#------------------------------------------------------------------------------ #$Date: 2019-12-16 11:18:39 +0200 (Mon, 16 Dec 2019) $ #$Revision: 245201 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556581.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_1556581 loop_ _publ_author_name 'Dankert, F.' 'Reuter, K.' 'Donsbach, C.' 'Von Hanisch, C.' _publ_section_title ; Hybrid Disila-Crown Ethers as Hosts for Ammonium Cations: The O-Si-Si-O Linkage as an Acceptor for Hydrogen Bonding ; _journal_name_full Inorganics _journal_page_first 15 _journal_paper_doi 10.3390/inorganics6010015 _journal_volume 6 _journal_year 2018 _chemical_formula_moiety 'C18 H32 O6 Si2, H4 N, 1.28(C0.78 H1.56 Cl1.56), F6 P' _chemical_formula_sum 'C19 H38 Cl2 F6 N O6 P Si2' _chemical_formula_weight 648.55 _space_group_crystal_system monoclinic _space_group_IT_number 9 _space_group_name_Hall 'C -2yc' _space_group_name_H-M_alt 'C 1 c 1' _atom_sites_solution_hydrogens mixed _cell_angle_alpha 90 _cell_angle_beta 104.950(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.9582(7) _cell_length_b 12.6454(6) _cell_length_c 16.3325(8) _cell_measurement_reflns_used 9983 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.57 _cell_measurement_theta_min 2.30 _cell_volume 2984.8(2) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _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 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker D8 Quest' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_unetI/netI 0.0256 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 68974 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.785 _diffrn_reflns_theta_min 2.140 _exptl_absorpt_coefficient_mu 0.422 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6985 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.443 _exptl_crystal_description rod _exptl_crystal_F_000 1352 _exptl_crystal_size_max 0.522 _exptl_crystal_size_mid 0.106 _exptl_crystal_size_min 0.076 _refine_diff_density_max 0.512 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.065 _refine_ls_abs_structure_details ; Flack x determined using 2451 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.048(16) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 461 _refine_ls_number_reflns 6355 _refine_ls_number_restraints 543 _refine_ls_restrained_S_all 1.103 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0535 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+7.3653P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1267 _refine_ls_wR_factor_ref 0.1329 _reflns_Friedel_coverage 0.997 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.998 _reflns_number_gt 5664 _reflns_number_total 6355 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file compound4.cif _cod_data_source_block compound4 _cod_database_code 1556581 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 1.01(14) -0.01(14) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All C(H,H,H,H,H, H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances N1-H2 = N1-H3 = N1-H4 = N1-H1 0.91 with sigma of 0.02 Si2A-Si1A \\sim Si1-Si2 with sigma of 0.02 H1-H3 \\sim H1-H2 \\sim H1-H4 \\sim H3-H3 \\sim H3-H4 \\sim H2-H4 with sigma of 0.02 Cl13-C20 \\sim Cl14-C20 \\sim Cl1-C19 \\sim Cl2-C19 \\sim Cl1-C19A \\sim Cl2A-C19A with sigma of 0.02 Cl14-Cl13 \\sim Cl1-Cl2 \\sim Cl1-Cl2A with sigma of 0.02 Si2-C4 \\sim Si2-C3 \\sim Si2A-C3A \\sim Si2A-C4A \\sim Si1-C1 \\sim Si1-C2 \\sim Si1A-C1A \\sim Si1A-C2A with sigma of 0.02 C4-C3 \\sim C4A-C3A \\sim C2-C1 \\sim C2A-C1A with sigma of 0.02 4. Uiso/Uaniso restraints and constraints Cl2 \\sim Cl2A \\sim Cl1 \\sim C19 \\sim Cl13 \\sim Cl14 \\sim C20 \\sim C19A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 Si2 \\sim Si1 \\sim O6 \\sim C2 \\sim C4 \\sim C1 \\sim C3 \\sim Si1A \\sim Si2A \\sim O6A \\sim C3A \\sim C4A \\sim C1A \\sim C2A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(Cl14) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl2A) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(Cl13) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(C19A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(Si2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O6A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(Si2A) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(Si1) \\sim Ueq, Uanis(Si1A) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C2A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C4) = Uanis(C4A) 5. Rigid body (RIGU) restrains Cl2, Cl2A, Cl1, C19, Cl13, Cl14, C20, C19A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 Si2, Si1, O6, C2, C4, C1, C3, Si1A, Si2A, O6A, C3A, C4A, C1A, C2A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Sof(H5BC)=Sof(H5BD)=Sof(Cl13)=Sof(Cl14)=Sof(Si1A)=Sof(Si2A)=Sof(O6A)=Sof(C20)= Sof(H20A)=Sof(H20B)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(H4AA)= Sof(H4AB)=Sof(H4AC)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=1-FVAR(1) Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(H2AD)=Sof(H2AE)=Sof(H2AF)=0.5*(1-FVAR(2)) Sof(Cl2A)=Sof(C19A)=Sof(H19C)=Sof(H19D)=0.4*FVAR(2) Sof(Cl2)=Sof(C19)=Sof(H19A)=Sof(H19B)=0.6*FVAR(2) Sof(H5AA)=Sof(H5AB)=Sof(Cl1)=Sof(Si2)=Sof(Si1)=Sof(O6)=Sof(C2)=Sof(H2A)= Sof(H2B)=Sof(H2C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C1)=Sof(H1A)=Sof(H1B)= Sof(H1C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1) 7.a Secondary CH2 refined with riding coordinates: C15(H15A,H15B), C7(H7A,H7B), C18(H18A,H18B), C16(H16A,H16B), C6(H6A,H6B), C8(H8A,H8B), C17(H17A,H17B), C5(H5AA,H5AB), C5(H5BC,H5BD), C19(H19A,H19B), C19A(H19C,H19D), C20(H20A,H20B) 7.b Aromatic/amide H refined with riding coordinates: C12(H12), C13(H13), C11(H11), C10(H10) 7.c Disordered Me refined with riding coordinates: C2A(H2AA,H2AB,H2AC,H2AD,H2AE,H2AF) 7.d Idealised Me refined as rotating group: C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C3A(H3AA, H3AB,H3AC), C4A(H4AA,H4AB,H4AC), C1A(H1AA,H1AB,H1AC) ; _shelx_res_file ; compound4.res created by SHELXL-2014/7 TITL compound4.res in Cc REM Old TITL compound4 in Cc REM SHELXT solution in Cc REM R1 0.190, Rweak 0.057, Alpha 0.006, Orientation as input REM Flack x = 0.245 ( 0.013 ) from Parsons' quotients REM Formula found by SHELXT: C25 N2 O7 Si2 Cl2 CELL 0.71073 14.9582 12.6454 16.3325 90 104.95 90 ZERR 4 0.0007 0.0006 0.0008 0 0.002 0 LATT -7 SYMM +X,-Y,0.5+Z SFAC C H Cl F N O P Si UNIT 76 152 8 24 4 24 4 8 DFIX 0.91 N1 H2 N1 H3 N1 H4 N1 H1 SADI Si2A Si1A Si1 Si2 SADI H1 H3 H1 H2 H1 H4 H3 H3 H3 H4 H2 H4 SADI Cl13 C20 Cl14 C20 Cl1 C19 Cl2 C19 Cl1 C19A Cl2A C19A SADI Cl14 Cl13 Cl1 Cl2 Cl1 Cl2A SADI Si2 C4 Si2 C3 Si2A C3A Si2A C4A Si1 C1 Si1 C2 Si1A C1A Si1A C2A SADI C4 C3 C4A C3A C2 C1 C2A C1A SIMU Cl2 Cl2A Cl1 C19 Cl13 Cl14 C20 C19A SIMU Si2 > C4 C1 C3 Si1A Si2A O6A C3A > C2A RIGU Cl2 Cl2A Cl1 C19 Cl13 Cl14 C20 C19A RIGU Si2 > C4 C1 C3 Si1A Si2A O6A C3A > C2A ISOR Cl14 Cl2 Cl2A C19 C20 Cl13 Cl1 C19A ISOR Si2 C3 O6 O6A C3A Si2A C4 C4A C1 Si1 Si1A C1A C2 C2A EADP C4 C4A L.S. 10 PLAN 50 TEMP -173(2) FREE C19 H19C FREE C19 H19D FREE Cl2 Cl2A FREE Cl2 C19A FREE Cl2 H19C FREE C19A C19 FREE C19A H19A FREE C19A H19B FREE Cl2A C19 list 4 fmap 2 acta TWIN -1 0 0 0 1 0 0 0 -1 2 REM REM REM WGHT 0.061500 7.365300 BASF -0.00670 FVAR 0.39710 0.77936 O3 6 0.702713 0.375693 0.477915 11.00000 0.01808 0.02351 = 0.02588 -0.00523 0.00225 -0.00402 O4 6 0.597033 0.263625 0.357973 11.00000 0.02549 0.02242 = 0.02510 -0.00444 0.00743 -0.00517 O5 6 0.402238 0.245861 0.333441 11.00000 0.02343 0.02648 = 0.02848 0.00039 -0.00009 -0.00286 O2 6 0.641107 0.473413 0.611577 11.00000 0.02169 0.02348 = 0.02785 -0.00236 0.00231 0.00504 O1 6 0.450700 0.485818 0.612341 11.00000 0.02409 0.03307 = 0.04636 -0.01402 -0.00082 0.00989 N1 5 0.509404 0.344932 0.491171 11.00000 0.02447 0.02631 = 0.02752 -0.00285 0.00210 -0.00299 H1 2 0.515247 0.283756 0.521441 11.00000 0.02819 H3 2 0.530979 0.396360 0.528239 11.00000 0.09864 H2 2 0.531592 0.332118 0.447068 11.00000 0.07072 H4 2 0.448093 0.354327 0.471851 11.00000 0.05167 C14 1 0.733658 0.363121 0.407360 11.00000 0.02366 0.01551 = 0.02635 0.00294 0.00440 0.00163 C9 1 0.677367 0.300363 0.342009 11.00000 0.02495 0.01814 = 0.02571 0.00378 0.00626 0.00031 C15 1 0.763309 0.431899 0.546875 11.00000 0.02123 0.02475 = 0.03019 -0.00588 0.00244 -0.00400 AFIX 23 H15A 2 0.765208 0.507692 0.532232 11.00000 -1.20000 H15B 2 0.826824 0.403047 0.557815 11.00000 -1.20000 AFIX 0 C12 1 0.841430 0.386285 0.321712 11.00000 0.03262 0.02168 = 0.04450 0.00443 0.01854 -0.00184 AFIX 43 H12 2 0.897227 0.415702 0.314231 11.00000 -1.20000 AFIX 0 C7 1 0.459464 0.158971 0.325352 11.00000 0.02775 0.01973 = 0.02258 -0.00141 -0.00091 -0.00554 AFIX 23 H7A 2 0.423188 0.106753 0.285010 11.00000 -1.20000 H7B 2 0.482543 0.123818 0.380968 11.00000 -1.20000 AFIX 0 C13 1 0.814938 0.406118 0.395690 11.00000 0.02760 0.02074 = 0.03998 0.00230 0.01049 -0.00150 AFIX 43 H13 2 0.852589 0.449322 0.438562 11.00000 -1.20000 AFIX 0 C18 1 0.524129 0.535809 0.672441 11.00000 0.02889 0.03508 = 0.04431 -0.01648 0.00382 0.00892 AFIX 23 H18A 2 0.506477 0.545597 0.726346 11.00000 -1.20000 H18B 2 0.535796 0.606448 0.651189 11.00000 -1.20000 AFIX 0 C16 1 0.727973 0.419814 0.624386 11.00000 0.02076 0.02108 = 0.02886 -0.00262 -0.00061 0.00325 AFIX 23 H16A 2 0.720039 0.343884 0.635505 11.00000 -1.20000 H16B 2 0.773162 0.450070 0.674134 11.00000 -1.20000 AFIX 0 C11 1 0.787446 0.324547 0.259615 11.00000 0.04065 0.02418 = 0.03962 0.00083 0.02100 0.00004 AFIX 43 H11 2 0.806463 0.310645 0.209479 11.00000 -1.20000 AFIX 0 C10 1 0.704651 0.281671 0.269033 11.00000 0.03329 0.02345 = 0.03215 -0.00128 0.01060 -0.00097 AFIX 43 H10 2 0.667217 0.239667 0.225139 11.00000 -1.20000 AFIX 0 C6 1 0.320095 0.211146 0.354243 11.00000 0.02541 0.03777 = 0.04027 -0.00835 0.00767 -0.00975 AFIX 23 H6A 2 0.336251 0.170347 0.407780 11.00000 -1.20000 H6B 2 0.283908 0.164780 0.308812 11.00000 -1.20000 AFIX 0 C8 1 0.539578 0.197368 0.294046 11.00000 0.02858 0.02607 = 0.02043 -0.00235 0.00207 -0.00510 AFIX 23 H8A 2 0.575828 0.136414 0.282163 11.00000 -1.20000 H8B 2 0.516722 0.237946 0.240916 11.00000 -1.20000 AFIX 0 C17 1 0.611164 0.469963 0.688084 11.00000 0.02642 0.02855 = 0.03262 -0.01050 0.00296 0.00341 AFIX 23 H17A 2 0.659486 0.499310 0.735966 11.00000 -1.20000 H17B 2 0.598321 0.396171 0.701806 11.00000 -1.20000 AFIX 0 C5 1 0.263924 0.306558 0.363878 11.00000 0.02421 0.04374 = 0.04553 -0.00756 -0.00150 -0.00260 PART 1 AFIX 23 H5AA 2 0.258382 0.354649 0.314989 21.00000 -1.20000 H5AB 2 0.200952 0.284698 0.365818 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H5BC 2 0.240685 0.339489 0.307384 -21.00000 -1.20000 H5BD 2 0.209396 0.282368 0.382545 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 CL2 3 0.418186 0.627142 0.428586 20.60000 0.10867 0.15281 = 0.16324 0.10495 0.09650 0.07376 CL2A 3 0.508522 0.758105 0.498467 20.40000 0.08202 0.08020 = 0.11693 -0.00394 -0.03172 0.00342 CL1 3 0.581987 0.583510 0.384969 21.00000 0.07587 0.04451 = 0.05854 0.00027 0.00860 0.00919 SI2 8 0.244384 0.413071 0.500897 21.00000 0.02193 0.03447 = 0.04093 0.00628 -0.00068 0.00467 SI1 8 0.339671 0.508186 0.612824 21.00000 0.02204 0.01952 = 0.07304 -0.01102 0.00958 0.00244 O6 6 0.309996 0.360592 0.442116 21.00000 0.02696 0.02522 = 0.04811 -0.00306 -0.00590 0.00306 C2 1 0.317205 0.654567 0.603922 21.00000 0.03911 0.01731 = 0.11416 -0.00506 0.00275 0.01249 AFIX 137 H2A 2 0.254286 0.668989 0.608450 21.00000 -1.50000 H2B 2 0.323781 0.679814 0.549045 21.00000 -1.50000 H2C 2 0.361837 0.691194 0.649631 21.00000 -1.50000 AFIX 0 C4 1 0.156127 0.497288 0.431804 21.00000 0.06568 0.08503 = 0.05926 -0.01669 -0.01945 0.05366 AFIX 137 H4A 2 0.185911 0.545512 0.399961 21.00000 -1.50000 H4B 2 0.124098 0.538410 0.466468 21.00000 -1.50000 H4C 2 0.111338 0.452822 0.392163 21.00000 -1.50000 AFIX 0 C19 1 0.489676 0.670207 0.364671 20.60000 0.05517 0.04948 = 0.05219 0.01929 0.01317 0.00814 AFIX 23 H19A 2 0.455806 0.668105 0.304006 20.60000 -1.20000 H19B 2 0.511268 0.743416 0.379589 20.60000 -1.20000 AFIX 0 C19A 1 0.500688 0.684221 0.400648 20.40000 0.12901 0.09339 = 0.06747 0.00409 -0.00246 0.04220 AFIX 23 H19C 2 0.439184 0.649753 0.386617 20.40000 -1.20000 H19D 2 0.498477 0.737993 0.356113 20.40000 -1.20000 AFIX 0 C1 1 0.317513 0.467699 0.715646 21.00000 0.05462 0.08248 = 0.07388 -0.03331 0.01473 -0.02864 AFIX 137 H1A 2 0.345465 0.398291 0.732288 21.00000 -1.50000 H1B 2 0.250650 0.463665 0.709347 21.00000 -1.50000 H1C 2 0.344783 0.519870 0.759325 21.00000 -1.50000 AFIX 0 C3 1 0.182250 0.306708 0.542563 21.00000 0.11773 0.10765 = 0.03931 -0.01222 0.00691 -0.06681 AFIX 137 H3A 2 0.224310 0.247123 0.561829 21.00000 -1.50000 H3B 2 0.129127 0.282866 0.497608 21.00000 -1.50000 H3C 2 0.160590 0.334114 0.590197 21.00000 -1.50000 AFIX 0 PART 0 PART 2 CL13 3 0.553827 0.603452 0.411230 -21.00000 0.11713 0.15414 = 0.09509 -0.00844 0.04933 0.04963 CL14 3 0.373226 0.545410 0.314006 -21.00000 0.06414 0.06149 = 0.23613 0.04412 0.05768 -0.00434 SI1A 8 0.370266 0.563912 0.554384 -21.00000 0.03820 0.02914 = 0.06579 -0.01586 -0.02591 0.02130 SI2A 8 0.265235 0.437542 0.486730 -21.00000 0.03142 0.03051 = 0.02412 -0.00010 -0.00014 0.01008 O6A 6 0.307657 0.381866 0.418425 -21.00000 0.03446 0.02467 = 0.01921 0.01233 -0.00225 0.01175 C20 1 0.466227 0.635845 0.316222 -21.00000 0.06582 0.03994 = 0.09448 0.00586 0.04402 -0.00140 AFIX 23 H20A 2 0.445318 0.709877 0.318093 -21.00000 -1.20000 H20B 2 0.490169 0.626618 0.265537 -21.00000 -1.20000 AFIX 0 C3A 1 0.244789 0.352706 0.570713 -21.00000 0.05363 0.04804 = 0.03698 -0.00227 0.00419 0.00945 AFIX 137 H3AA 2 0.247554 0.278392 0.554519 -21.00000 -1.50000 H3AB 2 0.183570 0.367999 0.579179 -21.00000 -1.50000 H3AC 2 0.292282 0.366251 0.623459 -21.00000 -1.50000 AFIX 0 C4A 1 0.159430 0.517483 0.444517 -21.00000 0.06568 0.08503 = 0.05926 -0.01669 -0.01945 0.05366 AFIX 137 H4AA 2 0.133361 0.500479 0.384553 -21.00000 -1.50000 H4AB 2 0.175167 0.592819 0.450299 -21.00000 -1.50000 H4AC 2 0.113849 0.501396 0.476392 -21.00000 -1.50000 AFIX 0 C1A 1 0.312723 0.616629 0.635033 -21.00000 0.04543 0.08891 = 0.07705 -0.05133 -0.02980 0.00827 AFIX 137 H1AA 2 0.257004 0.655997 0.606360 -21.00000 -1.50000 H1AB 2 0.355453 0.663787 0.674072 -21.00000 -1.50000 H1AC 2 0.295591 0.557698 0.666884 -21.00000 -1.50000 AFIX 0 C2A 1 0.405047 0.681653 0.502528 -21.00000 0.11172 0.08490 = 0.13222 0.00494 0.00895 -0.00744 AFIX 123 H2AA 2 0.349647 0.719308 0.470801 -20.50000 -1.20000 H2AB 2 0.442397 0.728664 0.545753 -20.50000 -1.20000 H2AC 2 0.441495 0.659272 0.463601 -20.50000 -1.20000 H2AD 2 0.472712 0.685522 0.515969 -20.50000 -1.20000 H2AE 2 0.379963 0.676166 0.441017 -20.50000 -1.20000 H2AF 2 0.380864 0.745557 0.523168 -20.50000 -1.20000 AFIX 0 PART 0 P1 7 0.513520 0.103127 0.642779 11.00000 0.02195 0.03927 = 0.02921 0.01069 0.00631 -0.00184 F5 4 0.436976 0.033436 0.667804 11.00000 0.05649 0.07809 = 0.05273 -0.00319 0.02292 -0.03611 F3 4 0.586938 0.178016 0.616492 11.00000 0.04674 0.08354 = 0.13398 0.04860 0.03845 -0.01009 F6 4 0.586699 0.015985 0.664485 11.00000 0.13008 0.09680 = 0.19288 0.09469 0.11565 0.07959 F1 4 0.478640 0.072801 0.548698 11.00000 0.11975 0.29397 = 0.03155 -0.03282 0.02358 -0.08880 F2 4 0.441090 0.194862 0.621714 11.00000 0.10270 0.13395 = 0.26863 0.13246 0.12180 0.08001 F4 4 0.543372 0.140316 0.736317 11.00000 0.10615 0.21865 = 0.06601 -0.06677 0.02307 -0.08710 HKLF 4 REM compound4.res in Cc REM R1 = 0.0535 for 5664 Fo > 4sig(Fo) and 0.0635 for all 6355 data REM 461 parameters refined using 543 restraints END WGHT 0.0615 7.3653 REM Highest difference peak 0.512, deepest hole -0.436, 1-sigma level 0.065 Q1 1 0.4867 0.2106 0.6599 11.00000 0.05 0.51 Q2 1 0.5746 0.0835 0.7281 11.00000 0.05 0.45 Q3 1 0.4714 -0.0216 0.6417 11.00000 0.05 0.42 Q4 1 0.5157 -0.0264 0.6062 11.00000 0.05 0.39 Q5 1 0.3933 0.5614 0.3705 11.00000 0.05 0.37 Q6 1 0.5011 0.0221 0.5716 11.00000 0.05 0.37 Q7 1 0.6051 0.0251 0.6845 11.00000 0.05 0.33 Q8 1 0.2368 0.2672 0.5322 11.00000 0.05 0.31 Q9 1 0.4379 0.1586 0.5913 11.00000 0.05 0.30 Q10 1 0.4251 0.1743 0.5989 11.00000 0.05 0.30 Q11 1 0.3245 0.5144 0.5654 11.00000 0.05 0.30 Q12 1 0.5431 0.2236 0.6516 11.00000 0.05 0.29 Q13 1 0.3197 0.6431 0.5499 11.00000 0.05 0.29 Q14 1 0.4461 0.1189 0.5619 11.00000 0.05 0.28 Q15 1 0.5214 0.1750 0.6986 11.00000 0.05 0.28 Q16 1 0.4984 0.7725 0.5245 11.00000 0.05 0.28 Q17 1 0.3897 0.5320 0.2965 11.00000 0.05 0.25 Q18 1 0.4659 0.2910 0.6326 11.00000 0.05 0.23 Q19 1 0.5417 0.1601 0.7521 11.00000 0.05 0.23 Q20 1 0.5138 0.1251 0.5549 11.00000 0.05 0.22 Q21 1 0.6252 0.0438 0.6541 11.00000 0.05 0.22 Q22 1 0.6740 0.4188 0.4765 11.00000 0.05 0.21 Q23 1 0.6822 0.5231 0.7764 11.00000 0.05 0.21 Q24 1 0.6178 0.1913 0.6746 11.00000 0.05 0.20 Q25 1 0.2690 0.5528 0.3492 11.00000 0.05 0.20 Q26 1 0.4446 0.6450 0.4425 11.00000 0.05 0.20 Q27 1 0.3320 0.4521 0.7329 11.00000 0.05 0.20 Q28 1 0.5013 0.4395 0.5898 11.00000 0.05 0.19 Q29 1 0.5903 0.2571 0.7858 11.00000 0.05 0.19 Q30 1 0.4443 -0.0953 0.6626 11.00000 0.05 0.19 Q31 1 0.2069 0.5919 0.4886 11.00000 0.05 0.19 Q32 1 0.8453 0.3064 0.5968 11.00000 0.05 0.19 Q33 1 0.7715 0.3181 0.1481 11.00000 0.05 0.19 Q34 1 0.4396 0.0977 0.7225 11.00000 0.05 0.19 Q35 1 0.2479 0.5833 0.3960 11.00000 0.05 0.18 Q36 1 0.1635 0.2615 0.4988 11.00000 0.05 0.18 Q37 1 0.6066 0.1009 0.5900 11.00000 0.05 0.18 Q38 1 0.3039 0.5144 0.6825 11.00000 0.05 0.18 Q39 1 0.2090 0.5373 0.4277 11.00000 0.05 0.18 Q40 1 0.2455 0.4806 0.6906 11.00000 0.05 0.18 Q41 1 0.3186 0.3374 0.4666 11.00000 0.05 0.18 Q42 1 0.4209 0.0340 0.3108 11.00000 0.05 0.18 Q43 1 0.7260 0.4182 0.4915 11.00000 0.05 0.18 Q44 1 0.2839 0.6850 0.3410 11.00000 0.05 0.18 Q45 1 0.4421 0.5630 0.4613 11.00000 0.05 0.17 Q46 1 0.6226 0.1337 0.6581 11.00000 0.05 0.17 Q47 1 0.2005 0.6379 0.5006 11.00000 0.05 0.17 Q48 1 0.6987 0.4033 0.4416 11.00000 0.05 0.17 Q49 1 0.5116 0.8577 0.5096 11.00000 0.05 0.17 Q50 1 0.2891 0.6562 0.4951 11.00000 0.05 0.17 ; _shelx_res_checksum 4525 _shelx_hkl_file ; 2 0 0 505.95 11.00 2 0 0 495.75 11.30 2 0 0 491.95 12.10 2 0 0 491.55 11.60 -2 0 0 487.05 11.50 -2 0 0 481.95 11.20 -2 0 0 486.15 12.00 -2 0 0 478.75 11.40 -2 0 0 523.45 11.20 2 0 0 463.55 11.50 2 0 0 500.45 11.50 2 0 0 475.25 11.30 -4 0 0 2929.61 59.09 -4 0 0 2803.92 58.79 4 0 0 2849.91 58.79 4 0 0 2860.01 60.19 -4 0 0 2983.00 60.49 -4 0 0 2494.75 60.19 -4 0 0 2925.41 58.19 -4 0 0 3007.30 58.19 4 0 0 2473.85 60.39 4 0 0 2938.91 59.09 4 0 0 2925.11 58.29 6 0 0 89.89 6.60 -6 0 0 98.79 6.10 -6 0 0 96.39 6.00 -6 0 0 99.29 6.20 6 0 0 95.49 7.20 -6 0 0 94.29 7.90 -6 0 0 95.39 7.00 6 0 0 105.99 7.80 6 0 0 90.09 7.10 6 0 0 100.49 5.50 6 0 0 90.19 6.60 -6 0 0 94.09 5.70 8 0 0 369.26 15.80 8 0 0 391.86 16.40 8 0 0 378.06 15.10 8 0 0 377.76 14.40 -8 0 0 388.26 13.60 -8 0 0 385.96 14.80 -8 0 0 380.76 12.80 -8 0 0 331.37 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655.43 17.50 -5 5 0 611.34 21.20 5 5 0 619.94 21.10 5 5 0 586.14 18.00 7 -5 0 1334.47 33.90 7 -5 0 1403.96 36.80 -7 -5 0 1400.76 31.60 7 -5 0 1362.86 32.10 7 -5 0 1364.76 32.10 7 -5 0 1463.85 39.10 7 -5 0 1371.96 34.10 -7 5 0 1367.66 31.90 7 5 0 1397.96 39.20 7 5 0 1339.07 37.20 -7 5 0 1403.26 38.30 -7 5 0 1335.67 31.90 -7 5 0 1370.96 33.10 7 5 0 1420.66 35.20 -7 5 0 1409.26 38.40 -7 5 0 1401.16 33.90 -7 5 0 1370.16 36.80 -7 5 0 1386.66 34.60 7 5 0 1410.06 34.90 7 5 0 1422.66 34.70 -7 5 0 1389.26 35.60 7 5 0 1418.06 36.30 7 5 0 1397.36 36.00 7 5 0 1456.15 33.50 -7 5 0 1392.46 33.20 9 -5 0 98.19 7.50 9 -5 0 58.59 7.30 -9 -5 0 85.89 5.00 9 -5 0 134.99 17.30 -9 -5 0 87.09 6.50 9 -5 0 92.29 8.40 9 -5 0 111.19 12.80 9 -5 0 107.19 12.40 9 -5 0 87.89 7.20 9 5 0 99.99 12.60 -9 5 0 89.69 10.20 9 5 0 70.49 9.20 -9 5 0 82.89 9.30 9 5 0 91.19 6.30 9 5 0 81.99 8.10 -9 5 0 93.39 8.30 -9 5 0 91.99 11.70 9 5 0 92.99 10.10 -9 5 0 91.59 7.60 -9 5 0 82.49 7.40 -9 5 0 93.99 11.20 -9 5 0 82.89 7.20 9 5 0 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6 6 0 1138.59 32.60 -6 6 0 1161.48 32.70 6 6 0 1146.59 30.40 6 6 0 1187.98 30.00 8 -6 0 522.45 17.90 8 -6 0 485.85 20.10 8 -6 0 491.75 17.40 8 -6 0 526.05 15.80 8 -6 0 514.75 16.00 8 -6 0 532.75 23.80 8 6 0 523.45 21.70 -8 6 0 543.35 17.00 8 6 0 531.65 20.60 -8 6 0 507.05 17.20 -8 6 0 542.05 17.70 -8 6 0 539.35 22.40 8 6 0 529.15 23.60 8 6 0 506.65 19.40 8 6 0 530.75 18.70 -8 6 0 522.35 20.30 -8 6 0 548.95 21.00 8 6 0 540.95 17.90 -8 6 0 524.95 17.70 -8 6 0 506.35 16.50 -8 6 0 522.75 18.70 -8 6 0 564.44 23.30 8 6 0 508.35 20.30 8 6 0 518.05 19.20 10 -6 0 233.18 22.00 10 -6 0 238.88 17.40 10 -6 0 231.68 12.70 -10 -6 0 223.38 10.00 10 -6 0 204.18 10.30 10 -6 0 215.48 11.00 10 -6 0 216.38 12.30 10 -6 0 247.58 25.70 10 6 0 204.68 17.00 -10 6 0 220.08 11.80 -10 6 0 206.38 15.60 10 6 0 213.38 14.50 -10 6 0 196.68 11.20 10 6 0 199.38 16.00 10 6 0 219.38 15.10 -10 6 0 186.58 16.20 -10 6 0 202.48 11.40 -10 6 0 217.28 17.40 10 6 0 208.18 12.50 10 6 0 222.48 21.40 -10 6 0 241.38 20.60 -10 6 0 213.48 11.70 -10 6 0 212.08 11.70 -10 6 0 195.68 15.20 10 6 0 205.48 9.40 10 6 0 232.38 15.40 10 6 0 231.98 15.10 12 -6 0 121.89 25.10 -12 -6 0 84.69 8.30 12 -6 0 101.19 15.40 12 -6 0 118.59 19.60 12 -6 0 88.79 9.90 12 -6 0 55.59 8.60 12 -6 0 85.39 9.00 12 -6 0 87.79 10.10 12 6 0 84.89 11.60 12 6 0 94.09 9.90 -12 6 0 87.79 8.40 -12 6 0 86.09 9.00 -12 6 0 93.89 9.60 12 6 0 72.29 11.70 12 6 0 93.49 12.90 -12 6 0 101.99 15.90 -12 6 0 86.59 10.40 -12 6 0 82.29 9.20 12 6 0 70.79 7.90 -12 6 0 72.19 17.60 -12 6 0 72.69 12.00 12 6 0 109.79 23.60 12 6 0 96.59 14.00 -12 6 0 76.59 12.00 12 6 0 68.89 14.20 12 6 0 80.09 9.40 12 6 0 69.29 10.50 14 -6 0 52.49 10.20 14 -6 0 43.20 7.30 14 -6 0 28.80 9.00 14 -6 0 30.90 8.60 14 6 0 39.80 9.90 14 6 0 33.10 12.60 14 6 0 47.40 6.40 -14 6 0 40.00 12.60 -14 6 0 46.80 16.60 14 6 0 48.20 13.80 14 6 0 37.40 9.10 14 6 0 37.30 11.20 14 6 0 32.30 10.40 -14 6 0 40.40 8.10 14 6 0 51.99 14.30 16 -6 0 32.70 11.50 16 -6 0 3.20 10.80 16 -6 0 12.20 9.50 16 -6 0 29.80 8.90 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16.90 3 7 0 477.85 13.50 3 7 0 487.85 13.70 -3 7 0 480.65 13.30 -3 7 0 477.85 17.90 3 7 0 471.35 17.30 3 7 0 468.25 12.90 -3 7 0 473.45 14.90 -3 7 0 495.15 16.10 -3 7 0 497.55 17.40 -5 -7 0 761.62 25.40 5 -7 0 792.22 21.80 5 -7 0 780.82 22.00 5 -7 0 777.82 20.40 5 -7 0 800.62 20.60 5 -7 0 823.32 25.90 5 -7 0 804.92 27.40 -5 7 0 793.22 24.60 -5 7 0 789.92 22.40 -5 7 0 770.22 24.80 -5 7 0 780.42 24.10 5 7 0 780.32 18.40 -5 7 0 802.92 20.50 -5 7 0 769.22 26.30 -5 7 0 771.92 24.10 -5 7 0 764.12 22.80 5 7 0 774.62 20.70 5 7 0 756.52 25.40 5 7 0 786.12 23.60 5 7 0 784.42 21.10 5 7 0 754.82 25.30 -5 7 0 773.52 20.70 5 7 0 737.13 25.50 7 -7 0 385.66 13.20 7 -7 0 388.66 21.10 7 -7 0 387.16 12.60 7 -7 0 361.56 18.90 7 -7 0 393.16 13.90 -7 7 0 381.56 15.20 -7 7 0 406.86 16.40 7 7 0 366.36 15.60 -7 7 0 415.96 17.70 -7 7 0 381.96 16.30 -7 7 0 428.16 19.80 7 7 0 348.27 18.70 -7 7 0 389.76 19.50 7 7 0 388.36 15.60 7 7 0 389.06 20.70 -7 7 0 396.86 15.10 -7 7 0 404.76 14.10 7 7 0 391.86 18.20 7 7 0 376.46 14.70 7 7 0 393.46 15.80 7 7 0 377.46 18.20 -7 7 0 379.56 17.80 9 -7 0 495.75 16.50 9 -7 0 487.85 25.00 9 -7 0 517.35 22.20 9 -7 0 499.55 26.40 9 -7 0 482.75 18.40 9 -7 0 493.15 17.70 9 -7 0 515.85 16.10 9 7 0 493.25 18.80 -9 7 0 510.95 20.40 -9 7 0 515.95 21.90 9 7 0 518.45 21.10 9 7 0 480.95 22.80 -9 7 0 507.75 17.80 -9 7 0 498.25 23.80 -9 7 0 506.05 18.10 9 7 0 499.75 20.70 9 7 0 466.85 21.60 9 7 0 513.55 19.50 9 7 0 514.05 19.40 -9 7 0 501.15 18.80 -9 7 0 491.35 25.00 -9 7 0 512.25 22.60 -9 7 0 516.75 19.30 9 7 0 482.75 22.00 9 7 0 496.55 26.20 -9 7 0 500.65 17.50 11 -7 0 63.89 8.00 11 -7 0 68.89 12.90 11 -7 0 70.89 17.80 11 -7 0 66.89 16.80 11 -7 0 73.49 8.30 11 -7 0 77.59 9.00 11 -7 0 84.69 9.80 -11 7 0 84.39 9.60 -11 7 0 75.89 12.30 11 7 0 71.59 11.40 -11 7 0 71.79 13.30 -11 7 0 74.19 9.00 -11 7 0 69.59 8.50 11 7 0 53.79 10.30 -11 7 0 76.99 10.70 -11 7 0 69.19 8.50 11 7 0 73.49 12.70 -11 7 0 78.89 13.20 11 7 0 69.79 12.60 -11 7 0 71.99 16.40 11 7 0 55.39 16.90 11 7 0 74.09 11.80 -11 7 0 85.89 10.70 11 7 0 67.79 9.30 13 -7 0 2.50 15.50 13 -7 0 0.80 19.50 13 -7 0 20.30 6.50 13 -7 0 11.60 6.00 13 -7 0 13.30 7.80 13 -7 0 12.20 8.00 13 7 0 7.60 10.30 13 7 0 14.10 11.90 -13 7 0 48.00 13.10 -13 7 0 6.30 6.10 13 7 0 15.10 8.50 -13 7 0 10.90 6.80 13 7 0 23.50 11.20 -13 7 0 10.30 6.50 -13 7 0 -4.50 15.00 -13 7 0 42.10 12.00 -13 7 0 23.80 7.50 -13 7 0 12.60 6.00 13 7 0 30.20 12.20 13 7 0 11.70 9.40 15 -7 0 -2.50 10.20 15 -7 0 -2.50 6.40 15 -7 0 0.90 7.90 15 -7 0 -5.50 9.30 -15 7 0 4.60 12.20 15 7 0 15.40 14.60 15 7 0 0.50 14.30 15 7 0 -5.90 10.60 15 7 0 17.70 12.40 -15 7 0 1.20 6.80 15 7 0 -3.80 5.40 15 7 0 -1.50 21.20 -15 7 0 -11.40 14.00 15 7 0 7.50 16.80 15 7 0 9.20 11.40 0 -8 0 198.18 8.80 0 -8 0 184.38 10.80 0 -8 0 186.08 9.80 0 -8 0 207.18 13.70 0 -8 0 181.78 7.70 0 8 0 195.18 7.70 0 8 0 202.08 12.70 0 8 0 191.38 9.90 0 8 0 177.28 8.60 0 8 0 194.18 13.00 0 8 0 182.98 12.30 0 8 0 192.98 11.40 0 8 0 196.98 8.60 2 -8 0 124.69 7.20 -2 -8 0 114.99 8.20 2 -8 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267.97 16.80 6 -8 0 279.27 11.50 6 -8 0 244.08 19.00 6 -8 0 273.07 12.40 6 -8 0 287.17 13.50 6 -8 0 288.37 11.20 -6 -8 0 264.67 16.40 -6 8 0 279.77 15.10 6 8 0 254.17 16.50 -6 8 0 271.97 15.20 6 8 0 266.47 14.40 -6 8 0 279.67 12.40 6 8 0 316.07 18.10 6 8 0 274.57 14.50 -6 8 0 295.37 18.00 6 8 0 279.37 14.40 -6 8 0 296.87 14.90 -6 8 0 283.47 13.90 6 8 0 301.57 15.80 6 8 0 291.67 9.30 -6 8 0 299.37 16.90 -6 8 0 290.27 11.20 6 8 0 293.37 12.00 6 8 0 311.67 17.60 8 -8 0 138.09 16.40 8 -8 0 159.98 8.70 8 -8 0 134.49 9.20 8 -8 0 168.78 13.40 8 -8 0 144.69 14.10 8 -8 0 128.39 9.00 8 -8 0 132.29 15.80 -8 8 0 150.78 12.80 8 8 0 133.59 13.90 8 8 0 143.49 15.30 -8 8 0 152.48 12.40 8 8 0 139.69 12.00 8 8 0 117.49 10.90 -8 8 0 138.89 12.50 8 8 0 163.48 12.70 8 8 0 163.68 14.10 -8 8 0 121.99 12.20 -8 8 0 122.59 14.10 -8 8 0 116.89 13.40 -8 8 0 156.48 9.60 8 8 0 151.18 12.70 -8 8 0 140.49 11.30 8 8 0 126.99 14.30 8 8 0 156.78 18.80 -8 8 0 104.69 13.50 -8 8 0 151.28 14.90 10 -8 0 269.07 13.70 10 -8 0 260.87 24.20 10 -8 0 239.58 28.00 10 -8 0 272.47 15.00 10 -8 0 298.17 20.10 10 -8 0 257.07 12.80 10 -8 0 265.57 12.10 -10 8 0 289.77 20.50 -10 8 0 256.57 15.80 -10 8 0 284.97 21.00 10 8 0 281.67 18.70 10 8 0 267.27 16.10 -10 8 0 301.67 16.70 10 8 0 278.67 19.00 10 8 0 276.97 19.50 10 8 0 262.17 19.00 10 8 0 221.78 16.20 -10 8 0 262.57 15.90 -10 8 0 252.67 18.50 10 8 0 270.97 15.70 10 8 0 242.18 19.20 -10 8 0 289.97 26.10 -10 8 0 258.57 12.90 10 8 0 251.07 25.90 -10 8 0 261.07 18.10 -10 8 0 287.27 15.50 12 -8 0 30.50 7.10 12 -8 0 21.10 7.10 12 -8 0 23.90 8.30 12 -8 0 21.70 14.20 12 -8 0 42.00 15.10 12 -8 0 31.00 5.80 12 8 0 25.90 11.00 -12 8 0 19.90 15.00 -12 8 0 23.70 8.90 12 8 0 -10.10 13.30 -12 8 0 28.10 14.60 -12 8 0 24.80 10.80 12 8 0 24.10 11.40 12 8 0 22.80 9.90 -12 8 0 42.80 7.50 12 8 0 34.50 12.40 -12 8 0 24.40 8.50 12 8 0 14.30 8.10 -12 8 0 12.50 11.20 12 8 0 46.50 12.60 -12 8 0 32.20 9.40 -12 8 0 14.00 8.00 14 -8 0 0.50 6.30 14 -8 0 5.50 10.00 14 -8 0 -0.40 8.00 14 -8 0 5.30 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218.18 15.10 3 9 0 239.78 13.50 -3 9 0 213.48 15.30 3 9 0 214.68 14.10 3 9 0 234.08 9.90 -3 9 0 217.48 9.60 -3 9 0 208.48 14.80 -3 9 0 216.98 8.10 -3 9 0 220.58 22.40 3 9 0 203.68 13.50 3 9 0 194.98 9.50 -3 9 0 228.28 13.40 3 9 0 229.38 9.80 -5 -9 0 190.98 8.30 -5 -9 0 199.78 14.80 5 -9 0 201.18 15.30 5 -9 0 204.58 9.30 5 -9 0 200.78 10.20 5 -9 0 198.68 10.90 -5 -9 0 193.08 8.00 5 -9 0 215.58 20.50 5 -9 0 201.98 10.80 -5 9 0 197.98 13.50 -5 9 0 200.08 13.60 -5 9 0 211.48 15.00 5 9 0 203.68 10.70 -5 9 0 194.18 12.80 5 9 0 204.58 13.80 5 9 0 190.78 15.30 -5 9 0 200.88 14.80 -5 9 0 194.98 10.30 5 9 0 200.98 6.60 5 9 0 194.28 8.70 5 9 0 195.88 16.10 -5 9 0 203.08 8.70 -5 9 0 210.08 17.40 5 9 0 178.18 13.50 -5 9 0 197.08 15.90 5 9 0 205.28 10.00 5 9 0 172.58 14.90 7 -9 0 259.97 23.20 7 -9 0 268.87 12.70 7 -9 0 262.37 24.00 7 -9 0 286.07 19.50 7 -9 0 299.37 12.20 7 -9 0 286.17 13.70 -7 9 0 298.47 20.50 -7 9 0 284.97 17.70 -7 9 0 307.27 20.40 7 9 0 274.47 18.90 -7 9 0 305.97 17.20 7 9 0 310.97 15.00 7 9 0 294.47 10.10 7 9 0 240.08 19.70 -7 9 0 264.57 15.10 7 9 0 274.87 17.70 7 9 0 316.27 20.20 -7 9 0 269.87 14.20 -7 9 0 286.47 17.30 7 9 0 270.67 16.10 -7 9 0 292.07 11.70 7 9 0 297.57 13.20 -7 9 0 297.77 16.00 7 9 0 266.57 16.30 -7 9 0 256.67 17.00 9 -9 0 159.48 17.20 9 -9 0 192.68 11.90 9 -9 0 183.28 13.10 9 -9 0 174.48 22.60 9 -9 0 174.48 10.70 9 9 0 186.08 19.60 -9 9 0 195.38 16.20 -9 9 0 186.58 16.30 -9 9 0 201.38 16.00 9 9 0 152.38 13.20 9 9 0 210.58 17.90 -9 9 0 161.98 18.80 -9 9 0 181.78 23.70 9 9 0 174.58 16.10 -9 9 0 184.28 10.50 9 9 0 172.58 16.10 9 9 0 197.98 19.00 -9 9 0 181.88 15.80 9 9 0 173.68 17.30 -9 9 0 209.98 19.20 -9 9 0 181.48 14.90 -9 9 0 176.68 16.10 9 9 0 186.38 14.90 9 9 0 199.08 24.00 11 -9 0 14.90 13.50 11 -9 0 26.50 6.50 11 -9 0 14.20 6.70 11 -9 0 12.20 7.80 11 -9 0 5.80 19.00 11 9 0 20.50 11.50 11 9 0 7.50 10.90 -11 9 0 14.90 9.30 -11 9 0 15.40 5.70 -11 9 0 14.20 8.90 -11 9 0 13.30 9.50 11 9 0 32.10 13.10 -11 9 0 0.50 9.40 11 9 0 11.40 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5.60 -2 -10 0 44.40 8.30 -2 -10 0 18.30 9.60 2 -10 0 37.60 11.10 -2 -10 0 34.20 4.40 -2 -10 0 34.50 6.90 -2 -10 0 32.00 6.00 2 -10 0 43.30 7.50 -2 10 0 33.60 9.00 2 10 0 40.90 8.00 -2 10 0 40.70 8.00 2 10 0 41.60 5.70 -2 10 0 34.60 9.10 -2 10 0 43.20 5.30 2 10 0 45.20 4.70 2 10 0 18.80 7.80 -2 10 0 39.40 6.70 2 10 0 41.00 4.20 2 10 0 40.90 8.90 2 10 0 47.10 6.50 -2 10 0 43.80 6.90 2 10 0 45.80 9.40 2 10 0 42.60 7.30 -2 10 0 53.39 10.00 -2 10 0 38.60 7.70 -4 -10 0 95.99 7.90 -4 -10 0 120.19 14.00 4 -10 0 97.89 10.60 4 -10 0 81.29 10.30 4 -10 0 93.29 7.30 4 -10 0 89.99 13.30 -4 -10 0 100.99 11.60 -4 -10 0 102.69 7.00 4 -10 0 91.69 8.30 4 -10 0 91.49 5.50 -4 10 0 108.39 13.30 4 10 0 96.39 11.40 4 10 0 96.99 5.20 -4 10 0 94.49 11.50 -4 10 0 83.19 11.20 -4 10 0 83.49 8.40 4 10 0 110.69 13.90 -4 10 0 86.59 11.10 4 10 0 87.79 7.70 -4 10 0 92.29 10.60 4 10 0 109.19 5.20 4 10 0 122.59 15.20 -4 10 0 92.89 10.50 4 10 0 102.29 8.10 4 10 0 95.89 11.00 -4 10 0 93.79 6.40 4 10 0 86.29 10.50 4 10 0 104.29 8.30 -4 10 0 91.99 12.50 -6 -10 0 160.28 16.20 6 -10 0 106.29 16.00 6 -10 0 176.38 9.40 6 -10 0 157.58 17.50 6 -10 0 169.38 11.00 6 -10 0 157.38 11.10 6 -10 0 168.88 11.60 6 10 0 163.28 18.40 6 10 0 178.98 17.80 -6 10 0 141.69 8.10 6 10 0 163.08 10.70 -6 10 0 150.98 17.90 6 10 0 143.39 15.40 -6 10 0 156.58 15.20 -6 10 0 154.88 15.40 -6 10 0 155.28 15.90 6 10 0 156.28 8.50 -6 10 0 181.18 14.80 6 10 0 183.88 17.80 -6 10 0 151.38 11.70 6 10 0 210.48 17.50 -6 10 0 165.88 18.40 6 10 0 167.88 6.50 -6 10 0 152.78 16.80 6 10 0 147.49 14.40 8 -10 0 60.49 8.30 8 -10 0 63.29 8.00 8 -10 0 70.49 11.00 8 -10 0 68.59 8.20 8 -10 0 68.59 13.80 -8 10 0 80.09 11.30 -8 10 0 66.29 10.30 -8 10 0 72.79 11.90 8 10 0 60.29 11.60 8 10 0 74.19 13.30 8 10 0 94.29 11.50 8 10 0 71.79 15.00 8 10 0 63.49 13.30 -8 10 0 74.39 12.00 -8 10 0 59.99 6.70 -8 10 0 76.99 11.40 8 10 0 68.19 11.40 8 10 0 68.29 10.50 8 10 0 56.09 8.10 -8 10 0 59.69 10.20 -8 10 0 70.99 12.90 -8 10 0 71.39 14.20 10 -10 0 85.39 9.80 10 -10 0 84.89 14.70 10 -10 0 52.59 16.70 10 -10 0 75.69 9.50 -10 10 0 74.19 13.80 10 10 0 63.29 14.40 -10 10 0 59.89 11.00 10 10 0 78.29 11.20 10 10 0 79.09 14.50 -10 10 0 70.39 7.80 -10 10 0 106.69 16.20 -10 10 0 76.39 12.80 -10 10 0 72.79 12.80 -10 10 0 74.39 13.60 10 10 0 100.89 14.80 -10 10 0 66.19 15.50 10 10 0 86.49 14.70 10 10 0 78.99 13.90 -10 10 0 88.89 12.50 10 10 0 64.89 13.40 12 -10 0 57.09 10.40 12 -10 0 71.39 9.40 12 -10 0 90.69 20.70 12 -10 0 39.10 18.30 12 -10 0 54.99 9.40 12 10 0 50.39 16.60 -12 10 0 74.59 9.10 -12 10 0 87.29 16.80 12 10 0 63.19 12.20 12 10 0 71.89 16.60 -12 10 0 60.49 15.00 12 10 0 55.19 17.70 -12 10 0 77.19 13.60 -12 10 0 70.69 21.50 -12 10 0 106.99 30.30 -12 10 0 46.10 15.20 12 10 0 96.79 14.50 12 10 0 77.99 16.60 -12 10 0 48.10 11.90 -12 10 0 66.19 13.70 14 -10 0 -1.90 11.00 14 -10 0 25.20 10.00 14 10 0 41.50 18.20 -14 10 0 6.20 8.20 -14 10 0 29.30 18.40 -14 10 0 -9.00 12.10 14 10 0 21.30 15.90 14 10 0 -9.30 18.70 14 10 0 11.80 20.60 14 10 0 7.90 14.60 14 10 0 8.20 11.80 1 -11 0 108.09 14.50 1 -11 0 136.89 12.90 1 -11 0 120.39 13.60 -1 -11 0 122.59 8.00 -1 -11 0 164.78 19.40 1 -11 0 121.59 8.50 -1 -11 0 108.59 13.40 1 -11 0 114.89 9.20 -1 -11 0 96.49 10.20 1 11 0 149.88 16.00 1 11 0 125.19 15.70 -1 11 0 117.09 9.70 1 11 0 88.09 12.10 -1 11 0 138.29 15.80 -1 11 0 123.69 11.80 1 11 0 121.09 10.60 1 11 0 103.19 10.10 -1 11 0 139.79 16.40 1 11 0 116.19 10.30 -1 11 0 118.39 9.10 -1 11 0 137.69 15.60 1 11 0 130.99 16.80 -1 11 0 140.09 14.00 -1 11 0 110.49 11.00 1 11 0 120.09 8.90 3 -11 0 3.40 3.90 3 -11 0 7.00 4.40 -3 -11 0 5.30 5.30 -3 -11 0 7.50 8.30 -3 -11 0 9.70 3.90 3 -11 0 12.40 6.80 3 -11 0 11.20 12.00 -3 -11 0 2.20 5.90 3 -11 0 7.20 7.80 -3 11 0 7.00 8.90 3 11 0 5.80 4.20 3 11 0 -0.60 7.20 -3 11 0 8.80 7.70 -3 11 0 11.60 9.10 -3 11 0 14.00 6.60 3 11 0 -3.70 4.20 3 11 0 11.90 7.40 -3 11 0 3.40 6.40 3 11 0 5.80 4.20 -3 11 0 10.00 4.80 3 11 0 7.20 8.30 3 11 0 13.60 10.40 -3 11 0 0.10 8.70 -3 11 0 0.30 7.20 3 11 0 3.00 5.00 3 11 0 4.50 3.10 3 11 0 -9.90 7.50 -5 -11 0 123.99 9.20 5 -11 0 127.69 7.00 -5 -11 0 139.29 15.50 5 -11 0 114.39 12.30 -5 -11 0 119.39 8.10 5 -11 0 131.59 8.90 5 -11 0 123.39 10.10 5 -11 0 131.39 17.50 5 -11 0 86.09 15.70 -5 11 0 126.69 6.80 5 11 0 118.59 10.80 5 11 0 136.59 15.60 -5 11 0 123.79 15.70 -5 11 0 135.79 17.10 5 11 0 131.99 6.40 5 11 0 117.79 14.10 5 11 0 100.59 10.40 5 11 0 133.79 17.20 5 11 0 156.28 17.80 -5 11 0 129.49 11.00 -5 11 0 108.39 13.10 5 11 0 126.19 9.00 5 11 0 124.79 6.20 -5 11 0 108.89 14.00 5 11 0 128.39 16.30 -5 11 0 144.29 17.00 -5 11 0 122.99 16.20 -5 11 0 138.79 17.10 7 -11 0 4.80 7.20 7 -11 0 22.70 5.30 7 -11 0 27.50 7.80 7 -11 0 24.20 12.20 7 -11 0 29.30 7.30 7 11 0 26.70 3.50 -7 11 0 20.70 4.50 7 11 0 35.70 12.20 -7 11 0 28.70 9.70 7 11 0 53.79 13.10 -7 11 0 53.49 12.70 -7 11 0 17.80 10.20 -7 11 0 25.00 8.80 7 11 0 28.50 5.20 -7 11 0 22.80 10.10 -7 11 0 32.80 12.10 -7 11 0 33.30 11.80 7 11 0 38.10 13.70 7 11 0 26.20 8.90 -7 11 0 33.70 9.90 7 11 0 11.70 12.10 7 11 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-4 12 0 91.59 15.30 -4 12 0 71.99 13.10 4 12 0 104.99 13.10 -4 12 0 80.89 8.40 4 12 0 78.19 6.80 -4 12 0 84.19 10.90 4 12 0 78.19 14.60 4 12 0 79.29 8.50 4 12 0 70.49 11.40 6 -12 0 74.49 7.30 -6 -12 0 66.39 13.70 6 -12 0 83.89 9.60 6 -12 0 75.29 10.50 -6 -12 0 81.59 9.10 6 -12 0 62.49 13.80 6 12 0 79.79 6.40 6 12 0 74.39 6.20 -6 12 0 72.49 14.90 6 12 0 74.89 8.70 6 12 0 73.69 13.80 -6 12 0 76.89 10.00 6 12 0 89.49 13.00 -6 12 0 98.59 14.40 -6 12 0 75.69 11.90 -6 12 0 81.09 6.00 6 12 0 62.09 14.00 -6 12 0 93.29 15.50 -6 12 0 53.39 12.00 -6 12 0 66.59 12.20 6 12 0 71.19 14.80 8 -12 0 39.80 8.70 8 -12 0 44.10 7.10 8 -12 0 45.60 9.50 8 -12 0 49.99 15.80 8 -12 0 38.10 9.70 8 12 0 46.60 5.50 8 12 0 45.10 11.90 8 12 0 44.80 11.40 8 12 0 14.40 15.50 8 12 0 51.79 5.10 -8 12 0 49.99 15.10 8 12 0 49.80 6.90 -8 12 0 41.60 11.20 8 12 0 -4.10 14.60 8 12 0 22.00 15.30 -8 12 0 31.60 14.90 -8 12 0 53.39 15.00 -8 12 0 40.60 13.20 -8 12 0 49.20 14.00 -8 12 0 56.69 13.70 -8 12 0 38.50 11.90 -8 12 0 37.60 5.50 10 -12 0 24.80 7.30 10 -12 0 10.50 16.70 10 -12 0 22.70 9.10 10 -12 0 20.90 10.10 10 12 0 22.20 14.60 -10 12 0 8.80 12.40 10 12 0 44.40 18.10 -10 12 0 21.50 5.70 -10 12 0 15.00 16.50 -10 12 0 15.00 13.30 10 12 0 2.90 11.00 -10 12 0 47.90 19.90 10 12 0 30.00 4.60 10 12 0 17.50 13.80 10 12 0 39.20 17.90 -10 12 0 12.20 14.70 10 12 0 24.20 15.40 -10 12 0 7.90 14.40 -10 12 0 40.30 17.30 -10 12 0 8.40 15.20 12 -12 0 68.39 13.80 12 -12 0 92.89 11.50 12 -12 0 96.29 13.80 -12 12 0 131.99 21.00 -12 12 0 95.39 12.00 12 12 0 107.49 20.50 -12 12 0 113.49 19.60 12 12 0 79.69 15.10 12 12 0 91.99 19.40 12 12 0 91.29 20.90 12 12 0 79.89 8.70 -12 12 0 116.89 18.30 -12 12 0 98.19 21.20 1 -13 0 105.19 11.10 1 -13 0 113.49 15.80 1 -13 0 138.99 17.10 -1 -13 0 124.09 13.40 -1 -13 0 134.39 14.90 -1 13 0 124.79 13.40 -1 13 0 120.79 18.60 -1 13 0 108.89 13.30 -1 13 0 83.79 14.90 -1 13 0 116.59 11.10 1 13 0 129.39 12.70 1 13 0 125.69 16.20 1 13 0 125.19 18.10 -1 13 0 124.59 18.30 1 13 0 103.69 11.70 -3 -13 0 13.60 10.20 3 -13 0 34.60 9.90 -3 -13 0 17.00 5.50 -3 -13 0 0.20 10.00 3 -13 0 27.00 6.50 -3 -13 0 12.70 7.40 3 -13 0 7.30 5.60 3 13 0 -4.00 9.90 3 13 0 15.80 9.70 -3 13 0 21.50 8.80 -3 13 0 21.00 7.10 3 13 0 -17.20 12.50 -3 13 0 13.60 10.60 3 13 0 23.70 6.80 -3 13 0 13.60 13.00 -3 13 0 11.90 8.50 3 13 0 -1.60 10.60 -3 13 0 30.70 15.00 3 13 0 9.20 5.00 -5 -13 0 111.39 16.00 -5 -13 0 101.09 10.30 5 -13 0 113.09 13.20 5 -13 0 116.19 10.70 5 -13 0 100.99 14.90 5 -13 0 87.99 9.90 -5 -13 0 117.19 12.10 5 13 0 98.79 11.90 -5 13 0 106.49 17.30 5 13 0 110.49 11.00 -5 13 0 108.49 11.40 5 13 0 117.99 17.40 -5 13 0 116.39 15.80 -5 13 0 107.49 13.40 5 13 0 115.99 8.10 5 13 0 118.39 15.10 -5 13 0 111.59 17.50 5 13 0 82.79 16.90 5 13 0 105.09 8.50 5 13 0 104.09 14.60 -5 13 0 103.79 16.50 -5 13 0 109.29 15.90 7 -13 0 24.90 13.90 7 -13 0 31.30 5.80 7 -13 0 34.30 7.50 7 -13 0 20.90 10.50 7 -13 0 29.20 16.40 -7 13 0 27.00 12.10 7 13 0 43.80 5.30 -7 13 0 24.70 13.60 -7 13 0 34.00 4.00 -7 13 0 31.40 15.80 -7 13 0 36.50 11.80 7 13 0 34.60 5.00 -7 13 0 35.80 16.20 7 13 0 36.90 18.10 7 13 0 37.90 7.20 7 13 0 40.60 11.40 -7 13 0 31.90 13.50 7 13 0 46.90 12.60 7 13 0 25.50 14.00 9 -13 0 -8.70 9.00 9 -13 0 -12.00 6.70 9 -13 0 -6.80 10.60 9 13 0 23.40 19.60 -9 13 0 27.40 15.80 -9 13 0 2.60 14.60 9 13 0 26.40 17.00 -9 13 0 -4.00 17.40 -9 13 0 7.20 14.10 9 13 0 -6.60 11.60 -9 13 0 28.20 14.50 9 13 0 4.30 4.60 -9 13 0 11.90 4.90 -9 13 0 12.50 16.00 0 -14 0 7.30 10.80 0 -14 0 3.90 5.80 0 -14 0 -5.70 8.10 0 -14 0 7.00 10.50 0 14 0 -14.50 23.30 0 14 0 -6.30 12.00 0 14 0 6.30 8.20 0 14 0 4.90 7.90 0 14 0 24.10 16.20 0 14 0 16.90 8.20 -2 -14 0 154.38 18.10 2 -14 0 141.09 12.80 2 -14 0 181.88 14.60 2 -14 0 132.69 16.00 -2 -14 0 195.08 21.60 -2 -14 0 144.49 11.60 -2 -14 0 112.49 13.00 2 -14 0 147.49 16.00 -2 14 0 134.59 18.30 -2 14 0 147.29 13.80 2 14 0 101.79 17.50 -2 14 0 139.09 17.40 -2 14 0 109.99 12.40 2 14 0 177.48 22.40 2 14 0 165.38 14.50 -2 14 0 117.39 20.90 2 14 0 122.59 11.80 -2 14 0 204.88 23.50 2 14 0 153.38 16.20 -4 -14 0 22.90 8.60 4 -14 0 15.40 11.50 4 -14 0 3.90 7.30 -4 -14 0 28.10 13.50 4 -14 0 14.10 7.60 4 -14 0 0.40 12.40 -4 -14 0 20.10 6.70 4 14 0 12.80 7.10 -4 14 0 29.50 15.30 4 14 0 49.00 16.80 -4 14 0 29.20 9.40 4 14 0 21.30 12.30 -4 14 0 4.00 13.80 4 14 0 7.60 5.40 -4 14 0 14.20 16.20 -4 14 0 5.10 8.60 -4 14 0 16.70 11.50 4 14 0 18.60 12.50 -4 14 0 40.80 13.80 6 -14 0 29.30 11.80 6 -14 0 -6.00 7.60 6 -14 0 11.50 7.30 -6 14 0 2.80 15.30 6 14 0 5.60 7.10 -6 14 0 -7.30 17.90 6 14 0 21.40 5.40 6 14 0 28.90 12.50 6 14 0 5.40 5.40 -6 14 0 8.00 11.80 -6 14 0 21.10 12.20 -6 14 0 24.20 13.90 -6 14 0 29.20 15.90 6 14 0 -40.80 14.40 8 -14 0 112.29 13.00 8 -14 0 113.29 15.30 8 -14 0 64.29 11.80 8 14 0 84.79 9.80 8 14 0 106.99 9.80 -8 14 0 32.60 17.40 -8 14 0 59.79 14.00 8 14 0 73.99 19.70 -8 14 0 57.49 19.50 -8 14 0 83.29 22.60 8 14 0 77.29 16.20 8 14 0 87.99 9.30 -8 14 0 94.09 19.00 1 -15 0 51.99 15.50 1 -15 0 55.59 14.70 1 -15 0 28.30 7.90 1 -15 0 24.70 10.80 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53.99 15.40 16 -4 -3 20.40 11.10 16 -4 -3 14.10 8.40 -16 -4 3 22.90 11.40 16 -4 -3 35.30 8.50 -16 4 3 23.00 12.90 -16 4 3 22.90 6.60 -16 4 3 20.90 13.00 16 4 -3 32.80 18.50 16 4 -3 38.20 11.80 16 4 -3 42.30 13.80 16 4 -3 25.90 4.50 14 -4 -3 0.30 13.30 14 -4 -3 0.90 7.10 14 -4 -3 16.40 7.00 -14 -4 3 5.50 8.30 14 -4 -3 -3.10 6.70 14 -4 -3 13.10 13.00 14 4 -3 7.10 7.60 14 4 -3 2.20 9.60 14 4 -3 4.90 6.40 14 4 -3 0.80 4.60 14 4 -3 7.60 6.30 14 4 -3 12.40 8.00 14 4 -3 2.20 7.70 -14 4 3 -10.20 13.30 14 4 -3 12.60 3.40 14 4 -3 18.70 12.50 -14 4 3 17.60 9.90 -14 4 3 3.00 4.40 12 -4 -3 132.09 16.80 12 -4 -3 125.79 10.70 12 -4 -3 98.09 15.80 12 -4 -3 127.29 10.80 12 -4 -3 122.79 10.60 12 -4 -3 136.19 14.60 -12 -4 3 121.99 13.20 -12 4 3 132.49 14.20 12 4 -3 124.89 11.20 -12 4 3 119.69 15.10 12 4 -3 135.69 6.20 12 4 -3 122.89 14.40 12 4 -3 117.69 12.60 12 4 -3 116.19 16.40 12 4 -3 130.59 14.20 -12 4 3 124.59 14.90 12 4 -3 120.59 11.40 -12 4 3 123.59 13.00 -12 4 3 135.49 14.90 12 4 -3 118.29 10.20 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344.67 12.70 8 4 -3 331.87 15.90 -8 4 3 345.77 16.50 6 -4 -3 2525.85 54.49 6 -4 -3 2584.24 55.39 6 -4 -3 2491.95 53.59 6 -4 -3 2503.75 56.99 6 -4 -3 2450.65 52.29 6 -4 -3 2610.24 59.19 6 -4 -3 2495.25 54.19 6 -4 -3 2553.04 54.19 6 4 -3 2498.75 55.29 -6 4 3 2561.84 55.79 -6 4 3 2316.47 55.79 6 4 -3 2528.15 55.09 -6 4 3 2516.75 56.39 -6 4 3 2444.36 58.39 6 4 -3 2522.65 57.09 -6 4 3 2465.45 53.29 6 4 -3 2518.35 56.99 6 4 -3 2485.75 55.19 6 4 -3 2528.55 52.49 -6 4 3 2477.85 51.49 -6 4 3 2503.25 55.69 -6 4 3 2526.95 55.29 6 4 -3 2457.25 53.09 4 -4 -3 160.78 5.70 4 -4 -3 162.08 9.00 4 -4 -3 155.78 9.80 -4 -4 3 163.28 7.60 4 -4 -3 149.19 7.00 4 -4 -3 161.18 6.20 -4 -4 3 168.78 7.10 4 -4 -3 154.08 8.70 4 -4 -3 150.28 8.90 -4 4 3 168.38 6.90 -4 4 3 144.69 9.70 -4 4 3 166.18 6.90 4 4 -3 156.88 5.50 -4 4 3 155.08 9.50 -4 4 3 156.68 9.10 4 4 -3 162.98 8.60 4 4 -3 160.08 8.50 -4 4 3 161.48 9.50 4 4 -3 157.98 9.20 -4 4 3 162.58 7.10 4 4 -3 161.08 5.30 4 4 -3 165.78 8.80 2 -4 -3 6.00 2.60 2 -4 -3 7.00 3.30 2 -4 -3 5.00 1.70 -2 -4 3 5.40 1.10 2 -4 -3 3.80 2.50 2 -4 -3 4.10 3.60 -2 -4 3 6.10 1.40 -2 -4 3 6.30 2.70 -2 -4 3 4.60 1.40 2 -4 -3 6.60 1.10 -2 -4 3 7.10 2.70 2 -4 -3 11.50 4.00 2 -4 -3 6.60 2.20 2 -4 -3 6.10 1.10 2 4 -3 5.50 2.90 2 4 -3 5.70 2.20 2 4 -3 8.00 3.30 2 4 -3 5.30 1.60 -2 4 3 0.40 2.80 -2 4 3 4.50 1.50 -2 4 3 5.50 2.20 -2 4 3 5.60 2.00 -2 4 3 8.20 3.20 -2 4 3 3.30 3.40 2 4 -3 5.10 3.30 2 4 -3 4.80 2.20 2 4 -3 3.30 2.30 -2 4 3 4.70 3.30 0 -4 -3 264.87 9.20 0 -4 -3 269.87 9.80 0 -4 3 301.57 8.60 0 -4 -3 255.87 11.90 0 -4 -3 293.57 9.60 0 -4 3 296.57 10.10 0 -4 3 285.77 8.30 0 -4 3 308.67 11.60 0 -4 -3 272.17 9.50 0 -4 3 295.97 8.50 0 -4 -3 257.67 10.70 0 -4 -3 277.87 11.80 0 -4 -3 270.47 7.50 0 4 3 275.97 9.50 0 4 3 286.57 8.50 0 4 -3 291.37 9.80 0 4 3 279.27 8.50 0 4 -3 261.47 9.80 0 4 -3 283.57 11.20 0 4 3 301.77 10.40 0 4 -3 283.07 11.40 0 4 -3 272.07 9.10 0 4 3 287.87 7.20 0 4 -3 286.47 10.30 0 4 3 302.17 10.10 0 4 -3 300.57 11.10 0 4 3 291.77 12.40 0 4 3 295.17 12.40 -2 -4 -3 2011.10 46.70 -2 -4 -3 1999.20 46.60 2 -4 3 2002.00 45.90 2 -4 3 1983.30 40.20 2 -4 3 1999.60 43.50 -2 -4 -3 1989.50 42.00 2 -4 3 2022.70 47.00 2 -4 3 1966.10 44.00 -2 -4 -3 2008.40 42.40 -2 -4 -3 2044.60 42.40 2 -4 3 1970.20 43.40 2 -4 3 1964.00 43.70 -2 -4 -3 2009.90 43.90 -2 -4 -3 2045.00 46.50 -2 4 -3 1969.60 40.90 2 4 3 1989.10 42.20 2 4 3 2015.10 47.30 2 4 3 2058.39 47.70 -2 4 -3 1995.20 46.30 -2 4 -3 1981.90 45.20 -2 4 -3 1996.90 44.90 -2 4 -3 2006.80 45.40 -2 4 -3 1973.20 44.80 -2 4 -3 1943.91 44.90 2 4 3 2004.80 43.80 2 4 3 2013.70 42.40 2 4 3 2049.40 46.00 2 4 3 2048.20 43.30 2 4 3 2017.10 43.10 4 -4 3 69.49 7.60 4 -4 3 65.59 6.50 -4 -4 -3 79.09 6.50 4 -4 3 68.69 6.70 4 -4 3 76.29 9.20 4 -4 3 64.79 7.80 -4 -4 -3 77.29 6.00 -4 -4 -3 73.59 8.00 4 -4 3 63.49 5.70 -4 -4 -3 71.69 8.90 4 -4 3 74.19 5.50 -4 -4 -3 73.69 4.90 -4 -4 -3 70.59 8.40 4 4 3 72.39 6.60 -4 4 -3 71.19 9.60 -4 4 -3 70.99 7.50 4 4 3 85.19 9.60 4 4 3 75.79 8.80 4 4 3 75.49 5.90 -4 4 -3 59.29 7.70 4 4 3 68.99 7.50 4 4 3 72.89 7.10 -4 4 -3 85.29 7.20 -4 4 -3 74.79 7.40 -4 4 -3 76.79 7.90 4 4 3 94.69 9.00 -4 4 -3 77.19 8.40 4 4 3 71.39 4.80 4 4 3 74.89 4.90 -6 -4 -3 595.24 19.50 6 -4 3 553.94 22.20 6 -4 3 592.04 15.90 -6 -4 -3 589.24 18.30 6 -4 3 610.54 20.10 6 -4 3 588.84 20.90 -6 -4 -3 569.34 21.60 -6 -4 -3 592.34 14.90 6 -4 3 575.44 20.70 -6 -4 -3 587.34 17.80 -6 -4 -3 580.34 19.10 6 -4 3 588.14 16.30 6 -4 3 576.14 18.10 -6 4 -3 592.74 18.60 6 4 3 608.44 22.70 -6 4 -3 594.34 22.60 -6 4 -3 557.44 19.70 6 4 3 589.94 20.70 6 4 3 598.94 15.40 -6 4 -3 602.74 20.50 -6 4 -3 579.34 18.30 -6 4 -3 575.14 20.30 6 4 3 575.14 20.50 6 4 3 581.14 17.50 6 4 3 588.34 21.90 6 4 3 602.54 17.40 8 -4 3 132.49 13.90 -8 -4 -3 120.19 6.90 -8 -4 -3 113.09 8.60 -8 -4 -3 132.59 9.30 8 -4 3 112.89 14.20 8 -4 3 140.99 11.50 8 -4 3 129.39 13.60 -8 -4 -3 114.69 10.10 8 -4 3 139.29 8.60 -8 -4 -3 126.79 7.20 8 -4 3 114.79 9.10 8 4 3 130.79 8.90 -8 4 -3 136.99 15.80 8 4 3 125.59 12.30 -8 4 -3 122.99 12.90 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43.90 7.70 2 8 3 37.30 8.60 -2 8 -3 42.20 8.00 2 8 3 44.10 6.70 -2 8 -3 35.90 7.40 2 8 3 36.50 5.10 -2 8 -3 33.70 7.10 -2 8 -3 35.20 5.90 -2 8 -3 37.70 7.00 2 8 3 39.20 4.40 -2 8 -3 28.40 5.20 -2 8 -3 42.00 7.20 2 8 3 38.30 4.90 4 -8 3 1.60 3.20 -4 -8 -3 -2.20 7.00 4 -8 3 9.20 5.10 -4 -8 -3 18.30 6.70 4 -8 3 0.40 6.70 4 -8 3 4.50 3.50 4 -8 3 -2.50 7.80 4 -8 3 6.40 3.40 -4 -8 -3 5.30 4.20 -4 8 -3 3.30 4.80 -4 8 -3 8.20 7.10 -4 8 -3 6.90 6.70 4 8 3 1.70 7.10 -4 8 -3 9.00 5.30 4 8 3 -1.30 6.90 -4 8 -3 1.00 6.90 4 8 3 7.70 3.80 4 8 3 12.70 4.60 -4 8 -3 3.90 3.60 -4 8 -3 -0.90 5.70 4 8 3 5.20 4.20 -4 8 -3 10.50 6.00 4 8 3 13.20 7.20 -4 8 -3 8.60 4.80 4 8 3 6.30 2.90 4 8 3 2.40 4.50 -4 8 -3 3.60 4.90 6 -8 3 142.39 13.20 -6 -8 -3 170.88 16.20 -6 -8 -3 121.79 13.50 -6 -8 -3 140.49 9.80 6 -8 3 148.69 13.10 -6 -8 -3 153.18 7.20 6 -8 3 158.68 17.60 6 -8 3 143.19 17.80 6 -8 3 152.18 8.20 6 -8 3 143.69 9.50 -6 8 -3 150.58 13.50 -6 8 -3 142.49 11.10 6 8 3 162.38 9.40 6 8 3 135.49 16.00 -6 8 -3 148.29 17.60 6 8 3 147.19 17.00 6 8 3 125.19 10.90 -6 8 -3 154.58 14.50 -6 8 -3 148.59 11.30 -6 8 -3 150.08 13.70 -6 8 -3 142.89 14.60 6 8 3 157.18 10.40 6 8 3 175.28 16.30 -6 8 -3 161.08 12.20 6 8 3 133.69 11.50 6 8 3 140.29 6.50 -6 8 -3 140.39 10.60 -6 8 -3 143.19 15.40 8 -8 3 539.75 29.50 8 -8 3 545.05 29.80 -8 -8 -3 535.95 26.40 -8 -8 -3 517.55 16.00 8 -8 3 583.34 24.70 -8 -8 -3 515.25 22.10 8 -8 3 524.95 16.10 8 -8 3 525.15 19.20 -8 -8 -3 503.15 17.60 8 -8 3 534.95 18.20 -8 8 -3 481.05 23.10 -8 8 -3 518.75 20.60 -8 8 -3 534.15 20.30 8 8 3 487.55 28.30 8 8 3 521.25 18.10 8 8 3 551.64 23.10 -8 8 -3 520.85 29.40 8 8 3 558.44 26.10 -8 8 -3 503.05 21.40 -8 8 -3 528.55 25.70 8 8 3 469.75 24.80 -8 8 -3 504.85 25.60 8 8 3 535.55 21.70 -8 8 -3 505.75 22.80 8 8 3 526.95 26.20 8 8 3 505.45 19.10 -8 8 -3 532.45 20.80 8 8 3 515.05 17.80 10 -8 3 50.89 7.00 10 -8 3 61.39 7.50 10 -8 3 50.29 8.70 -10 -8 -3 48.30 6.60 -10 -8 -3 53.99 7.30 10 -8 3 69.29 15.30 10 -8 3 72.89 17.70 -10 8 -3 59.49 9.50 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76.49 9.30 11 9 -3 64.09 6.40 -11 9 3 67.79 19.80 9 -9 -3 33.50 9.30 9 -9 -3 29.90 5.20 9 -9 -3 18.80 6.50 9 -9 -3 25.10 7.00 9 -9 -3 25.20 11.20 9 -9 -3 13.50 15.60 9 9 -3 26.50 9.00 9 9 -3 17.40 9.60 9 9 -3 24.20 3.90 -9 9 3 15.90 8.70 9 9 -3 31.00 12.90 9 9 -3 20.80 11.20 9 9 -3 22.20 5.50 -9 9 3 15.50 8.40 -9 9 3 20.90 11.60 -9 9 3 14.30 9.80 -9 9 3 38.50 9.70 9 9 -3 50.19 11.20 9 9 -3 18.30 9.10 9 9 -3 24.70 8.30 9 9 -3 24.60 8.50 -9 9 3 7.00 6.60 -9 9 3 43.10 8.10 -9 9 3 6.40 9.20 7 -9 -3 228.08 16.60 7 -9 -3 230.18 13.10 7 -9 -3 217.58 12.10 7 -9 -3 227.38 12.20 7 -9 -3 233.48 10.10 7 -9 -3 269.17 23.20 7 9 -3 222.88 16.90 -7 9 3 227.98 17.80 7 9 -3 230.18 11.70 7 9 -3 231.98 8.60 7 9 -3 228.38 18.10 -7 9 3 195.68 14.50 7 9 -3 240.68 16.80 7 9 -3 236.88 16.80 7 9 -3 221.58 18.00 7 9 -3 214.48 10.10 -7 9 3 198.58 12.80 -7 9 3 239.38 17.60 7 9 -3 228.38 16.20 -7 9 3 200.58 15.90 -7 9 3 236.98 14.10 5 -9 -3 437.86 14.20 5 -9 -3 440.36 17.50 -5 -9 3 423.06 11.00 5 -9 -3 412.26 18.90 5 -9 -3 435.16 16.00 5 -9 -3 409.06 23.30 5 -9 -3 427.86 18.70 -5 -9 3 441.46 17.30 -5 9 3 425.46 22.00 5 9 -3 426.16 13.70 -5 9 3 458.45 15.70 -5 9 3 440.76 18.70 -5 9 3 408.56 17.00 -5 9 3 421.36 15.50 5 9 -3 437.26 13.50 5 9 -3 413.86 12.60 -5 9 3 417.26 21.00 5 9 -3 450.15 20.10 5 9 -3 430.96 20.20 5 9 -3 406.06 20.20 5 9 -3 452.75 20.80 -5 9 3 431.26 21.30 5 9 -3 418.86 18.30 5 9 -3 423.86 12.20 5 9 -3 437.46 13.80 3 -9 -3 132.69 8.70 3 -9 -3 114.29 10.10 -3 -9 3 111.29 8.60 -3 -9 3 108.49 9.90 -3 -9 3 103.69 9.40 3 -9 -3 106.59 11.90 3 -9 -3 122.09 13.50 -3 -9 3 121.99 6.00 3 -9 -3 136.79 11.40 3 -9 -3 131.99 8.20 3 -9 -3 112.89 13.00 -3 9 3 112.89 13.20 -3 9 3 117.19 14.00 -3 9 3 128.59 9.10 3 9 -3 116.39 11.90 3 9 -3 112.29 12.20 3 9 -3 128.19 13.40 -3 9 3 120.59 13.70 3 9 -3 116.49 7.10 3 9 -3 122.79 7.80 3 9 -3 129.39 7.50 3 9 -3 123.79 9.10 -3 9 3 140.89 10.40 -3 9 3 116.59 8.60 3 9 -3 104.29 11.60 3 9 -3 130.89 8.40 -3 9 3 108.19 7.30 1 -9 -3 353.46 18.60 1 -9 -3 362.86 14.30 1 -9 -3 344.47 15.80 1 -9 -3 364.06 13.50 -1 -9 3 387.86 14.30 1 -9 -3 361.06 17.20 -1 -9 3 373.16 12.70 -1 -9 3 365.16 19.90 1 -9 -3 367.06 18.10 -1 -9 3 362.16 16.50 -1 -9 3 358.06 12.10 1 9 -3 376.66 11.30 -1 9 3 367.06 17.80 -1 9 3 398.26 13.00 1 9 -3 356.26 17.60 1 9 -3 364.76 18.60 1 9 -3 353.86 13.80 1 9 -3 368.16 15.10 -1 9 3 354.36 19.90 1 9 -3 386.86 18.20 1 9 -3 362.26 13.00 -1 9 3 355.16 14.80 1 9 -3 382.26 14.20 1 9 -3 357.86 17.40 -1 9 3 373.06 14.60 -1 9 3 370.36 20.20 -1 -9 -3 35.80 6.50 -1 -9 -3 35.20 7.80 1 -9 3 39.20 10.30 -1 -9 -3 42.60 8.50 1 -9 3 43.30 5.20 1 -9 3 45.40 4.30 1 -9 3 34.20 8.20 -1 -9 -3 44.10 8.90 1 -9 3 48.70 7.70 -1 -9 -3 49.00 6.10 -1 9 -3 52.99 7.80 1 9 3 38.30 5.90 -1 9 -3 52.39 9.70 1 9 3 50.49 6.20 1 9 3 60.09 6.30 -1 9 -3 42.90 7.60 -1 9 -3 34.60 6.90 1 9 3 44.50 7.40 1 9 3 35.70 9.00 -1 9 -3 48.00 7.10 -1 9 -3 45.80 8.40 1 9 3 48.40 7.80 -1 9 -3 41.80 4.40 -1 9 -3 50.59 9.80 -1 9 -3 43.80 6.30 1 9 3 44.30 9.10 3 -9 3 26.70 8.40 3 -9 3 27.20 9.70 -3 -9 -3 31.00 5.20 -3 -9 -3 44.60 9.20 -3 -9 -3 37.40 8.40 3 -9 3 26.80 5.30 3 -9 3 28.70 5.10 3 -9 3 23.00 4.20 -3 9 -3 28.40 7.70 -3 9 -3 31.80 5.90 -3 9 -3 19.30 8.00 -3 9 -3 31.30 6.50 -3 9 -3 30.50 6.90 3 9 3 38.40 5.10 3 9 3 37.60 9.30 -3 9 -3 26.10 4.10 -3 9 -3 33.60 5.90 3 9 3 53.79 10.50 -3 9 -3 31.20 7.90 -3 9 -3 35.30 8.50 3 9 3 37.10 8.80 3 9 3 34.50 5.40 -3 9 -3 19.10 7.40 3 9 3 30.40 5.40 3 9 3 52.09 7.10 3 9 3 37.20 4.30 5 -9 3 2025.10 56.39 -5 -9 -3 1948.01 47.50 5 -9 3 2092.39 45.90 5 -9 3 2059.49 45.20 5 -9 3 2011.10 55.89 5 -9 3 2079.89 47.20 -5 -9 -3 2007.10 55.19 5 -9 3 2057.79 48.20 -5 -9 -3 2058.09 53.39 5 9 3 2011.50 43.20 -5 9 -3 2034.40 53.29 -5 9 -3 2042.10 51.59 5 9 3 2017.00 47.70 5 9 3 2027.60 47.40 5 9 3 2071.19 57.29 -5 9 -3 2074.29 49.10 -5 9 -3 2085.09 55.89 -5 9 -3 2014.40 52.19 5 9 3 2002.10 53.59 -5 9 -3 2049.79 52.79 -5 9 -3 2060.89 45.90 5 9 3 2074.09 57.59 -5 9 -3 2062.29 52.39 5 9 3 2037.40 47.10 5 9 3 2027.80 49.00 -5 9 -3 2038.60 49.50 -5 9 -3 2029.80 54.79 -7 -9 -3 179.58 19.00 7 -9 3 201.58 11.50 -7 -9 -3 189.18 11.40 -7 -9 -3 185.08 16.70 7 -9 3 198.08 10.80 7 -9 3 148.49 17.10 7 -9 3 227.08 27.20 7 -9 3 188.48 10.00 7 -9 3 201.08 16.70 7 9 3 183.48 20.00 7 9 3 198.88 15.10 7 9 3 197.58 14.10 -7 9 -3 174.18 16.10 7 9 3 159.88 19.90 -7 9 -3 198.88 13.20 -7 9 -3 205.18 18.80 -7 9 -3 195.68 14.90 7 9 3 213.98 22.10 -7 9 -3 183.98 12.90 -7 9 -3 185.38 13.50 -7 9 -3 179.18 17.80 7 9 3 184.38 12.20 7 9 3 191.98 20.20 -7 9 -3 187.48 22.20 7 9 3 185.38 7.60 -7 9 -3 168.18 16.00 7 9 3 214.28 17.60 7 9 3 194.28 11.30 9 -9 3 29.20 12.80 9 -9 3 11.20 15.70 9 -9 3 40.50 7.30 -9 -9 -3 21.50 5.90 9 -9 3 28.60 5.70 9 -9 3 13.10 6.00 -9 9 -3 19.80 11.70 -9 9 -3 28.20 8.10 9 9 3 9.70 9.60 -9 9 -3 31.50 10.40 -9 9 -3 22.80 13.50 -9 9 -3 26.30 7.60 9 9 3 18.70 10.70 9 9 3 19.60 11.80 9 9 3 18.80 12.60 -9 9 -3 18.10 7.30 -9 9 -3 34.70 10.20 9 9 3 25.30 6.30 9 9 3 24.40 7.10 -9 9 -3 18.70 11.00 11 -9 3 37.60 7.40 11 -9 3 42.10 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3 4 1938.01 43.40 7 3 -4 1866.31 43.90 -7 3 4 1848.12 44.00 7 3 -4 1881.01 40.80 7 3 -4 1898.81 43.10 -7 3 4 1909.51 43.70 7 3 -4 1901.41 42.00 7 3 -4 1894.01 38.90 7 3 -4 1912.11 40.00 -7 3 4 1915.41 47.30 7 3 -4 1905.91 39.70 -5 -3 4 123.89 6.80 5 -3 -4 118.99 8.50 5 -3 -4 118.89 8.30 5 -3 -4 140.79 9.90 5 -3 -4 115.69 4.70 5 -3 -4 131.79 6.50 5 -3 -4 119.59 6.70 5 -3 -4 124.89 8.50 -5 -3 4 125.59 8.60 -5 -3 4 123.29 4.70 5 -3 -4 124.39 5.60 -5 -3 4 122.79 6.90 -5 3 4 127.29 6.50 -5 3 4 123.59 8.20 -5 3 4 119.59 8.90 -5 3 4 116.79 8.20 5 3 -4 127.19 8.30 5 3 -4 131.99 5.60 5 3 -4 130.79 6.60 5 3 -4 127.89 4.70 -5 3 4 127.69 6.70 5 3 -4 121.89 4.80 5 3 -4 123.89 8.40 -5 3 4 123.69 6.20 -5 3 4 124.19 5.20 5 3 -4 115.99 8.90 5 3 -4 124.09 5.70 -3 -3 4 2093.89 43.10 -3 -3 4 2007.60 41.10 3 -3 -4 1896.51 40.50 3 -3 -4 2034.40 46.10 -3 -3 4 1972.80 40.90 3 -3 -4 2022.80 46.40 3 -3 -4 2018.20 44.60 3 -3 -4 2077.39 45.60 3 -3 -4 1931.61 41.20 -3 -3 4 2030.10 44.70 -3 -3 4 2032.60 44.70 -3 -3 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22.20 -1 3 -19 70.59 15.00 1 3 19 36.60 16.70 -1 3 -19 80.79 19.70 1 3 19 72.99 21.80 -1 3 -19 41.50 14.10 1 3 19 17.40 18.50 -10 -4 19 -5.80 15.30 10 -4 -19 3.00 28.10 10 -4 -19 -1.50 13.80 10 -4 -19 1.50 15.30 10 4 -19 -1.20 11.00 10 4 -19 -15.90 13.50 10 4 -19 59.39 32.50 -10 4 19 -27.80 18.70 -10 4 19 10.50 15.70 -8 -4 19 -8.30 14.70 8 -4 -19 28.00 14.70 8 -4 -19 -22.60 18.70 8 -4 -19 -24.50 27.40 8 -4 -19 17.10 15.40 -8 4 19 18.40 17.20 8 4 -19 7.50 30.40 -8 4 19 17.90 13.70 -8 4 19 19.50 19.10 8 4 -19 24.80 11.80 8 4 -19 14.40 14.40 6 -4 -19 11.30 17.90 6 -4 -19 66.89 24.50 6 -4 -19 28.40 14.80 6 -4 -19 32.30 16.70 -6 -4 19 46.20 16.50 6 -4 -19 18.70 29.50 -6 4 19 20.60 9.70 6 4 -19 32.10 16.80 -6 4 19 45.20 18.00 6 4 -19 47.50 29.90 -6 4 19 20.70 13.00 6 4 -19 44.70 15.50 -6 4 19 26.10 18.30 6 4 -19 32.80 11.40 4 -4 -19 16.80 15.20 -4 -4 19 19.50 4.40 4 -4 -19 30.70 28.60 -4 -4 19 13.90 14.60 4 -4 -19 21.60 15.40 4 -4 -19 44.80 21.20 4 4 -19 -3.40 28.30 -4 4 19 25.50 11.70 -4 4 19 27.80 21.00 4 4 -19 32.50 15.30 -4 4 19 39.00 21.10 4 4 -19 28.10 15.30 4 4 -19 33.10 25.70 -4 4 19 48.80 17.90 4 4 -19 40.30 11.60 2 -4 -19 4.90 27.80 -2 -4 19 11.00 6.40 -2 -4 19 -0.80 15.20 2 -4 -19 10.00 16.50 2 -4 -19 8.10 16.80 2 -4 -19 14.60 17.40 2 4 -19 23.00 18.20 2 4 -19 14.70 11.60 2 4 -19 11.10 29.80 -2 4 19 27.40 20.00 -2 4 19 -5.40 13.70 -2 4 19 30.60 17.90 2 4 -19 21.10 15.80 0 -4 19 10.30 14.80 0 -4 -19 -2.10 17.20 0 -4 -19 31.10 28.50 0 -4 -19 29.30 21.90 0 -4 19 6.80 9.60 0 -4 -19 45.50 18.10 0 4 -19 -24.90 10.90 0 4 -19 -8.90 30.00 0 4 19 22.90 20.00 0 4 19 -31.50 14.90 0 4 19 7.10 18.80 0 4 -19 -3.10 17.30 0 4 -19 0.50 14.60 0 4 -19 -1.00 16.40 -9 -5 19 31.30 16.10 7 -5 -19 50.79 29.30 7 -5 -19 6.90 16.60 7 -5 -19 35.70 15.30 7 -5 -19 27.50 19.20 -7 -5 19 -1.40 14.30 7 5 -19 27.90 19.20 7 5 -19 22.00 29.60 -7 5 19 -2.80 17.30 7 5 -19 15.70 10.60 -7 5 19 5.60 14.40 -7 5 19 12.20 19.10 7 5 -19 3.10 14.50 5 -5 -19 31.70 17.40 5 -5 -19 20.80 15.70 5 -5 -19 -3.60 26.00 -5 -5 19 11.90 4.30 -5 -5 19 17.30 14.70 5 -5 -19 26.80 19.30 -5 5 19 16.50 17.70 -5 5 19 9.10 12.70 5 5 -19 8.90 14.80 5 5 -19 24.90 17.30 5 5 -19 27.10 10.40 5 5 -19 15.80 30.20 -5 5 19 14.10 19.60 -5 5 19 14.60 12.30 3 -5 -19 60.69 19.50 3 -5 -19 38.20 16.20 -3 -5 19 8.60 15.00 3 -5 -19 13.00 20.40 3 -5 -19 38.00 27.30 -3 -5 19 20.10 5.60 -3 5 19 0.20 18.20 -3 5 19 2.90 18.30 3 5 -19 -2.40 30.30 -3 5 19 28.30 14.10 3 5 -19 27.40 10.20 3 5 -19 44.70 17.10 3 5 -19 21.60 16.20 1 -5 -19 17.80 27.80 -1 -5 19 27.10 16.60 1 -5 -19 -5.70 18.90 1 -5 -19 8.40 19.10 -1 -5 19 16.80 7.80 1 -5 -19 65.69 18.50 -1 5 19 41.70 23.00 1 5 -19 19.20 16.50 -1 5 19 47.30 16.60 1 5 -19 4.10 16.30 1 5 -19 24.20 32.80 -1 5 19 16.20 18.80 -6 -6 19 2.60 15.10 6 -6 -19 -3.00 20.10 6 -6 -19 16.90 16.20 6 -6 -19 22.50 18.50 6 -6 -19 9.40 26.20 -6 6 19 2.40 13.20 6 6 -19 0.30 14.50 6 6 -19 -6.70 32.90 -6 6 19 27.90 20.00 -6 6 19 -2.20 22.50 -6 6 19 16.50 12.90 6 6 -19 -43.80 17.80 -4 -6 19 11.00 4.50 4 -6 -19 12.60 16.80 4 -6 -19 31.10 29.80 4 -6 -19 20.40 25.40 4 -6 -19 9.20 17.90 -4 -6 19 7.60 13.70 4 6 -19 38.60 16.80 4 6 -19 29.70 18.00 -4 6 19 47.40 18.90 -4 6 19 40.20 14.50 -4 6 19 26.30 20.40 4 6 -19 11.70 30.20 -4 6 19 18.40 12.70 -2 -6 19 23.70 15.50 8 0 -20 63.39 17.20 8 0 -20 43.30 15.90 8 0 -20 43.90 32.70 -8 0 20 72.19 18.90 -6 0 20 14.70 17.50 6 0 -20 -5.70 13.10 6 0 -20 20.10 15.30 6 0 -20 35.70 17.80 6 0 -20 26.10 32.10 4 0 -20 77.19 16.20 -4 0 20 70.79 21.90 -4 0 20 98.19 20.40 -4 0 20 68.29 8.80 4 0 -20 72.09 18.00 4 0 -20 34.50 18.90 4 0 -20 67.89 32.60 2 0 -20 83.59 15.20 2 0 -20 49.90 18.80 2 0 -20 77.29 21.80 -2 0 20 59.19 11.60 -2 0 20 55.79 17.90 -2 0 20 23.70 18.20 2 0 -20 75.49 17.30 2 0 -20 29.60 31.30 0 0 20 44.30 19.50 9 -1 -20 5.70 15.10 -9 -1 20 8.00 16.30 9 -1 -20 -5.40 31.90 9 -1 -20 33.20 15.40 -9 1 20 -24.50 16.50 9 1 -20 -6.90 14.30 9 1 -20 0.40 14.60 9 1 -20 -38.30 30.80 7 -1 -20 40.00 14.70 -7 -1 20 36.90 17.30 7 -1 -20 65.89 21.30 7 -1 -20 7.50 15.10 7 -1 -20 -18.40 29.30 -7 1 20 -23.30 17.50 7 1 -20 -25.00 30.70 7 1 -20 25.70 16.00 7 1 -20 39.00 14.40 -5 -1 20 75.09 18.60 5 -1 -20 72.79 17.10 5 -1 -20 41.90 33.90 5 -1 -20 64.49 17.60 5 -1 -20 46.50 19.30 5 1 -20 79.79 15.80 5 1 -20 90.39 33.10 -5 1 20 69.99 18.10 5 1 -20 35.30 21.20 -5 1 20 63.39 19.80 5 1 -20 67.29 17.90 -3 -1 20 -8.40 7.50 3 -1 -20 -31.70 15.40 3 -1 -20 20.00 29.60 3 -1 -20 5.10 16.30 -3 -1 20 -14.40 15.70 3 -1 -20 32.60 22.70 3 1 -20 -7.80 15.00 -3 1 20 -11.10 18.20 3 1 -20 21.80 14.50 3 1 -20 24.50 33.00 -3 1 20 -13.80 18.40 -3 1 20 6.50 9.80 3 1 -20 11.10 13.80 3 1 -20 -5.60 21.40 1 -1 -20 13.20 16.40 -1 -1 20 18.10 11.30 -1 -1 20 50.39 20.80 1 -1 -20 61.49 14.70 1 -1 -20 13.50 15.70 -1 -1 20 25.50 18.50 1 -1 -20 49.30 31.90 1 -1 -20 11.30 17.70 1 1 -20 40.50 20.60 -1 1 20 9.30 18.20 1 1 -20 -0.50 13.80 1 1 -20 0.00 17.50 1 1 -20 -2.10 30.70 -1 1 20 16.80 12.80 1 1 -20 34.80 15.30 -1 1 20 35.40 18.60 8 -2 -20 35.70 23.40 8 -2 -20 64.09 33.30 8 -2 -20 71.09 17.70 8 -2 -20 51.99 17.00 -8 -2 20 54.29 18.10 8 2 -20 59.39 17.00 8 2 -20 76.69 33.30 8 2 -20 78.69 15.30 -8 2 20 48.70 19.70 6 -2 -20 28.60 22.20 6 -2 -20 20.00 15.70 -6 -2 20 13.10 16.00 6 -2 -20 29.20 16.00 6 -2 -20 10.60 29.90 6 2 -20 11.80 15.30 -6 2 20 37.30 18.70 -6 2 20 28.90 27.50 6 2 -20 7.10 30.80 6 2 -20 2.50 12.70 4 -2 -20 14.10 15.40 4 -2 -20 32.80 19.40 4 -2 -20 -7.00 16.30 -4 -2 20 -4.40 16.90 -4 -2 20 10.90 5.30 4 -2 -20 -34.10 29.60 4 2 -20 19.30 17.20 4 2 -20 21.70 17.40 4 2 -20 -19.70 31.30 4 2 -20 2.40 13.80 -4 2 20 10.30 18.60 -4 2 20 6.00 9.80 -4 2 20 1.50 19.30 4 2 -20 -22.40 16.40 2 -2 -20 42.70 17.20 2 -2 -20 14.50 16.70 2 -2 -20 27.80 13.20 2 -2 -20 18.40 15.70 -2 -2 20 28.70 9.10 -2 -2 20 31.70 19.30 2 -2 -20 23.00 32.30 2 2 -20 46.80 14.60 2 2 -20 39.50 18.20 2 2 -20 1.10 32.90 -2 2 20 8.50 12.70 2 2 -20 14.40 14.60 -2 2 20 40.60 20.60 -2 2 20 -13.80 19.90 2 2 -20 45.10 20.30 -7 -3 20 27.40 16.80 7 -3 -20 31.70 31.50 7 -3 -20 -4.30 15.30 7 -3 -20 25.90 15.80 7 -3 -20 10.20 20.30 7 3 -20 17.00 16.60 7 3 -20 -52.29 30.30 7 3 -20 16.30 12.90 -7 3 20 10.60 17.70 5 -3 -20 -0.80 20.60 -5 -3 20 -16.20 14.90 5 -3 -20 13.30 16.40 5 -3 -20 42.30 32.50 5 -3 -20 22.20 17.10 5 3 -20 27.40 17.30 5 3 -20 22.80 16.10 -5 3 20 -12.80 17.50 5 3 -20 51.99 33.10 5 3 -20 22.60 12.60 -5 3 20 -15.80 12.30 -5 3 20 10.00 19.80 -3 -3 20 5.50 6.20 3 -3 -20 4.30 22.20 3 -3 -20 44.90 17.70 3 -3 -20 28.40 33.40 3 -3 -20 -16.90 16.90 -3 -3 20 8.30 17.60 -3 3 20 -16.70 16.90 -3 3 20 -1.60 17.90 3 3 -20 -6.50 17.00 -3 3 20 10.20 12.80 3 3 -20 22.30 35.50 3 3 -20 17.90 15.40 3 3 -20 14.30 13.90 -6 -4 20 7.80 15.20 -6 4 20 21.00 20.40 4 -4 -20 6.90 33.60 -4 -4 20 -5.60 14.70 4 4 -20 36.50 34.60 4 4 -20 44.80 17.90 -4 4 20 14.40 12.90 -4 4 20 28.80 21.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 95572 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' 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 O3 O 0.7027(2) 0.3757(3) 0.4779(2) 0.0231(7) Uani 1 1 d . . . . . O4 O 0.5970(2) 0.2636(3) 0.3580(2) 0.0242(7) Uani 1 1 d . . . . . O5 O 0.4022(2) 0.2459(3) 0.3334(2) 0.0274(7) Uani 1 1 d . . . . . O2 O 0.6411(2) 0.4734(3) 0.6116(2) 0.0251(7) Uani 1 1 d . . . . . O1 O 0.4507(2) 0.4858(3) 0.6123(3) 0.0363(9) Uani 1 1 d . . . . . N1 N 0.5094(3) 0.3449(3) 0.4912(3) 0.0269(9) Uani 1 1 d D . . . . H1 H 0.515(3) 0.284(3) 0.521(3) 0.028(14) Uiso 1 1 d D . . . . H3 H 0.531(5) 0.396(3) 0.528(4) 0.10(3) Uiso 1 1 d D . . . . H2 H 0.532(4) 0.332(5) 0.447(3) 0.07(3) Uiso 1 1 d D . . . . H4 H 0.448(2) 0.354(4) 0.472(3) 0.052(19) Uiso 1 1 d D . . . . C14 C 0.7337(3) 0.3631(3) 0.4074(3) 0.0222(9) Uani 1 1 d . . . . . C9 C 0.6774(3) 0.3004(3) 0.3420(3) 0.0230(9) Uani 1 1 d . . . . . C15 C 0.7633(3) 0.4319(4) 0.5469(3) 0.0262(10) Uani 1 1 d . . . . . H15A H 0.7652 0.5077 0.5322 0.031 Uiso 1 1 calc R . . . . H15B H 0.8268 0.4030 0.5578 0.031 Uiso 1 1 calc R . . . . C12 C 0.8414(4) 0.3863(4) 0.3217(4) 0.0314(11) Uani 1 1 d . . . . . H12 H 0.8972 0.4157 0.3142 0.038 Uiso 1 1 calc R . . . . C7 C 0.4595(3) 0.1590(4) 0.3254(3) 0.0247(10) Uani 1 1 d . . . . . H7A H 0.4232 0.1068 0.2850 0.030 Uiso 1 1 calc R . . . . H7B H 0.4825 0.1238 0.3810 0.030 Uiso 1 1 calc R . . . . C13 C 0.8149(3) 0.4061(4) 0.3957(3) 0.0291(11) Uani 1 1 d . . . . . H13 H 0.8526 0.4493 0.4386 0.035 Uiso 1 1 calc R . . . . C18 C 0.5241(4) 0.5358(4) 0.6724(4) 0.0371(13) Uani 1 1 d . . . . . H18A H 0.5065 0.5456 0.7263 0.045 Uiso 1 1 calc R . . . . H18B H 0.5358 0.6064 0.6512 0.045 Uiso 1 1 calc R . . . . C16 C 0.7280(3) 0.4198(4) 0.6244(3) 0.0249(10) Uani 1 1 d . . . . . H16A H 0.7200 0.3439 0.6355 0.030 Uiso 1 1 calc R . . . . H16B H 0.7732 0.4501 0.6741 0.030 Uiso 1 1 calc R . . . . C11 C 0.7874(4) 0.3245(4) 0.2596(4) 0.0329(11) Uani 1 1 d . . . . . H11 H 0.8065 0.3106 0.2095 0.039 Uiso 1 1 calc R . . . . C10 C 0.7047(4) 0.2817(4) 0.2690(3) 0.0292(10) Uani 1 1 d . . . . . H10 H 0.6672 0.2397 0.2251 0.035 Uiso 1 1 calc R . . . . C6 C 0.3201(4) 0.2111(5) 0.3542(4) 0.0346(12) Uani 1 1 d . . . . . H6A H 0.3363 0.1703 0.4078 0.042 Uiso 1 1 calc R . . . . H6B H 0.2839 0.1648 0.3088 0.042 Uiso 1 1 calc R . . . . C8 C 0.5396(3) 0.1974(4) 0.2940(3) 0.0258(10) Uani 1 1 d . . . . . H8A H 0.5758 0.1364 0.2822 0.031 Uiso 1 1 calc R . . . . H8B H 0.5167 0.2379 0.2409 0.031 Uiso 1 1 calc R . . . . C17 C 0.6112(4) 0.4700(4) 0.6881(3) 0.0301(11) Uani 1 1 d . . . . . H17A H 0.6595 0.4993 0.7360 0.036 Uiso 1 1 calc R . . . . H17B H 0.5983 0.3962 0.7018 0.036 Uiso 1 1 calc R . . . . C5 C 0.2639(4) 0.3066(5) 0.3639(4) 0.0398(13) Uani 1 1 d . . . . . H5AA H 0.2584 0.3546 0.3150 0.048 Uiso 0.779(5) 1 calc R . P A 1 H5AB H 0.2010 0.2847 0.3658 0.048 Uiso 0.779(5) 1 calc R . P A 1 H5BC H 0.2407 0.3395 0.3074 0.048 Uiso 0.221(5) 1 calc R . P A 2 H5BD H 0.2094 0.2824 0.3825 0.048 Uiso 0.221(5) 1 calc R . P A 2 Cl2 Cl 0.4182(5) 0.6271(6) 0.4286(5) 0.130(3) Uani 0.468(3) 1 d D U P A 1 Cl2A Cl 0.5085(6) 0.7581(7) 0.4985(6) 0.104(3) Uani 0.3117(19) 1 d D U P A 1 Cl1 Cl 0.5820(2) 0.5835(2) 0.38497(19) 0.0613(7) Uani 0.779(5) 1 d D U P A 1 Si2 Si 0.2444(2) 0.4131(3) 0.5009(2) 0.0341(8) Uani 0.779(5) 1 d D U P A 1 Si1 Si 0.33967(13) 0.50819(14) 0.61282(16) 0.0387(6) Uani 0.779(5) 1 d D U P A 1 O6 O 0.3100(7) 0.3606(7) 0.4421(6) 0.036(2) Uani 0.779(5) 1 d . U P A 1 C2 C 0.3172(8) 0.6546(6) 0.6039(9) 0.060(3) Uani 0.779(5) 1 d D U P A 1 H2A H 0.2543 0.6690 0.6085 0.090 Uiso 0.779(5) 1 calc GR . P A 1 H2B H 0.3238 0.6798 0.5490 0.090 Uiso 0.779(5) 1 calc GR . P A 1 H2C H 0.3618 0.6912 0.6496 0.090 Uiso 0.779(5) 1 calc GR . P A 1 C4 C 0.1561(11) 0.4973(12) 0.4318(9) 0.077(4) Uani 0.779(5) 1 d D U P A 1 H4A H 0.1859 0.5455 0.4000 0.115 Uiso 0.779(5) 1 calc GR . P A 1 H4B H 0.1241 0.5384 0.4665 0.115 Uiso 0.779(5) 1 calc GR . P A 1 H4C H 0.1113 0.4528 0.3922 0.115 Uiso 0.779(5) 1 calc GR . P A 1 C19 C 0.4897(10) 0.6702(13) 0.3647(12) 0.052(4) Uani 0.468(3) 1 d D U P A 1 H19A H 0.4558 0.6681 0.3040 0.063 Uiso 0.468(3) 1 calc R . P A 1 H19B H 0.5113 0.7434 0.3796 0.063 Uiso 0.468(3) 1 calc R . P A 1 C19A C 0.501(3) 0.684(3) 0.4006(18) 0.102(11) Uani 0.3117(19) 1 d D U P A 1 H19C H 0.4392 0.6498 0.3866 0.122 Uiso 0.3117(19) 1 calc R . P A 1 H19D H 0.4985 0.7380 0.3561 0.122 Uiso 0.3117(19) 1 calc R . P A 1 C1 C 0.3175(7) 0.4677(9) 0.7156(6) 0.071(3) Uani 0.779(5) 1 d D U P A 1 H1A H 0.3455 0.3983 0.7323 0.106 Uiso 0.779(5) 1 calc GR . P A 1 H1B H 0.2506 0.4637 0.7093 0.106 Uiso 0.779(5) 1 calc GR . P A 1 H1C H 0.3448 0.5199 0.7593 0.106 Uiso 0.779(5) 1 calc GR . P A 1 C3 C 0.1823(10) 0.3067(11) 0.5426(6) 0.091(4) Uani 0.779(5) 1 d D U P A 1 H3A H 0.2243 0.2471 0.5618 0.136 Uiso 0.779(5) 1 calc GR . P A 1 H3B H 0.1291 0.2829 0.4976 0.136 Uiso 0.779(5) 1 calc GR . P A 1 H3C H 0.1606 0.3341 0.5902 0.136 Uiso 0.779(5) 1 calc GR . P A 1 Cl13 Cl 0.5538(11) 0.6035(16) 0.4112(10) 0.118(6) Uani 0.221(5) 1 d D U P A 2 Cl14 Cl 0.3732(7) 0.5454(9) 0.3140(12) 0.117(6) Uani 0.221(5) 1 d D U P A 2 Si1A Si 0.3703(5) 0.5639(6) 0.5544(6) 0.052(3) Uani 0.221(5) 1 d D U P A 2 Si2A Si 0.2652(9) 0.4375(10) 0.4867(8) 0.030(2) Uani 0.221(5) 1 d D U P A 2 O6A O 0.308(3) 0.382(3) 0.4184(18) 0.028(6) Uani 0.221(5) 1 d . U P A 2 C20 C 0.4662(16) 0.636(2) 0.316(2) 0.062(7) Uani 0.221(5) 1 d D U P A 2 H20A H 0.4453 0.7099 0.3181 0.075 Uiso 0.221(5) 1 calc R . P A 2 H20B H 0.4902 0.6266 0.2655 0.075 Uiso 0.221(5) 1 calc R . P A 2 C3A C 0.245(2) 0.353(2) 0.5707(15) 0.048(6) Uani 0.221(5) 1 d D U P A 2 H3AA H 0.2476 0.2784 0.5545 0.071 Uiso 0.221(5) 1 calc GR . P A 2 H3AB H 0.1836 0.3680 0.5792 0.071 Uiso 0.221(5) 1 calc GR . P A 2 H3AC H 0.2923 0.3663 0.6235 0.071 Uiso 0.221(5) 1 calc GR . P A 2 C4A C 0.159(4) 0.517(5) 0.445(4) 0.077(4) Uani 0.221(5) 1 d D U P A 2 H4AA H 0.1334 0.5005 0.3846 0.115 Uiso 0.221(5) 1 calc GR . P A 2 H4AB H 0.1752 0.5928 0.4503 0.115 Uiso 0.221(5) 1 calc GR . P A 2 H4AC H 0.1138 0.5014 0.4764 0.115 Uiso 0.221(5) 1 calc GR . P A 2 C1A C 0.313(3) 0.617(4) 0.635(2) 0.079(10) Uani 0.221(5) 1 d D U P A 2 H1AA H 0.2570 0.6560 0.6064 0.118 Uiso 0.221(5) 1 calc GR . P A 2 H1AB H 0.3555 0.6638 0.6741 0.118 Uiso 0.221(5) 1 calc GR . P A 2 H1AC H 0.2956 0.5577 0.6669 0.118 Uiso 0.221(5) 1 calc GR . P A 2 C2A C 0.405(4) 0.682(3) 0.503(3) 0.114(14) Uani 0.221(5) 1 d D U P A 2 H2AA H 0.3496 0.7193 0.4708 0.137 Uiso 0.110(2) 1 calc R . P A 2 H2AB H 0.4424 0.7287 0.5458 0.137 Uiso 0.110(2) 1 calc R . P A 2 H2AC H 0.4415 0.6593 0.4636 0.137 Uiso 0.110(2) 1 calc R . P A 2 H2AD H 0.4727 0.6855 0.5160 0.137 Uiso 0.110(2) 1 calc R . P A 2 H2AE H 0.3800 0.6762 0.4410 0.137 Uiso 0.110(2) 1 calc R . P A 2 H2AF H 0.3809 0.7456 0.5232 0.137 Uiso 0.110(2) 1 calc R . P A 2 P1 P 0.51352(9) 0.10313(11) 0.64278(9) 0.0302(3) Uani 1 1 d . . . . . F5 F 0.4370(3) 0.0334(4) 0.6678(3) 0.0608(11) Uani 1 1 d . . . . . F3 F 0.5869(3) 0.1780(4) 0.6165(4) 0.0853(17) Uani 1 1 d . . . . . F6 F 0.5867(5) 0.0160(5) 0.6645(5) 0.126(3) Uani 1 1 d . . . . . F1 F 0.4786(5) 0.0728(8) 0.5487(3) 0.148(4) Uani 1 1 d . . . . . F2 F 0.4411(5) 0.1949(6) 0.6217(6) 0.155(4) Uani 1 1 d . . . . . F4 F 0.5434(5) 0.1403(7) 0.7363(4) 0.130(3) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O3 0.0181(15) 0.0235(16) 0.0259(17) -0.0052(13) 0.0023(13) -0.0040(12) O4 0.0255(17) 0.0224(16) 0.0251(16) -0.0044(13) 0.0074(13) -0.0052(13) O5 0.0234(16) 0.0265(17) 0.0285(17) 0.0004(14) -0.0001(13) -0.0029(13) O2 0.0217(16) 0.0235(16) 0.0279(17) -0.0024(13) 0.0023(13) 0.0050(13) O1 0.0241(18) 0.033(2) 0.046(2) -0.0140(17) -0.0008(15) 0.0099(15) N1 0.024(2) 0.026(2) 0.028(2) -0.0028(18) 0.0021(17) -0.0030(17) C14 0.024(2) 0.016(2) 0.026(2) 0.0029(17) 0.0044(18) 0.0016(17) C9 0.025(2) 0.018(2) 0.026(2) 0.0038(18) 0.0063(18) 0.0003(18) C15 0.021(2) 0.025(2) 0.030(3) -0.0059(19) 0.0024(19) -0.0040(18) C12 0.033(3) 0.022(2) 0.045(3) 0.004(2) 0.019(2) -0.002(2) C7 0.028(2) 0.020(2) 0.023(2) -0.0014(18) -0.0009(18) -0.0055(18) C13 0.028(2) 0.021(2) 0.040(3) 0.002(2) 0.010(2) -0.0015(19) C18 0.029(3) 0.035(3) 0.044(3) -0.016(2) 0.004(2) 0.009(2) C16 0.021(2) 0.021(2) 0.029(2) -0.0026(19) -0.0006(18) 0.0032(17) C11 0.041(3) 0.024(2) 0.040(3) 0.001(2) 0.021(2) 0.000(2) C10 0.033(3) 0.023(2) 0.032(3) -0.001(2) 0.011(2) -0.001(2) C6 0.025(3) 0.038(3) 0.040(3) -0.008(2) 0.008(2) -0.010(2) C8 0.029(2) 0.026(2) 0.020(2) -0.0024(18) 0.0021(18) -0.0051(19) C17 0.026(2) 0.029(3) 0.033(3) -0.010(2) 0.003(2) 0.003(2) C5 0.024(3) 0.044(3) 0.046(3) -0.008(3) -0.002(2) -0.003(2) Cl2 0.109(5) 0.153(6) 0.163(7) 0.105(6) 0.097(5) 0.074(5) Cl2A 0.082(5) 0.080(5) 0.117(6) -0.004(4) -0.032(5) 0.003(4) Cl1 0.0759(18) 0.0445(12) 0.0585(16) 0.0003(11) 0.0086(13) 0.0092(12) Si2 0.0219(14) 0.0345(16) 0.0409(18) 0.0063(12) -0.0007(11) 0.0047(10) Si1 0.0220(9) 0.0195(9) 0.0730(16) -0.0110(9) 0.0096(9) 0.0024(7) O6 0.027(3) 0.025(4) 0.048(6) -0.003(4) -0.006(4) 0.003(3) C2 0.039(5) 0.017(4) 0.114(10) -0.005(4) 0.003(6) 0.012(3) C4 0.066(5) 0.085(8) 0.059(7) -0.017(6) -0.019(4) 0.054(5) C19 0.055(8) 0.049(8) 0.052(9) 0.019(7) 0.013(7) 0.008(7) C19A 0.129(18) 0.093(16) 0.067(11) 0.004(10) -0.002(9) 0.042(15) C1 0.055(6) 0.082(7) 0.074(6) -0.033(5) 0.015(5) -0.029(5) C3 0.118(9) 0.108(8) 0.039(5) -0.012(5) 0.007(6) -0.067(8) Cl13 0.117(10) 0.154(15) 0.095(10) -0.008(9) 0.049(8) 0.050(9) Cl14 0.064(6) 0.061(6) 0.236(18) 0.044(9) 0.058(8) -0.004(5) Si1A 0.038(4) 0.029(4) 0.066(5) -0.016(3) -0.026(4) 0.021(3) Si2A 0.031(6) 0.031(5) 0.024(4) 0.000(4) 0.000(3) 0.010(4) O6A 0.034(10) 0.025(12) 0.019(10) 0.012(7) -0.002(8) 0.012(9) C20 0.066(13) 0.040(13) 0.094(16) 0.006(12) 0.044(11) -0.001(10) C3A 0.054(14) 0.048(12) 0.037(11) -0.002(9) 0.004(10) 0.009(11) C4A 0.066(5) 0.085(8) 0.059(7) -0.017(6) -0.019(4) 0.054(5) C1A 0.045(16) 0.09(2) 0.077(16) -0.051(17) -0.030(12) 0.008(18) C2A 0.11(3) 0.085(19) 0.13(3) 0.005(18) 0.01(2) -0.01(2) P1 0.0219(6) 0.0393(7) 0.0292(6) 0.0107(6) 0.0063(5) -0.0018(5) F5 0.056(2) 0.078(3) 0.053(2) -0.003(2) 0.0229(19) -0.036(2) F3 0.047(2) 0.084(3) 0.134(4) 0.049(3) 0.038(3) -0.010(2) F6 0.130(6) 0.097(4) 0.193(7) 0.095(5) 0.116(6) 0.080(4) F1 0.120(5) 0.294(11) 0.032(2) -0.033(4) 0.024(3) -0.089(6) F2 0.103(5) 0.134(5) 0.269(10) 0.132(6) 0.122(6) 0.080(4) F4 0.106(5) 0.219(8) 0.066(3) -0.067(4) 0.023(3) -0.087(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 C14 O3 C15 116.0(3) . . C9 O4 C8 116.6(4) . . C7 O5 C6 111.2(4) . . C16 O2 C17 109.5(3) . . C18 O1 Si1 120.6(3) . . C18 O1 Si1A 116.7(4) . . O3 C14 C9 116.0(4) . . O3 C14 C13 124.9(4) . . C13 C14 C9 119.1(4) . . O4 C9 C14 115.1(4) . . O4 C9 C10 125.1(4) . . C10 C9 C14 119.8(4) . . O3 C15 C16 108.8(4) . . C11 C12 C13 120.2(5) . . O5 C7 C8 109.6(4) . . C12 C13 C14 120.3(5) . . O1 C18 C17 110.5(4) . . O2 C16 C15 109.4(4) . . C12 C11 C10 120.7(5) . . C9 C10 C11 119.9(5) . . O5 C6 C5 108.5(5) . . O4 C8 C7 108.8(4) . . O2 C17 C18 106.6(4) . . O6 C5 C6 108.5(6) . . O6A C5 C6 116.5(16) . . C19 Cl1 C19A 19.0(9) . . O6 Si2 Si1 108.8(4) . . O6 Si2 C4 108.1(6) . . O6 Si2 C3 110.2(7) . . C4 Si2 Si1 112.2(6) . . C4 Si2 C3 107.2(7) . . C3 Si2 Si1 110.3(4) . . O1 Si1 Si2 108.19(18) . . O1 Si1 C2 108.7(4) . . O1 Si1 C1 111.2(4) . . C2 Si1 Si2 112.6(4) . . C1 Si1 Si2 110.4(3) . . C1 Si1 C2 105.7(5) . . C5 O6 Si2 118.3(7) . . Cl1 C19 Cl2 105.5(8) . . Cl1 C19A Cl2A 125.8(17) . . O1 Si1A Si2A 99.5(5) . . O1 Si1A C1A 102.0(15) . . O1 Si1A C2A 119.6(19) . . C1A Si1A Si2A 101.7(13) . . C2A Si1A Si2A 125.0(19) . . C2A Si1A C1A 105.7(15) . . O6A Si2A Si1A 107.3(17) . . O6A Si2A C3A 116.3(15) . . O6A Si2A C4A 116(3) . . C3A Si2A Si1A 105.8(11) . . C3A Si2A C4A 107.9(17) . . C4A Si2A Si1A 102(3) . . C5 O6A Si2A 124(3) . . Cl14 C20 Cl13 105.1(15) . . F5 P1 F3 177.1(3) . . F6 P1 F5 93.5(3) . . F6 P1 F3 89.4(3) . . F6 P1 F1 95.2(5) . . F6 P1 F2 178.2(5) . . F6 P1 F4 89.0(5) . . F1 P1 F5 92.2(3) . . F1 P1 F3 87.6(4) . . F1 P1 F2 85.9(6) . . F1 P1 F4 175.8(6) . . F2 P1 F5 87.9(3) . . F2 P1 F3 89.2(3) . . F4 P1 F5 87.6(3) . . F4 P1 F3 92.4(3) . . F4 P1 F2 89.9(5) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O3 C14 1.357(6) . O3 C15 1.438(5) . O4 C9 1.375(6) . O4 C8 1.438(5) . O5 C7 1.420(6) . O5 C6 1.426(6) . O2 C16 1.432(5) . O2 C17 1.433(6) . O1 C18 1.419(6) . O1 Si1 1.687(4) . O1 Si1A 1.653(7) . C14 C9 1.419(6) . C14 C13 1.389(7) . C9 C10 1.376(7) . C15 C16 1.500(7) . C12 C13 1.388(7) . C12 C11 1.367(8) . C7 C8 1.500(7) . C18 C17 1.511(7) . C11 C10 1.396(7) . C6 C5 1.502(8) . C5 O6 1.456(11) . C5 O6A 1.35(4) . Cl2 C19 1.762(14) . Cl2A C19A 1.83(2) . Cl1 C19 1.727(13) . Cl1 C19A 1.82(2) . Si2 Si1 2.340(4) . Si2 O6 1.677(10) . Si2 C4 1.839(9) . Si2 C3 1.861(10) . Si1 C2 1.880(8) . Si1 C1 1.865(10) . Cl13 C20 1.80(2) . Cl14 C20 1.79(2) . Si1A Si2A 2.312(13) . Si1A C1A 1.87(2) . Si1A C2A 1.85(2) . Si2A O6A 1.58(4) . Si2A C3A 1.828(19) . Si2A C4A 1.85(2) . P1 F5 1.580(4) . P1 F3 1.591(4) . P1 F6 1.529(5) . P1 F1 1.538(5) . P1 F2 1.564(5) . P1 F4 1.550(5) .