#------------------------------------------------------------------------------ #$Date: 2020-09-22 13:29:47 +0300 (Tue, 22 Sep 2020) $ #$Revision: 256620 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132575.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_4132575 loop_ _publ_author_name 'Liu, Liu Leo' 'Zhou, Jiliang' 'Andrews, Ryan' 'Stephan, Douglas W.' _publ_section_title ; A Room-Temperature-Stable Phosphanorcaradiene. ; _journal_issue 24 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 7466 _journal_page_last 7470 _journal_paper_doi 10.1021/jacs.8b04930 _journal_volume 140 _journal_year 2018 _chemical_formula_moiety 'C43 H45 N2 O4 P' _chemical_formula_sum 'C43 H45 N2 O4 P' _chemical_formula_weight 684.78 _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 geom _audit_creation_date 2018-03-16 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _cell_angle_alpha 99.452(4) _cell_angle_beta 103.114(3) _cell_angle_gamma 95.605(4) _cell_formula_units_Z 2 _cell_length_a 9.8219(11) _cell_length_b 13.2831(16) _cell_length_c 14.8369(18) _cell_measurement_reflns_used 5829 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 24.49 _cell_measurement_theta_min 2.32 _cell_volume 1841.2(4) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_unetI/netI 0.0661 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 39808 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.448 _diffrn_reflns_theta_min 2.747 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.120 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.7179 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0576 before and 0.0514 after correction. The Ratio of minimum to maximum transmission is 0.9631. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.235 _exptl_crystal_description block _exptl_crystal_F_000 728 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.244 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.052 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 462 _refine_ls_number_reflns 7529 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.006 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0463 _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^)+(0.0424P)^2^+0.6481P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0927 _refine_ls_wR_factor_ref 0.1091 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4940 _reflns_number_total 7529 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04930_si_002.cif _cod_data_source_block 5 _cod_depositor_comments ; 2020-09-22 Z value and formula fixed to values more according to usual chemical conventions. miguel ; _cod_original_formula_weight 342.39 _cod_original_formula_moiety '0.5(C43 H45 N2 O4 P)' _cod_original_formula_units_Z 4 _cod_original_formula_sum 'C21.50 H22.50 N O2 P0.50' _cod_database_code 4132575 _shelx_shelxl_version_number 2014/7 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C34(H34), C32(H32), C23(H23), C19(H19), C25(H25), C10(H10), C11(H11), C12(H12), C16(H16), C13(H13), C18(H18), C17(H17) 2.b Idealised Me refined as rotating group: C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C5(H5A,H5B,H5C), C36(H36A,H36B,H36C), C43(H43A,H43B,H43C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C) ; _shelx_res_file ; finalleo_a.res created by SHELXL-2014/7 TITL finalleo_a.res in P-1 REM Old TITL finalleo in P-1 REM SHELXT solution in P-1 REM R1 0.189, Rweak 0.012, Alpha 0.043, Orientation as input REM Formula found by SHELXT: C42 N2 O4 P CELL 0.71073 9.8219 13.2831 14.8369 99.452 103.114 95.605 ZERR 4 0.0011 0.0016 0.0018 0.004 0.003 0.004 LATT 1 SFAC C H N O P UNIT 86 90 4 8 2 L.S. 10 PLAN 20 TEMP 23 BOND $H LIST 6 fmap 2 acta OMIT 0 1 0 OMIT 1 0 0 OMIT 0 -1 1 OMIT -1 0 1 OMIT 0 1 1 OMIT 0 0 1 OMIT -1 1 0 OMIT -5 -1 4 REM REM REM WGHT 0.042400 0.648100 FVAR 0.60400 P1 5 0.265288 0.699766 0.365762 11.00000 0.01758 0.01987 = 0.01890 0.00468 0.00340 0.00502 O1 4 0.368644 0.757181 0.472903 11.00000 0.02374 0.02794 = 0.01779 0.00304 0.00083 0.00766 O2 4 0.379978 0.615745 0.346855 11.00000 0.02190 0.02374 = 0.02360 0.00440 0.00385 0.01039 O4 4 -0.156498 0.887276 0.263375 11.00000 0.02250 0.03394 = 0.02776 0.00996 0.01022 0.01216 O3 4 -0.060924 0.760601 -0.008165 11.00000 0.03914 0.05381 = 0.01750 -0.00257 -0.00426 0.02209 N1 3 0.046758 0.818769 0.267125 11.00000 0.01722 0.01900 = 0.01410 0.00417 0.00348 0.00417 N2 3 0.116129 0.772612 0.123635 11.00000 0.02170 0.02465 = 0.01397 0.00063 0.00257 0.00998 C33 1 0.085757 0.849422 0.561250 11.00000 0.03131 0.02375 = 0.02010 0.00328 0.01114 0.01055 C30 1 0.063260 0.829596 0.369133 11.00000 0.01679 0.02037 = 0.01524 0.00421 0.00479 0.00748 C31 1 0.144748 0.916843 0.430366 11.00000 0.01979 0.01778 = 0.02132 0.00276 0.00569 0.00577 C34 1 -0.005219 0.769735 0.497286 11.00000 0.02660 0.02218 = 0.02808 0.01075 0.01572 0.00849 AFIX 43 H34 2 -0.058909 0.722646 0.519793 11.00000 -1.20000 AFIX 0 C1 1 0.157514 0.790575 0.224133 11.00000 0.02116 0.01559 = 0.01453 0.00255 0.00664 0.00320 C35 1 -0.018915 0.757825 0.401357 11.00000 0.01650 0.01878 = 0.02471 0.00476 0.00634 0.00448 C39 1 -0.066509 0.862561 0.223225 11.00000 0.01790 0.01962 = 0.02099 0.00214 0.00318 0.00308 C32 1 0.156075 0.923250 0.526292 11.00000 0.02696 0.02017 = 0.02187 -0.00125 0.00479 0.00370 AFIX 43 H32 2 0.213061 0.979276 0.568422 11.00000 -1.20000 AFIX 0 C6 1 0.423412 0.894386 0.199057 11.00000 0.02718 0.03073 = 0.03021 0.00911 0.01265 0.00350 AFIX 137 H6A 2 0.361800 0.870512 0.137310 11.00000 -1.50000 H6B 2 0.516025 0.918304 0.193475 11.00000 -1.50000 H6C 2 0.387351 0.949860 0.232229 11.00000 -1.50000 AFIX 0 C2 1 0.287035 0.776433 0.276126 11.00000 0.01540 0.01542 = 0.01573 -0.00037 0.00179 0.00317 C4 1 0.539606 0.849792 0.348248 11.00000 0.01960 0.02878 = 0.02545 0.00209 0.00634 -0.00162 AFIX 137 H4A 2 0.625672 0.879287 0.336615 11.00000 -1.50000 H4B 2 0.558363 0.795438 0.382736 11.00000 -1.50000 H4C 2 0.502126 0.902022 0.384386 11.00000 -1.50000 AFIX 0 C7 1 0.479537 0.701728 0.496806 11.00000 0.01854 0.03022 = 0.02304 0.01391 0.00131 0.00169 C40 1 -0.066608 0.885211 0.126582 11.00000 0.02378 0.02894 = 0.01924 0.00761 0.00520 0.01146 C3 1 0.431484 0.805849 0.253533 11.00000 0.01744 0.02239 = 0.02023 0.00364 0.00634 0.00336 C8 1 0.486395 0.625387 0.427464 11.00000 0.01749 0.02790 = 0.02489 0.01414 0.00274 0.00233 C21 1 0.174574 0.694346 0.067963 11.00000 0.02312 0.03265 = 0.01737 -0.00304 -0.00121 0.01190 C41 1 -0.008056 0.800565 0.073517 11.00000 0.02460 0.03187 = 0.02041 0.00772 0.00323 0.00971 C37 1 0.109866 0.852504 0.665782 11.00000 0.06030 0.03457 = 0.02330 0.00663 0.01475 0.01071 AFIX 137 H37A 2 0.023329 0.827091 0.679408 11.00000 -1.50000 H37B 2 0.141003 0.922215 0.699167 11.00000 -1.50000 H37C 2 0.180616 0.810170 0.685320 11.00000 -1.50000 AFIX 0 C38 1 -0.114402 0.668063 0.335148 11.00000 0.02418 0.02674 = 0.03138 0.00680 0.00603 -0.00148 AFIX 137 H38A 2 -0.178590 0.692569 0.287230 11.00000 -1.50000 H38B 2 -0.166895 0.630920 0.369521 11.00000 -1.50000 H38C 2 -0.058899 0.623188 0.306273 11.00000 -1.50000 AFIX 0 C42 1 -0.216016 0.893502 0.073350 11.00000 0.02987 0.04918 = 0.02515 0.01105 0.00451 0.02096 AFIX 137 H42A 2 -0.275617 0.829396 0.065743 11.00000 -1.50000 H42B 2 -0.214578 0.908652 0.012467 11.00000 -1.50000 H42C 2 -0.251946 0.947679 0.108314 11.00000 -1.50000 AFIX 0 C5 1 0.493876 0.718935 0.201616 11.00000 0.02071 0.03108 = 0.02670 0.00250 0.00882 0.00577 AFIX 137 H5A 2 0.435151 0.695287 0.138930 11.00000 -1.50000 H5B 2 0.498232 0.662838 0.235075 11.00000 -1.50000 H5C 2 0.587218 0.744391 0.198412 11.00000 -1.50000 AFIX 0 C36 1 0.218155 1.002576 0.396701 11.00000 0.03075 0.02122 = 0.02443 0.00271 0.00781 -0.00020 AFIX 137 H36A 2 0.278963 0.975041 0.359473 11.00000 -1.50000 H36B 2 0.273273 1.052443 0.450046 11.00000 -1.50000 H36C 2 0.149146 1.035041 0.359067 11.00000 -1.50000 AFIX 0 C9 1 0.593719 0.561193 0.435425 11.00000 0.01783 0.02802 = 0.04823 0.02527 0.01102 0.00393 C26 1 0.163256 0.593058 0.082721 11.00000 0.02475 0.03151 = 0.02078 -0.00617 -0.00804 0.00798 C24 1 0.287071 0.547982 -0.040064 11.00000 0.03453 0.06471 = 0.02826 -0.01996 -0.00510 0.02556 C22 1 0.230566 0.721296 -0.005068 11.00000 0.03163 0.05380 = 0.01668 0.00076 0.00416 0.01836 C43 1 0.031622 0.987737 0.140701 11.00000 0.03845 0.03054 = 0.02446 0.01193 0.01464 0.01373 AFIX 137 H43A 2 -0.002856 1.041773 0.176892 11.00000 -1.50000 H43B 2 0.033417 1.004338 0.080363 11.00000 -1.50000 H43C 2 0.125336 0.980802 0.173619 11.00000 -1.50000 AFIX 0 C20 1 0.574867 0.721643 0.587256 11.00000 0.02836 0.03621 = 0.02884 0.01891 -0.00312 -0.00950 C23 1 0.287049 0.646947 -0.056788 11.00000 0.03727 0.07520 = 0.02203 -0.00574 0.00488 0.02400 AFIX 43 H23 2 0.326328 0.664550 -0.104484 11.00000 -1.20000 AFIX 0 C19 1 0.560671 0.796955 0.661775 11.00000 0.05008 0.04049 = 0.02525 0.01316 -0.00353 -0.01480 AFIX 43 H19 2 0.491335 0.839593 0.651309 11.00000 -1.20000 AFIX 0 C25 1 0.222929 0.522317 0.028485 11.00000 0.03714 0.03642 = 0.03626 -0.01521 -0.01344 0.01570 AFIX 43 H25 2 0.219388 0.455062 0.038904 11.00000 -1.20000 AFIX 0 C29 1 0.084659 0.555571 0.149071 11.00000 0.04097 0.02546 = 0.03466 -0.00096 -0.00728 0.00126 AFIX 137 H29A 2 0.149915 0.555498 0.208011 11.00000 -1.50000 H29B 2 0.037293 0.486861 0.122233 11.00000 -1.50000 H29C 2 0.016395 0.600328 0.159491 11.00000 -1.50000 AFIX 0 C14 1 0.694608 0.578507 0.523312 11.00000 0.01703 0.04172 = 0.06079 0.03869 0.00330 0.00065 C10 1 0.601034 0.483761 0.360460 11.00000 0.02827 0.02699 = 0.06852 0.02366 0.02283 0.00822 AFIX 43 H10 2 0.533185 0.472770 0.303481 11.00000 -1.20000 AFIX 0 C27 1 0.225694 0.824198 -0.035381 11.00000 0.05693 0.06951 = 0.02701 0.01724 0.01793 0.02295 AFIX 137 H27A 2 0.151531 0.817524 -0.091600 11.00000 -1.50000 H27B 2 0.314445 0.846637 -0.047704 11.00000 -1.50000 H27C 2 0.208006 0.873888 0.013881 11.00000 -1.50000 AFIX 0 C11 1 0.708090 0.424404 0.371234 11.00000 0.03670 0.03219 = 0.10955 0.03483 0.04023 0.01490 AFIX 43 H11 2 0.713590 0.373526 0.321536 11.00000 -1.20000 AFIX 0 C15 1 0.682352 0.657119 0.600617 11.00000 0.02071 0.04999 = 0.04555 0.03645 -0.00850 -0.01205 C12 1 0.808538 0.440780 0.457064 11.00000 0.02677 0.04851 = 0.13147 0.05856 0.02992 0.01933 AFIX 43 H12 2 0.880714 0.400130 0.464304 11.00000 -1.20000 AFIX 0 C16 1 0.771329 0.672290 0.692745 11.00000 0.03430 0.06840 = 0.06503 0.04788 -0.01868 -0.01663 AFIX 43 H16 2 0.843368 0.632081 0.704557 11.00000 -1.20000 AFIX 0 C13 1 0.802991 0.515049 0.530388 11.00000 0.01834 0.05802 = 0.09294 0.05888 0.00636 0.00352 AFIX 43 H13 2 0.872059 0.524499 0.586658 11.00000 -1.20000 AFIX 0 C18 1 0.649037 0.807661 0.750008 11.00000 0.07367 0.05494 = 0.03128 0.01747 -0.01281 -0.02738 AFIX 43 H18 2 0.638770 0.856766 0.799548 11.00000 -1.20000 AFIX 0 C17 1 0.753962 0.744739 0.764953 11.00000 0.06370 0.07648 = 0.04312 0.03542 -0.02727 -0.03227 AFIX 43 H17 2 0.813257 0.751936 0.824871 11.00000 -1.20000 AFIX 0 C28 1 0.348687 0.468380 -0.098646 11.00000 0.05433 0.09514 = 0.05107 -0.04011 -0.00589 0.04054 AFIX 137 H28A 2 0.306762 0.464807 -0.164374 11.00000 -1.50000 H28B 2 0.329364 0.402224 -0.082596 11.00000 -1.50000 H28C 2 0.448926 0.487739 -0.086036 11.00000 -1.50000 AFIX 0 HKLF 4 REM finalleo_a.res in P-1 REM R1 = 0.0463 for 4940 Fo > 4sig(Fo) and 0.0917 for all 7529 data REM 462 parameters refined using 0 restraints END WGHT 0.0424 0.6482 REM Highest difference peak 0.244, deepest hole -0.363, 1-sigma level 0.052 Q1 1 0.2192 0.9809 0.3099 11.00000 0.05 0.24 Q2 1 -0.1165 0.6747 0.2695 11.00000 0.05 0.23 Q3 1 0.8646 0.5489 0.6366 11.00000 0.05 0.23 Q4 1 0.3440 1.0004 0.4166 11.00000 0.05 0.22 Q5 1 -0.0661 0.8805 0.1715 11.00000 0.05 0.22 Q6 1 0.2990 0.7582 0.3276 11.00000 0.05 0.21 Q7 1 0.5761 0.8713 0.8166 11.00000 0.05 0.21 Q8 1 0.0504 0.7839 0.3896 11.00000 0.05 0.21 Q9 1 -0.0561 0.7177 0.3720 11.00000 0.05 0.21 Q10 1 0.4814 0.8171 0.2989 11.00000 0.05 0.21 Q11 1 0.6811 0.5986 0.5753 11.00000 0.05 0.21 Q12 1 0.3948 0.4217 -0.0573 11.00000 0.05 0.20 Q13 1 0.6160 0.5594 0.4878 11.00000 0.05 0.20 Q14 1 0.6055 0.6736 0.6036 11.00000 0.05 0.19 Q15 1 0.4710 0.6400 0.4755 11.00000 0.05 0.19 Q16 1 -0.0951 0.6298 0.2673 11.00000 0.05 0.19 Q17 1 0.1917 1.0773 0.4120 11.00000 0.05 0.19 Q18 1 -0.1198 0.8844 0.1034 11.00000 0.05 0.19 Q19 1 -0.2016 0.6740 0.3305 11.00000 0.05 0.18 Q20 1 0.6609 0.6013 0.4656 11.00000 0.05 0.18 ; _shelx_res_checksum 56066 _shelx_hkl_file ; -1 0 0 -0.30 1.20 -1 0 0 -0.20 1.20 -1 0 0 -2.80 1.20 -1 0 0 -0.70 0.80 -1 0 0 -1.20 1.90 1 0 0 0.70 1.30 1 0 0 -0.60 0.90 1 0 0 0.70 1.50 1 0 0 -1.20 1.50 1 0 0 -0.80 1.00 1 0 0 -0.70 1.10 -2 0 0 227.78 9.10 -2 0 0 227.08 8.60 -2 0 0 239.38 9.00 -2 0 0 252.17 10.80 -2 0 0 244.18 9.10 2 0 0 226.48 12.20 2 0 0 227.58 9.30 2 0 0 229.08 9.70 2 0 0 247.18 9.20 2 0 0 233.28 9.00 2 0 0 238.98 7.80 2 0 0 226.78 9.30 -3 0 0 126.39 7.40 -3 0 0 130.99 7.50 -3 0 0 129.99 9.40 -3 0 0 124.09 7.20 -3 0 0 132.89 7.80 3 0 0 143.49 10.70 3 0 0 119.09 8.20 3 0 0 141.09 8.70 3 0 0 141.09 8.10 3 0 0 114.59 8.30 3 0 0 133.29 6.40 3 0 0 126.99 7.40 -4 0 0 134.99 8.70 -4 0 0 119.09 11.50 -4 0 0 148.29 8.40 -4 0 0 135.79 9.00 -4 0 0 129.59 9.00 4 0 0 141.89 12.00 4 0 0 140.09 9.80 4 0 0 125.49 8.70 4 0 0 145.39 8.50 4 0 0 146.39 9.10 4 0 0 144.29 7.10 4 0 0 153.28 9.50 -5 0 0 20.00 5.30 -5 0 0 9.60 7.40 -5 0 0 17.70 5.40 -5 0 0 22.40 5.70 -5 0 0 13.10 5.40 5 0 0 26.10 5.70 5 0 0 23.70 9.60 5 0 0 18.60 6.00 5 0 0 15.30 6.20 5 0 0 25.70 6.00 5 0 0 13.80 4.00 5 0 0 16.70 5.70 -6 0 0 38.70 6.80 -6 0 0 36.10 6.40 6 0 0 25.70 7.50 6 0 0 45.60 7.60 6 0 0 37.00 6.70 6 0 0 24.20 10.50 6 0 0 33.00 7.10 6 0 0 30.80 7.50 6 0 0 38.70 4.90 -7 0 0 13.20 6.30 -7 0 0 17.40 6.60 7 0 0 20.30 6.20 7 0 0 22.20 8.00 7 0 0 24.60 7.30 7 0 0 22.70 9.10 7 0 0 7.40 4.50 7 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290.87 17.40 -5 5 0 296.37 16.90 -5 5 0 302.07 20.00 -5 5 0 267.27 16.90 -5 5 0 303.47 17.00 4 -5 0 4.80 6.60 4 -5 0 -4.20 10.20 4 -5 0 17.00 7.80 4 -5 0 11.90 7.70 4 -5 0 -1.00 8.70 4 -5 0 6.30 8.10 -4 5 0 8.30 6.70 -4 5 0 8.00 9.20 -4 5 0 5.40 7.10 -4 5 0 4.10 7.50 -4 5 0 -3.30 6.70 3 -5 0 1715.93 48.50 3 -5 0 1649.33 48.30 3 -5 0 1674.13 47.90 3 -5 0 1657.53 48.10 3 -5 0 1709.83 52.59 3 -5 0 1661.93 49.30 -3 5 0 1687.63 48.30 -3 5 0 1729.13 51.49 -3 5 0 1720.53 48.50 -3 5 0 1719.13 49.00 -3 5 0 1735.13 50.19 2 -5 0 216.68 12.80 2 -5 0 220.48 13.00 2 -5 0 213.68 16.90 2 -5 0 230.78 13.20 2 -5 0 209.48 12.10 2 -5 0 216.58 14.40 -2 5 0 229.08 11.70 -2 5 0 200.18 15.70 -2 5 0 195.08 15.00 -2 5 0 215.38 12.50 -2 5 0 201.78 13.00 -2 5 0 210.08 11.70 1 -5 0 -2.30 5.00 1 -5 0 7.10 5.60 1 -5 0 -2.00 3.60 1 -5 0 2.50 5.50 1 -5 0 0.20 6.30 -1 5 0 4.80 5.60 -1 5 0 6.90 5.60 -1 5 0 0.80 7.40 -1 5 0 7.20 5.20 -1 5 0 6.90 5.90 -1 5 0 12.20 7.50 0 -5 0 1.70 4.50 0 -5 0 5.40 4.50 0 -5 0 -0.90 5.50 0 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5.70 5 5 0 66.19 6.80 5 5 0 73.39 8.40 5 5 0 66.39 6.80 6 5 0 -0.60 10.10 6 5 0 -0.40 5.00 6 5 0 11.90 6.20 6 5 0 2.20 3.80 6 5 0 -4.10 5.00 6 5 0 -4.20 3.90 7 5 0 0.40 4.50 7 5 0 0.60 5.50 7 5 0 6.30 7.20 7 5 0 -0.90 11.10 7 5 0 1.70 5.80 8 5 0 49.40 8.20 8 5 0 61.49 8.80 8 5 0 67.09 14.60 8 5 0 61.79 7.00 9 5 0 38.80 8.90 9 5 0 39.80 16.70 9 5 0 34.20 6.50 10 5 0 9.10 8.20 10 5 0 2.40 16.20 11 -6 0 0.90 11.40 11 -6 0 -17.80 13.40 11 -6 0 18.10 14.10 10 -6 0 20.70 13.40 10 -6 0 7.40 18.00 10 -6 0 26.20 11.90 -10 6 0 5.20 11.50 9 -6 0 44.30 12.30 9 -6 0 3.20 17.10 9 -6 0 29.40 13.30 -9 6 0 50.39 12.40 8 -6 0 17.60 9.40 8 -6 0 21.00 16.50 8 -6 0 18.90 10.30 -8 6 0 31.10 11.00 -8 6 0 11.40 12.90 7 -6 0 267.77 23.00 7 -6 0 265.97 19.60 7 -6 0 251.87 19.30 7 -6 0 264.47 20.30 -7 6 0 316.97 20.20 -7 6 0 248.08 21.80 -7 6 0 237.28 18.90 6 -6 0 296.47 17.60 6 -6 0 261.77 17.90 6 -6 0 290.67 19.50 6 -6 0 258.57 23.20 -6 6 0 288.07 18.70 -6 6 0 294.27 19.60 -6 6 0 298.47 18.70 5 -6 0 116.59 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4.90 0 -6 0 3.80 6.10 0 -6 0 3.70 5.10 0 -6 0 -1.20 5.90 0 6 0 1.90 7.10 0 6 0 -3.80 5.00 0 6 0 -1.20 5.10 0 6 0 -0.10 5.50 0 6 0 -4.60 7.60 0 6 0 2.00 5.20 -1 -6 0 10.40 4.90 -1 -6 0 14.30 4.70 -1 -6 0 7.20 6.10 -1 -6 0 12.00 8.10 -1 -6 0 19.50 5.00 -1 -6 0 8.30 4.50 1 6 0 9.00 6.90 1 6 0 8.90 4.80 1 6 0 10.20 5.20 1 6 0 16.20 8.20 1 6 0 15.20 5.40 1 6 0 18.10 5.20 -2 -6 0 17.40 4.80 -2 -6 0 21.70 4.20 -2 -6 0 19.70 4.40 -2 -6 0 16.70 4.20 -2 -6 0 15.10 8.80 -2 -6 0 24.90 6.00 2 6 0 25.40 6.80 2 6 0 21.00 5.20 2 6 0 18.60 4.50 2 6 0 18.60 5.10 2 6 0 22.40 5.00 -3 -6 0 269.17 10.10 -3 -6 0 293.27 10.70 -3 -6 0 279.57 9.70 3 6 0 260.17 11.60 3 6 0 285.57 11.10 3 6 0 278.67 11.10 3 6 0 283.37 12.10 3 6 0 272.77 13.80 -4 -6 0 30.10 4.10 -4 -6 0 24.00 3.90 4 6 0 31.50 4.70 4 6 0 31.70 4.40 4 6 0 26.80 5.20 4 6 0 26.80 6.80 4 6 0 38.10 5.90 -5 -6 0 157.68 7.50 -5 -6 0 153.78 7.50 5 6 0 162.98 8.20 5 6 0 152.88 12.10 5 6 0 168.48 16.80 5 6 0 167.18 8.30 5 6 0 148.69 9.70 5 6 0 157.58 9.70 -6 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18.40 7.50 9 7 0 49.10 17.50 11 -8 0 -24.50 21.20 11 -8 0 -2.30 13.80 11 -8 0 9.80 15.30 10 -8 0 41.50 15.10 10 -8 0 3.40 20.30 10 -8 0 25.90 13.20 -10 8 0 14.00 13.10 9 -8 0 2.00 12.50 9 -8 0 -1.30 17.60 9 -8 0 20.10 10.10 -9 8 0 35.80 13.40 -9 8 0 -2.10 13.20 8 -8 0 47.60 15.80 8 -8 0 74.59 14.40 8 -8 0 74.69 15.80 -8 8 0 69.09 14.20 -8 8 0 77.39 17.10 7 -8 0 210.08 20.10 7 -8 0 171.58 23.50 7 -8 0 205.58 18.00 -7 8 0 183.48 18.20 -7 8 0 201.78 20.30 -7 8 0 205.38 19.50 6 -8 0 89.09 18.20 6 -8 0 91.19 14.50 6 -8 0 69.89 13.70 6 -8 0 85.99 13.40 -6 8 0 71.99 13.70 -6 8 0 85.19 13.70 -6 8 0 69.29 15.30 5 -8 0 19.30 9.70 5 -8 0 1.30 9.70 5 -8 0 -8.10 8.50 5 -8 0 5.20 8.50 -5 8 0 -7.20 6.30 -5 8 0 -4.20 6.20 -5 8 0 -4.20 10.20 -5 8 0 2.70 6.50 4 -8 0 228.98 16.50 4 -8 0 208.28 14.80 4 -8 0 224.28 15.30 4 -8 0 231.28 19.30 -4 8 0 271.97 20.70 -4 8 0 220.48 16.80 -4 8 0 253.57 17.90 -4 8 0 213.48 16.70 3 -8 0 63.99 11.80 3 -8 0 56.89 9.00 3 -8 0 44.60 9.40 -3 8 0 36.70 11.90 -3 8 0 58.09 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4.20 4 8 0 4.40 4.50 4 8 0 11.80 5.40 4 8 0 9.00 5.70 5 8 0 147.99 10.60 5 8 0 132.69 12.60 5 8 0 126.49 9.90 5 8 0 118.29 8.20 5 8 0 132.49 8.50 6 8 0 67.69 15.80 6 8 0 75.29 10.60 6 8 0 64.29 5.90 6 8 0 54.99 7.70 6 8 0 63.79 8.00 7 8 0 73.49 5.40 7 8 0 86.29 8.90 7 8 0 84.09 18.10 7 8 0 58.19 8.00 8 8 0 -7.20 13.70 8 8 0 -6.00 5.60 8 8 0 -3.80 5.70 9 8 0 4.50 14.80 9 8 0 45.50 8.00 10 -9 0 18.20 14.60 10 -9 0 -16.30 19.50 10 -9 0 9.70 13.30 -10 9 0 33.60 16.70 -10 9 0 27.50 14.50 9 -9 0 70.49 16.80 9 -9 0 83.19 14.50 9 -9 0 74.09 22.20 -9 9 0 77.39 16.00 -9 9 0 101.79 19.50 8 -9 0 11.60 12.20 8 -9 0 27.50 13.70 8 -9 0 9.60 17.60 -8 9 0 25.00 12.00 -8 9 0 23.60 12.60 7 -9 0 350.36 28.00 7 -9 0 331.67 24.50 7 -9 0 342.27 23.80 -7 9 0 374.66 28.40 -7 9 0 343.07 24.00 -7 9 0 306.27 23.80 6 -9 0 7.00 8.60 6 -9 0 -3.40 9.50 6 -9 0 9.20 15.10 -6 9 0 0.40 10.10 -6 9 0 -11.10 11.90 -6 9 0 -8.30 7.40 5 -9 0 50.59 12.70 5 -9 0 35.60 12.60 5 -9 0 51.89 11.70 -5 9 0 78.09 12.20 -5 9 0 43.30 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125.79 9.20 0 -5 3 113.79 8.10 0 -5 3 119.99 8.60 0 -5 3 116.69 10.10 0 -5 3 105.19 7.90 -1 5 -3 56.39 7.70 -1 5 -3 58.39 7.30 -1 5 -3 65.49 8.40 -1 5 -3 57.59 9.60 -1 5 -3 51.39 8.70 -1 5 -3 60.19 7.70 1 -5 3 66.79 9.40 1 -5 3 74.59 8.10 1 -5 3 73.09 7.90 1 -5 3 64.89 7.40 1 -5 3 50.59 8.70 -2 5 -3 1374.26 39.90 -2 5 -3 1333.07 41.00 -2 5 -3 1384.96 42.30 -2 5 -3 1369.76 39.60 -2 5 -3 1400.36 40.80 -2 5 -3 1306.97 39.90 2 -5 3 1311.77 38.80 2 -5 3 1339.97 40.00 2 -5 3 1395.36 42.90 2 -5 3 1338.97 40.20 2 -5 3 1326.77 41.00 2 -5 3 1354.56 39.40 -3 5 -3 20.50 8.20 -3 5 -3 22.90 5.00 -3 5 -3 29.90 9.70 -3 5 -3 21.50 6.60 -3 5 -3 17.20 7.60 -3 5 -3 13.30 8.20 -3 5 -3 27.60 7.30 3 -5 3 19.50 6.00 3 -5 3 24.90 7.90 3 -5 3 35.90 8.70 3 -5 3 29.60 10.50 3 -5 3 27.30 6.80 3 -5 3 32.30 8.40 -4 5 -3 62.09 9.10 -4 5 -3 72.29 10.20 -4 5 -3 69.49 5.80 -4 5 -3 65.69 10.00 -4 5 -3 96.49 12.30 4 -5 3 77.99 13.00 4 -5 3 71.09 10.80 4 -5 3 57.19 10.10 4 -5 3 80.59 10.80 -5 5 -3 7.90 8.20 -5 5 -3 8.80 6.60 -5 5 -3 3.50 9.00 -5 5 -3 3.00 7.40 5 -5 3 13.40 11.50 5 -5 3 6.40 8.00 5 -5 3 13.50 8.40 5 -5 3 4.40 8.30 -6 5 -3 95.39 11.40 -6 5 -3 79.89 12.20 -6 5 -3 83.49 13.50 6 -5 3 77.69 12.00 6 -5 3 76.69 10.90 6 -5 3 100.89 14.50 6 -5 3 95.09 13.30 -7 5 -3 47.60 11.30 -7 5 -3 43.00 11.40 -7 5 -3 30.00 11.70 7 -5 3 15.00 11.40 7 -5 3 37.60 11.60 7 -5 3 29.30 11.40 7 -5 3 17.90 10.00 -8 5 -3 -4.10 10.70 -8 5 -3 9.70 9.70 8 -5 3 16.40 11.60 8 -5 3 -7.00 10.10 8 -5 3 -6.50 15.10 -9 5 -3 17.80 13.60 -9 5 -3 18.50 11.20 9 -5 3 15.30 12.50 9 -5 3 4.50 10.50 9 -5 3 -2.00 17.10 -10 5 -3 23.40 12.60 10 -5 3 5.50 15.10 10 -5 3 19.20 11.90 10 -5 3 16.50 12.80 11 -5 3 93.49 18.00 11 -5 3 41.40 19.30 11 -5 3 70.79 15.00 11 4 -3 88.09 10.80 11 4 -3 104.09 22.10 10 4 -3 10.40 14.00 10 4 -3 3.60 6.70 9 4 -3 0.60 5.80 9 4 -3 40.80 15.10 9 4 -3 -0.60 3.70 9 4 -3 -6.50 5.40 8 4 -3 117.09 7.00 8 4 -3 139.89 9.80 8 4 -3 107.19 8.70 8 4 -3 118.09 17.50 7 4 -3 129.39 16.60 7 4 -3 123.69 8.50 7 4 -3 123.99 8.20 7 4 -3 130.89 6.00 6 4 -3 2.40 3.10 6 4 -3 3.00 3.20 6 4 -3 3.50 1.40 6 4 -3 2.40 1.40 6 4 -3 -3.60 8.00 5 4 -3 267.47 8.40 5 4 -3 253.47 14.80 5 4 -3 258.37 8.40 5 4 -3 281.57 17.70 4 4 -3 61.39 8.10 4 4 -3 54.79 2.30 4 4 -3 82.99 9.10 4 4 -3 68.19 9.30 3 4 -3 57.69 2.90 3 4 -3 56.49 8.50 3 4 -3 58.19 2.90 3 4 -3 50.99 7.70 3 4 -3 49.60 8.60 2 4 -3 433.96 12.30 2 4 -3 444.96 16.70 2 4 -3 441.86 17.90 2 4 -3 433.76 18.20 2 4 -3 417.16 12.20 2 4 -3 417.96 12.70 2 4 -3 445.06 12.80 -2 -4 3 408.86 12.00 -2 -4 3 416.16 17.20 -2 -4 3 432.86 12.00 1 4 -3 455.25 19.00 1 4 -3 488.95 15.40 1 4 -3 467.75 15.40 1 4 -3 519.15 18.70 1 4 -3 499.15 15.10 1 4 -3 479.05 15.00 1 4 -3 485.45 17.10 -1 -4 3 498.15 17.70 -1 -4 3 481.85 14.70 -1 -4 3 495.05 18.00 -1 -4 3 473.55 14.70 -1 -4 3 463.35 14.70 -1 -4 3 476.05 14.70 0 4 -3 863.01 25.30 0 4 -3 853.01 26.30 0 4 -3 876.31 27.40 0 4 -3 868.21 25.20 0 4 -3 847.12 24.80 0 4 -3 856.41 26.90 0 4 -3 835.92 25.30 0 -4 3 890.01 26.30 0 -4 3 855.51 25.10 0 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8.80 6.30 4 -4 3 10.20 7.30 4 -4 3 -3.40 6.90 -5 4 -3 225.88 15.70 -5 4 -3 235.68 14.30 -5 4 -3 265.07 17.40 -5 4 -3 266.07 15.90 5 -4 3 242.28 20.30 5 -4 3 223.48 14.40 5 -4 3 249.68 16.90 5 -4 3 260.77 14.20 5 -4 3 220.18 15.80 -6 4 -3 50.29 10.60 -6 4 -3 69.09 11.00 -6 4 -3 62.09 11.00 6 -4 3 88.79 12.10 6 -4 3 92.39 12.00 6 -4 3 64.59 10.40 6 -4 3 81.89 15.00 -7 4 -3 154.68 16.30 -7 4 -3 134.79 14.70 -7 4 -3 140.49 14.90 7 -4 3 175.18 16.40 7 -4 3 139.99 15.10 7 -4 3 157.08 16.30 7 -4 3 162.18 20.20 -8 4 -3 -2.30 11.20 -8 4 -3 -0.80 9.30 8 -4 3 7.20 10.50 8 -4 3 7.50 9.20 8 -4 3 9.70 15.20 -9 4 -3 21.00 11.30 9 -4 3 30.40 12.60 9 -4 3 10.40 12.60 9 -4 3 24.90 11.10 10 -4 3 -13.70 11.40 10 -4 3 -15.00 11.50 10 -4 3 3.50 10.70 11 -4 3 2.40 11.70 11 -4 3 3.50 19.90 11 -4 3 11.90 13.40 11 3 -3 178.98 25.70 11 3 -3 234.18 16.60 10 3 -3 7.30 5.80 10 3 -3 -0.40 14.40 10 3 -3 0.50 7.30 9 3 -3 -11.00 11.40 9 3 -3 5.50 5.00 9 3 -3 2.60 6.40 9 3 -3 2.80 6.50 8 3 -3 51.89 7.30 8 3 -3 52.79 7.60 8 3 -3 79.59 15.20 8 3 -3 65.79 8.00 8 3 -3 66.89 6.80 7 3 -3 95.39 8.10 7 3 -3 91.99 8.00 7 3 -3 102.09 14.50 7 3 -3 103.79 6.90 7 3 -3 85.19 6.50 -7 -3 3 98.19 6.10 -7 -3 3 97.59 6.40 6 3 -3 4.10 6.30 6 3 -3 1.20 2.80 6 3 -3 2.10 3.00 6 3 -3 -0.70 7.60 6 3 -3 2.00 3.80 6 3 -3 1.80 3.80 -6 -3 3 -4.90 2.30 -6 -3 3 0.90 2.30 5 3 -3 21.90 6.20 5 3 -3 20.90 2.80 5 3 -3 20.20 2.60 5 3 -3 17.70 7.50 5 3 -3 20.10 3.60 5 3 -3 18.50 3.40 -5 -3 3 15.40 2.20 -5 -3 3 20.80 2.40 4 3 -3 70.89 4.10 4 3 -3 72.69 4.10 4 3 -3 63.69 8.80 4 3 -3 63.39 2.90 4 3 -3 62.39 2.90 4 3 -3 68.49 8.10 3 3 -3 1955.40 52.99 3 3 -3 1913.21 52.79 3 3 -3 1935.21 53.09 3 3 -3 1961.40 46.50 3 3 -3 1909.61 47.20 3 3 -3 1990.20 47.10 3 3 -3 1914.01 46.50 2 3 -3 6778.52 167.58 2 3 -3 6911.91 170.98 2 3 -3 6970.50 166.58 2 3 -3 7059.49 166.28 2 3 -3 6411.36 171.08 2 3 -3 7033.50 170.18 2 3 -3 7102.39 166.58 -2 -3 3 7225.88 167.48 -2 -3 3 7075.79 167.38 1 3 -3 4434.96 105.59 1 3 -3 4443.76 105.19 1 3 -3 4227.18 105.09 1 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12.10 20.00 8 11 -4 11.90 13.90 7 11 -4 2.80 10.90 7 11 -4 14.20 13.80 6 11 -4 0.90 11.20 6 11 -4 -0.10 1.50 5 11 -4 60.89 6.50 5 11 -4 59.59 13.30 5 11 -4 57.99 6.50 4 11 -4 -4.50 5.30 4 11 -4 -6.00 11.30 4 11 -4 6.40 5.70 4 11 -4 4.30 3.40 3 11 -4 -4.00 4.80 3 11 -4 13.40 11.30 3 11 -4 5.40 6.30 3 11 -4 6.00 6.60 -3 -11 4 7.40 11.00 2 11 -4 4.20 7.50 2 11 -4 23.50 12.20 2 11 -4 5.50 6.00 2 11 -4 9.30 7.30 -2 -11 4 10.50 11.20 1 11 -4 308.17 18.30 1 11 -4 309.47 16.50 1 11 -4 320.17 17.50 1 11 -4 318.77 23.80 -1 -11 4 294.77 14.90 -1 -11 4 349.77 16.30 -1 -11 4 243.58 21.70 0 11 -4 4.00 7.70 0 11 -4 11.70 7.50 0 11 -4 4.50 11.90 0 11 -4 22.30 8.70 0 11 -4 13.20 8.10 0 -11 4 14.00 11.50 0 -11 4 -0.20 6.40 0 -11 4 10.30 6.70 -1 11 -4 50.79 10.30 -1 11 -4 52.59 10.50 -1 11 -4 34.60 10.50 -1 11 -4 57.39 10.40 -1 11 -4 58.99 15.40 1 -11 4 48.80 13.50 1 -11 4 49.60 10.00 1 -11 4 38.20 9.30 -2 11 -4 5.20 9.20 -2 11 -4 1.40 13.50 -2 11 -4 4.70 8.60 2 -11 4 7.00 6.70 2 -11 4 -8.70 10.80 2 -11 4 5.40 8.00 -3 11 -4 304.07 21.90 -3 11 -4 324.57 21.00 -3 11 -4 272.07 24.90 3 -11 4 330.57 24.60 3 -11 4 320.27 20.60 3 -11 4 246.18 23.80 -4 11 -4 15.20 14.90 -4 11 -4 5.90 10.20 -4 11 -4 39.70 12.50 4 -11 4 -1.20 13.60 4 -11 4 8.40 10.90 -5 11 -4 116.19 20.50 -5 11 -4 108.49 17.00 -5 11 -4 99.79 15.40 5 -11 4 97.49 19.70 5 -11 4 112.39 16.50 -6 11 -4 -1.70 12.10 -6 11 -4 13.00 11.90 -6 11 -4 3.10 11.50 6 -11 4 -0.90 11.50 6 -11 4 -5.90 15.10 -7 11 -4 -18.20 13.40 -7 11 -4 -17.80 10.30 7 -11 4 1.30 12.40 7 -11 4 -10.90 17.10 -8 11 -4 47.80 15.10 -8 11 -4 65.79 19.50 8 -11 4 35.00 20.90 8 -11 4 96.79 17.80 -9 11 -4 61.89 19.70 -9 11 -4 57.29 16.40 9 -11 4 47.90 14.20 9 -11 4 31.70 23.10 8 10 -4 119.89 20.00 7 10 -4 20.40 13.00 7 10 -4 17.80 12.10 6 10 -4 -10.50 9.70 6 10 -4 -3.20 10.60 5 10 -4 0.10 3.70 5 10 -4 11.00 10.00 5 10 -4 2.50 3.60 4 10 -4 52.49 6.80 4 10 -4 53.19 6.70 4 10 -4 50.79 4.10 4 10 -4 44.90 4.10 4 10 -4 62.29 12.60 3 10 -4 -0.40 5.50 3 10 -4 10.80 4.70 3 10 -4 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18.50 13.60 -4 -3 15 23.60 11.20 3 3 -15 74.69 16.20 3 3 -15 92.49 15.10 3 3 -15 95.69 16.20 -3 -3 15 85.39 17.30 -3 -3 15 83.79 14.40 2 3 -15 126.19 16.70 2 3 -15 121.49 17.50 2 3 -15 94.99 16.70 -2 -3 15 139.09 17.10 -2 -3 15 145.39 19.20 1 3 -15 -6.30 11.70 1 3 -15 10.20 11.10 1 3 -15 -0.40 12.60 -1 -3 15 6.10 12.00 -1 -3 15 10.80 11.60 0 3 -15 23.10 13.30 0 3 -15 61.09 15.30 0 3 -15 40.80 13.30 0 -3 15 36.70 13.20 0 -3 15 24.10 13.00 -1 3 -15 19.20 11.10 -1 3 -15 25.40 12.90 -1 3 -15 15.10 11.60 1 -3 15 18.50 13.30 1 -3 15 10.40 12.00 -2 3 -15 4.50 12.50 -2 3 -15 27.40 18.10 -2 3 -15 15.00 11.60 2 -3 15 14.80 11.60 2 -3 15 -0.20 10.10 -3 3 -15 24.80 13.90 3 -3 15 15.40 14.10 3 -3 15 15.20 11.10 -4 3 -15 19.70 11.60 4 -3 15 28.50 14.70 9 2 -15 10.50 12.50 -9 -2 15 3.80 14.40 8 2 -15 -10.40 11.30 -8 -2 15 0.30 13.90 7 2 -15 2.30 10.00 7 2 -15 -11.10 9.40 -7 -2 15 -6.70 13.20 6 2 -15 51.59 12.50 6 2 -15 56.09 13.90 -6 -2 15 72.49 17.50 5 2 -15 25.40 11.20 -5 -2 15 21.40 14.20 4 2 -15 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15.90 2 4 -17 50.99 14.40 2 4 -17 45.20 15.70 -2 -4 17 46.00 16.50 -2 -4 17 54.29 14.80 1 4 -17 52.99 14.40 1 4 -17 66.79 17.20 1 4 -17 39.90 16.80 -1 -4 17 58.99 17.00 -1 -4 17 47.40 14.60 0 4 -17 6.20 12.20 0 4 -17 -10.20 13.00 0 4 -17 3.00 12.70 0 -4 17 15.10 14.50 0 -4 17 -0.60 12.60 -1 4 -17 -15.40 12.30 1 -4 17 24.60 15.00 1 -4 17 9.60 12.60 -2 4 -17 -1.00 13.60 2 -4 17 -0.90 13.70 2 -4 17 40.50 15.50 7 3 -17 12.50 11.80 7 3 -17 13.90 13.70 -7 -3 17 -6.80 16.10 6 3 -17 112.79 22.30 6 3 -17 96.19 17.00 6 3 -17 93.59 15.00 -6 -3 17 89.89 19.60 5 3 -17 -3.40 10.30 5 3 -17 7.70 14.90 5 3 -17 19.90 14.50 -5 -3 17 6.10 15.30 4 3 -17 15.70 14.50 4 3 -17 6.00 11.80 4 3 -17 -6.90 12.30 -4 -3 17 -0.30 10.50 3 3 -17 3.00 13.00 3 3 -17 -0.70 13.50 3 3 -17 -7.60 10.20 -3 -3 17 -17.90 12.90 -3 -3 17 3.50 14.00 2 3 -17 28.00 15.60 2 3 -17 27.00 13.20 2 3 -17 27.30 14.90 -2 -3 17 36.40 15.90 -2 -3 17 36.40 14.00 1 3 -17 13.50 13.20 1 3 -17 -25.60 12.10 1 3 -17 28.50 15.10 -1 -3 17 -1.00 13.40 -1 -3 17 7.40 13.30 0 3 -17 11.70 11.60 0 3 -17 26.40 13.50 0 3 -17 4.40 13.70 0 -3 17 5.60 13.80 0 -3 17 19.40 13.80 -1 3 -17 19.60 14.40 1 -3 17 0.60 13.50 1 -3 17 4.10 12.80 -2 3 -17 -17.50 11.50 2 -3 17 10.00 14.80 2 -3 17 12.50 13.50 7 2 -17 44.00 14.00 -7 -2 17 48.20 18.20 6 2 -17 -9.40 9.90 -6 -2 17 11.40 16.00 5 2 -17 279.37 23.70 5 2 -17 335.47 30.10 5 2 -17 264.67 25.10 -5 -2 17 253.77 25.20 4 2 -17 17.70 13.50 4 2 -17 17.10 12.40 4 2 -17 19.50 16.40 -4 -2 17 41.80 16.40 3 2 -17 33.10 14.30 3 2 -17 5.80 12.70 3 2 -17 5.80 13.60 -3 -2 17 16.60 14.90 -3 -2 17 5.30 12.10 2 2 -17 24.30 14.60 2 2 -17 0.40 11.30 2 2 -17 -8.80 11.70 -2 -2 17 -13.20 11.70 -2 -2 17 23.70 15.50 1 2 -17 138.19 19.50 1 2 -17 147.99 21.70 1 2 -17 134.49 18.80 -1 -2 17 104.09 18.60 -1 -2 17 147.09 20.80 0 2 -17 33.40 15.10 0 2 -17 38.50 19.10 0 -2 17 30.10 14.50 0 -2 17 37.00 15.00 -1 2 -17 6.30 12.60 1 -2 17 2.70 13.90 1 -2 17 11.90 13.60 -2 2 -17 0.80 14.10 2 -2 17 -40.20 12.30 2 -2 17 28.20 15.10 7 1 -17 83.59 16.30 7 1 -17 62.19 16.80 -7 -1 17 72.99 20.40 6 1 -17 35.30 13.60 -6 -1 17 33.40 17.00 5 1 -17 87.59 16.50 -5 -1 17 123.89 20.80 4 1 -17 23.80 14.10 4 1 -17 50.39 14.40 4 1 -17 36.60 15.00 -4 -1 17 45.70 14.50 -4 -1 17 35.90 16.70 3 1 -17 3.00 13.90 3 1 -17 5.30 11.90 3 1 -17 8.30 14.50 -3 -1 17 12.10 12.90 -3 -1 17 -7.20 14.30 2 1 -17 28.90 15.30 2 1 -17 7.80 11.50 2 1 -17 -3.40 12.00 -2 -1 17 1.00 14.30 -2 -1 17 -8.10 12.20 1 1 -17 -30.40 12.00 1 1 -17 2.60 12.80 1 1 -17 10.00 13.30 -1 -1 17 6.80 14.80 -1 -1 17 -12.30 11.70 0 1 -17 104.89 18.00 0 -1 17 77.09 17.80 0 -1 17 80.89 18.50 -1 1 -17 38.00 16.40 1 -1 17 39.10 16.20 1 -1 17 37.40 15.20 7 0 -17 20.30 14.00 -7 0 17 -5.90 15.20 6 0 -17 49.99 14.60 6 0 -17 64.39 17.30 -6 0 17 63.09 18.90 5 0 -17 36.80 14.30 -5 0 17 32.60 17.20 4 0 -17 -12.30 11.40 4 0 -17 -9.70 13.10 -4 0 17 -12.90 14.30 -4 0 17 -5.10 12.20 3 0 -17 32.70 16.20 3 0 -17 44.70 14.50 3 0 -17 38.20 14.10 -3 0 17 37.50 16.60 -3 0 17 43.10 15.20 2 0 -17 21.30 13.50 2 0 -17 10.00 11.50 2 0 -17 1.20 12.60 -2 0 17 14.40 14.00 -2 0 17 4.30 14.70 1 0 -17 -8.40 11.60 -1 0 17 28.60 12.60 -1 0 17 29.70 15.10 0 0 -17 1.70 13.20 0 0 17 14.30 14.30 0 0 17 3.90 14.20 -1 0 -17 133.89 20.30 1 0 17 105.79 19.20 1 0 17 105.69 19.70 6 -1 -17 -23.20 12.20 -6 1 17 -14.80 14.60 5 -1 -17 30.20 13.80 5 -1 -17 35.90 16.30 -5 1 17 20.00 13.70 -5 1 17 3.20 16.30 4 -1 -17 53.49 14.60 -4 1 17 47.30 17.00 -4 1 17 46.70 15.10 3 -1 -17 18.90 13.30 3 -1 -17 22.10 15.70 3 -1 -17 23.20 14.00 -3 1 17 29.20 14.80 -3 1 17 8.20 15.70 2 -1 -17 -22.70 11.80 2 -1 -17 25.00 15.70 2 -1 -17 20.20 12.50 -2 1 17 7.80 13.40 -2 1 17 -9.70 15.20 1 -1 -17 23.20 14.80 -1 1 17 34.50 15.00 -1 1 17 24.30 17.80 0 -1 -17 50.79 17.10 0 1 17 29.30 15.80 0 1 17 61.99 18.50 -1 -1 -17 -10.10 9.50 1 1 17 -27.70 14.10 6 -2 -17 -13.60 11.60 6 -2 -17 -2.30 14.60 -6 2 17 -29.80 14.70 5 -2 -17 35.30 16.20 -5 2 17 25.10 17.30 -5 2 17 6.50 13.80 4 -2 -17 -4.10 11.90 4 -2 -17 2.40 14.30 -4 2 17 5.90 13.10 -4 2 17 7.20 16.90 3 -2 -17 -13.80 11.70 3 -2 -17 13.60 15.60 -3 2 17 -17.60 15.40 -3 2 17 5.10 14.30 2 -2 -17 -11.50 12.80 -2 2 17 9.30 16.70 -2 2 17 3.00 15.00 1 -2 -17 11.60 14.20 -1 2 17 25.00 12.30 0 -2 -17 38.50 15.90 0 2 17 21.20 15.60 5 -3 -17 11.50 11.70 -5 3 17 -4.90 13.40 -5 3 17 -25.00 17.10 -4 3 17 -18.50 15.70 -4 3 17 -2.00 13.50 3 -3 -17 21.90 12.00 -3 3 17 11.50 14.50 2 -3 -17 1.40 13.60 -2 3 17 -13.10 13.50 1 -3 -17 55.19 17.00 -1 3 17 61.79 17.20 3 -4 -17 3.50 14.40 3 6 -18 124.99 18.30 3 6 -18 161.38 23.00 3 6 -18 117.19 20.50 -3 -6 18 130.79 20.90 2 6 -18 -3.40 15.80 2 6 -18 0.30 12.20 2 6 -18 -6.00 13.50 -2 -6 18 10.90 15.00 1 6 -18 5.10 15.40 1 6 -18 11.00 16.40 -1 -6 18 2.80 13.90 4 5 -18 -28.00 11.40 4 5 -18 8.70 16.40 4 5 -18 -16.10 11.80 -4 -5 18 -2.80 10.70 3 5 -18 39.90 13.50 3 5 -18 62.39 18.60 3 5 -18 66.79 17.20 -3 -5 18 39.60 17.20 2 5 -18 33.70 14.40 2 5 -18 51.89 17.70 2 5 -18 55.79 16.50 -2 -5 18 30.80 15.60 1 5 -18 -4.60 14.90 1 5 -18 11.20 14.20 1 5 -18 4.40 14.30 -1 -5 18 34.00 16.10 5 4 -18 20.00 12.80 5 4 -18 46.70 15.50 5 4 -18 38.90 17.40 4 4 -18 -1.60 12.50 4 4 -18 3.60 13.30 4 4 -18 25.80 16.00 -4 -4 18 4.10 14.60 3 4 -18 -5.80 12.50 3 4 -18 18.30 14.60 3 4 -18 -7.60 13.70 -3 -4 18 17.60 12.60 2 4 -18 19.90 14.90 2 4 -18 15.30 13.00 2 4 -18 47.70 17.90 -2 -4 18 19.70 14.90 1 4 -18 26.80 15.40 1 4 -18 25.60 13.80 1 4 -18 20.00 14.60 -1 -4 18 22.10 15.90 -1 -4 18 16.10 14.80 0 4 -18 43.40 17.60 0 4 -18 -6.20 17.90 0 -4 18 -6.40 14.00 0 -4 18 6.10 14.40 5 3 -18 85.89 18.00 5 3 -18 60.29 18.60 5 3 -18 53.89 15.00 4 3 -18 -3.10 11.10 4 3 -18 -4.70 14.60 4 3 -18 -17.10 11.80 -4 -3 18 -1.90 15.40 3 3 -18 27.20 17.20 3 3 -18 -3.60 11.60 3 3 -18 9.10 10.80 -3 -3 18 17.10 15.30 2 3 -18 21.50 16.30 2 3 -18 22.20 14.20 2 3 -18 -5.80 14.30 -2 -3 18 8.20 15.00 -2 -3 18 -5.50 13.10 1 3 -18 -17.10 12.30 1 3 -18 -34.30 12.20 1 3 -18 -14.20 14.80 -1 -3 18 7.60 13.80 -1 -3 18 5.80 14.90 0 3 -18 46.00 16.10 0 -3 18 5.30 14.70 0 -3 18 8.90 14.90 5 2 -18 49.99 16.90 5 2 -18 38.10 15.90 5 2 -18 9.80 12.00 -5 -2 18 54.99 21.10 4 2 -18 -7.70 11.90 4 2 -18 4.30 14.00 4 2 -18 -2.80 13.10 -4 -2 18 10.30 15.40 3 2 -18 22.50 15.30 3 2 -18 18.60 14.30 3 2 -18 13.80 13.20 -3 -2 18 6.00 15.60 2 2 -18 18.90 15.40 2 2 -18 44.60 14.30 2 2 -18 16.20 15.00 -2 -2 18 49.60 16.60 -2 -2 18 25.90 14.40 1 2 -18 22.80 15.50 1 2 -18 -0.20 13.00 -1 -2 18 15.40 14.90 -1 -2 18 -0.70 14.30 0 2 -18 7.70 14.00 0 -2 18 49.10 16.50 5 1 -18 130.49 21.90 5 1 -18 52.19 17.10 5 1 -18 62.19 17.70 4 1 -18 26.30 13.10 4 1 -18 9.80 15.70 4 1 -18 -8.90 14.10 -4 -1 18 8.20 15.90 3 1 -18 52.09 15.20 3 1 -18 51.99 17.90 3 1 -18 36.00 14.40 -3 -1 18 34.30 15.10 -3 -1 18 31.70 16.80 2 1 -18 -18.60 14.20 2 1 -18 15.00 14.70 2 1 -18 16.70 14.20 -2 -1 18 -14.90 14.30 -2 -1 18 -22.20 11.00 1 1 -18 15.20 13.40 -1 -1 18 19.60 15.80 -1 -1 18 -9.80 13.30 5 0 -18 161.78 22.80 4 0 -18 77.79 16.90 4 0 -18 37.40 15.60 4 0 -18 48.50 17.40 -4 0 18 16.40 13.90 3 0 -18 17.20 16.20 3 0 -18 1.80 12.90 3 0 -18 -3.50 11.70 -3 0 18 -4.30 12.90 -3 0 18 9.70 16.30 2 0 -18 -4.50 13.00 -2 0 18 -8.40 15.70 -2 0 18 8.80 14.30 1 0 -18 48.50 16.90 -1 0 18 56.09 19.40 4 -1 -18 42.30 17.30 4 -1 -18 6.50 13.50 3 -1 -18 21.40 26.60 3 -1 -18 40.40 17.30 3 -1 -18 23.80 16.30 -3 1 18 10.20 18.00 -3 1 18 1.60 13.80 2 -1 -18 1.90 12.80 -2 1 18 -28.60 14.50 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 63342 _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 P1 P 0.26529(5) 0.69977(4) 0.36576(4) 0.01869(13) Uani 1 1 d . O1 O 0.36864(14) 0.75718(10) 0.47290(9) 0.0237(3) Uani 1 1 d . O2 O 0.37998(14) 0.61575(10) 0.34685(9) 0.0229(3) Uani 1 1 d . O4 O -0.15650(14) 0.88728(11) 0.26337(10) 0.0264(3) Uani 1 1 d . O3 O -0.06092(16) 0.76060(13) -0.00817(10) 0.0387(4) Uani 1 1 d . N1 N 0.04676(16) 0.81877(12) 0.26712(10) 0.0166(4) Uani 1 1 d . N2 N 0.11613(17) 0.77261(12) 0.12363(11) 0.0203(4) Uani 1 1 d . C33 C 0.0858(2) 0.84942(15) 0.56125(14) 0.0239(5) Uani 1 1 d . C30 C 0.06326(19) 0.82960(14) 0.36913(13) 0.0169(4) Uani 1 1 d . C31 C 0.1447(2) 0.91684(14) 0.43037(13) 0.0194(4) Uani 1 1 d . C34 C -0.0052(2) 0.76973(15) 0.49729(14) 0.0231(5) Uani 1 1 d . H34 H -0.0589 0.7226 0.5198 0.028 Uiso 1 1 calc R C1 C 0.15751(19) 0.79057(14) 0.22413(13) 0.0167(4) Uani 1 1 d . C35 C -0.01892(19) 0.75782(14) 0.40136(14) 0.0196(4) Uani 1 1 d . C39 C -0.0665(2) 0.86256(15) 0.22323(14) 0.0200(4) Uani 1 1 d . C32 C 0.1561(2) 0.92325(15) 0.52629(14) 0.0238(5) Uani 1 1 d . H32 H 0.2131 0.9793 0.5684 0.029 Uiso 1 1 calc R C6 C 0.4234(2) 0.89439(16) 0.19906(15) 0.0281(5) Uani 1 1 d . H6A H 0.3618 0.8705 0.1373 0.042 Uiso 1 1 calc GR H6B H 0.5160 0.9183 0.1935 0.042 Uiso 1 1 calc GR H6C H 0.3874 0.9499 0.2322 0.042 Uiso 1 1 calc GR C2 C 0.28703(19) 0.77643(14) 0.27613(13) 0.0162(4) Uani 1 1 d . C4 C 0.5396(2) 0.84979(16) 0.34825(14) 0.0252(5) Uani 1 1 d . H4A H 0.6257 0.8793 0.3366 0.038 Uiso 1 1 calc GR H4B H 0.5584 0.7954 0.3827 0.038 Uiso 1 1 calc GR H4C H 0.5021 0.9020 0.3844 0.038 Uiso 1 1 calc GR C7 C 0.4795(2) 0.70173(16) 0.49681(14) 0.0237(5) Uani 1 1 d . C40 C -0.0666(2) 0.88521(16) 0.12658(14) 0.0231(5) Uani 1 1 d . C3 C 0.43148(19) 0.80585(15) 0.25353(13) 0.0198(4) Uani 1 1 d . C8 C 0.4864(2) 0.62539(16) 0.42746(14) 0.0228(5) Uani 1 1 d . C21 C 0.1746(2) 0.69435(16) 0.06796(14) 0.0258(5) Uani 1 1 d . C41 C -0.0081(2) 0.80056(16) 0.07352(14) 0.0253(5) Uani 1 1 d . C37 C 0.1099(3) 0.85250(18) 0.66578(15) 0.0383(6) Uani 1 1 d . H37A H 0.0233 0.8271 0.6794 0.057 Uiso 1 1 calc GR H37B H 0.1410 0.9222 0.6992 0.057 Uiso 1 1 calc GR H37C H 0.1806 0.8102 0.6853 0.057 Uiso 1 1 calc GR C38 C -0.1144(2) 0.66806(16) 0.33515(15) 0.0278(5) Uani 1 1 d . H38A H -0.1786 0.6926 0.2872 0.042 Uiso 1 1 calc GR H38B H -0.1669 0.6309 0.3695 0.042 Uiso 1 1 calc GR H38C H -0.0589 0.6232 0.3063 0.042 Uiso 1 1 calc GR C42 C -0.2160(2) 0.89350(18) 0.07335(15) 0.0336(5) Uani 1 1 d . H42A H -0.2756 0.8294 0.0657 0.050 Uiso 1 1 calc GR H42B H -0.2146 0.9087 0.0125 0.050 Uiso 1 1 calc GR H42C H -0.2519 0.9477 0.1083 0.050 Uiso 1 1 calc GR C5 C 0.4939(2) 0.71894(16) 0.20162(15) 0.0259(5) Uani 1 1 d . H5A H 0.4352 0.6953 0.1389 0.039 Uiso 1 1 calc GR H5B H 0.4982 0.6628 0.2351 0.039 Uiso 1 1 calc GR H5C H 0.5872 0.7444 0.1984 0.039 Uiso 1 1 calc GR C36 C 0.2182(2) 1.00258(15) 0.39670(14) 0.0258(5) Uani 1 1 d . H36A H 0.2790 0.9750 0.3595 0.039 Uiso 1 1 calc GR H36B H 0.2733 1.0524 0.4500 0.039 Uiso 1 1 calc GR H36C H 0.1491 1.0350 0.3591 0.039 Uiso 1 1 calc GR C9 C 0.5937(2) 0.56119(16) 0.43542(16) 0.0287(5) Uani 1 1 d . C26 C 0.1633(2) 0.59306(17) 0.08272(14) 0.0290(5) Uani 1 1 d . C24 C 0.2871(3) 0.5480(2) -0.04006(17) 0.0467(7) Uani 1 1 d . C22 C 0.2306(2) 0.72130(19) -0.00507(15) 0.0342(6) Uani 1 1 d . C43 C 0.0316(2) 0.98774(16) 0.14070(15) 0.0286(5) Uani 1 1 d . H43A H -0.0029 1.0418 0.1769 0.043 Uiso 1 1 calc GR H43B H 0.0334 1.0043 0.0804 0.043 Uiso 1 1 calc GR H43C H 0.1253 0.9808 0.1736 0.043 Uiso 1 1 calc GR C20 C 0.5749(2) 0.72164(17) 0.58726(15) 0.0323(6) Uani 1 1 d . C23 C 0.2870(3) 0.6469(2) -0.05679(16) 0.0459(7) Uani 1 1 d . H23 H 0.3263 0.6645 -0.1045 0.055 Uiso 1 1 calc R C19 C 0.5607(3) 0.79695(19) 0.66178(16) 0.0414(6) Uani 1 1 d . H19 H 0.4913 0.8396 0.6513 0.050 Uiso 1 1 calc R C25 C 0.2229(2) 0.52232(19) 0.02848(17) 0.0422(6) Uani 1 1 d . H25 H 0.2194 0.4551 0.0389 0.051 Uiso 1 1 calc R C29 C 0.0847(2) 0.55557(17) 0.14907(16) 0.0375(6) Uani 1 1 d . H29A H 0.1499 0.5555 0.2080 0.056 Uiso 1 1 calc GR H29B H 0.0373 0.4869 0.1222 0.056 Uiso 1 1 calc GR H29C H 0.0164 0.6003 0.1595 0.056 Uiso 1 1 calc GR C14 C 0.6946(2) 0.57851(19) 0.52331(19) 0.0377(6) Uani 1 1 d . C10 C 0.6010(2) 0.48376(17) 0.36046(19) 0.0375(6) Uani 1 1 d . H10 H 0.5332 0.4728 0.3035 0.045 Uiso 1 1 calc R C27 C 0.2257(3) 0.8242(2) -0.03538(17) 0.0480(7) Uani 1 1 d . H27A H 0.1515 0.8175 -0.0916 0.072 Uiso 1 1 calc GR H27B H 0.3144 0.8466 -0.0477 0.072 Uiso 1 1 calc GR H27C H 0.2080 0.8739 0.0139 0.072 Uiso 1 1 calc GR C11 C 0.7081(3) 0.42440(19) 0.3712(2) 0.0527(8) Uani 1 1 d . H11 H 0.7136 0.3735 0.3215 0.063 Uiso 1 1 calc R C15 C 0.6824(2) 0.6571(2) 0.60062(17) 0.0395(7) Uani 1 1 d . C12 C 0.8085(3) 0.4408(2) 0.4571(3) 0.0614(10) Uani 1 1 d . H12 H 0.8807 0.4001 0.4643 0.074 Uiso 1 1 calc R C16 C 0.7713(3) 0.6723(2) 0.6927(2) 0.0585(9) Uani 1 1 d . H16 H 0.8434 0.6321 0.7046 0.070 Uiso 1 1 calc R C13 C 0.8030(2) 0.5150(2) 0.5304(2) 0.0526(8) Uani 1 1 d . H13 H 0.8721 0.5245 0.5867 0.063 Uiso 1 1 calc R C18 C 0.6490(3) 0.8077(2) 0.75001(18) 0.0590(9) Uani 1 1 d . H18 H 0.6388 0.8568 0.7995 0.071 Uiso 1 1 calc R C17 C 0.7540(3) 0.7447(3) 0.7650(2) 0.0678(10) Uani 1 1 d . H17 H 0.8133 0.7519 0.8249 0.081 Uiso 1 1 calc R C28 C 0.3487(3) 0.4684(3) -0.0986(2) 0.0742(11) Uani 1 1 d . H28A H 0.3068 0.4648 -0.1644 0.111 Uiso 1 1 calc GR H28B H 0.3294 0.4022 -0.0826 0.111 Uiso 1 1 calc GR H28C H 0.4489 0.4877 -0.0860 0.111 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 P1 0.0176(3) 0.0199(3) 0.0189(3) 0.0047(2) 0.0034(2) 0.0050(2) O1 0.0237(8) 0.0279(8) 0.0178(7) 0.0030(6) 0.0008(6) 0.0077(6) O2 0.0219(7) 0.0237(8) 0.0236(8) 0.0044(6) 0.0038(6) 0.0104(6) O4 0.0225(8) 0.0339(9) 0.0278(8) 0.0100(7) 0.0102(7) 0.0122(7) O3 0.0391(9) 0.0538(11) 0.0175(8) -0.0026(7) -0.0043(7) 0.0221(8) N1 0.0172(8) 0.0190(9) 0.0141(8) 0.0042(7) 0.0035(7) 0.0042(7) N2 0.0217(9) 0.0246(9) 0.0140(8) 0.0006(7) 0.0026(7) 0.0100(7) C33 0.0313(12) 0.0237(11) 0.0201(11) 0.0033(9) 0.0111(9) 0.0106(9) C30 0.0168(10) 0.0204(10) 0.0152(10) 0.0042(8) 0.0048(8) 0.0075(8) C31 0.0198(10) 0.0178(10) 0.0213(11) 0.0028(8) 0.0057(9) 0.0058(8) C34 0.0266(11) 0.0222(11) 0.0281(12) 0.0108(9) 0.0157(9) 0.0085(9) C1 0.0212(10) 0.0156(10) 0.0145(10) 0.0026(8) 0.0066(8) 0.0032(8) C35 0.0165(10) 0.0188(10) 0.0247(11) 0.0048(9) 0.0063(9) 0.0045(8) C39 0.0179(10) 0.0196(10) 0.0210(11) 0.0021(9) 0.0032(9) 0.0031(8) C32 0.0270(11) 0.0202(11) 0.0219(11) -0.0013(9) 0.0048(9) 0.0037(9) C6 0.0272(12) 0.0307(12) 0.0302(12) 0.0091(10) 0.0127(10) 0.0035(10) C2 0.0154(10) 0.0154(10) 0.0157(10) -0.0004(8) 0.0018(8) 0.0032(8) C4 0.0196(11) 0.0288(12) 0.0255(12) 0.0021(9) 0.0063(9) -0.0016(9) C7 0.0185(11) 0.0302(12) 0.0230(11) 0.0139(10) 0.0013(9) 0.0017(9) C40 0.0238(11) 0.0289(12) 0.0192(11) 0.0076(9) 0.0052(9) 0.0115(9) C3 0.0174(10) 0.0224(11) 0.0202(11) 0.0036(9) 0.0063(8) 0.0034(8) C8 0.0175(10) 0.0279(12) 0.0249(12) 0.0141(10) 0.0027(9) 0.0023(9) C21 0.0231(11) 0.0326(12) 0.0174(11) -0.0030(9) -0.0012(9) 0.0119(9) C41 0.0246(11) 0.0319(12) 0.0204(12) 0.0077(10) 0.0032(9) 0.0097(9) C37 0.0603(16) 0.0346(14) 0.0233(12) 0.0066(10) 0.0148(12) 0.0107(12) C38 0.0242(11) 0.0267(12) 0.0314(12) 0.0068(10) 0.0060(10) -0.0015(9) C42 0.0299(12) 0.0492(15) 0.0252(12) 0.0110(11) 0.0045(10) 0.0210(11) C5 0.0207(11) 0.0311(12) 0.0267(12) 0.0025(10) 0.0088(9) 0.0058(9) C36 0.0307(12) 0.0212(11) 0.0244(12) 0.0027(9) 0.0078(10) -0.0002(9) C9 0.0178(11) 0.0280(12) 0.0482(15) 0.0253(11) 0.0110(10) 0.0039(9) C26 0.0247(12) 0.0315(13) 0.0208(11) -0.0062(10) -0.0080(9) 0.0080(10) C24 0.0345(14) 0.0647(19) 0.0283(14) -0.0200(13) -0.0051(11) 0.0256(13) C22 0.0316(13) 0.0538(16) 0.0167(11) 0.0008(11) 0.0042(10) 0.0184(11) C43 0.0384(13) 0.0305(12) 0.0245(12) 0.0119(10) 0.0146(10) 0.0137(10) C20 0.0284(12) 0.0362(13) 0.0288(13) 0.0189(11) -0.0031(10) -0.0095(10) C23 0.0373(15) 0.075(2) 0.0220(13) -0.0057(13) 0.0049(11) 0.0240(14) C19 0.0501(15) 0.0405(14) 0.0253(13) 0.0132(11) -0.0035(11) -0.0148(12) C25 0.0371(14) 0.0364(14) 0.0363(14) -0.0152(11) -0.0134(12) 0.0157(11) C29 0.0410(14) 0.0255(12) 0.0347(14) -0.0010(10) -0.0073(11) 0.0013(11) C14 0.0170(11) 0.0417(14) 0.0608(17) 0.0387(14) 0.0033(11) 0.0007(10) C10 0.0283(13) 0.0270(13) 0.0685(18) 0.0237(13) 0.0228(12) 0.0082(10) C27 0.0569(17) 0.0695(19) 0.0270(14) 0.0172(13) 0.0179(12) 0.0230(14) C11 0.0367(15) 0.0322(14) 0.110(3) 0.0348(16) 0.0402(17) 0.0149(12) C15 0.0207(12) 0.0500(16) 0.0455(15) 0.0365(13) -0.0085(11) -0.0121(11) C12 0.0268(15) 0.0485(18) 0.131(3) 0.059(2) 0.0299(18) 0.0193(13) C16 0.0343(15) 0.068(2) 0.065(2) 0.0479(18) -0.0187(14) -0.0166(14) C13 0.0183(13) 0.0580(19) 0.093(2) 0.0589(18) 0.0064(14) 0.0035(12) C18 0.074(2) 0.0549(18) 0.0313(15) 0.0175(14) -0.0128(14) -0.0274(16) C17 0.064(2) 0.076(2) 0.0431(18) 0.0354(18) -0.0273(16) -0.0323(18) C28 0.0543(19) 0.095(2) 0.0511(18) -0.0401(17) -0.0059(15) 0.0405(17) 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' N N 0.0061 0.0033 '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 O1 P1 O2 92.84(7) O1 P1 C2 110.87(8) O2 P1 C2 98.38(8) C7 O1 P1 109.26(12) C8 O2 P1 109.63(12) C1 N1 C30 121.44(15) C39 N1 C30 113.15(15) C39 N1 C1 123.49(15) C1 N2 C21 120.18(15) C41 N2 C1 122.97(16) C41 N2 C21 113.83(16) C34 C33 C37 120.40(19) C32 C33 C34 118.06(18) C32 C33 C37 121.51(19) C31 C30 N1 119.99(16) C31 C30 C35 121.39(17) C35 C30 N1 118.09(16) C30 C31 C36 122.89(17) C32 C31 C30 117.50(17) C32 C31 C36 119.61(17) C33 C34 H34 118.9 C35 C34 C33 122.28(18) C35 C34 H34 118.9 N2 C1 N1 113.12(15) C2 C1 N1 122.20(16) C2 C1 N2 124.56(17) C30 C35 C38 121.74(17) C34 C35 C30 117.83(18) C34 C35 C38 120.39(17) O4 C39 N1 121.11(17) O4 C39 C40 121.80(17) N1 C39 C40 116.93(16) C33 C32 C31 122.34(19) C33 C32 H32 118.8 C31 C32 H32 118.8 H6A C6 H6B 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 C3 C6 H6A 109.5 C3 C6 H6B 109.5 C3 C6 H6C 109.5 C1 C2 P1 110.61(13) C1 C2 C3 125.25(16) C3 C2 P1 123.53(13) H4A C4 H4B 109.5 H4A C4 H4C 109.5 H4B C4 H4C 109.5 C3 C4 H4A 109.5 C3 C4 H4B 109.5 C3 C4 H4C 109.5 O1 C7 C20 123.3(2) C8 C7 O1 113.88(17) C8 C7 C20 122.8(2) C39 C40 C42 110.24(17) C39 C40 C43 107.54(16) C41 C40 C39 108.86(16) C41 C40 C42 110.56(17) C41 C40 C43 108.91(16) C42 C40 C43 110.66(17) C6 C3 C2 110.33(16) C6 C3 C4 105.36(16) C6 C3 C5 109.08(16) C4 C3 C2 107.26(15) C5 C3 C2 117.17(16) C5 C3 C4 106.94(16) O2 C8 C9 122.90(19) C7 C8 O2 113.69(18) C7 C8 C9 123.4(2) C26 C21 N2 120.07(18) C26 C21 C22 121.1(2) C22 C21 N2 118.61(19) O3 C41 N2 121.32(19) O3 C41 C40 123.25(19) N2 C41 C40 115.39(17) C33 C37 H37A 109.5 C33 C37 H37B 109.5 C33 C37 H37C 109.5 H37A C37 H37B 109.5 H37A C37 H37C 109.5 H37B C37 H37C 109.5 C35 C38 H38A 109.5 C35 C38 H38B 109.5 C35 C38 H38C 109.5 H38A C38 H38B 109.5 H38A C38 H38C 109.5 H38B C38 H38C 109.5 C40 C42 H42A 109.5 C40 C42 H42B 109.5 C40 C42 H42C 109.5 H42A C42 H42B 109.5 H42A C42 H42C 109.5 H42B C42 H42C 109.5 C3 C5 H5A 109.5 C3 C5 H5B 109.5 C3 C5 H5C 109.5 H5A C5 H5B 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 C31 C36 H36A 109.5 C31 C36 H36B 109.5 C31 C36 H36C 109.5 H36A C36 H36B 109.5 H36A C36 H36C 109.5 H36B C36 H36C 109.5 C8 C9 C14 116.7(2) C10 C9 C8 122.2(2) C10 C9 C14 121.1(2) C21 C26 C29 123.79(19) C25 C26 C21 117.4(2) C25 C26 C29 118.7(2) C23 C24 C25 117.8(2) C23 C24 C28 120.9(3) C25 C24 C28 121.2(3) C21 C22 C27 124.3(2) C23 C22 C21 118.2(2) C23 C22 C27 117.4(2) C40 C43 H43A 109.5 C40 C43 H43B 109.5 C40 C43 H43C 109.5 H43A C43 H43B 109.5 H43A C43 H43C 109.5 H43B C43 H43C 109.5 C7 C20 C15 116.3(2) C19 C20 C7 122.4(2) C19 C20 C15 121.2(2) C24 C23 C22 122.4(2) C24 C23 H23 118.8 C22 C23 H23 118.8 C20 C19 H19 119.9 C18 C19 C20 120.1(3) C18 C19 H19 119.9 C26 C25 H25 118.6 C24 C25 C26 122.8(2) C24 C25 H25 118.6 C26 C29 H29A 109.5 C26 C29 H29B 109.5 C26 C29 H29C 109.5 H29A C29 H29B 109.5 H29A C29 H29C 109.5 H29B C29 H29C 109.5 C9 C14 C15 120.0(2) C9 C14 C13 116.4(3) C13 C14 C15 123.6(2) C9 C10 H10 120.0 C11 C10 C9 120.1(3) C11 C10 H10 120.0 C22 C27 H27A 109.5 C22 C27 H27B 109.5 C22 C27 H27C 109.5 H27A C27 H27B 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C10 C11 H11 120.2 C10 C11 C12 119.6(3) C12 C11 H11 120.2 C20 C15 C14 120.6(2) C16 C15 C20 116.3(3) C16 C15 C14 123.1(3) C11 C12 H12 119.4 C13 C12 C11 121.2(3) C13 C12 H12 119.4 C15 C16 H16 119.2 C17 C16 C15 121.7(3) C17 C16 H16 119.2 C14 C13 H13 119.2 C12 C13 C14 121.7(3) C12 C13 H13 119.2 C19 C18 H18 120.1 C19 C18 C17 119.7(3) C17 C18 H18 120.1 C16 C17 C18 121.0(3) C16 C17 H17 119.5 C18 C17 H17 119.5 C24 C28 H28A 109.5 C24 C28 H28B 109.5 C24 C28 H28C 109.5 H28A C28 H28B 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance P1 O1 1.6904(14) P1 O2 1.6969(14) P1 C2 1.8392(19) O1 C7 1.386(2) O2 C8 1.377(2) O4 C39 1.215(2) O3 C41 1.212(2) N1 C30 1.466(2) N1 C1 1.431(2) N1 C39 1.386(2) N2 C1 1.426(2) N2 C21 1.464(2) N2 C41 1.395(2) C33 C34 1.386(3) C33 C32 1.380(3) C33 C37 1.508(3) C30 C31 1.397(3) C30 C35 1.401(3) C31 C32 1.390(3) C31 C36 1.502(3) C34 H34 0.9300 C34 C35 1.380(3) C1 C2 1.378(3) C35 C38 1.498(3) C39 C40 1.512(3) C32 H32 0.9300 C6 H6A 0.9600 C6 H6B 0.9600 C6 H6C 0.9600 C6 C3 1.531(3) C2 C3 1.558(3) C4 H4A 0.9600 C4 H4B 0.9600 C4 H4C 0.9600 C4 C3 1.541(3) C7 C8 1.339(3) C7 C20 1.419(3) C40 C41 1.502(3) C40 C42 1.524(3) C40 C43 1.545(3) C3 C5 1.537(3) C8 C9 1.416(3) C21 C26 1.396(3) C21 C22 1.401(3) C37 H37A 0.9600 C37 H37B 0.9600 C37 H37C 0.9600 C38 H38A 0.9600 C38 H38B 0.9600 C38 H38C 0.9600 C42 H42A 0.9600 C42 H42B 0.9600 C42 H42C 0.9600 C5 H5A 0.9600 C5 H5B 0.9600 C5 H5C 0.9600 C36 H36A 0.9600 C36 H36B 0.9600 C36 H36C 0.9600 C9 C14 1.416(3) C9 C10 1.405(3) C26 C25 1.395(3) C26 C29 1.498(3) C24 C23 1.377(4) C24 C25 1.382(4) C24 C28 1.517(3) C22 C23 1.387(3) C22 C27 1.509(3) C43 H43A 0.9600 C43 H43B 0.9600 C43 H43C 0.9600 C20 C19 1.406(3) C20 C15 1.423(3) C23 H23 0.9300 C19 H19 0.9300 C19 C18 1.373(3) C25 H25 0.9300 C29 H29A 0.9600 C29 H29B 0.9600 C29 H29C 0.9600 C14 C15 1.454(4) C14 C13 1.417(3) C10 H10 0.9300 C10 C11 1.371(3) C27 H27A 0.9600 C27 H27B 0.9600 C27 H27C 0.9600 C11 H11 0.9300 C11 C12 1.393(4) C15 C16 1.416(3) C12 H12 0.9300 C12 C13 1.358(4) C16 H16 0.9300 C16 C17 1.371(4) C13 H13 0.9300 C18 H18 0.9300 C18 C17 1.391(4) C17 H17 0.9300 C28 H28A 0.9600 C28 H28B 0.9600 C28 H28C 0.9600