#------------------------------------------------------------------------------ #$Date: 2021-12-07 05:55:55 +0200 (Tue, 07 Dec 2021) $ #$Revision: 271230 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/83/7158385.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7158385 loop_ _publ_author_name 'Kaur, Banni Preet' 'Sharma, Vivek' 'Sahoo, Subash Chandra' 'Chimni, Swapandeep Singh' _publ_section_title ; Low catalyst loading enabled organocatalytic synthesis of chiral bis-heterocyclic frameworks containing pyrazole and isoxazole. ; _journal_issue 45 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 9910 _journal_page_last 9924 _journal_paper_doi 10.1039/d1ob01313k _journal_volume 19 _journal_year 2021 _chemical_absolute_configuration syn _chemical_formula_moiety 'C22 H20 Cl N3 O4' _chemical_formula_sum 'C22 H20 Cl N3 O4' _chemical_formula_weight 425.86 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-08-29 _audit_creation_method ; Olex2 1.2-ac3 (compiled 2017.01.05 svn.r3372 for Rigaku Oxford Diffraction, GUI svn.r5289) ; _audit_update_record ; 2019-09-05 deposited with the CCDC. 2021-10-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.009(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.7803(2) _cell_length_b 9.3559(3) _cell_length_c 14.8204(4) _cell_measurement_reflns_used 9512 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.7420 _cell_measurement_theta_min 3.4770 _cell_volume 1078.80(5) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_type HyPix3000 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.947 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -17.00 11.00 0.50 8.00 -- -9.95 -90.00 5.00 56 2 \w -21.00 6.00 0.50 8.00 -- -9.95 90.00 120.00 54 3 \w -28.00 37.00 0.50 8.00 -- 10.22 -90.00 5.00 130 4 \w -9.00 31.00 0.50 8.00 -- 10.22 90.00 120.00 80 5 \w -74.00 4.00 0.50 8.00 -- -9.95 -38.00 0.00 156 6 \w -58.00 -15.00 0.50 8.00 -- -9.95 125.00-120.00 86 7 \w -6.00 31.00 0.50 8.00 -- -9.95 38.00 -90.00 74 8 \w -38.00 -6.00 0.50 8.00 -- 10.22 125.00-121.60 64 9 \w -23.00 3.00 0.50 8.00 -- 10.22 118.00 -3.63 52 10 \w -54.00 -16.00 0.50 8.00 -- 10.22 -19.00 120.00 76 11 \w -13.00 42.00 0.50 8.00 -- 10.22 -99.00-150.00 110 12 \w -54.00 -24.00 0.50 8.00 -- 10.22 -77.00-150.00 60 13 \w -19.00 36.00 0.50 8.00 -- 10.22 -77.00-150.00 110 14 \w -9.00 16.00 0.50 8.00 -- 10.22 -99.00 120.00 50 15 \w -54.00 17.00 0.50 8.00 -- 10.22 -38.00 -90.00 142 16 \w -14.00 12.00 0.50 8.00 -- 10.22 -99.00-180.00 52 17 \w -34.00 12.00 0.50 8.00 -- 10.22 -38.00-150.00 92 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, HyPix3000' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0125347000 _diffrn_orient_matrix_UB_12 0.0687071000 _diffrn_orient_matrix_UB_13 0.0191862000 _diffrn_orient_matrix_UB_21 0.0368114000 _diffrn_orient_matrix_UB_22 -0.0319258000 _diffrn_orient_matrix_UB_23 0.0388755000 _diffrn_orient_matrix_UB_31 0.0824229000 _diffrn_orient_matrix_UB_32 0.0037400000 _diffrn_orient_matrix_UB_33 -0.0202535000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0838 _diffrn_reflns_av_unetI/netI 0.0518 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.947 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 14001 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.920 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.467 _diffrn_reflns_theta_min 3.406 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.210 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.78948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.311 _exptl_crystal_description block _exptl_crystal_F_000 444 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.153 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.052 _refine_ls_abs_structure_details ; Flack x determined using 1066 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.14(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 273 _refine_ls_number_reflns 4537 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.087 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0561 _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^)+(0.0907P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1366 _refine_ls_wR_factor_ref 0.1700 _reflns_Friedel_coverage 0.830 _reflns_Friedel_fraction_full 0.980 _reflns_Friedel_fraction_max 0.889 _reflns_number_gt 3095 _reflns_number_total 4537 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL sub-gndu2_a.res in P2(1) sub-gndu2.res created by SHELXL-2017/1 at 15:08:18 on 29-Aug-2019 REM Old TITL sub-GNDU2 in P2(1) REM SHELXT solution in P2(1) REM R1 0.168, Rweak 0.053, Alpha 0.004, Orientation as input REM Flack x = 0.004 ( 0.131 ) from Parsons' quotients REM Formula found by SHELXT: C24 N2 O3 Cl CELL 0.71073 7.7803 9.3559 14.8204 90 90.009 90 ZERR 2 0.0002 0.0003 0.0004 0 0.003 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H Cl N O UNIT 44 40 2 6 8 L.S. 30 PLAN 5 BOND $H LIST 6 fmap 2 acta OMIT 5 7 5 OMIT -4 8 1 OMIT -5 7 1 OMIT 5 7 0 OMIT 5 6 1 REM REM REM WGHT 0.090700 FVAR 1.92828 CL1 3 0.664348 0.276031 0.090705 11.00000 0.10031 0.12817 = 0.09431 -0.04241 0.01130 -0.02400 O3 5 0.941972 0.142988 0.385144 11.00000 0.05834 0.06392 = 0.11009 -0.00069 0.00211 0.01225 N2 4 0.552458 0.687310 0.229151 11.00000 0.05630 0.05383 = 0.05176 0.00327 0.00713 0.00829 N1 4 0.658727 0.649989 0.160583 11.00000 0.05874 0.06197 = 0.04936 0.00483 0.00824 0.01116 N3 4 0.967536 0.580098 0.424960 11.00000 0.08284 0.05788 = 0.08068 0.00051 -0.01671 -0.00217 C13 1 0.791079 0.134404 0.370937 11.00000 0.05641 0.05376 = 0.06586 -0.00014 0.00820 0.00768 O1 5 0.919938 0.701357 0.434249 11.00000 0.13587 0.05232 = 0.14748 -0.00535 -0.04155 0.00066 C3 1 0.581042 0.609359 0.303982 11.00000 0.05901 0.06007 = 0.04995 -0.00089 0.01229 0.01190 AFIX 43 H3 2 0.522306 0.617157 0.358408 11.00000 -1.20000 AFIX 0 C2 1 0.712329 0.516493 0.285394 11.00000 0.05052 0.05359 = 0.04727 0.00110 0.00727 0.00607 C1 1 0.755364 0.546820 0.194945 11.00000 0.05649 0.05396 = 0.04806 0.00159 0.00670 0.00248 C17 1 0.425789 0.796321 0.216007 11.00000 0.06123 0.04646 = 0.06165 -0.00513 -0.00060 0.01232 C12 1 0.685492 0.266518 0.346660 11.00000 0.05145 0.05334 = 0.05146 0.00061 0.00260 0.00191 AFIX 13 H12 2 0.641972 0.250902 0.285392 11.00000 -1.20000 AFIX 0 C4 1 0.893691 0.478534 0.141753 11.00000 0.05723 0.06060 = 0.04411 0.00586 0.01048 0.01053 O4 5 0.547619 0.280957 0.487652 11.00000 0.08666 0.17255 = 0.07904 -0.00572 0.03565 -0.01065 O2 5 1.111975 0.547847 0.403481 11.00000 0.08627 0.09510 = 0.14522 -0.00700 0.02040 -0.02020 C10 1 0.793004 0.403781 0.343327 11.00000 0.05095 0.05322 = 0.04566 0.00421 0.00727 0.01000 AFIX 13 H10 2 0.901908 0.378272 0.314274 11.00000 -1.20000 AFIX 0 C5 1 1.058378 0.534348 0.142233 11.00000 0.06205 0.08143 = 0.07667 0.00502 0.01808 0.00365 AFIX 43 H5 2 1.081129 0.615268 0.176666 11.00000 -1.20000 AFIX 0 C15 1 0.528173 0.274713 0.408151 11.00000 0.05491 0.07237 = 0.08772 0.00425 0.01310 0.00107 C9 1 0.866384 0.356486 0.091709 11.00000 0.07105 0.08020 = 0.05327 -0.00266 0.00803 0.00804 C18 1 0.297038 0.813395 0.278337 11.00000 0.06309 0.07147 = 0.07923 0.00169 0.01079 0.01315 AFIX 43 H18 2 0.291775 0.754714 0.328912 11.00000 -1.20000 AFIX 0 C20 1 0.183686 1.004326 0.191776 11.00000 0.09851 0.08621 = 0.10408 -0.00422 0.00019 0.04202 AFIX 43 H20 2 0.102100 1.075913 0.183959 11.00000 -1.20000 AFIX 0 C11 1 0.839188 0.461890 0.437167 11.00000 0.06245 0.05988 = 0.05271 0.00200 0.00024 0.00137 AFIX 23 H11A 2 0.737029 0.497917 0.466995 11.00000 -1.20000 H11B 2 0.887931 0.386437 0.474051 11.00000 -1.20000 AFIX 0 C19 1 0.175774 0.918429 0.265098 11.00000 0.07881 0.08714 = 0.10734 -0.00311 0.01757 0.02862 AFIX 43 H19 2 0.087747 0.930447 0.306860 11.00000 -1.20000 AFIX 0 C22 1 0.433608 0.881107 0.140863 11.00000 0.10010 0.08636 = 0.06984 0.01405 0.01485 0.03801 AFIX 43 H22 2 0.519967 0.868285 0.098246 11.00000 -1.20000 AFIX 0 C6 1 1.189499 0.473386 0.093136 11.00000 0.06981 0.10610 = 0.10327 0.01534 0.02834 0.01663 AFIX 43 H6 2 1.298807 0.513576 0.094198 11.00000 -1.20000 AFIX 0 C8 1 0.997976 0.292769 0.041746 11.00000 0.10995 0.09208 = 0.07142 -0.01718 0.02130 0.02470 AFIX 43 H8 2 0.977660 0.210476 0.008201 11.00000 -1.20000 AFIX 0 C21 1 0.309943 0.986708 0.129532 11.00000 0.13131 0.09873 = 0.08930 0.02796 0.00613 0.05348 AFIX 43 H21 2 0.313661 1.045648 0.079040 11.00000 -1.20000 AFIX 0 C7 1 1.158956 0.354941 0.043373 11.00000 0.08467 0.10802 = 0.08918 0.01648 0.03951 0.03319 AFIX 43 H7 2 1.247591 0.314775 0.009769 11.00000 -1.20000 AFIX 0 C14 1 0.702568 -0.004085 0.372425 11.00000 0.09045 0.05963 = 0.18633 0.01768 -0.01476 -0.00880 AFIX 137 H14A 2 0.785775 -0.079469 0.377243 11.00000 -1.50000 H14B 2 0.637835 -0.015695 0.317764 11.00000 -1.50000 H14C 2 0.626192 -0.007689 0.423243 11.00000 -1.50000 AFIX 0 C16 1 0.355724 0.272750 0.363081 11.00000 0.04981 0.12791 = 0.16772 -0.00037 -0.00140 0.00815 AFIX 137 H16A 2 0.355590 0.338985 0.313608 11.00000 -1.50000 H16B 2 0.268832 0.299715 0.405797 11.00000 -1.50000 H16C 2 0.332295 0.178292 0.340969 11.00000 -1.50000 AFIX 0 HKLF 4 REM sub-gndu2_a.res in P2(1) REM R1 = 0.0561 for 3095 Fo > 4sig(Fo) and 0.0806 for all 4537 data REM 273 parameters refined using 1 restraints END WGHT 0.0907 0.0000 REM Highest difference peak 0.153, deepest hole -0.276, 1-sigma level 0.052 Q1 1 0.2250 0.3637 0.2691 11.00000 0.05 0.15 Q2 1 1.1800 0.2324 -0.0365 11.00000 0.05 0.15 Q3 1 0.4024 0.4334 0.2377 11.00000 0.05 0.15 Q4 1 0.7027 -0.1536 0.4789 11.00000 0.05 0.15 Q5 1 0.8093 -0.0781 0.4639 11.00000 0.05 0.14 REM The information below was added by Olex2. REM REM R1 = 0.0561 for 3095 Fo > 4sig(Fo) and 0.0806 for all 14023 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.15, deepest hole -0.28 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0806 REM R1_gt = 0.0561 REM wR_ref = 0.1700 REM GOOF = 1.087 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 14023 REM Reflections_gt = 3095 REM Parameters = n/a REM Hole = -0.28 REM Peak = 0.15 REM Flack = 0.14(7) ; _cod_data_source_file d1ob01313k2.cif _cod_data_source_block sub-gndu2 _cod_depositor_comments 'Adding full bibliography for 7158385.cif.' _cod_database_code 7158385 _shelx_shelxl_version_number 2017/1 _chemical_oxdiff_formula 'C H N O Cl' _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. ; _diffrn_oxdiff_ac3_digest_frames ; 014a5aeb4633fd442ac092326057c5eaec0144486b9 ; _diffrn_oxdiff_ac3_digest_hkl ; 015746d478f9845665fb65ce4a4b48c709fbcc ; _reflns_odcompleteness_completeness 99.70 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C12(H12), C10(H10) 2.b Secondary CH2 refined with riding coordinates: C11(H11A,H11B) 2.c Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C18(H18), C20(H20), C19(H19), C22(H22), C6(H6), C8(H8), C21(H21), C7(H7) 2.d Idealised Me refined as rotating group: C14(H14A,H14B,H14C), C16(H16A,H16B,H16C) ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.189 _oxdiff_exptl_absorpt_empirical_full_min 0.726 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 Cl1 Cl 0.66435(18) 0.2760(2) 0.09070(10) 0.1076(6) Uani 1 1 d . . . . . O3 O 0.9420(4) 0.1430(4) 0.3851(2) 0.0775(9) Uani 1 1 d . . . . . N2 N 0.5525(4) 0.6873(4) 0.2292(2) 0.0540(8) Uani 1 1 d . . . . . N1 N 0.6587(4) 0.6500(4) 0.1606(2) 0.0567(8) Uani 1 1 d . . . . . N3 N 0.9675(6) 0.5801(5) 0.4250(3) 0.0738(11) Uani 1 1 d . . . . . C13 C 0.7911(5) 0.1344(5) 0.3709(3) 0.0587(10) Uani 1 1 d . . . . . O1 O 0.9199(6) 0.7014(4) 0.4342(3) 0.1119(14) Uani 1 1 d . . . . . C3 C 0.5810(5) 0.6094(5) 0.3040(3) 0.0563(10) Uani 1 1 d . . . . . H3 H 0.522306 0.617157 0.358408 0.068 Uiso 1 1 calc R . . . . C2 C 0.7123(5) 0.5165(4) 0.2854(2) 0.0505(9) Uani 1 1 d . . . . . C1 C 0.7554(5) 0.5468(5) 0.1949(2) 0.0528(9) Uani 1 1 d . . . . . C17 C 0.4258(5) 0.7963(5) 0.2160(3) 0.0564(9) Uani 1 1 d . . . . . C12 C 0.6855(5) 0.2665(5) 0.3467(2) 0.0521(9) Uani 1 1 d . . . . . H12 H 0.641972 0.250902 0.285392 0.063 Uiso 1 1 calc R . . . . C4 C 0.8937(5) 0.4785(5) 0.1418(2) 0.0540(10) Uani 1 1 d . . . . . O4 O 0.5476(5) 0.2810(7) 0.4877(3) 0.1127(15) Uani 1 1 d . . . . . O2 O 1.1120(6) 0.5478(5) 0.4035(3) 0.1089(14) Uani 1 1 d . . . . . C10 C 0.7930(5) 0.4038(5) 0.3433(2) 0.0499(9) Uani 1 1 d . . . . . H10 H 0.901908 0.378272 0.314274 0.060 Uiso 1 1 calc R . . . . C5 C 1.0584(6) 0.5343(6) 0.1422(3) 0.0734(13) Uani 1 1 d . . . . . H5 H 1.081129 0.615268 0.176666 0.088 Uiso 1 1 calc R . . . . C15 C 0.5282(5) 0.2747(6) 0.4082(4) 0.0717(12) Uani 1 1 d . . . . . C9 C 0.8664(6) 0.3565(6) 0.0917(3) 0.0682(12) Uani 1 1 d . . . . . C18 C 0.2970(5) 0.8134(5) 0.2783(3) 0.0713(13) Uani 1 1 d . . . . . H18 H 0.291775 0.754714 0.328912 0.086 Uiso 1 1 calc R . . . . C20 C 0.1837(8) 1.0043(7) 0.1918(4) 0.0963(17) Uani 1 1 d . . . . . H20 H 0.102100 1.075913 0.183959 0.116 Uiso 1 1 calc R . . . . C11 C 0.8392(5) 0.4619(5) 0.4372(3) 0.0583(10) Uani 1 1 d . . . . . H11A H 0.737029 0.497917 0.466995 0.070 Uiso 1 1 calc R . . . . H11B H 0.887931 0.386437 0.474051 0.070 Uiso 1 1 calc R . . . . C19 C 0.1758(7) 0.9184(7) 0.2651(4) 0.0911(16) Uani 1 1 d . . . . . H19 H 0.087747 0.930447 0.306860 0.109 Uiso 1 1 calc R . . . . C22 C 0.4336(7) 0.8811(7) 0.1409(3) 0.0854(16) Uani 1 1 d . . . . . H22 H 0.519967 0.868285 0.098246 0.103 Uiso 1 1 calc R . . . . C6 C 1.1895(7) 0.4734(8) 0.0931(4) 0.0931(19) Uani 1 1 d . . . . . H6 H 1.298807 0.513576 0.094198 0.112 Uiso 1 1 calc R . . . . C8 C 0.9980(8) 0.2928(8) 0.0417(3) 0.0911(17) Uani 1 1 d . . . . . H8 H 0.977660 0.210476 0.008201 0.109 Uiso 1 1 calc R . . . . C21 C 0.3099(9) 0.9867(8) 0.1295(4) 0.106(2) Uani 1 1 d . . . . . H21 H 0.313661 1.045648 0.079040 0.128 Uiso 1 1 calc R . . . . C7 C 1.1590(8) 0.3549(8) 0.0434(4) 0.0940(19) Uani 1 1 d . . . . . H7 H 1.247591 0.314775 0.009769 0.113 Uiso 1 1 calc R . . . . C14 C 0.7026(8) -0.0041(7) 0.3724(6) 0.112(2) Uani 1 1 d . . . . . H14A H 0.785775 -0.079469 0.377243 0.168 Uiso 1 1 calc GR . . . . H14B H 0.637835 -0.015695 0.317764 0.168 Uiso 1 1 calc GR . . . . H14C H 0.626192 -0.007689 0.423243 0.168 Uiso 1 1 calc GR . . . . C16 C 0.3557(6) 0.2727(10) 0.3631(5) 0.115(2) Uani 1 1 d . . . . . H16A H 0.355590 0.338985 0.313608 0.173 Uiso 1 1 calc GR . . . . H16B H 0.268832 0.299715 0.405797 0.173 Uiso 1 1 calc GR . . . . H16C H 0.332295 0.178292 0.340969 0.173 Uiso 1 1 calc GR . . . . 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 Cl1 0.1003(10) 0.1282(14) 0.0943(9) -0.0424(9) 0.0113(7) -0.0240(10) O3 0.0583(18) 0.064(2) 0.110(2) -0.0007(18) 0.0021(16) 0.0122(15) N2 0.0563(17) 0.054(2) 0.0518(16) 0.0033(15) 0.0071(14) 0.0083(15) N1 0.0587(18) 0.062(2) 0.0494(16) 0.0048(16) 0.0082(14) 0.0112(17) N3 0.083(3) 0.058(3) 0.081(2) 0.001(2) -0.017(2) -0.002(2) C13 0.056(2) 0.054(2) 0.066(2) 0.000(2) 0.0082(19) 0.008(2) O1 0.136(3) 0.052(2) 0.147(4) -0.005(2) -0.042(3) 0.001(2) C3 0.059(2) 0.060(3) 0.0500(19) -0.0009(19) 0.0123(17) 0.0119(19) C2 0.0505(19) 0.054(2) 0.0473(18) 0.0011(17) 0.0073(15) 0.0061(17) C1 0.056(2) 0.054(2) 0.0481(18) 0.0016(18) 0.0067(16) 0.0025(19) C17 0.061(2) 0.046(2) 0.062(2) -0.0051(18) -0.0006(17) 0.0123(18) C12 0.0515(19) 0.053(2) 0.0515(19) 0.0006(18) 0.0026(15) 0.0019(18) C4 0.057(2) 0.061(3) 0.0441(17) 0.0059(19) 0.0105(16) 0.0105(19) O4 0.087(2) 0.173(5) 0.079(2) -0.006(3) 0.0356(18) -0.011(3) O2 0.086(3) 0.095(3) 0.145(4) -0.007(3) 0.020(2) -0.020(2) C10 0.0510(19) 0.053(2) 0.0457(18) 0.0042(17) 0.0073(15) 0.0100(17) C5 0.062(3) 0.081(3) 0.077(3) 0.005(3) 0.018(2) 0.004(2) C15 0.055(2) 0.072(3) 0.088(3) 0.004(3) 0.013(2) 0.001(2) C9 0.071(3) 0.080(3) 0.053(2) -0.003(2) 0.008(2) 0.008(2) C18 0.063(3) 0.071(3) 0.079(3) 0.002(3) 0.011(2) 0.013(2) C20 0.099(4) 0.086(4) 0.104(4) -0.004(4) 0.000(3) 0.042(3) C11 0.062(2) 0.060(3) 0.053(2) 0.0020(19) 0.0002(18) 0.001(2) C19 0.079(3) 0.087(4) 0.107(4) -0.003(4) 0.018(3) 0.029(3) C22 0.100(4) 0.086(4) 0.070(3) 0.014(3) 0.015(2) 0.038(3) C6 0.070(3) 0.106(5) 0.103(4) 0.015(4) 0.028(3) 0.017(3) C8 0.110(4) 0.092(4) 0.071(3) -0.017(3) 0.021(3) 0.025(4) C21 0.131(5) 0.099(5) 0.089(4) 0.028(3) 0.006(4) 0.053(4) C7 0.085(4) 0.108(5) 0.089(4) 0.016(4) 0.040(3) 0.033(4) C14 0.090(4) 0.060(4) 0.186(7) 0.018(4) -0.015(4) -0.009(3) C16 0.050(3) 0.128(6) 0.168(6) 0.000(5) -0.001(3) 0.008(3) 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' Cl Cl 0.1484 0.1585 '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 N2 C17 120.1(3) . . ? C3 N2 N1 112.2(3) . . ? C3 N2 C17 127.7(3) . . ? C1 N1 N2 104.2(3) . . ? O1 N3 O2 123.6(5) . . ? O1 N3 C11 118.5(5) . . ? O2 N3 C11 117.9(4) . . ? O3 C13 C12 121.0(4) . . ? O3 C13 C14 121.2(4) . . ? C14 C13 C12 117.8(4) . . ? N2 C3 H3 126.2 . . ? N2 C3 C2 107.5(3) . . ? C2 C3 H3 126.2 . . ? C3 C2 C1 103.9(3) . . ? C3 C2 C10 130.1(3) . . ? C1 C2 C10 125.9(3) . . ? N1 C1 C2 112.1(3) . . ? N1 C1 C4 121.5(3) . . ? C2 C1 C4 126.3(4) . . ? C18 C17 N2 119.6(4) . . ? C22 C17 N2 119.5(4) . . ? C22 C17 C18 120.9(4) . . ? C13 C12 H12 106.5 . . ? C13 C12 C10 113.1(3) . . ? C13 C12 C15 109.3(3) . . ? C10 C12 H12 106.5 . . ? C15 C12 H12 106.5 . . ? C15 C12 C10 114.5(4) . . ? C5 C4 C1 120.5(4) . . ? C9 C4 C1 122.2(4) . . ? C9 C4 C5 117.3(4) . . ? C2 C10 C12 112.3(3) . . ? C2 C10 H10 106.4 . . ? C2 C10 C11 111.6(4) . . ? C12 C10 H10 106.4 . . ? C12 C10 C11 113.3(3) . . ? C11 C10 H10 106.4 . . ? C4 C5 H5 119.1 . . ? C6 C5 C4 121.8(6) . . ? C6 C5 H5 119.1 . . ? O4 C15 C12 119.4(4) . . ? O4 C15 C16 123.8(5) . . ? C16 C15 C12 116.8(5) . . ? C4 C9 Cl1 120.1(3) . . ? C4 C9 C8 121.7(5) . . ? C8 C9 Cl1 118.2(4) . . ? C17 C18 H18 120.4 . . ? C17 C18 C19 119.2(5) . . ? C19 C18 H18 120.4 . . ? C19 C20 H20 119.8 . . ? C19 C20 C21 120.4(5) . . ? C21 C20 H20 119.8 . . ? N3 C11 C10 107.9(3) . . ? N3 C11 H11A 110.1 . . ? N3 C11 H11B 110.1 . . ? C10 C11 H11A 110.1 . . ? C10 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? C18 C19 H19 119.8 . . ? C20 C19 C18 120.5(5) . . ? C20 C19 H19 119.8 . . ? C17 C22 H22 120.7 . . ? C17 C22 C21 118.7(5) . . ? C21 C22 H22 120.7 . . ? C5 C6 H6 120.1 . . ? C7 C6 C5 119.8(6) . . ? C7 C6 H6 120.1 . . ? C9 C8 H8 120.8 . . ? C7 C8 C9 118.4(6) . . ? C7 C8 H8 120.8 . . ? C20 C21 C22 120.4(6) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C6 C7 C8 120.9(5) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? 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 Cl1 C9 1.743(5) . ? O3 C13 1.195(5) . ? N2 N1 1.356(4) . ? N2 C3 1.346(5) . ? N2 C17 1.432(5) . ? N1 C1 1.325(5) . ? N3 O1 1.201(6) . ? N3 O2 1.206(6) . ? N3 C11 1.501(6) . ? C13 C12 1.527(6) . ? C13 C14 1.467(8) . ? C3 H3 0.9300 . ? C3 C2 1.369(5) . ? C2 C1 1.411(5) . ? C2 C10 1.498(6) . ? C1 C4 1.479(5) . ? C17 C18 1.372(6) . ? C17 C22 1.369(7) . ? C12 H12 0.9800 . ? C12 C10 1.533(6) . ? C12 C15 1.528(6) . ? C4 C5 1.384(6) . ? C4 C9 1.378(7) . ? O4 C15 1.189(6) . ? C10 H10 0.9800 . ? C10 C11 1.536(6) . ? C5 H5 0.9300 . ? C5 C6 1.377(7) . ? C15 C16 1.499(7) . ? C9 C8 1.397(7) . ? C18 H18 0.9300 . ? C18 C19 1.376(7) . ? C20 H20 0.9300 . ? C20 C19 1.353(9) . ? C20 C21 1.358(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C19 H19 0.9300 . ? C22 H22 0.9300 . ? C22 C21 1.389(8) . ? C6 H6 0.9300 . ? C6 C7 1.352(10) . ? C8 H8 0.9300 . ? C8 C7 1.381(9) . ? C21 H21 0.9300 . ? C7 H7 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma _refln_scale_group_code 0 -12 -1 6.09058 11.6035 12 0 -12 -2 -2.77109 9.95313 12 0 -11 0 -2.04544 6.36264 10 0 -11 -1 12.6848 16.1288 12 0 -11 1 23.4138 11.1115 10 0 -11 2 26.499 11.5774 10 0 -11 -2 24.9628 14.1295 12 0 -11 3 12.6272 7.95976 10 0 -11 -3 21.0608 12.5238 12 0 -11 4 11.401 8.70417 10 0 -11 -4 2.47865 8.33199 12 0 -11 5 -2.02525 7.2743 10 0 -11 -5 -2.27346 7.07184 12 0 -11 6 2.09329 7.0375 10 0 -11 -6 14.3874 9.76877 12 0 -11 7 10.6487 9.37871 10 0 -10 0 34.1372 12.3688 10 0 -10 -1 -1.89418 6.80463 10 0 -10 1 10.5761 7.75494 10 0 -10 2 67.6878 14.9045 10 0 -10 -2 117.041 25.4909 12 0 -10 3 32.9863 11.1268 10 0 -10 -3 42.5993 15.3353 12 0 -10 4 41.5281 13.0894 10 0 -10 -4 75.1432 19.4459 12 0 -10 -5 2.18864 7.35387 12 0 -10 5 7.68327 8.44998 10 0 -10 -5 1.37585 5.24254 16 0 -10 -6 17.2271 9.74943 12 0 -10 6 17.5606 9.62329 10 0 -10 -7 6.45552 6.48312 12 0 -10 7 1.98528 7.13261 10 0 -10 8 1.82469 6.55629 10 0 -10 -8 7.29827 6.42351 12 0 -10 -9 38.6677 11.1025 12 0 -10 9 28.8789 11.3171 10 0 -10 10 3.79284 6.8129 10 0 -9 0 -1.60815 5.77611 10 0 -9 1 136.667 19.8492 10 0 -9 -1 124.819 22.4235 10 0 -9 -2 149.389 29.5791 12 0 -9 2 121.916 18.9828 10 0 -9 3 32.1959 11.1099 10 0 -9 -3 68.85 18.5546 12 0 -9 -4 273.951 34.5158 12 0 -9 4 271.781 30.5355 10 0 -9 -5 68.5175 17.4127 12 0 -9 5 92.4944 17.9064 10 0 -9 6 49.5379 13.0884 10 0 -9 -6 54.7868 15.122 12 0 -9 -6 46.3015 10.5382 16 0 -9 7 47.9895 12.8946 10 0 -9 -7 64.1595 14.1538 12 0 -9 8 11.7967 7.44393 10 0 -9 -8 21.7201 8.29469 12 0 -9 9 -1.76934 5.50431 10 0 -9 -9 8.35022 6.37257 12 0 -9 -10 20.0486 8.72533 12 0 -9 10 1.83055 5.70068 10 0 -9 -10 5.63606 6.93517 11 0 -9 -11 -1.45348 5.83669 11 0 -9 -12 6.14242 7.30043 11 0 -8 0 486.42 35.9859 15 0 -8 0 533.267 40.7029 10 0 -8 1 2.69398 4.53561 10 0 -8 -1 11.4151 5.80097 15 0 -8 -1 13.1008 7.62717 10 0 -8 -2 145.857 15.534 15 0 -8 2 116.967 17.8072 10 0 -8 3 71.7947 14.6143 10 0 -8 -3 88.0985 20.8582 12 0 -8 -4 605.291 52.064 12 0 -8 4 604.607 46.9355 10 0 -8 5 136.679 18.9839 10 0 -8 -5 161.872 24.2754 12 0 -8 -6 178.485 19.8934 16 0 -8 -6 206.358 26.0345 12 0 -8 6 191.132 23.4542 10 0 -8 -7 151.388 18.0129 16 0 -8 -7 170.964 20.9355 12 0 -8 -8 78.8808 13.8889 12 0 -8 -9 68.9829 13.634 12 0 -8 -10 6.73056 5.67336 12 0 -8 -10 3.90287 5.48335 11 0 -8 -11 16.1848 8.41742 11 0 -8 -12 2.92299 5.25043 11 0 -8 -13 1.81864 6.53205 13 0 -8 -13 1.49637 5.3747 11 0 -8 -14 -1.56201 7.42163 11 0 -7 0 -0.85801 3.44532 15 0 -7 0 1.15856 4.87921 10 0 -7 1 878.423 55.2241 10 0 -7 -1 858.263 48.8647 15 0 -7 -1 847.619 54.2023 10 0 -7 1 736.614 48.5633 15 0 -7 2 879.856 54.2441 10 0 -7 2 828.376 49.2276 15 0 -7 -2 931.354 47.945 15 0 -7 3 1402.3 78.2314 10 0 -7 3 1388.53 75.4046 15 0 -7 -3 1169.8 68.91 15 0 -7 -4 101.41 19.0454 12 0 -7 4 87.3421 14.3293 10 0 -7 4 78.9046 13.1144 15 0 -7 -4 92.8354 12.2386 15 0 -7 -5 36.633 11.5627 12 0 -7 5 20.5843 8.71452 10 0 -7 -6 331.894 32.8198 12 0 -7 -6 353.338 27.9156 16 0 -7 -7 106.88 15.9692 12 0 -7 -7 111.24 14.758 16 0 -7 -8 141.371 17.8407 12 0 -7 -8 128.787 16.0272 16 0 -7 -9 9.51859 5.46195 12 0 -7 -10 5.89384 5.80233 11 0 -7 -11 7.66545 5.85795 11 0 -7 -12 33.3502 11.0883 11 0 -7 -12 24.8558 12.1502 13 0 -7 -13 2.7882 5.87519 11 0 -7 -13 11.6239 8.69657 13 0 -7 -14 28.4332 11.0886 13 0 -7 -14 24.0474 9.41208 11 0 -6 0 912.541 49.827 15 0 -6 0 829.368 51.9961 10 0 -6 -1 310.239 26.7826 10 0 -6 1 303.689 27.4256 10 0 -6 1 285.895 23.9404 15 0 -6 -1 346.426 24.4722 15 0 -6 1 323.694 19.6046 14 0 -6 2 145.173 11.603 14 0 -6 2 105.673 13.7629 15 0 -6 -2 120.293 12.9587 15 0 -6 2 118.918 15.8799 10 0 -6 -3 478.823 44.1069 12 0 -6 3 425.697 32.6273 15 0 -6 3 470.96 33.8429 10 0 -6 -3 450.501 30.2046 15 0 -6 4 176.582 19.5133 10 0 -6 -4 187.02 23.7383 12 0 -6 -4 145.334 15.6848 15 0 -6 4 215.957 20.2188 15 0 -6 -5 138.23 20.292 12 0 -6 -5 151.415 15.7897 15 0 -6 -5 131.397 15.1629 16 0 -6 -6 6.66297 4.86554 15 0 -6 -6 4.84852 5.56622 12 0 -6 -6 17.8249 6.10179 16 0 -6 6 15.0319 6.11789 15 0 -6 7 155.285 17.5828 17 0 -6 -7 121.881 14.6292 16 0 -6 -7 134.407 16.3021 12 0 -6 8 42.8383 8.98518 13 0 -6 -8 27.8001 7.74469 12 0 -6 -8 29.9079 7.49409 16 0 -6 -9 140.121 17.6177 11 0 -6 -9 165.914 18.8537 12 0 -6 -9 196.637 19.231 16 0 -6 -10 14.1943 7.09448 11 0 -6 -11 1.48437 7.7875 13 0 -6 -11 23.9907 8.35771 11 0 -6 -12 66.0348 13.3843 11 0 -6 -12 78.6169 15.4089 13 0 -6 -13 96.2615 16.0864 11 0 -6 -13 81.1393 16.1068 13 0 -6 -14 6.13546 6.16411 13 0 -6 -14 5.57747 7.08657 11 0 -6 -15 16.4633 9.13941 17 0 -6 -15 17.1427 9.30842 13 0 -6 -16 1.64571 6.609 17 0 -6 -16 3.02506 6.37071 13 0 -5 0 -0.90788 3.64559 10 0 -5 0 -0.2914 1.33424 14 0 -5 0 -0.62886 2.64848 15 0 -5 -1 225.094 18.2796 15 0 -5 1 247.755 15.8183 14 0 -5 1 250.479 19.4422 15 0 -5 1 248.054 21.9975 10 0 -5 -1 226.601 20.6271 10 0 -5 2 912.627 55.4843 10 0 -5 -2 1022.04 59.6232 10 0 -5 -2 1077.29 53.5843 15 0 -5 2 1006.55 55.3728 15 0 -5 3 1124.74 69.783 15 0 -5 3 1106.22 70.3821 10 0 -5 -3 1168.36 81.6093 12 0 -5 -3 1014.89 66.8492 15 0 -5 4 17.3217 5.76299 15 0 -5 4 11.0981 2.60109 9 0 -5 -4 18.419 5.83682 15 0 -5 -4 14.5342 7.33385 12 0 -5 -5 419.989 35.7329 12 0 -5 5 478.011 33.5021 15 0 -5 6 664.682 39.9991 15 0 -5 -6 550.846 36.0367 16 0 -5 6 501.508 37.669 17 0 -5 -6 709.436 41.2785 12 0 -5 -7 200.875 18.4384 16 0 -5 7 206.551 20.1903 15 0 -5 -7 212.402 19.6357 12 0 -5 7 253.872 22.0884 17 0 -5 7 201.258 18.4901 13 0 -5 -8 142.621 15.6757 12 0 -5 8 175.067 17.8495 17 0 -5 8 153.726 16.203 13 0 -5 -8 172.453 16.251 16 0 -5 9 85.874 12.2045 13 0 -5 -9 37.1885 8.63998 11 0 -5 -10 63.2543 11.4545 11 0 -5 -11 134.15 16.9119 11 0 -5 -11 113.338 17.794 13 0 -5 -12 1.36432 5.19817 13 0 -5 -12 3.54683 5.61806 11 0 -5 -13 19.912 8.40217 11 0 -5 -13 19.3115 8.25643 13 0 -5 -14 13.5809 8.41921 17 0 -5 -14 39.9514 10.7833 11 0 -5 -14 29.7301 10.3812 13 0 -5 -15 30.515 9.70514 13 0 -5 -15 20.9626 8.98092 17 0 -5 -16 8.29067 6.33073 13 0 -5 -16 3.04283 6.4118 17 0 -5 -17 19.6432 8.58391 13 0 -4 0 5275.9 201.329 10 0 -4 0 5157.89 196.286 15 0 -4 -1 336.208 25.2696 10 0 -4 1 336.277 25.3897 10 0 -4 -1 401.349 24.1971 15 0 -4 -2 325.553 22.9915 15 0 -4 2 321.075 25.2034 10 0 -4 2 366.585 24.9739 15 0 -4 -2 323.658 26.2997 10 0 -4 2 413.949 19.0842 9 0 -4 -3 1366.28 68.4523 12 0 -4 3 1248.37 58.8338 15 0 -4 -4 82.3703 9.78398 16 0 -4 4 70.5652 9.76243 15 0 -4 -5 179.366 14.8898 16 0 -4 -5 148.302 16.242 12 0 -4 5 172.28 16.2852 15 0 -4 -6 390.035 25.402 12 0 -4 6 327.601 24.8598 15 0 -4 -6 335.683 22.7334 16 0 -4 6 310.095 24.203 17 0 -4 7 141.443 16.5036 15 0 -4 -7 172.584 15.626 16 0 -4 7 163.543 16.9026 17 0 -4 7 194.326 17.2631 13 0 -4 -7 166.499 16.2785 5 0 -4 -7 157.993 15.9705 12 0 -4 -8 226.127 20.4258 11 0 -4 8 301.64 24.3953 17 0 -4 -8 258.219 21.7645 5 0 -4 8 279.427 22.344 13 0 -4 9 489.19 32.5422 17 0 -4 -9 445.709 30.0534 11 0 -4 9 427.705 28.48 13 0 -4 10 675.678 38.4124 13 0 -4 -10 541.804 37.2455 5 0 -4 -10 519.501 37.6148 11 0 -4 -10 674.486 43.9414 13 0 -4 -11 9.33717 5.44558 11 0 -4 -11 7.7448 5.0225 5 0 -4 -11 11.9526 6.62714 13 0 -4 -12 1.2221 4.65571 13 0 -4 -12 1.0869 4.97641 11 0 -4 -13 97.4671 16.8377 17 0 -4 -13 97.273 15.7749 11 0 -4 -14 14.8212 7.68021 17 0 -4 -14 20.803 8.10142 13 0 -4 -14 12.6809 7.49368 11 0 -4 -15 12.4205 6.69919 13 0 -4 -15 4.17487 5.86974 17 0 -4 -16 15.0155 8.34487 17 0 -4 -16 20.711 8.08734 13 0 -4 -17 1.60503 6.11422 17 0 -4 -17 -1.39933 5.02578 13 0 -3 0 -0.55223 2.10366 10 0 -3 0 -0.38624 1.55093 15 0 -3 0 0.37932 0.79874 14 0 -3 1 4285.33 182.222 15 0 -3 1 3891 182.957 10 0 -3 -1 4362.55 181.907 15 0 -3 -1 4035.82 183.586 10 0 -3 -2 724.316 48.4773 12 0 -3 -2 773.044 39.5729 15 0 -3 2 770.955 40.808 15 0 -3 -3 2223.39 107.049 12 0 -3 3 2179.1 102.056 15 0 -3 4 642.224 35.5079 15 0 -3 -4 680.153 38.0815 12 0 -3 -4 635.419 33.1784 16 0 -3 5 464.516 29.7125 17 0 -3 5 479.113 29.0572 13 0 -3 5 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57.8208 10.569 6 -2 3 10 53.3503 9.19967 12 -2 3 9 12.2462 6.49827 7 2 3 -9 6.74469 4.43922 8 -2 3 9 9.94528 4.97816 8 2 3 -9 11.1268 5.15613 15 2 3 -9 13.5251 4.88291 7 2 3 -9 11.9212 5.35914 6 -2 3 9 22.1444 5.79032 12 -2 3 9 11.3164 5.15599 16 2 3 -8 314.663 20.901 15 2 3 -8 297.072 21.4298 8 -2 3 8 323.308 20.8849 16 -2 3 8 374.102 23.9221 7 -2 3 8 420.671 17.341 5 -2 3 8 324.803 18.1797 6 2 3 -8 334.63 22.0216 6 -2 3 8 386.662 21.8575 12 -2 3 8 421.955 22.5235 8 -2 3 7 299.655 14.5928 5 2 3 -7 311.393 15.6626 1 -2 3 7 311.338 20.0782 16 2 3 -7 303.061 20.0348 15 -2 3 7 360.13 21.3145 8 2 3 -7 319.845 20.5999 6 2 3 -7 373.13 23.1789 8 -2 3 7 333.966 17.8133 6 -2 3 7 289.861 18.4443 12 -2 3 6 314.762 16.1072 5 2 3 -6 378.941 15.3808 5 -2 3 6 451.507 22.9108 16 2 3 -6 446.542 23.7512 15 -2 3 6 387.206 22.8634 7 2 3 -6 487.331 25.3075 6 2 3 -6 390.388 17.7678 1 -2 3 6 581.255 22.9449 6 2 3 -6 0.89343 6.07431 3 -2 3 6 440.236 22.5493 12 -2 3 6 55.5084 10.3437 10 2 3 -6 510.17 26.4622 8 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28.8339 6 2 3 -1 505.806 27.7959 5 2 3 0 14298.4 182.009 10 2 3 0 13304.1 186.454 9 -2 3 0 12375.7 185.956 4 -2 3 0 13225.6 175.705 15 2 3 0 13523.7 183.059 1 -2 3 0 12600.3 186.556 14 2 3 0 13732.3 178.596 6 2 3 0 15304.7 185.479 5 -2 3 -1 628.998 32.3127 9 2 3 1 684.234 38.0122 9 2 3 1 728.247 37.431 1 -2 3 -1 705.644 36.942 15 2 3 1 670.317 37.1584 5 2 3 1 617.683 36.1471 10 2 3 2 2746.06 133.099 9 2 3 2 2143.99 128.033 7 -2 3 -2 2516.15 131.151 15 2 3 2 4225.53 128.808 14 2 3 2 2747.94 131.587 1 2 3 2 3031.42 128.172 6 2 3 2 2576.72 132.381 5 2 3 2 3220.97 134.931 10 2 3 2 3695.03 141.291 3 2 3 3 2370.2 99.8611 7 2 3 3 1997.4 98.638 1 -2 3 -3 1919.99 99.9983 15 2 3 3 2216.64 101.234 5 2 3 3 2492.49 106.225 3 2 3 4 587.194 32.2204 5 -2 3 -4 524.134 31.8453 15 2 3 4 590.597 30.244 1 2 3 5 2918.23 156.098 7 2 3 5 3718.41 159.316 5 -2 3 -5 4323.11 163.635 15 2 3 5 3506.85 156.044 1 2 3 6 241.67 18.3565 1 -2 3 -6 281.066 23.0531 15 2 3 6 290.6 21.5569 5 2 3 7 180.414 12.0485 1 2 3 7 221.917 14.8935 7 -2 3 -7 200.027 17.4931 15 -2 3 -8 232.634 19.8193 15 2 3 8 261.487 18.041 5 -2 3 -9 313.348 26.553 15 -2 3 -9 250.944 23.7074 17 2 3 9 261.436 22.293 5 -2 3 -10 224.408 23.1147 15 -2 3 -10 266.688 24.1988 17 2 3 10 213.702 20.0438 5 -2 3 -11 3.91008 4.30442 5 2 3 11 3.57992 4.25683 5 -2 3 -11 3.49176 4.6779 17 -2 3 -11 13.9575 7.38611 15 -2 3 -12 19.3466 7.24832 5 -2 3 -12 17.6979 7.57631 17 -2 3 -12 24.4797 8.50215 15 -2 3 -13 23.1876 9.38013 17 -2 3 -13 24.4013 8.98454 15 -2 3 -14 14.639 8.15739 17 -2 3 -14 36.4177 10.7694 15 -2 3 -15 4.71991 7.47899 17 -2 3 -15 11.3021 6.57924 7 -2 3 -15 3.19734 4.97844 15 -2 3 -16 43.389 12.7055 17 -2 3 -16 60.5245 14.4691 15 -2 3 -16 47.0292 12.0002 7 -2 3 -17 4.4261 6.75573 7 -2 3 -17 1.75753 5.46782 15 2 4 -17 13.4085 7.58797 6 2 4 -16 -1.41786 5.97153 6 2 4 -15 24.5707 8.89791 6 2 4 -14 9.53394 6.70129 15 2 4 -14 1.19654 5.04335 7 2 4 -14 6.53126 6.20958 6 2 4 -13 60.9518 11.7178 7 2 4 -13 76.9472 13.7984 6 2 4 -13 83.818 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12 2 4 -6 288.12 22.9879 8 -2 4 6 235.55 21.632 10 2 4 -6 301.058 23.7294 3 2 4 -5 33.4756 5.46667 5 -2 4 5 37.142 7.81563 10 -2 4 5 30.7722 6.80145 5 2 4 -5 39.1385 8.2452 3 2 4 -5 44.1615 8.5036 8 2 4 -5 34.4823 7.37461 15 2 4 -5 32.1268 7.09611 6 2 4 -5 39.8993 6.53125 1 -2 4 5 32.6535 9.24912 12 -2 4 4 993.942 60.6702 10 2 4 -4 968.976 58.8386 3 2 4 -4 989.473 53.2729 5 2 4 -4 1100.35 60.2302 15 2 4 -4 1091.76 57.8685 6 -2 4 4 1337.84 68.7235 12 2 4 -4 1185.09 56.7847 1 2 4 -4 1369.77 61.8708 8 2 4 -3 3376.69 149.719 5 2 4 -3 3704.81 156.951 3 2 4 -3 3384 154.162 8 2 4 -3 3323.45 156.789 15 2 4 -3 3375.08 152.941 6 -2 4 3 3911.37 154.879 14 2 4 -3 3560.72 152.349 1 2 4 -2 43.0997 5.92587 5 2 4 -2 50.4057 8.88376 3 -2 4 2 38.0897 7.25899 10 2 4 -2 34.0865 6.00924 6 2 4 -2 37.2281 7.57117 15 -2 4 2 43.8264 7.14939 14 -2 4 2 18.3186 3.83878 15 2 4 -2 40.8705 6.47443 1 2 4 -1 325.642 25.2489 3 2 4 -1 372.544 22.2642 8 2 4 -1 298.173 20.2631 6 -2 4 1 348.946 22.6226 14 2 4 -1 289.539 19.8819 5 -2 4 1 265.696 18.4788 15 2 4 -1 361.656 22.441 1 2 4 0 1301.3 59.541 1 2 4 0 1169.65 58.6185 10 2 4 0 1316.03 64.5648 3 -2 4 0 1178.45 56.5054 15 2 4 0 1059 55.8603 8 2 4 0 1040.09 58.1205 9 2 4 0 1221.25 56.4258 6 2 4 0 1116.45 57.2386 5 2 4 1 701.144 40.6247 10 2 4 1 864.789 45.0632 3 2 4 1 652.207 38.9369 9 2 4 1 783.412 40.114 1 -2 4 -1 776.665 39.251 15 2 4 1 770.259 36.7158 6 2 4 1 593.118 35.5539 8 2 4 1 767.676 40.1646 5 2 4 2 3177.7 119.893 3 2 4 2 3143.15 115.376 9 2 4 2 1712.31 110.358 5 -2 4 -2 2388.7 112.952 15 2 4 2 2412.34 106.938 6 2 4 2 2688.56 113.2 1 2 4 2 2184.07 111.726 10 2 4 3 4270.01 158.641 3 2 4 3 4110.29 151.348 7 2 4 3 3801.04 152.046 1 2 4 3 3589.79 154.095 5 -2 4 -3 3558.99 154.403 15 2 4 3 4215.47 156.66 10 2 4 4 179.337 16.2146 3 -2 4 -4 143.442 14.9411 15 2 4 4 86.1878 10.7841 7 2 4 4 172.508 13.791 1 2 4 4 160.77 15.0447 5 2 4 4 105.08 13.3834 10 -2 4 -5 344.255 26.9141 15 2 4 5 393.533 26.859 7 2 4 5 339.252 23.6944 1 2 4 5 402.032 26.9691 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6 475.909 34.9957 10 -2 6 -7 829.748 48.2204 15 2 6 7 768.788 43.9589 7 -2 6 -8 18.5035 8.40934 15 2 6 8 13.8698 6.52045 7 2 6 8 9.37118 6.3647 3 -2 6 -9 72.0987 14.7841 15 -2 6 -10 238.493 26.7745 15 -2 6 -11 33.7638 11.4546 15 -2 6 -12 44.0414 12.6767 15 -2 6 -13 126.298 20.8835 15 -2 6 -14 39.0631 13.0402 15 -2 6 -15 -1.93879 6.03087 15 2 7 -14 1.65929 5.5749 15 2 7 -14 1.49756 5.70519 6 2 7 -13 6.45842 6.79989 15 2 7 -13 -1.45079 5.52671 6 2 7 -12 103.185 17.4635 15 2 7 -12 14.0037 8.04684 6 2 7 -11 5.99147 6.01486 15 2 7 -11 -1.33812 4.49582 6 2 7 -10 72.0337 14.1368 15 2 7 -9 57.687 12.862 15 2 7 -8 302.977 27.3522 3 2 7 -8 318.774 30.3403 15 2 7 -7 204.852 21.8547 3 2 7 -7 222.141 24.5047 15 2 7 -6 27.5295 9.52003 15 2 7 -6 41.8935 10.3662 3 2 7 -5 403.654 31.6855 3 2 7 -5 361.929 30.5578 8 2 7 -5 353.221 32.3657 15 2 7 -4 30.7296 9.0443 15 2 7 -4 22.6025 8.19184 3 2 7 -3 245.874 20.4987 5 2 7 -3 249.972 23.8996 3 2 7 -3 218.28 24.9415 15 2 7 -2 41.0358 7.95707 5 2 7 -2 54.3897 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