#------------------------------------------------------------------------------ #$Date: 2020-04-16 04:25:44 +0300 (Thu, 16 Apr 2020) $ #$Revision: 250821 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557803.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_1557803 loop_ _publ_author_name 'Cobos, Katherine' 'Rodr\'iguez, Rafael' 'Domarco, Olaya' 'Fern\'andez, Berta' 'Qui\~no\'a, Emilio' 'Riguera, Ricardo' 'Freire, F\'elix' _publ_section_title ; Polymeric Helical Structures \`a la Carte by Rational Design of Monomers ; _journal_name_full Macromolecules _journal_paper_doi 10.1021/acs.macromol.0c00085 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C16 H12 Cl N O' _chemical_formula_sum 'C16 H12 Cl N O' _chemical_formula_weight 269.72 _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary dual _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.5 _audit_creation_date 2019-06-13T12:39:07-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 95.681(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.98630(10) _cell_length_b 11.0727(3) _cell_length_c 24.1254(7) _cell_measurement_reflns_used 1934 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 78.58 _cell_measurement_theta_min 6.82 _cell_measurement_wavelength 1.54178 _cell_volume 1325.46(6) _computing_cell_refinement 'APPEX3v2018.7-2 (BRUKER AXS, 2005)' _computing_data_collection 'APPEX3v2018.7-2 (BRUKER AXS, 2005)' _computing_data_reduction 'APPEX3v2018.7-2 (BRUKER AXS, 2005)' _computing_molecular_graphics 'Ortep for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker D8 VENTURE PHOTON III-14' _diffrn_measurement_method 'omega and phi' _diffrn_radiation_monochromator 'Incoatec multilayer mirror' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_unetI/netI 0.0192 _diffrn_reflns_Laue_measured_fraction_full 1 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 62788 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.99 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 74.437 _diffrn_reflns_theta_min 1.84 _diffrn_source 'INCOATEC microfocus sealed tube' _diffrn_source_type 'Incoatec I\mS 3.0' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.464 _exptl_absorpt_correction_T_max 0.7747 _exptl_absorpt_correction_T_min 0.6492 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS-2016/2' _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 560 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.15 _refine_diff_density_min -0.138 _refine_diff_density_rms 0.032 _refine_ls_abs_structure_details ; Flack x determined using 2374 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.003(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.06 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 351 _refine_ls_number_reflns 5374 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.06 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0249 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+0.4820P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.058 _reflns_Friedel_coverage 0.89 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.986 _reflns_number_gt 5203 _reflns_number_total 5374 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ma0c00085_si_006.cif _cod_data_source_block shelx _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 1557803 _shelx_estimated_absorpt_t_min 0.567 _shelx_estimated_absorpt_t_max 0.93 _shelx_shelxl_version_number 2018/3 _shelx_res_file ; TITL 19QCA010_a.res in P2(1) shelx.res created by SHELXL-2018/3 at 12:35:47 on 13-Jun-2019 CELL 1.54178 4.9863 11.0727 24.1254 90.000 95.681 90.000 ZERR 2.00 0.0001 0.0003 0.0007 0.000 0.002 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O CL UNIT 64 48 4 4 4 MERG 2 HTAB C7 O1 HTAB N1 Cl1 EQIV $1 x-1, y, z HTAB C10 O1_$1 HTAB C23 O2 HTAB N2 Cl2 OMIT -2 -1 7 FMAP 2 PLAN 20 SIZE 0.030 0.040 0.260 ACTA HTAB 2.00000 BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -173.15 WGHT 0.019900 0.482000 FVAR 0.78522 C1 1 0.277726 0.616121 0.526098 11.00000 0.06135 0.03218 = 0.02818 -0.00278 0.00475 -0.00536 AFIX 163 H1 2 0.192601 0.584862 0.556578 11.00000 -1.20000 AFIX 0 C2 1 0.384116 0.655189 0.488003 11.00000 0.04181 0.02335 = 0.02810 -0.00450 -0.00246 -0.00074 C3 1 0.494817 0.701781 0.439786 11.00000 0.02925 0.02072 = 0.02940 -0.00231 0.00142 0.00249 C4 1 0.700347 0.788221 0.444072 11.00000 0.03028 0.02421 = 0.04058 -0.00585 -0.00231 0.00077 AFIX 43 H4 2 0.770738 0.816935 0.479679 11.00000 -1.20000 AFIX 0 C5 1 0.801725 0.832155 0.396522 11.00000 0.02803 0.02172 = 0.05287 -0.00500 0.00790 -0.00441 AFIX 43 H5 2 0.943022 0.890051 0.399584 11.00000 -1.20000 AFIX 0 C6 1 0.696912 0.791596 0.344665 11.00000 0.03394 0.02258 = 0.04301 -0.00057 0.01450 -0.00132 AFIX 43 H6 2 0.765986 0.822555 0.312213 11.00000 -1.20000 AFIX 0 C7 1 0.492046 0.706222 0.339364 11.00000 0.03014 0.02264 = 0.03034 -0.00052 0.00612 -0.00064 AFIX 43 H7 2 0.419959 0.679609 0.303515 11.00000 -1.20000 AFIX 0 C8 1 0.393226 0.659988 0.386883 11.00000 0.02160 0.01782 = 0.02921 -0.00175 0.00418 0.00173 N1 3 0.187734 0.571969 0.384083 11.00000 0.02245 0.02344 = 0.02267 -0.00102 0.00685 -0.00188 H1N 2 0.105202 0.563522 0.412201 11.00000 0.03017 C9 1 0.142028 0.485295 0.344875 11.00000 0.01706 0.02007 = 0.02162 0.00284 -0.00095 0.00298 O1 4 0.266011 0.473477 0.304073 11.00000 0.02225 0.02776 = 0.02233 -0.00122 0.00448 -0.00183 C10 1 -0.094500 0.398996 0.351552 11.00000 0.01662 0.02701 = 0.02040 0.00303 0.00171 0.00051 AFIX 13 H10 2 -0.250031 0.426961 0.325345 11.00000 -1.20000 AFIX 0 CL1 5 -0.202756 0.402286 0.421215 11.00000 0.02461 0.02727 = 0.02433 0.00231 0.00719 -0.00083 C11 1 -0.031096 0.271751 0.335394 11.00000 0.02112 0.02466 = 0.02324 0.00025 0.00644 -0.00566 C12 1 0.183180 0.208739 0.363514 11.00000 0.02333 0.02613 = 0.03405 -0.00143 -0.00025 -0.00076 AFIX 43 H12 2 0.287277 0.245021 0.394191 11.00000 -1.20000 AFIX 0 C13 1 0.243899 0.093455 0.346699 11.00000 0.03044 0.02827 = 0.04717 0.00184 0.01059 0.00162 AFIX 43 H13 2 0.389387 0.050562 0.366037 11.00000 -1.20000 AFIX 0 C14 1 0.094362 0.040087 0.301919 11.00000 0.04303 0.02427 = 0.04773 -0.00711 0.02246 -0.00960 AFIX 43 H14 2 0.138584 -0.038785 0.290275 11.00000 -1.20000 AFIX 0 C15 1 -0.119735 0.101749 0.274106 11.00000 0.04311 0.03739 = 0.03588 -0.01166 0.01039 -0.01871 AFIX 43 H15 2 -0.223067 0.065171 0.243407 11.00000 -1.20000 AFIX 0 C16 1 -0.183778 0.217865 0.291221 11.00000 0.02658 0.03397 = 0.03013 0.00031 0.00366 -0.00696 AFIX 43 H16 2 -0.332349 0.259815 0.272490 11.00000 -1.20000 AFIX 0 C17 1 0.275904 0.264202 0.181364 11.00000 0.02522 0.03217 = 0.02878 0.00627 0.00412 -0.00087 AFIX 163 H17 2 0.192945 0.270635 0.215032 11.00000 -1.20000 AFIX 0 C18 1 0.379501 0.256169 0.139318 11.00000 0.01888 0.01754 = 0.02737 0.00360 -0.00066 -0.00078 C19 1 0.513932 0.250971 0.089234 11.00000 0.01863 0.02038 = 0.02322 0.00182 -0.00128 0.00356 C20 1 0.459231 0.157392 0.050778 11.00000 0.02082 0.01983 = 0.02731 0.00193 -0.00252 0.00211 AFIX 43 H20 2 0.325297 0.099085 0.056737 11.00000 -1.20000 AFIX 0 C21 1 0.599548 0.149190 0.003925 11.00000 0.02780 0.02500 = 0.02621 -0.00405 -0.00476 0.00577 AFIX 43 H21 2 0.565595 0.084258 -0.021543 11.00000 -1.20000 AFIX 0 C22 1 0.789407 0.236447 -0.005375 11.00000 0.02288 0.03313 = 0.02194 -0.00420 0.00131 0.00684 AFIX 43 H22 2 0.885149 0.230782 -0.037417 11.00000 -1.20000 AFIX 0 C23 1 0.841993 0.332160 0.031452 11.00000 0.01930 0.02705 = 0.02551 -0.00052 0.00136 0.00091 AFIX 43 H23 2 0.969657 0.392297 0.024094 11.00000 -1.20000 AFIX 0 C24 1 0.706904 0.339447 0.079082 11.00000 0.01631 0.01973 = 0.02234 -0.00182 -0.00011 0.00365 N2 3 0.750340 0.432015 0.119174 11.00000 0.01663 0.02322 = 0.02238 -0.00357 0.00527 -0.00065 H2N 2 0.632570 0.439736 0.143627 11.00000 0.02978 C25 1 0.963015 0.507003 0.127874 11.00000 0.01579 0.01773 = 0.02254 0.00203 0.00210 0.00259 O2 4 1.151687 0.514678 0.099105 11.00000 0.02073 0.02187 = 0.02882 -0.00051 0.00904 -0.00186 C26 1 0.970741 0.592018 0.178294 11.00000 0.01498 0.02143 = 0.02061 0.00126 0.00109 0.00090 AFIX 13 H26 2 1.148580 0.580090 0.200651 11.00000 -1.20000 AFIX 0 CL2 5 0.710522 0.560431 0.223751 11.00000 0.02020 0.02514 = 0.01945 0.00172 0.00397 0.00131 C27 1 0.955691 0.722713 0.160309 11.00000 0.01776 0.01914 = 0.02014 -0.00021 0.00350 0.00238 C28 1 0.745986 0.760737 0.121720 11.00000 0.02112 0.02137 = 0.02769 -0.00048 -0.00085 -0.00044 AFIX 43 H28 2 0.610676 0.705228 0.107678 11.00000 -1.20000 AFIX 0 C29 1 0.735658 0.880340 0.103851 11.00000 0.02481 0.02261 = 0.03104 0.00278 -0.00052 0.00439 AFIX 43 H29 2 0.594300 0.906117 0.077180 11.00000 -1.20000 AFIX 0 C30 1 0.930381 0.961845 0.124764 11.00000 0.02851 0.01884 = 0.03288 0.00196 0.00682 0.00215 AFIX 43 H30 2 0.921364 1.043629 0.112823 11.00000 -1.20000 AFIX 0 C31 1 1.139025 0.923922 0.163236 11.00000 0.02385 0.02307 = 0.03628 -0.00260 0.00307 -0.00450 AFIX 43 H31 2 1.273192 0.979730 0.177519 11.00000 -1.20000 AFIX 0 C32 1 1.151617 0.804479 0.180833 11.00000 0.02136 0.02467 = 0.02689 -0.00012 0.00065 0.00083 AFIX 43 H32 2 1.294965 0.778672 0.207028 11.00000 -1.20000 AFIX 0 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM 19QCA010_a.res in P2(1) REM wR2 = 0.0580, GooF = S = 1.060, Restrained GooF = 1.060 for all data REM R1 = 0.0249 for 5203 Fo > 4sig(Fo) and 0.0266 for all 5374 data REM 351 parameters refined using 1 restraints END WGHT 0.0199 0.4820 REM Instructions for potential hydrogen bonds HTAB C7 O1 HTAB C7 Cl2 HTAB N1 Cl1 HTAB C10 O1_$1 HTAB C10 Cl2_$1 HTAB C23 O2 HTAB N2 Cl2 REM Highest difference peak 0.150, deepest hole -0.138, 1-sigma level 0.032 Q1 1 0.2878 0.3152 0.1514 11.00000 0.05 0.15 Q2 1 0.0319 0.4316 0.3540 11.00000 0.05 0.15 Q3 1 0.9592 0.5569 0.1504 11.00000 0.05 0.13 Q4 1 0.2023 0.2421 0.1518 11.00000 0.05 0.13 Q5 1 0.6004 0.7377 0.4391 11.00000 0.05 0.13 Q6 1 0.4504 0.6877 0.4150 11.00000 0.05 0.12 Q7 1 0.9350 0.6621 0.1669 11.00000 0.05 0.12 Q8 1 0.3622 0.5872 0.4996 11.00000 0.05 0.12 Q9 1 0.4200 0.2995 0.1694 11.00000 0.05 0.12 Q10 1 -0.0628 0.3314 0.3430 11.00000 0.05 0.12 Q11 1 -0.1667 0.1547 0.2940 11.00000 0.05 0.12 Q12 1 0.5806 0.2998 0.0808 11.00000 0.05 0.12 Q13 1 0.5114 0.2831 0.1909 11.00000 0.05 0.11 Q14 1 1.3750 0.7231 0.2392 11.00000 0.05 0.11 Q15 1 0.4344 0.1567 0.0076 11.00000 0.05 0.11 Q16 1 0.8851 0.7405 0.1364 11.00000 0.05 0.11 Q17 1 0.2446 0.6753 0.4991 11.00000 0.05 0.11 Q18 1 0.6552 0.7225 0.3441 11.00000 0.05 0.11 Q19 1 -0.1204 0.4040 0.3790 11.00000 0.05 0.11 Q20 1 -0.4046 0.3238 0.2534 11.00000 0.05 0.11 ; _shelx_res_checksum 523 _shelx_hkl_file ; -1 0 0 877.21 24.50 -1 0 0 896.81 27.00 -1 0 0 918.41 27.90 1 0 0 888.91 22.10 2 0 0 4367.16 91.59 2 0 0 4275.97 86.19 -2 0 0 4108.69 91.99 -2 0 0 4231.88 98.89 -2 0 0 4060.89 101.19 3 0 0 352.96 19.10 -3 0 0 351.96 17.30 -3 0 0 348.77 18.20 -3 0 0 342.77 16.80 -3 0 0 321.97 25.70 3 0 0 339.67 22.60 -3 0 0 335.27 15.80 -3 0 0 334.17 22.60 -3 0 0 328.77 27.30 3 0 0 340.77 22.70 -4 0 0 302.77 16.30 -4 0 0 339.27 18.90 -4 0 0 328.07 18.30 -4 0 0 313.97 15.90 -4 0 0 345.77 19.70 -4 0 0 347.87 33.40 -4 0 0 311.37 15.70 -4 0 0 328.37 18.80 -4 0 0 327.97 16.10 -4 0 0 337.17 17.40 -4 0 0 265.77 24.80 -4 0 0 298.27 15.50 -4 0 0 322.97 18.00 -4 0 0 253.97 24.80 -4 0 0 290.97 16.30 -4 0 0 327.67 17.60 -4 0 0 333.17 17.00 4 0 0 299.37 29.10 -4 0 0 334.07 17.80 -5 0 0 -2.20 3.50 -5 0 0 10.60 3.30 -5 0 0 2.50 3.40 -5 0 0 -14.60 20.40 -5 0 0 7.20 3.30 -5 0 0 1.20 3.20 -5 0 0 -0.80 3.40 -5 0 0 0.70 3.00 -5 0 0 4.40 2.70 -5 0 0 0.40 2.80 -5 0 0 11.80 4.30 -5 0 0 2.10 3.30 -6 0 0 6.20 2.90 -6 0 0 8.10 3.00 -6 0 0 0.60 2.30 -6 0 0 2.50 2.30 0 -1 0 0.00 0.70 0 -1 0 0.90 1.00 0 -1 0 1.40 1.10 0 -1 0 0.90 1.10 0 1 0 0.60 0.90 0 1 0 -0.60 0.90 0 1 0 0.00 0.80 0 1 0 -0.30 0.70 -1 -1 0 197.68 11.90 -1 -1 0 203.88 11.30 1 -1 0 203.88 7.80 1 -1 0 194.48 10.30 -1 -1 0 199.48 10.30 -1 1 0 157.88 11.20 -1 1 0 166.48 12.20 1 1 0 163.28 6.40 -1 1 0 168.78 7.90 -1 1 0 161.48 7.10 1 1 0 156.78 7.60 2 -1 0 538.95 22.60 -2 -1 0 525.45 24.80 -2 -1 0 541.75 25.40 -2 -1 0 527.85 30.80 2 1 0 601.04 26.30 -2 1 0 574.94 29.90 2 1 0 565.74 18.90 -2 1 0 562.84 23.80 -3 -1 0 302.37 23.60 -3 -1 0 320.87 23.20 3 -1 0 311.47 20.30 -3 -1 0 301.77 17.00 3 -1 0 315.47 23.30 -3 -1 0 315.67 15.80 -3 -1 0 297.37 16.10 -3 -1 0 299.87 15.10 -3 -1 0 296.97 25.60 -3 -1 0 301.47 15.30 -3 1 0 360.46 16.30 -3 1 0 380.86 17.50 -3 1 0 355.86 16.50 3 1 0 363.56 21.70 -3 1 0 364.06 28.60 -3 1 0 354.46 16.90 -3 1 0 349.96 17.70 -3 1 0 362.26 29.40 3 1 0 372.36 26.60 3 1 0 374.16 16.20 -3 1 0 363.16 17.60 -3 1 0 387.86 23.80 -4 -1 0 425.46 23.60 -4 -1 0 437.66 37.00 -4 -1 0 456.75 23.70 -4 -1 0 399.46 18.70 4 -1 0 546.75 41.50 -4 -1 0 435.56 20.60 -4 -1 0 450.75 30.90 -4 -1 0 439.96 20.20 -4 -1 0 410.26 20.00 -4 -1 0 430.96 18.70 -4 -1 0 444.46 19.50 -4 -1 0 433.56 21.40 -4 -1 0 450.85 20.90 -4 -1 0 424.46 18.10 -4 -1 0 419.36 21.90 -4 -1 0 466.55 20.00 -4 -1 0 429.86 21.70 -4 -1 0 425.76 20.10 -4 1 0 454.75 22.10 -4 1 0 422.56 22.40 -4 1 0 468.75 24.10 4 1 0 473.85 35.20 -4 1 0 410.56 22.30 -4 1 0 381.96 20.70 -4 1 0 414.16 22.40 -4 1 0 461.95 22.70 -4 1 0 448.96 38.50 -4 1 0 408.96 21.30 -4 1 0 418.16 22.60 -5 -1 0 166.48 12.20 -5 -1 0 171.68 12.00 -5 -1 0 153.28 11.70 -5 -1 0 156.18 10.20 -5 -1 0 168.28 13.50 -5 -1 0 155.58 9.90 -5 -1 0 164.38 12.60 -5 -1 0 176.28 11.70 -5 -1 0 144.39 10.20 -5 -1 0 155.78 10.80 -5 -1 0 169.98 12.00 -5 1 0 176.48 13.30 -5 1 0 187.88 13.10 -5 1 0 179.48 12.70 -5 1 0 175.48 12.00 -5 1 0 189.48 12.90 -5 1 0 191.98 12.60 -5 1 0 158.38 12.20 -5 1 0 185.98 12.70 -5 1 0 182.58 12.90 -6 -1 0 23.30 3.80 -6 -1 0 23.00 4.60 -6 -1 0 23.90 3.90 -6 1 0 24.90 3.90 -6 1 0 17.00 3.20 -6 1 0 20.30 3.30 -6 1 0 20.30 3.30 0 -2 0 450.85 15.30 0 -2 0 469.55 15.60 0 -2 0 492.35 15.80 0 -2 0 449.36 15.70 0 -2 0 469.95 17.40 0 2 0 560.54 18.20 0 2 0 511.55 16.70 0 2 0 538.75 17.00 0 2 0 517.55 14.30 0 2 0 487.85 16.80 -1 -2 0 3569.74 68.19 -1 -2 0 3538.25 69.79 1 -2 0 3676.53 72.99 -1 -2 0 3603.84 76.49 1 -2 0 3506.95 74.69 -1 -2 0 3594.44 71.49 -1 -2 0 3404.76 76.49 1 -2 0 3560.44 70.89 -1 2 0 3643.84 73.99 1 2 0 3676.73 70.99 1 2 0 3721.63 77.59 1 2 0 3805.62 73.19 -1 2 0 3905.61 83.79 -1 2 0 3873.21 68.89 -1 2 0 3715.43 82.49 1 2 0 3771.42 69.99 -1 2 0 3661.73 77.29 2 -2 0 1300.77 31.70 -2 -2 0 1173.18 44.30 2 -2 0 1238.78 40.50 -2 -2 0 1211.08 38.00 2 -2 0 1215.78 41.10 2 2 0 1165.38 33.30 -2 2 0 1151.98 30.10 -2 2 0 1104.09 45.10 -2 2 0 1123.09 32.00 -2 2 0 1141.69 31.50 2 2 0 1112.99 27.90 -2 2 0 1130.09 45.20 2 2 0 1165.38 27.70 2 2 0 1116.89 38.60 3 -2 0 139.89 15.00 -3 -2 0 115.69 9.50 -3 -2 0 123.79 9.40 -3 -2 0 119.79 10.30 -3 -2 0 131.19 23.80 -3 -2 0 110.09 9.30 -3 -2 0 138.79 13.70 -3 -2 0 120.59 11.30 3 -2 0 140.69 18.80 -3 -2 0 135.59 15.50 -3 -2 0 129.69 11.10 -3 -2 0 108.99 8.90 -3 -2 0 99.49 15.70 3 2 0 126.79 15.60 -3 2 0 114.79 9.10 -3 2 0 120.29 18.10 3 2 0 113.59 11.10 -3 2 0 106.69 10.50 -3 2 0 127.59 10.60 -3 2 0 126.59 10.20 -3 2 0 134.89 22.10 -4 -2 0 25.30 8.50 -4 -2 0 28.10 11.60 -4 -2 0 19.70 5.10 -4 -2 0 16.90 7.30 4 -2 0 28.60 10.30 -4 -2 0 26.80 6.20 -4 -2 0 32.20 7.10 -4 -2 0 23.00 5.60 -4 -2 0 26.30 6.90 -4 -2 0 29.50 10.10 -4 -2 0 18.90 7.20 -4 -2 0 26.30 7.20 -4 -2 0 36.80 8.30 -4 -2 0 22.90 5.60 -4 -2 0 26.50 10.50 -4 2 0 9.80 5.10 -4 2 0 23.60 7.40 -4 2 0 17.10 5.30 -4 2 0 17.60 5.80 -4 2 0 15.60 5.40 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7.50 -4 8 0 42.60 8.10 -4 8 0 41.30 7.30 -4 8 0 46.20 6.70 -5 -8 0 62.99 5.80 -5 -8 0 63.99 5.10 -5 -8 0 56.79 4.40 -5 -8 0 57.09 4.60 -5 -8 0 65.19 5.10 -5 8 0 60.69 4.60 -5 8 0 58.89 4.70 -5 8 0 64.79 5.90 -5 8 0 61.09 5.10 -5 8 0 58.89 4.20 -5 8 0 61.39 6.10 0 -9 0 -6.50 4.40 0 -9 0 -10.60 10.70 0 -9 0 -3.20 3.50 0 -9 0 -7.50 3.60 0 -9 0 -3.50 4.40 0 -9 0 9.10 5.00 0 -9 0 1.40 3.80 0 -9 0 2.00 3.00 0 -9 0 4.10 4.30 0 -9 0 -2.50 2.70 0 9 0 0.70 3.10 0 9 0 6.00 4.00 0 9 0 -2.50 3.70 0 9 0 -0.70 2.30 0 9 0 -1.70 3.00 0 9 0 1.60 3.70 0 9 0 -2.50 2.50 0 9 0 2.20 2.60 -1 -9 0 317.47 15.70 1 -9 0 333.87 20.30 1 -9 0 300.17 18.40 1 -9 0 333.07 31.00 -1 -9 0 322.17 19.30 1 -9 0 360.76 23.70 -1 -9 0 336.97 27.10 -1 -9 0 390.46 33.50 -1 -9 0 265.67 23.50 -1 -9 0 395.26 24.50 1 -9 0 321.97 27.70 -1 -9 0 289.07 21.70 -1 -9 0 338.77 18.90 -1 -9 0 331.77 39.00 -1 -9 0 319.37 19.20 1 -9 0 384.56 26.90 1 -9 0 339.87 23.80 1 -9 0 321.37 20.10 1 -9 0 336.27 22.40 -1 -9 0 339.57 16.20 -1 9 0 356.06 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4.40 2 -6 -26 29.40 4.40 -2 -6 26 42.70 4.80 -2 -6 26 44.20 5.30 -2 6 26 36.80 4.10 -2 6 26 38.50 4.20 1 -6 -26 208.88 10.40 -1 -6 26 208.48 11.20 -1 -6 26 221.38 10.80 -1 -6 26 223.48 10.40 -1 -6 26 212.28 11.20 1 -6 -26 187.88 10.70 -1 6 26 218.08 11.00 1 6 -26 197.28 11.20 1 6 -26 205.48 11.00 -1 6 26 212.88 11.20 0 -6 -26 29.10 4.60 0 -6 26 29.20 5.00 0 -6 -26 27.10 4.60 0 -6 -26 33.00 3.80 0 -6 26 28.00 5.40 0 -6 -26 27.10 3.60 0 6 26 43.00 5.50 0 6 -26 43.20 6.40 0 6 -26 34.60 5.70 0 6 26 36.80 5.90 0 6 26 36.20 5.20 0 6 -26 45.10 5.70 0 6 -26 50.09 5.60 1 -6 26 61.39 7.50 1 -6 26 62.79 7.00 -1 -6 -26 68.39 5.70 -1 -6 -26 66.09 5.20 -1 6 -26 73.59 5.90 -1 6 -26 71.59 5.60 3 0 -27 139.79 10.30 3 0 -27 142.19 10.00 -3 0 27 147.89 8.90 3 0 -27 116.69 7.80 3 0 -27 145.89 8.00 3 0 -27 129.09 9.00 -3 0 27 144.59 8.50 -2 0 27 30.00 5.30 2 0 -27 49.90 5.70 2 0 -27 46.90 6.80 2 0 -27 53.29 6.80 -2 0 27 28.10 5.30 -2 0 27 35.90 5.20 -2 0 27 37.30 5.80 2 0 -27 35.60 6.20 -2 0 27 36.50 4.90 -2 0 27 31.20 5.30 2 0 -27 30.50 7.40 1 0 -27 100.29 9.50 -1 0 27 120.99 10.80 -1 0 27 125.19 10.30 1 0 -27 109.49 11.00 1 0 -27 127.39 10.60 1 0 -27 103.69 10.50 -1 0 27 102.39 10.20 1 0 -27 92.19 13.70 -1 0 27 111.19 10.40 0 0 -27 14.10 4.30 0 0 -27 13.70 4.80 0 0 27 18.10 5.60 0 0 27 9.70 4.20 0 0 27 13.90 4.40 0 0 27 12.10 4.20 0 0 -27 14.70 5.10 0 0 -27 12.80 5.10 1 0 27 7.20 3.50 -1 0 -27 -1.30 3.30 1 0 27 7.20 3.60 -1 0 -27 2.20 2.60 -2 0 -27 53.19 5.50 -2 0 -27 48.10 5.50 -2 0 -27 54.89 6.10 -2 0 -27 43.90 6.10 -3 -1 27 7.10 3.20 3 -1 -27 8.20 3.40 3 -1 -27 6.40 3.00 3 -1 -27 2.00 2.40 -3 -1 27 4.50 3.20 3 -1 -27 10.90 3.40 3 1 -27 8.10 3.30 3 1 -27 5.20 3.40 3 1 -27 -0.40 2.60 3 1 -27 3.20 2.90 3 1 -27 1.70 2.60 -3 1 27 5.20 3.20 -3 1 27 1.40 3.00 2 -1 -27 176.28 12.60 2 -1 -27 197.68 12.10 2 -1 -27 199.78 21.20 -2 -1 27 184.58 10.40 -2 -1 27 196.88 11.30 -2 -1 27 190.28 9.70 -2 -1 27 195.48 11.40 2 -1 -27 191.18 9.50 2 -1 -27 193.18 10.90 2 -1 -27 193.48 10.90 -2 -1 27 181.38 9.90 -2 -1 27 186.88 10.10 2 1 -27 201.28 14.80 2 1 -27 215.38 12.60 -2 1 27 198.98 10.50 -2 1 27 204.78 10.30 -2 1 27 206.38 12.30 2 1 -27 210.08 10.50 2 1 -27 194.18 13.20 2 1 -27 244.48 19.70 -2 1 27 206.48 12.30 2 1 -27 226.38 19.10 1 -1 -27 14.50 5.50 1 -1 -27 19.10 5.00 1 -1 -27 16.00 4.40 -1 -1 27 15.60 5.70 1 -1 -27 14.50 5.40 -1 -1 27 14.50 5.20 -1 -1 27 6.50 4.00 -1 -1 27 7.50 4.00 -1 1 27 22.40 6.90 1 1 -27 16.50 4.40 1 1 -27 12.90 5.30 -1 1 27 9.40 5.10 1 1 -27 22.60 6.40 -1 1 27 23.30 6.30 1 1 -27 19.80 10.90 1 1 -27 19.30 5.10 -1 1 27 15.60 5.90 0 -1 -27 80.79 8.20 0 -1 -27 65.49 11.60 0 -1 27 69.99 7.00 0 -1 27 75.09 10.20 0 -1 27 71.49 7.30 0 -1 27 85.49 10.20 0 -1 -27 73.69 8.60 0 -1 -27 59.29 9.60 0 1 27 78.49 10.60 0 1 -27 64.89 9.40 0 1 -27 88.19 8.90 0 1 -27 79.49 10.60 0 1 -27 84.79 9.20 0 1 27 69.29 11.40 -1 -1 -27 25.40 5.00 1 -1 27 35.00 5.60 -1 -1 -27 24.10 5.20 -1 1 -27 21.30 5.00 1 1 27 24.90 5.00 1 1 27 29.40 5.60 -1 1 -27 23.10 5.40 -2 -1 -27 57.69 4.90 -2 -1 -27 49.60 5.00 -2 -1 -27 61.79 5.40 -2 -1 -27 50.29 5.00 -2 1 -27 47.10 5.20 -2 1 -27 59.99 5.30 -2 1 -27 60.99 5.30 -2 1 -27 43.90 5.10 3 -2 -27 55.89 6.30 -3 -2 27 54.29 5.00 -3 -2 27 51.09 5.20 3 -2 -27 43.10 5.60 3 2 -27 44.10 5.10 3 2 -27 55.49 5.80 -3 2 27 54.09 5.40 -3 2 27 61.59 5.50 3 2 -27 52.29 6.20 3 2 -27 61.89 6.20 -2 -2 27 30.40 5.00 -2 -2 27 16.30 3.60 -2 -2 27 24.00 3.80 2 -2 -27 18.90 5.10 -2 -2 27 14.00 3.80 -2 -2 27 18.60 4.10 2 -2 -27 24.10 5.20 -2 -2 27 29.20 4.80 -2 2 27 26.10 4.20 2 2 -27 33.30 5.80 2 2 -27 28.10 5.90 -2 2 27 24.50 5.60 -2 2 27 31.90 5.80 2 2 -27 24.90 9.40 -2 2 27 25.40 4.50 2 2 -27 22.10 5.10 2 2 -27 20.10 4.00 2 2 -27 32.90 6.10 1 -2 -27 76.39 9.80 -1 -2 27 68.79 8.20 1 -2 -27 57.99 8.60 1 -2 -27 55.19 8.70 -1 -2 27 70.19 6.60 -1 -2 27 56.49 6.50 1 -2 -27 78.49 9.90 -1 -2 27 81.39 9.20 1 2 -27 70.39 9.00 1 2 -27 70.29 4.70 1 2 -27 74.19 8.40 -1 2 27 60.59 8.40 -1 2 27 73.49 9.20 1 2 -27 53.69 8.30 1 2 -27 65.29 9.70 1 2 -27 44.70 9.20 0 -2 -27 67.39 7.90 0 -2 27 83.29 8.90 0 -2 -27 74.29 7.90 0 -2 -27 71.19 8.20 0 -2 27 75.49 8.20 0 -2 -27 79.69 8.20 0 2 -27 74.19 11.20 0 2 27 125.59 10.60 0 2 -27 97.59 9.60 0 2 -27 101.69 9.20 0 2 -27 108.39 10.80 0 2 -27 88.19 10.50 0 2 27 107.29 10.10 0 2 -27 105.59 9.00 -1 -2 -27 88.49 8.00 1 -2 27 96.89 8.80 1 -2 27 86.69 7.50 -1 -2 -27 81.79 8.00 1 2 27 64.09 7.80 -1 2 -27 81.49 7.50 -1 2 -27 74.99 7.60 1 2 27 76.99 7.90 -2 -2 -27 5.70 2.20 -2 -2 -27 3.30 2.10 -2 -2 -27 6.90 2.10 -2 -2 -27 5.50 2.00 -2 2 -27 10.70 2.60 -2 2 -27 7.30 2.40 -2 2 -27 9.60 2.30 -2 2 -27 12.30 3.10 -2 -3 27 165.68 10.30 -2 -3 27 160.08 7.50 2 -3 -27 166.28 10.40 -2 -3 27 157.08 8.30 -2 -3 27 154.68 8.20 -2 -3 27 171.58 10.20 -2 -3 27 154.08 7.80 2 -3 -27 151.78 10.70 2 3 -27 165.08 10.40 2 3 -27 144.29 9.50 2 3 -27 164.08 10.20 -2 3 27 166.78 10.50 2 3 -27 155.68 11.10 -2 3 27 170.48 8.40 -2 3 27 158.58 8.50 -2 3 27 161.98 10.40 2 3 -27 147.19 10.20 -1 -3 27 72.59 8.70 -1 -3 27 74.59 9.30 -1 -3 27 96.99 8.50 -1 -3 27 88.99 8.60 1 -3 -27 95.09 8.60 1 -3 -27 80.19 8.80 1 3 -27 83.59 5.00 1 3 -27 94.59 8.30 1 3 -27 82.89 9.20 1 3 -27 94.79 9.00 -1 3 27 103.09 9.10 -1 3 27 98.99 8.70 1 3 -27 82.79 11.90 1 3 -27 93.09 8.00 0 -3 -27 147.59 9.60 0 -3 -27 132.69 10.00 0 -3 -27 140.09 10.40 0 -3 -27 156.28 10.70 0 -3 27 146.79 10.60 0 -3 27 143.69 11.20 0 3 27 133.79 10.70 0 3 -27 160.98 12.80 0 3 -27 145.49 11.70 0 3 -27 162.98 10.70 0 3 -27 129.69 11.50 0 3 27 143.69 10.70 0 3 -27 155.38 11.00 0 3 -27 149.69 11.40 1 -3 27 255.67 13.00 -1 -3 -27 262.97 12.70 1 -3 27 259.67 12.70 1 -3 27 276.97 13.40 -1 -3 -27 255.57 13.00 1 3 27 252.57 12.70 1 3 27 259.37 12.50 -1 3 -27 236.98 11.40 -1 3 -27 261.87 12.90 -1 3 -27 236.78 10.70 -1 3 -27 249.97 13.00 -2 -4 27 7.70 3.10 2 -4 -27 2.10 2.20 -2 -4 27 9.50 2.00 2 -4 -27 8.90 2.90 -2 -4 27 6.90 1.90 -2 -4 27 4.50 3.00 2 4 -27 4.20 2.80 2 4 -27 -3.60 2.40 2 4 -27 6.10 2.80 2 4 -27 1.80 1.70 -2 4 27 -2.20 2.20 2 4 -27 -1.10 2.60 -2 4 27 2.40 2.10 -2 4 27 1.70 1.90 -2 4 27 0.80 2.50 1 -4 -27 6.80 3.10 1 -4 -27 3.70 2.80 -1 -4 27 4.60 2.60 -1 -4 27 7.50 3.30 1 4 -27 6.10 3.50 -1 4 27 9.30 3.80 1 4 -27 14.60 4.10 1 4 -27 7.80 3.40 1 4 -27 12.90 3.80 -1 4 27 10.10 4.60 0 -4 27 142.19 9.70 0 -4 -27 143.89 11.70 0 -4 -27 125.99 10.30 0 -4 -27 140.29 8.30 0 -4 -27 129.69 8.80 0 4 27 129.89 9.70 0 4 -27 123.79 9.10 0 4 27 124.79 9.90 0 4 -27 126.39 9.70 0 4 -27 108.59 9.70 0 4 -27 105.59 8.70 1 -4 27 16.00 3.60 -1 -4 -27 17.50 4.30 -1 -4 -27 18.30 4.70 1 -4 27 10.80 3.70 1 -4 27 7.40 3.10 -1 4 -27 8.50 3.30 -1 4 -27 10.50 3.80 1 4 27 1.10 3.20 1 4 27 3.50 3.70 -2 -5 27 150.48 7.90 -2 -5 27 167.68 8.40 2 -5 -27 154.58 9.20 2 -5 -27 186.08 8.90 2 5 -27 202.48 14.40 -2 5 27 170.98 10.10 -2 5 27 172.78 10.00 2 5 -27 214.98 14.30 -1 -5 27 107.79 7.20 1 -5 -27 96.79 7.90 -1 -5 27 110.39 8.30 -1 -5 27 106.89 7.70 1 -5 -27 99.69 7.20 -1 -5 27 115.99 8.40 1 5 -27 87.79 7.60 -1 5 27 107.99 7.60 -1 5 27 100.69 7.80 1 5 -27 88.89 7.60 0 -5 27 18.50 4.10 0 -5 -27 23.70 3.60 0 -5 -27 20.80 3.40 0 -5 -27 22.20 4.40 0 -5 27 26.80 4.50 0 -5 -27 21.50 4.40 0 5 -27 17.20 3.50 0 5 27 18.20 4.20 0 5 -27 18.10 3.70 0 5 27 18.00 3.80 1 -5 27 68.89 8.10 -1 -5 -27 78.99 5.80 -1 -5 -27 79.99 6.20 1 -5 27 73.69 9.50 -1 5 -27 88.69 6.40 -1 5 -27 82.69 6.20 1 -6 -27 81.49 5.20 -1 -6 27 77.69 5.30 -1 -6 27 88.99 5.30 1 -6 -27 64.39 5.30 -1 -6 27 65.89 5.30 -1 -6 27 66.19 5.60 -1 6 27 75.59 5.30 -1 6 27 72.09 5.50 -1 6 27 76.49 6.20 0 -6 27 5.50 2.10 0 -6 27 2.00 2.20 0 -6 27 0.50 2.00 0 -6 27 4.40 3.00 0 6 27 -3.90 2.10 0 6 27 -2.70 2.00 -2 0 28 12.90 3.70 2 0 -28 10.30 3.20 2 0 -28 12.60 4.00 -2 0 28 9.40 3.30 -2 0 28 6.80 2.10 2 0 -28 12.40 4.00 2 0 -28 4.90 3.20 -2 0 28 6.40 2.30 -1 0 28 49.60 6.30 1 0 -28 37.30 6.40 1 0 -28 43.10 6.50 -1 0 28 44.60 6.20 -1 0 28 41.60 6.30 -1 0 28 42.50 5.90 1 0 -28 44.90 6.70 1 0 -28 37.10 7.10 0 0 -28 15.80 4.20 0 0 -28 28.00 4.90 0 0 28 20.80 4.90 0 0 28 20.40 4.80 0 0 -28 31.30 4.80 0 0 28 17.00 4.40 0 0 -28 19.30 4.40 0 0 28 19.40 4.20 1 0 28 63.19 6.40 1 0 28 78.49 6.80 -1 0 -28 64.89 6.30 -1 0 -28 65.09 6.80 2 -1 -28 9.70 3.30 2 -1 -28 19.30 4.10 -2 -1 28 19.10 4.20 -2 -1 28 16.60 3.30 2 -1 -28 16.80 4.30 2 -1 -28 20.40 5.40 -2 -1 28 19.80 3.40 -2 -1 28 16.70 3.90 -2 -1 28 16.70 3.60 -2 -1 28 23.40 4.20 2 1 -28 31.90 5.00 2 1 -28 21.20 4.60 -2 1 28 23.00 4.90 2 1 -28 17.50 4.50 2 1 -28 24.30 4.60 -2 1 28 25.30 4.80 -2 1 28 24.30 3.50 -2 1 28 22.70 3.50 1 -1 -28 17.20 4.10 -1 -1 28 10.30 3.40 -1 -1 28 19.30 5.10 1 -1 -28 14.20 4.00 -1 -1 28 23.90 5.20 -1 -1 28 14.40 3.90 1 1 -28 12.50 3.90 1 1 -28 18.40 4.40 -1 1 28 19.70 4.30 1 1 -28 25.90 5.00 -1 1 28 19.10 4.40 -1 1 28 13.90 4.40 -1 1 28 19.10 4.20 1 1 -28 20.10 4.70 0 -1 28 17.00 5.30 0 -1 -28 18.40 4.20 0 -1 -28 13.80 3.50 0 -1 -28 9.50 3.20 0 -1 -28 15.10 4.40 0 -1 28 20.60 5.20 0 1 -28 34.60 5.90 0 1 28 32.20 6.50 0 1 -28 37.50 5.50 0 1 -28 19.00 4.40 0 1 28 20.90 5.00 0 1 28 25.30 4.60 0 1 28 25.80 5.60 0 1 -28 24.30 5.10 1 -1 28 64.69 7.00 1 -1 28 61.19 6.10 -1 -1 -28 64.29 6.90 -1 -1 -28 65.69 6.50 1 1 28 57.59 6.30 -1 1 -28 72.09 6.40 -1 1 -28 63.79 6.60 1 1 28 60.19 6.60 -2 -2 28 24.70 4.00 2 -2 -28 21.80 4.60 -2 -2 28 22.40 3.90 -2 -2 28 22.20 3.70 -2 -2 28 26.10 2.90 -2 -2 28 25.50 3.30 -2 -2 28 24.10 3.80 2 -2 -28 27.80 4.60 2 2 -28 32.60 5.00 2 2 -28 29.90 4.90 2 2 -28 27.90 5.40 -2 2 28 29.40 5.10 -2 2 28 21.90 4.70 2 2 -28 27.00 5.20 -2 2 28 27.40 3.40 -2 2 28 24.90 3.60 1 -2 -28 252.87 14.30 -1 -2 28 268.87 10.70 -1 -2 28 264.47 10.40 1 -2 -28 272.27 13.50 -1 -2 28 259.37 13.30 -1 -2 28 268.07 13.00 1 2 -28 218.38 13.50 -1 2 28 246.68 13.40 1 2 -28 235.18 11.90 -1 2 28 236.78 12.50 1 2 -28 239.88 12.10 -1 2 28 254.37 13.10 -1 2 28 238.68 12.40 1 2 -28 261.97 13.30 0 -2 28 15.00 4.20 0 -2 28 12.40 3.60 0 -2 -28 5.90 3.40 0 -2 -28 14.20 3.00 0 -2 -28 13.10 3.50 0 -2 -28 7.30 3.20 0 2 -28 4.60 3.10 0 2 28 25.40 5.00 0 2 -28 9.60 3.20 0 2 28 14.70 4.30 0 2 -28 4.70 2.90 0 2 -28 12.80 3.20 1 -2 28 161.98 7.90 1 -2 28 154.38 9.30 1 -2 28 154.88 8.90 -1 -2 -28 149.88 10.60 -1 -2 -28 161.98 10.80 1 2 28 154.18 9.40 -1 2 -28 114.79 9.60 -1 2 -28 111.89 9.80 2 -3 -28 56.09 6.70 -2 -3 28 64.09 5.20 2 -3 -28 58.59 7.30 -2 -3 28 52.69 5.20 2 3 -28 52.29 6.40 2 3 -28 55.29 6.30 -2 3 28 59.89 5.90 2 3 -28 48.70 6.30 -2 3 28 44.50 6.00 -2 3 28 48.70 3.40 -2 3 28 51.19 3.30 2 3 -28 51.89 3.20 2 3 -28 45.70 5.70 -1 -3 28 14.40 3.40 -1 -3 28 12.70 3.30 1 -3 -28 13.30 3.80 1 -3 -28 12.90 3.40 1 3 -28 8.90 3.90 1 3 -28 12.50 4.20 -1 3 28 12.50 4.20 -1 3 28 10.90 4.00 -1 3 28 14.90 3.60 1 3 -28 11.80 3.20 1 3 -28 13.00 3.40 -1 3 28 11.80 3.40 0 -3 -28 82.39 7.40 0 -3 28 80.19 7.40 0 -3 -28 74.19 6.30 0 -3 28 80.49 7.00 0 -3 -28 79.79 6.80 0 -3 -28 60.79 6.40 0 3 28 75.89 7.40 0 3 -28 62.39 6.60 0 3 28 70.99 7.00 0 3 -28 63.29 6.50 -1 -3 -28 25.80 3.90 1 -3 28 18.80 4.60 -1 -3 -28 21.60 3.70 1 -3 28 17.40 5.00 -1 3 -28 15.30 3.40 1 3 28 9.60 3.80 -1 3 -28 17.50 3.10 1 3 28 18.40 4.70 -2 -4 28 96.29 7.70 2 -4 -28 89.49 6.60 -2 -4 28 101.79 8.30 2 -4 -28 105.99 6.50 -1 -4 28 138.99 8.40 -1 -4 28 134.69 7.60 1 -4 -28 143.39 8.20 -1 4 28 128.49 7.90 1 4 -28 126.59 9.00 1 4 -28 130.19 8.90 -1 4 28 132.79 8.50 -1 4 28 125.69 8.30 -1 4 28 128.39 8.80 0 -4 -28 77.69 5.40 0 -4 28 96.89 8.40 0 -4 -28 86.79 6.70 0 -4 -28 94.89 6.60 0 -4 28 90.19 8.60 0 -4 -28 91.29 5.70 0 4 28 99.29 8.60 0 4 28 104.89 8.30 0 4 -28 76.59 8.10 0 4 -28 74.39 7.40 1 -5 -28 69.09 5.40 1 -5 -28 76.79 5.20 -1 -5 28 66.69 5.40 -1 -5 28 76.79 5.20 -1 -5 28 72.59 4.90 -1 5 28 74.39 5.20 -1 5 28 69.89 5.30 -1 5 28 63.49 5.70 -1 5 28 68.89 5.60 -2 0 29 6.20 2.70 -2 0 29 3.90 2.40 2 0 -29 1.80 1.70 2 0 -29 4.20 2.20 1 0 -29 1.60 2.00 1 0 -29 1.90 2.00 -1 0 29 2.00 2.40 -1 0 29 -3.00 2.30 -1 0 29 0.50 2.50 -1 0 29 0.90 2.10 0 0 -29 0.60 2.00 0 0 29 2.50 2.70 0 0 -29 -1.00 2.70 0 0 -29 -0.20 2.50 0 0 29 0.90 1.90 0 0 -29 0.40 1.90 1 0 29 18.90 5.80 1 0 29 20.60 5.40 -1 0 -29 7.80 2.40 -1 0 -29 5.70 2.50 2 -1 -29 0.90 2.00 -2 -1 29 -1.30 2.50 -2 -1 29 -0.40 2.60 2 -1 -29 0.60 1.70 -2 1 29 4.40 2.30 2 1 -29 0.30 1.50 -2 1 29 7.20 3.20 2 1 -29 4.10 2.00 -1 -1 29 60.69 5.60 1 -1 -29 61.09 6.50 -1 -1 29 46.30 6.00 -1 -1 29 43.80 6.30 1 -1 -29 71.39 6.40 -1 -1 29 71.89 6.40 -1 1 29 64.89 5.90 -1 1 29 64.29 6.20 1 1 -29 66.49 6.10 0 -1 -29 53.79 5.90 0 -1 29 66.79 6.20 0 -1 29 67.09 6.80 0 -1 -29 47.60 5.80 0 -1 -29 48.00 4.80 0 -1 -29 57.89 4.80 0 1 -29 62.39 6.00 0 1 29 70.69 6.50 0 1 29 73.19 7.10 0 1 29 50.39 5.80 0 1 -29 56.69 5.80 0 1 29 49.90 5.50 0 1 -29 55.19 5.10 0 1 -29 63.39 5.10 -1 -1 -29 151.18 8.20 -1 -1 -29 158.38 8.10 -1 1 -29 155.18 8.40 -1 1 -29 161.68 8.30 2 -2 -29 29.70 4.00 2 -2 -29 29.80 4.10 2 2 -29 23.20 3.80 -2 2 29 28.80 4.20 -2 2 29 31.50 4.60 2 2 -29 27.90 4.10 1 -2 -29 85.09 7.20 1 -2 -29 101.19 7.20 -1 -2 29 107.59 6.80 -1 -2 29 105.19 7.20 -1 2 29 99.69 7.10 -1 2 29 111.59 7.30 1 2 -29 113.39 7.60 1 2 -29 97.89 7.80 0 -2 -29 11.20 3.20 0 -2 -29 10.30 3.80 0 -2 -29 13.70 2.70 0 -2 -29 11.10 2.60 0 2 29 14.80 4.30 0 2 29 7.80 3.20 0 2 29 13.90 3.50 0 2 -29 19.00 5.10 0 2 -29 14.30 5.00 0 2 29 15.00 4.20 -1 -3 29 92.39 6.10 -1 -3 29 91.29 6.20 1 -3 -29 91.19 6.70 -1 -3 29 79.59 6.20 -1 -3 29 78.29 6.30 1 -3 -29 102.99 6.40 1 3 -29 87.99 6.60 -1 3 29 89.99 6.40 -1 3 29 93.79 6.50 -1 3 29 87.19 5.90 1 3 -29 79.89 6.60 -1 3 29 98.89 6.80 0 -3 29 16.80 3.50 0 -3 -29 13.50 5.90 0 -3 -29 17.70 6.70 0 -3 29 15.00 3.20 0 3 29 25.50 3.80 0 3 29 15.00 3.70 0 3 29 28.30 4.00 -1 0 30 194.78 8.80 -1 0 30 198.48 8.40 1 0 -30 203.08 8.80 0 0 30 31.70 4.60 0 0 30 32.10 4.00 -1 -1 30 30.70 3.40 -1 -1 30 30.70 3.60 1 -1 -30 22.00 3.40 1 -1 -30 23.20 3.60 -1 1 30 29.00 3.40 -1 1 30 25.30 4.20 -1 1 30 27.10 3.50 -1 1 30 30.00 4.40 1 1 -30 27.30 3.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 44053 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2777(7) 0.6161(3) 0.52610(12) 0.0405(7) Uani 1 1 d . . . . . H1 H 0.192601 0.584862 0.556578 0.049 Uiso 1 1 calc R U . . . C2 C 0.3841(6) 0.6552(2) 0.48800(11) 0.0315(6) Uani 1 1 d . . . . . C3 C 0.4948(5) 0.7018(2) 0.43979(10) 0.0266(5) Uani 1 1 d . . . . . C4 C 0.7003(5) 0.7882(2) 0.44407(12) 0.0321(6) Uani 1 1 d . . . . . H4 H 0.770738 0.816935 0.479679 0.038 Uiso 1 1 calc R U . . . C5 C 0.8017(5) 0.8322(2) 0.39652(13) 0.0339(6) Uani 1 1 d . . . . . H5 H 0.943022 0.890051 0.399584 0.041 Uiso 1 1 calc R U . . . C6 C 0.6969(5) 0.7916(2) 0.34467(12) 0.0325(6) Uani 1 1 d . . . . . H6 H 0.765986 0.822555 0.312213 0.039 Uiso 1 1 calc R U . . . C7 C 0.4920(5) 0.7062(2) 0.33936(11) 0.0275(5) Uani 1 1 d . . . . . H7 H 0.419959 0.679609 0.303515 0.033 Uiso 1 1 calc R U . . . C8 C 0.3932(5) 0.6600(2) 0.38688(10) 0.0228(5) Uani 1 1 d . . . . . N1 N 0.1877(4) 0.57197(18) 0.38408(8) 0.0225(4) Uani 1 1 d . . . . . H1N H 0.105(6) 0.564(3) 0.4122(12) 0.030(7) Uiso 1 1 d . . . . . C9 C 0.1420(4) 0.4853(2) 0.34488(9) 0.0198(4) Uani 1 1 d . . . . . O1 O 0.2660(3) 0.47348(15) 0.30407(7) 0.0240(3) Uani 1 1 d . . . . . C10 C -0.0945(4) 0.3990(2) 0.35155(9) 0.0214(4) Uani 1 1 d . . . . . H10 H -0.250031 0.426961 0.325345 0.026 Uiso 1 1 calc R U . . . Cl1 Cl -0.20276(11) 0.40229(5) 0.42121(2) 0.02509(12) Uani 1 1 d . . . . . C11 C -0.0311(5) 0.2718(2) 0.33539(9) 0.0227(5) Uani 1 1 d . . . . . C12 C 0.1832(5) 0.2087(2) 0.36351(11) 0.0280(5) Uani 1 1 d . . . . . H12 H 0.287277 0.245021 0.394191 0.034 Uiso 1 1 calc R U . . . C13 C 0.2439(6) 0.0935(2) 0.34670(12) 0.0348(6) Uani 1 1 d . . . . . H13 H 0.389387 0.050562 0.366037 0.042 Uiso 1 1 calc R U . . . C14 C 0.0944(6) 0.0401(2) 0.30192(12) 0.0371(6) Uani 1 1 d . . . . . H14 H 0.138584 -0.038785 0.290275 0.045 Uiso 1 1 calc R U . . . C15 C -0.1197(6) 0.1017(3) 0.27411(12) 0.0384(7) Uani 1 1 d . . . . . H15 H -0.223067 0.065171 0.243407 0.046 Uiso 1 1 calc R U . . . C16 C -0.1838(5) 0.2179(2) 0.29122(10) 0.0302(5) Uani 1 1 d . . . . . H16 H -0.332349 0.259815 0.27249 0.036 Uiso 1 1 calc R U . . . C17 C 0.2759(5) 0.2642(2) 0.18136(11) 0.0286(5) Uani 1 1 d . . . . . H17 H 0.192945 0.270635 0.215032 0.034 Uiso 1 1 calc R U . . . C18 C 0.3795(4) 0.2562(2) 0.13932(9) 0.0215(5) Uani 1 1 d . . . . . C19 C 0.5139(4) 0.2510(2) 0.08923(9) 0.0210(4) Uani 1 1 d . . . . . C20 C 0.4592(5) 0.1574(2) 0.05078(10) 0.0230(5) Uani 1 1 d . . . . . H20 H 0.325297 0.099085 0.056737 0.028 Uiso 1 1 calc R U . . . C21 C 0.5995(5) 0.1492(2) 0.00393(10) 0.0268(5) Uani 1 1 d . . . . . H21 H 0.565595 0.084258 -0.021543 0.032 Uiso 1 1 calc R U . . . C22 C 0.7894(5) 0.2364(2) -0.00537(10) 0.0260(5) Uani 1 1 d . . . . . H22 H 0.885149 0.230782 -0.037417 0.031 Uiso 1 1 calc R U . . . C23 C 0.8420(5) 0.3322(2) 0.03145(10) 0.0240(5) Uani 1 1 d . . . . . H23 H 0.969657 0.392297 0.024094 0.029 Uiso 1 1 calc R U . . . C24 C 0.7069(4) 0.3394(2) 0.07908(9) 0.0196(4) Uani 1 1 d . . . . . N2 N 0.7503(4) 0.43201(17) 0.11917(8) 0.0205(4) Uani 1 1 d . . . . . H2N H 0.633(6) 0.440(3) 0.1436(12) 0.030(8) Uiso 1 1 d . . . . . C25 C 0.9630(4) 0.5070(2) 0.12787(9) 0.0187(4) Uani 1 1 d . . . . . O2 O 1.1517(3) 0.51468(14) 0.09911(7) 0.0234(3) Uani 1 1 d . . . . . C26 C 0.9707(4) 0.5920(2) 0.17829(9) 0.0190(4) Uani 1 1 d . . . . . H26 H 1.14858 0.58009 0.200651 0.023 Uiso 1 1 calc R U . . . Cl2 Cl 0.71052(10) 0.56043(5) 0.22375(2) 0.02146(11) Uani 1 1 d . . . . . C27 C 0.9557(4) 0.7227(2) 0.16031(9) 0.0189(4) Uani 1 1 d . . . . . C28 C 0.7460(5) 0.7607(2) 0.12172(10) 0.0236(5) Uani 1 1 d . . . . . H28 H 0.610676 0.705228 0.107678 0.028 Uiso 1 1 calc R U . . . C29 C 0.7357(5) 0.8803(2) 0.10385(10) 0.0264(5) Uani 1 1 d . . . . . H29 H 0.5943 0.906117 0.07718 0.032 Uiso 1 1 calc R U . . . C30 C 0.9304(5) 0.9618(2) 0.12476(10) 0.0265(5) Uani 1 1 d . . . . . H30 H 0.921364 1.043629 0.112823 0.032 Uiso 1 1 calc R U . . . C31 C 1.1390(5) 0.9239(2) 0.16324(10) 0.0277(5) Uani 1 1 d . . . . . H31 H 1.273192 0.97973 0.177519 0.033 Uiso 1 1 calc R U . . . C32 C 1.1516(5) 0.8045(2) 0.18083(10) 0.0244(5) Uani 1 1 d . . . . . H32 H 1.294965 0.778672 0.207028 0.029 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 C1 0.0613(19) 0.0322(15) 0.0282(14) -0.0028(11) 0.0048(13) -0.0054(13) C2 0.0418(15) 0.0234(13) 0.0281(13) -0.0045(10) -0.0025(11) -0.0007(11) C3 0.0292(13) 0.0207(12) 0.0294(12) -0.0023(10) 0.0014(10) 0.0025(9) C4 0.0303(13) 0.0242(13) 0.0406(15) -0.0059(11) -0.0023(11) 0.0008(10) C5 0.0280(13) 0.0217(13) 0.0529(17) -0.0050(12) 0.0079(12) -0.0044(10) C6 0.0339(14) 0.0226(13) 0.0430(15) -0.0006(11) 0.0145(11) -0.0013(10) C7 0.0301(13) 0.0226(12) 0.0303(13) -0.0005(10) 0.0061(10) -0.0006(10) C8 0.0216(11) 0.0178(11) 0.0292(12) -0.0018(9) 0.0042(9) 0.0017(9) N1 0.0225(9) 0.0234(10) 0.0227(9) -0.0010(8) 0.0069(7) -0.0019(8) C9 0.0171(10) 0.0201(11) 0.0216(11) 0.0028(9) -0.0010(8) 0.0030(8) O1 0.0222(8) 0.0278(9) 0.0223(8) -0.0012(7) 0.0045(6) -0.0018(6) C10 0.0166(10) 0.0270(11) 0.0204(10) 0.0030(10) 0.0017(8) 0.0005(9) Cl1 0.0246(3) 0.0273(3) 0.0243(3) 0.0023(2) 0.0072(2) -0.0008(2) C11 0.0211(11) 0.0247(12) 0.0232(11) 0.0002(9) 0.0064(9) -0.0057(9) C12 0.0233(12) 0.0261(13) 0.0341(13) -0.0014(11) -0.0002(10) -0.0008(10) C13 0.0304(13) 0.0283(14) 0.0472(16) 0.0018(11) 0.0106(11) 0.0016(10) C14 0.0430(15) 0.0243(14) 0.0477(15) -0.0071(11) 0.0225(12) -0.0096(11) C15 0.0431(16) 0.0374(15) 0.0359(15) -0.0117(12) 0.0104(12) -0.0187(13) C16 0.0266(13) 0.0340(14) 0.0301(13) 0.0003(11) 0.0037(10) -0.0070(11) C17 0.0252(12) 0.0322(14) 0.0288(13) 0.0063(11) 0.0041(10) -0.0009(10) C18 0.0189(11) 0.0175(11) 0.0274(12) 0.0036(9) -0.0007(9) -0.0008(8) C19 0.0186(10) 0.0204(11) 0.0232(11) 0.0018(9) -0.0013(8) 0.0036(8) C20 0.0208(11) 0.0198(11) 0.0273(12) 0.0019(9) -0.0025(9) 0.0021(9) C21 0.0278(12) 0.0250(12) 0.0262(12) -0.0041(10) -0.0048(10) 0.0058(10) C22 0.0229(11) 0.0331(13) 0.0219(11) -0.0042(10) 0.0013(9) 0.0068(10) C23 0.0193(11) 0.0270(12) 0.0255(12) -0.0005(10) 0.0014(9) 0.0009(9) C24 0.0163(10) 0.0197(11) 0.0223(11) -0.0018(9) -0.0001(8) 0.0037(8) N2 0.0166(9) 0.0232(10) 0.0224(9) -0.0036(7) 0.0053(7) -0.0006(7) C25 0.0158(10) 0.0177(10) 0.0225(10) 0.0020(8) 0.0021(8) 0.0026(8) O2 0.0207(8) 0.0219(8) 0.0288(8) -0.0005(7) 0.0090(6) -0.0019(6) C26 0.0150(10) 0.0214(11) 0.0206(10) 0.0013(8) 0.0011(8) 0.0009(8) Cl2 0.0202(2) 0.0251(3) 0.0194(2) 0.0017(2) 0.00397(18) 0.0013(2) C27 0.0178(10) 0.0191(11) 0.0201(10) -0.0002(8) 0.0035(8) 0.0024(8) C28 0.0211(11) 0.0214(12) 0.0277(12) -0.0005(9) -0.0009(9) -0.0004(9) C29 0.0248(12) 0.0226(13) 0.0310(12) 0.0028(9) -0.0005(9) 0.0044(9) C30 0.0285(12) 0.0188(11) 0.0329(13) 0.0020(10) 0.0068(10) 0.0021(9) C31 0.0239(12) 0.0231(13) 0.0363(13) -0.0026(10) 0.0031(9) -0.0045(9) C32 0.0214(12) 0.0247(12) 0.0269(12) -0.0001(9) 0.0007(9) 0.0008(9) 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1 180 . . ? C1 C2 C3 176.0(3) . . ? C4 C3 C8 119.2(2) . . ? C4 C3 C2 121.7(2) . . ? C8 C3 C2 119.1(2) . . ? C5 C4 C3 120.2(2) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C6 C5 C4 119.9(2) . . ? C6 C5 H5 120 . . ? C4 C5 H5 120 . . ? C5 C6 C7 120.9(3) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C7 C8 119.5(2) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C8 C3 120.2(2) . . ? C7 C8 N1 122.0(2) . . ? C3 C8 N1 117.8(2) . . ? C9 N1 C8 126.6(2) . . ? C9 N1 H1N 115(2) . . ? C8 N1 H1N 117(2) . . ? O1 C9 N1 125.3(2) . . ? O1 C9 C10 118.2(2) . . ? N1 C9 C10 116.47(19) . . ? C11 C10 C9 111.82(17) . . ? C11 C10 Cl1 110.37(16) . . ? C9 C10 Cl1 112.68(16) . . ? C11 C10 H10 107.2 . . ? C9 C10 H10 107.2 . . ? Cl1 C10 H10 107.2 . . ? C16 C11 C12 119.7(2) . . ? C16 C11 C10 119.4(2) . . ? C12 C11 C10 120.9(2) . . ? C13 C12 C11 119.9(2) . . ? C13 C12 H12 120 . . ? C11 C12 H12 120 . . ? C12 C13 C14 120.5(3) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 119.9(3) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 119.9(3) . . ? C14 C15 H15 120 . . ? C16 C15 H15 120 . . ? C11 C16 C15 120.0(3) . . ? C11 C16 H16 120 . . ? C15 C16 H16 120 . . ? C18 C17 H17 180 . . ? C17 C18 C19 177.3(3) . . ? C20 C19 C24 119.4(2) . . ? C20 C19 C18 120.6(2) . . ? C24 C19 C18 120.0(2) . . ? C21 C20 C19 120.4(2) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C20 119.5(2) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 121.1(2) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C24 C23 C22 119.7(2) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 N2 123.7(2) . . ? C23 C24 C19 119.8(2) . . ? N2 C24 C19 116.5(2) . . ? C25 N2 C24 128.29(19) . . ? C25 N2 H2N 113.9(19) . . ? C24 N2 H2N 117.7(19) . . ? O2 C25 N2 126.2(2) . . ? O2 C25 C26 116.5(2) . . ? N2 C25 C26 117.32(19) . . ? C27 C26 C25 111.29(18) . . ? C27 C26 Cl2 109.89(15) . . ? C25 C26 Cl2 113.41(15) . . ? C27 C26 H26 107.3 . . ? C25 C26 H26 107.3 . . ? Cl2 C26 H26 107.3 . . ? C32 C27 C28 119.8(2) . . ? C32 C27 C26 120.6(2) . . ? C28 C27 C26 119.6(2) . . ? C29 C28 C27 119.8(2) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C30 C29 C28 120.3(2) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C31 119.9(2) . . ? C29 C30 H30 120 . . ? C31 C30 H30 120 . . ? C32 C31 C30 120.0(2) . . ? C32 C31 H31 120 . . ? C30 C31 H31 120 . . ? C27 C32 C31 120.2(2) . . ? C27 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? 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 C1 C2 1.187(4) . ? C1 H1 0.95 . ? C2 C3 1.432(4) . ? C3 C4 1.399(4) . ? C3 C8 1.404(3) . ? C4 C5 1.387(4) . ? C4 H4 0.95 . ? C5 C6 1.382(4) . ? C5 H5 0.95 . ? C6 C7 1.388(4) . ? C6 H6 0.95 . ? C7 C8 1.390(3) . ? C7 H7 0.95 . ? C8 N1 1.411(3) . ? N1 C9 1.351(3) . ? N1 H1N 0.83(3) . ? C9 O1 1.220(3) . ? C9 C10 1.539(3) . ? C10 C11 1.504(3) . ? C10 Cl1 1.816(2) . ? C10 H10 1 . ? C11 C16 1.382(3) . ? C11 C12 1.395(3) . ? C12 C13 1.382(4) . ? C12 H12 0.95 . ? C13 C14 1.383(4) . ? C13 H13 0.95 . ? C14 C15 1.384(4) . ? C14 H14 0.95 . ? C15 C16 1.397(4) . ? C15 H15 0.95 . ? C16 H16 0.95 . ? C17 C18 1.186(4) . ? C17 H17 0.95 . ? C18 C19 1.440(3) . ? C19 C20 1.400(3) . ? C19 C24 1.411(3) . ? C20 C21 1.390(3) . ? C20 H20 0.95 . ? C21 C22 1.386(4) . ? C21 H21 0.95 . ? C22 C23 1.391(3) . ? C22 H22 0.95 . ? C23 C24 1.391(3) . ? C23 H23 0.95 . ? C24 N2 1.411(3) . ? N2 C25 1.347(3) . ? N2 H2N 0.88(3) . ? C25 O2 1.226(3) . ? C25 C26 1.536(3) . ? C26 C27 1.511(3) . ? C26 Cl2 1.814(2) . ? C26 H26 1 . ? C27 C32 1.387(3) . ? C27 C28 1.394(3) . ? C28 C29 1.392(3) . ? C28 H28 0.95 . ? C29 C30 1.384(4) . ? C29 H29 0.95 . ? C30 C31 1.389(3) . ? C30 H30 0.95 . ? C31 C32 1.389(4) . ? C31 H31 0.95 . ? C32 H32 0.95 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C7 H7 O1 0.95 2.41 2.906(3) 112.4 . yes N1 H1N Cl1 0.83(3) 2.38(3) 2.910(2) 122(3) . yes C10 H10 O1 1 2.47 3.382(3) 151.2 1_455 yes C23 H23 O2 0.95 2.37 2.938(3) 118.1 . yes N2 H2N Cl2 0.88(3) 2.35(3) 2.9199(19) 123(2) . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 C3 C4 C5 0.1(4) . . . . ? C2 C3 C4 C5 -179.5(2) . . . . ? C3 C4 C5 C6 0.9(4) . . . . ? C4 C5 C6 C7 -0.6(4) . . . . ? C5 C6 C7 C8 -0.7(4) . . . . ? C6 C7 C8 C3 1.7(4) . . . . ? C6 C7 C8 N1 -179.2(2) . . . . ? C4 C3 C8 C7 -1.4(4) . . . . ? C2 C3 C8 C7 178.2(2) . . . . ? C4 C3 C8 N1 179.4(2) . . . . ? C2 C3 C8 N1 -0.9(3) . . . . ? C7 C8 N1 C9 31.2(4) . . . . ? C3 C8 N1 C9 -149.7(2) . . . . ? C8 N1 C9 O1 -3.5(4) . . . . ? C8 N1 C9 C10 179.4(2) . . . . ? O1 C9 C10 C11 40.5(3) . . . . ? N1 C9 C10 C11 -142.1(2) . . . . ? O1 C9 C10 Cl1 165.56(17) . . . . ? N1 C9 C10 Cl1 -17.1(3) . . . . ? C9 C10 C11 C16 -117.6(2) . . . . ? Cl1 C10 C11 C16 116.1(2) . . . . ? C9 C10 C11 C12 60.9(3) . . . . ? Cl1 C10 C11 C12 -65.4(2) . . . . ? C16 C11 C12 C13 0.8(4) . . . . ? C10 C11 C12 C13 -177.7(2) . . . . ? C11 C12 C13 C14 0.3(4) . . . . ? C12 C13 C14 C15 -0.8(4) . . . . ? C13 C14 C15 C16 0.2(4) . . . . ? C12 C11 C16 C15 -1.4(4) . . . . ? C10 C11 C16 C15 177.1(2) . . . . ? C14 C15 C16 C11 0.9(4) . . . . ? C24 C19 C20 C21 2.1(3) . . . . ? C18 C19 C20 C21 -176.6(2) . . . . ? C19 C20 C21 C22 -1.8(3) . . . . ? C20 C21 C22 C23 0.0(4) . . . . ? C21 C22 C23 C24 1.5(3) . . . . ? C22 C23 C24 N2 178.9(2) . . . . ? C22 C23 C24 C19 -1.1(3) . . . . ? C20 C19 C24 C23 -0.6(3) . . . . ? C18 C19 C24 C23 178.1(2) . . . . ? C20 C19 C24 N2 179.32(19) . . . . ? C18 C19 C24 N2 -1.9(3) . . . . ? C23 C24 N2 C25 -19.1(4) . . . . ? C19 C24 N2 C25 161.0(2) . . . . ? C24 N2 C25 O2 6.2(4) . . . . ? C24 N2 C25 C26 -174.3(2) . . . . ? O2 C25 C26 C27 63.5(3) . . . . ? N2 C25 C26 C27 -116.0(2) . . . . ? O2 C25 C26 Cl2 -171.94(16) . . . . ? N2 C25 C26 Cl2 8.5(2) . . . . ? C25 C26 C27 C32 -125.0(2) . . . . ? Cl2 C26 C27 C32 108.5(2) . . . . ? C25 C26 C27 C28 53.6(3) . . . . ? Cl2 C26 C27 C28 -72.9(2) . . . . ? C32 C27 C28 C29 0.4(3) . . . . ? C26 C27 C28 C29 -178.2(2) . . . . ? C27 C28 C29 C30 -0.9(4) . . . . ? C28 C29 C30 C31 0.8(4) . . . . ? C29 C30 C31 C32 -0.2(4) . . . . ? C28 C27 C32 C31 0.2(3) . . . . ? C26 C27 C32 C31 178.7(2) . . . . ? C30 C31 C32 C27 -0.3(4) . . . . ?