#------------------------------------------------------------------------------ #$Date: 2021-07-28 04:29:40 +0300 (Wed, 28 Jul 2021) $ #$Revision: 267771 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/42/1564256.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_1564256 loop_ _publ_author_name 'Wang, Haiying' 'Yang, Weiwei' 'Baldridge, Kim K.' 'Zhan, Cai-Hong' 'Thikekar, Tushar Ulhas' 'Sue, Andrew C.-H.' _publ_section_title ; Spontaneous and induced chiral symmetry breaking of stereolabile pillar[5]arene derivatives upon crystallisation ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC02560K _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_moiety 'C43 H46 O10, C5 H10 O3' _chemical_formula_sum 'C48 H56 O13' _chemical_formula_weight 840.92 _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_Hall 'C 2y' _space_group_name_H-M_alt 'C 1 2 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2018-12-04 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-03-27 deposited with the CCDC. 2021-07-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 98.7260(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 21.2498(2) _cell_length_b 11.99340(10) _cell_length_c 17.88350(10) _cell_measurement_reflns_used 31207 _cell_measurement_temperature 200.00(10) _cell_measurement_theta_max 74.2060 _cell_measurement_theta_min 2.4810 _cell_volume 4504.99(6) _computing_cell_refinement 'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)' _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 (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 200.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.981 _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 -67.00 27.00 0.50 0.71 -- -46.12 71.00 12.00 188 2 \w -61.00 29.00 0.50 0.71 -- -46.12 19.00 0.00 180 3 \w -26.00 67.00 0.50 0.71 -- 46.12 -71.00-118.00 186 4 \w 29.00 123.00 0.50 2.85 -- 101.75 -71.00-118.00 188 5 \w 87.00 174.00 0.50 2.85 -- 101.75 45.00-180.00 174 6 \w 81.00 175.00 0.50 2.85 -- 101.75 71.00 12.00 188 7 \w 78.00 175.00 0.50 2.85 -- 101.75 77.00 90.00 194 8 \w 29.00 117.00 0.50 2.85 -- 101.75-125.00 30.00 176 9 \w 29.00 116.00 0.50 2.85 -- 101.75 -45.00-120.00 174 10 \w 25.00 118.00 0.50 0.71 -- 46.12 71.00 12.00 186 11 \w 29.00 116.00 0.50 2.85 -- 101.75 -45.00 -30.00 174 12 \w 29.00 109.00 0.50 2.85 -- 101.75 -94.00 90.00 160 13 \w 20.00 95.00 0.50 0.71 -- 46.12-125.00-150.00 150 14 \w 23.00 118.00 0.50 0.71 -- 46.12 77.00 90.00 190 15 \w -118.00 -25.00 0.50 0.71 -- -46.12 -71.00-118.00 186 16 \w -118.00 -73.00 0.50 0.71 -- -46.12-125.00-150.00 90 17 \w -118.00 -73.00 0.50 0.71 -- -46.12-125.00 -30.00 90 18 \w -118.00 -73.00 0.50 0.71 -- -46.12-125.00 60.00 90 19 \w -118.00 -22.00 0.50 0.71 -- -46.12 -77.00 -30.00 192 20 \w -115.00 -25.00 0.50 2.85 -- -100.00 30.00 -60.00 180 21 \w -117.00 -27.00 0.50 2.85 -- -100.00 61.00 120.00 180 22 \w -121.00 -27.00 0.50 2.85 -- -100.00 71.00 12.00 188 23 \w -173.00 -79.00 0.50 2.85 -- -100.00 -71.00-118.00 188 24 \w -173.00 -82.00 0.50 2.85 -- -100.00 -61.00 -30.00 182 25 \w -176.00 -82.00 0.50 2.85 -- -100.00 -15.00 120.00 188 26 \w -175.00 -84.00 0.50 2.85 -- -100.00 -30.00 90.00 182 27 \w -172.00 -85.00 0.50 2.85 -- -100.00 -45.00 -60.00 174 28 \w -176.00 -82.00 0.50 2.85 -- -100.00 -15.00-150.00 188 29 \w -173.00 -82.00 0.50 2.85 -- -100.00 -61.00 -60.00 182 30 \w -172.00 -85.00 0.50 2.85 -- -100.00 -45.00-180.00 174 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'ROD, Synergy Custom system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0056570000 _diffrn_orient_matrix_UB_12 -0.0615722000 _diffrn_orient_matrix_UB_13 -0.0742868000 _diffrn_orient_matrix_UB_21 -0.0478631000 _diffrn_orient_matrix_UB_22 0.0820628000 _diffrn_orient_matrix_UB_23 -0.0437435000 _diffrn_orient_matrix_UB_31 0.0552801000 _diffrn_orient_matrix_UB_32 0.0773088000 _diffrn_orient_matrix_UB_33 -0.0127704000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_unetI/netI 0.0179 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 42011 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.967 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.584 _diffrn_reflns_theta_min 2.500 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.737 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.95171 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.240 _exptl_crystal_description block _exptl_crystal_F_000 1792 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.332 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.038 _refine_ls_abs_structure_details ; Flack x determined using 3786 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 563 _refine_ls_number_reflns 8931 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0401 _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^)+(0.0755P)^2^+1.2004P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1126 _refine_ls_wR_factor_ref 0.1146 _reflns_Friedel_coverage 0.877 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.952 _reflns_number_gt 8567 _reflns_number_total 8931 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc02560k2.cif _cod_data_source_block dijydroxy_p5 _cod_database_code 1564256 _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 0.930 _shelx_estimated_absorpt_t_min 0.867 _reflns_odcompleteness_completeness 100.00 _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.a Ternary CH refined with riding coordinates: C43(H43) 2.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C47(H47A,H47B), C48(H48A,H48B), C33(H33A,H33B), C18(H18A,H18B), C45(H45A,H45B) 2.c Aromatic/amide H refined with riding coordinates: C6(H6), C11(H11), C35(H35), C26(H26), C14(H14), C3(H3), C38(H38), C24(H24), C29(H29), C21(H21) 2.d Idealised Me refined as rotating group: C32(H32A,H32B,H32C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C41(H41A,H41B, H41C), C31(H31A,H31B,H31C), C8(H8A,H8B,H8C), C40(H40A,H40B,H40C), C9(H9A,H9B, H9C), C46(H46A,H46B,H46C), C42(H42A,H42B,H42C) 2.e Idealised tetrahedral OH refined as rotating group: O9(H9), O8(H8), O1(H1) ; _shelx_res_file ; TITL dijydroxy_p5_a.res in C2 dijydroxy_p5.res created by SHELXL-2018/3 at 09:28:51 on 04-Dec-2018 REM Old TITL DIJYDROXY_P5 in C2/m REM SHELXT solution in C2 REM R1 0.126, Rweak 0.046, Alpha 0.006, Orientation as input REM Flack x = 0.115 ( 0.075 ) from Parsons' quotients REM Formula found by SHELXT: C50 N3 O8 CELL 1.54184 21.2498 11.9934 17.8835 90 98.726 90 ZERR 4 0.0002 0.0001 0.0001 0 0.001 0 LATT -7 SYMM -X,+Y,-Z SFAC C H O UNIT 192 224 52 L.S. 10 PLAN 20 SIZE 0.1 0.1 0.2 BOND $H list 4 fmap 2 acta OMIT -13 13 1 OMIT -13 13 2 OMIT -21 7 11 OMIT -8 14 2 OMIT -13 13 3 OMIT -13 13 4 OMIT -8 14 3 OMIT -4 14 2 OMIT -23 5 11 OMIT -6 14 3 OMIT -11 13 6 OMIT -6 14 4 REM REM REM WGHT 0.075500 1.200400 FVAR 0.27247 O11 3 0.514461 0.612936 0.390760 11.00000 0.05563 0.05923 = 0.03484 -0.00898 0.00315 -0.01259 O4 3 0.189892 0.242547 0.246890 11.00000 0.06025 0.03935 = 0.04123 -0.00649 0.00292 0.01013 O6 3 0.070098 0.521664 0.076165 11.00000 0.05792 0.04952 = 0.04628 -0.01872 0.00283 -0.00205 O7 3 0.178937 0.915800 0.192609 11.00000 0.05846 0.04715 = 0.05803 -0.01370 0.01234 -0.01112 O13 3 0.304741 0.436149 0.487453 11.00000 0.05246 0.05900 = 0.04700 -0.01722 0.01204 -0.00786 O9 3 0.381762 0.615004 -0.003204 11.00000 0.06050 0.08325 = 0.04180 -0.00878 -0.00293 0.00799 AFIX 147 H9 2 0.413532 0.583508 0.018771 11.00000 -1.50000 AFIX 0 O12 3 0.423498 0.218490 0.275313 11.00000 0.04224 0.06769 = 0.07946 -0.03735 0.01161 -0.00530 O10 3 0.467170 0.485854 0.089847 11.00000 0.06195 0.07498 = 0.03803 -0.01397 -0.00327 0.00752 O5 3 0.093810 0.612862 0.375778 11.00000 0.07068 0.06116 = 0.05309 -0.02313 -0.00128 0.02021 O8 3 0.299314 0.954123 0.166587 11.00000 0.06380 0.05899 = 0.06636 -0.01215 0.00906 -0.01164 AFIX 147 H8 2 0.261428 0.947610 0.169926 11.00000 -1.50000 AFIX 0 C7 1 0.164333 0.335028 0.277477 11.00000 0.03726 0.03273 = 0.03902 -0.00339 0.00931 -0.00385 C34 1 0.427837 0.352811 0.372436 11.00000 0.03816 0.03968 = 0.03876 0.00129 -0.00250 0.00021 C12 1 0.151031 0.816684 0.164502 11.00000 0.04108 0.03882 = 0.04307 -0.00461 -0.00086 0.00120 C25 1 0.485407 0.628004 0.180996 11.00000 0.03446 0.06105 = 0.03788 -0.00164 0.00402 -0.00717 C5 1 0.096543 0.498082 0.269978 11.00000 0.03084 0.03951 = 0.04319 -0.00667 0.00686 -0.00326 C6 1 0.120170 0.404769 0.236573 11.00000 0.03661 0.03819 = 0.03610 -0.00631 0.00485 -0.00398 AFIX 43 H6 2 0.105896 0.389348 0.185872 11.00000 -1.20000 AFIX 0 C10 1 0.087321 0.651630 0.175292 11.00000 0.03331 0.04062 = 0.03976 -0.00682 -0.00195 0.00933 C27 1 0.502691 0.583559 0.314963 11.00000 0.03077 0.05578 = 0.03616 -0.00601 0.00406 -0.00730 C11 1 0.113718 0.751461 0.204747 11.00000 0.03923 0.04123 = 0.03827 -0.00765 0.00171 0.00631 AFIX 43 H11 2 0.106264 0.774952 0.252184 11.00000 -1.20000 AFIX 0 C35 1 0.398557 0.408876 0.425658 11.00000 0.04167 0.03643 = 0.03428 0.00157 -0.00395 -0.00381 AFIX 43 H35 2 0.421050 0.463476 0.455513 11.00000 -1.20000 AFIX 0 C2 1 0.185671 0.355046 0.354078 11.00000 0.03681 0.03688 = 0.03774 0.00113 0.00749 -0.00791 C37 1 0.301547 0.303025 0.391099 11.00000 0.04105 0.03429 = 0.03578 0.00486 0.00132 -0.00147 C1 1 0.233296 0.277405 0.399374 11.00000 0.04390 0.03802 = 0.03758 0.00219 0.00669 -0.00718 AFIX 23 H1A 2 0.228648 0.282583 0.452388 11.00000 -1.20000 H1B 2 0.223652 0.201325 0.383132 11.00000 -1.20000 AFIX 0 C36 1 0.336055 0.384958 0.435263 11.00000 0.04415 0.03586 = 0.03165 0.00117 0.00197 0.00015 C39 1 0.392958 0.270872 0.328226 11.00000 0.03932 0.04157 = 0.05073 -0.00799 0.00298 0.00216 C28 1 0.494095 0.470423 0.299295 11.00000 0.02718 0.05053 = 0.04254 -0.00289 0.00103 -0.00171 C4 1 0.118272 0.518789 0.346359 11.00000 0.04062 0.04409 = 0.04398 -0.01110 0.00837 0.00047 C26 1 0.498749 0.660771 0.256735 11.00000 0.03780 0.05063 = 0.04077 -0.00436 0.00464 -0.00815 AFIX 43 H26 2 0.505114 0.735913 0.268322 11.00000 -1.20000 AFIX 0 C14 1 0.136147 0.684940 0.063808 11.00000 0.04542 0.05139 = 0.03331 -0.00434 -0.00165 0.00948 AFIX 43 H14 2 0.143492 0.661914 0.016229 11.00000 -1.20000 AFIX 0 C47 1 0.051405 0.577030 0.221927 11.00000 0.03087 0.04592 = 0.04561 -0.01062 0.00142 0.00241 AFIX 23 H47A 2 0.020010 0.534272 0.188697 11.00000 -1.20000 H47B 2 0.029115 0.622300 0.254445 11.00000 -1.20000 AFIX 0 C15 1 0.098346 0.619577 0.103046 11.00000 0.03899 0.04180 = 0.03851 -0.00841 -0.00339 0.00777 C48 1 0.474775 0.715524 0.119276 11.00000 0.04583 0.07054 = 0.04124 0.00620 0.00702 -0.01284 AFIX 23 H48A 2 0.489647 0.686988 0.074306 11.00000 -1.20000 H48B 2 0.499661 0.781280 0.135719 11.00000 -1.20000 AFIX 0 C13 1 0.163377 0.783894 0.093545 11.00000 0.04175 0.04729 = 0.03707 0.00255 -0.00240 0.00655 C20 1 0.318023 0.866670 0.125306 11.00000 0.05514 0.04828 = 0.04021 0.00394 0.00745 -0.01215 C3 1 0.161343 0.447452 0.387626 11.00000 0.04215 0.04741 = 0.03671 -0.00620 0.00613 -0.00517 AFIX 43 H3 2 0.174396 0.461273 0.438799 11.00000 -1.20000 AFIX 0 C23 1 0.363093 0.696562 0.042659 11.00000 0.05113 0.05996 = 0.03002 0.00624 0.00369 -0.00209 C38 1 0.331462 0.246513 0.338685 11.00000 0.04116 0.03591 = 0.04810 -0.00583 -0.00014 -0.00248 AFIX 43 H38 2 0.309406 0.190535 0.309730 11.00000 -1.20000 AFIX 0 C24 1 0.299992 0.729865 0.027520 11.00000 0.04979 0.05867 = 0.03116 0.00485 -0.00014 -0.00610 AFIX 43 H24 2 0.272809 0.694015 -0.010652 11.00000 -1.20000 AFIX 0 C29 1 0.483058 0.437567 0.223665 11.00000 0.03804 0.05233 = 0.04474 -0.00948 -0.00289 -0.00044 AFIX 43 H29 2 0.478380 0.362213 0.211850 11.00000 -1.20000 AFIX 0 C19 1 0.276028 0.815523 0.067804 11.00000 0.04876 0.05197 = 0.03464 0.00989 0.00348 -0.00708 O3 3 0.199121 0.203202 0.711699 11.00000 0.09135 0.10709 = 0.07860 -0.02165 0.03142 -0.00833 C22 1 0.404954 0.748140 0.099666 11.00000 0.04720 0.05864 = 0.03445 0.01051 0.00514 -0.01109 C30 1 0.478934 0.515377 0.165730 11.00000 0.03439 0.06587 = 0.03566 -0.00877 -0.00148 0.00051 C21 1 0.380749 0.832521 0.140346 11.00000 0.05084 0.05638 = 0.03878 0.00309 0.00515 -0.01794 AFIX 43 H21 2 0.407799 0.867299 0.179149 11.00000 -1.20000 AFIX 0 C33 1 0.494992 0.383262 0.360722 11.00000 0.03540 0.04954 = 0.04608 -0.00044 -0.00335 -0.00162 AFIX 23 H33A 2 0.518316 0.411768 0.407660 11.00000 -1.20000 H33B 2 0.516744 0.317059 0.346807 11.00000 -1.20000 AFIX 0 C32 1 0.542864 0.718768 0.408695 11.00000 0.06787 0.05547 = 0.04812 -0.01244 -0.00561 -0.00192 AFIX 137 H32A 2 0.513800 0.776522 0.388752 11.00000 -1.50000 H32B 2 0.581280 0.724774 0.386816 11.00000 -1.50000 H32C 2 0.552699 0.726500 0.462634 11.00000 -1.50000 AFIX 0 O1 3 0.209481 0.441372 0.592943 11.00000 0.10038 0.14009 = 0.07260 0.00430 0.02515 -0.00164 AFIX 147 H1 2 0.217110 0.402581 0.557639 11.00000 -1.50000 AFIX 0 C18 1 0.206451 0.850183 0.049703 11.00000 0.05387 0.05473 = 0.03844 0.00818 -0.00021 0.00251 AFIX 23 H18A 2 0.202838 0.928737 0.061241 11.00000 -1.20000 H18B 2 0.192156 0.840379 -0.004029 11.00000 -1.20000 AFIX 0 C16 1 0.084566 0.479836 0.006383 11.00000 0.06813 0.07042 = 0.05904 -0.03275 0.00786 0.00105 AFIX 137 H16A 2 0.067663 0.529398 -0.033849 11.00000 -1.50000 H16B 2 0.065901 0.407309 -0.002924 11.00000 -1.50000 H16C 2 0.129907 0.474546 0.008786 11.00000 -1.50000 AFIX 0 C17 1 0.160398 0.960779 0.259748 11.00000 0.05726 0.04950 = 0.05807 -0.01613 0.00770 -0.00734 AFIX 137 H17A 2 0.115404 0.974849 0.251507 11.00000 -1.50000 H17B 2 0.182841 1.029288 0.272506 11.00000 -1.50000 H17C 2 0.170463 0.908497 0.300453 11.00000 -1.50000 AFIX 0 C41 1 0.335072 0.528349 0.526265 11.00000 0.06856 0.06463 = 0.07246 -0.03127 0.01487 -0.00719 AFIX 137 H41A 2 0.342987 0.584300 0.490447 11.00000 -1.50000 H41B 2 0.374722 0.504957 0.555021 11.00000 -1.50000 H41C 2 0.308178 0.558624 0.559779 11.00000 -1.50000 AFIX 0 C31 1 0.453837 0.371174 0.073468 11.00000 0.08591 0.08572 = 0.05412 -0.03052 -0.01539 0.00859 AFIX 137 H31A 2 0.440081 0.362197 0.020151 11.00000 -1.50000 H31B 2 0.420842 0.346290 0.100707 11.00000 -1.50000 H31C 2 0.491611 0.327815 0.088516 11.00000 -1.50000 AFIX 0 C8 1 0.171493 0.222915 0.168919 11.00000 0.09437 0.05986 = 0.04039 -0.00988 0.00783 0.02758 AFIX 137 H8A 2 0.180588 0.287713 0.140909 11.00000 -1.50000 H8B 2 0.126682 0.207390 0.159017 11.00000 -1.50000 H8C 2 0.194680 0.160271 0.153732 11.00000 -1.50000 AFIX 0 C40 1 0.386240 0.148532 0.223177 11.00000 0.05151 0.11703 = 0.11081 -0.07546 0.01346 -0.00947 AFIX 137 H40A 2 0.411623 0.121069 0.187088 11.00000 -1.50000 H40B 2 0.350776 0.189853 0.197320 11.00000 -1.50000 H40C 2 0.370876 0.086898 0.249521 11.00000 -1.50000 AFIX 0 C44 1 0.217122 0.261720 0.655549 11.00000 0.09380 0.10388 = 0.06599 -0.02934 0.02561 -0.01602 O2 3 0.253539 0.233037 0.616499 11.00000 0.19200 0.12389 = 0.13365 -0.02534 0.10817 0.00110 C9 1 0.115813 0.637727 0.452858 11.00000 0.10076 0.07741 = 0.05534 -0.03084 -0.00186 0.02533 AFIX 137 H9A 2 0.160647 0.653108 0.459388 11.00000 -1.50000 H9B 2 0.108092 0.575118 0.483660 11.00000 -1.50000 H9C 2 0.093589 0.701782 0.467692 11.00000 -1.50000 AFIX 0 C43 1 0.183230 0.374547 0.645333 11.00000 0.07172 0.14599 = 0.04774 -0.01430 0.00995 -0.00043 AFIX 13 H43 2 0.192569 0.412783 0.694187 11.00000 -1.20000 AFIX 0 C45 1 0.228623 0.091785 0.727395 11.00000 0.09758 0.08078 = 0.14154 -0.03114 0.04017 -0.00520 AFIX 23 H45A 2 0.221794 0.046371 0.682004 11.00000 -1.20000 H45B 2 0.274123 0.099601 0.743265 11.00000 -1.20000 AFIX 0 C46 1 0.200241 0.040014 0.785722 11.00000 0.12619 0.10842 = 0.13721 0.00468 0.05654 0.01654 AFIX 137 H46A 2 0.156655 0.022282 0.766921 11.00000 -1.50000 H46B 2 0.201963 0.090011 0.827905 11.00000 -1.50000 H46C 2 0.222971 -0.027148 0.801658 11.00000 -1.50000 AFIX 0 C42 1 0.111213 0.370450 0.625977 11.00000 0.08716 0.34235 = 0.09383 0.01570 -0.00050 -0.04132 AFIX 137 H42A 2 0.094987 0.444592 0.616262 11.00000 -1.50000 H42B 2 0.093634 0.338975 0.667639 11.00000 -1.50000 H42C 2 0.099465 0.325193 0.581788 11.00000 -1.50000 AFIX 0 HKLF 4 REM dijydroxy_p5_a.res in C2 REM wR2 = 0.1146, GooF = S = 1.031, Restrained GooF = 1.031 for all data REM R1 = 0.0401 for 8567 Fo > 4sig(Fo) and 0.0416 for all 8931 data REM 563 parameters refined using 1 restraints END WGHT 0.0755 1.2012 REM Highest difference peak 0.332, deepest hole -0.247, 1-sigma level 0.038 Q1 1 0.1541 0.2392 0.6919 11.00000 0.05 0.33 Q2 1 0.1967 0.2501 0.5918 11.00000 0.05 0.27 Q3 1 0.1704 0.2809 0.6429 11.00000 0.05 0.27 Q4 1 0.1739 0.1166 0.7034 11.00000 0.05 0.26 Q5 1 0.0832 0.4325 0.6250 11.00000 0.05 0.22 Q6 1 0.1243 0.1947 0.6286 11.00000 0.05 0.20 Q7 1 0.4198 0.8827 0.1902 11.00000 0.05 0.20 Q8 1 0.2629 0.6714 -0.0177 11.00000 0.05 0.19 Q9 1 0.0258 0.4998 0.5190 11.00000 0.05 0.18 Q10 1 0.0614 0.5169 0.6031 11.00000 0.05 0.18 Q11 1 0.1682 0.4878 0.5929 11.00000 0.05 0.17 Q12 1 0.2182 -0.0376 0.8626 11.00000 0.05 0.16 Q13 1 0.1320 0.3796 0.6309 11.00000 0.05 0.15 Q14 1 0.1142 0.3153 0.5827 11.00000 0.05 0.15 Q15 1 0.4608 0.4776 0.1903 11.00000 0.05 0.14 Q16 1 0.1683 0.0598 0.6085 11.00000 0.05 0.14 Q17 1 0.4197 0.0797 0.3109 11.00000 0.05 0.13 Q18 1 0.2765 0.7442 0.0656 11.00000 0.05 0.12 Q19 1 0.2092 -0.1337 0.8479 11.00000 0.05 0.12 Q20 1 0.1616 0.1875 0.6478 11.00000 0.05 0.12 ; _shelx_res_checksum 97426 _shelx_hkl_file ; 0 0 -1 7.65 0.31 0 0 1 8.17 0.33 0 0 2 1560.77 35.67 0 0 -2 1511.07 35.49 0 0 -2 1487.79 35.65 0 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11.62 0 4 -4 470.04 12.11 0 4 5 623.86 15.73 0 -4 5 632.08 15.83 0 4 -5 652.24 16.32 0 4 -5 638.31 15.46 0 4 5 636.24 15.79 0 4 -5 663.44 15.64 0 4 5 654.27 16.43 0 -4 -5 669.79 15.65 0 4 -5 656.68 15.85 0 -4 5 637.66 15.75 0 -4 -5 639.87 15.82 0 -4 -5 648.34 15.66 0 -4 6 78.46 2.56 0 -4 -6 77.38 2.62 0 4 6 71.67 2.42 0 4 -6 78.59 2.43 0 4 -6 78.56 2.96 0 4 6 71.45 2.51 0 4 6 76.03 3.06 0 -4 6 74.68 3.10 0 -4 -6 80.13 2.46 0 4 -6 78.59 2.66 0 -4 7 141.54 4.13 0 4 -7 132.95 4.20 0 4 -7 135.12 4.43 0 4 7 131.72 4.07 0 -4 -7 137.06 3.98 0 4 -7 139.39 3.95 0 -4 -7 132.78 4.17 0 4 7 130.01 4.63 0 -4 7 133.36 4.67 0 4 7 127.14 3.81 0 4 8 39.16 1.84 0 -4 8 37.88 2.23 0 4 -8 37.21 1.67 0 -4 -8 39.21 1.71 0 4 8 37.84 1.49 0 4 -8 36.02 1.97 0 -4 8 40.04 1.87 0 -4 -8 40.70 1.95 0 4 8 38.83 2.28 0 4 -8 36.63 1.88 0 4 -9 42.87 2.13 0 4 -9 39.22 1.37 0 -4 -9 41.76 1.87 0 4 -9 40.27 1.33 0 -4 -9 40.65 1.39 0 4 -9 43.68 1.89 0 4 -9 44.37 2.20 0 -4 -9 41.94 2.11 0 4 -9 38.25 1.38 0 -4 9 43.72 2.44 0 4 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0 4 -18 1.93 0.44 0 4 18 2.09 0.50 0 -4 18 2.03 0.55 0 -4 -18 2.43 0.54 0 4 -18 2.07 0.68 0 -4 -18 2.29 0.72 0 4 18 2.68 0.57 0 4 -18 2.16 0.42 0 -4 -18 1.60 0.49 0 4 -18 2.58 0.98 0 -4 -19 1.90 0.37 0 4 -19 1.65 0.38 0 -4 -19 1.67 0.46 0 4 19 1.80 0.38 0 4 -19 -0.15 0.21 0 4 -19 2.62 0.55 0 -4 -19 1.94 0.41 0 4 -19 2.65 0.85 0 4 19 1.48 0.44 0 -4 19 1.89 0.47 0 -4 -19 2.06 0.67 0 4 -20 4.52 0.49 0 -4 -20 5.03 0.38 0 4 20 4.62 0.45 0 -4 -20 6.45 0.68 0 4 -20 4.83 0.38 0 -4 -20 4.66 0.37 0 -4 -20 5.88 0.48 0 -4 20 5.11 0.44 0 -4 -21 2.32 0.41 0 -4 -21 2.09 0.27 0 6 0 154.00 4.76 0 -6 0 155.28 4.34 0 6 0 155.18 4.90 0 -6 0 161.41 4.92 0 6 1 508.04 13.35 0 6 -1 515.79 13.54 0 -6 1 512.23 12.80 0 -6 -1 517.68 12.86 0 6 1 513.37 13.37 0 6 -1 520.08 13.17 0 6 1 504.98 13.39 0 -6 1 537.95 13.58 0 -6 -1 539.42 13.36 0 6 2 100.03 3.51 0 -6 -2 96.66 3.06 0 6 2 98.13 3.42 0 6 2 98.70 3.37 0 6 -2 102.92 3.68 0 -6 -2 103.89 3.37 0 -6 2 95.55 2.97 0 -6 2 101.03 3.69 0 6 -2 98.14 3.19 0 -6 -3 50.37 1.93 0 6 3 48.08 2.05 0 6 3 50.11 2.34 0 -6 3 49.97 1.83 0 -6 -3 53.96 2.10 0 6 -3 48.95 1.91 0 6 3 51.09 2.16 0 -6 3 48.44 2.45 0 6 -4 37.31 2.14 0 6 4 36.40 1.78 0 6 4 36.12 2.01 0 -6 -4 36.97 1.65 0 -6 4 32.99 1.48 0 -6 4 39.99 2.25 0 6 -4 36.87 1.50 0 6 5 326.31 9.17 0 6 -5 335.49 9.26 0 -6 -5 323.38 8.33 0 6 5 303.08 8.50 0 6 -5 313.17 8.06 0 -6 5 331.32 9.35 0 -6 5 306.07 8.25 0 6 6 9.81 0.89 0 6 6 11.29 0.69 0 -6 -6 10.49 0.63 0 6 -6 10.47 0.62 0 6 6 12.35 1.37 0 6 -6 10.38 0.63 0 6 -6 11.20 0.64 0 6 -6 10.61 1.31 0 6 -7 46.55 2.54 0 -6 -7 44.82 1.51 0 -6 7 46.41 1.50 0 6 -7 44.25 1.48 0 6 7 50.78 2.67 0 6 -7 45.89 1.49 0 6 -7 45.61 1.51 0 -6 -7 44.81 1.44 0 6 7 39.06 1.80 0 6 7 42.67 1.54 0 6 -8 85.04 2.47 0 6 8 82.98 3.83 0 -6 8 83.59 2.45 0 -6 -8 84.05 2.50 0 -6 8 84.22 3.88 0 6 -8 85.12 2.53 0 6 -8 86.43 2.47 0 -6 -8 82.54 2.43 0 6 -8 89.39 3.77 0 6 -8 87.36 2.50 0 6 -9 126.65 3.44 0 -6 -9 116.09 3.32 0 6 -9 122.11 3.35 0 6 -9 126.70 4.82 0 6 -9 122.65 3.63 0 -6 -9 118.19 3.40 0 -6 9 125.54 4.95 0 -6 9 116.81 3.30 0 6 -9 125.19 3.37 0 6 9 122.22 4.99 0 -6 10 323.35 8.28 0 6 -10 326.53 10.00 0 6 -10 338.08 8.67 0 -6 10 330.29 10.26 0 6 -10 345.93 8.45 0 6 -10 339.40 8.36 0 -6 -10 327.46 8.35 0 -6 -10 332.73 8.42 0 6 10 329.44 10.41 0 6 10 322.28 8.44 0 6 -10 342.07 8.34 0 -6 -11 151.42 4.15 0 -6 -11 150.84 4.38 0 -6 11 144.03 4.03 0 6 -11 155.71 4.19 0 6 11 154.42 6.11 0 6 11 151.47 4.26 0 6 -11 156.22 4.23 0 6 -11 154.59 4.46 0 -6 11 142.30 5.74 0 -6 -11 153.22 4.22 0 6 12 29.71 2.49 0 -6 12 28.87 2.32 0 -6 -12 30.75 1.53 0 -6 -12 29.69 1.34 0 6 -12 31.93 1.61 0 6 12 32.68 1.43 0 6 -12 31.73 1.38 0 -6 -12 29.88 1.29 0 6 -12 29.00 1.30 0 6 12 28.89 2.18 0 -6 -13 104.57 3.08 0 6 13 102.65 3.17 0 6 13 88.98 4.16 0 -6 -13 105.16 3.16 0 6 -13 104.67 3.07 0 6 -13 101.12 3.14 0 6 13 105.21 4.96 0 -6 -13 108.03 3.35 0 6 -13 106.31 3.38 0 -6 13 97.66 4.46 0 6 -14 123.02 3.63 0 6 -14 117.12 4.15 0 6 -14 135.19 3.92 0 6 -14 129.19 3.57 0 6 14 127.75 3.68 0 -6 -14 130.98 3.86 0 -6 -14 128.65 3.59 0 -6 14 112.99 4.87 0 6 -14 115.57 3.33 0 6 14 123.01 5.51 0 6 15 5.03 0.67 0 6 -15 5.91 0.68 0 6 -15 5.76 0.70 0 6 -15 5.17 0.45 0 -6 -15 5.46 0.65 0 6 -15 5.19 1.21 0 6 -15 4.98 0.88 0 -6 -15 6.88 0.93 0 -6 -16 1.40 0.73 0 6 16 1.16 0.55 0 -6 -16 0.52 0.49 0 6 -16 1.21 0.53 0 6 -16 0.69 0.49 0 6 -16 0.65 0.70 0 -6 -17 13.46 1.01 0 6 -17 13.36 0.78 0 -6 -17 15.57 0.89 0 6 17 13.54 0.85 0 -6 -17 13.89 0.82 0 6 -17 15.43 1.04 0 6 -18 15.81 0.97 0 -6 -18 17.68 1.02 0 6 18 16.86 0.82 0 -6 -18 16.54 0.82 0 -6 -18 15.74 0.79 0 6 -19 1.04 0.47 0 -6 -19 0.94 0.35 0 -6 -19 0.85 0.31 0 -6 -19 0.66 0.50 0 6 19 0.93 0.32 0 6 -19 1.27 0.33 0 -6 -20 8.42 0.55 0 8 0 290.28 7.36 0 8 0 307.55 8.60 0 -8 0 315.60 8.83 0 8 0 322.28 9.00 0 8 0 274.96 7.66 0 -8 0 299.82 7.41 0 8 0 306.24 7.43 0 8 -1 20.04 0.88 0 -8 -1 20.07 0.90 0 -8 -1 20.60 1.55 0 8 1 20.91 0.90 0 8 1 19.50 0.85 0 8 -1 20.56 0.91 0 8 -1 20.51 1.48 0 8 -1 20.91 1.74 0 8 1 23.99 1.71 0 8 -1 19.84 1.13 0 8 1 25.18 1.71 0 -8 1 20.81 1.68 0 8 -2 11.15 0.69 0 8 -2 10.01 1.38 0 8 2 9.49 1.24 0 8 -2 10.73 0.60 0 -8 -2 11.40 0.69 0 8 2 10.90 0.65 0 -8 -2 12.97 1.21 0 -8 -2 11.03 0.68 0 8 2 10.79 0.65 0 8 -2 9.48 0.87 0 -8 2 11.81 1.41 0 8 -2 11.63 1.08 0 8 -2 10.49 0.68 0 8 2 10.37 0.60 0 8 -2 11.35 0.60 0 -8 -3 224.74 6.56 0 8 -3 207.22 5.52 0 8 3 223.01 6.97 0 8 3 225.16 5.56 0 8 -3 223.97 5.57 0 8 -3 212.29 5.85 0 8 -3 215.26 6.24 0 8 -3 213.27 5.47 0 8 3 213.52 5.47 0 -8 -3 204.08 6.11 0 8 -3 220.36 7.23 0 8 -3 214.63 5.46 0 -8 3 230.92 7.23 0 -8 -3 217.94 5.58 0 8 4 70.86 3.33 0 8 4 67.38 2.03 0 8 -4 68.28 2.05 0 -8 4 72.97 3.48 0 8 -4 66.76 2.11 0 8 -4 68.31 2.07 0 -8 -4 71.21 2.80 0 8 4 71.90 2.15 0 8 -4 69.25 2.41 0 -8 -4 71.64 2.17 0 8 -4 68.86 2.12 0 -8 -4 72.15 2.72 0 8 -4 68.61 2.54 0 -8 -5 18.98 1.33 0 8 -5 19.41 0.96 0 -8 5 18.67 0.93 0 8 -5 19.96 1.20 0 8 5 22.38 1.00 0 8 5 17.69 1.73 0 8 -5 20.55 0.96 0 -8 -5 19.18 0.89 0 8 5 20.91 1.74 0 8 -5 19.57 0.91 0 8 -5 20.01 0.90 0 -8 5 17.63 1.80 0 8 5 18.66 0.83 0 8 -6 1.71 0.75 0 -8 6 1.26 1.01 0 8 6 2.53 0.53 0 -8 -6 1.66 0.45 0 8 -6 1.78 0.54 0 8 -6 2.02 1.03 0 8 -6 2.99 0.49 0 -8 -6 1.04 0.58 0 8 -6 1.87 0.43 0 8 6 3.34 1.02 0 -8 6 2.06 0.49 0 8 7 114.15 3.22 0 8 7 105.51 4.61 0 -8 7 111.23 4.82 0 8 -7 108.53 3.13 0 8 -7 114.17 3.25 0 8 -7 110.57 3.11 0 8 -7 108.38 4.76 0 8 7 108.18 4.60 0 -8 -7 109.91 3.96 0 -8 7 108.72 3.13 0 -8 -7 106.45 3.12 0 8 -7 110.62 3.46 0 8 -8 141.58 3.92 0 8 -8 138.34 3.83 0 -8 -8 137.73 3.71 0 8 -8 138.70 3.82 0 -8 -8 136.02 4.74 0 -8 8 132.76 3.77 0 8 -8 140.24 4.17 0 8 8 137.58 3.89 0 8 -8 136.78 3.79 0 8 8 138.70 5.54 0 8 -8 141.99 5.63 0 8 8 132.94 5.33 0 -8 -8 139.06 3.85 0 -8 -9 176.53 4.60 0 8 9 179.33 4.80 0 8 -9 168.03 4.69 0 -8 -9 163.40 5.66 0 8 9 168.14 6.37 0 8 -9 174.80 4.69 0 8 -9 179.53 4.81 0 8 -9 177.73 4.68 0 8 9 181.98 6.68 0 -8 9 170.85 4.62 0 -8 9 163.26 6.50 0 -8 -9 174.81 4.74 0 8 10 16.30 1.91 0 -8 -10 12.33 1.31 0 8 10 14.09 0.96 0 8 -10 13.12 0.85 0 8 -10 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2 -6 -6 105.92 3.46 2 6 -6 102.42 2.81 2 -6 -6 100.62 2.85 -2 -6 6 107.99 4.33 2 6 -6 102.44 2.82 -2 6 5 9.59 0.77 2 -6 -5 9.08 0.89 -2 6 5 9.27 0.62 2 6 -5 10.12 0.83 -2 6 5 9.89 1.04 -2 -6 5 10.06 1.35 2 6 -5 9.02 0.57 2 -6 -5 7.72 0.86 -2 6 5 9.48 1.11 2 6 -5 9.26 1.23 -2 6 4 328.24 9.19 -2 6 4 321.61 9.09 -2 -6 4 336.12 9.60 2 -6 -4 339.26 8.87 2 6 -4 333.73 8.71 2 6 -4 326.06 9.43 -2 6 4 334.61 8.79 2 -6 -4 336.22 8.96 -2 -6 3 151.24 4.96 2 -6 -3 145.76 4.47 2 6 -3 136.27 4.26 2 -6 -3 144.41 4.30 -2 6 3 137.70 4.36 -2 6 3 141.46 4.60 -2 6 3 142.02 4.52 -2 6 2 234.21 6.67 2 -6 -2 226.45 6.41 -2 6 2 223.64 6.79 2 6 -2 247.59 7.03 2 -6 -2 237.47 6.73 -2 -6 2 241.82 7.05 -2 6 2 236.03 6.60 2 6 -2 235.29 6.55 -2 6 1 100.86 3.60 -2 -6 1 107.54 3.77 -2 6 1 102.53 3.73 2 -6 -1 108.34 3.70 2 6 -1 108.32 3.80 2 -6 -1 106.10 3.34 2 6 -1 108.03 3.58 -2 -6 0 156.36 4.79 -2 -6 0 148.93 4.03 -2 6 0 148.88 4.88 2 6 0 150.65 4.82 2 -6 0 155.07 4.86 2 6 0 151.66 4.74 -2 6 0 150.91 4.82 2 -6 0 153.18 4.42 -2 6 -1 36.53 1.69 2 -6 1 34.56 1.92 -2 -6 -1 38.15 1.76 2 6 1 33.28 1.83 -2 -6 -1 36.84 1.36 2 -6 1 35.45 1.60 -2 6 -1 38.56 2.01 2 -6 2 99.20 3.68 -2 -6 -2 97.42 2.93 2 6 2 102.29 3.59 -2 6 -2 96.18 3.65 -2 6 -2 95.26 3.12 2 -6 2 92.95 3.14 -2 -6 -2 107.11 3.29 2 6 3 176.01 5.57 2 -6 3 169.55 5.55 -2 -6 -3 177.41 4.93 2 -6 3 169.99 5.00 -2 6 -3 168.59 4.75 2 -6 4 145.15 4.45 2 6 4 149.95 5.06 2 6 4 141.71 4.85 2 -6 4 152.98 5.08 -2 6 -4 146.21 5.01 -2 6 -4 145.45 3.99 -2 -6 -4 144.14 4.16 2 6 5 12.93 1.34 2 -6 5 11.59 0.99 2 6 5 11.58 1.31 -2 6 -5 11.21 0.65 -2 6 -5 11.10 0.65 -2 6 -5 11.06 1.27 -2 6 -5 11.58 0.65 2 6 5 11.16 0.67 -2 6 -6 241.59 7.28 2 6 6 226.55 5.84 -2 6 -6 229.07 5.81 2 -6 6 234.60 7.32 2 6 6 217.49 7.02 2 -6 6 221.60 6.56 -2 6 -6 230.52 5.80 -2 6 -6 227.31 5.79 2 -6 6 226.44 5.83 -2 6 -6 232.25 6.04 2 6 6 240.55 7.39 2 -6 7 157.76 4.10 -2 6 -7 155.52 4.42 -2 6 -7 161.10 4.21 2 6 7 163.03 5.81 -2 -6 -7 154.99 4.09 -2 6 -7 162.13 5.60 -2 6 -7 158.47 4.69 2 6 7 146.28 5.35 2 -6 7 168.20 5.69 2 -6 7 155.05 4.21 -2 6 -7 157.63 4.18 -2 6 -7 162.41 4.17 2 6 7 157.28 4.24 -2 6 -8 46.90 1.50 2 -6 8 48.51 2.69 2 6 8 48.01 1.62 2 -6 8 47.43 1.56 -2 6 -8 39.99 1.93 -2 6 -8 48.44 2.66 -2 6 -8 44.21 1.99 -2 6 -8 46.33 1.77 2 6 8 48.01 2.59 2 6 8 52.02 2.89 -2 6 -8 46.75 1.53 -2 6 -8 49.41 1.57 2 -6 8 46.52 1.44 -2 -6 -8 45.37 1.45 2 -6 9 37.61 1.29 -2 6 -9 36.75 1.35 2 -6 9 41.98 2.57 -2 6 -9 34.98 1.88 2 6 9 38.09 2.63 2 6 9 35.63 2.30 -2 6 -9 38.46 1.64 2 6 9 37.00 1.47 -2 6 -9 36.66 1.41 -2 6 -9 31.38 1.79 -2 6 -9 34.40 2.32 2 -6 9 36.37 1.40 -2 6 -9 36.69 1.31 -2 -6 -9 37.51 1.34 -2 6 -9 38.02 1.40 -2 6 -10 14.01 0.86 -2 6 -10 14.92 1.11 2 -6 10 14.32 0.73 -2 -6 -10 13.24 1.00 -2 6 -10 15.34 0.83 2 6 10 15.99 1.64 2 -6 10 13.47 1.55 2 6 10 14.94 1.82 -2 6 -10 11.19 1.27 -2 -6 -10 14.62 0.80 2 -6 10 14.19 0.85 -2 6 -10 13.49 0.75 -2 -6 -10 14.31 0.89 -2 6 -10 11.09 1.42 -2 6 -10 15.04 0.88 -2 -6 -11 281.86 7.36 -2 6 -11 281.04 7.16 -2 6 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1.53 2 -8 -4 97.34 3.65 -2 -8 4 102.52 4.21 -2 8 4 89.51 2.64 2 8 -4 93.70 2.92 2 -8 -4 90.77 2.62 2 -8 -4 95.19 2.76 -2 8 4 98.01 3.49 2 8 -4 96.53 2.67 -2 8 4 100.15 2.74 2 8 -4 92.87 3.33 -2 8 4 88.97 3.70 2 -8 -4 96.14 3.46 2 8 -4 89.36 2.54 2 8 -4 92.53 2.69 2 8 -4 90.22 2.58 -2 8 3 27.58 1.98 -2 -8 3 32.31 2.20 2 8 -3 30.62 1.15 2 -8 -3 32.93 1.23 -2 8 3 31.66 2.03 2 -8 -3 29.59 1.23 -2 8 3 33.01 1.90 2 -8 -3 30.16 1.88 2 8 -3 29.78 1.72 2 -8 -3 28.21 1.63 2 8 -3 29.02 1.06 2 8 -3 30.73 1.20 2 8 -3 30.13 1.38 -2 8 3 30.96 1.18 2 -8 -2 69.64 2.76 -2 -8 2 73.43 3.32 -2 8 2 73.48 3.29 -2 8 2 73.89 3.20 -2 8 2 70.19 2.15 2 8 -2 72.99 2.96 -2 8 2 74.15 3.16 2 -8 -2 74.15 2.22 2 -8 -2 79.98 3.22 2 8 -2 69.16 2.14 2 -8 -2 73.36 2.22 2 8 -2 67.32 2.34 2 8 -2 72.61 2.13 2 -8 -1 109.66 4.03 -2 8 1 98.30 2.74 2 8 -1 97.32 2.81 -2 8 1 108.26 3.94 2 -8 -1 100.79 2.88 -2 8 1 110.23 4.09 2 8 -1 99.46 2.78 -2 -8 1 105.14 4.00 2 8 -1 97.46 3.02 -2 8 1 103.82 2.86 2 8 -1 103.85 3.78 2 -8 -1 100.12 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1 2165.57 51.61 -4 2 -1 2288.49 51.72 -4 -2 -1 2270.90 51.71 4 2 1 2229.00 51.85 4 -2 2 2492.74 57.28 4 -2 2 2450.14 57.37 4 2 2 2348.58 57.31 4 -2 2 2392.92 56.82 -4 2 -2 2460.01 57.11 -4 -2 -2 2452.94 57.11 4 2 2 2436.57 57.21 4 -2 2 2408.06 57.24 -4 2 -2 2419.13 57.23 4 -2 3 181.61 4.96 4 -2 3 180.61 4.83 -4 2 -3 186.64 4.84 4 2 3 172.16 5.08 4 2 3 178.57 4.82 -4 2 -3 179.37 4.87 4 -2 3 175.64 4.37 4 2 3 176.80 5.08 4 -2 3 173.08 5.10 4 2 3 178.20 4.85 4 -2 3 183.09 4.90 -4 -2 -3 184.78 4.83 -4 -2 -4 273.89 7.00 -4 2 -4 266.03 6.97 4 -2 4 265.75 6.55 4 -2 4 260.80 6.94 -4 2 -4 276.01 6.93 4 2 4 265.50 7.23 4 2 4 244.76 7.23 4 2 4 259.12 6.89 4 -2 4 263.42 7.08 4 2 4 265.39 6.95 4 -2 4 249.00 7.28 4 -2 4 269.58 6.95 4 -2 5 223.92 6.00 4 2 5 223.02 6.00 4 -2 5 221.88 5.96 4 2 5 220.40 6.23 4 -2 5 213.86 6.15 -4 -2 -5 226.93 6.06 -4 2 -5 220.23 6.03 4 2 5 210.50 5.88 4 2 5 201.09 6.36 4 2 6 866.89 21.18 4 2 6 889.91 21.49 4 -2 6 849.80 21.35 4 2 6 822.38 20.98 4 -2 6 837.20 21.05 -4 2 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310.08 7.86 -4 4 5 303.02 7.75 -4 4 5 301.25 8.20 4 -4 -5 302.79 8.13 -4 -4 5 315.05 8.05 -4 -4 4 41.58 1.65 -4 4 4 42.30 1.89 4 -4 -4 45.06 1.58 4 4 -4 40.56 1.67 4 -4 -4 41.86 1.77 4 -4 -4 43.95 1.87 -4 4 4 42.98 1.67 4 4 -4 43.53 1.55 4 -4 -3 97.79 3.15 -4 4 3 94.59 3.19 4 4 -3 96.92 2.76 -4 4 3 91.03 2.84 4 4 -3 97.12 3.01 4 -4 -3 99.64 2.79 -4 -4 3 87.02 2.82 -4 4 3 93.73 3.00 4 -4 -3 101.64 3.06 4 4 -2 118.20 3.32 -4 4 2 113.21 3.77 4 -4 -2 120.83 3.33 4 4 -2 126.80 3.68 4 -4 -2 124.83 3.63 4 -4 -2 121.63 3.77 -4 4 2 127.29 3.51 4 -4 -1 109.91 2.94 4 -4 -1 102.12 2.97 4 -4 -1 110.45 3.47 4 4 -1 109.15 2.99 -4 4 1 106.05 2.99 4 -4 -1 110.23 3.30 4 4 -1 110.31 3.35 4 4 -1 108.58 2.92 4 -4 0 77.25 2.54 -4 4 0 77.25 2.16 -4 -4 0 74.66 1.95 4 4 0 77.79 2.19 4 -4 0 78.01 2.20 -4 4 0 77.28 2.76 -4 -4 0 76.30 2.15 4 -4 0 77.15 2.72 -4 -4 0 71.50 2.56 -4 4 -1 44.70 1.45 4 -4 1 45.55 1.51 4 -4 1 47.62 1.98 -4 -4 -1 43.06 1.42 -4 4 -1 47.96 2.01 -4 -4 -1 41.65 1.63 4 4 1 42.16 1.84 4 -4 1 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1.38 5 -7 -5 19.52 0.95 -5 -7 5 23.04 1.95 5 7 -5 20.86 0.88 5 -7 -5 20.40 1.01 5 7 -5 22.00 1.44 -5 7 5 20.60 1.31 5 -7 -5 18.57 1.46 5 7 -5 19.90 1.01 5 7 -5 19.14 0.81 5 7 -5 20.39 0.94 -5 7 5 19.77 0.93 5 7 -4 144.50 3.68 -5 7 4 144.55 3.78 5 7 -4 150.01 4.65 5 7 -4 149.63 3.78 -5 7 4 152.23 5.13 -5 7 4 145.55 4.62 5 -7 -4 151.97 3.84 5 -7 -4 154.20 4.79 5 7 -4 141.99 3.75 5 -7 -4 141.60 3.84 -5 -7 4 159.92 5.48 -5 7 4 138.45 3.65 5 -7 -4 158.09 4.98 -5 7 4 140.73 3.72 5 -7 -4 145.98 3.75 5 -7 -3 77.50 2.31 -5 7 3 76.39 2.15 5 7 -3 77.52 2.13 -5 7 3 76.64 2.24 5 7 -3 76.77 2.22 5 -7 -3 76.83 2.19 -5 -7 3 83.94 3.50 -5 7 3 82.31 3.42 5 -7 -3 78.83 3.25 5 -7 -3 81.33 2.32 5 -7 -3 83.90 3.11 5 7 -3 77.85 3.01 -5 7 3 79.48 3.12 -5 7 3 75.89 2.20 -5 7 2 5.42 0.55 5 7 -2 5.85 0.45 -5 7 2 6.36 1.11 5 -7 -2 5.70 0.58 -5 -7 2 4.81 0.99 -5 7 2 5.36 0.48 -5 7 2 6.53 0.53 5 -7 -2 5.65 0.48 5 -7 -2 5.75 0.87 5 -7 -2 4.97 1.00 5 -7 -2 5.49 0.60 5 7 -2 6.48 0.97 5 7 -2 5.56 0.54 -5 7 2 5.92 0.96 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8 -7 1.46 0.82 8 -8 7 1.86 0.58 8 8 7 1.53 0.50 8 8 7 1.13 0.93 -8 -8 -7 1.43 0.57 -8 8 -7 1.46 1.06 8 -8 7 1.26 0.93 8 -8 7 1.75 0.64 8 -8 7 1.42 0.66 -8 8 -7 1.79 0.51 -8 -8 -7 1.41 0.44 -8 8 -8 152.00 4.06 -8 8 -8 150.44 4.18 -8 8 -8 151.50 4.08 8 8 8 148.03 4.11 -8 -8 -8 148.09 4.14 -8 8 -8 147.25 5.93 8 -8 8 137.60 5.52 -8 -8 -8 146.46 4.05 8 -8 8 147.36 4.21 -8 8 -8 150.92 4.16 8 8 8 140.81 5.36 8 -8 8 148.83 4.23 8 -8 8 151.50 4.10 -8 8 -8 135.14 4.45 -8 8 -9 41.14 1.45 -8 -8 -9 39.94 1.50 -8 8 -9 38.46 1.46 8 8 9 38.26 1.53 -8 -8 -9 34.68 1.50 -8 8 -9 42.09 1.58 -8 8 -9 40.19 1.59 8 -8 9 40.41 1.62 8 -8 9 42.50 1.65 8 -8 9 40.92 1.51 -8 8 -9 34.98 1.80 -8 8 -10 112.02 3.10 -8 8 -10 109.69 3.11 8 8 10 111.04 3.25 -8 -8 -10 104.29 3.20 -8 8 -10 111.00 3.19 -8 -8 -10 113.88 3.21 -8 8 -10 113.30 3.27 8 -8 10 109.40 3.24 -8 8 -10 113.81 3.25 8 -8 10 107.14 3.27 8 -8 10 115.45 3.17 -8 8 -10 107.31 3.54 8 -8 11 4.85 0.63 -8 8 -11 5.11 0.89 -8 8 -11 5.72 0.60 8 8 11 5.48 0.69 -8 -8 -11 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30.71 1.63 -10 -2 9 41.54 2.54 -10 2 9 38.22 2.47 10 2 -9 36.85 1.45 10 -2 -9 37.51 1.47 10 2 -9 40.24 1.44 10 -2 -9 40.42 1.53 10 -2 -9 42.39 2.27 -10 2 9 37.99 2.21 10 2 -9 39.21 1.42 10 2 -9 38.45 1.43 10 -2 -9 38.84 1.42 10 2 -9 40.67 2.24 10 -2 -9 38.71 1.33 10 -2 -9 38.87 1.99 10 -2 -9 38.58 1.57 10 -2 -8 63.49 1.90 10 -2 -8 61.53 2.10 -10 -2 8 56.84 3.04 -10 2 8 64.53 3.17 10 2 -8 64.30 1.90 10 2 -8 60.58 1.98 10 -2 -8 61.46 2.02 10 -2 -8 67.01 2.08 -10 2 8 60.78 2.87 10 2 -8 64.22 1.98 10 -2 -8 66.89 2.88 10 2 -8 62.81 2.83 10 2 -8 63.70 1.96 10 -2 -8 63.80 1.96 10 -2 -8 57.38 1.87 10 -2 -8 63.75 1.88 10 -2 -8 64.24 2.62 10 2 -7 147.71 3.89 10 -2 -7 154.70 3.96 10 2 -7 162.39 3.98 -10 2 7 133.78 5.18 -10 -2 7 139.81 5.23 10 2 -7 139.65 3.95 10 -2 -7 147.48 4.00 10 2 -7 154.64 5.00 10 -2 -7 151.70 3.90 10 -2 -7 152.30 5.27 10 -2 -7 141.73 3.89 10 -2 -7 149.65 3.88 10 -2 -7 153.83 5.01 10 -2 -7 157.92 4.75 -10 2 6 41.08 2.16 10 -2 -6 41.33 2.30 10 -2 -6 43.69 1.97 10 -2 -6 44.36 2.17 10 2 -6 41.89 2.15 10 2 -6 41.30 1.44 10 -2 -5 10.32 1.14 10 2 -5 9.53 1.10 10 2 -5 8.96 0.57 10 2 -5 8.98 1.08 10 -2 -5 9.48 1.08 -10 2 5 11.36 1.21 10 -2 -5 8.96 1.13 10 -2 -5 11.29 1.01 10 2 -4 69.61 2.16 10 -2 -4 77.62 2.93 10 -2 -4 77.23 2.97 10 2 -4 73.69 2.92 -10 2 4 74.58 2.94 10 -2 -4 69.62 2.99 10 2 -4 75.57 2.85 10 -2 -4 74.43 2.71 10 2 -4 74.49 2.88 10 2 -3 48.68 2.21 10 -2 -3 51.39 2.26 10 2 -3 48.36 1.61 -10 2 3 50.58 2.26 10 -2 -3 46.97 2.24 10 2 -3 45.88 2.21 10 -2 -3 46.25 2.23 10 2 -3 50.33 2.18 10 -2 -3 46.71 2.07 10 2 -2 226.38 6.45 10 -2 -2 218.93 6.41 10 2 -2 215.09 5.71 -10 -2 2 219.03 6.11 -10 2 2 227.05 6.42 10 -2 -2 213.64 6.40 10 -2 -2 230.77 6.48 10 -2 -2 215.46 6.44 10 2 -2 219.97 6.49 10 2 -2 222.75 6.31 10 -2 -2 220.83 6.27 10 -2 -1 366.57 9.85 10 -2 -1 363.20 10.06 10 2 -1 369.96 10.08 10 2 -1 371.56 10.00 10 -2 -1 388.83 10.06 10 2 -1 364.00 9.35 -10 -2 1 373.82 9.56 -10 2 1 369.33 9.90 10 -2 -1 374.16 9.90 10 -2 -1 373.38 9.94 10 2 -1 376.43 9.83 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1.08 10 -4 -17 31.13 1.07 10 4 -16 10.42 0.97 10 4 -16 10.68 0.72 10 -4 -16 10.22 0.72 10 -4 -16 11.70 0.81 10 4 -16 10.11 0.76 10 -4 -16 8.88 0.98 10 4 -16 10.48 0.97 10 -4 -16 11.39 0.78 10 -4 -16 10.49 0.86 10 -4 -16 10.17 0.91 10 -4 -16 9.31 0.67 10 -4 -16 10.91 0.74 10 4 -15 10.03 1.00 10 4 -15 11.29 0.77 10 -4 -15 10.94 0.77 10 -4 -15 11.12 0.83 10 -4 -15 11.45 1.09 10 -4 -15 9.89 0.85 10 4 -15 8.94 0.94 10 4 -15 10.57 0.68 10 -4 -15 10.33 0.79 10 -4 -15 10.55 0.74 10 -4 -15 12.39 0.84 10 4 -15 12.13 0.82 10 -4 -14 30.46 1.30 10 4 -14 31.87 1.55 10 4 -14 31.22 1.26 10 -4 -14 34.30 1.35 10 4 -14 32.40 1.31 10 4 -14 26.38 1.44 -10 -4 14 31.29 2.28 -10 4 14 29.59 2.24 10 -4 -14 26.63 1.44 10 -4 -14 29.01 1.55 10 -4 -14 30.78 1.26 10 -4 -14 31.19 1.38 -10 -4 14 30.30 2.24 -10 4 14 21.40 1.91 10 4 -14 30.23 1.20 10 4 -14 26.51 1.31 10 -4 -14 26.80 1.34 10 -4 -14 30.16 2.40 10 -4 -14 28.72 2.16 10 4 -14 27.37 2.12 10 -4 -14 32.00 1.32 10 -4 -14 32.86 2.18 10 -4 -14 29.21 1.24 10 4 -13 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5.21 10 4 -7 139.77 3.90 10 -4 -7 149.68 5.36 10 -4 -7 140.46 3.85 10 -4 -7 147.31 3.93 10 -4 -7 148.93 4.06 10 -4 -7 156.47 3.93 10 -4 -7 152.92 4.97 10 4 -7 139.77 3.77 10 -4 -7 144.01 3.90 10 4 -7 142.88 3.85 10 4 -6 115.67 2.96 10 -4 -6 110.51 3.00 10 4 -6 108.94 2.99 10 -4 -6 114.23 4.02 10 4 -6 112.68 3.99 10 -4 -6 115.93 3.21 -10 4 6 99.86 4.14 -10 -4 6 95.42 4.06 10 4 -6 106.18 3.04 10 -4 -6 112.54 2.95 10 -4 -6 108.28 3.13 10 4 -6 109.02 3.04 10 -4 -6 115.21 4.38 10 4 -6 111.95 3.98 10 -4 -6 116.09 4.02 10 -4 -6 105.08 3.04 10 -4 -5 181.50 5.89 10 -4 -5 189.02 4.98 10 -4 -5 193.38 5.96 10 4 -5 206.95 6.03 10 4 -5 188.34 4.97 10 -4 -5 200.29 6.33 10 -4 -5 198.78 5.12 10 4 -5 210.75 6.06 10 4 -4 707.49 17.05 10 -4 -4 690.11 17.05 -10 4 4 698.88 17.50 10 -4 -4 671.07 17.41 10 -4 -4 688.03 17.15 10 -4 -4 638.37 16.05 10 4 -4 672.18 17.11 10 -4 -4 661.97 16.07 10 -4 -4 698.91 17.48 10 4 -3 373.10 9.38 -10 4 3 338.17 9.69 10 -4 -3 339.72 9.56 10 -4 -3 334.29 8.42 10 -4 -3 349.47 9.69 10 -4 -3 359.61 9.35 10 -4 -3 359.33 9.49 10 4 -3 339.29 9.41 -10 4 3 332.24 8.42 10 4 -2 273.24 7.54 10 -4 -2 284.57 7.62 10 -4 -2 271.25 7.68 10 4 -2 271.51 7.69 -10 4 2 271.91 7.95 10 -4 -2 252.48 7.63 10 -4 -2 261.83 6.70 10 4 -2 282.77 7.75 10 4 -1 36.35 1.80 10 -4 -1 37.49 1.84 10 -4 -1 34.32 1.22 -10 4 1 37.50 2.09 10 -4 -1 35.90 1.83 10 -4 -1 35.41 2.01 10 4 -1 35.64 1.93 10 -4 0 156.50 5.19 10 4 0 161.08 5.07 10 4 0 167.50 5.01 10 -4 0 169.73 5.06 10 -4 0 169.87 5.29 -10 4 0 164.62 5.30 10 -4 0 162.57 4.87 -10 -4 0 160.82 4.87 -10 4 0 165.12 4.88 10 -4 0 161.68 4.14 -10 4 0 152.79 4.17 10 -4 0 153.16 4.16 10 -4 1 41.73 2.18 10 4 1 40.77 2.00 10 -4 1 39.67 2.01 -10 4 -1 43.37 2.25 10 -4 1 44.12 1.38 10 -4 1 41.62 1.78 -10 -4 -1 41.12 1.93 -10 4 -1 39.13 1.89 10 -4 1 44.59 2.24 -10 4 -1 39.27 1.39 10 4 1 42.01 2.11 10 -4 1 39.92 1.40 -10 4 -1 41.45 1.41 10 -4 2 76.24 3.25 10 4 2 76.11 3.05 10 -4 2 76.50 3.07 10 -4 2 77.10 2.21 -10 4 -2 83.26 3.25 -10 4 -2 74.78 2.26 10 -4 2 81.04 2.30 -10 -4 -2 76.43 2.91 -10 4 -2 74.22 2.89 -10 4 -2 77.12 2.27 10 4 2 76.27 3.06 10 -4 2 79.76 3.19 10 -4 2 77.21 2.27 10 -4 3 286.29 7.98 10 -4 3 293.99 8.27 10 -4 3 285.31 6.88 10 4 3 300.26 8.04 10 -4 3 310.71 8.12 -10 4 -3 307.51 8.11 -10 -4 -3 293.87 7.81 -10 4 -3 293.77 7.82 -10 4 -3 280.89 6.85 -10 4 -3 285.63 6.84 10 4 3 301.11 7.90 10 -4 3 292.18 6.87 -10 4 -4 315.95 7.84 10 -4 4 301.54 7.74 10 4 4 307.25 7.76 10 -4 4 328.84 9.35 10 4 4 301.92 7.76 10 4 4 329.97 9.09 10 -4 4 323.56 9.13 -10 4 -4 317.53 8.98 -10 -4 -4 322.25 8.89 -10 4 -4 318.92 8.86 10 -4 4 318.30 7.88 -10 4 -4 318.39 7.83 10 -4 4 318.51 8.96 10 4 4 332.47 8.89 10 -4 4 313.34 7.84 10 -4 5 52.24 1.67 10 4 5 52.86 1.67 10 4 5 53.35 1.72 10 -4 5 54.78 2.52 10 -4 5 55.44 2.84 10 4 5 52.59 2.65 10 -4 5 56.67 2.81 -10 -4 -5 54.30 2.54 -10 4 -5 52.67 2.50 -10 4 -5 53.41 2.54 -10 4 -5 51.07 1.70 10 4 5 54.23 2.46 10 -4 5 51.78 1.77 -10 4 -5 53.21 1.74 10 -4 5 50.47 1.69 10 -4 5 54.34 1.81 10 4 5 52.54 1.79 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-4 2.16 0.52 24 0 -4 1.89 0.50 24 0 -4 1.82 0.41 24 0 -3 8.42 0.68 24 0 -3 8.97 0.62 24 0 -3 9.09 0.69 24 0 -2 0.77 0.46 24 0 -2 0.58 0.49 24 0 -2 0.73 0.39 24 0 -1 -0.02 0.44 24 0 -1 0.25 0.44 24 0 -1 0.40 0.36 24 0 0 2.46 0.51 24 0 0 1.64 0.45 24 0 0 1.91 0.40 24 0 1 3.02 0.50 24 0 1 3.01 0.47 24 0 1 3.55 0.43 24 0 2 0.28 0.42 24 0 2 0.23 0.37 24 0 2 -0.17 0.22 24 0 3 10.92 0.57 24 0 3 11.23 0.60 24 0 4 11.79 0.64 24 0 5 0.16 0.30 24 0 6 0.30 0.25 24 -2 -11 2.09 0.31 24 2 -11 2.91 0.30 24 -2 -11 2.99 0.36 24 2 -11 3.14 0.33 -24 2 11 2.51 0.29 24 -2 -11 2.44 0.33 24 -2 -10 1.36 0.33 24 2 -10 0.67 0.30 24 -2 -10 1.38 0.36 24 2 -10 0.40 0.25 -24 2 10 1.07 0.29 24 2 -10 0.51 0.32 24 -2 -10 0.74 0.34 24 -2 -9 0.84 0.36 24 2 -9 0.56 0.34 24 -2 -9 1.07 0.40 24 2 -9 0.06 0.27 -24 2 9 0.90 0.31 24 2 -9 0.41 0.35 24 -2 -9 0.79 0.37 24 -2 -8 3.33 0.45 24 2 -8 2.76 0.44 24 -2 -8 3.90 0.50 24 2 -8 2.34 0.33 -24 2 8 3.82 0.41 24 2 -8 3.28 0.47 24 -2 -8 3.50 0.48 24 -2 -7 11.24 0.66 24 2 -7 11.42 0.67 24 -2 -7 12.34 0.72 -24 2 7 11.00 0.60 24 2 -7 11.81 0.69 24 -2 -7 12.83 0.72 24 -2 -6 8.89 0.61 24 2 -6 9.54 0.60 24 -2 -6 10.10 0.66 24 -2 -6 8.18 0.67 -24 2 6 9.02 0.52 24 2 -6 10.11 0.64 24 -2 -6 10.85 0.65 24 2 -5 4.30 0.50 24 -2 -5 4.18 0.52 24 -2 -5 3.99 0.56 -24 2 5 4.22 0.42 24 -2 -5 4.85 0.56 24 2 -5 4.82 0.54 24 -2 -4 8.29 0.61 24 2 -4 8.96 0.62 24 -2 -4 8.59 0.69 -24 2 4 6.87 0.50 24 2 -4 8.97 0.65 24 -2 -4 8.08 0.64 24 2 -3 1.94 0.48 24 -2 -3 2.88 0.52 24 -2 -3 1.98 0.46 24 2 -3 2.43 0.46 24 -2 -3 2.65 0.54 24 -2 -2 8.99 0.64 24 2 -2 10.22 0.65 24 -2 -2 9.67 0.70 24 2 -2 9.82 0.68 24 -2 -2 9.76 0.68 24 2 -1 4.05 0.52 24 -2 -1 4.14 0.53 24 2 -1 4.33 0.51 24 -2 -1 3.91 0.50 24 -2 -1 4.63 0.55 24 2 0 0.44 0.41 24 -2 0 0.48 0.43 24 -2 0 0.55 0.42 24 2 0 0.29 0.39 24 -2 0 0.76 0.45 24 -2 1 16.73 0.78 24 2 1 15.34 0.75 24 -2 1 16.56 0.81 24 2 1 16.10 0.79 24 -2 1 16.03 0.79 24 -2 2 5.74 0.49 24 2 2 6.26 0.50 24 -2 2 5.50 0.51 24 2 2 5.62 0.50 24 -2 2 5.57 0.52 24 2 3 3.61 0.42 24 -2 3 4.67 0.42 24 -2 3 3.90 0.44 24 -2 3 4.75 0.45 24 2 4 0.93 0.32 24 -2 4 0.96 0.33 24 -2 4 1.40 0.32 24 2 5 0.88 0.27 24 -2 5 1.66 0.29 -24 2 -5 0.75 0.23 -24 -2 -5 1.05 0.23 24 -2 5 1.13 0.26 24 4 -9 27.33 0.71 -24 4 9 15.66 0.73 24 -4 -8 9.33 0.75 -24 4 8 10.75 0.62 24 -4 -7 9.02 0.50 24 4 -7 8.19 0.50 24 -4 -7 8.90 0.52 24 -4 -7 9.56 0.70 -24 4 7 10.51 0.57 24 -4 -6 4.84 0.39 24 4 -6 5.44 0.40 24 -4 -6 4.98 0.39 -24 4 6 5.82 0.45 24 -4 -6 4.95 0.58 24 -4 -5 3.61 0.36 24 4 -5 3.31 0.35 24 4 -5 3.69 0.37 24 -4 -5 3.83 0.39 -24 4 5 3.68 0.39 24 -4 -5 3.86 0.50 24 -4 -4 1.69 0.31 24 4 -4 2.33 0.33 -24 4 4 2.49 0.35 24 4 -4 2.25 0.34 24 -4 -4 1.90 0.35 24 -4 -3 2.43 0.35 24 4 -3 2.57 0.34 -24 4 3 2.69 0.36 24 4 -3 2.70 0.35 24 -4 -3 2.79 0.37 24 -4 -2 10.18 0.53 24 4 -2 9.78 0.51 -24 4 2 9.65 0.51 24 4 -2 9.23 0.52 24 -4 -2 10.24 0.55 24 -4 -1 6.75 0.44 24 4 -1 6.83 0.43 -24 4 1 5.82 0.38 24 4 -1 6.94 0.43 24 -4 -1 7.46 0.47 24 -4 0 2.86 0.31 24 4 0 2.80 0.33 24 -4 0 2.60 0.33 24 4 1 0.66 0.22 24 -4 1 1.21 0.27 24 -4 2 14.66 0.71 24 -4 3 4.03 0.40 24 -4 4 4.57 0.36 24 -6 -6 1.33 0.28 24 -6 -5 2.77 0.33 24 -6 -4 1.34 0.30 24 -6 -3 3.34 0.37 24 -6 -2 0.81 0.29 24 -6 -1 1.03 0.28 24 -6 0 0.72 0.25 25 1 -10 0.72 0.25 25 -1 -10 1.18 0.27 25 -1 -9 0.26 0.27 25 1 -9 0.08 0.26 25 1 -9 -0.10 0.29 25 -1 -9 0.21 0.30 25 -1 -8 0.80 0.33 25 1 -8 0.50 0.31 25 -1 -8 -0.01 0.27 25 1 -8 0.05 0.32 25 -1 -8 0.19 0.32 25 -1 -7 8.92 0.56 25 1 -7 9.17 0.55 25 -1 -7 9.39 0.52 25 1 -7 9.00 0.57 25 -1 -7 9.96 0.59 25 -1 -6 6.25 0.48 25 1 -6 5.65 0.48 25 -1 -6 6.05 0.47 25 1 -6 5.75 0.50 25 -1 -6 6.83 0.53 25 -1 -5 21.84 0.91 25 1 -5 22.48 0.91 25 -1 -5 22.09 0.88 25 1 -5 23.29 0.93 25 -1 -5 22.96 0.92 25 -1 -4 8.99 0.60 25 1 -4 9.16 0.59 25 -1 -4 8.27 0.54 25 1 -4 10.76 0.62 25 -1 -4 9.26 0.62 25 -1 -3 28.96 1.07 25 1 -3 28.51 1.07 25 -1 -3 28.60 1.03 25 1 -3 29.21 1.08 25 -1 -3 29.96 1.09 25 1 -2 0.89 0.40 25 -1 -2 0.76 0.39 25 -1 -2 0.45 0.36 25 1 -2 0.59 0.38 25 -1 -2 0.86 0.34 25 -1 -1 6.59 0.52 25 1 -1 6.89 0.53 25 -1 -1 7.16 0.50 25 1 -1 7.48 0.56 25 -1 -1 8.24 0.56 25 1 0 1.33 0.37 25 -1 0 1.38 0.38 25 -1 0 1.54 0.37 25 1 0 1.37 0.37 25 -1 0 1.43 0.32 25 1 1 2.48 0.38 25 -1 1 2.20 0.37 25 -1 1 2.05 0.35 25 1 1 2.02 0.36 25 -1 1 2.06 0.31 25 -1 2 4.22 0.39 25 1 2 3.51 0.36 25 1 2 3.89 0.40 25 -1 2 3.88 0.39 25 1 3 0.59 0.27 25 -1 3 0.56 0.28 25 1 4 6.20 0.36 25 -1 4 6.37 0.37 25 -3 -8 2.18 0.33 25 -3 -7 15.62 0.68 25 3 -7 14.27 0.59 25 -3 -7 15.00 0.61 25 -3 -6 8.81 0.47 25 3 -6 8.01 0.45 25 3 -6 9.03 0.48 25 -3 -6 9.56 0.49 25 -3 -5 3.55 0.35 25 3 -5 4.06 0.35 25 -3 -5 3.56 0.43 25 3 -5 3.63 0.37 25 -3 -5 3.64 0.37 25 -3 -4 11.35 0.56 25 3 -4 11.25 0.55 25 -3 -4 12.64 0.65 25 3 -4 12.64 0.58 25 -3 -4 11.79 0.58 25 -3 -3 1.73 0.32 25 3 -3 1.55 0.31 25 -3 -3 2.17 0.40 25 3 -3 1.68 0.33 25 -3 -3 2.27 0.35 25 -3 -2 12.08 0.56 25 3 -2 11.55 0.55 25 -3 -2 13.36 0.66 25 3 -2 11.20 0.56 25 -3 -2 12.31 0.58 25 -3 -1 3.34 0.34 25 3 -1 3.19 0.33 25 -3 -1 3.65 0.41 25 3 -1 3.48 0.35 25 -3 -1 3.65 0.37 25 -3 0 9.00 0.45 25 3 0 8.94 0.44 25 -3 0 9.75 0.54 25 3 0 8.31 0.45 25 -3 0 8.70 0.46 25 3 1 4.83 0.33 25 -3 1 5.24 0.36 25 -3 2 21.41 0.76 25 -5 -4 1.34 0.28 25 -5 -3 0.90 0.26 25 -5 -2 1.46 0.28 26 0 -7 6.43 0.41 26 0 -6 0.46 0.27 26 0 -6 0.48 0.27 26 0 -5 0.16 0.26 26 0 -5 0.11 0.29 26 0 -4 4.37 0.39 26 0 -4 4.09 0.39 26 0 -3 11.92 0.57 26 0 -3 12.39 0.59 26 0 -2 5.16 0.40 26 0 -2 5.14 0.42 26 0 -1 0.97 0.27 26 0 -1 1.24 0.30 26 0 0 8.61 0.44 26 0 0 8.01 0.45 26 0 1 17.10 0.64 26 2 -5 9.70 0.47 26 -2 -5 10.40 0.48 26 2 -4 6.07 0.37 26 -2 -4 4.82 0.37 26 2 -3 1.87 0.27 26 -2 -3 1.62 0.28 26 2 -2 4.01 0.32 26 -2 -2 3.81 0.33 26 -2 -1 0.55 0.23 0 0 0 0.00 0.00 TITL DIJYDROXY_P5 in C2/m REM C2/m (#12 in standard setting) CELL 1.54184 21.249845 11.993440 17.883495 90.0000 98.7257 90.0000 ZERR 20.00 0.000158 0.000098 0.000121 0.0000 0.0007 0.0000 LATT 7 SYMM -x, y,-z SFAC C H N O UNIT 220.00 200.00 20.00 20.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 85578 _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 1.758 _oxdiff_exptl_absorpt_empirical_full_min 0.514 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O11 O 0.51446(9) 0.61294(17) 0.39076(10) 0.0503(4) Uani 1 1 d . . . . . O4 O 0.18989(9) 0.24255(15) 0.24689(10) 0.0474(4) Uani 1 1 d . . . . . O6 O 0.07010(9) 0.52166(16) 0.07617(11) 0.0518(4) Uani 1 1 d . . . . . O7 O 0.17894(10) 0.91580(17) 0.19261(12) 0.0542(5) Uani 1 1 d . . . . . O13 O 0.30474(9) 0.43615(17) 0.48745(11) 0.0524(5) Uani 1 1 d . . . . . O9 O 0.38176(11) 0.6150(2) -0.00320(11) 0.0630(6) Uani 1 1 d . . . . . H9 H 0.413532 0.583508 0.018771 0.094 Uiso 1 1 calc GR . . . . O12 O 0.42350(9) 0.2185(2) 0.27531(14) 0.0629(6) Uani 1 1 d . . . . . O10 O 0.46717(10) 0.4859(2) 0.08985(10) 0.0594(5) Uani 1 1 d . . . . . O5 O 0.09381(11) 0.61286(19) 0.37578(12) 0.0627(6) Uani 1 1 d . . . . . O8 O 0.29931(11) 0.95412(19) 0.16659(13) 0.0631(5) Uani 1 1 d . . . . . H8 H 0.261428 0.947610 0.169926 0.095 Uiso 1 1 calc GR . . . . C7 C 0.16433(11) 0.33503(18) 0.27748(13) 0.0360(4) Uani 1 1 d . . . . . C34 C 0.42784(11) 0.3528(2) 0.37244(13) 0.0397(5) Uani 1 1 d . . . . . C12 C 0.15103(12) 0.8167(2) 0.16450(14) 0.0417(5) Uani 1 1 d . . . . . C25 C 0.48541(11) 0.6280(2) 0.18100(14) 0.0446(5) Uani 1 1 d . . . . . C5 C 0.09654(10) 0.4981(2) 0.26998(13) 0.0377(5) Uani 1 1 d . . . . . C6 C 0.12017(11) 0.4048(2) 0.23657(13) 0.0370(4) Uani 1 1 d . . . . . H6 H 0.105896 0.389348 0.185872 0.044 Uiso 1 1 calc R . . . . C10 C 0.08732(10) 0.6516(2) 0.17529(13) 0.0387(5) Uani 1 1 d . . . . . C27 C 0.50269(10) 0.5836(2) 0.31496(13) 0.0410(5) Uani 1 1 d . . . . . C11 C 0.11372(11) 0.7515(2) 0.20475(13) 0.0400(5) Uani 1 1 d . . . . . H11 H 0.106264 0.774952 0.252184 0.048 Uiso 1 1 calc R . . . . C35 C 0.39856(11) 0.4089(2) 0.42566(13) 0.0385(5) Uani 1 1 d . . . . . H35 H 0.421050 0.463476 0.455513 0.046 Uiso 1 1 calc R . . . . C2 C 0.18567(11) 0.35505(19) 0.35408(13) 0.0370(5) Uani 1 1 d . . . . . C37 C 0.30155(11) 0.30302(19) 0.39110(13) 0.0375(5) Uani 1 1 d . . . . . C1 C 0.23330(11) 0.2774(2) 0.39937(13) 0.0398(5) Uani 1 1 d . . . . . H1A H 0.228648 0.282583 0.452388 0.048 Uiso 1 1 calc R . . . . H1B H 0.223652 0.201325 0.383132 0.048 Uiso 1 1 calc R . . . . C36 C 0.33606(11) 0.38496(19) 0.43526(12) 0.0376(5) Uani 1 1 d . . . . . C39 C 0.39296(12) 0.2709(2) 0.32823(15) 0.0443(5) Uani 1 1 d . . . . . C28 C 0.49410(10) 0.4704(2) 0.29930(14) 0.0405(5) Uani 1 1 d . . . . . C4 C 0.11827(12) 0.5188(2) 0.34636(14) 0.0427(5) Uani 1 1 d . . . . . C26 C 0.49875(11) 0.6608(2) 0.25674(14) 0.0432(5) Uani 1 1 d . . . . . H26 H 0.505114 0.735913 0.268322 0.052 Uiso 1 1 calc R . . . . C14 C 0.13615(12) 0.6849(2) 0.06381(13) 0.0442(5) Uani 1 1 d . . . . . H14 H 0.143492 0.661914 0.016229 0.053 Uiso 1 1 calc R . . . . C47 C 0.05141(11) 0.5770(2) 0.22193(14) 0.0413(5) Uani 1 1 d . . . . . H47A H 0.020010 0.534272 0.188697 0.050 Uiso 1 1 calc R . . . . H47B H 0.029115 0.622300 0.254445 0.050 Uiso 1 1 calc R . . . . C15 C 0.09835(11) 0.6196(2) 0.10305(13) 0.0407(5) Uani 1 1 d . . . . . C48 C 0.47478(13) 0.7155(3) 0.11928(15) 0.0525(6) Uani 1 1 d . . . . . H48A H 0.489647 0.686988 0.074306 0.063 Uiso 1 1 calc R . . . . H48B H 0.499661 0.781280 0.135719 0.063 Uiso 1 1 calc R . . . . C13 C 0.16338(12) 0.7839(2) 0.09355(13) 0.0429(5) Uani 1 1 d . . . . . C20 C 0.31802(13) 0.8667(2) 0.12531(14) 0.0479(6) Uani 1 1 d . . . . . C3 C 0.16134(12) 0.4475(2) 0.38763(14) 0.0421(5) Uani 1 1 d . . . . . H3 H 0.174396 0.461273 0.438799 0.050 Uiso 1 1 calc R . . . . C23 C 0.36309(13) 0.6966(2) 0.04266(13) 0.0473(6) Uani 1 1 d . . . . . C38 C 0.33146(11) 0.2465(2) 0.33868(14) 0.0424(5) Uani 1 1 d . . . . . H38 H 0.309406 0.190535 0.309730 0.051 Uiso 1 1 calc R . . . . C24 C 0.29999(13) 0.7299(3) 0.02752(13) 0.0472(6) Uani 1 1 d . . . . . H24 H 0.272809 0.694015 -0.010652 0.057 Uiso 1 1 calc R . . . . C29 C 0.48306(12) 0.4376(2) 0.22366(15) 0.0460(6) Uani 1 1 d . . . . . H29 H 0.478380 0.362213 0.211850 0.055 Uiso 1 1 calc R . . . . C19 C 0.27603(12) 0.8155(2) 0.06780(14) 0.0454(6) Uani 1 1 d . . . . . O3 O 0.19912(15) 0.2032(3) 0.71170(17) 0.0904(9) Uani 1 1 d . . . . . C22 C 0.40495(12) 0.7481(2) 0.09967(13) 0.0469(6) Uani 1 1 d . . . . . C30 C 0.47893(11) 0.5154(3) 0.16573(14) 0.0460(6) Uani 1 1 d . . . . . C21 C 0.38075(13) 0.8325(2) 0.14035(14) 0.0488(6) Uani 1 1 d . . . . . H21 H 0.407799 0.867299 0.179149 0.059 Uiso 1 1 calc R . . . . C33 C 0.49499(11) 0.3833(2) 0.36072(14) 0.0447(5) Uani 1 1 d . . . . . H33A H 0.518316 0.411768 0.407660 0.054 Uiso 1 1 calc R . . . . H33B H 0.516744 0.317059 0.346807 0.054 Uiso 1 1 calc R . . . . C32 C 0.54286(16) 0.7188(3) 0.40870(17) 0.0586(7) Uani 1 1 d . . . . . H32A H 0.513800 0.776522 0.388752 0.088 Uiso 1 1 calc GR . . . . H32B H 0.581280 0.724774 0.386816 0.088 Uiso 1 1 calc GR . . . . H32C H 0.552699 0.726500 0.462634 0.088 Uiso 1 1 calc GR . . . . O1 O 0.20948(17) 0.4414(4) 0.59294(18) 0.1031(10) Uani 1 1 d . . . . . H1 H 0.217110 0.402581 0.557639 0.155 Uiso 1 1 calc GR . . . . C18 C 0.20645(13) 0.8502(3) 0.04970(15) 0.0498(6) Uani 1 1 d . . . . . H18A H 0.202838 0.928737 0.061241 0.060 Uiso 1 1 calc R . . . . H18B H 0.192156 0.840379 -0.004029 0.060 Uiso 1 1 calc R . . . . C16 C 0.08457(17) 0.4798(3) 0.00638(19) 0.0661(8) Uani 1 1 d . . . . . H16A H 0.067663 0.529398 -0.033849 0.099 Uiso 1 1 calc GR . . . . H16B H 0.065901 0.407309 -0.002924 0.099 Uiso 1 1 calc GR . . . . H16C H 0.129907 0.474546 0.008786 0.099 Uiso 1 1 calc GR . . . . C17 C 0.16040(15) 0.9608(3) 0.25975(17) 0.0550(7) Uani 1 1 d . . . . . H17A H 0.115404 0.974849 0.251507 0.083 Uiso 1 1 calc GR . . . . H17B H 0.182841 1.029288 0.272506 0.083 Uiso 1 1 calc GR . . . . H17C H 0.170463 0.908497 0.300453 0.083 Uiso 1 1 calc GR . . . . C41 C 0.33507(17) 0.5283(3) 0.5263(2) 0.0681(9) Uani 1 1 d . . . . . H41A H 0.342987 0.584300 0.490447 0.102 Uiso 1 1 calc GR . . . . H41B H 0.374722 0.504957 0.555021 0.102 Uiso 1 1 calc GR . . . . H41C H 0.308178 0.558624 0.559779 0.102 Uiso 1 1 calc GR . . . . C31 C 0.4538(2) 0.3712(4) 0.0735(2) 0.0779(11) Uani 1 1 d . . . . . H31A H 0.440081 0.362197 0.020151 0.117 Uiso 1 1 calc GR . . . . H31B H 0.420842 0.346290 0.100707 0.117 Uiso 1 1 calc GR . . . . H31C H 0.491611 0.327815 0.088516 0.117 Uiso 1 1 calc GR . . . . C8 C 0.17149(19) 0.2229(3) 0.16892(16) 0.0651(8) Uani 1 1 d . . . . . H8A H 0.180588 0.287713 0.140909 0.098 Uiso 1 1 calc GR . . . . H8B H 0.126682 0.207390 0.159017 0.098 Uiso 1 1 calc GR . . . . H8C H 0.194680 0.160271 0.153732 0.098 Uiso 1 1 calc GR . . . . C40 C 0.38624(17) 0.1485(4) 0.2232(3) 0.0930(15) Uani 1 1 d . . . . . H40A H 0.411623 0.121069 0.187088 0.140 Uiso 1 1 calc GR . . . . H40B H 0.350776 0.189853 0.197320 0.140 Uiso 1 1 calc GR . . . . H40C H 0.370876 0.086898 0.249521 0.140 Uiso 1 1 calc GR . . . . C44 C 0.2171(2) 0.2617(4) 0.6555(2) 0.0865(12) Uani 1 1 d . . . . . O2 O 0.2535(3) 0.2330(4) 0.6165(3) 0.1412(17) Uani 1 1 d . . . . . C9 C 0.1158(2) 0.6377(3) 0.4529(2) 0.0793(11) Uani 1 1 d . . . . . H9A H 0.160647 0.653108 0.459388 0.119 Uiso 1 1 calc GR . . . . H9B H 0.108092 0.575118 0.483660 0.119 Uiso 1 1 calc GR . . . . H9C H 0.093589 0.701782 0.467692 0.119 Uiso 1 1 calc GR . . . . C43 C 0.18323(19) 0.3745(5) 0.6453(2) 0.0884(13) Uani 1 1 d . . . . . H43 H 0.192569 0.412783 0.694187 0.106 Uiso 1 1 calc R . . . . C45 C 0.2286(3) 0.0918(4) 0.7274(4) 0.1044(16) Uani 1 1 d . . . . . H45A H 0.221794 0.046371 0.682004 0.125 Uiso 1 1 calc R . . . . H45B H 0.274123 0.099601 0.743265 0.125 Uiso 1 1 calc R . . . . C46 C 0.2002(3) 0.0400(6) 0.7857(4) 0.120(2) Uani 1 1 d . . . . . H46A H 0.156655 0.022282 0.766921 0.180 Uiso 1 1 calc GR . . . . H46B H 0.201963 0.090011 0.827905 0.180 Uiso 1 1 calc GR . . . . H46C H 0.222971 -0.027148 0.801658 0.180 Uiso 1 1 calc GR . . . . C42 C 0.1112(3) 0.3705(12) 0.6260(4) 0.176(4) Uani 1 1 d . . . . . H42A H 0.094987 0.444592 0.616262 0.264 Uiso 1 1 calc GR . . . . H42B H 0.093634 0.338975 0.667639 0.264 Uiso 1 1 calc GR . . . . H42C H 0.099465 0.325193 0.581788 0.264 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 O11 0.0556(10) 0.0592(11) 0.0348(8) -0.0090(8) 0.0031(7) -0.0126(9) O4 0.0603(10) 0.0394(9) 0.0412(9) -0.0065(7) 0.0029(7) 0.0101(8) O6 0.0579(11) 0.0495(10) 0.0463(9) -0.0187(8) 0.0028(8) -0.0021(8) O7 0.0585(11) 0.0472(10) 0.0580(11) -0.0137(9) 0.0123(9) -0.0111(8) O13 0.0525(10) 0.0590(11) 0.0470(9) -0.0172(8) 0.0120(8) -0.0079(8) O9 0.0605(12) 0.0833(15) 0.0418(10) -0.0088(10) -0.0029(8) 0.0080(11) O12 0.0422(9) 0.0677(13) 0.0795(14) -0.0374(11) 0.0116(9) -0.0053(9) O10 0.0619(11) 0.0750(14) 0.0380(9) -0.0140(9) -0.0033(8) 0.0075(10) O5 0.0707(13) 0.0612(12) 0.0531(11) -0.0231(10) -0.0013(9) 0.0202(10) O8 0.0638(12) 0.0590(13) 0.0664(13) -0.0122(10) 0.0091(10) -0.0116(10) C7 0.0373(11) 0.0327(10) 0.0390(11) -0.0034(9) 0.0093(8) -0.0038(8) C34 0.0382(11) 0.0397(12) 0.0388(11) 0.0013(9) -0.0025(9) 0.0002(9) C12 0.0411(11) 0.0388(12) 0.0431(12) -0.0046(9) -0.0009(9) 0.0012(9) C25 0.0345(11) 0.0610(16) 0.0379(12) -0.0016(11) 0.0040(9) -0.0072(11) C5 0.0308(10) 0.0395(12) 0.0432(12) -0.0067(9) 0.0069(8) -0.0033(8) C6 0.0366(10) 0.0382(11) 0.0361(10) -0.0063(9) 0.0048(8) -0.0040(9) C10 0.0333(10) 0.0406(12) 0.0398(11) -0.0068(9) -0.0020(8) 0.0093(9) C27 0.0308(10) 0.0558(14) 0.0362(11) -0.0060(10) 0.0041(8) -0.0073(10) C11 0.0392(11) 0.0412(12) 0.0383(11) -0.0076(9) 0.0017(9) 0.0063(9) C35 0.0417(11) 0.0364(11) 0.0343(10) 0.0016(9) -0.0039(8) -0.0038(9) C2 0.0368(11) 0.0369(11) 0.0377(11) 0.0011(9) 0.0075(8) -0.0079(9) C37 0.0411(11) 0.0343(11) 0.0358(11) 0.0049(8) 0.0013(9) -0.0015(9) C1 0.0439(12) 0.0380(12) 0.0376(11) 0.0022(9) 0.0067(9) -0.0072(9) C36 0.0442(12) 0.0359(11) 0.0317(10) 0.0012(8) 0.0020(8) 0.0001(9) C39 0.0393(12) 0.0416(13) 0.0507(13) -0.0080(10) 0.0030(10) 0.0022(10) C28 0.0272(9) 0.0505(13) 0.0425(12) -0.0029(10) 0.0010(8) -0.0017(9) C4 0.0406(11) 0.0441(12) 0.0440(12) -0.0111(10) 0.0084(9) 0.0005(10) C26 0.0378(11) 0.0506(14) 0.0408(12) -0.0044(10) 0.0046(9) -0.0081(10) C14 0.0454(12) 0.0514(14) 0.0333(11) -0.0043(10) -0.0016(9) 0.0095(10) C47 0.0309(10) 0.0459(13) 0.0456(12) -0.0106(10) 0.0014(9) 0.0024(9) C15 0.0390(11) 0.0418(12) 0.0385(11) -0.0084(9) -0.0034(9) 0.0078(9) C48 0.0458(13) 0.0705(18) 0.0412(12) 0.0062(12) 0.0070(10) -0.0128(12) C13 0.0418(12) 0.0473(13) 0.0371(11) 0.0026(10) -0.0024(9) 0.0066(10) C20 0.0551(14) 0.0483(14) 0.0402(12) 0.0039(10) 0.0075(10) -0.0121(11) C3 0.0421(12) 0.0474(13) 0.0367(11) -0.0062(9) 0.0061(9) -0.0052(10) C23 0.0511(13) 0.0600(15) 0.0300(11) 0.0062(10) 0.0037(9) -0.0021(12) C38 0.0412(12) 0.0359(11) 0.0481(12) -0.0058(10) -0.0001(9) -0.0025(9) C24 0.0498(13) 0.0587(15) 0.0312(10) 0.0048(10) -0.0001(9) -0.0061(11) C29 0.0380(12) 0.0523(14) 0.0447(12) -0.0095(11) -0.0029(9) -0.0004(10) C19 0.0488(13) 0.0520(15) 0.0346(11) 0.0099(10) 0.0035(9) -0.0071(11) O3 0.0914(19) 0.107(2) 0.0786(17) -0.0217(16) 0.0314(15) -0.0083(17) C22 0.0472(12) 0.0586(15) 0.0345(11) 0.0105(11) 0.0051(9) -0.0111(11) C30 0.0344(11) 0.0659(16) 0.0357(11) -0.0088(11) -0.0015(9) 0.0005(11) C21 0.0508(14) 0.0564(15) 0.0388(12) 0.0031(11) 0.0052(10) -0.0179(12) C33 0.0354(11) 0.0495(14) 0.0461(13) -0.0004(10) -0.0034(9) -0.0016(10) C32 0.0679(17) 0.0555(16) 0.0481(14) -0.0124(12) -0.0056(12) -0.0019(14) O1 0.100(2) 0.140(3) 0.0726(17) 0.0043(19) 0.0252(16) -0.002(2) C18 0.0539(14) 0.0547(15) 0.0384(12) 0.0082(11) -0.0002(10) 0.0025(12) C16 0.0681(18) 0.070(2) 0.0590(17) -0.0328(16) 0.0079(14) 0.0010(16) C17 0.0573(15) 0.0495(15) 0.0581(16) -0.0161(12) 0.0077(12) -0.0073(12) C41 0.0686(19) 0.0646(19) 0.072(2) -0.0313(17) 0.0149(16) -0.0072(16) C31 0.086(2) 0.086(2) 0.0541(17) -0.0305(17) -0.0154(16) 0.009(2) C8 0.094(2) 0.0599(17) 0.0404(13) -0.0099(12) 0.0078(14) 0.0276(17) C40 0.0515(17) 0.117(3) 0.111(3) -0.075(3) 0.0135(18) -0.0095(19) C44 0.094(3) 0.104(3) 0.066(2) -0.029(2) 0.026(2) -0.016(2) O2 0.192(4) 0.124(3) 0.134(3) -0.025(3) 0.108(3) 0.001(3) C9 0.101(3) 0.077(2) 0.0553(18) -0.0308(17) -0.0019(17) 0.025(2) C43 0.072(2) 0.146(4) 0.0477(17) -0.014(2) 0.0100(15) 0.000(3) C45 0.098(3) 0.081(3) 0.142(5) -0.031(3) 0.040(3) -0.005(2) C46 0.126(4) 0.108(4) 0.137(5) 0.005(4) 0.057(4) 0.017(3) C42 0.087(4) 0.342(14) 0.094(4) 0.016(6) 0.000(3) -0.041(6) 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 C27 O11 C32 117.1(2) . . ? C7 O4 C8 117.3(2) . . ? C15 O6 C16 117.9(2) . . ? C12 O7 C17 118.1(2) . . ? C36 O13 C41 117.0(2) . . ? C23 O9 H9 109.5 . . ? C39 O12 C40 116.8(2) . . ? C30 O10 C31 116.6(3) . . ? C4 O5 C9 117.1(2) . . ? C20 O8 H8 109.5 . . ? O4 C7 C2 115.9(2) . . ? C6 C7 O4 123.5(2) . . ? C6 C7 C2 120.6(2) . . ? C35 C34 C39 118.2(2) . . ? C35 C34 C33 120.5(2) . . ? C39 C34 C33 121.3(2) . . ? O7 C12 C11 122.7(2) . . ? O7 C12 C13 116.3(2) . . ? C11 C12 C13 121.0(2) . . ? C26 C25 C48 119.8(3) . . ? C30 C25 C26 117.8(2) . . ? C30 C25 C48 122.3(2) . . ? C6 C5 C47 119.6(2) . . ? C4 C5 C6 118.3(2) . . ? C4 C5 C47 122.0(2) . . ? C7 C6 C5 121.2(2) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C11 C10 C47 120.7(2) . . ? C11 C10 C15 118.1(2) . . ? C15 C10 C47 121.1(2) . . ? O11 C27 C28 116.3(2) . . ? O11 C27 C26 123.1(2) . . ? C26 C27 C28 120.6(2) . . ? C12 C11 C10 121.1(2) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C34 C35 H35 119.4 . . ? C34 C35 C36 121.3(2) . . ? C36 C35 H35 119.4 . . ? C7 C2 C1 120.6(2) . . ? C3 C2 C7 118.1(2) . . ? C3 C2 C1 121.2(2) . . ? C36 C37 C1 121.1(2) . . ? C38 C37 C1 120.8(2) . . ? C38 C37 C36 118.1(2) . . ? C2 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? C37 C1 C2 113.29(19) . . ? C37 C1 H1A 108.9 . . ? C37 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? O13 C36 C35 124.2(2) . . ? O13 C36 C37 115.6(2) . . ? C35 C36 C37 120.2(2) . . ? O12 C39 C34 116.3(2) . . ? O12 C39 C38 123.5(2) . . ? C38 C39 C34 120.2(2) . . ? C27 C28 C29 117.9(2) . . ? C27 C28 C33 122.7(2) . . ? C29 C28 C33 119.4(2) . . ? O5 C4 C5 115.5(2) . . ? O5 C4 C3 124.1(2) . . ? C3 C4 C5 120.4(2) . . ? C25 C26 H26 119.3 . . ? C27 C26 C25 121.4(2) . . ? C27 C26 H26 119.3 . . ? C15 C14 H14 119.1 . . ? C15 C14 C13 121.9(2) . . ? C13 C14 H14 119.1 . . ? C5 C47 H47A 109.5 . . ? C5 C47 H47B 109.5 . . ? C10 C47 C5 110.73(18) . . ? C10 C47 H47A 109.5 . . ? C10 C47 H47B 109.5 . . ? H47A C47 H47B 108.1 . . ? O6 C15 C10 115.6(2) . . ? O6 C15 C14 124.2(2) . . ? C14 C15 C10 120.1(2) . . ? C25 C48 H48A 109.2 . . ? C25 C48 H48B 109.2 . . ? C25 C48 C22 112.2(2) . . ? H48A C48 H48B 107.9 . . ? C22 C48 H48A 109.2 . . ? C22 C48 H48B 109.2 . . ? C12 C13 C18 122.4(2) . . ? C14 C13 C12 117.7(2) . . ? C14 C13 C18 119.9(2) . . ? O8 C20 C19 121.7(3) . . ? O8 C20 C21 118.1(2) . . ? C21 C20 C19 120.2(3) . . ? C2 C3 H3 119.3 . . ? C4 C3 C2 121.4(2) . . ? C4 C3 H3 119.3 . . ? O9 C23 C24 116.6(2) . . ? O9 C23 C22 122.9(2) . . ? C24 C23 C22 120.4(3) . . ? C37 C38 H38 119.0 . . ? C39 C38 C37 121.9(2) . . ? C39 C38 H38 119.0 . . ? C23 C24 H24 119.0 . . ? C23 C24 C19 122.0(2) . . ? C19 C24 H24 119.0 . . ? C28 C29 H29 119.4 . . ? C30 C29 C28 121.1(3) . . ? C30 C29 H29 119.4 . . ? C20 C19 C18 121.9(3) . . ? C24 C19 C20 117.5(2) . . ? C24 C19 C18 120.7(2) . . ? C44 O3 C45 117.2(4) . . ? C23 C22 C48 123.1(3) . . ? C21 C22 C48 119.4(2) . . ? C21 C22 C23 117.4(2) . . ? C25 C30 O10 116.1(2) . . ? C25 C30 C29 121.2(2) . . ? C29 C30 O10 122.7(3) . . ? C20 C21 C22 122.5(2) . . ? C20 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C34 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? C28 C33 C34 110.95(19) . . ? C28 C33 H33A 109.4 . . ? C28 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? O11 C32 H32A 109.5 . . ? O11 C32 H32B 109.5 . . ? O11 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C43 O1 H1 109.5 . . ? C13 C18 C19 112.9(2) . . ? C13 C18 H18A 109.0 . . ? C13 C18 H18B 109.0 . . ? C19 C18 H18A 109.0 . . ? C19 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? O6 C16 H16A 109.5 . . ? O6 C16 H16B 109.5 . . ? O6 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O7 C17 H17A 109.5 . . ? O7 C17 H17B 109.5 . . ? O7 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O13 C41 H41A 109.5 . . ? O13 C41 H41B 109.5 . . ? O13 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O10 C31 H31A 109.5 . . ? O10 C31 H31B 109.5 . . ? O10 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O4 C8 H8A 109.5 . . ? O4 C8 H8B 109.5 . . ? O4 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O12 C40 H40A 109.5 . . ? O12 C40 H40B 109.5 . . ? O12 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O3 C44 C43 111.9(3) . . ? O2 C44 O3 126.0(5) . . ? O2 C44 C43 122.0(5) . . ? O5 C9 H9A 109.5 . . ? O5 C9 H9B 109.5 . . ? O5 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C43 C44 110.8(3) . . ? O1 C43 H43 106.2 . . ? O1 C43 C42 110.7(5) . . ? C44 C43 H43 106.2 . . ? C42 C43 C44 116.0(7) . . ? C42 C43 H43 106.2 . . ? O3 C45 H45A 110.0 . . ? O3 C45 H45B 110.0 . . ? H45A C45 H45B 108.4 . . ? C46 C45 O3 108.5(4) . . ? C46 C45 H45A 110.0 . . ? C46 C45 H45B 110.0 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C43 C42 H42A 109.5 . . ? C43 C42 H42B 109.5 . . ? C43 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 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 O11 C27 1.386(3) . ? O11 C32 1.421(4) . ? O4 C7 1.384(3) . ? O4 C8 1.410(3) . ? O6 C15 1.372(3) . ? O6 C16 1.421(3) . ? O7 C12 1.388(3) . ? O7 C17 1.425(3) . ? O13 C36 1.371(3) . ? O13 C41 1.409(4) . ? O9 H9 0.8200 . ? O9 C23 1.373(4) . ? O12 C39 1.378(3) . ? O12 C40 1.406(4) . ? O10 C30 1.388(3) . ? O10 C31 1.426(5) . ? O5 C4 1.379(3) . ? O5 C9 1.418(4) . ? O8 H8 0.8200 . ? O8 C20 1.376(4) . ? C7 C6 1.381(3) . ? C7 C2 1.397(3) . ? C34 C35 1.387(3) . ? C34 C39 1.401(3) . ? C34 C33 1.518(3) . ? C12 C11 1.390(4) . ? C12 C13 1.391(3) . ? C25 C26 1.397(3) . ? C25 C48 1.515(4) . ? C25 C30 1.381(4) . ? C5 C6 1.397(3) . ? C5 C4 1.396(3) . ? C5 C47 1.518(3) . ? C6 H6 0.9300 . ? C10 C11 1.391(3) . ? C10 C47 1.507(4) . ? C10 C15 1.401(3) . ? C27 C28 1.392(4) . ? C27 C26 1.387(4) . ? C11 H11 0.9300 . ? C35 H35 0.9300 . ? C35 C36 1.395(3) . ? C2 C1 1.516(3) . ? C2 C3 1.396(3) . ? C37 C1 1.512(3) . ? C37 C36 1.397(3) . ? C37 C38 1.387(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C39 C38 1.379(4) . ? C28 C29 1.394(3) . ? C28 C33 1.514(4) . ? C4 C3 1.382(4) . ? C26 H26 0.9300 . ? C14 H14 0.9300 . ? C14 C15 1.387(4) . ? C14 C13 1.390(4) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 C22 1.523(4) . ? C13 C18 1.517(4) . ? C20 C19 1.397(4) . ? C20 C21 1.381(4) . ? C3 H3 0.9300 . ? C23 C24 1.386(4) . ? C23 C22 1.392(4) . ? C38 H38 0.9300 . ? C24 H24 0.9300 . ? C24 C19 1.395(4) . ? C29 H29 0.9300 . ? C29 C30 1.387(4) . ? C19 C18 1.523(4) . ? O3 C44 1.328(5) . ? O3 C45 1.485(7) . ? C22 C21 1.390(4) . ? C21 H21 0.9300 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? O1 H1 0.8200 . ? O1 C43 1.411(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C44 O2 1.170(5) . ? C44 C43 1.531(8) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C43 H43 0.9800 . ? C43 C42 1.518(7) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 C46 1.424(8) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ?