#------------------------------------------------------------------------------ #$Date: 2021-01-14 03:37:48 +0200 (Thu, 14 Jan 2021) $ #$Revision: 260924 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/00/1560077.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_1560077 loop_ _publ_author_name 'Diment, Wilfred T.' 'St\"o\&ser, Tim' 'Kerr, Ryan W. F.' 'Phanopoulos, Andreas' 'Durr, Christopher B.' 'Williams, Charlotte K.' _publ_section_title ; Ortho-vanillin derived Al(iii) and Co(iii) catalyst systems for switchable catalysis using \e-decalactone, phthalic anhydride and cyclohexene oxide ; _journal_name_full 'Catalysis Science & Technology' _journal_paper_doi 10.1039/D0CY02164D _journal_year 2021 _chemical_formula_moiety 'C23 H29 Al N2 O4' _chemical_formula_sum 'C23 H29 Al N2 O4' _chemical_formula_weight 424.46 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_date 2020-10-23 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-11-02 deposited with the CCDC. 2020-12-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.86900(10) _cell_length_b 15.7511(2) _cell_length_c 17.6113(3) _cell_measurement_reflns_used 6530 _cell_measurement_temperature 149.98(18) _cell_measurement_theta_max 75.7260 _cell_measurement_theta_min 3.7280 _cell_volume 2182.84(5) _computing_cell_refinement 'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 149.98(18) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.4102 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.990 _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 26.00 59.00 1.00 2.00 -- 42.66 -19.00 60.00 33 2 \w -93.00 -50.00 1.00 2.00 -- -42.66 127.00 101.00 43 3 \w -111.00 -24.00 1.00 2.00 -- -42.66 -57.00-150.00 87 4 \w 47.00 85.00 1.00 2.00 -- 111.00 -45.00 150.00 38 5 \w 38.00 90.00 1.00 2.00 -- 111.00 -30.00 90.00 52 6 \w 58.00 121.00 1.00 2.00 -- 111.00-125.00 120.00 63 7 \w 37.00 73.00 1.00 2.00 -- 111.00 -30.00-180.00 36 8 \w 150.00 176.00 1.00 2.00 -- 111.00 125.00 -30.00 26 9 \w 137.00 174.00 1.00 2.00 -- 111.00 127.00 101.00 37 10 \w 105.00 131.00 1.00 2.00 -- 111.00 127.00 101.00 26 11 \w 94.00 169.00 1.00 2.00 -- 111.00 125.00 120.00 75 12 \w 98.00 124.00 1.00 2.00 -- 111.00 125.00 -30.00 26 13 \w -23.00 14.00 1.00 2.00 -- -42.66 77.00 0.00 37 14 \w 46.00 81.00 1.00 2.00 -- 111.00 -77.00 -60.00 35 15 \w 145.00 173.00 1.00 2.00 -- 111.00 125.00-150.00 28 16 \w 86.00 141.00 1.00 2.00 -- 111.00 61.00 90.00 55 17 \w 78.00 99.00 1.00 2.00 -- 111.00 -95.00 0.00 21 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0855342000 _diffrn_orient_matrix_UB_12 0.0105132000 _diffrn_orient_matrix_UB_13 -0.0781158000 _diffrn_orient_matrix_UB_21 -0.1756425000 _diffrn_orient_matrix_UB_22 0.0016011000 _diffrn_orient_matrix_UB_23 0.0386889000 _diffrn_orient_matrix_UB_31 0.0121773000 _diffrn_orient_matrix_UB_32 0.0971886000 _diffrn_orient_matrix_UB_33 0.0078605000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_unetI/netI 0.0358 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 9972 _diffrn_reflns_point_group_measured_fraction_full 0.951 _diffrn_reflns_point_group_measured_fraction_max 0.929 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 75.942 _diffrn_reflns_theta_min 3.765 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.75048 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.292 _exptl_crystal_description cube _exptl_crystal_F_000 904 _exptl_crystal_size_max 0.241 _exptl_crystal_size_mid 0.174 _exptl_crystal_size_min 0.166 _refine_diff_density_max 0.308 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.050 _refine_ls_abs_structure_details ; Flack x determined using 1541 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 276 _refine_ls_number_reflns 4237 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0362 _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^)+(0.0601P)^2^+0.4573P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0957 _refine_ls_wR_factor_ref 0.0980 _reflns_Friedel_coverage 0.644 _reflns_Friedel_fraction_full 0.884 _reflns_Friedel_fraction_max 0.848 _reflns_number_gt 4049 _reflns_number_total 4237 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cy02164d2.cif _cod_data_source_block 062ckw17 _cod_database_code 1560077 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'Al1 C23 H29 N2 O4' _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_max 0.842 _shelx_estimated_absorpt_t_min 0.782 _reflns_odcompleteness_completeness 99.92 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 74.33 _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 Secondary CH2 refined with riding coordinates: C9(H9A,H9B), C13(H13A,H13B), C22(H22A,H22B) 2.b Aromatic/amide H refined with riding coordinates: C5(H5), C6(H6), C7(H7), C8(H8), C14(H14), C16(H16), C17(H17), C18(H18) 2.c Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C21(H21A,H21B, H21C), C23(H23A,H23B,H23C) ; _shelx_res_file ; TITL shelxt_a.res in P2(1)2(1)2(1) 062ckw17.res created by SHELXL-2018/3 at 17:27:21 on 23-Oct-2020 CELL 1.54184 7.869 15.7511 17.6113 90 90 90 ZERR 4 0.0001 0.0002 0.0003 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Al N O UNIT 92 116 4 8 16 L.S. 99 PLAN 20 SIZE 0.166 0.174 0.241 TEMP -123 BOND $H LIST 4 fmap 2 acta MERG 2 OMIT -4 1 18 OMIT -4 2 18 OMIT 3 18 2 OMIT -1 10 18 OMIT -3 10 16 OMIT -4 3 18 OMIT 7 12 3 OMIT 4 17 2 REM REM REM WGHT 0.060100 0.457300 FVAR 6.81819 C1 1 0.265585 0.706272 0.546459 11.00000 0.03248 0.03921 = 0.02216 -0.00178 0.00660 0.00325 AFIX 137 H1A 2 0.300962 0.760670 0.568359 11.00000 -1.50000 H1B 2 0.302233 0.659867 0.579713 11.00000 -1.50000 H1C 2 0.141562 0.705182 0.541491 11.00000 -1.50000 AFIX 0 C2 1 0.307365 0.757965 0.420937 11.00000 0.01839 0.02236 = 0.02310 -0.00191 -0.00004 -0.00249 C3 1 0.388878 0.746340 0.349673 11.00000 0.01955 0.02079 = 0.02225 -0.00480 -0.00227 -0.00163 C4 1 0.365357 0.808922 0.293783 11.00000 0.02178 0.02091 = 0.02611 -0.00201 -0.00010 -0.00332 C5 1 0.259457 0.879575 0.307559 11.00000 0.02753 0.02055 = 0.03511 0.00275 0.00171 0.00215 AFIX 43 H5 2 0.243920 0.921351 0.269276 11.00000 -1.20000 AFIX 0 C6 1 0.179242 0.887877 0.376012 11.00000 0.03001 0.02255 = 0.04210 -0.00366 0.00840 0.00266 AFIX 43 H6 2 0.106217 0.934901 0.384754 11.00000 -1.20000 AFIX 0 C7 1 0.204119 0.827274 0.433553 11.00000 0.02486 0.02562 = 0.03098 -0.00521 0.00797 -0.00160 AFIX 43 H7 2 0.149605 0.834099 0.481295 11.00000 -1.20000 AFIX 0 C8 1 0.454431 0.805376 0.222042 11.00000 0.02543 0.02061 = 0.02367 0.00204 -0.00285 -0.00032 AFIX 43 H8 2 0.441173 0.852001 0.188340 11.00000 -1.20000 AFIX 0 C9 1 0.633111 0.753390 0.125953 11.00000 0.03206 0.02800 = 0.01892 0.00133 0.00161 0.00235 AFIX 23 H9A 2 0.597994 0.808113 0.103185 11.00000 -1.20000 H9B 2 0.594439 0.707302 0.091860 11.00000 -1.20000 AFIX 0 C10 1 0.826651 0.750868 0.131780 11.00000 0.03114 0.02909 = 0.02038 -0.00010 0.00325 -0.00021 C11 1 0.893891 0.819391 0.185289 11.00000 0.03755 0.03477 = 0.03366 -0.00416 0.00524 -0.00642 AFIX 137 H11A 2 1.018257 0.816672 0.186939 11.00000 -1.50000 H11B 2 0.848112 0.810089 0.236366 11.00000 -1.50000 H11C 2 0.858447 0.875378 0.166895 11.00000 -1.50000 AFIX 0 C12 1 0.899467 0.764277 0.051685 11.00000 0.04045 0.03788 = 0.02502 0.00342 0.00930 0.00125 AFIX 137 H12A 2 0.863814 0.819875 0.032447 11.00000 -1.50000 H12B 2 0.857185 0.719653 0.017823 11.00000 -1.50000 H12C 2 1.023829 0.761853 0.053720 11.00000 -1.50000 AFIX 0 C13 1 0.883984 0.662716 0.157635 11.00000 0.02664 0.03353 = 0.02415 0.00017 0.00542 0.00404 AFIX 23 H13A 2 0.848651 0.620773 0.118859 11.00000 -1.20000 H13B 2 1.009679 0.661977 0.159944 11.00000 -1.20000 AFIX 0 C14 1 0.928909 0.619399 0.283535 11.00000 0.02087 0.02415 = 0.02884 -0.00030 0.00225 0.00035 AFIX 43 H14 2 1.042462 0.636630 0.273633 11.00000 -1.20000 AFIX 0 C15 1 0.896767 0.577563 0.354905 11.00000 0.02308 0.02185 = 0.02372 -0.00178 -0.00090 0.00174 C16 1 1.028083 0.573551 0.408912 11.00000 0.02448 0.02873 = 0.03340 -0.00025 -0.00367 -0.00157 AFIX 43 H16 2 1.131203 0.603433 0.400391 11.00000 -1.20000 AFIX 0 C17 1 1.007665 0.526506 0.474014 11.00000 0.02610 0.03644 = 0.02825 0.00209 -0.00802 0.00270 AFIX 43 H17 2 1.094664 0.525014 0.511390 11.00000 -1.20000 AFIX 0 C18 1 0.857347 0.480971 0.484429 11.00000 0.03092 0.02774 = 0.02547 0.00395 0.00092 0.00507 AFIX 43 H18 2 0.843930 0.447690 0.529015 11.00000 -1.20000 AFIX 0 C19 1 0.728687 0.482961 0.432134 11.00000 0.02517 0.01772 = 0.02788 -0.00128 0.00006 0.00237 C20 1 0.742159 0.532820 0.365315 11.00000 0.02330 0.01657 = 0.02215 -0.00485 0.00089 0.00514 C21 1 0.432883 0.481200 0.455471 11.00000 0.02690 0.03639 = 0.04392 -0.00087 0.00475 -0.00184 AFIX 137 H21A 2 0.437955 0.510555 0.504482 11.00000 -1.50000 H21B 2 0.335597 0.442359 0.455030 11.00000 -1.50000 H21C 2 0.420092 0.522998 0.414651 11.00000 -1.50000 AFIX 0 C22 1 0.409792 0.574053 0.181216 11.00000 0.03570 0.04613 = 0.02139 0.00050 -0.00880 -0.01200 AFIX 23 H22A 2 0.327778 0.617985 0.164685 11.00000 -1.20000 H22B 2 0.477389 0.557829 0.136081 11.00000 -1.20000 AFIX 0 C23 1 0.309137 0.496791 0.206084 11.00000 0.03178 0.03023 = 0.05227 -0.00278 -0.01147 -0.00220 AFIX 137 H23A 2 0.386189 0.448418 0.212364 11.00000 -1.50000 H23B 2 0.223643 0.483214 0.167486 11.00000 -1.50000 H23C 2 0.252537 0.508818 0.254470 11.00000 -1.50000 AFIX 0 N1 4 0.550486 0.743659 0.200418 11.00000 0.02409 0.02376 = 0.01891 0.00025 -0.00126 -0.00030 N2 4 0.817001 0.635534 0.231854 11.00000 0.02237 0.02360 = 0.02228 0.00052 0.00182 0.00319 O1 5 0.341350 0.696214 0.473336 11.00000 0.02433 0.02971 = 0.01982 -0.00134 0.00221 0.00282 O2 5 0.484725 0.678517 0.339422 11.00000 0.03033 0.02542 = 0.01906 -0.00028 0.00069 0.00788 O3 5 0.620384 0.533864 0.314711 11.00000 0.02267 0.02032 = 0.02227 -0.00242 -0.00409 0.00021 O4 5 0.586183 0.434027 0.444159 11.00000 0.02661 0.02341 = 0.03679 0.00391 0.00152 -0.00216 AL1 3 0.566514 0.627069 0.255681 11.00000 0.02001 0.02093 = 0.01744 -0.00168 -0.00111 0.00094 HKLF 4 REM shelxt_a.res in P2(1)2(1)2(1) REM wR2 = 0.0980, GooF = S = 1.039, Restrained GooF = 1.039 for all data REM R1 = 0.0362 for 4049 Fo > 4sig(Fo) and 0.0391 for all 4237 data REM 276 parameters refined using 0 restraints END WGHT 0.0604 0.4297 REM Highest difference peak 0.308, deepest hole -0.248, 1-sigma level 0.050 Q1 1 0.4299 0.5432 0.4603 11.00000 0.05 0.31 Q2 1 0.3622 0.4764 0.4100 11.00000 0.05 0.22 Q3 1 0.5450 0.6915 0.2278 11.00000 0.05 0.21 Q4 1 0.5928 0.6667 0.3729 11.00000 0.05 0.20 Q5 1 0.3626 0.4585 0.4976 11.00000 0.05 0.18 Q6 1 0.7432 0.6587 -0.0479 11.00000 0.05 0.17 Q7 1 0.4806 0.6416 0.3673 11.00000 0.05 0.16 Q8 1 0.5088 0.5865 0.2132 11.00000 0.05 0.16 Q9 1 0.4840 0.6900 0.4751 11.00000 0.05 0.15 Q10 1 0.8505 0.7079 0.1418 11.00000 0.05 0.15 Q11 1 0.3269 0.7547 0.1264 11.00000 0.05 0.15 Q12 1 0.3902 0.6053 0.3488 11.00000 0.05 0.15 Q13 1 0.4090 0.6022 0.1360 11.00000 0.05 0.15 Q14 1 0.5865 0.5709 0.2807 11.00000 0.05 0.14 Q15 1 0.5454 0.4987 0.2949 11.00000 0.05 0.14 Q16 1 0.2757 0.8054 0.4294 11.00000 0.05 0.14 Q17 1 0.3742 0.6417 0.4576 11.00000 0.05 0.14 Q18 1 0.2096 0.6594 0.5592 11.00000 0.05 0.14 Q19 1 0.4062 0.7965 0.3345 11.00000 0.05 0.14 Q20 1 0.4726 0.5328 0.3259 11.00000 0.05 0.14 ; _shelx_res_checksum 22465 _ins_header ; TITL 062ckw17 in P2(1)2(1)2(1) REM P2(1)2(1)2(1) (#19 in standard setting) CELL 1.54184 7.868963 15.751133 17.611285 90.0000 90.0000 90.0000 ZERR 4.00 0.000138 0.000208 0.000267 0.0000 0.0000 0.0000 LATT -1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H N O Al UNIT 92.00 116.00 8.00 16.00 4.00 TREF HKLF 4 END ; _olex2_submission_original_sample_id 062ckw17 _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 - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.269 _oxdiff_exptl_absorpt_empirical_full_min 0.806 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -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 C1 C 0.2656(4) 0.70627(17) 0.54646(14) 0.0313(6) Uani 1 1 d . . . . . H1A H 0.300962 0.760670 0.568359 0.047 Uiso 1 1 calc GR . . . . H1B H 0.302233 0.659867 0.579713 0.047 Uiso 1 1 calc GR . . . . H1C H 0.141562 0.705182 0.541491 0.047 Uiso 1 1 calc GR . . . . C2 C 0.3074(3) 0.75797(15) 0.42094(13) 0.0213(5) Uani 1 1 d . . . . . C3 C 0.3889(3) 0.74634(14) 0.34967(13) 0.0209(5) Uani 1 1 d . . . . . C4 C 0.3654(3) 0.80892(14) 0.29378(14) 0.0229(5) Uani 1 1 d . . . . . C5 C 0.2595(3) 0.87958(15) 0.30756(15) 0.0277(5) Uani 1 1 d . . . . . H5 H 0.243920 0.921351 0.269276 0.033 Uiso 1 1 calc R . . . . C6 C 0.1792(4) 0.88788(15) 0.37601(17) 0.0316(6) Uani 1 1 d . . . . . H6 H 0.106217 0.934901 0.384754 0.038 Uiso 1 1 calc R . . . . C7 C 0.2041(3) 0.82727(16) 0.43355(15) 0.0272(5) Uani 1 1 d . . . . . H7 H 0.149605 0.834099 0.481295 0.033 Uiso 1 1 calc R . . . . C8 C 0.4544(3) 0.80538(14) 0.22204(13) 0.0232(5) Uani 1 1 d . . . . . H8 H 0.441173 0.852001 0.188340 0.028 Uiso 1 1 calc R . . . . C9 C 0.6331(3) 0.75339(16) 0.12595(13) 0.0263(5) Uani 1 1 d . . . . . H9A H 0.597994 0.808113 0.103185 0.032 Uiso 1 1 calc R . . . . H9B H 0.594439 0.707302 0.091860 0.032 Uiso 1 1 calc R . . . . C10 C 0.8267(4) 0.75087(16) 0.13178(14) 0.0269(5) Uani 1 1 d . . . . . C11 C 0.8939(4) 0.81939(17) 0.18529(16) 0.0353(6) Uani 1 1 d . . . . . H11A H 1.018257 0.816672 0.186939 0.053 Uiso 1 1 calc GR . . . . H11B H 0.848112 0.810089 0.236366 0.053 Uiso 1 1 calc GR . . . . H11C H 0.858447 0.875378 0.166895 0.053 Uiso 1 1 calc GR . . . . C12 C 0.8995(4) 0.76428(18) 0.05169(14) 0.0344(6) Uani 1 1 d . . . . . H12A H 0.863814 0.819875 0.032447 0.052 Uiso 1 1 calc GR . . . . H12B H 0.857185 0.719653 0.017823 0.052 Uiso 1 1 calc GR . . . . H12C H 1.023829 0.761853 0.053720 0.052 Uiso 1 1 calc GR . . . . C13 C 0.8840(4) 0.66272(16) 0.15763(14) 0.0281(5) Uani 1 1 d . . . . . H13A H 0.848651 0.620773 0.118859 0.034 Uiso 1 1 calc R . . . . H13B H 1.009679 0.661977 0.159944 0.034 Uiso 1 1 calc R . . . . C14 C 0.9289(3) 0.61940(14) 0.28354(14) 0.0246(5) Uani 1 1 d . . . . . H14 H 1.042462 0.636630 0.273633 0.030 Uiso 1 1 calc R . . . . C15 C 0.8968(3) 0.57756(14) 0.35491(13) 0.0229(5) Uani 1 1 d . . . . . C16 C 1.0281(3) 0.57355(16) 0.40891(15) 0.0289(5) Uani 1 1 d . . . . . H16 H 1.131203 0.603433 0.400391 0.035 Uiso 1 1 calc R . . . . C17 C 1.0077(3) 0.52651(17) 0.47401(15) 0.0303(6) Uani 1 1 d . . . . . H17 H 1.094664 0.525014 0.511390 0.036 Uiso 1 1 calc R . . . . C18 C 0.8573(3) 0.48097(16) 0.48443(15) 0.0280(5) Uani 1 1 d . . . . . H18 H 0.843930 0.447690 0.529015 0.034 Uiso 1 1 calc R . . . . C19 C 0.7287(3) 0.48296(14) 0.43213(14) 0.0236(5) Uani 1 1 d . . . . . C20 C 0.7422(3) 0.53282(13) 0.36532(13) 0.0207(4) Uani 1 1 d . . . . . C21 C 0.4329(4) 0.48120(18) 0.45547(17) 0.0357(6) Uani 1 1 d . . . . . H21A H 0.437955 0.510555 0.504482 0.054 Uiso 1 1 calc GR . . . . H21B H 0.335597 0.442359 0.455030 0.054 Uiso 1 1 calc GR . . . . H21C H 0.420092 0.522998 0.414651 0.054 Uiso 1 1 calc GR . . . . C22 C 0.4098(4) 0.57405(19) 0.18122(14) 0.0344(6) Uani 1 1 d . . . . . H22A H 0.327778 0.617985 0.164685 0.041 Uiso 1 1 calc R . . . . H22B H 0.477389 0.557829 0.136081 0.041 Uiso 1 1 calc R . . . . C23 C 0.3091(4) 0.49679(18) 0.20608(19) 0.0381(7) Uani 1 1 d . . . . . H23A H 0.386189 0.448418 0.212364 0.057 Uiso 1 1 calc GR . . . . H23B H 0.223643 0.483214 0.167486 0.057 Uiso 1 1 calc GR . . . . H23C H 0.252537 0.508818 0.254470 0.057 Uiso 1 1 calc GR . . . . N1 N 0.5505(3) 0.74366(12) 0.20042(11) 0.0223(4) Uani 1 1 d . . . . . N2 N 0.8170(3) 0.63553(12) 0.23185(11) 0.0228(4) Uani 1 1 d . . . . . O1 O 0.3413(2) 0.69621(11) 0.47334(9) 0.0246(4) Uani 1 1 d . . . . . O2 O 0.4847(2) 0.67852(10) 0.33942(9) 0.0249(4) Uani 1 1 d . . . . . O3 O 0.6204(2) 0.53386(10) 0.31471(9) 0.0218(3) Uani 1 1 d . . . . . O4 O 0.5862(2) 0.43403(11) 0.44416(10) 0.0289(4) Uani 1 1 d . . . . . Al1 Al 0.56651(9) 0.62707(4) 0.25568(4) 0.01946(16) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0325(14) 0.0392(14) 0.0222(11) -0.0018(10) 0.0066(11) 0.0033(12) C2 0.0184(11) 0.0224(10) 0.0231(11) -0.0019(9) 0.0000(9) -0.0025(9) C3 0.0195(11) 0.0208(10) 0.0223(10) -0.0048(8) -0.0023(9) -0.0016(9) C4 0.0218(11) 0.0209(10) 0.0261(11) -0.0020(9) -0.0001(10) -0.0033(9) C5 0.0275(12) 0.0205(10) 0.0351(12) 0.0027(9) 0.0017(11) 0.0021(10) C6 0.0300(13) 0.0225(11) 0.0421(14) -0.0037(10) 0.0084(12) 0.0027(10) C7 0.0249(12) 0.0256(11) 0.0310(12) -0.0052(10) 0.0080(10) -0.0016(10) C8 0.0254(12) 0.0206(10) 0.0237(10) 0.0020(8) -0.0028(10) -0.0003(9) C9 0.0321(13) 0.0280(11) 0.0189(10) 0.0013(9) 0.0016(10) 0.0024(10) C10 0.0311(14) 0.0291(11) 0.0204(11) -0.0001(9) 0.0033(10) -0.0002(11) C11 0.0376(15) 0.0348(13) 0.0337(13) -0.0042(11) 0.0052(12) -0.0064(12) C12 0.0405(16) 0.0379(14) 0.0250(12) 0.0034(10) 0.0093(12) 0.0013(13) C13 0.0266(13) 0.0335(12) 0.0242(11) 0.0002(9) 0.0054(10) 0.0040(10) C14 0.0209(11) 0.0242(10) 0.0288(11) -0.0003(9) 0.0023(10) 0.0004(9) C15 0.0231(12) 0.0219(10) 0.0237(10) -0.0018(8) -0.0009(9) 0.0017(9) C16 0.0245(13) 0.0287(12) 0.0334(13) -0.0003(10) -0.0037(10) -0.0016(10) C17 0.0261(13) 0.0364(13) 0.0283(12) 0.0021(11) -0.0080(10) 0.0027(11) C18 0.0309(13) 0.0277(12) 0.0255(11) 0.0039(10) 0.0009(11) 0.0051(10) C19 0.0252(13) 0.0177(10) 0.0279(12) -0.0013(9) 0.0001(10) 0.0024(9) C20 0.0233(11) 0.0166(9) 0.0221(10) -0.0048(8) 0.0009(9) 0.0051(9) C21 0.0269(13) 0.0364(13) 0.0439(15) -0.0009(12) 0.0048(13) -0.0018(12) C22 0.0357(15) 0.0461(15) 0.0214(11) 0.0005(10) -0.0088(11) -0.0120(13) C23 0.0318(14) 0.0302(13) 0.0523(18) -0.0028(12) -0.0115(14) -0.0022(12) N1 0.0241(10) 0.0238(9) 0.0189(9) 0.0003(7) -0.0013(8) -0.0003(8) N2 0.0224(10) 0.0236(9) 0.0223(9) 0.0005(7) 0.0018(8) 0.0032(8) O1 0.0243(9) 0.0297(8) 0.0198(8) -0.0013(7) 0.0022(7) 0.0028(7) O2 0.0303(9) 0.0254(8) 0.0191(7) -0.0003(6) 0.0007(7) 0.0079(7) O3 0.0227(8) 0.0203(7) 0.0223(7) -0.0024(6) -0.0041(7) 0.0002(7) O4 0.0266(10) 0.0234(8) 0.0368(9) 0.0039(7) 0.0015(8) -0.0022(8) Al1 0.0200(3) 0.0209(3) 0.0174(3) -0.0017(2) -0.0011(3) 0.0009(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? C7 C2 C3 120.7(2) . . ? O1 C2 C3 114.6(2) . . ? O1 C2 C7 124.7(2) . . ? C4 C3 C2 117.9(2) . . ? O2 C3 C2 118.9(2) . . ? O2 C3 C4 123.2(2) . . ? C3 C4 C5 120.7(2) . . ? C3 C4 C8 121.4(2) . . ? C5 C4 C8 117.8(2) . . ? C4 C5 H5 120.0 . . ? C6 C5 C4 120.0(2) . . ? C6 C5 H5 120.0 . . ? C5 C6 H6 119.8 . . ? C5 C6 C7 120.4(2) . . ? C7 C6 H6 119.8 . . ? C2 C7 C6 120.2(2) . . ? C2 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C4 C8 H8 117.6 . . ? N1 C8 C4 124.9(2) . . ? N1 C8 H8 117.6 . . ? H9A C9 H9B 107.9 . . ? C10 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? N1 C9 H9A 109.2 . . ? N1 C9 H9B 109.2 . . ? N1 C9 C10 112.2(2) . . ? C9 C10 C11 111.6(2) . . ? C9 C10 C12 107.9(2) . . ? C9 C10 C13 109.7(2) . . ? C11 C10 C12 109.9(2) . . ? C11 C10 C13 110.8(2) . . ? C13 C10 C12 106.7(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 108.5 . . ? C10 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? N2 C13 C10 115.0(2) . . ? N2 C13 H13A 108.5 . . ? N2 C13 H13B 108.5 . . ? C15 C14 H14 117.1 . . ? N2 C14 H14 117.1 . . ? N2 C14 C15 125.8(2) . . ? C16 C15 C14 118.8(2) . . ? C16 C15 C20 121.4(2) . . ? C20 C15 C14 119.4(2) . . ? C15 C16 H16 119.9 . . ? C17 C16 C15 120.2(2) . . ? C17 C16 H16 119.9 . . ? C16 C17 H17 120.5 . . ? C16 C17 C18 119.1(2) . . ? C18 C17 H17 120.5 . . ? C17 C18 H18 119.1 . . ? C19 C18 C17 121.8(2) . . ? C19 C18 H18 119.1 . . ? C18 C19 C20 121.0(2) . . ? C18 C19 O4 119.1(2) . . ? O4 C19 C20 119.9(2) . . ? C19 C20 C15 116.5(2) . . ? O3 C20 C15 122.3(2) . . ? O3 C20 C19 121.1(2) . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O4 C21 H21A 109.5 . . ? O4 C21 H21B 109.5 . . ? O4 C21 H21C 109.5 . . ? H22A C22 H22B 107.1 . . ? C23 C22 H22A 107.8 . . ? C23 C22 H22B 107.8 . . ? C23 C22 Al1 118.12(19) . . ? Al1 C22 H22A 107.8 . . ? Al1 C22 H22B 107.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C8 N1 C9 116.3(2) . . ? C8 N1 Al1 124.24(17) . . ? C9 N1 Al1 118.79(15) . . ? C13 N2 Al1 123.56(17) . . ? C14 N2 C13 116.0(2) . . ? C14 N2 Al1 120.40(17) . . ? C2 O1 C1 116.62(19) . . ? C3 O2 Al1 132.85(15) . . ? C20 O3 Al1 124.12(14) . . ? C19 O4 C21 114.67(18) . . ? C22 Al1 N1 91.41(10) . . ? C22 Al1 N2 119.80(11) . . ? N2 Al1 N1 84.48(9) . . ? O2 Al1 C22 120.55(11) . . ? O2 Al1 N1 87.95(8) . . ? O2 Al1 N2 119.28(9) . . ? O2 Al1 O3 88.78(8) . . ? O3 Al1 C22 100.37(10) . . ? O3 Al1 N1 167.79(9) . . ? O3 Al1 N2 86.87(8) . . ? 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 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 O1 1.428(3) . ? C2 C3 1.421(3) . ? C2 C7 1.379(4) . ? C2 O1 1.367(3) . ? C3 C4 1.405(3) . ? C3 O2 1.320(3) . ? C4 C5 1.411(3) . ? C4 C8 1.446(3) . ? C5 H5 0.9500 . ? C5 C6 1.367(4) . ? C6 H6 0.9500 . ? C6 C7 1.406(4) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C8 N1 1.289(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.527(4) . ? C9 N1 1.472(3) . ? C10 C11 1.527(4) . ? C10 C12 1.537(3) . ? C10 C13 1.529(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 N2 1.473(3) . ? C14 H14 0.9500 . ? C14 C15 1.442(3) . ? C14 N2 1.292(3) . ? C15 C16 1.406(3) . ? C15 C20 1.418(3) . ? C16 H16 0.9500 . ? C16 C17 1.375(4) . ? C17 H17 0.9500 . ? C17 C18 1.395(4) . ? C18 H18 0.9500 . ? C18 C19 1.369(4) . ? C19 C20 1.419(3) . ? C19 O4 1.377(3) . ? C20 O3 1.309(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 O4 1.431(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 C23 1.517(4) . ? C22 Al1 1.984(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? N1 Al1 2.082(2) . ? N2 Al1 2.020(2) . ? O2 Al1 1.8016(18) . ? O3 Al1 1.8482(17) . ? loop_ _hkl_oxdiff_h _hkl_oxdiff_k _hkl_oxdiff_l _hkl_oxdiff_f2 _hkl_oxdiff_sig _hkl_oxdiff_ba 0 0 -1 16.4520 10.5827 3 0 0 -2 206326. 4778.99 3 0 0 -3 44.5451 45.2687 3 0 0 -4 55485.8 1419.66 3 0 0 -5 19.2285 54.7076 3 0 0 5 45.1046 64.1487 1 0 0 -6 25778.7 777.348 13 0 0 6 26917.0 849.754 1 0 0 7 62.4045 97.7007 1 0 0 -7 601.179 99.7852 13 0 0 -8 91001.3 2351.39 13 0 0 8 91513.0 2463.65 1 0 0 9 462.884 159.502 1 0 0 -9 238.300 83.1709 13 0 0 10 144902. 3741.86 1 0 0 -10 136860. 3530.55 13 0 0 11 -48.2684 149.885 1 0 0 12 11904.8 722.801 1 0 0 13 -35.4760 147.303 1 0 0 14 297.862 160.592 1 0 0 16 16918.6 998.115 5 0 0 17 239.571 168.643 5 0 0 18 29781.6 1342.29 5 0 0 19 220.164 178.829 5 0 0 -20 747.279 187.260 11 0 0 20 308.441 122.114 5 0 0 21 -9.21573 74.5105 5 0 0 -21 -25.8704 47.4774 11 0 0 -22 1516.60 168.715 10 0 1 0 20.3191 15.3963 2 0 -1 -1 102287. 2398.62 3 0 -1 1 104272. 2397.33 1 0 1 -1 104531. 2425.55 13 0 -1 2 271713. 6338.64 1 0 -1 -2 274879. 6323.28 3 0 1 -2 277649. 6349.98 13 0 1 -3 52264.8 1309.95 13 0 -1 3 51750.0 1315.44 1 0 -1 -3 51792.0 1286.02 3 0 -1 4 277532. 6525.98 1 0 -1 -4 278197. 6487.64 3 0 1 -4 279924. 6504.61 13 0 -1 5 7141.71 324.409 1 0 1 -5 6558.62 296.592 13 0 1 5 7207.67 329.235 1 0 -1 -5 6917.53 297.266 3 0 1 6 86343.6 2222.91 1 0 -1 -6 84145.2 2165.41 3 0 -1 6 86227.1 2216.81 1 0 1 -6 84535.0 2168.67 13 0 -1 7 276.194 113.757 1 0 -1 -7 81.5433 61.9003 13 0 1 -7 48.6838 73.8819 13 0 1 7 51.9098 103.104 1 0 1 -8 82413.0 2219.68 13 0 -1 -8 86582.4 2169.00 13 0 1 8 83760.2 2302.54 1 0 -1 8 83675.2 2298.49 1 0 1 9 13802.4 647.018 1 0 -1 9 14201.0 658.302 1 0 -1 -9 12489.8 520.856 13 0 1 -9 14185.6 581.975 13 0 1 10 3610.54 339.873 1 0 -1 -10 3322.94 244.270 13 0 -1 10 4165.42 359.452 1 0 1 -10 3860.58 294.478 13 0 1 -11 2307.74 238.398 13 0 1 11 2425.14 304.135 1 0 -1 11 2106.37 283.956 1 0 -1 12 3454.63 380.271 1 0 1 12 3687.37 393.646 1 0 1 13 23859.4 1139.62 1 0 -1 13 23544.9 1136.70 1 0 -1 14 10333.7 746.427 1 0 1 14 10687.0 764.713 1 0 1 15 11840.4 830.459 1 0 1 16 367.708 194.884 5 0 -1 16 778.758 248.937 5 0 -1 17 19657.1 1078.76 5 0 1 17 22364.9 1156.42 5 0 -1 18 3178.56 396.383 5 0 1 18 2927.42 400.798 5 0 1 19 457.975 211.245 5 0 -1 19 250.048 167.186 5 0 1 -19 145.665 147.427 11 0 -1 -20 3049.52 316.072 11 0 1 -20 2881.72 300.458 11 0 1 20 3177.18 344.450 5 0 -1 20 2909.01 312.659 5 0 -1 -21 113.285 47.7949 11 0 1 21 461.770 130.759 5 0 1 -22 3165.61 239.294 10 0 2 0 101862. 2433.68 2 0 2 -1 317114. 7397.38 13 0 2 -1 323776. 7413.54 2 0 2 -2 74568.7 1828.25 13 0 -2 -2 71781.7 1779.87 3 0 -2 2 77226.3 1778.42 1 0 2 -3 258060. 6181.31 13 0 -2 3 264990. 6151.97 1 0 -2 -3 268317. 6132.17 3 0 -2 4 41646.7 1128.32 1 0 -2 -4 42248.2 1097.63 3 0 2 -4 42258.7 1143.51 13 0 -2 -5 37505.3 1023.93 3 0 -2 5 36678.0 1063.45 1 0 2 -5 35861.4 1060.22 13 0 2 -6 3021.28 216.089 13 0 2 6 2951.61 228.253 1 0 -2 6 2734.20 213.195 1 0 -2 -6 2845.31 189.005 3 0 2 7 79296.9 2180.85 1 0 -2 -7 82882.7 2109.90 3 0 2 -7 81117.0 2132.93 13 0 -2 7 79682.0 2158.72 1 0 -2 8 149.708 108.647 1 0 2 -8 59.8289 101.077 13 0 2 8 235.115 145.021 1 0 -2 -8 240.171 72.6173 13 0 2 -9 216334. 5196.61 13 0 -2 9 221805. 5303.25 1 0 -2 -9 202059. 5039.68 13 0 2 9 213014. 5290.92 1 0 2 10 16157.5 774.183 1 0 -2 10 17845.6 802.806 1 0 2 -10 17074.3 717.600 13 0 2 11 66193.0 2081.49 1 0 2 -11 64967.6 1942.90 13 0 -2 11 65891.3 2081.23 1 0 -2 12 6176.44 507.812 1 0 2 -12 5546.94 406.479 13 0 2 12 6659.22 528.025 1 0 -2 13 129569. 3748.58 1 0 2 13 128198. 3740.88 1 0 2 14 7264.45 630.658 1 0 -2 15 6203.23 555.548 5 0 2 15 5715.62 570.276 1 0 -2 16 8074.98 655.863 5 0 2 16 8317.40 681.652 5 0 -2 17 313.661 142.267 5 0 2 17 229.491 200.252 5 0 2 -18 748.179 209.778 11 0 -2 18 527.980 183.021 5 0 2 18 972.288 267.100 5 0 2 19 12349.0 768.116 5 0 -2 19 11347.7 669.141 5 0 2 -19 11918.6 688.371 11 0 2 20 992.399 235.186 5 0 2 -20 1081.79 200.892 11 0 -2 -21 179.300 56.9827 11 0 2 21 151.505 103.051 5 0 2 -21 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600.527 7 8 -1 -3 5241.95 466.348 16 8 -1 -3 6337.51 515.138 7 8 1 3 5938.74 544.131 7 8 -1 -4 4811.98 456.400 16 8 -1 -4 4669.20 437.327 7 8 -1 -5 13334.2 767.226 16 8 1 6 2686.74 339.186 12 8 -1 -6 2306.97 329.458 16 8 1 7 910.435 213.250 12 8 -1 -7 1150.24 236.110 16 8 1 8 8048.55 566.894 12 8 -1 -8 7550.51 530.853 16 8 1 9 906.600 206.520 12 8 -1 -9 1335.99 232.535 16 8 1 10 148.766 145.925 12 8 -1 -10 204.298 144.107 16 8 1 11 1071.84 195.376 12 8 -1 -11 765.413 161.590 16 8 1 12 2030.23 222.926 12 8 -1 -12 2428.16 230.106 16 8 -2 12 3304.84 281.083 12 8 -2 11 324.157 139.492 12 8 2 -11 18.5322 83.3742 16 8 -2 10 4846.47 409.113 12 8 2 -10 4640.62 339.004 16 8 -2 9 971.741 228.909 12 8 2 -9 1213.84 200.565 16 8 -2 8 2421.78 320.912 12 8 2 -8 2729.52 292.755 16 8 -2 7 8320.16 584.524 12 8 2 -5 34610.1 1392.43 7 8 2 -4 5034.51 484.835 7 8 -2 4 5651.45 504.013 7 8 2 -3 52886.6 1902.27 7 8 -2 3 52311.7 1866.71 7 8 2 -2 419.795 196.109 7 8 -2 2 219.325 149.773 7 8 2 -1 12275.9 789.247 7 8 -2 1 12780.5 764.631 7 8 -2 0 2124.99 308.224 7 8 2 0 1946.24 333.937 7 8 2 1 12939.9 820.271 7 8 -2 -2 237.363 174.442 16 8 2 2 507.445 222.942 7 8 -2 -3 49610.3 1785.94 16 8 2 3 50319.0 1869.83 7 8 2 4 6016.91 530.638 4 8 -2 -4 5409.63 499.771 16 8 2 4 5672.07 522.326 7 8 2 5 32505.0 1349.16 4 8 -2 -5 33335.2 1349.98 16 8 2 6 1694.70 264.051 4 8 2 6 999.770 214.644 12 8 -2 -6 1042.94 241.942 16 8 2 7 8704.46 588.423 12 8 2 7 8375.57 576.773 4 8 -2 -7 8938.68 605.467 16 8 2 8 2818.93 337.313 12 8 2 8 2395.48 293.131 4 8 -2 -8 3006.68 350.317 16 8 2 9 1011.68 213.565 12 8 -2 -9 1279.22 232.545 16 8 2 10 4283.35 384.480 12 8 -2 -10 5095.87 395.881 16 8 2 11 343.060 131.730 12 8 -2 -11 404.700 142.604 16 8 -2 -12 3836.43 284.150 16 8 -3 12 626.105 127.830 12 8 -3 11 2746.25 285.122 12 8 -3 10 5285.04 398.618 12 8 3 -10 -67.9264 58.6883 16 8 -3 9 7298.17 519.588 12 8 -3 8 568.463 174.901 12 8 -3 7 674.866 189.641 12 8 -3 6 7605.12 536.237 7 8 3 -5 2839.02 372.097 7 8 3 -4 10688.5 702.621 7 8 3 -3 1673.60 292.574 7 8 3 -2 5249.74 499.243 7 8 3 -1 2144.07 346.998 7 8 3 0 10396.8 720.146 7 8 -3 -1 2312.23 328.435 16 8 3 1 1778.72 325.387 7 8 -3 -2 4282.59 457.073 16 8 3 2 5046.99 495.055 7 8 -3 -3 2297.60 345.073 16 8 3 3 1860.05 336.490 7 8 3 4 10430.2 712.885 4 8 -3 -4 11318.5 726.687 16 8 3 4 10685.3 728.783 7 8 3 5 2971.75 372.334 4 8 -3 -5 2708.00 360.843 16 8 3 6 7796.42 582.294 4 8 -3 -6 8502.68 613.913 16 8 3 7 852.665 218.500 4 8 3 7 631.059 161.468 12 8 -3 -7 768.998 212.833 16 8 3 8 872.420 189.918 4 8 3 8 383.953 151.156 12 8 -3 -8 353.460 187.907 16 8 -3 -9 8512.68 544.397 16 8 3 9 7440.00 487.421 4 8 -3 -10 5483.06 401.931 16 8 3 10 3596.28 307.640 4 8 -3 -11 3253.50 295.302 16 8 -3 -12 838.455 137.987 16 8 -4 11 5404.64 375.118 12 8 -4 10 15582.8 733.971 12 8 -4 9 2358.22 293.105 12 8 -4 8 33647.8 1284.27 12 8 -4 7 2710.32 317.204 12 8 4 -5 2284.42 338.180 7 8 4 -4 16946.3 901.982 7 8 4 -3 199.754 189.235 7 8 4 -2 14013.4 824.786 7 8 4 -1 4338.18 465.300 7 8 -4 0 24154.0 1126.73 16 8 4 0 27145.0 1211.13 7 8 -4 -1 3268.58 396.873 16 8 4 1 3896.66 443.674 7 8 -4 -2 11794.2 747.248 16 8 4 2 11188.0 741.093 7 8 -4 -3 37.3599 185.305 16 8 4 3 -174.004 229.612 7 8 4 4 18980.8 994.339 4 8 -4 -4 19171.4 975.256 16 8 4 4 19660.5 997.411 7 8 4 5 1900.62 318.773 4 8 -4 -5 1936.72 320.462 16 8 4 5 1886.31 321.217 7 8 4 6 8181.72 601.677 4 8 -4 -6 7965.34 590.993 16 8 4 7 3031.68 360.585 4 8 -4 -7 2768.61 351.525 16 8 -4 -8 40983.5 1442.21 16 8 4 8 37121.7 1399.68 4 8 4 9 2009.33 259.301 4 8 -4 -9 2403.13 297.247 16 8 -4 -10 17439.4 746.797 16 8 4 10 13632.6 657.574 4 8 -4 -11 6179.07 391.656 16 8 -4 -12 2571.81 219.206 16 8 4 12 2332.93 218.217 7 8 -5 11 1424.42 175.361 12 8 -5 10 4215.40 339.804 12 8 -5 9 1588.09 226.601 12 8 -5 8 2531.71 288.676 12 8 -5 7 5288.35 422.438 12 8 5 -5 4006.97 408.457 7 8 5 -4 3133.38 370.781 7 8 5 -3 15616.8 856.316 7 8 5 -2 4302.77 445.205 7 8 5 -1 5698.49 513.933 7 8 5 0 30851.3 1310.67 7 8 5 1 5501.64 507.557 7 8 -5 -2 3729.51 428.212 16 8 5 2 4557.28 462.384 7 8 -5 -3 13917.8 820.861 16 8 5 3 13358.9 799.603 7 8 5 4 3522.88 413.336 4 8 -5 -4 3114.70 399.723 16 8 5 4 3544.52 415.917 7 8 5 5 3400.58 387.430 4 8 -5 -5 3633.38 412.792 16 8 5 5 3672.46 407.554 7 8 5 6 4504.60 438.155 4 8 -5 -6 4758.87 447.688 16 8 5 6 4569.34 435.046 7 8 5 7 5665.94 474.851 4 8 -5 -7 6307.36 492.114 16 8 5 7 6056.72 481.940 7 8 -5 -8 2957.46 333.297 16 8 5 8 2922.75 321.474 4 8 5 8 2666.96 319.167 7 8 5 9 1743.90 244.605 4 8 -5 -9 2261.78 278.641 16 8 5 9 1675.60 254.569 7 8 -5 -10 4513.50 347.272 16 8 5 10 3970.91 319.224 4 8 5 10 3671.28 323.821 7 8 -5 -11 1767.34 206.296 16 8 5 11 1783.03 201.882 7 8 -6 10 2250.31 225.072 12 8 -6 9 4174.59 330.344 12 8 -6 8 1589.12 217.927 12 8 6 -5 11500.1 670.965 7 8 6 -4 2039.46 306.682 7 8 6 -3 25402.6 1103.96 7 8 6 -2 34.2786 190.383 7 8 6 -1 49015.2 1741.81 7 8 6 0 3660.88 413.915 7 8 6 1 48141.3 1725.13 7 8 -6 -2 348.242 192.957 16 8 6 2 195.336 189.341 7 8 -6 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16 8 7 6 3115.83 326.878 7 8 7 7 4520.32 390.598 4 8 -7 -7 5235.18 424.164 16 8 7 7 5033.03 394.764 7 8 7 8 1411.50 214.732 4 8 -7 -8 1447.60 228.844 16 8 7 8 1461.40 208.146 7 8 7 9 2343.37 244.522 4 8 -7 -9 2915.64 272.502 16 8 7 9 2411.37 235.667 7 8 7 10 954.019 144.637 4 8 -7 -10 989.515 148.909 16 -8 8 8 1827.30 185.415 6 8 8 -3 1611.73 243.756 7 8 8 -2 31268.8 1191.37 7 8 8 -1 5400.12 435.343 7 8 8 0 37820.0 1369.71 7 8 8 1 5155.08 427.627 7 8 8 2 30559.9 1175.49 7 8 -8 -3 1895.86 310.113 16 8 8 3 1542.13 244.813 7 8 -8 -4 10601.9 653.438 16 8 8 4 10393.0 588.709 7 8 -8 -5 2942.09 339.153 16 8 8 5 2653.32 288.223 7 8 8 6 13743.0 688.342 4 8 -8 -6 14233.6 711.017 16 8 8 6 12773.3 636.625 7 8 8 7 9257.49 533.250 4 8 -8 -7 10691.0 571.071 16 8 8 7 9639.10 508.625 7 8 8 8 2102.23 229.521 4 8 8 8 1959.91 203.703 7 8 -8 -9 4086.66 292.828 16 -8 9 7 2128.64 207.568 6 -8 9 6 2246.04 230.946 6 8 9 -2 1434.04 220.575 7 8 9 -1 309.569 130.814 7 8 9 0 563.965 162.209 7 8 9 1 311.200 140.054 7 8 9 2 2036.09 247.966 7 8 -9 -2 1604.11 274.584 16 8 -9 -3 3074.58 343.244 16 8 9 3 2798.51 280.342 7 8 -9 -4 5706.04 443.747 16 8 9 4 5386.87 376.284 7 8 -9 -5 2257.80 280.396 16 8 9 5 1640.95 203.421 7 8 -9 -6 2340.13 268.885 16 8 9 6 1895.72 198.284 7 8 -9 -7 2546.86 252.595 16 8 -9 -8 181.968 91.2114 16 -8 10 6 3079.12 236.635 6 -8 10 5 9634.18 475.226 6 -8 10 4 2577.19 246.747 6 -8 10 3 11432.0 558.273 6 -8 10 2 1790.94 213.047 6 -8 10 0 -133.289 114.538 6 8 10 0 80.3859 85.8224 7 -8 10 -1 10814.6 520.312 6 8 10 1 10287.5 509.431 7 -8 10 -2 1515.28 180.235 6 8 -10 -2 1758.93 253.328 16 8 10 2 1533.40 181.106 7 8 10 3 7947.21 418.003 7 8 -10 -3 10786.0 567.183 16 8 -10 -4 2500.52 268.730 16 8 10 4 194.181 57.4284 7 8 -10 -5 10575.0 544.633 16 8 -10 -6 3480.90 276.648 16 -8 11 4 200.570 82.3886 6 -8 11 3 165.164 84.6685 6 -8 11 2 558.564 119.186 6 -8 11 1 3469.00 259.329 6 -8 11 0 4886.88 303.082 6 8 -11 0 4724.44 349.105 16 -8 11 -1 2725.84 213.615 6 8 -11 -1 3769.63 308.288 16 8 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375.356 7 9 2 5 7138.36 469.635 7 9 2 6 2937.20 285.025 7 9 2 7 2417.41 242.775 7 9 2 8 11421.2 521.991 7 9 3 -3 1412.51 220.667 7 9 3 -2 171.738 135.123 7 9 3 -1 3775.47 342.935 7 9 3 0 20880.0 910.093 7 9 3 1 3126.94 322.309 7 9 3 2 296.726 135.465 7 9 3 3 2122.44 272.949 7 9 3 4 3226.98 319.812 7 9 -3 -5 -110.377 49.9415 16 9 3 5 4787.53 361.116 7 9 -3 -6 -54.0004 32.1058 16 9 3 6 2137.03 238.852 7 9 3 7 7935.75 441.635 7 9 3 8 1905.55 195.884 7 9 4 -3 295.741 136.601 7 9 4 -2 4311.81 360.242 7 9 4 -1 4829.30 390.097 7 9 4 0 1217.49 210.614 7 9 4 1 4207.70 370.163 7 9 4 2 3575.07 335.750 7 9 4 3 540.002 169.012 7 9 -4 -4 -269.012 82.9091 16 9 4 4 305.625 139.400 7 9 -4 -5 91.7474 48.7670 16 9 4 5 2303.29 248.149 7 9 -4 -6 523.319 106.805 16 9 4 6 1992.82 223.052 7 9 4 7 7044.33 396.097 7 9 4 8 356.429 98.8871 7 9 5 -2 6008.37 408.118 7 9 5 -1 15635.9 721.157 7 9 5 0 17528.4 772.947 7 9 5 1 15518.9 716.556 7 9 5 2 6313.64 426.684 7 9 5 3 13635.7 571.351 7 9 -5 -3 -83.3416 60.3591 16 9 -5 -4 218.098 72.2365 16 9 5 4 2584.95 256.688 7 9 -5 -5 1488.07 177.111 16 9 5 5 1664.55 202.683 7 9 -5 -6 5218.70 315.653 16 9 5 6 6505.41 377.331 7 9 5 7 717.942 127.486 7 9 6 -2 10575.0 531.810 7 9 6 -1 2181.69 238.994 7 9 6 0 7391.33 443.822 7 9 6 1 1767.69 219.105 7 9 6 2 12512.1 523.841 7 9 -6 -2 146.524 62.6594 16 9 6 3 3413.48 279.235 7 9 -6 -3 4.19003 28.1210 16 9 -6 -4 876.764 139.682 16 9 6 4 1022.83 158.140 7 9 6 5 747.760 138.139 7 9 6 6 888.875 136.662 7 9 7 -1 700.609 139.951 7 9 7 0 973.356 162.791 7 9 7 1 865.286 152.977 7 9 7 2 14641.4 614.879 7 9 7 3 2697.38 234.594 7 9 7 4 8564.82 416.783 7 9 8 1 483.092 96.2971 7