#------------------------------------------------------------------------------ #$Date: 2024-07-09 00:42:20 +0300 (Tue, 09 Jul 2024) $ #$Revision: 293301 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572060.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_1572060 loop_ _publ_author_name 'K\"orner, Lukas' 'Bockfeld, Dirk' 'Bannenberg, Thomas' 'Tamm, Matthias' _publ_section_title ; 2,3-Diamino-4,5-diarylcyclopentadienone iron carbonyl complexes as catalysts for reductive amination reactions ; _journal_name_full 'Catalysis Science & Technology' _journal_paper_doi 10.1039/D4CY00372A _journal_year 2024 _chemical_formula_moiety 'C27 H30 N2 O' _chemical_formula_sum 'C27 H30 N2 O' _chemical_formula_weight 398.53 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2024-03-06 deposited with the CCDC. 2024-07-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 115.442(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.5712(6) _cell_length_b 5.91540(10) _cell_length_c 20.8266(6) _cell_measurement_reflns_used 16544 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 76.4760 _cell_measurement_theta_min 2.4970 _cell_volume 2177.30(12) _computing_cell_refinement 'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)' _computing_publication_material 'OLEX2 v1.3 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)' _computing_structure_refinement 'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3-8)' _computing_structure_solution 'SHELXT 2018/2 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.979 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at home/near, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_unetI/netI 0.0262 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.979 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 34754 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.979 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 77.378 _diffrn_reflns_theta_min 2.500 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.569 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.65030 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.216 _exptl_crystal_description needle _exptl_crystal_F_000 856 _exptl_crystal_size_max 0.540 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.030 _refine_diff_density_max 0.266 _refine_diff_density_min -0.184 _refine_diff_density_rms 0.036 _refine_ls_extinction_coef 0.00069(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 272 _refine_ls_number_reflns 4537 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0367 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.8745P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0886 _refine_ls_wR_factor_ref 0.0926 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3919 _reflns_number_total 4537 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4cy00372a3.cif _cod_data_source_block lk29db _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1572060 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.749 _shelx_estimated_absorpt_t_max 0.983 _oxdiff_exptl_absorpt_empirical_full_min 0.682 _oxdiff_exptl_absorpt_empirical_full_max 1.361 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _shelx_res_file ; TITL lk29db_a.res in P2(1)/c lk29db.res created by SHELXL-2018/3 at 18:24:52 on 13-Jan-2022 REM Old TITL lk29db in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.119, Rweak 0.011, 0.026 REM 0.387 for 454 systematic absences, Orientation as input REM Formula found by SHELXT: C27 N2 O CELL 1.54184 19.5712 5.9154 20.8266 90 115.442 90 ZERR 4 0.0006 0.0001 0.0006 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 108 120 8 4 L.S. 4 0 0 PLAN 10 SIZE 0.03 0.05 0.54 TEMP -173 CONF BOND list 4 fmap 2 acta REM REM REM WGHT 0.039700 0.874500 EXTI 0.000685 FVAR 0.52990 O1 4 0.306401 0.248958 0.611831 11.00000 0.02260 0.02368 = 0.01585 -0.00283 0.00902 0.00146 N1 3 0.189839 0.620219 0.575249 11.00000 0.01758 0.02038 = 0.01326 0.00103 0.00582 -0.00139 N2 3 0.199892 0.755687 0.722710 11.00000 0.01987 0.02020 = 0.01748 0.00110 0.01016 0.00224 C1 1 0.293483 0.352287 0.656347 11.00000 0.01540 0.01832 = 0.01495 -0.00122 0.00644 -0.00305 C2 1 0.240974 0.541146 0.643984 11.00000 0.01719 0.01772 = 0.01541 -0.00024 0.00706 -0.00125 C3 1 0.239593 0.592306 0.707460 11.00000 0.01502 0.01641 = 0.01667 0.00005 0.00726 -0.00210 C4 1 0.296208 0.443526 0.765476 11.00000 0.01753 0.01625 = 0.01584 0.00015 0.00733 -0.00206 C5 1 0.328675 0.301573 0.736170 11.00000 0.01583 0.01675 = 0.01465 -0.00109 0.00539 -0.00293 C6 1 0.227710 0.710529 0.533021 11.00000 0.02238 0.02593 = 0.01702 0.00083 0.00894 -0.00501 AFIX 23 H6A 2 0.256370 0.588114 0.523163 11.00000 -1.20000 H6B 2 0.264045 0.829659 0.560496 11.00000 -1.20000 AFIX 0 C7 1 0.170106 0.808779 0.463142 11.00000 0.03237 0.02846 = 0.01760 0.00406 0.00993 -0.00345 AFIX 23 H7A 2 0.144919 0.940605 0.472994 11.00000 -1.20000 H7B 2 0.196391 0.861622 0.434552 11.00000 -1.20000 AFIX 0 C8 1 0.110877 0.633292 0.421043 11.00000 0.02887 0.03766 = 0.01404 0.00182 0.00494 -0.00316 AFIX 23 H8A 2 0.135004 0.508577 0.406582 11.00000 -1.20000 H8B 2 0.071928 0.703222 0.377522 11.00000 -1.20000 AFIX 0 C9 1 0.074077 0.540757 0.466929 11.00000 0.02112 0.04111 = 0.01881 0.00228 0.00241 -0.00633 AFIX 23 H9A 2 0.045616 0.662913 0.477176 11.00000 -1.20000 H9B 2 0.037863 0.419706 0.440773 11.00000 -1.20000 AFIX 0 C10 1 0.133608 0.446868 0.536336 11.00000 0.02067 0.02681 = 0.01893 0.00204 0.00537 -0.00613 AFIX 23 H10A 2 0.108876 0.392586 0.566119 11.00000 -1.20000 H10B 2 0.159222 0.316648 0.526203 11.00000 -1.20000 AFIX 0 C11 1 0.166941 0.948861 0.675262 11.00000 0.02087 0.01760 = 0.02368 0.00020 0.01037 0.00116 AFIX 23 H11A 2 0.190937 0.961869 0.642155 11.00000 -1.20000 H11B 2 0.178162 1.089079 0.703934 11.00000 -1.20000 AFIX 0 C12 1 0.081607 0.927233 0.632400 11.00000 0.02020 0.02549 = 0.02568 0.00355 0.00891 0.00311 AFIX 23 H12A 2 0.070354 0.801279 0.598048 11.00000 -1.20000 H12B 2 0.061295 1.068153 0.605214 11.00000 -1.20000 AFIX 0 C13 1 0.043234 0.883152 0.681465 11.00000 0.01957 0.03599 = 0.02999 -0.00209 0.01187 0.00306 AFIX 23 H13A 2 0.048411 1.017989 0.711368 11.00000 -1.20000 H13B 2 -0.011373 0.854473 0.652636 11.00000 -1.20000 AFIX 0 C14 1 0.079303 0.679573 0.728766 11.00000 0.02412 0.03745 = 0.02506 -0.00007 0.01565 -0.00166 AFIX 23 H14A 2 0.069985 0.542281 0.698995 11.00000 -1.20000 H14B 2 0.055847 0.656854 0.761978 11.00000 -1.20000 AFIX 0 C15 1 0.164521 0.714572 0.771090 11.00000 0.02388 0.03135 = 0.01914 -0.00004 0.01316 0.00305 AFIX 23 H15A 2 0.173899 0.845125 0.803533 11.00000 -1.20000 H15B 2 0.187271 0.578804 0.800270 11.00000 -1.20000 AFIX 0 C16 1 0.318046 0.473721 0.842518 11.00000 0.01715 0.01997 = 0.01549 0.00130 0.00769 0.00310 C17 1 0.309298 0.299183 0.883578 11.00000 0.02470 0.01925 = 0.02183 0.00175 0.01117 0.00132 AFIX 43 H17 2 0.287287 0.159907 0.861771 11.00000 -1.20000 AFIX 0 C18 1 0.332677 0.328478 0.956241 11.00000 0.03281 0.02719 = 0.02137 0.00902 0.01562 0.00729 AFIX 43 H18 2 0.325786 0.210148 0.983740 11.00000 -1.20000 AFIX 0 C19 1 0.365993 0.529779 0.988639 11.00000 0.03557 0.03180 = 0.01372 0.00219 0.01032 0.00905 AFIX 43 H19 2 0.382662 0.548764 1.038398 11.00000 -1.20000 AFIX 0 C20 1 0.374883 0.703001 0.948232 11.00000 0.03612 0.02360 = 0.01861 -0.00324 0.00973 0.00132 AFIX 43 H20 2 0.397820 0.840937 0.970412 11.00000 -1.20000 AFIX 0 C21 1 0.350466 0.676438 0.875403 11.00000 0.02795 0.01920 = 0.01726 0.00113 0.01074 0.00112 AFIX 43 H21 2 0.355934 0.797280 0.847927 11.00000 -1.20000 AFIX 0 C22 1 0.390867 0.139389 0.770336 11.00000 0.01727 0.01781 = 0.01528 0.00139 0.00819 -0.00056 C23 1 0.450093 0.180730 0.837739 11.00000 0.02193 0.01914 = 0.01701 -0.00092 0.00776 -0.00025 AFIX 43 H23 2 0.450931 0.317305 0.862065 11.00000 -1.20000 AFIX 0 C24 1 0.507300 0.022782 0.868834 11.00000 0.02090 0.02765 = 0.01643 0.00122 0.00445 0.00095 AFIX 43 H24 2 0.547036 0.052197 0.914437 11.00000 -1.20000 AFIX 0 C25 1 0.507265 -0.177835 0.834187 11.00000 0.02069 0.02179 = 0.02316 0.00584 0.00973 0.00471 AFIX 43 H25 2 0.546385 -0.285815 0.856145 11.00000 -1.20000 AFIX 0 C26 1 0.449601 -0.219311 0.767206 11.00000 0.02410 0.01597 = 0.02269 -0.00064 0.01277 -0.00012 AFIX 43 H26 2 0.449365 -0.355787 0.743068 11.00000 -1.20000 AFIX 0 C27 1 0.392238 -0.061631 0.735403 11.00000 0.01845 0.01894 = 0.01629 -0.00044 0.00758 -0.00274 AFIX 43 H27 2 0.353382 -0.090608 0.689290 11.00000 -1.20000 AFIX 0 HKLF 4 REM lk29db_a.res in P2(1)/c REM wR2 = 0.0926, GooF = S = 1.025, Restrained GooF = 1.025 for all data REM R1 = 0.0367 for 3919 Fo > 4sig(Fo) and 0.0440 for all 4537 data REM 272 parameters refined using 0 restraints END WGHT 0.0397 0.8746 REM Highest difference peak 0.266, deepest hole -0.184, 1-sigma level 0.036 Q1 1 0.3166 0.3277 0.6996 11.00000 0.05 0.27 Q2 1 0.3328 0.4280 0.7511 11.00000 0.05 0.26 Q3 1 0.3066 0.4634 0.8034 11.00000 0.05 0.25 Q4 1 0.2809 0.4897 0.6485 11.00000 0.05 0.25 Q5 1 0.2710 0.5270 0.7395 11.00000 0.05 0.24 Q6 1 0.4121 0.1408 0.8074 11.00000 0.05 0.23 Q7 1 0.2533 0.6087 0.6751 11.00000 0.05 0.22 Q8 1 0.2953 0.3103 0.7527 11.00000 0.05 0.22 Q9 1 0.3828 0.0086 0.7641 11.00000 0.05 0.21 Q10 1 0.4013 0.0643 0.7453 11.00000 0.05 0.19 ; _shelx_res_checksum 60564 _shelx_hkl_file ; 0 0 2 2089.27 100.86 0 0 -2 1998.82 100.85 0 0 -2 1998.98 100.82 0 0 3 0.37 1.36 0 0 3 0.10 1.40 0 0 -3 -0.81 2.50 0 0 -3 -0.69 1.13 0 0 3 -0.45 2.10 0 0 -3 -0.59 1.17 0 0 4 451.64 22.11 0 0 4 437.43 22.07 0 0 -4 435.13 22.42 0 0 4 427.17 22.29 0 0 -4 427.88 21.98 0 0 5 -0.18 2.05 0 0 5 -0.92 2.21 0 0 5 0.37 1.53 0 0 -5 -1.37 3.43 0 0 5 0.13 2.93 0 0 -5 -0.07 1.73 0 0 6 65.16 4.45 0 0 6 70.53 4.44 0 0 -6 65.16 4.58 0 0 -6 68.93 5.53 0 0 6 63.73 3.99 0 0 6 62.15 5.00 0 0 -6 72.21 4.21 0 0 7 -2.11 2.42 0 0 -7 1.47 2.06 0 0 -7 1.69 2.60 0 0 7 -0.18 3.24 0 0 7 -0.60 1.71 0 0 -7 -0.79 4.13 0 0 -8 766.59 39.11 0 0 8 741.06 38.24 0 0 8 760.99 38.58 0 0 -8 796.20 38.86 0 0 8 751.90 38.92 0 0 -9 -0.45 2.86 0 0 -9 -1.86 4.61 0 0 9 1.81 1.98 0 0 9 -0.49 3.83 0 0 9 1.57 2.71 0 0 10 1944.35 100.86 0 0 -10 2059.41 101.92 0 0 10 2057.97 101.76 0 0 10 2056.55 101.32 0 0 -10 2072.26 101.68 0 0 11 0.58 1.64 0 0 -11 0.34 4.71 0 0 11 -2.23 3.85 0 0 11 1.54 2.74 0 0 -11 2.94 2.80 0 0 -12 138.12 9.61 0 0 12 134.92 7.39 0 0 12 131.06 7.45 0 0 12 135.05 9.23 0 0 -12 128.00 8.60 0 0 12 141.13 8.23 0 0 -13 2.60 4.91 0 0 -13 -0.46 1.48 0 0 13 0.65 2.23 0 0 13 3.25 4.28 0 0 13 -0.21 2.06 0 0 13 -1.33 2.57 0 0 -13 1.45 2.84 0 0 -14 50.75 3.42 0 0 -14 63.17 6.89 0 0 14 57.57 4.09 0 0 14 52.97 3.90 0 0 14 70.24 6.57 0 0 14 44.99 4.61 0 0 -14 50.67 5.07 0 0 -15 -0.28 1.71 0 0 -15 -3.12 5.46 0 0 15 -0.13 2.78 0 0 15 1.24 2.47 0 0 15 -0.99 4.79 0 0 -15 -0.85 3.20 0 0 15 -0.91 2.88 0 0 -16 238.13 14.64 0 0 -16 227.24 11.69 0 0 16 218.32 12.07 0 0 16 227.81 11.98 0 0 16 214.40 14.10 0 0 16 208.70 12.69 0 0 -16 215.22 13.52 0 0 -17 -0.69 1.84 0 0 -17 -0.42 3.01 0 0 -17 -4.55 5.74 0 0 17 0.86 2.87 0 0 17 -0.27 2.51 0 0 17 0.55 4.97 0 0 -17 0.44 3.02 0 0 -18 71.92 4.48 0 0 -18 80.72 8.03 0 0 -18 61.12 5.94 0 0 18 70.91 5.18 0 0 18 68.41 4.98 0 0 18 73.49 7.45 0 0 18 81.23 4.75 0 0 -18 77.19 6.24 0 0 19 -0.40 2.79 0 0 19 1.07 2.07 0 0 19 1.09 2.40 0 0 -19 2.26 1.77 0 0 20 332.54 17.53 0 0 20 341.99 17.64 0 0 20 333.23 17.38 0 0 -20 348.37 17.34 0 0 21 1.90 2.20 0 0 21 -1.18 1.88 0 0 21 0.54 1.46 0 0 -21 -1.09 1.41 0 0 22 49.84 3.10 0 0 22 48.96 3.27 0 0 -22 45.82 2.76 0 0 23 -0.33 1.40 0 0 23 0.87 1.12 0 -1 0 0.62 2.03 0 -1 0 -0.14 1.72 0 -1 -1 205.54 10.16 0 -1 1 201.11 10.27 0 -1 -1 214.80 10.40 0 -1 1 181.59 10.02 0 -1 -2 3.81 2.47 0 -1 -2 2.78 0.92 0 -1 -2 3.88 1.90 0 -1 -2 3.50 2.13 0 -1 2 3.19 2.21 0 -1 2 0.98 1.80 0 1 2 1.15 1.25 0 -1 2 3.04 1.91 0 -1 -3 81.84 5.56 0 -1 -3 92.18 4.88 0 1 -3 84.14 4.55 0 -1 3 80.56 4.57 0 1 3 83.61 4.44 0 -1 -3 81.79 4.53 0 -1 3 86.17 4.78 0 -1 -3 81.76 4.80 0 -1 -3 79.65 4.97 0 -1 3 85.98 4.98 0 1 3 82.44 4.80 0 -1 3 88.72 5.15 0 1 -4 525.12 26.05 0 -1 -4 555.19 26.49 0 -1 -4 528.72 26.10 0 1 -4 512.56 25.80 0 -1 -4 537.23 25.95 0 -1 4 494.95 25.89 0 1 4 528.08 25.81 0 -1 4 494.69 25.98 0 -1 -4 469.13 25.96 0 -1 4 505.32 25.94 0 -1 -4 508.92 25.95 0 -1 4 517.37 26.26 0 1 4 540.41 26.10 0 1 -5 193.20 10.08 0 1 -5 195.86 9.69 0 -1 -5 191.32 9.76 0 1 -5 190.52 9.33 0 -1 -5 190.09 9.45 0 -1 5 188.98 9.42 0 -1 -5 172.03 9.49 0 -1 5 177.50 9.48 0 1 5 187.08 9.91 0 -1 5 184.82 10.14 0 1 5 209.49 9.45 0 -1 -5 159.31 9.14 0 -1 -5 184.70 9.58 0 -1 5 187.85 9.50 0 1 -6 179.35 9.43 0 -1 -6 180.17 9.53 0 1 -6 185.02 9.97 0 -1 6 168.37 9.10 0 -1 6 173.27 9.05 0 -1 -6 163.00 9.09 0 -1 -6 171.45 9.05 0 -1 6 176.64 9.26 0 -1 -6 173.53 9.37 0 1 6 188.71 9.21 0 1 -6 177.46 9.06 0 -1 6 173.66 9.98 0 1 6 176.27 9.75 0 -1 -7 166.82 8.87 0 1 7 159.89 8.65 0 1 7 146.49 9.21 0 -1 7 160.82 8.72 0 1 7 162.28 9.26 0 1 -7 163.51 8.47 0 -1 7 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1.81 4.33 5 -4 -3 3.82 1.47 -5 -4 3 2.15 1.77 -5 -4 3 3.54 1.70 5 -4 -3 2.72 1.99 5 -4 -3 -0.59 2.39 -5 -4 3 0.79 2.11 -5 -4 3 2.20 1.74 5 -4 -3 0.77 2.29 -5 -4 2 7.06 1.91 -5 -4 2 6.39 2.41 5 -4 -2 7.72 2.41 5 -4 -2 10.70 2.21 5 -4 -2 8.68 3.67 5 -4 -2 8.61 4.76 -5 4 2 8.34 2.97 5 -4 -2 7.12 2.17 5 -4 -2 5.83 1.58 -5 -4 2 7.49 1.78 5 -4 -2 7.74 2.09 -5 -4 2 7.33 1.86 5 -4 -2 6.74 2.48 -5 -4 2 9.93 2.13 -5 -4 2 8.15 1.75 5 -4 -2 7.19 1.59 5 -4 -2 9.48 2.48 -5 -4 1 154.22 7.56 -5 -4 1 109.53 7.24 5 4 -1 141.64 8.66 5 -4 -1 133.51 7.46 5 -4 -1 133.37 7.45 -5 4 1 136.28 8.84 5 -4 -1 129.27 7.33 5 -4 -1 144.33 7.22 -5 -4 1 137.81 7.30 -5 -4 1 131.44 7.24 -5 -4 1 137.67 7.27 5 -4 -1 133.09 7.53 -5 -4 1 132.07 7.24 5 -4 -1 131.79 7.21 5 -4 -1 143.10 9.31 5 -4 0 30.18 4.76 5 -4 0 36.06 5.48 5 -4 0 35.94 3.23 5 4 0 36.76 4.19 -5 -4 0 33.91 2.89 -5 -4 0 44.76 2.94 5 -4 0 33.95 3.23 -5 4 0 41.13 4.49 5 -4 0 34.09 3.02 5 -4 0 33.06 2.93 -5 -4 0 39.98 2.79 5 -4 0 43.04 2.67 -5 -4 0 40.75 2.81 -5 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-5 4 -7 12.22 3.29 5 -4 7 17.60 2.00 5 -4 7 11.11 3.18 -5 4 -8 72.59 6.16 -5 -4 -8 84.71 4.97 5 -4 8 77.55 5.34 -5 4 -9 83.80 7.30 5 4 9 78.84 7.73 5 -4 9 99.80 5.84 5 -4 9 91.25 5.66 -5 4 -9 94.20 6.77 -5 -4 -9 90.08 5.46 -5 -4 -10 5.07 2.10 -5 4 -10 3.95 2.68 5 4 10 5.67 3.97 -5 4 -10 10.01 3.53 5 -4 10 3.70 2.71 5 -4 10 3.65 2.41 5 4 10 7.28 2.03 5 4 10 11.69 4.40 5 -4 11 124.44 6.77 5 -4 11 124.63 6.79 5 4 11 107.63 6.56 -5 4 -12 28.60 2.16 5 4 12 27.97 2.58 5 -4 12 28.75 2.70 5 -4 12 28.77 2.70 -5 4 -13 13.91 1.62 5 4 13 17.95 2.14 5 -4 13 16.25 2.09 5 -4 13 16.87 2.24 -5 4 -14 4.21 1.18 5 -4 14 4.19 1.77 5 4 14 4.89 1.69 5 -4 15 51.36 3.10 5 4 15 57.61 3.14 5 -4 15 56.00 3.15 5 -4 16 82.87 4.55 5 4 16 87.81 4.54 5 -4 16 83.57 4.52 -5 -5 19 1.74 0.66 -5 -5 18 1.37 0.68 -5 -5 18 1.85 1.02 -5 -5 18 1.40 0.94 -5 -5 17 10.30 1.21 -5 -5 17 10.35 1.35 -5 -5 17 8.23 1.40 -5 -5 16 5.28 1.31 -5 -5 16 3.77 1.47 -5 -5 16 4.44 1.36 -5 -5 15 1.43 1.82 -5 -5 15 0.14 1.52 -5 -5 15 2.61 1.67 5 -5 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116.54 7.71 5 -5 -4 162.93 12.77 5 -5 -4 179.05 12.59 5 -5 -4 202.51 10.95 5 5 -4 176.48 12.12 -5 -5 4 208.13 10.68 -5 5 4 179.79 12.37 5 -5 -4 194.06 10.80 -5 -5 4 220.83 10.75 -5 -5 4 213.76 10.80 -5 -5 4 205.35 10.74 5 -5 -4 189.25 10.62 -5 -5 4 197.93 10.68 5 -5 -4 206.72 11.07 -5 -5 4 207.23 10.83 -5 -5 3 27.77 2.98 5 -5 -3 16.83 5.16 5 -5 -3 25.09 3.20 5 5 -3 36.03 4.49 -5 5 3 26.69 4.58 -5 -5 3 28.20 2.83 -5 -5 3 25.09 2.68 5 -5 -3 22.52 2.84 -5 -5 3 28.93 2.74 5 -5 -3 27.81 3.06 -5 -5 3 27.87 2.88 -5 -5 3 30.75 2.61 5 -5 -3 19.91 3.58 5 -5 -2 40.61 5.45 5 -5 -2 37.24 5.91 5 -5 -2 34.41 3.76 5 5 -2 50.81 4.85 5 -5 -2 51.35 3.66 5 -5 -2 48.00 3.25 -5 -5 2 52.32 3.46 -5 -5 2 44.33 3.44 5 -5 -2 36.60 4.16 -5 -5 2 48.50 3.94 -5 -5 2 47.40 3.48 -5 -5 2 46.88 3.68 -5 -5 2 47.73 3.55 5 -5 -2 43.26 3.78 -5 -5 2 49.72 3.30 -5 5 2 44.39 5.23 5 -5 -2 46.33 3.74 5 -5 -2 45.27 3.84 5 -5 -1 253.83 12.91 5 -5 -1 238.40 12.91 -5 5 1 227.68 14.09 -5 -5 1 219.02 12.76 -5 -5 1 270.10 12.98 5 -5 -1 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1.45 10 3 12 2.29 1.71 10 3 12 2.14 2.06 10 -3 12 -0.48 1.81 -10 3 -13 50.74 3.05 10 3 13 51.93 3.14 10 3 13 48.64 3.38 10 -3 13 50.72 3.20 -10 3 -14 11.52 1.26 10 3 14 13.30 1.32 10 3 14 11.13 1.55 10 -3 14 13.46 1.33 -10 -4 22 4.36 0.78 -10 -4 21 14.70 1.36 10 -4 -20 4.71 1.29 10 4 -20 6.93 0.97 -10 -4 20 5.31 1.28 -10 -4 19 56.38 3.47 10 -4 -19 52.10 3.49 -10 -4 19 61.72 3.50 10 4 -19 56.87 3.24 10 4 -18 25.27 1.95 10 -4 -18 29.33 2.51 -10 -4 18 28.71 2.30 -10 -4 18 28.14 2.35 -10 -4 17 73.06 3.96 10 4 -17 67.16 3.96 10 -4 -17 67.73 4.41 -10 -4 17 71.72 4.30 -10 -4 17 70.28 4.29 -10 -4 16 12.64 1.63 10 -4 -16 7.95 2.35 -10 -4 16 13.16 2.03 -10 -4 16 11.31 1.94 -10 -4 15 145.13 7.74 10 -4 -15 151.92 8.12 -10 -4 15 139.39 7.95 10 -4 -14 27.90 2.34 10 -4 -14 29.45 2.31 -10 -4 14 32.44 2.74 -10 -4 14 29.50 2.48 -10 -4 14 29.43 2.15 -10 -4 13 107.89 5.96 10 -4 -13 111.99 6.30 -10 -4 13 99.89 6.03 -10 4 13 94.70 7.68 10 4 -13 112.74 7.95 10 -4 -13 111.86 6.13 10 -4 -13 110.93 6.07 -10 4 13 105.14 7.87 -10 -4 13 104.13 6.19 -10 -4 13 111.90 6.05 10 -4 -13 104.75 6.12 -10 -4 12 177.04 9.78 10 -4 -12 199.06 10.08 -10 -4 12 170.09 9.84 10 -4 -12 151.14 11.33 -10 4 12 186.76 11.57 10 4 -12 189.20 11.64 10 -4 -12 183.56 9.92 10 -4 -12 187.69 9.91 -10 4 12 206.71 11.87 -10 -4 12 186.77 9.90 -10 -4 12 193.33 10.00 10 -4 -12 185.85 10.11 -10 -4 12 193.00 9.84 10 -4 -12 179.81 9.96 10 -4 -11 24.15 3.04 -10 -4 11 29.35 2.60 -10 -4 11 29.23 2.76 10 -4 -11 23.64 3.37 10 -4 -11 22.17 4.48 10 -4 -11 28.83 5.03 -10 4 11 30.77 4.58 10 4 -11 33.04 4.28 -10 4 11 28.86 4.94 10 -4 -11 23.50 2.84 10 -4 -11 21.37 2.27 -10 -4 11 27.75 2.61 10 -4 -11 29.72 3.15 -10 -4 11 27.95 2.54 10 -4 -11 29.43 3.00 -10 -4 10 129.08 6.86 -10 -4 10 120.03 6.94 10 -4 -10 146.17 7.37 10 -4 -10 126.60 9.02 10 -4 -10 102.60 8.98 -10 4 10 126.03 8.57 10 4 -10 141.00 9.29 10 4 -10 123.33 8.47 10 -4 -10 120.68 7.05 10 -4 -10 116.82 6.95 -10 4 10 142.16 9.06 -10 -4 10 114.92 6.77 10 -4 -10 103.66 6.67 10 -4 -10 122.00 7.12 -10 -4 10 123.81 6.80 10 -4 -10 129.24 7.09 -10 -4 9 151.69 7.93 10 -4 -9 141.60 8.32 -10 -4 9 147.06 8.01 10 -4 -9 147.71 10.06 10 -4 -9 132.95 10.34 -10 4 9 147.87 9.51 10 4 -9 156.12 10.18 10 4 -9 153.02 9.44 10 -4 -9 145.04 8.11 10 -4 -9 130.58 7.99 -10 4 9 143.33 9.93 10 -4 -9 143.21 8.08 10 -4 -9 133.39 7.78 -10 -4 9 137.47 7.81 -10 -4 9 150.32 7.85 10 -4 -9 145.60 8.13 10 -4 -8 23.81 3.20 -10 -4 8 21.96 2.94 10 -4 -8 31.26 3.81 -10 -4 8 32.74 2.83 10 -4 -8 27.75 5.03 10 -4 -8 41.46 6.37 -10 4 8 28.67 4.13 10 4 -8 26.35 3.83 10 4 -8 32.93 5.04 -10 4 8 32.43 5.20 10 -4 -8 26.88 3.11 10 -4 -8 23.49 2.45 10 -4 -8 26.81 3.03 -10 -4 8 24.36 2.46 10 -4 -8 27.68 2.76 -10 -4 8 28.29 2.57 10 -4 -8 23.98 3.16 -10 -4 7 22.23 2.72 -10 -4 7 24.56 3.00 10 -4 -7 20.10 3.74 10 -4 -7 28.19 3.40 10 -4 -7 25.26 5.02 10 -4 -7 32.47 5.74 -10 4 7 29.33 3.77 10 4 -7 27.01 4.83 10 -4 -7 22.46 3.08 10 -4 -7 24.31 2.91 10 -4 -7 23.15 2.36 -10 -4 7 28.57 2.44 10 -4 -7 24.33 2.98 -10 -4 7 27.79 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216.01 11.97 22 0 -5 3.07 1.96 -22 0 5 1.67 1.43 22 0 -5 1.37 1.79 22 0 -4 54.95 3.27 -22 0 4 52.10 2.94 -22 0 4 43.32 2.95 22 0 -4 44.75 3.23 22 0 -4 50.41 3.15 -22 0 3 1.45 1.00 22 0 -3 0.92 1.50 22 0 -3 -0.89 1.31 22 0 -2 51.16 3.48 22 0 -1 -2.37 1.75 22 0 0 0.15 1.39 22 -1 -20 0.04 0.88 22 -1 -19 54.10 3.14 22 -1 -18 48.89 3.02 22 -1 -17 42.10 2.57 22 1 -17 39.65 2.33 22 -1 -17 38.14 2.33 22 -1 -17 37.59 2.54 -22 1 17 32.54 2.20 -22 -1 17 33.81 2.22 22 -1 -16 22.67 2.07 22 -1 -16 21.92 1.94 22 1 -16 25.47 1.96 22 1 -16 21.43 2.02 22 -1 -16 25.75 2.03 -22 1 16 19.48 1.76 -22 -1 16 24.27 1.71 -22 -1 16 19.10 1.77 22 -1 -16 17.54 2.33 22 -1 -16 26.98 2.16 22 -1 -15 3.00 1.52 22 -1 -15 2.98 1.68 22 1 -15 4.13 1.68 22 1 -15 0.85 1.82 22 -1 -15 2.32 1.72 -22 1 15 4.42 1.38 -22 -1 15 2.03 1.25 -22 -1 15 2.12 1.40 22 -1 -15 4.25 2.22 22 -1 -15 5.12 1.93 22 -1 -14 18.22 1.99 22 -1 -14 18.57 2.21 22 1 -14 19.63 2.20 22 1 -14 22.35 2.38 22 -1 -14 22.90 2.31 -22 -1 14 21.94 1.88 -22 -1 14 17.47 1.94 22 -1 -14 21.61 2.46 -22 1 14 22.46 1.91 22 -1 -13 8.59 1.63 22 -1 -13 6.72 1.97 22 1 -13 3.35 2.01 22 1 -13 8.29 2.19 22 -1 -13 2.78 2.08 -22 -1 13 4.97 1.49 -22 -1 13 4.29 1.62 -22 1 13 5.94 1.56 22 -1 -13 5.24 2.27 22 -1 -12 11.17 1.79 22 -1 -12 6.42 2.15 22 1 -12 11.36 2.27 -22 -1 12 14.32 1.87 -22 -1 12 15.93 1.78 -22 1 12 9.64 1.72 22 1 -12 10.16 2.39 22 -1 -12 8.85 2.27 22 -1 -11 58.70 3.80 22 1 -11 67.90 4.27 22 -1 -11 58.04 4.12 -22 1 11 71.27 3.81 -22 -1 11 55.86 3.79 22 -1 -10 142.02 8.37 22 -1 -10 151.46 8.59 22 -1 -10 158.77 8.53 22 1 -10 163.41 8.56 22 1 -10 178.25 8.70 22 -1 -10 161.38 8.59 -22 -1 10 160.61 8.36 -22 1 10 175.65 8.39 -22 -1 10 137.91 8.34 -22 -1 9 10.82 1.74 22 -1 -9 10.30 2.51 22 -1 -9 9.13 1.64 22 -1 -9 8.12 2.18 22 1 -9 13.01 2.30 -22 -1 8 123.87 6.66 -22 1 8 121.36 6.66 -22 -1 8 126.01 6.72 22 -1 -8 128.96 6.95 22 -1 -8 117.80 6.85 22 1 -8 122.22 6.87 22 1 -7 -0.73 2.19 22 -1 -7 2.95 2.11 -22 -1 7 3.29 1.51 -22 -1 7 2.44 1.63 -22 1 7 0.91 1.50 22 -1 -7 1.06 2.25 22 -1 -7 3.25 1.98 22 1 -7 2.09 2.02 22 1 -6 20.55 2.46 22 -1 -6 21.44 2.48 -22 -1 6 24.28 1.99 -22 1 6 22.24 2.03 -22 -1 6 23.41 2.08 22 -1 -6 21.57 2.52 22 -1 -6 24.28 2.37 22 1 -6 21.87 2.34 22 1 -5 -0.96 1.82 22 -1 -5 -0.30 1.84 -22 1 5 0.12 1.33 -22 -1 5 -0.81 1.25 -22 -1 5 1.21 1.39 22 -1 -5 -3.76 2.37 22 -1 -5 -0.47 1.92 22 -1 -5 -0.48 1.70 22 1 -5 -1.24 1.68 22 1 -4 90.77 4.79 22 -1 -4 89.18 4.77 -22 -1 4 85.75 4.56 -22 1 4 78.41 4.53 -22 -1 4 81.43 4.56 22 -1 -4 87.95 4.70 22 1 -4 85.50 4.69 22 -1 -4 92.22 4.78 22 -1 -3 1.49 1.18 22 1 -3 1.70 1.19 22 -1 -3 1.24 1.70 -22 -1 3 2.23 0.90 -22 1 3 2.13 0.88 22 -1 -3 1.20 1.36 22 -1 -2 2.15 1.48 22 1 -2 2.61 1.73 22 1 -1 27.08 2.20 22 1 0 1.13 1.19 22 -2 -17 6.93 1.24 22 -2 -16 5.64 1.41 22 2 -16 9.58 1.28 22 -2 -16 9.13 1.23 -22 2 16 8.04 1.03 -22 -2 16 10.43 1.11 22 -2 -16 9.24 1.54 22 -2 -15 6.09 1.41 22 -2 -15 5.11 1.39 22 2 -15 4.27 1.42 22 2 -15 7.31 1.47 22 -2 -15 5.00 1.43 -22 -2 15 5.98 1.08 -22 -2 15 3.86 1.22 22 -2 -15 4.54 1.83 22 -2 -15 5.64 1.58 -22 2 15 5.67 1.15 22 -2 -14 4.70 1.46 22 -2 -14 5.98 1.54 22 2 -14 6.22 1.58 22 2 -14 8.54 1.78 22 -2 -14 8.28 1.69 -22 -2 14 4.66 1.37 -22 -2 14 6.78 1.23 22 -2 -14 9.44 2.06 -22 2 14 7.57 1.28 22 -2 -14 5.62 1.75 22 -2 -13 1.15 1.44 22 -2 -13 2.13 1.62 22 2 -13 0.72 1.69 22 2 -13 2.61 1.88 22 -2 -13 0.49 1.71 -22 -2 13 2.23 1.38 -22 -2 13 1.87 1.22 -22 2 13 3.97 1.29 22 -2 -13 1.52 2.18 22 -2 -13 2.59 1.84 22 -2 -12 2.44 1.47 22 -2 -12 2.78 1.73 22 2 -12 4.65 1.87 -22 -2 12 4.19 1.33 -22 2 12 3.41 1.36 22 -2 -12 3.62 2.28 22 -2 -12 1.25 1.99 -22 -2 12 0.83 1.46 22 2 -12 1.42 2.00 22 -2 -12 2.04 1.83 22 -2 -11 14.65 1.91 22 -2 -11 18.60 2.21 -22 2 11 17.53 1.75 22 -2 -11 13.07 2.60 -22 -2 11 17.84 1.84 22 -2 -10 10.30 1.79 22 2 -10 15.42 2.35 22 -2 -10 11.46 2.13 -22 -2 10 15.77 1.69 -22 2 10 15.48 1.71 22 -2 -10 14.11 2.60 22 -2 -10 17.50 2.30 -22 -2 10 14.37 1.80 22 -2 -10 12.06 2.04 22 2 -10 19.25 2.20 -22 -2 9 25.47 2.00 22 -2 -9 22.45 2.53 22 -2 -9 23.74 2.35 22 2 -9 23.49 2.38 22 -2 -8 13.41 2.07 -22 -2 8 8.46 1.46 -22 2 8 8.77 1.52 22 -2 -8 9.19 2.10 -22 -2 8 7.05 1.61 22 -2 -8 8.20 1.90 22 2 -8 9.72 1.96 22 2 -7 3.53 1.88 22 -2 -7 2.69 1.77 -22 -2 7 4.65 1.44 -22 -2 7 1.16 1.28 -22 2 7 2.62 1.29 22 -2 -7 4.46 2.29 22 -2 -7 6.26 1.94 22 -2 -7 2.67 1.67 22 2 -7 1.70 1.69 22 2 -6 1.41 1.71 22 -2 -6 1.77 1.66 -22 -2 6 0.06 1.34 -22 -2 6 2.04 1.17 22 -2 -6 -0.07 2.10 -22 2 6 0.40 1.19 22 -2 -6 3.98 1.84 22 -2 -6 1.99 1.53 22 2 -6 3.04 1.56 22 2 -5 3.37 1.52 22 -2 -5 -0.06 1.46 -22 -2 5 1.07 1.05 -22 -2 5 1.16 1.13 22 -2 -5 -0.06 1.87 22 -2 -5 1.99 1.56 -22 2 5 -0.39 1.05 22 2 -5 2.94 1.37 22 2 -4 0.57 0.71 22 2 -4 2.14 1.63 -22 -2 4 3.93 0.89 22 -2 -4 4.07 1.30 22 -2 -4 5.83 1.12 22 2 -4 2.32 1.14 22 2 -3 62.27 3.64 22 -2 -2 2.03 1.31 22 3 -13 -1.52 1.22 22 -3 -13 -0.16 1.10 -22 -3 13 1.29 0.81 -22 -3 13 2.11 0.92 -22 3 13 0.84 0.82 22 -3 -13 0.88 1.13 22 -3 -13 0.74 1.37 22 -3 -13 1.22 1.04 22 3 -13 -0.66 1.11 22 3 -12 5.35 1.47 22 -3 -12 5.96 1.26 -22 -3 12 5.32 0.99 -22 -3 12 4.95 1.11 -22 3 12 3.27 0.97 22 -3 -12 4.57 1.36 22 -3 -12 6.40 1.61 22 -3 -12 6.96 1.22 22 3 -12 7.16 1.30 22 3 -11 14.16 1.69 22 -3 -11 11.17 1.53 -22 -3 11 13.20 1.32 -22 3 11 10.92 1.22 22 -3 -11 10.81 1.82 22 3 -10 19.35 1.90 22 -3 -10 16.95 1.67 -22 -3 10 17.76 1.43 -22 -3 10 15.78 1.51 -22 3 10 12.84 1.41 22 -3 -10 18.55 1.76 22 -3 -10 21.76 2.02 22 -3 -10 18.25 1.65 22 3 -10 24.39 1.81 22 -3 -9 14.92 1.60 -22 -3 9 11.55 1.21 22 -3 -9 12.29 1.63 22 -3 -9 11.68 1.46 22 3 -9 13.66 1.57 22 3 -8 5.63 1.48 22 -3 -8 2.51 1.32 22 -3 -8 2.65 1.49 -22 -3 8 5.14 0.97 -22 -3 8 4.62 1.07 -22 3 8 3.05 0.95 22 -3 -8 3.67 1.40 22 -3 -8 3.86 1.68 22 -3 -8 3.72 1.20 22 3 -8 5.06 1.32 22 3 -7 11.55 1.45 22 -3 -7 12.68 1.34 22 -3 -7 10.99 1.23 22 3 -7 9.92 1.34 -22 -3 7 8.73 1.03 -22 3 7 7.26 1.02 22 -3 -7 12.09 1.40 -22 -3 7 12.37 1.13 22 -3 -7 10.93 1.64 22 -3 -7 6.72 1.53 22 -3 -6 0.88 1.34 23 0 -17 -0.35 0.87 23 0 -16 28.01 1.94 23 0 -16 31.33 2.07 23 0 -16 31.55 2.21 23 0 -16 27.91 2.11 -23 0 16 32.34 1.98 23 0 -15 1.40 1.00 23 0 -15 -2.14 1.51 23 0 -15 -0.06 1.50 -23 0 15 -0.79 1.19 -23 0 15 0.09 1.07 23 0 -15 -3.53 1.75 23 0 -14 333.90 17.86 23 0 -14 349.88 18.01 -23 0 14 347.80 17.90 -23 0 14 378.25 17.94 23 0 -14 368.93 17.99 23 0 -13 2.48 1.83 -23 0 13 -0.85 1.35 -23 0 13 0.41 1.25 23 0 -13 -1.73 1.70 23 0 -12 6.87 2.06 -23 0 12 3.16 1.46 23 0 -11 -0.91 1.99 -23 0 11 0.78 1.42 23 0 -10 22.82 2.53 23 0 -10 26.18 2.41 23 0 -9 2.53 1.86 23 0 -8 33.61 2.77 -23 0 8 37.35 2.40 23 0 -8 29.55 2.61 23 0 -7 1.80 1.79 -23 0 7 -2.62 1.41 -23 0 7 -0.49 1.18 23 0 -7 0.65 1.64 23 0 -6 42.50 2.84 -23 0 6 39.65 2.55 -23 0 6 44.70 2.63 23 0 -6 44.64 2.91 23 0 -6 39.13 2.74 23 0 -5 -0.61 1.36 -23 0 5 -1.31 0.94 -23 0 5 1.89 0.89 23 0 -5 -2.28 1.46 23 0 -5 2.19 1.25 23 0 -4 118.36 6.41 23 0 -3 -0.51 1.32 23 0 -2 5.24 1.15 23 -1 -18 274.67 13.90 23 -1 -17 8.10 1.14 23 -1 -16 39.06 2.48 23 1 -16 41.24 2.43 23 -1 -16 44.38 2.44 23 -1 -16 32.98 2.57 -23 1 16 40.74 2.30 -23 -1 16 37.25 2.31 23 -1 -15 11.18 1.45 23 -1 -15 12.89 1.55 23 1 -15 13.74 1.61 23 1 -15 14.14 1.65 23 -1 -15 13.14 1.60 -23 1 15 10.98 1.33 -23 -1 15 12.47 1.25 23 -1 -15 13.28 2.01 -23 -1 15 13.19 1.40 23 -1 -15 16.39 1.76 23 -1 -14 27.41 2.14 23 -1 -14 28.74 2.26 23 1 -14 30.78 2.31 23 -1 -14 31.15 2.41 23 1 -14 31.77 2.41 23 -1 -14 30.60 2.36 -23 -1 14 30.87 2.02 -23 1 14 31.73 2.08 -23 -1 14 27.44 2.10 23 -1 -14 26.43 2.66 23 -1 -13 0.49 1.22 23 -1 -13 -0.19 1.66 23 1 -13 0.84 1.64 -23 1 13 -1.16 1.29 -23 -1 13 -0.96 1.20 -23 -1 13 2.67 1.29 23 -1 -13 -1.41 2.22 23 -1 -13 1.83 1.88 23 1 -13 2.60 1.75 23 -1 -13 1.72 1.67 23 -1 -12 12.25 1.61 -23 1 12 19.84 1.73 -23 -1 12 14.65 1.69 23 1 -12 18.52 2.19 23 -1 -12 14.89 2.06 23 -1 -11 8.07 1.42 23 1 -11 12.96 2.13 23 -1 -11 13.72 2.08 -23 1 11 13.28 1.60 -23 -1 11 14.74 1.64 23 1 -10 1.74 1.99 23 -1 -10 3.16 1.89 -23 -1 10 0.87 1.27 23 -1 -10 1.25 2.02 23 -1 -10 2.19 1.76 23 1 -10 1.77 1.82 -23 -1 9 -0.97 1.26 23 -1 -9 -1.43 2.02 23 -1 -9 -0.21 1.72 23 1 -9 1.72 1.77 23 1 -8 1.46 1.89 23 -1 -8 7.63 1.84 -23 1 8 2.98 1.32 -23 -1 8 0.27 1.21 -23 -1 8 3.46 1.38 23 -1 -8 -1.27 2.28 23 -1 -8 3.48 1.96 23 -1 -8 5.35 1.71 23 1 -8 0.65 1.74 23 -1 -7 28.58 2.32 23 1 -7 27.20 2.34 -23 -1 7 26.71 1.92 -23 1 7 27.21 1.97 -23 -1 7 25.48 2.00 23 -1 -7 24.21 2.69 23 1 -7 24.13 2.19 23 -1 -7 27.97 2.23 23 -1 -7 29.64 2.37 23 1 -6 17.57 1.78 23 -1 -6 13.60 1.79 -23 1 6 12.10 1.39 -23 -1 6 15.09 1.37 23 -1 -6 10.05 2.08 -23 -1 6 15.21 1.43 23 -1 -6 11.28 1.80 23 -1 -6 16.24 1.66 23 1 -6 14.75 1.62 23 1 -5 14.25 1.24 23 -1 -5 11.76 1.17 23 -1 -5 13.52 1.26 23 1 -5 11.44 1.24 -23 -1 5 11.58 0.98 -23 1 5 12.01 1.00 23 -1 -5 8.75 1.44 23 -1 -5 9.05 1.40 23 -1 -5 11.55 1.28 23 1 -4 20.84 1.91 23 1 -3 233.92 11.96 23 -2 -16 7.16 1.03 23 -2 -15 2.11 1.01 23 -2 -14 -1.09 1.07 23 -2 -14 -0.21 1.11 23 2 -14 -1.52 1.16 23 2 -14 0.09 1.24 23 -2 -14 2.05 1.19 -23 2 14 0.78 0.92 -23 -2 14 1.21 0.83 -23 -2 14 0.68 0.92 23 -2 -14 -0.92 1.50 23 -2 -14 0.61 1.26 23 -2 -13 0.60 1.12 23 2 -13 1.11 1.43 23 -2 -13 1.83 1.29 -23 -2 13 1.00 0.93 -23 -2 13 -1.25 1.04 23 -2 -13 0.35 1.69 23 -2 -13 0.99 1.47 -23 2 13 -1.07 1.02 23 -2 -13 -1.01 1.26 23 2 -13 0.24 1.29 23 2 -12 2.05 1.53 23 -2 -12 -0.45 1.39 -23 -2 12 0.09 1.11 -23 -2 12 0.83 1.00 23 -2 -12 -0.33 1.77 -23 2 12 1.20 1.07 23 2 -11 2.04 1.67 23 -2 -11 2.05 1.51 -23 -2 11 3.19 1.15 23 -2 -11 1.50 1.86 -23 2 11 1.81 1.11 23 2 -10 1.12 1.64 -23 -2 10 1.32 1.02 23 -2 -10 -0.16 1.61 23 -2 -10 -0.05 1.36 23 2 -10 -2.54 1.49 -23 -2 9 16.90 1.43 23 -2 -9 16.09 1.81 23 -2 -9 14.79 1.70 23 2 -9 18.05 1.78 23 2 -8 101.66 5.25 23 -2 -8 100.91 5.20 -23 -2 8 97.29 5.04 23 -2 -8 81.44 5.29 -23 2 8 89.58 5.04 -23 -2 8 91.72 5.05 23 -2 -8 99.50 5.19 23 -2 -8 95.12 5.14 23 2 -8 102.13 5.17 23 2 -7 25.94 1.90 23 -2 -7 24.01 1.88 -23 -2 7 23.90 1.60 -23 2 7 21.12 1.61 -23 -2 7 22.01 1.67 23 -2 -7 22.59 2.14 23 -2 -7 22.47 1.89 23 -2 -7 27.59 1.82 23 2 -7 27.52 1.83 23 2 -6 8.30 1.31 -23 -2 6 6.18 0.83 -24 0 15 -0.49 0.69 -24 0 15 -0.66 0.84 24 0 -15 0.77 1.38 24 0 -15 -0.21 1.18 24 0 -15 -0.53 1.00 24 0 -14 2.75 1.21 -24 0 14 0.80 0.88 -24 0 14 0.74 0.93 24 0 -14 1.84 1.41 24 0 -14 2.22 1.25 24 0 -13 1.08 1.41 -24 0 13 -0.53 0.95 -24 0 13 -0.39 1.05 24 0 -13 -2.14 1.55 24 0 -13 -1.11 1.30 24 0 -12 82.44 4.47 -24 0 12 76.58 4.27 24 0 -11 0.18 1.55 -24 0 11 0.90 1.13 24 0 -11 -1.19 1.66 24 0 -11 -0.44 1.46 -24 0 10 176.88 9.05 24 0 -10 172.96 9.16 24 0 -10 178.14 9.14 24 0 -9 -0.46 1.49 -24 0 9 -0.93 0.96 -24 0 9 1.19 1.09 24 0 -9 -0.70 1.59 24 0 -9 0.46 1.35 24 0 -8 34.55 2.26 -24 0 8 29.90 1.96 -24 0 8 33.71 2.00 24 0 -8 31.41 2.15 24 0 -8 27.97 2.25 24 0 -7 1.25 1.12 -24 0 7 -0.29 0.75 -24 0 7 1.10 0.84 24 0 -7 1.43 1.53 24 0 -7 1.32 1.21 24 0 -7 -0.26 1.03 24 0 -6 44.60 2.70 24 1 -14 5.26 1.18 24 -1 -14 0.64 1.09 -24 -1 14 2.94 0.89 -24 1 14 2.40 0.89 -24 -1 14 2.60 0.77 -24 1 14 2.56 0.78 24 -1 -14 2.87 1.45 24 -1 -14 3.84 1.19 24 -1 -14 3.25 1.05 24 1 -14 2.53 1.08 24 1 -13 23.66 1.88 24 -1 -13 23.89 1.90 -24 -1 13 25.17 1.62 -24 1 13 26.90 1.69 -24 -1 13 21.23 1.67 24 -1 -13 18.07 2.13 24 -1 -13 24.58 1.85 24 -1 -13 25.10 1.94 24 1 -13 27.37 1.87 24 1 -12 -0.80 1.41 24 -1 -12 -0.41 1.30 -24 1 12 -0.66 0.99 24 -1 -12 -0.15 1.73 -24 -1 12 -0.04 1.00 24 1 -11 4.13 1.42 24 -1 -11 1.49 1.33 -24 1 11 0.51 1.01 24 -1 -11 1.64 1.75 -24 -1 11 1.18 1.03 24 -1 -11 2.85 1.44 24 -1 -11 0.74 1.25 24 1 -11 -1.15 1.39 -24 -1 10 1.30 0.94 24 -1 -10 2.62 1.43 24 -1 -10 0.39 1.30 24 1 -10 2.69 1.30 24 1 -9 0.36 1.37 24 -1 -9 2.50 1.35 -24 1 9 3.61 1.02 -24 -1 9 3.79 0.91 24 -1 -9 2.39 1.68 24 -1 -9 2.23 1.36 -24 -1 9 1.97 1.03 24 -1 -9 5.10 1.25 24 1 -9 2.83 1.24 24 1 -8 8.97 1.34 24 -1 -8 9.18 1.28 -24 -1 8 8.34 1.01 -24 1 8 8.66 1.03 -24 -1 8 7.85 0.93 -24 1 8 5.97 0.94 24 -1 -8 4.11 1.59 24 -1 -8 7.50 1.35 24 -1 -8 8.36 1.19 24 1 -8 6.08 1.19 24 1 -6 119.36 6.23 0 0 0 0.00 0.00 TITL lk29db in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 19.571156 5.915402 20.826581 90.0000 115.4416 90.0000 ZERR 1.00 0.000304 0.000058 0.000306 0.0000 0.0019 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 108.00 120.00 8.00 4.00 REM CrysAlisPro recorded range (K): Min=99.7; max=100.2; aver:100.0 TEMP -173 SIZE 0.03 0.05 0.54 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 94051 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.30640(5) 0.24896(14) 0.61183(4) 0.02044(19) Uani 1 1 d . . . . . N1 N 0.18984(5) 0.62022(17) 0.57525(5) 0.0174(2) Uani 1 1 d . . . . . N2 N 0.19989(5) 0.75569(17) 0.72271(5) 0.0184(2) Uani 1 1 d . . . . . C1 C 0.29348(6) 0.35229(19) 0.65635(6) 0.0162(2) Uani 1 1 d . . . . . C2 C 0.24097(6) 0.54115(19) 0.64398(6) 0.0168(2) Uani 1 1 d . . . . . C3 C 0.23959(6) 0.59231(19) 0.70746(6) 0.0159(2) Uani 1 1 d . . . . . C4 C 0.29621(6) 0.44353(19) 0.76548(6) 0.0165(2) Uani 1 1 d . . . . . C5 C 0.32868(6) 0.30157(19) 0.73617(6) 0.0162(2) Uani 1 1 d . . . . . C6 C 0.22771(7) 0.7105(2) 0.53302(6) 0.0216(2) Uani 1 1 d . . . . . H6A H 0.256370 0.588114 0.523163 0.026 Uiso 1 1 calc R U . . . H6B H 0.264045 0.829659 0.560496 0.026 Uiso 1 1 calc R U . . . C7 C 0.17011(7) 0.8088(2) 0.46314(6) 0.0264(3) Uani 1 1 d . . . . . H7A H 0.144919 0.940605 0.472994 0.032 Uiso 1 1 calc R U . . . H7B H 0.196391 0.861622 0.434552 0.032 Uiso 1 1 calc R U . . . C8 C 0.11088(7) 0.6333(2) 0.42104(6) 0.0284(3) Uani 1 1 d . . . . . H8A H 0.135004 0.508577 0.406582 0.034 Uiso 1 1 calc R U . . . H8B H 0.071928 0.703222 0.377522 0.034 Uiso 1 1 calc R U . . . C9 C 0.07408(7) 0.5408(3) 0.46693(6) 0.0292(3) Uani 1 1 d . . . . . H9A H 0.045616 0.662913 0.477176 0.035 Uiso 1 1 calc R U . . . H9B H 0.037863 0.419706 0.440773 0.035 Uiso 1 1 calc R U . . . C10 C 0.13361(7) 0.4469(2) 0.53634(6) 0.0232(3) Uani 1 1 d . . . . . H10A H 0.108876 0.392586 0.566119 0.028 Uiso 1 1 calc R U . . . H10B H 0.159222 0.316648 0.526203 0.028 Uiso 1 1 calc R U . . . C11 C 0.16694(6) 0.9489(2) 0.67526(6) 0.0204(2) Uani 1 1 d . . . . . H11A H 0.190937 0.961869 0.642155 0.025 Uiso 1 1 calc R U . . . H11B H 0.178162 1.089079 0.703934 0.025 Uiso 1 1 calc R U . . . C12 C 0.08161(7) 0.9272(2) 0.63240(7) 0.0241(3) Uani 1 1 d . . . . . H12A H 0.070354 0.801279 0.598048 0.029 Uiso 1 1 calc R U . . . H12B H 0.061295 1.068153 0.605214 0.029 Uiso 1 1 calc R U . . . C13 C 0.04323(7) 0.8832(2) 0.68146(7) 0.0281(3) Uani 1 1 d . . . . . H13A H 0.048411 1.017989 0.711368 0.034 Uiso 1 1 calc R U . . . H13B H -0.011373 0.854473 0.652636 0.034 Uiso 1 1 calc R U . . . C14 C 0.07930(7) 0.6796(2) 0.72877(7) 0.0271(3) Uani 1 1 d . . . . . H14A H 0.069985 0.542281 0.698995 0.033 Uiso 1 1 calc R U . . . H14B H 0.055847 0.656854 0.761978 0.033 Uiso 1 1 calc R U . . . C15 C 0.16452(7) 0.7146(2) 0.77109(6) 0.0234(3) Uani 1 1 d . . . . . H15A H 0.173899 0.845125 0.803533 0.028 Uiso 1 1 calc R U . . . H15B H 0.187271 0.578804 0.800270 0.028 Uiso 1 1 calc R U . . . C16 C 0.31805(6) 0.4737(2) 0.84252(6) 0.0173(2) Uani 1 1 d . . . . . C17 C 0.30930(7) 0.2992(2) 0.88358(6) 0.0215(2) Uani 1 1 d . . . . . H17 H 0.287287 0.159907 0.861771 0.026 Uiso 1 1 calc R U . . . C18 C 0.33268(7) 0.3285(2) 0.95624(6) 0.0257(3) Uani 1 1 d . . . . . H18 H 0.325786 0.210148 0.983740 0.031 Uiso 1 1 calc R U . . . C19 C 0.36599(8) 0.5298(2) 0.98864(6) 0.0271(3) Uani 1 1 d . . . . . H19 H 0.382662 0.548764 1.038398 0.033 Uiso 1 1 calc R U . . . C20 C 0.37488(8) 0.7030(2) 0.94823(6) 0.0268(3) Uani 1 1 d . . . . . H20 H 0.397820 0.840937 0.970412 0.032 Uiso 1 1 calc R U . . . C21 C 0.35047(7) 0.6764(2) 0.87540(6) 0.0211(2) Uani 1 1 d . . . . . H21 H 0.355934 0.797280 0.847927 0.025 Uiso 1 1 calc R U . . . C22 C 0.39087(6) 0.13939(19) 0.77034(6) 0.0164(2) Uani 1 1 d . . . . . C23 C 0.45009(6) 0.1807(2) 0.83774(6) 0.0196(2) Uani 1 1 d . . . . . H23 H 0.450931 0.317305 0.862065 0.023 Uiso 1 1 calc R U . . . C24 C 0.50730(7) 0.0228(2) 0.86883(6) 0.0229(3) Uani 1 1 d . . . . . H24 H 0.547036 0.052197 0.914437 0.027 Uiso 1 1 calc R U . . . C25 C 0.50726(7) -0.1778(2) 0.83419(6) 0.0218(2) Uani 1 1 d . . . . . H25 H 0.546385 -0.285815 0.856145 0.026 Uiso 1 1 calc R U . . . C26 C 0.44960(7) -0.2193(2) 0.76721(6) 0.0200(2) Uani 1 1 d . . . . . H26 H 0.449365 -0.355787 0.743068 0.024 Uiso 1 1 calc R U . . . C27 C 0.39224(6) -0.06163(19) 0.73540(6) 0.0179(2) Uani 1 1 d . . . . . H27 H 0.353382 -0.090608 0.689290 0.021 Uiso 1 1 calc R U . . . 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 0.0226(4) 0.0237(4) 0.0158(4) -0.0028(3) 0.0090(3) 0.0015(3) N1 0.0176(4) 0.0204(5) 0.0133(4) 0.0010(4) 0.0058(4) -0.0014(4) N2 0.0199(5) 0.0202(5) 0.0175(4) 0.0011(4) 0.0102(4) 0.0022(4) C1 0.0154(5) 0.0183(5) 0.0149(5) -0.0012(4) 0.0064(4) -0.0030(4) C2 0.0172(5) 0.0177(5) 0.0154(5) -0.0002(4) 0.0071(4) -0.0013(4) C3 0.0150(5) 0.0164(5) 0.0167(5) 0.0000(4) 0.0073(4) -0.0021(4) C4 0.0175(5) 0.0163(5) 0.0158(5) 0.0002(4) 0.0073(4) -0.0021(4) C5 0.0158(5) 0.0168(5) 0.0146(5) -0.0011(4) 0.0054(4) -0.0029(4) C6 0.0224(6) 0.0259(6) 0.0170(5) 0.0008(5) 0.0089(5) -0.0050(5) C7 0.0324(7) 0.0285(7) 0.0176(5) 0.0041(5) 0.0099(5) -0.0034(5) C8 0.0289(6) 0.0377(7) 0.0140(5) 0.0018(5) 0.0049(5) -0.0032(6) C9 0.0211(6) 0.0411(8) 0.0188(6) 0.0023(6) 0.0024(5) -0.0063(5) C10 0.0207(6) 0.0268(6) 0.0189(5) 0.0020(5) 0.0054(5) -0.0061(5) C11 0.0209(6) 0.0176(6) 0.0237(6) 0.0002(5) 0.0104(5) 0.0012(4) C12 0.0202(6) 0.0255(6) 0.0257(6) 0.0036(5) 0.0089(5) 0.0031(5) C13 0.0196(6) 0.0360(7) 0.0300(6) -0.0021(6) 0.0119(5) 0.0031(5) C14 0.0241(6) 0.0374(7) 0.0251(6) -0.0001(5) 0.0157(5) -0.0017(5) C15 0.0239(6) 0.0313(7) 0.0191(5) 0.0000(5) 0.0132(5) 0.0031(5) C16 0.0171(5) 0.0200(5) 0.0155(5) 0.0013(4) 0.0077(4) 0.0031(4) C17 0.0247(6) 0.0193(6) 0.0218(6) 0.0018(5) 0.0112(5) 0.0013(5) C18 0.0328(7) 0.0272(6) 0.0214(6) 0.0090(5) 0.0156(5) 0.0073(5) C19 0.0356(7) 0.0318(7) 0.0137(5) 0.0022(5) 0.0103(5) 0.0090(6) C20 0.0361(7) 0.0236(6) 0.0186(6) -0.0032(5) 0.0097(5) 0.0013(5) C21 0.0280(6) 0.0192(6) 0.0173(5) 0.0011(5) 0.0107(5) 0.0011(5) C22 0.0173(5) 0.0178(5) 0.0153(5) 0.0014(4) 0.0082(4) -0.0006(4) C23 0.0219(6) 0.0191(6) 0.0170(5) -0.0009(4) 0.0078(5) -0.0003(5) C24 0.0209(6) 0.0277(6) 0.0164(5) 0.0012(5) 0.0044(4) 0.0009(5) C25 0.0207(6) 0.0218(6) 0.0232(6) 0.0058(5) 0.0097(5) 0.0047(5) C26 0.0241(6) 0.0160(5) 0.0227(6) -0.0006(5) 0.0128(5) -0.0001(4) C27 0.0185(5) 0.0189(5) 0.0163(5) -0.0004(4) 0.0076(4) -0.0027(4) 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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 0 0.0781 0 1 0 0.4534 -6 0 13 0.0228 6 0 -14 0.0229 -11 0 0 0.0171 11 0 0 0.0114 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C10 111.17(9) . . ? C2 N1 C6 113.69(9) . . ? C10 N1 C6 111.97(9) . . ? C3 N2 C11 121.75(9) . . ? C3 N2 C15 121.86(10) . . ? C11 N2 C15 113.03(9) . . ? O1 C1 C2 127.27(10) . . ? O1 C1 C5 125.56(10) . . ? C2 C1 C5 107.15(9) . . ? C3 C2 N1 126.88(10) . . ? C3 C2 C1 107.62(9) . . ? N1 C2 C1 124.27(10) . . ? N2 C3 C2 129.29(10) . . ? N2 C3 C4 121.33(9) . . ? C2 C3 C4 109.26(10) . . ? C5 C4 C16 126.33(10) . . ? C5 C4 C3 108.98(9) . . ? C16 C4 C3 124.26(10) . . ? C4 C5 C22 129.84(10) . . ? C4 C5 C1 106.86(9) . . ? C22 C5 C1 123.08(9) . . ? N1 C6 C7 110.70(10) . . ? C8 C7 C6 111.00(11) . . ? C7 C8 C9 109.38(10) . . ? C10 C9 C8 110.61(10) . . ? N1 C10 C9 110.89(10) . . ? N2 C11 C12 112.54(10) . . ? C11 C12 C13 110.63(10) . . ? C14 C13 C12 110.05(10) . . ? C13 C14 C15 110.69(11) . . ? N2 C15 C14 110.25(10) . . ? C21 C16 C17 119.04(10) . . ? C21 C16 C4 119.66(10) . . ? C17 C16 C4 121.26(10) . . ? C18 C17 C16 120.28(11) . . ? C19 C18 C17 120.19(11) . . ? C20 C19 C18 119.74(11) . . ? C19 C20 C21 120.40(12) . . ? C20 C21 C16 120.33(11) . . ? C27 C22 C23 118.36(10) . . ? C27 C22 C5 119.94(10) . . ? C23 C22 C5 121.71(10) . . ? C24 C23 C22 120.21(11) . . ? C23 C24 C25 120.87(11) . . ? C26 C25 C24 119.46(11) . . ? C25 C26 C27 120.13(11) . . ? C26 C27 C22 120.95(10) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.2241(14) . ? N1 C2 1.4278(14) . ? N1 C10 1.4674(15) . ? N1 C6 1.4725(14) . ? N2 C3 1.3604(14) . ? N2 C11 1.4665(15) . ? N2 C15 1.4673(14) . ? C1 C2 1.4639(16) . ? C1 C5 1.5311(14) . ? C2 C3 1.3677(15) . ? C3 C4 1.5205(15) . ? C4 C5 1.3471(16) . ? C4 C16 1.4832(15) . ? C5 C22 1.4711(15) . ? C6 C7 1.5222(16) . ? C7 C8 1.5221(18) . ? C8 C9 1.5241(18) . ? C9 C10 1.5193(16) . ? C11 C12 1.5237(16) . ? C12 C13 1.5282(17) . ? C13 C14 1.5236(19) . ? C14 C15 1.5292(17) . ? C16 C21 1.3915(17) . ? C16 C17 1.3973(16) . ? C17 C18 1.3909(17) . ? C18 C19 1.3858(19) . ? C19 C20 1.3836(19) . ? C20 C21 1.3896(16) . ? C22 C27 1.4003(16) . ? C22 C23 1.4057(15) . ? C23 C24 1.3867(17) . ? C24 C25 1.3887(18) . ? C25 C26 1.3882(17) . ? C26 C27 1.3893(16) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 N1 C2 C3 -101.61(13) . . . . ? C6 N1 C2 C3 130.93(12) . . . . ? C10 N1 C2 C1 64.13(14) . . . . ? C6 N1 C2 C1 -63.32(14) . . . . ? O1 C1 C2 C3 174.95(11) . . . . ? C5 C1 C2 C3 -3.60(12) . . . . ? O1 C1 C2 N1 6.87(18) . . . . ? C5 C1 C2 N1 -171.68(10) . . . . ? C11 N2 C3 C2 -17.82(18) . . . . ? C15 N2 C3 C2 140.04(12) . . . . ? C11 N2 C3 C4 157.75(10) . . . . ? C15 N2 C3 C4 -44.39(15) . . . . ? N1 C2 C3 N2 -12.91(19) . . . . ? C1 C2 C3 N2 179.42(11) . . . . ? N1 C2 C3 C4 171.11(10) . . . . ? C1 C2 C3 C4 3.43(12) . . . . ? N2 C3 C4 C5 -178.34(10) . . . . ? C2 C3 C4 C5 -1.98(13) . . . . ? N2 C3 C4 C16 -5.46(16) . . . . ? C2 C3 C4 C16 170.91(10) . . . . ? C16 C4 C5 C22 1.63(19) . . . . ? C3 C4 C5 C22 174.33(11) . . . . ? C16 C4 C5 C1 -173.04(10) . . . . ? C3 C4 C5 C1 -0.34(12) . . . . ? O1 C1 C5 C4 -176.21(11) . . . . ? C2 C1 C5 C4 2.38(12) . . . . ? O1 C1 C5 C22 8.67(17) . . . . ? C2 C1 C5 C22 -172.74(10) . . . . ? C2 N1 C6 C7 -175.39(10) . . . . ? C10 N1 C6 C7 57.57(13) . . . . ? N1 C6 C7 C8 -56.33(14) . . . . ? C6 C7 C8 C9 55.40(15) . . . . ? C7 C8 C9 C10 -55.62(15) . . . . ? C2 N1 C10 C9 173.48(10) . . . . ? C6 N1 C10 C9 -58.14(13) . . . . ? C8 C9 C10 N1 57.13(15) . . . . ? C3 N2 C11 C12 104.31(12) . . . . ? C15 N2 C11 C12 -55.34(13) . . . . ? N2 C11 C12 C13 53.14(14) . . . . ? C11 C12 C13 C14 -53.73(14) . . . . ? C12 C13 C14 C15 56.39(14) . . . . ? C3 N2 C15 C14 -102.87(13) . . . . ? C11 N2 C15 C14 56.75(13) . . . . ? C13 C14 C15 N2 -57.38(14) . . . . ? C5 C4 C16 C21 112.06(14) . . . . ? C3 C4 C16 C21 -59.58(15) . . . . ? C5 C4 C16 C17 -65.54(16) . . . . ? C3 C4 C16 C17 122.81(12) . . . . ? C21 C16 C17 C18 0.06(17) . . . . ? C4 C16 C17 C18 177.68(11) . . . . ? C16 C17 C18 C19 -1.09(18) . . . . ? C17 C18 C19 C20 0.99(19) . . . . ? C18 C19 C20 C21 0.1(2) . . . . ? C19 C20 C21 C16 -1.18(19) . . . . ? C17 C16 C21 C20 1.07(17) . . . . ? C4 C16 C21 C20 -176.59(11) . . . . ? C4 C5 C22 C27 147.81(12) . . . . ? C1 C5 C22 C27 -38.28(15) . . . . ? C4 C5 C22 C23 -32.56(18) . . . . ? C1 C5 C22 C23 141.35(11) . . . . ? C27 C22 C23 C24 -1.25(17) . . . . ? C5 C22 C23 C24 179.11(11) . . . . ? C22 C23 C24 C25 0.10(18) . . . . ? C23 C24 C25 C26 0.73(18) . . . . ? C24 C25 C26 C27 -0.36(17) . . . . ? C25 C26 C27 C22 -0.83(17) . . . . ? C23 C22 C27 C26 1.62(16) . . . . ? C5 C22 C27 C26 -178.74(10) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0024 -1.0004 0.0004 0.0238 0.0101 0.2593 0.0024 1.0004 -0.0004 -0.0238 -0.0101 -0.2593 -5.7903 0.2689 13.4772 -0.9724 0.2330 0.0093 5.8601 0.0495 -13.5076 0.9683 -0.2321 -0.0923 -11.2675 0.1944 -0.4615 -0.2330 -0.9724 0.0091 11.2675 -0.1944 0.4615 0.2330 0.9724 -0.0091