#------------------------------------------------------------------------------ #$Date: 2023-10-10 04:19:25 +0200 (Tue, 10 Oct 2023) $ #$Revision: 286864 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022894.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2022894 loop_ _publ_author_name 'Rajendrakumar, Satyasree' 'Surampudi Venkata Sai Durga, Anuja' 'Balasubramanian, Sridhar' _publ_section_title ; Strategic synthon approach in obtaining cocrystals and cocrystal polymorphs of a high-Z′ system deferiprone -- an anti-thalassemia drug ; _journal_coeditor_code LO5093 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials' _journal_page_first 946 _journal_page_last 964 _journal_paper_doi 10.1107/S205252062100980X _journal_volume 77 _journal_year 2021 _chemical_formula_moiety '2(C7 H9 N O2), C6 H6 O2' _chemical_formula_sum 'C20 H24 N2 O6' _chemical_formula_weight 388.41 _chemical_name_common 'bis(Deferiprone) Resorcinol (2:1)' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 100.6076(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.71471(15) _cell_length_b 7.32566(10) _cell_length_c 22.0867(3) _cell_measurement_reflns_used 7177 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.49 _cell_measurement_theta_min 2.63 _cell_volume 1863.04(4) _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'DIAMOND (Brandenburg & Putz, 2005)' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON-100' _diffrn_measurement_method '\w and \f' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_unetI/netI 0.0674 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 16659 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.515 _diffrn_reflns_theta_min 2.149 _diffrn_source microfocus _exptl_absorpt_coefficient_mu 0.103 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.5702 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker, 2016' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.385 _exptl_crystal_description block _exptl_crystal_F_000 824 _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.180 _refine_diff_density_max 0.353 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.070 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 273 _refine_ls_number_reflns 5665 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0540 _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^)+(0.0401P)^2^+1.3362P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1161 _refine_ls_wR_factor_ref 0.1316 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4023 _reflns_number_total 5665 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lo5093sup1.cif _cod_data_source_block KA951_0mdef-res_2_1 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2022894 _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 0.964 _shelx_estimated_absorpt_t_max 0.982 _shelx_res_file ; TITL KA951_0m_a.res in P2(1)/n KA951_0m.res created by SHELXL-2018/3 at 17:31:37 on 15-Apr-2020 CELL 0.71073 11.71471 7.32566 22.08667 90.0000 100.6076 90.0000 ZERR 4.00 0.00015 0.00010 0.00030 0.0000 0.0007 0.0000 LATT 1 SYMM -x+1/2, y+1/2, -z+1/2 SFAC C H N O UNIT 80 96 8 24 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP 20.000 ACTA L.S. 10 FMAP 2 PLAN -5 0 0.00 TEMP -173 SIZE 0.36 0.28 0.18 EQIV $1 x+1, y, z EQIV $2 -x+1/2, y-1/2, -z+3/2 EQIV $3 -x, -y+1, -z+1 EQIV $4 x-1, y, z HTAB O1A O2B HTAB O1B O2A HTAB O3 O2A HTAB O4 O2B_$1 HTAB C5A O1B_$2 HTAB C4B O3_$3 HTAB C4B O4_$4 HTAB C5B O2A_$3 HTAB C11 O1A_$1 BOND $H CONF WGHT 0.040100 1.336200 FVAR 0.31964 MOLE 1 C1A 1 0.000478 0.740933 0.797733 11.00000 0.01232 0.01514 = 0.01303 -0.00211 0.00116 0.00018 C2A 1 0.028807 0.755858 0.740088 11.00000 0.00992 0.01444 = 0.01251 -0.00151 0.00026 0.00107 C3A 1 0.138763 0.695384 0.728056 11.00000 0.01138 0.01174 = 0.01461 -0.00095 0.00199 -0.00186 C4A 1 0.217680 0.629754 0.779448 11.00000 0.01011 0.01596 = 0.01830 0.00148 0.00145 0.00125 AFIX 43 H4A 2 0.292429 0.589378 0.774412 11.00000 -1.20000 AFIX 0 C5A 1 0.187972 0.623504 0.836413 11.00000 0.01480 0.01516 = 0.01674 0.00270 -0.00216 0.00070 AFIX 43 H5A 2 0.242986 0.579842 0.870381 11.00000 -1.20000 AFIX 0 C6A 1 0.054664 0.659147 0.907739 11.00000 0.02683 0.02186 = 0.01057 0.00164 0.00494 0.00010 AFIX 137 H6A 2 0.000468 0.557440 0.908146 11.00000 -1.50000 H6B 2 0.018974 0.772256 0.918922 11.00000 -1.50000 H6C 2 0.126136 0.635299 0.937474 11.00000 -1.50000 AFIX 0 C7A 1 -0.118125 0.789664 0.808811 11.00000 0.01557 0.02704 = 0.01405 -0.00321 0.00498 0.00181 AFIX 137 H7A 2 -0.169401 0.814112 0.769332 11.00000 -1.50000 H7B 2 -0.113139 0.898787 0.834833 11.00000 -1.50000 H7C 2 -0.149443 0.687982 0.829518 11.00000 -1.50000 AFIX 0 N1A 3 0.082350 0.677860 0.845611 11.00000 0.01509 0.01498 = 0.01102 0.00054 0.00186 -0.00124 O1A 4 -0.051014 0.829444 0.694252 11.00000 0.01376 0.03106 = 0.01032 -0.00121 0.00056 0.00923 H1O 2 -0.039489 0.800546 0.657496 11.00000 0.04563 O2A 4 0.160235 0.701373 0.673085 11.00000 0.01284 0.02112 = 0.01264 -0.00015 0.00448 0.00129 MOLE 2 C1B 1 0.102961 0.783281 0.469439 11.00000 0.01181 0.01243 = 0.01575 0.00280 0.00370 -0.00031 C2B 1 0.056805 0.804469 0.521957 11.00000 0.01183 0.01025 = 0.01286 0.00003 0.00109 -0.00020 C3B 1 -0.056454 0.738479 0.526141 11.00000 0.01022 0.01203 = 0.01278 0.00110 0.00242 0.00208 C4B 1 -0.119689 0.657865 0.471992 11.00000 0.01126 0.01363 = 0.01401 -0.00023 0.00240 -0.00140 AFIX 43 H4B 2 -0.195888 0.612945 0.471623 11.00000 -1.20000 AFIX 0 C5B 1 -0.072020 0.644246 0.420388 11.00000 0.01448 0.01374 = 0.01319 -0.00046 0.00236 -0.00066 AFIX 43 H5B 2 -0.116342 0.590157 0.384528 11.00000 -1.20000 AFIX 0 C6B 1 0.081516 0.683453 0.361125 11.00000 0.02526 0.02519 = 0.01581 -0.00244 0.01227 -0.00267 AFIX 137 H6D 2 0.023032 0.623332 0.330086 11.00000 -1.50000 H6E 2 0.152148 0.608886 0.369076 11.00000 -1.50000 H6F 2 0.099681 0.803789 0.345985 11.00000 -1.50000 AFIX 0 C7B 1 0.225163 0.838091 0.466538 11.00000 0.01385 0.02436 = 0.02351 0.00225 0.00813 -0.00264 AFIX 137 H7D 2 0.224097 0.937097 0.436599 11.00000 -1.50000 H7E 2 0.266981 0.733083 0.453876 11.00000 -1.50000 H7F 2 0.264275 0.879915 0.507242 11.00000 -1.50000 AFIX 0 N1B 3 0.036053 0.704978 0.418453 11.00000 0.01559 0.01359 = 0.01295 -0.00040 0.00688 -0.00038 O1B 4 0.121169 0.891642 0.571038 11.00000 0.01533 0.01860 = 0.01281 -0.00031 -0.00051 -0.00536 H2O 2 0.118388 0.836625 0.606982 11.00000 0.04415 O2B 4 -0.096579 0.751936 0.576502 11.00000 0.01277 0.02261 = 0.00967 -0.00139 0.00352 -0.00003 MOLE 3 C8 1 0.430276 0.659612 0.624816 11.00000 0.00946 0.01346 = 0.01711 -0.00039 0.00329 -0.00016 C9 1 0.499762 0.642582 0.580247 11.00000 0.01251 0.01682 = 0.01263 -0.00225 0.00230 0.00027 AFIX 43 H9 2 0.468191 0.593785 0.540871 11.00000 -1.20000 AFIX 0 C10 1 0.615494 0.697176 0.593511 11.00000 0.01324 0.01589 = 0.01191 0.00082 0.00586 0.00086 C11 1 0.661514 0.775251 0.650220 11.00000 0.01045 0.01782 = 0.01564 -0.00013 0.00354 -0.00194 AFIX 43 H11 2 0.740060 0.814780 0.659066 11.00000 -1.20000 AFIX 0 C12 1 0.590067 0.794207 0.693695 11.00000 0.01396 0.01897 = 0.01203 -0.00307 0.00257 -0.00149 AFIX 43 H12 2 0.620756 0.847754 0.732450 11.00000 -1.20000 AFIX 0 C13 1 0.475112 0.736906 0.681907 11.00000 0.01332 0.01789 = 0.01350 -0.00191 0.00661 -0.00030 AFIX 43 H13 2 0.427811 0.750170 0.712255 11.00000 -1.20000 AFIX 0 O3 4 0.319939 0.594539 0.610186 11.00000 0.00889 0.02527 = 0.02209 -0.00832 0.00586 -0.00317 H3O 2 0.277584 0.630756 0.637118 11.00000 0.04905 O4 4 0.680621 0.668891 0.549199 11.00000 0.01100 0.03277 = 0.01564 -0.00483 0.00715 -0.00263 H4O 2 0.754220 0.701879 0.562648 11.00000 0.02970 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM KA951_0m_a.res in P2(1)/n REM wR2 = 0.1316, GooF = S = 1.021, Restrained GooF = 1.021 for all data REM R1 = 0.0540 for 4023 Fo > 4sig(Fo) and 0.0855 for all 5665 data REM 273 parameters refined using 0 restraints END WGHT 0.0401 1.3364 REM Highest difference peak 0.353, deepest hole -0.396, 1-sigma level 0.070 Q1 1 0.0827 0.7148 0.7342 11.00000 0.05 0.35 Q2 1 0.1617 0.8166 0.4705 11.00000 0.05 0.35 Q3 1 0.0007 0.7801 0.5249 11.00000 0.05 0.35 Q4 1 0.1798 0.6339 0.7501 11.00000 0.05 0.34 Q5 1 0.5609 0.6500 0.5902 11.00000 0.05 0.33 ; _shelx_res_checksum 14719 _shelx_hkl_file ; -2 0 0 1234.99 78.65 -3 0 0 0.51 0.37 3 0 0 0.36 0.35 -3 0 0 0.11 0.27 3 0 0 -0.41 0.29 -3 0 0 -0.42 0.30 -4 0 0 389.10 27.51 4 0 0 417.77 27.53 -4 0 0 440.16 27.48 -4 0 0 472.95 27.53 5 0 0 0.58 0.44 -5 0 0 0.79 0.57 5 0 0 0.52 0.37 -5 0 0 0.32 0.37 6 0 0 32.28 2.37 -6 0 0 32.60 2.31 -6 0 0 33.86 2.49 7 0 0 2.22 0.92 -7 0 0 1.21 0.74 -8 0 0 56.44 4.03 8 0 0 55.34 4.02 9 0 0 0.70 1.11 -9 0 0 2.20 1.04 -10 0 0 5.42 1.53 10 0 0 9.08 1.64 11 0 0 1.74 1.57 -12 0 0 2.97 1.29 12 0 0 2.25 1.78 14 0 0 3.92 2.23 15 0 0 0.36 2.34 16 0 0 8.55 2.59 0 -1 0 0.20 0.09 0 -1 0 0.03 0.11 0 1 0 -0.01 0.07 0 1 0 -0.05 0.10 -1 -1 0 7.69 0.67 1 -1 0 8.07 0.54 -1 -1 0 8.15 0.58 1 1 0 8.00 0.58 1 1 0 7.95 0.63 -2 -1 0 1015.23 67.15 2 -1 0 1076.84 67.17 2 1 0 1070.50 67.18 -3 -1 0 2.05 0.47 -3 -1 0 1.92 0.30 3 -1 0 1.57 0.38 3 -1 0 1.65 0.36 -3 -1 0 2.34 0.55 3 1 0 1.65 0.44 3 1 0 1.38 0.34 -3 1 0 1.87 0.39 4 -1 0 207.71 14.48 -4 -1 0 228.47 14.48 -4 -1 0 232.01 14.52 4 -1 0 239.48 14.45 -4 1 0 211.40 14.47 4 1 0 218.02 14.46 4 1 0 238.73 14.52 -4 1 0 223.65 14.37 -4 1 0 223.46 14.36 5 -1 0 24.02 1.91 5 -1 0 26.91 1.96 -5 -1 0 25.90 2.06 -5 1 0 25.56 1.78 5 1 0 25.94 1.88 -5 1 0 25.72 1.82 -6 -1 0 -0.03 0.64 6 -1 0 -0.41 0.40 6 -1 0 -0.15 0.45 -6 1 0 0.19 0.47 6 1 0 0.20 0.40 -6 1 0 0.01 0.39 -7 -1 0 10.85 1.56 -7 1 0 12.72 1.13 -7 1 0 11.32 1.20 7 1 0 12.42 1.38 8 -1 0 9.83 1.34 -8 -1 0 11.00 1.41 -8 1 0 9.87 0.97 -8 1 0 10.74 1.27 8 1 0 9.69 1.29 -9 -1 0 1.46 0.91 9 -1 0 0.02 1.07 9 1 0 0.92 1.08 -9 1 0 0.46 0.44 -9 1 0 0.72 0.80 10 -1 0 0.91 1.38 -10 -1 0 0.57 0.98 10 1 0 0.45 1.19 -10 1 0 0.17 0.67 11 -1 0 0.88 1.51 -11 -1 0 0.23 1.07 11 1 0 1.67 1.49 -12 -1 0 -0.12 0.95 12 -1 0 1.99 1.80 12 1 0 -1.40 1.64 13 -1 0 13.66 2.92 -13 -1 0 12.71 1.76 13 1 0 12.42 2.35 14 -1 0 35.18 4.22 14 1 0 39.67 4.02 15 -1 0 2.68 2.51 15 1 0 2.17 2.18 16 -1 0 0.82 2.92 16 1 0 0.20 1.94 0 -2 0 9451.93 621.56 0 2 0 9999.00 621.53 -1 -2 0 218.66 13.65 -1 -2 0 215.48 13.71 1 -2 0 209.17 13.64 1 -2 0 221.56 13.63 -1 -2 0 208.10 13.69 1 2 0 210.45 13.64 1 2 0 209.30 13.67 -2 -2 0 1239.69 78.52 -2 -2 0 1255.21 78.46 -2 -2 0 1214.99 78.51 2 2 0 1216.58 78.49 -3 -2 0 50.16 3.59 3 -2 0 52.75 3.40 -3 -2 0 50.64 3.49 3 -2 0 53.07 3.50 -3 -2 0 53.28 3.58 3 2 0 52.30 3.45 3 2 0 52.04 3.57 4 -2 0 143.73 8.96 -4 -2 0 137.11 9.10 4 -2 0 135.66 9.05 4 2 0 138.72 9.01 5 -2 0 72.79 5.03 5 -2 0 77.50 4.95 -5 -2 0 72.28 5.09 5 2 0 75.96 4.97 6 -2 0 39.89 2.97 -6 -2 0 39.78 3.23 6 -2 0 45.04 2.97 -7 -2 0 233.54 15.16 7 2 0 230.61 15.07 8 -2 0 2.93 0.93 -8 -2 0 0.81 0.80 8 2 0 3.36 0.96 -9 -2 0 10.93 1.70 9 -2 0 14.97 2.01 9 2 0 13.29 1.79 -10 -2 0 1.35 1.00 10 -2 0 1.59 1.45 10 2 0 4.24 1.37 -11 -2 0 24.35 2.70 11 -2 0 28.68 3.40 11 2 0 29.04 2.87 -12 -2 0 2.08 1.56 12 -2 0 4.08 2.21 12 2 0 4.39 1.72 13 -2 0 1.81 2.44 -13 -2 0 2.04 1.57 13 2 0 1.96 1.89 14 -2 0 7.05 2.62 -14 -2 0 -2.26 2.16 14 2 0 0.47 2.00 15 -2 0 18.30 3.28 15 2 0 19.12 3.07 16 -2 0 4.79 3.05 16 2 0 3.46 1.94 0 -3 0 0.17 0.14 0 -3 0 -0.02 0.35 0 -3 0 -0.24 0.38 0 3 0 -0.04 0.19 -1 -3 0 7.44 0.79 1 -3 0 5.74 0.67 1 -3 0 5.86 0.74 -1 -3 0 7.78 0.58 1 -3 0 6.25 0.52 -1 -3 0 8.35 0.77 1 3 0 6.94 0.65 1 3 0 7.71 0.60 2 -3 0 68.75 4.47 -2 -3 0 66.43 4.60 2 -3 0 67.79 4.43 2 3 0 69.42 4.47 -3 -3 0 40.91 2.95 3 3 0 41.84 2.80 -4 -3 0 12.28 1.43 4 -3 0 12.85 1.16 4 -3 0 12.56 1.12 4 3 0 13.47 1.05 5 -3 0 36.73 2.62 -5 -3 0 37.92 2.75 5 -3 0 36.55 2.70 -6 -3 0 5.04 0.96 6 -3 0 6.54 0.86 6 -3 0 5.63 0.84 6 3 0 7.13 0.95 -7 -3 0 1.81 0.81 7 -3 0 0.80 0.92 7 3 0 1.59 0.78 -8 -3 0 65.71 4.75 8 -3 0 62.89 4.71 8 3 0 65.89 4.61 9 -3 0 10.69 1.95 -9 -3 0 10.48 1.65 9 3 0 14.18 1.77 -10 -3 0 30.69 2.92 10 -3 0 31.34 3.44 10 3 0 32.90 2.89 -11 -3 0 -1.11 1.43 11 -3 0 2.09 1.81 11 3 0 0.85 1.44 12 -3 0 3.66 2.42 -12 -3 0 1.18 1.71 12 3 0 -0.79 1.54 -13 -3 0 24.31 3.76 13 3 0 30.04 3.27 -14 -3 0 15.58 2.80 14 -3 0 19.26 3.25 14 3 0 21.26 2.74 15 -3 0 0.48 2.73 15 3 0 1.02 2.05 0 -4 0 28.65 2.04 0 4 0 26.79 1.91 1 -4 0 13.52 1.20 1 -4 0 13.47 1.20 -1 -4 0 14.30 1.27 1 4 0 15.06 1.10 2 -4 0 258.48 15.86 -2 -4 0 236.70 15.94 2 4 0 243.41 15.82 3 -4 0 250.00 16.34 -3 -4 0 253.47 16.48 3 4 0 258.72 16.34 -4 -4 0 0.07 0.49 4 -4 0 -0.04 0.58 4 4 0 0.88 0.59 5 -4 0 25.33 1.99 5 -4 0 26.09 2.01 -5 -4 0 25.54 2.14 5 4 0 24.44 1.94 -6 -4 0 0.84 0.79 6 -4 0 0.60 0.57 6 4 0 1.55 0.72 7 -4 0 2.61 1.06 7 -4 0 1.16 0.74 -7 -4 0 1.75 0.87 7 4 0 3.02 0.92 -8 -4 0 30.35 2.77 8 -4 0 28.89 2.82 8 4 0 33.31 2.63 9 -4 0 11.61 1.90 -9 -4 0 12.82 1.94 9 4 0 10.85 1.59 -10 -4 0 3.40 1.50 10 -4 0 3.11 1.97 10 4 0 3.96 1.37 -11 -4 0 21.64 3.12 11 -4 0 27.86 3.61 -12 -4 0 3.41 2.17 12 -4 0 6.40 2.33 12 4 0 4.76 1.75 13 -4 0 1.37 2.80 -13 -4 0 -0.87 2.31 13 4 0 1.12 1.72 -14 -4 0 12.89 3.35 14 -4 0 19.33 3.34 14 4 0 14.28 2.45 -15 -4 0 35.56 4.23 15 -4 0 39.31 4.99 15 4 0 37.20 3.63 0 -5 0 7.24 6.19 0 5 0 3.49 5.26 1 -5 0 34.98 2.50 -1 -5 0 34.02 2.56 1 5 0 35.70 2.44 2 -5 0 35.27 2.50 -2 -5 0 35.72 2.66 -3 -5 0 21.83 1.91 3 5 0 23.35 1.77 -4 -5 0 19.31 1.91 4 -5 0 21.47 1.77 4 5 0 23.19 1.77 5 -5 0 1.44 1.02 -5 -5 0 1.20 0.82 5 -5 0 0.38 0.70 5 5 0 1.56 0.74 6 -5 0 14.90 1.80 -6 -5 0 14.10 1.81 6 5 0 16.16 1.76 -7 -5 0 37.18 3.26 7 -5 0 40.42 3.35 7 5 0 40.81 3.09 -8 -5 0 20.34 2.46 8 -5 0 25.31 2.86 8 5 0 24.11 2.29 9 -5 0 17.99 2.46 -9 -5 0 16.65 2.41 9 5 0 15.20 2.10 10 -5 0 0.69 2.01 -10 -5 0 0.07 1.70 10 5 0 0.62 1.56 11 -5 0 10.79 2.59 -11 -5 0 6.24 1.99 11 5 0 4.23 1.71 -12 -5 0 -2.53 1.93 12 -5 0 0.93 2.69 12 5 0 1.49 1.76 13 -5 0 28.15 3.74 -13 -5 0 20.69 3.34 13 5 0 22.23 3.13 14 -5 0 1.36 1.96 -14 -5 0 -1.14 2.44 14 5 0 1.00 1.76 0 -6 0 54.26 3.80 -1 -6 0 11.53 1.20 1 -6 0 8.60 1.02 1 6 0 8.61 1.13 -2 -6 0 -1.12 0.62 2 -6 0 0.31 0.56 2 6 0 1.31 0.76 -3 -6 0 60.17 4.45 3 -6 0 64.56 4.24 3 6 0 60.05 4.30 -4 -6 0 8.47 1.35 4 6 0 6.92 1.18 -5 -6 0 13.69 1.91 5 6 0 17.21 1.71 6 -6 0 60.65 4.70 -6 -6 0 61.00 4.73 6 6 0 64.65 4.45 -7 -6 0 3.60 1.49 7 -6 0 1.76 1.56 7 6 0 4.19 1.18 8 -6 0 26.21 3.26 8 6 0 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-7 -4 26 6.14 2.48 7 4 -26 10.32 2.25 6 -4 -26 5.17 2.09 -6 -4 26 1.64 2.06 6 4 -26 3.90 2.78 5 -4 -26 6.02 2.18 -5 -4 26 6.24 2.13 5 4 -26 5.39 2.73 4 -4 -26 9.10 2.98 -4 -4 26 11.33 1.98 4 4 -26 11.57 3.18 -3 -4 26 22.37 3.15 3 -4 -26 22.82 3.69 3 4 -26 24.32 3.96 2 -4 -26 10.04 2.87 -2 -4 26 7.14 1.92 2 4 -26 7.21 3.12 1 -4 -26 47.90 5.24 -1 -4 26 51.04 4.38 1 4 -26 51.82 5.57 0 -4 -26 0.13 2.65 0 4 -26 -0.81 3.00 -1 -4 -26 2.14 2.58 -1 4 -26 6.11 3.29 -2 -4 -26 30.47 4.42 2 -4 26 24.83 3.88 -2 4 -26 17.57 4.26 3 -4 26 43.44 5.89 -3 -4 -26 49.70 4.47 -3 4 -26 45.38 6.31 4 -4 26 37.75 4.68 -4 -4 -26 50.34 4.32 -4 4 -26 51.94 5.94 -7 -5 26 1.43 1.69 7 5 -26 4.46 2.03 -6 -5 26 27.81 3.07 6 5 -26 19.72 2.78 -5 -5 26 -0.56 1.81 5 5 -26 2.42 2.24 -4 -5 26 19.85 3.00 4 -5 -26 19.99 2.88 4 5 -26 20.67 3.04 3 -5 -26 0.46 2.49 -3 -5 26 2.25 1.68 3 5 -26 5.52 3.01 -2 -5 26 2.07 1.58 2 -5 -26 3.73 2.86 2 5 -26 5.11 3.18 -1 -5 26 -0.80 1.41 1 -5 -26 -1.28 2.47 1 5 -26 -2.68 3.20 0 -5 26 22.29 2.45 0 -5 -26 32.76 4.68 0 5 -26 24.91 3.99 1 -5 26 24.44 2.40 -1 -5 -26 27.28 4.26 -1 5 -26 23.77 3.95 -2 -5 -26 5.92 2.02 -2 5 -26 2.67 3.05 11 0 -27 11.05 2.91 10 0 -27 0.05 3.02 9 0 -27 0.53 2.91 8 0 -27 -2.93 2.48 7 0 -27 35.95 4.82 6 0 -27 0.80 2.57 5 0 -27 3.99 2.47 4 0 -27 -1.02 2.21 -4 0 27 1.70 1.13 -3 0 27 3.59 1.60 3 0 -27 2.57 2.55 2 0 -27 3.77 2.27 1 0 -27 3.60 2.37 -1 0 27 -0.98 1.50 0 0 -27 0.70 2.20 0 0 27 1.82 1.56 -1 0 -27 20.41 3.58 1 0 27 26.11 3.06 -2 0 -27 2.91 2.65 -3 0 -27 2.44 2.37 3 0 27 2.50 2.20 -4 0 -27 3.01 2.63 4 0 27 -0.17 2.31 -5 0 -27 45.72 4.37 5 0 27 43.17 4.56 11 1 -27 47.12 4.53 10 -1 -27 12.59 2.81 10 1 -27 9.70 2.77 9 -1 -27 15.68 3.62 9 1 -27 19.09 3.28 8 -1 -27 11.82 3.02 8 1 -27 0.44 2.61 7 -1 -27 1.96 2.44 7 1 -27 6.98 2.99 -6 -1 27 10.63 1.55 6 -1 -27 12.23 2.76 6 1 -27 6.15 2.78 -5 -1 27 8.37 1.79 5 -1 -27 6.67 2.81 5 1 -27 14.96 2.78 4 -1 -27 2.18 2.70 4 1 -27 9.73 2.66 3 -1 -27 1.79 2.53 -3 -1 27 0.92 1.60 3 1 -27 -3.93 2.53 -3 1 27 0.02 1.14 -2 -1 27 12.09 1.91 2 -1 -27 11.01 2.78 -2 1 27 13.88 1.89 2 1 -27 9.89 2.83 -1 -1 27 0.62 2.28 1 -1 -27 -1.57 2.21 1 1 -27 -2.79 2.31 0 -1 -27 -2.74 2.24 0 -1 27 -1.27 2.38 0 1 -27 -1.15 2.53 -1 -1 -27 -0.86 2.13 1 -1 27 1.82 2.33 -1 1 -27 2.83 2.56 2 -1 27 -0.05 2.48 -2 -1 -27 -2.25 2.35 -2 1 -27 -2.81 2.37 -3 -1 -27 2.04 2.35 3 -1 27 5.17 3.02 -3 1 -27 11.19 3.02 -4 -1 -27 -4.78 2.32 4 -1 27 2.32 2.75 -4 1 -27 3.24 2.84 -5 -1 -27 38.73 3.99 5 -1 27 33.69 4.46 -5 1 -27 26.29 4.14 10 2 -27 40.91 4.25 9 -2 -27 12.12 2.13 9 2 -27 5.50 2.77 8 -2 -27 5.62 2.56 8 2 -27 4.79 2.91 -7 -2 27 22.13 2.59 7 -2 -27 19.20 3.56 7 2 -27 28.18 4.15 -6 -2 27 2.60 1.92 6 -2 -27 -1.75 2.51 6 2 -27 5.21 2.51 5 -2 -27 2.22 2.65 -5 -2 27 3.81 1.89 5 2 -27 5.39 2.63 -4 -2 27 36.53 3.74 4 -2 -27 30.82 4.69 4 2 -27 33.20 4.40 -3 -2 27 2.18 1.77 3 -2 -27 -1.00 2.33 3 2 -27 2.43 2.61 -2 -2 27 12.23 2.20 2 -2 -27 15.40 3.01 2 2 -27 18.44 3.27 1 -2 -27 3.63 2.74 1 2 -27 3.67 2.86 0 -2 -27 -0.10 2.46 0 2 -27 1.92 2.62 1 -2 27 8.36 3.13 -1 2 -27 13.90 3.31 2 -2 27 9.33 3.10 -2 -2 -27 12.83 2.98 -2 2 -27 5.81 3.17 -3 -2 -27 0.43 2.26 3 -2 27 1.94 2.69 -3 2 -27 -0.18 2.86 -4 -2 -27 0.04 2.16 4 -2 27 0.96 3.24 -4 2 -27 -0.45 2.80 5 -2 27 9.67 3.06 -5 -2 -27 12.09 2.45 -5 2 -27 9.18 2.52 9 3 -27 32.96 3.71 8 -3 -27 4.09 2.81 -8 -3 27 1.86 1.69 8 3 -27 1.19 2.30 -7 -3 27 13.91 2.68 7 -3 -27 24.60 3.20 7 3 -27 19.29 3.38 -6 -3 27 16.30 2.64 6 -3 -27 13.20 3.14 6 3 -27 8.78 3.17 -5 -3 27 27.84 3.46 5 -3 -27 23.04 3.76 5 3 -27 21.10 3.60 -4 -3 27 28.74 3.48 4 -3 -27 22.29 3.91 4 3 -27 26.35 3.86 -3 -3 27 3.51 1.68 3 -3 -27 4.45 2.77 3 3 -27 3.96 2.67 -2 -3 27 45.78 4.12 2 -3 -27 44.36 5.34 2 3 -27 39.38 5.03 1 -3 -27 19.30 3.33 -1 -3 27 19.56 2.83 1 3 -27 12.11 3.18 0 -3 -27 3.31 2.72 0 3 -27 -3.64 2.67 1 -3 27 2.95 2.79 -1 -3 -27 2.47 2.68 -1 3 -27 7.74 3.03 -2 -3 -27 3.28 2.65 2 -3 27 2.69 3.10 -2 3 -27 12.15 3.30 3 -3 27 -2.77 2.79 -3 -3 -27 1.60 1.93 -3 3 -27 5.43 3.18 -4 -3 -27 2.59 1.95 4 -3 27 -0.40 2.61 -4 3 -27 7.45 2.80 -8 -4 27 5.21 2.06 8 4 -27 8.89 2.25 -7 -4 27 -0.91 2.18 -6 -4 27 5.38 2.28 6 -4 -27 2.18 2.27 6 4 -27 5.21 2.48 5 -4 -27 0.11 2.19 -5 -4 27 4.56 1.99 5 4 -27 0.78 2.28 -4 -4 27 10.86 2.26 4 -4 -27 15.53 3.24 4 4 -27 10.03 3.30 -3 -4 27 1.97 1.66 3 -4 -27 -3.02 2.84 3 4 -27 1.67 3.09 2 -4 -27 1.35 2.79 -2 -4 27 1.49 1.59 2 4 -27 3.20 3.08 -1 -4 27 8.75 1.88 1 -4 -27 10.10 2.88 1 4 -27 12.29 3.20 0 -4 27 3.50 1.62 0 -4 -27 3.90 2.74 0 4 -27 5.67 3.13 -1 -4 -27 -0.44 2.50 -1 4 -27 8.98 3.49 2 -4 27 2.84 3.00 -2 -4 -27 -2.72 2.21 -2 4 -27 -5.03 2.84 -3 -4 -27 5.33 2.09 -5 -5 27 1.43 1.35 5 5 -27 1.00 2.09 -4 -5 27 11.50 1.75 4 -5 -27 8.34 2.60 4 5 -27 13.40 2.25 3 -5 -27 2.57 2.41 -3 -5 27 4.49 1.40 2 -5 -27 11.01 3.14 2 5 -27 10.14 2.61 1 -5 -27 -1.83 2.84 -1 -5 27 1.92 1.28 1 5 -27 4.02 2.55 0 -5 -27 3.58 2.41 0 -5 27 -0.84 1.22 0 5 -27 -1.53 2.29 10 0 -28 4.43 2.95 9 0 -28 -3.88 2.97 8 0 -28 6.62 3.32 7 0 -28 -2.41 2.70 6 0 -28 0.92 2.43 5 0 -28 -2.46 2.63 -4 0 28 8.61 1.57 4 0 -28 6.47 2.74 3 0 -28 -2.36 2.33 -2 0 28 27.29 3.22 2 0 -28 32.47 4.17 1 0 -28 1.36 2.33 0 0 -28 14.70 3.03 -1 0 -28 -2.44 2.29 2 0 28 12.65 2.23 -2 0 -28 13.02 2.86 3 0 28 -3.32 1.90 -3 0 -28 -0.39 2.20 4 0 28 6.41 2.11 -4 0 -28 2.16 2.21 10 -1 -28 22.80 3.23 10 1 -28 33.72 4.01 9 -1 -28 1.41 3.05 9 1 -28 11.43 2.81 8 1 -28 24.08 3.81 7 -1 -28 1.57 2.93 7 1 -28 4.57 3.04 6 -1 -28 21.74 3.70 6 1 -28 20.67 3.71 5 -1 -28 -1.75 2.77 -5 -1 28 0.57 1.22 5 1 -28 9.06 2.84 4 -1 -28 -4.05 2.71 -4 -1 28 1.67 1.81 4 1 -28 7.88 2.86 -3 -1 28 11.57 2.30 3 -1 -28 18.44 3.40 3 1 -28 13.95 3.01 2 -1 -28 -0.06 2.40 -2 -1 28 -0.16 1.62 -2 1 28 0.26 1.00 2 1 -28 -1.12 2.46 -1 -1 28 3.44 1.91 1 -1 -28 5.44 2.46 1 1 -28 5.04 2.63 0 -1 -28 -1.21 2.70 0 -1 28 -1.03 2.02 0 1 -28 -2.70 2.38 1 -1 28 -0.92 2.45 -1 -1 -28 -1.49 2.26 -1 1 -28 2.50 2.54 2 -1 28 8.43 2.85 -2 -1 -28 6.53 2.69 -2 1 -28 4.49 2.68 3 -1 28 0.55 2.85 -3 -1 -28 -1.13 2.22 -3 1 -28 8.34 2.46 4 -1 28 8.46 2.75 -4 1 -28 6.17 2.37 9 -2 -28 7.68 2.25 9 2 -28 8.46 2.36 8 -2 -28 4.30 2.56 8 2 -28 5.22 2.37 7 -2 -28 3.36 3.18 7 2 -28 3.81 2.61 6 -2 -28 -0.95 2.98 -6 -2 28 0.82 1.65 6 2 -28 1.82 2.55 5 -2 -28 4.56 2.92 -5 -2 28 2.16 2.04 5 2 -28 3.15 2.63 -4 -2 28 7.11 2.10 4 -2 -28 0.13 2.61 4 2 -28 3.92 2.77 -3 -2 28 9.31 2.01 3 -2 -28 7.28 2.99 3 2 -28 9.82 2.82 -2 -2 28 1.73 1.83 2 -2 -28 6.01 2.58 2 2 -28 13.07 2.73 1 -2 -28 0.86 2.37 -1 -2 28 -0.45 1.56 1 2 -28 -1.72 2.47 0 -2 28 12.18 3.04 0 -2 -28 13.20 3.10 0 2 -28 13.60 3.43 -1 -2 -28 10.70 2.89 1 -2 28 14.37 3.24 -1 2 -28 20.30 3.75 -2 -2 -28 2.55 2.20 2 -2 28 4.73 3.27 -2 2 -28 -0.96 2.98 -3 -2 -28 28.98 3.73 3 -2 28 28.26 4.08 -3 2 -28 28.06 4.43 -4 -2 -28 7.95 2.30 4 -2 28 1.58 2.93 -4 2 -28 9.11 2.52 8 3 -28 1.16 2.26 7 -3 -28 -1.07 2.23 -7 -3 28 0.98 1.73 7 3 -28 3.84 2.26 -6 -3 28 4.88 2.07 6 -3 -28 2.39 2.76 6 3 -28 0.46 2.47 -5 -3 28 5.77 2.23 5 -3 -28 3.49 3.30 5 3 -28 2.82 2.59 4 -3 -28 12.23 3.29 -4 -3 28 6.90 1.97 4 3 -28 6.27 2.95 3 -3 -28 6.96 3.17 -3 -3 28 10.18 2.35 3 3 -28 6.50 3.13 -2 -3 28 4.21 1.78 2 -3 -28 -3.52 2.50 2 3 -28 -6.34 2.90 -1 -3 28 -0.85 1.49 1 -3 -28 -3.77 2.45 1 3 -28 -2.08 2.89 0 -3 -28 0.70 2.85 0 3 -28 0.48 2.65 -1 -3 -28 4.93 2.62 1 -3 28 3.25 2.94 -2 -3 -28 11.24 2.40 2 -3 28 7.18 3.23 -3 -3 -28 4.94 2.16 3 -3 28 5.81 2.99 -3 3 -28 12.58 2.60 -6 -4 28 10.97 2.15 6 -4 -28 5.66 2.97 6 4 -28 14.90 2.49 -5 -4 28 1.79 1.92 5 -4 -28 5.65 2.45 5 4 -28 3.92 2.16 4 -4 -28 10.32 3.06 -4 -4 28 5.80 1.93 4 4 -28 7.70 2.36 3 -4 -28 -2.47 2.82 -3 -4 28 -3.00 1.63 3 4 -28 3.29 2.40 -2 -4 28 5.66 1.69 2 -4 -28 -4.86 2.92 2 4 -28 -3.69 2.32 1 -4 -28 5.80 2.84 1 4 -28 10.01 2.69 0 -4 28 1.87 1.30 0 -4 -28 6.14 2.62 0 4 -28 4.99 2.26 -1 -4 -28 8.11 2.27 -1 4 -28 5.75 2.42 9 0 -29 11.57 2.98 8 0 -29 0.74 3.06 7 0 -29 13.33 3.07 6 0 -29 3.37 2.84 5 0 -29 7.19 3.07 4 0 -29 -2.75 2.81 -3 0 29 36.73 3.25 3 0 -29 34.35 4.66 2 0 -29 0.34 2.59 -2 0 29 -0.61 1.60 1 0 -29 45.17 4.96 0 0 -29 3.12 2.80 -1 0 -29 40.35 4.71 -2 0 -29 3.16 1.99 -3 0 -29 39.59 4.38 9 1 -29 147.18 10.50 8 -1 -29 15.09 3.42 8 1 -29 14.31 3.17 7 -1 -29 2.35 3.10 7 1 -29 9.77 2.97 6 -1 -29 0.62 3.11 6 1 -29 -0.62 2.84 -5 -1 29 78.61 6.71 5 -1 -29 89.02 7.79 5 1 -29 100.64 7.47 4 -1 -29 0.29 2.87 -4 -1 29 2.35 1.66 4 1 -29 6.27 2.55 -3 -1 29 56.20 5.05 3 -1 -29 63.92 6.11 3 1 -29 51.03 5.58 -2 -1 29 5.90 2.13 2 -1 -29 9.70 3.03 2 1 -29 11.41 3.16 1 -1 -29 131.51 10.31 1 1 -29 137.02 10.22 0 -1 -29 -0.81 2.41 0 1 -29 2.01 2.51 -1 -1 -29 1.65 2.49 1 -1 29 1.77 1.77 -1 1 -29 -1.19 2.30 2 -1 29 7.70 2.12 -2 -1 -29 -1.41 2.18 -2 1 -29 3.11 2.08 3 -1 29 8.91 2.25 -3 -1 -29 20.88 3.12 -3 1 -29 13.29 2.62 8 -2 -29 27.79 4.12 7 -2 -29 8.85 3.35 7 2 -29 10.62 2.32 6 -2 -29 -2.75 3.11 -6 -2 29 3.64 1.51 6 2 -29 -0.26 2.28 -5 -2 29 1.39 1.89 5 -2 -29 0.79 3.14 5 2 -29 6.47 2.78 -4 -2 29 3.88 2.23 4 -2 -29 4.45 3.21 4 2 -29 2.60 2.62 -3 -2 29 12.69 2.54 3 -2 -29 15.84 3.56 3 2 -29 9.17 3.16 -2 -2 29 4.23 1.99 2 -2 -29 1.15 2.82 2 2 -29 10.88 2.86 -1 -2 29 13.87 2.23 1 -2 -29 11.75 3.21 1 2 -29 10.23 2.85 0 -2 29 3.12 3.02 0 -2 -29 -0.53 2.47 0 2 -29 2.69 2.62 -1 -2 -29 32.17 4.10 -1 2 -29 36.64 4.05 2 -2 29 -0.83 2.61 -2 -2 -29 -4.55 2.20 -2 2 -29 3.90 2.25 7 -3 -29 2.77 2.53 -7 -3 29 6.76 1.76 6 -3 -29 -0.50 2.68 -6 -3 29 -3.52 1.73 6 3 -29 -4.07 2.31 -5 -3 29 8.42 2.40 5 -3 -29 8.61 3.29 5 3 -29 9.32 2.29 4 -3 -29 2.66 3.27 -4 -3 29 4.96 2.05 4 3 -29 2.54 2.15 3 -3 -29 20.99 3.38 -3 -3 29 17.19 2.57 3 3 -29 18.80 3.04 -2 -3 29 6.70 1.89 2 -3 -29 7.23 3.15 2 3 -29 3.68 2.21 1 -3 -29 2.48 2.65 -1 -3 29 3.55 1.46 1 3 -29 -1.81 2.19 0 -3 -29 -1.60 2.38 0 3 -29 -1.39 2.34 -1 -3 -29 5.04 2.13 1 -3 29 7.94 3.32 -1 3 -29 11.09 2.54 -4 -4 29 3.13 1.49 4 -4 -29 6.83 2.81 4 4 -29 4.66 2.40 3 -4 -29 7.61 2.96 -3 -4 29 -0.62 1.41 3 4 -29 2.42 2.38 2 -4 -29 6.39 2.84 -2 -4 29 8.20 1.59 2 4 -29 8.09 2.51 8 0 -30 64.15 5.55 7 0 -30 4.06 2.72 6 0 -30 37.09 4.41 5 0 -30 5.33 2.71 4 0 -30 3.81 3.02 3 0 -30 1.28 2.57 2 0 -30 4.18 2.56 -2 0 30 4.63 1.46 1 0 -30 6.96 2.35 0 0 -30 -1.53 2.29 -1 0 -30 -2.56 2.27 -2 0 -30 0.86 2.65 7 -1 -30 15.97 3.37 7 1 -30 25.68 3.75 6 -1 -30 50.19 5.79 6 1 -30 47.08 4.79 5 -1 -30 3.85 3.13 5 1 -30 6.81 2.63 4 -1 -30 7.14 3.14 -4 -1 30 8.54 1.67 3 -1 -30 0.12 2.95 -3 -1 30 1.33 1.89 3 1 -30 2.80 2.67 -2 -1 30 18.65 2.78 2 -1 -30 25.26 3.79 2 1 -30 19.56 3.24 1 -1 -30 -3.74 2.42 -1 -1 30 0.62 1.98 1 1 -30 1.00 2.42 0 -1 -30 3.75 2.26 0 1 -30 6.60 2.20 -1 -1 -30 1.74 2.13 -1 1 -30 1.26 2.21 6 -2 -30 13.68 3.51 6 2 -30 8.64 2.58 5 -2 -30 1.51 3.12 -5 -2 30 1.59 1.59 5 2 -30 4.16 2.33 -4 -2 30 5.12 1.90 4 -2 -30 3.94 3.22 -3 -2 30 1.77 2.19 3 -2 -30 4.68 2.81 3 2 -30 -2.75 2.09 2 -2 -30 3.44 2.71 -2 -2 30 6.00 2.09 -1 -2 30 4.22 1.66 1 -2 -30 3.54 2.23 -1 -2 30 2.17 2.13 1 2 -30 11.13 2.44 0 -2 -30 1.82 2.35 0 -2 30 -1.95 2.06 0 2 -30 -1.73 2.19 -1 -2 -30 -1.82 2.38 -1 2 -30 3.07 2.42 4 -3 -30 1.29 2.96 -4 -3 30 4.13 1.76 4 3 -30 5.33 2.53 -3 -3 30 2.89 1.46 3 -3 -30 3.18 2.81 3 3 -30 5.62 2.43 2 -3 -30 3.00 2.55 -2 -3 30 1.62 1.48 2 3 -30 6.41 2.60 5 0 -31 6.07 2.27 4 0 -31 -0.08 2.44 3 0 -31 18.62 2.65 2 0 -31 -2.05 2.19 -1 0 31 3.71 1.50 1 0 -31 0.71 2.27 5 -1 -31 41.21 4.49 5 1 -31 43.23 4.22 4 -1 -31 6.80 2.67 4 1 -31 9.91 2.54 -3 -1 31 -1.71 1.51 3 -1 -31 -0.59 2.22 3 1 -31 -0.91 2.45 -2 -1 31 4.50 1.77 2 -1 -31 10.82 2.30 2 1 -31 1.06 2.56 1 -1 -31 9.02 2.36 -1 -1 31 9.06 2.01 1 1 -31 8.48 2.76 0 0 0 0.00 0.00 _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.5702 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71039 11.712 7.318 22.074 89.982 100.719 90.012 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 78491 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 C1A C 0.00048(13) 0.7409(2) 0.79773(7) 0.0136(3) Uani 1 1 d . . . . . C2A C 0.02881(12) 0.7559(2) 0.74009(7) 0.0125(3) Uani 1 1 d . . . . . C3A C 0.13876(13) 0.6954(2) 0.72806(7) 0.0126(3) Uani 1 1 d . . . . . C4A C 0.21768(13) 0.6298(2) 0.77945(7) 0.0149(3) Uani 1 1 d . . . . . H4A H 0.292429 0.589378 0.774412 0.018 Uiso 1 1 calc R U . . . C5A C 0.18797(13) 0.6235(2) 0.83641(7) 0.0162(3) Uani 1 1 d . . . . . H5A H 0.242986 0.579842 0.870381 0.019 Uiso 1 1 calc R U . . . C6A C 0.05466(15) 0.6591(2) 0.90774(7) 0.0196(3) Uani 1 1 d . . . . . H6A H 0.000468 0.557440 0.908146 0.029 Uiso 1 1 calc R U . . . H6B H 0.018974 0.772256 0.918922 0.029 Uiso 1 1 calc R U . . . H6C H 0.126136 0.635299 0.937474 0.029 Uiso 1 1 calc R U . . . C7A C -0.11812(14) 0.7897(2) 0.80881(7) 0.0186(3) Uani 1 1 d . . . . . H7A H -0.169401 0.814112 0.769332 0.028 Uiso 1 1 calc R U . . . H7B H -0.113139 0.898787 0.834833 0.028 Uiso 1 1 calc R U . . . H7C H -0.149443 0.687982 0.829518 0.028 Uiso 1 1 calc R U . . . N1A N 0.08235(11) 0.67786(18) 0.84561(6) 0.0138(3) Uani 1 1 d . . . . . O1A O -0.05101(10) 0.82944(17) 0.69425(5) 0.0186(3) Uani 1 1 d . . . . . H1O H -0.039(2) 0.801(3) 0.6575(12) 0.046(7) Uiso 1 1 d . . . . . O2A O 0.16024(9) 0.70137(16) 0.67308(5) 0.0153(2) Uani 1 1 d . . . . . C1B C 0.10296(13) 0.7833(2) 0.46944(7) 0.0132(3) Uani 1 1 d . . . . . C2B C 0.05680(13) 0.8045(2) 0.52196(7) 0.0118(3) Uani 1 1 d . . . . . C3B C -0.05645(12) 0.7385(2) 0.52614(7) 0.0116(3) Uani 1 1 d . . . . . C4B C -0.11969(13) 0.6579(2) 0.47199(7) 0.0130(3) Uani 1 1 d . . . . . H4B H -0.195888 0.612945 0.471623 0.016 Uiso 1 1 calc R U . . . C5B C -0.07202(13) 0.6442(2) 0.42039(7) 0.0138(3) Uani 1 1 d . . . . . H5B H -0.116342 0.590157 0.384528 0.017 Uiso 1 1 calc R U . . . C6B C 0.08152(16) 0.6835(2) 0.36112(8) 0.0210(4) Uani 1 1 d . . . . . H6D H 0.023032 0.623332 0.330086 0.032 Uiso 1 1 calc R U . . . H6E H 0.152148 0.608886 0.369076 0.032 Uiso 1 1 calc R U . . . H6F H 0.099681 0.803789 0.345985 0.032 Uiso 1 1 calc R U . . . C7B C 0.22516(14) 0.8381(2) 0.46654(8) 0.0200(3) Uani 1 1 d . . . . . H7D H 0.224097 0.937097 0.436599 0.030 Uiso 1 1 calc R U . . . H7E H 0.266981 0.733083 0.453876 0.030 Uiso 1 1 calc R U . . . H7F H 0.264275 0.879915 0.507242 0.030 Uiso 1 1 calc R U . . . N1B N 0.03605(11) 0.70498(18) 0.41845(6) 0.0135(3) Uani 1 1 d . . . . . O1B O 0.12117(9) 0.89164(16) 0.57104(5) 0.0160(2) Uani 1 1 d . . . . . H2O H 0.118(2) 0.837(3) 0.6070(12) 0.044(7) Uiso 1 1 d . . . . . O2B O -0.09658(9) 0.75194(16) 0.57650(5) 0.0148(2) Uani 1 1 d . . . . . C8 C 0.43028(13) 0.6596(2) 0.62482(7) 0.0132(3) Uani 1 1 d . . . . . C9 C 0.49976(13) 0.6426(2) 0.58025(7) 0.0140(3) Uani 1 1 d . . . . . H9 H 0.468191 0.593785 0.540871 0.017 Uiso 1 1 calc R U . . . C10 C 0.61549(13) 0.6972(2) 0.59351(7) 0.0132(3) Uani 1 1 d . . . . . C11 C 0.66151(13) 0.7753(2) 0.65022(7) 0.0145(3) Uani 1 1 d . . . . . H11 H 0.740060 0.814780 0.659066 0.017 Uiso 1 1 calc R U . . . C12 C 0.59007(13) 0.7942(2) 0.69370(7) 0.0150(3) Uani 1 1 d . . . . . H12 H 0.620756 0.847754 0.732450 0.018 Uiso 1 1 calc R U . . . C13 C 0.47511(13) 0.7369(2) 0.68191(7) 0.0144(3) Uani 1 1 d . . . . . H13 H 0.427811 0.750170 0.712255 0.017 Uiso 1 1 calc R U . . . O3 O 0.31994(9) 0.59454(17) 0.61019(5) 0.0184(3) Uani 1 1 d . . . . . H3O H 0.278(2) 0.631(4) 0.6371(12) 0.049(7) Uiso 1 1 d . . . . . O4 O 0.68062(10) 0.66889(17) 0.54920(5) 0.0192(3) Uani 1 1 d . . . . . H4O H 0.754(2) 0.702(3) 0.5626(10) 0.030(6) Uiso 1 1 d . . . . . 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 C1A 0.0123(7) 0.0151(7) 0.0130(7) -0.0021(6) 0.0012(5) 0.0002(6) C2A 0.0099(7) 0.0144(7) 0.0125(7) -0.0015(5) 0.0003(5) 0.0011(5) C3A 0.0114(7) 0.0117(7) 0.0146(7) -0.0009(5) 0.0020(5) -0.0019(5) C4A 0.0101(7) 0.0160(7) 0.0183(8) 0.0015(6) 0.0014(5) 0.0013(6) C5A 0.0148(7) 0.0152(7) 0.0167(7) 0.0027(6) -0.0022(6) 0.0007(6) C6A 0.0268(9) 0.0219(8) 0.0106(7) 0.0016(6) 0.0049(6) 0.0001(7) C7A 0.0156(7) 0.0270(9) 0.0140(7) -0.0032(6) 0.0050(6) 0.0018(7) N1A 0.0151(6) 0.0150(6) 0.0110(6) 0.0005(5) 0.0019(5) -0.0012(5) O1A 0.0138(5) 0.0311(7) 0.0103(5) -0.0012(5) 0.0006(4) 0.0092(5) O2A 0.0128(5) 0.0211(6) 0.0126(5) -0.0001(4) 0.0045(4) 0.0013(4) C1B 0.0118(7) 0.0124(7) 0.0158(7) 0.0028(6) 0.0037(5) -0.0003(5) C2B 0.0118(7) 0.0103(7) 0.0129(7) 0.0000(5) 0.0011(5) -0.0002(5) C3B 0.0102(6) 0.0120(7) 0.0128(7) 0.0011(5) 0.0024(5) 0.0021(5) C4B 0.0113(7) 0.0136(7) 0.0140(7) -0.0002(6) 0.0024(5) -0.0014(5) C5B 0.0145(7) 0.0137(7) 0.0132(7) -0.0005(6) 0.0024(5) -0.0007(6) C6B 0.0253(9) 0.0252(9) 0.0158(8) -0.0024(6) 0.0123(6) -0.0027(7) C7B 0.0138(7) 0.0244(9) 0.0235(8) 0.0023(7) 0.0081(6) -0.0026(6) N1B 0.0156(6) 0.0136(6) 0.0130(6) -0.0004(5) 0.0069(5) -0.0004(5) O1B 0.0153(5) 0.0186(6) 0.0128(5) -0.0003(4) -0.0005(4) -0.0054(4) O2B 0.0128(5) 0.0226(6) 0.0097(5) -0.0014(4) 0.0035(4) 0.0000(4) C8 0.0095(7) 0.0135(7) 0.0171(7) -0.0004(6) 0.0033(5) -0.0002(5) C9 0.0125(7) 0.0168(7) 0.0126(7) -0.0023(6) 0.0023(5) 0.0003(6) C10 0.0132(7) 0.0159(7) 0.0119(7) 0.0008(6) 0.0059(5) 0.0009(6) C11 0.0104(7) 0.0178(8) 0.0156(7) -0.0001(6) 0.0035(5) -0.0019(6) C12 0.0140(7) 0.0190(8) 0.0120(7) -0.0031(6) 0.0026(5) -0.0015(6) C13 0.0133(7) 0.0179(8) 0.0135(7) -0.0019(6) 0.0066(5) -0.0003(6) O3 0.0089(5) 0.0253(6) 0.0221(6) -0.0083(5) 0.0059(4) -0.0032(5) O4 0.0110(5) 0.0328(7) 0.0156(5) -0.0048(5) 0.0072(4) -0.0026(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N1A C1A C2A 119.10(13) . . ? N1A C1A C7A 119.53(13) . . ? C2A C1A C7A 121.37(14) . . ? O1A C2A C1A 118.08(13) . . ? O1A C2A C3A 120.27(13) . . ? C1A C2A C3A 121.64(14) . . ? O2A C3A C4A 123.97(14) . . ? O2A C3A C2A 120.25(13) . . ? C4A C3A C2A 115.77(13) . . ? C5A C4A C3A 120.82(14) . . ? C5A C4A H4A 119.6 . . ? C3A C4A H4A 119.6 . . ? N1A C5A C4A 121.63(14) . . ? N1A C5A H5A 119.2 . . ? C4A C5A H5A 119.2 . . ? N1A C6A H6A 109.5 . . ? N1A C6A H6B 109.5 . . ? H6A C6A H6B 109.5 . . ? N1A C6A H6C 109.5 . . ? H6A C6A H6C 109.5 . . ? H6B C6A H6C 109.5 . . ? C1A C7A H7A 109.5 . . ? C1A C7A H7B 109.5 . . ? H7A C7A H7B 109.5 . . ? C1A C7A H7C 109.5 . . ? H7A C7A H7C 109.5 . . ? H7B C7A H7C 109.5 . . ? C5A N1A C1A 120.92(13) . . ? C5A N1A C6A 118.53(13) . . ? C1A N1A C6A 120.48(13) . . ? C2A O1A H1O 113.2(16) . . ? N1B C1B C2B 119.00(13) . . ? N1B C1B C7B 118.82(13) . . ? C2B C1B C7B 122.16(14) . . ? O1B C2B C1B 118.59(13) . . ? O1B C2B C3B 119.45(13) . . ? C1B C2B C3B 121.96(14) . . ? O2B C3B C4B 122.97(13) . . ? O2B C3B C2B 121.32(13) . . ? C4B C3B C2B 115.71(13) . . ? C5B C4B C3B 120.43(14) . . ? C5B C4B H4B 119.8 . . ? C3B C4B H4B 119.8 . . ? N1B C5B C4B 122.25(14) . . ? N1B C5B H5B 118.9 . . ? C4B C5B H5B 118.9 . . ? N1B C6B H6D 109.5 . . ? N1B C6B H6E 109.5 . . ? H6D C6B H6E 109.5 . . ? N1B C6B H6F 109.5 . . ? H6D C6B H6F 109.5 . . ? H6E C6B H6F 109.5 . . ? C1B C7B H7D 109.5 . . ? C1B C7B H7E 109.5 . . ? H7D C7B H7E 109.5 . . ? C1B C7B H7F 109.5 . . ? H7D C7B H7F 109.5 . . ? H7E C7B H7F 109.5 . . ? C5B N1B C1B 120.57(13) . . ? C5B N1B C6B 118.85(13) . . ? C1B N1B C6B 120.57(13) . . ? C2B O1B H2O 112.9(16) . . ? O3 C8 C9 117.01(14) . . ? O3 C8 C13 122.74(13) . . ? C9 C8 C13 120.24(14) . . ? C10 C9 C8 119.90(14) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? O4 C10 C9 117.22(13) . . ? O4 C10 C11 122.23(14) . . ? C9 C10 C11 120.55(13) . . ? C12 C11 C10 118.63(14) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C13 C12 C11 121.73(14) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C12 C13 C8 118.91(13) . . ? C12 C13 H13 120.5 . . ? C8 C13 H13 120.5 . . ? C8 O3 H3O 111.2(17) . . ? C10 O4 H4O 110.7(13) . . ? 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 C1A N1A 1.3705(19) . ? C1A C2A 1.378(2) . ? C1A C7A 1.498(2) . ? C2A O1A 1.3570(18) . ? C2A C3A 1.433(2) . ? C3A O2A 1.2852(18) . ? C3A C4A 1.410(2) . ? C4A C5A 1.367(2) . ? C4A H4A 0.9500 . ? C5A N1A 1.350(2) . ? C5A H5A 0.9500 . ? C6A N1A 1.4734(19) . ? C6A H6A 0.9800 . ? C6A H6B 0.9800 . ? C6A H6C 0.9800 . ? C7A H7A 0.9800 . ? C7A H7B 0.9800 . ? C7A H7C 0.9800 . ? O1A H1O 0.87(3) . ? C1B N1B 1.374(2) . ? C1B C2B 1.376(2) . ? C1B C7B 1.499(2) . ? C2B O1B 1.3603(18) . ? C2B C3B 1.431(2) . ? C3B O2B 1.2886(17) . ? C3B C4B 1.415(2) . ? C4B C5B 1.362(2) . ? C4B H4B 0.9500 . ? C5B N1B 1.3500(19) . ? C5B H5B 0.9500 . ? C6B N1B 1.4697(19) . ? C6B H6D 0.9800 . ? C6B H6E 0.9800 . ? C6B H6F 0.9800 . ? C7B H7D 0.9800 . ? C7B H7E 0.9800 . ? C7B H7F 0.9800 . ? O1B H2O 0.90(2) . ? C8 O3 1.3596(18) . ? C8 C9 1.394(2) . ? C8 C13 1.394(2) . ? C9 C10 1.392(2) . ? C9 H9 0.9500 . ? C10 O4 1.3630(17) . ? C10 C11 1.392(2) . ? C11 C12 1.392(2) . ? C11 H11 0.9500 . ? C12 C13 1.389(2) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? O3 H3O 0.88(3) . ? O4 H4O 0.89(2) . ? 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 O1A H1O O2B 0.87(3) 1.83(3) 2.6191(15) 150(2) . yes O1B H2O O2A 0.90(2) 1.76(3) 2.6177(16) 160(2) . yes O3 H3O O2A 0.88(3) 1.79(3) 2.6457(15) 164(2) . yes O4 H4O O2B 0.89(2) 1.76(2) 2.6394(16) 170(2) 1_655 yes C5A H5A O1B 0.95 2.31 3.2218(19) 159.9 2_546 yes C4B H4B O3 0.95 2.59 3.2632(19) 127.9 3_566 yes C4B H4B O4 0.95 2.47 3.1393(18) 127.3 1_455 yes C5B H5B O2A 0.95 2.49 3.3098(19) 144.4 3_566 yes C11 H11 O1A 0.95 2.43 3.3524(19) 163.7 1_655 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 N1A C1A C2A O1A -175.89(14) . . . . ? C7A C1A C2A O1A 5.0(2) . . . . ? N1A C1A C2A C3A 4.4(2) . . . . ? C7A C1A C2A C3A -174.76(15) . . . . ? O1A C2A C3A O2A -3.7(2) . . . . ? C1A C2A C3A O2A 176.01(14) . . . . ? O1A C2A C3A C4A 176.86(14) . . . . ? C1A C2A C3A C4A -3.4(2) . . . . ? O2A C3A C4A C5A -178.50(15) . . . . ? C2A C3A C4A C5A 0.9(2) . . . . ? C3A C4A C5A N1A 0.6(2) . . . . ? C4A C5A N1A C1A 0.3(2) . . . . ? C4A C5A N1A C6A 177.19(15) . . . . ? C2A C1A N1A C5A -2.8(2) . . . . ? C7A C1A N1A C5A 176.39(15) . . . . ? C2A C1A N1A C6A -179.61(14) . . . . ? C7A C1A N1A C6A -0.5(2) . . . . ? N1B C1B C2B O1B -176.25(13) . . . . ? C7B C1B C2B O1B 5.5(2) . . . . ? N1B C1B C2B C3B 3.5(2) . . . . ? C7B C1B C2B C3B -174.80(14) . . . . ? O1B C2B C3B O2B -3.5(2) . . . . ? C1B C2B C3B O2B 176.85(14) . . . . ? O1B C2B C3B C4B 176.90(13) . . . . ? C1B C2B C3B C4B -2.8(2) . . . . ? O2B C3B C4B C5B -178.76(14) . . . . ? C2B C3B C4B C5B 0.9(2) . . . . ? C3B C4B C5B N1B 0.3(2) . . . . ? C4B C5B N1B C1B 0.3(2) . . . . ? C4B C5B N1B C6B 179.39(15) . . . . ? C2B C1B N1B C5B -2.1(2) . . . . ? C7B C1B N1B C5B 176.18(14) . . . . ? C2B C1B N1B C6B 178.76(14) . . . . ? C7B C1B N1B C6B -2.9(2) . . . . ? O3 C8 C9 C10 -176.45(14) . . . . ? C13 C8 C9 C10 2.2(2) . . . . ? C8 C9 C10 O4 176.84(14) . . . . ? C8 C9 C10 C11 -2.4(2) . . . . ? O4 C10 C11 C12 -178.02(15) . . . . ? C9 C10 C11 C12 1.2(2) . . . . ? C10 C11 C12 C13 0.2(2) . . . . ? C11 C12 C13 C8 -0.4(2) . . . . ? O3 C8 C13 C12 177.80(15) . . . . ? C9 C8 C13 C12 -0.8(2) . . . . ? _cod_database_fobs_code 2022894