#------------------------------------------------------------------------------ #$Date: 2021-10-02 02:03:01 +0300 (Sat, 02 Oct 2021) $ #$Revision: 269444 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/84/7708499.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_7708499 loop_ _publ_author_name 'Arp, Fabian Felix' 'Ashirov, Rahym' 'Bhuvanesh, Nattamai' 'Bluemel, Janet' _publ_section_title ; Di(hydroperoxy)adamantane Adducts: Synthesis, Characterization and Application as Oxidizers for the Direct Esterification of Aldehydes ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03243G _journal_year 2021 _chemical_formula_moiety 'C18 H33 O P, C10 H15 O4' _chemical_formula_sum 'C28 H48 O5 P' _chemical_formula_weight 495.63 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2019-11-21 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-01-29 deposited with the CCDC. 2021-09-30 downloaded from the CCDC. ; _cell_angle_alpha 99.3060(10) _cell_angle_beta 96.0350(10) _cell_angle_gamma 90.6870(10) _cell_formula_units_Z 2 _cell_length_a 9.6844(3) _cell_length_b 11.1339(4) _cell_length_c 13.0829(5) _cell_measurement_reflns_used 9176 _cell_measurement_temperature 110.0 _cell_measurement_theta_max 27.436 _cell_measurement_theta_min 2.235 _cell_volume 1383.78(8) _computing_cell_refinement 'SAINT V8.38 Bruker AXS Inc., Madison, WI, USA.' _computing_data_reduction 'SAINT V8.38 Bruker AXS Inc., Madison, WI, USA.' _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_temperature 110.0 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker PHOTON II' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_unetI/netI 0.0211 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 14566 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 24.998 _diffrn_reflns_theta_max 24.998 _diffrn_reflns_theta_min 2.234 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.134 _exptl_absorpt_correction_T_max 0.4305 _exptl_absorpt_correction_T_min 0.4023 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1273 before and 0.0534 after correction. The Ratio of minimum to maximum transmission is 0.9345. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.190 _exptl_crystal_description block _exptl_crystal_F_000 542 _exptl_crystal_size_max 0.526 _exptl_crystal_size_mid 0.397 _exptl_crystal_size_min 0.322 _refine_diff_density_max 0.381 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.041 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 410 _refine_ls_number_reflns 4842 _refine_ls_number_restraints 821 _refine_ls_restrained_S_all 0.984 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0395 _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^)+(0.0435P)^2^+0.8664P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0993 _refine_ls_wR_factor_ref 0.1015 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4456 _reflns_number_total 4842 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03243g2.cif _cod_data_source_block ffe409 _cod_database_code 7708499 _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 0.958 _shelx_estimated_absorpt_t_min 0.933 _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 O(H) groups 2. Restrained distances O5-O4 \\sim O5A-O4A \\sim O3A-O2A \\sim O3-O2 with sigma of 0.005 O4-C19 \\sim O4A-C19A \\sim O2A-C19A \\sim O2-C19 with sigma of 0.005 3. Uiso/Uaniso restraints and constraints O2 \\sim O3 \\sim O4 \\sim O5 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim O2A \\sim O3A \\sim O4A \\sim O5A \\sim C19A \\sim C20A \\sim C21A \\sim C22A \\sim C23A \\sim C24A \\sim C25A \\sim C26A \\sim C27A \\sim C28A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C19A) = Uanis(C19) Uanis(O3) = Uanis(O3A) Uanis(O5A) = Uanis(O5) Uanis(C21A) = Uanis(C27) 4. Rigid body (RIGU) restrains O2, O3, O4, O5, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, O2A, O3A, O4A, O5A, C19A, C20A, C21A, C22A, C23A, C24A, C25A, C26A, C27A, C28A with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 5. Same fragment restrains {O2, O3, O4, O5, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28} sigma for 1-2: 0.01, 1-3: 0.04 as {O2A, O3A, O4A, O5A, C19A, C20A, C21A, C22A, C23A, C24A, C25A, C26A, C27A, C28A} 6. Others Sof(O2A)=Sof(O3A)=Sof(H3AA)=Sof(O4A)=Sof(O5A)=Sof(H5AA)=Sof(C19A)=Sof(C20A)= Sof(H20A)=Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C22A)=Sof(H22A)=Sof(C23A)= Sof(H23C)=Sof(H23D)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25C)=Sof(H25D)= Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=1-FVAR(1) Sof(O2)=Sof(O3)=Sof(H3)=Sof(O4)=Sof(O5)=Sof(H5)=Sof(C19)=Sof(C20)=Sof(H20)= Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23A)=Sof(H23B)= Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)= Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=FVAR(1) 7.a Riding coordinates: O3(H3), O5(H5), O3A(H3AA), O5A(H5AA) 7.b Ternary CH refined with riding coordinates: C1(H1), C7(H7), C13(H13), C20(H20), C22(H22), C24(H24), C28(H28), C20A(H20A), C22A(H22A), C24A(H24A), C28A(H28A) 7.c Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C21(H21A,H21B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B), C21A(H21C,H21D), C23A(H23C, H23D), C25A(H25C,H25D), C26A(H26C,H26D) 7.d Aromatic/amide H refined with riding coordinates: C27(H27), C27A(H27A) ; _shelx_res_file ; TITL ffe409_a.res in P-1 ffe409.res created by SHELXL-2018/3 at 12:26:34 on 21-Nov-2019 REM Old TITL FFE409 in P-1 REM SHELXT solution in P-1: R1 0.211, Rweak 0.013, Alpha 0.070 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C36 O4 P CELL 0.71073 9.6844 11.1339 13.0829 99.306 96.035 90.687 ZERR 2 0.0003 0.0004 0.0005 0.001 0.001 0.001 LATT 1 SFAC C H O P UNIT 56 96 10 2 SADI 0.005 O5 O4 O5A O4A O3A O2A O3 O2 SADI 0.005 O4 C19 O4A C19A O2A C19A O2 C19 SIMU 0.01 0.02 2 O2 > C28A RIGU 0.01 0.01 O2 > C28A EADP C19A C19 EADP O3 O3A EADP O5A O5 EADP C21A C27 L.S. 8 PLAN 20 SIZE 0.322 0.397 0.526 TEMP -163.15 HTAB O3 O1 HTAB O5 O1 HTAB O3A O1 HTAB O5A O1 FREE C23A C21A acta BOND $H more -1 wpdb -1 htab conf list 4 fmap 2 53 OMIT -4 50 OMIT 1 1 0 OMIT 1 0 0 OMIT 0 1 0 OMIT 0 -2 6 OMIT 4 1 0 REM REM REM WGHT 0.043500 0.866400 FVAR 1.00321 0.59889 P1 4 0.591852 0.253757 0.387861 11.00000 0.01453 0.01592 = 0.01954 0.00245 0.00071 0.00171 O1 3 0.594139 0.279958 0.504760 11.00000 0.02601 0.02347 = 0.02068 0.00346 0.00051 0.00057 C1 1 0.657217 0.102960 0.346140 11.00000 0.01801 0.01486 = 0.02941 0.00301 0.00352 0.00087 AFIX 13 H1 2 0.577517 0.044375 0.344128 11.00000 -1.20000 AFIX 0 C2 1 0.771775 0.067297 0.425400 11.00000 0.02829 0.02372 = 0.03733 0.01055 0.00050 0.00667 AFIX 23 H2A 2 0.854648 0.121546 0.429668 11.00000 -1.20000 H2B 2 0.738531 0.077083 0.495208 11.00000 -1.20000 AFIX 0 C3 1 0.810646 -0.064828 0.392286 11.00000 0.04044 0.02587 = 0.05203 0.01632 0.00946 0.01316 AFIX 23 H3A 2 0.888087 -0.085261 0.441589 11.00000 -1.20000 H3B 2 0.730162 -0.119194 0.395602 11.00000 -1.20000 AFIX 0 C4 1 0.853670 -0.087042 0.282756 11.00000 0.03557 0.02127 = 0.06056 0.01145 0.01875 0.01246 AFIX 23 H4A 2 0.872453 -0.174450 0.262896 11.00000 -1.20000 H4B 2 0.940507 -0.039835 0.281249 11.00000 -1.20000 AFIX 0 C5 1 0.741606 -0.050234 0.204477 11.00000 0.03706 0.02386 = 0.04259 -0.00132 0.01542 0.00668 AFIX 23 H5A 2 0.658021 -0.103659 0.200122 11.00000 -1.20000 H5B 2 0.775178 -0.060946 0.134754 11.00000 -1.20000 AFIX 0 C6 1 0.703411 0.082232 0.236062 11.00000 0.02842 0.02281 = 0.03163 0.00399 0.00660 0.00814 AFIX 23 H6A 2 0.627285 0.103057 0.185865 11.00000 -1.20000 H6B 2 0.784714 0.136262 0.234152 11.00000 -1.20000 AFIX 0 C7 1 0.413051 0.259309 0.330159 11.00000 0.01512 0.01974 = 0.02577 0.00314 0.00125 0.00308 AFIX 13 H7 2 0.379015 0.340181 0.361028 11.00000 -1.20000 AFIX 0 C8 1 0.321593 0.163859 0.365760 11.00000 0.01747 0.04931 = 0.05344 0.02747 0.00012 -0.00385 AFIX 23 H8A 2 0.347025 0.081218 0.334415 11.00000 -1.20000 H8B 2 0.337309 0.170441 0.442492 11.00000 -1.20000 AFIX 0 C9 1 0.168506 0.183450 0.332806 11.00000 0.01699 0.05739 = 0.06617 0.02547 0.00113 -0.00426 AFIX 23 H9A 2 0.110870 0.119225 0.353422 11.00000 -1.20000 H9B 2 0.141338 0.263136 0.369380 11.00000 -1.20000 AFIX 0 C10 1 0.141281 0.180195 0.216625 11.00000 0.01997 0.03199 = 0.06210 0.00177 -0.01044 -0.00091 AFIX 23 H10A 2 0.042656 0.197910 0.198344 11.00000 -1.20000 H10B 2 0.158670 0.097617 0.180154 11.00000 -1.20000 AFIX 0 C11 1 0.234057 0.272945 0.180340 11.00000 0.02716 0.03875 = 0.03808 0.00679 -0.01104 0.00165 AFIX 23 H11A 2 0.209705 0.356153 0.211051 11.00000 -1.20000 H11B 2 0.217725 0.265587 0.103573 11.00000 -1.20000 AFIX 0 C12 1 0.387717 0.253296 0.212389 11.00000 0.02258 0.03487 = 0.02735 0.00541 -0.00333 0.00031 AFIX 23 H12A 2 0.414562 0.172883 0.177028 11.00000 -1.20000 H12B 2 0.445520 0.316752 0.190842 11.00000 -1.20000 AFIX 0 C13 1 0.692005 0.368647 0.341219 11.00000 0.01890 0.01496 = 0.02169 0.00270 0.00069 0.00139 AFIX 13 H13 2 0.686169 0.347662 0.263594 11.00000 -1.20000 AFIX 0 C14 1 0.630440 0.494864 0.368158 11.00000 0.02181 0.01728 = 0.04120 0.00271 -0.00099 0.00483 AFIX 23 H14A 2 0.533219 0.493109 0.335686 11.00000 -1.20000 H14B 2 0.629829 0.515675 0.444595 11.00000 -1.20000 AFIX 0 C15 1 0.714538 0.591926 0.329642 11.00000 0.03443 0.01762 = 0.05591 0.01171 -0.00519 0.00157 AFIX 23 H15A 2 0.707632 0.575336 0.252590 11.00000 -1.20000 H15B 2 0.675247 0.672716 0.350746 11.00000 -1.20000 AFIX 0 C16 1 0.866598 0.594136 0.373701 11.00000 0.03150 0.01758 = 0.04710 0.00750 -0.00072 -0.00432 AFIX 23 H16A 2 0.919156 0.655486 0.345097 11.00000 -1.20000 H16B 2 0.874433 0.617872 0.450394 11.00000 -1.20000 AFIX 0 C17 1 0.928545 0.469980 0.346223 11.00000 0.02232 0.02242 = 0.03864 0.00515 0.00403 -0.00312 AFIX 23 H17A 2 1.025969 0.472327 0.378364 11.00000 -1.20000 H17B 2 0.928837 0.449893 0.269716 11.00000 -1.20000 AFIX 0 C18 1 0.846059 0.371395 0.384325 11.00000 0.01674 0.01765 = 0.03702 0.00680 0.00163 0.00071 AFIX 23 H18A 2 0.854106 0.386820 0.461423 11.00000 -1.20000 H18B 2 0.885785 0.291092 0.362007 11.00000 -1.20000 AFIX 0 PART 1 O2 3 0.662870 0.387919 0.738418 21.00000 0.02722 0.02154 = 0.02080 0.00736 0.00646 0.00836 O3 3 0.758230 0.409773 0.662950 21.00000 0.02737 0.02667 = 0.02398 0.00999 -0.00229 -0.00896 AFIX 3 0.8500 H3 2 0.702340 0.379593 0.610310 21.00000 -1.50000 AFIX 0 O4 3 0.691239 0.177478 0.706249 21.00000 0.02311 0.01851 = 0.02261 0.00120 -0.00029 -0.00179 O5 3 0.546146 0.156178 0.659918 21.00000 0.03213 0.03809 = 0.02943 0.01149 -0.00532 -0.01930 AFIX 3 0.8500 H5 2 0.563446 0.179128 0.603568 21.00000 -1.50000 AFIX 0 C19 1 0.702929 0.283902 0.782910 21.00000 0.02227 0.01893 = 0.01890 0.00387 0.00311 0.00146 C20 1 0.855299 0.288780 0.828440 21.00000 0.02583 0.02197 = 0.02104 0.00559 -0.00201 0.00007 AFIX 13 H20 2 0.916323 0.288435 0.771306 21.00000 -1.20000 AFIX 0 C21 1 0.884920 0.177371 0.882414 21.00000 0.03395 0.02424 = 0.02760 0.00702 0.00274 0.00699 AFIX 23 H21A 2 0.868628 0.101765 0.830796 21.00000 -1.20000 H21B 2 0.983224 0.180605 0.912730 21.00000 -1.20000 AFIX 0 C22 1 0.789543 0.176718 0.968526 21.00000 0.05185 0.02911 = 0.02379 0.01245 0.00671 0.01095 AFIX 13 H22 2 0.808782 0.104128 1.003327 21.00000 -1.20000 AFIX 0 C23 1 0.639013 0.170084 0.920819 21.00000 0.04490 0.04050 = 0.03245 0.01684 0.02301 0.00903 AFIX 23 H23A 2 0.576767 0.166799 0.975742 21.00000 -1.20000 H23B 2 0.621929 0.095168 0.868482 21.00000 -1.20000 AFIX 0 C24 1 0.607421 0.282701 0.868488 21.00000 0.03391 0.03757 = 0.03045 0.01455 0.01662 0.01476 AFIX 13 H24 2 0.507920 0.280023 0.838416 21.00000 -1.20000 AFIX 0 C25 1 0.884457 0.404317 0.907763 21.00000 0.05604 0.02688 = 0.03045 0.00456 -0.01496 -0.00432 AFIX 23 H25A 2 0.866523 0.476473 0.873490 21.00000 -1.20000 H25B 2 0.983136 0.408347 0.937272 21.00000 -1.20000 AFIX 0 C26 1 0.822614 0.292519 1.047693 21.00000 0.06429 0.04620 = 0.02280 0.00739 0.00308 0.01466 AFIX 23 H26A 2 0.921783 0.295038 1.075798 21.00000 -1.20000 H26B 2 0.765710 0.293323 1.106378 21.00000 -1.20000 AFIX 0 C27 1 0.639831 0.399205 0.950177 21.00000 0.06077 0.03877 = 0.03178 0.00541 0.01806 0.02257 AFIX 43 H27 2 0.574138 0.458965 0.969781 21.00000 -1.20000 AFIX 0 C28 1 0.791153 0.404472 0.994464 21.00000 0.08297 0.03025 = 0.02291 -0.00365 -0.00471 0.01249 AFIX 13 H28 2 0.810493 0.480353 1.046811 21.00000 -1.20000 AFIX 0 SAME 0.01 0.04 O2 > C28 PART 0 PART 2 O2A 3 0.784057 0.325216 0.715333 -21.00000 0.02182 0.02711 = 0.02496 0.01018 0.00341 0.00074 O3A 3 0.720162 0.425232 0.669313 -21.00000 0.02737 0.02667 = 0.02398 0.00999 -0.00229 -0.00896 AFIX 3 0.8500 H3AA 2 0.698672 0.379652 0.610932 -21.00000 -1.50000 AFIX 0 O4A 3 0.563567 0.241833 0.726339 -21.00000 0.02100 0.02886 = 0.02486 0.00511 0.00425 0.00102 O5A 3 0.585650 0.137900 0.646532 -21.00000 0.03213 0.03809 = 0.02943 0.01149 -0.00532 -0.01930 AFIX 3 0.8500 H5AA 2 0.568380 0.182620 0.600162 -21.00000 -1.50000 AFIX 0 C19A 1 0.693831 0.283541 0.781783 -21.00000 0.02227 0.01893 = 0.01890 0.00387 0.00311 0.00146 C20A 1 0.655242 0.382655 0.869163 -21.00000 0.03651 0.02736 = 0.02181 0.00080 0.00638 0.00657 AFIX 13 H20A 2 0.604710 0.448475 0.838489 -21.00000 -1.20000 AFIX 0 C21A 1 0.564718 0.327931 0.938611 -21.00000 0.06077 0.03877 = 0.03178 0.00541 0.01806 0.02257 AFIX 23 H21C 2 0.476209 0.296031 0.897897 -21.00000 -1.20000 H21D 2 0.542951 0.391480 0.996363 -21.00000 -1.20000 AFIX 0 C22A 1 0.641428 0.223556 0.983361 -21.00000 0.03948 0.03421 = 0.02643 0.00974 0.01226 0.00384 AFIX 13 H22A 2 0.580208 0.185943 1.027251 -21.00000 -1.20000 AFIX 0 C23A 1 0.680032 0.127282 0.895985 -21.00000 0.03719 0.02668 = 0.02384 0.00981 0.00836 0.00616 AFIX 23 H23C 2 0.594679 0.091696 0.852883 -21.00000 -1.20000 H23D 2 0.728949 0.061177 0.925757 -21.00000 -1.20000 AFIX 0 C24A 1 0.774261 0.183369 0.827528 -21.00000 0.02735 0.02695 = 0.02226 0.00669 0.00420 0.00755 AFIX 13 H24A 2 0.799287 0.119445 0.770057 -21.00000 -1.20000 AFIX 0 C25A 1 0.790754 0.435049 0.933171 -21.00000 0.04877 0.02952 = 0.01864 -0.00198 -0.00048 -0.00886 AFIX 23 H25C 2 0.850830 0.469035 0.887476 -21.00000 -1.20000 H25D 2 0.769581 0.501808 0.988546 -21.00000 -1.20000 AFIX 0 C26A 1 0.769329 0.280237 1.050363 -21.00000 0.04198 0.04058 = 0.01652 0.00599 0.00378 -0.00054 AFIX 23 H26C 2 0.818965 0.217567 1.084425 -21.00000 -1.20000 H26D 2 0.742053 0.344557 1.105476 -21.00000 -1.20000 AFIX 0 C27A 1 0.905710 0.238058 0.894372 -21.00000 0.02684 0.03812 = 0.02909 0.00768 0.00232 0.00554 AFIX 43 H27A 2 0.997702 0.214797 0.883257 -21.00000 -1.20000 AFIX 0 C28A 1 0.866760 0.336138 0.982092 -21.00000 0.04467 0.04032 = 0.02464 0.00536 -0.00612 -0.00671 AFIX 13 H28A 2 0.952730 0.371705 1.026187 -21.00000 -1.20000 AFIX 0 HKLF 4 REM ffe409_a.res in P-1 REM wR2 = 0.1015, GooF = S = 1.021, Restrained GooF = 0.984 for all data REM R1 = 0.0395 for 4456 Fo > 4sig(Fo) and 0.0426 for all 4842 data REM 410 parameters refined using 821 restraints END WGHT 0.0436 0.8628 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y, -z+1 HTAB C1 O5_$1 HTAB C1 O5A_$1 HTAB C2 O5A HTAB C8 O5A_$1 EQIV $2 -x+1, -y+1, -z+1 HTAB C14 O2_$2 HTAB C14 O3A_$2 HTAB O3 O1 HTAB O5 O1 HTAB O3A O1 HTAB O5A O1 REM Highest difference peak 0.381, deepest hole -0.362, 1-sigma level 0.041 Q1 1 0.6241 0.4793 0.9127 11.00000 0.05 0.36 Q2 1 0.7074 0.3972 0.9887 11.00000 0.05 0.34 Q3 1 0.5914 0.4035 1.0159 11.00000 0.05 0.33 Q4 1 0.6359 0.1764 0.3653 11.00000 0.05 0.29 Q5 1 0.4964 0.2554 0.3545 11.00000 0.05 0.26 Q6 1 0.6643 0.4331 0.3553 11.00000 0.05 0.26 Q7 1 0.6439 0.3149 0.3630 11.00000 0.05 0.26 Q8 1 0.7630 0.3636 0.3616 11.00000 0.05 0.23 Q9 1 0.8929 0.5276 0.3608 11.00000 0.05 0.22 Q10 1 0.7242 0.0165 0.2247 11.00000 0.05 0.22 Q11 1 0.9511 0.1735 0.9386 11.00000 0.05 0.22 Q12 1 0.7876 -0.0019 0.4085 11.00000 0.05 0.21 Q13 1 0.6417 0.1515 0.6556 11.00000 0.05 0.21 Q14 1 0.8915 0.4175 0.3630 11.00000 0.05 0.21 Q15 1 0.7089 0.0815 0.3854 11.00000 0.05 0.21 Q16 1 0.9766 0.2845 0.8517 11.00000 0.05 0.19 Q17 1 0.3751 0.2045 0.3464 11.00000 0.05 0.19 Q18 1 0.6856 0.0975 0.2944 11.00000 0.05 0.17 Q19 1 0.2483 0.1803 0.3545 11.00000 0.05 0.17 Q20 1 0.6714 0.5395 0.3480 11.00000 0.05 0.17 ; _shelx_res_checksum 9793 _shelx_hkl_file ; 1 0 0 0.00 0.10 -3 0 0 37.10 1.80 -3 0 0 39.60 1.80 3 0 0 42.30 1.70 3 0 0 41.20 1.70 -4 0 0 3956.80 79.49 -4 0 0 3911.91 78.89 4 0 0 3954.60 79.29 -5 0 0 456.85 11.70 -5 0 0 477.85 11.10 5 0 0 464.25 11.50 5 0 0 469.45 11.20 5 0 0 479.45 11.30 -6 0 0 183.28 5.40 -6 0 0 193.38 6.30 6 0 0 178.98 5.60 6 0 0 189.38 6.00 6 0 0 171.88 5.60 -7 0 0 467.95 11.50 -7 0 0 473.85 12.80 7 0 0 471.85 12.20 7 0 0 465.95 11.90 -8 0 0 13.90 1.70 -8 0 0 14.20 1.60 -8 0 0 12.40 1.90 8 0 0 10.90 1.60 8 0 0 14.00 1.70 -9 0 0 10.00 2.10 -9 0 0 3.40 1.20 9 0 0 3.80 1.30 9 0 0 6.00 1.30 -10 0 0 45.80 3.10 -10 0 0 50.39 2.80 -10 0 0 50.59 4.00 10 0 0 53.29 3.50 10 0 0 47.60 3.00 -11 0 0 440.86 11.90 11 0 0 458.55 13.10 -12 0 0 70.89 5.50 12 0 0 59.89 4.30 12 -1 0 40.80 4.60 -12 1 0 38.90 4.60 11 -1 0 16.20 2.80 -11 1 0 6.50 1.50 -11 1 0 11.70 2.80 10 -1 0 112.69 5.60 -10 1 0 121.59 3.70 -10 1 0 122.59 6.60 -10 1 0 117.39 4.20 9 -1 0 402.76 10.20 9 -1 0 425.96 12.30 -9 1 0 416.26 10.40 -9 1 0 402.06 9.50 -9 1 0 413.96 12.90 8 -1 0 55.99 2.60 8 -1 0 52.39 3.40 -8 1 0 55.39 3.80 -8 1 0 52.29 2.20 -8 1 0 50.49 2.60 7 -1 0 67.19 3.70 7 -1 0 69.69 2.80 -7 1 0 74.39 4.00 -7 1 0 69.19 2.50 -7 1 0 68.39 2.90 6 -1 0 26.90 2.20 6 -1 0 27.00 1.60 6 -1 0 27.40 2.00 -6 1 0 25.50 1.30 -6 1 0 26.30 2.20 5 -1 0 16.40 1.20 5 -1 0 18.00 1.60 5 -1 0 11.60 1.40 -5 1 0 17.70 1.70 -5 1 0 15.30 0.90 4 -1 0 344.97 8.70 4 -1 0 347.17 9.10 4 -1 0 347.27 7.90 -4 1 0 340.97 9.00 -4 1 0 337.37 7.50 3 -1 0 1884.41 39.40 3 -1 0 1995.50 38.30 3 -1 0 1896.11 39.10 -3 1 0 1798.02 37.80 -3 1 0 1930.31 39.30 -3 1 0 1911.01 39.40 -2 1 0 2331.27 47.30 0 1 0 0.00 0.10 0 1 0 0.00 0.10 1 1 0 -0.10 0.40 -2 -1 0 5253.07 105.99 -2 -1 0 5092.79 111.39 2 1 0 4865.31 104.99 2 1 0 5230.88 111.79 -3 -1 0 335.47 8.00 -3 -1 0 336.47 8.40 3 1 0 353.36 8.50 3 1 0 331.47 7.50 3 1 0 334.47 7.60 -4 -1 0 6.40 0.80 -4 -1 0 6.50 1.00 -4 -1 0 6.00 0.70 4 1 0 7.40 0.80 4 1 0 7.50 0.70 4 1 0 6.80 1.00 -5 -1 0 261.37 7.20 -5 -1 0 272.27 7.50 -5 -1 0 255.17 7.00 5 1 0 259.87 6.70 5 1 0 260.87 6.80 5 1 0 266.77 7.60 -6 -1 0 41.60 2.50 -6 -1 0 41.60 2.60 6 1 0 45.90 2.40 6 1 0 48.00 2.40 6 1 0 47.00 2.80 -7 -1 0 9.10 1.50 -7 -1 0 6.50 1.40 7 1 0 8.50 1.30 7 1 0 9.00 1.60 7 1 0 8.40 1.30 -8 -1 0 3.80 1.30 -8 -1 0 2.60 1.10 -8 -1 0 2.30 1.10 8 1 0 2.90 1.10 8 1 0 4.20 1.10 -9 -1 0 132.49 5.80 -9 -1 0 115.29 4.90 -9 -1 0 113.69 5.20 9 1 0 115.79 4.80 9 1 0 123.89 5.30 -10 -1 0 75.79 4.70 10 1 0 74.29 3.90 -11 -1 0 3.70 2.00 -11 -1 0 1.60 1.50 11 1 0 6.10 1.70 11 1 0 2.50 1.40 -12 -1 0 -0.60 1.60 -12 -1 0 0.30 2.00 12 1 0 2.40 1.70 12 -2 0 183.48 8.10 -12 2 0 173.28 9.30 11 -2 0 139.99 7.80 -11 2 0 142.89 7.60 10 -2 0 283.77 10.10 -10 2 0 272.37 11.40 9 -2 0 17.00 2.60 -9 2 0 14.70 2.40 -9 2 0 19.20 1.30 8 -2 0 174.78 4.70 8 -2 0 187.08 7.30 -8 2 0 190.68 4.70 -8 2 0 180.28 7.50 -8 2 0 180.68 4.70 7 -2 0 245.88 8.30 7 -2 0 238.18 5.80 -7 2 0 245.88 8.50 -7 2 0 237.78 5.90 6 -2 0 419.26 11.70 6 -2 0 409.16 9.20 -6 2 0 428.26 8.80 -6 2 0 411.86 12.30 5 -2 0 3010.30 62.19 5 -2 0 3047.30 62.89 -5 2 0 3052.39 62.79 -5 2 0 2947.01 59.59 4 -2 0 885.81 20.10 4 -2 0 878.11 17.60 4 -2 0 853.31 19.50 -4 2 0 877.11 19.90 -4 2 0 854.81 17.40 3 -2 0 78.69 3.10 3 -2 0 80.19 3.30 3 -2 0 80.29 1.90 -3 2 0 81.29 3.20 -3 2 0 75.59 1.90 2 -2 0 142.59 4.50 2 -2 0 149.79 3.20 2 -2 0 146.79 3.30 2 -2 0 139.49 4.20 -2 2 0 137.29 3.30 -2 2 0 141.89 4.30 0 2 0 4409.56 99.09 0 2 0 4891.51 100.59 -1 -2 0 76.69 2.80 1 2 0 76.99 2.10 -2 -2 0 3175.98 66.49 -2 -2 0 3267.97 65.19 -2 -2 0 3260.47 77.39 2 2 0 2964.90 67.29 2 2 0 3018.90 64.49 2 2 0 3265.07 77.49 -3 -2 0 54.89 1.70 -3 -2 0 55.69 1.80 -3 -2 0 58.29 2.80 3 2 0 52.29 2.70 3 2 0 50.69 1.70 -4 -2 0 1670.53 35.60 -4 -2 0 1651.03 34.00 4 2 0 1655.63 33.70 4 2 0 1628.74 33.40 4 2 0 1687.23 35.70 -5 -2 0 170.08 5.10 -5 -2 0 168.88 4.80 -5 -2 0 170.68 6.00 5 2 0 171.28 4.50 5 2 0 174.68 4.70 5 2 0 179.48 6.10 -6 -2 0 293.27 8.80 -6 -2 0 285.77 8.00 6 2 0 289.07 7.30 6 2 0 287.97 7.20 6 2 0 294.77 8.90 -7 -2 0 677.13 17.10 -7 -2 0 688.83 16.50 -7 -2 0 681.53 17.40 7 2 0 694.73 15.40 7 2 0 661.23 15.40 7 2 0 691.33 17.40 -8 -2 0 12.80 2.00 -8 -2 0 11.80 2.20 8 2 0 11.70 2.20 8 2 0 10.50 1.30 -9 -2 0 5.20 1.50 -9 -2 0 3.70 1.40 9 2 0 5.30 1.50 9 2 0 1.90 0.90 -10 -2 0 188.38 7.60 -10 -2 0 185.38 7.50 10 2 0 184.58 7.40 10 2 0 186.48 6.10 -11 -2 0 618.14 17.40 -11 -2 0 610.24 16.90 11 2 0 617.54 15.10 11 2 0 607.64 16.70 -12 -2 0 3.30 2.30 -12 -2 0 7.50 2.30 12 2 0 2.90 1.40 12 -3 0 -0.10 2.20 -12 3 0 1.60 2.30 11 -3 0 0.30 1.50 -11 3 0 -1.70 1.80 10 -3 0 28.80 3.40 -10 3 0 28.70 3.50 9 -3 0 166.98 7.40 -9 3 0 162.28 7.60 8 -3 0 596.24 16.60 -8 3 0 595.34 17.00 7 -3 0 15.10 2.20 -7 3 0 19.90 2.40 6 -3 0 315.97 11.00 -6 3 0 326.37 10.20 5 -3 0 74.79 3.50 5 -3 0 75.99 3.90 -5 3 0 70.99 3.80 4 -3 0 81.49 3.60 4 -3 0 77.99 3.80 -4 3 0 86.89 3.90 3 -3 0 443.06 11.10 3 -3 0 427.86 9.50 3 -3 0 454.45 11.60 3 -3 0 452.75 9.60 -3 3 0 447.06 11.40 2 -3 0 50.39 1.90 2 -3 0 50.49 2.40 2 -3 0 51.19 1.80 -2 3 0 53.39 2.50 1 -3 0 168.48 4.90 1 -3 0 173.18 4.80 1 -3 0 171.38 5.10 1 -3 0 180.08 4.80 -1 3 0 181.18 5.10 -1 3 0 174.88 4.70 0 -3 0 180.88 5.30 0 -3 0 186.48 4.90 0 -3 0 179.38 5.30 0 -3 0 188.28 4.90 0 3 0 190.18 5.30 0 3 0 183.48 4.90 -1 -3 0 188.38 5.70 -1 -3 0 190.98 4.60 -1 -3 0 181.68 4.90 1 3 0 190.78 5.70 1 3 0 183.38 4.90 -2 -3 0 650.83 13.50 2 3 0 632.64 13.80 2 3 0 660.93 15.40 -3 -3 0 1333.27 29.40 -3 -3 0 1383.76 26.70 -3 -3 0 1334.77 27.00 3 3 0 1344.17 29.40 3 3 0 1279.47 27.20 -4 -3 0 1188.18 24.20 -4 -3 0 1160.28 26.50 -4 -3 0 1178.38 23.80 4 3 0 1167.58 26.60 4 3 0 1147.09 24.10 -5 -3 0 27.80 2.40 -5 -3 0 32.00 2.20 -5 -3 0 33.70 1.80 5 3 0 34.00 2.60 5 3 0 34.00 1.60 -6 -3 0 9.60 1.90 -6 -3 0 7.40 1.10 6 3 0 8.80 0.80 6 3 0 9.10 1.80 6 3 0 7.00 0.90 -7 -3 0 279.77 8.00 -7 -3 0 284.07 10.60 7 3 0 269.47 8.20 7 3 0 278.17 6.80 7 3 0 285.47 9.50 -8 -3 0 260.77 8.10 -8 -3 0 251.27 9.20 8 3 0 249.78 7.10 8 3 0 262.07 6.60 8 3 0 261.77 9.30 -9 -3 0 70.19 3.90 -9 -3 0 62.99 4.40 9 3 0 59.89 4.20 9 3 0 67.79 2.80 -10 -3 0 8.00 1.80 -10 -3 0 6.70 2.10 10 3 0 8.10 2.10 10 3 0 8.50 1.50 -11 -3 0 118.19 6.60 -11 -3 0 130.79 6.20 11 3 0 119.29 6.30 -12 -3 0 1.70 2.40 -12 -3 0 -0.50 1.80 12 3 0 -1.90 1.70 12 -4 0 163.18 8.40 11 -4 0 64.99 5.30 -11 4 0 55.99 5.50 10 -4 0 112.69 6.40 -10 4 0 97.89 6.40 9 -4 0 119.09 6.50 -9 4 0 119.19 7.50 8 -4 0 86.79 5.20 -8 4 0 79.49 5.20 7 -4 0 9.80 1.80 -7 4 0 11.80 2.20 6 -4 0 1063.09 26.00 -6 4 0 1076.19 25.90 -5 4 0 2868.41 60.79 4 -4 0 73.59 3.90 4 -4 0 72.79 2.30 4 -4 0 71.49 3.50 4 -4 0 74.09 1.90 -4 4 0 74.69 3.80 3 -4 0 6.60 0.60 3 -4 0 7.40 0.80 3 -4 0 6.10 1.20 -3 4 0 6.70 1.10 2 -4 0 2677.03 56.29 2 -4 0 2737.43 55.29 2 -4 0 2785.12 56.89 2 -4 0 2752.92 55.59 -2 4 0 2737.53 56.59 1 -4 0 773.02 17.40 1 -4 0 766.42 17.40 1 -4 0 762.22 17.30 1 -4 0 793.32 17.80 -1 4 0 767.52 17.20 -1 4 0 799.32 17.70 0 -4 0 245.78 6.50 0 -4 0 259.57 7.20 0 -4 0 243.58 6.50 0 -4 0 248.28 7.10 0 4 0 243.58 6.50 0 4 0 238.88 7.00 -1 -4 0 762.22 16.30 -1 -4 0 760.32 17.70 -1 -4 0 724.43 16.50 -2 -4 0 1540.25 33.90 -2 -4 0 1524.85 31.70 -2 -4 0 1601.64 31.70 2 4 0 1580.64 33.90 2 4 0 1494.95 31.70 3 4 0 27.70 1.40 3 4 0 25.50 2.10 -4 -4 0 75.29 2.00 -4 -4 0 77.69 2.40 -4 -4 0 71.79 4.00 4 4 0 76.99 2.60 4 4 0 75.99 4.10 -5 -4 0 566.94 12.40 -5 -4 0 550.24 11.90 5 4 0 535.05 15.00 5 4 0 561.24 12.50 -6 -4 0 2362.66 51.09 -6 -4 0 2355.96 47.80 6 4 0 2229.68 47.50 6 4 0 2368.16 51.09 -7 -4 0 8.30 1.30 -7 -4 0 8.10 2.00 7 4 0 8.30 2.10 7 4 0 7.80 1.20 -8 -4 0 292.37 10.60 -8 -4 0 308.67 8.70 8 4 0 308.07 10.70 8 4 0 283.67 7.90 -9 -4 0 271.67 10.30 9 4 0 274.77 10.20 -10 -4 0 386.36 13.30 -10 -4 0 388.06 11.50 10 4 0 395.06 13.10 -11 -4 0 10.30 2.30 -11 -4 0 12.00 3.20 11 4 0 15.20 3.80 11 -5 0 9.40 2.80 -11 5 0 16.20 3.70 10 -5 0 34.80 4.10 -10 5 0 41.20 4.60 9 -5 0 253.77 11.50 -9 5 0 247.98 10.40 8 -5 0 80.29 5.20 -8 5 0 69.89 5.10 7 -5 0 213.98 8.90 -7 5 0 230.18 9.00 6 -5 0 39.20 3.40 -6 5 0 49.70 3.60 5 -5 0 628.44 17.00 5 -5 0 626.64 12.90 5 -5 0 627.34 13.30 -5 5 0 638.84 17.00 4 -5 0 40.30 1.90 4 -5 0 44.60 1.80 3 -5 0 535.85 12.50 3 -5 0 554.34 14.30 3 -5 0 531.55 13.60 3 -5 0 529.25 12.10 -3 5 0 531.95 14.00 2 -5 0 6.10 1.00 2 -5 0 5.60 1.00 2 -5 0 5.60 0.90 2 -5 0 3.80 1.10 -2 5 0 5.10 0.90 -2 5 0 6.20 1.10 1 -5 0 592.64 14.30 1 -5 0 604.14 14.20 1 -5 0 568.34 14.10 1 -5 0 620.04 14.60 -1 5 0 574.34 14.10 -1 5 0 583.64 14.30 0 -5 0 61.09 3.20 0 -5 0 59.79 3.10 0 -5 0 58.29 2.70 0 -5 0 60.69 2.80 0 5 0 58.39 3.00 0 5 0 61.79 2.80 -1 -5 0 106.29 3.70 -1 -5 0 109.29 4.70 -1 -5 0 110.89 3.70 -1 -5 0 111.49 4.70 1 5 0 114.39 4.70 -2 -5 0 336.27 8.30 -2 -5 0 324.97 10.00 -2 -5 0 350.76 10.20 -2 -5 0 335.27 8.10 2 5 0 338.57 10.10 2 5 0 345.67 8.30 -3 -5 0 177.78 6.90 -3 -5 0 181.48 4.60 -3 -5 0 180.78 5.00 3 5 0 188.18 7.00 3 5 0 181.28 5.00 -4 -5 0 24.40 0.90 -4 -5 0 24.80 1.20 4 5 0 24.40 1.40 -5 -5 0 116.39 5.80 -5 -5 0 116.69 3.50 5 5 0 117.89 3.80 5 5 0 120.19 5.80 -6 -5 0 272.27 7.00 -6 -5 0 266.77 9.80 6 5 0 264.97 9.70 6 5 0 269.77 7.10 -7 -5 0 13.00 1.50 -7 -5 0 12.80 2.40 7 5 0 14.80 1.40 7 5 0 11.50 2.40 -8 -5 0 74.49 5.20 -8 -5 0 85.99 3.70 8 5 0 76.79 3.40 8 5 0 75.29 5.00 -9 -5 0 61.39 3.50 -9 -5 0 71.19 5.30 9 5 0 63.89 3.60 9 5 0 55.69 4.50 -10 -5 0 8.40 1.80 10 5 0 8.30 2.80 -11 -5 0 1.20 2.30 -11 -5 0 2.30 1.60 11 5 0 2.90 2.20 11 -6 0 137.29 8.30 10 -6 0 257.17 11.20 -10 6 0 253.57 11.40 9 -6 0 5.30 1.90 -9 6 0 7.50 2.30 8 -6 0 40.00 4.40 -8 6 0 43.20 4.70 7 -6 0 302.07 11.10 -7 6 0 280.57 10.80 6 -6 0 576.54 16.90 -6 6 0 595.74 17.10 5 -6 0 151.08 6.70 5 -6 0 143.89 4.20 -5 6 0 145.79 6.60 4 -6 0 7.90 1.10 4 -6 0 6.30 0.80 4 -6 0 10.40 1.80 -4 6 0 7.00 1.50 3 -6 0 83.89 3.20 3 -6 0 78.39 3.50 -3 6 0 80.89 4.30 2 -6 0 305.17 8.80 2 -6 0 307.17 8.60 2 -6 0 317.97 9.70 2 -6 0 309.17 9.10 -2 6 0 323.07 9.50 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578.84 13.60 -2 -7 0 587.14 16.30 -2 -7 0 572.24 13.90 -2 -7 0 573.34 13.90 2 7 0 597.34 16.30 -3 -7 0 40.00 1.90 -3 -7 0 36.10 3.30 -3 -7 0 36.10 2.00 -3 -7 0 33.70 2.10 3 7 0 33.40 3.10 -4 -7 0 17.80 1.20 -4 -7 0 17.40 1.10 -4 -7 0 18.40 1.60 -4 -7 0 20.60 2.70 4 7 0 17.10 2.60 4 7 0 15.60 1.40 -5 -7 0 135.59 3.80 -5 -7 0 133.39 4.40 -5 -7 0 131.59 7.00 5 7 0 127.89 6.80 5 7 0 138.09 4.50 -6 -7 0 184.28 5.60 -6 -7 0 186.28 5.20 -6 -7 0 197.98 8.90 6 7 0 206.58 8.90 6 7 0 187.08 5.70 -7 -7 0 56.49 2.60 -7 -7 0 61.49 4.90 7 7 0 59.69 2.90 7 7 0 64.39 4.90 -8 -7 0 74.29 3.20 -8 -7 0 72.69 5.70 8 7 0 72.79 3.50 8 7 0 77.69 5.60 -9 -7 0 21.50 3.90 -9 -7 0 23.80 2.10 9 7 0 28.80 4.10 -10 -7 0 0.50 2.20 10 7 0 1.40 2.00 -10 8 0 15.90 4.40 9 -8 0 16.90 3.60 -9 8 0 11.40 3.30 8 -8 0 20.60 3.50 -8 8 0 24.50 3.80 7 -8 0 64.29 5.30 -7 8 0 53.99 4.70 6 -8 0 181.88 8.50 6 -8 0 184.28 4.60 6 -8 0 176.38 5.10 -6 8 0 178.08 8.40 5 -8 0 268.07 10.30 5 -8 0 270.07 6.90 5 -8 0 248.78 7.60 -5 8 0 268.87 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97.29 4.90 -4 12 0 88.09 6.40 3 -12 0 3.90 2.10 3 -12 0 3.40 2.00 3 -12 0 3.10 1.70 -3 12 0 4.80 2.20 2 -12 0 17.60 3.00 2 -12 0 19.50 3.40 2 -12 0 23.90 3.30 -2 12 0 22.50 3.80 1 -12 0 172.28 8.10 1 -12 0 177.08 7.90 0 -12 0 324.67 12.20 0 -12 0 326.47 11.50 0 -12 0 335.97 11.00 -1 -12 0 32.60 3.10 -1 -12 0 27.30 3.20 -1 -12 0 29.60 3.90 1 12 0 37.40 4.30 -2 -12 0 13.40 2.20 -2 -12 0 10.00 2.70 -2 -12 0 7.40 1.90 2 12 0 16.30 3.40 -3 -12 0 21.10 3.90 -3 -12 0 19.60 2.10 3 12 0 16.20 3.60 -4 -12 0 10.20 1.90 -4 -12 0 8.80 2.60 -4 -12 0 9.00 1.60 4 12 0 7.40 2.70 -6 -12 0 131.39 8.60 6 12 0 136.19 8.70 5 -13 0 154.58 6.20 5 -13 0 163.38 10.20 -5 13 0 165.08 10.20 4 -13 0 11.10 2.30 4 -13 0 20.20 4.10 4 -13 0 21.30 3.80 -4 13 0 19.70 4.00 3 -13 0 28.50 4.00 3 -13 0 35.60 4.50 -3 13 0 39.30 4.50 2 -13 0 55.99 4.70 2 -13 0 52.39 4.50 2 -13 0 49.30 4.90 -2 13 0 49.99 4.60 1 -13 0 24.20 3.90 1 -13 0 20.30 3.60 1 -13 0 26.60 3.60 0 -13 0 16.80 3.20 0 -13 0 17.70 3.20 0 -13 0 19.30 3.30 -1 -13 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47.60 3.70 -2 -13 1 48.70 3.80 -2 -13 1 52.39 5.30 1 13 -1 225.98 10.40 -1 -13 1 246.38 9.10 -1 -13 1 238.88 10.80 -1 -13 1 225.78 8.70 0 13 -1 32.30 4.10 0 -13 1 29.00 3.30 0 -13 1 20.50 3.30 0 -13 1 27.60 4.20 1 -13 1 152.48 7.50 1 -13 1 165.28 7.80 1 -13 1 145.89 7.70 2 -13 1 87.99 6.00 2 -13 1 75.69 5.40 2 -13 1 80.89 5.80 -3 13 -1 107.19 6.90 3 -13 1 103.29 5.80 3 -13 1 104.19 6.80 3 -13 1 112.89 7.00 -4 13 -1 194.58 9.70 4 -13 1 184.58 7.40 4 -13 1 173.58 9.30 4 -13 1 187.38 9.60 5 -13 1 124.89 5.50 6 12 -1 28.10 4.70 -6 -12 1 31.80 5.20 5 12 -1 66.19 6.20 -5 -12 1 67.59 6.40 4 12 -1 8.70 2.80 -4 -12 1 10.30 1.60 -4 -12 1 9.30 3.10 -4 -12 1 5.80 1.40 3 12 -1 162.08 9.00 -3 -12 1 148.39 5.70 -3 -12 1 159.58 6.00 -3 -12 1 172.88 9.30 2 12 -1 67.69 5.50 -2 -12 1 66.79 4.00 -2 -12 1 71.69 5.90 -2 -12 1 67.19 4.00 1 12 -1 0.10 1.80 -1 -12 1 3.80 2.10 -1 -12 1 1.30 1.40 -1 -12 1 2.60 1.60 0 12 -1 7.50 2.40 0 -12 1 6.60 2.00 0 -12 1 8.50 2.10 0 -12 1 7.70 2.50 -1 12 -1 97.49 5.90 1 -12 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1.60 1.40 2 -11 1 2.90 1.50 2 -11 1 2.20 1.50 2 -11 1 3.40 1.60 -3 11 -1 79.09 6.10 3 -11 1 75.49 4.40 3 -11 1 79.09 8.10 3 -11 1 64.79 5.50 -4 11 -1 298.97 11.80 4 -11 1 294.87 11.80 4 -11 1 312.47 11.90 4 -11 1 286.67 9.20 -5 11 -1 112.29 7.00 5 -11 1 96.19 6.70 5 -11 1 93.79 6.50 5 -11 1 85.09 5.10 -6 11 -1 9.00 2.60 6 -11 1 6.00 2.30 6 -11 1 4.50 1.90 6 -11 1 4.90 1.10 -7 11 -1 3.10 2.50 7 -11 1 10.60 3.30 7 -11 1 2.30 2.90 -8 11 -1 5.50 3.10 8 -11 1 -0.90 2.40 8 -11 1 4.40 2.80 8 10 -1 -0.10 4.00 -8 -10 1 0.50 4.30 7 10 -1 9.90 2.90 -7 -10 1 19.00 3.60 -7 -10 1 14.70 1.70 6 10 -1 -1.40 1.70 -6 -10 1 2.20 1.90 -6 -10 1 1.50 0.80 5 10 -1 132.99 7.80 -5 -10 1 136.99 8.00 -5 -10 1 122.29 5.10 -5 -10 1 125.19 4.20 4 10 -1 33.70 3.80 -4 -10 1 41.30 4.30 -4 -10 1 40.60 2.10 -4 -10 1 40.10 3.00 -4 -10 1 41.60 2.40 3 10 -1 0.90 1.60 -3 -10 1 1.20 0.90 -3 -10 1 4.00 1.80 -3 -10 1 3.10 1.00 2 10 -1 60.29 4.90 -2 -10 1 76.59 5.40 -2 -10 1 76.89 3.90 -2 -10 1 74.99 3.80 1 10 -1 0.00 1.10 -1 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4 4.20 2.10 7 -9 4 3.10 2.30 -8 9 -4 121.89 7.90 8 -9 4 109.99 7.40 8 -9 4 127.59 7.60 -9 9 -4 87.69 8.30 9 -9 4 90.49 10.90 9 -9 4 88.79 7.30 10 8 -4 4.60 2.80 -10 -8 4 2.40 1.60 9 8 -4 1.60 2.60 -9 -8 4 0.50 1.30 8 8 -4 33.90 4.70 -8 -8 4 45.10 3.00 7 8 -4 10.10 2.80 -7 -8 4 11.80 1.70 6 8 -4 45.20 5.20 -6 -8 4 54.39 2.90 5 8 -4 124.19 7.20 -5 -8 4 130.79 4.80 4 8 -4 62.69 5.00 -4 -8 4 64.59 3.30 3 8 -4 26.70 3.20 -3 -8 4 35.70 2.50 -3 -8 4 28.30 1.50 2 8 -4 2.10 1.20 -2 -8 4 -0.30 0.50 -2 -8 4 0.70 0.80 1 8 -4 128.39 6.30 -1 -8 4 122.59 5.30 -1 -8 4 127.39 4.70 0 8 -4 836.12 21.50 0 -8 4 840.02 20.80 0 -8 4 831.42 19.80 -1 8 -4 252.37 8.90 1 -8 4 274.17 8.60 1 -8 4 269.37 9.20 -2 8 -4 -1.70 0.80 -2 8 -4 1.30 1.00 2 -8 4 -1.30 0.70 2 -8 4 -0.40 0.90 2 -8 4 -0.70 0.70 -3 8 -4 1008.10 23.20 -3 8 -4 1013.30 25.30 3 -8 4 987.10 22.90 3 -8 4 1022.30 24.80 3 -8 4 978.50 25.10 -4 8 -4 101.69 5.80 -4 8 -4 115.49 4.40 4 -8 4 113.09 6.10 4 -8 4 107.99 3.70 4 -8 4 119.89 4.40 4 -8 4 100.69 5.60 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159.78 8.90 10 -6 4 164.48 8.30 10 -6 4 174.98 9.20 11 5 -4 1.40 2.30 -11 -5 4 2.70 1.90 10 5 -4 103.09 6.80 -10 -5 4 97.79 5.20 9 5 -4 183.38 8.80 -9 -5 4 173.98 6.80 8 5 -4 81.79 5.60 -8 -5 4 85.69 4.20 7 5 -4 2.60 1.50 -7 -5 4 3.20 1.00 6 5 -4 31.10 3.30 -6 -5 4 28.60 2.00 5 5 -4 36.70 3.30 5 5 -4 33.10 2.60 -5 -5 4 31.80 2.00 4 5 -4 93.29 4.00 4 5 -4 90.19 5.00 -4 -5 4 97.49 3.60 3 5 -4 0.40 0.90 3 5 -4 0.90 0.50 3 5 -4 0.90 0.60 -3 -5 4 1.60 0.70 2 5 -4 1104.79 25.90 2 5 -4 1117.39 23.40 2 5 -4 1066.29 24.80 -2 -5 4 1124.19 22.90 -2 -5 4 1091.79 24.20 -2 -5 4 1083.89 25.00 1 5 -4 81.39 4.20 1 5 -4 90.99 3.40 -1 -5 4 86.59 3.70 -1 -5 4 80.79 3.00 -1 -5 4 76.79 4.10 0 5 -4 10.50 1.60 0 5 -4 7.00 1.30 0 5 -4 13.10 1.40 0 -5 4 9.40 1.50 0 -5 4 11.70 1.30 0 -5 4 10.70 1.30 0 -5 4 10.00 1.50 -1 5 -4 913.51 21.50 -1 5 -4 895.51 20.40 -1 5 -4 866.21 20.80 1 -5 4 860.01 19.50 1 -5 4 890.01 20.80 1 -5 4 874.51 20.90 1 -5 4 877.01 20.10 -2 5 -4 3.00 1.00 -2 5 -4 4.90 1.00 -2 5 -4 4.10 1.20 2 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49.20 4.90 11 2 -4 -1.50 1.80 11 2 -4 1.70 1.40 -11 -2 4 -1.40 1.50 10 2 -4 0.70 1.20 10 2 -4 1.70 1.40 -10 -2 4 2.50 1.30 9 2 -4 -0.60 1.20 9 2 -4 -1.00 0.90 -9 -2 4 -0.30 1.00 8 2 -4 13.90 1.80 8 2 -4 13.30 2.40 -8 -2 4 13.10 2.00 7 2 -4 32.40 2.20 7 2 -4 32.60 2.90 -7 -2 4 35.40 2.60 6 2 -4 87.89 4.60 -6 -2 4 84.09 3.80 5 2 -4 191.38 5.70 5 2 -4 191.38 6.90 -5 -2 4 184.48 5.70 -5 -2 4 184.58 6.00 4 2 -4 274.27 8.40 -4 -2 4 272.57 7.20 -3 -2 4 3729.03 75.49 2 2 -4 82.99 3.40 2 2 -4 78.89 3.00 -2 -2 4 76.99 3.00 -2 -2 4 84.49 2.90 1 2 -4 270.67 7.00 1 2 -4 265.77 7.10 1 2 -4 260.07 6.50 -1 -2 4 260.87 6.70 -1 -2 4 273.87 6.90 0 2 -4 39.60 1.90 0 2 -4 44.10 2.10 0 2 -4 39.60 1.80 0 -2 4 39.30 2.00 0 -2 4 40.80 1.70 0 -2 4 37.40 1.80 -1 2 -4 665.63 14.90 -1 2 -4 666.73 14.20 -1 2 -4 657.03 15.10 1 -2 4 649.43 15.00 1 -2 4 650.93 14.00 1 -2 4 663.63 15.10 1 -2 4 638.84 14.70 -2 2 -4 484.25 11.60 -2 2 -4 461.05 10.20 -2 2 -4 457.45 11.50 2 -2 4 448.16 10.20 2 -2 4 469.35 11.60 2 -2 4 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12.40 2.30 0 -12 5 12.90 2.80 -1 12 -5 70.79 5.30 1 -12 5 65.09 5.00 1 -12 5 70.19 4.60 1 -12 5 69.19 5.40 -2 12 -5 87.89 5.80 2 -12 5 92.29 5.60 2 -12 5 93.19 6.10 2 -12 5 99.29 6.10 -3 12 -5 4.10 2.00 3 -12 5 2.60 1.90 3 -12 5 3.90 2.40 3 -12 5 3.20 2.00 -4 12 -5 6.30 2.00 4 -12 5 7.90 2.80 4 -12 5 5.90 2.30 4 -12 5 11.30 2.40 -5 12 -5 143.19 8.50 5 -12 5 143.99 8.60 5 -12 5 130.09 7.70 5 -12 5 141.49 7.80 -6 12 -5 132.29 8.10 6 -12 5 120.09 8.10 6 -12 5 111.19 8.50 -7 -11 5 210.48 7.20 6 11 -5 50.19 5.30 -6 -11 5 37.50 2.90 5 11 -5 29.40 4.20 -5 -11 5 24.60 2.60 4 11 -5 112.69 7.60 -4 -11 5 105.69 5.10 3 11 -5 313.67 12.80 -3 -11 5 325.47 10.20 -3 -11 5 295.47 8.10 2 11 -5 39.50 4.30 -2 -11 5 45.20 3.50 -2 -11 5 37.00 2.90 1 11 -5 9.80 2.60 -1 -11 5 10.90 2.00 -1 -11 5 9.10 2.20 0 11 -5 1.10 1.90 0 -11 5 5.10 1.40 0 -11 5 4.60 1.70 -1 11 -5 12.10 2.70 1 -11 5 8.30 2.00 -2 11 -5 38.40 3.90 2 -11 5 47.60 4.20 2 -11 5 39.00 3.70 2 -11 5 45.50 4.00 -3 11 -5 22.30 3.00 3 -11 5 29.60 3.20 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73.49 3.40 4 -10 5 75.89 4.10 -5 10 -5 46.60 4.60 -5 10 -5 47.50 2.80 5 -10 5 49.60 2.80 5 -10 5 46.10 2.20 5 -10 5 48.10 4.30 5 -10 5 45.80 4.40 -6 10 -5 48.20 4.90 6 -10 5 50.89 4.80 6 -10 5 62.29 5.30 -7 10 -5 13.40 3.50 7 -10 5 9.40 3.10 7 -10 5 11.70 3.00 -8 10 -5 7.00 3.20 8 -10 5 10.80 2.90 8 -10 5 13.40 3.90 9 9 -5 3.70 4.60 -9 -9 5 0.40 1.40 8 9 -5 5.70 2.70 -8 -9 5 6.80 1.60 7 9 -5 133.19 8.30 -7 -9 5 142.99 5.40 6 9 -5 127.89 7.90 -6 -9 5 145.49 5.40 5 9 -5 40.20 4.40 -5 -9 5 31.70 2.50 4 9 -5 511.85 17.10 -4 -9 5 522.15 13.70 3 9 -5 271.07 11.00 -3 -9 5 262.17 6.90 -3 -9 5 263.47 8.60 2 9 -5 195.38 8.80 -2 -9 5 194.58 7.30 -2 -9 5 192.58 5.90 1 9 -5 0.60 1.10 -1 -9 5 0.10 0.70 -1 -9 5 1.20 1.20 0 9 -5 752.72 20.50 0 -9 5 748.63 18.50 0 -9 5 764.32 19.80 -1 9 -5 89.59 5.00 1 -9 5 85.59 5.00 1 -9 5 77.79 4.30 -2 9 -5 350.86 12.20 2 -9 5 334.27 11.60 2 -9 5 353.96 11.10 -3 9 -5 60.09 4.40 -3 9 -5 49.50 3.40 3 -9 5 55.89 4.40 3 -9 5 54.39 3.00 3 -9 5 45.40 3.80 -4 9 -5 62.69 3.50 -4 9 -5 58.89 4.60 4 -9 5 70.59 4.90 4 -9 5 63.69 4.50 4 -9 5 67.99 3.70 -5 9 -5 37.00 2.30 -5 9 -5 38.60 3.90 5 -9 5 43.40 4.00 5 -9 5 44.60 2.50 5 -9 5 37.60 1.80 5 -9 5 40.90 4.20 -6 9 -5 11.10 2.80 6 -9 5 12.60 2.50 6 -9 5 13.50 3.10 -7 9 -5 2.00 2.00 7 -9 5 3.20 2.10 7 -9 5 1.10 1.70 -8 9 -5 4.10 2.70 8 -9 5 2.10 2.00 8 -9 5 3.60 2.60 -9 9 -5 34.70 5.00 9 -9 5 32.60 4.20 9 -9 5 31.10 5.10 10 8 -5 38.50 8.10 -10 -8 5 25.20 3.20 9 8 -5 235.88 11.60 -9 -8 5 220.58 8.00 8 8 -5 81.59 6.50 -8 -8 5 84.39 4.20 7 8 -5 123.79 7.90 -7 -8 5 128.99 5.00 -6 -8 5 62.69 3.30 5 8 -5 148.49 7.90 -5 -8 5 124.19 4.90 4 8 -5 81.49 5.70 -4 -8 5 88.09 4.10 3 8 -5 75.19 5.30 -3 -8 5 77.69 2.80 -3 -8 5 84.09 4.10 2 8 -5 1.80 1.00 2 8 -5 0.60 1.20 -2 -8 5 0.00 0.50 -2 -8 5 0.40 0.90 1 8 -5 -0.50 0.90 1 8 -5 2.30 1.10 -1 -8 5 1.00 1.00 -1 -8 5 0.90 0.70 0 8 -5 515.75 15.00 0 -8 5 508.45 13.30 0 -8 5 515.45 14.40 1 -8 5 125.99 5.90 1 -8 5 113.29 5.10 -2 8 -5 285.77 9.20 2 -8 5 274.57 9.80 2 -8 5 274.67 8.20 2 -8 5 269.07 9.10 -3 8 -5 1.30 0.90 -3 8 -5 0.90 1.10 3 -8 5 2.20 1.00 3 -8 5 0.60 1.00 3 -8 5 -0.40 0.90 -4 8 -5 355.26 12.00 -4 8 -5 340.27 9.40 4 -8 5 323.37 11.60 4 -8 5 335.07 8.30 4 -8 5 337.77 11.30 -5 8 -5 75.59 5.10 -5 8 -5 68.29 2.80 5 -8 5 67.59 2.80 5 -8 5 68.99 5.10 5 -8 5 67.99 4.60 5 -8 5 66.49 2.30 -6 8 -5 84.09 5.60 6 -8 5 87.69 5.90 6 -8 5 70.79 5.10 -7 8 -5 -1.50 1.60 7 -8 5 2.70 1.80 7 -8 5 3.20 1.70 -8 8 -5 18.10 3.80 8 -8 5 16.70 3.40 8 -8 5 20.80 3.40 -9 8 -5 5.30 2.80 9 -8 5 5.50 2.70 9 -8 5 1.40 2.20 10 7 -5 13.10 3.70 9 7 -5 175.68 9.60 -9 -7 5 171.88 6.80 8 7 -5 153.98 8.70 -8 -7 5 160.98 6.10 -7 -7 5 51.59 3.00 6 7 -5 27.90 3.70 -6 -7 5 27.40 2.20 5 7 -5 57.39 4.70 -5 -7 5 59.99 3.10 4 7 -5 4.10 1.20 -4 -7 5 3.90 1.10 3 7 -5 138.79 6.80 3 7 -5 131.69 4.40 -3 -7 5 141.49 5.30 2 7 -5 656.33 18.10 2 7 -5 641.14 15.40 -2 -7 5 643.34 14.60 -2 -7 5 646.54 16.20 1 7 -5 841.22 21.20 1 7 -5 796.82 19.90 -1 -7 5 810.82 19.80 -1 -7 5 800.92 18.40 0 7 -5 83.89 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2.50 9 -5 7 3.60 2.00 -10 5 -7 9.70 2.70 10 -5 7 3.40 2.90 10 -5 7 3.50 2.50 11 4 -7 4.60 2.80 -11 -4 7 4.50 2.20 10 4 -7 1.90 2.00 10 4 -7 1.00 1.00 -10 -4 7 -0.60 1.50 9 4 -7 26.50 2.20 -9 -4 7 23.90 2.70 8 4 -7 37.00 2.40 8 4 -7 32.70 3.80 -8 -4 7 41.70 3.10 7 4 -7 443.56 14.70 -7 -4 7 431.96 12.10 6 4 -7 671.73 15.30 6 4 -7 709.23 19.60 -6 -4 7 699.23 16.90 5 4 -7 70.99 2.80 5 4 -7 77.49 4.80 -5 -4 7 74.69 3.60 4 4 -7 173.98 7.30 4 4 -7 175.38 5.30 -4 -4 7 184.88 6.00 3 4 -7 103.59 3.80 3 4 -7 109.49 5.30 -3 -4 7 109.69 4.30 2 4 -7 1826.52 39.00 -2 -4 7 1839.22 39.90 1 4 -7 29.30 2.00 1 4 -7 23.60 2.20 -1 -4 7 28.60 2.10 0 4 -7 1.60 0.70 0 4 -7 0.70 0.70 0 -4 7 0.50 0.50 0 -4 7 1.00 0.50 0 -4 7 1.20 0.80 -1 4 -7 68.09 3.40 1 -4 7 66.69 2.80 1 -4 7 69.29 3.30 -2 4 -7 150.48 5.20 2 -4 7 130.49 5.60 2 -4 7 147.99 5.50 -3 4 -7 58.19 2.80 3 -4 7 57.49 3.60 3 -4 7 56.79 3.30 3 -4 7 53.49 2.40 -4 4 -7 688.63 15.60 4 -4 7 651.03 17.50 4 -4 7 693.43 17.30 4 -4 7 658.13 15.20 -5 4 -7 219.68 6.20 5 -4 7 220.08 6.20 5 -4 7 217.58 8.20 5 -4 7 218.48 7.90 -6 4 -7 137.49 4.30 -6 4 -7 140.69 6.50 -6 4 -7 130.79 4.50 6 -4 7 135.29 6.10 6 -4 7 131.69 4.50 6 -4 7 147.29 6.70 -7 4 -7 187.28 5.10 -7 4 -7 198.48 8.20 -7 4 -7 180.98 5.30 7 -4 7 178.38 8.30 7 -4 7 192.98 8.10 -8 4 -7 22.30 3.10 8 -4 7 32.10 3.30 8 -4 7 27.50 3.30 -9 4 -7 169.58 8.20 9 -4 7 172.88 8.30 9 -4 7 173.78 7.90 -10 4 -7 84.29 6.10 10 -4 7 93.49 6.40 10 -4 7 87.09 5.80 11 3 -7 33.60 4.40 -11 -3 7 23.50 3.60 10 3 -7 33.10 4.20 10 3 -7 26.50 2.90 -10 -3 7 25.30 3.20 9 3 -7 1.40 1.10 9 3 -7 0.00 1.50 -9 -3 7 1.90 1.30 8 3 -7 0.40 1.50 -8 -3 7 0.80 1.10 7 3 -7 305.67 11.10 -7 -3 7 292.07 9.30 6 3 -7 45.60 3.70 -6 -3 7 39.00 2.70 5 3 -7 321.17 10.70 -5 -3 7 327.27 9.10 4 3 -7 884.51 22.40 -4 -3 7 941.61 20.90 3 3 -7 4.50 1.40 3 3 -7 4.90 0.90 -3 -3 7 5.90 1.10 2 3 -7 649.43 16.40 2 3 -7 672.23 15.80 -2 -3 7 643.14 15.60 1 3 -7 214.48 7.10 1 3 -7 231.68 6.60 1 3 -7 218.08 7.10 -1 -3 7 218.78 6.40 -1 -3 7 212.68 6.70 0 3 -7 120.69 4.50 0 3 -7 113.39 4.80 0 3 -7 120.89 4.60 0 -3 7 122.59 4.10 0 -3 7 117.09 4.60 -1 3 -7 11.50 1.40 -1 3 -7 9.70 1.20 -1 3 -7 8.80 1.50 1 -3 7 9.80 1.50 1 -3 7 11.10 1.40 1 -3 7 10.30 1.10 1 -3 7 11.40 1.40 -2 3 -7 78.69 4.00 -2 3 -7 86.09 3.40 2 -3 7 93.79 4.10 2 -3 7 84.19 4.20 2 -3 7 90.69 4.50 -3 3 -7 1.10 0.60 3 -3 7 1.50 0.90 3 -3 7 1.50 0.70 3 -3 7 1.30 0.70 -4 3 -7 618.94 14.20 4 -3 7 632.04 16.00 4 -3 7 634.44 14.50 4 -3 7 595.54 16.00 -5 3 -7 113.59 3.80 5 -3 7 121.19 5.50 5 -3 7 114.79 4.20 5 -3 7 117.79 5.20 -6 3 -7 63.39 3.10 -6 3 -7 62.59 4.10 -6 3 -7 66.39 2.60 6 -3 7 62.49 3.10 6 -3 7 62.39 4.00 6 -3 7 67.69 4.20 -7 3 -7 0.30 1.00 -7 3 -7 0.60 1.20 -7 3 -7 0.30 0.60 7 -3 7 1.20 1.10 7 -3 7 1.00 1.30 -8 3 -7 3.90 1.40 -8 3 -7 3.30 1.30 -8 3 -7 4.70 1.00 8 -3 7 4.60 1.60 8 -3 7 6.30 2.00 -9 3 -7 11.40 2.50 9 -3 7 12.20 2.50 9 -3 7 13.10 2.50 -10 3 -7 49.40 4.50 10 -3 7 47.10 4.60 10 -3 7 41.00 4.10 11 2 -7 -2.10 2.00 11 2 -7 1.30 1.80 -11 -2 7 -1.00 1.80 10 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4.10 4 -5 -14 -0.80 1.80 -4 5 14 3.60 2.30 -3 5 14 1.10 2.20 -1 5 14 24.80 3.40 0 -5 -14 36.30 4.40 0 5 14 43.30 3.80 -1 -5 -14 30.50 3.50 -2 -5 -14 165.48 7.70 2 -6 -14 3.50 1.70 -2 6 14 2.50 2.60 1 -6 -14 0.00 1.50 -1 6 14 -0.70 2.10 0 -6 -14 15.50 2.80 3 8 -15 41.70 5.40 -3 -8 15 32.80 3.90 -2 -8 15 14.20 2.90 1 8 -15 2.70 2.50 -1 -8 15 0.40 1.70 0 8 -15 0.40 2.40 0 -8 15 2.00 1.90 -1 8 -15 27.40 4.70 1 -8 15 15.70 3.30 4 7 -15 19.50 4.20 -4 -7 15 15.50 2.80 -3 -7 15 0.60 1.60 2 7 -15 -3.20 2.10 1 7 -15 8.80 2.60 -1 -7 15 10.70 3.70 0 7 -15 29.20 4.50 0 -7 15 19.70 3.80 -1 7 -15 -0.10 2.10 -2 7 -15 45.00 4.90 5 6 -15 131.09 8.60 -5 -6 15 141.09 7.00 3 6 -15 58.09 5.40 -3 -6 15 57.19 4.20 2 6 -15 4.50 2.30 -2 -6 15 9.40 2.10 1 6 -15 2.50 1.90 -1 -6 15 4.90 1.80 0 6 -15 7.30 2.70 0 -6 15 5.80 2.10 -1 6 -15 15.00 3.40 1 -6 15 8.50 2.40 -2 6 -15 3.60 2.30 2 -6 15 2.30 1.60 -3 6 -15 -0.10 2.20 3 -6 15 -1.90 1.80 6 5 -15 67.79 6.70 -6 -5 15 61.59 4.80 5 5 -15 12.30 4.20 4 5 -15 0.10 2.10 -4 -5 15 0.60 1.30 3 5 -15 -0.70 1.80 -3 -5 15 4.20 1.50 2 5 -15 -0.10 1.70 -2 -5 15 0.80 1.30 1 5 -15 2.50 2.00 -1 -5 15 3.90 1.80 0 5 -15 -2.40 1.70 0 -5 15 2.30 1.70 -1 5 -15 37.60 4.40 1 -5 15 42.10 3.70 -2 5 -15 114.19 6.90 2 -5 15 122.99 6.40 -3 5 -15 -0.20 1.90 3 -5 15 -0.60 1.80 -4 5 -15 31.10 4.30 4 -5 15 29.00 3.60 6 4 -15 -1.70 2.30 -6 -4 15 -0.20 1.80 4 4 -15 4.80 2.50 -4 -4 15 5.90 1.70 3 4 -15 82.99 6.00 -3 -4 15 75.19 4.70 2 4 -15 66.89 5.50 -2 -4 15 67.89 4.40 1 4 -15 18.40 3.50 -1 -4 15 21.20 2.90 0 4 -15 22.50 3.70 0 -4 15 28.60 3.10 -1 4 -15 16.50 3.30 1 -4 15 26.60 3.00 -2 4 -15 372.66 12.90 2 -4 15 369.26 12.10 -3 4 -15 49.00 4.40 3 -4 15 31.20 3.40 -4 4 -15 9.20 2.70 4 -4 15 2.10 1.80 6 3 -15 4.40 2.70 -6 -3 15 5.70 2.40 5 3 -15 3.00 2.40 -5 -3 15 8.40 2.00 4 3 -15 0.60 1.50 -4 -3 15 3.50 1.60 3 3 -15 133.99 7.50 -3 -3 15 130.59 6.20 2 3 -15 -0.40 1.70 -2 -3 15 10.10 2.20 1 3 -15 53.09 4.70 -1 -3 15 45.20 3.60 0 3 -15 343.27 12.20 0 -3 15 344.27 11.00 -1 3 -15 270.27 10.40 1 -3 15 265.67 9.40 -2 3 -15 139.39 7.10 2 -3 15 138.29 6.40 -3 3 -15 95.39 5.80 3 -3 15 95.89 5.20 -4 3 -15 -2.40 1.80 4 -3 15 0.20 1.80 5 2 -15 16.60 3.50 -5 -2 15 16.40 2.70 4 2 -15 68.99 5.40 -4 -2 15 73.69 4.70 3 2 -15 82.99 5.80 -3 -2 15 79.79 4.80 2 2 -15 2.70 1.60 -2 -2 15 -0.20 1.30 1 2 -15 88.09 5.70 -1 -2 15 82.79 4.70 0 2 -15 2.60 1.80 0 -2 15 3.50 1.40 -1 2 -15 820.02 21.90 1 -2 15 824.72 20.60 -2 2 -15 372.06 12.40 2 -2 15 375.06 11.30 -3 2 -15 28.50 3.40 3 -2 15 22.80 2.90 -4 2 -15 2.00 1.70 4 -2 15 2.00 1.60 5 1 -15 18.90 3.30 -5 -1 15 28.90 3.20 4 1 -15 -1.30 1.50 -4 -1 15 -1.10 1.70 3 1 -15 3.10 1.80 -3 -1 15 1.70 1.40 2 1 -15 2.70 1.50 -2 -1 15 3.50 1.50 1 1 -15 20.50 2.90 -1 -1 15 28.50 2.90 0 1 -15 292.57 10.50 0 -1 15 292.07 9.40 -1 1 -15 135.49 6.60 1 -1 15 133.79 5.70 -2 1 -15 181.58 7.70 -3 1 -15 26.70 3.30 -4 1 -15 39.50 3.70 5 0 -15 25.30 4.20 -5 0 15 30.20 3.40 4 0 -15 122.29 6.90 -4 0 15 122.89 6.20 3 0 -15 70.79 5.00 -3 0 15 77.99 4.90 2 0 -15 24.70 3.30 -2 0 15 36.50 3.30 1 0 -15 2.40 1.60 -1 0 15 -1.30 1.30 0 0 -15 35.10 3.50 0 0 15 33.50 3.50 -1 0 -15 193.18 8.10 1 0 15 194.58 6.90 -2 0 -15 53.69 4.10 2 0 15 52.09 3.50 -3 0 -15 46.20 4.00 3 0 15 43.80 3.10 -4 0 -15 115.99 6.00 4 0 15 108.19 4.90 6 -1 -15 31.90 3.80 -5 1 15 122.29 6.80 4 -1 -15 7.80 2.40 -4 1 15 7.50 2.10 3 -1 -15 16.60 2.80 -3 1 15 18.20 3.00 2 -1 -15 29.00 3.40 -2 1 15 26.50 3.10 1 -1 -15 48.70 4.00 -1 1 15 48.90 3.70 0 -1 -15 33.70 3.30 0 1 15 36.30 3.40 -1 -1 -15 19.40 2.80 1 1 15 16.60 2.30 -2 -1 -15 28.80 3.30 2 1 15 27.30 2.70 -3 -1 -15 21.30 3.00 3 1 15 22.60 2.50 5 -2 -15 33.00 6.10 -5 2 15 32.10 4.10 -4 2 15 76.39 5.30 3 -2 -15 100.49 6.50 -3 2 15 103.29 5.70 2 -2 -15 24.80 3.20 -2 2 15 31.00 3.30 1 -2 -15 3.50 1.50 -1 2 15 1.60 1.60 0 -2 -15 5.30 1.70 0 2 15 5.10 1.70 -1 -2 -15 4.70 2.00 1 2 15 5.60 1.60 2 2 15 115.29 5.00 3 2 15 174.78 6.10 5 -3 -15 2.20 1.80 -5 3 15 1.70 2.30 4 -3 -15 5.50 1.80 -4 3 15 8.20 2.40 -3 3 15 5.40 2.00 -2 3 15 -1.80 1.60 0 3 15 61.29 4.10 -1 -3 -15 39.30 4.40 1 3 15 48.60 3.60 -2 -3 -15 26.90 3.50 2 3 15 24.50 2.90 3 -4 -15 -0.50 1.50 -3 4 15 2.80 2.20 2 -4 -15 93.79 5.70 -2 4 15 96.69 5.60 1 -4 -15 117.89 6.30 0 -4 -15 16.80 2.90 0 4 15 18.30 3.30 -1 -4 -15 69.49 5.00 1 4 15 57.29 4.00 3 6 -16 38.80 5.30 -3 -6 16 46.90 4.10 2 6 -16 1.70 2.40 -2 -6 16 -1.30 1.40 0 6 -16 20.70 4.00 -1 6 -16 10.20 3.00 4 5 -16 268.17 12.30 -4 -5 16 259.17 10.00 3 5 -16 43.00 4.90 -3 -5 16 53.49 4.80 1 5 -16 5.50 2.50 -1 -5 16 4.00 1.80 0 5 -16 2.90 2.30 0 -5 16 1.00 1.80 -1 5 -16 63.79 5.70 1 -5 16 53.79 4.40 -2 5 -16 232.78 9.90 2 -5 16 187.08 8.60 5 4 -16 19.80 4.50 -5 -4 16 16.20 2.80 4 4 -16 19.80 4.30 -4 -4 16 15.40 3.40 -2 -4 16 19.20 2.80 1 4 -16 43.80 4.90 -1 -4 16 52.49 4.10 0 4 -16 2.70 2.30 0 -4 16 3.10 1.80 -1 4 -16 23.40 3.70 1 -4 16 23.60 3.20 -2 4 -16 5.50 2.50 2 -4 16 2.40 1.90 5 3 -16 0.90 2.30 -5 -3 16 0.50 1.60 4 3 -16 11.60 3.20 -3 -3 16 195.78 8.00 2 3 -16 79.69 6.60 -2 -3 16 71.59 4.50 1 3 -16 19.90 3.70 -1 -3 16 12.80 2.70 0 3 -16 98.19 6.30 0 -3 16 103.89 5.50 -1 3 -16 32.70 4.00 1 -3 16 36.10 3.40 -2 3 -16 2.40 2.20 2 -3 16 4.70 1.80 5 2 -16 0.20 2.00 -5 -2 16 -3.10 1.80 4 2 -16 25.40 3.60 -4 -2 16 22.70 4.70 -3 -2 16 0.80 1.30 2 2 -16 2.10 2.70 -2 -2 16 1.90 1.70 1 2 -16 38.60 4.10 -1 -2 16 33.20 3.40 0 2 -16 1.00 1.70 0 -2 16 0.40 1.40 -1 2 -16 7.40 2.30 1 -2 16 12.10 2.50 -2 2 -16 37.70 4.10 2 -2 16 41.90 3.60 5 1 -16 1.40 2.00 -5 -1 16 -1.10 1.90 4 1 -16 96.19 6.50 -4 -1 16 109.19 5.90 -3 -1 16 87.69 5.30 -2 -1 16 18.00 2.80 1 1 -16 44.20 4.80 -1 -1 16 42.60 3.60 0 1 -16 6.50 2.10 0 -1 16 5.30 1.80 -1 1 -16 -0.70 1.40 1 -1 16 1.10 1.50 -2 1 -16 73.09 5.80 2 -1 16 63.19 4.10 4 0 -16 1.70 2.00 -4 0 16 -0.60 1.70 3 0 -16 35.70 4.70 -3 0 16 43.50 4.00 -2 0 16 16.10 3.00 -1 0 16 9.00 2.10 0 0 16 8.20 2.00 1 0 16 1.30 1.50 2 0 16 1.90 1.60 4 -1 -16 269.17 11.00 -4 1 16 272.87 10.50 3 -1 -16 29.80 3.90 -3 1 16 35.40 3.60 2 -1 -16 20.90 3.20 -2 1 16 15.70 2.90 1 -1 -16 43.40 4.00 -1 1 16 33.30 3.40 0 -1 -16 76.99 5.20 0 1 16 81.69 4.70 -1 -1 -16 75.69 5.20 1 1 16 76.29 4.40 3 -2 -16 36.70 4.20 -3 2 16 40.50 4.20 2 -2 -16 100.59 6.10 -2 2 16 104.19 6.00 1 -2 -16 12.80 2.90 -1 2 16 15.10 2.70 0 -2 -16 1.20 1.50 0 2 16 0.80 1.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 18684 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 P1 P 0.59185(4) 0.25376(3) 0.38786(3) 0.01679(11) Uani 1 1 d . . . . . O1 O 0.59414(11) 0.27996(9) 0.50476(8) 0.0235(2) Uani 1 1 d . . . . . C1 C 0.65722(15) 0.10296(13) 0.34614(12) 0.0208(3) Uani 1 1 d . . . . . H1 H 0.577517 0.044375 0.344128 0.025 Uiso 1 1 calc R . . . . C2 C 0.77178(17) 0.06730(14) 0.42540(14) 0.0293(4) Uani 1 1 d . . . . . H2A H 0.854648 0.121546 0.429668 0.035 Uiso 1 1 calc R . . . . H2B H 0.738531 0.077083 0.495208 0.035 Uiso 1 1 calc R . . . . C3 C 0.8106(2) -0.06483(16) 0.39229(15) 0.0379(4) Uani 1 1 d . . . . . H3A H 0.888087 -0.085261 0.441589 0.046 Uiso 1 1 calc R . . . . H3B H 0.730162 -0.119194 0.395602 0.046 Uiso 1 1 calc R . . . . C4 C 0.85367(19) -0.08704(15) 0.28276(16) 0.0375(4) Uani 1 1 d . . . . . H4A H 0.872453 -0.174450 0.262896 0.045 Uiso 1 1 calc R . . . . H4B H 0.940507 -0.039835 0.281249 0.045 Uiso 1 1 calc R . . . . C5 C 0.74161(18) -0.05023(15) 0.20448(14) 0.0344(4) Uani 1 1 d . . . . . H5A H 0.658021 -0.103659 0.200122 0.041 Uiso 1 1 calc R . . . . H5B H 0.775178 -0.060946 0.134754 0.041 Uiso 1 1 calc R . . . . C6 C 0.70341(17) 0.08223(14) 0.23606(13) 0.0274(4) Uani 1 1 d . . . . . H6A H 0.627285 0.103057 0.185865 0.033 Uiso 1 1 calc R . . . . H6B H 0.784714 0.136262 0.234152 0.033 Uiso 1 1 calc R . . . . C7 C 0.41305(14) 0.25931(13) 0.33016(12) 0.0203(3) Uani 1 1 d . . . . . H7 H 0.379015 0.340181 0.361028 0.024 Uiso 1 1 calc R . . . . C8 C 0.32159(16) 0.16386(18) 0.36576(16) 0.0383(4) Uani 1 1 d . . . . . H8A H 0.347025 0.081218 0.334415 0.046 Uiso 1 1 calc R . . . . H8B H 0.337309 0.170441 0.442492 0.046 Uiso 1 1 calc R . . . . C9 C 0.16851(17) 0.1834(2) 0.33281(17) 0.0454(5) Uani 1 1 d . . . . . H9A H 0.110870 0.119225 0.353422 0.055 Uiso 1 1 calc R . . . . H9B H 0.141338 0.263136 0.369380 0.055 Uiso 1 1 calc R . . . . C10 C 0.14128(17) 0.18020(16) 0.21663(16) 0.0398(5) Uani 1 1 d . . . . . H10A H 0.042656 0.197910 0.198344 0.048 Uiso 1 1 calc R . . . . H10B H 0.158670 0.097617 0.180154 0.048 Uiso 1 1 calc R . . . . C11 C 0.23406(17) 0.27295(17) 0.18034(15) 0.0357(4) Uani 1 1 d . . . . . H11A H 0.209705 0.356153 0.211051 0.043 Uiso 1 1 calc R . . . . H11B H 0.217725 0.265587 0.103573 0.043 Uiso 1 1 calc R . . . . C12 C 0.38772(16) 0.25330(16) 0.21239(13) 0.0287(4) Uani 1 1 d . . . . . H12A H 0.414562 0.172883 0.177028 0.034 Uiso 1 1 calc R . . . . H12B H 0.445520 0.316752 0.190842 0.034 Uiso 1 1 calc R . . . . C13 C 0.69200(14) 0.36865(12) 0.34122(11) 0.0187(3) Uani 1 1 d . . . . . H13 H 0.686169 0.347662 0.263594 0.022 Uiso 1 1 calc R . . . . C14 C 0.63044(16) 0.49486(13) 0.36816(14) 0.0273(4) Uani 1 1 d . . . . . H14A H 0.533219 0.493109 0.335686 0.033 Uiso 1 1 calc R . . . . H14B H 0.629829 0.515675 0.444595 0.033 Uiso 1 1 calc R . . . . C15 C 0.71454(18) 0.59193(14) 0.32964(16) 0.0361(4) Uani 1 1 d . . . . . H15A H 0.707632 0.575336 0.252590 0.043 Uiso 1 1 calc R . . . . H15B H 0.675247 0.672716 0.350746 0.043 Uiso 1 1 calc R . . . . C16 C 0.86660(17) 0.59414(14) 0.37370(15) 0.0322(4) Uani 1 1 d . . . . . H16A H 0.919156 0.655486 0.345097 0.039 Uiso 1 1 calc R . . . . H16B H 0.874433 0.617872 0.450394 0.039 Uiso 1 1 calc R . . . . C17 C 0.92855(16) 0.46998(14) 0.34622(14) 0.0278(4) Uani 1 1 d . . . . . H17A H 1.025969 0.472327 0.378364 0.033 Uiso 1 1 calc R . . . . H17B H 0.928837 0.449893 0.269716 0.033 Uiso 1 1 calc R . . . . C18 C 0.84606(15) 0.37140(13) 0.38433(13) 0.0236(3) Uani 1 1 d . . . . . H18A H 0.854106 0.386820 0.461423 0.028 Uiso 1 1 calc R . . . . H18B H 0.885785 0.291092 0.362007 0.028 Uiso 1 1 calc R . . . . O2 O 0.66287(18) 0.38792(15) 0.73842(13) 0.0224(4) Uani 0.5989(14) 1 d D U P A 1 O3 O 0.7582(4) 0.4098(5) 0.6630(5) 0.0258(8) Uani 0.5989(14) 1 d D U P A 1 H3 H 0.702340 0.379593 0.610310 0.039 Uiso 0.5989(14) 1 d R . P A 1 O4 O 0.69124(17) 0.17748(15) 0.70625(13) 0.0219(4) Uani 0.5989(14) 1 d D U P A 1 O5 O 0.5461(3) 0.1562(5) 0.6599(4) 0.0333(8) Uani 0.5989(14) 1 d D U P A 1 H5 H 0.563446 0.179128 0.603568 0.050 Uiso 0.5989(14) 1 d R . P A 1 C19 C 0.7029(4) 0.2839(3) 0.7829(2) 0.0199(3) Uani 0.5989(14) 1 d D U P A 1 C20 C 0.8553(3) 0.2888(2) 0.82844(19) 0.0230(5) Uani 0.5989(14) 1 d D U P A 1 H20 H 0.916323 0.288435 0.771306 0.028 Uiso 0.5989(14) 1 calc R . P A 1 C21 C 0.8849(4) 0.1774(3) 0.8824(3) 0.0283(7) Uani 0.5989(14) 1 d D U P A 1 H21A H 0.868628 0.101765 0.830796 0.034 Uiso 0.5989(14) 1 calc R . P A 1 H21B H 0.983224 0.180605 0.912730 0.034 Uiso 0.5989(14) 1 calc R . P A 1 C22 C 0.7895(3) 0.1767(3) 0.9685(2) 0.0337(6) Uani 0.5989(14) 1 d D U P A 1 H22 H 0.808782 0.104128 1.003327 0.040 Uiso 0.5989(14) 1 calc R . P A 1 C23 C 0.6390(4) 0.1701(4) 0.9208(3) 0.0367(8) Uani 0.5989(14) 1 d D U P A 1 H23A H 0.576767 0.166799 0.975742 0.044 Uiso 0.5989(14) 1 calc R . P A 1 H23B H 0.621929 0.095168 0.868482 0.044 Uiso 0.5989(14) 1 calc R . P A 1 C24 C 0.6074(3) 0.2827(3) 0.8685(2) 0.0319(6) Uani 0.5989(14) 1 d D U P A 1 H24 H 0.507920 0.280023 0.838416 0.038 Uiso 0.5989(14) 1 calc R . P A 1 C25 C 0.8845(4) 0.4043(3) 0.9078(2) 0.0393(7) Uani 0.5989(14) 1 d D U P A 1 H25A H 0.866523 0.476473 0.873490 0.047 Uiso 0.5989(14) 1 calc R . P A 1 H25B H 0.983136 0.408347 0.937272 0.047 Uiso 0.5989(14) 1 calc R . P A 1 C26 C 0.8226(5) 0.2925(5) 1.0477(4) 0.0442(12) Uani 0.5989(14) 1 d D U P A 1 H26A H 0.921783 0.295038 1.075798 0.053 Uiso 0.5989(14) 1 calc R . P A 1 H26B H 0.765710 0.293323 1.106378 0.053 Uiso 0.5989(14) 1 calc R . P A 1 C27 C 0.6398(4) 0.3992(3) 0.9502(2) 0.0427(6) Uani 0.5989(14) 1 d D U P A 1 H27 H 0.574138 0.458965 0.969781 0.051 Uiso 0.5989(14) 1 calc R . P A 1 C28 C 0.7912(4) 0.4045(3) 0.9945(3) 0.0469(8) Uani 0.5989(14) 1 d D U P A 1 H28 H 0.810493 0.480353 1.046811 0.056 Uiso 0.5989(14) 1 calc R . P A 1 O2A O 0.7841(3) 0.3252(2) 0.7153(2) 0.0239(6) Uani 0.4011(14) 1 d D U P A 2 O3A O 0.7202(8) 0.4252(8) 0.6693(7) 0.0258(8) Uani 0.4011(14) 1 d D U P A 2 H3AA H 0.698672 0.379652 0.610932 0.039 Uiso 0.4011(14) 1 d R . P A 2 O4A O 0.5636(3) 0.2418(2) 0.7263(2) 0.0247(6) Uani 0.4011(14) 1 d D U P A 2 O5A O 0.5857(6) 0.1379(7) 0.6465(6) 0.0333(8) Uani 0.4011(14) 1 d D U P A 2 H5AA H 0.568380 0.182620 0.600162 0.050 Uiso 0.4011(14) 1 d R . P A 2 C19A C 0.6938(5) 0.2835(5) 0.7818(3) 0.0199(3) Uani 0.4011(14) 1 d D U P A 2 C20A C 0.6552(4) 0.3827(4) 0.8692(3) 0.0286(8) Uani 0.4011(14) 1 d D U P A 2 H20A H 0.604710 0.448475 0.838489 0.034 Uiso 0.4011(14) 1 calc R . P A 2 C21A C 0.5647(6) 0.3279(4) 0.9386(4) 0.0427(6) Uani 0.4011(14) 1 d D U P A 2 H21C H 0.476209 0.296031 0.897897 0.051 Uiso 0.4011(14) 1 calc R . P A 2 H21D H 0.542951 0.391480 0.996363 0.051 Uiso 0.4011(14) 1 calc R . P A 2 C22A C 0.6414(5) 0.2236(4) 0.9834(4) 0.0322(9) Uani 0.4011(14) 1 d D U P A 2 H22A H 0.580208 0.185943 1.027251 0.039 Uiso 0.4011(14) 1 calc R . P A 2 C23A C 0.6800(5) 0.1273(4) 0.8960(4) 0.0282(10) Uani 0.4011(14) 1 d D U P A 2 H23C H 0.594679 0.091696 0.852883 0.034 Uiso 0.4011(14) 1 calc R . P A 2 H23D H 0.728949 0.061177 0.925757 0.034 Uiso 0.4011(14) 1 calc R . P A 2 C24A C 0.7743(4) 0.1834(3) 0.8275(3) 0.0251(8) Uani 0.4011(14) 1 d D U P A 2 H24A H 0.799287 0.119445 0.770057 0.030 Uiso 0.4011(14) 1 calc R . P A 2 C25A C 0.7908(5) 0.4350(4) 0.9332(4) 0.0334(9) Uani 0.4011(14) 1 d D U P A 2 H25C H 0.850830 0.469035 0.887476 0.040 Uiso 0.4011(14) 1 calc R . P A 2 H25D H 0.769581 0.501808 0.988546 0.040 Uiso 0.4011(14) 1 calc R . P A 2 C26A C 0.7693(6) 0.2802(7) 1.0504(5) 0.0329(14) Uani 0.4011(14) 1 d D U P A 2 H26C H 0.818965 0.217567 1.084425 0.039 Uiso 0.4011(14) 1 calc R . P A 2 H26D H 0.742053 0.344557 1.105476 0.039 Uiso 0.4011(14) 1 calc R . P A 2 C27A C 0.9057(5) 0.2381(5) 0.8944(4) 0.0311(10) Uani 0.4011(14) 1 d D U P A 2 H27A H 0.997702 0.214797 0.883257 0.037 Uiso 0.4011(14) 1 calc R . P A 2 C28A C 0.8668(5) 0.3361(4) 0.9821(3) 0.0373(10) Uani 0.4011(14) 1 d D U P A 2 H28A H 0.952730 0.371705 1.026187 0.045 Uiso 0.4011(14) 1 calc R . P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.01453(19) 0.01592(19) 0.0195(2) 0.00245(14) 0.00071(14) 0.00171(13) O1 0.0260(6) 0.0235(5) 0.0207(5) 0.0035(4) 0.0005(4) 0.0006(4) C1 0.0180(7) 0.0149(7) 0.0294(8) 0.0030(6) 0.0035(6) 0.0009(5) C2 0.0283(8) 0.0237(8) 0.0373(9) 0.0106(7) 0.0005(7) 0.0067(6) C3 0.0404(10) 0.0259(9) 0.0520(11) 0.0163(8) 0.0095(9) 0.0132(7) C4 0.0356(9) 0.0213(8) 0.0606(12) 0.0115(8) 0.0187(9) 0.0125(7) C5 0.0371(9) 0.0239(8) 0.0426(10) -0.0013(7) 0.0154(8) 0.0067(7) C6 0.0284(8) 0.0228(8) 0.0316(9) 0.0040(7) 0.0066(7) 0.0081(6) C7 0.0151(7) 0.0197(7) 0.0258(8) 0.0031(6) 0.0013(6) 0.0031(6) C8 0.0175(8) 0.0493(11) 0.0534(12) 0.0275(9) 0.0001(7) -0.0038(7) C9 0.0170(8) 0.0574(12) 0.0662(14) 0.0255(11) 0.0011(8) -0.0043(8) C10 0.0200(8) 0.0320(9) 0.0621(13) 0.0018(9) -0.0104(8) -0.0009(7) C11 0.0272(9) 0.0388(10) 0.0381(10) 0.0068(8) -0.0110(7) 0.0017(7) C12 0.0226(8) 0.0349(9) 0.0274(8) 0.0054(7) -0.0033(6) 0.0003(7) C13 0.0189(7) 0.0150(7) 0.0217(7) 0.0027(6) 0.0007(6) 0.0014(5) C14 0.0218(8) 0.0173(7) 0.0412(9) 0.0027(7) -0.0010(7) 0.0048(6) C15 0.0344(9) 0.0176(8) 0.0559(12) 0.0117(8) -0.0052(8) 0.0016(7) C16 0.0315(9) 0.0176(8) 0.0471(10) 0.0075(7) -0.0007(8) -0.0043(6) C17 0.0223(8) 0.0224(8) 0.0386(9) 0.0052(7) 0.0040(7) -0.0031(6) C18 0.0167(7) 0.0177(7) 0.0370(9) 0.0068(6) 0.0016(6) 0.0007(6) O2 0.0272(9) 0.0215(9) 0.0208(9) 0.0074(7) 0.0065(7) 0.0084(7) O3 0.027(3) 0.0267(15) 0.0240(9) 0.0100(11) -0.0023(16) -0.0090(14) O4 0.0231(9) 0.0185(8) 0.0226(9) 0.0012(7) -0.0003(7) -0.0018(7) O5 0.032(2) 0.0381(17) 0.0294(14) 0.0115(9) -0.0053(15) -0.0193(16) C19 0.0223(8) 0.0189(7) 0.0189(7) 0.0039(6) 0.0031(6) 0.0015(6) C20 0.0258(12) 0.0220(12) 0.0210(12) 0.0056(10) -0.0020(10) 0.0001(10) C21 0.0339(17) 0.0242(16) 0.0276(15) 0.0070(15) 0.0027(12) 0.0070(14) C22 0.0519(16) 0.0291(13) 0.0238(13) 0.0125(11) 0.0067(12) 0.0110(12) C23 0.0449(19) 0.041(2) 0.0325(19) 0.0168(17) 0.0230(15) 0.0090(15) C24 0.0339(14) 0.0376(15) 0.0304(14) 0.0145(12) 0.0166(11) 0.0148(12) C25 0.0560(19) 0.0269(14) 0.0304(15) 0.0046(12) -0.0150(14) -0.0043(14) C26 0.064(3) 0.046(2) 0.0228(17) 0.0074(15) 0.003(2) 0.015(2) C27 0.0608(17) 0.0388(15) 0.0318(13) 0.0054(12) 0.0181(13) 0.0226(11) C28 0.083(2) 0.0303(16) 0.0229(16) -0.0037(13) -0.0047(16) 0.0125(16) O2A 0.0218(13) 0.0271(13) 0.0250(13) 0.0102(11) 0.0034(10) 0.0007(10) O3A 0.027(3) 0.0267(15) 0.0240(9) 0.0100(11) -0.0023(16) -0.0090(14) O4A 0.0210(13) 0.0289(14) 0.0249(13) 0.0051(11) 0.0043(11) 0.0010(11) O5A 0.032(2) 0.0381(17) 0.0294(14) 0.0115(9) -0.0053(15) -0.0193(16) C19A 0.0223(8) 0.0189(7) 0.0189(7) 0.0039(6) 0.0031(6) 0.0015(6) C20A 0.0365(19) 0.0274(18) 0.0218(18) 0.0008(15) 0.0064(16) 0.0066(16) C21A 0.0608(17) 0.0388(15) 0.0318(13) 0.0054(12) 0.0181(13) 0.0226(11) C22A 0.039(2) 0.034(2) 0.026(2) 0.0097(18) 0.0123(18) 0.0038(17) C23A 0.037(2) 0.027(2) 0.024(2) 0.0098(18) 0.0084(19) 0.0062(18) C24A 0.0274(18) 0.0269(17) 0.0223(17) 0.0067(14) 0.0042(15) 0.0075(14) C25A 0.049(2) 0.030(2) 0.019(2) -0.0020(18) -0.0005(19) -0.0089(19) C26A 0.042(3) 0.041(3) 0.017(2) 0.0060(18) 0.004(2) -0.001(2) C27A 0.027(2) 0.038(3) 0.029(2) 0.008(2) 0.0023(17) 0.006(2) C28A 0.045(2) 0.040(2) 0.025(2) 0.0054(18) -0.0061(18) -0.0067(19) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 O1 P1 C1 110.72(6) . . ? O1 P1 C7 108.44(6) . . ? O1 P1 C13 111.08(6) . . ? C7 P1 C1 108.85(7) . . ? C13 P1 C1 110.29(7) . . ? C13 P1 C7 107.35(7) . . ? P1 C1 H1 106.0 . . ? C2 C1 P1 112.44(11) . . ? C2 C1 H1 106.0 . . ? C6 C1 P1 114.90(10) . . ? C6 C1 H1 106.0 . . ? C6 C1 C2 110.70(12) . . ? C1 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C3 C2 C1 109.96(14) . . ? C3 C2 H2A 109.7 . . ? C3 C2 H2B 109.7 . . ? C2 C3 H3A 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C4 C3 C2 111.97(14) . . ? C4 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? C3 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? C3 C4 C5 111.49(14) . . ? H4A C4 H4B 108.0 . . ? C5 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 C6 110.91(14) . . ? H5A C5 H5B 108.0 . . ? C6 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? C5 C6 C1 110.64(13) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? P1 C7 H7 105.7 . . ? C8 C7 P1 110.42(10) . . ? C8 C7 H7 105.7 . . ? C12 C7 P1 117.68(10) . . ? C12 C7 H7 105.7 . . ? C12 C7 C8 110.62(13) . . ? C7 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.2 . . ? C9 C8 C7 110.10(14) . . ? C9 C8 H8A 109.6 . . ? C9 C8 H8B 109.6 . . ? C8 C9 H9A 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C10 C9 C8 111.37(16) . . ? C10 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? C9 C10 H10A 109.4 . . ? C9 C10 H10B 109.4 . . ? C9 C10 C11 111.20(14) . . ? H10A C10 H10B 108.0 . . ? C11 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C10 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C10 C11 C12 111.19(14) . . ? H11A C11 H11B 108.0 . . ? C12 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? C7 C12 C11 109.88(13) . . ? C7 C12 H12A 109.7 . . ? C7 C12 H12B 109.7 . . ? C11 C12 H12A 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? P1 C13 H13 107.9 . . ? C14 C13 P1 110.77(10) . . ? C14 C13 H13 107.9 . . ? C14 C13 C18 110.40(12) . . ? C18 C13 P1 111.96(10) . . ? C18 C13 H13 107.9 . . ? C13 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C15 C14 C13 111.03(13) . . ? C15 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C14 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C16 C15 C14 111.37(14) . . ? C16 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C17 C16 C15 110.68(13) . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? C16 C17 H17A 109.4 . . ? C16 C17 H17B 109.4 . . ? C16 C17 C18 111.24(13) . . ? H17A C17 H17B 108.0 . . ? C18 C17 H17A 109.4 . . ? C18 C17 H17B 109.4 . . ? C13 C18 H18A 109.3 . . ? C13 C18 H18B 109.3 . . ? C17 C18 C13 111.44(12) . . ? C17 C18 H18A 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? C19 O2 O3 110.0(2) . . ? O2 O3 H3 94.0 . . ? C19 O4 O5 110.1(2) . . ? O4 O5 H5 92.5 . . ? O2 C19 C20 113.6(2) . . ? O2 C19 C24 103.8(3) . . ? O4 C19 O2 111.0(2) . . ? O4 C19 C20 103.9(3) . . ? O4 C19 C24 114.2(2) . . ? C24 C19 C20 110.6(2) . . ? C19 C20 H20 109.6 . . ? C19 C20 C21 109.5(2) . . ? C21 C20 H20 109.6 . . ? C25 C20 C19 109.4(2) . . ? C25 C20 H20 109.6 . . ? C25 C20 C21 109.3(2) . . ? C20 C21 H21A 109.8 . . ? C20 C21 H21B 109.8 . . ? H21A C21 H21B 108.2 . . ? C22 C21 C20 109.5(2) . . ? C22 C21 H21A 109.8 . . ? C22 C21 H21B 109.8 . . ? C21 C22 H22 109.4 . . ? C23 C22 C21 109.3(3) . . ? C23 C22 H22 109.4 . . ? C23 C22 C26 111.9(3) . . ? C26 C22 C21 107.6(3) . . ? C26 C22 H22 109.4 . . ? C22 C23 H23A 109.7 . . ? C22 C23 H23B 109.7 . . ? C22 C23 C24 109.8(3) . . ? H23A C23 H23B 108.2 . . ? C24 C23 H23A 109.7 . . ? C24 C23 H23B 109.7 . . ? C19 C24 C23 108.5(2) . . ? C19 C24 H24 110.3 . . ? C19 C24 C27 108.2(2) . . ? C23 C24 H24 110.3 . . ? C23 C24 C27 109.1(3) . . ? C27 C24 H24 110.3 . . ? C20 C25 H25A 109.8 . . ? C20 C25 H25B 109.8 . . ? C20 C25 C28 109.4(3) . . ? H25A C25 H25B 108.3 . . ? C28 C25 H25A 109.8 . . ? C28 C25 H25B 109.8 . . ? C22 C26 H26A 109.8 . . ? C22 C26 H26B 109.8 . . ? C22 C26 C28 109.4(3) . . ? H26A C26 H26B 108.2 . . ? C28 C26 H26A 109.8 . . ? C28 C26 H26B 109.8 . . ? C24 C27 H27 124.8 . . ? C28 C27 C24 110.4(2) . . ? C28 C27 H27 124.8 . . ? C25 C28 C26 108.8(3) . . ? C25 C28 H28 109.4 . . ? C26 C28 H28 109.4 . . ? C27 C28 C25 110.2(3) . . ? C27 C28 C26 109.6(3) . . ? C27 C28 H28 109.4 . . ? C19A O2A O3A 109.5(4) . . ? O2A O3A H3AA 92.2 . . ? C19A O4A O5A 108.9(4) . . ? O4A O5A H5AA 89.2 . . ? O2A C19A O4A 111.4(3) . . ? O2A C19A C20A 114.0(3) . . ? O2A C19A C24A 104.2(4) . . ? O4A C19A C20A 103.7(4) . . ? O4A C19A C24A 113.2(3) . . ? C24A C19A C20A 110.5(3) . . ? C19A C20A H20A 109.9 . . ? C19A C20A C25A 107.6(3) . . ? C21A C20A C19A 110.0(3) . . ? C21A C20A H20A 109.9 . . ? C21A C20A C25A 109.6(4) . . ? C25A C20A H20A 109.9 . . ? C20A C21A H21C 109.7 . . ? C20A C21A H21D 109.7 . . ? C20A C21A C22A 109.8(4) . . ? H21C C21A H21D 108.2 . . ? C22A C21A H21C 109.7 . . ? C22A C21A H21D 109.7 . . ? C21A C22A H22A 109.5 . . ? C23A C22A C21A 110.5(4) . . ? C23A C22A H22A 109.5 . . ? C26A C22A C21A 106.7(5) . . ? C26A C22A H22A 109.5 . . ? C26A C22A C23A 111.0(5) . . ? C22A C23A H23C 109.6 . . ? C22A C23A H23D 109.6 . . ? C22A C23A C24A 110.3(4) . . ? H23C C23A H23D 108.1 . . ? C24A C23A H23C 109.6 . . ? C24A C23A H23D 109.6 . . ? C19A C24A C23A 107.8(3) . . ? C19A C24A H24A 109.9 . . ? C23A C24A H24A 109.9 . . ? C27A C24A C19A 109.8(3) . . ? C27A C24A C23A 109.4(3) . . ? C27A C24A H24A 109.9 . . ? C20A C25A H25C 109.6 . . ? C20A C25A H25D 109.6 . . ? H25C C25A H25D 108.1 . . ? C28A C25A C20A 110.2(3) . . ? C28A C25A H25C 109.6 . . ? C28A C25A H25D 109.6 . . ? C22A C26A H26C 109.7 . . ? C22A C26A H26D 109.7 . . ? C22A C26A C28A 109.8(4) . . ? H26C C26A H26D 108.2 . . ? C28A C26A H26C 109.7 . . ? C28A C26A H26D 109.7 . . ? C24A C27A H27A 125.2 . . ? C24A C27A C28A 109.7(4) . . ? C28A C27A H27A 125.2 . . ? C25A C28A C26A 109.1(5) . . ? C25A C28A C27A 108.3(4) . . ? C25A C28A H28A 109.8 . . ? C26A C28A H28A 109.8 . . ? C27A C28A C26A 110.1(4) . . ? C27A C28A H28A 109.8 . . ? 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 P1 O1 1.5077(11) . ? P1 C1 1.8219(14) . ? P1 C7 1.8207(14) . ? P1 C13 1.8156(14) . ? C1 H1 1.0000 . ? C1 C2 1.538(2) . ? C1 C6 1.536(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.528(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.517(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.519(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.527(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7 1.0000 . ? C7 C8 1.535(2) . ? C7 C12 1.525(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.528(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.510(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.525(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.531(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13 1.0000 . ? C13 C14 1.5358(19) . ? C13 C18 1.5366(19) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 C15 1.525(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.522(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.518(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.527(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? O2 O3 1.467(3) . ? O2 C19 1.418(3) . ? O3 H3 0.8500 . ? O4 O5 1.471(3) . ? O4 C19 1.418(3) . ? O5 H5 0.8501 . ? C19 C20 1.529(4) . ? C19 C24 1.527(4) . ? C20 H20 1.0000 . ? C20 C21 1.539(4) . ? C20 C25 1.520(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.531(4) . ? C22 H22 1.0000 . ? C22 C23 1.520(4) . ? C22 C26 1.525(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.542(4) . ? C24 H24 1.0000 . ? C24 C27 1.547(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C28 1.523(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 C28 1.542(5) . ? C27 H27 0.9500 . ? C27 C28 1.515(5) . ? C28 H28 1.0000 . ? O2A O3A 1.463(4) . ? O2A C19A 1.420(3) . ? O3A H3AA 0.8502 . ? O4A O5A 1.462(4) . ? O4A C19A 1.421(3) . ? O5A H5AA 0.8499 . ? C19A C20A 1.535(6) . ? C19A C24A 1.532(6) . ? C20A H20A 1.0000 . ? C20A C21A 1.516(6) . ? C20A C25A 1.535(5) . ? C21A H21C 0.9900 . ? C21A H21D 0.9900 . ? C21A C22A 1.547(5) . ? C22A H22A 1.0000 . ? C22A C23A 1.516(5) . ? C22A C26A 1.508(6) . ? C23A H23C 0.9900 . ? C23A H23D 0.9900 . ? C23A C24A 1.538(5) . ? C24A H24A 1.0000 . ? C24A C27A 1.527(6) . ? C25A H25C 0.9900 . ? C25A H25D 0.9900 . ? C25A C28A 1.521(6) . ? C26A H26C 0.9900 . ? C26A H26D 0.9900 . ? C26A C28A 1.555(6) . ? C27A H27A 0.9500 . ? C27A C28A 1.532(6) . ? C28A H28A 1.0000 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O3 H3 O1 0.85 1.85 2.680(7) 166.6 . yes O5 H5 O1 0.85 1.89 2.706(7) 161.3 . yes O3A H3AA O1 0.85 1.83 2.648(12) 159.7 . yes O5A H5AA O1 0.85 1.81 2.632(11) 160.9 . yes 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 P1 C1 C2 C3 173.62(11) . . . . ? P1 C1 C6 C5 -174.00(11) . . . . ? P1 C7 C8 C9 170.21(14) . . . . ? P1 C7 C12 C11 -173.94(11) . . . . ? P1 C13 C14 C15 179.72(11) . . . . ? P1 C13 C18 C17 -178.90(11) . . . . ? O1 P1 C1 C2 -33.46(13) . . . . ? O1 P1 C1 C6 -161.28(10) . . . . ? O1 P1 C7 C8 -60.15(13) . . . . ? O1 P1 C7 C12 171.55(11) . . . . ? O1 P1 C13 C14 -61.51(12) . . . . ? O1 P1 C13 C18 62.19(12) . . . . ? C1 P1 C7 C8 60.38(13) . . . . ? C1 P1 C7 C12 -67.93(13) . . . . ? C1 P1 C13 C14 175.34(10) . . . . ? C1 P1 C13 C18 -60.96(12) . . . . ? C1 C2 C3 C4 55.67(19) . . . . ? C2 C1 C6 C5 57.31(17) . . . . ? C2 C3 C4 C5 -55.6(2) . . . . ? C3 C4 C5 C6 55.58(19) . . . . ? C4 C5 C6 C1 -56.54(18) . . . . ? C6 C1 C2 C3 -56.37(17) . . . . ? C7 P1 C1 C2 -152.57(11) . . . . ? C7 P1 C1 C6 79.61(12) . . . . ? C7 P1 C13 C14 56.89(12) . . . . ? C7 P1 C13 C18 -179.42(10) . . . . ? C7 C8 C9 C10 56.5(2) . . . . ? C8 C7 C12 C11 57.86(17) . . . . ? C8 C9 C10 C11 -55.8(2) . . . . ? C9 C10 C11 C12 55.9(2) . . . . ? C10 C11 C12 C7 -56.78(19) . . . . ? C12 C7 C8 C9 -57.7(2) . . . . ? C13 P1 C1 C2 89.90(12) . . . . ? C13 P1 C1 C6 -37.92(13) . . . . ? C13 P1 C7 C8 179.76(12) . . . . ? C13 P1 C7 C12 51.46(13) . . . . ? C13 C14 C15 C16 -56.51(19) . . . . ? C14 C13 C18 C17 -55.00(17) . . . . ? C14 C15 C16 C17 56.8(2) . . . . ? C15 C16 C17 C18 -56.39(19) . . . . ? C16 C17 C18 C13 55.99(18) . . . . ? C18 C13 C14 C15 55.13(17) . . . . ? O2 C19 C20 C21 175.4(2) . . . . ? O2 C19 C20 C25 55.7(3) . . . . ? O2 C19 C24 C23 178.4(2) . . . . ? O2 C19 C24 C27 -63.3(3) . . . . ? O3 O2 C19 O4 -64.0(4) . . . . ? O3 O2 C19 C20 52.7(4) . . . . ? O3 O2 C19 C24 172.9(4) . . . . ? O4 C19 C20 C21 -63.9(3) . . . . ? O4 C19 C20 C25 176.4(2) . . . . ? O4 C19 C24 C23 57.4(4) . . . . ? O4 C19 C24 C27 175.7(2) . . . . ? O5 O4 C19 O2 -61.3(4) . . . . ? O5 O4 C19 C20 176.2(3) . . . . ? O5 O4 C19 C24 55.6(4) . . . . ? C19 C20 C21 C22 -58.8(3) . . . . ? C19 C20 C25 C28 59.8(3) . . . . ? C19 C24 C27 C28 -58.3(3) . . . . ? C20 C19 C24 C23 -59.4(3) . . . . ? C20 C19 C24 C27 58.9(3) . . . . ? C20 C21 C22 C23 60.1(3) . . . . ? C20 C21 C22 C26 -61.5(3) . . . . ? C20 C25 C28 C26 60.3(4) . . . . ? C20 C25 C28 C27 -59.8(3) . . . . ? C21 C20 C25 C28 -60.0(3) . . . . ? C21 C22 C23 C24 -61.3(4) . . . . ? C21 C22 C26 C28 62.1(4) . . . . ? C22 C23 C24 C19 60.4(4) . . . . ? C22 C23 C24 C27 -57.2(4) . . . . ? C22 C26 C28 C25 -62.0(4) . . . . ? C22 C26 C28 C27 58.6(4) . . . . ? C23 C22 C26 C28 -57.9(4) . . . . ? C23 C24 C27 C28 59.6(3) . . . . ? C24 C19 C20 C21 59.1(3) . . . . ? C24 C19 C20 C25 -60.6(3) . . . . ? C24 C27 C28 C25 59.4(3) . . . . ? C24 C27 C28 C26 -60.3(4) . . . . ? C25 C20 C21 C22 61.0(3) . . . . ? C26 C22 C23 C24 57.7(4) . . . . ? O2A C19A C20A C21A -177.3(3) . . . . ? O2A C19A C20A C25A -57.9(5) . . . . ? O2A C19A C24A C23A -176.6(3) . . . . ? O2A C19A C24A C27A 64.3(4) . . . . ? O3A O2A C19A O4A 59.6(7) . . . . ? O3A O2A C19A C20A -57.4(6) . . . . ? O3A O2A C19A C24A -178.0(6) . . . . ? O4A C19A C20A C21A 61.4(4) . . . . ? O4A C19A C20A C25A -179.2(3) . . . . ? O4A C19A C24A C23A -55.4(5) . . . . ? O4A C19A C24A C27A -174.5(3) . . . . ? O5A O4A C19A O2A 62.5(6) . . . . ? O5A O4A C19A C20A -174.4(5) . . . . ? O5A O4A C19A C24A -54.6(6) . . . . ? C19A C20A C21A C22A 57.3(5) . . . . ? C19A C20A C25A C28A -61.6(5) . . . . ? C19A C24A C27A C28A 58.8(5) . . . . ? C20A C19A C24A C23A 60.4(4) . . . . ? C20A C19A C24A C27A -58.7(4) . . . . ? C20A C21A C22A C23A -57.4(5) . . . . ? C20A C21A C22A C26A 63.3(5) . . . . ? C20A C25A C28A C26A -57.2(5) . . . . ? C20A C25A C28A C27A 62.6(5) . . . . ? C21A C20A C25A C28A 57.9(5) . . . . ? C21A C22A C23A C24A 59.3(5) . . . . ? C21A C22A C26A C28A -62.9(6) . . . . ? C22A C23A C24A C19A -60.1(4) . . . . ? C22A C23A C24A C27A 59.3(5) . . . . ? C22A C26A C28A C25A 61.2(6) . . . . ? C22A C26A C28A C27A -57.5(6) . . . . ? C23A C22A C26A C28A 57.6(6) . . . . ? C23A C24A C27A C28A -59.4(5) . . . . ? C24A C19A C20A C21A -60.2(4) . . . . ? C24A C19A C20A C25A 59.1(4) . . . . ? C24A C27A C28A C25A -60.5(5) . . . . ? C24A C27A C28A C26A 58.7(5) . . . . ? C25A C20A C21A C22A -60.9(5) . . . . ? C26A C22A C23A C24A -59.0(5) . . . . ?