#------------------------------------------------------------------------------ #$Date: 2024-12-07 19:04:45 +0200 (Sat, 07 Dec 2024) $ #$Revision: 296757 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312712.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_2312712 loop_ _publ_author_name 'Kanthapazham, Rajakumar' 'Osipov, Artyom A.' 'Zherebtsov, Dmitry A.' 'Efremov, Andrey N.' 'Nayfert, Sergey A.' 'Adonin, Sergey A.' 'Spiridonova, Dar'ya V.' 'Atapin, Sergey V.' _publ_section_title ; Structures of hexamethyl-[1,1'-biphenyl]-4,4'-diammonium salts. ; _journal_coeditor_code AW5097 _journal_issue 6 _journal_name_full 'Acta crystallographica Section B, Structural science, crystal engineering and materials' _journal_page_first 751 _journal_page_last 759 _journal_paper_doi 10.1107/S2052520624009818 _journal_volume 80 _journal_year 2024 _chemical_formula_moiety 'C4 H4 O4, 6(H2 O), C18 H26 N2' _chemical_formula_sum 'C22 H42 N2 O10' _chemical_formula_weight 494.57 _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_Hall '-P 2n 2ab' _space_group_name_H-M_alt 'P b c n' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2024-01-22 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 25.1134(3) _cell_length_b 8.38700(10) _cell_length_c 11.8570(2) _cell_measurement_reflns_used 12259 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 78.9090 _cell_measurement_theta_min 3.5400 _cell_volume 2497.39(6) _computing_cell_refinement 'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 -66.00 14.00 0.50 0.25 -- -47.51 67.00 116.00 160 2 \w -84.00 -33.00 0.50 1.00 -- -106.00 71.00 -13.00 102 3 \w 45.00 131.00 0.50 1.00 -- 113.25 -84.00 106.00 172 4 \w 103.00 170.00 0.50 1.00 -- 113.25 67.00 116.00 134 5 \w 76.00 102.00 0.50 0.25 -- 47.51 125.00 90.00 52 6 \w 90.00 115.00 0.50 0.25 -- 47.51 125.00 30.00 50 7 \w 74.00 120.00 0.50 0.25 -- 47.51 125.00 60.00 92 8 \w -59.00 -33.00 0.50 1.00 -- -106.00 61.00 60.00 52 9 \w -71.00 -41.00 0.50 1.00 -- -106.00 61.00-150.00 60 10 \w -71.00 -45.00 0.50 1.00 -- -106.00 61.00-180.00 52 11 \w -66.00 -33.00 0.50 1.00 -- -106.00 61.00 150.00 66 12 \w -71.00 -46.00 0.50 1.00 -- -106.00 61.00 -60.00 50 13 \w 60.00 106.00 0.50 1.00 -- 113.25 -77.00-150.00 92 14 \w 45.00 71.00 0.50 1.00 -- 113.25 -61.00 120.00 52 15 \w 42.00 67.00 0.50 1.00 -- 113.25 -61.00 0.00 50 16 \w 44.00 69.00 0.50 1.00 -- 113.25 -61.00 -90.00 50 17 \w 42.00 67.00 0.50 1.00 -- 113.25 -61.00-120.00 50 18 \w -172.00-146.00 0.50 1.00 -- -106.00 -84.00 106.00 52 19 \w -107.00 -81.00 0.50 0.25 -- -47.51-125.00 90.00 52 20 \w -22.00 23.00 0.50 0.25 -- -47.51 19.00-120.00 90 21 \w -21.00 5.00 0.50 0.25 -- 47.51 -19.00 -60.00 52 22 \w -135.00-106.00 0.50 1.00 -- -106.00 -30.00 -90.00 58 23 \w -177.00-146.00 0.50 1.00 -- -106.00 -30.00 -90.00 62 24 \w -104.00 -78.00 0.50 1.00 -- -106.00 77.00 60.00 52 25 \w -128.00 -88.00 0.50 1.00 -- -106.00 -84.00 106.00 80 26 \w -62.00 -33.00 0.50 1.00 -- -106.00 77.00 60.00 58 27 \w 42.00 67.00 0.50 1.00 -- 113.25 -61.00 60.00 50 28 \w 45.00 71.00 0.50 1.00 -- 113.25 -61.00 30.00 52 29 \w 108.00 144.00 0.50 1.00 -- 113.25 30.00-180.00 72 30 \w 71.00 102.00 0.50 1.00 -- 113.25-125.00 0.00 62 31 \w 46.00 72.00 0.50 1.00 -- 113.25-125.00-120.00 52 32 \w 42.00 68.00 0.50 1.00 -- 113.25 -61.00 -60.00 52 33 \w 42.00 84.00 0.50 1.00 -- 113.25 -77.00-180.00 84 34 \w 147.00 173.00 0.50 1.00 -- 113.25 30.00-180.00 52 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at home/near, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0090104000 _diffrn_orient_matrix_UB_12 -0.0907494000 _diffrn_orient_matrix_UB_13 0.1113828000 _diffrn_orient_matrix_UB_21 0.0479029000 _diffrn_orient_matrix_UB_22 -0.1083737000 _diffrn_orient_matrix_UB_23 -0.0267510000 _diffrn_orient_matrix_UB_31 0.0372277000 _diffrn_orient_matrix_UB_32 0.1173378000 _diffrn_orient_matrix_UB_33 0.0613299000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_unetI/netI 0.0253 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 17634 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 69.993 _diffrn_reflns_theta_min 3.520 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.864 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.75142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.315 _exptl_crystal_description prism _exptl_crystal_F_000 1072 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.646 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.059 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 166 _refine_ls_number_reflns 2369 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.094 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0495 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0722P)^2^+2.1081P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1375 _refine_ls_wR_factor_ref 0.1407 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2191 _reflns_number_total 2369 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file aw5097sup1.cif _cod_data_source_block hmb_yant _cod_depositor_comments 'Adding full bibliography for 2312709--2312717.cif.' _cod_database_code 2312712 _cod_database_fobs_code 2312712 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C22 H30 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 0.950 _shelx_estimated_absorpt_t_min 0.889 _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, All O(H,H) groups 2.a Free rotating group: O5(H5A,H5B), O4(H4A,H4B), O6(H6A,H6B) 2.b Secondary CH2 refined with riding coordinates: C11(H11A,H11B) 2.c Aromatic/amide H refined with riding coordinates: C2(H2), C6(H6), C5(H5), C3(H3) 2.d Idealised Me refined as rotating group: C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C) ; _shelx_res_file ; TITL hmb_yant_a.res in Pbcn hmb_yant.res created by SHELXL-2018/3 at 16:08:29 on 22-Jan-2024 REM Old TITL hmb_yant_a.res in Pbcn REM SHELXT solution in Pbcn: R1 0.126, Rweak 0.002, Alpha 0.012 REM 0.573 for 383 systematic absences, Orientation as input REM Formula found by SHELXT: C11 N3 O3 CELL 1.54184 25.1134 8.387 11.857 90 90 90 ZERR 4 0.0003 0.0001 0.0002 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,0.5+Z SYMM -X,+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O UNIT 88 168 8 40 L.S. 29 PLAN 2 SIZE 0.14 0.08 0.06 TEMP -173 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT -4 140 REM REM REM WGHT 0.072200 2.108100 FVAR 0.58561 O1 4 0.614013 0.601965 0.536849 11.00000 0.01658 0.02193 = 0.02388 0.00226 -0.00247 -0.00296 O2 4 0.569680 0.424791 0.641894 11.00000 0.01971 0.02098 = 0.02067 0.00423 -0.00228 0.00068 AFIX 6 O5 4 0.855613 0.869984 0.812289 11.00000 0.02035 0.03993 = 0.02242 0.00028 0.00084 -0.00663 H5A 2 0.870354 0.882650 0.878087 11.00000 -1.50000 H5B 2 0.880875 0.891800 0.764357 11.00000 -1.50000 AFIX 0 N1 3 0.654898 0.086119 0.517829 11.00000 0.01760 0.01524 = 0.02660 -0.00310 -0.00220 0.00034 AFIX 6 O4 4 0.749503 0.879948 0.774371 11.00000 0.03587 0.05514 = 0.04050 -0.00918 -0.00089 0.00715 H4A 2 0.735825 0.797349 0.740789 11.00000 -1.50000 H4B 2 0.782140 0.851977 0.789285 11.00000 -1.50000 AFIX 0 C10 1 0.572396 0.522754 0.563007 11.00000 0.01642 0.01361 = 0.01811 -0.00255 -0.00012 0.00213 C11 1 0.523085 0.557433 0.491295 11.00000 0.01493 0.01447 = 0.02086 0.00264 -0.00097 0.00051 AFIX 23 H11A 2 0.510628 0.666784 0.508395 11.00000 -1.20000 H11B 2 0.533491 0.554837 0.410783 11.00000 -1.20000 AFIX 0 C1 1 0.609129 0.091407 0.436636 11.00000 0.01678 0.01723 = 0.01893 -0.00260 0.00068 0.00027 C9 1 0.685791 0.239493 0.519607 11.00000 0.01997 0.01858 = 0.03330 -0.00575 -0.00354 -0.00344 AFIX 137 H9A 2 0.699226 0.262477 0.443730 11.00000 -1.50000 H9B 2 0.715806 0.229564 0.571955 11.00000 -1.50000 H9C 2 0.662491 0.326487 0.544294 11.00000 -1.50000 AFIX 0 C7 1 0.633888 0.056606 0.635207 11.00000 0.03083 0.03024 = 0.02302 0.00260 -0.00566 -0.00219 AFIX 137 H7A 2 0.607844 0.139213 0.654554 11.00000 -1.50000 H7B 2 0.663421 0.059729 0.689184 11.00000 -1.50000 H7C 2 0.616751 -0.048291 0.638119 11.00000 -1.50000 AFIX 0 C8 1 0.692388 -0.047459 0.487076 11.00000 0.02126 0.02083 = 0.04423 -0.00800 -0.00409 0.00470 AFIX 137 H8A 2 0.673059 -0.148957 0.488004 11.00000 -1.50000 H8B 2 0.721613 -0.051518 0.541772 11.00000 -1.50000 H8C 2 0.706854 -0.028701 0.411468 11.00000 -1.50000 AFIX 0 C4 1 0.522821 0.092261 0.289613 11.00000 0.02073 0.01538 = 0.01668 -0.00123 0.00198 0.00103 C2 1 0.598337 0.226936 0.374097 11.00000 0.02243 0.01389 = 0.02070 -0.00236 0.00257 -0.00339 AFIX 43 H2 2 0.620298 0.318683 0.380753 11.00000 -1.20000 AFIX 0 C6 1 0.577591 -0.044143 0.427179 11.00000 0.02006 0.01321 = 0.02269 0.00095 0.00009 0.00072 AFIX 43 H6 2 0.585283 -0.136318 0.470803 11.00000 -1.20000 AFIX 0 C5 1 0.534779 -0.043274 0.353350 11.00000 0.01921 0.01354 = 0.02301 0.00029 -0.00001 -0.00203 AFIX 43 H5 2 0.513308 -0.135948 0.345994 11.00000 -1.20000 AFIX 0 C3 1 0.554893 0.226918 0.301378 11.00000 0.02744 0.01400 = 0.01708 0.00074 0.00078 -0.00068 AFIX 43 H3 2 0.546946 0.320109 0.259059 11.00000 -1.20000 AFIX 6 O6 4 0.704386 0.636638 0.660108 11.00000 0.02886 0.06482 = 0.05696 0.01390 -0.01648 -0.01171 H6A 2 0.673933 0.624782 0.626070 11.00000 -1.50000 H6B 2 0.708854 0.548069 0.697107 11.00000 -1.50000 AFIX 0 HKLF 4 REM hmb_yant_a.res in Pbcn REM wR2 = 0.1407, GooF = S = 1.094, Restrained GooF = 1.094 for all data REM R1 = 0.0495 for 2191 Fo > 4sig(Fo) and 0.0524 for all 2369 data REM 166 parameters refined using 0 restraints END WGHT 0.0714 2.1204 REM Highest difference peak 0.646, deepest hole -0.524, 1-sigma level 0.059 Q1 1 0.6986 0.7168 0.7032 11.00000 0.05 0.65 Q2 1 0.5218 0.0416 0.3335 11.00000 0.05 0.24 ; _shelx_res_checksum 45789 _shelx_hkl_file ; 0 0 -1 0.13 0.37 0 0 1 -0.21 0.27 0 0 -2 3187.04 126.04 0 0 2 2976.14 125.52 0 0 2 3266.39 125.80 0 0 3 0.13 0.70 0 0 -3 -0.82 1.12 0 0 3 -0.33 0.90 0 0 4 549.54 23.94 0 0 4 546.58 23.45 0 0 -4 539.07 24.31 0 0 4 573.62 25.69 0 0 5 -0.68 0.99 0 0 5 0.30 1.27 0 0 -5 -0.37 1.48 0 0 5 1.73 2.01 0 0 6 4655.98 188.13 0 0 6 4582.10 184.90 0 0 6 4455.96 184.17 0 0 7 4.50 3.14 0 0 7 -0.47 1.34 0 0 8 7.76 1.38 0 0 9 -0.46 1.03 0 0 9 0.61 0.95 0 0 9 -0.23 1.01 0 0 10 62.70 4.18 0 0 10 68.14 4.47 0 0 11 0.86 1.03 0 0 11 0.26 1.19 0 0 11 0.25 1.08 0 0 12 181.65 9.36 0 0 12 190.18 9.29 0 0 13 1.44 1.19 0 0 13 -0.18 0.99 0 0 14 679.05 28.88 0 1 0 0.05 0.33 0 1 1 0.39 0.58 0 1 2 0.14 0.80 0 1 2 2.39 0.90 0 1 -2 -0.22 1.18 0 -1 2 1.02 1.35 0 1 3 -0.20 0.91 0 -1 3 -0.12 0.39 0 1 3 0.57 0.93 0 1 -3 0.60 1.37 0 -1 3 -0.37 1.59 0 -1 4 -0.21 0.88 0 1 4 0.72 0.93 0 -1 4 0.42 0.58 0 1 4 0.26 1.21 0 1 -4 0.38 1.60 0 -1 4 0.49 1.75 0 -1 5 0.56 1.13 0 1 5 0.66 1.39 0 1 5 1.81 0.86 0 1 5 1.64 1.74 0 1 -5 0.48 1.52 0 -1 6 0.72 1.32 0 1 6 0.83 1.45 0 1 6 2.96 1.14 0 1 6 -0.70 2.07 0 1 -6 -0.59 1.60 0 -1 7 2.22 1.55 0 1 -7 -1.43 2.36 0 1 7 0.86 2.13 0 -1 8 1.86 1.03 0 1 8 1.03 2.25 0 1 9 1.58 0.87 0 -1 9 1.58 0.95 0 -1 9 0.43 1.01 0 -1 9 -0.22 0.96 0 1 9 0.47 1.17 0 1 9 0.24 1.16 0 -1 10 2.51 1.19 0 1 10 2.26 1.32 0 -1 10 0.23 1.09 0 -1 10 1.20 1.04 0 1 10 0.75 1.18 0 1 10 0.78 1.46 0 -1 11 -0.69 1.05 0 1 11 -0.53 1.39 0 -1 11 0.23 1.14 0 1 11 -0.98 1.40 0 1 11 2.34 1.35 0 -1 11 1.29 1.10 0 1 12 1.43 1.40 0 -1 12 -0.20 1.03 0 1 12 -0.21 1.13 0 -1 12 1.68 1.17 0 1 12 2.90 1.24 0 1 13 -0.75 1.12 0 -1 13 3.11 1.09 0 1 13 1.58 1.15 0 1 13 0.57 1.60 0 1 14 -0.12 0.77 0 1 14 0.98 1.07 0 2 0 8550.05 343.72 0 2 0 8581.73 344.11 0 2 1 2124.27 86.24 0 2 1 2115.78 87.03 0 2 2 3222.54 130.79 0 2 3 4886.84 197.13 0 2 3 4928.36 197.03 0 2 -3 4744.99 198.36 0 2 4 45.59 3.90 0 2 -4 54.32 5.09 0 2 5 3.42 1.22 0 -2 5 1.84 1.11 0 2 -5 2.94 2.11 0 2 6 10.08 2.13 0 -2 6 7.43 1.66 0 2 6 11.56 2.87 0 2 -6 12.56 3.06 0 -2 7 459.98 22.23 0 2 -7 516.20 25.69 0 2 7 426.71 24.74 0 2 7 487.18 20.84 0 2 -8 6.74 2.97 0 2 8 7.63 1.52 0 2 8 8.85 3.34 0 -2 8 9.59 1.57 0 2 8 4.85 1.67 0 -2 8 5.21 1.12 0 2 8 5.59 1.56 0 2 9 916.13 38.99 0 2 9 903.16 38.69 0 -2 9 958.19 38.78 0 2 9 882.69 39.61 0 -2 9 927.15 39.01 0 -2 9 919.09 38.47 0 2 9 961.25 39.23 0 -2 9 896.44 38.26 0 -2 10 334.99 15.38 0 -2 10 359.08 16.03 0 2 10 335.68 15.92 0 2 10 357.02 16.12 0 -2 10 345.06 15.74 0 2 10 330.45 15.66 0 2 11 24.98 2.74 0 2 11 30.56 2.78 0 -2 11 28.14 2.71 0 -2 11 25.47 2.37 0 -2 11 25.22 2.68 0 2 11 29.23 3.54 0 2 11 31.54 3.01 0 2 12 102.65 5.72 0 -2 12 95.74 5.60 0 2 12 104.30 5.87 0 2 12 98.51 5.74 0 -2 12 92.07 5.52 0 2 12 103.30 6.57 0 2 13 202.35 9.45 0 2 13 189.50 9.27 0 -2 13 200.33 9.31 0 2 13 196.20 10.05 0 2 14 347.75 16.24 0 2 14 387.21 15.89 0 3 0 0.46 1.08 0 3 1 -0.79 1.65 0 3 -1 2.33 2.20 0 3 1 1.82 0.94 0 3 -1 -0.41 1.04 0 3 2 1.11 1.09 0 3 -2 0.90 0.90 0 3 2 0.29 1.36 0 3 -3 0.14 0.60 0 3 3 0.34 1.30 0 3 -4 -0.63 1.80 0 3 -4 0.26 0.40 0 3 -5 -0.73 2.42 0 3 5 2.84 1.35 0 -3 5 0.24 0.79 0 3 6 0.65 1.52 0 -3 6 0.60 0.89 0 3 6 0.56 1.66 0 3 -6 -0.85 2.31 0 3 7 -0.24 1.16 0 3 7 0.89 1.27 0 3 7 -0.78 1.43 0 3 8 -0.88 1.45 0 3 -8 1.09 2.37 0 -3 8 -0.57 0.96 0 3 8 -0.95 0.96 0 3 8 0.65 1.45 0 -3 8 -0.52 1.06 0 3 8 -0.26 1.11 0 3 8 0.34 1.45 0 3 8 -0.83 1.44 0 3 -9 -2.35 2.16 0 3 9 1.08 1.24 0 3 9 -1.21 1.66 0 -3 9 0.28 1.12 0 -3 9 1.27 0.89 0 3 9 0.64 0.92 0 3 9 0.36 1.69 0 3 9 0.37 1.65 0 3 10 2.33 2.10 0 -3 10 -0.29 1.33 0 3 10 1.23 1.60 0 3 10 -0.56 1.36 0 3 10 1.81 1.15 0 -3 10 4.19 1.12 0 3 11 0.37 1.94 0 -3 11 -0.54 1.22 0 3 11 -1.13 1.49 0 3 11 -1.08 1.22 0 -3 11 0.42 1.12 0 3 11 0.27 1.39 0 3 12 0.97 1.65 0 3 12 0.73 1.03 0 -3 12 -0.17 0.96 0 -3 12 -0.89 1.30 0 3 13 -0.97 1.44 0 3 14 0.57 0.71 0 3 14 -0.60 0.41 0 3 14 -0.88 0.85 0 4 0 1862.11 73.67 0 4 0 1616.41 75.33 0 4 1 43.77 4.09 0 4 -1 47.34 3.71 0 4 -2 1123.30 50.33 0 4 -2 1085.76 47.20 0 4 2 1195.33 48.38 0 4 -2 1118.14 50.88 0 4 -3 512.24 27.95 0 4 -3 566.51 24.68 0 4 -3 581.27 29.01 0 4 3 614.68 26.70 0 4 -4 340.65 19.75 0 4 4 330.10 17.35 0 4 5 51.67 5.02 0 4 5 64.69 4.00 0 4 -5 50.25 6.80 0 4 -5 60.63 7.09 0 4 5 63.70 4.41 0 4 -6 139.70 12.00 0 4 6 149.47 8.41 0 4 -6 162.74 12.55 0 4 6 153.41 7.97 0 4 -7 97.84 9.96 0 4 7 90.69 5.95 0 -4 7 103.64 5.87 0 4 7 90.89 6.15 0 4 -7 78.44 9.12 0 4 8 59.25 4.65 0 4 -8 41.15 7.00 0 4 -8 51.14 7.07 0 -4 8 57.23 4.29 0 4 8 56.42 4.72 0 4 9 15.47 2.80 0 4 9 21.78 2.90 0 4 -9 19.32 4.90 0 4 9 15.86 2.52 0 4 9 17.99 1.98 0 -4 10 11.80 2.03 0 4 10 16.37 2.66 0 4 10 14.23 2.38 0 4 10 12.92 2.61 0 -4 11 17.74 2.41 0 4 11 22.22 3.00 0 4 12 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509.98 23.22 -5 8 -3 537.78 23.57 -5 8 3 502.01 23.30 5 8 -3 512.12 23.28 5 8 -3 521.29 22.82 5 8 3 486.51 23.24 -5 8 4 8.61 1.97 5 8 4 3.72 1.86 5 8 -4 8.28 1.80 5 8 4 6.48 1.54 5 8 -4 8.25 1.99 -5 8 -4 10.18 2.02 -5 8 4 9.73 1.95 5 8 -4 7.96 1.65 -5 8 4 5.74 2.07 5 8 4 7.01 1.84 -5 8 5 2.42 1.45 5 8 5 1.74 1.58 5 8 -5 1.80 1.13 -5 8 -5 1.83 1.26 5 8 5 3.70 1.45 -5 8 5 1.50 1.60 5 -8 5 1.05 0.99 5 8 -5 2.94 1.56 5 8 -5 2.80 1.42 -5 8 6 2.18 1.40 5 8 6 1.06 1.44 5 -8 6 1.35 1.00 5 8 -6 2.76 1.40 5 8 7 87.94 5.23 -5 8 7 85.06 5.05 -5 8 7 90.26 5.28 5 -8 7 85.48 4.65 5 8 -7 84.02 4.84 5 8 -8 10.73 1.29 5 -8 8 14.17 1.47 -5 -8 8 12.75 1.23 -5 8 8 16.63 1.83 5 8 -8 13.98 1.53 -5 8 8 16.23 1.76 5 8 8 15.74 1.86 5 8 -9 9.12 1.09 5 -8 9 8.69 0.95 -5 9 0 19.71 2.68 5 9 0 20.14 2.67 5 9 0 15.65 2.22 -5 9 1 23.51 2.58 5 9 1 24.79 2.97 5 9 -1 25.61 2.81 -5 9 -1 20.04 2.70 -5 9 1 19.73 2.62 5 9 -1 23.83 2.17 5 9 -1 25.01 2.54 -5 9 2 58.65 4.03 5 9 -2 68.92 4.20 5 9 2 61.34 3.97 5 9 2 61.51 4.43 5 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5 11 44.23 2.79 11 -5 11 45.41 2.58 11 5 11 42.66 2.70 -11 -5 11 48.39 3.09 11 -5 11 47.81 3.00 -11 -5 12 0.63 0.60 -11 6 0 0.27 1.27 11 -6 0 -0.32 1.42 -11 6 0 2.03 2.50 11 6 0 1.27 1.31 11 6 0 0.65 1.28 11 6 0 0.65 1.35 -11 6 0 -0.34 1.57 -11 6 0 -0.83 1.92 11 6 1 35.96 3.17 11 -6 -1 35.68 3.52 11 -6 1 35.81 3.44 -11 6 -1 41.80 6.51 11 6 1 39.01 3.53 11 6 1 46.12 3.79 -11 6 1 38.12 3.61 -11 6 -1 37.87 3.70 11 6 -1 33.69 3.53 11 6 1 41.85 3.68 11 6 1 37.94 2.90 -11 6 1 38.53 5.33 -11 6 -1 37.14 5.36 11 6 -1 35.76 3.53 11 -6 -2 151.96 8.48 -11 6 -2 169.95 14.26 11 -6 2 139.06 7.98 11 6 2 146.08 8.46 11 6 -2 171.02 8.25 11 6 -2 162.13 8.66 11 6 2 153.28 8.50 11 6 2 146.93 7.44 -11 6 2 141.76 10.21 -11 6 2 168.08 8.77 -11 6 -2 149.68 8.62 -11 6 -2 149.45 11.15 11 -6 -3 1.25 1.59 -11 6 -3 2.82 3.66 11 -6 3 1.34 1.27 11 6 3 -1.25 1.54 11 6 3 1.25 1.24 11 6 -3 -0.25 1.21 11 6 -3 1.55 1.35 11 6 3 3.04 1.50 -11 6 3 2.84 1.85 -11 6 3 0.84 1.83 -11 6 -3 0.72 1.67 -11 6 3 1.24 1.30 -11 6 -3 1.28 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2.60 11 -7 5 28.13 2.79 -11 7 6 53.09 3.72 11 7 6 40.33 3.43 11 -7 -6 47.83 3.53 11 -7 6 44.58 3.67 11 7 -6 43.66 3.32 11 7 6 45.03 3.15 11 -7 6 49.69 3.60 11 -7 7 7.87 1.70 -11 -7 7 6.36 1.20 -11 7 7 5.45 1.39 11 -7 -7 6.32 1.41 11 7 -7 6.58 1.36 11 7 7 6.66 1.32 11 7 -7 6.77 1.38 11 -7 8 23.42 2.16 11 7 -8 21.70 1.91 11 7 8 22.21 1.87 11 -7 -8 20.81 1.87 11 7 -8 19.23 1.74 -11 -7 8 18.59 1.74 -11 7 8 20.09 1.97 -11 7 9 29.94 2.10 11 7 -9 26.01 1.65 -11 -7 9 26.76 1.82 -11 7 10 2.71 0.56 11 -8 0 0.24 1.24 11 8 0 2.72 1.79 11 8 0 0.56 1.61 -11 8 0 0.21 1.10 11 -8 1 217.84 10.57 11 8 -1 216.43 10.12 11 8 -1 227.29 10.93 11 8 1 210.94 10.98 11 8 -1 223.56 10.53 -11 8 1 204.72 10.46 11 8 -2 137.07 7.33 11 8 2 134.23 7.28 -11 8 2 126.05 7.11 11 8 2 123.57 7.13 11 8 2 140.14 7.56 11 8 -2 127.25 6.70 11 8 -2 138.38 7.09 11 -8 2 130.29 7.04 -11 8 3 7.45 1.73 11 8 3 14.15 1.80 11 8 -3 8.69 1.58 11 8 -3 11.42 2.24 11 8 3 10.11 2.04 11 8 -3 11.30 1.67 11 -8 3 7.17 1.62 11 8 -3 12.84 1.89 11 8 3 9.04 1.74 11 8 -4 79.74 5.22 11 8 4 83.40 5.07 11 8 -4 76.71 4.59 -11 8 4 73.61 4.92 11 -8 4 86.09 4.87 11 8 -4 84.43 4.77 -11 8 5 22.18 2.19 -11 8 5 18.05 2.18 11 8 -5 18.17 2.42 -11 8 -5 19.76 1.98 11 8 -5 17.39 1.79 11 8 -6 20.40 1.93 11 8 -6 23.40 1.96 -11 8 6 23.02 2.24 -11 8 6 22.18 2.08 11 8 -6 16.97 2.19 11 8 -7 12.24 1.38 11 8 -7 14.45 1.37 11 8 -7 11.36 1.53 -11 8 7 13.33 1.50 -11 8 7 11.17 1.54 11 8 -8 103.35 4.65 -11 8 8 110.36 4.81 -11 8 8 98.14 4.90 11 9 0 36.38 2.77 -11 9 0 32.11 2.88 11 9 -1 6.20 1.41 -11 9 -1 6.55 1.53 -11 9 1 7.15 1.59 11 9 1 5.79 1.59 11 9 2 4.45 1.23 11 9 -2 6.45 1.30 11 9 2 4.64 1.50 11 9 -2 6.88 1.59 -11 9 -2 1.74 1.28 -11 9 2 2.47 1.17 11 9 -3 3.34 1.35 11 9 -3 2.49 1.02 11 9 -3 2.32 0.83 -11 9 3 3.44 0.94 -11 9 -3 1.29 1.04 -11 9 4 141.42 6.23 11 9 -4 126.88 6.29 11 9 -4 116.78 5.71 -11 9 -4 111.12 5.81 -11 9 4 127.04 6.03 11 9 -4 126.53 5.84 11 9 -4 130.44 5.98 11 9 -5 60.14 3.12 -11 9 5 62.64 3.26 11 9 -5 62.18 3.39 -11 9 6 10.26 0.95 11 9 -6 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33.51 12 -1 7 160.81 8.41 -12 1 7 172.58 11.52 -12 1 7 192.23 11.68 -12 -1 7 152.94 10.32 12 1 7 152.94 7.98 12 -1 7 151.04 7.98 -12 -1 7 166.86 14.34 12 -1 7 154.74 7.91 12 1 7 155.16 7.61 12 1 7 151.24 7.98 12 1 8 32.71 2.96 12 1 8 44.07 3.24 12 -1 8 31.50 2.78 -12 -1 8 37.08 3.02 -12 1 8 29.27 2.80 12 -1 8 27.05 2.67 -12 -1 8 34.53 6.77 12 1 8 30.16 2.55 -12 1 8 33.97 4.67 -12 1 8 37.32 5.03 -12 1 9 0.71 1.54 12 1 9 1.84 1.26 -12 -1 9 0.24 1.00 -12 1 9 2.22 1.30 -12 -1 9 0.85 1.85 12 -1 9 0.22 0.95 12 1 9 1.58 1.02 12 1 9 0.77 1.53 12 -1 9 1.84 1.33 -12 -1 9 1.58 2.59 12 1 9 2.19 1.22 12 -1 9 1.37 1.34 -12 -1 10 50.33 3.80 -12 1 10 47.14 3.67 12 -1 10 52.57 3.69 12 -1 10 52.73 3.95 12 1 10 59.04 4.02 12 -1 11 0.67 1.30 12 1 11 0.39 1.17 -12 -1 11 0.86 1.13 -12 1 11 0.22 1.17 12 1 12 79.96 4.76 -12 -1 12 79.12 4.56 -12 1 12 84.08 4.67 12 -1 13 6.57 0.91 12 1 13 11.00 1.36 12 -1 13 11.27 1.36 -12 -1 13 13.24 1.23 -12 1 13 12.08 1.24 -12 1 13 7.40 0.84 12 -2 0 1.54 1.52 12 2 0 0.51 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12 -5 2 184.59 9.55 -12 5 2 195.54 11.77 12 5 2 189.03 9.20 12 -5 2 172.76 8.96 12 5 2 168.00 9.08 12 5 -2 168.94 8.70 12 5 2 170.44 8.56 -12 5 2 180.51 9.52 -12 5 -2 176.89 9.52 12 5 2 182.58 8.43 12 -5 -2 168.38 9.27 12 5 -2 163.11 9.18 12 5 2 163.66 9.16 12 5 -3 124.89 7.20 12 5 3 124.07 7.15 12 5 3 130.68 6.68 12 5 3 104.52 6.71 12 5 -3 129.15 7.51 -12 5 3 120.78 9.47 -12 5 3 137.29 10.33 -12 5 3 135.20 7.43 -12 5 -3 125.47 7.33 12 5 3 125.49 7.09 12 -5 3 125.77 7.07 12 5 -4 62.31 4.51 12 5 4 60.38 4.43 12 5 4 65.73 4.21 12 5 4 57.79 4.33 12 5 -4 66.69 4.93 -12 5 4 59.64 6.52 -12 5 4 64.42 6.76 -12 5 -4 71.08 4.78 -12 5 4 62.59 4.50 12 -5 4 67.45 4.88 12 5 4 60.94 4.51 12 -5 4 64.76 4.57 12 5 5 306.94 14.88 12 -5 5 327.50 15.19 -12 5 5 322.83 18.48 -12 5 5 307.05 18.54 12 5 -5 335.66 14.96 12 5 5 309.98 14.75 12 5 5 290.94 14.93 12 5 5 323.28 14.64 12 -5 5 343.81 15.68 12 5 5 319.24 14.43 -12 5 -5 329.62 14.95 -12 5 5 307.90 14.71 12 5 5 308.06 14.87 12 5 -5 314.53 15.39 12 5 6 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2.44 27 0 -5 0.12 0.76 27 0 5 0.16 0.97 27 0 -5 -0.36 0.75 27 0 -6 184.96 8.37 27 0 6 191.24 8.83 -27 0 6 198.19 8.69 -27 0 7 0.28 0.55 -27 0 8 1.76 0.45 27 1 0 2.97 1.31 27 1 0 3.34 1.78 27 -1 0 1.22 1.49 27 1 0 1.31 1.48 27 -1 -1 244.52 12.08 27 1 -1 263.35 12.34 27 -1 1 259.87 12.30 27 1 -1 263.02 12.43 27 1 -1 251.39 11.79 27 -1 -1 255.83 11.65 27 1 1 249.35 11.82 27 -1 2 82.89 5.15 27 -1 -2 78.53 4.85 27 -1 2 74.29 4.84 27 1 2 88.26 5.18 27 1 -2 77.75 5.03 27 1 2 91.10 5.21 27 1 -2 80.97 4.74 27 -1 -2 83.43 4.56 27 -1 3 24.70 2.62 27 -1 -3 20.56 2.13 27 1 3 28.38 2.59 27 1 -3 30.81 2.41 27 -1 -3 21.75 1.97 27 -1 3 23.00 2.02 27 1 -3 26.39 2.49 27 1 3 23.51 2.43 27 1 -4 4.74 1.17 27 -1 -4 6.93 1.10 27 -1 4 8.41 1.26 -27 1 -4 2.48 1.12 27 1 4 5.00 1.37 27 -1 4 3.48 1.37 27 1 -4 6.70 1.31 27 -1 4 4.82 1.46 27 1 -5 84.67 4.25 27 -1 -5 75.52 3.87 27 -1 5 84.35 4.20 27 -1 -5 67.46 3.93 27 1 -5 75.22 4.01 27 -1 5 83.49 4.55 27 -1 5 81.32 4.54 27 -1 6 9.58 1.16 -27 -1 6 9.72 1.23 -27 1 6 12.04 1.24 27 1 -6 7.83 1.10 27 -1 7 26.06 1.86 27 1 -7 22.24 1.49 -27 -1 7 26.97 1.69 -27 1 7 25.55 1.67 27 -1 7 22.64 1.62 -27 1 8 15.29 0.98 27 -2 0 0.65 1.37 27 2 0 0.25 1.31 27 2 1 10.23 1.58 27 2 1 7.70 1.85 27 2 -1 13.57 1.93 27 -2 -1 8.87 1.64 27 -2 1 9.18 1.86 27 2 2 49.18 3.68 27 -2 2 55.93 3.58 27 -2 -2 46.45 3.31 27 2 -2 54.62 3.78 27 2 2 52.29 3.66 -27 2 2 59.85 4.25 -27 2 -2 52.67 3.96 27 -2 -3 52.90 3.29 27 2 3 55.77 3.69 27 -2 3 56.23 3.63 27 2 -3 61.33 3.65 -27 2 3 65.31 4.24 -27 2 -3 48.41 3.80 27 2 -3 55.75 3.72 27 2 3 61.79 3.81 27 2 -4 2.89 1.14 27 -2 4 3.64 1.05 -27 2 -4 1.84 1.20 27 2 -4 2.08 0.97 27 -2 4 2.19 1.26 27 2 -5 13.19 1.50 27 -2 5 11.78 1.43 27 -2 5 13.94 1.77 -27 -2 5 19.86 1.55 -27 2 5 17.25 1.54 27 -2 5 15.34 1.77 27 2 -6 49.19 2.63 27 -2 6 42.30 2.60 27 -2 6 46.33 2.78 27 -2 6 44.38 2.81 -27 -2 6 42.84 2.46 27 2 -7 70.15 3.25 27 2 -7 71.45 3.55 27 3 0 26.66 2.17 -27 3 0 25.17 2.78 27 -3 0 19.95 2.11 27 3 0 26.89 2.54 27 3 -1 16.84 1.82 27 3 1 19.65 1.83 -27 3 -1 19.60 2.50 27 -3 1 19.40 2.10 27 3 -1 20.94 2.27 27 -3 -1 19.18 1.91 27 3 -2 4.99 1.23 27 -3 -2 4.11 0.98 -27 3 2 4.86 1.52 -27 3 -2 4.43 1.48 27 3 -2 5.65 1.49 27 3 2 4.54 1.37 27 -3 3 63.87 3.75 27 3 -3 64.78 3.77 -27 3 3 68.52 4.23 -27 3 -3 72.39 4.26 27 3 -3 70.69 4.06 27 3 3 63.69 3.93 -27 3 -4 15.48 1.63 27 -3 4 18.94 1.69 -27 -3 4 19.39 1.42 27 -3 4 14.86 1.66 27 3 -4 15.15 1.56 27 -3 5 188.78 7.55 -27 -3 5 149.73 6.92 27 3 -6 13.44 1.14 27 -3 6 11.07 1.14 27 -3 6 12.84 1.27 27 3 -6 12.62 1.32 27 4 0 -1.26 1.04 -27 4 0 -1.23 1.31 27 -4 0 -0.12 0.77 27 4 -1 5.13 1.27 27 -4 -1 6.45 0.92 -27 4 1 6.00 1.45 27 -4 1 6.72 1.25 -27 4 -1 8.68 1.60 27 4 -2 8.42 1.07 27 4 -2 8.69 1.45 27 4 2 7.39 1.34 -27 4 2 7.85 1.41 -27 4 -2 7.61 1.39 -27 4 -3 28.28 2.19 27 4 -3 26.10 2.14 27 4 -3 29.46 2.22 27 4 -3 33.88 2.04 27 -4 4 0.19 0.65 27 4 -4 -0.39 0.84 27 4 -4 -0.15 0.47 27 4 -4 0.43 0.58 27 -4 5 11.63 1.03 27 4 -5 11.11 0.96 -27 5 0 0.26 0.75 27 5 0 -0.12 0.73 27 5 1 14.78 1.35 27 5 -1 12.99 1.32 -27 5 1 14.41 1.42 -27 5 -1 12.99 1.34 27 -5 2 17.82 1.35 27 5 -2 21.36 1.59 27 5 2 19.74 1.53 -27 5 -2 23.07 1.64 -27 5 2 20.51 1.62 27 -5 3 6.08 0.78 27 -5 3 8.91 0.87 28 0 0 379.50 16.70 28 0 0 359.84 16.20 28 0 -1 -1.08 1.39 28 0 1 0.90 1.47 28 0 -1 -0.50 1.02 28 0 -2 2.35 1.12 28 0 -2 3.96 1.42 28 0 -3 0.14 0.85 28 0 3 0.59 1.24 28 0 -3 0.75 1.10 28 0 3 0.18 1.05 28 0 4 236.02 11.02 28 0 -4 241.39 10.81 28 0 -4 242.47 10.66 28 0 -5 0.75 0.72 -28 0 6 98.86 4.73 -28 0 7 -0.81 0.48 28 1 0 -0.52 1.13 28 1 0 1.57 1.45 28 -1 0 0.42 1.28 28 1 0 0.46 1.31 28 1 -1 -0.17 1.09 28 -1 -1 -1.00 1.24 28 -1 1 2.16 1.42 28 1 -1 0.22 1.27 28 1 -1 -0.44 1.42 28 1 -2 1.63 1.07 28 -1 -2 2.31 0.89 28 -1 -2 2.65 1.22 28 1 2 1.85 1.27 28 -1 2 1.26 1.32 28 1 -2 3.15 1.32 28 1 2 3.49 1.29 28 1 -3 63.48 3.68 28 -1 -3 58.36 3.39 28 1 -3 61.63 3.88 28 1 3 62.74 3.85 28 1 3 67.11 3.99 28 1 -4 230.46 9.79 28 -1 -4 207.25 9.39 28 1 4 221.21 9.91 28 -1 4 228.68 10.08 28 -1 4 236.52 10.19 28 -1 -4 208.00 9.74 28 1 -4 221.31 9.81 28 1 -5 21.33 1.67 -28 -1 5 20.95 1.71 -28 1 5 23.38 1.80 28 -1 5 21.78 1.95 28 -1 5 21.99 1.98 28 1 -6 8.65 0.91 -28 -1 6 10.43 1.03 -28 1 6 8.60 1.01 -28 -1 7 18.00 1.11 -28 1 7 17.18 1.13 -28 2 0 137.71 7.56 28 2 0 145.15 7.31 28 -2 0 135.37 7.04 -28 2 -1 80.91 5.02 28 2 -1 73.93 4.66 28 -2 1 79.51 4.64 28 -2 -1 79.37 4.47 -28 2 2 29.22 2.77 -28 2 -2 30.03 2.74 28 -2 2 28.20 2.55 28 -2 -2 25.94 2.10 28 2 -2 31.95 2.59 28 2 2 29.35 2.49 28 2 -3 2.82 1.05 28 -2 3 2.69 0.92 -28 2 3 1.42 1.11 -28 2 -3 3.37 1.24 28 -2 3 4.48 1.35 28 2 -3 2.97 1.09 28 2 3 2.26 1.01 28 -2 4 143.34 6.53 28 2 -4 135.76 6.34 28 -2 4 141.40 6.28 -28 2 -4 119.92 6.30 28 2 -4 124.60 6.25 28 2 -5 3.00 0.83 28 -2 5 1.23 0.73 28 -2 5 2.82 1.04 -28 -2 5 2.10 0.62 28 -2 5 2.86 1.01 28 -2 6 34.69 2.05 28 2 -6 30.82 1.80 28 2 -6 31.99 2.12 28 -2 6 31.65 1.85 -28 -2 6 28.68 1.64 28 3 0 -0.63 0.76 -28 3 0 0.22 1.24 28 -3 0 0.28 0.88 28 3 0 0.55 1.06 28 -3 -1 22.24 1.85 28 -3 1 25.50 2.08 -28 3 -1 22.80 2.33 28 3 -1 27.50 2.28 28 3 -1 18.96 1.80 28 -3 2 79.39 4.26 28 3 -2 76.01 4.00 28 3 -2 74.77 4.26 28 3 2 70.66 4.17 -28 3 2 71.07 4.43 -28 3 -2 73.08 4.36 28 -3 3 1.55 0.80 -28 3 -3 -0.14 0.78 28 -3 3 1.18 1.04 28 3 -3 1.49 0.81 28 3 -3 1.70 0.93 28 3 -3 1.35 0.87 -28 -3 3 1.42 0.57 -28 -3 4 0.65 0.39 28 -3 4 1.66 0.73 28 -3 4 1.96 0.91 28 3 -4 1.85 0.85 28 3 -4 1.09 0.58 28 3 -5 10.10 1.19 28 -3 5 9.32 0.99 28 3 -6 0.14 0.40 -28 4 0 54.96 3.19 28 4 0 52.17 3.00 28 -4 1 0.10 0.66 28 4 -1 1.10 0.92 28 4 1 1.22 0.91 -28 4 -1 1.04 0.86 -28 4 1 -0.92 0.91 -28 4 -2 53.95 3.07 -28 4 2 52.53 3.09 28 4 -2 50.54 2.98 28 4 2 52.04 2.97 28 -4 2 47.01 2.85 28 4 -3 0.09 0.55 28 -4 3 0.50 0.63 28 4 -4 4.76 0.73 28 -4 4 6.21 0.87 28 5 0 -0.08 0.48 28 5 -1 4.46 0.65 28 5 1 4.45 0.65 29 0 0 -0.57 1.22 29 0 0 0.40 1.24 29 0 -1 0.42 0.86 29 0 1 -0.19 1.12 29 0 -1 1.36 1.11 29 0 -1 0.90 1.06 29 0 -2 1.15 0.86 29 0 -2 2.31 1.14 29 0 2 0.88 1.08 29 0 -3 -0.22 0.80 29 0 3 0.16 0.97 29 0 -3 -0.59 0.91 29 0 3 0.15 0.92 29 0 -4 64.48 3.07 29 0 4 69.90 3.47 -29 0 5 0.18 0.64 -29 0 6 10.35 0.92 29 -1 0 122.86 6.28 29 1 0 118.76 6.35 29 1 -1 9.57 1.38 29 -1 -1 11.01 1.53 29 -1 1 12.77 1.77 29 1 -1 11.95 1.76 29 1 -2 3.76 1.14 29 -1 2 3.14 1.37 29 1 -2 3.43 1.16 29 1 2 3.37 1.17 29 1 2 2.88 1.25 29 1 3 34.68 2.60 29 1 -3 43.65 2.54 29 -1 -3 35.39 2.54 29 1 -3 41.28 2.67 -29 1 -3 34.91 2.66 29 -1 4 13.54 1.51 -29 1 -4 8.19 1.10 29 1 -4 13.00 1.27 29 1 -4 11.72 1.18 29 -1 -4 7.26 1.00 29 1 -5 16.80 1.30 -29 -1 5 21.61 1.44 -29 1 5 19.96 1.43 -29 -1 6 11.25 0.85 -29 1 6 10.38 0.85 29 2 0 0.17 0.99 -29 2 0 -0.21 1.11 29 -2 0 0.88 1.03 29 -2 1 20.90 2.01 29 -2 -1 21.29 1.82 29 2 -1 20.15 2.03 -29 2 -1 20.30 2.17 29 -2 2 27.15 2.24 -29 2 2 23.48 2.26 -29 2 -2 25.65 2.27 29 2 -2 28.54 2.21 29 2 2 26.71 2.18 29 2 -2 23.51 1.95 29 -2 3 22.03 1.95 29 2 -3 21.19 1.70 29 2 -3 19.45 1.78 -29 2 -3 19.03 1.76 29 2 -4 0.37 0.67 -29 -2 4 0.23 0.53 29 -2 -4 0.07 0.44 29 2 -4 0.65 0.50 29 2 -5 5.29 0.72 -29 -2 5 4.68 0.57 29 2 -5 4.91 0.84 29 -2 5 5.78 0.83 -29 3 0 9.27 1.47 29 -3 0 8.46 1.14 29 3 -1 37.13 2.24 -29 3 1 45.89 2.82 -29 3 -1 39.72 2.68 29 -3 1 38.06 2.41 29 -3 -1 29.36 1.99 29 3 -1 37.30 2.53 -29 -3 2 30.67 1.91 29 -3 2 46.84 2.61 29 3 -2 46.81 2.44 29 3 -2 43.97 2.60 29 3 2 43.32 2.55 -29 3 2 43.40 2.70 -29 3 -2 35.48 2.49 29 -3 3 1.58 0.64 29 -3 3 1.87 0.86 -29 3 -3 1.02 0.61 29 3 -3 1.35 0.61 29 3 -3 1.61 0.63 29 -3 4 8.30 0.84 29 -3 4 9.72 1.04 29 4 0 -0.10 0.61 -29 4 0 0.22 0.58 29 4 -1 0.09 0.57 29 4 1 0.09 0.56 -29 4 -1 0.10 0.55 -29 4 1 0.31 0.55 29 4 -2 50.86 2.47 29 -4 2 41.78 2.29 30 0 0 33.56 2.53 30 0 0 30.48 2.39 30 0 -1 0.46 0.90 30 0 1 -0.75 1.04 30 0 -2 68.12 3.75 30 0 2 66.21 3.75 30 0 -3 0.42 0.72 30 0 3 0.49 0.81 -30 0 -3 -0.12 0.71 -30 0 4 806.35 32.99 -30 0 5 0.11 0.38 30 -1 0 0.15 0.89 30 1 0 -0.76 0.86 30 -1 0 -0.82 0.93 -30 1 0 -0.54 1.10 30 -1 1 38.44 2.59 30 1 -1 42.52 2.69 30 -1 -1 34.75 2.56 -30 1 -1 34.77 2.68 30 -1 2 143.50 6.39 30 1 -2 124.35 6.00 30 -1 -2 126.76 6.20 30 -1 2 133.86 6.28 30 1 -2 133.90 6.24 30 1 2 135.82 6.25 -30 1 -2 117.14 6.25 -30 1 2 119.49 6.34 30 1 -3 37.31 2.09 30 -1 -3 32.56 2.05 30 1 -3 37.04 2.14 30 -1 4 253.09 10.89 30 1 -4 229.56 10.61 -30 -1 4 271.72 10.73 -30 1 4 259.96 10.74 -30 1 5 48.69 2.25 30 1 -5 42.02 2.35 -30 2 0 27.32 2.22 30 -2 0 26.29 1.93 30 2 0 28.86 2.17 -30 2 1 58.62 3.67 -30 2 -1 68.32 3.73 30 2 -1 68.40 3.60 30 2 1 58.48 3.45 30 -2 1 62.99 3.47 30 -2 -2 3.38 0.83 30 2 -2 2.47 0.76 30 2 2 1.44 0.71 -30 2 2 4.06 0.97 -30 2 -2 2.93 0.82 30 -2 2 2.64 0.89 30 2 -2 3.42 0.74 30 -2 3 103.92 4.08 30 2 -3 101.74 3.82 -30 3 0 0.23 0.68 30 3 0 -0.31 0.65 30 3 -1 4.20 0.82 30 3 1 5.30 0.86 -30 3 1 5.05 0.89 -30 3 -1 5.87 0.88 30 -3 1 3.71 0.66 30 3 -2 21.76 1.45 30 3 2 21.72 1.46 30 -3 2 21.40 1.46 30 -3 3 24.86 1.51 31 0 0 -0.47 0.79 -31 0 1 0.76 0.77 -31 0 -1 -0.62 0.75 31 0 -1 -0.22 0.63 31 0 1 -0.45 0.72 31 0 -2 48.58 2.38 31 0 2 56.15 2.51 31 -1 0 114.48 5.44 31 1 0 120.61 5.46 -31 1 0 104.25 5.47 31 -1 1 -0.10 0.66 -31 1 1 0.36 0.67 -31 1 -1 0.58 0.66 31 -1 -1 1.14 0.69 31 -1 1 0.21 0.71 31 1 -1 -0.10 0.59 31 1 1 0.73 0.63 31 -1 2 7.60 0.95 31 1 -2 7.27 0.91 31 1 2 7.47 0.92 31 -1 -2 7.45 0.90 31 -1 2 7.67 0.91 -31 -1 3 5.10 0.59 -31 1 3 5.26 0.62 -31 2 0 -0.20 0.54 31 -2 0 0.55 0.56 31 2 0 -0.27 0.55 31 2 -1 32.92 1.86 31 2 1 31.98 1.83 31 -2 1 32.57 1.73 31 -2 -2 4.39 0.61 31 -2 2 11.99 0.92 32 0 0 5.31 0.67 0 0 0 0.00 0.00 TITL HMB_yant_auto in Pbcn REM Pbcn (#60, found as Pbna in cab setting) CELL 1.54184 25.113360 8.387022 11.857041 90.0000 90.0000 90.0000 ZERR 5.00 0.000348 0.000109 0.000171 0.0000 0.0000 0.0000 LATT 1 SYMM -x+1/2,-y+1/2, z+1/2 SYMM -x, y,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H N O UNIT 110.00 150.00 10.00 20.00 REM CrysAlisPro recorded range (K): Min=99.9; max=100.1; aver:100.0 TEMP -173 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 79266 _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 1.475 _oxdiff_exptl_absorpt_empirical_full_min 0.674 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, 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 O1 O 0.61401(5) 0.60196(14) 0.53685(10) 0.0208(3) Uani 1 1 d . . . . . O2 O 0.56968(5) 0.42479(14) 0.64189(10) 0.0205(3) Uani 1 1 d . . . . . O5 O 0.85561(5) 0.86998(17) 0.81229(11) 0.0276(3) Uani 1 1 d G . . . . H5A H 0.870354 0.882650 0.878087 0.041 Uiso 1 1 d G U . . . H5B H 0.880875 0.891800 0.764357 0.041 Uiso 1 1 d G U . . . N1 N 0.65490(6) 0.08612(16) 0.51783(13) 0.0198(3) Uani 1 1 d . . . . . O4 O 0.74950(7) 0.8799(2) 0.77437(14) 0.0438(4) Uani 1 1 d G . . . . H4A H 0.735825 0.797349 0.740789 0.066 Uiso 1 1 d G U . . . H4B H 0.782140 0.851977 0.789285 0.066 Uiso 1 1 d G U . . . C10 C 0.57240(6) 0.52275(19) 0.56301(13) 0.0160(4) Uani 1 1 d . . . . . C11 C 0.52308(6) 0.55743(19) 0.49130(14) 0.0168(4) Uani 1 1 d . . . . . H11A H 0.510628 0.666784 0.508395 0.020 Uiso 1 1 calc R U . . . H11B H 0.533491 0.554837 0.410783 0.020 Uiso 1 1 calc R U . . . C1 C 0.60913(6) 0.09141(19) 0.43664(14) 0.0176(4) Uani 1 1 d . . . . . C9 C 0.68579(7) 0.2395(2) 0.51961(16) 0.0239(4) Uani 1 1 d . . . . . H9A H 0.699226 0.262477 0.443730 0.036 Uiso 1 1 calc R U . . . H9B H 0.715806 0.229564 0.571955 0.036 Uiso 1 1 calc R U . . . H9C H 0.662491 0.326487 0.544294 0.036 Uiso 1 1 calc R U . . . C7 C 0.63389(8) 0.0566(2) 0.63521(16) 0.0280(4) Uani 1 1 d . . . . . H7A H 0.607844 0.139213 0.654554 0.042 Uiso 1 1 calc R U . . . H7B H 0.663421 0.059729 0.689184 0.042 Uiso 1 1 calc R U . . . H7C H 0.616751 -0.048291 0.638119 0.042 Uiso 1 1 calc R U . . . C8 C 0.69239(7) -0.0475(2) 0.48708(19) 0.0288(4) Uani 1 1 d . . . . . H8A H 0.673059 -0.148957 0.488004 0.043 Uiso 1 1 calc R U . . . H8B H 0.721613 -0.051518 0.541772 0.043 Uiso 1 1 calc R U . . . H8C H 0.706854 -0.028701 0.411468 0.043 Uiso 1 1 calc R U . . . C4 C 0.52282(6) 0.09226(19) 0.28961(14) 0.0176(4) Uani 1 1 d . . . . . C2 C 0.59834(7) 0.22694(19) 0.37410(14) 0.0190(4) Uani 1 1 d . . . . . H2 H 0.620298 0.318683 0.380753 0.023 Uiso 1 1 calc R U . . . C6 C 0.57759(7) -0.04414(19) 0.42718(15) 0.0187(4) Uani 1 1 d . . . . . H6 H 0.585283 -0.136318 0.470803 0.022 Uiso 1 1 calc R U . . . C5 C 0.53478(7) -0.04327(19) 0.35335(14) 0.0186(4) Uani 1 1 d . . . . . H5 H 0.513308 -0.135948 0.345994 0.022 Uiso 1 1 calc R U . . . C3 C 0.55489(7) 0.22692(19) 0.30138(14) 0.0195(4) Uani 1 1 d . . . . . H3 H 0.546946 0.320109 0.259059 0.023 Uiso 1 1 calc R U . . . O6 O 0.70439(6) 0.6366(2) 0.66011(16) 0.0502(5) Uani 1 1 d G . . . . H6A H 0.673933 0.624782 0.626070 0.075 Uiso 1 1 d G U . . . H6B H 0.708854 0.548069 0.697107 0.075 Uiso 1 1 d G U . . . 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 O1 0.0166(6) 0.0219(6) 0.0239(6) 0.0023(5) -0.0025(5) -0.0030(5) O2 0.0197(6) 0.0210(6) 0.0207(6) 0.0042(5) -0.0023(5) 0.0007(5) O5 0.0204(6) 0.0399(8) 0.0224(6) 0.0003(6) 0.0008(5) -0.0066(5) N1 0.0176(7) 0.0152(7) 0.0266(8) -0.0031(6) -0.0022(6) 0.0003(5) O4 0.0359(8) 0.0551(10) 0.0405(9) -0.0092(8) -0.0009(7) 0.0071(7) C10 0.0164(8) 0.0136(8) 0.0181(8) -0.0025(6) -0.0001(6) 0.0021(6) C11 0.0149(8) 0.0145(7) 0.0209(8) 0.0026(6) -0.0010(6) 0.0005(6) C1 0.0168(8) 0.0172(8) 0.0189(8) -0.0026(6) 0.0007(6) 0.0003(6) C9 0.0200(8) 0.0186(8) 0.0333(10) -0.0058(7) -0.0035(7) -0.0034(7) C7 0.0308(10) 0.0302(10) 0.0230(9) 0.0026(8) -0.0057(7) -0.0022(8) C8 0.0213(9) 0.0208(9) 0.0442(11) -0.0080(8) -0.0041(8) 0.0047(7) C4 0.0207(8) 0.0154(8) 0.0167(8) -0.0012(6) 0.0020(7) 0.0010(6) C2 0.0224(8) 0.0139(8) 0.0207(8) -0.0024(6) 0.0026(6) -0.0034(6) C6 0.0201(8) 0.0132(8) 0.0227(8) 0.0010(6) 0.0001(7) 0.0007(6) C5 0.0192(8) 0.0135(8) 0.0230(8) 0.0003(6) 0.0000(6) -0.0020(6) C3 0.0274(9) 0.0140(8) 0.0171(8) 0.0007(6) 0.0008(7) -0.0007(6) O6 0.0289(8) 0.0648(12) 0.0570(11) 0.0139(9) -0.0165(7) -0.0117(8) 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' 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 H5A O5 H5B 104.4 . . ? C1 N1 C9 112.30(13) . . ? C1 N1 C7 109.20(13) . . ? C1 N1 C8 110.19(13) . . ? C9 N1 C7 107.95(14) . . ? C9 N1 C8 108.49(13) . . ? C8 N1 C7 108.63(15) . . ? H4A O4 H4B 104.5 . . ? O1 C10 C11 115.38(14) . . ? O2 C10 O1 124.75(14) . . ? O2 C10 C11 119.86(14) . . ? C10 C11 H11A 108.5 . . ? C10 C11 H11B 108.5 . . ? C11 C11 C10 114.90(17) 5_666 . ? C11 C11 H11A 108.5 5_666 . ? C11 C11 H11B 108.5 5_666 . ? H11A C11 H11B 107.5 . . ? C2 C1 N1 121.21(14) . . ? C2 C1 C6 121.13(15) . . ? C6 C1 N1 117.66(14) . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C4 C4 120.59(11) . 3_655 ? C3 C4 C4 120.68(11) . 3_655 ? C3 C4 C5 118.72(15) . . ? C1 C2 H2 120.5 . . ? C1 C2 C3 119.06(15) . . ? C3 C2 H2 120.5 . . ? C1 C6 H6 120.4 . . ? C5 C6 C1 119.24(15) . . ? C5 C6 H6 120.4 . . ? C4 C5 H5 119.6 . . ? C6 C5 C4 120.82(15) . . ? C6 C5 H5 119.6 . . ? C4 C3 H3 119.5 . . ? C2 C3 C4 121.02(15) . . ? C2 C3 H3 119.5 . . ? H6A O6 H6B 104.5 . . ? 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 O1 C10 1.277(2) . ? O2 C10 1.247(2) . ? O5 H5A 0.8700 . ? O5 H5B 0.8712 . ? N1 C1 1.500(2) . ? N1 C9 1.502(2) . ? N1 C7 1.509(2) . ? N1 C8 1.508(2) . ? O4 H4A 0.8697 . ? O4 H4B 0.8707 . ? C10 C11 1.530(2) . ? C11 C11 1.521(3) 5_666 ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C1 C2 1.384(2) . ? C1 C6 1.390(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C4 C4 1.482(3) 3_655 ? C4 C5 1.398(2) . ? C4 C3 1.394(2) . ? C2 H2 0.9500 . ? C2 C3 1.391(2) . ? C6 H6 0.9500 . ? C6 C5 1.386(2) . ? C5 H5 0.9500 . ? C3 H3 0.9500 . ? O6 H6A 0.8704 . ? O6 H6B 0.8700 . ? 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 O1 C10 C11 C11 169.51(17) . . . 5_666 ? O2 C10 C11 C11 -11.7(3) . . . 5_666 ? N1 C1 C2 C3 -178.89(15) . . . . ? N1 C1 C6 C5 179.69(15) . . . . ? C1 C2 C3 C4 -0.9(2) . . . . ? C1 C6 C5 C4 -0.6(2) . . . . ? C9 N1 C1 C2 -0.8(2) . . . . ? C9 N1 C1 C6 179.79(15) . . . . ? C7 N1 C1 C2 118.88(17) . . . . ? C7 N1 C1 C6 -60.52(19) . . . . ? C8 N1 C1 C2 -121.88(17) . . . . ? C8 N1 C1 C6 58.7(2) . . . . ? C4 C4 C5 C6 179.68(18) 3_655 . . . ? C4 C4 C3 C2 -178.88(18) 3_655 . . . ? C2 C1 C6 C5 0.3(2) . . . . ? C6 C1 C2 C3 0.5(2) . . . . ? C5 C4 C3 C2 0.6(2) . . . . ? C3 C4 C5 C6 0.2(2) . . . . ?