#------------------------------------------------------------------------------ #$Date: 2025-01-15 03:28:41 +0100 (Wed, 15 Jan 2025) $ #$Revision: 297318 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/33/2023347.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2023347 loop_ _publ_author_name 'Gienau, Trevor J.' 'Clay, Malachi' 'Brennessel, William W.' 'Reed, Carly R.' _publ_section_title ; (2,9-Dimethyl-1,10-phenanthroline)bis[2-(pyridin-2-yl)phenyl]iridium(III) hexafluorophosphate and (2,9-dimethyl-1,10-phenanthroline)bis[5-methyl-2-(pyridin-2-yl)phenyl]iridium(III) hexafluorophosphate--diethyl ether--acetonitrile (1/0.61/0.78) ; _journal_coeditor_code ZV2036 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989024012039 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac '[Ir (C14 H12 N2) (C12 H10 N)2] P F6, 0.61C4 H10 O, 0.78C2 H3 N' _chemical_formula_moiety 'C38 H32 Ir N4 +, F6 P -, 0.61(C4 H10 O), 0.78(C2 H3 N)' _chemical_formula_sum 'C42 H40.44 F6 Ir N4.78 O0.61 P' _chemical_formula_weight 959.08 _chemical_name_systematic '(2,9-Dimethyl-1,10-phenanthroline)bis[5-methyl-2-(pyridin-2-yl)phenyl]iridium(III) hexafluorophosphate--diethyl ether--acetonitrile (1/0.61/0.78)' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method ; Olex2 1.5-ac6-015 (compiled 2023.12.04 svn.r209d9fb2 for Rigaku Oxford Diffraction, GUI svn.r6873) ; _cell_angle_alpha 74.8888(6) _cell_angle_beta 78.9993(7) _cell_angle_gamma 88.7599(6) _cell_formula_units_Z 2 _cell_length_a 9.17379(7) _cell_length_b 13.10065(9) _cell_length_c 16.55352(14) _cell_measurement_reflns_used 40596 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 79.6750 _cell_measurement_theta_min 2.8070 _cell_volume 1884.53(3) _computing_cell_refinement ; CrysAlisPro 1.171.43.104a (Rigaku OD, 2023) ; _computing_data_collection 'CrysAlisPro system (CCD 43.104a 64-bit (release 22-12-2023))' _computing_data_reduction ; CrysAlisPro 1.171.43.104a (Rigaku OD, 2023) ; _computing_molecular_graphics ; Olex2 1.5-ac6-015 (Dolomanov et al., 2009) ; _computing_publication_material ; Olex2 1.5-ac6-015 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2019/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018/2 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_unetI/netI 0.0281 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 62414 _diffrn_reflns_theta_full 74.504 _diffrn_reflns_theta_max 80.263 _diffrn_reflns_theta_min 2.817 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 7.862 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.50939 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2023) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.690 _exptl_crystal_description plate _exptl_crystal_F_000 954 _exptl_crystal_size_max 0.157 _exptl_crystal_size_mid 0.132 _exptl_crystal_size_min 0.018 _refine_diff_density_max 1.249 _refine_diff_density_min -1.037 _refine_ls_extinction_coef 0.00030(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXT2018/2 (Sheldrick, 2015a) ; _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 624 _refine_ls_number_reflns 8074 _refine_ls_number_restraints 441 _refine_ls_restrained_S_all 1.041 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0259 _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^)+(0.0375P)^2^+2.8830P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.0667 _reflns_number_gt 7770 _reflns_number_total 8074 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file zv2036.cif _cod_data_source_block 2 _cod_database_code 2023347 _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 0.372 _shelx_estimated_absorpt_t_max 0.871 _shelx_hkl_file ; 0 0 -1 296098. 14825.7 60 0 0 -1 277722. 14919.3 58 0 0 1 299281. 14926.4 57 0 0 1 304771. 14922.8 55 0 0 -1 307064. 14860.5 5 0 0 -2 88300.9 5029.82 58 0 0 -2 94746.0 4842.67 60 0 0 -2 98945.9 5067.12 21 0 0 2 93338.1 4985.50 57 0 0 2 92488.0 4974.73 55 0 0 2 89074.0 5015.09 2 0 0 -2 96060.9 4871.47 5 0 0 -3 41678.4 2314.95 60 0 0 -3 42305.5 2573.25 21 0 0 -3 38393.9 2291.36 5 0 0 3 41770.3 2601.28 2 0 0 3 38697.9 2436.69 55 0 0 -4 14520.5 1324.18 21 0 0 4 15111.6 1389.24 2 0 0 4 14365.3 1317.71 1 0 0 4 14544.5 1301.17 56 0 0 4 13051.0 1179.05 55 0 0 -5 223272. 11564.4 21 0 0 5 233136. 11717.6 2 0 0 5 210755. 11434.5 1 0 0 5 202791. 11400.6 56 0 0 5 216680. 11381.9 55 0 0 -6 49496.2 3193.04 21 0 0 -6 43864.3 3030.95 4 0 0 6 49414.5 3319.94 2 0 0 6 46829.9 3084.90 1 0 0 6 44695.0 3011.77 55 0 0 6 43003.5 3032.15 56 0 0 -7 38884.6 2936.92 21 0 0 7 42017.3 2915.67 1 0 0 -7 40561.4 2892.25 4 0 0 7 38637.9 3053.93 2 0 0 7 42421.4 2950.00 56 0 0 7 42191.1 2915.58 55 0 0 -8 132404. 7963.10 21 0 0 8 137991. 7895.48 55 0 0 8 144390. 7969.00 56 0 0 -8 136962. 7172.21 53 0 0 -8 136276. 7919.57 4 0 0 8 135328. 8169.16 2 0 0 8 138075. 7886.79 1 0 0 9 8735.75 851.188 61 0 0 -9 10374.0 1410.48 21 0 0 9 11043.7 1473.99 56 0 0 -9 10149.4 850.371 53 0 0 9 9326.08 1292.46 1 0 0 -9 8308.60 1256.39 4 0 0 9 10935.5 1530.08 2 0 0 10 109427. 6127.74 61 0 0 -10 122761. 7308.58 21 0 0 -10 113501. 6172.59 53 0 0 10 121680. 7197.86 56 0 0 -10 120905. 7221.93 4 0 0 10 117096. 7080.71 1 0 0 -11 32298.8 2849.04 59 0 0 11 35202.2 2232.56 61 0 0 -11 33294.9 3110.38 21 0 0 -11 36063.3 2271.40 53 0 0 11 34841.5 3101.86 56 0 0 11 30059.1 2906.41 1 0 0 -11 36968.8 3143.99 4 0 0 -12 6835.14 1409.15 4 0 0 12 5903.79 1232.47 1 0 0 -12 5625.97 1145.13 59 0 0 12 5514.82 768.973 61 0 0 -12 4159.26 1200.74 21 0 0 -12 6153.03 784.826 53 0 0 12 5930.78 1421.24 56 0 0 -12 6255.70 817.551 16 0 0 12 5518.81 779.788 12 0 0 -12 5929.00 814.967 18 0 0 -12 6658.24 848.310 17 0 0 13 4151.46 1178.58 1 0 0 -13 5541.96 1305.33 4 0 0 -13 4871.02 951.863 59 0 0 13 5161.78 738.519 61 0 0 -13 2995.65 1099.09 21 0 0 -13 4031.83 684.929 53 0 0 13 5301.66 1366.33 56 0 0 -13 4548.72 750.844 16 0 0 -13 3957.22 745.576 17 0 0 13 4925.00 740.504 12 0 0 -13 2938.02 632.803 18 0 0 14 41127.0 3458.39 1 0 0 -14 36616.8 3585.20 4 0 0 14 35211.0 2461.91 61 0 0 -14 38114.0 3723.80 21 0 0 -14 40945.2 2609.92 53 0 0 14 40622.3 3510.39 56 0 0 -14 37382.6 3913.22 58 0 0 -14 35626.0 2546.60 18 0 0 14 41214.5 2631.85 12 0 0 -14 36551.7 2563.01 16 0 0 14 34174.4 2574.58 20 0 0 -14 34944.5 2532.17 17 0 0 -15 65487.1 4013.00 53 0 0 -15 64514.7 4038.80 18 0 0 15 67222.0 4110.23 20 0 0 -15 62183.2 4006.06 17 0 0 -15 66526.0 4068.53 16 0 0 15 72798.5 4088.15 12 0 0 15 65078.6 3896.31 61 0 0 -16 160.631 580.920 17 0 0 -16 82.5341 435.979 18 0 0 16-76.9876 406.686 12 0 0 16-83.7777 500.921 20 0 0 -16 331.333 437.559 16 0 0 -16 314.770 422.134 53 0 0 17 28171.7 1954.16 20 0 0 -17 23515.9 1844.72 18 0 0 -17 26473.5 1901.76 16 0 0 17 26331.7 1834.85 12 0 0 -17 26842.7 1910.06 17 0 0 -17 26437.8 1888.97 53 0 0 18 15274.8 1209.12 20 0 0 18 12587.5 1089.49 12 0 0 -18 15525.2 1213.92 15 0 0 -18 16389.0 1195.70 18 0 0 -18 15886.4 1224.62 17 0 0 -18 14832.8 1176.65 16 0 0 -18 14039.3 1151.86 53 0 0 -19 321.148 311.225 7 0 0 19 363.151 294.135 20 0 0 -19 455.887 303.544 15 0 0 -19 316.578 230.375 14 0 0 -19 229.514 371.564 17 0 1 -19 15382.9 1073.05 7 0 1 -19 16027.5 1087.50 17 0 1 -19 15943.0 1047.12 15 0 -1 19 14876.5 1057.39 20 0 1 -18 15771.1 1239.04 7 0 -1 18 17985.0 1324.01 62 0 1 -18 15484.3 1253.57 17 0 1 -18 17861.9 1266.38 15 0 -1 18 17652.9 1279.44 20 0 1 -18 17326.7 1269.43 18 0 1 -18 17397.4 1266.00 16 0 -1 18 15521.4 1155.89 12 0 1 -18 17179.7 1271.58 53 0 -1 17 263.041 471.700 62 0 1 -17 390.711 359.795 16 0 -1 17 65.5497 377.373 20 0 1 -17-64.1775 432.187 17 0 -1 17 446.846 346.034 12 0 1 -17 64.8898 401.977 18 0 1 -17-64.7221 367.677 53 0 -1 16 25216.8 1820.63 61 0 -1 16 27343.3 2017.80 62 0 -1 16 24860.6 1940.71 20 0 1 -16 26878.8 1956.68 18 0 1 -16 26962.6 1948.41 17 0 -1 16 25533.2 1884.37 12 0 1 -16 25718.4 1924.76 16 0 1 -16 26294.0 1944.76 53 0 -1 15 11324.5 1140.89 61 0 -1 15 10552.1 1229.84 62 0 1 -15 11424.2 1168.36 53 0 -1 15 12510.1 1250.26 20 0 -1 15 11176.5 1166.20 12 0 1 -15 11603.4 1215.98 16 0 1 -15 9957.37 1172.93 17 0 1 -15 13107.0 1231.14 18 0 1 -14 27612.2 2858.27 4 0 -1 14 28767.0 2114.33 61 0 -1 14 26993.1 2154.63 62 0 1 -14 31067.1 3140.50 21 0 1 -14 29274.2 2157.38 53 0 -1 14 33708.5 3171.81 56 0 1 -14 29906.4 2150.00 17 0 1 -14 26826.3 2103.61 16 0 1 -14 30679.7 2194.96 18 0 -1 14 29927.6 2144.00 12 0 -1 13 25352.8 2501.36 1 0 1 -13 25940.0 2803.23 4 0 -1 13 24036.9 1868.74 62 0 -1 13 24534.2 1848.06 61 0 1 -13 23591.7 2846.05 21 0 1 -13 22810.8 1827.40 53 0 -1 13 24071.3 2855.74 56 0 -1 13 23657.3 1841.83 12 0 1 -13 24650.4 1882.68 16 0 1 -13 22786.9 1838.35 18 0 1 -13 22730.1 1828.40 17 0 1 -12 19562.8 2268.65 4 0 -1 12 20678.4 2297.81 1 0 -1 12 17209.8 1487.57 62 0 1 -12 15664.9 1894.70 59 0 -1 12 16871.0 1426.87 61 0 1 -12 14656.4 2121.07 21 0 -1 12 14934.2 2147.97 56 0 1 -12 18702.9 1468.36 53 0 -1 12 16677.3 1436.23 12 0 1 -12 16962.5 1443.52 16 0 1 -12 15015.1 1402.16 18 0 1 -11 127802. 7892.19 4 0 -1 11 131955. 7839.17 1 0 -1 11 126411. 6786.10 61 0 -1 11 127871. 6814.50 62 0 1 -11 116201. 7591.16 59 0 1 -11 130685. 8173.66 21 0 1 -11 123880. 6819.87 53 0 -1 11 126352. 8054.65 56 0 1 -11 122661. 6811.79 16 0 1 -11 124404. 6828.25 18 0 -1 11 122032. 6816.64 12 0 1 -10 29194.9 2704.67 59 0 -1 10 33978.9 2181.75 62 0 -1 10 34925.9 2172.04 61 0 1 -10 32783.8 3037.01 21 0 1 -10 32795.2 2159.35 53 0 -1 10 34732.5 3063.82 56 0 -1 10 30563.6 2765.78 1 0 1 -10 36128.6 2963.42 4 0 -1 10 31478.8 3167.51 2 0 -1 9 95230.5 5100.54 61 0 -1 9 92824.9 5106.85 62 0 1 -9 86903.3 5789.33 59 0 1 -9 99039.9 6203.35 21 0 1 -9 96844.8 5151.92 53 0 -1 9 93114.6 6012.46 56 0 -1 9 93276.8 6346.38 2 0 -1 9 87813.1 5800.39 1 0 1 -9 93527.6 5906.11 4 0 -1 8 149479. 7950.16 62 0 1 -8 138669. 8601.26 59 0 -1 8 149985. 7947.01 61 0 1 -8 164574. 8977.90 21 0 -1 8 163848. 9247.68 2 0 1 -8 157126. 8715.67 4 0 -1 8 151914. 8656.85 1 0 1 -8 153314. 7992.04 53 0 -1 8 162824. 8893.80 56 0 1 -7 27432.5 2397.65 21 0 1 -7 29144.7 2282.72 4 0 -1 7 30471.2 2323.68 1 0 -1 7 30577.7 2582.09 2 0 -1 7 29289.6 2282.52 55 0 -1 7 27217.1 2373.01 56 0 1 -6 89264.6 5577.67 21 0 1 -6 100145. 5510.11 4 0 -1 6 89544.6 5417.14 1 0 -1 6 94888.1 5751.98 2 0 -1 6 94331.6 5429.63 55 0 -1 6 93107.8 5592.33 56 0 1 -5 24160.7 2025.08 21 0 1 -5 25846.6 2157.06 58 0 -1 5 30057.6 1991.42 55 0 -1 5 23876.6 1898.68 1 0 -1 5 23886.3 2067.41 2 0 1 -5 32012.9 2060.61 4 0 1 -5 25707.4 1871.49 5 0 1 -4 135716. 6767.68 4 0 1 -4 126622. 6692.07 5 0 -1 4 103047. 6593.77 1 0 -1 4 110053. 6785.50 2 0 1 -4 125526. 6262.05 66 0 1 -4 107763. 6773.38 21 0 1 -4 127673. 6269.01 47 0 -1 4 137205. 6728.09 55 0 1 -4 113962. 6849.65 58 0 1 -4 124032. 6213.97 42 0 1 -3 487885. 23424.1 66 0 -1 3 480355. 23676.1 1 0 1 -3 525087. 23747.5 4 0 1 -3 461804. 23723.7 5 0 -1 3 444009. 23638.1 55 0 1 -3 420282. 23425.4 47 0 1 -3 524381. 23950.5 58 0 1 -2 20570.8 1371.86 59 0 1 -2 23525.5 1383.48 66 0 1 -2 26259.0 1508.41 4 0 1 -2 20202.1 1489.06 5 0 -1 2 21750.1 1384.69 1 0 -1 2 23148.5 1396.11 55 0 -1 2 22624.5 1633.40 56 0 1 -2 21941.6 1480.85 58 0 -1 1 229787. 10773.3 3 0 1 -1 207169. 10757.8 4 0 1 -1 237560. 10908.4 58 0 -1 0 62866.9 3063.83 3 0 -1 0 54602.3 3037.06 51 0 1 0 59690.3 3087.84 49 0 -1 0 59319.8 3063.74 54 0 -1 0 58728.2 3053.31 56 0 -1 -1 204630. 10545.1 60 0 -1 -1 210956. 10538.9 54 0 1 1 212167. 10581.0 49 0 -1 -1 212514. 10541.8 4 0 -1 -2 84722.5 4396.86 60 0 -1 -2 81171.5 4416.89 21 0 -1 -2 84421.6 4397.60 52 0 1 2 84484.9 4402.94 56 0 -1 -2 86663.1 4378.53 54 0 -1 -2 87750.0 4590.92 4 0 -1 -3 145698. 7581.60 52 0 1 3 139683. 7749.49 55 0 1 3 133736. 7694.89 57 0 1 3 143410. 7613.56 56 0 1 3 155287. 7501.34 47 0 -1 -3 141155. 7519.37 60 0 1 3 157364. 7502.07 66 0 -1 -3 143815. 7615.72 21 0 1 4 517931. 25856.5 47 0 -1 -4 495116. 26178.3 52 0 1 4 518562. 26390.8 57 0 1 4 545326. 26355.8 55 0 1 4 565879. 26232.8 56 0 -1 -4 502347. 26038.3 60 0 1 4 520309. 25863.5 66 0 -1 -4 502901. 26247.8 21 0 -1 -5 7193.22 971.369 21 0 1 5 9165.51 1019.81 57 0 1 5 8633.94 993.587 55 0 1 5 9778.34 994.376 56 0 -1 -5 8417.82 954.703 4 0 1 5 10367.2 1120.23 1 0 -1 -6 57993.0 3551.44 60 0 -1 -6 62108.7 4019.40 21 0 1 6 67427.5 4081.02 1 0 1 6 60861.0 3846.95 55 0 1 6 63135.2 3777.30 56 0 -1 -7 110157. 6401.17 21 0 1 7 99303.2 5977.28 56 0 1 7 102876. 6101.00 55 0 1 7 108061. 6314.50 1 0 1 8 1409.93 456.670 62 0 -1 -8 2541.70 661.853 21 0 1 8 1386.20 672.563 55 0 1 8 1778.92 655.446 56 0 -1 -8 2141.49 405.644 53 0 1 8 3323.66 882.290 1 0 1 9 209887. 11362.8 61 0 -1 -9 259502. 12662.1 21 0 1 9 229367. 12386.1 55 0 1 9 219168. 12162.1 56 0 -1 -9 226744. 11456.9 53 0 1 9 233772. 12459.2 1 0 1 10 19332.6 1353.23 61 0 -1 -10 20403.6 2163.27 21 0 1 10 22397.5 2032.48 56 0 -1 -10 18248.5 1367.87 53 0 1 10 18897.9 2014.75 55 0 -1 -10 19574.8 1751.76 3 0 -1 -10 16903.4 1958.45 4 0 1 10 18068.2 2030.04 1 0 1 11 80649.4 4432.89 61 0 -1 -11 81830.3 5615.29 21 0 1 11 86235.7 5457.28 56 0 -1 -11 75786.9 4473.18 53 0 1 11 79066.2 5510.30 1 0 -1 -11 90044.2 5718.35 4 0 -1 -11 77759.1 4964.12 3 0 -1 -12 93922.1 6202.60 4 0 1 12 98359.3 6208.65 1 0 1 12 86355.9 4784.30 61 0 -1 -12 85610.9 6094.69 21 0 1 12 94604.2 5983.68 56 0 -1 -12 81069.5 4848.33 53 0 -1 -12 85989.8 4923.75 18 0 -1 -12 86737.8 4926.67 16 0 1 12 84908.1 4915.02 12 0 -1 -12 83497.3 4902.10 17 0 1 13 238.905 864.359 1 0 -1 -13 256.477 830.003 4 0 -1 -13 1429.86 505.309 59 0 1 13 252.587 409.351 61 0 -1 -13 264.280 698.457 21 0 -1 -13 374.510 390.291 53 0 -1 -13 562.103 830.284 58 0 1 13 1078.17 465.388 20 0 -1 -13 160.228 496.898 17 0 -1 -13 165.324 506.816 16 0 1 13 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878.834 401.202 8 7 12 2 914.179 371.082 10 7 12 2 1098.78 321.646 20 7 12 2 1295.15 324.664 19 7 12 3 20557.0 1370.67 19 -7 -12 -3 23513.1 1567.78 8 7 12 3 20037.3 1502.46 67 7 12 3 22668.2 1403.19 20 -7 -12 -3 20766.7 1518.21 33 7 12 3 21383.0 1519.16 48 -7 -12 -3 18497.4 1464.88 46 7 12 4 15299.4 1053.76 19 -7 -12 -4 14025.2 1250.34 8 -7 -12 -4 11593.8 1163.46 65 7 12 4 15522.9 1257.73 67 7 12 4 13868.5 1029.23 20 -7 -12 -4 14784.5 1268.86 33 7 12 4 12707.0 1206.02 48 -7 -12 -4 14747.1 1244.39 46 -7 -12 -5 462.693 467.195 65 -7 -12 -5 455.869 610.695 33 -7 -12 -5 544.773 612.724 8 7 12 5 417.588 290.053 19 7 12 5 227.627 303.506 20 7 12 5 583.102 218.137 13 -7 -12 -6 12301.0 1345.89 8 7 12 6 11027.8 1183.34 67 -7 -12 -6 12806.9 1345.81 33 7 12 6 12977.3 935.641 20 7 12 6 12543.7 1243.62 48 7 12 6 10764.9 841.674 13 7 12 6 12502.1 971.590 19 7 12 7 182.268 275.825 19 7 12 7 117.699 288.532 20 7 12 7 243.233 257.616 13 -7 -12 -7-278.189 574.379 65 7 12 7 254.884 441.750 67 7 12 7 167.887 476.819 48 -7 -12 -7-88.1214 604.683 46 7 12 8 18690.7 1263.93 13 7 12 8 19340.3 1351.37 19 -7 -12 -8 20771.6 1620.08 8 -7 -12 -8 17594.7 1552.81 65 7 12 8 22462.2 1697.57 67 7 12 8 17916.9 1270.91 20 -7 -12 -8 19131.0 1577.04 33 7 12 8 20483.7 1629.58 48 -7 -12 -8 15804.7 1500.72 46 7 12 9 19306.8 1277.58 13 7 12 9 19892.6 1349.28 19 -7 -12 -9 17302.5 1436.68 8 -7 -12 -9 18778.0 1483.66 65 7 12 9 19154.0 1490.39 67 7 12 9 17916.0 1255.86 20 -7 -12 -9 18232.9 1451.11 33 7 12 9 17436.9 1442.72 48 -7 -12 -9 17056.7 1433.09 46 7 12 10 798.830 338.848 19 -7 -12 -10 1233.26 372.039 14 7 12 10 583.788 322.868 20 7 12 10 533.594 293.991 13 -7 -12 -10 382.057 489.748 8 7 12 10 924.468 380.359 10 -7 -12 -10 616.843 440.005 33 -7 -12 -11 21520.8 1357.31 14 7 12 11 18223.8 1310.19 13 7 12 11 19143.5 1364.54 19 7 12 11 20121.8 1283.73 10 7 12 11 18900.6 1300.80 20 -7 -12 -11 19585.5 1288.45 33 -7 -12 -12 1735.75 405.379 14 7 12 12 1905.47 367.440 20 7 12 12 1527.76 404.739 13 -7 -12 -13 8034.01 679.585 14 7 12 13 8211.12 668.949 13 7 12 13 6961.80 613.105 20 7 13 2 7883.34 614.489 18 7 13 2 8702.59 626.469 16 7 13 3 11434.7 816.868 18 7 13 3 10715.9 801.723 16 -7 -13 -3 9665.59 758.197 8 7 13 4 1864.25 318.389 20 7 13 4 1768.94 329.837 19 -7 -13 -4 2228.34 459.960 8 7 13 4 1914.35 399.484 10 -7 -13 -4 2119.45 442.992 33 7 13 5 18361.3 1161.18 19 -7 -13 -5 16572.1 1290.62 8 7 13 5 17273.4 1259.97 10 7 13 5 18175.0 1134.08 20 -7 -13 -5 17953.0 1303.39 33 7 13 6 2852.02 394.780 19 7 13 6 3011.53 383.647 20 -7 -13 -6 2652.94 622.187 8 7 13 6 3015.84 540.774 10 -7 -13 -6 3305.98 619.934 33 7 13 7 12079.8 875.778 19 7 13 7 11577.6 830.087 20 7 13 8 10707.1 794.029 13 7 13 8 13691.8 933.022 19 -7 -13 -8 12098.1 1065.02 8 7 13 8 15175.6 1136.11 10 -7 -13 -8 12881.6 1090.35 33 7 13 8 13329.8 868.626 20 7 13 9 285.723 259.867 19 7 13 9 799.391 270.391 20 7 13 9 536.585 210.546 13 -7 -13 -9 444.170 368.409 8 7 13 9 838.605 369.266 10 -7 -13 -9 514.440 396.634 33 7 13 10 11011.5 772.972 13 7 13 10 11576.3 847.099 19 7 13 10 10775.8 774.674 20 7 13 10 12746.2 813.398 10 -8 11 4 17304.3 1159.52 39 -8 11 4 17707.4 1203.77 30 -8 11 4 17716.0 1251.68 31 -8 11 3 19443.1 1361.25 39 -8 11 3 22214.5 1462.99 30 -8 11 3 19510.6 1383.21 31 -8 11 2 6803.08 783.676 39 -8 11 2 8955.33 778.206 31 -8 11 1 182.339 380.778 39 -8 11 1 101.954 476.047 30 -8 11 0 9474.55 913.651 30 -8 11 -1 12583.2 1046.48 39 -8 11 -1 14563.4 1103.30 30 -8 11 -2 28421.8 1548.04 40 -8 11 -2 25887.5 1601.89 30 -8 11 -3 25054.9 1497.21 40 -8 11 -4 61.6628 324.583 40 -8 10 8 20717.4 1244.46 43 -8 10 8 20497.1 1242.92 44 -8 10 7 545.308 331.811 44 -8 10 7 543.951 316.995 43 -8 10 6 19585.9 1438.86 43 -8 10 6 20680.4 1447.04 44 -8 10 5 12810.9 1000.34 43 -8 10 5 13598.0 1018.93 44 -8 10 5 10620.8 948.322 30 -8 10 4 6829.58 720.885 43 -8 10 4 7746.15 776.686 39 -8 10 4 6750.13 733.881 44 -8 10 4 7116.07 817.976 30 -8 10 3 30340.7 1876.00 43 -8 10 3 32886.5 2032.43 39 -8 10 3 28082.6 1848.21 44 -8 10 3 30918.4 2031.57 30 -8 10 2 1091.13 586.880 39 -8 10 2 3042.50 588.686 31 -8 10 1 37680.5 2405.84 39 -8 10 1 33323.7 2128.45 29 -8 10 1 39851.5 2353.10 31 -8 10 0 20515.1 1763.17 30 -8 10 0 24038.4 1547.50 29 -8 10 0 25183.6 1655.91 31 -8 10 -1 2510.41 523.733 40 -8 10 -1 3591.41 708.993 30 -8 10 -1 2721.56 510.926 29 -8 10 -2 34680.9 2070.18 40 -8 10 -2 31702.1 2112.57 39 -8 10 -2 30748.5 2122.26 30 -8 10 -2 31878.9 2004.79 29 -8 10 -3 49.6850 412.367 39 -8 10 -3 184.687 510.126 40 -8 10 -3 46.4761 425.215 30 -8 10 -3 91.7171 465.159 29 -8 10 -4 23268.1 1566.26 40 -8 10 -4 20758.9 1520.70 39 -8 10 -4 22532.8 1490.40 30 -8 10 -5 7006.64 733.035 29 -8 10 -6 9274.87 787.110 29 -8 10 -7 18852.4 1127.42 40 -8 10 -7 18214.8 1129.81 29 -8 9 9 17828.4 1093.73 43 -8 9 9 17058.5 1089.71 44 -8 9 8 280.335 328.609 44 -8 9 8 439.872 334.435 43 -8 9 7 14239.7 1179.06 43 -8 9 7 15910.2 1223.45 38 -8 9 7 14448.9 1181.51 44 -8 9 7 18427.6 1148.06 31 -8 9 6 13873.6 1165.34 43 -8 9 6 14638.1 1202.65 38 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19169.7 1490.28 31 -8 9 -2 106.658 410.768 31 -8 9 -2 153.662 617.224 30 -8 9 -2 111.529 468.752 29 -8 9 -2 107.198 397.390 28 -8 9 -2 404.978 548.356 40 -8 9 -2 493.757 383.502 7 -8 9 -3 30008.2 2129.95 30 -8 9 -3 31695.3 2104.69 29 -8 9 -3 33528.7 2078.37 28 -8 9 -3 30238.8 1973.43 27 -8 9 -3 34168.4 2234.58 40 -8 9 -3 29709.0 2130.06 39 -8 9 -3 31390.4 2059.69 7 -8 9 -4 23763.3 1799.08 30 -8 9 -4 28865.7 1929.73 29 -8 9 -4 25271.5 1729.45 28 -8 9 -4 28881.6 1838.40 27 -8 9 -4 24428.6 1810.88 39 -8 9 -4 30532.2 1911.81 7 -8 9 -5 5860.16 689.413 30 -8 9 -5 6788.96 899.105 29 -8 9 -5 6708.36 896.010 27 -8 9 -5 5837.86 746.342 39 -8 9 -5 7443.64 844.054 7 -8 9 -6 24325.9 1627.83 27 -8 9 -6 21900.1 1591.10 7 -8 9 -7 2286.21 456.900 25 -8 9 -7 1923.17 574.574 27 -8 9 -7 1967.94 466.329 40 -8 9 -7 1529.84 445.342 7 -8 9 -8 11380.3 829.252 25 -8 9 -8 11777.5 913.402 27 -8 9 -8 11948.3 859.545 40 -8 9 -8 11120.3 856.838 7 -8 8 9 888.435 343.004 44 -8 8 9 1328.62 357.277 43 -8 8 8 37008.2 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2426.25 8 -10 -8 -6 58643.9 3174.49 34 -10 -8 -7 3669.61 549.052 34 -10 -8 -8 10500.3 911.792 33 -10 -8 -8 11174.7 887.414 34 -10 -8 -8 10340.8 922.263 8 -10 -8 -9 1038.89 458.210 34 -10 -8 -9 1096.56 366.885 33 -10 -8 -9 1249.28 357.166 8 -10 -8 -10 5866.09 623.706 34 -10 -9 -6 93.2588 349.643 33 -10 -9 -6 289.949 367.308 8 -11 4 -3 2702.15 407.041 41 -11 4 -4 19650.2 1246.90 41 -11 4 -5 26066.8 1546.50 41 -11 4 -6 589.666 261.598 41 -11 4 -6 154.503 288.185 28 -11 3 1 19021.2 1227.60 34 -11 3 0 5588.44 605.484 34 -11 3 0 3903.11 618.788 33 -11 3 -1 51615.7 3065.96 33 -11 3 -2 12256.6 884.793 41 -11 3 -2 9973.77 1092.06 33 -11 3 -3 18572.2 1236.56 41 -11 3 -4 45411.2 2575.09 41 -11 3 -5 2120.26 437.354 41 -11 3 -5 1138.99 402.337 28 -11 3 -5 2185.79 533.726 33 -11 3 -6 19566.4 1328.68 41 -11 3 -6 20135.0 1302.19 28 -11 3 -6 20514.7 1392.85 27 -11 3 -7 9566.91 750.744 41 -11 3 -7 8553.12 714.040 28 -11 3 -7 9925.76 835.766 27 -11 3 -8 8540.36 647.774 41 -11 3 -8 8696.84 673.195 27 -11 2 2 13571.8 964.985 34 -11 2 1 364.952 462.879 34 -11 2 1 284.323 337.983 33 -11 2 0 29893.5 1838.96 34 -11 2 0 27476.4 1675.28 26 -11 2 0 31626.6 1897.88 33 -11 2 -1 13994.5 1020.86 26 -11 2 -1 18428.6 1352.96 33 -11 2 -1 15534.3 1218.95 34 -11 2 -1 17527.8 1337.26 8 -11 2 -2 9303.45 738.307 26 -11 2 -2 10718.1 1085.40 33 -11 2 -2 8582.38 897.878 34 -11 2 -2 8018.99 1015.82 8 -11 2 -3 27778.9 1661.35 26 -11 2 -4 514.867 313.291 26 -11 2 -5 41952.9 2305.31 26 -11 2 -5 39869.7 2300.87 28 -11 2 -5 40993.8 2419.53 27 -11 2 -5 37233.5 2499.03 33 -11 2 -6 12874.4 930.137 26 -11 2 -6 13484.8 969.086 28 -11 2 -6 11900.8 1053.66 33 -11 2 -6 14759.9 1161.49 27 -11 2 -7 3961.99 559.366 41 -11 2 -7 2927.17 388.888 26 -11 2 -7 4067.35 502.161 28 -11 2 -7 3213.68 483.335 33 -11 2 -7 2597.73 621.918 27 -11 2 -8 11978.9 911.102 41 -11 2 -8 11383.4 826.136 28 -11 2 -8 13984.3 923.940 27 -11 2 -9 1137.50 289.548 41 -11 1 2-147.516 279.280 36 -11 1 2 24.5795 300.995 37 -11 1 2 71.2422 263.298 26 -11 1 1 13473.1 950.542 33 -11 1 1 11518.8 879.697 26 -11 1 0 8696.56 724.042 26 -11 1 0 9090.45 860.091 33 -11 1 0 7854.91 878.416 34 -11 1 0 9176.98 884.026 8 -11 1 -1 11986.4 868.617 26 -11 1 -1 12294.2 1095.30 33 -11 1 -1 9878.35 1029.58 34 -11 1 -1 9818.12 856.254 41 -11 1 -1 11873.5 1089.45 8 -11 1 -2 41907.3 2373.12 26 -11 1 -2 42378.4 2691.60 33 -11 1 -2 36973.3 2510.60 34 -11 1 -2 40885.3 2402.23 41 -11 1 -2 46653.8 2755.23 8 -11 1 -3 915.354 380.328 26 -11 1 -3 417.963 685.929 33 -11 1 -3 199.730 374.175 41 -11 1 -3 931.118 560.871 34 -11 1 -3 649.974 636.862 8 -11 1 -4 31572.1 2010.41 41 -11 1 -4 35527.9 2018.46 26 -11 1 -5 21220.7 1438.04 26 -11 1 -5 24540.9 1700.70 33 -11 1 -5 22148.6 1466.52 41 -11 1 -5 21211.2 1675.59 8 -11 1 -6 5666.28 624.119 26 -11 1 -6 5182.44 559.849 28 -11 1 -6 4414.16 703.140 33 -11 1 -6 5780.98 825.345 27 -11 1 -6 5333.21 655.748 41 -11 1 -6 5415.56 726.996 8 -11 1 -7 15022.6 1151.56 41 -11 1 -7 18450.6 1158.06 26 -11 1 -7 14658.8 1031.02 28 -11 1 -7 14871.7 1208.11 27 -11 1 -7 13751.1 1114.34 33 -11 1 -8 116.359 362.338 41 -11 1 -8 154.153 299.384 26 -11 1 -8 359.398 279.657 28 -11 1 -9 11177.8 836.301 41 -11 1 -9 11081.6 766.353 26 -11 0 3 1997.80 372.179 34 -11 0 2 21346.8 1288.74 37 -11 0 2 19622.0 1334.16 34 -11 0 2 22817.6 1302.32 36 -11 0 2 19710.2 1297.72 26 -11 0 1 17744.7 1145.83 37 -11 0 1 18500.1 1153.92 36 -11 0 1 15061.8 1102.85 33 -11 0 1 16227.8 1137.94 26 -11 0 0 3887.45 509.352 26 -11 0 0 3553.99 584.545 33 -11 0 0 3211.98 598.144 8 -11 0 -1 33096.0 1941.00 26 -11 0 -1 35700.0 2144.98 33 -11 0 -1 35477.5 2178.12 8 -11 0 -2 2255.94 423.086 26 -11 0 -2 2711.02 679.230 33 -11 0 -2 2525.42 473.902 41 -11 0 -2 2662.40 663.041 34 -11 0 -2 1248.23 624.617 8 -11 0 -3 16983.9 1147.97 26 -11 0 -3 15850.3 1449.32 33 -11 0 -3 15240.9 1298.38 34 -11 0 -3 15082.2 1138.87 41 -11 0 -3 15659.4 1442.74 8 -11 0 -4 8108.27 867.812 34 -11 0 -4 7157.04 731.743 41 -11 0 -4 6931.61 713.012 26 -11 0 -5 9567.45 823.604 41 -11 0 -5 9109.09 800.568 26 -11 0 -5 7600.47 840.713 34 -11 0 -6 32951.0 2060.59 26 -11 0 -6 35496.0 2238.80 33 -11 0 -6 33294.4 2069.40 41 -11 0 -6 35953.5 2308.23 8 -11 0 -7 337.044 405.322 26 -11 0 -7 46.6824 433.989 33 -11 0 -7 375.096 412.144 41 -11 0 -7 527.471 448.019 8 -11 0 -8 26778.7 1558.82 26 -11 0 -8 19616.9 1420.49 33 -11 0 -8 24778.4 1543.60 41 -11 0 -8 22238.4 1448.59 8 -11 0 -9 11667.8 900.432 41 -11 0 -9 12664.8 912.022 26 -11 0 -10 4659.14 421.203 41 -11 0 -10 3294.91 397.565 26 -11 -1 2 23252.0 1387.59 37 -11 -1 2 22719.3 1441.55 34 -11 -1 2 24409.3 1394.63 36 -11 -1 1 2554.22 418.368 36 -11 -1 1 2426.62 545.604 34 -11 -1 1 2646.13 449.496 37 -11 -1 0 37784.7 2186.95 33 -11 -1 0 33905.7 2102.38 36 -11 -1 0 37926.4 2133.61 37 -11 -1 0 36533.7 2182.02 8 -11 -1 -1 658.290 509.608 33 -11 -1 -1 156.303 477.046 8 -11 -1 -2 34927.5 2265.28 33 -11 -1 -2 34110.4 2276.78 8 -11 -1 -3 28385.5 1968.66 33 -11 -1 -3 23994.6 1623.12 41 -11 -1 -3 26523.9 1783.77 34 -11 -1 -3 28163.5 1976.50 8 -11 -1 -4 5128.55 602.779 41 -11 -1 -4 5784.62 822.201 34 -11 -1 -5 36378.7 2074.31 41 -11 -1 -5 32148.5 2133.45 34 -11 -1 -6 7066.30 849.674 33 -11 -1 -6 7220.57 782.077 34 -11 -1 -6 5835.10 670.170 41 -11 -1 -6 7018.44 876.971 8 -11 -1 -7 18458.4 1376.45 33 -11 -1 -7 17479.5 1254.88 41 -11 -1 -7 18700.0 1382.47 8 -11 -1 -8 17400.1 1231.81 33 -11 -1 -8 17489.6 1236.34 41 -11 -1 -8 18377.3 1259.97 8 -11 -1 -9 8387.02 703.186 41 -11 -2 2 3310.75 361.210 36 -11 -2 2 3404.72 371.181 37 -11 -2 2 2808.71 386.626 26 -11 -2 1 40880.9 2223.71 36 -11 -2 1 37383.7 2268.04 34 -11 -2 1 43941.4 2241.92 37 -11 -2 1 36357.3 2240.71 26 -11 -2 0 7807.94 717.408 26 -11 -2 0 7359.68 699.731 33 -11 -2 0 8198.58 710.880 36 -11 -2 0 7353.09 691.963 37 -11 -2 0 7273.14 784.349 34 -11 -2 0 7887.45 707.426 8 -11 -2 -1 26956.1 1658.50 26 -11 -2 -1 26761.2 1726.47 33 -11 -2 -1 26576.4 1624.85 36 -11 -2 -1 24517.6 1701.54 34 -11 -2 -1 26003.1 1628.28 37 -11 -2 -1 26996.5 1742.72 8 -11 -2 -2 32997.0 2068.10 26 -11 -2 -2 36954.0 2266.76 33 -11 -2 -2 35498.9 2272.49 8 -11 -2 -3 398.097 371.858 26 -11 -2 -3-600.942 584.952 33 -11 -2 -3-131.905 536.956 46 -11 -2 -3 1168.60 615.731 8 -11 -2 -4 17225.7 1151.22 26 -11 -2 -4 13494.1 1320.52 33 -11 -2 -4 14829.5 1071.52 41 -11 -2 -4 16229.8 1262.86 34 -11 -2 -4 15150.5 1385.66 8 -11 -2 -5 209.405 361.432 41 -11 -2 -5-136.035 553.675 46 -11 -2 -5-40.8712 358.011 26 -11 -2 -5 200.260 587.611 34 -11 -2 -6 31293.6 1851.44 26 -11 -2 -6 29041.0 2005.78 33 -11 -2 -6 28112.3 1757.94 41 -11 -2 -6 26739.1 1850.95 34 -11 -2 -6 32670.2 2052.95 8 -11 -2 -7 27686.1 1674.98 26 -11 -2 -7 24920.5 1731.90 33 -11 -2 -7 25977.7 1582.34 41 -11 -2 -7 23184.7 1596.32 34 -11 -2 -7 24961.1 1734.36 8 -11 -2 -8 2883.91 529.745 26 -11 -2 -8 2646.02 517.458 33 -11 -2 -8 1928.96 437.872 41 -11 -2 -8 2954.89 529.976 8 -11 -2 -9 35415.5 2005.45 41 -11 -2 -9 38840.7 2216.09 26 -11 -2 -10 3985.49 491.642 26 -11 -3 1 5510.59 505.324 36 -11 -3 1 6238.72 520.683 37 -11 -3 1 6230.68 546.505 26 -11 -3 0 18021.9 1083.29 36 -11 -3 0 12713.7 1087.54 34 -11 -3 0 18986.3 1096.95 37 -11 -3 0 14560.2 1063.18 26 -11 -3 -1 13392.7 975.944 26 -11 -3 -1 13481.9 1010.58 33 -11 -3 -1 13984.2 998.030 36 -11 -3 -1 12625.8 1025.62 34 -11 -3 -1 14577.8 1017.00 37 -11 -3 -1 13326.3 1025.63 8 -11 -3 -2 320.888 341.807 26 -11 -3 -2 658.423 473.391 34 -11 -3 -2 603.441 461.233 33 -11 -3 -2 424.154 335.404 36 -11 -3 -2 273.694 339.044 37 -11 -3 -2 572.724 434.885 8 -11 -3 -3 25217.4 1650.54 26 -11 -3 -3 28389.3 1896.28 33 -11 -3 -3 28293.9 1886.95 8 -11 -3 -4 8697.31 757.542 26 -11 -3 -4 8514.58 981.163 33 -11 -3 -4 7740.35 974.444 8 -11 -3 -5 17846.9 1233.82 26 -11 -3 -6 19774.9 1476.42 34 -11 -3 -6 22087.5 1402.69 26 -11 -3 -7 1861.36 443.162 26 -11 -3 -7 1849.49 534.689 34 -11 -3 -7 1750.34 559.923 33 -11 -3 -7 1039.79 487.099 8 -11 -3 -8 15497.8 1089.21 26 -11 -3 -8 14032.3 1074.89 33 -11 -3 -8 15041.8 1031.01 34 -11 -3 -8 13666.2 1087.13 8 -11 -3 -9 4577.40 580.202 26 -11 -3 -10 12943.5 905.969 26 -11 -4 -1 1743.37 352.104 36 -11 -4 -1 1210.97 414.349 34 -11 -4 -1 1197.34 344.072 37 -11 -4 -1 1505.89 331.165 26 -11 -4 -2 14120.4 975.086 26 -11 -4 -2 15196.2 1073.97 33 -11 -4 -2 13148.7 959.874 36 -11 -4 -2 14040.8 1038.99 34 -11 -4 -2 13661.4 965.318 37 -11 -4 -2 16839.7 1109.25 8 -11 -4 -3 7936.09 683.330 26 -11 -4 -3 8355.37 835.972 33 -11 -4 -3 8976.21 796.653 34 -11 -4 -3 8694.13 865.824 8 -11 -4 -4 7517.15 663.511 26 -11 -4 -4 8202.98 951.687 33 -11 -4 -4 8293.17 792.762 34 -11 -4 -4 7605.91 924.465 8 -11 -4 -5 14857.6 1027.35 26 -11 -4 -6 1430.83 353.363 26 -11 -4 -7 21135.5 1281.63 26 -11 -4 -7 21351.9 1413.32 33 -11 -4 -7 16721.0 1302.80 34 -11 -4 -7 18555.9 1372.15 8 -11 -4 -8 3937.48 483.814 26 -11 -4 -8 3993.06 537.195 34 -11 -4 -8 2867.86 474.165 33 -11 -4 -8 3902.88 534.528 8 -11 -4 -9 3976.82 483.291 26 -11 -5 -3 7061.82 684.759 33 -11 -5 -3 7294.07 641.322 34 -11 -5 -3 6399.68 669.660 8 -11 -5 -4 11159.0 797.767 26 -11 -5 -4 11358.5 1008.93 33 -11 -5 -4 12889.7 916.125 34 -11 -5 -4 12239.4 1039.81 8 -11 -5 -5 256.972 259.931 26 -11 -5 -5-127.808 416.616 34 -11 -5 -5 47.0778 450.435 33 -11 -5 -5-627.547 517.858 8 -11 -5 -6 12434.5 847.133 26 -11 -5 -7 7146.81 749.912 33 -11 -5 -7 7848.21 748.670 8 -11 -5 -8 4204.18 513.670 34 -11 -5 -8 3746.50 454.492 33 -11 -5 -8 3155.30 472.359 8 -11 -6 -5 7953.25 752.330 33 -11 -6 -5 9257.74 776.515 8 -11 -6 -6 3078.61 438.276 34 0 0 0 0.00 0.00 0 TITL Faces in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 9.173786 13.100646 16.553518 74.8888 78.9993 88.7599 ZERR 2.00 0.000074 0.000085 0.000139 0.0006 0.0007 0.0006 LATT 1 SFAC C H N O F P Ir UNIT 84.00 81.00 9.60 1.20 12.00 2.00 2.00 REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0 TEMP -173 SIZE 0.02 0.13 0.16 TREF HKLF 4 END ; _shelx_hkl_checksum 43460 _shelx_res_file ; TITL brocr24_a.res in P-1 brocr24.res created by SHELXL-2019/3 at 11:15:51 on 18-Jun-2024 REM Old TITL BROCR24_auto in P1 REM SHELXT solution in P-1: R1 0.070, Rweak 0.013, Alpha 0.041 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C42' N4 F3 P Ir CELL 1.54184 9.173786 13.100646 16.553518 74.8888 78.9993 88.7599 ZERR 2 0.000074 0.000085 0.000139 0.0006 0.0007 0.0006 LATT 1 SFAC C H F Ir N O P UNIT 84 80.88 12 2 9.56 1.22 2 SIMU 0.01 0.02 1.2 DFIX 1.136 0.01 N5' C39' N6' C41' SADI 0.01 P1 F1 P1 F2 P1 F3 P1 F4 P1 F5 P1 F6 P1' F1' P1' F2' P1' F3' P1' = F4' P1' F5' P1' F6' DFIX 1.47 0.01 C39' C40' C41' C42' SADI 0.04 F1 F3 F1 F4 F1 F5 F1 F6 F2 F3 F2 F4 F2 F5 F2 F6 F3 F4 F3 F6 F4 F5 = F5 F6 F1' F3' F1' F4' F1' F5' F1' F6' F2' F3' F2' F4' F2' F5' F2' F6' F3' = F4' F3' F6' F4' F5' F5' F6' DFIX 2.606 N5' C40' N6' C42' L.S. 12 PLAN 1 SIZE 0.157 0.132 0.018 TEMP -173 CONF BOND $H list 4 MORE -1 fmap 2 acta 149.008 REM REM REM WGHT 0.037500 2.883000 EXTI 0.000298 FVAR 3.42180 0.64453 0.60995 IR1 4 0.561767 0.313543 0.300089 11.00000 0.01239 0.01474 = 0.01579 -0.00338 -0.00104 0.00190 N1 5 0.742737 0.407939 0.290787 11.00000 0.01386 0.01808 = 0.01750 -0.00442 0.00071 0.00000 N2 5 0.387090 0.225323 0.290266 11.00000 0.01645 0.01579 = 0.01911 -0.00393 -0.00375 0.00196 N3 5 0.447286 0.368866 0.411495 11.00000 0.01244 0.01923 = 0.01834 -0.00715 -0.00026 0.00074 N4 5 0.604107 0.186593 0.410915 11.00000 0.01294 0.01768 = 0.01923 -0.00281 -0.00259 -0.00055 C1 1 0.529890 0.435043 0.201909 11.00000 0.01919 0.01990 = 0.01661 -0.00564 -0.00029 0.00366 C2 1 0.414285 0.446880 0.156421 11.00000 0.01962 0.02134 = 0.01942 -0.00598 -0.00169 0.00204 AFIX 43 H2 2 0.339988 0.392279 0.171112 11.00000 -1.20000 AFIX 0 C3 1 0.404395 0.536109 0.090241 11.00000 0.02396 0.02566 = 0.01810 -0.00671 -0.00563 0.00870 C4 1 0.515926 0.615297 0.067269 11.00000 0.02690 0.02300 = 0.02115 -0.00173 -0.00304 0.00580 AFIX 43 H4 2 0.510492 0.676558 0.022253 11.00000 -1.20000 AFIX 0 C5 1 0.633835 0.605202 0.109445 11.00000 0.02460 0.02058 = 0.02354 -0.00389 -0.00062 0.00069 AFIX 43 H5 2 0.709508 0.659043 0.093005 11.00000 -1.20000 AFIX 0 C6 1 0.641798 0.515723 0.176343 11.00000 0.01869 0.02163 = 0.01822 -0.00605 -0.00096 0.00321 C7 1 0.760497 0.498889 0.225727 11.00000 0.01713 0.01955 = 0.01637 -0.00571 0.00097 0.00309 C8 1 0.884696 0.565029 0.211230 11.00000 0.02103 0.02191 = 0.02444 -0.00407 -0.00023 -0.00212 AFIX 43 H8 2 0.897416 0.627800 0.165866 11.00000 -1.20000 AFIX 0 C9 1 0.989448 0.539786 0.262496 11.00000 0.01704 0.02725 = 0.03016 -0.00726 -0.00081 -0.00423 AFIX 43 H9 2 1.074258 0.584926 0.252567 11.00000 -1.20000 AFIX 0 C10 1 0.969984 0.447873 0.328740 11.00000 0.01691 0.02836 = 0.02883 -0.00640 -0.00634 0.00169 AFIX 43 H10 2 1.040461 0.429200 0.364984 11.00000 -1.20000 AFIX 0 C11 1 0.844977 0.384156 0.340524 11.00000 0.01678 0.02352 = 0.02066 -0.00473 -0.00192 0.00115 AFIX 43 H11 2 0.831069 0.321103 0.385616 11.00000 -1.20000 AFIX 0 C12 1 0.273897 0.548384 0.045458 11.00000 0.03146 0.03070 = 0.02566 -0.00559 -0.00939 0.00749 AFIX 137 H12A 2 0.216237 0.481534 0.062674 11.00000 -1.50000 H12B 2 0.309996 0.567350 -0.016366 11.00000 -1.50000 H12C 2 0.210703 0.604241 0.060979 11.00000 -1.50000 AFIX 0 C13 1 0.659046 0.257199 0.201160 11.00000 0.02158 0.01755 = 0.01669 -0.00355 -0.00129 0.00560 C14 1 0.805483 0.274512 0.156542 11.00000 0.02330 0.02056 = 0.02109 -0.00163 -0.00175 0.00365 AFIX 43 H14 2 0.870260 0.318147 0.172469 11.00000 -1.20000 AFIX 0 C15 1 0.859756 0.229722 0.089242 11.00000 0.02318 0.02665 = 0.02154 -0.00250 0.00489 0.00744 C16 1 0.763051 0.168076 0.064631 11.00000 0.03412 0.02523 = 0.02585 -0.00952 0.00279 0.00693 AFIX 43 H16 2 0.798347 0.137079 0.018951 11.00000 -1.20000 AFIX 0 C17 1 0.615353 0.151532 0.106343 11.00000 0.03058 0.02328 = 0.02301 -0.00651 -0.00348 0.00404 AFIX 43 H17 2 0.550003 0.110025 0.088789 11.00000 -1.20000 AFIX 0 C18 1 0.563599 0.196024 0.173928 11.00000 0.02148 0.02021 = 0.01876 -0.00427 -0.00275 0.00359 C19 1 0.412337 0.179339 0.223868 11.00000 0.02095 0.01820 = 0.01837 -0.00354 -0.00397 0.00383 C20 1 0.298721 0.121613 0.209380 11.00000 0.02460 0.02447 = 0.02947 -0.01177 -0.00889 0.00461 AFIX 43 H20 2 0.316023 0.089729 0.163159 11.00000 -1.20000 AFIX 0 C21 1 0.160640 0.110781 0.262404 11.00000 0.02028 0.03257 = 0.03631 -0.01376 -0.00955 -0.00061 AFIX 43 H21 2 0.082658 0.071690 0.252696 11.00000 -1.20000 AFIX 0 C22 1 0.136865 0.157416 0.329858 11.00000 0.01624 0.03136 = 0.03064 -0.00936 -0.00354 0.00094 AFIX 43 H22 2 0.042962 0.150330 0.367156 11.00000 -1.20000 AFIX 0 C23 1 0.252097 0.214219 0.341714 11.00000 0.01854 0.02108 = 0.02015 -0.00382 -0.00258 0.00238 AFIX 43 H23 2 0.235959 0.246633 0.387628 11.00000 -1.20000 AFIX 0 C24 1 1.018891 0.250768 0.043235 11.00000 0.02902 0.04515 = 0.03054 -0.01032 0.00623 0.00732 AFIX 137 H24A 2 1.031319 0.324148 0.008388 11.00000 -1.50000 H24B 2 1.044498 0.202773 0.006432 11.00000 -1.50000 H24C 2 1.084347 0.239071 0.084967 11.00000 -1.50000 AFIX 0 C25 1 0.371553 0.457125 0.412996 11.00000 0.01256 0.02075 = 0.02319 -0.00663 -0.00264 0.00129 C26 1 0.308344 0.481553 0.490003 11.00000 0.01552 0.02545 = 0.02729 -0.01400 -0.00017 0.00196 AFIX 43 H26 2 0.254593 0.544557 0.488837 11.00000 -1.20000 AFIX 0 C27 1 0.323990 0.415210 0.566103 11.00000 0.02033 0.02834 = 0.02369 -0.01213 0.00134 -0.00072 AFIX 43 H27 2 0.281885 0.431971 0.617965 11.00000 -1.20000 AFIX 0 C28 1 0.402609 0.322073 0.567374 11.00000 0.01776 0.02547 = 0.02123 -0.00848 -0.00123 -0.00122 C29 1 0.419936 0.249161 0.645056 11.00000 0.02835 0.03212 = 0.01604 -0.00835 0.00075 -0.00285 AFIX 43 H29 2 0.378477 0.263902 0.697809 11.00000 -1.20000 AFIX 0 C30 1 0.494528 0.159295 0.644782 11.00000 0.02806 0.02777 = 0.01714 -0.00059 -0.00446 -0.00315 AFIX 43 H30 2 0.505359 0.111531 0.697244 11.00000 -1.20000 AFIX 0 C31 1 0.556924 0.135628 0.566657 11.00000 0.01676 0.02257 = 0.02348 -0.00363 -0.00539 -0.00200 C32 1 0.637410 0.043414 0.564753 11.00000 0.02300 0.02087 = 0.02531 -0.00030 -0.00954 -0.00069 AFIX 43 H32 2 0.649516 -0.005589 0.616406 11.00000 -1.20000 AFIX 0 C33 1 0.697449 0.025039 0.488803 11.00000 0.01655 0.01678 = 0.02976 -0.00206 -0.00765 0.00136 AFIX 43 H33 2 0.752492 -0.036908 0.487234 11.00000 -1.20000 AFIX 0 C34 1 0.678942 0.097214 0.411846 11.00000 0.01313 0.01599 = 0.02446 -0.00249 -0.00360 0.00044 C35 1 0.543302 0.205843 0.488258 11.00000 0.01644 0.01884 = 0.01731 -0.00454 -0.00242 -0.00342 C36 1 0.462775 0.301505 0.488125 11.00000 0.01466 0.01754 = 0.01633 -0.00204 -0.00142 -0.00244 C37 1 0.349116 0.533559 0.332054 11.00000 0.02740 0.02537 = 0.02515 -0.00955 -0.00665 0.01172 AFIX 137 H37A 2 0.445488 0.563933 0.298570 11.00000 -1.50000 H37B 2 0.285437 0.590249 0.345523 11.00000 -1.50000 H37C 2 0.301724 0.496575 0.299036 11.00000 -1.50000 AFIX 0 C38 1 0.748501 0.071445 0.330707 11.00000 0.02541 0.02280 = 0.02536 -0.00351 -0.00213 0.00968 AFIX 137 H38A 2 0.671213 0.064410 0.298840 11.00000 -1.50000 H38B 2 0.800504 0.004744 0.343638 11.00000 -1.50000 H38C 2 0.819484 0.128252 0.296338 11.00000 -1.50000 AFIX 0 PART 2 P1' 7 0.979525 0.226839 0.581767 -21.00000 0.01717 0.01857 = 0.03118 -0.00803 -0.00716 0.00373 F1' 3 0.938415 0.110928 0.639083 -21.00000 0.07289 0.03439 = 0.10072 0.03011 -0.05294 -0.02455 F2' 3 1.022385 0.342630 0.522717 -21.00000 0.07576 0.05065 = 0.08704 0.02433 -0.04496 -0.03304 F3' 3 0.815259 0.263338 0.605511 -21.00000 0.01863 0.07679 = 0.14015 -0.07565 -0.00633 0.01049 F4' 3 1.026823 0.262309 0.657694 -21.00000 0.04442 0.07525 = 0.04020 -0.03141 -0.00380 -0.02103 F5' 3 1.144689 0.195651 0.551776 -21.00000 0.02287 0.09450 = 0.09932 -0.07075 -0.00356 0.00630 F6' 3 0.931580 0.194134 0.504039 -21.00000 0.04028 0.08013 = 0.03272 -0.01425 -0.00920 -0.01953 SAME 0.02 0.04 C42 < C39 PART 1 C39 1 1.065308 0.069375 0.857662 31.00000 0.07557 0.07096 = 0.09186 -0.00711 -0.01152 0.02528 AFIX 137 H39A 2 1.065509 0.021290 0.821140 31.00000 -1.50000 H39B 2 1.044449 0.028852 0.917608 31.00000 -1.50000 H39C 2 1.162689 0.105539 0.844568 31.00000 -1.50000 AFIX 0 C40 1 0.944928 0.151657 0.841453 31.00000 0.06554 0.05010 = 0.03569 -0.00863 -0.00860 -0.00369 AFIX 23 H40A 2 0.952585 0.204385 0.873883 31.00000 -1.20000 H40B 2 0.963505 0.189339 0.780110 31.00000 -1.20000 AFIX 0 O1 6 0.797541 0.106248 0.865377 31.00000 0.08694 0.03384 = 0.04407 -0.01334 -0.01777 0.00674 C41 1 0.693985 0.188399 0.838737 31.00000 0.07248 0.08503 = 0.07525 -0.05183 -0.01205 0.01200 AFIX 23 H41A 2 0.711661 0.214101 0.775799 31.00000 -1.20000 H41B 2 0.704928 0.248940 0.862746 31.00000 -1.20000 AFIX 0 C42 1 0.536895 0.135221 0.873873 31.00000 0.05412 0.06775 = 0.05151 -0.03127 -0.00484 0.00454 AFIX 137 H42A 2 0.530344 0.072823 0.852377 31.00000 -1.50000 H42B 2 0.461848 0.185540 0.855091 31.00000 -1.50000 H42C 2 0.519384 0.113749 0.936317 31.00000 -1.50000 AFIX 0 PART 2 N5' 5 0.894607 0.011679 0.902132 -31.00000 0.11178 0.09372 = 0.09093 -0.03290 -0.03086 0.02237 N6' 5 0.693406 0.205491 0.831119 -31.00000 0.09420 0.11896 = 0.10019 -0.04273 0.00277 0.02892 C39' 1 1.009985 0.051569 0.872519 -31.00000 0.05824 0.05748 = 0.04898 -0.02227 0.00103 0.01833 C40' 1 1.157272 0.103100 0.837549 -31.00000 0.07808 0.05444 = 0.12385 0.01705 0.05156 0.01231 AFIX 137 H40C 2 1.150402 0.164271 0.789652 -31.00000 -1.50000 H40D 2 1.226436 0.052786 0.817689 -31.00000 -1.50000 H40E 2 1.193331 0.126654 0.881952 -31.00000 -1.50000 AFIX 0 C41' 1 0.599829 0.144448 0.869043 -31.00000 0.08643 0.10228 = 0.07832 -0.04734 -0.00508 0.00124 C42' 1 0.446676 0.107080 0.909854 -31.00000 0.14380 0.09930 = 0.14220 -0.05175 0.00652 -0.02661 AFIX 137 H42D 2 0.379334 0.136728 0.870853 -31.00000 -1.50000 H42E 2 0.417843 0.129945 0.962383 -31.00000 -1.50000 H42F 2 0.440850 0.029678 0.923506 -31.00000 -1.50000 AFIX 0 PART 1 P1 7 0.972013 0.221134 0.577288 21.00000 0.01772 0.02117 = 0.02770 -0.00882 -0.00145 0.00116 F1 3 0.859937 0.145656 0.652996 21.00000 0.04267 0.03931 = 0.02775 0.00270 -0.00638 -0.01699 F2 3 1.083162 0.296457 0.499147 21.00000 0.02972 0.05619 = 0.03435 -0.01140 0.00317 -0.01797 F3 3 0.836163 0.269020 0.533292 21.00000 0.03148 0.04362 = 0.05915 0.00806 -0.01755 -0.00557 F4 3 0.960887 0.311808 0.625114 21.00000 0.04092 0.03633 = 0.05021 -0.02853 0.00512 -0.00515 F5 3 1.110133 0.173292 0.617303 21.00000 0.03647 0.03123 = 0.10338 -0.00256 -0.04126 0.00649 F6 3 0.982356 0.132183 0.526798 21.00000 0.04237 0.05696 = 0.07278 -0.04584 0.00342 -0.01011 HKLF 4 REM brocr24_a.res in P-1 REM wR2 = 0.0667, GooF = S = 1.039, Restrained GooF = 1.041 for all data REM R1 = 0.0259 for 7770 Fo > 4sig(Fo) and 0.0270 for all 8074 data REM 624 parameters refined using 441 restraints END WGHT 0.0375 2.8824 REM Highest difference peak 1.249, deepest hole -1.037, 1-sigma level 0.100 Q1 1 1.1009 0.3355 0.6991 11.00000 0.05 1.25 ; _shelx_res_checksum 75215 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ir Ir1 0.56177(2) 0.31354(2) 0.30009(2) 0.01467(5) Uani d 1 . . N N1 0.7427(3) 0.40794(19) 0.29079(15) 0.0170(5) Uani d 1 . . N N2 0.3871(3) 0.22532(18) 0.29027(15) 0.0172(4) Uani d 1 . . N N3 0.4473(3) 0.36887(19) 0.41150(15) 0.0166(4) Uani d 1 . . N N4 0.6041(3) 0.18659(19) 0.41092(15) 0.0171(4) Uani d 1 . . C C1 0.5299(3) 0.4350(2) 0.20191(18) 0.0189(5) Uani d 1 . . C C2 0.4143(3) 0.4469(2) 0.15642(18) 0.0203(6) Uani d 1 . . H H2 0.339988 0.392279 0.171112 0.024 Uiso calc 1 . . C C3 0.4044(3) 0.5361(2) 0.09024(19) 0.0223(6) Uani d 1 . . C C4 0.5159(4) 0.6153(2) 0.0673(2) 0.0247(6) Uani d 1 . . H H4 0.510492 0.676558 0.022253 0.030 Uiso calc 1 . . C C5 0.6338(4) 0.6052(2) 0.1094(2) 0.0238(6) Uani d 1 . . H H5 0.709508 0.659043 0.093005 0.029 Uiso calc 1 . . C C6 0.6418(3) 0.5157(2) 0.17634(18) 0.0197(5) Uani d 1 . . C C7 0.7605(3) 0.4989(2) 0.22573(18) 0.0181(5) Uani d 1 . . C C8 0.8847(3) 0.5650(2) 0.2112(2) 0.0234(6) Uani d 1 . . H H8 0.897416 0.627800 0.165866 0.028 Uiso calc 1 . . C C9 0.9894(3) 0.5398(3) 0.2625(2) 0.0253(6) Uani d 1 . . H H9 1.074258 0.584926 0.252567 0.030 Uiso calc 1 . . C C10 0.9700(3) 0.4479(3) 0.3287(2) 0.0247(6) Uani d 1 . . H H10 1.040461 0.429200 0.364984 0.030 Uiso calc 1 . . C C11 0.8450(3) 0.3842(2) 0.34052(19) 0.0208(6) Uani d 1 . . H H11 0.831069 0.321103 0.385616 0.025 Uiso calc 1 . . C C12 0.2739(4) 0.5484(3) 0.0455(2) 0.0292(7) Uani d 1 . . H H12A 0.216237 0.481534 0.062674 0.044 Uiso calc 1 . . H H12B 0.309996 0.567350 -0.016366 0.044 Uiso calc 1 . . H H12C 0.210703 0.604241 0.060979 0.044 Uiso calc 1 . . C C13 0.6590(3) 0.2572(2) 0.20116(18) 0.0192(5) Uani d 1 . . C C14 0.8055(3) 0.2745(2) 0.15654(19) 0.0228(6) Uani d 1 . . H H14 0.870260 0.318147 0.172469 0.027 Uiso calc 1 . . C C15 0.8598(4) 0.2297(3) 0.0892(2) 0.0259(6) Uani d 1 . . C C16 0.7631(4) 0.1681(3) 0.0646(2) 0.0291(7) Uani d 1 . . H H16 0.798347 0.137079 0.018951 0.035 Uiso calc 1 . . C C17 0.6154(4) 0.1515(2) 0.1063(2) 0.0258(6) Uani d 1 . . H H17 0.550003 0.110025 0.088789 0.031 Uiso calc 1 . . C C18 0.5636(3) 0.1960(2) 0.17393(18) 0.0205(6) Uani d 1 . . C C19 0.4123(3) 0.1793(2) 0.22387(18) 0.0194(5) Uani d 1 . . C C20 0.2987(4) 0.1216(2) 0.2094(2) 0.0248(6) Uani d 1 . . H H20 0.316023 0.089729 0.163159 0.030 Uiso calc 1 . . C C21 0.1606(4) 0.1108(3) 0.2624(2) 0.0282(7) Uani d 1 . . H H21 0.082658 0.071690 0.252696 0.034 Uiso calc 1 . . C C22 0.1369(3) 0.1574(3) 0.3299(2) 0.0260(6) Uani d 1 . . H H22 0.042962 0.150330 0.367156 0.031 Uiso calc 1 . . C C23 0.2521(3) 0.2142(2) 0.34171(19) 0.0204(6) Uani d 1 . . H H23 0.235959 0.246633 0.387628 0.024 Uiso calc 1 . . C C24 1.0189(4) 0.2508(3) 0.0432(2) 0.0366(8) Uani d 1 . . H H24A 1.031319 0.324148 0.008388 0.055 Uiso calc 1 . . H H24B 1.044498 0.202773 0.006432 0.055 Uiso calc 1 . . H H24C 1.084347 0.239071 0.084967 0.055 Uiso calc 1 . . C C25 0.3716(3) 0.4571(2) 0.41300(19) 0.0188(5) Uani d 1 . . C C26 0.3083(3) 0.4816(2) 0.4900(2) 0.0220(6) Uani d 1 . . H H26 0.254593 0.544557 0.488837 0.026 Uiso calc 1 . . C C27 0.3240(3) 0.4152(2) 0.5661(2) 0.0238(6) Uani d 1 . . H H27 0.281885 0.431971 0.617965 0.029 Uiso calc 1 . . C C28 0.4026(3) 0.3221(2) 0.56737(19) 0.0213(6) Uani d 1 . . C C29 0.4199(4) 0.2492(3) 0.64506(19) 0.0257(6) Uani d 1 . . H H29 0.378477 0.263902 0.697809 0.031 Uiso calc 1 . . C C30 0.4945(4) 0.1593(3) 0.64478(19) 0.0252(6) Uani d 1 . . H H30 0.505359 0.111531 0.697244 0.030 Uiso calc 1 . . C C31 0.5569(3) 0.1356(2) 0.56666(19) 0.0211(6) Uani d 1 . . C C32 0.6374(3) 0.0434(2) 0.5648(2) 0.0235(6) Uani d 1 . . H H32 0.649516 -0.005589 0.616406 0.028 Uiso calc 1 . . C C33 0.6974(3) 0.0250(2) 0.4888(2) 0.0214(6) Uani d 1 . . H H33 0.752492 -0.036908 0.487234 0.026 Uiso calc 1 . . C C34 0.6789(3) 0.0972(2) 0.41185(19) 0.0184(5) Uani d 1 . . C C35 0.5433(3) 0.2058(2) 0.48826(18) 0.0176(5) Uani d 1 . . C C36 0.4628(3) 0.3015(2) 0.48812(17) 0.0168(5) Uani d 1 . . C C37 0.3491(4) 0.5336(2) 0.3321(2) 0.0254(6) Uani d 1 . . H H37A 0.445488 0.563933 0.298570 0.038 Uiso calc 1 . . H H37B 0.285437 0.590249 0.345523 0.038 Uiso calc 1 . . H H37C 0.301724 0.496575 0.299036 0.038 Uiso calc 1 . . C C38 0.7485(4) 0.0714(2) 0.3307(2) 0.0256(6) Uani d 1 . . H H38A 0.671213 0.064410 0.298840 0.038 Uiso calc 1 . . H H38B 0.800504 0.004744 0.343638 0.038 Uiso calc 1 . . H H38C 0.819484 0.128252 0.296338 0.038 Uiso calc 1 . . P P1' 0.9795(7) 0.2268(5) 0.5818(4) 0.0217(17) Uani d 0.355(6) A 2 F F1' 0.9384(13) 0.1109(6) 0.6391(7) 0.073(3) Uani d 0.355(6) A 2 F F2' 1.0224(12) 0.3426(7) 0.5227(7) 0.075(3) Uani d 0.355(6) A 2 F F3' 0.8153(6) 0.2633(7) 0.6055(8) 0.071(3) Uani d 0.355(6) A 2 F F4' 1.0268(9) 0.2623(7) 0.6577(4) 0.050(2) Uani d 0.355(6) A 2 F F5' 1.1447(7) 0.1957(8) 0.5518(7) 0.065(3) Uani d 0.355(6) A 2 F F6' 0.9316(9) 0.1941(8) 0.5040(4) 0.051(2) Uani d 0.355(6) A 2 C C39 1.0653(17) 0.0694(15) 0.8577(14) 0.083(4) Uani d 0.610(7) B 1 H H39A 1.065509 0.021290 0.821140 0.125 Uiso calc 0.610(7) B 1 H H39B 1.044449 0.028852 0.917608 0.125 Uiso calc 0.610(7) B 1 H H39C 1.162689 0.105539 0.844568 0.125 Uiso calc 0.610(7) B 1 C C40 0.9449(9) 0.1517(6) 0.8415(5) 0.0510(19) Uani d 0.610(7) B 1 H H40A 0.952585 0.204385 0.873883 0.061 Uiso calc 0.610(7) B 1 H H40B 0.963505 0.189339 0.780110 0.061 Uiso calc 0.610(7) B 1 O O1 0.7975(7) 0.1062(4) 0.8654(3) 0.0537(16) Uani d 0.610(7) B 1 C C41 0.6940(18) 0.1884(13) 0.8387(14) 0.072(3) Uani d 0.610(7) B 1 H H41A 0.711661 0.214101 0.775799 0.087 Uiso calc 0.610(7) B 1 H H41B 0.704928 0.248940 0.862746 0.087 Uiso calc 0.610(7) B 1 C C42 0.5369(11) 0.1352(9) 0.8739(7) 0.056(2) Uani d 0.610(7) B 1 H H42A 0.530344 0.072823 0.852377 0.083 Uiso calc 0.610(7) B 1 H H42B 0.461848 0.185540 0.855091 0.083 Uiso calc 0.610(7) B 1 H H42C 0.519384 0.113749 0.936317 0.083 Uiso calc 0.610(7) B 1 N N5' 0.8946(17) 0.0117(13) 0.9021(11) 0.096(5) Uani d 0.390(7) B 2 N N6' 0.693(3) 0.205(2) 0.831(3) 0.105(6) Uani d 0.390(7) B 2 C C39' 1.0100(19) 0.0516(19) 0.8725(15) 0.055(4) Uani d 0.390(7) B 2 C C40' 1.1573(18) 0.1031(13) 0.8375(15) 0.103(7) Uani d 0.390(7) B 2 H H40C 1.150402 0.164271 0.789652 0.154 Uiso calc 0.390(7) B 2 H H40D 1.226436 0.052786 0.817689 0.154 Uiso calc 0.390(7) B 2 H H40E 1.193331 0.126654 0.881952 0.154 Uiso calc 0.390(7) B 2 C C41' 0.600(3) 0.144(2) 0.8690(18) 0.086(5) Uani d 0.390(7) B 2 C C42' 0.447(3) 0.1071(19) 0.9099(18) 0.129(7) Uani d 0.390(7) B 2 H H42D 0.379334 0.136728 0.870853 0.193 Uiso calc 0.390(7) B 2 H H42E 0.417843 0.129945 0.962383 0.193 Uiso calc 0.390(7) B 2 H H42F 0.440850 0.029678 0.923506 0.193 Uiso calc 0.390(7) B 2 P P1 0.9720(4) 0.2211(3) 0.5773(2) 0.0221(9) Uani d 0.645(6) A 1 F F1 0.8599(5) 0.1457(3) 0.6530(2) 0.0385(10) Uani d 0.645(6) A 1 F F2 1.0832(4) 0.2965(4) 0.4991(2) 0.0412(10) Uani d 0.645(6) A 1 F F3 0.8362(4) 0.2690(3) 0.5333(3) 0.0475(12) Uani d 0.645(6) A 1 F F4 0.9609(5) 0.3118(3) 0.6251(3) 0.0410(10) Uani d 0.645(6) A 1 F F5 1.1101(5) 0.1733(3) 0.6173(4) 0.0562(15) Uani d 0.645(6) A 1 F F6 0.9824(5) 0.1322(4) 0.5268(3) 0.0537(13) Uani d 0.645(6) A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir1 0.01239(7) 0.01474(7) 0.01579(7) 0.00190(4) -0.00104(4) -0.00338(4) N1 0.0139(11) 0.0181(11) 0.0175(11) 0.0000(9) 0.0007(9) -0.0044(9) N2 0.0164(11) 0.0158(11) 0.0191(11) 0.0020(9) -0.0037(9) -0.0039(9) N3 0.0124(10) 0.0192(11) 0.0183(11) 0.0007(9) -0.0003(9) -0.0072(9) N4 0.0129(11) 0.0177(11) 0.0192(11) -0.0006(9) -0.0026(9) -0.0028(9) C1 0.0192(13) 0.0199(13) 0.0166(12) 0.0037(11) -0.0003(10) -0.0056(10) C2 0.0196(14) 0.0213(14) 0.0194(13) 0.0020(11) -0.0017(11) -0.0060(11) C3 0.0240(15) 0.0257(15) 0.0181(13) 0.0087(12) -0.0056(11) -0.0067(11) C4 0.0269(16) 0.0230(14) 0.0211(14) 0.0058(12) -0.0030(12) -0.0017(11) C5 0.0246(15) 0.0206(14) 0.0235(14) 0.0007(11) -0.0006(12) -0.0039(11) C6 0.0187(14) 0.0216(14) 0.0182(13) 0.0032(11) -0.0010(11) -0.0061(11) C7 0.0171(13) 0.0196(13) 0.0164(12) 0.0031(10) 0.0010(10) -0.0057(10) C8 0.0210(14) 0.0219(14) 0.0244(14) -0.0021(11) -0.0002(11) -0.0041(11) C9 0.0170(14) 0.0272(15) 0.0302(16) -0.0042(11) -0.0008(12) -0.0073(13) C10 0.0169(14) 0.0284(15) 0.0288(15) 0.0017(11) -0.0063(12) -0.0064(12) C11 0.0168(13) 0.0235(14) 0.0207(13) 0.0012(11) -0.0019(11) -0.0047(11) C12 0.0315(17) 0.0307(16) 0.0257(15) 0.0075(13) -0.0094(13) -0.0056(13) C13 0.0216(14) 0.0175(13) 0.0167(12) 0.0056(11) -0.0013(11) -0.0035(10) C14 0.0233(15) 0.0206(14) 0.0211(14) 0.0036(11) -0.0018(11) -0.0016(11) C15 0.0232(15) 0.0266(15) 0.0215(14) 0.0074(12) 0.0049(12) -0.0025(12) C16 0.0341(18) 0.0252(15) 0.0258(15) 0.0069(13) 0.0028(13) -0.0095(13) C17 0.0306(17) 0.0233(14) 0.0230(14) 0.0040(12) -0.0035(12) -0.0065(12) C18 0.0215(14) 0.0202(13) 0.0188(13) 0.0036(11) -0.0027(11) -0.0043(11) C19 0.0209(14) 0.0182(13) 0.0184(13) 0.0038(11) -0.0040(11) -0.0035(10) C20 0.0246(15) 0.0245(15) 0.0295(15) 0.0046(12) -0.0089(12) -0.0118(12) C21 0.0203(15) 0.0326(17) 0.0363(17) -0.0006(12) -0.0095(13) -0.0138(14) C22 0.0162(14) 0.0314(16) 0.0306(16) 0.0009(12) -0.0035(12) -0.0094(13) C23 0.0185(14) 0.0211(13) 0.0201(13) 0.0024(11) -0.0026(11) -0.0038(11) C24 0.0290(18) 0.045(2) 0.0305(17) 0.0073(15) 0.0062(14) -0.0103(15) C25 0.0126(12) 0.0208(13) 0.0232(14) 0.0013(10) -0.0026(10) -0.0066(11) C26 0.0155(13) 0.0254(14) 0.0273(15) 0.0020(11) -0.0002(11) -0.0140(12) C27 0.0203(14) 0.0283(15) 0.0237(14) -0.0007(12) 0.0013(11) -0.0121(12) C28 0.0178(14) 0.0255(15) 0.0212(14) -0.0012(11) -0.0012(11) -0.0085(12) C29 0.0283(16) 0.0321(16) 0.0160(13) -0.0029(13) 0.0007(12) -0.0084(12) C30 0.0281(16) 0.0278(15) 0.0171(13) -0.0032(12) -0.0045(12) -0.0006(11) C31 0.0168(13) 0.0226(14) 0.0235(14) -0.0020(11) -0.0054(11) -0.0036(11) C32 0.0230(15) 0.0209(14) 0.0253(15) -0.0007(11) -0.0095(12) -0.0003(11) C33 0.0165(13) 0.0168(13) 0.0298(15) 0.0014(10) -0.0076(11) -0.0021(11) C34 0.0131(12) 0.0160(12) 0.0245(14) 0.0004(10) -0.0036(10) -0.0025(11) C35 0.0164(13) 0.0188(13) 0.0173(13) -0.0034(10) -0.0024(10) -0.0045(10) C36 0.0147(12) 0.0175(13) 0.0163(12) -0.0024(10) -0.0014(10) -0.0020(10) C37 0.0274(16) 0.0254(15) 0.0251(15) 0.0117(12) -0.0066(12) -0.0095(12) C38 0.0254(15) 0.0228(14) 0.0254(15) 0.0097(12) -0.0021(12) -0.0035(12) P1' 0.017(3) 0.019(3) 0.031(3) 0.0037(18) -0.007(2) -0.008(2) F1' 0.073(6) 0.034(4) 0.101(7) -0.025(4) -0.053(6) 0.030(4) F2' 0.076(7) 0.051(5) 0.087(7) -0.033(5) -0.045(6) 0.024(5) F3' 0.019(3) 0.077(5) 0.140(9) 0.010(3) -0.006(4) -0.076(6) F4' 0.044(4) 0.075(6) 0.040(4) -0.021(4) -0.004(3) -0.031(4) F5' 0.023(3) 0.095(6) 0.099(7) 0.006(4) -0.004(4) -0.071(6) F6' 0.040(4) 0.080(6) 0.033(3) -0.020(4) -0.009(3) -0.014(4) C39 0.076(11) 0.071(9) 0.092(11) 0.025(8) -0.012(9) -0.007(8) C40 0.066(5) 0.050(4) 0.036(3) -0.004(4) -0.009(3) -0.009(3) O1 0.087(4) 0.034(3) 0.044(3) 0.007(2) -0.018(3) -0.013(2) C41 0.072(7) 0.085(7) 0.075(7) 0.012(6) -0.012(6) -0.052(6) C42 0.054(6) 0.068(5) 0.052(5) 0.005(5) -0.005(5) -0.031(4) N5' 0.112(12) 0.094(10) 0.091(10) 0.022(9) -0.031(9) -0.033(8) N6' 0.094(10) 0.119(12) 0.100(11) 0.029(10) 0.003(9) -0.043(10) C39' 0.058(11) 0.057(9) 0.049(8) 0.018(8) 0.001(8) -0.022(7) C40' 0.078(11) 0.054(9) 0.124(13) 0.012(8) 0.052(10) 0.017(9) C41' 0.086(9) 0.102(9) 0.078(8) 0.001(9) -0.005(9) -0.047(7) C42' 0.144(16) 0.099(13) 0.142(16) -0.027(13) 0.007(14) -0.052(12) P1 0.0177(15) 0.0212(15) 0.0277(15) 0.0012(10) -0.0015(11) -0.0088(11) F1 0.043(2) 0.039(2) 0.0278(16) -0.0170(17) -0.0064(16) 0.0027(15) F2 0.030(2) 0.056(3) 0.0344(18) -0.0180(18) 0.0032(15) -0.0114(17) F3 0.0315(19) 0.044(2) 0.059(3) -0.0056(15) -0.0176(18) 0.0081(19) F4 0.041(2) 0.0363(19) 0.050(2) -0.0052(16) 0.0051(17) -0.0285(18) F5 0.036(2) 0.0312(18) 0.103(4) 0.0065(15) -0.041(3) -0.003(2) F6 0.042(2) 0.057(3) 0.073(3) -0.010(2) 0.003(2) -0.046(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Ir1 N2 . . 171.61(9) y N1 Ir1 N3 . . 89.41(9) y N1 Ir1 N4 . . 96.50(9) y N2 Ir1 N3 . . 97.19(9) y N2 Ir1 N4 . . 90.07(9) y N4 Ir1 N3 . . 76.79(9) y C1 Ir1 N1 . . 80.42(11) y C1 Ir1 N2 . . 93.13(11) y C1 Ir1 N3 . . 101.51(10) y C1 Ir1 N4 . . 176.54(10) y C13 Ir1 N1 . . 93.12(11) y C13 Ir1 N2 . . 80.39(11) y C13 Ir1 N3 . . 177.26(10) y C13 Ir1 N4 . . 101.85(10) y C13 Ir1 C1 . . 79.97(11) y C7 N1 Ir1 . . 115.65(19) ? C11 N1 Ir1 . . 124.8(2) ? C11 N1 C7 . . 119.5(2) ? C19 N2 Ir1 . . 115.46(19) ? C23 N2 Ir1 . . 124.8(2) ? C23 N2 C19 . . 119.7(2) ? C25 N3 Ir1 . . 129.3(2) ? C25 N3 C36 . . 117.9(2) ? C36 N3 Ir1 . . 112.78(18) ? C34 N4 Ir1 . . 129.1(2) ? C34 N4 C35 . . 117.8(2) ? C35 N4 Ir1 . . 113.05(18) ? C2 C1 Ir1 . . 128.0(2) ? C2 C1 C6 . . 117.5(3) ? C6 C1 Ir1 . . 114.4(2) ? C1 C2 H2 . . 118.9 ? C3 C2 C1 . . 122.2(3) ? C3 C2 H2 . . 118.9 ? C2 C3 C4 . . 118.8(3) ? C2 C3 C12 . . 120.6(3) ? C4 C3 C12 . . 120.6(3) ? C3 C4 H4 . . 119.7 ? C5 C4 C3 . . 120.6(3) ? C5 C4 H4 . . 119.7 ? C4 C5 H5 . . 120.0 ? C4 C5 C6 . . 120.0(3) ? C6 C5 H5 . . 120.0 ? C1 C6 C7 . . 115.2(3) ? C5 C6 C1 . . 120.8(3) ? C5 C6 C7 . . 124.0(3) ? N1 C7 C6 . . 114.2(2) ? N1 C7 C8 . . 119.9(3) ? C8 C7 C6 . . 126.0(3) ? C7 C8 H8 . . 119.9 ? C9 C8 C7 . . 120.3(3) ? C9 C8 H8 . . 119.9 ? C8 C9 H9 . . 120.2 ? C8 C9 C10 . . 119.5(3) ? C10 C9 H9 . . 120.2 ? C9 C10 H10 . . 120.9 ? C11 C10 C9 . . 118.2(3) ? C11 C10 H10 . . 120.9 ? N1 C11 C10 . . 122.7(3) ? N1 C11 H11 . . 118.7 ? C10 C11 H11 . . 118.7 ? C3 C12 H12A . . 109.5 ? C3 C12 H12B . . 109.5 ? C3 C12 H12C . . 109.5 ? H12A C12 H12B . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 109.5 ? C14 C13 Ir1 . . 127.8(2) ? C14 C13 C18 . . 117.8(3) ? C18 C13 Ir1 . . 114.4(2) ? C13 C14 H14 . . 119.0 ? C13 C14 C15 . . 122.1(3) ? C15 C14 H14 . . 119.0 ? C14 C15 C24 . . 120.0(3) ? C16 C15 C14 . . 118.7(3) ? C16 C15 C24 . . 121.3(3) ? C15 C16 H16 . . 119.7 ? C17 C16 C15 . . 120.6(3) ? C17 C16 H16 . . 119.7 ? C16 C17 H17 . . 120.1 ? C16 C17 C18 . . 119.8(3) ? C18 C17 H17 . . 120.1 ? C13 C18 C19 . . 115.3(3) ? C17 C18 C13 . . 120.9(3) ? C17 C18 C19 . . 123.7(3) ? N2 C19 C18 . . 114.3(3) ? N2 C19 C20 . . 119.9(3) ? C20 C19 C18 . . 125.8(3) ? C19 C20 H20 . . 120.1 ? C21 C20 C19 . . 119.9(3) ? C21 C20 H20 . . 120.1 ? C20 C21 H21 . . 120.2 ? C20 C21 C22 . . 119.5(3) ? C22 C21 H21 . . 120.2 ? C21 C22 H22 . . 120.6 ? C23 C22 C21 . . 118.7(3) ? C23 C22 H22 . . 120.6 ? N2 C23 C22 . . 122.2(3) ? N2 C23 H23 . . 118.9 ? C22 C23 H23 . . 118.9 ? C15 C24 H24A . . 109.5 ? C15 C24 H24B . . 109.5 ? C15 C24 H24C . . 109.5 ? H24A C24 H24B . . 109.5 ? H24A C24 H24C . . 109.5 ? H24B C24 H24C . . 109.5 ? N3 C25 C26 . . 122.0(3) ? N3 C25 C37 . . 120.8(3) ? C26 C25 C37 . . 117.2(3) ? C25 C26 H26 . . 119.9 ? C27 C26 C25 . . 120.3(3) ? C27 C26 H26 . . 119.9 ? C26 C27 H27 . . 120.2 ? C26 C27 C28 . . 119.6(3) ? C28 C27 H27 . . 120.2 ? C27 C28 C29 . . 121.8(3) ? C27 C28 C36 . . 117.6(3) ? C36 C28 C29 . . 120.6(3) ? C28 C29 H29 . . 119.6 ? C30 C29 C28 . . 120.8(3) ? C30 C29 H29 . . 119.6 ? C29 C30 H30 . . 119.8 ? C29 C30 C31 . . 120.5(3) ? C31 C30 H30 . . 119.8 ? C32 C31 C30 . . 121.5(3) ? C32 C31 C35 . . 117.9(3) ? C35 C31 C30 . . 120.6(3) ? C31 C32 H32 . . 120.3 ? C33 C32 C31 . . 119.5(3) ? C33 C32 H32 . . 120.3 ? C32 C33 H33 . . 119.7 ? C32 C33 C34 . . 120.5(3) ? C34 C33 H33 . . 119.7 ? N4 C34 C33 . . 121.8(3) ? N4 C34 C38 . . 120.8(3) ? C33 C34 C38 . . 117.3(3) ? N4 C35 C31 . . 122.5(3) ? N4 C35 C36 . . 118.4(2) ? C31 C35 C36 . . 119.2(3) ? N3 C36 C28 . . 122.7(3) ? N3 C36 C35 . . 119.0(2) ? C28 C36 C35 . . 118.3(3) ? C25 C37 H37A . . 109.5 ? C25 C37 H37B . . 109.5 ? C25 C37 H37C . . 109.5 ? H37A C37 H37B . . 109.5 ? H37A C37 H37C . . 109.5 ? H37B C37 H37C . . 109.5 ? C34 C38 H38A . . 109.5 ? C34 C38 H38B . . 109.5 ? C34 C38 H38C . . 109.5 ? H38A C38 H38B . . 109.5 ? H38A C38 H38C . . 109.5 ? H38B C38 H38C . . 109.5 ? F1' P1' F2' . . 179.0(8) ? F1' P1' F3' . . 91.8(6) ? F1' P1' F4' . . 92.1(6) ? F1' P1' F5' . . 91.4(6) ? F1' P1' F6' . . 89.3(6) ? F2' P1' F6' . . 89.9(6) ? F3' P1' F2' . . 88.9(6) ? F3' P1' F4' . . 91.7(5) ? F3' P1' F5' . . 176.1(7) ? F3' P1' F6' . . 87.9(5) ? F4' P1' F2' . . 88.7(6) ? F4' P1' F6' . . 178.6(6) ? F5' P1' F2' . . 87.8(6) ? F5' P1' F4' . . 90.4(5) ? F5' P1' F6' . . 90.0(5) ? H39A C39 H39B . . 109.5 ? H39A C39 H39C . . 109.5 ? H39B C39 H39C . . 109.5 ? C40 C39 H39A . . 109.5 ? C40 C39 H39B . . 109.5 ? C40 C39 H39C . . 109.5 ? C39 C40 H40A . . 108.9 ? C39 C40 H40B . . 108.9 ? H40A C40 H40B . . 107.7 ? O1 C40 C39 . . 113.2(9) ? O1 C40 H40A . . 108.9 ? O1 C40 H40B . . 108.9 ? C40 O1 C41 . . 108.8(7) ? O1 C41 H41A . . 110.7 ? O1 C41 H41B . . 110.7 ? O1 C41 C42 . . 105.4(11) ? H41A C41 H41B . . 108.8 ? C42 C41 H41A . . 110.7 ? C42 C41 H41B . . 110.7 ? C41 C42 H42A . . 109.5 ? C41 C42 H42B . . 109.5 ? C41 C42 H42C . . 109.5 ? H42A C42 H42B . . 109.5 ? H42A C42 H42C . . 109.5 ? H42B C42 H42C . . 109.5 ? N5' C39' C40' . . 178(2) ? C39' C40' H40C . . 109.5 ? C39' C40' H40D . . 109.5 ? C39' C40' H40E . . 109.5 ? H40C C40' H40D . . 109.5 ? H40C C40' H40E . . 109.5 ? H40D C40' H40E . . 109.5 ? N6' C41' C42' . . 156(3) ? C41' C42' H42D . . 109.5 ? C41' C42' H42E . . 109.5 ? C41' C42' H42F . . 109.5 ? H42D C42' H42E . . 109.5 ? H42D C42' H42F . . 109.5 ? H42E C42' H42F . . 109.5 ? F1 P1 F2 . . 178.5(3) ? F1 P1 F3 . . 90.0(3) ? F1 P1 F6 . . 88.8(3) ? F3 P1 F2 . . 89.0(3) ? F4 P1 F1 . . 92.2(3) ? F4 P1 F2 . . 88.9(3) ? F4 P1 F3 . . 90.2(3) ? F4 P1 F5 . . 91.4(3) ? F4 P1 F6 . . 178.4(4) ? F5 P1 F1 . . 91.6(3) ? F5 P1 F2 . . 89.4(3) ? F5 P1 F3 . . 177.7(4) ? F5 P1 F6 . . 89.8(3) ? F6 P1 F2 . . 90.1(3) ? F6 P1 F3 . . 88.6(3) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ir1 N1 . 2.050(2) y Ir1 N2 . 2.051(2) y Ir1 N3 . 2.226(2) y Ir1 N4 . 2.222(2) y Ir1 C1 . 2.018(3) y Ir1 C13 . 2.017(3) y N1 C7 . 1.371(4) ? N1 C11 . 1.343(4) ? N2 C19 . 1.366(4) ? N2 C23 . 1.349(4) ? N3 C25 . 1.339(4) ? N3 C36 . 1.374(4) ? N4 C34 . 1.343(4) ? N4 C35 . 1.380(4) ? C1 C2 . 1.397(4) ? C1 C6 . 1.414(4) ? C2 H2 . 0.9500 ? C2 C3 . 1.393(4) ? C3 C4 . 1.400(5) ? C3 C12 . 1.509(4) ? C4 H4 . 0.9500 ? C4 C5 . 1.382(5) ? C5 H5 . 0.9500 ? C5 C6 . 1.399(4) ? C6 C7 . 1.462(4) ? C7 C8 . 1.392(4) ? C8 H8 . 0.9500 ? C8 C9 . 1.380(5) ? C9 H9 . 0.9500 ? C9 C10 . 1.389(4) ? C10 H10 . 0.9500 ? C10 C11 . 1.386(4) ? C11 H11 . 0.9500 ? C12 H12A . 0.9800 ? C12 H12B . 0.9800 ? C12 H12C . 0.9800 ? C13 C14 . 1.396(4) ? C13 C18 . 1.408(4) ? C14 H14 . 0.9500 ? C14 C15 . 1.396(4) ? C15 C16 . 1.395(5) ? C15 C24 . 1.507(5) ? C16 H16 . 0.9500 ? C16 C17 . 1.392(5) ? C17 H17 . 0.9500 ? C17 C18 . 1.394(4) ? C18 C19 . 1.462(4) ? C19 C20 . 1.393(4) ? C20 H20 . 0.9500 ? C20 C21 . 1.383(5) ? C21 H21 . 0.9500 ? C21 C22 . 1.387(5) ? C22 H22 . 0.9500 ? C22 C23 . 1.378(4) ? C23 H23 . 0.9500 ? C24 H24A . 0.9800 ? C24 H24B . 0.9800 ? C24 H24C . 0.9800 ? C25 C26 . 1.409(4) ? C25 C37 . 1.496(4) ? C26 H26 . 0.9500 ? C26 C27 . 1.362(5) ? C27 H27 . 0.9500 ? C27 C28 . 1.401(4) ? C28 C29 . 1.422(4) ? C28 C36 . 1.414(4) ? C29 H29 . 0.9500 ? C29 C30 . 1.349(5) ? C30 H30 . 0.9500 ? C30 C31 . 1.420(4) ? C31 C32 . 1.406(4) ? C31 C35 . 1.407(4) ? C32 H32 . 0.9500 ? C32 C33 . 1.353(5) ? C33 H33 . 0.9500 ? C33 C34 . 1.412(4) ? C34 C38 . 1.492(4) ? C35 C36 . 1.441(4) ? C37 H37A . 0.9800 ? C37 H37B . 0.9800 ? C37 H37C . 0.9800 ? C38 H38A . 0.9800 ? C38 H38B . 0.9800 ? C38 H38C . 0.9800 ? P1' F1' . 1.576(6) ? P1' F2' . 1.587(6) ? P1' F3' . 1.579(6) ? P1' F4' . 1.583(6) ? P1' F5' . 1.581(6) ? P1' F6' . 1.595(6) ? C39 H39A . 0.9800 ? C39 H39B . 0.9800 ? C39 H39C . 0.9800 ? C39 C40 . 1.538(17) ? C40 H40A . 0.9900 ? C40 H40B . 0.9900 ? C40 O1 . 1.431(10) ? O1 C41 . 1.457(18) ? C41 H41A . 0.9900 ? C41 H41B . 0.9900 ? C41 C42 . 1.553(17) ? C42 H42A . 0.9800 ? C42 H42B . 0.9800 ? C42 H42C . 0.9800 ? N5' C39' . 1.152(9) ? N6' C41' . 1.154(10) ? C39' C40' . 1.468(9) ? C40' H40C . 0.9800 ? C40' H40D . 0.9800 ? C40' H40E . 0.9800 ? C41' C42' . 1.471(10) ? C42' H42D . 0.9800 ? C42' H42E . 0.9800 ? C42' H42F . 0.9800 ? P1 F1 . 1.585(4) ? P1 F2 . 1.600(4) ? P1 F3 . 1.597(4) ? P1 F4 . 1.582(4) ? P1 F5 . 1.583(4) ? P1 F6 . 1.593(4) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C10 H10 F2' . 0.95 2.54 3.270(9) 134.3 yes C10 H10 F2 . 0.95 2.53 3.329(5) 141.9 yes C11 H11 F6' . 0.95 2.53 3.373(9) 148.5 yes C11 H11 F3 . 0.95 2.37 3.140(5) 137.9 yes C22 H22 F6' 1_455 0.95 2.51 3.272(8) 137.8 yes C23 H23 F2 1_455 0.95 2.32 3.194(5) 152.1 yes C26 H26 F3 2_666 0.95 2.52 3.455(5) 167.6 yes C33 H33 F5' 2_756 0.95 2.45 3.372(8) 162.8 yes C37 H37B F3' 2_666 0.98 2.37 3.330(7) 164.7 yes C38 H38B F5 2_756 0.98 2.42 3.393(5) 170.9 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ir1 N1 C7 C6 . . . . 3.0(3) ? Ir1 N1 C7 C8 . . . . -176.3(2) ? Ir1 N1 C11 C10 . . . . 176.3(2) ? Ir1 N2 C19 C18 . . . . 3.4(3) ? Ir1 N2 C19 C20 . . . . -177.2(2) ? Ir1 N2 C23 C22 . . . . 177.2(2) ? Ir1 N3 C25 C26 . . . . -178.4(2) ? Ir1 N3 C25 C37 . . . . 2.4(4) ? Ir1 N3 C36 C28 . . . . 178.3(2) ? Ir1 N3 C36 C35 . . . . -1.8(3) ? Ir1 N4 C34 C33 . . . . 179.0(2) ? Ir1 N4 C34 C38 . . . . 0.2(4) ? Ir1 N4 C35 C31 . . . . -180.0(2) ? Ir1 N4 C35 C36 . . . . 0.2(3) ? Ir1 C1 C2 C3 . . . . 179.1(2) ? Ir1 C1 C6 C5 . . . . -179.6(2) ? Ir1 C1 C6 C7 . . . . -0.9(3) ? Ir1 C13 C14 C15 . . . . 179.4(2) ? Ir1 C13 C18 C17 . . . . -179.8(2) ? Ir1 C13 C18 C19 . . . . -2.7(3) ? N1 C7 C8 C9 . . . . -0.5(4) ? N2 C19 C20 C21 . . . . -0.1(5) ? N3 C25 C26 C27 . . . . 0.5(4) ? N4 C35 C36 N3 . . . . 1.1(4) ? N4 C35 C36 C28 . . . . -179.0(2) ? C1 C2 C3 C4 . . . . 1.6(4) ? C1 C2 C3 C12 . . . . -177.0(3) ? C1 C6 C7 N1 . . . . -1.4(4) ? C1 C6 C7 C8 . . . . 177.9(3) ? C2 C1 C6 C5 . . . . 1.8(4) ? C2 C1 C6 C7 . . . . -179.6(2) ? C2 C3 C4 C5 . . . . 0.0(5) ? C3 C4 C5 C6 . . . . -0.6(5) ? C4 C5 C6 C1 . . . . -0.3(4) ? C4 C5 C6 C7 . . . . -178.8(3) ? C5 C6 C7 N1 . . . . 177.2(3) ? C5 C6 C7 C8 . . . . -3.5(5) ? C6 C1 C2 C3 . . . . -2.4(4) ? C6 C7 C8 C9 . . . . -179.7(3) ? C7 N1 C11 C10 . . . . -0.4(4) ? C7 C8 C9 C10 . . . . 0.0(5) ? C8 C9 C10 C11 . . . . 0.3(5) ? C9 C10 C11 N1 . . . . -0.1(5) ? C11 N1 C7 C6 . . . . 180.0(2) ? C11 N1 C7 C8 . . . . 0.7(4) ? C12 C3 C4 C5 . . . . 178.6(3) ? C13 C14 C15 C16 . . . . 1.7(5) ? C13 C14 C15 C24 . . . . -179.9(3) ? C13 C18 C19 N2 . . . . -0.5(4) ? C13 C18 C19 C20 . . . . -179.8(3) ? C14 C13 C18 C17 . . . . 2.0(4) ? C14 C13 C18 C19 . . . . 179.1(3) ? C14 C15 C16 C17 . . . . 0.0(5) ? C15 C16 C17 C18 . . . . -0.6(5) ? C16 C17 C18 C13 . . . . -0.4(5) ? C16 C17 C18 C19 . . . . -177.3(3) ? C17 C18 C19 N2 . . . . 176.5(3) ? C17 C18 C19 C20 . . . . -2.8(5) ? C18 C13 C14 C15 . . . . -2.7(4) ? C18 C19 C20 C21 . . . . 179.1(3) ? C19 N2 C23 C22 . . . . 0.1(4) ? C19 C20 C21 C22 . . . . -0.2(5) ? C20 C21 C22 C23 . . . . 0.5(5) ? C21 C22 C23 N2 . . . . -0.4(5) ? C23 N2 C19 C18 . . . . -179.1(2) ? C23 N2 C19 C20 . . . . 0.2(4) ? C24 C15 C16 C17 . . . . -178.4(3) ? C25 N3 C36 C28 . . . . -0.2(4) ? C25 N3 C36 C35 . . . . 179.8(2) ? C25 C26 C27 C28 . . . . -0.4(4) ? C26 C27 C28 C29 . . . . -178.8(3) ? C26 C27 C28 C36 . . . . 0.0(4) ? C27 C28 C29 C30 . . . . 179.2(3) ? C27 C28 C36 N3 . . . . 0.2(4) ? C27 C28 C36 C35 . . . . -179.7(3) ? C28 C29 C30 C31 . . . . -0.2(5) ? C29 C28 C36 N3 . . . . 179.1(3) ? C29 C28 C36 C35 . . . . -0.8(4) ? C29 C30 C31 C32 . . . . 178.8(3) ? C29 C30 C31 C35 . . . . 0.6(5) ? C30 C31 C32 C33 . . . . -178.7(3) ? C30 C31 C35 N4 . . . . 179.0(3) ? C30 C31 C35 C36 . . . . -1.1(4) ? C31 C32 C33 C34 . . . . -0.4(4) ? C31 C35 C36 N3 . . . . -178.8(2) ? C31 C35 C36 C28 . . . . 1.2(4) ? C32 C31 C35 N4 . . . . 0.8(4) ? C32 C31 C35 C36 . . . . -179.4(3) ? C32 C33 C34 N4 . . . . 1.1(4) ? C32 C33 C34 C38 . . . . 180.0(3) ? C34 N4 C35 C31 . . . . -0.2(4) ? C34 N4 C35 C36 . . . . 180.0(2) ? C35 N4 C34 C33 . . . . -0.8(4) ? C35 N4 C34 C38 . . . . -179.6(3) ? C35 C31 C32 C33 . . . . -0.4(4) ? C36 N3 C25 C26 . . . . -0.2(4) ? C36 N3 C25 C37 . . . . -179.4(3) ? C36 C28 C29 C30 . . . . 0.3(5) ? C37 C25 C26 C27 . . . . 179.8(3) ? C39 C40 O1 C41 . . . . -173.7(13) ? C40 O1 C41 C42 . . . . -175.2(10) ?