#------------------------------------------------------------------------------ #$Date: 2018-01-13 03:57:05 +0200 (Sat, 13 Jan 2018) $ #$Revision: 205140 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/11/7121138.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_7121138 loop_ _publ_author_name 'Koner, Abhishek' 'Kelemen, Zsolt' 'Schnakenburg, Gregor' 'Nyul\'aszi, L\'aszl\'o' 'Streubel, Rainer' _publ_section_title ; 1,4-Additions of tricyclic 1,4-diphosphinines -- a novel system to study \s-bond activation and \p--\p dispersion interactions ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C7CC09349G _journal_year 2018 _chemical_formula_moiety '4(C32 H43 N5 O2 P2 S2), C H2 Cl2' _chemical_formula_sum 'C129 H174 Cl2 N20 O8 P8 S8' _chemical_formula_weight 2708.01 _chemical_name_systematic ABK-445 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2017-03-30 _audit_creation_method ; Olex2 1.2 (compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292) ; _audit_update_record ; 2017-12-05 deposited with the CCDC. 2018-01-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 126.3663(11) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 27.7111(12) _cell_length_b 14.5378(7) _cell_length_c 21.9682(16) _cell_measurement_reflns_used 9990 _cell_measurement_temperature 100 _cell_measurement_theta_max 28.72 _cell_measurement_theta_min 2.30 _cell_volume 7126.5(7) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker X8-KappaApexII' _diffrn_measurement_method 'fine slicing \w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_unetI/netI 0.0439 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 48634 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.000 _diffrn_reflns_theta_min 3.166 _diffrn_source 'sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.313 _exptl_absorpt_correction_T_max 0.7459 _exptl_absorpt_correction_T_min 0.6894 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0850 before and 0.0586 after correction. The Ratio of minimum to maximum transmission is 0.9243. The \l/2 correction factor is 0.00150.' _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.262 _exptl_crystal_description block _exptl_crystal_F_000 2868 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _refine_diff_density_max 1.256 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.093 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 439 _refine_ls_number_reflns 8586 _refine_ls_number_restraints 64 _refine_ls_restrained_S_all 1.076 _refine_ls_R_factor_all 0.0981 _refine_ls_R_factor_gt 0.0729 _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^)+(0.1137P)^2^+17.3882P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2022 _refine_ls_wR_factor_ref 0.2277 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6399 _reflns_number_total 8586 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7cc09349g2.cif _cod_data_source_block 2b _cod_database_code 7121138 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C33-Cl1 = C33-Cl2 1.74 with sigma of 0.01 C17S-C18S 1.49 with sigma of 0.01 C18-C17 = C18S-C17S = C17-C16 = C17S-C16 1.5 with sigma of 0.01 3. Uiso/Uaniso restraints and constraints C18S \\sim C18 \\sim C17 \\sim C17S \\sim C16 \\sim C15: within 2A with sigma of 0.003 and sigma for terminal atoms of 0.006 4. Rigid body (RIGU) restrains C18S, C18, C33, Cl1, Cl2 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 5. Others Sof(H16C)=Sof(H16D)=Sof(C18S)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C17S)= Sof(H17C)=Sof(H17D)=1-FVAR(1) Sof(H16A)=Sof(H16B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)= Sof(H18C)=FVAR(1) Fixed Sof: Cl1(0.25) C33(0.25) H33A(0.25) H33B(0.25) Cl2(0.25) 6.a Ternary CH refined with riding coordinates: C23(H23), C26(H26) 6.b Secondary CH2 refined with riding coordinates: C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A, H10B), C15(H15A,H15B), C16(H16A,H16B), C16(H16C,H16D), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C33(H33A,H33B), C17S(H17C,H17D) 6.c Aromatic/amide H refined with riding coordinates: C28(H28), C29(H29), C30(H30), C31(H31), C32(H32) 6.d Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C22(H22A,H22B, H22C), C18S(H18D,H18E,H18F) ; _shelx_res_file ; 5078f.res created by SHELXL-2014/7 TITL 5078f in C2/c #15 REM reset to C2/c #15 CELL 0.71073 27.7111 14.5378 21.96825 90 126.3663 90 ZERR 2 0.0012 0.0007 0.00163 0 0.0011 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cl N O P S UNIT 258 348 4 40 16 16 16 DFIX 1.74 0.01 C33 Cl1 C33 Cl2 DFIX 1.49 0.01 C17S C18S DFIX 1.5 0.01 C18 C17 C18S C17S C17 C16 C17S C16 SIMU 0.003 0.006 2 C18S C18 C17 C17S C16 C15 RIGU 0.002 0.002 C18S C18 C33 Cl1 Cl2 L.S. 4 0 0 PLAN 20 TEMP -173.15 BOND fmap 2 53 ACTA OMIT -2 56 OMIT 2 0 2 OMIT -3 1 2 OMIT 1 1 0 OMIT 2 2 0 OMIT 4 2 0 OMIT -6 0 2 OMIT -4 4 1 OMIT 2 2 2 OMIT 2 2 4 OMIT 3 1 0 REM REM REM WGHT 0.113700 17.388199 FVAR 0.07157 0.56874 S1 7 0.831226 0.517281 0.701336 11.00000 0.05799 0.03978 = 0.04372 0.01164 0.03745 0.00298 S2 7 0.641315 0.343577 0.936994 11.00000 0.07606 0.05013 = 0.04811 0.00466 0.04983 0.00597 P1 6 0.716851 0.249817 0.759201 11.00000 0.04892 0.03257 = 0.02795 -0.00487 0.02662 -0.00652 P2 6 0.837927 0.325914 0.926308 11.00000 0.05229 0.03030 = 0.02421 -0.00053 0.02394 -0.00282 O1 5 0.770619 0.090587 0.714021 11.00000 0.05677 0.05991 = 0.05027 -0.02683 0.03764 -0.01810 O2 5 0.932055 0.248573 0.908759 11.00000 0.04753 0.06974 = 0.03831 -0.01394 0.02129 -0.00642 N1 4 0.764227 0.389284 0.712497 11.00000 0.04612 0.03308 = 0.02344 0.00225 0.02228 -0.00051 N2 4 0.841138 0.440266 0.821527 11.00000 0.04180 0.03016 = 0.02711 0.00181 0.02117 -0.00211 N3 4 0.666642 0.288676 0.840119 11.00000 0.05631 0.03278 = 0.03579 -0.00082 0.03368 -0.00321 N4 4 0.745201 0.341627 0.947694 11.00000 0.06325 0.03365 = 0.02920 0.00008 0.03342 -0.00070 N5 4 0.857169 0.170644 0.801709 11.00000 0.04658 0.03414 = 0.03144 -0.00280 0.02569 -0.00301 C1 1 0.763313 0.345480 0.767968 11.00000 0.04756 0.02928 = 0.02618 0.00115 0.02397 -0.00307 C2 1 0.811777 0.448817 0.745384 11.00000 0.04017 0.02982 = 0.03014 0.00395 0.02196 0.00505 C3 1 0.811179 0.377985 0.835728 11.00000 0.04919 0.02850 = 0.02801 0.00108 0.02559 -0.00290 C4 1 0.722022 0.372961 0.630706 11.00000 0.05997 0.04829 = 0.02529 -0.00015 0.02575 -0.00699 AFIX 23 H4A 2 0.712530 0.306497 0.621768 11.00000 -1.20000 H4B 2 0.741494 0.390164 0.606411 11.00000 -1.20000 AFIX 0 C5 1 0.664107 0.426828 0.593953 11.00000 0.07515 0.04541 = 0.03570 -0.00046 0.00212 0.00195 AFIX 23 H5A 2 0.644658 0.407742 0.617891 11.00000 -1.20000 H5B 2 0.674442 0.492770 0.605729 11.00000 -1.20000 AFIX 0 C6 1 0.619452 0.417590 0.510722 11.00000 0.07312 0.08767 = 0.05576 0.00360 0.02646 0.00671 AFIX 23 H6A 2 0.612944 0.351092 0.498738 11.00000 -1.20000 H6B 2 0.637711 0.442991 0.486904 11.00000 -1.20000 AFIX 0 C7 1 0.559609 0.461287 0.473518 11.00000 0.06392 0.11909 = 0.09102 0.01089 0.02178 0.01483 AFIX 137 H7A 2 0.529873 0.427460 0.427263 11.00000 -1.50000 H7B 2 0.561382 0.525199 0.460776 11.00000 -1.50000 H7C 2 0.548159 0.459978 0.508013 11.00000 -1.50000 AFIX 0 C8 1 0.895907 0.487986 0.879959 11.00000 0.03805 0.03709 = 0.03482 0.00013 0.02122 -0.00348 AFIX 23 H8A 2 0.914565 0.515028 0.857154 11.00000 -1.20000 H8B 2 0.924471 0.442985 0.918707 11.00000 -1.20000 AFIX 0 C9 1 0.884755 0.563334 0.917628 11.00000 0.04638 0.03926 = 0.04674 -0.00744 0.02436 -0.00302 AFIX 23 H9A 2 0.857085 0.540354 0.928709 11.00000 -1.20000 H9B 2 0.865249 0.616081 0.882547 11.00000 -1.20000 AFIX 0 C10 1 0.942664 0.595653 0.990779 11.00000 0.04850 0.08046 = 0.06382 -0.03223 0.02936 -0.01520 AFIX 23 H10A 2 0.964198 0.541492 1.023251 11.00000 -1.20000 H10B 2 0.968477 0.624169 0.978665 11.00000 -1.20000 AFIX 0 C11 1 0.933161 0.663652 1.034316 11.00000 0.07808 0.14428 = 0.11762 -0.09306 0.05203 -0.03523 AFIX 137 H11A 2 0.921063 0.723036 1.008100 11.00000 -1.50000 H11B 2 0.970533 0.671194 1.085162 11.00000 -1.50000 H11C 2 0.901691 0.641054 1.038066 11.00000 -1.50000 AFIX 0 C12 1 0.715062 0.285345 0.837154 11.00000 0.05373 0.03347 = 0.02937 -0.00120 0.02939 -0.00114 C13 1 0.685145 0.324735 0.908589 11.00000 0.06796 0.02928 = 0.03656 0.00345 0.03868 0.00024 C14 1 0.763876 0.317426 0.903561 11.00000 0.05784 0.03138 = 0.02880 0.00015 0.03070 -0.00038 C15 1 0.605956 0.256298 0.782454 11.00000 0.06178 0.04247 = 0.04340 0.00133 0.03497 0.00396 AFIX 23 H15A 2 0.589429 0.227972 0.807479 11.00000 -1.20000 H15B 2 0.607480 0.208227 0.751713 11.00000 -1.20000 AFIX 0 C16 1 0.564848 0.332174 0.731183 11.00000 0.08127 0.05827 = 0.04941 0.00197 0.02826 0.01142 PART 1 AFIX 23 H16A 2 0.523642 0.314031 0.711978 21.00000 -1.20000 H16B 2 0.574967 0.387378 0.763055 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H16C 2 0.556001 0.371414 0.760285 -21.00000 -1.20000 H16D 2 0.586998 0.370618 0.718128 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C17 1 0.562841 0.360367 0.666693 21.00000 0.07588 0.06158 = 0.04730 0.00538 0.03516 0.00821 AFIX 23 H17A 2 0.604114 0.374909 0.684123 21.00000 -1.20000 H17B 2 0.538997 0.417624 0.645932 21.00000 -1.20000 AFIX 0 C18 1 0.536735 0.290740 0.604232 21.00000 0.09027 0.07736 = 0.05319 0.00290 0.02768 0.00284 AFIX 137 H18A 2 0.544389 0.309879 0.567896 21.00000 -1.50000 H18B 2 0.493421 0.286195 0.578568 21.00000 -1.50000 H18C 2 0.555352 0.230690 0.625457 21.00000 -1.50000 AFIX 0 PART 0 C19 1 0.782654 0.389204 1.020722 11.00000 0.07461 0.03662 = 0.02667 -0.00052 0.03300 -0.00041 AFIX 23 H19A 2 0.820100 0.353854 1.054806 11.00000 -1.20000 H19B 2 0.761156 0.391180 1.044041 11.00000 -1.20000 AFIX 0 C20 1 0.798421 0.487022 1.013305 11.00000 0.06601 0.03591 = 0.03740 -0.00363 0.03422 -0.00143 AFIX 23 H20A 2 0.822880 0.515993 1.063942 11.00000 -1.20000 H20B 2 0.823048 0.484632 0.994273 11.00000 -1.20000 AFIX 0 C21 1 0.743369 0.546489 0.960290 11.00000 0.07529 0.04124 = 0.05745 0.00429 0.03843 0.00655 AFIX 23 H21A 2 0.720368 0.520005 0.908767 11.00000 -1.20000 H21B 2 0.717315 0.545526 0.977273 11.00000 -1.20000 AFIX 0 C22 1 0.759460 0.645160 0.957463 11.00000 0.09121 0.03430 = 0.06317 0.00110 0.04195 0.00993 AFIX 137 H22A 2 0.780326 0.647373 0.933843 11.00000 -1.50000 H22B 2 0.785644 0.669790 1.008938 11.00000 -1.50000 H22C 2 0.722822 0.682172 0.927777 11.00000 -1.50000 AFIX 0 C23 1 0.782056 0.167996 0.819822 11.00000 0.05237 0.02870 = 0.03295 -0.00201 0.03008 -0.00533 AFIX 13 H23 2 0.768227 0.114098 0.834026 11.00000 -1.20000 AFIX 0 C24 1 0.800458 0.135519 0.771346 11.00000 0.05357 0.03308 = 0.03930 -0.00525 0.03280 -0.00641 C25 1 0.883296 0.213033 0.871824 11.00000 0.04688 0.03729 = 0.02799 0.00145 0.02130 0.00145 C26 1 0.839303 0.207215 0.891120 11.00000 0.05418 0.03019 = 0.02767 0.00168 0.02613 -0.00060 AFIX 13 H26 2 0.854877 0.162144 0.933301 11.00000 -1.20000 AFIX 0 C27 1 0.883108 0.172064 0.760457 11.00000 0.04167 0.03977 = 0.03259 -0.00143 0.02387 0.00043 C28 1 0.891092 0.090183 0.735693 11.00000 0.05838 0.04337 = 0.05069 -0.00369 0.03939 -0.00035 AFIX 43 H28 2 0.882391 0.032886 0.748007 11.00000 -1.20000 AFIX 0 C29 1 0.912408 0.094411 0.691891 11.00000 0.06862 0.05557 = 0.05878 -0.00858 0.04672 0.00273 AFIX 43 H29 2 0.917814 0.039081 0.673591 11.00000 -1.20000 AFIX 0 C30 1 0.925729 0.177466 0.674769 11.00000 0.05905 0.07528 = 0.04911 -0.00505 0.04167 -0.00640 AFIX 43 H30 2 0.941351 0.179276 0.646243 11.00000 -1.20000 AFIX 0 C31 1 0.916200 0.257607 0.699353 11.00000 0.06754 0.05315 = 0.05971 -0.00108 0.04596 -0.01093 AFIX 43 H31 2 0.924235 0.314999 0.686364 11.00000 -1.20000 AFIX 0 C32 1 0.895207 0.255939 0.742471 11.00000 0.05679 0.03964 = 0.05033 -0.00496 0.03716 -0.00631 AFIX 43 H32 2 0.889097 0.311618 0.759671 11.00000 -1.20000 AFIX 0 PART -1 CL1 3 0.529561 0.052803 0.821634 10.25000 0.08807 0.08946 = 0.09677 0.01660 0.06740 0.01475 C33 1 0.501039 0.006445 0.733204 10.25000 0.06330 0.05284 = 0.10943 0.01145 0.06420 0.00956 AFIX 23 H33A 2 0.533502 -0.027789 0.736742 10.25000 -1.20000 H33B 2 0.469319 -0.038385 0.720091 10.25000 -1.20000 AFIX 0 CL2 3 0.471845 0.084682 0.661292 10.25000 0.06243 0.04140 = 0.10096 -0.00119 0.05053 0.00668 PART 0 PART 2 C18S 1 0.510879 0.244096 0.609897 -21.00000 0.08592 0.08484 = 0.05792 0.00145 0.02406 -0.00442 AFIX 137 H18D 2 0.476134 0.256204 0.557827 -21.00000 -1.50000 H18E 2 0.509831 0.180037 0.622963 -21.00000 -1.50000 H18F 2 0.547787 0.254918 0.614410 -21.00000 -1.50000 AFIX 0 C17S 1 0.509180 0.306745 0.662436 -21.00000 0.08032 0.06698 = 0.05238 0.00466 0.02856 0.00767 AFIX 23 H17C 2 0.488322 0.363871 0.634473 -21.00000 -1.20000 H17D 2 0.484324 0.277092 0.675600 -21.00000 -1.20000 AFIX 0 HKLF 4 REM 5078f in C2/c #15 REM R1 = 0.0729 for 6399 Fo > 4sig(Fo) and 0.0981 for all 8586 data REM 439 parameters refined using 64 restraints END WGHT 0.1137 17.3881 REM Highest difference peak 1.256, deepest hole -0.514, 1-sigma level 0.093 Q1 1 0.5000 0.0819 0.7500 10.50000 0.05 1.26 Q2 1 0.5162 0.0200 0.8053 11.00000 0.05 0.94 Q3 1 0.5778 0.4659 0.5646 11.00000 0.05 0.88 Q4 1 0.5212 0.4250 0.6139 11.00000 0.05 0.55 Q5 1 0.7551 0.4966 1.0042 11.00000 0.05 0.36 Q6 1 0.7804 0.5389 0.9612 11.00000 0.05 0.35 Q7 1 0.6786 0.3991 0.5782 11.00000 0.05 0.34 Q8 1 0.7786 0.5569 0.6679 11.00000 0.05 0.31 Q9 1 0.7136 0.2704 0.8060 11.00000 0.05 0.28 Q10 1 0.7800 0.3563 0.7977 11.00000 0.05 0.26 Q11 1 0.5944 0.3158 0.8813 11.00000 0.05 0.25 Q12 1 0.7975 0.5222 0.6395 11.00000 0.05 0.24 Q13 1 0.8211 0.3786 0.8760 11.00000 0.05 0.24 Q14 1 0.9246 0.6246 0.9405 11.00000 0.05 0.24 Q15 1 0.6046 0.3985 0.9023 11.00000 0.05 0.23 Q16 1 0.7361 0.1216 0.8093 11.00000 0.05 0.23 Q17 1 0.7550 0.2004 0.7944 11.00000 0.05 0.23 Q18 1 1.0205 0.7763 1.1358 11.00000 0.05 0.21 Q19 1 0.8807 0.5256 0.8192 11.00000 0.05 0.21 Q20 1 0.9663 0.7235 1.0621 11.00000 0.05 0.21 ; _shelx_res_checksum 87747 _shelx_hkl_file ; -6 0 6 13.97 0.65 6 0 -6 13.95 0.93 6 0 -6 14.54 0.71 8 0 -8 57.87 2.48 -8 0 8 60.75 1.93 8 0 -8 57.72 2.03 -10 0 10 0.14 0.12 10 0 -10 -0.19 0.17 10 0 -10 0.29 0.34 -10 0 10 0.64 0.23 12 0 -12 221.07 6.69 -12 0 12 231.75 6.41 -12 0 12 228.12 6.49 12 0 -12 221.56 7.55 14 0 -14 5.10 0.61 -14 0 14 5.69 0.43 14 0 -14 4.15 0.94 -14 0 14 4.69 0.38 -16 0 16 12.02 0.61 -16 0 16 11.91 0.64 16 0 -16 12.51 0.97 16 0 -16 13.12 0.92 16 0 -16 13.42 1.47 18 0 -18 6.33 0.65 -18 0 18 5.70 0.28 18 0 -18 5.50 1.18 18 0 -18 6.78 0.78 -18 0 18 6.25 0.29 20 0 -20 2.90 0.54 20 0 -20 3.49 0.74 20 0 -20 4.49 1.18 22 0 -22 2.12 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16.41 1.29 -3 -5 1 15.56 1.17 1 5 1 183.95 6.06 1 5 1 180.41 6.22 -1 5 -1 192.32 6.16 1 5 1 185.71 5.53 1 5 1 174.25 5.89 1 -5 1 178.72 6.03 -1 -5 -1 183.17 6.01 1 -5 1 182.14 5.91 1 -5 1 182.62 5.93 -1 -5 -1 193.88 6.19 -1 -5 -1 179.10 5.87 -1 -5 -1 189.24 5.48 1 5 -3 114.35 4.12 1 5 -3 115.14 4.16 -1 5 3 111.38 4.13 1 5 -3 101.75 3.97 -1 5 3 106.32 4.19 -1 5 3 109.40 3.90 -1 5 3 114.22 3.61 -1 -5 3 115.84 4.10 -1 -5 3 113.59 4.04 1 -5 -3 111.78 4.09 1 -5 -3 106.93 3.86 1 -5 -3 117.51 3.60 1 -5 -3 112.76 4.11 -1 -5 3 107.92 3.99 -3 5 5 10.32 0.96 3 5 -5 9.68 0.97 -3 5 5 10.38 0.99 3 5 -5 9.32 0.97 3 5 -5 9.13 0.87 -3 5 5 9.84 0.79 3 -5 -5 9.54 0.78 -3 -5 5 9.20 0.90 3 -5 -5 9.30 0.98 -3 -5 5 8.32 0.85 3 -5 -5 9.51 0.88 3 -5 -5 8.87 0.79 -3 -5 5 9.29 0.86 5 5 -7 140.37 5.12 -5 5 7 137.76 4.54 -5 5 7 136.58 5.05 -5 5 7 143.22 4.93 5 5 -7 143.41 4.80 5 5 -7 141.57 5.06 5 -5 -7 128.86 4.66 5 -5 -7 147.75 5.07 5 -5 -7 136.34 4.53 5 -5 -7 139.17 4.81 -5 -5 7 138.22 4.70 -5 -5 7 143.14 5.07 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19 -0.13 0.14 19 5 -21 18.39 1.77 19 5 -21 16.44 1.92 19 -5 -21 17.60 2.11 19 -5 -21 14.14 1.47 19 -5 -21 17.15 1.08 21 5 -23 13.52 2.19 21 5 -23 14.98 1.63 21 -5 -23 13.68 2.34 21 -5 -23 13.32 0.90 23 5 -25 9.88 1.97 23 -5 -25 9.46 2.05 25 5 -27 12.27 2.26 25 -5 -27 14.35 2.55 27 5 -29 -0.41 0.33 27 -5 -29 0.01 0.37 28 6 -26 0.14 0.52 28 -6 -26 -0.03 0.32 26 6 -24 0.70 0.57 26 -6 -24 -0.08 0.40 24 6 -22 -0.64 0.35 24 6 -22 0.36 0.32 24 -6 -22 0.21 0.42 24 -6 -22 -0.37 0.45 22 6 -20 1.62 0.71 22 6 -20 0.99 0.70 22 -6 -20 0.74 0.66 22 -6 -20 1.61 0.84 20 6 -18 86.66 4.35 20 6 -18 94.09 4.62 -20 -6 18 89.51 3.94 20 -6 -18 86.38 4.61 20 -6 -18 87.53 4.81 18 6 -16 1.01 0.57 18 6 -16 1.78 0.73 -18 -6 16 1.44 0.50 18 -6 -16 1.98 0.28 18 -6 -16 0.93 0.61 18 -6 -16 1.76 0.28 16 6 -14 95.01 4.19 16 6 -14 94.36 4.53 16 -6 -14 91.03 2.97 -16 -6 14 101.78 4.18 16 -6 -14 88.76 3.01 16 -6 -14 92.35 4.58 14 6 -12 4.47 1.10 14 6 -12 3.80 0.85 14 -6 -12 2.16 0.83 -14 -6 12 2.98 0.75 14 -6 -12 3.82 0.54 12 6 -10 30.58 2.21 -12 6 10 31.54 1.54 12 6 -10 31.26 1.96 12 -6 -10 32.43 1.49 12 -6 -10 33.78 2.35 -12 -6 10 30.81 2.00 10 6 -8 6.96 1.00 10 6 -8 7.01 1.25 -10 6 8 7.39 0.73 10 -6 -8 8.24 0.75 10 -6 -8 6.24 1.18 -10 -6 8 7.20 0.80 -10 -6 8 7.81 1.16 -10 -6 8 8.36 1.18 8 6 -6 190.47 6.67 8 6 -6 190.48 6.97 -8 6 6 190.99 6.28 8 6 -6 201.21 6.37 8 6 -6 192.09 6.96 8 -6 -6 195.53 6.08 8 -6 -6 185.49 6.90 8 -6 -6 182.33 6.02 -8 -6 6 196.91 6.58 -8 -6 6 197.51 6.33 -8 -6 6 196.41 6.66 6 6 -4 23.99 1.69 -6 6 4 25.10 2.05 -6 6 4 25.28 1.56 6 6 -4 23.58 1.84 6 6 -4 23.83 1.54 6 6 -4 24.32 1.58 6 6 -4 24.28 1.61 -6 -6 4 23.32 1.63 6 -6 -4 23.16 1.47 6 -6 -4 22.01 0.84 -6 -6 4 23.84 1.45 6 -6 -4 23.91 1.79 6 -6 -4 23.69 0.83 6 -6 -4 23.13 1.39 -6 -6 4 23.10 1.61 -4 6 2 16.01 1.35 4 6 -2 13.53 1.17 4 6 -2 11.16 1.27 4 6 -2 12.89 1.22 -4 6 2 13.02 1.14 4 6 -2 13.97 1.06 -4 -6 2 14.49 1.26 -4 -6 2 12.16 1.01 -4 -6 2 13.50 1.24 4 -6 -2 12.78 1.27 4 -6 -2 12.39 1.05 4 -6 -2 12.25 1.13 -4 -6 2 14.62 1.26 -2 6 0 110.83 4.17 2 6 0 108.97 4.11 2 6 0 107.32 4.38 2 6 0 102.63 4.11 2 6 0 108.19 3.64 -2 6 0 105.48 4.25 -2 -6 0 100.62 3.97 2 -6 0 106.20 3.96 2 -6 0 107.60 4.19 2 -6 0 107.67 4.10 -2 -6 0 103.89 4.12 -2 -6 0 106.98 3.55 -2 -6 0 102.76 4.07 2 -6 0 105.08 4.03 0 6 2 171.63 5.08 0 6 -2 169.35 5.81 0 6 -2 166.87 5.84 0 6 2 159.76 5.78 0 6 2 167.28 6.00 0 6 2 153.13 5.53 0 -6 -2 162.57 5.54 0 -6 -2 164.18 5.70 0 -6 -2 163.03 5.73 0 -6 2 166.41 5.65 0 -6 2 164.74 5.80 0 -6 -2 165.32 4.98 0 -6 2 169.55 5.77 0 -6 2 160.53 5.58 -2 6 4 15.51 1.32 -2 6 4 16.48 1.41 -2 6 4 17.14 1.01 -2 6 4 15.64 1.19 2 6 -4 18.11 1.46 2 6 -4 17.28 1.42 2 6 -4 15.41 1.27 -2 -6 4 16.68 1.32 -2 -6 4 17.06 1.34 -2 -6 4 15.42 1.39 2 -6 -4 19.88 1.07 2 -6 -4 15.65 1.20 2 -6 -4 16.30 1.38 2 -6 -4 19.70 1.39 -2 -6 4 16.08 1.28 -4 6 6 22.43 1.61 -4 6 6 19.44 1.51 4 6 -6 21.39 1.47 4 6 -6 22.96 1.64 4 6 -6 22.48 1.69 -4 6 6 20.68 1.32 -4 -6 6 19.10 1.59 4 -6 -6 20.93 1.45 4 -6 -6 19.76 1.56 4 -6 -6 22.89 1.31 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3.66 0.57 15 -7 -13 2.22 0.86 15 -7 -13 3.61 0.58 -15 -7 13 2.76 0.76 13 7 -11 21.25 1.65 13 7 -11 15.95 1.71 -13 7 11 18.51 1.19 13 -7 -11 18.70 1.15 -13 -7 11 18.20 1.58 13 -7 -11 17.45 1.14 13 -7 -11 17.12 1.78 -13 -7 11 18.93 1.57 -11 7 9 8.24 0.85 11 7 -9 8.58 1.22 11 7 -9 8.19 1.44 -11 -7 9 8.73 1.35 -11 -7 9 9.20 1.31 11 -7 -9 8.31 1.42 11 -7 -9 8.37 0.79 11 -7 -9 7.86 0.78 9 7 -7 2.03 0.64 -9 7 7 1.44 0.46 9 7 -7 2.55 0.81 9 7 -7 2.11 0.65 -9 -7 7 2.59 0.74 -9 -7 7 1.48 0.58 -9 -7 7 2.36 0.67 9 -7 -7 1.64 0.50 9 -7 -7 2.32 0.79 9 -7 -7 1.74 0.57 7 7 -5 1.99 0.65 -7 7 5 2.33 0.59 7 7 -5 2.64 0.64 7 7 -5 2.44 0.77 7 -7 -5 2.11 0.61 -7 -7 5 1.80 0.50 7 -7 -5 1.98 0.24 7 -7 -5 1.56 0.19 -7 -7 5 1.71 0.59 -7 -7 5 1.44 0.56 7 -7 -5 2.09 0.55 7 -7 -5 0.69 0.56 5 7 -3 0.59 0.56 5 7 -3 0.54 0.37 -5 7 3 0.48 0.41 -5 -7 3 0.56 0.34 -5 -7 3 -0.41 0.34 5 -7 -3 0.77 0.58 5 -7 -3 0.48 0.49 -5 -7 3 0.66 0.46 5 -7 -3 0.57 0.39 3 7 -1 9.05 1.46 -3 7 1 7.07 1.12 3 7 -1 7.43 0.77 3 -7 -1 8.04 1.18 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-22 -2 -7 0.42 0.28 22 -2 7 0.64 0.68 -20 2 -9 2.31 0.69 20 2 9 1.08 0.96 -20 -2 -9 1.14 0.57 20 -2 9 0.49 0.85 18 2 11 0.92 0.81 -18 2 -11 0.04 0.32 18 -2 11 0.93 0.54 -18 -2 -11 0.41 0.31 -16 2 -13 0.98 0.38 16 2 13 0.56 0.60 16 -2 13 -0.12 0.50 -16 -2 -13 0.79 0.32 -14 2 -15 0.06 0.42 14 2 15 0.40 0.52 -14 -2 -15 1.48 0.37 -12 2 -17 1.23 0.39 -12 2 -17 -0.22 0.33 -12 -2 -17 0.18 0.27 -12 -2 -17 0.78 0.30 33 -3 -4 -0.10 0.77 31 3 -2 -0.97 0.81 31 -3 -2 0.14 0.88 29 3 0 -1.16 0.59 29 -3 0 -0.03 0.75 27 3 2 -0.10 0.80 27 -3 2 1.49 1.12 25 3 4 0.07 0.77 -25 -3 -4 0.19 0.31 25 -3 4 1.33 1.09 -23 3 -6 1.10 0.29 23 3 6 -0.01 0.78 23 -3 6 -0.43 0.52 -23 -3 -6 0.39 0.36 21 3 8 0.10 0.81 -21 3 -8 0.86 0.34 21 -3 8 -0.54 0.54 -21 -3 -8 0.02 0.29 -19 3 -10 0.63 0.29 19 3 10 0.23 0.53 -19 -3 -10 -0.57 0.28 19 -3 10 0.82 0.63 -17 3 -12 1.17 0.48 17 3 12 0.85 0.74 -17 -3 -12 0.88 0.37 17 -3 12 1.47 0.75 15 3 14 1.75 0.78 -15 3 -14 1.42 0.36 -15 -3 -14 0.72 0.35 -13 3 -16 0.68 0.38 -13 3 -16 0.20 0.50 -13 -3 -16 0.78 0.39 -11 3 -18 2.03 0.52 -11 3 -18 -0.24 0.37 -11 -3 -18 0.30 0.27 -11 -3 -18 2.06 0.60 32 4 -3 -0.20 0.70 32 -4 -3 -0.12 0.89 30 4 -1 0.05 0.94 30 -4 -1 0.82 0.90 28 4 1 -0.95 0.68 28 -4 1 -0.17 0.97 26 4 3 -0.69 0.71 -26 -4 -3 0.52 0.35 26 -4 3 -0.11 0.84 24 4 5 -0.35 0.72 -24 -4 -5 0.34 0.37 24 -4 5 1.03 0.85 -22 4 -7 0.84 0.27 -22 -4 -7 1.65 0.42 22 -4 7 -0.63 0.57 20 4 9 1.00 0.57 -20 4 -9 0.56 0.31 -20 -4 -9 0.92 0.33 20 -4 9 0.47 0.62 -18 4 -11 -0.37 0.32 18 4 11 0.16 0.57 -18 4 -11 -0.89 0.33 18 -4 11 1.03 0.63 -18 -4 -11 0.09 0.28 16 4 13 1.15 0.65 -16 4 -13 -0.24 0.38 -16 -4 -13 0.62 0.38 14 4 15 1.23 0.49 -14 4 -15 0.02 0.40 -14 -4 -15 0.82 0.41 -12 4 -17 1.64 0.44 -12 -4 -17 0.47 0.52 31 5 -2 0.53 1.00 31 -5 -2 -0.71 0.53 29 5 0 -0.80 0.30 29 -5 0 -0.19 0.83 27 5 2 0.13 0.74 27 -5 2 -0.31 0.73 25 5 4 0.09 0.41 -25 -5 -4 0.54 0.28 25 -5 4 1.01 0.98 23 5 6 0.00 0.62 -23 -5 -6 1.13 0.34 23 -5 6 -0.04 0.67 21 5 8 0.54 0.60 -21 5 -8 0.81 0.31 -21 -5 -8 1.19 0.34 21 -5 8 3.13 1.20 19 5 10 -0.10 0.38 -19 5 -10 0.50 0.33 19 -5 10 0.64 0.36 19 -5 10 1.66 0.73 -19 -5 -10 0.21 0.30 -17 5 -12 0.63 0.36 17 5 12 -0.31 0.35 -17 -5 -12 2.08 0.55 -15 5 -14 1.04 0.45 15 5 14 2.07 0.84 -15 -5 -14 1.87 0.58 -13 5 -16 0.58 0.32 -13 -5 -16 -0.14 0.34 30 6 -1 -0.60 0.56 30 -6 -1 -1.43 0.55 28 6 1 -0.36 0.72 28 -6 1 0.13 0.73 26 6 3 -0.11 0.66 26 -6 3 2.07 0.94 -26 -6 -3 1.01 0.35 26 -6 3 0.77 0.29 24 6 5 -0.65 0.31 24 -6 5 1.67 0.49 24 -6 5 1.06 0.91 -24 -6 -5 0.44 0.35 -22 -6 -7 -0.33 0.35 22 -6 7 1.96 0.83 22 -6 7 0.57 0.30 20 6 9 0.44 0.48 -20 6 -9 0.13 0.33 20 -6 9 0.63 0.63 -20 -6 -9 -0.33 0.29 20 -6 9 0.21 0.33 -18 6 -11 -0.45 0.43 -18 6 -11 0.66 0.37 18 6 11 1.35 0.76 -18 -6 -11 1.03 0.56 -16 6 -13 -0.53 0.33 16 6 13 -0.03 0.47 -16 -6 -13 -0.02 0.36 14 6 15 0.87 0.40 -14 6 -15 1.21 0.33 -14 -6 -15 0.81 0.38 29 7 0 -0.14 0.42 29 -7 0 1.18 0.37 27 7 2 -0.19 0.55 27 -7 2 0.67 0.62 27 -7 2 0.85 0.48 25 7 4 0.44 0.58 25 -7 4 0.60 0.67 -25 -7 -4 0.60 0.37 25 -7 4 0.87 0.41 23 7 6 -0.26 0.42 23 -7 6 -0.26 0.35 -23 -7 -6 0.28 0.33 23 -7 6 0.25 0.34 21 7 8 0.92 0.69 -21 -7 -8 0.42 0.33 21 -7 8 1.09 0.46 21 -7 8 0.28 0.32 19 7 10 0.81 0.54 -19 7 -10 0.03 0.32 -19 -7 -10 0.30 0.31 -17 7 -12 -0.41 0.30 17 7 12 -0.38 0.40 -17 7 -12 1.18 0.40 -17 -7 -12 -0.72 0.29 26 -8 3 0.98 0.32 -26 -8 -3 0.60 0.35 24 8 5 -0.07 0.39 -24 -8 -5 -0.99 0.31 24 -8 5 0.19 0.31 22 8 7 -0.18 0.53 22 -8 7 0.15 0.33 -22 -8 -7 0.87 0.32 20 8 9 -0.57 0.66 -20 -8 -9 1.25 0.40 32 0 -2 -0.78 0.76 30 0 0 -0.74 0.80 28 0 2 0.79 1.06 26 0 4 0.81 0.93 24 0 6 0.19 0.83 -24 0 -6 0.83 0.28 22 0 8 0.18 0.64 -22 0 -8 0.64 0.27 -20 0 -10 1.95 0.71 20 0 10 0.54 0.80 -18 0 -12 2.37 0.64 18 0 12 2.95 1.06 -16 0 -14 0.99 0.35 -14 0 -16 0.43 0.33 33 -1 -3 -1.28 0.47 31 1 -1 0.70 0.95 31 -1 -1 -0.96 0.75 29 1 1 -0.94 0.63 29 -1 1 0.17 0.84 27 1 3 -0.74 0.66 27 -1 3 0.43 0.87 25 1 5 2.30 1.37 25 -1 5 2.03 1.33 -25 -1 -5 2.66 0.74 -23 1 -7 1.00 0.54 23 1 7 2.69 1.39 23 -1 7 1.44 0.88 -23 -1 -7 3.62 0.83 21 1 9 0.91 0.75 -21 1 -9 0.25 0.35 -21 -1 -9 1.15 0.50 21 -1 9 1.02 0.95 19 1 11 -0.67 0.51 -19 1 -11 0.43 0.28 -19 -1 -11 1.24 0.41 19 -1 11 0.80 0.79 -17 1 -13 1.17 0.39 17 1 13 2.32 0.95 -17 -1 -13 0.83 0.36 17 -1 13 0.94 0.61 -15 1 -15 0.63 0.50 -15 -1 -15 0.28 0.41 32 2 -2 -1.20 0.72 32 -2 -2 -1.28 0.72 30 2 0 -1.04 0.72 30 -2 0 -0.04 0.84 28 2 2 0.29 0.96 28 -2 2 0.37 0.76 26 2 4 2.15 1.30 26 -2 4 -0.45 0.80 -24 2 -6 0.45 0.32 24 2 6 -0.59 0.80 -24 -2 -6 -0.78 0.29 24 -2 6 0.01 0.73 -22 2 -8 0.93 0.41 22 2 8 1.29 1.07 -22 -2 -8 0.31 0.31 22 -2 8 0.07 0.68 20 2 10 1.22 0.97 -20 2 -10 1.52 0.49 20 -2 10 1.28 0.90 -20 -2 -10 0.81 0.38 -18 2 -12 2.57 0.62 18 2 12 3.09 1.45 18 -2 12 3.40 1.11 -18 -2 -12 2.63 0.76 -16 2 -14 0.08 0.37 16 2 14 0.48 0.36 -16 -2 -14 1.30 0.52 -14 2 -16 0.95 0.34 -14 -2 -16 0.41 0.33 31 3 -1 -0.89 0.56 31 -3 -1 -0.10 0.76 29 3 1 -0.54 0.66 29 -3 1 1.46 1.17 27 3 3 0.81 1.06 27 -3 3 0.20 1.03 25 3 5 -0.03 0.94 -25 -3 -5 0.20 0.29 25 -3 5 -0.25 0.68 23 3 7 -0.36 1.00 -23 3 -7 0.81 0.47 23 -3 7 0.69 0.80 -23 -3 -7 -0.14 0.32 21 3 9 0.02 0.61 -21 3 -9 1.87 0.63 -21 -3 -9 0.97 0.34 21 -3 9 0.85 0.93 -19 3 -11 0.04 0.30 19 3 11 0.80 0.80 -19 -3 -11 0.29 0.36 19 -3 11 1.69 0.73 -17 3 -13 -0.06 0.33 17 3 13 0.00 0.67 -17 -3 -13 -0.11 0.31 -15 3 -15 0.10 0.34 15 3 15 1.37 0.68 -15 -3 -15 1.06 0.53 30 4 0 0.95 1.08 30 -4 0 -0.17 0.68 28 4 2 -0.36 0.74 28 -4 2 0.83 1.03 26 4 4 0.01 0.65 26 -4 4 -0.17 0.75 -26 -4 -4 0.02 0.32 24 4 6 0.43 0.87 -24 -4 -6 0.47 0.32 24 -4 6 0.59 0.90 -22 4 -8 0.98 0.35 22 4 8 0.41 0.83 -22 -4 -8 1.08 0.31 22 -4 8 0.81 0.86 20 4 10 -0.34 0.48 -20 4 -10 0.57 0.31 20 -4 10 0.99 0.76 -20 -4 -10 -0.23 0.29 -18 4 -12 1.15 0.35 18 4 12 0.62 0.83 -18 -4 -12 0.66 0.40 -16 4 -14 0.45 0.48 -16 -4 -14 0.33 0.33 29 5 1 -1.24 0.54 29 -5 1 -0.45 0.72 27 5 3 0.46 0.95 27 -5 3 1.71 0.88 25 5 5 -0.10 0.43 25 -5 5 -0.04 0.57 -25 -5 -5 1.17 0.39 23 5 7 -1.26 0.42 -23 -5 -7 0.56 0.40 23 -5 7 0.84 0.33 23 -5 7 -0.47 0.53 -21 5 -9 0.95 0.32 21 5 9 0.75 0.48 -21 -5 -9 0.51 0.33 21 -5 9 1.66 0.65 21 -5 9 1.00 0.32 19 5 11 1.39 0.73 -19 5 -11 0.31 0.30 -19 -5 -11 0.74 0.35 -17 5 -13 1.19 0.48 17 5 13 0.11 0.53 -17 -5 -13 1.09 0.41 28 6 2 2.89 1.44 28 -6 2 2.99 1.16 26 6 4 -0.51 0.40 26 -6 4 0.44 0.72 26 -6 4 1.31 0.38 -26 -6 -4 0.42 0.42 24 6 6 1.02 0.81 24 -6 6 0.38 0.32 -24 -6 -6 -0.19 0.36 24 -6 6 0.63 0.62 22 6 8 0.55 0.76 22 -6 8 0.48 0.50 22 -6 8 0.54 0.30 -22 -6 -8 -0.43 0.30 20 6 10 -0.15 0.36 -20 6 -10 0.17 0.32 -20 -6 -10 0.23 0.43 18 6 12 0.07 0.43 -18 6 -12 0.53 0.41 -18 -6 -12 0.95 0.45 30 0 1 -0.13 0.66 28 0 3 0.29 1.06 26 0 5 0.15 0.85 24 0 7 0.12 0.75 22 0 9 -0.81 0.53 -22 0 -9 0.45 0.32 -20 0 -11 0.19 0.36 20 0 11 0.68 0.94 -18 0 -13 0.87 0.47 18 0 13 2.08 1.10 29 1 2 -0.25 0.76 29 -1 2 0.64 0.78 27 1 4 0.05 0.87 27 -1 4 0.10 0.99 25 1 6 0.47 0.98 -25 -1 -6 1.13 0.36 25 -1 6 1.26 1.02 -23 1 -8 0.17 0.31 23 1 8 -0.67 0.54 -23 -1 -8 -0.57 0.30 23 -1 8 -0.35 0.58 -21 1 -10 -0.13 0.33 21 1 10 0.13 0.59 -21 -1 -10 -0.23 0.32 21 -1 10 0.89 0.79 19 1 12 0.42 0.61 19 -1 12 1.43 0.63 -19 -1 -12 0.80 0.41 17 1 14 1.62 0.60 -17 1 -14 0.98 0.40 -17 -1 -14 0.49 0.44 30 2 1 -0.74 0.62 30 -2 1 0.77 0.98 28 2 3 0.18 0.74 28 -2 3 -0.58 0.64 26 2 5 0.20 0.83 26 -2 5 -0.85 0.60 24 2 7 -0.95 0.54 24 -2 7 0.30 0.66 -24 -2 -7 0.25 0.30 22 2 9 1.07 0.78 -22 -2 -9 1.37 0.54 22 -2 9 1.96 1.15 20 2 11 -0.52 0.44 -20 2 -11 0.60 0.41 -20 -2 -11 0.91 0.41 20 -2 11 0.65 0.55 -18 2 -13 -0.47 0.33 18 2 13 0.39 0.50 18 -2 13 1.12 0.54 -18 -2 -13 0.24 0.31 29 -3 2 1.24 1.04 27 3 4 0.04 0.70 27 -3 4 0.14 0.77 25 3 6 0.27 0.84 25 -3 6 0.39 0.84 -25 -3 -6 -0.09 0.31 -23 3 -8 0.61 0.54 23 3 8 -0.25 0.70 23 -3 8 1.33 0.95 -23 -3 -8 0.00 0.34 -21 3 -10 0.37 0.32 21 3 10 0.17 0.66 -21 -3 -10 0.64 0.36 21 -3 10 1.59 0.78 -19 3 -12 0.43 0.37 19 3 12 1.35 0.92 -19 -3 -12 0.01 0.33 19 -3 12 0.69 0.52 26 4 5 -0.08 0.48 26 -4 5 0.34 0.60 -26 -4 -5 0.19 0.37 24 4 7 0.82 1.18 -24 -4 -7 1.47 0.66 24 -4 7 1.20 0.95 -22 4 -9 0.16 0.51 22 4 9 0.34 0.64 22 -4 9 1.02 0.59 -22 -4 -9 0.18 0.32 20 4 11 -0.30 0.39 -20 4 -11 0.64 0.36 -20 -4 -11 -0.17 0.32 20 -4 11 1.31 0.61 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 96241 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.83123(4) 0.51728(6) 0.70134(5) 0.0427(2) Uani 1 1 d . . . . . S2 S 0.64132(5) 0.34358(7) 0.93699(6) 0.0502(3) Uani 1 1 d . . . . . P1 P 0.71685(4) 0.24982(5) 0.75920(5) 0.0341(2) Uani 1 1 d . . . . . P2 P 0.83793(4) 0.32591(5) 0.92631(4) 0.0348(2) Uani 1 1 d . . . . . O1 O 0.77062(13) 0.0906(2) 0.71402(16) 0.0521(7) Uani 1 1 d . . . . . O2 O 0.93205(12) 0.2486(2) 0.90876(15) 0.0544(7) Uani 1 1 d . . . . . N1 N 0.76423(13) 0.38928(18) 0.71250(14) 0.0332(6) Uani 1 1 d . . . . . N2 N 0.84114(12) 0.44027(17) 0.82153(14) 0.0326(6) Uani 1 1 d . . . . . N3 N 0.66664(14) 0.28868(19) 0.84012(15) 0.0377(6) Uani 1 1 d . . . . . N4 N 0.74520(14) 0.34163(18) 0.94769(15) 0.0384(6) Uani 1 1 d . . . . . N5 N 0.85717(13) 0.17064(18) 0.80171(15) 0.0358(6) Uani 1 1 d . . . . . C1 C 0.76331(15) 0.3455(2) 0.76797(17) 0.0331(6) Uani 1 1 d . . . . . C2 C 0.81178(15) 0.4488(2) 0.74538(17) 0.0327(6) Uani 1 1 d . . . . . C3 C 0.81118(15) 0.3780(2) 0.83573(17) 0.0336(7) Uani 1 1 d . . . . . C4 C 0.72202(17) 0.3730(3) 0.63071(18) 0.0442(8) Uani 1 1 d . . . . . H4A H 0.7125 0.3065 0.6218 0.053 Uiso 1 1 calc R . . . . H4B H 0.7415 0.3902 0.6064 0.053 Uiso 1 1 calc R . . . . C5 C 0.6641(2) 0.4268(3) 0.5940(2) 0.0708(15) Uani 1 1 d . . . . . H5A H 0.6447 0.4077 0.6179 0.085 Uiso 1 1 calc R . . . . H5B H 0.6744 0.4928 0.6057 0.085 Uiso 1 1 calc R . . . . C6 C 0.6195(2) 0.4176(4) 0.5107(3) 0.0793(15) Uani 1 1 d . . . . . H6A H 0.6129 0.3511 0.4987 0.095 Uiso 1 1 calc R . . . . H6B H 0.6377 0.4430 0.4869 0.095 Uiso 1 1 calc R . . . . C7 C 0.5596(3) 0.4613(5) 0.4735(4) 0.106(2) Uani 1 1 d . . . . . H7A H 0.5299 0.4275 0.4273 0.159 Uiso 1 1 calc GR . . . . H7B H 0.5614 0.5252 0.4608 0.159 Uiso 1 1 calc GR . . . . H7C H 0.5482 0.4600 0.5080 0.159 Uiso 1 1 calc GR . . . . C8 C 0.89591(15) 0.4880(2) 0.87996(19) 0.0369(7) Uani 1 1 d . . . . . H8A H 0.9146 0.5150 0.8572 0.044 Uiso 1 1 calc R . . . . H8B H 0.9245 0.4430 0.9187 0.044 Uiso 1 1 calc R . . . . C9 C 0.88475(17) 0.5633(2) 0.9176(2) 0.0461(8) Uani 1 1 d . . . . . H9A H 0.8571 0.5404 0.9287 0.055 Uiso 1 1 calc R . . . . H9B H 0.8652 0.6161 0.8825 0.055 Uiso 1 1 calc R . . . . C10 C 0.9427(2) 0.5957(4) 0.9908(3) 0.0667(13) Uani 1 1 d . . . . . H10A H 0.9642 0.5415 1.0233 0.080 Uiso 1 1 calc R . . . . H10B H 0.9685 0.6242 0.9787 0.080 Uiso 1 1 calc R . . . . C11 C 0.9332(3) 0.6637(6) 1.0343(4) 0.117(3) Uani 1 1 d . . . . . H11A H 0.9211 0.7230 1.0081 0.175 Uiso 1 1 calc GR . . . . H11B H 0.9705 0.6712 1.0852 0.175 Uiso 1 1 calc GR . . . . H11C H 0.9017 0.6411 1.0381 0.175 Uiso 1 1 calc GR . . . . C12 C 0.71506(16) 0.2853(2) 0.83715(17) 0.0360(7) Uani 1 1 d . . . . . C13 C 0.68514(18) 0.3247(2) 0.90859(19) 0.0399(8) Uani 1 1 d . . . . . C14 C 0.76388(16) 0.3174(2) 0.90356(18) 0.0363(7) Uani 1 1 d . . . . . C15 C 0.60596(19) 0.2563(3) 0.7825(2) 0.0469(8) Uani 1 1 d . U . . . H15A H 0.5894 0.2280 0.8075 0.056 Uiso 1 1 calc R . . . . H15B H 0.6075 0.2082 0.7517 0.056 Uiso 1 1 calc R . . . . C16 C 0.5648(2) 0.3322(3) 0.7312(2) 0.0694(11) Uani 1 1 d D U . . . H16A H 0.5236 0.3140 0.7120 0.083 Uiso 0.569(7) 1 calc R . P A 1 H16B H 0.5750 0.3874 0.7631 0.083 Uiso 0.569(7) 1 calc R . P A 1 H16C H 0.5560 0.3714 0.7603 0.083 Uiso 0.431(7) 1 calc R . P A 2 H16D H 0.5870 0.3706 0.7181 0.083 Uiso 0.431(7) 1 calc R . P A 2 C17 C 0.5628(4) 0.3604(5) 0.6667(4) 0.0624(15) Uani 0.569(7) 1 d D U P A 1 H17A H 0.6041 0.3749 0.6841 0.075 Uiso 0.569(7) 1 calc R . P A 1 H17B H 0.5390 0.4176 0.6459 0.075 Uiso 0.569(7) 1 calc R . P A 1 C18 C 0.5367(5) 0.2907(7) 0.6042(5) 0.083(2) Uani 0.569(7) 1 d D U P A 1 H18A H 0.5444 0.3099 0.5679 0.124 Uiso 0.569(7) 1 calc GR . P A 1 H18B H 0.4934 0.2862 0.5786 0.124 Uiso 0.569(7) 1 calc GR . P A 1 H18C H 0.5554 0.2307 0.6255 0.124 Uiso 0.569(7) 1 calc GR . P A 1 C19 C 0.78265(19) 0.3892(2) 1.02072(18) 0.0442(8) Uani 1 1 d . . . . . H19A H 0.8201 0.3539 1.0548 0.053 Uiso 1 1 calc R . . . . H19B H 0.7612 0.3912 1.0440 0.053 Uiso 1 1 calc R . . . . C20 C 0.79842(18) 0.4870(2) 1.0133(2) 0.0443(8) Uani 1 1 d . . . . . H20A H 0.8229 0.5160 1.0639 0.053 Uiso 1 1 calc R . . . . H20B H 0.8230 0.4846 0.9943 0.053 Uiso 1 1 calc R . . . . C21 C 0.7434(2) 0.5465(3) 0.9603(3) 0.0586(11) Uani 1 1 d . . . . . H21A H 0.7204 0.5200 0.9088 0.070 Uiso 1 1 calc R . . . . H21B H 0.7173 0.5455 0.9773 0.070 Uiso 1 1 calc R . . . . C22 C 0.7595(2) 0.6452(3) 0.9575(3) 0.0652(12) Uani 1 1 d . . . . . H22A H 0.7803 0.6474 0.9338 0.098 Uiso 1 1 calc GR . . . . H22B H 0.7856 0.6698 1.0089 0.098 Uiso 1 1 calc GR . . . . H22C H 0.7228 0.6822 0.9278 0.098 Uiso 1 1 calc GR . . . . C23 C 0.78206(16) 0.1680(2) 0.81982(18) 0.0351(7) Uani 1 1 d . . . . . H23 H 0.7682 0.1141 0.8340 0.042 Uiso 1 1 calc R . . . . C24 C 0.80046(17) 0.1355(2) 0.77135(19) 0.0388(7) Uani 1 1 d . . . . . C25 C 0.88330(16) 0.2130(2) 0.87182(18) 0.0379(7) Uani 1 1 d . . . . . C26 C 0.83930(16) 0.2072(2) 0.89112(17) 0.0362(7) Uani 1 1 d . . . . . H26 H 0.8549 0.1621 0.9333 0.043 Uiso 1 1 calc R . . . . C27 C 0.88311(16) 0.1721(2) 0.76046(18) 0.0369(7) Uani 1 1 d . . . . . C28 C 0.89109(18) 0.0902(3) 0.7357(2) 0.0465(8) Uani 1 1 d . . . . . H28 H 0.8824 0.0329 0.7480 0.056 Uiso 1 1 calc R . . . . C29 C 0.9124(2) 0.0944(3) 0.6919(2) 0.0555(10) Uani 1 1 d . . . . . H29 H 0.9178 0.0391 0.6736 0.067 Uiso 1 1 calc R . . . . C30 C 0.9257(2) 0.1775(3) 0.6748(2) 0.0553(10) Uani 1 1 d . . . . . H30 H 0.9414 0.1793 0.6462 0.066 Uiso 1 1 calc R . . . . C31 C 0.9162(2) 0.2576(3) 0.6994(3) 0.0551(10) Uani 1 1 d . . . . . H31 H 0.9242 0.3150 0.6864 0.066 Uiso 1 1 calc R . . . . C32 C 0.89521(18) 0.2559(3) 0.7425(2) 0.0456(8) Uani 1 1 d . . . . . H32 H 0.8891 0.3116 0.7597 0.055 Uiso 1 1 calc R . . . . Cl1 Cl 0.5296(4) 0.0528(6) 0.8216(5) 0.084(2) Uani 0.25 1 d D U P B -1 C33 C 0.5010(9) 0.0064(9) 0.7332(7) 0.067(4) Uani 0.25 1 d D U P B -1 H33A H 0.5335 -0.0278 0.7367 0.081 Uiso 0.25 1 calc R . P B -1 H33B H 0.4693 -0.0384 0.7201 0.081 Uiso 0.25 1 calc R . P B -1 Cl2 Cl 0.4718(4) 0.0847(4) 0.6613(5) 0.0670(16) Uani 0.25 1 d D U P B -1 C18S C 0.5109(7) 0.2441(10) 0.6099(7) 0.088(3) Uani 0.431(7) 1 d D U P A 2 H18D H 0.4761 0.2562 0.5578 0.131 Uiso 0.431(7) 1 calc GR . P A 2 H18E H 0.5098 0.1800 0.6230 0.131 Uiso 0.431(7) 1 calc GR . P A 2 H18F H 0.5478 0.2549 0.6144 0.131 Uiso 0.431(7) 1 calc GR . P A 2 C17S C 0.5092(4) 0.3067(8) 0.6624(5) 0.0731(18) Uani 0.431(7) 1 d D U P A 2 H17C H 0.4883 0.3639 0.6345 0.088 Uiso 0.431(7) 1 calc R . P A 2 H17D H 0.4843 0.2771 0.6756 0.088 Uiso 0.431(7) 1 calc R . P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0580(6) 0.0398(4) 0.0437(5) 0.0116(3) 0.0374(4) 0.0030(4) S2 0.0761(7) 0.0501(5) 0.0481(5) 0.0047(4) 0.0498(5) 0.0060(5) P1 0.0489(5) 0.0326(4) 0.0280(4) -0.0049(3) 0.0266(4) -0.0065(3) P2 0.0523(5) 0.0303(4) 0.0242(4) -0.0005(3) 0.0239(4) -0.0028(3) O1 0.0568(16) 0.0599(16) 0.0503(15) -0.0268(13) 0.0376(14) -0.0181(13) O2 0.0475(16) 0.0697(19) 0.0383(14) -0.0139(13) 0.0213(12) -0.0064(13) N1 0.0461(15) 0.0331(13) 0.0234(12) 0.0022(10) 0.0223(11) -0.0005(11) N2 0.0418(15) 0.0302(12) 0.0271(12) 0.0018(10) 0.0212(12) -0.0021(10) N3 0.0563(18) 0.0328(13) 0.0358(14) -0.0008(11) 0.0337(14) -0.0032(12) N4 0.0633(19) 0.0336(13) 0.0292(13) 0.0001(10) 0.0334(14) -0.0007(12) N5 0.0466(16) 0.0341(13) 0.0314(13) -0.0028(10) 0.0257(12) -0.0030(11) C1 0.0476(18) 0.0293(14) 0.0262(14) 0.0011(11) 0.0240(14) -0.0031(12) C2 0.0402(17) 0.0298(14) 0.0301(15) 0.0039(11) 0.0220(14) 0.0051(12) C3 0.0492(19) 0.0285(14) 0.0280(15) 0.0011(11) 0.0256(14) -0.0029(12) C4 0.060(2) 0.0483(19) 0.0253(15) -0.0002(13) 0.0258(16) -0.0070(16) C5 0.075(3) 0.045(2) 0.036(2) -0.0005(16) 0.002(2) 0.002(2) C6 0.073(3) 0.088(4) 0.056(3) 0.004(3) 0.026(3) 0.007(3) C7 0.064(4) 0.119(5) 0.091(4) 0.011(4) 0.022(3) 0.015(3) C8 0.0380(17) 0.0371(16) 0.0348(16) 0.0001(13) 0.0212(14) -0.0035(13) C9 0.046(2) 0.0393(18) 0.047(2) -0.0074(15) 0.0244(17) -0.0030(15) C10 0.049(2) 0.080(3) 0.064(3) -0.032(2) 0.029(2) -0.015(2) C11 0.078(4) 0.144(6) 0.118(5) -0.093(5) 0.052(4) -0.035(4) C12 0.054(2) 0.0335(15) 0.0294(15) -0.0012(12) 0.0294(15) -0.0011(14) C13 0.068(2) 0.0293(15) 0.0366(16) 0.0034(12) 0.0387(17) 0.0002(14) C14 0.058(2) 0.0314(14) 0.0288(15) 0.0001(12) 0.0307(15) -0.0004(14) C15 0.062(2) 0.0425(17) 0.0434(17) 0.0013(13) 0.0350(16) 0.0040(15) C16 0.081(2) 0.0583(19) 0.0494(17) 0.0020(15) 0.0283(17) 0.0114(17) C17 0.076(3) 0.062(2) 0.047(2) 0.005(2) 0.035(2) 0.008(2) C18 0.090(4) 0.077(4) 0.053(3) 0.003(3) 0.028(3) 0.003(3) C19 0.075(3) 0.0366(16) 0.0267(15) -0.0005(13) 0.0330(17) -0.0004(16) C20 0.066(2) 0.0359(16) 0.0374(17) -0.0036(13) 0.0342(18) -0.0014(16) C21 0.075(3) 0.041(2) 0.057(2) 0.0043(17) 0.038(2) 0.0065(19) C22 0.091(3) 0.0343(19) 0.063(3) 0.0011(18) 0.042(3) 0.010(2) C23 0.052(2) 0.0287(14) 0.0330(15) -0.0020(11) 0.0301(15) -0.0053(13) C24 0.054(2) 0.0331(15) 0.0393(17) -0.0053(13) 0.0328(16) -0.0064(14) C25 0.047(2) 0.0373(16) 0.0280(15) 0.0014(12) 0.0213(15) 0.0015(14) C26 0.054(2) 0.0302(14) 0.0277(15) 0.0017(11) 0.0261(15) -0.0006(13) C27 0.0417(18) 0.0398(17) 0.0326(16) -0.0014(13) 0.0239(14) 0.0004(13) C28 0.058(2) 0.0434(19) 0.051(2) -0.0037(16) 0.0394(19) -0.0004(16) C29 0.069(3) 0.056(2) 0.059(2) -0.0086(19) 0.047(2) 0.003(2) C30 0.059(3) 0.075(3) 0.049(2) -0.0051(19) 0.042(2) -0.006(2) C31 0.068(3) 0.053(2) 0.060(2) -0.0011(18) 0.046(2) -0.0109(19) C32 0.057(2) 0.0396(18) 0.050(2) -0.0050(15) 0.0372(19) -0.0063(16) Cl1 0.088(4) 0.089(6) 0.097(5) 0.017(4) 0.067(4) 0.015(5) C33 0.063(9) 0.053(6) 0.109(7) 0.011(4) 0.064(6) 0.010(6) Cl2 0.062(3) 0.041(3) 0.101(4) -0.001(2) 0.051(3) 0.007(2) C18S 0.086(5) 0.085(5) 0.058(4) 0.001(4) 0.024(4) -0.004(4) C17S 0.080(3) 0.067(3) 0.052(2) 0.005(2) 0.029(2) 0.008(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 C1 P1 C23 94.87(15) C12 P1 C1 95.49(14) C12 P1 C23 93.64(15) C3 P2 C26 91.50(14) C14 P2 C3 93.81(15) C14 P2 C26 96.83(15) C1 N1 C4 125.7(3) C2 N1 C1 109.8(3) C2 N1 C4 124.5(3) C2 N2 C3 109.6(3) C2 N2 C8 126.1(3) C3 N2 C8 124.3(3) C12 N3 C15 126.8(3) C13 N3 C12 108.8(3) C13 N3 C15 124.3(3) C13 N4 C14 109.5(3) C13 N4 C19 125.4(3) C14 N4 C19 124.6(3) C24 N5 C25 113.0(3) C24 N5 C27 122.9(3) C25 N5 C27 123.8(3) N1 C1 P1 129.4(2) C3 C1 P1 123.2(2) C3 C1 N1 106.7(3) N1 C2 S1 127.3(2) N2 C2 S1 126.7(3) N2 C2 N1 106.1(3) N2 C3 P2 127.4(2) C1 C3 P2 123.4(2) C1 C3 N2 107.8(3) N1 C4 C5 113.0(3) C6 C5 C4 117.0(4) C5 C6 C7 118.7(5) N2 C8 C9 112.5(3) C8 C9 C10 111.8(3) C11 C10 C9 113.7(4) N3 C12 P1 128.6(3) C14 C12 P1 123.0(3) C14 C12 N3 108.3(3) N3 C13 S2 125.8(3) N4 C13 S2 127.9(3) N4 C13 N3 106.3(3) N4 C14 P2 128.5(3) C12 C14 P2 124.5(2) C12 C14 N4 107.0(3) N3 C15 C16 112.6(3) C17 C16 C15 121.0(5) C17S C16 C15 117.8(6) C16 C17 C18 115.0(7) N4 C19 C20 112.6(3) C21 C20 C19 113.0(3) C22 C21 C20 112.5(4) C24 C23 P1 106.4(2) C24 C23 C26 105.1(3) C26 C23 P1 117.5(2) O1 C24 N5 125.4(3) O1 C24 C23 126.7(3) N5 C24 C23 107.8(3) O2 C25 N5 124.9(3) O2 C25 C26 127.2(3) N5 C25 C26 107.9(3) C23 C26 P2 119.7(2) C25 C26 P2 106.1(2) C25 C26 C23 104.6(2) C28 C27 N5 119.2(3) C28 C27 C32 121.7(3) C32 C27 N5 119.0(3) C27 C28 C29 117.7(4) C30 C29 C28 121.2(4) C31 C30 C29 119.4(4) C30 C31 C32 121.0(4) C31 C32 C27 119.1(4) Cl2 C33 Cl1 115.2(7) C16 C17S C18S 117.8(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 C2 1.684(3) S2 C13 1.685(4) P1 C1 1.826(3) P1 C12 1.817(3) P1 C23 1.897(4) P2 C3 1.826(3) P2 C14 1.805(4) P2 C26 1.900(3) O1 C24 1.209(4) O2 C25 1.205(4) N1 C1 1.388(4) N1 C2 1.371(4) N1 C4 1.470(4) N2 C2 1.364(4) N2 C3 1.383(4) N2 C8 1.457(4) N3 C12 1.382(4) N3 C13 1.373(4) N3 C15 1.459(5) N4 C13 1.368(5) N4 C14 1.388(4) N4 C19 1.468(4) N5 C24 1.390(5) N5 C25 1.398(4) N5 C27 1.453(4) C1 C3 1.363(4) C4 C5 1.518(6) C5 C6 1.486(6) C6 C7 1.488(8) C8 C9 1.511(5) C9 C10 1.523(5) C10 C11 1.503(7) C12 C14 1.355(5) C15 C16 1.504(6) C16 C17 1.444(7) C16 C17S 1.426(8) C17 C18 1.501(8) C19 C20 1.525(5) C20 C21 1.524(6) C21 C22 1.514(6) C23 C24 1.504(4) C23 C26 1.532(5) C25 C26 1.512(5) C27 C28 1.380(5) C27 C32 1.383(5) C28 C29 1.397(5) C29 C30 1.379(6) C30 C31 1.374(6) C31 C32 1.375(5) Cl1 C33 1.741(9) C33 Cl2 1.711(9) C18S C17S 1.493(7)