#------------------------------------------------------------------------------ #$Date: 2020-04-23 23:27:30 +0300 (Thu, 23 Apr 2020) $ #$Revision: 251105 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557890.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_1557890 loop_ _publ_author_name 'Zhou, Jia' 'Gao, Ying' 'Chang, Jin-Ling' 'Yu, Heng-Yi' 'Chen, Juan' 'Zhou, Ming' 'Meng, Xiang-Gao' 'Ruan, Han-Li' _publ_section_title ; Resorcylic Acid Lactones from an Ilyonectria sp. ; _journal_name_full 'Journal of Natural Products' _journal_paper_doi 10.1021/acs.jnatprod.9b01167 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C20 H23 Cl O6' _chemical_formula_sum 'C20 H23 Cl O6' _chemical_formula_weight 394.83 _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_Hall 'C 2y' _space_group_name_H-M_alt 'C 1 2 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2019-10-14 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 131.699(3) _cell_angle_gamma 90 _cell_formula_units_Z 16 _cell_length_a 36.0878(7) _cell_length_b 10.82580(10) _cell_length_c 26.8601(9) _cell_measurement_reflns_used 19738 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 4.393 _cell_measurement_theta_min 73.380 _cell_volume 7835.1(5) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _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 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_unetI/netI 0.0370 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 44030 _diffrn_reflns_point_group_measured_fraction_full 0.886 _diffrn_reflns_point_group_measured_fraction_max 0.861 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 73.929 _diffrn_reflns_theta_min 3.280 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.017 _exptl_absorpt_correction_T_max 0.906 _exptl_absorpt_correction_T_min 0.752 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.339 _exptl_crystal_description block _exptl_crystal_F_000 3328 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.516 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.041 _refine_ls_abs_structure_details ; Flack x determined using 3903 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.015(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1018 _refine_ls_number_reflns 13690 _refine_ls_number_restraints 54 _refine_ls_restrained_S_all 1.067 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0482 _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^)+(0.0856P)^2^+2.3362P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1380 _refine_ls_wR_factor_ref 0.1452 _reflns_Friedel_coverage 0.651 _reflns_Friedel_fraction_full 0.758 _reflns_Friedel_fraction_max 0.718 _reflns_number_gt 11563 _reflns_number_total 13690 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file np9b01167_si_004.cif _cod_data_source_block t _cod_original_cell_volume 7835.1(4) _cod_database_code 1557890 _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. ; _shelx_estimated_absorpt_t_max 0.906 _shelx_estimated_absorpt_t_min 0.752 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances C2C-C1C 1.51 with sigma of 0.01 C4C-C3C = C4C-C3D = C3D-C2D = C3C-C2C = C2D-C1D = C2C-C1C 1.51 with sigma of 0.01 O2C-C2D = O2C-C2C 1.42 with sigma of 0.01 C1C-C2C \\sim C1D-C2D with sigma of 0.02 C2C-C3C \\sim C2D-C3D with sigma of 0.02 C2C-O2C \\sim C2D-O2C with sigma of 0.02 C3C-C4C \\sim C3D-C4C with sigma of 0.02 C1C-C3C \\sim C1D-C3D with sigma of 0.04 C1C-O2C \\sim C1D-O2C with sigma of 0.04 C2C-C4C \\sim C2D-C4C with sigma of 0.04 C3C-O2C \\sim C3D-O2C with sigma of 0.04 3. Uiso/Uaniso restraints and constraints Uanis(O1C) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Others Sof(H4CA)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=Sof(C2D)=Sof(H2D)=Sof(C3D)= Sof(H3DA)=Sof(H3DB)=1-FVAR(1) Sof(H4C)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=Sof(C2C)=Sof(H2C)=Sof(C3C)= Sof(H3CA)=Sof(H3CB)=FVAR(1) 5.a Ternary CH refined with riding coordinates: C2(H2), C10(H10), C2A(H2A), C10A(H10A), C2B(H2B), C10B(H10B), C10C(H10C), C2C(H2C), C2D(H2D) 5.b Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C11(H11C,H11D), C13(H13C,H13D), C3A(H3AA,H3AB), C6A(H6AA,H6AB), C7A(H7AA,H7AB), C11A(H11E,H11F), C13A(H13E, H13F), C3B(H3BA,H3BB), C6B(H6BA,H6BB), C7B(H7BA,H7BB), C11B(H11G,H11H), C13B(H13G,H13H), C6C(H6CA,H6CB), C7C(H7CA,H7CB), C11C(H11A,H11B), C13C(H13A, H13B), C3C(H3CA,H3CB), C3D(H3DA,H3DB) 5.c Aromatic/amide H refined with riding coordinates: C4(H4), C5(H5), C8(H8), C9(H9), C17(H17), C4A(H4A), C5A(H5AA), C8A(H8A), C9A(H9A), C17A(H17A), C4B(H4B), C5B(H5B), C8B(H8B), C9B(H9B), C17B(H17B), C4C(H4C), C4C(H4CA), C5C(H5C), C8C(H8C), C9C(H9C), C17C(H17C) 5.d Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB, H1CC), C1D(H1DA,H1DB,H1DC) 5.e Idealised tetrahedral OH refined as rotating group: O3(H3), O5(H5A), O6(H6), O3A(H3AC), O5A(H5AB), O6A(H6AC), O3B(H3BC), O5B(H5BA), O6B(H6BC), O3C(H3C), O5C(H5CA), O6C(H6C) ; _shelx_res_file ; t.res created by SHELXL-2014/7 TITL t in C2 #5 REM reset to C5C #5 CELL 1.54178 36.0878 10.8258 26.8601 90 131.699 90 ZERR 16 0.0007 0.0001 0.0009 0 0.003 0 LATT -7 SYMM -X,+Y,-Z SFAC C H Cl O UNIT 320 368 16 96 EQIV $1 +X,1+Y,+Z EQIV $2 -X,+Y,-Z EQIV $3 0.5-X,0.5+Y,-Z EQIV $4 -X,-1+Y,-Z DFIX 1.51 0.01 C2C C1C DFIX 1.51 0.01 C4C C3C C4C C3D C3D C2D C3C C2C C2D C1D C2C C1C DFIX 1.42 0.01 O2C C2D O2C C2C SADI C1C C2C C1D C2D SADI C2C C3C C2D C3D SADI C2C O2C C2D O2C SADI C3C C4C C3D C4C SADI 0.04 C1C C3C C1D C3D SADI 0.04 C1C O2C C1D O2C SADI 0.04 C2C C4C C2D C4C SADI 0.04 C3C O2C C3D O2C ISOR 0.01 0.02 O1C C5 C6 C7 C8 C9 L.S. 10 PLAN 10 SIZE 0.15 0.1 0.05 TEMP 20(2) HTAB O5 O3B_$1 HTAB O6 O1 HTAB C13A O2A HTAB O6A O1A HTAB O5B O3 HTAB O6B O1B HTAB O5C O3A_$2 HTAB O6C O1C HTAB O3A O1B_$3 HTAB O5A O3C_$4 HTAB CONF BOND fmap 2 acta REM REM REM WGHT 0.085600 2.336200 FVAR 0.16856 0.53599 C1 1 0.469252 0.304333 0.690260 11.00000 0.11853 0.05695 = 0.10502 -0.00213 0.08080 -0.00150 AFIX 137 H1A 2 0.458272 0.244593 0.704454 11.00000 -1.50000 H1B 2 0.488639 0.263878 0.682420 11.00000 -1.50000 H1C 2 0.440958 0.343026 0.649854 11.00000 -1.50000 AFIX 0 C2 1 0.500175 0.399956 0.743206 11.00000 0.10023 0.06246 = 0.07046 0.00615 0.06022 -0.00353 AFIX 13 H2 2 0.527248 0.359455 0.785490 11.00000 -1.20000 AFIX 0 C3 1 0.471739 0.480879 0.752843 11.00000 0.11372 0.07512 = 0.09078 -0.01110 0.08064 -0.01879 AFIX 23 H3A 2 0.458790 0.430453 0.768146 11.00000 -1.20000 H3B 2 0.494279 0.540835 0.787443 11.00000 -1.20000 AFIX 0 C4 1 0.429855 0.547709 0.691456 11.00000 0.09605 0.08680 = 0.12594 -0.02747 0.08905 -0.01641 AFIX 43 H4 2 0.438374 0.610428 0.677008 11.00000 -1.20000 AFIX 0 C5 1 0.381841 0.528014 0.655076 11.00000 0.11490 0.14886 = 0.14281 -0.04573 0.10596 -0.02321 AFIX 43 H5 2 0.372628 0.462593 0.667291 11.00000 -1.20000 AFIX 0 C6 1 0.341703 0.602156 0.596450 11.00000 0.08887 0.19670 = 0.13448 -0.05377 0.07826 0.00881 AFIX 23 H6A 2 0.355544 0.677789 0.595327 11.00000 -1.20000 H6B 2 0.317732 0.624455 0.600427 11.00000 -1.20000 AFIX 0 C7 1 0.315392 0.530476 0.531227 11.00000 0.09374 0.19424 = 0.12798 -0.04700 0.08461 -0.01105 AFIX 23 H7A 2 0.314216 0.443449 0.538689 11.00000 -1.20000 H7B 2 0.281553 0.559950 0.497707 11.00000 -1.20000 AFIX 0 C8 1 0.342217 0.546689 0.506432 11.00000 0.07819 0.14374 = 0.10886 -0.03909 0.06329 -0.00564 AFIX 43 H8 2 0.342479 0.626139 0.493500 11.00000 -1.20000 AFIX 0 C9 1 0.364256 0.465401 0.501204 11.00000 0.06747 0.10954 = 0.07654 -0.02296 0.05246 -0.01614 AFIX 43 H9 2 0.365487 0.386947 0.516355 11.00000 -1.20000 AFIX 0 C10 1 0.388599 0.479652 0.473693 11.00000 0.05309 0.06994 = 0.05238 -0.00596 0.03376 -0.00001 AFIX 13 H10 2 0.384376 0.564830 0.458315 11.00000 -1.20000 AFIX 0 C11 1 0.443194 0.448005 0.523083 11.00000 0.05236 0.06453 = 0.05034 -0.00611 0.02996 0.00103 AFIX 23 H11C 2 0.447399 0.369966 0.544077 11.00000 -1.20000 H11D 2 0.454157 0.436245 0.498813 11.00000 -1.20000 AFIX 0 C12 1 0.476345 0.542587 0.576955 11.00000 0.04845 0.05670 = 0.04424 0.00072 0.02955 0.00337 C13 1 0.530513 0.505817 0.628318 11.00000 0.04999 0.05973 = 0.04149 -0.00230 0.02578 0.00658 AFIX 23 H13C 2 0.533466 0.434493 0.652615 11.00000 -1.20000 H13D 2 0.541530 0.481135 0.605256 11.00000 -1.20000 AFIX 0 C14 1 0.564529 0.605870 0.677672 11.00000 0.04081 0.06498 = 0.04342 -0.00114 0.02310 0.00936 C15 1 0.580613 0.695652 0.659290 11.00000 0.04471 0.06966 = 0.04534 -0.00292 0.02690 0.00351 C16 1 0.613956 0.788651 0.702611 11.00000 0.04411 0.06585 = 0.05636 -0.00395 0.03077 0.00428 C17 1 0.632729 0.790442 0.767083 11.00000 0.04800 0.07737 = 0.05171 -0.01401 0.02705 -0.00368 AFIX 43 H17 2 0.655178 0.851297 0.796638 11.00000 -1.20000 AFIX 0 C18 1 0.617921 0.700934 0.787567 11.00000 0.05105 0.08428 = 0.04376 -0.01015 0.02610 -0.00010 C19 1 0.582637 0.610701 0.743481 11.00000 0.04761 0.07359 = 0.04028 0.00085 0.02423 0.00570 C20 1 0.565009 0.530068 0.768250 11.00000 0.06685 0.07327 = 0.04479 -0.00023 0.03264 0.00163 CL1 3 0.558720 0.699430 0.578777 11.00000 0.06772 0.09277 = 0.04967 -0.00479 0.03800 -0.00873 O1 4 0.587238 0.518853 0.827471 11.00000 0.10474 0.12595 = 0.04830 0.00626 0.04126 -0.01819 O2 4 0.521076 0.476537 0.721598 11.00000 0.06781 0.07335 = 0.05431 0.00579 0.03931 -0.00200 O3 4 0.365944 0.396523 0.418256 11.00000 0.04924 0.11533 = 0.05617 -0.02380 0.02838 -0.00288 AFIX 147 H3 2 0.335700 0.398588 0.394515 11.00000 -1.50000 AFIX 0 O4 4 0.461300 0.641240 0.577900 11.00000 0.05703 0.06000 = 0.07709 -0.00724 0.03623 0.00438 O5 4 0.629212 0.878957 0.685416 11.00000 0.06244 0.07922 = 0.07097 -0.00436 0.04409 -0.00830 AFIX 147 H5A 2 0.623928 0.858481 0.651783 11.00000 -1.50000 AFIX 0 O6 4 0.639531 0.706056 0.852283 11.00000 0.07308 0.11934 = 0.04164 -0.01758 0.02992 -0.01530 AFIX 147 H6 2 0.624273 0.661605 0.858056 11.00000 -1.50000 AFIX 0 C1A 1 0.291853 0.660985 0.301203 11.00000 0.10883 0.09820 = 0.11833 -0.03103 0.07521 -0.04395 AFIX 137 H1AA 2 0.325352 0.677750 0.321019 11.00000 -1.50000 H1AB 2 0.291497 0.636899 0.335279 11.00000 -1.50000 H1AC 2 0.272042 0.733916 0.279206 11.00000 -1.50000 AFIX 0 C2A 1 0.271063 0.558661 0.251457 11.00000 0.05995 0.07932 = 0.07711 -0.01263 0.04499 -0.02084 AFIX 13 H2A 2 0.293345 0.487165 0.272453 11.00000 -1.20000 AFIX 0 C3A 1 0.261455 0.594115 0.190236 11.00000 0.07542 0.08823 = 0.08620 -0.00369 0.05629 -0.01822 AFIX 23 H3AA 2 0.291403 0.630599 0.203387 11.00000 -1.20000 H3AB 2 0.235809 0.656981 0.166798 11.00000 -1.20000 AFIX 0 C4A 1 0.245766 0.490145 0.143219 11.00000 0.06122 0.09175 = 0.07428 -0.00609 0.04535 -0.01259 AFIX 43 H4A 2 0.224168 0.432039 0.137368 11.00000 -1.20000 AFIX 0 C5A 1 0.259706 0.473725 0.109655 11.00000 0.05210 0.11012 = 0.07263 0.01156 0.03936 0.00820 AFIX 43 H5AA 2 0.284496 0.525807 0.119992 11.00000 -1.20000 AFIX 0 C6A 1 0.240130 0.380568 0.056667 11.00000 0.06353 0.12384 = 0.08041 0.00014 0.04609 0.02346 AFIX 23 H6AA 2 0.227168 0.310789 0.063633 11.00000 -1.20000 H6AB 2 0.267102 0.350883 0.060064 11.00000 -1.20000 AFIX 0 C7A 1 0.199320 0.432266 -0.013002 11.00000 0.06049 0.15949 = 0.06935 -0.00257 0.04325 0.01807 AFIX 23 H7AA 2 0.210082 0.510598 -0.017199 11.00000 -1.20000 H7AB 2 0.193545 0.375841 -0.045612 11.00000 -1.20000 AFIX 0 C8A 1 0.152011 0.450859 -0.027388 11.00000 0.05626 0.09630 = 0.05724 -0.00070 0.03576 0.00962 AFIX 43 H8A 2 0.131722 0.381762 -0.042519 11.00000 -1.20000 AFIX 0 C9A 1 0.135716 0.550752 -0.021472 11.00000 0.05629 0.08271 = 0.05087 0.00179 0.03471 0.00199 AFIX 43 H9A 2 0.155919 0.620230 -0.005395 11.00000 -1.20000 AFIX 0 C10A 1 0.087611 0.564931 -0.038000 11.00000 0.05102 0.06486 = 0.04511 0.00275 0.03080 0.00547 AFIX 13 H10A 2 0.070166 0.485500 -0.053733 11.00000 -1.20000 AFIX 0 C11A 1 0.093064 0.609469 0.020723 11.00000 0.06318 0.06221 = 0.04635 0.00668 0.03616 0.01267 AFIX 23 H11E 2 0.116536 0.677384 0.042376 11.00000 -1.20000 H11F 2 0.061286 0.641159 0.003493 11.00000 -1.20000 AFIX 0 C12A 1 0.110280 0.511594 0.072436 11.00000 0.04309 0.05653 = 0.04416 -0.00013 0.02718 0.00067 C13A 1 0.120000 0.557098 0.133515 11.00000 0.05086 0.05680 = 0.04172 -0.00064 0.02775 0.00323 AFIX 23 H13E 2 0.092816 0.610321 0.119238 11.00000 -1.20000 H13F 2 0.150016 0.606566 0.160211 11.00000 -1.20000 AFIX 0 C14A 1 0.125677 0.454902 0.176928 11.00000 0.04609 0.06255 = 0.04138 0.00274 0.02929 0.00810 C15A 1 0.082509 0.395422 0.153547 11.00000 0.04293 0.07593 = 0.03982 -0.00325 0.02507 0.00123 C16A 1 0.082327 0.303842 0.189587 11.00000 0.05138 0.07901 = 0.05778 -0.00740 0.03959 -0.00675 C17A 1 0.126127 0.273794 0.252255 11.00000 0.05757 0.07907 = 0.05471 0.00979 0.03891 0.00185 AFIX 43 H17A 2 0.126343 0.214402 0.277463 11.00000 -1.20000 AFIX 0 C18A 1 0.169289 0.331288 0.277402 11.00000 0.04852 0.08549 = 0.04715 0.01281 0.02874 0.01083 C19A 1 0.170813 0.419435 0.239604 11.00000 0.04181 0.06527 = 0.04229 0.00158 0.02576 0.00352 C20A 1 0.220328 0.461658 0.267660 11.00000 0.04773 0.06610 = 0.04782 -0.00243 0.02853 -0.00406 CL1A 3 0.025831 0.436316 0.076778 11.00000 0.04376 0.13782 = 0.04813 0.01049 0.02195 0.00220 O1A 4 0.258381 0.432218 0.324019 11.00000 0.04324 0.12978 = 0.05318 0.00682 0.01974 -0.00839 O2A 4 0.221609 0.523790 0.227099 11.00000 0.05404 0.07147 = 0.06253 -0.00488 0.03744 -0.01100 O3A 4 0.057127 0.656288 -0.089913 11.00000 0.06485 0.10020 = 0.04870 0.01661 0.03772 0.02019 AFIX 147 H3AC 2 0.062833 0.655164 -0.114798 11.00000 -1.50000 AFIX 0 O4A 4 0.114691 0.404916 0.064833 11.00000 0.08038 0.05323 = 0.06230 -0.00058 0.05010 0.00397 O5A 4 0.041358 0.241912 0.166756 11.00000 0.06209 0.12029 = 0.07445 -0.00229 0.04795 -0.02102 AFIX 147 H5AB 2 0.018058 0.262384 0.128110 11.00000 -1.50000 AFIX 0 O6A 4 0.210202 0.297081 0.339987 11.00000 0.05444 0.14717 = 0.05620 0.03985 0.02500 0.00873 AFIX 147 H6AC 2 0.234696 0.331502 0.350228 11.00000 -1.50000 AFIX 0 C1B 1 0.476630 -0.180943 0.214691 11.00000 0.09482 0.09644 = 0.10418 -0.03251 0.07361 -0.01559 AFIX 137 H1BA 2 0.490756 -0.222578 0.199121 11.00000 -1.50000 H1BB 2 0.443695 -0.153646 0.177205 11.00000 -1.50000 H1BC 2 0.475278 -0.236636 0.241262 11.00000 -1.50000 AFIX 0 C2B 1 0.508235 -0.071155 0.256212 11.00000 0.06776 0.07170 = 0.06835 -0.00380 0.05224 0.00455 AFIX 13 H2B 2 0.509873 -0.013736 0.229518 11.00000 -1.20000 AFIX 0 C3B 1 0.559823 -0.106926 0.318464 11.00000 0.07702 0.07242 = 0.08663 0.01158 0.06308 0.01844 AFIX 23 H3BA 2 0.557417 -0.157523 0.346020 11.00000 -1.20000 H3BB 2 0.574774 -0.157009 0.305908 11.00000 -1.20000 AFIX 0 C4B 1 0.593455 0.000699 0.359245 11.00000 0.06274 0.07408 = 0.06885 0.01115 0.04543 0.01172 AFIX 43 H4B 2 0.580452 0.063897 0.367113 11.00000 -1.20000 AFIX 0 C5B 1 0.638843 0.014074 0.384542 11.00000 0.06392 0.12751 = 0.07558 0.01950 0.05160 0.00969 AFIX 43 H5B 2 0.651686 -0.044979 0.374426 11.00000 -1.20000 AFIX 0 C6B 1 0.671974 0.119858 0.429405 11.00000 0.07590 0.14393 = 0.08928 0.00844 0.05868 -0.02059 AFIX 23 H6BA 2 0.651786 0.192055 0.418238 11.00000 -1.20000 H6BB 2 0.694213 0.139992 0.422067 11.00000 -1.20000 AFIX 0 C7B 1 0.702660 0.087235 0.503355 11.00000 0.05596 0.18744 = 0.07141 0.00660 0.03894 -0.01840 AFIX 23 H7BA 2 0.718143 0.007191 0.512492 11.00000 -1.20000 H7BB 2 0.728801 0.147927 0.530974 11.00000 -1.20000 AFIX 0 C8B 1 0.671475 0.084056 0.520941 11.00000 0.05909 0.11868 = 0.06272 0.00640 0.03800 -0.01095 AFIX 43 H8B 2 0.667568 0.157821 0.534756 11.00000 -1.20000 AFIX 0 C9B 1 0.648696 -0.014542 0.518711 11.00000 0.05252 0.08601 = 0.05524 0.01198 0.03390 0.01319 AFIX 43 H9B 2 0.652600 -0.088782 0.505225 11.00000 -1.20000 AFIX 0 C10B 1 0.617370 -0.015126 0.536190 11.00000 0.05078 0.06925 = 0.04717 0.01052 0.03143 0.00327 AFIX 13 H10B 2 0.617538 0.068203 0.550594 11.00000 -1.20000 AFIX 0 C11B 1 0.564394 -0.053523 0.480867 11.00000 0.05124 0.06227 = 0.04999 0.01154 0.02882 0.00180 AFIX 23 H11G 2 0.550767 -0.079495 0.500432 11.00000 -1.20000 H11H 2 0.564089 -0.124762 0.458694 11.00000 -1.20000 AFIX 0 C12B 1 0.530644 0.043690 0.428943 11.00000 0.04518 0.05230 = 0.04149 0.00254 0.02861 -0.00045 C13B 1 0.477031 0.003811 0.374066 11.00000 0.04598 0.05555 = 0.04257 0.00461 0.02852 -0.00111 AFIX 23 H13G 2 0.476237 -0.061887 0.348813 11.00000 -1.20000 H13H 2 0.465286 -0.030572 0.394767 11.00000 -1.20000 AFIX 0 C14B 1 0.441228 0.103016 0.325936 11.00000 0.03685 0.05817 = 0.04048 -0.00010 0.02399 -0.00399 C15B 1 0.421327 0.179706 0.344472 11.00000 0.04063 0.06584 = 0.04001 -0.00261 0.02551 -0.00337 C16B 1 0.384149 0.266597 0.301344 11.00000 0.04324 0.07783 = 0.05301 0.00172 0.03139 0.00690 C17B 1 0.365575 0.275720 0.237343 11.00000 0.05087 0.10198 = 0.04846 0.01277 0.02944 0.01916 AFIX 43 H17B 2 0.339793 0.330307 0.207528 11.00000 -1.20000 AFIX 0 C18B 1 0.385151 0.203857 0.217163 11.00000 0.04920 0.09700 = 0.04121 0.01486 0.02732 0.01484 C19B 1 0.424264 0.118273 0.260915 11.00000 0.04162 0.06844 = 0.03989 0.00206 0.02582 0.00169 C20B 1 0.446817 0.061088 0.237397 11.00000 0.05038 0.07190 = 0.04467 -0.00022 0.03137 -0.00165 CL1B 3 0.442303 0.174150 0.424110 11.00000 0.06766 0.10176 = 0.04744 0.00552 0.04009 0.01200 O1B 4 0.431098 0.077911 0.180922 11.00000 0.07308 0.13064 = 0.04770 0.01037 0.04165 0.02235 O2B 4 0.486299 -0.009167 0.280316 11.00000 0.05738 0.07043 = 0.05413 0.00160 0.04028 0.00695 O3B 4 0.638062 -0.098797 0.590738 11.00000 0.05164 0.11618 = 0.05523 0.02992 0.03028 0.01107 AFIX 147 H3BC 2 0.668284 -0.101604 0.614351 11.00000 -1.50000 AFIX 0 O4B 4 0.544660 0.145941 0.431314 11.00000 0.05158 0.05539 = 0.06480 0.00610 0.03036 -0.00325 O5B 4 0.364501 0.340815 0.318130 11.00000 0.06736 0.11546 = 0.06552 0.00619 0.04424 0.03212 AFIX 147 H5BA 2 0.373912 0.319230 0.354239 11.00000 -1.50000 AFIX 0 O6B 4 0.364526 0.219893 0.153409 11.00000 0.07944 0.15250 = 0.04563 0.02926 0.03906 0.04441 AFIX 147 H6BC 2 0.381910 0.186581 0.147789 11.00000 -1.50000 AFIX 0 C4C 1 0.234564 0.965087 0.153358 11.00000 0.09409 0.14213 = 0.12145 -0.05568 0.08244 -0.04000 PART 1 AFIX 43 H4C 2 0.204216 0.931821 0.135839 21.00000 -1.20000 AFIX 43 PART 0 PART 2 H4CA 2 0.223309 0.893865 0.159026 -21.00000 -1.20000 AFIX 0 PART 0 C5C 1 0.242292 0.968741 0.112504 11.00000 0.07789 0.12810 = 0.10187 -0.00496 0.06349 0.00210 AFIX 43 H5C 2 0.266714 1.022086 0.122655 11.00000 -1.20000 AFIX 0 C6C 1 0.215060 0.894269 0.051232 11.00000 0.11695 0.15261 = 0.09483 0.01903 0.07954 0.03716 AFIX 23 H6CA 2 0.199695 0.824760 0.054284 11.00000 -1.20000 H6CB 2 0.238479 0.861609 0.048100 11.00000 -1.20000 AFIX 0 C7C 1 0.175275 0.966544 -0.011748 11.00000 0.14049 0.18124 = 0.09463 0.04819 0.08657 0.06911 AFIX 23 H7CA 2 0.189595 1.043587 -0.010507 11.00000 -1.20000 H7CB 2 0.165314 0.919743 -0.049780 11.00000 -1.20000 AFIX 0 C8C 1 0.130859 0.994812 -0.022044 11.00000 0.08236 0.12651 = 0.06048 0.00935 0.04213 0.00810 AFIX 43 H8C 2 0.106134 0.934879 -0.044493 11.00000 -1.20000 AFIX 0 C9C 1 0.121481 1.092231 -0.004012 11.00000 0.06523 0.09256 = 0.06333 0.02044 0.03520 0.00427 AFIX 43 H9C 2 0.145621 1.153627 0.017849 11.00000 -1.20000 AFIX 0 C10C 1 0.075811 1.115798 -0.014813 11.00000 0.05728 0.06993 = 0.06734 0.00713 0.03158 -0.00145 AFIX 13 H10C 2 0.051921 1.050272 -0.043870 11.00000 -1.20000 AFIX 0 C11C 1 0.082919 1.117462 0.045914 11.00000 0.08115 0.06695 = 0.09005 0.01348 0.05537 0.00123 AFIX 23 H11A 2 0.052644 1.149165 0.033638 11.00000 -1.20000 H11B 2 0.108952 1.176684 0.076421 11.00000 -1.20000 AFIX 0 C12C 1 0.095727 0.999672 0.083770 11.00000 0.05503 0.05563 = 0.06221 -0.00131 0.03411 -0.00585 C13C 1 0.101202 1.016657 0.144331 11.00000 0.07710 0.05142 = 0.08151 -0.00911 0.05465 -0.00335 AFIX 23 H13A 2 0.126580 1.078495 0.172916 11.00000 -1.20000 H13B 2 0.070210 1.049013 0.129575 11.00000 -1.20000 AFIX 0 C14C 1 0.114482 0.902310 0.185424 11.00000 0.06168 0.05695 = 0.05872 -0.00951 0.04283 -0.00269 C15C 1 0.075727 0.826284 0.165693 11.00000 0.05440 0.06036 = 0.05265 -0.00260 0.03503 0.00500 C16C 1 0.082129 0.726850 0.203659 11.00000 0.05509 0.07071 = 0.05129 -0.00228 0.03754 -0.00195 C17C 1 0.129114 0.702391 0.263039 11.00000 0.05921 0.09096 = 0.05167 0.00970 0.03799 0.00797 AFIX 43 H17C 2 0.133850 0.638397 0.289877 11.00000 -1.20000 AFIX 0 C18C 1 0.168841 0.770316 0.283220 11.00000 0.05284 0.10920 = 0.04746 0.00308 0.03253 0.00461 C19C 1 0.163055 0.871680 0.244831 11.00000 0.05052 0.09220 = 0.04807 -0.01461 0.03192 -0.00824 C20C 1 0.208515 0.934148 0.268278 11.00000 0.06748 0.10395 = 0.05855 -0.02361 0.04303 -0.02546 CL1C 3 0.015522 0.852152 0.090750 11.00000 0.05471 0.08443 = 0.07058 0.01530 0.03064 0.00531 O1C 4 0.249281 0.914898 0.322983 11.00000 0.06030 0.18459 = 0.07062 -0.02255 0.03638 -0.03323 O2C 4 0.203297 1.010149 0.224790 11.00000 0.09108 0.11179 = 0.08959 -0.04241 0.06887 -0.04915 O3C 4 0.053643 1.233043 -0.049395 11.00000 0.06696 0.07973 = 0.07219 0.02255 0.03005 0.00840 AFIX 147 H3C 2 0.071584 1.290021 -0.024377 11.00000 -1.50000 AFIX 0 O4C 4 0.100056 0.901582 0.067650 11.00000 0.12000 0.05584 = 0.07549 -0.00464 0.06867 -0.00411 O5C 4 0.045020 0.653619 0.186937 11.00000 0.06357 0.08147 = 0.06504 0.00785 0.03921 -0.00656 AFIX 147 H5CA 2 0.018753 0.675652 0.150859 11.00000 -1.50000 AFIX 0 O6C 4 0.213445 0.736521 0.341423 11.00000 0.05368 0.19676 = 0.05952 0.03211 0.02711 0.00345 AFIX 147 H6C 2 0.235482 0.762747 0.342909 11.00000 -1.50000 AFIX 0 PART 1 C1C 1 0.218172 1.202989 0.190514 21.00000 0.07308 0.05972 = 0.10928 0.00281 0.05665 0.00158 AFIX 137 H1CA 2 0.244297 1.258036 0.203948 21.00000 -1.50000 H1CB 2 0.196194 1.244922 0.193359 21.00000 -1.50000 H1CC 2 0.199999 1.176788 0.145401 21.00000 -1.50000 AFIX 0 C2C 1 0.240093 1.092363 0.235580 21.00000 0.08329 0.07662 = 0.06542 -0.00367 0.04855 -0.02221 AFIX 13 H2C 2 0.262455 1.121100 0.281907 21.00000 -1.20000 AFIX 0 C3C 1 0.268516 1.008055 0.227048 21.00000 0.04864 0.08498 = 0.07896 0.03175 0.03686 0.01245 AFIX 23 H3CA 2 0.280186 0.936829 0.255998 21.00000 -1.20000 H3CB 2 0.297179 1.051109 0.239388 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C1D 1 0.275229 1.150582 0.303815 -21.00000 0.11881 0.09153 = 0.08872 -0.02182 0.06618 -0.02436 AFIX 137 H1DA 2 0.251722 1.216898 0.285440 -21.00000 -1.50000 H1DB 2 0.305158 1.180489 0.315376 -21.00000 -1.50000 H1DC 2 0.282590 1.119247 0.343004 -21.00000 -1.50000 AFIX 0 C2D 1 0.253612 1.048821 0.253044 -21.00000 0.07220 0.06788 = 0.05491 -0.00742 0.03868 -0.02146 AFIX 13 H2D 2 0.275848 0.977233 0.273998 -21.00000 -1.20000 AFIX 0 C3D 1 0.244983 1.084526 0.191813 -21.00000 0.06120 0.09669 = 0.08871 0.00942 0.04485 -0.01344 AFIX 23 H3DA 2 0.274049 1.125729 0.204444 -21.00000 -1.20000 H3DB 2 0.216920 1.140305 0.164234 -21.00000 -1.20000 AFIX 0 HKLF 4 REM t in C2 #5 REM R1 = 0.0482 for 11563 Fo > 4sig(Fo) and 0.0567 for all 13690 data REM 1018 parameters refined using 54 restraints END WGHT 0.0856 2.3363 REM Instructions for potential hydrogen bonds EQIV $5 -x+1, y, -z+1 HTAB C11 O4B_$5 HTAB C13 O2 HTAB O3 O1A HTAB O5 Cl1 HTAB O5 O3B_$1 HTAB O6 O1 HTAB C1A O1A HTAB C2A O5B HTAB C13A O2A HTAB O3A O1B_$3 HTAB O5A Cl1A HTAB O5A O3C_$4 HTAB O6A O1A EQIV $6 x+1/2, y-1/2, z HTAB C1B O5A_$6 HTAB C1B O1B HTAB C10B Cl1B_$5 EQIV $7 -x+1, y-1, -z+1 HTAB C11B O4_$7 HTAB C13B O2B HTAB O3B O1C_$7 HTAB O5B O3 HTAB O5B Cl1B HTAB O6B O1B HTAB C10C Cl1C_$2 HTAB C11C O4A_$1 HTAB C13C O2C HTAB O3C O4A_$1 HTAB O5C O3A_$2 HTAB O5C Cl1C HTAB O6C O1C HTAB C3C O5_$5 HTAB C1D O1A_$1 HTAB C1D O1C REM Highest difference peak 0.516, deepest hole -0.233, 1-sigma level 0.041 Q1 1 0.0207 0.3388 0.0822 11.00000 0.05 0.52 Q2 1 0.0521 1.1476 -0.0837 11.00000 0.05 0.37 Q3 1 0.2860 0.5306 0.2303 11.00000 0.05 0.28 Q4 1 0.0540 0.1494 0.1904 11.00000 0.05 0.27 Q5 1 0.0856 1.0497 -0.0314 11.00000 0.05 0.26 Q6 1 0.2353 0.7112 0.1888 11.00000 0.05 0.26 Q7 1 0.0229 0.9307 0.0766 11.00000 0.05 0.25 Q8 1 0.0495 0.4310 0.0626 11.00000 0.05 0.24 Q9 1 0.2125 0.8317 0.3489 11.00000 0.05 0.24 Q10 1 0.1679 0.8441 0.2811 11.00000 0.05 0.20 ; _shelx_res_checksum 6606 _shelx_hkl_file ; 0 10 -8 -0.57 1.15 0 10 -9 0.19 1.19 0 10 -10 3.60 1.22 0 10 -11 0.94 1.19 0 10 -12 1.15 1.17 0 10 -13 3.20 1.11 0 10 -14 1.60 0.97 0 10 -15 7.10 1.00 0 10 -16 1.13 0.58 0 10 -16 0.08 0.66 0 8 -12 13.38 1.85 0 8 -13 22.61 2.13 0 8 -14 10.51 1.75 0 8 -17 13.84 1.53 0 8 -18 3.56 1.11 0 8 -19 3.39 0.88 0 8 -20 0.33 0.54 0 6 0 41.30 2.42 0 6 0 39.80 2.42 0 6 -1 104.08 5.41 0 6 -1 108.20 5.42 0 6 -2 1.21 0.76 0 6 2 0.74 0.70 0 6 2 0.34 0.76 0 6 -2 -0.19 0.77 0 6 3 56.37 3.06 0 6 3 54.46 3.14 0 6 3 55.95 3.11 0 6 3 58.79 2.99 0 6 3 53.68 2.93 0 6 -3 59.62 3.11 0 6 -3 52.98 3.11 0 6 -4 323.88 15.98 0 6 4 347.23 16.00 0 6 4 328.42 15.94 0 6 4 340.06 15.89 0 6 -4 333.88 15.96 0 6 5 109.94 5.48 0 6 -5 108.15 5.50 0 6 5 107.42 5.54 0 6 -6 114.75 5.83 0 6 6 117.32 5.79 0 6 -14 95.85 5.05 0 6 -14 93.34 4.79 0 6 -15 26.53 2.21 0 6 -15 22.31 1.72 0 6 -16 20.94 2.09 0 6 -16 19.31 1.56 0 6 -17 1.46 1.56 0 6 -18 2.54 1.42 0 6 -19 9.77 1.37 0 6 -20 4.76 1.09 0 6 -21 5.55 0.88 0 4 0 825.18 37.39 0 4 0 775.89 37.42 0 4 1 77.16 3.70 0 4 -1 75.89 3.79 0 4 1 72.05 3.74 0 4 -2 836.95 39.83 0 4 2 847.46 39.80 0 4 2 868.17 39.78 0 4 2 858.49 39.72 0 4 3 279.57 13.53 0 4 3 276.05 13.48 0 4 -3 281.77 13.57 0 4 3 300.37 13.61 0 4 3 295.52 13.48 0 4 3 291.64 13.55 0 4 -4 169.63 7.99 0 4 4 166.93 8.03 0 4 4 165.11 7.96 0 4 4 172.30 7.92 0 4 4 154.53 7.89 0 4 4 170.66 7.97 0 4 -5 12.19 0.97 0 4 5 11.91 0.90 0 4 5 11.75 0.97 0 4 5 11.72 0.97 0 4 5 10.77 0.95 0 4 5 12.97 1.10 0 4 -6 251.23 12.09 0 4 6 255.45 12.23 0 4 6 254.05 12.13 0 4 6 255.80 12.14 0 4 6 256.42 12.16 0 4 6 260.73 12.13 0 4 7 69.71 3.72 0 4 -7 67.31 3.53 0 4 7 70.97 3.62 0 4 7 67.72 3.61 0 4 7 73.56 3.68 0 4 7 75.00 3.62 0 4 -8 675.34 31.13 0 4 -8 634.04 31.17 0 4 8 690.84 31.37 0 4 8 687.50 31.26 0 4 8 692.78 31.33 0 4 8 659.23 31.31 0 4 8 649.52 31.39 0 4 9 82.26 4.61 0 4 9 92.27 4.63 0 4 9 87.79 4.58 0 4 -9 93.40 4.39 0 4 9 88.64 4.58 0 4 9 89.67 4.46 0 4 10 57.78 3.21 0 4 -12 304.13 14.38 0 4 -13 67.54 3.57 0 4 -14 109.53 5.24 0 4 -14 94.10 5.07 0 4 -15 56.09 3.02 0 4 -15 63.99 3.42 0 4 -15 54.92 3.19 0 4 -16 58.25 2.90 0 4 -16 50.41 3.04 0 4 -16 50.63 3.17 0 4 -17 13.77 1.69 0 4 -17 11.15 1.44 0 4 -17 12.00 1.14 0 4 -18 18.24 1.79 0 4 -18 16.63 1.60 0 4 -18 18.52 1.33 0 4 -19 32.12 2.20 0 4 -19 31.42 2.29 0 4 -19 34.70 1.94 0 4 -20 14.50 1.51 0 4 -20 13.00 1.45 0 4 -21 0.39 0.59 0 4 -21 -0.32 0.96 0 4 -21 0.02 0.89 0 4 -22 7.95 0.67 0 4 -22 7.20 0.97 0 2 0 6473.63 298.04 0 2 0 6456.38 298.02 0 2 0 6395.71 297.99 0 2 1 648.30 30.30 0 2 1 675.30 30.27 0 2 -1 650.61 30.32 0 2 1 624.95 30.29 0 2 -2 1584.68 70.45 0 2 2 1610.06 70.42 0 2 2 1571.60 70.42 0 2 2 1507.62 70.43 0 2 2 1574.57 70.44 0 2 3 472.34 21.48 0 2 3 443.47 21.48 0 2 3 466.12 21.47 0 2 4 821.46 38.21 0 2 -5 2585.96 114.52 0 2 5 2295.31 114.58 0 2 -6 33.06 1.66 0 2 6 32.82 1.70 0 2 7 975.55 44.00 0 2 -7 930.15 43.95 0 2 8 1329.64 60.57 0 2 8 1247.39 60.72 0 2 9 390.28 18.08 0 2 -9 379.22 17.93 0 2 10 1.89 0.68 0 2 -10 1.46 0.70 0 2 -11 71.28 3.64 0 2 -11 69.79 3.50 0 2 11 79.05 3.80 0 2 -12 1.62 0.88 0 2 -12 0.56 0.52 0 2 -12 0.64 0.93 0 2 -13 349.75 16.73 0 2 -13 366.09 16.86 0 2 -13 359.86 16.85 0 2 -14 96.01 4.72 0 2 -14 97.29 4.93 0 2 -14 96.40 4.90 0 2 -15 40.73 2.51 0 2 -15 41.40 2.52 0 2 -15 39.83 2.19 0 2 -15 40.34 2.34 0 2 -16 24.23 1.53 0 2 -16 25.47 1.75 0 2 -16 25.91 1.93 0 2 -17 1.15 0.69 0 2 -17 1.76 1.16 0 2 -17 2.28 1.08 0 2 -18 3.74 0.69 0 2 -18 5.07 1.10 0 2 -18 2.87 1.13 0 2 -19 25.12 1.82 0 2 -19 28.42 1.81 0 2 -19 23.70 2.05 0 2 -20 63.35 3.42 0 2 -20 67.71 3.25 0 2 -21 16.53 1.33 0 2 -21 17.46 1.64 0 2 -22 8.70 1.19 0 2 -22 6.80 0.92 0 2 -23 6.30 0.75 0 2 -23 5.74 1.01 0 2 -24 4.53 0.54 0 2 -24 5.36 0.79 0 0 2 2053.29 95.16 0 0 3 47.83 2.32 0 0 4 1900.78 88.14 0 0 5 0.35 0.49 0 0 6 56.50 2.81 0 0 7 9.58 0.78 0 0 8 791.32 36.87 0 0 9 4.47 0.64 0 0 10 41.66 2.07 0 0 -10 35.49 1.89 0 0 -10 40.19 1.98 0 0 -11 169.62 8.49 0 0 -11 186.58 8.54 0 0 -11 183.55 8.48 0 0 11 199.80 8.67 0 0 -11 164.82 8.50 0 0 -12 1919.24 88.28 0 0 -12 1915.16 88.57 0 0 -12 1886.44 88.23 0 0 12 1910.08 88.18 0 0 -12 1877.49 88.24 0 0 12 1904.94 88.40 0 0 -13 20.10 1.45 0 0 -13 21.72 1.51 0 0 13 22.54 1.30 0 0 -13 22.01 1.39 0 0 -14 63.36 3.34 0 0 -14 63.69 3.26 0 0 14 64.97 3.18 0 0 -14 61.12 3.30 0 0 -14 62.56 3.32 0 0 -15 12.14 1.29 0 0 -15 9.28 1.17 0 0 -15 12.07 1.12 0 0 -16 2.16 1.07 0 0 -16 1.49 0.90 0 0 -17 0.29 0.92 0 0 -17 1.01 1.11 0 0 -18 114.07 5.63 0 0 -18 109.25 5.52 0 0 -19 22.29 1.57 0 0 -19 23.45 1.81 0 0 -20 146.58 7.16 0 0 -20 136.09 7.13 0 0 -21 25.21 1.75 0 0 -21 29.47 1.77 0 0 -22 0.73 0.65 0 0 -22 0.71 0.93 0 0 -23 0.93 0.51 0 0 -23 0.02 0.74 0 0 -24 1.13 0.58 0 -2 0 6468.11 297.08 0 -2 0 6456.88 297.07 0 -2 0 6351.03 297.04 0 -2 1 729.27 31.90 0 -2 1 670.48 31.85 0 -2 -1 705.24 31.92 0 -2 -1 685.37 31.89 0 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2.81 2 6 -15 51.60 3.17 2 6 -16 8.00 1.79 2 6 -16 6.27 1.16 2 6 -17 7.98 1.20 2 6 -17 9.23 1.75 2 6 -18 3.90 1.60 2 6 -19 2.30 1.40 2 6 -20 3.80 1.30 2 6 -21 12.12 1.30 2 6 -22 0.48 0.75 -2 4 -21 2.11 0.55 -2 4 -21 3.40 0.84 -2 4 -20 5.36 0.76 -2 4 -20 4.16 1.02 -2 4 -20 5.95 0.95 -2 4 -19 4.35 1.09 -2 4 -19 2.79 1.11 -2 4 -19 4.42 0.82 -2 4 -18 35.93 2.01 -2 4 -18 32.33 2.26 -2 4 -18 33.72 2.20 -2 4 -17 2.67 0.92 -2 4 -17 2.59 1.36 -2 4 -17 2.81 1.17 -2 4 -16 5.56 1.24 -2 4 -16 6.86 0.99 -2 4 -16 5.94 1.49 -2 4 -15 143.77 6.81 -2 4 -15 133.35 6.89 -2 4 -15 141.30 7.02 -2 4 -14 54.36 3.14 -2 4 -14 61.19 3.37 -2 4 -13 100.30 5.16 2 4 8 53.53 2.99 2 4 8 51.48 3.00 2 4 8 54.88 3.03 2 4 8 59.74 2.91 2 4 8 54.05 3.13 2 4 7 236.28 10.99 2 4 7 230.54 11.06 2 4 7 232.43 11.08 2 4 7 229.49 11.18 2 4 7 236.27 11.05 -2 4 -7 221.67 10.90 2 4 6 475.33 21.99 2 4 6 466.51 22.09 2 4 6 452.83 21.96 2 4 6 482.37 21.96 -2 4 -6 460.06 21.87 2 4 5 310.85 15.09 2 4 5 326.77 14.96 -2 4 -5 311.20 14.91 2 4 5 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91.59 4.57 5 -5 1 92.85 4.54 -5 -5 0 25.09 1.57 -5 -5 0 25.36 1.54 5 -5 0 26.66 1.51 5 -5 0 23.02 1.46 -5 -5 0 30.40 1.59 5 -5 0 27.69 1.51 5 -5 0 32.11 1.59 -5 -5 1 113.55 5.62 5 -5 -1 122.84 5.65 5 -5 -1 113.65 5.56 5 -5 -1 114.92 5.58 5 -5 -1 111.15 5.56 -5 -5 1 123.51 5.77 -5 -5 1 115.10 5.59 -5 -5 1 124.27 5.66 5 -5 -1 115.63 5.78 5 -5 -2 189.46 9.13 5 -5 -2 196.94 9.22 -5 -5 2 206.56 9.21 -5 -5 2 198.63 9.32 5 -5 -2 180.14 9.13 -5 -5 2 198.56 9.17 5 -5 -2 184.55 9.15 -5 -5 2 200.52 9.29 5 -5 -2 210.55 9.38 -5 -5 3 22.37 1.52 -5 -5 3 25.43 1.60 -5 -5 3 27.20 1.47 -5 -5 3 27.47 1.63 -5 -5 3 23.53 1.49 5 -5 -3 27.04 1.45 -5 -5 4 147.83 7.66 -5 -5 4 155.98 7.71 -5 -5 4 173.88 7.84 -5 -5 4 158.86 7.70 5 -5 -4 159.84 7.67 5 -5 -4 165.49 7.70 5 -5 -4 162.99 7.69 -5 -5 4 174.35 7.87 -5 -5 4 174.66 7.70 5 -5 -5 91.61 4.39 -5 -5 5 87.79 4.43 -5 -5 5 94.94 4.39 5 -5 -5 87.73 4.40 -5 -5 5 97.40 4.61 -5 -5 5 93.05 4.57 -5 -5 5 89.83 4.41 -5 -5 5 90.10 4.43 5 -5 -5 91.70 4.43 -5 -5 5 89.41 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24.36 1.58 5 -7 -1 23.18 1.57 -5 -7 1 25.66 1.75 -5 -7 1 23.09 1.48 -5 -7 1 23.53 1.54 5 -7 -1 24.89 1.54 5 -7 -1 28.03 1.66 5 -7 -2 19.32 1.28 5 -7 -2 17.32 1.20 -5 -7 2 17.09 1.26 5 -7 -2 20.27 1.38 5 -7 -2 18.12 1.27 -5 -7 2 16.76 1.34 5 -7 -3 194.35 9.58 5 -7 -3 215.95 9.62 5 -7 -3 208.52 9.63 -5 -7 3 212.15 9.66 -5 -7 3 206.31 9.57 5 -7 -3 182.62 9.54 -5 -7 3 193.20 9.61 -5 -7 3 212.80 9.71 5 -7 -4 31.91 1.85 -5 -7 4 33.39 1.89 5 -7 -4 31.76 1.84 5 -7 -4 35.52 1.92 -5 -7 4 31.69 1.95 -5 -7 4 32.33 2.04 -5 -7 4 30.35 1.90 5 -7 -5 -0.08 0.69 5 -7 -5 1.17 0.83 -5 -7 5 0.90 0.90 5 -7 -5 1.39 0.75 -5 -7 5 1.56 0.93 -5 -7 5 0.34 1.06 -5 -7 6 19.84 1.42 5 -7 -6 19.22 1.30 5 -7 -6 18.71 1.31 -5 -7 6 17.38 1.54 5 -7 -6 15.73 1.22 5 -7 -6 16.53 1.18 -5 -7 7 56.04 3.14 -5 -7 7 60.79 3.16 5 -7 -7 60.43 3.02 -5 -7 7 54.44 3.06 -5 -7 8 7.33 1.08 -5 -7 8 5.83 1.17 5 -7 -8 6.27 0.92 -5 -7 8 7.78 1.21 5 -7 -9 4.87 0.86 -5 -7 9 1.64 1.09 -5 -7 9 3.16 1.03 -5 -7 10 9.08 1.19 5 -7 -10 9.79 0.97 5 -7 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6 55.29 2.81 10 -6 -6 51.00 2.74 -10 -6 6 56.09 2.89 -10 -6 6 59.08 2.98 -10 -6 7 248.06 11.07 -10 -6 7 241.90 11.09 10 -6 -7 228.63 10.97 10 -6 -7 226.07 10.98 10 -6 -7 228.65 10.99 -10 -6 7 235.94 11.02 10 -6 -7 224.24 11.02 10 -6 -8 17.02 1.17 -10 -6 8 15.27 1.46 10 -6 -8 17.35 1.23 10 -6 -8 17.96 1.25 -10 -6 8 15.90 1.41 10 -6 -8 15.58 1.07 -10 -6 9 26.64 1.83 10 -6 -9 26.64 1.60 10 -6 -9 27.03 1.57 10 -6 -9 24.29 1.49 10 -6 -9 29.00 1.67 10 -6 -10 141.70 6.90 10 -6 -10 146.73 6.97 10 -6 -10 140.29 6.89 10 -6 -10 149.04 6.95 10 -6 -11 35.64 2.00 10 -6 -11 38.73 2.06 10 -6 -11 34.41 1.96 10 -6 -11 34.45 1.99 10 -6 -11 36.02 2.08 -10 -6 11 38.81 2.24 10 -6 -11 36.45 1.98 10 -6 -12 4.37 0.84 10 -6 -12 4.63 0.93 10 -6 -12 4.42 0.84 10 -6 -12 4.46 0.72 10 -6 -12 4.13 0.80 -10 -6 12 6.03 1.12 10 -6 -12 5.33 0.90 10 -6 -13 146.74 7.20 10 -6 -13 139.74 7.20 10 -6 -13 147.10 7.21 10 -6 -13 151.08 7.21 -10 -6 13 159.27 7.32 10 -6 -13 154.56 7.18 10 -6 -14 33.12 1.87 10 -6 -14 31.23 1.84 10 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37.01 2.16 14 6 -8 70.58 3.67 14 6 -9 11.76 1.26 14 6 -10 86.37 4.41 14 6 -11 46.16 2.63 14 6 -11 46.36 2.55 14 6 -12 24.83 1.68 14 6 -12 17.56 1.54 14 6 -13 76.88 3.87 14 6 -13 68.77 3.77 14 6 -14 6.22 1.33 14 6 -15 5.82 1.37 14 6 -16 72.01 3.96 14 6 -17 93.62 4.95 14 6 -18 73.09 4.05 14 6 -19 57.39 3.25 14 6 -19 55.85 3.42 14 6 -20 7.79 1.39 14 6 -20 6.77 1.56 14 6 -21 2.08 1.13 14 6 -21 3.04 1.64 14 6 -22 15.91 1.40 14 6 -22 14.55 1.18 14 6 -22 15.85 1.78 14 6 -23 2.41 0.96 14 6 -23 0.64 1.43 14 6 -24 8.33 1.03 14 6 -25 0.68 0.65 14 6 -26 7.83 0.81 14 6 -27 4.43 0.56 14 6 -27 5.18 0.74 -14 4 -15 1.34 0.51 -14 4 -14 13.05 1.05 -14 4 -13 2.59 0.90 -14 4 -10 11.68 1.30 14 4 5 27.77 1.64 14 4 4 136.16 6.56 14 4 3 56.19 2.89 14 4 2 -0.48 0.69 14 4 1 83.12 4.10 -14 4 0 17.82 1.48 14 4 0 16.11 1.04 -14 4 1 172.11 8.05 14 4 -1 153.94 7.84 -14 4 2 49.09 2.89 14 4 -2 49.66 2.70 14 4 -3 134.36 6.77 -14 4 3 145.27 6.98 -14 4 4 74.16 3.78 14 4 -4 66.32 3.54 14 4 -4 68.92 3.72 -14 4 5 149.44 6.91 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179.13 8.76 20 2 -3 190.25 8.81 20 2 -4 23.25 1.46 20 2 -4 24.01 1.56 20 2 -5 136.87 6.58 -20 2 6 190.54 9.20 20 2 -8 212.99 10.46 20 2 -8 214.35 10.09 20 2 -9 290.21 13.67 20 2 -9 293.19 13.69 20 2 -10 98.82 4.94 -20 2 10 88.66 4.88 20 2 -11 33.12 2.22 -20 2 11 31.87 2.17 20 2 -12 17.59 1.07 20 2 -12 16.57 1.49 -20 2 12 17.54 1.55 20 2 -13 95.00 5.03 20 2 -13 94.09 4.77 20 2 -13 99.64 4.74 20 2 -14 133.72 6.41 20 2 -14 130.47 6.38 20 2 -15 150.75 7.41 20 2 -15 156.94 7.43 20 2 -16 170.02 8.19 20 2 -16 170.70 8.22 20 2 -17 106.08 5.33 20 2 -17 100.37 5.25 20 2 -17 112.53 5.36 20 2 -17 116.78 5.40 20 2 -18 13.34 1.19 20 2 -18 9.70 1.06 20 2 -18 15.03 1.34 20 2 -18 9.92 1.50 20 2 -18 10.94 1.42 20 2 -19 57.32 3.15 20 2 -19 59.87 3.20 20 2 -19 56.47 3.08 20 2 -19 66.05 3.37 20 2 -19 61.65 3.31 20 2 -20 255.64 12.56 20 2 -20 270.18 12.64 20 2 -20 278.13 12.59 20 2 -20 245.41 12.49 20 2 -20 290.35 12.72 20 2 -21 160.32 7.95 20 2 -21 175.02 7.99 20 2 -21 150.14 7.88 20 2 -21 172.12 8.10 20 2 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82.66 4.14 20 -4 -10 43.46 2.35 20 -4 -10 47.98 2.47 20 -4 -10 43.85 2.43 -20 -4 10 48.83 2.49 20 -4 -10 45.69 2.49 20 -4 -11 58.90 3.00 20 -4 -11 57.21 3.06 20 -4 -12 21.63 1.48 20 -4 -12 22.39 1.60 20 -4 -12 24.23 1.46 -20 -4 12 22.95 1.64 20 -4 -13 19.85 1.39 20 -4 -13 18.18 1.47 20 -4 -13 19.37 1.38 20 -4 -13 15.27 1.27 -20 -4 13 15.11 1.41 20 -4 -14 18.46 1.30 20 -4 -14 15.45 1.37 20 -4 -14 18.54 1.27 -20 -4 14 15.02 1.48 20 -4 -14 13.46 1.33 20 -4 -15 232.06 10.73 20 -4 -15 222.73 10.74 20 -4 -15 216.75 10.70 20 -4 -15 221.15 10.72 -20 -4 15 234.41 10.78 20 -4 -16 68.82 3.48 20 -4 -16 66.56 3.53 20 -4 -16 64.99 3.51 -20 -4 16 67.27 3.56 20 -4 -17 0.51 0.87 20 -4 -17 0.22 1.11 20 -4 -17 1.56 1.14 -20 -4 17 0.58 1.03 20 -4 -18 1.59 0.92 20 -4 -18 0.87 1.05 20 -4 -18 2.27 1.22 -20 -4 18 1.12 1.02 20 -4 -18 1.48 1.00 20 -4 -19 139.62 7.09 20 -4 -19 143.00 7.02 20 -4 -19 154.02 7.12 20 -4 -19 136.06 6.96 -20 -4 19 139.54 7.05 20 -4 -19 158.64 7.10 20 -4 -20 23.62 1.56 20 -4 -20 22.85 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17.82 1.38 -20 -6 -4 19.95 1.85 20 -6 4 20.84 1.51 -20 -6 -4 20.83 1.60 20 -6 3 4.77 1.05 -20 -6 -3 4.86 0.93 -20 -6 -3 5.01 1.51 20 -6 3 3.87 1.07 -20 -6 -3 3.74 1.10 20 -6 2 5.09 1.06 -20 -6 -2 4.59 0.91 -20 -6 -2 3.82 1.52 -20 -6 -2 4.55 1.19 -20 -6 -1 9.57 1.36 20 -6 1 10.79 1.17 20 -6 1 9.46 1.10 -20 -6 -1 8.59 1.07 -20 -6 -1 8.94 1.67 -20 -6 0 -0.06 1.13 20 -6 0 -0.13 0.96 20 -6 0 0.83 0.98 20 -6 0 1.15 0.79 -20 -6 0 0.93 0.78 -20 -6 0 1.56 1.54 20 -6 0 1.93 1.20 20 -6 -1 22.70 1.58 20 -6 -1 23.93 1.63 20 -6 -1 22.99 1.56 -20 -6 1 21.00 1.46 -20 -6 1 20.22 2.01 20 -6 -1 23.71 1.74 -20 -6 1 24.56 1.81 20 -6 -2 53.15 2.72 20 -6 -2 51.01 2.77 20 -6 -2 49.43 2.71 -20 -6 2 44.91 2.64 -20 -6 2 47.27 3.07 20 -6 -2 48.24 2.64 20 -6 -2 52.66 2.89 -20 -6 2 52.43 2.88 20 -6 -3 43.16 2.32 20 -6 -3 42.11 2.39 20 -6 -3 42.12 2.34 -20 -6 3 39.57 2.60 -20 -6 3 38.03 2.25 -20 -6 3 39.43 2.69 20 -6 -3 39.25 2.30 20 -6 -3 46.19 2.50 -20 -6 3 39.14 2.47 20 -6 -4 87.04 4.40 20 -6 -4 89.90 4.49 20 -6 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-1 -15 2.41 0.62 39 -1 -16 7.89 0.86 39 -1 -16 5.33 0.69 39 -1 -17 0.81 0.69 39 -1 -17 0.73 0.54 39 -1 -18 10.02 0.93 39 -1 -19 3.04 0.71 39 -1 -19 3.11 0.66 39 -1 -20 1.55 0.65 39 -1 -20 2.84 0.67 39 -1 -21 -0.53 0.58 39 -1 -21 0.50 0.69 39 -1 -22 3.13 0.58 39 -1 -22 3.58 0.74 39 -1 -23 3.41 0.78 39 -1 -24 3.16 0.76 39 -1 -25 0.05 0.70 39 -1 -26 1.12 0.69 39 -1 -27 1.39 0.69 39 -1 -28 3.40 0.69 39 -1 -28 1.55 0.46 39 -1 -29 0.24 0.55 39 -1 -29 -0.49 0.41 39 -1 -30 9.36 0.65 39 -1 -31 5.02 0.54 39 -3 -9 0.95 0.42 -39 -3 10 6.29 0.63 39 -3 -10 7.31 0.64 -39 -3 11 0.23 0.51 -39 -3 12 -0.29 0.58 39 -3 -13 3.32 0.59 39 -3 -13 1.80 0.53 39 -3 -14 0.29 0.56 39 -3 -15 1.52 0.58 39 -3 -16 0.91 0.56 39 -3 -17 16.73 1.00 39 -3 -17 12.83 1.01 39 -3 -18 6.57 0.64 39 -3 -18 6.42 0.76 39 -3 -19 1.01 0.66 39 -3 -20 3.21 0.74 39 -3 -21 3.74 0.76 39 -3 -22 0.52 0.71 39 -3 -23 2.75 0.76 39 -3 -24 2.71 0.77 39 -3 -25 2.43 0.72 39 -3 -25 1.39 0.50 39 -3 -26 1.02 0.68 39 -3 -26 1.44 0.56 39 -3 -26 1.08 0.49 39 -3 -27 0.41 0.44 39 -3 -27 0.29 0.46 39 -3 -28 0.54 0.44 39 -3 -29 1.14 0.48 39 -3 -29 0.53 0.37 39 -3 -30 4.34 0.48 39 -5 -14 0.47 0.40 39 -5 -15 0.26 0.46 39 -5 -16 2.17 0.47 39 -5 -16 3.13 0.59 39 -5 -17 1.08 0.51 39 -5 -17 1.74 0.59 39 -5 -18 2.09 0.57 39 -5 -18 2.04 0.63 39 -5 -19 3.38 0.63 39 -5 -19 3.85 0.70 39 -5 -20 -0.16 0.57 39 -5 -21 1.17 0.62 39 -5 -21 1.56 0.64 39 -5 -22 1.34 0.60 39 -5 -22 1.43 0.60 39 -5 -23 0.83 0.56 39 -5 -23 0.47 0.55 39 -5 -24 0.77 0.56 39 -5 -24 1.49 0.52 39 -5 -25 -0.12 0.44 39 -5 -26 0.72 0.47 39 -5 -27 0.92 0.39 40 6 -18 1.97 0.37 40 6 -19 1.45 0.37 40 6 -19 1.29 0.36 40 6 -20 0.77 0.37 40 6 -20 1.51 0.36 40 6 -21 2.13 0.38 40 6 -21 1.22 0.37 40 4 -13 1.14 0.40 40 4 -14 0.87 0.46 40 4 -14 0.39 0.50 40 4 -15 0.37 0.51 40 4 -15 0.29 0.52 40 4 -16 9.38 0.80 40 4 -16 9.49 0.81 40 4 -17 5.87 0.73 40 4 -17 7.06 0.71 40 4 -18 6.20 0.73 40 4 -19 15.56 1.05 40 4 -20 0.60 0.57 40 4 -20 0.47 0.62 40 4 -21 5.38 0.68 40 4 -21 4.89 0.70 40 4 -22 7.12 0.72 40 4 -22 8.49 0.77 40 4 -23 2.09 0.51 40 4 -23 2.98 0.61 40 4 -24 10.53 0.77 40 4 -24 7.71 0.64 40 4 -25 7.60 0.66 40 4 -26 2.34 0.43 40 2 -10 0.91 0.38 40 2 -10 1.09 0.43 -40 2 10 0.72 0.43 40 2 -11 8.10 0.66 40 2 -11 6.68 0.68 40 2 -12 5.44 0.65 40 2 -12 4.87 0.65 40 2 -13 7.88 0.78 40 2 -13 7.34 0.77 40 2 -14 3.13 0.68 40 2 -14 2.57 0.66 40 2 -15 0.46 0.64 40 2 -16 1.85 0.67 40 2 -17 1.11 0.66 40 2 -17 0.99 0.73 40 2 -18 5.79 0.76 40 2 -18 6.11 0.80 40 2 -19 2.54 0.68 40 2 -19 1.91 0.73 40 2 -20 15.40 1.09 40 2 -20 12.91 0.99 40 2 -21 -0.05 0.55 40 2 -21 -0.49 0.68 40 2 -22 5.38 0.64 40 2 -22 7.15 0.80 40 2 -23 12.11 0.95 40 2 -24 9.22 0.75 40 2 -24 5.64 0.65 40 2 -25 3.80 0.56 40 2 -25 2.36 0.52 40 2 -26 3.60 0.49 40 2 -26 3.12 0.56 40 2 -27 2.05 0.52 40 2 -28 4.06 0.54 40 2 -29 4.92 0.52 40 2 -30 4.90 0.47 40 0 -9 0.48 0.38 40 0 -10 15.41 0.91 40 0 -10 12.82 0.89 40 0 -11 24.47 1.38 40 0 -12 2.10 0.58 40 0 -13 1.39 0.63 40 0 -13 0.92 0.57 40 0 -14 0.93 0.67 40 0 -14 1.30 0.59 40 0 -15 1.68 0.68 40 0 -15 -0.14 0.59 40 0 -16 28.12 1.53 40 0 -16 22.90 1.44 40 0 -17 11.56 0.95 40 0 -17 8.64 0.81 40 0 -18 0.24 0.69 40 0 -18 0.68 0.53 40 0 -19 3.51 0.71 40 0 -19 3.02 0.57 40 0 -20 -0.46 0.66 40 0 -21 0.15 0.63 40 0 -21 -0.23 0.53 40 0 -22 9.50 0.80 40 0 -22 9.07 0.82 40 0 -23 8.63 0.75 40 0 -23 7.56 0.80 40 0 -24 4.71 0.57 40 0 -24 4.75 0.73 40 0 -25 0.83 0.62 40 0 -26 6.18 0.76 40 0 -27 -0.45 0.58 40 0 -28 14.15 0.98 40 0 -29 0.49 0.51 40 0 -30 4.98 0.56 40 0 -31 1.97 0.39 -40 -2 10 1.37 0.47 40 -2 -10 2.48 0.46 40 -2 -11 5.16 0.48 -40 -2 11 5.64 0.66 40 -2 -12 4.68 0.61 40 -2 -12 3.60 0.46 40 -2 -13 8.94 0.72 40 -2 -13 4.72 0.55 40 -2 -14 1.95 0.60 40 -2 -15 1.55 0.59 40 -2 -16 1.55 0.59 40 -2 -17 2.23 0.61 40 -2 -18 5.59 0.66 40 -2 -19 2.00 0.55 40 -2 -19 2.64 0.59 40 -2 -20 12.87 0.87 40 -2 -20 12.65 0.94 40 -2 -21 0.45 0.61 40 -2 -22 6.24 0.79 40 -2 -23 13.32 1.03 40 -2 -24 10.23 0.91 40 -2 -25 2.52 0.66 40 -2 -26 3.06 0.68 40 -2 -27 2.57 0.61 40 -2 -27 1.98 0.49 40 -2 -28 5.79 0.71 40 -4 -12 2.74 0.39 40 -4 -13 0.66 0.38 40 -4 -14 0.94 0.38 40 -4 -14 1.06 0.41 40 -4 -15 1.14 0.46 40 -4 -15 -0.07 0.39 40 -4 -16 7.62 0.69 40 -4 -16 5.45 0.53 40 -4 -17 7.29 0.76 40 -4 -18 5.12 0.62 40 -4 -18 7.27 0.76 40 -4 -19 13.87 0.98 40 -4 -19 17.29 1.11 40 -4 -20 1.10 0.57 40 -4 -21 5.28 0.69 40 -4 -22 8.05 0.81 40 -4 -22 10.59 0.87 40 -4 -23 5.02 0.68 40 -4 -23 3.25 0.66 40 -4 -24 7.67 0.76 40 -4 -24 8.46 0.79 40 -4 -25 5.71 0.67 40 -4 -25 7.33 0.67 40 -4 -26 3.01 0.55 40 -4 -26 1.84 0.46 40 -4 -28 0.39 0.38 40 -6 -19 1.76 0.41 40 -6 -20 1.28 0.41 40 -6 -22 0.37 0.36 41 5 -16 1.60 0.37 41 5 -17 1.57 0.36 41 5 -17 1.41 0.39 41 5 -18 0.06 0.37 41 5 -18 0.31 0.37 41 5 -19 3.34 0.46 41 5 -19 3.04 0.45 41 5 -20 0.16 0.39 41 5 -21 3.16 0.44 41 5 -22 1.83 0.38 41 5 -22 2.20 0.42 41 5 -23 0.89 0.38 41 5 -24 1.50 0.35 41 3 -12 0.03 0.34 41 3 -13 1.35 0.39 41 3 -13 0.96 0.44 41 3 -14 2.59 0.49 41 3 -14 2.58 0.50 41 3 -15 0.58 0.49 41 3 -15 1.17 0.51 41 3 -16 -0.16 0.55 41 3 -16 1.35 0.52 41 3 -17 0.62 0.51 41 3 -18 -0.47 0.55 41 3 -19 5.78 0.71 41 3 -19 7.52 0.75 41 3 -20 1.93 0.56 41 3 -20 1.72 0.61 41 3 -21 1.66 0.54 41 3 -21 2.47 0.63 41 3 -22 -0.25 0.47 41 3 -22 -0.06 0.57 41 3 -23 -0.12 0.39 41 3 -23 -0.62 0.54 41 3 -24 1.47 0.51 41 3 -25 1.12 0.45 41 3 -26 3.60 0.45 41 1 -11 0.48 0.38 41 1 -11 0.05 0.38 41 1 -12 6.89 0.63 41 1 -12 5.71 0.60 41 1 -13 2.01 0.53 41 1 -14 1.39 0.54 41 1 -15 0.49 0.59 41 1 -15 0.83 0.54 41 1 -16 0.56 0.62 41 1 -16 1.36 0.56 41 1 -17 1.00 0.64 41 1 -17 0.95 0.56 41 1 -18 3.84 0.68 41 1 -18 1.89 0.57 41 1 -19 11.47 0.87 41 1 -19 6.81 0.71 41 1 -20 5.92 0.63 41 1 -20 7.25 0.77 41 1 -21 1.12 0.63 41 1 -22 4.46 0.65 41 1 -23 0.17 0.52 41 1 -24 1.25 0.50 41 1 -24 1.08 0.46 41 1 -25 0.38 0.42 41 1 -25 1.07 0.49 41 1 -26 1.38 0.49 41 1 -27 3.19 0.52 41 1 -28 1.43 0.46 41 1 -29 2.07 0.44 41 1 -30 2.91 0.40 -41 -1 11 -0.69 0.47 41 -1 -12 6.32 0.59 41 -1 -12 4.50 0.48 41 -1 -13 3.01 0.54 41 -1 -13 1.47 0.43 41 -1 -14 2.22 0.54 41 -1 -14 1.89 0.44 41 -1 -15 0.90 0.57 41 -1 -15 0.31 0.43 41 -1 -16 0.73 0.58 41 -1 -17 2.06 0.60 41 -1 -18 1.79 0.59 41 -1 -19 10.61 0.84 41 -1 -20 6.97 0.69 41 -1 -21 -0.55 0.51 41 -1 -21 0.35 0.49 41 -1 -22 3.77 0.52 41 -1 -22 3.33 0.61 41 -1 -23 -0.23 0.55 41 -1 -24 1.68 0.58 41 -1 -25 1.00 0.58 41 -1 -26 1.78 0.60 41 -1 -27 2.60 0.57 41 -1 -28 3.17 0.56 41 -1 -29 1.79 0.48 41 -1 -30 3.27 0.43 41 -3 -13 0.56 0.36 41 -3 -14 2.03 0.44 -41 -3 15 0.72 0.42 41 -3 -15 0.97 0.42 41 -3 -15 0.26 0.41 41 -3 -16 -0.49 0.48 41 -3 -19 5.20 0.55 41 -3 -20 1.93 0.54 41 -3 -21 1.25 0.55 41 -3 -22 0.66 0.55 41 -3 -23 -0.41 0.55 41 -3 -24 0.53 0.54 41 -3 -25 0.21 0.54 41 -3 -25 1.06 0.54 41 -3 -26 3.53 0.59 41 -3 -26 4.01 0.54 41 -3 -27 2.62 0.49 41 -3 -28 0.59 0.40 41 -5 -18 0.28 0.37 41 -5 -19 3.08 0.48 41 -5 -20 0.41 0.42 41 -5 -21 2.28 0.41 41 -5 -22 2.73 0.45 41 -5 -22 2.21 0.47 41 -5 -23 0.92 0.40 41 -5 -23 0.46 0.41 41 -5 -24 1.21 0.39 41 -5 -24 1.48 0.39 42 4 -17 1.47 0.38 42 4 -17 1.78 0.38 42 4 -18 2.57 0.43 42 4 -18 2.03 0.41 42 4 -19 6.73 0.56 42 4 -20 1.52 0.40 42 4 -21 0.51 0.36 42 4 -21 0.81 0.42 42 4 -22 2.33 0.43 42 4 -23 3.43 0.46 42 4 -24 7.44 0.56 42 2 -13 0.80 0.33 42 2 -13 0.72 0.34 42 2 -14 0.40 0.38 42 2 -14 0.60 0.40 42 2 -15 2.51 0.48 42 2 -15 0.95 0.44 42 2 -16 0.19 0.45 42 2 -17 1.66 0.52 42 2 -17 1.47 0.47 42 2 -18 6.63 0.67 42 2 -18 4.06 0.57 42 2 -19 0.97 0.56 42 2 -19 1.15 0.45 42 2 -20 2.48 0.49 42 2 -20 2.51 0.58 42 2 -21 0.34 0.39 42 2 -21 0.80 0.55 42 2 -22 1.16 0.51 42 2 -23 3.33 0.54 42 2 -24 14.84 0.91 42 2 -25 1.93 0.40 42 0 -14 2.57 0.49 42 0 -14 2.45 0.43 42 0 -15 0.96 0.50 42 0 -15 0.59 0.39 42 0 -16 -0.13 0.53 42 0 -16 -0.61 0.39 42 0 -17 2.33 0.56 42 0 -17 1.05 0.40 42 0 -18 4.94 0.65 42 0 -19 10.76 0.85 42 0 -20 0.60 0.52 42 0 -21 10.94 0.80 42 0 -22 0.50 0.46 42 0 -23 0.98 0.41 42 0 -24 3.29 0.50 42 0 -25 1.39 0.47 42 0 -26 0.99 0.46 42 0 -27 0.20 0.41 42 0 -28 0.99 0.41 42 0 -29 4.25 0.45 42 -2 -13 -0.07 0.33 -42 -2 14 0.91 0.41 42 -2 -15 1.35 0.40 42 -2 -16 0.98 0.42 42 -2 -17 1.70 0.44 42 -2 -18 3.98 0.50 42 -2 -19 0.51 0.38 42 -2 -22 0.92 0.43 42 -2 -23 3.40 0.54 42 -2 -24 13.00 0.87 42 -2 -25 0.94 0.47 42 -2 -26 8.45 0.70 42 -2 -27 2.67 0.48 42 -2 -28 1.58 0.41 42 -4 -18 1.06 0.39 42 -4 -19 5.67 0.57 42 -4 -20 1.21 0.45 42 -4 -23 2.16 0.41 42 -4 -23 2.02 0.47 42 -4 -24 7.89 0.59 42 -4 -24 8.03 0.64 42 -4 -25 6.67 0.54 43 3 -17 0.14 0.32 43 3 -19 2.25 0.44 43 3 -20 1.21 0.41 43 3 -21 1.13 0.42 43 3 -22 0.78 0.39 43 3 -23 1.28 0.37 43 1 -16 0.58 0.42 43 1 -17 0.25 0.44 43 1 -18 0.50 0.46 43 1 -19 0.51 0.48 43 1 -20 2.39 0.51 43 1 -21 4.80 0.56 43 1 -22 1.07 0.42 43 1 -23 2.64 0.43 43 1 -24 2.47 0.37 43 -1 -15 0.06 0.33 43 -1 -16 1.26 0.38 43 -1 -17 0.14 0.38 43 -1 -18 0.61 0.40 43 -1 -19 0.22 0.40 43 -1 -20 1.55 0.39 43 -1 -21 4.07 0.42 43 -1 -25 -0.07 0.34 43 -1 -26 1.22 0.37 43 -3 -19 2.46 0.44 43 -3 -20 1.22 0.44 43 -3 -21 0.68 0.45 43 -3 -23 1.09 0.45 43 -3 -24 -0.18 0.38 43 -3 -25 0.94 0.37 44 2 -19 2.01 0.35 44 2 -20 0.40 0.34 44 2 -21 2.81 0.40 44 2 -22 1.44 0.34 44 0 -18 0.32 0.33 44 0 -19 1.15 0.36 44 0 -20 0.67 0.33 44 -2 -24 2.56 0.43 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 40210 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4693(3) 0.3043(5) 0.6903(3) 0.0884(17) Uani 1 1 d . . . . . H1A H 0.4583 0.2446 0.7045 0.133 Uiso 1 1 calc GR . . . . H1B H 0.4886 0.2639 0.6824 0.133 Uiso 1 1 calc GR . . . . H1C H 0.4410 0.3430 0.6499 0.133 Uiso 1 1 calc GR . . . . C2 C 0.5002(2) 0.4000(5) 0.7432(3) 0.0750(13) Uani 1 1 d . . . . . H2 H 0.5272 0.3595 0.7855 0.090 Uiso 1 1 calc R . . . . C3 C 0.4717(2) 0.4809(6) 0.7528(3) 0.0832(15) Uani 1 1 d . . . . . H3A H 0.4588 0.4305 0.7681 0.100 Uiso 1 1 calc R . . . . H3B H 0.4943 0.5408 0.7874 0.100 Uiso 1 1 calc R . . . . C4 C 0.4299(2) 0.5477(6) 0.6915(4) 0.0908(18) Uani 1 1 d . . . . . H4 H 0.4384 0.6104 0.6770 0.109 Uiso 1 1 calc R . . . . C5 C 0.3818(3) 0.5280(9) 0.6551(4) 0.119(3) Uani 1 1 d . U . . . H5 H 0.3726 0.4626 0.6673 0.143 Uiso 1 1 calc R . . . . C6 C 0.3417(3) 0.6022(11) 0.5965(4) 0.137(3) Uani 1 1 d . U . . . H6A H 0.3555 0.6778 0.5953 0.164 Uiso 1 1 calc R . . . . H6B H 0.3177 0.6245 0.6004 0.164 Uiso 1 1 calc R . . . . C7 C 0.3154(3) 0.5305(10) 0.5312(4) 0.130(3) Uani 1 1 d . U . . . H7A H 0.3142 0.4434 0.5387 0.156 Uiso 1 1 calc R . . . . H7B H 0.2816 0.5599 0.4977 0.156 Uiso 1 1 calc R . . . . C8 C 0.3422(2) 0.5467(9) 0.5064(4) 0.109(2) Uani 1 1 d . U . . . H8 H 0.3425 0.6261 0.4935 0.131 Uiso 1 1 calc R . . . . C9 C 0.36426(18) 0.4654(7) 0.5012(3) 0.0809(15) Uani 1 1 d . U . . . H9 H 0.3655 0.3869 0.5164 0.097 Uiso 1 1 calc R . . . . C10 C 0.38860(15) 0.4797(5) 0.4737(2) 0.0595(10) Uani 1 1 d . . . . . H10 H 0.3844 0.5648 0.4583 0.071 Uiso 1 1 calc R . . . . C11 C 0.44319(14) 0.4480(5) 0.52308(19) 0.0591(10) Uani 1 1 d . . . . . H11C H 0.4474 0.3700 0.5441 0.071 Uiso 1 1 calc R . . . . H11D H 0.4542 0.4362 0.4988 0.071 Uiso 1 1 calc R . . . . C12 C 0.47634(14) 0.5426(4) 0.57696(18) 0.0508(9) Uani 1 1 d . . . . . C13 C 0.53051(14) 0.5058(4) 0.62832(18) 0.0541(9) Uani 1 1 d . . . . . H13C H 0.5335 0.4345 0.6526 0.065 Uiso 1 1 calc R . . . . H13D H 0.5415 0.4811 0.6053 0.065 Uiso 1 1 calc R . . . . C14 C 0.56453(14) 0.6059(4) 0.67767(19) 0.0537(9) Uani 1 1 d . . . . . C15 C 0.58061(15) 0.6957(4) 0.65929(19) 0.0557(10) Uani 1 1 d . . . . . C16 C 0.61396(15) 0.7887(4) 0.7026(2) 0.0575(10) Uani 1 1 d . . . . . C17 C 0.63273(16) 0.7904(5) 0.7671(2) 0.0639(11) Uani 1 1 d . . . . . H17 H 0.6552 0.8513 0.7966 0.077 Uiso 1 1 calc R . . . . C18 C 0.61792(16) 0.7009(5) 0.7876(2) 0.0640(11) Uani 1 1 d . . . . . C19 C 0.58264(15) 0.6107(5) 0.74348(19) 0.0578(10) Uani 1 1 d . . . . . C20 C 0.56501(18) 0.5301(5) 0.7683(2) 0.0652(11) Uani 1 1 d . . . . . Cl1 Cl 0.55872(4) 0.69943(13) 0.57878(5) 0.0709(3) Uani 1 1 d . . . . . O1 O 0.58724(17) 0.5189(5) 0.82747(16) 0.1007(14) Uani 1 1 d . . . . . O2 O 0.52108(12) 0.4765(3) 0.72160(14) 0.0662(8) Uani 1 1 d . . . . . O3 O 0.36594(11) 0.3965(4) 0.41826(15) 0.0789(11) Uani 1 1 d . . . . . H3 H 0.3357 0.3986 0.3945 0.118 Uiso 1 1 calc GR . . . . O4 O 0.46130(12) 0.6412(3) 0.57790(17) 0.0714(9) Uani 1 1 d . . . . . O5 O 0.62921(12) 0.8790(3) 0.68542(17) 0.0711(9) Uani 1 1 d . . . . . H5A H 0.6239 0.8585 0.6518 0.107 Uiso 1 1 calc GR . . . . O6 O 0.63953(14) 0.7061(5) 0.85228(15) 0.0846(11) Uani 1 1 d . . . . . H6 H 0.6243 0.6616 0.8581 0.127 Uiso 1 1 calc GR . . . . C1A C 0.2919(3) 0.6610(7) 0.3012(4) 0.109(2) Uani 1 1 d . . . . . H1AA H 0.3254 0.6778 0.3210 0.163 Uiso 1 1 calc GR . . . . H1AB H 0.2915 0.6369 0.3353 0.163 Uiso 1 1 calc GR . . . . H1AC H 0.2720 0.7339 0.2792 0.163 Uiso 1 1 calc GR . . . . C2A C 0.27106(18) 0.5587(6) 0.2515(3) 0.0726(13) Uani 1 1 d . . . . . H2A H 0.2933 0.4872 0.2725 0.087 Uiso 1 1 calc R . . . . C3A C 0.2615(2) 0.5941(6) 0.1902(3) 0.0813(15) Uani 1 1 d . . . . . H3AA H 0.2914 0.6306 0.2034 0.098 Uiso 1 1 calc R . . . . H3AB H 0.2358 0.6570 0.1668 0.098 Uiso 1 1 calc R . . . . C4A C 0.24577(18) 0.4901(6) 0.1432(3) 0.0755(14) Uani 1 1 d . . . . . H4A H 0.2242 0.4320 0.1374 0.091 Uiso 1 1 calc R . . . . C5A C 0.25971(18) 0.4737(6) 0.1097(3) 0.0800(15) Uani 1 1 d . . . . . H5AA H 0.2845 0.5258 0.1200 0.096 Uiso 1 1 calc R . . . . C6A C 0.2401(2) 0.3806(7) 0.0567(3) 0.0907(19) Uani 1 1 d . . . . . H6AA H 0.2272 0.3108 0.0636 0.109 Uiso 1 1 calc R . . . . H6AB H 0.2671 0.3509 0.0601 0.109 Uiso 1 1 calc R . . . . C7A C 0.19932(18) 0.4323(9) -0.0130(3) 0.096(2) Uani 1 1 d . . . . . H7AA H 0.2101 0.5106 -0.0172 0.116 Uiso 1 1 calc R . . . . H7AB H 0.1935 0.3758 -0.0456 0.116 Uiso 1 1 calc R . . . . C8A C 0.15201(16) 0.4509(6) -0.0274(2) 0.0715(13) Uani 1 1 d . . . . . H8A H 0.1317 0.3818 -0.0425 0.086 Uiso 1 1 calc R . . . . C9A C 0.13572(16) 0.5508(5) -0.0215(2) 0.0640(11) Uani 1 1 d . . . . . H9A H 0.1559 0.6202 -0.0054 0.077 Uiso 1 1 calc R . . . . C10A C 0.08761(15) 0.5649(4) -0.03800(18) 0.0546(9) Uani 1 1 d . . . . . H10A H 0.0702 0.4855 -0.0537 0.066 Uiso 1 1 calc R . . . . C11A C 0.09306(17) 0.6095(4) 0.02072(19) 0.0575(10) Uani 1 1 d . . . . . H11E H 0.1165 0.6774 0.0424 0.069 Uiso 1 1 calc R . . . . H11F H 0.0613 0.6412 0.0035 0.069 Uiso 1 1 calc R . . . . C12A C 0.11028(14) 0.5116(4) 0.07244(18) 0.0494(8) Uani 1 1 d . . . . . C13A C 0.12000(15) 0.5571(4) 0.13352(18) 0.0522(9) Uani 1 1 d . . . . . H13E H 0.0928 0.6103 0.1192 0.063 Uiso 1 1 calc R . . . . H13F H 0.1500 0.6066 0.1602 0.063 Uiso 1 1 calc R . . . . C14A C 0.12568(13) 0.4549(4) 0.17693(17) 0.0498(8) Uani 1 1 d . . . . . C15A C 0.08251(14) 0.3954(4) 0.15355(18) 0.0548(10) Uani 1 1 d . . . . . C16A C 0.08233(16) 0.3038(5) 0.1896(2) 0.0601(11) Uani 1 1 d . . . . . C17A C 0.12613(17) 0.2738(5) 0.2523(2) 0.0625(11) Uani 1 1 d . . . . . H17A H 0.1263 0.2144 0.2775 0.075 Uiso 1 1 calc R . . . . C18A C 0.16929(15) 0.3313(5) 0.2774(2) 0.0628(11) Uani 1 1 d . . . . . C19A C 0.17081(13) 0.4194(4) 0.23960(17) 0.0515(9) Uani 1 1 d . . . . . C20A C 0.22033(14) 0.4617(5) 0.26766(19) 0.0565(10) Uani 1 1 d . . . . . Cl1A Cl 0.02583(4) 0.43632(18) 0.07678(5) 0.0834(4) Uani 1 1 d . . . . . O1A O 0.25838(11) 0.4322(5) 0.32402(15) 0.0852(11) Uani 1 1 d . . . . . O2A O 0.22161(11) 0.5238(3) 0.22710(15) 0.0637(8) Uani 1 1 d . . . . . O3A O 0.05713(12) 0.6563(4) -0.08991(15) 0.0713(9) Uani 1 1 d . . . . . H3AC H 0.0628 0.6552 -0.1148 0.107 Uiso 1 1 calc GR . . . . O4A O 0.11469(13) 0.4049(3) 0.06483(15) 0.0632(7) Uani 1 1 d . . . . . O5A O 0.04136(13) 0.2419(4) 0.16676(18) 0.0836(11) Uani 1 1 d . . . . . H5AB H 0.0181 0.2624 0.1281 0.125 Uiso 1 1 calc GR . . . . O6A O 0.21020(13) 0.2971(5) 0.33999(17) 0.0953(14) Uani 1 1 d . . . . . H6AC H 0.2347 0.3315 0.3502 0.143 Uiso 1 1 calc GR . . . . C1B C 0.4766(2) -0.1809(7) 0.2147(3) 0.0926(18) Uani 1 1 d . . . . . H1BA H 0.4908 -0.2226 0.1991 0.139 Uiso 1 1 calc GR . . . . H1BB H 0.4437 -0.1536 0.1772 0.139 Uiso 1 1 calc GR . . . . H1BC H 0.4753 -0.2366 0.2413 0.139 Uiso 1 1 calc GR . . . . C2B C 0.50823(16) -0.0712(5) 0.2562(2) 0.0637(11) Uani 1 1 d . . . . . H2B H 0.5099 -0.0137 0.2295 0.076 Uiso 1 1 calc R . . . . C3B C 0.55982(19) -0.1069(5) 0.3185(3) 0.0718(13) Uani 1 1 d . . . . . H3BA H 0.5574 -0.1575 0.3460 0.086 Uiso 1 1 calc R . . . . H3BB H 0.5748 -0.1570 0.3059 0.086 Uiso 1 1 calc R . . . . C4B C 0.59346(17) 0.0007(5) 0.3592(2) 0.0672(11) Uani 1 1 d . . . . . H4B H 0.5805 0.0639 0.3671 0.081 Uiso 1 1 calc R . . . . C5B C 0.63884(19) 0.0141(7) 0.3845(3) 0.0849(17) Uani 1 1 d . . . . . H5B H 0.6517 -0.0450 0.3744 0.102 Uiso 1 1 calc R . . . . C6B C 0.6720(2) 0.1199(8) 0.4294(3) 0.100(2) Uani 1 1 d . . . . . H6BA H 0.6518 0.1921 0.4182 0.120 Uiso 1 1 calc R . . . . H6BB H 0.6942 0.1400 0.4221 0.120 Uiso 1 1 calc R . . . . C7B C 0.7027(2) 0.0872(9) 0.5034(3) 0.108(3) Uani 1 1 d . . . . . H7BA H 0.7181 0.0072 0.5125 0.129 Uiso 1 1 calc R . . . . H7BB H 0.7288 0.1479 0.5310 0.129 Uiso 1 1 calc R . . . . C8B C 0.67148(18) 0.0841(7) 0.5209(2) 0.0822(16) Uani 1 1 d . . . . . H8B H 0.6676 0.1578 0.5348 0.099 Uiso 1 1 calc R . . . . C9B C 0.64870(15) -0.0145(5) 0.5187(2) 0.0661(12) Uani 1 1 d . . . . . H9B H 0.6526 -0.0888 0.5052 0.079 Uiso 1 1 calc R . . . . C10B C 0.61737(14) -0.0151(5) 0.53619(19) 0.0566(10) Uani 1 1 d . . . . . H10B H 0.6175 0.0682 0.5506 0.068 Uiso 1 1 calc R . . . . C11B C 0.56439(14) -0.0535(5) 0.48087(19) 0.0584(9) Uani 1 1 d . . . . . H11G H 0.5508 -0.0795 0.5004 0.070 Uiso 1 1 calc R . . . . H11H H 0.5641 -0.1248 0.4587 0.070 Uiso 1 1 calc R . . . . C12B C 0.53064(13) 0.0437(4) 0.42894(17) 0.0465(8) Uani 1 1 d . . . . . C13B C 0.47703(13) 0.0038(4) 0.37407(18) 0.0488(8) Uani 1 1 d . . . . . H13G H 0.4762 -0.0619 0.3488 0.059 Uiso 1 1 calc R . . . . H13H H 0.4653 -0.0306 0.3948 0.059 Uiso 1 1 calc R . . . . C14B C 0.44123(12) 0.1030(4) 0.32594(17) 0.0465(8) Uani 1 1 d . . . . . C15B C 0.42133(13) 0.1797(4) 0.34447(18) 0.0499(9) Uani 1 1 d . . . . . C16B C 0.38415(14) 0.2666(5) 0.3013(2) 0.0585(10) Uani 1 1 d . . . . . C17B C 0.36557(16) 0.2757(6) 0.2373(2) 0.0700(13) Uani 1 1 d . . . . . H17B H 0.3398 0.3303 0.2075 0.084 Uiso 1 1 calc R . . . . C18B C 0.38515(15) 0.2039(5) 0.21716(19) 0.0647(12) Uani 1 1 d . . . . . C19B C 0.42426(14) 0.1183(4) 0.26092(18) 0.0510(9) Uani 1 1 d . . . . . C20B C 0.44682(15) 0.0611(5) 0.23740(19) 0.0558(10) Uani 1 1 d . . . . . Cl1B Cl 0.44230(4) 0.17415(13) 0.42411(5) 0.0709(3) Uani 1 1 d . . . . . O1B O 0.43110(13) 0.0779(4) 0.18092(15) 0.0826(11) Uani 1 1 d . . . . . O2B O 0.48630(10) -0.0092(3) 0.28032(13) 0.0581(7) Uani 1 1 d . . . . . O3B O 0.63806(11) -0.0988(4) 0.59074(15) 0.0785(11) Uani 1 1 d . . . . . H3BC H 0.6683 -0.1016 0.6144 0.118 Uiso 1 1 calc GR . . . . O4B O 0.54466(11) 0.1459(3) 0.43131(15) 0.0639(8) Uani 1 1 d . . . . . O5B O 0.36450(13) 0.3408(4) 0.31813(17) 0.0828(11) Uani 1 1 d . . . . . H5BA H 0.3739 0.3192 0.3542 0.124 Uiso 1 1 calc GR . . . . O6B O 0.36453(14) 0.2199(5) 0.15341(16) 0.0945(14) Uani 1 1 d . . . . . H6BC H 0.3819 0.1866 0.1478 0.142 Uiso 1 1 calc GR . . . . C4C C 0.2346(2) 0.9651(8) 0.1534(3) 0.111(2) Uani 1 1 d D . . . . H4C H 0.2042 0.9318 0.1358 0.133 Uiso 0.536(10) 1 calc R . P A 1 H4CA H 0.2233 0.8939 0.1590 0.133 Uiso 0.464(10) 1 calc R . P A 2 C5C C 0.2423(2) 0.9687(8) 0.1125(3) 0.100(2) Uani 1 1 d . . . . . H5C H 0.2667 1.0221 0.1227 0.120 Uiso 1 1 calc R . . . . C6C C 0.2151(3) 0.8943(9) 0.0512(3) 0.114(3) Uani 1 1 d . . . . . H6CA H 0.1997 0.8248 0.0543 0.137 Uiso 1 1 calc R . . . . H6CB H 0.2385 0.8616 0.0481 0.137 Uiso 1 1 calc R . . . . C7C C 0.1753(3) 0.9665(10) -0.0117(4) 0.132(3) Uani 1 1 d . . . . . H7CA H 0.1896 1.0436 -0.0105 0.159 Uiso 1 1 calc R . . . . H7CB H 0.1653 0.9197 -0.0498 0.159 Uiso 1 1 calc R . . . . C8C C 0.1309(2) 0.9948(8) -0.0220(3) 0.0941(19) Uani 1 1 d . . . . . H8C H 0.1061 0.9349 -0.0445 0.113 Uiso 1 1 calc R . . . . C9C C 0.1215(2) 1.0922(6) -0.0040(3) 0.0797(15) Uani 1 1 d . . . . . H9C H 0.1456 1.1536 0.0178 0.096 Uiso 1 1 calc R . . . . C10C C 0.07581(18) 1.1158(5) -0.0148(3) 0.0727(13) Uani 1 1 d . . . . . H10C H 0.0519 1.0503 -0.0439 0.087 Uiso 1 1 calc R . . . . C11C C 0.0829(2) 1.1175(5) 0.0459(3) 0.0806(15) Uani 1 1 d . . . . . H11A H 0.0526 1.1492 0.0336 0.097 Uiso 1 1 calc R . . . . H11B H 0.1090 1.1767 0.0764 0.097 Uiso 1 1 calc R . . . . C12C C 0.09573(16) 0.9997(5) 0.0838(2) 0.0615(10) Uani 1 1 d . . . . . C13C C 0.1012(2) 1.0167(5) 0.1443(3) 0.0685(12) Uani 1 1 d . . . . . H13A H 0.1266 1.0785 0.1729 0.082 Uiso 1 1 calc R . . . . H13B H 0.0702 1.0490 0.1296 0.082 Uiso 1 1 calc R . . . . C14C C 0.11448(16) 0.9023(4) 0.1854(2) 0.0569(9) Uani 1 1 d . . . . . C15C C 0.07573(16) 0.8263(4) 0.1657(2) 0.0563(10) Uani 1 1 d . . . . . C16C C 0.08213(16) 0.7268(5) 0.2037(2) 0.0573(10) Uani 1 1 d . . . . . C17C C 0.12911(17) 0.7024(5) 0.2630(2) 0.0664(12) Uani 1 1 d . . . . . H17C H 0.1339 0.6384 0.2899 0.080 Uiso 1 1 calc R . . . . C18C C 0.16884(17) 0.7703(6) 0.2832(2) 0.0705(13) Uani 1 1 d . . . . . C19C C 0.16306(15) 0.8717(5) 0.2448(2) 0.0643(12) Uani 1 1 d . . . . . C20C C 0.20851(18) 0.9341(6) 0.2683(2) 0.0758(14) Uani 1 1 d . . . . . Cl1C Cl 0.01552(4) 0.85215(14) 0.09075(6) 0.0787(3) Uani 1 1 d . . . . . O1C O 0.24928(14) 0.9149(6) 0.32298(19) 0.1109(17) Uani 1 1 d . U . . . O2C O 0.20330(15) 1.0101(4) 0.2248(2) 0.0905(12) Uani 1 1 d D . . . . O3C O 0.05364(14) 1.2330(4) -0.04939(19) 0.0859(11) Uani 1 1 d . . . . . H3C H 0.0716 1.2900 -0.0244 0.129 Uiso 1 1 calc GR . . . . O4C O 0.10006(16) 0.9016(3) 0.06765(18) 0.0809(10) Uani 1 1 d . . . . . O5C O 0.04502(12) 0.6536(4) 0.18694(16) 0.0729(9) Uani 1 1 d . . . . . H5CA H 0.0188 0.6757 0.1509 0.109 Uiso 1 1 calc GR . . . . O6C O 0.21344(13) 0.7365(6) 0.34142(18) 0.1117(18) Uani 1 1 d . . . . . H6C H 0.2355 0.7627 0.3429 0.168 Uiso 1 1 calc GR . . . . C1C C 0.2182(4) 1.2030(9) 0.1905(6) 0.084(3) Uani 0.536(10) 1 d D . P A 1 H1CA H 0.2443 1.2580 0.2039 0.126 Uiso 0.536(10) 1 calc GR . P A 1 H1CB H 0.1962 1.2449 0.1934 0.126 Uiso 0.536(10) 1 calc GR . P A 1 H1CC H 0.2000 1.1768 0.1454 0.126 Uiso 0.536(10) 1 calc GR . P A 1 C2C C 0.2401(4) 1.0924(9) 0.2356(6) 0.076(4) Uani 0.536(10) 1 d D . P A 1 H2C H 0.2625 1.1211 0.2819 0.091 Uiso 0.536(10) 1 calc R . P A 1 C3C C 0.2685(3) 1.0081(9) 0.2270(4) 0.075(3) Uani 0.536(10) 1 d D . P A 1 H3CA H 0.2802 0.9368 0.2560 0.090 Uiso 0.536(10) 1 calc R . P A 1 H3CB H 0.2972 1.0511 0.2394 0.090 Uiso 0.536(10) 1 calc R . P A 1 C1D C 0.2752(6) 1.1506(14) 0.3038(7) 0.102(5) Uani 0.464(10) 1 d D . P A 2 H1DA H 0.2517 1.2169 0.2854 0.153 Uiso 0.464(10) 1 calc GR . P A 2 H1DB H 0.3052 1.1805 0.3154 0.153 Uiso 0.464(10) 1 calc GR . P A 2 H1DC H 0.2826 1.1192 0.3430 0.153 Uiso 0.464(10) 1 calc GR . P A 2 C2D C 0.2536(4) 1.0488(14) 0.2530(5) 0.068(4) Uani 0.464(10) 1 d D . P A 2 H2D H 0.2758 0.9772 0.2740 0.081 Uiso 0.464(10) 1 calc R . P A 2 C3D C 0.2450(4) 1.0845(10) 0.1918(5) 0.086(4) Uani 0.464(10) 1 d D . P A 2 H3DA H 0.2740 1.1257 0.2044 0.103 Uiso 0.464(10) 1 calc R . P A 2 H3DB H 0.2169 1.1403 0.1642 0.103 Uiso 0.464(10) 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 C1 0.119(5) 0.057(3) 0.105(4) -0.002(3) 0.081(4) -0.002(3) C2 0.100(4) 0.062(3) 0.070(3) 0.006(2) 0.060(3) -0.004(3) C3 0.114(4) 0.075(3) 0.091(4) -0.011(3) 0.081(4) -0.019(3) C4 0.096(4) 0.087(4) 0.126(5) -0.027(4) 0.089(4) -0.016(3) C5 0.115(5) 0.149(7) 0.143(6) -0.046(5) 0.106(5) -0.023(5) C6 0.089(4) 0.197(8) 0.134(6) -0.054(6) 0.078(4) 0.009(5) C7 0.094(4) 0.194(8) 0.128(5) -0.047(5) 0.085(4) -0.011(5) C8 0.078(3) 0.144(6) 0.109(4) -0.039(4) 0.063(3) -0.006(4) C9 0.067(3) 0.110(4) 0.077(3) -0.023(3) 0.052(2) -0.016(3) C10 0.053(2) 0.070(3) 0.052(2) -0.0060(19) 0.0338(18) 0.000(2) C11 0.052(2) 0.065(3) 0.0503(19) -0.006(2) 0.0300(17) 0.001(2) C12 0.0485(19) 0.057(2) 0.0442(18) 0.0007(17) 0.0295(16) 0.0034(18) C13 0.0500(19) 0.060(2) 0.0415(17) -0.0023(17) 0.0258(16) 0.0066(18) C14 0.0408(18) 0.065(3) 0.0434(18) -0.0011(17) 0.0231(15) 0.0094(18) C15 0.0447(19) 0.070(3) 0.0453(19) -0.0029(19) 0.0269(17) 0.0035(19) C16 0.0441(19) 0.066(3) 0.056(2) -0.004(2) 0.0308(18) 0.0043(19) C17 0.048(2) 0.077(3) 0.052(2) -0.014(2) 0.0270(19) -0.004(2) C18 0.051(2) 0.084(3) 0.044(2) -0.010(2) 0.0261(18) 0.000(2) C19 0.048(2) 0.074(3) 0.0403(18) 0.0009(18) 0.0242(16) 0.006(2) C20 0.067(3) 0.073(3) 0.045(2) 0.000(2) 0.033(2) 0.002(2) Cl1 0.0677(6) 0.0928(9) 0.0497(5) -0.0048(5) 0.0380(5) -0.0087(6) O1 0.105(3) 0.126(4) 0.0483(17) 0.006(2) 0.0413(19) -0.018(3) O2 0.0678(17) 0.073(2) 0.0543(15) 0.0058(15) 0.0393(14) -0.0020(16) O3 0.0492(15) 0.115(3) 0.0562(16) -0.0238(19) 0.0284(14) -0.0029(18) O4 0.0570(17) 0.060(2) 0.077(2) -0.0072(16) 0.0362(16) 0.0044(15) O5 0.0624(18) 0.079(2) 0.0710(19) -0.0044(17) 0.0441(17) -0.0083(16) O6 0.073(2) 0.119(3) 0.0416(15) -0.0176(18) 0.0299(15) -0.015(2) C1A 0.109(5) 0.098(5) 0.118(5) -0.031(4) 0.075(4) -0.044(4) C2A 0.060(2) 0.079(3) 0.077(3) -0.013(3) 0.045(2) -0.021(2) C3A 0.075(3) 0.088(4) 0.086(3) -0.004(3) 0.056(3) -0.018(3) C4A 0.061(2) 0.092(4) 0.074(3) -0.006(3) 0.045(2) -0.013(3) C5A 0.052(2) 0.110(5) 0.073(3) 0.012(3) 0.039(2) 0.008(3) C6A 0.064(3) 0.124(5) 0.080(3) 0.000(3) 0.046(3) 0.023(3) C7A 0.060(3) 0.159(6) 0.069(3) -0.003(4) 0.043(2) 0.018(4) C8A 0.056(2) 0.096(4) 0.057(2) -0.001(3) 0.0358(19) 0.010(3) C9A 0.056(2) 0.083(3) 0.051(2) 0.002(2) 0.0347(19) 0.002(2) C10A 0.051(2) 0.065(3) 0.0451(18) 0.0027(18) 0.0308(17) 0.0055(19) C11A 0.063(2) 0.062(3) 0.0464(19) 0.0067(18) 0.0362(19) 0.013(2) C12A 0.0431(17) 0.057(2) 0.0442(18) -0.0001(17) 0.0272(15) 0.0007(17) C13A 0.0509(19) 0.057(2) 0.0417(17) -0.0006(17) 0.0278(16) 0.0032(18) C14A 0.0461(17) 0.063(2) 0.0414(16) 0.0027(17) 0.0293(15) 0.0081(17) C15A 0.0429(18) 0.076(3) 0.0398(17) -0.0032(18) 0.0251(15) 0.0012(18) C16A 0.051(2) 0.079(3) 0.058(2) -0.007(2) 0.0396(19) -0.007(2) C17A 0.058(2) 0.079(3) 0.055(2) 0.010(2) 0.039(2) 0.002(2) C18A 0.049(2) 0.085(3) 0.047(2) 0.013(2) 0.0287(18) 0.011(2) C19A 0.0418(17) 0.065(3) 0.0423(16) 0.0016(18) 0.0258(15) 0.0035(18) C20A 0.0477(19) 0.066(3) 0.0478(19) -0.0024(19) 0.0285(17) -0.0041(19) Cl1A 0.0438(5) 0.1378(12) 0.0481(5) 0.0105(7) 0.0219(4) 0.0022(7) O1A 0.0432(14) 0.130(3) 0.0532(16) 0.007(2) 0.0197(13) -0.008(2) O2A 0.0540(15) 0.071(2) 0.0625(16) -0.0049(15) 0.0374(14) -0.0110(15) O3A 0.0649(18) 0.100(3) 0.0487(15) 0.0166(16) 0.0377(14) 0.0202(18) O4A 0.0804(19) 0.0532(18) 0.0623(16) -0.0006(14) 0.0501(16) 0.0040(15) O5A 0.0621(19) 0.120(3) 0.074(2) -0.002(2) 0.0480(18) -0.021(2) O6A 0.0544(18) 0.147(4) 0.0562(18) 0.040(2) 0.0250(16) 0.009(2) C1B 0.095(4) 0.096(5) 0.104(4) -0.033(4) 0.074(4) -0.016(3) C2B 0.068(2) 0.072(3) 0.068(2) -0.004(2) 0.052(2) 0.005(2) C3B 0.077(3) 0.072(3) 0.087(3) 0.012(3) 0.063(3) 0.018(2) C4B 0.063(2) 0.074(3) 0.069(3) 0.011(2) 0.045(2) 0.012(2) C5B 0.064(3) 0.128(5) 0.076(3) 0.020(3) 0.052(3) 0.010(3) C6B 0.076(3) 0.144(6) 0.089(4) 0.008(4) 0.059(3) -0.021(4) C7B 0.056(3) 0.187(8) 0.071(3) 0.007(4) 0.039(3) -0.018(4) C8B 0.059(3) 0.119(5) 0.063(3) 0.006(3) 0.038(2) -0.011(3) C9B 0.053(2) 0.086(3) 0.055(2) 0.012(2) 0.0339(19) 0.013(2) C10B 0.051(2) 0.069(3) 0.0472(19) 0.0105(19) 0.0314(17) 0.0033(19) C11B 0.0512(19) 0.062(3) 0.0500(18) 0.012(2) 0.0288(17) 0.002(2) C12B 0.0452(17) 0.052(2) 0.0415(17) 0.0025(16) 0.0286(15) -0.0005(16) C13B 0.0460(18) 0.056(2) 0.0426(17) 0.0046(16) 0.0285(15) -0.0011(17) C14B 0.0368(16) 0.058(2) 0.0405(17) -0.0001(16) 0.0240(14) -0.0040(16) C15B 0.0406(17) 0.066(3) 0.0400(17) -0.0026(17) 0.0255(15) -0.0034(17) C16B 0.0432(19) 0.078(3) 0.053(2) 0.002(2) 0.0314(18) 0.007(2) C17B 0.051(2) 0.102(4) 0.048(2) 0.013(2) 0.0294(19) 0.019(2) C18B 0.049(2) 0.097(4) 0.0412(19) 0.015(2) 0.0273(18) 0.015(2) C19B 0.0416(17) 0.068(3) 0.0399(17) 0.0021(17) 0.0258(15) 0.0017(17) C20B 0.050(2) 0.072(3) 0.0447(19) -0.0002(19) 0.0314(17) -0.0017(19) Cl1B 0.0677(6) 0.1018(10) 0.0474(5) 0.0055(5) 0.0401(5) 0.0120(6) O1B 0.073(2) 0.131(3) 0.0477(15) 0.0104(19) 0.0416(15) 0.022(2) O2B 0.0574(15) 0.0704(19) 0.0541(14) 0.0016(14) 0.0403(13) 0.0069(14) O3B 0.0516(15) 0.116(3) 0.0552(16) 0.0299(19) 0.0303(14) 0.0111(19) O4B 0.0516(15) 0.0554(18) 0.0648(17) 0.0061(14) 0.0304(14) -0.0033(14) O5B 0.0674(19) 0.115(3) 0.0655(19) 0.006(2) 0.0442(18) 0.032(2) O6B 0.079(2) 0.153(4) 0.0456(16) 0.029(2) 0.0391(17) 0.044(3) C4C 0.094(4) 0.142(7) 0.121(5) -0.056(5) 0.082(4) -0.040(4) C5C 0.078(3) 0.128(6) 0.102(4) -0.005(4) 0.063(3) 0.002(4) C6C 0.117(5) 0.153(7) 0.095(4) 0.019(5) 0.080(4) 0.037(5) C7C 0.140(6) 0.181(9) 0.095(4) 0.048(5) 0.087(5) 0.069(7) C8C 0.082(4) 0.127(6) 0.060(3) 0.009(3) 0.042(3) 0.008(4) C9C 0.065(3) 0.093(4) 0.063(3) 0.020(3) 0.035(2) 0.004(3) C10C 0.057(2) 0.070(3) 0.067(3) 0.007(2) 0.032(2) -0.001(2) C11C 0.081(3) 0.067(3) 0.090(4) 0.013(3) 0.055(3) 0.001(3) C12C 0.055(2) 0.056(3) 0.062(2) -0.001(2) 0.034(2) -0.006(2) C13C 0.077(3) 0.051(3) 0.082(3) -0.009(2) 0.055(3) -0.003(2) C14C 0.062(2) 0.057(2) 0.059(2) -0.0095(19) 0.043(2) -0.0027(19) C15C 0.054(2) 0.060(3) 0.053(2) -0.0026(19) 0.0350(19) 0.0050(19) C16C 0.055(2) 0.071(3) 0.051(2) -0.0023(19) 0.0375(19) -0.002(2) C17C 0.059(2) 0.091(4) 0.052(2) 0.010(2) 0.038(2) 0.008(2) C18C 0.053(2) 0.109(4) 0.047(2) 0.003(2) 0.0325(19) 0.005(2) C19C 0.051(2) 0.092(4) 0.048(2) -0.015(2) 0.0319(18) -0.008(2) C20C 0.067(3) 0.104(4) 0.059(2) -0.024(3) 0.043(2) -0.025(3) Cl1C 0.0547(6) 0.0844(8) 0.0706(7) 0.0153(6) 0.0306(5) 0.0053(6) O1C 0.060(2) 0.185(5) 0.071(2) -0.023(3) 0.0364(18) -0.033(3) O2C 0.091(2) 0.112(3) 0.090(2) -0.042(2) 0.069(2) -0.049(2) O3C 0.067(2) 0.080(2) 0.072(2) 0.0226(19) 0.0300(17) 0.0084(19) O4C 0.120(3) 0.056(2) 0.075(2) -0.0046(17) 0.069(2) -0.004(2) O5C 0.0636(18) 0.081(2) 0.0650(19) 0.0078(17) 0.0392(16) -0.0066(18) O6C 0.0537(19) 0.197(6) 0.060(2) 0.032(3) 0.0271(17) 0.003(3) C1C 0.073(6) 0.060(6) 0.109(8) 0.003(6) 0.057(6) 0.002(5) C2C 0.083(8) 0.077(9) 0.065(7) -0.004(6) 0.049(6) -0.022(7) C3C 0.049(4) 0.085(7) 0.079(6) 0.032(5) 0.037(4) 0.012(4) C1D 0.119(11) 0.092(10) 0.089(9) -0.022(8) 0.066(9) -0.024(9) C2D 0.072(7) 0.068(9) 0.055(7) -0.007(6) 0.039(6) -0.021(7) C3D 0.061(6) 0.097(10) 0.089(8) 0.009(8) 0.045(6) -0.013(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 C2 C3 114.0(5) . . ? O2 C2 C1 105.6(4) . . ? O2 C2 C3 109.1(4) . . ? C4 C3 C2 113.6(4) . . ? C5 C4 C3 127.3(7) . . ? C4 C5 C6 125.0(9) . . ? C5 C6 C7 111.4(8) . . ? C8 C7 C6 110.7(7) . . ? C9 C8 C7 127.5(9) . . ? C8 C9 C10 127.7(7) . . ? C9 C10 C11 113.4(4) . . ? O3 C10 C9 109.4(4) . . ? O3 C10 C11 106.1(3) . . ? C12 C11 C10 115.3(4) . . ? C11 C12 C13 114.5(4) . . ? O4 C12 C11 122.8(4) . . ? O4 C12 C13 122.7(4) . . ? C14 C13 C12 114.5(4) . . ? C15 C14 C13 118.8(4) . . ? C15 C14 C19 117.7(4) . . ? C19 C14 C13 123.5(4) . . ? C14 C15 C16 122.9(4) . . ? C14 C15 Cl1 120.6(3) . . ? C16 C15 Cl1 116.4(3) . . ? C17 C16 C15 119.2(4) . . ? O5 C16 C15 124.1(4) . . ? O5 C16 C17 116.7(4) . . ? C16 C17 C18 119.5(4) . . ? C17 C18 C19 121.7(4) . . ? O6 C18 C17 115.9(4) . . ? O6 C18 C19 122.4(5) . . ? C14 C19 C20 124.1(4) . . ? C18 C19 C14 118.9(4) . . ? C18 C19 C20 116.9(4) . . ? O1 C20 C19 122.7(5) . . ? O1 C20 O2 121.4(5) . . ? O2 C20 C19 115.7(3) . . ? C20 O2 C2 118.3(4) . . ? C3A C2A C1A 113.9(5) . . ? O2A C2A C1A 108.9(5) . . ? O2A C2A C3A 104.5(4) . . ? C2A C3A C4A 114.8(5) . . ? C5A C4A C3A 125.7(5) . . ? C4A C5A C6A 126.8(6) . . ? C5A C6A C7A 112.5(6) . . ? C8A C7A C6A 111.9(5) . . ? C9A C8A C7A 128.2(6) . . ? C8A C9A C10A 126.0(5) . . ? C9A C10A C11A 113.6(3) . . ? O3A C10A C9A 110.3(4) . . ? O3A C10A C11A 105.8(3) . . ? C12A C11A C10A 114.7(4) . . ? C11A C12A C13A 115.1(4) . . ? O4A C12A C11A 122.5(4) . . ? O4A C12A C13A 122.4(4) . . ? C12A C13A C14A 114.2(4) . . ? C15A C14A C13A 116.9(3) . . ? C15A C14A C19A 118.1(4) . . ? C19A C14A C13A 125.0(4) . . ? C14A C15A Cl1A 119.9(3) . . ? C16A C15A C14A 122.6(4) . . ? C16A C15A Cl1A 117.5(3) . . ? C17A C16A C15A 119.1(4) . . ? O5A C16A C15A 123.5(4) . . ? O5A C16A C17A 117.4(4) . . ? C18A C17A C16A 120.0(4) . . ? C17A C18A C19A 121.7(4) . . ? O6A C18A C17A 115.5(4) . . ? O6A C18A C19A 122.8(4) . . ? C14A C19A C18A 118.2(4) . . ? C14A C19A C20A 124.8(4) . . ? C18A C19A C20A 116.9(3) . . ? O1A C20A C19A 122.0(4) . . ? O1A C20A O2A 122.0(4) . . ? O2A C20A C19A 115.8(3) . . ? C20A O2A C2A 117.5(4) . . ? C1B C2B C3B 112.8(5) . . ? O2B C2B C1B 108.7(4) . . ? O2B C2B C3B 104.9(3) . . ? C4B C3B C2B 114.3(4) . . ? C5B C4B C3B 126.4(5) . . ? C4B C5B C6B 123.8(6) . . ? C5B C6B C7B 111.4(6) . . ? C8B C7B C6B 111.7(5) . . ? C9B C8B C7B 125.8(7) . . ? C8B C9B C10B 124.7(5) . . ? C9B C10B C11B 115.1(4) . . ? O3B C10B C9B 109.6(4) . . ? O3B C10B C11B 106.9(3) . . ? C10B C11B C12B 115.8(4) . . ? C11B C12B C13B 115.0(3) . . ? O4B C12B C11B 122.8(4) . . ? O4B C12B C13B 122.2(4) . . ? C14B C13B C12B 116.2(3) . . ? C15B C14B C13B 118.1(3) . . ? C15B C14B C19B 117.9(4) . . ? C19B C14B C13B 123.9(4) . . ? C14B C15B C16B 123.0(3) . . ? C14B C15B Cl1B 121.1(3) . . ? C16B C15B Cl1B 115.9(3) . . ? C17B C16B C15B 119.1(4) . . ? O5B C16B C15B 123.9(4) . . ? O5B C16B C17B 117.0(4) . . ? C16B C17B C18B 120.0(4) . . ? C17B C18B C19B 121.9(4) . . ? O6B C18B C17B 115.5(4) . . ? O6B C18B C19B 122.6(4) . . ? C14B C19B C20B 125.0(4) . . ? C18B C19B C14B 118.0(4) . . ? C18B C19B C20B 116.8(3) . . ? O1B C20B C19B 122.6(4) . . ? O1B C20B O2B 120.4(4) . . ? O2B C20B C19B 117.0(3) . . ? C20B O2B C2B 117.4(3) . . ? C5C C4C C3C 129.5(7) . . ? C5C C4C C3D 116.6(8) . . ? C4C C5C C6C 124.6(7) . . ? C5C C6C C7C 113.3(8) . . ? C8C C7C C6C 115.0(6) . . ? C9C C8C C7C 128.6(8) . . ? C8C C9C C10C 126.5(6) . . ? C11C C10C C9C 115.5(4) . . ? O3C C10C C9C 109.8(4) . . ? O3C C10C C11C 108.2(5) . . ? C10C C11C C12C 119.2(5) . . ? C11C C12C C13C 112.7(4) . . ? O4C C12C C11C 124.4(4) . . ? O4C C12C C13C 122.8(4) . . ? C14C C13C C12C 115.9(4) . . ? C15C C14C C13C 117.3(4) . . ? C15C C14C C19C 117.9(4) . . ? C19C C14C C13C 124.7(4) . . ? C14C C15C C16C 123.0(4) . . ? C14C C15C Cl1C 120.7(3) . . ? C16C C15C Cl1C 116.3(3) . . ? C17C C16C C15C 118.3(4) . . ? O5C C16C C15C 124.4(4) . . ? O5C C16C C17C 117.2(4) . . ? C18C C17C C16C 121.1(5) . . ? C17C C18C C19C 121.3(4) . . ? O6C C18C C17C 116.3(5) . . ? O6C C18C C19C 122.4(5) . . ? C14C C19C C18C 118.2(4) . . ? C14C C19C C20C 124.4(5) . . ? C18C C19C C20C 117.3(4) . . ? O1C C20C C19C 122.9(5) . . ? O1C C20C O2C 120.9(5) . . ? O2C C20C C19C 116.1(4) . . ? C20C O2C C2C 128.5(6) . . ? C20C O2C C2D 108.2(6) . . ? O2C C2C C1C 113.9(8) . . ? O2C C2C C3C 102.9(7) . . ? C3C C2C C1C 114.2(9) . . ? C2C C3C C4C 109.7(8) . . ? O2C C2D C1D 112.9(11) . . ? O2C C2D C3D 102.7(8) . . ? C1D C2D C3D 114.0(11) . . ? C2D C3D C4C 107.4(9) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.493(8) . ? C2 C3 1.497(8) . ? C2 O2 1.475(6) . ? C3 C4 1.487(9) . ? C4 C5 1.323(9) . ? C5 C6 1.479(13) . ? C6 C7 1.536(10) . ? C7 C8 1.506(10) . ? C8 C9 1.255(9) . ? C9 C10 1.485(6) . ? C10 C11 1.510(6) . ? C10 O3 1.441(5) . ? C11 C12 1.507(6) . ? C12 C13 1.515(5) . ? C12 O4 1.206(5) . ? C13 C14 1.507(6) . ? C14 C15 1.381(7) . ? C14 C19 1.420(5) . ? C15 C16 1.397(6) . ? C15 Cl1 1.741(4) . ? C16 C17 1.377(6) . ? C16 O5 1.346(6) . ? C17 C18 1.385(7) . ? C18 C19 1.404(7) . ? C18 O6 1.353(5) . ? C19 C20 1.474(7) . ? C20 O1 1.221(5) . ? C20 O2 1.333(6) . ? C1A C2A 1.497(9) . ? C2A C3A 1.488(8) . ? C2A O2A 1.484(5) . ? C3A C4A 1.494(8) . ? C4A C5A 1.304(7) . ? C5A C6A 1.485(9) . ? C6A C7A 1.522(8) . ? C7A C8A 1.492(6) . ? C8A C9A 1.290(7) . ? C9A C10A 1.486(6) . ? C10A C11A 1.532(5) . ? C10A O3A 1.446(5) . ? C11A C12A 1.513(6) . ? C12A C13A 1.514(5) . ? C12A O4A 1.202(5) . ? C13A C14A 1.519(6) . ? C14A C15A 1.391(6) . ? C14A C19A 1.409(5) . ? C15A C16A 1.389(6) . ? C15A Cl1A 1.738(4) . ? C16A C17A 1.378(6) . ? C16A O5A 1.344(5) . ? C17A C18A 1.368(6) . ? C18A C19A 1.421(6) . ? C18A O6A 1.357(5) . ? C19A C20A 1.476(5) . ? C20A O1A 1.230(5) . ? C20A O2A 1.307(5) . ? C1B C2B 1.505(8) . ? C2B C3B 1.507(7) . ? C2B O2B 1.476(5) . ? C3B C4B 1.504(8) . ? C4B C5B 1.298(7) . ? C5B C6B 1.509(10) . ? C6B C7B 1.539(8) . ? C7B C8B 1.483(8) . ? C8B C9B 1.324(8) . ? C9B C10B 1.485(6) . ? C10B C11B 1.502(6) . ? C10B O3B 1.438(5) . ? C11B C12B 1.509(6) . ? C12B C13B 1.519(5) . ? C12B O4B 1.201(5) . ? C13B C14B 1.507(6) . ? C14B C15B 1.389(6) . ? C14B C19B 1.425(5) . ? C15B C16B 1.400(6) . ? C15B Cl1B 1.731(4) . ? C16B C17B 1.372(6) . ? C16B O5B 1.333(5) . ? C17B C18B 1.381(7) . ? C18B C19B 1.423(6) . ? C18B O6B 1.349(5) . ? C19B C20B 1.459(6) . ? C20B O1B 1.229(5) . ? C20B O2B 1.324(5) . ? C4C C5C 1.300(9) . ? C4C C3C 1.552(9) . ? C4C C3D 1.537(10) . ? C5C C6C 1.474(10) . ? C6C C7C 1.518(10) . ? C7C C8C 1.466(10) . ? C8C C9C 1.296(9) . ? C9C C10C 1.493(8) . ? C10C C11C 1.473(8) . ? C10C O3C 1.458(6) . ? C11C C12C 1.499(7) . ? C12C C13C 1.514(7) . ? C12C O4C 1.196(6) . ? C13C C14C 1.509(7) . ? C14C C15C 1.389(6) . ? C14C C19C 1.417(6) . ? C15C C16C 1.392(6) . ? C15C Cl1C 1.741(4) . ? C16C C17C 1.375(6) . ? C16C O5C 1.350(5) . ? C17C C18C 1.362(7) . ? C18C C19C 1.423(8) . ? C18C O6C 1.349(6) . ? C19C C20C 1.473(7) . ? C20C O1C 1.221(6) . ? C20C O2C 1.336(7) . ? O2C C2C 1.459(9) . ? O2C C2D 1.488(10) . ? C1C C2C 1.500(8) . ? C2C C3C 1.500(10) . ? C1D C2D 1.505(11) . ? C2D C3D 1.507(10) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O3B 0.82 2.07 2.776(5) 144.5 1_565 O6 H6 O1 0.82 1.84 2.538(7) 142.0 . C13A H13F O2A 0.97 2.13 2.762(5) 121.5 . O3A H3AC O1B 0.82 2.10 2.874(4) 156.7 4 O5A H5AB O3C 0.82 2.00 2.706(5) 144.4 2_545 O6A H6AC O1A 0.82 1.79 2.518(6) 146.5 . O5B H5BA O3 0.82 2.10 2.723(4) 133.0 . O6B H6BC O1B 0.82 1.80 2.514(5) 145.3 . O5C H5CA O3A 0.82 2.06 2.757(5) 142.1 2 O6C H6C O1C 0.82 1.90 2.549(7) 135.6 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 -57.8(6) . . . . ? C1 C2 O2 C20 -150.4(5) . . . . ? C2 C3 C4 C5 109.8(7) . . . . ? C3 C2 O2 C20 86.6(6) . . . . ? C3 C4 C5 C6 176.4(6) . . . . ? C4 C5 C6 C7 107.3(9) . . . . ? C5 C6 C7 C8 -86.2(11) . . . . ? C6 C7 C8 C9 114.6(9) . . . . ? C7 C8 C9 C10 176.7(6) . . . . ? C8 C9 C10 C11 120.8(7) . . . . ? C8 C9 C10 O3 -121.0(6) . . . . ? C9 C10 C11 C12 -74.4(6) . . . . ? C10 C11 C12 C13 176.6(4) . . . . ? C10 C11 C12 O4 -5.8(6) . . . . ? C11 C12 C13 C14 173.5(4) . . . . ? C12 C13 C14 C15 -81.7(5) . . . . ? C12 C13 C14 C19 100.7(5) . . . . ? C13 C14 C15 C16 -177.0(4) . . . . ? C13 C14 C15 Cl1 4.3(5) . . . . ? C13 C14 C19 C18 173.9(4) . . . . ? C13 C14 C19 C20 -9.2(7) . . . . ? C14 C15 C16 C17 1.4(6) . . . . ? C14 C15 C16 O5 -178.2(4) . . . . ? C14 C19 C20 O1 165.4(5) . . . . ? C14 C19 C20 O2 -19.4(7) . . . . ? C15 C14 C19 C18 -3.7(6) . . . . ? C15 C14 C19 C20 173.2(4) . . . . ? C15 C16 C17 C18 -0.6(7) . . . . ? C16 C17 C18 C19 -2.5(7) . . . . ? C16 C17 C18 O6 177.4(4) . . . . ? C17 C18 C19 C14 4.7(7) . . . . ? C17 C18 C19 C20 -172.5(4) . . . . ? C18 C19 C20 O1 -17.5(8) . . . . ? C18 C19 C20 O2 157.7(4) . . . . ? C19 C14 C15 C16 0.8(6) . . . . ? C19 C14 C15 Cl1 -177.9(3) . . . . ? C19 C20 O2 C2 -176.8(4) . . . . ? Cl1 C15 C16 C17 -179.8(3) . . . . ? Cl1 C15 C16 O5 0.5(6) . . . . ? O1 C20 O2 C2 -1.6(8) . . . . ? O2 C2 C3 C4 60.0(6) . . . . ? O3 C10 C11 C12 165.4(4) . . . . ? O4 C12 C13 C14 -4.2(6) . . . . ? O5 C16 C17 C18 179.1(4) . . . . ? O6 C18 C19 C14 -175.2(4) . . . . ? O6 C18 C19 C20 7.6(7) . . . . ? C1A C2A C3A C4A 173.9(5) . . . . ? C1A C2A O2A C20A -73.5(6) . . . . ? C2A C3A C4A C5A -140.8(6) . . . . ? C3A C2A O2A C20A 164.4(5) . . . . ? C3A C4A C5A C6A -172.0(6) . . . . ? C4A C5A C6A C7A 95.2(8) . . . . ? C5A C6A C7A C8A -72.8(8) . . . . ? C6A C7A C8A C9A 95.8(8) . . . . ? C7A C8A C9A C10A 178.5(4) . . . . ? C8A C9A C10A C11A 122.5(5) . . . . ? C8A C9A C10A O3A -118.9(5) . . . . ? C9A C10A C11A C12A -76.2(5) . . . . ? C10A C11A C12A C13A 175.0(3) . . . . ? C10A C11A C12A O4A -6.8(6) . . . . ? C11A C12A C13A C14A 166.7(3) . . . . ? C12A C13A C14A C15A -75.2(4) . . . . ? C12A C13A C14A C19A 107.2(4) . . . . ? C13A C14A C15A C16A -177.4(4) . . . . ? C13A C14A C15A Cl1A 1.8(5) . . . . ? C13A C14A C19A C18A 173.3(4) . . . . ? C13A C14A C19A C20A -10.5(7) . . . . ? C14A C15A C16A C17A 2.9(7) . . . . ? C14A C15A C16A O5A -177.3(4) . . . . ? C14A C19A C20A O1A 176.5(5) . . . . ? C14A C19A C20A O2A -8.8(7) . . . . ? C15A C14A C19A C18A -4.3(6) . . . . ? C15A C14A C19A C20A 171.9(4) . . . . ? C15A C16A C17A C18A -1.9(7) . . . . ? C16A C17A C18A C19A -2.2(8) . . . . ? C16A C17A C18A O6A 178.7(5) . . . . ? C17A C18A C19A C14A 5.3(7) . . . . ? C17A C18A C19A C20A -171.2(5) . . . . ? C18A C19A C20A O1A -7.2(7) . . . . ? C18A C19A C20A O2A 167.5(4) . . . . ? C19A C14A C15A C16A 0.4(6) . . . . ? C19A C14A C15A Cl1A 179.6(3) . . . . ? C19A C20A O2A C2A -174.9(4) . . . . ? Cl1A C15A C16A C17A -176.4(4) . . . . ? Cl1A C15A C16A O5A 3.4(6) . . . . ? O1A C20A O2A C2A -0.2(7) . . . . ? O2A C2A C3A C4A -67.4(6) . . . . ? O3A C10A C11A C12A 162.7(4) . . . . ? O4A C12A C13A C14A -11.4(5) . . . . ? O5A C16A C17A C18A 178.2(5) . . . . ? O6A C18A C19A C14A -175.6(5) . . . . ? O6A C18A C19A C20A 7.8(7) . . . . ? C1B C2B C3B C4B 176.6(4) . . . . ? C1B C2B O2B C20B -77.3(5) . . . . ? C2B C3B C4B C5B -133.5(5) . . . . ? C3B C2B O2B C20B 161.8(4) . . . . ? C3B C4B C5B C6B -175.2(5) . . . . ? C4B C5B C6B C7B 91.6(7) . . . . ? C5B C6B C7B C8B -72.2(9) . . . . ? C6B C7B C8B C9B 91.4(9) . . . . ? C7B C8B C9B C10B -179.6(5) . . . . ? C8B C9B C10B C11B 119.8(5) . . . . ? C8B C9B C10B O3B -119.7(5) . . . . ? C9B C10B C11B C12B -78.4(5) . . . . ? C10B C11B C12B C13B -179.0(3) . . . . ? C10B C11B C12B O4B -0.5(6) . . . . ? C11B C12B C13B C14B 173.3(3) . . . . ? C12B C13B C14B C15B -82.9(4) . . . . ? C12B C13B C14B C19B 100.9(4) . . . . ? C13B C14B C15B C16B -173.5(4) . . . . ? C13B C14B C15B Cl1B 7.5(5) . . . . ? C13B C14B C19B C18B 171.0(4) . . . . ? C13B C14B C19B C20B -14.7(6) . . . . ? C14B C15B C16B C17B 1.2(7) . . . . ? C14B C15B C16B O5B 179.8(4) . . . . ? C14B C19B C20B O1B -179.3(5) . . . . ? C14B C19B C20B O2B -0.7(7) . . . . ? C15B C14B C19B C18B -5.1(6) . . . . ? C15B C14B C19B C20B 169.1(4) . . . . ? C15B C16B C17B C18B -3.0(8) . . . . ? C16B C17B C18B C19B 0.6(8) . . . . ? C16B C17B C18B O6B -179.7(5) . . . . ? C17B C18B C19B C14B 3.5(7) . . . . ? C17B C18B C19B C20B -171.2(5) . . . . ? C18B C19B C20B O1B -5.1(7) . . . . ? C18B C19B C20B O2B 173.6(4) . . . . ? C19B C14B C15B C16B 2.9(6) . . . . ? C19B C14B C15B Cl1B -176.2(3) . . . . ? C19B C20B O2B C2B 177.8(4) . . . . ? Cl1B C15B C16B C17B -179.7(4) . . . . ? Cl1B C15B C16B O5B -1.1(6) . . . . ? O1B C20B O2B C2B -3.6(6) . . . . ? O2B C2B C3B C4B -65.2(5) . . . . ? O3B C10B C11B C12B 159.6(4) . . . . ? O4B C12B C13B C14B -5.2(5) . . . . ? O5B C16B C17B C18B 178.3(5) . . . . ? O6B C18B C19B C14B -176.1(5) . . . . ? O6B C18B C19B C20B 9.2(7) . . . . ? C4C C5C C6C C7C 101.9(10) . . . . ? C5C C4C C3C C2C 128.1(10) . . . . ? C5C C4C C3D C2D -157.9(8) . . . . ? C5C C6C C7C C8C -73.4(11) . . . . ? C6C C7C C8C C9C 92.3(11) . . . . ? C7C C8C C9C C10C -179.0(6) . . . . ? C8C C9C C10C C11C 112.0(7) . . . . ? C8C C9C C10C O3C -125.4(6) . . . . ? C9C C10C C11C C12C -68.4(7) . . . . ? C10C C11C C12C C13C -179.4(5) . . . . ? C10C C11C C12C O4C -1.1(8) . . . . ? C11C C12C C13C C14C -179.6(4) . . . . ? C12C C13C C14C C15C -85.6(5) . . . . ? C12C C13C C14C C19C 98.7(5) . . . . ? C13C C14C C15C C16C -171.8(4) . . . . ? C13C C14C C15C Cl1C 8.0(5) . . . . ? C13C C14C C19C C18C 171.2(4) . . . . ? C13C C14C C19C C20C -11.7(7) . . . . ? C14C C15C C16C C17C -0.7(6) . . . . ? C14C C15C C16C O5C 177.8(4) . . . . ? C14C C19C C20C O1C 171.9(5) . . . . ? C14C C19C C20C O2C -11.1(7) . . . . ? C15C C14C C19C C18C -4.4(6) . . . . ? C15C C14C C19C C20C 172.7(4) . . . . ? C15C C16C C17C C18C -2.6(7) . . . . ? C16C C17C C18C C19C 2.2(8) . . . . ? C16C C17C C18C O6C -178.3(5) . . . . ? C17C C18C C19C C14C 1.4(7) . . . . ? C17C C18C C19C C20C -175.9(5) . . . . ? C18C C19C C20C O1C -10.9(8) . . . . ? C18C C19C C20C O2C 166.0(5) . . . . ? C19C C14C C15C C16C 4.2(6) . . . . ? C19C C14C C15C Cl1C -176.1(3) . . . . ? C19C C20C O2C C2C 173.8(7) . . . . ? C19C C20C O2C C2D -171.4(7) . . . . ? C20C O2C C2C C1C -152.9(8) . . . . ? C20C O2C C2C C3C 83.0(10) . . . . ? C20C O2C C2D C1D -80.1(11) . . . . ? C20C O2C C2D C3D 156.6(8) . . . . ? Cl1C C15C C16C C17C 179.6(4) . . . . ? Cl1C C15C C16C O5C -1.9(6) . . . . ? O1C C20C O2C C2C -9.2(10) . . . . ? O1C C20C O2C C2D 5.6(9) . . . . ? O2C C2C C3C C4C 67.3(10) . . . . ? O2C C2D C3D C4C -70.2(11) . . . . ? O3C C10C C11C C12C 168.0(4) . . . . ? O4C C12C C13C C14C 2.2(7) . . . . ? O5C C16C C17C C18C 178.8(5) . . . . ? O6C C18C C19C C14C -178.1(5) . . . . ? O6C C18C C19C C20C 4.6(7) . . . . ? C1C C2C C3C C4C -56.6(11) . . . . ? C3C C4C C5C C6C 161.2(8) . . . . ? C1D C2D C3D C4C 167.3(11) . . . . ? C3D C4C C5C C6C -150.3(8) . . . . ?