#------------------------------------------------------------------------------ #$Date: 2019-02-14 05:36:51 +0200 (Thu, 14 Feb 2019) $ #$Revision: 213640 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/15/2021508.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_2021508 loop_ _publ_author_name 'Losev, Evgeniy A.' 'Boldyreva, Elena' _publ_section_title ; Concomitant cocrystal and salt: no interconversion in the solid state ; _journal_coeditor_code KU3233 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229619001372 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac 'C3 H7 N O2 +, C4 H6 O6 -' _chemical_formula_moiety 'C3 H7 N O2 +, C4 H6 O6 -' _chemical_formula_sum 'C7 H13 N O8' _chemical_formula_weight 239.18 _chemical_name_common '\b-Alanine--DL-tartaric acid (1/1)' _chemical_name_systematic '\b-Alaninium DL-tartarate' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 103.063(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.8873(3) _cell_length_b 9.4416(4) _cell_length_c 21.7392(11) _cell_measurement_reflns_used 3010 _cell_measurement_temperature 293 _cell_measurement_theta_max 29.5530 _cell_measurement_theta_min 1.9360 _cell_volume 977.17(9) _computing_cell_refinement ; CrysAlis PRO (Agilent, 2014) ; _computing_data_collection ; CrysAlis PRO (Agilent, 2014) ; _computing_data_reduction ; CrysAlis PRO (Agilent, 2014) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; olex2.solve (Bourhis et al., 2015) ; _diffrn_ambient_temperature 293 _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_unetI/netI 0.0535 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 11029 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.371 _diffrn_reflns_theta_min 1.923 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.151 _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_correction_T_min 0.931 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; (CrysAlis PRO; Agilent, 2014) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.626 _exptl_crystal_description block _exptl_crystal_F_000 504 _exptl_crystal_size_max 1 _exptl_crystal_size_mid 0.0952 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.191 _refine_diff_density_min -0.201 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 151 _refine_ls_number_reflns 1996 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.017 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0402 _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^)+(0.0360P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0724 _refine_ls_wR_factor_ref 0.0822 _reflns_number_gt 1403 _reflns_number_total 1996 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ku3233sup1.cif _cod_data_source_block RT_cocrystal_heating _cod_database_code 2021508 _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 0.864 _shelx_estimated_absorpt_t_max 0.994 _shelx_hkl_file ; 0 0 -2 63.4624 1.78169 1 0 0 2 67.1716 1.87903 1 0 0 3-1.61012 1.17790 1 0 0 -3-0.14510 0.91144 1 0 0 3-1.82694 1.09485 2 0 0 4 17.2257 1.67707 2 0 0 4 17.7364 1.79364 1 0 0 -4 17.0134 1.58480 1 0 0 -5 0.32129 1.17582 1 0 0 5 0.14260 1.51575 1 0 0 5 0.00929 1.36785 2 0 0 6 95.3489 3.50060 2 0 0 -6 100.146 3.83365 1 0 0 6 93.8384 3.84550 1 0 0 -7-2.35214 1.59280 1 0 0 7 0.86838 1.86805 1 0 0 7-0.82133 1.60350 2 0 0 8 207.489 6.30871 1 0 0 8 228.120 5.99169 2 0 0 -8 214.914 6.32301 1 0 0 9-4.90447 2.41724 1 0 0 -9 1.12305 1.89858 1 0 0 9-0.91068 1.97886 2 0 0 -10 2.15010 2.15754 1 0 0 10 5.84542 2.29773 2 0 0 10 0.36143 2.37179 1 0 0 11-0.87724 2.57017 1 0 0 -11 1.42134 2.30141 1 0 0 11 0.96039 2.11328 2 0 0 -12 49.8308 4.40394 1 0 0 12 57.1706 4.22388 2 0 0 12 46.2954 4.48070 1 0 0 13 0.60157 2.67623 2 0 0 13-1.14701 2.95463 1 0 0 -13 0.79514 2.63600 1 0 0 14 103.481 5.93203 2 0 0 -14 113.130 6.65254 1 0 0 14 107.862 6.65690 1 0 0 15 4.90880 3.75991 1 0 0 -15 5.59107 3.36444 1 0 0 15 0.35439 2.91988 2 0 0 16 237.402 9.04935 2 0 0 -16 260.820 10.4577 1 0 0 16 248.918 10.3579 1 0 0 -17-0.29355 3.53073 1 0 0 17 0.34156 3.62763 2 0 0 17 1.90433 4.25192 1 0 0 18 234.857 10.9083 1 0 0 18 239.878 10.0022 2 0 0 -18 235.575 10.8193 1 0 0 -19-2.40813 4.08229 1 0 0 19-3.07860 4.17346 2 0 0 19 0.76240 4.81983 1 0 0 -20 59.2769 6.78920 1 0 0 20 43.1299 5.92088 2 0 0 20 39.7660 6.74145 1 0 0 21-4.93157 5.20992 2 0 0 -21 0.49364 4.45071 1 0 0 21-8.20672 5.92723 1 0 0 -22-2.27514 4.74560 1 0 0 22-1.73863 6.51563 1 0 0 22-7.42947 5.20859 2 0 0 23 7.45131 5.60318 2 0 0 -23 2.84808 5.28421 1 0 0 23 3.88967 6.71686 1 0 0 -24 3.15055 5.86128 1 0 0 24-3.87386 6.25173 2 0 0 24 6.83247 7.04592 1 0 0 25-1.47034 6.42962 2 0 0 25-5.86668 7.99083 1 0 0 -25-1.04281 6.90127 1 0 0 -26 0.80912 8.41741 1 0 0 26 6.01984 7.29145 2 0 0 26-3.11725 7.53573 1 0 0 27 4.00268 7.54832 1 0 0 -27-4.58285 10.0122 1 0 0 28 21.1553 9.43341 1 0 0 28 29.1431 8.78911 2 0 0 -28 11.8217 11.3335 1 0 0 29 1.57544 10.2828 1 0 0 29-9.09395 10.0666 2 0 0 -29 14.9053 12.9153 1 0 -1 0 0.71563 0.83457 2 0 1 0 0.86905 1.06878 2 0 1 1 17.0283 1.39954 2 0 1 1 15.8271 1.00150 1 0 -1 -1 15.8801 1.24218 2 0 -1 -1 15.9950 0.97389 1 0 1 2 59.4864 2.23284 2 0 1 2 65.1068 2.03291 1 0 1 -2 60.5429 1.77191 1 0 -1 -2 66.3634 2.05424 1 0 -1 2 62.8783 1.81106 1 0 -1 -2 62.5324 2.24100 2 0 -1 -3 246.359 4.35913 1 0 -1 3 243.904 4.01847 1 0 1 -3 248.890 4.03419 1 0 1 3 251.318 4.38926 1 0 -1 -3 250.360 4.54085 2 0 1 3 250.158 4.57345 2 0 1 4 2.98200 1.49550 1 0 1 4 4.23043 1.42927 2 0 -1 -4 4.32923 1.63517 2 0 -1 4 4.50356 1.41720 1 0 -1 -4 5.56757 1.36968 1 0 1 -4 5.00572 1.30785 1 0 -1 5 0.39821 1.41793 1 0 -1 -5-0.49599 1.49680 2 0 -1 -5-1.07782 1.31727 1 0 1 -5 0.95571 1.42630 1 0 1 5-1.38003 1.61128 2 0 1 5 1.24942 1.47912 1 0 1 6 174.932 4.89545 2 0 -1 -6 183.294 5.07065 2 0 -1 6 174.202 4.85939 1 0 -1 -6 176.823 5.19189 1 0 1 -6 177.061 4.98443 1 0 1 6 178.642 5.07309 1 0 -1 7 8.94344 2.04270 1 0 1 -7 10.3266 1.90247 1 0 -1 -7 9.88551 2.25030 1 0 1 7 11.3326 2.27284 1 0 1 7 7.56098 2.08721 2 0 -1 -7 9.89917 2.17966 2 0 1 8 2.75302 2.12009 1 0 -1 8-0.28029 1.85375 1 0 -1 -8-0.18668 2.08173 1 0 1 -8 1.35585 1.76804 1 0 -1 -8 2.88673 2.03706 2 0 1 8-1.03375 1.95937 2 0 1 -9 21.6288 2.63945 1 0 -1 -9 18.8064 2.82372 2 0 1 9 18.4602 2.76846 1 0 -1 -9 15.8166 2.59719 1 0 1 9 15.6788 2.55326 2 0 -1 9 15.8364 2.37934 1 0 -1 -10 3.39243 2.55084 1 0 1 10 4.32815 2.20336 2 0 1 -10 0.49334 2.22962 1 0 1 10 4.41710 2.35992 1 0 -1 10 3.79796 2.48394 1 0 1 -11 217.941 7.66299 1 0 -1 -11 204.154 7.45259 1 0 1 11 205.932 7.59231 1 0 -1 11 213.856 7.39651 1 0 1 11 204.069 7.03011 2 0 -1 12 12.6723 2.88088 2 0 -1 -12 8.14071 3.16428 1 0 1 -12 8.37969 3.01334 1 0 -1 12 7.34584 2.97830 1 0 1 12 9.23263 2.89176 2 0 1 12 8.59192 2.97510 1 0 -1 -13 270.099 9.51641 1 0 -1 13 245.602 8.05000 2 0 1 13 244.464 8.95057 1 0 1 -13 247.104 8.87829 1 0 1 13 248.999 8.47935 2 0 -1 13 243.811 8.83769 1 0 1 -14 67.9205 5.64630 1 0 -1 14 72.3546 5.33312 1 0 -1 14 67.2192 4.97914 2 0 1 14 62.7038 4.97495 2 0 1 14 69.5075 5.80908 1 0 -1 -14 59.7916 5.04000 1 0 1 15 36.4221 4.58080 2 0 -1 15 39.5556 4.90119 1 0 1 15 38.3150 4.92608 1 0 -1 -15 42.0008 5.07864 1 0 1 -15 43.8686 4.95754 1 0 -1 15 42.5396 4.55320 2 0 -1 -16 7.82933 4.19998 1 0 1 -16 16.3619 3.81073 1 0 -1 16 16.2381 4.46579 1 0 1 16 12.3471 3.37893 1 0 1 16 14.2498 3.90880 2 0 -1 16 8.42448 3.63422 2 0 1 17 8.06850 3.78499 2 0 1 -17 10.2537 4.47567 1 0 -1 -17 4.86981 4.46664 1 0 -1 17 9.53072 4.47224 1 0 1 17 7.71569 4.16348 1 0 -1 17 5.00415 3.52586 2 0 1 -18 100.832 7.94112 1 0 1 18 100.768 8.01443 1 0 1 18 104.968 7.17899 2 0 -1 -18 110.678 8.08522 1 0 -1 18 99.6861 6.82172 2 0 -1 18 109.122 7.72561 1 0 -1 19-3.49282 3.99125 2 0 1 19 3.14105 4.16474 2 0 1 -19 1.33108 4.88293 1 0 -1 19 1.31985 3.86752 1 0 -1 -19 8.97039 4.30900 1 0 1 19 1.21073 4.95148 1 0 1 -20 104.212 8.64386 1 0 -1 20 104.168 8.59543 1 0 -1 20 98.9656 7.58811 2 0 1 20 97.1275 7.86985 2 0 1 20 108.848 8.86698 1 0 -1 -20 98.4770 8.34023 1 0 1 21 63.9877 7.84482 1 0 1 -21 58.3287 7.14320 1 0 1 21 59.6103 7.19173 2 0 -1 21 53.9565 7.62268 1 0 -1 21 49.7010 6.33438 2 0 -1 -21 45.7532 7.45479 1 0 -1 22 38.6561 7.51104 1 0 -1 22 19.5597 5.82639 2 0 1 -22 30.6605 6.11460 1 0 -1 -22 37.4394 7.65402 1 0 1 22 36.1572 6.81516 1 0 1 22 33.3738 6.56722 2 0 1 -23 50.1846 7.56012 1 0 -1 23 57.5737 7.69845 2 0 -1 -23 58.3191 9.18652 1 0 -1 23 45.9100 8.40252 1 0 1 23 57.9376 7.85017 1 0 1 23 56.4046 7.62848 2 0 -1 -24 71.3610 9.72901 1 0 1 24 67.7163 8.68789 1 0 1 -24 78.8114 8.94959 1 0 -1 24 78.1115 9.31233 1 0 1 24 77.7294 8.64166 2 0 -1 24 70.8370 8.25673 2 0 -1 25 27.1181 7.45270 1 0 -1 -25 16.5967 7.36176 1 0 1 25 26.2703 7.06120 2 0 1 25 22.1200 7.20975 1 0 -1 25 6.48551 6.66605 2 0 1 -25 25.5136 8.03814 1 0 -1 26 5.71361 8.05758 1 0 1 -26 10.2018 8.26108 1 0 -1 -26 4.32952 7.02371 1 0 1 26-9.58825 7.62026 2 0 -1 26 6.92317 7.71717 2 0 1 26 8.40978 7.77806 1 0 -1 -27 2.36517 8.95285 1 0 -1 27-3.72942 10.0966 1 0 1 27 3.88918 8.15721 1 0 -1 27 13.3616 8.04844 2 0 1 -27 9.25435 8.68285 1 0 1 27 3.94078 8.46982 2 0 1 28 3.01883 8.92440 1 0 -1 -28-2.41249 11.1257 1 0 1 28-15.6299 10.6726 2 0 -1 28 3.37775 11.5755 1 0 1 -28-8.15974 10.4849 1 0 -1 28-11.6671 9.44222 2 0 1 29 3.09787 9.63466 1 0 -1 29 5.88174 10.0903 2 0 1 29 32.0397 11.0102 2 0 1 -29 8.11330 10.4843 1 0 -1 -29 1.40180 12.4231 1 0 -1 29 5.39066 12.0677 1 0 -2 0 312.085 5.53729 2 0 -2 0 316.575 3.89711 1 0 2 0 309.000 3.92545 1 0 2 0 304.381 5.54107 2 0 2 1 1.85175 1.57854 2 0 -2 -1 2.63683 1.57491 2 0 -2 -1 3.55659 0.97076 1 0 -2 1 2.29771 0.82828 1 0 -2 1 1.75835 1.53764 2 0 2 1 1.20528 0.99298 1 0 -2 1 0.80697 0.85417 1 0 -2 -2 2590.52 13.1773 1 0 2 -2 2603.24 11.8676 1 0 2 2 2563.12 13.2786 1 0 -2 2 2629.47 11.7714 1 0 -2 -2 2619.35 16.4943 2 0 2 2 2602.98 16.5032 2 0 -2 3 150.605 3.33060 1 0 2 3 152.569 3.77308 1 0 2 3 150.984 4.43159 2 0 -2 -3 152.956 4.46350 2 0 -2 -3 161.505 3.86435 1 0 2 -3 153.923 3.37936 1 0 -2 -4 199.531 5.21856 2 0 -2 -4 206.368 4.79585 1 0 2 4 188.300 4.64100 1 0 2 -4 191.772 4.18601 1 0 -2 4 189.505 4.18241 1 0 2 4 190.031 5.16206 2 0 -2 5 204.409 4.83041 1 0 2 5 213.641 5.34424 1 0 -2 -5 200.358 5.16455 1 0 2 5 197.397 5.57838 2 0 -2 -5 203.237 5.56781 2 0 2 -5 195.197 4.68905 1 0 2 6 23.2247 2.54112 1 0 2 -6 19.7080 2.12899 1 0 -2 -6 21.9909 2.44055 2 0 -2 6 22.0276 2.23163 1 0 2 6 23.4270 2.60478 2 0 -2 -6 22.6882 2.49613 1 0 2 -7 355.467 7.36971 1 0 -2 -7 354.226 7.89873 1 0 -2 7 348.439 7.33218 1 0 2 7 360.751 7.92979 1 0 2 7 332.503 7.84127 2 0 -2 -7 355.600 8.11241 2 0 2 -8 134.250 5.07572 1 0 -2 8 137.473 5.12794 1 0 2 8 140.234 5.46901 1 0 -2 -8 140.716 5.61857 2 0 2 8 139.774 5.56331 2 0 -2 -8 129.690 5.38555 1 0 -2 -9 294.160 8.23170 1 0 -2 -9 300.094 8.15189 2 0 -2 9 295.730 7.77948 1 0 2 9 298.319 8.15433 2 0 2 9 282.630 8.05228 1 0 2 -9 289.823 7.69141 1 0 2 10 16.1055 3.09611 1 0 -2 -10 22.6931 3.11009 2 0 2 10 21.4997 3.24972 2 0 -2 -10 19.4836 3.33588 1 0 2 -10 24.3082 3.08437 1 0 -2 10 22.6963 3.12719 1 0 2 11 1066.23 16.7898 1 0 -2 11 1021.56 15.7514 1 0 -2 -11 1072.45 16.3151 2 0 -2 -11 1053.90 16.7795 1 0 2 11 1019.44 15.9221 2 0 2 -11 1042.03 15.9064 1 0 2 12 48.0356 4.66556 1 0 2 12 45.2743 4.20527 2 0 -2 -12 48.2582 4.37318 1 0 -2 -12 47.5804 4.49450 2 0 2 -12 43.3222 4.30896 1 0 -2 12 51.6070 4.27049 1 0 -2 -13 109.670 6.59592 1 0 -2 -13 115.582 6.48181 2 0 -2 13 111.554 6.35815 1 0 2 13 111.315 6.27477 2 0 2 13 110.961 6.61750 1 0 2 -13 116.646 6.43032 1 0 2 14 8.03256 3.04749 1 0 -2 -14 8.97061 3.22884 1 0 -2 -14 10.4730 3.79673 2 0 2 14 11.9017 3.61771 2 0 2 -14 15.8235 3.43043 1 0 -2 14 10.0812 3.22979 1 0 2 -15 2.87992 3.33338 1 0 -2 -15 3.06735 3.78021 1 0 -2 15 3.08332 3.55459 1 0 2 15 3.81593 3.82704 1 0 2 15 1.10326 3.18225 2 0 -2 -16 29.1139 5.02323 1 0 2 -16 37.5120 5.19035 1 0 -2 16 34.2306 4.51406 1 0 2 16 34.0877 4.64363 2 0 2 16 37.7775 4.97672 1 0 -2 17 3.53160 3.55381 2 0 -2 -17 9.67875 3.78660 1 0 -2 17 6.07792 4.30612 1 0 2 17 14.5647 4.81194 1 0 2 -17 3.47439 3.86894 1 0 2 17 1.97731 4.12933 2 0 2 18 110.414 7.64295 2 0 2 18 110.091 7.97191 1 0 2 -18 106.403 7.82799 1 0 -2 -18 102.426 8.16470 1 0 -2 18 104.058 7.02692 2 0 -2 18 102.520 7.83923 1 0 -2 -19-2.75717 4.98275 1 0 -2 19 4.73684 3.90823 1 0 2 -19-1.03471 4.89650 1 0 2 19 1.84566 4.75926 2 0 2 19 1.79487 4.75598 1 0 -2 19 0.90821 4.02793 2 0 2 -20 13.8590 4.99858 1 0 2 20 13.9602 4.98609 2 0 -2 -20 14.3316 5.11848 1 0 -2 20 10.7638 4.45517 2 0 2 20-4.46872 6.00525 1 0 -2 20 3.01103 5.14015 1 0 -2 21 26.0087 6.56944 1 0 -2 21 22.7704 5.48122 2 0 2 -21 30.5631 6.26607 1 0 -2 -21 23.7494 6.28221 1 0 2 21 22.9090 6.37033 1 0 2 21 27.7075 6.46037 2 0 2 22 1.20854 5.19373 1 0 -2 22 2.93748 5.11155 2 0 -2 22 1.65747 5.29229 1 0 2 22 4.82689 5.79961 2 0 2 -22 2.51382 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1 2 -10 10.1254 2.58725 1 -1 2 9 77.7234 4.42353 1 -1 -2 9 76.6321 4.45663 1 1 2 -9 81.0520 4.79539 1 1 -2 -9 81.7278 4.44088 1 -1 2 9 87.4128 5.13586 2 1 -2 -9 74.0858 4.65322 2 1 -2 -8 11.3135 2.62278 2 -1 -2 8 10.8292 2.56604 1 -1 2 8 10.1216 2.24106 1 -1 2 8 12.8619 2.87793 2 1 -2 -8 9.92065 2.29127 1 1 2 -8 9.36730 2.55031 1 1 2 -7 485.608 9.65683 1 1 -2 -7 479.609 9.82157 2 1 -2 -7 480.695 8.63060 1 -1 2 7 478.647 9.78263 2 -1 -2 7 459.269 9.17933 1 -1 2 7 465.684 8.55856 1 -1 2 6 49.8307 2.93266 1 1 2 -6 47.0258 3.43683 1 1 -2 -6 48.9236 3.56938 2 -1 -2 6 46.1316 3.15383 1 1 -2 -6 43.5001 2.80025 1 -1 2 6 46.1607 3.54168 2 1 -2 -5 2372.80 16.1136 1 1 -2 -5 2489.47 19.7141 2 -1 -2 5 2396.54 19.3346 1 1 2 -5 2409.55 19.4554 1 -1 2 5 2405.22 16.2871 1 -1 2 5 2447.37 19.4774 2 -1 2 4 46.7132 2.95993 2 1 -2 -4 55.2822 3.27811 2 -1 -2 4 47.1733 3.29945 1 -1 -2 4 52.3422 3.10957 1 1 -2 -4 48.3124 2.35751 1 -1 2 4 49.6434 2.38324 1 -1 2 3 44.9751 2.84904 2 -1 2 3 48.7428 2.09191 1 1 -2 -3 47.3849 2.88575 2 -1 -2 3 47.6505 3.24440 1 1 -2 -3 45.3156 2.09731 1 -1 -2 3 49.1395 3.04743 1 1 -2 -2 1921.09 14.3232 2 -1 2 2 1910.48 14.2319 2 -1 -2 2 1934.94 16.6981 1 1 -2 -2 1989.22 10.7164 1 1 2 -2 1964.10 16.7673 1 -1 2 2 1979.08 10.3478 1 -1 2 1 44.4740 2.32436 2 -1 -2 1 39.1934 2.87294 1 -1 2 1 43.5959 1.62729 1 1 2 -1 42.6233 3.07233 1 -1 2 1 45.9055 1.60522 1 1 -2 -1 39.2863 2.26459 2 1 -2 0 635.419 5.37561 1 -1 -2 0 645.858 9.24834 2 1 2 0 646.903 9.79599 1 -1 2 0 632.272 7.01225 2 1 -2 0 634.887 7.07536 2 -1 2 0 628.235 5.25991 1 -1 -2 0 610.699 9.48368 1 1 -2 1 23.0749 1.55980 2 -1 -2 -1 25.4697 2.48568 2 -1 2 -1 22.7893 1.29279 1 -1 2 -1 20.6838 1.53276 2 1 2 1 27.2298 2.79104 1 1 -2 1 21.0668 1.35803 1 -1 -2 -1 21.6933 2.45193 1 1 -2 2 107.167 2.63340 2 -1 -2 -2 101.788 3.92515 2 -1 -2 -2 107.187 4.32203 1 1 2 2 103.756 4.46180 1 1 2 2 103.651 4.03651 2 -1 2 -2 108.477 2.71462 2 1 -2 2 107.810 2.82407 1 -1 2 -2 113.203 2.81782 1 1 -2 3 713.314 6.27659 2 1 -2 3 717.438 7.78214 1 -1 -2 -3 713.354 9.73065 2 1 2 3 706.534 9.82756 2 -1 -2 -3 713.428 10.8799 1 1 2 3 716.738 11.0895 1 -1 2 -3 700.798 7.56990 1 1 2 4 136.476 4.61722 2 1 -2 4 132.731 2.91576 2 1 -2 4 138.311 3.92294 1 -1 -2 -4 140.865 4.65559 2 -1 2 -4 139.422 3.91771 1 1 2 4 139.065 5.29807 1 -1 -2 -4 147.369 5.33269 1 -1 2 -5 1179.53 11.9972 1 1 2 5 1150.20 13.0295 2 -1 -2 -5 1208.51 13.2799 2 -1 -2 -5 1190.38 15.0057 1 1 -2 5 1217.51 12.1844 1 1 2 5 1162.55 15.1264 1 -1 -2 -6 17.2247 2.38784 2 1 -2 6 17.3385 2.19638 1 1 2 6 15.9151 2.45850 1 -1 -2 -6 16.2655 2.88353 1 1 2 6 17.1213 2.39571 2 -1 2 -6 16.4585 2.15325 1 -1 -2 -7 173.744 6.64928 1 -1 2 -7 160.316 5.42302 1 1 2 7 168.181 5.59267 2 1 -2 7 159.277 5.41110 1 -1 -2 -7 169.931 5.65363 2 1 2 7 171.946 6.64306 1 1 2 8 44.3864 3.88530 1 -1 -2 -8 40.7290 3.31476 2 -1 -2 -8 40.1784 4.03861 1 -1 2 -8 38.2912 3.35512 1 1 -2 8 36.5505 3.21395 1 1 2 8 38.8319 3.27756 2 -1 2 -9 13.7428 2.80448 1 1 2 9 10.2426 2.53014 2 1 2 9 10.5513 2.77223 1 1 -2 9 10.8352 2.47494 1 -1 -2 -9 10.0323 2.58411 2 -1 -2 -9 10.5645 2.94394 1 1 2 10 17.1235 2.92307 2 -1 -2 -10 14.3637 2.88024 2 1 2 10 15.0898 3.46753 1 -1 2 -10 14.6886 2.96879 1 -1 -2 -10 19.6693 3.26580 1 1 -2 10 16.1614 3.06029 1 -1 -2 -11 10.1971 2.95823 2 -1 -2 -11 6.97138 3.31986 1 1 -2 11 2.96192 2.69761 1 1 2 11 8.40969 2.77491 2 1 2 11 7.77419 3.54301 1 1 -2 11 9.77654 2.09961 2 -1 2 -11 9.83440 2.83875 1 -1 -2 -12 7.93913 3.01710 2 1 -2 12 6.15120 3.16383 1 1 2 12 16.3398 3.25350 2 -1 2 -12 14.1355 3.48464 1 -1 -2 -12 6.39526 3.54016 1 1 2 12 10.1114 3.69374 1 1 -2 12 14.5475 2.43684 2 1 2 13 5.13390 2.90461 2 -1 2 -13 8.29077 3.22878 1 1 -2 13 8.48946 2.52096 2 -1 -2 -13 10.6678 3.22004 2 -1 -2 -13 11.7895 4.03291 1 1 2 13 4.64306 3.04324 1 1 -2 13 7.48291 3.51137 1 1 2 14 104.375 6.14219 2 1 -2 14 110.075 5.29457 2 1 -2 14 107.904 6.79582 1 1 2 14 115.164 7.64603 1 -1 2 -14 109.255 6.87977 1 -1 -2 -14 107.675 6.41302 2 -1 -2 -14 119.470 7.44458 1 1 2 15 8.81747 4.52863 1 -1 -2 -15 7.46167 3.59665 1 1 -2 15 6.53278 2.94593 2 -1 2 -15 8.07908 4.00380 1 1 2 15 12.7322 3.78949 2 -1 -2 -15 7.31115 3.63349 2 1 -2 15 5.28314 3.31926 1 1 -2 16 24.5466 4.99482 1 1 2 16 15.6372 4.02967 2 1 -2 16 15.3706 3.39524 2 -1 -2 -16 19.5972 4.52425 1 -1 2 -16 17.4608 4.19996 1 1 2 16 26.0443 5.37931 1 1 -2 17 43.9181 4.66270 2 -1 2 -17 47.2830 6.16541 1 1 -2 17 42.9699 5.55407 1 -1 -2 -17 31.2243 5.35026 1 1 2 17 43.5849 5.27954 2 1 2 17 49.2659 6.68755 1 1 2 18 57.6656 6.01077 2 -1 -2 -18 50.6639 7.01411 1 1 -2 18 54.6402 6.81797 1 1 -2 18 49.9840 5.13460 2 1 2 18 52.2289 7.18834 1 -1 2 -18 59.6394 7.15052 1 1 -2 19 26.1807 4.74263 2 -1 2 -19 20.7072 5.82404 1 1 2 19 26.4331 7.05867 1 1 2 19 18.0759 4.99149 2 1 -2 19 11.1576 5.29798 1 -1 -2 -19 16.1342 6.60507 1 1 2 20 1.08869 4.65296 2 -1 -2 -20-5.11422 6.21937 1 1 2 20 8.79568 5.81726 1 1 -2 20 4.52808 4.20454 2 1 -2 20 1.77071 5.18285 1 -1 2 -20 1.50556 4.47004 1 -1 -2 -21 26.2699 6.69493 1 1 -2 21 5.45398 4.49632 2 1 2 21 16.9871 6.40630 1 1 2 21 4.95889 5.12297 2 1 -2 21 3.71863 6.47011 1 -1 2 -21 19.3502 6.90443 1 -1 2 -22 17.1073 7.40742 1 -1 -2 -22-3.50307 7.55313 1 1 -2 22 9.23889 4.80645 2 1 2 22 4.81136 5.67725 2 1 2 22 9.58967 8.03290 1 1 -2 22 0.48727 6.60407 1 1 -2 23 16.9009 6.55759 1 1 -2 23 1.04192 5.24230 2 -1 2 -23 14.0676 7.54815 1 -1 -2 -23 7.14039 6.82745 1 1 2 23 19.6416 6.43514 2 1 2 23 9.59310 6.77892 1 1 -2 24 6.72823 5.87618 2 1 2 24-8.22062 10.1271 1 1 2 24 6.88762 6.61346 2 -1 2 -24 4.50889 6.92433 1 1 -2 24-2.19611 7.22938 1 -1 -2 -24-4.66295 8.58657 1 -1 -2 -25 3.04819 9.12283 1 1 2 25 4.24448 8.68022 1 1 2 25-3.20667 6.99374 2 1 -2 25 5.36908 9.04217 1 -1 2 -25 3.32313 7.70154 1 1 -2 25-6.73359 6.32220 2 -1 2 -26 2.82418 10.5423 1 1 -2 26 6.91081 10.5172 1 -1 -2 -26 26.7934 10.8518 1 1 -2 26 9.33509 7.02718 2 1 2 26 3.53283 8.53231 2 1 2 26 20.7709 10.3253 1 1 2 27 20.0782 9.74181 2 -1 2 -27 1.12766 11.4895 1 1 -2 27 0.14743 7.60176 2 1 -2 27 6.00507 11.6099 1 1 2 27 26.2804 13.5585 1 -1 -2 -27-3.21570 10.7739 1 -1 -3 29-4.23717 10.4153 2 1 -3 -29 19.5773 11.8204 1 -1 3 29 8.29872 11.0493 2 -1 3 29 7.94435 12.7460 1 -1 -3 29 6.70298 10.3837 1 1 3 -29 15.9573 13.4005 1 1 3 -28 14.8928 9.03390 1 -1 3 28 24.1009 12.1181 1 1 -3 -28 9.21725 9.96751 1 -1 -3 28 9.46793 9.62577 2 -1 -3 28 4.42535 11.2624 1 -1 3 28 16.7497 10.0828 2 1 3 -27-0.38842 10.3323 1 -1 3 27-6.76947 8.43459 2 -1 -3 27 0.07630 7.34142 1 -1 -3 27-2.19961 8.81528 2 -1 3 27-9.85266 9.90808 1 1 -3 -27 6.53745 8.51719 1 -1 -3 26 0.93980 9.24999 1 -1 3 26 11.0737 8.09298 2 -1 3 26-5.24020 8.44596 1 1 -3 -26 2.28088 6.93638 1 1 3 -26-0.51478 6.93150 1 -1 -3 26 4.32599 8.25359 2 1 3 -25-9.66585 8.49747 1 -1 3 25 13.0161 7.98566 2 -1 -3 25 3.71590 7.26408 2 -1 3 25 22.5510 8.17056 1 -1 -3 25 12.3089 7.78799 1 1 -3 -25 0.13898 7.19351 1 1 3 -24 2.09804 7.22742 1 -1 -3 24 4.20204 6.15733 1 -1 3 24 17.5486 8.40435 2 1 -3 -24 3.99852 7.07215 1 -1 -3 24 13.5882 6.53826 2 -1 3 24 7.27853 6.41960 1 1 3 -23-0.37113 5.22827 1 -1 -3 23 6.89641 7.12393 1 -1 3 23-5.86516 5.41435 1 -1 3 23 1.99676 6.98808 2 1 -3 -23-2.66041 6.89488 1 -1 -3 23-2.50712 5.62745 2 1 -3 -22 11.9923 6.58301 1 1 3 -22 11.8905 5.79190 1 -1 3 22 11.2090 5.57743 1 -1 -3 22 16.4494 6.70151 1 -1 3 22 13.6919 5.80751 2 -1 3 21 7.31266 4.60176 1 -1 3 21 8.35638 6.42182 2 1 -3 -21 10.2368 5.27667 1 1 3 -21 7.35059 5.60172 1 -1 -3 21 3.84745 5.41756 1 -1 3 20 2.43550 5.20396 2 -1 -3 20 2.40186 4.70130 1 1 3 -20 0.51557 4.90927 1 1 -3 -20 9.40805 4.86008 1 -1 3 20-0.66587 4.01928 1 -1 -3 19 40.7760 5.99313 1 1 3 -19 37.0660 5.72090 1 -1 3 19 50.0716 5.94687 1 -1 3 19 38.5159 6.57194 2 1 -3 -19 47.2922 6.68420 1 1 3 -18 94.8658 7.65166 1 -1 3 18 93.5408 7.67336 2 1 -3 -18 99.2537 7.82428 1 -1 3 18 94.6797 7.27381 1 -1 -3 18 102.999 7.90347 1 -1 -3 17 33.2957 5.54081 1 -1 3 17 41.5727 5.18581 1 1 3 -17 39.9530 5.86100 1 1 -3 -17 36.7521 5.21775 1 -1 3 17 40.1922 6.10379 2 1 3 -16 33.2275 4.95535 1 1 -3 -16 19.3324 4.76060 1 -1 -3 16 20.8120 4.66766 1 -1 3 16 21.7066 5.11022 2 -1 3 16 28.2313 4.36030 1 -1 -3 15 182.346 8.73263 1 1 -3 -15 186.702 8.56451 1 1 3 -15 188.024 8.78245 1 -1 3 15 180.543 8.41419 1 -1 3 15 179.236 8.97678 2 -1 3 14-1.61694 3.17994 2 1 -3 -14 5.05223 3.44726 1 -1 -3 14 2.50629 3.05408 1 -1 3 14 2.79140 2.83668 1 1 -3 -14 3.71218 3.25223 2 1 3 -14 10.7875 3.46942 1 -1 -3 13 43.2360 4.74080 1 1 -3 -13 42.0078 4.69534 2 -1 3 13 39.9707 4.25073 1 -1 3 13 41.6654 4.91914 2 1 -3 -13 42.4966 4.57425 1 1 3 -13 44.6275 4.60204 1 -1 3 12 48.6122 4.33291 1 1 3 -12 47.1493 4.71032 1 -1 -3 12 45.8213 4.44203 1 -1 3 12 44.0421 4.97310 2 1 -3 -12 49.4810 4.30543 1 1 -3 -12 48.1294 4.64361 2 -1 3 11 44.4344 4.32752 2 -1 3 11 43.9743 4.00355 1 1 -3 -11 46.4442 4.52477 2 -1 -3 11 43.6707 4.29249 1 1 3 -11 43.4778 4.39487 1 1 -3 -11 46.7915 4.03394 1 1 3 -10 34.2724 3.60385 1 1 -3 -10 30.8053 3.33462 1 -1 3 10 37.2540 4.32302 2 1 -3 -10 24.7961 3.89082 2 -1 -3 10 34.5358 3.61347 1 -1 3 10 31.6487 3.40724 1 1 -3 -9 3.47805 2.29332 1 -1 -3 9 0.69357 2.29224 1 -1 3 9 7.74159 3.13515 2 1 3 -9 3.90015 2.39396 1 1 -3 -9 4.25138 3.00070 2 -1 3 9 4.12145 2.19407 1 1 3 -8 109.146 5.27901 1 -1 3 8 102.749 5.50204 2 -1 -3 8 115.046 5.21589 1 1 -3 -8 104.786 4.63739 1 -1 3 8 107.414 4.69955 1 1 -3 -8 116.100 5.72123 2 -1 3 7 104.410 5.40988 2 1 -3 -7 109.986 5.46532 2 -1 3 7 98.1098 4.19019 1 -1 -3 7 108.373 5.01820 1 1 3 -7 104.230 5.04834 1 1 -3 -7 107.928 4.36964 1 1 -3 -6 102.703 3.92832 1 -1 -3 6 97.2565 4.63301 1 -1 3 6 95.8720 5.01051 2 1 3 -6 89.4577 4.58366 1 -1 3 6 99.2899 3.84369 1 1 -3 -6 100.794 5.08417 2 1 -3 -5 116.135 5.11372 2 -1 3 5 109.889 4.88405 2 -1 -3 5 109.411 4.89699 1 -1 -3 5 118.580 4.86330 1 1 -3 -5 114.646 3.72866 1 -1 3 5 111.249 3.70214 1 -1 -3 4 209.814 6.17950 1 -1 -3 4 219.415 6.43875 1 -1 3 4 219.250 6.39987 2 1 -3 -4 216.581 6.38546 2 1 -3 -4 217.279 4.43954 1 -1 3 4 223.013 4.49779 1 -1 -3 3 119.525 4.73551 1 -1 3 3 118.965 4.68585 2 -1 3 3 119.673 2.89001 1 1 -3 -3 117.180 2.88929 1 1 -3 -3 123.991 4.70834 2 -1 -3 3 115.801 4.83436 1 1 -3 -2 205.489 3.04321 1 -1 -3 2 205.660 6.12023 1 -1 3 2 196.327 5.53839 2 1 3 -2 208.856 6.14830 1 -1 3 2 207.178 2.99678 1 1 -3 -2 193.029 5.51750 2 -1 -3 1 390.586 8.27813 1 1 -3 -1 419.758 7.56495 2 -1 3 1 398.749 7.34257 2 -1 -3 1 397.535 8.59837 2 1 3 -1 396.622 8.39491 1 -1 -3 0 64.9049 3.81428 1 -1 -3 0 64.3355 3.91001 2 1 -3 0 63.2752 3.10385 2 -1 3 0 66.8149 3.19248 2 1 3 0 64.2444 3.86386 1 -1 3 -1 35.0572 2.44490 2 1 3 1 40.3283 3.24066 1 -1 -3 -1 38.3153 3.35936 2 -1 -3 -1 32.6587 3.01919 1 1 -3 1 34.7375 2.41669 2 1 -3 2 122.861 2.41735 1 1 -3 2 125.754 3.87583 2 -1 -3 -2 132.122 5.18120 2 1 3 2 128.226 5.15505 1 1 3 2 130.489 5.16946 2 -1 -3 -2 121.064 5.01331 1 -1 3 -2 124.196 2.37095 1 -1 3 -2 121.666 3.92579 2 -1 3 -3 34.4430 1.72250 1 1 3 3 34.0516 3.11190 1 1 -3 3 32.0131 1.68071 1 -1 -3 -3 36.4623 3.10596 1 1 3 3 37.0385 3.18683 2 -1 -3 -3 34.5185 3.07572 2 1 -3 3 33.9100 2.23111 2 -1 3 -4 30.9528 1.96594 1 -1 -3 -4 27.3282 2.92482 2 -1 -3 -4 28.3311 3.09080 1 1 3 4 32.1152 3.26629 2 1 -3 4 30.3327 1.94541 1 1 -3 4 27.9585 2.11707 2 1 3 4 27.4825 3.03797 1 -1 -3 -5 259.837 7.54784 1 1 -3 5 249.669 5.36454 1 -1 3 -5 248.243 5.38005 1 -1 -3 -5 247.741 7.12946 2 1 3 5 249.880 7.27776 2 1 3 5 246.874 7.68607 1 1 -3 5 251.644 5.35122 2 -1 3 -6 230.356 5.72618 1 -1 -3 -6 241.456 7.30659 2 1 3 6 237.920 7.70199 1 1 3 6 221.502 7.05823 2 -1 -3 -6 206.104 7.17507 1 1 -3 6 222.684 5.58844 1 -1 -3 -7 4.28244 2.58755 2 1 3 7 6.69310 2.61376 1 1 3 7 7.32154 2.62909 2 -1 -3 -7 5.93653 2.67824 1 -1 3 -7 4.10384 1.83378 1 1 -3 7 7.06708 1.94743 1 -1 -3 -8 23.0058 3.32566 2 -1 -3 -8 15.4113 3.37219 1 1 3 8 18.1602 3.13562 2 1 3 8 19.0893 3.40407 1 -1 3 -8 21.4622 2.66443 1 1 -3 8 18.7794 2.58432 1 -1 -3 -9 15.1617 3.11025 2 1 3 9 13.8894 3.42406 1 -1 -3 -9 19.5874 3.51031 1 1 -3 9 14.8586 2.65806 1 -1 3 -9 12.1640 2.63836 1 1 3 9 11.8356 2.99972 2 1 3 10 20.0677 3.70689 1 1 3 10 21.5501 3.45967 2 -1 -3 -10 18.6043 3.36413 2 1 -3 10 22.1450 3.17200 1 -1 -3 -10 16.7170 3.47452 1 -1 3 -10 21.7280 3.21010 1 -1 -3 -11 40.1023 4.27617 2 1 -3 11 40.3622 4.01714 1 -1 -3 -11 41.7795 4.87386 1 1 3 11 40.8279 4.57067 1 -1 3 -11 39.7900 4.12096 1 1 3 11 41.0717 4.29605 2 -1 3 -12 0.28771 2.89678 1 -1 -3 -12 1.11691 3.51564 1 1 3 12-2.36396 3.38065 1 1 3 12 6.32610 3.29137 2 1 -3 12 3.95333 3.00058 1 -1 -3 -12 2.28338 3.20076 2 1 3 13 163.270 7.62982 2 1 3 13 164.350 8.45589 1 -1 -3 -13 162.412 7.74620 2 1 -3 13 165.484 7.56992 1 -1 -3 -13 162.731 8.54063 1 -1 3 -13 171.374 7.87640 1 -1 3 -14 5.45189 3.59520 1 1 3 14 13.1397 4.77310 1 1 -3 14 2.64773 3.35892 1 -1 -3 -14 6.99574 3.52226 1 -1 -3 -14 5.87382 3.49869 2 1 3 14 7.29506 3.71234 2 1 -3 15 97.0388 6.94841 1 1 -3 15 98.8442 5.43887 2 1 3 15 104.107 6.87748 2 -1 -3 -15 98.3284 7.66996 1 -1 -3 -15 101.548 6.92548 2 -1 3 -15 86.6986 6.71880 1 1 3 15 93.2289 7.20147 1 1 -3 16 40.4880 4.28361 2 1 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10.8719 1.04285 1 -2 6 -5 11.2050 1.01414 1 -2 -6 -5 16.3317 4.64752 1 2 -6 6 83.8238 3.11572 1 2 -6 6 93.2497 4.90075 2 2 6 6 97.3555 7.72776 1 -2 -6 -6 97.9712 7.30039 2 -2 -6 -6 100.272 7.31425 1 -2 6 -6 87.2069 3.00434 1 -2 6 -7 2.13297 1.61641 1 2 6 7 5.69761 4.45466 2 2 6 7 7.24982 4.94251 1 -2 -6 -7-0.82083 4.29794 2 2 -6 7-1.87633 2.46358 2 -2 -6 -7 3.24682 3.49277 1 2 -6 7 2.13587 1.74105 1 2 6 8 118.013 8.55596 1 -2 -6 -8 111.777 8.00653 2 2 6 8 109.020 7.81355 2 -2 -6 -8 124.589 8.08245 1 -2 6 -8 106.082 4.45694 1 2 -6 8 105.273 4.57241 1 2 -6 8 112.414 5.21730 2 2 6 9 59.0917 6.94278 1 -2 -6 -9 60.2454 6.49252 2 2 -6 9 46.7225 3.85289 2 -2 -6 -9 53.8075 6.35073 1 2 6 9 61.7168 6.97613 2 -2 6 -9 53.4300 3.80063 1 2 -6 9 56.8649 3.99272 1 2 6 10 25.4792 6.69256 1 2 6 10 21.6066 5.54316 2 2 -6 10 19.2139 3.06851 2 -2 -6 -10 20.6398 5.68937 2 2 -6 10 17.9533 3.20732 1 -2 6 -10 20.9174 3.24304 1 -2 -6 -10 31.2803 6.00428 1 2 6 11 87.3786 8.74761 1 2 -6 11 85.2918 4.73153 2 -2 -6 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13-3.24735 7.63207 1 -6 4 13 29.9134 9.13928 2 -6 4 13-5.38249 9.43866 1 -6 -4 13 1.13365 12.1627 1 -6 -4 13-7.94547 12.9765 1 -6 4 12 8.34337 8.19761 1 -6 4 12 7.60450 8.02820 2 -6 4 12 0.82447 8.98740 1 -6 -4 12-4.09185 12.7578 1 -6 -4 12 11.7874 11.2307 1 -6 4 11 3.47032 7.48139 1 -6 4 11 9.63451 8.05161 1 -6 -4 11 11.3540 11.9733 1 -6 4 11 12.4672 7.92171 2 -6 -4 11-14.2627 10.0213 1 -6 4 10 21.4028 8.02796 1 -6 4 10 6.54558 8.09510 1 -6 -4 10-4.60703 10.6762 1 -6 4 10 1.72441 6.85556 2 -6 -4 10 3.51431 9.95870 1 -6 4 9 7.25099 7.45097 1 -6 -4 9 5.71716 9.66220 1 -6 4 9-13.8071 6.82935 2 -6 -4 9-6.10506 11.8497 1 -6 4 9 15.3905 7.85182 1 -6 4 8 7.62881 6.90441 1 -6 -4 8-0.26540 9.70129 1 -6 4 8 10.0525 6.32283 2 -6 -4 8 11.6193 11.3191 1 -6 4 8 1.85678 7.71403 1 -6 4 7-2.49083 6.91494 1 -6 4 7 1.97487 5.81820 2 -6 4 7 3.88374 7.44010 1 -6 -4 7-18.4750 12.0801 1 -6 -4 7-14.6723 10.2913 1 -6 4 6 4.94321 5.29415 2 -6 4 6 8.21529 7.49887 1 -6 -4 6 5.54377 8.19245 2 -6 -4 6 1.43697 10.9929 1 -6 -4 6 18.8523 10.6831 1 -6 4 6 5.53697 7.15401 1 -6 4 5 5.77092 4.80039 2 -6 4 5-6.18485 7.31310 1 -6 -4 5-9.20703 8.58715 2 -6 -4 5 15.9215 10.8248 1 -6 -4 5-8.76910 11.3900 1 -6 4 5-3.45603 7.19596 1 -6 4 4-0.57024 7.35204 1 -6 4 4 2.24914 3.88025 2 -6 -4 4-4.73042 8.05023 2 -6 -4 4-13.2889 12.2835 1 -6 -4 4-0.84948 11.5256 1 -6 4 4 11.3782 7.38592 1 -6 4 3-5.60967 7.35107 1 -6 4 3-1.24918 2.72418 2 -6 -4 3-0.16251 7.86436 2 -6 -4 3 1.45685 11.3681 1 -6 -4 3-14.0168 11.9257 1 -6 4 3-7.09766 7.48834 1 -6 4 2-1.69356 7.36687 1 -6 -4 2 14.7473 9.95036 1 -6 -4 2 17.6913 7.81343 2 -6 4 2 21.3712 7.47514 1 -6 4 1 16.5608 7.29502 1 6 4 -1 4.61200 12.5749 1 -6 -4 1 9.48894 9.10354 1 -6 -4 1 20.4475 7.59483 2 -6 4 1 3.30634 7.38756 1 6 4 0-12.4354 12.0218 1 -6 4 0 0.30564 7.38944 1 -6 -4 0 19.4467 11.5484 1 -6 -4 0-5.29530 7.54826 2 -6 4 0-2.02632 8.02317 1 -6 4 -1-0.35914 7.23143 1 6 4 1 11.3140 9.99645 1 -6 -4 -1 10.3313 12.3209 1 -6 -4 -1-0.50367 7.19273 2 -6 4 -1 1.63273 8.16294 1 -6 4 -2-2.82756 7.48187 1 -6 -4 -2 31.4797 11.8468 1 -6 -4 -2 13.1521 7.49593 2 -6 4 -2 13.2502 8.49971 1 6 4 2 10.8384 13.6671 1 -6 -4 -3-2.85777 9.93563 1 -6 -4 -3 5.62556 7.42536 2 6 4 3-20.1431 11.5087 1 -6 4 -3 7.86559 8.42270 1 -6 4 -3 11.7325 7.98321 1 -6 -4 -4-4.97074 13.3243 1 6 4 4-5.28808 14.1341 1 -6 -4 -4-3.71863 6.65797 2 -6 4 -4 9.21815 8.47839 1 -6 4 -4 16.0203 8.16492 1 -6 5 14 14.4619 7.89399 1 -6 5 14-10.9031 8.40259 2 -6 5 14-4.95382 8.34039 1 -6 5 13-10.0443 7.81402 1 -6 5 13 18.7061 9.46093 1 -6 5 13 26.9892 9.89091 2 -6 -5 13 0.09846 14.1049 1 -6 -5 13 7.96239 12.2855 1 -6 5 12 15.8816 8.83299 1 -6 5 12 16.5712 8.44407 1 -6 -5 12 17.5298 12.1210 1 -6 5 12 16.3601 9.16776 2 -6 -5 12 10.1838 11.4990 1 -6 5 11 6.33217 8.40556 1 -6 5 11-0.70822 7.35043 1 -6 -5 11-4.77241 11.0915 1 -6 5 11 1.45895 8.25855 2 -6 -5 11-1.27048 9.42796 1 -6 5 10-4.26625 7.11816 1 -6 -5 10 4.61977 13.0495 1 -6 5 10-3.82857 7.27478 2 -6 -5 10-10.0849 10.3525 1 -6 5 10 9.58729 8.14774 1 -6 -5 9-1.96268 13.4128 1 -6 5 9 14.7751 7.69031 1 -6 5 9 0.04475 6.72707 2 -6 5 9-1.96242 7.51169 1 -6 -5 9 5.52593 12.1561 1 -6 -5 8-2.12985 12.7621 1 -6 5 8-15.7272 7.67110 1 -6 5 8 7.64671 6.82305 2 -6 -5 8-3.77731 10.0115 2 -6 5 8-1.83663 7.22654 1 -6 -5 8 13.8735 12.2974 1 -6 5 7 5.79023 6.90437 1 -6 5 7-8.63193 6.65807 2 -6 5 7 9.35961 7.32303 1 -6 -5 7-5.98382 8.94291 2 -6 -5 7 18.0172 12.5310 1 -6 -5 7-2.66681 13.6622 1 -6 5 6-2.63657 6.96843 1 -6 5 6-3.19807 5.81015 2 -6 5 6-2.95503 6.78077 1 -6 -5 6 5.15857 10.0911 2 -6 -5 6-1.69023 12.2355 1 -6 -5 6 16.4508 12.9400 1 -6 5 5-2.39027 7.17989 1 -6 5 5 2.06515 6.94212 1 -6 5 5 9.26328 5.03638 2 -6 -5 5-13.6815 9.63140 2 -6 -5 5-10.9914 13.5577 1 -6 -5 5 23.5358 13.3247 1 -6 5 4 12.0299 6.80752 1 -6 5 4 14.7528 7.33888 1 -6 5 4 1.60206 3.94857 2 -6 -5 4 1.81002 9.66586 2 -6 -5 4 0.54222 12.6013 1 -6 -5 4-13.0227 12.0158 1 -6 5 3-2.40337 6.70808 1 -6 -5 3-4.83562 9.03755 2 -6 5 3 0.40924 2.49482 2 -6 -5 3 18.5837 13.0048 1 -6 -5 3-7.10768 11.5538 1 -6 5 3-7.83019 6.33485 1 -6 5 2 1.27851 6.96531 1 -6 -5 2 22.7624 12.8396 1 -6 -5 2 9.71671 9.14462 2 -6 5 2 0.81718 7.01357 1 -6 5 1-13.7117 6.90222 1 6 5 -1-1.04609 10.2411 1 -6 -5 1-8.41642 10.8251 1 -6 -5 1 6.05515 8.73648 2 -6 5 1 7.18959 7.09112 1 -6 5 0 7.29993 7.12908 1 6 5 0 12.8999 13.9090 1 -6 -5 0-14.2987 10.8721 1 -6 -5 0 17.1172 8.79094 2 -6 5 0 9.27216 7.53444 1 -6 -5 -1 9.11182 8.18169 2 6 5 1 7.89842 14.6711 1 -6 5 -1-6.81113 7.39707 1 -6 5 -1 7.61252 7.26579 1 -6 -5 -2 13.7064 7.20835 2 -6 5 -2 4.99758 6.73185 1 -6 5 -2 12.8668 6.34975 1 -6 6 10 18.9102 5.13802 1 -6 6 10 11.8100 5.82275 2 -6 -6 10 13.5503 8.02781 2 -6 6 10 21.1852 5.40682 1 -6 6 9 9.14135 6.20192 1 -6 6 9 3.74608 6.24365 1 -6 -6 9-4.60858 10.0168 2 -6 6 8 29.7119 7.26319 1 -6 6 8 10.3770 7.21887 2 -6 6 8 22.7700 6.89211 1 -6 -6 8 10.7339 11.0699 2 -6 -6 8 19.1561 10.9509 1 -6 -6 8 38.2474 12.3284 1 -6 6 7 25.3421 6.97746 1 -6 6 7 4.40455 6.29062 1 -6 6 7 12.5022 6.74403 2 -6 -6 7 19.6186 11.5648 2 -6 -6 7-0.09318 10.5292 1 -6 -6 7-7.68752 10.1819 1 -6 6 6-1.39796 6.19573 1 -6 6 6-3.35165 6.54164 1 -6 6 6-8.91253 6.15771 2 -6 -6 6 5.93609 10.9473 2 -6 -6 6-8.01063 10.5573 1 -6 -6 6-4.77206 11.2902 1 -6 6 5 1.03581 6.07085 1 -6 6 5 0.85339 6.10772 1 -6 6 5-3.18363 5.31973 2 -6 -6 5 8.96324 9.69816 2 -6 -6 5-7.29401 10.7924 1 -6 -6 5 27.2285 12.0150 1 -6 6 4 20.6536 6.43036 1 -6 6 4 18.7430 6.32531 1 -6 -6 4 1.99540 9.87667 2 -6 6 4 18.7239 4.44393 2 -6 6 3 8.92006 5.44085 1 -6 6 3 5.42243 5.03870 1 -6 -6 3 14.7336 8.30372 2 -6 6 2 19.5830 4.49206 1 -6 6 2 16.2885 4.39157 1 0 0 0 0.00 0.00 0 TITL 293_II in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 4.887259 9.441645 21.739169 90.0000 103.0630 90.0000 ZERR 4.00 0.000289 0.000411 0.001115 0.0000 0.0055 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 28.00 52.00 4.00 32.00 TREF HKLF 4 END ; _shelx_hkl_checksum 20835 _shelx_res_file ; TITL RT_II_c in P2(1)/c 293_ii_.res created by SHELXL-2018/3 at 18:19:37 on 29-Nov-2018 REM P2(1)/c (#14 in standard setting) CELL 0.71073 4.887259 9.441645 21.739169 90 103.063 90 ZERR 4 0.000289 0.000411 0.001115 0 0.0055 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 28 52 4 32 EQIV $1 1-X,1-Y,-Z EQIV $2 1+X,+Y,+Z EQIV $3 2-X,0.5+Y,0.5-Z EQIV $4 -1+X,1.5-Y,-0.5+Z EQIV $5 1-X,0.5+Y,0.5-Z L.S. 10 PLAN 20 SIZE 0.04 0.0952 1 TEMP 19.85 HTAB O4 O3_$1 HTAB O3 O4_$2 HTAB O6 O8_$3 HTAB O1 O7_$4 HTAB N1 O7 HTAB N1 O8_$5 HTAB N1 O2_$1 CONF BOND $H BOND fmap 2 acta SHEL 40 0.8 TWIN -1 0 0 0 -1 0 2 0 1 2 REM REM REM WGHT 0.036000 BASF 0.22695 FVAR 0.45646 O4 4 0.283906 0.646805 0.001157 11.00000 0.02659 0.03771 = 0.03789 0.01123 0.00096 -0.00537 AFIX 147 H4 2 0.368203 0.583378 0.023417 11.00000 -1.20000 AFIX 0 O3 4 0.726287 0.617559 -0.066602 11.00000 0.01815 0.02915 = 0.03586 -0.00232 -0.00039 0.00755 AFIX 147 H3 2 0.891921 0.629047 -0.049121 11.00000 -1.20000 AFIX 0 O6 4 0.872886 0.872796 0.052630 11.00000 0.03873 0.03516 = 0.03000 -0.00068 -0.00982 -0.00855 AFIX 147 H6 2 0.995540 0.876826 0.085286 11.00000 -1.20000 AFIX 0 O1 4 0.174483 0.861715 -0.117770 11.00000 0.04183 0.03934 = 0.03053 -0.00771 -0.01046 0.02078 AFIX 147 H1 2 0.045136 0.865127 -0.149206 11.00000 -1.20000 AFIX 0 C4 1 0.717477 0.760511 0.053927 11.00000 0.02613 0.02831 = 0.02278 -0.00330 0.00679 0.00337 C3 1 0.472164 0.757594 -0.003266 11.00000 0.02601 0.02404 = 0.02491 0.00095 0.00307 0.00105 AFIX 13 H3A 2 0.370405 0.847368 -0.004515 11.00000 -1.20000 AFIX 0 O5 4 0.760344 0.669295 0.093304 11.00000 0.04154 0.04414 = 0.02829 0.01252 -0.00117 -0.00284 O7 4 0.730798 0.583597 0.300695 11.00000 0.02446 0.02956 = 0.03377 0.00224 -0.00423 -0.00787 O8 4 0.709361 0.380584 0.351143 11.00000 0.03860 0.03237 = 0.03767 0.00946 -0.01389 -0.00089 O2 4 0.287985 0.664999 -0.163207 11.00000 0.03061 0.03240 = 0.02894 -0.00908 -0.00373 0.00246 C2 1 0.576946 0.745343 -0.064269 11.00000 0.01973 0.02098 = 0.02437 0.00040 0.00229 -0.00062 AFIX 13 H2 2 0.701883 0.825344 -0.066658 11.00000 -1.20000 AFIX 0 C5 1 0.613561 0.469155 0.308837 11.00000 0.02177 0.02330 = 0.02174 -0.00316 0.00342 0.00246 C1 1 0.329269 0.750695 -0.121062 11.00000 0.02087 0.02248 = 0.02351 0.00263 0.00296 -0.00222 C6 1 0.335385 0.434010 0.264384 11.00000 0.02283 0.02473 = 0.02421 0.00219 0.00215 -0.00520 AFIX 23 H6A 2 0.201904 0.407860 0.289342 11.00000 -1.20000 H6B 2 0.361597 0.352169 0.239362 11.00000 -1.20000 AFIX 0 N1 3 0.390776 0.587207 0.175412 11.00000 0.04379 0.02883 = 0.02845 0.00388 0.01241 0.00897 AFIX 137 H1A 2 0.384640 0.516160 0.148228 11.00000 -1.50000 H1B 2 0.566953 0.599890 0.196901 11.00000 -1.50000 H1C 2 0.328822 0.666067 0.154405 11.00000 -1.50000 AFIX 0 C7 1 0.210232 0.552972 0.220015 11.00000 0.02234 0.03111 = 0.02782 -0.00008 0.00182 0.00049 AFIX 23 H7A 2 0.025180 0.525300 0.196323 11.00000 -1.20000 H7B 2 0.189313 0.636608 0.244457 11.00000 -1.20000 AFIX 0 HKLF 4 REM RT_II_c in P2(1)/c REM wR2 = 0.0822, GooF = S = 1.017, Restrained GooF = 1.017 for all data REM R1 = 0.0402 for 1403 Fo > 4sig(Fo) and 0.0773 for all 1996 data REM 151 parameters refined using 0 restraints END WGHT 0.0360 0.0000 REM Highest difference peak 0.191, deepest hole -0.201, 1-sigma level 0.046 Q1 1 0.1776 0.8294 -0.0727 11.00000 0.05 0.19 Q2 1 -0.1601 0.8531 -0.1619 11.00000 0.05 0.18 Q3 1 0.5403 0.7469 -0.0337 11.00000 0.05 0.17 Q4 1 0.4218 0.5609 -0.0243 11.00000 0.05 0.17 Q5 1 0.8255 0.5912 0.0605 11.00000 0.05 0.17 Q6 1 0.8292 0.3929 0.3624 11.00000 0.05 0.17 Q7 1 0.4648 0.7520 -0.0898 11.00000 0.05 0.16 Q8 1 0.2275 0.5226 -0.0586 11.00000 0.05 0.16 Q9 1 0.0444 0.4658 0.1790 11.00000 0.05 0.15 Q10 1 0.2157 0.7093 0.2910 11.00000 0.05 0.15 Q11 1 0.1202 0.6075 -0.1440 11.00000 0.05 0.15 Q12 1 0.8132 0.4012 0.3907 11.00000 0.05 0.15 Q13 1 0.6300 0.6096 -0.0251 11.00000 0.05 0.15 Q14 1 0.7366 0.4974 0.2850 11.00000 0.05 0.14 Q15 1 0.2599 0.5365 -0.1192 11.00000 0.05 0.14 Q16 1 0.4692 0.6477 -0.1714 11.00000 0.05 0.14 Q17 1 0.2850 0.6620 -0.1183 11.00000 0.05 0.14 Q18 1 0.7482 0.6135 0.2851 11.00000 0.05 0.14 Q19 1 0.2934 0.6049 0.0505 11.00000 0.05 0.14 Q20 1 0.1722 0.6811 -0.2077 11.00000 0.05 0.14 ; _shelx_res_checksum 30690 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy O O4 0.2839(4) 0.64680(16) 0.00116(9) 0.0351(4) Uani d 1 H H4 0.368203 0.583378 0.023417 0.042 Uiso calc 1 O O3 0.7263(3) 0.61756(15) -0.06660(8) 0.0288(4) Uani d 1 H H3 0.891921 0.629047 -0.049121 0.035 Uiso calc 1 O O6 0.8729(4) 0.87280(16) 0.05263(8) 0.0374(5) Uani d 1 H H6 0.995540 0.876826 0.085286 0.045 Uiso calc 1 O O1 0.1745(4) 0.86172(17) -0.11777(8) 0.0402(5) Uani d 1 H H1 0.045136 0.865127 -0.149206 0.048 Uiso calc 1 C C4 0.7175(5) 0.7605(2) 0.05393(11) 0.0255(5) Uani d 1 C C3 0.4722(5) 0.7576(2) -0.00327(11) 0.0254(6) Uani d 1 H H3A 0.370405 0.847368 -0.004515 0.030 Uiso calc 1 O O5 0.7603(4) 0.66930(17) 0.09330(8) 0.0394(5) Uani d 1 O O7 0.7308(4) 0.58360(16) 0.30069(8) 0.0310(4) Uani d 1 O O8 0.7094(4) 0.38058(16) 0.35114(8) 0.0398(5) Uani d 1 O O2 0.2880(4) 0.66500(15) -0.16321(8) 0.0323(4) Uani d 1 C C2 0.5769(5) 0.7453(2) -0.06427(10) 0.0221(5) Uani d 1 H H2 0.701883 0.825344 -0.066658 0.027 Uiso calc 1 C C5 0.6136(5) 0.4692(2) 0.30884(10) 0.0225(5) Uani d 1 C C1 0.3293(5) 0.7507(2) -0.12106(11) 0.0226(5) Uani d 1 C C6 0.3354(5) 0.4340(2) 0.26438(11) 0.0244(5) Uani d 1 H H6A 0.201904 0.407860 0.289342 0.029 Uiso calc 1 H H6B 0.361597 0.352169 0.239362 0.029 Uiso calc 1 N N1 0.3908(5) 0.58721(19) 0.17541(9) 0.0330(5) Uani d 1 H H1A 0.384640 0.516160 0.148228 0.050 Uiso calc 1 H H1B 0.566953 0.599890 0.196901 0.050 Uiso calc 1 H H1C 0.328822 0.666067 0.154405 0.050 Uiso calc 1 C C7 0.2102(5) 0.5530(2) 0.22001(11) 0.0277(6) Uani d 1 H H7A 0.025180 0.525300 0.196323 0.033 Uiso calc 1 H H7B 0.189313 0.636608 0.244457 0.033 Uiso calc 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O4 0.0266(10) 0.0377(9) 0.0379(11) -0.0054(8) 0.0010(9) 0.0112(8) O3 0.0182(9) 0.0291(8) 0.0359(10) 0.0075(7) -0.0004(9) -0.0023(7) O6 0.0387(12) 0.0352(9) 0.0300(10) -0.0086(9) -0.0098(9) -0.0007(7) O1 0.0418(12) 0.0393(9) 0.0305(11) 0.0208(9) -0.0105(9) -0.0077(8) C4 0.0261(14) 0.0283(12) 0.0228(13) 0.0034(11) 0.0068(11) -0.0033(11) C3 0.0260(14) 0.0240(11) 0.0249(13) 0.0011(11) 0.0031(12) 0.0009(10) O5 0.0415(12) 0.0441(10) 0.0283(10) -0.0028(9) -0.0012(9) 0.0125(8) O7 0.0245(9) 0.0296(8) 0.0338(10) -0.0079(8) -0.0042(8) 0.0022(7) O8 0.0386(12) 0.0324(9) 0.0377(11) -0.0009(8) -0.0139(9) 0.0095(8) O2 0.0306(10) 0.0324(9) 0.0289(10) 0.0025(8) -0.0037(8) -0.0091(8) C2 0.0197(13) 0.0210(11) 0.0244(13) -0.0006(10) 0.0023(11) 0.0004(9) C5 0.0218(13) 0.0233(11) 0.0217(13) 0.0025(11) 0.0034(11) -0.0032(10) C1 0.0209(13) 0.0225(11) 0.0235(13) -0.0022(10) 0.0030(11) 0.0026(10) C6 0.0228(13) 0.0247(12) 0.0242(13) -0.0052(11) 0.0021(11) 0.0022(10) N1 0.0438(14) 0.0288(10) 0.0285(11) 0.0090(10) 0.0124(11) 0.0039(8) C7 0.0223(13) 0.0311(13) 0.0278(14) 0.0005(11) 0.0018(12) -0.0001(10) 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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 1 2 0.0320 2 2 -3 0.2800 -1 -1 -2 0.0240 -4 3 4 0.0100 4 -3 -4 0.0300 -2 -2 3 0.2270 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C3 O4 H4 109.5 C2 O3 H3 109.5 C4 O6 H6 109.5 C1 O1 H1 109.5 O6 C4 C3 110.58(19) O5 C4 O6 126.1(2) O5 C4 C3 123.3(2) O4 C3 C4 111.33(19) O4 C3 H3A 108.0 O4 C3 C2 110.75(18) C4 C3 H3A 108.0 C4 C3 C2 110.71(19) C2 C3 H3A 108.0 O3 C2 C3 111.80(18) O3 C2 H2 108.8 O3 C2 C1 108.72(18) C3 C2 H2 108.8 C1 C2 C3 109.87(18) C1 C2 H2 108.8 O7 C5 C6 118.10(19) O8 C5 O7 124.9(2) O8 C5 C6 117.02(19) O1 C1 C2 110.31(19) O2 C1 O1 125.6(2) O2 C1 C2 124.1(2) C5 C6 H6A 108.6 C5 C6 H6B 108.6 C5 C6 C7 114.71(18) H6A C6 H6B 107.6 C7 C6 H6A 108.6 C7 C6 H6B 108.6 H1A N1 H1B 109.5 H1A N1 H1C 109.5 H1B N1 H1C 109.5 C7 N1 H1A 109.5 C7 N1 H1B 109.5 C7 N1 H1C 109.5 C6 C7 H7A 109.4 C6 C7 H7B 109.4 N1 C7 C6 111.25(18) N1 C7 H7A 109.4 N1 C7 H7B 109.4 H7A C7 H7B 108.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O4 H4 0.8200 O4 C3 1.411(3) O3 H3 0.8200 O3 C2 1.417(2) O6 H6 0.8200 O6 C4 1.308(3) O1 H1 0.8200 O1 C1 1.304(3) C4 C3 1.520(3) C4 O5 1.199(3) C3 H3A 0.9800 C3 C2 1.530(3) O7 C5 1.254(3) O8 C5 1.253(2) O2 C1 1.205(3) C2 H2 0.9800 C2 C1 1.522(3) C5 C6 1.516(3) C6 H6A 0.9700 C6 H6B 0.9700 C6 C7 1.516(3) N1 H1A 0.8900 N1 H1B 0.8900 N1 H1C 0.8900 N1 C7 1.487(3) C7 H7A 0.9700 C7 H7B 0.9700 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O4 H4 O3 3_665 0.82 2.21 2.879(2) 138.7 yes O3 H3 O4 1_655 0.82 1.99 2.803(2) 173.9 yes O6 H6 O8 2_755 0.82 1.76 2.573(2) 172.3 yes O1 H1 O7 4_475 0.82 1.74 2.524(2) 159.8 yes N1 H1A O2 3_665 0.89 2.31 2.897(2) 123.0 yes N1 H1B O7 . 0.89 2.22 2.852(2) 127.4 yes N1 H1C O8 2_655 0.89 2.04 2.849(2) 151.5 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 O4 C3 C2 O3 -61.7(2) O4 C3 C2 C1 59.1(2) O3 C2 C1 O1 175.04(19) O3 C2 C1 O2 -6.2(3) O6 C4 C3 O4 -172.90(19) O6 C4 C3 C2 63.4(2) C4 C3 C2 O3 62.3(2) C4 C3 C2 C1 -176.93(17) C3 C2 C1 O1 52.4(2) C3 C2 C1 O2 -128.8(2) O5 C4 C3 O4 8.6(3) O5 C4 C3 C2 -115.1(3) O7 C5 C6 C7 -8.1(3) O8 C5 C6 C7 172.1(2) C5 C6 C7 N1 64.7(3) loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.7730(12) 2 0.2270(12) _cod_database_fobs_code 2021508