#------------------------------------------------------------------------------ #$Date: 2021-11-10 01:16:51 +0200 (Wed, 10 Nov 2021) $ #$Revision: 270546 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/51/1565147.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_1565147 loop_ _publ_author_name 'Wang, Lele' 'Han, Hua-Bin' 'Gu, Lijie' 'Zhang, Wenjing' 'Zhao, Junwei' 'Wang, Qi-Lin' _publ_section_title ; Skeletal remodeling of chalcone-based pyridinium salts to access isoindoline polycycles and their bridged derivatives ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC05741C _journal_year 2021 _chemical_formula_moiety 'C26 H23 N3 O4' _chemical_formula_sum 'C26 H23 N3 O4' _chemical_formula_weight 441.47 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2019-12-18 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-03-18 deposited with the CCDC. 2021-11-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 115.198(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.0994(5) _cell_length_b 10.9354(3) _cell_length_c 16.3508(6) _cell_measurement_reflns_used 2870 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 70.3790 _cell_measurement_theta_min 5.0380 _cell_volume 2281.11(15) _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _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 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.2312 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _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 -52.00 35.00 1.00 2.10 -- -33.50 57.00 0.00 87 2 \w -4.00 77.00 1.00 2.10 -- 36.47 -99.00 150.00 81 3 \w 58.00 92.00 1.00 2.10 -- 36.47 178.00 -60.00 34 4 \w 66.00 96.00 1.00 2.10 -- 36.47 178.00-150.00 30 5 \w 76.00 110.00 1.00 2.10 -- 36.47 178.00 90.00 34 6 \w -1.00 77.00 1.00 2.10 -- 36.47 -99.00 -60.00 78 7 \w 9.00 38.00 1.00 2.10 -- 36.47 77.00 90.00 29 8 \w 63.00 104.00 1.00 2.10 -- 36.47 77.00 90.00 41 9 \w 47.00 73.00 1.00 14.50 -- 108.00 -30.00-150.00 26 10 \w 78.00 118.00 1.00 14.50 -- 108.00 -45.00 150.00 40 11 \w 46.00 103.00 1.00 14.50 -- 108.00 -94.00-180.00 57 12 \w 98.00 127.00 1.00 14.50 -- 108.00 -30.00-150.00 29 13 \w 113.00 172.00 1.00 14.50 -- 108.00 111.00 150.00 59 14 \w 96.00 173.00 1.00 14.50 -- 108.00 61.00 -60.00 77 15 \w 45.00 109.00 1.00 14.50 -- 108.00 -45.00 0.00 64 16 \w 63.00 178.00 1.00 14.50 -- 108.00 15.00-120.00 115 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0864300000 _diffrn_orient_matrix_UB_12 -0.0927519000 _diffrn_orient_matrix_UB_13 0.0536231000 _diffrn_orient_matrix_UB_21 -0.0744726000 _diffrn_orient_matrix_UB_22 -0.0620072000 _diffrn_orient_matrix_UB_23 0.0341683000 _diffrn_orient_matrix_UB_31 -0.0395202000 _diffrn_orient_matrix_UB_32 -0.0860887000 _diffrn_orient_matrix_UB_33 -0.0824242000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_unetI/netI 0.0288 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 8092 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 67.066 _diffrn_reflns_theta_max 67.066 _diffrn_reflns_theta_min 5.029 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.94327 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) 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 1.285 _exptl_crystal_description prism _exptl_crystal_F_000 928 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.253 _refine_diff_density_min -0.198 _refine_diff_density_rms 0.040 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 4065 _refine_ls_number_restraints 30 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0445 _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^)+(0.0652P)^2^+0.2535P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1156 _refine_ls_wR_factor_ref 0.1275 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3204 _reflns_number_total 4065 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc05741c2.cif _cod_data_source_block wll148 _cod_original_cell_volume 2281.11(14) _cod_database_code 1565147 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula C40H40O2N4 _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 0.938 _shelx_estimated_absorpt_t_min 0.894 _reflns_odcompleteness_completeness 99.72 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _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 C24-N3A 1.45 with sigma of 0.02 O4A-N3A 1.4 with sigma of 0.02 N2A-C11 1.45 with sigma of 0.02 N2A-O2A 1.2 with sigma of 0.02 3. Rigid bond restraints N3, O4 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 N2, O2 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(N2) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O4) = Uanis(O4A) Uanis(N3) = Uanis(N3A) Uanis(O2) = Uanis(O2A) Uanis(O1) = Uanis(O1A) Uanis(N2) = Uanis(N2A) 5. Others Sof(O4A)=Sof(N3A)=1-FVAR(1) Sof(O4)=Sof(N3)=FVAR(1) Sof(O2A)=Sof(O1A)=Sof(N2A)=1-FVAR(2) Sof(O1)=Sof(O2)=Sof(N2)=FVAR(2) 6.a Ternary CH refined with riding coordinates: C8(H8), C9(H9), C10(H10) 6.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B) 6.c Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21) 6.d Idealised Me refined as rotating group: C25(H25A,H25B,H25C), C26(H26A,H26B,H26C) ; _shelx_res_file ; wll148.res created by SHELXL-2014/7 TITL WLL148 in P21/c #14 REM reset to P21/c #14 CELL 1.54184 14.099395 10.935373 16.350793 90 115.1975 90 ZERR 4 0.000454 0.000274 0.000562 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 104 92 12 16 DFIX 1.45 C24 N3A DFIX 1.4 O4A N3A DFIX 1.45 N2A C11 DFIX 1.2 N2A O2A DELU N3 O4 DELU N2 O2 ISOR 0.01 0.02 N2 O2 N3 O4 EADP O4 O4A EADP N3 N3A EADP O2 O2A EADP O1 O1A EADP N2 N2A L.S. 4 0 0 PLAN 20 SIZE 0.09 0.1 0.16 MPLA C1 C2 C3 C4 C5 C6 MPLA C8 C10 C11 C12 N1 MPLA C8 C9 C10 MPLA C14 C15 C16 C17 C18 C19 MPLA C22 C23 C24 O4 N3 bond $h conf fmap 2 acta REM REM REM WGHT 0.065200 0.253500 FVAR 5.34776 0.64437 0.92146 PART 1 O1 4 0.038139 0.543267 0.652866 31.00000 0.05935 0.09567 = 0.06244 0.00350 0.03350 0.01040 O2 4 0.089115 0.667072 0.575161 31.00000 0.06380 0.05116 = 0.07316 -0.00678 0.02582 0.00040 PART 0 O3 4 0.371993 0.346462 0.479974 11.00000 0.05449 0.06698 = 0.07999 0.02009 0.03319 0.01542 PART 1 O4 4 0.590928 0.809853 0.675683 21.00000 0.06396 0.05525 = 0.05469 0.00046 0.02599 -0.01649 PART 0 N1 3 0.165162 0.252969 0.585929 11.00000 0.05162 0.05426 = 0.05001 0.01185 0.01760 -0.00703 PART 1 N2 3 0.086261 0.561991 0.604635 31.00000 0.03633 0.06921 = 0.04363 -0.00876 0.01115 -0.00556 N3 3 0.608296 0.739864 0.753230 21.00000 0.05137 0.06101 = 0.04581 -0.00189 0.01280 -0.02316 PART 0 C1 1 0.139269 -0.058619 0.498582 11.00000 0.07656 0.05089 = 0.09989 0.00924 0.00809 -0.01386 AFIX 43 H1 2 0.113096 -0.112412 0.528008 11.00000 -1.20000 AFIX 0 C2 1 0.154760 -0.096285 0.425163 11.00000 0.08580 0.05165 = 0.10699 -0.01084 0.00389 -0.00533 AFIX 43 H2 2 0.137738 -0.175987 0.404171 11.00000 -1.20000 AFIX 0 C3 1 0.195280 -0.017626 0.381888 11.00000 0.09381 0.06410 = 0.08018 -0.01441 0.01102 0.01028 AFIX 43 H3 2 0.204316 -0.044652 0.331739 11.00000 -1.20000 AFIX 0 C4 1 0.222749 0.101911 0.412718 11.00000 0.07456 0.05515 = 0.06348 -0.00068 0.01653 0.00820 AFIX 43 H4 2 0.251525 0.154517 0.384641 11.00000 -1.20000 AFIX 0 C5 1 0.206042 0.140026 0.486099 11.00000 0.05017 0.04353 = 0.05509 0.00594 0.00671 0.00150 C6 1 0.163321 0.061039 0.528127 11.00000 0.05650 0.05006 = 0.06956 0.01080 0.00734 -0.00712 C7 1 0.150039 0.124511 0.603674 11.00000 0.06487 0.06081 = 0.07103 0.01978 0.02157 -0.01302 AFIX 23 H7A 2 0.080690 0.110855 0.600755 11.00000 -1.20000 H7B 2 0.202361 0.098139 0.662146 11.00000 -1.20000 AFIX 0 C8 1 0.228722 0.262245 0.534343 11.00000 0.04134 0.04673 = 0.04277 0.00725 0.01144 -0.00103 AFIX 13 H8 2 0.302887 0.264439 0.577111 11.00000 -1.20000 AFIX 0 C9 1 0.203452 0.378020 0.476858 11.00000 0.04025 0.04183 = 0.03783 0.00330 0.01145 -0.00104 AFIX 13 H9 2 0.135861 0.368114 0.424347 11.00000 -1.20000 AFIX 0 C10 1 0.199449 0.493396 0.531764 11.00000 0.04037 0.04253 = 0.04025 0.00388 0.01303 -0.00071 AFIX 13 H10 2 0.164845 0.559422 0.488838 11.00000 -1.20000 AFIX 0 C11 1 0.134560 0.464627 0.581661 11.00000 0.03954 0.05662 = 0.04003 -0.00363 0.01192 -0.00396 C12 1 0.122476 0.348530 0.606063 11.00000 0.04228 0.06940 = 0.04194 0.00483 0.01399 -0.00799 AFIX 43 H12 2 0.082469 0.336377 0.638223 11.00000 -1.20000 AFIX 0 C13 1 0.289172 0.400207 0.444759 11.00000 0.04815 0.04514 = 0.04747 0.00143 0.01991 0.00160 C14 1 0.273128 0.494984 0.374672 11.00000 0.06353 0.04346 = 0.04841 0.00028 0.03077 0.00174 C15 1 0.175282 0.540522 0.317807 11.00000 0.06890 0.06316 = 0.05087 0.00885 0.02917 0.00768 AFIX 43 H15 2 0.115455 0.510788 0.321546 11.00000 -1.20000 AFIX 0 C16 1 0.166918 0.630747 0.255205 11.00000 0.09891 0.06901 = 0.05823 0.01791 0.03519 0.02077 AFIX 43 H16 2 0.101317 0.660996 0.216773 11.00000 -1.20000 AFIX 0 C17 1 0.255508 0.675545 0.249886 11.00000 0.12639 0.06379 = 0.07790 0.02033 0.06274 0.00576 AFIX 43 H17 2 0.249617 0.736386 0.208249 11.00000 -1.20000 AFIX 0 C18 1 0.352642 0.630337 0.306118 11.00000 0.10881 0.07097 = 0.09638 0.01289 0.06905 -0.00840 AFIX 43 H18 2 0.412270 0.660367 0.302180 11.00000 -1.20000 AFIX 0 C19 1 0.361777 0.540684 0.368246 11.00000 0.07273 0.06137 = 0.07288 0.00555 0.04326 -0.00034 AFIX 43 H19 2 0.427635 0.510529 0.406129 11.00000 -1.20000 AFIX 0 C20 1 0.307153 0.536762 0.595632 11.00000 0.04215 0.04496 = 0.04475 0.00278 0.01429 -0.00094 AFIX 43 H20 2 0.348195 0.485916 0.643152 11.00000 -1.20000 AFIX 0 C21 1 0.345982 0.643225 0.587403 11.00000 0.04517 0.04542 = 0.04787 -0.00048 0.01883 -0.00119 AFIX 43 H21 2 0.302168 0.692720 0.540163 11.00000 -1.20000 AFIX 0 C22 1 0.520201 0.665670 0.731921 11.00000 0.05180 0.05677 = 0.04715 -0.00984 0.01677 -0.00857 C23 1 0.449426 0.692520 0.643568 11.00000 0.04890 0.04045 = 0.05235 -0.00703 0.02441 -0.00364 C24 1 0.500085 0.780961 0.616664 11.00000 0.05724 0.04193 = 0.06268 -0.00676 0.03149 -0.00684 C25 1 0.513488 0.580218 0.799670 11.00000 0.07761 0.08690 = 0.05508 0.00657 0.01945 -0.01795 AFIX 137 H25A 2 0.525058 0.498123 0.785179 11.00000 -1.50000 H25B 2 0.445237 0.585952 0.799040 11.00000 -1.50000 H25C 2 0.565822 0.601252 0.858656 11.00000 -1.50000 AFIX 0 C26 1 0.467306 0.846850 0.529977 11.00000 0.07371 0.05461 = 0.08053 0.01116 0.03681 -0.00399 AFIX 137 H26A 2 0.411869 0.902823 0.522846 11.00000 -1.50000 H26B 2 0.442904 0.789156 0.481071 11.00000 -1.50000 H26C 2 0.525852 0.891371 0.529702 11.00000 -1.50000 AFIX 0 PART 2 O4A 4 0.603304 0.718726 0.762442 -21.00000 0.06396 0.05525 = 0.05469 0.00046 0.02599 -0.01649 N3A 3 0.598193 0.798352 0.695685 -21.00000 0.05137 0.06101 = 0.04581 -0.00189 0.01280 -0.02316 O2A 4 0.097850 0.640576 0.597370 -31.00000 0.06380 0.05116 = 0.07316 -0.00678 0.02582 0.00040 O1A 4 0.034265 0.491318 0.659622 -31.00000 0.05935 0.09567 = 0.06244 0.00350 0.03350 0.01040 N2A 3 0.070797 0.540814 0.612058 -31.00000 0.03633 0.06921 = 0.04363 -0.00876 0.01115 -0.00556 HKLF 4 REM WLL148 in P21/c #14 REM R1 = 0.0445 for 3204 Fo > 4sig(Fo) and 0.0575 for all 4065 data REM 317 parameters refined using 30 restraints END WGHT 0.0652 0.2535 REM Highest difference peak 0.253, deepest hole -0.198, 1-sigma level 0.040 Q1 1 -0.0411 0.7666 0.2413 11.00000 0.05 0.25 Q2 1 0.3835 0.8407 0.4854 11.00000 0.05 0.16 Q3 1 0.5968 0.5430 0.8378 11.00000 0.05 0.15 Q4 1 0.2079 0.3156 0.5029 11.00000 0.05 0.13 Q5 1 0.2002 0.4388 0.5049 11.00000 0.05 0.12 Q6 1 0.5185 0.8217 0.4991 11.00000 0.05 0.12 Q7 1 0.2290 0.3820 0.4499 11.00000 0.05 0.12 Q8 1 0.2728 0.4410 0.3995 11.00000 0.05 0.12 Q9 1 0.2579 0.5274 0.5603 11.00000 0.05 0.12 Q10 1 0.5015 0.6556 0.8499 11.00000 0.05 0.12 Q11 1 0.4903 0.6377 0.6742 11.00000 0.05 0.12 Q12 1 0.3135 0.6071 0.6217 11.00000 0.05 0.11 Q13 1 -0.0133 0.6114 0.6479 11.00000 0.05 0.11 Q14 1 0.1532 0.1119 0.4862 11.00000 0.05 0.11 Q15 1 0.3694 0.4590 0.6172 11.00000 0.05 0.11 Q16 1 0.7096 0.9093 0.7682 11.00000 0.05 0.11 Q17 1 0.6678 0.6847 0.7689 11.00000 0.05 0.11 Q18 1 0.1169 0.4765 0.2971 11.00000 0.05 0.11 Q19 1 0.4282 0.6459 0.2102 11.00000 0.05 0.11 Q20 1 0.3459 0.5595 0.5714 11.00000 0.05 0.11 ; _shelx_res_checksum 44121 _shelx_hkl_file ; 0 0 -2 352473. 1792.04 6 0 0 -3 171.136 65.4328 6 0 0 -4 15459.4 533.316 6 0 0 -4 15876.1 623.016 2 0 0 -5 49.0294 92.1891 3 0 0 5-54.5968 32.6658 7 0 0 -5 32.8940 79.0329 2 0 0 -6 75526.7 1712.91 2 0 0 -6 78487.9 1480.67 6 0 0 -7-11.7554 88.2244 6 0 0 -7-24.9717 125.210 3 0 0 -7 51.9045 110.240 2 0 0 -8 41492.3 1563.59 3 0 0 -8 43089.3 1552.67 2 0 0 -9 299.423 165.731 2 0 0 -9 62.8718 124.677 3 0 0 -10 12642.2 986.779 2 0 0 -10 11243.8 947.885 3 0 0 -11 10.8563 91.7000 3 0 0 -12 6567.48 306.656 11 0 0 -13 26.9837 50.4955 11 0 0 -14 10968.2 403.394 11 0 0 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1607.18 159.890 11 3 -3 -15-22.3870 63.1985 11 3 -3 -14 6.68643 65.2804 11 3 -3 -13 1159.29 135.866 11 3 -3 -12 2101.86 171.855 11 3 3 -11 2146.12 410.796 3 3 -3 -11 1511.83 369.487 6 3 3 -10-5.57438 114.515 3 3 -3 -10-54.6311 142.220 6 3 -3 -9 20125.2 1175.96 6 3 -3 -8 4986.84 555.604 6 3 -3 -8 6067.64 589.283 1 3 -3 -7 13186.8 817.077 1 3 -3 -7 14280.2 870.441 5 3 -3 -7 12074.1 817.374 6 3 -3 -6 881.014 239.887 5 3 3 -6 1001.77 197.404 8 3 -3 -6 929.285 217.728 1 3 -3 -6 882.350 233.896 6 3 -3 -5 10824.4 682.415 5 3 -3 -5 12015.7 701.306 1 3 -3 -5 10914.7 685.383 6 3 -3 -4 3867.22 385.381 1 3 -3 -4 3685.96 381.252 6 3 -3 -3 107826. 1863.71 6 3 -3 -3 110418. 1928.17 1 3 -3 -2 121809. 1842.63 6 3 -3 -2 120107. 2021.76 1 3 3 -1 73799.7 1615.86 7 3 -3 -1 72608.5 1319.33 6 3 -3 -1 70806.4 1564.84 1 -3 -3 0 116844. 2019.83 4 3 3 0 108624. 1993.99 7 -3 -3 0 114653. 1880.13 2 3 -3 0 111830. 1473.86 6 3 -3 0 112746. 2014.96 1 -3 -3 -1 870.025 208.848 4 -3 3 -1 1071.53 123.151 2 3 3 1 1077.75 234.430 7 -3 -3 -1 1056.65 208.580 2 3 -3 1 778.497 191.775 1 -3 -3 -2 39595.7 1313.67 4 3 3 2 38856.5 1266.90 7 -3 -3 -2 38647.2 1251.54 2 3 3 3 30547.7 1154.90 7 -3 -3 -3 29576.8 1182.49 4 -3 -3 -3 28887.9 1161.26 2 -3 -3 -4 1867.67 344.204 2 3 3 4 1372.87 273.195 7 -3 -3 -4 1225.94 261.665 4 3 3 5 6429.52 577.699 7 -3 -3 -5 5667.10 579.081 4 -3 -3 -5 5924.23 616.505 2 -3 -3 -6 2189.71 403.705 2 -3 -3 -7 4033.33 577.340 2 -3 3 -7 4558.17 618.268 3 -3 -3 -8-291.475 193.573 2 -3 3 -8-55.5871 166.605 3 3 -3 9 36.4739 42.5005 16 -3 -3 -9 63.2174 48.8183 11 -3 3 -9 17.0132 46.8236 14 -3 3 -10 96.6943 61.6766 14 3 -3 10 110.759 51.7888 16 -3 -3 -10 112.161 57.4426 11 -3 -3 -11 7822.13 342.777 11 -3 -3 -12 1129.17 134.374 11 -3 -3 -13 563.463 106.366 11 -3 -3 -14 361.678 69.3396 11 -3 -3 -15 232.130 55.5801 11 3 4 -18 1661.58 119.292 10 3 -4 -17 474.643 94.1628 11 3 -4 -16 187.714 90.7599 11 3 -4 -15 987.092 133.385 11 3 -4 -14 1693.25 166.620 11 -3 -4 13 1455.61 150.439 16 3 -4 -13 1459.48 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465.962 98.4008 16 -6 3 -8 372.571 89.1913 14 6 -3 9 11148.6 406.010 16 -6 3 -9 10679.7 410.760 14 -6 -3 -9 10747.3 393.434 11 6 -3 10 9360.05 352.101 16 -6 3 -10 8771.28 363.747 14 -6 -3 -10 8557.58 344.138 11 -6 3 -11 549.420 81.8466 11 -6 -3 -11 458.136 92.8068 11 -6 3 -12 1854.10 130.737 11 -6 -3 -12 1958.38 145.685 11 -6 -3 -13-79.4365 43.8580 11 6 4 -18 49.8317 43.5074 10 6 4 -17 291.189 77.3801 10 6 4 -16-8.78438 56.2464 10 6 4 -15 65.2279 61.2609 10 6 -4 -15 323.142 100.620 11 6 -4 -14 5980.09 311.044 11 -6 -4 14 5738.28 284.239 16 6 -4 -13 6737.61 319.852 11 -6 -4 13 6260.80 303.697 16 6 -4 -12 19472.5 533.264 11 -6 -4 12 18553.9 520.275 16 6 -4 -11 4471.87 252.473 11 -6 -4 11 4238.41 246.108 16 6 -4 -10 34784.0 1781.09 6 6 -4 -10 36992.1 1824.09 1 6 -4 -9 8449.07 816.799 5 6 -4 -9 7278.26 781.526 1 6 -4 -9 6842.60 756.782 6 6 -4 -8 12317.8 941.865 5 6 -4 -8 12977.2 1005.55 1 6 -4 -8 12310.4 968.472 6 6 -4 -7 10172.2 828.740 5 6 -4 -7 10044.5 852.817 1 6 4 -7 11081.7 937.319 8 6 -4 -7 9107.11 800.306 6 6 -4 -6 8385.27 757.002 1 6 4 -6 8704.11 837.953 8 6 -4 -6 8219.37 722.170 6 6 -4 -6 8573.41 752.215 5 6 -4 -5 6656.70 660.688 1 6 -4 -5 6782.48 618.008 6 6 -4 -4 9331.58 773.797 1 6 -4 -4 10266.8 717.013 6 6 -4 -3 12077.5 858.909 1 -6 -4 2 27138.2 1253.59 2 6 -4 -2 26627.4 1284.26 1 -6 -4 1 30335.9 1353.55 2 6 -4 -1 30248.3 1376.14 1 6 -4 0 1592.55 332.965 1 -6 -4 0 1477.34 335.801 4 -6 -4 0 1925.30 349.399 2 6 -4 1 1029.02 287.289 1 -6 -4 -1 1150.31 300.513 4 -6 -4 -1 659.921 214.896 2 6 -4 2 325.105 175.804 1 -6 -4 -2 92.5897 107.619 4 -6 -4 -2 112.442 148.569 2 -6 -4 -3 4394.94 598.505 4 6 -4 3 4010.16 571.898 1 -6 -4 -3 5964.06 709.130 2 -6 -4 -4 16178.5 1200.19 4 -6 4 -4 16072.9 1135.09 3 6 -4 4 15141.8 1118.99 1 -6 -4 -4 18009.1 1268.65 2 -6 4 -5 601.958 99.5812 14 -6 4 -6 2880.12 209.945 14 6 -4 7 2117.76 182.757 16 -6 -4 -7 2016.66 170.610 11 -6 4 -7 1845.20 171.293 14 6 -4 8 10848.1 411.994 16 -6 4 -8 11376.2 419.644 14 -6 -4 -8 11758.5 406.947 11 6 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156.856 16 8 5 -13 1889.12 167.390 10 -8 -5 13 1907.99 168.926 16 8 5 -12 3534.52 226.947 10 -8 -5 12 3138.45 221.110 16 -8 -5 11 804.572 116.075 16 8 5 -11 1135.46 131.055 10 -8 -5 10 1492.77 159.615 16 -8 -5 9 3148.97 218.770 16 -8 -5 8 14837.0 458.482 16 8 -5 -7 1021.38 282.537 5 8 5 -7 1411.69 393.957 8 -8 -5 7 1704.58 157.068 16 8 -5 -6 5346.03 688.628 5 8 5 -6 6163.79 848.342 8 8 -5 -5 43.4667 127.570 1 8 5 -5-11.3321 157.055 8 -8 -5 5 59.7453 143.856 2 -8 -5 4 835.679 289.115 4 8 -5 -4 1520.79 380.749 1 8 5 -4 1473.90 415.325 8 -8 -5 4 632.358 242.387 2 -8 -5 3 893.272 288.655 4 -8 -5 3 253.210 160.186 2 8 -5 -3 944.841 310.086 1 -8 -5 2 307.296 170.255 4 -8 -5 2 768.629 278.771 2 8 -5 -2 653.090 252.267 1 -8 -5 1 251.866 78.0338 15 -8 -5 1-97.3365 165.767 4 -8 -5 1 164.060 176.095 2 -8 -5 0 18.4062 60.5385 15 8 -5 0 49.5894 45.5567 12 -8 -5 -1 278.639 80.3705 15 -8 5 -1 186.427 59.9832 14 8 -5 1 275.777 80.7106 12 -8 -5 -2 495.994 98.5802 15 -8 5 -2 493.893 92.3007 14 8 -5 2 426.971 90.2213 12 -8 -5 -3 35.1571 50.6121 15 -8 5 -3 20.0283 47.0077 14 8 -5 3-6.52739 53.2605 12 -8 -5 -4 2779.75 199.088 15 -8 5 -4 2746.93 205.980 14 8 -5 4 2422.87 194.180 12 -8 5 -5 4.70904 55.1940 14 8 -5 6 926.428 127.949 16 -8 5 -6 947.464 124.828 14 8 -5 7 52.7650 60.1620 16 -8 5 -7 98.5651 61.9587 14 8 -5 8 1206.75 129.805 16 -8 5 -8 1079.64 121.555 14 8 -5 9 1039.01 106.387 16 8 -5 10 26.5358 29.3302 16 8 6 -17 18.8689 29.9695 10 8 6 -16 704.047 85.3264 10 -8 -6 16 649.758 81.0395 16 -8 -6 15 488.346 88.9092 16 8 6 -15 494.059 80.8268 10 -8 -6 14 1204.87 133.761 16 8 6 -14 1259.23 125.868 10 -8 -6 13 159.838 65.7591 16 -8 -6 12 388.049 90.5985 16 -8 -6 11 1464.36 156.462 16 -8 -6 10 1055.33 135.691 16 -8 -6 9 1809.61 175.256 16 -8 -6 8 1666.56 164.399 16 -8 -6 7 10438.1 383.173 15 -8 -6 7 10765.4 396.269 16 -8 -6 6 464.392 93.5711 16 -8 -6 6 494.175 91.1943 15 -8 -6 5 1983.31 172.224 15 -8 -6 5 2074.47 171.704 16 -8 -6 4 2482.23 193.601 15 -8 -6 4 2508.98 186.959 16 -8 -6 3 5948.27 299.721 15 -8 -6 3 5821.26 273.355 16 -8 -6 2 3168.30 218.221 15 8 -6 -2 3568.77 234.320 12 -8 -6 1 9435.35 376.466 15 8 -6 -1 8328.20 357.514 12 -8 -6 0-65.9738 61.0569 15 8 -6 0 20.6021 53.7338 12 -8 -6 -1 156.092 68.2053 15 8 -6 1 27.1847 50.7497 12 -8 -6 -2 2972.96 210.566 15 8 -6 2 2629.35 208.262 12 -8 -6 -3 5347.77 278.391 15 -8 6 -3 4951.85 265.566 14 8 -6 3 4694.00 275.223 12 8 -6 4-13.7741 61.3491 16 -8 -6 -4 68.1884 52.6816 15 -8 6 -4-39.2563 50.6558 14 8 -6 5 2414.36 197.497 16 -8 6 -5 2337.28 181.294 14 8 -6 6 2031.79 178.277 16 -8 6 -6 1925.21 159.064 14 8 -6 7 136.009 73.0204 16 -8 6 -7 128.745 51.1589 14 8 -6 8 42.5395 52.8993 16 8 -6 9 715.630 86.3928 16 -8 -7 16 297.506 54.6130 16 -8 -7 15 284.657 66.8045 16 -8 -7 14 192.099 61.1692 16 -8 -7 13 158.713 65.3693 16 -8 -7 12 143.823 62.4555 16 -8 -7 11 593.878 111.323 16 -8 -7 10 2285.09 189.439 16 -8 -7 9 8872.36 369.666 16 -8 -7 8 2856.17 206.364 15 -8 -7 8 2807.51 213.446 16 -8 -7 7 7451.89 333.280 15 -8 -7 7 7948.38 344.854 16 -8 -7 6 12208.0 429.808 15 -8 -7 6 13188.2 439.356 16 -8 -7 5 1001.77 131.722 15 -8 -7 5 1020.62 123.256 16 -8 -7 4 2117.55 183.011 15 -8 -7 4 2550.35 189.818 16 8 -7 -4 2611.14 206.182 12 -8 -7 3 7079.55 332.792 15 8 -7 -3 7558.59 343.321 12 -8 -7 2-50.8377 60.5705 15 8 -7 -2 30.4749 62.2597 12 -8 -7 1 1456.63 155.932 15 8 -7 -1 1443.04 160.454 12 -8 -7 0 900.377 125.704 15 8 -7 0 1020.05 138.372 12 8 -7 1 7303.98 333.144 16 -8 -7 -1 7208.07 330.778 15 8 -7 1 6692.74 330.681 12 8 -7 2 7846.60 345.150 16 -8 -7 -2 7758.26 334.701 15 8 -7 2 6739.96 331.697 12 8 -7 3-17.0631 68.6044 16 -8 -7 -3 27.4795 47.0465 15 8 -7 4-60.3329 65.7638 16 8 -7 5 1131.52 134.335 16 8 -7 6 1798.25 159.664 16 8 -7 7 38.5062 48.7038 16 8 -7 8 1634.14 126.158 16 -8 -8 15 212.387 53.5175 16 -8 -8 14 489.082 79.2072 16 -8 -8 13 10.8879 62.6243 16 -8 -8 12 891.687 119.159 16 -8 -8 11 2120.58 179.171 16 -8 -8 10 1269.67 147.223 16 -8 -8 9 1766.49 163.680 16 -8 -8 8 3251.64 217.901 15 -8 -8 8 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16.6318 49.0028 16 -9 -6 16 396.503 67.0790 16 9 6 -16 529.250 71.0708 10 9 6 -15 2247.95 148.087 10 -9 -6 15 1991.27 153.387 16 -9 -6 14 160.898 67.1084 16 -9 -6 13 709.605 107.593 16 -9 -6 12 2964.77 215.792 16 -9 -6 11 15676.5 484.728 16 -9 -6 10 64.4793 62.5309 16 -9 -6 9 1531.28 161.552 16 -9 -6 8 3863.07 243.949 16 -9 -6 7 5217.39 275.618 15 -9 -6 7 5176.42 278.984 16 -9 -6 6 14564.3 461.532 15 -9 -6 6 15160.1 466.655 16 -9 -6 5 7671.90 338.025 15 -9 -6 5 7874.92 335.408 16 -9 -6 4 2680.11 206.676 15 -9 -6 4 2798.31 200.975 16 -9 -6 3 1934.43 178.563 15 -9 -6 3 1973.17 167.918 16 -9 -6 2 1203.44 143.274 15 9 -6 -2 1432.56 156.106 12 -9 -6 1 7331.41 335.840 15 9 -6 -1 6472.38 319.558 12 -9 -6 0 6625.14 318.424 15 -9 6 0 5960.12 290.097 14 9 -6 0 6132.26 311.505 12 -9 -6 -1 433.385 94.8929 15 -9 6 -1 511.855 97.1332 14 9 -6 1 309.091 81.0800 12 -9 -6 -2-11.4290 49.2828 15 -9 6 -2-10.5612 43.2666 14 9 -6 2-8.47952 60.2142 12 -9 -6 -3 1325.85 140.988 15 -9 6 -3 1420.72 147.261 14 9 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5 192.268 78.3551 15 10 -7 -5 259.283 84.3550 12 -10 -7 4 4214.89 254.745 15 10 -7 -4 4773.72 275.448 12 -10 -7 4 4577.44 247.225 16 -10 -7 3 33.3022 57.0507 15 10 -7 -3 148.563 68.3129 12 -10 -7 2 322.771 88.0176 15 10 -7 -2 421.711 100.411 12 -10 -7 1 550.902 100.308 15 10 -7 -1 505.097 96.0794 12 10 -7 0 67.7449 52.7804 16 -10 -7 0 158.660 68.5973 15 10 -7 0 244.158 82.0040 12 10 -7 1 18.0437 52.3913 16 -10 -7 -1 11.6755 50.3450 15 10 -7 1-35.7724 59.9074 12 10 -7 2 13.7916 51.2534 16 -10 -7 -2-12.2076 42.8036 15 10 -7 3 1573.62 145.663 16 -10 -7 -3 1704.54 135.926 15 10 -7 4 261.973 68.4580 16 10 -7 5 130.119 52.5318 16 -10 -8 14 366.399 62.4426 16 -10 -8 13 3.51205 40.0601 16 -10 -8 12-58.1454 47.8193 16 -10 -8 11 795.667 102.427 16 -10 -8 10 815.599 113.040 16 -10 -8 9 872.437 116.225 16 -10 -8 8 5124.46 254.748 15 10 -8 -8 5027.02 255.677 12 -10 -8 8 4862.50 253.269 16 -10 -8 7 3471.89 218.292 15 10 -8 -7 4170.93 240.593 12 -10 -8 7 3671.58 219.952 16 -10 -8 6 3083.38 209.443 15 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78.9470 54.3295 14 -12 4 -2 4930.29 257.419 14 -12 4 -3 44.4359 49.1681 14 12 -4 4 1963.39 149.838 16 -12 4 -4 1988.57 149.130 14 12 -4 5 42.9811 38.5364 16 -12 4 -5 112.339 48.0230 14 -12 -5 16 17.2231 24.1088 16 -12 -5 15 1171.49 105.321 16 -12 -5 14-2.28793 45.5856 16 -12 -5 13 40.9728 45.4690 16 -12 -5 12 2292.21 177.042 16 -12 -5 11 453.008 94.0019 16 -12 5 10 13015.4 420.953 14 -12 -5 10 12819.9 425.255 16 -12 -5 9 189.638 67.0898 16 -12 5 9 195.816 81.6141 14 -12 5 8 1545.31 157.689 14 -12 -5 8 1517.94 153.298 16 -12 -5 7 546.444 95.7850 16 -12 -5 7 474.352 89.4540 15 -12 5 7 428.086 89.4185 14 -12 -5 6 532.682 103.496 16 -12 -5 6 493.563 96.2437 15 -12 5 6 514.647 93.6231 14 -12 -5 5 1138.01 134.971 16 -12 -5 5 1152.68 135.120 15 -12 5 5 1339.84 147.666 14 -12 -5 4 31.3635 48.6150 15 -12 5 4-86.2000 71.5348 14 -12 -5 3 538.406 101.431 15 -12 5 3 497.897 94.6974 14 12 -5 -3 612.802 106.572 12 -12 -5 2 869.207 126.675 15 -12 5 2 649.564 105.883 14 12 -5 -2 732.675 115.995 12 -12 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68.3664 12 -12 -7 5 219.290 65.5291 15 12 -7 -5 247.723 84.5515 12 -12 -7 4 3969.29 225.386 15 12 -7 -4 4078.33 241.408 12 -12 -7 3 207.149 68.1828 15 12 -7 -3 308.488 84.0643 12 -12 -7 2 3647.21 211.412 15 12 -7 -2 3991.03 228.195 12 12 -7 -1 254.815 70.5755 16 -12 -7 1 197.565 65.6681 15 12 -7 -1 218.625 75.4121 12 12 -7 0 61.6253 52.8645 16 -12 -7 0 74.9645 51.9419 15 12 -7 1-29.0520 45.5244 16 -12 -7 -1 45.8625 40.0849 15 12 -7 2 138.403 46.7489 16 -12 -8 11 31.5725 40.9767 16 -12 -8 10 614.367 82.7531 16 12 -8 -10 573.522 76.8483 12 -12 -8 9 101.774 45.1398 16 12 -8 -9 94.7727 47.5282 12 -12 -8 8 43.3044 41.4666 16 -12 -8 8 37.1576 39.8584 15 12 -8 -8-25.9307 41.1481 12 -12 -8 7-55.2958 44.5804 16 -12 -8 7 33.9678 38.3260 15 12 -8 -7-18.1511 45.3736 12 -12 -8 6 397.985 74.6119 15 12 -8 -6 644.388 99.7231 12 -12 -8 5 37.5260 44.2875 15 12 -8 -5 67.6389 63.6149 12 -12 -8 4 576.508 87.0972 15 12 -8 -4 437.066 82.3306 12 -12 -8 3 2854.92 172.495 15 12 -8 -3 3170.14 188.627 12 -12 -8 2 1624.75 130.806 15 12 -8 -2 1812.82 141.816 12 -12 -8 1 25.2476 46.5684 15 -12 -8 0 1041.06 91.7084 15 12 -9 -8 140.650 42.1405 12 -12 -9 7 48.8816 38.7631 15 12 -9 -7 58.7147 36.9444 12 -12 -9 6 45.0610 38.6041 15 12 -9 -6 7.78427 35.9407 12 -12 -9 5 10.5213 34.3863 15 12 -9 -5 26.8478 40.4400 12 -12 -9 4 48.6903 39.9079 15 13 0 -17 5.64047 39.2582 9 13 0 -16 67.7961 46.7411 9 13 0 -15 59.4345 64.5592 9 13 0 -14 328.026 79.3440 9 13 0 -13-33.3692 61.0277 9 13 0 -12 2838.25 201.893 9 13 0 -11 56.4762 57.2165 9 13 0 -10 1852.72 166.029 9 13 0 -9 1.06738 45.5242 9 13 0 -8-87.5140 56.3082 9 13 0 -7-28.5727 39.3161 9 -13 0 7 26.3055 59.6497 14 -13 0 6 1639.74 159.685 14 -13 0 5-2.71602 51.2247 14 -13 0 4 13748.1 452.813 14 -13 0 3 58.8149 69.2246 14 -13 0 2 3175.62 220.567 14 -13 0 1 19.9645 53.7664 14 -13 0 0 451.905 87.7714 14 -13 0 -1 36.5992 53.4137 14 -13 0 -2 62.1581 52.7907 14 -13 0 -3 24.6080 43.4466 14 -13 0 -4 761.383 84.4556 14 13 -1 -17 223.769 50.0840 9 13 1 -17 310.996 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103.085 59.2588 14 13 -4 -4 225.179 75.1162 12 -13 -4 3 590.115 105.868 15 -13 4 3 428.514 94.6133 14 13 -4 -3 227.282 71.8358 12 -13 -4 2 230.541 80.6774 15 -13 4 2 386.043 84.3739 14 13 -4 -2 327.034 78.3608 12 -13 -4 1 1730.41 157.401 15 -13 4 1 2182.34 178.433 14 13 -4 -1 1861.52 150.920 12 -13 4 0-65.8641 64.0755 14 -13 4 -1 200.906 64.3536 14 -13 4 -2 20.6721 47.0302 14 13 -4 3 459.076 72.2780 16 -13 4 -3 585.405 81.4236 14 -13 -5 15 59.7713 37.3163 16 13 5 -15 70.7269 31.8817 9 -13 5 15 72.5718 32.2343 14 13 5 -14 66.8740 38.1701 9 -13 5 14 44.3383 34.1070 14 -13 -5 13-27.5811 49.7186 16 13 5 -13-36.1678 33.9590 9 -13 5 13-2.86704 41.7113 14 -13 -5 12 147.550 54.7177 16 -13 5 12 212.780 60.8801 14 -13 -5 11 653.733 103.376 16 -13 5 11 704.312 101.138 14 -13 -5 10 580.418 100.005 16 -13 5 10 603.773 102.491 14 -13 -5 9 313.278 82.3003 16 -13 5 9 320.380 77.7454 14 -13 -5 8-8.00688 52.1434 16 -13 -5 8 43.2834 38.3747 15 -13 5 8-18.6580 49.6701 14 -13 -5 7 143.470 63.5669 16 -13 -5 7 105.454 56.8640 15 -13 5 7 196.830 67.0149 14 -13 -5 6 360.132 79.7303 15 -13 5 6 327.082 82.4445 14 -13 -5 5 3063.76 204.853 15 -13 5 5 3252.25 211.108 14 13 -5 -5 2970.26 206.916 12 -13 -5 4 713.394 108.206 15 -13 5 4 657.015 104.569 14 13 -5 -4 736.564 107.123 12 -13 -5 3 681.547 109.930 15 -13 5 3 711.481 106.177 14 13 -5 -3 617.737 103.375 12 -13 -5 2 1572.80 148.288 15 -13 5 2 1390.95 136.806 14 13 -5 -2 1455.53 141.708 12 -13 -5 1 380.667 85.9833 15 -13 5 1 369.436 86.7008 14 13 -5 -1 332.073 75.7206 12 -13 5 0 2347.17 167.114 14 13 -5 0 2219.08 150.402 12 -13 5 -1 1009.83 103.994 14 13 -5 2 1181.90 109.204 16 -13 5 -2 1210.19 105.966 14 -13 -6 14 925.530 89.9139 16 -13 -6 13 789.903 90.8453 16 -13 -6 12-16.6275 41.9461 16 -13 -6 11 1962.25 151.426 16 -13 -6 10-10.9043 52.1738 16 -13 -6 9 59.4748 51.0830 16 -13 6 9 38.9135 35.8723 14 -13 -6 8 568.852 96.6748 16 -13 -6 8 567.751 78.7231 15 -13 6 8 581.122 87.3166 14 -13 -6 7 33.7386 53.2420 16 -13 -6 7-12.2661 50.9082 15 -13 6 7 73.3574 42.6266 14 13 -6 -7-17.4757 70.6198 12 -13 -6 6 156.479 59.2457 15 -13 6 6 339.661 75.1064 14 13 -6 -6 186.599 76.6804 12 -13 -6 5 1.16785 49.2680 15 -13 6 5 46.9160 40.5037 14 13 -6 -5-39.8419 68.0234 12 -13 -6 4-68.7359 55.8125 15 -13 6 4 49.2293 42.6562 14 13 -6 -4 20.6562 53.3807 12 -13 -6 3 346.212 79.7442 15 -13 6 3 307.839 67.0462 14 13 -6 -3 366.135 79.5541 12 -13 -6 2 2459.87 171.983 15 -13 6 2 2520.97 166.733 14 13 -6 -2 2535.55 174.597 12 -13 -6 1 24.6811 44.8092 15 -13 6 1 21.3964 40.8515 14 13 -6 -1-23.0825 46.3249 12 13 -6 0 3522.83 182.427 16 -13 6 0 3214.81 171.074 14 13 -6 1 1172.39 104.075 16 -13 6 -1 1032.37 92.8536 14 -13 -7 12-97.0104 48.5804 16 13 -7 -12-74.4793 37.7669 12 -13 -7 11 47.3336 45.0409 16 13 -7 -11-53.1822 38.2480 12 -13 -7 10 102.252 51.4360 16 13 -7 -10 122.854 48.2056 12 -13 -7 9 526.645 81.8925 16 13 -7 -9 625.283 87.5044 12 -13 -7 8 11.8453 39.9333 16 -13 -7 8 40.7264 34.4060 15 13 -7 -8 127.630 51.8166 12 -13 -7 7 146.577 52.9463 15 13 -7 -7 61.4617 50.2080 12 -13 -7 6 1040.45 111.008 15 13 -7 -6 1169.72 124.696 12 -13 -7 5 1494.14 129.659 15 13 -7 -5 1527.50 139.791 12 -13 -7 4 3144.77 184.808 15 13 -7 -4 3008.77 186.705 12 -13 -7 3 532.631 80.9210 15 13 -7 -3 527.696 85.9604 12 -13 -7 2 1021.65 104.226 15 13 -7 -2 900.457 99.4630 12 13 -7 -1 1336.34 98.2998 16 -13 -7 1 1461.59 115.236 15 13 -8 -9 269.270 50.8301 12 -13 -8 8 84.1529 35.6022 15 13 -8 -8 56.2703 45.3625 12 -13 -8 7 199.176 45.7365 15 13 -8 -7 323.008 64.6266 12 -13 -8 6 41.3682 38.4011 15 13 -8 -6 34.7472 42.3475 12 -13 -8 5 755.193 83.2958 15 13 -8 -5 783.380 94.5282 12 -13 -8 4-8.11865 36.6452 15 13 -8 -4 28.1942 42.5867 12 14 0 -16 13.0215 42.8226 9 14 0 -15 50.1884 45.5900 9 14 0 -14 358.294 81.5790 9 14 0 -13-31.3363 50.4634 9 14 0 -12 1690.84 151.357 9 14 0 -11 23.4808 54.0525 9 14 0 -10 4402.76 244.032 9 -14 0 10 4597.76 255.440 14 14 0 -9-68.4503 49.2903 9 -14 0 9-20.7164 63.1168 14 -14 0 8 41.1888 51.7558 14 -14 0 7-32.8599 54.5048 14 -14 0 6 1470.06 148.011 14 -14 0 5-45.0226 57.4729 14 -14 0 4 501.338 94.9240 14 -14 0 3 74.1967 55.2931 14 -14 0 2 13789.9 429.358 14 -14 0 1 34.2778 54.0980 14 -14 0 0 1667.08 141.387 14 -14 0 -1 51.6184 47.4207 14 -14 0 -2 738.336 82.9202 14 14 -1 -16 849.544 91.5548 9 14 1 -16 635.955 81.6340 9 14 -1 -15 150.594 56.8216 9 14 1 -15 53.9915 48.6511 9 14 -1 -14-7.92339 46.2185 9 14 1 -14-25.4261 44.5631 9 14 -1 -13 1644.66 149.467 9 14 1 -13 1364.31 135.304 9 14 -1 -12 83.1899 63.3978 9 14 1 -12 31.9462 50.3841 9 14 -1 -11 418.784 94.9023 9 14 1 -11 324.889 74.0269 9 14 -1 -10 129.823 65.1944 9 14 1 -10 52.8851 41.4168 9 -14 -1 10 145.218 68.5654 14 -14 1 10 223.095 87.5993 14 14 1 -9 362.771 79.4047 9 -14 -1 9 388.251 78.3733 14 -14 1 9 403.773 86.8830 14 -14 -1 8 1121.93 132.952 14 -14 1 8 990.774 127.553 14 -14 -1 7 4587.93 253.137 14 -14 1 7 4165.59 247.841 14 -14 -1 6-23.0598 63.0880 14 -14 1 6-56.8770 62.1211 14 -14 -1 5 1327.49 138.483 14 -14 1 5 1179.62 140.634 14 -14 -1 4 2655.21 188.905 14 -14 1 4 2379.57 189.854 14 -14 -1 3 402.888 80.8350 14 -14 1 3 478.365 101.472 14 -14 -1 2 2530.79 179.656 14 -14 1 2 2183.84 177.309 14 -14 -1 1 513.668 82.6678 14 -14 1 1 409.136 83.4789 14 -14 -1 0 549.793 78.8904 14 -14 1 0 591.408 93.5481 14 -14 1 -1 22.4612 44.9512 14 -14 1 -2 344.776 64.6555 14 14 2 -16 26.4414 36.2843 9 14 2 -15 115.419 47.2184 9 14 2 -14 123.829 55.5690 9 14 2 -13 235.777 61.6199 9 14 2 -12 915.520 107.062 9 14 2 -11 510.784 90.1775 9 -14 -2 11 579.518 96.4543 14 14 2 -10 239.945 65.5866 9 -14 -2 10 204.345 72.6438 14 -14 2 10 164.605 73.3816 14 -14 -2 9 1670.53 147.406 14 -14 2 9 1588.10 157.061 14 -14 -2 8 397.770 81.3493 14 -14 2 8 287.834 82.2347 14 -14 2 7 401.550 88.0042 14 -14 2 6 9079.65 363.899 14 -14 2 5 8216.35 344.992 14 -14 2 4 212.114 69.0971 14 -14 2 3 1110.07 138.470 14 -14 2 2 180.023 62.4534 14 -14 2 1 765.078 108.043 14 -14 2 0 485.161 88.2397 14 -14 2 -1 934.485 106.173 14 -14 2 -2 14.8469 41.5981 14 14 3 -15 128.873 47.8569 9 14 3 -14 241.984 54.1428 9 14 3 -13 655.983 89.8290 9 14 3 -12 88.5352 47.1238 9 -14 3 12 242.834 71.5326 14 14 3 -11 375.854 71.8252 9 -14 3 11 310.880 79.5568 14 -14 3 10 1539.36 150.298 14 -14 3 9 47.7221 55.9206 14 -14 3 8 125.546 71.5247 14 -14 3 7 654.275 108.337 14 -14 3 6 4024.77 242.014 14 -14 3 5 3934.21 237.808 14 -14 3 4 449.401 94.3264 14 14 -3 -4 309.365 67.2131 12 -14 3 3-4.07354 63.6134 14 14 -3 -3 126.934 51.8235 12 -14 3 2 889.349 118.285 14 -14 3 1-41.8953 58.2664 14 -14 3 0 1364.60 130.403 14 -14 3 -1 35.0454 50.7083 14 -14 3 -2 190.793 54.4637 14 14 4 -15 109.521 40.8608 9 -14 4 15 43.9683 32.0015 14 14 4 -14 49.3455 34.7326 9 -14 4 14 98.9519 49.6710 14 -14 -4 13 357.219 70.0477 16 14 4 -13 300.705 58.9534 9 -14 4 13 341.473 73.3114 14 -14 -4 12 491.815 80.8173 16 14 4 -12 408.463 68.3945 9 -14 4 12 567.437 88.1335 14 -14 4 11 1683.68 147.631 14 -14 -4 11 1473.24 137.877 16 -14 -4 10 247.448 73.9623 16 -14 4 10 156.668 54.9893 14 -14 4 9 618.608 98.4713 14 -14 4 8-107.253 60.4846 14 -14 -4 7 19.6535 42.6618 15 -14 4 7 52.3257 55.5875 14 -14 -4 6 829.125 111.923 15 -14 4 6 694.278 107.198 14 -14 -4 5 94.3640 59.3636 15 -14 4 5 56.0813 49.0768 14 14 -4 -5 77.8273 54.6981 12 -14 -4 4 42.8173 59.2696 15 -14 4 4 82.2612 51.3849 14 14 -4 -4 29.2443 45.4238 12 -14 4 3 857.898 113.842 14 14 -4 -3 843.549 104.312 12 -14 4 2 1283.29 128.933 14 14 -4 -2 1266.26 115.725 12 -14 4 1 1395.48 130.213 14 -14 4 0 1152.75 112.654 14 -14 4 -1 878.422 93.0163 14 -14 5 14 275.632 50.1592 14 -14 -5 13 452.904 72.1626 16 -14 5 13 378.331 62.4069 14 -14 -5 12 328.761 67.4353 16 -14 5 12 366.863 67.7055 14 -14 -5 11 196.856 64.1158 16 -14 5 11 179.521 55.2724 14 -14 -5 10 600.862 92.0317 16 -14 5 10 646.778 86.0163 14 -14 5 9 917.435 107.894 14 -14 -5 8 391.968 68.5414 15 -14 5 8 229.228 61.7587 14 -14 -5 7 1071.63 111.431 15 -14 5 7 936.632 112.167 14 14 -5 -7 1028.93 125.973 12 -14 -5 6 169.457 54.7308 15 -14 5 6 236.732 67.6010 14 14 -5 -6 233.395 69.5528 12 -14 -5 5 93.3314 58.6211 15 -14 5 5-28.7610 44.7972 14 14 -5 -5-17.8896 51.8946 12 -14 -5 4 133.808 61.2092 15 -14 5 4 201.471 54.8429 14 14 -5 -4 201.882 63.9285 12 -14 -5 3 116.249 49.1754 15 -14 5 3 141.018 58.5547 14 14 -5 -3 95.9583 54.5270 12 -14 5 2-58.9824 50.2447 14 14 -5 -2 14.2125 36.7251 12 -14 5 1-30.3517 47.7337 14 14 -5 0 58.3256 42.5985 16 -14 5 0 32.7730 32.1909 14 14 -6 -12 1550.41 113.971 12 -14 -6 12 1551.13 114.679 16 -14 -6 11-26.9188 39.5028 16 14 -6 -11 25.0781 43.6651 12 14 -6 -10 199.178 65.0503 12 -14 6 9 1501.05 117.652 14 14 -6 -9 1833.08 143.047 12 -14 -6 8-31.6850 37.0594 15 -14 6 8 32.1819 39.2423 14 14 -6 -8-43.3572 52.0707 12 -14 -6 7 521.122 75.3160 15 -14 6 7 389.158 67.2959 14 14 -6 -7 399.038 77.4015 12 -14 -6 6 114.990 51.0712 15 -14 6 6 65.4070 38.6012 14 14 -6 -6 78.1732 49.2573 12 -14 -6 5 21.0819 41.3103 15 -14 6 5 39.8958 39.2357 14 14 -6 -5 21.6391 51.2421 12 -14 -6 4 2040.21 141.501 15 -14 6 4 2198.98 144.130 14 14 -6 -4 2300.42 153.573 12 -14 -6 3 1812.86 131.886 15 -14 6 3 1953.39 131.432 14 14 -6 -3 2046.23 141.692 12 14 -6 -2 214.524 48.4543 16 -14 6 2 290.621 55.1135 14 14 -6 -2 359.515 63.1490 12 14 -7 -9-59.2827 40.3577 12 14 -7 -8 74.0457 42.7256 12 -14 -7 7 260.976 50.3605 15 14 -7 -7 302.613 70.0759 12 -14 -7 6 1744.16 116.927 15 14 -7 -6 1692.32 124.870 12 -14 -7 5 67.6313 40.6807 15 14 -7 -5 50.9893 42.3833 12 15 0 -15 15.4388 36.9298 9 -15 0 15 19.4255 35.9614 14 15 0 -14 71.4933 47.0379 9 -15 0 14-34.8025 49.0236 14 15 0 -13-72.1228 44.4900 9 -15 0 13-49.2626 42.2085 14 15 0 -12 1688.57 138.698 9 -15 0 12 1760.08 148.835 14 -15 0 11 25.0353 51.7841 14 -15 0 10 383.819 79.7701 14 -15 0 9 49.4034 52.0141 14 -15 0 8 169.170 55.1791 14 -15 0 7 32.7534 51.9018 14 -15 0 6 176.111 58.1426 14 -15 0 5-30.2602 49.8399 14 -15 0 4 4246.36 226.037 14 -15 0 3 71.6164 53.0205 14 -15 0 2 93.0347 43.7646 14 -15 0 1 13.1047 36.7169 14 -15 0 0-11.6797 30.6196 14 15 1 -15-13.5117 33.5177 9 -15 1 15 39.8381 44.1314 14 15 1 -14 361.447 68.3379 9 -15 -1 14 425.502 71.4931 14 15 1 -13 327.804 64.5440 9 -15 -1 13 462.534 77.4592 14 -15 1 13 501.416 82.1624 14 15 1 -12 92.2803 50.8986 9 -15 -1 12 34.1208 44.9879 14 -15 1 12 70.3942 53.3522 14 15 1 -11 147.427 54.0705 9 -15 -1 11 158.126 66.1135 14 -15 1 11 176.280 72.0436 14 -15 -1 10 1292.26 128.501 14 -15 1 10 1004.36 118.377 14 -15 -1 9 182.450 58.3968 14 -15 1 9 164.406 71.9181 14 -15 -1 8 463.458 79.7622 14 -15 1 8 436.477 86.0489 14 -15 -1 7 406.902 77.0697 14 -15 1 7 377.624 83.3133 14 -15 -1 6 4769.41 235.782 14 -15 1 6 4020.66 226.389 14 -15 -1 5 181.363 60.2400 14 -15 1 5 19.4252 49.1570 14 -15 -1 4 198.116 62.9804 14 -15 1 4 86.1814 47.4837 14 -15 -1 3 562.880 80.0005 14 -15 1 3 711.748 98.8506 14 -15 -1 2 31.0952 39.9017 14 -15 1 2 33.8404 53.5668 14 -15 1 1 21.8304 44.0043 14 -15 1 0 177.519 51.7753 14 15 2 -14 82.5315 42.7202 9 -15 -2 14 77.7726 39.0092 14 -15 2 14 38.2291 41.8005 14 15 2 -13 199.490 52.6581 9 -15 -2 13 137.717 43.2291 14 -15 2 13 237.450 66.5619 14 15 2 -12 289.677 61.6347 9 -15 -2 12 299.154 62.8422 14 -15 2 12 397.833 84.0483 14 15 2 -11 3188.12 177.256 9 -15 -2 11 3494.13 182.777 14 -15 2 11 3517.04 208.334 14 -15 2 10 285.086 82.2576 14 -15 2 9 1283.80 136.534 14 -15 2 8-13.5292 61.0333 14 -15 2 7 16.0715 59.1759 14 -15 2 6 398.507 79.0184 14 -15 2 5 285.394 76.8742 14 -15 2 4 652.559 101.105 14 -15 2 3 405.551 81.2778 14 -15 2 2 2548.64 168.182 14 -15 2 1 757.355 89.0529 14 -15 2 0 191.369 53.5772 14 15 3 -14 308.311 53.4226 9 -15 3 14 322.281 60.8538 14 15 3 -13 710.635 76.8127 9 -15 3 13 673.230 90.2281 14 15 3 -12 217.179 48.9737 9 -15 3 12 232.190 63.1975 14 -15 3 11 89.7851 55.5144 14 -15 3 10 866.520 113.173 14 -15 3 9 72.0638 50.0661 14 -15 3 8 23.5093 56.9778 14 -15 3 7-4.03981 59.1933 14 -15 3 6 47.4116 53.7172 14 15 -3 -6-76.3713 58.1706 12 -15 3 5 232.215 65.4540 14 15 -3 -5 132.198 49.0870 12 -15 3 4 90.8651 60.7862 14 -15 3 3 752.415 100.950 14 -15 3 2 694.690 91.1479 14 -15 3 1 439.906 72.4289 14 -15 4 13-84.6880 42.3688 14 -15 4 12 30.5942 44.0115 14 -15 4 11 2007.03 144.856 14 -15 4 10 116.836 47.1011 14 -15 4 9 215.188 61.2200 14 -15 4 8 25.0918 45.3386 14 -15 4 7 12.8712 44.4875 14 15 -4 -7 131.625 55.4084 12 -15 4 6 71.6197 51.4542 14 15 -4 -6 199.154 54.6170 12 -15 4 5 206.075 64.7874 14 15 -4 -5 117.739 48.3064 12 -15 4 4 158.711 59.5724 14 15 -4 -4 121.880 46.0264 12 -15 4 3 103.085 49.8014 14 -15 4 2 548.822 76.0317 14 -15 5 11 507.097 66.4739 14 -15 5 10 365.081 63.7875 14 -15 5 9 18.0058 34.5710 14 15 -5 -9-48.9232 49.0733 12 -15 5 8 366.878 68.1055 14 15 -5 -8 302.038 66.0747 12 -15 5 7 381.931 72.0440 14 15 -5 -7 425.195 73.7409 12 -15 5 6 24.9457 41.4736 14 15 -5 -6-8.34168 38.5133 12 -15 5 5 13.7199 36.6682 14 15 -5 -5-38.9904 36.1252 12 -15 5 4 249.573 55.7906 14 15 -5 -4 172.797 48.1924 12 -16 0 13-49.0917 40.6893 14 -16 0 12 1826.19 129.236 14 -16 0 11-98.8575 48.0841 14 -16 0 10 87.5078 44.9326 14 -16 0 9-0.74186 40.8978 14 -16 0 8 317.158 59.9348 14 -16 0 7 62.1949 51.3658 14 -16 0 6 115.905 53.2532 14 -16 0 5 78.6571 43.4324 14 -16 0 4 148.099 45.8077 14 -16 0 3-10.2516 25.2657 14 -16 -1 13 173.540 42.2192 14 -16 1 13 388.124 66.4713 14 -16 -1 12 221.288 48.5952 14 -16 1 12 159.768 58.8242 14 -16 -1 11 794.246 84.5504 14 -16 1 11 799.499 93.8911 14 -16 -1 10 1819.98 127.906 14 -16 1 10 1782.31 136.381 14 -16 -1 9 81.4773 46.6981 14 -16 1 9-11.1211 48.7006 14 -16 -1 8 798.819 87.4262 14 -16 1 8 590.078 85.4062 14 -16 -1 7 285.489 62.8140 14 -16 1 7 226.382 62.7826 14 -16 -1 6-54.9700 32.3204 14 -16 1 6 27.7001 40.1003 14 -16 1 5 902.129 99.3607 14 -16 1 4 174.299 52.6092 14 -16 1 3 836.056 84.3137 14 -16 2 12 2895.36 161.252 14 -16 2 11 1073.57 104.280 14 -16 2 10-64.5272 55.8320 14 -16 2 9 340.246 72.5968 14 -16 2 8 996.135 106.077 14 -16 2 7 1954.78 145.987 14 16 -2 -7 1955.61 130.365 12 -16 2 6 16.8819 42.0627 14 -16 2 5 196.228 57.4147 14 -16 2 4 2251.29 144.710 14 -16 3 11 740.625 84.0736 14 -16 3 10 16.5327 37.4709 14 -16 3 9 1.89664 43.5932 14 -16 3 8 109.911 54.3273 14 16 -3 -8 54.5251 35.7653 12 -16 3 7 1341.86 118.548 14 16 -3 -7 1260.64 105.126 12 -16 3 6 760.115 93.2844 14 16 -3 -6 602.787 71.2504 12 -16 3 5 90.5222 43.4469 14 -16 4 9 167.420 48.2814 14 16 -4 -9 231.161 56.1161 12 -16 4 8 45.8982 41.0002 14 16 -4 -8-40.5342 38.7537 12 -16 4 7 854.661 87.9081 14 16 -4 -7 911.608 85.8427 12 0 0 0 0.00 0.00 0 TITL WLL148 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 14.098624 10.934614 16.350884 90.0000 115.1910 90.0000 ZERR 3.00 0.000439 0.000259 0.000541 0.0000 0.0039 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 120.00 120.00 12.00 6.00 TREF HKLF 4 END ; _shelx_hkl_checksum 51936 _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 1.317 _oxdiff_exptl_absorpt_empirical_full_min 0.919 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 0.03814(17) 0.5433(7) 0.65287(18) 0.0699(10) Uani 0.92(2) 1 d . . P A 1 O2 O 0.0891(2) 0.6671(4) 0.5752(3) 0.0639(7) Uani 0.92(2) 1 d . U P A 1 O3 O 0.37199(10) 0.34646(13) 0.47997(10) 0.0656(4) Uani 1 1 d . . . . . O4 O 0.5909(4) 0.8099(6) 0.6757(3) 0.0577(12) Uani 0.644(16) 1 d . U P B 1 N1 N 0.16516(12) 0.25297(14) 0.58593(10) 0.0534(4) Uani 1 1 d . . . . . N2 N 0.0863(3) 0.5620(3) 0.6046(3) 0.0518(7) Uani 0.92(2) 1 d . U P A 1 N3 N 0.6083(5) 0.7399(7) 0.7532(6) 0.0555(14) Uani 0.644(16) 1 d . U P B 1 C1 C 0.1393(2) -0.0586(2) 0.4986(2) 0.0860(8) Uani 1 1 d . . . . . H1 H 0.1131 -0.1124 0.5280 0.103 Uiso 1 1 calc R . . . . C2 C 0.1548(2) -0.0963(2) 0.4252(2) 0.0944(9) Uani 1 1 d . . . . . H2 H 0.1377 -0.1760 0.4042 0.113 Uiso 1 1 calc R . . . . C3 C 0.1953(2) -0.0176(2) 0.38189(19) 0.0884(8) Uani 1 1 d . . . . . H3 H 0.2043 -0.0447 0.3317 0.106 Uiso 1 1 calc R . . . . C4 C 0.22275(18) 0.1019(2) 0.41272(15) 0.0689(5) Uani 1 1 d . . . . . H4 H 0.2515 0.1545 0.3846 0.083 Uiso 1 1 calc R . . . . C5 C 0.20604(14) 0.14003(16) 0.48610(13) 0.0550(4) Uani 1 1 d . . . . . C6 C 0.16332(15) 0.06104(19) 0.52813(15) 0.0655(5) Uani 1 1 d . . . . . C7 C 0.15004(17) 0.12451(19) 0.60367(15) 0.0681(6) Uani 1 1 d . . . . . H7A H 0.0807 0.1109 0.6008 0.082 Uiso 1 1 calc R . . . . H7B H 0.2024 0.0981 0.6621 0.082 Uiso 1 1 calc R . . . . C8 C 0.22872(12) 0.26225(15) 0.53434(11) 0.0459(4) Uani 1 1 d . . . . . H8 H 0.3029 0.2644 0.5771 0.055 Uiso 1 1 calc R . . . . C9 C 0.20345(12) 0.37802(14) 0.47686(11) 0.0418(3) Uani 1 1 d . . . . . H9 H 0.1359 0.3681 0.4243 0.050 Uiso 1 1 calc R . . . . C10 C 0.19945(12) 0.49340(14) 0.53176(11) 0.0425(3) Uani 1 1 d . . . . . H10 H 0.1648 0.5594 0.4888 0.051 Uiso 1 1 calc R . . . . C11 C 0.13456(12) 0.46463(16) 0.58166(11) 0.0471(4) Uani 1 1 d D . . . . C12 C 0.12248(13) 0.34853(18) 0.60606(12) 0.0526(4) Uani 1 1 d . . . . . H12 H 0.0825 0.3364 0.6382 0.063 Uiso 1 1 calc R . . . . C13 C 0.28917(13) 0.40021(15) 0.44476(12) 0.0471(4) Uani 1 1 d . . . . . C14 C 0.27313(14) 0.49498(15) 0.37467(12) 0.0494(4) Uani 1 1 d . . . . . C15 C 0.17528(16) 0.54052(19) 0.31781(13) 0.0597(5) Uani 1 1 d . . . . . H15 H 0.1155 0.5108 0.3215 0.072 Uiso 1 1 calc R . . . . C16 C 0.1669(2) 0.6307(2) 0.25521(15) 0.0748(6) Uani 1 1 d . . . . . H16 H 0.1013 0.6610 0.2168 0.090 Uiso 1 1 calc R . . . . C17 C 0.2555(2) 0.6755(2) 0.24989(18) 0.0827(7) Uani 1 1 d . . . . . H17 H 0.2496 0.7364 0.2082 0.099 Uiso 1 1 calc R . . . . C18 C 0.3526(2) 0.6303(2) 0.3061(2) 0.0833(7) Uani 1 1 d . . . . . H18 H 0.4123 0.6604 0.3022 0.100 Uiso 1 1 calc R . . . . C19 C 0.36178(18) 0.54068(19) 0.36825(16) 0.0647(5) Uani 1 1 d . . . . . H19 H 0.4276 0.5105 0.4061 0.078 Uiso 1 1 calc R . . . . C20 C 0.30715(12) 0.53676(15) 0.59563(11) 0.0454(4) Uani 1 1 d . . . . . H20 H 0.3482 0.4859 0.6432 0.054 Uiso 1 1 calc R . . . . C21 C 0.34598(13) 0.64322(15) 0.58740(12) 0.0465(4) Uani 1 1 d . . . . . H21 H 0.3022 0.6927 0.5402 0.056 Uiso 1 1 calc R . . . . C22 C 0.52020(14) 0.66567(17) 0.73192(12) 0.0534(4) Uani 1 1 d . . . . . C23 C 0.44943(13) 0.69252(15) 0.64357(12) 0.0462(4) Uani 1 1 d . . . . . C24 C 0.50008(14) 0.78096(16) 0.61666(13) 0.0519(4) Uani 1 1 d D . . . . C25 C 0.51349(19) 0.5802(2) 0.79967(15) 0.0762(6) Uani 1 1 d . . . . . H25A H 0.5251 0.4981 0.7852 0.114 Uiso 1 1 calc GR . . . . H25B H 0.4452 0.5860 0.7990 0.114 Uiso 1 1 calc GR . . . . H25C H 0.5658 0.6013 0.8587 0.114 Uiso 1 1 calc GR . . . . C26 C 0.46731(17) 0.8468(2) 0.52998(16) 0.0682(5) Uani 1 1 d . . . . . H26A H 0.4119 0.9028 0.5228 0.102 Uiso 1 1 calc GR . . . . H26B H 0.4429 0.7892 0.4811 0.102 Uiso 1 1 calc GR . . . . H26C H 0.5259 0.8914 0.5297 0.102 Uiso 1 1 calc GR . . . . O4A O 0.6033(10) 0.7187(10) 0.7624(11) 0.0577(12) Uani 0.356(16) 1 d D . P B 2 N3A N 0.5982(8) 0.7984(16) 0.6957(10) 0.0555(14) Uani 0.356(16) 1 d D . P B 2 O2A O 0.098(3) 0.641(4) 0.597(4) 0.0639(7) Uani 0.08(2) 1 d D . P A 2 O1A O 0.034(2) 0.491(6) 0.660(2) 0.0699(10) Uani 0.08(2) 1 d . . P A 2 N2A N 0.071(3) 0.541(4) 0.612(3) 0.0518(7) Uani 0.08(2) 1 d D . P A 2 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 0.0594(8) 0.096(3) 0.0624(9) 0.0035(13) 0.0335(7) 0.0104(12) O2 0.0638(10) 0.0512(15) 0.0732(18) -0.0068(11) 0.0258(11) 0.0004(10) O3 0.0545(7) 0.0670(9) 0.0800(9) 0.0201(7) 0.0332(7) 0.0154(6) O4 0.0640(16) 0.0553(17) 0.055(2) 0.0005(18) 0.0260(16) -0.0165(12) N1 0.0516(8) 0.0543(9) 0.0500(8) 0.0119(7) 0.0176(6) -0.0070(7) N2 0.0363(12) 0.0692(16) 0.0436(10) -0.0088(12) 0.0112(8) -0.0056(11) N3 0.0514(17) 0.061(3) 0.046(2) -0.002(2) 0.0128(13) -0.0232(16) C1 0.0766(14) 0.0509(12) 0.0999(19) 0.0092(13) 0.0081(13) -0.0139(10) C2 0.0858(17) 0.0516(13) 0.107(2) -0.0108(14) 0.0039(15) -0.0053(11) C3 0.0938(17) 0.0641(14) 0.0802(16) -0.0144(12) 0.0110(13) 0.0103(13) C4 0.0746(13) 0.0551(11) 0.0635(12) -0.0007(9) 0.0165(10) 0.0082(9) C5 0.0502(9) 0.0435(9) 0.0551(10) 0.0059(8) 0.0067(8) 0.0015(7) C6 0.0565(10) 0.0501(10) 0.0696(12) 0.0108(9) 0.0073(9) -0.0071(8) C7 0.0649(12) 0.0608(12) 0.0710(13) 0.0198(10) 0.0216(10) -0.0130(9) C8 0.0413(8) 0.0467(9) 0.0428(8) 0.0073(7) 0.0114(6) -0.0010(6) C9 0.0403(7) 0.0418(8) 0.0378(7) 0.0033(6) 0.0115(6) -0.0010(6) C10 0.0404(7) 0.0425(8) 0.0402(8) 0.0039(6) 0.0130(6) -0.0007(6) C11 0.0395(8) 0.0566(10) 0.0400(8) -0.0036(7) 0.0119(6) -0.0040(7) C12 0.0423(8) 0.0694(12) 0.0419(9) 0.0048(8) 0.0140(7) -0.0080(8) C13 0.0482(9) 0.0451(9) 0.0475(9) 0.0014(7) 0.0199(7) 0.0016(7) C14 0.0635(10) 0.0435(8) 0.0484(9) 0.0003(7) 0.0308(8) 0.0017(7) C15 0.0689(11) 0.0632(11) 0.0509(10) 0.0089(9) 0.0292(9) 0.0077(9) C16 0.0989(17) 0.0690(13) 0.0582(12) 0.0179(10) 0.0352(12) 0.0208(12) C17 0.126(2) 0.0638(13) 0.0779(15) 0.0203(12) 0.0627(16) 0.0058(13) C18 0.109(2) 0.0710(14) 0.0964(18) 0.0129(13) 0.0691(17) -0.0084(13) C19 0.0727(12) 0.0614(12) 0.0729(13) 0.0056(10) 0.0433(11) -0.0003(9) C20 0.0422(8) 0.0450(9) 0.0448(8) 0.0028(7) 0.0143(7) -0.0009(6) C21 0.0452(8) 0.0454(9) 0.0479(9) -0.0005(7) 0.0188(7) -0.0012(7) C22 0.0518(10) 0.0568(10) 0.0471(9) -0.0098(8) 0.0168(8) -0.0086(8) C23 0.0489(9) 0.0405(8) 0.0523(9) -0.0070(7) 0.0244(7) -0.0036(7) C24 0.0572(10) 0.0419(9) 0.0627(11) -0.0068(8) 0.0315(9) -0.0068(7) C25 0.0776(14) 0.0869(16) 0.0551(11) 0.0066(11) 0.0195(10) -0.0179(12) C26 0.0737(13) 0.0546(11) 0.0805(14) 0.0112(10) 0.0368(11) -0.0040(9) O4A 0.0640(16) 0.0553(17) 0.055(2) 0.0005(18) 0.0260(16) -0.0165(12) N3A 0.0514(17) 0.061(3) 0.046(2) -0.002(2) 0.0128(13) -0.0232(16) O2A 0.0638(10) 0.0512(15) 0.0732(18) -0.0068(11) 0.0258(11) 0.0004(10) O1A 0.0594(8) 0.096(3) 0.0624(9) 0.0035(13) 0.0335(7) 0.0104(12) N2A 0.0363(12) 0.0692(16) 0.0436(10) -0.0088(12) 0.0112(8) -0.0056(11) 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' 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 C24 O4 N3 106.3(5) . . ? C7 N1 C8 110.74(16) . . ? C12 N1 C7 126.16(16) . . ? C12 N1 C8 122.91(15) . . ? O1 N2 C11 119.9(2) . . ? O2 N2 O1 120.3(4) . . ? O2 N2 C11 119.7(4) . . ? C22 N3 O4 107.2(6) . . ? C2 C1 H1 120.6 . . ? C2 C1 C6 118.8(3) . . ? C6 C1 H1 120.6 . . ? C1 C2 H2 119.5 . . ? C1 C2 C3 121.0(2) . . ? C3 C2 H2 119.5 . . ? C2 C3 H3 119.7 . . ? C2 C3 C4 120.6(3) . . ? C4 C3 H3 119.7 . . ? C3 C4 H4 120.9 . . ? C5 C4 C3 118.2(2) . . ? C5 C4 H4 120.9 . . ? C4 C5 C6 120.77(19) . . ? C4 C5 C8 129.93(18) . . ? C6 C5 C8 109.30(18) . . ? C1 C6 C5 120.5(2) . . ? C1 C6 C7 128.9(2) . . ? C5 C6 C7 110.64(18) . . ? N1 C7 C6 101.59(16) . . ? N1 C7 H7A 111.5 . . ? N1 C7 H7B 111.5 . . ? C6 C7 H7A 111.5 . . ? C6 C7 H7B 111.5 . . ? H7A C7 H7B 109.3 . . ? N1 C8 C5 101.09(14) . . ? N1 C8 H8 108.5 . . ? N1 C8 C9 111.75(14) . . ? C5 C8 H8 108.5 . . ? C5 C8 C9 117.97(14) . . ? C9 C8 H8 108.5 . . ? C8 C9 H9 109.4 . . ? C8 C9 C10 111.83(13) . . ? C8 C9 C13 109.38(13) . . ? C10 C9 H9 109.4 . . ? C13 C9 H9 109.4 . . ? C13 C9 C10 107.23(13) . . ? C9 C10 H10 108.2 . . ? C11 C10 C9 108.87(13) . . ? C11 C10 H10 108.2 . . ? C11 C10 C20 110.98(13) . . ? C20 C10 C9 112.32(13) . . ? C20 C10 H10 108.2 . . ? N2 C11 C10 117.9(3) . . ? C12 C11 N2 119.6(3) . . ? C12 C11 C10 122.50(16) . . ? C12 C11 N2A 105(2) . . ? N2A C11 C10 132(2) . . ? N1 C12 C11 122.61(16) . . ? N1 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? O3 C13 C9 120.19(15) . . ? O3 C13 C14 120.21(16) . . ? C14 C13 C9 119.44(14) . . ? C15 C14 C13 123.20(16) . . ? C15 C14 C19 119.32(18) . . ? C19 C14 C13 117.46(17) . . ? C14 C15 H15 120.1 . . ? C14 C15 C16 119.8(2) . . ? C16 C15 H15 120.1 . . ? C15 C16 H16 119.9 . . ? C17 C16 C15 120.2(2) . . ? C17 C16 H16 119.9 . . ? C16 C17 H17 120.0 . . ? C18 C17 C16 120.1(2) . . ? C18 C17 H17 120.0 . . ? C17 C18 H18 119.9 . . ? C17 C18 C19 120.2(2) . . ? C19 C18 H18 119.9 . . ? C14 C19 H19 119.8 . . ? C18 C19 C14 120.4(2) . . ? C18 C19 H19 119.8 . . ? C10 C20 H20 118.4 . . ? C21 C20 C10 123.18(15) . . ? C21 C20 H20 118.4 . . ? C20 C21 H21 116.2 . . ? C20 C21 C23 127.65(16) . . ? C23 C21 H21 116.2 . . ? N3 C22 C25 120.8(4) . . ? C23 C22 N3 107.7(4) . . ? C23 C22 C25 131.46(17) . . ? O4A C22 C23 117.9(8) . . ? O4A C22 C25 110.7(8) . . ? C22 C23 C21 131.20(16) . . ? C24 C23 C21 124.99(17) . . ? C24 C23 C22 103.81(16) . . ? O4 C24 C23 115.0(4) . . ? O4 C24 C26 114.1(3) . . ? C23 C24 C26 130.85(18) . . ? C23 C24 N3A 103.6(8) . . ? N3A C24 C26 125.6(9) . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 O4A N3A 105.2(13) . . ? O4A N3A C24 109.4(13) . . ? O2A N2A C11 99(3) . . ? O2A N2A O1A 141(4) . . ? O1A N2A C11 117(3) . . ? 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 N2 1.257(3) . ? O2 N2 1.253(3) . ? O3 C13 1.212(2) . ? O4 N3 1.410(5) . ? O4 C24 1.272(6) . ? N1 C7 1.468(2) . ? N1 C8 1.473(2) . ? N1 C12 1.316(3) . ? N2 C11 1.399(3) . ? N3 C22 1.398(6) . ? C1 H1 0.9300 . ? C1 C2 1.372(4) . ? C1 C6 1.386(3) . ? C2 H2 0.9300 . ? C2 C3 1.382(4) . ? C3 H3 0.9300 . ? C3 C4 1.395(3) . ? C4 H4 0.9300 . ? C4 C5 1.382(3) . ? C5 C6 1.391(3) . ? C5 C8 1.515(2) . ? C6 C7 1.497(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8 0.9800 . ? C8 C9 1.526(2) . ? C9 H9 0.9800 . ? C9 C10 1.563(2) . ? C9 C13 1.528(2) . ? C10 H10 0.9800 . ? C10 C11 1.496(2) . ? C10 C20 1.507(2) . ? C11 C12 1.363(3) . ? C11 N2A 1.46(2) . ? C12 H12 0.9300 . ? C13 C14 1.489(2) . ? C14 C15 1.387(3) . ? C14 C19 1.391(3) . ? C15 H15 0.9300 . ? C15 C16 1.390(3) . ? C16 H16 0.9300 . ? C16 C17 1.378(4) . ? C17 H17 0.9300 . ? C17 C18 1.376(4) . ? C18 H18 0.9300 . ? C18 C19 1.378(3) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C20 C21 1.318(2) . ? C21 H21 0.9300 . ? C21 C23 1.456(2) . ? C22 C23 1.393(3) . ? C22 C25 1.483(3) . ? C22 O4A 1.209(11) . ? C23 C24 1.381(2) . ? C24 C26 1.478(3) . ? C24 N3A 1.448(9) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? O4A N3A 1.374(10) . ? O2A N2A 1.21(2) . ? O1A N2A 1.23(5) . ? 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 N2 C11 C10 -174.2(2) . . . . ? O1 N2 C11 C12 4.9(4) . . . . ? O2 N2 C11 C10 7.5(5) . . . . ? O2 N2 C11 C12 -173.4(3) . . . . ? O3 C13 C14 C15 165.34(19) . . . . ? O3 C13 C14 C19 -16.0(3) . . . . ? O4 N3 C22 C23 -1.4(4) . . . . ? O4 N3 C22 C25 -179.9(3) . . . . ? N1 C8 C9 C10 46.75(18) . . . . ? N1 C8 C9 C13 165.40(13) . . . . ? N2 C11 C12 N1 179.5(2) . . . . ? N3 O4 C24 C23 -1.5(4) . . . . ? N3 O4 C24 C26 179.4(3) . . . . ? N3 C22 C23 C21 -180.0(4) . . . . ? N3 C22 C23 C24 0.6(4) . . . . ? C1 C2 C3 C4 0.8(4) . . . . ? C1 C6 C7 N1 -166.9(2) . . . . ? C2 C1 C6 C5 -2.4(3) . . . . ? C2 C1 C6 C7 177.7(2) . . . . ? C2 C3 C4 C5 -1.5(4) . . . . ? C3 C4 C5 C6 0.2(3) . . . . ? C3 C4 C5 C8 179.35(19) . . . . ? C4 C5 C6 C1 1.7(3) . . . . ? C4 C5 C6 C7 -178.31(18) . . . . ? C4 C5 C8 N1 164.00(19) . . . . ? C4 C5 C8 C9 41.9(3) . . . . ? C5 C6 C7 N1 13.1(2) . . . . ? C5 C8 C9 C10 163.27(15) . . . . ? C5 C8 C9 C13 -78.09(18) . . . . ? C6 C1 C2 C3 1.1(4) . . . . ? C6 C5 C8 N1 -16.78(18) . . . . ? C6 C5 C8 C9 -138.90(16) . . . . ? C7 N1 C8 C5 25.92(18) . . . . ? C7 N1 C8 C9 152.28(15) . . . . ? C7 N1 C12 C11 -175.27(17) . . . . ? C8 N1 C7 C6 -24.67(19) . . . . ? C8 N1 C12 C11 -0.8(3) . . . . ? C8 C5 C6 C1 -177.57(18) . . . . ? C8 C5 C6 C7 2.4(2) . . . . ? C8 C9 C10 C11 -47.43(17) . . . . ? C8 C9 C10 C20 75.90(17) . . . . ? C8 C9 C13 O3 -15.1(2) . . . . ? C8 C9 C13 C14 169.40(14) . . . . ? C9 C10 C11 N2 -155.0(2) . . . . ? C9 C10 C11 C12 25.9(2) . . . . ? C9 C10 C11 N2A -152(3) . . . . ? C9 C10 C20 C21 115.10(18) . . . . ? C9 C13 C14 C15 -19.1(3) . . . . ? C9 C13 C14 C19 159.51(17) . . . . ? C10 C9 C13 O3 106.37(19) . . . . ? C10 C9 C13 C14 -69.14(18) . . . . ? C10 C11 C12 N1 -1.4(3) . . . . ? C10 C11 N2A O2A -10(6) . . . . ? C10 C11 N2A O1A -173(2) . . . . ? C10 C20 C21 C23 -178.30(16) . . . . ? C11 C10 C20 C21 -122.76(18) . . . . ? C12 N1 C7 C6 150.39(18) . . . . ? C12 N1 C8 C5 -149.33(16) . . . . ? C12 N1 C8 C9 -23.0(2) . . . . ? C12 C11 N2A O2A 172(4) . . . . ? C12 C11 N2A O1A 9(4) . . . . ? C13 C9 C10 C11 -167.34(13) . . . . ? C13 C9 C10 C20 -44.01(17) . . . . ? C13 C14 C15 C16 178.75(18) . . . . ? C13 C14 C19 C18 -178.7(2) . . . . ? C14 C15 C16 C17 -0.4(3) . . . . ? C15 C14 C19 C18 0.1(3) . . . . ? C15 C16 C17 C18 0.5(4) . . . . ? C16 C17 C18 C19 -0.4(4) . . . . ? C17 C18 C19 C14 0.1(4) . . . . ? C19 C14 C15 C16 0.1(3) . . . . ? C20 C10 C11 N2 80.9(2) . . . . ? C20 C10 C11 C12 -98.21(18) . . . . ? C20 C10 C11 N2A 84(3) . . . . ? C20 C21 C23 C22 -22.8(3) . . . . ? C20 C21 C23 C24 156.53(18) . . . . ? C21 C23 C24 O4 -178.9(3) . . . . ? C21 C23 C24 C26 0.0(3) . . . . ? C21 C23 C24 N3A 179.7(6) . . . . ? C22 C23 C24 O4 0.6(3) . . . . ? C22 C23 C24 C26 179.5(2) . . . . ? C22 C23 C24 N3A -0.9(6) . . . . ? C22 O4A N3A C24 -3.1(10) . . . . ? C23 C22 O4A N3A 2.7(9) . . . . ? C23 C24 N3A O4A 2.4(9) . . . . ? C24 O4 N3 C22 1.8(4) . . . . ? C25 C22 C23 C21 -1.7(4) . . . . ? C25 C22 C23 C24 178.8(2) . . . . ? C25 C22 O4A N3A -177.3(6) . . . . ? C26 C24 N3A O4A -177.9(5) . . . . ? O4A C22 C23 C21 178.2(7) . . . . ? O4A C22 C23 C24 -1.2(7) . . . . ? N2A C11 C12 N1 177(2) . . . . ?