#------------------------------------------------------------------------------ #$Date: 2021-11-10 01:16:51 +0200 (Wed, 10 Nov 2021) $ #$Revision: 270546 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/51/1565149.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_1565149 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 O5' _chemical_formula_sum 'C26 H23 N3 O5' _chemical_formula_weight 457.47 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2019-12-15 _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 110.324(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.6642(4) _cell_length_b 18.5733(7) _cell_length_c 13.4479(6) _cell_measurement_reflns_used 1769 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 58.1690 _cell_measurement_theta_min 4.2220 _cell_volume 2263.57(17) _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 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 -47.00 31.00 0.50 8.50 -- -33.50 57.00 0.00 156 2 \w -32.00 64.00 0.50 8.50 -- 36.47 -77.00 150.00 192 3 \w -14.00 18.00 0.50 8.50 -- 36.47 -57.00 0.00 64 4 \w 58.00 97.00 0.50 8.50 -- 36.47 178.00 -90.00 78 5 \w 14.00 72.00 0.50 8.50 -- 36.47 37.00 -30.00 116 6 \w 57.00 110.00 0.50 8.50 -- 36.47 178.00 0.00 106 7 \w 37.00 78.00 0.50 8.50 -- 36.47 57.00-180.00 82 8 \w -32.00 27.00 0.50 8.50 -- 36.47 -77.00-150.00 118 9 \w 38.00 63.00 0.50 8.50 -- 36.47 -77.00-150.00 50 10 \w 40.00 78.00 0.50 35.00 -- 108.00 -94.00 -90.00 76 11 \w 82.00 176.00 0.50 35.00 -- 108.00 30.00-150.00 188 12 \w 50.00 112.00 0.50 35.00 -- 108.00-111.00-150.00 124 13 \w 48.00 129.00 0.50 35.00 -- 108.00 -77.00 -90.00 162 14 \w 101.00 130.00 0.50 35.00 -- 108.00 111.00-120.00 58 15 \w 63.00 131.00 0.50 35.00 -- 108.00 -30.00 150.00 136 16 \w 106.00 171.00 0.50 35.00 -- 108.00 61.00 -60.00 130 17 \w 79.00 144.00 0.50 35.00 -- 108.00 178.00-150.00 130 ; _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 -0.0416056000 _diffrn_orient_matrix_UB_12 0.0756337000 _diffrn_orient_matrix_UB_13 0.0273016000 _diffrn_orient_matrix_UB_21 0.1399874000 _diffrn_orient_matrix_UB_22 0.0311090000 _diffrn_orient_matrix_UB_23 -0.0138731000 _diffrn_orient_matrix_UB_31 -0.0870440000 _diffrn_orient_matrix_UB_32 0.0138644000 _diffrn_orient_matrix_UB_33 -0.1182468000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_unetI/netI 0.0376 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 9067 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.073 _diffrn_reflns_theta_max 67.073 _diffrn_reflns_theta_min 4.238 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.776 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.85403 _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 1.342 _exptl_crystal_description prism _exptl_crystal_F_000 960 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.289 _refine_diff_density_min -0.171 _refine_diff_density_rms 0.043 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 321 _refine_ls_number_reflns 4038 _refine_ls_number_restraints 45 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.1041 _refine_ls_R_factor_gt 0.0685 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1138P)^2^+0.3704P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1907 _refine_ls_wR_factor_ref 0.2181 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2516 _reflns_number_total 4038 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc05741c2.cif _cod_data_source_block zzy1062 _cod_database_code 1565149 _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 0.970 _shelx_estimated_absorpt_t_min 0.892 _reflns_odcompleteness_completeness 99.95 _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, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances N2A-C11A 1.44 with sigma of 0.02 C13A-N2A 1.44 with sigma of 0.02 C11A-C10 1.39 with sigma of 0.02 C14A-N2A 2.5 with sigma of 0.02 C13A-C15A 2.5 with sigma of 0.02 C13-C14 1.53 with sigma of 0.02 C14A-C13A 1.53 with sigma of 0.02 N2A-C12 1.43 with sigma of 0.02 N2-C11 1.43 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C21) = Uanis(C21A) Uanis(C20) = Uanis(C20A) Uanis(C15) = Uanis(C15A) Uanis(C16) = Uanis(C16A) Uanis(C17) = Uanis(C17A) Uanis(C18) = Uanis(C18A) Uanis(C19) = Uanis(C19A) Uanis(C14) = Uanis(C14A) Uanis(C13) = Uanis(C13A) Uanis(C11) = Uanis(C11A) Uanis(N2) = Uanis(N2A) 4. Others Sof(H9B)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=1-FVAR(1) Sof(H9A)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=FVAR(1) Sof(H12A)=Sof(N2A)=Sof(C11A)=Sof(H11A)=Sof(C13A)=Sof(H13C)=Sof(H13D)= Sof(C19A)=Sof(H19A)=Sof(C18A)=Sof(H18A)=Sof(C17A)=Sof(H17A)=Sof(C16A)= Sof(H16A)=Sof(C15A)=Sof(C14A)=1-FVAR(2) Sof(H12)=Sof(N2)=Sof(C11)=Sof(H11)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)= Sof(C19)=Sof(H19)=Sof(C18)=Sof(H18)=Sof(C17)=Sof(H17)=Sof(C16)=Sof(H16)= Sof(C15)=FVAR(2) 5.a Ternary CH refined with riding coordinates: C9(H9A), C9(H9B), C12(H12), C12(H12A) 5.b Secondary CH2 refined with riding coordinates: C13(H13A,H13B), C13A(H13C,H13D) 5.c Aromatic/amide H refined with riding coordinates: N1(H1), C1(H1A), C2(H2), C3(H3), C4(H4A), C11(H11), C19(H19), C18(H18), C17(H17), C16(H16), C20(H20), C21(H21), C11A(H11A), C19A(H19A), C18A(H18A), C17A(H17A), C16A(H16A), C20A(H20A), C21A(H21A) 5.d Fitted hexagon refined as free rotating group: C14(C19,C18,C17,C16,C15), C19A(C18A,C17A,C16A,C15A,C14A) 5.e Idealised Me refined as rotating group: C24(H24A,H24B,H24C), C26(H26A,H26B,H26C) 5.f Idealised tetrahedral OH refined as rotating group: O4(H4) ; _shelx_res_file ; zzy1062.res created by SHELXL-2014/7 TITL zzy1062 in P21/n #14 REM reset to P21/n #14 CELL 1.54184 9.664174 18.573294 13.447942 90 110.324 90 ZERR 4 0.0004 0.000701 0.000556 0 0.0044 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 104 92 12 20 EQIV $1 -0.5+X,1.5-Y,0.5+Z EQIV $2 1-X,1-Y,1-Z DFIX 1.44 N2A C11A DFIX 1.44 C13A N2A DFIX 1.39 C11A C10 DFIX 2.5 C14A N2A DFIX 2.5 C13A C15A DFIX 1.53 C13 C14 DFIX 1.53 C14A C13A DFIX 1.43 N2A C12 DFIX 1.43 N2 C11 ISOR 0.01 0.02 C17 C18 C19 C14 C15 C16 EADP C21 C21A EADP C20 C20A EADP C15 C15A EADP C16 C16A EADP C17 C17A EADP C18 C18A EADP C19 C19A EADP C14 C14A EADP C13 C13A EADP C11 C11A EADP N2 N2A L.S. 4 0 0 PLAN 20 SIZE 0.04 0.07 0.15 MPLA C1 C2 C3 C4 C5 C6 C7 C8 N1 MPLA C14 C15 C16 C17 C18 C19 HTAB O4 O5 HTAB N1 O2_$1 HTAB N1 O4_$2 bond $h conf fmap 2 acta REM REM REM WGHT 0.113800 0.370400 FVAR 5.30639 0.80774 0.69450 O1 4 0.437219 0.639153 0.524758 11.00000 0.09971 0.08123 = 0.08144 0.02086 0.03464 0.00348 O2 4 0.534715 0.815610 0.117310 11.00000 0.14330 0.09530 = 0.11395 0.00896 0.08678 -0.01293 O3 4 0.395126 0.721225 0.102150 11.00000 0.09403 0.11019 = 0.07236 -0.00690 0.03783 -0.01033 O4 4 0.836149 0.462497 0.436956 11.00000 0.08957 0.07562 = 0.14580 0.02774 0.03883 0.02208 AFIX 147 H4 2 0.833492 0.448597 0.378445 11.00000 -1.50000 AFIX 0 O5 4 0.802116 0.471474 0.245421 11.00000 0.09602 0.06459 = 0.14399 -0.00937 0.04818 0.01755 N1 3 0.225987 0.706946 0.482056 11.00000 0.07167 0.12026 = 0.06556 0.01550 0.02988 -0.00899 AFIX 43 H1 2 0.180903 0.682428 0.515747 11.00000 -1.20000 AFIX 0 N3 3 0.474693 0.769350 0.156592 11.00000 0.07450 0.08121 = 0.07778 0.00983 0.04240 0.00725 C1 1 0.232494 0.856305 0.317163 11.00000 0.06704 0.07268 = 0.07516 -0.00146 0.02351 0.01469 AFIX 43 H1A 2 0.297661 0.875175 0.286795 11.00000 -1.20000 AFIX 0 C2 1 0.094910 0.888036 0.298589 11.00000 0.08066 0.09909 = 0.09748 -0.00448 0.01946 0.03123 AFIX 43 H2 2 0.067559 0.928127 0.254656 11.00000 -1.20000 AFIX 0 C3 1 0.000287 0.860914 0.344116 11.00000 0.06641 0.17108 = 0.09455 -0.00743 0.02892 0.03903 AFIX 43 H3 2 -0.090228 0.883332 0.331679 11.00000 -1.20000 AFIX 0 C4 1 0.035837 0.801176 0.407965 11.00000 0.06662 0.17778 = 0.07800 0.00614 0.03662 0.01808 AFIX 43 H4A 2 -0.029425 0.782788 0.438614 11.00000 -1.20000 AFIX 0 C5 1 0.169239 0.769531 0.425254 11.00000 0.05945 0.11488 = 0.05087 -0.00452 0.02053 0.00231 C6 1 0.269785 0.796327 0.381555 11.00000 0.05481 0.07284 = 0.05196 -0.00930 0.01723 0.00395 C7 1 0.401717 0.746482 0.412055 11.00000 0.05698 0.05566 = 0.05938 0.00066 0.02299 0.00320 C8 1 0.359398 0.689105 0.478330 11.00000 0.07265 0.07452 = 0.05318 0.00179 0.02225 -0.00848 C9 1 0.428040 0.714048 0.312427 11.00000 0.05614 0.05760 = 0.06347 0.00344 0.02481 0.00155 PART 1 AFIX 13 H9A 2 0.329837 0.705465 0.259800 21.00000 -1.20000 AFIX 13 PART 0 PART 2 H9B 2 0.339881 0.692254 0.260842 -21.00000 -1.20000 AFIX 0 PART 0 C10 1 0.497450 0.772162 0.266225 11.00000 0.05548 0.06051 = 0.06813 0.00659 0.02756 0.00651 C12 1 0.549037 0.780864 0.484185 11.00000 0.05468 0.06027 = 0.07301 0.00756 0.01360 0.00739 PART 1 AFIX 13 H12 2 0.625186 0.743548 0.507777 31.00000 -1.20000 AFIX 13 PART 0 PART 2 H12A 2 0.619018 0.741316 0.511807 -31.00000 -1.20000 AFIX 0 PART 0 C22 1 0.707817 0.559370 0.331267 11.00000 0.08108 0.07207 = 0.10969 0.00616 0.03819 0.02294 C23 1 0.762418 0.522826 0.426644 11.00000 0.08444 0.08109 = 0.11964 0.01917 0.03783 0.01823 C24 1 0.746713 0.548095 0.527602 11.00000 0.14481 0.15798 = 0.11077 0.04079 0.04026 0.06619 AFIX 137 H24A 2 0.706026 0.510103 0.557333 11.00000 -1.50000 H24B 2 0.682207 0.589069 0.513477 11.00000 -1.50000 H24C 2 0.841810 0.561358 0.576903 11.00000 -1.50000 AFIX 0 C25 1 0.728254 0.527988 0.240629 11.00000 0.07715 0.06935 = 0.11816 -0.00797 0.03553 0.00733 C26 1 0.660064 0.562579 0.131889 11.00000 0.11496 0.09916 = 0.10720 -0.00024 0.03590 0.02659 AFIX 137 H26A 2 0.733714 0.567181 0.099357 11.00000 -1.50000 H26B 2 0.622736 0.609376 0.139480 11.00000 -1.50000 H26C 2 0.580730 0.533001 0.088234 11.00000 -1.50000 AFIX 0 PART 1 N2 3 0.599214 0.838307 0.429094 31.00000 0.05940 0.05195 = 0.08014 -0.00540 0.01558 -0.00189 C11 1 0.576551 0.823206 0.328117 31.00000 0.05194 0.05749 = 0.07406 0.03194 0.02261 0.00788 AFIX 43 H11 2 0.624472 0.853728 0.295777 31.00000 -1.20000 AFIX 0 C13 1 0.658076 0.899919 0.495667 31.00000 0.08658 0.06903 = 0.06072 -0.00531 0.00680 -0.01116 AFIX 23 H13A 2 0.620537 0.944559 0.458700 31.00000 -1.20000 H13B 2 0.765050 0.900510 0.520094 31.00000 -1.20000 AFIX 66 C14 1 0.604180 0.888508 0.584028 31.00000 0.06665 0.07074 = 0.08509 -0.00902 0.00466 0.00683 C19 1 0.617257 0.934616 0.668229 31.00000 0.09344 0.06905 = 0.09446 -0.01460 0.00877 0.00026 AFIX 43 H19 2 0.660425 0.979674 0.671031 31.00000 -1.20000 AFIX 65 C18 1 0.565815 0.913379 0.748240 31.00000 0.09585 0.08696 = 0.09524 -0.02660 0.00923 0.00958 AFIX 43 H18 2 0.574565 0.944229 0.804576 31.00000 -1.20000 AFIX 65 C17 1 0.501296 0.846035 0.744053 31.00000 0.08187 0.09549 = 0.07409 -0.01224 0.00910 0.01385 AFIX 43 H17 2 0.466878 0.831827 0.797586 31.00000 -1.20000 AFIX 65 C16 1 0.488218 0.799926 0.659853 31.00000 0.06093 0.07895 = 0.06702 -0.01327 0.00488 0.00089 AFIX 43 H16 2 0.445049 0.754869 0.657052 31.00000 -1.20000 AFIX 65 C15 1 0.539659 0.821162 0.579841 31.00000 0.04670 0.06632 = 0.07139 -0.00492 0.00562 0.00399 AFIX 0 C20 1 0.506547 0.642772 0.328882 21.00000 0.05508 0.05440 = 0.06396 0.00098 0.02256 -0.00529 AFIX 43 H20 2 0.458826 0.603516 0.345407 21.00000 -1.20000 AFIX 0 C21 1 0.636050 0.631451 0.321896 21.00000 0.06484 0.05271 = 0.09272 -0.00011 0.03529 -0.00225 AFIX 43 H21 2 0.687284 0.671068 0.310258 21.00000 -1.20000 AFIX 0 PART 0 PART 2 N2A 3 0.606560 0.824845 0.414637 -31.00000 0.05940 0.05195 = 0.08014 -0.00540 0.01558 -0.00189 C11A 1 0.568105 0.835135 0.307583 -31.00000 0.05194 0.05749 = 0.07406 0.03194 0.02261 0.00788 AFIX 43 H11A 2 0.585597 0.874992 0.271783 -31.00000 -1.20000 AFIX 0 C13A 1 0.662536 0.898600 0.459982 -31.00000 0.08658 0.06903 = 0.06072 -0.00531 0.00680 -0.01116 AFIX 23 H13C 2 0.610900 0.936944 0.412636 -31.00000 -1.20000 H13D 2 0.767793 0.903424 0.474986 -31.00000 -1.20000 AFIX 66 C19A 1 0.636295 0.951748 0.637145 -31.00000 0.09344 0.06905 = 0.09446 -0.01460 0.00877 0.00026 AFIX 43 H19A 2 0.675178 0.996404 0.629762 -31.00000 -1.20000 AFIX 65 C18A 1 0.589262 0.938955 0.722187 -31.00000 0.09585 0.08696 = 0.09524 -0.02660 0.00923 0.00958 AFIX 43 H18A 2 0.596678 0.975052 0.771704 -31.00000 -1.20000 AFIX 65 C17A 1 0.531147 0.872211 0.733221 -31.00000 0.08187 0.09549 = 0.07409 -0.01224 0.00910 0.01385 AFIX 43 H17A 2 0.499679 0.863652 0.790121 -31.00000 -1.20000 AFIX 65 C16A 1 0.520064 0.818260 0.659213 -31.00000 0.06093 0.07895 = 0.06702 -0.01327 0.00488 0.00089 AFIX 43 H16A 2 0.481181 0.773604 0.666596 -31.00000 -1.20000 AFIX 65 C15A 1 0.567096 0.831052 0.574170 -31.00000 0.04670 0.06632 = 0.07139 -0.00492 0.00562 0.00399 C14A 1 0.625211 0.897795 0.563134 -31.00000 0.06665 0.07074 = 0.08509 -0.00902 0.00466 0.00683 AFIX 0 C20A 1 0.578125 0.656656 0.355525 -21.00000 0.05508 0.05440 = 0.06396 0.00098 0.02256 -0.00529 AFIX 43 H20A 2 0.666151 0.668652 0.408947 -21.00000 -1.20000 AFIX 0 C21A 1 0.556425 0.595369 0.306399 -21.00000 0.06484 0.05271 = 0.09272 -0.00011 0.03529 -0.00225 AFIX 43 H21A 2 0.465927 0.576650 0.263943 -21.00000 -1.20000 AFIX 0 HKLF 4 REM zzy1062 in P21/n #14 REM R1 = 0.0685 for 2516 Fo > 4sig(Fo) and 0.1041 for all 4038 data REM 321 parameters refined using 45 restraints END WGHT 0.1140 0.3703 REM Highest difference peak 0.289, deepest hole -0.171, 1-sigma level 0.043 Q1 1 0.5574 0.6496 0.5395 11.00000 0.05 0.29 Q2 1 0.6162 0.5422 0.6246 11.00000 0.05 0.29 Q3 1 0.6798 0.5938 0.5962 11.00000 0.05 0.26 Q4 1 0.6271 0.6934 0.4799 11.00000 0.05 0.22 Q5 1 0.6350 0.5302 0.3334 11.00000 0.05 0.21 Q6 1 0.6102 0.8795 0.3976 11.00000 0.05 0.18 Q7 1 0.5906 0.7706 0.3004 11.00000 0.05 0.17 Q8 1 0.6231 0.9390 0.5560 11.00000 0.05 0.16 Q9 1 0.5509 0.5748 0.1220 11.00000 0.05 0.16 Q10 1 0.8159 0.6057 0.6171 11.00000 0.05 0.16 Q11 1 0.4955 0.7170 0.1382 11.00000 0.05 0.16 Q12 1 0.7797 0.4539 0.2988 11.00000 0.05 0.15 Q13 1 0.5659 0.8029 0.6392 11.00000 0.05 0.15 Q14 1 0.6662 0.5279 0.0643 11.00000 0.05 0.15 Q15 1 0.6094 0.8793 0.7101 11.00000 0.05 0.15 Q16 1 0.4579 0.7617 0.4437 11.00000 0.05 0.14 Q17 1 0.0860 0.9315 0.3350 11.00000 0.05 0.14 Q18 1 0.7134 0.6226 0.1428 11.00000 0.05 0.14 Q19 1 0.4105 0.7254 0.4663 11.00000 0.05 0.13 Q20 1 0.6375 0.8195 0.1831 11.00000 0.05 0.13 ; _shelx_res_checksum 98219 _shelx_hkl_file ; 0 0 -1 78.9658 41.2304 1 0 0 -2 908.847 128.459 8 0 0 -3 117.438 126.819 8 0 0 -4 1619.25 270.432 4 0 0 -4 2023.52 280.172 2 0 0 -5 104.410 220.629 4 0 0 -5 176.092 212.471 2 0 0 -6 1264.36 271.010 9 0 0 -6 1085.25 312.718 2 0 0 -7 127.123 187.077 9 0 0 -7 101.480 244.311 2 0 0 -8 244.638 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256.433 16 4 11 -8 1970.13 220.857 11 4 11 -7 2754.92 253.178 11 4 -11 -7 2922.89 294.556 16 4 -11 -6 432.347 177.275 16 4 11 -6 411.918 151.101 11 4 -11 -5 1620.80 615.459 8 4 11 -5 1080.82 178.211 11 -4 11 4 5685.94 695.467 1 -4 11 3 107.590 262.451 1 -4 11 2 5469.80 698.507 1 -4 11 1 571.768 326.481 1 -4 11 0 415.792 252.188 3 -4 11 0 110.051 316.462 1 -4 11 -1 105.967 267.986 3 -4 11 -2-22.1217 152.677 13 4 11 2 275.844 122.011 11 -4 11 -3 587.677 168.827 13 -4 11 -4 21529.4 668.506 13 -4 11 -5 327.139 169.039 13 -4 11 -6-52.7251 155.162 13 -4 11 -7 971.202 211.440 13 -4 11 -8 1405.48 217.848 13 -4 11 -9 558.145 158.946 13 -4 11 -10-0.81565 95.3563 13 -4 12 13-66.7609 90.4835 11 4 -12 -13 128.908 115.704 12 4 -12 -12 104.182 153.511 16 4 -12 -11 605.805 188.660 16 4 -12 -10 28.5485 182.495 16 4 -12 -9 39.5589 171.345 16 4 12 -8 1052.16 180.654 11 4 -12 -8 1055.37 228.041 16 4 12 -7 2839.00 254.855 11 4 -12 -7 2673.30 278.446 16 4 -12 -6 413.191 177.186 16 4 12 -6 389.055 159.818 11 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375.237 143.087 11 4 13 0 2438.99 244.717 11 4 13 1 1663.47 215.178 11 -4 13 -2 4279.04 318.634 13 4 13 2 4147.77 298.793 11 -4 13 -3 1825.89 233.128 13 4 13 3 2076.32 226.229 11 -4 13 -4 1907.03 246.867 13 -4 13 -5 1331.02 237.725 13 -4 13 -6 45.3077 168.197 13 -4 13 -7 356.337 182.501 13 -4 13 -8 841.138 169.837 13 -4 -13 -8 1016.34 144.134 15 -4 13 -9 318.248 126.568 13 -4 14 12 266.056 107.877 11 -4 14 11 315.359 124.647 11 4 -14 -11 124.077 141.370 16 -4 14 10 338.971 150.438 11 4 -14 -10 470.919 172.523 16 4 -14 -9-50.8615 155.837 16 4 -14 -8 310.041 167.975 16 4 14 -8 604.745 140.348 11 4 14 -7 327.899 145.508 11 4 -14 -7 425.400 164.573 16 4 14 -6 4825.79 323.404 11 4 -14 -6 4374.74 335.419 16 4 -14 -5 1139.27 199.916 16 4 14 -5 1231.34 202.887 11 4 14 -4 3525.59 292.361 11 4 14 -3 717.518 177.053 11 4 14 -2 425.417 152.168 11 4 14 -1 699.751 178.337 11 4 14 0 5322.01 343.503 11 4 14 1 74.0012 118.974 11 4 14 2 433.736 146.714 11 -4 14 -2 586.266 182.220 13 4 14 3 1444.37 194.216 11 -4 14 -3 1372.94 212.797 13 -4 14 -4 1918.24 246.424 13 -4 14 -5 552.740 184.505 13 -4 14 -6 198.505 163.525 13 -4 14 -7 71.3013 146.186 13 -4 -14 -8-55.9116 78.6844 15 -4 14 -8 92.5355 130.678 13 -4 15 11 981.302 151.200 11 -4 15 10 89.1686 123.576 11 4 -15 -10 19.3807 127.881 16 -4 15 9 307.883 153.183 11 4 -15 -9 226.044 153.493 16 -4 15 8-126.557 151.647 11 4 -15 -8-64.7838 156.877 16 -4 15 7 102.185 136.719 11 4 15 -7 554.895 150.499 11 4 -15 -7 129.280 147.967 16 -4 15 6 95.2554 132.967 11 4 15 -6 73.0106 134.822 11 4 -15 -6-19.3508 143.485 16 4 -15 -5 163.236 139.935 16 -4 15 5 30.7686 122.075 11 4 15 -5 293.690 143.953 11 -4 15 4 374.009 143.663 11 4 15 -4 263.164 155.311 11 4 15 -3 1284.29 210.260 11 4 15 -2 5151.44 343.788 11 4 15 -1 156.408 138.167 11 4 15 0 964.615 190.170 11 4 15 1 3929.44 296.930 11 4 15 2 259.157 136.089 11 -4 15 -2-69.7289 155.443 13 4 15 3-18.2714 116.827 11 -4 15 -3-267.356 182.482 13 -4 15 -4-197.451 175.181 13 -4 15 -5-340.284 177.227 13 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260.966 11 5 7 -8 3765.18 295.189 17 5 -7 -8 3581.09 303.001 16 5 -7 -7 13399.8 1089.59 4 5 -7 -7 11180.9 997.627 2 5 -7 -6 5481.72 695.756 2 -5 7 6 5156.07 625.085 7 -5 7 5 5608.89 614.856 7 5 -7 -5 4025.56 623.620 2 -5 7 4 4888.29 582.266 1 5 -7 -4 4980.90 673.936 2 5 7 -3 3733.72 520.235 5 5 -7 -3 3508.84 574.694 2 -5 7 3 3143.49 487.591 1 -5 7 2 753.285 360.454 1 5 7 -2 531.924 309.313 5 5 -7 -2 669.563 350.949 2 5 7 -1 8225.01 772.405 5 -5 7 1 7960.99 764.821 1 5 7 0 15100.3 1063.06 5 -5 7 0 15551.8 1070.04 1 5 7 1 9178.72 868.693 5 -5 -7 -1 10126.5 835.055 9 -5 7 -1 8418.01 828.817 1 -5 -7 -1 9354.09 882.688 6 5 7 2 1524.28 463.967 5 -5 -7 -2 2008.08 432.510 9 -5 7 -2 2075.53 475.759 1 -5 -7 -2 1300.56 388.289 6 -5 7 -3 2186.09 230.196 13 -5 7 -4 1658.65 217.884 10 -5 7 -4 1300.58 203.530 13 -5 7 -5 872.318 187.131 10 -5 -7 -5 798.109 161.713 15 -5 7 -5 899.969 198.482 13 -5 7 -6 4576.75 340.767 13 -5 -7 -7 300.445 164.021 10 -5 7 -7 627.775 179.785 13 -5 -7 -8 164.390 126.187 10 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263.159 280.790 1 -5 9 3 2915.55 532.447 1 5 9 -2 15839.5 1061.87 5 -5 9 2 16168.6 1136.30 1 -5 9 1 2204.24 493.839 1 5 9 -1 2603.02 536.361 5 5 9 0 15183.1 1096.19 5 -5 -9 0 14825.6 1095.55 6 -5 -9 -1 473.780 364.370 6 -5 9 -2 287.518 147.825 13 -5 9 -3 2834.74 276.488 13 -5 9 -4 182.170 169.768 13 -5 9 -5 2368.19 267.345 13 -5 -9 -6 2007.88 214.029 15 -5 9 -6 1594.07 240.722 13 -5 -9 -7 367.804 143.410 10 -5 9 -7 167.247 167.528 13 -5 -9 -8 22.3382 106.868 10 -5 9 -8 111.858 145.848 13 -5 9 -9 432.307 140.467 13 -5 10 14 70.6331 80.4614 11 5 -10 -14 25.8165 81.6455 12 5 10 -14-87.9739 85.0781 17 5 10 -13 70.6562 99.0986 17 5 -10 -13 126.017 126.844 16 5 10 -12-62.0457 116.283 17 5 -10 -12-112.475 162.551 16 5 -10 -11-55.8063 171.577 16 5 -10 -10 743.468 204.689 16 5 -10 -9 459.438 189.536 16 5 10 -9 145.720 124.167 11 5 -10 -8 1084.10 228.354 16 5 10 -8 1239.51 197.733 11 5 -10 -7 426.885 174.140 16 5 10 -7 394.527 151.616 11 5 10 -6 12664.2 490.123 11 5 -10 -6 11740.3 509.132 16 5 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351.730 158.420 13 -5 13 -3 197.704 153.683 13 -5 13 -4 339.212 170.117 13 -5 13 -5 47.3380 149.460 13 -5 -13 -6 725.762 155.258 15 -5 13 -6 772.424 183.162 13 -5 -13 -7 101.054 109.084 15 -5 13 -7 15.7660 126.746 13 -5 14 12-46.1761 94.7928 11 5 -14 -12-10.5776 109.891 16 -5 14 11 415.317 134.744 11 5 -14 -11 383.673 142.965 16 5 -14 -10-2.53096 142.617 16 5 14 -9 215.950 125.885 11 5 -14 -9-65.7988 153.023 16 5 14 -8 332.759 142.100 11 5 -14 -8 306.428 169.251 16 5 14 -7 1070.08 189.597 11 5 -14 -7 989.949 210.437 16 5 -14 -6 100.643 152.083 16 5 14 -6 116.201 141.591 11 5 14 -5 7296.26 398.724 11 5 -14 -5 7465.70 411.109 16 5 14 -4 120.451 138.543 11 5 14 -3 1794.76 224.389 11 -5 -14 2 81.4687 128.134 15 5 14 -2-163.463 148.147 11 5 14 -1 3052.06 271.200 11 5 14 0 74.6891 128.877 11 5 14 1 78.4249 118.812 11 -5 14 -2 709.773 181.852 13 5 14 2 700.894 151.714 11 -5 14 -3 1048.35 196.201 13 -5 14 -4 9.19186 148.672 13 -5 -14 -5 199.070 136.661 15 -5 14 -5 720.696 181.124 13 -5 -14 -6 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14 7 -4 -9 458.622 178.637 16 7 -4 -9 366.521 132.409 14 7 4 -9 622.319 190.377 14 7 -4 -8 2231.86 267.164 16 7 4 -8 2602.09 283.317 14 7 -4 -8 1788.93 221.657 14 7 -4 -7 4809.68 327.730 14 7 -4 -7 4577.44 343.602 16 -7 4 6 3865.29 298.886 15 -7 -4 6 3972.30 274.834 15 7 4 -6 4122.47 288.535 11 -7 4 5 1171.48 190.959 15 -7 4 4 305.699 139.711 15 7 4 -4 306.892 323.553 5 -7 4 3 641.367 155.340 15 7 4 -3 813.908 357.454 5 -7 4 3 1023.09 416.885 1 -7 4 2 6804.22 351.615 15 -7 -4 2 6526.76 346.655 15 -7 4 1 52.0211 120.210 15 -7 -4 1 192.995 130.427 15 -7 4 0 1641.71 198.758 15 -7 -4 0 1525.89 203.704 15 -7 -4 -1 883.941 177.805 15 -7 4 -2 1155.14 192.646 10 -7 -4 -2 939.435 178.418 15 -7 4 -3 1027.48 186.197 10 -7 -4 -3 1218.81 185.463 15 -7 4 -3 827.924 196.976 13 -7 4 -4 286.582 147.528 10 -7 -4 -4 251.416 135.686 10 -7 4 -4 286.405 154.778 13 -7 4 -5 20.5081 124.978 10 -7 -4 -5 42.9819 120.553 10 -7 4 -5-100.494 170.851 13 -7 4 -6 431.625 153.299 10 -7 -4 -6 25.0293 113.969 10 -7 4 -6 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1542.51 216.590 15 -8 1 2 1886.66 226.305 15 -8 -1 2 1939.81 219.361 15 -8 1 1 557.420 167.996 15 -8 -1 1 321.771 152.525 15 -8 1 0 781.131 172.420 15 -8 -1 0 532.800 160.202 15 -8 1 -1 26.6472 123.533 15 -8 -1 -1-121.470 132.721 15 -8 1 -1 48.9501 117.004 10 -8 -1 -1-170.321 138.797 10 -8 -1 -2 899.660 173.099 15 -8 1 -2 1014.16 181.973 10 -8 -1 -2 880.283 180.984 10 -8 1 -3-4.10826 113.447 10 -8 -1 -3 11.0285 121.145 10 -8 1 -4 1058.15 184.562 10 -8 -1 -4 945.093 174.781 10 -8 1 -4 698.381 179.373 13 -8 1 -5 113.051 122.907 10 -8 -1 -5 174.205 126.980 10 -8 1 -5-131.283 145.585 13 -8 -1 -5-1.09663 142.199 13 -8 1 -6 815.390 147.269 10 -8 -1 -6 726.255 143.290 10 -8 1 -6 754.541 153.569 13 -8 -1 -6 811.078 152.513 13 8 2 -14 190.146 115.598 17 8 -2 -14 125.130 102.894 17 8 2 -13 336.488 160.151 17 8 -2 -13 323.818 140.880 17 8 2 -12 1072.92 208.310 17 8 -2 -12 610.235 167.661 17 8 -2 -11 198.883 144.245 14 8 2 -11-69.2276 175.476 14 8 -2 -10 274.891 155.153 14 8 2 -10 320.527 163.508 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163.545 15 -8 -4 5 29.6530 128.095 15 -8 4 4 425.773 166.809 15 -8 -4 4 186.711 137.825 15 -8 4 3 2045.13 236.983 15 -8 -4 3 1836.60 219.500 15 -8 4 2 516.738 166.315 15 -8 -4 2 558.544 166.386 15 -8 4 1 2839.93 262.225 15 -8 -4 1 2809.87 256.810 15 -8 4 0 81.2431 128.398 15 -8 -4 0 124.847 144.417 15 -8 -4 -1 959.906 184.837 15 -8 4 -1 958.421 192.988 13 -8 -4 -2 2494.50 236.038 15 -8 -4 -2 2670.38 259.600 10 -8 4 -2 2584.76 262.699 13 -8 4 -3 716.965 166.110 10 -8 -4 -3 473.171 139.550 15 -8 -4 -3 233.748 135.784 10 -8 4 -3 455.734 164.683 13 -8 4 -4 383.043 150.174 10 -8 -4 -4 190.973 125.972 10 -8 -4 -5 223.380 122.964 10 -8 4 -5 421.025 160.266 13 -8 -4 -6 34.0415 101.293 10 -8 -4 -6 136.198 108.795 13 8 5 -14-32.0022 100.667 17 8 5 -13 506.104 144.134 17 8 -5 -13 275.391 107.626 17 8 5 -12 280.447 144.966 17 8 -5 -12 256.739 119.680 17 8 5 -11 3313.61 285.115 14 8 5 -11 3612.45 293.796 17 8 -5 -11 3719.56 283.207 16 8 -5 -10 2355.63 255.389 16 8 5 -10 2370.17 267.756 14 8 -5 -9 220.318 163.801 16 8 5 -9 742.081 208.498 14 8 5 -8 9857.86 470.985 14 8 -5 -8 9376.98 470.399 16 8 -5 -7 434.193 205.734 16 -8 -5 6 3568.54 276.511 15 -8 5 5 1183.17 203.383 15 -8 -5 5 1235.52 192.441 15 -8 5 4 286.248 156.887 15 -8 -5 4 297.616 143.378 15 -8 5 3 2377.31 246.690 15 -8 -5 3 2812.63 254.386 15 -8 5 2 133.905 138.136 15 -8 -5 2 105.470 135.785 15 -8 5 1 1475.74 208.225 15 -8 -5 1 1011.07 190.212 15 -8 -5 0 1093.99 185.826 15 -8 5 0 1460.42 210.732 13 -8 -5 -1 713.488 174.098 15 -8 5 -1 399.632 157.610 13 -8 -5 -2 6003.12 342.799 15 -8 5 -2 6753.27 387.295 13 -8 5 -3 1580.03 204.340 10 -8 -5 -3 1217.74 174.811 15 -8 -5 -3 1229.63 196.504 10 -8 5 -3 1419.03 217.129 13 -8 -5 -4 304.952 133.536 10 -8 5 -4 483.881 174.403 13 -8 -5 -5-38.3478 105.362 10 -8 5 -5-52.2842 129.310 13 -8 -5 -6 53.6045 103.649 10 -8 -5 -6-121.742 101.958 13 8 6 -13-60.3413 112.219 17 8 6 -12-64.5198 125.772 17 8 -6 -12 186.128 112.120 17 8 -6 -12 44.9991 123.648 16 8 -6 -11 1629.51 220.461 16 8 6 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202.865 16 8 -11 -8 90.6841 165.564 16 8 -11 -7 304.917 179.844 16 8 11 -7 514.176 158.704 11 8 -11 -6 99.3615 170.832 16 8 11 -6-0.64335 130.697 11 8 -11 -5 470.597 188.929 16 8 11 -5 176.201 134.309 11 8 -11 -4 778.052 192.595 16 -8 -11 4 578.224 144.874 15 8 11 -4 692.854 155.916 11 8 -11 -3 461.067 169.570 16 -8 -11 3 89.1841 128.704 15 8 11 -3 301.556 128.670 11 8 -11 -2 81.7948 143.684 16 -8 -11 2 154.507 132.960 15 -8 -11 1 939.072 184.110 15 -8 -11 0 501.603 165.032 15 -8 -11 -1 74.5902 133.600 15 -8 -11 -2 54.6272 125.687 15 -8 11 -2 53.5860 115.301 13 -8 -11 -3-166.441 118.139 15 -8 11 -3 132.963 115.115 13 -8 -11 -4 134.520 76.3443 15 -8 -11 -4 13.6505 94.9488 10 8 -12 -11-18.7819 106.195 16 8 -12 -10 29.1512 128.367 16 8 -12 -9 360.250 157.748 16 8 -12 -8 187.690 154.557 16 8 -12 -7 407.656 165.619 16 8 12 -7 6.79838 122.261 11 8 -12 -6-87.0901 166.468 16 8 12 -6 134.187 125.419 11 8 -12 -5-160.154 157.140 16 8 12 -5-209.575 131.822 11 8 -12 -4 49.1547 144.226 16 -8 -12 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1 33.5964 131.588 15 -9 -2 1 185.291 144.454 15 -9 2 0 425.914 149.850 15 -9 -2 0 869.033 182.188 15 -9 -2 -1 127.364 126.901 15 -9 -2 -1 241.911 120.808 10 -9 2 -1 148.531 139.012 13 -9 -2 -2 852.319 155.990 15 -9 -2 -2 805.754 155.855 10 -9 2 -2 529.508 156.311 13 -9 2 -3 676.551 146.045 10 -9 -2 -3 447.146 127.376 10 -9 2 -3 343.297 146.047 13 -9 2 -4 443.374 122.069 10 -9 -2 -4 822.506 143.992 10 -9 2 -4 390.271 140.129 13 -9 -2 -4 535.206 148.584 13 9 3 -13 19.4505 106.962 17 9 -3 -13 83.1449 101.072 17 9 3 -12 81.3350 129.852 17 9 -3 -12 123.993 127.296 17 9 -3 -11-98.5374 126.092 14 9 3 -11 97.7652 163.843 14 9 -3 -10 1397.99 198.039 16 9 -3 -10 1054.99 171.152 14 9 3 -10 1222.83 216.298 14 9 -3 -9 3721.96 281.944 14 9 3 -9 4047.60 328.830 14 9 -3 -9 4135.78 303.145 16 9 -3 -8 23.0762 155.002 16 -9 -3 8 30.1498 124.098 15 9 -3 -8 57.8999 143.288 14 9 3 -8 93.3434 174.637 14 -9 -3 7 2297.80 232.179 15 9 -3 -7 2337.78 256.157 14 -9 -3 6 2450.63 248.756 15 -9 3 6 2426.46 257.110 15 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14 9 4 -9 145.452 177.409 14 9 -4 -8 288.536 175.106 16 9 -4 -8 97.0440 134.757 14 9 4 -8 180.430 194.041 14 9 -4 -7 448.432 188.126 16 -9 -4 7 314.725 147.772 15 9 -4 -7 454.544 159.730 14 -9 -4 6 1754.62 219.759 15 -9 4 5 723.056 198.013 15 -9 -4 5 411.693 153.785 15 -9 4 4 4023.25 305.547 15 -9 -4 4 3921.36 298.283 15 -9 4 3 1336.56 210.927 15 -9 -4 3 1442.91 213.289 15 -9 4 2 2550.77 246.663 15 -9 -4 2 2849.43 266.063 15 -9 4 1 403.103 149.633 15 -9 -4 1 391.149 165.477 15 -9 4 1 352.271 133.804 13 -9 -4 0 262.444 146.013 15 -9 -4 0 296.020 136.641 10 -9 4 0 206.733 127.640 13 -9 -4 -1 112.272 129.216 15 -9 -4 -1 29.1631 120.286 10 -9 4 -1 8.49660 134.429 13 -9 -4 -2 120.272 110.261 15 -9 -4 -2 13.0500 107.316 10 -9 4 -2 102.668 140.424 13 -9 -4 -3-17.5883 104.575 10 -9 4 -3 177.717 129.631 13 -9 -4 -4-22.9405 90.8919 10 -9 4 -4 158.440 120.415 13 -9 -4 -4-133.567 120.160 13 9 5 -13 84.4747 95.1163 17 9 -5 -13-1.91146 77.7227 17 9 5 -12 168.914 119.566 17 9 -5 -12 512.455 125.203 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133.306 14 9 6 -11 33.4214 107.445 17 9 -6 -10 88.0009 142.549 16 9 6 -10 128.166 151.045 14 9 6 -10 96.6206 124.486 17 9 -6 -9 21.6949 160.340 16 9 6 -9 128.347 153.002 14 9 -6 -8 886.769 203.963 16 9 6 -8 876.196 201.603 14 9 -6 -7 282.081 192.212 16 -9 -6 7 395.175 140.699 15 9 6 -7 505.441 204.917 14 -9 -6 6 2928.79 253.274 15 9 -6 -6 3292.20 312.260 16 -9 -6 5 1139.21 193.842 15 -9 -6 4 198.771 147.543 15 -9 -6 3 431.172 159.355 15 -9 -6 2 6050.91 356.322 15 -9 -6 1-195.601 164.104 15 -9 -6 0 339.362 155.229 15 -9 6 0 292.571 140.041 13 -9 -6 -1 418.584 145.328 15 -9 -6 -1 450.978 132.580 10 -9 6 -1 484.420 144.414 13 -9 -6 -2 263.408 125.764 15 -9 -6 -2 540.615 137.701 10 -9 6 -2 691.989 156.416 13 -9 -6 -3-124.515 90.4165 15 -9 -6 -3-33.2659 105.093 10 -9 -6 -4 204.940 101.385 10 -9 6 -4-90.8536 110.350 13 9 7 -12 335.003 102.202 17 9 -7 -12 293.285 106.087 16 9 -7 -11 3.59438 117.019 16 9 7 -11-224.323 135.042 14 9 7 -11 6.46916 93.3089 17 9 -7 -10-14.7287 136.096 16 9 7 -10-28.4047 145.402 14 9 7 -10 158.114 116.781 17 9 -7 -9-122.444 163.137 16 9 7 -9-11.9136 147.753 14 9 -7 -8 1486.81 234.242 16 9 7 -8 1821.03 235.741 14 9 -7 -7 398.615 207.046 16 9 7 -7 527.627 189.124 14 9 -7 -6 344.310 198.569 16 -9 -7 6 290.385 134.338 15 9 -7 -5 432.446 195.203 16 -9 -7 5 418.611 141.409 15 -9 -7 4 89.1528 134.466 15 -9 -7 3 178.219 145.408 15 -9 -7 2 2241.26 241.420 15 -9 -7 1 1197.38 204.073 15 -9 -7 0 850.170 181.001 15 -9 -7 -1 471.404 148.204 15 -9 -7 -1 329.228 128.793 10 -9 -7 -2 374.912 132.456 15 -9 -7 -2 202.411 114.286 10 -9 7 -2 343.629 133.853 13 -9 -7 -3-149.183 92.2311 15 -9 -7 -3-78.7216 101.797 10 -9 7 -3-173.888 127.310 13 9 -8 -12 284.391 96.8209 16 9 -8 -11 174.705 119.990 16 9 -8 -10 105.850 141.739 16 9 8 -10-198.431 136.957 14 9 -8 -9 477.614 172.150 16 9 8 -9 385.270 153.462 14 9 -8 -8-60.7358 168.130 16 9 8 -8 401.512 158.597 14 9 -8 -7 2557.86 279.892 16 9 8 -7 3203.98 280.196 14 9 -8 -6 171.110 183.239 16 -9 -8 6 186.312 121.645 15 9 -8 -5 121.853 175.552 16 -9 -8 5 149.361 130.409 15 9 -8 -4 396.521 202.217 16 -9 -8 4 150.266 137.900 15 -9 -8 3 18.1945 135.050 15 -9 -8 2 361.801 163.709 15 -9 -8 1 271.454 151.684 15 -9 -8 0-66.5852 140.517 15 -9 -8 -1 184.403 132.101 15 -9 8 -1-1.78037 115.024 13 -9 -8 -2-42.5726 107.574 15 -9 -8 -2-191.245 116.680 10 -9 8 -2-325.530 132.398 13 -9 -8 -3 662.911 101.938 15 -9 -8 -3 923.764 142.817 10 -9 8 -3 1027.88 142.403 13 9 -9 -11 558.303 133.744 16 9 -9 -10 287.731 144.646 16 9 9 -10-67.0043 114.054 14 9 -9 -9 447.589 165.109 16 9 9 -9 15.9232 123.386 14 9 -9 -8 481.691 187.681 16 9 9 -8 532.839 146.813 14 9 -9 -7 311.684 184.204 16 9 9 -7 424.390 154.714 14 -9 -9 6 329.816 124.528 15 9 9 -6 578.627 175.706 14 9 -9 -5 65.8777 161.599 16 -9 -9 5 81.2957 120.894 15 9 -9 -4 215.059 175.626 16 -9 -9 4 57.3975 122.672 15 9 -9 -3 443.323 169.750 16 -9 -9 3 510.576 157.657 15 9 -9 -2 407.548 168.779 16 -9 -9 2 301.758 149.134 15 9 -9 -1 1399.82 199.916 16 -9 -9 1 874.817 174.843 15 -9 -9 0 156.247 135.108 15 -9 -9 -1 109.781 125.154 15 -9 -9 -2-65.8353 104.136 15 -9 -9 -2-23.4221 103.376 10 -9 9 -2-32.9616 101.181 13 9 -10 -10-47.9408 121.486 16 9 -10 -9 13.7200 136.292 16 9 -10 -8 182.432 160.961 16 9 -10 -7 53.8554 165.669 16 9 -10 -6 47.7932 158.820 16 9 -10 -5 155.252 167.937 16 -9 -10 5 221.049 126.785 15 9 -10 -4 302.027 162.744 16 -9 -10 4-67.8904 122.038 15 9 -10 -3 213.390 153.607 16 -9 -10 3-121.072 134.011 15 9 -10 -2 456.874 156.185 16 -9 -10 2 401.926 149.146 15 9 -10 -1 742.346 152.621 16 -9 -10 1 759.384 168.308 15 -9 -10 0 1023.16 166.940 15 -9 -10 -1 115.404 118.963 15 -9 -10 -2 40.4803 93.8181 15 -9 -10 -2-21.9051 93.0608 10 9 -11 -10 51.2158 107.192 16 9 -11 -9 2.56638 121.898 16 9 -11 -8 312.844 146.899 16 9 -11 -7 1133.08 181.354 16 9 -11 -6-82.8977 140.102 16 9 -11 -5-260.541 160.763 16 -9 -11 5-6.65591 98.4684 15 9 -11 -4 453.407 158.327 16 -9 -11 4 177.511 117.231 15 9 -11 -3 1546.31 200.468 16 -9 -11 3 1291.48 173.343 15 9 -11 -2 351.716 132.006 16 -9 -11 2 566.917 142.807 15 -9 -11 1 91.4223 119.662 15 -9 -11 0-112.101 114.940 15 -9 -11 -1-91.7257 98.5019 15 9 -12 -9 29.0904 106.872 16 9 -12 -8 695.209 154.203 16 9 -12 -7 929.204 164.078 16 9 -12 -6 105.909 129.423 16 9 -12 -5-196.012 131.473 16 9 -12 -4 94.1544 122.864 16 -9 -12 4 74.2963 94.2409 15 9 -12 -3 119.593 122.205 16 -9 -12 3-12.6595 101.038 15 -9 -12 2 652.927 135.506 15 -9 -12 1 525.602 127.336 15 -9 -12 0 162.973 102.415 15 9 -13 -7 253.443 115.943 16 9 -13 -6 201.143 119.075 16 9 -13 -5 274.707 112.331 16 9 -13 -4 466.232 122.741 16 -9 -13 4 582.160 107.404 15 -9 -13 3 321.577 105.971 15 -9 -13 2-100.219 97.7932 15 10 0 -12 453.804 130.327 17 10 0 -11-0.24570 118.817 14 10 0 -10 92.8963 128.666 14 10 0 -9 151.754 151.537 14 10 0 -8 798.394 185.899 14 -10 0 7 190.278 149.522 15 10 0 -7 372.473 171.272 14 -10 0 6 914.098 190.053 15 -10 0 5-14.3936 147.913 15 -10 0 4 150.473 156.154 15 -10 0 3 2.77632 139.720 15 -10 0 2 3055.26 255.660 15 -10 0 1-93.4981 132.833 15 -10 0 0 202.238 120.857 15 -10 0 -1-176.720 129.520 13 -10 0 -2 955.416 146.153 13 10 1 -12 829.221 144.747 17 10 -1 -12 793.042 148.825 17 10 -1 -11 414.849 125.450 14 10 1 -11 290.649 126.571 14 10 -1 -10 575.356 147.157 14 10 1 -10 440.708 144.404 14 10 -1 -9 130.750 137.519 14 10 1 -9 109.296 145.480 14 10 -1 -8 389.680 152.903 16 -10 -1 8 528.823 149.891 15 10 -1 -8 531.668 162.587 14 10 1 -8 725.669 192.730 14 10 -1 -7 280.694 172.445 16 -10 1 7-20.7185 144.388 15 -10 -1 7 182.750 140.721 15 10 -1 -7 191.172 160.032 14 -10 1 6 253.298 159.348 15 -10 -1 6 79.9990 141.087 15 -10 1 5-46.6098 155.054 15 -10 -1 5 114.071 157.350 15 -10 1 4 430.025 174.716 15 -10 -1 4 303.431 166.188 15 -10 1 3 35.8039 146.259 15 -10 -1 3 161.988 156.586 15 -10 1 2 11.7310 132.069 15 -10 -1 2 389.021 151.834 15 -10 1 1 979.066 169.934 15 -10 -1 1 913.827 169.056 15 -10 1 1 678.110 144.149 13 -10 1 0-89.3097 116.601 15 -10 -1 0 117.893 110.188 15 -10 1 0-76.7848 124.013 13 -10 -1 -1 190.764 108.301 15 -10 1 -1-57.6198 117.025 13 -10 1 -2 37.1192 104.692 13 -10 -1 -2-49.3980 112.364 13 10 2 -12-8.32139 102.195 17 10 -2 -12 138.305 103.897 17 10 -2 -11 0.22228 109.848 14 10 2 -11-0.50178 128.965 14 10 -2 -10 35.7467 117.892 14 10 2 -10-42.6366 147.480 14 10 -2 -9-144.862 137.810 16 10 -2 -9 103.708 129.873 14 10 2 -9 40.9308 145.856 14 10 -2 -8 479.530 166.686 16 -10 -2 8 266.231 139.353 15 10 -2 -8 116.230 132.649 14 10 2 -8 353.236 186.893 14 10 -2 -7 404.949 165.504 16 -10 -2 7 345.397 146.456 15 10 -2 -7 740.991 179.233 14 -10 2 6 1236.73 206.714 15 -10 -2 6 1635.48 215.139 15 -10 2 5 316.687 171.898 15 -10 -2 5 168.337 147.988 15 -10 2 4 36.7788 146.806 15 -10 -2 4 137.627 152.722 15 -10 2 3 24.1204 135.620 15 -10 -2 3 26.0133 143.172 15 -10 2 2 42.1967 129.504 15 -10 -2 2 104.170 135.403 15 -10 2 1 47.7312 117.774 15 -10 -2 1 232.247 142.627 15 -10 2 1-227.794 127.910 13 -10 -2 0 6.91332 114.613 15 -10 2 0-116.573 120.670 13 -10 -2 -1 194.521 107.881 15 -10 2 -1-27.8612 106.657 13 -10 -2 -2 197.568 100.994 10 -10 2 -2 270.790 118.487 13 -10 -2 -2-46.9001 114.297 13 10 3 -12 402.910 116.841 17 10 -3 -12 802.089 133.695 17 10 3 -11 8.02323 126.390 14 10 3 -11 554.203 137.791 17 10 -3 -10 40.6429 110.032 14 10 3 -10 249.798 140.767 14 10 -3 -9-153.375 141.728 16 10 -3 -9-125.667 116.737 14 10 3 -9 241.990 160.181 14 10 -3 -8 523.456 169.229 16 -10 -3 8 622.279 148.803 15 10 -3 -8 676.673 157.831 14 10 3 -8 547.088 179.302 14 10 -3 -7 1350.36 215.374 16 -10 -3 7 1289.54 190.038 15 10 -3 -7 1295.14 188.277 14 10 3 -7 1389.99 244.647 14 -10 -3 6 108.023 139.809 15 -10 3 5 131.205 155.031 15 -10 -3 5 135.575 143.111 15 -10 3 4 632.547 173.032 15 -10 -3 4 740.667 182.818 15 -10 3 3 323.872 150.085 15 -10 -3 3 241.535 158.000 15 -10 3 2 188.080 131.906 15 -10 -3 2 313.472 158.378 15 -10 3 1 425.812 137.096 15 -10 -3 1 303.135 140.638 15 -10 -3 0 130.956 117.791 15 -10 3 0 283.211 117.387 13 -10 -3 -1 125.311 101.013 15 -10 3 -1 214.058 114.115 13 -10 -3 -2 300.453 103.518 10 -10 3 -2 126.928 105.516 13 -10 -3 -2 191.658 107.509 13 10 4 -11-111.644 129.820 14 10 4 -11 420.479 126.837 17 10 -4 -10-134.082 122.210 16 10 4 -10-170.795 152.258 14 10 4 -10 261.109 132.730 17 10 -4 -9-139.015 136.287 16 10 4 -9-224.083 159.909 14 10 -4 -8 54.3577 156.196 16 -10 -4 8 41.1169 109.300 15 10 4 -8 219.665 171.272 14 10 -4 -7 824.732 193.653 16 -10 -4 7 543.473 145.810 15 10 4 -7 939.657 213.298 14 10 -4 -6 550.454 187.717 16 -10 -4 6 220.152 143.391 15 -10 -4 5-190.176 146.706 15 -10 -4 4 351.422 159.118 15 -10 -4 3 222.213 151.891 15 -10 -4 2 506.617 161.431 15 -10 -4 1 795.136 160.784 15 -10 -4 0-37.2047 118.042 15 -10 4 0 178.079 106.532 13 -10 -4 -1 190.654 106.268 15 -10 -4 -1 51.1520 87.1507 10 -10 4 -1 265.400 109.138 13 -10 -4 -2-31.0808 81.9617 10 -10 4 -2 228.558 106.365 13 10 5 -11 34.2409 116.436 14 10 5 -11-7.06084 90.3076 17 10 -5 -10 374.814 129.345 16 10 5 -10 524.059 130.867 17 10 -5 -9 217.149 138.987 16 10 5 -9 176.574 154.416 14 10 -5 -8-65.1502 151.586 16 10 5 -8 215.499 165.869 14 10 -5 -7 458.346 178.884 16 -10 -5 7 336.936 135.381 15 10 5 -7 439.589 180.640 14 10 -5 -6 410.910 179.803 16 -10 -5 6 301.004 142.292 15 -10 -5 5 83.0701 137.166 15 -10 -5 4-184.317 145.593 15 -10 -5 3 162.697 138.596 15 -10 -5 2 233.261 140.796 15 -10 -5 1 79.4997 128.661 15 -10 -5 0 228.113 126.710 15 -10 -5 0 237.876 99.2127 10 -10 -5 -1 242.001 107.020 15 -10 -5 -1 327.539 105.356 10 -10 5 -1 509.539 116.194 13 10 -6 -11 80.5805 91.5846 16 10 -6 -11 79.0147 78.9328 17 10 -6 -10 65.9296 120.667 16 10 6 -10-90.4196 130.724 14 10 -6 -9-216.752 148.640 16 10 6 -9-200.321 140.360 14 10 -6 -8 261.539 151.880 16 10 6 -8 602.571 173.380 14 10 -6 -7 277.531 165.217 16 -10 -6 7 23.8815 109.730 15 10 -6 -6 659.720 200.854 16 -10 -6 6 130.572 120.812 15 10 -6 -5 439.022 191.606 16 -10 -6 5 496.674 153.198 15 -10 -6 4 195.356 146.028 15 -10 -6 3 73.3725 137.515 15 -10 -6 2 218.708 134.041 15 -10 -6 1 141.635 126.438 15 -10 -6 0 153.720 118.118 15 -10 -6 0 151.638 96.9408 10 -10 -6 -1 152.430 97.1206 15 -10 -6 -1-80.4729 83.3549 10 10 -7 -10 156.714 115.930 16 10 7 -10-260.131 131.269 14 10 -7 -9-261.251 146.108 16 10 7 -9-148.693 130.125 14 10 -7 -8 425.360 157.076 16 10 7 -8 202.113 136.729 14 10 -7 -7 265.350 164.775 16 -10 -7 7 234.255 110.670 15 10 7 -7 275.543 159.702 14 10 -7 -6 543.781 181.577 16 -10 -7 6 395.336 134.072 15 10 7 -6 619.938 177.811 14 10 -7 -5 480.310 185.228 16 -10 -7 5 84.8667 119.969 15 10 -7 -4 595.517 182.693 16 -10 -7 4 469.014 144.465 15 -10 -7 3-17.7404 125.709 15 -10 -7 2 48.5149 128.724 15 -10 -7 1 37.9944 119.923 15 -10 -7 0-109.479 112.234 15 -10 -7 0-112.805 93.4127 10 -10 -7 -1 706.830 116.238 15 -10 -7 -1 609.604 109.385 10 10 -8 -10 501.518 120.318 16 10 8 -10-103.494 91.6454 14 10 -8 -9 196.582 133.841 16 10 8 -9-59.2647 117.287 14 10 -8 -8-68.9471 135.652 16 10 8 -8-226.138 128.814 14 10 -8 -7 655.496 176.543 16 10 8 -7 844.948 162.916 14 10 -8 -6 133.720 150.282 16 -10 -8 6 85.2751 103.639 15 10 8 -6 353.291 146.925 14 10 -8 -5 233.163 158.808 16 -10 -8 5 54.3196 111.016 15 10 -8 -4 214.750 155.271 16 -10 -8 4 207.026 124.941 15 10 -8 -3 1158.64 184.452 16 -10 -8 3 1396.95 179.329 15 10 -8 -2-38.3451 125.547 16 -10 -8 2 103.710 118.368 15 10 -8 -1 307.626 129.711 16 -10 -8 1 291.562 122.330 15 -10 -8 1 178.885 97.0151 10 10 -8 0 383.531 110.806 16 -10 -8 0 457.815 118.020 15 -10 -8 0 344.297 106.410 10 10 -9 -9 103.825 111.227 16 10 9 -9-185.386 98.8138 14 10 -9 -8 381.418 137.770 16 10 9 -8 240.663 99.5356 14 10 -9 -7 53.1746 131.671 16 10 9 -7 325.821 124.828 14 10 -9 -6 196.605 146.117 16 -10 -9 6 1.49140 94.3069 15 10 9 -6 251.313 129.417 14 10 -9 -5 26.4281 134.116 16 -10 -9 5 196.866 110.367 15 10 9 -5 383.328 142.164 14 10 -9 -4-7.98509 134.054 16 -10 -9 4 524.505 132.730 15 10 -9 -3 1158.68 176.598 16 -10 -9 3 1041.26 153.540 15 10 -9 -2 256.315 125.679 16 -10 -9 2 252.613 116.213 15 10 -9 -1 43.7705 101.594 16 -10 -9 1-1.19130 105.542 15 -10 -9 1-103.100 98.6148 10 10 -10 -8 279.491 124.210 16 10 -10 -7-200.496 133.954 16 10 -10 -6-103.152 127.883 16 10 -10 -5 405.355 138.141 16 -10 -10 5 241.133 99.2995 15 10 -10 -4-17.3885 117.015 16 -10 -10 4 246.013 105.277 15 -10 -10 3 2497.57 185.814 15 10 -10 -3 2490.98 199.571 16 10 -10 -2 17.9133 95.9823 16 -10 -10 2 195.024 109.624 15 10 -11 -5-34.8326 109.621 16 10 -11 -4-84.0796 106.560 16 -10 -11 4 277.290 91.6683 15 11 0 -9 10.5424 104.771 14 11 0 -8 104.903 114.537 14 11 0 -7 416.410 119.827 16 11 0 -7 868.426 160.241 14 11 0 -6 374.399 141.462 16 11 0 -6 194.688 137.375 14 -11 0 5 72.7109 125.897 15 -11 0 4 61.4961 118.616 15 -11 0 3 41.8685 111.623 15 -11 0 2 20.6657 101.729 15 -11 0 1 39.3636 82.2507 13 11 -1 -9 1481.52 159.594 14 11 1 -9 1629.80 175.637 14 11 -1 -8 27.4145 111.283 14 11 1 -8 173.768 125.050 14 11 -1 -7 205.032 128.153 16 11 -1 -7 268.715 134.491 14 11 1 -7 315.343 142.262 14 11 -1 -6 215.585 141.601 16 11 1 -6 349.977 139.147 16 -11 -1 6 40.8296 123.595 15 11 -1 -6 355.884 135.603 14 11 1 -6 308.485 150.673 14 -11 -1 5 423.809 143.152 15 -11 1 4-136.528 124.185 15 -11 -1 4 46.8261 122.115 15 -11 1 3 121.682 118.732 15 -11 -1 3 223.751 122.000 15 -11 -1 2 27.3870 98.9514 15 -11 -1 1 252.227 82.7165 15 -11 -1 1 321.862 98.1815 13 11 -2 -9-61.9464 96.7618 14 11 2 -9 112.309 113.095 14 11 -2 -8-60.6627 89.7931 16 11 -2 -8-63.9371 105.169 14 11 2 -8 76.9857 124.188 14 11 -2 -7 340.612 135.476 16 11 -2 -7 311.950 120.885 14 11 2 -7 496.118 151.847 14 11 -2 -6 407.016 148.477 16 -11 -2 6 174.524 118.493 15 11 -2 -6 454.239 131.891 14 -11 -2 5 65.7357 126.059 15 11 -2 -5 178.288 123.140 14 -11 -2 4-72.2127 120.968 15 -11 -2 3 644.681 148.138 15 -11 -2 2-31.0490 105.073 15 -11 -2 2-12.0375 87.0886 13 -11 -2 1 180.483 82.0844 15 -11 -2 1-45.2494 83.5333 13 11 -3 -9 124.429 93.0916 16 11 3 -9 181.385 116.036 14 11 -3 -8 800.672 138.084 16 11 3 -8 1138.06 167.279 14 11 -3 -7-36.2571 118.979 16 -11 -3 7 37.2782 105.008 15 11 -3 -7-2.39930 99.1642 14 11 3 -7 120.505 134.502 14 11 -3 -6 291.499 145.703 16 -11 -3 6 179.576 119.253 15 11 -3 -6-154.267 96.7864 14 11 3 -6 352.115 148.708 14 11 -3 -5 397.508 153.468 16 -11 -3 5 26.0530 113.958 15 11 -3 -5 175.851 111.178 14 -11 -3 4 7.78258 113.256 15 -11 -3 3 309.055 117.247 15 -11 -3 2 165.426 114.002 15 11 -4 -9-94.7970 99.2134 16 11 4 -9 120.755 111.067 14 11 -4 -8 445.952 129.826 16 11 4 -8 203.860 120.170 14 11 -4 -7 526.006 146.220 16 -11 -4 7 245.245 108.694 15 11 4 -7 358.071 146.145 14 11 -4 -6 16.0138 133.033 16 -11 -4 6-32.6534 105.552 15 11 4 -6 162.524 137.599 14 11 -4 -5 98.6902 139.804 16 -11 -4 5-4.99763 107.947 15 -11 -4 4 119.872 110.524 15 -11 -4 3 100.528 110.137 15 -11 -4 2 241.587 110.916 15 11 -5 -8 58.0243 107.791 16 11 5 -8 90.8169 112.272 14 11 -5 -7-5.57344 117.204 16 -11 -5 7 131.402 92.4286 15 11 -5 -6 284.407 137.764 16 -11 -5 6 83.6048 100.070 15 11 5 -6 343.235 137.049 14 11 -5 -5 97.5253 137.767 16 -11 -5 5-19.7835 104.797 15 11 -5 -4-5.41773 123.362 16 -11 -5 4 93.3165 111.198 15 11 -5 -3 551.283 143.558 16 -11 -5 3 583.874 129.817 15 11 -6 -7 46.8575 112.381 16 -11 -6 7-1.93064 82.2284 15 11 6 -7 183.561 123.480 14 11 -6 -6 422.753 134.304 16 -11 -6 6 249.056 101.403 15 11 6 -6 583.658 144.042 14 11 -6 -5 144.812 125.591 16 -11 -6 5 16.3284 101.344 15 11 6 -5 334.715 131.898 14 11 -6 -4 108.525 119.892 16 -11 -6 4 140.332 107.705 15 0 0 0 0.00 0.00 0 TITL zzy1062 in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 1.54184 9.664174 18.573294 13.447942 90.0000 110.3240 90.0000 ZERR 3.00 0.000400 0.000701 0.000556 0.0000 0.0044 0.0000 LATT 1 SYMM -x+1/2, 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 52170 _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 1.360 _oxdiff_exptl_absorpt_empirical_full_min 0.840 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 0.4372(3) 0.63915(16) 0.5248(2) 0.0866(8) Uani 1 1 d . . . . . O2 O 0.5347(4) 0.81561(17) 0.1173(3) 0.1064(10) Uani 1 1 d . . . . . O3 O 0.3951(3) 0.72123(18) 0.1022(2) 0.0898(8) Uani 1 1 d . . . . . O4 O 0.8361(4) 0.46250(17) 0.4370(3) 0.1042(10) Uani 1 1 d . . . . . H4 H 0.8335 0.4486 0.3784 0.156 Uiso 1 1 calc GR . . . . O5 O 0.8021(3) 0.47147(15) 0.2454(3) 0.0998(9) Uani 1 1 d . . . . . N1 N 0.2260(3) 0.7069(2) 0.4821(2) 0.0842(10) Uani 1 1 d . . . . . H1 H 0.1809 0.6824 0.5157 0.101 Uiso 1 1 calc R . . . . N3 N 0.4747(3) 0.76935(18) 0.1566(2) 0.0736(8) Uani 1 1 d . . . . . C1 C 0.2325(4) 0.8563(2) 0.3172(3) 0.0719(9) Uani 1 1 d . . . . . H1A H 0.2977 0.8752 0.2868 0.086 Uiso 1 1 calc R . . . . C2 C 0.0949(5) 0.8880(3) 0.2986(4) 0.0954(13) Uani 1 1 d . . . . . H2 H 0.0676 0.9281 0.2547 0.115 Uiso 1 1 calc R . . . . C3 C 0.0003(5) 0.8609(4) 0.3441(4) 0.1104(18) Uani 1 1 d . . . . . H3 H -0.0902 0.8833 0.3317 0.133 Uiso 1 1 calc R . . . . C4 C 0.0358(4) 0.8012(3) 0.4080(3) 0.1044(16) Uani 1 1 d . . . . . H4A H -0.0294 0.7828 0.4386 0.125 Uiso 1 1 calc R . . . . C5 C 0.1692(4) 0.7695(2) 0.4253(3) 0.0747(10) Uani 1 1 d . . . . . C6 C 0.2698(3) 0.79633(19) 0.3816(2) 0.0602(8) Uani 1 1 d . . . . . C7 C 0.4017(3) 0.74648(17) 0.4121(2) 0.0566(7) Uani 1 1 d . . . . . C8 C 0.3594(4) 0.6891(2) 0.4783(2) 0.0667(8) Uani 1 1 d . . . . . C9 C 0.4280(3) 0.71405(17) 0.3124(2) 0.0580(7) Uani 1 1 d . . . . . H9A H 0.3298 0.7055 0.2598 0.070 Uiso 0.808(6) 1 calc R . P A 1 H9B H 0.3399 0.6923 0.2608 0.070 Uiso 0.192(6) 1 calc R . P A 2 C10 C 0.4975(3) 0.77216(18) 0.2662(3) 0.0598(8) Uani 1 1 d D . . . . C12 C 0.5490(3) 0.78086(18) 0.4842(3) 0.0649(8) Uani 1 1 d D . . . . H12 H 0.6252 0.7435 0.5078 0.078 Uiso 0.695(17) 1 calc R . P B 1 H12A H 0.6190 0.7413 0.5118 0.078 Uiso 0.305(17) 1 calc R . P B 2 C22 C 0.7078(5) 0.5594(2) 0.3313(4) 0.0863(11) Uani 1 1 d . . . . . C23 C 0.7624(5) 0.5228(2) 0.4266(4) 0.0944(13) Uani 1 1 d . . . . . C24 C 0.7467(7) 0.5481(4) 0.5276(4) 0.139(2) Uani 1 1 d . . . . . H24A H 0.7060 0.5101 0.5573 0.208 Uiso 1 1 calc GR . . . . H24B H 0.6822 0.5891 0.5135 0.208 Uiso 1 1 calc GR . . . . H24C H 0.8418 0.5614 0.5769 0.208 Uiso 1 1 calc GR . . . . C25 C 0.7283(5) 0.5280(2) 0.2406(4) 0.0878(12) Uani 1 1 d . . . . . C26 C 0.6601(6) 0.5626(3) 0.1319(4) 0.1078(15) Uani 1 1 d . . . . . H26A H 0.7337 0.5672 0.0994 0.162 Uiso 1 1 calc GR . . . . H26B H 0.6227 0.6094 0.1395 0.162 Uiso 1 1 calc GR . . . . H26C H 0.5807 0.5330 0.0882 0.162 Uiso 1 1 calc GR . . . . N2 N 0.5992(19) 0.8383(5) 0.4291(9) 0.0661(17) Uani 0.695(17) 1 d D . P B 1 C11 C 0.5766(16) 0.8232(5) 0.3281(8) 0.0610(19) Uani 0.695(17) 1 d D . P B 1 H11 H 0.6245 0.8537 0.2958 0.073 Uiso 0.695(17) 1 calc R . P B 1 C13 C 0.6581(13) 0.8999(5) 0.4957(8) 0.077(2) Uani 0.695(17) 1 d D . P B 1 H13A H 0.6205 0.9446 0.4587 0.092 Uiso 0.695(17) 1 calc R . P B 1 H13B H 0.7651 0.9005 0.5201 0.092 Uiso 0.695(17) 1 calc R . P B 1 C14 C 0.6042(11) 0.8885(4) 0.5840(6) 0.0799(17) Uani 0.695(17) 1 d D U P B 1 C19 C 0.6173(9) 0.9346(4) 0.6682(7) 0.092(2) Uani 0.695(17) 1 d G U P B 1 H19 H 0.6604 0.9797 0.6710 0.110 Uiso 0.695(17) 1 calc R . P B 1 C18 C 0.5658(9) 0.9134(5) 0.7482(6) 0.099(3) Uani 0.695(17) 1 d G U P B 1 H18 H 0.5746 0.9442 0.8046 0.119 Uiso 0.695(17) 1 calc R . P B 1 C17 C 0.5013(9) 0.8460(5) 0.7441(5) 0.089(2) Uani 0.695(17) 1 d G U P B 1 H17 H 0.4669 0.8318 0.7976 0.106 Uiso 0.695(17) 1 calc R . P B 1 C16 C 0.4882(10) 0.7999(4) 0.6599(5) 0.0735(16) Uani 0.695(17) 1 d G U P B 1 H16 H 0.4450 0.7549 0.6571 0.088 Uiso 0.695(17) 1 calc R . P B 1 C15 C 0.5397(11) 0.8212(4) 0.5798(5) 0.0654(15) Uani 0.695(17) 1 d G U P B 1 C20 C 0.5065(5) 0.6428(2) 0.3289(3) 0.0573(10) Uani 0.808(6) 1 d . . P A 1 H20 H 0.4588 0.6035 0.3454 0.069 Uiso 0.808(6) 1 calc R . P A 1 C21 C 0.6360(5) 0.6315(2) 0.3219(4) 0.0680(11) Uani 0.808(6) 1 d . . P A 1 H21 H 0.6873 0.6711 0.3103 0.082 Uiso 0.808(6) 1 calc R . P A 1 N2A N 0.607(5) 0.8248(12) 0.415(2) 0.0661(17) Uani 0.305(17) 1 d D . P B 2 C11A C 0.568(4) 0.8351(12) 0.308(2) 0.0610(19) Uani 0.305(17) 1 d D . P B 2 H11A H 0.5856 0.8750 0.2718 0.073 Uiso 0.305(17) 1 calc R . P B 2 C13A C 0.663(4) 0.8986(13) 0.4600(17) 0.077(2) Uani 0.305(17) 1 d D . P B 2 H13C H 0.6109 0.9369 0.4126 0.092 Uiso 0.305(17) 1 calc R . P B 2 H13D H 0.7678 0.9034 0.4750 0.092 Uiso 0.305(17) 1 calc R . P B 2 C19A C 0.636(2) 0.9517(8) 0.6371(15) 0.092(2) Uani 0.305(17) 1 d . . P B 2 H19A H 0.6752 0.9964 0.6298 0.110 Uiso 0.305(17) 1 calc R . P B 2 C18A C 0.589(2) 0.9390(9) 0.7222(13) 0.099(3) Uani 0.305(17) 1 d G . P B 2 H18A H 0.5967 0.9751 0.7717 0.119 Uiso 0.305(17) 1 calc R . P B 2 C17A C 0.531(2) 0.8722(10) 0.7332(12) 0.089(2) Uani 0.305(17) 1 d G . P B 2 H17A H 0.4997 0.8637 0.7901 0.106 Uiso 0.305(17) 1 calc R . P B 2 C16A C 0.520(2) 0.8183(9) 0.6592(15) 0.0735(16) Uani 0.305(17) 1 d G . P B 2 H16A H 0.4812 0.7736 0.6666 0.088 Uiso 0.305(17) 1 calc R . P B 2 C15A C 0.567(3) 0.8311(9) 0.5742(15) 0.0654(15) Uani 0.305(17) 1 d DG . P B 2 C14A C 0.625(3) 0.8978(10) 0.5631(14) 0.0799(17) Uani 0.305(17) 1 d DG . P B 2 C20A C 0.578(2) 0.6567(11) 0.3555(17) 0.0573(10) Uani 0.192(6) 1 d . . P A 2 H20A H 0.6662 0.6687 0.4089 0.069 Uiso 0.192(6) 1 calc R . P A 2 C21A C 0.556(2) 0.5954(10) 0.3064(16) 0.0680(11) Uani 0.192(6) 1 d . . P A 2 H21A H 0.4659 0.5766 0.2639 0.082 Uiso 0.192(6) 1 calc R . 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 0.0997(18) 0.0812(18) 0.0814(16) 0.0209(14) 0.0346(14) 0.0035(16) O2 0.143(3) 0.095(2) 0.114(2) 0.0090(18) 0.087(2) -0.0129(19) O3 0.0940(18) 0.110(2) 0.0724(16) -0.0069(16) 0.0378(14) -0.0103(17) O4 0.0896(19) 0.0756(18) 0.146(3) 0.0277(19) 0.039(2) 0.0221(16) O5 0.0960(19) 0.0646(16) 0.144(3) -0.0094(16) 0.0482(18) 0.0176(15) N1 0.0717(18) 0.120(3) 0.0656(17) 0.0155(18) 0.0299(14) -0.0090(18) N3 0.0745(17) 0.081(2) 0.0778(19) 0.0098(17) 0.0424(15) 0.0072(16) C1 0.0670(19) 0.073(2) 0.075(2) -0.0015(18) 0.0235(16) 0.0147(18) C2 0.081(3) 0.099(3) 0.097(3) -0.004(2) 0.019(2) 0.031(2) C3 0.066(2) 0.171(5) 0.095(3) -0.007(3) 0.029(2) 0.039(3) C4 0.067(2) 0.178(5) 0.078(2) 0.006(3) 0.0366(19) 0.018(3) C5 0.0595(18) 0.115(3) 0.0509(17) -0.0045(19) 0.0205(14) 0.0023(19) C6 0.0548(15) 0.073(2) 0.0520(15) -0.0093(15) 0.0172(12) 0.0039(15) C7 0.0570(16) 0.0557(17) 0.0594(16) 0.0007(14) 0.0230(13) 0.0032(14) C8 0.073(2) 0.075(2) 0.0532(17) 0.0018(16) 0.0223(14) -0.0085(18) C9 0.0561(15) 0.0576(18) 0.0635(17) 0.0034(14) 0.0248(13) 0.0015(14) C10 0.0555(16) 0.0605(18) 0.0681(19) 0.0066(15) 0.0276(14) 0.0065(15) C12 0.0547(16) 0.0603(19) 0.073(2) 0.0076(16) 0.0136(14) 0.0074(14) C22 0.081(2) 0.072(2) 0.110(3) 0.006(2) 0.038(2) 0.023(2) C23 0.084(3) 0.081(3) 0.120(3) 0.019(3) 0.038(2) 0.018(2) C24 0.145(5) 0.158(6) 0.111(4) 0.041(4) 0.040(3) 0.066(4) C25 0.077(2) 0.069(2) 0.118(3) -0.008(2) 0.036(2) 0.007(2) C26 0.115(4) 0.099(3) 0.107(3) 0.000(3) 0.036(3) 0.027(3) N2 0.059(2) 0.052(4) 0.080(3) -0.005(2) 0.016(2) -0.002(4) C11 0.052(2) 0.057(4) 0.074(5) 0.032(3) 0.023(3) 0.008(3) C13 0.087(3) 0.069(2) 0.061(6) -0.005(4) 0.007(5) -0.011(2) C14 0.067(3) 0.071(3) 0.085(4) -0.009(3) 0.005(2) 0.007(2) C19 0.093(4) 0.069(4) 0.094(5) -0.015(4) 0.009(3) 0.000(3) C18 0.096(4) 0.087(6) 0.095(5) -0.027(4) 0.009(3) 0.010(4) C17 0.082(4) 0.095(5) 0.074(3) -0.012(3) 0.009(2) 0.014(4) C16 0.061(4) 0.079(4) 0.067(2) -0.013(3) 0.005(2) 0.001(3) C15 0.047(4) 0.066(3) 0.071(2) -0.005(2) 0.0056(19) 0.004(2) C20 0.055(3) 0.054(2) 0.064(2) 0.0010(18) 0.023(2) -0.005(2) C21 0.065(3) 0.053(2) 0.093(3) 0.000(2) 0.035(2) -0.0023(19) N2A 0.059(2) 0.052(4) 0.080(3) -0.005(2) 0.016(2) -0.002(4) C11A 0.052(2) 0.057(4) 0.074(5) 0.032(3) 0.023(3) 0.008(3) C13A 0.087(3) 0.069(2) 0.061(6) -0.005(4) 0.007(5) -0.011(2) C19A 0.093(4) 0.069(4) 0.094(5) -0.015(4) 0.009(3) 0.000(3) C18A 0.096(4) 0.087(6) 0.095(5) -0.027(4) 0.009(3) 0.010(4) C17A 0.082(4) 0.095(5) 0.074(3) -0.012(3) 0.009(2) 0.014(4) C16A 0.061(4) 0.079(4) 0.067(2) -0.013(3) 0.005(2) 0.001(3) C15A 0.047(4) 0.066(3) 0.071(2) -0.005(2) 0.0056(19) 0.004(2) C14A 0.067(3) 0.071(3) 0.085(4) -0.009(3) 0.005(2) 0.007(2) C20A 0.055(3) 0.054(2) 0.064(2) 0.0010(18) 0.023(2) -0.005(2) C21A 0.065(3) 0.053(2) 0.093(3) 0.000(2) 0.035(2) -0.0023(19) 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 C23 O4 H4 109.5 . . ? C5 N1 H1 123.7 . . ? C8 N1 H1 123.7 . . ? C8 N1 C5 112.6(3) . . ? O2 N3 C10 119.2(3) . . ? O3 N3 O2 122.0(3) . . ? O3 N3 C10 118.9(3) . . ? C2 C1 H1A 120.7 . . ? C6 C1 H1A 120.7 . . ? C6 C1 C2 118.6(4) . . ? C1 C2 H2 119.7 . . ? C3 C2 C1 120.7(4) . . ? C3 C2 H2 119.7 . . ? C2 C3 H3 119.4 . . ? C2 C3 C4 121.3(4) . . ? C4 C3 H3 119.4 . . ? C3 C4 H4A 120.9 . . ? C5 C4 C3 118.2(4) . . ? C5 C4 H4A 120.9 . . ? C4 C5 N1 128.5(4) . . ? C4 C5 C6 122.2(4) . . ? C6 C5 N1 109.3(3) . . ? C1 C6 C5 119.1(3) . . ? C1 C6 C7 132.5(3) . . ? C5 C6 C7 108.3(3) . . ? C6 C7 C8 102.3(3) . . ? C6 C7 C9 112.0(2) . . ? C6 C7 C12 114.9(3) . . ? C8 C7 C9 112.6(3) . . ? C8 C7 C12 107.1(3) . . ? C12 C7 C9 107.8(2) . . ? O1 C8 N1 126.5(3) . . ? O1 C8 C7 125.8(3) . . ? N1 C8 C7 107.6(3) . . ? C7 C9 H9A 106.0 . . ? C7 C9 H9B 113.8 . . ? C7 C9 C20A 108.4(7) . . ? C10 C9 C7 107.7(3) . . ? C10 C9 H9A 106.0 . . ? C10 C9 H9B 113.8 . . ? C10 C9 C20A 97.9(7) . . ? C20 C9 C7 115.8(3) . . ? C20 C9 H9A 106.0 . . ? C20 C9 C10 114.5(3) . . ? C20A C9 H9B 113.8 . . ? N3 C10 C9 118.1(3) . . ? C11 C10 N3 122.1(6) . . ? C11 C10 C9 119.8(6) . . ? C11A C10 N3 109.2(12) . . ? C11A C10 C9 132.2(13) . . ? C7 C12 H12 109.5 . . ? C7 C12 H12A 106.9 . . ? N2 C12 C7 111.9(6) . . ? N2 C12 H12 109.5 . . ? N2 C12 C15 101.3(4) . . ? C15 C12 C7 114.8(4) . . ? C15 C12 H12 109.5 . . ? N2A C12 C7 107.1(14) . . ? N2A C12 H12A 106.9 . . ? N2A C12 C15A 101.7(11) . . ? C15A C12 C7 126.0(9) . . ? C15A C12 H12A 106.9 . . ? C23 C22 C25 118.1(4) . . ? C23 C22 C21 122.3(4) . . ? C23 C22 C21A 116.3(8) . . ? C25 C22 C21 119.5(4) . . ? C25 C22 C21A 113.3(8) . . ? O4 C23 C22 122.4(5) . . ? O4 C23 C24 113.3(4) . . ? C22 C23 C24 124.2(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O5 C25 C22 122.8(4) . . ? O5 C25 C26 116.7(4) . . ? C22 C25 C26 120.4(4) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C11 N2 C12 113.3(9) . . ? C11 N2 C13 133.8(9) . . ? C13 N2 C12 113.0(6) . . ? C10 C11 N2 130.7(11) . . ? C10 C11 H11 114.7 . . ? N2 C11 H11 114.7 . . ? N2 C13 H13A 111.3 . . ? N2 C13 H13B 111.3 . . ? N2 C13 C14 102.3(6) . . ? H13A C13 H13B 109.2 . . ? C14 C13 H13A 111.3 . . ? C14 C13 H13B 111.3 . . ? C19 C14 C13 127.8(4) . . ? C19 C14 C15 120.0 . . ? C15 C14 C13 112.2(4) . . ? C14 C19 H19 120.0 . . ? C14 C19 C18 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C18 H18 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C17 H17 120.0 . . ? C18 C17 C16 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C16 H16 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C14 C15 C12 108.7(4) . . ? C16 C15 C12 131.2(4) . . ? C16 C15 C14 120.0 . . ? C9 C20 H20 117.3 . . ? C21 C20 C9 125.4(4) . . ? C21 C20 H20 117.3 . . ? C22 C21 H21 117.7 . . ? C20 C21 C22 124.6(4) . . ? C20 C21 H21 117.7 . . ? C12 N2A C13A 113.7(13) . . ? C11A N2A C12 136(3) . . ? C11A N2A C13A 103.0(18) . . ? C10 C11A H11A 128.6 . . ? N2A C11A C10 102.9(19) . . ? N2A C11A H11A 128.6 . . ? N2A C13A H13C 111.6 . . ? N2A C13A H13D 111.6 . . ? N2A C13A C14A 100.9(11) . . ? H13C C13A H13D 109.4 . . ? C14A C13A H13C 111.6 . . ? C14A C13A H13D 111.6 . . ? C18A C19A H19A 120.0 . . ? C18A C19A C14A 120.0 . . ? C14A C19A H19A 120.0 . . ? C19A C18A H18A 120.0 . . ? C17A C18A C19A 120.0 . . ? C17A C18A H18A 120.0 . . ? C18A C17A H17A 120.0 . . ? C18A C17A C16A 120.0 . . ? C16A C17A H17A 120.0 . . ? C17A C16A H16A 120.0 . . ? C15A C16A C17A 120.0 . . ? C15A C16A H16A 120.0 . . ? C16A C15A C12 125.6(10) . . ? C16A C15A C14A 120.0 . . ? C14A C15A C12 114.2(10) . . ? C19A C14A C13A 130.5(10) . . ? C15A C14A C13A 109.4(10) . . ? C15A C14A C19A 120.0 . . ? C9 C20A H20A 123.1 . . ? C21A C20A C9 113.7(18) . . ? C21A C20A H20A 123.1 . . ? C22 C21A H21A 126.3 . . ? C20A C21A C22 107.3(18) . . ? C20A C21A H21A 126.3 . . ? 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 C8 1.221(4) . ? O2 N3 1.252(4) . ? O3 N3 1.239(4) . ? O4 H4 0.8200 . ? O4 C23 1.309(5) . ? O5 C25 1.258(5) . ? N1 H1 0.8600 . ? N1 C5 1.394(5) . ? N1 C8 1.349(5) . ? N3 C10 1.414(4) . ? C1 H1A 0.9300 . ? C1 C2 1.395(5) . ? C1 C6 1.380(5) . ? C2 H2 0.9300 . ? C2 C3 1.362(7) . ? C3 H3 0.9300 . ? C3 C4 1.372(8) . ? C4 H4A 0.9300 . ? C4 C5 1.361(5) . ? C5 C6 1.391(5) . ? C6 C7 1.513(4) . ? C7 C8 1.533(5) . ? C7 C9 1.568(4) . ? C7 C12 1.554(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 C10 1.513(4) . ? C9 C20 1.503(5) . ? C9 C20A 1.73(2) . ? C10 C11 1.317(9) . ? C10 C11A 1.371(19) . ? C12 H12 0.9800 . ? C12 H12A 0.9800 . ? C12 N2 1.474(9) . ? C12 C15 1.518(6) . ? C12 N2A 1.487(18) . ? C12 C15A 1.489(12) . ? C22 C23 1.384(6) . ? C22 C25 1.425(6) . ? C22 C21 1.493(6) . ? C22 C21A 1.536(19) . ? C23 C24 1.493(7) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.522(6) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? N2 C11 1.328(9) . ? N2 C13 1.443(9) . ? C11 H11 0.9300 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.469(8) . ? C14 C19 1.3900 . ? C14 C15 1.3900 . ? C19 H19 0.9300 . ? C19 C18 1.3900 . ? C18 H18 0.9300 . ? C18 C17 1.3900 . ? C17 H17 0.9300 . ? C17 C16 1.3900 . ? C16 H16 0.9300 . ? C16 C15 1.3900 . ? C20 H20 0.9300 . ? C20 C21 1.304(7) . ? C21 H21 0.9300 . ? N2A C11A 1.370(18) . ? N2A C13A 1.520(18) . ? C11A H11A 0.9300 . ? C13A H13C 0.9700 . ? C13A H13D 0.9700 . ? C13A C14A 1.550(14) . ? C19A H19A 0.9300 . ? C19A C18A 1.3900 . ? C19A C14A 1.3900 . ? C18A H18A 0.9300 . ? C18A C17A 1.3900 . ? C17A H17A 0.9300 . ? C17A C16A 1.3900 . ? C16A H16A 0.9300 . ? C16A C15A 1.3900 . ? C15A C14A 1.3900 . ? C20A H20A 0.9300 . ? C20A C21A 1.30(3) . ? C21A H21A 0.9300 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O5 0.82 1.76 2.486(5) 146.8 . N1 H1 O2 0.86 2.28 3.039(4) 147.1 4_576 N1 H1 O4 0.86 2.78 3.450(5) 135.5 3_666 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 O2 N3 C10 C9 -177.9(3) . . . . ? O2 N3 C10 C11 2.0(9) . . . . ? O2 N3 C10 C11A 9.2(18) . . . . ? O3 N3 C10 C9 2.5(4) . . . . ? O3 N3 C10 C11 -177.7(8) . . . . ? O3 N3 C10 C11A -170.5(18) . . . . ? N1 C5 C6 C1 176.6(3) . . . . ? N1 C5 C6 C7 0.5(4) . . . . ? N3 C10 C11 N2 173.3(15) . . . . ? N3 C10 C11A N2A -169(3) . . . . ? C1 C2 C3 C4 -1.1(8) . . . . ? C1 C6 C7 C8 -175.5(3) . . . . ? C1 C6 C7 C9 -54.7(5) . . . . ? C1 C6 C7 C12 68.8(5) . . . . ? C2 C1 C6 C5 0.2(5) . . . . ? C2 C1 C6 C7 175.3(4) . . . . ? C2 C3 C4 C5 0.3(8) . . . . ? C3 C4 C5 N1 -176.4(4) . . . . ? C3 C4 C5 C6 0.8(7) . . . . ? C4 C5 C6 C1 -1.0(6) . . . . ? C4 C5 C6 C7 -177.2(4) . . . . ? C5 N1 C8 O1 176.3(3) . . . . ? C5 N1 C8 C7 0.7(4) . . . . ? C5 C6 C7 C8 -0.1(3) . . . . ? C5 C6 C7 C9 120.8(3) . . . . ? C5 C6 C7 C12 -115.8(3) . . . . ? C6 C1 C2 C3 0.8(6) . . . . ? C6 C7 C8 O1 -176.0(3) . . . . ? C6 C7 C8 N1 -0.3(3) . . . . ? C6 C7 C9 C10 76.3(3) . . . . ? C6 C7 C9 C20 -154.0(3) . . . . ? C6 C7 C9 C20A -178.8(8) . . . . ? C6 C7 C12 N2 -65.9(6) . . . . ? C6 C7 C12 C15 48.9(5) . . . . ? C6 C7 C12 N2A -78.9(13) . . . . ? C6 C7 C12 C15A 40.2(11) . . . . ? C7 C9 C10 N3 -153.1(3) . . . . ? C7 C9 C10 C11 27.1(8) . . . . ? C7 C9 C10 C11A 18(2) . . . . ? C7 C9 C20 C21 -115.5(5) . . . . ? C7 C9 C20A C21A 133.7(15) . . . . ? C7 C12 N2 C11 -39.0(16) . . . . ? C7 C12 N2 C13 139.1(11) . . . . ? C7 C12 C15 C14 -130.8(4) . . . . ? C7 C12 C15 C16 53.5(8) . . . . ? C7 C12 N2A C11A -7(5) . . . . ? C7 C12 N2A C13A 135(3) . . . . ? C7 C12 C15A C16A 53.7(19) . . . . ? C7 C12 C15A C14A -120.6(10) . . . . ? C8 N1 C5 C4 176.7(4) . . . . ? C8 N1 C5 C6 -0.8(4) . . . . ? C8 C7 C9 C10 -169.0(3) . . . . ? C8 C7 C9 C20 -39.3(4) . . . . ? C8 C7 C9 C20A -64.1(8) . . . . ? C8 C7 C12 N2 -178.8(6) . . . . ? C8 C7 C12 C15 -64.0(5) . . . . ? C8 C7 C12 N2A 168.2(13) . . . . ? C8 C7 C12 C15A -72.6(11) . . . . ? C9 C7 C8 O1 63.5(4) . . . . ? C9 C7 C8 N1 -120.8(3) . . . . ? C9 C7 C12 N2 59.7(6) . . . . ? C9 C7 C12 C15 174.5(4) . . . . ? C9 C7 C12 N2A 46.8(13) . . . . ? C9 C7 C12 C15A 165.9(11) . . . . ? C9 C10 C11 N2 -7(2) . . . . ? C9 C10 C11A N2A 19(4) . . . . ? C9 C20 C21 C22 -175.6(4) . . . . ? C9 C20A C21A C22 165.4(11) . . . . ? C10 C9 C20 C21 10.8(6) . . . . ? C10 C9 C20A C21A -114.6(16) . . . . ? C12 C7 C8 O1 -54.8(4) . . . . ? C12 C7 C8 N1 120.8(3) . . . . ? C12 C7 C9 C10 -51.1(3) . . . . ? C12 C7 C9 C20 78.6(4) . . . . ? C12 C7 C9 C20A 53.9(8) . . . . ? C12 N2 C11 C10 12(3) . . . . ? C12 N2 C13 C14 -15.9(16) . . . . ? C12 N2A C11A C10 -26(6) . . . . ? C12 N2A C13A C14A -3(4) . . . . ? C12 C15A C14A C13A -3.0(19) . . . . ? C12 C15A C14A C19A 174.7(18) . . . . ? C23 C22 C25 O5 -5.0(7) . . . . ? C23 C22 C25 C26 175.1(4) . . . . ? C23 C22 C21 C20 -71.2(7) . . . . ? C23 C22 C21A C20A 82.2(16) . . . . ? C25 C22 C23 O4 2.6(7) . . . . ? C25 C22 C23 C24 -178.7(5) . . . . ? C25 C22 C21 C20 112.1(6) . . . . ? C25 C22 C21A C20A -136.0(13) . . . . ? N2 C12 C15 C14 -9.9(8) . . . . ? N2 C12 C15 C16 174.3(9) . . . . ? N2 C13 C14 C19 -174.2(9) . . . . ? N2 C13 C14 C15 8.8(12) . . . . ? C11 N2 C13 C14 161.7(19) . . . . ? C13 N2 C11 C10 -165.3(14) . . . . ? C13 C14 C19 C18 -176.7(11) . . . . ? C13 C14 C15 C12 0.9(7) . . . . ? C13 C14 C15 C16 177.2(9) . . . . ? C14 C19 C18 C17 0.0 . . . . ? C19 C14 C15 C12 -176.3(7) . . . . ? C19 C14 C15 C16 0.0 . . . . ? C19 C18 C17 C16 0.0 . . . . ? C18 C17 C16 C15 0.0 . . . . ? C17 C16 C15 C12 175.4(9) . . . . ? C17 C16 C15 C14 0.0 . . . . ? C15 C12 N2 C11 -161.8(13) . . . . ? C15 C12 N2 C13 16.3(14) . . . . ? C15 C14 C19 C18 0.0 . . . . ? C20 C9 C10 N3 76.5(4) . . . . ? C20 C9 C10 C11 -103.3(8) . . . . ? C21 C22 C23 O4 -174.2(4) . . . . ? C21 C22 C23 C24 4.5(8) . . . . ? C21 C22 C25 O5 171.9(4) . . . . ? C21 C22 C25 C26 -8.0(6) . . . . ? N2A C12 C15A C16A 175(2) . . . . ? N2A C12 C15A C14A 1(2) . . . . ? N2A C13A C14A C19A -174(2) . . . . ? N2A C13A C14A C15A 4(3) . . . . ? C11A N2A C13A C14A 151(3) . . . . ? C13A N2A C11A C10 -171(3) . . . . ? C19A C18A C17A C16A 0.0 . . . . ? C18A C19A C14A C13A 177(3) . . . . ? C18A C19A C14A C15A 0.0 . . . . ? C18A C17A C16A C15A 0.0 . . . . ? C17A C16A C15A C12 -174(2) . . . . ? C17A C16A C15A C14A 0.0 . . . . ? C16A C15A C14A C13A -178(2) . . . . ? C16A C15A C14A C19A 0.0 . . . . ? C15A C12 N2A C11A -141(4) . . . . ? C15A C12 N2A C13A 2(4) . . . . ? C14A C19A C18A C17A 0.0 . . . . ? C20A C9 C10 N3 94.6(8) . . . . ? C20A C9 C10 C11A -94(2) . . . . ? C21A C22 C23 O4 142.5(9) . . . . ? C21A C22 C23 C24 -38.8(11) . . . . ? C21A C22 C25 O5 -146.0(9) . . . . ? C21A C22 C25 C26 34.1(10) . . . . ?