data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 D4 N8 O13' _chemical_formula_weight 718.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'D' 'D' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.871(2) _cell_length_b 10.724(4) _cell_length_c 21.829(7) _cell_angle_alpha 99.543(3) _cell_angle_beta 93.469(3) _cell_angle_gamma 105.766(5) _cell_volume 1517.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3300 _exptl_crystal_size_mid 0.2900 _exptl_crystal_size_min 0.2700 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 0.125 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7801 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11824 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6803 _reflns_number_gt 4788 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1201P)^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 ? _refine_ls_number_reflns 6803 _refine_ls_number_parameters 476 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1839 _refine_ls_wR_factor_gt 0.1671 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 C1 C 0.2363(3) 0.45529(19) 0.45507(9) 0.0163(4) Uani 1 1 d . . . H1A H 0.1534(3) 0.45470(19) 0.48894(9) 0.020 Uiso 1 1 d R . . H1B H 0.3495(3) 0.53359(19) 0.46498(9) 0.020 Uiso 1 1 d R . . C2 C 0.1332(3) 0.22016(19) 0.43255(10) 0.0174(4) Uani 1 1 d . . . H2A H 0.1808(3) 0.14322(19) 0.42842(10) 0.021 Uiso 1 1 d R . . H2B H 0.0497(3) 0.21855(19) 0.46628(10) 0.021 Uiso 1 1 d R . . C3 C 0.4345(3) 0.3423(2) 0.39486(10) 0.0178(4) Uani 1 1 d . . . H3A H 0.4864(3) 0.2671(2) 0.39007(10) 0.021 Uiso 1 1 d R . . H3B H 0.5485(3) 0.4202(2) 0.40399(10) 0.021 Uiso 1 1 d R . . C4 C 0.2461(3) 0.45669(19) 0.34266(9) 0.0175(4) Uani 1 1 d . . . H4A H 0.3601(3) 0.53460(19) 0.35153(9) 0.021 Uiso 1 1 d R . . H4B H 0.1698(3) 0.45721(19) 0.30442(9) 0.021 Uiso 1 1 d R . . C5 C 0.1418(3) 0.22163(19) 0.32308(10) 0.0179(4) Uani 1 1 d . . . H5A H 0.0631(3) 0.22012(19) 0.28496(10) 0.021 Uiso 1 1 d R . . H5B H 0.1901(3) 0.14492(19) 0.31739(10) 0.021 Uiso 1 1 d R . . C6 C -0.0640(3) 0.33114(19) 0.38130(10) 0.0171(4) Uani 1 1 d . . . H6A H -0.1489(3) 0.32984(19) 0.41468(10) 0.020 Uiso 1 1 d R . . H6B H -0.1447(3) 0.32945(19) 0.34353(10) 0.020 Uiso 1 1 d R . . C7 C 0.4881(3) 0.8307(2) -0.13993(10) 0.0195(4) Uani 1 1 d . . . H7A H 0.3877(3) 0.8446(2) -0.11292(10) 0.023 Uiso 1 1 d R . . H7B H 0.4327(3) 0.8233(2) -0.18226(10) 0.023 Uiso 1 1 d R . . C8 C 0.6924(3) 0.69242(19) -0.17471(10) 0.0201(4) Uani 1 1 d . . . H8A H 0.6384(3) 0.68556(19) -0.21713(10) 0.024 Uiso 1 1 d R . . H8B H 0.7228(3) 0.61137(19) -0.17142(10) 0.024 Uiso 1 1 d R . . C9 C 0.9599(3) 0.8139(2) -0.09420(10) 0.0200(4) Uani 1 1 d . . . H9A H 0.9952(3) 0.7352(2) -0.08934(10) 0.024 Uiso 1 1 d R . . H9B H 1.0813(3) 0.8867(2) -0.08372(10) 0.024 Uiso 1 1 d R . . C10 C 0.8353(3) 0.9231(2) -0.16653(10) 0.0199(4) Uani 1 1 d . . . H10A H 0.9572(3) 0.9956(2) -0.15646(10) 0.024 Uiso 1 1 d R . . H10B H 0.7837(3) 0.9172(2) -0.20910(10) 0.024 Uiso 1 1 d R . . C11 C 0.6227(3) 0.7232(2) -0.06789(10) 0.0196(4) Uani 1 1 d . . . H11A H 0.6526(3) 0.6429(2) -0.06285(10) 0.023 Uiso 1 1 d R . . H11B H 0.5239(3) 0.7368(2) -0.04019(10) 0.023 Uiso 1 1 d R . . C12 C 0.7616(3) 0.95528(19) -0.05672(10) 0.0184(4) Uani 1 1 d . . . H12A H 0.8817(3) 1.02885(19) -0.04509(10) 0.022 Uiso 1 1 d R . . H12B H 0.6622(3) 0.96851(19) -0.02921(10) 0.022 Uiso 1 1 d R . . C13 C 0.3388(2) 0.97027(16) -0.28509(8) 0.0079(3) Uani 1 1 d . . . C14 C 0.3461(3) 1.05672(18) -0.33137(9) 0.0154(4) Uani 1 1 d . . . C15 C 0.4888(3) 1.05761(18) -0.37347(9) 0.0164(4) Uani 1 1 d . . . H15A H 0.5809(3) 1.00454(18) -0.37313(9) 0.020 Uiso 1 1 d R . . C16 C 0.4900(3) 1.13982(18) -0.41610(9) 0.0149(4) Uani 1 1 d . . . C17 C 0.6409(2) 1.14360(16) -0.46191(8) 0.0081(3) Uani 1 1 d . . . C18 C 0.3585(3) 1.21594(18) -0.41839(9) 0.0148(4) Uani 1 1 d . . . H18A H 0.3645(3) 1.27081(18) -0.44920(9) 0.018 Uiso 1 1 d R . . C19 C 0.2168(3) 1.21217(18) -0.37523(9) 0.0145(4) Uani 1 1 d . . . C20 C 0.0727(3) 1.29708(18) -0.37615(9) 0.0154(4) Uani 1 1 d . . . C21 C 0.2105(3) 1.13192(19) -0.33074(9) 0.0160(4) Uani 1 1 d . . . H21A H 0.1146(3) 1.12884(19) -0.30042(9) 0.019 Uiso 1 1 d R . . C22 C 1.1104(3) 0.63130(18) 0.05324(9) 0.0122(4) Uani 1 1 d . . . C23 C 0.9531(3) 0.6446(2) 0.09510(10) 0.0195(4) Uani 1 1 d . . . C24 C 0.9293(3) 0.5723(2) 0.14226(10) 0.0205(4) Uani 1 1 d . . . H24A H 1.0103(3) 0.5141(2) 0.14791(10) 0.025 Uiso 1 1 d R . . C25 C 0.7823(3) 0.58852(19) 0.18098(10) 0.0190(4) Uani 1 1 d . . . C26 C 0.7546(3) 0.51568(18) 0.23260(9) 0.0136(4) Uani 1 1 d . . . C27 C 0.6606(3) 0.6701(2) 0.17300(10) 0.0187(4) Uani 1 1 d . . . H27A H 0.5584(3) 0.6776(2) 0.20033(10) 0.022 Uiso 1 1 d R . . C28 C 0.6895(3) 0.74085(19) 0.12452(9) 0.0162(4) Uani 1 1 d . . . C29 C 0.5654(3) 0.8351(2) 0.11483(10) 0.0179(4) Uani 1 1 d . . . C30 C 0.8377(3) 0.72784(19) 0.08502(10) 0.0164(4) Uani 1 1 d . . . H30A H 0.8591(3) 0.77593(19) 0.05145(10) 0.020 Uiso 1 1 d R . . N1 N 0.0103(2) 0.21633(16) 0.37429(8) 0.0166(4) Uani 1 1 d . . . N2 N 0.1128(2) 0.45625(16) 0.39547(8) 0.0150(4) Uani 1 1 d D . . N3 N 0.3097(2) 0.33984(16) 0.44759(8) 0.0160(4) Uani 1 1 d . . . N4 N 0.3171(2) 0.34084(16) 0.33592(8) 0.0169(4) Uani 1 1 d . . . N5 N 0.5368(3) 0.71040(16) -0.13273(8) 0.0194(4) Uani 1 1 d . . . N6 N 0.8102(2) 0.83446(17) -0.05090(8) 0.0177(4) Uani 1 1 d . . . N7 N 0.6789(3) 0.94704(17) -0.12368(8) 0.0175(4) Uani 1 1 d D . . N8 N 0.8815(3) 0.80203(17) -0.15966(8) 0.0191(4) Uani 1 1 d . . . O1 O 0.7390(2) 1.06355(14) -0.46499(7) 0.0232(3) Uani 1 1 d . . . O1W O 0.1948(3) 0.86294(16) 0.24912(8) 0.0290(4) Uani 1 1 d DU . . O2 O 0.6594(2) 1.22672(15) -0.49517(8) 0.0259(4) Uani 1 1 d . . . O3 O 0.0976(2) 1.37192(14) -0.41584(7) 0.0202(3) Uani 1 1 d . . . O4 O -0.0593(2) 1.28884(14) -0.33911(7) 0.0209(3) Uani 1 1 d . . . O5 O 0.2395(2) 0.98559(15) -0.24116(7) 0.0236(4) Uani 1 1 d . . . O6 O 0.4308(2) 0.88615(14) -0.29321(7) 0.0226(3) Uani 1 1 d . . . O7 O 1.1488(2) 0.70687(16) 0.01619(8) 0.0292(4) Uani 1 1 d . . . O8 O 1.1941(3) 0.54493(17) 0.05755(9) 0.0349(4) Uani 1 1 d . . . O9 O 0.8579(3) 0.43947(16) 0.23740(8) 0.0355(4) Uani 1 1 d . . . O10 O 0.6315(2) 0.53564(16) 0.26880(8) 0.0315(4) Uani 1 1 d . . . O11 O 0.4113(2) 0.82957(14) 0.14495(7) 0.0211(3) Uani 1 1 d . . . O12 O 0.6235(2) 0.91154(15) 0.07830(7) 0.0242(4) Uani 1 1 d . . . D1 D 0.265(5) 0.826(3) 0.2176(12) 0.085(12) Uiso 1 1 d D . . D2 D 0.157(6) 0.799(3) 0.2773(14) 0.105(15) Uiso 1 1 d D . . D3 D 0.054(3) 0.5293(19) 0.4013(11) 0.022(6) Uiso 1 1 d D . . D4 D 0.643(4) 1.025(2) -0.1268(12) 0.035(7) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0169(9) 0.0161(10) 0.0171(10) 0.0041(8) 0.0004(7) 0.0064(7) C2 0.0174(10) 0.0163(10) 0.0210(11) 0.0071(8) 0.0038(8) 0.0062(8) C3 0.0125(9) 0.0197(10) 0.0222(11) 0.0031(8) 0.0013(8) 0.0069(7) C4 0.0169(10) 0.0179(10) 0.0190(11) 0.0089(8) 0.0037(8) 0.0036(7) C5 0.0169(10) 0.0170(10) 0.0190(11) 0.0021(8) 0.0018(8) 0.0046(8) C6 0.0097(9) 0.0188(10) 0.0233(11) 0.0058(8) 0.0009(7) 0.0042(7) C7 0.0139(9) 0.0210(10) 0.0245(11) 0.0072(8) -0.0016(8) 0.0055(8) C8 0.0229(11) 0.0162(10) 0.0210(11) 0.0019(8) 0.0019(8) 0.0066(8) C9 0.0153(10) 0.0235(11) 0.0238(11) 0.0052(8) 0.0015(8) 0.0095(8) C10 0.0239(10) 0.0180(10) 0.0196(11) 0.0070(8) 0.0067(8) 0.0061(8) C11 0.0191(10) 0.0208(10) 0.0203(11) 0.0082(8) 0.0040(8) 0.0054(8) C12 0.0193(10) 0.0182(10) 0.0178(11) 0.0033(8) 0.0010(8) 0.0059(8) C13 0.0065(8) 0.0066(8) 0.0106(9) 0.0037(6) -0.0029(6) 0.0015(6) C14 0.0150(9) 0.0128(9) 0.0176(10) 0.0058(8) -0.0016(7) 0.0015(7) C15 0.0134(9) 0.0143(9) 0.0219(11) 0.0045(8) -0.0016(8) 0.0046(7) C16 0.0116(9) 0.0154(9) 0.0173(10) 0.0029(8) 0.0026(7) 0.0031(7) C17 0.0045(8) 0.0091(8) 0.0120(9) 0.0038(7) 0.0003(6) 0.0029(6) C18 0.0136(9) 0.0126(9) 0.0178(10) 0.0057(7) -0.0008(7) 0.0018(7) C19 0.0132(9) 0.0129(9) 0.0173(10) 0.0033(7) 0.0004(7) 0.0036(7) C20 0.0143(9) 0.0126(9) 0.0189(10) 0.0031(7) -0.0011(7) 0.0040(7) C21 0.0144(9) 0.0158(9) 0.0177(10) 0.0048(8) 0.0016(7) 0.0033(7) C22 0.0092(8) 0.0130(9) 0.0150(10) -0.0002(7) -0.0018(7) 0.0065(7) C23 0.0166(10) 0.0171(10) 0.0226(11) -0.0007(8) -0.0002(8) 0.0045(8) C24 0.0187(10) 0.0157(10) 0.0254(12) 0.0024(8) -0.0050(8) 0.0048(8) C25 0.0188(10) 0.0148(10) 0.0210(11) 0.0070(8) -0.0045(8) 0.0004(7) C26 0.0129(9) 0.0106(9) 0.0152(10) 0.0066(7) -0.0073(7) -0.0009(7) C27 0.0163(10) 0.0184(10) 0.0194(11) 0.0040(8) 0.0003(8) 0.0016(7) C28 0.0143(9) 0.0137(9) 0.0194(11) 0.0018(8) -0.0010(8) 0.0033(7) C29 0.0161(9) 0.0181(10) 0.0193(11) 0.0021(8) 0.0003(8) 0.0056(7) C30 0.0164(9) 0.0146(9) 0.0177(10) 0.0047(8) -0.0005(8) 0.0031(7) N1 0.0147(8) 0.0150(8) 0.0196(9) 0.0038(7) 0.0015(7) 0.0031(6) N2 0.0126(8) 0.0151(8) 0.0196(9) 0.0053(7) 0.0018(6) 0.0066(6) N3 0.0128(8) 0.0168(8) 0.0199(9) 0.0048(7) 0.0007(6) 0.0064(6) N4 0.0143(8) 0.0174(8) 0.0200(9) 0.0050(7) 0.0034(6) 0.0051(6) N5 0.0183(9) 0.0172(9) 0.0225(10) 0.0063(7) 0.0009(7) 0.0034(7) N6 0.0159(8) 0.0192(9) 0.0200(9) 0.0058(7) 0.0018(7) 0.0070(7) N7 0.0182(8) 0.0174(9) 0.0202(9) 0.0065(7) 0.0025(7) 0.0085(7) N8 0.0200(9) 0.0184(9) 0.0212(10) 0.0042(7) 0.0055(7) 0.0080(7) O1 0.0231(8) 0.0206(8) 0.0300(9) 0.0062(6) 0.0064(6) 0.0117(6) O1W 0.0334(9) 0.0282(9) 0.0301(10) 0.0131(7) 0.0097(7) 0.0110(7) O2 0.0246(8) 0.0292(9) 0.0326(9) 0.0172(7) 0.0126(7) 0.0134(7) O3 0.0230(8) 0.0216(8) 0.0234(8) 0.0115(6) 0.0067(6) 0.0137(6) O4 0.0179(7) 0.0233(8) 0.0258(9) 0.0103(6) 0.0074(6) 0.0086(6) O5 0.0280(8) 0.0244(8) 0.0206(8) 0.0095(6) 0.0025(6) 0.0080(6) O6 0.0216(8) 0.0194(8) 0.0294(9) 0.0093(6) -0.0004(6) 0.0083(6) O7 0.0231(8) 0.0410(10) 0.0278(9) 0.0076(8) 0.0051(7) 0.0150(7) O8 0.0307(9) 0.0292(9) 0.0488(12) 0.0018(8) 0.0033(8) 0.0186(7) O9 0.0400(10) 0.0277(9) 0.0383(11) 0.0142(8) -0.0097(8) 0.0073(7) O10 0.0304(9) 0.0290(9) 0.0290(10) 0.0119(7) -0.0038(7) -0.0038(7) O11 0.0177(7) 0.0234(8) 0.0257(9) 0.0065(6) 0.0063(6) 0.0099(6) O12 0.0282(8) 0.0230(8) 0.0292(9) 0.0128(7) 0.0100(7) 0.0141(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 C1 H1A 0.9599 . ? C1 H1B 0.9600 . ? C1 N3 1.448(2) . ? C1 N2 1.513(2) . ? C2 H2A 0.9599 . ? C2 H2B 0.9601 . ? C2 N1 1.472(3) . ? C2 N3 1.480(2) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 N4 1.472(3) . ? C3 N3 1.476(3) . ? C4 H4A 0.9600 . ? C4 H4B 0.9601 . ? C4 N4 1.442(2) . ? C4 N2 1.515(2) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 N4 1.472(2) . ? C5 N1 1.478(3) . ? C6 H6A 0.9599 . ? C6 H6B 0.9600 . ? C6 N1 1.445(2) . ? C6 N2 1.517(2) . ? C7 H7A 0.9601 . ? C7 H7B 0.9601 . ? C7 N5 1.448(2) . ? C7 N7 1.519(3) . ? C8 H8B 0.9600 . ? C8 H8A 0.9600 . ? C8 N8 1.472(3) . ? C8 N5 1.481(3) . ? C9 H9B 0.9600 . ? C9 H9A 0.9601 . ? C9 N8 1.469(3) . ? C9 N6 1.474(3) . ? C10 H10A 0.9600 . ? C10 H10B 0.9601 . ? C10 N8 1.446(2) . ? C10 N7 1.513(3) . ? C11 H11B 0.9600 . ? C11 H11A 0.9600 . ? C11 N5 1.470(3) . ? C11 N6 1.477(3) . ? C12 H12A 0.9600 . ? C12 H12B 0.9601 . ? C12 N6 1.446(2) . ? C12 N7 1.516(3) . ? C13 O5 1.225(2) . ? C13 O6 1.231(2) . ? C13 C14 1.474(3) . ? C14 C15 1.383(3) . ? C14 C21 1.388(3) . ? C15 H15A 0.9600 . ? C15 C16 1.383(3) . ? C16 C18 1.376(3) . ? C16 C17 1.481(2) . ? C17 O1 1.223(2) . ? C17 O2 1.226(2) . ? C18 H18A 0.9601 . ? C18 C19 1.393(3) . ? C19 C21 1.396(3) . ? C19 C20 1.518(2) . ? C20 O4 1.247(2) . ? C20 O3 1.264(2) . ? C21 H21A 0.9600 . ? C22 O7 1.228(2) . ? C22 O8 1.229(2) . ? C22 C23 1.478(3) . ? C23 C24 1.379(3) . ? C23 C30 1.380(3) . ? C24 H24A 0.9600 . ? C24 C25 1.384(3) . ? C25 C27 1.387(3) . ? C25 C26 1.467(3) . ? C26 O10 1.228(3) . ? C26 O9 1.232(2) . ? C27 H27A 0.9600 . ? C27 C28 1.395(3) . ? C28 C30 1.394(3) . ? C28 C29 1.520(3) . ? C29 O12 1.243(2) . ? C29 O11 1.273(2) . ? C30 H30A 0.9601 . ? N2 D3 0.970(15) . ? N7 D4 0.945(16) . ? O1W D1 0.960(17) . ? O1W D2 0.988(17) . ? 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 H1A C1 H1B 108.2 . . ? H1A C1 N3 109.65(10) . . ? H1B C1 N3 109.66(10) . . ? H1A C1 N2 109.64(10) . . ? H1B C1 N2 109.65(10) . . ? N3 C1 N2 110.05(15) . . ? H2A C2 H2B 108.0 . . ? H2A C2 N1 109.31(10) . . ? H2B C2 N1 109.29(10) . . ? H2A C2 N3 109.31(10) . . ? H2B C2 N3 109.26(10) . . ? N1 C2 N3 111.63(15) . . ? H3A C3 H3B 107.9 . . ? H3A C3 N4 109.23(10) . . ? H3B C3 N4 109.23(10) . . ? H3A C3 N3 109.25(10) . . ? H3B C3 N3 109.24(10) . . ? N4 C3 N3 111.90(15) . . ? H4A C4 H4B 108.2 . . ? H4A C4 N4 109.82(10) . . ? H4B C4 N4 109.81(11) . . ? H4A C4 N2 109.80(10) . . ? H4B C4 N2 109.80(10) . . ? N4 C4 N2 109.34(14) . . ? H5A C5 H5B 107.9 . . ? H5A C5 N4 109.22(10) . . ? H5B C5 N4 109.22(10) . . ? H5A C5 N1 109.20(10) . . ? H5B C5 N1 109.20(10) . . ? N4 C5 N1 112.01(16) . . ? H6A C6 H6B 108.1 . . ? H6A C6 N1 109.58(10) . . ? H6B C6 N1 109.62(11) . . ? H6A C6 N2 109.59(10) . . ? H6B C6 N2 109.62(10) . . ? N1 C6 N2 110.27(15) . . ? H7A C7 H7B 108.2 . . ? H7A C7 N5 109.68(11) . . ? H7B C7 N5 109.72(11) . . ? H7A C7 N7 109.70(11) . . ? H7B C7 N7 109.72(10) . . ? N5 C7 N7 109.81(15) . . ? H8B C8 H8A 107.9 . . ? H8B C8 N8 109.15(10) . . ? H8A C8 N8 109.15(11) . . ? H8B C8 N5 109.11(10) . . ? H8A C8 N5 109.16(11) . . ? N8 C8 N5 112.31(16) . . ? H9B C9 H9A 107.9 . . ? H9B C9 N8 109.20(11) . . ? H9A C9 N8 109.17(10) . . ? H9B C9 N6 109.23(11) . . ? H9A C9 N6 109.18(10) . . ? N8 C9 N6 112.08(15) . . ? H10A C10 H10B 108.2 . . ? H10A C10 N8 109.68(11) . . ? H10B C10 N8 109.65(11) . . ? H10A C10 N7 109.66(11) . . ? H10B C10 N7 109.65(11) . . ? N8 C10 N7 110.02(15) . . ? H11B C11 H11A 108.0 . . ? H11B C11 N5 109.29(10) . . ? H11A C11 N5 109.33(10) . . ? H11B C11 N6 109.29(11) . . ? H11A C11 N6 109.33(10) . . ? N5 C11 N6 111.57(16) . . ? H12A C12 H12B 108.2 . . ? H12A C12 N6 109.78(11) . . ? H12B C12 N6 109.78(10) . . ? H12A C12 N7 109.74(10) . . ? H12B C12 N7 109.79(10) . . ? N6 C12 N7 109.50(16) . . ? O5 C13 O6 123.90(17) . . ? O5 C13 C14 117.91(16) . . ? O6 C13 C14 118.18(17) . . ? C15 C14 C21 123.54(18) . . ? C15 C14 C13 117.62(17) . . ? C21 C14 C13 118.83(17) . . ? H15A C15 C14 122.14(11) . . ? H15A C15 C16 122.16(11) . . ? C14 C15 C16 115.70(17) . . ? C18 C16 C15 123.66(18) . . ? C18 C16 C17 119.06(17) . . ? C15 C16 C17 117.27(16) . . ? O1 C17 O2 123.51(17) . . ? O1 C17 C16 118.67(16) . . ? O2 C17 C16 117.82(16) . . ? H18A C18 C16 120.54(11) . . ? H18A C18 C19 120.54(11) . . ? C16 C18 C19 118.91(18) . . ? C18 C19 C21 119.75(17) . . ? C18 C19 C20 119.82(17) . . ? C21 C19 C20 120.41(17) . . ? O4 C20 O3 124.87(17) . . ? O4 C20 C19 119.35(17) . . ? O3 C20 C19 115.78(17) . . ? H21A C21 C14 120.80(12) . . ? H21A C21 C19 120.78(11) . . ? C14 C21 C19 118.42(18) . . ? O7 C22 O8 124.06(19) . . ? O7 C22 C23 118.03(17) . . ? O8 C22 C23 117.91(18) . . ? C24 C23 C30 123.46(19) . . ? C24 C23 C22 117.94(18) . . ? C30 C23 C22 118.60(18) . . ? H24A C24 C23 121.85(12) . . ? H24A C24 C25 121.84(12) . . ? C23 C24 C25 116.31(18) . . ? C24 C25 C27 122.91(19) . . ? C24 C25 C26 118.20(18) . . ? C27 C25 C26 118.89(19) . . ? O10 C26 O9 124.02(19) . . ? O10 C26 C25 117.97(17) . . ? O9 C26 C25 118.01(19) . . ? H27A C27 C25 120.60(12) . . ? H27A C27 C28 120.61(12) . . ? C25 C27 C28 118.79(19) . . ? C30 C28 C27 119.77(18) . . ? C30 C28 C29 119.11(17) . . ? C27 C28 C29 121.10(18) . . ? O12 C29 O11 125.47(18) . . ? O12 C29 C28 117.17(18) . . ? O11 C29 C28 117.36(17) . . ? H30A C30 C23 120.62(12) . . ? H30A C30 C28 120.64(11) . . ? C23 C30 C28 118.75(18) . . ? C6 N1 C2 108.98(16) . . ? C6 N1 C5 108.37(15) . . ? C2 N1 C5 108.67(15) . . ? C1 N2 C4 108.76(14) . . ? C1 N2 C6 108.10(15) . . ? C4 N2 C6 109.06(15) . . ? C1 N2 D3 110.5(14) . . ? C4 N2 D3 113.9(13) . . ? C6 N2 D3 106.4(14) . . ? C1 N3 C3 108.58(15) . . ? C1 N3 C2 108.92(15) . . ? C3 N3 C2 108.66(16) . . ? C4 N4 C3 108.96(16) . . ? C4 N4 C5 109.65(15) . . ? C3 N4 C5 108.45(15) . . ? C7 N5 C11 109.25(16) . . ? C7 N5 C8 108.27(15) . . ? C11 N5 C8 108.60(16) . . ? C12 N6 C9 109.26(15) . . ? C12 N6 C11 108.75(15) . . ? C9 N6 C11 108.96(16) . . ? C10 N7 C12 109.13(15) . . ? C10 N7 C7 108.87(16) . . ? C12 N7 C7 108.07(15) . . ? C10 N7 D4 113.2(16) . . ? C12 N7 D4 109.0(16) . . ? C7 N7 D4 108.4(16) . . ? C10 N8 C9 108.40(16) . . ? C10 N8 C8 108.76(15) . . ? C9 N8 C8 108.72(16) . . ? D1 O1W D2 107(2) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.829 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.094