#------------------------------------------------------------------------------ #$Date: 2019-12-16 12:02:30 +0200 (Mon, 16 Dec 2019) $ #$Revision: 245210 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556590.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_1556590 loop_ _publ_author_name 'Grotjahn, D.B.' 'Martin, J.K.' 'Tom, T.N.' 'Rheingold, A.L.' _publ_section_title ; Cationic Protic Imidazolylidene NHC Complexes of Cp*IrCl+ and Cp*RhCl+ with a Pyridyl Tether Formed at Ambient Temperature ; _journal_name_full Inorganics _journal_page_first 27 _journal_paper_doi 10.3390/inorganics6010027 _journal_volume 6 _journal_year 2018 _chemical_formula_moiety 'C23 H32 Cl Ir N3, F6 P, 1.5(C4 H8 O)' _chemical_formula_sum 'C29 H44 Cl F6 Ir N3 O1.5 P' _chemical_formula_weight 831.29 _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_Hall '-P 2n 2ab' _space_group_name_H-M_alt 'P b c n' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 11.9277(7) _cell_length_b 19.2100(11) _cell_length_c 28.2172(16) _cell_measurement_reflns_used 9938 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 28.15 _cell_measurement_theta_min 2.24 _cell_volume 6465.4(6) _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 'SIR2004 (Burla et al., 2007)' _diffrn_ambient_temperature 120.0 _diffrn_measured_fraction_theta_full 0.899 _diffrn_measured_fraction_theta_max 0.861 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_unetI/netI 0.0420 _diffrn_reflns_Laue_measured_fraction_full 0.899 _diffrn_reflns_Laue_measured_fraction_max 0.861 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 54283 _diffrn_reflns_point_group_measured_fraction_full 0.899 _diffrn_reflns_point_group_measured_fraction_max 0.861 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 28.551 _diffrn_reflns_theta_min 2.010 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.326 _exptl_absorpt_correction_T_max 0.6476 _exptl_absorpt_correction_T_min 0.4110 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 3312 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _refine_diff_density_max 1.198 _refine_diff_density_min -0.859 _refine_diff_density_rms 0.122 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 417 _refine_ls_number_reflns 7090 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0287 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0114P)^2^+11.8459P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.0563 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5367 _reflns_number_total 7090 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; grot304.res created by SHELXL-2014/7 TITL Grot304 in Pbcn CELL 0.71073 11.9277 19.21 28.2172 90 90 90 ZERR 8 0.0007 0.0011 0.0016 0 0 0 LATT 1 SYMM 0.5+X,0.5-Y,-Z SYMM -X,+Y,0.5-Z SYMM 0.5-X,0.5-Y,0.5+Z SFAC C H Cl F Ir N O P UNIT 232 352 8 48 8 24 12 8 EADP F4 F4B EADP F2 F2B L.S. 10 PLAN 5 SIZE 0.11 0.16 0.25 TEMP -153.15 BOND $H fmap 2 acta 50 MERG 2 REM REM REM WGHT 0.011400 11.845901 FVAR 0.04041 0.73974 IR1 5 0.538331 0.243549 0.362140 11.00000 0.01341 0.01283 = 0.01454 0.00086 -0.00026 0.00012 CL1 3 0.645294 0.240688 0.289529 11.00000 0.02241 0.02058 = 0.01775 0.00317 0.00500 0.00240 P1 8 0.018468 0.121671 0.436567 11.00000 0.02782 0.02948 = 0.02177 -0.00723 0.00587 -0.00657 PART 1 F1 4 -0.005396 0.052025 0.468137 21.00000 0.07034 0.02846 = 0.04300 0.00404 0.02320 -0.00805 F2 4 -0.055499 0.087916 0.396037 21.00000 0.03422 0.07459 = 0.03675 -0.02363 -0.00950 -0.00348 F3 4 0.049036 0.186012 0.406240 21.00000 0.04944 0.02873 = 0.03043 0.01089 0.01859 0.01088 F4 4 0.099602 0.148121 0.479113 21.00000 0.04845 0.04636 = 0.02994 -0.01849 -0.01621 -0.00879 PART 0 PART 2 F1B 4 -0.057116 0.059191 0.443034 -21.00000 0.04549 0.01861 = 0.08021 -0.01129 0.02753 -0.00849 F2B 4 -0.058151 0.139878 0.386448 -21.00000 0.03422 0.07459 = 0.03675 -0.02363 -0.00950 -0.00348 F3B 4 0.070714 0.202462 0.425934 -21.00000 0.03995 0.01813 = 0.04145 -0.01724 0.01849 -0.00962 F4B 4 0.075857 0.119351 0.480986 -21.00000 0.04845 0.04636 = 0.02994 -0.01849 -0.01621 -0.00879 PART 0 F5 4 0.122471 0.082062 0.412212 11.00000 0.04344 0.03716 = 0.04780 -0.01250 0.02143 0.00010 F6 4 -0.085540 0.161403 0.460621 11.00000 0.03222 0.04960 = 0.05131 -0.01013 0.02260 -0.00038 N1 6 0.664367 0.309856 0.388675 11.00000 0.01657 0.01577 = 0.01594 0.00236 -0.00155 -0.00427 N2 6 0.466959 0.391796 0.365387 11.00000 0.01544 0.01644 = 0.01191 0.00141 -0.00260 0.00021 N3 6 0.401363 0.347285 0.301670 11.00000 0.01781 0.01381 = 0.01588 -0.00044 -0.00068 0.00041 AFIX 43 H3 2 0.385987 0.317397 0.278947 11.00000 -1.20000 AFIX 0 C1 1 0.464209 0.332077 0.340017 11.00000 0.01473 0.01495 = 0.01464 0.00070 0.00295 0.00029 C2 1 0.363512 0.416181 0.302286 11.00000 0.01566 0.01863 = 0.01192 0.00170 0.00183 0.00398 C3 1 0.405453 0.443572 0.342278 11.00000 0.01910 0.01722 = 0.02014 0.00168 0.00451 0.00446 AFIX 43 H3A 2 0.395142 0.490012 0.352999 11.00000 -1.20000 AFIX 0 C4 1 0.523477 0.397283 0.410587 11.00000 0.02368 0.01949 = 0.01054 -0.00311 -0.00397 -0.00385 AFIX 23 H4A 2 0.481803 0.369592 0.434362 11.00000 -1.20000 H4B 2 0.522273 0.446493 0.420994 11.00000 -1.20000 AFIX 0 C5 1 0.643332 0.372418 0.409125 11.00000 0.02025 0.01311 = 0.02094 0.00222 -0.00073 -0.00355 C6 1 0.727773 0.411623 0.429284 11.00000 0.02809 0.01862 = 0.01935 -0.00026 -0.00224 -0.00445 AFIX 43 H6 2 0.711416 0.455689 0.442911 11.00000 -1.20000 AFIX 0 C7 1 0.836528 0.386308 0.429519 11.00000 0.02395 0.02868 = 0.02653 0.00117 -0.00575 -0.00815 AFIX 43 H7 2 0.895097 0.412116 0.444075 11.00000 -1.20000 AFIX 0 C8 1 0.858501 0.323081 0.408307 11.00000 0.01860 0.02977 = 0.03422 0.00076 -0.00147 -0.00071 AFIX 43 H8 2 0.932592 0.304959 0.407667 11.00000 -1.20000 AFIX 0 C9 1 0.771555 0.286697 0.388109 11.00000 0.02097 0.02028 = 0.02651 0.00054 -0.00201 -0.00142 AFIX 43 H9 2 0.787326 0.243505 0.373129 11.00000 -1.20000 AFIX 0 C10 1 0.285976 0.446078 0.265696 11.00000 0.02103 0.02085 = 0.01591 0.00245 0.00159 0.00436 C11 1 0.334772 0.438926 0.216242 11.00000 0.03659 0.03472 = 0.01716 0.00456 -0.00011 0.01458 AFIX 137 H11A 2 0.405663 0.464576 0.214426 11.00000 -1.50000 H11B 2 0.281855 0.457946 0.193043 11.00000 -1.50000 H11C 2 0.348294 0.389641 0.209334 11.00000 -1.50000 AFIX 0 C12 1 0.172623 0.407707 0.268221 11.00000 0.02373 0.04320 = 0.04210 0.00876 -0.00818 -0.00013 AFIX 137 H12A 2 0.183644 0.358479 0.260389 11.00000 -1.50000 H12B 2 0.120237 0.428588 0.245554 11.00000 -1.50000 H12C 2 0.141927 0.411660 0.300324 11.00000 -1.50000 AFIX 0 C13 1 0.269562 0.523438 0.276812 11.00000 0.04115 0.02584 = 0.02358 0.00268 -0.00045 0.01738 AFIX 137 H13A 2 0.236858 0.528466 0.308488 11.00000 -1.50000 H13B 2 0.219122 0.544127 0.253292 11.00000 -1.50000 H13C 2 0.342203 0.547226 0.275770 11.00000 -1.50000 AFIX 0 C14 1 0.414362 0.207516 0.412590 11.00000 0.02336 0.01476 = 0.01161 -0.00005 0.00632 -0.00071 C15 1 0.522879 0.182808 0.427554 11.00000 0.02366 0.01689 = 0.00485 0.00191 -0.00012 -0.00567 C16 1 0.567271 0.138259 0.391406 11.00000 0.01803 0.01476 = 0.01995 0.00290 -0.00064 -0.00154 C17 1 0.486242 0.135030 0.353858 11.00000 0.02230 0.01618 = 0.01489 0.00184 0.00313 -0.00678 C18 1 0.391445 0.177711 0.366559 11.00000 0.01818 0.01919 = 0.01204 0.00396 0.00034 -0.00315 C19 1 0.332142 0.247902 0.441612 11.00000 0.02856 0.02243 = 0.03272 -0.00282 0.01326 0.00132 AFIX 137 H19A 2 0.277717 0.215898 0.455833 11.00000 -1.50000 H19B 2 0.292824 0.281307 0.421295 11.00000 -1.50000 H19C 2 0.371978 0.272978 0.466736 11.00000 -1.50000 AFIX 0 C20 1 0.577522 0.199080 0.473335 11.00000 0.03274 0.03139 = 0.02122 0.00313 -0.00557 -0.00509 AFIX 137 H20A 2 0.562293 0.161625 0.496019 11.00000 -1.50000 H20B 2 0.547820 0.243045 0.485693 11.00000 -1.50000 H20C 2 0.658627 0.203343 0.468602 11.00000 -1.50000 AFIX 0 C21 1 0.675130 0.097605 0.393553 11.00000 0.02831 0.02061 = 0.03839 0.00597 0.00212 0.00597 AFIX 137 H21A 2 0.728414 0.121673 0.414299 11.00000 -1.50000 H21B 2 0.706963 0.093733 0.361644 11.00000 -1.50000 H21C 2 0.660188 0.050956 0.406113 11.00000 -1.50000 AFIX 0 C22 1 0.499311 0.093882 0.309756 11.00000 0.03448 0.02802 = 0.02186 -0.00806 0.00853 -0.01272 AFIX 137 H22A 2 0.479059 0.045275 0.315912 11.00000 -1.50000 H22B 2 0.577390 0.096267 0.299067 11.00000 -1.50000 H22C 2 0.450122 0.112903 0.285135 11.00000 -1.50000 AFIX 0 C23 1 0.284505 0.186159 0.338771 11.00000 0.01718 0.03002 = 0.02874 0.00625 -0.00393 -0.00535 AFIX 137 H23A 2 0.299711 0.178666 0.305023 11.00000 -1.50000 H23B 2 0.255000 0.233270 0.343462 11.00000 -1.50000 H23C 2 0.229218 0.152037 0.349745 11.00000 -1.50000 AFIX 0 O1S 7 0.155931 0.482055 0.493501 11.00000 0.03261 0.03020 = 0.02384 0.00257 -0.00431 0.00643 O2S 7 0.000000 0.118273 0.250000 10.50000 0.04853 0.04636 = 0.13367 0.00000 0.03491 0.00000 C1S 1 0.113047 0.528559 0.458057 11.00000 0.03253 0.02982 = 0.02937 0.01160 -0.00018 0.00802 AFIX 23 H1SA 2 0.158058 0.571837 0.457135 11.00000 -1.20000 H1SB 2 0.034224 0.540934 0.465114 11.00000 -1.20000 AFIX 0 C2S 1 0.120634 0.490509 0.410801 11.00000 0.03008 0.03707 = 0.02542 0.01004 0.00019 0.00456 AFIX 23 H2SA 2 0.164232 0.517865 0.387467 11.00000 -1.20000 H2SB 2 0.045083 0.481234 0.397719 11.00000 -1.20000 AFIX 0 C3S 1 0.181104 0.422211 0.423272 11.00000 0.03320 0.03190 = 0.02794 0.00500 0.00889 0.00658 AFIX 23 H3SA 2 0.127269 0.383453 0.427378 11.00000 -1.20000 H3SB 2 0.236574 0.409450 0.398661 11.00000 -1.20000 AFIX 0 C4S 1 0.237663 0.440456 0.469395 11.00000 0.02210 0.03033 = 0.02792 0.00925 -0.00005 0.00448 AFIX 23 H4SA 2 0.255801 0.398037 0.487785 11.00000 -1.20000 H4SB 2 0.307434 0.467134 0.463803 11.00000 -1.20000 AFIX 0 C5S 1 0.048359 0.161610 0.215222 11.00000 0.06956 0.07389 = 0.05235 0.00045 0.00520 -0.01033 AFIX 23 H5SA 2 0.024459 0.146164 0.183311 11.00000 -1.20000 H5SB 2 0.131108 0.158473 0.216918 11.00000 -1.20000 AFIX 0 C6S 1 0.012537 0.234391 0.223180 11.00000 0.05731 0.06285 = 0.06864 0.00989 -0.00612 -0.00969 AFIX 23 H6SA 2 -0.055207 0.245848 0.204469 11.00000 -1.20000 H6SB 2 0.073041 0.267657 0.215182 11.00000 -1.20000 AFIX 0 HKLF 4 REM Grot304 in Pbcn REM R1 = 0.0287 for 5367 Fo > 4sig(Fo) and 0.0487 for all 7090 data REM 417 parameters refined using 0 restraints END WGHT 0.0114 11.8436 REM Highest difference peak 1.198, deepest hole -0.859, 1-sigma level 0.122 Q1 1 0.9626 0.2555 0.4139 11.00000 0.05 1.20 Q2 1 0.3828 0.2451 0.3613 11.00000 0.05 1.19 Q3 1 0.5405 0.2810 0.3621 11.00000 0.05 0.77 Q4 1 0.5281 0.1929 0.3603 11.00000 0.05 0.65 Q5 1 0.4808 0.2385 0.3600 11.00000 0.05 0.58 REM The information below was added by Olex2. REM REM R1 = 0.0287 for 5367 Fo > 4sig(Fo) and 0.0487 for all 57518 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.20, deepest hole -0.86 REM Mean Shift 0, Max Shift 0.002. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0487 REM R1_gt = 0.0287 REM wR_ref = 0.0563 REM GOOF = 1.022 REM Shift_max = 0.002 REM Shift_mean = 0 REM Reflections_all = 57518 REM Reflections_gt = 5367 REM Parameters = n/a REM Hole = -0.86 REM Peak = 1.20 REM Flack = n/a ; _cod_data_source_file 9bIr_Fig2_Grot304.cif _cod_data_source_block grot304 _cod_original_formula_sum 'C29 H44 Cl F6 Ir N3 O1.50 P' _cod_database_code 1556590 _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 0.648 _shelx_estimated_absorpt_t_min 0.411 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(F4) = Uanis(F4B) Uanis(F2) = Uanis(F2B) 3. Others Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=1-FVAR(1) Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(1) 4.a Secondary CH2 refined with riding coordinates: C4(H4A,H4B), C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB), C6S(H6SA,H6SB) 4.b Aromatic/amide H refined with riding coordinates: N3(H3), C3(H3A), C6(H6), C7(H7), C8(H8), C9(H9) 4.c Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C19(H19A,H19B, H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A, H23B,H23C) ; loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' '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 Ir1 Ir 0.53833(2) 0.24355(2) 0.36214(2) 0.01359(4) Uani 1 1 d . . . . . Cl1 Cl 0.64529(7) 0.24069(4) 0.28953(4) 0.0202(2) Uani 1 1 d . . . . . P1 P 0.01847(9) 0.12167(5) 0.43657(5) 0.0264(3) Uani 1 1 d . . . . . F1 F -0.0054(4) 0.0520(2) 0.4681(2) 0.0473(14) Uani 0.740(5) 1 d . . . A 1 F2 F -0.0555(3) 0.0879(3) 0.39604(16) 0.0485(12) Uani 0.740(5) 1 d . . . A 1 F3 F 0.0490(5) 0.1860(2) 0.4062(2) 0.0362(13) Uani 0.740(5) 1 d . . . A 1 F4 F 0.0996(4) 0.1481(2) 0.47911(17) 0.0416(11) Uani 0.740(5) 1 d . . . A 1 F1B F -0.0571(11) 0.0592(6) 0.4430(7) 0.048(5) Uani 0.260(5) 1 d . . . A 2 F2B F -0.0582(9) 0.1399(7) 0.3864(4) 0.0485(12) Uani 0.260(5) 1 d . . . A 2 F3B F 0.0707(13) 0.2025(7) 0.4259(6) 0.033(4) Uani 0.260(5) 1 d . . . A 2 F4B F 0.0759(12) 0.1194(7) 0.4810(6) 0.0416(11) Uani 0.260(5) 1 d . . . A 2 F5 F 0.1225(2) 0.08206(12) 0.41221(10) 0.0428(7) Uani 1 1 d . . . . . F6 F -0.0855(2) 0.16140(13) 0.46062(10) 0.0444(8) Uani 1 1 d . . . . . N1 N 0.6644(2) 0.30986(13) 0.38868(12) 0.0161(7) Uani 1 1 d . . . . . N2 N 0.4670(2) 0.39180(13) 0.36539(12) 0.0146(7) Uani 1 1 d . . . . . N3 N 0.4014(2) 0.34729(13) 0.30167(12) 0.0158(7) Uani 1 1 d . . . . . H3 H 0.3860 0.3174 0.2789 0.019 Uiso 1 1 calc R . . . . C1 C 0.4642(3) 0.33208(16) 0.34002(14) 0.0148(8) Uani 1 1 d . . . . . C2 C 0.3635(3) 0.41618(17) 0.30229(15) 0.0154(8) Uani 1 1 d . . . . . C3 C 0.4055(3) 0.44357(17) 0.34228(15) 0.0188(9) Uani 1 1 d . . . . . H3A H 0.3951 0.4900 0.3530 0.023 Uiso 1 1 calc R . . . . C4 C 0.5235(3) 0.39728(17) 0.41059(15) 0.0179(9) Uani 1 1 d . . . . . H4A H 0.4818 0.3696 0.4344 0.021 Uiso 1 1 calc R . . . . H4B H 0.5223 0.4465 0.4210 0.021 Uiso 1 1 calc R . . . . C5 C 0.6433(3) 0.37242(16) 0.40913(15) 0.0181(9) Uani 1 1 d . . . . . C6 C 0.7278(3) 0.41162(18) 0.42928(15) 0.0220(9) Uani 1 1 d . . . . . H6 H 0.7114 0.4557 0.4429 0.026 Uiso 1 1 calc R . . . . C7 C 0.8365(3) 0.38631(19) 0.42952(16) 0.0264(10) Uani 1 1 d . . . . . H7 H 0.8951 0.4121 0.4441 0.032 Uiso 1 1 calc R . . . . C8 C 0.8585(3) 0.32308(19) 0.40831(16) 0.0275(11) Uani 1 1 d . . . . . H8 H 0.9326 0.3050 0.4077 0.033 Uiso 1 1 calc R . . . . C9 C 0.7716(3) 0.28670(18) 0.38811(15) 0.0226(10) Uani 1 1 d . . . . . H9 H 0.7873 0.2435 0.3731 0.027 Uiso 1 1 calc R . . . . C10 C 0.2860(3) 0.44608(17) 0.26570(15) 0.0193(9) Uani 1 1 d . . . . . C11 C 0.3348(3) 0.4389(2) 0.21624(15) 0.0295(11) Uani 1 1 d . . . . . H11A H 0.4057 0.4646 0.2144 0.044 Uiso 1 1 calc GR . . . . H11B H 0.2819 0.4579 0.1930 0.044 Uiso 1 1 calc GR . . . . H11C H 0.3483 0.3896 0.2093 0.044 Uiso 1 1 calc GR . . . . C12 C 0.1726(3) 0.4077(2) 0.26822(18) 0.0363(12) Uani 1 1 d . . . . . H12A H 0.1836 0.3585 0.2604 0.055 Uiso 1 1 calc GR . . . . H12B H 0.1202 0.4286 0.2456 0.055 Uiso 1 1 calc GR . . . . H12C H 0.1419 0.4117 0.3003 0.055 Uiso 1 1 calc GR . . . . C13 C 0.2696(4) 0.52344(18) 0.27681(16) 0.0302(11) Uani 1 1 d . . . . . H13A H 0.2369 0.5285 0.3085 0.045 Uiso 1 1 calc GR . . . . H13B H 0.2191 0.5441 0.2533 0.045 Uiso 1 1 calc GR . . . . H13C H 0.3422 0.5472 0.2758 0.045 Uiso 1 1 calc GR . . . . C14 C 0.4144(3) 0.20752(16) 0.41259(15) 0.0166(9) Uani 1 1 d . . . . . C15 C 0.5229(3) 0.18281(16) 0.42755(14) 0.0151(8) Uani 1 1 d . . . . . C16 C 0.5673(3) 0.13826(16) 0.39141(15) 0.0176(9) Uani 1 1 d . . . . . C17 C 0.4862(3) 0.13503(16) 0.35386(15) 0.0178(9) Uani 1 1 d . . . . . C18 C 0.3914(3) 0.17771(16) 0.36656(15) 0.0165(8) Uani 1 1 d . . . . . C19 C 0.3321(3) 0.24790(18) 0.44161(16) 0.0279(10) Uani 1 1 d . . . . . H19A H 0.2777 0.2159 0.4558 0.042 Uiso 1 1 calc GR . . . . H19B H 0.2928 0.2813 0.4213 0.042 Uiso 1 1 calc GR . . . . H19C H 0.3720 0.2730 0.4667 0.042 Uiso 1 1 calc GR . . . . C20 C 0.5775(3) 0.1991(2) 0.47334(16) 0.0285(10) Uani 1 1 d . . . . . H20A H 0.5623 0.1616 0.4960 0.043 Uiso 1 1 calc GR . . . . H20B H 0.5478 0.2430 0.4857 0.043 Uiso 1 1 calc GR . . . . H20C H 0.6586 0.2033 0.4686 0.043 Uiso 1 1 calc GR . . . . C21 C 0.6751(3) 0.09760(18) 0.39355(17) 0.0291(11) Uani 1 1 d . . . . . H21A H 0.7284 0.1217 0.4143 0.044 Uiso 1 1 calc GR . . . . H21B H 0.7070 0.0937 0.3616 0.044 Uiso 1 1 calc GR . . . . H21C H 0.6602 0.0510 0.4061 0.044 Uiso 1 1 calc GR . . . . C22 C 0.4993(3) 0.09388(19) 0.30976(16) 0.0281(11) Uani 1 1 d . . . . . H22A H 0.4791 0.0453 0.3159 0.042 Uiso 1 1 calc GR . . . . H22B H 0.5774 0.0963 0.2991 0.042 Uiso 1 1 calc GR . . . . H22C H 0.4501 0.1129 0.2851 0.042 Uiso 1 1 calc GR . . . . C23 C 0.2845(3) 0.18616(19) 0.33877(16) 0.0253(10) Uani 1 1 d . . . . . H23A H 0.2997 0.1787 0.3050 0.038 Uiso 1 1 calc GR . . . . H23B H 0.2550 0.2333 0.3435 0.038 Uiso 1 1 calc GR . . . . H23C H 0.2292 0.1520 0.3497 0.038 Uiso 1 1 calc GR . . . . O1S O 0.1559(2) 0.48205(13) 0.49350(11) 0.0289(7) Uani 1 1 d . . . . . O2S O 0.0000 0.1183(3) 0.2500 0.076(2) Uani 1 2 d S T P . . C1S C 0.1130(4) 0.5286(2) 0.45806(16) 0.0306(11) Uani 1 1 d . . . . . H1SA H 0.1581 0.5718 0.4571 0.037 Uiso 1 1 calc R . . . . H1SB H 0.0342 0.5409 0.4651 0.037 Uiso 1 1 calc R . . . . C2S C 0.1206(3) 0.4905(2) 0.41080(17) 0.0309(11) Uani 1 1 d . . . . . H2SA H 0.1642 0.5179 0.3875 0.037 Uiso 1 1 calc R . . . . H2SB H 0.0451 0.4812 0.3977 0.037 Uiso 1 1 calc R . . . . C3S C 0.1811(3) 0.4222(2) 0.42327(17) 0.0310(11) Uani 1 1 d . . . . . H3SA H 0.1273 0.3835 0.4274 0.037 Uiso 1 1 calc R . . . . H3SB H 0.2366 0.4094 0.3987 0.037 Uiso 1 1 calc R . . . . C4S C 0.2377(3) 0.44046(19) 0.46939(16) 0.0268(10) Uani 1 1 d . . . . . H4SA H 0.2558 0.3980 0.4878 0.032 Uiso 1 1 calc R . . . . H4SB H 0.3074 0.4671 0.4638 0.032 Uiso 1 1 calc R . . . . C5S C 0.0484(5) 0.1616(3) 0.2152(2) 0.0653(18) Uani 1 1 d . . . . . H5SA H 0.0245 0.1462 0.1833 0.078 Uiso 1 1 calc R . . . . H5SB H 0.1311 0.1585 0.2169 0.078 Uiso 1 1 calc R . . . . C6S C 0.0125(5) 0.2344(3) 0.2232(2) 0.0629(18) Uani 1 1 d . . . . . H6SA H -0.0552 0.2458 0.2045 0.076 Uiso 1 1 calc R . . . . H6SB H 0.0730 0.2677 0.2152 0.076 Uiso 1 1 calc R . . . . 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 Ir1 0.01341(6) 0.01283(6) 0.01454(10) 0.00086(6) -0.00026(6) 0.00012(5) Cl1 0.0224(4) 0.0206(4) 0.0178(6) 0.0032(4) 0.0050(4) 0.0024(3) P1 0.0278(6) 0.0295(5) 0.0218(8) -0.0072(5) 0.0059(5) -0.0066(4) F1 0.070(4) 0.0285(19) 0.043(4) 0.004(2) 0.023(3) -0.008(2) F2 0.0342(18) 0.075(3) 0.037(3) -0.024(3) -0.0095(18) -0.003(2) F3 0.049(3) 0.029(3) 0.030(4) 0.011(2) 0.019(3) 0.011(2) F4 0.048(3) 0.046(3) 0.030(2) -0.018(3) -0.0162(19) -0.009(2) F1B 0.045(8) 0.019(5) 0.080(16) -0.011(7) 0.028(8) -0.008(5) F2B 0.0342(18) 0.075(3) 0.037(3) -0.024(3) -0.0095(18) -0.003(2) F3B 0.040(7) 0.018(5) 0.041(13) -0.017(6) 0.018(7) -0.010(4) F4B 0.048(3) 0.046(3) 0.030(2) -0.018(3) -0.0162(19) -0.009(2) F5 0.0434(15) 0.0372(13) 0.048(2) -0.0125(13) 0.0214(15) 0.0001(11) F6 0.0322(14) 0.0496(15) 0.051(2) -0.0101(14) 0.0226(14) -0.0004(12) N1 0.0166(15) 0.0158(13) 0.016(2) 0.0024(13) -0.0016(14) -0.0043(11) N2 0.0154(14) 0.0164(12) 0.012(2) 0.0014(13) -0.0026(15) 0.0002(11) N3 0.0178(15) 0.0138(13) 0.016(2) -0.0004(13) -0.0007(14) 0.0004(11) C1 0.0147(16) 0.0149(14) 0.015(3) 0.0007(15) 0.0029(17) 0.0003(13) C2 0.0157(17) 0.0186(16) 0.012(3) 0.0017(15) 0.0018(16) 0.0040(13) C3 0.0191(18) 0.0172(16) 0.020(3) 0.0017(16) 0.0045(17) 0.0045(14) C4 0.0237(19) 0.0195(15) 0.011(3) -0.0031(16) -0.0040(17) -0.0039(14) C5 0.0202(18) 0.0131(15) 0.021(3) 0.0022(16) -0.0007(17) -0.0036(13) C6 0.028(2) 0.0186(17) 0.019(3) -0.0003(17) -0.0022(19) -0.0044(15) C7 0.024(2) 0.0287(19) 0.027(3) 0.0012(19) -0.0058(19) -0.0081(16) C8 0.0186(19) 0.0298(19) 0.034(3) 0.001(2) -0.0015(19) -0.0007(15) C9 0.0210(19) 0.0203(17) 0.027(3) 0.0005(18) -0.0020(18) -0.0014(14) C10 0.0210(18) 0.0209(17) 0.016(3) 0.0024(17) 0.0016(17) 0.0044(14) C11 0.037(2) 0.035(2) 0.017(3) 0.005(2) 0.000(2) 0.0146(18) C12 0.024(2) 0.043(2) 0.042(4) 0.009(2) -0.008(2) -0.0001(18) C13 0.041(3) 0.0258(19) 0.024(3) 0.0027(19) 0.000(2) 0.0174(17) C14 0.0234(18) 0.0148(15) 0.012(3) -0.0001(16) 0.0063(17) -0.0007(13) C15 0.0237(19) 0.0169(15) 0.005(2) 0.0019(14) -0.0001(16) -0.0057(13) C16 0.0180(18) 0.0148(15) 0.020(3) 0.0029(16) -0.0006(17) -0.0015(13) C17 0.0223(19) 0.0162(15) 0.015(3) 0.0018(16) 0.0031(17) -0.0068(13) C18 0.0182(17) 0.0192(15) 0.012(3) 0.0040(16) 0.0003(17) -0.0032(13) C19 0.029(2) 0.0224(18) 0.033(3) -0.0028(19) 0.0133(19) 0.0013(16) C20 0.033(2) 0.031(2) 0.021(3) 0.003(2) -0.006(2) -0.0051(17) C21 0.028(2) 0.0206(18) 0.038(3) 0.0060(19) 0.002(2) 0.0060(16) C22 0.034(2) 0.0280(19) 0.022(3) -0.0081(19) 0.009(2) -0.0127(16) C23 0.0172(19) 0.0300(19) 0.029(3) 0.0062(19) -0.0039(19) -0.0053(15) O1S 0.0326(15) 0.0302(14) 0.024(2) 0.0026(13) -0.0043(15) 0.0064(12) O2S 0.049(3) 0.046(3) 0.134(7) 0.000 0.035(4) 0.000 C1S 0.033(2) 0.030(2) 0.029(3) 0.012(2) 0.000(2) 0.0080(17) C2S 0.030(2) 0.037(2) 0.025(3) 0.010(2) 0.000(2) 0.0046(18) C3S 0.033(2) 0.032(2) 0.028(3) 0.005(2) 0.009(2) 0.0066(17) C4S 0.022(2) 0.030(2) 0.028(3) 0.009(2) 0.000(2) 0.0045(16) C5S 0.070(4) 0.074(4) 0.052(5) 0.000(3) 0.005(4) -0.010(3) C6S 0.057(3) 0.063(3) 0.069(5) 0.010(3) -0.006(4) -0.010(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Ir Ir -1.4442 7.9887 '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' 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 N1 Ir1 Cl1 86.46(9) . . N1 Ir1 C14 116.52(14) . . N1 Ir1 C15 94.73(12) . . N1 Ir1 C16 107.98(12) . . N1 Ir1 C17 144.71(12) . . N1 Ir1 C18 155.50(14) . . C1 Ir1 Cl1 89.32(11) . . C1 Ir1 N1 85.01(12) . . C1 Ir1 C14 100.00(13) . . C1 Ir1 C15 132.31(14) . . C1 Ir1 C16 162.85(13) . . C1 Ir1 C17 130.26(14) . . C1 Ir1 C18 98.96(13) . . C14 Ir1 Cl1 155.67(10) . . C14 Ir1 C15 38.64(13) . . C14 Ir1 C16 64.47(13) . . C14 Ir1 C17 64.65(13) . . C15 Ir1 Cl1 138.34(9) . . C15 Ir1 C16 37.98(13) . . C16 Ir1 Cl1 102.33(11) . . C17 Ir1 Cl1 92.16(11) . . C17 Ir1 C15 63.82(14) . . C17 Ir1 C16 38.08(13) . . C18 Ir1 Cl1 117.60(11) . . C18 Ir1 C14 39.00(14) . . C18 Ir1 C15 64.68(14) . . C18 Ir1 C16 64.56(12) . . C18 Ir1 C17 38.69(12) . . F2 P1 F1 87.8(2) . . F2 P1 F4 174.0(2) . . F2 P1 F5 85.84(18) . . F2 P1 F6 93.98(18) . . F3 P1 F1 176.3(3) . . F3 P1 F2 93.4(3) . . F3 P1 F4 91.1(2) . . F3 P1 F5 87.7(2) . . F3 P1 F6 92.1(2) . . F4 P1 F1 87.5(2) . . F1B P1 F2B 86.8(7) . . F1B P1 F3B 164.8(8) . . F1B P1 F5 97.8(5) . . F1B P1 F6 82.3(5) . . F3B P1 F2B 82.2(7) . . F4B P1 F1B 98.9(8) . . F4B P1 F2B 169.2(7) . . F4B P1 F3B 90.4(7) . . F4B P1 F5 89.5(6) . . F4B P1 F6 90.8(6) . . F5 P1 F1 88.9(2) . . F5 P1 F4 90.2(2) . . F5 P1 F2B 98.9(4) . . F5 P1 F3B 94.2(5) . . F6 P1 F1 91.4(2) . . F6 P1 F4 90.0(2) . . F6 P1 F2B 80.8(4) . . F6 P1 F3B 85.6(5) . . F6 P1 F5 179.70(19) . . C5 N1 Ir1 123.7(2) . . C9 N1 Ir1 118.1(2) . . C9 N1 C5 118.1(3) . . C1 N2 C3 110.1(3) . . C1 N2 C4 122.7(3) . . C3 N2 C4 127.2(3) . . C1 N3 H3 124.0 . . C1 N3 C2 112.0(3) . . C2 N3 H3 124.0 . . N2 C1 Ir1 122.8(3) . . N3 C1 Ir1 132.5(3) . . N3 C1 N2 104.7(3) . . N3 C2 C10 123.6(3) . . C3 C2 N3 105.1(3) . . C3 C2 C10 131.2(3) . . N2 C3 H3A 126.0 . . C2 C3 N2 108.0(3) . . C2 C3 H3A 126.0 . . N2 C4 H4A 108.9 . . N2 C4 H4B 108.9 . . N2 C4 C5 113.2(3) . . H4A C4 H4B 107.7 . . C5 C4 H4A 108.9 . . C5 C4 H4B 108.9 . . N1 C5 C4 117.9(3) . . N1 C5 C6 121.6(3) . . C6 C5 C4 120.5(3) . . C5 C6 H6 120.2 . . C5 C6 C7 119.6(3) . . C7 C6 H6 120.2 . . C6 C7 H7 120.5 . . C8 C7 C6 119.0(4) . . C8 C7 H7 120.5 . . C7 C8 H8 120.5 . . C9 C8 C7 119.0(4) . . C9 C8 H8 120.5 . . N1 C9 C8 122.7(3) . . N1 C9 H9 118.6 . . C8 C9 H9 118.6 . . C2 C10 C11 111.2(3) . . C2 C10 C12 109.0(3) . . C2 C10 C13 108.0(3) . . C11 C10 C12 109.6(4) . . C11 C10 C13 109.0(3) . . C13 C10 C12 110.0(3) . . C10 C11 H11A 109.5 . . C10 C11 H11B 109.5 . . C10 C11 H11C 109.5 . . H11A C11 H11B 109.5 . . H11A C11 H11C 109.5 . . H11B C11 H11C 109.5 . . C10 C12 H12A 109.5 . . C10 C12 H12B 109.5 . . C10 C12 H12C 109.5 . . H12A C12 H12B 109.5 . . H12A C12 H12C 109.5 . . H12B C12 H12C 109.5 . . C10 C13 H13A 109.5 . . C10 C13 H13B 109.5 . . C10 C13 H13C 109.5 . . H13A C13 H13B 109.5 . . H13A C13 H13C 109.5 . . H13B C13 H13C 109.5 . . C15 C14 Ir1 71.6(2) . . C15 C14 C18 107.6(3) . . C15 C14 C19 126.8(4) . . C18 C14 Ir1 70.4(2) . . C18 C14 C19 125.0(3) . . C19 C14 Ir1 129.9(2) . . C14 C15 Ir1 69.7(2) . . C14 C15 C20 125.5(3) . . C16 C15 Ir1 71.8(2) . . C16 C15 C14 108.7(3) . . C16 C15 C20 125.8(3) . . C20 C15 Ir1 125.8(2) . . C15 C16 Ir1 70.24(19) . . C15 C16 C17 107.6(3) . . C15 C16 C21 126.6(4) . . C17 C16 Ir1 70.05(19) . . C17 C16 C21 125.6(4) . . C21 C16 Ir1 128.5(2) . . C16 C17 Ir1 71.87(19) . . C16 C17 C18 108.7(3) . . C16 C17 C22 124.9(3) . . C18 C17 Ir1 69.78(18) . . C18 C17 C22 126.5(4) . . C22 C17 Ir1 124.6(3) . . C14 C18 Ir1 70.56(19) . . C14 C18 C23 125.8(3) . . C17 C18 Ir1 71.53(18) . . C17 C18 C14 107.5(3) . . C17 C18 C23 126.6(4) . . C23 C18 Ir1 126.3(2) . . C14 C19 H19A 109.5 . . C14 C19 H19B 109.5 . . C14 C19 H19C 109.5 . . H19A C19 H19B 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . C15 C20 H20A 109.5 . . C15 C20 H20B 109.5 . . C15 C20 H20C 109.5 . . H20A C20 H20B 109.5 . . H20A C20 H20C 109.5 . . H20B C20 H20C 109.5 . . C16 C21 H21A 109.5 . . C16 C21 H21B 109.5 . . C16 C21 H21C 109.5 . . H21A C21 H21B 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . C17 C22 H22A 109.5 . . C17 C22 H22B 109.5 . . C17 C22 H22C 109.5 . . H22A C22 H22B 109.5 . . H22A C22 H22C 109.5 . . H22B C22 H22C 109.5 . . C18 C23 H23A 109.5 . . C18 C23 H23B 109.5 . . C18 C23 H23C 109.5 . . H23A C23 H23B 109.5 . . H23A C23 H23C 109.5 . . H23B C23 H23C 109.5 . . C4S O1S C1S 105.0(3) . . C5S O2S C5S 107.6(6) . 3 O1S C1S H1SA 110.3 . . O1S C1S H1SB 110.3 . . O1S C1S C2S 106.9(3) . . H1SA C1S H1SB 108.6 . . C2S C1S H1SA 110.3 . . C2S C1S H1SB 110.3 . . C1S C2S H2SA 111.0 . . C1S C2S H2SB 111.0 . . C1S C2S C3S 103.7(3) . . H2SA C2S H2SB 109.0 . . C3S C2S H2SA 111.0 . . C3S C2S H2SB 111.0 . . C2S C3S H3SA 111.4 . . C2S C3S H3SB 111.4 . . H3SA C3S H3SB 109.2 . . C4S C3S C2S 102.1(3) . . C4S C3S H3SA 111.4 . . C4S C3S H3SB 111.4 . . O1S C4S C3S 103.6(3) . . O1S C4S H4SA 111.0 . . O1S C4S H4SB 111.0 . . C3S C4S H4SA 111.0 . . C3S C4S H4SB 111.0 . . H4SA C4S H4SB 109.0 . . O2S C5S H5SA 109.8 . . O2S C5S H5SB 109.8 . . O2S C5S C6S 109.5(5) . . H5SA C5S H5SB 108.2 . . C6S C5S H5SA 109.8 . . C6S C5S H5SB 109.8 . . C5S C6S C6S 101.8(4) . 3 C5S C6S H6SA 111.4 . . C5S C6S H6SB 111.4 . . C6S C6S H6SA 111.4 3 . C6S C6S H6SB 111.4 3 . H6SA C6S H6SB 109.3 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ir1 Cl1 2.4143(10) . Ir1 N1 2.108(3) . Ir1 C1 2.016(3) . Ir1 C14 2.166(4) . Ir1 C15 2.191(4) . Ir1 C16 2.212(3) . Ir1 C17 2.188(3) . Ir1 C18 2.164(3) . P1 F1 1.632(5) . P1 F2 1.583(4) . P1 F3 1.547(6) . P1 F4 1.624(4) . P1 F1B 1.512(11) . P1 F2B 1.720(12) . P1 F3B 1.699(14) . P1 F4B 1.429(15) . P1 F5 1.609(3) . P1 F6 1.607(3) . N1 C5 1.357(4) . N1 C9 1.354(4) . N2 C1 1.353(4) . N2 C3 1.397(4) . N2 C4 1.446(5) . N3 H3 0.8800 . N3 C1 1.348(5) . N3 C2 1.398(4) . C2 C3 1.342(5) . C2 C10 1.500(5) . C3 H3A 0.9500 . C4 H4A 0.9900 . C4 H4B 0.9900 . C4 C5 1.508(5) . C5 C6 1.380(5) . C6 H6 0.9500 . C6 C7 1.385(5) . C7 H7 0.9500 . C7 C8 1.379(5) . C8 H8 0.9500 . C8 C9 1.374(5) . C9 H9 0.9500 . C10 C11 1.518(6) . C10 C12 1.542(5) . C10 C13 1.531(5) . C11 H11A 0.9800 . C11 H11B 0.9800 . C11 H11C 0.9800 . C12 H12A 0.9800 . C12 H12B 0.9800 . C12 H12C 0.9800 . C13 H13A 0.9800 . C13 H13B 0.9800 . C13 H13C 0.9800 . C14 C15 1.442(5) . C14 C18 1.446(5) . C14 C19 1.495(5) . C15 C16 1.433(5) . C15 C20 1.480(5) . C16 C17 1.435(5) . C16 C21 1.506(5) . C17 C18 1.442(5) . C17 C22 1.482(5) . C18 C23 1.506(5) . C19 H19A 0.9800 . C19 H19B 0.9800 . C19 H19C 0.9800 . C20 H20A 0.9800 . C20 H20B 0.9800 . C20 H20C 0.9800 . C21 H21A 0.9800 . C21 H21B 0.9800 . C21 H21C 0.9800 . C22 H22A 0.9800 . C22 H22B 0.9800 . C22 H22C 0.9800 . C23 H23A 0.9800 . C23 H23B 0.9800 . C23 H23C 0.9800 . O1S C1S 1.435(4) . O1S C4S 1.432(4) . O2S C5S 1.410(6) 3 O2S C5S 1.410(6) . C1S H1SA 0.9900 . C1S H1SB 0.9900 . C1S C2S 1.523(6) . C2S H2SA 0.9900 . C2S H2SB 0.9900 . C2S C3S 1.538(5) . C3S H3SA 0.9900 . C3S H3SB 0.9900 . C3S C4S 1.507(6) . C4S H4SA 0.9900 . C4S H4SB 0.9900 . C5S H5SA 0.9900 . C5S H5SB 0.9900 . C5S C6S 1.479(7) . C6S C6S 1.543(12) 3 C6S H6SA 0.9900 . C6S H6SB 0.9900 . loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma -1 0 0 -0.18 0.18 1 0 0 -0.67 0.16 1 0 0 -0.63 0.17 2 0 0 1000 36.67 2 0 0 928.78 36.11 2 0 0 951.95 36.76 -2 0 0 970.02 36.72 3 0 0 -0.08 0.32 3 0 0 0.14 0.3 3 0 0 0.35 0.34 -3 0 0 0.08 0.31 -4 0 0 67.71 3.43 4 0 0 71.77 3.47 4 0 0 75.2 3.52 4 0 0 77.01 3.48 4 0 0 82.88 3.59 5 0 0 -0.63 0.4 -5 0 0 -0.24 0.38 5 0 0 0.1 0.44 5 0 0 -0.15 0.4 5 0 0 -0.35 0.37 5 0 0 -0.68 0.39 6 0 0 51.95 3.03 6 0 0 48.94 2.87 6 0 0 51.34 2.94 -6 0 0 50.01 2.83 6 0 0 52.36 2.9 7 0 0 -0.44 0.5 -7 0 0 -0.08 0.55 7 0 0 0.33 0.75 7 0 0 0.59 0.67 7 0 0 -0.85 0.47 8 0 0 4.23 1.15 8 0 0 5.49 1.22 8 0 0 4.57 1.13 -8 0 0 4.36 1.13 8 0 0 3.15 1.1 9 0 0 0.28 0.73 -9 0 0 -0.44 0.63 9 0 0 -0.74 0.68 9 0 0 -0.06 0.7 9 0 0 -0.01 0.62 10 0 0 114.79 6.33 -10 0 0 129.01 6.37 10 0 0 126.81 6.65 10 0 0 117.34 6.53 11 0 0 -1.29 0.7 -11 0 0 1.6 0.96 11 0 0 -0.12 0.91 11 0 0 0.27 0.97 12 0 0 77.65 5.12 12 0 0 66.67 4.91 12 0 0 85.31 5.11 13 0 0 -0.46 1.13 13 0 0 -0.37 1.3 13 0 0 3.16 1.36 14 0 0 61.68 4.87 14 0 0 53.67 4.8 14 0 0 71.73 5 15 0 0 1.63 1.58 15 0 0 0.82 1.49 -1 1 0 89.33 3.83 -1 -1 0 92.05 3.84 1 -1 0 99.51 3.85 1 -1 0 90.66 3.84 1 1 0 98.85 3.89 1 1 0 98.75 3.84 1 1 0 101.19 3.92 2 -1 0 0.09 0.23 2 -1 0 0.08 0.21 2 1 0 -0.04 0.22 -2 1 0 -0.27 0.18 2 1 0 0.03 0.25 2 1 0 0.32 0.28 2 -1 0 -0.24 0.23 2 -1 0 0.17 0.24 -2 -1 0 -0.04 0.21 -3 1 0 82.87 3.53 3 1 0 80.07 3.63 3 1 0 73.29 3.58 3 -1 0 77.71 3.51 -3 -1 0 83.58 3.53 3 1 0 78.05 3.54 3 1 0 81.21 3.57 -4 -1 0 -0.3 0.32 4 1 0 -0.24 0.37 4 -1 0 -0.26 0.35 4 1 0 -0.15 0.37 4 1 0 -0.47 0.32 4 -1 0 0.32 0.37 4 1 0 -0.3 0.34 4 -1 0 0.04 0.37 -4 1 0 -0.31 0.29 -5 -1 0 -0.32 0.37 5 1 0 0.79 0.48 -5 1 0 0.14 0.36 5 -1 0 0.37 0.47 5 1 0 -0.33 0.4 5 -1 0 0.68 0.49 5 1 0 -0.16 0.44 5 -1 0 1.64 0.55 5 1 0 0.04 0.43 6 -1 0 -0.72 0.41 6 1 0 0.42 0.53 6 1 0 -0.35 0.5 6 -1 0 -0.42 0.48 6 1 0 -0.52 0.41 -6 -1 0 0.06 0.48 6 1 0 -0.26 0.51 6 -1 0 0.15 0.55 -6 1 0 -0.18 0.46 7 1 0 2.87 0.87 7 -1 0 2.95 0.93 -7 1 0 2.65 0.81 7 -1 0 2.21 0.82 7 -1 0 2.33 0.87 7 1 0 2.18 0.85 7 1 0 1.96 0.84 7 -1 0 0.93 0.64 -7 -1 0 2.73 0.83 7 1 0 3.68 0.99 8 -1 0 0.05 0.64 -8 -1 0 -0.4 0.59 8 -1 0 -0.19 0.58 8 1 0 -0.77 0.66 -8 1 0 0.22 0.59 8 1 0 -0.35 0.69 8 -1 0 0.43 0.69 8 1 0 1.81 0.92 8 -1 0 0.23 0.75 9 -1 0 6.26 1.29 -9 1 0 4.56 1.19 9 1 0 6.53 1.34 9 -1 0 5.93 1.33 9 1 0 5.99 1.39 -9 -1 0 7.18 1.34 9 1 0 5.59 1.29 9 -1 0 4.18 1.22 9 -1 0 5.85 1.26 10 -1 0 -0.71 0.71 10 -1 0 -0.87 0.74 -10 -1 0 0.56 0.8 -10 1 0 -0.91 0.63 10 1 0 -0.4 0.7 10 -1 0 -0.97 0.6 10 1 0 -1.12 0.73 10 -1 0 -0.99 0.59 10 1 0 -0.4 0.76 11 -1 0 0.33 0.91 11 -1 0 -0.12 0.8 11 1 0 0.37 0.94 -11 1 0 1.57 0.93 11 -1 0 0.79 0.97 11 1 0 0.17 0.92 11 1 0 1.62 1.06 -11 -1 0 1.43 0.93 12 -1 0 0.67 1.04 12 -1 0 -0.88 0.98 12 -1 0 -1.18 0.95 12 1 0 -0.61 1.08 -12 1 0 0.13 0.82 12 1 0 -0.83 0.99 12 1 0 -1.15 0.83 13 -1 0 0.8 1.11 13 1 0 -0.96 1.13 13 -1 0 -1.55 1.12 13 -1 0 -0.26 1.15 13 1 0 2.84 1.4 13 1 0 1.29 1.42 14 1 0 -0.86 1.17 14 1 0 0.28 1.43 14 1 0 -0.09 1.4 14 -1 0 1.92 1.72 14 -1 0 -0.52 1.57 15 1 0 1.16 1.76 15 1 0 -0.32 1.48 15 -1 0 1.67 1.71 15 -1 0 -0.06 1.52 0 -2 0 642.97 24.89 0 2 0 681.49 24.96 0 -2 0 650.94 24.92 0 2 0 659.34 24.67 0 2 0 633.29 24.89 -1 2 0 0.05 0.15 -1 2 0 0.08 0.16 1 2 0 0.01 0.18 1 -2 0 0 0.16 1 -2 0 -0.05 0.14 1 -2 0 0.05 0.16 -1 -2 0 -0.12 0.16 1 2 0 0.17 0.19 1 2 0 0.86 0.22 2 -2 0 638.75 24.85 -2 -2 0 646.72 24.91 -2 2 0 658.77 24.9 2 -2 0 602.84 24.47 2 2 0 639.34 25.16 2 -2 0 670.07 24.94 2 2 0 642.46 24.71 2 -2 0 689 24.91 3 -2 0 -0.23 0.31 3 -2 0 0.08 0.33 3 2 0 0.39 0.34 3 2 0 -0.1 0.34 -3 -2 0 -0.14 0.28 -3 2 0 -0.18 0.25 3 2 0 0.18 0.36 3 -2 0 -0.01 0.3 3 -2 0 0.52 0.35 4 -2 0 89.15 4.09 4 -2 0 86.25 4.08 4 2 0 86.77 4.18 -4 2 0 92.89 4.08 -4 -2 0 88.47 4.07 4 2 0 92.45 4.24 4 -2 0 89.8 4.04 4 2 0 87.4 4.1 4 -2 0 92.01 4.1 5 -2 0 0.54 0.45 -5 -2 0 -0.59 0.31 5 2 0 -0.32 0.44 5 -2 0 -0.07 0.43 -5 2 0 0 0.4 5 -2 0 1.16 0.53 5 2 0 -0.58 0.35 5 2 0 0.11 0.48 5 -2 0 0.15 0.42 6 -2 0 0.62 0.54 6 -2 0 2.23 0.8 6 2 0 1.37 0.7 6 2 0 1.43 0.73 -6 -2 0 0.49 0.55 6 2 0 2.51 0.79 6 -2 0 2.24 0.74 -6 2 0 2.69 0.73 7 2 0 0.28 0.64 7 2 0 0.59 0.74 7 -2 0 0.54 0.65 7 2 0 1.16 0.72 7 -2 0 -0.43 0.57 7 -2 0 -0.7 0.51 -7 2 0 -0.8 0.41 -7 -2 0 -0.29 0.49 8 -2 0 51.74 3.2 8 -2 0 40.33 2.99 8 -2 0 43.86 3.07 -8 -2 0 46.95 3.03 8 2 0 45.75 3.11 8 2 0 49.95 3.35 8 2 0 49.94 3.31 -8 2 0 53.07 3.14 8 -2 0 48.48 3.15 9 2 0 -0.3 0.65 9 2 0 0.78 0.66 -9 -2 0 -0.45 0.71 -9 2 0 -0.02 0.79 9 -2 0 0.45 0.67 9 -2 0 -0.37 0.63 9 -2 0 -0.16 0.7 9 2 0 -0.43 0.68 9 -2 0 0.61 0.78 9 -2 0 -0.06 0.55 -10 -2 0 127.13 6.49 -10 2 0 137.19 6.54 10 2 0 117.01 6.65 10 2 0 114.03 6.44 10 -2 0 122.03 6.62 10 -2 0 113.71 6.49 10 -2 0 121.93 6.49 10 -2 0 140.22 6.7 10 2 0 130.32 6.81 11 -2 0 0.21 0.96 -11 -2 0 -0.21 0.79 11 -2 0 -0.04 0.86 -11 2 0 0.09 0.77 11 2 0 -0.81 0.88 11 -2 0 -0.24 0.78 11 2 0 -0.47 0.91 11 2 0 -0.06 0.84 11 -2 0 -0.11 0.75 12 -2 0 94.92 5.81 12 2 0 101.19 6.07 12 -2 0 103.39 6.12 12 -2 0 92.71 5.74 12 -2 0 99.62 6.01 -12 2 0 97.12 5.78 12 2 0 95.35 6.01 12 2 0 102.45 5.99 13 2 0 0.33 1.3 13 2 0 -0.93 1.05 13 -2 0 0.09 1.11 13 2 0 -0.34 1.02 13 -2 0 1.1 1.18 13 -2 0 0.58 1.23 14 2 0 59.22 4.8 14 2 0 52.15 4.57 14 2 0 48.16 4.48 14 -2 0 53.32 4.66 14 -2 0 57.42 4.72 15 2 0 0.06 1.74 15 -2 0 -1.96 1.29 15 2 0 -0.37 1.45 15 -2 0 0.83 1.81 0 -3 0 -0.41 0.22 0 3 0 -0.41 0.23 0 3 0 -0.4 0.24 0 -3 0 -0.32 0.22 0 3 0 0.16 0.27 -1 -3 0 38.01 1.77 1 3 0 38.33 1.81 1 3 0 39.62 1.86 -1 3 0 36.05 1.77 1 -3 0 38.53 1.78 -1 3 0 39.01 1.8 1 3 0 38.12 1.84 -1 3 0 38.67 1.77 1 -3 0 36.94 1.76 -2 -3 0 -0.09 0.28 -2 3 0 -0.1 0.25 2 -3 0 -0.11 0.27 2 3 0 0.49 0.34 2 -3 0 0.16 0.28 2 -3 0 -0.22 0.29 2 -3 0 0.1 0.28 2 3 0 -0.03 0.32 2 3 0 0.13 0.31 3 -3 0 3.09 0.58 3 3 0 2.02 0.54 3 -3 0 1.53 0.47 -3 3 0 2.37 0.5 3 -3 0 2.24 0.53 3 -3 0 2.67 0.57 -3 -3 0 2.27 0.52 3 3 0 2.72 0.58 3 3 0 1.64 0.55 4 3 0 -0.01 0.39 -4 3 0 0.2 0.37 4 -3 0 0.42 0.41 4 -3 0 0.08 0.36 4 3 0 -0.15 0.36 4 -3 0 -0.22 0.33 4 -3 0 0.17 0.44 4 3 0 -0.48 0.31 -4 -3 0 -0.22 0.35 5 3 0 16.95 1.51 5 -3 0 19.77 1.49 5 -3 0 17.39 1.45 5 -3 0 16.31 1.42 5 -3 0 16.67 1.43 5 3 0 17.6 1.52 -5 3 0 18.11 1.42 5 3 0 19.25 1.59 -5 -3 0 17.79 1.46 -6 -3 0 -0.15 0.49 -6 3 0 -0.1 0.46 6 -3 0 -0.17 0.45 6 3 0 -0.3 0.51 6 -3 0 -0.25 0.44 6 -3 0 -0.2 0.46 6 3 0 -0.51 0.53 6 3 0 -1.09 0.48 6 -3 0 -0.02 0.47 7 -3 0 6.75 1.2 7 3 0 3.66 1.01 7 -3 0 5.41 1.07 7 3 0 4.36 1.07 -7 3 0 4.63 0.98 7 3 0 4.99 1.13 -7 -3 0 4.25 0.99 7 -3 0 4.3 1.01 8 3 0 -0.46 0.65 8 -3 0 -0.19 0.66 -8 3 0 -0.23 0.55 8 -3 0 0.78 0.68 8 -3 0 -1.11 0.7 8 3 0 0.24 0.71 -8 -3 0 -0.22 0.62 8 3 0 -0.24 0.71 9 -3 0 -1.16 0.67 9 -3 0 -0.27 0.72 -9 -3 0 0.5 0.82 -9 3 0 -0.04 0.65 9 -3 0 0.33 0.8 9 3 0 0.08 0.68 9 3 0 -0.26 0.64 9 -3 0 0.65 0.72 9 3 0 -0.3 0.62 10 -3 0 0.47 0.8 -10 -3 0 0.85 1.01 10 -3 0 -1.08 0.64 10 3 0 0.28 0.88 10 3 0 -0.53 0.69 10 -3 0 -0.63 0.88 10 -3 0 0.44 0.77 10 3 0 0.42 0.83 -10 3 0 0.25 0.76 10 -3 0 0.58 0.81 11 -3 0 2.97 1.22 11 -3 0 0.9 0.95 11 3 0 2.98 1.24 -11 3 0 3.73 1.17 11 3 0 4.02 1.31 11 -3 0 1.58 1.03 11 3 0 1.61 1.08 11 -3 0 2.18 1.26 12 -3 0 -0.16 0.91 -12 3 0 0.1 0.95 12 -3 0 -0.59 1.06 12 3 0 -0.45 1.06 12 3 0 -0.6 1.1 12 -3 0 -1.03 0.76 12 3 0 -1.19 0.94 12 -3 0 0.19 0.95 13 3 0 -1.05 1.06 13 3 0 -0.9 1.21 13 3 0 0.62 1.11 13 -3 0 0.3 1.04 13 -3 0 -0.35 1.21 13 -3 0 0.66 1.33 14 -3 0 -1.45 1.25 14 -3 0 -2.16 1.29 14 3 0 0.87 1.52 14 3 0 -1.62 1.28 14 3 0 0.61 1.32 15 -3 0 -0.18 1.53 15 3 0 1.84 1.81 15 -3 0 2.26 1.77 15 3 0 1.41 1.71 0 4 0 91.17 3.93 0 4 0 97.31 3.98 0 -4 0 89.39 3.91 0 -4 0 92.95 3.9 0 4 0 95.33 3.93 1 -4 0 -0.16 0.27 1 4 0 -0.28 0.32 1 4 0 -1.1 0.24 -1 4 0 -0.39 0.26 -1 4 0 0.25 0.31 -1 -4 0 0.28 0.3 1 4 0 -0.18 0.29 1 -4 0 -0.38 0.26 -1 4 0 -0.05 0.29 2 4 0 32.27 1.76 2 -4 0 31.97 1.65 2 -4 0 30.77 1.6 2 4 0 30.86 1.73 2 -4 0 30.87 1.66 2 4 0 34.45 1.8 -2 -4 0 30.14 1.66 2 -4 0 29.11 1.63 -2 4 0 26.28 1.61 3 4 0 -0.34 0.33 3 -4 0 0.48 0.37 3 -4 0 0.05 0.33 3 4 0 0.57 0.4 3 4 0 -0.47 0.32 -3 4 0 0.4 0.33 3 -4 0 0.05 0.36 3 -4 0 0.12 0.36 -3 -4 0 -0.14 0.32 4 4 0 32.72 2.04 4 -4 0 32.05 1.94 4 -4 0 35.66 2.03 -4 4 0 34.49 1.97 4 4 0 31.96 2.11 4 -4 0 34.01 1.98 4 4 0 37.96 2.18 4 -4 0 30.07 1.93 -4 -4 0 32.09 1.96 -5 4 0 -0.02 0.43 5 -4 0 0.4 0.45 5 4 0 -0.58 0.44 5 -4 0 0.56 0.49 5 -4 0 0.32 0.44 -5 -4 0 0.23 0.48 5 4 0 0.22 0.55 5 4 0 -0.78 0.37 5 -4 0 0.15 0.46 6 -4 0 0.93 0.64 -6 4 0 2.83 0.73 6 4 0 1.9 0.78 6 -4 0 2.55 0.78 6 -4 0 1.35 0.68 6 -4 0 2.34 0.77 6 4 0 2.63 0.85 -6 -4 0 1.24 0.65 6 4 0 1.47 0.77 -7 -4 0 0.04 0.56 7 -4 0 -0.86 0.51 7 4 0 1.05 0.7 7 4 0 0.18 0.69 7 4 0 0.11 0.72 7 -4 0 0.59 0.65 7 -4 0 1.91 0.79 7 -4 0 -0.48 0.58 -7 4 0 -0.32 0.56 8 4 0 21.24 2.06 8 4 0 18.65 1.97 -8 4 0 20.5 1.89 8 -4 0 18.67 1.96 8 4 0 24.08 2.15 8 -4 0 22.72 2.02 -8 -4 0 23.01 2.02 8 -4 0 20.88 2.04 9 4 0 -0.16 0.79 9 4 0 -0.89 0.65 -9 -4 0 1.06 0.87 9 -4 0 0.41 0.75 -9 4 0 -0.38 0.58 9 -4 0 0.01 0.82 9 4 0 0.34 0.71 9 -4 0 -0.47 0.65 10 -4 0 135.73 7.03 10 -4 0 131.48 6.99 10 -4 0 143.87 7.04 10 4 0 142.87 7.39 10 4 0 137.57 7.21 10 -4 0 136.18 7.03 -10 4 0 140.87 7.04 -10 -4 0 138.48 7.06 10 4 0 144.77 7.41 11 -4 0 -0.1 0.8 11 4 0 -0.02 0.9 11 -4 0 0.21 0.82 11 4 0 -0.94 0.83 11 -4 0 0.08 0.91 11 -4 0 -0.61 0.81 11 4 0 -0.14 0.87 -11 4 0 0.14 0.86 12 4 0 119.27 7.04 12 -4 0 107.04 6.62 -12 4 0 121.74 6.62 12 -4 0 121.91 6.72 12 4 0 112.5 6.88 12 4 0 116.93 6.82 12 -4 0 124.55 6.75 12 -4 0 119.22 6.9 13 4 0 -0.76 1.13 13 -4 0 0.02 1.34 13 4 0 -0.54 1.11 13 4 0 1.37 1.32 13 -4 0 -0.9 1.04 13 -4 0 -0.25 1.09 14 -4 0 60.3 4.84 14 -4 0 50.75 4.57 14 4 0 53.28 4.54 14 4 0 55.74 4.74 14 4 0 57.53 4.99 15 4 0 1.73 1.9 15 -4 0 0.76 1.81 15 4 0 0.36 1.53 15 -4 0 -0.78 1.75 15 4 0 0.6 1.54 0 -5 0 0.11 0.32 0 5 0 0.02 0.3 0 5 0 -0.29 0.27 0 -5 0 -0.14 0.29 0 5 0 -0.44 0.27 1 -5 0 237.21 9.06 -1 -5 0 223.26 9.08 1 5 0 231.31 9.2 -1 5 0 228.46 9.14 -1 5 0 220.06 9.01 -1 5 0 225.23 9.07 1 -5 0 231.24 9.09 1 5 0 214.68 9.19 -2 -5 0 0.03 0.31 -2 5 0 0.58 0.36 2 5 0 -0.09 0.37 2 5 0 0.15 0.35 2 -5 0 -0.25 0.26 2 5 0 -0.06 0.34 -2 5 0 -0.02 0.3 2 -5 0 0.36 0.35 2 -5 0 -0.17 0.31 3 5 0 16.2 1.23 3 -5 0 13.21 1.08 -3 -5 0 12.79 1.17 3 5 0 14.58 1.24 -3 5 0 14.59 1.15 3 5 0 14.72 1.26 3 -5 0 14.97 1.16 3 -5 0 13.28 1.12 3 -5 0 14.2 1.12 4 5 0 0.1 0.5 4 5 0 -0.28 0.35 4 -5 0 -0.7 0.37 -4 -5 0 0.08 0.4 4 -5 0 0.14 0.37 4 -5 0 0.31 0.41 -4 5 0 0.39 0.37 4 5 0 -0.15 0.37 4 -5 0 -0.37 0.36 5 5 0 1.42 0.66 5 5 0 1.29 0.66 5 -5 0 1.23 0.58 -5 -5 0 1.86 0.63 5 5 0 1.79 0.71 5 -5 0 0.66 0.48 5 -5 0 0.62 0.48 -5 5 0 1.2 0.58 5 -5 0 1.55 0.61 6 -5 0 -0.33 0.55 6 5 0 -0.48 0.56 -6 -5 0 -0.06 0.48 6 -5 0 -0.18 0.46 6 -5 0 -0.28 0.46 6 5 0 -0.5 0.53 -6 5 0 -0.22 0.5 6 5 0 -0.65 0.53 6 -5 0 0.32 0.55 7 -5 0 3.09 0.89 7 5 0 4.72 1.14 -7 5 0 4.38 1 7 5 0 4.03 1.16 7 -5 0 3.53 1 7 5 0 3.64 1 -7 -5 0 3.58 0.91 7 -5 0 4.08 1.05 7 -5 0 4.03 0.95 8 -5 0 0.72 0.8 8 -5 0 0.18 0.74 8 -5 0 0.03 0.63 -8 5 0 -0.6 0.59 8 5 0 -0.01 0.59 8 -5 0 -0.27 0.54 8 5 0 0.08 0.69 8 5 0 -0.23 0.59 -8 -5 0 -0.26 0.65 9 -5 0 5.12 1.24 9 5 0 3.5 1.15 9 -5 0 5.35 1.28 -9 5 0 3.55 1.02 9 5 0 3.03 1.14 9 5 0 5.72 1.36 -9 -5 0 4.42 1.18 9 -5 0 5.53 1.25 10 5 0 -0.65 0.78 10 -5 0 -3 0.96 10 5 0 0.87 0.9 10 -5 0 0.92 0.85 10 5 0 0.28 0.85 -10 5 0 -0.8 0.57 10 -5 0 0.21 1.12 -10 -5 0 -0.97 0.85 11 -5 0 23.77 2.48 -11 5 0 23.87 2.4 11 5 0 23.16 2.66 11 5 0 28.66 2.76 11 5 0 26.1 2.83 11 -5 0 25.51 2.68 11 -5 0 29 2.65 12 -5 0 0.67 1.18 12 5 0 -0.67 1.03 12 -5 0 -0.29 0.99 12 -5 0 0.43 0.93 12 5 0 -0.03 1.04 12 -5 0 0.79 1 -12 5 0 -0.69 0.97 12 5 0 0.18 1.22 13 -5 0 3.89 1.55 13 5 0 1.97 1.51 13 -5 0 3.85 1.56 13 5 0 3.39 1.65 13 5 0 2.82 1.68 14 -5 0 0.09 1.33 14 5 0 -1.92 1.33 14 5 0 -0.13 1.35 14 5 0 -1.44 1.12 14 -5 0 0.09 1.23 15 -5 0 1.46 1.83 15 5 0 2.37 1.95 15 5 0 0.12 1.83 15 5 0 -1.56 1.63 0 6 0 659.96 26.29 0 -6 0 698.79 26.32 0 6 0 682.85 26.08 0 6 0 695.79 26.42 0 -6 0 662.42 26.26 -1 6 0 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7 -6 0 -0.97 0.56 -7 -6 0 -0.61 0.52 -7 6 0 -0.42 0.61 7 -6 0 -0.16 0.6 7 6 0 -0.16 0.73 7 6 0 1.32 0.78 7 -6 0 -0.97 0.38 8 6 0 11.17 1.78 8 6 0 12.04 1.59 -8 6 0 14.57 1.64 8 -6 0 7.97 1.4 8 -6 0 9.76 1.65 -8 -6 0 10.46 1.56 8 -6 0 10.11 1.59 8 6 0 9.96 1.65 8 -6 0 10.41 1.6 9 6 0 1.21 0.78 9 -6 0 -0.52 0.77 9 6 0 -0.47 0.63 9 -6 0 0.71 0.85 9 -6 0 0.79 0.73 -9 6 0 0.03 0.68 9 6 0 0.07 0.67 9 -6 0 -0.69 0.58 -9 -6 0 -0.15 0.78 10 -6 0 129.2 6.6 -10 6 0 121.18 6.48 10 6 0 135.11 7.04 10 6 0 118.99 6.66 10 -6 0 119.98 6.49 10 6 0 131.6 6.99 11 6 0 0.12 1.07 11 6 0 0.11 1.06 -11 6 0 -1.04 0.67 11 -6 0 -0.97 0.97 11 -6 0 0.91 0.98 11 6 0 0.5 0.91 -12 6 0 94.45 5.58 12 6 0 92.33 5.95 12 6 0 91 5.89 12 6 0 88.11 5.66 12 -6 0 80.2 5.34 12 -6 0 85.99 5.49 13 -6 0 -0.49 1.2 13 6 0 -0.9 1.24 13 -6 0 -0.25 1.18 13 6 0 0.89 1.49 13 6 0 -0.82 1.24 14 -6 0 55.49 4.67 14 6 0 53.86 4.83 14 6 0 59.64 4.92 14 -6 0 62.03 4.88 14 6 0 55.95 4.9 15 -6 0 0.28 1.57 15 6 0 -0.27 1.61 15 6 0 1.45 1.78 15 6 0 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0.55 -6 -7 0 0.26 0.59 6 -7 0 -0.13 0.5 6 -7 0 -0.22 0.56 7 -7 0 3.4 1 7 -7 0 2.76 0.88 7 7 0 1.8 0.85 -7 -7 0 3.06 0.97 7 7 0 3.51 1.01 7 7 0 4.36 1.17 7 -7 0 2.81 0.93 -7 7 0 3.07 0.88 7 -7 0 3.39 0.97 -8 -7 0 -0.48 0.67 8 7 0 -0.09 0.67 8 -7 0 -0.37 0.8 8 -7 0 -0.51 0.68 8 7 0 0.34 0.85 8 7 0 0.14 0.58 -8 7 0 0.73 0.61 8 -7 0 0.46 0.81 8 -7 0 -0.11 0.63 9 7 0 0.9 0.82 -9 7 0 -0.19 0.57 9 7 0 0.6 0.8 9 -7 0 1.52 1 9 -7 0 0.61 0.89 9 -7 0 2.16 0.97 9 7 0 1.66 0.9 10 7 0 0.29 1.02 10 -7 0 -0.65 0.71 10 7 0 0.45 0.93 -10 7 0 0.09 0.66 10 -7 0 0.22 0.81 10 7 0 0.55 1.09 11 -7 0 3.65 1.24 11 7 0 3.66 1.44 -11 7 0 1.68 0.98 11 -7 0 2.93 1.25 11 7 0 2.92 1.39 11 7 0 4.26 1.6 -12 7 0 -0.45 0.98 12 7 0 -1.17 0.92 12 7 0 -0.38 1.09 12 7 0 0.07 1.09 12 -7 0 0.05 1.04 13 -7 0 3.09 1.63 13 7 0 3.81 1.68 13 7 0 1.89 1.69 13 7 0 3.54 1.7 13 -7 0 2.45 1.43 14 -7 0 0.28 1.36 14 7 0 -1.74 1.39 14 7 0 -0.67 1.56 14 7 0 -0.81 1.12 15 7 0 9.81 2.59 0 -8 0 312.23 12.42 0 -8 0 309.98 12.38 0 8 0 318.75 12.54 0 8 0 300.94 12.34 0 8 0 296.4 12.4 -1 -8 0 -0.08 0.38 1 8 0 0.03 0.38 -1 8 0 0.04 0.35 1 -8 0 -0.47 0.32 1 8 0 -0.18 0.42 -1 -8 0 -0.69 0.34 1 -8 0 -0.29 0.37 -1 8 0 0.06 0.37 1 8 0 -0.36 0.36 -1 8 0 -0.39 0.38 -2 8 0 395.34 15.07 -2 -8 0 398.04 15.17 2 -8 0 379.24 15.11 -2 8 0 364.53 15.09 2 8 0 365.88 15.33 -2 8 0 359.04 15.18 2 -8 0 387.69 15.11 2 8 0 376.96 15.32 2 8 0 372.5 15.09 3 -8 0 0.05 0.45 -3 8 0 0.52 0.47 3 -8 0 -0.3 0.42 3 8 0 0.18 0.46 3 -8 0 -0.34 0.42 -3 8 0 -0.01 0.43 -3 -8 0 0.84 0.52 3 8 0 -0.09 0.44 3 8 0 -0.09 0.38 4 8 0 90.94 4.61 4 -8 0 92.58 4.43 4 8 0 93.95 4.67 4 -8 0 90.55 4.3 4 -8 0 92.01 4.38 4 -8 0 87.46 4.38 -4 8 0 88.74 4.41 4 8 0 89.1 4.54 -4 -8 0 95.26 4.48 5 -8 0 0.19 0.58 -5 8 0 -0.39 0.46 5 -8 0 -0.2 0.54 5 -8 0 0.04 0.52 -5 -8 0 -0.3 0.52 5 8 0 -0.24 0.46 5 8 0 0.18 0.61 5 8 0 -0.69 0.52 5 -8 0 -0.27 0.47 6 8 0 55.53 3.56 6 -8 0 58.56 3.37 6 8 0 56.21 3.45 -6 -8 0 60.73 3.4 -6 8 0 56.97 3.31 6 -8 0 59.63 3.3 6 -8 0 60.27 3.39 6 8 0 50.7 3.45 6 -8 0 56.97 3.32 -7 -8 0 -0.12 0.63 7 -8 0 0.7 0.68 7 8 0 0.23 0.63 7 -8 0 -0.85 0.5 7 8 0 -0.84 0.58 7 -8 0 0.58 0.77 7 8 0 -0.09 0.62 7 -8 0 -0.25 0.7 -7 8 0 -0.76 0.55 8 -8 0 2.9 1.03 8 -8 0 2.26 1.02 8 -8 0 2.34 1 8 8 0 3.19 1.07 8 8 0 3.36 1.12 8 8 0 1.91 0.98 -8 8 0 4.64 1.18 8 -8 0 4.25 1.12 -8 -8 0 7.74 1.46 9 -8 0 0.64 0.83 -9 8 0 -0.04 0.69 9 8 0 -0.85 0.77 9 -8 0 0.5 0.74 9 8 0 0.44 0.93 9 8 0 0.05 0.82 10 8 0 90.78 5.56 10 8 0 89.32 5.64 -10 8 0 93.16 5.31 10 -8 0 97.45 5.42 10 8 0 92.64 5.72 10 -8 0 93.57 5.28 -11 8 0 -0.79 0.78 11 -8 0 0.89 1.09 11 -8 0 -0.35 0.77 11 8 0 0.31 1.06 11 8 0 -0.34 0.89 11 8 0 -0.84 0.93 -12 8 0 71.16 4.79 12 8 0 66.25 5.1 12 8 0 77.07 5.21 12 -8 0 72.06 4.75 12 8 0 65.76 5.08 -13 8 0 -1.37 1.02 13 8 0 -1.44 1.18 13 8 0 -0.66 1.43 13 -8 0 -0.24 1.12 13 8 0 -1.37 1.06 14 8 0 47.28 4.57 14 8 0 55.47 4.71 14 -8 0 41.37 3.97 14 -8 0 46.89 4.28 14 8 0 47.4 4.38 15 8 0 1.18 1.9 0 9 0 -0.31 0.34 0 9 0 -0.38 0.42 0 9 0 0.15 0.49 0 -9 0 -0.32 0.35 0 -9 0 -0.17 0.44 -1 9 0 107.87 5.15 -1 9 0 121.37 5.35 1 9 0 118 5.27 1 -9 0 113.53 5.18 -1 9 0 110.31 5.17 -1 -9 0 116.1 5.17 1 9 0 113 5.2 1 -9 0 115.87 5.18 -1 -9 0 114.95 5.2 -2 -9 0 0.07 0.44 -2 9 0 0.38 0.47 2 -9 0 0.05 0.43 2 9 0 -0.06 0.5 2 9 0 0.19 0.43 -2 9 0 -0.22 0.35 2 -9 0 0.37 0.44 -2 9 0 0.43 0.44 -2 -9 0 -0.38 0.4 2 9 0 -0.64 0.4 3 9 0 2.38 0.75 3 9 0 3.35 0.92 3 -9 0 3.68 0.82 -3 9 0 3.16 0.82 3 9 0 2.82 0.83 -3 -9 0 2.83 0.71 3 -9 0 2.65 0.71 -3 9 0 3.06 0.79 3 -9 0 3.18 0.78 4 9 0 -0.82 0.43 4 -9 0 -0.22 0.46 4 -9 0 -0.77 0.37 4 9 0 0.11 0.63 4 9 0 -0.13 0.5 4 -9 0 -0.32 0.41 -4 9 0 0.22 0.52 -4 -9 0 0.06 0.48 4 -9 0 0.05 0.48 -5 -9 0 1.59 0.71 5 9 0 1.71 0.82 5 -9 0 1.71 0.67 5 -9 0 0.31 0.59 5 9 0 1.26 0.74 5 -9 0 0.72 0.61 -5 9 0 1.79 0.78 5 -9 0 0.23 0.6 5 9 0 1.02 0.72 6 9 0 0.25 0.67 -6 -9 0 -0.02 0.67 6 9 0 0.13 0.54 6 -9 0 -0.2 0.61 -6 9 0 0.29 0.63 6 -9 0 -0.23 0.56 6 -9 0 0.87 0.64 6 9 0 0.27 0.57 6 -9 0 0.42 0.68 -7 -9 0 3.71 1.1 7 -9 0 5.75 1.22 7 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