#------------------------------------------------------------------------------ #$Date: 2019-11-11 20:37:42 +0200 (Mon, 11 Nov 2019) $ #$Revision: 227286 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/58/4035878.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_4035878 loop_ _publ_author_name 'Zhao, Meng-Yao' 'Wang, De-Xian' 'Wang, Mei-Xiang' _publ_section_title ; Synthesis, Structure, and Properties of Corona[6]arenes and Their Assembly with Anions in the Crystalline State. ; _journal_issue 3 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 1502 _journal_page_last 1509 _journal_paper_doi 10.1021/acs.joc.7b03136 _journal_volume 83 _journal_year 2018 _chemical_formula_moiety 'C30 H19 N9 O7 S, 2(C2 H3 N)' _chemical_formula_sum 'C34 H25 N11 O7 S' _chemical_formula_weight 731.71 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2017-05-26 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 23.99410(19) _cell_length_b 11.75950(8) _cell_length_c 24.61960(16) _cell_measurement_reflns_used 5771 _cell_measurement_temperature 173.2(3) _cell_measurement_theta_max 76.5120 _cell_measurement_theta_min 4.0150 _cell_volume 6946.63(9) _computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (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)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 173.2(3) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2137 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.989 _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 -51.00 -1.00 1.00 4.76 -- -40.81 -19.00 60.00 50 2 \w 10.00 49.00 1.00 4.76 -- 40.81 -99.00 30.00 39 3 \w 38.00 64.00 1.00 19.04 -- 112.00-111.00 60.00 26 4 \w 88.00 114.00 1.00 19.04 -- 112.00-111.00 60.00 26 5 \w 100.00 136.00 1.00 19.04 -- 112.00 -45.00 60.00 36 6 \w 87.00 133.00 1.00 19.04 -- 112.00 30.00-120.00 46 7 \w 85.00 151.00 1.00 19.04 -- 112.00 30.00-180.00 66 8 \w 42.00 93.00 1.00 19.04 -- 112.00 -95.00-120.00 51 9 \w 41.00 71.00 1.00 19.04 -- 112.00-111.00 -60.00 30 10 \w 48.00 84.00 1.00 19.04 -- 112.00 -45.00 60.00 36 11 \w 111.00 171.00 1.00 19.04 -- 112.00 111.00 90.00 60 12 \w -41.00 -13.00 1.00 4.76 -- -40.81 -57.00-120.00 28 13 \w -112.00 -86.00 1.00 4.76 -- -40.81 -57.00-120.00 26 14 \w -121.00 -55.00 1.00 4.76 -- -40.81 -19.00 60.00 66 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0257527000 _diffrn_orient_matrix_UB_12 -0.0658476000 _diffrn_orient_matrix_UB_13 0.0478813000 _diffrn_orient_matrix_UB_21 0.0345063000 _diffrn_orient_matrix_UB_22 0.0717056000 _diffrn_orient_matrix_UB_23 0.0402082000 _diffrn_orient_matrix_UB_31 -0.0476437000 _diffrn_orient_matrix_UB_32 0.0875429000 _diffrn_orient_matrix_UB_33 0.0031075000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_unetI/netI 0.0408 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 22650 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.929 _diffrn_reflns_theta_min 3.591 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.390 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.57400 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.399 _exptl_crystal_description block _exptl_crystal_F_000 3024 _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.3 _refine_diff_density_max 0.757 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.049 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 481 _refine_ls_number_reflns 7254 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0445 _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^)+(0.0620P)^2^+1.2860P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1125 _refine_ls_wR_factor_ref 0.1246 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5543 _reflns_number_total 7254 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; zmy20170522-424.res created by SHELXL-2014/7 TITL zmy20170522-424_a.res in Pbca REM Old TITL zmy20170522-424 in Pbca REM SHELXT solution in Pbca REM R1 0.149, Rweak 0.013, Alpha 0.020, Orientation as input REM Formula found by SHELXT: C38 N12 O2 Cl CELL 1.54184 23.9941 11.7595 24.6196 90 90 90 ZERR 8 0.000187 0.00008 0.00016 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 N O S UNIT 272 200 88 56 8 L.S. 20 PLAN 20 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.062000 1.286000 FVAR 0.14656 S1 5 0.539958 0.559672 0.609669 11.00000 0.02504 0.03416 = 0.03277 0.00072 0.00487 -0.00453 O3 4 0.356069 0.362225 0.961219 11.00000 0.02436 0.05278 = 0.02524 0.00121 -0.00117 -0.00508 O7 4 0.062211 0.183934 0.871016 11.00000 0.03135 0.04100 = 0.02901 0.00189 -0.00342 -0.01017 O1 4 0.326665 0.399611 0.519459 11.00000 0.03268 0.05650 = 0.02341 -0.00271 0.00125 -0.01220 O2 4 0.162300 0.266781 0.641022 11.00000 0.03914 0.05344 = 0.02119 0.00171 -0.00133 -0.01939 O5 4 0.543441 0.681199 0.604298 11.00000 0.04621 0.03700 = 0.04725 0.00782 -0.00129 -0.01531 O6 4 0.583904 0.489734 0.588292 11.00000 0.02579 0.06165 = 0.04038 -0.00354 0.00859 0.00341 N5 3 0.153340 0.233933 0.867507 11.00000 0.02875 0.03468 = 0.02024 -0.00034 -0.00291 -0.00554 N9 3 0.389392 0.404693 0.875773 11.00000 0.02546 0.03333 = 0.02945 0.00608 -0.00262 -0.00158 N3 3 0.237863 0.345570 0.529024 11.00000 0.03269 0.03508 = 0.02189 0.00175 -0.00163 -0.00536 N4 3 0.196508 0.312207 0.560038 11.00000 0.03324 0.03371 = 0.02200 0.00193 -0.00195 -0.00683 O4 4 0.529022 0.453272 0.842904 11.00000 0.02417 0.11466 = 0.03519 0.01366 -0.00030 -0.00724 N8 3 0.434047 0.427151 0.845165 11.00000 0.02743 0.03307 = 0.03050 0.00604 -0.00100 -0.00278 N2 3 0.254721 0.325979 0.638357 11.00000 0.03516 0.03951 = 0.02282 0.00339 -0.00371 -0.00887 N6 3 0.446908 0.402788 0.954695 11.00000 0.02586 0.04055 = 0.02859 -0.00275 -0.00284 -0.00251 N1 3 0.297067 0.358399 0.606780 11.00000 0.03401 0.03840 = 0.02392 0.00121 -0.00270 -0.00604 N7 3 0.490737 0.426845 0.924904 11.00000 0.02661 0.04693 = 0.03152 0.00001 -0.00282 -0.00554 C17 1 0.398402 0.389903 0.928134 11.00000 0.02529 0.02672 = 0.02895 -0.00071 -0.00131 0.00126 C6 1 0.154427 0.242457 0.809083 11.00000 0.02887 0.03471 = 0.02058 0.00060 -0.00016 -0.00533 C9 1 0.106265 0.202357 0.894808 11.00000 0.03111 0.02891 = 0.02398 0.00082 -0.00074 -0.00361 C28 1 0.377310 0.438107 0.541685 11.00000 0.02982 0.04132 = 0.02291 0.00011 0.00268 -0.00632 C12 1 0.208713 0.366688 0.922524 11.00000 0.02687 0.03143 = 0.02979 -0.00258 -0.00192 0.00336 AFIX 43 H12 2 0.177366 0.412154 0.927212 11.00000 -1.20000 AFIX 0 C2 1 0.207198 0.303581 0.613493 11.00000 0.03467 0.03087 = 0.02047 0.00078 -0.00094 -0.00744 C1 1 0.286438 0.367056 0.554181 11.00000 0.03229 0.02871 = 0.02321 -0.00054 -0.00005 -0.00482 C22 1 0.532693 0.527949 0.679515 11.00000 0.02326 0.03346 = 0.03297 -0.00126 0.00319 -0.00171 C13 1 0.259892 0.399651 0.944484 11.00000 0.03082 0.03087 = 0.02717 -0.00475 -0.00135 -0.00193 AFIX 43 H13 2 0.263328 0.467173 0.963863 11.00000 -1.20000 AFIX 0 C11 1 0.204974 0.265870 0.893732 11.00000 0.02607 0.03209 = 0.02087 0.00131 -0.00164 -0.00323 C15 1 0.302166 0.228232 0.908534 11.00000 0.02831 0.03495 = 0.02764 0.00314 0.00350 0.00435 AFIX 43 H15 2 0.333462 0.182404 0.904355 11.00000 -1.20000 AFIX 0 C16 1 0.251187 0.196883 0.886696 11.00000 0.03303 0.02836 = 0.02581 -0.00233 0.00183 -0.00041 AFIX 43 H16 2 0.248010 0.129363 0.867274 11.00000 -1.20000 AFIX 0 C25 1 0.476529 0.513717 0.580585 11.00000 0.02564 0.02980 = 0.02858 -0.00091 0.00387 -0.00177 C14 1 0.305041 0.329608 0.936684 11.00000 0.02493 0.03830 = 0.02157 0.00310 -0.00044 -0.00379 C3 1 0.162952 0.260451 0.698078 11.00000 0.03597 0.04069 = 0.02001 0.00102 -0.00025 -0.01059 N11 3 0.230397 0.589540 0.582142 11.00000 0.06193 0.04516 = 0.06844 -0.00710 0.01037 -0.00235 C18 1 0.481882 0.435118 0.870960 11.00000 0.02463 0.04077 = 0.03059 0.00127 -0.00023 -0.00429 C27 1 0.380255 0.546711 0.561823 11.00000 0.02751 0.03914 = 0.03849 -0.00410 0.00254 0.00456 AFIX 43 H27 2 0.348895 0.593179 0.562173 11.00000 -1.20000 AFIX 0 C5 1 0.172213 0.343279 0.785688 11.00000 0.04295 0.03310 = 0.02569 -0.00207 -0.00019 -0.01235 AFIX 43 H5 2 0.181415 0.404766 0.807688 11.00000 -1.20000 AFIX 0 C26 1 0.430877 0.586055 0.581678 11.00000 0.03252 0.02915 = 0.03791 -0.00579 0.00167 0.00280 AFIX 43 H26 2 0.434107 0.659419 0.595429 11.00000 -1.20000 AFIX 0 C10 1 0.110724 0.190804 0.955554 11.00000 0.03722 0.04519 = 0.02276 0.00218 -0.00011 -0.00623 AFIX 137 H10A 2 0.111584 0.264999 0.971797 11.00000 -1.50000 H10B 2 0.144302 0.150608 0.964552 11.00000 -1.50000 H10C 2 0.079131 0.149440 0.969046 11.00000 -1.50000 AFIX 0 C8 1 0.144600 0.159857 0.720316 11.00000 0.04327 0.03659 = 0.02571 -0.00536 0.00098 -0.01307 AFIX 43 H8 2 0.135314 0.098729 0.698124 11.00000 -1.20000 AFIX 0 C7 1 0.140132 0.150930 0.776609 11.00000 0.04419 0.03105 = 0.02637 0.00054 0.00161 -0.00987 AFIX 43 H7 2 0.127587 0.083689 0.792291 11.00000 -1.20000 AFIX 0 C29 1 0.422767 0.366294 0.539051 11.00000 0.04272 0.02982 = 0.03614 -0.00779 0.00100 -0.00215 AFIX 43 H29 2 0.419619 0.293890 0.524167 11.00000 -1.20000 AFIX 0 C4 1 0.176405 0.353202 0.729581 11.00000 0.04787 0.03346 = 0.02806 0.00351 0.00038 -0.01337 AFIX 43 H4 2 0.188026 0.420918 0.713691 11.00000 -1.20000 AFIX 0 C30 1 0.473292 0.405250 0.559250 11.00000 0.03402 0.03381 = 0.04050 -0.00545 0.00061 0.00652 AFIX 43 H30 2 0.504651 0.358802 0.558429 11.00000 -1.20000 AFIX 0 C19 1 0.525711 0.477999 0.787293 11.00000 0.02353 0.06848 = 0.03231 0.00551 0.00100 -0.00579 C34 1 0.184261 0.584180 0.589960 11.00000 0.06026 0.03797 = 0.05581 0.00674 0.01479 -0.00204 C23 1 0.538678 0.416758 0.696242 11.00000 0.05667 0.03529 = 0.04107 -0.00104 0.00099 -0.00398 AFIX 43 H23 2 0.544415 0.359178 0.670959 11.00000 -1.20000 AFIX 0 C24 1 0.536045 0.391849 0.751137 11.00000 0.05411 0.04618 = 0.04618 0.00979 -0.00194 -0.00946 AFIX 43 H24 2 0.541211 0.317737 0.763320 11.00000 -1.20000 AFIX 0 C21 1 0.523807 0.613656 0.716411 11.00000 0.08041 0.04119 = 0.04352 -0.00278 0.00497 0.01911 AFIX 43 H21 2 0.520463 0.688463 0.704596 11.00000 -1.20000 AFIX 0 C20 1 0.519814 0.588428 0.771465 11.00000 0.08260 0.06545 = 0.03761 -0.01073 0.00616 0.02552 AFIX 43 H20 2 0.513286 0.645469 0.796844 11.00000 -1.20000 AFIX 0 C31 1 0.171356 0.840896 0.753875 11.00000 0.12235 0.07958 = 0.08578 0.01457 0.06137 0.04052 AFIX 137 H31A 2 0.198290 0.878183 0.731198 11.00000 -1.50000 H31B 2 0.175387 0.867091 0.790597 11.00000 -1.50000 H31C 2 0.134504 0.858117 0.741113 11.00000 -1.50000 AFIX 0 C32 1 0.180241 0.719133 0.751942 11.00000 0.11211 0.07991 = 0.06849 -0.00748 0.01237 -0.01683 C33 1 0.124992 0.576392 0.599007 11.00000 0.06050 0.10209 = 0.10424 0.04261 0.02861 0.00027 AFIX 137 H33A 2 0.106494 0.561590 0.565162 11.00000 -1.50000 H33B 2 0.111637 0.646751 0.613895 11.00000 -1.50000 H33C 2 0.117397 0.515650 0.623985 11.00000 -1.50000 AFIX 0 N10 3 0.187265 0.627146 0.751903 11.00000 0.24814 0.05244 = 0.14871 -0.01713 -0.00009 -0.03364 HKLF 4 REM zmy20170522-424_a.res in Pbca REM R1 = 0.0445 for 5543 Fo > 4sig(Fo) and 0.0638 for all 7254 data REM 481 parameters refined using 0 restraints END WGHT 0.0618 1.2862 REM Highest difference peak 0.757, deepest hole -0.350, 1-sigma level 0.049 Q1 1 0.0965 0.8253 0.7013 11.00000 0.05 0.76 Q2 1 0.5361 0.5523 0.6499 11.00000 0.05 0.28 Q3 1 0.2032 0.9042 0.7703 11.00000 0.05 0.28 Q4 1 0.5054 0.4213 0.7546 11.00000 0.05 0.26 Q5 1 0.3035 0.2822 0.9208 11.00000 0.05 0.24 Q6 1 0.2003 0.6442 0.7560 11.00000 0.05 0.24 Q7 1 0.1587 0.6316 0.7251 11.00000 0.05 0.22 Q8 1 0.1092 0.1978 0.9248 11.00000 0.05 0.22 Q9 1 0.1563 0.7520 0.7203 11.00000 0.05 0.21 Q10 1 0.1424 0.1639 0.7490 11.00000 0.05 0.21 Q11 1 0.2324 0.5859 0.6190 11.00000 0.05 0.20 Q12 1 0.1615 0.2058 0.7150 11.00000 0.05 0.20 Q13 1 0.0999 0.6362 0.5849 11.00000 0.05 0.19 Q14 1 0.1311 0.5785 0.6397 11.00000 0.05 0.19 Q15 1 0.5133 0.4527 0.6899 11.00000 0.05 0.19 Q16 1 0.2310 0.3603 0.9418 11.00000 0.05 0.18 Q17 1 0.5273 0.6373 0.6011 11.00000 0.05 0.18 Q18 1 0.1656 0.2793 0.7974 11.00000 0.05 0.17 Q19 1 0.5816 0.4789 0.6177 11.00000 0.05 0.17 Q20 1 0.1563 0.2316 0.8395 11.00000 0.05 0.17 REM The information below was added by Olex2. REM REM R1 = 0.0445 for 5543 Fo > 4sig(Fo) and 0.0638 for all 24134 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.76, deepest hole -0.35 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0638 REM R1_gt = 0.0445 REM wR_ref = 0.1246 REM GOOF = 1.022 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 24134 REM Reflections_gt = 5543 REM Parameters = n/a REM Hole = -0.35 REM Peak = 0.76 REM Flack = n/a ; _cod_data_source_file jo7b03136_si_002.cif _cod_data_source_block zmy20170522-424 _cod_original_cell_volume 6946.63(8) _cod_database_code 4035878 _shelx_shelxl_version_number 2014/7 _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. ; _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 64.99 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C12(H12), C13(H13), C15(H15), C16(H16), C27(H27), C5(H5), C26(H26), C8(H8), C7(H7), C29(H29), C4(H4), C30(H30), C23(H23), C24(H24), C21(H21), C20(H20) 2.b Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C) ; _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 1.586 _oxdiff_exptl_absorpt_empirical_full_min 0.629 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' '-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 S1 S 0.53996(2) 0.55967(4) 0.60967(2) 0.03066(12) Uani 1 1 d . O3 O 0.35607(6) 0.36223(14) 0.96122(5) 0.0341(3) Uani 1 1 d . O7 O 0.06221(6) 0.18393(13) 0.87102(5) 0.0338(3) Uani 1 1 d . O1 O 0.32667(6) 0.39961(14) 0.51946(5) 0.0375(3) Uani 1 1 d . O2 O 0.16230(6) 0.26678(14) 0.64102(5) 0.0379(3) Uani 1 1 d . O5 O 0.54344(7) 0.68120(14) 0.60430(6) 0.0435(4) Uani 1 1 d . O6 O 0.58390(6) 0.48973(16) 0.58829(6) 0.0426(4) Uani 1 1 d . N5 N 0.15334(7) 0.23393(14) 0.86751(6) 0.0279(3) Uani 1 1 d . N9 N 0.38939(7) 0.40469(14) 0.87577(6) 0.0294(3) Uani 1 1 d . N3 N 0.23786(7) 0.34557(15) 0.52902(6) 0.0299(3) Uani 1 1 d . N4 N 0.19651(7) 0.31221(14) 0.56004(6) 0.0297(3) Uani 1 1 d . O4 O 0.52902(6) 0.4533(2) 0.84290(6) 0.0580(6) Uani 1 1 d . N8 N 0.43405(7) 0.42715(14) 0.84516(6) 0.0303(3) Uani 1 1 d . N2 N 0.25472(7) 0.32598(15) 0.63836(6) 0.0325(4) Uani 1 1 d . N6 N 0.44691(7) 0.40279(15) 0.95469(6) 0.0317(3) Uani 1 1 d . N1 N 0.29707(7) 0.35840(15) 0.60678(6) 0.0321(4) Uani 1 1 d . N7 N 0.49074(7) 0.42685(17) 0.92490(7) 0.0350(4) Uani 1 1 d . C17 C 0.39840(8) 0.38990(16) 0.92813(7) 0.0270(4) Uani 1 1 d . C6 C 0.15443(8) 0.24246(17) 0.80908(7) 0.0281(4) Uani 1 1 d . C9 C 0.10626(8) 0.20236(16) 0.89481(7) 0.0280(4) Uani 1 1 d . C28 C 0.37731(8) 0.43811(19) 0.54168(7) 0.0314(4) Uani 1 1 d . C12 C 0.20871(8) 0.36669(17) 0.92252(7) 0.0294(4) Uani 1 1 d . H12 H 0.1774 0.4122 0.9272 0.035 Uiso 1 1 calc R C2 C 0.20720(9) 0.30358(16) 0.61349(7) 0.0287(4) Uani 1 1 d . C1 C 0.28644(8) 0.36706(16) 0.55418(7) 0.0281(4) Uani 1 1 d . C22 C 0.53269(8) 0.52795(17) 0.67952(8) 0.0299(4) Uani 1 1 d . C13 C 0.25989(8) 0.39965(17) 0.94448(7) 0.0296(4) Uani 1 1 d . H13 H 0.2633 0.4672 0.9639 0.036 Uiso 1 1 calc R C11 C 0.20497(8) 0.26587(16) 0.89373(7) 0.0263(4) Uani 1 1 d . C15 C 0.30217(8) 0.22823(17) 0.90853(7) 0.0303(4) Uani 1 1 d . H15 H 0.3335 0.1824 0.9044 0.036 Uiso 1 1 calc R C16 C 0.25119(8) 0.19688(16) 0.88670(7) 0.0291(4) Uani 1 1 d . H16 H 0.2480 0.1294 0.8673 0.035 Uiso 1 1 calc R C25 C 0.47653(8) 0.51372(17) 0.58059(7) 0.0280(4) Uani 1 1 d . C14 C 0.30504(8) 0.32961(17) 0.93668(7) 0.0283(4) Uani 1 1 d . C3 C 0.16295(9) 0.26045(18) 0.69808(7) 0.0322(4) Uani 1 1 d . N11 N 0.23040(11) 0.5895(2) 0.58214(11) 0.0585(6) Uani 1 1 d . C18 C 0.48188(8) 0.43512(19) 0.87096(8) 0.0320(4) Uani 1 1 d . C27 C 0.38026(9) 0.54671(19) 0.56182(8) 0.0350(4) Uani 1 1 d . H27 H 0.3489 0.5932 0.5622 0.042 Uiso 1 1 calc R C5 C 0.17221(9) 0.34328(18) 0.78569(8) 0.0339(4) Uani 1 1 d . H5 H 0.1814 0.4048 0.8077 0.041 Uiso 1 1 calc R C26 C 0.43088(9) 0.58606(17) 0.58168(8) 0.0332(4) Uani 1 1 d . H26 H 0.4341 0.6594 0.5954 0.040 Uiso 1 1 calc R C10 C 0.11072(9) 0.19080(19) 0.95555(7) 0.0351(4) Uani 1 1 d . H10A H 0.1116 0.2650 0.9718 0.053 Uiso 1 1 calc GR H10B H 0.1443 0.1506 0.9646 0.053 Uiso 1 1 calc GR H10C H 0.0791 0.1494 0.9690 0.053 Uiso 1 1 calc GR C8 C 0.14460(9) 0.15986(18) 0.72032(8) 0.0352(4) Uani 1 1 d . H8 H 0.1353 0.0987 0.6981 0.042 Uiso 1 1 calc R C7 C 0.14013(9) 0.15093(18) 0.77661(8) 0.0339(4) Uani 1 1 d . H7 H 0.1276 0.0837 0.7923 0.041 Uiso 1 1 calc R C29 C 0.42277(10) 0.36629(18) 0.53905(8) 0.0362(4) Uani 1 1 d . H29 H 0.4196 0.2939 0.5242 0.043 Uiso 1 1 calc R C4 C 0.17640(10) 0.35320(18) 0.72958(8) 0.0365(5) Uani 1 1 d . H4 H 0.1880 0.4209 0.7137 0.044 Uiso 1 1 calc R C30 C 0.47329(9) 0.40525(18) 0.55925(9) 0.0361(4) Uani 1 1 d . H30 H 0.5047 0.3588 0.5584 0.043 Uiso 1 1 calc R C19 C 0.52571(9) 0.4780(2) 0.78729(8) 0.0414(5) Uani 1 1 d . C34 C 0.18426(13) 0.5842(2) 0.58996(11) 0.0513(6) Uani 1 1 d . C23 C 0.53868(11) 0.4168(2) 0.69624(9) 0.0443(5) Uani 1 1 d . H23 H 0.5444 0.3592 0.6710 0.053 Uiso 1 1 calc R C24 C 0.53604(12) 0.3918(2) 0.75114(10) 0.0488(6) Uani 1 1 d . H24 H 0.5412 0.3177 0.7633 0.059 Uiso 1 1 calc R C21 C 0.52381(14) 0.6137(2) 0.71641(10) 0.0550(7) Uani 1 1 d . H21 H 0.5205 0.6885 0.7046 0.066 Uiso 1 1 calc R C20 C 0.51981(14) 0.5884(3) 0.77146(10) 0.0619(8) Uani 1 1 d . H20 H 0.5133 0.6455 0.7968 0.074 Uiso 1 1 calc R C31 C 0.1714(2) 0.8409(3) 0.75388(16) 0.0959(15) Uani 1 1 d . H31A H 0.1983 0.8782 0.7312 0.144 Uiso 1 1 calc GR H31B H 0.1754 0.8671 0.7906 0.144 Uiso 1 1 calc GR H31C H 0.1345 0.8581 0.7411 0.144 Uiso 1 1 calc GR C32 C 0.1802(2) 0.7191(4) 0.75194(15) 0.0868(11) Uani 1 1 d . C33 C 0.12499(15) 0.5764(4) 0.59901(18) 0.0889(13) Uani 1 1 d . H33A H 0.1065 0.5616 0.5652 0.133 Uiso 1 1 calc GR H33B H 0.1116 0.6468 0.6139 0.133 Uiso 1 1 calc GR H33C H 0.1174 0.5156 0.6240 0.133 Uiso 1 1 calc GR N10 N 0.1873(3) 0.6271(3) 0.7519(2) 0.150(2) 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 S1 0.0250(2) 0.0342(2) 0.0328(2) 0.00072(18) 0.00487(17) -0.00453(18) O3 0.0244(7) 0.0528(9) 0.0252(6) 0.0012(6) -0.0012(5) -0.0051(6) O7 0.0313(7) 0.0410(8) 0.0290(6) 0.0019(5) -0.0034(6) -0.0102(6) O1 0.0327(7) 0.0565(9) 0.0234(6) -0.0027(6) 0.0013(5) -0.0122(7) O2 0.0391(8) 0.0534(9) 0.0212(6) 0.0017(6) -0.0013(6) -0.0194(7) O5 0.0462(9) 0.0370(8) 0.0472(8) 0.0078(7) -0.0013(7) -0.0153(7) O6 0.0258(7) 0.0617(10) 0.0404(7) -0.0035(7) 0.0086(6) 0.0034(7) N5 0.0288(8) 0.0347(8) 0.0202(6) -0.0003(6) -0.0029(6) -0.0055(7) N9 0.0255(8) 0.0333(8) 0.0294(7) 0.0061(6) -0.0026(6) -0.0016(7) N3 0.0327(8) 0.0351(8) 0.0219(6) 0.0017(6) -0.0016(6) -0.0054(7) N4 0.0332(8) 0.0337(8) 0.0220(6) 0.0019(6) -0.0020(6) -0.0068(7) O4 0.0242(7) 0.1147(17) 0.0352(7) 0.0137(9) -0.0003(6) -0.0072(9) N8 0.0274(8) 0.0331(8) 0.0305(7) 0.0060(6) -0.0010(6) -0.0028(7) N2 0.0352(9) 0.0395(9) 0.0228(6) 0.0034(6) -0.0037(7) -0.0089(7) N6 0.0259(8) 0.0406(9) 0.0286(7) -0.0028(7) -0.0028(6) -0.0025(7) N1 0.0340(8) 0.0384(9) 0.0239(7) 0.0012(6) -0.0027(6) -0.0060(7) N7 0.0266(8) 0.0469(10) 0.0315(8) 0.0000(7) -0.0028(7) -0.0055(8) C17 0.0253(9) 0.0267(8) 0.0289(8) -0.0007(7) -0.0013(7) 0.0013(7) C6 0.0289(9) 0.0347(9) 0.0206(7) 0.0006(7) -0.0002(7) -0.0053(8) C9 0.0311(9) 0.0289(9) 0.0240(8) 0.0008(7) -0.0007(7) -0.0036(8) C28 0.0298(10) 0.0413(10) 0.0229(7) 0.0001(7) 0.0027(7) -0.0063(8) C12 0.0269(9) 0.0314(9) 0.0298(8) -0.0026(7) -0.0019(7) 0.0034(8) C2 0.0347(10) 0.0309(9) 0.0205(7) 0.0008(7) -0.0009(7) -0.0074(8) C1 0.0323(10) 0.0287(9) 0.0232(8) -0.0005(7) 0.0000(7) -0.0048(8) C22 0.0233(9) 0.0335(9) 0.0330(8) -0.0013(7) 0.0032(7) -0.0017(8) C13 0.0308(10) 0.0309(9) 0.0272(8) -0.0047(7) -0.0014(7) -0.0019(8) C11 0.0261(9) 0.0321(9) 0.0209(7) 0.0013(6) -0.0016(7) -0.0032(8) C15 0.0283(9) 0.0349(10) 0.0276(8) 0.0031(7) 0.0035(7) 0.0044(8) C16 0.0330(10) 0.0284(8) 0.0258(7) -0.0023(7) 0.0018(7) -0.0004(8) C25 0.0256(9) 0.0298(9) 0.0286(8) -0.0009(7) 0.0039(7) -0.0018(8) C14 0.0249(9) 0.0383(10) 0.0216(7) 0.0031(7) -0.0004(7) -0.0038(8) C3 0.0360(10) 0.0407(10) 0.0200(7) 0.0010(7) -0.0002(7) -0.0106(9) N11 0.0619(15) 0.0452(12) 0.0684(14) -0.0071(11) 0.0104(12) -0.0023(11) C18 0.0246(9) 0.0408(10) 0.0306(8) 0.0013(8) -0.0002(7) -0.0043(8) C27 0.0275(10) 0.0391(11) 0.0385(9) -0.0041(8) 0.0025(8) 0.0046(8) C5 0.0430(11) 0.0331(10) 0.0257(8) -0.0021(7) -0.0002(8) -0.0123(9) C26 0.0325(10) 0.0291(9) 0.0379(9) -0.0058(8) 0.0017(8) 0.0028(8) C10 0.0372(11) 0.0452(11) 0.0228(8) 0.0022(8) -0.0001(8) -0.0062(9) C8 0.0433(12) 0.0366(10) 0.0257(8) -0.0054(8) 0.0010(8) -0.0131(9) C7 0.0442(12) 0.0310(10) 0.0264(8) 0.0005(7) 0.0016(8) -0.0099(9) C29 0.0427(12) 0.0298(9) 0.0361(9) -0.0078(8) 0.0010(9) -0.0022(9) C4 0.0479(12) 0.0335(10) 0.0281(9) 0.0035(8) 0.0004(8) -0.0134(9) C30 0.0340(10) 0.0338(10) 0.0405(10) -0.0055(8) 0.0006(8) 0.0065(9) C19 0.0235(9) 0.0685(15) 0.0323(9) 0.0055(10) 0.0010(8) -0.0058(10) C34 0.0603(17) 0.0380(12) 0.0558(13) 0.0067(10) 0.0148(13) -0.0020(12) C23 0.0567(14) 0.0353(11) 0.0411(11) -0.0010(9) 0.0010(10) -0.0040(11) C24 0.0541(15) 0.0462(13) 0.0462(12) 0.0098(10) -0.0019(11) -0.0095(12) C21 0.080(2) 0.0412(13) 0.0435(12) -0.0028(10) 0.0050(12) 0.0191(13) C20 0.083(2) 0.0654(17) 0.0376(11) -0.0107(12) 0.0062(13) 0.0255(16) C31 0.122(3) 0.080(2) 0.086(2) 0.015(2) 0.061(2) 0.041(2) C32 0.112(3) 0.080(3) 0.0685(19) -0.0075(18) 0.012(2) -0.017(2) C33 0.060(2) 0.102(3) 0.104(3) 0.043(2) 0.029(2) 0.000(2) N10 0.248(7) 0.052(2) 0.149(4) -0.017(2) 0.000(4) -0.034(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' 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' S S 0.3331 0.5567 '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 O5 S1 C22 107.75(10) O5 S1 C25 108.47(10) O6 S1 O5 119.51(10) O6 S1 C22 107.92(9) O6 S1 C25 107.97(9) C25 S1 C22 104.16(9) C17 O3 C14 117.42(14) C1 O1 C28 117.65(14) C2 O2 C3 120.77(15) C6 N5 C11 114.31(15) C9 N5 C6 121.65(15) C9 N5 C11 124.00(14) C17 N9 N8 116.48(16) N4 N3 C1 116.35(15) N3 N4 C2 116.61(16) C18 O4 C19 119.19(16) C18 N8 N9 116.20(15) C2 N2 N1 116.37(15) N7 N6 C17 116.50(15) C1 N1 N2 116.42(17) N6 N7 C18 116.07(16) O3 C17 N6 112.80(15) N9 C17 O3 120.08(17) N9 C17 N6 127.08(18) C5 C6 N5 118.67(17) C7 C6 N5 121.18(17) C7 C6 C5 120.11(17) O7 C9 N5 121.68(16) O7 C9 C10 121.28(17) N5 C9 C10 117.04(16) C27 C28 O1 118.97(19) C27 C28 C29 123.07(19) C29 C28 O1 117.84(18) C13 C12 H12 120.2 C11 C12 H12 120.2 C11 C12 C13 119.53(18) O2 C2 N4 111.40(17) N2 C2 O2 121.49(15) N2 C2 N4 127.10(18) N3 C1 O1 112.52(15) N1 C1 O1 120.36(17) N1 C1 N3 127.12(18) C23 C22 S1 118.71(16) C21 C22 S1 120.24(18) C21 C22 C23 121.0(2) C12 C13 H13 120.9 C14 C13 C12 118.21(18) C14 C13 H13 120.9 C12 C11 N5 120.42(17) C12 C11 C16 120.92(17) C16 C11 N5 118.54(16) C16 C15 H15 121.0 C14 C15 H15 121.0 C14 C15 C16 117.93(18) C11 C16 C15 120.15(17) C11 C16 H16 119.9 C15 C16 H16 119.9 C26 C25 S1 119.00(15) C30 C25 S1 119.01(16) C30 C25 C26 121.95(19) C13 C14 O3 117.32(17) C13 C14 C15 123.24(18) C15 C14 O3 119.37(18) C8 C3 O2 116.06(18) C8 C3 C4 122.14(17) C4 C3 O2 121.55(18) O4 C18 N7 112.67(17) N8 C18 O4 119.88(17) N8 C18 N7 127.44(18) C28 C27 H27 120.6 C28 C27 C26 118.85(19) C26 C27 H27 120.6 C6 C5 H5 119.8 C6 C5 C4 120.48(18) C4 C5 H5 119.8 C25 C26 C27 118.66(18) C25 C26 H26 120.7 C27 C26 H26 120.7 C9 C10 H10A 109.5 C9 C10 H10B 109.5 C9 C10 H10C 109.5 H10A C10 H10B 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 C3 C8 H8 120.5 C3 C8 C7 119.01(19) C7 C8 H8 120.5 C6 C7 C8 119.78(19) C6 C7 H7 120.1 C8 C7 H7 120.1 C28 C29 H29 120.9 C28 C29 C30 118.11(19) C30 C29 H29 120.9 C3 C4 C5 118.45(19) C3 C4 H4 120.8 C5 C4 H4 120.8 C25 C30 C29 119.34(19) C25 C30 H30 120.3 C29 C30 H30 120.3 C24 C19 O4 118.1(2) C20 C19 O4 118.9(2) C20 C19 C24 122.5(2) N11 C34 C33 178.9(4) C22 C23 H23 120.4 C22 C23 C24 119.2(2) C24 C23 H23 120.4 C19 C24 C23 119.1(2) C19 C24 H24 120.5 C23 C24 H24 120.5 C22 C21 H21 120.0 C22 C21 C20 119.9(2) C20 C21 H21 120.0 C19 C20 C21 118.3(2) C19 C20 H20 120.8 C21 C20 H20 120.8 H31A C31 H31B 109.5 H31A C31 H31C 109.5 H31B C31 H31C 109.5 C32 C31 H31A 109.5 C32 C31 H31B 109.5 C32 C31 H31C 109.5 N10 C32 C31 178.1(5) C34 C33 H33A 109.5 C34 C33 H33B 109.5 C34 C33 H33C 109.5 H33A C33 H33B 109.5 H33A C33 H33C 109.5 H33B C33 H33C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 O5 1.4376(16) S1 O6 1.4371(16) S1 C22 1.7682(19) S1 C25 1.7666(19) O3 C17 1.342(2) O3 C14 1.418(2) O7 C9 1.228(2) O1 C28 1.407(2) O1 C1 1.345(2) O2 C2 1.344(2) O2 C3 1.407(2) N5 C6 1.442(2) N5 C9 1.366(2) N5 C11 1.447(2) N9 N8 1.336(2) N9 C17 1.319(2) N3 N4 1.312(2) N3 C1 1.344(3) N4 C2 1.345(2) O4 C18 1.342(2) O4 C19 1.402(3) N8 C18 1.315(3) N2 N1 1.335(2) N2 C2 1.321(3) N6 N7 1.313(2) N6 C17 1.344(2) N1 C1 1.324(2) N7 C18 1.348(3) C6 C5 1.385(3) C6 C7 1.384(3) C9 C10 1.506(2) C28 C27 1.372(3) C28 C29 1.381(3) C12 H12 0.9300 C12 C13 1.397(3) C12 C11 1.384(3) C22 C23 1.378(3) C22 C21 1.373(3) C13 H13 0.9300 C13 C14 1.374(3) C11 C16 1.385(3) C15 H15 0.9300 C15 C16 1.386(3) C15 C14 1.381(3) C16 H16 0.9300 C25 C26 1.387(3) C25 C30 1.382(3) C3 C8 1.376(3) C3 C4 1.377(3) N11 C34 1.125(4) C27 H27 0.9300 C27 C26 1.389(3) C5 H5 0.9300 C5 C4 1.390(3) C26 H26 0.9300 C10 H10A 0.9600 C10 H10B 0.9600 C10 H10C 0.9600 C8 H8 0.9300 C8 C7 1.394(3) C7 H7 0.9300 C29 H29 0.9300 C29 C30 1.388(3) C4 H4 0.9300 C30 H30 0.9300 C19 C24 1.371(4) C19 C20 1.363(4) C34 C33 1.442(4) C23 H23 0.9300 C23 C24 1.384(3) C24 H24 0.9300 C21 H21 0.9300 C21 C20 1.391(4) C20 H20 0.9300 C31 H31A 0.9600 C31 H31B 0.9600 C31 H31C 0.9600 C31 C32 1.448(5) C32 N10 1.095(6) C33 H33A 0.9600 C33 H33B 0.9600 C33 H33C 0.9600 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 0 -2 478.15 7.55 0 0 -3 0.69 0.6 0 0 -4 2008.11 25.73 0 0 -5 -1.37 1.2 0 0 -6 9999 105.04 0 0 -7 -0.3 1.34 0 0 -8 9.88 2.21 0 0 8 12.13 1.38 0 0 9 0.72 0.71 0 0 -9 0.61 1.38 0 0 -10 19.99 2.96 0 0 10 17.63 1.92 0 0 -11 -0.88 1.61 0 0 11 0.44 0.86 0 0 -12 862.93 22.23 0 0 12 906.48 16.89 0 0 13 0.75 0.81 0 0 14 40.33 3.53 0 0 15 0.21 0.86 0 0 16 13.36 2.28 0 0 17 -0.75 0.97 0 0 18 7.77 2.16 0 0 19 0.02 1.44 0 0 19 0.5 0.56 0 0 19 -0.3 0.78 0 0 20 9.08 1.12 0 0 20 7.74 1.3 0 0 21 -0.4 0.54 0 0 22 5.94 0.99 0 0 23 0.89 0.66 0 0 24 15.82 1.47 0 0 25 -0.49 0.56 0 0 26 9.34 1.1 0 0 27 0.13 0.44 0 0 28 25.31 1.43 0 0 29 -0.15 0.36 0 0 30 3.97 0.47 1 0 -2 85.87 2.6 -1 0 2 88.12 2.03 -1 0 -2 86.5 2.75 -1 0 -3 0.11 0.56 -1 0 3 0.07 0.26 1 0 -3 0.23 0.67 -1 0 4 14.45 1.1 1 0 -4 15.09 1.63 -1 0 -4 15.44 1.69 -1 0 5 1.58 0.76 1 0 -5 -0.05 1.17 -1 0 -5 -0.18 1.35 -1 0 -6 139.35 6.06 -1 0 6 129.77 3.95 1 0 -6 130.79 5.72 -1 0 -7 0.71 1.36 1 0 -7 -1.05 1.24 -1 0 7 -0.13 0.48 1 0 -8 226.52 8.68 -1 0 -8 230.59 8.85 -1 0 8 205.7 5.88 1 0 -9 1.07 1.16 -1 0 9 0.17 0.59 -1 0 -9 -0.14 1.4 -1 0 10 16.19 1.88 1 0 -10 17 3.04 -1 0 -10 17.3 3.11 1 0 -11 0.77 1.34 1 0 11 0.12 0.69 -1 0 -11 1.08 2.24 -1 0 11 0.94 1.06 -1 0 12 29.37 2.72 -1 0 -12 28.15 4.07 1 0 12 33.7 2.9 -1 0 -13 1.48 1.52 -1 0 13 -0.84 0.88 1 0 13 0.4 0.89 -1 0 14 91.12 5.34 1 0 14 92.83 5.38 -1 0 15 -0.18 0.81 1 0 15 0.31 0.75 -1 0 16 100.03 6.18 1 0 16 101.97 6.23 -1 0 16 90.26 6.9 -1 0 17 -0.58 1.13 1 0 17 0.45 1.25 1 0 18 -0.06 1.02 -1 0 18 -1.34 1.26 -1 0 19 1.23 0.79 1 0 19 -0.2 0.51 -1 0 19 0.41 0.5 1 0 19 0.01 1.07 1 0 19 -0.56 0.75 1 0 20 0.5 1.23 -1 0 20 0.76 0.62 -1 0 20 -0.28 0.65 1 0 20 0.21 0.51 1 0 21 0.48 0.6 -1 0 21 0.98 0.84 1 0 22 18.86 1.64 -1 0 22 17.41 1.53 1 0 23 -0.54 0.61 -1 0 23 -0.42 0.6 -1 0 24 2.46 0.73 1 0 24 2.53 0.76 1 0 25 0.73 0.62 -1 0 25 0.02 0.48 -1 0 26 5.98 0.92 1 0 26 6.91 1.01 1 0 27 -0.1 0.5 -1 0 27 0.49 0.5 -1 0 28 7.9 0.85 1 0 28 8.09 0.92 1 0 29 -0.01 0.36 -1 0 29 0.11 0.32 -1 0 30 1.53 0.32 1 0 30 1.28 0.34 -2 0 0 14.3 0.58 2 0 1 0.15 0.2 -2 0 -1 0.06 0.13 -2 0 -1 0.01 0.2 -2 0 -2 473.25 7.58 2 0 2 476.97 6.59 -2 0 -3 -0.79 0.73 -2 0 4 315.4 5.89 2 0 -4 321.12 7.39 -2 0 -4 303.14 7.69 -2 0 -5 -0.74 1.67 2 0 -5 -0.37 1.15 -2 0 5 0.24 0.63 -2 0 6 123.58 3.98 2 0 -6 122.8 5.4 -2 0 -6 122.87 5.69 2 0 -7 0.78 1.11 -2 0 7 -0.22 0.6 -2 0 -7 0.19 1.5 2 0 -8 65.89 4.6 -2 0 -8 73.75 5.02 -2 0 8 64.93 3.26 2 0 -9 2.33 1.31 -2 0 -9 0.95 1.6 -2 0 9 1.58 0.94 -2 0 -10 55.23 4.98 -2 0 10 49.06 3.25 -2 0 -11 -0.79 2.26 -2 0 11 -0.49 0.99 -2 0 12 15.46 2.04 -2 0 -12 14.71 3.46 -2 0 13 0.86 0.85 -2 0 -13 -0.11 1.6 2 0 13 -0.61 0.91 -2 0 -14 1.63 1.85 2 0 14 -0.03 0.72 -2 0 14 -0.13 1.06 2 0 15 1.19 0.96 -2 0 15 -0.32 1.07 -2 0 16 17.29 2.63 2 0 16 21.28 2.91 2 0 17 -1.6 1.41 -2 0 17 1.99 1.39 2 0 18 27.45 3.56 2 0 19 -0.02 0.55 -2 0 19 -0.11 0.52 2 0 19 1.05 0.83 2 0 19 -0.45 1.23 -2 0 20 2.82 0.85 2 0 20 0.8 0.85 -2 0 20 1.08 0.81 2 0 20 1.98 0.75 2 0 21 0.02 0.57 -2 0 21 1.21 0.97 -2 0 21 0.29 0.62 -2 0 22 1.58 0.76 2 0 22 1.93 0.75 -2 0 23 0.33 0.53 2 0 23 0.96 0.72 -2 0 24 57.49 2.62 2 0 24 60.83 2.81 2 0 25 -0.63 0.71 -2 0 25 0.35 0.6 2 0 26 38.17 2.1 -2 0 26 40.89 2.03 2 0 27 0.35 0.49 -2 0 27 -0.3 0.39 -2 0 28 2.89 0.57 2 0 28 3.54 0.64 -2 0 29 -0.16 0.31 2 0 29 -0.28 0.38 2 0 30 3.07 0.47 -3 0 0 0.14 0.19 -3 0 -1 -0.01 0.3 -3 0 -1 -0.02 0.28 3 0 2 2716.51 28.97 -3 0 -2 2774.55 29.81 -3 0 -3 -0.67 0.81 3 0 3 -0.43 0.46 -3 0 -4 8.49 1.54 -3 0 -5 0.1 1.2 -3 0 -6 647.38 14.08 -3 0 -7 0.76 1.29 -3 0 7 -0.35 0.68 -3 0 8 12.03 1.56 -3 0 -8 12.75 2.32 -3 0 9 -0.27 0.71 -3 0 -9 0.07 1.49 -3 0 10 438.23 10.52 -3 0 -10 474.52 14.88 -3 0 -11 -1.42 1.97 -3 0 11 -0.06 0.88 -3 0 -12 231.59 11.17 -3 0 12 231.56 8.19 -3 0 -13 -1.92 2.25 -3 0 13 -0.37 1 -3 0 -14 56.82 6.2 3 0 14 56.67 4.11 3 0 15 0.41 0.84 -3 0 -15 0.32 1.8 3 0 16 17.36 2.68 3 0 17 -0.16 1.03 -3 0 17 -0.74 1.37 3 0 18 0.31 0.94 -3 0 18 2.75 1.79 3 0 19 -0.4 0.55 -3 0 19 0.07 0.52 3 0 19 -0.06 0.9 -3 0 19 -1.59 0.79 3 0 20 2.13 1.41 -3 0 20 3.69 0.81 3 0 20 3.86 0.83 -3 0 20 3.56 1.09 -3 0 21 -0.47 0.88 3 0 21 0.44 0.66 -3 0 21 -0.61 0.61 3 0 22 -0.9 0.7 -3 0 22 -0.16 0.53 -3 0 23 -0.06 0.54 3 0 23 0.29 0.62 3 0 24 -0.12 0.59 -3 0 24 -0.65 0.54 3 0 25 1.18 0.69 -3 0 25 -0.33 0.49 -3 0 26 7.49 0.92 3 0 26 6.36 0.95 3 0 27 -0.49 0.47 -3 0 27 0.1 0.4 -3 0 28 -0.55 0.4 3 0 28 -0.63 0.51 3 0 29 0.3 0.38 3 0 30 0.92 0.33 -4 0 0 346.81 5.09 -4 0 -1 -0.38 0.47 -4 0 1 -0.07 0.28 -4 0 -1 0.33 0.51 4 0 2 0.64 0.53 -4 0 -2 2.03 0.72 -4 0 -2 1.88 0.41 -4 0 -3 -0.35 0.86 4 0 3 1.08 0.74 4 0 4 725.07 10.9 -4 0 -4 695.02 12.79 -4 0 -5 0.41 1.12 -4 0 -6 152.04 6.47 -4 0 -7 0.56 1.16 -4 0 -8 0.12 1.34 -4 0 -9 0.8 1.23 -4 0 -10 36.12 4.06 -4 0 -11 -0.61 1.87 -4 0 -12 174.92 9.9 -4 0 -13 8.14 2.92 -4 0 -14 0.93 1.93 4 0 15 -0.62 1.08 -4 0 -15 -3.23 2.62 -4 0 16 16.61 3.32 4 0 16 13.96 2.41 -4 0 17 -0.31 1.92 4 0 17 0.88 1.19 4 0 18 65.72 5.45 -4 0 18 92.23 7.93 -4 0 19 -0.95 0.6 4 0 19 -0.4 0.57 -4 0 19 -0.39 0.7 4 0 19 -1.56 1.82 -4 0 20 1.76 1.09 4 0 20 -0.3 0.62 -4 0 20 0.29 0.53 4 0 20 -0.67 1.03 -4 0 21 0.11 0.49 -4 0 21 -0.45 0.76 4 0 21 0.9 0.71 4 0 22 102.65 3.83 -4 0 22 103.83 3.51 -4 0 22 102.19 4.41 -4 0 23 0.26 0.46 4 0 23 1.04 0.79 4 0 24 17.82 1.58 -4 0 24 17.21 1.4 -4 0 25 0.16 0.47 4 0 25 0.35 0.66 4 0 26 0.65 0.61 -4 0 26 1.86 0.54 -4 0 27 -0.26 0.37 4 0 27 0.84 0.58 4 0 28 4.2 0.68 4 0 29 0.04 0.38 4 0 30 6.47 0.62 -5 0 0 -0.1 0.38 -5 0 1 0.34 0.46 -5 0 -1 -0.13 0.62 -5 0 -1 0.61 0.53 5 0 2 1025.74 14.38 -5 0 -2 1042.62 14.24 -5 0 -2 1044.77 12.45 -5 0 -3 -0.39 0.78 5 0 3 -0.84 0.68 -5 0 -4 0.05 1.02 5 0 4 -0.58 0.61 -5 0 -5 1.49 1.17 -5 0 -6 579.9 13.61 -5 0 -7 -0.01 1.25 -5 0 -8 174.58 8.08 -5 0 -9 0.74 1.47 -5 0 -10 33.66 4.13 -5 0 -11 0.04 1.69 -5 0 -12 253.91 12.08 -5 0 -13 -4.94 2.7 -5 0 -14 52.3 5.89 -5 0 -15 1.46 1.85 -5 0 -16 106.66 9.15 -5 0 16 94.1 8.28 5 0 16 89.78 5.86 5 0 17 -1.52 1.26 -5 0 17 0.79 1.7 -5 0 18 -0.23 0.68 5 0 18 0.86 1.02 5 0 18 0.9 0.59 -5 0 18 -0.8 1.53 -5 0 19 -0.26 0.86 -5 0 19 -2.37 2.2 5 0 19 -0.74 1.06 -5 0 19 -0.01 0.47 5 0 19 -0.74 0.7 5 0 20 120.24 7.98 -5 0 20 119.57 3.76 5 0 20 116.28 4.08 -5 0 20 116.18 4.6 -5 0 21 -0.16 0.56 -5 0 21 0.47 0.77 5 0 21 -0.25 0.6 -5 0 22 106.48 4.45 5 0 22 109.15 4.01 -5 0 22 114.36 3.63 -5 0 23 0.35 0.49 5 0 23 0.08 0.66 -5 0 24 0.71 0.53 5 0 24 0.43 0.65 5 0 25 0.02 0.66 -5 0 25 0.88 0.54 5 0 26 4.95 0.85 5 0 27 -0.75 0.58 5 0 28 3.1 0.68 5 0 29 0.75 0.44 5 0 30 4.94 0.55 -6 0 0 1651.53 22.09 -6 0 0 1651.04 18.8 -6 0 1 -0.2 0.41 -6 0 -1 -0.81 0.68 -6 0 -1 0.58 0.53 -6 0 2 3259.31 33.59 -6 0 -2 3237.9 34.19 -6 0 -2 3232.53 35.93 -6 0 -3 0.52 0.89 6 0 3 0.02 0.67 -6 0 -4 1488.9 22.08 6 0 4 1534.39 20.3 6 0 5 0.04 0.62 -6 0 -5 1 1.25 -6 0 -6 50.98 3.82 -6 0 -7 -0.8 1.19 -6 0 -8 7.41 2.01 -6 0 -9 -0.62 1.39 -6 0 -10 14.69 2.89 -6 0 -11 -0.85 1.61 -6 0 -12 -0.66 1.82 -6 0 -13 0.84 1.8 -6 0 -14 139.85 9.87 -6 0 -15 0.21 2.02 -6 0 16 3.48 2.3 -6 0 -16 -0.74 2.41 -6 0 17 -0.43 1.91 6 0 17 1.39 1.11 6 0 18 3.09 1.68 -6 0 18 2.72 2.2 6 0 18 2.26 0.7 -6 0 18 2.32 0.93 6 0 19 -1.09 1.45 6 0 19 0.76 0.7 -6 0 19 2.36 1.77 -6 0 19 -1.07 0.92 6 0 20 4.64 0.96 6 0 20 3.52 1.89 -6 0 20 3.26 1.05 6 0 21 0.2 0.62 -6 0 21 -1.56 1.07 6 0 22 0.3 0.6 -6 0 22 0.83 0.79 6 0 23 -0.18 0.7 6 0 24 27.65 1.94 6 0 25 0.5 0.72 6 0 26 9.77 1.13 6 0 27 -0.24 0.51 6 0 28 0.55 0.47 6 0 29 -0.49 0.35 -6 0 29 0.1 0.4 6 0 30 0.23 0.28 -7 0 0 -0.04 0.88 -7 0 0 -0.08 0.39 -7 0 -1 -0.39 0.61 -7 0 1 -0.47 0.36 -7 0 -1 0.21 0.63 -7 0 -2 115.56 4.08 -7 0 -2 123.63 3.63 -7 0 2 122.97 3.24 -7 0 -3 0.42 0.72 7 0 3 0.38 0.57 -7 0 -4 27.08 2.43 7 0 4 22.57 2 -7 0 -5 0.96 1.12 7 0 5 1.02 0.68 -7 0 -6 52.12 3.99 -7 0 -7 0.38 1.32 -7 0 -8 19.35 2.95 -7 0 -9 -1.81 1.79 -7 0 -10 1.75 1.61 -7 0 -11 -2.03 2.17 -7 0 -12 257.97 12.53 -7 0 -13 0.73 1.75 -7 0 -14 96.67 8.17 -7 0 15 -0.82 2 -7 0 -15 -0.98 2.12 -7 0 16 25.94 4.85 -7 0 -16 26.11 4.75 -7 0 17 1.14 1.84 7 0 18 9.92 2.45 -7 0 18 8.13 1.32 7 0 18 8.43 1.21 -7 0 18 8.37 3.06 7 0 19 0.45 1.14 -7 0 19 -0.06 2.17 7 0 19 0.11 0.67 -7 0 19 -0.29 0.75 -7 0 20 14.32 1.73 7 0 20 15.68 1.58 7 0 21 -0.42 0.64 -7 0 21 0.47 0.83 7 0 22 2.85 0.87 -7 0 22 4.71 1.21 7 0 23 1.13 0.76 7 0 24 -0.22 0.66 7 0 25 -0.23 0.62 7 0 26 23.7 1.62 7 0 27 0.5 0.48 7 0 28 5.59 0.76 -7 0 29 0.54 0.42 7 0 29 -0.35 0.41 -8 0 0 385.95 9.45 -8 0 1 0.37 0.46 -8 0 -1 -0.35 0.63 -8 0 -1 -0.05 0.47 -8 0 1 0.21 0.97 -8 0 -2 84.89 3.65 -8 0 -2 88.6 3.29 -8 0 2 88.94 2.87 -8 0 -3 0.02 0.7 -8 0 3 -0.02 0.35 8 0 3 0.12 0.63 -8 0 -4 23.17 2.38 8 0 4 24.14 2.14 8 0 5 0.42 0.85 -8 0 -5 1.05 1.08 8 0 6 163.43 5.97 -8 0 -6 158.44 7.19 -8 0 -7 -0.12 1.31 -8 0 -8 99.44 6.47 -8 0 -9 0.06 1.37 -8 0 -10 85.42 6.69 -8 0 -11 0.06 1.54 -8 0 -12 249.42 12.39 -8 0 -13 -1.29 2.06 -8 0 -14 49.23 5.93 -8 0 14 53.78 6.49 -8 0 -15 -0.42 1.85 -8 0 15 -0.91 2.18 -8 0 16 -0.87 1.65 -8 0 -16 -0.55 2.08 -8 0 17 -0.62 0.7 8 0 17 -0.04 0.65 -8 0 17 -1.61 2.11 8 0 18 0.84 1.28 -8 0 18 3.84 1.9 -8 0 18 1.49 0.98 8 0 18 0.18 0.59 8 0 19 -0.57 0.66 -8 0 19 -1.48 0.81 8 0 19 -0.17 0.95 -8 0 19 -1.58 2.26 -8 0 20 55.56 3.19 8 0 20 53.66 2.77 -8 0 21 0.49 0.73 8 0 21 -0.69 0.68 8 0 22 26.32 2.02 -8 0 22 26.43 2.19 8 0 23 -0.2 0.65 8 0 24 11.89 1.33 8 0 25 0.44 0.69 8 0 26 3.7 0.81 8 0 27 -0.33 0.48 8 0 28 5.69 0.76 8 0 29 -0.1 0.32 -8 0 29 -0.11 0.36 -9 0 0 0.49 0.74 -9 0 1 0.1 1.21 -9 0 -1 -0.47 0.52 -9 0 -1 -0.05 0.64 -9 0 1 -0.75 0.55 -9 0 -2 17.19 1.54 -9 0 2 19.53 2.5 -9 0 2 16.71 1.27 -9 0 -2 16.74 1.74 -9 0 -3 -0.33 0.67 -9 0 3 -0.57 0.48 9 0 3 0.14 0.72 -9 0 -4 13.72 2.02 9 0 4 12.54 1.8 -9 0 4 13.35 1.23 9 0 5 -0.53 0.86 -9 0 -5 0.28 1.05 -9 0 -6 1.64 1.29 9 0 6 2.99 1.22 -9 0 -7 -0.34 1.36 -9 0 -8 1.3 1.4 -9 0 -9 1.63 1.6 -9 0 -10 287.26 12.43 -9 0 -11 2.14 2.03 -9 0 -12 510.31 18.34 -9 0 13 1.92 2.19 -9 0 -13 2.08 1.95 -9 0 14 338.83 16.71 -9 0 -14 351.86 16.26 -9 0 -15 0.78 1.83 -9 0 15 2.32 2.34 -9 0 16 326.89 16.93 -9 0 -16 343.39 17.01 9 0 17 0.77 0.63 -9 0 17 0.72 0.76 -9 0 17 -1.5 2.37 -9 0 18 11.21 1.57 -9 0 18 7.25 2.89 9 0 18 11.44 1.36 9 0 19 0.37 0.71 -9 0 19 -0.55 0.82 -9 0 19 0.87 2.21 9 0 20 24.32 1.91 -9 0 20 25.38 2.17 9 0 21 -0.25 0.65 -9 0 21 0.36 0.79 9 0 22 9.55 1.31 9 0 23 0.36 0.66 9 0 24 1.76 0.75 9 0 25 -0.34 0.63 9 0 26 6.18 0.92 9 0 27 -0.08 0.46 -9 0 28 15.68 1.29 9 0 28 14.59 1.06 -9 0 29 -0.2 0.37 -10 0 0 465.6 11.21 -10 0 0 464.61 8.72 -10 0 1 -0.74 0.94 -10 0 -1 0.03 0.69 -10 0 -1 0.19 0.54 10 0 2 470.12 11.46 -10 0 -2 467.51 10.17 -10 0 2 469.06 13.05 -10 0 2 475.69 8.27 -10 0 -2 453.67 9.29 -10 0 3 -0.39 1.4 -10 0 -3 -0.49 0.73 10 0 3 0.52 0.87 -10 0 3 -0.33 0.46 -10 0 4 -0.72 1.33 -10 0 4 1.29 0.56 10 0 4 0.85 0.91 -10 0 -4 2 1.03 10 0 5 0.37 0.88 -10 0 5 0.97 0.56 -10 0 -5 0.48 0.99 -10 0 -6 1052.16 21.48 10 0 6 1100.97 19.42 -10 0 -7 0.11 1.27 -10 0 -8 289.8 11.59 -10 0 -9 1.14 1.35 -10 0 -10 35.95 4.58 -10 0 -11 -0.3 1.58 -10 0 12 482.07 19.61 -10 0 -12 515.64 18.53 -10 0 13 0.04 2.02 -10 0 -13 -0.47 1.87 -10 0 14 39.1 5.87 -10 0 -14 35.69 5.31 -10 0 -15 -0.72 1.62 -10 0 15 -0.8 1.86 -10 0 16 16.2 4.25 -10 0 16 12.65 1.48 10 0 16 12.99 1.37 -10 0 17 0.51 0.67 -10 0 17 -1.82 2.33 10 0 17 -0.9 0.67 -10 0 18 27.49 5.35 -10 0 18 22.23 2 10 0 18 21.19 1.74 10 0 19 0.1 0.68 -10 0 19 1.27 0.91 -10 0 20 5.31 1.15 10 0 20 4.12 0.93 10 0 21 0.68 0.8 -10 0 21 0.57 0.7 10 0 22 13.3 1.43 10 0 23 -0.34 0.65 10 0 24 0 0.64 10 0 25 -0.22 0.53 10 0 26 4.14 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