#------------------------------------------------------------------------------ #$Date: 2014-10-01 10:25:02 +0300 (Wed, 01 Oct 2014) $ #$Revision: 124449 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/12/27/4122721.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_4122721 loop_ _publ_author_name 'Hwang, Jungwun' 'Li, Ping' 'Carroll, William R.' 'Smith, Mark D.' 'Pellechia, Perry J.' 'Shimizu, Ken D.' _publ_section_title ; Additivity of Substituent Effects in Aromatic Stacking Interactions. ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 140930072231000 _journal_paper_doi 10.1021/ja504378p _journal_year 2014 _chemical_formula_moiety 'C47 H33 N O4, 1.34(C D Cl3)' _chemical_formula_sum 'C48.34 H33 Cl4.02 D1.34 N O4' _chemical_formula_weight 836.90 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2014-01-08 _audit_creation_method ; Olex2 1.2 (compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736) ; _cell_angle_alpha 90 _cell_angle_beta 103.762(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.158(3) _cell_length_b 15.794(3) _cell_length_c 16.302(3) _cell_measurement_reflns_used 2827 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 20.727 _cell_measurement_theta_min 2.579 _cell_volume 4040.8(13) _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_collection 'SMART v5.631 (Bruker, 2003)' _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.923 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_unetI/netI 0.0869 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 41215 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 24.332 _diffrn_reflns_theta_min 1.821 _diffrn_source 'sealed tube' _diffrn_source_current 38.0 _diffrn_source_power 1.8 _diffrn_source_voltage 47.0 _exptl_absorpt_coefficient_mu 0.342 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.376 _exptl_crystal_description plate _exptl_crystal_F_000 1727 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.611 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.053 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 571 _refine_ls_number_reflns 6571 _refine_ls_number_restraints 60 _refine_ls_restrained_S_all 0.986 _refine_ls_R_factor_all 0.1180 _refine_ls_R_factor_gt 0.0658 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0862P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1564 _refine_ls_wR_factor_ref 0.1795 _reflns_number_gt 3760 _reflns_number_total 6571 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file ja504378p_si_002.cif _[local]_cod_data_source_block hjb55m _cod_original_cell_volume 4041.0(12) _cod_database_code 4122721 _diffrn_reflns_laue_measured_fraction_full 0.923 _diffrn_reflns_laue_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.923 _diffrn_reflns_point_group_measured_fraction_max 0.997 _shelxl_version_number 2013-4 _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 0.980 _shelx_estimated_absorpt_t_min 0.923 _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. Same fragment restrains {Cl1, Cl2, Cl3, C81} as {Cl4, Cl5, Cl6, C82} {Cl1, Cl2, Cl3, C81} as {Cl10, Cl11, Cl12, C84} {Cl1, Cl2, Cl3, C81} as {Cl7, Cl8, Cl9, C83} {Cl1, Cl2, Cl3, C81} as {Cl13, Cl14, Cl15, C85} 3. Others Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=Sof(C81)=Sof(D81)=FVAR(1) Sof(Cl4)=Sof(Cl5)=Sof(Cl6)=Sof(C82)=Sof(D82)=FVAR(2) Sof(Cl7)=Sof(Cl8)=Sof(Cl9)=Sof(C83)=Sof(D83)=FVAR(3) Sof(Cl13)=Sof(Cl14)=Sof(Cl15)=Sof(C85)=Sof(D85)=FVAR(4) Sof(Cl10)=Sof(Cl11)=Sof(Cl12)=Sof(C84)=Sof(D84)=FVAR(5) 4.a Ternary CH refined with riding coordinates: C3(H3), C6(H6), C81(D81), C82(D82), C84(D84), C83(D83), C85(D85) 4.b Aromatic/amide H refined with riding coordinates: C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C43(H43), C45(H45) 4.c Idealised Me refined as rotating group: C46(H46A,H46B,H46C), C47(H47A,H47B,H47C) ; _shelx_res_file ; TITL HJb55m in P2(1)/c CELL 0.71073 16.1584 15.7938 16.3024 90 103.762 90 ZERR 4 0.0027 0.0027 0.0027 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C D Cl H N O UNIT 193.35536 5.35536 16.06608 132 4 16 L.S. 5 PLAN 33 SIZE 0.24 0.22 0.06 TEMP -173(2) BOND $H REM colorless plate REM 2827 refl / 2th = 5.158 - 41.453 fmap 2 MORE -1 ACTA 50 CONF REM C:/frames/HJb55/work/HJb55m.hkl WGHT 0.086200 FVAR 0.18442 0.35301 0.24880 0.29749 0.13721 0.30233 O1 6 -0.035358 0.383493 0.419248 11.00000 0.02576 0.03815 = 0.03680 -0.00322 0.00052 0.00506 O2 6 0.285368 0.281406 0.593949 11.00000 0.02750 0.03894 = 0.02872 0.00139 -0.00071 0.00661 O3 6 0.271798 0.556417 0.508194 11.00000 0.03310 0.04016 = 0.04349 0.00903 -0.00598 -0.00613 O4 6 0.397180 0.496676 0.692705 11.00000 0.03906 0.05585 = 0.03059 -0.00722 0.00536 -0.02233 N1 5 0.297195 0.419498 0.555750 11.00000 0.02470 0.03396 = 0.02456 0.00343 -0.00355 0.00064 C1 1 0.040918 0.383188 0.434970 11.00000 0.02591 0.03689 = 0.01986 -0.01079 0.00039 0.00353 C2 1 0.105779 0.314580 0.476267 11.00000 0.02349 0.03232 = 0.02472 -0.00801 -0.00506 0.00527 C3 1 0.159085 0.370640 0.550150 11.00000 0.02360 0.03021 = 0.02402 -0.00085 0.00195 0.00426 AFIX 13 H3 4 0.135758 0.367298 0.601640 11.00000 -1.20000 AFIX 0 C4 1 0.252735 0.348670 0.570115 11.00000 0.02756 0.03700 = 0.01831 -0.00478 -0.00215 0.00299 C5 1 0.245304 0.488756 0.524626 11.00000 0.03310 0.03868 = 0.01922 -0.00268 -0.00451 -0.00331 C6 1 0.153961 0.461752 0.514739 11.00000 0.02533 0.03190 = 0.02153 -0.00280 -0.00167 0.00325 AFIX 13 H6 4 0.123695 0.500191 0.546679 11.00000 -1.20000 AFIX 0 C7 1 0.102872 0.452380 0.420053 11.00000 0.01923 0.03786 = 0.02089 -0.00325 0.00063 0.00495 C8 1 0.156443 0.395610 0.376956 11.00000 0.01840 0.05299 = 0.02302 -0.00802 -0.00562 0.00613 C9 1 0.156409 0.315400 0.407768 11.00000 0.01913 0.04826 = 0.02449 -0.01318 -0.00696 0.00486 C10 1 0.206096 0.249142 0.382381 11.00000 0.02420 0.06066 = 0.03356 -0.02283 -0.01212 0.01434 C11 1 0.210992 0.166731 0.416862 11.00000 0.02722 0.05883 = 0.05106 -0.02644 -0.01376 0.00967 AFIX 43 H11 4 0.182002 0.154075 0.459692 11.00000 -1.20000 AFIX 0 C12 1 0.257416 0.104577 0.388937 11.00000 0.04384 0.07321 = 0.06404 -0.03799 -0.02400 0.02786 AFIX 43 H12 4 0.259994 0.049140 0.412019 11.00000 -1.20000 AFIX 0 C13 1 0.300906 0.123469 0.326237 11.00000 0.06082 0.12395 = 0.04834 -0.04984 -0.01963 0.05743 AFIX 43 H13 4 0.332379 0.080480 0.306396 11.00000 -1.20000 AFIX 0 C14 1 0.298230 0.202978 0.293740 11.00000 0.04464 0.13282 = 0.03644 -0.03028 -0.01149 0.05066 AFIX 43 H14 4 0.328739 0.214624 0.251884 11.00000 -1.20000 AFIX 0 C15 1 0.251530 0.268693 0.320289 11.00000 0.02336 0.09961 = 0.02710 -0.03188 -0.01012 0.02021 C16 1 0.250241 0.354223 0.286153 11.00000 0.02237 0.10051 = 0.02906 -0.02068 -0.00602 0.00796 C17 1 0.294713 0.375944 0.224040 11.00000 0.02188 0.13595 = 0.03815 -0.04110 0.00604 -0.00888 AFIX 43 H17 4 0.325608 0.333254 0.203028 11.00000 -1.20000 AFIX 0 C18 1 0.294480 0.456379 0.193502 11.00000 0.03831 0.15039 = 0.04165 -0.03377 0.01515 -0.03762 AFIX 43 H18 4 0.323273 0.468824 0.150471 11.00000 -1.20000 AFIX 0 C19 1 0.252158 0.519602 0.225490 11.00000 0.03606 0.11288 = 0.04005 -0.01754 0.01109 -0.02858 AFIX 43 H19 4 0.253517 0.575922 0.205392 11.00000 -1.20000 AFIX 0 C20 1 0.208056 0.502224 0.286034 11.00000 0.02869 0.07572 = 0.03240 -0.00815 0.00199 -0.01256 AFIX 43 H20 4 0.179808 0.546630 0.307756 11.00000 -1.20000 AFIX 0 C21 1 0.204521 0.418759 0.316098 11.00000 0.01528 0.08007 = 0.02215 -0.01727 -0.00623 -0.00093 C22 1 0.067486 0.234422 0.501152 11.00000 0.02601 0.03037 = 0.04110 -0.00755 -0.00204 0.00704 C23 1 0.098448 0.195842 0.579560 11.00000 0.03001 0.02653 = 0.05520 -0.00108 -0.00964 0.00541 AFIX 43 H23 4 0.147026 0.218871 0.617677 11.00000 -1.20000 AFIX 0 C24 1 0.059795 0.125148 0.602444 11.00000 0.04109 0.03040 = 0.05134 0.00106 -0.00772 0.00502 AFIX 43 H24 4 0.082115 0.099627 0.655903 11.00000 -1.20000 AFIX 0 C25 1 -0.011501 0.090767 0.548161 11.00000 0.03929 0.03400 = 0.06006 -0.00351 0.00215 0.00149 AFIX 43 H25 4 -0.039509 0.043003 0.564525 11.00000 -1.20000 AFIX 0 C26 1 -0.041263 0.127872 0.468892 11.00000 0.03589 0.03600 = 0.05373 -0.01222 -0.00388 0.00084 AFIX 43 H26 4 -0.089052 0.103873 0.430447 11.00000 -1.20000 AFIX 0 C27 1 -0.002769 0.198466 0.445366 11.00000 0.03123 0.03633 = 0.04501 -0.00797 -0.00123 0.00378 AFIX 43 H27 4 -0.024007 0.222764 0.391127 11.00000 -1.20000 AFIX 0 C28 1 0.060722 0.529754 0.374576 11.00000 0.02218 0.04941 = 0.02749 0.00605 0.00542 0.00192 C29 1 0.000213 0.518879 0.297769 11.00000 0.02732 0.06034 = 0.02756 0.00188 0.00133 0.00370 AFIX 43 H29 4 -0.013855 0.463414 0.276424 11.00000 -1.20000 AFIX 0 C30 1 -0.038846 0.587548 0.253178 11.00000 0.02913 0.07274 = 0.02741 0.01303 -0.00365 0.00627 AFIX 43 H30 4 -0.079544 0.579429 0.201170 11.00000 -1.20000 AFIX 0 C31 1 -0.019016 0.668542 0.283882 11.00000 0.03367 0.05888 = 0.04325 0.02234 0.00656 0.00875 AFIX 43 H31 4 -0.046130 0.716062 0.253098 11.00000 -1.20000 AFIX 0 C32 1 0.040368 0.680137 0.359490 11.00000 0.03231 0.04716 = 0.04108 0.01424 0.00282 0.00106 AFIX 43 H32 4 0.054097 0.735714 0.380673 11.00000 -1.20000 AFIX 0 C33 1 0.079804 0.611028 0.404322 11.00000 0.03036 0.04282 = 0.02716 0.00811 0.00034 0.00255 AFIX 43 H33 4 0.120536 0.619541 0.456235 11.00000 -1.20000 AFIX 0 C34 1 0.387604 0.420204 0.566388 11.00000 0.02131 0.04369 = 0.02887 0.01051 -0.00261 -0.00072 C35 1 0.437947 0.462355 0.635053 11.00000 0.03108 0.04895 = 0.02727 0.00872 -0.00059 -0.00657 C36 1 0.525188 0.465366 0.644601 11.00000 0.03029 0.07268 = 0.03775 0.01275 -0.00544 -0.02029 AFIX 43 H36 4 0.560075 0.494927 0.690874 11.00000 -1.20000 AFIX 0 C37 1 0.561154 0.425353 0.586771 11.00000 0.02497 0.08283 = 0.04872 0.02478 0.00486 0.00026 AFIX 43 H37 4 0.621061 0.428001 0.592955 11.00000 -1.20000 AFIX 0 C38 1 0.511370 0.381362 0.519811 11.00000 0.03715 0.06653 = 0.03961 0.01322 0.01290 0.00859 AFIX 43 H38 4 0.537073 0.352520 0.481119 11.00000 -1.20000 AFIX 0 C39 1 0.424110 0.379435 0.509281 11.00000 0.03411 0.05686 = 0.02856 0.00635 0.00152 0.00313 AFIX 43 H39 4 0.389390 0.350062 0.462769 11.00000 -1.20000 AFIX 0 C40 1 0.432992 0.570201 0.734271 11.00000 0.03622 0.05282 = 0.03236 -0.00024 0.00188 -0.01998 C41 1 0.424255 0.645754 0.689941 11.00000 0.04167 0.06448 = 0.02668 -0.00025 0.00092 -0.01695 AFIX 43 H41 4 0.394765 0.647000 0.632112 11.00000 -1.20000 AFIX 0 C42 1 0.458542 0.719467 0.729988 11.00000 0.03590 0.05716 = 0.04064 -0.00153 0.00677 -0.01075 C43 1 0.499350 0.715474 0.815485 11.00000 0.03644 0.05134 = 0.04437 -0.01197 0.00438 -0.01315 AFIX 43 H43 4 0.522683 0.765802 0.843656 11.00000 -1.20000 AFIX 0 C44 1 0.506932 0.640431 0.860629 11.00000 0.03900 0.06345 = 0.03531 -0.00700 -0.00325 -0.01146 C45 1 0.473405 0.566574 0.818660 11.00000 0.04166 0.06041 = 0.03269 0.00374 -0.00399 -0.01612 AFIX 43 H45 4 0.478422 0.514194 0.848080 11.00000 -1.20000 AFIX 0 C46 1 0.451038 0.802596 0.682298 11.00000 0.06390 0.05457 = 0.05680 0.00277 0.01205 -0.00916 AFIX 137 H46A 4 0.451337 0.791677 0.623193 11.00000 -1.50000 H46B 4 0.499266 0.839163 0.707918 11.00000 -1.50000 H46C 4 0.397661 0.830690 0.684952 11.00000 -1.50000 AFIX 0 C47 1 0.551919 0.638433 0.953217 11.00000 0.06747 0.07804 = 0.03847 -0.00517 -0.01347 -0.02063 AFIX 137 H47A 4 0.607779 0.665654 0.961268 11.00000 -1.50000 H47B 4 0.559446 0.579541 0.972483 11.00000 -1.50000 H47C 4 0.517694 0.668807 0.985916 11.00000 -1.50000 AFIX 0 PART 1 CL1 3 0.225529 0.718105 0.610214 21.00000 0.02672 0.04692 = 0.03188 -0.00204 0.00698 0.00242 CL2 3 0.218409 0.573044 0.719735 21.00000 0.02864 0.03289 = 0.05488 0.00033 0.00608 0.00149 CL3 3 0.162147 0.737652 0.760491 21.00000 0.04439 0.04967 = 0.03148 0.00236 0.01267 0.01585 C81 1 0.230763 0.681223 0.713036 21.00000 0.03246 AFIX 13 D81 2 0.289709 0.694160 0.746562 21.00000 -1.20000 AFIX 0 SAME 0.02 0.04 Cl1 > C81 PART 0 PART 2 CL4 3 0.248592 0.757504 0.501980 31.00000 0.06698 CL5 3 0.344956 0.867872 0.424715 31.00000 0.05553 CL6 3 0.250339 0.936227 0.529388 31.00000 0.04670 C82 1 0.245814 0.857440 0.448670 31.00000 0.06873 AFIX 13 D82 2 0.196362 0.864033 0.398861 31.00000 -1.20000 AFIX 0 SAME 0.02 0.04 Cl1 > C81 PART 0 PART 3 CL10 3 0.195404 0.626223 0.760377 61.00000 0.08232 CL11 3 0.263945 0.788596 0.821027 61.00000 0.09372 CL12 3 0.276142 0.651791 0.936494 61.00000 0.12473 C84 1 0.275365 0.680438 0.835576 61.00000 0.05314 AFIX 13 D84 2 0.331753 0.664250 0.825001 61.00000 -1.20000 AFIX 0 SAME 0.02 0.04 Cl1 > C81 PART 0 PART 4 CL7 3 0.272889 0.775003 0.891199 41.00000 0.06830 CL8 3 0.211767 0.751154 0.714859 41.00000 0.11336 CL9 3 0.203783 0.614616 0.820947 41.00000 0.10158 C83 1 0.262996 0.699980 0.806711 41.00000 0.04640 AFIX 13 D83 2 0.320817 0.681080 0.802213 41.00000 -1.20000 AFIX 0 SAME 0.02 0.04 Cl1 > C81 PART 0 PART 5 CL13 3 0.233005 0.762566 0.574257 51.00000 0.05264 CL14 3 0.260640 0.922482 0.507163 51.00000 0.15604 CL15 3 0.325654 0.775579 0.447688 51.00000 0.06691 C85 1 0.238667 0.818076 0.480577 51.00000 0.09851 AFIX 13 D85 2 0.184644 0.812158 0.435825 51.00000 -1.20000 AFIX 0 HKLF 4 REM HJb55m in P2(1)/c REM R1 = 0.0658 for 3760 Fo > 4sig(Fo) and 0.1180 for all 6571 data REM 571 parameters refined using 60 restraints END WGHT 0.0862 0.0000 REM Highest difference peak 0.611, deepest hole -0.468, 1-sigma level 0.053 Q1 1 0.3226 0.8889 0.4634 11.00000 0.05 0.61 Q2 1 0.2340 0.7871 0.7703 11.00000 0.05 0.61 Q3 1 0.1815 0.6634 0.7320 11.00000 0.05 0.53 Q4 1 0.2078 0.5985 0.7819 11.00000 0.05 0.52 Q5 1 0.2776 0.7573 0.9367 11.00000 0.05 0.45 Q6 1 0.2732 0.7861 0.8601 11.00000 0.05 0.44 Q7 1 0.2047 0.8805 0.3700 11.00000 0.05 0.41 Q8 1 0.3412 0.8172 0.4395 11.00000 0.05 0.41 Q9 1 0.2426 0.6734 0.9145 11.00000 0.05 0.33 Q10 1 0.2068 0.7199 0.6960 11.00000 0.05 0.30 Q11 1 0.3530 0.8737 0.4082 11.00000 0.05 0.26 Q12 1 0.2318 0.7659 0.5321 11.00000 0.05 0.25 Q13 1 0.2375 0.9172 0.4850 11.00000 0.05 0.24 Q14 1 0.2605 0.0995 0.3416 11.00000 0.05 0.20 Q15 1 0.2162 0.9738 0.5176 11.00000 0.05 0.20 Q16 1 0.4521 0.8567 0.7192 11.00000 0.05 0.19 Q17 1 0.2417 0.8234 0.4985 11.00000 0.05 0.19 Q18 1 0.5771 0.6993 0.9825 11.00000 0.05 0.19 Q19 1 0.2839 0.4756 0.1945 11.00000 0.05 0.19 Q20 1 0.3198 0.4167 0.2361 11.00000 0.05 0.18 Q21 1 0.2977 0.1569 0.3224 11.00000 0.05 0.18 Q22 1 0.2595 0.6816 0.7175 11.00000 0.05 0.17 Q23 1 0.1985 0.7403 0.8176 11.00000 0.05 0.17 Q24 1 0.3098 0.2265 0.2890 11.00000 0.05 0.17 Q25 1 0.2814 0.1225 0.3803 11.00000 0.05 0.17 Q26 1 0.2166 0.6161 0.7076 11.00000 0.05 0.17 Q27 1 0.0756 0.3411 0.4517 11.00000 0.05 0.16 Q28 1 -0.0620 0.4554 0.4296 11.00000 0.05 0.16 Q29 1 0.1957 0.3619 0.4111 11.00000 0.05 0.16 Q30 1 0.5368 0.6014 0.8378 11.00000 0.05 0.16 Q31 1 0.1394 0.4387 0.4071 11.00000 0.05 0.15 Q32 1 0.3964 0.7922 0.6406 11.00000 0.05 0.15 Q33 1 0.1946 0.2800 0.4124 11.00000 0.05 0.15 ; _shelx_res_checksum 71624 _shelx_hkl_file ; 0 0 -1 -0.01 0.31 0 0 -1 0.04 0.36 0 0 -1 -0.13 0.24 0 0 1 -0.02 0.30 0 0 -2 18.44 2.20 0 0 -2 18.80 1.42 0 0 2 18.71 1.08 0 0 2 19.55 1.91 0 0 -3 0.54 1.35 0 0 -3 0.16 0.95 0 0 3 0.21 0.71 0 0 3 0.70 1.30 0 0 -4 193.21 5.49 0 0 4 202.85 4.72 0 0 4 194.09 7.28 0 0 -5 1.79 1.95 0 0 -5 -0.67 1.03 0 0 5 -0.44 0.92 0 0 5 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2 52.60 4.43 0 7 -2 52.12 5.66 0 7 -2 58.80 6.27 0 7 2 57.99 5.76 0 7 2 57.72 6.13 0 -7 -3 4.29 2.86 0 -7 -3 4.26 2.69 0 -7 3 4.86 2.92 0 -7 3 7.44 2.25 0 7 -3 5.60 2.94 0 7 -3 3.57 2.56 0 7 3 6.43 2.77 0 7 3 6.30 3.11 0 -7 -4 98.97 8.19 0 -7 -4 101.07 8.19 0 -7 4 102.28 8.62 0 -7 4 107.87 5.66 0 7 -4 100.82 7.71 0 7 -4 91.79 7.60 0 7 4 104.49 7.47 0 7 4 104.74 8.29 0 -7 -5 232.63 12.76 0 -7 -5 239.07 12.92 0 -7 5 222.95 12.73 0 -7 5 238.35 8.25 0 7 -5 257.23 11.98 0 7 -5 218.29 11.48 0 7 5 222.59 10.54 0 7 5 216.16 11.68 0 -7 -6 92.05 8.68 0 -7 -6 85.11 8.26 0 -7 6 87.79 8.41 0 -7 6 101.78 5.69 0 7 -6 93.52 7.81 0 7 6 91.47 7.02 0 7 6 103.47 8.36 0 -7 -7 -3.02 1.82 0 -7 -7 -1.75 1.80 0 -7 7 0.30 2.66 0 -7 7 1.44 1.69 0 7 -7 -1.02 1.74 0 7 7 1.40 1.94 0 7 7 -1.96 1.76 0 -7 -8 8.90 4.03 0 -7 -8 6.88 3.89 0 -7 8 5.02 3.62 0 -7 8 5.78 2.49 0 7 -8 6.77 3.08 0 7 8 6.18 2.81 0 7 8 6.27 3.26 0 -7 -9 14.88 5.14 0 -7 -9 22.48 5.97 0 -7 9 10.25 4.57 0 -7 9 13.93 3.36 0 7 -9 12.87 4.22 0 7 9 16.21 4.14 0 7 9 16.26 4.49 0 -7 -10 0.75 2.63 0 -7 10 -0.77 2.94 0 -7 10 0.58 2.20 0 7 -10 -0.32 2.04 0 7 10 -0.19 2.08 0 7 10 -0.40 2.30 0 7 10 -1.62 2.09 0 -7 -11 5.30 4.36 0 -7 11 1.75 3.38 0 7 -11 3.49 2.94 0 7 11 2.34 2.27 0 7 11 3.88 3.60 0 7 11 6.34 3.47 0 -7 -12 2.14 3.50 0 -7 12 1.24 3.47 0 7 -12 1.28 2.69 0 7 12 3.00 2.47 0 7 12 -0.69 2.60 0 7 12 -0.06 2.51 0 -7 -13 8.88 5.62 0 -7 13 11.39 5.64 0 7 13 9.00 3.56 0 7 13 5.45 3.98 0 -7 -14 27.82 8.40 0 -7 14 20.85 7.38 0 7 14 18.31 6.62 0 -7 -15 16.52 6.91 0 -7 15 10.25 5.69 0 7 15 12.11 5.74 0 -7 -16 4.90 5.26 0 -7 16 -2.79 3.88 0 7 16 6.07 5.20 0 -8 0 104.58 8.54 0 -8 0 112.71 7.39 0 8 0 97.45 7.91 0 8 0 107.65 8.80 0 -8 -1 27.49 5.28 0 -8 -1 31.69 4.85 0 -8 1 22.30 4.99 0 -8 1 34.78 4.45 0 8 -1 32.97 5.37 0 8 -1 30.20 5.52 0 8 1 21.28 4.49 0 8 1 25.32 5.24 0 -8 -2 1.88 2.66 0 -8 -2 3.47 2.53 0 -8 2 2.53 2.49 0 -8 2 2.32 1.96 0 8 -2 3.17 2.61 0 8 -2 2.10 2.62 0 8 2 1.63 2.22 0 8 2 2.71 2.83 0 -8 -3 29.66 5.60 0 -8 -3 32.86 5.53 0 -8 3 28.03 5.68 0 -8 3 30.72 3.72 0 8 -3 25.03 4.89 0 8 -3 28.77 5.43 0 8 3 28.13 4.90 0 8 3 31.89 5.75 0 -8 -4 -0.91 1.83 0 -8 -4 2.46 2.51 0 -8 4 1.29 2.64 0 -8 4 -0.43 1.41 0 8 -4 -0.29 1.90 0 8 -4 0.88 2.30 0 8 4 1.26 2.02 0 8 4 0.88 2.36 0 -8 -5 6.12 3.33 0 -8 -5 8.31 3.64 0 -8 5 8.79 3.78 0 -8 5 12.25 2.73 0 8 -5 9.33 3.58 0 8 -5 10.38 3.92 0 8 5 9.09 3.24 0 8 5 8.47 3.70 0 -8 -6 1.94 2.61 0 -8 -6 1.23 2.60 0 -8 6 0.61 2.86 0 -8 6 2.61 1.69 0 8 -6 2.67 2.67 0 8 -6 0.99 2.25 0 8 6 1.49 2.23 0 8 6 2.59 2.94 0 -8 -7 1.12 2.69 0 -8 -7 4.09 3.11 0 -8 7 2.52 2.94 0 -8 7 4.39 2.08 0 8 -7 3.13 2.77 0 8 7 0.91 2.12 0 8 7 2.91 3.08 0 -8 -8 7.82 4.03 0 -8 -8 4.10 3.50 0 -8 8 4.85 3.71 0 -8 8 5.34 2.46 0 8 -8 3.88 2.97 0 8 8 5.75 2.98 0 8 8 6.67 3.69 0 -8 -9 15.27 5.24 0 -8 -9 12.89 5.05 0 -8 9 10.33 4.73 0 8 -9 8.91 3.84 0 8 9 18.08 4.61 0 8 9 20.53 5.51 0 -8 -10 0.71 3.42 0 -8 10 1.36 3.36 0 8 -10 0.97 2.32 0 8 10 0.76 1.84 0 8 10 -0.07 2.73 0 -8 -11 4.62 4.07 0 -8 11 8.02 4.65 0 8 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19.46 5.09 0 9 13 16.50 6.43 0 -9 -14 1.64 4.40 0 -9 14 1.48 4.30 0 9 14 1.37 2.91 0 9 14 3.25 3.97 0 -9 -15 -0.52 4.72 0 -9 15 -0.04 4.23 0 9 15 -0.86 3.58 0 -10 0 1.92 2.64 0 -10 0 4.62 2.81 0 10 0 6.20 3.36 0 10 0 6.05 3.57 0 -10 -1 -2.11 1.37 0 -10 -1 1.79 2.38 0 -10 1 0.32 2.39 0 -10 1 0.32 1.74 0 10 -1 -0.52 2.22 0 10 -1 0.81 2.44 0 10 1 1.54 2.55 0 10 1 -1.92 1.93 0 -10 -2 5.25 3.32 0 -10 -2 18.05 4.77 0 -10 2 5.59 3.49 0 -10 2 11.45 3.42 0 10 -2 14.33 4.60 0 10 -2 13.19 4.68 0 10 2 8.97 3.73 0 10 2 10.10 4.20 0 -10 -3 2.03 2.67 0 -10 -3 5.12 3.17 0 -10 3 4.28 3.28 0 -10 3 4.53 2.45 0 10 -3 2.17 2.87 0 10 -3 5.54 3.37 0 10 3 2.33 2.72 0 10 3 2.70 2.93 0 -10 -4 16.67 5.26 0 -10 -4 20.80 5.47 0 -10 4 11.22 4.53 0 -10 4 16.05 3.46 0 10 -4 16.35 4.97 0 10 -4 17.42 5.09 0 10 4 16.83 4.78 0 10 4 21.50 5.81 0 -10 -5 9.03 4.31 0 -10 -5 8.14 4.11 0 -10 5 7.59 4.23 0 -10 5 7.63 2.74 0 10 -5 7.13 3.78 0 10 -5 6.64 3.81 0 10 5 4.20 3.11 0 10 5 10.87 4.62 0 -10 -6 3.17 3.40 0 -10 -6 1.25 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2.77 -2 5 10 15.66 4.28 2 -5 -10 16.20 5.01 2 -5 -10 13.87 4.84 2 5 -10 16.31 4.38 -2 -5 9 0.16 2.24 -2 -5 9 -3.41 2.13 -2 -5 9 -0.64 1.36 -2 5 9 0.74 1.37 -2 5 9 0.47 2.05 2 -5 -9 -0.42 2.16 2 -5 -9 -0.82 1.95 2 5 -9 -0.87 1.86 -2 -5 8 5.33 2.86 -2 -5 8 4.18 3.08 -2 -5 8 4.01 1.72 -2 5 8 4.09 1.82 -2 5 8 3.54 2.54 2 -5 -8 4.12 2.89 2 -5 -8 4.75 2.91 2 5 -8 1.24 2.16 -2 -5 7 7.35 2.96 -2 -5 7 8.07 3.53 -2 -5 7 5.52 1.67 -2 5 7 8.00 2.25 -2 5 7 8.05 3.21 2 -5 -7 7.73 3.40 2 -5 -7 8.92 3.59 2 5 -7 5.92 2.81 -2 -5 6 0.65 2.20 -2 5 6 2.72 1.66 -2 5 6 4.00 2.47 2 -5 -6 1.63 2.22 2 -5 -6 3.77 2.66 2 5 -6 1.47 2.04 -2 -5 5 11.94 3.70 -2 5 5 13.34 2.63 -2 5 5 13.66 2.05 -2 5 5 14.11 3.85 2 -5 -5 10.42 3.33 2 -5 -5 17.25 4.32 2 5 -5 10.85 3.38 -2 -5 4 40.16 5.31 -2 5 4 45.43 4.09 -2 5 4 45.96 2.72 -2 5 4 47.79 5.41 2 -5 -4 45.65 4.93 2 -5 -4 48.54 5.37 2 5 -4 41.50 4.93 -2 -5 3 0.90 1.98 -2 -5 3 0.49 0.87 -2 5 3 -0.22 1.38 -2 5 3 1.36 0.97 -2 5 3 1.36 1.95 2 -5 -3 0.25 1.70 2 -5 -3 0.85 1.97 2 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2.74 3.40 -4 8 -6 5.60 3.42 -4 8 -6 4.70 2.80 4 -8 6 4.17 3.28 4 -8 6 6.05 3.19 4 8 6 2.97 3.03 4 8 6 4.90 3.14 -4 -8 -7 5.35 2.70 -4 -8 -7 3.79 3.84 -4 8 -7 2.68 3.02 -4 8 -7 6.04 3.18 4 -8 7 4.89 3.63 4 -8 7 3.28 3.11 4 8 7 4.48 3.49 4 8 7 4.70 3.31 -4 -8 -8 9.73 3.41 -4 -8 -8 9.74 4.55 -4 8 -8 15.79 5.83 -4 8 -8 11.56 3.94 4 -8 8 12.79 5.09 4 -8 8 15.91 4.70 4 8 8 14.06 5.73 4 8 8 20.11 5.14 -4 -8 -9 31.50 5.19 -4 -8 -9 41.23 8.64 -4 8 -9 34.65 5.65 4 -8 9 31.42 7.63 4 -8 9 38.01 6.90 4 8 9 36.53 8.35 4 8 9 40.44 6.52 -4 -8 -10 47.93 9.49 4 -8 10 36.10 8.64 4 -8 10 44.36 7.40 4 8 10 28.74 7.68 -4 -8 -11 2.41 3.46 4 -8 11 8.09 5.44 4 -8 11 2.34 3.56 4 8 11 1.16 3.47 -4 -8 -12 8.80 5.02 4 -8 12 10.12 5.84 4 8 12 14.57 6.21 -4 -8 -13 1.14 3.68 4 -8 13 -0.45 4.19 4 8 13 2.15 3.83 -4 -8 -14 -4.11 2.70 4 -8 14 5.62 5.74 4 8 14 -0.42 3.16 -4 -8 -15 3.58 4.54 4 -8 15 -0.92 4.13 4 8 15 -0.30 3.55 -4 -9 16 8.74 5.89 -4 9 16 3.46 2.89 4 -9 -16 4.21 5.43 -4 -9 15 2.16 3.98 -4 9 15 1.35 2.26 -4 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29.20 5.34 5 4 -6 22.33 2.25 5 4 -6 19.70 4.59 -5 -4 5 35.95 5.00 -5 4 5 27.84 3.92 5 -4 -5 33.67 3.73 5 -4 -5 31.66 5.24 5 -4 -5 29.05 5.22 5 4 -5 34.28 2.65 5 4 -5 33.50 5.40 -5 -4 4 0.05 1.87 -5 4 4 1.19 1.70 5 -4 -4 -0.28 1.35 5 -4 -4 0.68 1.85 5 4 -4 0.05 1.04 5 4 -4 0.07 1.94 -5 -4 3 4.20 2.49 -5 -4 3 6.93 2.92 -5 4 3 4.39 2.00 -5 4 3 5.65 2.34 -5 4 3 2.13 2.11 5 -4 -3 6.67 2.03 5 -4 -3 7.59 3.05 5 4 -3 5.11 1.80 5 4 -3 6.76 2.82 -5 -4 2 132.49 8.06 -5 -4 2 127.38 7.39 -5 4 2 117.18 6.90 -5 4 2 124.27 7.14 -5 4 2 121.55 7.93 5 -4 -2 129.55 5.56 5 -4 -2 129.76 8.40 5 4 -2 118.66 5.91 5 4 -2 126.28 8.23 -5 -4 1 1.93 2.05 -5 -4 1 2.66 2.12 -5 4 1 0.73 1.71 -5 4 1 2.79 2.13 -5 4 1 1.56 1.95 5 -4 -1 1.11 1.52 5 -4 -1 2.10 2.38 5 4 -1 2.71 1.84 5 4 -1 2.03 2.03 -5 -4 0 0.47 1.73 -5 -4 0 0.19 1.85 -5 4 0 1.17 1.90 -5 4 0 0.22 1.89 -5 4 0 1.79 1.87 5 -4 0 -0.30 1.38 5 -4 0 1.23 2.06 5 4 0 0.26 1.56 5 4 0 1.36 1.91 -5 -4 -1 34.65 4.52 -5 -4 -1 36.28 4.87 -5 4 -1 31.86 4.63 -5 4 -1 34.73 4.87 -5 4 -1 32.32 4.30 5 -4 1 32.68 3.81 5 -4 1 39.74 5.28 5 4 1 37.01 4.78 5 4 1 31.85 4.39 -5 -4 -2 -0.08 1.79 -5 -4 -2 1.24 1.93 -5 4 -2 -0.22 1.68 -5 4 -2 -0.09 2.07 -5 4 -2 -0.40 1.37 5 -4 2 0.60 1.82 5 -4 2 0.23 1.86 5 4 2 0.13 1.65 5 4 2 1.35 1.95 -5 -4 -3 19.39 3.87 -5 -4 -3 15.77 4.16 -5 4 -3 10.89 3.45 -5 4 -3 16.49 4.24 -5 4 -3 14.54 2.97 5 -4 3 13.56 3.49 5 -4 3 17.81 4.32 5 4 3 13.41 3.93 5 4 3 12.18 3.01 -5 -4 -4 3.21 2.36 -5 -4 -4 2.02 2.41 -5 4 -4 3.56 2.45 -5 4 -4 5.92 3.05 -5 4 -4 4.01 2.07 5 -4 4 6.30 2.90 5 -4 4 4.78 2.78 5 4 4 2.72 2.57 5 4 4 4.79 2.28 -5 -4 -5 35.66 5.15 -5 -4 -5 38.03 6.22 -5 4 -5 43.41 5.84 -5 4 -5 40.52 6.42 -5 4 -5 34.83 3.78 5 -4 5 35.42 5.62 5 -4 5 35.41 5.86 5 4 5 31.32 5.89 5 4 5 38.66 4.18 -5 -4 -6 0.97 2.32 -5 -4 -6 3.02 2.85 -5 4 -6 3.55 2.66 -5 4 -6 2.03 2.95 -5 4 -6 1.96 1.72 5 -4 6 2.58 2.79 5 -4 6 2.15 2.74 5 4 6 3.86 2.98 5 4 6 3.48 2.00 -5 -4 -7 7.84 3.57 -5 -4 -7 7.98 3.73 -5 4 -7 5.85 3.41 -5 4 -7 6.51 2.04 5 -4 7 4.76 3.33 5 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3.32 5 -5 12 3.47 4.02 5 5 12 3.30 3.67 -5 -5 -13 17.58 6.16 -5 -5 -13 13.02 5.91 5 -5 13 10.13 6.23 5 -5 13 17.07 5.70 5 5 13 20.14 7.08 -5 -5 -14 7.20 4.76 5 -5 14 1.56 5.01 5 -5 14 4.54 4.50 5 5 14 -0.01 2.83 -5 -5 -15 1.63 4.12 5 -5 15 -0.25 4.52 5 -5 15 6.10 4.75 5 5 15 -3.06 2.37 -5 -6 17 29.33 8.84 -5 6 17 32.58 8.96 5 -6 -17 26.35 8.54 -5 -6 16 0.68 3.71 -5 6 16 2.69 1.63 -5 6 16 7.00 3.81 5 -6 -16 2.61 4.49 5 -6 -16 0.84 3.87 5 6 -16 1.99 3.42 -5 -6 15 1.00 3.50 -5 6 15 2.40 1.65 -5 6 15 0.54 2.93 5 -6 -15 -0.68 3.68 5 -6 -15 -2.51 2.77 5 6 -15 0.35 3.46 -5 -6 14 1.08 3.21 -5 6 14 1.43 1.43 -5 6 14 -0.94 2.54 5 -6 -14 0.60 3.53 5 -6 -14 4.03 4.23 5 6 -14 3.65 3.47 -5 -6 13 58.64 9.94 -5 6 13 48.06 4.14 -5 6 13 61.09 9.33 5 -6 -13 55.23 9.09 5 -6 -13 53.74 9.79 5 6 -13 36.35 7.53 -5 -6 12 5.81 4.24 -5 6 12 5.28 1.93 -5 6 12 5.73 3.76 5 -6 -12 8.28 4.29 5 -6 -12 3.99 3.94 5 6 -12 3.36 3.34 -5 -6 11 20.37 6.16 -5 6 11 12.05 2.69 -5 6 11 14.41 4.28 -5 6 11 16.67 5.40 5 -6 -11 15.84 5.02 5 -6 -11 13.35 5.12 5 6 -11 11.35 4.42 -5 -6 10 3.19 3.51 -5 6 10 1.98 1.81 -5 6 10 2.46 2.66 -5 6 10 2.67 3.02 5 -6 -10 3.33 2.81 5 -6 -10 1.52 2.96 5 6 -10 3.10 2.89 -5 -6 9 0.34 2.83 -5 6 9 1.22 1.48 -5 6 9 1.70 2.29 -5 6 9 0.32 2.06 5 -6 -9 1.01 2.32 5 -6 -9 2.47 2.86 5 6 -9 0.68 2.26 -5 -6 8 19.00 5.34 -5 6 8 16.38 3.07 -5 6 8 16.66 3.48 -5 6 8 16.45 5.00 5 -6 -8 16.46 4.27 5 -6 -8 14.62 4.73 5 6 -8 15.94 4.86 -5 -6 7 133.22 10.01 -5 6 7 123.80 6.99 -5 6 7 130.44 7.29 -5 6 7 126.68 10.09 5 -6 -7 125.84 8.62 5 -6 -7 117.98 9.89 5 6 -7 110.77 9.35 -5 -6 6 19.48 4.74 -5 6 6 15.23 3.20 -5 6 6 16.23 3.16 -5 6 6 18.56 5.01 5 -6 -6 14.47 3.67 5 -6 -6 11.30 4.08 5 6 -6 14.24 4.39 -5 -6 5 85.69 7.82 -5 6 5 81.21 6.12 -5 6 5 88.11 5.83 -5 6 5 87.07 8.29 5 -6 -5 81.56 6.44 5 -6 -5 92.57 8.46 5 6 -5 80.90 7.92 -5 -6 4 16.57 4.38 -5 6 4 20.30 3.81 -5 6 4 23.32 3.49 -5 6 4 20.58 5.03 5 -6 -4 20.04 3.69 5 -6 -4 22.85 5.02 5 6 -4 19.41 2.23 5 6 -4 18.07 4.69 -5 -6 3 77.26 6.90 -5 -6 3 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4.43 -6 -5 -6 71.48 7.27 -6 -5 -6 72.75 8.15 -6 5 -6 77.26 7.95 -6 5 -6 68.40 8.27 -6 5 -6 67.56 5.52 6 -5 6 76.75 8.06 6 -5 6 69.94 7.86 6 5 6 62.83 7.81 6 5 6 67.20 5.79 -6 -5 -7 125.63 9.69 -6 -5 -7 114.05 10.69 -6 5 -7 129.32 11.61 -6 5 -7 116.69 6.65 6 -5 7 100.13 9.71 6 -5 7 122.22 10.39 6 5 7 101.99 10.24 6 5 7 125.99 7.47 -6 -5 -8 11.48 4.39 -6 -5 -8 8.95 4.57 -6 5 -8 10.56 4.66 6 -5 8 12.28 5.01 6 -5 8 10.69 4.66 6 5 8 9.24 4.19 -6 -5 -9 22.69 5.74 -6 -5 -9 21.58 6.36 -6 5 -9 25.25 6.96 6 -5 9 26.54 7.10 6 -5 9 18.39 5.74 6 5 9 21.07 6.39 -6 -5 -10 19.12 5.64 -6 -5 -10 21.89 6.57 -6 5 -10 14.68 5.52 6 -5 10 21.66 6.86 6 -5 10 18.53 5.82 6 5 10 27.71 7.61 -6 -5 -11 -1.65 2.89 -6 -5 -11 -1.60 2.84 -6 5 -11 3.52 4.32 6 -5 11 1.91 3.67 6 -5 11 1.46 3.33 6 5 11 1.44 3.30 -6 -5 -12 10.85 5.31 -6 -5 -12 8.25 5.18 -6 5 -12 6.46 5.00 6 -5 12 8.84 5.43 6 -5 12 14.53 5.48 6 5 12 5.75 4.35 -6 -5 -13 11.93 5.37 -6 -5 -13 11.25 5.52 6 -5 13 7.40 6.46 6 -5 13 9.01 4.69 6 5 13 11.42 5.52 -6 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48.95 8.45 -8 4 -6 38.12 4.16 8 -4 6 46.29 7.10 8 -4 6 48.19 8.34 8 4 6 48.96 8.77 8 4 6 43.24 4.80 -8 -4 -7 64.39 8.79 -8 -4 -7 64.15 9.10 -8 4 -7 45.82 8.61 8 -4 7 47.55 7.76 8 -4 7 48.23 8.66 8 4 7 49.01 9.39 -8 -4 -8 64.45 9.10 -8 -4 -8 69.90 10.03 -8 4 -8 61.19 9.96 8 -4 8 64.78 9.13 8 -4 8 75.91 10.44 8 4 8 88.92 11.06 -8 -4 -9 11.77 5.25 -8 -4 -9 11.89 5.20 -8 4 -9 7.28 4.67 8 -4 9 9.49 5.32 8 -4 9 13.19 5.39 8 4 9 9.45 4.77 -8 -4 -10 0.21 3.64 -8 -4 -10 1.12 3.03 -8 4 -10 1.45 3.94 8 -4 10 4.58 4.22 8 -4 10 0.33 3.44 8 4 10 1.35 2.89 -8 -4 -11 8.90 5.08 -8 -4 -11 11.44 5.39 -8 4 -11 7.54 5.21 8 -4 11 13.07 5.98 8 -4 11 6.31 4.52 8 4 11 16.82 6.81 -8 -4 -12 7.92 5.43 -8 -4 -12 8.68 5.21 -8 4 -12 5.55 5.37 8 -4 12 5.19 5.05 8 -4 12 9.41 5.21 8 4 12 7.27 4.77 -8 -4 -13 0.96 4.10 -8 -4 -13 2.04 4.08 -8 4 -13 -2.36 3.40 8 -4 13 0.03 4.38 8 -4 13 2.62 4.19 8 4 13 -1.02 3.19 -8 -4 -14 2.43 4.76 -8 -4 -14 0.33 3.73 -8 4 -14 3.61 5.35 8 -4 14 3.12 5.05 8 -4 14 1.13 3.99 8 4 14 2.58 3.86 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6.82 3.28 -8 6 3 4.18 3.04 8 -6 -3 9.02 2.41 8 -6 -3 6.11 3.51 8 6 -3 7.27 2.68 8 6 -3 5.99 3.74 -8 -6 2 22.97 5.24 -8 -6 2 26.06 5.26 -8 6 2 20.90 4.87 -8 6 2 24.81 5.15 -8 6 2 21.08 5.24 8 -6 -2 23.09 3.31 8 -6 -2 21.61 5.48 8 6 -2 18.92 4.03 8 6 -2 19.49 5.33 -8 -6 1 3.44 2.78 -8 -6 1 7.71 3.47 -8 6 1 6.74 3.19 -8 6 1 3.37 2.90 -8 6 1 6.39 3.28 8 -6 -1 6.26 2.43 8 -6 -1 8.46 3.90 8 6 -1 6.46 3.01 8 6 -1 6.81 3.32 -8 -6 0 56.09 6.75 -8 -6 0 52.34 6.42 -8 6 0 41.40 6.51 -8 6 0 45.95 6.68 -8 6 0 45.81 6.56 8 -6 0 45.14 4.77 8 -6 0 56.81 7.99 8 6 0 43.83 6.18 8 6 0 48.22 6.89 -8 -6 -1 41.75 6.29 -8 -6 -1 41.51 6.47 -8 6 -1 37.96 6.61 -8 6 -1 40.45 6.66 -8 6 -1 39.90 6.15 8 -6 1 39.49 4.74 8 -6 1 48.05 7.61 8 6 1 41.97 6.53 8 6 1 51.89 6.93 -8 -6 -2 4.36 3.01 -8 -6 -2 5.51 3.42 -8 6 -2 4.03 3.12 -8 6 -2 5.33 3.45 -8 6 -2 3.33 2.55 8 -6 2 6.51 3.01 8 -6 2 7.80 3.79 8 6 2 4.75 3.28 8 6 2 1.52 2.49 -8 -6 -3 69.01 7.45 -8 -6 -3 78.59 8.38 -8 6 -3 70.56 8.07 -8 6 -3 63.95 8.50 -8 6 -3 71.30 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1.42 3.84 -8 -6 -11 1.02 3.21 -8 6 -11 1.30 3.69 8 -6 11 0.96 4.22 8 -6 11 3.90 3.88 8 6 11 0.91 3.52 -8 -6 -12 6.11 5.11 -8 -6 -12 1.34 3.67 -8 6 -12 0.80 3.64 8 -6 12 -4.13 3.43 8 -6 12 -1.97 3.33 8 6 12 2.53 3.25 -8 -6 -13 4.54 5.26 -8 -6 -13 7.97 5.36 -8 6 -13 3.25 5.38 8 -6 13 0.06 4.76 8 -6 13 4.65 4.52 8 6 13 0.82 3.47 -8 -7 16 -1.48 3.82 -8 7 16 0.15 1.64 -8 7 16 1.05 3.32 8 -7 -16 0.58 3.72 8 -7 -16 -1.63 3.90 8 7 -16 -2.17 3.67 -8 -7 15 17.77 6.70 -8 7 15 10.48 2.93 -8 7 15 6.42 4.68 8 -7 -15 12.39 5.86 8 -7 -15 18.24 7.20 8 7 -15 15.96 6.66 -8 -7 14 12.06 5.61 -8 7 14 4.70 2.23 -8 7 14 8.64 5.05 8 -7 -14 5.83 4.60 8 -7 -14 8.83 5.52 8 7 -14 7.92 5.38 -8 -7 13 14.64 5.67 -8 7 13 11.16 3.08 -8 7 13 12.88 5.67 8 -7 -13 11.72 4.86 8 -7 -13 11.41 5.92 8 7 -13 16.95 6.27 -8 -7 12 5.99 4.20 -8 7 12 4.60 2.41 -8 7 12 3.74 3.88 8 -7 -12 2.72 3.15 8 -7 -12 6.42 4.64 8 7 -12 -0.03 3.48 -8 -7 11 9.69 5.11 -8 7 11 11.08 3.30 -8 7 11 14.16 4.55 -8 7 11 14.68 5.55 8 -7 -11 10.99 5.41 8 7 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2.12 4.44 17 2 -1 4.73 3.85 -17 -2 0 0.90 4.45 -17 2 0 1.83 3.87 17 -2 0 -0.06 4.43 17 2 0 -1.54 3.72 -17 -2 -1 3.44 4.50 -17 2 -1 2.76 4.22 17 -2 1 3.00 5.03 17 2 1 0.95 4.34 -17 -2 -2 4.33 5.80 -17 2 -2 1.37 5.58 17 -2 2 3.96 5.22 17 2 2 2.65 5.12 -17 -2 -3 -4.43 4.34 -17 2 -3 -3.36 2.79 17 -2 3 3.57 5.35 17 2 3 -2.37 4.12 -17 -3 11 1.72 4.49 -17 3 11 9.00 5.29 17 -3 -11 -2.78 3.67 17 -3 -11 5.92 4.68 17 3 -11 4.01 4.33 -17 -3 10 1.95 4.30 -17 3 10 0.56 4.08 17 -3 -10 4.52 5.05 17 -3 -10 3.49 4.59 17 3 -10 2.04 4.26 -17 -3 9 2.97 4.12 -17 3 9 6.13 4.84 17 -3 -9 -0.72 4.25 17 -3 -9 2.96 4.04 17 3 -9 1.73 3.96 -17 -3 8 4.08 4.38 -17 3 8 -0.40 3.32 17 -3 -8 -3.62 3.12 17 -3 -8 -1.92 2.98 17 3 -8 1.65 3.87 17 3 -8 4.14 4.37 -17 -3 7 7.79 5.29 -17 3 7 4.98 4.80 17 -3 -7 5.61 5.17 17 -3 -7 8.28 5.09 17 3 -7 6.59 5.33 17 3 -7 9.05 4.95 -17 -3 6 -2.83 4.31 -17 3 6 3.68 4.37 17 -3 -6 0.15 4.04 17 -3 -6 4.32 4.01 17 3 -6 1.92 3.92 17 3 -6 3.35 3.78 -17 -3 5 1.86 4.56 -17 3 5 2.89 4.04 17 -3 -5 5.10 5.03 17 -3 -5 1.37 3.09 17 3 -5 2.00 4.41 17 3 -5 2.35 3.87 -17 -3 4 -0.48 4.45 -17 3 4 3.65 4.74 17 -3 -4 2.38 4.53 17 -3 -4 3.65 3.72 17 3 -4 -2.20 3.75 17 3 -4 -1.15 3.33 -17 -3 3 1.61 4.64 -17 3 3 0.81 3.70 17 -3 -3 0.53 4.20 17 -3 -3 0.48 2.74 17 3 -3 -1.06 3.73 17 3 -3 0.50 2.97 -17 -3 2 4.99 5.71 -17 3 2 3.95 4.41 17 -3 -2 4.92 4.92 17 -3 -2 1.70 3.22 17 3 -2 1.68 4.22 17 3 -2 6.27 4.24 -17 -3 1 2.01 4.88 -17 3 1 2.88 4.70 17 -3 -1 2.16 4.79 17 -3 -1 0.45 3.16 17 3 -1 1.15 4.48 17 3 -1 -0.70 3.24 -17 -3 0 17.98 7.59 -17 3 0 20.73 7.64 17 -3 0 9.23 6.50 17 3 0 19.56 7.46 -17 -3 -1 7.25 5.75 -17 3 -1 1.77 4.16 17 -3 1 8.24 5.85 17 3 1 2.38 4.97 -17 -3 -2 22.00 8.48 -17 3 -2 16.21 7.14 17 -3 2 14.27 7.02 17 3 2 23.56 8.48 -17 -4 10 -1.16 4.01 -17 4 10 2.46 4.62 17 -4 -10 3.22 5.38 17 -4 -10 1.80 4.45 17 4 -10 5.34 5.02 -17 -4 9 6.64 5.39 -17 4 9 6.20 5.26 17 -4 -9 5.69 5.29 17 -4 -9 4.64 4.35 17 4 -9 3.82 4.72 -17 -4 8 0.26 3.90 -17 4 8 -3.26 3.27 17 -4 -8 -1.70 3.34 17 -4 -8 2.37 3.80 17 4 -8 0.37 3.78 -17 -4 7 7.92 6.17 -17 4 7 3.39 4.03 17 -4 -7 0.48 3.62 17 -4 -7 3.80 4.66 17 4 -7 3.11 4.40 17 4 -7 -2.86 2.82 -17 -4 6 -0.34 3.67 -17 4 6 0.08 3.52 17 -4 -6 -0.43 3.26 17 -4 -6 0.39 3.10 17 4 -6 4.08 4.37 17 4 -6 -0.54 2.90 -17 -4 5 19.09 7.81 -17 4 5 10.76 5.61 17 -4 -5 16.38 7.10 17 -4 -5 16.05 6.12 17 4 -5 10.48 5.62 17 4 -5 13.54 5.93 -17 -4 4 -0.87 4.00 -17 4 4 -0.12 3.87 17 -4 -4 -2.46 3.12 17 -4 -4 0.18 2.63 17 4 -4 3.02 4.58 17 4 -4 4.75 3.99 -17 -4 3 2.89 5.31 -17 4 3 7.96 5.41 17 -4 -3 4.58 5.02 17 -4 -3 8.29 4.60 17 4 -3 4.11 4.61 17 4 -3 5.59 4.35 -17 -4 2 0.10 4.66 -17 4 2 -1.24 3.57 17 -4 -2 0.39 4.56 17 -4 -2 0.14 2.95 17 4 -2 -1.64 3.91 17 4 -2 1.54 3.53 -17 -4 1 2.43 5.20 -17 4 1 2.06 4.25 17 -4 -1 2.46 4.84 17 4 -1 0.28 3.97 17 4 -1 2.55 3.50 -17 -4 0 11.23 6.36 -17 4 0 7.84 5.98 -17 4 0 11.90 6.34 -17 4 0 7.80 5.15 17 -4 0 10.60 6.20 17 4 0 4.21 5.34 -17 -4 -1 0.30 4.78 -17 4 -1 5.70 5.03 17 -4 1 2.51 5.17 17 4 1 -2.31 4.06 -17 -4 -2 14.03 7.25 -17 4 -2 7.27 5.62 17 -4 2 14.17 7.06 17 4 2 10.49 6.59 -17 -5 9 1.65 4.40 -17 5 9 -4.42 3.43 17 -5 -9 -0.52 3.88 17 -5 -9 0.41 3.38 17 5 -9 3.61 4.75 -17 -5 8 0.02 3.87 -17 5 8 3.80 3.76 17 -5 -8 -0.34 3.90 17 -5 -8 1.47 4.47 17 5 -8 -0.66 3.67 -17 -5 7 0.67 4.77 -17 5 7 0.97 4.00 17 -5 -7 1.20 4.31 17 -5 -7 3.48 4.34 17 5 -7 0.97 3.65 -17 -5 6 3.90 4.97 -17 5 6 1.55 3.83 17 -5 -6 1.47 4.50 17 -5 -6 0.92 3.18 17 5 -6 1.63 3.95 -17 -5 5 1.04 4.81 -17 5 5 0.47 3.38 17 -5 -5 1.27 4.71 17 -5 -5 1.28 3.82 17 5 -5 0.21 4.04 17 5 -5 -0.44 3.44 -17 -5 4 27.68 9.25 -17 5 4 20.30 7.67 17 -5 -4 16.27 7.31 17 -5 -4 24.01 7.35 17 5 -4 20.06 6.94 17 5 -4 21.67 7.05 -17 -5 3 3.20 5.21 -17 5 3 0.42 4.27 -17 5 3 -2.31 3.48 17 -5 -3 1.97 5.14 17 5 -3 5.64 5.06 17 5 -3 7.85 5.10 -17 -5 2 -0.43 4.35 -17 5 2 3.95 4.49 -17 5 2 1.15 3.54 -17 5 2 3.30 3.78 17 -5 -2 2.65 4.70 17 5 -2 4.61 5.14 17 5 -2 1.70 3.60 -17 -5 1 5.95 5.76 -17 5 1 4.08 4.77 -17 5 1 6.80 5.30 -17 5 1 7.91 4.56 17 -5 -1 5.67 5.78 17 5 -1 7.43 5.32 17 5 -1 2.98 4.09 -17 -5 0 1.57 4.80 -17 5 0 1.65 4.88 -17 5 0 -1.41 3.81 -17 5 0 1.15 2.99 17 -5 0 2.19 4.75 17 5 0 -0.77 3.91 -17 -5 -1 10.42 7.00 -17 5 -1 10.24 6.20 17 -5 1 3.75 5.60 17 5 1 3.40 5.38 -17 -6 8 5.45 5.77 -17 6 8 1.51 4.38 17 -6 -8 -1.44 3.92 17 6 -8 1.85 3.95 -17 -6 7 -3.94 3.68 -17 6 7 2.17 4.17 17 -6 -7 -0.84 3.60 17 6 -7 -1.81 3.27 -17 -6 6 -1.96 4.22 -17 6 6 0.98 3.83 -17 6 6 2.06 4.03 -17 6 6 -2.22 3.35 17 -6 -6 0.04 4.56 17 6 -6 -2.35 3.09 -17 -6 5 2.20 4.53 -17 6 5 4.14 4.62 -17 6 5 0.46 4.26 -17 6 5 1.99 3.60 17 -6 -5 2.29 4.80 17 6 -5 -1.47 3.09 -17 -6 4 -3.56 3.71 -17 6 4 3.00 4.65 -17 6 4 2.54 4.09 -17 6 4 0.27 3.86 17 -6 -4 0.01 3.74 17 6 -4 3.40 4.79 17 6 -4 -0.85 3.20 -17 -6 3 0.36 5.08 -17 6 3 -0.13 4.02 -17 6 3 -0.89 3.61 -17 6 3 1.50 3.39 17 -6 -3 1.82 4.29 17 6 -3 -0.59 3.72 17 6 -3 3.44 3.65 -17 -6 2 1.68 4.67 -17 6 2 5.10 4.90 -17 6 2 7.47 5.18 -17 6 2 2.22 3.94 17 -6 -2 6.96 6.24 17 6 -2 1.82 4.54 17 6 -2 8.36 4.89 -17 -6 1 -0.57 4.31 -17 6 1 -3.86 3.89 -17 6 1 -3.23 3.64 -17 6 1 -2.64 2.67 17 -6 -1 0.54 3.85 17 6 -1 -1.85 4.10 17 6 -1 -1.48 2.94 -17 -6 0 7.35 6.23 -17 6 0 3.87 4.85 -17 6 0 0.88 3.08 17 -6 0 6.08 5.53 17 6 0 2.97 5.03 -17 -7 7 2.10 5.25 -17 7 7 -4.05 3.50 -17 7 7 2.82 4.28 -17 7 7 9.02 6.28 17 -7 -7 -1.35 4.06 17 7 -7 5.17 4.73 -17 -7 6 3.33 5.58 -17 7 6 0.79 3.77 -17 7 6 0.24 4.38 -17 7 6 -0.27 3.16 17 -7 -6 2.02 4.73 17 7 -6 -2.27 3.75 -17 -7 5 12.16 6.77 -17 7 5 13.43 6.36 -17 7 5 10.60 6.51 -17 7 5 12.43 6.21 17 -7 -5 9.10 6.07 17 7 -5 15.98 7.08 -17 -7 4 2.16 4.93 -17 7 4 -2.19 3.58 -17 7 4 2.93 4.20 -17 7 4 0.69 3.56 17 -7 -4 4.17 5.01 17 7 -4 1.93 4.20 -17 -7 3 3.00 5.52 -17 7 3 -2.14 3.79 -17 7 3 4.72 4.48 -17 7 3 2.56 4.19 17 -7 -3 1.43 4.91 17 7 -3 4.94 5.18 17 7 -3 -0.06 4.07 -17 -7 2 -0.47 4.23 -17 7 2 1.21 4.44 -17 7 2 0.40 4.29 -17 7 2 -3.11 2.79 17 -7 -2 2.22 4.31 17 7 -2 1.16 4.63 17 7 -2 -0.26 3.63 -17 -7 1 11.77 6.67 -17 7 1 7.24 5.95 -17 7 1 3.16 4.40 -17 7 1 11.94 5.45 17 -7 -1 3.74 4.53 17 7 -1 5.74 5.69 -18 0 9 1.47 4.06 18 0 -9 1.40 4.53 18 0 -9 -0.13 3.48 -18 0 8 2.64 4.70 18 0 -8 1.23 4.36 18 0 -8 4.03 4.04 -18 0 7 4.95 4.84 18 0 -7 0.91 4.00 18 0 -7 0.91 3.82 -18 0 6 3.89 4.64 18 0 -6 1.80 4.55 18 0 -6 4.20 4.49 -18 0 5 2.91 4.64 18 0 -5 1.55 4.41 18 0 -5 0.95 3.51 -18 0 4 14.48 7.16 18 0 -4 16.78 7.32 18 0 -4 15.79 6.32 -18 0 3 -2.09 3.00 18 0 -3 0.51 4.53 18 0 -3 1.39 3.36 -18 0 2 54.74 12.52 18 0 -2 47.11 11.28 18 0 -2 49.95 10.13 -18 0 1 -0.71 3.88 18 0 -1 1.53 4.41 -18 0 0 6.49 6.19 18 0 0 6.23 5.66 -18 -1 9 3.45 4.60 -18 1 9 -0.59 4.42 18 -1 -9 0.05 3.92 18 -1 -9 3.43 4.13 18 1 -9 3.48 4.70 18 1 -9 -3.03 3.03 -18 -1 8 -2.80 3.82 -18 1 8 0.71 3.87 18 -1 -8 -1.22 4.02 18 -1 -8 1.72 4.10 18 1 -8 3.10 4.12 18 1 -8 2.26 3.73 -18 -1 7 1.46 4.19 -18 1 7 -1.45 3.71 18 -1 -7 4.39 5.14 18 -1 -7 0.35 3.61 18 1 -7 3.22 4.19 18 1 -7 0.14 2.99 -18 -1 6 4.91 5.03 -18 1 6 2.40 4.19 18 -1 -6 2.30 4.65 18 -1 -6 0.48 3.53 18 1 -6 3.11 4.68 18 1 -6 -0.23 3.63 -18 -1 5 -0.13 3.85 -18 1 5 3.92 5.21 18 -1 -5 7.04 5.63 18 -1 -5 3.26 4.01 18 1 -5 7.81 5.16 18 1 -5 4.52 4.31 -18 -1 4 14.83 7.91 -18 1 4 13.49 6.48 18 -1 -4 16.00 7.13 18 -1 -4 11.69 5.72 18 1 -4 12.85 6.31 18 1 -4 12.39 5.76 -18 -1 3 1.15 4.04 -18 1 3 -1.04 3.59 18 -1 -3 3.07 5.30 18 -1 -3 1.18 3.31 18 1 -3 0.36 3.81 18 1 -3 1.03 3.36 -18 -1 2 6.85 6.02 -18 1 2 13.19 6.56 18 -1 -2 18.04 7.47 18 -1 -2 12.14 5.78 18 1 -2 6.58 5.78 18 1 -2 9.26 5.16 -18 -1 1 3.56 5.39 -18 1 1 2.38 4.69 18 -1 -1 2.20 5.17 18 1 -1 2.63 4.51 -18 -1 0 3.18 5.23 -18 1 0 2.28 4.71 18 -1 0 2.60 4.57 18 1 0 0.94 4.41 18 -2 -9 1.77 4.26 18 2 -9 1.54 4.01 -18 -2 8 5.28 5.23 -18 2 8 0.18 4.34 18 -2 -8 0.76 4.06 18 -2 -8 3.92 4.34 18 2 -8 0.57 3.87 18 2 -8 2.31 4.35 -18 -2 7 0.95 4.40 -18 2 7 3.80 4.88 18 -2 -7 2.61 4.24 18 -2 -7 -0.83 3.71 18 2 -7 4.91 4.62 18 2 -7 -0.31 3.75 -18 -2 6 12.44 7.31 -18 2 6 8.13 5.59 18 -2 -6 7.75 6.07 18 -2 -6 7.28 4.53 18 2 -6 11.44 5.90 18 2 -6 11.65 5.95 -18 -2 5 -3.46 3.43 -18 2 5 2.90 4.43 18 -2 -5 -0.50 4.24 18 -2 -5 2.95 4.18 18 2 -5 -1.31 3.99 18 2 -5 3.18 3.91 -18 -2 4 -1.64 3.41 -18 2 4 1.52 3.43 18 -2 -4 2.93 4.68 18 -2 -4 1.47 3.82 18 2 -4 0.40 4.05 18 2 -4 1.47 3.69 -18 -2 3 0.49 5.18 -18 2 3 3.07 4.56 18 -2 -3 4.76 5.34 18 -2 -3 4.36 3.69 18 2 -3 -2.43 3.76 18 2 -3 3.81 3.89 -18 -2 2 8.70 5.74 -18 2 2 4.78 5.43 18 -2 -2 8.35 6.01 18 -2 -2 13.86 5.91 18 2 -2 5.68 5.36 18 2 -2 9.80 5.06 -18 -2 1 -0.11 4.79 -18 2 1 -3.56 2.48 18 -2 -1 3.43 4.98 18 2 -1 -5.78 3.35 18 2 -1 1.59 2.86 -18 -2 0 -2.06 3.86 -18 2 0 -2.64 4.49 18 -2 0 -0.32 4.33 18 2 0 -0.26 4.64 -18 -3 8 0.70 4.28 -18 3 8 0.63 4.25 18 -3 -8 5.99 5.61 18 -3 -8 3.23 4.44 18 3 -8 3.57 4.16 -18 -3 7 6.43 5.26 -18 3 7 7.14 5.65 18 -3 -7 6.24 5.50 18 -3 -7 7.99 5.24 18 3 -7 6.90 5.45 18 3 -7 11.35 5.75 -18 -3 6 0.35 4.67 -18 3 6 -3.67 3.30 18 -3 -6 -1.25 3.95 18 -3 -6 -0.66 3.60 18 3 -6 1.67 4.56 18 3 -6 4.09 3.95 -18 -3 5 6.47 5.97 -18 3 5 8.28 6.01 18 -3 -5 5.07 5.09 18 -3 -5 8.81 4.88 18 3 -5 11.46 5.93 18 3 -5 2.52 4.00 -18 -3 4 2.05 4.52 -18 3 4 5.26 4.93 18 -3 -4 5.46 5.06 18 -3 -4 1.39 3.65 18 3 -4 3.14 4.72 18 3 -4 1.27 3.52 -18 -3 3 13.40 7.13 -18 3 3 10.99 6.64 18 -3 -3 12.12 6.83 18 -3 -3 13.25 5.49 18 3 -3 7.38 5.70 18 3 -3 9.77 5.46 -18 -3 2 -0.86 4.52 -18 3 2 -0.28 4.03 18 -3 -2 0.80 4.63 18 -3 -2 1.78 3.29 18 3 -2 3.56 4.96 18 3 -2 1.97 3.65 -18 -3 1 2.99 5.47 -18 3 1 2.08 4.37 18 -3 -1 9.16 6.50 18 3 -1 0.71 4.21 18 3 -1 3.73 3.58 -18 -4 7 1.71 4.87 -18 4 7 -2.29 3.67 18 -4 -7 1.40 4.92 18 -4 -7 -3.65 3.16 18 4 -7 4.29 4.65 -18 -4 6 -1.26 4.57 -18 4 6 -0.51 4.03 18 -4 -6 -2.26 3.79 18 -4 -6 -3.02 3.02 18 4 -6 -2.86 3.82 18 4 -6 -3.02 3.22 -18 -4 5 3.23 5.79 -18 4 5 10.40 6.26 18 -4 -5 12.45 6.37 18 -4 -5 4.59 4.36 18 4 -5 6.16 4.98 18 4 -5 6.30 5.15 -18 -4 4 2.58 5.53 -18 4 4 0.31 4.37 18 -4 -4 0.93 4.05 18 -4 -4 0.30 3.66 18 4 -4 -3.10 3.61 18 4 -4 0.58 3.37 -18 -4 3 4.57 5.43 -18 4 3 0.33 4.35 18 -4 -3 -1.85 3.40 18 -4 -3 0.20 3.22 18 4 -3 2.55 4.65 18 4 -3 1.49 3.60 -18 -4 2 -3.92 4.30 -18 4 2 3.46 4.07 18 -4 -2 3.62 5.35 18 4 -2 -4.46 3.40 18 4 -2 -0.05 3.39 -18 -5 5 0.45 4.36 18 -5 -5 2.11 4.40 18 -5 -5 4.30 4.59 18 5 -5 0.40 3.96 -18 -5 4 1.04 5.25 -18 5 4 2.14 4.74 18 -5 -4 4.07 5.17 18 5 -4 1.51 4.67 18 5 -4 2.25 3.45 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 26422 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O -0.03536(15) 0.38349(15) 0.41925(15) 0.0347(6) Uani 1 1 d . . . . O2 O 0.28537(15) 0.28141(16) 0.59395(15) 0.0330(6) Uani 1 1 d . . . . O3 O 0.27180(15) 0.55642(17) 0.50819(16) 0.0415(7) Uani 1 1 d . . . . O4 O 0.39718(16) 0.49668(17) 0.69270(15) 0.0423(7) Uani 1 1 d . . . . N1 N 0.29720(17) 0.41950(18) 0.55575(17) 0.0293(7) Uani 1 1 d . . . . C1 C 0.0409(2) 0.3832(2) 0.4350(2) 0.0284(9) Uani 1 1 d . . . . C2 C 0.1058(2) 0.3146(2) 0.4763(2) 0.0287(9) Uani 1 1 d . . . . C3 C 0.1591(2) 0.3706(2) 0.5501(2) 0.0266(8) Uani 1 1 d . . . . H3 H 0.1358 0.3673 0.6016 0.032 Uiso 1 1 calc R . . . C4 C 0.2527(2) 0.3487(2) 0.5701(2) 0.0289(9) Uani 1 1 d . . . . C5 C 0.2453(2) 0.4888(2) 0.5246(2) 0.0321(9) Uani 1 1 d . . . . C6 C 0.1540(2) 0.4618(2) 0.5147(2) 0.0275(8) Uani 1 1 d . . . . H6 H 0.1237 0.5002 0.5467 0.033 Uiso 1 1 calc R . . . C7 C 0.1029(2) 0.4524(2) 0.4201(2) 0.0267(8) Uani 1 1 d . . . . C8 C 0.1564(2) 0.3956(2) 0.3770(2) 0.0332(9) Uani 1 1 d . . . . C9 C 0.1564(2) 0.3154(2) 0.4078(2) 0.0327(9) Uani 1 1 d . . . . C10 C 0.2061(2) 0.2491(3) 0.3824(3) 0.0427(11) Uani 1 1 d . . . . C11 C 0.2110(2) 0.1667(3) 0.4169(3) 0.0496(12) Uani 1 1 d . . . . H11 H 0.1820 0.1541 0.4597 0.059 Uiso 1 1 calc R . . . C12 C 0.2574(3) 0.1046(3) 0.3889(3) 0.0666(16) Uani 1 1 d . . . . H12 H 0.2600 0.0491 0.4120 0.080 Uiso 1 1 calc R . . . C13 C 0.3009(3) 0.1235(4) 0.3262(3) 0.083(2) Uani 1 1 d . . . . H13 H 0.3324 0.0805 0.3064 0.100 Uiso 1 1 calc R . . . C14 C 0.2982(3) 0.2030(4) 0.2937(3) 0.0749(18) Uani 1 1 d . . . . H14 H 0.3287 0.2146 0.2519 0.090 Uiso 1 1 calc R . . . C15 C 0.2515(2) 0.2687(3) 0.3203(3) 0.0527(13) Uani 1 1 d . . . . C16 C 0.2502(2) 0.3542(3) 0.2862(3) 0.0527(13) Uani 1 1 d . . . . C17 C 0.2947(3) 0.3759(4) 0.2240(3) 0.0655(16) Uani 1 1 d . . . . H17 H 0.3256 0.3333 0.2030 0.079 Uiso 1 1 calc R . . . C18 C 0.2945(3) 0.4564(5) 0.1935(3) 0.0758(18) Uani 1 1 d . . . . H18 H 0.3233 0.4688 0.1505 0.091 Uiso 1 1 calc R . . . C19 C 0.2522(3) 0.5196(4) 0.2255(3) 0.0627(14) Uani 1 1 d . . . . H19 H 0.2535 0.5759 0.2054 0.075 Uiso 1 1 calc R . . . C20 C 0.2081(2) 0.5022(3) 0.2860(2) 0.0465(11) Uani 1 1 d . . . . H20 H 0.1798 0.5466 0.3078 0.056 Uiso 1 1 calc R . . . C21 C 0.2045(2) 0.4188(3) 0.3161(2) 0.0410(11) Uani 1 1 d . . . . C22 C 0.0675(2) 0.2344(2) 0.5012(2) 0.0342(9) Uani 1 1 d . . . . C23 C 0.0984(2) 0.1958(2) 0.5796(3) 0.0406(10) Uani 1 1 d . . . . H23 H 0.1470 0.2189 0.6177 0.049 Uiso 1 1 calc R . . . C24 C 0.0598(2) 0.1251(2) 0.6024(3) 0.0441(11) Uani 1 1 d . . . . H24 H 0.0821 0.0996 0.6559 0.053 Uiso 1 1 calc R . . . C25 C -0.0115(3) 0.0908(3) 0.5482(3) 0.0461(11) Uani 1 1 d . . . . H25 H -0.0395 0.0430 0.5645 0.055 Uiso 1 1 calc R . . . C26 C -0.0413(2) 0.1279(2) 0.4689(3) 0.0443(11) Uani 1 1 d . . . . H26 H -0.0891 0.1039 0.4304 0.053 Uiso 1 1 calc R . . . C27 C -0.0028(2) 0.1985(2) 0.4454(3) 0.0393(10) Uani 1 1 d . . . . H27 H -0.0240 0.2228 0.3911 0.047 Uiso 1 1 calc R . . . C28 C 0.0607(2) 0.5298(2) 0.3746(2) 0.0331(9) Uani 1 1 d . . . . C29 C 0.0002(2) 0.5189(3) 0.2978(2) 0.0393(10) Uani 1 1 d . . . . H29 H -0.0139 0.4634 0.2764 0.047 Uiso 1 1 calc R . . . C30 C -0.0388(2) 0.5875(3) 0.2532(2) 0.0448(11) Uani 1 1 d . . . . H30 H -0.0795 0.5794 0.2012 0.054 Uiso 1 1 calc R . . . C31 C -0.0190(2) 0.6685(3) 0.2839(3) 0.0457(11) Uani 1 1 d . . . . H31 H -0.0461 0.7161 0.2531 0.055 Uiso 1 1 calc R . . . C32 C 0.0404(2) 0.6801(3) 0.3595(2) 0.0412(10) Uani 1 1 d . . . . H32 H 0.0541 0.7357 0.3807 0.049 Uiso 1 1 calc R . . . C33 C 0.0798(2) 0.6110(2) 0.4043(2) 0.0345(9) Uani 1 1 d . . . . H33 H 0.1205 0.6195 0.4562 0.041 Uiso 1 1 calc R . . . C34 C 0.3876(2) 0.4202(2) 0.5664(2) 0.0327(9) Uani 1 1 d . . . . C35 C 0.4379(2) 0.4624(2) 0.6351(2) 0.0370(10) Uani 1 1 d . . . . C36 C 0.5252(3) 0.4654(3) 0.6446(3) 0.0492(12) Uani 1 1 d . . . . H36 H 0.5601 0.4949 0.6909 0.059 Uiso 1 1 calc R . . . C37 C 0.5612(3) 0.4254(3) 0.5868(3) 0.0528(12) Uani 1 1 d . . . . H37 H 0.6211 0.4280 0.5930 0.063 Uiso 1 1 calc R . . . C38 C 0.5114(3) 0.3814(3) 0.5198(3) 0.0471(11) Uani 1 1 d . . . . H38 H 0.5371 0.3525 0.4811 0.057 Uiso 1 1 calc R . . . C39 C 0.4241(2) 0.3794(3) 0.5093(2) 0.0408(10) Uani 1 1 d . . . . H39 H 0.3894 0.3501 0.4628 0.049 Uiso 1 1 calc R . . . C40 C 0.4330(2) 0.5702(3) 0.7343(2) 0.0415(10) Uani 1 1 d . . . . C41 C 0.4243(2) 0.6458(3) 0.6899(3) 0.0455(11) Uani 1 1 d . . . . H41 H 0.3948 0.6470 0.6321 0.055 Uiso 1 1 calc R . . . C42 C 0.4585(2) 0.7195(3) 0.7300(3) 0.0450(11) Uani 1 1 d . . . . C43 C 0.4993(2) 0.7155(3) 0.8155(3) 0.0449(11) Uani 1 1 d . . . . H43 H 0.5227 0.7658 0.8437 0.054 Uiso 1 1 calc R . . . C44 C 0.5069(3) 0.6404(3) 0.8606(3) 0.0480(11) Uani 1 1 d . . . . C45 C 0.4734(3) 0.5666(3) 0.8187(2) 0.0471(11) Uani 1 1 d . . . . H45 H 0.4784 0.5142 0.8481 0.056 Uiso 1 1 calc R . . . C46 C 0.4510(3) 0.8026(3) 0.6823(3) 0.0588(13) Uani 1 1 d . . . . H46A H 0.4513 0.7917 0.6232 0.088 Uiso 1 1 calc GR . . . H46B H 0.4993 0.8392 0.7079 0.088 Uiso 1 1 calc GR . . . H46C H 0.3977 0.8307 0.6850 0.088 Uiso 1 1 calc GR . . . C47 C 0.5519(3) 0.6384(3) 0.9532(3) 0.0657(14) Uani 1 1 d . . . . H47A H 0.6078 0.6657 0.9613 0.099 Uiso 1 1 calc GR . . . H47B H 0.5594 0.5795 0.9725 0.099 Uiso 1 1 calc GR . . . H47C H 0.5177 0.6688 0.9859 0.099 Uiso 1 1 calc GR . . . Cl1 Cl 0.22553(16) 0.71811(19) 0.61021(17) 0.0352(8) Uani 0.353(2) 1 d . P A 1 Cl2 Cl 0.21841(16) 0.57304(17) 0.71974(18) 0.0395(9) Uani 0.353(2) 1 d . P A 1 Cl3 Cl 0.16215(18) 0.73765(18) 0.76049(17) 0.0412(9) Uani 0.353(2) 1 d . P A 1 C81 C 0.2308(6) 0.6812(6) 0.7130(6) 0.032(3) Uiso 0.353(2) 1 d . P A 1 D81 D 0.2897 0.6942 0.7466 0.039 Uiso 0.353(2) 1 calc R P A 1 Cl4 Cl 0.2486(3) 0.7575(3) 0.5020(3) 0.0670(18) Uiso 0.249(3) 1 d . P B 2 Cl5 Cl 0.3450(3) 0.8679(3) 0.4247(3) 0.0555(16) Uiso 0.249(3) 1 d . P B 2 Cl6 Cl 0.2503(3) 0.9362(3) 0.5294(4) 0.0467(15) Uiso 0.249(3) 1 d . P B 2 C82 C 0.2458(11) 0.8574(10) 0.4487(11) 0.069(8) Uiso 0.249(3) 1 d . P B 2 D82 D 0.1964 0.8640 0.3989 0.082 Uiso 0.249(3) 1 calc R P B 2 Cl10 Cl 0.1954(3) 0.6262(3) 0.7604(4) 0.0823(18) Uiso 0.302(3) 1 d . P C 3 Cl11 Cl 0.2639(3) 0.7886(3) 0.8210(4) 0.094(2) Uiso 0.302(3) 1 d . P C 3 Cl12 Cl 0.2761(6) 0.6518(5) 0.9365(5) 0.125(3) Uiso 0.302(3) 1 d . P C 3 C84 C 0.2754(9) 0.6804(8) 0.8356(9) 0.053(5) Uiso 0.302(3) 1 d . P C 3 D84 D 0.3318 0.6643 0.8250 0.064 Uiso 0.302(3) 1 calc R P C 3 Cl7 Cl 0.2729(3) 0.7750(3) 0.8912(3) 0.0683(16) Uiso 0.297(3) 1 d . P D 4 Cl8 Cl 0.2118(4) 0.7512(4) 0.7149(4) 0.113(2) Uiso 0.297(3) 1 d . P D 4 Cl9 Cl 0.2038(4) 0.6146(4) 0.8209(4) 0.102(2) Uiso 0.297(3) 1 d . P D 4 C83 C 0.2630(9) 0.7000(8) 0.8067(8) 0.046(4) Uiso 0.297(3) 1 d . P D 4 D83 D 0.3208 0.6811 0.8022 0.056 Uiso 0.297(3) 1 calc R P D 4 Cl13 Cl 0.2330(5) 0.7626(6) 0.5743(6) 0.053(3) Uiso 0.137(3) 1 d . P E 5 Cl14 Cl 0.2606(14) 0.9225(11) 0.5072(14) 0.156(10) Uiso 0.137(3) 1 d . P E 5 Cl15 Cl 0.3257(6) 0.7756(6) 0.4477(6) 0.067(3) Uiso 0.137(3) 1 d . P E 5 C85 C 0.2387(16) 0.8181(14) 0.4806(15) 0.099(15) Uiso 0.137(3) 1 d . P E 5 D85 D 0.1846 0.8122 0.4358 0.118 Uiso 0.137(3) 1 calc R P E 5 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 0.0258(15) 0.0382(16) 0.0368(16) -0.0032(12) 0.0005(12) 0.0051(11) O2 0.0275(14) 0.0389(16) 0.0287(15) 0.0014(12) -0.0007(11) 0.0066(12) O3 0.0331(16) 0.0402(17) 0.0435(17) 0.0090(13) -0.0060(13) -0.0061(12) O4 0.0391(16) 0.0559(18) 0.0306(16) -0.0072(13) 0.0054(13) -0.0223(13) N1 0.0247(17) 0.0340(18) 0.0246(17) 0.0034(14) -0.0036(13) 0.0006(14) C1 0.026(2) 0.037(2) 0.020(2) -0.0108(16) 0.0004(16) 0.0035(16) C2 0.0235(19) 0.032(2) 0.025(2) -0.0080(16) -0.0051(16) 0.0053(16) C3 0.0236(19) 0.030(2) 0.024(2) -0.0009(16) 0.0020(16) 0.0043(15) C4 0.028(2) 0.037(2) 0.018(2) -0.0048(17) -0.0021(16) 0.0030(18) C5 0.033(2) 0.039(2) 0.019(2) -0.0027(18) -0.0045(17) -0.0033(19) C6 0.025(2) 0.032(2) 0.022(2) -0.0028(16) -0.0017(16) 0.0033(15) C7 0.0192(19) 0.038(2) 0.021(2) -0.0033(16) 0.0006(15) 0.0049(15) C8 0.0184(19) 0.053(3) 0.023(2) -0.0080(19) -0.0056(16) 0.0061(17) C9 0.019(2) 0.048(3) 0.024(2) -0.0132(18) -0.0070(16) 0.0049(17) C10 0.024(2) 0.061(3) 0.034(2) -0.023(2) -0.0121(18) 0.0143(19) C11 0.027(2) 0.059(3) 0.051(3) -0.026(2) -0.014(2) 0.010(2) C12 0.044(3) 0.073(3) 0.064(4) -0.038(3) -0.024(3) 0.028(2) C13 0.061(4) 0.124(5) 0.048(3) -0.050(3) -0.020(3) 0.057(4) C14 0.045(3) 0.133(5) 0.036(3) -0.030(3) -0.011(2) 0.051(3) C15 0.023(2) 0.100(4) 0.027(2) -0.032(3) -0.0101(19) 0.020(2) C16 0.022(2) 0.101(4) 0.029(3) -0.021(3) -0.0060(19) 0.008(2) C17 0.022(2) 0.136(5) 0.038(3) -0.041(3) 0.006(2) -0.009(3) C18 0.038(3) 0.150(6) 0.042(3) -0.034(4) 0.015(2) -0.038(3) C19 0.036(3) 0.113(4) 0.040(3) -0.018(3) 0.011(2) -0.029(3) C20 0.029(2) 0.076(3) 0.032(2) -0.008(2) 0.0020(19) -0.013(2) C21 0.015(2) 0.080(3) 0.022(2) -0.017(2) -0.0062(16) -0.001(2) C22 0.026(2) 0.030(2) 0.041(2) -0.0075(19) -0.0020(18) 0.0070(16) C23 0.030(2) 0.027(2) 0.055(3) -0.001(2) -0.010(2) 0.0054(17) C24 0.041(3) 0.030(2) 0.051(3) 0.001(2) -0.008(2) 0.0050(19) C25 0.039(3) 0.034(2) 0.060(3) -0.004(2) 0.002(2) 0.0015(19) C26 0.036(2) 0.036(2) 0.054(3) -0.012(2) -0.004(2) 0.0008(19) C27 0.031(2) 0.036(2) 0.045(3) -0.0080(19) -0.0012(19) 0.0038(18) C28 0.022(2) 0.049(3) 0.027(2) 0.0061(19) 0.0054(16) 0.0019(17) C29 0.027(2) 0.060(3) 0.028(2) 0.002(2) 0.0013(18) 0.0037(19) C30 0.029(2) 0.073(3) 0.027(2) 0.013(2) -0.0036(18) 0.006(2) C31 0.034(2) 0.059(3) 0.043(3) 0.022(2) 0.007(2) 0.009(2) C32 0.032(2) 0.047(3) 0.041(3) 0.014(2) 0.003(2) 0.0011(19) C33 0.030(2) 0.043(3) 0.027(2) 0.0081(19) 0.0003(17) 0.0025(18) C34 0.021(2) 0.044(2) 0.029(2) 0.0105(18) -0.0026(17) -0.0007(17) C35 0.031(2) 0.049(3) 0.027(2) 0.0087(19) -0.0006(18) -0.0066(18) C36 0.030(2) 0.073(3) 0.038(3) 0.013(2) -0.005(2) -0.020(2) C37 0.025(2) 0.083(3) 0.049(3) 0.025(3) 0.005(2) 0.000(2) C38 0.037(3) 0.067(3) 0.040(3) 0.013(2) 0.013(2) 0.009(2) C39 0.034(2) 0.057(3) 0.029(2) 0.006(2) 0.0015(19) 0.003(2) C40 0.036(2) 0.053(3) 0.032(2) 0.000(2) 0.0019(19) -0.020(2) C41 0.042(3) 0.064(3) 0.027(2) 0.000(2) 0.0009(19) -0.017(2) C42 0.036(2) 0.057(3) 0.041(3) -0.002(2) 0.007(2) -0.011(2) C43 0.036(2) 0.051(3) 0.044(3) -0.012(2) 0.004(2) -0.013(2) C44 0.039(2) 0.063(3) 0.035(3) -0.007(2) -0.003(2) -0.011(2) C45 0.042(3) 0.060(3) 0.033(2) 0.004(2) -0.004(2) -0.016(2) C46 0.064(3) 0.055(3) 0.057(3) 0.003(2) 0.012(3) -0.009(2) C47 0.067(3) 0.078(4) 0.038(3) -0.005(2) -0.013(2) -0.021(3) Cl1 0.0267(15) 0.0469(19) 0.0319(16) -0.0020(14) 0.0070(12) 0.0024(12) Cl2 0.0286(15) 0.0329(17) 0.055(2) 0.0003(14) 0.0061(13) 0.0015(12) Cl3 0.0444(17) 0.0497(19) 0.0315(17) 0.0024(13) 0.0127(13) 0.0159(13) 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' D D 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C35 O4 C40 116.5(3) C4 N1 C5 113.9(3) C4 N1 C34 123.0(3) C5 N1 C34 123.0(3) O1 C1 C2 130.7(3) O1 C1 C7 129.6(3) C7 C1 C2 99.6(3) C1 C2 C3 97.5(2) C9 C2 C1 95.8(3) C9 C2 C3 105.2(3) C22 C2 C1 115.3(3) C22 C2 C3 116.8(3) C22 C2 C9 121.8(3) C2 C3 H3 111.4 C4 C3 C2 111.9(3) C4 C3 H3 111.4 C4 C3 C6 104.9(3) C6 C3 C2 105.5(3) C6 C3 H3 111.4 O2 C4 N1 124.2(3) O2 C4 C3 127.5(3) N1 C4 C3 108.2(3) O3 C5 N1 124.1(3) O3 C5 C6 128.2(3) N1 C5 C6 107.7(3) C3 C6 H6 111.1 C3 C6 C7 104.3(3) C5 C6 C3 105.0(3) C5 C6 H6 111.1 C5 C6 C7 113.8(3) C7 C6 H6 111.1 C1 C7 C6 96.9(3) C8 C7 C1 96.7(3) C8 C7 C6 106.5(3) C28 C7 C1 114.8(3) C28 C7 C6 118.5(3) C28 C7 C8 119.3(3) C9 C8 C7 109.0(3) C9 C8 C21 122.4(3) C21 C8 C7 128.5(4) C8 C9 C2 108.9(3) C8 C9 C10 121.4(4) C10 C9 C2 129.4(4) C11 C10 C9 122.6(4) C11 C10 C15 119.7(4) C15 C10 C9 117.8(4) C10 C11 H11 119.7 C12 C11 C10 120.6(5) C12 C11 H11 119.7 C11 C12 H12 120.1 C11 C12 C13 119.7(5) C13 C12 H12 120.1 C12 C13 H13 119.8 C14 C13 C12 120.3(5) C14 C13 H13 119.8 C13 C14 H14 119.0 C13 C14 C15 122.0(5) C15 C14 H14 119.0 C10 C15 C16 120.7(4) C14 C15 C10 117.7(5) C14 C15 C16 121.6(5) C17 C16 C15 122.2(5) C21 C16 C15 119.8(4) C21 C16 C17 117.9(5) C16 C17 H17 119.0 C18 C17 C16 121.9(5) C18 C17 H17 119.0 C17 C18 H18 120.2 C17 C18 C19 119.6(5) C19 C18 H18 120.2 C18 C19 H19 119.5 C20 C19 C18 121.0(5) C20 C19 H19 119.5 C19 C20 H20 119.8 C19 C20 C21 120.4(5) C21 C20 H20 119.8 C16 C21 C8 117.7(4) C20 C21 C8 123.2(4) C20 C21 C16 119.1(4) C23 C22 C2 122.2(3) C27 C22 C2 119.3(3) C27 C22 C23 118.5(4) C22 C23 H23 119.5 C24 C23 C22 121.1(4) C24 C23 H23 119.5 C23 C24 H24 119.7 C23 C24 C25 120.5(4) C25 C24 H24 119.7 C24 C25 H25 120.7 C24 C25 C26 118.5(4) C26 C25 H25 120.7 C25 C26 H26 119.4 C27 C26 C25 121.3(4) C27 C26 H26 119.4 C22 C27 H27 120.0 C26 C27 C22 120.0(4) C26 C27 H27 120.0 C29 C28 C7 118.5(3) C33 C28 C7 123.0(3) C33 C28 C29 118.5(3) C28 C29 H29 119.7 C30 C29 C28 120.7(4) C30 C29 H29 119.7 C29 C30 H30 120.0 C29 C30 C31 120.1(4) C31 C30 H30 120.0 C30 C31 H31 120.1 C32 C31 C30 119.8(4) C32 C31 H31 120.1 C31 C32 H32 119.9 C33 C32 C31 120.1(4) C33 C32 H32 119.9 C28 C33 C32 120.8(4) C28 C33 H33 119.6 C32 C33 H33 119.6 C35 C34 N1 119.2(3) C39 C34 N1 120.3(3) C39 C34 C35 120.5(3) O4 C35 C34 117.0(3) O4 C35 C36 123.3(4) C36 C35 C34 119.6(4) C35 C36 H36 120.2 C37 C36 C35 119.6(4) C37 C36 H36 120.2 C36 C37 H37 119.6 C36 C37 C38 120.8(4) C38 C37 H37 119.6 C37 C38 H38 120.1 C39 C38 C37 119.7(4) C39 C38 H38 120.1 C34 C39 C38 119.7(4) C34 C39 H39 120.1 C38 C39 H39 120.1 C41 C40 O4 118.9(3) C45 C40 O4 119.5(4) C45 C40 C41 121.5(4) C40 C41 H41 120.0 C42 C41 C40 119.9(4) C42 C41 H41 120.0 C41 C42 C43 118.3(4) C41 C42 C46 120.8(4) C43 C42 C46 120.9(4) C42 C43 H43 119.0 C44 C43 C42 122.1(4) C44 C43 H43 119.0 C43 C44 C45 118.7(4) C43 C44 C47 120.6(4) C45 C44 C47 120.7(4) C40 C45 C44 119.5(4) C40 C45 H45 120.3 C44 C45 H45 120.3 C42 C46 H46A 109.5 C42 C46 H46B 109.5 C42 C46 H46C 109.5 H46A C46 H46B 109.5 H46A C46 H46C 109.5 H46B C46 H46C 109.5 C44 C47 H47A 109.5 C44 C47 H47B 109.5 C44 C47 H47C 109.5 H47A C47 H47B 109.5 H47A C47 H47C 109.5 H47B C47 H47C 109.5 Cl1 C81 D81 106.1 Cl2 C81 Cl1 114.1(5) Cl2 C81 Cl3 112.5(5) Cl2 C81 D81 106.1 Cl3 C81 Cl1 111.3(5) Cl3 C81 D81 106.1 Cl4 C82 Cl6 105.2(9) Cl4 C82 D82 114.0 Cl5 C82 Cl4 105.8(9) Cl5 C82 Cl6 102.6(9) Cl5 C82 D82 114.0 Cl6 C82 D82 114.0 Cl10 C84 D84 107.5 Cl11 C84 Cl10 110.2(8) Cl11 C84 D84 107.5 Cl12 C84 Cl10 112.1(8) Cl12 C84 Cl11 111.8(8) Cl12 C84 D84 107.5 Cl7 C83 D83 109.8 Cl8 C83 Cl7 107.0(8) Cl8 C83 D83 109.8 Cl9 C83 Cl7 111.6(8) Cl9 C83 Cl8 108.6(8) Cl9 C83 D83 109.8 Cl13 C85 D85 111.4 Cl14 C85 Cl13 107.8(14) Cl14 C85 Cl15 108.2(14) Cl14 C85 D85 111.4 Cl15 C85 Cl13 106.4(12) Cl15 C85 D85 111.4 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C1 1.198(4) O2 C4 1.208(4) O3 C5 1.205(4) O4 C35 1.380(4) O4 C40 1.399(4) N1 C4 1.379(4) N1 C5 1.398(5) N1 C34 1.430(4) C1 C2 1.546(5) C1 C7 1.540(5) C2 C3 1.576(5) C2 C9 1.533(5) C2 C22 1.507(5) C3 H3 1.0000 C3 C4 1.511(5) C3 C6 1.545(5) C5 C6 1.508(5) C6 H6 1.0000 C6 C7 1.575(5) C7 C8 1.528(5) C7 C28 1.506(5) C8 C9 1.363(5) C8 C21 1.445(5) C9 C10 1.438(5) C10 C11 1.413(6) C10 C15 1.419(6) C11 H11 0.9500 C11 C12 1.377(6) C12 H12 0.9500 C12 C13 1.403(8) C13 H13 0.9500 C13 C14 1.360(8) C14 H14 0.9500 C14 C15 1.410(6) C15 C16 1.459(6) C16 C17 1.416(6) C16 C21 1.412(6) C17 H17 0.9500 C17 C18 1.364(7) C18 H18 0.9500 C18 C19 1.381(7) C19 H19 0.9500 C19 C20 1.376(6) C20 H20 0.9500 C20 C21 1.412(6) C22 C23 1.397(5) C22 C27 1.395(5) C23 H23 0.9500 C23 C24 1.374(5) C24 H24 0.9500 C24 C25 1.386(5) C25 H25 0.9500 C25 C26 1.396(6) C26 H26 0.9500 C26 C27 1.375(5) C27 H27 0.9500 C28 C29 1.404(5) C28 C33 1.381(5) C29 H29 0.9500 C29 C30 1.373(5) C30 H30 0.9500 C30 C31 1.383(6) C31 H31 0.9500 C31 C32 1.382(5) C32 H32 0.9500 C32 C33 1.382(5) C33 H33 0.9500 C34 C35 1.387(5) C34 C39 1.375(5) C35 C36 1.382(5) C36 H36 0.9500 C36 C37 1.374(6) C37 H37 0.9500 C37 C38 1.380(6) C38 H38 0.9500 C38 C39 1.380(5) C39 H39 0.9500 C40 C41 1.385(5) C40 C45 1.377(5) C41 H41 0.9500 C41 C42 1.384(5) C42 C43 1.394(5) C42 C46 1.516(6) C43 H43 0.9500 C43 C44 1.385(6) C44 C45 1.395(6) C44 C47 1.512(6) C45 H45 0.9500 C46 H46A 0.9800 C46 H46B 0.9800 C46 H46C 0.9800 C47 H47A 0.9800 C47 H47B 0.9800 C47 H47C 0.9800 Cl1 C81 1.758(9) Cl2 C81 1.727(10) Cl3 C81 1.741(9) C81 D81 1.0000 Cl4 C82 1.797(16) Cl5 C82 1.745(16) Cl6 C82 1.800(16) C82 D82 1.0000 Cl10 C84 1.775(13) Cl11 C84 1.728(13) Cl12 C84 1.703(13) C84 D84 1.0000 Cl7 C83 1.795(13) Cl8 C83 1.729(14) Cl9 C83 1.701(13) C83 D83 1.0000 Cl13 C85 1.782(18) Cl14 C85 1.720(18) Cl15 C85 1.753(18) C85 D85 1.0000 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 O1 C1 C2 C3 -124.4(4) O1 C1 C2 C9 129.4(4) O1 C1 C2 C22 0.0(5) O1 C1 C7 C6 122.0(4) O1 C1 C7 C8 -130.4(4) O1 C1 C7 C28 -3.8(5) O3 C5 C6 C3 -177.0(4) O3 C5 C6 C7 69.5(5) O4 C35 C36 C37 176.2(4) O4 C40 C41 C42 179.4(4) O4 C40 C45 C44 -178.2(4) N1 C5 C6 C3 4.1(4) N1 C5 C6 C7 -109.3(3) N1 C34 C35 O4 4.3(5) N1 C34 C35 C36 -178.2(3) N1 C34 C39 C38 179.3(3) C1 C2 C3 C4 -144.3(3) C1 C2 C3 C6 -30.8(3) C1 C2 C9 C8 33.5(3) C1 C2 C9 C10 -153.4(3) C1 C2 C22 C23 -134.3(3) C1 C2 C22 C27 43.8(5) C1 C7 C8 C9 -30.0(3) C1 C7 C8 C21 152.8(3) C1 C7 C28 C29 -52.4(4) C1 C7 C28 C33 128.6(4) C2 C1 C7 C6 -57.6(3) C2 C1 C7 C8 50.0(3) C2 C1 C7 C28 176.6(3) C2 C3 C4 O2 -60.9(5) C2 C3 C4 N1 118.6(3) C2 C3 C6 C5 -123.6(3) C2 C3 C6 C7 -3.6(3) C2 C9 C10 C11 4.0(6) C2 C9 C10 C15 -175.9(3) C2 C22 C23 C24 176.7(4) C2 C22 C27 C26 -176.6(3) C3 C2 C9 C8 -65.8(3) C3 C2 C9 C10 107.2(4) C3 C2 C22 C23 -20.8(5) C3 C2 C22 C27 157.3(3) C3 C6 C7 C1 36.7(3) C3 C6 C7 C8 -62.4(3) C3 C6 C7 C28 159.8(3) C4 N1 C5 O3 179.9(3) C4 N1 C5 C6 -1.3(4) C4 N1 C34 C35 -107.1(4) C4 N1 C34 C39 72.7(5) C4 C3 C6 C5 -5.3(3) C4 C3 C6 C7 114.7(3) C5 N1 C4 O2 177.1(3) C5 N1 C4 C3 -2.3(4) C5 N1 C34 C35 77.2(4) C5 N1 C34 C39 -103.0(4) C5 C6 C7 C1 150.6(3) C5 C6 C7 C8 51.5(4) C5 C6 C7 C28 -86.3(4) C6 C3 C4 O2 -174.7(3) C6 C3 C4 N1 4.7(4) C6 C7 C8 C9 69.3(3) C6 C7 C8 C21 -107.9(4) C6 C7 C28 C29 -166.1(3) C6 C7 C28 C33 15.0(5) C7 C1 C2 C3 55.2(3) C7 C1 C2 C9 -51.0(3) C7 C1 C2 C22 179.6(3) C7 C8 C9 C2 -2.4(4) C7 C8 C9 C10 -176.1(3) C7 C8 C21 C16 179.1(3) C7 C8 C21 C20 -0.5(5) C7 C28 C29 C30 -178.8(3) C7 C28 C33 C32 178.9(3) C8 C7 C28 C29 61.6(4) C8 C7 C28 C33 -117.4(4) C8 C9 C10 C11 176.4(3) C8 C9 C10 C15 -3.6(5) C9 C2 C3 C4 -46.2(4) C9 C2 C3 C6 67.3(3) C9 C2 C22 C23 110.5(4) C9 C2 C22 C27 -71.3(4) C9 C8 C21 C16 2.3(5) C9 C8 C21 C20 -177.4(3) C9 C10 C11 C12 178.1(3) C9 C10 C15 C14 -178.2(3) C9 C10 C15 C16 2.4(5) C10 C11 C12 C13 0.6(6) C10 C15 C16 C17 -179.9(3) C10 C15 C16 C21 1.1(5) C11 C10 C15 C14 1.9(5) C11 C10 C15 C16 -177.5(3) C11 C12 C13 C14 0.8(7) C12 C13 C14 C15 -0.8(7) C13 C14 C15 C10 -0.5(6) C13 C14 C15 C16 178.9(4) C14 C15 C16 C17 0.7(6) C14 C15 C16 C21 -178.3(3) C15 C10 C11 C12 -1.9(5) C15 C16 C17 C18 -178.8(4) C15 C16 C21 C8 -3.4(5) C15 C16 C21 C20 176.3(3) C16 C17 C18 C19 2.1(7) C17 C16 C21 C8 177.6(3) C17 C16 C21 C20 -2.8(5) C17 C18 C19 C20 -1.9(7) C18 C19 C20 C21 -0.7(6) C19 C20 C21 C8 -177.3(3) C19 C20 C21 C16 3.0(5) C21 C8 C9 C2 175.0(3) C21 C8 C9 C10 1.3(5) C21 C16 C17 C18 0.3(6) C22 C2 C3 C4 92.4(4) C22 C2 C3 C6 -154.1(3) C22 C2 C9 C8 158.1(3) C22 C2 C9 C10 -28.8(5) C22 C23 C24 C25 -0.5(6) C23 C22 C27 C26 1.6(5) C23 C24 C25 C26 2.1(6) C24 C25 C26 C27 -1.9(6) C25 C26 C27 C22 0.0(6) C27 C22 C23 C24 -1.4(6) C28 C7 C8 C9 -153.3(3) C28 C7 C8 C21 29.5(5) C28 C29 C30 C31 -0.2(6) C29 C28 C33 C32 -0.1(5) C29 C30 C31 C32 0.1(6) C30 C31 C32 C33 0.0(6) C31 C32 C33 C28 0.0(6) C33 C28 C29 C30 0.2(5) C34 N1 C4 O2 1.1(5) C34 N1 C4 C3 -178.4(3) C34 N1 C5 O3 -4.1(5) C34 N1 C5 C6 174.8(3) C34 C35 C36 C37 -1.1(6) C35 O4 C40 C41 73.2(5) C35 O4 C40 C45 -109.1(4) C35 C34 C39 C38 -0.8(6) C35 C36 C37 C38 -0.8(6) C36 C37 C38 C39 1.9(6) C37 C38 C39 C34 -1.1(6) C39 C34 C35 O4 -175.6(3) C39 C34 C35 C36 1.9(6) C40 O4 C35 C34 -148.8(3) C40 O4 C35 C36 33.8(5) C40 C41 C42 C43 -1.7(6) C40 C41 C42 C46 179.0(4) C41 C40 C45 C44 -0.4(6) C41 C42 C43 C44 0.5(6) C42 C43 C44 C45 0.7(6) C42 C43 C44 C47 179.8(4) C43 C44 C45 C40 -0.8(6) C45 C40 C41 C42 1.7(6) C46 C42 C43 C44 179.8(4) C47 C44 C45 C40 -179.8(4)