#------------------------------------------------------------------------------ #$Date: 2024-12-07 19:02:42 +0200 (Sat, 07 Dec 2024) $ #$Revision: 296755 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312701.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_2312701 loop_ _publ_author_name 'Kanagavel, Manimurugan' 'Balasubramanian, Sridhar' 'Nechipadappu, Sunil Kumar' _publ_section_title ; Variable stoichiometry and a salt-cocrystal intermediate in multicomponent systems of flucytosine: structural elucidation and their impact on stability. ; _journal_coeditor_code YH5039 _journal_issue 6 _journal_name_full 'Acta crystallographica Section B, Structural science, crystal engineering and materials' _journal_page_first 793 _journal_page_last 806 _journal_paper_doi 10.1107/S2052520624010278 _journal_volume 80 _journal_year 2024 _chemical_formula_moiety 'C7 H3.50 Cl N O4, C4 H4.50 F N3 O' _chemical_formula_sum 'C11 H8 Cl F N4 O5' _chemical_formula_weight 330.66 _space_group_crystal_system monoclinic _space_group_IT_number 13 _space_group_name_Hall '-P 2yac' _space_group_name_H-M_alt 'P 1 2/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary difmap _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2019/3 _cell_angle_alpha 90 _cell_angle_beta 96.781(15) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.632(6) _cell_length_b 8.420(6) _cell_length_c 16.959(12) _cell_measurement_reflns_used 8674 _cell_measurement_temperature 294(2) _cell_measurement_theta_max 29.4 _cell_measurement_theta_min 2.41 _cell_volume 1365.8(16) _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL2014 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 294(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON-III' _diffrn_measurement_method '\w and \f' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_unetI/netI 0.0570 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 18052 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.593 _diffrn_reflns_theta_min 2.419 _exptl_absorpt_coefficient_mu 0.323 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.5647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_density_diffrn 1.608 _exptl_crystal_description block _exptl_crystal_F_000 672 _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.130 _refine_diff_density_max 0.310 _refine_diff_density_min -0.255 _refine_diff_density_rms 0.058 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 227 _refine_ls_number_reflns 4156 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.1100 _refine_ls_R_factor_gt 0.0771 _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^)+(0.0753P)^2^+1.5660P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2145 _refine_ls_wR_factor_ref 0.2313 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2630 _reflns_number_total 4156 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file yh5039sup1.cif _cod_data_source_block FCY-CNB _cod_depositor_comments 'Adding full bibliography for 2312700--2312704.cif.' _cod_original_cell_volume 1365.7(16) _cod_original_sg_symbol_H-M 'P 2/n' _cod_database_code 2312701 _cod_database_fobs_code 2312701 _shelx_shelxl_version_number 2019/3 _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 0.950 _shelx_estimated_absorpt_t_max 0.959 _shelx_res_file ; CELL 0.71073 9.6316 8.4201 16.9588 90.000 96.781 90.000 ZERR 4.00 0.0061 0.0057 0.0119 0.000 0.015 0.000 LATT 1 SYMM -x+1/2, y, -z+1/2 SFAC C H N O CL F UNIT 44 32 16 20 4 4 LIST 4! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP 21.000 OMIT 2 2 0 OMIT 1 1 0 OMIT 3 2 1 OMIT 4 2 2 OMIT 0 4 3 SIZE 0.16 0.14 0.13 DFIX 0.90 0.02 N3 H3N N3 H4N L.S. 10 ACTA FMAP 2 PLAN 5 EQIV $1 -x+2, -y+1, -z+1 HTAB N2 N2_$1 EQIV $2 -x+2, -y+2, -z+1 HTAB N1 O1_$2 HTAB N3 O2 HTAB N3 O1_$1 EQIV $3 -x+3/2, y, -z+1/2 HTAB O3 O3_$3 HTAB BOND $H CONF WGHT 0.075300 1.566000 FVAR 0.81835 0.67199 MOLE 1 C1 1 0.949789 0.769403 0.472449 11.00000 0.05003 0.02930 = 0.04481 -0.00131 -0.00137 -0.00310 C2 1 0.808267 0.570328 0.404140 11.00000 0.04508 0.03626 = 0.04363 0.00111 -0.00341 -0.00030 C3 1 0.727921 0.693270 0.363737 11.00000 0.04758 0.04681 = 0.05842 0.00678 -0.01294 -0.00262 C4 1 0.756958 0.844286 0.379134 11.00000 0.05313 0.03651 = 0.06864 0.01263 -0.00975 0.00321 AFIX 43 H4 2 0.702825 0.923909 0.352869 11.00000 -1.20000 AFIX 0 F1 6 0.620654 0.649523 0.310114 11.00000 0.07313 0.06044 = 0.10085 0.00915 -0.04849 -0.00589 N2 3 0.916534 0.614753 0.456969 11.00000 0.04905 0.02620 = 0.04398 -0.00142 -0.00835 -0.00055 H2N 2 0.959878 0.517628 0.480738 10.50000 0.08572 N1 3 0.866373 0.881832 0.433562 11.00000 0.06049 0.02786 = 0.06521 0.00346 -0.00791 0.00092 H1N 2 0.874434 0.972468 0.446975 11.00000 0.07519 N3 3 0.780310 0.420484 0.391696 11.00000 0.05845 0.03610 = 0.06458 -0.00488 -0.02194 -0.00360 H3N 2 0.712792 0.388371 0.355911 11.00000 -1.50000 H4N 2 0.841607 0.353488 0.415283 11.00000 -1.50000 O1 4 1.051288 0.806673 0.519990 11.00000 0.06804 0.02901 = 0.06288 -0.00347 -0.02134 -0.00337 MOLE 2 C5 1 0.543224 0.213346 0.232537 11.00000 0.04617 0.06074 = 0.04962 -0.00294 -0.00347 -0.01274 C6 1 0.401866 0.205887 0.183691 11.00000 0.04022 0.06646 = 0.04812 -0.00698 0.00004 -0.01006 C7 1 0.335416 0.063324 0.163734 11.00000 0.04828 0.05642 = 0.05450 -0.00799 -0.00185 -0.00552 PART 2 AFIX 43 H7D 2 0.378844 -0.031804 0.179937 -21.00000 -1.20000 AFIX 0 PART 0 C8 1 0.203954 0.061151 0.119556 11.00000 0.04902 0.07736 = 0.06451 -0.01489 -0.00124 -0.01625 AFIX 43 H8 2 0.156739 -0.033892 0.107939 11.00000 -1.20000 AFIX 0 C9 1 0.146366 0.203653 0.093737 11.00000 0.04046 0.08826 = 0.05428 -0.00512 -0.00063 -0.00181 C10 1 0.208325 0.345417 0.111415 11.00000 0.06025 0.07438 = 0.06257 0.00759 0.00321 0.00550 AFIX 43 H10 2 0.166232 0.439753 0.092784 11.00000 -1.20000 AFIX 0 C11 1 0.336559 0.345810 0.158180 11.00000 0.05846 0.06283 = 0.06043 -0.00541 0.00292 -0.01086 PART 1 AFIX 43 H11 2 0.379399 0.442178 0.172639 21.00000 -1.20000 AFIX 0 PART 0 N4 3 0.007326 0.203297 0.045673 11.00000 0.04898 0.11336 = 0.07329 -0.01185 -0.00456 0.00531 O2 4 0.560128 0.309338 0.286042 11.00000 0.05237 0.10276 = 0.08191 -0.04118 -0.00807 -0.01158 O3 4 0.633924 0.120238 0.211755 11.00000 0.05218 0.06914 = 0.07486 -0.01753 -0.01752 0.00597 H3O 2 0.709221 0.145697 0.235364 10.50000 0.04106 O4 4 -0.071172 0.092200 0.056507 11.00000 0.05045 0.15716 = 0.11898 -0.02639 -0.00960 -0.02204 O5 4 -0.020382 0.308749 -0.001044 11.00000 0.08695 0.16549 = 0.10466 0.03036 -0.03049 0.01498 PART 1 CL1 5 0.398611 -0.120516 0.199502 21.00000 0.06270 0.05206 = 0.08834 0.00292 0.00163 -0.00021 PART 2 CL1D 5 0.376298 0.543964 0.184131 -21.00000 0.08346 0.08185 = 0.10744 0.00611 -0.00402 -0.02718 PART 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM REM wR2 = 0.2313, GooF = S = 1.053, Restrained GooF = 1.053 for all data REM R1 = 0.0771 for 2630 Fo > 4sig(Fo) and 0.1100 for all 4156 data REM 227 parameters refined using 2 restraints END WGHT 0.0753 1.5660 REM Instructions for potential hydrogen bonds EQIV $4 -x+1/2, y+1, -z+1/2 HTAB C4 O4_$4 HTAB N2 N2_$1 HTAB N1 O1_$2 HTAB N3 O2 HTAB N3 O1_$1 HTAB O3 O3_$3 REM Highest difference peak 0.310, deepest hole -0.255, 1-sigma level 0.058 Q1 1 0.9273 0.6942 0.4663 11.00000 0.05 0.31 Q2 1 0.7423 0.6276 0.3928 11.00000 0.05 0.25 Q3 1 0.5918 0.2063 0.2991 11.00000 0.05 0.25 Q4 1 0.3224 -0.1912 0.2232 11.00000 0.05 0.25 Q5 1 0.6000 0.3475 0.2482 11.00000 0.05 0.22 ; _shelx_res_checksum 13049 _shelx_hkl_file ; -1 0 0 1.88 0.41 -1 0 0 2.73 0.38 -2 0 0 515.57 39.93 -2 0 0 524.31 39.89 -2 0 0 515.38 39.98 2 0 0 513.54 39.87 2 0 0 505.66 40.20 2 0 0 466.50 40.07 -3 0 0 2.82 0.68 3 0 0 1.21 0.36 -3 0 0 0.96 0.45 3 0 0 2.35 0.87 -3 0 0 1.50 0.42 -3 0 0 1.63 0.84 3 0 0 0.72 0.84 -3 0 0 1.36 0.44 4 0 0 1218.27 101.13 4 0 0 1343.94 100.44 -4 0 0 1296.81 100.61 -4 0 0 1285.87 100.54 -4 0 0 1262.18 100.53 4 0 0 1310.84 100.82 -4 0 0 1208.21 100.65 -4 0 0 1297.24 101.04 5 0 0 10.29 2.03 -5 0 0 11.01 2.03 -5 0 0 9.28 1.26 -5 0 0 7.83 1.21 5 0 0 9.67 1.07 -5 0 0 9.33 1.37 5 0 0 8.17 2.10 -6 0 0 256.82 21.36 6 0 0 231.41 22.25 -6 0 0 282.46 21.49 -6 0 0 273.66 22.10 6 0 0 282.42 21.87 -6 0 0 278.04 21.39 -7 0 0 0.86 0.81 -7 0 0 0.97 0.88 -7 0 0 1.35 1.05 7 0 0 2.68 1.78 -7 0 0 3.25 1.76 8 0 0 7.35 2.48 -8 0 0 7.05 1.47 -8 0 0 7.59 1.46 -8 0 0 4.54 1.53 -9 0 0 -0.84 1.31 9 0 0 1.82 2.14 10 0 0 1.43 2.35 -10 0 0 -0.97 1.26 11 0 0 1.45 2.47 -11 0 0 1.60 1.47 -12 0 0 4.49 1.81 -13 0 0 2.96 1.95 0 1 0 423.21 31.15 0 1 0 367.73 31.17 1 1 0 -0.02 0.33 -2 -1 0 593.52 46.32 -2 -1 0 573.77 46.32 -2 -1 0 643.70 46.46 -2 -1 0 557.55 46.33 2 1 0 590.63 46.32 2 1 0 574.74 46.32 2 1 0 584.18 46.33 2 1 0 589.32 46.72 3 1 0 1813.47 143.09 -4 -1 0 448.48 37.34 -4 -1 0 434.11 37.36 4 -1 0 525.38 37.57 4 -1 0 514.27 37.93 -4 -1 0 461.24 37.53 -4 -1 0 456.88 37.37 -4 -1 0 478.20 37.96 -4 1 0 519.14 37.35 4 1 0 451.98 38.07 4 1 0 504.79 37.74 4 1 0 445.43 37.30 4 1 0 438.73 37.37 -5 -1 0 799.02 67.04 -5 -1 0 869.37 67.07 5 -1 0 847.39 67.71 -5 -1 0 832.15 67.71 -5 -1 0 853.50 67.02 5 -1 0 905.27 67.31 5 1 0 765.63 67.84 5 1 0 834.53 67.44 -5 1 0 940.40 67.05 -6 -1 0 14.49 1.70 -6 -1 0 13.47 1.62 -6 -1 0 18.47 2.72 -6 -1 0 11.91 1.53 6 -1 0 12.30 2.28 -6 1 0 8.65 1.54 6 1 0 16.96 2.63 6 1 0 18.34 3.04 -7 -1 0 78.55 6.23 -7 -1 0 83.84 6.29 7 -1 0 58.53 6.54 -7 -1 0 86.69 6.17 -7 1 0 63.95 6.15 -7 1 0 60.99 6.10 7 1 0 87.07 7.10 -7 1 0 62.84 6.23 8 -1 0 12.97 2.80 -8 -1 0 9.95 1.74 -8 -1 0 7.06 1.69 -8 -1 0 8.89 1.64 -8 -1 0 10.12 2.97 8 1 0 13.39 3.18 -8 1 0 10.36 1.81 -8 1 0 12.05 1.87 -8 1 0 16.58 2.38 -9 -1 0 0.74 1.39 9 -1 0 5.80 2.38 9 1 0 2.71 2.40 -9 1 0 5.20 1.53 -9 1 0 5.71 1.79 10 -1 0 8.00 2.69 -10 -1 0 12.25 2.29 -10 1 0 10.11 2.40 10 1 0 9.69 3.30 -11 -1 0 2.97 1.77 11 1 0 4.24 2.78 -11 1 0 2.94 1.69 -12 -1 0 3.79 2.00 12 1 0 0.66 2.64 -12 1 0 2.93 1.72 -13 -1 0 3.65 2.15 -13 1 0 3.81 1.99 1 -2 0 1057.88 75.04 -1 -2 0 900.70 74.91 -1 -2 0 917.17 74.93 -1 -2 0 901.26 74.94 -1 2 0 1038.19 74.92 1 2 0 927.85 74.99 1 2 0 846.72 74.90 -1 2 0 1080.65 75.05 1 2 0 897.58 74.94 2 2 0 -0.07 0.66 3 -2 0 3156.53 259.89 3 2 0 3463.32 260.66 -4 -2 0 477.55 35.12 4 -2 0 403.43 35.08 -4 -2 0 474.73 35.12 -4 -2 0 436.79 35.76 -4 -2 0 438.52 35.15 4 -2 0 392.55 35.39 4 2 0 469.84 35.54 4 2 0 474.40 35.12 4 2 0 434.82 35.10 4 2 0 455.54 35.09 4 2 0 453.03 35.97 -4 2 0 413.19 35.06 -5 -2 0 30.39 2.84 -5 -2 0 35.35 2.87 -5 -2 0 28.97 3.83 -5 -2 0 33.00 2.80 5 2 0 23.91 3.80 5 2 0 27.63 2.77 5 2 0 29.53 3.52 5 2 0 29.11 2.70 5 2 0 29.58 2.73 -6 -2 0 24.73 2.57 -6 -2 0 23.44 3.50 -6 -2 0 26.46 2.51 -6 -2 0 31.70 2.66 6 2 0 24.66 2.38 6 2 0 21.95 2.47 6 2 0 22.98 3.28 6 2 0 26.13 2.38 -7 -2 0 111.05 9.49 7 -2 0 92.74 8.37 -7 -2 0 84.34 8.08 -7 -2 0 96.65 8.14 -7 -2 0 94.54 8.01 7 -2 0 87.63 9.05 -7 2 0 95.34 8.08 7 2 0 104.75 9.05 -7 2 0 97.19 8.33 7 2 0 105.63 7.89 -8 -2 0 4.53 1.28 -8 -2 0 2.09 1.43 -8 -2 0 2.19 2.45 -8 -2 0 7.59 2.25 8 -2 0 4.70 1.96 8 2 0 5.54 2.78 -8 2 0 8.99 2.92 -8 2 0 5.48 2.15 -9 -2 0 100.28 9.58 -9 -2 0 88.02 8.06 9 -2 0 88.94 8.59 -9 2 0 95.78 8.10 -9 2 0 99.16 8.24 9 2 0 84.35 9.16 -10 -2 0 44.64 4.38 -10 2 0 35.33 4.38 10 2 0 44.64 5.71 -11 -2 0 3.81 1.80 -11 2 0 4.69 2.07 11 2 0 7.22 3.35 -12 -2 0 -0.14 1.74 12 2 0 -0.43 2.75 -12 2 0 2.08 1.79 -13 -2 0 -1.52 1.89 13 2 0 1.05 3.30 -13 2 0 -0.10 1.75 0 -3 0 310.78 24.61 0 -3 0 309.53 24.58 0 3 0 304.97 24.59 0 3 0 300.79 24.49 0 3 0 305.80 24.51 0 3 0 318.74 24.51 1 -3 0 5.37 1.16 -1 -3 0 7.64 1.41 -1 -3 0 7.68 1.23 -1 -3 0 6.72 1.04 1 3 0 6.12 1.12 1 3 0 7.24 1.35 -1 3 0 6.59 0.91 -1 3 0 6.28 1.04 1 3 0 6.71 1.08 -1 3 0 4.40 1.04 -2 -3 0 501.92 37.84 -2 -3 0 462.19 37.39 -2 -3 0 506.92 37.47 -2 3 0 412.22 37.49 2 3 0 465.27 37.40 2 3 0 454.23 37.27 2 3 0 511.10 37.63 2 3 0 466.53 37.43 -3 -3 0 93.31 9.32 -3 -3 0 112.16 8.84 -3 -3 0 110.69 8.81 3 -3 0 125.99 8.85 3 3 0 93.16 9.42 3 3 0 112.42 8.83 3 3 0 103.30 8.79 3 3 0 99.90 9.11 3 3 0 106.22 8.68 -4 -3 0 147.02 11.32 4 -3 0 149.37 11.53 -4 -3 0 139.76 11.32 -4 -3 0 126.35 11.94 -4 -3 0 149.91 11.23 4 3 0 139.66 11.30 4 3 0 132.13 11.72 -4 3 0 157.10 11.28 4 3 0 115.90 12.00 4 3 0 127.71 11.20 4 3 0 133.73 11.27 -5 -3 0 4.40 1.15 -5 -3 0 6.67 2.07 -5 -3 0 4.58 1.17 -5 -3 0 2.08 0.90 5 3 0 3.77 1.04 5 3 0 4.53 1.08 5 3 0 5.16 1.07 -5 3 0 5.47 1.41 5 3 0 2.44 1.89 5 3 0 6.23 1.94 6 -3 0 32.11 4.03 6 -3 0 36.67 3.19 -6 -3 0 38.45 4.48 -6 -3 0 30.99 3.33 -6 -3 0 35.48 3.29 -6 -3 0 33.90 3.29 -6 3 0 34.72 3.27 6 3 0 32.24 3.17 6 3 0 36.11 3.23 6 3 0 33.40 4.16 -6 3 0 36.54 3.65 7 -3 0 280.02 25.57 -7 -3 0 325.56 24.81 -7 -3 0 315.74 26.01 -7 -3 0 325.50 24.78 -7 -3 0 291.64 25.10 7 -3 0 302.00 24.76 7 3 0 296.63 25.67 7 3 0 314.17 24.59 -7 3 0 323.48 25.11 -7 3 0 314.00 24.78 -8 -3 0 62.04 5.62 -8 -3 0 64.84 7.30 -8 -3 0 60.44 5.51 8 3 0 60.70 6.87 -9 -3 0 14.50 2.39 -9 -3 0 8.88 3.13 9 3 0 6.88 3.02 -10 -3 0 3.81 1.62 10 3 0 0.71 2.82 -11 -3 0 2.01 1.61 11 3 0 1.20 3.08 -11 3 0 3.31 1.89 -12 -3 0 -0.94 1.61 12 3 0 -0.51 2.86 -12 3 0 2.39 2.11 -13 -3 0 0.90 1.91 -13 3 0 2.21 2.08 13 3 0 1.20 3.14 0 4 0 4408.45 346.60 1 -4 0 424.69 39.93 -1 -4 0 570.40 40.04 -1 -4 0 508.48 39.84 -1 -4 0 549.09 40.15 1 4 0 498.95 39.84 1 4 0 523.67 39.95 -1 4 0 437.19 39.93 -1 4 0 468.18 39.82 1 4 0 543.53 39.86 -2 -4 0 555.47 40.17 -2 -4 0 502.13 40.04 -2 -4 0 526.28 40.49 2 4 0 523.16 40.13 2 4 0 501.67 40.05 2 4 0 567.42 40.36 -2 4 0 423.29 39.75 -2 4 0 445.53 40.17 -3 -4 0 446.06 31.24 -3 -4 0 384.90 31.14 3 4 0 406.59 31.18 3 4 0 400.70 31.19 -3 4 0 328.34 31.27 3 4 0 378.57 30.98 -4 -4 0 936.27 75.27 -4 -4 0 972.60 75.97 -4 -4 0 1059.66 75.36 4 -4 0 932.57 74.89 4 -4 0 865.95 75.24 4 4 0 959.99 76.19 -4 4 0 969.51 75.53 4 4 0 915.90 75.13 4 4 0 996.15 75.76 4 4 0 965.03 75.27 4 4 0 913.61 75.25 -4 4 0 950.06 75.22 -5 -4 0 35.33 3.51 -5 -4 0 43.35 4.72 -5 -4 0 31.44 3.41 5 4 0 35.37 3.50 5 4 0 34.92 3.45 5 4 0 31.83 3.39 5 4 0 43.78 4.38 -6 -4 0 81.34 6.67 -6 -4 0 76.03 7.94 -6 -4 0 78.21 6.78 6 4 0 73.35 6.72 -6 4 0 94.13 7.30 6 4 0 75.34 6.62 6 4 0 75.98 6.69 6 4 0 72.06 7.72 -7 -4 0 17.37 2.40 -7 -4 0 20.37 3.84 -7 -4 0 15.66 2.27 7 4 0 14.55 2.21 7 4 0 12.80 3.66 -8 -4 0 34.21 4.03 -8 -4 0 48.98 6.24 8 4 0 45.84 5.71 -9 -4 0 8.57 2.04 -9 -4 0 11.92 3.85 9 4 0 8.03 3.14 -10 -4 0 17.39 2.62 10 4 0 13.38 4.01 -11 -4 0 1.24 1.64 11 4 0 2.75 3.54 -12 -4 0 -0.15 1.79 -12 4 0 3.36 2.17 12 4 0 4.15 3.75 0 -5 0 9.54 1.79 0 -5 0 15.17 2.20 0 5 0 18.71 2.13 0 5 0 12.09 2.02 0 5 0 14.49 1.79 -1 -5 0 98.03 9.19 -1 -5 0 117.29 9.23 1 -5 0 107.26 9.25 1 -5 0 94.62 8.79 -1 5 0 118.44 9.06 -1 5 0 93.95 8.87 1 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3 1.61 2.13 -12 -3 3 -0.51 1.69 12 3 -3 0.50 3.18 -12 3 3 0.77 1.86 -11 -3 3 0.03 1.58 -11 3 3 -0.37 1.66 11 3 -3 0.42 3.01 -10 -3 3 7.43 2.00 -10 3 3 13.93 2.61 10 3 -3 5.04 2.94 -10 3 3 7.81 2.32 -9 -3 3 229.53 19.13 -9 -3 3 237.11 19.02 -8 -3 3 272.40 23.03 -8 -3 3 279.71 22.87 8 -3 -3 299.39 22.82 8 3 -3 289.16 22.84 8 3 -3 277.24 23.74 7 -3 -3 4.85 3.08 -7 -3 3 8.59 1.77 -7 -3 3 8.12 1.59 7 -3 -3 4.39 1.69 7 3 -3 6.22 1.49 7 3 -3 6.74 1.56 7 3 -3 0.25 2.29 6 -3 -3 564.71 46.84 -6 -3 3 605.19 46.92 6 -3 -3 595.60 46.94 6 -3 -3 538.92 47.41 -6 -3 3 634.06 47.16 -6 3 3 597.36 47.25 6 3 -3 614.33 47.04 6 3 -3 588.10 47.06 5 -3 -3 630.02 47.08 -5 -3 3 537.76 47.16 -5 -3 3 611.73 47.25 -5 -3 3 610.44 47.02 5 -3 -3 615.52 46.90 5 3 -3 574.58 47.02 -5 3 3 595.79 47.13 5 3 -3 623.10 47.48 5 3 -3 593.88 47.18 5 3 -3 546.51 47.90 5 3 -3 595.73 47.21 -4 -3 3 853.17 65.51 4 -3 -3 860.78 65.37 -4 -3 3 840.19 65.26 -4 -3 3 786.51 65.44 4 3 -3 852.29 65.48 4 3 -3 812.00 65.47 4 3 -3 809.04 65.28 4 3 -3 862.82 65.63 -4 3 3 802.41 65.37 4 3 -3 796.80 66.01 3 -3 -3 695.62 52.88 -3 -3 3 683.76 53.22 3 -3 -3 689.99 53.09 -3 -3 3 655.22 53.15 3 3 -3 649.61 52.97 3 3 -3 676.65 53.18 3 3 -3 666.26 53.56 -3 3 3 672.06 53.09 3 3 -3 654.55 53.19 -2 -3 3 1827.32 134.32 -2 -3 3 1664.46 134.19 2 -3 -3 1625.57 134.04 2 3 -3 1685.42 134.02 2 3 -3 1678.69 134.26 2 3 -3 1689.42 134.43 2 3 -3 1762.93 134.24 -1 -3 3 10.48 1.50 1 -3 -3 6.40 1.16 1 -3 -3 7.77 1.28 -1 -3 3 6.96 1.22 1 3 -3 9.45 1.34 -1 3 3 6.24 1.10 1 3 -3 6.95 1.24 -1 3 3 7.09 1.20 1 3 -3 8.35 1.32 0 -3 -3 214.11 18.24 0 -3 3 219.79 18.11 0 -3 3 246.41 18.35 0 -3 -3 225.46 18.16 0 3 3 222.08 18.24 0 3 -3 219.22 18.15 0 3 3 230.70 18.13 0 3 3 235.38 18.29 0 3 -3 240.81 18.07 0 3 -3 217.73 18.26 -1 -3 -3 2014.13 160.67 1 -3 3 2128.28 160.64 1 3 3 1958.27 160.43 1 3 3 2165.73 160.77 -1 3 -3 1998.11 160.61 -1 3 -3 1994.97 160.46 1 3 3 2024.30 160.51 -2 -3 -3 1289.84 109.09 2 -3 3 1548.46 109.34 -2 -3 -3 1384.03 109.11 -2 -3 -3 1277.56 109.36 2 -3 3 1502.89 108.98 -2 3 -3 1493.18 108.98 -2 3 -3 1389.16 109.25 2 3 3 1327.62 109.04 2 3 3 1383.66 109.02 2 3 3 1372.74 109.51 2 3 3 1334.43 109.07 2 3 3 1328.77 109.10 3 -3 3 255.65 19.77 -3 -3 -3 225.45 20.25 -3 -3 -3 248.24 20.89 -3 -3 -3 256.53 19.96 3 -3 3 252.33 20.13 3 3 3 254.89 19.90 3 3 3 243.47 19.83 3 3 3 245.43 20.49 -3 3 -3 262.41 19.97 -3 3 -3 257.48 19.93 3 3 3 234.29 19.86 3 3 3 251.70 19.90 -3 3 -3 257.31 20.13 -4 -3 -3 4.06 2.08 -4 -3 -3 6.64 1.06 4 -3 3 8.64 0.85 -4 -3 -3 4.42 1.52 -4 -3 -3 6.51 1.02 -4 -3 -3 6.78 1.16 4 3 3 5.52 0.95 4 3 3 5.32 1.97 4 3 3 5.60 1.00 4 3 3 6.82 0.98 4 3 3 5.99 1.02 -5 -3 -3 167.29 14.23 -5 -3 -3 187.84 13.66 -5 -3 -3 180.28 15.11 -5 -3 -3 165.80 13.76 -5 -3 -3 168.38 13.74 5 3 3 184.48 13.53 5 3 3 179.17 14.64 -5 3 -3 154.82 13.68 -5 3 -3 161.13 13.94 -5 3 -3 167.90 14.07 -5 3 -3 161.50 13.80 5 3 3 173.63 13.63 5 3 3 164.93 13.76 -6 -3 -3 13.88 3.12 -6 -3 -3 7.34 1.33 -6 -3 -3 6.71 1.30 -6 3 -3 3.42 1.11 6 3 3 9.43 2.89 6 3 3 6.96 0.97 -6 3 -3 2.59 1.30 -6 3 -3 4.60 1.35 7 -3 3 133.87 10.99 -7 -3 -3 144.33 12.83 -7 -3 -3 134.52 10.98 -7 -3 -3 121.92 11.00 -7 3 -3 127.76 11.10 7 3 3 140.07 12.19 -8 -3 -3 30.39 3.30 -8 -3 -3 29.66 5.15 8 3 3 31.24 4.70 -9 -3 -3 88.56 7.81 -9 -3 -3 99.94 9.99 9 3 3 81.94 8.97 -10 -3 -3 2.83 1.51 -10 -3 -3 4.85 3.46 10 3 3 0.10 2.59 -10 3 -3 1.68 1.56 -11 -3 -3 6.44 2.01 -11 -3 -3 3.89 4.17 -11 3 -3 7.42 2.18 11 3 3 6.26 3.52 -12 -3 -3 9.58 2.45 12 3 3 4.01 3.62 -12 3 -3 10.68 2.56 -13 -4 3 -0.01 1.78 -13 4 3 0.86 2.12 -12 -4 3 2.76 1.85 -12 4 3 -1.01 1.85 12 4 -3 -0.75 3.48 -11 -4 3 -1.45 1.47 11 4 -3 0.29 3.24 -10 -4 3 34.78 3.96 10 4 -3 35.97 5.66 -9 -4 3 3.72 1.58 9 4 -3 1.65 2.56 -8 -4 3 218.39 18.53 -8 -4 3 209.64 18.32 8 4 -3 248.53 18.46 -7 -4 3 14.27 2.06 7 -4 -3 14.71 2.45 -7 -4 3 12.29 2.19 7 4 -3 11.98 2.15 7 4 -3 5.98 3.12 6 -4 -3 10.61 2.48 -6 -4 3 18.08 2.08 -6 -4 3 19.44 2.40 6 -4 -3 14.00 2.43 6 4 -3 16.99 2.35 6 4 -3 19.11 2.49 6 4 -3 11.65 3.26 -5 -4 3 33.52 3.57 5 -4 -3 42.34 3.60 5 4 -3 32.45 3.60 5 4 -3 31.36 4.51 5 4 -3 27.97 3.42 5 4 -3 32.07 3.48 5 4 -3 40.17 4.04 -4 -4 3 72.92 5.91 -4 -4 3 59.83 5.67 4 4 -3 63.42 5.83 4 4 -3 73.06 6.66 4 4 -3 65.07 5.77 4 4 -3 58.84 5.46 -3 -4 3 190.63 14.91 3 -4 -3 160.82 14.79 -3 4 3 161.81 15.01 -3 4 3 162.55 14.77 3 4 -3 224.12 15.63 3 4 -3 175.89 14.64 3 4 -3 196.57 14.97 3 4 -3 197.88 15.00 -2 -4 3 25.36 2.61 2 -4 -3 21.28 2.64 -2 -4 3 30.94 2.94 2 4 -3 29.10 2.86 2 4 -3 29.86 2.81 2 4 -3 23.52 3.04 -2 4 3 20.78 2.73 1 -4 -3 65.92 5.99 -1 -4 3 77.84 6.11 1 -4 -3 68.91 6.12 -1 4 3 67.71 6.02 -1 4 3 65.37 6.02 -1 4 3 65.50 6.18 1 4 -3 81.05 6.20 1 4 -3 73.23 6.26 1 4 -3 76.28 6.25 0 -4 -3 31.10 2.87 0 -4 -3 27.97 2.81 0 4 3 29.65 2.70 0 4 3 26.10 2.67 0 4 -3 21.03 2.69 0 4 3 26.73 2.93 0 4 3 29.52 2.84 1 -4 3 460.58 34.41 -1 -4 -3 421.97 34.31 1 4 3 444.82 34.14 1 4 3 402.24 34.13 1 4 3 399.04 34.20 -1 4 -3 424.11 34.33 -1 4 -3 434.04 34.17 1 4 3 455.20 34.51 -2 -4 -3 117.77 9.41 -2 -4 -3 109.24 9.62 -2 -4 -3 106.66 10.20 2 4 3 112.95 9.89 2 4 3 104.95 9.40 2 4 3 112.17 9.34 2 4 3 130.18 9.26 2 4 3 114.56 9.38 3 -4 3 78.72 5.87 -3 -4 -3 68.39 6.17 3 -4 3 82.85 6.49 -3 -4 -3 65.93 6.41 -3 -4 -3 69.34 7.21 -3 -4 -3 67.83 6.11 3 4 3 67.66 6.01 3 4 3 67.93 5.95 3 4 3 68.18 6.08 -3 4 -3 78.24 5.95 3 4 3 69.61 6.09 -3 4 -3 78.21 6.42 3 4 3 70.22 6.75 -4 -4 -3 131.85 10.80 -4 -4 -3 139.76 11.76 -4 -4 -3 135.20 10.36 -4 -4 -3 113.20 10.32 4 4 3 123.75 10.30 4 4 3 132.75 10.24 4 4 3 113.87 10.23 4 4 3 114.75 10.26 4 4 3 138.91 11.21 -5 -4 -3 49.26 4.28 -5 -4 -3 48.18 5.95 -5 -4 -3 43.47 4.33 5 4 3 51.31 4.28 5 4 3 42.20 5.25 5 4 3 48.51 4.15 5 4 3 51.31 4.28 -6 -4 -3 79.68 8.12 -6 -4 -3 67.24 6.13 -6 -4 -3 70.68 6.07 -6 -4 -3 73.83 6.01 -6 4 -3 57.14 6.35 6 4 3 74.77 7.46 6 4 3 71.84 5.83 -7 -4 -3 72.77 6.12 -7 -4 -3 71.26 8.14 -7 4 -3 72.64 6.91 7 4 3 58.35 7.27 -8 -4 -3 8.92 1.81 -8 -4 -3 7.43 3.54 8 4 3 4.15 2.96 -9 -4 -3 16.44 2.54 -9 -4 -3 21.15 4.78 9 4 3 17.97 4.17 -10 -4 -3 1.54 1.49 -10 -4 -3 0.17 3.43 10 4 3 2.08 3.04 -11 -4 -3 3.71 1.78 -11 -4 -3 3.71 3.75 11 4 3 1.84 3.40 -11 4 -3 3.73 2.05 -12 -4 -3 4.27 1.96 -12 -4 -3 7.98 4.72 12 4 3 6.40 3.94 -12 4 -3 6.87 2.33 12 5 -3 -3.12 3.46 11 5 -3 0.08 3.41 10 5 -3 0.24 3.28 9 5 -3 49.99 6.52 -8 -5 3 59.83 5.72 8 5 -3 59.75 5.81 8 5 -3 48.86 6.59 -7 -5 3 17.68 2.93 7 5 -3 19.71 3.02 7 5 -3 16.12 3.62 -6 -5 3 36.94 3.97 6 5 -3 29.85 4.72 6 5 -3 35.02 3.83 6 5 -3 37.81 4.04 -5 -5 3 37.29 3.94 5 5 -3 36.97 3.95 5 5 -3 30.88 3.70 5 5 -3 41.02 4.51 4 -5 -3 2.70 1.49 -4 -5 3 7.13 1.84 4 5 -3 9.66 2.30 4 5 -3 8.31 1.87 4 5 -3 5.49 1.52 4 5 -3 5.13 2.13 -3 -5 3 10.71 2.16 3 -5 -3 15.35 2.33 3 5 -3 11.67 1.53 3 5 -3 12.44 2.11 3 5 -3 12.35 2.63 3 5 -3 15.63 2.37 -3 5 3 17.19 2.59 3 5 -3 11.47 2.06 2 -5 -3 382.67 26.52 -2 -5 3 282.24 26.34 -2 -5 3 332.28 26.64 2 5 -3 344.84 26.54 -2 5 3 351.20 26.69 2 5 -3 320.65 26.78 -2 5 3 334.67 26.53 2 5 -3 296.00 26.51 2 5 -3 321.83 26.48 -1 -5 3 474.06 35.67 -1 5 3 417.25 35.59 -1 5 3 390.22 35.78 1 5 -3 510.64 35.93 0 -5 -3 16.11 2.12 0 -5 3 16.11 2.47 0 5 3 20.58 2.49 0 5 3 18.26 2.11 0 5 -3 17.01 2.20 0 5 3 17.28 2.29 0 5 -3 12.13 2.19 0 5 3 18.72 2.23 1 -5 3 199.12 17.50 -1 -5 -3 233.17 17.40 1 5 3 214.97 17.26 -1 5 -3 196.65 17.26 -1 5 -3 182.82 17.39 1 5 3 239.87 17.69 1 5 3 229.00 17.26 1 5 3 212.06 17.35 2 -5 3 34.28 3.71 -2 -5 -3 40.96 4.46 -2 -5 -3 36.88 3.65 2 5 3 33.85 3.41 2 5 3 34.57 3.11 2 5 3 38.99 3.35 2 5 3 36.55 4.03 -2 5 -3 32.23 3.39 -2 5 -3 30.01 3.56 2 5 3 31.15 3.35 -3 -5 -3 65.68 6.17 3 5 3 66.99 5.74 -3 5 -3 52.35 5.85 3 5 3 70.92 5.98 3 5 3 73.33 6.69 3 5 3 76.84 5.91 3 5 3 71.78 5.98 -4 -5 -3 12.17 1.96 -4 -5 -3 10.86 3.01 4 5 3 11.32 2.83 4 5 3 12.07 1.76 4 5 3 8.79 1.69 -4 5 -3 18.95 2.56 4 5 3 12.52 1.86 -5 -5 -3 270.56 21.91 -5 -5 -3 273.92 23.32 5 5 3 260.17 22.82 5 5 3 280.85 21.89 -6 -5 -3 223.18 19.93 6 5 3 235.02 18.37 6 5 3 222.12 19.56 -7 -5 -3 7.67 3.32 7 5 3 7.40 3.24 -8 -5 -3 2.32 2.94 8 5 3 1.71 2.66 -9 -5 -3 0.32 2.93 9 5 3 0.72 2.71 -10 -5 -3 8.09 4.32 10 5 3 8.02 3.61 -11 -5 -3 -1.89 3.70 11 5 3 1.00 3.40 -12 -5 -3 2.25 4.28 -12 5 -3 5.18 2.32 12 5 3 3.07 3.94 11 6 -3 -0.23 3.70 10 6 -3 5.22 3.84 9 6 -3 11.00 3.92 -8 -6 3 20.05 3.28 8 6 -3 12.12 3.74 8 6 -3 23.19 3.47 -7 -6 3 5.27 2.04 7 6 -3 4.74 3.04 7 6 -3 5.81 2.31 -6 -6 3 206.76 17.85 6 6 -3 205.33 18.39 6 6 -3 229.67 17.88 -5 -6 3 0.15 1.58 5 6 -3 0.52 1.69 5 6 -3 -2.70 2.06 -4 -6 3 1.99 1.71 4 6 -3 2.47 2.22 4 6 -3 -1.32 1.86 4 6 -3 0.44 1.56 -3 -6 3 86.77 7.80 3 6 -3 96.03 8.02 3 6 -3 77.93 7.65 -2 -6 3 675.66 54.25 2 6 -3 702.28 54.19 -2 6 3 664.19 53.71 2 6 -3 678.12 54.11 -1 -6 3 23.15 3.32 -1 6 3 21.75 2.99 -1 6 3 27.70 2.97 1 6 -3 25.18 3.06 1 6 -3 26.06 3.16 0 -6 -3 61.13 5.94 0 6 -3 81.87 6.31 0 6 3 60.40 6.19 0 6 3 66.93 6.32 0 6 3 72.44 6.20 -1 -6 -3 198.94 18.23 1 -6 3 241.82 18.10 -1 -6 -3 189.06 17.58 1 6 3 208.96 18.00 -1 6 -3 246.74 17.55 -1 6 -3 239.31 17.80 1 6 3 212.83 17.66 1 6 3 196.48 17.76 2 -6 3 20.58 2.85 -2 -6 -3 10.39 2.79 -2 -6 -3 12.43 2.29 2 6 3 13.02 2.24 2 6 3 12.61 2.10 2 6 3 13.32 2.88 3 -6 3 0.95 1.65 -3 -6 -3 2.39 2.08 3 -6 3 -0.81 0.87 3 6 3 1.37 1.17 -3 6 -3 0.04 0.75 3 6 3 2.65 2.09 3 6 3 1.07 1.26 -3 6 -3 1.57 1.24 -4 -6 -3 10.02 3.00 4 6 3 5.99 2.63 -4 6 -3 6.19 1.81 4 6 3 10.07 1.99 4 6 3 8.58 1.73 4 6 3 6.21 2.85 -5 -6 -3 3.02 2.73 5 6 3 1.41 1.59 5 6 3 2.14 2.56 -6 -6 -3 10.78 3.59 6 6 3 12.51 2.69 6 6 3 7.87 3.13 -7 -6 -3 0.86 2.92 7 6 3 2.29 2.78 -8 -6 -3 3.92 3.21 8 6 3 1.26 2.67 -9 -6 -3 3.85 3.73 9 6 3 0.44 2.55 -10 -6 -3 -0.50 3.44 10 6 3 0.31 3.28 -11 -6 -3 -1.85 3.95 11 6 3 2.44 3.78 11 7 -3 3.83 4.05 10 7 -3 -3.02 3.31 9 7 -3 1.21 3.18 8 7 -3 0.89 3.02 -7 -7 3 6.33 2.18 7 7 -3 2.47 2.92 7 7 -3 6.69 2.74 -6 -7 3 11.94 2.62 6 7 -3 12.64 3.47 -5 -7 3 4.41 2.11 5 7 -3 8.08 3.17 -4 -7 3 182.43 16.15 4 7 -3 201.77 16.17 4 7 -3 190.41 16.52 -3 -7 3 22.31 3.39 3 7 -3 21.75 3.83 3 7 -3 25.44 3.48 -2 -7 3 104.29 9.40 2 7 -3 105.35 9.25 -2 7 3 94.95 8.58 2 7 -3 121.65 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-21 8.03 4.10 -4 5 21 -1.74 2.77 -3 -5 21 0.82 2.83 3 -5 -21 1.61 1.75 3 -5 -21 1.68 3.60 3 5 -21 8.13 4.19 -3 5 21 -0.59 2.74 2 -5 -21 -1.75 3.16 -2 -5 21 2.29 2.83 2 -5 -21 1.23 1.66 2 5 -21 2.35 3.80 1 -5 -21 0.68 1.65 1 -5 -21 -4.09 3.02 -1 -5 21 1.13 2.83 1 5 -21 3.91 3.67 0 -5 21 -1.14 2.44 0 -5 -21 0.53 1.67 0 -5 -21 -3.38 2.89 0 5 -21 4.05 4.42 -1 -5 -21 0.43 1.87 -2 -5 -21 0.97 2.00 7 0 -22 5.02 4.22 -7 0 22 2.69 3.49 6 0 -22 4.73 3.88 -6 0 22 -0.85 3.12 -5 0 22 -0.63 2.86 5 0 -22 1.30 3.54 4 0 -22 0.12 1.62 -4 0 22 1.96 3.03 4 0 -22 3.34 3.58 -3 0 22 0.11 2.56 3 0 -22 0.51 3.32 3 0 -22 -1.50 1.50 -2 0 22 -0.55 2.51 2 0 -22 1.95 3.21 2 0 -22 -1.37 1.45 -1 0 22 -1.24 2.36 1 0 -22 -2.05 1.36 1 0 -22 -1.86 2.64 0 0 -22 -1.47 1.46 -1 0 -22 0.50 1.64 -2 0 -22 1.85 1.66 -3 0 -22 -0.12 1.51 -4 0 -22 2.36 1.74 7 -1 -22 6.06 4.24 6 -1 -22 1.10 3.76 -6 -1 22 0.75 3.16 6 1 -22 1.53 4.05 -6 1 22 -1.60 3.15 5 -1 -22 1.59 3.56 -5 -1 22 -1.75 2.74 -5 1 22 -1.13 2.95 5 1 -22 0.33 3.66 4 -1 -22 2.98 3.44 -4 -1 22 0.34 2.86 4 -1 -22 -1.45 1.50 -4 1 22 2.12 3.05 4 1 -22 5.96 3.74 3 -1 -22 8.62 3.58 3 -1 -22 3.64 1.82 -3 -1 22 4.24 3.04 3 1 -22 10.58 3.88 -3 1 22 4.83 3.22 2 -1 -22 1.87 2.95 -2 -1 22 -0.96 2.31 2 -1 -22 -0.67 1.63 2 1 -22 0.98 3.11 -2 1 22 -1.76 2.49 2 1 -22 -1.44 1.41 1 -1 -22 4.83 1.84 -1 -1 22 3.55 2.71 1 -1 -22 10.31 3.21 -1 1 22 2.05 3.95 1 1 -22 5.63 1.99 1 1 -22 8.07 3.13 0 -1 -22 9.39 2.15 0 -1 -22 6.70 4.29 0 1 -22 2.90 1.71 -1 -1 -22 0.22 1.52 -1 1 -22 -1.49 1.42 -2 -1 -22 -0.87 1.58 -2 1 -22 0.39 1.52 -3 -1 -22 -1.22 1.60 -3 1 -22 0.40 1.59 -4 -1 -22 -0.11 1.65 -4 1 -22 0.22 1.58 -6 -2 22 -5.10 2.82 6 -2 -22 1.95 3.67 -6 2 22 -1.00 3.41 6 2 -22 2.98 4.11 -5 -2 22 2.84 3.12 5 -2 -22 1.31 3.67 5 -2 -22 -1.69 1.70 -5 2 22 -1.56 3.24 5 2 -22 3.06 3.83 4 -2 -22 0.12 3.29 -4 -2 22 2.00 3.01 4 -2 -22 0.36 1.59 4 2 -22 5.23 3.74 -4 2 22 -0.91 3.12 -3 -2 22 2.81 2.97 3 -2 -22 1.09 1.57 3 -2 -22 -0.32 3.24 3 2 -22 7.72 3.78 -3 2 22 -0.66 2.89 2 -2 -22 2.77 1.66 -2 -2 22 1.48 2.78 2 -2 -22 1.31 3.10 -2 2 22 2.09 2.77 2 2 -22 7.16 3.46 1 -2 -22 8.60 3.31 -1 -2 22 2.37 2.70 1 -2 -22 1.49 1.81 1 2 -22 6.83 3.20 1 2 -22 3.36 1.78 0 -2 -22 4.66 3.17 0 -2 -22 1.19 1.72 0 2 -22 -0.08 1.38 -1 -2 -22 1.68 1.81 -1 2 -22 0.88 1.64 -2 -2 -22 -0.75 1.47 -2 2 -22 -2.49 1.27 -3 -2 -22 1.26 1.78 -3 2 -22 -0.90 1.49 -5 -3 22 2.61 3.24 5 -3 -22 1.39 3.55 -5 3 22 -0.28 3.39 5 3 -22 9.31 4.23 4 -3 -22 -1.31 1.57 -4 -3 22 -1.05 2.92 4 -3 -22 -1.96 3.31 4 3 -22 4.16 3.84 -4 3 22 -3.68 2.93 3 -3 -22 0.38 1.57 -3 -3 22 0.59 2.86 3 -3 -22 2.44 3.43 -3 3 22 -0.67 2.86 3 3 -22 2.20 3.56 2 -3 -22 -0.58 3.19 2 -3 -22 0.75 1.71 -2 -3 22 2.95 2.83 -2 3 22 -0.83 2.77 2 3 -22 4.36 3.56 1 -3 -22 3.73 1.96 1 -3 -22 9.84 3.49 -1 -3 22 3.19 2.85 1 3 -22 10.86 3.61 0 -3 -22 2.54 1.86 0 -3 -22 2.08 2.94 -1 -3 -22 1.05 1.78 -2 -3 -22 0.54 1.51 -2 3 -22 -1.43 1.44 -3 -3 -22 1.20 1.81 -3 3 -22 -1.27 1.42 4 -4 -22 0.87 3.75 -4 -4 22 -1.01 2.84 4 4 -22 8.05 4.13 -4 4 22 0.01 3.27 3 -4 -22 -0.16 3.61 3 -4 -22 1.94 1.82 -3 -4 22 -1.23 2.76 3 4 -22 6.25 4.10 -3 4 22 -1.21 2.97 2 -4 -22 -1.95 3.37 -2 -4 22 1.26 2.85 2 -4 -22 -0.47 1.71 2 4 -22 8.20 3.91 -1 -4 22 4.82 3.02 1 -4 -22 10.20 3.78 1 -4 -22 6.77 2.10 1 4 -22 14.19 4.14 0 -4 -22 2.08 3.30 0 -4 22 2.96 2.97 0 -4 -22 3.36 1.91 -1 -4 -22 3.33 1.91 -2 -4 -22 5.34 2.16 2 -5 -22 0.81 1.74 1 -5 -22 1.53 1.79 1 -5 -22 -1.84 3.29 5 0 -23 7.28 3.83 -5 0 23 2.68 3.17 4 0 -23 3.42 3.72 -4 0 23 0.25 2.84 3 0 -23 6.41 3.85 3 0 -23 2.43 1.88 -3 0 23 4.05 3.08 2 0 -23 -2.20 1.46 2 0 -23 1.31 3.21 -2 0 23 0.60 2.73 1 0 -23 0.00 1.58 1 0 -23 0.39 3.15 0 0 -23 -0.90 1.48 -1 0 -23 8.61 2.28 -2 0 -23 0.23 1.61 -5 -1 23 -2.01 2.91 5 -1 -23 4.36 3.82 5 1 -23 5.98 3.99 -5 1 23 -0.32 3.37 4 -1 -23 -1.51 3.52 4 -1 -23 -1.80 1.56 -4 -1 23 -1.84 2.83 -4 1 23 -1.16 2.91 4 1 -23 4.15 4.03 3 -1 -23 1.77 3.53 -3 -1 23 1.01 2.90 3 -1 -23 -0.12 1.62 3 1 -23 0.07 3.56 -3 1 23 1.76 3.09 2 -1 -23 7.31 3.45 -2 -1 23 4.86 3.02 2 -1 -23 3.99 1.96 2 1 -23 12.89 3.92 -2 1 23 2.96 2.86 2 1 -23 3.43 1.79 1 -1 -23 5.30 3.26 1 -1 -23 0.86 1.73 -1 -1 23 7.36 4.82 1 1 -23 5.44 3.37 1 1 -23 1.34 1.79 0 -1 -23 1.63 1.63 0 1 -23 -1.55 1.36 -1 -1 -23 -0.19 1.57 -1 1 -23 -1.91 1.45 -2 -1 -23 -0.32 1.58 -2 1 -23 1.29 1.66 5 -2 -23 1.10 3.65 5 2 -23 3.92 4.12 -4 -2 23 -1.04 2.95 4 -2 -23 -3.44 1.50 4 -2 -23 0.24 3.48 4 2 -23 2.54 3.65 -4 2 23 -2.54 3.04 -3 -2 23 2.43 3.02 3 -2 -23 5.78 3.70 3 -2 -23 0.24 1.65 -3 2 23 2.05 3.12 3 2 -23 6.20 3.88 -2 -2 23 -0.88 2.87 2 -2 -23 0.75 1.71 2 -2 -23 8.86 3.62 -2 2 23 1.86 4.11 2 2 -23 6.12 3.69 1 -2 -23 14.66 3.87 -1 -2 23 9.45 3.50 1 -2 -23 11.30 2.49 1 2 -23 17.43 4.12 0 -2 -23 7.54 2.28 0 2 -23 4.73 1.88 -1 -2 -23 -1.96 1.60 -1 2 -23 -0.82 1.48 -2 -2 -23 -0.46 1.78 -2 2 -23 1.33 1.74 4 -3 -23 -1.76 1.59 4 -3 -23 -4.30 3.37 3 -3 -23 -0.49 3.61 3 -3 -23 -0.32 1.59 -3 -3 23 0.57 2.83 -3 3 23 -3.06 3.00 3 3 -23 4.17 3.92 -2 -3 23 2.83 2.90 2 -3 -23 2.11 1.80 2 -3 -23 3.73 3.68 2 3 -23 6.22 3.80 1 -3 -23 10.31 2.60 1 -3 -23 20.16 4.25 -1 -3 23 7.78 3.35 1 3 -23 23.31 4.50 0 -3 -23 5.01 2.25 -1 -3 -23 1.43 1.74 3 0 -24 3.82 3.64 3 0 -24 -1.59 1.60 -2 0 24 2.33 4.29 2 0 -24 -2.15 1.54 2 0 -24 0.87 3.35 1 0 -24 -0.30 1.59 0 0 -24 -0.63 1.61 3 -1 -24 -1.43 1.66 2 -1 -24 5.70 3.73 -2 -1 24 1.68 3.07 2 -1 -24 0.83 1.70 2 1 -24 0.48 1.85 2 1 -24 11.07 4.25 1 -1 -24 -0.70 1.59 1 1 -24 -1.55 1.52 0 0 0 0.00 0.00 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.5647 _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 0.71097 9.640 8.427 16.915 89.984 96.674 90.150 ) _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 7983 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9498(3) 0.7694(3) 0.47245(16) 0.0419(6) Uani 1 1 d . . . . . C2 C 0.8083(3) 0.5703(3) 0.40414(16) 0.0423(6) Uani 1 1 d . . . . . C3 C 0.7279(3) 0.6933(4) 0.36374(19) 0.0525(7) Uani 1 1 d . . . . . C4 C 0.7570(3) 0.8443(4) 0.3791(2) 0.0541(8) Uani 1 1 d . . . . . H4 H 0.702825 0.923909 0.352869 0.065 Uiso 1 1 calc R U . . . F1 F 0.6207(2) 0.6495(3) 0.31011(14) 0.0828(8) Uani 1 1 d . . . . . N2 N 0.9165(2) 0.6148(3) 0.45697(13) 0.0409(5) Uani 1 1 d . . . . . H2N H 0.960(9) 0.518(13) 0.481(5) 0.09(3) Uiso 0.5 1 d . . P . . N1 N 0.8664(3) 0.8818(3) 0.43356(17) 0.0524(6) Uani 1 1 d . . . . . H1N H 0.874(4) 0.972(6) 0.447(2) 0.075(13) Uiso 1 1 d . . . . . N3 N 0.7803(3) 0.4205(3) 0.39170(17) 0.0554(7) Uani 1 1 d D . . . . H3N H 0.713(3) 0.388(5) 0.3559(19) 0.083 Uiso 1 1 d D U . . . H4N H 0.842(4) 0.353(4) 0.415(2) 0.083 Uiso 1 1 d D U . . . O1 O 1.0513(2) 0.8067(2) 0.51999(13) 0.0556(6) Uani 1 1 d . . . . . C5 C 0.5432(3) 0.2133(4) 0.23254(18) 0.0529(7) Uani 1 1 d . . . . . C6 C 0.4019(3) 0.2059(4) 0.18369(18) 0.0520(7) Uani 1 1 d . . . . . C7 C 0.3354(3) 0.0633(4) 0.16373(19) 0.0537(7) Uani 1 1 d . . . . . H7D H 0.378844 -0.031804 0.179937 0.064 Uiso 0.328(3) 1 calc R U P A 2 C8 C 0.2040(3) 0.0612(5) 0.1196(2) 0.0643(9) Uani 1 1 d . . . . . H8 H 0.156739 -0.033892 0.107939 0.077 Uiso 1 1 calc R U . . . C9 C 0.1464(3) 0.2037(5) 0.0937(2) 0.0615(9) Uani 1 1 d . . . . . C10 C 0.2083(4) 0.3454(5) 0.1114(2) 0.0661(9) Uani 1 1 d . . . . . H10 H 0.166232 0.439753 0.092784 0.079 Uiso 1 1 calc R U . . . C11 C 0.3366(4) 0.3458(5) 0.1582(2) 0.0609(8) Uani 1 1 d . . . . . H11 H 0.379399 0.442178 0.172639 0.073 Uiso 0.672(3) 1 calc R U P A 1 N4 N 0.0073(3) 0.2033(5) 0.0457(2) 0.0795(10) Uani 1 1 d . . . . . O2 O 0.5601(3) 0.3093(4) 0.28604(17) 0.0803(9) Uani 1 1 d . . . . . O3 O 0.6339(3) 0.1202(3) 0.21176(15) 0.0674(7) Uani 1 1 d . . . . . H3O H 0.709(6) 0.146(7) 0.235(4) 0.041(17) Uiso 0.5 1 d . . P . . O4 O -0.0712(3) 0.0922(6) 0.0565(2) 0.1104(13) Uani 1 1 d . . . . . O5 O -0.0204(4) 0.3087(6) -0.0010(3) 0.1224(15) Uani 1 1 d . . . . . Cl1 Cl 0.39861(15) -0.12052(16) 0.19950(9) 0.0683(5) Uani 0.672(3) 1 d . . P A 1 Cl1D Cl 0.3763(4) 0.5440(5) 0.1841(2) 0.0921(14) Uani 0.328(3) 1 d . . P A 2 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 0.0500(14) 0.0293(12) 0.0448(13) -0.0013(10) -0.0014(11) -0.0031(11) C2 0.0451(14) 0.0363(13) 0.0436(13) 0.0011(11) -0.0034(11) -0.0003(11) C3 0.0476(15) 0.0468(16) 0.0584(17) 0.0068(13) -0.0129(13) -0.0026(13) C4 0.0531(16) 0.0365(14) 0.0686(19) 0.0126(13) -0.0097(14) 0.0032(13) F1 0.0731(13) 0.0604(13) 0.1008(16) 0.0092(11) -0.0485(12) -0.0059(11) N2 0.0491(12) 0.0262(10) 0.0440(11) -0.0014(9) -0.0084(9) -0.0005(9) N1 0.0605(15) 0.0279(12) 0.0652(16) 0.0035(11) -0.0079(12) 0.0009(11) N3 0.0585(16) 0.0361(13) 0.0646(16) -0.0049(11) -0.0219(12) -0.0036(11) O1 0.0680(14) 0.0290(9) 0.0629(13) -0.0035(9) -0.0213(10) -0.0034(9) C5 0.0462(15) 0.0607(19) 0.0496(15) -0.0029(14) -0.0035(12) -0.0127(14) C6 0.0402(14) 0.066(2) 0.0481(15) -0.0070(14) 0.0000(11) -0.0101(14) C7 0.0483(16) 0.0564(18) 0.0545(16) -0.0080(14) -0.0018(13) -0.0055(14) C8 0.0490(17) 0.077(2) 0.0645(19) -0.0149(18) -0.0012(15) -0.0163(17) C9 0.0405(15) 0.088(3) 0.0543(17) -0.0051(17) -0.0006(13) -0.0018(17) C10 0.0602(19) 0.074(2) 0.0626(19) 0.0076(18) 0.0032(16) 0.0055(18) C11 0.0585(19) 0.063(2) 0.0604(18) -0.0054(16) 0.0029(15) -0.0109(17) N4 0.0490(16) 0.113(3) 0.073(2) -0.012(2) -0.0046(14) 0.0053(19) O2 0.0524(13) 0.103(2) 0.0819(17) -0.0412(16) -0.0081(12) -0.0116(14) O3 0.0522(13) 0.0691(16) 0.0749(16) -0.0175(13) -0.0175(11) 0.0060(12) O4 0.0505(15) 0.157(4) 0.119(3) -0.026(3) -0.0096(16) -0.022(2) O5 0.087(2) 0.165(4) 0.105(2) 0.030(3) -0.0305(19) 0.015(2) Cl1 0.0627(8) 0.0521(7) 0.0883(10) 0.0029(6) 0.0016(6) -0.0002(6) Cl1D 0.083(2) 0.082(2) 0.107(3) 0.0061(19) -0.0040(19) -0.0272(18) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 O1 C1 N2 121.4(2) . . ? O1 C1 N1 121.2(3) . . ? N2 C1 N1 117.4(3) . . ? N3 C2 N2 120.4(2) . . ? N3 C2 C3 122.5(3) . . ? N2 C2 C3 117.0(3) . . ? C4 C3 F1 121.7(3) . . ? C4 C3 C2 121.1(3) . . ? F1 C3 C2 117.3(3) . . ? C3 C4 N1 119.3(3) . . ? C3 C4 H4 120.4 . . ? N1 C4 H4 120.4 . . ? C2 N2 C1 122.8(2) . . ? C2 N2 H2N 107(5) . . ? C1 N2 H2N 130(5) . . ? C4 N1 C1 122.4(3) . . ? C4 N1 H1N 117(3) . . ? C1 N1 H1N 120(3) . . ? C2 N3 H3N 122(3) . . ? C2 N3 H4N 116(3) . . ? H3N N3 H4N 121(4) . . ? O2 C5 O3 126.2(3) . . ? O2 C5 C6 118.1(3) . . ? O3 C5 C6 115.6(3) . . ? C11 C6 C7 118.9(3) . . ? C11 C6 C5 119.0(3) . . ? C7 C6 C5 122.1(3) . . ? C6 C7 C8 120.5(3) . . ? C6 C7 Cl1 123.5(2) . . ? C8 C7 Cl1 115.6(3) . . ? C6 C7 H7D 119.7 . . ? C8 C7 H7D 119.7 . . ? C9 C8 C7 117.9(3) . . ? C9 C8 H8 121.1 . . ? C7 C8 H8 121.1 . . ? C10 C9 C8 123.4(3) . . ? C10 C9 N4 118.0(4) . . ? C8 C9 N4 118.6(4) . . ? C9 C10 C11 118.0(4) . . ? C9 C10 H10 121.0 . . ? C11 C10 H10 121.0 . . ? C6 C11 C10 121.3(3) . . ? C6 C11 Cl1D 130.9(3) . . ? C10 C11 Cl1D 107.4(3) . . ? C6 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? O5 N4 O4 124.7(4) . . ? O5 N4 C9 118.5(4) . . ? O4 N4 C9 116.8(4) . . ? C5 O3 H3O 108(4) . . ? 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 O1 1.232(3) . ? C1 N2 1.359(3) . ? C1 N1 1.361(4) . ? C2 N3 1.302(4) . ? C2 N2 1.345(3) . ? C2 C3 1.419(4) . ? C3 C4 1.321(5) . ? C3 F1 1.345(3) . ? C4 N1 1.354(4) . ? C4 H4 0.9300 . ? N2 H2N 0.98(9) . ? N1 H1N 0.80(5) . ? N3 H3N 0.878(19) . ? N3 H4N 0.878(19) . ? C5 O2 1.212(4) . ? C5 O3 1.255(4) . ? C5 C6 1.509(4) . ? C6 C11 1.381(5) . ? C6 C7 1.383(5) . ? C7 C8 1.393(4) . ? C7 Cl1 1.746(4) . ? C7 H7D 0.9300 . ? C8 C9 1.372(6) . ? C8 H8 0.9300 . ? C9 C10 1.352(6) . ? C9 N4 1.483(4) . ? C10 C11 1.387(5) . ? C10 H10 0.9300 . ? C11 Cl1D 1.756(5) . ? C11 H11 0.9300 . ? N4 O5 1.199(5) . ? N4 O4 1.230(5) . ? O3 H3O 0.81(6) . ? 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 N2 H2N N2 0.98(9) 1.87(8) 2.810(5) 160(8) 3_766 yes N1 H1N O1 0.80(5) 2.05(5) 2.825(4) 165(4) 3_776 yes N3 H3N O2 0.878(19) 1.90(2) 2.772(4) 175(4) . yes N3 H4N O1 0.878(19) 1.95(2) 2.821(3) 169(4) 3_766 yes O3 H3O O3 0.81(6) 1.68(6) 2.449(5) 157(6) 2_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 N3 C2 C3 C4 178.3(3) . . . . ? N2 C2 C3 C4 -1.6(5) . . . . ? N3 C2 C3 F1 -0.9(5) . . . . ? N2 C2 C3 F1 179.2(3) . . . . ? F1 C3 C4 N1 -179.9(3) . . . . ? C2 C3 C4 N1 0.9(5) . . . . ? N3 C2 N2 C1 -179.7(3) . . . . ? C3 C2 N2 C1 0.2(4) . . . . ? O1 C1 N2 C2 -178.5(3) . . . . ? N1 C1 N2 C2 1.7(4) . . . . ? C3 C4 N1 C1 1.1(5) . . . . ? O1 C1 N1 C4 177.8(3) . . . . ? N2 C1 N1 C4 -2.4(5) . . . . ? O2 C5 C6 C11 44.8(5) . . . . ? O3 C5 C6 C11 -133.4(3) . . . . ? O2 C5 C6 C7 -135.1(4) . . . . ? O3 C5 C6 C7 46.7(4) . . . . ? C11 C6 C7 C8 -0.9(5) . . . . ? C5 C6 C7 C8 179.0(3) . . . . ? C11 C6 C7 Cl1 -174.0(3) . . . . ? C5 C6 C7 Cl1 5.9(5) . . . . ? C6 C7 C8 C9 2.9(5) . . . . ? Cl1 C7 C8 C9 176.6(3) . . . . ? C7 C8 C9 C10 -2.5(5) . . . . ? C7 C8 C9 N4 179.2(3) . . . . ? C8 C9 C10 C11 -0.1(6) . . . . ? N4 C9 C10 C11 178.3(3) . . . . ? C7 C6 C11 C10 -1.8(5) . . . . ? C5 C6 C11 C10 178.3(3) . . . . ? C7 C6 C11 Cl1D 169.2(3) . . . . ? C5 C6 C11 Cl1D -10.7(5) . . . . ? C9 C10 C11 C6 2.3(5) . . . . ? C9 C10 C11 Cl1D -170.6(3) . . . . ? C10 C9 N4 O5 29.7(6) . . . . ? C8 C9 N4 O5 -151.9(4) . . . . ? C10 C9 N4 O4 -151.0(4) . . . . ? C8 C9 N4 O4 27.4(5) . . . . ?