#------------------------------------------------------------------------------ #$Date: 2024-11-08 03:42:07 +0200 (Fri, 08 Nov 2024) $ #$Revision: 295829 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/16/02/7160222.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7160222 loop_ _publ_author_name 'Dolas, Atul Jankiram' 'Yadav, Jyothi' 'Nagare, Yadav Kacharu' 'Rangan, Krishnan' 'Iype, Eldhose' 'Kumar, Indresh' _publ_section_title ; Enantioselective synthesis of -(3-pyrrolyl)methanamines with aza-tetrasubstituted center under metal-free conditions ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D4OB01729C _journal_year 2024 _chemical_absolute_configuration unk _chemical_formula_moiety 'C25 H22 N2 O' _chemical_formula_sum 'C25 H22 N2 O' _chemical_formula_weight 366.44 _space_group_crystal_system orthorhombic _space_group_IT_number 18 _space_group_name_Hall 'P 2 2ab' _space_group_name_H-M_alt 'P 21 21 2' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2024-08-28 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-08-28 deposited with the CCDC. 2024-11-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.9908(8) _cell_length_b 15.7652(5) _cell_length_c 5.8187(2) _cell_measurement_reflns_used 8496 _cell_measurement_temperature 100 _cell_measurement_theta_max 27.8170 _cell_measurement_theta_min 1.6410 _cell_volume 1833.82(11) _computing_cell_refinement 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100 _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.970 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -11.00 14.00 0.50 7.36 -- 11.50 -22.00-102.00 50 2 \w -13.00 12.00 0.50 7.36 -- 11.50 22.00 62.00 50 3 \w 20.00 46.00 0.50 7.36 -- -11.70 22.00 62.00 52 4 \w 28.00 54.00 0.50 7.36 -- 11.50 77.00 150.00 52 5 \w -77.00 35.00 0.50 7.36 -- 11.50 -77.00-150.00 224 6 \w 74.00 100.00 0.50 7.36 -- 11.50 77.00 150.00 52 7 \w -13.00 19.00 0.50 7.36 -- 11.50 77.00 30.00 64 8 \w 59.00 85.00 0.50 7.36 -- 11.50 77.00 30.00 52 9 \w -101.00 8.00 0.50 7.36 -- -11.70 -77.00 120.00 218 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Pro II AFC12 (RINC): Kappa single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0225205000 _diffrn_orient_matrix_UB_12 0.0325853000 _diffrn_orient_matrix_UB_13 0.0327938000 _diffrn_orient_matrix_UB_21 0.0271795000 _diffrn_orient_matrix_UB_22 -0.0285796000 _diffrn_orient_matrix_UB_23 -0.0119357000 _diffrn_orient_matrix_UB_31 0.0035849000 _diffrn_orient_matrix_UB_32 0.0120903000 _diffrn_orient_matrix_UB_33 -0.1167884000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_unetI/netI 0.0435 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.970 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 14236 _diffrn_reflns_point_group_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.929 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.049 _diffrn_reflns_theta_min 1.645 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.24763 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.327 _exptl_crystal_description block _exptl_crystal_F_000 776 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.195 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.042 _refine_ls_abs_structure_details ; Flack x determined using 1308 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.9(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 254 _refine_ls_number_reflns 4140 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.094 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0382 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+0.0739P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0828 _refine_ls_wR_factor_ref 0.0860 _reflns_Friedel_coverage 0.656 _reflns_Friedel_fraction_full 0.968 _reflns_Friedel_fraction_max 0.871 _reflns_number_gt 3673 _reflns_number_total 4140 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL ad959_20240828_a.res in P2(1)2(1)2 ad959_20240828.res created by SHELXL-2018/3 at 12:04:55 on 28-Aug-2024 REM Old TITL AD959_20240828 in P2(1)2(1)2 REM SHELXT solution in P2(1)2(1)2: R1 0.089, Rweak 0.021, Alpha 0.002 REM 0.568 for 20 systematic absences, Orientation as input REM Flack x = -0.611 ( 0.622 ) from 1268 Parsons' quotients REM Formula found by SHELXT: C25 N2 O CELL 0.71073 19.9908 15.7652 5.8187 90 90 90 ZERR 4 0.0008 0.0005 0.0002 0 0 0 LATT -1 SYMM -X,-Y,+Z SYMM 0.5-X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O UNIT 100 88 8 4 L.S. 4 0 0 PLAN 1 SIZE 0.11 0.2 0.4 TEMP -173.15 CONF list 4 fmap 2 53 MORE -1 BOND $H ACTA REM REM REM WGHT 0.041200 0.073900 FVAR 0.63230 O1 4 0.252704 0.188583 0.787691 11.00000 0.02939 0.02082 = 0.01462 0.00161 0.00014 -0.00389 AFIX 147 H1 2 0.276309 0.226094 0.850421 11.00000 -1.50000 AFIX 0 N1 3 0.303655 0.268521 0.225159 11.00000 0.02041 0.01560 = 0.01592 0.00162 0.00426 0.00172 AFIX 3 H1A 2 0.324975 0.313731 0.175229 11.00000 -1.20000 AFIX 0 N2 3 0.314743 0.457122 0.824925 11.00000 0.01759 0.01539 = 0.01856 -0.00297 -0.00018 0.00019 C1 1 0.345829 0.197841 0.264804 11.00000 0.01849 0.01517 = 0.01583 -0.00118 -0.00439 -0.00184 C2 1 0.399753 0.171548 0.133944 11.00000 0.02135 0.01979 = 0.01927 -0.00085 0.00040 -0.00110 AFIX 43 H2 2 0.413869 0.202809 0.003060 11.00000 -1.20000 AFIX 0 C3 1 0.432723 0.097464 0.200890 11.00000 0.01962 0.02147 = 0.02971 -0.00367 0.00141 0.00178 AFIX 43 H3 2 0.469745 0.077827 0.113443 11.00000 -1.20000 AFIX 0 C4 1 0.412385 0.051978 0.392926 11.00000 0.02150 0.01784 = 0.03137 0.00025 -0.00468 0.00118 AFIX 43 H4 2 0.436087 0.002359 0.437111 11.00000 -1.20000 AFIX 0 C5 1 0.357690 0.078541 0.520586 11.00000 0.02299 0.01611 = 0.02393 0.00240 -0.00363 -0.00335 AFIX 43 H5 2 0.343224 0.047052 0.650611 11.00000 -1.20000 AFIX 0 C6 1 0.324507 0.151830 0.455146 11.00000 0.01809 0.01540 = 0.01798 -0.00195 -0.00350 -0.00362 C7 1 0.261938 0.191571 0.547978 11.00000 0.02084 0.01589 = 0.01240 0.00199 -0.00140 -0.00194 AFIX 13 H7 2 0.223546 0.160181 0.477939 11.00000 -1.20000 AFIX 0 C8 1 0.262299 0.283090 0.435913 11.00000 0.01931 0.01514 = 0.01236 0.00060 0.00165 -0.00083 C9 1 0.191422 0.311215 0.376807 11.00000 0.02006 0.01226 = 0.01584 -0.00196 -0.00156 -0.00080 C10 1 0.139728 0.296012 0.531872 11.00000 0.02403 0.01824 = 0.01631 -0.00039 -0.00078 -0.00113 AFIX 43 H10 2 0.148884 0.267775 0.672632 11.00000 -1.20000 AFIX 0 C11 1 0.074998 0.321780 0.482357 11.00000 0.02044 0.02127 = 0.02246 -0.00334 0.00188 0.00012 AFIX 43 H11 2 0.040033 0.310826 0.588868 11.00000 -1.20000 AFIX 0 C12 1 0.061057 0.363539 0.277705 11.00000 0.02118 0.02417 = 0.02534 -0.00526 -0.00429 0.00433 AFIX 43 H12 2 0.016777 0.381681 0.244586 11.00000 -1.20000 AFIX 0 C13 1 0.112055 0.378506 0.122622 11.00000 0.02805 0.02486 = 0.01880 0.00064 -0.00380 0.00510 AFIX 43 H13 2 0.102837 0.406885 -0.017880 11.00000 -1.20000 AFIX 0 C14 1 0.176821 0.352099 0.171901 11.00000 0.02419 0.01981 = 0.01758 0.00144 0.00114 0.00001 AFIX 43 H14 2 0.211530 0.362193 0.063789 11.00000 -1.20000 AFIX 0 C15 1 0.268317 0.418031 0.689276 11.00000 0.01604 0.01688 = 0.01559 0.00119 -0.00217 -0.00265 AFIX 43 H15 2 0.223776 0.437075 0.665272 11.00000 -1.20000 AFIX 0 C16 1 0.296341 0.346557 0.592714 11.00000 0.01811 0.01413 = 0.01361 0.00287 0.00132 -0.00348 C17 1 0.363452 0.343129 0.674160 11.00000 0.01895 0.01377 = 0.01983 0.00097 -0.00008 0.00101 AFIX 43 H17 2 0.395745 0.301130 0.636770 11.00000 -1.20000 AFIX 0 C18 1 0.373054 0.411602 0.816707 11.00000 0.01636 0.01898 = 0.01907 0.00034 -0.00161 0.00003 AFIX 43 H18 2 0.413236 0.425039 0.895912 11.00000 -1.20000 AFIX 0 C19 1 0.300136 0.530101 0.976931 11.00000 0.02229 0.01991 = 0.02396 -0.00877 0.00270 -0.00023 AFIX 23 H19A 2 0.272089 0.510828 1.107069 11.00000 -1.20000 H19B 2 0.274492 0.573190 0.890005 11.00000 -1.20000 AFIX 0 C20 1 0.363336 0.569833 1.068985 11.00000 0.02110 0.01441 = 0.01830 -0.00464 0.00128 0.00318 C21 1 0.398776 0.628269 0.937580 11.00000 0.02388 0.01917 = 0.01981 0.00150 -0.00014 0.00309 AFIX 43 H21 2 0.381862 0.645369 0.792209 11.00000 -1.20000 AFIX 0 C22 1 0.458333 0.661610 1.016762 11.00000 0.02518 0.01913 = 0.03563 -0.00035 0.00341 -0.00184 AFIX 43 H22 2 0.482491 0.700899 0.924917 11.00000 -1.20000 AFIX 0 C23 1 0.482852 0.637987 1.229059 11.00000 0.02260 0.02655 = 0.03526 -0.01183 -0.00494 0.00274 AFIX 43 H23 2 0.524114 0.660398 1.282657 11.00000 -1.20000 AFIX 0 C24 1 0.447326 0.581875 1.362751 11.00000 0.03113 0.03089 = 0.02020 -0.00634 -0.00423 0.01050 AFIX 43 H24 2 0.463721 0.566555 1.510264 11.00000 -1.20000 AFIX 0 C25 1 0.387763 0.547513 1.283789 11.00000 0.03011 0.01998 = 0.01897 0.00039 0.00333 0.00290 AFIX 43 H25 2 0.363636 0.508616 1.376949 11.00000 -1.20000 AFIX 0 HKLF 4 REM ad959_20240828_a.res in P2(1)2(1)2 REM wR2 = 0.0860, GooF = S = 1.094, Restrained GooF = 1.094 for all data REM R1 = 0.0382 for 3673 Fo > 4sig(Fo) and 0.0452 for all 4140 data REM 254 parameters refined using 0 restraints END WGHT 0.0412 0.0739 REM Highest difference peak 0.195, deepest hole -0.217, 1-sigma level 0.042 Q1 1 0.2612 0.2396 0.5104 11.00000 0.05 0.20 REM The information below was added by Olex2. REM REM R1 = 0.0382 for 3673 Fo > 4sig(Fo) and 0.0452 for all 14314 data REM 254 parameters refined using n/a restraints REM Highest difference peak 0.20, deepest hole -0.22 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0452 REM R1_gt = 0.0382 REM wR_ref = 0.0860 REM GOOF = 1.094 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 14314 REM Reflections_gt = 3673 REM Parameters = 254 REM Hole = -0.22 REM Peak = 0.20 REM Flack = -0.9(7) ; _cod_data_source_file d4ob01729c2.cif _cod_data_source_block ad959_20240828 _cod_database_code 7160222 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C25 H22 N2 O ' _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. ; _shelx_estimated_absorpt_t_max 0.991 _shelx_estimated_absorpt_t_min 0.968 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All O(H) groups 2.a Riding coordinates: N1(H1A) 2.b Ternary CH refined with riding coordinates: C7(H7) 2.c Secondary CH2 refined with riding coordinates: C19(H19A,H19B) 2.d Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25) 2.e Idealised tetrahedral OH refined as rotating group: O1(H1) ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.416 _oxdiff_exptl_absorpt_empirical_full_min 0.423 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' 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 O1 O 0.25270(6) 0.18858(8) 0.7877(2) 0.0216(3) Uani 1 1 d . . . . . H1 H 0.276309 0.226094 0.850421 0.032 Uiso 1 1 calc R U . . . N1 N 0.30366(7) 0.26852(9) 0.2252(3) 0.0173(4) Uani 1 1 d . . . . . H1A H 0.324975 0.313731 0.175229 0.021 Uiso 1 1 d R U . . . N2 N 0.31474(7) 0.45712(9) 0.8249(3) 0.0172(4) Uani 1 1 d . . . . . C1 C 0.34583(9) 0.19784(11) 0.2648(3) 0.0165(4) Uani 1 1 d . . . . . C2 C 0.39975(9) 0.17155(11) 0.1339(4) 0.0201(4) Uani 1 1 d . . . . . H2 H 0.413869 0.202809 0.003060 0.024 Uiso 1 1 calc R U . . . C3 C 0.43272(10) 0.09746(11) 0.2009(4) 0.0236(5) Uani 1 1 d . . . . . H3 H 0.469745 0.077827 0.113443 0.028 Uiso 1 1 calc R U . . . C4 C 0.41239(10) 0.05198(12) 0.3929(4) 0.0236(5) Uani 1 1 d . . . . . H4 H 0.436087 0.002359 0.437111 0.028 Uiso 1 1 calc R U . . . C5 C 0.35769(9) 0.07854(11) 0.5206(4) 0.0210(4) Uani 1 1 d . . . . . H5 H 0.343224 0.047052 0.650611 0.025 Uiso 1 1 calc R U . . . C6 C 0.32451(9) 0.15183(11) 0.4551(3) 0.0172(4) Uani 1 1 d . . . . . C7 C 0.26194(10) 0.19157(10) 0.5480(3) 0.0164(4) Uani 1 1 d . . . . . H7 H 0.223546 0.160181 0.477939 0.020 Uiso 1 1 calc R U . . . C8 C 0.26230(9) 0.28309(10) 0.4359(3) 0.0156(4) Uani 1 1 d . . . . . C9 C 0.19142(9) 0.31122(10) 0.3768(3) 0.0161(4) Uani 1 1 d . . . . . C10 C 0.13973(9) 0.29601(11) 0.5319(4) 0.0195(4) Uani 1 1 d . . . . . H10 H 0.148884 0.267775 0.672632 0.023 Uiso 1 1 calc R U . . . C11 C 0.07500(10) 0.32178(11) 0.4824(4) 0.0214(4) Uani 1 1 d . . . . . H11 H 0.040033 0.310826 0.588868 0.026 Uiso 1 1 calc R U . . . C12 C 0.06106(10) 0.36354(12) 0.2777(4) 0.0236(5) Uani 1 1 d . . . . . H12 H 0.016777 0.381681 0.244586 0.028 Uiso 1 1 calc R U . . . C13 C 0.11206(10) 0.37851(12) 0.1226(4) 0.0239(5) Uani 1 1 d . . . . . H13 H 0.102837 0.406885 -0.017880 0.029 Uiso 1 1 calc R U . . . C14 C 0.17682(10) 0.35210(11) 0.1719(4) 0.0205(4) Uani 1 1 d . . . . . H14 H 0.211530 0.362193 0.063789 0.025 Uiso 1 1 calc R U . . . C15 C 0.26832(9) 0.41803(11) 0.6893(3) 0.0162(4) Uani 1 1 d . . . . . H15 H 0.223776 0.437075 0.665272 0.019 Uiso 1 1 calc R U . . . C16 C 0.29634(9) 0.34656(11) 0.5927(3) 0.0153(4) Uani 1 1 d . . . . . C17 C 0.36345(9) 0.34313(11) 0.6742(3) 0.0175(4) Uani 1 1 d . . . . . H17 H 0.395745 0.301130 0.636770 0.021 Uiso 1 1 calc R U . . . C18 C 0.37305(9) 0.41160(11) 0.8167(4) 0.0181(4) Uani 1 1 d . . . . . H18 H 0.413236 0.425039 0.895912 0.022 Uiso 1 1 calc R U . . . C19 C 0.30014(10) 0.53010(11) 0.9769(4) 0.0221(5) Uani 1 1 d . . . . . H19A H 0.272089 0.510828 1.107069 0.026 Uiso 1 1 calc R U . . . H19B H 0.274492 0.573190 0.890005 0.026 Uiso 1 1 calc R U . . . C20 C 0.36334(9) 0.56983(11) 1.0690(4) 0.0179(4) Uani 1 1 d . . . . . C21 C 0.39878(10) 0.62827(11) 0.9376(4) 0.0210(4) Uani 1 1 d . . . . . H21 H 0.381862 0.645369 0.792209 0.025 Uiso 1 1 calc R U . . . C22 C 0.45833(10) 0.66161(12) 1.0168(4) 0.0266(5) Uani 1 1 d . . . . . H22 H 0.482491 0.700899 0.924917 0.032 Uiso 1 1 calc R U . . . C23 C 0.48285(10) 0.63799(13) 1.2291(4) 0.0281(5) Uani 1 1 d . . . . . H23 H 0.524114 0.660398 1.282657 0.034 Uiso 1 1 calc R U . . . C24 C 0.44733(10) 0.58188(13) 1.3628(4) 0.0274(5) Uani 1 1 d . . . . . H24 H 0.463721 0.566555 1.510264 0.033 Uiso 1 1 calc R U . . . C25 C 0.38776(10) 0.54751(12) 1.2838(4) 0.0230(4) Uani 1 1 d . . . . . H25 H 0.363636 0.508616 1.376949 0.028 Uiso 1 1 calc R 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 O1 0.0294(8) 0.0208(7) 0.0146(7) 0.0016(5) 0.0001(7) -0.0039(6) N1 0.0204(8) 0.0156(7) 0.0159(9) 0.0016(6) 0.0043(8) 0.0017(6) N2 0.0176(8) 0.0154(7) 0.0186(9) -0.0030(7) -0.0002(8) 0.0002(6) C1 0.0185(10) 0.0152(8) 0.0158(10) -0.0012(7) -0.0044(9) -0.0018(7) C2 0.0213(10) 0.0198(9) 0.0193(11) -0.0009(8) 0.0004(10) -0.0011(8) C3 0.0196(10) 0.0215(9) 0.0297(12) -0.0037(9) 0.0014(10) 0.0018(8) C4 0.0215(11) 0.0178(9) 0.0314(12) 0.0002(9) -0.0047(10) 0.0012(8) C5 0.0230(10) 0.0161(8) 0.0239(11) 0.0024(8) -0.0036(10) -0.0034(8) C6 0.0181(9) 0.0154(8) 0.0180(10) -0.0019(8) -0.0035(9) -0.0036(8) C7 0.0208(10) 0.0159(8) 0.0124(10) 0.0020(7) -0.0014(9) -0.0019(8) C8 0.0193(10) 0.0151(8) 0.0124(10) 0.0006(7) 0.0016(9) -0.0008(7) C9 0.0201(10) 0.0123(8) 0.0158(10) -0.0020(7) -0.0016(9) -0.0008(7) C10 0.0240(11) 0.0182(8) 0.0163(10) -0.0004(8) -0.0008(10) -0.0011(8) C11 0.0204(10) 0.0213(9) 0.0225(11) -0.0033(8) 0.0019(10) 0.0001(8) C12 0.0212(10) 0.0242(9) 0.0253(12) -0.0053(9) -0.0043(10) 0.0043(8) C13 0.0281(11) 0.0249(9) 0.0188(11) 0.0006(9) -0.0038(10) 0.0051(9) C14 0.0242(10) 0.0198(8) 0.0176(10) 0.0014(8) 0.0011(9) 0.0000(8) C15 0.0160(9) 0.0169(8) 0.0156(10) 0.0012(8) -0.0022(9) -0.0026(7) C16 0.0181(9) 0.0141(7) 0.0136(9) 0.0029(7) 0.0013(9) -0.0035(7) C17 0.0189(9) 0.0138(8) 0.0198(10) 0.0010(8) -0.0001(9) 0.0010(7) C18 0.0164(9) 0.0190(8) 0.0191(11) 0.0003(8) -0.0016(9) 0.0000(8) C19 0.0223(10) 0.0199(8) 0.0240(11) -0.0088(9) 0.0027(10) -0.0002(8) C20 0.0211(10) 0.0144(8) 0.0183(10) -0.0046(8) 0.0013(9) 0.0032(7) C21 0.0239(10) 0.0192(9) 0.0198(11) 0.0015(8) -0.0001(10) 0.0031(8) C22 0.0252(11) 0.0191(9) 0.0356(13) -0.0004(10) 0.0034(11) -0.0018(9) C23 0.0226(10) 0.0265(10) 0.0353(14) -0.0118(10) -0.0049(11) 0.0027(9) C24 0.0311(11) 0.0309(10) 0.0202(12) -0.0063(9) -0.0042(10) 0.0105(10) C25 0.0301(11) 0.0200(9) 0.0190(11) 0.0004(8) 0.0033(10) 0.0029(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l _diffrn_refln_intensity_net _diffrn_refln_intensity_u 0 0 1 874.3 23.6 0 0 -1 916.19 23.97 0 0 2 117.86 7.88 0 0 -2 129.83 8.52 0 0 3 669.04 24.9 0 0 -3 629.87 25.55 0 0 4 233.67 14.8 0 0 4 222.14 10.95 0 0 -4 213.81 15.08 0 0 4 224.33 8.69 0 0 -5 66.94 9.2 0 0 5 76.81 6.72 0 0 6 11.16 2.99 0 0 7 0.55 1.67 0 1 1 41.74 2.96 0 -1 -1 39.47 3.15 0 1 1 42.19 2.38 0 1 -1 46.19 3.77 0 -1 1 42.73 3.68 0 -1 2 29.03 4.1 0 1 -2 27.43 3.93 0 1 2 27.81 3.53 0 -1 -2 29.76 4 0 1 2 19.28 2.16 0 1 3 72.56 6.81 0 -1 3 80.5 7.84 0 1 3 71.57 5.17 0 1 -3 71.06 7.55 0 -1 -3 64.89 7.25 0 1 -4 64.23 8 0 -1 4 41.07 6.6 0 -1 -4 52.78 7.46 0 1 4 53.94 6.73 0 1 4 58.93 5.32 0 1 4 58.47 3.65 0 1 -5 43.7 7.66 0 -1 -5 33.13 6.85 0 1 5 40.24 4.9 0 -1 5 34.38 4.5 0 1 6 21.1 3.96 0 -1 6 20.51 3.89 0 -1 7 51.85 6.2 0 1 7 58.34 6.68 0 -2 0 1517.69 31.94 0 2 0 1479.26 31.17 0 -2 0 1433.47 31.15 0 2 1 1490.74 34.11 0 -2 -1 1538.06 35.45 0 2 1 1508.99 33.46 0 2 -1 1497.37 33.42 0 -2 -1 1550.61 34.38 0 2 1 1571.05 34.26 0 -2 1 1416.89 37.74 0 -2 2 0.95 1.6 0 2 2 1.09 1.01 0 -2 -2 3.41 1.86 0 2 -2 2.59 1.66 0 2 2 1.02 0.45 0 -2 -2 1.12 0.34 0 -2 2 0.22 0.26 0 2 -2 0.52 0.37 0 2 2 1.49 0.83 0 2 2 0.7 0.31 0 2 3 429.32 17.27 0 -2 3 398.94 19.6 0 -2 -3 425.2 19.49 0 -2 -3 433.2 9.81 0 -2 3 425.1 9.76 0 2 3 419.69 14.73 0 2 -3 390.5 19.18 0 2 3 403.69 11.21 0 2 4 177.48 11.62 0 -2 4 172.7 13.42 0 2 4 180.91 9.7 0 -2 -4 165.68 13.24 0 2 -4 165.81 13.03 0 -2 -5 10.55 4.25 0 2 5 14.35 3.01 0 -2 5 14.09 2.83 0 -2 6 55.16 5.96 0 2 6 56.55 6.12 0 -2 7 -4.22 2.33 0 2 7 3.44 2.45 0 3 0 0.12 0.21 0 -3 0 0.15 0.19 0 3 0 0.33 0.45 0 -3 0 0.32 0.4 0 3 1 710.77 16.91 0 -3 -1 764.03 18.19 0 3 -1 705.81 17.87 0 3 1 717.54 17.94 0 3 1 723.51 17.85 0 -3 -1 734.64 18.03 0 3 2 339.34 11.51 0 -3 -2 329.32 13.74 0 -3 2 342 9.15 0 3 2 338.86 9.6 0 -3 -2 336.75 9.14 0 3 -2 325.46 9.4 0 3 2 324.92 11.16 0 -3 2 310.5 15.46 0 3 3 118.32 7.57 0 -3 -3 122.19 9.72 0 -3 3 116.99 4.05 0 -3 -3 128.8 4.25 0 3 3 109.45 6.63 0 3 3 121.71 3.95 0 -3 3 120.12 10.4 0 -3 4 389.15 21.23 0 3 4 367.48 14.86 0 -3 -4 351.58 19.74 0 3 5 1.35 1.52 0 -3 5 0.32 1.08 0 3 6 135 9.54 0 -3 6 112.76 8.56 0 3 7 4.03 2.22 0 -4 0 5452.41 115.32 0 4 0 5196 116.24 0 -4 0 5419.74 113.55 0 4 0 5450.31 113.63 0 -4 -1 178.16 6.04 0 4 1 183.93 8.22 0 4 1 168.77 6.68 0 4 -1 181.3 6.8 0 4 1 168.88 5.99 0 -4 -1 185.81 6.43 0 -4 1 184.51 5.64 0 -4 1 180.32 5.17 0 -4 -2 35.97 3.96 0 -4 2 44.97 5.66 0 4 2 37.79 2.78 0 4 2 43.32 3.3 0 -4 -2 36.4 3.2 0 -4 2 40.33 2.57 0 4 -2 38.54 2.72 0 -4 -2 39.66 2.53 0 4 2 41.4 2.85 0 -4 3 23.94 5.02 0 -4 -3 20.94 4 0 4 3 21.06 2.86 0 4 3 20.32 2.72 0 -4 -3 20.54 1.74 0 -4 3 18.8 1.61 0 4 3 24.4 2.01 0 -4 4 43.2 7.43 0 4 4 32.37 3.91 0 4 5 39.07 4.93 0 -4 5 41.62 4.37 0 -4 6 13.18 3.16 0 4 6 12.06 3.24 0 4 7 0.58 2.04 0 5 0 0.75 0.57 0 -5 0 -0.14 0.6 0 5 0 0.07 0.33 0 -5 0 0.25 0.33 0 -5 -1 342.78 9.91 0 5 1 339.43 11.33 0 5 1 374.41 12.86 0 5 -1 351.84 11.42 0 -5 1 337.53 9.34 0 -5 -1 344.62 10.34 0 5 1 336.06 9.81 0 -5 1 350.22 8.9 0 -5 2 1.7 2.02 0 5 2 1.89 0.7 0 -5 -2 1.55 1.24 0 -5 -2 0.44 0.66 0 5 2 0.79 0.67 0 5 2 1.29 0.77 0 5 -2 1.45 0.73 0 5 2 1.65 1.6 0 5 3 24.32 2.69 0 -5 -3 28.63 4.57 0 -5 3 34.5 6.23 0 5 3 34.71 2.73 0 -5 -3 28.63 2.32 0 5 -3 30.3 2.61 0 -5 3 31.6 2.35 0 5 3 30.91 3.36 0 -5 -4 287.52 17.28 0 5 4 273.4 12.43 0 -5 4 268.87 18.8 0 5 5 9.83 2.71 0 -5 5 3.82 1.74 0 5 6 118.24 9 0 5 7 42.58 5.88 0 5 7 42.86 8.29 0 6 0 734.32 17.11 0 -6 0 699.71 16.97 0 -6 0 734.37 19.45 0 6 0 697.01 20.3 0 -6 -1 80.39 3.82 0 6 -1 74.81 4.81 0 6 1 78.65 5.25 0 6 1 86.76 5.17 0 6 1 85.35 3.87 0 -6 -1 74.09 4.02 0 -6 1 80.01 3.34 0 6 2 239.83 7.7 0 -6 -2 265.66 10.87 0 6 -2 244.16 9.49 0 6 2 248.88 9.59 0 6 2 254.61 12.58 0 6 2 235.43 9.03 0 -6 -2 245.42 9.64 0 -6 2 238.08 8.24 0 -6 2 243.41 7.51 0 -6 -3 3.74 2.07 0 6 3 3.82 1.13 0 -6 3 1.69 2.86 0 6 3 5.63 1.6 0 -6 3 5.43 1.17 0 6 3 7.53 1.42 0 6 -3 4.81 1.27 0 -6 -3 6.57 1.26 0 6 3 5.2 2.63 0 -6 -4 9.14 3.47 0 -6 4 6.2 3.84 0 6 4 15.89 2.75 0 6 5 14.55 3.17 0 -6 5 7.89 2.41 0 6 6 2.02 3.24 0 6 6 -0.52 1.75 0 6 7 65.66 10.26 0 6 7 57.5 6.57 0 -7 0 0.88 0.97 0 7 0 0.53 0.64 0 -7 0 -0.09 0.38 0 7 0 0.1 0.37 0 -7 -1 78.34 3.96 0 7 1 80.23 5.37 0 7 -1 84.82 5.49 0 7 1 74.89 5.15 0 -7 1 78.15 3.33 0 -7 -1 81.69 4.3 0 7 1 76.57 3.76 0 7 -1 76.88 3.75 0 7 -1 76.52 3.58 0 -7 -2 482.34 16.05 0 -7 2 491.43 14.99 0 7 2 452.7 18.25 0 -7 -2 495.97 14.79 0 7 2 480.01 15.73 0 7 -2 485.23 15.72 0 -7 -2 451.02 15 0 7 2 478.44 14.55 0 -7 2 459.99 13.31 0 -7 2 471.89 12.46 0 -7 -3 601.26 23.54 0 7 3 642.92 19.08 0 7 -3 665.53 19.32 0 7 3 645.77 25.02 0 -7 3 635.43 18.16 0 -7 -3 626.38 18.07 0 7 3 660.92 19.93 0 -7 3 585.21 28.05 0 7 4 2.24 2.53 0 7 4 3.95 1.68 0 7 5 102.87 10.85 0 7 5 108.76 7.92 0 7 6 14.34 5.16 0 7 6 15.7 3.53 0 7 7 -1.11 4.13 0 7 7 1.68 2.08 0 -8 0 2869.43 64.68 0 8 0 2637.82 65.23 0 8 0 2735.08 60.54 0 -8 0 2804.42 60.41 0 -8 -1 875.56 22.05 0 8 -1 861.03 25.28 0 8 1 911.02 24.95 0 8 1 846.75 25.06 0 8 1 839.14 21.3 0 8 -1 871.36 21.66 0 -8 1 875.98 20.51 0 -8 -1 857.7 22.34 0 8 -1 857.25 21.12 0 -8 -2 95.37 6.04 0 -8 2 104.2 5.96 0 -8 -2 88.19 5.48 0 8 -2 102.31 6.41 0 8 2 99.97 6.29 0 8 2 100.95 7.63 0 8 2 101.16 5.32 0 -8 2 101.53 4.65 0 -8 -2 99.67 5.84 0 -8 -2 95.64 2.88 0 -8 2 96.64 4.12 0 -8 3 16.76 5.1 0 -8 -3 20.51 3.92 0 8 3 21.12 2.81 0 8 3 14.49 3.56 0 -8 3 17.86 2.4 0 -8 -3 17.24 2.33 0 8 -3 15.75 2.5 0 -8 -3 17.7 2.87 0 8 3 18.91 2.64 0 8 4 2.27 2.69 0 8 4 2.84 1.78 0 8 5 0.9 2.73 0 8 5 0.43 1.22 0 -8 5 -0.97 1.65 0 8 6 27.63 6.69 0 8 6 28.79 4.49 0 -8 6 28.02 4.7 0 9 0 0.34 0.74 0 -9 0 0.92 1.18 0 -9 0 0.24 0.45 0 9 0 -0.13 0.52 0 -9 -1 134.73 6.1 0 9 -1 141.15 8.14 0 9 1 141.75 8.18 0 -9 1 137.7 5.03 0 9 1 137.47 5.63 0 9 -1 143.59 5.92 0 -9 -1 146.47 6.42 0 9 -1 143 5.65 0 -9 -2 51.52 4.41 0 9 2 46.83 3.57 0 -9 -2 43.82 3.86 0 9 -2 51.63 4.73 0 9 2 51.3 4.69 0 -9 2 48.31 4.2 0 9 2 45.67 5.15 0 -9 -2 46.69 4.11 0 -9 -3 77.3 7.33 0 -9 3 85.32 5.58 0 9 3 79.49 5.82 0 -9 -3 80.85 5.39 0 9 -3 86.11 6.05 0 9 3 90.32 8.27 0 -9 -3 84.36 6.15 0 9 3 87.49 5.71 0 9 4 95.71 9.66 0 9 4 87.02 6.41 0 9 5 48.31 7.8 0 9 5 58.95 5.63 0 -9 5 46.95 5.69 0 9 6 16.21 5.33 0 9 6 19.47 3.78 0 -9 6 16.47 3.78 0 -10 0 139.6 8.26 0 10 0 131.88 8.25 0 10 0 126.37 5.52 0 -10 0 128.76 5.36 0 -10 -1 112.15 5.6 0 10 -1 114.75 7.58 0 10 1 111.89 7.48 0 -10 -1 110.05 5.69 0 10 -1 116.6 5.41 0 10 1 101.18 4.84 0 10 -1 106.41 4.95 0 -10 -2 8.77 2.03 0 10 2 7.95 1.54 0 -10 -2 10.28 2.12 0 -10 -2 9.07 2.05 0 10 -2 6.77 1.98 0 10 2 7.13 2.13 0 -10 2 7.95 1.99 0 10 2 10.58 2.8 0 -10 -3 86.05 7.73 0 10 3 84.57 8.13 0 10 -3 94.45 6.71 0 -10 -3 103.16 6.41 0 10 3 96.35 6.78 0 -10 3 93.29 6.28 0 10 3 99.53 6.12 0 10 4 26.8 5.43 0 10 4 19.74 3.02 0 10 5 -0.88 2.67 0 10 5 2.49 1.83 0 -10 5 1.11 1.88 0 10 6 1 3.2 0 10 6 -0.48 1.44 0 -10 6 -1.18 2.53 0 11 0 0.84 1.01 0 -11 0 -0.4 1.84 0 -11 0 1.36 1.03 0 11 0 0.17 0.69 0 11 0 0.36 0.93 0 -11 -1 203.08 8.48 0 -11 -1 193.41 9.87 0 -11 1 180.74 9.56 0 11 1 190.43 10.6 0 11 -1 211.41 11.15 0 11 -1 214.31 8.14 0 11 1 201.28 7.58 0 -11 -1 222 8.68 0 11 -1 203.62 7.67 0 -11 -2 165.38 8.67 0 -11 -2 165.03 9.01 0 11 2 168.02 9.75 0 11 -2 167.82 9.78 0 11 2 195.73 10.78 0 -11 2 172.15 9.21 0 11 2 172.93 7.46 0 -11 -2 162.32 8.27 0 11 -3 622.97 21.43 0 11 3 614.47 21.29 0 -11 3 630.85 20.64 0 -11 -3 598.78 20 0 11 3 625.92 24.34 0 11 3 595.9 18.93 0 11 4 19.04 4.59 0 11 4 14.47 2.85 0 11 5 2.59 2.93 0 11 5 2.04 1.57 0 -11 5 -1.77 2.28 0 11 6 92.38 11.12 0 11 6 101.58 7.94 0 -11 6 103.37 9.32 0 -12 0 0.75 0.69 0 12 0 1.38 1.2 0 12 0 -0.18 0.81 0 12 0 -0.58 1.08 0 12 1 17.36 3.23 0 -12 -1 20.96 3.26 0 12 -1 18.78 3.35 0 -12 -1 16.05 2.32 0 -12 1 22.75 3.37 0 12 1 20.2 2.24 0 12 -1 21.17 2.3 0 -12 -2 16.6 2.9 0 12 2 12.42 2.91 0 12 -2 17.17 3.23 0 -12 -2 20.72 3.18 0 -12 2 20.71 3.15 0 12 2 17.53 3.25 0 12 2 19.33 2.38 0 -12 3 2.73 1.39 0 12 3 -0.58 2.06 0 -12 -3 2.23 1.38 0 12 3 3.04 1.47 0 12 -3 1.31 1.41 0 12 3 3.29 1.41 0 12 4 13.68 4.16 0 12 4 15.73 2.9 0 12 5 0.85 2.72 0 12 5 0.4 1.62 0 -12 5 2.48 2.2 0 12 6 139.55 13.52 0 12 6 156.1 9.83 0 -12 6 158.97 11.92 0 -13 0 -0.41 1.07 0 13 0 0.99 1.41 0 13 0 -0.21 1.1 0 13 1 6.62 1.42 0 13 -1 8.42 2.55 0 -13 -1 6.66 2.1 0 -13 -1 4.79 1.54 0 -13 1 7.68 2.17 0 13 1 7.42 2.31 0 -13 -2 191.11 10.03 0 13 -2 200.72 11.61 0 -13 -2 204.16 11.02 0 13 2 197.45 11.47 0 -13 2 201.13 10.87 0 13 2 214.17 8.64 0 13 3 2.86 2.45 0 -13 3 2.14 1.45 0 13 -3 0.95 1.14 0 -13 -3 2.44 1.57 0 13 3 1.88 1.67 0 13 3 4.68 1.67 0 13 4 2.11 2.82 0 13 4 -0.34 1.4 0 13 5 32.15 6.22 0 13 5 32.6 4.25 0 -13 5 31.04 5.49 0 -14 0 83.17 6.89 0 14 0 81.51 7.51 0 14 0 84.61 5.07 0 -14 -1 91.1 5.98 0 14 1 96.1 8.12 0 14 -1 95.2 8.05 0 -14 -1 96.16 7.53 0 -14 1 93.08 7.29 0 14 -2 10.02 2.6 0 14 2 20.48 3.74 0 -14 -2 11.5 2.76 0 -14 2 13.93 2.94 0 14 2 15.29 2.32 0 14 -3 8.15 2.79 0 14 3 11.61 3.07 0 -14 -3 11.12 2.74 0 14 3 9.67 3.11 0 14 3 8.31 2.02 0 14 4 1.38 2.21 0 14 4 1.01 1.34 0 -14 4 0.58 2.33 0 14 5 20.82 5.3 0 14 5 22.17 3.59 0 -14 5 17.45 4.45 0 -15 0 0.48 1.25 0 15 0 0.57 1.37 0 15 -1 154.87 10.76 0 -15 -1 149.96 9.88 0 -15 1 152.18 9.74 0 15 1 140.49 10.23 0 -15 -1 143.22 8 0 15 2 24.71 4.53 0 -15 -2 25.05 4.15 0 -15 2 24.16 3.97 0 15 -2 20.31 4.13 0 -15 -3 25.13 4.13 0 15 -3 16.24 3.6 0 15 4 22.97 4.94 0 15 4 26.56 3.51 0 -15 4 28.37 4.82 0 15 5 38.97 6.66 0 15 5 29.62 4.05 0 -16 0 16.88 3.65 0 16 0 18.2 4.23 0 -16 1 -1.01 2.09 0 16 -1 2.42 2.42 0 -16 -1 2.13 1.97 0 16 1 0.6 2.15 0 -16 -1 2.4 1.42 0 -16 1 1.36 1.61 0 -16 2 -1.55 2.21 0 16 -2 -1.79 3 0 16 2 -0.59 2.3 0 -16 -2 -2.72 2.85 0 -16 2 0.5 1.84 0 -16 -3 0.52 1.77 0 16 -3 -1.14 2.45 0 -16 3 -0.55 2.43 0 -16 4 -0.62 2.5 0 -17 0 1.65 1.67 0 17 0 -0.64 1.68 0 17 1 97.08 9.05 0 -17 1 114.09 9 0 17 -1 120.57 9.99 0 -17 -1 126.8 9.79 0 17 -2 0.63 2.43 0 -17 -2 0.59 2.27 0 17 2 -0.63 2.01 0 -17 2 -0.55 2.35 0 -17 2 1.58 2.11 0 -17 3 4.6 2.68 0 -17 4 3.21 2.38 0 18 0 184.36 12.99 0 -18 0 209.31 12.83 0 18 1 13.4 3.74 0 18 -1 16.05 3.87 0 -18 -1 17.25 4.03 0 -18 1 10.89 3.43 0 18 -2 15.7 4.22 0 -18 -2 16.43 4.45 0 18 2 13.75 3.79 0 -18 2 20.97 4.47 0 -18 2 17.35 4.04 0 -18 3 -1.2 3.08 0 -19 0 1.61 1.56 0 19 0 0.7 2.6 0 -19 0 -1.25 2.33 0 19 1 143.56 11.55 0 -19 1 152.58 11.22 0 19 -1 149.96 11.92 0 -19 -1 158.42 11.8 0 19 -2 79 8.61 0 -19 2 75.28 8.11 0 19 2 78.52 8.6 0 -19 -2 95.23 9.28 0 -19 3 10.01 3.55 0 -20 0 13.34 4.11 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11.43 4.01 -9 0 2 17.14 1.49 -9 0 -2 19.47 2.75 9 0 -2 17.47 1.93 -9 0 2 16.46 1.67 9 0 -2 16.75 2 9 0 2 16.07 3.59 -9 0 -3 165.01 15.53 9 0 3 177.64 12.93 9 0 -3 174.59 7.73 9 0 3 178.8 7.85 9 0 -3 174.56 7.9 -9 0 3 167.48 6.88 9 0 -3 170.37 7.44 9 0 3 154.21 11.32 -9 0 -4 13.84 5.75 -9 0 4 14.76 2.24 -9 0 -5 14.51 6.7 -9 0 -6 30.32 8.98 -9 0 -7 11.16 7.46 -9 -1 -7 97.64 15.97 -9 -1 -6 12.49 7.16 -9 -1 -5 44.84 10.19 -9 1 5 43.28 4.19 -9 -1 -4 231.49 20.34 -9 1 4 223.92 9.35 9 -1 3 2.28 2.57 -9 -1 -3 1.12 2.68 9 1 -3 3.52 1.13 9 1 -3 2.7 1.21 -9 1 3 5.09 1.28 9 1 -3 2.02 1.08 9 -1 3 4.77 2.92 9 -1 2 155.68 11.24 -9 1 2 148.78 5.19 -9 -1 -2 143.67 12.59 -9 -1 -2 141.27 7.78 9 1 -2 148.15 7.11 9 1 -2 144.95 5.9 -9 1 2 145.26 5.75 9 -1 2 137.9 10.3 9 -1 2 142.24 5.25 9 1 -2 138.65 6.36 -9 -1 -1 1915.2 54.97 -9 1 1 1972.37 47.13 9 -1 1 1943.03 51.8 9 1 -1 1929.51 46.68 -9 1 1 1897.4 44.29 9 -1 1 1961.33 45.26 9 1 -1 1998.03 42.96 -9 -1 -1 1997.16 55.28 9 -1 1 1947.72 51.81 -9 1 0 875.35 28.01 -9 -1 0 867.36 26.89 9 -1 0 856.36 24.1 9 1 0 933.26 22.91 9 -1 0 869.32 21.43 9 1 0 884.22 21.09 -9 1 0 865.35 22.55 -9 -1 0 868.84 21.33 -9 1 0 873.05 30.25 -9 1 0 871.74 21.05 9 -1 -1 1988.26 42.32 -9 1 -1 2007.03 56.04 9 1 1 1916.71 49.09 -9 -1 1 1974.2 45.43 9 1 1 1976.42 46.68 -9 -1 1 1910.15 43.39 9 -1 -1 1896.65 43.22 9 1 1 1924.22 44.75 9 1 1 1917.29 43.58 -9 1 -1 1952.2 57.7 -9 1 -2 146.28 13.03 9 1 2 140.95 9.82 -9 -1 2 146.52 5.24 -9 1 -2 153.13 7.42 9 1 2 138.96 7.01 9 -1 -2 144.51 6.17 -9 -1 2 145.27 5.32 9 1 2 144.96 9.18 -9 1 -3 5.75 3.9 9 1 3 3.9 2.41 9 1 3 2.43 1.01 9 -1 -3 3.38 1.24 -9 -1 3 2.82 0.94 9 -1 -3 4.05 1.21 9 1 3 1.58 1.96 9 1 4 224.64 10.92 9 -1 -4 227.24 10.4 -9 -1 4 226.86 9.1 -9 1 -4 227.57 20.17 -9 1 -5 24.26 7.96 -9 1 -6 31.98 9.54 -9 1 -7 75.06 13.81 -9 -2 -6 30.26 9.56 -9 2 6 38.81 4.44 -9 -2 -5 78.07 12.85 -9 2 5 64.98 5.25 -9 -2 -4 61.07 10.4 -9 2 4 80.25 5.23 9 -2 3 86.25 9.65 -9 -2 -3 99.42 11.84 9 2 -3 101.43 5.57 -9 2 3 102.19 5.31 9 2 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489.92 12.34 9 -3 -1 478.27 13.35 9 3 1 478.68 13.79 -9 -3 1 498.16 14.21 -9 3 -1 492.59 22.79 -9 3 -2 71.74 9.33 9 3 2 53.17 5.44 9 3 2 52.38 4.06 9 -3 -2 58.53 3.83 -9 -3 2 51.2 2.53 9 3 3 84.42 7.58 -9 3 -3 81.48 11.37 9 -3 -3 77.91 5.35 9 -3 -3 82.09 4.49 -9 3 -4 97.08 13.29 9 3 4 95.02 7.28 -9 3 -5 33.55 8.75 -9 3 -6 6.88 5.83 9 3 6 12.1 3.44 -9 3 -7 22.79 8.2 -9 -4 -6 10.58 6.54 -9 4 6 4.95 2.27 -9 -4 -5 320.61 25.55 -9 4 5 292.55 12.37 -9 -4 -4 32.08 7.75 -9 4 4 38.74 3.72 -9 -4 -3 189.23 16.22 9 -4 3 190.56 15.08 -9 4 3 207.19 8.4 9 -4 3 187.87 8.98 -9 4 3 204.66 11.59 9 4 -3 193.03 9.12 -9 -4 -2 283.82 17.48 9 -4 2 278.74 17.09 -9 -4 -2 300.49 13.1 9 -4 2 291.36 10.94 -9 4 2 297.1 10.02 9 4 -2 276.47 10.65 -9 4 2 286.11 14.73 -9 -4 -2 288.55 15.5 9 -4 1 120.05 9.73 -9 -4 -1 136.58 9.67 -9 -4 -1 125.56 6.74 9 4 -1 129.9 6.87 -9 4 1 138.11 6.26 9 -4 1 136.9 6.25 9 4 -1 146.42 4.12 9 -4 1 141.92 11.11 -9 4 1 154.92 11.48 9 4 -1 125.66 6.13 9 -4 0 481.09 18.08 -9 -4 0 483.63 16.56 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302.26 9.15 11 -2 -2 296.92 10.18 11 2 2 310.62 10.24 -11 2 -3 68.96 11.06 11 2 3 71.34 5.15 11 -2 -3 79.91 5.27 11 -2 -3 82.04 4.83 -11 2 -4 95.79 13.58 -11 2 -5 125.08 16.74 -11 2 -6 15.14 7.03 -11 -3 -6 218.33 23.47 -11 -3 -5 18.96 8.05 -11 3 5 13.07 2.5 -11 -3 -4 128.96 15.75 -11 3 4 166.42 7.84 -11 -3 -3 274.55 21.11 11 3 -3 281.59 11.17 -11 3 3 277.13 10.11 11 3 -3 266.48 10.97 11 -3 3 256.45 17.07 11 -3 2 15.13 4.24 -11 -3 -2 16.82 4.81 11 3 -2 11.1 2.18 -11 -3 -2 14.96 2.87 -11 3 2 20.27 2.28 11 3 -2 16.61 2.31 -11 -3 -2 15.72 4.22 11 -3 2 18.09 4.33 11 -3 2 14.92 2.4 -11 3 2 22.58 4.35 11 -3 1 320.22 16.03 -11 -3 -1 338.61 18 11 3 -1 319.73 12.53 -11 3 1 314.89 11.16 11 -3 1 318.48 11.06 11 3 -1 328.81 8.73 -11 3 1 321.67 18 11 -3 1 322.31 16.6 -11 -3 -1 320.51 16.67 11 3 -1 336.8 11.51 -11 3 1 327.43 13.67 -11 3 0 297.12 15.72 11 -3 0 303.42 12.96 -11 -3 0 297.44 13.88 11 3 0 313.39 10.27 11 3 0 300.3 12.08 11 -3 0 311.48 9.91 11 3 0 297.56 8.87 -11 3 0 317.77 11.43 -11 -3 0 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4.95 -23 -3 1 24.13 7.47 23 3 2 1.73 2.05 -23 -3 2 2.68 3.8 -23 -3 3 64.31 10.67 -23 -4 -3 5.93 6.36 23 4 -2 6.29 2.88 -23 -4 -2 8.77 6.24 -23 -4 -2 12.04 6.64 -23 4 2 5.34 5.39 23 4 -1 15.75 3.96 -23 4 1 11.23 6.95 -23 -4 -1 11.24 6.21 23 4 0 7.05 2.89 -23 -4 0 7.37 5.47 23 4 1 8.24 3.16 -23 -4 1 10.98 5.5 23 4 2 8.72 3.3 -23 -4 2 10.47 5.06 -23 -5 -3 55.22 12.55 -23 -5 -2 3.49 4.95 -23 5 2 12.77 6.77 23 5 -1 62.25 7.07 -23 -5 -1 62.06 11.82 23 5 0 3.56 2.46 -23 -5 0 2.84 4.03 23 5 1 81.96 8.02 -23 -5 1 75.93 11.8 -23 -6 -2 -1.74 4.57 -23 -6 -1 6.01 4.83 -23 -6 0 125.52 15.36 -23 -6 1 10.43 4.84 -23 -7 -2 -1.73 5.56 -23 7 1 12.45 3.52 -23 -7 -1 14.61 6.46 -23 -7 0 1.34 3.81 -23 -7 1 17.95 6 -23 -8 -2 17.26 7.63 -23 8 1 33.7 5.36 -23 -8 0 1.31 3.72 -23 -9 -1 15.26 6.74 -23 9 1 5.51 2.64 -23 -9 0 1.29 3.38 -23 -10 0 36.61 8.04 24 0 0 154.47 11.57 -24 0 0 181.72 21.07 24 0 -1 -0.63 3.16 24 0 1 1.88 2.42 -24 0 1 -1.71 4.5 24 0 -2 25.2 5 24 0 2 24.41 4.87 -24 0 2 19.3 7.53 -24 0 3 15.03 6.64 -24 1 3 14.1 6.29 24 -1 2 48.32 6.53 24 1 -2 42.49 6.23 -24 1 2 38.52 10.03 24 1 -1 0.62 2.82 -24 -1 -1 7.51 6.36 -24 1 1 1.79 4.69 24 -1 0 52.81 6.93 24 1 0 54.34 6.82 -24 1 0 58.92 12.6 -24 -1 0 66.98 12.99 24 -1 -1 -0.64 2.74 24 1 1 -1.86 2.97 -24 -1 1 1.65 4.67 24 -1 -2 38.77 6.03 24 1 2 51.99 6.64 -24 -1 2 55.52 10.87 -24 2 3 3.27 5.25 24 -2 2 0.63 2.7 24 2 -2 -1.79 3.07 -24 2 2 3.49 5.9 24 2 -1 17.76 4.47 24 -2 1 23.4 5.09 -24 -2 -1 21.86 8.52 -24 2 1 31.58 10.16 24 2 0 1.85 2.56 24 -2 0 -1.97 2.54 -24 -2 0 1.69 5.13 24 2 1 21.41 4.61 24 -2 -1 23.49 5.16 -24 -2 1 22.19 7.41 24 -2 -2 -0.64 2.89 24 2 2 1.19 2.56 -24 -2 2 5.94 4.77 -24 -3 -3 22.3 8.96 24 3 -2 25.41 4.89 24 -3 2 25.67 5.13 -24 3 2 34.42 10.1 24 3 -1 17.54 4.26 -24 -3 -1 5.28 5.35 24 3 0 32.92 5.51 -24 -3 0 35.94 9.92 24 3 1 22.4 4.65 -24 -3 1 15.24 6.54 24 3 2 24.36 4.83 24 -3 -2 21.33 4.92 -24 -3 2 28.74 8.01 24 4 -2 9.48 3.48 -24 4 2 11.23 6.65 24 4 -1 13.29 3.73 -24 -4 -1 28.96 9.49 24 4 0 8.52 3.13 -24 -4 0 9.49 6.34 24 4 1 17.02 4.18 -24 -4 1 19.17 6.71 24 4 2 10.19 3.46 -24 -4 2 8.39 4.97 -24 5 2 28.55 9.14 24 5 -1 15.18 3.97 -24 -5 -1 29.66 9.01 24 5 0 4.29 2.78 -24 -5 0 1.53 4.01 24 5 1 14.09 3.84 -24 -5 1 11.47 5.75 -24 -6 -1 1.6 4.2 -24 -6 0 14.79 6.14 -24 -6 1 5.59 4.97 -24 -7 -1 26.47 8.36 -24 -7 0 61.99 11.21 -24 8 1 33.52 5.53 -24 -8 0 1.41 3.37 25 0 0 -0.65 2.88 -25 0 0 7.72 7.45 25 0 -1 1.3 2.6 25 0 1 4.52 3.39 25 0 -2 -1.27 2.35 25 0 2 0.63 2.23 25 -1 2 2.54 2.45 25 1 -2 1.87 2.32 25 -1 1 82.03 8.55 25 1 -1 80.12 8.38 -25 1 1 85.04 15.11 25 -1 0 8.63 3.63 25 1 0 13.53 4.09 -25 1 0 17.88 7.97 -25 -1 0 13.06 7.21 25 -1 -1 94.26 9.08 25 1 1 84.92 8.62 -25 -1 1 73.71 13.28 25 -1 -2 4.49 3 25 1 2 0.62 2.39 25 -2 2 4.53 3.02 25 2 -2 6.76 3.42 25 -2 1 6.68 3.12 25 2 -1 1.89 2.61 -25 -2 -1 1.91 5.4 -25 2 1 3.91 5.92 25 -2 0 18.9 4.77 25 2 0 31.1 5.46 -25 -2 0 25.18 8.41 25 -2 -1 8.71 3.59 25 2 1 5.67 3.17 25 -2 -2 8.49 3.5 25 2 2 5.52 3.08 25 3 -2 31.08 5.34 25 3 -1 7.46 3.33 25 -3 1 5.44 3.26 -25 3 1 2 5.26 -25 -3 -1 11.12 6.88 25 3 0 7.53 3.23 25 -3 0 17.12 4.53 -25 -3 0 5.21 4.93 25 3 1 5.6 3.13 25 -3 -1 5.43 3.33 -25 -3 1 6.53 5.25 25 -3 -2 34.5 5.9 25 4 -1 9.35 3.28 -25 -4 -1 10.78 6.67 25 4 0 2.51 2.6 -25 -4 0 1.68 5.1 25 4 1 10.63 3.55 -25 -5 -1 64.53 13.14 -25 -5 0 1.64 4.29 -25 -6 -1 3.39 5.44 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 C7 O1 H1 109.5 . . ? C1 N1 H1A 113.8 . . ? C1 N1 C8 108.43(15) . . ? C8 N1 H1A 114.4 . . ? C15 N2 C18 108.77(14) . . ? C15 N2 C19 124.20(15) . . ? C18 N2 C19 126.58(16) . . ? C2 C1 N1 127.59(18) . . ? C2 C1 C6 121.39(17) . . ? C6 C1 N1 110.95(16) . . ? C1 C2 H2 121.2 . . ? C1 C2 C3 117.70(19) . . ? C3 C2 H2 121.2 . . ? C2 C3 H3 119.4 . . ? C4 C3 C2 121.21(19) . . ? C4 C3 H3 119.4 . . ? C3 C4 H4 119.8 . . ? C5 C4 C3 120.40(18) . . ? C5 C4 H4 119.8 . . ? C4 C5 H5 120.6 . . ? C6 C5 C4 118.82(19) . . ? C6 C5 H5 120.6 . . ? C1 C6 C7 108.94(16) . . ? C5 C6 C1 120.46(18) . . ? C5 C6 C7 130.44(18) . . ? O1 C7 C6 116.89(16) . . ? O1 C7 H7 106.7 . . ? O1 C7 C8 116.05(15) . . ? C6 C7 H7 106.7 . . ? C6 C7 C8 103.21(15) . . ? C8 C7 H7 106.7 . . ? N1 C8 C7 101.54(13) . . ? N1 C8 C9 111.92(15) . . ? N1 C8 C16 110.28(14) . . ? C9 C8 C7 110.72(15) . . ? C16 C8 C7 110.84(15) . . ? C16 C8 C9 111.18(14) . . ? C10 C9 C8 119.58(17) . . ? C14 C9 C8 121.67(17) . . ? C14 C9 C10 118.75(17) . . ? C9 C10 H10 119.8 . . ? C11 C10 C9 120.50(19) . . ? C11 C10 H10 119.8 . . ? C10 C11 H11 119.9 . . ? C10 C11 C12 120.3(2) . . ? C12 C11 H11 119.9 . . ? C11 C12 H12 120.2 . . ? C13 C12 C11 119.52(18) . . ? C13 C12 H12 120.2 . . ? C12 C13 H13 120.0 . . ? C12 C13 C14 120.09(19) . . ? C14 C13 H13 120.0 . . ? C9 C14 C13 120.85(19) . . ? C9 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? N2 C15 H15 125.4 . . ? N2 C15 C16 109.17(16) . . ? C16 C15 H15 125.4 . . ? C15 C16 C8 127.07(17) . . ? C15 C16 C17 106.16(16) . . ? C17 C16 C8 126.76(16) . . ? C16 C17 H17 126.2 . . ? C18 C17 C16 107.61(16) . . ? C18 C17 H17 126.2 . . ? N2 C18 C17 108.28(16) . . ? N2 C18 H18 125.9 . . ? C17 C18 H18 125.9 . . ? N2 C19 H19A 109.3 . . ? N2 C19 H19B 109.3 . . ? N2 C19 C20 111.70(15) . . ? H19A C19 H19B 107.9 . . ? C20 C19 H19A 109.3 . . ? C20 C19 H19B 109.3 . . ? C21 C20 C19 120.42(19) . . ? C25 C20 C19 120.62(18) . . ? C25 C20 C21 118.94(19) . . ? C20 C21 H21 119.7 . . ? C22 C21 C20 120.5(2) . . ? C22 C21 H21 119.7 . . ? C21 C22 H22 119.9 . . ? C23 C22 C21 120.1(2) . . ? C23 C22 H22 119.9 . . ? C22 C23 H23 120.1 . . ? C24 C23 C22 119.76(19) . . ? C24 C23 H23 120.1 . . ? C23 C24 H24 119.8 . . ? C23 C24 C25 120.5(2) . . ? C25 C24 H24 119.8 . . ? C20 C25 H25 119.9 . . ? C24 C25 C20 120.1(2) . . ? C24 C25 H25 119.9 . . ? 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 O1 H1 0.8400 . ? O1 C7 1.408(2) . ? N1 H1A 0.8798 . ? N1 C1 1.416(2) . ? N1 C8 1.497(2) . ? N2 C15 1.365(2) . ? N2 C18 1.370(2) . ? N2 C19 1.480(2) . ? C1 C2 1.383(3) . ? C1 C6 1.391(3) . ? C2 H2 0.9500 . ? C2 C3 1.397(2) . ? C3 H3 0.9500 . ? C3 C4 1.389(3) . ? C4 H4 0.9500 . ? C4 C5 1.387(3) . ? C5 H5 0.9500 . ? C5 C6 1.386(2) . ? C6 C7 1.500(3) . ? C7 H7 1.0000 . ? C7 C8 1.583(2) . ? C8 C9 1.524(3) . ? C8 C16 1.515(3) . ? C9 C10 1.393(3) . ? C9 C14 1.386(3) . ? C10 H10 0.9500 . ? C10 C11 1.387(3) . ? C11 H11 0.9500 . ? C11 C12 1.389(3) . ? C12 H12 0.9500 . ? C12 C13 1.382(3) . ? C13 H13 0.9500 . ? C13 C14 1.390(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C15 C16 1.378(2) . ? C16 C17 1.424(3) . ? C17 H17 0.9500 . ? C17 C18 1.375(3) . ? C18 H18 0.9500 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.508(3) . ? C20 C21 1.391(3) . ? C20 C25 1.387(3) . ? C21 H21 0.9500 . ? C21 C22 1.381(3) . ? C22 H22 0.9500 . ? C22 C23 1.380(3) . ? C23 H23 0.9500 . ? C23 C24 1.376(3) . ? C24 H24 0.9500 . ? C24 C25 1.386(3) . ? C25 H25 0.9500 . ? 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 O1 C7 C8 N1 154.01(15) . . . . ? O1 C7 C8 C9 -87.0(2) . . . . ? O1 C7 C8 C16 36.9(2) . . . . ? N1 C1 C2 C3 -177.43(17) . . . . ? N1 C1 C6 C5 178.15(16) . . . . ? N1 C1 C6 C7 2.2(2) . . . . ? N1 C8 C9 C10 154.80(16) . . . . ? N1 C8 C9 C14 -25.4(2) . . . . ? N1 C8 C16 C15 129.41(19) . . . . ? N1 C8 C16 C17 -52.2(2) . . . . ? N2 C15 C16 C8 178.28(17) . . . . ? N2 C15 C16 C17 -0.4(2) . . . . ? N2 C19 C20 C21 82.7(2) . . . . ? N2 C19 C20 C25 -96.0(2) . . . . ? C1 N1 C8 C7 -24.68(17) . . . . ? C1 N1 C8 C9 -142.81(14) . . . . ? C1 N1 C8 C16 92.87(16) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C1 C6 C7 O1 -146.05(16) . . . . ? C1 C6 C7 C8 -17.39(19) . . . . ? C2 C1 C6 C5 0.9(3) . . . . ? C2 C1 C6 C7 -175.01(16) . . . . ? C2 C3 C4 C5 1.2(3) . . . . ? C3 C4 C5 C6 -1.0(3) . . . . ? C4 C5 C6 C1 0.0(3) . . . . ? C4 C5 C6 C7 174.89(19) . . . . ? C5 C6 C7 O1 38.6(3) . . . . ? C5 C6 C7 C8 167.22(18) . . . . ? C6 C1 C2 C3 -0.7(3) . . . . ? C6 C7 C8 N1 24.82(18) . . . . ? C6 C7 C8 C9 143.81(16) . . . . ? C6 C7 C8 C16 -92.32(17) . . . . ? C7 C8 C9 C10 42.3(2) . . . . ? C7 C8 C9 C14 -137.95(16) . . . . ? C7 C8 C16 C15 -118.9(2) . . . . ? C7 C8 C16 C17 59.5(2) . . . . ? C8 N1 C1 C2 -167.73(17) . . . . ? C8 N1 C1 C6 15.26(19) . . . . ? C8 C9 C10 C11 179.41(16) . . . . ? C8 C9 C14 C13 -178.95(17) . . . . ? C8 C16 C17 C18 -178.22(18) . . . . ? C9 C8 C16 C15 4.7(3) . . . . ? C9 C8 C16 C17 -176.91(17) . . . . ? C9 C10 C11 C12 -0.4(3) . . . . ? C10 C9 C14 C13 0.8(3) . . . . ? C10 C11 C12 C13 0.6(3) . . . . ? C11 C12 C13 C14 -0.2(3) . . . . ? C12 C13 C14 C9 -0.5(3) . . . . ? C14 C9 C10 C11 -0.4(3) . . . . ? C15 N2 C18 C17 0.1(2) . . . . ? C15 N2 C19 C20 -168.95(17) . . . . ? C15 C16 C17 C18 0.5(2) . . . . ? C16 C8 C9 C10 -81.38(19) . . . . ? C16 C8 C9 C14 98.4(2) . . . . ? C16 C17 C18 N2 -0.4(2) . . . . ? C18 N2 C15 C16 0.2(2) . . . . ? C18 N2 C19 C20 19.5(3) . . . . ? C19 N2 C15 C16 -172.60(17) . . . . ? C19 N2 C18 C17 172.69(18) . . . . ? C19 C20 C21 C22 -176.84(17) . . . . ? C19 C20 C25 C24 177.40(17) . . . . ? C20 C21 C22 C23 -0.9(3) . . . . ? C21 C20 C25 C24 -1.3(3) . . . . ? C21 C22 C23 C24 -0.8(3) . . . . ? C22 C23 C24 C25 1.3(3) . . . . ? C23 C24 C25 C20 -0.3(3) . . . . ? C25 C20 C21 C22 1.9(3) . . . . ?