.246(3) 0.1068(9) 0.099(11) Uiso 0.287(8) 1 d PDU A 2 O2P O 0.940(3) 0.261(3) 0.0240(10) 0.066(7) Uiso 0.287(8) 1 d PDU A 2 O3P O 0.740(3) 0.5846(17) -0.0485(9) 0.145(8) Uiso 0.287(8) 1 d PDU A 2 O4P O 0.617(3) 0.480(2) 0.0036(7) 0.118(8) Uiso 0.287(8) 1 d PDU A 2 C1P C 0.672(2) -0.195(2) 0.2010(5) 0.094(11) Uiso 0.287(8) 1 d PDU A 2 C2P C 0.756(2) -0.215(2) 0.2386(5) 0.086(9) Uiso 0.287(8) 1 d PD A 2 H2P H 0.7327 -0.1820 0.2666 0.103 Uiso 0.287(8) 1 calc PR A 2 C3P C 0.877(2) -0.288(2) 0.2329(6) 0.086(8) Uiso 0.287(8) 1 d PD A 2 C4P C 0.909(3) -0.332(3) 0.1908(6) 0.118(15) Uiso 0.287(8) 1 d PD A 2 H4P H 0.9954 -0.3736 0.1871 0.142 Uiso 0.287(8) 1 calc PR A 2 C5P C 0.820(2) -0.319(2) 0.1530(5) 0.076(8) Uiso 0.287(8) 1 d PD A 2 C6P C 0.710(2) -0.238(2) 0.1595(5) 0.085(14) Uiso 0.287(8) 1 d PDU A 2 C7P C 0.5987(16) -0.1678(14) 0.1326(4) 0.086(8) Uiso 0.287(8) 1 d PDU A 2 C8P C 0.657(2) -0.0652(16) 0.1028(5) 0.070(8) Uiso 0.287(8) 1 d PDU A 2 C9P C 0.6020(17) -0.0464(14) 0.0607(5) 0.051(5) Uiso 0.287(8) 1 d PDU A 2 H9P H 0.5255 -0.0948 0.0515 0.062 Uiso 0.287(8) 1 calc PR A 2 C10P C 0.654(2) 0.0409(18) 0.0311(6) 0.057(8) Uiso 0.287(8) 1 d PDU A 2 H10P H 0.6146 0.0494 0.0024 0.068 Uiso 0.287(8) 1 calc PR A 2 C11P C 0.764(3) 0.115(2) 0.0445(7) 0.058(9) Uiso 0.287(8) 1 d PDU A 2 C12P C 0.827(2) 0.089(2) 0.0855(7) 0.071(7) Uiso 0.287(8) 1 d PDU A 2 H12P H 0.9153 0.1233 0.0921 0.085 Uiso 0.287(8) 1 calc PR A 2 C13P C 0.765(3) 0.014(2) 0.1167(6) 0.073(12) Uiso 0.287(8) 1 d PD A 2 H13P H 0.7935 0.0152 0.1468 0.088 Uiso 0.287(8) 1 calc PR A 2 C14P C 0.5340(16) -0.1376(17) 0.1836(5) 0.092(7) Uiso 0.287(8) 1 d PDU A 2 C15P C 0.399(2) -0.212(3) 0.1915(9) 0.131(12) Uiso 0.287(8) 1 d PDU A 2 H15D H 0.4138 -0.2953 0.1815 0.197 Uiso 0.287(8) 1 calc PR A 2 H15E H 0.3218 -0.1762 0.1748 0.197 Uiso 0.287(8) 1 calc PR A 2 H15F H 0.3764 -0.2120 0.2232 0.197 Uiso 0.287(8) 1 calc PR A 2 C16P C 0.513(3) -0.0052(18) 0.1959(10) 0.132(10) Uiso 0.287(8) 1 d PDU A 2 H16D H 0.4283 0.0253 0.1812 0.197 Uiso 0.287(8) 1 calc PR A 2 H16E H 0.5935 0.0419 0.1861 0.197 Uiso 0.287(8) 1 calc PR A 2 H16F H 0.5020 0.0022 0.2280 0.197 Uiso 0.287(8) 1 calc PR A 2 C17P C 0.956(2) -0.340(2) 0.2743(7) 0.107(9) Uiso 0.287(8) 1 d PDU A 2 H17P H 0.8967 -0.3193 0.3005 0.129 Uiso 0.287(8) 1 calc PR A 2 C18P C 1.092(3) -0.277(3) 0.2819(12) 0.136(13) Uiso 0.287(8) 1 d PDU A 2 H18D H 1.0786 -0.1900 0.2796 0.203 Uiso 0.287(8) 1 calc PR A 2 H18E H 1.1600 -0.3038 0.2596 0.203 Uiso 0.287(8) 1 calc PR A 2 H18F H 1.1271 -0.2972 0.3116 0.203 Uiso 0.287(8) 1 calc PR A 2 C19P C 0.965(4) -0.473(2) 0.2739(14) 0.169(16) Uiso 0.287(8) 1 d PDU A 2 H19D H 0.8704 -0.5072 0.2715 0.254 Uiso 0.287(8) 1 calc PR A 2 H19E H 1.0082 -0.5013 0.3014 0.254 Uiso 0.287(8) 1 calc PR A 2 H19F H 1.0208 -0.4995 0.2486 0.254 Uiso 0.287(8) 1 calc PR A 2 C20P C 0.873(3) -0.356(3) 0.1063(6) 0.114(9) Uiso 0.287(8) 1 d PDU A 2 H20P H 0.8176 -0.3118 0.0834 0.137 Uiso 0.287(8) 1 calc PR A 2 C21P C 0.855(4) -0.493(3) 0.0994(14) 0.130(13) Uiso 0.287(8) 1 d PDU A 2 H21D H 0.8873 -0.5146 0.0697 0.195 Uiso 0.287(8) 1 calc PR A 2 H21E H 0.7560 -0.5137 0.1025 0.195 Uiso 0.287(8) 1 calc PR A 2 H21F H 0.9096 -0.5364 0.1216 0.195 Uiso 0.287(8) 1 calc PR A 2 C22P C 1.029(3) -0.321(4) 0.1012(16) 0.147(14) Uiso 0.287(8) 1 d PDU A 2 H22D H 1.0591 -0.3391 0.0709 0.221 Uiso 0.287(8) 1 calc PR A 2 H22E H 1.0847 -0.3683 0.1221 0.221 Uiso 0.287(8) 1 calc PR A 2 H22F H 1.0404 -0.2353 0.1072 0.221 Uiso 0.287(8) 1 calc PR A 2 C23P C 0.821(3) 0.217(3) 0.0169(10) 0.074(9) Uiso 0.287(8) 1 d PDU A 2 C24P C 0.775(3) 0.3677(15) -0.0426(6) 0.083(7) Uiso 0.287(8) 1 d PDU A 2 H24P H 0.8781 0.3781 -0.0394 0.100 Uiso 0.287(8) 1 calc PR A 2 C25P C 0.707(2) 0.4874(14) -0.0303(7) 0.072(7) Uiso 0.287(8) 1 d PDU A 2 C26P C 0.540(4) 0.588(3) 0.0174(13) 0.136(14) Uiso 0.287(8) 1 d PDU A 2 H26D H 0.4936 0.5725 0.0457 0.204 Uiso 0.287(8) 1 calc PR A 2 H26E H 0.4706 0.6085 -0.0051 0.204 Uiso 0.287(8) 1 calc PR A 2 H26F H 0.6058 0.6554 0.0209 0.204 Uiso 0.287(8) 1 calc PR A 2 C27P C 0.745(2) 0.337(2) -0.0919(6) 0.089(10) Uiso 0.287(8) 1 d PD A 2 H27C H 0.6459 0.3138 -0.0950 0.107 Uiso 0.287(8) 1 calc PR A 2 H27D H 0.7612 0.4096 -0.1101 0.107 Uiso 0.287(8) 1 calc PR A 2 C28P C 0.8344(15) 0.2360(14) -0.1097(5) 0.060(5) Uiso 0.287(8) 1 d PGDU A 2 C29P C 0.7796(16) 0.1222(15) -0.1192(7) 0.114(9) Uiso 0.287(8) 1 d PGD A 2 H29P H 0.6824 0.1080 -0.1158 0.137 Uiso 0.287(8) 1 d PG A 2 C30P C 0.867(2) 0.0284(13) -0.1339(9) 0.140(12) Uiso 0.287(8) 1 d PG A 2 H30P H 0.8281 -0.0490 -0.1392 0.168 Uiso 0.287(8) 1 d PG A 2 C31P C 1.010(2) 0.0471(18) -0.1407(9) 0.161(15) Uiso 0.287(8) 1 d PG A 2 H31P H 1.0677 -0.0161 -0.1512 0.193 Uiso 0.287(8) 1 d PG A 2 C32P C 1.0641(16) 0.161(2) -0.1317(9) 0.132(12) Uiso 0.287(8) 1 d PG A 2 H32P H 1.1607 0.1760 -0.1363 0.158 Uiso 0.287(8) 1 d PG A 2 C33P C 0.9781(16) 0.2543(16) -0.1161(6) 0.080(6) Uiso 0.287(8) 1 d PGDU A 2 H33P H 1.0176 0.3308 -0.1097 0.096 Uiso 0.287(8) 1 d PG 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 N1R 0.055(4) 0.083(5) 0.079(5) 0.011(5) -0.007(4) -0.020(4) O1R 0.130(9) 0.080(5) 0.107(6) 0.024(4) -0.039(5) -0.035(6) O2R 0.049(3) 0.096(6) 0.086(6) -0.006(5) -0.010(3) -0.001(4) O3R 0.123(6) 0.094(5) 0.212(11) 0.005(6) 0.009(6) -0.031(5) O4R 0.079(4) 0.091(5) 0.120(6) -0.019(4) -0.013(4) -0.007(4) C7R 0.072(5) 0.061(5) 0.073(5) -0.006(4) 0.002(4) 0.010(4) C14R 0.107(7) 0.087(6) 0.094(7) 0.003(6) 0.021(6) 0.017(6) C15R 0.110(9) 0.140(12) 0.242(19) 0.034(12) 0.044(10) 0.026(9) C16R 0.192(14) 0.139(11) 0.166(13) -0.050(9) -0.021(11) 0.063(11) C17R 0.129(8) 0.130(9) 0.079(6) 0.038(7) -0.009(6) 0.029(8) C18R 0.184(14) 0.154(12) 0.120(10) 0.018(10) -0.064(11) -0.046(13) C19R 0.160(11) 0.146(10) 0.083(7) 0.048(7) -0.048(8) -0.021(9) C20R 0.100(8) 0.116(9) 0.114(8) -0.008(7) -0.014(6) 0.045(7) C21R 0.163(15) 0.113(11) 0.157(12) -0.033(9) 0.012(11) 0.037(10) C22R 0.119(9) 0.171(16) 0.172(13) -0.015(12) 0.048(10) 0.005(11) C23R 0.056(4) 0.068(6) 0.056(5) -0.005(5) 0.004(4) 0.019(4) C24R 0.058(4) 0.072(6) 0.097(6) 0.017(5) -0.015(4) -0.009(5) C25R 0.097(7) 0.085(7) 0.069(6) 0.004(5) -0.005(5) -0.021(6) C26R 0.103(8) 0.102(8) 0.137(11) -0.035(8) -0.009(8) 0.008(7) C27R 0.072(5) 0.084(7) 0.088(6) 0.018(6) -0.017(5) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1R C23R 1.319(6) . ? N1R C24R 1.439(7) . ? N1R H1R 0.8600 . ? O1R C7R 1.220(7) . ? O2R C23R 1.222(7) . ? O3R C25R 1.171(7) . ? O4R C25R 1.297(7) . ? O4R C26R 1.433(8) . ? C1R C2R 1.387(7) . ? C1R C6R 1.403(7) . ? C1R C14R 1.488(8) . ? C2R C3R 1.373(8) . ? C2R H2R 0.9300 . ? C3R C4R 1.377(8) . ? C3R C17R 1.505(7) . ? C4R C5R 1.423(8) . ? C4R H4R 0.9300 . ? C5R C6R 1.382(7) . ? C5R C20R 1.509(8) . ? C6R C7R 1.504(7) . ? C7R C8R 1.479(7) . ? C8R C13R 1.385(7) . ? C8R C9R 1.394(7) . ? C9R C10R 1.386(8) . ? C9R H9R 0.9300 . ? C10R C11R 1.387(8) . ? C10R H10R 0.9300 . ? C11R C12R 1.396(7) . ? C11R C23R 1.477(7) . ? C12R C13R 1.370(8) . ? C12R H12R 0.9300 . ? C13R H13R 0.9300 . ? C14R C15R 1.498(8) . ? C14R C16R 1.523(9) . ? C14R H14R 0.9800 . ? C15R H15A 0.9600 . ? C15R H15B 0.9600 . ? C15R H15C 0.9600 . ? C16R H16A 0.9600 . ? C16R H16B 0.9600 . ? C16R H16C 0.9600 . ? C17R C19R 1.421(9) . ? C17R C18R 1.460(9) . ? C17R H17R 0.9800 . ? C18R H18A 0.9600 . ? C18R H18B 0.9600 . ? C18R H18C 0.9600 . ? C19R H19A 0.9600 . ? C19R H19B 0.9600 . ? C19R H19C 0.9600 . ? C20R C21R 1.505(9) . ? C20R C22R 1.520(9) . ? C20R H20R 0.9800 . ? C21R H21A 0.9600 . ? C21R H21B 0.9600 . ? C21R H21C 0.9600 . ? C22R H22A 0.9600 . ? C22R H22B 0.9600 . ? C22R H22C 0.9600 . ? C24R C25R 1.511(8) . ? C24R C27R 1.514(8) . ? C24R H24R 0.9800 . ? C26R H26A 0.9600 . ? C26R H26B 0.9600 . ? C26R H26C 0.9600 . ? C27R C28R 1.489(7) . ? C27R H27A 0.9700 . ? C27R H27B 0.9700 . ? C28R C29R 1.3754 . ? C28R C33R 1.3831 . ? C29R C30R 1.3701 . ? C29R H29R 0.9300 . ? C30R C31R 1.3770 . ? C30R H30R 0.9300 . ? C31R C32R 1.3617 . ? C31R H31R 0.9300 . ? C32R C33R 1.3725 . ? C32R H32R 0.9301 . ? C33R H33R 0.9300 . ? N1P C23P 1.340(9) . ? N1P C24P 1.435(10) . ? N1P H1P 0.8600 . ? O1P C7P 1.412(9) . ? O2P C23P 1.232(9) . ? O3P C25P 1.223(9) . ? O4P C25P 1.314(9) . ? O4P C26P 1.434(10) . ? C1P C6P 1.357(9) . ? C1P C2P 1.380(9) . ? C1P C14P 1.528(9) . ? C2P C3P 1.393(9) . ? C2P H2P 0.9300 . ? C3P C4P 1.368(9) . ? C3P C17P 1.539(9) . ? C4P C5P 1.406(9) . ? C4P H4P 0.9300 . ? C5P C6P 1.376(8) . ? C5P C20P 1.520(9) . ? C6P C7P 1.514(9) . ? C7P C8P 1.523(9) . ? C7P C14P 1.659(9) . ? C8P C9P 1.364(9) . ? C8P C13P 1.382(9) . ? C9P C10P 1.381(9) . ? C9P H9P 0.9300 . ? C10P C11P 1.367(9) . ? C10P H10P 0.9300 . ? C11P C12P 1.379(9) . ? C11P C23P 1.480(9) . ? C12P C13P 1.365(9) . ? C12P H12P 0.9300 . ? C13P H13P 0.9300 . ? C14P C16P 1.498(9) . ? C14P C15P 1.521(9) . ? C15P H15D 0.9600 . ? C15P H15E 0.9600 . ? C15P H15F 0.9600 . ? C16P H16D 0.9600 . ? C16P H16E 0.9600 . ? C16P H16F 0.9600 . ? C17P C19P 1.449(10) . ? C17P C18P 1.464(10) . ? C17P H17P 0.9800 . ? C18P H18D 0.9600 . ? C18P H18E 0.9600 . ? C18P H18F 0.9600 . ? C19P H19D 0.9600 . ? C19P H19E 0.9600 . ? C19P H19F 0.9600 . ? C20P C22P 1.511(10) . ? C20P C21P 1.511(10) . ? C20P H20P 0.9800 . ? C21P H21D 0.9600 . ? C21P H21E 0.9600 . ? C21P H21F 0.9600 . ? C22P H22D 0.9600 . ? C22P H22E 0.9600 . ? C22P H22F 0.9600 . ? C24P C25P 1.493(9) . ? C24P C27P 1.522(10) . ? C24P H24P 0.9800 . ? C26P H26D 0.9600 . ? C26P H26E 0.9600 . ? C26P H26F 0.9600 . ? C27P C28P 1.472(9) . ? C27P H27C 0.9700 . ? C27P H27D 0.9700 . ? C28P C29P 1.3689 . ? C28P C33P 1.3759 . ? C29P C30P 1.3762 . ? C29P H29P 0.9300 . ? C30P C31P 1.3694 . ? C30P H30P 0.9300 . ? C31P C32P 1.3674 . ? C31P H31P 0.9300 . ? C32P C33P 1.3743 . ? C32P H32P 0.9300 . ? C33P H33P 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23R N1R C24R 122.8(6) . . ? C23R N1R H1R 118.6 . . ? C24R N1R H1R 118.6 . . ? C25R O4R C26R 117.9(8) . . ? C2R C1R C6R 119.3(7) . . ? C2R C1R C14R 118.9(7) . . ? C6R C1R C14R 121.8(7) . . ? C3R C2R C1R 121.0(7) . . ? C3R C2R H2R 119.5 . . ? C1R C2R H2R 119.5 . . ? C2R C3R C4R 119.0(7) . . ? C2R C3R C17R 119.0(8) . . ? C4R C3R C17R 121.9(8) . . ? C3R C4R C5R 122.3(7) . . ? C3R C4R H4R 118.8 . . ? C5R C4R H4R 118.8 . . ? C6R C5R C4R 116.5(6) . . ? C6R C5R C20R 121.3(6) . . ? C4R C5R C20R 121.6(7) . . ? C5R C6R C1R 121.5(6) . . ? C5R C6R C7R 120.1(6) . . ? C1R C6R C7R 118.3(6) . . ? O1R C7R C8R 121.7(7) . . ? O1R C7R C6R 119.2(7) . . ? C8R C7R C6R 119.1(7) . . ? C13R C8R C9R 118.3(6) . . ? C13R C8R C7R 120.7(6) . . ? C9R C8R C7R 121.1(6) . . ? C10R C9R C8R 120.1(7) . . ? C10R C9R H9R 120.0 . . ? C8R C9R H9R 120.0 . . ? C9R C10R C11R 120.8(7) . . ? C9R C10R H10R 119.6 . . ? C11R C10R H10R 119.6 . . ? C10R C11R C12R 118.9(6) . . ? C10R C11R C23R 123.0(7) . . ? C12R C11R C23R 118.1(7) . . ? C13R C12R C11R 119.7(7) . . ? C13R C12R H12R 120.2 . . ? C11R C12R H12R 120.2 . . ? C12R C13R C8R 121.7(7) . . ? C12R C13R H13R 119.2 . . ? C8R C13R H13R 119.2 . . ? C1R C14R C15R 109.7(7) . . ? C1R C14R C16R 113.0(8) . . ? C15R C14R C16R 112.4(10) . . ? C1R C14R H14R 107.1 . . ? C15R C14R H14R 107.1 . . ? C16R C14R H14R 107.1 . . ? C14R C15R H15A 109.5 . . ? C14R C15R H15B 109.5 . . ? H15A C15R H15B 109.5 . . ? C14R C15R H15C 109.5 . . ? H15A C15R H15C 109.5 . . ? H15B C15R H15C 109.5 . . ? C14R C16R H16A 109.5 . . ? C14R C16R H16B 109.5 . . ? H16A C16R H16B 109.5 . . ? C14R C16R H16C 109.5 . . ? H16A C16R H16C 109.5 . . ? H16B C16R H16C 109.5 . . ? C19R C17R C18R 122.8(9) . . ? C19R C17R C3R 114.1(8) . . ? C18R C17R C3R 115.5(8) . . ? C19R C17R H17R 99.2 . . ? C18R C17R H17R 99.2 . . ? C3R C17R H17R 99.2 . . ? C17R C18R H18A 109.5 . . ? C17R C18R H18B 109.5 . . ? H18A C18R H18B 109.5 . . ? C17R C18R H18C 109.5 . . ? H18A C18R H18C 109.5 . . ? H18B C18R H18C 109.5 . . ? C17R C19R H19A 109.5 . . ? C17R C19R H19B 109.5 . . ? H19A C19R H19B 109.5 . . ? C17R C19R H19C 109.5 . . ? H19A C19R H19C 109.5 . . ? H19B C19R H19C 109.5 . . ? C21R C20R C5R 113.0(9) . . ? C21R C20R C22R 111.4(9) . . ? C5R C20R C22R 112.0(9) . . ? C21R C20R H20R 106.6 . . ? C5R C20R H20R 106.6 . . ? C22R C20R H20R 106.6 . . ? C20R C21R H21A 109.5 . . ? C20R C21R H21B 109.5 . . ? H21A C21R H21B 109.5 . . ? C20R C21R H21C 109.5 . . ? H21A C21R H21C 109.5 . . ? H21B C21R H21C 109.5 . . ? C20R C22R H22A 109.5 . . ? C20R C22R H22B 109.5 . . ? H22A C22R H22B 109.5 . . ? C20R C22R H22C 109.5 . . ? H22A C22R H22C 109.5 . . ? H22B C22R H22C 109.5 . . ? O2R C23R N1R 122.4(7) . . ? O2R C23R C11R 120.7(7) . . ? N1R C23R C11R 116.8(6) . . ? N1R C24R C25R 111.2(7) . . ? N1R C24R C27R 111.7(7) . . ? C25R C24R C27R 112.1(6) . . ? N1R C24R H24R 107.2 . . ? C25R C24R H24R 107.2 . . ? C27R C24R H24R 107.2 . . ? O3R C25R O4R 125.3(8) . . ? O3R C25R C24R 123.8(8) . . ? O4R C25R C24R 110.4(7) . . ? C28R C27R C24R 113.2(6) . . ? C28R C27R H27A 108.9 . . ? C24R C27R H27A 108.9 . . ? C28R C27R H27B 108.9 . . ? C24R C27R H27B 108.9 . . ? H27A C27R H27B 107.8 . . ? C29R C28R C33R 117.2 . . ? C29R C28R C27R 121.2(5) . . ? C33R C28R C27R 121.6(5) . . ? C30R C29R C28R 121.3 . . ? C29R C30R C31R 121.0 . . ? C32R C31R C30R 118.1 . . ? C31R C32R C33R 121.2 . . ? C32R C33R C28R 121.2 . . ? C23P N1P C24P 123.0(15) . . ? C23P N1P H1P 118.5 . . ? C24P N1P H1P 118.5 . . ? C25P O4P C26P 119.3(16) . . ? C6P C1P C2P 121.8(10) . . ? C6P C1P C14P 93.1(8) . . ? C2P C1P C14P 145.1(11) . . ? C1P C2P C3P 117.3(11) . . ? C1P C2P H2P 121.4 . . ? C3P C2P H2P 121.4 . . ? C4P C3P C2P 119.3(10) . . ? C4P C3P C17P 119.1(11) . . ? C2P C3P C17P 120.4(11) . . ? C3P C4P C5P 123.8(12) . . ? C3P C4P H4P 118.1 . . ? C5P C4P H4P 118.1 . . ? C6P C5P C4P 113.8(11) . . ? C6P C5P C20P 123.0(12) . . ? C4P C5P C20P 120.0(12) . . ? C1P C6P C5P 122.7(10) . . ? C1P C6P C7P 97.3(8) . . ? C5P C6P C7P 139.9(10) . . ? O1P C7P C6P 112.9(14) . . ? O1P C7P C8P 109.9(12) . . ? C6P C7P C8P 115.0(12) . . ? O1P C7P C14P 113.2(13) . . ? C6P C7P C14P 82.6(7) . . ? C8P C7P C14P 120.9(13) . . ? C9P C8P C13P 117.2(10) . . ? C9P C8P C7P 119.9(10) . . ? C13P C8P C7P 123.0(10) . . ? C8P C9P C10P 123.1(11) . . ? C8P C9P H9P 118.4 . . ? C10P C9P H9P 118.4 . . ? C11P C10P C9P 119.2(11) . . ? C11P C10P H10P 120.4 . . ? C9P C10P H10P 120.4 . . ? C10P C11P C12P 117.2(10) . . ? C10P C11P C23P 123.8(11) . . ? C12P C11P C23P 119.0(11) . . ? C13P C12P C11P 122.3(12) . . ? C13P C12P H12P 118.9 . . ? C11P C12P H12P 118.9 . . ? C12P C13P C8P 118.8(12) . . ? C12P C13P H13P 120.6 . . ? C8P C13P H13P 120.6 . . ? C16P C14P C15P 111.2(12) . . ? C16P C14P C1P 115.1(12) . . ? C15P C14P C1P 116.0(13) . . ? C16P C14P C7P 117.3(12) . . ? C15P C14P C7P 109.8(11) . . ? C1P C14P C7P 85.2(7) . . ? C14P C15P H15D 109.5 . . ? C14P C15P H15E 109.5 . . ? H15D C15P H15E 109.5 . . ? C14P C15P H15F 109.5 . . ? H15D C15P H15F 109.5 . . ? H15E C15P H15F 109.5 . . ? C14P C16P H16D 109.5 . . ? C14P C16P H16E 109.5 . . ? H16D C16P H16E 109.5 . . ? C14P C16P H16F 109.5 . . ? H16D C16P H16F 109.5 . . ? H16E C16P H16F 109.5 . . ? C19P C17P C18P 114.7(15) . . ? C19P C17P C3P 112.8(14) . . ? C18P C17P C3P 111.8(14) . . ? C19P C17P H17P 105.5 . . ? C18P C17P H17P 105.5 . . ? C3P C17P H17P 105.5 . . ? C17P C18P H18D 109.5 . . ? C17P C18P H18E 109.5 . . ? H18D C18P H18E 109.5 . . ? C17P C18P H18F 109.5 . . ? H18D C18P H18F 109.5 . . ? H18E C18P H18F 109.5 . . ? C17P C19P H19D 109.5 . . ? C17P C19P H19E 109.5 . . ? H19D C19P H19E 109.5 . . ? C17P C19P H19F 109.5 . . ? H19D C19P H19F 109.5 . . ? H19E C19P H19F 109.5 . . ? C22P C20P C21P 109.8(14) . . ? C22P C20P C5P 110.0(14) . . ? C21P C20P C5P 110.3(14) . . ? C22P C20P H20P 108.9 . . ? C21P C20P H20P 108.9 . . ? C5P C20P H20P 108.9 . . ? C20P C21P H21D 109.5 . . ? C20P C21P H21E 109.5 . . ? H21D C21P H21E 109.5 . . ? C20P C21P H21F 109.5 . . ? H21D C21P H21F 109.5 . . ? H21E C21P H21F 109.5 . . ? C20P C22P H22D 109.5 . . ? C20P C22P H22E 109.5 . . ? H22D C22P H22E 109.5 . . ? C20P C22P H22F 109.5 . . ? H22D C22P H22F 109.5 . . ? H22E C22P H22F 109.5 . . ? O2P C23P N1P 121.1(13) . . ? O2P C23P C11P 121.5(13) . . ? N1P C23P C11P 117.2(12) . . ? N1P C24P C25P 114.0(13) . . ? N1P C24P C27P 110.3(13) . . ? C25P C24P C27P 110.4(12) . . ? N1P C24P H24P 107.3 . . ? C25P C24P H24P 107.3 . . ? C27P C24P H24P 107.3 . . ? O3P C25P O4P 123.3(13) . . ? O3P C25P C24P 122.6(13) . . ? O4P C25P C24P 114.0(12) . . ? O4P C26P H26D 109.5 . . ? O4P C26P H26E 109.5 . . ? H26D C26P H26E 109.5 . . ? O4P C26P H26F 109.5 . . ? H26D C26P H26F 109.5 . . ? H26E C26P H26F 109.5 . . ? C28P C27P C24P 113.8(12) . . ? C28P C27P H27C 108.8 . . ? C24P C27P H27C 108.8 . . ? C28P C27P H27D 108.8 . . ? C24P C27P H27D 108.8 . . ? H27C C27P H27D 107.7 . . ? C29P C28P C33P 118.1 . . ? C29P C28P C27P 122.1(10) . . ? C33P C28P C27P 119.8(10) . . ? C28P C29P C30P 120.7 . . ? C28P C29P H29P 119.7 . . ? C30P C29P H29P 119.7 . . ? C31P C30P C29P 121.2 . . ? C31P C30P H30P 119.4 . . ? C29P C30P H30P 119.4 . . ? C32P C31P C30P 118.1 . . ? C32P C31P H31P 120.9 . . ? C30P C31P H31P 120.9 . . ? C31P C32P C33P 120.9 . . ? C31P C32P H32P 119.6 . . ? C33P C32P H32P 119.6 . . ? C32P C33P C28P 121.0 . . ? C32P C33P H33P 119.5 . . ? C28P C33P H33P 119.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.196 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.037 #===END data_55.6%P _database_code_depnum_ccdc_archive 'CCDC 799257' #TrackingRef '- 1.cif' #==================================================================== # start Validation Reply Form _vrf_PLAT201_55.6%P ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 18 RESPONSE: In the crystal there are reactant and photoproduct molecules. Part of atoms were refined isotropically in order to decrease a large number of the parameters in the refinement. ; # end Validation Reply Form #==================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 N O4' _chemical_formula_weight 513.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.3702(13) _cell_length_b 11.016(2) _cell_length_c 29.134(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3007.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 13.3 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.135 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14678 _diffrn_reflns_av_R_equivalents 0.0774 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.96 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2990 _reflns_number_gt 1769 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSALIS (Oxford Diffraction, 2003)' _computing_cell_refinement 'CRYSALIS (Oxford Diffraction, 2003)' _computing_data_reduction 'CRYSALIS (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Owing to a reactant-product disorder, the following weak restraints from SHELXL97 were applied: DFIX, DANG and SIMU. DFIX and DANG restrained bond lengths and valence angles to target values. The target values were taken from the structures of the pure reactant and the pure product of crystal 1a. SIMU restrained displacement parameters of atoms of the products. The R1(obs) value above 0.10 is the result of the strong reactant-product disorder in the crystal containing a similar number of reactant and product molecules. ; _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^)+(0.1553P)^2^+0.0969P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration syn _refine_ls_number_reflns 2990 _refine_ls_number_parameters 384 _refine_ls_number_restraints 282 _refine_ls_R_factor_all 0.1574 _refine_ls_R_factor_gt 0.1011 _refine_ls_wR_factor_ref 0.3158 _refine_ls_wR_factor_gt 0.2707 _refine_ls_goodness_of_fit_ref 1.222 _refine_ls_restrained_S_all 1.273 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1R N 0.722(2) 0.2989(15) -0.0013(6) 0.088(7) Uiso 0.444(12) 1 d PDU A 1 H1R H 0.6324 0.2831 0.0013 0.105 Uiso 0.444(12) 1 calc PR A 1 O1R O 0.523(3) -0.252(3) 0.1052(9) 0.112(11) Uiso 0.444(12) 1 d PDU A 1 O2R O 0.931(3) 0.270(2) 0.0340(11) 0.094(7) Uiso 0.444(12) 1 d PDU A 1 O3R O 0.7599(19) 0.6088(14) -0.0088(7) 0.142(7) Uiso 0.444(12) 1 d PDU A 1 O4R O 0.5632(18) 0.5032(18) -0.0055(8) 0.104(6) Uiso 0.444(12) 1 d PDU A 1 C1R C 0.6474(19) -0.193(2) 0.2009(4) 0.082(10) Uiso 0.444(12) 1 d PDU A 1 C2R C 0.710(2) -0.233(2) 0.2411(5) 0.090(8) Uiso 0.444(12) 1 d PDU A 1 H2R H 0.6646 -0.2182 0.2688 0.108 Uiso 0.444(12) 1 calc PR A 1 C3R C 0.838(2) -0.295(2) 0.2414(5) 0.088(8) Uiso 0.444(12) 1 d PDU A 1 C4R C 0.9064(19) -0.312(2) 0.2004(5) 0.088(7) Uiso 0.444(12) 1 d PDU A 1 H4R H 0.9969 -0.3469 0.2005 0.105 Uiso 0.444(12) 1 calc PR A 1 C5R C 0.8439(16) -0.2793(19) 0.1579(4) 0.079(6) Uiso 0.444(12) 1 d PDU A 1 C6R C 0.7108(19) -0.225(2) 0.1593(4) 0.082(11) Uiso 0.444(12) 1 d PDU A 1 C7R C 0.6315(16) -0.1960(13) 0.1158(5) 0.075(6) Uiso 0.444(12) 1 d PDU A 1 C8R C 0.6749(17) -0.0875(13) 0.0897(5) 0.068(5) Uiso 0.444(12) 1 d PD A 1 C9R C 0.6248(18) -0.0639(14) 0.0458(5) 0.074(6) Uiso 0.444(12) 1 d PD A 1 H9R H 0.5637 -0.1189 0.0316 0.089 Uiso 0.444(12) 1 calc PR A 1 C10R C 0.665(3) 0.0399(17) 0.0232(6) 0.082(8) Uiso 0.444(12) 1 d PDU A 1 H10R H 0.6272 0.0572 -0.0057 0.098 Uiso 0.444(12) 1 calc PR A 1 C11R C 0.760(3) 0.1186(17) 0.0434(7) 0.065(10) Uiso 0.444(12) 1 d PD A 1 C12R C 0.819(2) 0.0892(15) 0.0862(6) 0.059(6) Uiso 0.444(12) 1 d PDU A 1 H12R H 0.8861 0.1404 0.0993 0.070 Uiso 0.444(12) 1 calc PR A 1 C13R C 0.7783(19) -0.0127(15) 0.1086(6) 0.077(7) Uiso 0.444(12) 1 d PD A 1 H13R H 0.8198 -0.0324 0.1367 0.092 Uiso 0.444(12) 1 calc PR A 1 C14R C 0.5159(17) -0.1162(17) 0.2039(6) 0.100(8) Uiso 0.444(12) 1 d PD A 1 H14R H 0.4874 -0.0918 0.1729 0.120 Uiso 0.444(12) 1 calc PR A 1 C15R C 0.398(2) -0.191(2) 0.2249(11) 0.156(12) Uiso 0.444(12) 1 d PD A 1 H15A H 0.3125 -0.1437 0.2265 0.234 Uiso 0.444(12) 1 calc PR A 1 H15B H 0.4256 -0.2161 0.2552 0.234 Uiso 0.444(12) 1 calc PR A 1 H15C H 0.3815 -0.2618 0.2063 0.234 Uiso 0.444(12) 1 calc PR A 1 C16R C 0.542(3) -0.0027(19) 0.2327(10) 0.158(12) Uiso 0.444(12) 1 d PD A 1 H16A H 0.4561 0.0451 0.2337 0.237 Uiso 0.444(12) 1 calc PR A 1 H16B H 0.6174 0.0441 0.2193 0.237 Uiso 0.444(12) 1 calc PR A 1 H16C H 0.5678 -0.0260 0.2634 0.237 Uiso 0.444(12) 1 calc PR A 1 C17R C 0.906(3) -0.319(2) 0.2866(7) 0.125(9) Uiso 0.444(12) 1 d PDU A 1 H17R H 0.8275 -0.2927 0.3064 0.150 Uiso 0.444(12) 1 calc PR A 1 C18R C 1.014(3) -0.230(2) 0.3018(10) 0.144(12) Uiso 0.444(12) 1 d PD A 1 H18A H 0.9914 -0.1515 0.2892 0.216 Uiso 0.444(12) 1 calc PR A 1 H18B H 1.1066 -0.2545 0.2914 0.216 Uiso 0.444(12) 1 calc PR A 1 H18C H 1.0134 -0.2249 0.3347 0.216 Uiso 0.444(12) 1 calc PR A 1 C19R C 0.912(3) -0.4426(19) 0.3008(9) 0.118(11) Uiso 0.444(12) 1 d PD A 1 H19A H 0.8330 -0.4861 0.2879 0.177 Uiso 0.444(12) 1 calc PR A 1 H19B H 0.9076 -0.4467 0.3337 0.177 Uiso 0.444(12) 1 calc PR A 1 H19C H 0.9998 -0.4783 0.2904 0.177 Uiso 0.444(12) 1 calc PR A 1 C20R C 0.908(3) -0.317(3) 0.1122(6) 0.104(11) Uiso 0.444(12) 1 d PD A 1 H20R H 0.8445 -0.2830 0.0886 0.125 Uiso 0.444(12) 1 calc PR A 1 C21R C 0.905(5) -0.452(3) 0.1053(15) 0.159(15) Uiso 0.444(12) 1 d PDU A 1 H21A H 0.9427 -0.4707 0.0755 0.239 Uiso 0.444(12) 1 calc PR A 1 H21B H 0.8086 -0.4803 0.1075 0.239 Uiso 0.444(12) 1 calc PR A 1 H21C H 0.9622 -0.4899 0.1285 0.239 Uiso 0.444(12) 1 calc PR A 1 C22R C 1.052(4) -0.261(4) 0.1040(17) 0.178(17) Uiso 0.444(12) 1 d PDU A 1 H22A H 1.0466 -0.1743 0.1086 0.267 Uiso 0.444(12) 1 calc PR A 1 H22B H 1.0825 -0.2770 0.0732 0.267 Uiso 0.444(12) 1 calc PR A 1 H22C H 1.1202 -0.2943 0.1252 0.267 Uiso 0.444(12) 1 calc PR A 1 C23R C 0.817(3) 0.229(2) 0.0208(11) 0.11(2) Uiso 0.444(12) 1 d PD A 1 C24R C 0.767(2) 0.4000(13) -0.0293(5) 0.084(6) Uiso 0.444(12) 1 d PDU A 1 H24R H 0.8700 0.4092 -0.0260 0.101 Uiso 0.444(12) 1 calc PR A 1 C25R C 0.6967(19) 0.5162(14) -0.0137(9) 0.103(7) Uiso 0.444(12) 1 d PDU A 1 C26R C 0.483(3) 0.605(3) 0.0106(13) 0.122(7) Uiso 0.444(12) 1 d PDU A 1 H26A H 0.4980 0.6153 0.0430 0.183 Uiso 0.444(12) 1 calc PR A 1 H26B H 0.3832 0.5921 0.0049 0.183 Uiso 0.444(12) 1 calc PR A 1 H26C H 0.5135 0.6773 -0.0052 0.183 Uiso 0.444(12) 1 calc PR A 1 C27R C 0.734(2) 0.3807(15) -0.0799(5) 0.086(6) Uiso 0.444(12) 1 d PDU A 1 H27A H 0.6321 0.3661 -0.0835 0.103 Uiso 0.444(12) 1 calc PR A 1 H27B H 0.7571 0.4540 -0.0967 0.103 Uiso 0.444(12) 1 calc PR A 1 C28R C 0.8139(14) 0.2769(12) -0.1000(5) 0.074(5) Uiso 0.444(12) 1 d PGDU A 1 C29R C 0.7546(13) 0.1627(12) -0.1013(5) 0.098(6) Uiso 0.444(12) 1 d PGDU A 1 H29R H 0.6631 0.1509 -0.0897 0.117 Uiso 0.444(12) 1 d PG A 1 C30R C 0.8275(18) 0.0660(12) -0.1193(7) 0.120(7) Uiso 0.444(12) 1 d PG A 1 H30R H 0.7852 -0.0103 -0.1196 0.145 Uiso 0.444(12) 1 d PG A 1 C31R C 0.9627(18) 0.0803(15) -0.1371(7) 0.144(10) Uiso 0.444(12) 1 d PG A 1 H31R H 1.0129 0.0144 -0.1488 0.173 Uiso 0.444(12) 1 d PG A 1 C32R C 1.0207(15) 0.1936(17) -0.1370(7) 0.122(8) Uiso 0.444(12) 1 d PG A 1 H32R H 1.1109 0.2055 -0.1496 0.147 Uiso 0.444(12) 1 d PG A 1 C33R C 0.9486(15) 0.2906(14) -0.1187(6) 0.109(6) Uiso 0.444(12) 1 d PGDU A 1 H33R H 0.9909 0.3669 -0.1189 0.131 Uiso 0.444(12) 1 d PG A 1 N1P N 0.7367(12) 0.2712(12) -0.0135(4) 0.073(4) Uani 0.556(12) 1 d PDU A 2 H1P H 0.6577 0.2341 -0.0190 0.088 Uiso 0.556(12) 1 calc PR A 2 O1P O 0.508(2) -0.2423(18) 0.1035(6) 0.106(8) Uani 0.556(12) 1 d PDU A 2 O2P O 0.9377(13) 0.2756(19) 0.0279(8) 0.085(5) Uani 0.556(12) 1 d PDU A 2 O3P O 0.7423(16) 0.5826(12) -0.0467(7) 0.160(7) Uani 0.556(12) 1 d PDU A 2 O4P O 0.6013(18) 0.4776(13) 0.0002(6) 0.122(5) Uani 0.556(12) 1 d PDU A 2 C1P C 0.6570(17) -0.2017(19) 0.2005(4) 0.093(9) Uiso 0.556(12) 1 d PDU A 2 C2P C 0.7325(18) -0.228(2) 0.2399(5) 0.111(9) Uiso 0.556(12) 1 d PDU A 2 H2P H 0.7024 -0.2004 0.2685 0.133 Uiso 0.556(12) 1 calc PR A 2 C3P C 0.8560(18) -0.2979(19) 0.2352(4) 0.104(7) Uiso 0.556(12) 1 d PDU A 2 C4P C 0.8930(18) -0.3396(19) 0.1927(4) 0.112(7) Uiso 0.556(12) 1 d PDU A 2 H4P H 0.9713 -0.3912 0.1905 0.134 Uiso 0.556(12) 1 calc PR A 2 C5P C 0.8203(15) -0.3095(15) 0.1522(4) 0.090(6) Uiso 0.556(12) 1 d PDU A 2 C6P C 0.7029(17) -0.2364(18) 0.1586(4) 0.081(8) Uiso 0.556(12) 1 d PDU A 2 C7P C 0.5936(11) -0.1663(9) 0.1310(3) 0.086(4) Uani 0.556(12) 1 d PDU A 2 C8P C 0.6547(14) -0.0626(11) 0.1023(4) 0.076(5) Uiso 0.556(12) 1 d PD A 2 C9P C 0.6051(13) -0.0408(11) 0.0587(4) 0.063(4) Uiso 0.556(12) 1 d PD A 2 H9P H 0.5337 -0.0902 0.0467 0.076 Uiso 0.556(12) 1 calc PR A 2 C10P C 0.6588(18) 0.0526(14) 0.0321(5) 0.073(6) Uiso 0.556(12) 1 d PDU A 2 H10P H 0.6243 0.0640 0.0025 0.087 Uiso 0.556(12) 1 calc PR A 2 C11P C 0.762(2) 0.1289(16) 0.0490(6) 0.074(9) Uiso 0.556(12) 1 d PD A 2 C12P C 0.812(2) 0.1065(16) 0.0928(5) 0.086(7) Uiso 0.556(12) 1 d PDU A 2 H12P H 0.8812 0.1573 0.1052 0.104 Uiso 0.556(12) 1 calc PR A 2 C13P C 0.7622(15) 0.0125(13) 0.1181(5) 0.077(6) Uiso 0.556(12) 1 d PD A 2 H13P H 0.8014 -0.0018 0.1470 0.092 Uiso 0.556(12) 1 calc PR A 2 C14P C 0.5266(11) -0.1337(11) 0.1821(4) 0.105(6) Uani 0.556(12) 1 d PD A 2 C15P C 0.3864(13) -0.1985(15) 0.1924(7) 0.113(6) Uani 0.556(12) 1 d PD A 2 H15D H 0.3936 -0.2820 0.1832 0.170 Uiso 0.556(12) 1 calc PR A 2 H15E H 0.3105 -0.1601 0.1757 0.170 Uiso 0.556(12) 1 calc PR A 2 H15F H 0.3669 -0.1942 0.2247 0.170 Uiso 0.556(12) 1 calc PR A 2 C16P C 0.5162(19) -0.0032(11) 0.1965(7) 0.128(7) Uani 0.556(12) 1 d PD A 2 H16D H 0.4333 0.0329 0.1829 0.192 Uiso 0.556(12) 1 calc PR A 2 H16E H 0.6000 0.0397 0.1866 0.192 Uiso 0.556(12) 1 calc PR A 2 H16F H 0.5089 0.0014 0.2293 0.192 Uiso 0.556(12) 1 calc PR A 2 C17P C 0.938(2) -0.3362(16) 0.2787(6) 0.140(9) Uani 0.556(12) 1 d PDU A 2 H17P H 0.8791 -0.3090 0.3045 0.168 Uiso 0.556(12) 1 calc PR A 2 C18P C 1.075(2) -0.273(2) 0.2839(7) 0.138(8) Uani 0.556(12) 1 d PD A 2 H18D H 1.0600 -0.1874 0.2815 0.207 Uiso 0.556(12) 1 calc PR A 2 H18E H 1.1389 -0.2995 0.2602 0.207 Uiso 0.556(12) 1 calc PR A 2 H18F H 1.1148 -0.2923 0.3133 0.207 Uiso 0.556(12) 1 calc PR A 2 C19P C 0.947(3) -0.4667(16) 0.2830(8) 0.161(11) Uani 0.556(12) 1 d PD A 2 H19D H 0.8527 -0.5010 0.2806 0.241 Uiso 0.556(12) 1 calc PR A 2 H19E H 0.9869 -0.4872 0.3123 0.241 Uiso 0.556(12) 1 calc PR A 2 H19F H 1.0060 -0.4987 0.2590 0.241 Uiso 0.556(12) 1 calc PR A 2 C20P C 0.879(2) -0.3430(18) 0.1053(5) 0.118(8) Uani 0.556(12) 1 d PD A 2 H20P H 0.8216 -0.3012 0.0819 0.141 Uiso 0.556(12) 1 calc PR A 2 C21P C 0.865(3) -0.478(2) 0.0975(12) 0.167(11) Uani 0.556(12) 1 d PDU A 2 H21D H 0.8993 -0.4978 0.0673 0.250 Uiso 0.556(12) 1 calc PR A 2 H21E H 0.7672 -0.5018 0.1003 0.250 Uiso 0.556(12) 1 calc PR A 2 H21F H 0.9213 -0.5206 0.1200 0.250 Uiso 0.556(12) 1 calc PR A 2 C22P C 1.032(3) -0.303(3) 0.1003(12) 0.167(11) Uani 0.556(12) 1 d PDU A 2 H22D H 1.0638 -0.3204 0.0697 0.250 Uiso 0.556(12) 1 calc PR A 2 H22E H 1.0898 -0.3468 0.1219 0.250 Uiso 0.556(12) 1 calc PR A 2 H22F H 1.0387 -0.2179 0.1061 0.250 Uiso 0.556(12) 1 calc PR A 2 C23P C 0.8171(13) 0.2331(15) 0.0221(6) 0.060(10) Uani 0.556(12) 1 d PD A 2 C24P C 0.7761(15) 0.3702(10) -0.0426(4) 0.086(4) Uani 0.556(12) 1 d PDU A 2 H24P H 0.8794 0.3811 -0.0391 0.104 Uiso 0.556(12) 1 calc PR A 2 C25P C 0.7082(17) 0.4873(11) -0.0288(6) 0.111(6) Uani 0.556(12) 1 d PDU A 2 C26P C 0.528(3) 0.588(2) 0.0126(11) 0.159(8) Uani 0.556(12) 1 d PDU A 2 H26D H 0.4712 0.5746 0.0394 0.238 Uiso 0.556(12) 1 calc PR A 2 H26E H 0.4680 0.6134 -0.0123 0.238 Uiso 0.556(12) 1 calc PR A 2 H26F H 0.5972 0.6507 0.0188 0.238 Uiso 0.556(12) 1 calc PR A 2 C27P C 0.7495(15) 0.3420(13) -0.0928(4) 0.087(4) Uani 0.556(12) 1 d PDU A 2 H27C H 0.6485 0.3263 -0.0971 0.104 Uiso 0.556(12) 1 calc PR A 2 H27D H 0.7740 0.4129 -0.1109 0.104 Uiso 0.556(12) 1 calc PR A 2 C28P C 0.8306(11) 0.2377(11) -0.1101(4) 0.089(4) Uiso 0.556(12) 1 d PGDU A 2 C29P C 0.7695(12) 0.1267(12) -0.1180(6) 0.133(6) Uiso 0.556(12) 1 d PGDU A 2 H29P H 0.6721 0.1164 -0.1132 0.160 Uiso 0.556(12) 1 d PG A 2 C30P C 0.8506(17) 0.0304(10) -0.1329(6) 0.171(10) Uiso 0.556(12) 1 d PG A 2 H30P H 0.8078 -0.0450 -0.1370 0.205 Uiso 0.556(12) 1 d PG A 2 C31P C 0.9934(17) 0.0433(11) -0.1417(6) 0.148(8) Uiso 0.556(12) 1 d PG A 2 H31P H 1.0474 -0.0217 -0.1524 0.178 Uiso 0.556(12) 1 d PG A 2 C32P C 1.0542(12) 0.1545(13) -0.1344(6) 0.130(7) Uiso 0.556(12) 1 d PG A 2 H32P H 1.1509 0.1654 -0.1404 0.156 Uiso 0.556(12) 1 d PG A 2 C33P C 0.9744(11) 0.2503(11) -0.1185(4) 0.088(4) Uiso 0.556(12) 1 d PGDU A 2 H33P H 1.0182 0.3248 -0.1133 0.106 Uiso 0.556(12) 1 d PG 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 N1P 0.053(5) 0.094(8) 0.073(8) 0.018(8) 0.010(5) 0.003(6) O1P 0.122(11) 0.083(9) 0.113(11) 0.025(6) -0.037(7) -0.030(8) O2P 0.038(5) 0.124(9) 0.094(9) 0.042(6) 0.001(4) 0.002(4) O3P 0.138(10) 0.120(10) 0.223(18) 0.047(12) 0.047(12) 0.024(9) O4P 0.116(10) 0.111(9) 0.139(11) 0.000(8) 0.024(9) 0.026(8) C7P 0.082(8) 0.077(9) 0.099(10) 0.004(8) 0.002(8) 0.007(8) C14P 0.083(11) 0.096(13) 0.135(17) 0.012(11) 0.001(10) 0.010(9) C15P 0.075(9) 0.129(14) 0.137(17) 0.021(12) 0.019(9) -0.001(9) C16P 0.112(13) 0.095(13) 0.18(2) -0.020(12) 0.015(13) 0.014(10) C17P 0.143(16) 0.142(16) 0.135(15) 0.096(13) -0.022(13) 0.036(14) C18P 0.114(13) 0.19(2) 0.109(14) 0.063(14) -0.026(12) -0.027(17) C19P 0.16(2) 0.21(3) 0.106(17) 0.061(17) -0.047(17) 0.06(2) C20P 0.081(11) 0.12(2) 0.157(19) 0.002(13) -0.007(12) 0.032(12) C21P 0.16(2) 0.147(19) 0.19(2) -0.070(18) 0.01(2) 0.037(18) C22P 0.130(18) 0.20(3) 0.17(2) 0.02(2) 0.067(15) -0.018(18) C23P 0.036(8) 0.078(14) 0.065(12) 0.008(6) -0.004(5) 0.016(6) C24P 0.066(7) 0.104(10) 0.089(10) 0.032(9) 0.017(8) -0.003(8) C25P 0.099(10) 0.095(11) 0.137(14) 0.038(11) 0.035(10) 0.019(10) C26P 0.172(17) 0.143(14) 0.160(14) 0.000(13) 0.064(15) 0.060(14) C27P 0.078(8) 0.097(10) 0.086(9) 0.029(9) 0.017(8) 0.018(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1R C23R 1.339(10) . ? N1R C24R 1.444(10) . ? N1R H1R 0.8600 . ? O1R C7R 1.226(10) . ? O2R C23R 1.227(10) . ? O3R C25R 1.187(10) . ? O4R C25R 1.281(10) . ? O4R C26R 1.434(10) . ? C1R C2R 1.384(9) . ? C1R C6R 1.396(9) . ? C1R C14R 1.494(9) . ? C2R C3R 1.372(9) . ? C2R H2R 0.9300 . ? C3R C4R 1.370(9) . ? C3R C17R 1.491(9) . ? C4R C5R 1.417(9) . ? C4R H4R 0.9300 . ? C5R C6R 1.385(9) . ? C5R C20R 1.517(9) . ? C6R C7R 1.503(9) . ? C7R C8R 1.473(9) . ? C8R C13R 1.387(9) . ? C8R C9R 1.387(9) . ? C9R C10R 1.372(9) . ? C9R H9R 0.9300 . ? C10R C11R 1.379(9) . ? C10R H10R 0.9300 . ? C11R C12R 1.398(9) . ? C11R C23R 1.482(9) . ? C12R C13R 1.353(9) . ? C12R H12R 0.9300 . ? C13R H13R 0.9300 . ? C14R C15R 1.507(10) . ? C14R C16R 1.525(10) . ? C14R H14R 0.9800 . ? C15R H15A 0.9600 . ? C15R H15B 0.9600 . ? C15R H15C 0.9600 . ? C16R H16A 0.9600 . ? C16R H16B 0.9600 . ? C16R H16C 0.9600 . ? C17R C19R 1.424(10) . ? C17R C18R 1.477(10) . ? C17R H17R 0.9800 . ? C18R H18A 0.9600 . ? C18R H18B 0.9600 . ? C18R H18C 0.9600 . ? C19R H19A 0.9600 . ? C19R H19B 0.9600 . ? C19R H19C 0.9600 . ? C20R C21R 1.496(11) . ? C20R C22R 1.512(11) . ? C20R H20R 0.9800 . ? C21R H21A 0.9600 . ? C21R H21B 0.9600 . ? C21R H21C 0.9600 . ? C22R H22A 0.9600 . ? C22R H22B 0.9600 . ? C22R H22C 0.9600 . ? C24R C25R 1.509(9) . ? C24R C27R 1.520(10) . ? C24R H24R 0.9800 . ? C26R H26A 0.9600 . ? C26R H26B 0.9600 . ? C26R H26C 0.9600 . ? C27R C28R 1.489(9) . ? C27R H27A 0.9700 . ? C27R H27B 0.9700 . ? C28R C29R 1.3754 . ? C28R C33R 1.3832 . ? C29R C30R 1.3702 . ? C29R H29R 0.9299 . ? C30R C31R 1.3771 . ? C30R H30R 0.9300 . ? C31R C32R 1.3617 . ? C31R H31R 0.9300 . ? C32R C33R 1.3725 . ? C32R H32R 0.9300 . ? C33R H33R 0.9300 . ? N1P C23P 1.349(9) . ? N1P C24P 1.429(8) . ? N1P H1P 0.8600 . ? O1P C7P 1.407(9) . ? O2P C23P 1.235(8) . ? O3P C25P 1.216(9) . ? O4P C25P 1.315(9) . ? O4P C26P 1.444(10) . ? C1P C6P 1.352(9) . ? C1P C2P 1.379(9) . ? C1P C14P 1.530(9) . ? C2P C3P 1.396(9) . ? C2P H2P 0.9300 . ? C3P C4P 1.366(9) . ? C3P C17P 1.540(9) . ? C4P C5P 1.403(9) . ? C4P H4P 0.9300 . ? C5P C6P 1.376(8) . ? C5P C20P 1.516(9) . ? C6P C7P 1.514(8) . ? C7P C8P 1.527(8) . ? C7P C14P 1.655(10) . ? C8P C9P 1.373(9) . ? C8P C13P 1.384(9) . ? C9P C10P 1.383(9) . ? C9P H9P 0.9300 . ? C10P C11P 1.375(9) . ? C10P H10P 0.9300 . ? C11P C12P 1.380(9) . ? C11P C23P 1.480(8) . ? C12P C13P 1.355(9) . ? C12P H12P 0.9300 . ? C13P H13P 0.9300 . ? C14P C16P 1.501(9) . ? C14P C15P 1.525(9) . ? C15P H15D 0.9600 . ? C15P H15E 0.9600 . ? C15P H15F 0.9600 . ? C16P H16D 0.9600 . ? C16P H16E 0.9600 . ? C16P H16F 0.9600 . ? C17P C19P 1.446(10) . ? C17P C18P 1.464(10) . ? C17P H17P 0.9800 . ? C18P H18D 0.9600 . ? C18P H18E 0.9600 . ? C18P H18F 0.9600 . ? C19P H19D 0.9600 . ? C19P H19E 0.9600 . ? C19P H19F 0.9600 . ? C20P C22P 1.506(10) . ? C20P C21P 1.510(10) . ? C20P H20P 0.9800 . ? C21P H21D 0.9600 . ? C21P H21E 0.9600 . ? C21P H21F 0.9600 . ? C22P H22D 0.9600 . ? C22P H22E 0.9600 . ? C22P H22F 0.9600 . ? C24P C25P 1.494(9) . ? C24P C27P 1.517(9) . ? C24P H24P 0.9800 . ? C26P H26D 0.9600 . ? C26P H26E 0.9600 . ? C26P H26F 0.9600 . ? C27P C28P 1.468(8) . ? C27P H27C 0.9700 . ? C27P H27D 0.9700 . ? C28P C29P 1.3689 . ? C28P C33P 1.3760 . ? C29P C30P 1.3762 . ? C29P H29P 0.9300 . ? C30P C31P 1.3693 . ? C30P H30P 0.9300 . ? C31P C32P 1.3674 . ? C31P H31P 0.9300 . ? C32P C33P 1.3743 . ? C32P H32P 0.9300 . ? C33P H33P 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23R N1R C24R 121.5(14) . . ? C23R N1R H1R 119.2 . . ? C24R N1R H1R 119.2 . . ? C25R O4R C26R 119.0(15) . . ? C2R C1R C6R 118.1(10) . . ? C2R C1R C14R 118.9(10) . . ? C6R C1R C14R 123.0(11) . . ? C3R C2R C1R 122.3(11) . . ? C3R C2R H2R 118.8 . . ? C1R C2R H2R 118.8 . . ? C4R C3R C2R 118.3(10) . . ? C4R C3R C17R 122.7(12) . . ? C2R C3R C17R 118.0(12) . . ? C3R C4R C5R 122.0(10) . . ? C3R C4R H4R 119.0 . . ? C5R C4R H4R 119.0 . . ? C6R C5R C4R 117.2(9) . . ? C6R C5R C20R 119.9(11) . . ? C4R C5R C20R 122.3(11) . . ? C5R C6R C1R 121.3(9) . . ? C5R C6R C7R 120.8(10) . . ? C1R C6R C7R 117.9(10) . . ? O1R C7R C8R 120.4(13) . . ? O1R C7R C6R 121.1(13) . . ? C8R C7R C6R 118.0(11) . . ? C13R C8R C9R 119.4(9) . . ? C13R C8R C7R 118.1(9) . . ? C9R C8R C7R 122.3(10) . . ? C10R C9R C8R 120.5(11) . . ? C10R C9R H9R 119.7 . . ? C8R C9R H9R 119.7 . . ? C9R C10R C11R 119.7(11) . . ? C9R C10R H10R 120.2 . . ? C11R C10R H10R 120.2 . . ? C10R C11R C12R 119.4(9) . . ? C10R C11R C23R 123.9(12) . . ? C12R C11R C23R 116.5(11) . . ? C13R C12R C11R 120.9(11) . . ? C13R C12R H12R 119.6 . . ? C11R C12R H12R 119.6 . . ? C12R C13R C8R 119.8(11) . . ? C12R C13R H13R 120.1 . . ? C8R C13R H13R 120.1 . . ? C1R C14R C15R 108.6(13) . . ? C1R C14R C16R 111.3(13) . . ? C15R C14R C16R 110.0(13) . . ? C1R C14R H14R 109.0 . . ? C15R C14R H14R 109.0 . . ? C16R C14R H14R 109.0 . . ? C14R C15R H15A 109.5 . . ? C14R C15R H15B 109.5 . . ? H15A C15R H15B 109.5 . . ? C14R C15R H15C 109.5 . . ? H15A C15R H15C 109.5 . . ? H15B C15R H15C 109.5 . . ? C14R C16R H16A 109.5 . . ? C14R C16R H16B 109.5 . . ? H16A C16R H16B 109.5 . . ? C14R C16R H16C 109.5 . . ? H16A C16R H16C 109.5 . . ? H16B C16R H16C 109.5 . . ? C19R C17R C18R 121.6(14) . . ? C19R C17R C3R 116.4(14) . . ? C18R C17R C3R 116.2(13) . . ? C19R C17R H17R 98.1 . . ? C18R C17R H17R 98.1 . . ? C3R C17R H17R 98.1 . . ? C17R C18R H18A 109.5 . . ? C17R C18R H18B 109.5 . . ? H18A C18R H18B 109.5 . . ? C17R C18R H18C 109.5 . . ? H18A C18R H18C 109.5 . . ? H18B C18R H18C 109.5 . . ? C17R C19R H19A 109.5 . . ? C17R C19R H19B 109.5 . . ? H19A C19R H19B 109.5 . . ? C17R C19R H19C 109.5 . . ? H19A C19R H19C 109.5 . . ? H19B C19R H19C 109.5 . . ? C21R C20R C22R 113.6(15) . . ? C21R C20R C5R 112.5(14) . . ? C22R C20R C5R 112.3(15) . . ? C21R C20R H20R 105.9 . . ? C22R C20R H20R 105.9 . . ? C5R C20R H20R 105.9 . . ? C20R C21R H21A 109.5 . . ? C20R C21R H21B 109.5 . . ? H21A C21R H21B 109.5 . . ? C20R C21R H21C 109.5 . . ? H21A C21R H21C 109.5 . . ? H21B C21R H21C 109.5 . . ? C20R C22R H22A 109.5 . . ? C20R C22R H22B 109.5 . . ? H22A C22R H22B 109.5 . . ? C20R C22R H22C 109.5 . . ? H22A C22R H22C 109.5 . . ? H22B C22R H22C 109.5 . . ? O2R C23R N1R 121.4(16) . . ? O2R C23R C11R 118.4(14) . . ? N1R C23R C11R 116.6(14) . . ? N1R C24R C25R 111.0(12) . . ? N1R C24R C27R 112.5(13) . . ? C25R C24R C27R 108.8(12) . . ? N1R C24R H24R 108.1 . . ? C25R C24R H24R 108.1 . . ? C27R C24R H24R 108.1 . . ? O3R C25R O4R 124.1(13) . . ? O3R C25R C24R 123.3(13) . . ? O4R C25R C24R 112.6(12) . . ? C28R C27R C24R 112.7(11) . . ? C28R C27R H27A 109.1 . . ? C24R C27R H27A 109.1 . . ? C28R C27R H27B 109.1 . . ? C24R C27R H27B 109.1 . . ? H27A C27R H27B 107.8 . . ? C29R C28R C33R 117.2 . . ? C29R C28R C27R 120.6(9) . . ? C33R C28R C27R 122.1(9) . . ? C30R C29R C28R 121.3 . . ? C29R C30R C31R 121.0 . . ? C32R C31R C30R 118.1 . . ? C31R C32R C33R 121.2 . . ? C32R C33R C28R 121.2 . . ? C23P N1P C24P 123.3(10) . . ? C23P N1P H1P 118.4 . . ? C24P N1P H1P 118.4 . . ? C25P O4P C26P 116.9(12) . . ? C6P C1P C2P 122.0(9) . . ? C6P C1P C14P 94.3(7) . . ? C2P C1P C14P 143.6(10) . . ? C1P C2P C3P 117.3(10) . . ? C1P C2P H2P 121.3 . . ? C3P C2P H2P 121.3 . . ? C4P C3P C2P 119.0(9) . . ? C4P C3P C17P 121.8(11) . . ? C2P C3P C17P 118.9(11) . . ? C3P C4P C5P 124.1(10) . . ? C3P C4P H4P 118.0 . . ? C5P C4P H4P 118.0 . . ? C6P C5P C4P 114.4(9) . . ? C6P C5P C20P 123.5(9) . . ? C4P C5P C20P 121.7(10) . . ? C1P C6P C5P 122.9(8) . . ? C1P C6P C7P 96.9(7) . . ? C5P C6P C7P 140.2(9) . . ? O1P C7P C6P 112.4(11) . . ? O1P C7P C8P 110.3(9) . . ? C6P C7P C8P 114.7(10) . . ? O1P C7P C14P 115.2(11) . . ? C6P C7P C14P 83.7(6) . . ? C8P C7P C14P 118.2(10) . . ? C9P C8P C13P 116.8(8) . . ? C9P C8P C7P 120.7(8) . . ? C13P C8P C7P 122.5(8) . . ? C8P C9P C10P 121.7(9) . . ? C8P C9P H9P 119.2 . . ? C10P C9P H9P 119.2 . . ? C11P C10P C9P 120.8(10) . . ? C11P C10P H10P 119.6 . . ? C9P C10P H10P 119.6 . . ? C10P C11P C12P 117.3(9) . . ? C10P C11P C23P 122.0(9) . . ? C12P C11P C23P 120.7(9) . . ? C13P C12P C11P 121.7(10) . . ? C13P C12P H12P 119.1 . . ? C11P C12P H12P 119.1 . . ? C12P C13P C8P 121.7(10) . . ? C12P C13P H13P 119.2 . . ? C8P C13P H13P 119.2 . . ? C16P C14P C15P 109.7(10) . . ? C16P C14P C1P 115.0(11) . . ? C15P C14P C1P 112.9(10) . . ? C16P C14P C7P 119.0(10) . . ? C15P C14P C7P 113.6(10) . . ? C1P C14P C7P 84.7(6) . . ? C14P C15P H15D 109.5 . . ? C14P C15P H15E 109.5 . . ? H15D C15P H15E 109.5 . . ? C14P C15P H15F 109.5 . . ? H15D C15P H15F 109.5 . . ? H15E C15P H15F 109.5 . . ? C14P C16P H16D 109.5 . . ? C14P C16P H16E 109.5 . . ? H16D C16P H16E 109.5 . . ? C14P C16P H16F 109.5 . . ? H16D C16P H16F 109.5 . . ? H16E C16P H16F 109.5 . . ? C19P C17P C18P 114.3(14) . . ? C19P C17P C3P 111.9(11) . . ? C18P C17P C3P 113.1(11) . . ? C19P C17P H17P 105.6 . . ? C18P C17P H17P 105.6 . . ? C3P C17P H17P 105.6 . . ? C17P C18P H18D 109.5 . . ? C17P C18P H18E 109.5 . . ? H18D C18P H18E 109.5 . . ? C17P C18P H18F 109.5 . . ? H18D C18P H18F 109.5 . . ? H18E C18P H18F 109.5 . . ? C17P C19P H19D 109.5 . . ? C17P C19P H19E 109.5 . . ? H19D C19P H19E 109.5 . . ? C17P C19P H19F 109.5 . . ? H19D C19P H19F 109.5 . . ? H19E C19P H19F 109.5 . . ? C22P C20P C21P 110.4(13) . . ? C22P C20P C5P 111.1(12) . . ? C21P C20P C5P 110.2(12) . . ? C22P C20P H20P 108.4 . . ? C21P C20P H20P 108.4 . . ? C5P C20P H20P 108.4 . . ? C20P C21P H21D 109.5 . . ? C20P C21P H21E 109.5 . . ? H21D C21P H21E 109.5 . . ? C20P C21P H21F 109.5 . . ? H21D C21P H21F 109.5 . . ? H21E C21P H21F 109.5 . . ? C20P C22P H22D 109.5 . . ? C20P C22P H22E 109.5 . . ? H22D C22P H22E 109.5 . . ? C20P C22P H22F 109.5 . . ? H22D C22P H22F 109.5 . . ? H22E C22P H22F 109.5 . . ? O2P C23P N1P 119.9(10) . . ? O2P C23P C11P 122.6(10) . . ? N1P C23P C11P 117.0(8) . . ? N1P C24P C25P 112.9(9) . . ? N1P C24P C27P 111.9(10) . . ? C25P C24P C27P 111.5(10) . . ? N1P C24P H24P 106.7 . . ? C25P C24P H24P 106.7 . . ? C27P C24P H24P 106.7 . . ? O3P C25P O4P 123.1(11) . . ? O3P C25P C24P 121.2(11) . . ? O4P C25P C24P 115.3(10) . . ? O4P C26P H26D 109.5 . . ? O4P C26P H26E 109.5 . . ? H26D C26P H26E 109.5 . . ? O4P C26P H26F 109.5 . . ? H26D C26P H26F 109.5 . . ? H26E C26P H26F 109.5 . . ? C28P C27P C24P 114.0(9) . . ? C28P C27P H27C 108.8 . . ? C24P C27P H27C 108.8 . . ? C28P C27P H27D 108.8 . . ? C24P C27P H27D 108.8 . . ? H27C C27P H27D 107.6 . . ? C29P C28P C33P 118.0 . . ? C29P C28P C27P 122.7(8) . . ? C33P C28P C27P 119.3(8) . . ? C28P C29P C30P 120.7 . . ? C28P C29P H29P 119.7 . . ? C30P C29P H29P 119.7 . . ? C31P C30P C29P 121.2 . . ? C31P C30P H30P 119.4 . . ? C29P C30P H30P 119.4 . . ? C32P C31P C30P 118.1 . . ? C32P C31P H31P 120.9 . . ? C30P C31P H31P 120.9 . . ? C31P C32P C33P 120.9 . . ? C31P C32P H32P 119.6 . . ? C33P C32P H32P 119.6 . . ? C32P C33P C28P 121.0 . . ? C32P C33P H33P 119.5 . . ? C28P C33P H33P 119.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.173 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.038 #===END data_66.9%P _database_code_depnum_ccdc_archive 'CCDC 799258' #TrackingRef '- 1.cif' #==================================================================== # start Validation Reply Form _vrf_PLAT201_66.9%P ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 18 RESPONSE: In the crystal there are reactant and photoproduct molecules. Part of atoms were refined isotropically in order to decrease a large number of the parameters in the refinement. ; # end Validation Reply Form #==================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 N O4' _chemical_formula_weight 513.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.3364(13) _cell_length_b 11.1836(19) _cell_length_c 28.721(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2998.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 13.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14635 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2980 _reflns_number_gt 1770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSALIS (Oxford Diffraction, 2003)' _computing_cell_refinement 'CRYSALIS (Oxford Diffraction, 2003)' _computing_data_reduction 'CRYSALIS (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Owing to a reactant-product disorder, the following weak restraints from SHELXL97 were applied: DFIX, DANG and SIMU. DFIX and DANG restrained bond lengths and valence angles to target values. The target values were taken from the structures of the pure reactant and the pure product of crystal 1a. SIMU restrained displacement parameters of atoms of the products. ; _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^)+(0.1537P)^2^+0.0809P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration syn _refine_ls_number_reflns 2980 _refine_ls_number_parameters 384 _refine_ls_number_restraints 287 _refine_ls_R_factor_all 0.1461 _refine_ls_R_factor_gt 0.0924 _refine_ls_wR_factor_ref 0.2981 _refine_ls_wR_factor_gt 0.2534 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.302 _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 N1R N 0.725(3) 0.290(2) -0.0019(10) 0.107(10) Uiso 0.331(11) 1 d PDU A 1 H1R H 0.6357 0.2710 -0.0006 0.129 Uiso 0.331(11) 1 calc PR A 1 O1R O 0.512(3) -0.246(3) 0.1040(12) 0.103(15) Uiso 0.331(11) 1 d PDU A 1 O2R O 0.934(3) 0.266(3) 0.0360(15) 0.086(8) Uiso 0.331(11) 1 d PDU A 1 O3R O 0.755(3) 0.5974(19) -0.0087(12) 0.164(11) Uiso 0.331(11) 1 d PD A 1 O4R O 0.572(3) 0.481(2) 0.0063(13) 0.120(8) Uiso 0.331(11) 1 d PDU A 1 C1R C 0.645(2) -0.195(3) 0.1990(6) 0.073(11) Uiso 0.331(11) 1 d PDU A 1 C2R C 0.705(3) -0.242(3) 0.2391(6) 0.095(11) Uiso 0.331(11) 1 d PDU A 1 H2R H 0.6583 -0.2283 0.2673 0.114 Uiso 0.331(11) 1 calc PR A 1 C3R C 0.830(3) -0.306(3) 0.2394(6) 0.093(11) Uiso 0.331(11) 1 d PDU A 1 C4R C 0.904(3) -0.314(3) 0.1981(7) 0.105(12) Uiso 0.331(11) 1 d PDU A 1 H4R H 0.9991 -0.3392 0.1987 0.126 Uiso 0.331(11) 1 calc PR A 1 C5R C 0.841(2) -0.284(2) 0.1547(6) 0.070(8) Uiso 0.331(11) 1 d PDU A 1 C6R C 0.706(3) -0.232(3) 0.1570(5) 0.086(16) Uiso 0.331(11) 1 d PDU A 1 C7R C 0.628(2) -0.2005(16) 0.1129(6) 0.086(8) Uiso 0.331(11) 1 d PDU A 1 C8R C 0.671(2) -0.0890(16) 0.0892(6) 0.061(7) Uiso 0.331(11) 1 d PD A 1 C9R C 0.624(2) -0.0651(18) 0.0442(6) 0.078(8) Uiso 0.331(11) 1 d PD A 1 H9R H 0.5654 -0.1199 0.0289 0.093 Uiso 0.331(11) 1 calc PR A 1 C10R C 0.662(4) 0.039(2) 0.0226(9) 0.083(11) Uiso 0.331(11) 1 d PDU A 1 H10R H 0.6193 0.0605 -0.0054 0.100 Uiso 0.331(11) 1 calc PR A 1 C11R C 0.764(3) 0.1123(19) 0.0422(8) 0.065(7) Uiso 0.331(11) 1 d PDU A 1 C12R C 0.824(3) 0.080(2) 0.0849(8) 0.074(7) Uiso 0.331(11) 1 d PDU A 1 H12R H 0.8958 0.1276 0.0978 0.089 Uiso 0.331(11) 1 calc PR A 1 C13R C 0.779(2) -0.0188(19) 0.1079(7) 0.079(9) Uiso 0.331(11) 1 d PD A 1 H13R H 0.8199 -0.0395 0.1362 0.095 Uiso 0.331(11) 1 calc PR A 1 C14R C 0.514(2) -0.119(2) 0.2026(8) 0.096(8) Uiso 0.331(11) 1 d PDU A 1 H14R H 0.4845 -0.0949 0.1712 0.115 Uiso 0.331(11) 1 calc PR A 1 C15R C 0.395(3) -0.192(3) 0.2244(13) 0.136(11) Uiso 0.331(11) 1 d PDU A 1 H15A H 0.3097 -0.1450 0.2261 0.204 Uiso 0.331(11) 1 calc PR A 1 H15B H 0.4233 -0.2162 0.2552 0.204 Uiso 0.331(11) 1 calc PR A 1 H15C H 0.3777 -0.2621 0.2058 0.204 Uiso 0.331(11) 1 calc PR A 1 C16R C 0.539(3) -0.008(2) 0.2321(13) 0.140(9) Uiso 0.331(11) 1 d PDU A 1 H16A H 0.4530 0.0393 0.2329 0.209 Uiso 0.331(11) 1 calc PR A 1 H16B H 0.6154 0.0384 0.2189 0.209 Uiso 0.331(11) 1 calc PR A 1 H16C H 0.5641 -0.0312 0.2633 0.209 Uiso 0.331(11) 1 calc PR A 1 C17R C 0.899(3) -0.330(3) 0.2853(9) 0.126(9) Uiso 0.331(11) 1 d PDU A 1 H17R H 0.8196 -0.3059 0.3053 0.151 Uiso 0.331(11) 1 calc PR A 1 C18R C 1.005(4) -0.240(3) 0.3008(14) 0.147(14) Uiso 0.331(11) 1 d PDU A 1 H18A H 0.9807 -0.1634 0.2878 0.221 Uiso 0.331(11) 1 calc PR A 1 H18B H 1.0990 -0.2627 0.2904 0.221 Uiso 0.331(11) 1 calc PR A 1 H18C H 1.0043 -0.2349 0.3342 0.221 Uiso 0.331(11) 1 calc PR A 1 C19R C 0.909(5) -0.452(3) 0.3004(15) 0.149(12) Uiso 0.331(11) 1 d PDU A 1 H19A H 0.8302 -0.4967 0.2879 0.224 Uiso 0.331(11) 1 calc PR A 1 H19B H 0.9061 -0.4548 0.3338 0.224 Uiso 0.331(11) 1 calc PR A 1 H19C H 0.9975 -0.4859 0.2896 0.224 Uiso 0.331(11) 1 calc PR A 1 C20R C 0.893(3) -0.339(3) 0.1094(8) 0.118(9) Uiso 0.331(11) 1 d PDU A 1 H20R H 0.8422 -0.2967 0.0844 0.142 Uiso 0.331(11) 1 calc PR A 1 C21R C 0.855(6) -0.468(4) 0.104(2) 0.155(16) Uiso 0.331(11) 1 d PDU A 1 H21A H 0.8907 -0.4974 0.0749 0.232 Uiso 0.331(11) 1 calc PR A 1 H21B H 0.7531 -0.4777 0.1052 0.232 Uiso 0.331(11) 1 calc PR A 1 H21C H 0.8980 -0.5132 0.1291 0.232 Uiso 0.331(11) 1 calc PR A 1 C22R C 1.051(4) -0.316(4) 0.1016(17) 0.133(14) Uiso 0.331(11) 1 d PDU A 1 H22A H 1.0701 -0.2319 0.1041 0.199 Uiso 0.331(11) 1 calc PR A 1 H22B H 1.0781 -0.3437 0.0712 0.199 Uiso 0.331(11) 1 calc PR A 1 H22C H 1.1058 -0.3582 0.1248 0.199 Uiso 0.331(11) 1 calc PR A 1 C23R C 0.821(3) 0.224(3) 0.0216(13) 0.079(5) Uiso 0.331(11) 1 d PDU A 1 C24R C 0.768(3) 0.3918(17) -0.0296(7) 0.087(8) Uiso 0.331(11) 1 d PDU A 1 H24R H 0.8715 0.4024 -0.0254 0.104 Uiso 0.331(11) 1 calc PR A 1 C25R C 0.695(3) 0.5038(18) -0.0120(10) 0.095(12) Uiso 0.331(11) 1 d PD A 1 C26R C 0.481(4) 0.578(4) 0.0193(19) 0.146(11) Uiso 0.331(11) 1 d PDU A 1 H26A H 0.5045 0.6042 0.0502 0.219 Uiso 0.331(11) 1 calc PR A 1 H26B H 0.3826 0.5522 0.0185 0.219 Uiso 0.331(11) 1 calc PR A 1 H26C H 0.4936 0.6430 -0.0022 0.219 Uiso 0.331(11) 1 calc PR A 1 C27R C 0.740(3) 0.373(2) -0.0812(8) 0.107(12) Uiso 0.331(11) 1 d PD A 1 H27A H 0.6385 0.3628 -0.0862 0.129 Uiso 0.331(11) 1 calc PR A 1 H27B H 0.7701 0.4445 -0.0980 0.129 Uiso 0.331(11) 1 calc PR A 1 C28R C 0.818(2) 0.2680(16) -0.1001(7) 0.084(7) Uiso 0.331(11) 1 d PGDU A 1 C29R C 0.7539(18) 0.1575(17) -0.1017(7) 0.104(8) Uiso 0.331(11) 1 d PGD A 1 H29R H 0.6588 0.1500 -0.0926 0.125 Uiso 0.331(11) 1 d PG A 1 C30R C 0.827(2) 0.0583(15) -0.1165(9) 0.131(11) Uiso 0.331(11) 1 d PG A 1 H30R H 0.7811 -0.0155 -0.1169 0.157 Uiso 0.331(11) 1 d PG A 1 C31R C 0.968(2) 0.0662(18) -0.1306(9) 0.118(10) Uiso 0.331(11) 1 d PG A 1 H31R H 1.0179 -0.0014 -0.1401 0.141 Uiso 0.331(11) 1 d PG A 1 C32R C 1.0312(19) 0.176(2) -0.1303(10) 0.116(11) Uiso 0.331(11) 1 d PG A 1 H32R H 1.1253 0.1833 -0.1405 0.140 Uiso 0.331(11) 1 d PG A 1 C33R C 0.959(2) 0.2754(18) -0.1153(9) 0.112(12) Uiso 0.331(11) 1 d PGD A 1 H33R H 1.0049 0.3491 -0.1152 0.135 Uiso 0.331(11) 1 d PG A 1 N1P N 0.7330(11) 0.2717(11) -0.0133(4) 0.082(4) Uani 0.669(11) 1 d PDU A 2 H1P H 0.6520 0.2373 -0.0182 0.098 Uiso 0.669(11) 1 calc PR A 2 O1P O 0.506(2) -0.2415(17) 0.1015(6) 0.112(8) Uani 0.669(11) 1 d PDU A 2 O2P O 0.9360(12) 0.2741(16) 0.0284(7) 0.088(4) Uani 0.669(11) 1 d PDU A 2 O3P O 0.7452(12) 0.5799(10) -0.0474(6) 0.145(5) Uani 0.669(11) 1 d PD A 2 O4P O 0.5941(15) 0.4794(12) -0.0040(6) 0.125(4) Uani 0.669(11) 1 d PDU A 2 C1P C 0.6556(15) -0.2040(16) 0.2001(4) 0.095(7) Uiso 0.669(11) 1 d PDU A 2 C2P C 0.7289(15) -0.2308(15) 0.2404(4) 0.104(7) Uiso 0.669(11) 1 d PDU A 2 H2P H 0.6966 -0.2051 0.2694 0.125 Uiso 0.669(11) 1 calc PR A 2 C3P C 0.8535(16) -0.2983(16) 0.2358(4) 0.108(6) Uiso 0.669(11) 1 d PDU A 2 C4P C 0.8924(16) -0.3391(16) 0.1925(4) 0.100(6) Uiso 0.669(11) 1 d PDU A 2 H4P H 0.9691 -0.3920 0.1905 0.120 Uiso 0.669(11) 1 calc PR A 2 C5P C 0.8232(15) -0.3058(15) 0.1511(4) 0.099(6) Uiso 0.669(11) 1 d PDU A 2 C6P C 0.7042(16) -0.2347(16) 0.1575(4) 0.084(8) Uiso 0.669(11) 1 d PDU A 2 C7P C 0.5921(10) -0.1671(8) 0.1297(3) 0.079(3) Uani 0.669(11) 1 d PDU A 2 C8P C 0.6514(12) -0.0628(10) 0.1015(4) 0.074(4) Uiso 0.669(11) 1 d PD A 2 C9P C 0.6037(11) -0.0404(9) 0.0572(4) 0.065(3) Uiso 0.669(11) 1 d PD A 2 H9P H 0.5327 -0.0891 0.0447 0.078 Uiso 0.669(11) 1 calc PR A 2 C10P C 0.6573(16) 0.0514(12) 0.0309(4) 0.077(5) Uiso 0.669(11) 1 d PDU A 2 H10P H 0.6240 0.0621 0.0007 0.092 Uiso 0.669(11) 1 calc PR A 2 C11P C 0.7594(16) 0.1282(11) 0.0483(4) 0.067(4) Uiso 0.669(11) 1 d PDU A 2 C12P C 0.8122(14) 0.1029(11) 0.0922(4) 0.073(4) Uiso 0.669(11) 1 d PDU A 2 H12P H 0.8847 0.1504 0.1045 0.087 Uiso 0.669(11) 1 calc PR A 2 C13P C 0.7602(12) 0.0098(10) 0.1178(4) 0.073(4) Uiso 0.669(11) 1 d PD A 2 H13P H 0.7990 -0.0052 0.1470 0.088 Uiso 0.669(11) 1 calc PR A 2 C14P C 0.5265(10) -0.1354(9) 0.1817(4) 0.094(4) Uani 0.669(11) 1 d PDU A 2 C15P C 0.3839(11) -0.1989(13) 0.1898(5) 0.115(5) Uani 0.669(11) 1 d PDU A 2 H15D H 0.3922 -0.2811 0.1806 0.172 Uiso 0.669(11) 1 calc PR A 2 H15E H 0.3105 -0.1608 0.1717 0.172 Uiso 0.669(11) 1 calc PR A 2 H15F H 0.3594 -0.1946 0.2222 0.172 Uiso 0.669(11) 1 calc PR A 2 C16P C 0.5138(15) -0.0075(8) 0.1965(5) 0.107(4) Uani 0.669(11) 1 d PDU A 2 H16D H 0.4303 0.0273 0.1825 0.161 Uiso 0.669(11) 1 calc PR A 2 H16E H 0.5974 0.0357 0.1866 0.161 Uiso 0.669(11) 1 calc PR A 2 H16F H 0.5057 -0.0036 0.2298 0.161 Uiso 0.669(11) 1 calc PR A 2 C17P C 0.9339(17) -0.3386(13) 0.2802(5) 0.133(6) Uani 0.669(11) 1 d PDU A 2 H17P H 0.8769 -0.3098 0.3066 0.160 Uiso 0.669(11) 1 calc PR A 2 C18P C 1.0740(19) -0.280(2) 0.2840(7) 0.166(8) Uani 0.669(11) 1 d PDU A 2 H18D H 1.0616 -0.1945 0.2818 0.249 Uiso 0.669(11) 1 calc PR A 2 H18E H 1.1351 -0.3065 0.2593 0.249 Uiso 0.669(11) 1 calc PR A 2 H18F H 1.1168 -0.2990 0.3134 0.249 Uiso 0.669(11) 1 calc PR A 2 C19P C 0.939(2) -0.4673(14) 0.2845(7) 0.166(8) Uani 0.669(11) 1 d PDU A 2 H19D H 0.8435 -0.4990 0.2819 0.249 Uiso 0.669(11) 1 calc PR A 2 H19E H 0.9782 -0.4885 0.3142 0.249 Uiso 0.669(11) 1 calc PR A 2 H19F H 0.9975 -0.4998 0.2602 0.249 Uiso 0.669(11) 1 calc PR A 2 C20P C 0.8841(17) -0.3309(16) 0.1033(5) 0.134(6) Uani 0.669(11) 1 d PDU A 2 H20P H 0.8196 -0.2939 0.0806 0.161 Uiso 0.669(11) 1 calc PR A 2 C21P C 0.886(3) -0.4630(18) 0.0933(10) 0.167(9) Uani 0.669(11) 1 d PDU A 2 H21D H 0.9221 -0.4761 0.0623 0.251 Uiso 0.669(11) 1 calc PR A 2 H21E H 0.7911 -0.4945 0.0957 0.251 Uiso 0.669(11) 1 calc PR A 2 H21F H 0.9475 -0.5025 0.1153 0.251 Uiso 0.669(11) 1 calc PR A 2 C22P C 1.029(2) -0.276(2) 0.0966(10) 0.186(11) Uani 0.669(11) 1 d PDU A 2 H22D H 1.0633 -0.2927 0.0658 0.278 Uiso 0.669(11) 1 calc PR A 2 H22E H 1.0950 -0.3080 0.1190 0.278 Uiso 0.669(11) 1 calc PR A 2 H22F H 1.0228 -0.1905 0.1008 0.278 Uiso 0.669(11) 1 calc PR A 2 C23P C 0.8156(14) 0.2323(14) 0.0223(6) 0.084(3) Uani 0.669(11) 1 d PDU A 2 C24P C 0.7746(13) 0.3684(9) -0.0432(4) 0.088(4) Uani 0.669(11) 1 d PDU A 2 H24P H 0.8783 0.3781 -0.0394 0.106 Uiso 0.669(11) 1 calc PR A 2 C25P C 0.7081(12) 0.4854(10) -0.0304(6) 0.100(4) Uani 0.669(11) 1 d PD A 2 C26P C 0.524(3) 0.5878(16) 0.0096(8) 0.159(7) Uani 0.669(11) 1 d PDU A 2 H26D H 0.4962 0.5825 0.0417 0.239 Uiso 0.669(11) 1 calc PR A 2 H26E H 0.4404 0.5996 -0.0094 0.239 Uiso 0.669(11) 1 calc PR A 2 H26F H 0.5882 0.6540 0.0055 0.239 Uiso 0.669(11) 1 calc PR A 2 C27P C 0.7491(14) 0.3384(11) -0.0941(4) 0.090(4) Uani 0.669(11) 1 d PD A 2 H27C H 0.6479 0.3224 -0.0985 0.108 Uiso 0.669(11) 1 calc PR A 2 H27D H 0.7730 0.4080 -0.1127 0.108 Uiso 0.669(11) 1 calc PR A 2 C28P C 0.8308(10) 0.2358(8) -0.1118(4) 0.085(4) Uiso 0.669(11) 1 d PGDU A 2 C29P C 0.7678(10) 0.1273(9) -0.1199(4) 0.121(5) Uiso 0.669(11) 1 d PGD A 2 H29P H 0.6708 0.1171 -0.1137 0.145 Uiso 0.669(11) 1 d PG A 2 C30P C 0.8465(14) 0.0332(8) -0.1372(5) 0.146(6) Uiso 0.669(11) 1 d PG A 2 H30P H 0.8025 -0.0406 -0.1415 0.175 Uiso 0.669(11) 1 d PG A 2 C31P C 0.9883(14) 0.0461(10) -0.1482(5) 0.154(7) Uiso 0.669(11) 1 d PG A 2 H31P H 1.0406 -0.0173 -0.1605 0.185 Uiso 0.669(11) 1 d PG A 2 C32P C 1.0510(10) 0.1549(12) -0.1407(5) 0.137(7) Uiso 0.669(11) 1 d PG A 2 H32P H 1.1471 0.1658 -0.1481 0.164 Uiso 0.669(11) 1 d PG A 2 C33P C 0.9738(11) 0.2484(10) -0.1224(5) 0.095(5) Uiso 0.669(11) 1 d PGD A 2 H33P H 1.0188 0.3213 -0.1171 0.115 Uiso 0.669(11) 1 d PG 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 N1P 0.049(4) 0.110(8) 0.085(8) 0.044(7) -0.002(4) 0.003(5) O1P 0.122(11) 0.099(9) 0.116(10) 0.008(5) -0.029(6) -0.040(7) O2P 0.041(4) 0.124(8) 0.099(9) 0.039(6) -0.002(4) 0.002(4) O3P 0.122(8) 0.104(8) 0.208(15) 0.044(8) 0.035(9) 0.022(7) O4P 0.122(8) 0.132(8) 0.121(9) -0.008(6) 0.068(7) -0.011(7) C7P 0.085(7) 0.079(7) 0.073(7) -0.008(6) -0.012(6) 0.007(6) C14P 0.080(7) 0.093(9) 0.111(10) 0.012(7) 0.020(7) 0.023(7) C15P 0.095(9) 0.128(11) 0.120(12) 0.011(9) 0.034(8) -0.004(8) C16P 0.114(9) 0.090(8) 0.118(10) 0.031(7) 0.041(8) 0.031(7) C17P 0.140(12) 0.166(13) 0.094(9) 0.080(9) 0.004(9) 0.056(11) C18P 0.124(13) 0.22(2) 0.158(16) 0.090(15) -0.015(12) -0.020(15) C19P 0.153(13) 0.196(14) 0.149(15) 0.113(12) 0.010(11) 0.064(12) C20P 0.107(10) 0.160(13) 0.135(11) 0.047(10) 0.041(8) 0.076(9) C21P 0.19(2) 0.137(15) 0.170(19) -0.034(13) 0.065(15) 0.070(14) C22P 0.171(18) 0.22(2) 0.170(17) 0.070(17) 0.069(16) 0.037(18) C23P 0.064(5) 0.096(7) 0.092(6) 0.030(6) 0.031(5) 0.042(6) C24P 0.063(6) 0.111(9) 0.089(9) 0.019(8) -0.002(6) 0.000(7) C25P 0.088(9) 0.096(12) 0.117(15) 0.001(10) -0.006(9) -0.009(8) C26P 0.186(15) 0.131(11) 0.161(14) 0.015(10) 0.101(12) 0.033(12) C27P 0.077(7) 0.113(10) 0.080(8) 0.032(8) -0.013(7) -0.016(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1R C23R 1.339(11) . ? N1R C24R 1.446(11) . ? N1R H1R 0.8600 . ? O1R C7R 1.229(11) . ? O2R C23R 1.225(10) . ? O3R C25R 1.190(10) . ? O4R C25R 1.289(11) . ? O4R C26R 1.431(11) . ? C1R C2R 1.381(10) . ? C1R C6R 1.397(10) . ? C1R C14R 1.494(10) . ? C2R C3R 1.371(10) . ? C2R H2R 0.9300 . ? C3R C4R 1.377(10) . ? C3R C17R 1.494(10) . ? C4R C5R 1.421(10) . ? C4R H4R 0.9300 . ? C5R C6R 1.387(10) . ? C5R C20R 1.519(10) . ? C6R C7R 1.502(10) . ? C7R C8R 1.477(10) . ? C8R C13R 1.382(10) . ? C8R C9R 1.391(10) . ? C9R C10R 1.369(10) . ? C9R H9R 0.9300 . ? C10R C11R 1.377(10) . ? C10R H10R 0.9300 . ? C11R C12R 1.394(10) . ? C11R C23R 1.484(10) . ? C12R C13R 1.359(10) . ? C12R H12R 0.9300 . ? C13R H13R 0.9300 . ? C14R C15R 1.512(11) . ? C14R C16R 1.527(11) . ? C14R H14R 0.9800 . ? C15R H15A 0.9600 . ? C15R H15B 0.9600 . ? C15R H15C 0.9600 . ? C16R H16A 0.9600 . ? C16R H16B 0.9600 . ? C16R H16C 0.9600 . ? C17R C19R 1.429(11) . ? C17R C18R 1.484(11) . ? C17R H17R 0.9800 . ? C18R H18A 0.9600 . ? C18R H18B 0.9600 . ? C18R H18C 0.9600 . ? C19R H19A 0.9600 . ? C19R H19B 0.9600 . ? C19R H19C 0.9600 . ? C20R C21R 1.497(11) . ? C20R C22R 1.519(11) . ? C20R H20R 0.9800 . ? C21R H21A 0.9600 . ? C21R H21B 0.9600 . ? C21R H21C 0.9600 . ? C22R H22A 0.9600 . ? C22R H22B 0.9600 . ? C22R H22C 0.9600 . ? C24R C25R 1.513(10) . ? C24R C27R 1.518(11) . ? C24R H24R 0.9800 . ? C26R H26A 0.9600 . ? C26R H26B 0.9600 . ? C26R H26C 0.9600 . ? C27R C28R 1.489(10) . ? C27R H27A 0.9700 . ? C27R H27B 0.9700 . ? C28R C29R 1.3754 . ? C28R C33R 1.3831 . ? C29R C30R 1.3701 . ? C29R H29R 0.9300 . ? C30R C31R 1.3771 . ? C30R H30R 0.9300 . ? C31R C32R 1.3617 . ? C31R H31R 0.9300 . ? C32R C33R 1.3726 . ? C32R H32R 0.9300 . ? C33R H33R 0.9300 . ? N1P C23P 1.354(9) . ? N1P C24P 1.434(8) . ? N1P H1P 0.8600 . ? O1P C7P 1.409(9) . ? O2P C23P 1.230(8) . ? O3P C25P 1.215(9) . ? O4P C25P 1.309(9) . ? O4P C26P 1.432(10) . ? C1P C6P 1.351(9) . ? C1P C2P 1.377(9) . ? C1P C14P 1.524(9) . ? C2P C3P 1.393(9) . ? C2P H2P 0.9300 . ? C3P C4P 1.373(9) . ? C3P C17P 1.548(9) . ? C4P C5P 1.404(9) . ? C4P H4P 0.9300 . ? C5P C6P 1.379(8) . ? C5P C20P 1.512(9) . ? C6P C7P 1.518(8) . ? C7P C8P 1.524(8) . ? C7P C14P 1.652(9) . ? C8P C9P 1.369(9) . ? C8P C13P 1.383(9) . ? C9P C10P 1.371(9) . ? C9P H9P 0.9300 . ? C10P C11P 1.377(9) . ? C10P H10P 0.9300 . ? C11P C12P 1.382(8) . ? C11P C23P 1.480(8) . ? C12P C13P 1.364(9) . ? C12P H12P 0.9300 . ? C13P H13P 0.9300 . ? C14P C16P 1.497(9) . ? C14P C15P 1.527(9) . ? C15P H15D 0.9600 . ? C15P H15E 0.9600 . ? C15P H15F 0.9600 . ? C16P H16D 0.9600 . ? C16P H16E 0.9600 . ? C16P H16F 0.9600 . ? C17P C19P 1.445(10) . ? C17P C18P 1.469(10) . ? C17P H17P 0.9800 . ? C18P H18D 0.9600 . ? C18P H18E 0.9600 . ? C18P H18F 0.9600 . ? C19P H19D 0.9600 . ? C19P H19E 0.9600 . ? C19P H19F 0.9600 . ? C20P C22P 1.504(10) . ? C20P C21P 1.505(10) . ? C20P H20P 0.9800 . ? C21P H21D 0.9600 . ? C21P H21E 0.9600 . ? C21P H21F 0.9600 . ? C22P H22D 0.9600 . ? C22P H22E 0.9600 . ? C22P H22F 0.9600 . ? C24P C25P 1.494(9) . ? C24P C27P 1.520(9) . ? C24P H24P 0.9800 . ? C26P H26D 0.9600 . ? C26P H26E 0.9600 . ? C26P H26F 0.9600 . ? C27P C28P 1.468(9) . ? C27P H27C 0.9700 . ? C27P H27D 0.9700 . ? C28P C29P 1.3689 . ? C28P C33P 1.3759 . ? C29P C30P 1.3762 . ? C29P H29P 0.9300 . ? C30P C31P 1.3693 . ? C30P H30P 0.9300 . ? C31P C32P 1.3674 . ? C31P H31P 0.9300 . ? C32P C33P 1.3743 . ? C32P H32P 0.9300 . ? C33P H33P 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23R N1R C24R 121.4(18) . . ? C23R N1R H1R 119.3 . . ? C24R N1R H1R 119.3 . . ? C25R O4R C26R 119.0(18) . . ? C2R C1R C6R 116.6(11) . . ? C2R C1R C14R 119.1(12) . . ? C6R C1R C14R 124.1(12) . . ? C3R C2R C1R 123.0(12) . . ? C3R C2R H2R 118.5 . . ? C1R C2R H2R 118.5 . . ? C2R C3R C4R 117.2(12) . . ? C2R C3R C17R 118.0(14) . . ? C4R C3R C17R 121.8(14) . . ? C3R C4R C5R 122.0(13) . . ? C3R C4R H4R 119.0 . . ? C5R C4R H4R 119.0 . . ? C6R C5R C4R 115.9(11) . . ? C6R C5R C20R 119.9(13) . . ? C4R C5R C20R 121.7(14) . . ? C5R C6R C1R 122.2(11) . . ? C5R C6R C7R 119.9(12) . . ? C1R C6R C7R 117.5(12) . . ? O1R C7R C8R 119.8(16) . . ? O1R C7R C6R 120.4(16) . . ? C8R C7R C6R 117.1(14) . . ? C13R C8R C9R 118.9(11) . . ? C13R C8R C7R 119.8(11) . . ? C9R C8R C7R 120.2(11) . . ? C10R C9R C8R 120.0(13) . . ? C10R C9R H9R 120.0 . . ? C8R C9R H9R 120.0 . . ? C9R C10R C11R 120.2(13) . . ? C9R C10R H10R 119.9 . . ? C11R C10R H10R 119.9 . . ? C10R C11R C12R 119.0(11) . . ? C10R C11R C23R 125.9(12) . . ? C12R C11R C23R 115.1(12) . . ? C13R C12R C11R 120.7(12) . . ? C13R C12R H12R 119.6 . . ? C11R C12R H12R 119.6 . . ? C12R C13R C8R 120.1(12) . . ? C12R C13R H13R 120.0 . . ? C8R C13R H13R 120.0 . . ? C1R C14R C15R 108.8(14) . . ? C1R C14R C16R 112.2(14) . . ? C15R C14R C16R 108.8(14) . . ? C1R C14R H14R 109.0 . . ? C15R C14R H14R 109.0 . . ? C16R C14R H14R 109.0 . . ? C14R C15R H15A 109.5 . . ? C14R C15R H15B 109.5 . . ? H15A C15R H15B 109.5 . . ? C14R C15R H15C 109.5 . . ? H15A C15R H15C 109.5 . . ? H15B C15R H15C 109.5 . . ? C14R C16R H16A 109.5 . . ? C14R C16R H16B 109.5 . . ? H16A C16R H16B 109.5 . . ? C14R C16R H16C 109.5 . . ? H16A C16R H16C 109.5 . . ? H16B C16R H16C 109.5 . . ? C19R C17R C18R 121.0(16) . . ? C19R C17R C3R 117.8(16) . . ? C18R C17R C3R 115.6(15) . . ? C19R C17R H17R 97.9 . . ? C18R C17R H17R 97.9 . . ? C3R C17R H17R 97.9 . . ? C17R C18R H18A 109.5 . . ? C17R C18R H18B 109.5 . . ? H18A C18R H18B 109.5 . . ? C17R C18R H18C 109.5 . . ? H18A C18R H18C 109.5 . . ? H18B C18R H18C 109.5 . . ? C17R C19R H19A 109.5 . . ? C17R C19R H19B 109.5 . . ? H19A C19R H19B 109.5 . . ? C17R C19R H19C 109.5 . . ? H19A C19R H19C 109.5 . . ? H19B C19R H19C 109.5 . . ? C21R C20R C22R 112.1(16) . . ? C21R C20R C5R 113.7(16) . . ? C22R C20R C5R 111.6(15) . . ? C21R C20R H20R 106.3 . . ? C22R C20R H20R 106.3 . . ? C5R C20R H20R 106.3 . . ? C20R C21R H21A 109.5 . . ? C20R C21R H21B 109.5 . . ? H21A C21R H21B 109.5 . . ? C20R C21R H21C 109.5 . . ? H21A C21R H21C 109.5 . . ? H21B C21R H21C 109.5 . . ? C20R C22R H22A 109.5 . . ? C20R C22R H22B 109.5 . . ? H22A C22R H22B 109.5 . . ? C20R C22R H22C 109.5 . . ? H22A C22R H22C 109.5 . . ? H22B C22R H22C 109.5 . . ? O2R C23R N1R 122.6(17) . . ? O2R C23R C11R 119.5(15) . . ? N1R C23R C11R 115.2(14) . . ? N1R C24R C25R 110.1(14) . . ? N1R C24R C27R 112.5(16) . . ? C25R C24R C27R 111.1(14) . . ? N1R C24R H24R 107.7 . . ? C25R C24R H24R 107.7 . . ? C27R C24R H24R 107.7 . . ? O3R C25R O4R 124.1(16) . . ? O3R C25R C24R 122.9(16) . . ? O4R C25R C24R 111.9(14) . . ? C28R C27R C24R 112.4(14) . . ? C28R C27R H27A 109.1 . . ? C24R C27R H27A 109.1 . . ? C28R C27R H27B 109.1 . . ? C24R C27R H27B 109.1 . . ? H27A C27R H27B 107.9 . . ? C29R C28R C33R 117.2 . . ? C29R C28R C27R 120.7(12) . . ? C33R C28R C27R 122.0(12) . . ? C30R C29R C28R 121.3 . . ? C29R C30R C31R 121.0 . . ? C32R C31R C30R 118.1 . . ? C31R C32R C33R 121.2 . . ? C32R C33R C28R 121.2 . . ? C23P N1P C24P 122.9(8) . . ? C23P N1P H1P 118.6 . . ? C24P N1P H1P 118.6 . . ? C25P O4P C26P 119.1(11) . . ? C6P C1P C2P 122.7(9) . . ? C6P C1P C14P 94.5(7) . . ? C2P C1P C14P 142.7(9) . . ? C1P C2P C3P 116.9(9) . . ? C1P C2P H2P 121.5 . . ? C3P C2P H2P 121.5 . . ? C4P C3P C2P 119.2(9) . . ? C4P C3P C17P 121.4(10) . . ? C2P C3P C17P 118.9(10) . . ? C3P C4P C5P 123.8(10) . . ? C3P C4P H4P 118.1 . . ? C5P C4P H4P 118.1 . . ? C6P C5P C4P 114.3(8) . . ? C6P C5P C20P 122.0(9) . . ? C4P C5P C20P 123.1(9) . . ? C1P C6P C5P 122.5(8) . . ? C1P C6P C7P 96.8(7) . . ? C5P C6P C7P 140.7(9) . . ? O1P C7P C6P 113.6(10) . . ? O1P C7P C8P 110.7(8) . . ? C6P C7P C8P 114.2(9) . . ? O1P C7P C14P 115.8(10) . . ? C6P C7P C14P 83.5(6) . . ? C8P C7P C14P 116.8(8) . . ? C9P C8P C13P 116.5(7) . . ? C9P C8P C7P 121.0(7) . . ? C13P C8P C7P 122.4(8) . . ? C8P C9P C10P 122.0(9) . . ? C8P C9P H9P 119.0 . . ? C10P C9P H9P 119.0 . . ? C9P C10P C11P 121.3(9) . . ? C9P C10P H10P 119.4 . . ? C11P C10P H10P 119.4 . . ? C10P C11P C12P 116.8(8) . . ? C10P C11P C23P 123.5(8) . . ? C12P C11P C23P 119.7(8) . . ? C13P C12P C11P 121.4(9) . . ? C13P C12P H12P 119.3 . . ? C11P C12P H12P 119.3 . . ? C12P C13P C8P 121.8(8) . . ? C12P C13P H13P 119.1 . . ? C8P C13P H13P 119.1 . . ? C16P C14P C1P 116.4(10) . . ? C16P C14P C15P 109.4(9) . . ? C1P C14P C15P 113.8(9) . . ? C16P C14P C7P 119.4(8) . . ? C1P C14P C7P 85.0(6) . . ? C15P C14P C7P 111.2(8) . . ? C14P C15P H15D 109.5 . . ? C14P C15P H15E 109.5 . . ? H15D C15P H15E 109.5 . . ? C14P C15P H15F 109.5 . . ? H15D C15P H15F 109.5 . . ? H15E C15P H15F 109.5 . . ? C14P C16P H16D 109.5 . . ? C14P C16P H16E 109.5 . . ? H16D C16P H16E 109.5 . . ? C14P C16P H16F 109.5 . . ? H16D C16P H16F 109.5 . . ? H16E C16P H16F 109.5 . . ? C19P C17P C18P 114.4(13) . . ? C19P C17P C3P 112.0(11) . . ? C18P C17P C3P 111.2(11) . . ? C19P C17P H17P 106.2 . . ? C18P C17P H17P 106.2 . . ? C3P C17P H17P 106.2 . . ? C17P C18P H18D 109.5 . . ? C17P C18P H18E 109.5 . . ? H18D C18P H18E 109.5 . . ? C17P C18P H18F 109.5 . . ? H18D C18P H18F 109.5 . . ? H18E C18P H18F 109.5 . . ? C17P C19P H19D 109.5 . . ? C17P C19P H19E 109.5 . . ? H19D C19P H19E 109.5 . . ? C17P C19P H19F 109.5 . . ? H19D C19P H19F 109.5 . . ? H19E C19P H19F 109.5 . . ? C22P C20P C21P 111.5(12) . . ? C22P C20P C5P 112.3(12) . . ? C21P C20P C5P 111.2(11) . . ? C22P C20P H20P 107.2 . . ? C21P C20P H20P 107.2 . . ? C5P C20P H20P 107.2 . . ? C20P C21P H21D 109.5 . . ? C20P C21P H21E 109.5 . . ? H21D C21P H21E 109.5 . . ? C20P C21P H21F 109.5 . . ? H21D C21P H21F 109.5 . . ? H21E C21P H21F 109.5 . . ? C20P C22P H22D 109.5 . . ? C20P C22P H22E 109.5 . . ? H22D C22P H22E 109.5 . . ? C20P C22P H22F 109.5 . . ? H22D C22P H22F 109.5 . . ? H22E C22P H22F 109.5 . . ? O2P C23P N1P 120.4(9) . . ? O2P C23P C11P 123.4(9) . . ? N1P C23P C11P 115.8(8) . . ? N1P C24P C25P 113.6(9) . . ? N1P C24P C27P 111.6(9) . . ? C25P C24P C27P 111.4(9) . . ? N1P C24P H24P 106.6 . . ? C25P C24P H24P 106.6 . . ? C27P C24P H24P 106.6 . . ? O3P C25P O4P 120.6(10) . . ? O3P C25P C24P 123.1(11) . . ? O4P C25P C24P 115.8(9) . . ? O4P C26P H26D 109.5 . . ? O4P C26P H26E 109.5 . . ? H26D C26P H26E 109.5 . . ? O4P C26P H26F 109.5 . . ? H26D C26P H26F 109.5 . . ? H26E C26P H26F 109.5 . . ? C28P C27P C24P 115.1(8) . . ? C28P C27P H27C 108.5 . . ? C24P C27P H27C 108.5 . . ? C28P C27P H27D 108.5 . . ? C24P C27P H27D 108.5 . . ? H27C C27P H27D 107.5 . . ? C29P C28P C33P 118.0 . . ? C29P C28P C27P 121.9(7) . . ? C33P C28P C27P 120.0(7) . . ? C28P C29P C30P 120.7 . . ? C28P C29P H29P 119.7 . . ? C30P C29P H29P 119.7 . . ? C31P C30P C29P 121.2 . . ? C31P C30P H30P 119.4 . . ? C29P C30P H30P 119.4 . . ? C32P C31P C30P 118.1 . . ? C32P C31P H31P 120.9 . . ? C30P C31P H31P 120.9 . . ? C31P C32P C33P 120.9 . . ? C31P C32P H32P 119.6 . . ? C33P C32P H32P 119.6 . . ? C32P C33P C28P 121.0 . . ? C32P C33P H33P 119.5 . . ? C28P C33P H33P 119.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.213 _refine_diff_density_min -0.155 _refine_diff_density_rms 0.037 #===END data_79.9%P _database_code_depnum_ccdc_archive 'CCDC 799259' #TrackingRef '- 1.cif' #==================================================================== # start Validation Reply Form _vrf_PLAT201_79.9%P ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 18 RESPONSE: In the crystal there are reactant and photoproduct molecules. Part of atoms were refined isotropically in order to decrease a large number of the parameters in the refinement. ; # end Validation Reply Form #==================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 N O4' _chemical_formula_weight 513.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.3006(12) _cell_length_b 11.3515(16) _cell_length_c 28.334(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2991.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 13.4 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14608 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 4.02 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2979 _reflns_number_gt 1900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSALIS (Oxford Diffraction, 2003)' _computing_cell_refinement 'CRYSALIS (Oxford Diffraction, 2003)' _computing_data_reduction 'CRYSALIS (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Owing to a reactant-product disorder, the following weak restraints from SHELXL97 were applied: DFIX, DANG and SIMU. DFIX and DANG restrained bond lengths and valence angles to target values. The target values were taken from the structures of the pure reactant and the pure product of crystal 1a. SIMU restrained displacement parameters of atoms of the products. ; _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^)+(0.1291P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration syn _refine_ls_number_reflns 2979 _refine_ls_number_parameters 384 _refine_ls_number_restraints 303 _refine_ls_R_factor_all 0.1245 _refine_ls_R_factor_gt 0.0816 _refine_ls_wR_factor_ref 0.2429 _refine_ls_wR_factor_gt 0.2102 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.257 _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 N1R N 0.720(4) 0.285(3) -0.0022(13) 0.092(11) Uiso 0.201(10) 1 d PDU A 1 H1R H 0.6310 0.2662 -0.0009 0.110 Uiso 0.201(10) 1 calc PR A 1 O1R O 0.510(4) -0.245(4) 0.1035(15) 0.076(13) Uiso 0.201(10) 1 d PDU A 1 O2R O 0.925(5) 0.267(4) 0.039(2) 0.073(13) Uiso 0.201(10) 1 d PDU A 1 O3R O 0.756(4) 0.590(2) -0.0154(15) 0.139(15) Uiso 0.201(10) 1 d PD A 1 O4R O 0.568(4) 0.486(4) 0.002(2) 0.101(10) Uiso 0.201(10) 1 d PDU A 1 C1R C 0.639(3) -0.208(3) 0.1978(7) 0.071(15) Uiso 0.201(10) 1 d PDU A 1 C2R C 0.697(3) -0.258(3) 0.2381(7) 0.066(11) Uiso 0.201(10) 1 d PD A 1 H2R H 0.6481 -0.2488 0.2665 0.080 Uiso 0.201(10) 1 calc PR A 1 C3R C 0.824(3) -0.319(3) 0.2378(8) 0.072(11) Uiso 0.201(10) 1 d PDU A 1 C4R C 0.903(3) -0.320(4) 0.1969(8) 0.096(14) Uiso 0.201(10) 1 d PDU A 1 H4R H 0.9985 -0.3442 0.1980 0.115 Uiso 0.201(10) 1 calc PR A 1 C5R C 0.842(3) -0.287(3) 0.1531(7) 0.066(11) Uiso 0.201(10) 1 d PDU A 1 C6R C 0.710(3) -0.232(3) 0.1554(7) 0.073(17) Uiso 0.201(10) 1 d PDU A 1 C7R C 0.630(3) -0.203(2) 0.1106(8) 0.098(10) Uiso 0.201(10) 1 d PDU A 1 C8R C 0.676(3) -0.094(2) 0.0864(8) 0.074(11) Uiso 0.201(10) 1 d PD A 1 C9R C 0.623(3) -0.066(2) 0.0422(8) 0.066(10) Uiso 0.201(10) 1 d PD A 1 H9R H 0.5552 -0.1142 0.0278 0.079 Uiso 0.201(10) 1 calc PR A 1 C10R C 0.670(3) 0.034(2) 0.0194(9) 0.081(12) Uiso 0.201(10) 1 d PDU A 1 H10R H 0.6385 0.0504 -0.0110 0.098 Uiso 0.201(10) 1 calc PR A 1 C11R C 0.765(4) 0.108(2) 0.0416(10) 0.065(18) Uiso 0.201(10) 1 d PD A 1 C12R C 0.825(3) 0.075(2) 0.0847(9) 0.049(9) Uiso 0.201(10) 1 d PDU A 1 H12R H 0.8931 0.1237 0.0991 0.058 Uiso 0.201(10) 1 calc PR A 1 C13R C 0.785(3) -0.027(2) 0.1060(9) 0.073(11) Uiso 0.201(10) 1 d PD A 1 H13R H 0.8299 -0.0510 0.1336 0.087 Uiso 0.201(10) 1 calc PR A 1 C14R C 0.512(3) -0.128(3) 0.2027(10) 0.103(11) Uiso 0.201(10) 1 d PDU A 1 H14R H 0.4748 -0.1102 0.1711 0.124 Uiso 0.201(10) 1 calc PR A 1 C15R C 0.397(3) -0.191(4) 0.2305(18) 0.138(14) Uiso 0.201(10) 1 d PDU A 1 H15A H 0.3123 -0.1430 0.2319 0.207 Uiso 0.201(10) 1 calc PR A 1 H15B H 0.4312 -0.2060 0.2619 0.207 Uiso 0.201(10) 1 calc PR A 1 H15C H 0.3747 -0.2644 0.2153 0.207 Uiso 0.201(10) 1 calc PR A 1 C16R C 0.550(5) -0.012(3) 0.227(2) 0.149(16) Uiso 0.201(10) 1 d PDU A 1 H16A H 0.4663 0.0373 0.2283 0.224 Uiso 0.201(10) 1 calc PR A 1 H16B H 0.6243 0.0274 0.2094 0.224 Uiso 0.201(10) 1 calc PR A 1 H16C H 0.5836 -0.0276 0.2584 0.224 Uiso 0.201(10) 1 calc PR A 1 C17R C 0.893(4) -0.345(4) 0.2845(10) 0.118(11) Uiso 0.201(10) 1 d PDU A 1 H17R H 0.8116 -0.3310 0.3059 0.142 Uiso 0.201(10) 1 calc PR A 1 C18R C 0.996(6) -0.254(6) 0.301(2) 0.17(2) Uiso 0.201(10) 1 d PDU A 1 H18A H 0.9703 -0.1791 0.2880 0.255 Uiso 0.201(10) 1 calc PR A 1 H18B H 1.0914 -0.2748 0.2911 0.255 Uiso 0.201(10) 1 calc PR A 1 H18C H 0.9932 -0.2498 0.3350 0.255 Uiso 0.201(10) 1 calc PR A 1 C19R C 0.924(10) -0.467(4) 0.295(3) 0.146(19) Uiso 0.201(10) 1 d PDU A 1 H19A H 0.8473 -0.5156 0.2836 0.219 Uiso 0.201(10) 1 calc PR A 1 H19B H 0.9318 -0.4761 0.3288 0.219 Uiso 0.201(10) 1 calc PR A 1 H19C H 1.0124 -0.4889 0.2804 0.219 Uiso 0.201(10) 1 calc PR A 1 C20R C 0.891(4) -0.347(3) 0.1078(10) 0.092(10) Uiso 0.201(10) 1 d PDU A 1 H20R H 0.8361 -0.3117 0.0818 0.110 Uiso 0.201(10) 1 calc PR A 1 C21R C 0.860(7) -0.476(4) 0.108(2) 0.15(2) Uiso 0.201(10) 1 d PDU A 1 H21A H 0.8931 -0.5106 0.0789 0.232 Uiso 0.201(10) 1 calc PR A 1 H21B H 0.7579 -0.4884 0.1107 0.232 Uiso 0.201(10) 1 calc PR A 1 H21C H 0.9079 -0.5128 0.1340 0.232 Uiso 0.201(10) 1 calc PR A 1 C22R C 1.049(5) -0.322(5) 0.098(2) 0.109(16) Uiso 0.201(10) 1 d PDU A 1 H22A H 1.0669 -0.2391 0.1005 0.163 Uiso 0.201(10) 1 calc PR A 1 H22B H 1.0729 -0.3485 0.0668 0.163 Uiso 0.201(10) 1 calc PR A 1 H22C H 1.1072 -0.3633 0.1207 0.163 Uiso 0.201(10) 1 calc PR A 1 C23R C 0.817(5) 0.222(3) 0.0219(19) 0.071(11) Uiso 0.201(10) 1 d PDU A 1 C24R C 0.765(4) 0.3847(19) -0.0303(9) 0.079(9) Uiso 0.201(10) 1 d PDU A 1 H24R H 0.8683 0.3939 -0.0252 0.095 Uiso 0.201(10) 1 calc PR A 1 C25R C 0.696(4) 0.498(2) -0.0142(15) 0.093(11) Uiso 0.201(10) 1 d PDU A 1 C26R C 0.485(7) 0.590(5) 0.011(4) 0.114(16) Uiso 0.201(10) 1 d PDU A 1 H26A H 0.5491 0.6541 0.0184 0.171 Uiso 0.201(10) 1 calc PR A 1 H26B H 0.4215 0.5770 0.0372 0.171 Uiso 0.201(10) 1 calc PR A 1 H26C H 0.4302 0.6097 -0.0165 0.171 Uiso 0.201(10) 1 calc PR A 1 C27R C 0.744(5) 0.363(3) -0.0827(10) 0.102(10) Uiso 0.201(10) 1 d PDU A 1 H27A H 0.6426 0.3530 -0.0894 0.123 Uiso 0.201(10) 1 calc PR A 1 H27B H 0.7780 0.4308 -0.1003 0.123 Uiso 0.201(10) 1 calc PR A 1 C28R C 0.824(3) 0.256(2) -0.0986(10) 0.100(12) Uiso 0.201(10) 1 d PGDU A 1 C29R C 0.754(2) 0.150(2) -0.1022(10) 0.100(12) Uiso 0.201(10) 1 d PGD A 1 H29R H 0.6560 0.1456 -0.0955 0.120 Uiso 0.201(10) 1 d PG A 1 C30R C 0.825(3) 0.0494(19) -0.1156(11) 0.109(13) Uiso 0.201(10) 1 d PG A 1 H30R H 0.7754 -0.0215 -0.1175 0.131 Uiso 0.201(10) 1 d PG A 1 C31R C 0.970(3) 0.052(2) -0.1262(12) 0.106(12) Uiso 0.201(10) 1 d PG A 1 H31R H 1.0185 -0.0162 -0.1347 0.127 Uiso 0.201(10) 1 d PG A 1 C32R C 1.039(2) 0.158(3) -0.1239(13) 0.104(13) Uiso 0.201(10) 1 d PG A 1 H32R H 1.1359 0.1617 -0.1318 0.125 Uiso 0.201(10) 1 d PG A 1 C33R C 0.968(3) 0.258(2) -0.1103(12) 0.117(19) Uiso 0.201(10) 1 d PGD A 1 H33R H 1.0182 0.3290 -0.1088 0.140 Uiso 0.201(10) 1 d PG A 1 N1P N 0.7354(9) 0.2711(7) -0.0130(3) 0.079(3) Uani 0.799(10) 1 d PDU A 2 H1P H 0.6523 0.2398 -0.0176 0.094 Uiso 0.799(10) 1 calc PR A 2 O1P O 0.5013(15) -0.2374(13) 0.0988(5) 0.105(5) Uani 0.799(10) 1 d PDU A 2 O2P O 0.9373(10) 0.2712(11) 0.0299(5) 0.081(3) Uani 0.799(10) 1 d PDU A 2 O3P O 0.7443(8) 0.5732(7) -0.0482(4) 0.130(3) Uani 0.799(10) 1 d PD A 2 O4P O 0.6019(12) 0.4706(9) -0.0004(5) 0.109(3) Uani 0.799(10) 1 d PDU A 2 C1P C 0.6548(10) -0.2039(10) 0.1990(3) 0.083(5) Uiso 0.799(10) 1 d PDU A 2 C2P C 0.7265(10) -0.2348(9) 0.2398(3) 0.093(4) Uiso 0.799(10) 1 d PD A 2 H2P H 0.6947 -0.2108 0.2694 0.112 Uiso 0.799(10) 1 calc PR A 2 C3P C 0.8484(11) -0.3035(11) 0.2343(3) 0.101(4) Uiso 0.799(10) 1 d PDU A 2 C4P C 0.8916(11) -0.3393(11) 0.1902(3) 0.092(4) Uiso 0.799(10) 1 d PDU A 2 H4P H 0.9711 -0.3886 0.1879 0.110 Uiso 0.799(10) 1 calc PR A 2 C5P C 0.8222(10) -0.3054(10) 0.1483(3) 0.089(4) Uiso 0.799(10) 1 d PDU A 2 C6P C 0.7014(10) -0.2370(10) 0.1558(3) 0.078(5) Uiso 0.799(10) 1 d PDU A 2 C7P C 0.5900(7) -0.1674(5) 0.1280(2) 0.069(2) Uani 0.799(10) 1 d PDU A 2 C8P C 0.6524(8) -0.0651(6) 0.0997(3) 0.064(2) Uiso 0.799(10) 1 d PD A 2 C9P C 0.6031(8) -0.0407(7) 0.0551(3) 0.068(2) Uiso 0.799(10) 1 d PD A 2 H9P H 0.5330 -0.0887 0.0418 0.082 Uiso 0.799(10) 1 calc PR A 2 C10P C 0.6551(9) 0.0531(7) 0.0296(3) 0.069(3) Uiso 0.799(10) 1 d PDU A 2 H10P H 0.6179 0.0684 -0.0003 0.082 Uiso 0.799(10) 1 calc PR A 2 C11P C 0.7611(10) 0.1247(8) 0.0474(3) 0.062(4) Uiso 0.799(10) 1 d PD A 2 C12P C 0.8134(10) 0.0985(8) 0.0919(3) 0.070(3) Uiso 0.799(10) 1 d PDU A 2 H12P H 0.8850 0.1456 0.1050 0.084 Uiso 0.799(10) 1 calc PR A 2 C13P C 0.7621(8) 0.0052(7) 0.1168(3) 0.066(2) Uiso 0.799(10) 1 d PD A 2 H13P H 0.8018 -0.0118 0.1461 0.079 Uiso 0.799(10) 1 calc PR A 2 C14P C 0.5251(7) -0.1366(6) 0.1806(3) 0.085(3) Uani 0.799(10) 1 d PDU A 2 C15P C 0.3820(8) -0.1987(8) 0.1890(4) 0.108(3) Uani 0.799(10) 1 d PDU A 2 H15D H 0.3901 -0.2799 0.1799 0.162 Uiso 0.799(10) 1 calc PR A 2 H15E H 0.3084 -0.1614 0.1705 0.162 Uiso 0.799(10) 1 calc PR A 2 H15F H 0.3573 -0.1938 0.2218 0.162 Uiso 0.799(10) 1 calc PR A 2 C16P C 0.5146(11) -0.0108(6) 0.1960(3) 0.095(3) Uani 0.799(10) 1 d PDU A 2 H16D H 0.4310 0.0246 0.1821 0.142 Uiso 0.799(10) 1 calc PR A 2 H16E H 0.5989 0.0311 0.1859 0.142 Uiso 0.799(10) 1 calc PR A 2 H16F H 0.5072 -0.0074 0.2297 0.142 Uiso 0.799(10) 1 calc PR A 2 C17P C 0.9305(13) -0.3439(11) 0.2789(3) 0.123(4) Uani 0.799(10) 1 d PDU A 2 H17P H 0.8726 -0.3177 0.3058 0.148 Uiso 0.799(10) 1 calc PR A 2 C18P C 1.0695(16) -0.2841(16) 0.2835(5) 0.174(7) Uani 0.799(10) 1 d PDU A 2 H18D H 1.0556 -0.2005 0.2813 0.261 Uiso 0.799(10) 1 calc PR A 2 H18E H 1.1326 -0.3097 0.2588 0.261 Uiso 0.799(10) 1 calc PR A 2 H18F H 1.1113 -0.3029 0.3136 0.261 Uiso 0.799(10) 1 calc PR A 2 C19P C 0.937(2) -0.4715(12) 0.2824(7) 0.173(9) Uani 0.799(10) 1 d PDU A 2 H19D H 0.8421 -0.5036 0.2798 0.260 Uiso 0.799(10) 1 calc PR A 2 H19E H 0.9781 -0.4932 0.3123 0.260 Uiso 0.799(10) 1 calc PR A 2 H19F H 0.9962 -0.5019 0.2574 0.260 Uiso 0.799(10) 1 calc PR A 2 C20P C 0.8819(12) -0.3303(11) 0.0997(3) 0.105(4) Uani 0.799(10) 1 d PDU A 2 H20P H 0.8189 -0.2918 0.0767 0.126 Uiso 0.799(10) 1 calc PR A 2 C21P C 0.8797(18) -0.4607(10) 0.0897(5) 0.138(5) Uani 0.799(10) 1 d PDU A 2 H21D H 0.9157 -0.4748 0.0584 0.207 Uiso 0.799(10) 1 calc PR A 2 H21E H 0.7829 -0.4894 0.0920 0.207 Uiso 0.799(10) 1 calc PR A 2 H21F H 0.9392 -0.5009 0.1122 0.207 Uiso 0.799(10) 1 calc PR A 2 C22P C 1.0304(17) -0.2803(16) 0.0937(7) 0.158(7) Uani 0.799(10) 1 d PDU A 2 H22D H 1.0647 -0.2975 0.0625 0.237 Uiso 0.799(10) 1 calc PR A 2 H22E H 1.0938 -0.3148 0.1165 0.237 Uiso 0.799(10) 1 calc PR A 2 H22F H 1.0274 -0.1965 0.0981 0.237 Uiso 0.799(10) 1 calc PR A 2 C23P C 0.8188(12) 0.2285(10) 0.0219(5) 0.067(3) Uani 0.799(10) 1 d PDU A 2 C24P C 0.7793(10) 0.3667(7) -0.0429(3) 0.081(3) Uani 0.799(10) 1 d PDU A 2 H24P H 0.8834 0.3765 -0.0394 0.098 Uiso 0.799(10) 1 calc PR A 2 C25P C 0.7091(10) 0.4808(8) -0.0301(4) 0.091(3) Uani 0.799(10) 1 d PDU A 2 C26P C 0.527(2) 0.5747(13) 0.0145(9) 0.141(6) Uani 0.799(10) 1 d PDU A 2 H26D H 0.4641 0.5554 0.0403 0.211 Uiso 0.799(10) 1 calc PR A 2 H26E H 0.4709 0.6050 -0.0112 0.211 Uiso 0.799(10) 1 calc PR A 2 H26F H 0.5949 0.6331 0.0245 0.211 Uiso 0.799(10) 1 calc PR A 2 C27P C 0.7486(11) 0.3380(8) -0.0945(3) 0.089(3) Uani 0.799(10) 1 d PDU A 2 H27C H 0.6469 0.3215 -0.0980 0.107 Uiso 0.799(10) 1 calc PR A 2 H27D H 0.7706 0.4067 -0.1135 0.107 Uiso 0.799(10) 1 calc PR A 2 C28P C 0.8307(7) 0.2376(5) -0.1125(3) 0.078(2) Uiso 0.799(10) 1 d PGDU A 2 C29P C 0.7663(6) 0.1313(6) -0.1210(3) 0.114(4) Uiso 0.799(10) 1 d PGD A 2 H29P H 0.6685 0.1221 -0.1151 0.137 Uiso 0.799(10) 1 d PG A 2 C30P C 0.8446(9) 0.0378(5) -0.1382(3) 0.138(4) Uiso 0.799(10) 1 d PG A 2 H30P H 0.7996 -0.0345 -0.1427 0.166 Uiso 0.799(10) 1 d PG A 2 C31P C 0.9876(9) 0.0493(6) -0.1489(3) 0.131(4) Uiso 0.799(10) 1 d PG A 2 H31P H 1.0396 -0.0136 -0.1611 0.157 Uiso 0.799(10) 1 d PG A 2 C32P C 1.0516(6) 0.1560(7) -0.1410(3) 0.122(4) Uiso 0.799(10) 1 d PG A 2 H32P H 1.1485 0.1658 -0.1481 0.146 Uiso 0.799(10) 1 d PG A 2 C33P C 0.9747(7) 0.2487(6) -0.1227(3) 0.088(3) Uiso 0.799(10) 1 d PGD A 2 H33P H 1.0207 0.3201 -0.1171 0.105 Uiso 0.799(10) 1 d PG 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 N1P 0.052(3) 0.102(5) 0.082(5) 0.026(5) 0.004(3) -0.006(4) O1P 0.112(6) 0.091(6) 0.114(7) 0.002(4) -0.020(4) -0.024(5) O2P 0.052(4) 0.101(6) 0.090(7) 0.020(4) 0.001(4) -0.004(3) O3P 0.120(5) 0.102(5) 0.167(9) 0.033(6) 0.017(6) 0.025(5) O4P 0.113(7) 0.107(5) 0.107(5) -0.018(4) 0.023(6) 0.008(5) C7P 0.069(4) 0.062(4) 0.076(5) -0.001(4) -0.004(4) -0.002(4) C14P 0.082(5) 0.081(6) 0.093(6) 0.006(5) 0.022(5) 0.015(5) C15P 0.089(6) 0.108(7) 0.126(9) 0.013(6) 0.032(6) -0.005(6) C16P 0.103(6) 0.088(6) 0.093(7) 0.005(5) 0.005(5) 0.009(5) C17P 0.136(9) 0.142(9) 0.091(7) 0.055(6) 0.002(7) 0.049(9) C18P 0.161(12) 0.210(15) 0.152(12) 0.099(11) -0.060(11) -0.063(12) C19P 0.164(13) 0.167(12) 0.188(17) 0.116(12) -0.075(14) -0.015(11) C20P 0.096(6) 0.130(9) 0.091(6) 0.021(6) 0.012(5) 0.050(6) C21P 0.163(11) 0.124(10) 0.127(11) -0.023(8) 0.038(9) 0.036(9) C22P 0.154(12) 0.178(17) 0.143(11) 0.031(11) 0.053(10) -0.008(12) C23P 0.053(4) 0.082(5) 0.066(5) 0.007(4) -0.003(3) 0.017(4) C24P 0.060(5) 0.096(6) 0.088(7) 0.024(5) 0.003(5) 0.004(4) C25P 0.084(6) 0.098(7) 0.093(8) 0.020(6) 0.005(5) 0.005(6) C26P 0.149(14) 0.114(10) 0.160(13) -0.038(9) 0.012(13) 0.027(10) C27P 0.080(5) 0.114(7) 0.075(5) 0.033(5) -0.007(5) -0.011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1R C23R 1.338(11) . ? N1R C24R 1.442(11) . ? N1R H1R 0.8600 . ? O1R C7R 1.227(11) . ? O2R C23R 1.225(11) . ? O3R C25R 1.189(10) . ? O4R C25R 1.288(11) . ? O4R C26R 1.435(11) . ? C1R C2R 1.381(10) . ? C1R C6R 1.396(10) . ? C1R C14R 1.496(10) . ? C2R C3R 1.370(10) . ? C2R H2R 0.9300 . ? C3R C4R 1.373(10) . ? C3R C17R 1.499(10) . ? C4R C5R 1.417(10) . ? C4R H4R 0.9300 . ? C5R C6R 1.385(10) . ? C5R C20R 1.522(10) . ? C6R C7R 1.506(10) . ? C7R C8R 1.477(10) . ? C8R C9R 1.384(10) . ? C8R C13R 1.389(10) . ? C9R C10R 1.373(10) . ? C9R H9R 0.9300 . ? C10R C11R 1.377(10) . ? C10R H10R 0.9300 . ? C11R C12R 1.393(10) . ? C11R C23R 1.485(10) . ? C12R C13R 1.359(10) . ? C12R H12R 0.9300 . ? C13R H13R 0.9300 . ? C14R C15R 1.512(11) . ? C14R C16R 1.525(11) . ? C14R H14R 0.9800 . ? C15R H15A 0.9600 . ? C15R H15B 0.9600 . ? C15R H15C 0.9600 . ? C16R H16A 0.9600 . ? C16R H16B 0.9600 . ? C16R H16C 0.9600 . ? C17R C19R 1.437(11) . ? C17R C18R 1.491(11) . ? C17R H17R 0.9800 . ? C18R H18A 0.9600 . ? C18R H18B 0.9600 . ? C18R H18C 0.9600 . ? C19R H19A 0.9600 . ? C19R H19B 0.9600 . ? C19R H19C 0.9600 . ? C20R C21R 1.501(11) . ? C20R C22R 1.519(11) . ? C20R H20R 0.9800 . ? C21R H21A 0.9600 . ? C21R H21B 0.9600 . ? C21R H21C 0.9600 . ? C22R H22A 0.9600 . ? C22R H22B 0.9600 . ? C22R H22C 0.9600 . ? C24R C25R 1.505(10) . ? C24R C27R 1.519(11) . ? C24R H24R 0.9800 . ? C26R H26A 0.9600 . ? C26R H26B 0.9600 . ? C26R H26C 0.9600 . ? C27R C28R 1.492(10) . ? C27R H27A 0.9700 . ? C27R H27B 0.9700 . ? C28R C29R 1.3754 . ? C28R C33R 1.3832 . ? C29R C30R 1.3701 . ? C29R H29R 0.9300 . ? C30R C31R 1.3771 . ? C30R H30R 0.9300 . ? C31R C32R 1.3617 . ? C31R H31R 0.9300 . ? C32R C33R 1.3726 . ? C32R H32R 0.9300 . ? C33R H33R 0.9300 . ? N1P C23P 1.347(7) . ? N1P C24P 1.436(7) . ? N1P H1P 0.8600 . ? O1P C7P 1.413(8) . ? O2P C23P 1.225(7) . ? O3P C25P 1.212(7) . ? O4P C25P 1.310(8) . ? O4P C26P 1.436(9) . ? C1P C6P 1.352(8) . ? C1P C2P 1.380(8) . ? C1P C14P 1.521(8) . ? C2P C3P 1.385(8) . ? C2P H2P 0.9300 . ? C3P C4P 1.373(8) . ? C3P C17P 1.547(8) . ? C4P C5P 1.403(8) . ? C4P H4P 0.9300 . ? C5P C6P 1.382(7) . ? C5P C20P 1.512(8) . ? C6P C7P 1.522(7) . ? C7P C8P 1.526(7) . ? C7P C14P 1.646(8) . ? C8P C9P 1.373(7) . ? C8P C13P 1.383(7) . ? C9P C10P 1.375(7) . ? C9P H9P 0.9300 . ? C10P C11P 1.374(8) . ? C10P H10P 0.9300 . ? C11P C12P 1.382(7) . ? C11P C23P 1.484(7) . ? C12P C13P 1.360(7) . ? C12P H12P 0.9300 . ? C13P H13P 0.9300 . ? C14P C16P 1.496(8) . ? C14P C15P 1.525(8) . ? C15P H15D 0.9600 . ? C15P H15E 0.9600 . ? C15P H15F 0.9600 . ? C16P H16D 0.9600 . ? C16P H16E 0.9600 . ? C16P H16F 0.9600 . ? C17P C19P 1.452(10) . ? C17P C18P 1.466(10) . ? C17P H17P 0.9800 . ? C18P H18D 0.9600 . ? C18P H18E 0.9600 . ? C18P H18F 0.9600 . ? C19P H19D 0.9600 . ? C19P H19E 0.9600 . ? C19P H19F 0.9600 . ? C20P C22P 1.503(9) . ? C20P C21P 1.507(9) . ? C20P H20P 0.9800 . ? C21P H21D 0.9600 . ? C21P H21E 0.9600 . ? C21P H21F 0.9600 . ? C22P H22D 0.9600 . ? C22P H22E 0.9600 . ? C22P H22F 0.9600 . ? C24P C25P 1.496(8) . ? C24P C27P 1.523(8) . ? C24P H24P 0.9800 . ? C26P H26D 0.9600 . ? C26P H26E 0.9600 . ? C26P H26F 0.9600 . ? C27P C28P 1.464(7) . ? C27P H27C 0.9700 . ? C27P H27D 0.9700 . ? C28P C29P 1.3688 . ? C28P C33P 1.3759 . ? C29P C30P 1.3762 . ? C29P H29P 0.9300 . ? C30P C31P 1.3694 . ? C30P H30P 0.9300 . ? C31P C32P 1.3674 . ? C31P H31P 0.9300 . ? C32P C33P 1.3743 . ? C32P H32P 0.9300 . ? C33P H33P 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23R N1R C24R 120.7(19) . . ? C23R N1R H1R 119.7 . . ? C24R N1R H1R 119.7 . . ? C25R O4R C26R 118(2) . . ? C2R C1R C6R 116.6(11) . . ? C2R C1R C14R 118.7(13) . . ? C6R C1R C14R 124.5(13) . . ? C3R C2R C1R 122.7(13) . . ? C3R C2R H2R 118.7 . . ? C1R C2R H2R 118.7 . . ? C2R C3R C4R 118.1(12) . . ? C2R C3R C17R 117.8(15) . . ? C4R C3R C17R 120.9(15) . . ? C3R C4R C5R 121.6(14) . . ? C3R C4R H4R 119.2 . . ? C5R C4R H4R 119.2 . . ? C6R C5R C4R 115.7(11) . . ? C6R C5R C20R 120.6(15) . . ? C4R C5R C20R 119.9(15) . . ? C5R C6R C1R 123.2(11) . . ? C5R C6R C7R 119.8(13) . . ? C1R C6R C7R 116.8(13) . . ? O1R C7R C8R 120.6(17) . . ? O1R C7R C6R 120.4(17) . . ? C8R C7R C6R 115.2(14) . . ? C9R C8R C13R 119.3(11) . . ? C9R C8R C7R 121.0(13) . . ? C13R C8R C7R 119.4(12) . . ? C10R C9R C8R 120.4(13) . . ? C10R C9R H9R 119.8 . . ? C8R C9R H9R 119.8 . . ? C9R C10R C11R 119.8(13) . . ? C9R C10R H10R 120.1 . . ? C11R C10R H10R 120.1 . . ? C10R C11R C12R 119.4(11) . . ? C10R C11R C23R 124.8(14) . . ? C12R C11R C23R 115.7(13) . . ? C13R C12R C11R 120.5(13) . . ? C13R C12R H12R 119.7 . . ? C11R C12R H12R 119.7 . . ? C12R C13R C8R 119.8(13) . . ? C12R C13R H13R 120.1 . . ? C8R C13R H13R 120.1 . . ? C1R C14R C15R 108.3(15) . . ? C1R C14R C16R 112.7(16) . . ? C15R C14R C16R 109.8(16) . . ? C1R C14R H14R 108.6 . . ? C15R C14R H14R 108.6 . . ? C16R C14R H14R 108.6 . . ? C14R C15R H15A 109.5 . . ? C14R C15R H15B 109.5 . . ? H15A C15R H15B 109.5 . . ? C14R C15R H15C 109.5 . . ? H15A C15R H15C 109.5 . . ? H15B C15R H15C 109.5 . . ? C14R C16R H16A 109.5 . . ? C14R C16R H16B 109.5 . . ? H16A C16R H16B 109.5 . . ? C14R C16R H16C 109.5 . . ? H16A C16R H16C 109.5 . . ? H16B C16R H16C 109.5 . . ? C19R C17R C18R 117.9(18) . . ? C19R C17R C3R 117.7(18) . . ? C18R C17R C3R 114.5(17) . . ? C19R C17R H17R 100.6 . . ? C18R C17R H17R 100.6 . . ? C3R C17R H17R 100.6 . . ? C17R C18R H18A 109.5 . . ? C17R C18R H18B 109.5 . . ? H18A C18R H18B 109.5 . . ? C17R C18R H18C 109.5 . . ? H18A C18R H18C 109.5 . . ? H18B C18R H18C 109.5 . . ? C17R C19R H19A 109.5 . . ? C17R C19R H19B 109.5 . . ? H19A C19R H19B 109.5 . . ? C17R C19R H19C 109.5 . . ? H19A C19R H19C 109.5 . . ? H19B C19R H19C 109.5 . . ? C21R C20R C22R 111.6(17) . . ? C21R C20R C5R 112.3(17) . . ? C22R C20R C5R 111.1(16) . . ? C21R C20R H20R 107.2 . . ? C22R C20R H20R 107.2 . . ? C5R C20R H20R 107.2 . . ? C20R C21R H21A 109.5 . . ? C20R C21R H21B 109.5 . . ? H21A C21R H21B 109.5 . . ? C20R C21R H21C 109.5 . . ? H21A C21R H21C 109.5 . . ? H21B C21R H21C 109.5 . . ? C20R C22R H22A 109.5 . . ? C20R C22R H22B 109.5 . . ? H22A C22R H22B 109.5 . . ? C20R C22R H22C 109.5 . . ? H22A C22R H22C 109.5 . . ? H22B C22R H22C 109.5 . . ? O2R C23R N1R 122(2) . . ? O2R C23R C11R 118.9(18) . . ? N1R C23R C11R 116.1(17) . . ? N1R C24R C25R 112.4(16) . . ? N1R C24R C27R 112.1(17) . . ? C25R C24R C27R 112.4(16) . . ? N1R C24R H24R 106.5 . . ? C25R C24R H24R 106.5 . . ? C27R C24R H24R 106.5 . . ? O3R C25R O4R 122.8(17) . . ? O3R C25R C24R 122.9(17) . . ? O4R C25R C24R 114.3(15) . . ? C28R C27R C24R 111.5(16) . . ? C28R C27R H27A 109.3 . . ? C24R C27R H27A 109.3 . . ? C28R C27R H27B 109.3 . . ? C24R C27R H27B 109.3 . . ? H27A C27R H27B 108.0 . . ? C29R C28R C33R 117.2 . . ? C29R C28R C27R 120.1(13) . . ? C33R C28R C27R 122.6(13) . . ? C30R C29R C28R 121.3 . . ? C29R C30R C31R 121.0 . . ? C32R C31R C30R 118.1 . . ? C31R C32R C33R 121.2 . . ? C32R C33R C28R 121.2 . . ? C23P N1P C24P 122.7(6) . . ? C23P N1P H1P 118.6 . . ? C24P N1P H1P 118.6 . . ? C25P O4P C26P 119.2(9) . . ? C6P C1P C2P 122.3(7) . . ? C6P C1P C14P 94.7(6) . . ? C2P C1P C14P 143.0(7) . . ? C1P C2P C3P 116.3(7) . . ? C1P C2P H2P 121.8 . . ? C3P C2P H2P 121.8 . . ? C4P C3P C2P 120.6(7) . . ? C4P C3P C17P 120.8(8) . . ? C2P C3P C17P 118.6(8) . . ? C3P C4P C5P 123.5(7) . . ? C3P C4P H4P 118.2 . . ? C5P C4P H4P 118.2 . . ? C6P C5P C4P 113.6(7) . . ? C6P C5P C20P 122.8(7) . . ? C4P C5P C20P 123.3(7) . . ? C1P C6P C5P 123.7(6) . . ? C1P C6P C7P 96.1(6) . . ? C5P C6P C7P 140.0(7) . . ? O1P C7P C6P 114.1(8) . . ? O1P C7P C8P 110.0(6) . . ? C6P C7P C8P 114.0(6) . . ? O1P C7P C14P 115.8(8) . . ? C6P C7P C14P 83.7(5) . . ? C8P C7P C14P 117.0(6) . . ? C9P C8P C13P 116.9(6) . . ? C9P C8P C7P 120.7(5) . . ? C13P C8P C7P 122.4(6) . . ? C8P C9P C10P 121.5(6) . . ? C8P C9P H9P 119.2 . . ? C10P C9P H9P 119.2 . . ? C11P C10P C9P 121.1(7) . . ? C11P C10P H10P 119.4 . . ? C9P C10P H10P 119.4 . . ? C10P C11P C12P 117.5(6) . . ? C10P C11P C23P 123.3(6) . . ? C12P C11P C23P 119.2(7) . . ? C13P C12P C11P 121.1(7) . . ? C13P C12P H12P 119.5 . . ? C11P C12P H12P 119.5 . . ? C12P C13P C8P 121.8(6) . . ? C12P C13P H13P 119.1 . . ? C8P C13P H13P 119.1 . . ? C16P C14P C1P 115.5(7) . . ? C16P C14P C15P 109.8(7) . . ? C1P C14P C15P 114.0(7) . . ? C16P C14P C7P 119.4(6) . . ? C1P C14P C7P 85.0(5) . . ? C15P C14P C7P 111.3(6) . . ? C14P C15P H15D 109.5 . . ? C14P C15P H15E 109.5 . . ? H15D C15P H15E 109.5 . . ? C14P C15P H15F 109.5 . . ? H15D C15P H15F 109.5 . . ? H15E C15P H15F 109.5 . . ? C14P C16P H16D 109.5 . . ? C14P C16P H16E 109.5 . . ? H16D C16P H16E 109.5 . . ? C14P C16P H16F 109.5 . . ? H16D C16P H16F 109.5 . . ? H16E C16P H16F 109.5 . . ? C19P C17P C18P 114.7(11) . . ? C19P C17P C3P 111.9(8) . . ? C18P C17P C3P 111.8(8) . . ? C19P C17P H17P 105.9 . . ? C18P C17P H17P 105.9 . . ? C3P C17P H17P 105.9 . . ? C17P C18P H18D 109.5 . . ? C17P C18P H18E 109.5 . . ? H18D C18P H18E 109.5 . . ? C17P C18P H18F 109.5 . . ? H18D C18P H18F 109.5 . . ? H18E C18P H18F 109.5 . . ? C17P C19P H19D 109.5 . . ? C17P C19P H19E 109.5 . . ? H19D C19P H19E 109.5 . . ? C17P C19P H19F 109.5 . . ? H19D C19P H19F 109.5 . . ? H19E C19P H19F 109.5 . . ? C22P C20P C21P 111.2(9) . . ? C22P C20P C5P 111.8(9) . . ? C21P C20P C5P 110.5(9) . . ? C22P C20P H20P 107.7 . . ? C21P C20P H20P 107.7 . . ? C5P C20P H20P 107.7 . . ? C20P C21P H21D 109.5 . . ? C20P C21P H21E 109.5 . . ? H21D C21P H21E 109.5 . . ? C20P C21P H21F 109.5 . . ? H21D C21P H21F 109.5 . . ? H21E C21P H21F 109.5 . . ? C20P C22P H22D 109.5 . . ? C20P C22P H22E 109.5 . . ? H22D C22P H22E 109.5 . . ? C20P C22P H22F 109.5 . . ? H22D C22P H22F 109.5 . . ? H22E C22P H22F 109.5 . . ? O2P C23P N1P 120.8(7) . . ? O2P C23P C11P 123.3(7) . . ? N1P C23P C11P 115.8(6) . . ? N1P C24P C25P 112.8(7) . . ? N1P C24P C27P 110.6(7) . . ? C25P C24P C27P 109.6(6) . . ? N1P C24P H24P 107.9 . . ? C25P C24P H24P 107.9 . . ? C27P C24P H24P 107.9 . . ? O3P C25P O4P 123.6(8) . . ? O3P C25P C24P 121.9(8) . . ? O4P C25P C24P 114.3(7) . . ? O4P C26P H26D 109.5 . . ? O4P C26P H26E 109.5 . . ? H26D C26P H26E 109.5 . . ? O4P C26P H26F 109.5 . . ? H26D C26P H26F 109.5 . . ? H26E C26P H26F 109.5 . . ? C28P C27P C24P 113.8(6) . . ? C28P C27P H27C 108.8 . . ? C24P C27P H27C 108.8 . . ? C28P C27P H27D 108.8 . . ? C24P C27P H27D 108.8 . . ? H27C C27P H27D 107.7 . . ? C29P C28P C33P 118.1 . . ? C29P C28P C27P 121.3(5) . . ? C33P C28P C27P 120.6(5) . . ? C28P C29P C30P 120.7 . . ? C28P C29P H29P 119.7 . . ? C30P C29P H29P 119.7 . . ? C31P C30P C29P 121.2 . . ? C31P C30P H30P 119.4 . . ? C29P C30P H30P 119.4 . . ? C32P C31P C30P 118.1 . . ? C32P C31P H31P 120.9 . . ? C30P C31P H31P 120.9 . . ? C31P C32P C33P 120.9 . . ? C31P C32P H32P 119.6 . . ? C33P C32P H32P 119.6 . . ? C32P C33P C28P 121.0 . . ? C32P C33P H33P 119.5 . . ? C28P C33P H33P 119.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.176 _refine_diff_density_min -0.155 _refine_diff_density_rms 0.034 #===END data_81.2%P _database_code_depnum_ccdc_archive 'CCDC 799260' #TrackingRef '- 1.cif' #==================================================================== # start Validation Reply Form _vrf_PLAT201_81.2%P ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 18 RESPONSE: In the crystal there are reactant and photoproduct molecules. Part of atoms were refined isotropically in order to decrease a large number of the parameters in the refinement. ; # end Validation Reply Form #==================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 N O4' _chemical_formula_weight 513.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.2818(15) _cell_length_b 11.418(2) _cell_length_c 28.183(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2986.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 13.4 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14591 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 4.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2968 _reflns_number_gt 1944 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSALIS (Oxford Diffraction, 2003)' _computing_cell_refinement 'CRYSALIS (Oxford Diffraction, 2003)' _computing_data_reduction 'CRYSALIS (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Owing to a reactant-product disorder, the following weak restraints from SHELXL97 were applied: DFIX, DANG and SIMU. DFIX and DANG restrained bond lengths and valence angles to target values. The target values were taken from the structures of the pure reactant and the pure product of crystal 1a. SIMU restrained displacement parameters of atoms of the products. ; _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^)+(0.1395P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration syn _refine_ls_number_reflns 2968 _refine_ls_number_parameters 384 _refine_ls_number_restraints 280 _refine_ls_R_factor_all 0.1173 _refine_ls_R_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.2464 _refine_ls_wR_factor_gt 0.2164 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.259 _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 N1R N 0.733(5) 0.275(3) -0.0055(16) 0.085(11) Uiso 0.188(10) 1 d PDU A 1 H1R H 0.6445 0.2513 -0.0065 0.102 Uiso 0.188(10) 1 calc PR A 1 O1R O 0.507(5) -0.242(5) 0.101(2) 0.089(11) Uiso 0.188(10) 1 d PDU A 1 O2R O 0.932(6) 0.266(4) 0.039(2) 0.065(9) Uiso 0.188(10) 1 d PDU A 1 O3R O 0.758(4) 0.581(2) -0.0190(16) 0.128(16) Uiso 0.188(10) 1 d PD A 1 O4R O 0.582(7) 0.468(4) 0.005(3) 0.103(10) Uiso 0.188(10) 1 d PDU A 1 C1R C 0.631(3) -0.217(3) 0.1953(8) 0.075(18) Uiso 0.188(10) 1 d PD A 1 C2R C 0.690(3) -0.261(3) 0.2366(8) 0.071(8) Uiso 0.188(10) 1 d PDU A 1 H2R H 0.6390 -0.2524 0.2649 0.085 Uiso 0.188(10) 1 calc PR A 1 C3R C 0.820(3) -0.317(3) 0.2373(8) 0.073(13) Uiso 0.188(10) 1 d PDU A 1 C4R C 0.899(3) -0.324(5) 0.1962(9) 0.096(15) Uiso 0.188(10) 1 d PDU A 1 H4R H 0.9929 -0.3524 0.1976 0.115 Uiso 0.188(10) 1 calc PR A 1 C5R C 0.842(3) -0.289(3) 0.1518(8) 0.075(9) Uiso 0.188(10) 1 d PDU A 1 C6R C 0.706(3) -0.238(4) 0.1533(7) 0.074(18) Uiso 0.188(10) 1 d PDU A 1 C7R C 0.630(3) -0.205(2) 0.1082(9) 0.093(10) Uiso 0.188(10) 1 d PDU A 1 C8R C 0.674(4) -0.092(3) 0.0872(11) 0.089(15) Uiso 0.188(10) 1 d PD A 1 C9R C 0.623(4) -0.064(3) 0.0423(10) 0.077(13) Uiso 0.188(10) 1 d PD A 1 H9R H 0.5573 -0.1124 0.0272 0.093 Uiso 0.188(10) 1 calc PR A 1 C10R C 0.671(4) 0.036(3) 0.0200(10) 0.064(14) Uiso 0.188(10) 1 d PD A 1 H10R H 0.6333 0.0570 -0.0094 0.077 Uiso 0.188(10) 1 calc PR A 1 C11R C 0.773(5) 0.105(3) 0.0414(13) 0.08(2) Uiso 0.188(10) 1 d PD A 1 C12R C 0.829(4) 0.073(3) 0.0853(12) 0.078(18) Uiso 0.188(10) 1 d PD A 1 H12R H 0.8914 0.1227 0.1012 0.094 Uiso 0.188(10) 1 calc PR A 1 C13R C 0.792(3) -0.032(3) 0.1051(10) 0.071(11) Uiso 0.188(10) 1 d PD A 1 H13R H 0.8453 -0.0627 0.1301 0.086 Uiso 0.188(10) 1 calc PR A 1 C14R C 0.507(3) -0.134(3) 0.1974(12) 0.098(11) Uiso 0.188(10) 1 d PDU A 1 H14R H 0.4769 -0.1175 0.1647 0.118 Uiso 0.188(10) 1 calc PR A 1 C15R C 0.382(3) -0.192(4) 0.222(2) 0.139(17) Uiso 0.188(10) 1 d PDU A 1 H15A H 0.3011 -0.1406 0.2226 0.209 Uiso 0.188(10) 1 calc PR A 1 H15B H 0.4097 -0.2106 0.2544 0.209 Uiso 0.188(10) 1 calc PR A 1 H15C H 0.3574 -0.2633 0.2060 0.209 Uiso 0.188(10) 1 calc PR A 1 C16R C 0.543(6) -0.018(3) 0.221(2) 0.16(2) Uiso 0.188(10) 1 d PDU A 1 H16A H 0.4587 0.0300 0.2223 0.237 Uiso 0.188(10) 1 calc PR A 1 H16B H 0.6170 0.0209 0.2033 0.237 Uiso 0.188(10) 1 calc PR A 1 H16C H 0.5770 -0.0327 0.2528 0.237 Uiso 0.188(10) 1 calc PR A 1 C17R C 0.889(4) -0.339(4) 0.2845(10) 0.130(7) Uiso 0.188(10) 1 d PDU A 1 H17R H 0.8089 -0.3178 0.3056 0.156 Uiso 0.188(10) 1 calc PR A 1 C18R C 0.998(6) -0.251(5) 0.300(2) 0.160(13) Uiso 0.188(10) 1 d PDU A 1 H18A H 0.9733 -0.1760 0.2868 0.240 Uiso 0.188(10) 1 calc PR A 1 H18B H 1.0912 -0.2742 0.2882 0.240 Uiso 0.188(10) 1 calc PR A 1 H18C H 0.9998 -0.2468 0.3337 0.240 Uiso 0.188(10) 1 calc PR A 1 C19R C 0.908(8) -0.460(4) 0.298(2) 0.132(13) Uiso 0.188(10) 1 d PDU A 1 H19A H 0.8297 -0.5054 0.2857 0.198 Uiso 0.188(10) 1 calc PR A 1 H19B H 0.9097 -0.4655 0.3320 0.198 Uiso 0.188(10) 1 calc PR A 1 H19C H 0.9972 -0.4881 0.2853 0.198 Uiso 0.188(10) 1 calc PR A 1 C20R C 0.894(4) -0.349(3) 0.1066(10) 0.084(10) Uiso 0.188(10) 1 d PDU A 1 H20R H 0.8405 -0.3137 0.0801 0.100 Uiso 0.188(10) 1 calc PR A 1 C21R C 0.860(7) -0.477(4) 0.106(2) 0.14(2) Uiso 0.188(10) 1 d PDU A 1 H21A H 0.8937 -0.5116 0.0773 0.206 Uiso 0.188(10) 1 calc PR A 1 H21B H 0.7579 -0.4885 0.1090 0.206 Uiso 0.188(10) 1 calc PR A 1 H21C H 0.9073 -0.5144 0.1328 0.206 Uiso 0.188(10) 1 calc PR A 1 C22R C 1.052(5) -0.326(5) 0.098(2) 0.111(18) Uiso 0.188(10) 1 d PDU A 1 H22A H 1.0712 -0.2434 0.1001 0.167 Uiso 0.188(10) 1 calc PR A 1 H22B H 1.0779 -0.3529 0.0666 0.167 Uiso 0.188(10) 1 calc PR A 1 H22C H 1.1088 -0.3670 0.1210 0.167 Uiso 0.188(10) 1 calc PR A 1 C23R C 0.828(5) 0.217(3) 0.0210(19) 0.067(11) Uiso 0.188(10) 1 d PDU A 1 C24R C 0.776(5) 0.376(2) -0.0326(11) 0.063(14) Uiso 0.188(10) 1 d PD A 1 H24R H 0.8798 0.3851 -0.0283 0.075 Uiso 0.188(10) 1 calc PR A 1 C25R C 0.706(4) 0.486(2) -0.0140(14) 0.079(18) Uiso 0.188(10) 1 d PD A 1 C26R C 0.503(9) 0.568(7) 0.022(4) 0.111(19) Uiso 0.188(10) 1 d PDU A 1 H26A H 0.4710 0.6139 -0.0047 0.166 Uiso 0.188(10) 1 calc PR A 1 H26B H 0.5632 0.6145 0.0419 0.166 Uiso 0.188(10) 1 calc PR A 1 H26C H 0.4203 0.5416 0.0396 0.166 Uiso 0.188(10) 1 calc PR A 1 C27R C 0.750(6) 0.358(3) -0.0854(12) 0.12(3) Uiso 0.188(10) 1 d PD A 1 H27A H 0.6473 0.3500 -0.0913 0.138 Uiso 0.188(10) 1 calc PR A 1 H27B H 0.7847 0.4249 -0.1029 0.138 Uiso 0.188(10) 1 calc PR A 1 C28R C 0.826(4) 0.250(2) -0.1020(13) 0.11(2) Uiso 0.188(10) 1 d PGD A 1 C29R C 0.756(3) 0.144(2) -0.1040(11) 0.088(12) Uiso 0.188(10) 1 d PGD A 1 H29R H 0.6582 0.1403 -0.0962 0.106 Uiso 0.188(10) 1 d PG A 1 C30R C 0.826(3) 0.0438(19) -0.1172(12) 0.093(12) Uiso 0.188(10) 1 d PG A 1 H30R H 0.7762 -0.0269 -0.1179 0.111 Uiso 0.188(10) 1 d PG A 1 C31R C 0.970(3) 0.046(2) -0.1293(13) 0.092(12) Uiso 0.188(10) 1 d PG A 1 H31R H 1.0181 -0.0222 -0.1376 0.110 Uiso 0.188(10) 1 d PG A 1 C32R C 1.039(3) 0.151(3) -0.1286(15) 0.107(17) Uiso 0.188(10) 1 d PG A 1 H32R H 1.1355 0.1549 -0.1375 0.128 Uiso 0.188(10) 1 d PG A 1 C33R C 0.969(4) 0.252(2) -0.1151(15) 0.107(17) Uiso 0.188(10) 1 d PGDU A 1 H33R H 1.0193 0.3223 -0.1148 0.128 Uiso 0.188(10) 1 d PG A 1 N1P N 0.7347(10) 0.2719(8) -0.0129(4) 0.078(3) Uani 0.812(10) 1 d PDU A 2 H1P H 0.6513 0.2410 -0.0174 0.094 Uiso 0.812(10) 1 calc PR A 2 O1P O 0.4992(14) -0.2363(12) 0.0982(5) 0.094(3) Uani 0.812(10) 1 d PDU A 2 O2P O 0.9365(12) 0.2713(11) 0.0303(5) 0.077(3) Uani 0.812(10) 1 d PDU A 2 O3P O 0.7448(9) 0.5722(7) -0.0489(4) 0.121(3) Uani 0.812(10) 1 d PD A 2 O4P O 0.6004(17) 0.4721(10) -0.0010(7) 0.106(3) Uani 0.812(10) 1 d PDU A 2 C1P C 0.6549(10) -0.2038(9) 0.1988(3) 0.077(4) Uiso 0.812(10) 1 d PD A 2 C2P C 0.7250(9) -0.2368(8) 0.2398(3) 0.086(3) Uiso 0.812(10) 1 d PDU A 2 H2P H 0.6927 -0.2143 0.2696 0.103 Uiso 0.812(10) 1 calc PR A 2 C3P C 0.8472(11) -0.3059(10) 0.2337(3) 0.095(4) Uiso 0.812(10) 1 d PDU A 2 C4P C 0.8924(11) -0.3397(11) 0.1893(3) 0.092(4) Uiso 0.812(10) 1 d PDU A 2 H4P H 0.9731 -0.3876 0.1869 0.110 Uiso 0.812(10) 1 calc PR A 2 C5P C 0.8222(10) -0.3050(9) 0.1475(3) 0.083(3) Uiso 0.812(10) 1 d PDU A 2 C6P C 0.7013(10) -0.2362(10) 0.1551(3) 0.073(4) Uiso 0.812(10) 1 d PDU A 2 C7P C 0.5896(7) -0.1673(5) 0.1273(2) 0.064(2) Uani 0.812(10) 1 d PDU A 2 C8P C 0.6518(8) -0.0655(6) 0.0992(3) 0.060(2) Uiso 0.812(10) 1 d PD A 2 C9P C 0.6033(9) -0.0407(7) 0.0543(3) 0.065(3) Uiso 0.812(10) 1 d PD A 2 H9P H 0.5335 -0.0884 0.0407 0.078 Uiso 0.812(10) 1 calc PR A 2 C10P C 0.6557(10) 0.0532(8) 0.0291(3) 0.071(4) Uiso 0.812(10) 1 d PD A 2 H10P H 0.6188 0.0688 -0.0009 0.085 Uiso 0.812(10) 1 calc PR A 2 C11P C 0.7608(10) 0.1242(8) 0.0471(3) 0.059(3) Uiso 0.812(10) 1 d PD A 2 C12P C 0.8140(9) 0.0975(8) 0.0916(3) 0.062(3) Uiso 0.812(10) 1 d PD A 2 H12P H 0.8864 0.1437 0.1046 0.075 Uiso 0.812(10) 1 calc PR A 2 C13P C 0.7620(8) 0.0046(6) 0.1166(3) 0.061(2) Uiso 0.812(10) 1 d PD A 2 H13P H 0.8013 -0.0124 0.1462 0.073 Uiso 0.812(10) 1 calc PR A 2 C14P C 0.5248(8) -0.1367(6) 0.1799(3) 0.080(2) Uani 0.812(10) 1 d PDU A 2 C15P C 0.3812(9) -0.1987(8) 0.1872(4) 0.101(3) Uani 0.812(10) 1 d PDU A 2 H15D H 0.3902 -0.2794 0.1781 0.152 Uiso 0.812(10) 1 calc PR A 2 H15E H 0.3086 -0.1618 0.1681 0.152 Uiso 0.812(10) 1 calc PR A 2 H15F H 0.3542 -0.1940 0.2201 0.152 Uiso 0.812(10) 1 calc PR A 2 C16P C 0.5148(11) -0.0119(6) 0.1956(3) 0.088(3) Uani 0.812(10) 1 d PDU A 2 H16D H 0.4311 0.0237 0.1817 0.132 Uiso 0.812(10) 1 calc PR A 2 H16E H 0.5994 0.0297 0.1856 0.132 Uiso 0.812(10) 1 calc PR A 2 H16F H 0.5074 -0.0089 0.2295 0.132 Uiso 0.812(10) 1 calc PR A 2 C17P C 0.9287(12) -0.3474(10) 0.2787(3) 0.141(4) Uani 0.812(10) 1 d PDU A 2 H17P H 0.8725 -0.3221 0.3063 0.169 Uiso 0.812(10) 1 calc PR A 2 C18P C 1.0720(14) -0.2900(14) 0.2817(5) 0.170(6) Uani 0.812(10) 1 d PDU A 2 H18D H 1.0604 -0.2066 0.2796 0.255 Uiso 0.812(10) 1 calc PR A 2 H18E H 1.1318 -0.3168 0.2561 0.255 Uiso 0.812(10) 1 calc PR A 2 H18F H 1.1165 -0.3094 0.3114 0.255 Uiso 0.812(10) 1 calc PR A 2 C19P C 0.9391(16) -0.4746(10) 0.2805(5) 0.143(6) Uani 0.812(10) 1 d PDU A 2 H19D H 0.8446 -0.5080 0.2780 0.215 Uiso 0.812(10) 1 calc PR A 2 H19E H 0.9820 -0.4977 0.3101 0.215 Uiso 0.812(10) 1 calc PR A 2 H19F H 0.9977 -0.5018 0.2547 0.215 Uiso 0.812(10) 1 calc PR A 2 C20P C 0.8824(12) -0.3303(10) 0.0985(3) 0.099(3) Uani 0.812(10) 1 d PDU A 2 H20P H 0.8199 -0.2915 0.0753 0.118 Uiso 0.812(10) 1 calc PR A 2 C21P C 0.8798(18) -0.4598(10) 0.0879(5) 0.133(5) Uani 0.812(10) 1 d PDU A 2 H21D H 0.9161 -0.4732 0.0565 0.199 Uiso 0.812(10) 1 calc PR A 2 H21E H 0.7826 -0.4882 0.0900 0.199 Uiso 0.812(10) 1 calc PR A 2 H21F H 0.9390 -0.5005 0.1105 0.199 Uiso 0.812(10) 1 calc PR A 2 C22P C 1.0317(15) -0.2816(14) 0.0925(6) 0.141(6) Uani 0.812(10) 1 d PDU A 2 H22D H 1.0661 -0.2990 0.0611 0.212 Uiso 0.812(10) 1 calc PR A 2 H22E H 1.0949 -0.3164 0.1155 0.212 Uiso 0.812(10) 1 calc PR A 2 H22F H 1.0297 -0.1983 0.0970 0.212 Uiso 0.812(10) 1 calc PR A 2 C23P C 0.8169(11) 0.2292(9) 0.0222(4) 0.063(3) Uani 0.812(10) 1 d PDU A 2 C24P C 0.7780(13) 0.3663(7) -0.0432(4) 0.081(4) Uani 0.812(10) 1 d PD A 2 H24P H 0.8822 0.3766 -0.0394 0.097 Uiso 0.812(10) 1 calc PR A 2 C25P C 0.7072(10) 0.4803(8) -0.0312(4) 0.085(3) Uani 0.812(10) 1 d PD A 2 C26P C 0.523(3) 0.5773(15) 0.0116(9) 0.129(6) Uani 0.812(10) 1 d PDU A 2 H26D H 0.4673 0.5634 0.0398 0.194 Uiso 0.812(10) 1 calc PR A 2 H26E H 0.4597 0.5988 -0.0139 0.194 Uiso 0.812(10) 1 calc PR A 2 H26F H 0.5902 0.6396 0.0173 0.194 Uiso 0.812(10) 1 calc PR A 2 C27P C 0.7494(12) 0.3367(8) -0.0951(3) 0.084(3) Uani 0.812(10) 1 d PD A 2 H27C H 0.6474 0.3205 -0.0990 0.101 Uiso 0.812(10) 1 calc PR A 2 H27D H 0.7722 0.4047 -0.1143 0.101 Uiso 0.812(10) 1 calc PR A 2 C28P C 0.8314(8) 0.2365(5) -0.1130(3) 0.075(3) Uiso 0.812(10) 1 d PGD A 2 C29P C 0.7659(7) 0.1317(6) -0.1225(3) 0.110(4) Uiso 0.812(10) 1 d PGD A 2 H29P H 0.6676 0.1232 -0.1171 0.131 Uiso 0.812(10) 1 d PG A 2 C30P C 0.8440(9) 0.0389(5) -0.1400(3) 0.137(4) Uiso 0.812(10) 1 d PG A 2 H30P H 0.7982 -0.0324 -0.1453 0.164 Uiso 0.812(10) 1 d PG A 2 C31P C 0.9878(10) 0.0495(7) -0.1500(3) 0.126(4) Uiso 0.812(10) 1 d PG A 2 H31P H 1.0397 -0.0130 -0.1624 0.151 Uiso 0.812(10) 1 d PG A 2 C32P C 1.0530(7) 0.1546(8) -0.1410(3) 0.118(5) Uiso 0.812(10) 1 d PG A 2 H32P H 1.1505 0.1639 -0.1477 0.141 Uiso 0.812(10) 1 d PG A 2 C33P C 0.9762(8) 0.2468(6) -0.1224(3) 0.088(3) Uiso 0.812(10) 1 d PGDU A 2 H33P H 1.0230 0.3171 -0.1162 0.106 Uiso 0.812(10) 1 d PG 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 N1P 0.054(3) 0.094(5) 0.085(6) 0.037(4) 0.000(3) -0.003(3) O1P 0.097(5) 0.082(4) 0.102(5) 0.001(3) -0.018(3) -0.020(4) O2P 0.053(3) 0.094(5) 0.083(7) 0.023(4) -0.002(4) -0.005(3) O3P 0.116(6) 0.092(5) 0.154(8) 0.040(5) 0.004(6) 0.022(4) O4P 0.116(7) 0.102(5) 0.100(8) -0.014(4) 0.026(5) 0.004(4) C7P 0.066(4) 0.056(4) 0.072(5) -0.007(3) 0.004(4) -0.001(4) C14P 0.078(5) 0.080(5) 0.082(6) 0.013(4) 0.020(4) 0.010(4) C15P 0.094(6) 0.094(6) 0.116(8) 0.006(5) 0.041(6) -0.011(5) C16P 0.099(6) 0.080(6) 0.084(6) -0.004(4) 0.001(5) 0.006(5) C17P 0.144(8) 0.157(8) 0.120(7) 0.090(6) 0.051(6) 0.079(7) C18P 0.155(10) 0.211(13) 0.144(10) 0.106(10) 0.000(9) -0.009(10) C19P 0.131(10) 0.152(10) 0.147(12) 0.086(9) -0.030(9) 0.009(8) C20P 0.101(7) 0.115(8) 0.080(6) 0.016(5) 0.015(5) 0.048(6) C21P 0.154(11) 0.114(9) 0.130(11) -0.020(8) 0.032(9) 0.025(9) C22P 0.145(11) 0.148(13) 0.131(10) 0.024(10) 0.048(9) -0.018(11) C23P 0.052(4) 0.082(5) 0.056(4) 0.003(4) 0.003(3) 0.021(4) C24P 0.071(6) 0.092(7) 0.080(7) 0.013(5) -0.002(5) -0.003(5) C25P 0.083(7) 0.097(9) 0.076(8) 0.010(5) -0.011(5) -0.003(5) C26P 0.154(14) 0.106(8) 0.128(15) -0.022(9) 0.039(9) 0.015(9) C27P 0.080(6) 0.110(7) 0.063(5) 0.029(5) -0.005(5) -0.014(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1R C23R 1.337(11) . ? N1R C24R 1.444(12) . ? N1R H1R 0.8600 . ? O1R C7R 1.230(11) . ? O2R C23R 1.225(11) . ? O3R C25R 1.190(11) . ? O4R C25R 1.290(11) . ? O4R C26R 1.435(12) . ? C1R C2R 1.378(10) . ? C1R C6R 1.396(10) . ? C1R C14R 1.495(10) . ? C2R C3R 1.371(10) . ? C2R H2R 0.9300 . ? C3R C4R 1.372(11) . ? C3R C17R 1.497(10) . ? C4R C5R 1.418(10) . ? C4R H4R 0.9300 . ? C5R C6R 1.383(10) . ? C5R C20R 1.524(11) . ? C6R C7R 1.505(10) . ? C7R C8R 1.481(10) . ? C8R C9R 1.387(11) . ? C8R C13R 1.391(11) . ? C9R C10R 1.373(11) . ? C9R H9R 0.9300 . ? C10R C11R 1.378(10) . ? C10R H10R 0.9300 . ? C11R C12R 1.391(10) . ? C11R C23R 1.483(10) . ? C12R C13R 1.363(11) . ? C12R H12R 0.9300 . ? C13R H13R 0.9300 . ? C14R C15R 1.507(11) . ? C14R C16R 1.522(12) . ? C14R H14R 0.9800 . ? C15R H15A 0.9600 . ? C15R H15B 0.9600 . ? C15R H15C 0.9600 . ? C16R H16A 0.9600 . ? C16R H16B 0.9600 . ? C16R H16C 0.9600 . ? C17R C19R 1.435(11) . ? C17R C18R 1.490(11) . ? C17R H17R 0.9800 . ? C18R H18A 0.9600 . ? C18R H18B 0.9600 . ? C18R H18C 0.9600 . ? C19R H19A 0.9600 . ? C19R H19B 0.9600 . ? C19R H19C 0.9600 . ? C20R C21R 1.501(12) . ? C20R C22R 1.518(11) . ? C20R H20R 0.9800 . ? C21R H21A 0.9600 . ? C21R H21B 0.9600 . ? C21R H21C 0.9600 . ? C22R H22A 0.9600 . ? C22R H22B 0.9600 . ? C22R H22C 0.9600 . ? C24R C25R 1.507(11) . ? C24R C27R 1.522(12) . ? C24R H24R 0.9800 . ? C26R H26A 0.9600 . ? C26R H26B 0.9600 . ? C26R H26C 0.9600 . ? C27R C28R 1.491(10) . ? C27R H27A 0.9700 . ? C27R H27B 0.9700 . ? C28R C29R 1.3754 . ? C28R C33R 1.3831 . ? C29R C30R 1.3701 . ? C29R H29R 0.9300 . ? C30R C31R 1.3771 . ? C30R H30R 0.9300 . ? C31R C32R 1.3617 . ? C31R H31R 0.9300 . ? C32R C33R 1.3725 . ? C32R H32R 0.9300 . ? C33R H33R 0.9300 . ? N1P C23P 1.340(7) . ? N1P C24P 1.432(7) . ? N1P H1P 0.8600 . ? O1P C7P 1.413(9) . ? O2P C23P 1.232(7) . ? O3P C25P 1.213(8) . ? O4P C25P 1.310(8) . ? O4P C26P 1.444(9) . ? C1P C6P 1.355(8) . ? C1P C2P 1.377(8) . ? C1P C14P 1.527(8) . ? C2P C3P 1.392(8) . ? C2P H2P 0.9300 . ? C3P C4P 1.375(8) . ? C3P C17P 1.551(8) . ? C4P C5P 1.404(8) . ? C4P H4P 0.9300 . ? C5P C6P 1.387(7) . ? C5P C20P 1.516(8) . ? C6P C7P 1.520(7) . ? C7P C8P 1.520(7) . ? C7P C14P 1.637(8) . ? C8P C9P 1.372(7) . ? C8P C13P 1.388(7) . ? C9P C10P 1.375(7) . ? C9P H9P 0.9300 . ? C10P C11P 1.366(7) . ? C10P H10P 0.9300 . ? C11P C12P 1.380(7) . ? C11P C23P 1.485(7) . ? C12P C13P 1.363(7) . ? C12P H12P 0.9300 . ? C13P H13P 0.9300 . ? C14P C16P 1.495(8) . ? C14P C15P 1.523(8) . ? C15P H15D 0.9600 . ? C15P H15E 0.9600 . ? C15P H15F 0.9600 . ? C16P H16D 0.9600 . ? C16P H16E 0.9600 . ? C16P H16F 0.9600 . ? C17P C19P 1.456(9) . ? C17P C18P 1.486(10) . ? C17P H17P 0.9800 . ? C18P H18D 0.9600 . ? C18P H18E 0.9600 . ? C18P H18F 0.9600 . ? C19P H19D 0.9600 . ? C19P H19E 0.9600 . ? C19P H19F 0.9600 . ? C20P C22P 1.504(9) . ? C20P C21P 1.508(9) . ? C20P H20P 0.9800 . ? C21P H21D 0.9600 . ? C21P H21E 0.9600 . ? C21P H21F 0.9600 . ? C22P H22D 0.9600 . ? C22P H22E 0.9600 . ? C22P H22F 0.9600 . ? C24P C25P 1.498(8) . ? C24P C27P 1.526(9) . ? C24P H24P 0.9800 . ? C26P H26D 0.9600 . ? C26P H26E 0.9600 . ? C26P H26F 0.9600 . ? C27P C28P 1.463(8) . ? C27P H27C 0.9700 . ? C27P H27D 0.9700 . ? C28P C29P 1.3689 . ? C28P C33P 1.3759 . ? C29P C30P 1.3762 . ? C29P H29P 0.9300 . ? C30P C31P 1.3694 . ? C30P H30P 0.9300 . ? C31P C32P 1.3674 . ? C31P H31P 0.9299 . ? C32P C33P 1.3743 . ? C32P H32P 0.9300 . ? C33P H33P 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23R N1R C24R 121(2) . . ? C23R N1R H1R 119.7 . . ? C24R N1R H1R 119.7 . . ? C25R O4R C26R 118(2) . . ? C2R C1R C6R 117.2(12) . . ? C2R C1R C14R 120.2(14) . . ? C6R C1R C14R 121.9(14) . . ? C3R C2R C1R 122.0(13) . . ? C3R C2R H2R 119.0 . . ? C1R C2R H2R 119.0 . . ? C2R C3R C4R 119.1(13) . . ? C2R C3R C17R 117.8(15) . . ? C4R C3R C17R 120.9(15) . . ? C3R C4R C5R 121.9(14) . . ? C3R C4R H4R 119.1 . . ? C5R C4R H4R 119.1 . . ? C6R C5R C4R 115.7(12) . . ? C6R C5R C20R 120.0(15) . . ? C4R C5R C20R 119.5(15) . . ? C5R C6R C1R 123.4(11) . . ? C5R C6R C7R 120.7(13) . . ? C1R C6R C7R 115.8(13) . . ? O1R C7R C8R 119.2(19) . . ? O1R C7R C6R 119.3(18) . . ? C8R C7R C6R 115.3(16) . . ? C9R C8R C13R 118.9(14) . . ? C9R C8R C7R 118.5(14) . . ? C13R C8R C7R 120.2(14) . . ? C10R C9R C8R 120.1(14) . . ? C10R C9R H9R 119.9 . . ? C8R C9R H9R 119.9 . . ? C9R C10R C11R 120.0(13) . . ? C9R C10R H10R 120.0 . . ? C11R C10R H10R 120.0 . . ? C10R C11R C12R 119.3(12) . . ? C10R C11R C23R 124.1(14) . . ? C12R C11R C23R 116.5(13) . . ? C13R C12R C11R 120.5(14) . . ? C13R C12R H12R 119.7 . . ? C11R C12R H12R 119.7 . . ? C12R C13R C8R 118.8(14) . . ? C12R C13R H13R 120.6 . . ? C8R C13R H13R 120.6 . . ? C1R C14R C15R 109.3(16) . . ? C1R C14R C16R 113.3(17) . . ? C15R C14R C16R 110.4(16) . . ? C1R C14R H14R 107.9 . . ? C15R C14R H14R 107.9 . . ? C16R C14R H14R 107.9 . . ? C14R C15R H15A 109.5 . . ? C14R C15R H15B 109.5 . . ? H15A C15R H15B 109.5 . . ? C14R C15R H15C 109.5 . . ? H15A C15R H15C 109.5 . . ? H15B C15R H15C 109.5 . . ? C14R C16R H16A 109.5 . . ? C14R C16R H16B 109.5 . . ? H16A C16R H16B 109.5 . . ? C14R C16R H16C 109.5 . . ? H16A C16R H16C 109.5 . . ? H16B C16R H16C 109.5 . . ? C19R C17R C18R 119.0(18) . . ? C19R C17R C3R 116.6(17) . . ? C18R C17R C3R 115.5(17) . . ? C19R C17R H17R 100.0 . . ? C18R C17R H17R 100.0 . . ? C3R C17R H17R 100.0 . . ? C17R C18R H18A 109.5 . . ? C17R C18R H18B 109.5 . . ? H18A C18R H18B 109.5 . . ? C17R C18R H18C 109.5 . . ? H18A C18R H18C 109.5 . . ? H18B C18R H18C 109.5 . . ? C17R C19R H19A 109.5 . . ? C17R C19R H19B 109.5 . . ? H19A C19R H19B 109.5 . . ? C17R C19R H19C 109.5 . . ? H19A C19R H19C 109.5 . . ? H19B C19R H19C 109.5 . . ? C21R C20R C22R 111.7(17) . . ? C21R C20R C5R 112.0(17) . . ? C22R C20R C5R 111.6(16) . . ? C21R C20R H20R 107.1 . . ? C22R C20R H20R 107.1 . . ? C5R C20R H20R 107.1 . . ? C20R C21R H21A 109.5 . . ? C20R C21R H21B 109.5 . . ? H21A C21R H21B 109.5 . . ? C20R C21R H21C 109.5 . . ? H21A C21R H21C 109.5 . . ? H21B C21R H21C 109.5 . . ? C20R C22R H22A 109.5 . . ? C20R C22R H22B 109.5 . . ? H22A C22R H22B 109.5 . . ? C20R C22R H22C 109.5 . . ? H22A C22R H22C 109.5 . . ? H22B C22R H22C 109.5 . . ? O2R C23R N1R 122(2) . . ? O2R C23R C11R 119.9(18) . . ? N1R C23R C11R 114.4(17) . . ? N1R C24R C25R 111.6(17) . . ? N1R C24R C27R 111.2(17) . . ? C25R C24R C27R 113.0(16) . . ? N1R C24R H24R 106.9 . . ? C25R C24R H24R 106.9 . . ? C27R C24R H24R 106.9 . . ? O3R C25R O4R 123.7(18) . . ? O3R C25R C24R 123.0(17) . . ? O4R C25R C24R 113.1(16) . . ? C28R C27R C24R 110.4(16) . . ? C28R C27R H27A 109.6 . . ? C24R C27R H27A 109.6 . . ? C28R C27R H27B 109.6 . . ? C24R C27R H27B 109.6 . . ? H27A C27R H27B 108.1 . . ? C29R C28R C33R 117.2 . . ? C29R C28R C27R 120.9(13) . . ? C33R C28R C27R 121.8(13) . . ? C30R C29R C28R 121.3 . . ? C29R C30R C31R 121.0 . . ? C32R C31R C30R 118.1 . . ? C31R C32R C33R 121.2 . . ? C32R C33R C28R 121.2 . . ? C23P N1P C24P 123.6(7) . . ? C23P N1P H1P 118.2 . . ? C24P N1P H1P 118.2 . . ? C25P O4P C26P 118.5(9) . . ? C6P C1P C2P 122.4(6) . . ? C6P C1P C14P 94.0(6) . . ? C2P C1P C14P 143.5(7) . . ? C1P C2P C3P 115.9(7) . . ? C1P C2P H2P 122.1 . . ? C3P C2P H2P 122.1 . . ? C4P C3P C2P 121.3(7) . . ? C4P C3P C17P 120.7(7) . . ? C2P C3P C17P 118.0(7) . . ? C3P C4P C5P 122.9(7) . . ? C3P C4P H4P 118.5 . . ? C5P C4P H4P 118.5 . . ? C6P C5P C4P 113.9(6) . . ? C6P C5P C20P 123.2(7) . . ? C4P C5P C20P 122.6(7) . . ? C1P C6P C5P 123.6(6) . . ? C1P C6P C7P 96.4(5) . . ? C5P C6P C7P 139.9(7) . . ? O1P C7P C8P 110.5(6) . . ? O1P C7P C6P 114.6(7) . . ? C8P C7P C6P 113.9(6) . . ? O1P C7P C14P 115.2(8) . . ? C8P C7P C14P 116.6(6) . . ? C6P C7P C14P 83.9(4) . . ? C9P C8P C13P 116.6(5) . . ? C9P C8P C7P 120.9(5) . . ? C13P C8P C7P 122.5(5) . . ? C8P C9P C10P 121.4(7) . . ? C8P C9P H9P 119.3 . . ? C10P C9P H9P 119.3 . . ? C11P C10P C9P 121.5(7) . . ? C11P C10P H10P 119.2 . . ? C9P C10P H10P 119.2 . . ? C10P C11P C12P 117.5(6) . . ? C10P C11P C23P 123.6(6) . . ? C12P C11P C23P 118.8(6) . . ? C13P C12P C11P 121.0(7) . . ? C13P C12P H12P 119.5 . . ? C11P C12P H12P 119.5 . . ? C12P C13P C8P 121.8(6) . . ? C12P C13P H13P 119.1 . . ? C8P C13P H13P 119.1 . . ? C16P C14P C15P 110.4(6) . . ? C16P C14P C1P 115.1(7) . . ? C15P C14P C1P 114.3(7) . . ? C16P C14P C7P 119.6(6) . . ? C15P C14P C7P 110.2(6) . . ? C1P C14P C7P 85.3(5) . . ? C14P C15P H15D 109.5 . . ? C14P C15P H15E 109.5 . . ? H15D C15P H15E 109.5 . . ? C14P C15P H15F 109.5 . . ? H15D C15P H15F 109.5 . . ? H15E C15P H15F 109.5 . . ? C14P C16P H16D 109.5 . . ? C14P C16P H16E 109.5 . . ? H16D C16P H16E 109.5 . . ? C14P C16P H16F 109.5 . . ? H16D C16P H16F 109.5 . . ? H16E C16P H16F 109.5 . . ? C19P C17P C18P 112.2(9) . . ? C19P C17P C3P 111.5(9) . . ? C18P C17P C3P 110.4(8) . . ? C19P C17P H17P 107.5 . . ? C18P C17P H17P 107.5 . . ? C3P C17P H17P 107.5 . . ? C17P C18P H18D 109.5 . . ? C17P C18P H18E 109.5 . . ? H18D C18P H18E 109.5 . . ? C17P C18P H18F 109.5 . . ? H18D C18P H18F 109.5 . . ? H18E C18P H18F 109.5 . . ? C17P C19P H19D 109.5 . . ? C17P C19P H19E 109.5 . . ? H19D C19P H19E 109.5 . . ? C17P C19P H19F 109.5 . . ? H19D C19P H19F 109.5 . . ? H19E C19P H19F 109.5 . . ? C22P C20P C21P 110.8(9) . . ? C22P C20P C5P 111.8(8) . . ? C21P C20P C5P 111.2(8) . . ? C22P C20P H20P 107.6 . . ? C21P C20P H20P 107.6 . . ? C5P C20P H20P 107.6 . . ? C20P C21P H21D 109.5 . . ? C20P C21P H21E 109.5 . . ? H21D C21P H21E 109.5 . . ? C20P C21P H21F 109.5 . . ? H21D C21P H21F 109.5 . . ? H21E C21P H21F 109.5 . . ? C20P C22P H22D 109.5 . . ? C20P C22P H22E 109.5 . . ? H22D C22P H22E 109.5 . . ? C20P C22P H22F 109.5 . . ? H22D C22P H22F 109.5 . . ? H22E C22P H22F 109.5 . . ? O2P C23P N1P 120.6(7) . . ? O2P C23P C11P 122.9(6) . . ? N1P C23P C11P 116.3(6) . . ? N1P C24P C25P 113.4(8) . . ? N1P C24P C27P 110.9(7) . . ? C25P C24P C27P 109.4(8) . . ? N1P C24P H24P 107.7 . . ? C25P C24P H24P 107.7 . . ? C27P C24P H24P 107.7 . . ? O3P C25P O4P 123.2(9) . . ? O3P C25P C24P 122.2(8) . . ? O4P C25P C24P 114.6(7) . . ? O4P C26P H26D 109.5 . . ? O4P C26P H26E 109.5 . . ? H26D C26P H26E 109.5 . . ? O4P C26P H26F 109.5 . . ? H26D C26P H26F 109.5 . . ? H26E C26P H26F 109.5 . . ? C28P C27P C24P 114.4(6) . . ? C28P C27P H27C 108.7 . . ? C24P C27P H27C 108.7 . . ? C28P C27P H27D 108.7 . . ? C24P C27P H27D 108.7 . . ? H27C C27P H27D 107.6 . . ? C29P C28P C33P 118.0 . . ? C29P C28P C27P 121.3(5) . . ? C33P C28P C27P 120.6(5) . . ? C28P C29P C30P 120.7 . . ? C28P C29P H29P 119.7 . . ? C30P C29P H29P 119.7 . . ? C31P C30P C29P 121.2 . . ? C31P C30P H30P 119.4 . . ? C29P C30P H30P 119.4 . . ? C32P C31P C30P 118.1 . . ? C32P C31P H31P 120.9 . . ? C30P C31P H31P 120.9 . . ? C31P C32P C33P 120.9 . . ? C31P C32P H32P 119.6 . . ? C33P C32P H32P 119.6 . . ? C32P C33P C28P 121.0 . . ? C32P C33P H33P 119.5 . . ? C28P C33P H33P 119.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.199 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.037 #===END data_87.4%P _database_code_depnum_ccdc_archive 'CCDC 799261' #TrackingRef '- 1.cif' #==================================================================== # start Validation Reply Form _vrf_PLAT201_87.4%P ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 18 RESPONSE: In the crystal there are reactant and photoproduct molecules. Part of atoms were refined isotropically in order to decrease a large number of the parameters in the refinement. ; # end Validation Reply Form #==================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 N O4' _chemical_formula_weight 513.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.2671(14) _cell_length_b 11.4608(18) _cell_length_c 28.078(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2982.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 13.4 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14559 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 4.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2960 _reflns_number_gt 1998 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSALIS (Oxford Diffraction, 2003)' _computing_cell_refinement 'CRYSALIS (Oxford Diffraction, 2003)' _computing_data_reduction 'CRYSALIS (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Owing to a reactant-product disorder, the following weak restraints from SHELXL97 were applied: DFIX, DANG and SIMU. DFIX and DANG restrained bond lengths and valence angles to target values. The target values were taken from the structures of the pure reactant and the pure product of crystal 1a. SIMU restrained displacement parameters of atoms of the products. ; _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^)+(0.1227P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration syn _refine_ls_number_reflns 2960 _refine_ls_number_parameters 384 _refine_ls_number_restraints 298 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.2259 _refine_ls_wR_factor_gt 0.2002 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.241 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1R N 0.729(6) 0.287(3) -0.0023(17) 0.079(12) Uiso 0.126(8) 1 d PDU A 1 H1R H 0.6387 0.2697 0.0002 0.095 Uiso 0.126(8) 1 calc PR A 1 O1R O 0.545(4) -0.264(3) 0.0870(14) 0.099(16) Uiso 0.126(8) 1 d PDU A 1 O2R O 0.934(10) 0.269(7) 0.039(4) 0.066(17) Uiso 0.126(8) 1 d PDU A 1 O3R O 0.762(6) 0.591(3) -0.025(2) 0.12(3) Uiso 0.126(8) 1 d PD A 1 O4R O 0.576(6) 0.491(4) -0.002(4) 0.093(11) Uiso 0.126(8) 1 d PDU A 1 C1R C 0.630(3) -0.223(3) 0.1931(9) 0.058(13) Uiso 0.126(8) 1 d PDU A 1 C2R C 0.685(3) -0.269(3) 0.2347(9) 0.065(9) Uiso 0.126(8) 1 d PDU A 1 H2R H 0.6317 -0.2625 0.2626 0.078 Uiso 0.126(8) 1 calc PR A 1 C3R C 0.817(4) -0.324(4) 0.2364(9) 0.072(9) Uiso 0.126(8) 1 d PDU A 1 C4R C 0.901(3) -0.322(5) 0.1962(10) 0.07(2) Uiso 0.126(8) 1 d PD A 1 H4R H 0.9981 -0.3415 0.1987 0.085 Uiso 0.126(8) 1 calc PR A 1 C5R C 0.844(3) -0.292(4) 0.1510(9) 0.063(15) Uiso 0.126(8) 1 d PDU A 1 C6R C 0.709(3) -0.240(4) 0.1515(8) 0.07(5) Uiso 0.126(8) 1 d PD A 1 C7R C 0.640(4) -0.206(3) 0.1053(10) 0.099(11) Uiso 0.126(8) 1 d PDU A 1 C8R C 0.695(4) -0.100(3) 0.0815(11) 0.080(9) Uiso 0.126(8) 1 d PDU A 1 C9R C 0.636(4) -0.065(3) 0.0386(10) 0.061(12) Uiso 0.126(8) 1 d PD A 1 H9R H 0.5672 -0.1115 0.0236 0.073 Uiso 0.126(8) 1 calc PR A 1 C10R C 0.677(4) 0.039(3) 0.0180(11) 0.058(16) Uiso 0.126(8) 1 d PD A 1 H10R H 0.6389 0.0603 -0.0114 0.069 Uiso 0.126(8) 1 calc PR A 1 C11R C 0.775(5) 0.110(3) 0.0406(13) 0.053(15) Uiso 0.126(8) 1 d PDU A 1 C12R C 0.838(4) 0.072(3) 0.0827(13) 0.065(18) Uiso 0.126(8) 1 d PD A 1 H12R H 0.9076 0.1181 0.0973 0.078 Uiso 0.126(8) 1 calc PR A 1 C13R C 0.800(4) -0.031(3) 0.1029(12) 0.063(12) Uiso 0.126(8) 1 d PD A 1 H13R H 0.8436 -0.0558 0.1309 0.076 Uiso 0.126(8) 1 calc PR A 1 C14R C 0.508(4) -0.137(3) 0.1962(14) 0.093(12) Uiso 0.126(8) 1 d PDU A 1 H14R H 0.4737 -0.1220 0.1637 0.111 Uiso 0.126(8) 1 calc PR A 1 C15R C 0.385(4) -0.191(5) 0.224(2) 0.114(17) Uiso 0.126(8) 1 d PDU A 1 H15A H 0.3043 -0.1385 0.2239 0.170 Uiso 0.126(8) 1 calc PR A 1 H15B H 0.4154 -0.2050 0.2561 0.170 Uiso 0.126(8) 1 calc PR A 1 H15C H 0.3575 -0.2634 0.2094 0.170 Uiso 0.126(8) 1 calc PR A 1 C16R C 0.553(7) -0.022(4) 0.218(3) 0.13(2) Uiso 0.126(8) 1 d PDU A 1 H16A H 0.4711 0.0294 0.2200 0.201 Uiso 0.126(8) 1 calc PR A 1 H16B H 0.6266 0.0137 0.1989 0.201 Uiso 0.126(8) 1 calc PR A 1 H16C H 0.5902 -0.0350 0.2497 0.201 Uiso 0.126(8) 1 calc PR A 1 C17R C 0.882(5) -0.348(5) 0.2841(11) 0.105(12) Uiso 0.126(8) 1 d PDU A 1 H17R H 0.8005 -0.3313 0.3054 0.126 Uiso 0.126(8) 1 calc PR A 1 C18R C 0.989(8) -0.259(8) 0.300(3) 0.15(2) Uiso 0.126(8) 1 d PDU A 1 H18A H 0.9636 -0.1838 0.2869 0.227 Uiso 0.126(8) 1 calc PR A 1 H18B H 1.0835 -0.2802 0.2890 0.227 Uiso 0.126(8) 1 calc PR A 1 H18C H 0.9892 -0.2541 0.3341 0.227 Uiso 0.126(8) 1 calc PR A 1 C19R C 0.912(13) -0.468(6) 0.295(3) 0.15(2) Uiso 0.126(8) 1 d PDU A 1 H19A H 0.8355 -0.5162 0.2836 0.218 Uiso 0.126(8) 1 calc PR A 1 H19B H 0.9199 -0.4768 0.3292 0.218 Uiso 0.126(8) 1 calc PR A 1 H19C H 1.0014 -0.4905 0.2806 0.218 Uiso 0.126(8) 1 calc PR A 1 C20R C 0.897(5) -0.356(4) 0.1068(12) 0.079(11) Uiso 0.126(8) 1 d PDU A 1 H20R H 0.8344 -0.3319 0.0804 0.095 Uiso 0.126(8) 1 calc PR A 1 C21R C 0.884(10) -0.486(4) 0.111(3) 0.13(2) Uiso 0.126(8) 1 d PDU A 1 H21A H 0.9171 -0.5220 0.0826 0.188 Uiso 0.126(8) 1 calc PR A 1 H21B H 0.7854 -0.5063 0.1170 0.188 Uiso 0.126(8) 1 calc PR A 1 H21C H 0.9425 -0.5119 0.1376 0.188 Uiso 0.126(8) 1 calc PR A 1 C22R C 1.050(8) -0.319(8) 0.094(4) 0.13(2) Uiso 0.126(8) 1 d PDU A 1 H22A H 1.0587 -0.2361 0.0969 0.201 Uiso 0.126(8) 1 calc PR A 1 H22B H 1.0694 -0.3414 0.0615 0.201 Uiso 0.126(8) 1 calc PR A 1 H22C H 1.1168 -0.3570 0.1147 0.201 Uiso 0.126(8) 1 calc PR A 1 C23R C 0.827(6) 0.223(4) 0.021(2) 0.065(12) Uiso 0.126(8) 1 d PDU A 1 C24R C 0.772(6) 0.383(2) -0.0318(12) 0.062(10) Uiso 0.126(8) 1 d PDU A 1 H24R H 0.8765 0.3915 -0.0271 0.074 Uiso 0.126(8) 1 calc PR A 1 C25R C 0.708(6) 0.498(3) -0.0169(18) 0.096(12) Uiso 0.126(8) 1 d PDU A 1 C26R C 0.498(8) 0.598(6) 0.004(4) 0.096(19) Uiso 0.126(8) 1 d PDU A 1 H26A H 0.4340 0.6086 -0.0228 0.144 Uiso 0.126(8) 1 calc PR A 1 H26B H 0.5643 0.6619 0.0054 0.144 Uiso 0.126(8) 1 calc PR A 1 H26C H 0.4424 0.5946 0.0327 0.144 Uiso 0.126(8) 1 calc PR A 1 C27R C 0.752(6) 0.358(3) -0.0845(13) 0.08(2) Uiso 0.126(8) 1 d PD A 1 H27A H 0.6501 0.3493 -0.0913 0.100 Uiso 0.126(8) 1 calc PR A 1 H27B H 0.7880 0.4236 -0.1030 0.100 Uiso 0.126(8) 1 calc PR A 1 C28R C 0.830(4) 0.250(2) -0.0987(14) 0.090(14) Uiso 0.126(8) 1 d PGDU A 1 C29R C 0.758(3) 0.146(3) -0.1026(13) 0.066(12) Uiso 0.126(8) 1 d PGD A 1 H29R H 0.6593 0.1433 -0.0966 0.080 Uiso 0.126(8) 1 d PG A 1 C30R C 0.828(3) 0.045(2) -0.1153(14) 0.088(15) Uiso 0.126(8) 1 d PG A 1 H30R H 0.7769 -0.0242 -0.1174 0.105 Uiso 0.126(8) 1 d PG A 1 C31R C 0.974(3) 0.046(3) -0.1249(15) 0.081(12) Uiso 0.126(8) 1 d PGU A 1 H31R H 1.0222 -0.0227 -0.1329 0.097 Uiso 0.126(8) 1 d PG A 1 C32R C 1.046(3) 0.149(3) -0.1223(16) 0.081(15) Uiso 0.126(8) 1 d PG A 1 H32R H 1.1437 0.1518 -0.1295 0.098 Uiso 0.126(8) 1 d PG A 1 C33R C 0.976(4) 0.250(3) -0.1093(16) 0.100(16) Uiso 0.126(8) 1 d PGDU A 1 H33R H 1.0277 0.3195 -0.1076 0.120 Uiso 0.126(8) 1 d PG A 1 N1P N 0.7368(8) 0.2698(6) -0.0130(2) 0.073(2) Uani 0.874(8) 1 d PDU A 2 H1P H 0.6537 0.2385 -0.0179 0.088 Uiso 0.874(8) 1 calc PR A 2 O1P O 0.4966(6) -0.2354(4) 0.09855(19) 0.0781(15) Uani 0.874(8) 1 d PDU A 2 O2P O 0.9363(13) 0.2695(12) 0.0313(6) 0.076(3) Uani 0.874(8) 1 d PDU A 2 O3P O 0.7435(9) 0.5698(7) -0.0486(4) 0.124(3) Uani 0.874(8) 1 d PD A 2 O4P O 0.6021(10) 0.4670(6) 0.0006(4) 0.100(2) Uani 0.874(8) 1 d PDU A 2 C1P C 0.6539(7) -0.2057(7) 0.1984(2) 0.075(3) Uiso 0.874(8) 1 d PDU A 2 C2P C 0.7229(8) -0.2397(6) 0.2394(2) 0.083(2) Uiso 0.874(8) 1 d PDU A 2 H2P H 0.6897 -0.2180 0.2694 0.099 Uiso 0.874(8) 1 calc PR A 2 C3P C 0.8453(8) -0.3081(8) 0.2335(3) 0.089(2) Uiso 0.874(8) 1 d PDU A 2 C4P C 0.8909(9) -0.3404(9) 0.1886(3) 0.089(4) Uiso 0.874(8) 1 d PD A 2 H4P H 0.9712 -0.3887 0.1860 0.107 Uiso 0.874(8) 1 calc PR A 2 C5P C 0.8224(9) -0.3042(8) 0.1466(2) 0.080(3) Uiso 0.874(8) 1 d PDU A 2 C6P C 0.7009(8) -0.2368(7) 0.1546(3) 0.072(7) Uiso 0.874(8) 1 d PD A 2 C7P C 0.5897(6) -0.1675(4) 0.12657(18) 0.0616(17) Uani 0.874(8) 1 d PDU A 2 C8P C 0.6518(6) -0.0662(5) 0.09848(19) 0.0540(15) Uiso 0.874(8) 1 d PDU A 2 C9P C 0.6024(7) -0.0409(5) 0.0539(2) 0.0621(17) Uiso 0.874(8) 1 d PD A 2 H9P H 0.5308 -0.0872 0.0404 0.075 Uiso 0.874(8) 1 calc PR A 2 C10P C 0.6564(8) 0.0514(6) 0.0286(3) 0.070(3) Uiso 0.874(8) 1 d PD A 2 H10P H 0.6209 0.0663 -0.0018 0.084 Uiso 0.874(8) 1 calc PR A 2 C11P C 0.7608(8) 0.1221(6) 0.0468(2) 0.057(2) Uiso 0.874(8) 1 d PDU A 2 C12P C 0.8143(7) 0.0955(6) 0.0913(2) 0.061(2) Uiso 0.874(8) 1 d PD A 2 H12P H 0.8866 0.1415 0.1045 0.073 Uiso 0.874(8) 1 calc PR A 2 C13P C 0.7627(7) 0.0029(5) 0.1161(2) 0.0630(18) Uiso 0.874(8) 1 d PD A 2 H13P H 0.8026 -0.0147 0.1456 0.076 Uiso 0.874(8) 1 calc PR A 2 C14P C 0.5246(7) -0.1373(5) 0.1795(2) 0.079(2) Uani 0.874(8) 1 d PDU A 2 C15P C 0.3802(7) -0.1982(7) 0.1873(3) 0.098(3) Uani 0.874(8) 1 d PDU A 2 H15D H 0.3884 -0.2787 0.1783 0.147 Uiso 0.874(8) 1 calc PR A 2 H15E H 0.3075 -0.1612 0.1682 0.147 Uiso 0.874(8) 1 calc PR A 2 H15F H 0.3538 -0.1930 0.2203 0.147 Uiso 0.874(8) 1 calc PR A 2 C16P C 0.5145(9) -0.0135(6) 0.1955(3) 0.086(2) Uani 0.874(8) 1 d PDU A 2 H16D H 0.4308 0.0222 0.1816 0.130 Uiso 0.874(8) 1 calc PR A 2 H16E H 0.5993 0.0280 0.1856 0.130 Uiso 0.874(8) 1 calc PR A 2 H16F H 0.5070 -0.0109 0.2296 0.130 Uiso 0.874(8) 1 calc PR A 2 C17P C 0.9288(10) -0.3492(9) 0.2781(3) 0.114(3) Uani 0.874(8) 1 d PDU A 2 H17P H 0.8723 -0.3242 0.3058 0.137 Uiso 0.874(8) 1 calc PR A 2 C18P C 1.0706(13) -0.2916(13) 0.2819(4) 0.172(6) Uani 0.874(8) 1 d PDU A 2 H18D H 1.0583 -0.2086 0.2798 0.259 Uiso 0.874(8) 1 calc PR A 2 H18E H 1.1319 -0.3178 0.2566 0.259 Uiso 0.874(8) 1 calc PR A 2 H18F H 1.1138 -0.3108 0.3120 0.259 Uiso 0.874(8) 1 calc PR A 2 C19P C 0.9375(16) -0.4764(9) 0.2803(5) 0.155(7) Uani 0.874(8) 1 d PDU A 2 H19D H 0.8424 -0.5089 0.2778 0.233 Uiso 0.874(8) 1 calc PR A 2 H19E H 0.9798 -0.4994 0.3101 0.233 Uiso 0.874(8) 1 calc PR A 2 H19F H 0.9961 -0.5045 0.2546 0.233 Uiso 0.874(8) 1 calc PR A 2 C20P C 0.8823(10) -0.3304(8) 0.0977(3) 0.092(3) Uani 0.874(8) 1 d PDU A 2 H20P H 0.8217 -0.2904 0.0743 0.110 Uiso 0.874(8) 1 calc PR A 2 C21P C 0.8759(13) -0.4600(7) 0.0873(4) 0.119(3) Uani 0.874(8) 1 d PDU A 2 H21D H 0.9121 -0.4744 0.0558 0.179 Uiso 0.874(8) 1 calc PR A 2 H21E H 0.7777 -0.4862 0.0894 0.179 Uiso 0.874(8) 1 calc PR A 2 H21F H 0.9337 -0.5014 0.1101 0.179 Uiso 0.874(8) 1 calc PR A 2 C22P C 1.0339(14) -0.2857(14) 0.0922(6) 0.145(5) Uani 0.874(8) 1 d PDU A 2 H22D H 1.0682 -0.3032 0.0607 0.218 Uiso 0.874(8) 1 calc PR A 2 H22E H 1.0953 -0.3225 0.1152 0.218 Uiso 0.874(8) 1 calc PR A 2 H22F H 1.0351 -0.2028 0.0970 0.218 Uiso 0.874(8) 1 calc PR A 2 C23P C 0.8178(9) 0.2267(8) 0.0221(3) 0.064(2) Uani 0.874(8) 1 d PDU A 2 C24P C 0.7788(9) 0.3646(6) -0.0430(2) 0.074(2) Uani 0.874(8) 1 d PDU A 2 H24P H 0.8831 0.3752 -0.0393 0.089 Uiso 0.874(8) 1 calc PR A 2 C25P C 0.7079(9) 0.4777(6) -0.0302(3) 0.087(2) Uani 0.874(8) 1 d PDU A 2 C26P C 0.5233(15) 0.5702(10) 0.0147(5) 0.123(5) Uani 0.874(8) 1 d PDU A 2 H26D H 0.4603 0.5514 0.0408 0.185 Uiso 0.874(8) 1 calc PR A 2 H26E H 0.4672 0.5980 -0.0117 0.185 Uiso 0.874(8) 1 calc PR A 2 H26F H 0.5900 0.6296 0.0245 0.185 Uiso 0.874(8) 1 calc PR A 2 C27P C 0.7501(10) 0.3370(7) -0.0952(3) 0.082(3) Uani 0.874(8) 1 d PD A 2 H27C H 0.6478 0.3223 -0.0993 0.098 Uiso 0.874(8) 1 calc PR A 2 H27D H 0.7745 0.4049 -0.1142 0.098 Uiso 0.874(8) 1 calc PR A 2 C28P C 0.8308(6) 0.2366(4) -0.1133(2) 0.0720(19) Uiso 0.874(8) 1 d PGDU A 2 C29P C 0.7651(5) 0.1320(5) -0.1224(3) 0.108(3) Uiso 0.874(8) 1 d PGD A 2 H29P H 0.6667 0.1236 -0.1168 0.130 Uiso 0.874(8) 1 d PG A 2 C30P C 0.8432(7) 0.0390(4) -0.1396(3) 0.133(4) Uiso 0.874(8) 1 d PG A 2 H30P H 0.7973 -0.0322 -0.1445 0.160 Uiso 0.874(8) 1 d PG A 2 C31P C 0.9872(7) 0.0492(5) -0.1497(3) 0.119(3) Uiso 0.874(8) 1 d PGU A 2 H31P H 1.0391 -0.0134 -0.1619 0.142 Uiso 0.874(8) 1 d PG A 2 C32P C 1.0525(5) 0.1542(6) -0.1412(3) 0.107(3) Uiso 0.874(8) 1 d PG A 2 H32P H 1.1502 0.1632 -0.1480 0.128 Uiso 0.874(8) 1 d PG A 2 C33P C 0.9758(6) 0.2465(4) -0.1229(2) 0.082(2) Uiso 0.874(8) 1 d PGDU A 2 H33P H 1.0227 0.3167 -0.1169 0.098 Uiso 0.874(8) 1 d PG 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 N1P 0.056(3) 0.089(4) 0.075(4) 0.023(4) 0.002(3) -0.004(3) O1P 0.080(3) 0.070(3) 0.084(3) -0.010(3) -0.003(3) -0.009(3) O2P 0.056(3) 0.089(4) 0.084(8) 0.014(4) -0.006(4) -0.001(2) O3P 0.119(5) 0.092(4) 0.162(8) 0.030(5) 0.012(6) 0.024(4) O4P 0.113(5) 0.088(4) 0.099(4) -0.013(4) 0.015(5) 0.014(4) C7P 0.058(3) 0.057(3) 0.070(4) -0.005(3) 0.004(3) -0.001(3) C14P 0.073(4) 0.074(5) 0.089(5) 0.008(4) 0.019(4) 0.007(4) C15P 0.092(5) 0.093(5) 0.108(7) 0.005(4) 0.036(5) -0.011(5) C16P 0.092(5) 0.086(5) 0.082(5) 0.003(4) -0.001(4) 0.008(4) C17P 0.127(7) 0.129(8) 0.085(6) 0.045(5) 0.008(5) 0.029(7) C18P 0.173(11) 0.211(13) 0.133(10) 0.090(9) -0.060(9) -0.057(11) C19P 0.143(10) 0.149(10) 0.175(13) 0.093(9) -0.053(11) -0.007(8) C20P 0.096(5) 0.104(6) 0.076(5) 0.013(4) 0.006(4) 0.035(5) C21P 0.139(8) 0.108(7) 0.111(7) -0.016(6) 0.013(7) 0.018(7) C22P 0.134(9) 0.171(13) 0.130(8) 0.007(9) 0.049(7) -0.026(10) C23P 0.049(3) 0.083(5) 0.059(4) 0.004(3) 0.001(3) 0.018(3) C24P 0.066(4) 0.081(5) 0.076(5) 0.016(4) 0.003(4) -0.001(4) C25P 0.080(5) 0.089(6) 0.091(6) 0.013(5) -0.007(4) 0.008(5) C26P 0.140(9) 0.099(8) 0.130(12) -0.017(7) 0.015(9) 0.027(7) C27P 0.077(5) 0.103(6) 0.065(4) 0.028(4) -0.001(4) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1R C23R 1.339(11) . ? N1R C24R 1.440(11) . ? N1R H1R 0.8600 . ? O1R C7R 1.221(10) . ? O2R C23R 1.228(11) . ? O3R C25R 1.194(11) . ? O4R C25R 1.293(11) . ? O4R C26R 1.436(11) . ? C1R C2R 1.381(10) . ? C1R C6R 1.396(10) . ? C1R C14R 1.497(10) . ? C2R C3R 1.369(10) . ? C2R H2R 0.9300 . ? C3R C4R 1.373(10) . ? C3R C17R 1.497(10) . ? C4R C5R 1.417(10) . ? C4R H4R 0.9300 . ? C5R C6R 1.384(10) . ? C5R C20R 1.523(11) . ? C6R C7R 1.499(10) . ? C7R C8R 1.474(10) . ? C8R C13R 1.385(10) . ? C8R C9R 1.386(10) . ? C9R C10R 1.373(10) . ? C9R H9R 0.9300 . ? C10R C11R 1.376(10) . ? C10R H10R 0.9300 . ? C11R C12R 1.391(10) . ? C11R C23R 1.484(10) . ? C12R C13R 1.361(10) . ? C12R H12R 0.9300 . ? C13R H13R 0.9300 . ? C14R C15R 1.509(11) . ? C14R C16R 1.524(11) . ? C14R H14R 0.9800 . ? C15R H15A 0.9600 . ? C15R H15B 0.9600 . ? C15R H15C 0.9600 . ? C16R H16A 0.9600 . ? C16R H16B 0.9600 . ? C16R H16C 0.9600 . ? C17R C19R 1.440(11) . ? C17R C18R 1.493(11) . ? C17R H17R 0.9800 . ? C18R H18A 0.9600 . ? C18R H18B 0.9600 . ? C18R H18C 0.9600 . ? C19R H19A 0.9600 . ? C19R H19B 0.9600 . ? C19R H19C 0.9600 . ? C20R C21R 1.501(11) . ? C20R C22R 1.518(11) . ? C20R H20R 0.9800 . ? C21R H21A 0.9600 . ? C21R H21B 0.9600 . ? C21R H21C 0.9600 . ? C22R H22A 0.9600 . ? C22R H22B 0.9600 . ? C22R H22C 0.9600 . ? C24R C25R 1.503(10) . ? C24R C27R 1.518(11) . ? C24R H24R 0.9800 . ? C26R H26A 0.9600 . ? C26R H26B 0.9600 . ? C26R H26C 0.9600 . ? C27R C28R 1.490(10) . ? C27R H27A 0.9700 . ? C27R H27B 0.9700 . ? C28R C29R 1.3754 . ? C28R C33R 1.3831 . ? C29R C30R 1.3701 . ? C29R H29R 0.9300 . ? C30R C31R 1.3771 . ? C30R H30R 0.9300 . ? C31R C32R 1.3617 . ? C31R H31R 0.9300 . ? C32R C33R 1.3726 . ? C32R H32R 0.9300 . ? C33R H33R 0.9300 . ? N1P C23P 1.334(6) . ? N1P C24P 1.429(6) . ? N1P H1P 0.8600 . ? O1P C7P 1.403(6) . ? O2P C23P 1.230(6) . ? O3P C25P 1.221(7) . ? O4P C25P 1.314(7) . ? O4P C26P 1.445(8) . ? C1P C6P 1.354(8) . ? C1P C2P 1.373(7) . ? C1P C14P 1.527(7) . ? C2P C3P 1.388(7) . ? C2P H2P 0.9300 . ? C3P C4P 1.381(8) . ? C3P C17P 1.546(7) . ? C4P C5P 1.401(7) . ? C4P H4P 0.9300 . ? C5P C6P 1.383(7) . ? C5P C20P 1.510(7) . ? C6P C7P 1.520(7) . ? C7P C8P 1.517(6) . ? C7P C14P 1.642(7) . ? C8P C9P 1.365(6) . ? C8P C13P 1.388(6) . ? C9P C10P 1.368(7) . ? C9P H9P 0.9300 . ? C10P C11P 1.361(6) . ? C10P H10P 0.9300 . ? C11P C12P 1.379(6) . ? C11P C23P 1.484(6) . ? C12P C13P 1.355(6) . ? C12P H12P 0.9300 . ? C13P H13P 0.9300 . ? C14P C16P 1.491(7) . ? C14P C15P 1.525(7) . ? C15P H15D 0.9600 . ? C15P H15E 0.9600 . ? C15P H15F 0.9600 . ? C16P H16D 0.9600 . ? C16P H16E 0.9600 . ? C16P H16F 0.9600 . ? C17P C19P 1.461(9) . ? C17P C18P 1.474(9) . ? C17P H17P 0.9800 . ? C18P H18D 0.9600 . ? C18P H18E 0.9600 . ? C18P H18F 0.9600 . ? C19P H19D 0.9600 . ? C19P H19E 0.9600 . ? C19P H19F 0.9600 . ? C20P C22P 1.504(8) . ? C20P C21P 1.515(8) . ? C20P H20P 0.9800 . ? C21P H21D 0.9600 . ? C21P H21E 0.9600 . ? C21P H21F 0.9600 . ? C22P H22D 0.9600 . ? C22P H22E 0.9600 . ? C22P H22F 0.9600 . ? C24P C25P 1.496(7) . ? C24P C27P 1.522(8) . ? C24P H24P 0.9800 . ? C26P H26D 0.9600 . ? C26P H26E 0.9600 . ? C26P H26F 0.9600 . ? C27P C28P 1.463(7) . ? C27P H27C 0.9700 . ? C27P H27D 0.9700 . ? C28P C29P 1.3689 . ? C28P C33P 1.3759 . ? C29P C30P 1.3762 . ? C29P H29P 0.9300 . ? C30P C31P 1.3694 . ? C30P H30P 0.9300 . ? C31P C32P 1.3674 . ? C31P H31P 0.9300 . ? C32P C33P 1.3743 . ? C32P H32P 0.9300 . ? C33P H33P 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23R N1R C24R 121(2) . . ? C23R N1R H1R 119.6 . . ? C24R N1R H1R 119.6 . . ? C25R O4R C26R 117(2) . . ? C2R C1R C6R 117.2(12) . . ? C2R C1R C14R 118.9(14) . . ? C6R C1R C14R 122.6(14) . . ? C3R C2R C1R 122.4(13) . . ? C3R C2R H2R 118.8 . . ? C1R C2R H2R 118.8 . . ? C2R C3R C4R 118.1(13) . . ? C2R C3R C17R 118.3(15) . . ? C4R C3R C17R 120.5(15) . . ? C3R C4R C5R 121.8(14) . . ? C3R C4R H4R 119.1 . . ? C5R C4R H4R 119.1 . . ? C6R C5R C4R 115.7(12) . . ? C6R C5R C20R 120.2(17) . . ? C4R C5R C20R 119.5(16) . . ? C5R C6R C1R 123.0(11) . . ? C5R C6R C7R 119.4(14) . . ? C1R C6R C7R 117.6(14) . . ? O1R C7R C8R 120.7(15) . . ? O1R C7R C6R 121.8(16) . . ? C8R C7R C6R 117.4(14) . . ? C13R C8R C9R 119.3(12) . . ? C13R C8R C7R 120.9(13) . . ? C9R C8R C7R 119.7(13) . . ? C10R C9R C8R 120.5(13) . . ? C10R C9R H9R 119.8 . . ? C8R C9R H9R 119.8 . . ? C9R C10R C11R 120.3(13) . . ? C9R C10R H10R 119.9 . . ? C11R C10R H10R 119.9 . . ? C10R C11R C12R 118.8(12) . . ? C10R C11R C23R 124.4(15) . . ? C12R C11R C23R 116.6(13) . . ? C13R C12R C11R 121.3(13) . . ? C13R C12R H12R 119.4 . . ? C11R C12R H12R 119.4 . . ? C12R C13R C8R 119.7(13) . . ? C12R C13R H13R 120.1 . . ? C8R C13R H13R 120.1 . . ? C1R C14R C15R 109.5(16) . . ? C1R C14R C16R 112.6(17) . . ? C15R C14R C16R 110.6(16) . . ? C1R C14R H14R 108.0 . . ? C15R C14R H14R 108.0 . . ? C16R C14R H14R 108.0 . . ? C14R C15R H15A 109.5 . . ? C14R C15R H15B 109.5 . . ? H15A C15R H15B 109.5 . . ? C14R C15R H15C 109.5 . . ? H15A C15R H15C 109.5 . . ? H15B C15R H15C 109.5 . . ? C14R C16R H16A 109.5 . . ? C14R C16R H16B 109.5 . . ? H16A C16R H16B 109.5 . . ? C14R C16R H16C 109.5 . . ? H16A C16R H16C 109.5 . . ? H16B C16R H16C 109.5 . . ? C19R C17R C18R 117.4(19) . . ? C19R C17R C3R 116.7(18) . . ? C18R C17R C3R 114.2(17) . . ? C19R C17R H17R 101.5 . . ? C18R C17R H17R 101.5 . . ? C3R C17R H17R 101.5 . . ? C17R C18R H18A 109.5 . . ? C17R C18R H18B 109.5 . . ? H18A C18R H18B 109.5 . . ? C17R C18R H18C 109.5 . . ? H18A C18R H18C 109.5 . . ? H18B C18R H18C 109.5 . . ? C17R C19R H19A 109.5 . . ? C17R C19R H19B 109.5 . . ? H19A C19R H19B 109.5 . . ? C17R C19R H19C 109.5 . . ? H19A C19R H19C 109.5 . . ? H19B C19R H19C 109.5 . . ? C21R C20R C22R 111.5(17) . . ? C21R C20R C5R 112.4(17) . . ? C22R C20R C5R 111.3(17) . . ? C21R C20R H20R 107.1 . . ? C22R C20R H20R 107.1 . . ? C5R C20R H20R 107.1 . . ? C20R C21R H21A 109.5 . . ? C20R C21R H21B 109.5 . . ? H21A C21R H21B 109.5 . . ? C20R C21R H21C 109.5 . . ? H21A C21R H21C 109.5 . . ? H21B C21R H21C 109.5 . . ? C20R C22R H22A 109.5 . . ? C20R C22R H22B 109.5 . . ? H22A C22R H22B 109.5 . . ? C20R C22R H22C 109.5 . . ? H22A C22R H22C 109.5 . . ? H22B C22R H22C 109.5 . . ? O2R C23R N1R 121(2) . . ? O2R C23R C11R 119(2) . . ? N1R C23R C11R 115.8(18) . . ? N1R C24R C25R 113.8(17) . . ? N1R C24R C27R 112.3(17) . . ? C25R C24R C27R 112.9(16) . . ? N1R C24R H24R 105.7 . . ? C25R C24R H24R 105.7 . . ? C27R C24R H24R 105.7 . . ? O3R C25R O4R 121.2(19) . . ? O3R C25R C24R 123.7(18) . . ? O4R C25R C24R 113.9(16) . . ? C28R C27R C24R 111.1(16) . . ? C28R C27R H27A 109.4 . . ? C24R C27R H27A 109.4 . . ? C28R C27R H27B 109.4 . . ? C24R C27R H27B 109.4 . . ? H27A C27R H27B 108.0 . . ? C29R C28R C33R 117.2 . . ? C29R C28R C27R 120.6(13) . . ? C33R C28R C27R 122.2(13) . . ? C30R C29R C28R 121.3 . . ? C29R C30R C31R 121.0 . . ? C32R C31R C30R 118.1 . . ? C31R C32R C33R 121.2 . . ? C32R C33R C28R 121.2 . . ? C23P N1P C24P 124.3(6) . . ? C23P N1P H1P 117.8 . . ? C24P N1P H1P 117.8 . . ? C25P O4P C26P 118.8(7) . . ? C6P C1P C2P 122.5(5) . . ? C6P C1P C14P 94.2(5) . . ? C2P C1P C14P 143.3(6) . . ? C1P C2P C3P 116.1(6) . . ? C1P C2P H2P 121.9 . . ? C3P C2P H2P 121.9 . . ? C4P C3P C2P 120.7(6) . . ? C4P C3P C17P 120.4(6) . . ? C2P C3P C17P 118.9(6) . . ? C3P C4P C5P 123.4(6) . . ? C3P C4P H4P 118.3 . . ? C5P C4P H4P 118.3 . . ? C6P C5P C4P 113.5(6) . . ? C6P C5P C20P 123.9(6) . . ? C4P C5P C20P 122.5(6) . . ? C1P C6P C5P 123.8(5) . . ? C1P C6P C7P 96.6(5) . . ? C5P C6P C7P 139.5(7) . . ? O1P C7P C8P 111.5(4) . . ? O1P C7P C6P 114.7(5) . . ? C8P C7P C6P 114.3(5) . . ? O1P C7P C14P 113.5(5) . . ? C8P C7P C14P 116.6(4) . . ? C6P C7P C14P 83.8(4) . . ? C9P C8P C13P 117.0(5) . . ? C9P C8P C7P 120.8(4) . . ? C13P C8P C7P 122.2(4) . . ? C8P C9P C10P 121.2(5) . . ? C8P C9P H9P 119.4 . . ? C10P C9P H9P 119.4 . . ? C11P C10P C9P 121.7(6) . . ? C11P C10P H10P 119.2 . . ? C9P C10P H10P 119.2 . . ? C10P C11P C12P 117.7(5) . . ? C10P C11P C23P 123.9(5) . . ? C12P C11P C23P 118.4(5) . . ? C13P C12P C11P 120.7(5) . . ? C13P C12P H12P 119.6 . . ? C11P C12P H12P 119.6 . . ? C12P C13P C8P 121.7(5) . . ? C12P C13P H13P 119.2 . . ? C8P C13P H13P 119.2 . . ? C16P C14P C15P 109.7(6) . . ? C16P C14P C1P 115.7(6) . . ? C15P C14P C1P 113.8(5) . . ? C16P C14P C7P 119.7(5) . . ? C15P C14P C7P 110.8(5) . . ? C1P C14P C7P 85.2(4) . . ? C14P C15P H15D 109.5 . . ? C14P C15P H15E 109.5 . . ? H15D C15P H15E 109.5 . . ? C14P C15P H15F 109.5 . . ? H15D C15P H15F 109.5 . . ? H15E C15P H15F 109.5 . . ? C14P C16P H16D 109.5 . . ? C14P C16P H16E 109.5 . . ? H16D C16P H16E 109.5 . . ? C14P C16P H16F 109.5 . . ? H16D C16P H16F 109.5 . . ? H16E C16P H16F 109.5 . . ? C19P C17P C18P 113.2(9) . . ? C19P C17P C3P 111.5(7) . . ? C18P C17P C3P 111.6(7) . . ? C19P C17P H17P 106.7 . . ? C18P C17P H17P 106.7 . . ? C3P C17P H17P 106.7 . . ? C17P C18P H18D 109.5 . . ? C17P C18P H18E 109.5 . . ? H18D C18P H18E 109.5 . . ? C17P C18P H18F 109.5 . . ? H18D C18P H18F 109.5 . . ? H18E C18P H18F 109.5 . . ? C17P C19P H19D 109.5 . . ? C17P C19P H19E 109.5 . . ? H19D C19P H19E 109.5 . . ? C17P C19P H19F 109.5 . . ? H19D C19P H19F 109.5 . . ? H19E C19P H19F 109.5 . . ? C22P C20P C5P 111.8(7) . . ? C22P C20P C21P 110.5(8) . . ? C5P C20P C21P 110.9(7) . . ? C22P C20P H20P 107.8 . . ? C5P C20P H20P 107.8 . . ? C21P C20P H20P 107.8 . . ? C20P C21P H21D 109.5 . . ? C20P C21P H21E 109.5 . . ? H21D C21P H21E 109.5 . . ? C20P C21P H21F 109.5 . . ? H21D C21P H21F 109.5 . . ? H21E C21P H21F 109.5 . . ? C20P C22P H22D 109.5 . . ? C20P C22P H22E 109.5 . . ? H22D C22P H22E 109.5 . . ? C20P C22P H22F 109.5 . . ? H22D C22P H22F 109.5 . . ? H22E C22P H22F 109.5 . . ? O2P C23P N1P 120.7(6) . . ? O2P C23P C11P 122.8(6) . . ? N1P C23P C11P 116.4(5) . . ? N1P C24P C25P 113.4(6) . . ? N1P C24P C27P 111.2(6) . . ? C25P C24P C27P 109.5(6) . . ? N1P C24P H24P 107.5 . . ? C25P C24P H24P 107.5 . . ? C27P C24P H24P 107.5 . . ? O3P C25P O4P 124.1(7) . . ? O3P C25P C24P 122.0(7) . . ? O4P C25P C24P 113.9(6) . . ? O4P C26P H26D 109.5 . . ? O4P C26P H26E 109.5 . . ? H26D C26P H26E 109.5 . . ? O4P C26P H26F 109.5 . . ? H26D C26P H26F 109.5 . . ? H26E C26P H26F 109.5 . . ? C28P C27P C24P 114.1(5) . . ? C28P C27P H27C 108.7 . . ? C24P C27P H27C 108.7 . . ? C28P C27P H27D 108.7 . . ? C24P C27P H27D 108.7 . . ? H27C C27P H27D 107.6 . . ? C29P C28P C33P 118.1 . . ? C29P C28P C27P 121.8(4) . . ? C33P C28P C27P 120.2(4) . . ? C28P C29P C30P 120.7 . . ? C28P C29P H29P 119.7 . . ? C30P C29P H29P 119.7 . . ? C31P C30P C29P 121.2 . . ? C31P C30P H30P 119.4 . . ? C29P C30P H30P 119.4 . . ? C32P C31P C30P 118.1 . . ? C32P C31P H31P 120.9 . . ? C30P C31P H31P 120.9 . . ? C31P C32P C33P 120.9 . . ? C31P C32P H32P 119.6 . . ? C33P C32P H32P 119.6 . . ? C32P C33P C28P 121.0 . . ? C32P C33P H33P 119.5 . . ? C28P C33P H33P 119.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.174 _refine_diff_density_min -0.196 _refine_diff_density_rms 0.034 #===END data_87.9%P _database_code_depnum_ccdc_archive 'CCDC 799262' #TrackingRef '- 1.cif' #==================================================================== # start Validation Reply Form _vrf_PLAT201_87.9%P ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 18 RESPONSE: In the crystal there are reactant and photoproduct molecules. Part of atoms were refined isotropically in order to decrease a large number of the parameters in the refinement. ; # end Validation Reply Form #==================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 N O4' _chemical_formula_weight 513.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.2515(16) _cell_length_b 11.479(2) _cell_length_c 28.054(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2979.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 13.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14549 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 4.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2953 _reflns_number_gt 2009 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSALIS (Oxford Diffraction, 2003)' _computing_cell_refinement 'CRYSALIS (Oxford Diffraction, 2003)' _computing_data_reduction 'CRYSALIS (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Owing to a reactant-product disorder, the following weak restraints from SHELXL97 were applied: DFIX, DANG and SIMU. DFIX and DANG restrained bond lengths and valence angles to target values. The target values were taken from the structures of the pure reactant and the pure product of crystal 1a. SIMU restrained displacement parameters of atoms of the products. ; _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^)+(0.1267P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration syn _refine_ls_number_reflns 2953 _refine_ls_number_parameters 384 _refine_ls_number_restraints 303 _refine_ls_R_factor_all 0.1085 _refine_ls_R_factor_gt 0.0747 _refine_ls_wR_factor_ref 0.2239 _refine_ls_wR_factor_gt 0.1956 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.232 _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 N1R N 0.727(6) 0.282(3) -0.0013(17) 0.083(12) Uiso 0.121(8) 1 d PDU A 1 H1R H 0.6368 0.2641 0.0004 0.100 Uiso 0.121(8) 1 calc PR A 1 O1R O 0.505(6) -0.243(7) 0.099(3) 0.082(11) Uiso 0.121(8) 1 d PDU A 1 O2R O 0.932(8) 0.264(6) 0.040(3) 0.060(16) Uiso 0.121(8) 1 d PDU A 1 O3R O 0.754(6) 0.583(3) -0.021(2) 0.12(2) Uiso 0.121(8) 1 d PD A 1 O4R O 0.576(9) 0.474(5) 0.004(5) 0.097(11) Uiso 0.121(8) 1 d PDU A 1 C1R C 0.624(4) -0.222(3) 0.1943(9) 0.063(9) Uiso 0.121(8) 1 d PDU A 1 C2R C 0.682(3) -0.268(3) 0.2357(9) 0.059(8) Uiso 0.121(8) 1 d PDU A 1 H2R H 0.6290 -0.2610 0.2638 0.071 Uiso 0.121(8) 1 calc PR A 1 C3R C 0.813(4) -0.322(4) 0.2368(10) 0.073(10) Uiso 0.121(8) 1 d PDU A 1 C4R C 0.896(4) -0.322(5) 0.1963(11) 0.083(17) Uiso 0.121(8) 1 d PDU A 1 H4R H 0.9932 -0.3429 0.1983 0.100 Uiso 0.121(8) 1 calc PR A 1 C5R C 0.838(4) -0.290(4) 0.1514(10) 0.065(16) Uiso 0.121(8) 1 d PDU A 1 C6R C 0.702(4) -0.241(4) 0.1523(9) 0.07(2) Uiso 0.121(8) 1 d PDU A 1 C7R C 0.629(4) -0.209(3) 0.1063(10) 0.077(6) Uiso 0.121(8) 1 d PDU A 1 C8R C 0.683(4) -0.102(3) 0.0831(11) 0.072(9) Uiso 0.121(8) 1 d PDU A 1 C9R C 0.624(4) -0.065(3) 0.0403(10) 0.053(13) Uiso 0.121(8) 1 d PD A 1 H9R H 0.5539 -0.1098 0.0253 0.064 Uiso 0.121(8) 1 calc PR A 1 C10R C 0.669(4) 0.038(3) 0.0199(12) 0.054(19) Uiso 0.121(8) 1 d PD A 1 H10R H 0.6322 0.0602 -0.0095 0.064 Uiso 0.121(8) 1 calc PR A 1 C11R C 0.769(5) 0.107(3) 0.0428(15) 0.061(17) Uiso 0.121(8) 1 d PDU A 1 C12R C 0.834(4) 0.066(3) 0.0842(12) 0.047(8) Uiso 0.121(8) 1 d PDU A 1 H12R H 0.9079 0.1084 0.0983 0.057 Uiso 0.121(8) 1 calc PR A 1 C13R C 0.791(4) -0.036(3) 0.1044(12) 0.062(11) Uiso 0.121(8) 1 d PDU A 1 H13R H 0.8341 -0.0621 0.1325 0.074 Uiso 0.121(8) 1 calc PR A 1 C14R C 0.506(4) -0.133(4) 0.1974(14) 0.088(12) Uiso 0.121(8) 1 d PDU A 1 H14R H 0.4723 -0.1178 0.1649 0.106 Uiso 0.121(8) 1 calc PR A 1 C15R C 0.380(4) -0.182(5) 0.225(3) 0.125(18) Uiso 0.121(8) 1 d PDU A 1 H15A H 0.3014 -0.1280 0.2244 0.188 Uiso 0.121(8) 1 calc PR A 1 H15B H 0.4090 -0.1959 0.2574 0.188 Uiso 0.121(8) 1 calc PR A 1 H15C H 0.3502 -0.2545 0.2108 0.188 Uiso 0.121(8) 1 calc PR A 1 C16R C 0.556(7) -0.018(4) 0.218(3) 0.14(2) Uiso 0.121(8) 1 d PDU A 1 H16A H 0.4759 0.0346 0.2205 0.214 Uiso 0.121(8) 1 calc PR A 1 H16B H 0.6294 0.0152 0.1982 0.214 Uiso 0.121(8) 1 calc PR A 1 H16C H 0.5956 -0.0309 0.2496 0.214 Uiso 0.121(8) 1 calc PR A 1 C17R C 0.878(5) -0.351(5) 0.2842(12) 0.102(12) Uiso 0.121(8) 1 d PDU A 1 H17R H 0.7971 -0.3352 0.3057 0.122 Uiso 0.121(8) 1 calc PR A 1 C18R C 0.987(8) -0.264(7) 0.301(3) 0.15(2) Uiso 0.121(8) 1 d PDU A 1 H18A H 0.9639 -0.1886 0.2888 0.221 Uiso 0.121(8) 1 calc PR A 1 H18B H 1.0816 -0.2868 0.2906 0.221 Uiso 0.121(8) 1 calc PR A 1 H18C H 0.9856 -0.2614 0.3355 0.221 Uiso 0.121(8) 1 calc PR A 1 C19R C 0.907(12) -0.472(6) 0.294(3) 0.13(2) Uiso 0.121(8) 1 d PDU A 1 H19A H 0.8290 -0.5184 0.2820 0.189 Uiso 0.121(8) 1 calc PR A 1 H19B H 0.9156 -0.4829 0.3278 0.189 Uiso 0.121(8) 1 calc PR A 1 H19C H 0.9955 -0.4944 0.2788 0.189 Uiso 0.121(8) 1 calc PR A 1 C20R C 0.893(5) -0.350(4) 0.1065(12) 0.076(11) Uiso 0.121(8) 1 d PDU A 1 H20R H 0.8398 -0.3172 0.0795 0.091 Uiso 0.121(8) 1 calc PR A 1 C21R C 0.863(10) -0.479(5) 0.107(3) 0.13(2) Uiso 0.121(8) 1 d PDU A 1 H21A H 0.8963 -0.5130 0.0777 0.191 Uiso 0.121(8) 1 calc PR A 1 H21B H 0.7605 -0.4916 0.1099 0.191 Uiso 0.121(8) 1 calc PR A 1 H21C H 0.9118 -0.5143 0.1333 0.191 Uiso 0.121(8) 1 calc PR A 1 C22R C 1.052(6) -0.326(8) 0.098(3) 0.12(2) Uiso 0.121(8) 1 d PDU A 1 H22A H 1.0695 -0.2438 0.1004 0.177 Uiso 0.121(8) 1 calc PR A 1 H22B H 1.0785 -0.3524 0.0667 0.177 Uiso 0.121(8) 1 calc PR A 1 H22C H 1.1088 -0.3663 0.1214 0.177 Uiso 0.121(8) 1 calc PR A 1 C23R C 0.823(7) 0.220(4) 0.024(2) 0.065(12) Uiso 0.121(8) 1 d PDU A 1 C24R C 0.772(6) 0.378(2) -0.0310(12) 0.065(11) Uiso 0.121(8) 1 d PDU A 1 H24R H 0.8760 0.3884 -0.0264 0.078 Uiso 0.121(8) 1 calc PR A 1 C25R C 0.699(6) 0.490(3) -0.0166(19) 0.084(12) Uiso 0.121(8) 1 d PDU A 1 C26R C 0.495(12) 0.573(8) 0.019(6) 0.10(2) Uiso 0.121(8) 1 d PDU A 1 H26A H 0.4921 0.6296 -0.0059 0.157 Uiso 0.121(8) 1 calc PR A 1 H26B H 0.5395 0.6071 0.0470 0.157 Uiso 0.121(8) 1 calc PR A 1 H26C H 0.3980 0.5497 0.0271 0.157 Uiso 0.121(8) 1 calc PR A 1 C27R C 0.747(6) 0.352(3) -0.0836(13) 0.063(19) Uiso 0.121(8) 1 d PD A 1 H27A H 0.6444 0.3415 -0.0893 0.075 Uiso 0.121(8) 1 calc PR A 1 H27B H 0.7797 0.4175 -0.1026 0.075 Uiso 0.121(8) 1 calc PR A 1 C28R C 0.826(4) 0.245(3) -0.0986(14) 0.073(13) Uiso 0.121(8) 1 d PGDU A 1 C29R C 0.754(3) 0.140(3) -0.1025(15) 0.088(13) Uiso 0.121(8) 1 d PGDU A 1 H29R H 0.6559 0.1372 -0.0959 0.105 Uiso 0.121(8) 1 d PG A 1 C30R C 0.825(4) 0.041(2) -0.1158(15) 0.093(17) Uiso 0.121(8) 1 d PG A 1 H30R H 0.7744 -0.0289 -0.1179 0.111 Uiso 0.121(8) 1 d PG A 1 C31R C 0.971(4) 0.042(3) -0.1261(16) 0.075(12) Uiso 0.121(8) 1 d PGU A 1 H31R H 1.0193 -0.0255 -0.1346 0.090 Uiso 0.121(8) 1 d PG A 1 C32R C 1.042(3) 0.146(3) -0.1236(17) 0.084(16) Uiso 0.121(8) 1 d PG A 1 H32R H 1.1394 0.1494 -0.1312 0.101 Uiso 0.121(8) 1 d PG A 1 C33R C 0.971(4) 0.246(3) -0.1099(16) 0.093(16) Uiso 0.121(8) 1 d PGDU A 1 H33R H 1.0225 0.3157 -0.1083 0.112 Uiso 0.121(8) 1 d PG A 1 N1P N 0.7368(7) 0.2700(6) -0.0132(2) 0.0719(19) Uani 0.879(8) 1 d PDU A 2 H1P H 0.6535 0.2388 -0.0179 0.086 Uiso 0.879(8) 1 calc PR A 2 O1P O 0.4977(11) -0.2355(10) 0.0975(4) 0.089(2) Uani 0.879(8) 1 d PDU A 2 O2P O 0.9368(10) 0.2704(9) 0.0315(4) 0.073(3) Uani 0.879(8) 1 d PDU A 2 O3P O 0.7453(8) 0.5706(6) -0.0484(3) 0.116(2) Uani 0.879(8) 1 d PD A 2 O4P O 0.6020(13) 0.4685(7) -0.0001(6) 0.100(2) Uani 0.879(8) 1 d PDU A 2 C1P C 0.6532(7) -0.2065(6) 0.1982(2) 0.074(2) Uiso 0.879(8) 1 d PDU A 2 C2P C 0.7226(8) -0.2403(6) 0.2392(2) 0.082(2) Uiso 0.879(8) 1 d PDU A 2 H2P H 0.6895 -0.2187 0.2692 0.099 Uiso 0.879(8) 1 calc PR A 2 C3P C 0.8451(8) -0.3088(7) 0.2332(2) 0.088(2) Uiso 0.879(8) 1 d PDU A 2 C4P C 0.8917(9) -0.3406(8) 0.1884(2) 0.084(3) Uiso 0.879(8) 1 d PDU A 2 H4P H 0.9730 -0.3879 0.1859 0.101 Uiso 0.879(8) 1 calc PR A 2 C5P C 0.8224(8) -0.3049(8) 0.1462(2) 0.078(3) Uiso 0.879(8) 1 d PDU A 2 C6P C 0.7012(7) -0.2369(7) 0.1543(2) 0.071(3) Uiso 0.879(8) 1 d PDU A 2 C7P C 0.5888(6) -0.1673(5) 0.12651(19) 0.0634(17) Uani 0.879(8) 1 d PDU A 2 C8P C 0.6517(6) -0.0658(5) 0.0986(2) 0.0547(15) Uiso 0.879(8) 1 d PDU A 2 C9P C 0.6030(7) -0.0405(6) 0.0540(2) 0.0632(19) Uiso 0.879(8) 1 d PD A 2 H9P H 0.5313 -0.0868 0.0406 0.076 Uiso 0.879(8) 1 calc PR A 2 C10P C 0.6573(8) 0.0519(7) 0.0283(3) 0.069(3) Uiso 0.879(8) 1 d PD A 2 H10P H 0.6218 0.0663 -0.0021 0.083 Uiso 0.879(8) 1 calc PR A 2 C11P C 0.7624(8) 0.1232(6) 0.0466(2) 0.057(2) Uiso 0.879(8) 1 d PDU A 2 C12P C 0.8142(7) 0.0962(6) 0.0913(2) 0.0604(19) Uiso 0.879(8) 1 d PDU A 2 H12P H 0.8861 0.1424 0.1047 0.073 Uiso 0.879(8) 1 calc PR A 2 C13P C 0.7626(7) 0.0036(6) 0.1164(2) 0.0635(17) Uiso 0.879(8) 1 d PDU A 2 H13P H 0.8024 -0.0137 0.1460 0.076 Uiso 0.879(8) 1 calc PR A 2 C14P C 0.5242(6) -0.1375(5) 0.1793(2) 0.0740(19) Uani 0.879(8) 1 d PDU A 2 C15P C 0.3790(7) -0.1989(7) 0.1870(3) 0.098(3) Uani 0.879(8) 1 d PDU A 2 H15D H 0.3876 -0.2793 0.1780 0.147 Uiso 0.879(8) 1 calc PR A 2 H15E H 0.3063 -0.1620 0.1678 0.147 Uiso 0.879(8) 1 calc PR A 2 H15F H 0.3524 -0.1938 0.2200 0.147 Uiso 0.879(8) 1 calc PR A 2 C16P C 0.5145(9) -0.0135(5) 0.1952(3) 0.086(2) Uani 0.879(8) 1 d PDU A 2 H16D H 0.4307 0.0222 0.1813 0.129 Uiso 0.879(8) 1 calc PR A 2 H16E H 0.5996 0.0277 0.1852 0.129 Uiso 0.879(8) 1 calc PR A 2 H16F H 0.5071 -0.0107 0.2293 0.129 Uiso 0.879(8) 1 calc PR A 2 C17P C 0.9291(10) -0.3496(8) 0.2778(3) 0.113(3) Uani 0.879(8) 1 d PDU A 2 H17P H 0.8728 -0.3245 0.3056 0.135 Uiso 0.879(8) 1 calc PR A 2 C18P C 1.0712(13) -0.2918(12) 0.2814(4) 0.168(6) Uani 0.879(8) 1 d PDU A 2 H18D H 1.0587 -0.2090 0.2792 0.252 Uiso 0.879(8) 1 calc PR A 2 H18E H 1.1323 -0.3180 0.2559 0.252 Uiso 0.879(8) 1 calc PR A 2 H18F H 1.1151 -0.3110 0.3114 0.252 Uiso 0.879(8) 1 calc PR A 2 C19P C 0.9381(16) -0.4766(9) 0.2801(5) 0.153(6) Uani 0.879(8) 1 d PDU A 2 H19D H 0.8428 -0.5092 0.2776 0.229 Uiso 0.879(8) 1 calc PR A 2 H19E H 0.9804 -0.4994 0.3100 0.229 Uiso 0.879(8) 1 calc PR A 2 H19F H 0.9969 -0.5047 0.2544 0.229 Uiso 0.879(8) 1 calc PR A 2 C20P C 0.8818(10) -0.3311(8) 0.0973(3) 0.089(3) Uani 0.879(8) 1 d PDU A 2 H20P H 0.8201 -0.2916 0.0740 0.107 Uiso 0.879(8) 1 calc PR A 2 C21P C 0.8773(14) -0.4600(8) 0.0867(4) 0.121(4) Uani 0.879(8) 1 d PDU A 2 H21D H 0.9137 -0.4737 0.0551 0.182 Uiso 0.879(8) 1 calc PR A 2 H21E H 0.7794 -0.4872 0.0887 0.182 Uiso 0.879(8) 1 calc PR A 2 H21F H 0.9359 -0.5010 0.1094 0.182 Uiso 0.879(8) 1 calc PR A 2 C22P C 1.0329(12) -0.2851(12) 0.0912(5) 0.139(5) Uani 0.879(8) 1 d PDU A 2 H22D H 1.0667 -0.3028 0.0597 0.208 Uiso 0.879(8) 1 calc PR A 2 H22E H 1.0955 -0.3209 0.1143 0.208 Uiso 0.879(8) 1 calc PR A 2 H22F H 1.0331 -0.2022 0.0958 0.208 Uiso 0.879(8) 1 calc PR A 2 C23P C 0.8196(9) 0.2272(7) 0.0216(3) 0.060(2) Uani 0.879(8) 1 d PDU A 2 C24P C 0.7791(8) 0.3651(6) -0.0433(2) 0.072(2) Uani 0.879(8) 1 d PDU A 2 H24P H 0.8837 0.3753 -0.0396 0.087 Uiso 0.879(8) 1 calc PR A 2 C25P C 0.7089(9) 0.4786(6) -0.0305(3) 0.085(2) Uani 0.879(8) 1 d PDU A 2 C26P C 0.524(2) 0.5725(12) 0.0129(9) 0.128(4) Uani 0.879(8) 1 d PDU A 2 H26D H 0.4665 0.5575 0.0408 0.192 Uiso 0.879(8) 1 calc PR A 2 H26E H 0.4620 0.5953 -0.0129 0.192 Uiso 0.879(8) 1 calc PR A 2 H26F H 0.5912 0.6341 0.0196 0.192 Uiso 0.879(8) 1 calc PR A 2 C27P C 0.7503(10) 0.3371(7) -0.0957(3) 0.081(3) Uani 0.879(8) 1 d PD A 2 H27C H 0.6480 0.3218 -0.0998 0.098 Uiso 0.879(8) 1 calc PR A 2 H27D H 0.7744 0.4048 -0.1148 0.098 Uiso 0.879(8) 1 calc PR A 2 C28P C 0.8321(6) 0.2370(4) -0.1135(2) 0.073(2) Uiso 0.879(8) 1 d PGDU A 2 C29P C 0.7655(5) 0.1327(5) -0.1223(3) 0.105(3) Uiso 0.879(8) 1 d PGDU A 2 H29P H 0.6669 0.1250 -0.1167 0.126 Uiso 0.879(8) 1 d PG A 2 C30P C 0.8429(7) 0.0393(4) -0.1394(3) 0.129(3) Uiso 0.879(8) 1 d PG A 2 H30P H 0.7963 -0.0316 -0.1442 0.155 Uiso 0.879(8) 1 d PG A 2 C31P C 0.9871(7) 0.0487(5) -0.1496(3) 0.118(3) Uiso 0.879(8) 1 d PGU A 2 H31P H 1.0385 -0.0142 -0.1618 0.141 Uiso 0.879(8) 1 d PG A 2 C32P C 1.0535(5) 0.1532(6) -0.1414(3) 0.109(3) Uiso 0.879(8) 1 d PG A 2 H32P H 1.1513 0.1617 -0.1482 0.131 Uiso 0.879(8) 1 d PG A 2 C33P C 0.9775(6) 0.2460(4) -0.1232(2) 0.084(2) Uiso 0.879(8) 1 d PGDU A 2 H33P H 1.0250 0.3160 -0.1174 0.101 Uiso 0.879(8) 1 d PG 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 N1P 0.057(3) 0.089(4) 0.070(4) 0.024(3) 0.003(3) -0.007(3) O1P 0.094(4) 0.077(4) 0.096(4) -0.006(3) -0.012(3) -0.020(3) O2P 0.055(3) 0.084(4) 0.078(6) 0.016(3) -0.005(3) -0.004(2) O3P 0.119(5) 0.083(4) 0.147(7) 0.033(4) 0.017(5) 0.022(4) O4P 0.108(6) 0.094(4) 0.097(5) -0.014(3) 0.022(4) 0.007(4) C7P 0.061(3) 0.055(3) 0.074(4) -0.003(3) 0.008(3) 0.005(3) C14P 0.072(4) 0.076(5) 0.073(4) 0.005(4) 0.019(3) 0.009(4) C15P 0.085(5) 0.091(5) 0.117(7) 0.004(5) 0.037(5) -0.007(4) C16P 0.094(5) 0.079(5) 0.085(5) 0.001(4) 0.003(4) 0.006(4) C17P 0.132(8) 0.126(7) 0.080(5) 0.045(5) 0.004(5) 0.028(7) C18P 0.177(11) 0.196(12) 0.131(9) 0.082(9) -0.066(9) -0.064(10) C19P 0.142(11) 0.143(9) 0.173(13) 0.088(9) -0.051(11) -0.009(8) C20P 0.091(5) 0.108(6) 0.069(5) 0.006(4) 0.005(4) 0.031(5) C21P 0.134(8) 0.111(8) 0.119(8) -0.018(6) 0.023(7) 0.019(7) C22P 0.137(9) 0.160(12) 0.119(8) 0.013(8) 0.048(8) -0.021(9) C23P 0.050(3) 0.076(4) 0.055(4) 0.007(3) 0.001(3) 0.021(3) C24P 0.060(4) 0.083(5) 0.073(5) 0.016(4) 0.000(4) 0.001(3) C25P 0.079(5) 0.093(6) 0.084(6) 0.015(5) -0.001(4) 0.006(4) C26P 0.140(12) 0.104(7) 0.139(11) -0.022(7) 0.029(9) 0.020(7) C27P 0.081(5) 0.099(6) 0.064(5) 0.028(4) -0.007(4) -0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1R C23R 1.336(11) . ? N1R C24R 1.445(11) . ? N1R H1R 0.8600 . ? O1R C7R 1.227(11) . ? O2R C23R 1.225(11) . ? O3R C25R 1.191(11) . ? O4R C25R 1.289(11) . ? O4R C26R 1.433(11) . ? C1R C2R 1.381(10) . ? C1R C6R 1.396(10) . ? C1R C14R 1.496(10) . ? C2R C3R 1.371(10) . ? C2R H2R 0.9300 . ? C3R C4R 1.373(10) . ? C3R C17R 1.496(10) . ? C4R C5R 1.418(10) . ? C4R H4R 0.9300 . ? C5R C6R 1.383(10) . ? C5R C20R 1.523(11) . ? C6R C7R 1.505(10) . ? C7R C8R 1.477(10) . ? C8R C9R 1.385(10) . ? C8R C13R 1.386(10) . ? C9R C10R 1.373(10) . ? C9R H9R 0.9300 . ? C10R C11R 1.379(10) . ? C10R H10R 0.9300 . ? C11R C12R 1.391(10) . ? C11R C23R 1.483(10) . ? C12R C13R 1.360(10) . ? C12R H12R 0.9300 . ? C13R H13R 0.9300 . ? C14R C15R 1.507(11) . ? C14R C16R 1.520(11) . ? C14R H14R 0.9800 . ? C15R H15A 0.9600 . ? C15R H15B 0.9600 . ? C15R H15C 0.9600 . ? C16R H16A 0.9600 . ? C16R H16B 0.9600 . ? C16R H16C 0.9600 . ? C17R C19R 1.440(11) . ? C17R C18R 1.493(11) . ? C17R H17R 0.9800 . ? C18R H18A 0.9600 . ? C18R H18B 0.9600 . ? C18R H18C 0.9600 . ? C19R H19A 0.9600 . ? C19R H19B 0.9600 . ? C19R H19C 0.9600 . ? C20R C21R 1.501(11) . ? C20R C22R 1.517(11) . ? C20R H20R 0.9800 . ? C21R H21A 0.9600 . ? C21R H21B 0.9600 . ? C21R H21C 0.9600 . ? C22R H22A 0.9600 . ? C22R H22B 0.9600 . ? C22R H22C 0.9600 . ? C24R C25R 1.511(11) . ? C24R C27R 1.523(11) . ? C24R H24R 0.9800 . ? C26R H26A 0.9600 . ? C26R H26B 0.9600 . ? C26R H26C 0.9600 . ? C27R C28R 1.488(10) . ? C27R H27A 0.9700 . ? C27R H27B 0.9700 . ? C28R C29R 1.3754 . ? C28R C33R 1.3831 . ? C29R C30R 1.3701 . ? C29R H29R 0.9300 . ? C30R C31R 1.3771 . ? C30R H30R 0.9300 . ? C31R C32R 1.3617 . ? C31R H31R 0.9300 . ? C32R C33R 1.3726 . ? C32R H32R 0.9300 . ? C33R H33R 0.9300 . ? N1P C23P 1.336(6) . ? N1P C24P 1.435(6) . ? N1P H1P 0.8600 . ? O1P C7P 1.409(8) . ? O2P C23P 1.224(6) . ? O3P C25P 1.217(7) . ? O4P C25P 1.311(7) . ? O4P C26P 1.443(8) . ? C1P C6P 1.355(7) . ? C1P C2P 1.374(7) . ? C1P C14P 1.527(7) . ? C2P C3P 1.389(7) . ? C2P H2P 0.9300 . ? C3P C4P 1.380(8) . ? C3P C17P 1.545(7) . ? C4P C5P 1.405(7) . ? C4P H4P 0.9300 . ? C5P C6P 1.385(7) . ? C5P C20P 1.508(7) . ? C6P C7P 1.525(7) . ? C7P C8P 1.519(6) . ? C7P C14P 1.634(7) . ? C8P C9P 1.361(6) . ? C8P C13P 1.391(6) . ? C9P C10P 1.378(7) . ? C9P H9P 0.9300 . ? C10P C11P 1.370(7) . ? C10P H10P 0.9300 . ? C11P C12P 1.378(6) . ? C11P C23P 1.482(6) . ? C12P C13P 1.361(7) . ? C12P H12P 0.9300 . ? C13P H13P 0.9300 . ? C14P C16P 1.494(7) . ? C14P C15P 1.531(7) . ? C15P H15D 0.9600 . ? C15P H15E 0.9600 . ? C15P H15F 0.9600 . ? C16P H16D 0.9600 . ? C16P H16E 0.9600 . ? C16P H16F 0.9600 . ? C17P C19P 1.463(9) . ? C17P C18P 1.476(9) . ? C17P H17P 0.9800 . ? C18P H18D 0.9600 . ? C18P H18E 0.9600 . ? C18P H18F 0.9600 . ? C19P H19D 0.9600 . ? C19P H19E 0.9600 . ? C19P H19F 0.9600 . ? C20P C22P 1.504(8) . ? C20P C21P 1.511(8) . ? C20P H20P 0.9800 . ? C21P H21D 0.9600 . ? C21P H21E 0.9600 . ? C21P H21F 0.9600 . ? C22P H22D 0.9600 . ? C22P H22E 0.9600 . ? C22P H22F 0.9600 . ? C24P C25P 1.500(7) . ? C24P C27P 1.527(8) . ? C24P H24P 0.9800 . ? C26P H26D 0.9600 . ? C26P H26E 0.9600 . ? C26P H26F 0.9600 . ? C27P C28P 1.464(7) . ? C27P H27C 0.9700 . ? C27P H27D 0.9700 . ? C28P C29P 1.3689 . ? C28P C33P 1.3759 . ? C29P C30P 1.3762 . ? C29P H29P 0.9300 . ? C30P C31P 1.3694 . ? C30P H30P 0.9300 . ? C31P C32P 1.3674 . ? C31P H31P 0.9300 . ? C32P C33P 1.3743 . ? C32P H32P 0.9300 . ? C33P H33P 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23R N1R C24R 121(2) . . ? C23R N1R H1R 119.3 . . ? C24R N1R H1R 119.3 . . ? C25R O4R C26R 119(2) . . ? C2R C1R C6R 116.7(12) . . ? C2R C1R C14R 119.3(14) . . ? C6R C1R C14R 122.2(14) . . ? C3R C2R C1R 122.5(13) . . ? C3R C2R H2R 118.8 . . ? C1R C2R H2R 118.8 . . ? C2R C3R C4R 118.4(13) . . ? C2R C3R C17R 118.7(15) . . ? C4R C3R C17R 120.8(15) . . ? C3R C4R C5R 121.7(14) . . ? C3R C4R H4R 119.2 . . ? C5R C4R H4R 119.2 . . ? C6R C5R C4R 115.7(12) . . ? C6R C5R C20R 120.4(17) . . ? C4R C5R C20R 119.4(16) . . ? C5R C6R C1R 123.5(12) . . ? C5R C6R C7R 119.5(14) . . ? C1R C6R C7R 117.0(13) . . ? O1R C7R C8R 120(2) . . ? O1R C7R C6R 119.5(19) . . ? C8R C7R C6R 115.4(16) . . ? C9R C8R C13R 119.4(12) . . ? C9R C8R C7R 120.1(13) . . ? C13R C8R C7R 120.5(13) . . ? C10R C9R C8R 120.3(13) . . ? C10R C9R H9R 119.9 . . ? C8R C9R H9R 119.9 . . ? C9R C10R C11R 120.3(14) . . ? C9R C10R H10R 119.9 . . ? C11R C10R H10R 119.9 . . ? C10R C11R C12R 118.7(12) . . ? C10R C11R C23R 124.0(15) . . ? C12R C11R C23R 117.1(13) . . ? C13R C12R C11R 121.1(13) . . ? C13R C12R H12R 119.5 . . ? C11R C12R H12R 119.5 . . ? C12R C13R C8R 119.9(13) . . ? C12R C13R H13R 120.1 . . ? C8R C13R H13R 120.1 . . ? C1R C14R C15R 109.8(16) . . ? C1R C14R C16R 113.1(17) . . ? C15R C14R C16R 111.4(17) . . ? C1R C14R H14R 107.4 . . ? C15R C14R H14R 107.4 . . ? C16R C14R H14R 107.4 . . ? C14R C15R H15A 109.5 . . ? C14R C15R H15B 109.5 . . ? H15A C15R H15B 109.5 . . ? C14R C15R H15C 109.5 . . ? H15A C15R H15C 109.5 . . ? H15B C15R H15C 109.5 . . ? C14R C16R H16A 109.5 . . ? C14R C16R H16B 109.5 . . ? H16A C16R H16B 109.5 . . ? C14R C16R H16C 109.5 . . ? H16A C16R H16C 109.5 . . ? H16B C16R H16C 109.5 . . ? C19R C17R C18R 117.2(19) . . ? C19R C17R C3R 117.0(18) . . ? C18R C17R C3R 114.3(17) . . ? C19R C17R H17R 101.4 . . ? C18R C17R H17R 101.4 . . ? C3R C17R H17R 101.4 . . ? C17R C18R H18A 109.5 . . ? C17R C18R H18B 109.5 . . ? H18A C18R H18B 109.5 . . ? C17R C18R H18C 109.5 . . ? H18A C18R H18C 109.5 . . ? H18B C18R H18C 109.5 . . ? C17R C19R H19A 109.5 . . ? C17R C19R H19B 109.5 . . ? H19A C19R H19B 109.5 . . ? C17R C19R H19C 109.5 . . ? H19A C19R H19C 109.5 . . ? H19B C19R H19C 109.5 . . ? C21R C20R C22R 111.4(17) . . ? C21R C20R C5R 112.2(17) . . ? C22R C20R C5R 111.7(17) . . ? C21R C20R H20R 107.1 . . ? C22R C20R H20R 107.1 . . ? C5R C20R H20R 107.1 . . ? C20R C21R H21A 109.5 . . ? C20R C21R H21B 109.5 . . ? H21A C21R H21B 109.5 . . ? C20R C21R H21C 109.5 . . ? H21A C21R H21C 109.5 . . ? H21B C21R H21C 109.5 . . ? C20R C22R H22A 109.5 . . ? C20R C22R H22B 109.5 . . ? H22A C22R H22B 109.5 . . ? C20R C22R H22C 109.5 . . ? H22A C22R H22C 109.5 . . ? H22B C22R H22C 109.5 . . ? O2R C23R N1R 122(2) . . ? O2R C23R C11R 119.8(19) . . ? N1R C23R C11R 115.8(18) . . ? N1R C24R C25R 111.6(17) . . ? N1R C24R C27R 111.5(17) . . ? C25R C24R C27R 111.0(17) . . ? N1R C24R H24R 107.5 . . ? C25R C24R H24R 107.5 . . ? C27R C24R H24R 107.5 . . ? O3R C25R O4R 123.6(18) . . ? O3R C25R C24R 123.2(18) . . ? O4R C25R C24R 112.9(16) . . ? C28R C27R C24R 111.2(16) . . ? C28R C27R H27A 109.4 . . ? C24R C27R H27A 109.4 . . ? C28R C27R H27B 109.4 . . ? C24R C27R H27B 109.4 . . ? H27A C27R H27B 108.0 . . ? C29R C28R C33R 117.2 . . ? C29R C28R C27R 120.4(13) . . ? C33R C28R C27R 122.3(13) . . ? C30R C29R C28R 121.3 . . ? C29R C30R C31R 121.0 . . ? C32R C31R C30R 118.1 . . ? C31R C32R C33R 121.2 . . ? C32R C33R C28R 121.2 . . ? C23P N1P C24P 123.6(5) . . ? C23P N1P H1P 118.2 . . ? C24P N1P H1P 118.2 . . ? C25P O4P C26P 117.9(8) . . ? C6P C1P C2P 122.4(5) . . ? C6P C1P C14P 94.3(5) . . ? C2P C1P C14P 143.3(6) . . ? C1P C2P C3P 116.1(6) . . ? C1P C2P H2P 121.9 . . ? C3P C2P H2P 121.9 . . ? C4P C3P C2P 121.0(6) . . ? C4P C3P C17P 120.1(6) . . ? C2P C3P C17P 118.9(6) . . ? C3P C4P C5P 123.2(6) . . ? C3P C4P H4P 118.4 . . ? C5P C4P H4P 118.4 . . ? C6P C5P C4P 113.4(6) . . ? C6P C5P C20P 123.7(6) . . ? C4P C5P C20P 122.7(6) . . ? C1P C6P C5P 124.0(5) . . ? C1P C6P C7P 96.1(5) . . ? C5P C6P C7P 139.8(6) . . ? O1P C7P C8P 111.0(5) . . ? O1P C7P C6P 114.3(6) . . ? C8P C7P C6P 113.8(5) . . ? O1P C7P C14P 114.9(7) . . ? C8P C7P C14P 116.5(5) . . ? C6P C7P C14P 84.0(4) . . ? C9P C8P C13P 116.8(5) . . ? C9P C8P C7P 120.7(5) . . ? C13P C8P C7P 122.5(5) . . ? C8P C9P C10P 121.6(6) . . ? C8P C9P H9P 119.2 . . ? C10P C9P H9P 119.2 . . ? C11P C10P C9P 121.5(6) . . ? C11P C10P H10P 119.2 . . ? C9P C10P H10P 119.2 . . ? C10P C11P C12P 116.9(5) . . ? C10P C11P C23P 123.9(5) . . ? C12P C11P C23P 119.2(5) . . ? C13P C12P C11P 121.6(5) . . ? C13P C12P H12P 119.2 . . ? C11P C12P H12P 119.2 . . ? C12P C13P C8P 121.4(5) . . ? C12P C13P H13P 119.3 . . ? C8P C13P H13P 119.3 . . ? C16P C14P C1P 115.9(6) . . ? C16P C14P C15P 110.1(5) . . ? C1P C14P C15P 113.5(5) . . ? C16P C14P C7P 119.4(5) . . ? C1P C14P C7P 85.4(4) . . ? C15P C14P C7P 110.6(5) . . ? C14P C15P H15D 109.5 . . ? C14P C15P H15E 109.5 . . ? H15D C15P H15E 109.5 . . ? C14P C15P H15F 109.5 . . ? H15D C15P H15F 109.5 . . ? H15E C15P H15F 109.5 . . ? C14P C16P H16D 109.5 . . ? C14P C16P H16E 109.5 . . ? H16D C16P H16E 109.5 . . ? C14P C16P H16F 109.5 . . ? H16D C16P H16F 109.5 . . ? H16E C16P H16F 109.5 . . ? C19P C17P C18P 113.2(9) . . ? C19P C17P C3P 111.5(7) . . ? C18P C17P C3P 111.5(7) . . ? C19P C17P H17P 106.7 . . ? C18P C17P H17P 106.7 . . ? C3P C17P H17P 106.7 . . ? C17P C18P H18D 109.5 . . ? C17P C18P H18E 109.5 . . ? H18D C18P H18E 109.5 . . ? C17P C18P H18F 109.5 . . ? H18D C18P H18F 109.5 . . ? H18E C18P H18F 109.5 . . ? C17P C19P H19D 109.5 . . ? C17P C19P H19E 109.5 . . ? H19D C19P H19E 109.5 . . ? C17P C19P H19F 109.5 . . ? H19D C19P H19F 109.5 . . ? H19E C19P H19F 109.5 . . ? C22P C20P C5P 111.9(7) . . ? C22P C20P C21P 110.3(8) . . ? C5P C20P C21P 111.4(7) . . ? C22P C20P H20P 107.7 . . ? C5P C20P H20P 107.7 . . ? C21P C20P H20P 107.7 . . ? C20P C21P H21D 109.5 . . ? C20P C21P H21E 109.5 . . ? H21D C21P H21E 109.5 . . ? C20P C21P H21F 109.5 . . ? H21D C21P H21F 109.5 . . ? H21E C21P H21F 109.5 . . ? C20P C22P H22D 109.5 . . ? C20P C22P H22E 109.5 . . ? H22D C22P H22E 109.5 . . ? C20P C22P H22F 109.5 . . ? H22D C22P H22F 109.5 . . ? H22E C22P H22F 109.5 . . ? O2P C23P N1P 121.7(6) . . ? O2P C23P C11P 122.4(6) . . ? N1P C23P C11P 116.0(5) . . ? N1P C24P C25P 113.7(6) . . ? N1P C24P C27P 111.0(5) . . ? C25P C24P C27P 109.8(5) . . ? N1P C24P H24P 107.4 . . ? C25P C24P H24P 107.4 . . ? C27P C24P H24P 107.4 . . ? O3P C25P O4P 123.7(7) . . ? O3P C25P C24P 122.3(7) . . ? O4P C25P C24P 114.0(6) . . ? O4P C26P H26D 109.5 . . ? O4P C26P H26E 109.5 . . ? H26D C26P H26E 109.5 . . ? O4P C26P H26F 109.5 . . ? H26D C26P H26F 109.5 . . ? H26E C26P H26F 109.5 . . ? C28P C27P C24P 113.8(5) . . ? C28P C27P H27C 108.8 . . ? C24P C27P H27C 108.8 . . ? C28P C27P H27D 108.8 . . ? C24P C27P H27D 108.8 . . ? H27C C27P H27D 107.7 . . ? C29P C28P C33P 118.0 . . ? C29P C28P C27P 121.0(4) . . ? C33P C28P C27P 120.9(4) . . ? C28P C29P C30P 120.7 . . ? C28P C29P H29P 119.7 . . ? C30P C29P H29P 119.7 . . ? C31P C30P C29P 121.2 . . ? C31P C30P H30P 119.4 . . ? C29P C30P H30P 119.4 . . ? C32P C31P C30P 118.1 . . ? C32P C31P H31P 120.9 . . ? C30P C31P H31P 120.9 . . ? C31P C32P C33P 120.9 . . ? C31P C32P H32P 119.6 . . ? C33P C32P H32P 119.6 . . ? C32P C33P C28P 121.0 . . ? C32P C33P H33P 119.5 . . ? C28P C33P H33P 119.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.192 _refine_diff_density_min -0.194 _refine_diff_density_rms 0.035 #===END data_100%P _database_code_depnum_ccdc_archive 'CCDC 799263' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 N O4' _chemical_formula_weight 513.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.2509(16) _cell_length_b 11.481(2) _cell_length_c 28.074(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2981.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 13.4 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14562 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 4.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2959 _reflns_number_gt 1998 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSALIS (Oxford Diffraction, 2003)' _computing_cell_refinement 'CRYSALIS (Oxford Diffraction, 2003)' _computing_data_reduction 'CRYSALIS (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Owing to a reactant-product disorder, the following weak restraints from SHELXL97 were applied: DFIX, DANG and SIMU. DFIX and DANG restrained bond lengths and valence angles to target values. The target values were taken from the structures of the pure reactant and the pure product of crystal 1a. SIMU restrained displacement parameters of atoms of the products. ; _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^)+(0.0916P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration syn _refine_ls_number_reflns 2959 _refine_ls_number_parameters 352 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.1781 _refine_ls_wR_factor_gt 0.1559 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.134 _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 N1 N 0.7352(5) 0.2714(4) -0.01225(15) 0.0754(12) Uani 1 1 d . . . HN1 H 0.650(6) 0.245(4) -0.0149(16) 0.078(16) Uiso 1 1 d . . . O1 O 0.4993(4) -0.2370(3) 0.09790(13) 0.0885(10) Uani 1 1 d . . . HO1 H 0.409(10) -0.195(8) 0.091(3) 0.19(4) Uiso 1 1 d . . . O2 O 0.9366(3) 0.2699(3) 0.03263(11) 0.0750(9) Uani 1 1 d . . . O3 O 0.7449(5) 0.5712(4) -0.0470(2) 0.1345(17) Uani 1 1 d . . . O4 O 0.5994(5) 0.4690(3) 0.00038(14) 0.1006(12) Uani 1 1 d . . . C1 C 0.6516(5) -0.2085(4) 0.19793(18) 0.0772(14) Uani 1 1 d . . . C2 C 0.7185(6) -0.2429(5) 0.23899(19) 0.0913(16) Uani 1 1 d . . . H2 H 0.6837 -0.2218 0.2688 0.110 Uiso 1 1 calc R . . C3 C 0.8409(6) -0.3109(5) 0.2337(2) 0.0923(16) Uani 1 1 d . . . C4 C 0.8912(6) -0.3386(5) 0.1894(2) 0.0927(16) Uani 1 1 d . . . H4 H 0.9747 -0.3834 0.1873 0.111 Uiso 1 1 calc R . . C5 C 0.8243(6) -0.3034(4) 0.14704(18) 0.0768(13) Uani 1 1 d . . . C6 C 0.7009(5) -0.2376(4) 0.15419(17) 0.0702(12) Uani 1 1 d . . . C7 C 0.5900(5) -0.1675(4) 0.12650(18) 0.0741(13) Uani 1 1 d . . . C8 C 0.6525(5) -0.0672(4) 0.09763(16) 0.0644(11) Uani 1 1 d . . . C9 C 0.6052(5) -0.0431(4) 0.05280(16) 0.0713(13) Uani 1 1 d . . . H9 H 0.5353 -0.0904 0.0390 0.086 Uiso 1 1 calc R . . C10 C 0.6592(5) 0.0502(4) 0.02745(16) 0.0700(12) Uani 1 1 d . . . H10 H 0.6248 0.0648 -0.0031 0.084 Uiso 1 1 calc R . . C11 C 0.7624(4) 0.1216(4) 0.04649(15) 0.0601(11) Uani 1 1 d . . . C12 C 0.8167(4) 0.0930(4) 0.09056(16) 0.0640(11) Uani 1 1 d . . . H12 H 0.8906 0.1376 0.1037 0.077 Uiso 1 1 calc R . . C13 C 0.7639(5) 0.0005(4) 0.11522(16) 0.0728(13) Uani 1 1 d . . . H13 H 0.8037 -0.0177 0.1447 0.087 Uiso 1 1 calc R . . C14 C 0.5232(6) -0.1379(5) 0.17969(19) 0.0822(15) Uani 1 1 d . . . C15 C 0.3788(7) -0.1988(6) 0.1882(3) 0.117(2) Uani 1 1 d . . . H15A H 0.3846 -0.2778 0.1772 0.175 Uiso 1 1 calc R . . H15B H 0.3040 -0.1586 0.1712 0.175 Uiso 1 1 calc R . . H15C H 0.3572 -0.1982 0.2217 0.175 Uiso 1 1 calc R . . C16 C 0.5167(7) -0.0141(5) 0.1961(2) 0.0986(17) Uani 1 1 d . . . H16A H 0.4343 0.0235 0.1821 0.148 Uiso 1 1 calc R . . H16B H 0.6032 0.0257 0.1866 0.148 Uiso 1 1 calc R . . H16C H 0.5083 -0.0121 0.2302 0.148 Uiso 1 1 calc R . . C17 C 0.9239(8) -0.3505(7) 0.2782(2) 0.119(2) Uani 1 1 d . . . H17 H 0.8656 -0.3261 0.3056 0.143 Uiso 1 1 calc R . . C18 C 1.0632(12) -0.2889(9) 0.2826(3) 0.207(5) Uani 1 1 d . . . H18A H 1.0471 -0.2064 0.2808 0.310 Uiso 1 1 calc R . . H18B H 1.1262 -0.3125 0.2572 0.310 Uiso 1 1 calc R . . H18C H 1.1069 -0.3077 0.3126 0.310 Uiso 1 1 calc R . . C19 C 0.9363(9) -0.4764(7) 0.2815(3) 0.156(3) Uani 1 1 d . . . H19A H 0.8420 -0.5109 0.2790 0.235 Uiso 1 1 calc R . . H19B H 0.9787 -0.4972 0.3115 0.235 Uiso 1 1 calc R . . H19C H 0.9964 -0.5045 0.2560 0.235 Uiso 1 1 calc R . . C20 C 0.8834(6) -0.3328(6) 0.0983(2) 0.0939(17) Uani 1 1 d . . . H20 H 0.8230 -0.2931 0.0747 0.113 Uiso 1 1 calc R . . C21 C 0.8766(9) -0.4617(6) 0.0880(3) 0.131(2) Uani 1 1 d . . . H21A H 0.9123 -0.4762 0.0564 0.197 Uiso 1 1 calc R . . H21B H 0.7782 -0.4878 0.0903 0.197 Uiso 1 1 calc R . . H21C H 0.9348 -0.5030 0.1107 0.197 Uiso 1 1 calc R . . C22 C 1.0359(8) -0.2906(8) 0.0918(3) 0.150(3) Uani 1 1 d . . . H22A H 1.0683 -0.3092 0.0602 0.226 Uiso 1 1 calc R . . H22B H 1.0977 -0.3278 0.1146 0.226 Uiso 1 1 calc R . . H22C H 1.0392 -0.2077 0.0963 0.226 Uiso 1 1 calc R . . C23 C 0.8198(5) 0.2258(4) 0.02177(15) 0.0620(11) Uani 1 1 d . . . C24 C 0.7787(5) 0.3662(4) -0.04205(18) 0.0769(14) Uani 1 1 d . . . H24 H 0.8831 0.3764 -0.0381 0.092 Uiso 1 1 calc R . . C25 C 0.7077(6) 0.4791(6) -0.0293(2) 0.0926(17) Uani 1 1 d . . . C26 C 0.5205(8) 0.5719(6) 0.0132(3) 0.135(3) Uani 1 1 d . . . H26A H 0.5872 0.6328 0.0214 0.203 Uiso 1 1 calc R . . H26B H 0.4597 0.5554 0.0401 0.203 Uiso 1 1 calc R . . H26C H 0.4620 0.5963 -0.0132 0.203 Uiso 1 1 calc R . . C27 C 0.7507(6) 0.3395(5) -0.09439(18) 0.0865(15) Uani 1 1 d . . . H27A H 0.6481 0.3256 -0.0988 0.104 Uiso 1 1 calc R . . H27B H 0.7766 0.4071 -0.1132 0.104 Uiso 1 1 calc R . . C28 C 0.8314(5) 0.2380(5) -0.11228(18) 0.0805(14) Uani 1 1 d D . . C29 C 0.7639(7) 0.1338(5) -0.1206(2) 0.115(2) Uani 1 1 d D . . H29 H 0.6653 0.1267 -0.1149 0.138 Uiso 1 1 calc R . . C30 C 0.8406(9) 0.0395(6) -0.1372(3) 0.142(3) Uani 1 1 d D . . H30 H 0.7935 -0.0313 -0.1416 0.171 Uiso 1 1 calc R . . C31 C 0.9849(9) 0.0479(6) -0.1475(3) 0.129(2) Uani 1 1 d D . . H31 H 1.0359 -0.0156 -0.1594 0.155 Uiso 1 1 calc R . . C32 C 1.0520(7) 0.1524(6) -0.1398(2) 0.113(2) Uani 1 1 d D . . H32 H 1.1499 0.1601 -0.1467 0.136 Uiso 1 1 calc R . . C33 C 0.9768(5) 0.2460(5) -0.1221(2) 0.0900(15) Uani 1 1 d D . . H33 H 1.0248 0.3159 -0.1166 0.108 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 N1 0.056(2) 0.090(3) 0.081(3) 0.030(2) -0.0050(19) -0.007(2) O1 0.095(2) 0.076(2) 0.095(3) -0.0029(19) -0.014(2) -0.014(2) O2 0.0551(17) 0.086(2) 0.083(2) 0.0097(18) -0.0072(15) -0.0002(17) O3 0.115(3) 0.097(3) 0.192(5) 0.040(3) 0.029(3) 0.023(3) O4 0.109(3) 0.094(3) 0.100(3) -0.011(2) 0.015(2) 0.001(2) C1 0.083(3) 0.075(3) 0.073(3) 0.010(3) 0.009(3) 0.003(3) C2 0.112(4) 0.092(4) 0.070(3) 0.013(3) 0.014(3) 0.012(4) C3 0.107(4) 0.098(4) 0.072(3) 0.024(3) 0.001(3) 0.016(4) C4 0.095(4) 0.086(4) 0.097(4) 0.026(3) 0.004(3) 0.021(3) C5 0.091(3) 0.066(3) 0.074(3) 0.013(2) 0.007(3) 0.009(3) C6 0.077(3) 0.057(3) 0.076(3) 0.011(2) 0.002(2) 0.008(3) C7 0.072(3) 0.069(3) 0.081(3) 0.002(3) -0.004(3) -0.008(3) C8 0.060(2) 0.068(3) 0.065(3) 0.001(2) -0.007(2) 0.004(2) C9 0.072(3) 0.068(3) 0.074(3) 0.010(2) -0.022(2) -0.001(3) C10 0.075(3) 0.076(3) 0.059(3) 0.006(2) -0.019(2) 0.006(3) C11 0.054(2) 0.065(3) 0.061(3) 0.005(2) -0.003(2) 0.008(2) C12 0.053(2) 0.075(3) 0.064(3) 0.009(2) -0.009(2) -0.004(2) C13 0.069(3) 0.087(3) 0.063(3) 0.012(2) -0.017(2) -0.002(3) C14 0.074(3) 0.077(4) 0.096(4) 0.002(3) 0.018(3) -0.001(3) C15 0.094(4) 0.104(5) 0.151(6) 0.001(4) 0.039(4) -0.010(4) C16 0.107(4) 0.080(4) 0.108(4) -0.001(3) 0.011(3) 0.010(3) C17 0.134(5) 0.135(6) 0.087(4) 0.043(4) -0.003(4) 0.018(5) C18 0.249(11) 0.202(10) 0.169(8) 0.094(7) -0.120(8) -0.094(9) C19 0.145(6) 0.141(7) 0.183(8) 0.093(6) -0.051(5) -0.012(5) C20 0.087(4) 0.112(5) 0.083(4) 0.001(3) 0.001(3) 0.023(3) C21 0.137(5) 0.121(6) 0.136(6) -0.029(5) 0.018(5) 0.012(5) C22 0.136(6) 0.189(8) 0.126(6) 0.007(6) 0.044(5) -0.038(6) C23 0.055(2) 0.074(3) 0.057(3) 0.003(2) 0.004(2) 0.013(2) C24 0.065(3) 0.076(3) 0.089(4) 0.023(3) -0.002(3) 0.000(3) C25 0.079(4) 0.091(4) 0.107(5) 0.024(4) -0.006(3) -0.002(3) C26 0.144(6) 0.103(5) 0.159(6) -0.034(5) 0.025(5) 0.017(5) C27 0.074(3) 0.105(4) 0.081(4) 0.032(3) -0.008(3) -0.005(3) C28 0.073(3) 0.082(4) 0.087(4) 0.023(3) -0.012(2) -0.001(3) C29 0.098(4) 0.099(5) 0.147(6) 0.011(4) -0.005(4) -0.020(4) C30 0.144(7) 0.094(5) 0.190(8) -0.001(5) -0.017(6) -0.022(5) C31 0.133(6) 0.097(5) 0.158(7) -0.013(5) -0.003(5) 0.015(5) C32 0.088(4) 0.113(5) 0.139(6) 0.006(4) 0.000(4) 0.010(4) C33 0.072(3) 0.090(4) 0.108(4) 0.006(3) -0.003(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C23 1.342(5) . ? N1 C24 1.430(6) . ? N1 HN1 0.85(5) . ? O1 C7 1.409(6) . ? O1 HO1 0.99(9) . ? O2 C23 1.232(5) . ? O3 C25 1.217(7) . ? O4 C25 1.308(7) . ? O4 C26 1.435(7) . ? C1 C6 1.352(6) . ? C1 C2 1.367(7) . ? C1 C14 1.526(7) . ? C2 C3 1.384(7) . ? C2 H2 0.9300 . ? C3 C4 1.364(8) . ? C3 C17 1.537(8) . ? C4 C5 1.401(7) . ? C4 H4 0.9300 . ? C5 C6 1.383(6) . ? C5 C20 1.512(7) . ? C6 C7 1.518(6) . ? C7 C8 1.523(7) . ? C7 C14 1.651(7) . ? C8 C9 1.361(6) . ? C8 C13 1.382(6) . ? C9 C10 1.379(6) . ? C9 H9 0.9300 . ? C10 C11 1.367(6) . ? C10 H10 0.9300 . ? C11 C12 1.375(6) . ? C11 C23 1.481(6) . ? C12 C13 1.358(6) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C16 1.495(7) . ? C14 C15 1.526(8) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C19 1.453(10) . ? C17 C18 1.475(11) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C22 1.504(9) . ? C20 C21 1.509(9) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C24 C25 1.497(8) . ? C24 C27 1.523(7) . ? C24 H24 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.472(7) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.369(5) . ? C28 C33 1.376(5) . ? C29 C30 1.376(6) . ? C29 H29 0.9300 . ? C30 C31 1.369(6) . ? C30 H30 0.9300 . ? C31 C32 1.367(6) . ? C31 H31 0.9300 . ? C32 C33 1.374(5) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 N1 C24 123.4(4) . . ? C23 N1 HN1 118(3) . . ? C24 N1 HN1 119(3) . . ? C7 O1 HO1 110(5) . . ? C25 O4 C26 118.4(5) . . ? C6 C1 C2 122.8(5) . . ? C6 C1 C14 95.1(4) . . ? C2 C1 C14 142.1(5) . . ? C1 C2 C3 116.3(5) . . ? C1 C2 H2 121.9 . . ? C3 C2 H2 121.9 . . ? C4 C3 C2 120.6(5) . . ? C4 C3 C17 120.2(6) . . ? C2 C3 C17 119.2(6) . . ? C3 C4 C5 123.8(5) . . ? C3 C4 H4 118.1 . . ? C5 C4 H4 118.1 . . ? C6 C5 C4 113.5(5) . . ? C6 C5 C20 123.5(5) . . ? C4 C5 C20 123.0(5) . . ? C1 C6 C5 123.1(5) . . ? C1 C6 C7 96.1(4) . . ? C5 C6 C7 140.6(5) . . ? O1 C7 C6 113.2(4) . . ? O1 C7 C8 110.6(4) . . ? C6 C7 C8 114.6(4) . . ? O1 C7 C14 114.2(4) . . ? C6 C7 C14 84.2(4) . . ? C8 C7 C14 117.9(4) . . ? C9 C8 C13 117.1(4) . . ? C9 C8 C7 121.6(4) . . ? C13 C8 C7 121.2(4) . . ? C8 C9 C10 121.2(4) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C11 C10 C9 121.1(4) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 117.6(4) . . ? C10 C11 C23 123.5(4) . . ? C12 C11 C23 118.9(4) . . ? C13 C12 C11 120.9(4) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C8 121.7(4) . . ? C12 C13 H13 119.1 . . ? C8 C13 H13 119.1 . . ? C16 C14 C1 115.6(5) . . ? C16 C14 C15 110.5(5) . . ? C1 C14 C15 112.7(4) . . ? C16 C14 C7 119.3(4) . . ? C1 C14 C7 84.5(4) . . ? C15 C14 C7 112.0(5) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 113.8(7) . . ? C19 C17 C3 112.6(7) . . ? C18 C17 C3 111.2(6) . . ? C19 C17 H17 106.2 . . ? C18 C17 H17 106.2 . . ? C3 C17 H17 106.2 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C21 109.4(6) . . ? C22 C20 C5 112.2(6) . . ? C21 C20 C5 112.2(5) . . ? C22 C20 H20 107.6 . . ? C21 C20 H20 107.6 . . ? C5 C20 H20 107.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O2 C23 N1 121.8(4) . . ? O2 C23 C11 122.1(4) . . ? N1 C23 C11 116.1(4) . . ? N1 C24 C25 113.3(4) . . ? N1 C24 C27 111.3(4) . . ? C25 C24 C27 109.3(4) . . ? N1 C24 H24 107.6 . . ? C25 C24 H24 107.6 . . ? C27 C24 H24 107.6 . . ? O3 C25 O4 123.6(6) . . ? O3 C25 C24 122.0(5) . . ? O4 C25 C24 114.3(5) . . ? O4 C26 H26A 109.5 . . ? O4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C24 113.7(4) . . ? C28 C27 H27A 108.8 . . ? C24 C27 H27A 108.8 . . ? C28 C27 H27B 108.8 . . ? C24 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? C29 C28 C33 118.1(6) . . ? C29 C28 C27 121.2(5) . . ? C33 C28 C27 120.7(5) . . ? C28 C29 C30 120.7(6) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C31 C30 C29 121.2(7) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C32 C31 C30 118.1(7) . . ? C32 C31 H31 120.9 . . ? C30 C31 H31 120.9 . . ? C31 C32 C33 120.9(6) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C32 C33 C28 121.0(5) . . ? C32 C33 H33 119.5 . . ? C28 C33 H33 119.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.181 _refine_diff_density_min -0.139 _refine_diff_density_rms 0.031 #===END data_15.9%C,17.4%D _database_code_depnum_ccdc_archive 'CCDC 799264' #TrackingRef '- 1.cif' #==================================================================== # start Validation Reply Form _vrf_PLAT201_15.9%C,17.4%D ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 24 RESPONSE: In the crystal there are reactant and photoproduct molecules. Part of atoms were refined isotropically in order to decrease a large number of the parameters in the refinement. ; # end Validation Reply Form #==================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 N O4' _chemical_formula_weight 513.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 22.093(4) _cell_length_b 9.3747(19) _cell_length_c 28.939(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5994(2) _cell_formula_units_Z 8 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 3.64 _cell_measurement_theta_max 13.74 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27901 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5369 _reflns_number_gt 3865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSALIS (Oxford Diffraction, 2003)' _computing_cell_refinement 'CRYSALIS (Oxford Diffraction, 2003)' _computing_data_reduction 'CRYSALIS (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SXELXL97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Owing to a reactant-product disorder, the following weak restraints from SHELXL97 were applied: DFIX, DANG and SIMU. DFIX and DANG restrained bond lengths and valence angles to target values. The target values were taken from the structures of the pure reactant and the pure product of crystal 1a. SIMU restrained displacement parameters of atoms of the products. ; _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^)+(0.1386P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5369 _refine_ls_number_parameters 777 _refine_ls_number_restraints 633 _refine_ls_R_factor_all 0.1016 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.2226 _refine_ls_wR_factor_gt 0.1992 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1A N 0.3871(3) 0.9420(7) 0.4499(3) 0.0562(17) Uani 0.841(8) 1 d PDU A 1 H1A H 0.3721 1.0255 0.4544 0.067 Uiso 0.841(8) 1 calc PR A 1 O1A O 0.1014(3) 1.1009(11) 0.3555(3) 0.109(3) Uani 0.841(8) 1 d PDU A 1 O2A O 0.3805(3) 0.7381(7) 0.4098(3) 0.065(2) Uani 0.841(8) 1 d PDU A 1 O3A O 0.5459(3) 0.9311(10) 0.4672(4) 0.159(4) Uani 0.841(8) 1 d PDU A 1 O4A O 0.4878(4) 1.0895(9) 0.4347(3) 0.088(3) Uani 0.841(8) 1 d PDU A 1 C1A C 0.1351(5) 1.0430(9) 0.2484(3) 0.070(2) Uani 0.841(8) 1 d PDU A 1 C2A C 0.1178(10) 0.9822(16) 0.2065(3) 0.079(3) Uani 0.841(8) 1 d PDU A 1 H2A H 0.1249 1.0336 0.1796 0.094 Uiso 0.841(8) 1 calc PR A 1 C3A C 0.0912(5) 0.8512(10) 0.2028(2) 0.070(2) Uani 0.841(8) 1 d PDU A 1 C4A C 0.0797(4) 0.7770(8) 0.2427(2) 0.069(2) Uani 0.841(8) 1 d PDU A 1 H4A H 0.0610 0.6883 0.2411 0.082 Uiso 0.841(8) 1 calc PR A 1 C5A C 0.0957(4) 0.8328(8) 0.2861(2) 0.065(2) Uani 0.841(8) 1 d PDU A 1 C6A C 0.1212(4) 0.9665(8) 0.2884(2) 0.062(2) Uani 0.841(8) 1 d PDU A 1 C7A C 0.1366(2) 1.0251(6) 0.3351(2) 0.0548(17) Uani 0.841(8) 1 d PDU A 1 C23A C 0.3595(4) 0.8536(9) 0.4206(4) 0.051(2) Uani 0.841(8) 1 d PDU A 1 C11A C 0.30204(19) 0.9060(6) 0.40015(18) 0.051(3) Uiso 0.841(8) 1 d PGDU A 1 C12A C 0.28708(19) 0.8548(5) 0.35649(18) 0.055(2) Uiso 0.841(8) 1 d PGDU A 1 H12A H 0.3134 0.7936 0.3411 0.065 Uiso 0.841(8) 1 d PG A 1 C13A C 0.2341(2) 0.8939(5) 0.33611(16) 0.0566(18) Uiso 0.841(8) 1 d PGDU A 1 H13A H 0.2247 0.8585 0.3069 0.068 Uiso 0.841(8) 1 d PG A 1 C8A C 0.19378(18) 0.9849(5) 0.35778(18) 0.0481(16) Uiso 0.841(8) 1 d PGDU A 1 C9A C 0.20843(19) 1.0366(5) 0.40131(17) 0.0515(16) Uiso 0.841(8) 1 d PGDU A 1 H9A H 0.1820 1.0977 0.4166 0.062 Uiso 0.841(8) 1 d PG A 1 C10A C 0.2621(2) 0.9974(6) 0.42185(15) 0.0533(19) Uiso 0.841(8) 1 d PGDU A 1 H10A H 0.2716 1.0332 0.4509 0.064 Uiso 0.841(8) 1 d PG A 1 C14A C 0.1674(3) 1.1824(7) 0.2480(3) 0.088(3) Uani 0.841(8) 1 d PDU A 1 H14A H 0.1765 1.2084 0.2801 0.106 Uiso 0.841(8) 1 calc PR A 1 C15A C 0.1283(5) 1.2987(10) 0.2275(6) 0.142(5) Uani 0.841(8) 1 d PDU A 1 H15A H 0.1506 1.3866 0.2269 0.214 Uiso 0.841(8) 1 calc PR A 1 H15B H 0.0926 1.3105 0.2460 0.214 Uiso 0.841(8) 1 calc PR A 1 H15C H 0.1170 1.2728 0.1966 0.214 Uiso 0.841(8) 1 calc PR A 1 C16A C 0.2270(4) 1.1733(12) 0.2217(5) 0.132(4) Uani 0.841(8) 1 d PDU A 1 H16A H 0.2467 1.2646 0.2223 0.198 Uiso 0.841(8) 1 calc PR A 1 H16B H 0.2192 1.1460 0.1903 0.198 Uiso 0.841(8) 1 calc PR A 1 H16C H 0.2527 1.1035 0.2361 0.198 Uiso 0.841(8) 1 calc PR A 1 C17A C 0.0755(4) 0.7905(10) 0.1562(3) 0.087(3) Uani 0.841(8) 1 d PDU A 1 H17A H 0.0687 0.8727 0.1359 0.104 Uiso 0.841(8) 1 calc PR A 1 C18A C 0.1296(5) 0.7149(17) 0.1371(4) 0.153(5) Uani 0.841(8) 1 d PDU A 1 H18A H 0.1646 0.7749 0.1401 0.229 Uiso 0.841(8) 1 calc PR A 1 H18B H 0.1230 0.6933 0.1051 0.229 Uiso 0.841(8) 1 calc PR A 1 H18C H 0.1360 0.6280 0.1539 0.229 Uiso 0.841(8) 1 calc PR A 1 C19A C 0.0197(5) 0.7067(14) 0.1545(4) 0.133(5) Uani 0.841(8) 1 d PDU A 1 H19A H 0.0126 0.6752 0.1234 0.199 Uiso 0.841(8) 1 calc PR A 1 H19B H -0.0136 0.7646 0.1646 0.199 Uiso 0.841(8) 1 calc PR A 1 H19C H 0.0235 0.6254 0.1745 0.199 Uiso 0.841(8) 1 calc PR A 1 C20A C 0.0823(4) 0.7467(8) 0.3295(3) 0.081(2) Uani 0.841(8) 1 d PDU A 1 H20A H 0.0998 0.7985 0.3557 0.097 Uiso 0.841(8) 1 calc PR A 1 C21A C 0.0155(4) 0.736(2) 0.3379(6) 0.141(5) Uani 0.841(8) 1 d PDU A 1 H21A H -0.0046 0.8162 0.3243 0.212 Uiso 0.841(8) 1 calc PR A 1 H21B H 0.0079 0.7344 0.3706 0.212 Uiso 0.841(8) 1 calc PR A 1 H21C H 0.0003 0.6494 0.3243 0.212 Uiso 0.841(8) 1 calc PR A 1 C22A C 0.1130(6) 0.6034(11) 0.3271(4) 0.125(4) Uani 0.841(8) 1 d PDU A 1 H22A H 0.1559 0.6157 0.3308 0.187 Uiso 0.841(8) 1 calc PR A 1 H22B H 0.1049 0.5601 0.2977 0.187 Uiso 0.841(8) 1 calc PR A 1 H22C H 0.0979 0.5432 0.3513 0.187 Uiso 0.841(8) 1 calc PR A 1 C24A C 0.4414(3) 0.9020(7) 0.4743(2) 0.0616(18) Uani 0.841(8) 1 d PDU A 1 H24A H 0.4471 0.7994 0.4696 0.074 Uiso 0.841(8) 1 calc PR A 1 C25A C 0.4975(3) 0.9748(7) 0.4576(3) 0.072(2) Uani 0.841(8) 1 d PDU A 1 C26A C 0.5393(6) 1.1689(17) 0.4186(6) 0.102(5) Uani 0.841(8) 1 d PDU A 1 H26A H 0.5568 1.2205 0.4439 0.153 Uiso 0.841(8) 1 calc PR A 1 H26B H 0.5267 1.2348 0.3951 0.153 Uiso 0.841(8) 1 calc PR A 1 H26C H 0.5688 1.1044 0.4060 0.153 Uiso 0.841(8) 1 calc PR A 1 C27A C 0.4332(3) 0.9258(9) 0.5258(2) 0.075(2) Uani 0.841(8) 1 d PDU A 1 H27A H 0.4704 0.9004 0.5415 0.090 Uiso 0.841(8) 1 calc PR A 1 H27B H 0.4258 1.0264 0.5313 0.090 Uiso 0.841(8) 1 calc PR A 1 C28A C 0.3825(2) 0.8417(5) 0.5458(2) 0.071(2) Uiso 0.841(8) 1 d PGDU A 1 C29A C 0.3281(3) 0.9049(5) 0.5565(3) 0.103(3) Uiso 0.841(8) 1 d PGDU A 1 H29A H 0.3234 1.0025 0.5520 0.124 Uiso 0.841(8) 1 d PG A 1 C30A C 0.2807(2) 0.8270(7) 0.5736(3) 0.129(4) Uiso 0.841(8) 1 d PGU A 1 H30A H 0.2445 0.8726 0.5808 0.155 Uiso 0.841(8) 1 d PG A 1 C31A C 0.2859(3) 0.6821(7) 0.5805(3) 0.117(3) Uiso 0.841(8) 1 d PGU A 1 H31A H 0.2539 0.6295 0.5926 0.140 Uiso 0.841(8) 1 d PG A 1 C32A C 0.3391(3) 0.6181(5) 0.5689(3) 0.106(3) Uiso 0.841(8) 1 d PGU A 1 H32A H 0.3431 0.5200 0.5724 0.128 Uiso 0.841(8) 1 d PG A 1 C33A C 0.3868(2) 0.6958(5) 0.5520(2) 0.081(2) Uiso 0.841(8) 1 d PGDU A 1 H33A H 0.4228 0.6495 0.5445 0.098 Uiso 0.841(8) 1 d PG A 1 N1B N 0.3507(3) 0.4389(9) 0.4261(3) 0.058(2) Uani 0.826(8) 1 d PDU B 2 H1B H 0.3662 0.5208 0.4198 0.070 Uiso 0.826(8) 1 calc PR B 2 O1B O 0.6351(3) 0.6238(12) 0.5171(3) 0.117(3) Uani 0.826(8) 1 d PDU B 2 O2B O 0.3564(5) 0.2404(9) 0.4693(5) 0.066(3) Uani 0.826(8) 1 d PDU B 2 O3B O 0.1920(2) 0.4032(8) 0.4209(4) 0.122(3) Uani 0.826(8) 1 d PDU B 2 O4B O 0.2494(3) 0.5863(7) 0.4397(3) 0.081(2) Uani 0.826(8) 1 d PDU B 2 C1B C 0.6049(6) 0.5776(10) 0.6241(3) 0.072(2) Uani 0.826(8) 1 d PDU B 2 C2B C 0.6224(8) 0.5234(12) 0.6666(3) 0.085(4) Uani 0.826(8) 1 d PDU B 2 H2B H 0.6128 0.5747 0.6931 0.101 Uiso 0.826(8) 1 calc PR B 2 C3B C 0.6535(7) 0.3975(12) 0.6713(3) 0.088(3) Uani 0.826(8) 1 d PDU B 2 C4B C 0.6681(5) 0.3218(10) 0.6324(3) 0.075(3) Uani 0.826(8) 1 d PDU B 2 H4B H 0.6910 0.2389 0.6351 0.090 Uiso 0.826(8) 1 calc PR B 2 C5B C 0.6490(6) 0.3672(9) 0.5885(3) 0.072(3) Uani 0.826(8) 1 d PDU B 2 C6B C 0.6178(4) 0.4942(9) 0.5851(2) 0.0640(18) Uani 0.826(8) 1 d PDU B 2 C7B C 0.6015(2) 0.5459(7) 0.5375(2) 0.0550(17) Uani 0.826(8) 1 d PDU B 2 C23B C 0.3771(3) 0.3562(8) 0.4571(3) 0.0478(16) Uani 0.826(8) 1 d PDU B 2 C11B C 0.43587(18) 0.4065(6) 0.47646(18) 0.048(2) Uiso 0.826(8) 1 d PGDU B 2 C12B C 0.45254(18) 0.3595(5) 0.52024(17) 0.0495(17) Uiso 0.826(8) 1 d PGDU B 2 H12B H 0.4272 0.2981 0.5365 0.059 Uiso 0.826(8) 1 d PG B 2 C13B C 0.50570(19) 0.4029(5) 0.53944(15) 0.0526(17) Uiso 0.826(8) 1 d PGDU B 2 H13B H 0.5162 0.3703 0.5687 0.063 Uiso 0.826(8) 1 d PG B 2 C8B C 0.54444(17) 0.4945(5) 0.51642(18) 0.0510(17) Uiso 0.826(8) 1 d PGDU B 2 C9B C 0.52809(19) 0.5421(5) 0.47276(17) 0.0516(16) Uiso 0.826(8) 1 d PGDU B 2 H9B H 0.5535 0.6035 0.4566 0.062 Uiso 0.826(8) 1 d PG B 2 C10B C 0.4743(2) 0.4985(6) 0.45341(15) 0.0497(18) Uiso 0.826(8) 1 d PGDU B 2 H10B H 0.4636 0.5316 0.4242 0.060 Uiso 0.826(8) 1 d PG B 2 C14B C 0.5717(4) 0.7167(7) 0.6220(3) 0.090(3) Uani 0.826(8) 1 d PDU B 2 H14B H 0.5649 0.7412 0.5895 0.108 Uiso 0.826(8) 1 calc PR B 2 C15B C 0.6078(5) 0.8348(11) 0.6442(5) 0.141(4) Uani 0.826(8) 1 d PDU B 2 H15D H 0.5856 0.9225 0.6423 0.212 Uiso 0.826(8) 1 calc PR B 2 H15E H 0.6458 0.8451 0.6283 0.212 Uiso 0.826(8) 1 calc PR B 2 H15F H 0.6152 0.8119 0.6760 0.212 Uiso 0.826(8) 1 calc PR B 2 C16B C 0.5106(4) 0.7088(12) 0.6463(4) 0.112(3) Uani 0.826(8) 1 d PDU B 2 H16D H 0.4915 0.6194 0.6393 0.169 Uiso 0.826(8) 1 calc PR B 2 H16E H 0.4853 0.7856 0.6358 0.169 Uiso 0.826(8) 1 calc PR B 2 H16F H 0.5163 0.7164 0.6791 0.169 Uiso 0.826(8) 1 calc PR B 2 C17B C 0.6723(5) 0.3475(13) 0.7186(3) 0.129(4) Uani 0.826(8) 1 d PDU B 2 H17B H 0.6523 0.4142 0.7397 0.154 Uiso 0.826(8) 1 calc PR B 2 C18B C 0.6461(7) 0.2061(15) 0.7308(5) 0.160(5) Uani 0.826(8) 1 d PDU B 2 H18D H 0.6027 0.2122 0.7305 0.240 Uiso 0.826(8) 1 calc PR B 2 H18E H 0.6596 0.1788 0.7611 0.240 Uiso 0.826(8) 1 calc PR B 2 H18F H 0.6591 0.1361 0.7087 0.240 Uiso 0.826(8) 1 calc PR B 2 C19B C 0.7358(5) 0.3654(14) 0.7284(4) 0.137(5) Uani 0.826(8) 1 d PDU B 2 H19D H 0.7524 0.4371 0.7083 0.205 Uiso 0.826(8) 1 calc PR B 2 H19E H 0.7565 0.2767 0.7233 0.205 Uiso 0.826(8) 1 calc PR B 2 H19F H 0.7408 0.3942 0.7600 0.205 Uiso 0.826(8) 1 calc PR B 2 C20B C 0.6614(6) 0.2740(11) 0.5469(3) 0.099(3) Uani 0.826(8) 1 d PDU B 2 H20B H 0.6453 0.3231 0.5197 0.118 Uiso 0.826(8) 1 calc PR B 2 C21B C 0.7278(6) 0.2522(16) 0.5395(6) 0.140(5) Uani 0.826(8) 1 d PDU B 2 H21D H 0.7499 0.3270 0.5545 0.209 Uiso 0.826(8) 1 calc PR B 2 H21E H 0.7364 0.2538 0.5069 0.209 Uiso 0.826(8) 1 calc PR B 2 H21F H 0.7397 0.1617 0.5521 0.209 Uiso 0.826(8) 1 calc PR B 2 C22B C 0.6295(6) 0.1309(12) 0.5507(5) 0.135(5) Uani 0.826(8) 1 d PDU B 2 H22D H 0.5868 0.1439 0.5463 0.202 Uiso 0.826(8) 1 calc PR B 2 H22E H 0.6368 0.0907 0.5807 0.202 Uiso 0.826(8) 1 calc PR B 2 H22F H 0.6449 0.0675 0.5274 0.202 Uiso 0.826(8) 1 calc PR B 2 C24B C 0.2964(3) 0.3946(9) 0.4026(3) 0.057(2) Uani 0.826(8) 1 d PDU B 2 H24B H 0.2929 0.2909 0.4060 0.069 Uiso 0.826(8) 1 calc PR B 2 C25B C 0.2398(3) 0.4613(9) 0.4226(3) 0.071(3) Uani 0.826(8) 1 d PDU B 2 C26B C 0.1978(4) 0.6628(9) 0.4583(4) 0.089(3) Uani 0.826(8) 1 d PDU B 2 H26D H 0.1867 0.7382 0.4375 0.133 Uiso 0.826(8) 1 calc PR B 2 H26E H 0.2082 0.7026 0.4878 0.133 Uiso 0.826(8) 1 calc PR B 2 H26F H 0.1644 0.5983 0.4618 0.133 Uiso 0.826(8) 1 calc PR B 2 C27B C 0.3007(3) 0.4281(9) 0.3508(3) 0.067(2) Uani 0.826(8) 1 d PDU B 2 H27C H 0.2637 0.3972 0.3357 0.081 Uiso 0.826(8) 1 calc PR B 2 H27D H 0.3040 0.5305 0.3467 0.081 Uiso 0.826(8) 1 calc PR B 2 C28B C 0.3529(3) 0.3583(6) 0.3281(2) 0.068(2) Uiso 0.826(8) 1 d PGDU B 2 C29B C 0.4062(3) 0.4289(6) 0.3192(3) 0.086(2) Uiso 0.826(8) 1 d PGDU B 2 H29B H 0.4094 0.5253 0.3263 0.104 Uiso 0.826(8) 1 d PG B 2 C30B C 0.4547(3) 0.3600(8) 0.2999(3) 0.116(3) Uiso 0.826(8) 1 d PGU B 2 H30B H 0.4901 0.4105 0.2939 0.140 Uiso 0.826(8) 1 d PG B 2 C31B C 0.4518(3) 0.2171(9) 0.2891(3) 0.129(4) Uiso 0.826(8) 1 d PGU B 2 H31B H 0.4845 0.1707 0.2755 0.154 Uiso 0.826(8) 1 d PG B 2 C32B C 0.3998(3) 0.1455(6) 0.2990(3) 0.112(3) Uiso 0.826(8) 1 d PGU B 2 H32B H 0.3973 0.0484 0.2928 0.135 Uiso 0.826(8) 1 d PG B 2 C33B C 0.3509(3) 0.2142(6) 0.3181(3) 0.094(3) Uiso 0.826(8) 1 d PGDU B 2 H33B H 0.3158 0.1629 0.3243 0.112 Uiso 0.826(8) 1 d PG B 2 N1C N 0.3775(14) 0.956(4) 0.4583(11) 0.061(10) Uiso 0.159(8) 1 d PDU A 3 H1C H 0.3555 1.0282 0.4656 0.074 Uiso 0.159(8) 1 calc PR A 3 O1C O 0.1136(12) 1.148(3) 0.3469(10) 0.069(11) Uiso 0.159(8) 1 d PDU A 3 O2C O 0.3887(19) 0.763(4) 0.4130(18) 0.067(13) Uiso 0.159(8) 1 d PDU A 3 O3C O 0.5291(15) 1.017(5) 0.4978(13) 0.144(14) Uiso 0.159(8) 1 d PDU A 3 O4C O 0.486(2) 1.058(6) 0.4303(12) 0.080(10) Uiso 0.159(8) 1 d PDU A 3 C1C C 0.135(3) 1.023(5) 0.2475(8) 0.073(10) Uiso 0.159(8) 1 d PDU A 3 C2C C 0.119(6) 0.964(10) 0.2058(8) 0.083(11) Uiso 0.159(8) 1 d PDU A 3 H2C H 0.1353 0.9974 0.1781 0.099 Uiso 0.159(8) 1 calc PR A 3 C3C C 0.079(3) 0.850(5) 0.2075(9) 0.069(6) Uiso 0.159(8) 1 d PDU A 3 C4C C 0.062(2) 0.793(4) 0.2489(9) 0.068(6) Uiso 0.159(8) 1 d PDU A 3 H4C H 0.0366 0.7150 0.2487 0.082 Uiso 0.159(8) 1 calc PR A 3 C5C C 0.082(2) 0.847(4) 0.2918(9) 0.060(10) Uiso 0.159(8) 1 d PDU A 3 C6C C 0.1209(17) 0.961(3) 0.2885(8) 0.062(10) Uiso 0.159(8) 1 d PDU A 3 C7C C 0.1535(9) 1.071(2) 0.3181(7) 0.088(10) Uiso 0.159(8) 1 d PDU A 3 C23C C 0.362(2) 0.875(6) 0.4217(19) 0.050(10) Uiso 0.159(8) 1 d PDU A 3 C11C C 0.3066(9) 0.922(3) 0.3967(7) 0.033(10) Uiso 0.159(8) 1 d PGDU A 3 C12C C 0.2964(9) 0.876(3) 0.3522(7) 0.050(9) Uiso 0.159(8) 1 d PGDU A 3 H12C H 0.3236 0.8138 0.3384 0.059 Uiso 0.159(8) 1 d PG A 3 C13C C 0.2471(10) 0.921(2) 0.3283(6) 0.046(7) Uiso 0.159(8) 1 d PGDU A 3 H13C H 0.2416 0.8899 0.2980 0.055 Uiso 0.159(8) 1 d PG A 3 C8C C 0.2048(8) 1.012(2) 0.3476(6) 0.035(6) Uiso 0.159(8) 1 d PGDU A 3 C9C C 0.2169(8) 1.063(2) 0.3906(6) 0.038(6) Uiso 0.159(8) 1 d PGDU A 3 H9C H 0.1909 1.1298 0.4037 0.045 Uiso 0.159(8) 1 d PG A 3 C10C C 0.2671(9) 1.019(3) 0.4150(6) 0.042(7) Uiso 0.159(8) 1 d PGDU A 3 H10C H 0.2743 1.0558 0.4443 0.050 Uiso 0.159(8) 1 d PG A 3 C14C C 0.1648(14) 1.154(3) 0.2682(8) 0.095(10) Uiso 0.159(8) 1 d PDU A 3 C15C C 0.125(3) 1.287(4) 0.2644(18) 0.141(12) Uiso 0.159(8) 1 d PDU A 3 H15G H 0.0853 1.2661 0.2755 0.211 Uiso 0.159(8) 1 calc PR A 3 H15H H 0.1231 1.3168 0.2327 0.211 Uiso 0.159(8) 1 calc PR A 3 H15I H 0.1425 1.3625 0.2827 0.211 Uiso 0.159(8) 1 calc PR A 3 C16C C 0.2267(18) 1.185(6) 0.2503(16) 0.134(12) Uiso 0.159(8) 1 d PDU A 3 H16G H 0.2514 1.1011 0.2531 0.201 Uiso 0.159(8) 1 calc PR A 3 H16H H 0.2444 1.2611 0.2679 0.201 Uiso 0.159(8) 1 calc PR A 3 H16I H 0.2242 1.2123 0.2184 0.201 Uiso 0.159(8) 1 calc PR A 3 C17C C 0.060(2) 0.779(5) 0.1621(10) 0.087(11) Uiso 0.159(8) 1 d PDU A 3 H17C H 0.0658 0.8491 0.1374 0.105 Uiso 0.159(8) 1 calc PR A 3 C18C C 0.100(3) 0.656(6) 0.152(2) 0.136(12) Uiso 0.159(8) 1 d PDU A 3 H18G H 0.1411 0.6863 0.1525 0.204 Uiso 0.159(8) 1 calc PR A 3 H18H H 0.0902 0.6202 0.1214 0.204 Uiso 0.159(8) 1 calc PR A 3 H18I H 0.0932 0.5827 0.1742 0.204 Uiso 0.159(8) 1 calc PR A 3 C19C C -0.0042(19) 0.741(8) 0.162(2) 0.121(12) Uiso 0.159(8) 1 d PDU A 3 H19G H -0.0277 0.8236 0.1707 0.182 Uiso 0.159(8) 1 calc PR A 3 H19H H -0.0110 0.6667 0.1844 0.182 Uiso 0.159(8) 1 calc PR A 3 H19I H -0.0159 0.7093 0.1322 0.182 Uiso 0.159(8) 1 calc PR A 3 C20C C 0.064(2) 0.776(4) 0.3368(10) 0.091(11) Uiso 0.159(8) 1 d PDU A 3 H20C H 0.0683 0.8463 0.3617 0.109 Uiso 0.159(8) 1 calc PR A 3 C21C C -0.001(2) 0.725(9) 0.336(3) 0.145(11) Uiso 0.159(8) 1 d PDU A 3 H21G H -0.0272 0.8047 0.3408 0.217 Uiso 0.159(8) 1 calc PR A 3 H21H H -0.0066 0.6569 0.3607 0.217 Uiso 0.159(8) 1 calc PR A 3 H21I H -0.0092 0.6807 0.3071 0.217 Uiso 0.159(8) 1 calc PR A 3 C22C C 0.105(3) 0.652(6) 0.348(2) 0.117(11) Uiso 0.159(8) 1 d PDU A 3 H22G H 0.0960 0.6150 0.3778 0.176 Uiso 0.159(8) 1 calc PR A 3 H22H H 0.1467 0.6829 0.3469 0.176 Uiso 0.159(8) 1 calc PR A 3 H22I H 0.0994 0.5779 0.3250 0.176 Uiso 0.159(8) 1 calc PR A 3 C24C C 0.4302(11) 0.924(4) 0.4851(8) 0.063(10) Uiso 0.159(8) 1 d PDU A 3 H24C H 0.4399 0.8247 0.4781 0.076 Uiso 0.159(8) 1 calc PR A 3 C25C C 0.4855(13) 1.006(5) 0.4725(10) 0.087(11) Uiso 0.159(8) 1 d PDU A 3 C26C C 0.538(4) 1.140(12) 0.417(2) 0.097(18) Uiso 0.159(8) 1 d PDU A 3 C27C C 0.4174(16) 0.927(4) 0.5365(8) 0.079(10) Uiso 0.159(8) 1 d PDU A 3 H27E H 0.4547 0.9065 0.5529 0.094 Uiso 0.159(8) 1 calc PR A 3 H27F H 0.4049 1.0228 0.5450 0.094 Uiso 0.159(8) 1 calc PR A 3 C28C C 0.3704(11) 0.826(3) 0.5522(9) 0.054(7) Uiso 0.159(8) 1 d PGDU A 3 C29C C 0.3265(13) 0.870(3) 0.5823(12) 0.105(12) Uiso 0.159(8) 1 d PGDU A 3 H29C H 0.3283 0.9614 0.5946 0.126 Uiso 0.159(8) 1 d PG A 3 C30C C 0.2797(13) 0.781(4) 0.5944(13) 0.098(9) Uiso 0.159(8) 1 d PGU A 3 H30C H 0.2510 0.8115 0.6157 0.118 Uiso 0.159(8) 1 d PG A 3 C31C C 0.2745(15) 0.647(4) 0.5756(15) 0.163(18) Uiso 0.159(8) 1 d PGU A 3 H31C H 0.2423 0.5877 0.5835 0.196 Uiso 0.159(8) 1 d PG A 3 C32C C 0.3179(19) 0.603(3) 0.5451(16) 0.119(14) Uiso 0.159(8) 1 d PGU A 3 H32C H 0.3152 0.5131 0.5319 0.143 Uiso 0.159(8) 1 d PG A 3 C33C C 0.3656(16) 0.691(3) 0.5337(12) 0.108(13) Uiso 0.159(8) 1 d PGDU A 3 H33C H 0.3950 0.6584 0.5133 0.130 Uiso 0.159(8) 1 d PG A 3 N1D N 0.3552(14) 0.449(4) 0.4269(13) 0.054(9) Uiso 0.174(8) 1 d PDU B 4 H1D H 0.3658 0.5369 0.4251 0.065 Uiso 0.174(8) 1 calc PR B 4 O1D O 0.6341(16) 0.668(5) 0.5242(12) 0.143(18) Uiso 0.174(8) 1 d PDU B 4 O2D O 0.368(2) 0.244(4) 0.466(2) 0.056(12) Uiso 0.174(8) 1 d PDU B 4 O3D O 0.1983(11) 0.455(4) 0.3958(12) 0.100(11) Uiso 0.174(8) 1 d PDU B 4 O4D O 0.2516(15) 0.556(4) 0.4516(11) 0.077(9) Uiso 0.174(8) 1 d PDU B 4 C1D C 0.611(3) 0.569(4) 0.6248(8) 0.074(10) Uiso 0.174(8) 1 d PDU B 4 C2D C 0.633(4) 0.535(5) 0.6672(12) 0.086(11) Uiso 0.174(8) 1 d PDU B 4 H2D H 0.6321 0.5975 0.6922 0.104 Uiso 0.174(8) 1 calc PR B 4 C3D C 0.659(3) 0.400(4) 0.6701(12) 0.092(10) Uiso 0.174(8) 1 d PDU B 4 C4D C 0.654(3) 0.308(3) 0.6339(11) 0.075(11) Uiso 0.174(8) 1 d PDU B 4 H4D H 0.6595 0.2107 0.6394 0.090 Uiso 0.174(8) 1 calc PR B 4 C5D C 0.641(3) 0.352(4) 0.5886(10) 0.069(10) Uiso 0.174(8) 1 d PDU B 4 C6D C 0.6228(18) 0.493(3) 0.5862(9) 0.065(5) Uiso 0.174(8) 1 d PDU B 4 C7D C 0.5925(10) 0.596(2) 0.5528(7) 0.080(10) Uiso 0.174(8) 1 d PDU B 4 C23D C 0.3875(16) 0.362(4) 0.4541(14) 0.052(5) Uiso 0.174(8) 1 d PDU B 4 C11D C 0.4395(8) 0.428(2) 0.4783(7) 0.031(7) Uiso 0.174(8) 1 d PGDU B 4 C12D C 0.4517(8) 0.388(2) 0.5231(7) 0.077(12) Uiso 0.174(8) 1 d PGDU B 4 H12D H 0.4257 0.3259 0.5382 0.092 Uiso 0.174(8) 1 d PG B 4 C13D C 0.5013(8) 0.439(2) 0.5456(5) 0.038(6) Uiso 0.174(8) 1 d PGDU B 4 H13D H 0.5081 0.4114 0.5760 0.046 Uiso 0.174(8) 1 d PG B 4 C8D C 0.5419(7) 0.530(2) 0.5244(6) 0.040(6) Uiso 0.174(8) 1 d PGDU B 4 C9D C 0.5277(8) 0.576(2) 0.4811(6) 0.050(6) Uiso 0.174(8) 1 d PGDU B 4 H9D H 0.5525 0.6428 0.4667 0.060 Uiso 0.174(8) 1 d PG B 4 C10D C 0.4772(8) 0.526(2) 0.4583(5) 0.038(6) Uiso 0.174(8) 1 d PGDU B 4 H10D H 0.4687 0.5592 0.4287 0.045 Uiso 0.174(8) 1 d PG B 4 C14D C 0.5740(13) 0.685(3) 0.6002(9) 0.105(10) Uiso 0.174(8) 1 d PDU B 4 C15D C 0.606(2) 0.829(3) 0.6038(17) 0.137(7) Uiso 0.174(8) 1 d PDU B 4 H15J H 0.6457 0.8216 0.5915 0.205 Uiso 0.174(8) 1 calc PR B 4 H15K H 0.6076 0.8571 0.6357 0.205 Uiso 0.174(8) 1 calc PR B 4 H15L H 0.5831 0.8988 0.5867 0.205 Uiso 0.174(8) 1 calc PR B 4 C16D C 0.5098(16) 0.696(5) 0.6160(17) 0.136(11) Uiso 0.174(8) 1 d PDU B 4 H16J H 0.4917 0.6026 0.6158 0.204 Uiso 0.174(8) 1 calc PR B 4 H16K H 0.4878 0.7573 0.5955 0.204 Uiso 0.174(8) 1 calc PR B 4 H16L H 0.5087 0.7340 0.6467 0.204 Uiso 0.174(8) 1 calc PR B 4 C17D C 0.681(2) 0.346(4) 0.7174(11) 0.135(11) Uiso 0.174(8) 1 d PDU B 4 H17D H 0.6938 0.4299 0.7347 0.162 Uiso 0.174(8) 1 calc PR B 4 C18D C 0.630(2) 0.284(8) 0.744(2) 0.152(8) Uiso 0.174(8) 1 d PDU B 4 H18J H 0.5921 0.3136 0.7299 0.228 Uiso 0.174(8) 1 calc PR B 4 H18K H 0.6314 0.3159 0.7750 0.228 Uiso 0.174(8) 1 calc PR B 4 H18L H 0.6323 0.1817 0.7427 0.228 Uiso 0.174(8) 1 calc PR B 4 C19D C 0.733(2) 0.254(7) 0.7129(19) 0.144(12) Uiso 0.174(8) 1 d PDU B 4 H19J H 0.7692 0.3120 0.7118 0.216 Uiso 0.174(8) 1 calc PR B 4 H19K H 0.7302 0.1992 0.6851 0.216 Uiso 0.174(8) 1 calc PR B 4 H19L H 0.7355 0.1913 0.7390 0.216 Uiso 0.174(8) 1 calc PR B 4 C20D C 0.664(2) 0.269(4) 0.5471(12) 0.102(11) Uiso 0.174(8) 1 d PDU B 4 H20D H 0.6361 0.2870 0.5212 0.123 Uiso 0.174(8) 1 calc PR B 4 C21D C 0.726(3) 0.315(6) 0.533(3) 0.130(12) Uiso 0.174(8) 1 d PDU B 4 H21J H 0.7300 0.4162 0.5364 0.195 Uiso 0.174(8) 1 calc PR B 4 H21K H 0.7337 0.2878 0.5017 0.195 Uiso 0.174(8) 1 calc PR B 4 H21L H 0.7555 0.2688 0.5529 0.195 Uiso 0.174(8) 1 calc PR B 4 C22D C 0.663(3) 0.111(3) 0.557(2) 0.130(12) Uiso 0.174(8) 1 d PDU B 4 H22J H 0.6234 0.0824 0.5670 0.196 Uiso 0.174(8) 1 calc PR B 4 H22K H 0.6917 0.0904 0.5815 0.196 Uiso 0.174(8) 1 calc PR B 4 H22L H 0.6743 0.0590 0.5300 0.196 Uiso 0.174(8) 1 calc PR B 4 C24D C 0.3039(10) 0.403(4) 0.4006(9) 0.063(10) Uiso 0.174(8) 1 d PDU B 4 H24D H 0.2981 0.3007 0.4065 0.076 Uiso 0.174(8) 1 calc PR B 4 C25D C 0.2467(11) 0.478(6) 0.4142(13) 0.079(10) Uiso 0.174(8) 1 d PDU B 4 C26D C 0.197(2) 0.611(7) 0.4723(19) 0.125(18) Uiso 0.174(8) 1 d PDU B 4 C27D C 0.3154(14) 0.421(4) 0.3488(9) 0.074(10) Uiso 0.174(8) 1 d PDU B 4 H27G H 0.2784 0.3992 0.3323 0.088 Uiso 0.174(8) 1 calc PR B 4 H27H H 0.3249 0.5207 0.3429 0.088 Uiso 0.174(8) 1 calc PR B 4 C28D C 0.3647(10) 0.332(2) 0.3302(8) 0.041(7) Uiso 0.174(8) 1 d PGDU B 4 C29D C 0.4174(11) 0.391(2) 0.3143(11) 0.103(12) Uiso 0.174(8) 1 d PGDU B 4 H29D H 0.4218 0.4893 0.3136 0.124 Uiso 0.174(8) 1 d PG B 4 C30D C 0.4641(10) 0.305(3) 0.2993(12) 0.085(8) Uiso 0.174(8) 1 d PGU B 4 H30D H 0.4991 0.3472 0.2876 0.102 Uiso 0.174(8) 1 d PG B 4 C31D C 0.4601(10) 0.160(3) 0.3013(12) 0.114(13) Uiso 0.174(8) 1 d PGU B 4 H31D H 0.4921 0.1023 0.2917 0.136 Uiso 0.174(8) 1 d PG B 4 C32D C 0.4078(12) 0.101(2) 0.3178(12) 0.079(9) Uiso 0.174(8) 1 d PGU B 4 H32D H 0.4041 0.0020 0.3195 0.095 Uiso 0.174(8) 1 d PG B 4 C33D C 0.3604(10) 0.185(2) 0.3317(10) 0.065(8) Uiso 0.174(8) 1 d PGDU B 4 H33D H 0.3249 0.1433 0.3423 0.078 Uiso 0.174(8) 1 d PG B 4 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 N1A 0.053(3) 0.042(3) 0.073(4) -0.002(3) -0.014(3) 0.003(2) O1A 0.073(4) 0.139(7) 0.116(6) -0.061(6) -0.036(4) 0.041(5) O2A 0.062(3) 0.044(3) 0.089(5) -0.013(3) -0.007(3) 0.001(3) O3A 0.058(4) 0.149(6) 0.271(12) 0.089(8) -0.019(5) -0.002(4) O4A 0.078(4) 0.069(5) 0.117(5) 0.013(4) 0.027(3) -0.004(3) C1A 0.075(5) 0.062(4) 0.073(5) -0.003(3) -0.012(4) -0.009(4) C2A 0.086(6) 0.082(7) 0.068(5) 0.010(4) -0.013(4) 0.001(6) C3A 0.077(6) 0.071(4) 0.061(4) -0.004(3) -0.009(4) -0.006(4) C4A 0.077(5) 0.064(4) 0.065(4) -0.010(3) -0.012(4) -0.001(4) C5A 0.061(5) 0.084(5) 0.052(4) -0.003(4) -0.002(3) 0.003(4) C6A 0.046(4) 0.067(4) 0.073(5) -0.012(3) -0.012(3) 0.006(3) C7A 0.047(3) 0.059(3) 0.058(4) -0.014(3) 0.000(3) 0.013(3) C23A 0.052(4) 0.041(4) 0.059(4) 0.005(3) 0.001(3) -0.007(3) C14A 0.098(6) 0.077(5) 0.090(6) 0.006(4) -0.008(5) -0.027(4) C15A 0.135(8) 0.075(5) 0.217(13) 0.006(7) 0.012(9) -0.013(6) C16A 0.108(7) 0.123(7) 0.164(11) 0.005(8) 0.002(7) -0.033(6) C17A 0.103(7) 0.103(5) 0.053(4) -0.002(4) -0.024(5) 0.000(5) C18A 0.166(11) 0.207(12) 0.085(7) -0.053(8) -0.023(7) 0.038(9) C19A 0.165(11) 0.140(10) 0.092(7) -0.003(6) -0.049(8) -0.050(9) C20A 0.088(6) 0.096(6) 0.060(5) 0.008(4) 0.007(4) -0.002(5) C21A 0.111(8) 0.168(10) 0.144(10) 0.052(8) 0.042(8) 0.016(8) C22A 0.160(9) 0.115(7) 0.099(7) 0.043(6) 0.017(7) 0.032(7) C24A 0.055(4) 0.052(3) 0.078(5) -0.006(3) -0.011(4) 0.005(3) C25A 0.054(4) 0.066(5) 0.095(6) -0.006(4) -0.006(4) -0.006(3) C26A 0.078(6) 0.077(9) 0.151(10) 0.002(6) 0.050(6) -0.011(5) C27A 0.078(5) 0.080(4) 0.069(5) -0.013(4) -0.018(4) 0.012(4) N1B 0.056(4) 0.040(3) 0.079(4) -0.001(3) -0.013(3) -0.003(2) O1B 0.082(4) 0.168(8) 0.101(5) 0.076(5) -0.039(3) -0.068(5) O2B 0.053(4) 0.055(3) 0.090(5) 0.006(2) -0.007(4) -0.007(3) O3B 0.058(3) 0.097(4) 0.210(10) -0.038(6) 0.013(4) -0.017(3) O4B 0.063(3) 0.068(4) 0.113(5) -0.006(4) 0.028(3) 0.000(3) C1B 0.065(5) 0.081(5) 0.069(5) 0.006(4) -0.001(4) -0.003(4) C2B 0.097(10) 0.105(6) 0.051(4) 0.004(4) -0.002(4) -0.004(6) C3B 0.086(6) 0.124(7) 0.052(4) 0.022(4) -0.019(4) -0.004(5) C4B 0.066(7) 0.089(5) 0.069(5) 0.023(4) -0.004(4) 0.014(5) C5B 0.076(6) 0.084(5) 0.056(4) 0.005(4) -0.006(4) -0.006(5) C6B 0.055(4) 0.081(4) 0.056(4) 0.021(3) -0.010(3) -0.010(3) C7B 0.053(3) 0.065(4) 0.047(4) 0.011(3) 0.003(3) -0.009(3) C23B 0.043(4) 0.042(3) 0.059(4) -0.003(3) 0.011(3) 0.006(3) C14B 0.110(6) 0.082(5) 0.077(5) -0.004(4) 0.009(5) 0.017(5) C15B 0.134(7) 0.114(7) 0.176(9) -0.007(7) -0.001(7) 0.001(6) C16B 0.087(6) 0.138(7) 0.113(8) -0.005(6) 0.007(6) 0.032(5) C17B 0.139(9) 0.171(10) 0.075(6) 0.033(7) -0.021(6) 0.015(8) C18B 0.181(9) 0.182(9) 0.118(8) 0.048(7) -0.035(7) -0.024(8) C19B 0.125(8) 0.155(9) 0.130(8) 0.043(7) -0.085(7) -0.032(7) C20B 0.126(7) 0.106(6) 0.064(5) -0.002(4) 0.002(5) 0.019(6) C21B 0.113(8) 0.168(12) 0.138(10) -0.042(10) 0.035(7) -0.015(9) C22B 0.130(9) 0.109(7) 0.165(11) -0.036(7) 0.025(8) -0.004(7) C24B 0.049(4) 0.048(3) 0.076(5) -0.004(3) -0.015(3) -0.004(3) C25B 0.055(4) 0.069(5) 0.089(6) 0.000(5) -0.010(4) 0.002(4) C26B 0.077(5) 0.065(5) 0.125(7) 0.005(5) 0.047(5) 0.016(4) C27B 0.057(4) 0.072(4) 0.073(5) 0.002(4) -0.022(4) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1A C23A 1.334(6) . ? N1A C24A 1.441(6) . ? N1A H1A 0.8600 . ? O1A C7A 1.207(6) . ? O2A C23A 1.218(6) . ? O3A C25A 1.177(7) . ? O4A C25A 1.282(7) . ? O4A C26A 1.437(7) . ? C1A C2A 1.392(7) . ? C1A C6A 1.396(7) . ? C1A C14A 1.489(7) . ? C2A C3A 1.366(7) . ? C2A H2A 0.9300 . ? C3A C4A 1.373(7) . ? C3A C17A 1.505(7) . ? C4A C5A 1.404(7) . ? C4A H4A 0.9300 . ? C5A C6A 1.375(7) . ? C5A C20A 1.523(7) . ? C6A C7A 1.499(6) . ? C7A C8A 1.472(5) . ? C23A C11A 1.485(5) . ? C11A C10A 1.3819 . ? C11A C12A 1.3912 . ? C12A C13A 1.3616 . ? C12A H12A 0.9300 . ? C13A C8A 1.3833 . ? C13A H13A 0.9300 . ? C8A C9A 1.3878 . ? C9A C10A 1.3759 . ? C9A H9A 0.9299 . ? C10A H10A 0.9300 . ? C14A C15A 1.512(8) . ? C14A C16A 1.523(8) . ? C14A H14A 0.9800 . ? C15A H15A 0.9600 . ? C15A H15B 0.9600 . ? C15A H15C 0.9600 . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C17A C19A 1.462(8) . ? C17A C18A 1.496(8) . ? C17A H17A 0.9800 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C19A H19A 0.9600 . ? C19A H19B 0.9600 . ? C19A H19C 0.9600 . ? C20A C21A 1.499(8) . ? C20A C22A 1.507(8) . ? C20A H20A 0.9800 . ? C21A H21A 0.9600 . ? C21A H21B 0.9600 . ? C21A H21C 0.9600 . ? C22A H22A 0.9600 . ? C22A H22B 0.9600 . ? C22A H22C 0.9600 . ? C24A C25A 1.496(7) . ? C24A C27A 1.517(7) . ? C24A H24A 0.9800 . ? C26A H26A 0.9600 . ? C26A H26B 0.9600 . ? C26A H26C 0.9600 . ? C27A C28A 1.487(7) . ? C27A H27A 0.9700 . ? C27A H27B 0.9700 . ? C28A C29A 1.3755 . ? C28A C33A 1.3831 . ? C29A C30A 1.3701 . ? C29A H29A 0.9300 . ? C30A C31A 1.3771 . ? C30A H30A 0.9299 . ? C31A C32A 1.3617 . ? C31A H31A 0.9300 . ? C32A C33A 1.3725 . ? C32A H32A 0.9300 . ? C33A H33A 0.9300 . ? N1B C23B 1.322(6) . ? N1B C24B 1.439(6) . ? N1B H1B 0.8600 . ? O1B C7B 1.197(6) . ? O2B C23B 1.230(6) . ? O3B C25B 1.188(7) . ? O4B C25B 1.290(7) . ? O4B C26B 1.450(6) . ? C1B C2B 1.386(7) . ? C1B C6B 1.402(7) . ? C1B C14B 1.497(7) . ? C2B C3B 1.371(7) . ? C2B H2B 0.9300 . ? C3B C4B 1.370(8) . ? C3B C17B 1.505(7) . ? C4B C5B 1.404(7) . ? C4B H4B 0.9300 . ? C5B C6B 1.380(7) . ? C5B C20B 1.511(7) . ? C6B C7B 1.504(7) . ? C7B C8B 1.481(5) . ? C23B C11B 1.491(5) . ? C11B C10B 1.3819 . ? C11B C12B 1.3912 . ? C12B C13B 1.3616 . ? C12B H12B 0.9300 . ? C13B C8B 1.3834 . ? C13B H13B 0.9300 . ? C8B C9B 1.3878 . ? C9B C10B 1.3759 . ? C9B H9B 0.9299 . ? C10B H10B 0.9300 . ? C14B C15B 1.507(9) . ? C14B C16B 1.525(8) . ? C14B H14B 0.9800 . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? C17B C19B 1.440(9) . ? C17B C18B 1.490(9) . ? C17B H17B 0.9800 . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? C19B H19D 0.9600 . ? C19B H19E 0.9600 . ? C19B H19F 0.9600 . ? C20B C21B 1.498(9) . ? C20B C22B 1.519(9) . ? C20B H20B 0.9800 . ? C21B H21D 0.9600 . ? C21B H21E 0.9600 . ? C21B H21F 0.9600 . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? C24B C25B 1.514(7) . ? C24B C27B 1.535(7) . ? C24B H24B 0.9800 . ? C26B H26D 0.9600 . ? C26B H26E 0.9600 . ? C26B H26F 0.9600 . ? C27B C28B 1.479(7) . ? C27B H27C 0.9700 . ? C27B H27D 0.9700 . ? C28B C29B 1.3754 . ? C28B C33B 1.3831 . ? C29B C30B 1.3701 . ? C29B H29B 0.9300 . ? C30B C31B 1.3771 . ? C30B H30B 0.9300 . ? C31B C32B 1.3618 . ? C31B H31B 0.9299 . ? C32B C33B 1.3726 . ? C32B H32B 0.9300 . ? C33B H33B 0.9300 . ? N1C C23C 1.350(10) . ? N1C C24C 1.430(10) . ? N1C H1C 0.8600 . ? O1C C7C 1.413(10) . ? O2C C23C 1.230(10) . ? O3C C25C 1.215(10) . ? O4C C25C 1.312(10) . ? O4C C26C 1.434(11) . ? C1C C6C 1.355(9) . ? C1C C2C 1.367(9) . ? C1C C14C 1.524(9) . ? C2C C3C 1.384(10) . ? C2C H2C 0.9300 . ? C3C C4C 1.364(10) . ? C3C C17C 1.537(10) . ? C4C C5C 1.404(10) . ? C4C H4C 0.9300 . ? C5C C6C 1.381(9) . ? C5C C20C 1.514(9) . ? C6C C7C 1.522(9) . ? C7C C8C 1.525(9) . ? C7C C14C 1.657(10) . ? C23C C11C 1.482(9) . ? C11C C10C 1.3672 . ? C11C C12C 1.3750 . ? C12C C13C 1.3582 . ? C12C H12C 0.9300 . ? C13C C8C 1.3818 . ? C13C H13C 0.9300 . ? C8C C9C 1.3609 . ? C9C C10C 1.3794 . ? C9C H9C 0.9300 . ? C10C H10C 0.9299 . ? C14C C16C 1.491(10) . ? C14C C15C 1.528(10) . ? C15C H15G 0.9600 . ? C15C H15H 0.9600 . ? C15C H15I 0.9600 . ? C16C H16G 0.9600 . ? C16C H16H 0.9600 . ? C16C H16I 0.9600 . ? C17C C19C 1.458(11) . ? C17C C18C 1.477(11) . ? C17C H17C 0.9800 . ? C18C H18G 0.9600 . ? C18C H18H 0.9600 . ? C18C H18I 0.9600 . ? C19C H19G 0.9600 . ? C19C H19H 0.9600 . ? C19C H19I 0.9600 . ? C20C C21C 1.508(11) . ? C20C C22C 1.511(11) . ? C20C H20C 0.9800 . ? C21C H21G 0.9600 . ? C21C H21H 0.9600 . ? C21C H21I 0.9600 . ? C22C H22G 0.9600 . ? C22C H22H 0.9600 . ? C22C H22I 0.9600 . ? C24C C25C 1.489(10) . ? C24C C27C 1.514(10) . ? C24C H24C 0.9800 . ? C27C C28C 1.479(9) . ? C27C H27E 0.9700 . ? C27C H27F 0.9700 . ? C28C C29C 1.3689 . ? C28C C33C 1.3759 . ? C29C C30C 1.3761 . ? C29C H29C 0.9300 . ? C30C C31C 1.3694 . ? C30C H30C 0.9301 . ? C31C C32C 1.3674 . ? C31C H31C 0.9300 . ? C32C C33C 1.3744 . ? C32C H32C 0.9300 . ? C33C H33C 0.9300 . ? N1D C23D 1.341(10) . ? N1D C24D 1.431(11) . ? N1D H1D 0.8600 . ? O1D C7D 1.406(10) . ? O2D C23D 1.236(10) . ? O3D C25D 1.215(10) . ? O4D C25D 1.310(10) . ? O4D C26D 1.434(11) . ? C1D C6D 1.355(10) . ? C1D C2D 1.365(9) . ? C1D C14D 1.527(9) . ? C2D C3D 1.387(10) . ? C2D H2D 0.9300 . ? C3D C4D 1.366(10) . ? C3D C17D 1.536(10) . ? C4D C5D 1.403(10) . ? C4D H4D 0.9300 . ? C5D C6D 1.384(10) . ? C5D C20D 1.514(10) . ? C6D C7D 1.522(9) . ? C7D C8D 1.524(9) . ? C7D C14D 1.651(10) . ? C23D C11D 1.484(9) . ? C11D C10D 1.3672 . ? C11D C12D 1.3750 . ? C12D C13D 1.3582 . ? C12D H12D 0.9300 . ? C13D C8D 1.3818 . ? C13D H13D 0.9300 . ? C8D C9D 1.3608 . ? C9D C10D 1.3794 . ? C9D H9D 0.9300 . ? C10D H10D 0.9300 . ? C14D C16D 1.494(10) . ? C14D C15D 1.524(10) . ? C15D H15J 0.9600 . ? C15D H15K 0.9600 . ? C15D H15L 0.9600 . ? C16D H16J 0.9600 . ? C16D H16K 0.9600 . ? C16D H16L 0.9600 . ? C17D C19D 1.454(11) . ? C17D C18D 1.474(11) . ? C17D H17D 0.9800 . ? C18D H18J 0.9600 . ? C18D H18K 0.9600 . ? C18D H18L 0.9600 . ? C19D H19J 0.9600 . ? C19D H19K 0.9600 . ? C19D H19L 0.9600 . ? C20D C21D 1.507(11) . ? C20D C22D 1.512(11) . ? C20D H20D 0.9800 . ? C21D H21J 0.9600 . ? C21D H21K 0.9600 . ? C21D H21L 0.9600 . ? C22D H22J 0.9600 . ? C22D H22K 0.9600 . ? C22D H22L 0.9600 . ? C24D C25D 1.501(10) . ? C24D C27D 1.528(10) . ? C24D H24D 0.9800 . ? C27D C28D 1.478(9) . ? C27D H27G 0.9700 . ? C27D H27H 0.9700 . ? C28D C29D 1.3688 . ? C28D C33D 1.3759 . ? C29D C30D 1.3762 . ? C29D H29D 0.9300 . ? C30D C31D 1.3694 . ? C30D H30D 0.9300 . ? C31D C32D 1.3674 . ? C31D H31D 0.9300 . ? C32D C33D 1.3744 . ? C32D H32D 0.9300 . ? C33D H33D 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23A N1A C24A 122.0(5) . . ? C23A N1A H1A 119.0 . . ? C24A N1A H1A 119.0 . . ? C25A O4A C26A 118.0(8) . . ? C2A C1A C6A 116.9(5) . . ? C2A C1A C14A 118.9(6) . . ? C6A C1A C14A 124.2(6) . . ? C3A C2A C1A 123.7(6) . . ? C3A C2A H2A 118.1 . . ? C1A C2A H2A 118.2 . . ? C2A C3A C4A 117.9(5) . . ? C2A C3A C17A 120.7(6) . . ? C4A C3A C17A 121.4(6) . . ? C3A C4A C5A 121.1(5) . . ? C3A C4A H4A 119.5 . . ? C5A C4A H4A 119.5 . . ? C6A C5A C4A 119.2(5) . . ? C6A C5A C20A 121.5(6) . . ? C4A C5A C20A 119.3(6) . . ? C5A C6A C1A 121.1(5) . . ? C5A C6A C7A 118.1(6) . . ? C1A C6A C7A 120.7(5) . . ? O1A C7A C8A 119.1(5) . . ? O1A C7A C6A 120.7(5) . . ? C8A C7A C6A 120.2(5) . . ? O2A C23A N1A 122.8(6) . . ? O2A C23A C11A 121.1(5) . . ? N1A C23A C11A 116.0(5) . . ? C10A C11A C12A 118.3 . . ? C10A C11A C23A 124.8(4) . . ? C12A C11A C23A 116.8(4) . . ? C13A C12A C11A 120.3 . . ? C12A C13A C8A 121.5 . . ? C13A C8A C9A 118.5 . . ? C13A C8A C7A 120.5(3) . . ? C9A C8A C7A 121.0(3) . . ? C10A C9A C8A 120.0 . . ? C9A C10A C11A 121.3 . . ? C1A C14A C15A 111.2(7) . . ? C1A C14A C16A 111.7(7) . . ? C15A C14A C16A 109.7(8) . . ? C1A C14A H14A 108.0 . . ? C15A C14A H14A 108.0 . . ? C16A C14A H14A 108.0 . . ? C14A C15A H15A 109.5 . . ? C14A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C14A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C14A C16A H16A 109.5 . . ? C14A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C14A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C19A C17A C18A 114.0(9) . . ? C19A C17A C3A 115.2(7) . . ? C18A C17A C3A 109.0(7) . . ? C19A C17A H17A 105.9 . . ? C18A C17A H17A 105.9 . . ? C3A C17A H17A 105.9 . . ? C17A C18A H18A 109.5 . . ? C17A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C17A C19A H19A 109.5 . . ? C17A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C17A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C21A C20A C22A 113.0(8) . . ? C21A C20A C5A 111.3(7) . . ? C22A C20A C5A 110.3(6) . . ? C21A C20A H20A 107.3 . . ? C22A C20A H20A 107.3 . . ? C5A C20A H20A 107.3 . . ? C20A C21A H21A 109.5 . . ? C20A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C20A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C20A C22A H22A 109.5 . . ? C20A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C20A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? N1A C24A C25A 114.4(5) . . ? N1A C24A C27A 110.1(6) . . ? C25A C24A C27A 110.4(5) . . ? N1A C24A H24A 107.2 . . ? C25A C24A H24A 107.2 . . ? C27A C24A H24A 107.2 . . ? O3A C25A O4A 124.5(7) . . ? O3A C25A C24A 121.2(6) . . ? O4A C25A C24A 114.2(6) . . ? C28A C27A C24A 113.3(5) . . ? C28A C27A H27A 108.9 . . ? C24A C27A H27A 108.9 . . ? C28A C27A H27B 108.9 . . ? C24A C27A H27B 108.9 . . ? H27A C27A H27B 107.7 . . ? C29A C28A C33A 117.2 . . ? C29A C28A C27A 121.1(4) . . ? C33A C28A C27A 121.5(4) . . ? C30A C29A C28A 121.3 . . ? C29A C30A C31A 121.0 . . ? C32A C31A C30A 118.1 . . ? C31A C32A C33A 121.2 . . ? C32A C33A C28A 121.2 . . ? C23B N1B C24B 121.3(6) . . ? C23B N1B H1B 119.4 . . ? C24B N1B H1B 119.4 . . ? C25B O4B C26B 117.5(6) . . ? C2B C1B C6B 116.9(6) . . ? C2B C1B C14B 119.4(7) . . ? C6B C1B C14B 123.6(6) . . ? C3B C2B C1B 122.9(7) . . ? C3B C2B H2B 118.6 . . ? C1B C2B H2B 118.6 . . ? C4B C3B C2B 118.9(6) . . ? C4B C3B C17B 121.4(7) . . ? C2B C3B C17B 119.8(7) . . ? C3B C4B C5B 121.0(6) . . ? C3B C4B H4B 119.5 . . ? C5B C4B H4B 119.5 . . ? C6B C5B C4B 118.4(5) . . ? C6B C5B C20B 122.2(6) . . ? C4B C5B C20B 119.4(6) . . ? C5B C6B C1B 121.7(5) . . ? C5B C6B C7B 117.5(6) . . ? C1B C6B C7B 120.6(6) . . ? O1B C7B C8B 121.5(5) . . ? O1B C7B C6B 120.0(6) . . ? C8B C7B C6B 118.4(5) . . ? O2B C23B N1B 123.3(6) . . ? O2B C23B C11B 119.6(5) . . ? N1B C23B C11B 117.0(5) . . ? C10B C11B C12B 118.3 . . ? C10B C11B C23B 123.4(3) . . ? C12B C11B C23B 118.2(3) . . ? C13B C12B C11B 120.3 . . ? C13B C12B H12B 119.8 . . ? C11B C12B H12B 119.8 . . ? C12B C13B C8B 121.5 . . ? C12B C13B H13B 119.2 . . ? C8B C13B H13B 119.2 . . ? C13B C8B C9B 118.5 . . ? C13B C8B C7B 122.0(3) . . ? C9B C8B C7B 119.5(3) . . ? C10B C9B C8B 120.0 . . ? C10B C9B H9B 120.0 . . ? C8B C9B H9B 120.0 . . ? C9B C10B C11B 121.3 . . ? C9B C10B H10B 119.3 . . ? C11B C10B H10B 119.3 . . ? C1B C14B C15B 111.4(8) . . ? C1B C14B C16B 111.9(7) . . ? C15B C14B C16B 108.0(8) . . ? C1B C14B H14B 108.5 . . ? C15B C14B H14B 108.5 . . ? C16B C14B H14B 108.5 . . ? C14B C15B H15D 109.5 . . ? C14B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C14B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C14B C16B H16D 109.5 . . ? C14B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C14B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C19B C17B C18B 115.8(10) . . ? C19B C17B C3B 114.4(8) . . ? C18B C17B C3B 112.7(8) . . ? C19B C17B H17B 104.1 . . ? C18B C17B H17B 104.1 . . ? C3B C17B H17B 104.1 . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C17B C19B H19D 109.5 . . ? C17B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C17B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C21B C20B C5B 111.8(8) . . ? C21B C20B C22B 110.1(9) . . ? C5B C20B C22B 111.7(8) . . ? C21B C20B H20B 107.7 . . ? C5B C20B H20B 107.7 . . ? C22B C20B H20B 107.7 . . ? C20B C21B H21D 109.5 . . ? C20B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C20B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C20B C22B H22D 109.5 . . ? C20B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C20B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? N1B C24B C25B 112.9(5) . . ? N1B C24B C27B 110.5(6) . . ? C25B C24B C27B 109.8(5) . . ? N1B C24B H24B 107.8 . . ? C25B C24B H24B 107.8 . . ? C27B C24B H24B 107.8 . . ? O3B C25B O4B 125.4(6) . . ? O3B C25B C24B 121.9(6) . . ? O4B C25B C24B 112.7(5) . . ? O4B C26B H26D 109.5 . . ? O4B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? O4B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C28B C27B C24B 113.0(5) . . ? C28B C27B H27C 109.0 . . ? C24B C27B H27C 109.0 . . ? C28B C27B H27D 109.0 . . ? C24B C27B H27D 109.0 . . ? H27C C27B H27D 107.8 . . ? C29B C28B C33B 117.2 . . ? C29B C28B C27B 122.6(4) . . ? C33B C28B C27B 120.0(4) . . ? C30B C29B C28B 121.3 . . ? C30B C29B H29B 119.3 . . ? C28B C29B H29B 119.3 . . ? C29B C30B C31B 121.0 . . ? C29B C30B H30B 119.5 . . ? C31B C30B H30B 119.5 . . ? C32B C31B C30B 118.1 . . ? C32B C31B H31B 121.0 . . ? C30B C31B H31B 121.0 . . ? C31B C32B C33B 121.2 . . ? C31B C32B H32B 119.4 . . ? C33B C32B H32B 119.4 . . ? C32B C33B C28B 121.2 . . ? C32B C33B H33B 119.4 . . ? C28B C33B H33B 119.4 . . ? C23C N1C C24C 121.3(17) . . ? C23C N1C H1C 119.3 . . ? C24C N1C H1C 119.3 . . ? C25C O4C C26C 116.9(19) . . ? C6C C1C C2C 123.0(14) . . ? C6C C1C C14C 95.6(9) . . ? C2C C1C C14C 141.4(15) . . ? C1C C2C C3C 115.9(15) . . ? C1C C2C H2C 122.1 . . ? C3C C2C H2C 122.1 . . ? C4C C3C C2C 120.4(13) . . ? C4C C3C C17C 120.3(14) . . ? C2C C3C C17C 118.9(13) . . ? C3C C4C C5C 123.6(12) . . ? C3C C4C H4C 118.2 . . ? C5C C4C H4C 118.2 . . ? C6C C5C C4C 113.9(11) . . ? C6C C5C C20C 124.1(14) . . ? C4C C5C C20C 121.8(13) . . ? C1C C6C C5C 122.1(12) . . ? C1C C6C C7C 95.6(9) . . ? C5C C6C C7C 141.6(14) . . ? O1C C7C C6C 112.6(15) . . ? O1C C7C C8C 108.7(12) . . ? C6C C7C C8C 114.7(14) . . ? O1C C7C C14C 111.6(13) . . ? C6C C7C C14C 84.2(8) . . ? C8C C7C C14C 123.2(18) . . ? O2C C23C N1C 120.9(16) . . ? O2C C23C C11C 123.4(17) . . ? N1C C23C C11C 115.3(12) . . ? C10C C11C C12C 117.6 . . ? C10C C11C C23C 122.2(10) . . ? C12C C11C C23C 120.0(11) . . ? C13C C12C C11C 120.9 . . ? C12C C13C C8C 121.7 . . ? C9C C8C C13C 117.1 . . ? C9C C8C C7C 121.9(9) . . ? C13C C8C C7C 120.0(9) . . ? C8C C9C C10C 121.2 . . ? C11C C10C C9C 121.1 . . ? C16C C14C C1C 114.9(14) . . ? C16C C14C C15C 110.0(13) . . ? C1C C14C C15C 112.4(14) . . ? C16C C14C C7C 122.1(15) . . ? C1C C14C C7C 84.2(8) . . ? C15C C14C C7C 111.1(13) . . ? C14C C15C H15G 109.5 . . ? C14C C15C H15H 109.5 . . ? H15G C15C H15H 109.5 . . ? C14C C15C H15I 109.5 . . ? H15G C15C H15I 109.5 . . ? H15H C15C H15I 109.5 . . ? C14C C16C H16G 109.5 . . ? C14C C16C H16H 109.5 . . ? H16G C16C H16H 109.5 . . ? C14C C16C H16I 109.5 . . ? H16G C16C H16I 109.5 . . ? H16H C16C H16I 109.5 . . ? C19C C17C C18C 112.9(17) . . ? C19C C17C C3C 111.8(16) . . ? C18C C17C C3C 110.4(16) . . ? C19C C17C H17C 107.1 . . ? C18C C17C H17C 107.1 . . ? C3C C17C H17C 107.1 . . ? C17C C18C H18G 109.5 . . ? C17C C18C H18H 109.5 . . ? H18G C18C H18H 109.5 . . ? C17C C18C H18I 109.5 . . ? H18G C18C H18I 109.5 . . ? H18H C18C H18I 109.5 . . ? C17C C19C H19G 109.5 . . ? C17C C19C H19H 109.5 . . ? H19G C19C H19H 109.5 . . ? C17C C19C H19I 109.5 . . ? H19G C19C H19I 109.5 . . ? H19H C19C H19I 109.5 . . ? C21C C20C C22C 109.2(16) . . ? C21C C20C C5C 111.9(16) . . ? C22C C20C C5C 111.2(16) . . ? C21C C20C H20C 108.1 . . ? C22C C20C H20C 108.1 . . ? C5C C20C H20C 108.1 . . ? C20C C21C H21G 109.5 . . ? C20C C21C H21H 109.5 . . ? H21G C21C H21H 109.5 . . ? C20C C21C H21I 109.5 . . ? H21G C21C H21I 109.5 . . ? H21H C21C H21I 109.5 . . ? C20C C22C H22G 109.5 . . ? C20C C22C H22H 109.5 . . ? H22G C22C H22H 109.5 . . ? C20C C22C H22I 109.5 . . ? H22G C22C H22I 109.5 . . ? H22H C22C H22I 109.5 . . ? N1C C24C C25C 115.3(16) . . ? N1C C24C C27C 112.2(16) . . ? C25C C24C C27C 112.7(14) . . ? N1C C24C H24C 105.2 . . ? C25C C24C H24C 105.2 . . ? C27C C24C H24C 105.2 . . ? O3C C25C O4C 121.5(16) . . ? O3C C25C C24C 123.0(16) . . ? O4C C25C C24C 115.3(14) . . ? C28C C27C C24C 114.9(14) . . ? C28C C27C H27E 108.5 . . ? C24C C27C H27E 108.5 . . ? C28C C27C H27F 108.5 . . ? C24C C27C H27F 108.5 . . ? H27E C27C H27F 107.5 . . ? C29C C28C C33C 118.1 . . ? C29C C28C C27C 119.8(11) . . ? C33C C28C C27C 121.8(11) . . ? C28C C29C C30C 120.7 . . ? C31C C30C C29C 121.2 . . ? C32C C31C C30C 118.1 . . ? C31C C32C C33C 120.9 . . ? C32C C33C C28C 121.0 . . ? C23D N1D C24D 123.4(19) . . ? C23D N1D H1D 118.3 . . ? C24D N1D H1D 118.3 . . ? C25D O4D C26D 118.3(18) . . ? C6D C1D C2D 123.0(15) . . ? C6D C1D C14D 95.4(9) . . ? C2D C1D C14D 141.4(13) . . ? C1D C2D C3D 114.8(13) . . ? C1D C2D H2D 122.6 . . ? C3D C2D H2D 122.6 . . ? C4D C3D C2D 120.1(15) . . ? C4D C3D C17D 119.8(15) . . ? C2D C3D C17D 118.9(14) . . ? C3D C4D C5D 122.9(15) . . ? C3D C4D H4D 118.6 . . ? C5D C4D H4D 118.6 . . ? C6D C5D C4D 113.1(12) . . ? C6D C5D C20D 123.1(16) . . ? C4D C5D C20D 121.4(16) . . ? C1D C6D C5D 121.3(14) . . ? C1D C6D C7D 95.7(9) . . ? C5D C6D C7D 140.4(16) . . ? O1D C7D C6D 112.8(15) . . ? O1D C7D C8D 110.9(13) . . ? C6D C7D C8D 113.9(13) . . ? O1D C7D C14D 114.4(14) . . ? C6D C7D C14D 84.4(8) . . ? C8D C7D C14D 118.1(18) . . ? O2D C23D N1D 121.4(16) . . ? O2D C23D C11D 121.1(16) . . ? N1D C23D C11D 115.8(15) . . ? C10D C11D C12D 117.6 . . ? C10D C11D C23D 123.5(11) . . ? C12D C11D C23D 118.9(10) . . ? C13D C12D C11D 120.9 . . ? C12D C13D C8D 121.7 . . ? C9D C8D C13D 117.1 . . ? C9D C8D C7D 122.4(9) . . ? C13D C8D C7D 119.3(9) . . ? C8D C9D C10D 121.2 . . ? C11D C10D C9D 121.1 . . ? C16D C14D C15D 110.6(13) . . ? C16D C14D C1D 114.0(15) . . ? C15D C14D C1D 110.8(14) . . ? C16D C14D C7D 121.5(14) . . ? C15D C14D C7D 112.9(13) . . ? C1D C14D C7D 84.3(8) . . ? C14D C15D H15J 109.5 . . ? C14D C15D H15K 109.5 . . ? H15J C15D H15K 109.5 . . ? C14D C15D H15L 109.5 . . ? H15J C15D H15L 109.5 . . ? H15K C15D H15L 109.5 . . ? C14D C16D H16J 109.5 . . ? C14D C16D H16K 109.5 . . ? H16J C16D H16K 109.5 . . ? C14D C16D H16L 109.5 . . ? H16J C16D H16L 109.5 . . ? H16K C16D H16L 109.5 . . ? C19D C17D C18D 115.2(17) . . ? C19D C17D C3D 111.5(16) . . ? C18D C17D C3D 110.5(16) . . ? C19D C17D H17D 106.3 . . ? C18D C17D H17D 106.3 . . ? C3D C17D H17D 106.3 . . ? C17D C18D H18J 109.5 . . ? C17D C18D H18K 109.5 . . ? H18J C18D H18K 109.5 . . ? C17D C18D H18L 109.5 . . ? H18J C18D H18L 109.5 . . ? H18K C18D H18L 109.5 . . ? C17D C19D H19J 109.5 . . ? C17D C19D H19K 109.5 . . ? H19J C19D H19K 109.5 . . ? C17D C19D H19L 109.5 . . ? H19J C19D H19L 109.5 . . ? H19K C19D H19L 109.5 . . ? C21D C20D C22D 109.6(15) . . ? C21D C20D C5D 111.3(16) . . ? C22D C20D C5D 110.4(15) . . ? C21D C20D H20D 108.5 . . ? C22D C20D H20D 108.5 . . ? C5D C20D H20D 108.5 . . ? C20D C21D H21J 109.5 . . ? C20D C21D H21K 109.5 . . ? H21J C21D H21K 109.5 . . ? C20D C21D H21L 109.5 . . ? H21J C21D H21L 109.5 . . ? H21K C21D H21L 109.5 . . ? C20D C22D H22J 109.5 . . ? C20D C22D H22K 109.5 . . ? H22J C22D H22K 109.5 . . ? C20D C22D H22L 109.5 . . ? H22J C22D H22L 109.5 . . ? H22K C22D H22L 109.5 . . ? N1D C24D C25D 112.6(15) . . ? N1D C24D C27D 110.8(16) . . ? C25D C24D C27D 110.1(15) . . ? N1D C24D H24D 107.7 . . ? C25D C24D H24D 107.7 . . ? C27D C24D H24D 107.7 . . ? O3D C25D O4D 122.5(15) . . ? O3D C25D C24D 122.6(16) . . ? O4D C25D C24D 114.3(14) . . ? C28D C27D C24D 114.5(15) . . ? C28D C27D H27G 108.6 . . ? C24D C27D H27G 108.6 . . ? C28D C27D H27H 108.6 . . ? C24D C27D H27H 108.6 . . ? H27G C27D H27H 107.6 . . ? C29D C28D C33D 118.1 . . ? C29D C28D C27D 121.5(12) . . ? C33D C28D C27D 120.3(11) . . ? C28D C29D C30D 120.7 . . ? C31D C30D C29D 121.2 . . ? C32D C31D C30D 118.1 . . ? C31D C32D C33D 120.9 . . ? C32D C33D C28D 121.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.184 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.039 #===END data_17.4%C,23.6%D _database_code_depnum_ccdc_archive 'CCDC 799265' #TrackingRef '- 1.cif' #==================================================================== # start Validation Reply Form _vrf_PLAT201_17.4%C,23.6%D ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 24 RESPONSE: In the crystal there are reactant and photoproduct molecules. Part of atoms were refined isotropically in order to decrease a large number of the parameters in the refinement. ; _vrf_PLAT220_17.4%C,23.6%D ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.84 Ratio PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.14 Ratio RESPONSE: This is a consequence of the strong reactant-product disorder in the crystal. ; _vrf_PLAT242_17.4%C,23.6%D ; PROBLEM: Check Low Ueq as Compared to Neighbors for C28C RESPONSE: This is a consequence of the strong reactant-product disorder in the crystal. ; _vrf_PLAT770_17.4%C,23.6%D ; PROBLEM: Suspect C-H Bond in CIF: C30D -- H31B ... 1.53 Ang. RESPONSE: Atom H31B is in the reactant molecule and atom C30D in the product molecule. Both molecules are overlapped owing to the reactant - product disorder. ; # end Validation Reply Form #==================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 N O4' _chemical_formula_weight 513.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 22.121(4) _cell_length_b 9.3817(18) _cell_length_c 28.942(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6006.4(19) _cell_formula_units_Z 8 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 3.61 _cell_measurement_theta_max 12.82 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27966 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5379 _reflns_number_gt 3693 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSALIS (Oxford Diffraction, 2003)' _computing_cell_refinement 'CRYSALIS (Oxford Diffraction, 2003)' _computing_data_reduction 'CRYSALIS (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SXELXL97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Owing to a reactant-product disorder, the following weak restraints from SHELXL97 were applied: DFIX, DANG and SIMU. DFIX and DANG restrained bond lengths and valence angles to target values. The target values were taken from the structures of the pure reactant and the pure product of crystal 1a. SIMU restrained displacement parameters of atoms of the products. ; _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^)+(0.1274P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5379 _refine_ls_number_parameters 777 _refine_ls_number_restraints 618 _refine_ls_R_factor_all 0.1058 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.2178 _refine_ls_wR_factor_gt 0.1906 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.088 _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 N1A N 0.3869(3) 0.9441(8) 0.4491(3) 0.060(2) Uani 0.826(8) 1 d PDU A 1 H1A H 0.3722 1.0281 0.4531 0.072 Uiso 0.826(8) 1 calc PR A 1 O1A O 0.1019(3) 1.1028(11) 0.3549(3) 0.114(3) Uani 0.826(8) 1 d PDU A 1 O2A O 0.3828(4) 0.7431(7) 0.4079(4) 0.067(2) Uani 0.826(8) 1 d PDU A 1 O3A O 0.5447(3) 0.9356(9) 0.4703(5) 0.157(4) Uani 0.826(8) 1 d PDU A 1 O4A O 0.4870(4) 1.0892(8) 0.4341(3) 0.089(3) Uani 0.826(8) 1 d PDU A 1 C1A C 0.1342(5) 1.0416(9) 0.2479(3) 0.073(2) Uani 0.826(8) 1 d PDU A 1 C2A C 0.1169(6) 0.9807(10) 0.2063(3) 0.083(3) Uani 0.826(8) 1 d PDU A 1 H2A H 0.1245 1.0312 0.1792 0.099 Uiso 0.826(8) 1 calc PR A 1 C3A C 0.0896(6) 0.8514(10) 0.2028(2) 0.073(2) Uani 0.826(8) 1 d PDU A 1 C4A C 0.0785(6) 0.7761(10) 0.2429(2) 0.076(3) Uani 0.826(8) 1 d PDU A 1 H4A H 0.0600 0.6872 0.2413 0.091 Uiso 0.826(8) 1 calc PR A 1 C5A C 0.0948(5) 0.8325(9) 0.2860(2) 0.071(3) Uani 0.826(8) 1 d PDU A 1 C6A C 0.1208(4) 0.9659(8) 0.2879(2) 0.066(2) Uani 0.826(8) 1 d PDU A 1 C7A C 0.1365(3) 1.0255(7) 0.3347(2) 0.0617(19) Uani 0.826(8) 1 d PDU A 1 C23A C 0.3596(4) 0.8562(10) 0.4199(4) 0.054(2) Uani 0.826(8) 1 d PDU A 1 C11A C 0.30198(19) 0.9059(6) 0.39939(18) 0.052(3) Uiso 0.826(8) 1 d PGDU A 1 C12A C 0.28712(19) 0.8547(5) 0.35574(18) 0.054(2) Uiso 0.826(8) 1 d PGD A 1 H12A H 0.3135 0.7935 0.3404 0.064 Uiso 0.826(8) 1 d PG A 1 C13A C 0.2342(2) 0.8936(5) 0.33528(16) 0.0589(18) Uiso 0.826(8) 1 d PGDU A 1 H13A H 0.2249 0.8582 0.3061 0.071 Uiso 0.826(8) 1 d PG A 1 C8A C 0.19394(18) 0.9847(5) 0.35687(18) 0.0507(16) Uiso 0.826(8) 1 d PGDU A 1 C9A C 0.20847(19) 1.0365(5) 0.40039(18) 0.0613(18) Uiso 0.826(8) 1 d PGDU A 1 H9A H 0.1820 1.0976 0.4156 0.074 Uiso 0.826(8) 1 d PG A 1 C10A C 0.2620(2) 0.9974(6) 0.42101(16) 0.056(2) Uiso 0.826(8) 1 d PGDU A 1 H10A H 0.2715 1.0333 0.4501 0.068 Uiso 0.826(8) 1 d PG A 1 C14A C 0.1675(4) 1.1803(8) 0.2480(3) 0.098(3) Uani 0.826(8) 1 d PDU A 1 H14A H 0.1768 1.2059 0.2801 0.117 Uiso 0.826(8) 1 calc PR A 1 C15A C 0.1289(5) 1.2972(10) 0.2272(7) 0.171(7) Uani 0.826(8) 1 d PDU A 1 H15A H 0.1514 1.3847 0.2266 0.256 Uiso 0.826(8) 1 calc PR A 1 H15B H 0.0931 1.3096 0.2454 0.256 Uiso 0.826(8) 1 calc PR A 1 H15C H 0.1178 1.2714 0.1962 0.256 Uiso 0.826(8) 1 calc PR A 1 C16A C 0.2266(4) 1.1700(13) 0.2213(5) 0.141(4) Uani 0.826(8) 1 d PDU A 1 H16A H 0.2466 1.2608 0.2216 0.212 Uiso 0.826(8) 1 calc PR A 1 H16B H 0.2183 1.1429 0.1899 0.212 Uiso 0.826(8) 1 calc PR A 1 H16C H 0.2522 1.0997 0.2354 0.212 Uiso 0.826(8) 1 calc PR A 1 C17A C 0.0738(5) 0.7890(11) 0.1564(3) 0.095(3) Uani 0.826(8) 1 d PDU A 1 H17A H 0.0677 0.8713 0.1361 0.114 Uiso 0.826(8) 1 calc PR A 1 C18A C 0.1273(6) 0.712(2) 0.1369(5) 0.184(7) Uani 0.826(8) 1 d PDU A 1 H18A H 0.1626 0.7713 0.1398 0.275 Uiso 0.826(8) 1 calc PR A 1 H18B H 0.1203 0.6915 0.1049 0.275 Uiso 0.826(8) 1 calc PR A 1 H18C H 0.1335 0.6251 0.1536 0.275 Uiso 0.826(8) 1 calc PR A 1 C19A C 0.0173(6) 0.7091(18) 0.1544(5) 0.153(6) Uani 0.826(8) 1 d PDU A 1 H19A H 0.0103 0.6776 0.1233 0.230 Uiso 0.826(8) 1 calc PR A 1 H19B H -0.0155 0.7692 0.1641 0.230 Uiso 0.826(8) 1 calc PR A 1 H19C H 0.0198 0.6279 0.1745 0.230 Uiso 0.826(8) 1 calc PR A 1 C20A C 0.0820(4) 0.7475(8) 0.3297(3) 0.082(2) Uani 0.826(8) 1 d PDU A 1 H20A H 0.1003 0.7996 0.3555 0.099 Uiso 0.826(8) 1 calc PR A 1 C21A C 0.0155(4) 0.7368(18) 0.3395(6) 0.140(5) Uani 0.826(8) 1 d PDU A 1 H21A H -0.0050 0.8169 0.3260 0.210 Uiso 0.826(8) 1 calc PR A 1 H21B H 0.0090 0.7366 0.3723 0.210 Uiso 0.826(8) 1 calc PR A 1 H21C H -0.0001 0.6502 0.3265 0.210 Uiso 0.826(8) 1 calc PR A 1 C22A C 0.1122(5) 0.6042(10) 0.3275(4) 0.133(4) Uani 0.826(8) 1 d PDU A 1 H22A H 0.1551 0.6158 0.3312 0.200 Uiso 0.826(8) 1 calc PR A 1 H22B H 0.1039 0.5605 0.2982 0.200 Uiso 0.826(8) 1 calc PR A 1 H22C H 0.0970 0.5447 0.3519 0.200 Uiso 0.826(8) 1 calc PR A 1 C24A C 0.4404(3) 0.9039(8) 0.4745(2) 0.066(2) Uani 0.826(8) 1 d PDU A 1 H24A H 0.4460 0.8012 0.4699 0.079 Uiso 0.826(8) 1 calc PR A 1 C25A C 0.4967(3) 0.9753(9) 0.4578(3) 0.078(3) Uani 0.826(8) 1 d PDU A 1 C26A C 0.5392(7) 1.167(2) 0.4180(6) 0.111(5) Uani 0.826(8) 1 d PDU A 1 H26A H 0.5594 1.2098 0.4438 0.166 Uiso 0.826(8) 1 calc PR A 1 H26B H 0.5265 1.2399 0.3969 0.166 Uiso 0.826(8) 1 calc PR A 1 H26C H 0.5663 1.1027 0.4026 0.166 Uiso 0.826(8) 1 calc PR A 1 C27A C 0.4318(4) 0.9276(9) 0.5258(2) 0.081(2) Uani 0.826(8) 1 d PDU A 1 H27A H 0.4689 0.9033 0.5418 0.097 Uiso 0.826(8) 1 calc PR A 1 H27B H 0.4237 1.0277 0.5313 0.097 Uiso 0.826(8) 1 calc PR A 1 C28A C 0.3814(3) 0.8413(5) 0.5453(2) 0.075(2) Uiso 0.826(8) 1 d PGDU A 1 C29A C 0.3276(3) 0.9050(5) 0.5572(3) 0.110(3) Uiso 0.826(8) 1 d PGD A 1 H29A H 0.3232 1.0029 0.5534 0.132 Uiso 0.826(8) 1 d PG A 1 C30A C 0.2803(3) 0.8271(7) 0.5744(3) 0.136(4) Uiso 0.826(8) 1 d PGU A 1 H30A H 0.2446 0.8731 0.5824 0.163 Uiso 0.826(8) 1 d PG A 1 C31A C 0.2850(3) 0.6818(7) 0.5801(3) 0.121(3) Uiso 0.826(8) 1 d PGU A 1 H31A H 0.2531 0.6292 0.5924 0.145 Uiso 0.826(8) 1 d PG A 1 C32A C 0.3375(3) 0.6173(5) 0.5673(3) 0.111(3) Uiso 0.826(8) 1 d PG A 1 H32A H 0.3411 0.5190 0.5701 0.133 Uiso 0.826(8) 1 d PG A 1 C33A C 0.3852(3) 0.6949(5) 0.5502(2) 0.087(2) Uiso 0.826(8) 1 d PGD A 1 H33A H 0.4206 0.6483 0.5419 0.105 Uiso 0.826(8) 1 d PG A 1 N1B N 0.3514(4) 0.4383(10) 0.4261(4) 0.060(3) Uani 0.764(10) 1 d PDU B 2 H1B H 0.3662 0.5213 0.4205 0.072 Uiso 0.764(10) 1 calc PR B 2 O1B O 0.6349(4) 0.6279(15) 0.5164(3) 0.126(4) Uani 0.764(10) 1 d PDU B 2 O2B O 0.3573(4) 0.2411(7) 0.4699(3) 0.059(2) Uani 0.764(10) 1 d PDU B 2 O3B O 0.1930(3) 0.4030(8) 0.4200(5) 0.120(3) Uani 0.764(10) 1 d PDU B 2 O4B O 0.2502(3) 0.5846(9) 0.4393(4) 0.083(3) Uani 0.764(10) 1 d PDU B 2 C1B C 0.6066(6) 0.5814(12) 0.6228(3) 0.079(5) Uani 0.764(10) 1 d PD B 2 C2B C 0.6260(6) 0.5320(13) 0.6654(3) 0.092(3) Uani 0.764(10) 1 d PDU B 2 H2B H 0.6180 0.5866 0.6915 0.110 Uiso 0.764(10) 1 calc PR B 2 C3B C 0.6563(7) 0.4060(14) 0.6705(3) 0.092(3) Uani 0.764(10) 1 d PDU B 2 C4B C 0.6667(8) 0.3252(15) 0.6318(3) 0.090(4) Uani 0.764(10) 1 d PDU B 2 H4B H 0.6876 0.2398 0.6348 0.108 Uiso 0.764(10) 1 calc PR B 2 C5B C 0.6469(7) 0.3670(11) 0.5877(3) 0.072(4) Uani 0.764(10) 1 d PD B 2 C6B C 0.6179(6) 0.4962(10) 0.5841(3) 0.067(7) Uani 0.764(10) 1 d PD B 2 C7B C 0.6011(3) 0.5497(8) 0.5370(2) 0.069(2) Uani 0.764(10) 1 d PDU B 2 C23B C 0.3787(4) 0.3543(10) 0.4563(4) 0.053(3) Uani 0.764(10) 1 d PDU B 2 C11B C 0.4369(2) 0.4077(7) 0.4755(2) 0.053(3) Uiso 0.764(10) 1 d PGDU B 2 C12B C 0.4535(2) 0.3615(6) 0.5193(2) 0.056(2) Uiso 0.764(10) 1 d PGDU B 2 H12B H 0.4284 0.2997 0.5356 0.067 Uiso 0.764(10) 1 d PG B 2 C13B C 0.5064(2) 0.4063(6) 0.53864(17) 0.0571(19) Uiso 0.764(10) 1 d PGDU B 2 H13B H 0.5168 0.3743 0.5680 0.069 Uiso 0.764(10) 1 d PG B 2 C8B C 0.54478(19) 0.4985(6) 0.5156(2) 0.0576(18) Uiso 0.764(10) 1 d PGD B 2 C9B C 0.5285(2) 0.5453(6) 0.47188(19) 0.0525(17) Uiso 0.764(10) 1 d PGD B 2 H9B H 0.5537 0.6070 0.4557 0.063 Uiso 0.764(10) 1 d PG B 2 C10B C 0.4750(2) 0.5003(6) 0.45243(17) 0.053(2) Uiso 0.764(10) 1 d PGDU B 2 H10B H 0.4643 0.5328 0.4232 0.063 Uiso 0.764(10) 1 d PG B 2 C14B C 0.5709(4) 0.7167(10) 0.6196(4) 0.108(3) Uani 0.764(10) 1 d PDU B 2 H14B H 0.5635 0.7366 0.5869 0.129 Uiso 0.764(10) 1 calc PR B 2 C15B C 0.6068(7) 0.8392(13) 0.6393(8) 0.182(8) Uani 0.764(10) 1 d PDU B 2 H15D H 0.5835 0.9254 0.6370 0.273 Uiso 0.764(10) 1 calc PR B 2 H15E H 0.6438 0.8497 0.6224 0.273 Uiso 0.764(10) 1 calc PR B 2 H15F H 0.6158 0.8205 0.6712 0.273 Uiso 0.764(10) 1 calc PR B 2 C16B C 0.5102(4) 0.7067(14) 0.6437(5) 0.125(4) Uani 0.764(10) 1 d PDU B 2 H16D H 0.4916 0.6170 0.6364 0.188 Uiso 0.764(10) 1 calc PR B 2 H16E H 0.4846 0.7831 0.6333 0.188 Uiso 0.764(10) 1 calc PR B 2 H16F H 0.5159 0.7137 0.6765 0.188 Uiso 0.764(10) 1 calc PR B 2 C17B C 0.6735(5) 0.3534(16) 0.7178(4) 0.143(5) Uani 0.764(10) 1 d PDU B 2 H17B H 0.6528 0.4193 0.7387 0.171 Uiso 0.764(10) 1 calc PR B 2 C18B C 0.6471(9) 0.212(2) 0.7293(5) 0.201(10) Uani 0.764(10) 1 d PDU B 2 H18D H 0.6038 0.2191 0.7291 0.302 Uiso 0.764(10) 1 calc PR B 2 H18E H 0.6606 0.1836 0.7594 0.302 Uiso 0.764(10) 1 calc PR B 2 H18F H 0.6599 0.1434 0.7068 0.302 Uiso 0.764(10) 1 calc PR B 2 C19B C 0.7366(5) 0.3736(14) 0.7283(4) 0.128(5) Uani 0.764(10) 1 d PDU B 2 H19D H 0.7531 0.4454 0.7083 0.192 Uiso 0.764(10) 1 calc PR B 2 H19E H 0.7579 0.2856 0.7237 0.192 Uiso 0.764(10) 1 calc PR B 2 H19F H 0.7408 0.4033 0.7598 0.192 Uiso 0.764(10) 1 calc PR B 2 C20B C 0.6629(7) 0.2793(13) 0.5458(4) 0.107(4) Uani 0.764(10) 1 d PDU B 2 H20B H 0.6493 0.3329 0.5186 0.128 Uiso 0.764(10) 1 calc PR B 2 C21B C 0.7292(7) 0.256(2) 0.5403(8) 0.157(7) Uani 0.764(10) 1 d PDU B 2 H21D H 0.7509 0.3310 0.5555 0.236 Uiso 0.764(10) 1 calc PR B 2 H21E H 0.7394 0.2549 0.5081 0.236 Uiso 0.764(10) 1 calc PR B 2 H21F H 0.7401 0.1659 0.5539 0.236 Uiso 0.764(10) 1 calc PR B 2 C22B C 0.6279(7) 0.1397(15) 0.5462(8) 0.158(7) Uani 0.764(10) 1 d PDU B 2 H22D H 0.5856 0.1589 0.5417 0.237 Uiso 0.764(10) 1 calc PR B 2 H22E H 0.6336 0.0930 0.5754 0.237 Uiso 0.764(10) 1 calc PR B 2 H22F H 0.6422 0.0793 0.5218 0.237 Uiso 0.764(10) 1 calc PR B 2 C24B C 0.2974(3) 0.3940(9) 0.4022(3) 0.057(2) Uani 0.764(10) 1 d PDU B 2 H24B H 0.2941 0.2904 0.4055 0.069 Uiso 0.764(10) 1 calc PR B 2 C25B C 0.2407(3) 0.4594(9) 0.4223(3) 0.069(3) Uani 0.764(10) 1 d PDU B 2 C26B C 0.1984(5) 0.6629(11) 0.4565(5) 0.095(4) Uani 0.764(10) 1 d PDU B 2 H26D H 0.1870 0.7345 0.4344 0.142 Uiso 0.764(10) 1 calc PR B 2 H26E H 0.2086 0.7076 0.4853 0.142 Uiso 0.764(10) 1 calc PR B 2 H26F H 0.1652 0.5985 0.4611 0.142 Uiso 0.764(10) 1 calc PR B 2 C27B C 0.3016(4) 0.4278(10) 0.3505(3) 0.069(2) Uani 0.764(10) 1 d PDU B 2 H27C H 0.2645 0.3978 0.3355 0.083 Uiso 0.764(10) 1 calc PR B 2 H27D H 0.3053 0.5301 0.3465 0.083 Uiso 0.764(10) 1 calc PR B 2 C28B C 0.3536(3) 0.3567(7) 0.3277(3) 0.068(3) Uiso 0.764(10) 1 d PGDU B 2 C29B C 0.4068(3) 0.4277(6) 0.3188(3) 0.093(3) Uiso 0.764(10) 1 d PGD B 2 H29B H 0.4102 0.5233 0.3268 0.111 Uiso 0.764(10) 1 d PG B 2 C30B C 0.4548(3) 0.3603(9) 0.2984(4) 0.130(4) Uiso 0.764(10) 1 d PG B 2 H30B H 0.4901 0.4111 0.2925 0.156 Uiso 0.764(10) 1 d PG B 2 C31B C 0.4516(3) 0.2185(10) 0.2864(4) 0.136(4) Uiso 0.764(10) 1 d PG B 2 H31B H 0.4839 0.1732 0.2720 0.164 Uiso 0.764(10) 1 d PG B 2 C32B C 0.3997(4) 0.1464(7) 0.2962(4) 0.122(4) Uiso 0.764(10) 1 d PGU B 2 H32B H 0.3970 0.0499 0.2891 0.147 Uiso 0.764(10) 1 d PG B 2 C33B C 0.3513(3) 0.2136(7) 0.3163(3) 0.099(3) Uiso 0.764(10) 1 d PGDU B 2 H33B H 0.3163 0.1620 0.3224 0.119 Uiso 0.764(10) 1 d PG B 2 N1C N 0.3779(14) 0.944(4) 0.4559(12) 0.069(10) Uiso 0.174(8) 1 d PDU A 3 H1C H 0.3579 1.0200 0.4624 0.083 Uiso 0.174(8) 1 calc PR A 3 O1C O 0.1140(12) 1.150(3) 0.3454(10) 0.078(11) Uiso 0.174(8) 1 d PDU A 3 O2C O 0.373(2) 0.735(4) 0.4175(16) 0.062(13) Uiso 0.174(8) 1 d PDU A 3 O3C O 0.5276(15) 1.007(5) 0.4977(12) 0.149(14) Uiso 0.174(8) 1 d PDU A 3 O4C O 0.4869(19) 1.054(5) 0.4302(11) 0.075(9) Uiso 0.174(8) 1 d PDU A 3 C1C C 0.135(2) 1.015(4) 0.2466(7) 0.073(9) Uiso 0.174(8) 1 d PDU A 3 C2C C 0.118(3) 0.955(5) 0.2055(8) 0.090(10) Uiso 0.174(8) 1 d PDU A 3 H2C H 0.1291 0.9945 0.1773 0.108 Uiso 0.174(8) 1 calc PR A 3 C3C C 0.083(3) 0.833(5) 0.2080(9) 0.080(10) Uiso 0.174(8) 1 d PDU A 3 C4C C 0.067(3) 0.778(4) 0.2499(10) 0.072(10) Uiso 0.174(8) 1 d PDU A 3 H4C H 0.0437 0.6952 0.2504 0.087 Uiso 0.174(8) 1 calc PR A 3 C5C C 0.084(2) 0.839(4) 0.2922(8) 0.066(10) Uiso 0.174(8) 1 d PDU A 3 C6C C 0.1192(15) 0.959(3) 0.2881(7) 0.068(10) Uiso 0.174(8) 1 d PDU A 3 C7C C 0.1527(8) 1.069(2) 0.3169(6) 0.083(9) Uiso 0.174(8) 1 d PDU A 3 C23C C 0.359(2) 0.862(4) 0.4208(16) 0.054(10) Uiso 0.174(8) 1 d PDU A 3 C11C C 0.3068(9) 0.921(3) 0.3945(7) 0.035(9) Uiso 0.174(8) 1 d PGDU A 3 C12C C 0.2961(9) 0.875(2) 0.3502(7) 0.061(12) Uiso 0.174(8) 1 d PGD A 3 H12C H 0.3228 0.8110 0.3365 0.073 Uiso 0.174(8) 1 d PG A 3 C13C C 0.2470(9) 0.921(2) 0.3262(6) 0.058(8) Uiso 0.174(8) 1 d PGDU A 3 H13C H 0.2412 0.8886 0.2961 0.070 Uiso 0.174(8) 1 d PG A 3 C8C C 0.2055(7) 1.013(2) 0.3454(6) 0.031(5) Uiso 0.174(8) 1 d PGDU A 3 C9C C 0.2182(8) 1.066(2) 0.3881(6) 0.046(7) Uiso 0.174(8) 1 d PGDU A 3 H9C H 0.1928 1.1341 0.4011 0.055 Uiso 0.174(8) 1 d PG A 3 C10C C 0.2682(9) 1.021(2) 0.4125(6) 0.055(9) Uiso 0.174(8) 1 d PGDU A 3 H10C H 0.2758 1.0585 0.4416 0.066 Uiso 0.174(8) 1 d PG A 3 C14C C 0.1648(12) 1.147(3) 0.2665(8) 0.101(10) Uiso 0.174(8) 1 d PDU A 3 C15C C 0.126(2) 1.281(4) 0.2618(16) 0.17(2) Uiso 0.174(8) 1 d PDU A 3 H15G H 0.0860 1.2617 0.2727 0.261 Uiso 0.174(8) 1 calc PR A 3 H15H H 0.1245 1.3092 0.2299 0.261 Uiso 0.174(8) 1 calc PR A 3 H15I H 0.1435 1.3567 0.2797 0.261 Uiso 0.174(8) 1 calc PR A 3 C16C C 0.2275(14) 1.174(4) 0.2495(12) 0.090(12) Uiso 0.174(8) 1 d PDU A 3 H16G H 0.2511 1.0891 0.2527 0.135 Uiso 0.174(8) 1 calc PR A 3 H16H H 0.2455 1.2494 0.2674 0.135 Uiso 0.174(8) 1 calc PR A 3 H16I H 0.2261 1.2019 0.2176 0.135 Uiso 0.174(8) 1 calc PR A 3 C17C C 0.060(2) 0.762(4) 0.1633(10) 0.098(11) Uiso 0.174(8) 1 d PDU A 3 H17C H 0.0650 0.8323 0.1384 0.118 Uiso 0.174(8) 1 calc PR A 3 C18C C 0.099(2) 0.639(5) 0.152(2) 0.122(16) Uiso 0.174(8) 1 d PDU A 3 H18G H 0.1410 0.6682 0.1524 0.183 Uiso 0.174(8) 1 calc PR A 3 H18H H 0.0894 0.6056 0.1212 0.183 Uiso 0.174(8) 1 calc PR A 3 H18I H 0.0929 0.5644 0.1736 0.183 Uiso 0.174(8) 1 calc PR A 3 C19C C -0.0034(19) 0.724(9) 0.166(3) 0.147(19) Uiso 0.174(8) 1 d PDU A 3 H19G H -0.0267 0.8065 0.1738 0.221 Uiso 0.174(8) 1 calc PR A 3 H19H H -0.0091 0.6510 0.1884 0.221 Uiso 0.174(8) 1 calc PR A 3 H19I H -0.0164 0.6894 0.1360 0.221 Uiso 0.174(8) 1 calc PR A 3 C20C C 0.0595(18) 0.783(4) 0.3378(10) 0.093(10) Uiso 0.174(8) 1 d PDU A 3 H20C H 0.0584 0.8626 0.3599 0.112 Uiso 0.174(8) 1 calc PR A 3 C21C C -0.0037(18) 0.725(8) 0.333(2) 0.145(19) Uiso 0.174(8) 1 d PDU A 3 H21G H -0.0325 0.8001 0.3369 0.218 Uiso 0.174(8) 1 calc PR A 3 H21H H -0.0103 0.6528 0.3561 0.218 Uiso 0.174(8) 1 calc PR A 3 H21I H -0.0084 0.6834 0.3028 0.218 Uiso 0.174(8) 1 calc PR A 3 C22C C 0.100(3) 0.668(6) 0.357(2) 0.157(18) Uiso 0.174(8) 1 d PDU A 3 H22G H 0.0868 0.6421 0.3872 0.236 Uiso 0.174(8) 1 calc PR A 3 H22H H 0.1410 0.7036 0.3586 0.236 Uiso 0.174(8) 1 calc PR A 3 H22I H 0.0990 0.5866 0.3370 0.236 Uiso 0.174(8) 1 calc PR A 3 C24C C 0.4300(11) 0.911(4) 0.4830(8) 0.079(10) Uiso 0.174(8) 1 d PDU A 3 H24C H 0.4394 0.8111 0.4767 0.095 Uiso 0.174(8) 1 calc PR A 3 C25C C 0.4857(13) 0.993(6) 0.4709(9) 0.081(10) Uiso 0.174(8) 1 d PDU A 3 C26C C 0.538(4) 1.142(11) 0.420(2) 0.102(17) Uiso 0.174(8) 1 d PDU A 3 C27C C 0.4165(15) 0.919(4) 0.5344(8) 0.084(10) Uiso 0.174(8) 1 d PDU A 3 H27E H 0.4529 0.8938 0.5513 0.101 Uiso 0.174(8) 1 calc PR A 3 H27F H 0.4070 1.0176 0.5421 0.101 Uiso 0.174(8) 1 calc PR A 3 C28C C 0.3666(9) 0.828(2) 0.5506(7) 0.043(7) Uiso 0.174(8) 1 d PGDU A 3 C29C C 0.3263(10) 0.878(2) 0.5827(9) 0.087(11) Uiso 0.174(8) 1 d PGD A 3 H29C H 0.3303 0.9700 0.5940 0.105 Uiso 0.174(8) 1 d PG A 3 C30C C 0.2799(10) 0.793(3) 0.5984(10) 0.086(9) Uiso 0.174(8) 1 d PGU A 3 H30C H 0.2539 0.8273 0.6209 0.103 Uiso 0.174(8) 1 d PG A 3 C31C C 0.2714(12) 0.658(3) 0.5813(12) 0.181(18) Uiso 0.174(8) 1 d PGU A 3 H31C H 0.2395 0.6016 0.5915 0.217 Uiso 0.174(8) 1 d PG A 3 C32C C 0.3111(16) 0.609(2) 0.5488(12) 0.109(14) Uiso 0.174(8) 1 d PG A 3 H32C H 0.3061 0.5177 0.5367 0.131 Uiso 0.174(8) 1 d PG A 3 C33C C 0.3584(14) 0.692(2) 0.5339(9) 0.111(14) Uiso 0.174(8) 1 d PGD A 3 H33C H 0.3853 0.6557 0.5121 0.133 Uiso 0.174(8) 1 d PG A 3 N1D N 0.3580(13) 0.446(4) 0.4243(11) 0.059(8) Uiso 0.236(10) 1 d PDU B 4 H1D H 0.3747 0.5272 0.4188 0.071 Uiso 0.236(10) 1 calc PR B 4 O1D O 0.6228(11) 0.684(3) 0.5274(9) 0.112(12) Uiso 0.236(10) 1 d PDU B 4 O2D O 0.3683(13) 0.235(3) 0.4591(12) 0.073(11) Uiso 0.236(10) 1 d PDU B 4 O3D O 0.2003(9) 0.449(3) 0.3968(9) 0.103(9) Uiso 0.236(10) 1 d PDU B 4 O4D O 0.2555(14) 0.561(4) 0.4500(11) 0.086(9) Uiso 0.236(10) 1 d PDU B 4 C1D C 0.6050(16) 0.559(3) 0.6270(6) 0.068(14) Uiso 0.236(10) 1 d PD B 4 C2D C 0.6187(19) 0.506(4) 0.6696(7) 0.090(9) Uiso 0.236(10) 1 d PDU B 4 H2D H 0.6048 0.5481 0.6967 0.109 Uiso 0.236(10) 1 calc PR B 4 C3D C 0.654(2) 0.384(4) 0.6702(8) 0.097(9) Uiso 0.236(10) 1 d PDU B 4 C4D C 0.674(2) 0.325(4) 0.6300(9) 0.092(9) Uiso 0.236(10) 1 d PDU B 4 H4D H 0.6979 0.2440 0.6318 0.110 Uiso 0.236(10) 1 calc PR B 4 C5D C 0.6605(17) 0.379(3) 0.5859(8) 0.077(19) Uiso 0.236(10) 1 d PD B 4 C6D C 0.6235(13) 0.498(3) 0.5869(7) 0.07(2) Uiso 0.236(10) 1 d PD B 4 C7D C 0.5871(7) 0.5958(18) 0.5559(5) 0.086(8) Uiso 0.236(10) 1 d PDU B 4 C23D C 0.3823(16) 0.362(4) 0.4570(14) 0.064(9) Uiso 0.236(10) 1 d PDU B 4 C11D C 0.4369(7) 0.4190(19) 0.4806(6) 0.037(8) Uiso 0.236(10) 1 d PGDU B 4 C12D C 0.4491(7) 0.3774(18) 0.5252(6) 0.076(11) Uiso 0.236(10) 1 d PGDU B 4 H12D H 0.4242 0.3107 0.5395 0.091 Uiso 0.236(10) 1 d PG B 4 C13D C 0.4969(7) 0.4323(17) 0.5487(5) 0.050(6) Uiso 0.236(10) 1 d PGDU B 4 H13D H 0.5036 0.4035 0.5790 0.060 Uiso 0.236(10) 1 d PG B 4 C8D C 0.5357(6) 0.5299(16) 0.5287(5) 0.045(5) Uiso 0.236(10) 1 d PGD B 4 C9D C 0.5213(6) 0.5774(16) 0.4856(5) 0.047(5) Uiso 0.236(10) 1 d PGD B 4 H9D H 0.5448 0.6481 0.4720 0.057 Uiso 0.236(10) 1 d PG B 4 C10D C 0.4726(7) 0.5227(18) 0.4618(5) 0.049(6) Uiso 0.236(10) 1 d PGDU B 4 H10D H 0.4639 0.5570 0.4324 0.059 Uiso 0.236(10) 1 d PG B 4 C14D C 0.5678(10) 0.677(2) 0.6044(7) 0.103(9) Uiso 0.236(10) 1 d PDU B 4 C15D C 0.5972(17) 0.824(2) 0.6070(11) 0.112(12) Uiso 0.236(10) 1 d PDU B 4 H15J H 0.6375 0.8187 0.5947 0.169 Uiso 0.236(10) 1 calc PR B 4 H15K H 0.5988 0.8544 0.6386 0.169 Uiso 0.236(10) 1 calc PR B 4 H15L H 0.5739 0.8904 0.5892 0.169 Uiso 0.236(10) 1 calc PR B 4 C16D C 0.5031(11) 0.685(4) 0.6186(12) 0.129(15) Uiso 0.236(10) 1 d PDU B 4 H16J H 0.4857 0.5913 0.6182 0.193 Uiso 0.236(10) 1 calc PR B 4 H16K H 0.4815 0.7454 0.5975 0.193 Uiso 0.236(10) 1 calc PR B 4 H16L H 0.5004 0.7239 0.6492 0.193 Uiso 0.236(10) 1 calc PR B 4 C17D C 0.6815(17) 0.335(4) 0.7162(9) 0.150(10) Uiso 0.236(10) 1 d PDU B 4 H17D H 0.6914 0.4217 0.7333 0.180 Uiso 0.236(10) 1 calc PR B 4 C18D C 0.636(2) 0.260(8) 0.7444(18) 0.19(2) Uiso 0.236(10) 1 d PDU B 4 H18J H 0.5964 0.2843 0.7335 0.284 Uiso 0.236(10) 1 calc PR B 4 H18K H 0.6402 0.2890 0.7761 0.284 Uiso 0.236(10) 1 calc PR B 4 H18L H 0.6421 0.1593 0.7420 0.284 Uiso 0.236(10) 1 calc PR B 4 C19D C 0.7384(18) 0.260(6) 0.7101(17) 0.170(16) Uiso 0.236(10) 1 d PDU B 4 H19J H 0.7709 0.3283 0.7098 0.255 Uiso 0.236(10) 1 calc PR B 4 H19K H 0.7378 0.2093 0.6813 0.255 Uiso 0.236(10) 1 calc PR B 4 H19L H 0.7443 0.1945 0.7351 0.255 Uiso 0.236(10) 1 calc PR B 4 C20D C 0.666(2) 0.280(4) 0.5447(10) 0.110(10) Uiso 0.236(10) 1 d PDU B 4 H20D H 0.6378 0.3101 0.5205 0.132 Uiso 0.236(10) 1 calc PR B 4 C21D C 0.730(3) 0.281(7) 0.526(2) 0.153(19) Uiso 0.236(10) 1 d PDU B 4 H21J H 0.7445 0.3772 0.5253 0.230 Uiso 0.236(10) 1 calc PR B 4 H21K H 0.7296 0.2432 0.4950 0.230 Uiso 0.236(10) 1 calc PR B 4 H21L H 0.7551 0.2237 0.5451 0.230 Uiso 0.236(10) 1 calc PR B 4 C22D C 0.651(3) 0.129(4) 0.559(2) 0.140(17) Uiso 0.236(10) 1 d PDU B 4 H22J H 0.6094 0.1230 0.5680 0.210 Uiso 0.236(10) 1 calc PR B 4 H22K H 0.6760 0.1030 0.5854 0.210 Uiso 0.236(10) 1 calc PR B 4 H22L H 0.6590 0.0648 0.5343 0.210 Uiso 0.236(10) 1 calc PR B 4 C24D C 0.3057(9) 0.407(3) 0.3981(7) 0.069(9) Uiso 0.236(10) 1 d PDU B 4 H24D H 0.2990 0.3050 0.4028 0.083 Uiso 0.236(10) 1 calc PR B 4 C25D C 0.2491(9) 0.483(4) 0.4128(10) 0.081(9) Uiso 0.236(10) 1 d PDU B 4 C26D C 0.204(2) 0.630(5) 0.4696(15) 0.105(15) Uiso 0.236(10) 1 d PDU B 4 C27D C 0.3161(12) 0.431(3) 0.3463(8) 0.070(8) Uiso 0.236(10) 1 d PDU B 4 H27G H 0.2790 0.4098 0.3298 0.084 Uiso 0.236(10) 1 calc PR B 4 H27H H 0.3260 0.5301 0.3411 0.084 Uiso 0.236(10) 1 calc PR B 4 C28D C 0.3652(9) 0.3409(19) 0.3276(8) 0.067(8) Uiso 0.236(10) 1 d PGDU B 4 C29D C 0.4166(10) 0.3990(18) 0.3091(10) 0.112(12) Uiso 0.236(10) 1 d PGD B 4 H29D H 0.4204 0.4976 0.3071 0.134 Uiso 0.236(10) 1 d PG B 4 C30D C 0.4628(9) 0.313(2) 0.2936(10) 0.105(11) Uiso 0.236(10) 1 d PG B 4 H30D H 0.4967 0.3546 0.2802 0.126 Uiso 0.236(10) 1 d PG B 4 C31D C 0.4597(8) 0.168(2) 0.2975(9) 0.102(10) Uiso 0.236(10) 1 d PG B 4 H31D H 0.4914 0.1104 0.2876 0.122 Uiso 0.236(10) 1 d PG B 4 C32D C 0.4088(10) 0.1098(17) 0.3165(9) 0.082(7) Uiso 0.236(10) 1 d PGU B 4 H32D H 0.4058 0.0113 0.3196 0.099 Uiso 0.236(10) 1 d PG B 4 C33D C 0.3619(9) 0.195(2) 0.3310(8) 0.086(8) Uiso 0.236(10) 1 d PGDU B 4 H33D H 0.3274 0.1530 0.3434 0.103 Uiso 0.236(10) 1 d PG B 4 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 N1A 0.059(3) 0.046(3) 0.076(4) 0.005(3) -0.015(3) 0.005(3) O1A 0.081(4) 0.136(7) 0.126(6) -0.062(6) -0.035(4) 0.044(5) O2A 0.066(4) 0.052(3) 0.082(6) -0.006(3) 0.006(4) 0.003(3) O3A 0.056(4) 0.137(6) 0.278(12) 0.059(7) -0.027(5) -0.001(4) O4A 0.085(4) 0.067(5) 0.116(5) 0.007(4) 0.027(3) 0.001(3) C1A 0.078(5) 0.066(5) 0.076(5) -0.002(4) -0.020(4) -0.004(4) C2A 0.091(6) 0.087(6) 0.069(5) 0.014(4) -0.015(4) 0.002(5) C3A 0.087(6) 0.073(5) 0.058(4) -0.004(4) -0.021(4) -0.006(4) C4A 0.091(7) 0.076(4) 0.060(5) -0.008(4) -0.008(4) -0.012(4) C5A 0.068(6) 0.086(5) 0.057(4) 0.003(4) -0.005(4) -0.003(4) C6A 0.057(4) 0.067(4) 0.073(5) -0.009(4) -0.014(3) 0.007(3) C7A 0.056(4) 0.066(4) 0.063(4) -0.012(3) -0.004(3) 0.011(3) C23A 0.056(4) 0.043(4) 0.061(4) -0.001(3) 0.002(3) -0.005(3) C14A 0.097(6) 0.088(5) 0.108(7) 0.009(5) -0.004(5) -0.028(5) C15A 0.136(10) 0.076(6) 0.30(2) 0.023(9) 0.008(11) -0.010(6) C16A 0.117(9) 0.136(9) 0.172(13) 0.015(9) -0.003(8) -0.034(7) C17A 0.111(7) 0.107(6) 0.067(5) -0.001(5) -0.023(5) -0.002(6) C18A 0.220(16) 0.232(16) 0.098(9) -0.067(11) -0.040(10) 0.066(14) C19A 0.200(14) 0.161(11) 0.099(9) 0.010(8) -0.065(10) -0.071(12) C20A 0.086(5) 0.100(6) 0.060(5) 0.005(4) 0.005(4) 0.001(4) C21A 0.103(8) 0.174(11) 0.143(11) 0.059(9) 0.035(8) 0.016(9) C22A 0.168(10) 0.124(8) 0.108(8) 0.056(7) 0.025(7) 0.040(7) C24A 0.063(4) 0.056(4) 0.079(5) 0.004(4) -0.013(4) 0.000(3) C25A 0.057(4) 0.072(5) 0.106(7) -0.012(5) 0.001(4) -0.009(4) C26A 0.087(6) 0.079(9) 0.167(11) -0.004(6) 0.052(7) -0.018(5) C27A 0.087(6) 0.075(4) 0.081(6) -0.009(4) -0.022(4) 0.006(4) N1B 0.055(4) 0.043(3) 0.082(5) 0.002(3) -0.011(3) -0.001(3) O1B 0.092(5) 0.176(10) 0.111(6) 0.076(7) -0.044(5) -0.075(7) O2B 0.056(3) 0.047(3) 0.074(5) 0.001(3) 0.004(4) -0.004(2) O3B 0.061(4) 0.088(4) 0.210(10) -0.027(6) 0.014(5) -0.017(3) O4B 0.069(4) 0.074(4) 0.108(6) -0.011(5) 0.026(4) 0.003(3) C1B 0.075(7) 0.090(7) 0.073(7) 0.002(5) 0.003(4) -0.005(5) C2B 0.102(7) 0.116(8) 0.057(5) -0.005(5) 0.000(5) -0.011(7) C3B 0.097(6) 0.122(8) 0.057(5) 0.017(5) -0.024(5) -0.005(6) C4B 0.087(7) 0.094(6) 0.088(7) 0.028(5) -0.010(5) 0.026(5) C5B 0.069(6) 0.091(8) 0.057(6) 0.005(4) -0.004(4) -0.007(6) C6B 0.057(6) 0.084(10) 0.059(7) 0.024(4) -0.011(4) -0.002(4) C7B 0.069(5) 0.072(4) 0.068(5) 0.020(4) -0.002(4) -0.009(4) C23B 0.053(4) 0.042(4) 0.064(5) -0.008(3) 0.005(3) 0.009(3) C14B 0.119(8) 0.099(7) 0.105(7) 0.001(6) 0.011(6) 0.016(6) C15B 0.153(12) 0.104(9) 0.29(2) -0.008(11) -0.002(14) -0.003(8) C16B 0.087(7) 0.149(10) 0.139(12) 0.004(9) 0.013(7) 0.036(6) C17B 0.152(10) 0.202(12) 0.074(6) 0.044(8) -0.029(7) 0.014(9) C18B 0.250(17) 0.26(2) 0.089(10) 0.103(14) -0.070(11) -0.091(16) C19B 0.126(8) 0.153(10) 0.104(8) 0.037(7) -0.068(7) -0.030(7) C20B 0.136(9) 0.106(7) 0.078(6) -0.006(5) -0.004(6) 0.023(6) C21B 0.123(10) 0.204(15) 0.145(16) -0.053(13) 0.040(10) -0.019(10) C22B 0.139(13) 0.125(10) 0.211(18) -0.059(11) 0.023(13) -0.002(8) C24B 0.051(4) 0.046(4) 0.075(5) 0.000(3) -0.016(4) -0.006(3) C25B 0.063(5) 0.058(5) 0.088(6) 0.003(5) -0.012(4) 0.003(4) C26B 0.081(6) 0.071(6) 0.132(10) 0.003(6) 0.048(7) 0.023(5) C27B 0.053(5) 0.073(5) 0.082(6) 0.009(4) -0.015(4) 0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1A C23A 1.327(6) . ? N1A C24A 1.443(6) . ? N1A H1A 0.8600 . ? O1A C7A 1.205(6) . ? O2A C23A 1.228(6) . ? O3A C25A 1.182(7) . ? O4A C25A 1.287(7) . ? O4A C26A 1.442(7) . ? C1A C2A 1.387(7) . ? C1A C6A 1.391(7) . ? C1A C14A 1.496(7) . ? C2A C3A 1.359(7) . ? C2A H2A 0.9300 . ? C3A C4A 1.380(7) . ? C3A C17A 1.506(7) . ? C4A C5A 1.404(7) . ? C4A H4A 0.9300 . ? C5A C6A 1.379(7) . ? C5A C20A 1.520(7) . ? C6A C7A 1.506(7) . ? C7A C8A 1.473(5) . ? C23A C11A 1.482(5) . ? C11A C10A 1.3820 . ? C11A C12A 1.3913 . ? C12A C13A 1.3616 . ? C12A H12A 0.9300 . ? C13A C8A 1.3834 . ? C13A H13A 0.9300 . ? C8A C9A 1.3878 . ? C9A C10A 1.3758 . ? C9A H9A 0.9301 . ? C10A H10A 0.9300 . ? C14A C15A 1.515(9) . ? C14A C16A 1.521(9) . ? C14A H14A 0.9800 . ? C15A H15A 0.9600 . ? C15A H15B 0.9600 . ? C15A H15C 0.9600 . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C17A C19A 1.460(8) . ? C17A C18A 1.495(8) . ? C17A H17A 0.9800 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C19A H19A 0.9600 . ? C19A H19B 0.9600 . ? C19A H19C 0.9600 . ? C20A C21A 1.502(8) . ? C20A C22A 1.502(8) . ? C20A H20A 0.9800 . ? C21A H21A 0.9600 . ? C21A H21B 0.9600 . ? C21A H21C 0.9600 . ? C22A H22A 0.9600 . ? C22A H22B 0.9600 . ? C22A H22C 0.9600 . ? C24A C25A 1.494(7) . ? C24A C27A 1.514(7) . ? C24A H24A 0.9800 . ? C26A H26A 0.9600 . ? C26A H26B 0.9600 . ? C26A H26C 0.9600 . ? C27A C28A 1.488(7) . ? C27A H27A 0.9700 . ? C27A H27B 0.9700 . ? C28A C29A 1.3754 . ? C28A C33A 1.3831 . ? C29A C30A 1.3702 . ? C29A H29A 0.9300 . ? C30A C31A 1.3771 . ? C30A H30A 0.9300 . ? C31A C32A 1.3617 . ? C31A H31A 0.9300 . ? C32A C33A 1.3726 . ? C32A H32A 0.9300 . ? C33A H33A 0.9300 . ? N1B C23B 1.323(6) . ? N1B C24B 1.439(7) . ? N1B H1B 0.8600 . ? O1B C7B 1.204(6) . ? O2B C23B 1.227(7) . ? O3B C25B 1.181(7) . ? O4B C25B 1.292(7) . ? O4B C26B 1.449(7) . ? C1B C2B 1.385(8) . ? C1B C6B 1.399(7) . ? C1B C14B 1.499(8) . ? C2B C3B 1.367(8) . ? C2B H2B 0.9300 . ? C3B C4B 1.372(8) . ? C3B C17B 1.504(8) . ? C4B C5B 1.405(7) . ? C4B H4B 0.9300 . ? C5B C6B 1.375(7) . ? C5B C20B 1.508(8) . ? C6B C7B 1.499(7) . ? C7B C8B 1.472(6) . ? C23B C11B 1.489(6) . ? C11B C10B 1.3819 . ? C11B C12B 1.3912 . ? C12B C13B 1.3615 . ? C12B H12B 0.9300 . ? C13B C8B 1.3834 . ? C13B H13B 0.9301 . ? C8B C9B 1.3878 . ? C9B C10B 1.3759 . ? C9B H9B 0.9300 . ? C10B H10B 0.9300 . ? C14B C15B 1.509(9) . ? C14B C16B 1.515(8) . ? C14B H14B 0.9800 . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? C17B C19B 1.440(9) . ? C17B C18B 1.484(9) . ? C17B H17B 0.9800 . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? C19B H19D 0.9600 . ? C19B H19E 0.9600 . ? C19B H19F 0.9600 . ? C20B C21B 1.492(9) . ? C20B C22B 1.521(9) . ? C20B H20B 0.9800 . ? C21B H21D 0.9600 . ? C21B H21E 0.9600 . ? C21B H21F 0.9600 . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? C24B C25B 1.513(7) . ? C24B C27B 1.533(7) . ? C24B H24B 0.9800 . ? C26B H26D 0.9600 . ? C26B H26E 0.9600 . ? C26B H26F 0.9600 . ? C27B C28B 1.485(7) . ? C27B H27C 0.9700 . ? C27B H27D 0.9700 . ? C28B C29B 1.3754 . ? C28B C33B 1.3831 . ? C29B C30B 1.3702 . ? C29B H29B 0.9300 . ? C30B C31B 1.3770 . ? C30B H30B 0.9300 . ? C31B C32B 1.3617 . ? C31B H31B 0.9300 . ? C32B C33B 1.3726 . ? C32B H32B 0.9300 . ? C33B H33B 0.9300 . ? N1C C23C 1.346(10) . ? N1C C24C 1.427(10) . ? N1C H1C 0.8600 . ? O1C C7C 1.411(10) . ? O2C C23C 1.234(10) . ? O3C C25C 1.218(10) . ? O4C C25C 1.311(10) . ? O4C C26C 1.436(11) . ? C1C C6C 1.353(9) . ? C1C C2C 1.367(9) . ? C1C C14C 1.525(9) . ? C2C C3C 1.382(9) . ? C2C H2C 0.9300 . ? C3C C4C 1.365(9) . ? C3C C17C 1.537(9) . ? C4C C5C 1.402(9) . ? C4C H4C 0.9300 . ? C5C C6C 1.381(9) . ? C5C C20C 1.515(9) . ? C6C C7C 1.520(9) . ? C7C C8C 1.522(8) . ? C7C C14C 1.654(10) . ? C23C C11C 1.484(8) . ? C11C C10C 1.3672 . ? C11C C12C 1.3750 . ? C12C C13C 1.3582 . ? C12C H12C 0.9300 . ? C13C C8C 1.3818 . ? C13C H13C 0.9300 . ? C8C C9C 1.3608 . ? C9C C10C 1.3794 . ? C9C H9C 0.9300 . ? C10C H10C 0.9300 . ? C14C C16C 1.492(9) . ? C14C C15C 1.526(10) . ? C15C H15G 0.9600 . ? C15C H15H 0.9600 . ? C15C H15I 0.9600 . ? C16C H16G 0.9600 . ? C16C H16H 0.9600 . ? C16C H16I 0.9600 . ? C17C C19C 1.459(11) . ? C17C C18C 1.477(10) . ? C17C H17C 0.9800 . ? C18C H18G 0.9600 . ? C18C H18H 0.9600 . ? C18C H18I 0.9600 . ? C19C H19G 0.9600 . ? C19C H19H 0.9600 . ? C19C H19I 0.9600 . ? C20C C21C 1.508(11) . ? C20C C22C 1.512(10) . ? C20C H20C 0.9800 . ? C21C H21G 0.9600 . ? C21C H21H 0.9600 . ? C21C H21I 0.9600 . ? C22C H22G 0.9600 . ? C22C H22H 0.9600 . ? C22C H22I 0.9600 . ? C24C C25C 1.490(10) . ? C24C C27C 1.520(10) . ? C24C H24C 0.9800 . ? C27C C28C 1.477(9) . ? C27C H27E 0.9700 . ? C27C H27F 0.9700 . ? C28C C29C 1.3688 . ? C28C C33C 1.3759 . ? C29C C30C 1.3762 . ? C29C H29C 0.9300 . ? C30C C31C 1.3693 . ? C30C H30C 0.9300 . ? C31C C32C 1.3674 . ? C31C H31C 0.9300 . ? C32C C33C 1.3743 . ? C32C H32C 0.9300 . ? C33C H33C 0.9300 . ? N1D C23D 1.344(10) . ? N1D C24D 1.430(10) . ? N1D H1D 0.8600 . ? O1D C7D 1.408(9) . ? O2D C23D 1.235(10) . ? O3D C25D 1.218(10) . ? O4D C25D 1.310(10) . ? O4D C26D 1.433(10) . ? C1D C6D 1.358(9) . ? C1D C2D 1.366(9) . ? C1D C14D 1.524(9) . ? C2D C3D 1.383(9) . ? C2D H2D 0.9300 . ? C3D C4D 1.362(9) . ? C3D C17D 1.535(9) . ? C4D C5D 1.404(9) . ? C4D H4D 0.9300 . ? C5D C6D 1.382(9) . ? C5D C20D 1.519(10) . ? C6D C7D 1.514(9) . ? C7D C8D 1.516(8) . ? C7D C14D 1.652(10) . ? C23D C11D 1.487(8) . ? C11D C10D 1.3671 . ? C11D C12D 1.3750 . ? C12D C13D 1.3582 . ? C12D H12D 0.9300 . ? C13D C8D 1.3817 . ? C13D H13D 0.9300 . ? C8D C9D 1.3608 . ? C9D C10D 1.3794 . ? C9D H9D 0.9300 . ? C10D H10D 0.9300 . ? C14D C16D 1.492(9) . ? C14D C15D 1.527(10) . ? C15D H15J 0.9600 . ? C15D H15K 0.9600 . ? C15D H15L 0.9600 . ? C16D H16J 0.9600 . ? C16D H16K 0.9600 . ? C16D H16L 0.9600 . ? C17D C19D 1.450(10) . ? C17D C18D 1.469(10) . ? C17D H17D 0.9800 . ? C18D H18J 0.9600 . ? C18D H18K 0.9600 . ? C18D H18L 0.9600 . ? C19D H19J 0.9600 . ? C19D H19K 0.9600 . ? C19D H19L 0.9600 . ? C20D C21D 1.509(10) . ? C20D C22D 1.517(10) . ? C20D H20D 0.9800 . ? C21D H21J 0.9600 . ? C21D H21K 0.9600 . ? C21D H21L 0.9600 . ? C22D H22J 0.9600 . ? C22D H22K 0.9600 . ? C22D H22L 0.9600 . ? C24D C25D 1.502(10) . ? C24D C27D 1.531(10) . ? C24D H24D 0.9800 . ? C27D C28D 1.478(9) . ? C27D H27G 0.9700 . ? C27D H27H 0.9700 . ? C28D C29D 1.3688 . ? C28D C33D 1.3759 . ? C29D C30D 1.3762 . ? C29D H29B 1.2816 . ? C29D H29D 0.9300 . ? C30D C31D 1.3694 . ? C30D H30B 1.0994 . ? C30D H31B 1.5277 . ? C30D H30D 0.9300 . ? C31D C32D 1.3674 . ? C31D H31B 0.9138 . ? C31D H31D 0.9300 . ? C32D C33D 1.3743 . ? C32D H32B 1.0073 . ? C32D H32D 0.9300 . ? C33D H33B 1.0834 . ? C33D H33D 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23A N1A C24A 122.3(5) . . ? C23A N1A H1A 118.8 . . ? C24A N1A H1A 118.8 . . ? C25A O4A C26A 117.3(9) . . ? C2A C1A C6A 117.0(5) . . ? C2A C1A C14A 119.7(6) . . ? C6A C1A C14A 123.2(6) . . ? C3A C2A C1A 123.6(6) . . ? C3A C2A H2A 118.2 . . ? C1A C2A H2A 118.2 . . ? C2A C3A C4A 118.3(5) . . ? C2A C3A C17A 121.1(6) . . ? C4A C3A C17A 120.6(6) . . ? C3A C4A C5A 120.6(6) . . ? C3A C4A H4A 119.7 . . ? C5A C4A H4A 119.7 . . ? C6A C5A C4A 119.0(5) . . ? C6A C5A C20A 121.4(6) . . ? C4A C5A C20A 119.6(6) . . ? C5A C6A C1A 121.3(5) . . ? C5A C6A C7A 118.0(6) . . ? C1A C6A C7A 120.7(6) . . ? O1A C7A C8A 119.6(5) . . ? O1A C7A C6A 120.7(5) . . ? C8A C7A C6A 119.6(5) . . ? O2A C23A N1A 121.8(6) . . ? O2A C23A C11A 121.2(5) . . ? N1A C23A C11A 116.8(5) . . ? C10A C11A C12A 118.3 . . ? C10A C11A C23A 124.4(4) . . ? C12A C11A C23A 117.2(4) . . ? C13A C12A C11A 120.3 . . ? C12A C13A C8A 121.5 . . ? C13A C8A C9A 118.5 . . ? C13A C8A C7A 121.3(3) . . ? C9A C8A C7A 120.2(3) . . ? C10A C9A C8A 120.0 . . ? C9A C10A C11A 121.3 . . ? C1A C14A C15A 110.6(7) . . ? C1A C14A C16A 111.5(7) . . ? C15A C14A C16A 109.1(8) . . ? C1A C14A H14A 108.5 . . ? C15A C14A H14A 108.5 . . ? C16A C14A H14A 108.5 . . ? C14A C15A H15A 109.5 . . ? C14A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C14A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C14A C16A H16A 109.5 . . ? C14A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C14A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C19A C17A C18A 114.6(10) . . ? C19A C17A C3A 115.7(8) . . ? C18A C17A C3A 109.8(7) . . ? C19A C17A H17A 105.2 . . ? C18A C17A H17A 105.2 . . ? C3A C17A H17A 105.2 . . ? C17A C18A H18A 109.5 . . ? C17A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C17A C19A H19A 109.5 . . ? C17A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C17A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C21A C20A C22A 112.6(8) . . ? C21A C20A C5A 112.0(7) . . ? C22A C20A C5A 110.6(7) . . ? C21A C20A H20A 107.1 . . ? C22A C20A H20A 107.1 . . ? C5A C20A H20A 107.1 . . ? C20A C21A H21A 109.5 . . ? C20A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C20A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C20A C22A H22A 109.5 . . ? C20A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C20A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? N1A C24A C25A 113.7(6) . . ? N1A C24A C27A 110.9(6) . . ? C25A C24A C27A 110.9(6) . . ? N1A C24A H24A 107.0 . . ? C25A C24A H24A 107.0 . . ? C27A C24A H24A 107.0 . . ? O3A C25A O4A 125.0(7) . . ? O3A C25A C24A 120.5(7) . . ? O4A C25A C24A 114.0(6) . . ? C28A C27A C24A 112.7(5) . . ? C28A C27A H27A 109.0 . . ? C24A C27A H27A 109.0 . . ? C28A C27A H27B 109.0 . . ? C24A C27A H27B 109.0 . . ? H27A C27A H27B 107.8 . . ? C29A C28A C33A 117.2 . . ? C29A C28A C27A 120.4(5) . . ? C33A C28A C27A 122.3(5) . . ? C30A C29A C28A 121.3 . . ? C29A C30A C31A 121.0 . . ? C32A C31A C30A 118.1 . . ? C31A C32A C33A 121.2 . . ? C32A C33A C28A 121.2 . . ? C23B N1B C24B 121.6(7) . . ? C23B N1B H1B 119.2 . . ? C24B N1B H1B 119.2 . . ? C25B O4B C26B 117.6(7) . . ? C2B C1B C6B 117.9(7) . . ? C2B C1B C14B 120.0(7) . . ? C6B C1B C14B 121.9(8) . . ? C3B C2B C1B 122.4(7) . . ? C3B C2B H2B 118.8 . . ? C1B C2B H2B 118.8 . . ? C2B C3B C4B 118.2(6) . . ? C2B C3B C17B 120.4(8) . . ? C4B C3B C17B 121.3(8) . . ? C3B C4B C5B 122.4(7) . . ? C3B C4B H4B 118.8 . . ? C5B C4B H4B 118.8 . . ? C6B C5B C4B 117.4(6) . . ? C6B C5B C20B 122.0(7) . . ? C4B C5B C20B 120.3(7) . . ? C5B C6B C1B 121.7(6) . . ? C5B C6B C7B 118.6(6) . . ? C1B C6B C7B 119.5(7) . . ? O1B C7B C8B 121.1(5) . . ? O1B C7B C6B 120.0(7) . . ? C8B C7B C6B 118.8(6) . . ? O2B C23B N1B 123.4(6) . . ? O2B C23B C11B 120.3(5) . . ? N1B C23B C11B 116.2(5) . . ? C10B C11B C12B 118.3 . . ? C10B C11B C23B 124.0(4) . . ? C12B C11B C23B 117.7(4) . . ? C13B C12B C11B 120.3 . . ? C13B C12B H12B 119.8 . . ? C11B C12B H12B 119.8 . . ? C12B C13B C8B 121.5 . . ? C12B C13B H13B 119.2 . . ? C8B C13B H13B 119.2 . . ? C13B C8B C9B 118.5 . . ? C13B C8B C7B 121.5(3) . . ? C9B C8B C7B 120.0(3) . . ? C10B C9B C8B 120.0 . . ? C10B C9B H9B 120.0 . . ? C8B C9B H9B 120.0 . . ? C9B C10B C11B 121.3 . . ? C9B C10B H10B 119.3 . . ? C11B C10B H10B 119.3 . . ? C1B C14B C15B 110.2(9) . . ? C1B C14B C16B 112.8(8) . . ? C15B C14B C16B 109.9(9) . . ? C1B C14B H14B 108.0 . . ? C15B C14B H14B 108.0 . . ? C16B C14B H14B 108.0 . . ? C14B C15B H15D 109.5 . . ? C14B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C14B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C14B C16B H16D 109.5 . . ? C14B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C14B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C19B C17B C18B 116.8(10) . . ? C19B C17B C3B 113.3(9) . . ? C18B C17B C3B 113.4(9) . . ? C19B C17B H17B 103.8 . . ? C18B C17B H17B 103.8 . . ? C3B C17B H17B 103.8 . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C17B C19B H19D 109.5 . . ? C17B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C17B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C21B C20B C5B 113.3(9) . . ? C21B C20B C22B 112.0(9) . . ? C5B C20B C22B 110.1(9) . . ? C21B C20B H20B 107.0 . . ? C5B C20B H20B 107.0 . . ? C22B C20B H20B 107.0 . . ? C20B C21B H21D 109.5 . . ? C20B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C20B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C20B C22B H22D 109.5 . . ? C20B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C20B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? N1B C24B C25B 112.8(6) . . ? N1B C24B C27B 111.0(6) . . ? C25B C24B C27B 109.9(6) . . ? N1B C24B H24B 107.6 . . ? C25B C24B H24B 107.6 . . ? C27B C24B H24B 107.6 . . ? O3B C25B O4B 125.1(7) . . ? O3B C25B C24B 122.5(6) . . ? O4B C25B C24B 112.3(6) . . ? O4B C26B H26D 109.5 . . ? O4B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? O4B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C28B C27B C24B 112.9(6) . . ? C28B C27B H27C 109.0 . . ? C24B C27B H27C 109.0 . . ? C28B C27B H27D 109.0 . . ? C24B C27B H27D 109.0 . . ? H27C C27B H27D 107.8 . . ? C29B C28B C33B 117.2 . . ? C29B C28B C27B 121.8(5) . . ? C33B C28B C27B 120.9(5) . . ? C30B C29B C28B 121.3 . . ? C30B C29B H29B 119.3 . . ? C28B C29B H29B 119.3 . . ? C29B C30B C31B 121.0 . . ? C29B C30B H30B 119.5 . . ? C31B C30B H30B 119.5 . . ? C32B C31B C30B 118.1 . . ? C32B C31B H31B 120.9 . . ? C30B C31B H31B 120.9 . . ? C31B C32B C33B 121.2 . . ? C31B C32B H32B 119.4 . . ? C33B C32B H32B 119.4 . . ? C32B C33B C28B 121.2 . . ? C32B C33B H33B 119.4 . . ? C28B C33B H33B 119.4 . . ? C23C N1C C24C 123.3(19) . . ? C23C N1C H1C 118.4 . . ? C24C N1C H1C 118.4 . . ? C25C O4C C26C 116.5(18) . . ? C6C C1C C2C 123.0(11) . . ? C6C C1C C14C 95.1(9) . . ? C2C C1C C14C 141.6(13) . . ? C1C C2C C3C 116.5(12) . . ? C1C C2C H2C 121.7 . . ? C3C C2C H2C 121.7 . . ? C4C C3C C2C 120.3(11) . . ? C4C C3C C17C 120.1(13) . . ? C2C C3C C17C 119.6(13) . . ? C3C C4C C5C 123.6(12) . . ? C3C C4C H4C 118.2 . . ? C5C C4C H4C 118.2 . . ? C6C C5C C4C 114.1(11) . . ? C6C C5C C20C 123.9(13) . . ? C4C C5C C20C 121.8(13) . . ? C1C C6C C5C 122.4(10) . . ? C1C C6C C7C 95.9(9) . . ? C5C C6C C7C 141.7(12) . . ? O1C C7C C6C 113.0(14) . . ? O1C C7C C8C 109.6(12) . . ? C6C C7C C8C 116.0(13) . . ? O1C C7C C14C 111.9(12) . . ? C6C C7C C14C 84.0(7) . . ? C8C C7C C14C 120.4(16) . . ? O2C C23C N1C 121.6(18) . . ? O2C C23C C11C 121.9(18) . . ? N1C C23C C11C 114.7(13) . . ? C10C C11C C12C 117.6 . . ? C10C C11C C23C 122.9(11) . . ? C12C C11C C23C 119.5(11) . . ? C13C C12C C11C 120.9 . . ? C12C C13C C8C 121.7 . . ? C9C C8C C13C 117.1 . . ? C9C C8C C7C 121.7(9) . . ? C13C C8C C7C 120.6(9) . . ? C8C C9C C10C 121.2 . . ? C11C C10C C9C 121.1 . . ? C16C C14C C1C 114.9(14) . . ? C16C C14C C15C 110.6(12) . . ? C1C C14C C15C 112.9(14) . . ? C16C C14C C7C 121.0(14) . . ? C1C C14C C7C 84.4(7) . . ? C15C C14C C7C 110.7(13) . . ? C14C C15C H15G 109.5 . . ? C14C C15C H15H 109.5 . . ? H15G C15C H15H 109.5 . . ? C14C C15C H15I 109.5 . . ? H15G C15C H15I 109.5 . . ? H15H C15C H15I 109.5 . . ? C14C C16C H16G 109.5 . . ? C14C C16C H16H 109.5 . . ? H16G C16C H16H 109.5 . . ? C14C C16C H16I 109.5 . . ? H16G C16C H16I 109.5 . . ? H16H C16C H16I 109.5 . . ? C19C C17C C18C 112.5(16) . . ? C19C C17C C3C 112.3(16) . . ? C18C C17C C3C 110.0(15) . . ? C19C C17C H17C 107.2 . . ? C18C C17C H17C 107.2 . . ? C3C C17C H17C 107.2 . . ? C17C C18C H18G 109.5 . . ? C17C C18C H18H 109.5 . . ? H18G C18C H18H 109.5 . . ? C17C C18C H18I 109.5 . . ? H18G C18C H18I 109.5 . . ? H18H C18C H18I 109.5 . . ? C17C C19C H19G 109.5 . . ? C17C C19C H19H 109.5 . . ? H19G C19C H19H 109.5 . . ? C17C C19C H19I 109.5 . . ? H19G C19C H19I 109.5 . . ? H19H C19C H19I 109.5 . . ? C21C C20C C22C 109.0(15) . . ? C21C C20C C5C 111.9(16) . . ? C22C C20C C5C 110.6(15) . . ? C21C C20C H20C 108.4 . . ? C22C C20C H20C 108.4 . . ? C5C C20C H20C 108.4 . . ? C20C C21C H21G 109.5 . . ? C20C C21C H21H 109.5 . . ? H21G C21C H21H 109.5 . . ? C20C C21C H21I 109.5 . . ? H21G C21C H21I 109.5 . . ? H21H C21C H21I 109.5 . . ? C20C C22C H22G 109.5 . . ? C20C C22C H22H 109.5 . . ? H22G C22C H22H 109.5 . . ? C20C C22C H22I 109.5 . . ? H22G C22C H22I 109.5 . . ? H22H C22C H22I 109.5 . . ? N1C C24C C25C 115.3(17) . . ? N1C C24C C27C 111.6(16) . . ? C25C C24C C27C 111.5(14) . . ? N1C C24C H24C 105.9 . . ? C25C C24C H24C 105.9 . . ? C27C C24C H24C 105.9 . . ? O3C C25C O4C 120.6(15) . . ? O3C C25C C24C 122.4(15) . . ? O4C C25C C24C 117.0(14) . . ? C28C C27C C24C 115.4(14) . . ? C28C C27C H27E 108.4 . . ? C24C C27C H27E 108.4 . . ? C28C C27C H27F 108.4 . . ? C24C C27C H27F 108.4 . . ? H27E C27C H27F 107.5 . . ? C29C C28C C33C 118.0 . . ? C29C C28C C27C 120.2(11) . . ? C33C C28C C27C 121.8(11) . . ? C28C C29C C30C 120.7 . . ? C31C C30C C29C 121.2 . . ? C32C C31C C30C 118.1 . . ? C31C C32C C33C 120.9 . . ? C32C C33C C28C 121.0 . . ? C23D N1D C24D 123.2(17) . . ? C23D N1D H1D 118.4 . . ? C24D N1D H1D 118.4 . . ? C25D O4D C26D 119.3(18) . . ? C6D C1D C2D 123.4(11) . . ? C6D C1D C14D 95.8(8) . . ? C2D C1D C14D 140.7(12) . . ? C1D C2D C3D 116.1(12) . . ? C1D C2D H2D 122.0 . . ? C3D C2D H2D 122.0 . . ? C4D C3D C2D 120.4(11) . . ? C4D C3D C17D 119.5(12) . . ? C2D C3D C17D 119.0(13) . . ? C3D C4D C5D 124.2(12) . . ? C3D C4D H4D 117.9 . . ? C5D C4D H4D 117.9 . . ? C6D C5D C4D 113.5(11) . . ? C6D C5D C20D 123.9(14) . . ? C4D C5D C20D 118.3(13) . . ? C1D C6D C5D 122.4(10) . . ? C1D C6D C7D 95.2(9) . . ? C5D C6D C7D 142.2(11) . . ? O1D C7D C6D 113.8(13) . . ? O1D C7D C8D 110.8(12) . . ? C6D C7D C8D 117.3(13) . . ? O1D C7D C14D 111.9(12) . . ? C6D C7D C14D 85.0(7) . . ? C8D C7D C14D 115.8(14) . . ? O2D C23D N1D 120.1(16) . . ? O2D C23D C11D 121.8(17) . . ? N1D C23D C11D 116.0(12) . . ? C10D C11D C12D 117.6 . . ? C10D C11D C23D 122.8(10) . . ? C12D C11D C23D 119.3(11) . . ? C13D C12D C11D 120.9 . . ? C12D C13D C8D 121.7 . . ? C9D C8D C13D 117.1 . . ? C9D C8D C7D 121.1(8) . . ? C13D C8D C7D 121.3(8) . . ? C8D C9D C10D 121.2 . . ? C11D C10D C9D 121.1 . . ? C16D C14D C1D 116.0(13) . . ? C16D C14D C15D 110.4(12) . . ? C1D C14D C15D 113.7(14) . . ? C16D C14D C7D 120.4(14) . . ? C1D C14D C7D 83.8(7) . . ? C15D C14D C7D 110.3(12) . . ? C14D C15D H15J 109.5 . . ? C14D C15D H15K 109.5 . . ? H15J C15D H15K 109.5 . . ? C14D C15D H15L 109.5 . . ? H15J C15D H15L 109.5 . . ? H15K C15D H15L 109.5 . . ? C14D C16D H16J 109.5 . . ? C14D C16D H16K 109.5 . . ? H16J C16D H16K 109.5 . . ? C14D C16D H16L 109.5 . . ? H16J C16D H16L 109.5 . . ? H16K C16D H16L 109.5 . . ? C19D C17D C18D 115.8(17) . . ? C19D C17D C3D 112.4(15) . . ? C18D C17D C3D 111.0(16) . . ? C19D C17D H17D 105.6 . . ? C18D C17D H17D 105.6 . . ? C3D C17D H17D 105.6 . . ? C17D C18D H18J 109.5 . . ? C17D C18D H18K 109.5 . . ? H18J C18D H18K 109.5 . . ? C17D C18D H18L 109.5 . . ? H18J C18D H18L 109.5 . . ? H18K C18D H18L 109.5 . . ? C17D C19D H19J 109.5 . . ? C17D C19D H19K 109.5 . . ? H19J C19D H19K 109.5 . . ? C17D C19D H19L 109.5 . . ? H19J C19D H19L 109.5 . . ? H19K C19D H19L 109.5 . . ? C21D C20D C22D 108.0(15) . . ? C21D C20D C5D 110.8(15) . . ? C22D C20D C5D 109.6(14) . . ? C21D C20D H20D 109.5 . . ? C22D C20D H20D 109.5 . . ? C5D C20D H20D 109.5 . . ? C20D C21D H21J 109.5 . . ? C20D C21D H21K 109.5 . . ? H21J C21D H21K 109.5 . . ? C20D C21D H21L 109.5 . . ? H21J C21D H21L 109.5 . . ? H21K C21D H21L 109.5 . . ? C20D C22D H22J 109.5 . . ? C20D C22D H22K 109.5 . . ? H22J C22D H22K 109.5 . . ? C20D C22D H22L 109.5 . . ? H22J C22D H22L 109.5 . . ? H22K C22D H22L 109.5 . . ? N1D C24D C25D 113.7(15) . . ? N1D C24D C27D 111.1(15) . . ? C25D C24D C27D 109.6(14) . . ? N1D C24D H24D 107.4 . . ? C25D C24D H24D 107.4 . . ? C27D C24D H24D 107.4 . . ? O3D C25D O4D 123.6(15) . . ? O3D C25D C24D 120.6(15) . . ? O4D C25D C24D 114.1(13) . . ? C28D C27D C24D 112.9(14) . . ? C28D C27D H27G 109.0 . . ? C24D C27D H27G 109.0 . . ? C28D C27D H27H 109.0 . . ? C24D C27D H27H 109.0 . . ? H27G C27D H27H 107.8 . . ? C29D C28D C33D 118.1 . . ? C29D C28D C27D 121.8(11) . . ? C33D C28D C27D 120.1(11) . . ? C28D C29D C30D 120.7 . . ? C31D C30D C29D 121.2 . . ? C32D C31D C30D 118.1 . . ? C31D C32D C33D 120.9 . . ? C32D C33D C28D 121.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.212 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.035 #===END data_20.4%C,30.6%D _database_code_depnum_ccdc_archive 'CCDC 799266' #TrackingRef '- 1.cif' #==================================================================== # start Validation Reply Form _vrf_PLAT201_20.4%C,30.6%D ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 24 RESPONSE: In the crystal there are reactant and photoproduct molecules. Part of atoms were refined isotropically in order to decrease a large number of the parameters in the refinement. ; # end Validation Reply Form #==================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 N O4' _chemical_formula_weight 513.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 22.142(4) _cell_length_b 9.3891(17) _cell_length_c 28.954(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6019.3(19) _cell_formula_units_Z 8 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 3.61 _cell_measurement_theta_max 12.79 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28026 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5390 _reflns_number_gt 3548 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSALIS (Oxford Diffraction, 2003)' _computing_cell_refinement 'CRYSALIS (Oxford Diffraction, 2003)' _computing_data_reduction 'CRYSALIS (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SXELXL97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Owing to a reactant-product disorder, the following weak restraints from SHELXL97 were applied: DFIX, DANG and SIMU. DFIX and DANG restrained bond lengths and valence angles to target values. The target values were taken from the structures of the pure reactant and the pure product of crystal 1a. SIMU restrained displacement parameters of atoms of the products. ; _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^)+(0.1315P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5390 _refine_ls_number_parameters 777 _refine_ls_number_restraints 602 _refine_ls_R_factor_all 0.1143 _refine_ls_R_factor_gt 0.0774 _refine_ls_wR_factor_ref 0.2291 _refine_ls_wR_factor_gt 0.1980 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.092 _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 N1A N 0.3867(4) 0.9445(9) 0.4487(3) 0.061(2) Uani 0.796(9) 1 d PDU A 1 H1A H 0.3726 1.0292 0.4519 0.074 Uiso 0.796(9) 1 calc PR A 1 O1A O 0.1017(4) 1.1029(12) 0.3549(4) 0.117(4) Uani 0.796(9) 1 d PDU A 1 O2A O 0.3804(8) 0.7396(13) 0.4092(7) 0.074(4) Uani 0.796(9) 1 d PDU A 1 O3A O 0.5438(3) 0.9371(10) 0.4716(5) 0.149(4) Uani 0.796(9) 1 d PDU A 1 O4A O 0.4869(4) 1.0887(10) 0.4337(3) 0.093(3) Uani 0.796(9) 1 d PDU A 1 C1A C 0.1341(5) 1.0398(10) 0.2480(3) 0.077(3) Uani 0.796(9) 1 d PDU A 1 C2A C 0.1159(6) 0.9808(13) 0.2064(3) 0.083(4) Uani 0.796(9) 1 d PD A 1 H2A H 0.1225 1.0321 0.1794 0.100 Uiso 0.796(9) 1 calc PR A 1 C3A C 0.0889(7) 0.8509(12) 0.2033(3) 0.080(3) Uani 0.796(9) 1 d PDU A 1 C4A C 0.0777(7) 0.7759(12) 0.2433(3) 0.081(3) Uani 0.796(9) 1 d PDU A 1 H4A H 0.0592 0.6870 0.2419 0.097 Uiso 0.796(9) 1 calc PR A 1 C5A C 0.0940(7) 0.8336(9) 0.2864(3) 0.072(4) Uani 0.796(9) 1 d PD A 1 C6A C 0.1212(5) 0.9647(9) 0.2880(2) 0.064(7) Uani 0.796(9) 1 d PD A 1 C7A C 0.1368(3) 1.0263(8) 0.3346(3) 0.070(2) Uani 0.796(9) 1 d PDU A 1 C23A C 0.3588(4) 0.8550(10) 0.4201(4) 0.054(2) Uani 0.796(9) 1 d PDU A 1 C11A C 0.3017(2) 0.9061(6) 0.3994(2) 0.057(3) Uiso 0.796(9) 1 d PGDU A 1 C12A C 0.2868(2) 0.8546(6) 0.3558(2) 0.058(2) Uiso 0.796(9) 1 d PGDU A 1 H12A H 0.3131 0.7931 0.3406 0.070 Uiso 0.796(9) 1 d PG A 1 C13A C 0.2341(2) 0.8938(5) 0.33521(18) 0.063(2) Uiso 0.796(9) 1 d PGDU A 1 H13A H 0.2248 0.8582 0.3061 0.075 Uiso 0.796(9) 1 d PG A 1 C8A C 0.1940(2) 0.9853(6) 0.3567(2) 0.0543(18) Uiso 0.796(9) 1 d PGD A 1 C9A C 0.2084(2) 1.0373(6) 0.4001(2) 0.066(2) Uiso 0.796(9) 1 d PGDU A 1 H9A H 0.1821 1.0987 0.4153 0.079 Uiso 0.796(9) 1 d PG A 1 C10A C 0.2618(2) 0.9980(6) 0.42086(18) 0.060(2) Uiso 0.796(9) 1 d PGDU A 1 H10A H 0.2713 1.0340 0.4499 0.072 Uiso 0.796(9) 1 d PG A 1 C14A C 0.1672(4) 1.1787(9) 0.2485(4) 0.110(3) Uani 0.796(9) 1 d PDU A 1 H14A H 0.1766 1.2023 0.2807 0.132 Uiso 0.796(9) 1 calc PR A 1 C15A C 0.1280(6) 1.2966(11) 0.2290(8) 0.185(8) Uani 0.796(9) 1 d PDU A 1 H15A H 0.1504 1.3841 0.2284 0.278 Uiso 0.796(9) 1 calc PR A 1 H15B H 0.0928 1.3081 0.2480 0.278 Uiso 0.796(9) 1 calc PR A 1 H15C H 0.1158 1.2723 0.1981 0.278 Uiso 0.796(9) 1 calc PR A 1 C16A C 0.2262(5) 1.1716(16) 0.2220(6) 0.156(5) Uani 0.796(9) 1 d PDU A 1 H16A H 0.2455 1.2631 0.2228 0.234 Uiso 0.796(9) 1 calc PR A 1 H16B H 0.2183 1.1452 0.1906 0.234 Uiso 0.796(9) 1 calc PR A 1 H16C H 0.2522 1.1020 0.2360 0.234 Uiso 0.796(9) 1 calc PR A 1 C17A C 0.0726(5) 0.7890(13) 0.1570(3) 0.106(3) Uani 0.796(9) 1 d PDU A 1 H17A H 0.0670 0.8708 0.1365 0.127 Uiso 0.796(9) 1 calc PR A 1 C18A C 0.1249(7) 0.708(2) 0.1375(5) 0.192(8) Uani 0.796(9) 1 d PDU A 1 H18A H 0.1609 0.7640 0.1398 0.289 Uiso 0.796(9) 1 calc PR A 1 H18B H 0.1171 0.6860 0.1056 0.289 Uiso 0.796(9) 1 calc PR A 1 H18C H 0.1301 0.6206 0.1544 0.289 Uiso 0.796(9) 1 calc PR A 1 C19A C 0.0158(7) 0.710(2) 0.1554(6) 0.158(7) Uani 0.796(9) 1 d PDU A 1 H19A H 0.0084 0.6782 0.1244 0.236 Uiso 0.796(9) 1 calc PR A 1 H19B H -0.0166 0.7710 0.1652 0.236 Uiso 0.796(9) 1 calc PR A 1 H19C H 0.0182 0.6293 0.1757 0.236 Uiso 0.796(9) 1 calc PR A 1 C20A C 0.0821(4) 0.7485(9) 0.3301(3) 0.084(3) Uani 0.796(9) 1 d PDU A 1 H20A H 0.1009 0.8005 0.3557 0.101 Uiso 0.796(9) 1 calc PR A 1 C21A C 0.0157(5) 0.7390(18) 0.3404(6) 0.139(5) Uani 0.796(9) 1 d PDU A 1 H21A H -0.0047 0.8190 0.3269 0.208 Uiso 0.796(9) 1 calc PR A 1 H21B H 0.0096 0.7398 0.3732 0.208 Uiso 0.796(9) 1 calc PR A 1 H21C H -0.0002 0.6524 0.3277 0.208 Uiso 0.796(9) 1 calc PR A 1 C22A C 0.1116(6) 0.6042(12) 0.3280(5) 0.139(5) Uani 0.796(9) 1 d PDU A 1 H22A H 0.1545 0.6147 0.3316 0.209 Uiso 0.796(9) 1 calc PR A 1 H22B H 0.1031 0.5608 0.2987 0.209 Uiso 0.796(9) 1 calc PR A 1 H22C H 0.0961 0.5452 0.3523 0.209 Uiso 0.796(9) 1 calc PR A 1 C24A C 0.4400(3) 0.9044(9) 0.4745(3) 0.070(2) Uani 0.796(9) 1 d PDU A 1 H24A H 0.4458 0.8019 0.4700 0.083 Uiso 0.796(9) 1 calc PR A 1 C25A C 0.4965(3) 0.9767(10) 0.4582(4) 0.084(3) Uani 0.796(9) 1 d PDU A 1 C26A C 0.5386(5) 1.1675(12) 0.4180(6) 0.112(5) Uani 0.796(9) 1 d PDU A 1 H26A H 0.5583 1.2107 0.4439 0.168 Uiso 0.796(9) 1 calc PR A 1 H26B H 0.5258 1.2402 0.3968 0.168 Uiso 0.796(9) 1 calc PR A 1 H26C H 0.5661 1.1042 0.4027 0.168 Uiso 0.796(9) 1 calc PR A 1 C27A C 0.4308(4) 0.9277(10) 0.5258(3) 0.085(3) Uani 0.796(9) 1 d PDU A 1 H27A H 0.4678 0.9037 0.5419 0.102 Uiso 0.796(9) 1 calc PR A 1 H27B H 0.4226 1.0277 0.5313 0.102 Uiso 0.796(9) 1 calc PR A 1 C28A C 0.3803(3) 0.8409(6) 0.5451(3) 0.074(2) Uiso 0.796(9) 1 d PGD A 1 C29A C 0.3271(3) 0.9055(5) 0.5577(3) 0.117(3) Uiso 0.796(9) 1 d PGDU A 1 H29A H 0.3230 1.0034 0.5541 0.140 Uiso 0.796(9) 1 d PG A 1 C30A C 0.2799(3) 0.8284(8) 0.5754(4) 0.145(4) Uiso 0.796(9) 1 d PGU A 1 H30A H 0.2446 0.8749 0.5839 0.174 Uiso 0.796(9) 1 d PG A 1 C31A C 0.2842(3) 0.6830(8) 0.5808(3) 0.122(4) Uiso 0.796(9) 1 d PGU A 1 H31A H 0.2524 0.6309 0.5934 0.147 Uiso 0.796(9) 1 d PG A 1 C32A C 0.3361(4) 0.6177(5) 0.5672(3) 0.119(4) Uiso 0.796(9) 1 d PG A 1 H32A H 0.3395 0.5193 0.5699 0.143 Uiso 0.796(9) 1 d PG A 1 C33A C 0.3837(3) 0.6945(6) 0.5498(3) 0.092(3) Uiso 0.796(9) 1 d PGD A 1 H33A H 0.4187 0.6473 0.5410 0.110 Uiso 0.796(9) 1 d PG A 1 N1B N 0.3528(5) 0.4363(10) 0.4253(4) 0.062(3) Uani 0.694(11) 1 d PDU B 2 H1B H 0.3689 0.5170 0.4186 0.074 Uiso 0.694(11) 1 calc PR B 2 O1B O 0.6351(4) 0.6280(14) 0.5150(4) 0.117(4) Uani 0.694(11) 1 d PDU B 2 O2B O 0.3573(3) 0.2428(6) 0.4706(3) 0.0548(19) Uani 0.694(11) 1 d PDU B 2 O3B O 0.1940(3) 0.4040(9) 0.4206(5) 0.119(4) Uani 0.694(11) 1 d PDU B 2 O4B O 0.2518(4) 0.5851(11) 0.4395(4) 0.085(3) Uani 0.694(11) 1 d PDU B 2 C1B C 0.6072(7) 0.5755(12) 0.6225(4) 0.081(7) Uani 0.694(11) 1 d PD B 2 C2B C 0.6251(8) 0.5213(16) 0.6647(3) 0.104(4) Uani 0.694(11) 1 d PDU B 2 H2B H 0.6164 0.5730 0.6913 0.125 Uiso 0.694(11) 1 calc PR B 2 C3B C 0.6552(6) 0.3947(14) 0.6691(3) 0.093(4) Uani 0.694(11) 1 d PDU B 2 C4B C 0.6666(6) 0.3197(13) 0.6297(3) 0.085(3) Uani 0.694(11) 1 d PDU B 2 H4B H 0.6862 0.2325 0.6321 0.102 Uiso 0.694(11) 1 calc PR B 2 C5B C 0.6500(7) 0.3683(13) 0.5858(3) 0.071(5) Uani 0.694(11) 1 d PD B 2 C6B C 0.6201(5) 0.4960(11) 0.5830(3) 0.067(3) Uani 0.694(11) 1 d PDU B 2 C7B C 0.6015(3) 0.5516(9) 0.5370(3) 0.075(3) Uani 0.694(11) 1 d PDU B 2 C23B C 0.3791(5) 0.3556(12) 0.4569(5) 0.056(3) Uani 0.694(11) 1 d PDU B 2 C11B C 0.4371(3) 0.4087(8) 0.4760(2) 0.054(4) Uiso 0.694(11) 1 d PGDU B 2 C12B C 0.4540(3) 0.3628(7) 0.5198(2) 0.053(3) Uiso 0.694(11) 1 d PGD B 2 H12B H 0.4291 0.3011 0.5362 0.064 Uiso 0.694(11) 1 d PG B 2 C13B C 0.5069(3) 0.4079(6) 0.5389(2) 0.058(2) Uiso 0.694(11) 1 d PGD B 2 H13B H 0.5176 0.3760 0.5682 0.070 Uiso 0.694(11) 1 d PG B 2 C8B C 0.5451(2) 0.4999(7) 0.5157(2) 0.064(2) Uiso 0.694(11) 1 d PGDU B 2 C9B C 0.5285(2) 0.5463(7) 0.4720(2) 0.059(2) Uiso 0.694(11) 1 d PGD B 2 H9B H 0.5535 0.6080 0.4557 0.070 Uiso 0.694(11) 1 d PG B 2 C10B C 0.4750(3) 0.5011(8) 0.45274(19) 0.058(3) Uiso 0.694(11) 1 d PGD B 2 H10B H 0.4641 0.5334 0.4235 0.069 Uiso 0.694(11) 1 d PG B 2 C14B C 0.5716(5) 0.7105(13) 0.6181(5) 0.122(4) Uani 0.694(11) 1 d PDU B 2 H14B H 0.5643 0.7252 0.5851 0.146 Uiso 0.694(11) 1 calc PR B 2 C15B C 0.6065(8) 0.8371(14) 0.6348(10) 0.196(9) Uani 0.694(11) 1 d PDU B 2 H15D H 0.5821 0.9212 0.6320 0.295 Uiso 0.694(11) 1 calc PR B 2 H15E H 0.6425 0.8478 0.6166 0.295 Uiso 0.694(11) 1 calc PR B 2 H15F H 0.6174 0.8235 0.6666 0.295 Uiso 0.694(11) 1 calc PR B 2 C16B C 0.5101(5) 0.7031(19) 0.6411(7) 0.142(6) Uani 0.694(11) 1 d PDU B 2 H16D H 0.4914 0.6136 0.6340 0.214 Uiso 0.694(11) 1 calc PR B 2 H16E H 0.4852 0.7795 0.6300 0.214 Uiso 0.694(11) 1 calc PR B 2 H16F H 0.5149 0.7115 0.6740 0.214 Uiso 0.694(11) 1 calc PR B 2 C17B C 0.6759(6) 0.3453(17) 0.7158(4) 0.142(5) Uani 0.694(11) 1 d PDU B 2 H17B H 0.6518 0.4057 0.7363 0.171 Uiso 0.694(11) 1 calc PR B 2 C18B C 0.6530(10) 0.202(2) 0.7273(7) 0.175(8) Uani 0.694(11) 1 d PDU B 2 H18D H 0.6097 0.2029 0.7275 0.262 Uiso 0.694(11) 1 calc PR B 2 H18E H 0.6677 0.1741 0.7572 0.262 Uiso 0.694(11) 1 calc PR B 2 H18F H 0.6669 0.1347 0.7046 0.262 Uiso 0.694(11) 1 calc PR B 2 C19B C 0.7364(6) 0.3845(16) 0.7285(5) 0.127(5) Uani 0.694(11) 1 d PDU B 2 H19D H 0.7510 0.4565 0.7078 0.191 Uiso 0.694(11) 1 calc PR B 2 H19E H 0.7621 0.3023 0.7267 0.191 Uiso 0.694(11) 1 calc PR B 2 H19F H 0.7366 0.4207 0.7595 0.191 Uiso 0.694(11) 1 calc PR B 2 C20B C 0.6643(8) 0.2825(15) 0.5428(4) 0.118(5) Uani 0.694(11) 1 d PDU B 2 H20B H 0.6524 0.3387 0.5158 0.142 Uiso 0.694(11) 1 calc PR B 2 C21B C 0.7302(8) 0.249(3) 0.5388(10) 0.162(9) Uani 0.694(11) 1 d PDU B 2 H21D H 0.7533 0.3228 0.5536 0.243 Uiso 0.694(11) 1 calc PR B 2 H21E H 0.7412 0.2442 0.5067 0.243 Uiso 0.694(11) 1 calc PR B 2 H21F H 0.7385 0.1596 0.5533 0.243 Uiso 0.694(11) 1 calc PR B 2 C22B C 0.6273(8) 0.1452(18) 0.5430(9) 0.165(8) Uani 0.694(11) 1 d PDU B 2 H22D H 0.5854 0.1675 0.5384 0.248 Uiso 0.694(11) 1 calc PR B 2 H22E H 0.6322 0.0977 0.5721 0.248 Uiso 0.694(11) 1 calc PR B 2 H22F H 0.6410 0.0839 0.5186 0.248 Uiso 0.694(11) 1 calc PR B 2 C24B C 0.2985(4) 0.3949(11) 0.4017(3) 0.061(3) Uani 0.694(11) 1 d PDU B 2 H24B H 0.2949 0.2913 0.4047 0.073 Uiso 0.694(11) 1 calc PR B 2 C25B C 0.2420(4) 0.4595(11) 0.4224(4) 0.074(3) Uani 0.694(11) 1 d PDU B 2 C26B C 0.1993(8) 0.661(2) 0.4568(9) 0.112(7) Uani 0.694(11) 1 d PDU B 2 H26D H 0.1911 0.7415 0.4373 0.167 Uiso 0.694(11) 1 calc PR B 2 H26E H 0.2071 0.6934 0.4877 0.167 Uiso 0.694(11) 1 calc PR B 2 H26F H 0.1650 0.5986 0.4569 0.167 Uiso 0.694(11) 1 calc PR B 2 C27B C 0.3019(5) 0.4285(13) 0.3502(3) 0.072(3) Uani 0.694(11) 1 d PDU B 2 H27C H 0.2648 0.3974 0.3356 0.087 Uiso 0.694(11) 1 calc PR B 2 H27D H 0.3049 0.5309 0.3463 0.087 Uiso 0.694(11) 1 calc PR B 2 C28B C 0.3537(4) 0.3601(9) 0.3266(3) 0.075(3) Uiso 0.694(11) 1 d PGDU B 2 C29B C 0.4062(4) 0.4320(8) 0.3167(4) 0.098(4) Uiso 0.694(11) 1 d PGD B 2 H29B H 0.4096 0.5277 0.3246 0.118 Uiso 0.694(11) 1 d PG B 2 C30B C 0.4538(4) 0.3654(11) 0.2955(4) 0.126(5) Uiso 0.694(11) 1 d PG B 2 H30B H 0.4887 0.4168 0.2890 0.152 Uiso 0.694(11) 1 d PG B 2 C31B C 0.4507(4) 0.2235(11) 0.2838(4) 0.134(5) Uiso 0.694(11) 1 d PG B 2 H31B H 0.4827 0.1787 0.2689 0.161 Uiso 0.694(11) 1 d PG B 2 C32B C 0.3995(4) 0.1506(8) 0.2945(4) 0.122(4) Uiso 0.694(11) 1 d PG B 2 H32B H 0.3969 0.0540 0.2876 0.147 Uiso 0.694(11) 1 d PG B 2 C33B C 0.3515(4) 0.2170(8) 0.3155(4) 0.103(4) Uiso 0.694(11) 1 d PGD B 2 H33B H 0.3169 0.1648 0.3223 0.124 Uiso 0.694(11) 1 d PG B 2 N1C N 0.3753(13) 0.949(4) 0.4553(10) 0.068(9) Uiso 0.204(9) 1 d PDU A 3 H1C H 0.3527 1.0198 0.4628 0.082 Uiso 0.204(9) 1 calc PR A 3 O1C O 0.1133(11) 1.150(3) 0.3437(9) 0.078(10) Uiso 0.204(9) 1 d PDU A 3 O2C O 0.384(3) 0.755(6) 0.410(2) 0.069(14) Uiso 0.204(9) 1 d PDU A 3 O3C O 0.5261(14) 0.999(5) 0.4972(12) 0.164(15) Uiso 0.204(9) 1 d PDU A 3 O4C O 0.4842(17) 1.055(5) 0.4308(12) 0.092(9) Uiso 0.204(9) 1 d PDU A 3 C1C C 0.1323(19) 1.014(4) 0.2457(7) 0.074(9) Uiso 0.204(9) 1 d PDU A 3 C2C C 0.116(2) 0.953(5) 0.2047(8) 0.11(3) Uiso 0.204(9) 1 d PD A 3 H2C H 0.1271 0.9922 0.1765 0.130 Uiso 0.204(9) 1 calc PR A 3 C3C C 0.082(3) 0.829(5) 0.2075(9) 0.083(9) Uiso 0.204(9) 1 d PDU A 3 C4C C 0.067(3) 0.773(4) 0.2494(9) 0.075(9) Uiso 0.204(9) 1 d PDU A 3 H4C H 0.0454 0.6881 0.2500 0.091 Uiso 0.204(9) 1 calc PR A 3 C5C C 0.083(2) 0.837(4) 0.2915(8) 0.09(3) Uiso 0.204(9) 1 d PD A 3 C6C C 0.1175(14) 0.957(3) 0.2871(7) 0.08(4) Uiso 0.204(9) 1 d PD A 3 C7C C 0.1514(7) 1.066(2) 0.3161(6) 0.080(9) Uiso 0.204(9) 1 d PDU A 3 C23C C 0.3613(18) 0.873(5) 0.4174(14) 0.063(10) Uiso 0.204(9) 1 d PDU A 3 C11C C 0.3059(7) 0.920(2) 0.3930(6) 0.037(8) Uiso 0.204(9) 1 d PGDU A 3 C12C C 0.2945(8) 0.872(2) 0.3491(6) 0.053(8) Uiso 0.204(9) 1 d PGDU A 3 H12C H 0.3207 0.8064 0.3356 0.063 Uiso 0.204(9) 1 d PG A 3 C13C C 0.2455(8) 0.918(2) 0.3251(5) 0.057(7) Uiso 0.204(9) 1 d PGDU A 3 H13C H 0.2393 0.8843 0.2952 0.069 Uiso 0.204(9) 1 d PG A 3 C8C C 0.2047(7) 1.0126(18) 0.3439(6) 0.041(6) Uiso 0.204(9) 1 d PGD A 3 C9C C 0.2181(7) 1.0671(17) 0.3862(6) 0.044(6) Uiso 0.204(9) 1 d PGDU A 3 H9C H 0.1931 1.1364 0.3989 0.053 Uiso 0.204(9) 1 d PG A 3 C10C C 0.2680(7) 1.022(2) 0.4106(5) 0.049(7) Uiso 0.204(9) 1 d PGDU A 3 H10C H 0.2760 1.0605 0.4395 0.059 Uiso 0.204(9) 1 d PG A 3 C14C C 0.1657(11) 1.142(2) 0.2658(7) 0.108(10) Uiso 0.204(9) 1 d PDU A 3 C15C C 0.131(2) 1.282(4) 0.2617(15) 0.18(2) Uiso 0.204(9) 1 d PDU A 3 H15G H 0.0903 1.2682 0.2722 0.263 Uiso 0.204(9) 1 calc PR A 3 H15H H 0.1305 1.3121 0.2300 0.263 Uiso 0.204(9) 1 calc PR A 3 H15I H 0.1503 1.3533 0.2803 0.263 Uiso 0.204(9) 1 calc PR A 3 C16C C 0.2295(12) 1.160(4) 0.2502(12) 0.092(11) Uiso 0.204(9) 1 d PDU A 3 H16G H 0.2509 1.0720 0.2541 0.138 Uiso 0.204(9) 1 calc PR A 3 H16H H 0.2486 1.2332 0.2682 0.138 Uiso 0.204(9) 1 calc PR A 3 H16I H 0.2300 1.1867 0.2182 0.138 Uiso 0.204(9) 1 calc PR A 3 C17C C 0.060(2) 0.755(4) 0.1634(10) 0.112(11) Uiso 0.204(9) 1 d PDU A 3 H17C H 0.0671 0.8201 0.1374 0.135 Uiso 0.204(9) 1 calc PR A 3 C18C C 0.095(3) 0.624(5) 0.155(2) 0.165(19) Uiso 0.204(9) 1 d PDU A 3 H18G H 0.1373 0.6463 0.1551 0.248 Uiso 0.204(9) 1 calc PR A 3 H18H H 0.0840 0.5850 0.1254 0.248 Uiso 0.204(9) 1 calc PR A 3 H18I H 0.0865 0.5559 0.1787 0.248 Uiso 0.204(9) 1 calc PR A 3 C19C C -0.0051(19) 0.727(9) 0.165(3) 0.141(18) Uiso 0.204(9) 1 d PDU A 3 H19G H -0.0260 0.8129 0.1736 0.212 Uiso 0.204(9) 1 calc PR A 3 H19H H -0.0130 0.6548 0.1879 0.212 Uiso 0.204(9) 1 calc PR A 3 H19I H -0.0188 0.6954 0.1355 0.212 Uiso 0.204(9) 1 calc PR A 3 C20C C 0.0582(16) 0.780(3) 0.3370(9) 0.093(9) Uiso 0.204(9) 1 d PDU A 3 H20C H 0.0544 0.8592 0.3589 0.112 Uiso 0.204(9) 1 calc PR A 3 C21C C -0.0030(17) 0.712(7) 0.330(2) 0.135(18) Uiso 0.204(9) 1 d PDU A 3 H21G H -0.0340 0.7829 0.3337 0.202 Uiso 0.204(9) 1 calc PR A 3 H21H H -0.0087 0.6385 0.3528 0.202 Uiso 0.204(9) 1 calc PR A 3 H21I H -0.0053 0.6718 0.2998 0.202 Uiso 0.204(9) 1 calc PR A 3 C22C C 0.101(2) 0.669(6) 0.357(2) 0.168(18) Uiso 0.204(9) 1 d PDU A 3 H22G H 0.0875 0.6430 0.3870 0.252 Uiso 0.204(9) 1 calc PR A 3 H22H H 0.1407 0.7081 0.3582 0.252 Uiso 0.204(9) 1 calc PR A 3 H22I H 0.1007 0.5870 0.3370 0.252 Uiso 0.204(9) 1 calc PR A 3 C24C C 0.4264(10) 0.917(4) 0.4835(7) 0.080(9) Uiso 0.204(9) 1 d PDU A 3 H24C H 0.4335 0.8146 0.4787 0.096 Uiso 0.204(9) 1 calc PR A 3 C25C C 0.4841(12) 0.987(5) 0.4704(9) 0.084(10) Uiso 0.204(9) 1 d PDU A 3 C26C C 0.539(2) 1.125(8) 0.418(2) 0.127(18) Uiso 0.204(9) 1 d PDU A 3 C27C C 0.4128(13) 0.931(4) 0.5346(8) 0.084(9) Uiso 0.204(9) 1 d PDU A 3 H27E H 0.4494 0.9113 0.5519 0.101 Uiso 0.204(9) 1 calc PR A 3 H27F H 0.4014 1.0291 0.5409 0.101 Uiso 0.204(9) 1 calc PR A 3 C28C C 0.3643(10) 0.836(2) 0.5512(8) 0.066(9) Uiso 0.204(9) 1 d PGD A 3 C29C C 0.3225(10) 0.884(2) 0.5825(9) 0.092(9) Uiso 0.204(9) 1 d PGDU A 3 H29C H 0.3243 0.9772 0.5930 0.110 Uiso 0.204(9) 1 d PG A 3 C30C C 0.2779(9) 0.794(3) 0.5985(10) 0.088(9) Uiso 0.204(9) 1 d PGU A 3 H30C H 0.2508 0.8276 0.6205 0.105 Uiso 0.204(9) 1 d PG A 3 C31C C 0.2727(13) 0.658(3) 0.5826(12) 0.178(17) Uiso 0.204(9) 1 d PGU A 3 H31C H 0.2420 0.5982 0.5931 0.213 Uiso 0.204(9) 1 d PG A 3 C32C C 0.3139(16) 0.611(2) 0.5510(12) 0.143(18) Uiso 0.204(9) 1 d PG A 3 H32C H 0.3111 0.5181 0.5396 0.172 Uiso 0.204(9) 1 d PG A 3 C33C C 0.3595(13) 0.698(2) 0.5357(9) 0.097(11) Uiso 0.204(9) 1 d PGD A 3 H33C H 0.3874 0.6636 0.5145 0.116 Uiso 0.204(9) 1 d PG A 3 N1D N 0.3556(11) 0.452(3) 0.4258(10) 0.071(8) Uiso 0.306(11) 1 d PDU B 4 H1D H 0.3690 0.5375 0.4228 0.086 Uiso 0.306(11) 1 calc PR B 4 O1D O 0.6202(7) 0.6866(16) 0.5287(6) 0.081(6) Uiso 0.306(11) 1 d PDU B 4 O2D O 0.3682(10) 0.236(2) 0.4574(8) 0.077(8) Uiso 0.306(11) 1 d PDU B 4 O3D O 0.1994(9) 0.444(3) 0.3964(8) 0.114(8) Uiso 0.306(11) 1 d PDU B 4 O4D O 0.2537(13) 0.558(3) 0.4499(9) 0.096(9) Uiso 0.306(11) 1 d PDU B 4 C1D C 0.6031(14) 0.575(3) 0.6281(6) 0.092(19) Uiso 0.306(11) 1 d PD B 4 C2D C 0.6241(16) 0.543(3) 0.6711(6) 0.100(8) Uiso 0.306(11) 1 d PDU B 4 H2D H 0.6133 0.5949 0.6972 0.120 Uiso 0.306(11) 1 calc PR B 4 C3D C 0.6626(15) 0.428(3) 0.6727(7) 0.097(8) Uiso 0.306(11) 1 d PDU B 4 C4D C 0.6772(13) 0.354(3) 0.6339(7) 0.081(8) Uiso 0.306(11) 1 d PDU B 4 H4D H 0.7030 0.2762 0.6370 0.097 Uiso 0.306(11) 1 calc PR B 4 C5D C 0.6559(16) 0.387(3) 0.5898(7) 0.10(2) Uiso 0.306(11) 1 d PD B 4 C6D C 0.6181(12) 0.504(2) 0.5894(6) 0.072(8) Uiso 0.306(11) 1 d PDU B 4 C7D C 0.5838(6) 0.6003(15) 0.5570(4) 0.077(6) Uiso 0.306(11) 1 d PDU B 4 C23D C 0.3824(15) 0.363(3) 0.4559(14) 0.064(8) Uiso 0.306(11) 1 d PDU B 4 C11D C 0.4369(6) 0.4184(18) 0.4797(5) 0.050(9) Uiso 0.306(11) 1 d PGDU B 4 C12D C 0.4478(6) 0.3776(17) 0.5245(5) 0.099(14) Uiso 0.306(11) 1 d PGD B 4 H12D H 0.4229 0.3102 0.5384 0.118 Uiso 0.306(11) 1 d PG B 4 C13D C 0.4945(6) 0.4342(15) 0.5488(4) 0.067(6) Uiso 0.306(11) 1 d PGD B 4 H13D H 0.5004 0.4059 0.5793 0.080 Uiso 0.306(11) 1 d PG B 4 C8D C 0.5333(5) 0.5328(13) 0.5295(4) 0.042(4) Uiso 0.306(11) 1 d PGDU B 4 C9D C 0.5201(5) 0.5795(13) 0.4862(4) 0.049(4) Uiso 0.306(11) 1 d PGD B 4 H9D H 0.5436 0.6508 0.4730 0.059 Uiso 0.306(11) 1 d PG B 4 C10D C 0.4725(6) 0.5231(16) 0.4614(4) 0.053(6) Uiso 0.306(11) 1 d PGD B 4 H10D H 0.4646 0.5568 0.4319 0.064 Uiso 0.306(11) 1 d PG B 4 C14D C 0.5637(9) 0.686(2) 0.6043(6) 0.109(8) Uiso 0.306(11) 1 d PDU B 4 C15D C 0.5919(16) 0.834(2) 0.6057(11) 0.129(12) Uiso 0.306(11) 1 d PDU B 4 H15J H 0.6322 0.8298 0.5935 0.194 Uiso 0.306(11) 1 calc PR B 4 H15K H 0.5933 0.8672 0.6370 0.194 Uiso 0.306(11) 1 calc PR B 4 H15L H 0.5681 0.8984 0.5875 0.194 Uiso 0.306(11) 1 calc PR B 4 C16D C 0.4992(11) 0.689(4) 0.6191(12) 0.148(15) Uiso 0.306(11) 1 d PDU B 4 H16J H 0.4831 0.5942 0.6183 0.221 Uiso 0.306(11) 1 calc PR B 4 H16K H 0.4765 0.7488 0.5986 0.221 Uiso 0.306(11) 1 calc PR B 4 H16L H 0.4965 0.7259 0.6500 0.221 Uiso 0.306(11) 1 calc PR B 4 C17D C 0.6827(14) 0.373(3) 0.7204(8) 0.154(9) Uiso 0.306(11) 1 d PDU B 4 H17D H 0.6851 0.4547 0.7413 0.184 Uiso 0.306(11) 1 calc PR B 4 C18D C 0.6367(17) 0.274(4) 0.7386(14) 0.139(14) Uiso 0.306(11) 1 d PDU B 4 H18J H 0.5977 0.3002 0.7269 0.208 Uiso 0.306(11) 1 calc PR B 4 H18K H 0.6362 0.2792 0.7718 0.208 Uiso 0.306(11) 1 calc PR B 4 H18L H 0.6462 0.1787 0.7292 0.208 Uiso 0.306(11) 1 calc PR B 4 C19D C 0.7426(13) 0.310(5) 0.7173(15) 0.165(16) Uiso 0.306(11) 1 d PDU B 4 H19J H 0.7725 0.3835 0.7174 0.248 Uiso 0.306(11) 1 calc PR B 4 H19K H 0.7457 0.2558 0.6892 0.248 Uiso 0.306(11) 1 calc PR B 4 H19L H 0.7490 0.2477 0.7432 0.248 Uiso 0.306(11) 1 calc PR B 4 C20D C 0.6645(16) 0.289(3) 0.5489(8) 0.109(8) Uiso 0.306(11) 1 d PDU B 4 H20D H 0.6368 0.3191 0.5244 0.131 Uiso 0.306(11) 1 calc PR B 4 C21D C 0.728(2) 0.297(5) 0.530(2) 0.149(17) Uiso 0.306(11) 1 d PDU B 4 H21J H 0.7413 0.3942 0.5304 0.224 Uiso 0.306(11) 1 calc PR B 4 H21K H 0.7286 0.2610 0.4992 0.224 Uiso 0.306(11) 1 calc PR B 4 H21L H 0.7543 0.2407 0.5492 0.224 Uiso 0.306(11) 1 calc PR B 4 C22D C 0.650(2) 0.136(3) 0.5612(16) 0.149(15) Uiso 0.306(11) 1 d PDU B 4 H22J H 0.6085 0.1285 0.5700 0.223 Uiso 0.306(11) 1 calc PR B 4 H22K H 0.6753 0.1060 0.5864 0.223 Uiso 0.306(11) 1 calc PR B 4 H22L H 0.6575 0.0760 0.5349 0.223 Uiso 0.306(11) 1 calc PR B 4 C24D C 0.3050(8) 0.406(3) 0.3987(7) 0.074(8) Uiso 0.306(11) 1 d PDU B 4 H24D H 0.2998 0.3038 0.4038 0.089 Uiso 0.306(11) 1 calc PR B 4 C25D C 0.2475(8) 0.479(4) 0.4130(9) 0.087(8) Uiso 0.306(11) 1 d PDU B 4 C26D C 0.203(2) 0.644(7) 0.464(2) 0.123(15) Uiso 0.306(11) 1 d PDU B 4 C27D C 0.3158(11) 0.429(3) 0.3473(7) 0.076(7) Uiso 0.306(11) 1 d PDU B 4 H27G H 0.2788 0.4081 0.3307 0.091 Uiso 0.306(11) 1 calc PR B 4 H27H H 0.3253 0.5288 0.3420 0.091 Uiso 0.306(11) 1 calc PR B 4 C28D C 0.3649(8) 0.3410(18) 0.3282(7) 0.069(7) Uiso 0.306(11) 1 d PGDU B 4 C29D C 0.4179(9) 0.4007(16) 0.3134(8) 0.106(10) Uiso 0.306(11) 1 d PGD B 4 H29D H 0.4224 0.4992 0.3139 0.127 Uiso 0.306(11) 1 d PG B 4 C30D C 0.4645(8) 0.317(2) 0.2977(9) 0.113(9) Uiso 0.306(11) 1 d PG B 4 H30D H 0.4995 0.3593 0.2868 0.135 Uiso 0.306(11) 1 d PG B 4 C31D C 0.4601(8) 0.171(2) 0.2979(8) 0.123(10) Uiso 0.306(11) 1 d PG B 4 H31D H 0.4920 0.1146 0.2879 0.147 Uiso 0.306(11) 1 d PG B 4 C32D C 0.4075(9) 0.1112(16) 0.3133(9) 0.102(8) Uiso 0.306(11) 1 d PG B 4 H32D H 0.4037 0.0126 0.3139 0.122 Uiso 0.306(11) 1 d PG B 4 C33D C 0.3603(8) 0.1949(18) 0.3280(8) 0.102(9) Uiso 0.306(11) 1 d PGD B 4 H33D H 0.3247 0.1521 0.3378 0.123 Uiso 0.306(11) 1 d PG B 4 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 N1A 0.065(4) 0.041(3) 0.077(5) 0.002(3) -0.013(4) 0.003(3) O1A 0.086(5) 0.133(7) 0.130(7) -0.059(7) -0.034(5) 0.047(6) O2A 0.080(5) 0.049(4) 0.094(6) -0.011(3) -0.005(3) 0.004(4) O3A 0.062(4) 0.134(6) 0.253(12) 0.048(7) -0.033(5) -0.004(4) O4A 0.091(4) 0.068(5) 0.119(5) 0.004(4) 0.024(4) -0.002(4) C1A 0.075(5) 0.078(6) 0.078(6) 0.001(4) -0.022(4) -0.009(4) C2A 0.094(8) 0.087(6) 0.068(7) 0.018(4) -0.014(4) -0.001(5) C3A 0.084(6) 0.089(6) 0.065(5) -0.002(4) -0.020(4) -0.006(5) C4A 0.095(8) 0.081(5) 0.068(6) -0.003(5) -0.008(5) -0.015(5) C5A 0.069(6) 0.089(8) 0.059(5) 0.000(4) -0.012(4) -0.005(4) C6A 0.058(7) 0.067(8) 0.068(9) -0.004(4) -0.010(4) 0.007(3) C7A 0.063(4) 0.070(4) 0.077(6) -0.011(4) -0.004(4) 0.012(4) C23A 0.058(4) 0.041(4) 0.062(5) 0.002(3) 0.004(3) -0.011(3) C14A 0.111(8) 0.094(6) 0.125(9) 0.012(6) -0.008(7) -0.015(5) C15A 0.140(11) 0.088(7) 0.33(3) 0.009(11) 0.015(14) -0.019(7) C16A 0.137(11) 0.156(11) 0.174(15) 0.029(11) -0.003(10) -0.027(8) C17A 0.125(8) 0.120(7) 0.073(6) -0.006(6) -0.035(6) 0.003(7) C18A 0.208(16) 0.263(19) 0.107(10) -0.088(12) -0.038(10) 0.059(15) C19A 0.198(15) 0.169(13) 0.106(10) 0.021(9) -0.057(11) -0.069(14) C20A 0.089(6) 0.104(6) 0.060(5) 0.009(4) 0.016(4) 0.006(5) C21A 0.104(9) 0.173(12) 0.140(12) 0.052(10) 0.029(8) -0.004(9) C22A 0.162(10) 0.145(10) 0.111(9) 0.069(8) 0.028(8) 0.041(8) C24A 0.068(5) 0.061(4) 0.080(5) -0.004(4) -0.014(4) 0.002(4) C25A 0.064(5) 0.072(5) 0.116(8) -0.015(6) 0.000(5) -0.020(5) C26A 0.091(7) 0.069(7) 0.177(11) -0.004(6) 0.056(7) -0.021(5) C27A 0.086(6) 0.080(5) 0.090(6) -0.015(5) -0.026(5) 0.013(4) N1B 0.068(5) 0.036(3) 0.081(6) -0.002(3) -0.016(4) -0.001(3) O1B 0.093(6) 0.156(9) 0.103(7) 0.059(7) -0.029(5) -0.058(7) O2B 0.056(4) 0.048(3) 0.060(4) -0.003(3) 0.011(4) -0.002(2) O3B 0.060(4) 0.088(5) 0.209(12) -0.019(7) 0.011(5) -0.014(3) O4B 0.075(5) 0.073(5) 0.108(7) -0.011(5) 0.034(4) 0.004(4) C1B 0.070(8) 0.100(11) 0.073(8) -0.008(6) 0.005(5) -0.006(5) C2B 0.117(9) 0.134(10) 0.062(6) -0.016(6) 0.002(6) 0.002(8) C3B 0.104(8) 0.118(9) 0.059(6) 0.001(6) -0.026(5) -0.014(7) C4B 0.083(7) 0.078(7) 0.094(8) 0.025(6) -0.022(6) 0.001(7) C5B 0.078(8) 0.078(7) 0.057(7) -0.005(5) -0.008(5) -0.007(5) C6B 0.060(5) 0.087(7) 0.054(5) 0.018(4) -0.002(4) -0.006(4) C7B 0.080(6) 0.071(5) 0.073(6) 0.025(5) -0.005(5) -0.010(5) C23B 0.064(6) 0.043(5) 0.061(6) -0.004(4) 0.007(4) 0.011(4) C14B 0.106(8) 0.146(10) 0.113(9) 0.018(8) 0.009(8) 0.015(8) C15B 0.146(14) 0.111(11) 0.33(3) 0.021(14) -0.009(18) -0.001(9) C16B 0.081(8) 0.167(12) 0.179(17) 0.026(12) 0.002(9) 0.049(8) C17B 0.142(10) 0.207(13) 0.078(7) 0.039(9) -0.031(7) -0.011(10) C18B 0.216(18) 0.204(19) 0.104(11) 0.073(13) -0.046(12) -0.044(16) C19B 0.138(11) 0.129(11) 0.115(10) 0.013(8) -0.077(9) -0.020(8) C20B 0.137(10) 0.123(9) 0.094(8) -0.018(7) -0.013(8) 0.037(8) C21B 0.123(12) 0.189(19) 0.174(18) -0.037(17) 0.028(12) -0.022(13) C22B 0.136(14) 0.133(11) 0.23(2) -0.071(13) 0.016(14) -0.011(10) C24B 0.057(5) 0.045(4) 0.080(6) -0.004(4) -0.022(4) -0.007(4) C25B 0.071(6) 0.062(6) 0.088(7) 0.003(6) -0.018(5) 0.006(4) C26B 0.092(8) 0.083(8) 0.160(15) -0.009(9) 0.069(9) 0.028(6) C27B 0.058(6) 0.074(5) 0.085(7) 0.009(5) -0.020(5) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1A C23A 1.332(6) . ? N1A C24A 1.446(7) . ? N1A H1A 0.8600 . ? O1A C7A 1.211(7) . ? O2A C23A 1.226(6) . ? O3A C25A 1.177(7) . ? O4A C25A 1.287(8) . ? O4A C26A 1.436(7) . ? C1A C6A 1.385(7) . ? C1A C2A 1.386(7) . ? C1A C14A 1.497(8) . ? C2A C3A 1.362(8) . ? C2A H2A 0.9300 . ? C3A C4A 1.379(8) . ? C3A C17A 1.503(7) . ? C4A C5A 1.405(7) . ? C4A H4A 0.9300 . ? C5A C6A 1.372(7) . ? C5A C20A 1.522(7) . ? C6A C7A 1.509(7) . ? C7A C8A 1.468(6) . ? C23A C11A 1.480(5) . ? C11A C10A 1.3819 . ? C11A C12A 1.3913 . ? C12A C13A 1.3616 . ? C12A H12A 0.9300 . ? C13A C8A 1.3834 . ? C13A H13A 0.9300 . ? C8A C9A 1.3878 . ? C9A C10A 1.3759 . ? C9A H9A 0.9300 . ? C10A H10A 0.9300 . ? C14A C16A 1.514(9) . ? C14A C15A 1.517(9) . ? C14A H14A 0.9800 . ? C15A H15A 0.9600 . ? C15A H15B 0.9600 . ? C15A H15C 0.9600 . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C17A C19A 1.461(9) . ? C17A C18A 1.497(9) . ? C17A H17A 0.9800 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C19A H19A 0.9600 . ? C19A H19B 0.9600 . ? C19A H19C 0.9600 . ? C20A C21A 1.503(9) . ? C20A C22A 1.505(8) . ? C20A H20A 0.9800 . ? C21A H21A 0.9600 . ? C21A H21B 0.9600 . ? C21A H21C 0.9600 . ? C22A H22A 0.9600 . ? C22A H22B 0.9600 . ? C22A H22C 0.9600 . ? C24A C25A 1.500(7) . ? C24A C27A 1.513(8) . ? C24A H24A 0.9800 . ? C26A H26A 0.9600 . ? C26A H26B 0.9600 . ? C26A H26C 0.9600 . ? C27A C28A 1.492(7) . ? C27A H27A 0.9700 . ? C27A H27B 0.9700 . ? C28A C29A 1.3754 . ? C28A C33A 1.3831 . ? C29A C30A 1.3701 . ? C29A H29A 0.9300 . ? C30A C31A 1.3770 . ? C30A H30A 0.9300 . ? C31A C32A 1.3617 . ? C31A H31A 0.9301 . ? C32A C33A 1.3726 . ? C32A H32A 0.9300 . ? C33A H33A 0.9300 . ? N1B C23B 1.322(7) . ? N1B C24B 1.437(7) . ? N1B H1B 0.8600 . ? O1B C7B 1.214(7) . ? O2B C23B 1.230(7) . ? O3B C25B 1.185(7) . ? O4B C25B 1.296(8) . ? O4B C26B 1.453(8) . ? C1B C2B 1.383(8) . ? C1B C6B 1.395(8) . ? C1B C14B 1.498(8) . ? C2B C3B 1.369(8) . ? C2B H2B 0.9300 . ? C3B C4B 1.363(8) . ? C3B C17B 1.500(8) . ? C4B C5B 1.399(8) . ? C4B H4B 0.9300 . ? C5B C6B 1.372(7) . ? C5B C20B 1.516(8) . ? C6B C7B 1.490(7) . ? C7B C8B 1.475(6) . ? C23B C11B 1.485(6) . ? C11B C10B 1.3820 . ? C11B C12B 1.3912 . ? C12B C13B 1.3616 . ? C12B H12B 0.9300 . ? C13B C8B 1.3834 . ? C13B H13B 0.9300 . ? C8B C9B 1.3878 . ? C9B C10B 1.3759 . ? C9B H9B 0.9300 . ? C10B H10B 0.9300 . ? C14B C15B 1.499(10) . ? C14B C16B 1.517(9) . ? C14B H14B 0.9800 . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? C17B C19B 1.438(9) . ? C17B C18B 1.479(9) . ? C17B H17B 0.9800 . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? C19B H19D 0.9600 . ? C19B H19E 0.9600 . ? C19B H19F 0.9600 . ? C20B C21B 1.497(9) . ? C20B C22B 1.528(9) . ? C20B H20B 0.9800 . ? C21B H21D 0.9600 . ? C21B H21E 0.9600 . ? C21B H21F 0.9600 . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? C24B C25B 1.514(7) . ? C24B C27B 1.525(8) . ? C24B H24B 0.9800 . ? C26B H26D 0.9600 . ? C26B H26E 0.9600 . ? C26B H26F 0.9600 . ? C27B C28B 1.481(7) . ? C27B H27C 0.9700 . ? C27B H27D 0.9700 . ? C28B C29B 1.3754 . ? C28B C33B 1.3831 . ? C29B C30B 1.3701 . ? C29B H29B 0.9300 . ? C30B C31B 1.3771 . ? C30B H30B 0.9300 . ? C31B C32B 1.3617 . ? C31B H31B 0.9300 . ? C32B C33B 1.3726 . ? C32B H32B 0.9300 . ? C33B H33B 0.9300 . ? N1C C23C 1.349(10) . ? N1C C24C 1.427(10) . ? N1C H1C 0.8600 . ? O1C C7C 1.407(9) . ? O2C C23C 1.234(10) . ? O3C C25C 1.217(10) . ? O4C C25C 1.313(10) . ? O4C C26C 1.434(10) . ? C1C C6C 1.353(9) . ? C1C C2C 1.368(9) . ? C1C C14C 1.524(9) . ? C2C C3C 1.382(9) . ? C2C H2C 0.9300 . ? C3C C4C 1.366(9) . ? C3C C17C 1.537(9) . ? C4C C5C 1.401(9) . ? C4C H4C 0.9300 . ? C5C C6C 1.378(9) . ? C5C C20C 1.517(9) . ? C6C C7C 1.518(9) . ? C7C C8C 1.513(8) . ? C7C C14C 1.654(10) . ? C23C C11C 1.484(9) . ? C11C C10C 1.3671 . ? C11C C12C 1.3750 . ? C12C C13C 1.3582 . ? C12C H12C 0.9301 . ? C13C C8C 1.3818 . ? C13C H13C 0.9300 . ? C8C C9C 1.3608 . ? C9C C10C 1.3794 . ? C9C H9C 0.9300 . ? C10C H10C 0.9300 . ? C14C C16C 1.492(9) . ? C14C C15C 1.525(10) . ? C15C H15G 0.9600 . ? C15C H15H 0.9600 . ? C15C H15I 0.9600 . ? C16C H16G 0.9600 . ? C16C H16H 0.9600 . ? C16C H16I 0.9600 . ? C17C C19C 1.461(11) . ? C17C C18C 1.479(10) . ? C17C H17C 0.9800 . ? C18C H18G 0.9600 . ? C18C H18H 0.9600 . ? C18C H18I 0.9600 . ? C19C H19G 0.9600 . ? C19C H19H 0.9600 . ? C19C H19I 0.9600 . ? C20C C21C 1.511(10) . ? C20C C22C 1.514(10) . ? C20C H20C 0.9800 . ? C21C H21G 0.9600 . ? C21C H21H 0.9600 . ? C21C H21I 0.9600 . ? C22C H22G 0.9600 . ? C22C H22H 0.9600 . ? C22C H22I 0.9600 . ? C24C C25C 1.487(9) . ? C24C C27C 1.517(10) . ? C24C H24C 0.9800 . ? C27C C28C 1.478(9) . ? C27C H27E 0.9700 . ? C27C H27F 0.9700 . ? C28C C29C 1.3689 . ? C28C C33C 1.3759 . ? C29C C30C 1.3762 . ? C29C H29C 0.9300 . ? C30C C31C 1.3694 . ? C30C H30C 0.9300 . ? C31C C32C 1.3674 . ? C31C H31C 0.9300 . ? C32C C33C 1.3744 . ? C32C H32C 0.9300 . ? C33C H33C 0.9299 . ? N1D C23D 1.343(9) . ? N1D C24D 1.433(10) . ? N1D H1D 0.8600 . ? O1D C7D 1.408(9) . ? O2D C23D 1.233(10) . ? O3D C25D 1.213(10) . ? O4D C25D 1.311(10) . ? O4D C26D 1.437(10) . ? C1D C6D 1.350(9) . ? C1D C2D 1.363(9) . ? C1D C14D 1.523(9) . ? C2D C3D 1.379(9) . ? C2D H2D 0.9300 . ? C3D C4D 1.360(9) . ? C3D C17D 1.538(9) . ? C4D C5D 1.398(9) . ? C4D H4D 0.9300 . ? C5D C6D 1.380(9) . ? C5D C20D 1.512(9) . ? C6D C7D 1.508(9) . ? C7D C8D 1.512(8) . ? C7D C14D 1.649(9) . ? C23D C11D 1.483(8) . ? C11D C10D 1.3671 . ? C11D C12D 1.3750 . ? C12D C13D 1.3583 . ? C12D H12D 0.9301 . ? C13D C8D 1.3817 . ? C13D H13D 0.9299 . ? C8D C9D 1.3608 . ? C9D C10D 1.3794 . ? C9D H9D 0.9300 . ? C10D H10D 0.9300 . ? C14D C16D 1.490(9) . ? C14D C15D 1.524(10) . ? C15D H15J 0.9600 . ? C15D H15K 0.9600 . ? C15D H15L 0.9600 . ? C16D H16J 0.9600 . ? C16D H16K 0.9600 . ? C16D H16L 0.9600 . ? C17D C19D 1.456(10) . ? C17D C18D 1.477(10) . ? C17D H17D 0.9800 . ? C18D H18J 0.9600 . ? C18D H18K 0.9600 . ? C18D H18L 0.9600 . ? C19D H19J 0.9600 . ? C19D H19K 0.9600 . ? C19D H19L 0.9600 . ? C20D C21D 1.505(10) . ? C20D C22D 1.515(10) . ? C20D H20D 0.9800 . ? C21D H21J 0.9600 . ? C21D H21K 0.9600 . ? C21D H21L 0.9600 . ? C22D H22J 0.9600 . ? C22D H22K 0.9600 . ? C22D H22L 0.9600 . ? C24D C25D 1.502(10) . ? C24D C27D 1.525(10) . ? C24D H24D 0.9800 . ? C27D C28D 1.475(9) . ? C27D H27G 0.9700 . ? C27D H27H 0.9700 . ? C28D C29D 1.3689 . ? C28D C33D 1.3759 . ? C29D C30D 1.3762 . ? C29D H29D 0.9300 . ? C30D C31D 1.3694 . ? C30D H30D 0.9300 . ? C31D C32D 1.3674 . ? C31D H31D 0.9300 . ? C32D C33D 1.3744 . ? C32D H32D 0.9300 . ? C33D H33D 0.9299 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23A N1A C24A 122.4(6) . . ? C23A N1A H1A 118.8 . . ? C24A N1A H1A 118.8 . . ? C25A O4A C26A 117.7(8) . . ? C6A C1A C2A 117.6(6) . . ? C6A C1A C14A 122.5(7) . . ? C2A C1A C14A 119.9(7) . . ? C3A C2A C1A 122.9(7) . . ? C3A C2A H2A 118.6 . . ? C1A C2A H2A 118.6 . . ? C2A C3A C4A 118.8(6) . . ? C2A C3A C17A 120.7(7) . . ? C4A C3A C17A 120.6(7) . . ? C3A C4A C5A 120.2(6) . . ? C3A C4A H4A 119.9 . . ? C5A C4A H4A 119.9 . . ? C6A C5A C4A 119.3(6) . . ? C6A C5A C20A 121.3(6) . . ? C4A C5A C20A 119.4(6) . . ? C5A C6A C1A 121.2(6) . . ? C5A C6A C7A 118.4(6) . . ? C1A C6A C7A 120.4(7) . . ? O1A C7A C8A 119.9(6) . . ? O1A C7A C6A 120.9(6) . . ? C8A C7A C6A 119.1(5) . . ? O2A C23A N1A 122.4(7) . . ? O2A C23A C11A 121.1(6) . . ? N1A C23A C11A 116.4(5) . . ? C10A C11A C12A 118.3 . . ? C10A C11A C23A 124.5(4) . . ? C12A C11A C23A 117.1(4) . . ? C13A C12A C11A 120.3 . . ? C12A C13A C8A 121.5 . . ? C13A C8A C9A 118.5 . . ? C13A C8A C7A 121.4(4) . . ? C9A C8A C7A 120.1(4) . . ? C10A C9A C8A 120.0 . . ? C9A C10A C11A 121.3 . . ? C1A C14A C16A 112.4(8) . . ? C1A C14A C15A 110.6(8) . . ? C16A C14A C15A 109.7(9) . . ? C1A C14A H14A 108.0 . . ? C16A C14A H14A 108.0 . . ? C15A C14A H14A 108.0 . . ? C14A C15A H15A 109.5 . . ? C14A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C14A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C14A C16A H16A 109.5 . . ? C14A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C14A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C19A C17A C18A 113.3(11) . . ? C19A C17A C3A 115.5(9) . . ? C18A C17A C3A 110.5(8) . . ? C19A C17A H17A 105.6 . . ? C18A C17A H17A 105.6 . . ? C3A C17A H17A 105.6 . . ? C17A C18A H18A 109.5 . . ? C17A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C17A C19A H19A 109.5 . . ? C17A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C17A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C21A C20A C22A 112.3(8) . . ? C21A C20A C5A 111.5(9) . . ? C22A C20A C5A 111.3(8) . . ? C21A C20A H20A 107.1 . . ? C22A C20A H20A 107.1 . . ? C5A C20A H20A 107.1 . . ? C20A C21A H21A 109.5 . . ? C20A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C20A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C20A C22A H22A 109.5 . . ? C20A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C20A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? N1A C24A C25A 113.5(6) . . ? N1A C24A C27A 111.2(6) . . ? C25A C24A C27A 110.8(6) . . ? N1A C24A H24A 107.0 . . ? C25A C24A H24A 107.0 . . ? C27A C24A H24A 107.0 . . ? O3A C25A O4A 125.9(7) . . ? O3A C25A C24A 119.8(7) . . ? O4A C25A C24A 113.9(6) . . ? C28A C27A C24A 112.8(6) . . ? C28A C27A H27A 109.0 . . ? C24A C27A H27A 109.0 . . ? C28A C27A H27B 109.0 . . ? C24A C27A H27B 109.0 . . ? H27A C27A H27B 107.8 . . ? C29A C28A C33A 117.2 . . ? C29A C28A C27A 120.1(5) . . ? C33A C28A C27A 122.7(5) . . ? C30A C29A C28A 121.3 . . ? C29A C30A C31A 121.0 . . ? C32A C31A C30A 118.1 . . ? C31A C32A C33A 121.2 . . ? C32A C33A C28A 121.2 . . ? C23B N1B C24B 122.8(7) . . ? C23B N1B H1B 118.6 . . ? C24B N1B H1B 118.6 . . ? C25B O4B C26B 116.4(10) . . ? C2B C1B C6B 117.9(7) . . ? C2B C1B C14B 122.6(9) . . ? C6B C1B C14B 119.4(8) . . ? C3B C2B C1B 122.8(8) . . ? C3B C2B H2B 118.6 . . ? C1B C2B H2B 118.6 . . ? C4B C3B C2B 117.5(7) . . ? C4B C3B C17B 122.5(9) . . ? C2B C3B C17B 120.0(9) . . ? C3B C4B C5B 122.9(8) . . ? C3B C4B H4B 118.5 . . ? C5B C4B H4B 118.5 . . ? C6B C5B C4B 117.7(7) . . ? C6B C5B C20B 121.2(7) . . ? C4B C5B C20B 121.2(8) . . ? C5B C6B C1B 121.3(6) . . ? C5B C6B C7B 119.5(7) . . ? C1B C6B C7B 119.2(7) . . ? O1B C7B C8B 119.6(6) . . ? O1B C7B C6B 120.4(7) . . ? C8B C7B C6B 119.6(6) . . ? O2B C23B N1B 123.0(7) . . ? O2B C23B C11B 120.5(6) . . ? N1B C23B C11B 116.5(6) . . ? C10B C11B C12B 118.3 . . ? C10B C11B C23B 123.7(5) . . ? C12B C11B C23B 118.0(5) . . ? C13B C12B C11B 120.3 . . ? C13B C12B H12B 119.8 . . ? C11B C12B H12B 119.8 . . ? C12B C13B C8B 121.5 . . ? C12B C13B H13B 119.2 . . ? C8B C13B H13B 119.2 . . ? C13B C8B C9B 118.5 . . ? C13B C8B C7B 121.3(4) . . ? C9B C8B C7B 120.2(4) . . ? C10B C9B C8B 120.0 . . ? C10B C9B H9B 120.0 . . ? C8B C9B H9B 120.0 . . ? C9B C10B C11B 121.3 . . ? C9B C10B H10B 119.3 . . ? C11B C10B H10B 119.3 . . ? C1B C14B C15B 111.8(10) . . ? C1B C14B C16B 113.3(9) . . ? C15B C14B C16B 111.0(11) . . ? C1B C14B H14B 106.8 . . ? C15B C14B H14B 106.8 . . ? C16B C14B H14B 106.8 . . ? C14B C15B H15D 109.5 . . ? C14B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C14B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C14B C16B H16D 109.5 . . ? C14B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C14B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C19B C17B C18B 119.6(11) . . ? C19B C17B C3B 115.9(9) . . ? C18B C17B C3B 112.4(9) . . ? C19B C17B H17B 101.8 . . ? C18B C17B H17B 101.8 . . ? C3B C17B H17B 101.8 . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C17B C19B H19D 109.5 . . ? C17B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C17B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C21B C20B C5B 112.3(10) . . ? C21B C20B C22B 110.4(11) . . ? C5B C20B C22B 109.5(10) . . ? C21B C20B H20B 108.2 . . ? C5B C20B H20B 108.2 . . ? C22B C20B H20B 108.2 . . ? C20B C21B H21D 109.5 . . ? C20B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C20B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C20B C22B H22D 109.5 . . ? C20B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C20B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? N1B C24B C25B 113.2(7) . . ? N1B C24B C27B 111.5(7) . . ? C25B C24B C27B 110.2(7) . . ? N1B C24B H24B 107.2 . . ? C25B C24B H24B 107.2 . . ? C27B C24B H24B 107.2 . . ? O3B C25B O4B 124.5(8) . . ? O3B C25B C24B 123.2(7) . . ? O4B C25B C24B 112.2(7) . . ? O4B C26B H26D 109.5 . . ? O4B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? O4B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C28B C27B C24B 113.6(7) . . ? C28B C27B H27C 108.9 . . ? C24B C27B H27C 108.9 . . ? C28B C27B H27D 108.9 . . ? C24B C27B H27D 108.9 . . ? H27C C27B H27D 107.7 . . ? C29B C28B C33B 117.2 . . ? C29B C28B C27B 122.6(6) . . ? C33B C28B C27B 120.1(6) . . ? C30B C29B C28B 121.3 . . ? C30B C29B H29B 119.3 . . ? C28B C29B H29B 119.3 . . ? C29B C30B C31B 121.0 . . ? C29B C30B H30B 119.5 . . ? C31B C30B H30B 119.5 . . ? C32B C31B C30B 118.1 . . ? C32B C31B H31B 120.9 . . ? C30B C31B H31B 120.9 . . ? C31B C32B C33B 121.2 . . ? C31B C32B H32B 119.4 . . ? C33B C32B H32B 119.4 . . ? C32B C33B C28B 121.2 . . ? C32B C33B H33B 119.4 . . ? C28B C33B H33B 119.4 . . ? C23C N1C C24C 122.3(18) . . ? C23C N1C H1C 118.8 . . ? C24C N1C H1C 118.8 . . ? C25C O4C C26C 116.7(18) . . ? C6C C1C C2C 122.6(11) . . ? C6C C1C C14C 95.2(9) . . ? C2C C1C C14C 142.2(12) . . ? C1C C2C C3C 116.5(12) . . ? C1C C2C H2C 121.7 . . ? C3C C2C H2C 121.7 . . ? C4C C3C C2C 120.7(11) . . ? C4C C3C C17C 118.8(13) . . ? C2C C3C C17C 120.5(13) . . ? C3C C4C C5C 123.2(12) . . ? C3C C4C H4C 118.4 . . ? C5C C4C H4C 118.4 . . ? C6C C5C C4C 114.0(11) . . ? C6C C5C C20C 124.6(13) . . ? C4C C5C C20C 121.3(12) . . ? C1C C6C C5C 122.9(10) . . ? C1C C6C C7C 96.0(9) . . ? C5C C6C C7C 141.1(11) . . ? O1C C7C C8C 110.6(12) . . ? O1C C7C C6C 113.3(14) . . ? C8C C7C C6C 117.2(13) . . ? O1C C7C C14C 111.8(12) . . ? C8C C7C C14C 117.6(15) . . ? C6C C7C C14C 84.2(7) . . ? O2C C23C N1C 121.7(18) . . ? O2C C23C C11C 121.7(18) . . ? N1C C23C C11C 114.7(12) . . ? C10C C11C C12C 117.6 . . ? C10C C11C C23C 122.7(9) . . ? C12C C11C C23C 119.4(10) . . ? C13C C12C C11C 120.9 . . ? C12C C13C C8C 121.7 . . ? C9C C8C C13C 117.1 . . ? C9C C8C C7C 121.6(8) . . ? C13C C8C C7C 120.9(8) . . ? C8C C9C C10C 121.2 . . ? C11C C10C C9C 121.1 . . ? C16C C14C C1C 115.7(13) . . ? C16C C14C C15C 110.8(12) . . ? C1C C14C C15C 113.8(14) . . ? C16C C14C C7C 119.8(14) . . ? C1C C14C C7C 84.4(7) . . ? C15C C14C C7C 110.2(13) . . ? C14C C15C H15G 109.5 . . ? C14C C15C H15H 109.5 . . ? H15G C15C H15H 109.5 . . ? C14C C15C H15I 109.5 . . ? H15G C15C H15I 109.5 . . ? H15H C15C H15I 109.5 . . ? C14C C16C H16G 109.5 . . ? C14C C16C H16H 109.5 . . ? H16G C16C H16H 109.5 . . ? C14C C16C H16I 109.5 . . ? H16G C16C H16I 109.5 . . ? H16H C16C H16I 109.5 . . ? C19C C17C C18C 111.9(16) . . ? C19C C17C C3C 111.8(16) . . ? C18C C17C C3C 109.9(15) . . ? C19C C17C H17C 107.7 . . ? C18C C17C H17C 107.7 . . ? C3C C17C H17C 107.7 . . ? C17C C18C H18G 109.5 . . ? C17C C18C H18H 109.5 . . ? H18G C18C H18H 109.5 . . ? C17C C18C H18I 109.5 . . ? H18G C18C H18I 109.5 . . ? H18H C18C H18I 109.5 . . ? C17C C19C H19G 109.5 . . ? C17C C19C H19H 109.5 . . ? H19G C19C H19H 109.5 . . ? C17C C19C H19I 109.5 . . ? H19G C19C H19I 109.5 . . ? H19H C19C H19I 109.5 . . ? C21C C20C C22C 108.4(15) . . ? C21C C20C C5C 110.7(15) . . ? C22C C20C C5C 110.1(15) . . ? C21C C20C H20C 109.2 . . ? C22C C20C H20C 109.2 . . ? C5C C20C H20C 109.2 . . ? C20C C21C H21G 109.5 . . ? C20C C21C H21H 109.5 . . ? H21G C21C H21H 109.5 . . ? C20C C21C H21I 109.5 . . ? H21G C21C H21I 109.5 . . ? H21H C21C H21I 109.5 . . ? C20C C22C H22G 109.5 . . ? C20C C22C H22H 109.5 . . ? H22G C22C H22H 109.5 . . ? C20C C22C H22I 109.5 . . ? H22G C22C H22I 109.5 . . ? H22H C22C H22I 109.5 . . ? N1C C24C C25C 116.2(16) . . ? N1C C24C C27C 112.4(15) . . ? C25C C24C C27C 112.2(13) . . ? N1C C24C H24C 104.9 . . ? C25C C24C H24C 104.9 . . ? C27C C24C H24C 104.9 . . ? O3C C25C O4C 120.6(16) . . ? O3C C25C C24C 122.5(15) . . ? O4C C25C C24C 116.1(14) . . ? C28C C27C C24C 114.0(14) . . ? C28C C27C H27E 108.8 . . ? C24C C27C H27E 108.8 . . ? C28C C27C H27F 108.8 . . ? C24C C27C H27F 108.8 . . ? H27E C27C H27F 107.7 . . ? C29C C28C C33C 118.1 . . ? C29C C28C C27C 120.7(11) . . ? C33C C28C C27C 121.3(11) . . ? C28C C29C C30C 120.7 . . ? C31C C30C C29C 121.2 . . ? C32C C31C C30C 118.1 . . ? C31C C32C C33C 120.9 . . ? C32C C33C C28C 121.0 . . ? C23D N1D C24D 120.9(15) . . ? C23D N1D H1D 119.6 . . ? C24D N1D H1D 119.6 . . ? C25D O4D C26D 117.6(17) . . ? C6D C1D C2D 124.4(11) . . ? C6D C1D C14D 96.0(8) . . ? C2D C1D C14D 139.6(12) . . ? C1D C2D C3D 114.6(11) . . ? C1D C2D H2D 122.7 . . ? C3D C2D H2D 122.7 . . ? C4D C3D C2D 121.3(11) . . ? C4D C3D C17D 120.0(12) . . ? C2D C3D C17D 118.2(12) . . ? C3D C4D C5D 124.2(12) . . ? C3D C4D H4D 117.9 . . ? C5D C4D H4D 117.9 . . ? C6D C5D C4D 112.9(10) . . ? C6D C5D C20D 123.6(13) . . ? C4D C5D C20D 122.6(12) . . ? C1D C6D C5D 122.6(10) . . ? C1D C6D C7D 95.3(8) . . ? C5D C6D C7D 142.1(11) . . ? O1D C7D C6D 114.7(12) . . ? O1D C7D C8D 110.9(10) . . ? C6D C7D C8D 116.6(11) . . ? O1D C7D C14D 111.0(10) . . ? C6D C7D C14D 85.1(7) . . ? C8D C7D C14D 116.3(12) . . ? O2D C23D N1D 120.8(14) . . ? O2D C23D C11D 121.9(15) . . ? N1D C23D C11D 116.2(11) . . ? C10D C11D C12D 117.6 . . ? C10D C11D C23D 122.8(9) . . ? C12D C11D C23D 119.0(11) . . ? C13D C12D C11D 120.9 . . ? C12D C13D C8D 121.7 . . ? C9D C8D C13D 117.1 . . ? C9D C8D C7D 120.6(7) . . ? C13D C8D C7D 121.8(7) . . ? C8D C9D C10D 121.2 . . ? C11D C10D C9D 121.1 . . ? C16D C14D C1D 115.5(13) . . ? C16D C14D C15D 111.7(12) . . ? C1D C14D C15D 112.0(13) . . ? C16D C14D C7D 120.4(14) . . ? C1D C14D C7D 83.6(7) . . ? C15D C14D C7D 110.9(11) . . ? C14D C15D H15J 109.5 . . ? C14D C15D H15K 109.5 . . ? H15J C15D H15K 109.5 . . ? C14D C15D H15L 109.5 . . ? H15J C15D H15L 109.5 . . ? H15K C15D H15L 109.5 . . ? C14D C16D H16J 109.5 . . ? C14D C16D H16K 109.5 . . ? H16J C16D H16K 109.5 . . ? C14D C16D H16L 109.5 . . ? H16J C16D H16L 109.5 . . ? H16K C16D H16L 109.5 . . ? C19D C17D C18D 113.2(16) . . ? C19D C17D C3D 110.2(14) . . ? C18D C17D C3D 109.4(15) . . ? C19D C17D H17D 108.0 . . ? C18D C17D H17D 108.0 . . ? C3D C17D H17D 108.0 . . ? C17D C18D H18J 109.5 . . ? C17D C18D H18K 109.5 . . ? H18J C18D H18K 109.5 . . ? C17D C18D H18L 109.5 . . ? H18J C18D H18L 109.5 . . ? H18K C18D H18L 109.5 . . ? C17D C19D H19J 109.5 . . ? C17D C19D H19K 109.5 . . ? H19J C19D H19K 109.5 . . ? C17D C19D H19L 109.5 . . ? H19J C19D H19L 109.5 . . ? H19K C19D H19L 109.5 . . ? C21D C20D C5D 111.6(15) . . ? C21D C20D C22D 109.1(14) . . ? C5D C20D C22D 111.5(14) . . ? C21D C20D H20D 108.2 . . ? C5D C20D H20D 108.2 . . ? C22D C20D H20D 108.2 . . ? C20D C21D H21J 109.5 . . ? C20D C21D H21K 109.5 . . ? H21J C21D H21K 109.5 . . ? C20D C21D H21L 109.5 . . ? H21J C21D H21L 109.5 . . ? H21K C21D H21L 109.5 . . ? C20D C22D H22J 109.5 . . ? C20D C22D H22K 109.5 . . ? H22J C22D H22K 109.5 . . ? C20D C22D H22L 109.5 . . ? H22J C22D H22L 109.5 . . ? H22K C22D H22L 109.5 . . ? N1D C24D C25D 112.1(14) . . ? N1D C24D C27D 111.8(14) . . ? C25D C24D C27D 109.6(13) . . ? N1D C24D H24D 107.7 . . ? C25D C24D H24D 107.7 . . ? C27D C24D H24D 107.7 . . ? O3D C25D O4D 124.4(14) . . ? O3D C25D C24D 121.0(14) . . ? O4D C25D C24D 113.2(13) . . ? C28D C27D C24D 113.6(13) . . ? C28D C27D H27G 108.8 . . ? C24D C27D H27G 108.8 . . ? C28D C27D H27H 108.8 . . ? C24D C27D H27H 108.8 . . ? H27G C27D H27H 107.7 . . ? C29D C28D C33D 118.1 . . ? C29D C28D C27D 121.3(10) . . ? C33D C28D C27D 120.5(10) . . ? C28D C29D C30D 120.7 . . ? C31D C30D C29D 121.2 . . ? C32D C31D C30D 118.1 . . ? C31D C32D C33D 120.9 . . ? C32D C33D C28D 121.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.175 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.035 #===END data_25.5%C,54.9%D _database_code_depnum_ccdc_archive 'CCDC 799267' #TrackingRef '- 1.cif' #==================================================================== # start Validation Reply Form _vrf_PLAT201_25.5%C,54.9%D ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 36 RESPONSE: In the crystal there are reactant and photoproduct molecules. Part of atoms were refined isotropically in order to decrease a large number of the parameters in the refinement. ; _vrf_PLAT220_25.5%C,54.9%D ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.25 Ratio RESPONSE: This is a consequence of the strong reactant-product disorder in the crystal. ; # end Validation Reply Form #==================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 N O4' _chemical_formula_weight 513.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 22.179(4) _cell_length_b 9.3739(17) _cell_length_c 28.978(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6025(2) _cell_formula_units_Z 8 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 3.66 _cell_measurement_theta_max 13.18 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28066 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5393 _reflns_number_gt 3402 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSALIS (Oxford Diffraction, 2003)' _computing_cell_refinement 'CRYSALIS (Oxford Diffraction, 2003)' _computing_data_reduction 'CRYSALIS (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SXELXL97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Owing to a reactant-product disorder, the following weak restraints from SHELXL97 were applied: DFIX, DANG and SIMU. DFIX and DANG restrained bond lengths and valence angles to target values. The target values were taken from the structures of the pure reactant and the pure product of crystal 1a. SIMU restrained displacement parameters of atoms of the products. ; _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^)+(0.1554P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5393 _refine_ls_number_parameters 718 _refine_ls_number_restraints 578 _refine_ls_R_factor_all 0.1307 _refine_ls_R_factor_gt 0.0878 _refine_ls_wR_factor_ref 0.2715 _refine_ls_wR_factor_gt 0.2321 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.154 _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 N1A N 0.3867(4) 0.9483(11) 0.4482(4) 0.064(3) Uani 0.745(10) 1 d PDU A 1 H1A H 0.3731 1.0339 0.4507 0.077 Uiso 0.745(10) 1 calc PR A 1 O1A O 0.1012(5) 1.1039(15) 0.3548(5) 0.121(5) Uani 0.745(10) 1 d PDU A 1 O2A O 0.3825(11) 0.7448(18) 0.4078(9) 0.076(6) Uani 0.745(10) 1 d PDU A 1 O3A O 0.5434(4) 0.9359(12) 0.4736(6) 0.143(4) Uani 0.745(10) 1 d PDU A 1 O4A O 0.4875(5) 1.0870(14) 0.4344(5) 0.096(3) Uani 0.745(10) 1 d PDU A 1 C1A C 0.1328(5) 1.0399(11) 0.2487(3) 0.085(5) Uiso 0.745(10) 1 d PD A 1 C2A C 0.1157(5) 0.9799(12) 0.2072(3) 0.093(5) Uiso 0.745(10) 1 d PD A 1 H2A H 0.1229 1.0308 0.1802 0.112 Uiso 0.745(10) 1 calc PR A 1 C3A C 0.0886(6) 0.8494(11) 0.2038(3) 0.087(4) Uiso 0.745(10) 1 d PDU A 1 C4A C 0.0788(6) 0.7739(11) 0.2440(3) 0.082(4) Uiso 0.745(10) 1 d PD A 1 H4A H 0.0616 0.6835 0.2425 0.098 Uiso 0.745(10) 1 calc PR A 1 C5A C 0.0942(5) 0.8316(9) 0.2872(3) 0.075(3) Uiso 0.745(10) 1 d PDU A 1 C6A C 0.1209(5) 0.9641(10) 0.2886(3) 0.072(5) Uiso 0.745(10) 1 d PDU A 1 C7A C 0.1369(4) 1.0274(10) 0.3348(3) 0.074(3) Uani 0.745(10) 1 d PDU A 1 C23A C 0.3594(6) 0.8578(13) 0.4196(5) 0.060(3) Uani 0.745(10) 1 d PDU A 1 C11A C 0.3014(3) 0.9061(8) 0.3995(3) 0.058(4) Uiso 0.745(10) 1 d PGDU A 1 C12A C 0.2862(3) 0.8540(8) 0.3561(3) 0.063(3) Uiso 0.745(10) 1 d PGDU A 1 H12A H 0.3121 0.7917 0.3409 0.076 Uiso 0.745(10) 1 d PG A 1 C13A C 0.2336(3) 0.8937(7) 0.3357(2) 0.068(3) Uiso 0.745(10) 1 d PGD A 1 H13A H 0.2241 0.8577 0.3067 0.082 Uiso 0.745(10) 1 d PG A 1 C8A C 0.1939(3) 0.9864(7) 0.3570(3) 0.061(2) Uiso 0.745(10) 1 d PGDU A 1 C9A C 0.2088(3) 1.0391(7) 0.4003(2) 0.069(2) Uiso 0.745(10) 1 d PGDU A 1 H9A H 0.1827 1.1013 0.4154 0.082 Uiso 0.745(10) 1 d PG A 1 C10A C 0.2620(3) 0.9992(8) 0.4209(2) 0.067(3) Uiso 0.745(10) 1 d PGDU A 1 H10A H 0.2717 1.0357 0.4497 0.080 Uiso 0.745(10) 1 d PG A 1 C14A C 0.1679(5) 1.1756(11) 0.2494(5) 0.116(4) Uani 0.745(10) 1 d PDU A 1 H14A H 0.1779 1.1958 0.2817 0.139 Uiso 0.745(10) 1 calc PR A 1 C15A C 0.1288(7) 1.2967(14) 0.2324(11) 0.197(10) Uani 0.745(10) 1 d PDU A 1 H15A H 0.1519 1.3834 0.2320 0.295 Uiso 0.745(10) 1 calc PR A 1 H15B H 0.0948 1.3078 0.2526 0.295 Uiso 0.745(10) 1 calc PR A 1 H15C H 0.1149 1.2758 0.2017 0.295 Uiso 0.745(10) 1 calc PR A 1 C16A C 0.2268(6) 1.1692(19) 0.2230(8) 0.156(6) Uani 0.745(10) 1 d PDU A 1 H16A H 0.2459 1.2610 0.2238 0.235 Uiso 0.745(10) 1 calc PR A 1 H16B H 0.2189 1.1430 0.1915 0.235 Uiso 0.745(10) 1 calc PR A 1 H16C H 0.2528 1.0995 0.2368 0.235 Uiso 0.745(10) 1 calc PR A 1 C17A C 0.0718(6) 0.7895(16) 0.1576(4) 0.114(4) Uani 0.745(10) 1 d PDU A 1 H17A H 0.0652 0.8735 0.1381 0.137 Uiso 0.745(10) 1 calc PR A 1 C18A C 0.1244(8) 0.715(3) 0.1361(6) 0.190(9) Uani 0.745(10) 1 d PDU A 1 H18A H 0.1597 0.7742 0.1388 0.285 Uiso 0.745(10) 1 calc PR A 1 H18B H 0.1162 0.6977 0.1041 0.285 Uiso 0.745(10) 1 calc PR A 1 H18C H 0.1313 0.6262 0.1516 0.285 Uiso 0.745(10) 1 calc PR A 1 C19A C 0.0152(9) 0.712(3) 0.1556(7) 0.171(8) Uani 0.745(10) 1 d PDU A 1 H19A H 0.0081 0.6799 0.1246 0.257 Uiso 0.745(10) 1 calc PR A 1 H19B H -0.0172 0.7730 0.1651 0.257 Uiso 0.745(10) 1 calc PR A 1 H19C H 0.0171 0.6306 0.1758 0.257 Uiso 0.745(10) 1 calc PR A 1 C20A C 0.0817(5) 0.7481(10) 0.3309(3) 0.082(3) Uani 0.745(10) 1 d PDU A 1 H20A H 0.1011 0.8006 0.3561 0.099 Uiso 0.745(10) 1 calc PR A 1 C21A C 0.0160(6) 0.740(2) 0.3426(7) 0.135(6) Uani 0.745(10) 1 d PDU A 1 H21A H -0.0046 0.8206 0.3293 0.203 Uiso 0.745(10) 1 calc PR A 1 H21B H 0.0111 0.7421 0.3755 0.203 Uiso 0.745(10) 1 calc PR A 1 H21C H -0.0007 0.6537 0.3305 0.203 Uiso 0.745(10) 1 calc PR A 1 C22A C 0.1115(7) 0.6039(14) 0.3293(6) 0.147(6) Uani 0.745(10) 1 d PDU A 1 H22A H 0.1543 0.6151 0.3328 0.221 Uiso 0.745(10) 1 calc PR A 1 H22B H 0.1031 0.5594 0.3001 0.221 Uiso 0.745(10) 1 calc PR A 1 H22C H 0.0961 0.5454 0.3538 0.221 Uiso 0.745(10) 1 calc PR A 1 C24A C 0.4387(4) 0.9058(11) 0.4752(3) 0.071(3) Uani 0.745(10) 1 d PDU A 1 H24A H 0.4439 0.8028 0.4708 0.086 Uiso 0.745(10) 1 calc PR A 1 C25A C 0.4961(4) 0.9762(12) 0.4597(4) 0.083(3) Uani 0.745(10) 1 d PDU A 1 C26A C 0.5385(6) 1.1669(15) 0.4188(7) 0.116(6) Uani 0.745(10) 1 d PDU A 1 H26A H 0.5582 1.2102 0.4447 0.174 Uiso 0.745(10) 1 calc PR A 1 H26B H 0.5254 1.2398 0.3978 0.174 Uiso 0.745(10) 1 calc PR A 1 H26C H 0.5662 1.1044 0.4033 0.174 Uiso 0.745(10) 1 calc PR A 1 C27A C 0.4288(5) 0.9304(13) 0.5263(3) 0.091(3) Uani 0.745(10) 1 d PDU A 1 H27A H 0.4657 0.9078 0.5427 0.109 Uiso 0.745(10) 1 calc PR A 1 H27B H 0.4201 1.0306 0.5314 0.109 Uiso 0.745(10) 1 calc PR A 1 C28A C 0.3787(4) 0.8434(8) 0.5456(3) 0.077(3) Uiso 0.745(10) 1 d PGDU A 1 C29A C 0.3262(4) 0.9089(7) 0.5591(4) 0.118(4) Uiso 0.745(10) 1 d PGDU A 1 H29A H 0.3222 1.0071 0.5556 0.142 Uiso 0.745(10) 1 d PG A 1 C30A C 0.2795(4) 0.8323(11) 0.5776(5) 0.147(6) Uiso 0.745(10) 1 d PGU A 1 H30A H 0.2446 0.8794 0.5867 0.176 Uiso 0.745(10) 1 d PG A 1 C31A C 0.2835(4) 0.6866(11) 0.5830(4) 0.126(5) Uiso 0.745(10) 1 d PGU A 1 H31A H 0.2521 0.6349 0.5961 0.151 Uiso 0.745(10) 1 d PG A 1 C32A C 0.3348(5) 0.6204(7) 0.5686(4) 0.122(5) Uiso 0.745(10) 1 d PG A 1 H32A H 0.3380 0.5218 0.5712 0.146 Uiso 0.745(10) 1 d PG A 1 C33A C 0.3819(4) 0.6967(8) 0.5503(4) 0.100(4) Uiso 0.745(10) 1 d PGD A 1 H33A H 0.4165 0.6489 0.5409 0.121 Uiso 0.745(10) 1 d PG A 1 N1B N 0.3512(7) 0.435(2) 0.4295(7) 0.051(5) Uiso 0.451(11) 1 d PDU B 2 H1B H 0.3645 0.5204 0.4255 0.061 Uiso 0.451(11) 1 calc PR B 2 O1B O 0.6393(6) 0.6152(16) 0.5118(5) 0.097(5) Uiso 0.451(11) 1 d PDU B 2 O2B O 0.3595(8) 0.2380(18) 0.4734(7) 0.057(5) Uiso 0.451(11) 1 d PDU B 2 O3B O 0.1949(6) 0.3977(17) 0.4278(7) 0.105(6) Uiso 0.451(11) 1 d PDU B 2 O4B O 0.2496(7) 0.5894(15) 0.4367(7) 0.078(5) Uiso 0.451(11) 1 d PDU B 2 C1B C 0.6052(9) 0.5901(17) 0.6212(4) 0.092(8) Uiso 0.451(11) 1 d PD B 2 C2B C 0.6258(7) 0.5509(17) 0.6646(5) 0.096(7) Uiso 0.451(11) 1 d PD B 2 H2B H 0.6163 0.6076 0.6899 0.115 Uiso 0.451(11) 1 calc PR B 2 C3B C 0.6596(7) 0.4308(17) 0.6709(4) 0.079(5) Uiso 0.451(11) 1 d PD B 2 C4B C 0.6754(7) 0.3506(17) 0.6332(4) 0.072(5) Uiso 0.451(11) 1 d PD B 2 H4B H 0.7013 0.2736 0.6372 0.086 Uiso 0.451(11) 1 calc PR B 2 C5B C 0.6535(12) 0.381(2) 0.5886(5) 0.103(17) Uiso 0.451(11) 1 d PD B 2 C6B C 0.6196(8) 0.5037(17) 0.5837(4) 0.064(9) Uiso 0.451(11) 1 d PDU B 2 C7B C 0.6032(5) 0.5514(14) 0.5362(4) 0.063(4) Uiso 0.451(11) 1 d PDU B 2 C23B C 0.3806(10) 0.350(3) 0.4588(11) 0.062(6) Uiso 0.451(11) 1 d PDU B 2 C11B C 0.4379(5) 0.4087(16) 0.4775(4) 0.084(11) Uiso 0.451(11) 1 d PGDU B 2 C12B C 0.4558(5) 0.3640(13) 0.5211(4) 0.048(5) Uiso 0.451(11) 1 d PGDU B 2 H12B H 0.4310 0.3042 0.5383 0.058 Uiso 0.451(11) 1 d PG B 2 C13B C 0.5095(5) 0.4075(11) 0.5389(3) 0.061(4) Uiso 0.451(11) 1 d PGDU B 2 H13B H 0.5209 0.3764 0.5681 0.073 Uiso 0.451(11) 1 d PG B 2 C8B C 0.5476(4) 0.4968(12) 0.5146(4) 0.065(4) Uiso 0.451(11) 1 d PGDU B 2 C9B C 0.5300(4) 0.5421(12) 0.4711(4) 0.056(4) Uiso 0.451(11) 1 d PGDU B 2 H9B H 0.5549 0.6019 0.4540 0.067 Uiso 0.451(11) 1 d PG B 2 C10B C 0.4756(5) 0.4985(14) 0.4531(3) 0.058(5) Uiso 0.451(11) 1 d PGDU B 2 H10B H 0.4641 0.5300 0.4240 0.070 Uiso 0.451(11) 1 d PG B 2 C14B C 0.5675(10) 0.7216(19) 0.6169(8) 0.121(7) Uiso 0.451(11) 1 d PDU B 2 H14B H 0.5612 0.7432 0.5842 0.145 Uiso 0.451(11) 1 calc PR B 2 C15B C 0.6024(13) 0.842(2) 0.6392(12) 0.155(11) Uiso 0.451(11) 1 d PDU B 2 H15D H 0.5796 0.9290 0.6369 0.233 Uiso 0.451(11) 1 calc PR B 2 H15E H 0.6403 0.8538 0.6237 0.233 Uiso 0.451(11) 1 calc PR B 2 H15F H 0.6094 0.8205 0.6711 0.233 Uiso 0.451(11) 1 calc PR B 2 C16B C 0.5065(11) 0.702(4) 0.6403(16) 0.162(13) Uiso 0.451(11) 1 d PDU B 2 H16D H 0.4900 0.6107 0.6319 0.243 Uiso 0.451(11) 1 calc PR B 2 H16E H 0.4795 0.7760 0.6305 0.243 Uiso 0.451(11) 1 calc PR B 2 H16F H 0.5114 0.7064 0.6732 0.243 Uiso 0.451(11) 1 calc PR B 2 C17B C 0.6732(10) 0.383(2) 0.7190(6) 0.151(12) Uiso 0.451(11) 1 d PDU B 2 H17B H 0.6540 0.4584 0.7373 0.181 Uiso 0.451(11) 1 calc PR B 2 C18B C 0.6395(13) 0.254(3) 0.7340(10) 0.143(11) Uiso 0.451(11) 1 d PDU B 2 H18D H 0.5971 0.2693 0.7299 0.215 Uiso 0.451(11) 1 calc PR B 2 H18E H 0.6477 0.2359 0.7660 0.215 Uiso 0.451(11) 1 calc PR B 2 H18F H 0.6521 0.1736 0.7160 0.215 Uiso 0.451(11) 1 calc PR B 2 C19B C 0.7346(10) 0.393(3) 0.7338(10) 0.124(10) Uiso 0.451(11) 1 d PDU B 2 H19D H 0.7560 0.4586 0.7143 0.185 Uiso 0.451(11) 1 calc PR B 2 H19E H 0.7531 0.3006 0.7319 0.185 Uiso 0.451(11) 1 calc PR B 2 H19F H 0.7359 0.4261 0.7651 0.185 Uiso 0.451(11) 1 calc PR B 2 C20B C 0.6685(9) 0.288(2) 0.5471(7) 0.113(7) Uiso 0.451(11) 1 d PDU B 2 H20B H 0.6622 0.3469 0.5196 0.136 Uiso 0.451(11) 1 calc PR B 2 C21B C 0.7333(9) 0.243(3) 0.5467(10) 0.118(8) Uiso 0.451(11) 1 d PDU B 2 H21D H 0.7574 0.3149 0.5615 0.177 Uiso 0.451(11) 1 calc PR B 2 H21E H 0.7465 0.2315 0.5154 0.177 Uiso 0.451(11) 1 calc PR B 2 H21F H 0.7375 0.1544 0.5629 0.177 Uiso 0.451(11) 1 calc PR B 2 C22B C 0.6255(15) 0.163(4) 0.544(2) 0.207(17) Uiso 0.451(11) 1 d PDU B 2 H22D H 0.5851 0.1980 0.5396 0.310 Uiso 0.451(11) 1 calc PR B 2 H22E H 0.6277 0.1071 0.5712 0.310 Uiso 0.451(11) 1 calc PR B 2 H22F H 0.6363 0.1052 0.5175 0.310 Uiso 0.451(11) 1 calc PR B 2 C24B C 0.2983(6) 0.391(2) 0.4042(5) 0.068(6) Uiso 0.451(11) 1 d PDU B 2 H24B H 0.2948 0.2871 0.4066 0.081 Uiso 0.451(11) 1 calc PR B 2 C25B C 0.2420(6) 0.4568(18) 0.4248(7) 0.067(6) Uiso 0.451(11) 1 d PDU B 2 C26B C 0.1963(9) 0.669(2) 0.4492(9) 0.086(7) Uiso 0.451(11) 1 d PDU B 2 H26D H 0.1850 0.7303 0.4241 0.129 Uiso 0.451(11) 1 calc PR B 2 H26E H 0.2044 0.7254 0.4761 0.129 Uiso 0.451(11) 1 calc PR B 2 H26F H 0.1639 0.6039 0.4556 0.129 Uiso 0.451(11) 1 calc PR B 2 C27B C 0.3017(9) 0.430(3) 0.3534(6) 0.073(6) Uiso 0.451(11) 1 d PDU B 2 H27C H 0.2638 0.4044 0.3389 0.088 Uiso 0.451(11) 1 calc PR B 2 H27D H 0.3059 0.5330 0.3509 0.088 Uiso 0.451(11) 1 calc PR B 2 C28B C 0.3515(7) 0.3624(17) 0.3269(6) 0.081(6) Uiso 0.451(11) 1 d PGDU B 2 C29B C 0.4032(8) 0.4376(15) 0.3172(7) 0.108(7) Uiso 0.451(11) 1 d PGDU B 2 H29B H 0.4065 0.5318 0.3269 0.129 Uiso 0.451(11) 1 d PG B 2 C30B C 0.4498(7) 0.3764(19) 0.2934(7) 0.129(8) Uiso 0.451(11) 1 d PGU B 2 H30B H 0.4841 0.4300 0.2870 0.154 Uiso 0.451(11) 1 d PG B 2 C31B C 0.4467(7) 0.237(2) 0.2787(7) 0.138(9) Uiso 0.451(11) 1 d PG B 2 H31B H 0.4780 0.1958 0.2621 0.165 Uiso 0.451(11) 1 d PG B 2 C32B C 0.3964(8) 0.1605(15) 0.2893(7) 0.117(7) Uiso 0.451(11) 1 d PG B 2 H32B H 0.3938 0.0653 0.2804 0.140 Uiso 0.451(11) 1 d PG B 2 C33B C 0.3493(7) 0.2215(16) 0.3129(6) 0.108(7) Uiso 0.451(11) 1 d PGDU B 2 H33B H 0.3153 0.1671 0.3195 0.129 Uiso 0.451(11) 1 d PG B 2 N1C N 0.3726(11) 0.946(4) 0.4556(9) 0.056(8) Uiso 0.255(10) 1 d PDU A 3 H1C H 0.3506 1.0178 0.4631 0.067 Uiso 0.255(10) 1 calc PR A 3 O1C O 0.1128(11) 1.152(3) 0.3437(9) 0.097(12) Uiso 0.255(10) 1 d PDU A 3 O2C O 0.376(3) 0.744(6) 0.414(3) 0.069(13) Uiso 0.255(10) 1 d PDU A 3 O3C O 0.5254(12) 0.999(4) 0.4919(11) 0.149(13) Uiso 0.255(10) 1 d PDU A 3 O4C O 0.4755(16) 1.067(5) 0.4294(14) 0.102(9) Uiso 0.255(10) 1 d PDU A 3 C1C C 0.1326(12) 1.011(3) 0.2459(6) 0.070(11) Uiso 0.255(10) 1 d PD A 3 C2C C 0.1145(14) 0.949(3) 0.2053(6) 0.106(17) Uiso 0.255(10) 1 d PD A 3 H2C H 0.1258 0.9872 0.1769 0.127 Uiso 0.255(10) 1 calc PR A 3 C3C C 0.0786(14) 0.829(3) 0.2082(6) 0.078(10) Uiso 0.255(10) 1 d PDU A 3 C4C C 0.0622(12) 0.775(2) 0.2502(6) 0.064(9) Uiso 0.255(10) 1 d PD A 3 H4C H 0.0378 0.6949 0.2510 0.077 Uiso 0.255(10) 1 calc PR A 3 C5C C 0.0805(14) 0.836(3) 0.2921(6) 0.096(13) Uiso 0.255(10) 1 d PDU A 3 C6C C 0.1163(12) 0.956(2) 0.2872(6) 0.066(13) Uiso 0.255(10) 1 d PDU A 3 C7C C 0.1496(7) 1.0652(18) 0.3160(5) 0.079(8) Uiso 0.255(10) 1 d PDU A 3 C23C C 0.357(2) 0.866(5) 0.4189(15) 0.067(9) Uiso 0.255(10) 1 d PDU A 3 C11C C 0.3040(7) 0.921(2) 0.3929(6) 0.040(8) Uiso 0.255(10) 1 d PGDU A 3 C12C C 0.2926(7) 0.869(2) 0.3494(6) 0.052(8) Uiso 0.255(10) 1 d PGDU A 3 H12C H 0.3183 0.8017 0.3366 0.063 Uiso 0.255(10) 1 d PG A 3 C13C C 0.2442(8) 0.9153(19) 0.3248(5) 0.065(8) Uiso 0.255(10) 1 d PGD A 3 H13C H 0.2380 0.8797 0.2953 0.078 Uiso 0.255(10) 1 d PG A 3 C8C C 0.2041(6) 1.0137(17) 0.3426(6) 0.048(5) Uiso 0.255(10) 1 d PGDU A 3 C9C C 0.2176(6) 1.0713(16) 0.3844(6) 0.049(5) Uiso 0.255(10) 1 d PGDU A 3 H9C H 0.1931 1.1428 0.3964 0.059 Uiso 0.255(10) 1 d PG A 3 C10C C 0.2669(7) 1.0256(19) 0.4094(5) 0.059(7) Uiso 0.255(10) 1 d PGDU A 3 H10C H 0.2750 1.0667 0.4379 0.071 Uiso 0.255(10) 1 d PG A 3 C14C C 0.1642(10) 1.142(2) 0.2657(7) 0.117(10) Uiso 0.255(10) 1 d PDU A 3 C15C C 0.129(2) 1.280(3) 0.2606(15) 0.20(2) Uiso 0.255(10) 1 d PDU A 3 H15G H 0.0883 1.2658 0.2711 0.295 Uiso 0.255(10) 1 calc PR A 3 H15H H 0.1285 1.3082 0.2287 0.295 Uiso 0.255(10) 1 calc PR A 3 H15I H 0.1477 1.3533 0.2787 0.295 Uiso 0.255(10) 1 calc PR A 3 C16C C 0.2285(11) 1.162(4) 0.2518(11) 0.095(11) Uiso 0.255(10) 1 d PDU A 3 H16G H 0.2501 1.0741 0.2557 0.143 Uiso 0.255(10) 1 calc PR A 3 H16H H 0.2464 1.2346 0.2707 0.143 Uiso 0.255(10) 1 calc PR A 3 H16I H 0.2302 1.1906 0.2200 0.143 Uiso 0.255(10) 1 calc PR A 3 C17C C 0.0574(15) 0.753(3) 0.1640(8) 0.125(11) Uiso 0.255(10) 1 d PDU A 3 H17C H 0.0642 0.8197 0.1384 0.150 Uiso 0.255(10) 1 calc PR A 3 C18C C 0.095(2) 0.626(5) 0.1549(19) 0.160(17) Uiso 0.255(10) 1 d PDU A 3 H18G H 0.1364 0.6515 0.1555 0.240 Uiso 0.255(10) 1 calc PR A 3 H18H H 0.0845 0.5877 0.1251 0.240 Uiso 0.255(10) 1 calc PR A 3 H18I H 0.0868 0.5551 0.1781 0.240 Uiso 0.255(10) 1 calc PR A 3 C19C C -0.0070(15) 0.721(7) 0.165(2) 0.131(15) Uiso 0.255(10) 1 d PDU A 3 H19G H -0.0291 0.8057 0.1731 0.196 Uiso 0.255(10) 1 calc PR A 3 H19H H -0.0148 0.6475 0.1869 0.196 Uiso 0.255(10) 1 calc PR A 3 H19I H -0.0195 0.6901 0.1347 0.196 Uiso 0.255(10) 1 calc PR A 3 C20C C 0.0550(14) 0.786(3) 0.3378(7) 0.087(8) Uiso 0.255(10) 1 d PDU A 3 H20C H 0.0484 0.8690 0.3576 0.104 Uiso 0.255(10) 1 calc PR A 3 C21C C -0.0045(16) 0.710(6) 0.3314(16) 0.137(17) Uiso 0.255(10) 1 d PDU A 3 H21G H -0.0369 0.7772 0.3349 0.205 Uiso 0.255(10) 1 calc PR A 3 H21H H -0.0084 0.6361 0.3541 0.205 Uiso 0.255(10) 1 calc PR A 3 H21I H -0.0060 0.6690 0.3010 0.205 Uiso 0.255(10) 1 calc PR A 3 C22C C 0.098(2) 0.686(6) 0.3619(17) 0.179(18) Uiso 0.255(10) 1 d PDU A 3 H22G H 0.0830 0.6622 0.3918 0.269 Uiso 0.255(10) 1 calc PR A 3 H22H H 0.1369 0.7322 0.3651 0.269 Uiso 0.255(10) 1 calc PR A 3 H22I H 0.1031 0.6008 0.3439 0.269 Uiso 0.255(10) 1 calc PR A 3 C24C C 0.4252(9) 0.914(4) 0.4824(7) 0.081(9) Uiso 0.255(10) 1 d PDU A 3 H24C H 0.4337 0.8128 0.4774 0.098 Uiso 0.255(10) 1 calc PR A 3 C25C C 0.4805(11) 0.992(5) 0.4677(9) 0.084(9) Uiso 0.255(10) 1 d PDU A 3 C26C C 0.529(2) 1.135(8) 0.413(2) 0.142(18) Uiso 0.255(10) 1 d PDU A 3 C27C C 0.4131(13) 0.931(4) 0.5337(7) 0.090(9) Uiso 0.255(10) 1 d PDU A 3 H27E H 0.4498 0.9092 0.5505 0.108 Uiso 0.255(10) 1 calc PR A 3 H27F H 0.4029 1.0298 0.5399 0.108 Uiso 0.255(10) 1 calc PR A 3 C28C C 0.3640(9) 0.839(2) 0.5512(8) 0.073(8) Uiso 0.255(10) 1 d PGDU A 3 C29C C 0.3225(9) 0.8886(19) 0.5822(9) 0.092(8) Uiso 0.255(10) 1 d PGDU A 3 H29C H 0.3239 0.9835 0.5916 0.110 Uiso 0.255(10) 1 d PG A 3 C30C C 0.2788(9) 0.800(3) 0.5997(9) 0.092(9) Uiso 0.255(10) 1 d PGU A 3 H30C H 0.2519 0.8345 0.6215 0.110 Uiso 0.255(10) 1 d PG A 3 C31C C 0.2742(11) 0.661(2) 0.5855(10) 0.165(16) Uiso 0.255(10) 1 d PGU A 3 H31C H 0.2441 0.6013 0.5970 0.198 Uiso 0.255(10) 1 d PG A 3 C32C C 0.3152(13) 0.6113(19) 0.5541(10) 0.103(11) Uiso 0.255(10) 1 d PG A 3 H32C H 0.3128 0.5174 0.5439 0.124 Uiso 0.255(10) 1 d PG A 3 C33C C 0.3598(12) 0.699(2) 0.5374(8) 0.091(9) Uiso 0.255(10) 1 d PGD A 3 H33C H 0.3876 0.6627 0.5165 0.109 Uiso 0.255(10) 1 d PG A 3 N1D N 0.3576(7) 0.4463(17) 0.4220(6) 0.071(5) Uani 0.549(11) 1 d PDU B 4 H1D H 0.3752 0.5247 0.4145 0.085 Uiso 0.549(11) 1 calc PR B 4 O1D O 0.6220(4) 0.6802(11) 0.5272(3) 0.076(3) Uani 0.549(11) 1 d PDU B 4 O2D O 0.3610(8) 0.2453(14) 0.4627(7) 0.082(5) Uani 0.549(11) 1 d PDU B 4 O3D O 0.1974(5) 0.4277(14) 0.4029(7) 0.112(4) Uani 0.549(11) 1 d PDU B 4 O4D O 0.2567(6) 0.5662(14) 0.4489(5) 0.093(4) Uani 0.549(11) 1 d PDU B 4 C1D C 0.6068(6) 0.5620(13) 0.6265(4) 0.073(5) Uiso 0.549(11) 1 d PD B 4 C2D C 0.6251(6) 0.5092(15) 0.6682(4) 0.092(5) Uiso 0.549(11) 1 d PD B 4 H2D H 0.6163 0.5564 0.6956 0.111 Uiso 0.549(11) 1 calc PR B 4 C3D C 0.6573(6) 0.3833(15) 0.6680(4) 0.094(5) Uiso 0.549(11) 1 d PD B 4 C4D C 0.6680(7) 0.3130(16) 0.6278(4) 0.091(6) Uiso 0.549(11) 1 d PD B 4 H4D H 0.6864 0.2240 0.6289 0.109 Uiso 0.549(11) 1 calc PR B 4 C5D C 0.6520(9) 0.3701(16) 0.5849(4) 0.076(10) Uiso 0.549(11) 1 d PD B 4 C6D C 0.6197(8) 0.4950(14) 0.5862(4) 0.079(9) Uiso 0.549(11) 1 d PDU B 4 C7D C 0.5844(4) 0.5965(10) 0.5559(3) 0.090(4) Uani 0.549(11) 1 d PDU B 4 C23D C 0.3810(7) 0.3663(17) 0.4560(7) 0.056(5) Uani 0.549(11) 1 d PDU B 4 C11D C 0.4373(4) 0.4164(11) 0.4784(3) 0.040(5) Uiso 0.549(11) 1 d PGDU B 4 C12D C 0.4492(4) 0.3723(11) 0.5227(3) 0.091(8) Uiso 0.549(11) 1 d PGDU B 4 H12D H 0.4246 0.3042 0.5364 0.109 Uiso 0.549(11) 1 d PG B 4 C13D C 0.4965(4) 0.4267(10) 0.5466(3) 0.068(4) Uiso 0.549(11) 1 d PGDU B 4 H13D H 0.5032 0.3963 0.5767 0.082 Uiso 0.549(11) 1 d PG B 4 C8D C 0.5350(4) 0.5263(9) 0.5275(3) 0.056(3) Uiso 0.549(11) 1 d PGDU B 4 C9D C 0.5209(4) 0.5762(9) 0.4848(3) 0.066(3) Uiso 0.549(11) 1 d PGDU B 4 H9D H 0.5441 0.6482 0.4717 0.079 Uiso 0.549(11) 1 d PG B 4 C10D C 0.4726(4) 0.5220(11) 0.4604(3) 0.068(5) Uiso 0.549(11) 1 d PGDU B 4 H10D H 0.4640 0.5579 0.4312 0.082 Uiso 0.549(11) 1 d PG B 4 C14D C 0.5690(6) 0.6801(13) 0.6050(4) 0.125(6) Uani 0.549(11) 1 d PDU B 4 C15D C 0.5989(10) 0.8265(14) 0.6062(8) 0.135(7) Uani 0.549(11) 1 d PDU B 4 H15J H 0.6389 0.8196 0.5939 0.202 Uiso 0.549(11) 1 calc PR B 4 H15K H 0.6007 0.8597 0.6375 0.202 Uiso 0.549(11) 1 calc PR B 4 H15L H 0.5757 0.8923 0.5880 0.202 Uiso 0.549(11) 1 calc PR B 4 C16D C 0.5057(7) 0.689(3) 0.6226(10) 0.168(12) Uani 0.549(11) 1 d PDU B 4 H16J H 0.4879 0.5957 0.6225 0.253 Uiso 0.549(11) 1 calc PR B 4 H16K H 0.4827 0.7513 0.6031 0.253 Uiso 0.549(11) 1 calc PR B 4 H16L H 0.5059 0.7259 0.6535 0.253 Uiso 0.549(11) 1 calc PR B 4 C17D C 0.6815(8) 0.330(2) 0.7146(5) 0.138(8) Uani 0.549(11) 1 d PDU B 4 H17D H 0.6629 0.3910 0.7380 0.166 Uiso 0.549(11) 1 calc PR B 4 C18D C 0.6588(12) 0.186(3) 0.7237(9) 0.191(12) Uani 0.549(11) 1 d PDU B 4 H18J H 0.6168 0.1812 0.7158 0.286 Uiso 0.549(11) 1 calc PR B 4 H18K H 0.6639 0.1637 0.7558 0.286 Uiso 0.549(11) 1 calc PR B 4 H18L H 0.6808 0.1183 0.7053 0.286 Uiso 0.549(11) 1 calc PR B 4 C19D C 0.7457(9) 0.350(3) 0.7194(9) 0.164(11) Uani 0.549(11) 1 d PDU B 4 H19J H 0.7549 0.4497 0.7182 0.247 Uiso 0.549(11) 1 calc PR B 4 H19K H 0.7662 0.3014 0.6947 0.247 Uiso 0.549(11) 1 calc PR B 4 H19L H 0.7588 0.3113 0.7484 0.247 Uiso 0.549(11) 1 calc PR B 4 C20D C 0.6616(9) 0.284(2) 0.5411(5) 0.142(7) Uani 0.549(11) 1 d PDU B 4 H20D H 0.6375 0.3264 0.5163 0.170 Uiso 0.549(11) 1 calc PR B 4 C21D C 0.7267(10) 0.286(3) 0.5270(9) 0.158(10) Uani 0.549(11) 1 d PDU B 4 H21J H 0.7411 0.3822 0.5267 0.237 Uiso 0.549(11) 1 calc PR B 4 H21K H 0.7307 0.2451 0.4968 0.237 Uiso 0.549(11) 1 calc PR B 4 H21L H 0.7499 0.2307 0.5486 0.237 Uiso 0.549(11) 1 calc PR B 4 C22D C 0.6398(15) 0.133(2) 0.5495(15) 0.208(14) Uani 0.549(11) 1 d PDU B 4 H22J H 0.5980 0.1350 0.5579 0.312 Uiso 0.549(11) 1 calc PR B 4 H22K H 0.6628 0.0910 0.5740 0.312 Uiso 0.549(11) 1 calc PR B 4 H22L H 0.6449 0.0779 0.5219 0.312 Uiso 0.549(11) 1 calc PR B 4 C24D C 0.3037(5) 0.4044(18) 0.3979(4) 0.068(5) Uani 0.549(11) 1 d PDU B 4 H24D H 0.2992 0.3012 0.4021 0.081 Uiso 0.549(11) 1 calc PR B 4 C25D C 0.2471(5) 0.4730(19) 0.4150(6) 0.089(5) Uani 0.549(11) 1 d PDU B 4 C26D C 0.2059(8) 0.6452(18) 0.4664(7) 0.104(6) Uani 0.549(11) 1 d PDU B 4 H26J H 0.2080 0.7420 0.4557 0.155 Uiso 0.549(11) 1 calc PR B 4 H26K H 0.2066 0.6440 0.4995 0.155 Uiso 0.549(11) 1 calc PR B 4 H26L H 0.1692 0.6023 0.4556 0.155 Uiso 0.549(11) 1 calc PR B 4 C27D C 0.3113(7) 0.431(2) 0.3462(5) 0.076(4) Uani 0.549(11) 1 d PDU B 4 H27G H 0.2746 0.4044 0.3302 0.091 Uiso 0.549(11) 1 calc PR B 4 H27H H 0.3184 0.5319 0.3409 0.091 Uiso 0.549(11) 1 calc PR B 4 C28D C 0.3625(6) 0.3473(13) 0.3280(5) 0.076(5) Uiso 0.549(11) 1 d PGDU B 4 C29D C 0.4143(6) 0.4118(11) 0.3130(6) 0.108(6) Uiso 0.549(11) 1 d PGDU B 4 H29D H 0.4180 0.5105 0.3149 0.129 Uiso 0.549(11) 1 d PG B 4 C30D C 0.4609(5) 0.3321(15) 0.2953(6) 0.128(7) Uiso 0.549(11) 1 d PGU B 4 H30D H 0.4951 0.3782 0.2843 0.154 Uiso 0.549(11) 1 d PG B 4 C31D C 0.4578(6) 0.1863(15) 0.2934(6) 0.132(7) Uiso 0.549(11) 1 d PG B 4 H31D H 0.4897 0.1327 0.2819 0.158 Uiso 0.549(11) 1 d PG B 4 C32D C 0.4064(7) 0.1216(11) 0.3089(6) 0.126(6) Uiso 0.549(11) 1 d PG B 4 H32D H 0.4034 0.0226 0.3081 0.152 Uiso 0.549(11) 1 d PG B 4 C33D C 0.3591(6) 0.2009(13) 0.3256(5) 0.106(6) Uiso 0.549(11) 1 d PGDU B 4 H33D H 0.3243 0.1548 0.3355 0.128 Uiso 0.549(11) 1 d PG B 4 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 N1A 0.071(5) 0.043(4) 0.079(6) 0.006(4) -0.009(5) -0.005(4) O1A 0.090(6) 0.134(9) 0.140(8) -0.066(8) -0.038(6) 0.053(7) O2A 0.077(8) 0.054(5) 0.096(11) -0.007(5) -0.002(9) 0.005(4) O3A 0.072(5) 0.114(7) 0.244(13) 0.033(8) -0.023(7) 0.001(5) O4A 0.088(6) 0.079(6) 0.119(7) -0.002(5) 0.025(5) -0.008(5) C7A 0.075(6) 0.071(5) 0.076(7) -0.004(5) -0.007(5) 0.013(5) C23A 0.069(6) 0.041(5) 0.069(6) 0.012(4) -0.001(4) -0.008(4) C14A 0.127(10) 0.085(7) 0.136(11) 0.005(7) 0.004(8) -0.031(7) C15A 0.158(15) 0.090(9) 0.34(3) 0.023(14) 0.030(18) -0.014(10) C16A 0.124(12) 0.162(14) 0.183(18) 0.018(14) -0.005(12) -0.041(10) C17A 0.124(10) 0.138(10) 0.080(8) -0.011(8) -0.052(7) 0.000(8) C18A 0.21(2) 0.26(2) 0.098(11) -0.057(14) -0.030(12) 0.050(18) C19A 0.21(2) 0.187(17) 0.117(14) 0.023(12) -0.026(15) -0.064(18) C20A 0.080(7) 0.107(7) 0.059(6) 0.008(5) 0.004(5) 0.019(6) C21A 0.108(11) 0.169(14) 0.129(13) 0.038(11) 0.013(10) -0.013(11) C22A 0.153(12) 0.159(13) 0.130(12) 0.074(11) 0.010(10) 0.021(10) C24A 0.078(6) 0.053(5) 0.082(6) -0.001(5) -0.023(6) 0.004(5) C25A 0.062(6) 0.069(7) 0.117(9) -0.024(6) -0.001(6) -0.011(6) C26A 0.094(8) 0.081(8) 0.171(14) -0.031(8) 0.064(9) -0.031(6) C27A 0.105(8) 0.075(6) 0.092(8) -0.018(6) -0.022(7) 0.013(6) N1D 0.084(8) 0.051(6) 0.077(10) 0.013(6) 0.004(7) -0.007(5) O1D 0.061(5) 0.079(6) 0.087(6) 0.020(5) -0.006(5) -0.021(5) O2D 0.105(8) 0.054(6) 0.085(11) 0.034(6) -0.016(7) -0.012(4) O3D 0.066(6) 0.118(9) 0.152(13) 0.000(9) -0.023(7) 0.004(6) O4D 0.097(8) 0.093(7) 0.089(9) 0.002(7) 0.024(7) 0.032(6) C7D 0.098(9) 0.078(8) 0.093(9) 0.042(7) 0.017(8) 0.017(7) C23D 0.072(8) 0.043(7) 0.054(8) 0.012(5) 0.017(6) 0.024(5) C14D 0.121(11) 0.118(12) 0.138(14) 0.055(11) 0.046(10) 0.048(10) C15D 0.160(17) 0.110(13) 0.134(17) 0.016(12) -0.004(14) -0.001(12) C16D 0.120(15) 0.155(17) 0.23(3) 0.084(18) 0.059(16) 0.078(13) C17D 0.116(15) 0.23(2) 0.072(11) 0.052(13) -0.032(10) 0.051(15) C18D 0.21(2) 0.24(3) 0.117(17) 0.104(19) 0.014(17) 0.04(2) C19D 0.18(2) 0.21(2) 0.108(17) 0.045(19) -0.080(17) 0.026(19) C20D 0.171(15) 0.134(13) 0.120(13) 0.040(11) 0.066(12) 0.067(12) C21D 0.17(2) 0.17(2) 0.131(17) 0.073(16) 0.046(15) 0.021(15) C22D 0.24(3) 0.121(16) 0.27(3) -0.02(2) 0.12(2) 0.021(18) C24D 0.057(7) 0.052(7) 0.094(10) 0.010(7) -0.012(6) 0.000(5) C25D 0.102(11) 0.069(9) 0.096(12) 0.006(9) 0.015(9) 0.009(8) C26D 0.116(13) 0.093(10) 0.101(14) 0.024(11) 0.043(11) 0.045(9) C27D 0.081(9) 0.072(8) 0.076(9) 0.016(7) -0.006(7) 0.001(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1A C23A 1.331(7) . ? N1A C24A 1.450(8) . ? N1A H1A 0.8600 . ? O1A C7A 1.216(8) . ? O2A C23A 1.226(8) . ? O3A C25A 1.185(8) . ? O4A C25A 1.286(8) . ? O4A C26A 1.430(8) . ? C1A C2A 1.381(8) . ? C1A C6A 1.384(8) . ? C1A C14A 1.492(8) . ? C2A C3A 1.366(9) . ? C2A H2A 0.9300 . ? C3A C4A 1.381(8) . ? C3A C17A 1.499(8) . ? C4A C5A 1.408(8) . ? C4A H4A 0.9300 . ? C5A C6A 1.376(8) . ? C5A C20A 1.514(8) . ? C6A C7A 1.506(8) . ? C7A C8A 1.471(6) . ? C23A C11A 1.484(7) . ? C11A C10A 1.3814 . ? C11A C12A 1.3903 . ? C12A C13A 1.3605 . ? C12A H12A 0.9296 . ? C13A C8A 1.3829 . ? C13A H13A 0.9293 . ? C8A C9A 1.3868 . ? C9A C10A 1.3747 . ? C9A H9A 0.9297 . ? C10A H10A 0.9293 . ? C14A C15A 1.511(10) . ? C14A C16A 1.515(10) . ? C14A H14A 0.9800 . ? C15A H15A 0.9600 . ? C15A H15B 0.9600 . ? C15A H15C 0.9600 . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C17A C19A 1.454(10) . ? C17A C18A 1.495(9) . ? C17A H17A 0.9800 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C19A H19A 0.9600 . ? C19A H19B 0.9600 . ? C19A H19C 0.9600 . ? C20A C21A 1.498(9) . ? C20A C22A 1.505(9) . ? C20A H20A 0.9800 . ? C21A H21A 0.9600 . ? C21A H21B 0.9600 . ? C21A H21C 0.9600 . ? C22A H22A 0.9600 . ? C22A H22B 0.9600 . ? C22A H22C 0.9600 . ? C24A C25A 1.502(8) . ? C24A C27A 1.515(8) . ? C24A H24A 0.9800 . ? C26A H26A 0.9600 . ? C26A H26B 0.9600 . ? C26A H26C 0.9600 . ? C27A C28A 1.488(8) . ? C27A H27A 0.9700 . ? C27A H27B 0.9700 . ? C28A C29A 1.3745 . ? C28A C33A 1.3837 . ? C29A C30A 1.3695 . ? C29A H29A 0.9303 . ? C30A C31A 1.3776 . ? C30A H30A 0.9295 . ? C31A C32A 1.3609 . ? C31A H31A 0.9295 . ? C32A C33A 1.3719 . ? C32A H32A 0.9304 . ? C33A H33A 0.9294 . ? N1B C23B 1.334(9) . ? N1B C24B 1.445(10) . ? N1B H1B 0.8600 . ? O1B C7B 1.225(9) . ? O2B C23B 1.223(9) . ? O3B C25B 1.185(9) . ? O4B C25B 1.302(9) . ? O4B C26B 1.443(10) . ? C1B C2B 1.385(9) . ? C1B C6B 1.394(9) . ? C1B C14B 1.495(9) . ? C2B C3B 1.366(9) . ? C2B H2B 0.9300 . ? C3B C4B 1.372(9) . ? C3B C17B 1.493(9) . ? C4B C5B 1.411(9) . ? C4B H4B 0.9300 . ? C5B C6B 1.380(9) . ? C5B C20B 1.521(9) . ? C6B C7B 1.491(9) . ? C7B C8B 1.476(8) . ? C23B C11B 1.488(8) . ? C11B C10B 1.3814 . ? C11B C12B 1.3901 . ? C12B C13B 1.3605 . ? C12B H12B 0.9297 . ? C12B H12D 0.9949 . ? C13B C8B 1.3828 . ? C13B H13B 0.9295 . ? C13B H13D 1.1098 . ? C8B C9B 1.3868 . ? C9B C10B 1.3748 . ? C9B H9B 0.9297 . ? C9B H9D 1.0436 . ? C10B H10B 0.9292 . ? C10B H10D 0.8826 . ? C14B C15B 1.515(10) . ? C14B C16B 1.524(10) . ? C14B H14B 0.9800 . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? C17B C19B 1.430(10) . ? C17B C18B 1.490(10) . ? C17B H17B 0.9800 . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? C19B H19D 0.9600 . ? C19B H19E 0.9600 . ? C19B H19F 0.9600 . ? C20B C21B 1.496(10) . ? C20B C22B 1.515(10) . ? C20B H20B 0.9800 . ? C21B H21D 0.9600 . ? C21B H21E 0.9600 . ? C21B H21F 0.9600 . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? C24B C25B 1.515(9) . ? C24B C27B 1.521(10) . ? C24B H24B 0.9800 . ? C26B H26D 0.9600 . ? C26B H26E 0.9600 . ? C26B H26F 0.9600 . ? C27B C28B 1.488(9) . ? C27B H27C 0.9700 . ? C27B H27D 0.9700 . ? C28B C29B 1.3746 . ? C28B C33B 1.3835 . ? C29B C30B 1.3692 . ? C29B H29B 0.9302 . ? C30B C31B 1.3774 . ? C30B H30B 0.9296 . ? C31B C32B 1.3609 . ? C31B H31B 0.9295 . ? C32B C33B 1.3716 . ? C32B H32B 0.9303 . ? C33B H33B 0.9296 . ? N1C C23C 1.347(10) . ? N1C C24C 1.433(11) . ? N1C H1C 0.8600 . ? O1C C7C 1.405(10) . ? O2C C23C 1.233(10) . ? O3C C25C 1.218(10) . ? O4C C25C 1.315(10) . ? O4C C26C 1.434(11) . ? C1C C6C 1.354(9) . ? C1C C2C 1.372(9) . ? C1C C14C 1.523(9) . ? C2C C3C 1.384(10) . ? C2C H2C 0.9300 . ? C3C C4C 1.366(10) . ? C3C C17C 1.536(10) . ? C4C C5C 1.402(10) . ? C4C H4C 0.9300 . ? C5C C6C 1.380(9) . ? C5C C20C 1.516(10) . ? C6C C7C 1.514(9) . ? C7C C8C 1.514(9) . ? C7C C14C 1.656(10) . ? C23C C11C 1.483(9) . ? C11C C10C 1.3669 . ? C11C C12C 1.3740 . ? C12C C13C 1.3572 . ? C12C H12C 0.9299 . ? C13C C8C 1.3813 . ? C13C H13C 0.9294 . ? C8C C9C 1.3600 . ? C9C C10C 1.3784 . ? C9C H9C 0.9298 . ? C10C H10C 0.9294 . ? C14C C16C 1.493(10) . ? C14C C15C 1.523(10) . ? C15C H15G 0.9600 . ? C15C H15H 0.9600 . ? C15C H15I 0.9600 . ? C16C H16G 0.9600 . ? C16C H16H 0.9600 . ? C16C H16I 0.9600 . ? C17C C19C 1.459(11) . ? C17C C18C 1.477(11) . ? C17C H17C 0.9800 . ? C18C H18G 0.9600 . ? C18C H18H 0.9600 . ? C18C H18I 0.9600 . ? C19C H19G 0.9600 . ? C19C H19H 0.9600 . ? C19C H19I 0.9600 . ? C20C C21C 1.510(11) . ? C20C C22C 1.511(11) . ? C20C H20C 0.9800 . ? C21C H21G 0.9600 . ? C21C H21H 0.9600 . ? C21C H21I 0.9600 . ? C22C H22G 0.9600 . ? C22C H22H 0.9600 . ? C22C H22I 0.9600 . ? C24C C25C 1.490(10) . ? C24C C27C 1.519(10) . ? C24C H24C 0.9800 . ? C27C C28C 1.480(9) . ? C27C H27E 0.9700 . ? C27C H27F 0.9700 . ? C28C C29C 1.3679 . ? C28C C33C 1.3764 . ? C29C C30C 1.3757 . ? C29C H29C 0.9303 . ? C30C C31C 1.3699 . ? C30C H30C 0.9293 . ? C31C C32C 1.3663 . ? C31C H31C 0.9296 . ? C32C C33C 1.3738 . ? C32C H32C 0.9303 . ? C33C H33C 0.9293 . ? N1D C23D 1.342(9) . ? N1D C24D 1.437(9) . ? N1D H1D 0.8600 . ? O1D C7D 1.414(8) . ? O2D C23D 1.234(9) . ? O3D C25D 1.231(9) . ? O4D C25D 1.331(9) . ? O4D C26D 1.441(9) . ? C1D C6D 1.357(9) . ? C1D C2D 1.368(9) . ? C1D C14D 1.521(9) . ? C2D C3D 1.379(9) . ? C2D H2D 0.9300 . ? C3D C4D 1.359(9) . ? C3D C17D 1.536(9) . ? C4D C5D 1.398(9) . ? C4D H4D 0.9300 . ? C5D C6D 1.374(8) . ? C5D C20D 1.518(9) . ? C6D C7D 1.513(8) . ? C7D C8D 1.520(8) . ? C7D C14D 1.660(9) . ? C23D C11D 1.484(7) . ? C11D C10D 1.3669 . ? C11D C12D 1.3740 . ? C12D C13D 1.3574 . ? C12D H12D 0.9297 . ? C13D C8D 1.3814 . ? C13D H13D 0.9293 . ? C8D C9D 1.3598 . ? C9D C10D 1.3785 . ? C9D H9D 0.9299 . ? C10D H10D 0.9294 . ? C14D C16D 1.496(9) . ? C14D C15D 1.524(10) . ? C15D H15J 0.9600 . ? C15D H15K 0.9600 . ? C15D H15L 0.9600 . ? C16D H16J 0.9600 . ? C16D H16K 0.9600 . ? C16D H16L 0.9600 . ? C17D C19D 1.444(10) . ? C17D C18D 1.463(10) . ? C17D H17D 0.9800 . ? C18D H18J 0.9600 . ? C18D H18K 0.9600 . ? C18D H18L 0.9600 . ? C19D H19J 0.9600 . ? C19D H19K 0.9600 . ? C19D H19L 0.9600 . ? C20D C21D 1.500(10) . ? C20D C22D 1.514(10) . ? C20D H20D 0.9800 . ? C21D H21J 0.9600 . ? C21D H21K 0.9600 . ? C21D H21L 0.9600 . ? C22D H22J 0.9600 . ? C22D H22K 0.9600 . ? C22D H22L 0.9600 . ? C24D C25D 1.496(9) . ? C24D C27D 1.528(9) . ? C24D H24D 0.9800 . ? C26D H26J 0.9600 . ? C26D H26K 0.9600 . ? C26D H26L 0.9600 . ? C27D C28D 1.480(8) . ? C27D H27G 0.9700 . ? C27D H27H 0.9700 . ? C28D C29D 1.3680 . ? C28D C33D 1.3765 . ? C29D C30D 1.3755 . ? C29D H29D 0.9304 . ? C30D C31D 1.3699 . ? C30D H30D 0.9294 . ? C31D C32D 1.3665 . ? C31D H31D 0.9296 . ? C32D C33D 1.3736 . ? C32D H32D 0.9304 . ? C33D H33D 0.9295 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23A N1A C24A 121.5(7) . . ? C23A N1A H1A 119.3 . . ? C24A N1A H1A 119.3 . . ? C25A O4A C26A 119.1(10) . . ? C2A C1A C6A 117.8(8) . . ? C2A C1A C14A 120.3(8) . . ? C6A C1A C14A 121.7(9) . . ? C3A C2A C1A 123.3(8) . . ? C3A C2A H2A 118.3 . . ? C1A C2A H2A 118.3 . . ? C2A C3A C4A 117.8(7) . . ? C2A C3A C17A 120.6(9) . . ? C4A C3A C17A 121.5(8) . . ? C3A C4A C5A 121.1(7) . . ? C3A C4A H4A 119.5 . . ? C5A C4A H4A 119.5 . . ? C6A C5A C4A 118.5(7) . . ? C6A C5A C20A 121.4(7) . . ? C4A C5A C20A 120.1(7) . . ? C5A C6A C1A 121.4(7) . . ? C5A C6A C7A 118.9(7) . . ? C1A C6A C7A 119.7(8) . . ? O1A C7A C8A 120.3(7) . . ? O1A C7A C6A 120.2(7) . . ? C8A C7A C6A 119.3(7) . . ? O2A C23A N1A 122.3(8) . . ? O2A C23A C11A 121.1(8) . . ? N1A C23A C11A 116.4(6) . . ? C10A C11A C12A 118.4 . . ? C10A C11A C23A 124.3(5) . . ? C12A C11A C23A 117.3(5) . . ? C13A C12A C11A 120.3 . . ? C12A C13A C8A 121.5 . . ? C13A C8A C9A 118.5 . . ? C13A C8A C7A 121.0(4) . . ? C9A C8A C7A 120.5(4) . . ? C10A C9A C8A 120.0 . . ? C9A C10A C11A 121.3 . . ? C1A C14A C15A 109.6(9) . . ? C1A C14A C16A 114.2(9) . . ? C15A C14A C16A 111.0(11) . . ? C1A C14A H14A 107.2 . . ? C15A C14A H14A 107.2 . . ? C16A C14A H14A 107.2 . . ? C14A C15A H15A 109.5 . . ? C14A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C14A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C14A C16A H16A 109.5 . . ? C14A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C14A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C19A C17A C18A 115.1(13) . . ? C19A C17A C3A 116.0(11) . . ? C18A C17A C3A 110.6(9) . . ? C19A C17A H17A 104.6 . . ? C18A C17A H17A 104.6 . . ? C3A C17A H17A 104.6 . . ? C17A C18A H18A 109.5 . . ? C17A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C17A C19A H19A 109.5 . . ? C17A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C17A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C21A C20A C22A 113.1(10) . . ? C21A C20A C5A 113.1(9) . . ? C22A C20A C5A 110.9(8) . . ? C21A C20A H20A 106.4 . . ? C22A C20A H20A 106.4 . . ? C5A C20A H20A 106.4 . . ? C20A C21A H21A 109.5 . . ? C20A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C20A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C20A C22A H22A 109.5 . . ? C20A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C20A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? N1A C24A C25A 113.1(7) . . ? N1A C24A C27A 111.7(8) . . ? C25A C24A C27A 110.3(7) . . ? N1A C24A H24A 107.1 . . ? C25A C24A H24A 107.1 . . ? C27A C24A H24A 107.1 . . ? O3A C25A O4A 125.7(9) . . ? O3A C25A C24A 120.5(8) . . ? O4A C25A C24A 113.5(7) . . ? C28A C27A C24A 113.1(7) . . ? C28A C27A H27A 109.0 . . ? C24A C27A H27A 109.0 . . ? C28A C27A H27B 109.0 . . ? C24A C27A H27B 109.0 . . ? H27A C27A H27B 107.8 . . ? C29A C28A C33A 117.3 . . ? C29A C28A C27A 119.7(6) . . ? C33A C28A C27A 123.0(6) . . ? C30A C29A C28A 121.3 . . ? C29A C30A C31A 121.0 . . ? C32A C31A C30A 118.1 . . ? C31A C32A C33A 121.1 . . ? C32A C33A C28A 121.2 . . ? C23B N1B C24B 123.2(13) . . ? C23B N1B H1B 118.4 . . ? C24B N1B H1B 118.4 . . ? C25B O4B C26B 116.9(13) . . ? C2B C1B C6B 118.6(10) . . ? C2B C1B C14B 118.6(11) . . ? C6B C1B C14B 122.8(11) . . ? C3B C2B C1B 121.4(11) . . ? C3B C2B H2B 119.3 . . ? C1B C2B H2B 119.3 . . ? C2B C3B C4B 119.1(9) . . ? C2B C3B C17B 118.8(12) . . ? C4B C3B C17B 121.9(12) . . ? C3B C4B C5B 122.0(10) . . ? C3B C4B H4B 119.0 . . ? C5B C4B H4B 119.0 . . ? C6B C5B C4B 116.8(9) . . ? C6B C5B C20B 121.1(11) . . ? C4B C5B C20B 122.1(11) . . ? C5B C6B C1B 121.9(9) . . ? C5B C6B C7B 118.5(9) . . ? C1B C6B C7B 119.4(10) . . ? O1B C7B C8B 118.1(9) . . ? O1B C7B C6B 121.4(11) . . ? C8B C7B C6B 119.4(10) . . ? O2B C23B N1B 123.2(12) . . ? O2B C23B C11B 121.1(11) . . ? N1B C23B C11B 115.2(10) . . ? C10B C11B C12B 118.4 . . ? C10B C11B C23B 123.9(9) . . ? C12B C11B C23B 117.7(8) . . ? C13B C12B C11B 120.3 . . ? C13B C12B H12B 119.8 . . ? C11B C12B H12B 119.8 . . ? C12B C13B C8B 121.5 . . ? C12B C13B H13B 119.2 . . ? C8B C13B H13B 119.2 . . ? C13B C8B C9B 118.5 . . ? C13B C8B C7B 120.3(6) . . ? C9B C8B C7B 121.0(6) . . ? C10B C9B C8B 120.0 . . ? C10B C9B H9B 120.0 . . ? C8B C9B H9B 120.0 . . ? C9B C10B C11B 121.3 . . ? C9B C10B H10B 119.3 . . ? C11B C10B H10B 119.4 . . ? C1B C14B C15B 107.1(13) . . ? C1B C14B C16B 111.1(14) . . ? C15B C14B C16B 110.9(14) . . ? C1B C14B H14B 109.2 . . ? C15B C14B H14B 109.2 . . ? C16B C14B H14B 109.2 . . ? C14B C15B H15D 109.5 . . ? C14B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C14B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C14B C16B H16D 109.5 . . ? C14B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C14B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C19B C17B C18B 116.1(14) . . ? C19B C17B C3B 117.0(14) . . ? C18B C17B C3B 114.5(14) . . ? C19B C17B H17B 101.9 . . ? C18B C17B H17B 101.9 . . ? C3B C17B H17B 101.9 . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C17B C19B H19D 109.5 . . ? C17B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C17B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C21B C20B C22B 112.8(15) . . ? C21B C20B C5B 112.3(13) . . ? C22B C20B C5B 111.1(14) . . ? C21B C20B H20B 106.8 . . ? C22B C20B H20B 106.8 . . ? C5B C20B H20B 106.8 . . ? C20B C21B H21D 109.5 . . ? C20B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C20B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C20B C22B H22D 109.5 . . ? C20B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C20B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? N1B C24B C25B 110.8(11) . . ? N1B C24B C27B 112.5(13) . . ? C25B C24B C27B 108.9(11) . . ? N1B C24B H24B 108.2 . . ? C25B C24B H24B 108.2 . . ? C27B C24B H24B 108.2 . . ? O3B C25B O4B 122.8(12) . . ? O3B C25B C24B 124.4(12) . . ? O4B C25B C24B 112.7(11) . . ? O4B C26B H26D 109.5 . . ? O4B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? O4B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C28B C27B C24B 115.6(12) . . ? C28B C27B H27C 108.4 . . ? C24B C27B H27C 108.4 . . ? C28B C27B H27D 108.4 . . ? C24B C27B H27D 108.4 . . ? H27C C27B H27D 107.4 . . ? C29B C28B C33B 117.3 . . ? C29B C28B C27B 120.4(10) . . ? C33B C28B C27B 122.2(10) . . ? C30B C29B C28B 121.3 . . ? C30B C29B H29B 119.4 . . ? C28B C29B H29B 119.4 . . ? C29B C30B C31B 121.0 . . ? C29B C30B H30B 119.5 . . ? C31B C30B H30B 119.6 . . ? C32B C31B C30B 118.1 . . ? C32B C31B H31B 120.9 . . ? C30B C31B H31B 121.0 . . ? C31B C32B C33B 121.1 . . ? C31B C32B H32B 119.4 . . ? C33B C32B H32B 119.4 . . ? C32B C33B C28B 121.2 . . ? C32B C33B H33B 119.4 . . ? C28B C33B H33B 119.5 . . ? C23C N1C C24C 121.7(18) . . ? C23C N1C H1C 119.1 . . ? C24C N1C H1C 119.1 . . ? C25C O4C C26C 116.7(19) . . ? C6C C1C C2C 121.4(11) . . ? C6C C1C C14C 95.6(9) . . ? C2C C1C C14C 142.8(12) . . ? C1C C2C C3C 117.3(12) . . ? C1C C2C H2C 121.4 . . ? C3C C2C H2C 121.4 . . ? C4C C3C C2C 120.5(11) . . ? C4C C3C C17C 119.4(13) . . ? C2C C3C C17C 120.1(13) . . ? C3C C4C C5C 123.1(12) . . ? C3C C4C H4C 118.4 . . ? C5C C4C H4C 118.4 . . ? C6C C5C C4C 114.0(10) . . ? C6C C5C C20C 123.9(12) . . ? C4C C5C C20C 121.5(12) . . ? C1C C6C C5C 123.7(10) . . ? C1C C6C C7C 95.6(8) . . ? C5C C6C C7C 140.7(11) . . ? O1C C7C C6C 115.2(14) . . ? O1C C7C C8C 110.9(12) . . ? C6C C7C C8C 117.0(12) . . ? O1C C7C C14C 111.5(12) . . ? C6C C7C C14C 84.5(7) . . ? C8C C7C C14C 115.5(15) . . ? O2C C23C N1C 121.4(19) . . ? O2C C23C C11C 122.2(18) . . ? N1C C23C C11C 114.6(12) . . ? C10C C11C C12C 117.6 . . ? C10C C11C C23C 123.0(10) . . ? C12C C11C C23C 119.3(10) . . ? C13C C12C C11C 120.9 . . ? C12C C13C C8C 121.7 . . ? C9C C8C C13C 117.1 . . ? C9C C8C C7C 120.2(8) . . ? C13C C8C C7C 122.5(8) . . ? C8C C9C C10C 121.2 . . ? C11C C10C C9C 121.1 . . ? C16C C14C C1C 116.2(13) . . ? C16C C14C C15C 110.8(13) . . ? C1C C14C C15C 114.3(15) . . ? C16C C14C C7C 118.7(14) . . ? C1C C14C C7C 83.9(7) . . ? C15C C14C C7C 110.7(13) . . ? C14C C15C H15G 109.5 . . ? C14C C15C H15H 109.5 . . ? H15G C15C H15H 109.5 . . ? C14C C15C H15I 109.5 . . ? H15G C15C H15I 109.5 . . ? H15H C15C H15I 109.5 . . ? C14C C16C H16G 109.5 . . ? C14C C16C H16H 109.5 . . ? H16G C16C H16H 109.5 . . ? C14C C16C H16I 109.5 . . ? H16G C16C H16I 109.5 . . ? H16H C16C H16I 109.5 . . ? C19C C17C C18C 112.5(16) . . ? C19C C17C C3C 112.5(16) . . ? C18C C17C C3C 110.6(15) . . ? C19C C17C H17C 106.9 . . ? C18C C17C H17C 106.9 . . ? C3C C17C H17C 106.9 . . ? C17C C18C H18G 109.5 . . ? C17C C18C H18H 109.5 . . ? H18G C18C H18H 109.5 . . ? C17C C18C H18I 109.5 . . ? H18G C18C H18I 109.5 . . ? H18H C18C H18I 109.5 . . ? C17C C19C H19G 109.5 . . ? C17C C19C H19H 109.5 . . ? H19G C19C H19H 109.5 . . ? C17C C19C H19I 109.5 . . ? H19G C19C H19I 109.5 . . ? H19H C19C H19I 109.5 . . ? C21C C20C C22C 108.9(15) . . ? C21C C20C C5C 111.3(15) . . ? C22C C20C C5C 111.0(16) . . ? C21C C20C H20C 108.5 . . ? C22C C20C H20C 108.5 . . ? C5C C20C H20C 108.5 . . ? C20C C21C H21G 109.5 . . ? C20C C21C H21H 109.5 . . ? H21G C21C H21H 109.5 . . ? C20C C21C H21I 109.5 . . ? H21G C21C H21I 109.5 . . ? H21H C21C H21I 109.5 . . ? C20C C22C H22G 109.5 . . ? C20C C22C H22H 109.5 . . ? H22G C22C H22H 109.5 . . ? C20C C22C H22I 109.5 . . ? H22G C22C H22I 109.5 . . ? H22H C22C H22I 109.5 . . ? N1C C24C C25C 114.5(15) . . ? N1C C24C C27C 111.3(15) . . ? C25C C24C C27C 112.0(14) . . ? N1C C24C H24C 106.1 . . ? C25C C24C H24C 106.1 . . ? C27C C24C H24C 106.1 . . ? O3C C25C O4C 121.7(16) . . ? O3C C25C C24C 122.3(15) . . ? O4C C25C C24C 115.6(14) . . ? C28C C27C C24C 114.0(13) . . ? C28C C27C H27E 108.7 . . ? C24C C27C H27E 108.7 . . ? C28C C27C H27F 108.7 . . ? C24C C27C H27F 108.7 . . ? H27E C27C H27F 107.6 . . ? C29C C28C C33C 118.1 . . ? C29C C28C C27C 121.5(11) . . ? C33C C28C C27C 120.4(11) . . ? C28C C29C C30C 120.6 . . ? C31C C30C C29C 121.3 . . ? C32C C31C C30C 118.1 . . ? C31C C32C C33C 120.8 . . ? C32C C33C C28C 121.1 . . ? C23D N1D C24D 121.6(11) . . ? C23D N1D H1D 119.2 . . ? C24D N1D H1D 119.2 . . ? C25D O4D C26D 118.2(12) . . ? C6D C1D C2D 122.0(9) . . ? C6D C1D C14D 95.8(7) . . ? C2D C1D C14D 142.1(9) . . ? C1D C2D C3D 117.4(9) . . ? C1D C2D H2D 121.3 . . ? C3D C2D H2D 121.3 . . ? C4D C3D C2D 120.5(9) . . ? C4D C3D C17D 122.2(10) . . ? C2D C3D C17D 117.2(10) . . ? C3D C4D C5D 122.2(10) . . ? C3D C4D H4D 118.9 . . ? C5D C4D H4D 118.9 . . ? C6D C5D C4D 115.8(9) . . ? C6D C5D C20D 123.2(10) . . ? C4D C5D C20D 120.3(10) . . ? C1D C6D C5D 121.8(8) . . ? C1D C6D C7D 95.7(7) . . ? C5D C6D C7D 142.3(9) . . ? O1D C7D C6D 112.6(10) . . ? O1D C7D C8D 110.3(7) . . ? C6D C7D C8D 114.5(9) . . ? O1D C7D C14D 111.2(8) . . ? C6D C7D C14D 84.6(6) . . ? C8D C7D C14D 121.4(9) . . ? O2D C23D N1D 119.4(10) . . ? O2D C23D C11D 121.5(10) . . ? N1D C23D C11D 118.1(8) . . ? C10D C11D C12D 117.6 . . ? C10D C11D C23D 123.0(6) . . ? C12D C11D C23D 118.5(7) . . ? C13D C12D C11D 120.9 . . ? C12D C13D C8D 121.7 . . ? C9D C8D C13D 117.1 . . ? C9D C8D C7D 120.7(5) . . ? C13D C8D C7D 121.3(5) . . ? C8D C9D C10D 121.2 . . ? C11D C10D C9D 121.1 . . ? C16D C14D C1D 114.7(10) . . ? C16D C14D C15D 110.4(11) . . ? C1D C14D C15D 114.0(11) . . ? C16D C14D C7D 120.8(13) . . ? C1D C14D C7D 83.9(6) . . ? C15D C14D C7D 110.9(10) . . ? C14D C15D H15J 109.5 . . ? C14D C15D H15K 109.5 . . ? H15J C15D H15K 109.5 . . ? C14D C15D H15L 109.5 . . ? H15J C15D H15L 109.5 . . ? H15K C15D H15L 109.5 . . ? C14D C16D H16J 109.5 . . ? C14D C16D H16K 109.5 . . ? H16J C16D H16K 109.5 . . ? C14D C16D H16L 109.5 . . ? H16J C16D H16L 109.5 . . ? H16K C16D H16L 109.5 . . ? C19D C17D C18D 116.2(14) . . ? C19D C17D C3D 112.7(11) . . ? C18D C17D C3D 109.9(11) . . ? C19D C17D H17D 105.7 . . ? C18D C17D H17D 105.7 . . ? C3D C17D H17D 105.7 . . ? C17D C18D H18J 109.5 . . ? C17D C18D H18K 109.5 . . ? H18J C18D H18K 109.5 . . ? C17D C18D H18L 109.5 . . ? H18J C18D H18L 109.5 . . ? H18K C18D H18L 109.5 . . ? C17D C19D H19J 109.5 . . ? C17D C19D H19K 109.5 . . ? H19J C19D H19K 109.5 . . ? C17D C19D H19L 109.5 . . ? H19J C19D H19L 109.5 . . ? H19K C19D H19L 109.5 . . ? C21D C20D C22D 111.1(13) . . ? C21D C20D C5D 110.9(13) . . ? C22D C20D C5D 108.5(12) . . ? C21D C20D H20D 108.7 . . ? C22D C20D H20D 108.7 . . ? C5D C20D H20D 108.7 . . ? C20D C21D H21J 109.5 . . ? C20D C21D H21K 109.5 . . ? H21J C21D H21K 109.5 . . ? C20D C21D H21L 109.5 . . ? H21J C21D H21L 109.5 . . ? H21K C21D H21L 109.5 . . ? C20D C22D H22J 109.5 . . ? C20D C22D H22K 109.5 . . ? H22J C22D H22K 109.5 . . ? C20D C22D H22L 109.5 . . ? H22J C22D H22L 109.5 . . ? H22K C22D H22L 109.5 . . ? N1D C24D C25D 114.8(10) . . ? N1D C24D C27D 109.9(11) . . ? C25D C24D C27D 110.2(10) . . ? N1D C24D H24D 107.2 . . ? C25D C24D H24D 107.2 . . ? C27D C24D H24D 107.2 . . ? O3D C25D O4D 125.5(11) . . ? O3D C25D C24D 120.6(10) . . ? O4D C25D C24D 113.1(9) . . ? C28D C27D C24D 110.3(9) . . ? C28D C27D H27G 109.6 . . ? C24D C27D H27G 109.6 . . ? C28D C27D H27H 109.6 . . ? C24D C27D H27H 109.6 . . ? H27G C27D H27H 108.1 . . ? C29D C28D C33D 118.1 . . ? C29D C28D C27D 121.5(8) . . ? C33D C28D C27D 120.4(8) . . ? C28D C29D C30D 120.6 . . ? C31D C30D C29D 121.3 . . ? C32D C31D C30D 118.2 . . ? C31D C32D C33D 120.8 . . ? C32D C33D C28D 121.1 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.194 _refine_diff_density_min -0.198 _refine_diff_density_rms 0.038 #===END data_32.7%C,59.6%D _database_code_depnum_ccdc_archive 'CCDC 799268' #TrackingRef '- 1.cif' #==================================================================== # start Validation Reply Form _vrf_PLAT201_32.7%C,59.6%D ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 36 RESPONSE: In the crystal there are reactant and photoproduct molecules. Part of atoms were refined isotropically in order to decrease a large number of the parameters in the refinement. ; _vrf_PLAT220_32.7%C,59.6%D ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.05 Ratio RESPONSE: This is a consequence of the strong reactant-product disorder in the crystal. ; # end Validation Reply Form #==================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 N O4' _chemical_formula_weight 513.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 22.199(4) _cell_length_b 9.3700(17) _cell_length_c 29.003(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6033(2) _cell_formula_units_Z 8 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 3.61 _cell_measurement_theta_max 13.19 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28179 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5399 _reflns_number_gt 3268 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CRYSALIS (Oxford Diffraction, 2003)' _computing_cell_refinement 'CRYSALIS (Oxford Diffraction, 2003)' _computing_data_reduction 'CRYSALIS (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SXELXL97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Owing to a reactant-product disorder, the following weak restraints from SHELXL97 were applied: DFIX, DANG and SIMU. DFIX and DANG restrained bond lengths and valence angles to target values. The target values were taken from the structures of the pure reactant and the pure product of crystal 1a. SIMU restrained displacement parameters of atoms of the products. ; _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^)+(0.1597P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5399 _refine_ls_number_parameters 719 _refine_ls_number_restraints 578 _refine_ls_R_factor_all 0.1427 _refine_ls_R_factor_gt 0.0910 _refine_ls_wR_factor_ref 0.2889 _refine_ls_wR_factor_gt 0.2415 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.175 _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 N1A N 0.3866(5) 0.9481(11) 0.4479(4) 0.064(3) Uani 0.673(11) 1 d PDU A 1 H1A H 0.3734 1.0340 0.4503 0.077 Uiso 0.673(11) 1 calc PR A 1 O1A O 0.1011(5) 1.1042(17) 0.3556(5) 0.117(5) Uani 0.673(11) 1 d PDU A 1 O2A O 0.3834(6) 0.7477(11) 0.4065(5) 0.073(4) Uani 0.673(11) 1 d PDU A 1 O3A O 0.5428(4) 0.9346(14) 0.4736(6) 0.143(5) Uani 0.673(11) 1 d PDU A 1 O4A O 0.4875(6) 1.0853(17) 0.4339(6) 0.101(4) Uani 0.673(11) 1 d PDU A 1 C1A C 0.1309(6) 1.0407(12) 0.2493(3) 0.084(5) Uiso 0.673(11) 1 d PD A 1 C2A C 0.1133(6) 0.9806(13) 0.2079(4) 0.098(5) Uiso 0.673(11) 1 d PD A 1 H2A H 0.1198 1.0324 0.1810 0.117 Uiso 0.673(11) 1 calc PR A 1 C3A C 0.0869(6) 0.8493(13) 0.2042(3) 0.088(4) Uiso 0.673(11) 1 d PDU A 1 C4A C 0.0790(8) 0.7732(13) 0.2443(3) 0.092(6) Uiso 0.673(11) 1 d PD A 1 H4A H 0.0635 0.6810 0.2428 0.111 Uiso 0.673(11) 1 calc PR A 1 C5A C 0.0937(7) 0.8316(10) 0.2876(3) 0.079(4) Uiso 0.673(11) 1 d PDU A 1 C6A C 0.1201(7) 0.9636(12) 0.2893(3) 0.081(6) Uiso 0.673(11) 1 d PDU A 1 C7A C 0.1367(4) 1.0283(11) 0.3351(3) 0.080(3) Uani 0.673(11) 1 d PDU A 1 C23A C 0.3591(6) 0.8580(14) 0.4194(6) 0.064(4) Uani 0.673(11) 1 d PDU A 1 C11A C 0.3010(3) 0.9064(11) 0.3994(3) 0.070(5) Uiso 0.673(11) 1 d PGDU A 1 C12A C 0.2853(4) 0.8527(10) 0.3563(3) 0.080(5) Uiso 0.673(11) 1 d PGDU A 1 H12A H 0.3109 0.7892 0.3414 0.096 Uiso 0.673(11) 1 d PG A 1 C13A C 0.2327(4) 0.8927(9) 0.3360(3) 0.077(4) Uiso 0.673(11) 1 d PGD A 1 H13A H 0.2229 0.8556 0.3072 0.092 Uiso 0.673(11) 1 d PG A 1 C8A C 0.1936(3) 0.9872(9) 0.3571(3) 0.070(3) Uiso 0.673(11) 1 d PGDU A 1 C9A C 0.2090(3) 1.0415(9) 0.4000(3) 0.077(3) Uiso 0.673(11) 1 d PGDU A 1 H9A H 0.1833 1.1049 0.4149 0.092 Uiso 0.673(11) 1 d PG A 1 C10A C 0.2622(4) 1.0013(10) 0.4205(3) 0.073(3) Uiso 0.673(11) 1 d PGDU A 1 H10A H 0.2723 1.0388 0.4492 0.087 Uiso 0.673(11) 1 d PG A 1 C14A C 0.1670(7) 1.1743(13) 0.2498(6) 0.130(5) Uani 0.673(11) 1 d PDU A 1 H14A H 0.1767 1.1965 0.2820 0.156 Uiso 0.673(11) 1 calc PR A 1 C15A C 0.1289(9) 1.2953(17) 0.2310(13) 0.209(11) Uani 0.673(11) 1 d PDU A 1 H15A H 0.1522 1.3817 0.2307 0.313 Uiso 0.673(11) 1 calc PR A 1 H15B H 0.0941 1.3080 0.2502 0.313 Uiso 0.673(11) 1 calc PR A 1 H15C H 0.1163 1.2728 0.2002 0.313 Uiso 0.673(11) 1 calc PR A 1 C16A C 0.2258(7) 1.166(2) 0.2232(10) 0.170(8) Uani 0.673(11) 1 d PDU A 1 H16A H 0.2454 1.2569 0.2237 0.255 Uiso 0.673(11) 1 calc PR A 1 H16B H 0.2176 1.1389 0.1918 0.255 Uiso 0.673(11) 1 calc PR A 1 H16C H 0.2515 1.0954 0.2371 0.255 Uiso 0.673(11) 1 calc PR A 1 C17A C 0.0709(7) 0.7872(18) 0.1581(4) 0.121(5) Uani 0.673(11) 1 d PDU A 1 H17A H 0.0635 0.8713 0.1389 0.146 Uiso 0.673(11) 1 calc PR A 1 C18A C 0.1245(9) 0.719(3) 0.1362(7) 0.183(10) Uani 0.673(11) 1 d PDU A 1 H18A H 0.1589 0.7799 0.1395 0.274 Uiso 0.673(11) 1 calc PR A 1 H18B H 0.1165 0.7031 0.1040 0.274 Uiso 0.673(11) 1 calc PR A 1 H18C H 0.1324 0.6289 0.1509 0.274 Uiso 0.673(11) 1 calc PR A 1 C19A C 0.0148(10) 0.710(3) 0.1562(8) 0.177(9) Uani 0.673(11) 1 d PDU A 1 H19A H 0.0078 0.6779 0.1252 0.266 Uiso 0.673(11) 1 calc PR A 1 H19B H -0.0176 0.7709 0.1657 0.266 Uiso 0.673(11) 1 calc PR A 1 H19C H 0.0168 0.6286 0.1763 0.266 Uiso 0.673(11) 1 calc PR A 1 C20A C 0.0820(5) 0.7469(12) 0.3313(3) 0.090(4) Uani 0.673(11) 1 d PDU A 1 H20A H 0.1024 0.7988 0.3562 0.108 Uiso 0.673(11) 1 calc PR A 1 C21A C 0.0167(7) 0.743(3) 0.3442(8) 0.142(7) Uani 0.673(11) 1 d PDU A 1 H21A H -0.0035 0.8238 0.3307 0.213 Uiso 0.673(11) 1 calc PR A 1 H21B H 0.0128 0.7471 0.3771 0.213 Uiso 0.673(11) 1 calc PR A 1 H21C H -0.0011 0.6567 0.3329 0.213 Uiso 0.673(11) 1 calc PR A 1 C22A C 0.1110(9) 0.6020(16) 0.3294(6) 0.152(7) Uani 0.673(11) 1 d PDU A 1 H22A H 0.1538 0.6118 0.3330 0.228 Uiso 0.673(11) 1 calc PR A 1 H22B H 0.1024 0.5580 0.3003 0.228 Uiso 0.673(11) 1 calc PR A 1 H22C H 0.0954 0.5435 0.3539 0.228 Uiso 0.673(11) 1 calc PR A 1 C24A C 0.4385(4) 0.9052(12) 0.4751(3) 0.070(3) Uani 0.673(11) 1 d PDU A 1 H24A H 0.4436 0.8021 0.4709 0.084 Uiso 0.673(11) 1 calc PR A 1 C25A C 0.4959(4) 0.9758(13) 0.4596(4) 0.083(4) Uani 0.673(11) 1 d PDU A 1 C26A C 0.5390(8) 1.1653(19) 0.4188(9) 0.128(7) Uani 0.673(11) 1 d PDU A 1 H26A H 0.5605 1.2007 0.4452 0.192 Uiso 0.673(11) 1 calc PR A 1 H26B H 0.5259 1.2441 0.4002 0.192 Uiso 0.673(11) 1 calc PR A 1 H26C H 0.5650 1.1047 0.4011 0.192 Uiso 0.673(11) 1 calc PR A 1 C27A C 0.4279(6) 0.9313(14) 0.5262(3) 0.086(4) Uani 0.673(11) 1 d PDU A 1 H27A H 0.4646 0.9095 0.5429 0.103 Uiso 0.673(11) 1 calc PR A 1 H27B H 0.4190 1.0315 0.5309 0.103 Uiso 0.673(11) 1 calc PR A 1 C28A C 0.3778(4) 0.8441(9) 0.5454(4) 0.075(3) Uiso 0.673(11) 1 d PGDU A 1 C29A C 0.3253(5) 0.9097(8) 0.5592(5) 0.113(5) Uiso 0.673(11) 1 d PGDU A 1 H29A H 0.3213 1.0079 0.5555 0.136 Uiso 0.673(11) 1 d PG A 1 C30A C 0.2789(4) 0.8334(12) 0.5781(5) 0.134(6) Uiso 0.673(11) 1 d PGU A 1 H30A H 0.2441 0.8806 0.5874 0.161 Uiso 0.673(11) 1 d PG A 1 C31A C 0.2830(5) 0.6877(12) 0.5837(5) 0.129(6) Uiso 0.673(11) 1 d PGU A 1 H31A H 0.2518 0.6362 0.5971 0.154 Uiso 0.673(11) 1 d PG A 1 C32A C 0.3341(6) 0.6214(8) 0.5690(5) 0.120(5) Uiso 0.673(11) 1 d PG A 1 H32A H 0.3373 0.5228 0.5717 0.144 Uiso 0.673(11) 1 d PG A 1 C33A C 0.3810(5) 0.6975(9) 0.5503(4) 0.100(4) Uiso 0.673(11) 1 d PGD A 1 H33A H 0.4155 0.6496 0.5408 0.120 Uiso 0.673(11) 1 d PG A 1 N1B N 0.3522(9) 0.449(3) 0.4286(8) 0.058(6) Uiso 0.404(11) 1 d PDU B 2 H1B H 0.3674 0.5309 0.4218 0.069 Uiso 0.404(11) 1 calc PR B 2 O1B O 0.6394(7) 0.6193(18) 0.5118(5) 0.094(5) Uiso 0.404(11) 1 d PDU B 2 O2B O 0.3538(10) 0.256(2) 0.4734(11) 0.081(9) Uiso 0.404(11) 1 d PDU B 2 O3B O 0.1963(7) 0.4004(19) 0.4274(8) 0.105(7) Uiso 0.404(11) 1 d PDU B 2 O4B O 0.2500(7) 0.5939(15) 0.4355(6) 0.074(5) Uiso 0.404(11) 1 d PDU B 2 C1B C 0.6052(9) 0.5904(19) 0.6208(5) 0.084(8) Uiso 0.404(11) 1 d PD B 2 C2B C 0.6252(9) 0.552(2) 0.6641(5) 0.100(8) Uiso 0.404(11) 1 d PD B 2 H2B H 0.6152 0.6087 0.6893 0.120 Uiso 0.404(11) 1 calc PR B 2 C3B C 0.6595(8) 0.4329(19) 0.6707(5) 0.080(6) Uiso 0.404(11) 1 d PD B 2 C4B C 0.6752(9) 0.352(2) 0.6332(5) 0.072(6) Uiso 0.404(11) 1 d PD B 2 H4B H 0.7001 0.2736 0.6376 0.087 Uiso 0.404(11) 1 calc PR B 2 C5B C 0.6551(14) 0.383(2) 0.5881(5) 0.12(2) Uiso 0.404(11) 1 d PD B 2 C6B C 0.6206(9) 0.5047(18) 0.5831(4) 0.069(10) Uiso 0.404(11) 1 d PDU B 2 C7B C 0.6036(6) 0.5544(17) 0.5359(4) 0.073(5) Uiso 0.404(11) 1 d PDU B 2 C23B C 0.3768(8) 0.369(3) 0.4617(8) 0.058(7) Uiso 0.404(11) 1 d PDU B 2 C11B C 0.4377(5) 0.4093(19) 0.4783(5) 0.100(12) Uiso 0.404(11) 1 d PGDU B 2 C12B C 0.4561(6) 0.3648(16) 0.5219(5) 0.053(7) Uiso 0.404(11) 1 d PGDU B 2 H12B H 0.4315 0.3045 0.5391 0.064 Uiso 0.404(11) 1 d PG B 2 C13B C 0.5098(6) 0.4091(13) 0.5395(4) 0.060(5) Uiso 0.404(11) 1 d PGDU B 2 H13B H 0.5214 0.3782 0.5686 0.072 Uiso 0.404(11) 1 d PG B 2 C8B C 0.5474(5) 0.4992(14) 0.5150(4) 0.073(5) Uiso 0.404(11) 1 d PGDU B 2 C9B C 0.5294(5) 0.5442(14) 0.4716(4) 0.057(4) Uiso 0.404(11) 1 d PGDU B 2 H9B H 0.5540 0.6046 0.4544 0.068 Uiso 0.404(11) 1 d PG B 2 C10B C 0.4750(6) 0.4997(17) 0.4538(4) 0.061(6) Uiso 0.404(11) 1 d PGDU B 2 H10B H 0.4632 0.5311 0.4248 0.073 Uiso 0.404(11) 1 d PG B 2 C14B C 0.5667(11) 0.721(2) 0.6152(9) 0.125(8) Uiso 0.404(11) 1 d PDU B 2 H14B H 0.5619 0.7417 0.5823 0.150 Uiso 0.404(11) 1 calc PR B 2 C15B C 0.5997(17) 0.843(3) 0.6384(14) 0.158(13) Uiso 0.404(11) 1 d PDU B 2 H15D H 0.5762 0.9284 0.6357 0.238 Uiso 0.404(11) 1 calc PR B 2 H15E H 0.6380 0.8566 0.6237 0.238 Uiso 0.404(11) 1 calc PR B 2 H15F H 0.6057 0.8208 0.6704 0.238 Uiso 0.404(11) 1 calc PR B 2 C16B C 0.5049(12) 0.698(5) 0.637(2) 0.168(15) Uiso 0.404(11) 1 d PDU B 2 H16D H 0.4895 0.6068 0.6280 0.252 Uiso 0.404(11) 1 calc PR B 2 H16E H 0.4780 0.7718 0.6265 0.252 Uiso 0.404(11) 1 calc PR B 2 H16F H 0.5084 0.7028 0.6699 0.252 Uiso 0.404(11) 1 calc PR B 2 C17B C 0.6729(10) 0.386(3) 0.7188(6) 0.144(12) Uiso 0.404(11) 1 d PDU B 2 H17B H 0.6537 0.4622 0.7367 0.173 Uiso 0.404(11) 1 calc PR B 2 C18B C 0.6392(14) 0.258(3) 0.7349(11) 0.147(13) Uiso 0.404(11) 1 d PDU B 2 H18D H 0.5968 0.2739 0.7307 0.221 Uiso 0.404(11) 1 calc PR B 2 H18E H 0.6474 0.2427 0.7670 0.221 Uiso 0.404(11) 1 calc PR B 2 H18F H 0.6515 0.1765 0.7175 0.221 Uiso 0.404(11) 1 calc PR B 2 C19B C 0.7341(10) 0.399(3) 0.7336(9) 0.097(8) Uiso 0.404(11) 1 d PDU B 2 H19D H 0.7550 0.4645 0.7139 0.146 Uiso 0.404(11) 1 calc PR B 2 H19E H 0.7533 0.3070 0.7320 0.146 Uiso 0.404(11) 1 calc PR B 2 H19F H 0.7352 0.4330 0.7648 0.146 Uiso 0.404(11) 1 calc PR B 2 C20B C 0.6701(11) 0.291(3) 0.5468(7) 0.124(8) Uiso 0.404(11) 1 d PDU B 2 H20B H 0.6680 0.3527 0.5196 0.149 Uiso 0.404(11) 1 calc PR B 2 C21B C 0.7331(11) 0.234(3) 0.5486(12) 0.125(10) Uiso 0.404(11) 1 d PDU B 2 H21D H 0.7589 0.3025 0.5632 0.187 Uiso 0.404(11) 1 calc PR B 2 H21E H 0.7471 0.2157 0.5178 0.187 Uiso 0.404(11) 1 calc PR B 2 H21F H 0.7336 0.1464 0.5659 0.187 Uiso 0.404(11) 1 calc PR B 2 C22B C 0.6236(16) 0.175(5) 0.540(2) 0.212(19) Uiso 0.404(11) 1 d PDU B 2 H22D H 0.5846 0.2172 0.5357 0.319 Uiso 0.404(11) 1 calc PR B 2 H22E H 0.6231 0.1126 0.5659 0.319 Uiso 0.404(11) 1 calc PR B 2 H22F H 0.6337 0.1206 0.5125 0.319 Uiso 0.404(11) 1 calc PR B 2 C24B C 0.2994(7) 0.397(3) 0.4039(6) 0.077(7) Uiso 0.404(11) 1 d PDU B 2 H24B H 0.2977 0.2927 0.4075 0.092 Uiso 0.404(11) 1 calc PR B 2 C25B C 0.2433(7) 0.4600(19) 0.4252(9) 0.080(7) Uiso 0.404(11) 1 d PDU B 2 C26B C 0.1974(11) 0.670(3) 0.4511(10) 0.083(8) Uiso 0.404(11) 1 d PDU B 2 H26D H 0.1935 0.7577 0.4340 0.125 Uiso 0.404(11) 1 calc PR B 2 H26E H 0.2016 0.6920 0.4833 0.125 Uiso 0.404(11) 1 calc PR B 2 H26F H 0.1622 0.6128 0.4464 0.125 Uiso 0.404(11) 1 calc PR B 2 C27B C 0.3016(10) 0.431(3) 0.3528(6) 0.078(6) Uiso 0.404(11) 1 d PDU B 2 H27C H 0.2640 0.4014 0.3388 0.094 Uiso 0.404(11) 1 calc PR B 2 H27D H 0.3048 0.5338 0.3492 0.094 Uiso 0.404(11) 1 calc PR B 2 C28B C 0.3522(8) 0.363(2) 0.3272(7) 0.078(7) Uiso 0.404(11) 1 d PGDU B 2 C29B C 0.4042(10) 0.4378(19) 0.3183(9) 0.119(9) Uiso 0.404(11) 1 d PGDU B 2 H29B H 0.4080 0.5308 0.3292 0.143 Uiso 0.404(11) 1 d PG B 2 C30B C 0.4505(9) 0.378(2) 0.2938(9) 0.145(10) Uiso 0.404(11) 1 d PGU B 2 H30B H 0.4851 0.4315 0.2881 0.173 Uiso 0.404(11) 1 d PG B 2 C31B C 0.4467(9) 0.240(3) 0.2775(9) 0.145(11) Uiso 0.404(11) 1 d PG B 2 H31B H 0.4778 0.2006 0.2603 0.175 Uiso 0.404(11) 1 d PG B 2 C32B C 0.3960(10) 0.164(2) 0.2871(8) 0.129(9) Uiso 0.404(11) 1 d PG B 2 H32B H 0.3930 0.0703 0.2771 0.155 Uiso 0.404(11) 1 d PG B 2 C33B C 0.3493(9) 0.224(2) 0.3114(7) 0.113(8) Uiso 0.404(11) 1 d PGDU B 2 H33B H 0.3150 0.1697 0.3174 0.136 Uiso 0.404(11) 1 d PG B 2 N1C N 0.3711(9) 0.949(3) 0.4558(7) 0.063(7) Uiso 0.327(11) 1 d PDU A 3 H1C H 0.3490 1.0208 0.4630 0.075 Uiso 0.327(11) 1 calc PR A 3 O1C O 0.1129(10) 1.154(2) 0.3415(7) 0.101(10) Uiso 0.327(11) 1 d PDU A 3 O2C O 0.3737(14) 0.744(3) 0.4163(11) 0.073(10) Uiso 0.327(11) 1 d PDU A 3 O3C O 0.5259(10) 0.987(4) 0.4902(10) 0.148(12) Uiso 0.327(11) 1 d PDU A 3 O4C O 0.4739(14) 1.071(5) 0.4304(13) 0.108(8) Uiso 0.327(11) 1 d PDU A 3 C1C C 0.1339(11) 1.009(2) 0.2444(5) 0.087(11) Uiso 0.327(11) 1 d PD A 3 C2C C 0.1159(12) 0.945(3) 0.2042(6) 0.110(13) Uiso 0.327(11) 1 d PD A 3 H2C H 0.1272 0.9814 0.1756 0.132 Uiso 0.327(11) 1 calc PR A 3 C3C C 0.0802(13) 0.825(3) 0.2079(6) 0.101(11) Uiso 0.327(11) 1 d PDU A 3 C4C C 0.0639(11) 0.772(2) 0.2500(6) 0.063(8) Uiso 0.327(11) 1 d PD A 3 H4C H 0.0398 0.6913 0.2511 0.076 Uiso 0.327(11) 1 calc PR A 3 C5C C 0.0818(13) 0.836(2) 0.2915(5) 0.099(12) Uiso 0.327(11) 1 d PDU A 3 C6C C 0.1173(10) 0.955(2) 0.2860(5) 0.065(10) Uiso 0.327(11) 1 d PDU A 3 C7C C 0.1502(6) 1.0659(16) 0.3147(5) 0.092(8) Uiso 0.327(11) 1 d PDU A 3 C23C C 0.3557(15) 0.868(3) 0.4194(12) 0.072(8) Uiso 0.327(11) 1 d PDU A 3 C11C C 0.3024(6) 0.9194(18) 0.3936(5) 0.046(7) Uiso 0.327(11) 1 d PGDU A 3 C12C C 0.2908(6) 0.8656(16) 0.3504(5) 0.042(6) Uiso 0.327(11) 1 d PGDU A 3 H12C H 0.3161 0.7962 0.3381 0.050 Uiso 0.327(11) 1 d PG A 3 C13C C 0.2430(6) 0.9124(15) 0.3254(4) 0.060(6) Uiso 0.327(11) 1 d PGD A 3 H13C H 0.2366 0.8754 0.2961 0.072 Uiso 0.327(11) 1 d PG A 3 C8C C 0.2036(5) 1.0136(15) 0.3425(5) 0.052(5) Uiso 0.327(11) 1 d PGDU A 3 C9C C 0.2173(6) 1.0730(14) 0.3840(5) 0.059(5) Uiso 0.327(11) 1 d PGDU A 3 H9C H 0.1933 1.1463 0.3955 0.071 Uiso 0.327(11) 1 d PG A 3 C10C C 0.2660(6) 1.0266(17) 0.4093(4) 0.068(7) Uiso 0.327(11) 1 d PGDU A 3 H10C H 0.2743 1.0689 0.4377 0.082 Uiso 0.327(11) 1 d PG A 3 C14C C 0.1648(9) 1.1404(19) 0.2640(6) 0.125(9) Uiso 0.327(11) 1 d PDU A 3 C15C C 0.1295(18) 1.279(3) 0.2592(13) 0.189(19) Uiso 0.327(11) 1 d PDU A 3 H15G H 0.0890 1.2647 0.2697 0.284 Uiso 0.327(11) 1 calc PR A 3 H15H H 0.1291 1.3080 0.2274 0.284 Uiso 0.327(11) 1 calc PR A 3 H15I H 0.1484 1.3521 0.2774 0.284 Uiso 0.327(11) 1 calc PR A 3 C16C C 0.2292(10) 1.162(3) 0.2511(10) 0.108(10) Uiso 0.327(11) 1 d PDU A 3 H16G H 0.2509 1.0743 0.2550 0.161 Uiso 0.327(11) 1 calc PR A 3 H16H H 0.2466 1.2343 0.2705 0.161 Uiso 0.327(11) 1 calc PR A 3 H16I H 0.2317 1.1918 0.2195 0.161 Uiso 0.327(11) 1 calc PR A 3 C17C C 0.0572(13) 0.751(3) 0.1640(7) 0.129(10) Uiso 0.327(11) 1 d PDU A 3 H17C H 0.0641 0.8180 0.1386 0.155 Uiso 0.327(11) 1 calc PR A 3 C18C C 0.0938(17) 0.624(4) 0.1540(15) 0.154(14) Uiso 0.327(11) 1 d PDU A 3 H18G H 0.1358 0.6492 0.1545 0.231 Uiso 0.327(11) 1 calc PR A 3 H18H H 0.0835 0.5876 0.1240 0.231 Uiso 0.327(11) 1 calc PR A 3 H18I H 0.0862 0.5521 0.1768 0.231 Uiso 0.327(11) 1 calc PR A 3 C19C C -0.0074(12) 0.724(6) 0.1652(19) 0.134(13) Uiso 0.327(11) 1 d PDU A 3 H19G H -0.0281 0.8103 0.1736 0.201 Uiso 0.327(11) 1 calc PR A 3 H19H H -0.0159 0.6511 0.1875 0.201 Uiso 0.327(11) 1 calc PR A 3 H19I H -0.0207 0.6936 0.1353 0.201 Uiso 0.327(11) 1 calc PR A 3 C20C C 0.0585(13) 0.785(3) 0.3378(6) 0.108(9) Uiso 0.327(11) 1 d PDU A 3 H20C H 0.0536 0.8687 0.3578 0.129 Uiso 0.327(11) 1 calc PR A 3 C21C C -0.0019(14) 0.713(5) 0.3335(16) 0.148(16) Uiso 0.327(11) 1 d PDU A 3 H21G H -0.0334 0.7822 0.3371 0.223 Uiso 0.327(11) 1 calc PR A 3 H21H H -0.0057 0.6409 0.3569 0.223 Uiso 0.327(11) 1 calc PR A 3 H21I H -0.0052 0.6693 0.3036 0.223 Uiso 0.327(11) 1 calc PR A 3 C22C C 0.1023(19) 0.684(5) 0.3608(15) 0.192(17) Uiso 0.327(11) 1 d PDU A 3 H22G H 0.0875 0.6593 0.3908 0.289 Uiso 0.327(11) 1 calc PR A 3 H22H H 0.1408 0.7301 0.3637 0.289 Uiso 0.327(11) 1 calc PR A 3 H22I H 0.1064 0.5997 0.3424 0.289 Uiso 0.327(11) 1 calc PR A 3 C24C C 0.4236(8) 0.918(3) 0.4828(6) 0.088(8) Uiso 0.327(11) 1 d PDU A 3 H24C H 0.4318 0.8158 0.4784 0.106 Uiso 0.327(11) 1 calc PR A 3 C25C C 0.4792(9) 0.994(4) 0.4681(8) 0.088(8) Uiso 0.327(11) 1 d PDU A 3 C26C C 0.527(2) 1.139(7) 0.413(2) 0.148(16) Uiso 0.327(11) 1 d PDU A 3 H26G H 0.5588 1.1312 0.4347 0.222 Uiso 0.327(11) 1 calc PR A 3 H26H H 0.5182 1.2380 0.4070 0.222 Uiso 0.327(11) 1 calc PR A 3 H26I H 0.5385 1.0940 0.3843 0.222 Uiso 0.327(11) 1 calc PR A 3 C27C C 0.4106(11) 0.937(3) 0.5339(6) 0.086(8) Uiso 0.327(11) 1 d PDU A 3 H27E H 0.4471 0.9179 0.5512 0.103 Uiso 0.327(11) 1 calc PR A 3 H27F H 0.3992 1.0353 0.5394 0.103 Uiso 0.327(11) 1 calc PR A 3 C28C C 0.3621(8) 0.8422(18) 0.5510(7) 0.080(7) Uiso 0.327(11) 1 d PGDU A 3 C29C C 0.3197(8) 0.8900(17) 0.5816(8) 0.099(8) Uiso 0.327(11) 1 d PGDU A 3 H29C H 0.3192 0.9857 0.5900 0.119 Uiso 0.327(11) 1 d PG A 3 C30C C 0.2780(8) 0.798(2) 0.6001(8) 0.105(8) Uiso 0.327(11) 1 d PGU A 3 H30C H 0.2505 0.8315 0.6217 0.127 Uiso 0.327(11) 1 d PG A 3 C31C C 0.2763(11) 0.657(2) 0.5874(10) 0.164(14) Uiso 0.327(11) 1 d PGU A 3 H31C H 0.2475 0.5955 0.5995 0.197 Uiso 0.327(11) 1 d PG A 3 C32C C 0.3180(13) 0.6096(17) 0.5563(10) 0.136(14) Uiso 0.327(11) 1 d PG A 3 H32C H 0.3175 0.5146 0.5471 0.163 Uiso 0.327(11) 1 d PG A 3 C33C C 0.3607(11) 0.700(2) 0.5386(8) 0.102(9) Uiso 0.327(11) 1 d PGD A 3 H33C H 0.3891 0.6657 0.5178 0.122 Uiso 0.327(11) 1 d PG A 3 N1D N 0.3584(7) 0.4392(17) 0.4233(6) 0.074(5) Uani 0.596(11) 1 d PDU B 4 H1D H 0.3752 0.5195 0.4170 0.089 Uiso 0.596(11) 1 calc PR B 4 O1D O 0.6213(4) 0.6821(10) 0.5271(3) 0.081(3) Uani 0.596(11) 1 d PDU B 4 O2D O 0.3641(7) 0.2384(12) 0.4657(6) 0.067(4) Uani 0.596(11) 1 d PDU B 4 O3D O 0.1992(5) 0.4336(16) 0.4017(7) 0.128(5) Uani 0.596(11) 1 d PDU B 4 O4D O 0.2576(5) 0.5662(13) 0.4494(4) 0.100(4) Uani 0.596(11) 1 d PDU B 4 C1D C 0.6069(6) 0.5618(13) 0.6268(4) 0.085(5) Uiso 0.596(11) 1 d PD B 4 C2D C 0.6263(6) 0.5097(15) 0.6682(4) 0.099(5) Uiso 0.596(11) 1 d PD B 4 H2D H 0.6173 0.5559 0.6958 0.119 Uiso 0.596(11) 1 calc PR B 4 C3D C 0.6598(6) 0.3851(15) 0.6675(4) 0.100(5) Uiso 0.596(11) 1 d PD B 4 C4D C 0.6709(8) 0.3170(16) 0.6272(4) 0.100(6) Uiso 0.596(11) 1 d PD B 4 H4D H 0.6910 0.2300 0.6280 0.120 Uiso 0.596(11) 1 calc PR B 4 C5D C 0.6531(7) 0.3724(14) 0.5845(4) 0.071(8) Uiso 0.596(11) 1 d PD B 4 C6D C 0.6204(7) 0.4963(14) 0.5863(4) 0.084(8) Uiso 0.596(11) 1 d PDU B 4 C7D C 0.5848(4) 0.5977(10) 0.5562(3) 0.088(4) Uani 0.596(11) 1 d PDU B 4 C23D C 0.3839(5) 0.3573(14) 0.4557(4) 0.062(5) Uani 0.596(11) 1 d PDU B 4 C11D C 0.4374(3) 0.4176(10) 0.4789(3) 0.037(4) Uiso 0.596(11) 1 d PGDU B 4 C12D C 0.4494(4) 0.3737(10) 0.5233(3) 0.089(8) Uiso 0.596(11) 1 d PGDU B 4 H12D H 0.4249 0.3052 0.5369 0.107 Uiso 0.596(11) 1 d PG B 4 C13D C 0.4964(4) 0.4288(10) 0.5473(3) 0.070(4) Uiso 0.596(11) 1 d PGDU B 4 H13D H 0.5030 0.3984 0.5774 0.084 Uiso 0.596(11) 1 d PG B 4 C8D C 0.5347(4) 0.5290(9) 0.5282(3) 0.062(3) Uiso 0.596(11) 1 d PGDU B 4 C9D C 0.5206(4) 0.5787(9) 0.4855(3) 0.068(3) Uiso 0.596(11) 1 d PGDU B 4 H9D H 0.5437 0.6511 0.4725 0.082 Uiso 0.596(11) 1 d PG B 4 C10D C 0.4726(4) 0.5237(10) 0.4610(3) 0.074(5) Uiso 0.596(11) 1 d PGDU B 4 H10D H 0.4640 0.5595 0.4318 0.089 Uiso 0.596(11) 1 d PG B 4 C14D C 0.5695(6) 0.6806(12) 0.6051(4) 0.117(6) Uani 0.596(11) 1 d PDU B 4 C15D C 0.5992(9) 0.8266(13) 0.6066(8) 0.128(6) Uani 0.596(11) 1 d PDU B 4 H15J H 0.6393 0.8200 0.5943 0.192 Uiso 0.596(11) 1 calc PR B 4 H15K H 0.6011 0.8594 0.6379 0.192 Uiso 0.596(11) 1 calc PR B 4 H15L H 0.5761 0.8927 0.5885 0.192 Uiso 0.596(11) 1 calc PR B 4 C16D C 0.5062(7) 0.689(3) 0.6224(10) 0.162(11) Uani 0.596(11) 1 d PDU B 4 H16J H 0.4885 0.5959 0.6223 0.243 Uiso 0.596(11) 1 calc PR B 4 H16K H 0.4833 0.7515 0.6028 0.243 Uiso 0.596(11) 1 calc PR B 4 H16L H 0.5062 0.7264 0.6533 0.243 Uiso 0.596(11) 1 calc PR B 4 C17D C 0.6848(8) 0.335(2) 0.7142(5) 0.149(9) Uani 0.596(11) 1 d PDU B 4 H17D H 0.6679 0.3995 0.7374 0.178 Uiso 0.596(11) 1 calc PR B 4 C18D C 0.6604(11) 0.193(3) 0.7247(9) 0.186(11) Uani 0.596(11) 1 d PDU B 4 H18J H 0.6185 0.1904 0.7167 0.278 Uiso 0.596(11) 1 calc PR B 4 H18K H 0.6650 0.1740 0.7570 0.278 Uiso 0.596(11) 1 calc PR B 4 H18L H 0.6818 0.1224 0.7072 0.278 Uiso 0.596(11) 1 calc PR B 4 C19D C 0.7495(8) 0.349(3) 0.7176(9) 0.171(10) Uani 0.596(11) 1 d PDU B 4 H19J H 0.7601 0.4484 0.7165 0.257 Uiso 0.596(11) 1 calc PR B 4 H19K H 0.7682 0.3000 0.6923 0.257 Uiso 0.596(11) 1 calc PR B 4 H19L H 0.7630 0.3086 0.7461 0.257 Uiso 0.596(11) 1 calc PR B 4 C20D C 0.6624(9) 0.2851(19) 0.5409(5) 0.151(7) Uani 0.596(11) 1 d PDU B 4 H20D H 0.6388 0.3252 0.5155 0.182 Uiso 0.596(11) 1 calc PR B 4 C21D C 0.7284(10) 0.283(2) 0.5284(9) 0.162(10) Uani 0.596(11) 1 d PDU B 4 H21J H 0.7436 0.3787 0.5279 0.243 Uiso 0.596(11) 1 calc PR B 4 H21K H 0.7333 0.2404 0.4986 0.243 Uiso 0.596(11) 1 calc PR B 4 H21L H 0.7501 0.2281 0.5509 0.243 Uiso 0.596(11) 1 calc PR B 4 C22D C 0.6423(15) 0.133(2) 0.5510(13) 0.226(14) Uani 0.596(11) 1 d PDU B 4 H22J H 0.6004 0.1333 0.5594 0.339 Uiso 0.596(11) 1 calc PR B 4 H22K H 0.6657 0.0951 0.5759 0.339 Uiso 0.596(11) 1 calc PR B 4 H22L H 0.6479 0.0753 0.5240 0.339 Uiso 0.596(11) 1 calc PR B 4 C24D C 0.3046(5) 0.4015(17) 0.3985(4) 0.075(5) Uani 0.596(11) 1 d PDU B 4 H24D H 0.2987 0.2984 0.4021 0.091 Uiso 0.596(11) 1 calc PR B 4 C25D C 0.2487(5) 0.4733(18) 0.4156(6) 0.089(5) Uani 0.596(11) 1 d PDU B 4 C26D C 0.2065(9) 0.643(2) 0.4673(8) 0.125(8) Uani 0.596(11) 1 d PDU B 4 H26J H 0.2147 0.7438 0.4664 0.187 Uiso 0.596(11) 1 calc PR B 4 H26K H 0.1991 0.6145 0.4985 0.187 Uiso 0.596(11) 1 calc PR B 4 H26L H 0.1717 0.6229 0.4488 0.187 Uiso 0.596(11) 1 calc PR B 4 C27D C 0.3126(7) 0.432(2) 0.3471(5) 0.086(5) Uani 0.596(11) 1 d PDU B 4 H27G H 0.2757 0.4076 0.3310 0.103 Uiso 0.596(11) 1 calc PR B 4 H27H H 0.3200 0.5329 0.3427 0.103 Uiso 0.596(11) 1 calc PR B 4 C28D C 0.3630(6) 0.3499(14) 0.3270(5) 0.085(5) Uiso 0.596(11) 1 d PGDU B 4 C29D C 0.4138(7) 0.4153(12) 0.3106(7) 0.126(7) Uiso 0.596(11) 1 d PGDU B 4 H29D H 0.4173 0.5141 0.3122 0.151 Uiso 0.596(11) 1 d PG B 4 C30D C 0.4599(6) 0.3364(16) 0.2917(7) 0.150(8) Uiso 0.596(11) 1 d PGU B 4 H30D H 0.4935 0.3830 0.2797 0.180 Uiso 0.596(11) 1 d PG B 4 C31D C 0.4573(6) 0.1904(16) 0.2901(6) 0.142(8) Uiso 0.596(11) 1 d PG B 4 H31D H 0.4889 0.1374 0.2779 0.170 Uiso 0.596(11) 1 d PG B 4 C32D C 0.4069(7) 0.1248(12) 0.3070(6) 0.135(7) Uiso 0.596(11) 1 d PG B 4 H32D H 0.4043 0.0258 0.3064 0.162 Uiso 0.596(11) 1 d PG B 4 C33D C 0.3601(6) 0.2033(14) 0.3249(5) 0.109(5) Uiso 0.596(11) 1 d PGDU B 4 H33D H 0.3260 0.1567 0.3358 0.131 Uiso 0.596(11) 1 d PG B 4 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 N1A 0.074(6) 0.046(4) 0.071(6) 0.004(4) 0.002(6) -0.002(5) O1A 0.094(7) 0.132(10) 0.126(9) -0.060(9) -0.024(7) 0.051(8) O2A 0.081(7) 0.054(5) 0.085(8) -0.005(4) 0.013(7) 0.003(4) O3A 0.079(6) 0.119(8) 0.230(15) 0.023(9) -0.013(8) 0.011(6) O4A 0.091(7) 0.085(7) 0.128(8) -0.002(6) 0.030(6) -0.009(6) C7A 0.078(7) 0.077(6) 0.084(8) -0.005(6) 0.004(6) 0.015(6) C23A 0.082(8) 0.039(5) 0.072(7) 0.014(5) -0.007(6) -0.010(5) C14A 0.145(12) 0.091(9) 0.155(13) -0.004(9) 0.002(11) -0.015(9) C15A 0.172(19) 0.101(11) 0.35(4) 0.028(18) 0.03(2) -0.015(12) C16A 0.142(16) 0.189(18) 0.18(2) 0.020(18) 0.002(15) -0.048(13) C17A 0.130(11) 0.140(11) 0.095(9) -0.008(9) -0.066(9) -0.004(10) C18A 0.23(2) 0.22(2) 0.100(12) -0.052(14) -0.029(14) 0.049(19) C19A 0.22(2) 0.21(2) 0.105(14) 0.027(14) -0.021(17) -0.06(2) C20A 0.099(9) 0.110(9) 0.060(7) 0.012(6) 0.000(6) 0.026(7) C21A 0.111(12) 0.187(18) 0.128(15) 0.051(14) 0.013(11) -0.022(13) C22A 0.179(16) 0.163(15) 0.115(13) 0.078(12) 0.006(11) 0.030(13) C24A 0.071(7) 0.055(5) 0.083(7) 0.001(5) -0.027(6) 0.010(5) C25A 0.063(7) 0.063(7) 0.123(10) -0.022(7) 0.004(7) -0.004(6) C26A 0.117(12) 0.083(10) 0.184(17) -0.033(10) 0.074(13) -0.037(8) C27A 0.097(9) 0.077(7) 0.084(8) -0.013(6) -0.017(7) 0.010(7) N1D 0.088(8) 0.040(5) 0.094(9) -0.005(6) -0.004(7) 0.008(5) O1D 0.065(5) 0.079(6) 0.099(6) 0.015(5) 0.001(5) -0.018(5) O2D 0.073(6) 0.041(5) 0.088(9) 0.005(5) -0.004(6) 0.011(5) O3D 0.081(7) 0.134(10) 0.168(15) -0.004(10) -0.015(8) 0.022(7) O4D 0.116(8) 0.104(8) 0.079(8) 0.007(7) 0.020(6) 0.041(6) C7D 0.098(9) 0.077(7) 0.090(9) 0.044(7) 0.028(8) 0.016(7) C23D 0.075(8) 0.057(7) 0.052(7) 0.000(5) 0.029(6) 0.037(6) C14D 0.119(11) 0.108(11) 0.123(12) 0.050(10) 0.034(9) 0.056(9) C15D 0.134(14) 0.097(11) 0.153(18) 0.013(11) -0.005(13) -0.002(10) C16D 0.108(14) 0.160(16) 0.22(3) 0.077(17) 0.041(14) 0.067(12) C17D 0.133(16) 0.23(2) 0.084(11) 0.053(14) -0.022(10) 0.076(16) C18D 0.18(2) 0.24(3) 0.134(17) 0.098(19) 0.023(16) 0.03(2) C19D 0.158(19) 0.22(2) 0.131(19) 0.034(18) -0.034(16) 0.050(18) C20D 0.166(15) 0.148(13) 0.140(14) 0.041(12) 0.067(12) 0.058(12) C21D 0.18(2) 0.155(18) 0.151(18) 0.070(15) 0.041(16) 0.025(15) C22D 0.26(3) 0.153(19) 0.26(3) -0.01(2) 0.11(3) 0.05(2) C24D 0.072(8) 0.059(7) 0.095(10) 0.000(6) -0.010(7) 0.018(6) C25D 0.082(10) 0.095(10) 0.089(11) 0.015(9) 0.019(8) 0.018(7) C26D 0.129(14) 0.118(14) 0.128(17) 0.020(12) 0.047(13) 0.063(11) C27D 0.090(10) 0.073(8) 0.095(10) 0.016(7) -0.012(8) 0.005(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1A C23A 1.330(8) . ? N1A C24A 1.453(8) . ? N1A H1A 0.8600 . ? O1A C7A 1.218(8) . ? O2A C23A 1.225(8) . ? O3A C25A 1.183(8) . ? O4A C25A 1.281(9) . ? O4A C26A 1.436(9) . ? C1A C2A 1.382(9) . ? C1A C6A 1.388(8) . ? C1A C14A 1.488(9) . ? C2A C3A 1.367(9) . ? C2A H2A 0.9300 . ? C3A C4A 1.375(9) . ? C3A C17A 1.500(8) . ? C4A C5A 1.408(8) . ? C4A H4A 0.9300 . ? C5A C6A 1.370(8) . ? C5A C20A 1.520(8) . ? C6A C7A 1.504(8) . ? C7A C8A 1.467(7) . ? C23A C11A 1.484(7) . ? C11A C10A 1.3819 . ? C11A C12A 1.3913 . ? C12A C13A 1.3615 . ? C12A H12A 0.9300 . ? C13A C8A 1.3834 . ? C13A H13A 0.9300 . ? C8A C9A 1.3878 . ? C9A C10A 1.3759 . ? C9A H9A 0.9301 . ? C10A H10A 0.9300 . ? C14A C15A 1.516(10) . ? C14A C16A 1.518(10) . ? C14A H14A 0.9800 . ? C15A H15A 0.9600 . ? C15A H15B 0.9600 . ? C15A H15C 0.9600 . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C17A C19A 1.444(10) . ? C17A C18A 1.493(10) . ? C17A H17A 0.9800 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C19A H19A 0.9600 . ? C19A H19B 0.9600 . ? C19A H19C 0.9600 . ? C20A C21A 1.497(10) . ? C20A C22A 1.505(10) . ? C20A H20A 0.9800 . ? C21A H21A 0.9600 . ? C21A H21B 0.9600 . ? C21A H21C 0.9600 . ? C22A H22A 0.9600 . ? C22A H22B 0.9600 . ? C22A H22C 0.9600 . ? C24A C25A 1.504(8) . ? C24A C27A 1.520(9) . ? C24A H24A 0.9800 . ? C26A H26A 0.9600 . ? C26A H26B 0.9600 . ? C26A H26C 0.9600 . ? C27A C28A 1.489(8) . ? C27A H27A 0.9700 . ? C27A H27B 0.9700 . ? C28A C29A 1.3755 . ? C28A C33A 1.3831 . ? C29A C30A 1.3701 . ? C29A H29A 0.9300 . ? C30A C31A 1.3771 . ? C30A H30A 0.9300 . ? C31A C32A 1.3617 . ? C31A H31A 0.9300 . ? C32A C33A 1.3726 . ? C32A H32A 0.9300 . ? C33A H33A 0.9299 . ? N1B C23B 1.335(9) . ? N1B C24B 1.457(10) . ? N1B H1B 0.8600 . ? O1B C7B 1.222(9) . ? O2B C23B 1.223(9) . ? O3B C25B 1.186(9) . ? O4B C25B 1.298(10) . ? O4B C26B 1.443(10) . ? C1B C2B 1.380(9) . ? C1B C6B 1.397(9) . ? C1B C14B 1.497(9) . ? C2B C3B 1.365(9) . ? C2B H2B 0.9300 . ? C3B C4B 1.369(9) . ? C3B C17B 1.492(9) . ? C4B C5B 1.411(9) . ? C4B H4B 0.9300 . ? C5B C6B 1.379(9) . ? C5B C20B 1.519(9) . ? C6B C7B 1.496(9) . ? C7B C8B 1.479(8) . ? C23B C11B 1.484(8) . ? C11B C10B 1.3819 . ? C11B C12B 1.3911 . ? C12B C13B 1.3615 . ? C12B H12B 0.9300 . ? C13B C8B 1.3834 . ? C13B H13B 0.9301 . ? C8B C9B 1.3879 . ? C9B C10B 1.3759 . ? C9B H9B 0.9301 . ? C10B H10B 0.9299 . ? C14B C15B 1.516(11) . ? C14B C16B 1.523(11) . ? C14B H14B 0.9800 . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? C17B C19B 1.429(10) . ? C17B C18B 1.488(10) . ? C17B H17B 0.9800 . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? C19B H19D 0.9600 . ? C19B H19E 0.9600 . ? C19B H19F 0.9600 . ? C20B C21B 1.498(10) . ? C20B C22B 1.512(11) . ? C20B H20B 0.9800 . ? C21B H21D 0.9600 . ? C21B H21E 0.9600 . ? C21B H21F 0.9600 . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? C24B C25B 1.512(9) . ? C24B C27B 1.519(10) . ? C24B H24B 0.9800 . ? C26B H26D 0.9600 . ? C26B H26E 0.9600 . ? C26B H26F 0.9600 . ? C27B C28B 1.488(9) . ? C27B H27C 0.9700 . ? C27B H27D 0.9700 . ? C28B C29B 1.3754 . ? C28B C33B 1.3832 . ? C29B C30B 1.3702 . ? C29B H29B 0.9300 . ? C30B C31B 1.3770 . ? C30B H30B 0.9301 . ? C31B C32B 1.3616 . ? C31B H31B 0.9301 . ? C32B C33B 1.3726 . ? C32B H32B 0.9300 . ? C33B H33B 0.9300 . ? N1C C23C 1.346(10) . ? N1C C24C 1.435(10) . ? N1C H1C 0.8600 . ? O1C C7C 1.406(10) . ? O2C C23C 1.232(10) . ? O3C C25C 1.218(10) . ? O4C C25C 1.312(10) . ? O4C C26C 1.432(11) . ? C1C C6C 1.357(9) . ? C1C C2C 1.371(9) . ? C1C C14C 1.520(9) . ? C2C C3C 1.384(10) . ? C2C H2C 0.9300 . ? C3C C4C 1.364(10) . ? C3C C17C 1.536(10) . ? C4C C5C 1.401(9) . ? C4C H4C 0.9300 . ? C5C C6C 1.378(9) . ? C5C C20C 1.516(10) . ? C6C C7C 1.517(9) . ? C7C C8C 1.515(8) . ? C7C C14C 1.659(10) . ? C23C C11C 1.482(9) . ? C11C C10C 1.3672 . ? C11C C12C 1.3750 . ? C12C C13C 1.3582 . ? C12C H12C 0.9301 . ? C13C C8C 1.3817 . ? C13C H13C 0.9301 . ? C8C C9C 1.3608 . ? C9C C10C 1.3795 . ? C9C H9C 0.9300 . ? C10C H10C 0.9300 . ? C14C C16C 1.492(10) . ? C14C C15C 1.524(10) . ? C15C H15G 0.9600 . ? C15C H15H 0.9600 . ? C15C H15I 0.9600 . ? C16C H16G 0.9600 . ? C16C H16H 0.9600 . ? C16C H16I 0.9600 . ? C17C C19C 1.455(11) . ? C17C C18C 1.471(11) . ? C17C H17C 0.9800 . ? C18C H18G 0.9600 . ? C18C H18H 0.9600 . ? C18C H18I 0.9600 . ? C19C H19G 0.9600 . ? C19C H19H 0.9600 . ? C19C H19I 0.9600 . ? C20C C21C 1.507(11) . ? C20C C22C 1.510(11) . ? C20C H20C 0.9800 . ? C21C H21G 0.9600 . ? C21C H21H 0.9600 . ? C21C H21I 0.9600 . ? C22C H22G 0.9600 . ? C22C H22H 0.9600 . ? C22C H22I 0.9600 . ? C24C C25C 1.490(10) . ? C24C C27C 1.519(10) . ? C24C H24C 0.9800 . ? C26C H26G 0.9600 . ? C26C H26H 0.9600 . ? C26C H26I 0.9600 . ? C27C C28C 1.480(9) . ? C27C H27E 0.9700 . ? C27C H27F 0.9700 . ? C28C C29C 1.3689 . ? C28C C33C 1.3759 . ? C29C C30C 1.3762 . ? C29C H29C 0.9300 . ? C30C C31C 1.3694 . ? C30C H30C 0.9300 . ? C31C C32C 1.3674 . ? C31C H31C 0.9299 . ? C32C C33C 1.3743 . ? C32C H32C 0.9300 . ? C33C H33C 0.9300 . ? N1D C23D 1.338(8) . ? N1D C24D 1.439(9) . ? N1D H1D 0.8600 . ? O1D C7D 1.413(8) . ? O2D C23D 1.232(8) . ? O3D C25D 1.227(9) . ? O4D C25D 1.327(9) . ? O4D C26D 1.439(9) . ? C1D C6D 1.358(9) . ? C1D C2D 1.367(9) . ? C1D C14D 1.525(9) . ? C2D C3D 1.384(9) . ? C2D H2D 0.9300 . ? C3D C4D 1.354(9) . ? C3D C17D 1.536(9) . ? C4D C5D 1.400(9) . ? C4D H4D 0.9300 . ? C5D C6D 1.371(8) . ? C5D C20D 1.522(9) . ? C6D C7D 1.513(8) . ? C7D C8D 1.521(8) . ? C7D C14D 1.652(9) . ? C23D C11D 1.480(7) . ? C11D C10D 1.3671 . ? C11D C12D 1.3750 . ? C12D C13D 1.3583 . ? C12D H12D 0.9300 . ? C13D C8D 1.3818 . ? C13D H13D 0.9300 . ? C8D C9D 1.3608 . ? C9D C10D 1.3795 . ? C9D H9D 0.9300 . ? C10D H10D 0.9300 . ? C14D C16D 1.494(9) . ? C14D C15D 1.519(10) . ? C15D H15J 0.9600 . ? C15D H15K 0.9600 . ? C15D H15L 0.9600 . ? C16D H16J 0.9600 . ? C16D H16K 0.9600 . ? C16D H16L 0.9600 . ? C17D C19D 1.445(10) . ? C17D C18D 1.465(10) . ? C17D H17D 0.9800 . ? C18D H18J 0.9600 . ? C18D H18K 0.9600 . ? C18D H18L 0.9600 . ? C19D H19J 0.9600 . ? C19D H19K 0.9600 . ? C19D H19L 0.9600 . ? C20D C21D 1.507(10) . ? C20D C22D 1.520(10) . ? C20D H20D 0.9800 . ? C21D H21J 0.9600 . ? C21D H21K 0.9600 . ? C21D H21L 0.9600 . ? C22D H22J 0.9600 . ? C22D H22K 0.9600 . ? C22D H22L 0.9600 . ? C24D C25D 1.495(9) . ? C24D C27D 1.529(9) . ? C24D H24D 0.9800 . ? C26D H26J 0.9600 . ? C26D H26K 0.9600 . ? C26D H26L 0.9600 . ? C27D C28D 1.477(8) . ? C27D H27G 0.9700 . ? C27D H27H 0.9700 . ? C28D C29D 1.3689 . ? C28D C33D 1.3759 . ? C29D C30D 1.3762 . ? C29D H29D 0.9300 . ? C30D C31D 1.3694 . ? C30D H30D 0.9300 . ? C31D C32D 1.3673 . ? C31D H31D 0.9300 . ? C32D C33D 1.3743 . ? C32D H32D 0.9300 . ? C33D H33D 0.9301 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23A N1A C24A 121.8(8) . . ? C23A N1A H1A 119.1 . . ? C24A N1A H1A 119.1 . . ? C25A O4A C26A 118.7(12) . . ? C2A C1A C6A 117.8(8) . . ? C2A C1A C14A 120.3(9) . . ? C6A C1A C14A 121.5(10) . . ? C3A C2A C1A 123.7(9) . . ? C3A C2A H2A 118.2 . . ? C1A C2A H2A 118.2 . . ? C2A C3A C4A 117.2(8) . . ? C2A C3A C17A 121.3(10) . . ? C4A C3A C17A 121.4(9) . . ? C3A C4A C5A 121.5(9) . . ? C3A C4A H4A 119.3 . . ? C5A C4A H4A 119.3 . . ? C6A C5A C4A 118.9(8) . . ? C6A C5A C20A 120.9(8) . . ? C4A C5A C20A 120.2(8) . . ? C5A C6A C1A 120.8(7) . . ? C5A C6A C7A 120.1(8) . . ? C1A C6A C7A 119.1(8) . . ? O1A C7A C8A 119.9(8) . . ? O1A C7A C6A 120.6(9) . . ? C8A C7A C6A 119.2(8) . . ? O2A C23A N1A 121.5(9) . . ? O2A C23A C11A 121.4(8) . . ? N1A C23A C11A 116.6(7) . . ? C10A C11A C12A 118.3 . . ? C10A C11A C23A 124.4(6) . . ? C12A C11A C23A 117.3(6) . . ? C13A C12A C11A 120.3 . . ? C12A C13A C8A 121.5 . . ? C13A C8A C9A 118.5 . . ? C13A C8A C7A 121.1(5) . . ? C9A C8A C7A 120.4(5) . . ? C10A C9A C8A 120.0 . . ? C9A C10A C11A 121.3 . . ? C1A C14A C15A 108.9(10) . . ? C1A C14A C16A 114.4(11) . . ? C15A C14A C16A 109.7(12) . . ? C1A C14A H14A 107.9 . . ? C15A C14A H14A 107.9 . . ? C16A C14A H14A 107.9 . . ? C14A C15A H15A 109.5 . . ? C14A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C14A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C14A C16A H16A 109.5 . . ? C14A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C14A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C19A C17A C18A 117.0(14) . . ? C19A C17A C3A 115.7(12) . . ? C18A C17A C3A 111.0(10) . . ? C19A C17A H17A 103.7 . . ? C18A C17A H17A 103.7 . . ? C3A C17A H17A 103.7 . . ? C17A C18A H18A 109.5 . . ? C17A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C17A C19A H19A 109.5 . . ? C17A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C17A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C21A C20A C22A 113.8(11) . . ? C21A C20A C5A 112.6(10) . . ? C22A C20A C5A 111.6(9) . . ? C21A C20A H20A 106.0 . . ? C22A C20A H20A 106.0 . . ? C5A C20A H20A 106.0 . . ? C20A C21A H21A 109.5 . . ? C20A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C20A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C20A C22A H22A 109.5 . . ? C20A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C20A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? N1A C24A C25A 112.8(8) . . ? N1A C24A C27A 111.3(9) . . ? C25A C24A C27A 110.5(8) . . ? N1A C24A H24A 107.3 . . ? C25A C24A H24A 107.3 . . ? C27A C24A H24A 107.3 . . ? O3A C25A O4A 126.1(10) . . ? O3A C25A C24A 120.0(9) . . ? O4A C25A C24A 113.7(8) . . ? C28A C27A C24A 113.0(8) . . ? C28A C27A H27A 109.0 . . ? C24A C27A H27A 109.0 . . ? C28A C27A H27B 109.0 . . ? C24A C27A H27B 109.0 . . ? H27A C27A H27B 107.8 . . ? C29A C28A C33A 117.2 . . ? C29A C28A C27A 119.7(7) . . ? C33A C28A C27A 123.0(7) . . ? C30A C29A C28A 121.3 . . ? C29A C30A C31A 121.0 . . ? C32A C31A C30A 118.1 . . ? C31A C32A C33A 121.2 . . ? C32A C33A C28A 121.2 . . ? C23B N1B C24B 119.4(14) . . ? C23B N1B H1B 120.3 . . ? C24B N1B H1B 120.3 . . ? C25B O4B C26B 117.4(13) . . ? C2B C1B C6B 118.8(10) . . ? C2B C1B C14B 119.6(11) . . ? C6B C1B C14B 121.6(12) . . ? C3B C2B C1B 121.4(11) . . ? C3B C2B H2B 119.3 . . ? C1B C2B H2B 119.3 . . ? C2B C3B C4B 118.8(10) . . ? C2B C3B C17B 118.9(12) . . ? C4B C3B C17B 122.0(12) . . ? C3B C4B C5B 122.7(11) . . ? C3B C4B H4B 118.6 . . ? C5B C4B H4B 118.6 . . ? C6B C5B C4B 116.4(10) . . ? C6B C5B C20B 120.7(11) . . ? C4B C5B C20B 122.9(11) . . ? C5B C6B C1B 121.8(9) . . ? C5B C6B C7B 119.5(10) . . ? C1B C6B C7B 118.4(10) . . ? O1B C7B C8B 119.3(10) . . ? O1B C7B C6B 121.0(12) . . ? C8B C7B C6B 118.6(11) . . ? O2B C23B N1B 121.0(13) . . ? O2B C23B C11B 120.7(13) . . ? N1B C23B C11B 117.6(11) . . ? C10B C11B C12B 118.3 . . ? C10B C11B C23B 122.3(8) . . ? C12B C11B C23B 119.1(8) . . ? C13B C12B C11B 120.3 . . ? C13B C12B H12B 119.8 . . ? C11B C12B H12B 119.8 . . ? C12B C13B C8B 121.5 . . ? C12B C13B H13B 119.2 . . ? C8B C13B H13B 119.2 . . ? C13B C8B C9B 118.5 . . ? C13B C8B C7B 120.8(7) . . ? C9B C8B C7B 120.6(7) . . ? C10B C9B C8B 120.0 . . ? C10B C9B H9B 120.0 . . ? C8B C9B H9B 120.0 . . ? C9B C10B C11B 121.3 . . ? C9B C10B H10B 119.3 . . ? C11B C10B H10B 119.3 . . ? C1B C14B C15B 107.0(13) . . ? C1B C14B C16B 111.0(15) . . ? C15B C14B C16B 110.7(15) . . ? C1B C14B H14B 109.3 . . ? C15B C14B H14B 109.3 . . ? C16B C14B H14B 109.3 . . ? C14B C15B H15D 109.5 . . ? C14B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C14B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C14B C16B H16D 109.5 . . ? C14B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C14B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C19B C17B C18B 116.7(14) . . ? C19B C17B C3B 116.6(14) . . ? C18B C17B C3B 115.4(14) . . ? C19B C17B H17B 101.3 . . ? C18B C17B H17B 101.3 . . ? C3B C17B H17B 101.3 . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C17B C19B H19D 109.5 . . ? C17B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C17B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C21B C20B C22B 112.7(15) . . ? C21B C20B C5B 112.4(13) . . ? C22B C20B C5B 111.8(15) . . ? C21B C20B H20B 106.5 . . ? C22B C20B H20B 106.5 . . ? C5B C20B H20B 106.5 . . ? C20B C21B H21D 109.5 . . ? C20B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C20B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C20B C22B H22D 109.5 . . ? C20B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C20B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? N1B C24B C25B 109.3(13) . . ? N1B C24B C27B 112.4(14) . . ? C25B C24B C27B 109.9(12) . . ? N1B C24B H24B 108.4 . . ? C25B C24B H24B 108.4 . . ? C27B C24B H24B 108.4 . . ? O3B C25B O4B 122.9(13) . . ? O3B C25B C24B 124.2(13) . . ? O4B C25B C24B 112.3(12) . . ? O4B C26B H26D 109.5 . . ? O4B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? O4B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C28B C27B C24B 114.8(13) . . ? C28B C27B H27C 108.6 . . ? C24B C27B H27C 108.6 . . ? C28B C27B H27D 108.6 . . ? C24B C27B H27D 108.6 . . ? H27C C27B H27D 107.5 . . ? C29B C28B C33B 117.2 . . ? C29B C28B C27B 120.5(11) . . ? C33B C28B C27B 122.3(11) . . ? C30B C29B C28B 121.3 . . ? C30B C29B H29B 119.3 . . ? C28B C29B H29B 119.3 . . ? C29B C30B C31B 121.0 . . ? C29B C30B H30B 119.5 . . ? C31B C30B H30B 119.5 . . ? C32B C31B C30B 118.1 . . ? C32B C31B H31B 120.9 . . ? C30B C31B H31B 120.9 . . ? C31B C32B C33B 121.2 . . ? C31B C32B H32B 119.4 . . ? C33B C32B H32B 119.4 . . ? C32B C33B C28B 121.2 . . ? C32B C33B H33B 119.4 . . ? C28B C33B H33B 119.4 . . ? C23C N1C C24C 121.2(15) . . ? C23C N1C H1C 119.4 . . ? C24C N1C H1C 119.4 . . ? C25C O4C C26C 118.1(18) . . ? C6C C1C C2C 121.0(11) . . ? C6C C1C C14C 95.3(8) . . ? C2C C1C C14C 143.4(12) . . ? C1C C2C C3C 117.2(12) . . ? C1C C2C H2C 121.4 . . ? C3C C2C H2C 121.4 . . ? C4C C3C C2C 120.9(11) . . ? C4C C3C C17C 119.5(12) . . ? C2C C3C C17C 119.5(12) . . ? C3C C4C C5C 122.9(11) . . ? C3C C4C H4C 118.6 . . ? C5C C4C H4C 118.6 . . ? C6C C5C C4C 114.0(10) . . ? C6C C5C C20C 123.6(12) . . ? C4C C5C C20C 122.1(11) . . ? C1C C6C C5C 124.1(10) . . ? C1C C6C C7C 95.9(8) . . ? C5C C6C C7C 140.0(10) . . ? O1C C7C C8C 110.9(11) . . ? O1C C7C C6C 115.0(13) . . ? C8C C7C C6C 116.6(11) . . ? O1C C7C C14C 111.0(11) . . ? C8C C7C C14C 117.0(13) . . ? C6C C7C C14C 84.0(7) . . ? O2C C23C N1C 120.6(17) . . ? O2C C23C C11C 122.1(17) . . ? N1C C23C C11C 114.4(11) . . ? C10C C11C C12C 117.6 . . ? C10C C11C C23C 122.9(9) . . ? C12C C11C C23C 119.3(9) . . ? C13C C12C C11C 120.9 . . ? C12C C13C C8C 121.7 . . ? C9C C8C C13C 117.1 . . ? C9C C8C C7C 120.9(7) . . ? C13C C8C C7C 121.8(7) . . ? C8C C9C C10C 121.2 . . ? C11C C10C C9C 121.1 . . ? C16C C14C C1C 116.7(13) . . ? C16C C14C C15C 110.7(13) . . ? C1C C14C C15C 115.2(14) . . ? C16C C14C C7C 117.9(13) . . ? C1C C14C C7C 84.3(7) . . ? C15C C14C C7C 109.8(13) . . ? C14C C15C H15G 109.5 . . ? C14C C15C H15H 109.5 . . ? H15G C15C H15H 109.5 . . ? C14C C15C H15I 109.5 . . ? H15G C15C H15I 109.5 . . ? H15H C15C H15I 109.5 . . ? C14C C16C H16G 109.5 . . ? C14C C16C H16H 109.5 . . ? H16G C16C H16H 109.5 . . ? C14C C16C H16I 109.5 . . ? H16G C16C H16I 109.5 . . ? H16H C16C H16I 109.5 . . ? C19C C17C C18C 114.2(16) . . ? C19C C17C C3C 112.6(15) . . ? C18C C17C C3C 110.1(15) . . ? C19C C17C H17C 106.5 . . ? C18C C17C H17C 106.5 . . ? C3C C17C H17C 106.5 . . ? C17C C18C H18G 109.5 . . ? C17C C18C H18H 109.5 . . ? H18G C18C H18H 109.5 . . ? C17C C18C H18I 109.5 . . ? H18G C18C H18I 109.5 . . ? H18H C18C H18I 109.5 . . ? C17C C19C H19G 109.5 . . ? C17C C19C H19H 109.5 . . ? H19G C19C H19H 109.5 . . ? C17C C19C H19I 109.5 . . ? H19G C19C H19I 109.5 . . ? H19H C19C H19I 109.5 . . ? C21C C20C C22C 109.2(15) . . ? C21C C20C C5C 111.7(15) . . ? C22C C20C C5C 111.5(15) . . ? C21C C20C H20C 108.1 . . ? C22C C20C H20C 108.1 . . ? C5C C20C H20C 108.1 . . ? C20C C21C H21G 109.5 . . ? C20C C21C H21H 109.5 . . ? H21G C21C H21H 109.5 . . ? C20C C21C H21I 109.5 . . ? H21G C21C H21I 109.5 . . ? H21H C21C H21I 109.5 . . ? C20C C22C H22G 109.5 . . ? C20C C22C H22H 109.5 . . ? H22G C22C H22H 109.5 . . ? C20C C22C H22I 109.5 . . ? H22G C22C H22I 109.5 . . ? H22H C22C H22I 109.5 . . ? N1C C24C C25C 114.8(14) . . ? N1C C24C C27C 110.6(14) . . ? C25C C24C C27C 112.4(13) . . ? N1C C24C H24C 106.1 . . ? C25C C24C H24C 106.1 . . ? C27C C24C H24C 106.1 . . ? O3C C25C O4C 122.8(15) . . ? O3C C25C C24C 121.9(14) . . ? O4C C25C C24C 115.3(13) . . ? C28C C27C C24C 113.2(12) . . ? C28C C27C H27E 108.9 . . ? C24C C27C H27E 108.9 . . ? C28C C27C H27F 108.9 . . ? C24C C27C H27F 108.9 . . ? H27E C27C H27F 107.7 . . ? C29C C28C C33C 118.0 . . ? C29C C28C C27C 121.4(10) . . ? C33C C28C C27C 120.4(10) . . ? C28C C29C C30C 120.7 . . ? C31C C30C C29C 121.2 . . ? C32C C31C C30C 118.1 . . ? C31C C32C C33C 120.9 . . ? C32C C33C C28C 121.0 . . ? C23D N1D C24D 124.1(11) . . ? C23D N1D H1D 117.9 . . ? C24D N1D H1D 117.9 . . ? C25D O4D C26D 118.5(12) . . ? C6D C1D C2D 122.0(9) . . ? C6D C1D C14D 95.4(7) . . ? C2D C1D C14D 142.6(9) . . ? C1D C2D C3D 117.2(9) . . ? C1D C2D H2D 121.4 . . ? C3D C2D H2D 121.4 . . ? C4D C3D C2D 120.5(9) . . ? C4D C3D C17D 123.4(10) . . ? C2D C3D C17D 116.1(10) . . ? C3D C4D C5D 122.6(10) . . ? C3D C4D H4D 118.7 . . ? C5D C4D H4D 118.7 . . ? C6D C5D C4D 115.5(9) . . ? C6D C5D C20D 124.0(9) . . ? C4D C5D C20D 119.9(10) . . ? C1D C6D C5D 122.2(8) . . ? C1D C6D C7D 95.7(7) . . ? C5D C6D C7D 141.9(9) . . ? O1D C7D C6D 113.4(9) . . ? O1D C7D C8D 109.7(7) . . ? C6D C7D C8D 115.1(8) . . ? O1D C7D C14D 111.6(8) . . ? C6D C7D C14D 84.7(6) . . ? C8D C7D C14D 120.5(9) . . ? O2D C23D N1D 122.2(9) . . ? O2D C23D C11D 121.7(9) . . ? N1D C23D C11D 116.1(8) . . ? C10D C11D C12D 117.6 . . ? C10D C11D C23D 124.3(6) . . ? C12D C11D C23D 117.8(6) . . ? C13D C12D C11D 120.9 . . ? C12D C13D C8D 121.7 . . ? C9D C8D C13D 117.1 . . ? C9D C8D C7D 120.6(5) . . ? C13D C8D C7D 121.6(5) . . ? C8D C9D C10D 121.2 . . ? C11D C10D C9D 121.1 . . ? C16D C14D C15D 110.4(11) . . ? C16D C14D C1D 114.5(10) . . ? C15D C14D C1D 114.2(10) . . ? C16D C14D C7D 120.5(13) . . ? C15D C14D C7D 111.0(10) . . ? C1D C14D C7D 84.2(6) . . ? C14D C15D H15J 109.5 . . ? C14D C15D H15K 109.5 . . ? H15J C15D H15K 109.5 . . ? C14D C15D H15L 109.5 . . ? H15J C15D H15L 109.5 . . ? H15K C15D H15L 109.5 . . ? C14D C16D H16J 109.5 . . ? C14D C16D H16K 109.5 . . ? H16J C16D H16K 109.5 . . ? C14D C16D H16L 109.5 . . ? H16J C16D H16L 109.5 . . ? H16K C16D H16L 109.5 . . ? C19D C17D C18D 115.9(14) . . ? C19D C17D C3D 112.9(12) . . ? C18D C17D C3D 109.1(12) . . ? C19D C17D H17D 106.0 . . ? C18D C17D H17D 106.0 . . ? C3D C17D H17D 106.0 . . ? C17D C18D H18J 109.5 . . ? C17D C18D H18K 109.5 . . ? H18J C18D H18K 109.5 . . ? C17D C18D H18L 109.5 . . ? H18J C18D H18L 109.5 . . ? H18K C18D H18L 109.5 . . ? C17D C19D H19J 109.5 . . ? C17D C19D H19K 109.5 . . ? H19J C19D H19K 109.5 . . ? C17D C19D H19L 109.5 . . ? H19J C19D H19L 109.5 . . ? H19K C19D H19L 109.5 . . ? C21D C20D C22D 108.6(13) . . ? C21D C20D C5D 109.8(12) . . ? C22D C20D C5D 107.6(12) . . ? C21D C20D H20D 110.3 . . ? C22D C20D H20D 110.3 . . ? C5D C20D H20D 110.3 . . ? C20D C21D H21J 109.5 . . ? C20D C21D H21K 109.5 . . ? H21J C21D H21K 109.5 . . ? C20D C21D H21L 109.5 . . ? H21J C21D H21L 109.5 . . ? H21K C21D H21L 109.5 . . ? C20D C22D H22J 109.5 . . ? C20D C22D H22K 109.5 . . ? H22J C22D H22K 109.5 . . ? C20D C22D H22L 109.5 . . ? H22J C22D H22L 109.5 . . ? H22K C22D H22L 109.5 . . ? N1D C24D C25D 114.4(10) . . ? N1D C24D C27D 110.2(10) . . ? C25D C24D C27D 109.7(9) . . ? N1D C24D H24D 107.4 . . ? C25D C24D H24D 107.4 . . ? C27D C24D H24D 107.4 . . ? O3D C25D O4D 125.1(10) . . ? O3D C25D C24D 119.8(10) . . ? O4D C25D C24D 114.6(9) . . ? C28D C27D C24D 112.2(9) . . ? C28D C27D H27G 109.2 . . ? C24D C27D H27G 109.2 . . ? C28D C27D H27H 109.2 . . ? C24D C27D H27H 109.2 . . ? H27G C27D H27H 107.9 . . ? C29D C28D C33D 118.0 . . ? C29D C28D C27D 121.9(8) . . ? C33D C28D C27D 120.0(8) . . ? C28D C29D C30D 120.7 . . ? C31D C30D C29D 121.2 . . ? C32D C31D C30D 118.1 . . ? C31D C32D C33D 120.9 . . ? C32D C33D C28D 121.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.203 _refine_diff_density_min -0.184 _refine_diff_density_rms 0.038 #===END