#------------------------------------------------------------------------------ #$Date: 2017-08-20 01:42:18 +0300 (Sun, 20 Aug 2017) $ #$Revision: 199858 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/12/63/4126329.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_4126329 loop_ _publ_author_name 'Li, Zhanyu' 'Zhao, Jinbo' 'Sun, Baozhen' 'Zhou, Tingting' 'Liu, Mingzhu' 'Liu, Shuang' 'Zhang, Mengru' 'Zhang, Qian' _publ_section_title ; Asymmetric Nitrone Synthesis via Ligand-Enabled Copper-Catalyzed Cope-Type Hydroamination of Cyclopropene with Oxime. ; _journal_name_full 'Journal of the American Chemical Society' _journal_paper_doi 10.1021/jacs.7b06523 _journal_year 2017 _chemical_absolute_configuration ad _chemical_formula_moiety 'C27 H23 N O' _chemical_formula_sum 'C26 H23 N2 O' _chemical_formula_weight 379.46 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2017-07-30 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.7558(3) _cell_length_b 11.1462(4) _cell_length_c 21.2016(7) _cell_measurement_reflns_used 9957 _cell_measurement_temperature 293.0 _cell_measurement_theta_max 72.32 _cell_measurement_theta_min 4.48 _cell_volume 2069.15(12) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _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 292.7 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_unetI/netI 0.0195 _diffrn_reflns_Laue_measured_fraction_full 0.988 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 35129 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 72.773 _diffrn_reflns_theta_min 4.170 _exptl_absorpt_coefficient_mu 0.580 _exptl_absorpt_correction_T_max 0.944 _exptl_absorpt_correction_T_min 0.901 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ad _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.218 _exptl_crystal_description cube _exptl_crystal_F_000 804 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.126 _refine_diff_density_min -0.124 _refine_diff_density_rms 0.027 _refine_ls_abs_structure_details ; Flack x determined using 1580 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.04(9) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 263 _refine_ls_number_reflns 4085 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.067 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0430 _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^)+(0.0463P)^2^+0.3577P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1055 _refine_ls_wR_factor_ref 0.1094 _reflns_Friedel_coverage 0.749 _reflns_Friedel_fraction_full 0.993 _reflns_Friedel_fraction_max 0.990 _reflns_number_gt 3822 _reflns_number_total 4085 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja7b06523_si_002.cif _cod_data_source_block 2 _cod_database_code 4126329 _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, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C1(H1) 2.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B) 2.c Aromatic/amide H refined with riding coordinates: C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27) 2.d Idealised Me refined as rotating group: C14(H14A,H14B,H14C) ; _shelx_res_file ; 2.res created by SHELXL-2014/7 TITL 2_a.res in P2(1)2(1)2(1) REM Old TITL 2 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.150, Rweak 0.033, Alpha 0.006, Orientation as input REM Flack x = 0.173 ( 0.080 ) from Parsons' quotients REM Formula found by SHELXT: C26 N2 O CELL 1.54178 8.7558 11.1462 21.2016 90 90 90 ZERR 4 0.0003 0.0004 0.0007 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O UNIT 104 92 8 4 L.S. 20 PLAN 20 TEMP 19.55 HTAB C17 O1 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.046300 0.357700 FVAR 1.65018 O1 4 0.480452 0.849759 0.592854 11.00000 0.09231 0.03895 = 0.10742 0.01289 -0.00310 0.00371 N1 3 0.517754 0.738675 0.602566 11.00000 0.06248 0.04000 = 0.06416 0.00609 0.00955 0.00035 C1 1 0.433805 0.649255 0.565096 11.00000 0.06195 0.04703 = 0.05092 0.00437 0.00150 0.00358 AFIX 13 H1 2 0.494028 0.580408 0.550674 11.00000 -1.20000 AFIX 0 C2 1 0.316809 0.692870 0.520351 11.00000 0.08771 0.06182 = 0.06884 0.02286 -0.01530 -0.00390 AFIX 23 H2A 2 0.309639 0.653126 0.479757 11.00000 -1.20000 H2B 2 0.296371 0.778383 0.519418 11.00000 -1.20000 AFIX 0 C3 1 0.266326 0.624199 0.577411 11.00000 0.05801 0.04542 = 0.06301 0.00814 0.00242 0.00595 C4 1 0.215169 0.496951 0.567386 11.00000 0.05114 0.05085 = 0.05110 0.00221 0.00303 0.00422 C5 1 0.098640 0.472197 0.523456 11.00000 0.06674 0.06309 = 0.06814 0.01164 -0.01346 0.00672 AFIX 43 H5 2 0.055229 0.534938 0.500769 11.00000 -1.20000 AFIX 0 C6 1 0.048395 0.358142 0.513595 11.00000 0.07968 0.07319 = 0.07504 0.00478 -0.02748 -0.00549 AFIX 43 H6 2 -0.028919 0.344407 0.484398 11.00000 -1.20000 AFIX 0 C7 1 0.111463 0.260525 0.546848 11.00000 0.06556 0.05626 = 0.05324 -0.00393 -0.00208 -0.00423 C8 1 0.061662 0.140659 0.537957 11.00000 0.10021 0.06723 = 0.07862 -0.01160 -0.01641 -0.01540 AFIX 43 H8 2 -0.015785 0.124281 0.509200 11.00000 -1.20000 AFIX 0 C9 1 0.125905 0.050055 0.570961 11.00000 0.11051 0.05453 = 0.07788 -0.00782 0.00054 -0.01654 AFIX 43 H9 2 0.092116 -0.028118 0.564607 11.00000 -1.20000 AFIX 0 C10 1 0.241973 0.072047 0.614350 11.00000 0.09495 0.04789 = 0.07184 0.00545 0.00735 0.00520 AFIX 43 H10 2 0.285575 0.008720 0.636519 11.00000 -1.20000 AFIX 0 C11 1 0.291417 0.185715 0.624281 11.00000 0.07377 0.05194 = 0.06681 0.00691 -0.00670 -0.00002 AFIX 43 H11 2 0.368682 0.199546 0.653488 11.00000 -1.20000 AFIX 0 C12 1 0.227580 0.283845 0.590994 11.00000 0.05459 0.04757 = 0.04780 -0.00054 0.00352 0.00165 C13 1 0.276228 0.403620 0.600403 11.00000 0.05781 0.04917 = 0.05251 0.00308 -0.00723 -0.00096 AFIX 43 H13 2 0.352115 0.419101 0.629995 11.00000 -1.20000 AFIX 0 C14 1 0.186931 0.689865 0.630386 11.00000 0.07923 0.05846 = 0.11696 -0.01821 0.02660 0.00265 AFIX 137 H14A 2 0.226945 0.769831 0.633511 11.00000 -1.50000 H14B 2 0.204082 0.648138 0.669359 11.00000 -1.50000 H14C 2 0.079295 0.693369 0.621966 11.00000 -1.50000 AFIX 0 C15 1 0.625914 0.705411 0.642191 11.00000 0.05465 0.04263 = 0.05404 -0.00081 0.00857 -0.00234 C16 1 0.728282 0.791104 0.673822 11.00000 0.05990 0.04791 = 0.06183 -0.00908 0.01974 -0.00757 C17 1 0.741708 0.912235 0.657682 11.00000 0.09687 0.05310 = 0.09078 -0.00546 0.01117 -0.01862 AFIX 43 H17 2 0.680171 0.945104 0.626382 11.00000 -1.20000 AFIX 0 C18 1 0.849297 0.983640 0.689333 11.00000 0.10995 0.06381 = 0.12965 -0.01960 0.02234 -0.03085 AFIX 43 H18 2 0.859806 1.063888 0.678135 11.00000 -1.20000 AFIX 0 C19 1 0.938659 0.937799 0.736129 11.00000 0.08557 0.09729 = 0.11596 -0.03434 0.00958 -0.03450 AFIX 43 H19 2 1.008353 0.986874 0.756867 11.00000 -1.20000 AFIX 0 C20 1 0.925902 0.820805 0.752399 11.00000 0.07336 0.09009 = 0.10004 -0.02153 -0.00112 -0.02254 AFIX 43 H20 2 0.986613 0.789652 0.784449 11.00000 -1.20000 AFIX 0 C21 1 0.823391 0.747891 0.721653 11.00000 0.05956 0.06808 = 0.07834 -0.00867 0.00075 -0.00841 AFIX 43 H21 2 0.817158 0.667453 0.733020 11.00000 -1.20000 AFIX 0 C22 1 0.642263 0.575020 0.656486 11.00000 0.05303 0.04271 = 0.05464 0.00130 -0.00157 -0.00318 C23 1 0.732260 0.500109 0.620230 11.00000 0.07423 0.05892 = 0.07069 0.00412 0.00826 0.01167 AFIX 43 H23 2 0.783953 0.530488 0.585397 11.00000 -1.20000 AFIX 0 C24 1 0.745597 0.379813 0.635694 11.00000 0.08660 0.05762 = 0.10129 -0.00199 0.00140 0.01968 AFIX 43 H24 2 0.802904 0.328876 0.610260 11.00000 -1.20000 AFIX 0 C25 1 0.674490 0.335743 0.688405 11.00000 0.07908 0.05312 = 0.11297 0.02290 -0.01657 0.00190 AFIX 43 H25 2 0.685066 0.255165 0.698916 11.00000 -1.20000 AFIX 0 C26 1 0.588593 0.408961 0.725446 11.00000 0.07206 0.06991 = 0.07818 0.02582 -0.00667 -0.01279 AFIX 43 H26 2 0.542546 0.378936 0.761686 11.00000 -1.20000 AFIX 0 C27 1 0.569928 0.527592 0.709203 11.00000 0.06140 0.05936 = 0.06173 0.00513 0.00537 -0.00538 AFIX 43 H27 2 0.508088 0.576648 0.733836 11.00000 -1.20000 AFIX 0 HKLF 4 REM 2_a.res in P2(1)2(1)2(1) REM R1 = 0.0430 for 3822 Fo > 4sig(Fo) and 0.0468 for all 4085 data REM 263 parameters refined using 0 restraints END WGHT 0.0463 0.3577 REM Highest difference peak 0.126, deepest hole -0.124, 1-sigma level 0.027 Q1 1 0.6347 0.5180 0.6264 11.00000 0.05 0.13 Q2 1 0.2122 0.6948 0.5436 11.00000 0.05 0.11 Q3 1 0.2048 0.2626 0.5551 11.00000 0.05 0.11 Q4 1 0.5955 0.3825 0.6912 11.00000 0.05 0.10 Q5 1 0.8044 1.0531 0.6511 11.00000 0.05 0.10 Q6 1 0.4234 0.2025 0.6328 11.00000 0.05 0.10 Q7 1 0.8017 0.4344 0.6495 11.00000 0.05 0.10 Q8 1 0.6391 0.6374 0.6497 11.00000 0.05 0.10 Q9 1 0.7873 1.0192 0.7270 11.00000 0.05 0.09 Q10 1 0.6052 0.3852 0.6450 11.00000 0.05 0.09 Q11 1 -0.0022 0.5484 0.5660 11.00000 0.05 0.09 Q12 1 0.6324 0.7189 0.6038 11.00000 0.05 0.09 Q13 1 0.3630 0.6141 0.5928 11.00000 0.05 0.09 Q14 1 -0.0753 0.3398 0.5102 11.00000 0.05 0.09 Q15 1 0.6486 0.5573 0.6964 11.00000 0.05 0.09 Q16 1 0.4138 0.7404 0.6452 11.00000 0.05 0.08 Q17 1 0.0620 0.6045 0.4561 11.00000 0.05 0.08 Q18 1 -0.0065 0.1639 0.4781 11.00000 0.05 0.08 Q19 1 0.4997 0.7116 0.6486 11.00000 0.05 0.08 Q20 1 0.6019 0.8059 0.5583 11.00000 0.05 0.08 ; _shelx_res_checksum 90391 _shelx_hkl_file ; 3 0 0 -0.50 1.10 -3 0 0 1.40 1.20 -3 0 0 0.50 1.60 4 0 0 5289.77 190.08 -4 0 0 5084.39 188.18 4 0 0 5226.68 188.48 -4 0 0 4870.41 190.68 -5 0 0 3.00 3.70 -5 0 0 -1.70 3.10 -5 0 0 1.80 3.10 5 0 0 -1.20 4.40 5 0 0 3.20 2.20 5 0 0 0.40 2.30 6 0 0 2103.29 75.79 -6 0 0 1986.80 75.49 6 0 0 1994.40 75.09 6 0 0 1944.11 75.09 -6 0 0 2027.00 75.39 -6 0 0 2007.20 75.39 6 0 0 1981.20 74.89 -6 0 0 2077.39 75.39 6 0 0 1957.90 74.59 7 0 0 0.40 2.10 7 0 0 -2.40 2.50 -7 0 0 -2.80 3.20 -7 0 0 -1.70 3.30 7 0 0 -0.90 2.90 7 0 0 -1.90 2.30 -7 0 0 -4.90 3.10 7 0 0 -2.10 3.10 -8 0 0 3.70 3.40 8 0 0 12.20 3.30 8 0 0 8.10 3.90 -8 0 0 18.40 4.20 -8 0 0 2.10 4.20 8 0 0 7.30 2.80 8 0 0 8.50 3.00 -9 0 0 -0.10 4.30 9 0 0 7.10 3.30 -9 0 0 2.80 3.60 9 0 0 0.40 2.60 9 0 0 6.40 4.10 -10 0 0 10.40 3.20 10 0 0 12.80 3.70 10 0 0 9.70 2.60 -10 0 0 9.90 2.90 0 1 0 3.60 0.40 -1 -1 0 499.95 19.40 -1 -1 0 534.55 19.50 1 -1 0 484.35 19.40 1 -1 0 535.05 19.90 1 1 0 547.85 19.60 1 1 0 527.35 19.70 -1 1 0 543.05 19.50 -1 1 0 531.25 20.00 -3 -1 0 559.34 22.40 3 -1 0 584.04 21.60 3 -1 0 567.24 22.80 -3 -1 0 556.44 21.50 -3 1 0 567.04 23.00 -3 1 0 561.14 21.70 3 1 0 570.44 22.50 3 1 0 562.34 21.90 4 -1 0 2131.19 79.59 -4 -1 0 2214.68 81.19 4 -1 0 2210.98 81.69 -4 -1 0 2070.09 79.49 -4 1 0 2102.89 79.69 4 1 0 2107.69 79.99 4 1 0 2169.18 81.19 -4 1 0 2164.78 81.79 -5 -1 0 234.58 9.70 5 -1 0 233.08 9.90 5 -1 0 204.58 9.90 -5 -1 0 237.88 11.70 5 -1 0 201.68 9.80 5 -1 0 215.68 11.10 5 -1 0 190.58 10.30 -5 -1 0 202.08 10.70 -5 -1 0 217.58 10.50 5 1 0 198.78 12.90 -5 1 0 212.78 11.20 5 1 0 216.98 9.90 5 1 0 231.78 10.40 -5 1 0 212.78 13.40 -5 1 0 211.38 10.00 5 1 0 216.98 10.00 -5 1 0 215.48 10.90 -6 -1 0 268.77 12.50 6 -1 0 276.27 12.00 6 -1 0 238.98 11.50 6 -1 0 272.47 12.20 -6 -1 0 280.77 12.90 6 -1 0 281.27 12.60 -6 -1 0 282.07 13.10 6 -1 0 297.97 12.60 -6 -1 0 287.77 12.40 -6 1 0 271.07 13.70 -6 1 0 294.57 13.50 -6 1 0 278.17 13.30 -6 1 0 268.37 12.90 6 1 0 281.47 13.20 6 1 0 275.07 12.10 6 1 0 285.27 12.30 6 1 0 280.87 12.90 7 -1 0 6.90 2.60 7 -1 0 0.80 2.70 -7 -1 0 0.10 3.10 -7 -1 0 -1.50 3.10 -7 -1 0 0.90 3.00 7 -1 0 3.50 3.20 -7 -1 0 -0.70 3.70 7 -1 0 5.80 2.60 -7 1 0 6.70 3.70 7 1 0 -0.90 3.40 7 1 0 3.60 2.20 -7 1 0 -2.90 3.40 -7 1 0 -3.80 3.40 -7 1 0 2.90 3.50 7 1 0 1.20 2.60 7 1 0 2.60 3.20 8 -1 0 0.70 2.90 -8 -1 0 2.20 4.00 -8 -1 0 -3.20 3.10 8 -1 0 -1.40 3.40 8 -1 0 0.30 2.80 8 -1 0 4.40 2.70 -8 -1 0 0.10 4.00 8 1 0 -4.30 2.50 -8 1 0 -2.10 3.80 8 1 0 -0.50 3.20 -8 1 0 -4.70 4.40 8 1 0 -3.90 3.80 -9 -1 0 42.70 6.60 9 -1 0 44.30 5.90 9 -1 0 43.90 5.70 -9 -1 0 50.89 6.30 9 1 0 59.29 7.00 9 1 0 51.49 7.50 9 1 0 36.40 5.50 -9 1 0 30.80 5.40 -9 1 0 41.70 7.10 10 -1 0 101.19 6.20 10 -1 0 104.99 6.90 -10 -1 0 95.69 6.60 -10 -1 0 87.49 9.10 -10 1 0 94.69 6.30 10 1 0 103.09 6.20 -10 1 0 83.39 7.10 1 -2 0 1025.00 37.90 1 2 0 1017.30 37.30 -1 2 0 989.30 37.90 -1 2 0 1012.10 37.20 2 -2 0 96.09 5.20 2 -2 0 93.49 3.80 -2 -2 0 94.09 3.80 2 -2 0 102.19 3.80 2 -2 0 87.39 3.80 2 2 0 89.89 4.50 -2 2 0 94.29 5.20 2 2 0 91.39 4.50 -2 2 0 93.89 4.30 3 -2 0 16.40 2.40 3 -2 0 12.10 1.60 3 -2 0 9.20 1.80 -3 -2 0 11.60 1.70 -3 2 0 14.60 2.90 3 2 0 15.10 2.80 -3 2 0 14.10 2.40 -4 -2 0 393.56 15.60 4 -2 0 437.96 16.00 4 -2 0 407.56 15.70 4 -2 0 377.76 19.30 4 2 0 394.76 16.50 4 2 0 396.76 17.40 -4 2 0 399.86 18.60 -4 2 0 390.46 16.20 -5 -2 0 702.63 28.20 -5 -2 0 711.63 28.30 -5 -2 0 738.43 27.60 5 -2 0 767.02 28.70 5 -2 0 696.23 28.00 5 -2 0 683.63 27.70 -5 -2 0 718.33 28.20 5 -2 0 760.72 27.70 5 -2 0 702.43 28.00 -5 2 0 744.63 29.00 5 2 0 715.23 28.70 -5 2 0 714.63 32.20 5 2 0 725.73 31.00 -5 2 0 711.13 28.60 -5 2 0 737.23 28.40 5 2 0 719.73 28.10 5 2 0 715.03 28.00 6 -2 0 1133.69 43.80 6 -2 0 1141.29 43.60 6 -2 0 1205.58 43.40 6 -2 0 1093.89 43.30 -6 -2 0 1178.68 43.90 -6 -2 0 1136.79 43.90 -6 -2 0 1165.18 43.40 6 2 0 1186.78 45.00 6 2 0 1133.89 43.60 -6 2 0 1179.58 44.70 6 2 0 1104.19 43.90 -6 2 0 1158.08 44.50 6 2 0 1161.58 43.70 -6 2 0 1072.59 44.60 -6 2 0 1168.38 44.40 -7 -2 0 11.00 3.80 7 -2 0 11.00 3.40 7 -2 0 10.00 2.60 -7 -2 0 9.80 3.20 7 -2 0 10.90 2.70 -7 -2 0 10.40 2.90 7 2 0 17.60 3.00 7 2 0 10.40 3.10 7 2 0 12.30 2.60 7 2 0 14.60 3.90 -7 2 0 7.10 3.80 -7 2 0 11.80 4.60 7 2 0 14.40 4.40 -8 -2 0 11.70 3.40 8 -2 0 16.40 3.50 8 -2 0 12.00 3.30 8 -2 0 11.60 2.90 -8 -2 0 9.70 3.80 8 2 0 8.70 2.70 8 2 0 11.40 5.00 8 2 0 9.70 2.70 -8 2 0 19.00 4.50 -8 2 0 11.80 5.10 8 2 0 8.70 3.10 -8 2 0 10.50 4.20 -8 2 0 2.10 3.70 8 2 0 17.20 4.20 9 -2 0 21.50 3.30 9 -2 0 24.10 3.60 -9 -2 0 30.60 6.00 -9 -2 0 30.60 5.90 -9 2 0 24.30 4.70 9 2 0 29.40 5.60 -9 2 0 21.20 3.60 -9 2 0 17.60 4.30 9 2 0 18.80 3.10 10 -2 0 18.20 4.20 -10 -2 0 14.10 3.00 10 -2 0 12.60 2.80 10 -2 0 18.20 3.30 -10 2 0 15.90 3.10 -10 2 0 9.10 4.70 10 2 0 10.30 2.40 0 3 0 29.00 2.00 1 -3 0 1045.30 38.60 -1 3 0 1047.60 37.70 -1 3 0 1038.90 38.70 -1 3 0 1001.70 37.80 1 3 0 985.60 37.70 2 -3 0 575.34 22.50 -2 3 0 580.54 22.80 2 3 0 575.54 21.70 -2 3 0 533.45 21.60 -3 3 0 581.14 22.60 3 3 0 589.04 23.00 -4 -3 0 3034.70 113.09 -4 -3 0 3146.79 112.89 4 -3 0 3073.39 116.19 4 3 0 3038.50 114.39 -4 3 0 3080.29 114.09 -4 3 0 3094.09 116.69 -5 -3 0 1258.07 47.20 5 -3 0 1214.98 47.20 -5 -3 0 1225.08 47.40 5 -3 0 1167.38 47.60 5 -3 0 1227.78 48.40 5 -3 0 1220.08 47.10 -5 -3 0 1271.77 47.50 -5 -3 0 1347.77 46.30 5 3 0 1311.17 48.30 5 3 0 1234.68 47.20 5 3 0 1257.47 47.40 -5 3 0 1290.77 47.80 5 3 0 1204.08 49.80 -5 3 0 1231.18 48.10 -5 3 0 1251.67 47.80 6 -3 0 54.99 9.80 6 -3 0 63.49 8.50 -6 -3 0 59.19 7.10 -6 -3 0 81.89 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8.10 9 4 0 89.09 6.70 9 4 0 101.99 6.70 -9 4 0 101.19 7.90 -9 4 0 96.39 8.00 10 -4 0 59.99 5.10 -10 -4 0 57.29 4.60 10 -4 0 48.00 5.20 -10 4 0 49.80 4.80 10 4 0 52.89 4.50 0 5 0 0.80 1.40 0 5 0 2.50 1.50 -1 5 0 1304.87 47.30 1 5 0 1303.37 45.90 -1 5 0 1088.09 45.80 2 5 0 204.28 8.10 -2 5 0 214.88 9.30 2 5 0 198.08 10.00 2 5 0 211.98 8.30 -3 -5 0 138.89 8.10 -3 -5 0 142.39 8.50 3 -5 0 147.89 10.20 3 -5 0 146.59 8.80 3 -5 0 150.68 8.60 3 5 0 154.88 6.50 -3 5 0 158.88 8.20 -3 5 0 149.59 10.90 -4 -5 0 1147.79 45.10 -4 -5 0 1138.79 44.40 -4 -5 0 1190.68 45.10 4 -5 0 1217.48 45.80 4 -5 0 1173.98 44.80 4 -5 0 1187.98 45.80 4 -5 0 1191.48 45.30 4 5 0 1152.88 46.00 -4 5 0 1209.68 45.50 4 5 0 1223.48 46.30 -5 -5 0 62.99 5.10 -5 -5 0 76.09 7.70 5 -5 0 70.39 8.20 -5 -5 0 64.89 6.60 5 -5 0 67.29 6.90 5 -5 0 74.69 5.90 5 5 0 66.79 8.70 5 5 0 89.39 8.80 -5 5 0 77.29 8.60 -5 5 0 76.59 8.00 -5 5 0 94.59 9.50 -6 -5 0 624.34 24.90 6 -5 0 621.64 24.40 6 -5 0 588.94 24.90 -6 -5 0 616.84 24.00 -6 -5 0 572.74 24.90 -6 -5 0 615.14 24.70 6 -5 0 630.14 25.90 6 5 0 564.54 27.10 6 5 0 614.24 24.20 -6 5 0 608.74 25.80 -6 5 0 579.94 26.40 6 5 0 630.14 24.50 -6 5 0 602.34 25.30 -7 -5 0 5.50 3.30 -7 -5 0 0.80 7.20 -7 -5 0 7.70 2.90 7 -5 0 6.40 3.30 7 -5 0 4.90 4.00 7 -5 0 3.80 4.50 -7 5 0 1.40 4.00 7 5 0 4.60 3.10 7 5 0 8.00 6.40 7 5 0 6.10 2.60 -7 5 0 2.10 4.10 -7 5 0 6.10 6.20 7 5 0 9.70 3.00 8 -5 0 92.39 11.50 -8 -5 0 100.89 8.90 8 -5 0 110.29 8.10 -8 -5 0 96.49 11.30 8 5 0 83.09 10.10 -8 5 0 95.29 9.80 8 5 0 105.89 7.60 9 -5 0 77.79 6.00 -9 -5 0 70.49 5.50 9 -5 0 67.89 5.80 -9 -5 0 75.39 7.20 9 5 0 75.89 5.60 -9 5 0 78.09 7.10 9 5 0 68.49 5.70 -9 5 0 73.49 7.00 10 -5 0 2.40 2.50 -10 -5 0 1.30 1.90 10 -5 0 3.10 2.20 10 5 0 2.40 1.90 -10 5 0 -0.10 2.40 0 6 0 536.05 21.60 0 6 0 549.65 22.10 -1 6 0 4008.90 144.89 -1 6 0 3949.41 146.49 1 6 0 3851.71 144.59 -2 -6 0 142.49 8.30 -2 -6 0 123.69 7.70 2 -6 0 148.89 9.10 2 -6 0 145.09 8.00 2 -6 0 141.69 8.50 -2 6 0 148.09 10.00 3 -6 0 8.70 3.40 3 -6 0 7.50 3.10 -3 -6 0 5.30 2.50 -3 -6 0 1.90 2.50 -3 -6 0 15.10 3.30 -3 -6 0 8.60 3.20 -3 6 0 0.00 5.60 4 -6 0 0.60 2.50 4 -6 0 -5.20 3.50 -4 -6 0 -0.60 2.00 -4 -6 0 -4.20 2.80 -4 -6 0 -0.80 3.00 4 -6 0 4.10 3.80 4 -6 0 -0.80 2.90 -4 -6 0 -3.20 2.80 -5 -6 0 70.69 7.50 5 -6 0 69.49 8.20 -5 -6 0 63.99 6.80 5 -6 0 70.89 6.00 -5 -6 0 77.09 7.10 5 -6 0 82.89 11.10 -5 -6 0 73.49 5.20 5 -6 0 59.59 7.00 5 6 0 71.89 7.90 5 6 0 57.59 7.90 -6 -6 0 6.30 3.50 6 -6 0 13.50 3.20 -6 -6 0 12.70 3.80 -6 -6 0 7.70 2.60 6 -6 0 7.60 3.50 6 -6 0 9.10 4.80 -6 -6 0 4.70 3.40 6 6 0 12.30 3.30 6 6 0 12.50 3.10 -6 6 0 16.10 4.70 -6 6 0 11.50 4.50 -7 -6 0 4.10 4.40 7 -6 0 5.30 4.80 7 -6 0 2.60 2.90 -7 -6 0 1.90 2.70 -7 -6 0 1.80 3.30 7 -6 0 -0.40 3.70 -7 6 0 0.90 3.70 7 6 0 4.00 2.80 7 6 0 -0.30 2.70 -7 6 0 3.70 3.90 7 6 0 3.30 3.20 8 -6 0 299.77 13.50 8 -6 0 258.47 14.30 -8 -6 0 294.97 12.70 -8 -6 0 305.57 14.00 8 -6 0 292.57 15.70 8 6 0 299.67 13.10 8 6 0 310.27 13.10 8 6 0 285.07 13.20 -8 6 0 309.97 14.70 -8 6 0 293.27 14.10 9 -6 0 9.50 2.70 -9 -6 0 8.80 2.30 -9 -6 0 6.40 3.10 9 -6 0 8.40 2.80 -9 6 0 9.20 3.30 9 6 0 10.10 2.40 -9 6 0 9.30 3.40 0 -7 0 -2.40 3.20 0 -7 0 0.70 2.50 0 -7 0 7.50 3.80 0 -7 0 2.40 2.60 0 7 0 1.50 3.50 1 -7 0 37.50 5.90 -1 -7 0 30.60 5.10 1 -7 0 27.00 4.90 1 -7 0 23.60 3.90 -1 -7 0 34.20 5.10 1 -7 0 22.10 3.90 1 -7 0 38.90 5.90 -1 -7 0 31.20 4.50 1 7 0 37.40 7.80 -2 -7 0 9.70 2.70 2 -7 0 15.80 3.00 2 -7 0 15.30 3.60 -2 -7 0 17.60 3.40 -2 -7 0 16.90 4.10 -2 -7 0 16.80 4.80 2 -7 0 19.00 3.60 2 7 0 17.10 8.80 -2 7 0 15.10 8.20 3 -7 0 926.11 35.50 -3 -7 0 901.11 35.20 -3 -7 0 905.11 35.20 3 -7 0 894.91 35.90 -3 -7 0 917.71 35.40 3 -7 0 942.11 35.00 3 -7 0 860.51 35.00 3 -7 0 899.11 35.30 -4 -7 0 59.19 6.90 4 -7 0 54.39 6.30 -4 -7 0 58.39 6.40 4 -7 0 64.59 5.90 4 -7 0 72.19 7.50 -4 -7 0 64.49 7.20 4 -7 0 48.10 9.70 4 -7 0 63.19 6.90 5 -7 0 462.65 20.90 5 -7 0 474.75 19.60 5 -7 0 472.75 21.20 -5 -7 0 462.15 19.90 -5 -7 0 461.45 18.70 5 -7 0 503.65 19.80 5 -7 0 457.85 20.40 -5 -7 0 486.15 20.30 -5 -7 0 496.65 20.20 5 7 0 463.25 20.10 5 7 0 447.36 19.60 -5 7 0 460.25 21.50 -5 7 0 478.25 21.90 -6 -7 0 2.60 3.30 -6 -7 0 1.80 2.50 -6 -7 0 0.60 3.10 6 -7 0 -2.10 4.30 -6 -7 0 -0.10 3.40 6 -7 0 8.00 3.40 6 -7 0 -0.70 3.10 6 7 0 8.40 3.40 6 7 0 4.20 2.80 6 7 0 2.60 2.80 -6 7 0 8.80 4.40 -6 7 0 5.70 4.20 -7 -7 0 8.70 3.70 7 -7 0 12.40 4.60 7 -7 0 6.70 4.50 -7 -7 0 10.40 3.70 7 -7 0 3.10 3.00 -7 7 0 9.80 4.40 7 7 0 7.70 3.40 7 7 0 2.90 2.90 8 -7 0 21.30 3.40 -8 -7 0 22.00 3.60 8 -7 0 22.40 3.40 8 -7 0 25.30 4.50 8 -7 0 25.60 5.00 -8 -7 0 24.70 3.80 8 7 0 19.00 3.00 -8 7 0 18.10 3.80 8 7 0 26.70 4.60 -8 7 0 23.50 4.40 -9 -7 0 -2.70 2.70 9 -7 0 -2.30 2.30 9 -7 0 0.50 2.10 -9 7 0 -1.70 2.60 -9 7 0 -1.70 2.80 9 7 0 1.30 2.40 0 -8 0 52.89 6.20 0 -8 0 53.29 7.60 0 -8 0 64.59 7.10 1 -8 0 38.10 6.20 -1 -8 0 31.10 5.50 1 -8 0 32.90 6.20 -1 -8 0 39.60 6.90 1 -8 0 39.00 6.60 1 -8 0 40.20 6.50 -1 -8 0 31.40 5.60 1 -8 0 30.70 5.40 -2 -8 0 90.79 7.00 -2 -8 0 102.39 7.80 2 -8 0 105.29 8.10 -2 -8 0 87.89 7.20 2 -8 0 80.09 7.30 2 -8 0 93.59 7.80 3 -8 0 43.20 6.50 3 -8 0 35.40 6.60 3 -8 0 27.80 4.70 3 -8 0 32.80 5.60 -3 -8 0 43.90 6.00 4 -8 0 434.36 19.90 -4 -8 0 418.96 19.20 4 -8 0 465.45 20.40 -4 -8 0 466.25 19.30 -4 -8 0 455.25 19.60 4 -8 0 468.05 19.00 4 -8 0 440.46 19.00 4 -8 0 456.05 19.70 5 -8 0 249.28 13.40 5 -8 0 260.67 12.30 -5 -8 0 248.68 12.70 -5 -8 0 256.77 12.80 -5 -8 0 221.08 12.00 5 -8 0 278.77 13.40 5 -8 0 261.67 13.90 5 -8 0 260.17 12.40 -5 -8 0 266.87 13.00 5 8 0 238.18 12.50 -5 8 0 266.57 15.60 -6 -8 0 69.79 7.20 6 -8 0 62.79 6.50 6 -8 0 75.59 7.50 -6 -8 0 78.19 7.70 6 -8 0 55.99 6.40 -6 8 0 48.70 9.10 6 8 0 52.09 6.20 -6 8 0 61.89 9.10 7 -8 0 349.17 16.20 7 -8 0 351.36 15.20 7 -8 0 337.27 15.10 -7 -8 0 344.77 15.60 7 -8 0 350.06 16.40 -7 -8 0 361.36 15.60 -7 8 0 353.96 16.30 -7 8 0 368.06 16.80 7 8 0 379.66 15.10 7 8 0 329.67 15.00 8 -8 0 34.30 4.60 8 -8 0 34.10 5.90 8 -8 0 24.30 4.30 8 -8 0 28.40 4.50 -8 -8 0 25.60 3.30 -8 8 0 23.90 4.10 -8 8 0 22.30 3.80 0 -9 0 -2.70 3.80 0 -9 0 -0.10 3.00 0 -9 0 -5.90 4.60 1 -9 0 767.72 31.40 -1 -9 0 819.72 30.90 1 -9 0 760.02 30.50 1 -9 0 808.92 30.80 -1 -9 0 790.62 31.10 1 -9 0 781.02 31.70 -1 -9 0 774.82 31.60 1 -9 0 740.73 30.90 -2 -9 0 1726.43 64.19 -2 -9 0 1595.64 63.99 2 -9 0 1724.93 65.09 2 -9 0 1703.23 64.19 -2 -9 0 1710.03 64.39 -2 -9 0 1673.33 64.49 2 -9 0 1674.73 63.89 2 -9 0 1773.22 64.69 -3 -9 0 662.53 26.30 -3 -9 0 604.04 26.10 3 -9 0 627.74 26.40 3 -9 0 649.74 26.00 3 -9 0 639.04 27.20 3 -9 0 678.33 26.80 -3 -9 0 658.13 26.50 4 -9 0 320.57 15.10 4 -9 0 294.87 15.10 -4 -9 0 281.17 14.40 -4 -9 0 333.77 14.60 4 -9 0 308.97 14.30 4 -9 0 308.17 15.60 -4 -9 0 309.77 14.90 -5 -9 0 4.40 3.20 5 -9 0 0.30 3.40 5 -9 0 1.70 3.10 5 -9 0 9.20 5.50 -5 -9 0 -2.90 3.40 -5 -9 0 1.80 3.10 5 -9 0 2.20 3.60 -5 9 0 3.00 9.00 -6 -9 0 6.00 2.90 6 -9 0 1.00 2.60 6 -9 0 8.30 3.60 6 -9 0 5.00 3.70 -6 -9 0 0.80 3.00 -6 9 0 5.80 4.60 -7 -9 0 2.50 2.50 7 -9 0 2.60 3.50 7 -9 0 4.70 2.50 7 -9 0 4.70 3.30 -7 -9 0 6.00 3.20 -7 9 0 3.80 3.80 -8 -9 0 25.60 4.30 -8 9 0 30.90 5.70 0 -10 0 0.10 2.80 0 -10 0 -1.40 2.80 0 -10 0 8.20 4.20 1 -10 0 225.98 12.50 1 -10 0 227.28 12.60 -1 -10 0 222.78 11.50 1 -10 0 234.18 11.70 -1 -10 0 231.18 11.70 1 -10 0 216.08 11.60 -1 -10 0 224.48 12.90 -2 -10 0 2522.15 93.29 2 -10 0 2483.85 93.09 2 -10 0 2400.66 92.49 2 -10 0 2579.04 93.59 -2 -10 0 2493.05 92.99 -2 -10 0 2399.96 93.29 2 -10 0 2534.45 93.89 3 -10 0 23.40 3.80 3 -10 0 21.70 4.10 -3 -10 0 24.30 7.00 3 -10 0 15.10 4.50 3 -10 0 23.00 4.50 -3 -10 0 31.10 6.20 -3 -10 0 16.10 3.40 4 -10 0 93.99 8.20 4 -10 0 83.99 8.00 -4 -10 0 71.29 6.90 -4 -10 0 83.89 8.10 -4 -10 0 89.09 7.20 4 -10 0 86.89 9.00 5 -10 0 2.00 3.20 5 -10 0 1.30 2.70 -5 -10 0 0.40 2.90 5 -10 0 2.50 3.90 -5 -10 0 3.90 3.00 -5 10 0 2.80 5.70 5 10 0 -1.30 3.20 6 -10 0 75.29 7.20 6 -10 0 68.29 5.60 -6 -10 0 75.79 6.20 6 -10 0 69.09 7.10 -6 -10 0 76.79 6.10 -6 10 0 83.99 9.60 -7 -10 0 26.10 4.00 7 -10 0 18.70 3.40 -7 -10 0 17.20 3.10 7 -10 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234.18 10.70 3 -3 -9 242.38 11.30 -3 -3 9 243.18 10.60 3 -3 -9 235.28 14.50 3 -3 -9 268.67 12.10 3 3 -9 239.08 11.90 -3 3 9 250.57 11.30 -3 3 9 233.68 15.20 -2 -3 9 581.94 25.40 2 -3 -9 609.44 25.60 -2 -3 9 569.64 22.90 -2 -3 9 594.54 23.00 2 -3 -9 602.24 25.70 2 3 -9 609.94 24.20 -2 3 9 584.24 23.30 2 3 -9 630.64 25.60 -2 3 9 559.94 25.70 -2 3 9 582.54 24.90 1 -3 -9 2042.30 76.69 -1 -3 9 1995.70 74.69 -1 -3 9 1989.80 74.39 -1 3 9 1959.60 74.49 1 3 -9 2012.40 75.19 -1 3 9 2028.90 76.89 1 3 -9 2009.50 76.19 -1 3 9 2020.80 76.19 0 -3 9 5938.91 217.08 0 -3 -9 5984.20 218.28 0 3 9 5835.02 216.08 0 3 9 6041.40 217.88 0 3 -9 5824.72 217.48 0 3 -9 5665.93 216.38 1 -3 9 2065.89 76.39 1 -3 9 1958.20 74.49 1 3 9 2031.60 74.89 1 3 9 1993.90 76.69 -1 3 -9 2012.60 74.99 -1 3 -9 2017.70 75.99 -2 -3 -9 601.94 23.80 2 -3 9 586.34 25.80 -2 -3 -9 529.15 25.00 2 -3 9 601.64 22.70 2 -3 9 626.74 25.50 2 3 9 579.94 25.50 -2 3 -9 598.84 23.30 -2 3 -9 618.64 24.20 2 3 9 580.24 23.30 3 -3 9 222.08 11.90 -3 -3 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77.89 5.80 3 -2 23 15.20 4.60 3 -2 23 9.70 2.70 3 2 23 10.20 2.60 3 2 23 10.30 2.80 -4 -2 -23 37.70 4.30 -4 -2 -23 42.90 5.60 4 -2 23 29.70 7.40 4 -2 23 28.70 4.00 -4 2 -23 33.30 5.10 4 2 23 38.70 6.20 4 2 23 34.70 5.30 4 2 23 31.60 4.40 5 2 23 5.20 2.10 4 -3 -23 5.60 2.80 -4 -3 23 2.70 2.80 -4 3 23 3.40 3.00 -4 3 23 4.60 3.40 4 3 -23 7.40 2.70 -3 -3 23 43.60 7.40 3 -3 -23 57.69 5.60 -3 -3 23 47.20 5.90 -3 3 23 58.49 4.60 3 3 -23 48.70 6.60 3 3 -23 57.79 5.30 -3 3 23 60.89 5.00 -2 -3 23 10.00 2.80 2 -3 -23 15.10 3.20 -2 -3 23 18.30 3.80 2 3 -23 14.80 3.20 -2 3 23 16.50 2.90 -2 3 23 14.10 2.80 2 3 -23 14.90 3.20 -1 -3 23 63.89 5.70 1 -3 -23 80.59 6.90 -1 -3 23 67.99 7.00 1 3 -23 72.69 7.00 1 3 -23 71.69 6.50 -1 3 23 83.49 6.20 -1 3 23 79.79 6.00 0 -3 -23 31.30 6.20 0 -3 23 35.10 5.20 0 -3 -23 41.00 7.80 0 3 23 29.60 5.10 0 3 -23 32.90 6.70 0 3 23 38.90 5.30 -1 -3 -23 71.89 7.10 1 -3 23 66.49 7.40 1 -3 23 70.39 5.70 -1 3 -23 84.29 14.00 1 3 23 76.69 5.80 -1 3 -23 63.29 6.30 1 3 23 74.79 6.00 -2 -3 -23 14.30 3.50 2 -3 23 17.30 4.20 2 -3 23 15.40 3.00 2 3 23 15.10 3.00 -2 3 -23 28.80 5.60 2 3 23 13.70 2.70 3 -3 23 61.09 6.40 -3 -3 -23 59.49 6.40 3 -3 23 50.79 6.30 -3 -3 -23 56.09 4.80 3 3 23 63.29 5.20 -3 3 -23 63.89 9.00 3 3 23 53.49 5.20 -4 -3 -23 10.70 2.20 -4 -3 -23 7.90 2.70 -4 3 -23 8.20 3.10 4 3 23 7.40 3.20 4 3 23 3.40 2.40 4 3 23 4.90 2.70 -4 -4 23 23.20 3.60 4 4 -23 17.00 2.70 -4 4 23 26.30 3.70 -4 4 23 26.30 3.40 -3 -4 23 17.20 2.80 -3 4 23 19.40 4.20 -3 4 23 19.60 3.40 3 4 -23 15.70 3.90 3 4 -23 13.90 3.00 -2 -4 23 2.00 2.70 2 -4 -23 1.70 2.50 -2 4 23 7.70 2.60 -2 4 23 4.70 2.40 2 4 -23 1.40 3.00 2 4 -23 4.70 2.70 -1 -4 23 -0.70 2.80 1 -4 -23 0.50 2.80 -1 4 23 6.40 2.70 1 4 -23 9.40 4.10 -1 4 23 4.40 2.40 1 4 -23 3.60 2.70 0 -4 -23 54.79 7.60 0 -4 23 68.59 6.20 0 -4 -23 52.59 6.30 0 4 23 59.49 5.40 0 4 23 71.89 5.60 0 4 -23 53.39 5.80 -1 -4 -23 -2.50 3.60 1 -4 23 4.50 3.00 1 4 23 4.00 2.40 1 4 23 4.00 2.60 -1 4 -23 4.10 2.90 2 -4 23 6.10 3.20 -2 -4 -23 4.20 3.30 2 4 23 2.60 2.40 2 4 23 0.80 2.50 -2 4 -23 2.80 2.90 3 -4 23 15.80 3.20 3 4 23 23.20 4.40 3 4 23 17.40 3.20 -3 4 -23 17.20 3.40 -4 -4 -23 25.90 4.40 4 4 23 20.20 3.90 -4 4 -23 17.70 3.90 4 4 23 19.80 3.20 -3 -5 23 2.40 2.40 3 5 -23 5.80 2.30 3 5 -23 8.40 3.40 -3 5 23 6.20 3.70 -3 5 23 3.60 2.60 -2 -5 23 3.40 2.40 -2 -5 23 2.40 3.10 -2 5 23 -0.30 2.20 2 5 -23 3.40 2.50 -2 5 23 -1.90 2.60 2 5 -23 2.70 4.60 -1 -5 23 1.00 2.50 1 -5 -23 1.30 4.10 -1 -5 23 -2.00 3.40 -1 5 23 1.60 2.30 -1 5 23 4.50 3.60 1 5 -23 3.70 2.50 0 -5 -23 1.70 4.50 0 -5 23 0.30 2.60 0 5 -23 3.20 2.60 0 5 23 5.30 2.40 1 -5 23 0.20 2.60 -1 -5 -23 6.10 3.80 1 5 23 2.60 2.40 -1 5 -23 1.60 2.60 1 5 23 -1.80 3.00 2 -5 23 0.20 2.60 -2 -5 -23 -0.50 3.20 2 5 23 4.40 2.20 2 5 23 4.20 2.70 -2 5 -23 7.60 3.00 -3 -5 -23 -2.20 2.70 3 5 23 1.70 3.70 -3 5 -23 5.90 2.60 3 5 23 0.30 3.40 3 5 23 2.90 2.60 -2 -6 23 -1.20 2.80 -2 -6 23 1.90 2.20 2 6 -23 3.90 2.20 -2 6 23 0.90 2.00 -1 -6 23 -4.20 3.60 -1 -6 23 0.60 2.60 1 -6 -23 -2.60 5.30 -1 6 23 2.70 3.00 1 6 -23 -0.10 2.50 0 -6 23 6.10 2.50 0 -6 -23 8.70 2.80 0 6 -23 4.70 3.60 0 6 23 7.30 3.30 1 -6 23 2.10 2.80 -1 6 -23 1.40 3.30 1 6 23 -0.80 3.20 2 -6 23 0.20 2.10 -2 6 -23 2.10 2.70 2 6 23 -1.00 2.10 4 0 -24 -0.80 3.60 -4 0 24 4.50 2.20 3 0 -24 -1.50 2.40 -3 0 24 0.00 2.10 -2 0 24 7.50 2.40 2 0 -24 3.10 2.70 -1 0 24 5.90 2.40 1 0 -24 -0.70 2.80 0 0 24 38.90 5.00 0 0 24 43.00 4.80 0 0 -24 31.60 6.10 -1 0 -24 1.20 3.30 1 0 24 -0.40 2.30 2 0 24 6.40 2.40 2 0 24 8.00 3.90 3 0 24 -2.30 2.10 3 0 24 -2.20 4.70 4 0 24 1.80 3.00 4 0 24 5.40 2.80 -4 -1 24 6.50 2.00 4 -1 -24 0.40 2.30 4 1 -24 4.60 3.00 -4 1 24 2.10 2.20 3 -1 -24 -1.40 2.50 -3 -1 24 -3.80 5.50 -3 -1 24 1.70 2.00 -3 1 24 2.30 2.20 3 1 -24 1.40 2.40 -2 -1 24 -5.80 5.10 2 -1 -24 0.60 2.70 -2 -1 24 0.50 2.30 -2 1 24 -0.80 2.20 -2 1 24 -0.30 2.50 2 1 -24 0.20 2.70 1 -1 -24 43.90 5.80 -1 -1 24 49.10 4.70 -1 -1 24 44.80 7.50 -1 1 24 48.60 5.10 -1 1 24 44.10 4.80 1 1 -24 39.60 5.80 0 -1 24 4.80 5.40 0 -1 -24 0.60 3.00 0 -1 24 5.30 2.40 0 1 24 3.30 2.50 0 1 24 5.00 2.50 1 -1 24 47.50 7.70 1 -1 24 43.70 4.80 -1 -1 -24 37.00 6.20 -1 1 -24 36.20 6.40 1 1 24 38.40 4.90 1 1 24 34.70 4.70 2 -1 24 -0.90 6.20 2 -1 24 7.90 4.70 2 -1 24 0.20 2.40 2 1 24 0.50 2.30 2 1 24 -2.70 2.30 3 -1 24 1.10 2.30 -3 -1 -24 -2.60 2.40 3 -1 24 -6.70 3.90 3 1 24 1.40 2.30 3 1 24 -1.00 3.10 4 -1 24 4.60 2.20 -4 -1 -24 1.40 3.10 -4 -1 -24 2.00 2.40 4 1 24 3.50 2.70 4 1 24 4.30 1.90 -4 1 -24 3.20 2.40 4 -2 -24 3.00 2.30 -4 2 24 2.70 1.90 4 2 -24 5.00 2.30 3 -2 -24 6.10 2.60 -3 -2 24 3.60 2.60 -3 -2 24 4.10 3.80 3 2 -24 5.10 2.60 -3 2 24 4.50 2.20 -3 2 24 3.70 3.50 -2 -2 24 28.90 5.50 -2 -2 24 29.90 4.10 -2 2 24 31.60 4.10 2 2 -24 33.20 4.90 -2 2 24 23.40 4.40 -1 -2 24 9.70 2.50 1 -2 -24 12.10 3.20 -1 -2 24 7.50 4.00 -1 2 24 8.10 2.50 1 2 -24 10.70 3.20 -1 2 24 9.50 2.60 0 -2 24 6.00 4.00 0 -2 -24 9.10 3.20 0 2 -24 8.50 3.60 1 -2 24 6.20 2.50 1 -2 24 13.50 4.60 -1 -2 -24 7.60 3.10 1 2 24 8.60 2.50 -1 2 -24 10.80 6.00 1 2 24 9.40 2.70 2 -2 24 26.70 4.30 2 -2 24 25.10 5.70 2 2 24 27.20 4.50 2 2 24 32.80 4.30 -3 -2 -24 4.10 2.50 3 -2 24 4.20 2.50 -3 -2 -24 2.30 2.80 3 2 24 6.60 3.10 3 2 24 3.50 2.60 3 2 24 2.90 2.20 -4 -2 -24 0.40 2.60 -4 -2 -24 -0.50 1.90 4 2 24 2.50 2.30 4 2 24 -2.70 1.90 -4 2 -24 3.00 2.80 3 -3 -24 19.00 3.10 3 3 -24 22.70 4.10 -3 3 24 18.40 3.30 -3 3 24 18.70 3.20 -2 -3 24 18.20 3.10 2 -3 -24 23.90 4.80 -2 -3 24 25.20 4.10 -2 3 24 27.60 4.40 2 3 -24 32.60 5.50 -2 3 24 27.80 4.20 1 -3 -24 54.39 5.40 -1 -3 24 48.60 6.40 -1 -3 24 50.29 6.70 -1 3 24 46.80 4.90 1 3 -24 51.09 6.40 1 3 -24 43.50 6.60 -1 3 24 53.79 4.90 0 -3 24 31.10 6.30 0 -3 24 37.40 4.80 0 -3 -24 42.20 5.70 0 3 -24 48.30 6.90 0 3 24 46.60 5.00 0 3 24 40.40 4.90 0 3 -24 50.59 8.30 1 -3 24 40.00 6.10 1 -3 24 35.00 6.20 -1 -3 -24 46.00 6.60 -1 3 -24 50.89 6.60 1 3 24 51.39 5.10 1 3 24 46.80 5.00 2 -3 24 18.30 3.10 2 -3 24 25.50 4.20 -2 -3 -24 22.10 4.00 2 3 24 20.20 2.90 2 3 24 23.00 4.30 -3 -3 -24 11.50 3.90 3 3 24 13.30 2.80 3 3 24 14.80 3.60 -3 -4 24 -3.10 2.20 -3 4 24 -0.20 2.10 -2 -4 24 13.80 3.50 -2 -4 24 6.00 3.30 2 -4 -24 13.80 3.40 2 4 -24 7.70 3.40 2 4 -24 11.10 3.00 -2 4 24 13.00 2.60 -2 4 24 14.30 2.50 -1 -4 24 15.20 3.10 1 -4 -24 15.60 3.00 1 4 -24 19.20 3.30 -1 4 24 14.20 4.50 1 4 -24 21.50 7.30 -1 4 24 23.50 4.30 0 -4 24 4.00 2.80 0 4 -24 3.60 3.50 0 4 24 2.40 2.30 0 4 24 1.20 2.60 1 -4 24 19.30 3.40 -1 -4 -24 15.40 3.90 -1 4 -24 10.70 3.10 1 4 24 14.20 3.40 1 4 24 16.50 2.60 2 -4 24 7.40 3.40 -2 -4 -24 11.40 3.20 2 4 24 10.10 2.50 2 4 24 12.50 2.70 -2 4 -24 15.30 3.10 -3 -4 -24 0.20 2.40 3 4 24 0.80 2.20 3 4 24 -0.50 2.40 -1 -5 24 5.80 2.40 1 5 -24 -1.50 2.50 -1 5 24 1.90 2.70 -1 5 24 2.10 2.80 0 -5 24 5.90 3.00 0 5 24 5.40 2.80 0 5 -24 4.90 2.60 0 5 24 8.30 3.40 1 -5 24 0.00 2.60 1 5 24 -2.00 2.70 -1 5 -24 4.10 2.60 1 5 24 0.40 4.10 3 0 -25 -1.90 2.50 -3 0 25 -0.70 1.80 2 0 -25 -0.20 2.50 -2 0 25 7.10 2.20 -1 0 25 7.70 2.30 1 0 -25 3.00 2.80 0 0 25 4.80 2.30 0 0 -25 -3.90 2.90 1 0 25 4.40 2.30 -1 0 -25 2.20 3.50 2 0 25 5.40 2.20 2 0 25 -0.50 4.00 3 0 25 -2.00 1.90 3 -1 -25 4.10 2.20 3 1 -25 -0.60 1.90 -2 -1 25 8.30 2.50 2 -1 -25 5.80 2.60 2 1 -25 5.20 2.60 -2 1 25 8.30 2.30 1 -1 -25 38.00 5.10 -1 -1 25 32.30 3.90 -1 -1 25 28.90 8.00 -1 1 25 35.40 4.00 1 1 -25 38.10 5.50 0 -1 25 50.09 4.40 0 -1 -25 54.19 5.40 0 -1 25 47.90 7.10 0 1 25 60.89 4.50 0 1 25 54.19 5.70 0 1 -25 45.70 5.40 1 -1 25 32.60 4.10 -1 -1 -25 31.30 5.50 1 1 25 32.00 4.00 -1 1 -25 35.50 5.80 2 -1 25 4.50 3.10 2 1 25 4.50 2.20 2 1 25 7.60 3.40 -3 -1 -25 0.70 2.20 3 -1 25 -1.80 2.00 3 1 25 -1.20 2.80 3 1 25 -0.80 2.10 -3 1 -25 -2.90 2.40 2 -2 -25 1.80 2.80 -2 -2 25 -3.00 2.30 -2 -2 25 0.80 4.10 -2 2 25 0.20 2.30 2 2 -25 3.50 2.60 -2 2 25 -3.60 2.50 -1 -2 25 54.49 6.70 1 -2 -25 54.59 5.30 -1 -2 25 58.79 6.60 -1 2 25 59.89 7.00 -1 2 25 60.49 4.70 1 2 -25 56.39 6.10 0 -2 25 45.20 5.30 0 -2 25 39.40 7.20 0 -2 -25 46.80 5.20 0 2 25 48.30 7.00 0 2 25 51.39 4.70 0 2 -25 36.90 5.70 1 -2 25 63.29 7.40 -1 -2 -25 55.19 6.40 1 -2 25 52.09 4.90 1 2 25 41.80 6.30 1 2 25 50.39 4.60 -2 -2 -25 -2.40 2.40 2 -2 25 2.20 2.40 -2 -2 -25 2.30 3.00 2 2 25 3.60 2.50 2 2 25 -1.40 2.90 -2 -3 25 18.70 3.50 2 -3 -25 18.70 2.90 -2 3 25 23.60 3.80 -2 3 25 22.00 3.90 2 3 -25 24.30 5.00 1 -3 -25 53.09 5.90 -1 -3 25 45.70 5.50 1 3 -25 50.59 6.40 -1 3 25 51.59 5.00 -1 3 25 48.60 5.80 0 -3 -25 162.68 8.40 0 -3 25 150.28 8.90 0 3 25 189.98 9.40 0 3 25 160.88 9.30 1 -3 25 44.80 5.90 -1 -3 -25 43.00 6.60 1 3 25 45.70 5.10 1 3 25 45.60 5.00 -2 -3 -25 11.20 3.10 2 -3 25 16.50 3.40 2 3 25 19.90 3.90 2 3 25 16.10 3.00 2 3 25 13.70 2.40 -1 4 25 2.40 2.20 0 4 25 24.50 3.90 0 4 25 17.20 2.50 1 4 25 5.70 2.30 1 0 -26 -2.30 2.30 -1 0 26 -0.10 1.90 0 0 26 10.30 2.20 0 0 -26 10.60 2.90 1 0 26 0.50 2.00 -1 -1 26 18.80 3.50 1 -1 -26 18.50 4.00 -1 1 26 21.30 3.20 1 1 -26 17.10 2.90 0 -1 26 5.30 1.90 0 -1 -26 5.20 2.60 0 1 -26 6.30 3.20 0 1 26 6.10 2.00 1 -1 26 12.30 2.20 -1 -1 -26 21.30 4.30 1 1 26 13.80 2.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 85953 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn O1 O 0.4805(3) 0.84976(15) 0.59285(10) 0.0796(6) Uani 1 1 d . N1 N 0.5178(2) 0.73868(16) 0.60257(9) 0.0555(5) Uani 1 1 d . C1 C 0.4338(3) 0.6493(2) 0.56510(10) 0.0533(5) Uani 1 1 d . H1 H 0.4940 0.5804 0.5507 0.064 Uiso 1 1 calc R C2 C 0.3168(4) 0.6929(3) 0.52035(13) 0.0728(8) Uani 1 1 d . H2A H 0.3096 0.6531 0.4798 0.087 Uiso 1 1 calc R H2B H 0.2964 0.7784 0.5194 0.087 Uiso 1 1 calc R C3 C 0.2663(3) 0.6242(2) 0.57741(11) 0.0555(5) Uani 1 1 d . C4 C 0.2152(3) 0.4970(2) 0.56739(10) 0.0510(5) Uani 1 1 d . C5 C 0.0986(3) 0.4722(2) 0.52346(13) 0.0660(7) Uani 1 1 d . H5 H 0.0552 0.5349 0.5008 0.079 Uiso 1 1 calc R C6 C 0.0484(4) 0.3581(3) 0.51360(14) 0.0760(8) Uani 1 1 d . H6 H -0.0289 0.3444 0.4844 0.091 Uiso 1 1 calc R C7 C 0.1115(3) 0.2605(2) 0.54685(11) 0.0584(6) Uani 1 1 d . C8 C 0.0617(4) 0.1407(3) 0.53796(15) 0.0820(9) Uani 1 1 d . H8 H -0.0158 0.1243 0.5092 0.098 Uiso 1 1 calc R C9 C 0.1259(4) 0.0501(3) 0.57096(14) 0.0810(9) Uani 1 1 d . H9 H 0.0921 -0.0281 0.5646 0.097 Uiso 1 1 calc R C10 C 0.2420(4) 0.0720(2) 0.61435(13) 0.0716(7) Uani 1 1 d . H10 H 0.2856 0.0087 0.6365 0.086 Uiso 1 1 calc R C11 C 0.2914(3) 0.1857(2) 0.62428(12) 0.0642(6) Uani 1 1 d . H11 H 0.3687 0.1995 0.6535 0.077 Uiso 1 1 calc R C12 C 0.2276(3) 0.2838(2) 0.59099(10) 0.0500(5) Uani 1 1 d . C13 C 0.2762(3) 0.4036(2) 0.60040(11) 0.0532(5) Uani 1 1 d . H13 H 0.3521 0.4191 0.6300 0.064 Uiso 1 1 calc R C14 C 0.1869(4) 0.6899(3) 0.63039(17) 0.0849(9) Uani 1 1 d . H14A H 0.2269 0.7698 0.6335 0.127 Uiso 1 1 calc GR H14B H 0.2041 0.6481 0.6694 0.127 Uiso 1 1 calc GR H14C H 0.0793 0.6934 0.6220 0.127 Uiso 1 1 calc GR C15 C 0.6259(3) 0.7054(2) 0.64219(11) 0.0504(5) Uani 1 1 d . C16 C 0.7283(3) 0.7911(2) 0.67382(11) 0.0565(6) Uani 1 1 d . C17 C 0.7417(4) 0.9122(3) 0.65768(16) 0.0802(8) Uani 1 1 d . H17 H 0.6802 0.9451 0.6264 0.096 Uiso 1 1 calc R C18 C 0.8493(5) 0.9836(3) 0.6893(2) 0.1011(12) Uani 1 1 d . H18 H 0.8598 1.0639 0.6781 0.121 Uiso 1 1 calc R C19 C 0.9387(5) 0.9378(4) 0.7361(2) 0.0996(12) Uani 1 1 d . H19 H 1.0084 0.9869 0.7569 0.120 Uiso 1 1 calc R C20 C 0.9259(4) 0.8208(3) 0.75240(17) 0.0878(10) Uani 1 1 d . H20 H 0.9866 0.7897 0.7844 0.105 Uiso 1 1 calc R C21 C 0.8234(3) 0.7479(3) 0.72165(14) 0.0687(7) Uani 1 1 d . H21 H 0.8172 0.6675 0.7330 0.082 Uiso 1 1 calc R C22 C 0.6423(3) 0.57502(19) 0.65649(11) 0.0501(5) Uani 1 1 d . C23 C 0.7323(3) 0.5001(3) 0.62023(13) 0.0679(7) Uani 1 1 d . H23 H 0.7840 0.5305 0.5854 0.082 Uiso 1 1 calc R C24 C 0.7456(4) 0.3798(3) 0.63569(17) 0.0818(8) Uani 1 1 d . H24 H 0.8029 0.3289 0.6103 0.098 Uiso 1 1 calc R C25 C 0.6745(4) 0.3357(3) 0.68840(18) 0.0817(9) Uani 1 1 d . H25 H 0.6851 0.2552 0.6989 0.098 Uiso 1 1 calc R C26 C 0.5886(4) 0.4090(3) 0.72545(14) 0.0734(8) Uani 1 1 d . H26 H 0.5425 0.3789 0.7617 0.088 Uiso 1 1 calc R C27 C 0.5699(3) 0.5276(2) 0.70920(12) 0.0608(6) Uani 1 1 d . H27 H 0.5081 0.5766 0.7338 0.073 Uiso 1 1 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0923(14) 0.0389(8) 0.1074(15) 0.0129(9) -0.0031(12) 0.0037(9) N1 0.0625(11) 0.0400(9) 0.0642(11) 0.0061(8) 0.0095(9) 0.0004(8) C1 0.0620(13) 0.0470(11) 0.0509(11) 0.0044(9) 0.0015(10) 0.0036(10) C2 0.0877(19) 0.0618(15) 0.0688(15) 0.0229(13) -0.0153(14) -0.0039(14) C3 0.0580(13) 0.0454(11) 0.0630(13) 0.0081(10) 0.0024(11) 0.0059(10) C4 0.0511(11) 0.0509(12) 0.0511(11) 0.0022(9) 0.0030(10) 0.0042(10) C5 0.0667(15) 0.0631(15) 0.0681(15) 0.0116(12) -0.0135(12) 0.0067(13) C6 0.0797(18) 0.0732(18) 0.0750(17) 0.0048(14) -0.0275(15) -0.0055(15) C7 0.0656(15) 0.0563(13) 0.0532(12) -0.0039(10) -0.0021(11) -0.0042(11) C8 0.100(2) 0.0672(17) 0.0786(18) -0.0116(15) -0.0164(17) -0.0154(17) C9 0.111(2) 0.0545(15) 0.0779(18) -0.0078(13) 0.0005(18) -0.0165(16) C10 0.095(2) 0.0479(13) 0.0718(15) 0.0055(11) 0.0073(15) 0.0052(14) C11 0.0738(15) 0.0519(14) 0.0668(14) 0.0069(11) -0.0067(13) 0.0000(12) C12 0.0546(12) 0.0476(11) 0.0478(10) -0.0005(9) 0.0035(9) 0.0016(9) C13 0.0578(12) 0.0492(11) 0.0525(11) 0.0031(9) -0.0072(10) -0.0010(10) C14 0.0792(19) 0.0585(16) 0.117(2) -0.0182(16) 0.0266(18) 0.0026(14) C15 0.0546(12) 0.0426(10) 0.0540(11) -0.0008(9) 0.0086(10) -0.0023(9) C16 0.0599(13) 0.0479(11) 0.0618(13) -0.0091(10) 0.0197(11) -0.0076(11) C17 0.097(2) 0.0531(14) 0.0908(19) -0.0055(13) 0.0112(18) -0.0186(14) C18 0.110(3) 0.0638(19) 0.130(3) -0.020(2) 0.022(3) -0.031(2) C19 0.086(2) 0.097(3) 0.116(3) -0.034(2) 0.010(2) -0.035(2) C20 0.0734(19) 0.090(2) 0.100(2) -0.0215(18) -0.0011(17) -0.0225(17) C21 0.0596(14) 0.0681(16) 0.0783(17) -0.0087(13) 0.0008(13) -0.0084(13) C22 0.0530(12) 0.0427(11) 0.0546(12) 0.0013(9) -0.0016(9) -0.0032(9) C23 0.0742(16) 0.0589(14) 0.0707(15) 0.0041(12) 0.0083(13) 0.0117(13) C24 0.087(2) 0.0576(15) 0.101(2) -0.0020(15) 0.0014(18) 0.0197(15) C25 0.0791(18) 0.0531(15) 0.113(2) 0.0229(16) -0.0166(18) 0.0019(14) C26 0.0721(16) 0.0699(17) 0.0782(17) 0.0258(14) -0.0067(14) -0.0128(14) C27 0.0614(14) 0.0594(14) 0.0617(13) 0.0051(11) 0.0054(11) -0.0054(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 N1 C1 115.8(2) O1 N1 C15 123.4(2) C15 N1 C1 120.81(19) N1 C1 H1 115.5 N1 C1 C2 118.0(2) N1 C1 C3 121.0(2) C2 C1 H1 115.5 C2 C1 C3 60.04(17) C3 C1 H1 115.5 C1 C2 H2A 117.6 C1 C2 H2B 117.6 C1 C2 C3 61.20(16) H2A C2 H2B 114.8 C3 C2 H2A 117.6 C3 C2 H2B 117.6 C2 C3 C1 58.75(17) C2 C3 C4 117.1(2) C2 C3 C14 119.3(2) C4 C3 C1 116.0(2) C4 C3 C14 115.2(2) C14 C3 C1 119.0(2) C5 C4 C3 119.6(2) C13 C4 C3 122.1(2) C13 C4 C5 118.3(2) C4 C5 H5 119.4 C6 C5 C4 121.2(2) C6 C5 H5 119.4 C5 C6 H6 119.4 C5 C6 C7 121.2(2) C7 C6 H6 119.4 C6 C7 C8 122.7(3) C12 C7 C6 118.3(2) C12 C7 C8 119.0(2) C7 C8 H8 119.8 C9 C8 C7 120.5(3) C9 C8 H8 119.8 C8 C9 H9 119.5 C8 C9 C10 121.0(3) C10 C9 H9 119.5 C9 C10 H10 120.0 C11 C10 C9 120.0(3) C11 C10 H10 120.0 C10 C11 H11 119.4 C10 C11 C12 121.2(3) C12 C11 H11 119.4 C7 C12 C11 118.3(2) C7 C12 C13 119.1(2) C13 C12 C11 122.6(2) C4 C13 C12 122.0(2) C4 C13 H13 119.0 C12 C13 H13 119.0 C3 C14 H14A 109.5 C3 C14 H14B 109.5 C3 C14 H14C 109.5 H14A C14 H14B 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 N1 C15 C16 123.0(2) N1 C15 C22 118.2(2) C16 C15 C22 118.8(2) C17 C16 C15 124.5(3) C21 C16 C15 118.0(2) C21 C16 C17 117.4(3) C16 C17 H17 120.4 C16 C17 C18 119.1(3) C18 C17 H17 120.4 C17 C18 H18 119.3 C19 C18 C17 121.4(3) C19 C18 H18 119.3 C18 C19 H19 120.0 C20 C19 C18 120.0(3) C20 C19 H19 120.0 C19 C20 H20 119.9 C19 C20 C21 120.2(4) C21 C20 H20 119.9 C16 C21 H21 119.0 C20 C21 C16 121.9(3) C20 C21 H21 119.0 C23 C22 C15 122.0(2) C23 C22 C27 118.5(2) C27 C22 C15 119.4(2) C22 C23 H23 120.0 C22 C23 C24 120.1(3) C24 C23 H23 120.0 C23 C24 H24 119.9 C25 C24 C23 120.1(3) C25 C24 H24 119.9 C24 C25 H25 119.8 C26 C25 C24 120.5(3) C26 C25 H25 119.8 C25 C26 H26 120.1 C25 C26 C27 119.9(3) C27 C26 H26 120.1 C22 C27 H27 119.6 C26 C27 C22 120.9(3) C26 C27 H27 119.6 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 N1 1.297(2) N1 C1 1.471(3) N1 C15 1.319(3) C1 H1 0.9800 C1 C2 1.478(3) C1 C3 1.515(3) C2 H2A 0.9700 C2 H2B 0.9700 C2 C3 1.498(3) C3 C4 1.502(3) C3 C14 1.510(4) C4 C5 1.409(3) C4 C13 1.363(3) C5 H5 0.9300 C5 C6 1.361(4) C6 H6 0.9300 C6 C7 1.409(4) C7 C8 1.418(4) C7 C12 1.406(3) C8 H8 0.9300 C8 C9 1.351(4) C9 H9 0.9300 C9 C10 1.393(4) C10 H10 0.9300 C10 C11 1.355(4) C11 H11 0.9300 C11 C12 1.417(3) C12 C13 1.415(3) C13 H13 0.9300 C14 H14A 0.9600 C14 H14B 0.9600 C14 H14C 0.9600 C15 C16 1.472(3) C15 C22 1.492(3) C16 C17 1.398(4) C16 C21 1.398(4) C17 H17 0.9300 C17 C18 1.404(5) C18 H18 0.9300 C18 C19 1.363(6) C19 H19 0.9300 C19 C20 1.354(5) C20 H20 0.9300 C20 C21 1.375(4) C21 H21 0.9300 C22 C23 1.382(3) C22 C27 1.389(3) C23 H23 0.9300 C23 C24 1.385(4) C24 H24 0.9300 C24 C25 1.370(5) C25 H25 0.9300 C25 C26 1.360(4) C26 H26 0.9300 C26 C27 1.376(4) C27 H27 0.9300 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C17 H17 O1 0.93 2.17 2.758(4) 120.6