# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_CCDC_904086 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; 4-amino-1-[(2R,5S)-2-(hydroxymethyl)-1,3-oxathiolan-5-yl]-(1H)-pyrimidin-2-one 4,5-dichloro hydrogen phthalate ; _chemical_name_common 'lamivudine 4,5-dichloro hydrogen phthalate' _chemical_formula_moiety 'C8 H12 N3 O3 S, C8 H3 Cl2 O4' _chemical_formula_sum 'C16 H15 Cl2 N3 O7 S' _chemical_formula_weight 464.28 _chemical_compound_source 'Crystal Screening' _chemical_absolute_configuration rmad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 _symmetry_space_group_name_Hall 'P 1' _symmetry_Int_Tables_number 1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.9680(3) _cell_length_b 10.3880(4) _cell_length_c 11.4140(4) _cell_angle_alpha 99.427(3) _cell_angle_beta 112.791(2) _cell_angle_gamma 90.988(3) _cell_volume 963.25(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3250 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 25.682 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.492 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.104924E-1 _diffrn_orient_matrix_ub_12 -0.266568E-1 _diffrn_orient_matrix_ub_13 0.829633E-1 _diffrn_orient_matrix_ub_21 -0.109525 _diffrn_orient_matrix_ub_22 -0.497519E-1 _diffrn_orient_matrix_ub_23 -0.446643E-1 _diffrn_orient_matrix_ub_31 0.513754E-1 _diffrn_orient_matrix_ub_32 -0.800757E-1 _diffrn_orient_matrix_ub_33 -0.217467E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_unetI/netI 0.0569 _diffrn_reflns_number 6022 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.39 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.952 _diffrn_measured_fraction_theta_max 0.952 _reflns_number_total 6022 _reflns_number_gt 4918 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia,1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0780P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6022 _refine_ls_number_parameters 553 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.12 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.057 _refine_ls_shift/su_mean 0.003 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(5) _refine_diff_density_max 0.207 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.038 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' S S 0.1246 0.1234 '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_ _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 Cl7A Cl 0.92028(12) 0.02743(10) 0.58274(10) 0.0678(3) Uani 1 1 d . . . Cl6B Cl 0.48727(12) 1.04866(10) 0.03693(10) 0.0634(3) Uani 1 1 d . . . Cl7B Cl 0.40404(13) 0.93704(11) 0.24966(11) 0.0718(3) Uani 1 1 d . . . Cl6A Cl 0.98297(13) 0.12816(12) 0.35643(11) 0.0713(3) Uani 1 1 d . . . O1XA O 0.4487(4) 0.2733(4) 0.6168(3) 0.0780(10) Uani 1 1 d . . . S3'A S 0.82605(14) 0.12916(11) 0.89274(11) 0.0662(3) Uani 1 1 d . . . N3A N 1.1966(4) 0.3363(3) 0.6978(3) 0.0493(7) Uani 1 1 d . . . C7A' C 0.7998(5) 0.1364(4) 0.4977(4) 0.0510(9) Uani 1 1 d . . . C8A' C 0.6747(5) 0.1821(4) 0.5314(4) 0.0501(9) Uani 1 1 d . . . H8A' H 0.6608 0.1551 0.6005 0.06 Uiso 1 1 calc R . . C6A' C 0.8261(5) 0.1787(4) 0.3995(4) 0.0500(9) Uani 1 1 d . . . O1'B O 0.5177(3) 0.8766(3) 0.7290(3) 0.0592(6) Uani 1 1 d . . . O4YA O 0.3637(5) 0.4355(5) 0.2767(4) 0.0970(13) Uani 1 1 d . . . C2B C 0.2027(4) 0.7994(4) 0.8267(4) 0.0493(9) Uani 1 1 d . . . C4A C 1.0856(4) 0.4182(4) 0.6383(4) 0.0490(8) Uani 1 1 d . . . O2A O 1.3104(3) 0.2203(3) 0.8554(3) 0.0693(8) Uani 1 1 d . . . C5A C 0.9693(5) 0.4534(4) 0.6908(4) 0.0514(9) Uani 1 1 d . . . H5A H 0.8915 0.5093 0.6543 0.062 Uiso 1 1 calc R . . N4A N 1.0918(5) 0.4614(4) 0.5398(4) 0.0621(9) Uani 1 1 d . . . O1YA O 0.3187(4) 0.3576(4) 0.4472(4) 0.0899(12) Uani 1 1 d . . . C4'A C 0.8591(5) 0.2738(4) 1.0147(4) 0.0590(10) Uani 1 1 d . . . H4'A H 0.8843 0.2466 1.098 0.071 Uiso 1 1 calc R . . C1A' C 0.4392(5) 0.3037(4) 0.5146(4) 0.0569(10) Uani 1 1 d . . . S3'B S 0.37969(16) 0.71012(14) 0.51311(12) 0.0825(4) Uani 1 1 d . . . C6A C 0.9729(4) 0.4052(4) 0.7941(4) 0.0524(9) Uani 1 1 d . . . H6A H 0.8962 0.4283 0.8283 0.063 Uiso 1 1 calc R . . N1A N 1.0858(4) 0.3232(3) 0.8503(3) 0.0479(7) Uani 1 1 d . . . O1'A O 1.0000(3) 0.3497(3) 1.0217(3) 0.0586(6) Uani 1 1 d . . . C2A' C 0.5696(5) 0.2669(4) 0.4655(4) 0.0484(8) Uani 1 1 d . . . C2B' C 0.7819(5) 0.7429(4) 0.2415(4) 0.0495(9) Uani 1 1 d . . . O1XB O 0.8387(4) 0.6303(4) 0.4166(3) 0.0783(9) Uani 1 1 d . . . C4B C 0.3022(4) 0.6446(3) 0.9707(4) 0.0486(8) Uani 1 1 d . . . C3A' C 0.5953(5) 0.3107(4) 0.3611(4) 0.0496(8) Uani 1 1 d . . . N4B N 0.2890(5) 0.5913(4) 1.0610(4) 0.0598(9) Uani 1 1 d . . . C1B' C 0.8709(5) 0.6447(4) 0.3260(4) 0.0586(10) Uani 1 1 d . . . O4XA O 0.5384(4) 0.4267(4) 0.1900(3) 0.0816(10) Uani 1 1 d . . . O2B O 0.1005(3) 0.8738(3) 0.7813(3) 0.0612(7) Uani 1 1 d . . . C8B' C 0.6543(5) 0.7908(4) 0.2711(4) 0.0550(9) Uani 1 1 d . . . H8B' H 0.6299 0.7591 0.3338 0.066 Uiso 1 1 calc R . . O5'B O 0.7214(5) 0.6671(4) 0.7270(5) 0.0975(12) Uani 1 1 d . . . C3B' C 0.8140(4) 0.7866(4) 0.1422(4) 0.0488(8) Uani 1 1 d . . . C5B C 0.4192(5) 0.6151(4) 0.9174(4) 0.0531(9) Uani 1 1 d . . . H5B H 0.487 0.5491 0.942 0.064 Uiso 1 1 calc R . . O5'A O 0.6715(4) 0.4054(4) 0.8728(3) 0.0747(8) Uani 1 1 d . . . C5B' C 0.7206(5) 0.8821(4) 0.0830(4) 0.0533(9) Uani 1 1 d . . . H5B' H 0.7425 0.913 0.0188 0.064 Uiso 1 1 calc R . . N1B N 0.3291(4) 0.7769(3) 0.7889(3) 0.0490(7) Uani 1 1 d . . . C5A' C 0.7248(5) 0.2665(4) 0.3326(4) 0.0538(9) Uani 1 1 d . . . H5A' H 0.7448 0.2962 0.2671 0.065 Uiso 1 1 calc R . . C1'A C 1.0979(5) 0.2765(4) 0.9710(4) 0.0541(9) Uani 1 1 d . . . H1'A H 1.2108 0.291 1.034 0.065 Uiso 1 1 calc R . . O4YB O 1.0425(5) 0.6683(4) 0.1431(4) 0.0871(11) Uani 1 1 d . . . O1YB O 0.9777(4) 0.5806(4) 0.3005(3) 0.0799(10) Uani 1 1 d . . . C2A C 1.2058(4) 0.2883(4) 0.8047(4) 0.0513(9) Uani 1 1 d . . . N3B N 0.1976(4) 0.7338(3) 0.9214(3) 0.0505(7) Uani 1 1 d . . . C6B C 0.4308(5) 0.6835(4) 0.8312(4) 0.0537(9) Uani 1 1 d . . . H6B H 0.5108 0.6667 0.7992 0.064 Uiso 1 1 calc R . . C4B' C 0.9417(5) 0.7454(4) 0.0903(4) 0.0565(10) Uani 1 1 d . . . C5'A C 0.7171(6) 0.3564(5) 0.9894(4) 0.0690(12) Uani 1 1 d . . . H5'1 H 0.6247 0.3043 0.9868 0.083 Uiso 1 1 calc R . . H5'2 H 0.7444 0.4298 1.0608 0.083 Uiso 1 1 calc R . . C4A' C 0.4982(5) 0.3978(4) 0.2722(4) 0.0558(9) Uani 1 1 d . . . C2'A C 1.0413(5) 0.1324(4) 0.9428(4) 0.0645(10) Uani 1 1 d . . . H2'1 H 1.0896 0.094 1.0196 0.077 Uiso 1 1 calc R . . H2'2 H 1.0695 0.085 0.8747 0.077 Uiso 1 1 calc R . . C5'B C 0.7144(6) 0.7705(6) 0.6603(5) 0.0776(13) Uani 1 1 d . . . H5'3 H 0.7376 0.7394 0.5848 0.093 Uiso 1 1 calc R . . H5'4 H 0.7975 0.8397 0.7158 0.093 Uiso 1 1 calc R . . C4'B C 0.5487(5) 0.8264(5) 0.6174(4) 0.0638(11) Uani 1 1 d . . . H4'B H 0.5521 0.8986 0.5726 0.077 Uiso 1 1 calc R . . O4XB O 0.9424(4) 0.7860(4) -0.0047(4) 0.0864(11) Uani 1 1 d . . . C6B' C 0.5979(5) 0.9328(4) 0.1152(4) 0.0507(9) Uani 1 1 d . . . C7B' C 0.5632(5) 0.8838(4) 0.2097(4) 0.0530(9) Uani 1 1 d . . . C1'B C 0.3528(4) 0.8670(4) 0.7056(4) 0.0557(9) Uani 1 1 d . . . H1'B H 0.3216 0.9538 0.7308 0.067 Uiso 1 1 calc R . . C2'B C 0.2535(6) 0.8173(6) 0.5642(5) 0.0782(13) Uani 1 1 d . . . H2'3 H 0.2291 0.8889 0.5169 0.094 Uiso 1 1 calc R . . H2'4 H 0.1524 0.7702 0.5515 0.094 Uiso 1 1 calc R . . H4B H 1.010(7) 0.614(7) 0.238(7) 0.117 Uiso 1 1 d . . . H5'A H 0.586(8) 0.335(7) 0.802(7) 0.117 Uiso 1 1 d . . . H4A H 0.341(8) 0.395(7) 0.340(7) 0.117 Uiso 1 1 d . . . H3A H 1.258(8) 0.318(6) 0.668(6) 0.094 Uiso 1 1 d . . . H4XA H 1.153(7) 0.421(6) 0.501(6) 0.094 Uiso 1 1 d . . . H4YA H 1.022(7) 0.511(6) 0.511(6) 0.094 Uiso 1 1 d . . . H3B H 0.116(7) 0.757(6) 0.961(6) 0.094 Uiso 1 1 d . . . H4YB H 0.360(8) 0.545(6) 1.099(6) 0.094 Uiso 1 1 d . . . H4XB H 0.206(7) 0.612(6) 1.098(6) 0.094 Uiso 1 1 d . . . H5'B H 0.754(8) 0.704(7) 0.828(8) 0.117 Uiso 1 1 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 Cl7A 0.0726(6) 0.0729(6) 0.0684(6) 0.0347(5) 0.0294(5) 0.0322(5) Cl6B 0.0665(6) 0.0624(6) 0.0660(6) 0.0278(5) 0.0244(5) 0.0231(5) Cl7B 0.0703(7) 0.0849(8) 0.0768(7) 0.0246(6) 0.0422(6) 0.0292(6) Cl6A 0.0694(6) 0.0862(7) 0.0754(7) 0.0260(6) 0.0415(6) 0.0306(6) O1XA 0.0681(19) 0.123(3) 0.070(2) 0.049(2) 0.0433(17) 0.0368(19) S3'A 0.0715(6) 0.0616(6) 0.0752(7) 0.0197(5) 0.0364(5) 0.0085(5) N3A 0.0471(17) 0.0568(18) 0.0516(18) 0.0221(15) 0.0223(14) 0.0193(14) C7A' 0.050(2) 0.050(2) 0.053(2) 0.0151(17) 0.0178(17) 0.0119(16) C8A' 0.054(2) 0.058(2) 0.043(2) 0.0203(17) 0.0201(17) 0.0100(18) C6A' 0.054(2) 0.053(2) 0.047(2) 0.0129(17) 0.0214(17) 0.0149(17) O1'B 0.0546(14) 0.0681(16) 0.0598(16) 0.0122(13) 0.0276(12) 0.0063(12) O4YA 0.093(2) 0.152(4) 0.093(2) 0.080(3) 0.062(2) 0.074(2) C2B 0.050(2) 0.049(2) 0.053(2) 0.0160(17) 0.0217(17) 0.0161(17) C4A 0.0463(19) 0.053(2) 0.054(2) 0.0202(17) 0.0217(17) 0.0117(16) O2A 0.0627(17) 0.095(2) 0.0744(19) 0.0499(17) 0.0386(15) 0.0384(16) C5A 0.053(2) 0.053(2) 0.058(2) 0.0236(18) 0.0266(18) 0.0184(17) N4A 0.065(2) 0.076(2) 0.063(2) 0.0379(19) 0.0339(18) 0.0280(19) O1YA 0.077(2) 0.138(3) 0.091(2) 0.069(2) 0.0513(19) 0.056(2) C4'A 0.064(2) 0.076(3) 0.055(2) 0.026(2) 0.0355(19) 0.019(2) C1A' 0.055(2) 0.071(3) 0.055(2) 0.027(2) 0.0263(18) 0.0170(19) S3'B 0.0909(8) 0.0965(9) 0.0593(7) 0.0050(6) 0.0331(6) -0.0023(7) C6A 0.0437(19) 0.062(2) 0.056(2) 0.0175(18) 0.0210(17) 0.0149(17) N1A 0.0492(16) 0.0570(17) 0.0463(17) 0.0215(14) 0.0230(13) 0.0179(13) O1'A 0.0629(16) 0.0648(16) 0.0539(16) 0.0113(13) 0.0288(13) 0.0133(13) C2A' 0.052(2) 0.0509(19) 0.046(2) 0.0124(16) 0.0216(16) 0.0060(16) C2B' 0.052(2) 0.054(2) 0.043(2) 0.0153(16) 0.0163(16) 0.0094(17) O1XB 0.097(2) 0.101(2) 0.0653(19) 0.0509(19) 0.0471(18) 0.0459(19) C4B 0.050(2) 0.0415(18) 0.052(2) 0.0152(17) 0.0157(17) 0.0105(16) C3A' 0.053(2) 0.056(2) 0.047(2) 0.0193(17) 0.0222(17) 0.0159(17) N4B 0.060(2) 0.065(2) 0.067(2) 0.0311(18) 0.0308(18) 0.0196(17) C1B' 0.059(2) 0.067(2) 0.052(2) 0.0219(19) 0.0192(18) 0.0164(19) O4XA 0.089(2) 0.112(3) 0.079(2) 0.058(2) 0.053(2) 0.053(2) O2B 0.0583(15) 0.0685(17) 0.0711(18) 0.0329(14) 0.0320(14) 0.0281(14) C8B' 0.062(2) 0.060(2) 0.050(2) 0.0206(18) 0.0246(18) 0.0128(18) O5'B 0.107(3) 0.117(3) 0.111(3) 0.058(3) 0.072(3) 0.062(2) C3B' 0.050(2) 0.052(2) 0.047(2) 0.0162(17) 0.0195(17) 0.0102(16) C5B 0.052(2) 0.051(2) 0.066(2) 0.0221(19) 0.0277(19) 0.0216(17) O5'A 0.0712(19) 0.095(2) 0.073(2) 0.0340(18) 0.0369(17) 0.0341(17) C5B' 0.055(2) 0.058(2) 0.054(2) 0.0241(19) 0.0232(18) 0.0116(18) N1B 0.0510(16) 0.0525(17) 0.0513(18) 0.0183(14) 0.0247(14) 0.0143(14) C5A' 0.057(2) 0.066(2) 0.047(2) 0.0211(18) 0.0256(18) 0.0146(19) C1'A 0.053(2) 0.071(2) 0.0438(19) 0.0204(18) 0.0202(17) 0.0149(17) O4YB 0.092(2) 0.112(3) 0.106(3) 0.071(2) 0.070(2) 0.058(2) O1YB 0.089(2) 0.103(2) 0.081(2) 0.056(2) 0.0527(19) 0.054(2) C2A 0.049(2) 0.060(2) 0.055(2) 0.0268(19) 0.0255(18) 0.0167(18) N3B 0.0507(17) 0.0526(17) 0.0594(19) 0.0231(15) 0.0284(15) 0.0176(14) C6B 0.054(2) 0.052(2) 0.063(2) 0.0156(18) 0.0285(19) 0.0199(17) C4B' 0.054(2) 0.065(2) 0.061(2) 0.027(2) 0.0275(19) 0.0158(19) C5'A 0.072(3) 0.088(3) 0.064(3) 0.024(2) 0.040(2) 0.020(2) C4A' 0.064(2) 0.063(2) 0.048(2) 0.0234(18) 0.0244(19) 0.0188(19) C2'A 0.080(3) 0.066(2) 0.070(3) 0.035(2) 0.044(2) 0.027(2) C5'B 0.075(3) 0.103(4) 0.084(3) 0.040(3) 0.053(3) 0.031(3) C4'B 0.069(3) 0.075(3) 0.063(3) 0.025(2) 0.038(2) 0.015(2) O4XB 0.089(2) 0.124(3) 0.088(2) 0.065(2) 0.060(2) 0.053(2) C6B' 0.051(2) 0.049(2) 0.049(2) 0.0128(17) 0.0150(17) 0.0095(17) C7B' 0.052(2) 0.056(2) 0.053(2) 0.0101(18) 0.0222(18) 0.0092(18) C1'B 0.055(2) 0.059(2) 0.064(2) 0.0237(19) 0.0303(19) 0.0158(17) C2'B 0.065(2) 0.108(4) 0.061(3) 0.032(3) 0.017(2) 0.008(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cl7A C7A' 1.726(4) . ? Cl6B C6B' 1.714(4) . ? Cl7B C7B' 1.731(4) . ? Cl6A C6A' 1.724(4) . ? O1XA C1A' 1.230(5) . ? S3'A C2'A 1.787(4) . ? S3'A C4'A 1.806(5) . ? N3A C2A 1.366(5) . ? N3A C4A 1.368(5) . ? N3A H3A 0.76(6) . ? C7A' C6A' 1.366(5) . ? C7A' C8A' 1.388(5) . ? C8A' C2A' 1.388(6) . ? C8A' H8A' 0.93 . ? C6A' C5A' 1.401(6) . ? O1'B C1'B 1.396(4) . ? O1'B C4'B 1.426(5) . ? O4YA C4A' 1.292(5) . ? O4YA H4A 0.97(8) . ? C2B O2B 1.223(5) . ? C2B N1B 1.371(5) . ? C2B N3B 1.383(5) . ? C4A N4A 1.296(5) . ? C4A C5A 1.417(5) . ? O2A C2A 1.204(5) . ? C5A C6A 1.344(6) . ? C5A H5A 0.93 . ? N4A H4XA 0.91(6) . ? N4A H4YA 0.82(7) . ? O1YA C1A' 1.262(5) . ? C4'A O1'A 1.447(5) . ? C4'A C5'A 1.508(6) . ? C4'A H4'A 0.98 . ? C1A' C2A' 1.510(5) . ? S3'B C2'B 1.790(5) . ? S3'B C4'B 1.800(5) . ? C6A N1A 1.367(5) . ? C6A H6A 0.93 . ? N1A C2A 1.395(4) . ? N1A C1'A 1.501(5) . ? O1'A C1'A 1.399(4) . ? C2A' C3A' 1.437(5) . ? C2B' C8B' 1.391(5) . ? C2B' C3B' 1.411(5) . ? C2B' C1B' 1.537(5) . ? O1XB C1B' 1.206(5) . ? C4B N4B 1.288(5) . ? C4B N3B 1.359(5) . ? C4B C5B 1.417(5) . ? C3A' C5A' 1.388(5) . ? C3A' C4A' 1.501(6) . ? N4B H4YB 0.83(7) . ? N4B H4XB 1.00(6) . ? C1B' O1YB 1.273(5) . ? O4XA C4A' 1.203(5) . ? C8B' C7B' 1.378(6) . ? C8B' H8B' 0.93 . ? O5'B C5'B 1.404(6) . ? O5'B H5'B 1.07(8) . ? C3B' C5B' 1.397(6) . ? C3B' C4B' 1.518(5) . ? C5B C6B 1.337(6) . ? C5B H5B 0.93 . ? O5'A C5'A 1.416(6) . ? O5'A H5'A 1.04(7) . ? C5B' C6B' 1.376(5) . ? C5B' H5B' 0.93 . ? N1B C6B 1.360(5) . ? N1B C1'B 1.506(5) . ? C5A' H5A' 0.93 . ? C1'A C2'A 1.513(6) . ? C1'A H1'A 0.98 . ? O4YB C4B' 1.258(5) . ? O4YB H4B 1.41(8) . ? O1YB H4B 0.98(7) . ? N3B H3B 1.01(6) . ? C6B H6B 0.93 . ? C4B' O4XB 1.228(5) . ? C5'A H5'1 0.97 . ? C5'A H5'2 0.97 . ? C2'A H2'1 0.97 . ? C2'A H2'2 0.97 . ? C5'B C4'B 1.531(6) . ? C5'B H5'3 0.97 . ? C5'B H5'4 0.97 . ? C4'B H4'B 0.98 . ? C6B' C7B' 1.398(6) . ? C1'B C2'B 1.504(7) . ? C1'B H1'B 0.98 . ? C2'B H2'3 0.97 . ? C2'B H2'4 0.97 . ? 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 C2'A S3'A C4'A 88.0(2) . . ? C2A N3A C4A 125.3(3) . . ? C2A N3A H3A 119(5) . . ? C4A N3A H3A 116(5) . . ? C6A' C7A' C8A' 119.8(4) . . ? C6A' C7A' Cl7A 121.5(3) . . ? C8A' C7A' Cl7A 118.7(3) . . ? C7A' C8A' C2A' 122.3(3) . . ? C7A' C8A' H8A' 118.9 . . ? C2A' C8A' H8A' 118.9 . . ? C7A' C6A' C5A' 119.5(3) . . ? C7A' C6A' Cl6A 121.7(3) . . ? C5A' C6A' Cl6A 118.7(3) . . ? C1'B O1'B C4'B 113.0(3) . . ? C4A' O4YA H4A 109(4) . . ? O2B C2B N1B 122.7(3) . . ? O2B C2B N3B 121.2(3) . . ? N1B C2B N3B 116.1(3) . . ? N4A C4A N3A 119.9(3) . . ? N4A C4A C5A 123.2(4) . . ? N3A C4A C5A 116.9(3) . . ? C6A C5A C4A 119.2(3) . . ? C6A C5A H5A 120.4 . . ? C4A C5A H5A 120.4 . . ? C4A N4A H4XA 118(4) . . ? C4A N4A H4YA 113(4) . . ? H4XA N4A H4YA 128(6) . . ? O1'A C4'A C5'A 110.1(4) . . ? O1'A C4'A S3'A 106.6(2) . . ? C5'A C4'A S3'A 114.6(3) . . ? O1'A C4'A H4'A 108.5 . . ? C5'A C4'A H4'A 108.5 . . ? S3'A C4'A H4'A 108.5 . . ? O1XA C1A' O1YA 121.3(4) . . ? O1XA C1A' C2A' 118.8(4) . . ? O1YA C1A' C2A' 119.9(3) . . ? C2'B S3'B C4'B 87.1(2) . . ? C5A C6A N1A 121.9(3) . . ? C5A C6A H6A 119 . . ? N1A C6A H6A 119 . . ? C6A N1A C2A 121.3(3) . . ? C6A N1A C1'A 122.2(3) . . ? C2A N1A C1'A 116.3(3) . . ? C1'A O1'A C4'A 113.5(3) . . ? C8A' C2A' C3A' 118.2(3) . . ? C8A' C2A' C1A' 114.6(3) . . ? C3A' C2A' C1A' 127.2(3) . . ? C8B' C2B' C3B' 119.0(3) . . ? C8B' C2B' C1B' 112.6(3) . . ? C3B' C2B' C1B' 128.4(3) . . ? N4B C4B N3B 119.0(3) . . ? N4B C4B C5B 124.1(4) . . ? N3B C4B C5B 117.0(3) . . ? C5A' C3A' C2A' 118.1(3) . . ? C5A' C3A' C4A' 112.6(3) . . ? C2A' C3A' C4A' 129.3(3) . . ? C4B N4B H4YB 120(4) . . ? C4B N4B H4XB 124(3) . . ? H4YB N4B H4XB 116(6) . . ? O1XB C1B' O1YB 120.9(4) . . ? O1XB C1B' C2B' 119.1(4) . . ? O1YB C1B' C2B' 120.0(4) . . ? C7B' C8B' C2B' 121.7(3) . . ? C7B' C8B' H8B' 119.2 . . ? C2B' C8B' H8B' 119.2 . . ? C5'B O5'B H5'B 111(4) . . ? C5B' C3B' C2B' 117.8(3) . . ? C5B' C3B' C4B' 113.7(3) . . ? C2B' C3B' C4B' 128.5(3) . . ? C6B C5B C4B 119.2(3) . . ? C6B C5B H5B 120.4 . . ? C4B C5B H5B 120.4 . . ? C5'A O5'A H5'A 106(4) . . ? C6B' C5B' C3B' 123.2(3) . . ? C6B' C5B' H5B' 118.4 . . ? C3B' C5B' H5B' 118.4 . . ? C6B N1B C2B 121.2(3) . . ? C6B N1B C1'B 122.9(3) . . ? C2B N1B C1'B 115.8(3) . . ? C3A' C5A' C6A' 122.0(3) . . ? C3A' C5A' H5A' 119 . . ? C6A' C5A' H5A' 119 . . ? O1'A C1'A N1A 107.8(3) . . ? O1'A C1'A C2'A 109.6(3) . . ? N1A C1'A C2'A 111.3(3) . . ? O1'A C1'A H1'A 109.4 . . ? N1A C1'A H1'A 109.4 . . ? C2'A C1'A H1'A 109.4 . . ? C4B' O4YB H4B 114(3) . . ? C1B' O1YB H4B 113(4) . . ? O2A C2A N3A 122.0(3) . . ? O2A C2A N1A 122.6(3) . . ? N3A C2A N1A 115.4(3) . . ? C4B N3B C2B 124.0(3) . . ? C4B N3B H3B 117(4) . . ? C2B N3B H3B 119(3) . . ? C5B C6B N1B 122.0(3) . . ? C5B C6B H6B 119 . . ? N1B C6B H6B 119 . . ? O4XB C4B' O4YB 121.1(4) . . ? O4XB C4B' C3B' 119.1(4) . . ? O4YB C4B' C3B' 119.8(4) . . ? O5'A C5'A C4'A 114.0(3) . . ? O5'A C5'A H5'1 108.8 . . ? C4'A C5'A H5'1 108.8 . . ? O5'A C5'A H5'2 108.8 . . ? C4'A C5'A H5'2 108.8 . . ? H5'1 C5'A H5'2 107.7 . . ? O4XA C4A' O4YA 118.9(4) . . ? O4XA C4A' C3A' 120.7(4) . . ? O4YA C4A' C3A' 120.3(4) . . ? C1'A C2'A S3'A 104.3(3) . . ? C1'A C2'A H2'1 110.9 . . ? S3'A C2'A H2'1 110.9 . . ? C1'A C2'A H2'2 110.9 . . ? S3'A C2'A H2'2 110.9 . . ? H2'1 C2'A H2'2 108.9 . . ? O5'B C5'B C4'B 112.6(4) . . ? O5'B C5'B H5'3 109.1 . . ? C4'B C5'B H5'3 109.1 . . ? O5'B C5'B H5'4 109.1 . . ? C4'B C5'B H5'4 109.1 . . ? H5'3 C5'B H5'4 107.8 . . ? O1'B C4'B C5'B 109.0(4) . . ? O1'B C4'B S3'B 106.8(3) . . ? C5'B C4'B S3'B 114.9(4) . . ? O1'B C4'B H4'B 108.7 . . ? C5'B C4'B H4'B 108.7 . . ? S3'B C4'B H4'B 108.7 . . ? C5B' C6B' C7B' 118.1(4) . . ? C5B' C6B' Cl6B 120.4(3) . . ? C7B' C6B' Cl6B 121.4(3) . . ? C8B' C7B' C6B' 120.1(4) . . ? C8B' C7B' Cl7B 119.2(3) . . ? C6B' C7B' Cl7B 120.7(3) . . ? O1'B C1'B C2'B 110.0(3) . . ? O1'B C1'B N1B 107.4(3) . . ? C2'B C1'B N1B 112.0(4) . . ? O1'B C1'B H1'B 109.1 . . ? C2'B C1'B H1'B 109.1 . . ? N1B C1'B H1'B 109.1 . . ? C1'B C2'B S3'B 104.3(3) . . ? C1'B C2'B H2'3 110.9 . . ? S3'B C2'B H2'3 110.9 . . ? C1'B C2'B H2'4 110.9 . . ? S3'B C2'B H2'4 110.9 . . ? H2'3 C2'B H2'4 108.9 . . ? _vrf_PLAT_029_CCDC904086 ; RESPONSE: This error message appears because Bragg reflections had low intensity at high resolution. ; _vrf_PLAT_111_CCDC904086 ; RESPONSE: False inversion centre incompatible with the enantiopure crystal of lamivudine. ; _vrf_PLAT_431_CCDC904086 ; RESPONSE: This error message appears because of the close packing of lamivudine and counterion units. ; _vrf_PLAT_772_CCDC904086 ; RESPONSE: This error message appears because of the intramolecular hydrogen bond in counterion. ; # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of _database_code_depnum_ccdc_archive 'CCDC 904086' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_CCDC_912146 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; 4-amino-1-[(2R,5S)-2-(hydroxymethyl)-1,3-oxathiolan-5-yl]-(1H)-pyrimidin-2-one hydrogen hemihydrate phthalate ; _chemical_name_common 'lamivudine hydrogen hemihydrate phthalate' _chemical_formula_moiety '2(C8 H12 N3 O3 S), 2(C8 H5 O4), H2 O' _chemical_formula_sum 'C32 H36 N6 O15 S2' _chemical_formula_weight 808.81 _chemical_absolute_configuration rmad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 5.3110(5) _cell_length_b 21.103(2) _cell_length_c 33.059 _cell_angle_alpha 90 _cell_angle_beta 94.675(6) _cell_angle_gamma 90 _cell_volume 3692.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3202 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 22.53 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.223 _exptl_absorpt_correction_T_min 0.5461 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Sheldrick, G. M.: SADABS --- Bruker AXS area detector scaling and absorption, version 2008/1, University of G\"ottingen, Germany 2008 ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_unetI/netI 0.1202 _diffrn_reflns_number 20849 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.4 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.98 _reflns_number_total 11695 _reflns_number_gt 5733 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.1369P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 11695 _refine_ls_number_parameters 992 _refine_ls_number_restraints 861 _refine_ls_R_factor_all 0.1503 _refine_ls_R_factor_gt 0.065 _refine_ls_wR_factor_ref 0.2532 _refine_ls_wR_factor_gt 0.1757 _refine_ls_goodness_of_fit_ref 0.99 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.135 _refine_ls_shift/su_mean 0.023 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.13(15) _refine_diff_density_max 0.479 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.118 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 and6.1.1.4' H H 0 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 S3'D S 0.4132(9) 0.4566(2) 0.11541(12) 0.0514(11) Uani 1 1 d . . . O1'D O 0.7212(18) 0.5489(5) 0.1021(3) 0.043(2) Uani 1 1 d U . . O5'D O 0.656(3) 0.5316(8) 0.1875(4) 0.092(4) Uani 1 1 d U . . H5'D H 0.7179 0.5342 0.2116 0.138 Uiso 1 1 calc R . . O2D O 0.176(2) 0.6167(6) 0.0203(3) 0.060(3) Uani 1 1 d U . . N1D N 0.335(3) 0.6026(6) 0.0864(3) 0.046(2) Uani 1 1 d U . . N3D N 0.004(2) 0.6702(5) 0.0699(3) 0.041(3) Uani 1 1 d U . . H3D H -0.0949 0.6889 0.0509 0.049 Uiso 1 1 calc R . . N4D N -0.214(3) 0.7256(6) 0.1189(3) 0.055(4) Uani 1 1 d U . . H4D1 H -0.3181 0.7405 0.0991 0.065 Uiso 1 1 calc R . . H4D2 H -0.2333 0.7361 0.1442 0.065 Uiso 1 1 calc R . . C4'D C 0.724(3) 0.4885(8) 0.1207(4) 0.043(3) Uani 1 1 d U . . H4'D H 0.8347 0.4602 0.1057 0.051 Uiso 1 1 calc R . . C5'D C 0.833(4) 0.4930(9) 0.1626(4) 0.056(4) Uani 1 1 d U . . H5'1 H 1.0006 0.5138 0.1634 0.068 Uiso 1 1 calc R . . H5'2 H 0.8564 0.45 0.1744 0.068 Uiso 1 1 calc R . . C2'D C 0.404(4) 0.4939(8) 0.0647(4) 0.050(3) Uani 1 1 d U . . H2'1 H 0.5012 0.4686 0.0462 0.06 Uiso 1 1 calc R . . H2'2 H 0.2272 0.4977 0.0527 0.06 Uiso 1 1 calc R . . C1'D C 0.514(3) 0.5549(8) 0.0712(4) 0.044(3) Uani 1 1 d U . . H1'D H 0.5786 0.5706 0.0455 0.053 Uiso 1 1 calc R . . C2D C 0.167(3) 0.6293(7) 0.0577(4) 0.045(3) Uani 1 1 d U . . C6D C 0.317(3) 0.6198(8) 0.1273(4) 0.048(3) Uani 1 1 d U . . H6D H 0.4234 0.5988 0.1475 0.058 Uiso 1 1 calc R . . C5D C 0.171(3) 0.6601(8) 0.1382(4) 0.049(3) Uani 1 1 d U . . H5D H 0.1881 0.674 0.1656 0.059 Uiso 1 1 calc R . . C4D C -0.029(3) 0.6876(7) 0.1107(4) 0.045(3) Uani 1 1 d U . . S3'B S 0.0842(8) -0.04141(18) 0.38458(13) 0.0422(9) Uani 1 1 d . . . O1'B O -0.2265(16) 0.0525(4) 0.3987(3) 0.034(2) Uani 1 1 d U . . O5'B O -0.165(2) 0.0302(6) 0.3130(3) 0.066(3) Uani 1 1 d U . . H5'B H -0.2325 0.0358 0.2894 0.099 Uiso 1 1 calc R . . O2B O 0.301(2) 0.1223(5) 0.4778(3) 0.053(3) Uani 1 1 d U . . N1B N 0.1537(19) 0.1068(5) 0.4140(3) 0.028(2) Uani 1 1 d U . . N3B N 0.495(2) 0.1757(5) 0.4290(4) 0.032(2) Uani 1 1 d U . . H3B H 0.6004 0.1949 0.4468 0.038 Uiso 1 1 calc R . . N4B N 0.687(2) 0.2250(6) 0.3815(4) 0.047(3) Uani 1 1 d U . . H4B1 H 0.7918 0.2419 0.4005 0.057 Uiso 1 1 calc R . . H4B2 H 0.7032 0.2339 0.3558 0.057 Uiso 1 1 calc R . . C4'B C -0.241(3) -0.0104(6) 0.3762(5) 0.037(3) Uani 1 1 d U . . H4'B H -0.3593 -0.0394 0.3894 0.044 Uiso 1 1 calc R . . C5'B C -0.328(3) -0.0023(7) 0.3351(5) 0.048(3) Uani 1 1 d U . . H5'3 H -0.3585 -0.0445 0.3227 0.058 Uiso 1 1 calc R . . H5'4 H -0.4909 0.0205 0.3337 0.058 Uiso 1 1 calc R . . C2'B C 0.119(3) -0.0092(6) 0.4343(4) 0.036(3) Uani 1 1 d U . . H2'3 H 0.0345 -0.036 0.4537 0.044 Uiso 1 1 calc R . . H2'4 H 0.2994 -0.0043 0.4439 0.044 Uiso 1 1 calc R . . C1'B C -0.019(3) 0.0591(6) 0.4281(4) 0.033(2) Uani 1 1 d U . . H1'B H -0.0817 0.0732 0.4544 0.04 Uiso 1 1 calc R . . C2B C 0.317(2) 0.1338(6) 0.4441(4) 0.030(2) Uani 1 1 d U . . C6B C 0.170(3) 0.1176(6) 0.3737(4) 0.034(3) Uani 1 1 d U . . H6B H 0.0553 0.0969 0.3545 0.041 Uiso 1 1 calc R . . C5B C 0.355(2) 0.1597(6) 0.3599(4) 0.031(2) Uani 1 1 d U . . H5B H 0.3698 0.1679 0.3319 0.037 Uiso 1 1 calc R . . C4B C 0.516(2) 0.1882(5) 0.3910(4) 0.025(2) Uani 1 1 d U . . S3'A S 0.1529(8) 0.1510(2) 0.11155(11) 0.0455(10) Uani 1 1 d . . . O1'A O -0.1625(19) 0.0593(5) 0.0935(3) 0.042(2) Uani 1 1 d U . . O5'A O -0.065(2) 0.0686(5) 0.1803(3) 0.056(3) Uani 1 1 d U . . H5'A H -0.1094 0.0636 0.2039 0.084 Uiso 1 1 calc R . . O2A O 0.323(3) -0.0045(7) 0.0158(2) 0.076(4) Uani 1 1 d U . . N1A N 0.187(2) 0.0066(6) 0.0792(3) 0.043(2) Uani 1 1 d U . . N3A N 0.528(3) -0.0612(6) 0.0637(3) 0.042(3) Uani 1 1 d U . . H3A H 0.6205 -0.0783 0.0457 0.05 Uiso 1 1 calc R . . N4A N 0.745(3) -0.1187(6) 0.1134(4) 0.048(3) Uani 1 1 d U . . H4A1 H 0.8371 -0.1335 0.0946 0.057 Uiso 1 1 calc R . . H4A2 H 0.7746 -0.1311 0.1388 0.057 Uiso 1 1 calc R . . C4'A C -0.173(3) 0.1185(7) 0.1148(4) 0.039(3) Uani 1 1 d U . . H4'A H -0.3001 0.1472 0.1002 0.047 Uiso 1 1 calc R . . C5'A C -0.237(3) 0.1099(7) 0.1586(4) 0.047(3) Uani 1 1 d U . . H5'5 H -0.2333 0.1517 0.1722 0.057 Uiso 1 1 calc R . . H5'6 H -0.4101 0.0926 0.1588 0.057 Uiso 1 1 calc R . . C2'A C 0.140(3) 0.1214(8) 0.0593(4) 0.052(3) Uani 1 1 d U . . H2'5 H 0.0367 0.1492 0.0403 0.062 Uiso 1 1 calc R . . H2'6 H 0.3109 0.1167 0.0497 0.062 Uiso 1 1 calc R . . C1'A C 0.013(3) 0.0570(8) 0.0646(4) 0.046(3) Uani 1 1 d U . . H1'A H -0.0748 0.0438 0.038 0.055 Uiso 1 1 calc R . . C2A C 0.349(3) -0.0175(7) 0.0513(4) 0.044(3) Uani 1 1 d U . . C6A C 0.218(3) -0.0090(7) 0.1179(4) 0.041(3) Uani 1 1 d U . . H6A H 0.1198 0.0108 0.137 0.05 Uiso 1 1 calc R . . C5A C 0.398(3) -0.0553(7) 0.1305(5) 0.046(3) Uani 1 1 d U . . H5A H 0.4052 -0.0706 0.1576 0.056 Uiso 1 1 calc R . . C4A C 0.568(3) -0.0792(7) 0.1039(4) 0.041(3) Uani 1 1 d U . . S3'C S 0.3389(7) 0.65254(18) 0.38816(13) 0.0431(9) Uani 1 1 d . . . O1'C O 0.6780(18) 0.5636(4) 0.4077(3) 0.035(2) Uani 1 1 d U . . O5'C O 0.579(2) 0.5665(5) 0.3191(3) 0.053(3) Uani 1 1 d U . . H5'C H 0.636 0.5641 0.2962 0.08 Uiso 1 1 calc R . . O2C O 0.169(2) 0.5022(5) 0.4855(3) 0.049(3) Uani 1 1 d U . . N1C N 0.292(2) 0.5075(5) 0.4205(3) 0.031(2) Uani 1 1 d U . . N3C N -0.037(2) 0.4433(5) 0.4345(4) 0.041(2) Uani 1 1 d U . . H3C H -0.1439 0.4287 0.4513 0.049 Uiso 1 1 calc R . . N4C N -0.262(2) 0.3828(5) 0.3864(4) 0.048(3) Uani 1 1 d U . . H4C1 H -0.3617 0.3696 0.4046 0.058 Uiso 1 1 calc R . . H4C2 H -0.2856 0.3694 0.3611 0.058 Uiso 1 1 calc R . . C4'C C 0.648(3) 0.6208(7) 0.3856(5) 0.041(3) Uani 1 1 d U . . H4'C H 0.7689 0.6521 0.3991 0.049 Uiso 1 1 calc R . . C2'C C 0.353(3) 0.6191(7) 0.4388(4) 0.040(3) Uani 1 1 d U . . H2'7 H 0.4483 0.6474 0.4584 0.048 Uiso 1 1 calc R . . H2'8 H 0.1803 0.6134 0.4475 0.048 Uiso 1 1 calc R . . C1'C C 0.481(3) 0.5576(6) 0.4367(4) 0.036(2) Uani 1 1 d U . . H1'C H 0.5584 0.5452 0.4641 0.044 Uiso 1 1 calc R . . C2C C 0.145(3) 0.4844(6) 0.4514(5) 0.037(3) Uani 1 1 d U . . C6C C 0.261(3) 0.4885(6) 0.3824(4) 0.033(3) Uani 1 1 d U . . H6C H 0.3742 0.5047 0.3641 0.039 Uiso 1 1 calc R . . C5C C 0.084(3) 0.4480(6) 0.3677(4) 0.037(3) Uani 1 1 d U . . H5C H 0.0637 0.4366 0.3399 0.045 Uiso 1 1 calc R . . C4C C -0.074(3) 0.4230(6) 0.3970(4) 0.035(3) Uani 1 1 d U . . O1XA O 1.187(2) 0.3862(6) -0.0088(3) 0.064(3) Uani 1 1 d U . . O1YA O 0.912(2) 0.3361(5) -0.0527(3) 0.051(3) Uani 1 1 d U . . C1A' C 0.994(3) 0.3539(7) -0.0152(3) 0.046(3) Uani 1 1 d DU . . C2A' C 0.860(3) 0.3253(6) 0.0193(3) 0.042(3) Uani 1 1 d DU . . C8A' C 0.986(3) 0.3392(7) 0.0579(3) 0.051(3) Uani 1 1 d DU . . H8A' H 1.1422 0.3613 0.0591 0.061 Uiso 1 1 calc R . . C7A' C 0.891(3) 0.3219(8) 0.0932(3) 0.057(3) Uani 1 1 d DU . . H7A' H 0.9778 0.3333 0.1184 0.069 Uiso 1 1 calc R . . C6A' C 0.668(3) 0.2879(8) 0.0928(3) 0.053(3) Uani 1 1 d DU . . H6A' H 0.5917 0.2788 0.1172 0.063 Uiso 1 1 calc R . . C5A' C 0.561(3) 0.2680(7) 0.0564(3) 0.045(3) Uani 1 1 d DU . . H5A' H 0.4182 0.2408 0.0562 0.054 Uiso 1 1 calc R . . C3A' C 0.649(2) 0.2852(7) 0.0185(3) 0.041(3) Uani 1 1 d DU . . C4A' C 0.495(3) 0.2566(7) -0.0164(3) 0.046(3) Uani 1 1 d DU . . O4YA O 0.543(2) 0.2737(6) -0.0549(3) 0.066(3) Uani 1 1 d U . . H4YA H 0.6709 0.2972 -0.0539 0.099 Uiso 1 1 calc R . . O4XA O 0.305(2) 0.2233(6) -0.0111(3) 0.055(3) Uani 1 1 d U . . O1XB O -0.186(2) 0.2282(5) 0.4896(3) 0.051(3) Uani 1 1 d U . . O1YB O 0.0583(16) 0.2714(5) 0.4472(3) 0.039(2) Uani 1 1 d U . . C1B' C -0.005(2) 0.2607(6) 0.4834(4) 0.034(3) Uani 1 1 d DU . . C2B' C 0.151(2) 0.2871(5) 0.5194(3) 0.031(2) Uani 1 1 d DU . . C8B' C 0.062(3) 0.2705(7) 0.5558(3) 0.047(3) Uani 1 1 d DU . . H8B' H -0.0892 0.2466 0.5553 0.056 Uiso 1 1 calc R . . C7B' C 0.181(3) 0.2868(7) 0.5926(3) 0.046(3) Uani 1 1 d DU . . H7B' H 0.1185 0.2726 0.6171 0.055 Uiso 1 1 calc R . . C6B' C 0.398(2) 0.3250(6) 0.5933(3) 0.038(3) Uani 1 1 d DU . . H6B' H 0.4813 0.3379 0.6184 0.046 Uiso 1 1 calc R . . C5B' C 0.487(2) 0.3435(6) 0.5577(3) 0.036(3) Uani 1 1 d DU . . H5B' H 0.6338 0.3694 0.5585 0.044 Uiso 1 1 calc R . . C3B' C 0.370(2) 0.3256(5) 0.5197(3) 0.032(2) Uani 1 1 d DU . . C4B' C 0.496(3) 0.3515(6) 0.4842(4) 0.039(3) Uani 1 1 d DU . . O4YB O 0.4272(19) 0.3371(5) 0.4474(3) 0.052(3) Uani 1 1 d U . . H4YB H 0.3103 0.3102 0.4469 0.078 Uiso 1 1 calc R . . O4XB O 0.669(2) 0.3906(5) 0.4912(4) 0.059(3) Uani 1 1 d U . . O1XC O 0.689(3) 0.8466(6) 0.1932(5) 0.089(4) Uani 1 1 d U . . O1YC O 0.673(3) 0.7397(6) 0.2006(3) 0.085(4) Uani 1 1 d U . . H1YC H 0.603 0.714 0.2155 0.127 Uiso 1 1 calc R . . C1C' C 0.606(3) 0.7978(8) 0.2093(4) 0.063(4) Uani 1 1 d DU . . C2C' C 0.428(3) 0.8069(6) 0.2425(4) 0.056(3) Uani 1 1 d DU . . C8C' C 0.370(4) 0.8698(6) 0.2490(5) 0.071(4) Uani 1 1 d DU . . H8C' H 0.4534 0.902 0.2351 0.085 Uiso 1 1 calc R . . C7C' C 0.194(4) 0.8865(8) 0.2752(5) 0.085(4) Uani 1 1 d DU . . H7C' H 0.1426 0.9294 0.2772 0.102 Uiso 1 1 calc R . . C6C' C 0.089(4) 0.8404(8) 0.2990(6) 0.086(4) Uani 1 1 d DU . . H6C' H -0.0159 0.8524 0.3197 0.103 Uiso 1 1 calc R . . C5C' C 0.139(3) 0.7776(7) 0.2924(5) 0.078(4) Uani 1 1 d DU . . H5C' H 0.06 0.7462 0.3077 0.093 Uiso 1 1 calc R . . C3C' C 0.305(3) 0.7586(6) 0.2634(4) 0.059(3) Uani 1 1 d DU . . C4C' C 0.353(4) 0.6892(6) 0.2613(5) 0.068(4) Uani 1 1 d DU . . O4YC O 0.486(3) 0.6623(7) 0.2386(4) 0.089(4) Uani 1 1 d U . . O4XC O 0.230(2) 0.6546(6) 0.2873(4) 0.080(4) Uani 1 1 d U . . O4XD O 0.260(3) 0.1536(7) 0.2153(4) 0.082(4) Uani 1 1 d U . . O4YD O -0.001(3) 0.1664(7) 0.2634(5) 0.112(5) Uani 1 1 d U . . H4YD H -0.0651 0.1974 0.2748 0.168 Uiso 1 1 calc R . . C4D' C 0.160(4) 0.1875(6) 0.2372(5) 0.068(4) Uani 1 1 d DU . . C3D' C 0.184(3) 0.2583(6) 0.2364(4) 0.063(3) Uani 1 1 d DU . . C5D' C 0.352(3) 0.2773(8) 0.2087(5) 0.080(4) Uani 1 1 d DU . . H5D' H 0.4244 0.2453 0.193 0.096 Uiso 1 1 calc R . . C6D' C 0.422(4) 0.3392(7) 0.2024(5) 0.079(4) Uani 1 1 d DU . . H6D' H 0.5498 0.35 0.1851 0.095 Uiso 1 1 calc R . . C7D' C 0.292(3) 0.3856(8) 0.2235(5) 0.078(4) Uani 1 1 d DU . . H7D' H 0.3223 0.4294 0.2193 0.094 Uiso 1 1 calc R . . C8D' C 0.122(3) 0.3673(7) 0.2499(5) 0.068(4) Uani 1 1 d DU . . H8D' H 0.0434 0.3996 0.2645 0.082 Uiso 1 1 calc R . . C2D' C 0.055(3) 0.3051(6) 0.2571(4) 0.059(3) Uani 1 1 d DU . . C1D' C -0.127(3) 0.2977(9) 0.2900(4) 0.067(4) Uani 1 1 d DU . . O1YD O -0.205(3) 0.2436(7) 0.2988(4) 0.088(4) Uani 1 1 d U . . O1XD O -0.201(3) 0.3433(7) 0.3076(4) 0.100(5) Uani 1 1 d U . . O1W O 0.929(2) 0.5386(6) 0.2608(3) 0.074(4) Uani 1 1 d . . . H11W H 1.0172 0.5105 0.2742 0.112 Uiso 1 1 d R . . H21W H 1.0126 0.5736 0.2616 0.112 Uiso 1 1 d R . . O2W O 0.558(4) 0.0411(8) 0.2403(5) 0.132(7) Uani 1 1 d . . . H12W H 0.4351 0.0681 0.2386 0.199 Uiso 1 1 d R . . H22W H 0.5102 0.0082 0.2265 0.199 Uiso 1 1 d R . . C5'C C 0.729(3) 0.6099(9) 0.3441(5) 0.060(4) Uani 1 1 d U . . H5'7 H 0.7306 0.6511 0.3299 0.072 Uiso 1 1 calc R . . H5'8 H 0.9053 0.5939 0.3468 0.072 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 S3'D 0.055(3) 0.060(3) 0.040(2) 0.008(2) 0.008(2) -0.006(2) O1'D 0.042(5) 0.051(5) 0.036(4) 0.002(4) 0.009(4) 0.003(5) O5'D 0.067(8) 0.141(11) 0.063(7) 0.006(8) -0.025(6) 0.044(8) O2D 0.092(8) 0.071(7) 0.018(4) -0.003(5) 0.001(5) 0.015(7) N1D 0.065(5) 0.053(5) 0.021(4) 0.003(4) 0.007(4) 0.009(5) N3D 0.063(6) 0.047(6) 0.013(4) 0.004(4) 0.004(4) 0.009(5) N4D 0.076(9) 0.060(8) 0.030(5) -0.014(6) 0.019(6) 0.022(7) C4'D 0.040(6) 0.058(7) 0.031(5) 0.006(5) 0.008(5) -0.002(6) C5'D 0.052(7) 0.074(8) 0.042(6) 0.006(6) -0.002(6) -0.002(7) C2'D 0.071(8) 0.056(7) 0.025(5) 0.002(6) 0.011(6) 0.004(7) C1'D 0.055(6) 0.055(6) 0.025(4) -0.005(5) 0.008(5) 0.004(5) C2D 0.067(6) 0.053(6) 0.014(4) 0.006(4) 0.002(5) 0.009(6) C6D 0.070(7) 0.057(6) 0.016(5) -0.001(5) -0.005(5) 0.010(6) C5D 0.076(7) 0.054(6) 0.016(4) 0.003(5) 0.000(5) 0.012(6) C4D 0.073(7) 0.044(6) 0.019(4) 0.008(5) 0.007(5) 0.007(6) S3'B 0.033(2) 0.0284(18) 0.067(2) -0.0049(18) 0.013(2) 0.0031(17) O1'B 0.025(4) 0.014(4) 0.063(5) 0.000(4) -0.001(4) 0.004(4) O5'B 0.067(7) 0.090(8) 0.042(5) 0.013(6) 0.013(5) -0.027(6) O2B 0.034(5) 0.062(7) 0.059(6) 0.013(6) -0.010(5) -0.018(5) N1B 0.021(4) 0.022(4) 0.040(4) 0.002(4) -0.004(4) 0.004(4) N3B 0.022(4) 0.015(4) 0.057(5) -0.004(4) -0.004(4) -0.003(4) N4B 0.034(7) 0.032(6) 0.075(8) -0.016(6) -0.002(6) 0.002(5) C4'B 0.030(5) 0.021(5) 0.059(6) -0.005(5) 0.001(5) -0.009(5) C5'B 0.040(7) 0.038(6) 0.067(7) -0.003(6) 0.005(6) -0.017(6) C2'B 0.040(7) 0.024(6) 0.046(6) 0.015(5) 0.011(6) 0.011(5) C1'B 0.027(5) 0.022(5) 0.049(5) 0.006(4) -0.002(4) 0.003(4) C2B 0.019(5) 0.027(5) 0.044(5) 0.008(4) 0.002(5) 0.002(4) C6B 0.033(5) 0.027(5) 0.043(5) 0.005(5) 0.009(5) 0.003(5) C5B 0.026(5) 0.025(5) 0.044(5) 0.008(5) 0.010(5) 0.014(4) C4B 0.020(5) 0.008(4) 0.050(5) -0.001(4) 0.012(5) 0.010(4) S3'A 0.055(3) 0.047(2) 0.0334(17) -0.0037(18) -0.0016(19) -0.005(2) O1'A 0.047(5) 0.049(5) 0.031(4) -0.004(4) 0.004(4) 0.002(4) O5'A 0.077(8) 0.047(6) 0.043(6) 0.004(5) 0.003(6) 0.015(6) O2A 0.096(9) 0.125(10) 0.010(4) 0.003(5) 0.012(5) 0.014(8) N1A 0.050(5) 0.052(5) 0.028(4) -0.002(4) 0.006(4) -0.010(5) N3A 0.058(6) 0.039(5) 0.030(5) -0.001(4) 0.013(5) -0.005(5) N4A 0.062(8) 0.045(7) 0.037(6) -0.005(6) 0.016(6) -0.008(6) C4'A 0.050(6) 0.042(6) 0.027(5) -0.002(5) 0.003(5) 0.015(6) C5'A 0.054(7) 0.051(7) 0.039(6) 0.012(6) 0.009(6) 0.014(6) C2'A 0.071(8) 0.056(7) 0.028(6) 0.001(6) -0.003(6) -0.014(7) C1'A 0.051(6) 0.056(6) 0.031(5) 0.001(5) 0.004(5) -0.008(5) C2A 0.052(6) 0.056(6) 0.025(5) 0.001(5) 0.014(5) -0.007(5) C6A 0.047(6) 0.051(6) 0.026(5) -0.002(5) 0.011(5) 0.004(5) C5A 0.057(7) 0.041(6) 0.042(6) 0.009(5) 0.015(6) 0.007(6) C4A 0.059(7) 0.031(6) 0.036(5) 0.001(5) 0.012(5) 0.001(5) S3'C 0.032(2) 0.0313(19) 0.066(2) 0.007(2) 0.0032(19) -0.0011(17) O1'C 0.034(4) 0.023(4) 0.050(4) -0.010(4) 0.016(4) -0.006(4) O5'C 0.050(6) 0.081(8) 0.031(5) 0.005(5) 0.013(5) -0.022(6) O2C 0.053(6) 0.045(6) 0.054(6) -0.007(5) 0.022(5) -0.013(5) N1C 0.028(4) 0.027(4) 0.040(4) -0.002(4) 0.016(4) -0.013(4) N3C 0.041(5) 0.026(5) 0.060(5) 0.013(5) 0.024(5) 0.005(4) N4C 0.048(7) 0.032(7) 0.066(8) -0.010(6) 0.020(7) -0.022(6) C4'C 0.031(6) 0.035(6) 0.058(6) -0.008(5) 0.012(5) -0.009(5) C2'C 0.039(7) 0.030(6) 0.051(6) -0.017(6) 0.008(6) -0.004(6) C1'C 0.034(5) 0.020(4) 0.056(5) -0.014(4) 0.011(5) -0.014(4) C2C 0.039(5) 0.026(5) 0.050(5) 0.002(5) 0.020(5) -0.002(5) C6C 0.039(5) 0.028(5) 0.033(5) 0.000(5) 0.017(5) -0.008(5) C5C 0.045(6) 0.029(6) 0.041(5) -0.001(5) 0.019(5) -0.004(5) C4C 0.039(6) 0.020(5) 0.047(5) 0.006(5) 0.014(5) -0.006(5) O1XA 0.083(9) 0.073(8) 0.040(6) -0.008(5) 0.028(6) -0.020(7) O1YA 0.069(7) 0.062(7) 0.021(4) 0.001(5) 0.001(5) -0.001(6) C1A' 0.062(7) 0.052(7) 0.025(5) -0.002(5) 0.003(6) -0.011(6) C2A' 0.059(6) 0.047(6) 0.022(4) -0.007(4) 0.013(5) -0.010(5) C8A' 0.063(7) 0.062(7) 0.030(5) -0.009(5) 0.015(5) -0.019(6) C7A' 0.074(8) 0.059(7) 0.039(5) -0.004(6) 0.008(6) -0.010(6) C6A' 0.071(7) 0.057(7) 0.032(5) 0.007(6) 0.013(6) -0.009(6) C5A' 0.057(7) 0.049(6) 0.032(5) 0.013(5) 0.017(5) -0.005(6) C3A' 0.057(6) 0.045(6) 0.023(4) 0.005(4) 0.015(5) -0.003(5) C4A' 0.062(7) 0.054(7) 0.022(5) -0.007(5) 0.014(5) -0.004(6) O4YA 0.079(8) 0.091(8) 0.027(5) 0.006(5) 0.003(5) -0.025(7) O4XA 0.061(7) 0.064(7) 0.039(6) 0.002(5) -0.008(6) -0.014(6) O1XB 0.049(6) 0.049(6) 0.057(6) 0.006(5) 0.009(6) -0.037(5) O1YB 0.023(5) 0.044(5) 0.049(5) -0.011(5) -0.004(4) -0.004(4) C1B' 0.021(5) 0.021(5) 0.060(6) 0.008(5) 0.000(5) 0.001(5) C2B' 0.024(5) 0.010(4) 0.061(5) -0.001(5) 0.002(5) 0.003(4) C8B' 0.036(6) 0.034(6) 0.069(6) -0.008(6) -0.003(6) -0.004(5) C7B' 0.046(6) 0.037(6) 0.052(6) -0.016(5) 0.002(6) -0.003(5) C6B' 0.035(6) 0.026(5) 0.054(6) -0.009(5) -0.004(6) -0.001(5) C5B' 0.020(5) 0.017(5) 0.071(6) -0.003(5) -0.004(5) 0.001(4) C3B' 0.019(5) 0.010(4) 0.069(5) -0.001(4) 0.005(5) 0.009(4) C4B' 0.022(5) 0.020(5) 0.074(7) 0.000(6) 0.011(6) 0.001(5) O4YB 0.034(6) 0.051(7) 0.073(7) 0.015(6) 0.015(6) -0.018(5) O4XB 0.049(7) 0.053(7) 0.077(7) 0.000(6) 0.016(6) -0.018(6) O1XC 0.099(9) 0.058(7) 0.116(9) 0.052(7) 0.049(8) 0.015(7) O1YC 0.111(10) 0.080(8) 0.069(7) -0.005(7) 0.045(8) 0.019(8) C1C' 0.089(8) 0.053(7) 0.049(6) 0.005(6) 0.011(6) 0.017(7) C2C' 0.076(7) 0.053(6) 0.040(5) 0.000(5) 0.010(5) 0.018(6) C8C' 0.095(8) 0.060(7) 0.056(7) -0.007(6) -0.001(7) 0.017(7) C7C' 0.099(9) 0.075(8) 0.080(8) -0.015(7) 0.002(7) 0.017(8) C6C' 0.096(9) 0.079(8) 0.085(8) -0.009(7) 0.026(7) 0.015(8) C5C' 0.091(8) 0.074(7) 0.072(7) -0.004(7) 0.029(7) 0.004(7) C3C' 0.085(7) 0.056(6) 0.037(5) 0.005(5) 0.017(5) 0.012(6) C4C' 0.089(8) 0.066(8) 0.049(7) 0.000(6) 0.010(7) 0.004(7) O4YC 0.129(10) 0.062(8) 0.085(8) -0.002(6) 0.059(8) 0.011(8) O4XC 0.079(8) 0.069(8) 0.093(8) 0.028(7) 0.003(7) -0.005(7) O4XD 0.108(10) 0.084(9) 0.059(7) -0.020(7) 0.034(7) 0.004(8) O4YD 0.148(12) 0.072(9) 0.123(11) -0.022(8) 0.054(10) -0.018(9) C4D' 0.089(9) 0.067(8) 0.048(7) 0.014(7) 0.016(7) 0.009(8) C3D' 0.076(7) 0.076(7) 0.037(5) 0.019(6) 0.006(5) 0.011(7) C5D' 0.078(8) 0.100(8) 0.062(6) 0.014(7) 0.009(7) 0.004(8) C6D' 0.089(9) 0.084(8) 0.064(7) 0.014(7) 0.009(7) -0.003(8) C7D' 0.088(9) 0.081(8) 0.064(7) 0.016(7) -0.004(7) -0.006(7) C8D' 0.083(8) 0.072(8) 0.048(6) 0.007(6) -0.002(6) 0.011(7) C2D' 0.073(7) 0.078(7) 0.025(5) 0.009(5) 0.005(5) 0.012(6) C1D' 0.077(8) 0.089(8) 0.037(6) 0.000(7) 0.013(6) 0.021(8) O1YD 0.109(10) 0.090(9) 0.069(7) 0.041(7) 0.041(8) 0.013(8) O1XD 0.131(11) 0.110(10) 0.063(7) -0.042(7) 0.030(8) 0.000(9) O1W 0.093(10) 0.078(9) 0.057(6) -0.023(6) 0.031(7) -0.004(7) O2W 0.145(16) 0.100(13) 0.138(13) -0.013(10) -0.071(12) -0.005(12) C5'C 0.040(7) 0.068(8) 0.074(7) -0.007(7) 0.016(6) -0.007(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 S3'D C4'D 1.776(16) . ? S3'D C2'D 1.851(13) . ? O1'D C4'D 1.416(17) . ? O1'D C1'D 1.445(18) . ? O5'D C5'D 1.53(2) . ? O5'D H5'D 0.84 . ? O2D C2D 1.270(14) . ? N1D C2D 1.371(17) . ? N1D C6D 1.411(16) . ? N1D C1'D 1.496(18) . ? N3D C2D 1.309(18) . ? N3D C4D 1.421(16) . ? N3D H3D 0.88 . ? N4D C4D 1.31(2) . ? N4D H4D1 0.88 . ? N4D H4D2 0.88 . ? C4'D C5'D 1.46(2) . ? C4'D H4'D 1 . ? C5'D H5'1 0.99 . ? C5'D H5'2 0.99 . ? C2'D C1'D 1.42(2) . ? C2'D H2'1 0.99 . ? C2'D H2'2 0.99 . ? C1'D H1'D 1 . ? C6D C5D 1.23(2) . ? C6D H6D 0.95 . ? C5D C4D 1.46(2) . ? C5D H5D 0.95 . ? S3'B C2'B 1.773(14) . ? S3'B C4'B 1.849(15) . ? O1'B C1'B 1.414(16) . ? O1'B C4'B 1.521(15) . ? O5'B C5'B 1.359(17) . ? O5'B H5'B 0.84 . ? O2B C2B 1.152(15) . ? N1B C6B 1.360(16) . ? N1B C2B 1.389(16) . ? N1B C1'B 1.466(16) . ? N3B C4B 1.297(16) . ? N3B C2B 1.412(16) . ? N3B H3B 0.88 . ? N4B C4B 1.256(16) . ? N4B H4B1 0.88 . ? N4B H4B2 0.88 . ? C4'B C5'B 1.41(2) . ? C4'B H4'B 1 . ? C5'B H5'3 0.99 . ? C5'B H5'4 0.99 . ? C2'B C1'B 1.624(18) . ? C2'B H2'3 0.99 . ? C2'B H2'4 0.99 . ? C1'B H1'B 1 . ? C6B C5B 1.430(18) . ? C6B H6B 0.95 . ? C5B C4B 1.416(18) . ? C5B H5B 0.95 . ? S3'A C2'A 1.834(14) . ? S3'A C4'A 1.875(16) . ? O1'A C1'A 1.388(17) . ? O1'A C4'A 1.439(17) . ? O5'A C5'A 1.413(17) . ? O5'A H5'A 0.84 . ? O2A C2A 1.202(16) . ? N1A C6A 1.315(16) . ? N1A C2A 1.408(18) . ? N1A C1'A 1.47(2) . ? N3A C2A 1.364(19) . ? N3A C4A 1.381(18) . ? N3A H3A 0.88 . ? N4A C4A 1.28(2) . ? N4A H4A1 0.88 . ? N4A H4A2 0.88 . ? C4'A C5'A 1.523(18) . ? C4'A H4'A 1 . ? C5'A H5'5 0.99 . ? C5'A H5'6 0.99 . ? C2'A C1'A 1.53(2) . ? C2'A H2'5 0.99 . ? C2'A H2'6 0.99 . ? C1'A H1'A 1 . ? C6A C5A 1.41(2) . ? C6A H6A 0.95 . ? C5A C4A 1.40(2) . ? C5A H5A 0.95 . ? S3'C C4'C 1.782(15) . ? S3'C C2'C 1.812(15) . ? O1'C C4'C 1.413(18) . ? O1'C C1'C 1.482(16) . ? O5'C C5'C 1.432(19) . ? O5'C H5'C 0.84 . ? O2C C2C 1.187(16) . ? N1C C6C 1.320(15) . ? N1C C2C 1.419(17) . ? N1C C1'C 1.525(16) . ? N3C C4C 1.312(18) . ? N3C C2C 1.385(19) . ? N3C H3C 0.88 . ? N4C C4C 1.334(18) . ? N4C H4C1 0.88 . ? N4C H4C2 0.88 . ? C4'C C5'C 1.49(2) . ? C4'C H4'C 1 . ? C2'C C1'C 1.469(19) . ? C2'C H2'7 0.99 . ? C2'C H2'8 0.99 . ? C1'C H1'C 1 . ? C6C C5C 1.333(18) . ? C6C H6C 0.95 . ? C5C C4C 1.431(18) . ? C5C H5C 0.95 . ? O1XA C1A' 1.234(17) . ? O1YA C1A' 1.334(15) . ? C1A' C2A' 1.516(11) . ? C2A' C3A' 1.402(11) . ? C2A' C8A' 1.424(11) . ? C8A' C7A' 1.360(11) . ? C8A' H8A' 0.95 . ? C7A' C6A' 1.384(13) . ? C7A' H7A' 0.95 . ? C6A' C5A' 1.353(11) . ? C6A' H6A' 0.95 . ? C5A' C3A' 1.422(10) . ? C5A' H5A' 0.95 . ? C3A' C4A' 1.487(11) . ? C4A' O4XA 1.254(17) . ? C4A' O4YA 1.365(15) . ? O4YA H4YA 0.84 . ? O1XB C1B' 1.213(16) . ? O1YB C1B' 1.289(15) . ? C1B' C2B' 1.502(11) . ? C2B' C8B' 1.371(11) . ? C2B' C3B' 1.415(11) . ? C8B' C7B' 1.369(11) . ? C8B' H8B' 0.95 . ? C7B' C6B' 1.403(12) . ? C7B' H7B' 0.95 . ? C6B' C5B' 1.362(11) . ? C6B' H6B' 0.95 . ? C5B' C3B' 1.407(11) . ? C5B' H5B' 0.95 . ? C3B' C4B' 1.504(11) . ? C4B' O4XB 1.241(16) . ? C4B' O4YB 1.277(16) . ? O4YB H4YB 0.84 . ? O1XC C1C' 1.255(18) . ? O1YC C1C' 1.315(18) . ? O1YC H1YC 0.84 . ? C1C' C2C' 1.519(12) . ? C2C' C8C' 1.385(12) . ? C2C' C3C' 1.421(12) . ? C8C' C7C' 1.373(13) . ? C8C' H8C' 0.95 . ? C7C' C6C' 1.394(14) . ? C7C' H7C' 0.95 . ? C6C' C5C' 1.373(12) . ? C6C' H6C' 0.95 . ? C5C' C3C' 1.412(12) . ? C5C' H5C' 0.95 . ? C3C' C4C' 1.489(12) . ? C4C' O4YC 1.214(19) . ? C4C' O4XC 1.34(2) . ? O4XD C4D' 1.175(19) . ? O4YD C4D' 1.34(2) . ? O4YD H4YD 0.84 . ? C4D' C3D' 1.500(12) . ? C3D' C5D' 1.388(12) . ? C3D' C2D' 1.413(12) . ? C5D' C6D' 1.379(13) . ? C5D' H5D' 0.95 . ? C6D' C7D' 1.418(14) . ? C6D' H6D' 0.95 . ? C7D' C8D' 1.359(12) . ? C7D' H7D' 0.95 . ? C8D' C2D' 1.385(12) . ? C8D' H8D' 0.95 . ? C2D' C1D' 1.519(12) . ? C1D' O1XD 1.208(19) . ? C1D' O1YD 1.26(2) . ? O1W H11W 0.8584 . ? O1W H21W 0.8617 . ? O2W H12W 0.8641 . ? O2W H22W 0.8554 . ? C5'C H5'7 0.99 . ? C5'C H5'8 0.99 . ? 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 C4'D S3'D C2'D 83.4(8) . . ? C4'D O1'D C1'D 111.5(11) . . ? C5'D O5'D H5'D 109.5 . . ? C2D N1D C6D 117.7(13) . . ? C2D N1D C1'D 116.1(10) . . ? C6D N1D C1'D 126.1(12) . . ? C2D N3D C4D 127.0(12) . . ? C2D N3D H3D 116.5 . . ? C4D N3D H3D 116.5 . . ? C4D N4D H4D1 120 . . ? C4D N4D H4D2 120 . . ? H4D1 N4D H4D2 120 . . ? O1'D C4'D C5'D 110.1(13) . . ? O1'D C4'D S3'D 108.8(10) . . ? C5'D C4'D S3'D 114.4(11) . . ? O1'D C4'D H4'D 107.8 . . ? C5'D C4'D H4'D 107.8 . . ? S3'D C4'D H4'D 107.8 . . ? C4'D C5'D O5'D 109.1(14) . . ? C4'D C5'D H5'1 109.9 . . ? O5'D C5'D H5'1 109.8 . . ? C4'D C5'D H5'2 109.9 . . ? O5'D C5'D H5'2 109.8 . . ? H5'1 C5'D H5'2 108.3 . . ? C1'D C2'D S3'D 105.4(10) . . ? C1'D C2'D H2'1 110.7 . . ? S3'D C2'D H2'1 110.7 . . ? C1'D C2'D H2'2 110.6 . . ? S3'D C2'D H2'2 110.6 . . ? H2'1 C2'D H2'2 108.8 . . ? C2'D C1'D O1'D 108.0(13) . . ? C2'D C1'D N1D 113.3(14) . . ? O1'D C1'D N1D 106.9(10) . . ? C2'D C1'D H1'D 109.6 . . ? O1'D C1'D H1'D 109.5 . . ? N1D C1'D H1'D 109.5 . . ? O2D C2D N3D 121.2(13) . . ? O2D C2D N1D 121.0(14) . . ? N3D C2D N1D 117.8(11) . . ? C5D C6D N1D 123.8(14) . . ? C5D C6D H6D 118.1 . . ? N1D C6D H6D 118.1 . . ? C6D C5D C4D 122.5(13) . . ? C6D C5D H5D 118.7 . . ? C4D C5D H5D 118.7 . . ? N4D C4D N3D 120.6(13) . . ? N4D C4D C5D 129.1(13) . . ? N3D C4D C5D 110.3(13) . . ? C2'B S3'B C4'B 91.7(7) . . ? C1'B O1'B C4'B 115.3(9) . . ? C5'B O5'B H5'B 109.4 . . ? C6B N1B C2B 123.2(11) . . ? C6B N1B C1'B 121.2(11) . . ? C2B N1B C1'B 115.2(10) . . ? C4B N3B C2B 125.7(12) . . ? C4B N3B H3B 117.2 . . ? C2B N3B H3B 117.2 . . ? C4B N4B H4B1 120 . . ? C4B N4B H4B2 120 . . ? H4B1 N4B H4B2 120 . . ? C5'B C4'B O1'B 111.3(12) . . ? C5'B C4'B S3'B 114.5(11) . . ? O1'B C4'B S3'B 103.0(8) . . ? C5'B C4'B H4'B 109.3 . . ? O1'B C4'B H4'B 109.3 . . ? S3'B C4'B H4'B 109.3 . . ? O5'B C5'B C4'B 114.3(13) . . ? O5'B C5'B H5'3 108.7 . . ? C4'B C5'B H5'3 108.7 . . ? O5'B C5'B H5'4 108.7 . . ? C4'B C5'B H5'4 108.7 . . ? H5'3 C5'B H5'4 107.6 . . ? C1'B C2'B S3'B 102.2(9) . . ? C1'B C2'B H2'3 111.3 . . ? S3'B C2'B H2'3 111.3 . . ? C1'B C2'B H2'4 111.3 . . ? S3'B C2'B H2'4 111.3 . . ? H2'3 C2'B H2'4 109.2 . . ? O1'B C1'B N1B 108.7(10) . . ? O1'B C1'B C2'B 108.6(10) . . ? N1B C1'B C2'B 111.1(11) . . ? O1'B C1'B H1'B 109.4 . . ? N1B C1'B H1'B 109.5 . . ? C2'B C1'B H1'B 109.4 . . ? O2B C2B N1B 121.0(13) . . ? O2B C2B N3B 125.4(13) . . ? N1B C2B N3B 113.5(11) . . ? N1B C6B C5B 121.1(13) . . ? N1B C6B H6B 119.4 . . ? C5B C6B H6B 119.5 . . ? C4B C5B C6B 114.9(12) . . ? C4B C5B H5B 122.5 . . ? C6B C5B H5B 122.5 . . ? N4B C4B N3B 119.3(13) . . ? N4B C4B C5B 119.2(13) . . ? N3B C4B C5B 121.5(12) . . ? C2'A S3'A C4'A 88.1(7) . . ? C1'A O1'A C4'A 115.1(11) . . ? C5'A O5'A H5'A 109.4 . . ? C6A N1A C2A 120.8(14) . . ? C6A N1A C1'A 121.9(12) . . ? C2A N1A C1'A 116.5(12) . . ? C2A N3A C4A 121.6(13) . . ? C2A N3A H3A 119.2 . . ? C4A N3A H3A 119.2 . . ? C4A N4A H4A1 120 . . ? C4A N4A H4A2 120 . . ? H4A1 N4A H4A2 120 . . ? O1'A C4'A C5'A 112.6(12) . . ? O1'A C4'A S3'A 102.4(9) . . ? C5'A C4'A S3'A 112.1(11) . . ? O1'A C4'A H4'A 109.8 . . ? C5'A C4'A H4'A 109.9 . . ? S3'A C4'A H4'A 109.8 . . ? O5'A C5'A C4'A 111.8(12) . . ? O5'A C5'A H5'5 109.3 . . ? C4'A C5'A H5'5 109.2 . . ? O5'A C5'A H5'6 109.3 . . ? C4'A C5'A H5'6 109.3 . . ? H5'5 C5'A H5'6 107.9 . . ? C1'A C2'A S3'A 100.1(9) . . ? C1'A C2'A H2'5 111.8 . . ? S3'A C2'A H2'5 111.7 . . ? C1'A C2'A H2'6 111.8 . . ? S3'A C2'A H2'6 111.7 . . ? H2'5 C2'A H2'6 109.5 . . ? O1'A C1'A N1A 103.8(11) . . ? O1'A C1'A C2'A 112.0(13) . . ? N1A C1'A C2'A 114.2(13) . . ? O1'A C1'A H1'A 108.9 . . ? N1A C1'A H1'A 108.9 . . ? C2'A C1'A H1'A 108.9 . . ? O2A C2A N3A 118.1(15) . . ? O2A C2A N1A 122.1(16) . . ? N3A C2A N1A 119.6(12) . . ? N1A C6A C5A 119.3(13) . . ? N1A C6A H6A 120.3 . . ? C5A C6A H6A 120.4 . . ? C4A C5A C6A 121.4(13) . . ? C4A C5A H5A 119.3 . . ? C6A C5A H5A 119.3 . . ? N4A C4A N3A 117.9(14) . . ? N4A C4A C5A 125.3(13) . . ? N3A C4A C5A 116.6(15) . . ? C4'C S3'C C2'C 86.0(7) . . ? C4'C O1'C C1'C 110.6(10) . . ? C5'C O5'C H5'C 109.5 . . ? C6C N1C C2C 123.5(12) . . ? C6C N1C C1'C 124.8(10) . . ? C2C N1C C1'C 111.7(11) . . ? C4C N3C C2C 129.2(12) . . ? C4C N3C H3C 115.4 . . ? C2C N3C H3C 115.4 . . ? C4C N4C H4C1 120 . . ? C4C N4C H4C2 120 . . ? H4C1 N4C H4C2 120 . . ? O1'C C4'C C5'C 108.3(12) . . ? O1'C C4'C S3'C 111.2(9) . . ? C5'C C4'C S3'C 116.1(12) . . ? O1'C C4'C H4'C 107 . . ? C5'C C4'C H4'C 106.9 . . ? S3'C C4'C H4'C 106.9 . . ? C1'C C2'C S3'C 106.5(9) . . ? C1'C C2'C H2'7 110.4 . . ? S3'C C2'C H2'7 110.4 . . ? C1'C C2'C H2'8 110.4 . . ? S3'C C2'C H2'8 110.4 . . ? H2'7 C2'C H2'8 108.6 . . ? C2'C C1'C O1'C 108.0(11) . . ? C2'C C1'C N1C 109.6(11) . . ? O1'C C1'C N1C 108.3(10) . . ? C2'C C1'C H1'C 110.3 . . ? O1'C C1'C H1'C 110.3 . . ? N1C C1'C H1'C 110.3 . . ? O2C C2C N3C 126.8(14) . . ? O2C C2C N1C 123.6(14) . . ? N3C C2C N1C 109.4(12) . . ? N1C C6C C5C 124.7(12) . . ? N1C C6C H6C 117.7 . . ? C5C C6C H6C 117.6 . . ? C6C C5C C4C 115.3(12) . . ? C6C C5C H5C 122.3 . . ? C4C C5C H5C 122.4 . . ? N3C C4C N4C 120.4(13) . . ? N3C C4C C5C 117.9(13) . . ? N4C C4C C5C 121.6(13) . . ? O1XA C1A' O1YA 121.2(11) . . ? O1XA C1A' C2A' 121.7(11) . . ? O1YA C1A' C2A' 116.6(11) . . ? C3A' C2A' C8A' 117.2(9) . . ? C3A' C2A' C1A' 130.4(9) . . ? C8A' C2A' C1A' 112.2(9) . . ? C7A' C8A' C2A' 122.4(11) . . ? C7A' C8A' H8A' 118.8 . . ? C2A' C8A' H8A' 118.8 . . ? C8A' C7A' C6A' 120.5(11) . . ? C8A' C7A' H7A' 119.8 . . ? C6A' C7A' H7A' 119.7 . . ? C5A' C6A' C7A' 117.8(11) . . ? C5A' C6A' H6A' 121.1 . . ? C7A' C6A' H6A' 121.1 . . ? C6A' C5A' C3A' 124.1(10) . . ? C6A' C5A' H5A' 118 . . ? C3A' C5A' H5A' 118 . . ? C2A' C3A' C5A' 117.3(9) . . ? C2A' C3A' C4A' 130.5(9) . . ? C5A' C3A' C4A' 112.3(10) . . ? O4XA C4A' O4YA 119.5(11) . . ? O4XA C4A' C3A' 121.2(11) . . ? O4YA C4A' C3A' 118.7(11) . . ? C4A' O4YA H4YA 109.5 . . ? O1XB C1B' O1YB 121.6(11) . . ? O1XB C1B' C2B' 118.1(12) . . ? O1YB C1B' C2B' 120.2(10) . . ? C8B' C2B' C3B' 118.7(9) . . ? C8B' C2B' C1B' 113.1(9) . . ? C3B' C2B' C1B' 128.1(10) . . ? C7B' C8B' C2B' 123.2(11) . . ? C7B' C8B' H8B' 118.4 . . ? C2B' C8B' H8B' 118.4 . . ? C8B' C7B' C6B' 118.4(11) . . ? C8B' C7B' H7B' 120.8 . . ? C6B' C7B' H7B' 120.8 . . ? C5B' C6B' C7B' 119.6(10) . . ? C5B' C6B' H6B' 120.2 . . ? C7B' C6B' H6B' 120.2 . . ? C6B' C5B' C3B' 122.2(10) . . ? C6B' C5B' H5B' 118.9 . . ? C3B' C5B' H5B' 118.9 . . ? C5B' C3B' C2B' 117.7(9) . . ? C5B' C3B' C4B' 113.9(10) . . ? C2B' C3B' C4B' 128.4(10) . . ? O4XB C4B' O4YB 119.1(11) . . ? O4XB C4B' C3B' 117.8(12) . . ? O4YB C4B' C3B' 123.1(11) . . ? C4B' O4YB H4YB 109.5 . . ? C1C' O1YC H1YC 109.4 . . ? O1XC C1C' O1YC 124.2(13) . . ? O1XC C1C' C2C' 117.7(13) . . ? O1YC C1C' C2C' 118.1(12) . . ? C8C' C2C' C3C' 119.7(10) . . ? C8C' C2C' C1C' 113.1(11) . . ? C3C' C2C' C1C' 127.0(10) . . ? C7C' C8C' C2C' 121.0(12) . . ? C7C' C8C' H8C' 119.5 . . ? C2C' C8C' H8C' 119.5 . . ? C8C' C7C' C6C' 120.1(13) . . ? C8C' C7C' H7C' 120 . . ? C6C' C7C' H7C' 119.9 . . ? C5C' C6C' C7C' 119.6(13) . . ? C5C' C6C' H6C' 120.2 . . ? C7C' C6C' H6C' 120.2 . . ? C6C' C5C' C3C' 121.4(12) . . ? C6C' C5C' H5C' 119.3 . . ? C3C' C5C' H5C' 119.3 . . ? C5C' C3C' C2C' 117.7(10) . . ? C5C' C3C' C4C' 115.5(11) . . ? C2C' C3C' C4C' 126.4(11) . . ? O4YC C4C' O4XC 118.8(14) . . ? O4YC C4C' C3C' 126.9(15) . . ? O4XC C4C' C3C' 114.3(14) . . ? C4D' O4YD H4YD 109.5 . . ? O4XD C4D' O4YD 122.8(15) . . ? O4XD C4D' C3D' 123.3(15) . . ? O4YD C4D' C3D' 113.8(14) . . ? C5D' C3D' C2D' 118.8(11) . . ? C5D' C3D' C4D' 111.2(11) . . ? C2D' C3D' C4D' 129.9(11) . . ? C6D' C5D' C3D' 124.7(13) . . ? C6D' C5D' H5D' 117.7 . . ? C3D' C5D' H5D' 117.7 . . ? C5D' C6D' C7D' 115.6(13) . . ? C5D' C6D' H6D' 122.2 . . ? C7D' C6D' H6D' 122.2 . . ? C8D' C7D' C6D' 119.7(13) . . ? C8D' C7D' H7D' 120.1 . . ? C6D' C7D' H7D' 120.1 . . ? C7D' C8D' C2D' 125.0(12) . . ? C7D' C8D' H8D' 117.5 . . ? C2D' C8D' H8D' 117.5 . . ? C8D' C2D' C3D' 115.9(10) . . ? C8D' C2D' C1D' 114.1(12) . . ? C3D' C2D' C1D' 129.6(12) . . ? O1XD C1D' O1YD 118.8(14) . . ? O1XD C1D' C2D' 121.0(16) . . ? O1YD C1D' C2D' 120.2(14) . . ? H11W O1W H21W 108.4 . . ? H12W O2W H22W 108.3 . . ? O5'C C5'C C4'C 116.1(13) . . ? O5'C C5'C H5'7 108.3 . . ? C4'C C5'C H5'7 108.3 . . ? O5'C C5'C H5'8 108.2 . . ? C4'C C5'C H5'8 108.2 . . ? H5'7 C5'C H5'8 107.4 . . ? _vrf_PLAT_213_CCDC912146 ; RESPONSE: This error message appears because the presence of disorder involving this atom and neighbors. In spite of this, we used the classical harmonic model based upon a development of ADPs with just one site instead of the split position model. It is important to comment that trial refinements were used with the split-atom approach. However, since the extra disordered sites are very close together, high correlation and unstable refinements were observed applying the classical split-atom approach to the structural model. From a statistical point of view, the one-site model was better than the split-atom one. The former model also converges easier, which is probably due to lower correlations between the refined ADP and occupancy parameters. ; _vrf_SHFSU_01_PLAT_080_CCDC912146 ; RESPONSE: Even after 50 refinement cycles the proper convergence had not yet been achieved, which has been caused by disorder on atoms group. In attempt to get a better convergence of the refinement, we have used the split position model, but this was unsuccessful. The classical harmonic model based upon a development of ADPs with just one site did converge better than that splitting each atom into two occupancy sites due to high correlations between the refined ADPs and occupancy parameters. ; _vrf_PLAT_340_CCDC912146 ; RESPONSE: This error message appears because precision on atom positions are affected by disorder involving several atoms in the structure. ; _vrf_PLAT_420_CCDC912146 ; RESPONSE: This error message appears because these OH water moieties are only involved in weak contacts instead of classical hydrogen bonding donors. Concerning the position assignment of these water hydrogens, the electronic density peak regarding these atoms was first found from the difference Fourier map so that their position was fixed. Therefore, there is no problem of assigning their position. ; # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF _database_code_depnum_ccdc_archive 'CCDC 912146'