# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 207 loop_ _publ_author_name 'Matsuda, Akira' 'Endo, Kanji' 'Kaga, Daisuke' 'Yuka Kato' 'Minakawa, Noriaki' 'Sasaki, Takuma' 'Tanaka, Motohiro' _publ_contact_author_name 'Dr Akira Matsuda ' _publ_contact_author_address ; Graduate School of Pharmaceutical Sciences Hokkaido University, Kita-12 Nishi-6, Kita-ku Sapporo 060-0012 Japan ; _publ_contact_author_email ' matuda@pharm.hokudai.ac.jp ' _publ_contact_author_fax ' +81-11-706-4980' _publ_contact_author_phone ' +81-11-706-3228' _publ_contact_letter ; ? ; _publ_requested_journal ' J. Chem. Soc., Perkin Trans. 1' _publ_section_title ; Synthesis and Structural Elucidation of 1-(3-C-Ethynyl-4-thio-beta-D-ribofuranosyl)cytosine(4'-thioECyd) ; _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; #------------------------------------------------------------------------------ data_12139-H0071-038 _database_code_CSD 186372 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C11 H13 N3 O5 ' _chemical_formula_moiety 'C11 H13 N3 O5 ' _chemical_formula_weight 267.24 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 10.657(4) _cell_length_b 10.894(3) _cell_length_c 10.362(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1202.9(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 15.0 _cell_measurement_theta_max 20.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prisms' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.300 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.012 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.668 _exptl_absorpt_correction_T_max 0.738 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K¥a' _diffrn_radiation_wavelength 1.5418 _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method ¥w-2¥q _diffrn_reflns_number 2273 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_theta_max 65.07 _diffrn_measured_fraction_theta_max 1.8663 _diffrn_reflns_theta_full 65.07 _diffrn_measured_fraction_theta_full 1.8663 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.69 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 4.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 4.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2249 _reflns_number_gt 2151 _reflns_threshold_expression F^2^>4.0¥s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.0816 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2151 _refine_ls_number_parameters 174 _refine_ls_goodness_of_fit_ref 1.948 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w == 1/[¥s^2^(Fo) + 0.00152|Fo|^2^]' _refine_ls_shift/su_max 0.0004 _refine_diff_density_max 0.15 _refine_diff_density_min -0.18 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.78(3) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack -0.1(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.018 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.031 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(2) O 0.4694(1) 0.2070(1) 0.2422(1) 0.0437(4) Uani 1.00 d . . . O(4') O 0.4635(1) 0.3417(1) -0.1102(1) 0.0354(3) Uani 1.00 d . . . O(2') O 0.6311(1) 0.4642(1) 0.1601(1) 0.0354(3) Uani 1.00 d . . . O(3') O 0.4624(1) 0.5995(1) 0.0092(1) 0.0350(3) Uani 1.00 d . . . O(5') O 0.6866(1) 0.3717(1) -0.2553(1) 0.0432(4) Uani 1.00 d . . . N(1) N 0.5547(1) 0.2099(1) 0.0406(1) 0.0301(4) Uani 1.00 d . . . N(3) N 0.5718(1) 0.0363(2) 0.1776(1) 0.0328(4) Uani 1.00 d . . . N(4) N 0.6919(2) -0.1275(2) 0.1190(2) 0.0432(5) Uani 1.00 d . . . C(2) C 0.5296(2) 0.1518(2) 0.1571(2) 0.0308(4) Uani 1.00 d . . . C(4) C 0.6491(2) -0.0162(2) 0.0939(2) 0.0317(4) Uani 1.00 d . . . C(5) C 0.6843(2) 0.0460(2) -0.0250(2) 0.0337(4) Uani 1.00 d . . . C(6) C 0.6344(2) 0.1564(2) -0.0452(2) 0.0324(4) Uani 1.00 d . . . C(1') C 0.5073(2) 0.3335(2) 0.0177(2) 0.0286(4) Uani 1.00 d . . . C(2') C 0.6095(2) 0.4303(2) 0.0315(2) 0.0268(4) Uani 1.00 d . . . C(3') C 0.5594(2) 0.5341(2) -0.0569(2) 0.0299(4) Uani 1.00 d . . . C(4') C 0.4962(2) 0.4594(2) -0.1660(2) 0.0335(4) Uani 1.00 d . . . C(5') C 0.5735(2) 0.4360(2) -0.2857(2) 0.0371(5) Uani 1.00 d . . . C(6') C 0.6588(2) 0.6178(2) -0.0988(2) 0.0431(6) Uani 1.00 d . . . C(7') C 0.7418(3) 0.6810(3) -0.1306(3) 0.0744(9) Uani 1.00 d . . . H(1) H 0.6484 -0.1792 0.1910 0.0449 Uiso 1.00 calc . . . H(2) H 0.7456 -0.1743 0.0586 0.0449 Uiso 1.00 calc . . . H(3) H 0.7401 0.0096 -0.0853 0.0404 Uiso 1.00 calc . . . H(4) H 0.6552 0.1993 -0.1221 0.0388 Uiso 1.00 calc . . . H(5) H 0.4324 0.3557 0.0949 0.0449 Uiso 1.00 calc . . . H(6) H 0.7003 0.3863 -0.0120 0.0449 Uiso 1.00 calc . . . H(7) H 0.5590 0.4741 0.2130 0.0449 Uiso 1.00 calc . . . H(8) H 0.4982 0.6585 0.0607 0.0449 Uiso 1.00 calc . . . H(9) H 0.8093 0.7325 -0.1565 0.0893 Uiso 1.00 calc . . . H(10) H 0.4008 0.5302 -0.1833 0.0449 Uiso 1.00 calc . . . H(11) H 0.5942 0.5124 -0.3244 0.0445 Uiso 1.00 calc . . . H(12) H 0.5256 0.3883 -0.3445 0.0445 Uiso 1.00 calc . . . H(13) H 0.7563 0.4279 -0.2851 0.0449 Uiso 1.00 calc . . . 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 O(2) 0.0548(9) 0.0401(7) 0.0362(7) 0.0120(7) 0.0216(6) 0.0023(6) O(4') 0.0354(7) 0.0395(7) 0.0313(6) -0.0054(6) -0.0085(5) 0.0000(6) O(2') 0.0349(7) 0.0443(8) 0.0271(6) -0.0012(7) -0.0052(5) -0.0060(6) O(3') 0.0333(7) 0.0374(7) 0.0344(6) 0.0082(6) 0.0021(5) -0.0034(5) O(5') 0.0379(7) 0.0467(8) 0.0450(8) 0.0018(6) 0.0087(6) 0.0050(7) N(1) 0.0321(8) 0.0302(8) 0.0279(7) -0.0005(6) 0.0016(6) -0.0006(6) N(3) 0.0382(9) 0.0288(7) 0.0313(8) -0.0011(6) 0.0085(6) 0.0004(6) N(4) 0.050(1) 0.0338(8) 0.0458(10) 0.0067(8) 0.0159(8) 0.0040(7) C(2) 0.0311(9) 0.0330(9) 0.0282(8) -0.0021(8) 0.0056(7) -0.0037(7) C(4) 0.0309(9) 0.0290(8) 0.0351(9) -0.0060(7) 0.0006(8) -0.0007(7) C(5) 0.0333(9) 0.0362(9) 0.0315(8) 0.0006(8) 0.0077(8) -0.0031(8) C(6) 0.0357(9) 0.0356(9) 0.0258(8) -0.0042(8) 0.0064(7) -0.0010(7) C(1') 0.0263(8) 0.0318(9) 0.0276(8) -0.0024(7) 0.0038(7) 0.0024(7) C(2') 0.0223(8) 0.0312(9) 0.0268(8) 0.0015(7) -0.0021(7) -0.0036(7) C(3') 0.0279(8) 0.0318(9) 0.0300(9) 0.0032(7) 0.0051(6) 0.0016(7) C(4') 0.0328(10) 0.0414(10) 0.0263(8) 0.0030(8) 0.0006(6) 0.0013(7) C(5') 0.0398(10) 0.044(1) 0.0276(8) 0.0014(8) 0.0012(7) 0.0014(8) C(6') 0.052(1) 0.038(1) 0.039(1) -0.0029(8) 0.0151(10) -0.0019(9) C(7') 0.092(2) 0.064(2) 0.068(1) -0.048(2) 0.043(2) -0.025(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(2) C(2) 1.246(3) . . yes O(4') C(1') 1.408(3) . . yes O(4') C(4') 1.449(3) . . yes O(2') C(2') 1.401(3) . . yes O(2') H(7) 0.949 . . no O(3') C(3') 1.430(3) . . yes O(3') H(8) 0.919 . . no O(5') C(5') 1.429(3) . . yes O(5') H(13) 1.012 . . no N(1) C(2) 1.388(3) . . yes N(1) C(6) 1.361(3) . . yes N(1) C(1') 1.458(3) . . yes N(3) C(2) 1.353(4) . . yes N(3) C(4) 1.326(3) . . yes N(4) C(4) 1.321(4) . . yes N(4) H(1) 1.044 . . no N(4) H(2) 0.989 . . no C(4) C(5) 1.455(3) . . yes C(5) C(6) 1.331(4) . . yes C(5) H(3) 0.950 . . no C(6) H(4) 0.950 . . no C(1') C(2') 1.523(3) . . yes C(1') H(5) 1.156 . . no C(2') C(3') 1.551(3) . . yes C(2') H(6) 1.169 . . no C(2') C(4') 1.547(4) . . yes C(3') C(6') 1.464(4) . . yes C(4') C(5') 1.510(3) . . yes C(4') H(10) 1.289 . . no C(4') H(11) 0.950 . . no C(4') H(12) 0.950 . . no C(6') C(7') 1.168(4) . . yes C(7') H(9) 0.950 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1') O(4') C(4') 110.7(2) . . . yes C(2') O(2') H(7) 116.5 . . . no C(3') O(3') H(8) 109.1 . . . no C(5') O(5') H(13) 104.8 . . . no C(2) N(1) C(6) 119.5(2) . . . yes C(2) N(1) C(1') 119.7(2) . . . yes C(6) N(1) C(1') 120.4(2) . . . yes C(2) N(3) C(4) 120.3(2) . . . yes C(4) N(4) H(1) 118.8 . . . no C(4) N(4) H(2) 123.3 . . . no H(1) N(4) H(2) 115.5 . . . no O(2) C(2) N(1) 119.6(2) . . . yes O(2) C(2) N(3) 120.6(2) . . . yes N(1) C(2) N(3) 119.8(2) . . . yes N(3) C(4) N(4) 118.8(2) . . . yes N(3) C(4) C(5) 120.9(2) . . . yes N(4) C(4) C(5) 120.3(2) . . . yes C(4) C(5) C(6) 116.8(2) . . . yes C(4) C(5) H(3) 121.6 . . . no C(6) C(5) H(3) 121.6 . . . no N(1) C(6) C(5) 122.2(2) . . . yes N(1) C(6) H(4) 118.9 . . . no C(5) C(6) H(4) 118.9 . . . no O(4') C(1') N(1) 109.1(2) . . . yes O(4') C(1') C(2') 106.3(2) . . . yes O(4') C(1') H(5) 114.1 . . . no N(1) C(1') C(2') 112.1(2) . . . yes N(1) C(1') H(5) 108.7 . . . no C(2') C(1') H(5) 106.5 . . . no O(2') C(2') C(1') 112.9(2) . . . yes O(2') C(2') C(3') 115.2(2) . . . yes O(2') C(2') H(6) 109.8 . . . no C(1') C(2') C(3') 101.7(2) . . . yes C(1') C(2') H(6) 105.7 . . . no C(3') C(2') H(6) 110.9 . . . no O(3') C(3') C(2') 109.2(2) . . . yes O(3') C(3') C(4') 107.3(2) . . . yes O(3') C(3') C(6') 110.8(2) . . . yes C(2') C(3') C(4') 101.4(2) . . . yes C(2') C(3') C(6') 112.3(2) . . . yes C(4') C(3') C(6') 115.2(2) . . . yes O(4') C(4') C(3') 106.1(2) . . . yes O(4') C(4') C(5') 108.1(2) . . . yes O(4') C(4') H(10) 113.3 . . . no C(3') C(4') C(5') 116.8(2) . . . yes C(3') C(4') H(10) 97.5 . . . no C(5') C(4') H(10) 114.7 . . . no O(5') C(5') C(4') 111.2(2) . . . yes O(5') C(5') H(11) 109.0 . . . no O(5') C(5') H(12) 109.1 . . . no C(4') C(5') H(11) 109.0 . . . no C(4') C(5') H(12) 109.0 . . . no H(11) C(5') H(12) 109.4 . . . no C(3') C(6') C(7') 177.2(4) . . . yes C(6') C(7') H(9) 180.0 . . . no #------------------------------------------------------------------------------ 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(2) C(2) N(1) C(6) 171.2(2) . . . . yes O(2) C(2) N(1) C(1') -1.7(3) . . . . yes O(2) C(2) N(3) C(4) -171.4(3) . . . . yes O(4') C(1') N(1) C(2) -139.2(2) . . . . yes O(4') C(1') N(1) C(6) 47.9(3) . . . . yes O(4') C(1') C(2') O(2') 158.5(2) . . . . yes O(4') C(1') C(2') C(3') 34.5(2) . . . . yes O(4') C(4') C(3') O(3') -89.5(2) . . . . yes O(4') C(4') C(3') C(2') 25.0(2) . . . . yes O(4') C(4') C(3') C(6') 146.6(2) . . . . yes O(4') C(4') C(5') O(5') -60.9(3) . . . . yes O(2') C(2') C(1') N(1) -82.3(3) . . . . yes O(2') C(2') C(3') O(3') -44.6(3) . . . . yes O(2') C(2') C(3') C(4') -157.6(2) . . . . yes O(2') C(2') C(3') C(6') 78.8(3) . . . . yes O(3') C(3') C(2') C(1') 77.9(2) . . . . yes O(3') C(3') C(4') C(5') 149.9(2) . . . . yes O(3') C(3') C(6') C(7') 137(6) . . . . yes O(5') C(5') C(4') C(3') 58.6(3) . . . . yes N(1) C(2) N(3) C(4) 8.0(4) . . . . yes N(1) C(6) C(5) C(4) 0.3(4) . . . . yes N(1) C(1') O(4') C(4') -140.6(2) . . . . yes N(1) C(1') C(2') C(3') 153.7(2) . . . . yes N(3) C(2) N(1) C(6) -8.2(3) . . . . yes N(3) C(2) N(1) C(1') 178.8(2) . . . . yes N(3) C(4) C(5) C(6) -0.5(4) . . . . yes N(4) C(4) N(3) C(2) 177.7(2) . . . . yes N(4) C(4) C(5) C(6) 178.0(3) . . . . yes C(2) N(1) C(6) C(5) 4.0(4) . . . . yes C(2) N(1) C(1') C(2') 103.3(2) . . . . yes C(2) N(3) C(4) C(5) -3.7(4) . . . . yes C(5) C(6) N(1) C(1') 176.9(2) . . . . yes C(6) N(1) C(1') C(2') -69.6(3) . . . . yes C(1') O(4') C(4') C(3') -4.0(3) . . . . yes C(1') O(4') C(4') C(5') 122.0(2) . . . . yes C(1') C(2') C(3') C(4') -35.2(2) . . . . yes C(1') C(2') C(3') C(6') -158.8(2) . . . . yes C(2') C(1') O(4') C(4') -19.5(3) . . . . yes C(2') C(3') C(4') C(5') -95.5(3) . . . . yes C(2') C(3') C(6') C(7') 15(6) . . . . yes C(4') C(3') C(6') C(7') -100(6) . . . . yes C(5') C(4') C(3') C(6') 26.0(4) . . . . yes C(5') C(4') C(3') C(6') 26.0(4) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(2) N(4) 2.876(3) . 4_655 ? O(2) O(3') 2.922(3) . 4_645 ? O(2) O(2') 3.028(3) . 4_645 ? O(2) O(5') 3.136(3) . 3_455 ? O(2) C(7') 3.563(4) . 2_665 ? O(4') C(5) 3.508(3) . 3_455 ? O(2') O(5') 2.783(3) . 2_665 ? O(2') N(3) 2.849(3) . 4_655 ? O(2') C(7') 3.007(4) . 2_665 ? O(2') C(2) 3.271(3) . 4_655 ? O(2') C(5') 3.378(4) . 2_665 ? O(2') C(6') 3.472(3) . 2_665 ? O(3') N(4) 3.188(3) . 3_455 ? O(3') N(3) 3.338(3) . 4_655 ? O(3') C(5) 3.365(3) . 3_455 ? O(3') C(2) 3.506(3) . 4_655 ? O(3') C(7') 3.582(4) . 3_465 ? O(5') N(4) 3.233(3) . 2_654 ? N(4 C(7') 3.365(4) . 1_545 ? N(4) C(6') 3.594(4) . 1_545 ? C(5) C(5') 3.582(4) . 4_644 ? #------------------------------------------------------------------------------ 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_site_distance_DH _geom_hbond_site_distance_HA _geom_hbond_site_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O(2') H(7) O(2) . . . 0.949 3.077 3.397(2) 101.600 no N(4) H(1) O(5') . . 2_655 1.044 2.793 3.233(2) 105.536 no #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_master_file_afc7r.xtl _database_code_CSD 186373 _audit_creation_date 'Tue May 14 16:27:17 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C11 H13 N3 O4 S ' _chemical_formula_moiety 'C11 H13 N3 O4 S ' _chemical_formula_weight 283.30 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 10.887(3) _cell_length_b 10.892(3) _cell_length_c 10.385(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1231.4(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.3 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.278 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K¥a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method ¥w-2¥q _diffrn_reflns_number 1655 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 1.0006 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.0006 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.16 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1637 _reflns_number_gt 1494 _reflns_threshold_expression F^2^>2.0¥s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0824 _refine_ls_wR_factor_ref 0.0440 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 1637 _refine_ls_number_parameters 226 _refine_ls_goodness_of_fit_ref 2.591 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w == 1/[¥s^2^(Fo^2^) + (0.00200(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.1604 _refine_diff_density_max 0.22 _refine_diff_density_min -0.19 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack -0.8(1) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S(4') S 0.43087(4) 0.33533(4) 0.35811(4) 0.0354(1) Uani 1.00 d . . . O(5') O 0.6927(1) 0.3755(1) 0.2432(1) 0.0415(4) Uani 1.00 d . . . O(2) O 0.4631(1) 0.19684(9) 0.7424(1) 0.0442(3) Uani 1.00 d . . . O(2') O 0.6273(1) 0.4499(1) 0.6540(1) 0.0336(3) Uani 1.00 d . . . O(3') O 0.4681(1) 0.5971(1) 0.5065(1) 0.0348(3) Uani 1.00 d . . . N(1) N 0.5490(1) 0.19905(10) 0.5417(1) 0.0270(3) Uani 1.00 d . . . N(3) N 0.5713(1) 0.0286(1) 0.6818(1) 0.0321(3) Uani 1.00 d . . . N(4) N 0.6971(2) -0.1311(1) 0.6282(2) 0.0448(5) Uani 1.00 d . . . C(2) C 0.5253(1) 0.1426(1) 0.6599(1) 0.0314(4) Uani 1.00 d . . . C(4) C 0.6485(1) -0.0224(1) 0.5981(1) 0.0307(4) Uani 1.00 d . . . C(5) C 0.6814(1) 0.0375(1) 0.4801(2) 0.0308(4) Uani 1.00 d . . . C(6) C 0.6285(1) 0.1465(1) 0.4556(1) 0.0282(4) Uani 1.00 d . . . C(1') C 0.5004(1) 0.3230(1) 0.5167(1) 0.0257(4) Uani 1.00 d . . . C(2') C 0.6015(1) 0.4199(1) 0.5248(1) 0.0247(4) Uani 1.00 d . . . C(3') C 0.5635(1) 0.5304(1) 0.4428(1) 0.0278(4) Uani 1.00 d . . . C(4') C 0.5089(1) 0.4797(1) 0.3161(1) 0.0306(4) Uani 1.00 d . . . C(5') C 0.5982(2) 0.4584(2) 0.2064(2) 0.0375(5) Uani 1.00 d . . . C(6') C 0.6719(2) 0.6100(1) 0.4180(2) 0.0340(4) Uani 1.00 d . . . C(7') C 0.7606(2) 0.6657(2) 0.3979(2) 0.0520(6) Uani 1.00 d . . . H(1) H 0.654(2) -0.180(1) 0.695(2) 0.066(6) Uiso 1.00 calc . . . H(2) H 0.742(1) -0.172(1) 0.575(2) 0.058(6) Uiso 1.00 calc . . . H(3) H 0.736(1) 0.000(1) 0.423(1) 0.035(4) Uiso 1.00 calc . . . H(4) H 0.642(1) 0.191(1) 0.365(1) 0.038(4) Uiso 1.00 calc . . . H(5) H 0.439(1) 0.334(1) 0.588(1) 0.024(4) Uiso 1.00 calc . . . H(6) H 0.681(1) 0.385(1) 0.487(1) 0.015(4) Uiso 1.00 calc . . . H(7) H 0.441(1) 0.538(1) 0.285(1) 0.033(4) Uiso 1.00 calc . . . H(8) H 0.628(1) 0.537(1) 0.182(1) 0.038(5) Uiso 1.00 calc . . . H(9) H 0.553(1) 0.421(1) 0.128(1) 0.049(5) Uiso 1.00 calc . . . H(10) H 0.754(2) 0.401(2) 0.217(2) 0.090(8) Uiso 1.00 calc . . . H(11) H 0.568(2) 0.463(2) 0.702(2) 0.078(8) Uiso 1.00 calc . . . H(12) H 0.494(2) 0.633(1) 0.575(1) 0.055(6) Uiso 1.00 calc . . . H(13) H 0.832(2) 0.716(1) 0.378(2) 0.067(6) Uiso 1.00 calc . . . 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 S(4') 0.0305(2) 0.0443(2) 0.0314(2) -0.0036(2) -0.0064(2) -0.0014(2) O(5') 0.0370(7) 0.0435(8) 0.0439(7) 0.0062(6) 0.0109(6) 0.0023(6) O(2) 0.0611(8) 0.0356(6) 0.0358(6) 0.0144(6) 0.0231(6) 0.0035(5) O(2') 0.0385(7) 0.0389(7) 0.0234(5) -0.0027(6) -0.0056(6) -0.0024(6) O(3') 0.0355(7) 0.0369(6) 0.0319(6) 0.0100(5) 0.0013(5) -0.0044(6) N(1) 0.0295(7) 0.0242(6) 0.0273(6) 0.0007(6) 0.0052(6) 0.0003(5) N(3) 0.0392(8) 0.0257(6) 0.0313(7) 0.0008(6) 0.0072(6) 0.0011(6) N(4) 0.056(1) 0.0287(8) 0.0500(10) 0.0107(7) 0.0167(9) 0.0039(8) C(2) 0.0351(9) 0.0308(8) 0.0284(7) -0.0034(7) 0.0035(7) 0.0011(7) C(4) 0.0311(8) 0.0265(7) 0.0344(8) -0.0034(7) -0.0001(7) -0.0023(7) C(5) 0.0309(8) 0.0317(8) 0.0299(8) 0.0012(7) 0.0055(7) -0.0063(7) C(6) 0.0283(8) 0.0309(8) 0.0254(8) -0.0039(7) 0.0021(7) -0.0048(7) C(1') 0.0272(7) 0.0269(7) 0.0230(7) 0.0018(6) 0.0016(6) 0.0014(7) C(2') 0.0265(8) 0.0266(7) 0.0211(7) 0.0017(6) -0.0003(7) -0.0013(6) C(3') 0.0303(7) 0.0274(7) 0.0257(7) 0.0051(7) 0.0011(7) 0.0006(6) C(4') 0.0326(8) 0.0331(8) 0.0261(7) 0.0056(7) -0.0027(6) 0.0029(7) C(5') 0.044(1) 0.0405(10) 0.0283(8) 0.0043(8) 0.0041(7) 0.0052(8) C(6') 0.0442(9) 0.0296(9) 0.0282(8) 0.0011(7) 0.0031(8) 0.0012(8) C(7') 0.061(1) 0.047(1) 0.048(1) -0.019(1) 0.013(1) -0.007(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag S(4') C(1') 1.818(2) . . yes S(4') C(4') 1.840(3) . . yes O(5') C(5') 1.420(3) . . yes O(5') H(10) 0.77(3) . . no O(2) C(2) 1.241(3) . . yes O(2') C(2') 1.410(3) . . yes O(2') H(11) 0.83(3) . . no O(3') C(3') 1.429(3) . . yes O(3') H(12) 0.86(2) . . no N(1) C(2) 1.397(3) . . yes N(1) C(6) 1.370(3) . . yes N(1) C(1') 1.473(3) . . yes N(3) C(2) 1.359(3) . . yes N(3) C(4) 1.330(3) . . yes N(4) C(4) 1.334(3) . . yes N(4) H(1) 1.00(3) . . no N(4) H(2) 0.86(3) . . no C(4) C(5) 1.434(3) . . yes C(5) C(6) 1.343(3) . . yes C(5) H(3) 0.93(2) . . no C(6) H(4) 1.07(2) . . no C(1') C(2') 1.527(3) . . yes C(1') H(5) 1.00(2) . . no C(2') C(3') 1.532(3) . . yes C(2') H(6) 1.03(2) . . no C(3') C(4') 1.546(3) . . yes C(3') C(6') 1.487(3) . . yes C(4') C(5') 1.516(3) . . yes C(4') H(3') 1.03(2) . . no C(5') H(8) 0.95(2) . . no C(5') H(9) 1.04(2) . . no C(6') C(7') 1.159(4) . . yes C(7') H(13) 0.97(3) . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1') S(4') C(4') 94.9(1) . 1_555 1_555 yes C(5') O(5') H(10) 107(2) . 1_555 1_555 no C(2') O(2') H(11) 117(2) . 1_555 1_555 no C(3') O(3') H(12) 112(1) . 1_555 1_555 no C(2) N(1) C(6) 120.4(2) . 1_555 1_555 yes C(2) N(1) C(1') 119.5(2) . 1_555 1_555 yes C(6) N(1) C(1') 119.6(2) . 1_555 1_555 yes C(2) N(3) C(4) 120.3(2) . 1_555 1_555 yes C(4) N(4) H(1) 116(1) . 1_555 1_555 no C(4) N(4) H(2) 122(1) . 1_555 1_555 no H(1) N(4) H(2) 115(2) . 1_555 1_555 no O(2) C(2) N(1) 119.9(2) . 1_555 1_555 yes O(2) C(2) N(3) 121.4(2) . 1_555 1_555 yes N(1) C(2) N(3) 118.8(2) . 1_555 1_555 yes N(3) C(4) N(4) 117.9(2) . 1_555 1_555 yes N(3) C(4) C(5) 121.8(2) . 1_555 1_555 yes N(4) C(4) C(5) 120.3(2) . 1_555 1_555 yes C(4) C(5) C(6) 117.2(2) . 1_555 1_555 yes C(4) C(5) H(3) 119(1) . 1_555 1_555 no C(6) C(5) H(3) 122(1) . 1_555 1_555 no N(1) C(6) C(5) 121.1(2) . 1_555 1_555 yes N(1) C(6) H(4) 118(1) . 1_555 1_555 no C(5) C(6) H(4) 120(1) . 1_555 1_555 no S(4') C(1') N(1) 112.2(2) . 1_555 1_555 yes S(4') C(1') C(2') 107.4(2) . 1_555 1_555 yes S(4') C(1') H(5) 112(1) . 1_555 1_555 no N(1) C(1') C(2') 111.4(2) . 1_555 1_555 yes N(1) C(1') H(5) 102(1) . 1_555 1_555 no C(2') C(1') H(5) 111(1) . 1_555 1_555 no O(2') C(2') C(1') 110.9(2) . 1_555 1_555 yes O(2') C(2') C(3') 113.6(2) . 1_555 1_555 yes O(2') C(2') H(6) 106(1) . 1_555 1_555 no C(1') C(2') C(3') 108.6(2) . 1_555 1_555 yes C(1') C(2') H(6) 109(1) . 1_555 1_555 no C(3') C(2') H(6) 107(1) . 1_555 1_555 no O(3') C(3') C(2') 109.8(2) . 1_555 1_555 yes O(3') C(3') C(4') 107.2(2) . 1_555 1_555 yes O(3') C(3') C(6') 111.1(2) . 1_555 1_555 yes C(2') C(3') C(4') 107.2(2) . 1_555 1_555 yes C(2') C(3') C(6') 109.9(2) . 1_555 1_555 yes C(4') C(3') C(6') 111.5(2) . 1_555 1_555 yes S(4') C(4') C(3') 106.3(2) . 1_555 1_555 yes S(4') C(4') C(5') 110.1(2) . 1_555 1_555 yes S(4') C(4') H(7) 105(1) . 1_555 1_555 no C(3') C(4') C(5') 116.6(2) . 1_555 1_555 yes C(3') C(4') H(7) 108(1) . 1_555 1_555 no C(5') C(4') H(7) 108(1) . 1_555 1_555 no O(5') C(5') C(4') 111.0(2) . 1_555 1_555 yes O(5') C(5') H(8) 113(1) . 1_555 1_555 no O(5') C(5') H(9) 107(1) . 1_555 1_555 no C(4') C(5') H(8) 106(1) . 1_555 1_555 no C(4') C(5') H(9) 110(1) . 1_555 1_555 no H(8) C(5') H(9) 108(1) . 1_555 1_555 no C(3') C(6') C(7') 175.9(3) . 1_555 1_555 yes C(6') C(7') H(13) 176(1) . 1_555 1_555 no #------------------------------------------------------------------------------ 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S(4') C(1') N(1) C(2) -134.6(2) 1_555 1_555 1_555 1_555 yes S(4') C(1') N(1) C(6) 53.1(2) 1_555 1_555 1_555 1_555 yes S(4') C(1') C(2') O(2') 157.2(2) 1_555 1_555 1_555 1_555 yes S(4') C(1') C(2') C(3') 31.7(2) 1_555 1_555 1_555 1_555 yes S(4') C(4') C(3') O(3') -84.1(2) 1_555 1_555 1_555 1_555 yes S(4') C(4') C(3') C(2') 33.7(2) 1_555 1_555 1_555 1_555 yes S(4') C(4') C(3') C(6') 154.1(2) 1_555 1_555 1_555 1_555 yes S(4') C(4') C(5') O(5') -63.2(3) 1_555 1_555 1_555 1_555 yes O(5') C(5') C(4') C(3') 58.1(3) 1_555 1_555 1_555 1_555 yes O(2) C(2) N(1) C(6) 172.7(2) 1_555 1_555 1_555 1_555 yes O(2) C(2) N(1) C(1') 0.4(3) 1_555 1_555 1_555 1_555 yes O(2) C(2) N(3) C(4) -172.7(2) 1_555 1_555 1_555 1_555 yes O(2') C(1') C(1') N(1) -79.6(2) 1_555 1_555 1_555 1_555 yes O(2') C(2') C(3') O(3') -50.4(3) 1_555 1_555 1_555 1_555 yes O(2') C(2') C(3') C(4') -166.6(2) 1_555 1_555 1_555 1_555 yes O(2') C(2') C(3') C(6') 72.1(3) 1_555 1_555 1_555 1_555 yes O(3') C(3') C(2') C(1') 73.4(2) 1_555 1_555 1_555 1_555 yes O(3') C(3') C(4') C(5') 152.7(2) 1_555 1_555 1_555 1_555 yes O(3') C(3') C(6') C(7') 160(4) 1_555 1_555 1_555 1_555 yes N(1) C(2) N(3) C(4) 7.3(3) 1_555 1_555 1_555 1_555 yes N(1) C(6) C(5) C(4) 1.6(4) 1_555 1_555 1_555 1_555 yes N(1) C(1') S(4') C(4') -132.8(2) 1_555 1_555 1_555 1_555 yes N(1) C(1') C(2') C(3') 154.9(2) 1_555 1_555 1_555 1_555 yes N(3) C(2) N(1) C(6) -7.4(3) 1_555 1_555 1_555 1_555 yes N(3) C(2) N(1) C(1') -179.6(2) 1_555 1_555 1_555 1_555 yes N(3) C(4) C(5) C(6) -1.6(4) 1_555 1_555 1_555 1_555 yes N(4) C(4) N(3) C(2) 175.8(2) 1_555 1_555 1_555 1_555 yes N(4) C(3) C(5) C(6) 179.7(2) 1_555 1_555 1_555 1_555 yes C(2) N(1) C(6) C(5) 2.9(3) 1_555 1_555 1_555 1_555 yes C(2) N(1) C(1') C(2') 105.0(2) 1_555 1_555 1_555 1_555 yes C(2) N(3) C(4) C(5) -2.9(4) 1_555 1_555 1_555 1_555 yes C(5) C(6) N(1) C(1') 175.1(2) 1_555 1_555 1_555 1_555 yes C(6) N(1) C(1') C(2') -67.3(3) 1_555 1_555 1_555 1_555 yes C(1') S(4') C(4') C(3') -13.7(2) 1_555 1_555 1_555 1_555 yes C(1') S(4') C(4') C(5') 113.5(2) 1_555 1_555 1_555 1_555 yes C(1') C(2') C(3') C(4') -42.8(3) 1_555 1_555 1_555 1_555 yes C(1' C(2') C(3') C(6') -164.1(2) 1_555 1_555 1_555 1_555 yes C(2') C(1') S(4') C(4') -10.1(2) 1_555 1_555 1_555 1_555 yes C(2') C(3') C(4') C(5') -89.4(3) 1_555 1_555 1_555 1_555 yes C(2') C(3') C(6') C(7') 38(4) 1_555 1_555 1_555 1_555 yes C(4') C(3') C(6') C(7') -80(4) 1_555 1_555 1_555 1_555 yes C(5') C(4') C(3') C(6') 30.9(3) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S(4') H(8) 3.34(2) . 4_645 ? S(4') C(5) 3.481(3) . 3_456 ? S(4') H(3) 3.59(2) . 3_456 ? O(5') H(1) 2.75(3) . 2_654 ? O(5') O(2') 2.883(3) . 2_664 ? O(5') H(2) 2.91(3) . 2_654 ? O(5') O(2) 3.051(3) . 3_556 ? O(5') N(4) 3.155(3) . 2_654 ? O(5') H(11) 3.17(3) . 2_664 ? O(2) H(10) 2.55(3) . 3_456 ? O(2) H(11) 2.63(3) . 4_646 ? O(2) H(13) 2.81(3) . 2_665 ? O(2) N(4) 2.891(3) . 4_656 ? O(2) O(3') 2.923(3) . 4_646 ? O(2) O(2') 3.059(3) . 4_646 ? O(2) H(2) 3.26(3) . 4_656 ? O(2') H(8) 2.68(2) . 2_665 ? O(2') N(3) 2.884(3) . 4_656 ? O(2') H(13) 2.98(3) . 2_665 ? O(2') C(7') 3.080(3) . 2_665 ? O(2') C(5') 3.197(4) . 2_665 ? O(2') C(2) 3.302(3) . 4_656 ? O(2') C(6') 3.566(3) . 2_665 ? O(3') H(2) 2.73(3) . 3_456 ? O(3') H(13) 2.79(3) . 3_466 ? O(3') H(3) 2.84(3) . 3_456 ? O(3') N(4) 3.287(3) . 3_456 ? O(3') N(3) 3.350(3) . 4_656 ? O(3') C(5) 3.452(3) . 3_456 ? O(3') C(2) 3.501(3) . 4_656 ? O(3') C(7') 3.573(4) . 3_466 ? N(1) H(8) 3.50(2) . 4_645 ? N(3) H(12) 2.87(3) . 4_646 ? N(3) H(5) 3.20(2) . 4_646 ? N(3) H(3) 3.29(2) . 2_655 ? N(4) H(7) 2.98(2) . 3_556 ? N(4) H(4) 3.09(2) . 2_655 ? N(4) H(10) 3.13(3) . 2_655 ? N(4) H(5) 3.32(2) . 4_646 ? N(4) C(7') 3.332(4) . 1_545 ? N(4) H(13) 3.42(3) . 1_545 ? N(4) H(12) 3.43(3) . 1_545 ? N(4) H(3) 3.46(2) . 2_655 ? N(4) H(11) 3.54(3) . 4_646 ? N(4) C(6') 3.576(3) . 1_545 ? C(2) H(11) 2.63(3) . 4_646 ? C(2) H(12) 2.77(2) . 4_646 ? C(2) H(1) 3.13(3) . 4_656 ? C(2) H(13) 3.15(3) . 2_665 ? C(2) H(10) 3.25(3) . 3_456 ? C(4) H(11) 3.15(3) . 4_646 ? C(4) H(9) 3.27(2) . 4_645 ? C(4) H(7) 3.41(2) . 3_556 ? C(5) H(7) 3.06(2) . 4_645 ? C(5) H(9) 3.06(2) . 4_645 ? C(5) H(5) 3.21(2) . 3_556 ? C(6) H(7) 2.86(2) . 4_645 ? C(6) H(9) 3.27(2) . 4_645 ? C(6) H(8) 3.36(2) . 4_645 ? C(6) H(5) 3.42(2) . 3_556 ? C(1') H(1) 3.43(3) . 4_656 ? C(1') H(3) 3.53(3) . 3_456 ? C(2') H(10) 3.20(3) . 2_665 ? C(2') H(8) 3.40(2) . 2_665 ? C(3') H(10) 3.55(3) . 2_665 ? C(4') H(4) 3.39(2) . 4_655 ? C(6') H(2) 2.98(3) . 1_565 ? C(6') H(10) 3.21(3) . 2_665 ? C(7') H(2) 2.56(3) . 1_565 ? C(7') H(11) 3.09(3) . 2_664 ? C(7') H(9) 3.27(2) . 2_665 ? C(7') H(12) 3.37(3) . 3_566 ? C(7') H(10) 3.40(3) . 2_665 ? H(1) H(10) 2.62(4) . 2_655 ? H(1) H(4) 2.84(4) . 2_655 ? H(1) H(12) 2.95(4) . 1_545 ? H(1) H(11) 3.07(4) . 4_646 ? H(1) H(3) 3.30(4) . 2_655 ? H(1) H(7) 3.49(4) . 3_556 ? H(2) H(13) 2.58(3) . 1_545 ? H(2) H(10) 2.90(4) . 2_655 ? H(2) H(7) 2.99(3) . 3_556 ? H(2) H(12) 3.18(4) . 3_556 ? H(2) H(4) 3.27(3) . 2_655 ? H(2) H(12) 3.43(4) . 1_545 ? H(2) H(9) 3.55(3) . 2_655 ? H(3) H(5) 2.87(3) . 3_556 ? H(3) H(7) 2.92(3) . 4_645 ? H(3) H(12) 3.16(4) . 3_556 ? H(3) H(13) 3.30(4) . 1_545 ? H(3) H(9) 3.30(4) . 4_645 ? H(4) H(5) 3.28(3) . 3_556 ? H(4) H(8) 3.42(3) . 4_645 ? H(6) H(8) 3.03(3) . 2_665 ? H(6) H(10) 3.42(4) . 2_665 ? H(8) H(11) 3.31(4) . 2_664 ? H(9) H(13) 3.25(3) . 2_664 ? H(10) H(12) 3.14(4) . 2_664 ? H(11) H(13) 2.89(4) . 2_665 ? #------------------------------------------------------------------------------