#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:35:14 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242518 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132558.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_4132558 loop_ _publ_author_name 'Lai, Po-Ni' 'Brysacz, Caroline H.' 'Alam, Md Kamrul' 'Ayoub, Nicholas A.' 'Gray, Thomas G.' 'Bao, Jiming' 'Teets, Thomas S.' _publ_section_title ; Highly Efficient Red-Emitting Bis-Cyclometalated Iridium Complexes. ; _journal_issue 32 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 10198 _journal_page_last 10207 _journal_paper_doi 10.1021/jacs.8b04841 _journal_volume 140 _journal_year 2018 _chemical_formula_sum 'C40 H37 Cl2 Ir N4 S2' _chemical_formula_weight 900.95 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 102.2146(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.2791(8) _cell_length_b 21.2737(13) _cell_length_c 13.2932(13) _cell_measurement_reflns_used 4426 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.25 _cell_measurement_theta_min 2.19 _cell_volume 3670.3(5) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_unetI/netI 0.0354 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 11375 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.588 _diffrn_reflns_theta_min 1.838 _exptl_absorpt_coefficient_mu 3.932 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6244 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.630 _exptl_crystal_description Block _exptl_crystal_F_000 1792 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.020 _refine_diff_density_max 1.094 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.099 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 226 _refine_ls_number_reflns 4250 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.016 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0259 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+7.7179P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.0609 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3159 _reflns_number_total 4250 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04841_si_002.cif _cod_data_source_block 6 _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 4132558 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.590 _shelx_estimated_absorpt_t_max 0.925 _shelx_res_file ; bl15.res created by SHELXL-2014/7 TITL BL15 in C2/c CELL 0.71073 13.27910 21.27370 13.29321 90.0000 102.2146 90.0000 ZERR 4.00 0.00080 0.00130 0.00128 0.0000 0.0006 0.0000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N S IR CL UNIT 160 148 16 8 4 8 TEMP -100.000 SIZE 0.02 0.10 0.15 L.S. 16 BOND FMAP 2 PLAN 20 simu c1s cl1s delu c1s cl1s 1 acta WGHT 0.024700 7.717900 FVAR 0.05063 CL1S 6 -0.000110 0.439591 0.856318 11.00000 0.13280 0.18352 = 0.16808 0.03174 0.03939 -0.06962 S1 4 0.218625 0.384087 1.145463 11.00000 0.03943 0.02906 = 0.03909 -0.00160 0.01955 -0.01179 IR1 5 0.000000 0.249140 1.250000 10.50000 0.01863 0.01363 = 0.01953 0.00000 0.00438 0.00000 N1 3 0.005155 0.248216 1.097279 11.00000 0.02616 0.01808 = 0.02044 -0.00256 0.00558 0.00236 N2 3 -0.083879 0.161470 1.238216 11.00000 0.01818 0.01348 = 0.02889 0.00072 0.00624 -0.00069 C1 1 0.000000 0.126426 1.250000 10.50000 0.02575 0.01264 = 0.02389 0.00000 0.00778 0.00000 C1S 1 0.000000 0.485722 0.750000 10.50000 0.04281 0.02585 = 0.21571 0.00000 0.00817 0.00000 AFIX 23 H1S1 2 -0.061752 0.513041 0.736888 10.50000 -1.20000 H1S2 2 0.061754 0.513040 0.763111 10.50000 -1.20000 AFIX 0 C12 1 -0.051598 0.210435 1.025613 11.00000 0.02721 0.02043 = 0.03045 -0.00179 0.00361 0.00269 AFIX 43 H12 2 -0.104228 0.185571 1.044217 11.00000 -1.20000 AFIX 0 C13 1 -0.036340 0.206450 0.926609 11.00000 0.04569 0.03476 = 0.02440 -0.00802 0.00209 0.00482 AFIX 43 H13 2 -0.078116 0.179623 0.877773 11.00000 -1.20000 AFIX 0 C14 1 0.040710 0.242082 0.899316 11.00000 0.05463 0.05130 = 0.02560 -0.00397 0.01580 0.00097 AFIX 43 H14 2 0.054117 0.238950 0.832073 11.00000 -1.20000 AFIX 0 C15 1 0.097821 0.282150 0.970543 11.00000 0.04304 0.03751 = 0.03343 0.00120 0.01741 -0.00534 AFIX 43 H15 2 0.149710 0.307691 0.952012 11.00000 -1.20000 AFIX 0 C16 1 0.079559 0.285235 1.069573 11.00000 0.02835 0.02339 = 0.02677 0.00413 0.01010 0.00294 C17 1 0.130193 0.324131 1.153301 11.00000 0.02386 0.02100 = 0.03161 0.00158 0.01139 -0.00325 C20 1 0.103305 0.317991 1.246584 11.00000 0.02279 0.01694 = 0.02367 0.00207 0.00606 0.00182 C21 1 0.155628 0.365024 1.317961 11.00000 0.02180 0.01735 = 0.02728 0.00140 0.00205 -0.00056 C22 1 0.147420 0.377516 1.419014 11.00000 0.03642 0.02593 = 0.02831 0.00147 0.00185 -0.01147 AFIX 43 H22 2 0.106019 0.351183 1.451465 11.00000 -1.20000 AFIX 0 C23 1 0.198606 0.427493 1.471951 11.00000 0.05317 0.03263 = 0.02717 -0.00283 0.00097 -0.01168 AFIX 43 H23 2 0.192159 0.435685 1.540558 11.00000 -1.20000 AFIX 0 C24 1 0.260221 0.466377 1.425131 11.00000 0.04053 0.02360 = 0.03741 -0.00319 -0.00405 -0.01162 AFIX 43 H24 2 0.294995 0.500883 1.462566 11.00000 -1.20000 AFIX 0 C25 1 0.271581 0.455715 1.325850 11.00000 0.02737 0.02392 = 0.04722 0.00149 0.00416 -0.00843 AFIX 43 H25 2 0.313622 0.482272 1.294532 11.00000 -1.20000 AFIX 0 C26 1 0.219413 0.404692 1.272709 11.00000 0.02834 0.02002 = 0.03256 0.00063 0.00869 -0.00023 C31 1 0.000000 0.055773 1.250000 10.50000 0.02282 0.01398 = 0.03179 0.00000 0.01285 0.00000 C32 1 -0.037223 0.022951 1.158994 11.00000 0.02416 0.02142 = 0.02992 0.00065 0.00670 0.00135 AFIX 43 H32 2 -0.063109 0.045123 1.096871 11.00000 -1.20000 AFIX 0 C33 1 -0.036281 -0.042644 1.159573 11.00000 0.02656 0.02435 = 0.03250 -0.00890 0.00870 -0.00252 AFIX 43 H33 2 -0.060713 -0.065141 1.097470 11.00000 -1.20000 AFIX 0 C34 1 0.000000 -0.074967 1.250000 10.50000 0.03393 0.02056 = 0.04460 0.00000 0.01682 0.00000 AFIX 43 H34 2 0.000002 -0.119623 1.250002 10.50000 -1.20000 AFIX 0 C41 1 -0.184979 0.138293 1.248732 11.00000 0.02144 0.01519 = 0.04361 -0.00475 0.00879 -0.00342 AFIX 13 H41 2 -0.197053 0.096708 1.213146 11.00000 -1.20000 AFIX 0 C42 1 -0.190153 0.128764 1.361991 11.00000 0.03624 0.03259 = 0.04793 -0.00493 0.02380 -0.00571 AFIX 137 H42A 2 -0.135653 0.099693 1.394470 11.00000 -1.50000 H42B 2 -0.257464 0.111247 1.365939 11.00000 -1.50000 H42C 2 -0.180644 0.169267 1.397870 11.00000 -1.50000 AFIX 0 C43 1 -0.268122 0.183493 1.195486 11.00000 0.02035 0.03096 = 0.06635 -0.00293 0.00379 0.00074 AFIX 137 H43A 2 -0.259719 0.224029 1.231309 11.00000 -1.50000 H43B 2 -0.336136 0.166099 1.196940 11.00000 -1.50000 H43C 2 -0.262075 0.189471 1.123904 11.00000 -1.50000 AFIX 0 HKLF 4 REM BL15 in C2/c REM R1 = 0.0259 for 3159 Fo > 4sig(Fo) and 0.0412 for all 4250 data REM 226 parameters refined using 7 restraints END WGHT 0.0247 7.7063 REM Highest difference peak 1.094, deepest hole -0.901, 1-sigma level 0.099 Q1 1 0.0325 0.2508 1.1829 11.00000 0.05 1.09 Q2 1 -0.0769 0.2510 1.2317 11.00000 0.05 1.02 Q3 1 0.0207 0.4307 0.8827 11.00000 0.05 0.92 Q4 1 -0.0362 0.2501 1.1764 11.00000 0.05 0.92 Q5 1 0.0032 0.4172 0.8319 11.00000 0.05 0.81 Q6 1 -0.0576 0.4649 0.8504 11.00000 0.05 0.81 Q7 1 0.0363 0.2920 1.2186 11.00000 0.05 0.69 Q8 1 0.0324 0.2075 1.2182 11.00000 0.05 0.53 Q9 1 0.0231 0.2790 1.0760 11.00000 0.05 0.49 Q10 1 0.0256 0.4608 0.8122 11.00000 0.05 0.45 Q11 1 -0.0215 -0.0633 1.1211 11.00000 0.05 0.43 Q12 1 0.2374 0.3884 1.2036 11.00000 0.05 0.40 Q13 1 0.1762 0.2873 0.9674 11.00000 0.05 0.38 Q14 1 -0.1369 0.1578 1.2315 11.00000 0.05 0.37 Q15 1 -0.1517 0.1554 1.4366 11.00000 0.05 0.36 Q16 1 0.2400 0.4298 1.4378 11.00000 0.05 0.35 Q17 1 -0.2211 0.1238 1.2988 11.00000 0.05 0.35 Q18 1 -0.0057 -0.0077 1.1565 11.00000 0.05 0.34 Q19 1 0.1031 0.2501 0.9459 11.00000 0.05 0.34 Q20 1 0.0246 0.3102 0.7987 11.00000 0.05 0.33 ; _shelx_res_checksum 96467 _shelx_hkl_file ; -2 0 2 136.26 2.89 -2 0 2 138.85 2.89 2 0 -2 133.09 2.84 -4 0 4 120.44 2.84 -4 0 4 120.73 2.83 4 0 -4 124.07 2.79 -6 0 6 130.64 3.27 -6 0 6 136.69 3.36 6 0 -6 138.78 3.28 8 0 -8 28.72 1.30 -8 0 8 29.58 1.30 -8 0 8 27.10 1.34 -10 0 10 82.53 2.72 -12 0 12 40.46 2.01 -1 1 1 396.65 7.70 1 1 -1 387.99 7.67 -1 -1 1 384.45 7.74 -1 -1 1 389.70 7.67 1 -1 -1 400.23 7.70 -3 1 3 241.78 4.98 3 1 -3 238.13 4.89 -3 1 3 233.24 4.86 3 -1 -3 239.29 4.93 -3 -1 3 234.59 4.95 -3 -1 3 235.04 5.02 -5 1 5 145.64 3.43 -5 1 5 144.17 3.31 5 1 -5 144.81 3.32 -5 -1 5 140.68 3.44 -5 -1 5 146.04 3.40 5 -1 -5 147.44 3.38 7 1 -7 77.61 2.22 -7 1 7 77.86 2.19 -7 1 7 79.07 2.34 -7 -1 7 83.61 2.34 -7 -1 7 74.96 2.29 7 -1 -7 77.01 2.26 -9 1 9 48.11 1.92 9 -1 -9 49.64 1.93 -9 -1 9 52.08 1.91 -9 -1 9 51.48 1.94 -11 1 11 33.92 1.77 -11 -1 11 37.26 1.81 -13 1 13 30.46 1.89 -13 -1 13 31.53 1.88 0 -2 0 292.44 5.53 0 -2 0 266.82 5.52 -2 2 2 5.65 0.38 2 2 -2 6.24 0.36 2 -2 -2 6.42 0.40 -2 -2 2 6.04 0.37 -2 -2 2 6.13 0.49 4 2 -4 110.16 2.53 -4 2 4 109.74 2.64 -4 2 4 111.30 2.45 -4 -2 4 109.71 2.60 4 -2 -4 108.40 2.60 -4 -2 4 111.21 2.74 -6 2 6 93.87 2.30 6 2 -6 92.83 2.37 -6 2 6 90.41 2.51 -6 -2 6 91.51 2.56 6 -2 -6 92.66 2.48 -6 -2 6 89.35 2.44 8 2 -8 100.56 2.74 -8 2 8 93.73 2.84 -8 -2 8 101.94 2.84 -8 -2 8 98.49 2.87 8 -2 -8 99.89 2.86 -10 2 10 39.13 1.81 -10 -2 10 39.29 1.75 -12 2 12 28.29 1.74 -12 -2 12 26.89 1.65 -1 3 1 171.45 3.59 -1 -3 1 172.23 3.59 1 -3 -1 182.02 3.68 -1 -3 1 181.13 3.74 -3 3 3 39.06 1.15 3 3 -3 39.78 1.08 3 -3 -3 39.39 1.16 -3 -3 3 38.71 1.27 -3 -3 3 38.48 1.08 -5 3 5 126.21 3.04 -5 3 5 123.85 2.73 5 3 -5 122.43 2.87 -5 -3 5 118.32 3.12 -5 -3 5 122.56 2.93 5 -3 -5 122.34 3.01 -7 3 7 104.78 2.84 7 3 -7 95.60 2.60 -7 3 7 99.57 2.48 -7 -3 7 101.89 2.71 7 -3 -7 101.50 2.79 -7 -3 7 97.51 2.83 -9 3 9 16.58 1.18 -9 -3 9 18.46 1.22 9 -3 -9 15.93 1.17 -9 -3 9 18.09 1.14 -11 3 11 43.52 2.03 -11 -3 11 45.17 1.96 -13 3 13 19.06 1.68 -13 -3 13 20.57 1.64 0 -4 0 122.16 2.68 0 -4 0 128.21 2.69 -2 4 2 256.77 5.29 -2 -4 2 253.02 5.50 -2 -4 2 254.93 5.24 2 -4 -2 267.87 5.40 4 4 -4 90.48 2.15 -4 4 4 89.45 2.27 -4 -4 4 89.71 2.45 4 -4 -4 92.54 2.30 -4 -4 4 88.19 2.17 -6 4 6 42.71 1.17 6 4 -6 39.27 1.33 -6 4 6 42.20 1.51 -6 -4 6 42.51 1.42 6 -4 -6 41.34 1.48 -6 -4 6 42.85 1.62 -8 4 8 120.61 3.41 -8 -4 8 121.92 3.29 8 -4 -8 128.74 3.44 -8 -4 8 123.43 3.50 -10 4 10 16.64 1.31 -10 -4 10 17.27 1.30 10 -4 -10 16.44 1.40 -10 -4 10 16.60 1.19 -12 4 12 14.21 1.38 -12 -4 12 14.14 1.29 -1 5 1 51.62 1.26 1 -5 -1 52.76 1.40 -1 -5 1 52.95 1.46 1 -5 -1 54.81 1.25 -1 -5 1 51.38 1.31 -3 5 3 97.64 2.34 3 5 -3 96.63 2.24 -3 -5 3 97.99 2.58 3 -5 -3 104.69 2.45 -5 5 5 281.13 6.18 5 5 -5 281.75 6.00 -5 -5 5 285.86 6.42 -5 -5 5 284.36 6.03 5 -5 -5 284.56 6.22 -7 5 7 108.16 3.01 7 5 -7 108.78 2.76 -7 -5 7 106.90 2.84 7 -5 -7 112.42 3.05 -7 -5 7 104.90 3.14 -9 5 9 20.43 1.29 -9 -5 9 18.83 1.14 9 -5 -9 17.94 1.23 -9 -5 9 19.19 1.34 -11 5 11 38.11 1.96 -11 -5 11 41.53 1.87 -13 5 13 17.58 1.66 0 -6 0 260.25 5.51 0 -6 0 269.82 5.53 -2 6 2 180.82 3.93 -2 -6 2 182.18 3.95 2 -6 -2 194.08 4.11 -4 6 4 95.20 2.39 4 6 -4 96.14 2.28 -4 -6 4 92.91 2.24 4 -6 -4 94.60 2.48 -4 -6 4 93.27 2.65 6 6 -6 189.23 4.24 -6 -6 6 188.42 4.30 6 -6 -6 190.05 4.54 -6 -6 6 187.13 4.71 -8 6 8 72.81 2.42 -8 -6 8 70.73 2.23 8 -6 -8 74.64 2.46 -8 -6 8 77.18 2.60 -10 6 10 47.78 2.07 -10 -6 10 42.99 1.82 -10 -6 10 45.25 2.07 10 -6 -10 44.96 2.06 -12 6 12 26.43 1.79 -1 -7 1 84.71 2.21 1 -7 -1 84.42 2.14 1 -7 -1 89.89 2.03 -1 -7 1 83.38 2.06 -3 7 3 256.69 5.51 -3 -7 3 258.48 5.49 3 -7 -3 265.73 5.70 -3 -7 3 262.74 5.88 -5 7 5 102.12 2.68 5 7 -5 103.08 2.51 -5 -7 5 100.32 2.49 5 -7 -5 104.58 2.79 -5 -7 5 102.34 2.97 -7 7 7 132.32 3.57 7 -7 -7 137.47 3.68 -7 -7 7 133.35 3.81 -7 -7 7 137.92 3.38 -9 7 9 45.41 1.94 9 -7 -9 45.74 2.00 -9 -7 9 46.36 2.08 -9 -7 9 44.45 1.75 -11 7 11 14.91 1.44 -11 -7 11 18.07 1.58 -13 7 13 18.69 1.66 0 -8 0 170.83 3.76 0 -8 0 162.00 3.73 -2 8 2 123.75 2.85 2 -8 -2 124.51 3.07 -2 -8 2 124.40 2.92 -2 -8 2 129.65 3.22 2 -8 -2 131.84 2.77 -4 8 4 88.21 2.28 -4 -8 4 86.20 2.20 -4 -8 4 84.78 2.59 4 -8 -4 88.62 2.42 6 8 -6 196.94 4.41 -6 8 6 194.17 4.65 -6 -8 6 192.71 4.41 6 -8 -6 198.99 4.78 -6 -8 6 193.55 4.98 -8 8 8 26.18 1.41 -8 -8 8 28.15 1.28 8 -8 -8 29.05 1.52 -8 -8 8 27.73 1.61 -10 8 10 33.64 1.77 10 -8 -10 34.51 1.87 -10 -8 10 36.39 1.97 -12 8 12 33.25 1.97 1 -9 -1 217.30 4.87 -1 -9 1 216.00 4.78 -1 -9 1 221.69 4.97 1 -9 -1 220.30 4.73 -3 9 3 167.61 3.83 -3 -9 3 174.65 4.26 -3 -9 3 171.57 3.87 3 -9 -3 170.13 4.05 5 9 -5 68.28 1.88 -5 9 5 71.13 2.03 5 -9 -5 68.16 2.16 -5 -9 5 67.93 1.82 -5 -9 5 67.07 2.34 -7 9 7 64.13 2.13 -7 -9 7 58.12 2.31 -7 -9 7 59.52 1.87 7 -9 -7 59.59 2.17 -9 9 9 40.86 1.86 -9 -9 9 40.15 2.03 9 -9 -9 39.94 1.91 -11 9 11 27.55 1.74 -11 -9 11 30.18 1.94 11 -9 -11 30.06 1.87 0 -10 0 203.44 4.62 0 -10 0 205.49 4.64 -2 -10 2 270.86 6.10 2 -10 -2 260.17 5.93 2 -10 -2 275.24 5.63 -2 -10 2 263.90 5.78 -4 10 4 50.59 1.60 -4 -10 4 53.03 1.99 -4 -10 4 51.76 1.59 4 -10 -4 53.80 1.80 -6 10 6 57.17 1.88 6 10 -6 55.37 1.77 -6 -10 6 54.07 1.65 6 -10 -6 54.38 2.01 -6 -10 6 56.23 2.22 -8 10 8 58.94 2.14 8 -10 -8 52.86 2.20 -8 -10 8 58.25 2.44 -10 10 10 28.35 1.70 -10 -10 10 32.14 1.96 10 -10 -10 31.55 1.86 -12 10 12 27.14 1.91 -12 -10 12 26.11 1.96 -1 -11 1 135.02 3.35 -1 -11 1 143.96 3.55 1 -11 -1 137.55 3.44 1 -11 -1 138.98 3.32 -3 11 3 38.92 1.26 -3 -11 3 38.86 1.33 3 -11 -3 36.59 1.44 -3 -11 3 38.99 1.63 -5 11 5 164.42 3.91 5 11 -5 161.16 3.76 -5 -11 5 158.93 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46.39 1.86 -8 -4 10 51.58 2.06 8 -4 -10 47.67 1.88 -10 4 12 45.46 2.09 -10 -4 12 45.23 1.99 -12 4 14 8.17 1.16 -12 -4 14 8.44 1.15 -13 5 11 17.62 1.56 -11 5 9 18.95 1.37 11 -5 -9 18.60 1.53 -11 -5 9 20.50 1.43 -11 -5 9 21.09 1.26 -9 5 7 99.84 2.95 9 5 -7 99.32 2.83 9 -5 -7 93.46 3.02 -9 -5 7 96.90 3.05 -9 -5 7 102.18 2.77 -7 5 5 130.94 3.23 7 5 -5 122.04 3.16 -7 -5 5 120.55 3.38 7 -5 -5 127.44 3.34 -7 -5 5 124.70 3.03 -5 5 3 184.59 4.17 5 5 -3 186.54 4.21 5 -5 -3 188.02 4.31 -5 -5 3 185.09 4.43 -5 -5 3 189.70 3.99 -3 -5 1 91.10 2.35 -3 -5 1 93.84 1.92 -3 -5 1 92.23 2.25 3 -5 -1 94.57 2.29 3 -5 -1 93.37 2.04 1 5 1 2.93 0.18 1 -5 1 2.42 0.28 -1 -5 -1 2.75 0.31 1 -5 1 3.36 0.33 -1 -5 -1 2.93 0.34 -1 5 3 211.83 4.34 1 -5 -3 208.48 4.44 -1 -5 3 195.81 4.47 -1 -5 3 206.04 4.16 -3 5 5 166.80 3.84 3 5 -5 166.10 3.46 3 -5 -5 171.31 3.83 -3 -5 5 162.62 3.96 5 5 -7 98.90 2.31 -5 5 7 98.23 2.74 -5 -5 7 100.80 2.64 5 -5 -7 101.24 2.68 -5 -5 7 98.80 2.88 -7 5 9 80.53 2.58 -7 -5 9 78.36 2.44 7 -5 -9 81.71 2.51 -7 -5 9 80.47 2.70 -9 5 11 31.58 1.71 -9 -5 11 30.92 1.58 -9 -5 11 36.64 1.84 -11 5 13 26.89 1.79 -11 -5 13 26.73 1.67 -14 6 12 21.66 1.83 -12 6 10 32.52 1.81 12 -6 -10 31.63 1.92 -12 -6 10 32.09 1.85 -10 6 8 54.75 2.11 -10 -6 8 57.61 2.26 -10 -6 8 52.78 1.89 10 -6 -8 49.92 2.17 -8 6 6 67.06 2.19 8 6 -6 70.64 2.14 8 -6 -6 71.77 2.36 -8 -6 6 70.71 2.04 -8 -6 6 68.16 2.39 -6 6 4 85.67 2.33 6 6 -4 89.94 2.36 -6 -6 4 85.34 2.59 6 -6 -4 88.64 2.48 -6 -6 4 83.55 2.14 -4 6 2 249.51 5.42 4 -6 -2 262.35 5.19 4 -6 -2 266.49 5.62 -4 -6 2 257.02 5.18 -4 -6 2 245.43 5.70 -4 -6 2 255.39 5.51 -2 -6 0 283.55 5.87 2 -6 0 280.49 5.66 -2 -6 0 266.07 5.80 2 -6 0 274.88 5.80 0 6 2 51.59 1.23 0 -6 2 50.52 1.29 0 -6 -2 52.37 1.26 0 -6 2 49.71 1.42 0 -6 -2 50.92 1.43 -2 6 4 62.71 1.65 -2 -6 4 58.83 1.41 2 -6 -4 63.27 1.74 -2 -6 4 58.71 1.79 4 6 -6 82.85 1.91 -4 6 6 82.36 2.29 -4 -6 6 79.49 2.46 4 -6 -6 85.10 2.30 -6 6 8 138.37 3.73 6 -6 -8 148.48 3.74 -6 -6 8 145.48 3.62 -6 -6 8 140.46 3.93 -8 6 10 45.80 1.96 -8 -6 10 47.90 2.11 8 -6 -10 47.14 1.95 -8 -6 10 48.01 1.84 -10 6 12 32.72 1.83 -10 -6 12 33.49 2.15 -10 -6 12 32.86 1.74 -12 6 14 14.42 1.59 -13 7 11 31.14 1.91 -11 7 9 34.99 1.78 -11 -7 9 30.92 1.82 11 -7 -9 29.72 1.79 -9 7 7 44.22 1.80 -9 -7 7 44.51 1.61 -9 -7 7 44.42 1.96 9 -7 -7 40.84 1.86 7 7 -5 205.44 4.69 -7 7 5 194.29 4.71 7 -7 -5 205.90 4.91 -7 -7 5 199.50 4.47 -7 -7 5 197.31 5.03 -5 7 3 43.53 1.39 5 7 -3 42.46 1.39 5 -7 -3 42.88 1.50 -5 -7 3 43.09 1.17 3 -7 -1 166.18 3.85 3 -7 -1 172.25 3.56 -3 -7 1 169.90 3.97 -3 -7 1 166.22 3.80 1 7 1 361.05 7.26 -1 -7 -1 356.43 7.64 -1 -7 -1 383.18 7.59 1 -7 1 368.05 7.56 1 -7 1 374.67 7.57 -1 7 3 12.42 0.55 1 -7 -3 10.19 0.63 -1 -7 3 11.42 0.50 -3 7 5 133.34 3.23 3 7 -5 134.34 2.91 3 -7 -5 144.10 3.35 -3 -7 5 129.65 3.43 -5 7 7 114.06 3.12 -5 -7 7 119.23 3.02 -5 -7 7 117.94 3.39 5 -7 -7 122.45 3.17 -7 7 9 21.18 1.28 -7 -7 9 23.55 1.50 7 -7 -9 22.18 1.30 -7 -7 9 22.14 1.20 -9 7 11 46.44 2.07 -9 -7 11 49.10 2.26 -9 -7 11 44.04 1.90 -11 7 13 25.04 1.77 -12 8 10 23.75 1.62 -12 -8 10 22.71 1.71 12 -8 -10 23.31 1.78 -10 8 8 62.56 2.36 10 -8 -8 65.73 2.53 -10 -8 8 61.56 2.52 8 8 -6 65.82 2.08 -8 8 6 63.82 2.15 -8 -8 6 67.51 2.44 -8 -8 6 65.42 1.92 8 -8 -6 63.16 2.28 -6 8 4 102.71 2.77 6 8 -4 107.83 2.80 -6 -8 4 109.05 3.15 6 -8 -4 111.39 2.99 -6 -8 4 107.64 2.52 -4 8 2 190.35 4.29 4 -8 -2 190.02 4.47 -4 -8 2 195.62 4.65 4 -8 -2 195.21 4.03 -4 -8 2 195.38 4.40 -4 -8 2 197.37 3.97 2 -8 0 56.18 1.61 -2 -8 0 58.60 1.70 -2 -8 0 54.06 1.61 2 -8 0 56.54 1.48 0 8 2 166.66 3.50 0 -8 2 166.53 3.66 0 -8 -2 161.55 3.81 0 -8 2 167.43 3.81 0 -8 -2 172.04 3.61 -2 8 4 207.72 4.59 -2 -8 4 210.16 4.45 2 -8 -4 213.91 4.80 -2 -8 4 212.40 4.91 -4 8 6 75.94 2.16 4 8 -6 75.84 1.82 -4 -8 6 71.42 2.38 4 -8 -6 75.21 2.24 -6 8 8 114.74 3.21 -6 -8 8 112.33 3.46 6 -8 -8 113.52 3.24 -6 -8 8 117.53 3.07 -8 8 10 27.21 1.51 8 -8 -10 25.00 1.49 -8 -8 10 23.63 1.33 -8 -8 10 29.26 1.75 -10 8 12 18.13 1.52 -10 -8 12 16.09 1.57 -10 -8 12 13.81 1.27 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1.77 -10 -10 8 40.03 2.07 10 -10 -8 34.89 1.93 -8 10 6 78.40 2.46 8 10 -6 73.09 2.37 8 -10 -6 75.85 2.63 -8 -10 6 83.48 2.86 -6 10 4 59.57 1.89 6 10 -4 60.91 1.91 6 -10 -4 62.46 2.11 -6 -10 4 63.54 2.28 -6 -10 4 62.74 1.61 -4 -10 2 100.78 2.17 4 -10 -2 101.48 2.32 -4 -10 2 103.68 2.70 4 -10 -2 98.50 2.75 -4 -10 2 104.70 2.95 2 -10 0 249.04 5.56 -2 -10 0 245.97 5.55 -2 -10 0 253.77 5.65 2 -10 0 255.27 5.40 0 10 2 187.60 4.03 0 -10 -2 201.93 4.23 0 -10 2 191.07 4.43 0 -10 -2 192.69 4.46 0 -10 2 188.44 4.28 -2 10 4 59.44 1.68 2 -10 -4 60.80 1.93 -2 -10 4 60.52 2.01 -2 -10 4 61.56 1.64 -4 10 6 115.60 3.01 4 -10 -6 121.17 3.23 -4 -10 6 113.46 3.39 -6 10 8 68.49 2.26 -6 -10 8 66.74 2.09 -6 -10 8 66.52 2.58 6 -10 -8 63.37 2.29 -8 10 10 27.36 1.57 -8 -10 10 27.06 1.40 -8 -10 10 28.58 1.86 8 -10 -10 26.02 1.60 -10 10 12 30.06 1.85 -10 -10 12 29.34 2.00 -13 11 11 11.19 1.36 13 -11 -11 12.69 1.62 -13 -11 11 9.37 1.40 -11 11 9 42.29 2.06 -11 -11 9 45.12 2.32 11 -11 -9 45.92 2.28 -9 11 7 49.09 1.98 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52.19 1.77 6 -12 -4 50.89 1.95 -6 -12 4 52.68 2.14 4 -12 -2 43.52 1.69 4 -12 -2 47.05 1.33 -4 -12 2 46.65 1.85 -4 -12 2 43.61 1.60 -2 -12 0 175.49 4.31 2 -12 0 178.98 4.31 -2 -12 0 185.26 4.42 2 -12 0 181.98 4.15 0 -12 2 164.57 4.00 0 -12 2 157.11 3.84 0 -12 -2 162.59 4.02 0 -12 -2 164.98 3.77 -2 12 4 36.57 1.22 -2 -12 4 36.55 1.25 2 -12 -4 37.28 1.52 -2 -12 4 36.01 1.58 -4 12 6 129.06 3.33 4 -12 -6 131.36 3.60 -4 -12 6 130.56 3.85 -6 12 8 34.92 1.57 -6 -12 8 30.43 1.84 6 -12 -8 30.33 1.61 -6 -12 8 33.57 1.60 -8 12 10 45.50 2.06 8 -12 -10 43.95 2.13 -8 -12 10 46.90 2.39 -10 12 12 35.59 2.00 -10 -12 12 34.61 2.26 10 -12 -12 30.80 2.37 -11 13 9 23.00 1.60 -11 -13 9 26.56 1.93 11 -13 -9 23.39 1.80 -9 13 7 33.54 1.67 -9 -13 7 35.99 2.04 9 -13 -7 35.82 1.90 -7 13 5 42.38 1.70 7 13 -5 44.48 1.70 7 -13 -5 44.69 1.93 -7 -13 5 43.23 2.07 -5 -13 3 72.45 2.26 -5 -13 3 68.44 2.50 5 -13 -3 71.67 2.39 3 -13 -1 120.38 3.26 -3 -13 1 118.85 3.39 -3 -13 1 118.05 3.20 3 -13 -1 127.41 2.99 1 -13 1 140.55 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1.86 10 -2 8 29.35 1.84 8 2 10 18.47 1.64 8 -2 10 19.15 1.70 6 2 12 35.56 1.95 6 -2 12 34.84 1.98 4 2 14 23.89 1.65 4 -2 14 21.66 1.70 2 -2 16 9.80 1.34 15 3 3 11.42 1.56 15 -3 3 16.71 1.79 13 3 5 30.73 2.08 13 -3 5 27.55 1.91 11 3 7 46.30 2.40 11 -3 7 46.51 2.29 9 3 9 14.62 1.52 9 -3 9 16.84 1.64 7 -3 11 21.93 1.63 5 3 13 32.53 1.85 5 -3 13 31.11 1.93 3 -3 15 12.85 1.52 16 4 2 21.58 2.09 16 -4 2 17.72 1.86 14 4 4 31.97 2.17 14 -4 4 28.14 2.02 12 4 6 24.52 2.08 12 -4 6 23.80 1.98 10 4 8 29.24 1.93 10 -4 8 31.53 1.95 10 -4 8 31.15 1.83 8 4 10 28.45 1.86 8 -4 10 24.58 1.72 6 4 12 20.16 1.50 6 -4 12 16.07 1.54 4 -4 14 22.50 1.74 2 4 16 10.24 1.37 2 -4 16 8.10 1.29 15 5 3 13.33 1.64 15 -5 3 13.04 1.64 13 5 5 34.22 2.18 13 -5 5 32.39 2.06 11 5 7 24.13 1.84 11 -5 7 25.85 1.75 9 5 9 23.33 1.77 9 -5 9 23.30 1.70 7 5 11 20.64 2.39 7 -5 11 24.39 1.71 5 5 13 31.15 1.82 5 -5 13 31.37 1.98 3 5 15 23.52 1.92 3 -5 15 24.60 1.84 14 6 4 20.87 2.03 14 -6 4 18.82 1.80 12 6 6 28.36 2.00 12 -6 6 25.24 1.81 10 6 8 16.73 1.67 10 -6 8 18.32 1.74 8 6 10 25.99 1.83 8 -6 10 28.35 1.83 6 -6 12 41.50 2.22 4 -6 14 35.05 2.13 15 7 3 24.13 2.21 15 -7 3 29.00 2.15 13 7 5 21.36 1.95 13 -7 5 21.24 1.84 11 7 7 26.78 2.22 11 -7 7 27.67 1.74 11 -7 7 25.74 1.85 9 7 9 28.95 1.96 9 -7 9 30.20 1.94 7 7 11 24.26 1.74 7 -7 11 24.88 1.80 5 -7 13 36.73 2.15 3 7 15 29.24 1.95 3 -7 15 29.50 2.06 14 8 4 14.67 1.71 14 -8 4 17.88 1.84 12 8 6 28.22 2.03 12 -8 6 29.02 1.97 12 -8 6 38.47 2.09 10 8 8 27.52 1.97 10 -8 8 24.36 1.82 8 8 10 18.26 1.70 8 -8 10 23.92 1.78 6 -8 12 46.85 2.41 4 -8 14 17.42 1.74 15 9 3 19.21 1.99 15 -9 3 19.15 1.96 15 -9 3 15.07 1.64 13 -9 5 20.56 1.87 13 -9 5 17.45 1.75 11 9 7 44.64 2.45 11 -9 7 44.11 2.37 9 9 9 33.94 2.12 9 -9 9 35.70 2.13 7 9 11 22.48 1.72 7 -9 11 22.90 1.79 5 -9 13 25.39 1.90 3 -9 15 12.02 1.58 14 10 4 19.71 1.97 14 -10 4 22.82 2.07 14 -10 4 21.01 1.84 12 10 6 25.67 2.20 12 -10 6 23.22 1.75 12 -10 6 25.82 1.89 10 10 8 38.23 2.30 10 -10 8 35.72 2.16 8 10 10 33.84 2.04 8 -10 10 27.14 1.89 6 10 12 16.95 1.68 6 -10 12 18.65 1.78 4 -10 14 25.10 2.24 13 11 5 15.92 1.79 13 -11 5 15.52 1.62 13 -11 5 18.15 1.76 11 11 7 32.14 2.18 11 -11 7 30.26 2.01 9 11 9 17.77 1.79 9 -11 9 13.38 1.56 7 11 11 22.10 1.92 7 -11 11 20.03 1.90 5 -11 13 25.23 1.94 12 12 6 21.89 2.15 12 -12 6 20.12 1.88 10 12 8 22.01 1.94 10 -12 8 16.92 1.68 8 12 10 20.18 1.85 8 -12 10 19.13 1.83 6 12 12 12.15 1.54 6 -12 12 10.45 1.40 13 13 5 19.76 2.01 13 -13 5 20.69 1.92 13 -13 5 21.19 1.93 11 13 7 23.20 2.15 11 -13 7 24.74 1.92 9 13 9 20.95 1.99 9 -13 9 20.75 1.91 7 13 11 14.28 1.63 7 -13 11 13.46 1.64 5 -13 13 6.95 1.32 12 14 6 20.42 2.04 12 -14 6 24.60 1.88 10 14 8 21.79 2.03 10 -14 8 19.52 1.86 8 14 10 19.26 1.89 8 -14 10 19.17 1.91 -6 -14 -12 10.33 1.46 6 -14 12 11.75 1.55 9 15 9 26.48 2.31 9 -15 9 28.18 2.01 16 0 3 0.54 0.79 14 0 5 -0.35 0.71 12 0 7 1.32 0.79 10 0 9 2.49 0.83 8 0 11 0.38 0.60 6 0 13 -0.20 0.54 4 0 15 0.10 0.69 15 1 4 1.89 0.93 15 -1 4 0.23 0.76 13 1 6 0.13 0.72 13 -1 6 -0.33 0.73 11 1 8 2.17 0.83 11 -1 8 3.44 0.94 9 -1 10 3.42 0.90 7 1 12 0.79 0.68 7 -1 12 0.51 0.62 5 1 14 0.69 0.69 5 -1 14 0.95 0.70 3 -1 16 0.99 0.81 14 2 5 1.42 0.88 14 -2 5 1.45 0.88 12 2 7 0.70 0.73 12 -2 7 0.11 0.69 10 2 9 0.55 0.72 10 -2 9 -0.07 0.72 8 -2 11 0.43 0.66 6 2 13 0.94 0.62 6 -2 13 1.49 0.78 4 2 15 0.73 0.74 4 -2 15 0.17 0.67 15 3 4 -0.85 0.69 15 -3 4 0.46 0.80 13 3 6 -0.63 0.69 13 -3 6 0.31 0.75 11 3 8 0.48 0.74 11 -3 8 -0.70 0.56 9 3 10 0.18 0.65 9 -3 10 1.33 0.71 7 3 12 0.22 0.60 7 -3 12 0.60 0.69 5 3 14 0.61 0.69 5 -3 14 0.37 0.70 14 4 5 1.56 0.89 14 -4 5 0.65 0.77 12 4 7 0.28 0.69 12 -4 7 -0.15 0.64 10 4 9 -0.32 0.62 10 -4 9 -0.13 0.59 8 -4 11 -0.01 0.58 6 4 13 -0.47 0.56 6 -4 13 -0.46 0.63 4 -4 15 0.17 0.68 15 5 4 0.69 0.85 15 -5 4 2.04 0.99 13 5 6 0.51 0.76 13 -5 6 1.79 0.87 11 5 8 -0.27 0.65 11 -5 8 0.50 0.72 11 -5 8 -0.33 0.55 9 5 10 -1.54 0.54 9 -5 10 -0.83 0.58 7 -5 12 0.32 0.69 5 -5 14 -0.10 0.70 14 6 5 0.01 0.76 14 -6 5 -1.14 0.58 12 6 7 0.56 0.75 12 -6 7 0.02 0.70 12 -6 7 -0.53 0.66 10 6 9 -0.57 0.63 10 -6 9 0.03 0.66 8 6 11 -0.18 0.64 8 -6 11 0.36 0.71 6 6 13 0.11 0.57 6 -6 13 0.56 0.78 4 6 15 0.01 0.69 4 -6 15 -0.22 0.73 15 7 4 1.89 0.99 15 -7 4 1.73 0.91 13 7 6 -0.60 0.69 13 -7 6 0.70 0.72 13 -7 6 -0.60 0.66 11 7 8 0.18 0.71 11 -7 8 1.51 0.83 9 7 10 0.05 0.71 9 -7 10 0.82 0.71 7 -7 12 2.84 0.88 5 -7 14 -0.12 0.66 14 8 5 -0.37 0.73 14 -8 5 1.36 0.82 14 -8 5 -0.32 0.73 12 8 7 0.55 0.82 12 -8 7 0.19 0.73 12 -8 7 -0.78 0.58 10 8 9 1.19 0.79 10 -8 9 0.83 0.72 8 8 11 1.58 0.82 8 -8 11 0.96 0.72 6 -8 13 1.40 0.81 13 9 6 0.78 0.84 13 -9 6 0.53 0.79 13 -9 6 -0.29 0.66 11 9 8 0.18 0.78 11 -9 8 -0.48 0.66 9 9 10 1.21 0.82 9 -9 10 0.14 0.65 7 -9 12 0.11 0.70 5 -9 14 0.87 0.84 12 10 7 -0.77 0.73 12 -10 7 0.64 0.80 10 10 9 -0.52 0.67 10 -10 9 0.09 0.70 8 10 11 0.53 0.79 8 -10 11 -0.46 0.68 6 -10 13 1.36 0.89 13 11 6 1.33 0.96 13 -11 6 1.82 0.86 13 -11 6 0.87 0.85 11 11 8 2.13 0.97 11 -11 8 0.37 0.71 9 11 10 1.35 0.83 9 -11 10 1.75 0.84 7 11 12 -0.35 0.77 7 -11 12 -0.94 0.66 12 12 7 -0.73 0.80 12 -12 7 -0.43 0.73 10 12 9 -0.35 0.72 10 -12 9 -0.38 0.69 8 12 11 0.23 0.79 8 -12 11 -0.72 0.61 11 13 8 -0.42 0.83 11 -13 8 0.59 0.77 9 13 10 0.08 0.78 9 -13 10 2.47 0.97 14 0 6 21.05 1.99 12 0 8 33.00 2.18 8 0 12 27.92 1.90 6 0 14 16.14 1.65 15 1 5 16.20 1.84 15 -1 5 13.97 1.73 13 1 7 34.11 2.25 13 -1 7 34.19 2.22 11 1 9 18.14 1.81 11 -1 9 16.98 1.69 9 1 11 36.95 2.17 9 -1 11 34.28 2.11 7 1 13 27.11 1.83 7 -1 13 26.38 1.85 5 1 15 12.33 1.49 5 -1 15 10.30 1.41 14 2 6 18.51 1.92 14 -2 6 16.64 1.81 12 2 8 20.09 1.93 12 -2 8 21.27 1.90 10 2 10 28.89 2.07 10 -2 10 30.48 2.02 8 2 12 24.45 1.80 8 -2 12 25.56 1.85 6 2 14 18.58 1.73 6 -2 14 16.92 1.75 15 3 5 18.89 2.04 15 -3 5 17.61 1.93 13 3 7 20.10 1.96 13 -3 7 19.55 1.90 11 3 9 22.61 1.97 11 -3 9 22.02 2.03 7 3 13 13.48 1.51 7 -3 13 10.58 1.38 5 -3 15 18.53 1.89 14 4 6 23.72 2.16 14 -4 6 25.14 2.22 12 4 8 20.33 1.97 12 -4 8 20.10 1.84 10 4 10 9.93 1.39 10 -4 10 15.07 1.69 8 4 12 17.49 1.70 8 -4 12 19.11 1.81 6 4 14 16.32 1.60 6 -4 14 12.28 1.50 13 5 7 27.78 2.12 13 -5 7 23.95 2.10 11 5 9 15.21 1.75 11 -5 9 16.51 1.76 9 -5 11 13.27 1.54 7 5 13 26.67 1.84 7 -5 13 23.35 2.05 14 6 6 18.75 2.05 14 -6 6 22.39 2.03 12 6 8 22.98 2.08 12 -6 8 25.67 1.99 10 6 10 17.51 1.87 10 -6 10 19.06 1.90 8 -6 12 17.87 1.79 6 -6 14 20.28 1.91 13 7 7 22.64 2.18 13 -7 7 24.54 2.12 13 -7 7 27.16 1.96 11 7 9 16.16 1.82 11 -7 9 18.05 1.83 9 7 11 13.10 1.64 9 -7 11 14.39 1.70 7 7 13 26.92 1.90 7 -7 13 31.36 2.15 12 8 8 18.52 1.98 12 -8 8 19.96 1.90 10 8 10 18.36 1.87 10 -8 10 22.07 1.97 8 -8 12 12.02 1.56 11 9 9 18.72 1.95 11 -9 9 22.33 2.02 9 9 11 11.68 1.52 9 -9 11 12.22 1.56 12 10 8 22.35 2.14 12 -10 8 16.74 1.84 10 10 10 12.98 1.66 10 -10 10 12.75 1.58 8 10 12 19.85 1.99 8 -10 12 15.67 1.76 12 0 9 0.91 0.87 10 0 11 -0.59 0.65 8 0 13 -0.42 0.63 13 1 8 0.72 0.84 13 -1 8 -1.01 0.62 11 -1 10 1.27 0.86 9 1 12 1.18 0.82 9 -1 12 0.68 0.73 12 2 9 0.83 0.86 10 -2 11 1.32 0.85 8 2 13 0.64 0.72 8 -2 13 0.12 0.70 13 3 8 0.16 0.83 13 -3 8 0.43 0.77 11 3 10 1.12 0.85 11 -3 10 -0.73 0.65 9 3 12 0.71 0.75 9 -3 12 1.38 0.85 12 4 9 1.20 0.87 12 -4 9 -0.78 0.68 10 -4 11 -0.56 0.66 8 4 13 0.04 0.68 8 -4 13 0.02 0.76 11 5 10 2.32 0.92 11 -5 10 0.02 0.75 9 -5 12 -0.55 0.63 12 6 9 -0.08 0.84 12 -6 9 1.20 0.88 10 6 11 0.73 1.00 10 -6 11 0.53 0.78 11 7 10 0.28 0.87 11 -7 10 0.49 0.79 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 15299 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Cl1S Cl -0.0001(2) 0.43959(14) 0.8563(2) 0.1603(11) Uani 1 1 d . U . S1 S 0.21863(8) 0.38409(5) 1.14546(8) 0.0342(2) Uani 1 1 d . . . Ir1 Ir 0.0000 0.24914(2) 1.2500 0.01722(6) Uani 1 2 d S T P N1 N 0.0052(2) 0.24822(13) 1.0973(2) 0.0215(5) Uani 1 1 d . . . N2 N -0.0839(2) 0.16147(12) 1.2382(2) 0.0200(6) Uani 1 1 d . . . C1 C 0.0000 0.1264(2) 1.2500 0.0204(10) Uani 1 2 d S T P C1S C 0.0000 0.4857(3) 0.7500 0.098(4) Uani 1 2 d S TU P H1S1 H -0.0618 0.5130 0.7369 0.117 Uiso 0.5 1 calc R U P H1S2 H 0.0618 0.5130 0.7631 0.117 Uiso 0.5 1 calc R U P C12 C -0.0516(3) 0.21043(16) 1.0256(3) 0.0264(8) Uani 1 1 d . . . H12 H -0.1042 0.1856 1.0442 0.032 Uiso 1 1 calc R U . C13 C -0.0363(3) 0.20645(18) 0.9266(3) 0.0357(9) Uani 1 1 d . . . H13 H -0.0781 0.1796 0.8778 0.043 Uiso 1 1 calc R U . C14 C 0.0407(4) 0.24208(19) 0.8993(3) 0.0428(11) Uani 1 1 d . . . H14 H 0.0541 0.2389 0.8321 0.051 Uiso 1 1 calc R U . C15 C 0.0978(3) 0.28215(19) 0.9705(3) 0.0366(9) Uani 1 1 d . . . H15 H 0.1497 0.3077 0.9520 0.044 Uiso 1 1 calc R U . C16 C 0.0796(3) 0.28523(16) 1.0696(3) 0.0255(8) Uani 1 1 d . . . C17 C 0.1302(3) 0.32413(16) 1.1533(3) 0.0247(8) Uani 1 1 d . . . C20 C 0.1033(3) 0.31799(15) 1.2466(3) 0.0210(7) Uani 1 1 d . . . C21 C 0.1556(3) 0.36502(15) 1.3180(3) 0.0226(7) Uani 1 1 d . . . C22 C 0.1474(3) 0.37752(17) 1.4190(3) 0.0310(8) Uani 1 1 d . . . H22 H 0.1060 0.3512 1.4515 0.037 Uiso 1 1 calc R U . C23 C 0.1986(4) 0.42749(18) 1.4720(3) 0.0388(10) Uani 1 1 d . . . H23 H 0.1922 0.4357 1.5406 0.047 Uiso 1 1 calc R U . C24 C 0.2602(3) 0.46638(17) 1.4251(3) 0.0357(9) Uani 1 1 d . . . H24 H 0.2950 0.5009 1.4626 0.043 Uiso 1 1 calc R U . C25 C 0.2716(3) 0.45572(17) 1.3258(3) 0.0334(9) Uani 1 1 d . . . H25 H 0.3136 0.4823 1.2945 0.040 Uiso 1 1 calc R U . C26 C 0.2194(3) 0.40469(16) 1.2727(3) 0.0266(8) Uani 1 1 d . . . C31 C 0.0000 0.0558(2) 1.2500 0.0218(10) Uani 1 2 d S T P C32 C -0.0372(3) 0.02295(16) 1.1590(3) 0.0250(7) Uani 1 1 d . . . H32 H -0.0631 0.0451 1.0969 0.030 Uiso 1 1 calc R U . C33 C -0.0363(3) -0.04264(16) 1.1596(3) 0.0274(8) Uani 1 1 d . . . H33 H -0.0607 -0.0651 1.0975 0.033 Uiso 1 1 calc R U . C34 C 0.0000 -0.0750(2) 1.2500 0.0318(12) Uani 1 2 d S T P H34 H 0.0000 -0.1196 1.2500 0.038 Uiso 1 2 calc R U P C41 C -0.1850(3) 0.13829(15) 1.2487(3) 0.0265(8) Uani 1 1 d . . . H41 H -0.1971 0.0967 1.2131 0.032 Uiso 1 1 calc R U . C42 C -0.1902(3) 0.12876(18) 1.3620(3) 0.0367(10) Uani 1 1 d . . . H42A H -0.1357 0.0997 1.3945 0.055 Uiso 1 1 calc R U . H42B H -0.2575 0.1112 1.3659 0.055 Uiso 1 1 calc R U . H42C H -0.1806 0.1693 1.3979 0.055 Uiso 1 1 calc R U . C43 C -0.2681(3) 0.18349(18) 1.1955(4) 0.0400(10) Uani 1 1 d . . . H43A H -0.2597 0.2240 1.2313 0.060 Uiso 1 1 calc R U . H43B H -0.3361 0.1661 1.1969 0.060 Uiso 1 1 calc R U . H43C H -0.2621 0.1895 1.1239 0.060 Uiso 1 1 calc R U . 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 Cl1S 0.133(2) 0.184(3) 0.168(2) 0.032(2) 0.0394(19) -0.0696(19) S1 0.0394(6) 0.0291(5) 0.0391(6) -0.0016(4) 0.0196(5) -0.0118(4) Ir1 0.01863(9) 0.01363(9) 0.01953(9) 0.000 0.00438(6) 0.000 N1 0.0262(14) 0.0181(13) 0.0204(13) -0.0026(13) 0.0056(11) 0.0024(13) N2 0.0182(15) 0.0135(13) 0.0289(16) 0.0007(11) 0.0062(12) -0.0007(11) C1 0.026(3) 0.013(2) 0.024(2) 0.000 0.008(2) 0.000 C1S 0.043(5) 0.026(4) 0.216(12) 0.000 0.008(6) 0.000 C12 0.027(2) 0.0204(17) 0.030(2) -0.0018(15) 0.0036(16) 0.0027(14) C13 0.046(3) 0.035(2) 0.024(2) -0.0080(17) 0.0021(18) 0.0048(18) C14 0.055(3) 0.051(3) 0.026(2) -0.0040(19) 0.0158(19) 0.001(2) C15 0.043(3) 0.038(2) 0.033(2) 0.0012(18) 0.0174(19) -0.0053(19) C16 0.028(2) 0.0234(19) 0.0268(19) 0.0041(15) 0.0101(16) 0.0029(15) C17 0.0239(19) 0.0210(17) 0.032(2) 0.0016(15) 0.0114(16) -0.0033(14) C20 0.0228(18) 0.0169(16) 0.0237(18) 0.0021(13) 0.0061(14) 0.0018(13) C21 0.0218(18) 0.0173(16) 0.0273(19) 0.0014(14) 0.0020(14) -0.0006(13) C22 0.036(2) 0.0259(19) 0.028(2) 0.0015(15) 0.0018(17) -0.0115(16) C23 0.053(3) 0.033(2) 0.027(2) -0.0028(17) 0.0010(19) -0.0117(19) C24 0.041(2) 0.0236(19) 0.037(2) -0.0032(17) -0.0041(18) -0.0116(16) C25 0.027(2) 0.0239(19) 0.047(3) 0.0015(17) 0.0042(18) -0.0084(15) C26 0.028(2) 0.0200(18) 0.033(2) 0.0006(15) 0.0087(16) -0.0002(14) C31 0.023(3) 0.014(2) 0.032(3) 0.000 0.013(2) 0.000 C32 0.0242(19) 0.0214(17) 0.030(2) 0.0006(14) 0.0067(15) 0.0013(14) C33 0.027(2) 0.0244(18) 0.032(2) -0.0089(15) 0.0087(16) -0.0025(15) C34 0.034(3) 0.021(3) 0.045(3) 0.000 0.017(3) 0.000 C41 0.0214(18) 0.0152(17) 0.044(2) -0.0047(15) 0.0088(16) -0.0034(13) C42 0.036(2) 0.033(2) 0.048(3) -0.0049(18) 0.024(2) -0.0057(18) C43 0.020(2) 0.031(2) 0.066(3) -0.003(2) 0.0038(19) 0.0007(16) 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 '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' 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 C26 S1 C17 89.53(17) . . C20 Ir1 C20 86.67(18) . 2_557 C20 Ir1 N1 79.55(12) . . C20 Ir1 N1 101.26(12) 2_557 . C20 Ir1 N1 101.27(12) . 2_557 C20 Ir1 N1 79.55(12) 2_557 2_557 N1 Ir1 N1 178.90(15) . 2_557 C20 Ir1 N2 165.74(11) . . C20 Ir1 N2 106.63(12) 2_557 . N1 Ir1 N2 92.56(11) . . N1 Ir1 N2 86.48(11) 2_557 . C20 Ir1 N2 106.63(12) . 2_557 C20 Ir1 N2 165.74(11) 2_557 2_557 N1 Ir1 N2 86.49(10) . 2_557 N1 Ir1 N2 92.56(11) 2_557 2_557 N2 Ir1 N2 60.67(14) . 2_557 C20 Ir1 C1 136.66(9) . . C20 Ir1 C1 136.66(9) 2_557 . N1 Ir1 C1 89.45(8) . . N1 Ir1 C1 89.45(8) 2_557 . N2 Ir1 C1 30.34(7) . . N2 Ir1 C1 30.34(7) 2_557 . C12 N1 C16 118.6(3) . . C12 N1 Ir1 125.2(2) . . C16 N1 Ir1 116.0(2) . . C1 N2 C41 124.4(3) . . C1 N2 Ir1 94.0(2) . . C41 N2 Ir1 138.8(2) . . N2 C1 N2 111.3(4) 2_557 . N2 C1 C31 124.33(19) 2_557 . N2 C1 C31 124.33(19) . . N2 C1 Ir1 55.67(19) 2_557 . N2 C1 Ir1 55.67(19) . . C31 C1 Ir1 180.0 . . Cl1S C1S Cl1S 110.5(4) 2_556 . N1 C12 C13 122.6(3) . . C12 C13 C14 119.0(4) . . C15 C14 C13 119.3(4) . . C14 C15 C16 120.0(4) . . N1 C16 C15 120.4(3) . . N1 C16 C17 111.6(3) . . C15 C16 C17 128.0(3) . . C20 C17 C16 118.6(3) . . C20 C17 S1 115.5(3) . . C16 C17 S1 125.7(3) . . C17 C20 C21 110.3(3) . . C17 C20 Ir1 113.6(3) . . C21 C20 Ir1 136.1(2) . . C22 C21 C26 118.1(3) . . C22 C21 C20 129.5(3) . . C26 C21 C20 112.3(3) . . C23 C22 C21 120.6(3) . . C22 C23 C24 120.2(4) . . C25 C24 C23 121.4(3) . . C24 C25 C26 118.0(3) . . C25 C26 C21 121.7(3) . . C25 C26 S1 125.9(3) . . C21 C26 S1 112.4(3) . . C32 C31 C32 119.9(4) 2_557 . C32 C31 C1 120.1(2) 2_557 . C32 C31 C1 120.1(2) . . C31 C32 C33 119.7(3) . . C34 C33 C32 120.3(4) . . C33 C34 C33 120.2(5) 2_557 . N2 C41 C43 109.4(3) . . N2 C41 C42 111.7(3) . . C43 C41 C42 111.2(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cl1S C1S 1.721(4) . S1 C26 1.745(4) . S1 C17 1.752(3) . Ir1 C20 2.014(3) . Ir1 C20 2.014(3) 2_557 Ir1 N1 2.046(3) . Ir1 N1 2.046(3) 2_557 Ir1 N2 2.161(3) . Ir1 N2 2.161(3) 2_557 Ir1 C1 2.611(4) . N1 C12 1.348(4) . N1 C16 1.373(4) . N2 C1 1.322(4) . N2 C41 1.464(4) . C1 N2 1.322(4) 2_557 C1 C31 1.503(6) . C1S Cl1S 1.721(4) 2_556 C12 C13 1.376(5) . C13 C14 1.382(6) . C14 C15 1.376(6) . C15 C16 1.390(5) . C16 C17 1.435(5) . C17 C20 1.367(5) . C20 C21 1.451(5) . C21 C22 1.396(5) . C21 C26 1.417(5) . C22 C23 1.373(5) . C23 C24 1.399(5) . C24 C25 1.378(5) . C25 C26 1.396(5) . C31 C32 1.394(4) 2_557 C31 C32 1.394(4) . C32 C33 1.396(5) . C33 C34 1.380(4) . C34 C33 1.380(5) 2_557 C41 C43 1.521(5) . C41 C42 1.535(5) .