# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry. # This journal is © The Royal Society of Chemistry 2023 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_hari_se_sx _database_code_depnum_ccdc_archive 'CCDC 2207173' loop_ _audit_author_name _audit_author_address 'Geoffrey Jameson' ;School of Natural Sciences, Massey University New Zealand ; _audit_update_record ; 2022-09-14 deposited with the CCDC. 2023-05-23 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT029_hari_se_sx ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.887 Why? RESPONSE: High mosaicity cuasing reflection overlap and consequent elimination of reflections. Main aim of structure determination was establishing connectivity and stereochemistry at C5 knowing configuration of beta-D-2'-deoxyribose. Accomplished. ; _vrf_PLAT241_hari_se_sx ; PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of C13T Check RESPONSE: Loose crystal packing and room temperature data (XStream died) led to very high torsional motion of the benzyl group and one of the toluoyl groups. ; _vrf_PLAT242_hari_se_sx ; PROBLEM: Low 'MainMol' Ueq as Compared to Neighbors of C11T Check RESPONSE: Loose crystal packing and room temperature data (XStream died) led to very high torsional motion of the benzyl group and one of the toluoyl groups. ; _vrf_PLAT315_hari_se_sx ; PROBLEM: Singly Bonded Carbon Detected (H-atoms Missing). C16T Check RESPONSE: Riding refinkment of this methyl group was unstable and therefore eliminated. ; _vrf_PLAT340_hari_se_sx ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.01634 Ang. RESPONSE: Overall high atomic displacement parameters, exacerbated by high torsional motions of benzyl group and one toluoyl group. ; _vrf_PLAT911_hari_se_sx ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.595 276 Report RESPONSE: Eliminated 4 reflections with very poor agreement between Fcalc and Fobs (see Plat029). ; # Added during the CSD deposition process: Wednesday 14 September 2022 10:34 AM # end Validation Reply Form _audit_creation_date 2022-09-07 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2017/1 _chemical_name_common ? _chemical_name_systematic 1-[2-deoxy-3,5-bis-O-(4-methylbenzoyl)-\b-D-erythro-pentofuranosyl]-(R)-5-benzyloxyazepan-2-one _chemical_formula_moiety 'C34 H34 N O7' _chemical_formula_sum 'C34 H34 N O7' _chemical_formula_weight 568.62 _chemical_absolute_configuration rmad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_H-M_alt 'I 1 2 1' _space_group_name_Hall 'I 2y' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 19.200(2) _cell_length_b 5.3821(5) _cell_length_c 32.153(4) _cell_angle_alpha 90 _cell_angle_beta 98.636(9) _cell_angle_gamma 90 _cell_volume 3284.9(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4610 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 66.554 _cell_measurement_theta_min 5.567 _shelx_estimated_absorpt_T_max 0.968 _shelx_estimated_absorpt_T_min 0.877 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_absorpt_special_details ; Note that the experimental absorption process corrects not only for absorption but for mis-alignment. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'flattened needle' _exptl_crystal_F_000 1284 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_unetI/netI 0.0735 _diffrn_reflns_Laue_measured_fraction_full 0.887 _diffrn_reflns_Laue_measured_fraction_max 0.887 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_number 6980 _diffrn_reflns_point_group_measured_fraction_full 0.735 _diffrn_reflns_point_group_measured_fraction_max 0.735 _diffrn_reflns_theta_full 66.554 _diffrn_reflns_theta_max 66.554 _diffrn_reflns_theta_min 5.567 _diffrn_ambient_temperature 293(2) _diffrn_detector 'Image plate' _diffrn_detector_area_resol_mean 10 _diffrn_measured_fraction_theta_full 0.887 _diffrn_measured_fraction_theta_max 0.887 _diffrn_measurement_device_type 'Rigaku Spider/Rapide' _diffrn_measurement_method \w-scans _diffrn_radiation_monochromator 'Rigaku VariMax-HF Confocal Optical System' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54187 _diffrn_source 'Rigaku MM007 microfocus roating anode/' _reflns_Friedel_coverage 0.485 _reflns_Friedel_fraction_full 0.543 _reflns_Friedel_fraction_max 0.543 _reflns_number_gt 1774 _reflns_number_total 4270 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_data_collection 'CrystalClear (Rigaku, 2005)' _computing_data_reduction 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _refine_diff_density_max 0.155 _refine_diff_density_min -0.173 _refine_diff_density_rms 0.043 _refine_ls_abs_structure_details ; Flack x determined using 505 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.2(3) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 380 _refine_ls_number_reflns 4270 _refine_ls_number_restraints 187 _refine_ls_R_factor_all 0.1303 _refine_ls_R_factor_gt 0.0693 _refine_ls_restrained_S_all 0.917 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1410P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1842 _refine_ls_wR_factor_ref 0.2434 _refine_special_details ; Absolute structure was weakly determined by Flack x (-0.2(3) and Hooft y (0.0(2) parameters. The expected beta-D-2-deoxyribose was observed, establishing the S-diasteromer at nucleobase atom C5. Data were collected at 293 K due to breakdown of XStream. As a result, and also due to loose packing, one benzyl group suffers very high torsional motions. Tight restrainsts were applied to interatomic distances, planarity, and atomic displacement parameters for the toluoyl and benzyl groups. The methyl hydrogens on one toluoyl group were omitted as their positions were unstable under riding refinement. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C22T-C28T = C27T-C25T = C24T-C23T 1.392 with sigma of 0.01 C2T-C7T = C6T-C5T = C4T-C3T 1.392 with sigma of 0.01 C15T-C12T = C17T-C13T = C18T-C14T 2.784 with sigma of 0.01 C12T-C18T = C17T-C15T = C14T-C13T 1.392 with sigma of 0.01 C15T-C12T 2.784 with sigma of 0.01 C17T-C13T 2.784 with sigma of 0.01 C18T-C14T 2.784 with sigma of 0.01 3. Restrained planarity O3', O11T, C11T, C12T with sigma of 0.1 C21T, C22T, C28T, C27T, C25T, C26T, C24T, C23T with sigma of 0.1 C22T, C21T, O21T, O5' with sigma of 0.1 C11T, C12T, C13T, C14T, C15T, C16T, C17T, C18T with sigma of 0.1 C1T, C2T, C7T, C6T, C5T, C4T, C3T with sigma of 0.1 C1', N1, C2, O2, C3 with sigma of 0.1 4. Rigid bond restraints C11T, C12T, C18T, C17T, C15T, C16T, C14T, C13T with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C1T, C2T, C7T, C6T, C5T, C4T, C3T with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 5. Uiso/Uaniso restraints and constraints C12T \\sim C18T \\sim C17T \\sim C15T \\sim C16T \\sim C14T \\sim C13T: within 2A with sigma of 0.1 and sigma for terminal atoms of 0.1 C1T \\sim C2T \\sim C7T \\sim C6T \\sim C5T \\sim C4T \\sim C3T: within 2A with sigma of 0.1 and sigma for terminal atoms of 0.1 Uanis(C16T) \\sim Ueq, Uanis(C18T) \\sim Ueq, Uanis(C13T) \\sim Ueq, Uanis(C14T) \\sim Ueq, Uanis(C17T) \\sim Ueq, Uanis(C15T) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 6.a Ternary CH refined with riding coordinates: C1'(H1'), C4'(H4'), C3'(H3'), C5(H5) 6.b Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C7(H7A,H7B), C5'(H5'A,H5'B), C6(H6A,H6B), C2'(H2'A,H2'B), C4(H4A, H4B), C1T(H1TA,H1TB) 6.c Aromatic/amide H refined with riding coordinates: C28T(H28T), C23T(H23T), C24T(H24T), C27T(H27T), C7T(H7T), C3T(H3T), C17T(H17T), C6T(H6T), C13T(H13T), C18T(H18T), C4T(H4T), C5T(H5T), C14T(H14T) 6.d Idealised Me refined as rotating group: C26T(H26A,H26B,H26C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O5' O 0.6981(2) 0.6398(11) 0.30230(14) 0.1004(16) Uani 1 1 d . . . . . O21T O 0.7898(3) 0.4840(13) 0.27587(18) 0.1130(19) Uani 1 1 d . . . . . O1' O 0.5754(3) 0.3627(12) 0.31910(19) 0.1097(18) Uani 1 1 d . . . . . O5 O 0.7258(3) 0.3326(14) 0.48472(19) 0.131(2) Uani 1 1 d . . . . . O3' O 0.4764(3) 0.7811(15) 0.2723(2) 0.136(2) Uani 1 1 d . . . . . C21T C 0.7675(4) 0.6230(18) 0.2990(3) 0.093(2) Uani 1 1 d . . . . . N1 N 0.5768(3) 0.4283(14) 0.3905(2) 0.111(2) Uani 1 1 d . . . . . C1' C 0.5433(4) 0.510(2) 0.3477(3) 0.102(3) Uani 1 1 d . . . . . H1' H 0.492620 0.476136 0.344033 0.122 Uiso 1 1 calc R . . . . O2 O 0.4743(3) 0.303(2) 0.40662(18) 0.177(3) Uani 1 1 d . . . . . C4' C 0.5795(4) 0.506(2) 0.2806(3) 0.104(3) Uani 1 1 d . . . . . H4' H 0.547830 0.432018 0.257143 0.125 Uiso 1 1 calc R . . . . C22T C 0.8115(3) 0.7903(16) 0.3278(2) 0.091(2) Uani 1 1 d D . . . . C3 C 0.5723(4) 0.251(2) 0.4592(3) 0.121(3) Uani 1 1 d . . . . . H3A H 0.608771 0.130210 0.456262 0.146 Uiso 1 1 calc R . . . . H3B H 0.537259 0.168308 0.473200 0.146 Uiso 1 1 calc R . . . . C7 C 0.6564(3) 0.4424(18) 0.4009(2) 0.101(3) Uani 1 1 d . . . . . H7A H 0.674318 0.278988 0.409515 0.121 Uiso 1 1 calc R . . . . H7B H 0.675324 0.486908 0.375558 0.121 Uiso 1 1 calc R . . . . C2 C 0.5392(4) 0.326(2) 0.4175(3) 0.119(3) Uani 1 1 d . . . . . C5' C 0.6528(4) 0.4939(19) 0.2716(2) 0.109(3) Uani 1 1 d . . . . . H5'A H 0.668763 0.322631 0.272757 0.130 Uiso 1 1 calc R . . . . H5'B H 0.654901 0.557441 0.243628 0.130 Uiso 1 1 calc R . . . . C25T C 0.9000(4) 1.113(2) 0.3824(3) 0.122(3) Uani 1 1 d D . . . . C3' C 0.5521(4) 0.760(2) 0.2903(3) 0.107(3) Uani 1 1 d . . . . . H3' H 0.579963 0.892367 0.280029 0.129 Uiso 1 1 calc R . . . . C28T C 0.7848(4) 0.9780(19) 0.3518(3) 0.113(3) Uani 1 1 d D . . . . H28T H 0.736342 0.992861 0.350758 0.136 Uiso 1 1 calc R . . . . C23T C 0.8850(4) 0.7638(18) 0.3324(2) 0.108(3) Uani 1 1 d D . . . . H23T H 0.904952 0.636745 0.318558 0.130 Uiso 1 1 calc R . . . . C24T C 0.9269(4) 0.927(2) 0.3575(3) 0.135(4) Uani 1 1 d D . . . . H24T H 0.975476 0.915999 0.358334 0.162 Uiso 1 1 calc R . . . . C2T C 0.8099(5) 0.091(2) 0.5309(4) 0.148(4) Uani 1 1 d D U . . . C5 C 0.6786(5) 0.544(2) 0.4782(3) 0.124(3) Uani 1 1 d . . . . . H5 H 0.696658 0.677999 0.497588 0.148 Uiso 1 1 calc R . . . . C6 C 0.6823(4) 0.622(2) 0.4343(3) 0.125(3) Uani 1 1 d . . . . . H6A H 0.655555 0.774892 0.428825 0.150 Uiso 1 1 calc R . . . . H6B H 0.731039 0.660821 0.432137 0.150 Uiso 1 1 calc R . . . . C2' C 0.5555(4) 0.771(2) 0.3379(3) 0.108(3) Uani 1 1 d . . . . . H2'A H 0.601241 0.828250 0.351524 0.129 Uiso 1 1 calc R . . . . H2'B H 0.519118 0.878411 0.345908 0.129 Uiso 1 1 calc R . . . . C4 C 0.6050(4) 0.462(2) 0.4874(3) 0.122(3) Uani 1 1 d . . . . . H4A H 0.609056 0.410115 0.516540 0.146 Uiso 1 1 calc R . . . . H4B H 0.573528 0.604334 0.483757 0.146 Uiso 1 1 calc R . . . . C27T C 0.8275(4) 1.136(2) 0.3761(3) 0.120(3) Uani 1 1 d D . . . . H27T H 0.807310 1.266121 0.389158 0.144 Uiso 1 1 calc R . . . . C1T C 0.7537(6) 0.283(3) 0.5274(4) 0.170(4) Uani 1 1 d . U . . . H1TA H 0.716147 0.227067 0.542220 0.204 Uiso 1 1 calc R . . . . H1TB H 0.772859 0.435533 0.540716 0.204 Uiso 1 1 calc R . . . . C26T C 0.9472(5) 1.285(2) 0.4100(3) 0.154(4) Uani 1 1 d . . . . . H26A H 0.983163 1.191207 0.427069 0.231 Uiso 1 1 calc GR . . . . H26B H 0.920084 1.375336 0.427772 0.231 Uiso 1 1 calc GR . . . . H26C H 0.968594 1.400042 0.392880 0.231 Uiso 1 1 calc GR . . . . C12T C 0.3844(4) 0.853(2) 0.2185(3) 0.160(4) Uani 1 1 d D U . . . C7T C 0.8382(6) 0.030(3) 0.4952(4) 0.176(5) Uani 1 1 d D U . . . H7T H 0.824070 0.107688 0.469446 0.211 Uiso 1 1 calc R . . . . C3T C 0.8291(6) -0.022(3) 0.5673(4) 0.182(6) Uani 1 1 d D U . . . H3T H 0.807922 0.023874 0.590314 0.219 Uiso 1 1 calc R . . . . C17T C 0.2806(10) 0.959(5) 0.1670(5) 0.270(10) Uani 1 1 d D U . . . H17T H 0.260381 1.048866 0.143604 0.324 Uiso 1 1 calc R . . . . C6T C 0.8900(7) -0.159(3) 0.5002(4) 0.201(6) Uani 1 1 d D U . . . H6T H 0.909844 -0.210838 0.477073 0.242 Uiso 1 1 calc R . . . . C13T C 0.3415(6) 0.684(4) 0.2360(6) 0.350(15) Uani 1 1 d D U . . . H13T H 0.361849 0.577205 0.257106 0.420 Uiso 1 1 calc R . . . . C18T C 0.3537(7) 0.985(4) 0.1842(4) 0.277(10) Uani 1 1 d D U . . . H18T H 0.381254 1.095835 0.171549 0.333 Uiso 1 1 calc R . . . . C4T C 0.8794(7) -0.205(3) 0.5721(5) 0.201(6) Uani 1 1 d D U . . . H4T H 0.891430 -0.285861 0.597715 0.241 Uiso 1 1 calc R . . . . C15T C 0.2417(6) 0.793(5) 0.1872(7) 0.276(10) Uani 1 1 d D U . . . C5T C 0.9113(8) -0.265(3) 0.5384(5) 0.196(6) Uani 1 1 d D U . . . H5T H 0.947965 -0.380092 0.541453 0.235 Uiso 1 1 calc R . . . . C11T C 0.4561(5) 0.867(2) 0.2357(4) 0.141(4) Uani 1 1 d . U . . . O11T O 0.4975(4) 0.952(3) 0.2182(3) 0.288(9) Uani 1 1 d . . . . . C14T C 0.2680(7) 0.672(5) 0.2225(7) 0.396(18) Uani 1 1 d D U . . . H14T H 0.238807 0.581922 0.237570 0.475 Uiso 1 1 calc R . . . . C16T C 0.1603(8) 0.807(8) 0.1722(7) 0.412(18) Uani 1 1 d . U . . . 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 O5' 0.081(3) 0.110(5) 0.111(4) -0.005(4) 0.017(2) -0.012(3) O21T 0.118(3) 0.109(5) 0.118(4) -0.012(4) 0.035(3) -0.004(4) O1' 0.113(3) 0.103(5) 0.114(4) -0.014(4) 0.022(3) -0.003(3) O5 0.126(4) 0.149(7) 0.110(4) 0.010(5) -0.010(3) 0.014(4) O3' 0.096(3) 0.162(6) 0.145(5) 0.040(5) -0.003(3) -0.006(4) C21T 0.098(5) 0.093(7) 0.089(6) 0.005(6) 0.014(4) -0.006(5) N1 0.083(3) 0.116(6) 0.144(6) -0.009(5) 0.043(4) -0.001(4) C1' 0.085(4) 0.111(9) 0.110(7) 0.015(7) 0.015(5) 0.002(5) O2 0.114(4) 0.266(11) 0.155(5) 0.038(7) 0.033(4) -0.026(5) C4' 0.099(5) 0.095(8) 0.117(7) -0.006(6) 0.012(4) -0.005(5) C22T 0.085(4) 0.102(7) 0.089(5) 0.007(5) 0.020(4) 0.002(5) C3 0.107(5) 0.124(10) 0.139(8) 0.019(8) 0.037(6) 0.002(6) C7 0.064(3) 0.115(8) 0.124(6) 0.009(6) 0.017(4) 0.001(4) C2 0.078(4) 0.160(10) 0.123(7) 0.001(7) 0.025(5) -0.020(5) C5' 0.104(5) 0.121(8) 0.102(5) -0.026(6) 0.019(4) -0.018(5) C25T 0.112(6) 0.119(9) 0.126(7) 0.021(7) -0.008(5) -0.018(6) C3' 0.089(5) 0.099(8) 0.127(7) 0.017(6) -0.001(4) -0.008(5) C28T 0.090(5) 0.136(9) 0.113(6) 0.016(7) 0.012(5) -0.010(6) C23T 0.090(5) 0.110(8) 0.124(6) 0.007(6) 0.015(4) 0.003(5) C24T 0.088(5) 0.164(12) 0.148(8) 0.005(9) 0.005(5) -0.009(7) C2T 0.101(6) 0.183(12) 0.149(8) 0.034(8) -0.019(5) -0.020(6) C5 0.143(8) 0.106(9) 0.117(8) -0.006(6) 0.001(6) 0.006(7) C6 0.119(6) 0.118(9) 0.136(8) 0.000(8) 0.010(5) -0.005(6) C2' 0.093(4) 0.121(10) 0.108(7) 0.006(6) 0.014(4) -0.002(5) C4 0.124(6) 0.119(9) 0.127(7) 0.011(7) 0.038(5) 0.031(6) C27T 0.109(6) 0.135(9) 0.114(6) -0.016(7) 0.012(5) -0.020(6) C1T 0.149(8) 0.183(12) 0.172(11) -0.005(9) 0.008(7) 0.004(7) C26T 0.147(7) 0.138(10) 0.162(8) -0.036(8) -0.026(6) -0.031(7) C12T 0.111(6) 0.224(14) 0.138(8) 0.002(9) 0.001(5) 0.012(7) C7T 0.153(8) 0.171(13) 0.204(10) 0.051(10) 0.025(8) 0.045(8) C3T 0.131(7) 0.247(17) 0.156(8) 0.048(10) -0.017(7) -0.007(8) C17T 0.206(11) 0.40(3) 0.172(12) 0.033(15) -0.067(10) 0.052(14) C6T 0.192(11) 0.209(16) 0.203(11) 0.066(12) 0.028(9) 0.072(10) C13T 0.143(8) 0.52(4) 0.35(2) 0.20(2) -0.083(11) -0.101(15) C18T 0.168(9) 0.48(3) 0.175(11) 0.100(15) -0.017(8) 0.034(13) C4T 0.170(11) 0.225(17) 0.194(11) 0.081(13) -0.016(9) -0.015(9) C15T 0.175(10) 0.33(3) 0.28(2) 0.003(17) -0.088(12) 0.008(13) C5T 0.169(10) 0.162(13) 0.241(15) 0.070(12) -0.014(9) 0.035(9) C11T 0.112(6) 0.175(11) 0.135(9) 0.038(9) 0.012(6) -0.007(7) O11T 0.144(6) 0.50(2) 0.203(8) 0.167(13) -0.016(5) -0.026(9) C14T 0.154(10) 0.51(4) 0.47(3) 0.23(3) -0.126(15) -0.119(17) C16T 0.163(9) 0.62(5) 0.40(2) -0.01(3) -0.129(13) 0.022(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O5' C21T 1.357(8) . ? O5' C5' 1.444(8) . ? O21T C21T 1.180(9) . ? O1' C1' 1.421(9) . ? O1' C4' 1.470(10) . ? O5 C5 1.450(11) . ? O5 C1T 1.422(11) . ? O3' C3' 1.485(8) . ? O3' C11T 1.270(11) . ? C21T C22T 1.465(11) . ? N1 C1' 1.495(10) . ? N1 C7 1.515(8) . ? N1 C2 1.330(10) . ? C1' H1' 0.9800 . ? C1' C2' 1.469(13) . ? O2 C2 1.250(8) . ? C4' H4' 0.9800 . ? C4' C5' 1.481(10) . ? C4' C3' 1.512(12) . ? C22T C28T 1.413(9) . ? C22T C23T 1.403(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C2 1.453(11) . ? C3 C4 1.530(13) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C6 1.477(12) . ? C5' H5'A 0.9700 . ? C5' H5'B 0.9700 . ? C25T C24T 1.427(13) . ? C25T C27T 1.382(9) . ? C25T C26T 1.491(13) . ? C3' H3' 0.9800 . ? C3' C2' 1.523(10) . ? C28T H28T 0.9300 . ? C28T C27T 1.346(11) . ? C23T H23T 0.9300 . ? C23T C24T 1.370(9) . ? C24T H24T 0.9300 . ? C2T C1T 1.485(16) . ? C2T C7T 1.382(10) . ? C2T C3T 1.323(14) . ? C5 H5 0.9800 . ? C5 C6 1.487(12) . ? C5 C4 1.551(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C2' H2'A 0.9700 . ? C2' H2'B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C27T H27T 0.9300 . ? C1T H1TA 0.9700 . ? C1T H1TB 0.9700 . ? C26T H26A 0.9600 . ? C26T H26B 0.9600 . ? C26T H26C 0.9600 . ? C12T C13T 1.402(17) . ? C12T C18T 1.367(10) . ? C12T C11T 1.407(12) . ? C7T H7T 0.9300 . ? C7T C6T 1.413(16) . ? C3T H3T 0.9300 . ? C3T C4T 1.372(11) . ? C17T H17T 0.9300 . ? C17T C18T 1.44(2) . ? C17T C15T 1.388(12) . ? C6T H6T 0.9300 . ? C6T C5T 1.360(10) . ? C13T H13T 0.9300 . ? C13T C14T 1.414(11) . ? C18T H18T 0.9300 . ? C4T H4T 0.9300 . ? C4T C5T 1.362(19) . ? C15T C14T 1.34(2) . ? C15T C16T 1.567(16) . ? C5T H5T 0.9300 . ? C11T O11T 1.137(11) . ? C14T H14T 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21T O5' C5' 114.1(6) . . ? C1' O1' C4' 109.6(7) . . ? C1T O5 C5 114.9(9) . . ? C11T O3' C3' 122.4(7) . . ? O5' C21T C22T 112.9(8) . . ? O21T C21T O5' 123.0(8) . . ? O21T C21T C22T 124.0(7) . . ? C1' N1 C7 117.9(6) . . ? C2 N1 C1' 121.5(7) . . ? C2 N1 C7 120.4(7) . . ? O1' C1' N1 105.3(7) . . ? O1' C1' H1' 109.8 . . ? O1' C1' C2' 107.3(7) . . ? N1 C1' H1' 109.8 . . ? C2' C1' N1 114.7(9) . . ? C2' C1' H1' 109.8 . . ? O1' C4' H4' 109.3 . . ? O1' C4' C5' 108.3(7) . . ? O1' C4' C3' 103.7(7) . . ? C5' C4' H4' 109.3 . . ? C5' C4' C3' 116.8(8) . . ? C3' C4' H4' 109.3 . . ? C28T C22T C21T 124.2(7) . . ? C23T C22T C21T 118.6(8) . . ? C23T C22T C28T 117.2(8) . . ? H3A C3 H3B 107.5 . . ? C2 C3 H3A 108.5 . . ? C2 C3 H3B 108.5 . . ? C2 C3 C4 115.0(9) . . ? C4 C3 H3A 108.5 . . ? C4 C3 H3B 108.5 . . ? N1 C7 H7A 108.7 . . ? N1 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C6 C7 N1 114.3(6) . . ? C6 C7 H7A 108.7 . . ? C6 C7 H7B 108.7 . . ? N1 C2 C3 120.9(7) . . ? O2 C2 N1 118.4(9) . . ? O2 C2 C3 120.7(8) . . ? O5' C5' C4' 109.6(6) . . ? O5' C5' H5'A 109.8 . . ? O5' C5' H5'B 109.8 . . ? C4' C5' H5'A 109.8 . . ? C4' C5' H5'B 109.8 . . ? H5'A C5' H5'B 108.2 . . ? C24T C25T C26T 122.1(8) . . ? C27T C25T C24T 115.0(9) . . ? C27T C25T C26T 122.7(11) . . ? O3' C3' C4' 109.9(8) . . ? O3' C3' H3' 111.4 . . ? O3' C3' C2' 106.3(6) . . ? C4' C3' H3' 111.4 . . ? C4' C3' C2' 106.3(8) . . ? C2' C3' H3' 111.4 . . ? C22T C28T H28T 119.0 . . ? C27T C28T C22T 122.0(8) . . ? C27T C28T H28T 119.0 . . ? C22T C23T H23T 120.3 . . ? C24T C23T C22T 119.3(8) . . ? C24T C23T H23T 120.3 . . ? C25T C24T H24T 118.3 . . ? C23T C24T C25T 123.4(8) . . ? C23T C24T H24T 118.3 . . ? C7T C2T C1T 118.5(11) . . ? C3T C2T C1T 119.3(12) . . ? C3T C2T C7T 122.2(14) . . ? O5 C5 H5 109.4 . . ? O5 C5 C6 104.0(8) . . ? O5 C5 C4 108.5(8) . . ? C6 C5 H5 109.4 . . ? C6 C5 C4 115.8(8) . . ? C4 C5 H5 109.4 . . ? C7 C6 C5 116.5(9) . . ? C7 C6 H6A 108.2 . . ? C7 C6 H6B 108.2 . . ? C5 C6 H6A 108.2 . . ? C5 C6 H6B 108.2 . . ? H6A C6 H6B 107.3 . . ? C1' C2' C3' 101.0(8) . . ? C1' C2' H2'A 111.6 . . ? C1' C2' H2'B 111.6 . . ? C3' C2' H2'A 111.6 . . ? C3' C2' H2'B 111.6 . . ? H2'A C2' H2'B 109.4 . . ? C3 C4 C5 113.8(7) . . ? C3 C4 H4A 108.8 . . ? C3 C4 H4B 108.8 . . ? C5 C4 H4A 108.8 . . ? C5 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C25T C27T H27T 118.7 . . ? C28T C27T C25T 122.7(10) . . ? C28T C27T H27T 118.7 . . ? O5 C1T C2T 111.5(10) . . ? O5 C1T H1TA 109.3 . . ? O5 C1T H1TB 109.3 . . ? C2T C1T H1TA 109.3 . . ? C2T C1T H1TB 109.3 . . ? H1TA C1T H1TB 108.0 . . ? C25T C26T H26A 109.5 . . ? C25T C26T H26B 109.5 . . ? C25T C26T H26C 109.5 . . ? H26A C26T H26B 109.5 . . ? H26A C26T H26C 109.5 . . ? H26B C26T H26C 109.5 . . ? C13T C12T C11T 118.4(11) . . ? C18T C12T C13T 116.9(10) . . ? C18T C12T C11T 124.6(12) . . ? C2T C7T H7T 122.2 . . ? C2T C7T C6T 115.7(13) . . ? C6T C7T H7T 122.2 . . ? C2T C3T H3T 119.0 . . ? C2T C3T C4T 121.9(15) . . ? C4T C3T H3T 119.0 . . ? C18T C17T H17T 121.7 . . ? C15T C17T H17T 121.7 . . ? C15T C17T C18T 116.6(12) . . ? C7T C6T H6T 119.4 . . ? C5T C6T C7T 121.3(14) . . ? C5T C6T H6T 119.4 . . ? C12T C13T H13T 119.1 . . ? C12T C13T C14T 121.8(14) . . ? C14T C13T H13T 119.1 . . ? C12T C18T C17T 122.5(14) . . ? C12T C18T H18T 118.8 . . ? C17T C18T H18T 118.8 . . ? C3T C4T H4T 120.8 . . ? C5T C4T C3T 118.4(16) . . ? C5T C4T H4T 120.8 . . ? C17T C15T C16T 114(2) . . ? C14T C15T C17T 123.3(11) . . ? C14T C15T C16T 121.2(19) . . ? C6T C5T C4T 120.4(16) . . ? C6T C5T H5T 119.8 . . ? C4T C5T H5T 119.8 . . ? O3' C11T C12T 119.5(10) . . ? O11T C11T O3' 117.8(11) . . ? O11T C11T C12T 122.8(13) . . ? C13T C14T H14T 121.0 . . ? C15T C14T C13T 118.0(15) . . ? C15T C14T H14T 121.0 . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 0.283 0.500 9.6 0.7 ? 2 0.122 0.311 0.087 73.7 15.8 ? 3 -0.122 0.311 0.913 73.7 15.9 ? 4 0.378 0.811 0.413 73.7 15.9 ? 5 0.500 0.783 0.000 9.6 0.7 ? 6 0.622 0.811 0.587 73.7 15.8 ? _shelx_res_file ; TITL hari_se_a.res in I2 hari_se_sx.res created by SHELXL-2017/1 at 21:45:41 on 07-Sep-2022 REM Old TITL hari_se_a.res in I2 REM SHELXT solution in I2 REM R1 0.246, Rweak 0.056, Alpha 0.022, Orientation as input REM Flack x = 0.045 ( 0.286 ) from Parsons' quotients REM Formula found by SHELXT: C30 N2 O6 CELL 1.54187 19.1997 5.3821 32.153 90 98.636 90 ZERR 4 0.002 0.0005 0.0043 0 0.009 0 LATT -2 SYMM -X,+Y,-Z SFAC C H N O UNIT 140 160 4 32 DFIX 1.392 0.01 C22T C28T C27T C25T C24T C23T DFIX 1.392 0.01 C2T C7T C6T C5T C4T C3T DFIX 2.784 0.01 C15T C12T C17T C13T C18T C14T DFIX 1.392 0.01 C12T C18T C17T C15T C14T C13T DFIX 2.784 0.01 C15T C12T DFIX 2.784 0.01 C17T C13T DFIX 2.784 0.01 C18T C14T FLAT O3' O11T C11T C12T FLAT C21T C22T C28T C27T C25T C26T C24T C23T FLAT C22T C21T O21T O5' FLAT C11T C12T C13T C14T C15T C16T C17T C18T FLAT C1T C2T C7T C6T C5T C4T C3T FLAT C1' N1 C2 O2 C3 DELU C11T C12T C18T C17T C15T C16T C14T C13T DELU C1T C2T C7T C6T C5T C4T C3T SIMU 0.1 0.1 2 C12T C18T C17T C15T C16T C14T C13T SIMU 0.1 0.1 2 C1T C2T C7T C6T C5T C4T C3T ISOR C16T C18T C13T C14T C17T C15T L.S. 20 0 0 PLAN 20 BOND $H list 4 ABIN fmap 2 53 acta SHEL 8 0.84 REM REM REM WGHT 0.141000 FVAR 0.33831 O5' 4 0.698058 0.639822 0.302301 11.00000 0.08149 0.10989 = 0.11061 -0.00505 0.01729 -0.01150 O21T 4 0.789780 0.484019 0.275866 11.00000 0.11791 0.10896 = 0.11758 -0.01201 0.03532 -0.00397 O1' 4 0.575388 0.362668 0.319103 11.00000 0.11312 0.10336 = 0.11414 -0.01360 0.02185 -0.00316 O5 4 0.725760 0.332609 0.484719 11.00000 0.12587 0.14857 = 0.11004 0.01047 -0.01027 0.01374 O3' 4 0.476420 0.781066 0.272317 11.00000 0.09567 0.16166 = 0.14454 0.04023 -0.00262 -0.00639 C21T 1 0.767524 0.622998 0.299021 11.00000 0.09772 0.09307 = 0.08879 0.00518 0.01415 -0.00643 N1 3 0.576837 0.428296 0.390502 11.00000 0.08257 0.11571 = 0.14391 -0.00905 0.04296 -0.00064 C1' 1 0.543338 0.509757 0.347686 11.00000 0.08453 0.11143 = 0.10987 0.01543 0.01518 0.00193 AFIX 13 H1' 2 0.492620 0.476136 0.344033 11.00000 -1.20000 AFIX 0 O2 4 0.474261 0.302654 0.406623 11.00000 0.11414 0.26598 = 0.15465 0.03780 0.03276 -0.02569 C4' 1 0.579494 0.505964 0.280630 11.00000 0.09916 0.09546 = 0.11719 -0.00613 0.01166 -0.00493 AFIX 13 H4' 2 0.547830 0.432018 0.257143 11.00000 -1.20000 AFIX 0 C22T 1 0.811505 0.790305 0.327828 11.00000 0.08478 0.10229 = 0.08876 0.00701 0.02000 0.00165 C3 1 0.572272 0.250705 0.459234 11.00000 0.10746 0.12355 = 0.13907 0.01870 0.03742 0.00202 AFIX 23 H3A 2 0.608771 0.130210 0.456262 11.00000 -1.20000 H3B 2 0.537259 0.168308 0.473200 11.00000 -1.20000 AFIX 0 C7 1 0.656381 0.442430 0.400871 11.00000 0.06398 0.11547 = 0.12450 0.00905 0.01667 0.00103 AFIX 23 H7A 2 0.674318 0.278988 0.409515 11.00000 -1.20000 H7B 2 0.675324 0.486908 0.375558 11.00000 -1.20000 AFIX 0 C2 1 0.539193 0.326043 0.417516 11.00000 0.07793 0.16046 = 0.12257 0.00070 0.02516 -0.01982 C5' 1 0.652849 0.493886 0.271648 11.00000 0.10428 0.12105 = 0.10200 -0.02590 0.01916 -0.01774 AFIX 23 H5'A 2 0.668763 0.322631 0.272757 11.00000 -1.20000 H5'B 2 0.654901 0.557441 0.243628 11.00000 -1.20000 AFIX 0 C25T 1 0.900014 1.113124 0.382411 11.00000 0.11207 0.11876 = 0.12617 0.02051 -0.00811 -0.01757 C3' 1 0.552053 0.759530 0.290296 11.00000 0.08942 0.09937 = 0.12736 0.01736 -0.00052 -0.00763 AFIX 13 H3' 2 0.579963 0.892367 0.280029 11.00000 -1.20000 AFIX 0 C28T 1 0.784832 0.978026 0.351794 11.00000 0.09020 0.13608 = 0.11301 0.01612 0.01244 -0.00973 AFIX 43 H28T 2 0.736342 0.992861 0.350758 11.00000 -1.20000 AFIX 0 C23T 1 0.884964 0.763831 0.332412 11.00000 0.09021 0.11031 = 0.12365 0.00664 0.01548 0.00288 AFIX 43 H23T 2 0.904952 0.636745 0.318558 11.00000 -1.20000 AFIX 0 C24T 1 0.926946 0.927035 0.357497 11.00000 0.08820 0.16363 = 0.14822 0.00478 0.00538 -0.00949 AFIX 43 H24T 2 0.975476 0.915999 0.358334 11.00000 -1.20000 AFIX 0 C2T 1 0.809882 0.091494 0.530869 11.00000 0.10108 0.18255 = 0.14935 0.03428 -0.01868 -0.01950 C5 1 0.678650 0.544229 0.478237 11.00000 0.14297 0.10551 = 0.11685 -0.00563 0.00084 0.00614 AFIX 13 H5 2 0.696658 0.677999 0.497588 11.00000 -1.20000 AFIX 0 C6 1 0.682339 0.622489 0.434276 11.00000 0.11897 0.11807 = 0.13605 -0.00026 0.00999 -0.00469 AFIX 23 H6A 2 0.655555 0.774892 0.428825 11.00000 -1.20000 H6B 2 0.731039 0.660821 0.432137 11.00000 -1.20000 AFIX 0 C2' 1 0.555521 0.771407 0.337883 11.00000 0.09319 0.12093 = 0.10839 0.00619 0.01364 -0.00152 AFIX 23 H2'A 2 0.601241 0.828250 0.351524 11.00000 -1.20000 H2'B 2 0.519118 0.878411 0.345908 11.00000 -1.20000 AFIX 0 C4 1 0.604980 0.462374 0.487402 11.00000 0.12428 0.11882 = 0.12748 0.01063 0.03831 0.03130 AFIX 23 H4A 2 0.609056 0.410115 0.516540 11.00000 -1.20000 H4B 2 0.573528 0.604334 0.483757 11.00000 -1.20000 AFIX 0 C27T 1 0.827476 1.136114 0.376090 11.00000 0.10865 0.13533 = 0.11440 -0.01626 0.01202 -0.02022 AFIX 43 H27T 2 0.807310 1.266121 0.389158 11.00000 -1.20000 AFIX 0 C1T 1 0.753704 0.283403 0.527433 11.00000 0.14894 0.18260 = 0.17237 -0.00538 0.00828 0.00392 AFIX 23 H1TA 2 0.716147 0.227067 0.542220 11.00000 -1.20000 H1TB 2 0.772859 0.435533 0.540716 11.00000 -1.20000 AFIX 0 C26T 1 0.947161 1.285250 0.409988 11.00000 0.14717 0.13805 = 0.16237 -0.03645 -0.02572 -0.03055 AFIX 137 H26A 2 0.983163 1.191207 0.427069 11.00000 -1.50000 H26B 2 0.920084 1.375336 0.427772 11.00000 -1.50000 H26C 2 0.968594 1.400042 0.392880 11.00000 -1.50000 AFIX 0 C12T 1 0.384385 0.853306 0.218480 11.00000 0.11107 0.22356 = 0.13843 0.00167 0.00080 0.01203 C7T 1 0.838195 0.029965 0.495162 11.00000 0.15268 0.17090 = 0.20406 0.05127 0.02461 0.04473 AFIX 43 H7T 2 0.824070 0.107688 0.469446 11.00000 -1.20000 AFIX 0 C3T 1 0.829116 -0.021859 0.567285 11.00000 0.13132 0.24736 = 0.15597 0.04841 -0.01708 -0.00739 AFIX 43 H3T 2 0.807922 0.023874 0.590314 11.00000 -1.20000 AFIX 0 C17T 1 0.280610 0.958975 0.167041 11.00000 0.20649 0.40260 = 0.17193 0.03266 -0.06733 0.05185 AFIX 43 H17T 2 0.260381 1.048866 0.143604 11.00000 -1.20000 AFIX 0 C6T 1 0.889984 -0.158637 0.500249 11.00000 0.19216 0.20856 = 0.20269 0.06642 0.02837 0.07214 AFIX 43 H6T 2 0.909844 -0.210838 0.477073 11.00000 -1.20000 AFIX 0 C13T 1 0.341457 0.684101 0.236003 11.00000 0.14329 0.51892 = 0.35197 0.20457 -0.08274 -0.10101 AFIX 43 H13T 2 0.361849 0.577205 0.257106 11.00000 -1.20000 AFIX 0 C18T 1 0.353731 0.985103 0.184215 11.00000 0.16775 0.47622 = 0.17485 0.10041 -0.01665 0.03401 AFIX 43 H18T 2 0.381254 1.095835 0.171549 11.00000 -1.20000 AFIX 0 C4T 1 0.879428 -0.204967 0.572082 11.00000 0.16979 0.22486 = 0.19423 0.08147 -0.01631 -0.01547 AFIX 43 H4T 2 0.891430 -0.285861 0.597715 11.00000 -1.20000 AFIX 0 C15T 1 0.241700 0.792675 0.187224 11.00000 0.17536 0.33186 = 0.28291 0.00289 -0.08801 0.00764 C5T 1 0.911348 -0.265297 0.538378 11.00000 0.16930 0.16250 = 0.24125 0.07018 -0.01362 0.03536 AFIX 43 H5T 2 0.947965 -0.380092 0.541453 11.00000 -1.20000 AFIX 0 C11T 1 0.456098 0.867306 0.235740 11.00000 0.11209 0.17509 = 0.13476 0.03814 0.01201 -0.00736 O11T 4 0.497502 0.951732 0.218175 11.00000 0.14353 0.50337 = 0.20341 0.16670 -0.01645 -0.02577 C14T 1 0.267985 0.671604 0.222452 11.00000 0.15400 0.50774 = 0.47293 0.22842 -0.12571 -0.11926 AFIX 43 H14T 2 0.238807 0.581922 0.237570 11.00000 -1.20000 AFIX 0 C16T 1 0.160278 0.807468 0.172208 11.00000 0.16288 0.61664 = 0.40284 -0.01127 -0.12863 0.02190 HKLF 4 REM hari_se_a.res in I2 REM R1 = 0.0693 for 1774 Fo > 4sig(Fo) and 0.1303 for all 4270 data REM 380 parameters refined using 187 restraints END WGHT 0.1408 0.0000 REM Highest difference peak 0.155, deepest hole -0.173, 1-sigma level 0.043 Q1 1 0.1609 0.8030 0.1304 11.00000 0.05 0.15 Q2 1 0.3926 0.2376 0.4046 11.00000 0.05 0.15 Q3 1 0.8971 1.4595 0.3827 11.00000 0.05 0.15 Q4 1 0.3510 0.8432 0.1813 11.00000 0.05 0.15 Q5 1 0.5592 1.1342 0.3613 11.00000 0.05 0.14 Q6 1 0.6927 0.8610 0.3582 11.00000 0.05 0.14 Q7 1 0.2865 0.8797 0.1737 11.00000 0.05 0.14 Q8 1 0.7346 0.7352 0.3629 11.00000 0.05 0.13 Q9 1 0.6981 0.9497 0.3000 11.00000 0.05 0.13 Q10 1 0.6336 0.8957 0.3429 11.00000 0.05 0.13 Q11 1 0.6958 0.2828 0.4224 11.00000 0.05 0.13 Q12 1 0.6398 1.0104 0.3455 11.00000 0.05 0.12 Q13 1 0.5585 0.8446 0.4015 11.00000 0.05 0.12 Q14 1 0.9037 1.2391 0.3185 11.00000 0.05 0.12 Q15 1 0.5442 0.7795 0.4054 11.00000 0.05 0.11 Q16 1 0.8033 0.3727 0.4881 11.00000 0.05 0.11 Q17 1 0.4475 0.9910 0.3155 11.00000 0.05 0.11 Q18 1 0.1912 0.4662 0.1774 11.00000 0.05 0.11 Q19 1 0.7317 0.9578 0.3020 11.00000 0.05 0.11 Q20 1 0.4195 1.2786 0.1602 11.00000 0.05 0.11 ; _shelx_res_checksum 54903 _shelx_hkl_file ; 1 0 -1 80.03 2.08 1 0 -1 90.11 2.34 -1 0 1 86.36 2.24 -1 0 1 83.49 2.18 0 0 2 553.04 22.41 0 0 -2 616.88 24.82 1 0 1 1782.28 116.22 1 0 1 1890.62 108.67 -1 0 -1 1773.15 101.15 -1 0 -1 1884.85 107.61 -1 0 -1 1776.78 111.73 -1 0 3 150.96 4.58 1 0 -3 141.43 4.25 1 0 -3 149.54 4.88 -1 0 3 137.74 4.58 2 0 0 136.65 4.22 2 0 0 122.45 4.61 -2 0 0 127.23 4.48 -2 0 0 133.55 4.12 2 0 -2 808.97 37.87 2 0 -2 854.39 39.78 -2 0 2 849.25 39.55 -2 0 2 860.55 40.01 -1 0 -3 18.66 0.66 1 0 3 18.00 0.89 0 0 4 852.78 40.54 0 0 -4 842.92 40.38 -2 0 -2 101.68 3.33 -2 0 -2 92.29 7.28 2 0 2 116.48 4.35 2 0 2 111.70 10.48 2 0 -4 767.01 36.88 -2 0 4 790.32 37.24 2 0 -4 738.34 34.18 -2 0 4 747.47 36.55 -3 0 1 20.63 1.55 -3 0 1 19.58 0.92 3 0 -1 19.61 1.32 3 0 -1 19.31 0.92 1 0 -5 260.81 9.59 -1 0 5 295.85 11.44 1 0 -5 296.74 11.21 -1 0 5 289.36 10.71 3 0 1 1807.76 111.14 3 0 1 2099.13 149.80 -3 0 -1 1940.76 126.07 -3 0 -1 2177.67 137.87 -3 0 -1 1880.44 116.05 -3 0 3 1454.99 82.00 -3 0 3 1531.13 86.22 3 0 -3 1380.80 78.38 3 0 -3 1538.71 87.94 -1 0 -5 532.50 23.04 1 0 5 527.62 23.40 -2 0 -4 176.60 19.08 2 0 4 227.03 9.33 0 -1 1 582.01 28.77 0 1 -1 604.26 27.46 0 1 1 569.42 25.68 0 1 1 625.85 28.44 0 -1 -1 616.75 25.94 0 0 -6 128.35 4.85 0 0 6 121.42 5.60 1 1 0 1588.84 91.56 -1 -1 0 1711.68 101.85 -1 -1 0 1848.14 117.93 -1 1 0 1700.71 95.25 1 -1 0 1620.28 102.41 -1 1 0 1730.27 104.78 -1 1 0 1730.50 106.10 1 -1 0 1818.77 102.24 3 0 3 51.25 13.09 -3 0 -3 61.80 3.13 -3 0 -3 61.80 3.39 3 0 3 56.43 2.83 -3 0 -3 72.22 6.66 1 1 -2 2152.69 137.34 -1 -1 2 2224.54 134.15 1 1 -2 2263.99 151.42 -1 -1 2 2160.70 140.21 1 -1 -2 2221.21 138.89 1 -1 -2 2239.54 144.86 -1 1 2 2339.80 155.74 -1 1 2 2171.15 139.62 -2 0 6 9793.63 1001.56 2 0 -6 9181.49 935.34 2 0 -6 8907.03 900.54 -2 0 6 9999.00 1013.82 -1 1 -2 1339.76 68.95 -1 1 -2 1423.45 82.33 1 -1 2 1463.86 86.78 -3 0 5 1672.46 97.86 -3 0 5 1576.97 96.74 3 0 -5 1574.27 94.27 1 1 2 1487.55 80.36 1 1 2 1508.39 82.07 0 -1 3 763.36 40.94 0 1 -3 791.37 40.61 0 1 -3 827.17 35.17 0 1 -3 872.72 42.95 0 -1 -3 874.69 41.73 0 1 3 845.76 40.41 0 -1 -3 818.20 38.46 -4 0 2 1412.83 81.28 -4 0 2 1402.81 81.71 4 0 -2 1484.69 86.26 4 0 -2 1427.57 84.71 -4 0 0 116.05 5.21 -4 0 0 103.69 4.81 4 0 0 119.12 7.15 4 0 0 104.02 4.12 2 1 -1 1781.92 128.35 2 1 -1 1478.26 85.10 -2 -1 1 1596.19 93.84 -2 -1 1 1608.81 93.87 2 -1 -1 1586.57 95.95 2 -1 -1 1595.27 90.38 -2 1 1 1681.69 104.42 -2 1 1 1566.10 93.84 -2 1 1 1594.74 89.35 2 1 1 2228.69 134.35 -2 -1 -1 2035.98 144.20 -2 -1 -1 2107.93 126.50 2 -1 1 2244.12 145.35 2 -1 1 2189.24 150.17 -2 1 -1 2073.72 136.98 -2 1 -1 2140.92 142.35 -2 1 -1 2138.29 130.82 -1 0 7 87.61 3.69 1 0 -7 96.51 3.82 1 0 -7 87.97 3.49 -1 -1 4 3671.75 285.24 -1 -1 4 3680.65 266.05 1 1 -4 3661.01 276.80 1 1 -4 3815.69 276.17 1 -1 -4 3777.59 286.62 1 -1 -4 3715.95 275.65 -1 1 4 3762.46 284.31 -2 -1 3 225.91 9.99 2 1 -3 231.91 8.80 2 1 -3 226.01 9.76 -2 -1 3 212.79 7.38 2 -1 -3 235.53 9.95 -2 1 3 231.45 9.39 -2 1 3 222.84 8.08 2 -1 -3 228.81 8.37 -4 0 4 2264.23 150.53 -4 0 4 2363.50 155.54 4 0 -4 2383.74 158.54 4 0 -4 2334.43 155.01 -4 0 -2 378.78 18.46 4 0 2 391.10 17.07 4 0 2 354.68 26.10 -4 0 -2 388.14 20.07 -4 0 -2 380.85 16.25 2 0 6 271.53 11.57 -2 0 -6 317.80 12.92 1 0 7 343.48 16.15 -1 0 -7 348.88 14.60 1 -1 4 665.23 34.31 -1 1 -4 710.26 36.92 1 1 4 739.00 32.50 -1 -1 -4 754.72 33.85 -3 0 -5 486.75 21.16 -3 0 -5 397.30 33.55 3 0 5 386.19 18.79 -2 1 -3 507.91 23.04 -2 1 -3 544.07 26.27 2 -1 3 522.09 28.58 -2 -1 -3 483.33 40.28 0 1 -5 1744.64 99.24 0 1 -5 1794.58 112.29 0 -1 5 1766.50 111.67 0 -1 -5 1752.16 103.99 0 1 5 1760.93 102.77 0 -1 -5 1787.89 106.96 3 1 0 1291.34 98.91 -3 -1 0 1254.23 77.65 -3 -1 0 1458.85 81.58 3 1 0 1561.09 85.80 3 -1 0 1469.69 90.28 3 -1 0 1623.02 97.89 -3 1 0 1496.06 93.87 -3 1 0 1452.09 90.15 -3 1 0 1514.85 86.69 -3 -1 2 774.73 38.17 -3 -1 2 831.91 41.07 3 1 -2 892.89 50.76 3 1 -2 827.69 40.51 3 -1 -2 844.73 44.50 3 -1 -2 821.07 40.24 -3 1 2 820.34 39.49 -3 1 2 931.85 53.69 -3 1 2 811.77 42.19 -3 0 7 18.03 1.25 -3 0 7 19.84 1.68 3 0 -7 19.94 1.68 0 0 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18 1 9 0.1216 -0.3699 18 1 11 -0.0014 -0.0384 18 1 13 -0.0717 -0.0285 18 1 15 0.1095 0.0564 18 1 17 0.3608 0.2822 18 2 0 -0.6441 0.3257 18 2 2 0.0296 -0.0526 18 2 4 -0.1237 -0.1087 18 2 6 -0.0927 0.0823 18 2 8 0.2679 0.4600 18 2 10 0.2602 0.6233 18 2 12 0.1227 0.1495 18 3 1 -0.1913 -0.0829 18 3 3 -0.2832 0.0357 18 3 5 0.3956 -0.2182 18 3 7 0.3029 0.4030 18 3 9 -0.3200 0.6952 19 -2 -15 -0.3814 0.0983 19 -2 -13 -0.2652 0.5104 19 -2 -11 -0.5156 0.2905 19 -2 -9 -0.5354 0.2119 19 -2 -7 0.6079 0.6034 19 -2 -5 0.7146 0.1594 19 -2 -3 -0.5175 -0.6842 19 -2 -1 -0.4524 -0.3930 19 -1 -24 -0.7629 0.3096 19 -1 -22 0.1984 0.3263 19 -1 -20 0.5837 -0.3581 19 -1 -18 0.3162 -0.6197 19 -1 -16 0.1479 -0.2528 19 -1 -14 -0.1436 -0.0046 19 -1 -12 -0.0002 -0.0399 19 -1 -10 0.6193 -0.2912 19 -1 -8 0.4060 0.1169 19 -1 -6 -0.2754 0.6895 19 -1 -4 -0.1166 0.1112 19 -1 -2 0.1690 -0.5498 19 0 1 1.2845 0.0011 19 0 3 0.2467 -0.0053 19 0 5 -1.5550 -0.0081 19 0 7 -1.3508 -0.0049 19 0 9 -0.3228 0.0009 19 0 11 -0.0355 0.0020 19 0 13 0.0672 -0.0007 19 0 15 0.0185 -0.0016 19 1 0 -0.1604 0.5727 19 1 2 -0.0310 0.2202 19 1 4 0.6126 -0.6405 19 1 6 0.5687 -0.8502 19 1 8 0.1230 -0.1929 19 1 10 0.0595 -0.0474 19 1 12 0.1985 -0.1790 19 1 14 0.4480 0.0205 19 2 1 0.3078 -0.3375 19 2 3 0.2009 -0.2725 19 2 5 0.0442 0.1084 19 2 7 0.1872 0.2751 19 2 9 0.1860 0.1823 19 3 0 -0.1219 -0.2377 19 3 2 -0.1433 0.2179 19 3 4 0.2386 -0.0028 19 3 6 0.2330 0.3137 20 -2 -14 -0.3465 0.2703 20 -2 -12 -0.2270 0.3295 20 -2 -10 -0.4528 0.1528 20 -2 -8 0.0324 0.4577 20 -2 -6 0.2600 0.0010 20 -2 -4 -0.4433 -0.9242 20 -2 -2 -0.2903 -0.4991 20 -1 -17 0.2065 -0.1711 20 -1 -15 0.0594 0.0433 20 -1 -13 -0.0899 0.1780 20 -1 -11 0.2916 0.0962 20 -1 -9 0.1302 -0.0009 20 -1 -7 -0.4163 0.2530 20 -1 -5 -0.0440 0.2008 20 -1 -3 0.4281 0.0495 20 -1 -1 -0.0156 0.0222 20 0 0 1.2573 0.0027 20 0 2 0.4271 -0.0006 20 0 4 -1.3310 -0.0065 20 0 6 -1.0919 -0.0076 20 0 8 -0.0108 -0.0020 20 0 10 -0.0057 0.0016 20 0 12 -0.0698 0.0003 20 1 1 -0.2154 0.0164 20 1 3 0.2868 -0.4751 20 1 5 0.2742 -0.6466 20 1 7 -0.1494 -0.0731 20 1 9 -0.1140 -0.0653 20 1 11 0.1376 -0.2240 20 2 0 0.3836 -0.4493 20 2 2 0.2146 -0.2736 20 2 4 -0.0687 0.2534 20 2 6 -0.0261 0.2405 21 -2 -11 -0.2145 0.1021 21 -2 -9 -0.2030 0.2739 21 -2 -7 0.1679 -0.0552 21 -2 -5 0.0301 -0.9369 21 -2 -3 0.2155 -0.5238 21 -2 -1 0.6105 0.4856 21 -1 -14 -0.0144 0.2169 21 -1 -12 0.1433 0.1842 21 -1 -10 0.0509 -0.3616 21 -1 -8 -0.3688 -0.4386 21 -1 -6 0.0771 -0.0133 21 -1 -4 0.6027 0.2943 21 -1 -2 0.0598 0.1637 21 0 1 0.3197 0.0044 21 0 3 -1.1225 -0.0034 21 0 5 -0.9501 -0.0075 21 0 7 0.0487 -0.0035 21 0 9 -0.0680 0.0008 21 1 0 -0.3940 0.3123 21 1 2 -0.0079 0.1601 21 1 4 0.1121 -0.1831 21 1 6 -0.1289 0.0630 21 1 8 0.0493 -0.0649 21 2 1 0.2653 -0.3187 22 -1 -13 -0.0181 0.4207 22 -1 -11 0.0297 -0.2280 22 -1 -9 -0.2231 -0.4299 22 -1 -7 0.1898 0.3202 22 -1 -5 0.6464 0.8781 22 -1 -3 0.0660 0.5873 22 -1 -1 -0.5065 -0.2202 22 0 0 0.7662 0.0062 22 0 2 -0.3685 -0.0010 22 0 4 -0.4689 -0.0063 22 1 1 -0.2396 0.3267 0 0 0 0.0 0.0 ; _shelx_fab_checksum 86115 _olex2_submission_special_instructions 'No special instructions were received' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_hari_0m _database_code_depnum_ccdc_archive 'CCDC 2207174' loop_ _audit_author_name _audit_author_address 'Geoffrey Jameson' ;School of Natural Sciences, Massey University New Zealand ; _audit_update_record ; 2022-09-14 deposited with the CCDC. 2023-05-23 downloaded from the CCDC. ; _audit_creation_date 2022-09-07 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2017/1 _chemical_name_common ? _chemical_name_systematic '1-[2-deoxy-3,5-bis-O-(4-methylbenzoyl)-\b-D-erythro-pentofuranosyl]-(S)-5-benzyloxyazepan-2-one ' _chemical_formula_moiety 'C34 H37 N O7' _chemical_formula_sum 'C34 H37 N O7' _chemical_formula_weight 571.64 _chemical_absolute_configuration rmad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_H-M_alt 'C 1 2 1' _space_group_name_Hall 'C 2y' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 33.3058(16) _cell_length_b 5.5217(3) _cell_length_c 17.9538(8) _cell_angle_alpha 90 _cell_angle_beta 106.418(2) _cell_angle_gamma 90 _cell_volume 3167.2(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9873 _cell_measurement_temperature 150.0 _cell_measurement_theta_max 58.810 _cell_measurement_theta_min 2.566 _shelx_estimated_absorpt_T_max 0.993 _shelx_estimated_absorpt_T_min 0.876 _exptl_absorpt_coefficient_mu 0.680 _exptl_absorpt_correction_T_max 0.7516 _exptl_absorpt_correction_T_min 0.6311 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1035 before and 0.0444 after correction. The Ratio of minimum to maximum transmission is 0.8397. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier . _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 1216 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_unetI/netI 0.0332 _diffrn_reflns_Laue_measured_fraction_full 0.986 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 18253 _diffrn_reflns_point_group_measured_fraction_full 0.968 _diffrn_reflns_point_group_measured_fraction_max 0.968 _diffrn_reflns_theta_full 59.414 _diffrn_reflns_theta_max 59.414 _diffrn_reflns_theta_min 2.566 _diffrn_ambient_temperature 150.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'Micro-focus sealed source' _reflns_Friedel_coverage 0.751 _reflns_Friedel_fraction_full 0.945 _reflns_Friedel_fraction_max 0.945 _reflns_number_gt 4102 _reflns_number_total 4471 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _atom_sites_solution_primary . _refine_diff_density_max 0.765 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.059 _refine_ls_abs_structure_details ; Flack x determined using 1573 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.02(9) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 381 _refine_ls_number_reflns 4471 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0536 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0935P)^2^+2.5551P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1439 _refine_ls_wR_factor_ref 0.1481 _refine_special_details ; Residual positive electron density (0.76 e A^-3^)was concentrated near the phenyl ring undergoing substantial torsional motion about C5-O5 and C1T-C2T bonds, leading to Alert B for Hirshfeld Tests. Absolute structure was determined by Flack x (-0.02(9) and Hooft y (0.04(8) parameters. The expected beta-D-2-deoxyribose was observed, establishing the S-diasteromer at nucleobase atom C5. The data:parameter ratio is 6.70, partly due to chiral space group and partly due to data cutoff in processing at sine(theta_max)/wavelength of 0.5584 A^-1^. Four reflections were jected for poor agreement of Fcalc and Fobs. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C3'(H3'), C4'(H4'), C1'(H1'), C5(H5) 2.b Secondary CH2 refined with riding coordinates: C2'(H2'A,H2'B), C7(H7A,H7B), C4(H4A,H4B), C6(H6A,H6B), C5'(H5'A,H5'B), C3(H3A, H3B), C1T(H1TA,H1TB) 2.c Aromatic/amide H refined with riding coordinates: C18T(H18T), C17T(H17T), C13T(H13T), C28T(H28T), C14T(H14T), C23T(H23T), C24T(H24T), C27T(H27T), C7T(H7T), C4T(H4T), C5T(H5T), C3T(H3T), C6T(H6T) 2.d Idealised Me refined as rotating group: C16T(H16A,H16B,H16C), C26T(H26A,H26B,H26C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O3' O 0.74601(8) 0.0105(5) 0.22987(15) 0.0296(7) Uani 1 1 d . . . . . O5' O 0.68916(8) -0.0348(6) 0.41864(15) 0.0334(7) Uani 1 1 d . . . . . O1' O 0.66652(8) -0.2045(5) 0.26164(16) 0.0343(7) Uani 1 1 d . . . . . O11T O 0.77523(10) 0.3801(6) 0.24439(17) 0.0404(8) Uani 1 1 d . . . . . O5 O 0.51760(10) 0.6260(6) 0.19243(19) 0.0424(8) Uani 1 1 d . . . . . O2 O 0.60686(10) -0.0504(7) 0.06171(17) 0.0470(9) Uani 1 1 d . . . . . O21T O 0.72042(10) -0.1636(7) 0.53978(17) 0.0467(9) Uani 1 1 d . . . . . N1 N 0.61280(10) 0.0443(7) 0.18746(19) 0.0318(8) Uani 1 1 d . . . . . C12T C 0.78664(12) 0.1124(8) 0.1472(2) 0.0284(9) Uani 1 1 d . . . . . C11T C 0.76950(12) 0.1851(8) 0.2117(2) 0.0302(10) Uani 1 1 d . . . . . C3' C 0.72500(12) 0.0621(8) 0.2890(2) 0.0282(9) Uani 1 1 d . . . . . H3' H 0.743602 0.145117 0.335586 0.034 Uiso 1 1 calc R . . . . C2 C 0.59041(13) 0.0174(9) 0.1110(2) 0.0353(10) Uani 1 1 d . . . . . C2' C 0.68517(12) 0.2006(8) 0.2531(2) 0.0281(9) Uani 1 1 d . . . . . H2'A H 0.689462 0.328740 0.217501 0.034 Uiso 1 1 calc R . . . . H2'B H 0.673706 0.273677 0.293084 0.034 Uiso 1 1 calc R . . . . C4' C 0.70956(12) -0.1843(8) 0.3083(2) 0.0307(9) Uani 1 1 d . . . . . H4' H 0.726288 -0.313559 0.291901 0.037 Uiso 1 1 calc R . . . . C18T C 0.77478(13) -0.1023(8) 0.1065(2) 0.0334(10) Uani 1 1 d . . . . . H18T H 0.756973 -0.213242 0.122286 0.040 Uiso 1 1 calc R . . . . C1' C 0.65720(12) -0.0013(8) 0.2092(2) 0.0290(9) Uani 1 1 d . . . . . H1' H 0.665738 -0.041523 0.161549 0.035 Uiso 1 1 calc R . . . . C17T C 0.78897(14) -0.1539(9) 0.0429(2) 0.0368(10) Uani 1 1 d . . . . . H17T H 0.780692 -0.300583 0.015123 0.044 Uiso 1 1 calc R . . . . C15T C 0.81519(13) 0.0056(9) 0.0189(2) 0.0359(10) Uani 1 1 d . . . . . C21T C 0.69682(13) -0.0279(9) 0.4964(2) 0.0345(11) Uani 1 1 d . . . . . C13T C 0.81368(14) 0.2711(8) 0.1246(2) 0.0363(10) Uani 1 1 d . . . . . H13T H 0.822284 0.417149 0.152535 0.044 Uiso 1 1 calc R . . . . C5 C 0.53401(14) 0.3875(9) 0.1888(3) 0.0377(11) Uani 1 1 d . . . . . H5 H 0.514200 0.268173 0.201092 0.045 Uiso 1 1 calc R . . . . C7 C 0.59289(13) 0.0982(9) 0.2491(2) 0.0358(11) Uani 1 1 d . . . . . H7A H 0.613506 0.068758 0.300075 0.043 Uiso 1 1 calc R . . . . H7B H 0.569344 -0.015829 0.244271 0.043 Uiso 1 1 calc R . . . . C4 C 0.53512(14) 0.3439(10) 0.1061(3) 0.0416(11) Uani 1 1 d . . . . . H4A H 0.556548 0.451116 0.094938 0.050 Uiso 1 1 calc R . . . . H4B H 0.507667 0.389510 0.070293 0.050 Uiso 1 1 calc R . . . . C6 C 0.57642(13) 0.3557(9) 0.2479(2) 0.0372(11) Uani 1 1 d . . . . . H6A H 0.574075 0.397299 0.300148 0.045 Uiso 1 1 calc R . . . . H6B H 0.596659 0.468988 0.235526 0.045 Uiso 1 1 calc R . . . . C5' C 0.71248(13) -0.2212(9) 0.3925(2) 0.0343(10) Uani 1 1 d . . . . . H5'A H 0.701095 -0.382295 0.399798 0.041 Uiso 1 1 calc R . . . . H5'B H 0.742168 -0.215575 0.423789 0.041 Uiso 1 1 calc R . . . . C28T C 0.64715(15) 0.3297(10) 0.4713(3) 0.0454(12) Uani 1 1 d . . . . . H28T H 0.643739 0.317292 0.417104 0.054 Uiso 1 1 calc R . . . . C22T C 0.67287(13) 0.1681(10) 0.5217(2) 0.0399(11) Uani 1 1 d . . . . . C3 C 0.54487(14) 0.0814(9) 0.0895(3) 0.0400(11) Uani 1 1 d . . . . . H3A H 0.530770 -0.027473 0.117980 0.048 Uiso 1 1 calc R . . . . H3B H 0.532643 0.049756 0.033331 0.048 Uiso 1 1 calc R . . . . C14T C 0.82783(15) 0.2145(9) 0.0616(3) 0.0403(11) Uani 1 1 d . . . . . H14T H 0.846679 0.321477 0.047103 0.048 Uiso 1 1 calc R . . . . C16T C 0.82914(17) -0.0497(10) -0.0525(3) 0.0503(13) Uani 1 1 d . . . . . H16A H 0.835478 -0.222758 -0.053623 0.076 Uiso 1 1 calc GR . . . . H16B H 0.854246 0.044917 -0.051045 0.076 Uiso 1 1 calc GR . . . . H16C H 0.806721 -0.007090 -0.099150 0.076 Uiso 1 1 calc GR . . . . C23T C 0.67806(15) 0.1905(12) 0.6020(3) 0.0528(14) Uani 1 1 d . . . . . H23T H 0.696103 0.082107 0.637129 0.063 Uiso 1 1 calc R . . . . C24T C 0.65754(18) 0.3654(13) 0.6298(3) 0.0614(17) Uani 1 1 d . . . . . H24T H 0.661101 0.376409 0.684077 0.074 Uiso 1 1 calc R . . . . C25T C 0.6316(2) 0.5275(13) 0.5803(4) 0.0667(19) Uani 1 1 d . . . . . C27T C 0.62637(18) 0.5092(12) 0.4992(3) 0.0605(15) Uani 1 1 d . . . . . H27T H 0.608704 0.619814 0.464349 0.073 Uiso 1 1 calc R . . . . C7T C 0.4475(2) 0.9038(14) 0.1594(5) 0.078(2) Uani 1 1 d . . . . . H7T H 0.452568 0.799745 0.120870 0.093 Uiso 1 1 calc R . . . . C4T C 0.4275(2) 1.1500(15) 0.2707(4) 0.079(2) Uani 1 1 d . . . . . H4T H 0.419902 1.215783 0.313720 0.094 Uiso 1 1 calc R . . . . C5T C 0.4083(2) 1.2355(17) 0.1995(6) 0.096(3) Uani 1 1 d . . . . . H5T H 0.389870 1.370210 0.191392 0.116 Uiso 1 1 calc R . . . . C2T C 0.4666(2) 0.8644(14) 0.2316(6) 0.085(2) Uani 1 1 d . . . . . C26T C 0.6087(3) 0.7219(15) 0.6110(5) 0.093(2) Uani 1 1 d . . . . . H26A H 0.583190 0.653976 0.619401 0.139 Uiso 1 1 calc GR . . . . H26B H 0.601373 0.854540 0.573317 0.139 Uiso 1 1 calc GR . . . . H26C H 0.626827 0.783699 0.660277 0.139 Uiso 1 1 calc GR . . . . C3T C 0.4559(3) 0.9821(19) 0.2838(6) 0.110(3) Uani 1 1 d . . . . . H3T H 0.469837 0.944282 0.336385 0.132 Uiso 1 1 calc R . . . . C6T C 0.4178(2) 1.107(2) 0.1353(4) 0.119(4) Uani 1 1 d . . . . . H6T H 0.405921 1.151247 0.082534 0.143 Uiso 1 1 calc R . . . . C1T C 0.5007(3) 0.6621(17) 0.2533(5) 0.102(3) Uani 1 1 d . . . . . H1TA H 0.523048 0.710534 0.300261 0.122 Uiso 1 1 calc R . . . . H1TB H 0.488065 0.509599 0.264947 0.122 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 O3' 0.0370(15) 0.0248(16) 0.0294(14) -0.0027(12) 0.0134(12) -0.0027(13) O5' 0.0347(15) 0.0395(19) 0.0252(14) 0.0053(13) 0.0072(11) 0.0029(13) O1' 0.0338(15) 0.0259(17) 0.0381(16) 0.0035(13) 0.0020(12) -0.0005(13) O11T 0.0540(18) 0.0323(19) 0.0386(17) -0.0087(14) 0.0193(14) -0.0086(15) O5 0.0426(17) 0.035(2) 0.0553(19) -0.0015(15) 0.0230(15) 0.0003(15) O2 0.0478(18) 0.058(2) 0.0305(16) -0.0074(16) 0.0040(14) 0.0062(17) O21T 0.0485(18) 0.054(2) 0.0330(16) 0.0131(17) 0.0048(14) 0.0013(18) N1 0.0300(17) 0.033(2) 0.0286(17) -0.0027(15) 0.0027(14) 0.0006(16) C12T 0.032(2) 0.026(2) 0.027(2) -0.0019(17) 0.0073(16) 0.0010(18) C11T 0.031(2) 0.032(3) 0.026(2) -0.001(2) 0.0054(17) -0.003(2) C3' 0.033(2) 0.026(2) 0.0248(19) -0.0044(17) 0.0079(16) 0.0004(18) C2 0.039(2) 0.030(3) 0.032(2) -0.002(2) 0.0022(19) -0.004(2) C2' 0.035(2) 0.024(2) 0.0238(19) -0.0025(18) 0.0059(17) 0.0001(18) C4' 0.031(2) 0.027(2) 0.031(2) 0.0013(19) 0.0036(17) 0.0008(19) C18T 0.038(2) 0.027(2) 0.037(2) -0.0011(19) 0.0127(18) -0.002(2) C1' 0.033(2) 0.025(2) 0.027(2) 0.0024(18) 0.0041(16) 0.0015(18) C17T 0.047(2) 0.031(3) 0.032(2) -0.006(2) 0.0102(19) 0.002(2) C15T 0.042(2) 0.035(3) 0.033(2) 0.002(2) 0.0142(19) 0.008(2) C21T 0.030(2) 0.044(3) 0.027(2) 0.005(2) 0.0044(18) -0.009(2) C13T 0.046(2) 0.030(3) 0.035(2) -0.0027(19) 0.014(2) -0.001(2) C5 0.035(2) 0.032(3) 0.048(3) 0.000(2) 0.0139(19) -0.002(2) C7 0.036(2) 0.041(3) 0.030(2) 0.002(2) 0.0070(18) -0.004(2) C4 0.039(2) 0.041(3) 0.041(2) 0.003(2) 0.0054(19) 0.006(2) C6 0.039(2) 0.036(3) 0.038(2) -0.008(2) 0.0131(19) -0.007(2) C5' 0.035(2) 0.032(3) 0.036(2) 0.0087(19) 0.0092(18) 0.007(2) C28T 0.048(3) 0.049(3) 0.043(3) -0.007(3) 0.018(2) -0.004(3) C22T 0.033(2) 0.053(3) 0.034(2) -0.004(2) 0.0100(18) -0.013(2) C3 0.038(2) 0.039(3) 0.035(2) -0.002(2) -0.0032(19) 0.003(2) C14T 0.047(3) 0.036(3) 0.045(3) 0.003(2) 0.023(2) -0.002(2) C16T 0.068(3) 0.047(3) 0.046(3) 0.000(2) 0.031(2) 0.005(3) C23T 0.045(3) 0.083(4) 0.034(2) -0.009(3) 0.016(2) -0.020(3) C24T 0.059(3) 0.082(5) 0.053(3) -0.020(3) 0.031(3) -0.027(4) C25T 0.072(4) 0.066(4) 0.083(4) -0.035(4) 0.056(3) -0.033(4) C27T 0.066(3) 0.052(3) 0.073(4) -0.013(3) 0.035(3) -0.003(3) C7T 0.046(3) 0.071(5) 0.124(6) -0.057(5) 0.037(4) -0.023(3) C4T 0.082(4) 0.078(5) 0.091(5) -0.010(4) 0.049(4) 0.010(4) C5T 0.057(4) 0.091(6) 0.141(7) 0.021(6) 0.028(4) 0.028(4) C2T 0.071(4) 0.046(4) 0.143(8) 0.007(5) 0.037(5) -0.007(3) C26T 0.117(6) 0.064(5) 0.128(6) -0.028(5) 0.085(5) -0.011(4) C3T 0.113(6) 0.101(7) 0.149(8) 0.060(7) 0.090(6) 0.033(6) C6T 0.071(5) 0.194(12) 0.067(4) -0.001(6) -0.023(4) -0.030(7) C1T 0.094(5) 0.084(6) 0.133(7) 0.015(5) 0.041(5) 0.019(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O3' C11T 1.338(5) . ? O3' C3' 1.456(5) . ? O5' C21T 1.347(5) . ? O5' C5' 1.445(5) . ? O1' C4' 1.446(5) . ? O1' C1' 1.441(5) . ? O11T C11T 1.216(5) . ? O5 C5 1.434(6) . ? O5 C1T 1.378(9) . ? O2 C2 1.224(5) . ? O21T C21T 1.200(5) . ? N1 C2 1.372(5) . ? N1 C1' 1.441(5) . ? N1 C7 1.472(5) . ? C12T C11T 1.484(6) . ? C12T C18T 1.390(6) . ? C12T C13T 1.396(6) . ? C3' H3' 1.0000 . ? C3' C2' 1.509(6) . ? C3' C4' 1.528(6) . ? C2 C3 1.498(6) . ? C2' H2'A 0.9900 . ? C2' H2'B 0.9900 . ? C2' C1' 1.522(6) . ? C4' H4' 1.0000 . ? C4' C5' 1.501(6) . ? C18T H18T 0.9500 . ? C18T C17T 1.383(6) . ? C1' H1' 1.0000 . ? C17T H17T 0.9500 . ? C17T C15T 1.391(7) . ? C15T C14T 1.382(7) . ? C15T C16T 1.514(6) . ? C21T C22T 1.489(7) . ? C13T H13T 0.9500 . ? C13T C14T 1.380(6) . ? C5 H5 1.0000 . ? C5 C4 1.516(6) . ? C5 C6 1.518(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C6 1.522(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C3 1.533(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C5' H5'A 0.9900 . ? C5' H5'B 0.9900 . ? C28T H28T 0.9500 . ? C28T C22T 1.382(7) . ? C28T C27T 1.381(8) . ? C22T C23T 1.409(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C14T H14T 0.9500 . ? C16T H16A 0.9800 . ? C16T H16B 0.9800 . ? C16T H16C 0.9800 . ? C23T H23T 0.9500 . ? C23T C24T 1.356(9) . ? C24T H24T 0.9500 . ? C24T C25T 1.380(10) . ? C25T C27T 1.420(9) . ? C25T C26T 1.507(9) . ? C27T H27T 0.9500 . ? C7T H7T 0.9500 . ? C7T C2T 1.291(11) . ? C7T C6T 1.478(14) . ? C4T H4T 0.9500 . ? C4T C5T 1.343(10) . ? C4T C3T 1.298(11) . ? C5T H5T 0.9500 . ? C5T C6T 1.460(13) . ? C2T C3T 1.271(12) . ? C2T C1T 1.562(11) . ? C26T H26A 0.9800 . ? C26T H26B 0.9800 . ? C26T H26C 0.9800 . ? C3T H3T 0.9500 . ? C6T H6T 0.9500 . ? C1T H1TA 0.9900 . ? C1T H1TB 0.9900 . ? 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 C11T O3' C3' 118.2(3) . . ? C21T O5' C5' 113.2(3) . . ? C1' O1' C4' 108.3(3) . . ? C1T O5 C5 114.5(5) . . ? C2 N1 C1' 118.6(3) . . ? C2 N1 C7 122.7(3) . . ? C1' N1 C7 118.5(3) . . ? C18T C12T C11T 121.7(4) . . ? C18T C12T C13T 119.6(4) . . ? C13T C12T C11T 118.6(4) . . ? O3' C11T C12T 112.1(4) . . ? O11T C11T O3' 122.9(4) . . ? O11T C11T C12T 125.0(4) . . ? O3' C3' H3' 112.8 . . ? O3' C3' C2' 109.4(3) . . ? O3' C3' C4' 104.7(3) . . ? C2' C3' H3' 112.8 . . ? C2' C3' C4' 103.7(3) . . ? C4' C3' H3' 112.8 . . ? O2 C2 N1 121.9(4) . . ? O2 C2 C3 120.8(4) . . ? N1 C2 C3 117.2(4) . . ? C3' C2' H2'A 111.6 . . ? C3' C2' H2'B 111.6 . . ? C3' C2' C1' 100.7(3) . . ? H2'A C2' H2'B 109.4 . . ? C1' C2' H2'A 111.6 . . ? C1' C2' H2'B 111.6 . . ? O1' C4' C3' 106.2(3) . . ? O1' C4' H4' 108.5 . . ? O1' C4' C5' 110.2(3) . . ? C3' C4' H4' 108.5 . . ? C5' C4' C3' 114.8(4) . . ? C5' C4' H4' 108.5 . . ? C12T C18T H18T 120.1 . . ? C17T C18T C12T 119.8(4) . . ? C17T C18T H18T 120.1 . . ? O1' C1' C2' 104.2(3) . . ? O1' C1' H1' 109.0 . . ? N1 C1' O1' 109.1(3) . . ? N1 C1' C2' 116.3(4) . . ? N1 C1' H1' 109.0 . . ? C2' C1' H1' 109.0 . . ? C18T C17T H17T 119.5 . . ? C18T C17T C15T 121.0(4) . . ? C15T C17T H17T 119.5 . . ? C17T C15T C16T 120.2(4) . . ? C14T C15T C17T 118.5(4) . . ? C14T C15T C16T 121.3(4) . . ? O5' C21T C22T 112.1(4) . . ? O21T C21T O5' 123.5(4) . . ? O21T C21T C22T 124.4(4) . . ? C12T C13T H13T 120.2 . . ? C14T C13T C12T 119.6(4) . . ? C14T C13T H13T 120.2 . . ? O5 C5 H5 108.2 . . ? O5 C5 C4 107.8(4) . . ? O5 C5 C6 111.5(4) . . ? C4 C5 H5 108.2 . . ? C4 C5 C6 113.0(4) . . ? C6 C5 H5 108.2 . . ? N1 C7 H7A 108.6 . . ? N1 C7 H7B 108.6 . . ? N1 C7 C6 114.5(4) . . ? H7A C7 H7B 107.6 . . ? C6 C7 H7A 108.6 . . ? C6 C7 H7B 108.6 . . ? C5 C4 H4A 108.8 . . ? C5 C4 H4B 108.8 . . ? C5 C4 C3 113.9(4) . . ? H4A C4 H4B 107.7 . . ? C3 C4 H4A 108.8 . . ? C3 C4 H4B 108.8 . . ? C5 C6 C7 112.2(4) . . ? C5 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6A 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? O5' C5' C4' 110.0(3) . . ? O5' C5' H5'A 109.7 . . ? O5' C5' H5'B 109.7 . . ? C4' C5' H5'A 109.7 . . ? C4' C5' H5'B 109.7 . . ? H5'A C5' H5'B 108.2 . . ? C22T C28T H28T 119.7 . . ? C27T C28T H28T 119.7 . . ? C27T C28T C22T 120.5(5) . . ? C28T C22T C21T 123.8(4) . . ? C28T C22T C23T 119.1(5) . . ? C23T C22T C21T 117.0(5) . . ? C2 C3 C4 115.3(4) . . ? C2 C3 H3A 108.4 . . ? C2 C3 H3B 108.4 . . ? C4 C3 H3A 108.4 . . ? C4 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? C15T C14T H14T 119.3 . . ? C13T C14T C15T 121.5(4) . . ? C13T C14T H14T 119.3 . . ? C15T C16T H16A 109.5 . . ? C15T C16T H16B 109.5 . . ? C15T C16T H16C 109.5 . . ? H16A C16T H16B 109.5 . . ? H16A C16T H16C 109.5 . . ? H16B C16T H16C 109.5 . . ? C22T C23T H23T 119.7 . . ? C24T C23T C22T 120.7(6) . . ? C24T C23T H23T 119.7 . . ? C23T C24T H24T 119.5 . . ? C23T C24T C25T 120.9(5) . . ? C25T C24T H24T 119.5 . . ? C24T C25T C27T 119.1(6) . . ? C24T C25T C26T 121.0(6) . . ? C27T C25T C26T 119.8(7) . . ? C28T C27T C25T 119.6(6) . . ? C28T C27T H27T 120.2 . . ? C25T C27T H27T 120.2 . . ? C2T C7T H7T 119.3 . . ? C2T C7T C6T 121.4(7) . . ? C6T C7T H7T 119.3 . . ? C5T C4T H4T 118.4 . . ? C3T C4T H4T 118.4 . . ? C3T C4T C5T 123.3(8) . . ? C4T C5T H5T 122.3 . . ? C4T C5T C6T 115.5(7) . . ? C6T C5T H5T 122.3 . . ? C7T C2T C1T 119.3(8) . . ? C3T C2T C7T 119.5(8) . . ? C3T C2T C1T 121.1(9) . . ? C25T C26T H26A 109.5 . . ? C25T C26T H26B 109.5 . . ? C25T C26T H26C 109.5 . . ? H26A C26T H26B 109.5 . . ? H26A C26T H26C 109.5 . . ? H26B C26T H26C 109.5 . . ? C4T C3T H3T 117.5 . . ? C2T C3T C4T 125.0(10) . . ? C2T C3T H3T 117.5 . . ? C7T C6T H6T 122.8 . . ? C5T C6T C7T 114.5(7) . . ? C5T C6T H6T 122.8 . . ? O5 C1T C2T 109.6(7) . . ? O5 C1T H1TA 109.7 . . ? O5 C1T H1TB 109.7 . . ? C2T C1T H1TA 109.7 . . ? C2T C1T H1TB 109.7 . . ? H1TA C1T H1TB 108.2 . . ? 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 O3' C3' C2' C1' 75.5(4) . . . . ? O3' C3' C4' O1' -95.8(3) . . . . ? O3' C3' C4' C5' 142.2(3) . . . . ? O5' C21T C22T C28T -2.5(6) . . . . ? O5' C21T C22T C23T 179.2(4) . . . . ? O1' C4' C5' O5' -62.3(5) . . . . ? O5 C5 C4 C3 -170.1(4) . . . . ? O5 C5 C6 C7 175.8(3) . . . . ? O2 C2 C3 C4 -118.7(5) . . . . ? O21T C21T C22T C28T 177.1(5) . . . . ? O21T C21T C22T C23T -1.2(7) . . . . ? N1 C2 C3 C4 59.6(6) . . . . ? N1 C7 C6 C5 81.0(4) . . . . ? C12T C18T C17T C15T 0.2(6) . . . . ? C12T C13T C14T C15T 1.3(7) . . . . ? C11T O3' C3' C2' 81.5(4) . . . . ? C11T O3' C3' C4' -167.9(3) . . . . ? C11T C12T C18T C17T 174.9(4) . . . . ? C11T C12T C13T C14T -175.8(4) . . . . ? C3' O3' C11T O11T 2.9(6) . . . . ? C3' O3' C11T C12T -176.3(3) . . . . ? C3' C2' C1' O1' 40.8(4) . . . . ? C3' C2' C1' N1 161.0(3) . . . . ? C3' C4' C5' O5' 57.6(4) . . . . ? C2 N1 C1' O1' -116.3(4) . . . . ? C2 N1 C1' C2' 126.2(4) . . . . ? C2 N1 C7 C6 -72.6(5) . . . . ? C2' C3' C4' O1' 18.9(4) . . . . ? C2' C3' C4' C5' -103.1(4) . . . . ? C4' O1' C1' N1 -155.2(3) . . . . ? C4' O1' C1' C2' -30.3(4) . . . . ? C4' C3' C2' C1' -35.8(4) . . . . ? C18T C12T C11T O3' 6.9(5) . . . . ? C18T C12T C11T O11T -172.2(4) . . . . ? C18T C12T C13T C14T 0.9(6) . . . . ? C18T C17T C15T C14T 1.9(6) . . . . ? C18T C17T C15T C16T -177.8(4) . . . . ? C1' O1' C4' C3' 7.1(4) . . . . ? C1' O1' C4' C5' 132.0(4) . . . . ? C1' N1 C2 O2 2.1(7) . . . . ? C1' N1 C2 C3 -176.2(4) . . . . ? C1' N1 C7 C6 112.6(4) . . . . ? C17T C15T C14T C13T -2.7(7) . . . . ? C21T O5' C5' C4' -167.9(3) . . . . ? C21T C22T C23T C24T 179.6(5) . . . . ? C13T C12T C11T O3' -176.5(4) . . . . ? C13T C12T C11T O11T 4.4(6) . . . . ? C13T C12T C18T C17T -1.6(6) . . . . ? C5 O5 C1T C2T -153.3(5) . . . . ? C5 C4 C3 C2 -84.0(5) . . . . ? C7 N1 C2 O2 -172.8(4) . . . . ? C7 N1 C2 C3 9.0(6) . . . . ? C7 N1 C1' O1' 58.8(5) . . . . ? C7 N1 C1' C2' -58.7(5) . . . . ? C4 C5 C6 C7 -62.7(5) . . . . ? C6 C5 C4 C3 66.3(5) . . . . ? C5' O5' C21T O21T -0.5(6) . . . . ? C5' O5' C21T C22T 179.1(3) . . . . ? C28T C22T C23T C24T 1.2(7) . . . . ? C22T C28T C27T C25T 0.1(8) . . . . ? C22T C23T C24T C25T -0.9(8) . . . . ? C16T C15T C14T C13T 177.0(4) . . . . ? C23T C24T C25T C27T 0.1(8) . . . . ? C23T C24T C25T C26T 180.0(5) . . . . ? C24T C25T C27T C28T 0.3(8) . . . . ? C27T C28T C22T C21T -179.1(5) . . . . ? C27T C28T C22T C23T -0.8(7) . . . . ? C7T C2T C3T C4T -2.5(14) . . . . ? C7T C2T C1T O5 25.6(10) . . . . ? C4T C5T C6T C7T -0.4(11) . . . . ? C5T C4T C3T C2T -6.2(15) . . . . ? C2T C7T C6T C5T -7.5(11) . . . . ? C26T C25T C27T C28T -179.6(6) . . . . ? C3T C4T C5T C6T 7.0(13) . . . . ? C3T C2T C1T O5 -157.9(8) . . . . ? C6T C7T C2T C3T 9.2(11) . . . . ? C6T C7T C2T C1T -174.3(7) . . . . ? C1T O5 C5 C4 157.9(5) . . . . ? C1T O5 C5 C6 -77.6(6) . . . . ? C1T C2T C3T C4T -178.9(8) . . . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 -0.231 0.500 152.2 35.8 '2 methanol' 2 0.073 0.000 0.975 7.3 0.3 ? 3 0.500 -0.997 0.500 152.2 35.8 '2 methanol' 4 0.427 0.500 0.025 7.3 0.3 ? 5 0.573 0.500 0.975 7.3 0.3 ? 6 0.927 0.000 0.025 7.3 0.3 ? _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL hari_0m_a.res in C2 hari_0m.res created by SHELXL-2017/1 at 21:56:23 on 07-Sep-2022 REM Old TITL Hari_0m in C2 REM SHELXT solution in C2: R1 0.150, Rweak 0.028, Alpha 0.006 REM 0.000 for 0 systematic absences, Orientation as input REM Flack x = 0.057 ( 0.080 ) from 1619 Parsons' quotients REM Formula found by SHELXT: C34 N O7 CELL 1.54178 33.3058 5.5217 17.9538 90 106.418 90 ZERR 4 0.0016 0.0003 0.0008 0 0.002 0 LATT -7 SYMM -X,+Y,-Z SFAC C H N O UNIT 136 148 4 28 L.S. 20 PLAN 5 SIZE 0.01 0.05 0.2 TEMP -123.15 CONF BOND list 4 MORE -1 BOND $H ABIN fmap 2 acta REM REM REM WGHT 0.093500 2.555100 FVAR 0.37772 O3' 4 0.746015 0.010524 0.229873 11.00000 0.03695 0.02483 = 0.02938 -0.00268 0.01345 -0.00266 O5' 4 0.689157 -0.034826 0.418640 11.00000 0.03474 0.03949 = 0.02517 0.00534 0.00725 0.00285 O1' 4 0.666518 -0.204547 0.261645 11.00000 0.03384 0.02593 = 0.03806 0.00348 0.00198 -0.00054 O11T 4 0.775226 0.380108 0.244391 11.00000 0.05403 0.03228 = 0.03862 -0.00869 0.01932 -0.00860 O5 4 0.517605 0.626013 0.192433 11.00000 0.04258 0.03499 = 0.05535 -0.00145 0.02305 0.00029 O2 4 0.606861 -0.050375 0.061708 11.00000 0.04782 0.05835 = 0.03047 -0.00737 0.00399 0.00622 O21T 4 0.720415 -0.163563 0.539783 11.00000 0.04851 0.05440 = 0.03303 0.01311 0.00483 0.00126 N1 3 0.612800 0.044286 0.187464 11.00000 0.03002 0.03342 = 0.02860 -0.00269 0.00269 0.00058 C12T 1 0.786642 0.112409 0.147174 11.00000 0.03196 0.02564 = 0.02706 -0.00189 0.00732 0.00098 C11T 1 0.769498 0.185055 0.211679 11.00000 0.03094 0.03152 = 0.02636 -0.00111 0.00542 -0.00261 C3' 1 0.724997 0.062077 0.289034 11.00000 0.03346 0.02605 = 0.02483 -0.00436 0.00786 0.00044 AFIX 13 H3' 2 0.743602 0.145117 0.335586 11.00000 -1.20000 AFIX 0 C2 1 0.590408 0.017392 0.111034 11.00000 0.03866 0.03043 = 0.03215 -0.00224 0.00219 -0.00380 C2' 1 0.685173 0.200613 0.253062 11.00000 0.03510 0.02398 = 0.02377 -0.00247 0.00591 0.00013 AFIX 23 H2'A 2 0.689462 0.328740 0.217501 11.00000 -1.20000 H2'B 2 0.673706 0.273677 0.293084 11.00000 -1.20000 AFIX 0 C4' 1 0.709561 -0.184266 0.308335 11.00000 0.03072 0.02731 = 0.03092 0.00128 0.00362 0.00076 AFIX 13 H4' 2 0.726288 -0.313559 0.291901 11.00000 -1.20000 AFIX 0 C18T 1 0.774776 -0.102307 0.106476 11.00000 0.03784 0.02725 = 0.03656 -0.00110 0.01273 -0.00152 AFIX 43 H18T 2 0.756973 -0.213242 0.122286 11.00000 -1.20000 AFIX 0 C1' 1 0.657205 -0.001267 0.209214 11.00000 0.03252 0.02510 = 0.02667 0.00240 0.00411 0.00154 AFIX 13 H1' 2 0.665738 -0.041523 0.161549 11.00000 -1.20000 AFIX 0 C17T 1 0.788974 -0.153923 0.042879 11.00000 0.04705 0.03055 = 0.03215 -0.00585 0.01021 0.00164 AFIX 43 H17T 2 0.780692 -0.300583 0.015123 11.00000 -1.20000 AFIX 0 C15T 1 0.815194 0.005621 0.018938 11.00000 0.04178 0.03464 = 0.03339 0.00196 0.01422 0.00785 C21T 1 0.696823 -0.027884 0.496399 11.00000 0.03009 0.04397 = 0.02712 0.00452 0.00438 -0.00915 C13T 1 0.813679 0.271086 0.124625 11.00000 0.04575 0.02962 = 0.03523 -0.00269 0.01436 -0.00099 AFIX 43 H13T 2 0.822284 0.417149 0.152535 11.00000 -1.20000 AFIX 0 C5 1 0.534013 0.387491 0.188836 11.00000 0.03465 0.03215 = 0.04777 0.00028 0.01393 -0.00224 AFIX 13 H5 2 0.514200 0.268173 0.201092 11.00000 -1.20000 AFIX 0 C7 1 0.592887 0.098171 0.249107 11.00000 0.03579 0.04078 = 0.02955 0.00210 0.00704 -0.00381 AFIX 23 H7A 2 0.613506 0.068758 0.300075 11.00000 -1.20000 H7B 2 0.569344 -0.015829 0.244271 11.00000 -1.20000 AFIX 0 C4 1 0.535122 0.343927 0.106071 11.00000 0.03931 0.04149 = 0.04050 0.00346 0.00543 0.00624 AFIX 23 H4A 2 0.556548 0.451116 0.094938 11.00000 -1.20000 H4B 2 0.507667 0.389510 0.070293 11.00000 -1.20000 AFIX 0 C6 1 0.576418 0.355660 0.247905 11.00000 0.03907 0.03605 = 0.03789 -0.00799 0.01312 -0.00711 AFIX 23 H6A 2 0.574075 0.397299 0.300148 11.00000 -1.20000 H6B 2 0.596659 0.468988 0.235526 11.00000 -1.20000 AFIX 0 C5' 1 0.712475 -0.221172 0.392538 11.00000 0.03456 0.03216 = 0.03565 0.00867 0.00918 0.00666 AFIX 23 H5'A 2 0.701095 -0.382295 0.399798 11.00000 -1.20000 H5'B 2 0.742168 -0.215575 0.423789 11.00000 -1.20000 AFIX 0 C28T 1 0.647152 0.329734 0.471318 11.00000 0.04787 0.04851 = 0.04323 -0.00706 0.01842 -0.00427 AFIX 43 H28T 2 0.643739 0.317292 0.417104 11.00000 -1.20000 AFIX 0 C22T 1 0.672871 0.168105 0.521678 11.00000 0.03334 0.05285 = 0.03389 -0.00436 0.01002 -0.01285 C3 1 0.544866 0.081449 0.089464 11.00000 0.03816 0.03893 = 0.03475 -0.00232 -0.00319 0.00287 AFIX 23 H3A 2 0.530770 -0.027473 0.117980 11.00000 -1.20000 H3B 2 0.532643 0.049756 0.033331 11.00000 -1.20000 AFIX 0 C14T 1 0.827830 0.214501 0.061560 11.00000 0.04699 0.03562 = 0.04467 0.00264 0.02320 -0.00170 AFIX 43 H14T 2 0.846679 0.321477 0.047103 11.00000 -1.20000 AFIX 0 C16T 1 0.829139 -0.049705 -0.052520 11.00000 0.06821 0.04670 = 0.04556 0.00024 0.03146 0.00487 AFIX 137 H16A 2 0.835478 -0.222758 -0.053623 11.00000 -1.50000 H16B 2 0.854246 0.044917 -0.051045 11.00000 -1.50000 H16C 2 0.806721 -0.007090 -0.099150 11.00000 -1.50000 AFIX 0 C23T 1 0.678057 0.190535 0.602042 11.00000 0.04461 0.08252 = 0.03413 -0.00934 0.01567 -0.01966 AFIX 43 H23T 2 0.696103 0.082107 0.637129 11.00000 -1.20000 AFIX 0 C24T 1 0.657543 0.365372 0.629788 11.00000 0.05931 0.08157 = 0.05276 -0.02041 0.03130 -0.02692 AFIX 43 H24T 2 0.661101 0.376409 0.684077 11.00000 -1.20000 AFIX 0 C25T 1 0.631571 0.527490 0.580284 11.00000 0.07221 0.06598 = 0.08260 -0.03463 0.05553 -0.03251 C27T 1 0.626371 0.509232 0.499204 11.00000 0.06566 0.05176 = 0.07333 -0.01287 0.03472 -0.00312 AFIX 43 H27T 2 0.608704 0.619814 0.464349 11.00000 -1.20000 AFIX 0 C7T 1 0.447478 0.903786 0.159358 11.00000 0.04611 0.07140 = 0.12377 -0.05720 0.03731 -0.02302 AFIX 43 H7T 2 0.452568 0.799745 0.120870 11.00000 -1.20000 AFIX 0 C4T 1 0.427523 1.150039 0.270736 11.00000 0.08199 0.07834 = 0.09070 -0.01021 0.04852 0.01028 AFIX 43 H4T 2 0.419902 1.215783 0.313720 11.00000 -1.20000 AFIX 0 C5T 1 0.408348 1.235510 0.199491 11.00000 0.05669 0.09127 = 0.14131 0.02143 0.02799 0.02848 AFIX 43 H5T 2 0.389870 1.370210 0.191392 11.00000 -1.20000 AFIX 0 C2T 1 0.466607 0.864410 0.231568 11.00000 0.07087 0.04646 = 0.14323 0.00698 0.03726 -0.00708 C26T 1 0.608744 0.721932 0.611007 11.00000 0.11650 0.06433 = 0.12840 -0.02825 0.08464 -0.01145 AFIX 137 H26A 2 0.583190 0.653976 0.619401 11.00000 -1.50000 H26B 2 0.601373 0.854540 0.573317 11.00000 -1.50000 H26C 2 0.626827 0.783699 0.660277 11.00000 -1.50000 AFIX 0 C3T 1 0.455946 0.982096 0.283785 11.00000 0.11284 0.10111 = 0.14911 0.06018 0.08955 0.03270 AFIX 43 H3T 2 0.469837 0.944282 0.336385 11.00000 -1.20000 AFIX 0 C6T 1 0.417830 1.107365 0.135347 11.00000 0.07093 0.19385 = 0.06677 -0.00117 -0.02252 -0.03049 AFIX 43 H6T 2 0.405921 1.151247 0.082534 11.00000 -1.20000 AFIX 0 C1T 1 0.500727 0.662097 0.253329 11.00000 0.09430 0.08381 = 0.13275 0.01526 0.04072 0.01927 AFIX 23 H1TA 2 0.523048 0.710534 0.300261 11.00000 -1.20000 H1TB 2 0.488065 0.509599 0.264947 11.00000 -1.20000 AFIX 0 HKLF 4 REM hari_0m_a.res in C2 REM R1 = 0.0536 for 4102 Fo > 4sig(Fo) and 0.0582 for all 4471 data REM 381 parameters refined using 1 restraints END WGHT 0.0936 2.5498 REM Highest difference peak 0.765, deepest hole -0.374, 1-sigma level 0.059 Q1 1 0.4722 0.6516 0.1499 11.00000 0.05 0.76 Q2 1 0.4362 1.0447 0.1193 11.00000 0.05 0.36 Q3 1 0.4160 1.2945 0.1412 11.00000 0.05 0.34 Q4 1 0.4717 0.3774 0.1606 11.00000 0.05 0.25 Q5 1 0.4389 0.5837 0.1065 11.00000 0.05 0.19 ; _shelx_res_checksum 28778 _shelx_hkl_file ; 2 0 0 1436.66 84.19 -2 0 0 1373.96 48.70 -2 0 0 1266.77 77.59 2 0 0 1335.77 48.40 -4 0 0 541.55 17.40 4 0 0 524.75 18.00 -4 0 0 541.25 17.30 -4 0 0 517.15 17.90 -4 0 0 522.65 17.90 4 0 0 559.44 17.90 -6 0 0 337.67 12.60 6 0 0 373.86 12.40 6 0 0 380.96 12.60 6 0 0 375.36 12.70 -6 0 0 323.47 12.60 -6 0 0 372.76 12.60 -6 0 0 369.76 12.00 -6 0 0 361.86 11.80 -8 0 0 1066.19 35.40 -8 0 0 1096.99 35.10 10 0 0 850.21 28.50 10 0 0 832.12 28.60 -10 0 0 830.12 28.50 12 0 0 11.40 0.90 -12 0 0 10.40 1.70 12 0 0 7.30 1.50 12 0 0 12.40 1.70 12 0 0 9.50 1.90 -14 0 0 600.04 21.30 14 0 0 586.14 19.90 14 0 0 600.34 21.60 14 0 0 609.04 21.10 -16 0 0 802.02 27.60 16 0 0 795.62 27.90 16 0 0 772.12 25.80 16 0 0 754.92 27.20 18 0 0 199.48 9.30 18 0 0 194.78 8.60 -18 0 0 193.98 8.70 18 0 0 186.18 6.90 20 0 0 229.68 8.30 20 0 0 237.98 10.20 -20 0 0 226.98 10.40 20 0 0 246.78 11.00 -22 0 0 106.39 6.40 22 0 0 113.69 6.40 22 0 0 106.79 6.90 24 0 0 7.10 2.20 -24 0 0 5.70 1.80 24 0 0 6.70 3.20 -26 0 0 1.30 1.50 26 0 0 3.10 2.10 26 0 0 -0.50 2.50 28 0 0 31.00 4.00 28 0 0 33.80 3.20 -28 0 0 32.30 4.70 -28 0 0 32.90 3.00 28 0 0 33.40 5.20 30 0 0 48.30 5.00 -30 0 0 42.90 5.30 30 0 0 44.80 3.70 30 0 0 53.49 6.00 32 0 0 22.40 2.90 32 0 0 27.50 2.70 32 0 0 27.20 4.40 -32 0 0 26.50 4.70 34 0 0 6.20 2.70 34 0 0 6.20 1.90 34 0 0 9.50 1.90 -34 0 0 4.30 4.00 -1 -1 0 743.83 24.90 -1 -1 0 756.22 25.00 1 -1 0 725.13 25.10 -1 -1 0 747.33 24.90 1 -1 0 757.22 24.90 1 -1 0 790.92 24.70 1 -1 0 770.02 25.00 -1 -1 0 750.92 25.00 -1 -1 0 744.73 24.90 1 -1 0 752.52 25.40 -1 -1 0 756.62 25.30 1 -1 0 793.52 24.90 1 -1 0 733.13 25.00 -1 -1 0 752.42 24.90 -1 -1 0 746.83 24.90 1 -1 0 773.32 24.90 1 -1 0 774.62 24.80 1 -1 0 758.72 24.90 -3 -1 0 276.07 9.50 -3 -1 0 266.17 9.90 3 -1 0 281.77 9.60 -3 -1 0 263.67 9.90 3 -1 0 261.37 10.00 -3 -1 0 279.57 9.70 3 -1 0 264.37 9.80 -3 -1 0 275.57 9.70 3 -1 0 292.97 9.70 3 -1 0 276.67 9.60 -3 -1 0 265.27 9.50 -3 -1 0 268.87 9.90 -3 1 0 296.47 9.60 3 1 0 290.97 9.50 -3 1 0 290.37 9.70 -3 1 0 285.37 9.70 -3 1 0 287.37 9.60 3 1 0 295.67 9.50 -3 1 0 302.57 9.90 3 1 0 296.77 9.80 3 1 0 293.37 9.60 3 1 0 289.67 9.60 3 1 0 282.67 9.50 -3 1 0 295.17 9.40 -3 1 0 290.77 9.70 -3 1 0 296.37 9.40 3 1 0 295.47 9.60 -5 -1 0 1690.63 55.99 -5 -1 0 1714.13 55.89 -5 -1 0 1696.23 56.59 5 -1 0 1771.12 55.89 -5 1 0 1723.83 56.19 -5 1 0 1713.33 56.29 -7 -1 0 2565.04 83.59 7 -1 0 2505.05 83.69 -7 1 0 2536.45 84.49 -7 1 0 2649.33 83.59 7 1 0 2643.94 84.49 9 -1 0 1141.89 38.70 -9 -1 0 1215.48 39.50 9 -1 0 1220.58 39.40 9 -1 0 1219.58 39.70 9 1 0 1222.98 38.90 9 1 0 1197.78 39.50 9 1 0 1120.99 39.90 -9 1 0 1128.59 38.90 -11 -1 0 460.95 16.20 11 -1 0 457.55 16.50 11 -1 0 449.56 16.20 11 -1 0 452.75 16.20 11 1 0 447.46 15.30 11 1 0 458.35 15.50 11 1 0 470.15 15.40 11 1 0 394.36 17.10 -11 1 0 454.25 15.30 -11 1 0 456.05 16.30 11 1 0 468.75 16.40 11 1 0 463.85 15.50 11 1 0 461.95 15.80 13 -1 0 157.78 6.90 13 -1 0 150.68 6.90 -13 -1 0 154.38 6.90 13 -1 0 162.38 7.40 -13 1 0 157.88 7.00 -13 1 0 162.38 5.80 13 1 0 158.38 7.20 13 1 0 160.98 6.20 13 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6.50 3.10 27 1 3 5.80 1.60 27 1 3 5.20 1.70 -27 1 -3 4.90 2.50 27 1 3 4.40 2.20 29 -1 3 13.90 4.20 29 -1 3 26.00 4.70 29 -1 3 13.50 2.30 -29 -1 -3 15.80 3.80 29 1 3 12.70 2.20 29 1 3 16.80 2.20 -29 1 -3 15.00 3.40 31 -1 3 4.80 3.10 31 -1 3 1.70 1.60 31 -1 3 -0.80 1.30 31 -1 3 6.70 3.70 31 1 3 -0.20 1.90 31 1 3 1.50 1.40 -31 1 -3 0.70 2.40 31 1 3 2.50 1.70 -33 1 -3 4.40 3.70 -33 1 -3 2.70 4.10 33 1 3 4.60 2.50 34 -2 -3 11.00 4.90 34 -2 -3 15.80 4.80 34 2 -3 17.20 3.30 -34 2 3 15.10 4.00 34 2 -3 12.50 2.20 -34 2 3 11.00 3.50 32 -2 -3 36.10 5.20 32 -2 -3 29.70 5.00 -32 2 3 43.30 4.10 32 2 -3 46.40 4.20 32 2 -3 52.49 3.60 -32 2 3 51.99 5.20 30 -2 -3 12.80 3.80 30 -2 -3 14.90 4.00 30 2 -3 16.30 2.70 30 2 -3 18.40 2.40 -30 2 3 18.30 2.70 30 2 -3 15.40 2.70 -30 2 3 17.60 3.50 28 -2 -3 19.40 3.80 28 -2 -3 21.00 4.60 28 2 -3 24.50 2.60 28 2 -3 18.60 2.90 -28 2 3 19.30 2.50 -28 2 3 18.30 2.50 -28 2 3 19.20 3.40 28 2 -3 18.80 2.70 28 2 -3 18.40 2.30 26 -2 -3 196.28 10.50 26 -2 -3 204.28 11.50 -26 2 3 204.98 8.60 26 2 -3 198.78 9.00 26 2 -3 210.88 9.20 -26 2 3 203.28 9.00 26 2 -3 195.48 8.50 -26 2 3 203.78 10.30 26 2 -3 210.18 8.40 24 -2 -3 130.39 8.50 24 -2 -3 115.49 7.30 24 -2 -3 109.89 7.30 -24 2 3 112.99 5.90 24 2 -3 109.19 5.40 24 2 -3 112.19 6.00 -24 2 3 122.39 7.00 24 2 -3 110.29 5.40 24 2 -3 114.59 5.90 22 -2 -3 151.38 9.00 22 -2 -3 163.38 8.60 22 -2 -3 155.38 8.40 -22 2 3 159.28 7.20 -22 2 3 159.58 6.50 -22 2 3 155.38 8.20 22 2 -3 149.39 7.10 22 2 -3 153.58 7.00 22 2 -3 160.78 6.70 22 2 -3 152.48 6.70 20 -2 -3 60.09 5.40 20 -2 -3 65.79 5.00 20 -2 -3 67.99 4.90 -20 2 3 66.49 4.80 20 2 -3 65.19 3.80 20 2 -3 66.69 3.60 -20 2 3 66.99 3.90 20 2 -3 59.79 3.40 20 2 -3 57.09 3.40 20 2 -3 63.49 3.80 -20 2 3 63.39 3.40 -18 -2 3 65.49 4.60 18 -2 -3 61.29 4.50 18 -2 -3 66.99 5.10 18 -2 -3 58.29 4.50 18 2 -3 67.99 3.70 18 2 -3 65.59 3.50 -18 2 3 65.89 4.50 -18 2 3 71.39 3.60 18 2 -3 71.69 3.40 18 2 -3 63.89 3.60 -18 2 3 64.89 3.80 18 2 -3 63.19 3.50 -16 -2 3 388.06 15.30 16 -2 -3 391.46 15.30 16 -2 -3 391.96 15.20 16 -2 -3 419.36 15.40 -16 2 3 371.56 14.30 -16 2 3 387.76 13.90 -16 2 3 384.36 14.00 16 2 -3 413.76 14.00 16 2 -3 385.66 13.80 16 2 -3 391.06 14.00 16 2 -3 386.06 14.00 16 2 -3 395.16 14.10 -16 2 3 394.16 15.10 14 -2 -3 106.69 5.60 -14 -2 3 112.69 5.80 14 -2 -3 108.49 5.70 14 -2 -3 121.29 6.20 14 2 -3 108.49 4.90 -14 2 3 119.49 5.10 14 2 -3 120.89 4.90 -14 2 3 103.69 5.10 14 2 -3 120.69 4.90 -14 2 3 116.59 4.70 14 2 -3 105.99 4.40 14 2 -3 115.49 5.00 14 2 -3 119.99 4.70 -14 2 3 127.39 5.90 12 -2 -3 2040.20 66.89 12 -2 -3 2005.80 66.79 12 -2 -3 1998.20 66.89 -12 -2 3 1995.00 66.89 12 2 -3 1951.50 65.69 12 2 -3 2007.50 65.79 -12 2 3 2013.00 65.79 -12 2 3 2044.80 66.69 -12 2 3 2047.90 66.89 12 2 -3 2006.20 65.99 -10 -2 3 1326.27 44.70 10 -2 -3 1337.47 44.60 10 -2 -3 1294.37 44.60 10 2 -3 1340.77 43.60 -10 2 3 1372.16 44.70 10 2 -3 1278.27 43.60 -10 2 3 1385.56 44.80 10 2 -3 1303.07 43.90 10 2 -3 1330.87 43.90 -10 2 3 1353.36 43.70 10 2 -3 1299.47 43.90 -10 2 3 1362.96 44.30 8 -2 -3 121.29 5.20 8 -2 -3 124.39 5.40 -8 -2 3 118.89 5.30 8 -2 -3 120.99 4.80 -8 2 3 119.49 4.50 8 2 -3 119.49 4.80 8 2 -3 119.59 4.90 -8 2 3 117.59 5.00 8 2 -3 112.19 4.70 -8 2 3 124.59 5.40 8 2 -3 127.79 4.70 8 2 -3 111.89 4.70 8 2 -3 119.59 4.90 -8 2 3 125.99 5.10 6 -2 -3 296.87 11.30 -6 -2 3 309.77 11.10 6 -2 -3 317.17 11.20 6 -2 -3 313.97 11.00 -6 2 3 310.67 11.10 -6 2 3 319.67 10.50 -6 2 3 282.87 10.90 6 2 -3 313.37 10.80 -6 2 3 309.97 11.10 6 2 -3 305.77 10.70 6 2 -3 309.07 10.70 6 2 -3 315.67 10.70 6 2 -3 310.97 10.90 -6 2 3 310.57 11.50 6 2 -3 309.17 11.10 6 2 -3 305.87 10.80 -6 2 3 308.17 10.90 -4 -2 3 203.18 7.10 4 -2 -3 204.18 7.60 -4 -2 3 201.88 7.50 4 -2 -3 203.98 7.80 4 2 -3 207.38 7.50 4 2 -3 208.08 7.30 4 2 -3 203.38 7.20 4 2 -3 199.58 7.80 -4 2 3 209.18 7.70 -4 2 3 202.98 7.40 -4 2 3 209.18 7.30 4 2 -3 200.98 7.40 -4 2 3 208.48 7.60 4 2 -3 205.38 7.40 -4 2 3 210.18 8.20 4 2 -3 196.78 7.30 -4 2 3 208.68 7.10 -4 2 3 198.78 7.50 4 2 -3 210.38 7.50 -2 -2 3 757.22 25.10 2 -2 -3 768.42 25.60 -2 -2 3 760.12 24.90 2 -2 -3 724.83 25.00 -2 -2 3 667.43 24.70 2 2 -3 752.92 25.00 -2 2 3 724.93 25.10 -2 2 3 743.53 24.80 -2 2 3 770.52 24.80 2 2 -3 781.42 25.00 -2 2 3 743.33 24.70 -2 2 3 762.22 24.60 -2 2 3 750.42 24.90 2 2 -3 761.52 24.80 -2 2 3 750.32 25.70 2 2 -3 765.72 24.80 2 2 -3 741.03 24.90 -2 2 3 767.72 25.20 2 2 -3 740.73 25.00 0 -2 3 201.68 7.30 0 -2 -3 197.88 7.10 0 -2 3 198.38 7.40 0 -2 -3 199.58 7.90 0 2 -3 190.48 7.20 0 2 3 197.18 7.40 0 2 3 202.98 7.10 0 2 -3 203.48 6.90 0 2 3 198.38 6.80 0 2 -3 198.38 6.70 0 2 -3 201.28 7.00 0 2 -3 180.88 7.10 0 2 3 200.58 7.00 0 2 3 194.98 7.40 0 2 3 189.38 7.10 0 2 3 200.58 7.90 0 2 -3 197.18 7.20 0 2 3 204.48 6.90 0 2 -3 185.98 6.80 0 2 -3 199.88 7.20 2 -2 3 514.05 17.60 -2 -2 -3 485.25 17.00 -2 2 -3 503.45 17.10 2 2 3 504.15 17.00 -2 2 -3 520.55 17.20 -2 2 -3 499.65 16.90 -2 2 -3 505.75 16.90 -2 2 -3 509.75 17.20 2 2 3 496.45 17.00 2 2 3 500.85 16.80 2 2 3 496.75 17.30 2 2 3 519.35 17.80 2 2 3 508.35 17.20 4 -2 3 533.65 17.80 4 -2 3 499.75 17.90 -4 -2 -3 513.65 17.30 4 2 3 516.15 17.30 -4 2 -3 485.45 17.40 4 2 3 530.05 17.20 4 2 3 478.35 17.00 4 2 3 511.95 16.80 4 2 3 504.55 17.50 -4 2 -3 495.75 17.70 -4 2 -3 511.15 16.90 4 2 3 514.85 17.90 -4 2 -3 465.75 17.30 -4 2 -3 503.15 17.10 4 2 3 523.65 17.00 4 2 3 530.15 17.20 -4 2 -3 514.75 17.30 6 -2 3 133.99 5.70 -6 -2 -3 123.49 5.20 6 -2 3 129.09 6.10 -6 2 -3 124.09 5.20 6 2 3 124.39 4.80 6 2 3 126.39 4.90 -6 2 -3 122.79 4.80 -6 2 -3 124.49 5.00 -6 2 -3 127.39 4.50 6 2 3 127.09 4.90 6 2 3 124.59 5.20 6 2 3 129.79 4.90 6 2 3 126.89 5.70 6 2 3 119.89 5.20 -6 2 -3 118.59 5.10 -6 2 -3 127.39 5.10 8 -2 3 171.18 8.00 8 -2 3 182.88 7.50 -8 -2 -3 171.48 7.00 -8 2 -3 167.08 7.00 8 2 3 179.78 7.40 -8 2 -3 182.48 6.90 8 2 3 175.98 6.50 8 2 3 163.58 6.50 -8 2 -3 174.28 6.70 8 2 3 161.08 6.80 8 2 3 172.48 6.50 -8 2 -3 175.08 6.60 -8 2 -3 171.58 6.30 8 2 3 178.98 6.40 10 -2 3 461.55 18.00 -10 -2 -3 472.05 17.10 10 -2 3 490.65 17.60 10 2 3 451.35 16.40 10 2 3 460.45 16.70 10 2 3 495.15 17.30 10 2 3 453.15 16.30 10 2 3 482.05 16.30 -10 2 -3 475.05 16.80 -10 2 -3 509.55 17.30 -10 2 -3 477.55 16.00 10 2 3 466.05 15.90 -10 2 -3 489.55 16.70 -10 2 -3 477.05 16.30 12 -2 3 520.85 18.90 -12 -2 -3 493.55 18.40 -12 2 -3 505.65 17.00 12 2 3 525.05 17.50 -12 2 -3 512.55 18.00 12 2 3 496.85 17.90 12 2 3 496.95 18.30 -12 2 -3 524.25 18.50 12 2 3 515.45 17.40 12 2 3 481.95 17.60 -12 2 -3 501.65 17.40 -14 -2 -3 2.70 1.40 14 -2 3 -0.10 1.70 14 -2 3 1.20 1.30 14 2 3 2.00 1.00 14 2 3 2.20 1.20 14 2 3 1.90 0.80 14 2 3 1.60 0.90 14 2 3 0.30 0.70 -14 2 -3 0.40 1.20 -14 2 -3 1.00 0.80 -16 -2 -3 57.49 4.60 16 -2 3 59.39 5.20 16 -2 3 60.39 4.70 16 2 3 70.59 3.60 16 2 3 60.39 3.10 16 2 3 66.89 4.00 16 2 3 65.39 4.20 -16 2 -3 70.89 4.50 -16 2 -3 68.49 3.70 16 2 3 63.79 3.80 18 -2 3 13.60 2.40 18 -2 3 18.10 3.90 18 2 3 17.00 1.70 -18 2 -3 20.40 2.90 18 2 3 17.00 2.60 18 2 3 16.00 2.30 -18 2 -3 13.60 1.80 18 2 3 17.80 2.00 18 2 3 16.00 2.30 20 -2 3 38.30 5.10 20 -2 3 27.60 4.70 20 2 3 32.30 2.80 20 2 3 35.90 3.10 -20 2 -3 33.20 2.70 20 2 3 36.80 3.60 20 2 3 31.30 2.30 -20 2 -3 35.00 3.80 20 2 3 27.40 3.20 22 -2 3 265.57 13.20 22 -2 3 272.07 13.90 -22 2 -3 286.57 12.60 -22 2 -3 279.27 10.90 22 2 3 269.17 11.60 22 2 3 284.57 11.00 22 2 3 276.97 11.50 24 -2 3 165.08 10.10 24 -2 3 154.88 9.50 -24 2 -3 165.98 7.20 24 2 3 165.58 8.00 24 2 3 154.28 7.20 24 2 3 159.98 7.70 -24 2 -3 160.68 7.70 -24 2 -3 150.78 8.30 26 -2 3 11.30 3.60 26 -2 3 8.70 4.10 -26 2 -3 7.90 2.00 -26 2 -3 6.50 2.40 26 2 3 8.50 2.20 26 2 3 9.10 1.80 -26 2 -3 7.90 2.00 26 2 3 11.30 2.40 28 -2 3 1.20 2.80 -28 -2 -3 1.00 2.30 28 -2 3 1.80 3.20 -28 2 -3 -0.50 2.00 28 2 3 0.30 1.40 -28 2 -3 2.80 1.60 28 2 3 1.40 1.30 30 -2 3 0.00 2.20 30 -2 3 3.30 3.40 30 -2 3 7.60 4.40 -30 -2 -3 5.70 3.30 -30 2 -3 0.90 1.80 30 2 3 6.00 2.00 30 2 3 4.10 1.70 -30 2 -3 7.00 2.80 31 -3 -3 11.00 3.80 -31 3 3 5.70 2.50 31 3 -3 8.50 3.20 31 3 -3 4.70 1.70 -31 3 3 2.80 2.90 29 -3 -3 10.00 3.80 -29 3 3 2.90 2.10 -29 3 3 6.60 2.00 29 3 -3 2.90 2.20 29 3 -3 4.50 1.60 27 -3 -3 62.19 6.50 27 3 -3 50.29 4.40 27 3 -3 66.79 4.10 -27 3 3 57.49 4.70 27 3 -3 51.99 3.70 -27 3 3 63.59 4.40 25 -3 -3 40.60 6.10 -25 3 3 34.90 3.70 25 3 -3 39.40 3.30 25 3 -3 36.50 3.80 25 3 -3 35.30 3.10 -25 3 3 39.70 3.50 23 -3 -3 372.76 17.10 23 -3 -3 396.86 16.40 -23 3 3 354.86 14.90 -23 3 3 360.96 13.90 23 3 -3 391.76 14.90 23 3 -3 376.46 14.20 23 3 -3 360.56 14.10 -23 3 3 377.96 14.60 21 -3 -3 98.29 7.60 21 -3 -3 107.69 7.00 21 3 -3 103.09 5.30 -21 3 3 102.59 5.10 21 3 -3 100.19 5.30 -21 3 3 103.49 5.70 21 3 -3 104.99 5.20 21 3 -3 113.09 5.90 -21 3 3 101.79 6.00 19 -3 -3 31.20 4.80 19 -3 -3 34.90 5.90 19 -3 -3 31.00 4.00 19 3 -3 29.60 2.70 19 3 -3 26.30 2.60 -19 3 3 28.40 3.10 -19 3 3 24.50 2.80 -19 3 3 29.50 2.60 19 3 -3 25.70 2.40 19 3 -3 24.90 2.80 17 -3 -3 32.80 4.30 17 -3 -3 36.70 3.80 17 -3 -3 42.70 4.70 17 3 -3 34.20 2.80 -17 3 3 35.80 3.10 -17 3 3 37.60 2.90 17 3 -3 40.30 3.00 -17 3 3 39.10 3.30 17 3 -3 36.50 2.60 17 3 -3 43.50 3.10 15 -3 -3 91.89 5.50 15 -3 -3 94.89 6.10 -15 3 3 96.69 5.00 15 3 -3 93.49 4.60 15 3 -3 95.99 4.70 -15 3 3 83.99 4.10 -15 3 3 89.39 4.90 -15 3 3 98.39 4.80 15 3 -3 94.49 4.50 15 3 -3 100.79 4.70 13 -3 -3 8.10 1.80 13 -3 -3 13.10 2.50 13 3 -3 8.20 1.20 13 3 -3 8.40 1.40 -13 3 3 8.80 1.20 13 3 -3 9.60 1.40 -13 3 3 10.40 1.70 -13 3 3 7.90 1.50 -13 3 3 8.20 1.70 13 3 -3 7.10 1.40 11 -3 -3 37.80 3.20 11 -3 -3 38.20 3.50 11 3 -3 31.70 2.50 11 3 -3 34.00 2.60 -11 3 3 33.20 2.70 11 3 -3 35.10 2.30 -11 3 3 34.30 3.20 11 3 -3 35.40 2.30 -11 3 3 37.80 2.80 -11 3 3 33.20 2.40 11 3 -3 33.20 2.40 11 3 -3 34.70 2.40 -11 3 3 36.90 2.10 9 -3 -3 166.08 7.40 -9 3 3 165.78 6.20 -9 3 3 162.88 7.00 -9 3 3 163.38 6.90 9 3 -3 162.88 7.00 9 3 -3 165.08 6.70 9 3 -3 156.88 6.60 -9 3 3 169.38 7.70 9 3 -3 158.38 6.40 9 3 -3 169.28 6.80 9 3 -3 166.88 6.60 -9 3 3 176.58 6.30 7 -3 -3 155.08 7.10 7 3 -3 170.78 6.60 7 3 -3 169.38 6.50 7 3 -3 168.38 6.40 7 3 -3 166.58 6.60 -7 3 3 165.38 6.90 7 3 -3 165.88 6.70 7 3 -3 167.58 7.10 7 3 -3 160.78 6.30 -7 3 3 169.28 6.20 -7 3 3 162.38 7.60 -7 3 3 151.48 6.60 -5 -3 3 815.62 28.10 5 -3 -3 813.72 28.40 5 -3 -3 820.42 29.00 5 3 -3 850.21 28.40 -5 3 3 846.92 28.00 -5 3 3 838.42 29.70 5 3 -3 858.31 28.20 5 3 -3 842.72 28.50 5 3 -3 868.61 28.40 -5 3 3 836.72 28.50 5 3 -3 863.71 28.50 5 3 -3 830.92 29.10 -5 3 3 862.51 28.80 5 3 -3 841.72 28.20 3 -3 -3 98.99 4.80 -3 -3 3 103.39 4.40 3 -3 -3 107.59 5.10 3 3 -3 106.39 4.40 3 3 -3 101.99 4.50 3 3 -3 97.09 4.30 3 3 -3 104.89 4.50 -3 3 3 101.89 4.70 -3 3 3 98.59 4.80 3 3 -3 95.69 4.20 -3 3 3 99.99 4.20 -3 3 3 98.79 4.00 -3 3 3 92.49 4.30 -3 3 3 98.99 5.30 3 3 -3 104.19 4.40 -1 -3 3 200.48 7.90 1 -3 -3 203.38 8.40 1 3 -3 204.18 7.70 1 3 -3 204.78 7.60 -1 3 3 211.68 8.80 1 3 -3 198.98 7.70 -1 3 3 200.28 7.20 -1 3 3 199.48 7.50 -1 3 3 195.88 8.00 1 3 -3 205.58 7.40 -1 3 3 204.68 8.00 -1 3 3 189.88 7.40 1 3 -3 194.98 7.50 1 3 -3 196.98 7.60 -1 -3 -3 735.63 25.80 1 -3 3 777.52 25.40 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