#------------------------------------------------------------------------------ #$Date: 2023-10-10 04:19:25 +0200 (Tue, 10 Oct 2023) $ #$Revision: 286864 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022893.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_2022893 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 'C7 H9 N O2, 0.5(C6 H6 O2)' _chemical_formula_sum 'C10 H12 N O3' _chemical_formula_weight 194.21 _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-2014/7 _cell_angle_alpha 72.4243(4) _cell_angle_beta 85.7351(4) _cell_angle_gamma 73.9285(4) _cell_formula_units_Z 2 _cell_length_a 6.83171(9) _cell_length_b 7.09634(10) _cell_length_c 10.01294(14) _cell_measurement_reflns_used 8964 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.54 _cell_measurement_theta_min 3.10 _cell_volume 444.659(11) _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 'SHELXL2014 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _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 0.0240 _diffrn_reflns_av_unetI/netI 0.0239 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 11173 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.537 _diffrn_reflns_theta_min 2.134 _exptl_absorpt_coefficient_mu 0.108 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.7189 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker,2016' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.450 _exptl_crystal_description block _exptl_crystal_F_000 206 _exptl_crystal_size_max 0.410 _exptl_crystal_size_mid 0.380 _exptl_crystal_size_min 0.220 _refine_diff_density_max 0.452 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.055 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 137 _refine_ls_number_reflns 2708 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0364 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+0.1917P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1001 _refine_ls_wR_factor_ref 0.1023 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2471 _reflns_number_total 2708 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lo5093sup1.cif _cod_data_source_block KA254_0M_def-hq_1_0.5 _cod_original_cell_volume 444.660(11) _cod_database_code 2022893 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.957 _shelx_estimated_absorpt_t_max 0.977 _shelx_res_file ; ka254_0m.res created by SHELXL-2014/7 TITL KA254_0m_a.res in P-1 CELL 0.71073 6.83171 7.09634 10.01294 72.4243 85.7351 73.9285 ZERR 2.000 0.00009 0.00010 0.00014 0.0004 0.0004 0.0004 LATT 1 SFAC C H N O UNIT 20 24 2 6 L.S. 10 ACTA BOND $H FMAP 2 PLAN 5 EQIV $1 -x+1, -y+2, -z+1 EQIV $2 x+1, y, z HTAB O1 O2_$1 HTAB O3 O2 HTAB C4 O3 HTAB C7 O2_$2 HTAB C9 O1_$1 SIZE 0.41 0.38 0.22 CONF TEMP -172.290 WGHT 0.051200 0.191700 FVAR 1.36271 MOLE 1 C1 1 1.067640 0.643783 0.600132 11.00000 0.00847 0.01015 = 0.00846 -0.00227 0.00005 -0.00192 C2 1 0.866152 0.754799 0.579495 11.00000 0.00905 0.00991 = 0.00709 -0.00170 -0.00011 -0.00167 C3 1 0.718075 0.732750 0.688327 11.00000 0.00799 0.01048 = 0.00863 -0.00299 0.00020 -0.00176 C4 1 0.790959 0.582474 0.816650 11.00000 0.00947 0.01242 = 0.00856 -0.00160 0.00109 -0.00209 AFIX 43 H4 2 0.699710 0.557209 0.892174 11.00000 -1.20000 AFIX 0 C5 1 0.991765 0.473346 0.832758 11.00000 0.01092 0.01022 = 0.00848 -0.00086 0.00000 -0.00173 AFIX 43 H5 2 1.036618 0.372747 0.919544 11.00000 -1.20000 AFIX 0 C6 1 1.342545 0.384209 0.755397 11.00000 0.00750 0.01545 = 0.01467 -0.00151 -0.00158 0.00102 AFIX 137 H6A 2 1.378975 0.292136 0.696310 11.00000 -1.50000 H6B 2 1.360615 0.303108 0.854214 11.00000 -1.50000 H6C 2 1.430574 0.477436 0.733320 11.00000 -1.50000 AFIX 0 C7 1 1.222357 0.669291 0.486945 11.00000 0.00944 0.01644 = 0.01157 -0.00258 0.00283 -0.00241 AFIX 137 H7A 2 1.154439 0.762161 0.399394 11.00000 -1.50000 H7B 2 1.291049 0.535468 0.473611 11.00000 -1.50000 H7C 2 1.322928 0.726953 0.513687 11.00000 -1.50000 AFIX 0 N1 3 1.128138 0.504474 0.728840 11.00000 0.00733 0.01010 = 0.00944 -0.00181 -0.00070 -0.00058 O1 4 0.807211 0.885975 0.450669 11.00000 0.00972 0.01680 = 0.00766 0.00131 -0.00024 0.00139 H1O 2 0.677274 0.948919 0.452041 11.00000 0.05203 O2 4 0.532335 0.841611 0.665729 11.00000 0.00742 0.01670 = 0.01042 -0.00107 -0.00038 0.00120 MOLE 2 C8 1 0.200474 0.926364 0.958920 11.00000 0.00773 0.01015 = 0.00907 -0.00139 0.00203 -0.00081 C9 1 0.036779 0.953511 0.873176 11.00000 0.01075 0.01089 = 0.00757 -0.00210 0.00113 -0.00207 AFIX 43 H9 2 0.061152 0.922296 0.786592 11.00000 -1.20000 AFIX 0 C10 1 -0.162448 1.026336 0.914295 11.00000 0.00920 0.01171 = 0.00854 -0.00181 -0.00020 -0.00176 AFIX 43 H10 2 -0.273184 1.043919 0.855630 11.00000 -1.20000 AFIX 0 O3 4 0.399035 0.851266 0.925927 11.00000 0.00749 0.02318 = 0.01158 -0.00571 0.00229 0.00122 H2O 2 0.412127 0.850723 0.839720 11.00000 0.04147 HKLF 4 REM KA254_0m_a.res in P-1 REM R1 = 0.0364 for 2471 Fo > 4sig(Fo) and 0.0395 for all 2708 data REM 137 parameters refined using 0 restraints END WGHT 0.0512 0.1918 REM Highest difference peak 0.452, deepest hole -0.264, 1-sigma level 0.055 Q1 1 0.7931 0.7410 0.6334 11.00000 0.05 0.45 Q2 1 0.9686 0.7022 0.5870 11.00000 0.05 0.43 Q3 1 -0.1792 1.0464 0.9773 11.00000 0.05 0.43 Q4 1 0.1195 0.9370 0.9161 11.00000 0.05 0.43 Q5 1 -0.0609 0.9820 0.8971 11.00000 0.05 0.41 ; _shelx_res_checksum 21480 _shelx_hkl_file ; -1 0 0 1320.84 42.1730 1 -2 0 0 276.560 8.17758 5 -2 0 0 285.057 8.27466 5 -2 0 0 282.659 8.29259 4 -2 0 0 277.455 8.17491 3 2 0 0 270.083 8.22237 5 2 0 0 285.496 8.28187 5 2 0 0 281.861 8.30207 4 2 0 0 278.571 8.18406 3 -3 0 0 555.130 16.7671 4 -3 0 0 574.728 16.5933 5 -3 0 0 568.252 16.7275 5 3 0 0 566.088 16.6898 5 3 0 0 558.475 16.7452 5 3 0 0 564.826 16.6044 3 3 0 0 601.280 16.8060 4 -4 0 0 1.85526 0.24115 5 -4 0 0 1.99664 0.34745 5 -4 0 0 1.19646 0.34274 4 4 0 0 1.95165 0.28392 3 4 0 0 2.13589 0.45613 2 4 0 0 2.85132 0.37958 5 4 0 0 1.46795 0.32554 4 4 0 0 1.44754 0.53831 5 -5 0 0 335.821 10.4588 4 -5 0 0 340.397 10.0741 5 -5 0 0 338.398 10.2758 5 5 0 0 350.998 10.5153 4 5 0 0 333.700 10.3536 5 5 0 0 347.735 10.3997 5 5 0 0 343.962 10.7737 2 5 0 0 336.639 10.1092 3 -6 0 0 81.9245 2.64965 5 -6 0 0 80.8929 2.85706 5 -6 0 0 78.5252 3.13687 4 6 0 0 81.2401 3.43707 2 6 0 0 83.3763 3.19213 4 6 0 0 85.2622 3.07289 5 6 0 0 80.0682 3.03512 5 6 0 0 83.4325 2.69971 3 -7 0 0 9.71940 0.93122 5 -7 0 0 9.34869 0.73267 5 7 0 0 9.21896 1.47822 4 7 0 0 11.2286 1.41089 2 7 0 0 8.95199 0.76378 3 7 0 0 8.61133 1.12863 5 8 0 0 7.37207 1.37432 2 8 0 0 7.46630 1.08439 5 8 0 0 4.25400 1.07630 4 9 0 0 2.54616 1.38839 5 9 0 0 2.63787 1.52207 2 9 0 0 3.11900 1.24739 4 9 -1 0 29.8400 3.48426 2 9 -1 0 36.8765 2.94272 5 9 -1 0 28.8483 2.91920 4 8 -1 0 172.931 6.24939 5 8 -1 0 164.411 6.35203 4 8 -1 0 170.220 6.68259 2 -8 1 0 174.276 5.74538 5 7 -1 0 64.2713 2.98480 4 7 -1 0 67.6566 3.26584 2 -7 1 0 64.3597 2.73147 5 -7 1 0 62.6358 2.36566 5 6 -1 0 153.396 4.62582 3 6 -1 0 153.030 5.52671 2 6 -1 0 148.886 5.06533 5 6 -1 0 142.565 5.09421 5 6 -1 0 151.235 5.27895 4 -6 1 0 150.218 4.73739 5 -6 1 0 150.916 5.06955 5 5 -1 0 38.9588 1.84217 4 5 -1 0 39.5452 1.41273 3 5 -1 0 37.6116 1.97814 2 5 -1 0 37.5519 1.69440 5 5 -1 0 40.7339 1.74287 5 -5 1 0 37.9891 1.74643 5 -5 1 0 39.0919 1.78846 4 -5 1 0 38.2593 1.47870 5 -5 1 0 37.8845 1.41454 3 4 -1 0 3.98442 0.56773 4 4 -1 0 1.83585 0.35163 5 4 -1 0 3.88885 0.54708 5 4 -1 0 3.34471 0.37468 3 -4 1 0 2.49340 0.33232 3 -4 1 0 2.36865 0.45368 5 -4 1 0 2.65117 0.45985 4 3 -1 0 935.797 26.9523 4 3 -1 0 947.177 26.8776 5 3 -1 0 909.394 26.8496 5 3 -1 0 936.076 26.6834 3 -3 1 0 922.620 26.9274 5 -3 1 0 882.752 26.9127 4 -3 1 0 899.280 26.7367 5 2 -1 0 -0.0616 0.12653 4 2 -1 0 0.01040 0.11703 3 2 -1 0 -0.1293 0.13367 5 2 -1 0 0.19282 0.11916 5 -2 1 0 0.40666 0.18046 4 -2 1 0 0.41692 0.13109 5 -2 1 0 0.10457 0.13254 3 -2 1 0 0.11544 0.14918 5 1 -1 0 4.80833 0.33521 4 1 -1 0 4.87900 0.30579 5 1 -1 0 5.21962 0.26970 3 -1 1 0 4.88757 0.32550 5 -1 1 0 5.03550 0.28651 5 -1 1 0 4.93589 0.27748 3 -1 1 0 5.13950 0.31661 4 0 -1 0 38.2617 1.15499 5 0 -1 0 38.3552 1.11418 2 0 -1 0 37.3281 1.14748 4 0 -1 0 35.7994 1.13226 5 0 1 0 35.5211 1.14518 5 0 1 0 36.7962 1.14167 4 0 1 0 36.4198 1.13892 5 -1 -1 0 1359.61 40.8792 1 1 1 0 1316.34 41.1380 1 -2 -1 0 15.2560 0.61416 4 2 1 0 15.8560 0.57780 5 2 1 0 15.3233 0.55180 5 2 1 0 15.5380 0.74155 2 2 1 0 15.6173 0.61202 4 -3 -1 0 163.200 4.94996 4 3 1 0 161.401 5.14587 2 3 1 0 158.898 4.84736 5 3 1 0 159.357 4.85673 3 3 1 0 161.794 4.94239 4 3 1 0 163.741 4.91222 5 -4 -1 0 27.6751 1.35848 4 4 1 0 29.3253 1.24107 4 4 1 0 29.4476 1.15638 5 4 1 0 30.2725 1.13948 3 4 1 0 29.5015 1.45897 2 4 1 0 31.2675 1.23904 5 -5 -1 0 384.955 11.3578 4 5 1 0 362.888 11.3287 4 5 1 0 371.907 11.2730 5 5 1 0 375.048 11.2238 5 5 1 0 376.406 11.6774 2 5 1 0 370.978 11.1033 3 -6 -1 0 378.513 11.9620 4 6 1 0 387.934 11.6310 3 6 1 0 408.761 12.0258 4 6 1 0 382.905 11.8495 5 6 1 0 393.173 12.3766 2 6 1 0 390.028 11.8890 5 7 1 0 73.5106 3.01712 5 7 1 0 80.2904 2.70741 3 7 1 0 75.3846 3.12160 4 7 1 0 79.5325 3.02646 5 7 1 0 76.8263 3.49422 2 8 1 0 37.9192 2.68584 2 8 1 0 41.9097 2.35119 4 8 1 0 42.2404 2.28227 5 9 1 0 373.437 12.1243 5 9 1 0 383.811 12.2943 4 9 1 0 369.470 12.7466 2 8 -2 0 58.8942 3.31767 5 8 -2 0 69.1866 3.56643 4 8 -2 0 62.5328 3.71976 2 -8 2 0 69.1382 3.72170 5 7 -2 0 20.0084 1.87655 4 7 -2 0 20.0626 1.78176 5 7 -2 0 19.6192 2.05251 2 -7 2 0 17.7741 1.76505 5 -7 2 0 22.0920 1.47107 5 6 -2 0 7.14453 1.10133 4 6 -2 0 6.72620 0.92591 5 6 -2 0 6.16308 1.02037 2 -6 2 0 6.16527 0.69540 3 -6 2 0 5.99033 0.72056 5 -6 2 0 8.04767 1.01518 5 5 -2 0 474.530 14.3474 4 5 -2 0 475.693 13.7292 3 5 -2 0 483.228 14.2262 5 5 -2 0 476.018 14.1044 5 -5 2 0 460.636 14.2443 5 -5 2 0 449.899 13.8748 5 -5 2 0 463.228 13.8037 3 -5 2 0 445.301 14.2076 4 4 -2 0 20.1565 1.23107 4 4 -2 0 22.0367 1.12892 5 4 -2 0 20.2470 1.13709 5 4 -2 0 22.3008 0.90681 3 -4 2 0 21.4317 1.00738 5 -4 2 0 20.6061 1.24268 5 -4 2 0 20.6926 0.95932 3 -4 2 0 20.6707 1.19333 4 3 -2 0 40.7673 1.38488 3 3 -2 0 39.1048 1.64341 4 3 -2 0 38.1912 1.53537 5 3 -2 0 39.0102 1.56816 5 -3 2 0 38.2983 1.63264 5 -3 2 0 39.2459 1.58842 4 -3 2 0 38.4567 1.46102 5 -3 2 0 39.1036 1.43807 3 2 -2 0 694.727 19.6255 3 2 -2 0 666.855 19.7663 5 2 -2 0 654.355 19.8090 4 2 -2 0 659.501 19.7191 5 -2 2 0 689.642 19.6853 5 -2 2 0 684.588 19.7863 4 -2 2 0 683.012 19.6703 3 -2 2 0 652.980 19.8074 5 1 -2 0 598.201 17.0858 4 1 -2 0 581.221 17.0579 5 1 -2 0 576.999 17.0112 5 -1 2 0 572.852 17.0443 4 -1 2 0 584.358 17.0133 3 0 -2 0 406.255 11.4511 4 0 -2 0 397.733 11.4117 5 0 -2 0 380.964 11.3694 2 0 -2 0 368.680 11.5291 5 0 2 0 393.911 11.4200 4 0 2 0 381.402 11.4439 5 0 2 0 409.044 11.4415 5 -1 -2 0 2970.69 90.2956 1 1 2 0 2992.95 90.6164 1 -2 -2 0 392.801 11.5200 2 2 2 0 388.523 11.5035 2 2 2 0 379.496 11.3173 5 2 2 0 392.816 11.2758 5 -3 -2 0 7.17775 0.61775 2 -3 -2 0 6.46264 0.43043 4 3 2 0 5.67558 0.53549 2 3 2 0 6.84814 0.39489 5 3 2 0 7.02696 0.40330 4 3 2 0 6.55558 0.37273 5 -4 -2 0 49.1158 1.74688 4 4 2 0 47.4768 1.98130 2 4 2 0 48.5389 1.72139 4 4 2 0 46.4991 1.66159 5 4 2 0 48.2531 1.69913 5 -5 -2 0 1.36803 0.39945 4 5 2 0 0.63581 0.45625 2 5 2 0 1.15988 0.31100 5 5 2 0 1.86970 0.41669 5 5 2 0 1.45829 0.38313 3 5 2 0 1.06041 0.33788 4 -6 -2 0 442.419 13.6427 4 6 2 0 455.694 13.4432 3 6 2 0 453.019 13.6424 4 6 2 0 449.466 13.5323 5 6 2 0 454.492 13.5865 5 6 2 0 448.869 14.0709 2 -7 -2 0 25.4229 1.62728 4 7 2 0 24.3401 1.56767 5 7 2 0 27.1245 1.55079 4 7 2 0 24.7758 1.47241 5 7 2 0 24.6517 1.40057 3 8 2 0 37.0087 2.59251 2 8 2 0 41.5303 2.21701 4 8 2 0 40.8396 2.16418 5 9 2 0 7.72817 1.35912 4 9 2 0 5.60767 1.28594 5 9 2 0 8.39301 1.70481 2 8 -3 0 458.597 15.6683 2 8 -3 0 484.182 15.6397 4 8 -3 0 479.799 15.4165 5 -8 3 0 484.942 15.2172 5 7 -3 0 52.9397 3.18738 2 7 -3 0 51.1005 2.97966 4 7 -3 0 49.5219 2.86755 5 -7 3 0 51.0656 2.92517 5 6 -3 0 12.8039 1.53430 4 6 -3 0 14.9819 1.63345 2 6 -3 0 14.3627 1.47384 5 -6 3 0 15.1022 1.08594 3 -6 3 0 14.9036 1.83655 5 5 -3 0 39.8307 2.08577 4 5 -3 0 41.3545 2.02459 5 -5 3 0 40.0255 1.65001 3 -5 3 0 36.8254 1.69993 5 -5 3 0 38.9278 2.09764 5 4 -3 0 9.24543 0.88751 5 4 -3 0 10.3821 0.92825 5 4 -3 0 12.2981 1.07084 4 -4 3 0 10.9236 0.79706 3 -4 3 0 10.6735 1.01460 4 -4 3 0 11.1306 0.82243 5 -4 3 0 12.4446 1.10115 5 3 -3 0 -0.1140 0.33472 4 3 -3 0 0.08971 0.32161 5 3 -3 0 0.46268 0.30678 5 -3 3 0 -0.5253 0.29864 4 -3 3 0 0.13735 0.26158 3 -3 3 0 0.64416 0.35552 5 -3 3 0 0.20480 0.26965 5 2 -3 0 729.742 21.5245 4 2 -3 0 726.333 21.3672 5 2 -3 0 711.177 21.4776 5 -2 3 0 710.715 21.5171 5 -2 3 0 742.986 21.4653 4 -2 3 0 715.504 21.3691 3 -2 3 0 763.839 21.3898 5 1 -3 0 169.638 5.44296 5 1 -3 0 174.405 5.37151 5 1 -3 0 173.073 5.45826 4 -1 3 0 178.055 5.46285 5 -1 3 0 184.955 5.42499 4 -1 3 0 177.288 5.41066 3 0 -3 0 159.324 4.87077 5 0 -3 0 160.675 4.79835 5 0 -3 0 162.666 4.74863 2 0 -3 0 154.940 4.86453 4 0 3 0 150.084 4.82443 5 0 3 0 156.029 4.79905 4 0 3 0 166.318 4.90100 3 0 3 0 162.142 4.83572 5 -1 -3 0 755.532 21.6015 2 -1 -3 0 743.659 21.5603 5 -1 -3 0 755.881 21.5784 5 1 3 0 719.566 21.5485 5 1 3 0 745.023 21.5622 5 1 3 0 730.693 21.5262 2 -2 -3 0 139.266 4.32037 2 2 3 0 135.248 4.16557 5 2 3 0 138.147 4.26120 2 2 3 0 138.472 4.11977 5 -3 -3 0 726.949 21.0939 2 3 3 0 706.867 20.7410 5 3 3 0 716.699 21.0557 2 3 3 0 713.291 20.8034 5 3 3 0 708.620 20.7347 4 4 3 0 226.092 6.73725 5 4 3 0 218.414 7.10303 2 4 3 0 230.055 6.75847 4 5 3 0 1.08443 0.37055 5 5 3 0 0.48926 0.30040 5 5 3 0 0.24866 0.40041 2 5 3 0 0.85853 0.28655 4 -6 -3 0 76.4499 2.81655 4 6 3 0 77.3865 2.76883 3 6 3 0 77.1365 2.78054 5 6 3 0 72.9754 2.73262 4 6 3 0 77.3107 2.70184 5 6 3 0 75.5294 3.18014 2 -7 -3 0 220.716 7.41938 4 7 3 0 236.773 7.29809 3 7 3 0 236.274 7.38566 5 7 3 0 236.306 7.41195 4 7 3 0 224.660 8.09248 2 7 3 0 230.252 7.31882 5 8 3 0 27.3308 1.98405 5 8 3 0 25.5921 2.22249 2 8 3 0 26.3348 1.74395 4 8 3 0 26.0047 1.82238 3 8 3 0 24.5730 1.69542 5 9 3 0 1.20241 1.29285 2 9 3 0 -0.3349 1.01706 5 9 3 0 -0.6739 0.94749 4 7 -4 0 132.922 5.45478 5 7 -4 0 137.684 5.78592 2 7 -4 0 138.690 5.60325 4 -7 4 0 129.893 5.56581 5 6 -4 0 4.31322 1.07599 5 6 -4 0 4.23109 1.26635 2 6 -4 0 5.92684 1.22846 4 -6 4 0 3.54581 0.84097 3 -6 4 0 5.67251 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15.7462 1.74281 5 2 -2 -11 16.7241 1.20980 2 2 -2 -11 18.5540 1.51414 5 -2 2 11 17.7904 1.63708 5 -2 2 11 19.7933 1.66518 3 1 -2 -11 13.3727 1.19962 5 -1 2 11 15.3018 1.48549 5 -1 2 11 14.3892 1.44511 3 0 -2 -11 532.590 15.5288 5 0 2 11 477.575 16.3972 3 0 2 11 529.739 15.9325 5 -1 -2 -11 1.42858 0.44337 5 -1 -2 -11 1.77667 0.98922 5 1 2 11 0.54093 0.66429 5 -2 -2 -11 -0.6020 0.92910 5 -2 -2 -11 -0.1187 0.33926 5 -2 -2 -11 -0.2550 0.93452 3 -3 -2 -11 1.77036 0.88179 3 -3 -2 -11 1.25773 0.44733 5 3 2 11 0.64776 0.58384 5 4 2 11 37.3347 1.94419 5 4 2 11 33.9204 2.28295 4 5 2 11 -0.1106 0.74746 5 5 2 11 -1.6071 0.79648 4 6 2 11 40.4074 2.25199 5 6 2 11 42.1281 2.72089 4 5 -3 -11 0.45997 1.05077 2 5 -3 -11 2.41953 1.36815 5 -5 3 11 0.57650 1.39837 5 -5 3 11 1.20500 1.38639 3 4 -3 -11 12.9626 1.78811 5 4 -3 -11 9.42826 1.24344 2 -4 3 11 10.6340 1.46628 3 -4 3 11 12.8893 1.72868 5 3 -3 -11 189.839 6.26344 2 3 -3 -11 184.915 6.65014 5 -3 3 11 190.254 6.91598 5 -3 3 11 189.420 6.70729 3 2 -3 -11 40.3151 2.14099 5 -2 3 11 40.4778 2.33429 3 -2 3 11 37.4928 2.43548 5 1 -3 -11 5.55238 0.84549 5 1 -3 -11 5.87460 0.80604 2 -1 3 11 5.40664 0.98271 5 -1 3 11 6.53467 1.05654 3 0 -3 -11 456.527 13.5404 5 0 -3 -11 439.956 13.8784 5 0 3 11 429.922 13.9516 5 0 3 11 454.868 13.8520 3 -1 -3 -11 806.564 22.8423 5 -1 -3 -11 753.592 23.1634 5 1 3 11 769.573 23.2048 3 1 3 11 765.050 23.3939 5 -2 -3 -11 41.3376 2.09902 5 -2 -3 -11 43.2649 1.63409 5 2 3 11 40.1892 2.04957 3 -3 -3 -11 47.0455 1.68072 5 -3 -3 -11 46.5984 2.25002 3 3 3 11 46.2647 2.12167 3 4 3 11 27.1133 2.12124 5 5 3 11 122.213 4.22666 5 5 3 11 108.736 4.67203 4 6 3 11 9.49738 1.49779 4 6 3 11 9.81097 1.12981 5 4 -4 -11 3.22406 1.19811 5 4 -4 -11 3.41567 1.04105 2 -4 4 11 2.89663 1.28169 5 -4 4 11 0.52683 1.15638 3 3 -4 -11 4.19542 1.08294 5 3 -4 -11 3.86615 0.80346 2 -3 4 11 7.09632 1.36160 5 -3 4 11 5.64454 1.22712 3 2 -4 -11 17.2363 1.23013 2 2 -4 -11 19.5213 1.66302 5 -2 4 11 14.1615 1.90834 5 -2 4 11 19.0933 1.88467 3 1 -4 -11 6.98822 0.92740 5 1 -4 -11 6.19341 0.79176 2 -1 4 11 6.57849 1.18892 5 -1 4 11 5.37889 1.04654 3 -1 4 11 6.99733 1.33233 2 0 -4 -11 24.7915 1.41625 5 0 -4 -11 23.7809 1.89338 5 0 4 11 24.8800 1.81188 3 0 4 11 24.0837 1.90052 5 0 4 11 21.1466 1.94118 2 -1 -4 -11 86.0019 2.93212 5 -1 -4 -11 84.4647 3.28637 5 1 4 11 80.6709 3.42577 2 1 4 11 87.4192 3.44606 3 1 4 11 81.8142 3.52888 5 -2 -4 -11 -0.0377 0.29722 5 2 4 11 0.42178 0.71033 5 2 4 11 1.39808 0.72390 3 2 4 11 -0.6219 0.84004 2 3 4 11 1.15411 0.74340 3 3 4 11 0.40971 0.71805 5 4 4 11 20.4620 1.51790 3 5 4 11 159.375 5.58546 5 5 4 11 162.935 5.22361 3 5 4 11 155.283 5.98701 4 6 4 11 7.14286 1.35997 4 6 4 11 7.39625 1.03175 5 4 -5 -11 4.19816 1.09598 2 4 -5 -11 4.31276 1.33641 5 -4 5 11 5.37055 1.77401 5 -4 5 11 3.67249 1.62540 3 3 -5 -11 1.49266 1.04709 5 -3 5 11 1.30134 1.31431 5 -3 5 11 -0.9101 1.12479 3 2 -5 -11 324.174 10.1518 2 2 -5 -11 352.325 10.7834 5 -2 5 11 337.444 10.9836 3 -2 5 11 318.499 11.1377 5 1 -5 -11 14.5790 1.39487 5 -1 5 11 14.5942 1.78210 3 -1 5 11 15.0535 1.98955 5 0 -5 -11 103.063 3.60970 5 0 -5 -11 99.7365 3.81986 5 0 5 11 102.684 4.24673 5 0 5 11 97.3888 4.08061 3 0 5 11 101.073 3.91828 2 -1 -5 -11 58.1261 2.17832 5 1 5 11 60.6086 2.73535 2 1 5 11 59.8668 2.88814 3 1 5 11 59.5119 2.89770 5 2 5 11 0.92793 0.88678 2 2 5 11 0.39164 0.82474 3 2 5 11 0.57254 1.00533 5 3 5 11 15.7050 1.60983 5 3 5 11 10.8801 1.55974 2 3 5 11 16.4739 1.95808 3 4 5 11 7.00026 1.09288 5 4 5 11 7.85233 1.14102 3 5 5 11 20.7220 2.01570 4 5 5 11 22.0847 1.70472 3 6 5 11 94.0886 3.62421 5 6 5 11 92.6729 4.19467 4 3 -6 -11 2.85011 1.39243 5 -3 6 11 7.12463 1.81300 5 -3 6 11 1.74880 1.45827 3 2 -6 -11 4.51196 1.21925 5 -2 6 11 8.35131 1.43032 3 -2 6 11 6.80217 1.63577 5 1 -6 -11 48.3778 2.43773 5 -1 6 11 49.9480 2.87466 3 -1 6 11 45.0282 2.97280 5 0 -6 -11 0.66164 0.68122 5 0 6 11 -0.6134 1.08739 5 0 6 11 2.54273 1.11676 3 -1 -6 -11 15.4736 0.95927 5 1 6 11 16.0872 1.90103 3 1 6 11 14.8085 1.92542 5 2 6 11 13.1850 1.75191 5 2 6 11 12.3373 1.48400 3 3 6 11 25.9574 2.01349 5 3 6 11 24.4729 2.02400 3 4 6 11 46.1306 2.61928 5 4 6 11 54.2943 2.68687 3 5 6 11 53.3506 2.59272 5 6 6 11 0.61279 1.08724 4 2 -7 -11 88.9244 4.04602 5 -2 7 11 78.5712 4.38616 3 -2 7 11 87.8426 4.59703 5 -1 7 11 10.9457 1.74769 5 -1 7 11 9.89342 1.70938 3 0 -7 -11 53.1321 2.35096 5 0 7 11 52.7445 3.01913 3 0 7 11 46.4700 3.15663 5 1 7 11 38.8222 2.57080 3 1 7 11 35.1687 2.70915 5 2 7 11 32.4212 2.51130 5 2 7 11 32.8781 2.45880 3 3 7 11 45.6745 2.80326 3 3 7 11 43.4810 2.70783 5 4 7 11 64.7532 3.27576 3 4 7 11 60.4314 3.07263 5 5 7 11 8.71909 1.47778 3 0 8 11 33.7327 2.96889 3 0 8 11 36.6987 3.18907 5 1 8 11 32.3230 2.93602 5 1 8 11 28.2298 2.59229 3 2 8 11 113.173 4.88671 3 2 8 11 119.996 5.06467 5 3 8 11 18.2368 2.45476 5 3 8 11 16.9557 1.99306 3 4 8 11 6.13151 1.45817 3 3 2 -12 3.11605 1.05026 2 3 2 -12 2.02417 1.07646 5 -3 -2 12 1.86072 1.02970 5 2 2 -12 -0.4442 0.73357 2 2 2 -12 -0.1454 0.80522 5 -2 -2 12 1.23948 0.90180 5 1 2 -12 51.6814 2.47855 5 -1 -2 12 53.6355 2.86327 4 -1 -2 12 52.4525 2.60833 5 0 2 -12 98.0401 3.87932 5 0 -2 12 103.449 4.28506 4 0 -2 12 107.468 4.08942 5 -1 2 -12 3.44265 0.85557 5 1 -2 12 1.74811 0.86864 5 1 -2 12 3.94342 1.25938 4 4 1 -12 53.7628 3.26981 5 4 1 -12 64.2192 3.05656 2 -4 -1 12 59.2009 3.02832 5 3 1 -12 86.4354 3.62920 5 3 1 -12 85.8418 3.52510 2 -3 -1 12 86.4514 3.70008 5 2 1 -12 2.49534 0.78420 2 2 1 -12 3.85943 0.91225 5 -2 -1 12 2.49018 0.96727 5 1 1 -12 95.6628 3.63683 5 -1 -1 12 91.8485 3.78652 5 0 1 -12 151.036 5.11314 5 0 -1 12 143.090 5.28381 5 -1 1 -12 61.0811 2.51939 5 1 -1 12 59.8580 3.01144 4 1 -1 12 52.3211 2.66936 5 -2 1 -12 -0.2722 0.74401 5 2 -1 12 0.49753 0.79400 5 2 -1 12 -0.5146 0.97060 4 -3 1 -12 97.8686 3.83932 5 3 -1 12 98.6962 4.25312 4 3 -1 12 93.8331 3.86997 5 4 0 -12 14.0274 1.68920 2 4 0 -12 13.3850 1.56885 5 -4 0 12 13.8602 1.91743 5 3 0 -12 51.1325 2.48551 2 3 0 -12 48.6652 2.60137 5 -3 0 12 52.7127 2.79164 5 2 0 -12 10.8322 1.30436 5 2 0 -12 9.19030 1.18773 2 -2 0 12 7.20464 1.11288 5 1 0 -12 40.8641 2.09447 5 -1 0 12 42.1182 2.31926 5 0 0 -12 141.353 4.82925 5 0 0 12 136.564 5.08508 5 -1 0 -12 2.67250 0.66226 5 1 0 12 1.86270 0.80141 5 -2 0 -12 50.8427 2.30139 5 2 0 12 52.3303 2.85404 4 2 0 12 56.1283 2.61033 5 -3 0 -12 59.8493 2.59231 5 3 0 12 58.0590 3.06420 4 3 0 12 57.0073 2.73872 5 -4 0 -12 33.8388 2.31345 5 4 0 12 31.4696 2.47612 4 4 0 12 32.3156 2.03561 5 4 -1 -12 56.8211 2.98763 5 4 -1 -12 55.5450 2.76842 2 -4 1 12 55.6834 3.13682 5 3 -1 -12 22.1174 1.80453 5 3 -1 -12 17.8702 1.57031 2 -3 1 12 18.9077 1.94224 5 2 -1 -12 18.2820 1.39861 2 2 -1 -12 19.0170 1.59630 5 -2 1 12 18.1825 1.77594 5 1 -1 -12 90.9003 3.46464 2 1 -1 -12 93.2628 3.55900 5 0 -1 -12 26.4798 1.52884 5 0 1 12 26.5804 1.89277 5 -1 -1 -12 102.367 3.69234 5 1 1 12 108.590 4.13953 5 -2 -1 -12 2.01989 0.58586 5 2 1 12 2.87770 0.91529 5 -3 -1 -12 63.2760 2.56858 5 3 1 12 66.7619 2.92239 5 3 1 12 62.4070 3.21497 4 4 1 12 60.5234 2.76412 5 4 1 12 55.4923 3.08595 4 5 1 12 34.3320 2.13929 5 5 1 12 29.6430 2.67356 4 4 -2 -12 8.62361 1.20035 2 4 -2 -12 6.40740 1.19458 5 -4 2 12 7.35337 1.37651 5 3 -2 -12 74.7542 3.28143 5 3 -2 -12 70.2589 2.96414 2 -3 2 12 63.6921 3.35018 5 2 -2 -12 47.0357 2.42841 5 2 -2 -12 48.7294 2.17449 2 -2 2 12 41.6999 2.61586 5 1 -2 -12 6.78301 0.90579 5 1 -2 -12 7.56441 1.00986 2 -1 2 12 8.94493 1.30798 5 0 -2 -12 3.28739 0.69824 5 0 2 12 3.97324 1.01786 5 -2 -2 -12 52.7363 2.08474 5 2 2 12 52.9896 2.62574 5 -3 -2 -12 48.7365 1.97858 5 3 2 12 47.4268 2.43861 5 4 2 12 0.10022 0.84017 5 4 2 12 0.77503 1.08132 4 5 2 12 11.6093 1.89692 4 5 2 12 12.2765 1.31986 5 4 -3 -12 2.20140 1.01839 2 4 -3 -12 2.82669 1.19039 5 -4 3 12 3.52789 1.41921 3 -4 3 12 4.85313 1.51501 5 3 -3 -12 17.6398 1.85176 5 3 -3 -12 22.1150 1.65077 2 -3 3 12 23.0516 2.14040 3 -3 3 12 18.7856 2.18052 5 2 -3 -12 7.28118 0.89009 2 2 -3 -12 5.55002 1.02181 5 -2 3 12 6.19710 1.19191 5 -2 3 12 4.95111 1.13615 3 1 -3 -12 38.1866 2.04106 5 1 -3 -12 39.2504 1.84505 2 -1 3 12 38.6315 2.37217 3 -1 3 12 39.1510 2.43981 5 0 -3 -12 33.7076 1.71589 5 0 3 12 34.2229 2.20686 5 0 3 12 35.5115 2.17675 3 -1 -3 -12 25.0231 2.73545 5 -1 -3 -12 26.2626 1.39431 5 1 3 12 29.0595 1.87580 3 1 3 12 26.2468 1.98712 5 -2 -3 -12 95.0644 3.20464 5 2 3 12 96.1344 3.88963 5 2 3 12 95.5960 4.22753 3 -3 -3 -12 88.3244 2.95162 5 3 3 12 89.9833 3.64119 5 4 3 12 237.770 7.80969 5 4 3 12 233.519 8.31484 4 5 3 12 1.79060 0.95005 5 5 3 12 0.98203 1.06856 4 3 -4 -12 99.3269 4.18464 5 3 -4 -12 91.6751 3.66836 2 -3 4 12 99.7285 4.47034 5 -3 4 12 95.1875 4.24878 3 2 -4 -12 21.0434 1.41678 2 2 -4 -12 18.6673 1.78154 5 -2 4 12 26.3816 2.31535 5 -2 4 12 17.5441 2.07860 3 1 -4 -12 30.2969 1.88841 5 -1 4 12 33.8921 2.45495 5 -1 4 12 31.8161 2.33280 3 0 4 12 27.4432 2.12189 3 0 4 12 26.5329 2.17394 5 -1 -4 -12 424.561 12.7011 5 1 4 12 416.395 13.4109 5 1 4 12 426.666 13.2859 3 -2 -4 -12 34.4724 1.43240 5 2 4 12 38.1639 2.28401 5 2 4 12 35.5188 2.17505 3 3 4 12 26.3146 2.00097 5 4 4 12 0.72630 0.85495 3 4 4 12 0.99289 0.94914 5 5 4 12 0.50906 0.94241 5 5 4 12 1.17050 1.09886 4 3 -5 -12 29.3032 1.96122 2 3 -5 -12 22.0523 2.37388 5 -3 5 12 22.6920 2.97771 5 -3 5 12 22.0129 2.74266 3 2 -5 -12 -0.5528 0.99292 5 -2 5 12 0.04427 1.17530 3 -2 5 12 -1.1100 1.22897 5 1 -5 -12 152.472 5.39331 5 -1 5 12 151.729 5.79530 3 -1 5 12 155.605 6.02989 5 0 -5 -12 22.9858 1.50153 5 0 5 12 22.9832 2.28483 5 0 5 12 25.3031 2.14477 3 -1 -5 -12 371.355 11.2680 5 1 5 12 381.423 12.0653 3 1 5 12 372.934 12.1566 5 2 5 12 454.154 14.2547 3 2 5 12 456.063 14.3691 5 3 5 12 16.3431 1.83441 5 3 5 12 20.6668 1.89978 3 4 5 12 22.6633 1.97775 5 4 5 12 18.3371 1.85353 3 5 5 12 -0.0198 0.96477 5 5 5 12 -0.5139 1.16779 4 2 -6 -12 3.07910 1.34161 5 -2 6 12 2.19877 1.45703 3 -2 6 12 5.91383 1.75548 5 1 -6 -12 16.8736 1.91176 5 -1 6 12 19.7266 2.55565 5 -1 6 12 16.6478 2.18080 3 0 -6 -12 59.3513 2.56366 5 0 6 12 61.6703 3.40398 5 0 6 12 61.8151 3.26857 3 1 6 12 2.64234 1.11017 3 1 6 12 -0.8745 1.15329 5 2 6 12 151.353 5.81286 3 2 6 12 158.778 5.90623 5 3 6 12 35.7674 2.56570 5 3 6 12 40.7001 2.64407 3 4 6 12 3.41171 1.19485 5 4 6 12 1.70434 1.22267 3 5 6 12 -0.3644 1.21038 5 5 6 12 1.27251 1.25462 3 0 7 12 16.5198 2.02894 5 0 7 12 16.5986 1.93076 3 1 7 12 0.41389 1.29205 3 1 7 12 3.80880 1.56457 5 2 7 12 18.0230 2.35314 3 2 7 12 20.8208 2.54167 5 3 7 12 17.1216 2.41218 5 3 7 12 21.2106 2.40545 3 4 7 12 11.5939 1.67813 3 4 7 12 11.9465 1.69052 5 1 1 -13 6.94425 1.04091 5 -1 -1 13 5.32342 1.15882 5 0 1 -13 39.3834 2.05928 5 0 -1 13 38.9060 2.69698 4 0 -1 13 30.8140 2.34981 5 -1 1 -13 2.82322 0.84018 5 1 -1 13 4.78687 1.36161 4 1 -1 13 0.99099 1.74505 5 2 0 -13 31.6984 1.97568 2 2 0 -13 31.5451 2.06234 5 -2 0 13 32.6283 2.27732 5 1 0 -13 20.9407 1.64422 5 -1 0 13 23.2308 1.93573 5 0 0 -13 5.17309 0.96700 5 0 0 13 7.97445 1.19117 5 -1 0 -13 218.281 6.94771 5 1 0 13 205.098 7.22942 5 -2 0 -13 36.3380 2.04963 5 2 0 13 36.5364 2.58522 4 2 0 13 30.5995 2.14361 5 3 -1 -13 56.6459 2.97549 5 3 -1 -13 53.3762 2.69472 2 2 -1 -13 49.7572 2.39456 2 2 -1 -13 49.6412 2.58080 5 1 -1 -13 25.9457 1.73382 5 -1 1 13 25.5900 2.06080 5 0 -1 -13 0.17362 0.64391 5 0 1 13 0.14902 0.87632 5 -1 -1 -13 33.7158 1.80883 5 1 1 13 36.8762 2.24986 5 -2 -1 -13 66.4217 2.71685 5 2 1 13 64.9797 3.07492 5 -3 -1 -13 0.27026 0.85836 5 3 1 13 4.31443 1.01660 5 3 1 13 0.03729 1.03591 4 3 -2 -13 9.56787 1.21925 2 3 -2 -13 9.94561 1.35182 5 -3 2 13 8.54094 1.61163 5 2 -2 -13 334.810 10.7539 5 2 -2 -13 327.400 10.5278 2 -2 2 13 342.599 11.1376 5 1 -2 -13 72.1252 3.15268 5 -1 2 13 80.5060 3.63476 5 0 -2 -13 34.0539 1.84679 5 -1 -2 -13 13.9910 1.23153 5 1 2 13 12.2318 1.66142 5 -2 -2 -13 62.3112 2.44156 5 2 2 13 59.1075 2.91311 5 3 2 13 4.92550 1.10185 5 4 2 13 9.91080 1.37872 5 4 2 13 8.48283 1.53517 4 3 -3 -13 6.12594 1.17871 2 3 -3 -13 8.55744 1.34170 5 -3 3 13 9.77585 1.80746 5 2 -3 -13 97.5492 3.71327 2 2 -3 -13 98.9201 3.99032 5 -2 3 13 92.5094 4.29378 5 -2 3 13 99.4918 4.25315 3 1 -3 -13 8.99310 1.09968 5 -1 3 13 8.33239 1.39799 5 -1 3 13 9.63399 1.34971 3 0 -3 -13 13.4530 1.34647 5 0 3 13 17.2751 1.86915 5 0 3 13 12.0688 1.43318 3 -1 -3 -13 1.97295 0.62572 5 1 3 13 4.74183 1.12644 3 1 3 13 1.57519 1.02528 5 -2 -3 -13 32.0530 1.55851 5 3 3 13 12.8534 1.77126 5 4 3 13 -0.2114 1.19771 4 4 3 13 2.21832 1.03627 5 2 -4 -13 10.2320 1.42740 2 2 -4 -13 11.3804 1.46982 5 -2 4 13 12.5401 1.84359 5 -2 4 13 10.3387 1.58063 3 1 -4 -13 31.1167 2.02991 5 -1 4 13 26.0292 2.39642 3 -1 4 13 29.2449 2.44948 5 0 -4 -13 0.62258 0.71451 5 0 4 13 2.17325 1.11870 3 0 4 13 -0.1234 1.08038 5 -1 -4 -13 134.787 4.44204 5 1 4 13 135.373 5.11680 3 1 4 13 128.570 5.19737 5 2 4 13 37.8947 2.43034 3 2 4 13 37.8968 2.49307 5 3 4 13 39.3323 2.39119 3 4 4 13 79.7055 3.56886 5 2 -5 -13 4.22105 1.35242 5 -2 5 13 8.86092 2.06024 3 -2 5 13 3.68460 1.89995 5 1 -5 -13 24.3183 2.02662 5 -1 5 13 20.1065 2.43564 5 -1 5 13 19.1339 2.41481 3 0 -5 -13 53.2424 2.42614 5 0 5 13 55.8929 3.18824 3 0 5 13 50.8472 3.18101 5 1 5 13 94.3183 4.33192 5 1 5 13 101.906 4.27890 3 2 5 13 209.404 7.39649 3 2 5 13 215.232 7.52924 5 3 5 13 41.9714 2.70754 5 3 5 13 34.0867 2.58261 3 4 5 13 15.4609 2.00862 3 0 6 13 53.1139 3.26818 3 0 6 13 52.2833 3.35510 5 1 6 13 14.3004 1.80126 3 1 6 13 14.2593 1.94254 5 2 6 13 10.9715 1.64700 3 2 6 13 10.9460 1.69825 5 3 6 13 66.7194 3.54961 3 3 6 13 73.5115 3.62163 5 0 -1 -14 115.327 4.29628 5 0 1 14 120.093 5.55846 5 1 -2 -14 26.4748 1.92268 5 0 -2 -14 8.64276 1.08727 5 0 2 14 9.08903 1.51959 5 -1 -2 -14 99.5774 3.62083 5 1 2 14 93.8960 4.15677 5 -2 -2 -14 119.977 4.51258 5 2 2 14 122.147 4.82255 5 1 -3 -14 15.0532 1.77329 5 -1 3 14 15.4341 1.94152 5 0 -3 -14 74.2786 3.01152 5 0 3 14 66.5278 3.55558 5 -1 -3 -14 38.4583 2.00007 5 2 3 14 4.55475 1.26331 5 0 -4 -14 27.1910 1.92133 5 0 4 14 29.5056 2.59070 5 0 4 14 27.1315 2.50731 3 1 4 14 14.2850 1.74189 3 1 4 14 14.9478 2.05789 5 2 4 14 6.23857 1.30069 3 2 4 14 0.71178 1.24332 5 1 5 14 56.0458 3.28638 3 0 0 0 0.00 0.00 0 _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 0.7189 _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 0.71092 6.838 7.104 10.019 72.417 85.744 73.900 ) ; _shelx_hkl_checksum 55008 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 C1 C 1.06764(12) 0.64378(13) 0.60013(8) 0.00925(16) Uani 1 1 d . . . . . C2 C 0.86615(13) 0.75480(13) 0.57949(8) 0.00904(16) Uani 1 1 d . . . . . C3 C 0.71807(12) 0.73275(13) 0.68833(9) 0.00915(16) Uani 1 1 d . . . . . C4 C 0.79096(13) 0.58247(13) 0.81665(9) 0.01072(16) Uani 1 1 d . . . . . H4 H 0.6997 0.5572 0.8922 0.013 Uiso 1 1 calc R U . . . C5 C 0.99177(13) 0.47335(13) 0.83276(9) 0.01053(16) Uani 1 1 d . . . . . H5 H 1.0366 0.3727 0.9195 0.013 Uiso 1 1 calc R U . . . C6 C 1.34255(13) 0.38421(14) 0.75540(10) 0.01397(18) Uani 1 1 d . . . . . H6A H 1.3790 0.2921 0.6963 0.021 Uiso 1 1 calc R U . . . H6B H 1.3606 0.3031 0.8542 0.021 Uiso 1 1 calc R U . . . H6C H 1.4306 0.4774 0.7333 0.021 Uiso 1 1 calc R U . . . C7 C 1.22236(13) 0.66929(14) 0.48694(9) 0.01321(17) Uani 1 1 d . . . . . H7A H 1.1544 0.7622 0.3994 0.020 Uiso 1 1 calc R U . . . H7B H 1.2910 0.5355 0.4736 0.020 Uiso 1 1 calc R U . . . H7C H 1.3229 0.7270 0.5137 0.020 Uiso 1 1 calc R U . . . N1 N 1.12814(11) 0.50447(11) 0.72884(8) 0.00952(15) Uani 1 1 d . . . . . O1 O 0.80721(10) 0.88597(10) 0.45067(7) 0.01354(15) Uani 1 1 d . . . . . H1O H 0.677(3) 0.949(3) 0.452(2) 0.052(6) Uiso 1 1 d . . . . . O2 O 0.53234(10) 0.84161(10) 0.66573(7) 0.01308(15) Uani 1 1 d . . . . . C8 C 0.20047(12) 0.92636(13) 0.95892(8) 0.00975(16) Uani 1 1 d . . . . . C9 C 0.03678(13) 0.95351(13) 0.87318(8) 0.01011(16) Uani 1 1 d . . . . . H9 H 0.0612 0.9223 0.7866 0.012 Uiso 1 1 calc R U . . . C10 C -0.16245(13) 1.02634(13) 0.91429(9) 0.01028(16) Uani 1 1 d . . . . . H10 H -0.2732 1.0439 0.8556 0.012 Uiso 1 1 calc R U . . . O3 O 0.39904(10) 0.85127(11) 0.92593(7) 0.01518(15) Uani 1 1 d . . . . . H2O H 0.412(3) 0.851(3) 0.840(2) 0.041(5) 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 C1 0.0085(3) 0.0101(3) 0.0085(3) -0.0023(3) 0.0000(3) -0.0019(3) C2 0.0091(3) 0.0099(3) 0.0071(3) -0.0017(3) -0.0001(3) -0.0017(3) C3 0.0080(3) 0.0105(3) 0.0086(3) -0.0030(3) 0.0002(3) -0.0018(3) C4 0.0095(4) 0.0124(4) 0.0086(3) -0.0016(3) 0.0011(3) -0.0021(3) C5 0.0109(4) 0.0102(3) 0.0085(3) -0.0009(3) 0.0000(3) -0.0017(3) C6 0.0075(4) 0.0154(4) 0.0147(4) -0.0015(3) -0.0016(3) 0.0010(3) C7 0.0094(4) 0.0164(4) 0.0116(4) -0.0026(3) 0.0028(3) -0.0024(3) N1 0.0073(3) 0.0101(3) 0.0094(3) -0.0018(2) -0.0007(2) -0.0006(2) O1 0.0097(3) 0.0168(3) 0.0077(3) 0.0013(2) -0.0002(2) 0.0014(2) O2 0.0074(3) 0.0167(3) 0.0104(3) -0.0011(2) -0.0004(2) 0.0012(2) C8 0.0077(3) 0.0102(3) 0.0091(3) -0.0014(3) 0.0020(3) -0.0008(3) C9 0.0108(4) 0.0109(4) 0.0076(3) -0.0021(3) 0.0011(3) -0.0021(3) C10 0.0092(4) 0.0117(4) 0.0085(3) -0.0018(3) -0.0002(3) -0.0018(3) O3 0.0075(3) 0.0232(3) 0.0116(3) -0.0057(3) 0.0023(2) 0.0012(2) 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 N1 C1 C2 118.91(8) . . ? N1 C1 C7 118.94(7) . . ? C2 C1 C7 122.15(7) . . ? O1 C2 C1 118.26(7) . . ? O1 C2 C3 119.45(7) . . ? C1 C2 C3 122.28(8) . . ? O2 C3 C4 124.12(8) . . ? O2 C3 C2 120.44(8) . . ? C4 C3 C2 115.42(7) . . ? C5 C4 C3 120.61(8) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? N1 C5 C4 122.01(8) . . ? N1 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 N1 C1 120.70(7) . . ? C5 N1 C6 118.77(7) . . ? C1 N1 C6 120.53(7) . . ? C2 O1 H1O 109.2(13) . . ? O3 C8 C9 122.95(8) . . ? O3 C8 C10 117.73(8) . 2_577 ? C9 C8 C10 119.31(7) . 2_577 ? C10 C9 C8 120.17(7) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C8 120.52(8) . 2_577 ? C9 C10 H10 119.7 . . ? C8 C10 H10 119.7 2_577 . ? C8 O3 H2O 112.1(12) . . ? 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 N1 1.3757(10) . ? C1 C2 1.3790(11) . ? C1 C7 1.4961(12) . ? C2 O1 1.3554(10) . ? C2 C3 1.4339(11) . ? C3 O2 1.2855(10) . ? C3 C4 1.4177(11) . ? C4 C5 1.3700(11) . ? C4 H4 0.9500 . ? C5 N1 1.3529(11) . ? C5 H5 0.9500 . ? C6 N1 1.4742(11) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? O1 H1O 0.88(2) . ? C8 O3 1.3685(10) . ? C8 C9 1.3959(12) . ? C8 C10 1.3971(12) 2_577 ? C9 C10 1.3946(11) . ? C9 H9 0.9500 . ? C10 C8 1.3970(12) 2_577 ? C10 H10 0.9500 . ? O3 H2O 0.86(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 O1 H1O O2 0.88(2) 1.91(2) 2.6523(9) 140.7(18) 2_676 O3 H2O O2 0.86(2) 1.88(2) 2.7097(9) 160.6(18) . C4 H4 O3 0.95 2.58 3.1625(11) 120.2 . C7 H7C O2 0.98 2.60 3.5361(12) 160.6 1_655 C9 H9 O1 0.95 2.59 3.2978(10) 131.5 2_676 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 N1 C1 C2 O1 -177.62(7) . . . . ? C7 C1 C2 O1 2.13(13) . . . . ? N1 C1 C2 C3 1.13(13) . . . . ? C7 C1 C2 C3 -179.13(8) . . . . ? O1 C2 C3 O2 -2.48(13) . . . . ? C1 C2 C3 O2 178.79(8) . . . . ? O1 C2 C3 C4 176.02(7) . . . . ? C1 C2 C3 C4 -2.71(12) . . . . ? O2 C3 C4 C5 -179.66(8) . . . . ? C2 C3 C4 C5 1.90(12) . . . . ? C3 C4 C5 N1 0.48(14) . . . . ? C4 C5 N1 C1 -2.23(13) . . . . ? C4 C5 N1 C6 178.60(8) . . . . ? C2 C1 N1 C5 1.40(12) . . . . ? C7 C1 N1 C5 -178.35(8) . . . . ? C2 C1 N1 C6 -179.45(8) . . . . ? C7 C1 N1 C6 0.80(12) . . . . ? O3 C8 C9 C10 178.52(8) . . . . ? C10 C8 C9 C10 -0.26(14) 2_577 . . . ? C8 C9 C10 C8 0.26(14) . . . 2_577 ? _cod_database_fobs_code 2022893