#------------------------------------------------------------------------------ #$Date: 2023-05-27 04:29:44 +0300 (Sat, 27 May 2023) $ #$Revision: 284037 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/68/7246846.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_7246846 loop_ _publ_author_name 'Bao, Xiaobo' 'Yu, Wei' 'Wang, Lilin' 'Dong, Xu' 'Wang, Guoli' 'Chen, Weilin' 'Li, Fei' 'Chen, Dongyin' _publ_section_title ; Synthesis of 4-aryl-3,4-dihydrocoumarins and 4-aryl-4H-chromenes via Er(OTf)3-catalyzed cascade reactions of p-quinone methides with 1,3-dicarbonyl compounds ; _journal_issue 23 _journal_name_full 'RSC Advances' _journal_page_first 15942 _journal_page_last 15946 _journal_paper_doi 10.1039/D3RA02267F _journal_volume 13 _journal_year 2023 _chemical_formula_moiety 'C32 H42 O4' _chemical_formula_sum 'C32 H42 O4' _chemical_formula_weight 490.65 _chemical_name_systematic 1 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_block_doi 10.5517/ccdc.csd.cc2fgfkx _audit_creation_date 2023-03-12 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2023-03-13 deposited with the CCDC. 2023-05-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.3630(10) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 18.6928(2) _cell_length_b 14.67570(10) _cell_length_c 21.8092(3) _cell_measurement_reflns_used 16469 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 68.0150 _cell_measurement_theta_min 2.0260 _cell_volume 5903.21(11) _computing_cell_refinement 'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.994 _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 18.00 123.00 0.50 0.50 -- 42.00 65.00 0.00 210 2 \w 74.00 111.00 0.50 0.50 -- 42.00 82.00 -60.00 74 3 \w 29.00 66.00 0.50 0.50 -- 42.00 -82.00 -90.00 74 4 \w -47.00 -5.00 0.50 0.50 -- 42.00 -82.00 120.00 84 5 \w 43.00 85.00 0.50 0.50 -- 42.00 -21.00 90.00 84 6 \w 17.00 65.00 0.50 0.50 -- 42.00 82.00 -60.00 96 7 \w -47.00 -5.00 0.50 0.50 -- 42.00 -21.00 90.00 84 8 \w -42.00 64.00 0.50 0.50 -- 42.00 -82.00 90.00 212 9 \w 3.00 69.00 0.50 0.50 -- 42.00 -82.00-180.00 132 10 \w 10.00 68.00 0.50 0.50 -- 42.00 -82.00 120.00 116 11 \w -47.00 -20.00 0.50 0.50 -- 42.00 -82.00 -60.00 54 12 \w -15.00 29.00 0.50 0.50 -- 42.00 -82.00 -60.00 88 13 \w 23.00 63.00 0.50 0.50 -- 42.00 -65.00-180.00 80 14 \w -32.00 -6.00 0.50 0.50 -- 42.00 -65.00-180.00 52 15 \w -23.00 66.00 0.50 0.50 -- 42.00 -77.00 30.00 178 16 \w -1.00 30.00 0.50 0.50 -- 42.00 -21.00 90.00 62 17 \w -28.00 -3.00 0.50 0.50 -- 42.00 -82.00 -30.00 50 18 \w 40.00 65.00 0.50 0.50 -- 42.00 65.00-150.00 50 19 \w 41.00 69.00 0.50 0.50 -- 42.00 -82.00 -30.00 56 20 \w 91.00 130.00 0.50 0.50 -- 42.00 -21.00 90.00 78 21 \w 4.00 108.00 0.50 0.50 -- 93.70 -59.00 90.00 208 22 \w 4.00 109.00 0.50 0.50 -- 93.70 -59.00 -90.00 210 23 \w 4.00 69.00 0.50 0.50 -- 93.70 -33.00 -90.00 130 24 \w 26.00 120.00 0.50 0.50 -- 93.70 -82.00 90.00 188 25 \w 59.00 99.00 0.50 0.50 -- 93.70 -82.00 -30.00 80 26 \w 41.00 90.00 0.50 0.50 -- 93.70 -82.00-180.00 98 27 \w 4.00 104.00 0.50 0.50 -- 93.70 -82.00 30.00 200 28 \w 19.00 60.00 0.50 0.50 -- 93.70 -33.00 -60.00 82 29 \w 67.00 126.00 0.50 0.50 -- 93.70 -33.00 -60.00 118 30 \w 71.00 102.00 0.50 0.50 -- 93.70 -82.00 120.00 62 31 \w 65.00 90.00 0.50 0.50 -- 93.70 -82.00 150.00 50 32 \w 118.00 144.00 0.50 0.50 -- 93.70 68.00-180.00 52 33 \w 34.00 104.00 0.50 0.50 -- 93.70 -82.00-150.00 140 34 \w 4.00 105.00 0.50 0.50 -- 93.70 -82.00 -90.00 202 35 \w 70.00 96.00 0.50 0.50 -- 93.70 -82.00 0.00 52 36 \w 75.00 100.00 0.50 0.50 -- 93.70 -82.00 60.00 50 37 \w 5.00 63.00 0.50 0.50 -- 93.70 -82.00 60.00 116 38 \w 63.00 88.00 0.50 0.50 -- 93.70 -82.00-120.00 50 39 \w 12.00 57.00 0.50 0.50 -- 93.70 -77.00-120.00 90 40 \w 4.00 182.00 0.50 0.50 -- 93.70 0.00 0.00 356 41 \w 12.00 38.00 0.50 0.50 -- 93.70 -82.00-120.00 52 42 \w 91.00 135.00 0.50 0.50 -- 93.70 33.00-180.00 88 43 \w 8.00 121.00 0.50 0.50 -- 93.70 -33.00 90.00 226 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Pro II AFC12 (RINC): Kappa single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0574128000 _diffrn_orient_matrix_UB_12 0.0561333000 _diffrn_orient_matrix_UB_13 -0.0266782000 _diffrn_orient_matrix_UB_21 0.0452621000 _diffrn_orient_matrix_UB_22 0.0075266000 _diffrn_orient_matrix_UB_23 0.0654280000 _diffrn_orient_matrix_UB_31 0.0403569000 _diffrn_orient_matrix_UB_32 -0.0884416000 _diffrn_orient_matrix_UB_33 -0.0113969000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_unetI/netI 0.0181 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 28471 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.115 _diffrn_reflns_theta_min 3.849 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.558 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.34916 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dull greenish green' _exptl_crystal_colour_lustre dull _exptl_crystal_colour_modifier greenish _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.104 _exptl_crystal_description block _exptl_crystal_F_000 2128 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.289 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.033 _refine_ls_extinction_coef 0.00135(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 334 _refine_ls_number_reflns 5373 _refine_ls_number_restraints 495 _refine_ls_restrained_S_all 1.413 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0530 _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^)+(0.0725P)^2^+2.9105P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1516 _refine_ls_wR_factor_ref 0.1558 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4691 _reflns_number_total 5373 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ra02267f2.cif _cod_data_source_block mzl_auto _cod_database_code 7246846 _shelx_shelxl_version_number 2018/3 _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 0.978 _shelx_estimated_absorpt_t_min 0.967 _diffrn_oxdiff_digest_frames ; 01c30b2523971ee83ec29f7799c1c8522700029b493 ; _diffrn_oxdiff_digest_hkl ; 01377fb9a0c05181699eb3a735108a66bfcc41 ; _reflns_odcompleteness_completeness 99.96 _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, All O(H) groups 2. Restrained distances H1-H8A 2 with sigma of 0.002 H1-H10C 2 with sigma of 0.002 3. Rigid bond restraints C2, C3 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 4. Uiso/Uaniso restraints and constraints C13 \\sim C7 \\sim C25 \\sim C12 \\sim C15 \\sim C24 \\sim C6 \\sim C26 \\sim C16 \\sim C14 \\sim C5 \\sim C9 \\sim C27 \\sim C21 \\sim C23 \\sim C10 \\sim C17 \\sim C2 \\sim C32 \\sim C28 \\sim C8 \\sim C20 \\sim C19 \\sim C18 \\sim C11 \\sim C29 \\sim C31 \\sim C30 \\sim C3 \\sim C22 \\sim C1 \\sim C4: within 2.7A with sigma of 0.004 and sigma for terminal atoms of 0.008 5.a Ternary CH refined with riding coordinates: C15(H15), C27(H27) 5.b Secondary CH2 refined with riding coordinates: C23(H23A,H23B), C32(H32A,H32B), C28(H28A,H28B), C29(H29A,H29B), C31(H31A, H31B), C30(H30A,H30B) 5.c Aromatic/amide H refined with riding coordinates: C12(H12), C14(H14), C17(H17), C20(H20), C19(H19), C18(H18) 5.d Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C3(H3A,H3B,H3C), C22(H22A,H22B,H22C), C1(H1A,H1B,H1C), C4(H4A,H4B,H4C) 5.e Idealised tetrahedral OH refined as rotating group: O1(H1) ; _shelx_res_file ; TITL mzl_auto_a.res in C2/c mzl_auto.res created by SHELXL-2018/3 at 19:57:40 on 12-Mar-2023 REM Old TITL MZL_auto in C2/c REM SHELXT solution in C2/c REM R1 0.210, Rweak 0.100, Alpha 0.035, Orientation as input REM Formula found by SHELXT: C1 C7 O4 CELL 1.54184 18.6928 14.6757 21.8092 90 99.363 90 ZERR 8 0.0002 0.0001 0.0003 0 0.001 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H O UNIT 256 336 32 DFIX 2 0.002 H1 H8a DFIX 2 0.002 H1 H10c DELU 0.001 0.001 C2 C3 SIMU 0.004 0.008 2.7 $C L.S. 40 PLAN 8 SIZE 0.05 0.06 0.04 MORE -1 BOND $H CONF fmap 2 acta REM REM REM WGHT 0.072500 2.910500 EXTI 0.001353 FVAR 0.30672 O2 3 0.187453 0.296722 0.408209 11.00000 0.05163 0.06513 = 0.05802 -0.00377 0.00994 0.00285 O1 3 0.255920 0.639203 0.278210 11.00000 0.08536 0.06404 = 0.05593 0.01575 0.02011 0.01193 AFIX 147 H1 2 0.266274 0.623265 0.244697 11.00000 -1.50000 AFIX 0 O3 3 0.232296 0.193352 0.350100 11.00000 0.06040 0.08080 = 0.07164 -0.02571 -0.01175 0.01462 O4 3 0.433975 0.232771 0.471366 11.00000 0.05478 0.07422 = 0.08671 -0.00889 -0.01564 -0.00516 C13 1 0.300801 0.437322 0.412529 11.00000 0.05926 0.04965 = 0.04294 0.00067 0.00720 -0.00784 C7 1 0.317711 0.496763 0.311666 11.00000 0.04849 0.05655 = 0.04466 0.00288 0.00772 -0.00483 C25 1 0.311210 0.269404 0.432368 11.00000 0.05305 0.05142 = 0.04151 0.00541 0.00480 -0.00576 C12 1 0.330583 0.431810 0.358645 11.00000 0.05191 0.05443 = 0.04544 0.00235 0.00725 -0.00357 AFIX 43 H12 2 0.360467 0.382648 0.353579 11.00000 -1.20000 AFIX 0 C15 1 0.315899 0.363018 0.462238 11.00000 0.06275 0.05513 = 0.04204 0.00263 0.00787 -0.00858 AFIX 13 H15 2 0.278597 0.366956 0.488927 11.00000 -1.20000 AFIX 0 C24 1 0.241664 0.246826 0.392567 11.00000 0.05084 0.05205 = 0.04646 0.00339 0.00681 0.00119 C6 1 0.272798 0.570368 0.320974 11.00000 0.05798 0.05097 = 0.04601 0.00506 0.00838 -0.00541 C26 1 0.367923 0.212062 0.436922 11.00000 0.05018 0.06009 = 0.05273 0.00622 -0.00161 -0.00521 C16 1 0.389421 0.376398 0.502657 11.00000 0.07553 0.06363 = 0.04052 0.00455 0.00217 -0.01993 C14 1 0.256996 0.510950 0.419807 11.00000 0.07194 0.05352 = 0.04552 -0.00172 0.01648 -0.00525 AFIX 43 H14 2 0.236949 0.515236 0.456032 11.00000 -1.20000 AFIX 0 C5 1 0.241592 0.578991 0.375220 11.00000 0.07138 0.05018 = 0.05018 -0.00155 0.01439 -0.00117 C9 1 0.351500 0.486523 0.252276 11.00000 0.05427 0.07205 = 0.04950 0.00834 0.01315 0.00448 C27 1 0.373009 0.120832 0.407627 11.00000 0.05056 0.06159 = 0.06011 0.00246 0.00119 0.00292 AFIX 13 H27 2 0.323889 0.102707 0.388742 11.00000 -1.20000 AFIX 0 C21 1 0.443767 0.313308 0.503803 11.00000 0.06815 0.07014 = 0.05344 0.00529 -0.00371 -0.01567 C23 1 0.118300 0.291822 0.367577 11.00000 0.04890 0.07933 = 0.07236 0.00031 0.00566 0.00776 AFIX 23 H23A 2 0.080321 0.312237 0.389810 11.00000 -1.20000 H23B 2 0.108245 0.229071 0.355092 11.00000 -1.20000 AFIX 0 C10 1 0.291818 0.475386 0.195134 11.00000 0.07612 0.08284 = 0.05087 -0.00292 0.00864 0.00370 AFIX 137 H10A 2 0.250439 0.446052 0.207348 11.00000 -1.50000 H10B 2 0.309835 0.438907 0.164438 11.00000 -1.50000 H10C 2 0.277977 0.534258 0.177999 11.00000 -1.50000 AFIX 0 C17 1 0.404968 0.454085 0.539084 11.00000 0.09602 0.07695 = 0.05351 -0.00388 -0.00123 -0.01763 AFIX 43 H17 2 0.369420 0.498175 0.539992 11.00000 -1.20000 AFIX 0 C2 1 0.193168 0.660646 0.384934 11.00000 0.10269 0.05752 = 0.06385 0.00052 0.02864 0.01055 C32 1 0.402467 0.047605 0.454859 11.00000 0.07431 0.06846 = 0.07149 0.00946 0.00987 0.00928 AFIX 23 H32A 2 0.450669 0.064558 0.475231 11.00000 -1.20000 H32B 2 0.371480 0.043057 0.486344 11.00000 -1.20000 AFIX 0 C28 1 0.418730 0.125712 0.356048 11.00000 0.08044 0.07979 = 0.07015 0.00612 0.01497 0.00265 AFIX 23 H28A 2 0.397310 0.169467 0.325077 11.00000 -1.20000 H28B 2 0.466936 0.147095 0.373217 11.00000 -1.20000 AFIX 0 C8 1 0.400517 0.568503 0.243995 11.00000 0.05651 0.10895 = 0.07022 0.02231 0.01755 -0.00687 AFIX 137 H8A 2 0.372577 0.623616 0.242080 11.00000 -1.50000 H8B 2 0.420047 0.561477 0.206191 11.00000 -1.50000 H8C 2 0.439469 0.571499 0.278553 11.00000 -1.50000 AFIX 0 C20 1 0.512423 0.325578 0.538698 11.00000 0.07533 0.08944 = 0.06521 0.00503 -0.00991 -0.02383 AFIX 43 H20 2 0.548195 0.281639 0.538305 11.00000 -1.20000 AFIX 0 C19 1 0.526648 0.402796 0.573487 11.00000 0.08840 0.09779 = 0.06445 0.00421 -0.01159 -0.02881 AFIX 43 H19 2 0.572463 0.411997 0.596575 11.00000 -1.20000 AFIX 0 C18 1 0.473943 0.466049 0.574353 11.00000 0.10687 0.08881 = 0.05717 -0.00814 -0.00695 -0.03291 AFIX 43 H18 2 0.483712 0.518026 0.598667 11.00000 -1.20000 AFIX 0 C11 1 0.398715 0.400702 0.254874 11.00000 0.08698 0.10584 = 0.06901 0.01417 0.03191 0.03236 AFIX 137 H11A 2 0.436039 0.403441 0.290703 11.00000 -1.50000 H11B 2 0.420477 0.397154 0.217994 11.00000 -1.50000 H11C 2 0.369182 0.347792 0.257550 11.00000 -1.50000 AFIX 0 C29 1 0.424656 0.034064 0.325037 11.00000 0.08456 0.09104 = 0.07918 -0.00524 0.02053 0.01045 AFIX 23 H29A 2 0.457973 0.039061 0.295434 11.00000 -1.20000 H29B 2 0.377559 0.016909 0.302391 11.00000 -1.20000 AFIX 0 C31 1 0.405597 -0.043992 0.423044 11.00000 0.08363 0.07012 = 0.08619 0.00686 0.00945 0.01575 AFIX 23 H31A 2 0.425625 -0.089160 0.453541 11.00000 -1.20000 H31B 2 0.356856 -0.062926 0.405440 11.00000 -1.20000 AFIX 0 C30 1 0.451296 -0.039589 0.372415 11.00000 0.07755 0.08422 = 0.09353 -0.00622 0.01138 0.02202 AFIX 23 H30A 2 0.449951 -0.098133 0.351614 11.00000 -1.20000 H30B 2 0.501202 -0.027133 0.390630 11.00000 -1.20000 AFIX 0 C3 1 0.126703 0.665256 0.333438 11.00000 0.09573 0.09704 = 0.08925 0.00930 0.02755 0.03196 AFIX 137 H3A 2 0.142154 0.677232 0.294339 11.00000 -1.50000 H3B 2 0.095100 0.713210 0.342525 11.00000 -1.50000 H3C 2 0.101279 0.608211 0.331240 11.00000 -1.50000 AFIX 0 C22 1 0.118051 0.349385 0.311271 11.00000 0.08134 0.11802 = 0.08996 0.02488 -0.00189 0.02216 AFIX 137 H22A 2 0.070335 0.349553 0.287033 11.00000 -1.50000 H22B 2 0.151945 0.325138 0.286846 11.00000 -1.50000 H22C 2 0.131714 0.410555 0.323655 11.00000 -1.50000 AFIX 0 C1 1 0.237464 0.748868 0.387259 11.00000 0.15399 0.05872 = 0.09696 -0.00694 0.02581 0.00281 AFIX 137 H1A 2 0.279445 0.743886 0.418919 11.00000 -1.50000 H1B 2 0.208214 0.799179 0.396581 11.00000 -1.50000 H1C 2 0.252469 0.758778 0.347733 11.00000 -1.50000 AFIX 0 C4 1 0.163562 0.652509 0.446385 11.00000 0.15582 0.08409 = 0.08292 0.00273 0.05386 0.03841 AFIX 137 H4A 2 0.137142 0.596475 0.446775 11.00000 -1.50000 H4B 2 0.131878 0.702901 0.450321 11.00000 -1.50000 H4C 2 0.203158 0.653065 0.480475 11.00000 -1.50000 AFIX 0 HKLF 4 REM mzl_auto_a.res in C2/c REM wR2 = 0.1558, GooF = S = 1.105, Restrained GooF = 1.413 for all data REM R1 = 0.0530 for 4691 Fo > 4sig(Fo) and 0.0577 for all 5373 data REM 334 parameters refined using 495 restraints END WGHT 0.0725 2.9105 REM Highest difference peak 0.289, deepest hole -0.183, 1-sigma level 0.033 Q1 1 0.2483 0.5263 0.1927 11.00000 0.05 0.29 Q2 1 0.4369 0.5034 0.5734 11.00000 0.05 0.27 Q3 1 0.2692 0.4021 0.1974 11.00000 0.05 0.24 Q4 1 0.3140 0.4870 0.1533 11.00000 0.05 0.24 Q5 1 0.2245 0.1652 0.3879 11.00000 0.05 0.19 Q6 1 0.2622 0.5794 0.3546 11.00000 0.05 0.18 Q7 1 0.4497 -0.0079 0.3431 11.00000 0.05 0.16 Q8 1 0.3402 0.2595 0.4142 11.00000 0.05 0.16 ; _shelx_res_checksum 82797 _shelx_hkl_file ; 0 0 -1 0.34 0.05 0 0 1 3.44 0.12 0 0 -2 1510.26 39.96 0 0 2 1462.06 39.91 0 0 2 1398.93 39.88 0 0 -3 0.63 0.12 0 0 -3 1.37 0.14 0 0 3 0.35 0.09 0 0 3 1.19 0.11 0 0 -4 1548.40 41.16 0 0 4 1501.04 41.09 0 0 4 1506.32 41.01 0 0 -5 0.34 0.14 0 0 5 0.05 0.08 0 0 5 0.48 0.15 0 0 -6 1175.29 32.12 0 0 6 1162.96 32.05 0 0 6 1182.18 32.19 0 0 6 1156.49 31.91 0 0 6 1196.56 32.02 0 0 -7 0.32 0.18 0 0 7 0.44 0.13 0 0 7 2.78 0.36 0 0 7 0.25 0.17 0 0 7 3.11 0.32 0 0 -8 76.84 2.73 0 0 8 79.49 2.85 0 0 8 76.12 2.64 0 0 8 80.80 2.64 0 0 -9 0.18 0.19 0 0 9 0.06 0.17 0 0 9 0.06 0.18 0 0 9 0.29 0.23 0 0 -10 100.61 3.66 0 0 10 110.26 3.55 0 0 10 106.55 3.81 0 0 10 104.73 3.58 0 0 11 1.41 0.37 0 0 11 0.76 0.32 0 0 12 120.04 4.49 0 0 12 129.21 4.20 0 0 12 119.97 4.23 0 0 13 0.07 0.26 0 0 13 0.15 0.30 0 0 13 0.48 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4 -8 11 0.25 0.43 -4 -8 -11 0.11 0.57 4 -8 11 0.19 0.44 -4 -8 -11 0.11 0.55 -4 -8 -11 0.49 0.49 4 -8 11 -0.09 0.46 -4 -8 -12 31.97 2.28 4 -8 12 26.48 1.93 4 -8 12 30.41 2.17 -4 -8 -12 29.65 2.14 -4 -8 -12 32.28 2.30 4 -8 12 31.20 2.05 -4 -8 -13 28.33 2.13 4 -8 13 25.00 1.87 4 -8 13 25.73 2.02 4 -8 13 25.70 1.87 -4 -8 -13 22.39 1.91 -4 -8 -13 24.74 2.05 4 -8 14 3.47 0.77 -4 -8 -14 3.89 0.85 -4 -8 -14 3.28 0.86 -4 -8 -14 3.03 0.79 4 -8 14 3.27 0.89 4 -8 15 5.48 0.95 -4 -8 -15 5.18 0.93 -4 -8 -15 5.71 1.09 -4 -8 -15 7.87 1.20 4 -8 15 7.46 1.15 -4 -8 -16 19.61 1.82 -4 -8 -16 25.02 1.91 4 -8 16 22.87 1.79 4 -8 16 20.05 1.77 -4 -8 -16 18.80 1.71 -4 -8 -17 14.27 1.49 4 -8 17 14.31 1.41 -4 -8 -17 9.41 1.22 4 -8 17 14.46 1.44 4 -8 18 5.56 0.93 -4 -8 -18 5.03 0.93 -4 -8 -18 7.31 1.09 4 -8 18 7.77 1.06 4 -8 19 12.07 1.17 -4 -8 -19 9.66 1.15 4 -8 19 10.46 1.13 -4 -8 -20 4.82 0.78 4 -8 20 6.21 0.82 -4 -8 -21 14.90 1.16 4 -8 21 14.57 1.13 -4 -8 -21 13.66 1.11 4 10 -21 3.63 0.64 -4 -10 21 3.80 0.58 4 -10 -21 3.26 0.57 -4 -10 20 11.02 1.03 4 -10 -20 10.89 1.04 -4 -10 19 1.07 0.46 4 -10 -19 1.10 0.49 4 -10 -19 1.14 0.54 4 -10 -19 1.96 0.56 -4 -10 18 43.43 2.42 4 -10 -18 44.06 2.35 4 -10 -18 41.28 2.32 4 -10 -18 43.03 2.41 -4 -10 17 10.63 1.24 4 -10 -17 12.94 1.31 4 -10 -17 10.33 1.18 4 -10 -17 11.33 1.20 -4 -10 16 1.03 0.63 4 -10 -16 1.13 0.59 4 -10 -16 0.09 0.57 4 -10 -16 0.81 0.58 -4 -10 15 22.57 1.82 4 -10 -15 20.19 1.76 4 -10 -15 22.20 1.76 -4 -10 14 106.79 4.56 4 -10 -14 100.88 4.48 4 -10 -14 99.20 4.39 -4 -10 13 18.53 1.71 4 -10 -13 19.43 1.63 4 -10 -13 18.21 1.71 4 -10 -13 17.10 1.58 4 -10 -13 18.43 1.64 -4 -10 12 2.17 0.74 4 -10 -12 2.15 0.73 4 -10 -12 1.75 0.68 4 -10 -12 2.29 0.73 4 -10 -12 2.28 0.67 -4 10 11 22.08 1.83 -4 -10 11 21.78 1.74 -4 -10 11 25.24 1.89 -4 -10 11 20.90 1.81 4 -10 -11 20.70 1.79 4 -10 -11 21.96 1.76 4 -10 -11 25.45 1.86 4 -10 -11 22.17 1.73 -4 -10 10 79.00 3.69 -4 10 10 78.09 3.77 -4 -10 10 80.80 3.78 -4 -10 10 84.00 3.91 4 -10 -10 82.80 3.74 4 -10 -10 82.94 3.93 4 -10 -10 81.39 3.71 4 -10 -10 83.67 3.65 -4 -10 9 10.98 1.30 -4 10 9 13.42 1.36 -4 -10 9 9.35 1.14 -4 -10 9 9.30 1.20 4 -10 -9 11.89 1.23 4 -10 -9 12.17 1.33 4 -10 -9 12.57 1.23 4 -10 -9 12.68 1.37 -4 -10 8 140.28 5.44 -4 -10 8 141.90 5.51 -4 -10 8 143.44 5.65 4 -10 -8 143.06 5.58 4 -10 -8 140.19 5.40 4 -10 -8 145.90 5.62 4 -10 -8 142.71 5.30 4 -10 -7 61.67 2.89 -4 -10 7 60.06 3.02 -4 -10 7 60.38 3.05 -4 -10 7 61.88 3.21 4 -10 -7 62.68 3.01 4 -10 -7 63.37 2.93 4 -10 -7 64.51 3.19 4 -10 -6 65.41 2.99 -4 -10 6 68.52 3.21 -4 -10 6 69.36 3.26 -4 -10 6 66.53 3.34 4 -10 -6 68.06 3.13 4 -10 -6 65.50 3.01 4 -10 -6 69.93 3.32 -4 -10 5 10.03 1.10 4 -10 -5 7.73 0.92 -4 -10 5 10.35 1.15 -4 -10 5 8.20 1.09 4 -10 -5 8.83 1.14 4 -10 -5 8.70 1.11 4 -10 -5 7.62 0.93 4 -10 -5 7.40 0.95 -4 -10 4 23.32 1.69 4 -10 -4 25.97 1.64 -4 -10 4 23.35 1.69 -4 -10 4 25.02 1.88 -4 -10 4 27.38 1.92 4 10 -4 25.23 2.17 4 -10 -4 25.24 1.86 4 -10 -4 23.36 1.56 4 -10 -4 27.35 1.86 -4 -10 3 339.88 10.58 4 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3.13 4 -10 6 56.70 3.10 -4 -10 -6 52.06 2.99 4 -10 6 59.56 3.09 -4 -10 -6 59.92 3.24 -4 -10 -6 59.87 2.73 -4 -10 -6 51.16 2.80 4 -10 7 20.37 1.67 -4 -10 -7 21.94 1.60 4 -10 7 18.71 1.64 -4 -10 -7 18.67 1.71 4 -10 7 20.99 1.74 4 -10 7 21.75 1.81 -4 -10 -7 20.21 1.79 -4 -10 -7 20.27 1.64 -4 -10 -7 20.30 1.76 4 -10 7 18.53 1.65 -4 -10 -7 18.97 1.58 -4 -10 -8 31.55 2.01 4 -10 8 30.49 2.13 4 -10 8 28.95 2.09 -4 -10 -8 31.31 2.30 4 -10 8 35.54 2.35 4 -10 8 33.25 2.25 -4 -10 -8 33.07 2.12 -4 -10 -8 33.28 2.31 4 -10 8 33.15 2.27 4 -10 8 31.75 2.21 -4 -10 -8 33.05 2.15 -4 -10 -9 29.44 1.97 4 -10 9 31.26 2.14 4 -10 9 26.44 2.05 -4 -10 -9 33.18 2.37 4 -10 9 30.86 2.21 4 -10 9 34.03 2.32 4 -10 9 34.41 2.31 -4 -10 -9 35.17 2.19 -4 -10 -9 35.28 2.42 4 -10 9 33.97 2.33 4 -10 10 8.01 1.09 4 -10 10 8.09 1.19 -4 -10 -10 8.15 1.02 4 -10 10 6.80 1.02 -4 -10 -10 6.87 1.15 4 -10 10 8.41 1.17 -4 -10 -10 8.21 1.23 4 -10 10 7.87 1.13 4 -10 10 5.68 1.06 -4 -10 -10 9.48 1.14 -4 -10 -11 30.02 2.28 4 -10 11 27.56 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0.44 4 -12 -16 1.29 0.51 4 -12 -16 1.62 0.55 4 -12 -16 1.63 0.56 -4 -12 16 2.12 0.62 4 12 -16 0.59 0.50 4 -12 -15 1.02 0.52 4 -12 -15 1.85 0.60 4 -12 -15 2.05 0.60 -4 -12 15 1.68 0.59 4 -12 -14 8.06 1.05 4 -12 -14 5.61 0.87 4 -12 -14 7.44 1.01 -4 -12 14 8.11 1.07 4 -12 -13 0.60 0.58 -4 -12 13 0.27 0.54 -4 -12 12 7.24 1.11 -4 -12 12 7.77 1.13 4 -12 -12 6.48 1.01 4 -12 -12 7.20 1.02 -4 -12 11 41.95 2.54 -4 -12 11 43.46 2.65 4 -12 -11 41.97 2.52 4 -12 -11 46.85 2.54 -4 -12 10 109.08 4.55 -4 -12 10 103.71 4.64 4 -12 -10 98.94 4.36 4 -12 -10 103.76 4.33 -4 -12 9 25.30 1.92 -4 -12 9 26.91 2.08 4 -12 -9 25.05 1.88 4 -12 -9 25.96 1.85 4 -12 -9 27.25 2.05 -4 -12 8 12.74 1.45 4 -12 -8 12.25 1.32 4 -12 -8 11.79 1.39 4 -12 -8 11.86 1.26 -4 -12 8 11.43 1.32 -4 -12 7 2.79 0.83 4 -12 -7 4.57 0.84 4 -12 -7 5.52 0.90 4 -12 -7 3.18 0.87 4 -12 -7 3.24 0.83 -4 -12 7 3.92 0.86 -4 -12 6 7.18 1.13 -4 -12 6 7.35 1.06 4 -12 -6 7.30 1.02 4 -12 -6 4.91 1.02 4 -12 -6 7.11 1.14 4 -12 -6 6.52 0.95 -4 -12 5 7.57 1.07 4 -12 -5 7.53 0.97 -4 -12 5 6.59 1.03 -4 -12 5 7.04 1.16 4 12 -5 7.29 1.43 -4 -12 5 7.59 1.18 4 -12 -5 6.69 1.12 4 -12 -5 6.70 0.99 4 -12 -5 8.03 1.18 -4 -12 4 6.12 1.01 -4 -12 4 10.54 1.24 -4 -12 4 8.82 1.27 -4 -12 4 8.52 1.25 4 12 -4 8.33 1.56 4 -12 -4 9.67 1.29 4 -12 -4 9.38 1.09 4 -12 -4 9.91 1.26 -4 -12 3 69.77 3.42 -4 -12 3 69.31 3.39 4 -12 -3 71.08 3.58 -4 -12 3 75.37 3.75 -4 -12 3 70.69 3.66 4 12 -3 75.81 4.81 4 -12 -3 78.03 3.35 4 -12 -3 68.45 3.65 4 -12 -3 75.35 3.62 -4 -12 2 41.44 2.48 -4 -12 2 41.19 2.47 -4 -12 2 44.83 2.76 -4 -12 2 47.08 2.85 4 -12 -2 46.23 2.75 4 12 -2 38.09 3.47 4 -12 -2 44.95 2.79 -4 -12 2 46.19 2.73 4 12 -1 115.72 6.56 -4 -12 1 112.02 4.70 -4 -12 1 120.67 5.12 -4 -12 1 117.86 5.13 4 -12 -1 117.11 5.04 -4 -12 1 119.64 4.81 4 -12 -1 122.07 5.01 -4 -12 1 124.50 5.13 4 12 0 187.36 9.45 -4 -12 0 213.44 7.43 4 -12 0 198.56 7.60 4 -12 0 218.98 7.86 -4 -12 0 215.95 7.83 -4 -12 0 225.24 7.98 -4 -12 0 211.64 7.44 4 -12 0 217.50 7.78 -4 -12 0 216.07 7.80 4 12 1 141.34 8.00 -4 -12 -1 160.33 5.99 4 -12 1 156.58 6.23 -4 -12 -1 161.33 6.43 -4 -12 -1 171.30 6.44 4 -12 1 155.65 6.33 -4 -12 -1 163.76 6.01 4 -12 1 174.56 6.46 -4 -12 -1 161.50 6.36 -4 -12 -1 161.30 5.93 4 12 2 220.44 10.83 -4 -12 -2 245.59 8.46 4 -12 2 245.55 8.76 4 -12 2 264.42 9.01 -4 -12 -2 245.78 8.80 -4 -12 -2 258.51 9.07 -4 -12 -2 252.59 8.45 4 -12 2 250.60 8.90 -4 -12 -2 258.11 8.43 4 -12 2 254.38 8.73 -4 -12 -2 243.21 8.56 -4 -12 -2 256.58 8.95 -4 -12 -3 5.88 1.15 -4 -12 -3 3.96 0.85 4 -12 3 5.02 1.00 -4 -12 -3 6.33 1.24 4 -12 3 4.39 1.04 -4 -12 -3 4.67 0.83 4 -12 3 5.68 1.14 -4 -12 -3 4.64 1.14 4 -12 3 3.76 0.95 -4 -12 -3 4.63 0.88 -4 -12 -3 4.52 0.97 -4 -12 -4 170.38 6.19 4 -12 4 155.89 6.35 -4 -12 -4 165.63 6.06 4 -12 4 169.35 6.44 -4 -12 -4 177.53 6.77 4 -12 4 164.97 6.58 -4 -12 -4 169.05 6.53 -4 -12 -4 168.37 6.35 4 -12 4 166.57 6.60 -4 -12 -4 176.33 6.13 -4 -12 -4 175.21 6.72 -4 -12 -4 159.38 6.24 4 -12 4 161.47 6.40 -4 -12 -5 73.58 3.82 4 -12 5 80.94 3.88 4 -12 5 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6.39 1.08 -8 -8 14 8.18 1.14 8 -8 -13 1.62 0.78 8 -8 -13 1.74 0.82 8 -8 -13 1.43 0.81 8 -8 -13 2.33 0.68 -8 8 13 0.72 0.56 -8 -8 13 2.54 0.80 -8 -8 13 3.54 0.87 8 -8 -12 334.52 11.48 8 -8 -12 360.34 11.72 8 -8 -12 384.67 11.80 8 -8 -12 356.60 11.60 -8 -8 12 345.85 11.49 -8 -8 12 390.16 11.81 -8 -8 12 366.89 11.72 8 -8 -11 13.15 1.33 8 -8 -11 13.97 1.41 8 -8 -11 12.20 1.37 8 -8 -11 15.30 1.43 -8 -8 11 12.35 1.31 -8 -8 11 14.01 1.43 -8 -8 11 12.75 1.36 8 -8 -10 37.94 2.27 8 -8 -10 44.44 2.48 8 -8 -10 40.79 2.39 8 -8 -10 40.71 2.36 -8 -8 10 38.91 2.32 -8 -8 10 40.81 2.44 -8 -8 10 41.48 2.42 8 8 -10 43.33 2.77 8 -8 -9 15.00 1.34 8 -8 -9 15.63 1.43 8 -8 -9 17.86 1.48 8 -8 -9 18.58 1.48 -8 -8 9 14.57 1.38 8 8 -9 15.84 1.66 -8 -8 9 19.32 1.56 -8 -8 9 18.70 1.57 8 -8 -8 25.70 1.73 -8 -8 8 24.62 1.76 8 -8 -8 25.89 1.77 8 -8 -8 27.14 1.78 8 -8 -8 25.71 1.76 -8 -8 8 25.17 1.76 8 8 -8 27.09 2.09 -8 -8 8 26.46 1.81 -8 -8 8 25.16 1.83 8 -8 -7 0.14 0.37 -8 -8 7 0.39 0.41 8 -8 -7 0.07 0.40 8 -8 -7 0.22 0.43 -8 -8 7 -0.16 0.48 -8 -8 7 0.25 0.45 -8 -8 7 0.71 0.49 8 8 -7 0.21 0.56 8 -8 -6 112.99 4.30 -8 -8 6 109.89 4.38 8 8 -6 102.13 4.64 -8 -8 6 109.09 4.40 -8 -8 6 109.78 4.31 -8 -8 6 105.69 4.32 -8 -8 5 3.96 0.77 -8 -8 5 4.81 0.76 8 8 -5 4.06 0.88 8 8 -5 3.32 1.06 -8 -8 5 4.59 0.72 -8 -8 5 4.15 0.75 -8 -8 4 4.53 0.81 -8 -8 4 6.22 0.86 8 8 -4 3.93 0.85 -8 -8 4 3.06 0.61 -8 -8 4 3.83 0.71 8 8 -4 3.82 1.14 -8 -8 3 158.87 5.77 -8 -8 3 164.37 5.73 8 8 -3 153.39 5.96 -8 -8 3 149.19 5.72 8 8 -3 142.38 7.21 -8 -8 3 161.05 5.70 -8 -8 3 160.02 5.69 -8 -8 2 0.14 0.36 -8 -8 2 0.92 0.55 -8 -8 2 1.65 0.53 -8 -8 2 0.50 0.40 8 8 -2 0.78 0.91 -8 -8 2 2.52 0.68 8 8 -1 7.66 1.65 8 -8 -1 9.46 1.00 -8 -8 1 9.86 1.06 -8 -8 1 10.21 1.06 -8 -8 1 12.55 1.18 -8 -8 1 11.82 1.21 8 -8 -1 9.60 1.07 8 -8 -1 9.32 1.04 8 -8 0 61.81 2.94 -8 -8 0 64.90 3.08 -8 -8 0 65.81 2.97 8 -8 0 62.70 3.01 -8 -8 0 67.07 3.11 8 -8 0 64.79 2.95 -8 -8 0 66.58 3.18 -8 -8 0 64.31 3.08 8 -8 0 66.15 3.18 8 -8 0 66.17 3.08 8 -8 1 65.15 3.02 -8 -8 -1 68.73 3.15 -8 -8 -1 68.24 2.99 8 -8 1 65.71 3.07 -8 -8 -1 60.16 2.99 8 -8 1 62.39 3.09 -8 -8 -1 65.90 3.21 -8 -8 -1 63.90 3.11 8 -8 1 63.24 2.93 8 -8 1 63.46 3.15 8 -8 1 61.18 2.97 8 -8 1 62.77 3.05 -8 -8 -2 10.72 1.00 8 -8 2 9.33 1.07 8 -8 2 9.62 1.09 -8 -8 -2 9.46 0.99 -8 -8 -2 10.83 1.13 8 -8 2 12.39 1.25 8 -8 2 12.14 1.14 -8 -8 -2 9.42 1.14 8 -8 2 9.73 1.13 8 -8 2 11.26 1.15 8 -8 2 11.27 1.17 8 -8 3 7.59 0.97 8 -8 3 8.57 1.07 -8 -8 -3 8.40 1.01 -8 -8 -3 9.62 1.15 8 -8 3 10.32 1.18 8 -8 3 8.12 0.99 8 -8 3 8.01 1.07 8 -8 3 9.65 1.09 8 -8 3 8.07 1.03 8 -8 4 9.78 1.08 8 -8 4 7.97 1.05 -8 -8 -4 9.96 1.11 8 -8 4 6.99 1.06 8 -8 4 9.70 1.07 8 -8 4 7.60 1.09 8 -8 4 8.76 1.07 8 -8 4 8.67 1.11 8 -8 5 6.38 1.00 -8 -8 -5 8.67 1.06 8 -8 5 8.75 1.15 8 -8 5 9.39 1.08 8 -8 5 8.22 1.14 8 -8 5 10.74 1.21 8 -8 5 8.22 1.09 -8 -8 -6 267.51 8.64 8 -8 6 267.63 8.68 8 -8 6 257.95 8.95 -8 -8 -6 268.31 8.75 8 -8 6 254.59 8.95 8 -8 6 255.85 8.98 8 -8 6 250.81 8.77 8 -8 6 252.63 8.81 -8 -8 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16.12 10 -6 -10 519.77 16.18 10 -6 -10 536.83 16.14 10 -6 -10 534.03 16.14 10 -6 -10 550.88 16.05 -10 -6 10 498.46 15.93 -10 -6 9 213.26 7.36 -10 -6 9 211.49 7.51 10 6 -9 207.23 7.82 10 -6 -9 225.55 7.33 10 -6 -9 218.24 7.46 10 -6 -9 214.00 7.41 10 -6 -9 225.07 7.44 10 -6 -9 217.16 7.31 -10 -6 9 204.91 7.25 -10 -6 8 19.29 1.44 -10 -6 8 17.64 1.41 10 -6 -8 16.57 1.40 10 -6 -8 17.88 1.42 -10 -6 8 14.34 1.27 10 -6 -8 17.32 1.36 10 6 -8 15.22 1.59 -10 -6 7 36.05 2.04 -10 -6 7 33.13 1.99 10 -6 -7 32.93 1.97 10 -6 -7 36.30 2.05 -10 -6 7 33.59 1.95 10 -6 -7 34.45 1.97 -10 -6 7 32.57 2.05 10 6 -7 31.15 2.23 -10 -6 6 46.40 2.49 -10 -6 6 49.99 2.54 10 -6 -6 54.31 2.60 10 -6 -6 51.55 2.53 -10 -6 6 48.78 2.44 10 -6 -6 51.72 2.52 -10 -6 6 56.54 2.76 10 6 -6 47.18 2.81 -10 -6 5 15.05 1.27 -10 -6 5 14.86 1.27 10 -6 -5 15.92 1.30 -10 -6 5 15.36 1.22 10 -6 -5 14.33 1.22 10 6 -5 14.71 1.50 -10 -6 5 14.30 1.23 -10 -6 4 0.37 0.38 -10 -6 4 0.49 0.43 -10 -6 4 0.34 0.38 -10 -6 4 0.08 0.43 10 6 -4 0.74 0.52 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7.66 -10 -6 -7 29.36 1.98 10 -6 7 25.76 1.90 10 -6 7 29.74 2.10 10 6 7 27.24 1.93 -10 -6 -7 25.44 1.90 -10 -6 -7 29.02 2.01 10 -6 7 31.41 2.20 10 -6 7 27.87 2.08 10 -6 7 29.20 2.02 10 -6 7 32.61 2.12 10 -6 8 1.00 0.54 10 -6 8 0.75 0.63 10 -6 8 0.52 0.51 10 6 8 1.35 0.59 -10 -6 -8 1.02 0.67 10 -6 8 -0.21 0.75 10 -6 8 0.21 0.68 10 -6 8 0.83 0.69 10 6 8 1.64 0.74 10 -6 8 0.91 0.59 10 -6 9 87.94 4.17 10 6 9 90.23 3.96 10 6 9 85.94 4.23 -10 -6 -9 89.54 4.05 10 -6 9 86.69 4.18 10 -6 9 85.54 4.02 10 -6 9 86.11 4.10 10 -6 9 88.11 3.99 -10 -6 -9 87.31 4.04 10 -6 10 29.17 2.18 10 6 10 28.77 2.02 10 6 10 29.34 2.29 10 -6 10 32.80 2.36 10 -6 10 29.52 2.15 -10 -6 -10 29.54 2.16 10 -6 10 33.31 2.27 10 -6 11 6.92 1.17 10 6 11 8.25 1.28 10 -6 11 8.91 1.23 10 6 12 87.48 4.43 10 -6 12 97.03 4.49 10 -6 12 101.84 4.47 10 -6 13 2.80 0.81 10 6 13 3.88 0.95 10 -6 13 3.57 0.85 10 6 14 57.31 3.27 10 -6 14 62.98 3.29 10 -6 14 62.22 3.26 10 6 15 5.05 0.93 10 -6 15 5.29 0.93 -10 -6 -15 4.90 0.91 10 -6 15 6.09 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1.97 11 -5 3 30.54 1.95 11 -5 3 30.49 2.10 11 -5 3 29.45 1.98 -11 -5 -4 14.21 1.30 11 -5 4 14.43 1.32 -11 -5 -4 15.06 1.35 -11 -5 -4 14.52 1.38 11 -5 4 14.29 1.37 -11 -5 -4 13.84 1.32 11 5 4 17.26 1.37 11 -5 4 13.81 1.44 11 -5 4 13.28 1.30 11 -5 4 15.55 1.36 11 -5 4 11.80 1.25 -11 -5 -5 322.76 10.43 11 -5 5 312.14 10.48 -11 -5 -5 316.99 10.46 -11 -5 -5 323.44 10.55 11 -5 5 328.97 10.69 11 5 5 347.79 10.53 11 -5 5 321.12 10.79 11 -5 5 310.20 10.41 11 -5 5 326.09 10.56 11 -5 5 333.30 10.53 -11 -5 -6 142.42 5.47 11 -5 6 131.70 5.39 -11 -5 -6 139.07 5.46 -11 -5 -6 145.99 5.54 11 -5 6 137.97 5.58 11 5 6 148.22 5.44 11 -5 6 138.88 5.69 11 -5 6 139.28 5.41 11 -5 6 145.18 5.50 11 -5 6 144.48 5.50 -11 -5 -7 1.39 0.66 11 -5 7 0.27 0.46 -11 -5 -7 1.30 0.67 11 -5 7 1.42 0.63 11 5 7 1.36 0.60 11 -5 7 2.32 0.79 11 -5 7 0.44 0.51 11 -5 7 0.89 0.59 11 -5 8 233.35 8.52 11 5 8 240.28 8.23 11 5 8 244.23 8.67 -11 -5 -8 232.07 8.34 11 -5 8 247.39 8.62 -11 -5 -8 241.99 8.44 11 -5 9 45.76 2.85 11 5 9 53.34 2.80 11 5 9 50.88 3.06 11 -5 9 54.49 2.94 11 -5 9 46.70 2.86 -11 -5 -9 46.64 2.83 11 -5 10 100.40 4.51 11 5 10 95.46 4.67 11 -5 10 104.20 4.56 11 5 11 7.35 1.27 11 -5 11 7.27 1.12 11 5 12 71.11 3.88 11 -5 12 77.29 3.81 11 5 13 21.61 1.98 11 -5 13 25.63 2.04 11 -5 13 24.57 1.96 11 5 14 2.28 0.80 11 -5 14 0.92 0.61 11 -5 14 0.70 0.58 11 5 15 0.95 0.59 11 -5 15 1.88 0.69 11 -5 15 1.51 0.65 -11 -5 -16 25.10 1.82 11 5 16 27.50 1.98 11 -5 16 26.42 1.84 11 -5 16 28.88 1.95 11 5 17 0.17 0.38 -11 -5 -17 0.29 0.47 11 -5 17 -0.54 0.46 -11 -5 -18 9.81 0.97 11 5 18 8.98 0.99 11 -5 18 11.59 1.05 11 5 19 0.17 0.31 -11 -5 -19 -0.10 0.32 11 -5 19 0.27 0.33 -11 -7 22 24.86 1.44 11 -7 -22 30.08 1.51 -11 -7 21 0.18 0.38 11 -7 -21 0.49 0.43 11 -7 -20 4.11 0.70 -11 -7 20 3.44 0.70 11 -7 -20 4.52 0.76 11 -7 -19 3.56 0.72 -11 -7 19 2.81 0.71 11 -7 -19 3.93 0.80 11 -7 -18 2.25 0.72 -11 -7 18 2.41 0.75 11 -7 -18 2.83 0.71 11 -7 -17 13.01 1.35 -11 -7 17 12.48 1.34 11 7 -17 11.87 1.52 11 -7 -17 14.16 1.34 11 -7 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9 25.67 2.00 11 7 -9 25.50 2.18 -11 -7 8 2.59 0.67 11 -7 -8 3.04 0.74 11 -7 -8 2.11 0.69 11 -7 -8 2.11 0.63 -11 -7 8 3.87 0.77 -11 -7 8 2.26 0.69 11 7 -8 1.75 0.78 -11 -7 7 31.64 2.07 -11 -7 7 31.93 2.07 11 -7 -7 34.45 2.10 11 -7 -7 33.48 2.09 -11 -7 7 35.40 2.10 11 -7 -7 31.30 2.01 11 7 -7 28.99 2.28 -11 -7 7 35.67 2.24 -11 -7 6 33.06 2.12 -11 -7 6 32.22 2.06 11 7 -6 32.08 2.32 -11 -7 6 32.65 2.04 -11 -7 6 36.47 2.26 11 -7 -6 38.68 2.19 11 -7 -6 33.46 2.06 -11 -7 5 0.09 0.41 -11 -7 5 0.49 0.44 -11 -7 5 0.57 0.49 -11 -7 5 0.36 0.49 11 7 -5 0.53 0.58 11 -7 -5 1.08 0.55 11 -7 -5 1.17 0.52 11 -7 -5 0.40 0.51 -11 -7 4 65.14 3.23 -11 -7 4 64.00 3.15 11 7 -4 65.90 3.45 -11 -7 4 63.76 3.12 -11 -7 4 73.98 3.38 11 -7 -4 70.71 3.29 11 -7 -4 71.47 3.19 11 -7 -4 66.44 3.15 -11 -7 3 2.91 0.70 -11 -7 3 2.02 0.63 -11 -7 3 3.23 0.71 -11 -7 3 2.94 0.72 11 7 -3 2.84 0.79 11 -7 -3 3.72 0.75 11 -7 -3 2.29 0.61 11 -7 -3 2.37 0.64 -11 -7 2 13.67 1.35 -11 -7 2 16.64 1.37 11 7 -2 15.32 1.49 -11 -7 2 13.48 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38.11 2.35 -11 -7 -4 41.00 2.40 11 -7 4 38.38 2.44 11 -7 4 37.29 2.50 11 -7 4 39.25 2.45 11 -7 4 40.76 2.44 11 -7 4 38.12 2.43 -11 -7 -5 251.95 8.54 11 -7 5 240.91 8.59 11 7 5 251.35 8.66 11 -7 5 243.63 8.74 -11 -7 -5 253.48 8.62 -11 -7 -5 251.44 8.59 11 -7 5 253.77 8.82 11 -7 5 245.58 8.87 11 -7 5 260.31 8.72 11 -7 5 248.04 8.68 11 -7 5 250.29 8.64 -11 -7 -6 223.76 7.86 11 -7 6 205.30 7.79 11 7 6 218.71 7.86 11 -7 6 214.60 8.03 -11 -7 -6 227.90 7.93 -11 -7 -6 222.73 7.87 11 -7 6 227.57 8.15 11 -7 6 231.31 8.28 11 -7 6 233.19 8.00 11 -7 6 230.98 8.03 -11 -7 -7 25.34 1.94 11 -7 7 23.19 1.88 11 7 7 28.72 2.04 11 -7 7 23.14 1.99 -11 -7 -7 26.78 1.98 11 -7 7 25.41 2.08 11 -7 7 25.62 2.10 11 -7 7 29.95 2.08 11 -7 7 23.00 1.90 11 7 8 114.58 5.26 -11 -7 -8 123.90 5.13 11 -7 8 123.86 5.38 11 -7 8 127.69 5.40 11 -7 8 130.46 5.22 11 -7 8 128.91 5.20 11 -7 9 -0.33 0.62 11 7 9 0.23 0.62 -11 -7 -9 -0.10 0.72 11 -7 9 -0.23 0.72 11 -7 10 57.24 3.19 11 7 10 51.36 3.15 11 -7 10 59.76 3.27 11 -7 10 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6 0.48 0.45 19 3 6 0.40 0.43 19 3 7 4.75 0.79 19 -3 7 5.15 0.80 19 3 7 5.54 0.80 19 3 8 0.77 0.42 19 -3 8 0.70 0.40 19 3 9 -0.06 0.29 19 -3 9 0.22 0.32 19 -5 -15 1.84 0.46 19 -5 -15 1.21 0.44 19 -5 -14 2.06 0.54 19 -5 -14 3.63 0.61 19 5 -14 1.99 0.48 19 5 -14 1.85 0.49 19 -5 -13 6.79 0.85 19 -5 -13 6.46 0.82 19 5 -13 6.02 0.77 19 5 -13 5.90 0.77 19 -5 -12 0.44 0.49 19 -5 -12 0.83 0.45 19 5 -12 0.43 0.41 19 5 -12 0.42 0.45 19 -5 -11 14.12 1.25 19 -5 -11 16.05 1.31 19 5 -11 18.22 1.37 19 5 -11 14.66 1.22 19 -5 -10 8.78 0.99 19 -5 -10 8.79 1.00 19 5 -10 9.64 1.07 19 -5 -9 0.79 0.49 19 -5 -9 1.67 0.58 19 5 -9 1.59 0.59 19 -5 -8 6.11 0.91 19 -5 -8 7.62 0.97 19 5 -8 8.23 1.01 19 -5 -7 6.06 0.89 19 -5 -7 6.40 0.91 19 5 -7 7.42 0.99 19 -5 -7 5.94 0.94 -19 -5 6 1.13 0.53 19 -5 -6 2.41 0.66 19 -5 -6 1.39 0.58 19 5 -6 1.73 0.64 19 5 -6 1.92 0.65 19 -5 -6 1.52 0.65 19 5 -6 1.20 0.54 -19 -5 5 0.58 0.46 19 -5 -5 0.16 0.46 19 5 -5 0.22 0.45 19 5 -5 0.09 0.49 19 -5 -5 -0.09 0.56 19 5 -5 -0.15 0.44 -19 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9.98 0.96 19 5 7 7.55 0.92 -19 -7 12 4.85 0.64 19 -7 -12 5.28 0.68 19 7 -12 4.68 0.65 -19 -7 11 0.26 0.33 19 -7 -11 0.72 0.40 19 7 -11 1.07 0.44 -19 -7 10 4.80 0.70 19 -7 -10 4.59 0.71 19 7 -10 5.10 0.73 -19 -7 9 1.23 0.46 19 -7 -9 0.49 0.40 19 7 -9 0.41 0.42 -19 -7 8 0.12 0.37 19 -7 -8 0.26 0.39 19 7 -8 0.54 0.46 -19 -7 7 1.41 0.52 19 -7 -7 1.38 0.52 19 7 -7 1.40 0.52 19 7 -7 1.56 0.51 -19 -7 6 8.75 0.97 19 -7 -6 9.85 1.03 19 -7 -6 8.29 0.97 19 7 -6 9.97 0.99 19 7 -6 10.27 1.00 -19 -7 5 8.13 0.95 19 -7 -5 7.81 0.95 19 -7 -5 7.20 0.93 19 -7 -5 6.73 0.91 19 7 -5 7.47 0.88 -19 -7 4 0.34 0.46 19 -7 -4 0.14 0.43 19 -7 -4 0.14 0.42 19 7 -4 0.26 0.44 19 -7 -4 -0.42 0.45 -19 -7 3 18.66 1.47 19 -7 -3 21.46 1.53 19 -7 -3 22.47 1.59 19 7 -3 22.34 1.51 19 -7 -3 21.40 1.52 -19 -7 2 0.41 0.46 19 -7 -2 0.61 0.50 19 -7 -2 0.29 0.48 19 7 -2 1.17 0.49 19 -7 -2 0.69 0.50 -19 -7 1 1.09 0.50 19 -7 -1 1.07 0.47 19 -7 -1 1.01 0.52 19 7 -1 0.51 0.46 19 -7 0 2.85 0.60 19 -7 0 2.73 0.65 19 7 0 3.28 0.67 19 -7 1 -0.07 0.35 19 7 1 0.21 0.38 19 7 1 -0.24 0.44 19 -7 1 0.06 0.36 19 -7 1 0.13 0.39 19 7 1 -0.06 0.39 19 -7 2 -0.14 0.37 19 7 2 0.27 0.36 19 7 2 0.08 0.48 19 -7 2 0.23 0.35 19 -7 2 0.51 0.42 19 7 2 -0.12 0.42 19 -7 3 1.74 0.51 19 7 3 3.49 0.65 19 7 3 2.18 0.60 19 -7 3 2.25 0.56 19 -7 4 4.74 0.70 19 7 4 3.37 0.61 19 7 4 3.57 0.69 19 -7 4 3.02 0.56 19 -7 5 0.06 0.32 19 7 5 0.22 0.34 19 7 5 -0.25 0.38 -19 -9 7 1.82 0.46 19 -9 -7 2.07 0.48 -19 -9 6 18.90 1.25 19 -9 -6 19.94 1.26 19 -9 -6 20.50 1.27 19 9 -6 20.86 1.25 -19 -9 5 0.10 0.32 19 -9 -5 0.05 0.32 19 -9 -5 0.15 0.31 19 9 -5 0.62 0.35 -19 -9 4 1.28 0.43 19 -9 -4 1.96 0.48 19 9 -4 2.46 0.50 19 -9 -4 2.01 0.45 -19 -9 3 8.80 0.86 19 -9 -3 9.57 0.87 19 9 -3 8.53 0.81 19 -9 -3 8.64 0.85 19 -9 -2 0.10 0.32 19 9 -2 0.10 0.30 19 -9 -2 0.10 0.30 19 -9 -1 2.27 0.50 19 9 -1 1.25 0.43 19 -9 -1 1.19 0.40 19 9 -1 1.98 0.53 19 -9 0 -0.05 0.32 19 9 0 -0.05 0.29 19 -9 0 0.05 0.30 19 9 0 -0.06 0.33 20 0 -14 0.76 0.42 20 0 -13 -0.06 0.40 20 0 -12 12.81 1.16 20 0 -11 -0.07 0.45 20 0 -11 0.35 0.46 20 0 -10 14.00 1.29 20 0 -10 12.79 1.23 20 0 -9 0.78 0.61 20 0 -9 0.61 0.57 20 0 -8 39.65 2.34 20 0 -8 41.49 2.34 20 0 -7 1.34 0.70 20 0 -7 1.62 0.69 20 0 -6 158.67 5.92 20 0 -6 156.53 5.98 20 0 -5 0.77 0.64 20 0 -5 -0.37 0.65 20 0 -4 42.55 2.47 20 0 -4 45.61 2.61 20 0 -3 0.09 0.50 20 0 -3 0.09 0.55 20 0 -2 1.93 0.68 20 0 -2 1.71 0.69 20 0 -2 2.79 0.75 20 0 -1 -0.19 0.64 20 0 -1 0.33 0.49 20 0 -1 -0.09 0.50 20 0 0 1.03 0.61 20 0 0 0.08 0.46 20 0 0 0.75 0.59 20 0 1 -0.18 0.57 20 0 1 -0.46 0.53 20 0 2 -0.27 0.53 20 0 2 -0.09 0.50 20 0 3 -0.09 0.44 20 0 3 -0.35 0.54 20 0 4 16.79 1.44 20 0 4 16.32 1.40 20 0 5 -0.23 0.46 20 0 5 0.69 0.49 20 0 6 0.07 0.37 20 0 6 0.56 0.42 20 0 7 -0.06 0.33 20 0 7 -0.12 0.34 20 0 8 5.00 0.68 20 2 -15 0.05 0.30 20 -2 -15 0.05 0.32 20 2 -14 5.65 0.71 20 -2 -14 6.31 0.77 20 2 -13 0.94 0.43 20 2 -13 1.19 0.45 20 -2 -13 0.36 0.41 20 2 -12 18.61 1.35 20 -2 -12 17.52 1.35 20 2 -11 20.29 1.47 20 -2 -11 21.25 1.51 20 2 -10 11.03 1.12 20 -2 -10 9.73 1.07 20 -2 -10 8.21 1.02 20 -2 -9 26.47 1.77 20 2 -9 25.65 1.74 20 -2 -9 24.12 1.69 20 -2 -8 15.49 1.41 20 2 -8 17.81 1.44 20 -2 -8 16.34 1.42 20 -2 -7 0.50 0.58 20 2 -7 0.32 0.49 20 -2 -7 0.32 0.54 20 -2 -6 26.88 1.88 20 2 -6 24.25 1.75 20 2 -6 26.77 1.92 20 -2 -6 25.19 1.78 20 2 -5 0.32 0.50 20 2 -5 1.10 0.64 20 -2 -5 0.43 0.62 20 2 -4 2.33 0.67 20 -2 -4 2.37 0.68 20 2 -4 2.97 0.79 20 -2 -4 2.59 0.73 20 2 -3 6.49 0.94 20 -2 -3 5.64 0.93 20 2 -3 5.60 0.98 20 -2 -3 5.16 0.94 20 2 -3 4.59 0.84 20 2 -2 5.99 0.88 20 -2 -2 6.26 0.99 20 2 -2 5.88 0.95 20 -2 -2 6.11 0.97 20 2 -2 6.12 0.95 20 -2 -1 1.03 0.61 20 2 -1 1.67 0.67 20 -2 -1 1.98 0.68 20 -2 -1 2.26 0.68 20 2 -1 1.45 0.60 20 -2 0 12.11 1.25 20 -2 0 14.14 1.37 20 2 0 12.53 1.33 20 2 0 13.67 1.39 20 -2 0 12.04 1.29 20 -2 1 1.66 0.64 20 2 1 1.79 0.63 20 -2 1 1.97 0.63 20 -2 1 1.70 0.61 20 2 1 2.41 0.69 20 -2 2 9.19 1.09 20 2 2 8.94 1.14 20 -2 2 8.87 1.07 20 2 2 8.18 1.06 20 -2 3 10.61 1.12 20 2 3 8.98 1.10 20 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0.67 20 4 -3 2.77 0.66 20 4 -3 2.56 0.64 20 4 -2 0.91 0.51 20 -4 -2 0.08 0.54 20 4 -2 -0.22 0.49 20 4 -2 -0.16 0.46 20 4 -1 -0.33 0.46 20 -4 -1 -0.77 0.53 20 4 -1 0.14 0.46 20 4 -1 -0.08 0.43 20 4 0 5.54 0.86 20 -4 0 4.31 0.80 20 -4 0 4.16 0.76 20 4 0 4.15 0.79 20 4 1 1.63 0.56 20 -4 1 1.06 0.51 20 -4 1 1.90 0.59 20 4 1 1.28 0.55 20 4 2 0.15 0.39 20 -4 2 0.46 0.40 20 -4 2 0.08 0.40 20 4 2 -0.23 0.46 20 4 3 1.48 0.52 20 -4 3 1.03 0.46 20 4 3 0.89 0.43 20 4 4 7.22 0.86 20 -4 4 7.77 0.91 20 4 4 8.87 0.97 20 4 5 0.36 0.33 20 -4 5 0.64 0.42 20 4 5 0.58 0.40 20 -4 6 3.45 0.60 20 -6 -11 3.38 0.55 20 6 -11 4.85 0.64 20 -6 -10 1.29 0.45 20 6 -10 1.04 0.41 20 -6 -9 1.20 0.45 20 6 -9 2.28 0.55 20 -6 -8 -0.06 0.34 20 6 -8 0.34 0.37 20 -6 -7 10.70 1.00 20 6 -7 9.74 0.96 -20 -6 6 0.72 0.41 20 -6 -6 1.36 0.51 20 -6 -6 1.07 0.52 20 6 -6 1.08 0.46 20 -6 -6 0.70 0.42 20 6 -6 0.72 0.39 -20 -6 5 3.55 0.63 20 -6 -5 4.31 0.69 20 -6 -5 3.80 0.69 20 -6 -5 5.19 0.80 20 6 -5 5.37 0.73 -20 -6 4 4.60 0.70 20 -6 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0.99 0.52 21 1 -8 8.11 0.96 21 -1 -8 6.78 0.89 21 1 -8 7.42 0.94 21 -1 -8 7.22 0.94 21 1 -7 0.49 0.47 21 -1 -7 1.07 0.53 21 1 -7 0.08 0.48 21 -1 -7 0.79 0.57 21 1 -6 8.80 1.04 21 -1 -6 10.75 1.13 21 1 -6 10.80 1.15 21 -1 -6 10.95 1.15 21 1 -5 3.45 0.72 21 -1 -5 2.77 0.70 21 1 -5 3.22 0.73 21 -1 -5 2.74 0.71 21 -1 -4 37.69 2.18 21 1 -4 37.76 2.14 21 -1 -4 39.21 2.22 21 1 -4 41.54 2.31 21 1 -3 2.11 0.59 21 -1 -3 1.91 0.63 21 1 -3 3.04 0.73 21 -1 -3 1.90 0.62 21 -1 -2 3.43 0.73 21 1 -2 2.47 0.66 21 -1 -2 3.71 0.72 21 1 -2 3.08 0.66 21 1 -2 2.69 0.65 21 -1 -1 -0.38 0.52 21 1 -1 0.24 0.42 21 -1 -1 0.07 0.46 21 -1 -1 0.46 0.45 21 1 -1 -0.31 0.45 21 -1 0 2.81 0.66 21 1 0 2.01 0.61 21 -1 0 2.79 0.63 21 -1 0 2.96 0.65 21 1 0 3.07 0.67 21 -1 1 6.46 0.87 21 1 1 5.47 0.86 21 -1 1 6.60 0.90 21 1 1 6.17 0.89 21 -1 2 7.14 0.88 21 1 2 7.40 0.92 21 -1 2 6.30 0.85 21 1 2 7.95 0.95 21 -1 3 0.19 0.35 21 1 3 0.20 0.36 21 -1 3 0.14 0.39 21 1 3 1.09 0.45 21 -1 4 -0.06 0.34 21 1 4 0.06 0.36 21 -1 4 -0.13 0.31 21 1 4 0.19 0.36 21 1 5 8.28 0.87 21 -1 5 7.87 0.83 21 1 5 7.05 0.79 21 -3 -12 9.47 0.87 21 3 -11 0.05 0.35 21 -3 -11 0.16 0.37 21 3 -10 1.79 0.50 21 3 -10 2.05 0.54 21 -3 -10 0.94 0.44 21 3 -9 1.71 0.52 21 3 -9 1.90 0.57 21 -3 -9 1.52 0.49 21 -3 -9 1.04 0.51 21 3 -8 0.49 0.43 21 3 -8 0.48 0.42 21 -3 -8 -0.25 0.43 21 3 -7 1.26 0.48 21 3 -7 1.34 0.56 21 -3 -7 2.13 0.57 21 -3 -6 11.07 1.11 21 3 -6 12.32 1.12 21 3 -6 11.65 1.16 21 3 -5 1.02 0.47 21 3 -5 1.24 0.56 21 -3 -5 0.77 0.52 21 -3 -4 11.66 1.16 21 3 -4 10.09 1.03 21 3 -4 11.88 1.16 21 3 -3 0.49 0.42 21 3 -3 0.07 0.41 21 -3 -3 0.69 0.51 21 3 -2 6.58 0.88 21 3 -2 6.75 0.93 21 -3 -2 6.04 0.85 21 3 -1 0.50 0.41 21 3 -1 0.58 0.48 21 -3 -1 0.59 0.43 21 -3 0 3.46 0.64 21 3 0 4.33 0.74 21 3 0 3.72 0.67 21 -3 0 2.73 0.58 21 -3 1 0.40 0.37 21 3 1 1.11 0.48 21 3 1 1.08 0.44 21 -3 1 0.98 0.41 21 -3 2 0.71 0.44 21 3 2 1.26 0.47 21 3 2 1.09 0.46 21 -3 3 1.76 0.48 21 3 3 2.24 0.53 21 3 3 0.83 0.41 21 -3 4 0.11 0.31 21 3 4 0.06 0.32 21 5 -9 1.30 0.42 21 5 -8 6.49 0.74 21 5 -8 7.23 0.80 21 -5 -7 0.42 0.34 21 5 -7 0.72 0.40 21 5 -7 0.85 0.42 21 -5 -7 0.48 0.37 21 -5 -6 4.89 0.68 21 5 -6 4.99 0.67 21 5 -6 4.25 0.67 21 -5 -6 5.09 0.70 21 -5 -5 3.76 0.60 21 5 -5 3.26 0.58 21 5 -5 4.61 0.69 21 -5 -5 3.28 0.61 21 -5 -4 0.05 0.32 21 -5 -4 0.06 0.38 21 5 -3 -0.06 0.34 21 -5 -3 0.05 0.31 21 -5 -3 -0.06 0.35 21 5 -2 0.24 0.34 21 -5 -2 0.23 0.34 21 5 -1 8.01 0.88 21 -5 -1 9.86 0.92 21 5 0 4.51 0.67 21 -5 0 5.53 0.69 21 5 1 0.11 0.35 21 -5 1 -0.10 0.30 22 0 -9 0.31 0.35 22 0 -8 3.36 0.58 22 0 -8 3.92 0.62 22 0 -7 0.23 0.35 22 0 -7 -0.06 0.39 22 0 -6 12.44 1.08 22 0 -6 12.85 1.11 22 0 -5 -0.12 0.37 22 0 -5 0.23 0.36 22 0 -4 0.37 0.40 22 0 -4 -0.06 0.37 22 0 -3 -0.19 0.41 22 0 -3 0.22 0.37 22 0 -2 7.03 0.84 22 0 -2 5.96 0.75 22 0 -1 -0.24 0.39 22 0 0 3.37 0.59 22 0 0 4.23 0.63 22 0 1 0.17 0.32 22 2 -8 2.40 0.52 22 2 -8 2.30 0.52 22 -2 -8 1.07 0.42 22 2 -7 0.05 0.33 22 2 -7 0.51 0.38 22 -2 -7 -0.05 0.35 22 2 -6 4.77 0.67 22 2 -6 5.87 0.77 22 -2 -6 4.37 0.66 22 2 -5 8.22 0.85 22 -2 -5 9.65 0.96 22 2 -5 10.36 1.00 22 2 -4 5.02 0.73 22 -2 -4 4.86 0.70 22 2 -4 5.72 0.73 22 2 -3 0.24 0.35 22 -2 -3 0.17 0.35 22 2 -2 0.12 0.36 22 -2 -2 0.37 0.37 22 -2 -1 10.35 0.90 22 2 -1 11.40 1.01 22 2 0 0.22 0.31 0 0 0 0.00 0.00 TITL MZL_auto in C2/c REM C2/c (#15 in standard setting) CELL 1.54184 18.692810 14.675721 21.809231 90.0000 99.3631 90.0000 ZERR 26.00 0.000215 0.000143 0.000265 0.0000 0.0012 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H N O UNIT 286.00 260.00 26.00 26.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 38530 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.665 _oxdiff_exptl_absorpt_empirical_full_min 0.760 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 O2 O 0.18745(6) 0.29672(8) 0.40821(5) 0.0581(3) Uani 1 1 d . . . . . O1 O 0.25592(8) 0.63920(9) 0.27821(6) 0.0675(4) Uani 1 1 d . . . . . H1 H 0.266274 0.623265 0.244697 0.101 Uiso 1 1 calc DGR . . . . O3 O 0.23230(7) 0.19335(10) 0.35010(6) 0.0735(4) Uani 1 1 d . . . . . O4 O 0.43398(7) 0.23277(10) 0.47137(7) 0.0749(4) Uani 1 1 d . . . . . C13 C 0.30080(9) 0.43732(11) 0.41253(7) 0.0507(4) Uani 1 1 d . U . . . C7 C 0.31771(8) 0.49676(11) 0.31167(7) 0.0499(4) Uani 1 1 d . U . . . C25 C 0.31121(9) 0.26940(11) 0.43237(7) 0.0490(4) Uani 1 1 d . U . . . C12 C 0.33058(9) 0.43181(12) 0.35865(7) 0.0507(4) Uani 1 1 d . U . . . H12 H 0.360467 0.382648 0.353579 0.061 Uiso 1 1 calc R . . . . C15 C 0.31590(10) 0.36302(11) 0.46224(7) 0.0534(4) Uani 1 1 d . U . . . H15 H 0.278597 0.366956 0.488927 0.064 Uiso 1 1 calc R . . . . C24 C 0.24166(9) 0.24683(11) 0.39257(7) 0.0499(4) Uani 1 1 d . U . . . C6 C 0.27280(9) 0.57037(11) 0.32097(7) 0.0517(4) Uani 1 1 d . U . . . C26 C 0.36792(9) 0.21206(12) 0.43692(8) 0.0554(4) Uani 1 1 d . U . . . C16 C 0.38942(11) 0.37640(13) 0.50266(8) 0.0607(4) Uani 1 1 d . U . . . C14 C 0.25700(10) 0.51095(12) 0.41981(8) 0.0562(4) Uani 1 1 d . U . . . H14 H 0.236949 0.515236 0.456032 0.067 Uiso 1 1 calc R . . . . C5 C 0.24159(10) 0.57899(12) 0.37522(8) 0.0567(4) Uani 1 1 d . U . . . C9 C 0.35150(9) 0.48652(13) 0.25228(8) 0.0581(4) Uani 1 1 d . U . . . C27 C 0.37301(9) 0.12083(13) 0.40763(8) 0.0583(4) Uani 1 1 d . U . . . H27 H 0.323889 0.102707 0.388742 0.070 Uiso 1 1 calc R . . . . C21 C 0.44377(11) 0.31331(14) 0.50380(9) 0.0654(5) Uani 1 1 d . U . . . C23 C 0.11830(10) 0.29182(15) 0.36758(9) 0.0673(5) Uani 1 1 d . U . . . H23A H 0.080321 0.312237 0.389810 0.081 Uiso 1 1 calc R . . . . H23B H 0.108245 0.229071 0.355092 0.081 Uiso 1 1 calc R . . . . C10 C 0.29182(12) 0.47539(15) 0.19513(9) 0.0701(5) Uani 1 1 d . U . . . H10A H 0.250439 0.446052 0.207348 0.105 Uiso 1 1 calc GR . . . . H10B H 0.309835 0.438907 0.164438 0.105 Uiso 1 1 calc GR . . . . H10C H 0.277977 0.534258 0.177999 0.105 Uiso 1 1 calc DGR . . . . C17 C 0.40497(13) 0.45408(16) 0.53908(9) 0.0770(5) Uani 1 1 d . U . . . H17 H 0.369420 0.498175 0.539992 0.092 Uiso 1 1 calc R . . . . C2 C 0.19317(13) 0.66065(14) 0.38493(10) 0.0730(5) Uani 1 1 d . U . . . C32 C 0.40247(12) 0.04761(14) 0.45486(10) 0.0716(5) Uani 1 1 d . U . . . H32A H 0.450669 0.064558 0.475231 0.086 Uiso 1 1 calc R . . . . H32B H 0.371480 0.043057 0.486344 0.086 Uiso 1 1 calc R . . . . C28 C 0.41873(13) 0.12571(16) 0.35605(10) 0.0765(5) Uani 1 1 d . U . . . H28A H 0.397310 0.169467 0.325077 0.092 Uiso 1 1 calc R . . . . H28B H 0.466936 0.147095 0.373217 0.092 Uiso 1 1 calc R . . . . C8 C 0.40052(11) 0.56850(17) 0.24400(10) 0.0778(6) Uani 1 1 d . U . . . H8A H 0.372577 0.623616 0.242080 0.117 Uiso 1 1 calc DGR . . . . H8B H 0.420047 0.561477 0.206191 0.117 Uiso 1 1 calc GR . . . . H8C H 0.439469 0.571499 0.278553 0.117 Uiso 1 1 calc GR . . . . C20 C 0.51242(12) 0.32558(17) 0.53870(10) 0.0790(6) Uani 1 1 d . U . . . H20 H 0.548195 0.281639 0.538305 0.095 Uiso 1 1 calc R . . . . C19 C 0.52665(14) 0.40280(18) 0.57349(10) 0.0862(6) Uani 1 1 d . U . . . H19 H 0.572463 0.411997 0.596575 0.103 Uiso 1 1 calc R . . . . C18 C 0.47394(15) 0.46605(18) 0.57435(10) 0.0865(6) Uani 1 1 d . U . . . H18 H 0.483712 0.518026 0.598667 0.104 Uiso 1 1 calc R . . . . C11 C 0.39871(13) 0.40070(18) 0.25487(10) 0.0851(7) Uani 1 1 d . U . . . H11A H 0.436039 0.403441 0.290703 0.128 Uiso 1 1 calc GR . . . . H11B H 0.420477 0.397154 0.217994 0.128 Uiso 1 1 calc GR . . . . H11C H 0.369182 0.347792 0.257550 0.128 Uiso 1 1 calc GR . . . . C29 C 0.42466(14) 0.03406(17) 0.32504(11) 0.0841(6) Uani 1 1 d . U . . . H29A H 0.457973 0.039061 0.295434 0.101 Uiso 1 1 calc R . . . . H29B H 0.377559 0.016909 0.302391 0.101 Uiso 1 1 calc R . . . . C31 C 0.40560(13) -0.04399(16) 0.42304(11) 0.0805(6) Uani 1 1 d . U . . . H31A H 0.425625 -0.089160 0.453541 0.097 Uiso 1 1 calc R . . . . H31B H 0.356856 -0.062926 0.405440 0.097 Uiso 1 1 calc R . . . . C30 C 0.45130(13) -0.03959(18) 0.37241(12) 0.0854(6) Uani 1 1 d . U . . . H30A H 0.449951 -0.098133 0.351614 0.102 Uiso 1 1 calc R . . . . H30B H 0.501202 -0.027133 0.390630 0.102 Uiso 1 1 calc R . . . . C3 C 0.12670(14) 0.66526(19) 0.33344(12) 0.0926(7) Uani 1 1 d . U . . . H3A H 0.142154 0.677232 0.294339 0.139 Uiso 1 1 calc GR . . . . H3B H 0.095100 0.713210 0.342525 0.139 Uiso 1 1 calc GR . . . . H3C H 0.101279 0.608211 0.331240 0.139 Uiso 1 1 calc GR . . . . C22 C 0.11805(14) 0.3494(2) 0.31127(12) 0.0982(8) Uani 1 1 d . U . . . H22A H 0.070335 0.349553 0.287033 0.147 Uiso 1 1 calc GR . . . . H22B H 0.151945 0.325138 0.286846 0.147 Uiso 1 1 calc GR . . . . H22C H 0.131714 0.410555 0.323655 0.147 Uiso 1 1 calc GR . . . . C1 C 0.23746(18) 0.74887(16) 0.38726(13) 0.1026(8) Uani 1 1 d . U . . . H1A H 0.279445 0.743886 0.418919 0.154 Uiso 1 1 calc GR . . . . H1B H 0.208214 0.799179 0.396581 0.154 Uiso 1 1 calc GR . . . . H1C H 0.252469 0.758778 0.347733 0.154 Uiso 1 1 calc GR . . . . C4 C 0.16356(18) 0.65251(18) 0.44638(12) 0.1038(8) Uani 1 1 d . U . . . H4A H 0.137142 0.596475 0.446775 0.156 Uiso 1 1 calc GR . . . . H4B H 0.131878 0.702901 0.450321 0.156 Uiso 1 1 calc GR . . . . H4C H 0.203158 0.653065 0.480475 0.156 Uiso 1 1 calc GR . . . . 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 O2 0.0516(6) 0.0651(7) 0.0580(7) -0.0038(6) 0.0099(5) 0.0029(5) O1 0.0854(9) 0.0640(8) 0.0559(7) 0.0158(6) 0.0201(6) 0.0119(6) O3 0.0604(7) 0.0808(9) 0.0716(8) -0.0257(7) -0.0118(6) 0.0146(6) O4 0.0548(7) 0.0742(9) 0.0867(10) -0.0089(7) -0.0156(7) -0.0052(6) C13 0.0593(8) 0.0497(8) 0.0429(7) 0.0007(6) 0.0072(6) -0.0078(6) C7 0.0485(8) 0.0566(8) 0.0447(8) 0.0029(6) 0.0077(6) -0.0048(6) C25 0.0531(8) 0.0514(8) 0.0415(7) 0.0054(6) 0.0048(6) -0.0058(6) C12 0.0519(8) 0.0544(8) 0.0454(7) 0.0024(6) 0.0073(6) -0.0036(7) C15 0.0628(8) 0.0551(8) 0.0420(7) 0.0026(6) 0.0079(6) -0.0086(7) C24 0.0508(8) 0.0521(8) 0.0465(8) 0.0034(7) 0.0068(6) 0.0012(7) C6 0.0580(8) 0.0510(8) 0.0460(8) 0.0051(6) 0.0084(6) -0.0054(7) C26 0.0502(8) 0.0601(8) 0.0527(8) 0.0062(7) -0.0016(7) -0.0052(7) C16 0.0755(9) 0.0636(9) 0.0405(7) 0.0045(7) 0.0022(7) -0.0199(8) C14 0.0719(9) 0.0535(8) 0.0455(8) -0.0017(6) 0.0165(7) -0.0052(7) C5 0.0714(9) 0.0502(8) 0.0502(8) -0.0016(7) 0.0144(7) -0.0012(7) C9 0.0543(9) 0.0720(10) 0.0495(8) 0.0083(7) 0.0132(7) 0.0045(8) C27 0.0506(8) 0.0616(9) 0.0601(9) 0.0025(7) 0.0012(7) 0.0029(7) C21 0.0681(9) 0.0701(10) 0.0534(9) 0.0053(8) -0.0037(8) -0.0157(8) C23 0.0489(9) 0.0793(12) 0.0724(11) 0.0003(10) 0.0057(8) 0.0078(9) C10 0.0761(12) 0.0828(13) 0.0509(10) -0.0029(9) 0.0086(9) 0.0037(10) C17 0.0960(12) 0.0769(11) 0.0535(9) -0.0039(8) -0.0012(9) -0.0176(10) C2 0.1027(12) 0.0575(10) 0.0638(10) 0.0005(8) 0.0286(8) 0.0106(9) C32 0.0743(10) 0.0685(10) 0.0715(10) 0.0095(9) 0.0099(9) 0.0093(9) C28 0.0804(11) 0.0798(11) 0.0702(10) 0.0061(9) 0.0150(9) 0.0026(9) C8 0.0565(10) 0.1090(16) 0.0702(12) 0.0223(11) 0.0176(9) -0.0069(10) C20 0.0753(11) 0.0894(12) 0.0652(10) 0.0050(10) -0.0099(9) -0.0238(10) C19 0.0884(13) 0.0978(13) 0.0645(11) 0.0042(10) -0.0116(10) -0.0288(11) C18 0.1069(14) 0.0888(13) 0.0572(10) -0.0081(10) -0.0069(10) -0.0329(11) C11 0.0870(14) 0.1058(16) 0.0690(12) 0.0142(12) 0.0319(11) 0.0324(12) C29 0.0846(12) 0.0910(13) 0.0792(12) -0.0052(10) 0.0205(10) 0.0104(11) C31 0.0836(12) 0.0701(11) 0.0862(12) 0.0069(10) 0.0094(10) 0.0157(10) C30 0.0775(11) 0.0842(12) 0.0935(13) -0.0062(11) 0.0114(10) 0.0220(10) C3 0.0957(14) 0.0970(16) 0.0893(14) 0.0093(13) 0.0276(10) 0.0320(13) C22 0.0813(15) 0.118(2) 0.0900(17) 0.0249(15) -0.0019(13) 0.0222(14) C1 0.154(2) 0.0587(12) 0.0970(16) -0.0069(12) 0.0258(16) 0.0028(14) C4 0.156(2) 0.0841(15) 0.0829(15) 0.0027(12) 0.0539(15) 0.0384(15) 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' 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 O2 C23 117.08(14) . . ? C6 O1 H1 109.5 . . ? C26 O4 C21 120.36(15) . . ? C12 C13 C15 120.46(15) . . ? C14 C13 C12 118.17(15) . . ? C14 C13 C15 121.37(14) . . ? C12 C7 C6 117.18(14) . . ? C12 C7 C9 120.51(15) . . ? C6 C7 C9 122.31(14) . . ? C24 C25 C15 116.04(14) . . ? C26 C25 C15 123.05(15) . . ? C26 C25 C24 120.70(15) . . ? C13 C12 C7 122.73(16) . . ? C13 C12 H12 118.6 . . ? C7 C12 H12 118.6 . . ? C13 C15 H15 108.2 . . ? C25 C15 C13 110.48(13) . . ? C25 C15 H15 108.2 . . ? C25 C15 C16 110.47(15) . . ? C16 C15 C13 111.33(13) . . ? C16 C15 H15 108.2 . . ? O2 C24 C25 110.95(14) . . ? O3 C24 O2 122.06(15) . . ? O3 C24 C25 126.96(15) . . ? O1 C6 C7 122.94(14) . . ? O1 C6 C5 115.02(15) . . ? C7 C6 C5 122.04(15) . . ? O4 C26 C27 108.60(15) . . ? C25 C26 O4 122.06(16) . . ? C25 C26 C27 129.34(15) . . ? C21 C16 C15 121.36(16) . . ? C21 C16 C17 117.19(18) . . ? C17 C16 C15 121.44(19) . . ? C13 C14 H14 118.6 . . ? C13 C14 C5 122.74(15) . . ? C5 C14 H14 118.6 . . ? C6 C5 C2 121.33(15) . . ? C14 C5 C6 117.14(16) . . ? C14 C5 C2 121.53(15) . . ? C7 C9 C10 110.44(14) . . ? C7 C9 C8 110.85(16) . . ? C10 C9 C8 110.75(16) . . ? C11 C9 C7 111.21(15) . . ? C11 C9 C10 106.23(17) . . ? C11 C9 C8 107.22(17) . . ? C26 C27 H27 107.6 . . ? C26 C27 C32 112.53(15) . . ? C26 C27 C28 110.90(16) . . ? C32 C27 H27 107.6 . . ? C28 C27 H27 107.6 . . ? C28 C27 C32 110.33(16) . . ? O4 C21 C20 115.2(2) . . ? C16 C21 O4 122.34(16) . . ? C16 C21 C20 122.4(2) . . ? O2 C23 H23A 109.4 . . ? O2 C23 H23B 109.4 . . ? O2 C23 C22 111.08(17) . . ? H23A C23 H23B 108.0 . . ? C22 C23 H23A 109.4 . . ? C22 C23 H23B 109.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C17 H17 119.9 . . ? C16 C17 C18 120.2(2) . . ? C18 C17 H17 119.9 . . ? C3 C2 C5 110.99(17) . . ? C3 C2 C4 106.2(2) . . ? C1 C2 C5 109.63(19) . . ? C1 C2 C3 110.8(2) . . ? C1 C2 C4 107.8(2) . . ? C4 C2 C5 111.32(17) . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? C31 C32 C27 110.55(17) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C27 C28 H28A 109.2 . . ? C27 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C29 C28 C27 112.23(18) . . ? C29 C28 H28A 109.2 . . ? C29 C28 H28B 109.2 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C21 C20 H20 120.3 . . ? C19 C20 C21 119.3(2) . . ? C19 C20 H20 120.3 . . ? C20 C19 H19 120.0 . . ? C18 C19 C20 120.0(2) . . ? C18 C19 H19 120.0 . . ? C17 C18 H18 119.6 . . ? C19 C18 C17 120.8(2) . . ? C19 C18 H18 119.6 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C28 C29 H29A 109.3 . . ? C28 C29 H29B 109.3 . . ? C28 C29 C30 111.49(19) . . ? H29A C29 H29B 108.0 . . ? C30 C29 H29A 109.3 . . ? C30 C29 H29B 109.3 . . ? C32 C31 H31A 109.3 . . ? C32 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? C30 C31 C32 111.5(2) . . ? C30 C31 H31A 109.3 . . ? C30 C31 H31B 109.3 . . ? C29 C30 H30A 109.3 . . ? C29 C30 H30B 109.3 . . ? C31 C30 C29 111.52(18) . . ? C31 C30 H30A 109.3 . . ? C31 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? 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 O2 C24 1.339(2) . ? O2 C23 1.445(2) . ? O1 H1 0.8200 . ? O1 C6 1.3763(19) . ? O3 C24 1.205(2) . ? O4 C26 1.371(2) . ? O4 C21 1.374(2) . ? C13 C12 1.382(2) . ? C13 C15 1.531(2) . ? C13 C14 1.380(2) . ? C7 C12 1.391(2) . ? C7 C6 1.403(2) . ? C7 C9 1.538(2) . ? C25 C15 1.517(2) . ? C25 C24 1.479(2) . ? C25 C26 1.344(2) . ? C12 H12 0.9300 . ? C15 H15 0.9800 . ? C15 C16 1.520(2) . ? C6 C5 1.407(2) . ? C26 C27 1.493(3) . ? C16 C21 1.372(3) . ? C16 C17 1.393(3) . ? C14 H14 0.9300 . ? C14 C5 1.391(2) . ? C5 C2 1.537(3) . ? C9 C10 1.540(3) . ? C9 C8 1.541(3) . ? C9 C11 1.534(3) . ? C27 H27 0.9800 . ? C27 C32 1.528(3) . ? C27 C28 1.521(3) . ? C21 C20 1.393(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 C22 1.490(3) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C17 H17 0.9300 . ? C17 C18 1.401(3) . ? C2 C3 1.535(3) . ? C2 C1 1.533(3) . ? C2 C4 1.536(3) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 C31 1.518(3) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 C29 1.518(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C20 H20 0.9300 . ? C20 C19 1.366(3) . ? C19 H19 0.9300 . ? C19 C18 1.356(4) . ? C18 H18 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 C30 1.522(3) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 C30 1.503(3) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? 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 C6 C5 C14 179.90(15) . . . . ? O1 C6 C5 C2 -0.7(3) . . . . ? O4 C26 C27 C32 52.8(2) . . . . ? O4 C26 C27 C28 -71.34(19) . . . . ? O4 C21 C20 C19 -178.64(19) . . . . ? C13 C15 C16 C21 -116.50(18) . . . . ? C13 C15 C16 C17 62.1(2) . . . . ? C13 C14 C5 C6 0.0(3) . . . . ? C13 C14 C5 C2 -179.42(18) . . . . ? C7 C6 C5 C14 -0.1(3) . . . . ? C7 C6 C5 C2 179.34(17) . . . . ? C25 C15 C16 C21 6.6(2) . . . . ? C25 C15 C16 C17 -174.73(16) . . . . ? C25 C26 C27 C32 -128.1(2) . . . . ? C25 C26 C27 C28 107.8(2) . . . . ? C12 C13 C15 C25 -42.8(2) . . . . ? C12 C13 C15 C16 80.32(19) . . . . ? C12 C13 C14 C5 0.3(3) . . . . ? C12 C7 C6 O1 179.88(15) . . . . ? C12 C7 C6 C5 -0.1(2) . . . . ? C12 C7 C9 C10 116.61(18) . . . . ? C12 C7 C9 C8 -120.26(18) . . . . ? C12 C7 C9 C11 -1.1(2) . . . . ? C15 C13 C12 C7 179.03(15) . . . . ? C15 C13 C14 C5 -179.26(16) . . . . ? C15 C25 C24 O2 -23.66(19) . . . . ? C15 C25 C24 O3 154.34(17) . . . . ? C15 C25 C26 O4 2.8(3) . . . . ? C15 C25 C26 C27 -176.28(16) . . . . ? C15 C16 C21 O4 -3.5(3) . . . . ? C15 C16 C21 C20 177.61(17) . . . . ? C15 C16 C17 C18 -177.93(18) . . . . ? C24 O2 C23 C22 -78.7(2) . . . . ? C24 C25 C15 C13 -57.46(18) . . . . ? C24 C25 C15 C16 178.91(13) . . . . ? C24 C25 C26 O4 177.23(15) . . . . ? C24 C25 C26 C27 -1.8(3) . . . . ? C6 C7 C12 C13 0.4(2) . . . . ? C6 C7 C9 C10 -63.0(2) . . . . ? C6 C7 C9 C8 60.1(2) . . . . ? C6 C7 C9 C11 179.32(17) . . . . ? C6 C5 C2 C3 59.9(3) . . . . ? C6 C5 C2 C1 -62.9(3) . . . . ? C6 C5 C2 C4 177.9(2) . . . . ? C26 O4 C21 C16 -1.0(3) . . . . ? C26 O4 C21 C20 178.01(17) . . . . ? C26 C25 C15 C13 117.25(17) . . . . ? C26 C25 C15 C16 -6.4(2) . . . . ? C26 C25 C24 O2 161.50(15) . . . . ? C26 C25 C24 O3 -20.5(3) . . . . ? C26 C27 C32 C31 179.19(17) . . . . ? C26 C27 C28 C29 -179.70(17) . . . . ? C16 C21 C20 C19 0.4(3) . . . . ? C16 C17 C18 C19 0.3(3) . . . . ? C14 C13 C12 C7 -0.5(2) . . . . ? C14 C13 C15 C25 136.72(17) . . . . ? C14 C13 C15 C16 -100.1(2) . . . . ? C14 C5 C2 C3 -120.7(2) . . . . ? C14 C5 C2 C1 116.5(2) . . . . ? C14 C5 C2 C4 -2.7(3) . . . . ? C9 C7 C12 C13 -179.20(15) . . . . ? C9 C7 C6 O1 -0.5(3) . . . . ? C9 C7 C6 C5 179.50(16) . . . . ? C27 C32 C31 C30 57.5(2) . . . . ? C27 C28 C29 C30 -53.4(3) . . . . ? C21 O4 C26 C25 1.4(3) . . . . ? C21 O4 C26 C27 -179.40(16) . . . . ? C21 C16 C17 C18 0.8(3) . . . . ? C21 C20 C19 C18 0.7(3) . . . . ? C23 O2 C24 O3 -7.0(2) . . . . ? C23 O2 C24 C25 171.16(14) . . . . ? C17 C16 C21 O4 177.84(18) . . . . ? C17 C16 C21 C20 -1.1(3) . . . . ? C32 C27 C28 C29 54.9(2) . . . . ? C32 C31 C30 C29 -55.9(3) . . . . ? C28 C27 C32 C31 -56.4(2) . . . . ? C28 C29 C30 C31 53.5(3) . . . . ? C20 C19 C18 C17 -1.1(4) . . . . ?