#------------------------------------------------------------------------------ #$Date: 2016-02-21 00:03:34 +0000 (Sun, 21 Feb 2016) $ #$Revision: 176798 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/90/2239064.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2239064 loop_ _publ_author_name 'Novosjolova, Irina' 'Stepanovs, Dmitrijs' 'Bizd\=ena, \=Erika' 'Mishnev, Anatoly' 'Turks, M\=aris' _publ_section_title ; 2,6-Dichloro-9-(2',3',5'-tri-O-acetyl-\b-D-ribofuranosyl)-9H-purine ; _journal_coeditor_code LD2116 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o108 _journal_page_last o109 _journal_paper_doi 10.1107/S1600536813034521 _journal_volume 70 _journal_year 2014 _chemical_formula_iupac 'C16 H16 Cl2 N4 O7' _chemical_formula_moiety 'C16 H16 Cl2 N4 O7' _chemical_formula_sum 'C16 H16 Cl2 N4 O7' _chemical_formula_weight 447.23 _chemical_name_systematic 2,6-Dichloro-9-(2',3',5'-tri-O-acetyl-\b-D-ribofuranosyl)-9H-purine _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 106.537(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 10.1324(2) _cell_length_b 9.6887(3) _cell_length_c 10.5399(2) _cell_measurement_reflns_used 17407 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.485 _cell_measurement_theta_min 0.998 _cell_volume 991.90(4) _computing_cell_refinement 'SCALEPACK (Otwinovski & Minor, 1997)' _computing_data_collection 'KappaCCD Server Software (Nonius, 1997)' _computing_data_reduction 'DENZO and SCALEPACK (Otwinovski & Minor, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae et al., 2008)' _computing_publication_material ; SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and publCIF (Westrip, 2010) ; _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method CCD _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 3898 _diffrn_reflns_theta_full 27.46 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_min 2.02 _exptl_absorpt_coefficient_mu 0.374 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 460 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.223 _refine_diff_density_min -0.195 _refine_ls_abs_structure_details 'Flack (1983), 1518 Friedel pairs' _refine_ls_abs_structure_Flack 0.00(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 265 _refine_ls_number_reflns 3898 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0461 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.3514P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0942 _refine_ls_wR_factor_ref 0.1070 _reflns_number_gt 2846 _reflns_number_total 3898 _reflns_threshold_expression I>2sigma(I) _iucr_refine_instructions_details ; TITL test structure: IrN-313 CELL 0.71073 10.1324 9.6887 10.5399 90.000 106.537 90.000 ZERR 2.00 0.0002 0.0003 0.0002 0.000 0.002 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O CL UNIT 32 32 8 14 4 MERG 2 OMIT 1 0 0 OMIT -1 -1 1 OMIT -1 1 1 OMIT 1 -1 0 OMIT 1 1 0 OMIT -1 0 1 OMIT 0 1 1 FMAP 2 PLAN -20 SIZE 0.15 0.32 0.38 ACTA BOND $H CONF L.S. 12 WGHT 0.035100 0.353200 FVAR 1.00343 N1 3 1.084971 0.113861 0.478539 11.00000 0.06302 0.05455 = 0.04978 -0.00497 0.02696 0.00152 C2 1 0.964970 0.178746 0.460212 11.00000 0.06435 0.05220 = 0.03760 -0.00283 0.01730 -0.00827 N3 3 0.917788 0.255297 0.539859 11.00000 0.05509 0.04372 = 0.04445 0.00228 0.02386 0.00097 C4 1 1.016974 0.270363 0.657404 11.00000 0.05114 0.03778 = 0.03620 0.00515 0.01890 -0.00141 C5 1 1.147662 0.213487 0.691488 11.00000 0.04513 0.04563 = 0.04056 0.00399 0.01660 0.00162 C6 1 1.176086 0.130948 0.595154 11.00000 0.05695 0.05002 = 0.05329 -0.00004 0.02749 0.00526 N7 3 1.221075 0.250821 0.819552 11.00000 0.04651 0.05524 = 0.04950 -0.00087 0.01256 0.00141 C8 1 1.133071 0.326565 0.859605 11.00000 0.05044 0.04815 = 0.04373 -0.00119 0.01430 -0.00147 AFIX 43 H8 2 1.154028 0.367072 0.942967 11.00000 -1.20000 AFIX 0 N9 3 1.007071 0.340448 0.766897 11.00000 0.04503 0.04255 = 0.03634 0.00161 0.01536 0.00327 CL10 5 1.329583 0.045481 0.623120 11.00000 0.07122 0.10992 = 0.09067 -0.01556 0.02989 0.03243 CL11 5 0.850379 0.155486 0.303785 11.00000 0.08241 0.09028 = 0.04335 -0.01394 0.01184 -0.00457 C1' 1 0.887651 0.420522 0.776944 11.00000 0.05008 0.04204 = 0.03191 0.00395 0.01374 0.01004 AFIX 13 H1 2 0.857394 0.482651 0.700797 11.00000 -1.20000 AFIX 0 C2' 1 0.769507 0.328151 0.784450 11.00000 0.04133 0.04060 = 0.03636 -0.00491 0.00961 0.00432 AFIX 13 H2 2 0.764163 0.242056 0.734433 11.00000 -1.20000 AFIX 0 C3' 1 0.803428 0.306243 0.934286 11.00000 0.03828 0.04190 = 0.03661 -0.00133 0.01297 0.00324 AFIX 13 H3 2 0.877156 0.237960 0.963883 11.00000 -1.20000 AFIX 0 C4' 1 0.853668 0.447237 0.986216 11.00000 0.04050 0.03969 = 0.03573 -0.00427 0.01294 0.00539 AFIX 13 H4 2 0.773301 0.506342 0.978646 11.00000 -1.20000 AFIX 0 C5' 1 0.945536 0.457036 1.125081 11.00000 0.04916 0.04361 = 0.03642 -0.00547 0.01157 0.00297 AFIX 23 H5A 2 0.978777 0.550877 1.143675 11.00000 -1.20000 H5B 2 0.894581 0.432535 1.187016 11.00000 -1.20000 AFIX 0 O6' 4 0.926372 0.498151 0.894862 11.00000 0.04933 0.03669 = 0.03708 -0.00351 0.01618 -0.00126 O7' 4 0.646031 0.408144 0.745761 11.00000 0.04256 0.05966 = 0.03804 -0.01041 0.00055 0.01325 C8' 1 0.547885 0.372788 0.633674 11.00000 0.04449 0.06037 = 0.04512 -0.00377 0.00280 -0.00444 C9' 1 0.429734 0.470365 0.609575 11.00000 0.04682 0.08436 = 0.06510 -0.00610 -0.00439 0.01070 AFIX 137 H9A 2 0.461590 0.562688 0.603071 11.00000 -1.50000 H9C 2 0.389452 0.465087 0.681585 11.00000 -1.50000 H9B 2 0.362005 0.446211 0.528535 11.00000 -1.50000 AFIX 0 O10' 4 0.563587 0.280864 0.564895 11.00000 0.07939 0.09627 = 0.08873 -0.04819 -0.01737 0.00980 O11' 4 0.688286 0.270122 0.980369 11.00000 0.03822 0.05310 = 0.04921 0.00044 0.01742 -0.00089 C12' 1 0.647362 0.136970 0.963610 11.00000 0.04367 0.05401 = 0.04843 0.01482 0.00503 -0.00013 C13' 1 0.528612 0.109842 1.018946 11.00000 0.05347 0.10866 = 0.08653 0.02717 0.02153 -0.01575 AFIX 137 H13A 2 0.518797 0.012191 1.028770 11.00000 -1.50000 H13B 2 0.445647 0.146201 0.959733 11.00000 -1.50000 H13C 2 0.545501 0.153797 1.103700 11.00000 -1.50000 AFIX 0 O14' 4 0.701220 0.054413 0.911040 11.00000 0.07615 0.05040 = 0.11188 0.00043 0.03636 -0.00122 O15' 4 1.059888 0.364362 1.139944 11.00000 0.04547 0.04694 = 0.03563 -0.00403 0.00490 0.00332 C16' 1 1.155062 0.367656 1.259490 11.00000 0.05135 0.04835 = 0.04006 -0.00438 -0.00289 -0.00358 C17' 1 1.274594 0.279442 1.262772 11.00000 0.05609 0.06240 = 0.05731 0.00298 0.00060 0.00624 AFIX 137 H17A 2 1.356967 0.334182 1.286468 11.00000 -1.50000 H17B 2 1.263000 0.239257 1.177033 11.00000 -1.50000 H17C 2 1.281630 0.207461 1.326953 11.00000 -1.50000 AFIX 0 O18' 4 1.138456 0.436970 1.347822 11.00000 0.08655 0.11990 = 0.04817 -0.03457 -0.01009 0.02586 HKLF 4 REM test structure: IrN-313 REM R1 = 0.0461 for 2846 Fo > 4sig(Fo) and 0.0754 for all 3898 data REM 265 parameters refined using 1 restraints END WGHT 0.0351 0.3532 REM Highest difference peak 0.223, deepest hole -0.195, 1-sigma level 0.040 Q1 1 1.3407 -0.0220 0.5534 11.00000 0.05 0.22 Q2 1 0.5063 0.2734 0.6242 11.00000 0.05 0.19 Q3 1 0.7920 0.3119 0.8799 11.00000 0.05 0.17 Q4 1 1.1013 0.3652 1.1774 11.00000 0.05 0.15 Q5 1 1.3280 0.3107 1.1610 11.00000 0.05 0.15 Q6 1 0.8457 0.2234 0.4707 11.00000 0.05 0.15 Q7 1 1.1823 0.5013 1.3129 11.00000 0.05 0.15 Q8 1 0.4945 0.2722 1.0989 11.00000 0.05 0.14 Q9 1 0.7718 0.6561 0.9963 11.00000 0.05 0.14 Q10 1 0.6827 0.0849 0.9976 11.00000 0.05 0.14 ; _cod_data_source_file ld2116sup1.cf _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 2239064 _cod_database_fobs_code 2239064 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity N N1 1.0850(3) 0.1139(3) 0.4785(3) 0.0535(8) Uani d . 1 1 C C2 0.9650(4) 0.1787(4) 0.4602(3) 0.0508(9) Uani d . 1 1 N N3 0.9178(3) 0.2553(3) 0.5399(2) 0.0458(6) Uani d . 1 1 C C4 1.0170(3) 0.2704(3) 0.6574(3) 0.0404(7) Uani d . 1 1 C C5 1.1477(3) 0.2135(4) 0.6915(3) 0.0429(8) Uani d . 1 1 C C6 1.1761(4) 0.1309(4) 0.5952(3) 0.0510(9) Uani d . 1 1 N N7 1.2211(3) 0.2508(3) 0.8196(3) 0.0506(7) Uani d . 1 1 C C8 1.1331(3) 0.3266(4) 0.8596(3) 0.0473(8) Uani d . 1 1 H H8 1.1540 0.3671 0.9430 0.057 Uiso calc R 1 1 N N9 1.0071(2) 0.3404(3) 0.7669(2) 0.0405(6) Uani d . 1 1 Cl Cl10 1.32958(12) 0.04548(15) 0.62312(11) 0.0892(4) Uani d . 1 1 Cl Cl11 0.85038(11) 0.15549(12) 0.30379(9) 0.0733(3) Uani d . 1 1 C C1' 0.8877(3) 0.4205(4) 0.7769(3) 0.0409(7) Uani d . 1 1 H H1 0.8574 0.4827 0.7008 0.049 Uiso calc R 1 1 C C2' 0.7695(3) 0.3282(4) 0.7845(3) 0.0397(7) Uani d . 1 1 H H2 0.7642 0.2421 0.7344 0.048 Uiso calc R 1 1 C C3' 0.8034(3) 0.3062(3) 0.9343(3) 0.0385(7) Uani d . 1 1 H H3 0.8772 0.2380 0.9639 0.046 Uiso calc R 1 1 C C4' 0.8537(3) 0.4472(3) 0.9862(3) 0.0382(7) Uani d . 1 1 H H4 0.7733 0.5063 0.9786 0.046 Uiso calc R 1 1 C C5' 0.9455(3) 0.4570(4) 1.1251(3) 0.0432(8) Uani d . 1 1 H H5A 0.9788 0.5509 1.1437 0.052 Uiso calc R 1 1 H H5B 0.8946 0.4325 1.1870 0.052 Uiso calc R 1 1 O O6' 0.9264(2) 0.4982(2) 0.89486(18) 0.0402(5) Uani d . 1 1 O O7' 0.6460(2) 0.4081(2) 0.74576(19) 0.0490(6) Uani d . 1 1 C C8' 0.5479(3) 0.3728(4) 0.6337(3) 0.0520(9) Uani d . 1 1 C C9' 0.4297(4) 0.4704(5) 0.6096(4) 0.0696(12) Uani d . 1 1 H H9A 0.4616 0.5627 0.6031 0.104 Uiso calc R 1 1 H H9C 0.3895 0.4651 0.6816 0.104 Uiso calc R 1 1 H H9B 0.3620 0.4462 0.5285 0.104 Uiso calc R 1 1 O O10' 0.5636(3) 0.2809(4) 0.5649(3) 0.0967(11) Uani d . 1 1 O O11' 0.6883(2) 0.2701(2) 0.9804(2) 0.0458(6) Uani d . 1 1 C C12' 0.6474(4) 0.1370(4) 0.9636(3) 0.0504(9) Uani d . 1 1 C C13' 0.5286(4) 0.1098(5) 1.0189(5) 0.0826(15) Uani d . 1 1 H H13A 0.5188 0.0122 1.0288 0.124 Uiso calc R 1 1 H H13B 0.4456 0.1462 0.9597 0.124 Uiso calc R 1 1 H H13C 0.5455 0.1538 1.1037 0.124 Uiso calc R 1 1 O O14' 0.7012(3) 0.0544(3) 0.9110(3) 0.0775(8) Uani d . 1 1 O O15' 1.0599(2) 0.3644(2) 1.13994(18) 0.0441(5) Uani d . 1 1 C C16' 1.1551(3) 0.3677(4) 1.2595(3) 0.0499(8) Uani d . 1 1 C C17' 1.2746(4) 0.2794(4) 1.2628(3) 0.0618(10) Uani d . 1 1 H H17A 1.3570 0.3342 1.2865 0.093 Uiso calc R 1 1 H H17B 1.2630 0.2393 1.1770 0.093 Uiso calc R 1 1 H H17C 1.2816 0.2075 1.3270 0.093 Uiso calc R 1 1 O O18' 1.1385(3) 0.4370(4) 1.3478(2) 0.0909(10) Uani d . 1 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N1 0.063(2) 0.055(2) 0.0498(17) 0.0015(15) 0.0270(14) -0.0050(14) C2 0.064(2) 0.052(2) 0.0376(17) -0.0083(19) 0.0173(14) -0.0028(16) N3 0.0551(17) 0.0437(17) 0.0444(15) 0.0010(13) 0.0239(12) 0.0023(13) C4 0.0511(19) 0.0378(19) 0.0362(16) -0.0014(15) 0.0189(13) 0.0051(14) C5 0.0451(19) 0.046(2) 0.0406(16) 0.0016(15) 0.0166(13) 0.0040(15) C6 0.057(2) 0.050(2) 0.0533(19) 0.0053(17) 0.0275(16) 0.0000(17) N7 0.0465(16) 0.0552(19) 0.0495(15) 0.0014(14) 0.0126(12) -0.0009(14) C8 0.050(2) 0.048(2) 0.0437(17) -0.0015(16) 0.0143(14) -0.0012(15) N9 0.0450(15) 0.0425(16) 0.0363(13) 0.0033(12) 0.0154(11) 0.0016(12) Cl10 0.0712(7) 0.1099(11) 0.0907(7) 0.0324(7) 0.0299(6) -0.0156(7) Cl11 0.0824(7) 0.0903(9) 0.0433(5) -0.0046(6) 0.0118(4) -0.0139(5) C1' 0.0501(18) 0.0420(19) 0.0319(14) 0.0100(15) 0.0137(12) 0.0040(14) C2' 0.0413(17) 0.0406(19) 0.0364(15) 0.0043(14) 0.0096(12) -0.0049(14) C3' 0.0383(16) 0.0419(19) 0.0366(15) 0.0032(14) 0.0130(12) -0.0013(14) C4' 0.0405(16) 0.0397(19) 0.0357(14) 0.0054(14) 0.0129(12) -0.0043(14) C5' 0.0492(18) 0.044(2) 0.0364(15) 0.0030(15) 0.0116(13) -0.0055(14) O6' 0.0493(12) 0.0367(13) 0.0371(11) -0.0013(10) 0.0162(9) -0.0035(9) O7' 0.0426(12) 0.0597(17) 0.0380(11) 0.0133(11) 0.0005(9) -0.0104(10) C8' 0.044(2) 0.060(3) 0.0451(18) -0.0044(17) 0.0028(14) -0.0038(18) C9' 0.047(2) 0.084(3) 0.065(2) 0.011(2) -0.0044(16) -0.006(2) O10' 0.079(2) 0.096(3) 0.089(2) 0.0098(18) -0.0174(16) -0.048(2) O11' 0.0382(12) 0.0531(16) 0.0492(12) -0.0009(11) 0.0174(9) 0.0004(11) C12' 0.044(2) 0.054(2) 0.0484(18) -0.0001(18) 0.0050(14) 0.0148(18) C13' 0.053(3) 0.109(4) 0.087(3) -0.016(2) 0.022(2) 0.027(3) O14' 0.0762(19) 0.0504(18) 0.112(2) -0.0012(16) 0.0364(17) 0.0004(17) O15' 0.0455(12) 0.0469(14) 0.0356(10) 0.0033(10) 0.0049(9) -0.0040(10) C16' 0.051(2) 0.048(2) 0.0401(18) -0.0036(17) -0.0029(14) -0.0044(17) C17' 0.056(2) 0.062(3) 0.057(2) 0.006(2) 0.0006(16) 0.0030(19) O18' 0.087(2) 0.120(3) 0.0482(14) 0.026(2) -0.0101(13) -0.0346(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C6 N1 C2 116.3(3) N3 C2 N1 131.2(3) N3 C2 Cl11 114.5(3) N1 C2 Cl11 114.3(2) C2 N3 C4 109.5(3) N3 C4 N9 127.5(3) N3 C4 C5 126.6(3) N9 C4 C5 105.9(3) C4 C5 C6 115.0(3) C4 C5 N7 110.9(3) C6 C5 N7 134.1(3) N1 C6 C5 121.2(3) N1 C6 Cl10 117.4(2) C5 C6 Cl10 121.4(3) C8 N7 C5 103.5(3) N7 C8 N9 113.8(3) N7 C8 H8 123.1 N9 C8 H8 123.1 C4 N9 C8 105.9(3) C4 N9 C1' 125.7(2) C8 N9 C1' 128.2(3) O6' C1' N9 108.5(2) O6' C1' C2' 107.2(2) N9 C1' C2' 111.8(3) O6' C1' H1 109.8 N9 C1' H1 109.8 C2' C1' H1 109.8 O7' C2' C1' 107.8(3) O7' C2' C3' 106.9(2) C1' C2' C3' 100.8(2) O7' C2' H2 113.5 C1' C2' H2 113.5 C3' C2' H2 113.5 O11' C3' C4' 108.8(2) O11' C3' C2' 114.8(2) C4' C3' C2' 101.7(2) O11' C3' H3 110.4 C4' C3' H3 110.4 C2' C3' H3 110.4 O6' C4' C5' 109.5(2) O6' C4' C3' 104.5(2) C5' C4' C3' 117.7(3) O6' C4' H4 108.3 C5' C4' H4 108.3 C3' C4' H4 108.3 O15' C5' C4' 108.9(2) O15' C5' H5A 109.9 C4' C5' H5A 109.9 O15' C5' H5B 109.9 C4' C5' H5B 109.9 H5A C5' H5B 108.3 C1' O6' C4' 109.7(2) C8' O7' C2' 118.5(3) O10' C8' O7' 122.0(3) O10' C8' C9' 127.8(3) O7' C8' C9' 110.1(3) C8' C9' H9A 109.5 C8' C9' H9C 109.5 H9A C9' H9C 109.5 C8' C9' H9B 109.5 H9A C9' H9B 109.5 H9C C9' H9B 109.5 C12' O11' C3' 116.1(3) O14' C12' O11' 122.6(3) O14' C12' C13' 126.0(4) O11' C12' C13' 111.5(4) C12' C13' H13A 109.5 C12' C13' H13B 109.5 H13A C13' H13B 109.5 C12' C13' H13C 109.5 H13A C13' H13C 109.5 H13B C13' H13C 109.5 C16' O15' C5' 115.2(2) O18' C16' O15' 121.1(3) O18' C16' C17' 127.1(3) O15' C16' C17' 111.8(3) C16' C17' H17A 109.5 C16' C17' H17B 109.5 H17A C17' H17B 109.5 C16' C17' H17C 109.5 H17A C17' H17C 109.5 H17B C17' H17C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C6 1.321(4) N1 C2 1.333(4) C2 N3 1.308(4) C2 Cl11 1.740(3) N3 C4 1.363(4) C4 N9 1.367(4) C4 C5 1.384(4) C5 C6 1.386(4) C5 N7 1.391(4) C6 Cl10 1.712(4) N7 C8 1.314(4) C8 N9 1.376(4) C8 H8 0.9300 N9 C1' 1.466(4) C1' O6' 1.409(4) C1' C2' 1.515(5) C1' H1 0.9800 C2' O7' 1.429(4) C2' C3' 1.532(4) C2' H2 0.9800 C3' O11' 1.429(3) C3' C4' 1.505(5) C3' H3 0.9800 C4' O6' 1.455(3) C4' C5' 1.497(4) C4' H4 0.9800 C5' O15' 1.439(4) C5' H5A 0.9700 C5' H5B 0.9700 O7' C8' 1.354(4) C8' O10' 1.187(4) C8' C9' 1.489(5) C9' H9A 0.9600 C9' H9C 0.9600 C9' H9B 0.9600 O11' C12' 1.351(5) C12' O14' 1.190(4) C12' C13' 1.502(5) C13' H13A 0.9600 C13' H13B 0.9600 C13' H13C 0.9600 O15' C16' 1.352(3) C16' O18' 1.198(4) C16' C17' 1.475(5) C17' H17A 0.9600 C17' H17B 0.9600 C17' H17C 0.9600 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C8 H8 O15' 1_555 1_555 1_555 0.93 2.52 3.265(4) 137 y C8 H8 O14' 1_555 1_555 2_757 0.93 2.56 3.350(4) 143 y C1' H1 N1 1_555 1_555 2_756 0.98 2.48 3.355(5) 148 y C9' H9B O18' 1_555 1_555 1_454 0.96 2.51 3.434(4) 161 y C13' H13B N7 1_555 1_555 1_455 0.96 2.54 3.502(5) 175 y C5' H5A Cg 1_555 1_555 2_757 0.97 2.69 3.454 136 y loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C6 N1 C2 N3 -2.3(6) C6 N1 C2 Cl11 178.7(3) N1 C2 N3 C4 3.0(5) Cl11 C2 N3 C4 -178.0(2) C2 N3 C4 N9 -178.6(3) C2 N3 C4 C5 -0.9(5) N3 C4 C5 C6 -1.5(5) N9 C4 C5 C6 176.6(3) N3 C4 C5 N7 180.0(3) N9 C4 C5 N7 -1.9(4) C2 N1 C6 C5 -0.8(5) C2 N1 C6 Cl10 178.4(3) C4 C5 C6 N1 2.4(5) N7 C5 C6 N1 -179.6(4) C4 C5 C6 Cl10 -176.8(3) N7 C5 C6 Cl10 1.2(6) C4 C5 N7 C8 0.9(4) C6 C5 N7 C8 -177.2(4) C5 N7 C8 N9 0.4(4) N3 C4 N9 C8 -179.9(3) C5 C4 N9 C8 2.0(3) N3 C4 N9 C1' -3.4(5) C5 C4 N9 C1' 178.5(3) N7 C8 N9 C4 -1.6(4) N7 C8 N9 C1' -177.9(3) C4 N9 C1' O6' -168.8(3) C8 N9 C1' O6' 6.9(4) C4 N9 C1' C2' 73.2(4) C8 N9 C1' C2' -111.1(3) O6' C1' C2' O7' 82.0(3) N9 C1' C2' O7' -159.2(2) O6' C1' C2' C3' -29.8(3) N9 C1' C2' C3' 89.0(3) O7' C2' C3' O11' 44.0(4) C1' C2' C3' O11' 156.5(3) O7' C2' C3' C4' -73.3(3) C1' C2' C3' C4' 39.2(3) O11' C3' C4' O6' -157.0(2) C2' C3' C4' O6' -35.5(3) O11' C3' C4' C5' 81.3(3) C2' C3' C4' C5' -157.2(2) O6' C4' C5' O15' -65.6(3) C3' C4' C5' O15' 53.4(3) N9 C1' O6' C4' -112.7(3) C2' C1' O6' C4' 8.2(3) C5' C4' O6' C1' 144.5(2) C3' C4' O6' C1' 17.6(3) C1' C2' O7' C8' 115.0(3) C3' C2' O7' C8' -137.4(3) C2' O7' C8' O10' -2.6(5) C2' O7' C8' C9' -178.7(3) C4' C3' O11' C12' -168.0(2) C2' C3' O11' C12' 78.9(3) C3' O11' C12' O14' -1.6(5) C3' O11' C12' C13' 178.4(3) C4' C5' O15' C16' 176.9(3) C5' O15' C16' O18' 4.7(5) C5' O15' C16' C17' -174.8(3)