#------------------------------------------------------------------------------ #$Date: 2023-10-10 04:19:25 +0200 (Tue, 10 Oct 2023) $ #$Revision: 286864 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022897.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_2022897 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 O3, 2(H2 O)' _chemical_formula_sum 'C20 H28 N2 O9' _chemical_formula_weight 440.44 _chemical_name_common 'Deferiprone Phloroglucinol hydrate (2:1:2)' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 91.088(8) _cell_angle_beta 93.874(7) _cell_angle_gamma 90.209(7) _cell_formula_units_Z 2 _cell_length_a 7.9892(19) _cell_length_b 10.197(3) _cell_length_c 12.876(4) _cell_measurement_reflns_used 9849 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.54 _cell_measurement_theta_min 2.53 _cell_volume 1046.4(5) _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 0.995 _diffrn_measured_fraction_theta_max 0.995 _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 0.0567 _diffrn_reflns_av_unetI/netI 0.0477 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 20542 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.997 _diffrn_reflns_theta_min 2.527 _diffrn_source microfocus _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.5383 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker, 2016' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.398 _exptl_crystal_description block _exptl_crystal_F_000 468 _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_min 0.170 _refine_diff_density_max 0.475 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.100 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.246 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 300 _refine_ls_number_reflns 4542 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.246 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0841 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+4.4439P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2036 _refine_ls_wR_factor_ref 0.2045 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4349 _reflns_number_total 4542 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lo5093sup1.cif _cod_data_source_block KA1017_0m_def-phghyd_2_1_2 _cod_database_code 2022897 _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 0.965 _shelx_estimated_absorpt_t_max 0.981 _shelx_res_file ; TITL KA1017_0m_a.res in P-1 KA1017_0m.res created by SHELXL-2018/3 at 11:14:01 on 16-Mar-2021 CELL 0.71073 7.9892 10.1972 12.8765 91.088 93.874 90.209 ZERR 2.00 0.0019 0.0027 0.0037 0.008 0.007 0.007 LATT 1 SFAC C H N O UNIT 40 56 4 18 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! L.S. 25 ACTA BOND $H OMIT -3 54 OMIT 2 5 8 OMIT -2 1 1 OMIT 2 4 9 FMAP 2 PLAN 5 EQIV $1 -x+1, -y+1, -z+2 EQIV $2 -x+1, -y+1, -z+1 EQIV $3 x-1, y, z EQIV $4 x+1, y, z EQIV $5 -x+1, -y+2, -z+1 HTAB O1A O2A HTAB O1A O2A_$1 HTAB O1B O2B_$2 HTAB O3 O1W HTAB O4 O1W_$3 HTAB O5 O2W HTAB O1W O2B HTAB O1W O4_$4 HTAB O1W O1W_$5 HTAB O2W O2A HTAB O2W O4_$4 CONF SIZE 0.32 0.26 0.17 TEMP -173 WGHT 0.000000 4.443900 FVAR 0.78231 MOLE 1 C1A 1 0.765349 0.544637 1.275586 11.00000 0.00988 0.00586 = 0.01517 -0.00021 0.00009 -0.00206 C2A 1 0.679182 0.541469 1.179303 11.00000 0.00711 0.00979 = 0.01479 -0.00139 0.00040 -0.00142 C3A 1 0.670514 0.653880 1.113614 11.00000 0.01022 0.00991 = 0.01548 0.00047 0.00192 0.00072 C4A 1 0.761097 0.765434 1.153269 11.00000 0.01508 0.00955 = 0.02303 0.00465 -0.00106 -0.00176 AFIX 43 H4A 2 0.762921 0.842147 1.112628 11.00000 -1.20000 AFIX 0 C5A 1 0.846003 0.764831 1.248959 11.00000 0.01207 0.01071 = 0.02424 0.00096 -0.00101 -0.00277 AFIX 43 H5A 2 0.905462 0.841341 1.273594 11.00000 -1.20000 AFIX 0 C6A 1 0.933700 0.665387 1.415012 11.00000 0.01403 0.01904 = 0.01806 -0.00294 -0.00802 -0.00199 AFIX 137 H6A 2 1.013010 0.592687 1.423615 11.00000 -1.50000 H6B 2 0.850697 0.659934 1.467449 11.00000 -1.50000 H6C 2 0.994574 0.748908 1.423700 11.00000 -1.50000 AFIX 0 C7A 1 0.770998 0.427748 1.345095 11.00000 0.02162 0.01217 = 0.01466 0.00222 -0.00265 0.00017 AFIX 137 H7A 2 0.697749 0.358410 1.313651 11.00000 -1.50000 H7B 2 0.732598 0.453297 1.413248 11.00000 -1.50000 H7C 2 0.886330 0.395327 1.353705 11.00000 -1.50000 AFIX 0 N1A 3 0.847355 0.657282 1.309720 11.00000 0.01073 0.01136 = 0.01592 -0.00157 -0.00300 -0.00079 O1A 4 0.599170 0.428607 1.146389 11.00000 0.01839 0.00796 = 0.01447 0.00031 -0.00464 -0.00412 O2A 4 0.584347 0.649147 1.025700 11.00000 0.01691 0.01234 = 0.01480 0.00252 -0.00403 -0.00029 H1OA 2 0.551449 0.439491 1.084295 11.00000 0.04434 MOLE 2 C1B 1 0.238084 0.529431 0.228611 11.00000 0.01919 0.00975 = 0.01812 0.00439 0.00873 0.00605 C2B 1 0.322757 0.534995 0.324002 11.00000 0.02313 0.01322 = 0.01489 0.00587 0.00746 0.00843 C3B 1 0.402591 0.653068 0.365976 11.00000 0.02039 0.01230 = 0.01409 0.00195 0.00523 0.00778 C4B 1 0.382058 0.764450 0.301614 11.00000 0.02228 0.01016 = 0.01728 0.00357 0.00358 0.00299 AFIX 43 H4B 2 0.428248 0.846557 0.325218 11.00000 -1.20000 AFIX 0 C5B 1 0.296900 0.754689 0.206506 11.00000 0.02339 0.00859 = 0.01924 0.00514 0.00516 0.00466 AFIX 43 H5B 2 0.286583 0.830421 0.164751 11.00000 -1.20000 AFIX 0 C6B 1 0.142447 0.635112 0.064199 11.00000 0.02826 0.01823 = 0.01554 0.00620 0.00455 0.00719 AFIX 137 H6D 2 0.144101 0.722251 0.033457 11.00000 -1.50000 H6E 2 0.026000 0.606206 0.068303 11.00000 -1.50000 H6F 2 0.201202 0.572865 0.020752 11.00000 -1.50000 AFIX 0 C7B 1 0.157560 0.405111 0.184371 11.00000 0.02892 0.01449 = 0.01844 0.00264 0.00362 0.00269 AFIX 137 H7D 2 0.038753 0.421044 0.164962 11.00000 -1.50000 H7E 2 0.167422 0.336550 0.236714 11.00000 -1.50000 H7F 2 0.214041 0.376744 0.122612 11.00000 -1.50000 AFIX 0 N1B 3 0.226715 0.641151 0.169590 11.00000 0.01916 0.01404 = 0.01191 0.00451 0.00260 0.00577 O1B 4 0.329927 0.423955 0.381172 11.00000 0.03486 0.01047 = 0.01911 0.00631 -0.00325 -0.00054 H1OB 2 0.401996 0.433171 0.433982 11.00000 0.01541 O2B 4 0.483744 0.654219 0.454840 11.00000 0.02866 0.01455 = 0.01467 0.00259 -0.00137 0.00818 MOLE 3 C8 1 0.071964 0.899889 0.654140 11.00000 0.01348 0.00881 = 0.00806 -0.00188 0.00112 -0.00152 C9 1 -0.101383 0.910233 0.653433 11.00000 0.00972 0.01223 = 0.01100 0.00180 -0.00163 0.00063 AFIX 43 H9 2 -0.168462 0.911490 0.589668 11.00000 -1.20000 AFIX 0 C10 1 -0.174454 0.918716 0.748449 11.00000 0.00619 0.00240 = 0.01375 0.00016 0.00048 -0.00230 C11 1 -0.078931 0.921872 0.842880 11.00000 0.01170 0.00781 = 0.01078 0.00004 0.00227 -0.00156 AFIX 43 H11 2 -0.130662 0.931263 0.906883 11.00000 -1.20000 AFIX 0 C12 1 0.094867 0.910877 0.841097 11.00000 0.01160 0.00573 = 0.01084 0.00190 -0.00068 -0.00132 C13 1 0.172210 0.899208 0.747237 11.00000 0.00745 0.01025 = 0.01188 -0.00083 -0.00085 0.00101 AFIX 43 H13 2 0.290568 0.890981 0.746785 11.00000 -1.20000 AFIX 0 O3 4 0.139643 0.890567 0.560042 11.00000 0.00915 0.03768 = 0.01022 -0.00332 0.00166 -0.00077 H3O 2 0.248780 0.890024 0.568664 11.00000 0.03482 O4 4 -0.346838 0.922147 0.749283 11.00000 0.00635 0.01520 = 0.01183 0.00126 -0.00135 0.00009 AFIX 3 H4O 2 -0.383223 0.933341 0.687952 11.00000 -1.50000 AFIX 0 O5 4 0.184947 0.912248 0.934965 11.00000 0.01016 0.01834 = 0.01179 0.00086 -0.00255 -0.00166 H5O 2 0.282693 0.911366 0.929740 11.00000 0.05628 MOLE 4 O1W 4 0.479900 0.885957 0.558057 11.00000 0.01210 0.01014 = 0.01594 0.00171 0.00029 0.00011 AFIX 3 H1W 2 0.491418 0.813132 0.524821 11.00000 -1.50000 H2W 2 0.535172 0.877486 0.625250 10.50000 -1.50000 H2WD 2 0.492888 0.952574 0.520027 10.50000 -1.50000 AFIX 0 MOLE 5 O2W 4 0.517319 0.881887 0.936954 11.00000 0.01774 0.00987 = 0.01252 0.00294 -0.00383 0.00075 AFIX 3 H3W 2 0.541136 0.810013 0.966539 11.00000 -1.50000 H4W 2 0.558828 0.894838 0.873059 11.00000 -1.50000 REM ##### REM ##### AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM KA1017_0m_a.res in P-1 REM wR2 = 0.2045, GooF = S = 1.246, Restrained GooF = 1.246 for all data REM R1 = 0.0841 for 4349 Fo > 4sig(Fo) and 0.0860 for all 4542 data REM 300 parameters refined using 0 restraints END WGHT 0.0000 4.4408 REM Highest difference peak 0.475, deepest hole -0.559, 1-sigma level 0.100 Q1 1 -0.1318 0.8571 0.8995 11.00000 0.05 0.48 Q2 1 0.3598 0.5971 0.3472 11.00000 0.05 0.39 Q3 1 0.6792 0.6016 1.1449 11.00000 0.05 0.39 Q4 1 -0.3866 0.8874 0.8046 11.00000 0.05 0.39 Q5 1 0.2926 0.6619 0.0389 11.00000 0.05 0.38 ; _shelx_res_checksum 67527 _shelx_hkl_file ; -2 0 0 1171.59 90.71 2 0 0 1165.02 90.58 -3 0 0 1890.52 147.34 3 0 0 1907.61 147.10 -4 0 0 364.19 31.23 4 0 0 398.45 30.99 4 0 0 432.75 30.95 4 0 0 414.36 31.24 -5 0 0 45.94 4.73 5 0 0 52.07 4.63 5 0 0 61.00 4.25 5 0 0 53.20 4.30 6 0 0 192.15 13.90 6 0 0 171.73 13.95 6 0 0 171.99 13.94 6 0 0 180.48 14.32 7 0 0 85.41 7.23 7 0 0 86.40 6.84 7 0 0 85.09 6.80 7 0 0 82.81 6.75 8 0 0 3.65 0.86 8 0 0 3.26 0.73 8 0 0 2.68 0.89 8 0 0 3.81 1.23 9 0 0 11.24 1.61 9 0 0 10.29 1.53 9 0 0 10.08 1.69 9 0 0 12.24 2.54 10 0 0 3.91 1.08 11 0 0 84.95 8.19 11 -1 0 63.88 6.02 10 -1 0 47.53 4.42 9 -1 0 46.41 3.96 9 -1 0 41.60 3.87 9 -1 0 48.22 4.70 9 -1 0 41.18 3.95 8 -1 0 17.78 1.82 8 -1 0 16.20 1.90 8 -1 0 16.10 2.00 8 -1 0 18.41 2.46 -8 1 0 11.37 2.51 7 -1 0 14.16 1.72 7 -1 0 17.30 1.66 7 -1 0 14.35 1.61 -7 1 0 10.70 2.12 6 -1 0 77.28 6.34 6 -1 0 80.08 5.97 6 -1 0 76.87 6.02 -6 1 0 63.12 6.46 5 -1 0 495.13 36.51 5 -1 0 516.95 36.45 5 -1 0 508.31 36.50 5 -1 0 497.59 36.76 -5 1 0 433.13 36.36 -5 1 0 423.17 36.74 -5 1 0 440.28 36.35 4 -1 0 4.86 0.75 4 -1 0 7.22 0.85 3 -1 0 844.35 59.87 -3 1 0 737.64 59.86 -3 1 0 750.33 59.69 2 -1 0 1990.38 154.25 -1 -1 0 1077.30 84.56 1 1 0 1119.00 84.52 2 1 0 643.97 49.60 3 1 0 1089.48 83.83 4 1 0 325.77 23.36 4 1 0 290.02 23.72 4 1 0 295.89 23.39 5 1 0 132.41 10.65 5 1 0 132.26 10.18 5 1 0 130.55 10.25 6 1 0 88.24 7.94 6 1 0 96.04 7.52 6 1 0 101.47 7.46 7 1 0 124.71 10.49 7 1 0 127.54 9.98 7 1 0 128.75 9.92 8 1 0 2.75 1.13 8 1 0 1.71 0.53 8 1 0 1.92 0.73 8 1 0 2.05 0.83 9 1 0 73.22 6.73 9 1 0 72.52 5.92 9 1 0 71.67 5.89 10 1 0 -0.50 0.72 11 -2 0 40.87 4.17 11 -2 0 38.09 5.11 10 -2 0 7.21 1.64 10 -2 0 7.40 2.35 9 -2 0 130.44 11.14 9 -2 0 146.42 11.30 9 -2 0 147.28 11.74 9 -2 0 137.38 11.19 8 -2 0 126.06 10.58 8 -2 0 125.64 10.21 8 -2 0 126.30 10.15 8 -2 0 131.91 10.21 7 -2 0 431.19 33.83 7 -2 0 425.16 34.19 7 -2 0 427.42 33.91 7 -2 0 467.74 33.90 6 -2 0 89.19 6.55 6 -2 0 90.39 6.61 6 -2 0 83.96 6.61 6 -2 0 85.34 6.89 -6 2 0 71.39 7.02 -6 2 0 73.17 6.47 -6 2 0 78.45 6.40 5 -2 0 135.91 9.78 5 -2 0 122.74 9.52 5 -2 0 124.26 9.52 5 -2 0 119.18 9.50 -5 2 0 107.05 9.44 -5 2 0 115.31 9.38 4 -2 0 52.29 3.87 4 -2 0 51.74 3.89 4 -2 0 44.94 3.91 4 -2 0 52.67 4.13 -4 2 0 41.38 4.16 -4 2 0 43.61 3.90 -4 2 0 46.55 3.82 3 -2 0 2.73 0.47 3 -2 0 2.06 0.54 3 -2 0 1.95 0.45 -3 2 0 2.81 0.62 2 -2 0 1082.71 93.33 -2 2 0 1298.49 93.87 1 -2 0 86.36 6.57 1 -2 0 79.62 6.61 1 -2 0 87.40 6.59 -1 2 0 96.10 6.60 -1 2 0 77.58 6.57 -1 2 0 79.38 6.60 0 -2 0 1027.56 79.59 0 2 0 1013.43 79.60 -1 -2 0 309.21 26.32 1 2 0 375.46 26.33 2 2 0 28.95 2.35 3 2 0 86.39 7.91 3 2 0 117.61 8.26 4 2 0 8.06 1.40 4 2 0 9.67 0.75 4 2 0 9.22 0.74 5 2 0 207.57 17.25 5 2 0 224.38 16.72 5 2 0 219.55 16.76 6 2 0 16.44 1.40 6 2 0 15.56 1.55 6 2 0 15.08 2.07 7 2 0 16.03 1.52 8 2 0 13.16 1.39 8 2 0 10.16 1.60 8 2 0 17.25 2.33 9 2 0 43.64 4.36 9 2 0 32.59 3.18 9 2 0 35.43 3.12 9 2 0 35.47 3.07 10 2 0 19.63 2.36 10 2 0 27.94 4.18 10 2 0 31.39 2.47 11 2 0 11.99 2.74 11 2 0 13.37 2.48 11 -3 0 -0.07 1.96 11 -3 0 -1.06 1.71 10 -3 0 -0.17 1.46 10 -3 0 0.70 1.81 9 -3 0 60.19 5.58 9 -3 0 52.05 4.88 9 -3 0 57.11 5.07 8 -3 0 62.84 5.22 8 -3 0 58.39 5.07 8 -3 0 62.91 5.53 8 -3 0 57.12 5.19 7 -3 0 104.44 7.96 7 -3 0 107.00 7.64 7 -3 0 100.39 7.65 7 -3 0 93.76 7.53 -7 3 0 81.49 7.35 -7 3 0 77.12 7.46 6 -3 0 26.69 2.56 6 -3 0 21.58 2.21 6 -3 0 24.85 2.21 6 -3 0 21.23 2.18 -6 3 0 22.17 2.01 -6 3 0 17.19 2.28 -6 3 0 20.38 2.82 5 -3 0 17.42 1.90 5 -3 0 22.68 1.97 5 -3 0 19.64 1.95 -5 3 0 24.73 2.13 -5 3 0 17.15 1.81 4 -3 0 167.89 13.09 4 -3 0 177.68 13.08 4 -3 0 159.27 13.01 -4 3 0 175.37 13.11 -4 3 0 156.07 12.99 3 -3 0 24.49 2.02 3 -3 0 21.25 2.04 3 -3 0 22.18 2.00 -3 3 0 21.69 1.96 -3 3 0 22.02 1.96 -3 3 0 23.66 2.11 2 -3 0 484.35 36.98 2 -3 0 504.43 37.04 -2 3 0 499.95 37.04 -2 3 0 452.68 36.97 -2 3 0 462.49 37.00 1 -3 0 29.01 2.37 1 -3 0 26.89 2.31 1 -3 0 30.64 2.34 -1 3 0 26.05 2.30 -1 3 0 27.85 2.34 -1 3 0 29.11 2.38 0 -3 0 46.28 3.65 0 -3 0 47.28 3.71 0 3 0 41.97 3.68 0 3 0 48.95 3.70 -1 -3 0 155.01 12.22 -1 -3 0 171.20 12.22 -1 -3 0 155.93 12.30 1 3 0 154.14 12.17 1 3 0 145.05 12.33 1 3 0 165.53 12.23 1 3 0 162.76 12.24 -2 -3 0 1974.58 162.42 2 3 0 2230.07 162.45 3 3 0 136.76 10.32 3 3 0 145.54 10.31 3 3 0 119.72 10.44 4 3 0 1087.95 91.44 4 3 0 1294.73 91.90 5 3 0 370.12 28.41 5 3 0 358.35 29.05 5 3 0 381.53 28.43 6 3 0 0.96 0.31 6 3 0 1.58 0.43 6 3 0 1.36 0.94 6 3 0 1.58 0.51 7 3 0 2.53 0.65 7 3 0 4.86 0.76 7 3 0 4.24 0.60 8 3 0 4.74 0.81 8 3 0 5.78 0.87 8 3 0 5.15 1.58 9 3 0 3.29 0.74 9 3 0 5.13 1.91 9 3 0 4.71 0.65 10 3 0 6.15 1.89 10 3 0 3.10 2.17 11 3 0 -0.66 2.23 11 3 0 2.51 1.90 10 -4 0 5.01 1.89 10 -4 0 6.73 2.22 9 -4 0 17.94 3.15 8 -4 0 3.61 1.17 8 -4 0 1.27 1.22 8 -4 0 2.33 1.00 -8 4 0 0.98 1.55 -8 4 0 1.14 0.97 7 -4 0 9.35 1.49 7 -4 0 9.25 1.57 7 -4 0 10.89 1.66 -7 4 0 10.17 2.22 -7 4 0 9.55 1.31 -7 4 0 7.76 1.51 6 -4 0 20.58 2.20 6 -4 0 20.49 2.15 6 -4 0 19.49 2.11 -6 4 0 19.94 2.42 -6 4 0 24.37 3.08 -6 4 0 17.35 1.94 5 -4 0 47.84 3.69 5 -4 0 45.31 3.70 5 -4 0 39.12 3.57 -5 4 0 42.25 3.54 -5 4 0 37.14 4.00 -5 4 0 40.75 3.78 4 -4 0 322.28 23.25 4 -4 0 292.62 23.20 4 -4 0 302.25 23.28 4 -4 0 337.07 23.48 -4 4 0 275.76 23.46 -4 4 0 281.32 23.18 -4 4 0 286.65 23.28 3 -4 0 2679.48 232.56 -3 4 0 3292.36 233.72 -2 4 0 1659.55 130.72 -2 4 0 1745.53 130.85 1 -4 0 41.45 3.34 1 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0 137.19 9.80 -7 5 0 108.55 9.83 -7 5 0 115.27 9.61 6 -5 0 71.07 6.14 6 -5 0 85.15 6.18 6 -5 0 73.41 6.05 6 -5 0 86.18 6.45 -6 5 0 72.61 5.99 -6 5 0 63.37 6.22 -6 5 0 59.98 6.54 5 -5 0 180.57 14.32 5 -5 0 187.44 14.24 5 -5 0 194.38 14.30 -5 5 0 163.90 14.31 -5 5 0 181.40 14.63 -5 5 0 180.14 14.20 4 -5 0 4.80 1.03 4 -5 0 5.32 0.95 4 -5 0 4.72 0.88 -4 5 0 5.13 1.25 -4 5 0 5.74 0.97 -4 5 0 4.25 1.04 -4 5 0 4.05 0.78 3 -5 0 179.13 14.67 3 -5 0 206.23 14.68 3 -5 0 191.46 14.61 -3 5 0 177.41 14.64 -3 5 0 182.98 14.69 -3 5 0 186.71 14.60 2 -5 0 8.79 1.20 2 -5 0 8.18 1.16 2 -5 0 6.31 1.09 -2 5 0 7.65 1.00 -2 5 0 9.00 1.34 -2 5 0 10.91 1.12 1 -5 0 63.28 5.07 1 -5 0 62.30 5.04 -1 5 0 69.07 5.10 -1 5 0 54.04 5.22 -1 5 0 57.82 5.01 -1 5 0 71.42 5.58 0 -5 0 1482.43 134.45 0 5 0 1950.56 135.54 -1 -5 0 209.26 15.24 -1 -5 0 186.40 15.23 -1 -5 0 192.78 15.35 -1 -5 0 176.09 15.13 1 5 0 221.85 15.34 1 5 0 196.37 15.24 -2 -5 0 375.40 28.86 -2 -5 0 350.49 28.86 -2 -5 0 336.11 29.03 2 5 0 415.55 28.93 2 5 0 401.56 28.96 3 5 0 813.56 62.18 3 5 0 805.62 62.27 4 5 0 12.54 1.13 4 5 0 13.60 1.23 4 5 0 11.21 1.18 4 5 0 12.69 1.30 5 5 0 290.88 23.59 5 5 0 310.34 23.65 5 5 0 291.45 24.28 5 5 0 310.75 23.47 5 5 0 320.75 23.50 6 5 0 26.23 2.56 6 5 0 26.36 3.57 6 5 0 30.14 2.35 6 5 0 30.88 2.42 6 5 0 27.18 2.53 7 5 0 57.42 4.95 7 5 0 66.80 4.84 7 5 0 63.23 4.85 7 5 0 55.82 5.95 7 5 0 55.92 5.01 8 5 0 105.06 8.79 8 5 0 125.31 8.68 8 5 0 101.23 8.92 8 5 0 107.42 9.91 8 5 0 110.56 8.80 9 5 0 19.48 2.70 9 5 0 22.85 3.88 9 5 0 19.23 1.94 10 5 0 9.76 3.18 10 5 0 8.02 1.83 10 -6 0 13.54 2.96 10 -6 0 15.68 2.67 9 -6 0 -0.93 1.70 9 -6 0 0.41 1.93 -9 6 0 -0.40 0.83 8 -6 0 31.47 3.91 8 -6 0 24.17 3.22 -8 6 0 26.43 2.88 -8 6 0 19.96 2.69 7 -6 0 47.90 4.22 -7 6 0 36.75 4.57 -7 6 0 49.98 4.01 -7 6 0 41.60 4.37 6 -6 0 39.22 3.50 6 -6 0 38.96 3.70 6 -6 0 45.09 3.97 6 -6 0 35.08 3.52 -6 6 0 33.51 3.91 -6 6 0 29.08 4.14 -6 6 0 42.57 3.50 5 -6 0 4.98 1.05 5 -6 0 4.40 1.14 5 -6 0 3.31 0.99 -5 6 0 5.15 1.04 -5 6 0 6.23 1.39 -5 6 0 4.22 1.60 4 -6 0 91.00 7.50 4 -6 0 99.01 7.56 4 -6 0 94.62 7.59 -4 6 0 85.06 7.50 -4 6 0 96.75 7.49 -4 6 0 91.55 7.67 3 -6 0 82.87 6.89 3 -6 0 84.17 6.97 3 -6 0 92.52 6.97 -3 6 0 85.57 6.87 -3 6 0 84.50 7.01 -3 6 0 84.96 7.28 -3 6 0 84.07 6.92 2 -6 0 465.75 36.20 2 -6 0 485.96 36.27 -2 6 0 475.38 36.27 -2 6 0 456.50 36.27 -2 6 0 500.56 36.49 -2 6 0 430.37 36.18 1 -6 0 14.19 1.53 1 -6 0 14.97 1.51 1 -6 0 12.57 1.47 -1 6 0 14.56 1.66 -1 6 0 15.17 1.51 -1 6 0 12.56 1.39 0 -6 0 1643.72 131.93 0 -6 0 1802.16 132.03 0 -6 0 1742.92 131.92 0 6 0 1685.77 131.98 -1 -6 0 611.34 43.99 -1 -6 0 549.67 43.97 -1 -6 0 564.51 44.12 -1 -6 0 507.72 43.86 1 6 0 635.71 44.10 1 6 0 562.32 43.99 -2 -6 0 43.15 3.64 2 6 0 44.56 3.69 2 6 0 47.17 3.78 2 6 0 49.36 3.81 3 6 0 17.64 1.54 3 6 0 18.39 1.68 3 6 0 17.59 1.38 3 6 0 16.44 1.68 4 6 0 310.97 23.34 4 6 0 306.62 23.23 4 6 0 294.76 23.17 4 6 0 291.63 23.19 5 6 0 20.58 1.81 5 6 0 18.45 1.75 5 6 0 19.19 1.66 5 6 0 19.82 1.86 6 6 0 13.44 2.97 6 6 0 16.13 1.67 6 6 0 18.20 1.73 6 6 0 18.22 1.69 7 6 0 31.37 2.71 7 6 0 29.02 4.08 7 6 0 27.68 2.74 7 6 0 32.36 2.64 8 6 0 33.53 3.21 8 6 0 35.31 3.06 9 6 0 12.00 1.44 9 6 0 7.98 1.56 9 6 0 10.40 2.87 10 6 0 1.18 2.96 -9 7 0 3.46 1.41 8 -7 0 31.95 3.64 -8 7 0 24.72 3.22 7 -7 0 30.85 3.33 -7 7 0 25.76 3.13 -7 7 0 31.61 3.32 6 -7 0 -2.02 1.06 -6 7 0 -0.34 1.09 -6 7 0 0.05 1.26 -6 7 0 -0.13 0.98 5 -7 0 8.75 1.38 5 -7 0 9.77 1.55 5 -7 0 6.74 1.56 -5 7 0 10.45 1.68 -5 7 0 9.48 1.45 -5 7 0 9.05 1.59 -5 7 0 8.21 1.97 4 -7 0 227.37 17.94 4 -7 0 252.41 18.05 -4 7 0 228.30 18.00 -4 7 0 218.68 18.05 -4 7 0 221.53 18.33 -4 7 0 226.48 17.94 3 -7 0 273.25 20.38 3 -7 0 258.97 20.29 -3 7 0 249.11 20.27 -3 7 0 243.97 20.39 -3 7 0 286.61 20.70 -3 7 0 250.55 20.34 2 -7 0 86.14 7.33 2 -7 0 95.17 7.43 2 -7 0 85.53 7.36 -2 7 0 104.45 7.80 -2 7 0 89.01 7.38 -2 7 0 98.80 7.43 -2 7 0 81.97 7.29 1 -7 0 6.02 1.13 1 -7 0 5.24 0.95 1 -7 0 6.93 0.91 1 -7 0 7.02 1.16 -1 7 0 7.89 1.01 -1 7 0 9.53 1.17 -1 7 0 7.29 1.20 0 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21.10 4.13 9 8 0 13.30 3.52 8 -9 0 14.04 2.27 -8 9 0 16.49 2.68 7 -9 0 19.35 2.94 -7 9 0 24.34 3.04 6 -9 0 10.10 1.89 -6 9 0 14.33 2.27 5 -9 0 0.42 1.11 -5 9 0 0.50 1.14 -5 9 0 0.38 1.02 -4 9 0 49.09 4.63 -4 9 0 44.79 4.44 3 -9 0 53.15 4.88 -3 9 0 57.24 4.90 -3 9 0 54.86 4.76 2 -9 0 56.27 4.92 2 -9 0 57.66 4.92 2 -9 0 56.22 4.64 2 -9 0 57.66 4.85 -2 9 0 52.88 5.36 -2 9 0 57.40 4.91 -2 9 0 57.16 4.82 -2 9 0 55.16 5.00 1 -9 0 295.72 24.42 1 -9 0 303.87 24.12 1 -9 0 317.78 24.31 1 -9 0 320.12 24.36 -1 9 0 292.39 24.40 -1 9 0 305.03 24.30 -1 9 0 305.18 24.39 -1 9 0 361.29 24.86 0 -9 0 1504.48 116.25 0 -9 0 1474.90 116.40 0 -9 0 1562.75 116.24 0 -9 0 1387.75 116.04 0 9 0 1500.58 116.25 0 9 0 1578.51 116.38 0 9 0 1580.63 116.37 -1 -9 0 22.80 3.15 -1 -9 0 31.00 2.73 -1 -9 0 29.62 2.84 1 9 0 33.23 2.90 1 9 0 32.09 2.73 1 9 0 29.49 3.03 -2 -9 0 9.17 1.26 -2 -9 0 10.62 1.45 -2 -9 0 8.90 1.62 2 9 0 12.05 1.37 2 9 0 12.66 1.55 2 9 0 11.25 1.65 3 9 0 93.74 7.52 3 9 0 86.47 7.37 3 9 0 98.29 7.63 4 9 0 64.30 5.27 4 9 0 60.48 5.09 4 9 0 63.06 5.41 5 9 0 66.40 5.20 5 9 0 56.74 4.97 6 9 0 1.29 0.72 6 9 0 1.81 0.54 7 9 0 3.39 0.62 7 9 0 1.66 2.61 7 9 0 2.22 0.87 8 9 0 0.36 2.61 8 -10 0 4.30 1.44 -8 10 0 3.43 2.12 7 -10 0 -1.29 1.40 -7 10 0 3.39 1.82 6 -10 0 -0.67 1.50 -6 10 0 0.46 1.59 5 -10 0 16.62 2.62 -5 10 0 16.28 2.49 -5 10 0 16.68 2.51 4 -10 0 5.42 1.62 -4 10 0 5.86 1.43 -4 10 0 5.84 1.39 3 -10 0 232.98 21.05 3 -10 0 268.16 20.10 -3 10 0 255.22 20.27 -3 10 0 271.86 20.41 2 -10 0 239.71 17.76 2 -10 0 227.63 17.45 -2 10 0 205.15 17.80 1 -10 0 222.56 18.24 1 -10 0 234.02 18.49 1 -10 0 235.49 18.46 -1 10 0 238.57 18.47 -1 10 0 246.91 18.58 0 -10 0 129.44 10.01 0 -10 0 125.44 10.01 0 -10 0 112.65 9.70 0 10 0 130.08 10.10 0 10 0 128.34 9.99 -1 -10 0 121.75 10.10 -1 -10 0 121.00 10.14 1 10 0 125.94 10.16 1 10 0 142.11 10.32 1 10 0 127.38 10.31 -2 -10 0 1.72 0.60 -2 -10 0 1.67 0.82 -2 -10 0 2.71 1.06 2 10 0 2.97 0.90 2 10 0 5.04 1.10 -3 -10 0 12.32 2.14 3 10 0 16.17 2.30 3 10 0 18.50 1.85 3 10 0 18.82 2.06 -4 -10 0 15.08 1.98 4 10 0 12.70 1.82 4 10 0 10.36 1.50 5 10 0 29.36 2.86 5 10 0 28.44 3.21 5 10 0 37.53 3.16 6 10 0 25.65 2.63 6 10 0 34.14 3.06 7 10 0 26.17 4.99 7 10 0 40.38 3.41 8 10 0 8.34 3.24 7 -11 0 93.44 8.13 -7 11 0 95.78 8.31 6 -11 0 1.00 1.48 -6 11 0 -0.86 1.50 5 -11 0 12.26 2.28 -5 11 0 13.75 2.15 -5 11 0 14.64 2.53 4 -11 0 69.87 6.24 -4 11 0 68.03 6.17 -4 11 0 69.67 6.09 3 -11 0 21.21 2.27 3 -11 0 26.27 3.01 -3 11 0 24.05 2.83 -3 11 0 22.59 2.80 2 -11 0 132.04 11.18 2 -11 0 129.63 10.78 -2 11 0 139.93 11.08 -2 11 0 147.98 11.22 1 -11 0 14.42 2.04 1 -11 0 17.55 2.42 -1 11 0 15.30 2.16 -1 11 0 15.08 2.04 0 -11 0 255.33 21.05 0 -11 0 252.98 20.78 0 -11 0 282.77 21.12 0 11 0 288.88 21.25 -1 -11 0 177.62 14.43 -1 -11 0 171.86 14.41 1 11 0 195.31 14.68 1 11 0 190.25 14.54 -2 -11 0 18.80 1.78 -2 -11 0 17.53 1.93 2 11 0 20.62 2.22 3 11 0 15.69 2.00 4 11 0 37.38 3.45 5 11 0 74.06 6.45 5 11 0 70.99 6.04 6 11 0 5.56 1.28 6 11 0 3.65 0.91 7 11 0 0.08 2.67 7 11 0 6.33 1.64 6 -12 0 4.22 1.41 -6 12 0 5.28 1.50 5 -12 0 -1.13 1.63 -5 12 0 -1.03 1.13 -5 12 0 -0.48 1.38 4 -12 0 19.94 3.34 -4 12 0 25.35 2.93 -4 12 0 16.88 2.72 3 -12 0 -0.30 1.64 -3 12 0 2.83 1.31 -3 12 0 2.24 1.31 2 -12 0 126.50 9.82 -2 12 0 116.35 9.74 -2 12 0 109.80 9.66 1 -12 0 0.06 1.37 -1 12 0 1.62 1.11 -1 12 0 0.98 1.09 0 -12 0 256.30 19.97 0 12 0 254.70 20.09 0 12 0 250.87 20.01 -1 -12 0 149.92 12.72 1 12 0 176.42 13.04 1 12 0 156.35 13.18 2 12 0 85.58 7.56 2 12 0 96.65 7.70 3 12 0 6.00 1.36 3 12 0 4.33 1.29 4 12 0 377.41 29.51 5 12 0 10.09 1.82 6 12 0 0.51 1.09 5 -13 0 1.96 1.74 -5 13 0 4.34 1.37 -5 13 0 3.88 1.47 4 -13 0 36.93 4.23 -4 13 0 32.63 3.63 -4 13 0 38.26 3.70 3 -13 0 40.80 4.45 -3 13 0 36.73 3.91 -3 13 0 37.68 4.01 2 -13 0 46.33 4.98 -2 13 0 46.56 4.49 -2 13 0 43.51 4.38 1 -13 0 68.87 6.62 -1 13 0 75.66 6.52 -1 13 0 75.45 6.50 0 13 0 14.80 2.36 0 13 0 10.87 1.90 -1 -13 0 91.01 8.06 1 13 0 103.96 8.44 1 13 0 105.04 8.42 2 13 0 212.57 17.16 2 13 0 218.98 17.23 3 13 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73.60 6.37 8 -4 9 76.14 6.94 8 -4 9 71.84 7.48 9 -4 9 2.39 2.03 9 -4 9 6.35 1.87 10 3 -9 26.14 4.50 10 3 -9 39.12 3.94 9 3 -9 53.93 6.84 9 3 -9 83.05 6.49 8 3 -9 70.73 6.22 8 3 -9 65.40 5.62 7 3 -9 0.35 1.18 7 3 -9 -0.63 0.66 7 3 -9 0.64 1.04 6 3 -9 31.98 3.29 6 3 -9 28.64 3.18 6 3 -9 30.27 2.80 5 3 -9 13.90 1.63 5 3 -9 10.94 1.84 5 3 -9 16.77 2.22 4 3 -9 3.81 1.02 4 3 -9 5.00 0.95 4 3 -9 2.80 1.19 4 3 -9 5.77 1.27 4 3 -9 4.73 0.87 -4 -3 9 3.81 1.20 3 3 -9 119.00 9.47 3 3 -9 120.54 9.48 3 3 -9 109.90 9.38 3 3 -9 117.11 9.56 -3 -3 9 125.44 9.30 -3 -3 9 107.88 9.52 -3 -3 9 127.43 9.34 2 3 -9 2.50 0.80 2 3 -9 1.95 0.86 2 3 -9 2.78 1.10 2 3 -9 0.14 0.77 -2 -3 9 1.81 0.69 -2 -3 9 0.89 0.91 -2 -3 9 1.24 0.75 1 3 -9 63.98 4.94 1 3 -9 57.37 5.20 1 3 -9 57.51 4.97 1 3 -9 48.32 5.02 1 3 -9 56.13 5.08 -1 -3 9 60.44 5.00 -1 -3 9 68.29 5.04 -1 -3 9 61.92 4.97 0 3 -9 188.78 15.56 0 3 -9 212.53 15.53 0 3 -9 167.44 15.47 0 3 -9 189.77 15.72 0 3 -9 215.58 15.44 0 -3 9 196.30 15.46 0 -3 9 202.30 15.53 0 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-1 -16 9.02 1.75 2 -1 -16 6.29 1.81 -2 1 16 5.03 1.17 -2 1 16 7.38 2.27 1 -1 -16 54.33 4.64 1 -1 -16 43.30 4.79 -1 1 16 44.80 4.64 -1 1 16 50.50 5.18 0 -1 -16 0.96 1.37 0 -1 -16 -0.67 1.38 0 -1 -16 1.57 1.50 0 1 16 3.86 2.00 0 1 16 0.83 1.65 -1 -1 -16 21.32 3.35 -1 -1 -16 31.36 3.26 -1 -1 -16 29.97 3.66 1 1 16 31.51 4.54 1 1 16 31.55 4.12 -2 -1 -16 0.65 0.99 -2 -1 -16 2.71 1.74 -2 -1 -16 3.78 1.40 2 1 16 2.48 2.37 2 1 16 3.21 1.86 -3 -1 -16 53.92 5.26 -3 -1 -16 60.07 4.99 3 1 16 53.77 5.53 3 1 16 42.59 6.49 -4 -1 -16 154.66 12.05 4 1 16 140.44 13.07 4 1 16 138.96 12.17 6 -2 -16 31.46 3.88 6 -2 -16 34.63 3.88 5 -2 -16 2.88 1.34 5 -2 -16 5.86 1.80 -5 2 16 4.79 2.20 4 -2 -16 13.43 2.32 4 -2 -16 11.23 2.11 -4 2 16 12.28 2.77 3 -2 -16 152.65 12.26 3 -2 -16 146.31 12.47 -3 2 16 150.59 12.59 2 -2 -16 170.85 12.89 2 -2 -16 154.05 12.97 -2 2 16 161.63 13.17 -2 2 16 145.81 12.85 1 -2 -16 42.41 4.07 1 -2 -16 43.16 4.29 -1 2 16 32.89 4.12 -1 2 16 43.16 4.63 0 -2 -16 4.20 1.77 0 -2 -16 4.31 1.46 0 2 16 3.06 1.91 0 2 16 5.86 2.00 -1 -2 -16 13.99 2.63 -1 -2 -16 13.16 2.38 -1 -2 -16 17.38 2.69 1 2 16 15.71 2.96 1 2 16 19.40 2.83 -2 -2 -16 10.74 2.09 -2 -2 -16 6.88 1.26 2 2 16 9.94 2.36 2 2 16 12.11 2.98 -3 -2 -16 12.22 2.02 -3 -2 -16 11.33 2.23 3 2 16 10.84 3.15 3 2 16 11.37 2.46 -4 -2 -16 54.37 4.99 4 2 16 39.78 4.79 4 2 16 47.97 6.08 5 -3 -16 8.41 1.92 5 -3 -16 11.72 1.86 -5 3 16 10.84 2.65 4 -3 -16 4.65 1.77 -4 3 16 8.15 2.52 3 -3 -16 9.62 2.10 3 -3 -16 10.29 2.00 -3 3 16 10.19 2.52 2 -3 -16 27.78 3.80 2 -3 -16 32.76 3.52 -2 3 16 31.99 4.27 1 -3 -16 60.22 5.10 1 -3 -16 50.72 5.35 -1 3 16 51.35 5.31 -1 3 16 53.40 5.59 0 -3 -16 24.40 2.96 0 -3 -16 18.34 3.21 0 3 16 24.01 3.59 0 3 16 24.16 4.16 -1 -3 -16 16.88 2.58 -1 -3 -16 16.65 2.76 1 3 16 14.98 3.24 1 3 16 14.09 2.70 -2 -3 -16 10.65 2.00 -2 -3 -16 13.41 2.31 2 3 16 10.30 3.07 2 3 16 17.34 2.70 -3 -3 -16 -0.07 1.46 -3 -3 -16 -3.27 1.65 3 3 16 2.78 1.57 3 3 16 -0.57 2.55 -4 -3 -16 48.11 5.05 4 3 16 43.74 5.99 4 3 16 49.96 5.07 5 -4 -16 26.48 2.86 5 -4 -16 22.45 3.19 -5 4 16 18.26 3.23 4 -4 -16 3.46 1.55 4 -4 -16 5.89 1.75 -4 4 16 3.88 2.36 3 -4 -16 32.41 4.27 3 -4 -16 43.62 4.30 -3 4 16 44.26 4.74 2 -4 -16 28.07 3.43 2 -4 -16 27.12 3.52 -2 4 16 30.33 4.23 1 -4 -16 8.29 1.99 1 -4 -16 12.60 2.02 -1 4 16 6.81 2.06 -1 4 16 12.75 2.40 0 -4 -16 58.69 5.28 0 -4 -16 57.25 5.68 0 4 16 54.72 5.91 0 4 16 56.34 6.51 -1 -4 -16 3.30 1.83 -1 -4 -16 2.02 1.59 1 4 16 2.30 1.70 1 4 16 2.00 2.58 -2 -4 -16 113.05 10.17 -2 -4 -16 140.11 9.99 2 4 16 108.05 11.29 2 4 16 113.59 10.24 -3 -4 -16 140.45 11.50 3 4 16 140.98 11.69 3 4 16 130.75 12.48 4 -5 -16 22.98 2.89 4 -5 -16 15.47 2.45 -4 5 16 18.37 3.16 3 -5 -16 68.17 6.24 3 -5 -16 65.82 6.14 -3 5 16 66.36 6.69 2 -5 -16 4.01 1.52 2 -5 -16 3.40 1.68 -2 5 16 7.15 2.13 1 -5 -16 187.71 14.20 1 -5 -16 166.43 14.34 -1 5 16 172.15 14.54 0 -5 -16 1.30 1.84 0 -5 -16 3.16 1.74 0 5 16 2.95 1.72 0 5 16 1.41 2.59 -1 -5 -16 58.71 5.68 1 5 16 54.64 5.43 1 5 16 54.82 7.32 -2 -5 -16 8.78 1.98 -2 -5 -16 7.35 2.20 2 5 16 5.18 3.08 2 5 16 7.93 1.84 -3 -5 -16 34.42 4.28 3 5 16 26.28 4.65 3 5 16 43.06 4.50 3 -6 -16 8.36 2.02 3 -6 -16 3.39 1.71 -3 6 16 7.30 1.90 2 -6 -16 61.89 6.60 2 -6 -16 86.76 6.83 -2 6 16 74.67 6.90 1 -6 -16 15.62 2.40 1 -6 -16 16.87 2.59 -1 6 16 19.45 3.10 0 -6 -16 5.74 1.79 0 -6 -16 10.24 2.00 0 6 16 7.86 3.00 -1 -6 -16 19.98 3.23 -1 -6 -16 18.28 2.66 1 6 16 12.08 3.45 1 6 16 12.74 2.30 -2 -6 -16 9.30 2.09 2 6 16 12.18 3.51 2 6 16 12.39 3.50 3 5 -17 40.04 4.41 2 5 -17 1.33 1.19 2 5 -17 1.45 1.49 2 5 -17 0.04 1.55 -2 -5 17 3.55 1.96 1 5 -17 13.30 2.06 1 5 -17 8.90 2.38 1 5 -17 17.81 2.59 -1 -5 17 15.00 3.02 0 5 -17 -1.12 1.96 0 5 -17 3.48 1.33 0 -5 17 2.80 2.37 -1 5 -17 -0.23 1.50 -1 5 -17 1.26 1.18 -1 5 -17 -0.84 1.72 1 -5 17 -0.88 1.82 1 -5 17 -0.05 2.20 3 4 -17 3.95 1.21 3 4 -17 -0.56 1.55 3 4 -17 0.56 1.62 2 4 -17 0.14 1.79 2 4 -17 0.96 1.06 2 4 -17 -0.70 1.49 -2 -4 17 0.97 2.34 1 4 -17 52.25 4.51 1 4 -17 42.29 4.61 1 4 -17 44.32 5.17 -1 -4 17 53.87 5.71 0 4 -17 21.58 2.30 0 4 -17 13.73 2.65 0 -4 17 16.54 3.46 0 -4 17 16.32 3.01 -1 4 -17 71.06 6.25 -1 4 -17 73.04 6.45 -1 4 -17 69.46 7.01 1 -4 17 75.24 7.10 1 -4 17 78.79 7.63 -2 4 -17 4.77 1.76 -2 4 -17 5.50 1.41 -2 4 -17 1.59 1.37 2 -4 17 7.16 2.94 4 3 -17 -2.47 1.50 4 3 -17 -0.70 1.24 4 3 -17 2.15 1.61 3 3 -17 60.91 5.80 3 3 -17 51.33 5.79 3 3 -17 62.14 5.25 2 3 -17 57.36 6.49 2 3 -17 65.34 6.17 2 3 -17 69.29 5.85 -2 -3 17 71.53 6.81 1 3 -17 2.18 1.23 1 3 -17 0.78 1.75 1 3 -17 3.01 1.50 -1 -3 17 4.04 2.36 0 3 -17 66.67 6.44 0 3 -17 73.60 6.32 0 -3 17 74.35 7.12 0 -3 17 75.99 6.86 -1 3 -17 12.27 1.94 -1 3 -17 7.21 2.11 -1 3 -17 7.79 1.63 1 -3 17 8.39 2.30 1 -3 17 9.59 2.71 -2 3 -17 61.61 6.14 -2 3 -17 68.89 6.04 -2 3 -17 75.14 6.01 2 -3 17 68.31 7.37 2 -3 17 65.19 6.35 -3 3 -17 7.54 1.72 3 -3 17 5.66 2.25 4 2 -17 22.57 3.31 4 2 -17 28.26 3.28 4 2 -17 18.56 2.70 3 2 -17 17.91 2.38 3 2 -17 15.57 2.57 -3 -2 17 17.59 2.95 2 2 -17 44.82 4.25 2 2 -17 40.67 4.46 -2 -2 17 40.17 5.31 1 2 -17 10.30 2.02 1 2 -17 6.86 1.68 1 2 -17 7.05 2.16 -1 -2 17 11.81 2.64 -1 -2 17 7.90 1.93 0 2 -17 0.66 1.26 0 2 -17 5.05 1.66 0 2 -17 1.04 1.98 0 -2 17 4.40 2.03 -1 2 -17 11.45 1.80 -1 2 -17 8.18 2.20 -1 2 -17 9.39 1.87 1 -2 17 9.24 2.74 1 -2 17 9.81 2.51 -2 2 -17 73.35 6.45 -2 2 -17 67.14 6.43 -2 2 -17 87.12 6.42 2 -2 17 70.72 6.85 2 -2 17 66.82 7.83 -3 2 -17 13.94 2.16 3 -2 17 16.50 2.44 3 -2 17 13.45 3.39 5 1 -17 17.33 3.08 5 1 -17 15.81 2.48 4 1 -17 14.22 2.53 4 1 -17 20.90 3.10 4 1 -17 14.88 2.34 3 1 -17 2.26 1.69 3 1 -17 3.06 1.76 3 1 -17 1.40 1.22 -3 -1 17 2.00 2.29 2 1 -17 8.66 2.28 2 1 -17 17.73 2.55 2 1 -17 13.06 2.27 -2 -1 17 14.57 2.84 1 1 -17 36.34 4.95 1 1 -17 42.85 4.67 1 1 -17 50.71 4.30 -1 -1 17 38.51 4.54 -1 -1 17 46.48 5.22 0 1 -17 5.41 1.63 0 1 -17 4.63 1.73 0 1 -17 3.67 1.95 0 -1 17 3.44 2.14 0 -1 17 7.63 2.14 -1 1 -17 50.17 5.25 -1 1 -17 43.58 5.35 -1 1 -17 65.28 5.08 1 -1 17 53.95 5.60 1 -1 17 53.95 6.30 -2 1 -17 4.68 1.53 -2 1 -17 6.02 1.45 -2 1 -17 1.70 1.45 2 -1 17 10.01 1.97 2 -1 17 -0.78 2.59 -3 1 -17 7.88 1.58 3 -1 17 5.39 2.76 5 0 -17 -0.81 1.54 4 0 -17 12.05 1.84 4 0 -17 12.04 2.19 -4 0 17 16.87 2.66 3 0 -17 2.86 1.35 3 0 -17 1.26 1.60 -3 0 17 3.05 2.45 2 0 -17 44.92 4.40 2 0 -17 42.59 4.62 -2 0 17 38.91 5.11 1 0 -17 46.68 4.79 1 0 -17 48.88 4.46 -1 0 17 37.29 4.67 -1 0 17 52.08 5.13 0 0 -17 0.54 1.36 0 0 -17 2.01 1.77 0 0 -17 1.18 1.64 0 0 17 0.89 1.80 0 0 17 3.23 2.05 -1 0 -17 10.16 2.13 -1 0 -17 18.04 2.86 -1 0 -17 15.92 2.39 1 0 17 9.03 2.80 1 0 17 13.94 2.60 -2 0 -17 21.99 3.02 2 0 17 17.25 2.85 2 0 17 14.65 3.55 -3 0 -17 61.06 5.08 3 0 17 50.17 5.31 3 0 17 43.69 6.57 4 -1 -17 5.33 1.34 -4 1 17 3.46 2.60 3 -1 -17 62.91 5.76 3 -1 -17 65.40 5.97 -3 1 17 62.19 6.71 2 -1 -17 13.37 2.19 2 -1 -17 12.55 2.24 -2 1 17 15.62 2.88 1 -1 -17 2.21 1.80 1 -1 -17 3.10 1.44 1 -1 -17 2.62 1.68 -1 1 17 4.38 2.06 0 -1 -17 3.40 1.45 0 -1 -17 0.48 1.67 0 -1 -17 1.71 1.60 0 1 17 2.19 2.07 -1 -1 -17 2.40 1.64 -1 -1 -17 -0.14 1.29 -1 -1 -17 -0.64 1.40 1 1 17 -0.24 2.42 1 1 17 0.44 1.83 -2 -1 -17 87.56 7.67 -2 -1 -17 98.56 7.47 2 1 17 80.37 7.83 2 1 17 76.43 8.82 -3 -1 -17 63.41 5.76 3 1 17 61.15 7.22 3 1 17 60.46 6.01 4 -2 -17 -1.44 1.25 4 -2 -17 1.23 1.41 -4 2 17 0.99 2.51 3 -2 -17 2.90 1.48 -3 2 17 3.11 2.27 2 -2 -17 31.65 3.58 2 -2 -17 31.55 3.66 -2 2 17 33.04 4.25 1 -2 -17 44.80 4.45 1 -2 -17 42.68 4.53 -1 2 17 44.03 5.11 0 -2 -17 4.75 1.66 0 -2 -17 0.15 1.79 0 -2 -17 3.74 1.61 0 2 17 5.96 2.14 0 2 17 2.14 1.99 -1 -2 -17 -0.67 1.32 -1 -2 -17 3.48 1.50 -1 -2 -17 1.75 1.63 1 2 17 1.12 2.36 1 2 17 4.40 1.78 -2 -2 -17 12.91 2.07 -2 -2 -17 13.05 2.10 2 2 17 10.42 3.20 2 2 17 7.75 1.86 -3 -2 -17 8.02 1.83 3 2 17 8.64 2.98 3 2 17 12.57 2.13 4 -3 -17 7.44 1.60 4 -3 -17 10.77 1.82 -4 3 17 9.31 2.67 3 -3 -17 66.78 6.29 3 -3 -17 73.05 6.39 -3 3 17 74.28 7.02 2 -3 -17 3.04 1.56 2 -3 -17 4.11 1.54 -2 3 17 4.55 2.18 1 -3 -17 32.25 3.72 1 -3 -17 30.72 3.71 -1 3 17 30.73 4.33 0 -3 -17 -0.64 1.50 0 -3 -17 1.55 1.55 0 3 17 2.20 1.79 0 3 17 -0.86 1.82 -1 -3 -17 35.03 4.14 -1 -3 -17 28.53 4.05 -1 -3 -17 47.83 4.21 1 3 17 43.01 4.44 1 3 17 41.15 5.94 -2 -3 -17 56.74 5.17 -2 -3 -17 56.76 5.18 2 3 17 44.93 6.94 2 3 17 55.04 5.41 3 -4 -17 17.32 2.64 3 -4 -17 11.38 2.21 -3 4 17 13.92 2.64 2 -4 -17 64.47 6.19 2 -4 -17 76.51 6.40 -2 4 17 66.13 6.65 1 -4 -17 2.98 1.73 1 -4 -17 -0.25 1.33 -1 4 17 6.51 1.90 0 -4 -17 7.78 1.68 0 -4 -17 4.63 1.91 0 4 17 2.47 2.17 0 4 17 8.59 1.94 -1 -4 -17 4.42 1.74 -1 -4 -17 5.26 1.61 1 4 17 4.72 2.81 1 4 17 6.27 1.83 -2 -4 -17 17.11 2.37 -2 -4 -17 13.21 2.14 2 4 17 13.10 3.41 2 -5 -17 21.44 3.00 -2 5 17 22.73 3.28 1 -5 -17 7.31 1.78 1 -5 -17 11.28 2.17 -1 5 17 10.79 2.08 0 -5 -17 11.64 2.04 0 -5 -17 11.94 2.11 0 5 17 6.36 2.51 0 5 17 11.33 2.21 1 3 -18 75.72 6.52 1 3 -18 54.56 6.31 0 3 -18 67.94 6.58 0 -3 18 77.20 6.94 2 2 -18 3.46 1.55 2 2 -18 2.11 1.82 -2 -2 18 8.69 2.65 1 2 -18 5.83 1.67 1 2 -18 8.04 1.48 1 2 -18 7.90 2.37 -1 -2 18 9.90 2.70 0 2 -18 104.64 8.67 0 2 -18 107.16 8.95 0 2 -18 93.59 9.21 0 -2 18 110.03 9.20 -1 2 -18 4.57 1.58 -1 2 -18 3.02 2.55 -1 2 -18 1.37 1.75 1 -2 18 10.12 2.07 1 -2 18 2.17 2.10 3 1 -18 7.74 1.81 -3 -1 18 7.45 2.44 2 1 -18 91.48 7.82 2 1 -18 82.37 7.53 -2 -1 18 95.67 8.43 1 1 -18 35.37 3.79 1 1 -18 34.68 3.53 1 1 -18 34.98 4.56 -1 -1 18 40.28 4.79 0 1 -18 0.35 2.00 0 1 -18 -0.48 1.20 0 1 -18 0.12 1.40 0 -1 18 2.24 1.89 -1 1 -18 3.41 1.24 -1 1 -18 -0.34 1.53 -1 1 -18 3.87 1.54 1 -1 18 0.30 2.09 1 -1 18 7.57 1.93 3 0 -18 3.68 1.60 3 0 -18 5.18 1.69 -3 0 18 5.81 2.45 2 0 -18 11.87 2.06 2 0 -18 11.43 2.53 -2 0 18 16.98 2.99 1 0 -18 0.54 1.06 1 0 -18 1.04 1.36 1 0 -18 0.67 2.11 -1 0 18 3.98 2.18 0 0 -18 17.57 2.74 0 0 -18 16.43 2.34 -1 0 -18 1.96 1.45 -1 0 -18 5.28 1.60 1 0 18 8.51 2.03 2 -1 -18 2.64 1.57 2 -1 -18 2.10 1.36 2 -1 -18 1.93 2.16 -2 1 18 2.47 2.12 1 -1 -18 14.97 2.25 1 -1 -18 9.91 1.80 1 -1 -18 7.45 2.46 -1 1 18 15.49 2.48 0 -1 -18 0.82 1.90 0 -1 -18 -0.06 1.37 0 -1 -18 2.52 1.18 0 1 18 4.96 1.83 -1 -1 -18 0.69 1.18 -1 -1 -18 2.12 1.60 1 1 18 3.43 1.95 2 -2 -18 0.59 2.68 2 -2 -18 0.04 1.24 -2 2 18 -1.23 1.94 1 -2 -18 -0.56 1.18 1 -2 -18 0.39 1.63 1 -2 -18 3.39 2.20 -1 2 18 2.67 1.88 0 -2 -18 2.25 1.27 0 -2 -18 2.60 1.69 0 -2 -18 0.06 1.75 0 2 18 7.16 2.01 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 0.5383 _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 0.71075 7.991 10.185 12.879 91.091 93.917 90.297 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 17447 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1A C 0.7653(4) 0.5446(3) 1.2756(2) 0.0103(6) Uani 1 1 d . . . . . C2A C 0.6792(4) 0.5415(3) 1.1793(2) 0.0106(6) Uani 1 1 d . . . . . C3A C 0.6705(4) 0.6539(3) 1.1136(3) 0.0118(6) Uani 1 1 d . . . . . C4A C 0.7611(4) 0.7654(3) 1.1533(3) 0.0159(7) Uani 1 1 d . . . . . H4A H 0.762921 0.842147 1.112628 0.019 Uiso 1 1 calc R U . . . C5A C 0.8460(4) 0.7648(3) 1.2490(3) 0.0158(7) Uani 1 1 d . . . . . H5A H 0.905462 0.841341 1.273594 0.019 Uiso 1 1 calc R U . . . C6A C 0.9337(4) 0.6654(4) 1.4150(3) 0.0175(7) Uani 1 1 d . . . . . H6A H 1.013010 0.592687 1.423615 0.026 Uiso 1 1 calc R U . . . H6B H 0.850697 0.659934 1.467449 0.026 Uiso 1 1 calc R U . . . H6C H 0.994574 0.748908 1.423700 0.026 Uiso 1 1 calc R U . . . C7A C 0.7710(5) 0.4277(3) 1.3451(3) 0.0163(7) Uani 1 1 d . . . . . H7A H 0.697749 0.358410 1.313651 0.024 Uiso 1 1 calc R U . . . H7B H 0.732598 0.453297 1.413248 0.024 Uiso 1 1 calc R U . . . H7C H 0.886330 0.395327 1.353705 0.024 Uiso 1 1 calc R U . . . N1A N 0.8474(3) 0.6573(3) 1.3097(2) 0.0129(6) Uani 1 1 d . . . . . O1A O 0.5992(3) 0.4286(2) 1.14639(19) 0.0139(5) Uani 1 1 d . . . . . O2A O 0.5843(3) 0.6491(2) 1.02570(18) 0.0149(5) Uani 1 1 d . . . . . H1OA H 0.551(7) 0.439(5) 1.084(4) 0.044(15) Uiso 1 1 d . . . . . C1B C 0.2381(4) 0.5294(3) 0.2286(3) 0.0153(7) Uani 1 1 d . . . . . C2B C 0.3228(5) 0.5350(3) 0.3240(3) 0.0167(7) Uani 1 1 d . . . . . C3B C 0.4026(4) 0.6531(3) 0.3660(3) 0.0154(7) Uani 1 1 d . . . . . C4B C 0.3821(4) 0.7644(3) 0.3016(3) 0.0164(7) Uani 1 1 d . . . . . H4B H 0.428248 0.846557 0.325218 0.020 Uiso 1 1 calc R U . . . C5B C 0.2969(5) 0.7547(3) 0.2065(3) 0.0168(7) Uani 1 1 d . . . . . H5B H 0.286583 0.830421 0.164751 0.020 Uiso 1 1 calc R U . . . C6B C 0.1424(5) 0.6351(4) 0.0642(3) 0.0204(7) Uani 1 1 d . . . . . H6D H 0.144101 0.722251 0.033457 0.031 Uiso 1 1 calc R U . . . H6E H 0.026000 0.606206 0.068303 0.031 Uiso 1 1 calc R U . . . H6F H 0.201202 0.572865 0.020752 0.031 Uiso 1 1 calc R U . . . C7B C 0.1576(5) 0.4051(3) 0.1844(3) 0.0205(7) Uani 1 1 d . . . . . H7D H 0.038753 0.421044 0.164962 0.031 Uiso 1 1 calc R U . . . H7E H 0.167422 0.336550 0.236714 0.031 Uiso 1 1 calc R U . . . H7F H 0.214041 0.376744 0.122612 0.031 Uiso 1 1 calc R U . . . N1B N 0.2267(4) 0.6412(3) 0.1696(2) 0.0149(6) Uani 1 1 d . . . . . O1B O 0.3299(4) 0.4240(2) 0.3812(2) 0.0216(6) Uani 1 1 d . . . . . H1OB H 0.402(6) 0.433(4) 0.434(3) 0.015(10) Uiso 1 1 d . . . . . O2B O 0.4837(3) 0.6542(2) 0.45484(19) 0.0194(5) Uani 1 1 d . . . . . C8 C 0.0720(4) 0.8999(3) 0.6541(2) 0.0101(6) Uani 1 1 d . . . . . C9 C -0.1014(4) 0.9102(3) 0.6534(2) 0.0111(6) Uani 1 1 d . . . . . H9 H -0.168462 0.911490 0.589668 0.013 Uiso 1 1 calc R U . . . C10 C -0.1745(4) 0.9187(3) 0.7484(2) 0.0075(6) Uani 1 1 d . . . . . C11 C -0.0789(4) 0.9219(3) 0.8429(2) 0.0100(6) Uani 1 1 d . . . . . H11 H -0.130662 0.931263 0.906883 0.012 Uiso 1 1 calc R U . . . C12 C 0.0949(4) 0.9109(3) 0.8411(2) 0.0094(6) Uani 1 1 d . . . . . C13 C 0.1722(4) 0.8992(3) 0.7472(2) 0.0099(6) Uani 1 1 d . . . . . H13 H 0.290568 0.890981 0.746785 0.012 Uiso 1 1 calc R U . . . O3 O 0.1396(3) 0.8906(3) 0.56004(18) 0.0190(6) Uani 1 1 d . . . . . H3O H 0.249(7) 0.890(5) 0.569(4) 0.035(14) Uiso 1 1 d . . . . . O4 O -0.3468(3) 0.9221(2) 0.74928(17) 0.0112(5) Uani 1 1 d . . . . . H4O H -0.383223 0.933341 0.687952 0.017 Uiso 1 1 d R U . . . O5 O 0.1849(3) 0.9122(2) 0.93497(18) 0.0136(5) Uani 1 1 d . . . . . H5O H 0.283(8) 0.911(6) 0.930(5) 0.056(19) Uiso 1 1 d . . . . . O1W O 0.4799(3) 0.8860(2) 0.55806(18) 0.0127(5) Uani 1 1 d . . . . . H1W H 0.491418 0.813132 0.524821 0.019 Uiso 1 1 d R U . . . H2W H 0.535172 0.877486 0.625250 0.019 Uiso 0.5 1 d R U P . . H2WD H 0.492888 0.952574 0.520027 0.019 Uiso 0.5 1 d R U P . . O2W O 0.5173(3) 0.8819(2) 0.93695(17) 0.0136(5) Uani 1 1 d . . . . . H3W H 0.541136 0.810013 0.966539 0.020 Uiso 1 1 d R U . . . H4W H 0.558828 0.894838 0.873059 0.020 Uiso 1 1 d 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 C1A 0.0099(14) 0.0059(14) 0.0152(15) -0.0002(11) 0.0001(11) -0.0021(11) C2A 0.0071(14) 0.0098(14) 0.0148(15) -0.0014(11) 0.0004(11) -0.0014(11) C3A 0.0102(14) 0.0099(15) 0.0155(15) 0.0005(12) 0.0019(12) 0.0007(11) C4A 0.0151(16) 0.0096(15) 0.0230(17) 0.0046(13) -0.0011(13) -0.0018(12) C5A 0.0121(15) 0.0107(15) 0.0242(17) 0.0010(13) -0.0010(13) -0.0028(12) C6A 0.0140(16) 0.0190(17) 0.0181(17) -0.0029(13) -0.0080(13) -0.0020(13) C7A 0.0216(17) 0.0122(15) 0.0147(15) 0.0022(12) -0.0026(13) 0.0002(13) N1A 0.0107(13) 0.0114(13) 0.0159(13) -0.0016(10) -0.0030(10) -0.0008(10) O1A 0.0184(12) 0.0080(11) 0.0145(11) 0.0003(9) -0.0046(9) -0.0041(9) O2A 0.0169(12) 0.0123(11) 0.0148(11) 0.0025(9) -0.0040(9) -0.0003(9) C1B 0.0192(17) 0.0098(15) 0.0181(16) 0.0044(12) 0.0087(13) 0.0060(12) C2B 0.0231(18) 0.0132(16) 0.0149(15) 0.0059(12) 0.0075(13) 0.0084(13) C3B 0.0204(17) 0.0123(16) 0.0141(15) 0.0019(12) 0.0052(13) 0.0078(13) C4B 0.0223(17) 0.0102(15) 0.0173(16) 0.0036(12) 0.0036(13) 0.0030(13) C5B 0.0234(18) 0.0086(15) 0.0192(16) 0.0051(12) 0.0052(14) 0.0047(13) C6B 0.0283(19) 0.0182(17) 0.0155(16) 0.0062(13) 0.0046(14) 0.0072(14) C7B 0.0289(19) 0.0145(17) 0.0184(17) 0.0026(13) 0.0036(14) 0.0027(14) N1B 0.0192(14) 0.0140(14) 0.0119(13) 0.0045(11) 0.0026(11) 0.0058(11) O1B 0.0349(16) 0.0105(12) 0.0191(13) 0.0063(10) -0.0033(11) -0.0005(10) O2B 0.0287(14) 0.0146(12) 0.0147(12) 0.0026(9) -0.0014(10) 0.0082(10) C8 0.0135(15) 0.0088(14) 0.0081(14) -0.0019(11) 0.0011(11) -0.0015(11) C9 0.0097(14) 0.0122(15) 0.0110(14) 0.0018(11) -0.0016(11) 0.0006(11) C10 0.0062(13) 0.0024(12) 0.0137(14) 0.0002(10) 0.0005(11) -0.0023(10) C11 0.0117(15) 0.0078(14) 0.0108(14) 0.0000(11) 0.0023(11) -0.0016(11) C12 0.0116(14) 0.0057(13) 0.0108(14) 0.0019(11) -0.0007(11) -0.0013(11) C13 0.0074(14) 0.0103(14) 0.0119(14) -0.0008(11) -0.0009(11) 0.0010(11) O3 0.0092(12) 0.0377(15) 0.0102(11) -0.0033(10) 0.0017(9) -0.0008(10) O4 0.0064(10) 0.0152(11) 0.0118(10) 0.0013(8) -0.0013(8) 0.0001(8) O5 0.0102(12) 0.0183(12) 0.0118(11) 0.0009(9) -0.0025(9) -0.0017(9) O1W 0.0121(11) 0.0101(11) 0.0159(11) 0.0017(8) 0.0003(9) 0.0001(8) O2W 0.0177(12) 0.0099(11) 0.0125(11) 0.0029(8) -0.0038(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 0.0033 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 119.4(3) . . ? N1A C1A C7A 118.9(3) . . ? C2A C1A C7A 121.7(3) . . ? O1A C2A C1A 118.7(3) . . ? O1A C2A C3A 119.5(3) . . ? C1A C2A C3A 121.8(3) . . ? O2A C3A C4A 124.3(3) . . ? O2A C3A C2A 120.3(3) . . ? C4A C3A C2A 115.4(3) . . ? C5A C4A C3A 121.2(3) . . ? C5A C4A H4A 119.4 . . ? C3A C4A H4A 119.4 . . ? N1A C5A C4A 121.5(3) . . ? N1A C5A H5A 119.3 . . ? C4A C5A H5A 119.3 . . ? 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 120.6(3) . . ? C5A N1A C6A 118.8(3) . . ? C1A N1A C6A 120.5(3) . . ? C2A O1A H1OA 109(4) . . ? C2B C1B N1B 119.2(3) . . ? C2B C1B C7B 122.3(3) . . ? N1B C1B C7B 118.6(3) . . ? O1B C2B C1B 117.9(3) . . ? O1B C2B C3B 119.5(3) . . ? C1B C2B C3B 122.5(3) . . ? O2B C3B C4B 124.2(3) . . ? O2B C3B C2B 120.9(3) . . ? C4B C3B C2B 114.9(3) . . ? C5B C4B C3B 120.7(3) . . ? C5B C4B H4B 119.6 . . ? C3B C4B H4B 119.6 . . ? N1B C5B C4B 122.2(3) . . ? 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 120.4(3) . . ? C5B N1B C6B 119.8(3) . . ? C1B N1B C6B 119.8(3) . . ? C2B O1B H1OB 110(3) . . ? O3 C8 C9 117.0(3) . . ? O3 C8 C13 121.6(3) . . ? C9 C8 C13 121.4(3) . . ? C8 C9 C10 118.4(3) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? O4 C10 C11 118.8(3) . . ? O4 C10 C9 119.1(3) . . ? C11 C10 C9 122.0(3) . . ? C10 C11 C12 118.2(3) . . ? C10 C11 H11 120.9 . . ? C12 C11 H11 120.9 . . ? O5 C12 C11 116.9(3) . . ? O5 C12 C13 121.9(3) . . ? C11 C12 C13 121.3(3) . . ? C8 C13 C12 118.6(3) . . ? C8 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C8 O3 H3O 110(3) . . ? C10 O4 H4O 106.4 . . ? C12 O5 H5O 113(4) . . ? H1W O1W H2W 107.5 . . ? H1W O1W H2WD 112.5 . . ? H2W O1W H2WD 122.9 . . ? H3W O2W H4W 117.2 . . ? 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 1.371(4) . ? C1A C2A 1.377(4) . ? C1A C7A 1.503(4) . ? C2A O1A 1.361(4) . ? C2A C3A 1.437(4) . ? C3A O2A 1.285(4) . ? C3A C4A 1.414(5) . ? C4A C5A 1.366(5) . ? C4A H4A 0.9500 . ? C5A N1A 1.359(4) . ? C5A H5A 0.9500 . ? C6A N1A 1.480(4) . ? 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 H1OA 0.87(6) . ? C1B C2B 1.362(5) . ? C1B N1B 1.381(4) . ? C1B C7B 1.504(5) . ? C2B O1B 1.362(4) . ? C2B C3B 1.439(5) . ? C3B O2B 1.276(4) . ? C3B C4B 1.422(4) . ? C4B C5B 1.362(5) . ? C4B H4B 0.9500 . ? C5B N1B 1.349(5) . ? C5B H5B 0.9500 . ? C6B N1B 1.474(4) . ? 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 H1OB 0.86(4) . ? C8 O3 1.362(4) . ? C8 C9 1.389(4) . ? C8 C13 1.396(4) . ? C9 C10 1.392(4) . ? C9 H9 0.9500 . ? C10 O4 1.379(4) . ? C10 C11 1.391(4) . ? C11 C12 1.395(4) . ? C11 H11 0.9500 . ? C12 O5 1.364(4) . ? C12 C13 1.397(4) . ? C13 H13 0.9500 . ? O3 H3O 0.87(6) . ? O4 H4O 0.8330 . ? O5 H5O 0.79(7) . ? O1W H1W 0.8584 . ? O1W H2W 0.9500 . ? O1W H2WD 0.8550 . ? O2W H3W 0.8487 . ? O2W H4W 0.9192 . ? 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 H1OA O2A 0.87(6) 2.30(6) 2.756(3) 113(4) . yes O1A H1OA O2A 0.87(6) 1.93(6) 2.678(3) 143(5) 2_667 yes O1B H1OB O2B 0.86(4) 1.89(4) 2.638(4) 145(4) 2_666 yes O3 H3O O1W 0.87(6) 1.86(6) 2.721(3) 168(5) . yes O4 H4O O1W 0.83 1.99 2.760(3) 154.1 1_455 yes O5 H5O O2W 0.79(7) 1.90(7) 2.673(3) 168(6) . yes O1W H1W O2B 0.86 1.84 2.690(3) 171.8 . yes O1W H2W O4 0.95 1.85 2.760(3) 160.1 1_655 yes O1W H2WD O1W 0.85 1.96 2.818(5) 175.7 2_676 yes O2W H3W O2A 0.85 1.85 2.693(3) 176.8 . yes O2W H4W O4 0.92 1.83 2.752(3) 176.8 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 179.7(3) . . . . ? C7A C1A C2A O1A -0.8(5) . . . . ? N1A C1A C2A C3A -0.9(5) . . . . ? C7A C1A C2A C3A 178.6(3) . . . . ? O1A C2A C3A O2A 1.8(5) . . . . ? C1A C2A C3A O2A -177.6(3) . . . . ? O1A C2A C3A C4A -178.4(3) . . . . ? C1A C2A C3A C4A 2.1(5) . . . . ? O2A C3A C4A C5A 178.0(3) . . . . ? C2A C3A C4A C5A -1.8(5) . . . . ? C3A C4A C5A N1A 0.2(5) . . . . ? C4A C5A N1A C1A 1.2(5) . . . . ? C4A C5A N1A C6A -176.6(3) . . . . ? C2A C1A N1A C5A -0.8(5) . . . . ? C7A C1A N1A C5A 179.6(3) . . . . ? C2A C1A N1A C6A 176.9(3) . . . . ? C7A C1A N1A C6A -2.6(4) . . . . ? N1B C1B C2B O1B 179.1(3) . . . . ? C7B C1B C2B O1B -1.6(5) . . . . ? N1B C1B C2B C3B -0.5(5) . . . . ? C7B C1B C2B C3B 178.9(3) . . . . ? O1B C2B C3B O2B 1.9(5) . . . . ? C1B C2B C3B O2B -178.6(3) . . . . ? O1B C2B C3B C4B -177.7(3) . . . . ? C1B C2B C3B C4B 1.8(5) . . . . ? O2B C3B C4B C5B 178.4(3) . . . . ? C2B C3B C4B C5B -2.0(5) . . . . ? C3B C4B C5B N1B 0.9(5) . . . . ? C4B C5B N1B C1B 0.6(5) . . . . ? C4B C5B N1B C6B -177.3(3) . . . . ? C2B C1B N1B C5B -0.8(5) . . . . ? C7B C1B N1B C5B 179.9(3) . . . . ? C2B C1B N1B C6B 177.1(3) . . . . ? C7B C1B N1B C6B -2.3(5) . . . . ? O3 C8 C9 C10 179.4(3) . . . . ? C13 C8 C9 C10 -0.6(5) . . . . ? C8 C9 C10 O4 -176.7(3) . . . . ? C8 C9 C10 C11 2.4(5) . . . . ? O4 C10 C11 C12 176.4(3) . . . . ? C9 C10 C11 C12 -2.6(4) . . . . ? C10 C11 C12 O5 -179.0(3) . . . . ? C10 C11 C12 C13 1.1(4) . . . . ? O3 C8 C13 C12 179.2(3) . . . . ? C9 C8 C13 C12 -0.8(5) . . . . ? O5 C12 C13 C8 -179.3(3) . . . . ? C11 C12 C13 C8 0.6(4) . . . . ? _cod_database_fobs_code 2022897